data_global _audit_creation_method 'APEX2 v2013.6-2' _publ_requested_journal 'Organometallics' loop_ _publ_contact_author_name _publ_contact_author_address 'Ryan J. Trovitch' ; Department of Chemistry and Biochemistry Arizona State University Tempe, AZ 85287 ; 'John C. Gordon' ; Chemistry Division Los Alamos National Laboratory Los Alamos, NM 87545 ; loop_ _publ_contact_author_email _publ_contact_author_fax _publ_contact_author_phone 'ryan.trovitch@asu.edu' '480-965-2747' '480-727-8930' 'jgordon@lanl.gov' '505-667-9905' '505-665-6962' loop_ _publ_author_name _publ_author_address 'Tufan K. Mukhopadhyay' ;Department of Chemistry and Biochemistry Arizona State University Tempe, AZ 85287 ; 'Marco Flores' ;Department of Chemistry and Biochemistry Arizona State University Tempe, AZ 85287 ; 'Russell K. Feller' ;Materials Physics and Applications Division Los Alamos National Laboratory Los Alamos, NM 87545 ; 'Brian L. Scott' ;Materials Physics and Applications Division Los Alamos National Laboratory Los Alamos, NM 87545 ; 'R. Dean Taylor' ;Materials Physics and Applications Division Los Alamos National Laboratory Los Alamos, NM 87545 ; 'Moshe Paz-Pasternak' ;School of Physics and Astronomy Tel Aviv University 69978 Tel Aviv, Israel ; 'Neil J. Henson' ;Theoretical Division Los Alamos National Laboratory Los Alamos, NM 87545 ; 'Francisca N. Rein' ;Chemistry Division Los Alamos National Laboratory Los Alamos, NM 87545 ; 'Nathan C. Smythe' ;Chemistry Division Los Alamos National Laboratory Los Alamos, NM 87545 ; 'Ryan J. Trovitch' ;Department of Chemistry and Biochemistry Arizona State University Tempe, AZ 85287 ; 'John C. Gordon' ;Chemistry Division Los Alamos National Laboratory Los Alamos, NM 87545 ; _publ_section_title ; A New Spin on Cyclooctatetraene (COT) Redox-Activity: Low-Spin Fe(I) Complexes that Exhibit Antiferromagnetic Coupling to a Singly Reduced \e^4^-COT Ligand ; _publ_section_abstract ; ; _publ_section_references ; ; _publ_section_comment ; ; data_TriphosFeCOT _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C42 H41 Fe P3, C7 H8' _chemical_formula_sum 'C49 H49 Fe P3' _chemical_formula_iupac ? _chemical_formula_weight 786.64 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.8369(13) _cell_length_b 21.470(2) _cell_length_c 15.3475(15) _cell_angle_alpha 90 _cell_angle_beta 107.5420(10) _cell_angle_gamma 90 _cell_volume 4033.2(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 140.(2) _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.527 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.95 _exptl_special_details ; ; _diffrn_ambient_temperature 140.(2) _diffrn_source 'fine-focus sealed tube' _diffrn_source_type ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44849 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.87 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measured_fraction_theta_full 0.982 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _reflns_number_total 9426 _reflns_number_gt 8284 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.0792 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_number_reflns 9426 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+2.3037P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.433 _refine_diff_density_min -0.304 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material 'Bruker APEX2 v1013.6-2 (Bruker-AXS, 2013)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe1 0.39543(2) 0.23692(2) -0.05160(2) 0.01378(6) Uani d . . . 1 . . P P1 0.57377(3) 0.22853(2) -0.00556(2) 0.01529(8) Uani d . . . 1 . . P P2 0.42335(3) 0.32526(2) 0.02124(2) 0.01593(8) Uani d . . . 1 . . P P3 0.36223(3) 0.19800(2) 0.06934(2) 0.01398(7) Uani d . . . 1 . . C C1 0.23477(12) 0.27170(7) -0.13360(10) 0.0220(3) Uani d . . . 1 . . H H1 0.2229(15) 0.3147(9) -0.1205(12) 0.026 Uiso d U . . 1 . . C C2 0.31627(12) 0.26743(7) -0.17968(10) 0.0215(3) Uani d . . . 1 . . H H2 0.3373(15) 0.3053(9) -0.2015(12) 0.026 Uiso d U . . 1 . . C C3 0.37731(12) 0.21397(7) -0.18386(9) 0.0206(3) Uani d . . . 1 . . H H3 0.4359(15) 0.2189(8) -0.2072(12) 0.025 Uiso d U . . 1 . . C C4 0.36677(12) 0.15500(7) -0.14374(9) 0.0200(3) Uani d . . . 1 . . H H4 0.4329(15) 0.1301(8) -0.1344(12) 0.024 Uiso d U . . 1 . . C C5 0.27395(12) 0.11381(7) -0.15729(9) 0.0212(3) Uani d . . . 1 . . H H5 0.2936 0.0711 -0.1561 0.025 Uiso calc U . R 1 . . C C6 0.16522(12) 0.12220(7) -0.17129(10) 0.0225(3) Uani d . . . 1 . . H H6 0.1219 0.086 -0.1909 0.027 Uiso calc U . R 1 . . C C7 0.10524(12) 0.17621(7) -0.16144(10) 0.0224(3) Uani d . . . 1 . . H H7 0.0294 0.1692 -0.172 0.027 Uiso calc U . R 1 . . C C8 0.13760(12) 0.23579(7) -0.13966(10) 0.0219(3) Uani d . . . 1 . . H H8 0.0832 0.2598 -0.1247 0.026 Uiso calc U . R 1 . . C C9 0.62896(11) 0.27610(7) 0.09863(9) 0.0187(3) Uani d . . . 1 . . H H9A 0.6155 0.2554 0.1518 0.022 Uiso calc U . R 1 . . H H9B 0.7087 0.282 0.1116 0.022 Uiso calc U . R 1 . . C C10 0.57012(11) 0.33866(7) 0.08029(9) 0.0195(3) Uani d . . . 1 . . H H10A 0.6021 0.3649 0.0418 0.023 Uiso calc U . R 1 . . H H10B 0.5789 0.3607 0.1387 0.023 Uiso calc U . R 1 . . C C11 0.36531(12) 0.32275(6) 0.11715(10) 0.0194(3) Uani d . . . 1 . . H H11A 0.3998 0.355 0.1629 0.023 Uiso calc U . R 1 . . H H11B 0.2857 0.3309 0.0949 0.023 Uiso calc U . R 1 . . C C12 0.38702(11) 0.25794(6) 0.16041(9) 0.0174(3) Uani d . . . 1 . . H H12A 0.3382 0.2505 0.1985 0.021 Uiso calc U . R 1 . . H H12B 0.4635 0.2553 0.2002 0.021 Uiso calc U . R 1 . . C C13 0.64978(12) 0.26585(6) -0.07697(10) 0.0191(3) Uani d . . . 1 . . C C14 0.76249(13) 0.25822(8) -0.05794(12) 0.0283(3) Uani d . . . 1 . . H H14 0.8004 0.2298 -0.0118 0.034 Uiso calc U . R 1 . . C C15 0.81961(15) 0.29188(9) -0.10611(13) 0.0368(4) Uani d . . . 1 . . H H15 0.8962 0.2862 -0.0927 0.044 Uiso calc U . R 1 . . C C16 0.76592(15) 0.33337(8) -0.17316(13) 0.0346(4) Uani d . . . 1 . . H H16 0.8056 0.3566 -0.2053 0.042 Uiso calc U . R 1 . . C C17 0.65421(14) 0.34111(8) -0.19352(11) 0.0285(3) Uani d . . . 1 . . H H17 0.6167 0.3693 -0.2401 0.034 Uiso calc U . R 1 . . C C18 0.59687(12) 0.30736(7) -0.14538(10) 0.0220(3) Uani d . . . 1 . . H H18 0.5201 0.3129 -0.1596 0.026 Uiso calc U . R 1 . . C C19 0.65233(11) 0.15619(6) 0.02410(10) 0.0183(3) Uani d . . . 1 . . C C20 0.70296(12) 0.13826(7) 0.11427(10) 0.0223(3) Uani d . . . 1 . . H H20 0.6978 0.1642 0.1629 0.027 Uiso calc U . R 1 . . C C21 0.76095(12) 0.08273(7) 0.13370(11) 0.0275(3) Uani d . . . 1 . . H H21 0.7952 0.0711 0.1954 0.033 Uiso calc U . R 1 . . C C22 0.76920(12) 0.04427(7) 0.06382(12) 0.0279(3) Uani d . . . 1 . . H H22 0.8092 0.0064 0.0774 0.034 Uiso calc U . R 1 . . C C23 0.71871(12) 0.06130(7) -0.02631(12) 0.0263(3) Uani d . . . 1 . . H H23 0.724 0.035 -0.0746 0.032 Uiso calc U . R 1 . . C C24 0.66048(12) 0.11666(7) -0.04587(10) 0.0226(3) Uani d . . . 1 . . H H24 0.6257 0.1278 -0.1077 0.027 Uiso calc U . R 1 . . C C25 0.37891(12) 0.40187(6) -0.02922(10) 0.0224(3) Uani d . . . 1 . . C C26 0.43171(16) 0.42904(7) -0.08726(11) 0.0326(4) Uani d . . . 1 . . H H26 0.4921 0.4084 -0.0981 0.039 Uiso calc U . R 1 . . C C27 0.39689(18) 0.48603(8) -0.12944(12) 0.0389(4) Uani d . . . 1 . . H H27 0.4338 0.504 -0.1685 0.047 Uiso calc U . R 1 . . C C28 0.30939(15) 0.51640(7) -0.11479(13) 0.0392(5) Uani d . . . 1 . . H H28 0.2846 0.5548 -0.1448 0.047 Uiso calc U . R 1 . . C C29 0.25814(15) 0.49103(8) -0.05673(15) 0.0423(5) Uani d . . . 1 . . H H29 0.1988 0.5125 -0.0454 0.051 Uiso calc U . R 1 . . C C30 0.29223(13) 0.43394(7) -0.01412(13) 0.0330(4) Uani d . . . 1 . . H H30 0.2556 0.4169 0.0257 0.04 Uiso calc U . R 1 . . C C31 0.44007(10) 0.13102(6) 0.12977(9) 0.0160(3) Uani d . . . 1 . . C C32 0.45349(11) 0.07946(6) 0.07893(9) 0.0189(3) Uani d . . . 1 . . H H32 0.4264 0.0808 0.0141 0.023 Uiso calc U . R 1 . . C C33 0.50598(12) 0.02616(7) 0.12176(10) 0.0224(3) Uani d . . . 1 . . H H33 0.5127 -0.009 0.0863 0.027 Uiso calc U . R 1 . . C C34 0.54848(13) 0.02418(7) 0.21597(11) 0.0270(3) Uani d . . . 1 . . H H34 0.5842 -0.0123 0.2454 0.032 Uiso calc U . R 1 . . C C35 0.53854(14) 0.07577(8) 0.26720(10) 0.0291(3) Uani d . . . 1 . . H H35 0.569 0.0749 0.3318 0.035 Uiso calc U . R 1 . . C C36 0.48428(12) 0.12867(7) 0.22454(10) 0.0216(3) Uani d . . . 1 . . H H36 0.4772 0.1636 0.2603 0.026 Uiso calc U . R 1 . . C C37 0.22282(11) 0.17243(7) 0.06360(9) 0.0179(3) Uani d . . . 1 . . C C38 0.18987(12) 0.11065(7) 0.04689(10) 0.0242(3) Uani d . . . 1 . . H H38 0.2405 0.0802 0.0398 0.029 Uiso calc U . R 1 . . C C39 0.08323(13) 0.09303(8) 0.04047(12) 0.0322(4) Uani d . . . 1 . . H H39 0.0618 0.0507 0.0288 0.039 Uiso calc U . R 1 . . C C40 0.00875(13) 0.13623(9) 0.05090(12) 0.0336(4) Uani d . . . 1 . . H H40 -0.0639 0.124 0.0461 0.04 Uiso calc U . R 1 . . C C41 0.04089(13) 0.19766(8) 0.06847(12) 0.0308(3) Uani d . . . 1 . . H H41 -0.0096 0.2277 0.0767 0.037 Uiso calc U . R 1 . . C C42 0.14643(12) 0.21551(7) 0.07413(11) 0.0244(3) Uani d . . . 1 . . H H42 0.1671 0.2579 0.0854 0.029 Uiso calc U . R 1 . . C C43 0.7256(3) 0.06005(13) 0.7161(3) 0.0859(11) Uani d . . . 1 . . C C44 0.7107(3) 0.11936(12) 0.7451(2) 0.0732(9) Uani d . . . 1 . . H H44 0.7671 0.138 0.7929 0.088 Uiso calc U . R 1 . . C C45 0.6160(3) 0.15200(14) 0.7062(2) 0.0800(10) Uani d . . . 1 . . H H45 0.6077 0.1929 0.7267 0.096 Uiso calc U . R 1 . . C C46 0.5331(3) 0.1252(2) 0.6373(3) 0.0944(11) Uani d . . . 1 . . H H46 0.4671 0.1471 0.6098 0.113 Uiso calc U . R 1 . . C C47 0.5484(4) 0.0658(3) 0.6093(3) 0.1264(18) Uani d . . . 1 . . H H47 0.4934 0.0462 0.5614 0.152 Uiso calc U . R 1 . . C C48 0.6474(5) 0.03442(19) 0.6531(4) 0.1195(18) Uani d . . . 1 . . H H48 0.6565 -0.0071 0.6353 0.143 Uiso calc U . R 1 . . C C49 0.8286(4) 0.02411(18) 0.7575(3) 0.138(2) Uani d . . . 1 . . H H49A 0.8745 0.0465 0.811 0.206 Uiso calc U . R 1 . . H H49B 0.8683 0.0194 0.7123 0.206 Uiso calc U . R 1 . . H H49C 0.8106 -0.0171 0.7761 0.206 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.01396(10) 0.01357(10) 0.01183(9) -0.00139(7) 0.00088(7) 0.00034(7) P1 0.01421(16) 0.01689(16) 0.01360(16) -0.00174(12) 0.00242(12) 0.00035(12) P2 0.01786(16) 0.01309(16) 0.01501(16) -0.00211(12) 0.00217(13) 0.00028(12) P3 0.01299(15) 0.01372(16) 0.01387(15) -0.00142(12) 0.00203(12) 0.00028(12) C1 0.0203(7) 0.0177(7) 0.0216(7) 0.0016(5) -0.0033(6) 0.0009(5) C2 0.0224(7) 0.0215(7) 0.0146(6) -0.0050(5) -0.0034(5) 0.0039(5) C3 0.0209(7) 0.0267(7) 0.0122(6) -0.0056(6) 0.0021(5) -0.0017(5) C4 0.0194(7) 0.0208(7) 0.0176(6) 0.0001(5) 0.0021(5) -0.0029(5) C5 0.0257(7) 0.0173(6) 0.0173(6) -0.0021(5) 0.0015(5) -0.0016(5) C6 0.0236(7) 0.0206(7) 0.0182(7) -0.0060(6) -0.0014(5) -0.0004(5) C7 0.0161(6) 0.0271(7) 0.0188(7) -0.0020(5) -0.0026(5) 0.0037(6) C8 0.0177(7) 0.0246(7) 0.0188(7) 0.0035(5) -0.0015(5) 0.0028(5) C9 0.0161(6) 0.0230(7) 0.0147(6) -0.0040(5) 0.0009(5) -0.0025(5) C10 0.0199(7) 0.0191(7) 0.0181(6) -0.0062(5) 0.0035(5) -0.0029(5) C11 0.0215(7) 0.0167(6) 0.0205(7) -0.0012(5) 0.0069(5) -0.0023(5) C12 0.0189(6) 0.0174(6) 0.0157(6) -0.0025(5) 0.0052(5) -0.0022(5) C13 0.0202(7) 0.0193(7) 0.0191(7) -0.0036(5) 0.0077(5) -0.0018(5) C14 0.0230(8) 0.0302(8) 0.0337(8) -0.0003(6) 0.0114(7) 0.0054(7) C15 0.0274(8) 0.0408(10) 0.0489(11) -0.0004(7) 0.0217(8) 0.0072(8) C16 0.0398(9) 0.0339(9) 0.0403(10) -0.0053(7) 0.0271(8) 0.0032(7) C17 0.0386(9) 0.0252(8) 0.0244(7) -0.0036(7) 0.0133(7) 0.0030(6) C18 0.0246(7) 0.0221(7) 0.0198(7) -0.0033(6) 0.0073(6) -0.0005(5) C19 0.0132(6) 0.0188(6) 0.0214(7) -0.0019(5) 0.0028(5) 0.0020(5) C20 0.0179(7) 0.0251(7) 0.0218(7) -0.0020(5) 0.0029(5) 0.0024(6) C21 0.0197(7) 0.0286(8) 0.0299(8) -0.0007(6) 0.0010(6) 0.0105(6) C22 0.0189(7) 0.0198(7) 0.0430(9) -0.0010(6) 0.0062(6) 0.0059(6) C23 0.0220(7) 0.0198(7) 0.0367(9) -0.0019(6) 0.0086(6) -0.0031(6) C24 0.0201(7) 0.0226(7) 0.0234(7) -0.0018(6) 0.0039(6) -0.0005(6) C25 0.0269(7) 0.0147(6) 0.0194(7) -0.0035(5) -0.0023(6) -0.0010(5) C26 0.0525(11) 0.0194(7) 0.0264(8) -0.0007(7) 0.0125(7) 0.0019(6) C27 0.0639(13) 0.0206(8) 0.0266(8) -0.0083(8) 0.0054(8) 0.0043(6) C28 0.0423(10) 0.0156(7) 0.0397(10) -0.0096(7) -0.0178(8) 0.0058(7) C29 0.0274(9) 0.0200(8) 0.0679(13) 0.0021(7) -0.0030(8) 0.0069(8) C30 0.0252(8) 0.0201(7) 0.0488(10) -0.0002(6) 0.0040(7) 0.0070(7) C31 0.0131(6) 0.0157(6) 0.0181(6) -0.0014(5) 0.0031(5) 0.0024(5) C32 0.0178(6) 0.0187(6) 0.0178(6) -0.0011(5) 0.0019(5) 0.0003(5) C33 0.0215(7) 0.0175(7) 0.0269(7) 0.0005(5) 0.0055(6) -0.0002(6) C34 0.0277(8) 0.0218(7) 0.0281(8) 0.0069(6) 0.0034(6) 0.0078(6) C35 0.0347(8) 0.0305(8) 0.0180(7) 0.0070(7) 0.0016(6) 0.0052(6) C36 0.0238(7) 0.0214(7) 0.0182(7) 0.0022(6) 0.0044(6) 0.0006(5) C37 0.0149(6) 0.0219(7) 0.0153(6) -0.0033(5) 0.0022(5) 0.0024(5) C38 0.0210(7) 0.0221(7) 0.0274(7) -0.0040(6) 0.0043(6) 0.0004(6) C39 0.0257(8) 0.0289(8) 0.0385(9) -0.0119(7) 0.0043(7) 0.0023(7) C40 0.0169(7) 0.0464(10) 0.0359(9) -0.0093(7) 0.0055(6) 0.0052(8) C41 0.0176(7) 0.0390(9) 0.0348(9) 0.0017(6) 0.0066(6) 0.0015(7) C42 0.0182(7) 0.0246(7) 0.0293(8) -0.0012(6) 0.0053(6) 0.0016(6) C43 0.134(3) 0.0460(14) 0.119(3) 0.0071(17) 0.101(3) 0.0182(16) C44 0.115(2) 0.0579(15) 0.0753(17) 0.0171(15) 0.0723(18) 0.0220(13) C45 0.121(3) 0.0619(17) 0.089(2) 0.0222(18) 0.079(2) 0.0263(16) C46 0.090(2) 0.112(3) 0.102(3) -0.006(2) 0.060(2) 0.016(2) C47 0.124(4) 0.150(4) 0.135(4) -0.079(3) 0.083(3) -0.035(3) C48 0.143(4) 0.075(2) 0.191(5) -0.034(3) 0.127(4) -0.013(3) C49 0.215(5) 0.096(3) 0.158(4) 0.089(3) 0.142(4) 0.077(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 C2 . 2.0302(14) ? Fe1 C3 . 2.0330(14) ? Fe1 P2 . 2.1758(4) ? Fe1 P1 . 2.1903(4) ? Fe1 P3 . 2.1913(4) ? Fe1 C1 . 2.1978(14) ? Fe1 C4 . 2.2170(14) ? P1 C19 . 1.8332(14) ? P1 C9 . 1.8490(14) ? P1 C13 . 1.8547(14) ? P2 C25 . 1.8342(15) ? P2 C11 . 1.8401(14) ? P2 C10 . 1.8506(14) ? P3 C31 . 1.8353(14) ? P3 C37 . 1.8485(14) ? P3 C12 . 1.8554(14) ? C1 C2 . 1.432(2) ? C1 C8 . 1.445(2) ? C1 H1 . 0.966(18) ? C2 C3 . 1.402(2) ? C2 H2 . 0.949(18) ? C3 C4 . 1.432(2) ? C3 H3 . 0.932(18) ? C4 C5 . 1.448(2) ? C4 H4 . 0.976(18) ? C5 C6 . 1.359(2) ? C5 H5 . 0.95 ? C6 C7 . 1.425(2) ? C6 H6 . 0.95 ? C7 C8 . 1.355(2) ? C7 H7 . 0.95 ? C8 H8 . 0.95 ? C9 C10 . 1.525(2) ? C9 H9A . 0.99 ? C9 H9B . 0.99 ? C10 H10A . 0.99 ? C10 H10B . 0.99 ? C11 C12 . 1.5307(19) ? C11 H11A . 0.99 ? C11 H11B . 0.99 ? C12 H12A . 0.99 ? C12 H12B . 0.99 ? C13 C18 . 1.389(2) ? C13 C14 . 1.397(2) ? C14 C15 . 1.390(2) ? C14 H14 . 0.95 ? C15 C16 . 1.378(3) ? C15 H15 . 0.95 ? C16 C17 . 1.382(2) ? C16 H16 . 0.95 ? C17 C18 . 1.393(2) ? C17 H17 . 0.95 ? C18 H18 . 0.95 ? C19 C20 . 1.394(2) ? C19 C24 . 1.397(2) ? C20 C21 . 1.389(2) ? C20 H20 . 0.95 ? C21 C22 . 1.383(2) ? C21 H21 . 0.95 ? C22 C23 . 1.388(2) ? C22 H22 . 0.95 ? C23 C24 . 1.388(2) ? C23 H23 . 0.95 ? C24 H24 . 0.95 ? C25 C30 . 1.386(2) ? C25 C26 . 1.399(2) ? C26 C27 . 1.393(2) ? C26 H26 . 0.95 ? C27 C28 . 1.375(3) ? C27 H27 . 0.95 ? C28 C29 . 1.370(3) ? C28 H28 . 0.95 ? C29 C30 . 1.396(2) ? C29 H29 . 0.95 ? C30 H30 . 0.95 ? C31 C36 . 1.3938(19) ? C31 C32 . 1.3946(19) ? C32 C33 . 1.389(2) ? C32 H32 . 0.95 ? C33 C34 . 1.384(2) ? C33 H33 . 0.95 ? C34 C35 . 1.386(2) ? C34 H34 . 0.95 ? C35 C36 . 1.389(2) ? C35 H35 . 0.95 ? C36 H36 . 0.95 ? C37 C38 . 1.392(2) ? C37 C42 . 1.392(2) ? C38 C39 . 1.395(2) ? C38 H38 . 0.95 ? C39 C40 . 1.376(3) ? C39 H39 . 0.95 ? C40 C41 . 1.384(3) ? C40 H40 . 0.95 ? C41 C42 . 1.385(2) ? C41 H41 . 0.95 ? C42 H42 . 0.95 ? C43 C48 . 1.289(6) ? C43 C44 . 1.381(4) ? C43 C49 . 1.497(5) ? C44 C45 . 1.374(4) ? C44 H44 . 0.95 ? C45 C46 . 1.380(5) ? C45 H45 . 0.95 ? C46 C47 . 1.379(6) ? C46 H46 . 0.95 ? C47 C48 . 1.416(7) ? C47 H47 . 0.95 ? C48 H48 . 0.95 ? C49 H49A . 0.98 ? C49 H49B . 0.98 ? C49 H49C . 0.98 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 Fe1 C3 . . 40.38(6) ? C2 Fe1 P2 . . 99.96(4) ? C3 Fe1 P2 . . 132.52(4) ? C2 Fe1 P1 . . 120.55(5) ? C3 Fe1 P1 . . 95.51(4) ? P2 Fe1 P1 . . 84.929(14) ? C2 Fe1 P3 . . 140.79(5) ? C3 Fe1 P3 . . 139.50(4) ? P2 Fe1 P3 . . 86.625(15) ? P1 Fe1 P3 . . 98.432(15) ? C2 Fe1 C1 . . 39.33(6) ? C3 Fe1 C1 . . 72.87(6) ? P2 Fe1 C1 . . 88.79(4) ? P1 Fe1 C1 . . 157.19(4) ? P3 Fe1 C1 . . 103.07(4) ? C2 Fe1 C4 . . 72.54(6) ? C3 Fe1 C4 . . 39.08(6) ? P2 Fe1 C4 . . 171.60(4) ? P1 Fe1 C4 . . 95.56(4) ? P3 Fe1 C4 . . 101.57(4) ? C1 Fe1 C4 . . 87.57(5) ? C19 P1 C9 . . 102.38(6) ? C19 P1 C13 . . 99.48(6) ? C9 P1 C13 . . 98.04(6) ? C19 P1 Fe1 . . 126.37(4) ? C9 P1 Fe1 . . 108.93(5) ? C13 P1 Fe1 . . 117.31(5) ? C25 P2 C11 . . 102.40(7) ? C25 P2 C10 . . 102.04(7) ? C11 P2 C10 . . 102.17(7) ? C25 P2 Fe1 . . 125.63(5) ? C11 P2 Fe1 . . 109.98(5) ? C10 P2 Fe1 . . 111.89(5) ? C31 P3 C37 . . 99.39(6) ? C31 P3 C12 . . 102.67(6) ? C37 P3 C12 . . 100.70(6) ? C31 P3 Fe1 . . 120.77(5) ? C37 P3 Fe1 . . 120.36(4) ? C12 P3 Fe1 . . 109.92(5) ? C2 C1 C8 . . 132.78(14) ? C2 C1 Fe1 . . 64.00(8) ? C8 C1 Fe1 . . 119.88(10) ? C2 C1 H1 . . 110.4(11) ? C8 C1 H1 . . 109.6(11) ? Fe1 C1 H1 . . 112.6(11) ? C3 C2 C1 . . 125.22(13) ? C3 C2 Fe1 . . 69.92(8) ? C1 C2 Fe1 . . 76.67(8) ? C3 C2 H2 . . 117.6(11) ? C1 C2 H2 . . 116.6(11) ? Fe1 C2 H2 . . 120.3(11) ? C2 C3 C4 . . 125.28(14) ? C2 C3 Fe1 . . 69.71(8) ? C4 C3 Fe1 . . 77.42(8) ? C2 C3 H3 . . 116.8(11) ? C4 C3 H3 . . 117.3(11) ? Fe1 C3 H3 . . 119.6(11) ? C3 C4 C5 . . 131.21(13) ? C3 C4 Fe1 . . 63.50(8) ? C5 C4 Fe1 . . 123.19(10) ? C3 C4 H4 . . 110.9(10) ? C5 C4 H4 . . 109.2(10) ? Fe1 C4 H4 . . 111.8(10) ? C6 C5 C4 . . 134.71(14) ? C6 C5 H5 . . 112.6 ? C4 C5 H5 . . 112.6 ? C5 C6 C7 . . 130.79(13) ? C5 C6 H6 . . 114.6 ? C7 C6 H6 . . 114.6 ? C8 C7 C6 . . 131.23(14) ? C8 C7 H7 . . 114.4 ? C6 C7 H7 . . 114.4 ? C7 C8 C1 . . 135.54(14) ? C7 C8 H8 . . 112.2 ? C1 C8 H8 . . 112.2 ? C10 C9 P1 . . 106.71(9) ? C10 C9 H9A . . 110.4 ? P1 C9 H9A . . 110.4 ? C10 C9 H9B . . 110.4 ? P1 C9 H9B . . 110.4 ? H9A C9 H9B . . 108.6 ? C9 C10 P2 . . 109.14(9) ? C9 C10 H10A . . 109.9 ? P2 C10 H10A . . 109.9 ? C9 C10 H10B . . 109.9 ? P2 C10 H10B . . 109.9 ? H10A C10 H10B . . 108.3 ? C12 C11 P2 . . 107.99(9) ? C12 C11 H11A . . 110.1 ? P2 C11 H11A . . 110.1 ? C12 C11 H11B . . 110.1 ? P2 C11 H11B . . 110.1 ? H11A C11 H11B . . 108.4 ? C11 C12 P3 . . 109.65(9) ? C11 C12 H12A . . 109.7 ? P3 C12 H12A . . 109.7 ? C11 C12 H12B . . 109.7 ? P3 C12 H12B . . 109.7 ? H12A C12 H12B . . 108.2 ? C18 C13 C14 . . 118.25(13) ? C18 C13 P1 . . 119.96(11) ? C14 C13 P1 . . 121.47(11) ? C15 C14 C13 . . 120.46(15) ? C15 C14 H14 . . 119.8 ? C13 C14 H14 . . 119.8 ? C16 C15 C14 . . 120.51(16) ? C16 C15 H15 . . 119.7 ? C14 C15 H15 . . 119.7 ? C15 C16 C17 . . 119.84(15) ? C15 C16 H16 . . 120.1 ? C17 C16 H16 . . 120.1 ? C16 C17 C18 . . 119.70(15) ? C16 C17 H17 . . 120.1 ? C18 C17 H17 . . 120.1 ? C13 C18 C17 . . 121.24(14) ? C13 C18 H18 . . 119.4 ? C17 C18 H18 . . 119.4 ? C20 C19 C24 . . 118.35(13) ? C20 C19 P1 . . 122.51(11) ? C24 C19 P1 . . 119.13(11) ? C21 C20 C19 . . 120.61(14) ? C21 C20 H20 . . 119.7 ? C19 C20 H20 . . 119.7 ? C22 C21 C20 . . 120.49(15) ? C22 C21 H21 . . 119.8 ? C20 C21 H21 . . 119.8 ? C21 C22 C23 . . 119.59(14) ? C21 C22 H22 . . 120.2 ? C23 C22 H22 . . 120.2 ? C24 C23 C22 . . 120.02(15) ? C24 C23 H23 . . 120.0 ? C22 C23 H23 . . 120.0 ? C23 C24 C19 . . 120.94(14) ? C23 C24 H24 . . 119.5 ? C19 C24 H24 . . 119.5 ? C30 C25 C26 . . 117.83(14) ? C30 C25 P2 . . 122.55(12) ? C26 C25 P2 . . 119.61(12) ? C27 C26 C25 . . 120.85(17) ? C27 C26 H26 . . 119.6 ? C25 C26 H26 . . 119.6 ? C28 C27 C26 . . 