data_011212a_on _audit_creation_date 2012-02-02 _audit_creation_method ; Olex2 1.1 (compiled 2011.08.18 svn.r1932, GUI svn.r3819) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C17 H10 Br N2 O5 Re, 0.38(C H Cl3)' _chemical_formula_sum 'C17.38 H10.38 Br Cl1.13 N2 O5 Re' _chemical_formula_weight 633.14 _chemical_melting_point ? _chemical_oxdiff_formula 'C11 H10 S O2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 10.9098(5) _cell_length_b 14.1254(5) _cell_length_c 14.4369(6) _cell_angle_alpha 110.622(4) _cell_angle_beta 102.013(4) _cell_angle_gamma 90.398(3) _cell_volume 2028.80(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9635 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 71.6564 _cell_measurement_theta_min 3.3526 _exptl_absorpt_coefficient_mu 15.665 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.14282 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.073 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1191 _exptl_crystal_size_max 0.71 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_unetI/netI 0.0320 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 13213 _diffrn_reflns_theta_full 67.00 _diffrn_reflns_theta_max 67.00 _diffrn_reflns_theta_min 3.36 _diffrn_ambient_temperature 133(2) _diffrn_detector_area_resol_mean 16.1270 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 25.00 50.00 1.0000 2.5000 omega____ theta____ kappa____ phi______ frames - 0.0000 -122.0000 34.0000 25 #__ type_ start__ end____ width___ exp.time_ 2 omega -15.00 25.00 1.0000 2.5000 omega____ theta____ kappa____ phi______ frames - 0.0000 -37.0000 -30.0000 40 #__ type_ start__ end____ width___ exp.time_ 3 omega 16.00 56.00 1.0000 2.5000 omega____ theta____ kappa____ phi______ frames - 0.0000 77.0000 120.0000 40 #__ type_ start__ end____ width___ exp.time_ 4 omega -70.00 -34.00 1.0000 2.5000 omega____ theta____ kappa____ phi______ frames - 0.0000 -37.0000 -30.0000 36 #__ type_ start__ end____ width___ exp.time_ 5 omega -22.00 12.00 1.0000 2.5000 omega____ theta____ kappa____ phi______ frames - 0.0000 77.0000 120.0000 34 #__ type_ start__ end____ width___ exp.time_ 6 omega -111.00 -22.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -55.0000 125.0000 0.0000 89 #__ type_ start__ end____ width___ exp.time_ 7 omega 28.00 125.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 77.0000 -150.0000 97 #__ type_ start__ end____ width___ exp.time_ 8 omega 84.00 114.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 122.0000 145.0000 30 #__ type_ start__ end____ width___ exp.time_ 9 omega 44.00 113.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 77.0000 90.0000 69 #__ type_ start__ end____ width___ exp.time_ 10 omega 26.00 118.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 77.0000 150.0000 92 #__ type_ start__ end____ width___ exp.time_ 11 omega -83.00 0.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 50.0000 0.0000 83 #__ type_ start__ end____ width___ exp.time_ 12 omega -134.00 -109.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 -149.0000 81.0000 25 #__ type_ start__ end____ width___ exp.time_ 13 omega 130.00 157.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 50.0000 60.0000 27 #__ type_ start__ end____ width___ exp.time_ 14 omega 37.00 67.