120.27(18) ? C28 C27 H27 . . 119.9 ? C26 C27 H27 . . 119.9 ? C29 C28 C27 . . 119.60(16) ? C29 C28 H28 . . 120.2 ? C27 C28 H28 . . 120.2 ? C28 C29 C30 . . 120.63(18) ? C28 C29 H29 . . 119.7 ? C30 C29 H29 . . 119.7 ? C25 C30 C29 . . 120.79(17) ? C25 C30 H30 . . 119.6 ? C29 C30 H30 . . 119.6 ? C36 C31 C32 . . 118.37(12) ? C36 C31 P3 . . 122.96(11) ? C32 C31 P3 . . 118.66(10) ? C33 C32 C31 . . 120.89(13) ? C33 C32 H32 . . 119.6 ? C31 C32 H32 . . 119.6 ? C34 C33 C32 . . 120.14(14) ? C34 C33 H33 . . 119.9 ? C32 C33 H33 . . 119.9 ? C33 C34 C35 . . 119.57(14) ? C33 C34 H34 . . 120.2 ? C35 C34 H34 . . 120.2 ? C34 C35 C36 . . 120.33(14) ? C34 C35 H35 . . 119.8 ? C36 C35 H35 . . 119.8 ? C35 C36 C31 . . 120.67(14) ? C35 C36 H36 . . 119.7 ? C31 C36 H36 . . 119.7 ? C38 C37 C42 . . 117.95(13) ? C38 C37 P3 . . 121.86(11) ? C42 C37 P3 . . 120.18(11) ? C37 C38 C39 . . 120.58(15) ? C37 C38 H38 . . 119.7 ? C39 C38 H38 . . 119.7 ? C40 C39 C38 . . 120.71(15) ? C40 C39 H39 . . 119.6 ? C38 C39 H39 . . 119.6 ? C39 C40 C41 . . 119.23(15) ? C39 C40 H40 . . 120.4 ? C41 C40 H40 . . 120.4 ? C40 C41 C42 . . 120.28(15) ? C40 C41 H41 . . 119.9 ? C42 C41 H41 . . 119.9 ? C41 C42 C37 . . 121.24(15) ? C41 C42 H42 . . 119.4 ? C37 C42 H42 . . 119.4 ? C48 C43 C44 . . 118.9(4) ? C48 C43 C49 . . 119.1(4) ? C44 C43 C49 . . 122.0(4) ? C45 C44 C43 . . 121.4(4) ? C45 C44 H44 . . 119.3 ? C43 C44 H44 . . 119.3 ? C44 C45 C46 . . 119.8(3) ? C44 C45 H45 . . 120.1 ? C46 C45 H45 . . 120.1 ? C47 C46 C45 . . 118.4(4) ? C47 C46 H46 . . 120.8 ? C45 C46 H46 . . 120.8 ? C46 C47 C48 . . 118.9(4) ? C46 C47 H47 . . 120.5 ? C48 C47 H47 . . 120.5 ? C43 C48 C47 . . 122.5(4) ? C43 C48 H48 . . 118.7 ? C47 C48 H48 . . 118.7 ? C43 C49 H49A . . 109.5 ? C43 C49 H49B . . 109.5 ? H49A C49 H49B . . 109.5 ? C43 C49 H49C . . 109.5 ? H49A C49 H49C . . 109.5 ? H49B C49 H49C . . 109.5 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C8 C1 C2 C3 . . . . -54.5(2) ? Fe1 C1 C2 C3 . . . . 53.18(13) ? C8 C1 C2 Fe1 . . . . -107.70(16) ? C1 C2 C3 C4 . . . . 0.9(2) ? Fe1 C2 C3 C4 . . . . 56.90(13) ? C1 C2 C3 Fe1 . . . . -56.03(13) ? C2 C3 C4 C5 . . . . 58.5(2) ? Fe1 C3 C4 C5 . . . . 112.12(16) ? C2 C3 C4 Fe1 . . . . -53.61(12) ? C3 C4 C5 C6 . . . . -37.7(3) ? Fe1 C4 C5 C6 . . . . 44.5(2) ? C4 C5 C6 C7 . . . . -13.0(3) ? C5 C6 C7 C8 . . . . 3.7(3) ? C6 C7 C8 C1 . . . . 13.2(3) ? C2 C1 C8 C7 . . . . 28.5(3) ? Fe1 C1 C8 C7 . . . . -52.5(2) ? C19 P1 C9 C10 . . . . 178.81(9) ? C13 P1 C9 C10 . . . . 77.19(10) ? Fe1 P1 C9 C10 . . . . -45.37(10) ? P1 C9 C10 P2 . . . . 42.06(11) ? C25 P2 C10 C9 . . . . -160.90(10) ? C11 P2 C10 C9 . . . . 93.41(10) ? Fe1 P2 C10 C9 . . . . -24.20(11) ? C25 P2 C11 C12 . . . . 174.59(9) ? C10 P2 C11 C12 . . . . -79.99(10) ? Fe1 P2 C11 C12 . . . . 38.97(10) ? P2 C11 C12 P3 . . . . -41.84(11) ? C31 P3 C12 C11 . . . . 159.03(9) ? C37 P3 C12 C11 . . . . -98.69(10) ? Fe1 P3 C12 C11 . . . . 29.31(10) ? C19 P1 C13 C18 . . . . 152.30(12) ? C9 P1 C13 C18 . . . . -103.63(12) ? Fe1 P1 C13 C18 . . . . 12.57(13) ? C19 P1 C13 C14 . . . . -34.29(14) ? C9 P1 C13 C14 . . . . 69.79(13) ? Fe1 P1 C13 C14 . . . . -174.01(11) ? C18 C13 C14 C15 . . . . 0.5(2) ? P1 C13 C14 C15 . . . . -173.03(14) ? C13 C14 C15 C16 . . . . 0.2(3) ? C14 C15 C16 C17 . . . . -0.8(3) ? C15 C16 C17 C18 . . . . 0.7(3) ? C14 C13 C18 C17 . . . . -0.6(2) ? P1 C13 C18 C17 . . . . 173.06(12) ? C16 C17 C18 C13 . . . . 0.0(2) ? C9 P1 C19 C20 . . . . 21.99(13) ? C13 P1 C19 C20 . . . . 122.46(12) ? Fe1 P1 C19 C20 . . . . -103.05(11) ? C9 P1 C19 C24 . . . . -159.25(11) ? C13 P1 C19 C24 . . . . -58.78(12) ? Fe1 P1 C19 C24 . . . . 75.71(12) ? C24 C19 C20 C21 . . . . 0.7(2) ? P1 C19 C20 C21 . . . . 179.43(11) ? C19 C20 C21 C22 . . . . -0.1(2) ? C20 C21 C22 C23 . . . . -0.3(2) ? C21 C22 C23 C24 . . . . 0.1(2) ? C22 C23 C24 C19 . . . . 0.5(2) ? C20 C19 C24 C23 . . . . -0.9(2) ? P1 C19 C24 C23 . . . . -179.66(11) ? C11 P2 C25 C30 . . . . -19.98(14) ? C10 P2 C25 C30 . . . . -125.50(13) ? Fe1 P2 C25 C30 . . . . 106.04(13) ? C11 P2 C25 C26 . . . . 161.70(12) ? C10 P2 C25 C26 . . . . 56.18(14) ? Fe1 P2 C25 C26 . . . . -72.28(14) ? C30 C25 C26 C27 . . . . -1.0(2) ? P2 C25 C26 C27 . . . . 177.43(13) ? C25 C26 C27 C28 . . . . -0.3(3) ? C26 C27 C28 C29 . . . . 1.5(3) ? C27 C28 C29 C30 . . . . -1.6(3) ? C26 C25 C30 C29 . . . . 0.9(2) ? P2 C25 C30 C29 . . . . -177.41(13) ? C28 C29 C30 C25 . . . . 0.3(3) ? C37 P3 C31 C36 . . . . -92.37(12) ? C12 P3 C31 C36 . . . . 10.93(13) ? Fe1 P3 C31 C36 . . . . 133.62(11) ? C37 P3 C31 C32 . . . . 86.05(11) ? C12 P3 C31 C32 . . . . -170.65(11) ? Fe1 P3 C31 C32 . . . . -47.96(12) ? C36 C31 C32 C33 . . . . 2.4(2) ? P3 C31 C32 C33 . . . . -176.10(11) ? C31 C32 C33 C34 . . . . -1.7(2) ? C32 C33 C34 C35 . . . . -0.2(2) ? C33 C34 C35 C36 . . . . 1.4(3) ? C34 C35 C36 C31 . . . . -0.7(2) ? C32 C31 C36 C35 . . . . -1.2(2) ? P3 C31 C36 C35 . . . . 177.23(12) ? C31 P3 C37 C38 . . . . -39.06(13) ? C12 P3 C37 C38 . . . . -143.98(12) ? Fe1 P3 C37 C38 . . . . 95.19(12) ? C31 P3 C37 C42 . . . . 142.33(12) ? C12 P3 C37 C42 . . . . 37.41(13) ? Fe1 P3 C37 C42 . . . . -83.42(12) ? C42 C37 C38 C39 . . . . 0.4(2) ? P3 C37 C38 C39 . . . . -178.25(12) ? C37 C38 C39 C40 . . . . -0.3(2) ? C38 C39 C40 C41 . . . . -0.4(3) ? C39 C40 C41 C42 . . . . 0.9(3) ? C40 C41 C42 C37 . . . . -0.8(2) ? C38 C37 C42 C41 . . . . 0.2(2) ? P3 C37 C42 C41 . . . . 178.83(12) ? C48 C43 C44 C45 . . . . -2.1(4) ? C49 C43 C44 C45 . . . . 179.6(2) ? C43 C44 C45 C46 . . . . 0.6(4) ? C44 C45 C46 C47 . . . . -0.1(4) ? C45 C46 C47 C48 . . . . 1.0(5) ? C44 C43 C48 C47 . . . . 3.0(5) ? C49 C43 C48 C47 . . . . -178.7(3) ? C46 C47 C48 C43 . . . . -2.5(6) ? _iucr_refine_instructions_details ; TITL apx1334_0m in P2(1)/n CELL 0.71073 12.8369 21.4700 15.3475 90.000 107.542 90.000 ZERR 4.00 0.0013 0.0022 0.0015 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H P Fe UNIT 196 196 12 4 L.S. 4 SHEL 50 0.76 ACTA BOND $H FMAP 2 PLAN 10 CONF SIZE 0.4 0.25 0.1 TEMP -133.000 WGHT 0.037400 2.303700 FVAR 0.32743 FE1 4 0.395429 0.236918 -0.051598 11.00000 0.01396 0.01357 = 0.01183 0.00034 0.00088 -0.00139 P1 3 0.573768 0.228534 -0.005562 11.00000 0.01421 0.01689 = 0.01360 0.00035 0.00242 -0.00174 P2 3 0.423350 0.325261 0.021243 11.00000 0.01786 0.01309 = 0.01501 0.00028 0.00217 -0.00211 P3 3 0.362230 0.198004 0.069344 11.00000 0.01299 0.01372 = 0.01387 0.00028 0.00203 -0.00142 C1 1 0.234767 0.271702 -0.133601 11.00000 0.02026 0.01771 = 0.02159 0.00095 -0.00334 0.00161 H1 2 0.222883 0.314664 -0.120476 11.00000 -1.20000 C2 1 0.316275 0.267433 -0.179681 11.00000 0.02243 0.02154 = 0.01462 0.00393 -0.00341 -0.00500 H2 2 0.337330 0.305298 -0.201472 11.00000 -1.20000 C3 1 0.377314 0.213965 -0.183864 11.00000 0.02092 0.02672 = 0.01218 -0.00173 0.00209 -0.00557 H3 2 0.435910 0.218921 -0.207203 11.00000 -1.20000 C4 1 0.366766 0.154998 -0.143744 11.00000 0.01937 0.02082 = 0.01758 -0.00294 0.00213 0.00007 H4 2 0.432880 0.130108 -0.134427 11.00000 -1.20000 C5 1 0.273953 0.113810 -0.157287 11.00000 0.02574 0.01735 = 0.01734 -0.00159 0.00150 -0.00214 AFIX 43 H5 2 0.293585 0.071086 -0.156116 11.00000 -1.20000 AFIX 0 C6 1 0.165223 0.122197 -0.171289 11.00000 0.02358 0.02061 = 0.01817 -0.00040 -0.00143 -0.00599 AFIX 43 H6 2 0.121945 0.086000 -0.190926 11.00000 -1.20000 AFIX 0 C7 1 0.105245 0.176211 -0.161444 11.00000 0.01609 0.02712 = 0.01876 0.00373 -0.00255 -0.00204 AFIX 43 H7 2 0.029358 0.169246 -0.171990 11.00000 -1.20000 AFIX 0 C8 1 0.137604 0.235787 -0.139657 11.00000 0.01771 0.02455 = 0.01881 0.00281 -0.00153 0.00346 AFIX 43 H8 2 0.083176 0.259783 -0.124733 11.00000 -1.20000 AFIX 0 C9 1 0.628959 0.276097 0.098632 11.00000 0.01607 0.02297 = 0.01469 -0.00247 0.00092 -0.00400 AFIX 23 H9A 2 0.615472 0.255363 0.151835 11.00000 -1.20000 H9B 2 0.708672 0.282023 0.111606 11.00000 -1.20000 AFIX 0 C10 1 0.570123 0.338662 0.080292 11.00000 0.01988 0.01913 = 0.01814 -0.00291 0.00349 -0.00616 AFIX 23 H10A 2 0.602055 0.364865 0.041773 11.00000 -1.20000 H10B 2 0.578944 0.360745 0.138704 11.00000 -1.20000 AFIX 0 C11 1 0.365307 0.322751 0.117151 11.00000 0.02145 0.01673 = 0.02054 -0.00228 0.00693 -0.00123 AFIX 23 H11A 2 0.399848 0.354974 0.162875 11.00000 -1.20000 H11B 2 0.285738 0.330880 0.094927 11.00000 -1.20000 AFIX 0 C12 1 0.387015 0.257940 0.160407 11.00000 0.01895 0.01742 = 0.01573 -0.00215 0.00522 -0.00251 AFIX 23 H12A 2 0.338235 0.250511 0.198503 11.00000 -1.20000 H12B 2 0.463545 0.255258 0.200238 11.00000 -1.20000 AFIX 0 C13 1 0.649783 0.265850 -0.076970 11.00000 0.02022 0.01929 = 0.01908 -0.00183 0.00770 -0.00358 C14 1 0.762492 0.258217 -0.057939 11.00000 0.02301 0.03020 = 0.03369 0.00539 0.01139 -0.00035 AFIX 43 H14 2 0.800388 0.229830 -0.011763 11.00000 -1.20000 AFIX 0 C15 1 0.819613 0.291876 -0.106108 11.00000 0.02737 0.04080 = 0.04887 0.00720 0.02174 -0.00038 AFIX 43 H15 2 0.896236 0.286234 -0.092707 11.00000 -1.20000 AFIX 0 C16 1 0.765916 0.333372 -0.173159 11.00000 0.03976 0.03385 = 0.04028 0.00323 0.02707 -0.00532 AFIX 43 H16 2 0.805575 0.356594 -0.205302 11.00000 -1.20000 AFIX 0 C17 1 0.654215 0.341113 -0.193518 11.00000 0.03855 0.02520 = 0.02442 0.00300 0.01334 -0.00356 AFIX 43 H17 2 0.616731 0.369320 -0.240128 11.00000 -1.20000 AFIX 0 C18 1 0.596868 0.307364 -0.145376 11.00000 0.02456 0.02207 = 0.01982 -0.00054 0.00729 -0.00330 AFIX 43 H18 2 0.520120 0.312854 -0.159613 11.00000 -1.20000 AFIX 0 C19 1 0.652334 0.156186 0.024103 11.00000 0.01321 0.01881 = 0.02141 0.00201 0.00279 -0.00192 C20 1 0.702959 0.138257 0.114275 11.00000 0.01788 0.02508 = 0.02181 0.00239 0.00290 -0.00195 AFIX 43 H20 2 0.697760 0.164245 0.162890 11.00000 -1.20000 AFIX 0 C21 1 0.760949 0.082728 0.133696 11.00000 0.01968 0.02856 = 0.02987 0.01051 0.00103 -0.00070 AFIX 43 H21 2 0.795178 0.071099 0.195445 11.00000 -1.20000 AFIX 0 C22 1 0.769204 0.044273 0.063822 11.00000 0.01891 0.01983 = 0.04299 0.00590 0.00623 -0.00101 AFIX 43 H22 2 0.809188 0.006432 0.077411 11.00000 -1.20000 AFIX 0 C23 1 0.718712 0.061297 -0.026306 11.00000 0.02202 0.01983 = 0.03673 -0.00306 0.00856 -0.00189 AFIX 43 H23 2 0.724011 0.035046 -0.074620 11.00000 -1.20000 AFIX 0 C24 1 0.660482 0.116661 -0.045867 11.00000 0.02012 0.02257 = 0.02344 -0.00053 0.00393 -0.00184 AFIX 43 H24 2 0.625672 0.127837 -0.107712 11.00000 -1.20000 AFIX 0 C25 1 0.378907 0.401866 -0.029225 11.00000 0.02686 0.01469 = 0.01939 -0.00096 -0.00226 -0.00354 C26 1 0.431709 0.429035 -0.087257 11.00000 0.05245 0.01942 = 0.02643 0.00192 0.01248 -0.00072 AFIX 43 H26 2 0.492085 0.408364 -0.098051 11.00000 -1.20000 AFIX 0 C27 1 0.396890 0.486030 -0.129436 11.00000 0.06393 0.02063 = 0.02663 0.00434 0.00536 -0.00826 AFIX 43 H27 2 0.433777 0.503969 -0.168471 11.00000 -1.20000 AFIX 0 C28 1 0.309385 0.516403 -0.114795 11.00000 0.04231 0.01559 = 0.03966 0.00575 -0.01775 -0.00962 AFIX 43 H28 2 0.284599 0.554755 -0.144758 11.00000 -1.20000 AFIX 0 C29 1 0.258136 0.491034 -0.056734 11.00000 0.02742 0.01999 = 0.06791 0.00689 -0.00297 0.00214 AFIX 43 H29 2 0.198831 0.512497 -0.045359 11.00000 -1.20000 AFIX 0 C30 1 0.292231 0.433936 -0.014117 11.00000 0.02522 0.02012 = 0.04878 0.00702 0.00402 -0.00025 AFIX 43 H30 2 0.255588 0.416864 0.025708 11.00000 -1.20000 AFIX 0 C31 1 0.440067 0.131016 0.129768 11.00000 0.01310 0.01570 = 0.01807 0.00245 0.00314 -0.00136 C32 1 0.453488 0.079456 0.078927 11.00000 0.01775 0.01872 = 0.01784 0.00032 0.00193 -0.00108 AFIX 43 H32 2 0.426353 0.080811 0.014124 11.00000 -1.20000 AFIX 0 C33 1 0.505984 0.026161 0.121757 11.00000 0.02146 0.01752 = 0.02690 -0.00019 0.00547 0.00046 AFIX 43 H33 2 0.512738 -0.009014 0.086298 11.00000 -1.20000 AFIX 0 C34 1 0.548477 0.024182 0.215974 11.00000 0.02769 0.02185 = 0.02810 0.00784 0.00335 0.00694 AFIX 43 H34 2 0.584224 -0.012293 0.245359 11.00000 -1.20000 AFIX 0 C35 1 0.538542 0.075770 0.267196 11.00000 0.03466 0.03049 = 0.01803 0.00521 0.00156 0.00700 AFIX 43 H35 2 0.568995 0.074934 0.331797 11.00000 -1.20000 AFIX 0 C36 1 0.484285 0.128675 0.224538 11.00000 0.02381 0.02139 = 0.01822 0.00065 0.00435 0.00224 AFIX 43 H36 2 0.477242 0.163618 0.260318 11.00000 -1.20000 AFIX 0 C37 1 0.222820 0.172428 0.063596 11.00000 0.01490 0.02187 = 0.01526 0.00238 0.00219 -0.00333 C38 1 0.189866 0.110650 0.046886 11.00000 0.02100 0.02214 = 0.02743 0.00041 0.00433 -0.00399 AFIX 43 H38 2 0.240452 0.080238 0.039794 11.00000 -1.20000 AFIX 0 C39 1 0.083232 0.093027 0.040468 11.00000 0.02571 0.02892 = 0.03845 0.00229 0.00427 -0.01191 AFIX 43 H39 2 0.061810 0.050737 0.028766 11.00000 -1.20000 AFIX 0 C40 1 0.008749 0.136227 0.050903 11.00000 0.01689 0.04642 = 0.03592 0.00519 0.00553 -0.00930 AFIX 43 H40 2 -0.063909 0.124033 0.046105 11.00000 -1.20000 AFIX 0 C41 1 0.040889 0.197663 0.068472 11.00000 0.01756 0.03903 = 0.03483 0.00150 0.00663 0.00172 AFIX 43 H41 2 -0.009647 0.227722 0.076682 11.00000 -1.20000 AFIX 0 C42 1 0.146434 0.215507 0.074134 11.00000 0.01821 0.02464 = 0.02926 0.00160 0.00529 -0.00121 AFIX 43 H42 2 0.167087 0.257938 0.085420 11.00000 -1.20000 AFIX 0 C43 1 0.725632 0.060054 0.716093 11.00000 0.13445 0.04603 = 0.11873 0.01816 0.10092 0.00707 C44 1 0.710731 0.119360 0.745073 11.00000 0.11534 0.05788 = 0.07533 0.02204 0.07226 0.01711 AFIX 43 H44 2 0.767141 0.137980 0.792897 11.00000 -1.20000 AFIX 0 C45 1 0.616022 0.152004 0.706187 11.00000 0.12095 0.06190 = 0.08872 0.02628 0.07916 0.02220 AFIX 43 H45 2 0.607658 0.192921 0.726676 11.00000 -1.20000 AFIX 0 C46 1 0.533083 0.125186 0.637282 11.00000 0.08995 0.11224 = 0.10155 0.01568 0.05983 -0.00554 AFIX 43 H46 2 0.467056 0.147119 0.609809 11.00000 -1.20000 AFIX 0 C47 1 0.548416 0.065763 0.609290 11.00000 0.12391 0.14978 = 0.13473 -0.03486 0.08298 -0.07947 AFIX 43 H47 2 0.493439 0.046177 0.561395 11.00000 -1.20000 AFIX 0 C48 1 0.647405 0.034418 0.653077 11.00000 0.14272 0.07513 = 0.19143 -0.01254 0.12672 -0.03418 AFIX 43 H48 2 0.656522 -0.007120 0.635323 11.00000 -1.20000 AFIX 0 C49 1 0.828643 0.024108 0.757451 11.00000 0.21494 0.09644 = 0.15847 0.07711 0.14235 0.08882 AFIX 137 H49A 2 0.874512 0.046490 0.810953 11.00000 -1.50000 H49B 2 0.868266 0.019445 0.712338 11.00000 -1.50000 H49C 2 0.810584 -0.017142 0.776136 11.00000 -1.50000 AFIX 0 HKLF 4 REM apx1334_0m in P2(1)/n REM R1 = 0.0295 for 8284 Fo > 4sig(Fo) and 0.0357 for all 9426 data REM 491 parameters refined using 0 restraints END WGHT 0.0374 2.3039 REM Highest difference peak 0.433, deepest hole -0.304, 1-sigma level 0.050 Q1 1 0.8440 0.0630 0.7978 11.00000 0.05 0.43 Q2 1 0.3758 0.2309 0.1207 11.00000 0.05 0.39 Q3 1 0.8008 0.1223 0.8050 11.00000 0.05 0.39 Q4 1 0.7450 0.0081 0.7226 11.00000 0.05 0.38 Q5 1 0.6152 0.2471 -0.0443 11.00000 0.05 0.35 Q6 1 0.4109 0.1621 0.1038 11.00000 0.05 0.34 Q7 1 0.5400 0.0513 0.2397 11.00000 0.05 0.34 Q8 1 0.6217 0.1874 0.0060 11.00000 0.05 0.32 Q9 1 0.8539 0.0263 0.7698 11.00000 0.05 0.30 Q10 1 0.5025 0.3319 0.0575 11.00000 0.05 0.30 ; _shelx_res_checksum 20699 _shelx_hkl_file ; -2 0 0 348.177 8.577 2 2 0 0 355.319 8.636 4 -2 0 0 351.754 8.647 1 -3 0 0 -1.7166 0.5206 2 -3 0 0 -1.2692 0.6440 1 3 0 0 -0.8692 0.5608 4 -4 0 0 2471.02 58.78 1 4 0 0 2569.94 58.84 4 -4 0 0 2517.99 58.58 2 -5 0 0 -0.1972 0.6948 1 -5 0 0 -0.2809 0.6313 2 5 0 0 0.38776 0.59482 4 6 0 0 1274.60 30.39 4 -6 0 0 1249.43 30.28 2 -7 0 0 0.37351 0.90937 2 -7 0 0 0.57574 0.86804 1 7 0 0 0.06198 0.73005 4 8 0 0 239.984 7.270 4 -8 0 0 240.210 7.334 2 -8 0 0 243.316 7.532 1 -9 0 0 -0.4331 0.9282 2 -9 0 0 1.65611 1.16765 1 9 0 0 1.38006 1.04767 4 -10 0 0 0.29322 1.27946 1 10 0 0 1.07639 1.16932 4 -10 0 0 0.08995 1.24079 2 -11 0 0 -0.1266 1.2754 2 -11 0 0 -0.0969 1.3957 1 11 0 0 1.41000 1.30642 4 -12 0 0 1.52507 1.62061 2 -12 0 0 1.30779 1.72157 1 12 0 0 2.28396 1.54657 4 12 0 0 3.00260 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706.577 17.485 3 -3 8 0 704.053 17.047 2 3 8 0 711.499 17.298 3 -4 -8 0 75.1324 3.0668 1 -4 -8 0 75.2907 2.3913 2 4 -8 0 75.3997 3.1590 1 4 -8 0 74.9428 2.5616 4 -4 8 0 75.6527 2.8497 3 -4 8 0 72.6888 2.8625 2 4 8 0 69.9248 3.1802 4 4 8 0 76.9677 2.7144 3 5 -8 0 537.973 13.998 1 -5 -8 0 529.396 13.078 2 -5 -8 0 540.245 13.950 1 5 -8 0 546.916 13.229 4 5 8 0 533.199 13.305 3 -5 8 0 539.467 13.672 2 5 8 0 511.469 14.005 4 -5 8 0 521.627 13.601 3 -6 -8 0 37.9611 2.4975 1 -6 -8 0 39.9454 1.9677 2 6 -8 0 38.1837 2.4677 1 6 -8 0 40.4116 1.9970 4 6 8 0 39.5866 2.6129 4 6 8 0 43.7491 1.8428 3 -6 8 0 39.7338 2.3171 2 -6 8 0 38.8160 2.1432 3 -7 -8 0 117.065 3.976 2 7 -8 0 111.404 4.672 1 7 -8 0 116.159 3.948 4 -7 -8 0 117.672 4.609 1 -7 8 0 121.167 4.541 2 7 8 0 115.122 4.657 4 -7 8 0 119.355 3.981 3 8 -8 0 22.5218 2.4551 1 -8 -8 0 25.0525 1.9507 2 -8 -8 0 24.2740 2.3862 1 8 -8 0 25.0487 1.9387 4 8 8 0 22.3043 2.3656 4 -8 8 0 21.8504 2.2775 2 9 -8 0 43.8781 3.1319 1 -9 -8 0 46.1605 3.2815 1 -9 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783.657 20.102 4 -8 -9 0 413.393 11.062 2 -8 -9 0 404.022 11.902 1 8 -9 0 408.093 12.007 1 -8 9 0 415.373 11.109 3 -8 9 0 424.576 11.810 2 8 9 0 417.337 12.103 4 9 -9 0 51.0640 3.4445 1 -9 -9 0 49.1781 2.7815 2 -9 -9 0 44.2570 3.1609 1 9 9 0 42.6867 3.2871 4 -9 9 0 46.7828 3.2001 2 10 -9 0 23.7718 2.8665 1 -10 -9 0 24.5887 2.7448 1 10 9 0 27.8378 2.9319 4 -10 9 0 27.1311 2.7364 2 11 -9 0 76.1793 4.6099 1 -11 -9 0 76.0771 4.4655 1 -11 9 0 78.5351 4.2772 2 11 9 0 74.0990 4.3665 4 -12 -9 0 369.287 12.049 1 12 -9 0 369.857 12.194 1 -12 9 0 380.847 12.023 2 12 9 0 376.596 12.133 4 13 -9 0 134.695 6.392 1 -13 -9 0 106.350 5.784 1 13 9 0 124.992 6.077 4 -13 9 0 129.663 6.084 2 14 -9 0 31.4553 3.8156 1 -14 -9 0 26.5351 3.4625 1 -14 9 0 37.6883 3.9228 2 14 9 0 32.4706 3.6833 4 15 -9 0 1.93078 2.38868 1 15 9 0 3.00136 2.37663 4 0 -10 0 454.541 11.617 4 0 -10 0 449.389 11.831 1 0 10 0 459.517 11.999 3 0 10 0 467.390 10.905 2 -1 -10 0 224.150 6.736 1 -1 -10 0 251.879 6.746 4 1 -10 0 234.100 6.435 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178.625 5.664 3 -6 10 0 176.103 5.812 2 6 10 0 172.080 6.163 4 6 10 0 185.736 5.391 3 7 -10 0 57.9496 3.4822 1 -7 -10 0 59.7988 3.3428 1 7 10 0 68.0334 3.6813 4 -7 10 0 68.3740 3.0132 3 -7 10 0 66.2139 3.2333 2 8 -10 0 4.57621 1.55549 1 -8 -10 0 4.43305 1.55940 1 -8 10 0 4.09370 1.50205 2 8 10 0 1.87596 1.52975 4 -8 10 0 3.63153 1.15349 3 -9 -10 0 1.53797 1.38738 1 9 -10 0 2.69683 1.52170 1 -9 10 0 -1.5623 1.2337 2 9 10 0 1.72947 1.45551 4 -10 -10 0 98.1356 4.8607 1 10 -10 0 103.241 4.993 1 -10 10 0 97.4651 4.7237 2 10 10 0 91.8304 4.8888 4 -11 -10 0 46.4986 3.6751 1 11 -10 0 41.2883 3.8018 1 11 10 0 50.4147 3.8216 4 -11 10 0 40.6378 3.6101 2 12 -10 0 15.4008 2.8177 1 -12 -10 0 14.6203 2.6592 1 -12 10 0 11.7499 2.4679 2 12 10 0 14.4596 2.6213 4 13 -10 0 2.49484 2.12132 1 -13 -10 0 3.38189 2.19024 1 -13 10 0 2.28579 1.84044 2 13 10 0 0.88493 1.84713 4 -14 -10 0 -0.4735 1.8856 1 14 -10 0 5.03021 2.37622 1 -14 10 0 4.87871 2.27695 2 14 10 0 -1.0723 1.9517 4 0 -11 0 1.18098 0.71625 4 0 -11 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45.6202 2.6041 2 -6 11 0 42.0932 2.3972 3 6 11 0 41.8848 2.8235 4 7 -11 0 1084.57 27.84 1 -7 -11 0 1063.19 27.77 1 -7 11 0 1152.98 27.48 2 7 11 0 1106.07 28.08 4 -7 11 0 1110.66 27.44 3 8 -11 0 130.042 5.452 1 -8 -11 0 122.029 5.236 1 -8 11 0 131.338 5.148 2 8 11 0 137.459 5.597 4 -8 11 0 125.482 4.723 3 9 -11 0 119.614 5.425 1 -9 -11 0 121.707 5.332 1 -9 11 0 118.258 5.050 2 9 11 0 126.636 5.487 4 -10 -11 0 34.2714 3.2324 1 10 -11 0 35.0889 3.2800 1 10 11 0 31.9892 3.3117 4 -10 11 0 36.8977 3.2435 2 11 -11 0 194.238 7.710 1 -11 -11 0 200.378 7.663 1 11 11 0 196.522 7.788 4 -11 11 0 196.675 7.460 2 -12 -11 0 178.846 7.502 1 12 -11 0 180.573 7.650 1 12 11 0 199.982 7.976 4 -12 11 0 191.682 7.525 2 13 -11 0 18.7815 3.1819 1 -13 -11 0 21.0046 3.1650 1 13 11 0 20.3820 3.0650 4 -13 11 0 24.8261 3.1256 2 -14 -11 0 -0.3611 1.9591 1 14 -11 0 -3.4397 1.9612 1 -14 11 0 3.13159 2.25437 2 14 11 0 3.20319 2.16179 4 0 -12 0 515.374 13.412 4 0 -12 0 532.611 13.730 1 0 12 0 521.522 12.523 2 0 12 0 542.420 13.938 3 -1 -12 0 34.0490 2.0983 1 -1 -12 0 33.1270 2.0353 4 1 -12 0 30.2729 1.8457 4 1 -12 0 28.6871 2.1145 1 -1 12 0 30.2298 2.0272 3 1 12 0 31.4042 2.0139 3 -1 12 0 31.1090 1.4419 2 -2 -12 0 14.2276 1.4906 4 -2 -12 0 12.2503 1.4738 1 2 -12 0 12.3257 1.5136 1 2 -12 0 13.7153 1.2838 4 2 12 0 13.5692 1.4488 3 -2 12 0 13.5581 1.5447 3 -2 12 0 12.3767 1.0865 2 3 -12 0 537.119 14.491 1 3 -12 0 555.555 13.765 4 -3 -12 0 573.396 14.476 4 -3 -12 0 532.287 14.421 1 3 12 0 535.769 14.577 4 -3 12 0 557.714 13.758 2 3 12 0 563.728 14.354 3 -3 12 0 549.392 14.540 3 -4 -12 0 79.7628 3.6370 1 4 -12 0 89.0485 3.8298 1 4 -12 0 81.2898 2.9967 4 4 12 0 90.5754 3.4417 3 -4 12 0 83.9320 3.5903 3 -4 12 0 88.4011 3.2570 2 4 12 0 84.8987 3.8567 4 5 -12 0 207.627 6.953 1 -5 -12 0 210.322 6.844 1 5 -12 0 203.812 5.944 4 5 12 0 215.337 7.075 4 -5 12 0 213.169 6.399 2 5 12 0 213.880 6.368 3 -5 12 0 211.387 6.670 3 6 -12 0 908.293 22.868 1 -6 -12 0 863.369 22.696 1 6 12 0 892.270 22.050 3 6 12 0 888.392 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4.2895 1 10 -2 6 67.6350 4.4186 1 10 2 6 66.8712 4.5398 1 -10 2 -6 70.3901 4.1053 2 -11 -2 -6 161.208 6.675 2 11 -2 6 162.195 7.271 1 11 2 6 174.828 7.420 1 -11 2 -6 159.658 6.743 2 12 -2 6 13.7763 2.8796 1 -12 -2 -6 18.2737 2.7451 2 12 2 6 18.6348 3.0470 1 -12 2 -6 19.4339 2.8901 2 13 -2 6 35.5517 4.1938 1 -13 -2 -6 32.6322 3.6337 2 13 2 6 47.7069 4.6773 1 -13 2 -6 37.7015 3.9011 2 -14 -2 -6 6.15425 2.41242 2 -16 -3 6 4.17700 2.37300 2 16 -3 -6 4.60932 2.33042 4 -16 3 6 7.06616 2.35518 2 16 3 -6 7.11470 2.59351 4 -15 -3 6 0.05446 1.85375 1 15 -3 -6 0.04447 1.97202 4 -15 -3 6 0.18563 1.70575 2 15 3 -6 1.42691 2.06353 4 -15 3 6 0.90915 1.70241 2 -14 -3 6 73.5215 4.4982 2 -14 -3 6 66.6194 4.2224 1 14 -3 -6 73.4900 4.5729 4 14 3 -6 68.6205 4.4886 4 -14 3 6 65.2804 4.4767 2 13 -3 -6 23.5765 2.9979 4 -13 -3 6 28.8548 3.0827 2 -13 -3 6 22.9435 2.6430 1 13 3 -6 24.2158 2.9840 4 -13 3 6 26.3533 2.9665 2 12 -3 -6 7.36043 1.86444 1 -12 -3 6 8.12395 1.97275 2 -12 -3 6 9.88218 1.97951 1 12 -3 -6 8.46315 2.13835 4 12 3 -6 5.99106 1.87522 4 -12 3 6 6.31228 1.87680 2 11 -3 -6 264.168 8.494 1 -11 -3 6 264.240 8.742 2 11 -3 -6 261.596 8.777 4 -11 -3 6 270.902 8.419 1 -11 3 6 285.661 8.979 2 11 3 -6 272.047 9.027 4 10 -3 -6 363.628 10.104 1 -10 -3 6 354.878 9.921 1 10 -3 -6 331.719 10.309 4 -10 -3 6 329.510 10.169 2 -10 3 6 334.075 10.267 2 10 3 -6 344.872 10.557 4 9 -3 -6 59.7054 3.0765 1 9 -3 -6 61.0041 3.3046 4 -9 -3 6 57.8796 2.9614 1 -9 -3 6 64.1122 3.3017 2 -9 3 6 59.8799 3.2612 2 9 3 -6 60.6774 3.5112 4 -8 -3 6 120.863 4.221 1 8 -3 -6 122.190 4.235 1 8 -3 -6 118.746 4.665 4 -8 -3 6 119.123 4.609 2 8 3 -6 114.546 4.711 4 -8 3 6 124.225 3.985 3 -8 3 6 123.620 4.640 2 7 -3 -6 239.538 7.315 4 -7 -3 6 234.928 7.146 2 7 -3 -6 233.442 6.623 1 -7 -3 6 238.334 6.691 1 7 3 -6 245.140 7.402 4 -7 3 6 230.072 6.681 3 7 3 -6 237.336 6.376 3 -7 3 6 230.854 7.174 2 6 -3 -6 276.139 8.031 4 6 -3 -6 295.287 7.337 1 -6 -3 6 269.827 7.940 2 -6 -3 6 263.350 7.348 1 -6 3 6 267.901 7.896 2 6 3 -6 278.388 8.077 4 -6 3 6 277.589 7.689 3 6 3 -6 275.139 7.356 3 -5 -3 6 141.620 4.635 2 -5 -3 6 141.826 4.083 1 5 -3 -6 131.681 4.639 4 5 -3 -6 144.872 3.925 1 5 -3 -6 143.435 4.355 3 5 3 -6 139.235 4.670 4 5 3 -6 134.556 4.216 3 -5 3 6 141.326 4.609 2 4 -3 -6 67.5714 2.6401 3 4 -3 -6 67.6831 1.9206 1 -4 -3 6 59.9691 2.1648 1 -4 -3 6 60.9897 2.6980 2 4 3 -6 64.6113 2.6972 4 4 3 -6 64.5351 2.5351 3 -4 3 6 67.1979 2.8060 2 3 -3 -6 560.432 14.301 3 -3 -3 6 582.745 14.288 2 -3 -3 6 544.137 13.552 1 3 -3 -6 560.417 14.280 4 3 3 -6 582.606 14.279 3 3 3 -6 552.530 14.104 4 -3 3 6 572.417 14.160 2 2 -3 -6 242.357 6.965 3 -2 -3 6 255.381 7.006 2 -2 -3 6 260.252 6.368 1 2 -3 -6 237.998 6.893 4 -2 3 6 249.065 6.802 2 2 3 -6 257.939 6.986 3 2 3 -6 245.940 6.666 4 1 -3 -6 205.694 5.973 3 1 -3 -6 205.550 5.107 1 -1 -3 6 207.933 5.471 1 -1 -3 6 198.683 6.006 2 1 -3 -6 202.036 5.823 4 1 3 -6 203.326 5.450 4 -1 3 6 207.512 5.773 2 1 3 -6 208.998 5.979 3 0 -3 6 153.627 4.901 2 0 -3 6 155.908 4.461 1 0 -3 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9.98569 1.54342 1 -5 -3 -6 9.13909 1.49497 1 -5 3 -6 8.86144 1.43048 2 -5 3 -6 6.77499 1.20822 3 5 3 6 7.63554 1.39598 4 -6 -3 -6 193.144 5.856 3 -6 -3 -6 180.752 6.348 1 6 -3 6 190.763 6.652 1 -6 -3 -6 190.405 6.194 2 -6 3 -6 189.643 6.413 2 -6 3 -6 192.803 6.008 3 6 3 6 190.059 6.225 4 -7 -3 -6 19.2821 2.3204 1 7 -3 6 18.8495 2.3816 1 -7 -3 -6 21.7329 2.1987 2 -7 3 -6 20.7695 2.3029 2 7 3 6 16.5113 1.9640 4 8 -3 6 296.920 9.570 1 -8 -3 -6 286.655 8.812 2 -8 -3 -6 287.263 9.258 1 -8 3 -6 273.711 9.067 2 8 3 6 276.945 8.713 4 9 -3 6 12.3136 2.3563 1 -9 -3 -6 14.6673 2.4095 1 -9 -3 -6 12.5081 2.1100 2 9 3 6 13.1077 2.0040 4 -9 3 -6 14.1759 2.2121 2 -10 -3 -6 242.218 8.832 1 -10 -3 -6 252.261 8.522 2 10 -3 6 242.502 9.204 1 -10 3 -6 253.958 8.811 2 11 -3 6 4.59817 2.11081 1 -11 -3 -6 2.54194 1.84177 2 -11 -3 -6 -0.3684 1.8924 1 -11 3 -6 3.83220 2.01000 2 11 3 6 2.96516 1.95942 1 12 -3 6 9.63879 2.81349 1 -12 -3 -6 7.26953 2.06812 2 12 3 6 14.3617 2.8235 1 -12 3 -6 9.65923 2.37895 2 -13 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24.7087 2.0309 3 -6 4 -6 26.2655 2.4239 2 6 4 6 25.5681 2.3048 4 -7 -4 -6 304.983 8.824 2 7 -4 6 274.352 9.273 1 -7 -4 -6 296.840 9.229 1 7 4 6 302.946 8.969 4 -7 4 -6 287.782 8.496 3 -8 -4 -6 18.9753 2.1818 2 8 -4 6 18.3649 2.5579 1 -8 -4 -6 16.6843 2.3207 1 8 4 6 23.5022 2.4521 4 -8 4 -6 21.7158 2.4518 2 -9 -4 -6 10.9334 2.0114 2 9 -4 6 15.3620 2.4817 1 -9 -4 -6 12.2215 2.2095 1 9 4 6 15.9993 2.2118 4 -9 4 -6 10.7493 2.2060 2 10 -4 6 6.01879 2.29023 1 -10 -4 -6 4.15989 1.88924 1 -10 -4 -6 2.20435 1.75938 2 -10 4 -6 3.75242 1.75869 2 -11 -4 -6 297.356 10.436 1 11 -4 6 318.526 10.913 1 -11 -4 -6 295.188 9.892 2 -11 4 -6 290.435 10.160 2 -12 -4 -6 26.6024 3.1466 2 12 -4 6 28.4050 3.6646 1 -12 -4 -6 34.4222 3.6896 1 12 4 6 25.8365 3.5579 1 -12 4 -6 30.2447 3.5377 2 13 -4 6 2.68465 2.43702 1 -13 4 -6 7.14852 2.47226 2 13 4 6 7.95693 2.65197 1 16 -5 -6 0.52870 2.05145 4 -16 -5 6 -0.2123 1.7193 2 -16 5 6 -1.3237 2.0680 2 16 5 -6 1.13069 2.13193 4 -15 -5 6 5.38887 2.03061 1 15 -5 -6 1.76916 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326.277 9.327 2 6 3 -9 310.736 9.272 4 5 -3 -9 148.907 5.016 3 5 -3 -9 141.783 5.107 4 -5 -3 9 143.691 5.180 2 -5 3 9 141.903 5.071 2 5 3 -9 152.706 4.981 3 5 3 -9 144.083 5.004 4 4 -3 -9 451.366 12.159 4 -4 -3 9 431.034 12.101 2 4 -3 -9 438.042 12.092 3 -4 -3 9 450.063 10.930 1 -4 3 9 477.040 12.152 2 4 3 -9 440.508 11.899 4 4 3 -9 451.586 12.081 3 3 -3 -9 2393.20 56.58 3 3 -3 -9 2379.76 56.01 4 -3 -3 9 2394.74 55.94 2 -3 -3 9 2414.40 54.73 1 3 3 -9 2334.66 55.65 4 -3 3 9 2260.39 55.61 2 3 3 -9 2324.64 56.48 3 2 -3 -9 260.506 7.629 4 -2 -3 9 259.643 7.883 2 -2 -3 9 284.353 6.839 1 2 -3 -9 256.520 7.824 3 2 3 -9 239.429 7.668 3 -2 3 9 265.314 7.640 2 2 3 -9 253.428 7.225 4 -1 -3 9 206.545 6.780 2 -1 -3 9 219.121 5.959 1 1 -3 -9 210.153 6.505 4 1 -3 -9 221.372 6.819 3 1 3 -9 222.918 6.111 4 -1 3 9 209.793 6.553 2 0 -3 9 571.655 14.035 1 0 -3 -9 558.600 14.894 3 0 -3 -9 559.957 14.482 4 0 -3 9 572.232 14.939 2 0 3 9 554.606 13.758 1 0 3 9 560.980 14.591 2 0 3 -9 545.405 13.868 4 0 3 -9 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307.792 9.106 3 8 4 -10 294.299 8.524 3 8 4 -10 293.484 9.253 4 -8 4 10 291.608 9.129 2 7 -4 -10 55.2891 3.2654 4 7 -4 -10 58.2746 2.9776 3 -7 -4 10 52.3525 3.1679 2 -7 4 10 57.3811 3.2988 2 7 4 -10 57.4914 3.3343 4 7 4 -10 60.7530 2.9437 3 6 -4 -10 253.831 8.097 4 6 -4 -10 249.997 7.727 3 -6 -4 10 259.217 8.070 2 -6 4 10 259.232 7.929 2 6 4 -10 243.897 7.846 4 6 4 -10 262.403 7.730 3 -5 -4 10 43.4479 2.7825 2 5 -4 -10 48.9687 2.6746 3 5 -4 -10 46.3273 2.8499 4 -5 4 10 44.2725 2.7956 2 5 4 -10 49.4178 2.7479 4 5 4 -10 46.0757 2.6886 3 4 -4 -10 550.880 14.837 4 4 -4 -10 579.913 15.001 3 -4 -4 10 560.990 14.907 2 -4 4 10 553.226 14.651 2 4 4 -10 542.926 14.786 3 4 4 -10 549.166 14.493 4 -3 -4 10 37.0204 2.5120 2 3 -4 -10 34.2857 2.3805 4 3 -4 -10 38.9162 2.4973 3 3 4 -10 34.3712 2.3977 3 -3 4 10 36.4853 2.3016 2 3 4 -10 36.0963 2.1248 4 -2 -4 10 2.94899 1.27788 2 2 -4 -10 0.06531 0.97183 3 2 -4 -10 2.06151 1.02266 4 2 4 -10 1.85837 0.87410 4 -2 4 10 2.00205 1.04508 2 2 4 -10 -0.1180 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57.1746 2.9964 3 -6 5 10 58.1797 3.2119 2 6 5 -10 68.2932 3.3336 4 5 -5 -10 6.44263 1.39471 4 -5 -5 10 5.43716 1.44445 2 5 -5 -10 2.11491 1.10127 3 -5 5 10 5.89469 1.41148 2 5 5 -10 2.89919 1.11220 3 5 5 -10 2.81695 1.16185 4 4 -5 -10 138.244 5.158 3 4 -5 -10 141.091 5.182 4 -4 -5 10 141.565 5.223 2 4 5 -10 140.700 5.117 3 -4 5 10 141.676 5.041 2 4 5 -10 138.182 4.813 4 -3 -5 10 420.819 11.958 2 3 -5 -10 423.231 11.897 4 3 -5 -10 443.946 12.038 3 3 5 -10 421.888 11.898 3 -3 5 10 429.388 11.619 2 3 5 -10 422.965 11.298 4 2 -5 -10 451.555 12.561 3 -2 -5 10 447.751 12.516 2 2 -5 -10 448.195 12.346 4 -2 -5 10 461.868 11.489 1 2 5 -10 437.488 11.612 4 -2 5 10 464.997 12.150 2 2 5 -10 443.367 12.510 3 -1 -5 10 133.009 5.312 2 1 -5 -10 146.242 5.183 4 1 -5 -10 152.635 5.409 3 -1 -5 10 147.268 4.660 1 -1 5 10 147.155 5.050 2 1 5 -10 145.800 5.345 3 0 -5 -10 268.278 8.245 4 0 -5 10 281.314 7.890 1 0 -5 -10 276.223 8.540 3 0 -5 10 287.257 8.723 2 0 5 -10 264.469 8.519 3 0 5 10 282.455 8.176 2 1 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222.274 7.903 4 -10 6 10 202.802 7.479 2 -9 -6 10 56.4720 3.4332 2 9 -6 -10 61.2763 3.6573 4 -9 6 10 58.0890 3.4709 2 9 6 -10 53.8050 3.5129 4 -9 6 10 64.6603 3.4218 3 -8 -6 10 250.753 8.356 2 8 -6 -10 266.239 8.584 4 -8 6 10 261.026 8.312 2 8 6 -10 251.840 8.406 4 8 6 -10 256.238 7.745 3 -8 6 10 268.088 8.340 3 7 -6 -10 76.0276 3.9524 4 -7 -6 10 73.5354 3.8061 2 -7 6 10 73.0668 3.6360 2 7 6 -10 78.0566 3.4463 3 7 6 -10 75.8302 3.8287 4 -7 6 10 71.3900 3.6828 3 6 -6 -10 194.133 6.666 4 -6 -6 10 189.723 6.555 2 6 6 -10 184.898 6.304 4 6 6 -10 189.935 6.216 3 -6 6 10 187.008 6.336 2 -6 6 10 192.936 6.720 3 -5 -6 10 17.8859 2.0919 2 5 -6 -10 18.6013 2.0771 4 5 -6 -10 22.3832 2.1458 3 5 6 -10 15.4776 1.7893 3 -5 6 10 18.5193 2.1691 3 -5 6 10 19.8494 1.9983 2 5 6 -10 18.9809 1.9303 4 -4 -6 10 529.891 14.140 2 4 -6 -10 533.360 14.191 3 4 -6 -10 499.801 14.064 4 4 6 -10 498.772 14.008 3 -4 6 10 544.535 13.854 2 4 6 -10 509.016 13.586 4 -3 -6 10 230.821 6.293 1 -3 -6 10 211.179 7.193 2 3 -6 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448.201 12.454 1 -3 -6 -10 439.473 12.510 4 -3 6 -10 456.982 12.919 3 -3 6 -10 432.808 12.609 2 3 6 10 451.007 12.453 2 4 -6 10 1.35596 1.44082 1 -4 -6 -10 1.80210 1.40394 4 -4 -6 -10 0.75087 1.25143 1 -4 -6 -10 -0.7933 1.2310 3 -4 6 -10 1.65791 1.36792 3 4 6 10 0.32471 1.40996 2 -4 6 -10 -0.6098 1.1442 2 -5 -6 -10 2.65839 1.43870 1 -5 -6 -10 1.82130 1.37262 4 5 -6 10 2.26416 1.54053 1 -5 -6 -10 0.87759 1.28394 2 -5 -6 -10 2.23125 1.25829 3 -5 6 -10 3.18856 1.64391 2 -5 6 -10 1.73455 1.44676 3 6 -6 10 1.81576 1.54996 1 -6 -6 -10 1.04355 1.35994 1 -6 -6 -10 0.52124 1.45163 4 -6 -6 -10 2.05891 1.40095 2 -6 6 -10 -0.3861 1.5542 2 -6 6 -10 0.21641 1.35495 3 7 -6 10 11.0795 2.3662 1 -7 -6 -10 12.5362 2.1784 1 -7 6 -10 10.1402 2.1231 2 8 -6 10 2.67255 1.98115 1 -8 -6 -10 3.25723 1.88266 1 -8 6 -10 1.63710 1.77183 2 -9 -6 -10 7.08013 2.19502 1 9 -6 10 5.51980 2.34672 1 -9 6 -10 8.67640 2.30382 2 10 -6 10 7.45699 2.52023 1 -10 6 -10 3.18968 1.97001 2 10 6 10 5.90698 2.32830 1 11 6 10 0.33445 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237.027 8.304 2 -6 -11 -10 79.6769 4.6260 4 6 -11 10 78.0673 4.6211 1 -6 11 -10 73.4707 4.3258 3 -6 11 -10 69.0271 4.2306 2 7 -11 10 29.8116 3.3079 1 -7 -11 -10 32.8316 3.2953 1 7 11 10 29.6118 3.4714 4 -7 11 -10 22.4957 3.0084 2 8 -11 10 7.09338 2.46445 1 -8 -11 -10 3.68600 2.03537 1 -8 11 -10 1.25436 1.86717 2 8 11 10 4.78204 2.11613 4 9 -11 10 79.3333 5.3354 1 -9 -11 -10 80.8120 5.1314 1 -9 11 -10 79.1350 4.9964 2 9 11 10 94.5008 5.4893 4 -10 -11 -10 33.7439 3.8471 1 14 -12 -10 18.1327 2.9550 4 -14 12 10 17.6595 2.9535 2 14 12 -10 22.3312 3.3992 4 13 -12 -10 14.2581 2.6414 4 13 12 -10 14.5715 2.7814 4 -13 12 10 10.7286 2.6319 2 12 -12 -10 88.3661 5.0878 4 12 12 -10 91.7299 5.1737 4 -12 12 10 76.3279 4.7206 2 11 -12 -10 6.36671 2.08208 4 -11 -12 10 5.34139 1.90979 2 11 12 -10 5.34460 1.98618 4 -11 12 10 8.23291 2.07972 2 10 -12 -10 49.0936 3.5448 4 -10 -12 10 43.5058 3.3051 2 -10 12 10 43.3641 3.3645 2 10 12 -10 38.3670 3.5168 4 9 -12 -10 95.8566 4.9003 4 -9 -12 10 97.1460 4.6894 2 9 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122.286 5.289 2 9 -5 -11 123.228 5.378 4 9 5 -11 125.206 5.365 4 -9 5 11 121.468 5.289 2 -9 5 11 120.559 5.031 3 -8 -5 11 0.32223 1.36904 2 8 -5 -11 -1.6052 1.3580 4 8 5 -11 -0.6727 1.3324 4 -8 5 11 1.08132 1.42906 2 -8 5 11 1.69790 1.41428 3 8 5 -11 0.65822 1.12373 3 7 -5 -11 1024.04 26.03 3 -7 -5 11 1003.04 26.10 2 7 -5 -11 1005.41 26.29 4 -7 5 11 1000.51 25.99 2 7 5 -11 1092.03 25.97 3 -7 5 11 1046.25 26.53 3 7 5 -11 1014.73 26.08 4 -6 -5 11 129.862 5.389 2 6 -5 -11 136.084 5.200 3 6 -5 -11 132.564 5.394 4 -6 5 11 150.202 5.430 2 6 5 -11 135.623 5.231 4 6 5 -11 143.264 5.131 3 -5 -5 11 0.30307 1.15082 2 5 -5 -11 0.18919 1.12029 4 5 -5 -11 0.31605 1.10257 3 5 5 -11 0.48876 1.02921 4 -5 5 11 0.45415 1.10948 2 5 5 -11 -0.3791 0.9781 3 -4 -5 11 34.1948 2.8520 2 4 -5 -11 37.0768 2.6207 4 4 -5 -11 37.7517 2.7034 3 -4 5 11 37.0794 2.6175 2 4 5 -11 34.1559 2.4784 3 4 5 -11 37.2471 2.3423 4 3 -5 -11 401.650 11.544 3 -3 -5 11 396.362 11.536 2 3 -5 -11 410.332 11.458 4 3 5 -11 404.311 11.545 3 3 5 -11 388.050 10.759 4 -3 5 11 403.420 11.138 2 -2 -5 11 35.2929 2.7010 2 2 -5 -11 45.6809 2.8562 3 2 -5 -11 38.2109 2.5832 4 2 5 -11 42.4934 2.8798 3 -2 5 11 45.2726 2.6952 2 -1 -5 11 82.5968 4.0792 2 1 -5 -11 86.1610 4.0762 3 1 -5 -11 88.4183 3.8604 4 -1 5 11 80.4256 3.7154 2 1 5 -11 88.9527 4.0399 3 0 -5 -11 29.0692 2.6110 3 0 -5 -11 32.9919 2.5015 4 0 -5 11 32.1009 2.9757 2 0 5 11 35.4852 2.3920 2 0 5 -11 31.1086 2.7320 3 -1 -5 -11 7.73321 1.62971 3 -1 -5 -11 7.90131 1.63458 4 1 -5 11 8.54738 1.83217 2 1 -5 11 5.61806 1.39508 1 -1 5 -11 8.78946 1.78681 3 1 5 11 8.16340 1.63989 2 -2 -5 -11 61.3278 3.5401 3 2 -5 11 57.8974 3.1491 1 -2 -5 -11 64.1876 3.4342 4 2 -5 11 58.5104 3.6819 2 2 5 11 64.4718 3.5182 2 -2 5 -11 62.6165 3.5418 3 3 -5 11 209.574 7.026 1 -3 -5 -11 221.527 7.202 4 -3 -5 -11 209.140 7.279 3 -3 5 -11 212.092 7.337 2 -3 5 -11 209.325 7.453 3 3 5 11 217.796 7.302 2 -4 -5 -11 4.11004 1.51170 3 -4 -5 -11 5.97661 1.66351 4 4 -5 11 4.74168 1.62788 1 -4 5 -11 4.31488 1.54523 3 -4 5 -11 7.21742 1.74246 2 4 5 11 5.41050 1.75206 2 5 -5 11 26.7038 2.7769 1 -5 -5 -11 29.7747 2.7610 4 -5 -5 -11 29.1535 2.7315 3 -5 -5 -11 30.5546 2.7436 2 -5 5 -11 23.4799 2.6583 2 -5 5 -11 30.1126 2.8684 3 -6 -5 -11 3.20942 1.56353 2 6 -5 11 -0.4439 1.5159 1 -6 5 -11 -0.1029 1.5395 2 -6 5 -11 -0.8503 1.3887 3 7 -5 11 15.8547 2.5819 1 7 5 11 14.8702 2.5708 1 -7 5 -11 16.6709 2.5045 2 8 -5 11 0.78147 1.90968 1 -8 5 -11 3.96952 2.03744 2 8 5 11 3.19629 2.11279 1 9 -5 11 14.0912 2.9354 1 -9 5 -11 14.8760 2.7625 2 9 5 11 7.85729 2.64117 1 10 -5 11 29.6707 3.8438 1 10 5 11 29.3280 3.6460 1 -15 -6 11 26.7583 3.5369 2 15 -6 -11 29.3705 3.6855 4 15 6 -11 23.6226 3.4288 4 -15 6 11 24.3056 3.6115 2 14 -6 -11 314.464 11.052 4 -14 -6 11 340.469 11.144 2 14 6 -11 305.832 11.133 4 -14 6 11 311.974 11.027 2 -13 -6 11 37.3088 3.6193 2 13 -6 -11 33.7674 3.6561 4 -13 6 11 38.5247 3.6573 2 13 6 -11 33.0643 3.6373 4 -12 -6 11 -0.5861 1.5109 2 12 -6 -11 0.03924 1.75669 4 12 6 -11 1.58802 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11 4.88976 1.65114 2 4 -6 -11 4.98931 1.43233 4 -4 6 11 2.71120 1.22280 2 4 6 -11 5.25729 1.24444 4 4 6 -11 6.46607 1.48760 3 -3 -6 11 79.3312 3.9358 2 3 -6 -11 87.1773 4.0653 3 3 -6 -11 86.8969 3.9277 4 3 6 -11 79.9357 3.3178 4 -3 6 11 83.8320 3.7152 2 3 6 -11 74.8684 3.7869 3 2 -6 -11 1.43068 1.23856 3 2 -6 -11 2.32892 1.32687 4 -2 -6 11 2.98668 1.53386 2 -2 6 11 4.94119 1.37027 2 2 6 -11 4.63066 1.40913 3 -1 -6 11 11.1028 1.9827 2 1 -6 -11 11.0619 1.7457 3 1 -6 -11 11.3619 1.7654 4 -1 6 11 14.7866 1.7914 2 1 6 -11 14.1675 1.9321 3 0 -6 11 571.498 15.805 2 0 -6 11 566.736 14.770 1 0 -6 -11 570.107 15.680 3 0 -6 -11 574.092 15.398 4 0 6 11 563.990 15.026 2 0 6 -11 565.819 15.710 3 -1 -6 -11 35.9087 2.7334 3 -1 -6 -11 36.5604 2.5947 4 1 -6 11 40.3595 3.0387 2 1 -6 11 33.3845 2.4373 1 -1 6 -11 31.4061 2.7758 3 1 6 11 35.4948 2.6140 2 -2 -6 -11 194.087 6.957 3 2 -6 11 188.275 7.289 2 -2 -6 -11 195.860 6.788 4 2 -6 11 203.874 6.609 1 2 6 11 210.278 6.806 2 -2 6 -11 193.624 7.068 3 -3 -6 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30.7325 3.6998 4 -14 7 11 30.4373 3.6479 2 14 7 -11 28.6605 3.7147 4 13 -7 -11 75.6776 4.7113 4 -13 -7 11 76.0068 4.6869 2 -13 7 11 74.4927 4.7061 2 13 7 -11 71.4466 4.7471 4 12 -7 -11 -2.7411 1.4477 4 -12 -7 11 1.78320 1.74640 2 -12 7 11 -0.9798 1.6788 2 12 7 -11 -2.3505 1.5246 4 -11 -7 11 122.929 5.495 2 11 -7 -11 123.380 5.704 4 11 7 -11 107.919 5.583 4 -11 7 11 127.788 5.694 2 10 -7 -11 20.6555 2.7232 4 -10 -7 11 13.6458 2.3055 2 10 7 -11 23.0651 2.8009 4 -10 7 11 19.7919 2.6114 2 -9 -7 11 203.407 7.474 2 9 -7 -11 211.705 7.675 4 9 7 -11 211.267 7.583 4 -9 7 11 218.368 7.461 2 -9 7 11 204.893 7.286 3 8 -7 -11 -0.2498 1.3131 4 -8 -7 11 1.73593 1.43939 2 -8 7 11 1.49188 1.37147 2 -8 7 11 2.46867 1.50484 3 8 7 -11 0.08530 1.14912 3 8 7 -11 -1.1268 1.3752 4 -7 -7 11 264.613 8.556 2 7 -7 -11 263.710 8.742 4 7 7 -11 258.715 8.120 3 -7 7 11 271.585 8.435 2 7 7 -11 260.798 8.354 4 -7 7 11 252.688 8.621 3 -6 -7 11 59.4986 3.5277 2 6 -7 -11 55.1931 3.3849 4 6 7 -11 53.8512 3.1439 4 -6 7 11 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68.6589 3.7933 3 7 -4 -14 55.3949 3.7435 4 -7 -4 14 63.2842 3.8799 2 7 -4 -14 65.2257 3.6682 3 -7 4 14 61.8459 3.8932 2 7 4 -14 59.7434 3.5772 4 7 4 -14 63.2643 3.5619 3 6 -4 -14 59.2954 3.7249 4 -6 -4 14 58.8183 3.7476 2 6 -4 -14 66.8347 3.7327 3 6 4 -14 59.6365 3.5811 3 -6 4 14 64.8276 3.9094 2 6 4 -14 61.6860 3.5814 4 -5 -4 14 12.7142 2.1522 2 5 -4 -14 10.3716 2.0995 4 5 -4 -14 11.4669 2.0552 3 -5 4 14 8.70812 1.92206 2 5 4 -14 13.4828 2.1160 3 5 4 -14 12.0642 1.9153 4 4 -4 -14 107.705 5.046 3 -4 -4 14 109.187 5.022 2 4 -4 -14 104.681 4.773 4 -4 4 14 111.189 4.817 2 4 4 -14 97.4960 4.7639 3 3 -4 -14 15.1703 2.2765 3 -3 -4 14 11.8109 2.2938 2 3 -4 -14 15.2621 2.1241 4 -3 4 14 9.20427 1.90261 2 3 4 -14 12.9500 2.1925 3 2 -4 -14 335.863 10.149 4 -2 -4 14 327.656 10.436 2 -2 4 14 313.166 9.929 2 2 4 -14 320.160 10.367 3 1 -4 -14 26.0336 2.8094 3 -1 -4 14 23.6341 2.8982 2 1 -4 -14 21.2100 2.4835 4 1 4 -14 19.6585 2.6065 3 -1 4 14 19.0658 2.4909 2 0 -4 -14 113.289 4.914 4 0 -4 14 112.792 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49.9746 3.5343 3 4 5 -14 55.7030 3.5014 3 -4 5 14 45.8367 3.1524 2 -3 -5 14 17.0755 2.4914 2 3 -5 -14 15.9347 2.2112 4 3 -5 -14 11.1071 2.1531 3 -3 5 14 13.4793 2.1141 2 3 5 -14 15.0895 2.3237 3 2 -5 -14 169.780 6.889 3 -2 -5 14 194.590 7.214 2 2 -5 -14 193.257 6.934 4 -2 5 14 184.508 6.737 2 2 5 -14 193.474 7.167 3 -1 -5 14 2.01409 1.80829 2 1 -5 -14 1.80899 1.46810 4 1 -5 -14 0.34631 1.46447 3 1 5 -14 3.28610 1.70353 3 -1 5 14 1.83987 1.46814 2 0 -5 -14 53.3824 3.6014 3 0 -5 14 50.2866 4.1204 2 0 -5 -14 52.0514 3.2957 4 0 5 14 56.5730 3.5619 2 0 5 -14 59.1299 3.7700 3 1 -5 14 2.85836 1.83740 2 -1 -5 -14 0.95822 1.55868 3 -1 -5 -14 -0.2576 1.4201 4 -1 5 -14 -0.6382 1.4115 3 1 5 14 0.00257 1.49031 2 2 -5 14 45.9488 4.0924 2 -2 -5 -14 45.3549 3.5603 3 -2 5 -14 42.0116 3.6884 3 2 5 14 50.8793 3.5417 2 3 -5 14 12.2143 2.5966 2 -3 -5 -14 8.61431 1.95780 3 -3 5 -14 9.78817 2.28973 3 3 5 14 7.69182 2.12939 2 4 -5 14 87.4941 5.3795 2 -4 -5 -14 86.8968 4.7921 3 -4 5 -14 95.7844 5.0856 3 5 -5 14 43.1691 4.3280 2 -5 -5 -14 39.2659 3.5735 3 -5 5 -14 52.1478 3.9334 3 -6 5 -14 65.9015 4.3845 2 -7 5 -14 2.30136 1.99854 2 -14 -6 14 17.1106 3.1230 2 14 6 -14 20.0945 3.3253 4 13 -6 -14 44.6158 4.3562 4 -13 -6 14 40.3780 3.9937 2 -13 6 14 45.7238 4.1351 2 13 6 -14 45.8634 4.2189 4 -12 -6 14 1.94635 2.11212 2 12 -6 -14 2.76964 1.99282 4 -12 6 14 5.21982 2.15234 2 12 6 -14 2.43016 2.06046 4 11 -6 -14 10.6682 2.3579 4 -11 -6 14 12.6857 2.6358 2 11 6 -14 14.1761 2.6277 4 -11 6 14 13.6127 2.4591 2 -10 -6 14 78.6382 4.6149 2 10 -6 -14 78.5585 4.6984 4 10 6 -14 81.0489 4.6721 4 -10 6 14 77.9472 4.4825 2 -9 -6 14 203.858 7.807 2 9 -6 -14 201.468 7.912 4 -9 6 14 205.965 7.622 2 9 6 -14 204.283 7.633 4 -9 6 14 194.665 7.632 3 8 -6 -14 33.6481 3.2752 4 -8 -6 14 34.9175 3.2904 2 8 6 -14 36.5831 3.0760 3 -8 6 14 33.9439 3.2652 3 -8 6 14 29.3108 2.9940 2 8 6 -14 36.1214 3.1579 4 -7 -6 14 6.28143 1.92365 2 7 -6 -14 6.46636 1.84306 3 7 -6 -14 5.80462 1.99399 4 -7 6 14 7.46019 1.98993 2 -7 6 14 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3.7351 2 6 -6 -18 135.201 6.661 4 6 -6 -18 158.276 6.967 3 -6 -6 18 143.651 6.921 2 -6 6 18 148.405 6.639 2 6 6 -18 157.482 6.940 3 5 -6 -18 7.88021 2.22093 4 5 -6 -18 8.74702 2.45336 3 -5 -6 18 4.62905 2.31366 2 -5 6 18 9.59975 2.43931 2 5 6 -18 6.36587 2.34194 3 -4 -6 18 224.698 8.858 2 4 -6 -18 222.782 8.699 3 4 -6 -18 217.600 8.474 4 -4 6 18 210.330 8.217 2 4 6 -18 206.165 8.487 3 3 -6 -18 20.2981 2.9790 3 3 -6 -18 12.8049 2.4699 4 -3 -6 18 10.4744 2.7584 2 -3 6 18 14.4444 2.5739 2 3 6 -18 11.9914 2.7587 3 2 -6 -18 14.3344 2.6209 3 -2 -6 18 20.2419 3.3026 2 2 6 -18 14.4188 2.7761 3 -1 -6 18 5.98729 2.43441 2 1 -6 -18 6.21844 2.27800 3 1 6 -18 6.89836 2.36771 3 0 -6 18 82.0020 5.4312 2 0 -6 -18 90.6506 5.3043 3 0 6 -18 86.8710 5.3759 3 -1 -6 -18 10.0947 2.6495 3 -10 7 18 47.2365 4.1893 2 9 -7 -18 -0.9354 1.8117 4 -9 -7 18 2.72760 2.18164 2 -9 7 18 2.70607 2.09143 3 -9 7 18 -0.1190 1.9653 2 -8 -7 18 46.4647 4.3017 2 8 -7 -18 48.4178 4.5218 4 8 7 -18 49.0759 3.8342 3 -8 7 18 53.0154 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11.0653 2.7991 2 -8 8 18 8.92335 2.47945 2 -8 8 18 11.4751 2.7909 3 8 8 -18 9.50752 2.39653 3 -7 -8 18 18.5817 3.1514 2 7 -8 -18 20.0764 3.2522 4 -7 8 18 17.3696 2.9102 2 -7 8 18 16.0239 3.0816 3 7 8 -18 19.4209 2.8938 3 -6 -8 18 118.308 6.320 2 6 -8 -18 121.693 6.180 4 6 8 -18 125.845 6.138 3 -6 8 18 108.013 6.333 3 -5 -8 18 18.1461 3.1236 2 5 -8 -18 19.0963 3.0359 4 -5 8 18 20.0948 3.3961 3 5 8 -18 22.4715 3.1457 3 4 -8 -18 42.2339 4.1344 4 -4 -8 18 46.7662 4.4991 2 4 8 -18 49.3605 4.3200 3 -4 8 18 38.6392 4.1922 3 3 -8 -18 78.2801 4.9814 3 -3 -8 18 76.7661 5.2072 2 3 -8 -18 79.8482 4.8481 4 -3 8 18 70.9734 5.3247 3 3 8 -18 70.9836 4.8744 3 2 -8 -18 46.5906 4.1346 4 2 -8 -18 34.2748 3.7788 3 -2 -8 18 43.2320 4.3257 2 2 8 -18 40.5002 4.0446 3 -2 8 18 42.1578 4.3835 3 -1 -8 18 26.6422 3.6927 2 1 -8 -18 21.2713 3.1210 3 1 8 -18 26.5736 3.3821 3 -1 8 18 22.3519 3.4780 3 -10 9 18 120.084 6.166 2 -9 9 18 95.7996 5.4213 2 -9 9 18 101.231 5.947 3 -8 -9 18 35.8648 3.9267 2 8 -9 -18 33.9662 3.9789 4 8 9 -18 35.8403 3.7612 3 -8 9 18 29.2445 3.7860 3 -7 -9 18 39.9840 4.0470 2 7 -9 -18 39.5455 4.1053 4 7 9 -18 42.8381 4.0690 3 -7 9 18 40.9001 4.2190 3 6 -9 -18 23.6307 3.4691 4 -6 -9 18 24.4208 3.4855 2 -6 9 18 25.2875 3.6265 3 6 9 -18 26.5641 3.4400 3 5 -9 -18 130.172 6.487 4 -5 -9 18 124.302 6.463 2 -5 9 18 106.433 6.218 3 5 9 -18 111.246 6.119 3 4 -9 -18 89.8027 5.3170 4 -4 -9 18 93.4663 5.6540 2 4 9 -18 89.3118 5.5061 3 -4 9 18 81.2734 5.6643 3 3 -9 -18 96.5059 5.4359 4 -3 -9 18 96.3520 5.7940 2 3 9 -18 94.6478 5.5597 3 -3 9 18 92.8293 5.9639 3 2 -9 -18 80.5887 5.0728 4 -2 -9 18 73.8170 5.2831 2 -2 9 18 76.2306 5.4978 3 2 9 -18 77.9200 5.2012 3 -9 10 18 54.3403 4.8613 3 8 10 -18 87.7882 5.1009 3 -8 10 18 78.8190 5.2583 3 -7 -10 18 4.66048 2.39344 2 7 -10 -18 10.0650 2.7155 4 7 10 -18 11.6898 2.5644 3 -7 10 18 7.65782 2.67702 3 -6 -10 18 64.8022 4.9266 2 6 -10 -18 68.8218 5.0134 4 6 10 -18 68.8881 4.7464 3 -6 10 18 71.3461 5.1290 3 5 -10 -18 32.2384 3.7921 4 -5 -10 18 38.0854 4.0892 2 -5 10 18 30.3681 3.8649 3 5 10 -18 28.3075 3.6256 3 -4 -10 18 56.4412 4.8335 2 4 -10 -18 55.8733 4.7684 4 4 10 -18 46.9288 4.3611 3 -4 10 18 51.5713 4.8242 3 -3 -10 18 22.3440 3.3975 2 3 -10 -18 30.7013 3.5990 4 -3 10 18 24.8742 3.6587 3 3 10 -18 30.2110 3.7542 3 2 -10 -18 8.28965 2.57687 4 1 -10 -18 49.8298 4.5230 4 -8 11 18 14.1558 3.0667 3 8 11 -18 17.7221 3.0385 3 7 11 -18 8.21883 2.51090 3 -7 11 18 9.84901 2.86839 3 6 -11 -18 150.388 7.501 4 -6 11 18 154.030 7.694 3 6 11 -18 179.933 7.737 3 -5 -11 18 97.5799 5.9834 2 5 -11 -18 112.468 6.148 4 5 11 -18 116.062 6.157 3 4 -11 -18 7.91779 2.51749 4 4 11 -18 9.15777 2.63178 3 3 -11 -18 64.6518 4.8128 4 2 -11 -18 81.5000 5.3256 4 1 -11 -18 10.6995 2.7869 4 0 -11 -18 5.95077 2.46736 4 8 12 -18 58.5406 4.6277 3 7 12 -18 43.5954 4.1853 3 3 -12 -18 3.91927 2.40479 4 2 -12 -18 3.94398 2.19408 4 10 0 -19 0.04390 1.94347 4 9 0 -19 4.65417 2.18951 4 9 0 -19 6.17136 2.11289 3 -8 0 19 -2.1855 2.0177 2 8 0 -19 -3.3277 1.4521 3 -7 0 19 20.0601 3.1185 2 7 0 -19 20.6866 2.9660 3 -6 0 19 0.48646 2.13524 2 6 0 -19 -1.4836 1.7538 3 5 0 -19 43.8704 4.1700 3 -5 0 19 39.8108 3.9509 2 4 0 -19 -1.9506 1.6536 3 -4 0 19 -0.0396 1.8404 2 3 0 -19 103.757 5.905 3 -3 0 19 106.476 5.775 2 2 0 -19 5.14480 2.09626 3 -2 0 19 -1.9932 2.0737 2 -1 0 19 31.0127 3.6446 2 0 0 19 -5.1537 1.9413 2 10 -1 -19 14.6379 2.8656 4 10 1 -19 4.70120 2.32106 4 9 -1 -19 8.81745 2.67291 4 9 -1 -19 9.79151 2.44065 3 9 1 -19 13.9282 2.6729 3 8 -1 -19 5.78590 2.24653 3 8 -1 -19 8.64172 2.46681 4 -8 -1 19 9.61298 2.60741 2 8 1 -19 7.08596 2.24061 3 -8 1 19 8.01342 2.46822 2 7 -1 -19 12.9387 2.6828 3 -7 -1 19 10.8113 2.8537 2 -7 1 19 16.0971 2.9644 2 7 1 -19 13.1078 2.7027 3 -6 -1 19 0.10920 2.16031 2 6 -1 -19 -1.8798 1.6317 3 6 1 -19 -0.4512 1.8903 3 -6 1 19 -0.9949 1.7991 2 -5 -1 19 66.0739 4.7714 2 5 -1 -19 58.0460 4.3221 3 -5 1 19 57.3911 4.4876 2 5 1 -19 53.3806 4.5970 3 4 -1 -19 0.21102 1.99861 3 -4 -1 19 6.20148 2.45865 2 -4 1 19 0.15418 2.07214 2 4 1 -19 -0.8110 1.8153 3 -3 -1 19 41.8455 4.2062 2 3 -1 -19 35.2952 3.8874 3 3 1 -19 37.6391 3.9083 3 -3 1 19 42.6852 4.1056 2 2 -1 -19 2.22937 1.88399 3 -2 -1 19 0.88861 2.03820 2 2 1 -19 -0.3361 1.7083 3 -2 1 19 1.34487 2.07053 2 -1 -1 19 33.9515 3.9750 2 -1 1 19 32.7934 3.8096 2 0 1 19 19.9933 3.2431 2 10 -2 -19 3.65528 2.21571 4 9 -2 -19 26.9547 3.4819 4 9 -2 -19 28.9156 3.3853 3 -8 -2 19 -0.7002 2.1501 2 8 -2 -19 0.65688 1.81310 3 8 -2 -19 -0.0007 1.7453 4 -8 2 19 0.90252 1.95763 2 8 2 -19 1.60278 1.97995 3 -7 -2 19 -1.6414 1.9449 2 7 -2 -19 -0.1539 1.7799 3 7 2 -19 -2.6652 1.8112 3 -7 2 19 2.16055 2.25401 2 6 -2 -19 2.41871 2.03462 3 -6 -2 19 3.18990 2.36775 2 -6 2 19 0.23775 1.97374 2 6 2 -19 1.19143 1.92062 3 -5 -2 19 93.8001 5.5817 2 5 -2 -19 107.189 5.852 3 -5 2 19 104.229 5.715 2 5 2 -19 104.902 5.679 3 -4 -2 19 10.6503 2.6835 2 4 -2 -19 6.17020 2.30426 3 4 2 -19 7.75372 2.35425 3 -4 2 19 12.1124 2.7603 2 -3 -2 19 64.4872 4.5761 2 3 -2 -19 49.7748 4.4525 3 3 2 -19 61.7740 4.4954 3 -3 2 19 51.6563 4.5573 2 2 -2 -19 12.6622 2.7094 3 -2 -2 19 9.97874 2.89044 2 -2 2 19 6.79221 2.37334 2 2 2 -19 13.7192 2.8449 3 -1 -2 19 2.60156 2.47463 2 -1 2 19 5.99031 2.55272 2 0 2 19 7.62624 2.68878 2 9 -3 -19 9.93279 2.48914 3 9 -3 -19 10.0830 2.6627 4 8 -3 -19 81.3018 5.0464 3 8 -3 -19 81.2765 5.2018 4 8 3 -19 80.7261 5.0083 3 -8 3 19 72.3283 4.8319 2 -7 -3 19 0.94520 2.29946 2 7 -3 -19 3.09519 2.00472 4 7 -3 -19 3.65883 2.20335 3 -7 3 19 1.89673 2.21425 2 7 3 -19 5.60092 2.23143 3 -6 -3 19 12.0412 2.7636 2 6 -3 -19 6.01443 2.23595 3 -6 3 19 10.0273 2.5988 2 6 3 -19 7.10520 2.29193 3 -5 -3 19 19.5578 3.1718 2 5 -3 -19 18.6342 2.9743 3 5 3 -19 22.9705 3.1758 3 -5 3 19 22.6529 3.1643 2 4 -3 -19 3.63676 2.21925 3 -4 -3 19 1.53590 2.29172 2 4 3 -19 0.84441 1.90608 3 -4 3 19 3.90913 2.30875 2 3 -3 -19 70.0604 4.9120 3 -3 -3 19 68.0542 4.8535 2 -3 3 19 71.0339 4.8645 2 3 3 -19 77.0415 4.9846 3 2 -3 -19 6.07404 2.23597 3 -2 -3 19 -0.1576 2.2532 2 -2 3 19 3.39638 2.12231 2 2 3 -19 1.13496 2.04938 3 -1 3 19 39.7807 4.1027 2 0 3 19 34.3168 3.9061 2 9 -4 -19 25.3466 3.5704 4 9 -4 -19 23.2565 3.1707 3 8 -4 -19 30.9911 3.4816 3 8 -4 -19 26.0591 3.5208 4 8 4 -19 32.9044 3.5757 3 -8 4 19 35.4762 3.8366 2 -7 -4 19 18.4541 3.3516 2 7 -4 -19 23.2495 3.2562 4 7 -4 -19 17.2769 2.8651 3 -7 4 19 18.4580 2.9838 2 7 4 -19 20.7192 3.0621 3 6 -4 -19 33.9515 3.7169 3 -6 -4 19 30.0864 3.6386 2 6 -4 -19 25.6598 3.3242 4 -6 4 19 42.0213 4.0663 2 6 4 -19 35.6975 3.7178 3 -5 -4 19 101.565 5.920 2 5 -4 -19 112.995 6.007 3 5 4 -19 102.307 5.739 3 -5 4 19 114.658 5.935 2 4 -4 -19 0.89461 1.87090 3 -4 -4 19 4.00004 2.47965 2 4 4 -19 3.25926 2.09917 3 -4 4 19 2.05001 2.06235 2 3 -4 -19 10.4316 2.5712 3 -3 -4 19 14.7414 2.9517 2 3 4 -19 13.8558 2.7897 3 -3 4 19 9.44935 2.55600 2 -2 -4 19 15.2882 3.1829 2 -2 4 19 20.4895 3.1208 2 -1 4 19 75.7730 4.8357 2 0 4 19 5.47482 2.31942 2 9 -5 -19 6.90344 2.50398 4 -9 5 19 3.52039 2.33797 3 8 -5 -19 25.0606 3.3700 3 8 -5 -19 26.0688 3.4321 4 8 5 -19 24.8084 3.2992 3 -8 5 19 27.2833 3.4775 2 7 -5 -19 62.9883 4.5797 3 7 -5 -19 60.6279 4.4391 4 7 5 -19 58.5806 4.4450 3 -7 5 19 54.4347 4.6127 2 -6 -5 19 48.8238 4.4789 2 6 -5 -19 44.4606 4.1554 4 6 -5 -19 47.7021 4.2321 3 6 5 -19 40.9780 4.0631 3 -6 5 19 45.9249 4.1141 2 5 -5 -19 -0.7868 1.7944 3 5 -5 -19 0.56178 2.02011 4 -5 -5 19 0.13479 2.00743 2 5 5 -19 3.24585 2.16986 3 -5 5 19 3.26306 2.19931 2 -4 -5 19 1.16796 2.08754 2 4 -5 -19 1.90170 2.12244 3 -4 5 19 0.98015 1.98239 2 4 5 -19 1.45013 2.04822 3 -3 -5 19 107.137 6.044 2 3 -5 -19 104.165 5.849 3 -3 5 19 115.667 5.929 2 3 5 -19 114.740 6.125 3 -2 5 19 1.10598 2.12539 2 -9 6 19 61.5737 4.8459 3 8 -6 -19 8.63111 2.68957 4 8 6 -19 6.72444 2.41848 3 -8 6 19 4.45633 2.48833 3 -8 6 19 8.74444 2.65241 2 7 -6 -19 8.30556 2.54862 4 7 -6 -19 8.00245 2.48166 3 -7 6 19 7.19617 2.63775 3 -7 6 19 15.8136 2.9097 2 7 6 -19 6.73077 2.48563 3 6 -6 -19 42.5707 4.2093 4 6 -6 -19 43.6917 4.1287 3 -6 6 19 40.3812 3.9876 2 6 6 -19 39.1726 3.9605 3 5 -6 -19 210.362 8.682 3 5 -6 -19 213.847 8.670 4 -5 -6 19 216.235 8.778 2 5 6 -19 202.624 8.652 3 -5 6 19 216.744 8.425 2 4 -6 -19 4.30078 2.22388 3 -4 -6 19 4.35889 2.43703 2 4 6 -19 7.72229 2.38071 3 -4 6 19 4.29836 2.32406 2 -9 7 19 -1.9615 2.0017 3 8 7 -19 4.89803 2.29165 3 -8 7 19 4.05280 2.33593 2 -8 7 19 5.12128 2.42735 3 7 -7 -19 95.8502 5.8028 4 -7 7 19 107.362 5.551 2 7 7 -19 104.534 5.828 3 -7 7 19 97.6103 5.8957 3 6 -7 -19 30.6739 3.6034 4 -6 7 19 21.7740 3.1765 2 -6 7 19 23.4501 3.6878 3 6 7 -19 24.8593 3.4458 3 5 -7 -19 31.2870 3.6375 4 5 7 -19 21.3252 3.2674 3 4 -7 -19 6.34631 2.49096 4 8 8 -19 -2.0156 1.7485 3 7 -8 -19 10.2517 2.6410 4 7 8 -19 8.38326 2.39275 3 6 -8 -19 -3.1495 1.9397 4 6 8 -19 -0.7446 1.9190 3 5 -8 -19 207.431 8.671 4 4 -8 -19 39.9635 4.0791 4 5 -9 -19 2.27522 2.38214 4 4 -9 -19 38.5168 4.0249 4 3 -9 -19 177.374 7.807 4 8 -3 -20 0.90213 2.13587 4 -4 4 20 39.0597 4.1299 2 -3 4 20 0.13177 2.22061 2 7 -5 -20 84.0521 5.4790 4 -5 5 20 0.47536 2.20878 2 -4 5 20 30.8053 3.6917 2 6 -6 -20 185.815 8.242 4 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 27892 data_Triphos*FeCOT _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C49 H47 Fe P3' _chemical_formula_sum 'C49 H47 Fe P3' _chemical_formula_iupac ? _chemical_formula_weight 784.62 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.839(2) _cell_length_b 10.8349(12) _cell_length_c 18.785(2) _cell_angle_alpha 90 _cell_angle_beta 97.2960(10) _cell_angle_gamma 90 _cell_volume 3803.3(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 120(1) _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.060 _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS v. 1 (Sheldrick, 2008)' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.97 _exptl_special_details ; ; _diffrn_ambient_temperature 120(1) _diffrn_source 'fine focus sealed tube' _diffrn_source_type ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker D8 with APEXII CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36297 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.45 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogen atoms associated with the Fe bound carbon atom positions of the COT ligand were located on the difference map and refined with isotropic temperature factors set to 1.2 times the Uiso of the corresponding carbon atom. ; _reflns_number_total 6995 _reflns_number_gt 5100 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.0928 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_number_reflns 6995 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+2.2664P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.386 _refine_diff_density_min -0.348 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'APEX II, v. 7.0 (Bruker AXS, 2009)' _computing_cell_refinement 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_data_reduction 'SAINT+, v. 7.66a (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'XShell ver. 6.3.1 (Bruker AXS, 2004)' _computing_publication_material 'Bruker APEX2 v1013.6-2 (Bruker-AXS, 2013)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe1 0.22100(2) 0.83744(3) 0.28688(2) 0.01342(11) Uani d . . . 1 . . P P1 0.18893(4) 0.80527(6) 0.39259(4) 0.01403(16) Uani d . . . 1 . . P P2 0.25629(4) 0.64334(6) 0.28602(4) 0.01382(16) Uani d . . . 1 . . P P3 0.32688(4) 0.90303(6) 0.33322(4) 0.01431(16) Uani d . . . 1 . . C C1 0.16699(14) 1.0209(3) 0.27309(15) 0.0158(6) Uani d . . . 1 . . H H1 0.1533(14) 1.056(2) 0.3169(14) 0.019 Uiso d U . . 1 . . C C2 0.12475(14) 0.9161(3) 0.24925(14) 0.0162(6) Uani d . . . 1 . . H H2 0.0838(15) 0.901(2) 0.2742(14) 0.019 Uiso d U . . 1 . . C C3 0.14240(15) 0.8287(3) 0.20021(14) 0.0174(6) Uani d . . . 1 . . H H3 0.1123(14) 0.757(3) 0.1930(14) 0.021 Uiso d U . . 1 . . C C4 0.20560(15) 0.8295(3) 0.16540(14) 0.0183(6) Uani d . . . 1 . . H H4 0.2144(14) 0.749(3) 0.1446(14) 0.022 Uiso d U . . 1 . . C C5 0.23864(15) 0.9211(3) 0.12515(15) 0.0220(7) Uani d . . . 1 . . H H5 0.267 0.8856 0.0936 0.026 Uiso calc U . R 1 . . C C6 0.23896(15) 1.0455(3) 0.12142(15) 0.0234(7) Uani d . . . 1 . . H H6 0.2553 1.0778 0.0806 0.028 Uiso calc U . R 1 . . C C7 0.21822(14) 1.1349(3) 0.17013(15) 0.0193(6) Uani d . . . 1 . . H H7 0.221 1.2162 0.1548 0.023 Uiso calc U . R 1 . . C C8 0.19523(14) 1.1215(3) 0.23481(15) 0.0192(6) Uani d . . . 1 . . H H8 0.1983 1.1946 0.261 0.023 Uiso calc U . R 1 . . C C9 0.25574(13) 0.7183(2) 0.45432(14) 0.0151(6) Uani d . . . 1 . . H H9A 0.2648 0.7645 0.4988 0.018 Uiso calc U . R 1 . . H H9B 0.2342 0.6405 0.4655 0.018 Uiso calc U . R 1 . . C C10 0.32219(14) 0.6020(2) 0.36433(14) 0.0153(6) Uani d . . . 1 . . H H10A 0.3099 0.5208 0.3808 0.018 Uiso calc U . R 1 . . H H10B 0.3689 0.5954 0.348 0.018 Uiso calc U . R 1 . . C C11 0.36740(14) 0.8093(2) 0.41166(14) 0.0169(6) Uani d . . . 1 . . H H11A 0.4158 0.7877 0.4038 0.02 Uiso calc U . R 1 . . H H11B 0.371 0.8614 0.4539 0.02 Uiso calc U . R 1 . . C C12 0.32872(14) 0.6897(2) 0.42856(14) 0.0138(6) Uani d . . . 1 . . C C13 0.37557(14) 0.6249(2) 0.49058(14) 0.0175(6) Uani d . . . 1 . . H H13A 0.3519 0.5516 0.5039 0.026 Uiso calc U . R 1 . . H H13B 0.3833 0.6795 0.5311 0.026 Uiso calc U . R 1 . . H H13C 0.4208 0.6032 0.4755 0.026 Uiso calc U . R 1 . . C C14 0.10604(14) 0.7197(2) 0.40178(14) 0.0154(6) Uani d . . . 1 . . C C15 0.05931(14) 0.6834(2) 0.34214(15) 0.0185(6) Uani d . . . 1 . . H H15 0.0719 0.696 0.2964 0.022 Uiso calc U . R 1 . . C C16 -0.00591(15) 0.6288(3) 0.34994(17) 0.0233(7) Uani d . . . 1 . . H H16 -0.0369 0.6059 0.3096 0.028 Uiso calc U . R 1 . . C C17 -0.02445(16) 0.6088(3) 0.41726(17) 0.0256(7) Uani d . . . 1 . . H H17 -0.0682 0.5724 0.4226 0.031 Uiso calc U . R 1 . . C C18 0.02204(15) 0.6427(3) 0.47741(17) 0.0245(7) Uani d . . . 1 . . H H18 0.0094 0.6287 0.523 0.029 Uiso calc U . R 1 . . C C19 0.08671(15) 0.6970(3) 0.47004(15) 0.0207(7) Uani d . . . 1 . . H H19 0.1177 0.7186 0.5106 0.025 Uiso calc U . R 1 . . C C20 0.16760(14) 0.9372(2) 0.44845(14) 0.0150(6) Uani d . . . 1 . . C C21 0.09928(15) 0.9897(3) 0.43591(15) 0.0193(6) Uani d . . . 1 . . H H21 0.0657 0.9568 0.4004 0.023 Uiso calc U . R 1 . . C C22 0.08091(15) 1.0896(3) 0.47538(15) 0.0236(7) Uani d . . . 1 . . H H22 0.0354 1.1237 0.4661 0.028 Uiso calc U . R 1 . . C C23 0.13000(16) 1.1391(3) 0.52862(16) 0.0264(7) Uani d . . . 1 . . H H23 0.1174 1.2054 0.5559 0.032 Uiso calc U . R 1 . . C C24 0.19807(16) 1.0891(3) 0.54102(15) 0.0251(7) Uani d . . . 1 . . H H24 0.2317 1.1229 0.5762 0.03 Uiso calc U . R 1 . . C C25 0.21633(15) 0.9893(3) 0.50138(14) 0.0191(6) Uani d . . . 1 . . H H25 0.2622 0.9565 0.5104 0.023 Uiso calc U . R 1 . . C C26 0.30528(14) 0.5699(2) 0.21743(14) 0.0161(6) Uani d . . . 1 . . C C27 0.34071(14) 0.6387(3) 0.17049(14) 0.0178(6) Uani d . . . 1 . . H H27 0.3364 0.7242 0.1697 0.021 Uiso calc U . R 1 . . C C28 0.38252(14) 0.5806(3) 0.12489(15) 0.0223(7) Uani d . . . 1 . . H H28 0.4061 0.6279 0.0939 0.027 Uiso calc U . R 1 . . C C29 0.38978(15) 0.4542(3) 0.12471(15) 0.0228(7) Uani d . . . 1 . . H H29 0.4173 0.4162 0.0933 0.027 Uiso calc U . R 1 . . C C30 0.35563(14) 0.3847(3) 0.17184(15) 0.0207(7) Uani d . . . 1 . . H H30 0.3606 0.2993 0.1726 0.025 Uiso calc U . R 1 . . C C31 0.31392(14) 0.4417(3) 0.21798(15) 0.0183(6) Uani d . . . 1 . . H H31 0.2914 0.3941 0.2497 0.022 Uiso calc U . R 1 . . C C32 0.18666(14) 0.5241(2) 0.28768(14) 0.0162(6) Uani d . . . 1 . . C C33 0.14264(14) 0.4970(2) 0.22409(15) 0.0191(6) Uani d . . . 1 . . H H33 0.1504 0.5365 0.1818 0.023 Uiso calc U . R 1 . . C C34 0.08756(15) 0.4121(3) 0.22303(16) 0.0220(7) Uani d . . . 1 . . H H34 0.0588 0.3947 0.1802 0.026 Uiso calc U . R 1 . . C C35 0.07526(15) 0.3532(3) 0.28563(16) 0.0230(7) Uani d . . . 1 . . H H35 0.0378 0.2971 0.285 0.028 Uiso calc U . R 1 . . C C36 0.11816(15) 0.3772(3) 0.34870(15) 0.0209(7) Uani d . . . 1 . . H H36 0.1103 0.3366 0.3906 0.025 Uiso calc U . R 1 . . C C37 0.17340(15) 0.4626(2) 0.34975(15) 0.0184(6) Uani d . . . 1 . . H H37 0.2021 0.4789 0.3928 0.022 Uiso calc U . R 1 . . C C38 0.34808(14) 1.0548(2) 0.37705(14) 0.0167(6) Uani d . . . 1 . . C C39 0.29697(15) 1.1374(2) 0.39390(14) 0.0186(6) Uani d . . . 1 . . H H39 0.249 1.1226 0.3779 0.022 Uiso calc U . R 1 . . C C40 0.31613(16) 1.2425(3) 0.43456(15) 0.0232(7) Uani d . . . 1 . . H H40 0.2809 1.2971 0.4453 0.028 Uiso calc U . R 1 . . C C41 0.38652(16) 1.2660(3) 0.45879(15) 0.0229(7) Uani d . . . 1 . . H H41 0.3991 1.3356 0.4865 0.028 Uiso calc U . R 1 . . C C42 0.43865(15) 1.1853(3) 0.44174(15) 0.0211(7) Uani d . . . 1 . . H H42 0.4866 1.201 0.4576 0.025 Uiso calc U . R 1 . . C C43 0.41959(15) 1.0815(3) 0.40124(15) 0.0203(6) Uani d . . . 1 . . H H43 0.4551 1.0282 0.3898 0.024 Uiso calc U . R 1 . . C C44 0.39627(14) 0.9071(3) 0.27280(14) 0.0158(6) Uani d . . . 1 . . C C45 0.39433(15) 1.0069(3) 0.22564(15) 0.0203(7) Uani d . . . 1 . . H H45 0.3606 1.069 0.2279 0.024 Uiso calc U . R 1 . . C C46 0.44191(16) 1.0144(3) 0.17559(15) 0.0253(7) Uani d . . . 1 . . H H46 0.4402 1.0819 0.1448 0.03 Uiso calc U . R 1 . . C C47 0.49175(16) 0.9232(3) 0.17074(16) 0.0264(7) Uani d . . . 1 . . H H47 0.5236 0.929 0.1369 0.032 Uiso calc U . R 1 . . C C48 0.49445(15) 0.8226(3) 0.21655(15) 0.0241(7) Uani d . . . 1 . . H H48 0.5278 0.7602 0.2132 0.029 Uiso calc U . R 1 . . C C49 0.44715(14) 0.8153(3) 0.26742(15) 0.0201(6) Uani d . . . 1 . . H H49 0.4495 0.7481 0.2984 0.024 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.0128(2) 0.0137(2) 0.0135(2) 0.00060(16) 0.00039(16) 0.00058(16) P1 0.0125(4) 0.0145(4) 0.0151(4) 0.0001(3) 0.0015(3) -0.0007(3) P2 0.0143(4) 0.0137(4) 0.0133(4) -0.0005(3) 0.0014(3) -0.0004(3) P3 0.0136(4) 0.0134(4) 0.0158(4) -0.0001(3) 0.0011(3) 0.0000(3) C1 0.0159(15) 0.0168(15) 0.0146(15) 0.0044(12) 0.0018(12) 0.0013(12) C2 0.0120(14) 0.0190(16) 0.0173(15) 0.0017(12) 0.0009(12) 0.0055(12) C3 0.0159(15) 0.0169(16) 0.0179(15) -0.0009(12) -0.0033(12) 0.0037(12) C4 0.0189(15) 0.0206(16) 0.0140(15) 0.0012(13) -0.0028(12) -0.0028(12) C5 0.0268(17) 0.0243(17) 0.0157(15) 0.0017(13) 0.0058(13) -0.0009(12) C6 0.0284(17) 0.0266(18) 0.0150(15) -0.0007(14) 0.0024(13) 0.0063(13) C7 0.0193(15) 0.0163(15) 0.0209(16) -0.0003(12) -0.0034(12) 0.0078(12) C8 0.0179(15) 0.0168(15) 0.0222(16) 0.0028(12) -0.0003(12) 0.0005(12) C9 0.0149(14) 0.0161(15) 0.0143(15) 0.0024(12) 0.0017(11) 0.0027(11) C10 0.0156(14) 0.0132(14) 0.0175(15) -0.0004(12) 0.0037(12) 0.0004(11) C11 0.0127(14) 0.0197(16) 0.0175(15) -0.0005(12) -0.0013(11) 0.0002(12) C12 0.0157(14) 0.0136(14) 0.0120(14) 0.0000(12) 0.0010(11) 0.0004(11) C13 0.0176(15) 0.0172(15) 0.0172(15) 0.0013(12) 0.0005(12) -0.0011(12) C14 0.0128(14) 0.0111(14) 0.0225(16) 0.0011(12) 0.0028(12) 0.0011(12) C15 0.0167(15) 0.0134(15) 0.0254(16) 0.0045(12) 0.0029(12) 0.0027(12) C16 0.0172(16) 0.0158(16) 0.0355(19) -0.0005(12) -0.0024(14) 0.0013(13) C17 0.0152(15) 0.0154(16) 0.046(2) 0.0018(13) 0.0054(14) 0.0037(14) C18 0.0248(17) 0.0192(16) 0.0324(18) 0.0025(13) 0.0150(14) 0.0050(14) C19 0.0201(16) 0.0210(16) 0.0216(16) 0.0020(13) 0.0047(13) 0.0024(13) C20 0.0175(15) 0.0138(14) 0.0146(14) -0.0009(12) 0.0059(12) -0.0001(11) C21 0.0173(15) 0.0195(16) 0.0215(16) 0.0001(13) 0.0038(12) -0.0005(12) C22 0.0197(16) 0.0228(16) 0.0283(17) 0.0055(13) 0.0041(13) 0.0004(14) C23 0.0340(18) 0.0208(17) 0.0257(17) 0.0074(14) 0.0089(14) -0.0067(13) C24 0.0301(18) 0.0234(17) 0.0203(16) 0.0048(14) -0.0025(13) -0.0056(13) C25 0.0184(15) 0.0213(16) 0.0172(15) 0.0014(13) 0.0005(12) -0.0012(12) C26 0.0142(14) 0.0187(15) 0.0143(14) -0.0003(12) -0.0025(11) -0.0022(12) C27 0.0142(15) 0.0202(16) 0.0179(15) 0.0000(12) -0.0027(12) -0.0035(12) C28 0.0167(15) 0.0308(18) 0.0198(16) -0.0042(13) 0.0041(12) 0.0001(13) C29 0.0180(16) 0.0283(18) 0.0221(16) 0.0032(13) 0.0023(13) -0.0060(13) C30 0.0171(15) 0.0165(15) 0.0281(17) 0.0007(12) 0.0004(13) -0.0042(13) C31 0.0169(15) 0.0157(15) 0.0216(16) -0.0013(12) 0.0002(12) 0.0011(12) C32 0.0158(14) 0.0133(14) 0.0193(15) 0.0022(12) 0.0015(12) -0.0027(12) C33 0.0163(15) 0.0178(15) 0.0231(16) 0.0019(12) 0.0027(12) -0.0012(12) C34 0.0161(15) 0.0187(16) 0.0300(17) 0.0032(13) -0.0020(13) -0.0060(13) C35 0.0151(15) 0.0149(15) 0.0395(19) -0.0007(12) 0.0055(14) -0.0008(14) C36 0.0232(16) 0.0167(16) 0.0239(17) 0.0010(13) 0.0073(13) 0.0023(12) C37 0.0186(15) 0.0156(15) 0.0211(16) 0.0017(12) 0.0034(12) -0.0021(12) C38 0.0204(15) 0.0136(14) 0.0164(15) -0.0016(12) 0.0039(12) 0.0018(11) C39 0.0196(15) 0.0174(15) 0.0180(15) -0.0004(12) -0.0011(12) 0.0012(12) C40 0.0253(17) 0.0165(16) 0.0277(17) 0.0053(13) 0.0031(14) -0.0013(13) C41 0.0321(18) 0.0131(15) 0.0233(17) -0.0045(13) 0.0025(14) -0.0034(12) C42 0.0162(15) 0.0215(16) 0.0250(16) -0.0061(13) 0.0004(12) -0.0028(13) C43 0.0168(15) 0.0189(16) 0.0258(16) 0.0001(13) 0.0042(13) -0.0038(13) C44 0.0125(14) 0.0191(15) 0.0147(14) -0.0040(12) -0.0022(11) -0.0035(12) C45 0.0191(16) 0.0207(16) 0.0212(16) 0.0011(13) 0.0030(12) -0.0026(13) C46 0.0300(18) 0.0252(17) 0.0212(16) -0.0033(14) 0.0054(14) 0.0025(13) C47 0.0223(17) 0.0363(19) 0.0216(17) -0.0108(15) 0.0065(13) -0.0080(14) C48 0.0181(16) 0.0276(18) 0.0263(17) 0.0009(13) 0.0022(13) -0.0074(14) C49 0.0179(15) 0.0192(16) 0.0229(16) -0.0013(13) 0.0017(12) -0.0021(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 C2 . 2.047(3) ? Fe1 C3 . 2.059(3) ? Fe1 P1 . 2.1759(8) ? Fe1 P3 . 2.1909(8) ? Fe1 P2 . 2.2063(8) ? Fe1 C1 . 2.233(3) ? Fe1 C4 . 2.265(3) ? P1 C14 . 1.843(3) ? P1 C20 . 1.847(3) ? P1 C9 . 1.856(3) ? P2 C32 . 1.844(3) ? P2 C10 . 1.855(3) ? P2 C26 . 1.857(3) ? P3 C44 . 1.837(3) ? P3 C38 . 1.860(3) ? P3 C11 . 1.871(3) ? C1 C2 . 1.426(4) ? C1 C8 . 1.444(4) ? C1 H1 . 0.97(3) ? C2 C3 . 1.391(4) ? C2 H2 . 0.97(3) ? C3 C4 . 1.429(4) ? C3 H3 . 0.96(3) ? C4 C5 . 1.437(4) ? C4 H4 . 0.98(3) ? C5 C6 . 1.350(4) ? C5 H5 . 0.93 ? C6 C7 . 1.421(4) ? C6 H6 . 0.93 ? C7 C8 . 1.349(4) ? C7 H7 . 0.93 ? C8 H8 . 0.93 ? C9 C12 . 1.546(4) ? C9 H9A . 0.97 ? C9 H9B . 0.97 ? C10 C12 . 1.528(3) ? C10 H10A . 0.97 ? C10 H10B . 0.97 ? C11 C12 . 1.539(4) ? C11 H11A . 0.97 ? C11 H11B . 0.97 ? C12 C13 . 1.539(3) ? C13 H13A . 0.96 ? C13 H13B . 0.96 ? C13 H13C . 0.96 ? C14 C15 . 1.391(4) ? C14 C19 . 1.399(4) ? C15 C16 . 1.388(4) ? C15 H15 . 0.93 ? C16 C17 . 1.371(4) ? C16 H16 . 0.93 ? C17 C18 . 1.388(4) ? C17 H17 . 0.93 ? C18 C19 . 1.376(4) ? C18 H18 . 0.93 ? C19 H19 . 0.93 ? C20 C25 . 1.385(4) ? C20 C21 . 1.400(4) ? C21 C22 . 1.381(4) ? C21 H21 . 0.93 ? C22 C23 . 1.381(4) ? C22 H22 . 0.93 ? C23 C24 . 1.384(4) ? C23 H23 . 0.93 ? C24 C25 . 1.381(4) ? C24 H24 . 0.93 ? C25 H25 . 0.93 ? C26 C27 . 1.389(4) ? C26 C31 . 1.398(4) ? C27 C28 . 1.386(4) ? C27 H27 . 0.93 ? C28 C29 . 1.376(4) ? C28 H28 . 0.93 ? C29 C30 . 1.382(4) ? C29 H29 . 0.93 ? C30 C31 . 1.387(4) ? C30 H30 . 0.93 ? C31 H31 . 0.93 ? C32 C37 . 1.393(4) ? C32 C33 . 1.396(4) ? C33 C34 . 1.385(4) ? C33 H33 . 0.93 ? C34 C35 . 1.383(4) ? C34 H34 . 0.93 ? C35 C36 . 1.372(4) ? C35 H35 . 0.93 ? C36 C37 . 1.391(4) ? C36 H36 . 0.93 ? C37 H37 . 0.93 ? C38 C39 . 1.380(4) ? C38 C43 . 1.396(4) ? C39 C40 . 1.394(4) ? C39 H39 . 0.93 ? C40 C41 . 1.370(4) ? C40 H40 . 0.93 ? C41 C42 . 1.382(4) ? C41 H41 . 0.93 ? C42 C43 . 1.379(4) ? C42 H42 . 0.93 ? C43 H43 . 0.93 ? C44 C49 . 1.393(4) ? C44 C45 . 1.396(4) ? C45 C46 . 1.381(4) ? C45 H45 . 0.93 ? C46 C47 . 1.374(4) ? C46 H46 . 0.93 ? C47 C48 . 1.386(4) ? C47 H47 . 0.93 ? C48 C49 . 1.389(4) ? C48 H48 . 0.93 ? C49 H49 . 0.93 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 Fe1 C3 . . 39.60(11) ? C2 Fe1 P1 . . 92.60(8) ? C3 Fe1 P1 . . 117.32(8) ? C2 Fe1 P3 . . 136.39(8) ? C3 Fe1 P3 . . 148.89(8) ? P1 Fe1 P3 . . 91.93(3) ? C2 Fe1 P2 . . 130.47(8) ? C3 Fe1 P2 . . 97.89(8) ? P1 Fe1 P2 . . 88.44(3) ? P3 Fe1 P2 . . 92.99(3) ? C2 Fe1 C1 . . 38.60(10) ? C3 Fe1 C1 . . 71.22(11) ? P1 Fe1 C1 . . 94.20(7) ? P3 Fe1 C1 . . 97.81(7) ? P2 Fe1 C1 . . 168.79(7) ? C2 Fe1 C4 . . 70.94(11) ? C3 Fe1 C4 . . 38.23(10) ? P1 Fe1 C4 . . 153.94(8) ? P3 Fe1 C4 . . 113.98(8) ? P2 Fe1 C4 . . 87.50(8) ? C1 Fe1 C4 . . 85.35(10) ? C14 P1 C20 . . 95.05(12) ? C14 P1 C9 . . 101.62(12) ? C20 P1 C9 . . 102.53(12) ? C14 P1 Fe1 . . 120.19(9) ? C20 P1 Fe1 . . 120.01(9) ? C9 P1 Fe1 . . 113.99(9) ? C32 P2 C10 . . 102.90(12) ? C32 P2 C26 . . 97.39(12) ? C10 P2 C26 . . 96.04(12) ? C32 P2 Fe1 . . 116.87(9) ? C10 P2 Fe1 . . 113.35(9) ? C26 P2 Fe1 . . 126.20(9) ? C44 P3 C38 . . 97.05(12) ? C44 P3 C11 . . 104.37(12) ? C38 P3 C11 . . 95.06(12) ? C44 P3 Fe1 . . 116.46(9) ? C38 P3 Fe1 . . 126.60(9) ? C11 P3 Fe1 . . 113.37(9) ? C2 C1 C8 . . 132.1(3) ? C2 C1 Fe1 . . 63.61(15) ? C8 C1 Fe1 . . 122.58(19) ? C2 C1 H1 . . 112.1(16) ? C8 C1 H1 . . 106.6(16) ? Fe1 C1 H1 . . 114.4(16) ? C3 C2 C1 . . 125.4(3) ? C3 C2 Fe1 . . 70.68(16) ? C1 C2 Fe1 . . 77.79(16) ? C3 C2 H2 . . 118.7(16) ? C1 C2 H2 . . 115.4(16) ? Fe1 C2 H2 . . 119.3(16) ? C2 C3 C4 . . 125.6(3) ? C2 C3 Fe1 . . 69.72(15) ? C4 C3 Fe1 . . 78.71(16) ? C2 C3 H3 . . 117.1(17) ? C4 C3 H3 . . 116.9(17) ? Fe1 C3 H3 . . 120.1(16) ? C3 C4 C5 . . 133.4(3) ? C3 C4 Fe1 . . 63.06(15) ? C5 C4 Fe1 . . 119.69(19) ? C3 C4 H4 . . 111.7(16) ? C5 C4 H4 . . 107.4(16) ? Fe1 C4 H4 . . 115.5(16) ? C6 C5 C4 . . 136.2(3) ? C6 C5 H5 . . 111.9 ? C4 C5 H5 . . 111.9 ? C5 C6 C7 . . 130.1(3) ? C5 C6 H6 . . 115.0 ? C7 C6 H6 . . 115.0 ? C8 C7 C6 . . 130.8(3) ? C8 C7 H7 . . 114.6 ? C6 C7 H7 . . 114.6 ? C7 C8 C1 . . 135.3(3) ? C7 C8 H8 . . 112.4 ? C1 C8 H8 . . 112.4 ? C12 C9 P1 . . 117.76(18) ? C12 C9 H9A . . 107.9 ? P1 C9 H9A . . 107.9 ? C12 C9 H9B . . 107.9 ? P1 C9 H9B . . 107.9 ? H9A C9 H9B . . 107.2 ? C12 C10 P2 . . 117.04(18) ? C12 C10 H10A . . 108.0 ? P2 C10 H10A . . 108.0 ? C12 C10 H10B . . 108.0 ? P2 C10 H10B . . 108.0 ? H10A C10 H10B . . 107.3 ? C12 C11 P3 . . 117.58(18) ? C12 C11 H11A . . 107.9 ? P3 C11 H11A . . 107.9 ? C12 C11 H11B . . 107.9 ? P3 C11 H11B . . 107.9 ? H11A C11 H11B . . 107.2 ? C10 C12 C13 . . 107.2(2) ? C10 C12 C11 . . 110.7(2) ? C13 C12 C11 . . 107.4(2) ? C10 C12 C9 . . 112.7(2) ? C13 C12 C9 . . 107.6(2) ? C11 C12 C9 . . 111.0(2) ? C12 C13 H13A . . 109.5 ? C12 C13 H13B . . 109.5 ? H13A C13 H13B . . 109.5 ? C12 C13 H13C . . 109.5 ? H13A C13 H13C . . 109.5 ? H13B C13 H13C . . 109.5 ? C15 C14 C19 . . 118.5(3) ? C15 C14 P1 . . 121.6(2) ? C19 C14 P1 . . 119.8(2) ? C16 C15 C14 . . 120.9(3) ? C16 C15 H15 . . 119.5 ? C14 C15 H15 . . 119.5 ? C17 C16 C15 . . 119.8(3) ? C17 C16 H16 . . 120.1 ? C15 C16 H16 . . 120.1 ? C16 C17 C18 . . 120.0(3) ? C16 C17 H17 . . 120.0 ? C18 C17 H17 . . 120.0 ? C19 C18 C17 . . 120.4(3) ? C19 C18 H18 . . 119.8 ? C17 C18 H18 . . 119.8 ? C18 C19 C14 . . 120.3(3) ? C18 C19 H19 . . 119.8 ? C14 C19 H19 . . 119.8 ? C25 C20 C21 . . 117.8(3) ? C25 C20 P1 . . 123.4(2) ? C21 C20 P1 . . 118.7(2) ? C22 C21 C20 . . 121.1(3) ? C22 C21 H21 . . 119.5 ? C20 C21 H21 . . 119.5 ? C21 C22 C23 . . 120.2(3) ? C21 C22 H22 . . 119.9 ? C23 C22 H22 . . 119.9 ? C22 C23 C24 . . 119.4(3) ? C22 C23 H23 . . 120.3 ? C24 C23 H23 . . 120.3 ? C25 C24 C23 . . 120.3(3) ? C25 C24 H24 . . 119.8 ? C23 C24 H24 . . 119.8 ? C24 C25 C20 . . 121.2(3) ? C24 C25 H25 . . 119.4 ? C20 C25 H25 . . 119.4 ? C27 C26 C31 . . 118.2(3) ? C27 C26 P2 . . 122.1(2) ? C31 C26 P2 . . 119.2(2) ? C28 C27 C26 . . 120.3(3) ? C28 C27 H27 . . 119.8 ? C26 C27 H27 . . 119.8 ? C29 C28 C27 . . 121.2(3) ? C29 C28 H28 . . 119.4 ? C27 C28 H28 . . 119.4 ? C28 C29 C30 . . 119.1(3) ? C28 C29 H29 . . 120.4 ? C30 C29 H29 . . 120.4 ? C29 C30 C31 . . 120.3(3) ? C29 C30 H30 . . 119.9 ? C31 C30 H30 . . 119.9 ? C30 C31 C26 . . 120.8(3) ? C30 C31 H31 . . 119.6 ? C26 C31 H31 . . 119.6 ? C37 C32 C33 . . 117.7(3) ? C37 C32 P2 . . 123.6(2) ? C33 C32 P2 . . 118.7(2) ? C34 C33 C32 . . 121.0(3) ? C34 C33 H33 . . 119.5 ? C32 C33 H33 . . 119.5 ? C35 C34 C33 . . 120.0(3) ? C35 C34 H34 . . 120.0 ? C33 C34 H34 . . 120.0 ? C36 C35 C34 . . 120.2(3) ? C36 C35 H35 . . 119.9 ? C34 C35 H35 . . 119.9 ? C35 C36 C37 . . 119.8(3) ? C35 C36 H36 . . 120.1 ? C37 C36 H36 . . 120.1 ? C36 C37 C32 . . 121.3(3) ? C36 C37 H37 . . 119.3 ? C32 C37 H37 . . 119.3 ? C39 C38 C43 . . 117.6(3) ? C39 C38 P3 . . 123.9(2) ? C43 C38 P3 . . 118.1(2) ? C38 C39 C40 . . 121.1(3) ? C38 C39 H39 . . 119.5 ? C40 C39 H39 . . 119.5 ? C41 C40 C39 . . 120.4(3) ? C41 C40 H40 . . 119.8 ? C39 C40 H40 . . 119.8 ? C40 C41 C42 . . 119.5(3) ? C40 C41 H41 . . 120.3 ? C42 C41 H41 . . 120.3 ? C43 C42 C41 . . 120.0(3) ? C43 C42 H42 . . 120.0 ? C41 C42 H42 . . 120.0 ? C42 C43 C38 . . 121.4(3) ? C42 C43 H43 . . 119.3 ? C38 C43 H43 . . 119.3 ? C49 C44 C45 . . 118.0(3) ? C49 C44 P3 . . 125.3(2) ? C45 C44 P3 . . 116.6(2) ? C46 C45 C44 . . 120.7(3) ? C46 C45 H45 . . 119.6 ? C44 C45 H45 . . 119.6 ? C47 C46 C45 . . 120.7(3) ? C47 C46 H46 . . 119.6 ? C45 C46 H46 . . 119.6 ? C46 C47 C48 . . 119.7(3) ? C46 C47 H47 . . 120.1 ? C48 C47 H47 . . 120.1 ? C47 C48 C49 . . 119.7(3) ? C47 C48 H48 . . 120.1 ? C49 C48 H48 . . 120.1 ? C48 C49 C44 . . 121.1(3) ? C48 C49 H49 . . 119.4 ? C44 C49 H49 . . 119.4 ? _iucr_refine_instructions_details ; TITL apx1240a in P2(1)/c CELL 0.71073 18.8393 10.8349 18.7846 90.000 97.296 90.000 ZERR 4.00 0.0021 0.0012 0.0021 0.000 0.001 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H P Fe UNIT 196 188 12 4 L.S. 4 ACTA 50 BOND $H FMAP 2 PLAN 11 SIZE 0.06 0.16 0.24 WGHT 0.029600 2.266400 FVAR 0.10480 FE1 4 0.221004 0.837444 0.286880 11.00000 0.01278 0.01367 = 0.01348 0.00058 0.00039 0.00060 P1 3 0.188930 0.805266 0.392591 11.00000 0.01247 0.01448 = 0.01507 -0.00069 0.00148 0.00013 P2 3 0.256293 0.643343 0.286024 11.00000 0.01431 0.01372 = 0.01335 -0.00041 0.00140 -0.00046 P3 3 0.326879 0.903028 0.333222 11.00000 0.01357 0.01337 = 0.01578 0.00003 0.00107 -0.00006 C1 1 0.166986 1.020920 0.273086 11.00000 0.01592 0.01675 = 0.01464 0.00132 0.00178 0.00444 H1 2 0.153293 1.055501 0.316856 11.00000 -1.20000 C2 1 0.124747 0.916131 0.249252 11.00000 0.01196 0.01903 = 0.01727 0.00548 0.00086 0.00174 H2 2 0.083807 0.901150 0.274242 11.00000 -1.20000 C3 1 0.142398 0.828668 0.200212 11.00000 0.01593 0.01690 = 0.01788 0.00366 -0.00328 -0.00088 H3 2 0.112346 0.757409 0.193021 11.00000 -1.20000 C4 1 0.205602 0.829460 0.165405 11.00000 0.01892 0.02062 = 0.01396 -0.00282 -0.00282 0.00120 H4 2 0.214357 0.748947 0.144600 11.00000 -1.20000 C5 1 0.238636 0.921061 0.125150 11.00000 0.02679 0.02431 = 0.01569 -0.00093 0.00583 0.00169 AFIX 43 H5 2 0.267033 0.885616 0.093623 11.00000 -1.20000 AFIX 0 C6 1 0.238961 1.045529 0.121423 11.00000 0.02838 0.02662 = 0.01496 0.00627 0.00241 -0.00072 AFIX 43 H6 2 0.255314 1.077766 0.080602 11.00000 -1.20000 AFIX 0 C7 1 0.218221 1.134905 0.170126 11.00000 0.01929 0.01633 = 0.02089 0.00778 -0.00336 -0.00029 AFIX 43 H7 2 0.220961 1.216214 0.154849 11.00000 -1.20000 AFIX 0 C8 1 0.195226 1.121549 0.234805 11.00000 0.01793 0.01685 = 0.02220 0.00052 -0.00034 0.00278 AFIX 43 H8 2 0.198280 1.194582 0.261027 11.00000 -1.20000 AFIX 0 C9 1 0.255741 0.718310 0.454324 11.00000 0.01492 0.01612 = 0.01431 0.00273 0.00166 0.00236 AFIX 23 H9A 2 0.264800 0.764545 0.498768 11.00000 -1.20000 H9B 2 0.234183 0.640525 0.465492 11.00000 -1.20000 AFIX 0 C10 1 0.322185 0.601997 0.364326 11.00000 0.01564 0.01317 = 0.01746 0.00035 0.00366 -0.00039 AFIX 23 H10A 2 0.309911 0.520847 0.380831 11.00000 -1.20000 H10B 2 0.368870 0.595413 0.348019 11.00000 -1.20000 AFIX 0 C11 1 0.367402 0.809269 0.411661 11.00000 0.01274 0.01968 = 0.01754 0.00021 -0.00135 -0.00047 AFIX 23 H11A 2 0.415766 0.787736 0.403768 11.00000 -1.20000 H11B 2 0.371014 0.861436 0.453932 11.00000 -1.20000 AFIX 0 C12 1 0.328723 0.689675 0.428563 11.00000 0.01566 0.01359 = 0.01204 0.00045 0.00103 -0.00001 C13 1 0.375568 0.624906 0.490579 11.00000 0.01762 0.01719 = 0.01720 -0.00108 0.00050 0.00134 AFIX 137 H13A 2 0.351851 0.551582 0.503879 11.00000 -1.50000 H13B 2 0.383327 0.679546 0.531050 11.00000 -1.50000 H13C 2 0.420756 0.603179 0.475500 11.00000 -1.50000 AFIX 0 C14 1 0.106043 0.719677 0.401777 11.00000 0.01282 0.01110 = 0.02249 0.00108 0.00283 0.00114 C15 1 0.059310 0.683445 0.342143 11.00000 0.01668 0.01338 = 0.02539 0.00269 0.00285 0.00446 AFIX 43 H15 2 0.071922 0.695976 0.296405 11.00000 -1.20000 AFIX 0 C16 1 -0.005909 0.628829 0.349940 11.00000 0.01721 0.01580 = 0.03550 0.00132 -0.00243 -0.00048 AFIX 43 H16 2 -0.036949 0.605909 0.309615 11.00000 -1.20000 AFIX 0 C17 1 -0.024447 0.608763 0.417259 11.00000 0.01522 0.01538 = 0.04649 0.00372 0.00540 0.00176 AFIX 43 H17 2 -0.068171 0.572410 0.422621 11.00000 -1.20000 AFIX 0 C18 1 0.022037 0.642697 0.477413 11.00000 0.02483 0.01921 = 0.03242 0.00504 0.01501 0.00246 AFIX 43 H18 2 0.009365 0.628654 0.522986 11.00000 -1.20000 AFIX 0 C19 1 0.086710 0.696954 0.470044 11.00000 0.02011 0.02100 = 0.02164 0.00242 0.00474 0.00204 AFIX 43 H19 2 0.117724 0.718630 0.510640 11.00000 -1.20000 AFIX 0 C20 1 0.167595 0.937163 0.448448 11.00000 0.01752 0.01382 = 0.01463 -0.00012 0.00588 -0.00091 C21 1 0.099277 0.989711 0.435914 11.00000 0.01728 0.01954 = 0.02146 -0.00048 0.00379 0.00007 AFIX 43 H21 2 0.065701 0.956780 0.400419 11.00000 -1.20000 AFIX 0 C22 1 0.080911 1.089625 0.475375 11.00000 0.01975 0.02285 = 0.02833 0.00042 0.00409 0.00546 AFIX 43 H22 2 0.035369 1.123703 0.466083 11.00000 -1.20000 AFIX 0 C23 1 0.130003 1.139106 0.528622 11.00000 0.03401 0.02080 = 0.02575 -0.00667 0.00890 0.00735 AFIX 43 H23 2 0.117443 1.205395 0.555885 11.00000 -1.20000 AFIX 0 C24 1 0.198067 1.089098 0.541021 11.00000 0.03009 0.02341 = 0.02035 -0.00555 -0.00253 0.00484 AFIX 43 H24 2 0.231650 1.122863 0.576213 11.00000 -1.20000 AFIX 0 C25 1 0.216334 0.989315 0.501383 11.00000 0.01841 0.02128 = 0.01716 -0.00119 0.00053 0.00140 AFIX 43 H25 2 0.262213 0.956509 0.510390 11.00000 -1.20000 AFIX 0 C26 1 0.305275 0.569863 0.217434 11.00000 0.01421 0.01865 = 0.01432 -0.00224 -0.00252 -0.00029 C27 1 0.340713 0.638722 0.170490 11.00000 0.01421 0.02023 = 0.01789 -0.00348 -0.00267 0.00000 AFIX 43 H27 2 0.336369 0.724227 0.169650 11.00000 -1.20000 AFIX 0 C28 1 0.382516 0.580642 0.124891 11.00000 0.01672 0.03080 = 0.01981 0.00013 0.00414 -0.00417 AFIX 43 H28 2 0.406074 0.627924 0.093862 11.00000 -1.20000 AFIX 0 C29 1 0.389783 0.454247 0.124713 11.00000 0.01801 0.02835 = 0.02205 -0.00604 0.00228 0.00323 AFIX 43 H29 2 0.417304 0.416159 0.093305 11.00000 -1.20000 AFIX 0 C30 1 0.355633 0.384686 0.171840 11.00000 0.01706 0.01647 = 0.02807 -0.00422 0.00040 0.00065 AFIX 43 H30 2 0.360648 0.299290 0.172612 11.00000 -1.20000 AFIX 0 C31 1 0.313918 0.441699 0.217982 11.00000 0.01693 0.01570 = 0.02161 0.00114 0.00016 -0.00131 AFIX 43 H31 2 0.291412 0.394073 0.249687 11.00000 -1.20000 AFIX 0 C32 1 0.186659 0.524093 0.287677 11.00000 0.01576 0.01333 = 0.01931 -0.00274 0.00154 0.00219 C33 1 0.142637 0.496987 0.224089 11.00000 0.01632 0.01780 = 0.02310 -0.00121 0.00271 0.00191 AFIX 43 H33 2 0.150412 0.536528 0.181823 11.00000 -1.20000 AFIX 0 C34 1 0.087557 0.412076 0.223026 11.00000 0.01608 0.01866 = 0.03005 -0.00599 -0.00200 0.00321 AFIX 43 H34 2 0.058833 0.394661 0.180206 11.00000 -1.20000 AFIX 0 C35 1 0.075257 0.353169 0.285630 11.00000 0.01508 0.01493 = 0.03946 -0.00080 0.00552 -0.00067 AFIX 43 H35 2 0.037800 0.297102 0.284960 11.00000 -1.20000 AFIX 0 C36 1 0.118161 0.377227 0.348703 11.00000 0.02320 0.01668 = 0.02388 0.00230 0.00732 0.00105 AFIX 43 H36 2 0.110330 0.336591 0.390613 11.00000 -1.20000 AFIX 0 C37 1 0.173404 0.462594 0.349753 11.00000 0.01861 0.01564 = 0.02109 -0.00213 0.00343 0.00173 AFIX 43 H37 2 0.202070 0.478947 0.392760 11.00000 -1.20000 AFIX 0 C38 1 0.348079 1.054797 0.377047 11.00000 0.02037 0.01363 = 0.01639 0.00182 0.00389 -0.00164 C39 1 0.296966 1.137374 0.393896 11.00000 0.01957 0.01742 = 0.01803 0.00117 -0.00114 -0.00044 AFIX 43 H39 2 0.248968 1.122594 0.377854 11.00000 -1.20000 AFIX 0 C40 1 0.316133 1.242539 0.434562 11.00000 0.02527 0.01650 = 0.02770 -0.00129 0.00306 0.00530 AFIX 43 H40 2 0.280923 1.297143 0.445317 11.00000 -1.20000 AFIX 0 C41 1 0.386518 1.265981 0.458791 11.00000 0.03205 0.01311 = 0.02333 -0.00338 0.00246 -0.00446 AFIX 43 H41 2 0.399129 1.335611 0.486488 11.00000 -1.20000 AFIX 0 C42 1 0.438652 1.185302 0.441743 11.00000 0.01619 0.02154 = 0.02498 -0.00276 0.00040 -0.00609 AFIX 43 H42 2 0.486591 1.201004 0.457587 11.00000 -1.20000 AFIX 0 C43 1 0.419593 1.081517 0.401239 11.00000 0.01678 0.01888 = 0.02575 -0.00375 0.00419 0.00008 AFIX 43 H43 2 0.455137 1.028196 0.389798 11.00000 -1.20000 AFIX 0 C44 1 0.396273 0.907061 0.272802 11.00000 0.01255 0.01911 = 0.01468 -0.00350 -0.00215 -0.00396 C45 1 0.394325 1.006874 0.225635 11.00000 0.01915 0.02072 = 0.02120 -0.00264 0.00303 0.00108 AFIX 43 H45 2 0.360627 1.068998 0.227923 11.00000 -1.20000 AFIX 0 C46 1 0.441907 1.014392 0.175591 11.00000 0.02998 0.02522 = 0.02123 0.00253 0.00545 -0.00331 AFIX 43 H46 2 0.440181 1.081901 0.144845 11.00000 -1.20000 AFIX 0 C47 1 0.491753 0.923238 0.170739 11.00000 0.02231 0.03626 = 0.02158 -0.00802 0.00651 -0.01085 AFIX 43 H47 2 0.523554 0.929035 0.136854 11.00000 -1.20000 AFIX 0 C48 1 0.494451 0.822600 0.216549 11.00000 0.01808 0.02762 = 0.02634 -0.00737 0.00221 0.00094 AFIX 43 H48 2 0.527782 0.760217 0.213248 11.00000 -1.20000 AFIX 0 C49 1 0.447149 0.815333 0.267416 11.00000 0.01789 0.01920 = 0.02294 -0.00213 0.00171 -0.00132 AFIX 43 H49 2 0.449478 0.748099 0.298402 11.00000 -1.20000 AFIX 0 HKLF 4 REM apx1240a in P2(1)/c REM R1 = 0.0403 for 5100 Fo > 4sig(Fo) and 0.0656 for all 6995 data REM 491 parameters refined using 0 restraints END WGHT 0.0296 2.2669 REM Highest difference peak 0.386, deepest hole -0.348, 1-sigma level 0.071 Q1 1 0.1780 0.8445 0.3384 11.00000 0.05 0.39 Q2 1 0.1414 0.7325 0.3947 11.00000 0.05 0.36 Q3 1 0.2867 0.6247 0.3342 11.00000 0.05 0.34 Q4 1 0.2622 0.7833 0.3353 11.00000 0.05 0.33 Q5 1 0.2923 0.7315 0.4373 11.00000 0.05 0.31 Q6 1 0.2649 0.9219 0.2959 11.00000 0.05 0.30 Q7 1 0.2466 1.2355 0.1532 11.00000 0.05 0.30 Q8 1 0.1155 1.1456 0.4868 11.00000 0.05 0.30 Q9 1 0.2894 0.9339 0.5192 11.00000 0.05 0.29 Q10 1 0.0996 0.6586 0.3814 11.00000 0.05 0.29 Q11 1 0.2113 0.7400 0.2701 11.00000 0.05 0.29 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18.61 3.42 -20 3 11 23.59 3.96 20 -3 -11 14.74 3.08 -20 -3 11 20.67 3.55 20 3 -10 8.73 2.79 -20 3 10 9.89 2.95 20 3 -10 11.79 2.73 -20 3 10 7.83 2.38 -20 -3 10 13.46 2.96 20 -3 -10 8.52 2.41 20 3 -9 1.92 1.89 -20 3 9 4.46 1.98 -20 -3 9 5.20 2.10 20 -3 -9 3.18 1.77 -20 3 8 -2.53 1.32 20 3 -8 -0.73 1.56 -20 -3 8 0.04 1.41 20 -3 -8 1.76 1.69 -20 3 7 1.76 1.58 20 3 -7 0.90 1.66 20 -3 -7 -0.35 1.43 -20 -3 7 2.87 1.83 20 3 -6 2.69 1.89 -20 3 6 2.77 1.88 20 -3 -6 2.39 1.56 -20 -3 6 3.45 1.84 -20 3 5 7.25 2.27 20 3 -5 10.85 2.68 20 -3 -5 9.35 2.33 -20 -3 5 7.13 2.24 20 3 -4 2.42 1.78 -20 3 4 3.32 1.71 20 -3 -4 2.19 1.79 -20 -3 4 1.11 1.82 -20 3 3 15.53 2.86 20 3 -3 18.51 3.25 20 -3 -3 20.25 3.29 -20 -3 3 27.50 3.83 -20 3 2 3.65 1.82 20 3 -2 1.86 1.69 20 -3 -2 2.38 1.62 -20 -3 2 0.77 1.60 -20 3 1 0.95 1.55 20 3 -1 -0.30 1.51 20 -3 -1 2.09 1.64 -20 -3 1 3.67 1.98 20 3 0 -1.04 1.48 -20 3 0 -0.34 1.42 20 -3 0 -0.18 1.33 -20 -3 0 -0.36 1.52 20 3 1 3.98 2.05 -20 3 -1 4.90 1.99 -20 -3 -1 0.89 1.67 20 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0.75 1.49 20 4 -2 2.17 1.53 20 -4 -2 0.01 1.48 -20 -4 2 0.42 1.46 20 4 -1 4.11 1.99 -20 4 1 3.07 1.95 20 -4 -1 4.85 2.02 -20 -4 1 4.39 1.91 -20 4 0 16.79 3.03 20 4 0 11.68 2.85 -20 -4 0 16.41 3.09 20 -4 0 15.45 3.00 20 4 1 1.18 1.79 -20 4 -1 -2.02 1.24 20 -4 1 -0.83 1.47 -20 -4 -1 0.00 1.53 20 4 2 -0.45 1.54 -20 4 -2 -0.55 1.60 20 -4 2 -1.80 1.18 -20 -4 -2 -1.92 1.42 -20 4 -3 0.79 1.68 20 4 3 1.26 1.88 -20 -4 -3 0.28 1.72 20 -4 3 -1.19 1.38 20 4 4 2.36 1.93 -20 4 -4 0.85 1.56 20 -4 4 2.72 1.88 -20 -4 -4 0.31 1.74 -20 4 -5 19.08 3.44 20 4 5 17.12 3.37 20 -4 5 14.12 2.99 -20 -4 -5 20.89 3.54 20 -5 -8 -1.48 1.31 -20 -5 8 0.38 1.57 20 5 -7 1.44 2.00 -20 5 7 -1.37 1.55 -20 -5 7 1.43 1.94 20 -5 -7 0.97 1.77 -20 5 6 9.28 2.50 20 5 -6 12.78 2.90 20 -5 -6 7.26 2.41 -20 -5 6 9.59 2.59 20 5 -5 3.39 2.00 -20 5 5 2.35 1.78 -20 -5 5 2.36 1.86 20 -5 -5 0.68 1.62 20 5 -4 -0.66 1.54 -20 5 4 2.77 1.78 20 -5 -4 3.74 1.93 -20 -5 4 1.02 1.75 -20 5 3 1.72 1.72 20 5 -3 5.76 2.25 -20 -5 3 0.24 1.62 20 -5 -3 9.20 2.44 20 5 -2 11.08 2.70 -20 5 2 17.54 3.18 20 -5 -2 22.31 3.43 -20 5 1 1.07 1.53 20 5 -1 0.77 1.81 -20 -5 1 -1.75 1.50 20 -5 -1 -0.11 1.45 20 5 0 -0.43 1.76 -20 5 0 3.14 2.03 20 -5 0 1.51 1.54 -20 -5 0 3.23 1.95 -20 5 -1 0.76 1.76 20 5 1 -0.12 1.78 20 -5 1 1.48 1.70 -20 -5 -1 -0.21 1.52 -20 5 -2 0.80 1.65 20 5 2 2.99 2.09 20 -5 2 0.23 1.69 -20 -5 -2 1.24 1.87 20 5 3 6.68 2.35 -20 5 -3 10.09 2.71 -20 -5 -3 11.02 2.75 20 -5 3 5.64 2.27 20 -6 -5 8.12 2.47 -20 -6 5 7.28 2.41 -20 6 4 1.28 1.69 20 6 -4 3.56 2.17 20 -6 -4 2.11 1.78 -20 -6 4 2.14 1.99 -20 6 3 1.03 1.70 20 6 -3 4.16 2.14 -20 -6 3 2.85 1.93 20 -6 -3 0.75 1.66 20 6 -2 2.12 1.92 -20 6 2 0.01 1.68 -20 -6 2 0.40 1.58 20 -6 -2 1.49 1.71 -20 6 1 3.71 1.96 20 6 -1 0.89 1.90 -20 -6 1 1.47 1.97 20 -6 -1 0.19 1.51 20 6 0 1.53 2.04 -20 6 0 -0.19 1.69 -20 -6 0 2.85 2.13 20 -6 0 -0.62 1.58 -21 0 11 0.84 1.60 21 0 -11 3.32 2.14 21 0 -11 -0.26 2.14 21 0 -10 -0.24 1.55 -21 0 10 -1.41 1.29 -21 0 9 -0.43 1.35 21 0 -9 -0.60 1.68 -21 0 8 7.49 2.34 21 0 -8 13.44 2.96 -21 0 7 0.16 1.48 21 0 -7 -0.80 1.62 21 0 -6 2.03 1.82 -21 0 6 -0.41 1.35 -21 0 5 0.45 1.36 21 0 -5 1.68 1.67 -21 0 4 108.16 7.43 21 0 -4 104.85 7.46 -21 0 3 0.29 1.41 21 0 -3 2.33 1.76 -21 0 2 63.95 6.16 21 0 -2 75.70 6.58 21 0 -1 -2.41 1.23 -21 0 1 -0.26 1.37 21 0 0 4.66 2.08 -21 0 0 1.52 1.70 21 0 1 1.04 1.47 -21 0 -1 1.16 1.79 -21 0 -2 2.02 1.87 21 0 2 2.09 1.67 21 0 3 1.25 1.58 -21 0 -3 0.15 1.71 21 0 4 5.70 2.15 -21 0 -4 10.69 2.78 -21 0 -5 2.24 1.88 21 0 5 -1.00 1.30 -21 0 -6 1.78 1.92 -21 1 11 7.33 2.33 -21 1 11 6.65 2.57 21 1 -11 3.01 2.39 21 1 -11 4.70 2.24 -21 -1 11 7.75 2.40 21 -1 -11 5.48 2.32 21 1 -10 6.76 2.32 -21 1 10 1.65 1.76 21 -1 -10 1.36 1.89 -21 -1 10 5.73 2.17 -21 1 9 19.71 3.37 21 1 -9 15.11 3.22 -21 -1 9 17.71 3.24 21 -1 -9 18.56 3.36 -21 1 8 1.20 1.55 21 1 -8 -1.01 1.45 -21 -1 8 2.17 1.72 21 -1 -8 -0.58 1.59 -21 1 7 3.36 1.89 21 1 -7 5.03 2.20 21 -1 -7 -0.53 1.56 -21 -1 7 5.67 2.11 21 1 -6 18.41 3.31 -21 1 6 10.35 2.60 21 -1 -6 16.23 3.14 -21 -1 6 18.30 3.21 21 1 -5 1.84 1.86 -21 1 5 -0.43 1.33 -21 -1 5 2.46 1.64 21 -1 -5 5.47 2.12 21 1 -4 5.82 2.28 -21 1 4 7.07 2.30 21 -1 -4 7.87 2.35 -21 -1 4 4.25 1.90 21 1 -3 3.61 2.04 -21 1 3 2.39 1.77 21 -1 -3 4.19 1.99 -21 -1 3 0.16 1.65 -21 1 2 -0.12 1.41 21 1 -2 -1.02 1.16 -21 -1 2 0.47 1.55 21 -1 -2 1.39 1.46 -21 1 1 -0.07 1.60 21 1 -1 3.10 1.90 -21 -1 1 3.52 1.96 21 -1 -1 2.67 1.68 -21 1 0 4.53 2.16 21 1 0 -0.44 1.58 -21 -1 0 3.86 1.80 21 -1 0 2.17 1.80 -21 1 -1 -0.24 1.40 21 1 1 -1.71 1.25 -21 -1 -1 0.79 1.63 21 -1 1 -0.19 1.38 21 1 2 2.19 1.79 -21 1 -2 0.74 1.50 -21 -1 -2 1.92 1.86 21 -1 2 3.67 1.79 21 1 3 2.73 1.69 -21 1 -3 1.60 1.72 21 -1 3 2.12 1.82 -21 -1 -3 1.47 1.76 21 1 4 1.98 1.70 -21 1 -4 0.30 1.65 -21 -1 -4 0.91 1.98 21 -1 4 1.21 1.71 -21 1 -5 4.39 2.15 21 1 5 3.21 2.00 21 -1 5 1.74 1.73 -21 -1 -5 2.39 2.08 -21 2 10 2.21 1.73 21 2 -10 0.72 1.87 21 -2 -10 -1.37 1.57 -21 -2 10 -0.30 1.56 21 2 -9 -0.03 1.64 -21 2 9 -1.63 1.22 -21 -2 9 0.17 1.42 21 -2 -9 1.28 1.81 -21 2 8 1.34 1.73 21 2 -8 -1.53 1.60 -21 -2 8 2.43 1.83 21 -2 -8 1.21 1.72 21 2 -7 8.92 2.59 -21 2 7 4.97 2.05 21 -2 -7 7.44 2.42 -21 -2 7 7.88 2.39 21 2 -6 -0.69 1.63 -21 2 6 0.06 1.48 21 -2 -6 -0.52 1.26 -21 -2 6 -1.01 1.27 21 2 -5 7.08 2.23 -21 2 5 7.68 2.31 21 -2 -5 5.80 2.29 -21 -2 5 5.79 2.02 -21 2 4 0.37 1.50 21 2 -4 0.18 1.73 21 -2 -4 -0.25 1.34 -21 -2 4 0.66 1.65 -21 2 3 43.19 4.78 21 2 -3 47.45 5.03 -21 -2 3 34.77 4.47 21 -2 -3 43.12 4.97 -21 2 2 1.33 1.64 21 2 -2 0.82 1.74 21 -2 -2 1.94 1.63 -21 -2 2 0.81 1.68 -21 2 1 7.18 2.28 21 2 -1 7.27 2.44 21 -2 -1 10.30 2.54 -21 -2 1 6.75 2.40 -21 2 0 -0.32 1.51 21 2 0 2.95 1.80 21 -2 0 -0.49 1.39 -21 -2 0 -0.69 1.78 -21 2 -1 0.78 1.47 21 2 1 2.25 1.81 -21 -2 -1 0.50 1.57 21 -2 1 0.54 1.61 21 2 2 11.41 2.58 -21 2 -2 6.67 2.34 -21 -2 -2 6.86 2.61 21 -2 2 7.33 2.39 -21 2 -3 3.16 1.86 21 2 3 6.48 2.31 21 -2 3 2.85 1.90 -21 -2 -3 5.00 2.28 21 2 4 1.79 1.87 -21 2 -4 3.20 1.95 21 -2 4 1.26 1.69 -21 -2 -4 -0.59 1.89 21 2 5 -2.38 1.03 -21 2 -5 1.45 1.85 -21 -2 -5 -1.10 1.70 21 -2 5 3.00 1.91 21 3 -9 3.32 2.16 -21 3 9 0.47 1.69 21 -3 -9 -0.75 1.62 -21 -3 9 0.49 1.54 21 3 -8 4.60 2.20 -21 3 8 4.96 2.01 21 -3 -8 4.17 2.05 -21 -3 8 5.35 2.23 21 3 -7 0.65 1.76 -21 3 7 4.32 2.00 -21 -3 7 3.01 1.97 21 -3 -7 4.75 2.07 21 3 -6 1.27 1.83 -21 3 6 1.54 1.54 21 -3 -6 2.01 1.58 -21 -3 6 0.45 1.60 21 3 -5 1.90 1.87 -21 3 5 2.38 1.78 -21 -3 5 1.18 1.71 21 -3 -5 0.97 1.66 -21 3 4 -0.39 1.45 21 3 -4 0.48 1.63 21 -3 -4 2.10 1.71 -21 -3 4 1.15 1.86 21 3 -3 10.27 2.61 -21 3 3 10.21 2.49 21 -3 -3 6.46 2.25 -21 -3 3 11.26 2.71 21 3 -2 -0.63 1.57 -21 3 2 0.43 1.44 21 -3 -2 0.16 1.34 -21 -3 2 1.70 1.72 -21 3 1 24.17 3.79 21 3 -1 27.72 4.02 21 -3 -1 43.74 4.77 -21 -3 1 26.43 4.02 21 3 0 1.59 1.86 -21 3 0 2.80 1.78 -21 -3 0 -0.82 1.67 21 -3 0 0.25 1.41 -21 3 -1 7.22 2.39 21 3 1 7.82 2.45 21 -3 1 8.01 2.39 -21 -3 -1 7.07 2.39 -21 3 -2 -1.03 1.46 21 3 2 0.69 1.58 21 -3 2 -1.59 1.32 -21 -3 -2 1.61 1.89 -21 3 -3 1.47 1.79 21 3 3 -1.04 1.32 -21 -3 -3 0.55 1.84 21 -3 3 1.85 1.86 21 3 4 9.31 2.67 -21 3 -4 12.04 3.00 21 -3 4 10.27 2.68 -21 -3 -4 12.04 2.82 -21 4 7 8.66 2.53 21 4 -7 12.87 2.91 -21 -4 7 7.98 2.41 21 -4 -7 9.39 2.66 21 4 -6 4.63 2.34 -21 4 6 2.80 2.10 -21 -4 6 2.15 1.73 21 -4 -6 6.59 2.34 -21 4 5 4.45 2.00 21 4 -5 5.20 2.28 -21 -4 5 1.71 1.87 21 -4 -5 9.40 2.60 21 4 -4 5.12 2.28 -21 4 4 7.60 2.33 -21 -4 4 5.17 2.12 21 -4 -4 2.64 1.71 -21 4 3 15.86 3.08 21 4 -3 15.99 3.19 21 -4 -3 17.55 3.16 -21 -4 3 11.29 2.89 -21 4 2 14.81 2.97 21 4 -2 14.36 3.03 21 -4 -2 9.93 2.53 -21 -4 2 13.76 3.10 21 4 -1 3.96 2.16 -21 4 1 6.28 2.14 -21 -4 1 5.65 2.33 21 -4 -1 4.01 1.96 -21 4 0 5.23 2.07 21 4 0 6.81 2.39 21 -4 0 1.15 1.83 -21 -4 0 9.01 2.62 -21 4 -1 0.05 1.52 21 4 1 0.71 1.75 21 -4 1 1.76 1.88 -21 -4 -1 0.27 1.81 -21 4 -2 -1.22 1.65 21 4 2 0.68 1.87 21 -4 2 1.90 1.88 -21 -4 -2 0.61 1.76 21 5 -3 2.22 1.99 -21 5 3 1.61 1.78 21 -5 -3 3.58 1.99 -21 -5 3 -0.85 1.61 -21 5 2 2.10 1.81 21 -5 -2 3.02 2.14 -21 -5 2 2.82 2.13 22 0 -8 13.40 3.00 -22 0 8 10.56 2.81 22 0 -7 2.69 1.92 -22 0 7 -0.07 1.42 -22 0 6 21.65 3.55 22 0 -6 22.09 3.65 22 0 -5 0.58 1.72 -22 0 5 1.55 1.79 22 0 -4 2.84 1.82 -22 0 4 1.22 1.77 22 0 -3 0.02 1.62 -22 0 3 -0.47 1.42 22 0 -2 22.81 3.60 -22 0 2 10.17 2.62 -22 0 1 0.75 1.68 22 0 -1 -0.64 1.43 -22 0 0 2.02 1.86 22 0 0 -0.26 1.32 -22 0 -1 0.96 1.79 22 0 1 0.66 1.64 -22 0 -2 1.45 1.94 22 0 2 -0.96 1.48 -22 1 8 -0.80 1.54 22 1 -8 -1.51 1.63 22 -1 -8 2.43 1.94 -22 -1 8 -0.77 1.50 -22 1 7 9.31 2.55 22 1 -7 10.22 2.89 22 -1 -7 9.45 2.57 -22 -1 7 10.87 2.68 22 1 -6 -0.84 1.82 -22 1 6 0.87 1.82 22 -1 -6 0.62 1.81 -22 -1 6 3.53 1.84 22 1 -5 30.88 4.37 -22 1 5 32.83 4.31 -22 -1 5 31.11 4.26 22 -1 -5 31.08 4.37 22 1 -4 56.24 5.74 -22 1 4 48.08 5.36 22 -1 -4 56.22 5.72 -22 -1 4 51.57 5.59 -22 1 3 1.63 1.73 22 1 -3 3.80 2.15 -22 -1 3 5.06 2.07 22 -1 -3 10.38 2.58 -22 1 2 50.27 5.47 22 1 -2 47.39 5.30 -22 -1 2 45.81 5.20 22 -1 -2 49.86 5.36 22 1 -1 0.06 1.52 -22 1 1 0.72 1.55 22 -1 -1 -0.24 1.60 -22 -1 1 0.86 1.50 22 1 0 3.12 1.87 -22 1 0 1.91 1.91 22 -1 0 2.34 1.86 -22 -1 0 0.62 1.67 -22 1 -1 -1.52 1.44 22 1 1 -1.15 1.64 -22 -1 -1 -1.22 1.56 22 -1 1 0.96 1.62 -22 1 -2 -1.83 1.57 22 1 2 -1.63 1.44 -22 -1 -2 -0.72 1.60 22 -1 2 -0.50 1.61 22 2 -7 1.65 2.04 -22 2 7 1.85 1.98 -22 -2 7 -0.11 1.46 22 -2 -7 2.06 1.76 -22 2 6 9.69 2.57 22 2 -6 6.32 2.46 22 -2 -6 6.32 2.33 -22 -2 6 4.80 2.13 22 2 -5 1.70 2.01 -22 2 5 -1.30 1.40 22 -2 -5 0.87 1.79 -22 -2 5 -0.83 1.46 22 2 -4 11.48 2.89 -22 2 4 9.01 2.60 22 -2 -4 10.24 2.62 -22 -2 4 11.65 2.77 -22 2 3 2.11 1.98 22 2 -3 7.33 2.52 -22 -2 3 7.48 2.53 22 -2 -3 7.84 2.49 -22 2 2 -0.52 1.47 22 2 -2 -0.05 1.66 22 -2 -2 0.82 1.79 -22 -2 2 3.07 1.98 22 2 -1 29.78 4.25 -22 2 1 34.68 4.47 -22 -2 1 30.53 4.33 22 -2 -1 37.38 4.66 -22 2 0 1.21 1.74 22 2 0 -1.27 1.63 22 -2 0 0.73 1.59 -22 -2 0 0.28 1.80 -22 2 -1 14.78 3.12 22 2 1 24.11 3.73 -22 -2 -1 9.57 2.76 22 -2 1 16.28 3.21 22 3 -5 6.64 2.33 -22 3 5 6.12 2.34 -22 -3 5 4.56 2.04 22 -3 -5 4.80 2.14 -22 3 4 10.62 2.83 22 3 -4 9.52 2.68 -22 -3 4 11.78 2.83 22 -3 -4 7.63 2.49 -22 3 3 3.33 2.01 22 3 -3 2.26 1.92 -22 -3 3 1.26 1.87 22 -3 -3 4.43 2.03 22 3 -2 -0.68 1.52 -22 3 2 0.72 1.69 -22 -3 2 -2.12 1.56 22 -3 -2 1.41 1.68 22 3 -1 0.77 2.00 -22 3 1 2.28 1.99 -22 -3 1 3.04 2.02 22 -3 -1 2.65 2.00 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 44942 data_Triphos2Fe _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C68 H66 Fe P6' _chemical_formula_sum 'C68 H66 Fe P6' _chemical_formula_iupac ? _chemical_formula_weight 1124.87 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.8705(5) _cell_length_b 28.4738(13) _cell_length_c 20.7566(10) _cell_angle_alpha 90 _cell_angle_beta 93.4300(10) _cell_angle_gamma 90 _cell_volume 5823.2(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4185 _cell_measurement_theta_min 2.3468 _cell_measurement_theta_max 22.1414 _cell_measurement_temperature 293.(2) _exptl_crystal_description needle _exptl_crystal_colour 'clear dark red' _exptl_crystal_size_max 0.279 _exptl_crystal_size_mid 0.114 _exptl_crystal_size_min 0.088 _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 0.465 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.96 _exptl_special_details ; ; _diffrn_ambient_temperature 293.(2) _diffrn_source ? _diffrn_source_type 'sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.3330 _diffrn_reflns_number 48641 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.34 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _refine_special_details ; ; _reflns_number_total 10651 _reflns_number_gt 6978 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_gt 0.0889 _refine_ls_wR_factor_ref 0.1027 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_number_reflns 10651 _refine_ls_number_parameters 676 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.9885P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.332 _refine_diff_density_min -0.308 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Instrument Service v2010.9.0.0' _computing_cell_refinement 'SAINT V8.32B (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.32B (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'XShell ver. 6.3.1 (Bruker AXS, 2004)' _computing_publication_material 'Bruker APEX2 v1013.6-2 (Bruker-AXS, 2013)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe1 0.44751(4) 0.38030(2) 0.70440(2) 0.02807(11) Uani d . . . 1 . . P P1 0.28521(7) 0.32674(3) 0.69723(4) 0.03173(18) Uani d . . . 1 . . P P2 0.61082(7) 0.43382(3) 0.70862(4) 0.03470(19) Uani d . . . 1 . . P P3 0.32911(7) 0.40838(3) 0.78312(4) 0.03378(19) Uani d . . . 1 . . P P4 0.62272(7) 0.33154(3) 0.70924(4) 0.03242(18) Uani d . . . 1 . . P P5 0.38182(7) 0.41397(3) 0.61289(4) 0.03373(19) Uani d . . . 1 . . P P6 0.21371(9) 0.55656(3) 0.82866(5) 0.0523(2) Uani d . . . 1 . . C C1 0.2279(3) 0.29658(10) 0.62206(14) 0.0348(7) Uani d . . . 1 . . C C2 0.3242(3) 0.27666(11) 0.58518(15) 0.0485(8) Uani d . . . 1 . . H H2 0.415 0.2778 0.5999 0.058 Uiso calc U . R 1 . . C C3 0.2896(3) 0.25503(13) 0.52683(17) 0.0593(10) Uani d . . . 1 . . H H3 0.3567 0.2416 0.5032 0.071 Uiso calc U . R 1 . . C C4 0.1560(4) 0.25342(13) 0.50376(16) 0.0613(10) Uani d . . . 1 . . H H4 0.1325 0.2401 0.4637 0.074 Uiso calc U . R 1 . . C C5 0.0589(3) 0.27158(13) 0.54041(18) 0.0644(11) Uani d . . . 1 . . H H5 -0.0319 0.2697 0.5258 0.077 Uiso calc U . R 1 . . C C6 0.0934(3) 0.29273(12) 0.59913(16) 0.0540(9) Uani d . . . 1 . . H H6 0.0253 0.3046 0.6236 0.065 Uiso calc U . R 1 . . C C7 0.2875(3) 0.27565(10) 0.75255(15) 0.0407(8) Uani d . . . 1 . . C C8 0.3696(3) 0.27666(12) 0.80905(15) 0.0475(8) Uani d . . . 1 . . H H8 0.4264 0.3023 0.8176 0.057 Uiso calc U . R 1 . . C C9 0.3685(4) 0.24010(14) 0.85290(18) 0.0668(11) Uani d . . . 1 . . H H9 0.4242 0.2412 0.8906 0.08 Uiso calc U . R 1 . . C C10 0.2854(5) 0.20227(15) 0.8408(2) 0.0857(14) Uani d . . . 1 . . H H10 0.2842 0.1777 0.8703 0.103 Uiso calc U . R 1 . . C C11 0.2044(5) 0.20063(14) 0.7855(2) 0.0893(14) Uani d . . . 1 . . H H11 0.1479 0.1749 0.7773 0.107 Uiso calc U . R 1 . . C C12 0.2055(4) 0.23676(12) 0.74143(18) 0.0638(10) Uani d . . . 1 . . H H12 0.1502 0.235 0.7036 0.077 Uiso calc U . R 1 . . C C13 0.1274(3) 0.35404(10) 0.72229(14) 0.0381(7) Uani d . . . 1 . . H H13A 0.0938 0.3767 0.6903 0.046 Uiso calc U . R 1 . . H H13B 0.0582 0.3303 0.7271 0.046 Uiso calc U . R 1 . . C C14 0.1623(3) 0.37829(11) 0.78667(15) 0.0438(8) Uani d . . . 1 . . H H14A 0.1667 0.3553 0.8212 0.053 Uiso calc U . R 1 . . H H14B 0.0925 0.401 0.7954 0.053 Uiso calc U . R 1 . . C C15 0.3861(3) 0.40921(11) 0.87004(14) 0.0373(7) Uani d . . . 1 . . C C16 0.4643(3) 0.44644(12) 0.89442(16) 0.0500(9) Uani d . . . 1 . . H H16 0.4801 0.4718 0.8676 0.06 Uiso calc U . R 1 . . C C17 0.5195(4) 0.44700(14) 0.95741(18) 0.0646(10) Uani d . . . 1 . . H H17 0.5729 0.4722 0.9718 0.077 Uiso calc U . R 1 . . C C18 0.4963(4) 0.41095(15) 0.99848(18) 0.0682(11) Uani d . . . 1 . . H H18 0.5328 0.4115 1.0408 0.082 Uiso calc U . R 1 . . C C19 0.4184(4) 0.37392(14) 0.97644(17) 0.0646(10) Uani d . . . 1 . . H H19 0.4009 0.3493 1.0042 0.078 Uiso calc U . R 1 . . C C20 0.3650(3) 0.37261(12) 0.91269(16) 0.0524(9) Uani d . . . 1 . . H H20 0.3141 0.3467 0.8984 0.063 Uiso calc U . R 1 . . C C21 0.2708(3) 0.47018(11) 0.77562(15) 0.0451(8) Uani d . . . 1 . . H H21A 0.3506 0.4895 0.7715 0.054 Uiso calc U . R 1 . . H H21B 0.2166 0.4728 0.7352 0.054 Uiso calc U . R 1 . . C C22 0.1883(3) 0.49232(11) 0.82845(16) 0.0498(9) Uani d . . . 1 . . H H22A 0.2177 0.4794 0.8702 0.06 Uiso calc U . R 1 . . H H22B 0.0927 0.4852 0.8202 0.06 Uiso calc U . R 1 . . C C23 0.1155(3) 0.57350(11) 0.75484(17) 0.0499(9) Uani d . . . 1 . . C C24 -0.0187(4) 0.56135(13) 0.7414(2) 0.0662(11) Uani d . . . 1 . . H H24 -0.062 0.5427 0.7708 0.079 Uiso calc U . R 1 . . C C25 -0.0903(4) 0.57587(14) 0.6862(2) 0.0726(11) Uani d . . . 1 . . H H25 -0.1811 0.5676 0.6789 0.087 Uiso calc U . R 1 . . C C26 -0.0292(5) 0.60192(18) 0.6430(2) 0.0902(15) Uani d . . . 1 . . H H26 -0.077 0.6114 0.6052 0.108 Uiso calc U . R 1 . . C C27 0.1031(6) 0.6146(2) 0.6542(3) 0.138(2) Uani d . . . 1 . . H H27 0.1452 0.6331 0.6242 0.165 Uiso calc U . R 1 . . C C28 0.1755(4) 0.60020(18) 0.7102(2) 0.0995(16) Uani d . . . 1 . . H H28 0.266 0.6089 0.7172 0.119 Uiso calc U . R 1 . . C C29 0.1031(3) 0.57677(12) 0.89057(18) 0.0521(9) Uani d . . . 1 . . C C30 0.0300(4) 0.61826(13) 0.8828(2) 0.0709(11) Uani d . . . 1 . . H H30 0.0309 0.6345 0.844 0.085 Uiso calc U . R 1 . . C C31 -0.0441(4) 0.63571(17) 0.9319(3) 0.0889(15) Uani d . . . 1 . . H H31 -0.092 0.6636 0.9259 0.107 Uiso calc U . R 1 . . C C32 -0.0476(5) 0.6125(2) 0.9890(3) 0.0954(17) Uani d . . . 1 . . H H32 -0.0983 0.6243 1.0218 0.114 Uiso calc U . R 1 . . C C33 0.0236(5) 0.5718(2) 0.9979(2) 0.0996(16) Uani d . . . 1 . . H H33 0.0218 0.5559 1.0369 0.12 Uiso calc U . R 1 . . C C34 0.0990(4) 0.55396(15) 0.9489(2) 0.0748(12) Uani d . . . 1 . . H H34 0.1474 0.5262 0.9557 0.09 Uiso calc U . R 1 . . C C35 0.6489(3) 0.48071(11) 0.76845(16) 0.0439(8) Uani d . . . 1 . . C C36 0.5939(3) 0.52538(12) 0.76004(17) 0.0541(9) Uani d . . . 1 . . H H36 0.5381 0.5319 0.7235 0.065 Uiso calc U . R 1 . . C C37 0.6214(4) 0.56057(14) 0.8057(2) 0.0790(13) Uani d . . . 1 . . H H37 0.5832 0.5902 0.7994 0.095 Uiso calc U . R 1 . . C C38 0.7042(4) 0.55189(18) 0.8599(2) 0.0875(15) Uani d . . . 1 . . H H38 0.7229 0.5755 0.8901 0.105 Uiso calc U . R 1 . . C C39 0.7587(4) 0.50830(18) 0.8688(2) 0.0804(13) Uani d . . . 1 . . H H39 0.815 0.5022 0.9054 0.096 Uiso calc U . R 1 . . C C40 0.7314(3) 0.47297(13) 0.82424(17) 0.0594(10) Uani d . . . 1 . . H H40 0.769 0.4434 0.8317 0.071 Uiso calc U . R 1 . . C C41 0.7831(3) 0.40829(10) 0.70653(15) 0.0427(8) Uani d . . . 1 . . H H41A 0.8411 0.4287 0.6829 0.051 Uiso calc U . R 1 . . H H41B 0.8232 0.4045 0.75 0.051 Uiso calc U . R 1 . . C C42 0.7680(3) 0.36113(11) 0.67340(15) 0.0410(8) Uani d . . . 1 . . H H42A 0.8501 0.3427 0.6807 0.049 Uiso calc U . R 1 . . H H42B 0.7501 0.3652 0.6273 0.049 Uiso calc U . R 1 . . C C43 0.7143(3) 0.31691(10) 0.78803(15) 0.0383(7) Uani d . . . 1 . . C C44 0.6835(3) 0.34186(11) 0.84214(15) 0.0456(8) Uani d . . . 1 . . H H44 0.6125 0.3634 0.8393 0.055 Uiso calc U . R 1 . . C C45 0.7568(4) 0.33552(13) 0.90116(17) 0.0625(10) Uani d . . . 1 . . H H45 0.7347 0.3527 0.9371 0.075 Uiso calc U . R 1 . . C C46 0.8613(4) 0.30379(14) 0.90579(18) 0.0690(11) Uani d . . . 1 . . H H46 0.9106 0.2995 0.9449 0.083 Uiso calc U . R 1 . . C C47 0.8935(4) 0.27823(14) 0.85239(19) 0.0694(11) Uani d . . . 1 . . H H47 0.9638 0.2565 0.8557 0.083 Uiso calc U . R 1 . . C C48 0.8212(3) 0.28486(12) 0.79398(17) 0.0539(9) Uani d . . . 1 . . H H48 0.8442 0.2677 0.7581 0.065 Uiso calc U . R 1 . . C C49 0.6365(3) 0.27253(10) 0.67168(15) 0.0389(7) Uani d . . . 1 . . C C50 0.5838(3) 0.23374(11) 0.70105(18) 0.0559(9) Uani d . . . 1 . . H H50 0.5445 0.2371 0.7404 0.067 Uiso calc U . R 1 . . C C51 0.5889(4) 0.18971(13) 0.6725(2) 0.0760(12) Uani d . . . 1 . . H H51 0.5513 0.164 0.6925 0.091 Uiso calc U . R 1 . . C C52 0.6483(4) 0.18399(16) 0.6156(3) 0.0845(14) Uani d . . . 1 . . H H52 0.652 0.1544 0.597 0.101 Uiso calc U . R 1 . . C C53 0.7021(4) 0.22158(16) 0.5860(2) 0.0757(12) Uani d . . . 1 . . H H53 0.7422 0.2177 0.5469 0.091 Uiso calc U . R 1 . . C C54 0.6976(3) 0.26569(12) 0.61390(16) 0.0529(9) Uani d . . . 1 . . H H54 0.7361 0.2911 0.5936 0.063 Uiso calc U . R 1 . . C C55 0.6025(3) 0.46859(11) 0.63295(14) 0.0431(8) Uani d . . . 1 . . H H55A 0.6431 0.4992 0.6407 0.052 Uiso calc U . R 1 . . H H55B 0.652 0.4527 0.6004 0.052 Uiso calc U . R 1 . . C C56 0.4542(3) 0.47392(10) 0.60983(15) 0.0436(8) Uani d . . . 1 . . H H56A 0.4462 0.4862 0.5662 0.052 Uiso calc U . R 1 . . H H56B 0.4077 0.495 0.6378 0.052 Uiso calc U . R 1 . . C C57 0.2038(3) 0.42639(11) 0.58417(14) 0.0383(7) Uani d . . . 1 . . C C58 0.1325(3) 0.39414(12) 0.54489(15) 0.0505(9) Uani d . . . 1 . . H H58 0.177 0.3675 0.5312 0.061 Uiso calc U . R 1 . . C C59 -0.0029(3) 0.40062(14) 0.52565(16) 0.0595(10) Uani d . . . 1 . . H H59 -0.049 0.3779 0.5007 0.071 Uiso calc U . R 1 . . C C60 -0.0685(4) 0.44008(16) 0.54308(18) 0.0682(11) Uani d . . . 1 . . H H60 -0.1589 0.4448 0.5294 0.082 Uiso calc U . R 1 . . C C61 -0.0008(4) 0.47312(15) 0.58101(18) 0.0658(11) Uani d . . . 1 . . H H61 -0.0459 0.5002 0.5929 0.079 Uiso calc U . R 1 . . C C62 0.1343(3) 0.46647(12) 0.60175(15) 0.0517(9) Uani d . . . 1 . . H H62 0.1787 0.489 0.6276 0.062 Uiso calc U . R 1 . . C C63 0.4415(3) 0.39450(10) 0.53353(14) 0.0377(7) Uani d . . . 1 . . C C64 0.5294(3) 0.35711(12) 0.53143(16) 0.0508(9) Uani d . . . 1 . . H H64 0.5527 0.341 0.5695 0.061 Uiso calc U . R 1 . . C C65 0.5849(4) 0.34236(14) 0.47486(18) 0.0649(10) Uani d . . . 1 . . H H65 0.644 0.3169 0.4753 0.078 Uiso calc U . R 1 . . C C66 0.5518(4) 0.36579(14) 0.41823(18) 0.0650(10) Uani d . . . 1 . . H H66 0.5884 0.3565 0.38 0.078 Uiso calc U . R 1 . . C C67 0.4638(4) 0.40302(13) 0.41901(16) 0.0626(10) Uani d . . . 1 . . H H67 0.4407 0.419 0.3808 0.075 Uiso calc U . R 1 . . C C68 0.4092(4) 0.41711(12) 0.47500(16) 0.0534(9) Uani d . . . 1 . . H H68 0.3493 0.4423 0.474 0.064 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.0207(2) 0.0305(2) 0.0329(2) -0.00056(17) 0.00060(16) 0.00103(19) P1 0.0239(4) 0.0343(4) 0.0367(4) -0.0025(3) -0.0006(3) 0.0015(3) P2 0.0269(4) 0.0350(4) 0.0422(5) -0.0037(3) 0.0014(3) -0.0002(4) P3 0.0257(4) 0.0380(4) 0.0377(4) 0.0003(3) 0.0027(3) -0.0018(4) P4 0.0239(4) 0.0350(4) 0.0380(5) 0.0028(3) -0.0005(3) -0.0001(3) P5 0.0305(4) 0.0343(4) 0.0362(4) 0.0004(3) 0.0002(3) 0.0037(4) P6 0.0399(5) 0.0499(6) 0.0673(6) 0.0056(4) 0.0054(5) -0.0093(5) C1 0.0281(16) 0.0345(17) 0.0419(18) -0.0064(13) 0.0014(14) -0.0019(14) C2 0.0367(18) 0.064(2) 0.044(2) -0.0009(16) -0.0071(15) -0.0045(17) C3 0.047(2) 0.079(3) 0.053(2) 0.0011(19) 0.0029(18) -0.018(2) C4 0.061(2) 0.079(3) 0.042(2) -0.019(2) -0.0060(19) -0.0151(19) C5 0.036(2) 0.087(3) 0.068(3) -0.0138(19) -0.0080(19) -0.019(2) C6 0.0326(18) 0.070(2) 0.060(2) -0.0057(17) 0.0002(16) -0.0186(19) C7 0.0337(17) 0.0419(19) 0.047(2) -0.0006(14) 0.0024(15) 0.0077(15) C8 0.0436(19) 0.054(2) 0.045(2) -0.0025(16) 0.0028(16) 0.0050(17) C9 0.074(3) 0.073(3) 0.053(2) 0.010(2) 0.002(2) 0.024(2) C10 0.102(4) 0.064(3) 0.093(4) 0.000(3) 0.014(3) 0.043(3) C11 0.105(4) 0.063(3) 0.098(4) -0.027(3) -0.012(3) 0.033(3) C12 0.070(3) 0.049(2) 0.070(3) -0.0186(19) -0.011(2) 0.0163(19) C13 0.0232(15) 0.0446(19) 0.0463(19) -0.0035(13) -0.0001(13) 0.0030(15) C14 0.0279(16) 0.055(2) 0.050(2) -0.0038(15) 0.0085(14) -0.0063(16) C15 0.0327(16) 0.0428(18) 0.0370(17) 0.0064(14) 0.0056(13) -0.0034(15) C16 0.046(2) 0.057(2) 0.047(2) 0.0001(17) 0.0034(16) -0.0028(17) C17 0.064(2) 0.075(3) 0.054(2) -0.004(2) -0.008(2) -0.016(2) C18 0.070(3) 0.095(3) 0.038(2) 0.011(2) -0.0083(19) -0.005(2) C19 0.077(3) 0.072(3) 0.045(2) 0.007(2) 0.005(2) 0.011(2) C20 0.054(2) 0.058(2) 0.046(2) 0.0017(17) 0.0047(17) -0.0018(17) C21 0.0403(18) 0.048(2) 0.048(2) 0.0095(15) 0.0062(15) 0.0008(16) C22 0.047(2) 0.048(2) 0.055(2) 0.0125(16) 0.0114(17) -0.0014(17) C23 0.044(2) 0.047(2) 0.060(2) 0.0070(16) 0.0093(17) -0.0060(17) C24 0.059(2) 0.063(3) 0.077(3) 0.002(2) 0.000(2) 0.008(2) C25 0.066(3) 0.077(3) 0.074(3) 0.008(2) -0.004(2) -0.009(2) C26 0.081(3) 0.133(4) 0.057(3) 0.027(3) 0.006(3) 0.003(3) C27 0.089(4) 0.237(7) 0.087(4) -0.016(4) 0.012(3) 0.072(4) C28 0.059(3) 0.160(5) 0.081(3) -0.014(3) 0.014(2) 0.038(3) C29 0.0401(19) 0.053(2) 0.063(2) 0.0000(17) -0.0017(17) -0.0206(19) C30 0.064(3) 0.062(3) 0.088(3) 0.007(2) 0.008(2) -0.021(2) C31 0.069(3) 0.087(3) 0.111(4) 0.013(3) 0.008(3) -0.050(3) C32 0.068(3) 0.133(5) 0.086(4) -0.005(3) 0.016(3) -0.065(4) C33 0.107(4) 0.130(5) 0.062(3) 0.006(4) 0.012(3) -0.026(3) C34 0.080(3) 0.079(3) 0.065(3) 0.016(2) 0.000(2) -0.020(2) C35 0.0334(17) 0.045(2) 0.053(2) -0.0107(15) 0.0051(16) -0.0096(16) C36 0.046(2) 0.049(2) 0.067(2) -0.0095(17) 0.0095(18) -0.0093(19) C37 0.064(3) 0.056(3) 0.119(4) -0.009(2) 0.019(3) -0.035(3) C38 0.060(3) 0.100(4) 0.103(4) -0.032(3) 0.014(3) -0.058(3) C39 0.056(3) 0.109(4) 0.076(3) -0.022(3) 0.000(2) -0.040(3) C40 0.047(2) 0.070(3) 0.061(2) -0.0113(19) 0.0004(19) -0.018(2) C41 0.0245(16) 0.0481(19) 0.056(2) -0.0046(14) 0.0035(14) -0.0001(16) C42 0.0252(16) 0.0484(19) 0.050(2) 0.0018(14) 0.0034(14) -0.0019(16) C43 0.0267(16) 0.0430(18) 0.0444(19) -0.0002(14) -0.0043(14) 0.0031(15) C44 0.0359(18) 0.057(2) 0.043(2) 0.0095(16) -0.0044(15) 0.0027(17) C45 0.057(2) 0.083(3) 0.046(2) 0.016(2) -0.0078(18) -0.003(2) C46 0.064(3) 0.089(3) 0.051(2) 0.019(2) -0.022(2) 0.007(2) C47 0.056(2) 0.077(3) 0.072(3) 0.028(2) -0.020(2) 0.004(2) C48 0.045(2) 0.059(2) 0.057(2) 0.0166(17) -0.0074(17) -0.0011(18) C49 0.0244(15) 0.0393(18) 0.052(2) 0.0085(14) -0.0066(14) -0.0054(15) C50 0.042(2) 0.042(2) 0.083(3) 0.0056(17) -0.0025(19) -0.0046(19) C51 0.060(3) 0.042(2) 0.126(4) -0.004(2) -0.001(3) -0.004(2) C52 0.070(3) 0.056(3) 0.125(4) 0.015(2) -0.012(3) -0.040(3) C53 0.067(3) 0.080(3) 0.079(3) 0.020(2) 0.001(2) -0.034(3) C54 0.045(2) 0.053(2) 0.060(2) 0.0129(17) 0.0011(17) -0.0127(18) C55 0.0423(18) 0.0410(18) 0.0461(19) -0.0110(15) 0.0037(15) 0.0015(15) C56 0.0450(19) 0.0358(18) 0.049(2) -0.0013(15) -0.0037(15) 0.0061(15) C57 0.0336(16) 0.0477(19) 0.0330(17) 0.0019(15) -0.0026(14) 0.0091(15) C58 0.0372(19) 0.067(2) 0.047(2) 0.0040(17) -0.0016(16) 0.0080(17) C59 0.039(2) 0.090(3) 0.048(2) -0.010(2) -0.0043(17) 0.001(2) C60 0.040(2) 0.114(4) 0.050(2) 0.012(2) 0.0001(18) 0.017(2) C61 0.052(2) 0.084(3) 0.063(3) 0.028(2) 0.010(2) 0.014(2) C62 0.048(2) 0.059(2) 0.048(2) 0.0109(18) -0.0008(17) 0.0033(17) C63 0.0381(17) 0.0371(17) 0.0377(18) -0.0074(14) 0.0008(14) 0.0055(14) C64 0.046(2) 0.066(2) 0.039(2) 0.0033(18) -0.0014(16) 0.0026(17) C65 0.061(2) 0.080(3) 0.055(2) 0.019(2) 0.007(2) -0.006(2) C66 0.068(3) 0.083(3) 0.045(2) -0.009(2) 0.020(2) -0.006(2) C67 0.085(3) 0.065(3) 0.038(2) -0.008(2) 0.012(2) 0.0072(19) C68 0.065(2) 0.049(2) 0.047(2) -0.0003(18) 0.0083(18) 0.0112(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 P5 . 2.1909(8) ? Fe1 P1 . 2.2104(8) ? Fe1 P3 . 2.2143(8) ? Fe1 P4 . 2.2154(8) ? Fe1 P2 . 2.2162(8) ? P1 C1 . 1.840(3) ? P1 C13 . 1.843(3) ? P1 C7 . 1.853(3) ? P2 C35 . 1.847(3) ? P2 C41 . 1.852(3) ? P2 C55 . 1.854(3) ? P3 C21 . 1.855(3) ? P3 C15 . 1.858(3) ? P3 C14 . 1.861(3) ? P4 C42 . 1.857(3) ? P4 C49 . 1.861(3) ? P4 C43 . 1.868(3) ? P5 C56 . 1.853(3) ? P5 C57 . 1.856(3) ? P5 C63 . 1.867(3) ? P6 C29 . 1.828(3) ? P6 C23 . 1.828(4) ? P6 C22 . 1.846(3) ? C1 C2 . 1.378(4) ? C1 C6 . 1.388(4) ? C2 C3 . 1.383(4) ? C2 H2 . 0.93 ? C3 C4 . 1.376(4) ? C3 H3 . 0.93 ? C4 C5 . 1.361(5) ? C4 H4 . 0.93 ? C5 C6 . 1.384(4) ? C5 H5 . 0.93 ? C6 H6 . 0.93 ? C7 C12 . 1.383(4) ? C7 C8 . 1.385(4) ? C8 C9 . 1.383(4) ? C8 H8 . 0.93 ? C9 C10 . 1.368(5) ? C9 H9 . 0.93 ? C10 C11 . 1.360(6) ? C10 H10 . 0.93 ? C11 C12 . 1.377(5) ? C11 H11 . 0.93 ? C12 H12 . 0.93 ? C13 C14 . 1.525(4) ? C13 H13A . 0.97 ? C13 H13B . 0.97 ? C14 H14A . 0.97 ? C14 H14B . 0.97 ? C15 C16 . 1.389(4) ? C15 C20 . 1.391(4) ? C16 C17 . 1.386(4) ? C16 H16 . 0.93 ? C17 C18 . 1.362(5) ? C17 H17 . 0.93 ? C18 C19 . 1.367(5) ? C18 H18 . 0.93 ? C19 C20 . 1.395(4) ? C19 H19 . 0.93 ? C20 H20 . 0.93 ? C21 C22 . 1.540(4) ? C21 H21A . 0.97 ? C21 H21B . 0.97 ? C22 H22A . 0.97 ? C22 H22B . 0.97 ? C23 C28 . 1.362(5) ? C23 C24 . 1.381(5) ? C24 C25 . 1.375(5) ? C24 H24 . 0.93 ? C25 C26 . 1.336(6) ? C25 H25 . 0.93 ? C26 C27 . 1.361(6) ? C26 H26 . 0.93 ? C27 C28 . 1.390(6) ? C27 H27 . 0.93 ? C28 H28 . 0.93 ? C29 C34 . 1.378(5) ? C29 C30 . 1.389(5) ? C30 C31 . 1.382(5) ? C30 H30 . 0.93 ? C31 C32 . 1.359(6) ? C31 H31 . 0.93 ? C32 C33 . 1.362(6) ? C32 H32 . 0.93 ? C33 C34 . 1.391(5) ? C33 H33 . 0.93 ? C34 H34 . 0.93 ? C35 C36 . 1.390(4) ? C35 C40 . 1.393(4) ? C36 C37 . 1.395(5) ? C36 H36 . 0.93 ? C37 C38 . 1.373(6) ? C37 H37 . 0.93 ? C38 C39 . 1.361(6) ? C38 H38 . 0.93 ? C39 C40 . 1.383(5) ? C39 H39 . 0.93 ? C40 H40 . 0.93 ? C41 C42 . 1.512(4) ? C41 H41A . 0.97 ? C41 H41B . 0.97 ? C42 H42A . 0.97 ? C42 H42B . 0.97 ? C43 C44 . 1.378(4) ? C43 C48 . 1.395(4) ? C44 C45 . 1.397(4) ? C44 H44 . 0.93 ? C45 C46 . 1.371(5) ? C45 H45 . 0.93 ? C46 C47 . 1.379(5) ? C46 H46 . 0.93 ? C47 C48 . 1.382(4) ? C47 H47 . 0.93 ? C48 H48 . 0.93 ? C49 C50 . 1.379(4) ? C49 C54 . 1.388(4) ? C50 C51 . 1.388(5) ? C50 H50 . 0.93 ? C51 C52 . 1.360(6) ? C51 H51 . 0.93 ? C52 C53 . 1.358(6) ? C52 H52 . 0.93 ? C53 C54 . 1.385(5) ? C53 H53 . 0.93 ? C54 H54 . 0.93 ? C55 C56 . 1.521(4) ? C55 H55A . 0.97 ? C55 H55B . 0.97 ? C56 H56A . 0.97 ? C56 H56B . 0.97 ? C57 C58 . 1.391(4) ? C57 C62 . 1.391(4) ? C58 C59 . 1.384(4) ? C58 H58 . 0.93 ? C59 C60 . 1.356(5) ? C59 H59 . 0.93 ? C60 C61 . 1.374(5) ? C60 H60 . 0.93 ? C61 C62 . 1.390(4) ? C61 H61 . 0.93 ? C62 H62 . 0.93 ? C63 C64 . 1.376(4) ? C63 C68 . 1.395(4) ? C64 C65 . 1.390(4) ? C64 H64 . 0.93 ? C65 C66 . 1.374(5) ? C65 H65 . 0.93 ? C66 C67 . 1.371(5) ? C66 H66 . 0.93 ? C67 C68 . 1.370(4) ? C67 H67 . 0.93 ? C68 H68 . 0.93 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag P5 Fe1 P1 . . 93.89(3) ? P5 Fe1 P3 . . 109.87(3) ? P1 Fe1 P3 . . 83.48(3) ? P5 Fe1 P4 . . 120.22(3) ? P1 Fe1 P4 . . 97.54(3) ? P3 Fe1 P4 . . 129.63(3) ? P5 Fe1 P2 . . 84.85(3) ? P1 Fe1 P2 . . 178.39(4) ? P3 Fe1 P2 . . 97.89(3) ? P4 Fe1 P2 . . 82.25(3) ? C1 P1 C13 . . 102.36(13) ? C1 P1 C7 . . 98.68(14) ? C13 P1 C7 . . 97.79(13) ? C1 P1 Fe1 . . 124.32(9) ? C13 P1 Fe1 . . 108.13(10) ? C7 P1 Fe1 . . 121.20(10) ? C35 P2 C41 . . 98.58(14) ? C35 P2 C55 . . 100.41(15) ? C41 P2 C55 . . 100.60(14) ? C35 P2 Fe1 . . 129.94(10) ? C41 P2 Fe1 . . 113.31(10) ? C55 P2 Fe1 . . 109.78(10) ? C21 P3 C15 . . 98.27(14) ? C21 P3 C14 . . 99.73(15) ? C15 P3 C14 . . 100.65(14) ? C21 P3 Fe1 . . 117.10(10) ? C15 P3 Fe1 . . 125.35(9) ? C14 P3 Fe1 . . 111.72(10) ? C42 P4 C49 . . 99.46(14) ? C42 P4 C43 . . 96.16(13) ? C49 P4 C43 . . 97.00(13) ? C42 P4 Fe1 . . 108.46(10) ? C49 P4 Fe1 . . 128.57(9) ? C43 P4 Fe1 . . 121.00(10) ? C56 P5 C57 . . 99.96(13) ? C56 P5 C63 . . 95.78(14) ? C57 P5 C63 . . 96.66(13) ? C56 P5 Fe1 . . 109.77(10) ? C57 P5 Fe1 . . 125.97(9) ? C63 P5 Fe1 . . 122.85(10) ? C29 P6 C23 . . 101.36(16) ? C29 P6 C22 . . 103.10(15) ? C23 P6 C22 . . 101.19(15) ? C2 C1 C6 . . 117.0(3) ? C2 C1 P1 . . 118.4(2) ? C6 C1 P1 . . 124.5(2) ? C1 C2 C3 . . 121.8(3) ? C1 C2 H2 . . 119.1 ? C3 C2 H2 . . 119.1 ? C4 C3 C2 . . 120.0(3) ? C4 C3 H3 . . 120.0 ? C2 C3 H3 . . 120.0 ? C5 C4 C3 . . 119.0(3) ? C5 C4 H4 . . 120.5 ? C3 C4 H4 . . 120.5 ? C4 C5 C6 . . 120.9(3) ? C4 C5 H5 . . 119.6 ? C6 C5 H5 . . 119.6 ? C5 C6 C1 . . 121.1(3) ? C5 C6 H6 . . 119.5 ? C1 C6 H6 . . 119.5 ? C12 C7 C8 . . 117.7(3) ? C12 C7 P1 . . 122.7(2) ? C8 C7 P1 . . 119.6(2) ? C9 C8 C7 . . 120.9(3) ? C9 C8 H8 . . 119.5 ? C7 C8 H8 . . 119.5 ? C10 C9 C8 . . 120.0(4) ? C10 C9 H9 . . 120.0 ? C8 C9 H9 . . 120.0 ? C11 C10 C9 . . 119.9(4) ? C11 C10 H10 . . 120.1 ? C9 C10 H10 . . 120.1 ? C10 C11 C12 . . 120.5(4) ? C10 C11 H11 . . 119.8 ? C12 C11 H11 . . 119.8 ? C11 C12 C7 . . 121.0(4) ? C11 C12 H12 . . 119.5 ? C7 C12 H12 . . 119.5 ? C14 C13 P1 . . 106.73(18) ? C14 C13 H13A . . 110.4 ? P1 C13 H13A . . 110.4 ? C14 C13 H13B . . 110.4 ? P1 C13 H13B . . 110.4 ? H13A C13 H13B . . 108.6 ? C13 C14 P3 . . 109.12(19) ? C13 C14 H14A . . 109.9 ? P3 C14 H14A . . 109.9 ? C13 C14 H14B . . 109.9 ? P3 C14 H14B . . 109.9 ? H14A C14 H14B . . 108.3 ? C16 C15 C20 . . 116.2(3) ? C16 C15 P3 . . 119.5(2) ? C20 C15 P3 . . 124.1(2) ? C17 C16 C15 . . 122.1(3) ? C17 C16 H16 . . 119.0 ? C15 C16 H16 . . 119.0 ? C18 C17 C16 . . 120.7(4) ? C18 C17 H17 . . 119.6 ? C16 C17 H17 . . 119.6 ? C17 C18 C19 . . 118.9(3) ? C17 C18 H18 . . 120.5 ? C19 C18 H18 . . 120.5 ? C18 C19 C20 . . 120.7(4) ? C18 C19 H19 . . 119.6 ? C20 C19 H19 . . 119.6 ? C15 C20 C19 . . 121.4(3) ? C15 C20 H20 . . 119.3 ? C19 C20 H20 . . 119.3 ? C22 C21 P3 . . 120.2(2) ? C22 C21 H21A . . 107.3 ? P3 C21 H21A . . 107.3 ? C22 C21 H21B . . 107.3 ? P3 C21 H21B . . 107.3 ? H21A C21 H21B . . 106.9 ? C21 C22 P6 . . 109.2(2) ? C21 C22 H22A . . 109.8 ? P6 C22 H22A . . 109.8 ? C21 C22 H22B . . 109.8 ? P6 C22 H22B . . 109.8 ? H22A C22 H22B . . 108.3 ? C28 C23 C24 . . 117.0(4) ? C28 C23 P6 . . 119.2(3) ? C24 C23 P6 . . 123.8(3) ? C25 C24 C23 . . 122.1(4) ? C25 C24 H24 . . 118.9 ? C23 C24 H24 . . 118.9 ? C26 C25 C24 . . 119.8(4) ? C26 C25 H25 . . 120.1 ? C24 C25 H25 . . 120.1 ? C25 C26 C27 . . 120.0(5) ? C25 C26 H26 . . 120.0 ? C27 C26 H26 . . 120.0 ? C26 C27 C28 . . 120.3(5) ? C26 C27 H27 . . 119.9 ? C28 C27 H27 . . 119.9 ? C23 C28 C27 . . 120.8(4) ? C23 C28 H28 . . 119.6 ? C27 C28 H28 . . 119.6 ? C34 C29 C30 . . 117.4(3) ? C34 C29 P6 . . 121.3(3) ? C30 C29 P6 . . 121.0(3) ? C31 C30 C29 . . 121.0(4) ? C31 C30 H30 . . 119.5 ? C29 C30 H30 . . 119.5 ? C32 C31 C30 . . 120.7(5) ? C32 C31 H31 . . 119.6 ? C30 C31 H31 . . 119.6 ? C31 C32 C33 . . 119.4(4) ? C31 C32 H32 . . 120.3 ? C33 C32 H32 . . 120.3 ? C32 C33 C34 . . 120.5(5) ? C32 C33 H33 . . 119.8 ? C34 C33 H33 . . 119.8 ? C29 C34 C33 . . 121.0(4) ? C29 C34 H34 . . 119.5 ? C33 C34 H34 . . 119.5 ? C36 C35 C40 . . 117.0(3) ? C36 C35 P2 . . 121.0(3) ? C40 C35 P2 . . 122.0(3) ? C35 C36 C37 . . 120.9(4) ? C35 C36 H36 . . 119.6 ? C37 C36 H36 . . 119.6 ? C38 C37 C36 . . 120.6(4) ? C38 C37 H37 . . 119.7 ? C36 C37 H37 . . 119.7 ? C39 C38 C37 . . 119.1(4) ? C39 C38 H38 . . 120.4 ? C37 C38 H38 . . 120.4 ? C38 C39 C40 . . 120.9(4) ? C38 C39 H39 . . 119.6 ? C40 C39 H39 . . 119.6 ? C39 C40 C35 . . 121.5(4) ? C39 C40 H40 . . 119.3 ? C35 C40 H40 . . 119.3 ? C42 C41 P2 . . 107.06(19) ? C42 C41 H41A . . 110.3 ? P2 C41 H41A . . 110.3 ? C42 C41 H41B . . 110.3 ? P2 C41 H41B . . 110.3 ? H41A C41 H41B . . 108.6 ? C41 C42 P4 . . 106.2(2) ? C41 C42 H42A . . 110.5 ? P4 C42 H42A . . 110.5 ? C41 C42 H42B . . 110.5 ? P4 C42 H42B . . 110.5 ? H42A C42 H42B . . 108.7 ? C44 C43 C48 . . 117.9(3) ? C44 C43 P4 . . 118.7(2) ? C48 C43 P4 . . 123.2(2) ? C43 C44 C45 . . 121.4(3) ? C43 C44 H44 . . 119.3 ? C45 C44 H44 . . 119.3 ? C46 C45 C44 . . 119.7(3) ? C46 C45 H45 . . 120.2 ? C44 C45 H45 . . 120.2 ? C45 C46 C47 . . 120.0(3) ? C45 C46 H46 . . 120.0 ? C47 C46 H46 . . 120.0 ? C46 C47 C48 . . 120.1(3) ? C46 C47 H47 . . 120.0 ? C48 C47 H47 . . 120.0 ? C47 C48 C43 . . 121.0(3) ? C47 C48 H48 . . 119.5 ? C43 C48 H48 . . 119.5 ? C50 C49 C54 . . 117.7(3) ? C50 C49 P4 . . 119.9(2) ? C54 C49 P4 . . 122.4(3) ? C49 C50 C51 . . 120.7(4) ? C49 C50 H50 . . 119.6 ? C51 C50 H50 . . 119.6 ? C52 C51 C50 . . 120.5(4) ? C52 C51 H51 . . 119.8 ? C50 C51 H51 . . 119.8 ? C53 C52 C51 . . 120.0(4) ? C53 C52 H52 . . 120.0 ? C51 C52 H52 . . 120.0 ? C52 C53 C54 . . 120.1(4) ? C52 C53 H53 . . 119.9 ? C54 C53 H53 . . 119.9 ? C53 C54 C49 . . 121.0(4) ? C53 C54 H54 . . 119.5 ? C49 C54 H54 . . 119.5 ? C56 C55 P2 . . 108.3(2) ? C56 C55 H55A . . 110.0 ? P2 C55 H55A . . 110.0 ? C56 C55 H55B . . 110.0 ? P2 C55 H55B . . 110.0 ? H55A C55 H55B . . 108.4 ? C55 C56 P5 . . 105.2(2) ? C55 C56 H56A . . 110.7 ? P5 C56 H56A . . 110.7 ? C55 C56 H56B . . 110.7 ? P5 C56 H56B . . 110.7 ? H56A C56 H56B . . 108.8 ? C58 C57 C62 . . 117.1(3) ? C58 C57 P5 . . 119.9(2) ? C62 C57 P5 . . 123.0(2) ? C59 C58 C57 . . 121.8(3) ? C59 C58 H58 . . 119.1 ? C57 C58 H58 . . 119.1 ? C60 C59 C58 . . 120.1(4) ? C60 C59 H59 . . 120.0 ? C58 C59 H59 . . 120.0 ? C59 C60 C61 . . 119.8(3) ? C59 C60 H60 . . 120.1 ? C61 C60 H60 . . 120.1 ? C60 C61 C62 . . 120.6(4) ? C60 C61 H61 . . 119.7 ? C62 C61 H61 . . 119.7 ? C61 C62 C57 . . 120.6(3) ? C61 C62 H62 . . 119.7 ? C57 C62 H62 . . 119.7 ? C64 C63 C68 . . 116.2(3) ? C64 C63 P5 . . 119.4(2) ? C68 C63 P5 . . 124.3(2) ? C63 C64 C65 . . 122.8(3) ? C63 C64 H64 . . 118.6 ? C65 C64 H64 . . 118.6 ? C66 C65 C64 . . 119.3(3) ? C66 C65 H65 . . 120.3 ? C64 C65 H65 . . 120.3 ? C67 C66 C65 . . 118.9(3) ? C67 C66 H66 . . 120.5 ? C65 C66 H66 . . 120.5 ? C68 C67 C66 . . 121.2(3) ? C68 C67 H67 . . 119.4 ? C66 C67 H67 . . 119.4 ? C67 C68 C63 . . 121.5(3) ? C67 C68 H68 . . 119.2 ? C63 C68 H68 . . 119.2 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C13 P1 C1 C2 . . . . 172.2(2) ? C7 P1 C1 C2 . . . . -87.8(3) ? Fe1 P1 C1 C2 . . . . 49.9(3) ? C13 P1 C1 C6 . . . . -7.1(3) ? C7 P1 C1 C6 . . . . 92.9(3) ? Fe1 P1 C1 C6 . . . . -129.5(3) ? C6 C1 C2 C3 . . . . 2.0(5) ? P1 C1 C2 C3 . . . . -177.4(3) ? C1 C2 C3 C4 . . . . 0.7(5) ? C2 C3 C4 C5 . . . . -2.8(6) ? C3 C4 C5 C6 . . . . 2.0(6) ? C4 C5 C6 C1 . . . . 0.8(6) ? C2 C1 C6 C5 . . . . -2.8(5) ? P1 C1 C6 C5 . . . . 176.6(3) ? C1 P1 C7 C12 . . . . -26.6(3) ? C13 P1 C7 C12 . . . . 77.2(3) ? Fe1 P1 C7 C12 . . . . -166.0(2) ? C1 P1 C7 C8 . . . . 156.3(2) ? C13 P1 C7 C8 . . . . -99.8(3) ? Fe1 P1 C7 C8 . . . . 16.9(3) ? C12 C7 C8 C9 . . . . -0.5(5) ? P1 C7 C8 C9 . . . . 176.7(3) ? C7 C8 C9 C10 . . . . -0.1(5) ? C8 C9 C10 C11 . . . . 0.3(7) ? C9 C10 C11 C12 . . . . 0.1(7) ? C10 C11 C12 C7 . . . . -0.6(7) ? C8 C7 C12 C11 . . . . 0.8(5) ? P1 C7 C12 C11 . . . . -176.3(3) ? C1 P1 C13 C14 . . . . 177.3(2) ? C7 P1 C13 C14 . . . . 76.6(2) ? Fe1 P1 C13 C14 . . . . -49.9(2) ? P1 C13 C14 P3 . . . . 41.7(2) ? C21 P3 C14 C13 . . . . 105.4(2) ? C15 P3 C14 C13 . . . . -154.1(2) ? Fe1 P3 C14 C13 . . . . -19.0(2) ? C21 P3 C15 C16 . . . . -45.7(3) ? C14 P3 C15 C16 . . . . -147.3(2) ? Fe1 P3 C15 C16 . . . . 86.2(3) ? C21 P3 C15 C20 . . . . 139.7(3) ? C14 P3 C15 C20 . . . . 38.1(3) ? Fe1 P3 C15 C20 . . . . -88.4(3) ? C20 C15 C16 C17 . . . . 0.7(5) ? P3 C15 C16 C17 . . . . -174.3(3) ? C15 C16 C17 C18 . . . . -1.3(5) ? C16 C17 C18 C19 . . . . 0.5(6) ? C17 C18 C19 C20 . . . . 0.9(6) ? C16 C15 C20 C19 . . . . 0.7(5) ? P3 C15 C20 C19 . . . . 175.5(3) ? C18 C19 C20 C15 . . . . -1.5(5) ? C15 P3 C21 C22 . . . . -42.8(3) ? C14 P3 C21 C22 . . . . 59.5(3) ? Fe1 P3 C21 C22 . . . . -179.8(2) ? P3 C21 C22 P6 . . . . 153.82(18) ? C29 P6 C22 C21 . . . . 177.3(2) ? C23 P6 C22 C21 . . . . 72.6(2) ? C29 P6 C23 C28 . . . . 126.5(3) ? C22 P6 C23 C28 . . . . -127.5(3) ? C29 P6 C23 C24 . . . . -52.6(3) ? C22 P6 C23 C24 . . . . 53.4(3) ? C28 C23 C24 C25 . . . . -0.9(6) ? P6 C23 C24 C25 . . . . 178.1(3) ? C23 C24 C25 C26 . . . . 1.2(6) ? C24 C25 C26 C27 . . . . -1.0(7) ? C25 C26 C27 C28 . . . . 0.7(9) ? C24 C23 C28 C27 . . . . 0.6(7) ? P6 C23 C28 C27 . . . . -178.5(4) ? C26 C27 C28 C23 . . . . -0.5(9) ? C23 P6 C29 C34 . . . . 148.9(3) ? C22 P6 C29 C34 . . . . 44.4(3) ? C23 P6 C29 C30 . . . . -37.3(3) ? C22 P6 C29 C30 . . . . -141.8(3) ? C34 C29 C30 C31 . . . . -0.2(6) ? P6 C29 C30 C31 . . . . -174.2(3) ? C29 C30 C31 C32 . . . . -0.3(6) ? C30 C31 C32 C33 . . . . 0.5(7) ? C31 C32 C33 C34 . . . . -0.2(7) ? C30 C29 C34 C33 . . . . 0.4(6) ? P6 C29 C34 C33 . . . . 174.4(3) ? C32 C33 C34 C29 . . . . -0.2(7) ? C41 P2 C35 C36 . . . . 138.2(3) ? C55 P2 C35 C36 . . . . 35.6(3) ? Fe1 P2 C35 C36 . . . . -91.4(3) ? C41 P2 C35 C40 . . . . -42.9(3) ? C55 P2 C35 C40 . . . . -145.5(3) ? Fe1 P2 C35 C40 . . . . 87.5(3) ? C40 C35 C36 C37 . . . . 0.2(5) ? P2 C35 C36 C37 . . . . 179.1(3) ? C35 C36 C37 C38 . . . . 0.4(6) ? C36 C37 C38 C39 . . . . -0.5(6) ? C37 C38 C39 C40 . . . . -0.1(6) ? C38 C39 C40 C35 . . . . 0.7(6) ? C36 C35 C40 C39 . . . . -0.7(5) ? P2 C35 C40 C39 . . . . -179.7(3) ? C35 P2 C41 C42 . . . . 165.4(2) ? C55 P2 C41 C42 . . . . -92.2(2) ? Fe1 P2 C41 C42 . . . . 24.9(2) ? P2 C41 C42 P4 . . . . -45.4(2) ? C49 P4 C42 C41 . . . . -172.4(2) ? C43 P4 C42 C41 . . . . -74.2(2) ? Fe1 P4 C42 C41 . . . . 51.4(2) ? C42 P4 C43 C44 . . . . 106.9(3) ? C49 P4 C43 C44 . . . . -152.7(2) ? Fe1 P4 C43 C44 . . . . -8.9(3) ? C42 P4 C43 C48 . . . . -67.0(3) ? C49 P4 C43 C48 . . . . 33.3(3) ? Fe1 P4 C43 C48 . . . . 177.1(2) ? C48 C43 C44 C45 . . . . 0.1(5) ? P4 C43 C44 C45 . . . . -174.2(3) ? C43 C44 C45 C46 . . . . -0.2(5) ? C44 C45 C46 C47 . . . . -0.2(6) ? C45 C46 C47 C48 . . . . 0.6(6) ? C46 C47 C48 C43 . . . . -0.7(6) ? C44 C43 C48 C47 . . . . 0.3(5) ? P4 C43 C48 C47 . . . . 174.3(3) ? C42 P4 C49 C50 . . . . 155.8(2) ? C43 P4 C49 C50 . . . . 58.4(3) ? Fe1 P4 C49 C50 . . . . -81.2(3) ? C42 P4 C49 C54 . . . . -24.8(3) ? C43 P4 C49 C54 . . . . -122.3(3) ? Fe1 P4 C49 C54 . . . . 98.1(2) ? C54 C49 C50 C51 . . . . -1.7(5) ? P4 C49 C50 C51 . . . . 177.7(3) ? C49 C50 C51 C52 . . . . 1.2(6) ? C50 C51 C52 C53 . . . . -0.6(6) ? C51 C52 C53 C54 . . . . 0.5(6) ? C52 C53 C54 C49 . . . . -1.0(6) ? C50 C49 C54 C53 . . . . 1.6(5) ? P4 C49 C54 C53 . . . . -177.7(3) ? C35 P2 C55 C56 . . . . -104.7(2) ? C41 P2 C55 C56 . . . . 154.4(2) ? Fe1 P2 C55 C56 . . . . 34.8(2) ? P2 C55 C56 P5 . . . . -48.6(2) ? C57 P5 C56 C55 . . . . 179.7(2) ? C63 P5 C56 C55 . . . . -82.4(2) ? Fe1 P5 C56 C55 . . . . 45.6(2) ? C56 P5 C57 C58 . . . . 143.3(3) ? C63 P5 C57 C58 . . . . 46.2(3) ? Fe1 P5 C57 C58 . . . . -93.2(3) ? C56 P5 C57 C62 . . . . -38.8(3) ? C63 P5 C57 C62 . . . . -135.9(3) ? Fe1 P5 C57 C62 . . . . 84.7(3) ? C62 C57 C58 C59 . . . . -2.1(5) ? P5 C57 C58 C59 . . . . 175.9(2) ? C57 C58 C59 C60 . . . . 2.5(5) ? C58 C59 C60 C61 . . . . -1.4(5) ? C59 C60 C61 C62 . . . . 0.0(6) ? C60 C61 C62 C57 . . . . 0.4(5) ? C58 C57 C62 C61 . . . . 0.6(5) ? P5 C57 C62 C61 . . . . -177.3(3) ? C56 P5 C63 C64 . . . . 118.8(3) ? C57 P5 C63 C64 . . . . -140.4(3) ? Fe1 P5 C63 C64 . . . . 0.8(3) ? C56 P5 C63 C68 . . . . -57.3(3) ? C57 P5 C63 C68 . . . . 43.4(3) ? Fe1 P5 C63 C68 . . . . -175.4(2) ? C68 C63 C64 C65 . . . . 0.5(5) ? P5 C63 C64 C65 . . . . -175.9(3) ? C63 C64 C65 C66 . . . . 0.1(6) ? C64 C65 C66 C67 . . . . -0.4(6) ? C65 C66 C67 C68 . . . . 0.2(6) ? C66 C67 C68 C63 . . . . 0.5(6) ? C64 C63 C68 C67 . . . . -0.8(5) ? P5 C63 C68 C67 . . . . 175.4(3) ? _iucr_refine_instructions_details ; TITL P21c in P2(1)/c CELL 0.71073 9.8705 28.4738 20.7566 90.000 93.430 90.000 ZERR 4.00 0.0005 0.0013 0.0010 0.000 0.001 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H P Fe UNIT 272 264 24 4 L.S. 8 ACTA BOND $H FMAP 2 PLAN -10 CONF HTAB SIZE 0.088 0.114 0.279 TEMP 20.000 WGHT 0.039300 0.988500 FVAR 0.07421 FE1 4 0.447512 0.380300 0.704398 11.00000 0.02073 0.03049 = 0.03286 0.00103 0.00060 -0.00056 P1 3 0.285210 0.326740 0.697231 11.00000 0.02390 0.03435 = 0.03665 0.00147 -0.00061 -0.00245 P2 3 0.610825 0.433822 0.708616 11.00000 0.02688 0.03497 = 0.04218 -0.00024 0.00141 -0.00373 P3 3 0.329113 0.408381 0.783115 11.00000 0.02568 0.03804 = 0.03771 -0.00182 0.00268 0.00032 P4 3 0.622715 0.331537 0.709241 11.00000 0.02391 0.03502 = 0.03804 -0.00005 -0.00053 0.00276 P5 3 0.381823 0.413971 0.612887 11.00000 0.03053 0.03431 = 0.03615 0.00368 0.00021 0.00042 P6 3 0.213709 0.556560 0.828659 11.00000 0.03994 0.04994 = 0.06725 -0.00930 0.00542 0.00564 C1 1 0.227909 0.296584 0.622057 11.00000 0.02807 0.03447 = 0.04187 -0.00192 0.00136 -0.00643 C2 1 0.324212 0.276663 0.585175 11.00000 0.03666 0.06377 = 0.04396 -0.00452 -0.00705 -0.00091 AFIX 43 H2 2 0.414998 0.277794 0.599921 11.00000 -1.20000 AFIX 0 C3 1 0.289626 0.255030 0.526830 11.00000 0.04676 0.07854 = 0.05273 -0.01755 0.00291 0.00106 AFIX 43 H3 2 0.356669 0.241562 0.503176 11.00000 -1.20000 AFIX 0 C4 1 0.156044 0.253422 0.503761 11.00000 0.06144 0.07902 = 0.04232 -0.01513 -0.00601 -0.01926 AFIX 43 H4 2 0.132510 0.240127 0.463721 11.00000 -1.20000 AFIX 0 C5 1 0.058871 0.271580 0.540410 11.00000 0.03637 0.08749 = 0.06788 -0.01941 -0.00799 -0.01377 AFIX 43 H5 2 -0.031891 0.269743 0.525788 11.00000 -1.20000 AFIX 0 C6 1 0.093367 0.292732 0.599134 11.00000 0.03263 0.06965 = 0.05952 -0.01863 0.00025 -0.00569 AFIX 43 H6 2 0.025279 0.304562 0.623645 11.00000 -1.20000 AFIX 0 C7 1 0.287530 0.275654 0.752554 11.00000 0.03367 0.04186 = 0.04668 0.00766 0.00245 -0.00062 C8 1 0.369644 0.276660 0.809052 11.00000 0.04363 0.05351 = 0.04526 0.00496 0.00283 -0.00255 AFIX 43 H8 2 0.426351 0.302273 0.817619 11.00000 -1.20000 AFIX 0 C9 1 0.368468 0.240103 0.852897 11.00000 0.07435 0.07319 = 0.05257 0.02352 0.00161 0.00964 AFIX 43 H9 2 0.424188 0.241239 0.890613 11.00000 -1.20000 AFIX 0 C10 1 0.285353 0.202274 0.840792 11.00000 0.10182 0.06381 = 0.09261 0.04320 0.01427 0.00035 AFIX 43 H10 2 0.284230 0.177736 0.870327 11.00000 -1.20000 AFIX 0 C11 1 0.204381 0.200629 0.785477 11.00000 0.10465 0.06342 = 0.09782 0.03259 -0.01157 -0.02701 AFIX 43 H11 2 0.147856 0.174908 0.777339 11.00000 -1.20000 AFIX 0 C12 1 0.205476 0.236764 0.741433 11.00000 0.07035 0.04870 = 0.07047 0.01632 -0.01070 -0.01855 AFIX 43 H12 2 0.150194 0.234996 0.703625 11.00000 -1.20000 AFIX 0 C13 1 0.127432 0.354040 0.722287 11.00000 0.02321 0.04458 = 0.04627 0.00299 -0.00011 -0.00353 AFIX 23 H13A 2 0.093778 0.376710 0.690319 11.00000 -1.20000 H13B 2 0.058181 0.330338 0.727106 11.00000 -1.20000 AFIX 0 C14 1 0.162314 0.378291 0.786665 11.00000 0.02785 0.05482 = 0.04952 -0.00626 0.00853 -0.00377 AFIX 23 H14A 2 0.166684 0.355294 0.821204 11.00000 -1.20000 H14B 2 0.092542 0.401028 0.795362 11.00000 -1.20000 AFIX 0 C15 1 0.386148 0.409214 0.870038 11.00000 0.03266 0.04275 = 0.03700 -0.00343 0.00560 0.00637 C16 1 0.464298 0.446444 0.894422 11.00000 0.04605 0.05718 = 0.04686 -0.00278 0.00338 0.00014 AFIX 43 H16 2 0.480121 0.471801 0.867649 11.00000 -1.20000 AFIX 0 C17 1 0.519454 0.446997 0.957406 11.00000 0.06364 0.07471 = 0.05399 -0.01595 -0.00784 -0.00389 AFIX 43 H17 2 0.572858 0.472244 0.971784 11.00000 -1.20000 AFIX 0 C18 1 0.496285 0.410955 0.998482 11.00000 0.07019 0.09465 = 0.03836 -0.00541 -0.00834 0.01144 AFIX 43 H18 2 0.532822 0.411527 1.040826 11.00000 -1.20000 AFIX 0 C19 1 0.418436 0.373925 0.976438 11.00000 0.07680 0.07230 = 0.04479 0.01117 0.00478 0.00684 AFIX 43 H19 2 0.400930 0.349339 1.004240 11.00000 -1.20000 AFIX 0 C20 1 0.364958 0.372609 0.912694 11.00000 0.05363 0.05784 = 0.04598 -0.00176 0.00466 0.00168 AFIX 43 H20 2 0.314101 0.346730 0.898423 11.00000 -1.20000 AFIX 0 C21 1 0.270775 0.470179 0.775616 11.00000 0.04034 0.04760 = 0.04778 0.00082 0.00623 0.00946 AFIX 23 H21A 2 0.350645 0.489548 0.771529 11.00000 -1.20000 H21B 2 0.216585 0.472763 0.735220 11.00000 -1.20000 AFIX 0 C22 1 0.188260 0.492318 0.828451 11.00000 0.04707 0.04826 = 0.05520 -0.00140 0.01137 0.01255 AFIX 23 H22A 2 0.217674 0.479433 0.870234 11.00000 -1.20000 H22B 2 0.092703 0.485163 0.820247 11.00000 -1.20000 AFIX 0 C23 1 0.115481 0.573498 0.754843 11.00000 0.04365 0.04712 = 0.05972 -0.00605 0.00928 0.00696 C24 1 -0.018701 0.561350 0.741437 11.00000 0.05872 0.06252 = 0.07700 0.00847 0.00014 0.00208 AFIX 43 H24 2 -0.062018 0.542745 0.770754 11.00000 -1.20000 AFIX 0 C25 1 -0.090312 0.575866 0.686169 11.00000 0.06621 0.07664 = 0.07385 -0.00913 -0.00384 0.00801 AFIX 43 H25 2 -0.181066 0.567570 0.678886 11.00000 -1.20000 AFIX 0 C26 1 -0.029173 0.601921 0.642960 11.00000 0.08059 0.13275 = 0.05748 0.00326 0.00639 0.02682 AFIX 43 H26 2 -0.076959 0.611381 0.605206 11.00000 -1.20000 AFIX 0 C27 1 0.103090 0.614630 0.654177 11.00000 0.08927 0.23724 = 0.08706 0.07219 0.01169 -0.01623 AFIX 43 H27 2 0.145171 0.633055 0.624236 11.00000 -1.20000 AFIX 0 C28 1 0.175504 0.600199 0.710163 11.00000 0.05894 0.15991 = 0.08093 0.03841 0.01410 -0.01443 AFIX 43 H28 2 0.266016 0.608873 0.717206 11.00000 -1.20000 AFIX 0 C29 1 0.103121 0.576773 0.890565 11.00000 0.04013 0.05266 = 0.06297 -0.02060 -0.00167 0.00003 C30 1 0.029999 0.618256 0.882822 11.00000 0.06366 0.06184 = 0.08763 -0.02057 0.00827 0.00696 AFIX 43 H30 2 0.030872 0.634537 0.844007 11.00000 -1.20000 AFIX 0 C31 1 -0.044068 0.635710 0.931950 11.00000 0.06946 0.08682 = 0.11069 -0.05012 0.00799 0.01335 AFIX 43 H31 2 -0.091992 0.663637 0.925864 11.00000 -1.20000 AFIX 0 C32 1 -0.047639 0.612524 0.989030 11.00000 0.06778 0.13329 = 0.08648 -0.06452 0.01579 -0.00480 AFIX 43 H32 2 -0.098250 0.624330 1.021766 11.00000 -1.20000 AFIX 0 C33 1 0.023586 0.571829 0.997868 11.00000 0.10722 0.13022 = 0.06215 -0.02597 0.01183 0.00580 AFIX 43 H33 2 0.021770 0.555871 1.036899 11.00000 -1.20000 AFIX 0 C34 1 0.099027 0.553960 0.948942 11.00000 0.07997 0.07932 = 0.06462 -0.02038 -0.00014 0.01559 AFIX 43 H34 2 0.147421 0.526199 0.955746 11.00000 -1.20000 AFIX 0 C35 1 0.648907 0.480707 0.768453 11.00000 0.03336 0.04550 = 0.05312 -0.00959 0.00509 -0.01070 C36 1 0.593946 0.525382 0.760038 11.00000 0.04645 0.04941 = 0.06732 -0.00929 0.00953 -0.00949 AFIX 43 H36 2 0.538113 0.531907 0.723450 11.00000 -1.20000 AFIX 0 C37 1 0.621405 0.560574 0.805742 11.00000 0.06369 0.05587 = 0.11923 -0.03514 0.01913 -0.00874 AFIX 43 H37 2 0.583217 0.590200 0.799439 11.00000 -1.20000 AFIX 0 C38 1 0.704234 0.551891 0.859915 11.00000 0.05980 0.10037 = 0.10334 -0.05808 0.01448 -0.03219 AFIX 43 H38 2 0.722904 0.575491 0.890126 11.00000 -1.20000 AFIX 0 C39 1 0.758675 0.508302 0.868841 11.00000 0.05564 0.10879 = 0.07625 -0.03958 0.00028 -0.02174 AFIX 43 H39 2 0.814954 0.502197 0.905423 11.00000 -1.20000 AFIX 0 C40 1 0.731428 0.472968 0.824241 11.00000 0.04659 0.06993 = 0.06135 -0.01801 0.00040 -0.01125 AFIX 43 H40 2 0.769042 0.443372 0.831658 11.00000 -1.20000 AFIX 0 C41 1 0.783083 0.408291 0.706532 11.00000 0.02445 0.04808 = 0.05563 -0.00012 0.00348 -0.00456 AFIX 23 H41A 2 0.841081 0.428709 0.682856 11.00000 -1.20000 H41B 2 0.823238 0.404456 0.750017 11.00000 -1.20000 AFIX 0 C42 1 0.767961 0.361135 0.673398 11.00000 0.02516 0.04837 = 0.04951 -0.00186 0.00342 0.00178 AFIX 23 H42A 2 0.850111 0.342715 0.680710 11.00000 -1.20000 H42B 2 0.750054 0.365200 0.627276 11.00000 -1.20000 AFIX 0 C43 1 0.714270 0.316913 0.788033 11.00000 0.02673 0.04297 = 0.04442 0.00314 -0.00432 -0.00016 C44 1 0.683517 0.341862 0.842142 11.00000 0.03594 0.05701 = 0.04308 0.00267 -0.00438 0.00953 AFIX 43 H44 2 0.612498 0.363368 0.839296 11.00000 -1.20000 AFIX 0 C45 1 0.756781 0.335523 0.901163 11.00000 0.05672 0.08323 = 0.04617 -0.00260 -0.00780 0.01581 AFIX 43 H45 2 0.734743 0.352742 0.937143 11.00000 -1.20000 AFIX 0 C46 1 0.861342 0.303790 0.905786 11.00000 0.06429 0.08890 = 0.05086 0.00716 -0.02177 0.01892 AFIX 43 H46 2 0.910625 0.299505 0.944946 11.00000 -1.20000 AFIX 0 C47 1 0.893458 0.278226 0.852391 11.00000 0.05561 0.07724 = 0.07234 0.00359 -0.02038 0.02763 AFIX 43 H47 2 0.963842 0.256483 0.855675 11.00000 -1.20000 AFIX 0 C48 1 0.821205 0.284863 0.793984 11.00000 0.04484 0.05881 = 0.05694 -0.00114 -0.00739 0.01657 AFIX 43 H48 2 0.844219 0.267706 0.758112 11.00000 -1.20000 AFIX 0 C49 1 0.636515 0.272534 0.671678 11.00000 0.02440 0.03930 = 0.05185 -0.00542 -0.00660 0.00854 C50 1 0.583821 0.233736 0.701051 11.00000 0.04223 0.04214 = 0.08269 -0.00457 -0.00246 0.00561 AFIX 43 H50 2 0.544474 0.237088 0.740398 11.00000 -1.20000 AFIX 0 C51 1 0.588855 0.189711 0.672532 11.00000 0.05972 0.04158 = 0.12582 -0.00405 -0.00135 -0.00364 AFIX 43 H51 2 0.551330 0.163958 0.692491 11.00000 -1.20000 AFIX 0 C52 1 0.648275 0.183994 0.615621 11.00000 0.06990 0.05647 = 0.12503 -0.03959 -0.01180 0.01480 AFIX 43 H52 2 0.652030 0.154359 0.596976 11.00000 -1.20000 AFIX 0 C53 1 0.702143 0.221577 0.586012 11.00000 0.06710 0.08046 = 0.07899 -0.03394 0.00078 0.02031 AFIX 43 H53 2 0.742165 0.217678 0.546927 11.00000 -1.20000 AFIX 0 C54 1 0.697602 0.265685 0.613895 11.00000 0.04537 0.05308 = 0.05989 -0.01270 0.00112 0.01291 AFIX 43 H54 2 0.736070 0.291109 0.593597 11.00000 -1.20000 AFIX 0 C55 1 0.602496 0.468588 0.632945 11.00000 0.04230 0.04103 = 0.04614 0.00151 0.00372 -0.01104 AFIX 23 H55A 2 0.643073 0.499249 0.640717 11.00000 -1.20000 H55B 2 0.652048 0.452691 0.600369 11.00000 -1.20000 AFIX 0 C56 1 0.454170 0.473923 0.609825 11.00000 0.04502 0.03578 = 0.04928 0.00611 -0.00374 -0.00131 AFIX 23 H56A 2 0.446210 0.486170 0.566155 11.00000 -1.20000 H56B 2 0.407728 0.495032 0.637819 11.00000 -1.20000 AFIX 0 C57 1 0.203785 0.426388 0.584166 11.00000 0.03357 0.04773 = 0.03304 0.00910 -0.00263 0.00194 C58 1 0.132474 0.394139 0.544888 11.00000 0.03719 0.06666 = 0.04713 0.00804 -0.00156 0.00399 AFIX 43 H58 2 0.176994 0.367490 0.531173 11.00000 -1.20000 AFIX 0 C59 1 -0.002938 0.400620 0.525651 11.00000 0.03883 0.09047 = 0.04843 0.00105 -0.00429 -0.00981 AFIX 43 H59 2 -0.049035 0.377893 0.500747 11.00000 -1.20000 AFIX 0 C60 1 -0.068466 0.440078 0.543080 11.00000 0.04008 0.11428 = 0.04985 0.01737 0.00014 0.01182 AFIX 43 H60 2 -0.158905 0.444754 0.529398 11.00000 -1.20000 AFIX 0 C61 1 -0.000834 0.473123 0.581012 11.00000 0.05157 0.08378 = 0.06292 0.01386 0.01002 0.02843 AFIX 43 H61 2 -0.045869 0.500171 0.592912 11.00000 -1.20000 AFIX 0 C62 1 0.134296 0.466472 0.601746 11.00000 0.04763 0.05948 = 0.04754 0.00333 -0.00081 0.01095 AFIX 43 H62 2 0.178706 0.489028 0.627619 11.00000 -1.20000 AFIX 0 C63 1 0.441511 0.394504 0.533527 11.00000 0.03809 0.03708 = 0.03773 0.00549 0.00075 -0.00741 C64 1 0.529401 0.357111 0.531435 11.00000 0.04646 0.06650 = 0.03900 0.00263 -0.00143 0.00328 AFIX 43 H64 2 0.552658 0.341015 0.569487 11.00000 -1.20000 AFIX 0 C65 1 0.584940 0.342358 0.474859 11.00000 0.06075 0.07968 = 0.05465 -0.00648 0.00735 0.01876 AFIX 43 H65 2 0.643952 0.316881 0.475340 11.00000 -1.20000 AFIX 0 C66 1 0.551775 0.365790 0.418230 11.00000 0.06811 0.08339 = 0.04535 -0.00638 0.01963 -0.00880 AFIX 43 H66 2 0.588431 0.356548 0.379980 11.00000 -1.20000 AFIX 0 C67 1 0.463764 0.403021 0.419014 11.00000 0.08536 0.06501 = 0.03837 0.00723 0.01162 -0.00812 AFIX 43 H67 2 0.440676 0.418990 0.380840 11.00000 -1.20000 AFIX 0 C68 1 0.409246 0.417114 0.475004 11.00000 0.06457 0.04896 = 0.04722 0.01122 0.00826 -0.00026 AFIX 43 H68 2 0.349324 0.442345 0.473973 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM P21c in P2(1)/c REM R1 = 0.0453 for 6978 Fo > 4sig(Fo) and 0.0852 for all 10651 data REM 676 parameters refined using 0 restraints END WGHT 0.0393 0.9885 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.332, deepest hole -0.308, 1-sigma level 0.052 Q1 1 0.4483 0.3707 0.6601 11.00000 0.05 0.33 Q2 1 0.4098 0.4007 0.6638 11.00000 0.05 0.32 Q3 1 0.4034 0.4060 0.5671 11.00000 0.05 0.29 Q4 1 0.3464 0.4031 0.8391 11.00000 0.05 0.27 Q5 1 0.2953 0.2980 0.7238 11.00000 0.05 0.27 Q6 1 0.5278 0.4702 0.6218 11.00000 0.05 0.26 Q7 1 0.3510 0.4102 0.7367 11.00000 0.05 0.26 Q8 1 0.6048 0.4461 0.6624 11.00000 0.05 0.25 Q9 1 0.0212 0.6287 0.6594 11.00000 0.05 0.25 Q10 1 0.2768 0.3087 0.6565 11.00000 0.05 0.25 ; _shelx_res_checksum 97058 _shelx_hkl_file ; -1 0 0 363.53 6.49 -1 0 0 364.76 6.48 -1 0 0 359.94 6.42 -2 0 0 2.10 0.35 -2 0 0 2.41 0.34 -2 0 0 1.69 0.32 -3 0 0 50.00 1.40 -3 0 0 49.48 1.42 -3 0 0 48.42 1.40 -4 0 0 64.39 1.84 -4 0 0 63.22 1.82 -4 0 0 63.06 1.79 -5 0 0 44.15 1.59 -5 0 0 45.68 1.61 -5 0 0 42.65 1.54 -6 0 0 15.33 1.17 -6 0 0 16.91 1.10 -6 0 0 16.95 1.06 -7 0 0 4.57 0.85 -7 0 0 2.29 0.63 -7 0 0 3.20 0.67 -8 0 0 -0.99 0.42 -8 0 0 0.37 0.60 -8 0 0 0.17 0.50 -9 0 0 0.20 0.56 -9 0 0 1.39 0.71 -9 0 0 -0.01 0.57 -10 0 0 1.61 0.88 -10 0 0 2.51 0.82 -10 0 0 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1.18 0.86 11 -6 0 1.13 0.70 -11 6 0 1.06 0.90 0 -7 0 0.20 0.32 0 7 0 0.38 0.25 0 7 0 0.06 0.24 1 -7 0 170.38 3.62 -1 -7 0 172.05 3.61 1 7 0 168.65 3.54 1 7 0 175.26 3.30 -1 7 0 176.28 3.58 -1 7 0 171.64 3.27 -2 -7 0 206.14 4.21 -2 -7 0 198.88 4.19 2 -7 0 198.99 4.19 2 7 0 198.31 3.76 -2 7 0 198.89 3.74 -2 7 0 198.00 4.22 3 -7 0 212.95 4.57 -3 -7 0 213.59 4.56 -3 -7 0 215.87 4.64 -3 7 0 215.16 4.11 3 7 0 216.27 4.14 -3 7 0 215.04 4.66 -4 -7 0 19.16 1.02 -4 -7 0 18.70 1.08 4 -7 0 19.52 1.06 4 7 0 19.73 0.80 -4 7 0 20.71 1.15 -4 7 0 21.05 0.80 -5 -7 0 5.37 0.80 -5 -7 0 4.17 0.68 5 -7 0 5.12 0.73 5 7 0 4.57 0.55 -5 7 0 5.15 0.55 -5 7 0 5.15 0.78 -6 -7 0 14.66 1.32 -6 -7 0 10.72 1.02 6 -7 0 11.17 1.06 6 7 0 11.62 0.90 -6 7 0 12.08 0.80 -6 7 0 11.12 1.14 -7 -7 0 2.09 0.73 -7 -7 0 1.42 0.62 7 -7 0 0.76 0.53 7 7 0 1.44 0.55 -7 7 0 1.01 0.62 -7 7 0 1.62 0.47 -8 -7 0 5.92 0.98 8 -7 0 7.62 1.06 -8 -7 0 5.65 1.07 8 7 0 6.57 0.85 -8 7 0 7.24 1.14 -8 7 0 6.48 0.83 9 -7 0 2.37 0.78 -9 -7 0 1.95 0.89 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