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -30.0000 30 #__ type_ start__ end____ width___ exp.time_ 15 omega 83.00 165.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 77.0000 -120.0000 82 #__ type_ start__ end____ width___ exp.time_ 16 omega 89.00 177.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 50.0000 -60.0000 88 #__ type_ start__ end____ width___ exp.time_ 17 omega 40.00 78.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 150.0000 38 #__ type_ start__ end____ width___ exp.time_ 18 omega 39.00 115.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -88.0000 37.0000 76 #__ type_ start__ end____ width___ exp.time_ 19 omega 122.00 146.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -88.0000 -15.0000 24 #__ type_ start__ end____ width___ exp.time_ 20 omega 46.00 71.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 0.0000 25 #__ type_ start__ end____ width___ exp.time_ 21 omega 41.00 72.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 30.0000 31 #__ type_ start__ end____ width___ exp.time_ 22 omega 38.00 146.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -88.0000 149.0000 108 #__ type_ start__ end____ width___ exp.time_ 23 omega 42.00 69.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 60.0000 27 #__ type_ start__ end____ width___ exp.time_ 24 omega 48.00 83.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 120.0000 35 #__ type_ start__ end____ width___ exp.time_ 25 omega 40.00 83.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 -120.0000 43 #__ type_ start__ end____ width___ exp.time_ 26 omega 106.00 170.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 111.0000 0.0000 64 #__ type_ start__ end____ width___ exp.time_ 27 omega 41.00 67.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -60.0000 26 #__ type_ start__ end____ width___ exp.time_ 28 omega 90.00 117.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 50.0000 60.0000 27 #__ type_ start__ end____ width___ exp.time_ 29 omega 98.00 174.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 25.0000 0.0000 76 #__ type_ start__ end____ width___ exp.time_ 30 omega 50.00 75.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 -90.0000 25 #__ type_ start__ end____ width___ exp.time_ 31 omega 75.00 127.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -88.0000 -109.0000 52 #__ type_ start__ end____ width___ exp.time_ 32 omega 46.00 81.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 -60.0000 35 #__ type_ start__ end____ width___ exp.time_ 33 omega 76.00 101.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -88.0000 -15.0000 25 #__ type_ start__ end____ width___ exp.time_ 34 omega 94.00 119.00 1.0000 24.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -88.0000 -84.0000 25 ; _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0480612000 _diffrn_orient_matrix_UB_12 -0.1116474000 _diffrn_orient_matrix_UB_13 -0.0286068000 _diffrn_orient_matrix_UB_21 0.0348135000 _diffrn_orient_matrix_UB_22 0.0122577000 _diffrn_orient_matrix_UB_23 0.1128599000 _diffrn_orient_matrix_UB_31 -0.1323271000 _diffrn_orient_matrix_UB_32 0.0326309000 _diffrn_orient_matrix_UB_33 0.0113458000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_source_current n/a _diffrn_source_voltage n/a _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6881 _reflns_number_total 7174 _reflns_odcompleteness_completeness 99.37 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 2.970 _refine_diff_density_min -2.991 _refine_diff_density_rms 0.304 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 541 _refine_ls_number_reflns 7174 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0456 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+7.8962P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1429 _refine_ls_wR_factor_ref 0.1446 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.09966(3) 0.90237(2) 0.19577(2) 0.01314(13) Uani 1 1 d . . . Re2 Re 0.79650(2) 0.51369(2) 0.161635(19) 0.01176(13) Uani 1 1 d . . . Br1 Br 0.13580(7) 0.89170(5) 0.01621(5) 0.02060(18) Uani 1 1 d . . . Br2 Br 0.63074(7) 0.37964(5) 0.00958(5) 0.01930(18) Uani 1 1 d . . . O1 O 0.0611(6) 0.9246(4) 0.4059(4) 0.0315(13) Uani 1 1 d . . . O2 O -0.1853(5) 0.9014(4) 0.1056(5) 0.0341(13) Uani 1 1 d . . . O3 O 0.0688(5) 0.6684(4) 0.1314(4) 0.0276(12) Uani 1 1 d . . . O4 O 0.1571(5) 1.1253(4) 0.3399(4) 0.0196(10) Uani 1 1 d . . . O5 O 0.3739(5) 0.9513(4) 0.3316(4) 0.0283(12) Uani 1 1 d . . . O6 O 0.9695(5) 0.6748(4) 0.3421(4) 0.0276(12) Uani 1 1 d . . . O7 O 1.0373(5) 0.4429(4) 0.0810(4) 0.0229(11) Uani 1 1 d . . . O8 O 0.7604(6) 0.6581(4) 0.0397(4) 0.0304(12) Uani 1 1 d . . . O9 O 0.8470(5) 0.4211(4) 0.3320(3) 0.0188(10) Uani 1 1 d . . . O10 O 0.6547(5) 0.6294(5) 0.3253(4) 0.0275(12) Uani 1 1 d . . . N1 N 0.1112(6) 1.1218(4) 0.1853(4) 0.0190(12) Uani 1 1 d . . . H1 H 0.0928 1.0986 0.1184 0.023 Uiso 1 1 calc R . . N2 N 0.3737(6) 0.8432(5) 0.1827(4) 0.0220(13) Uani 1 1 d . . . H2 H 0.3475 0.8033 0.1187 0.026 Uiso 1 1 calc R . . N3 N 0.7923(6) 0.3020(4) 0.1852(4) 0.0186(12) Uani 1 1 d . . . H3 H 0.7684 0.2709 0.1189 0.022 Uiso 1 1 calc R . . N4 N 0.5185(6) 0.5522(5) 0.1868(5) 0.0225(13) Uani 1 1 d . . . H4 H 0.4855 0.5140 0.1232 0.027 Uiso 1 1 calc R . . C1 C 0.0774(7) 0.9152(5) 0.3258(6) 0.0241(15) Uani 1 1 d . . . C2 C -0.0816(6) 0.9029(5) 0.1409(5) 0.0177(13) Uani 1 1 d . . . C3 C 0.0799(6) 0.7553(5) 0.1537(5) 0.0182(14) Uani 1 1 d . . . C4 C 0.1256(6) 1.0624(5) 0.2415(5) 0.0168(13) Uani 1 1 d . . . C5 C 0.1289(7) 1.2242(5) 0.2460(5) 0.0205(14) Uani 1 1 d . . . C6 C 0.1262(8) 1.3144(6) 0.2261(7) 0.0347(19) Uani 1 1 d . . . H6 H 0.1080 1.3143 0.1588 0.042 Uiso 1 1 calc R . . C7 C 0.1509(8) 1.4020(6) 0.3084(7) 0.036(2) Uani 1 1 d . . . H7 H 0.1479 1.4650 0.2984 0.043 Uiso 1 1 calc R . . C8 C 0.1808(8) 1.4023(6) 0.4082(7) 0.036(2) Uani 1 1 d . . . H8 H 0.1989 1.4655 0.4634 0.043 Uiso 1 1 calc R . . C9 C 0.1848(8) 1.3132(6) 0.4287(6) 0.0310(18) Uani 1 1 d . . . H9 H 0.2034 1.3127 0.4957 0.037 Uiso 1 1 calc R . . C10 C 0.1595(6) 1.2254(5) 0.3432(5) 0.0199(14) Uani 1 1 d . . . C11 C 0.2986(6) 0.8993(5) 0.2391(5) 0.0156(13) Uani 1 1 d . . . C12 C 0.4989(7) 0.8553(5) 0.2371(5) 0.0197(14) Uani 1 1 d . . . C13 C 0.6073(7) 0.8148(6) 0.2129(6) 0.0263(16) Uani 1 1 d . . . H13 H 0.6086 0.7685 0.1469 0.032 Uiso 1 1 calc R . . C14 C 0.7151(7) 0.8457(6) 0.2907(6) 0.0275(16) Uani 1 1 d . . . H14 H 0.7919 0.8184 0.2781 0.033 Uiso 1 1 calc R . . C15 C 0.7133(8) 0.9149(8) 0.3854(6) 0.037(2) Uani 1 1 d . . . H15 H 0.7886 0.9331 0.4370 0.044 Uiso 1 1 calc R . . C16 C 0.6036(8) 0.9588(8) 0.4078(6) 0.042(2) Uani 1 1 d . . . H16 H 0.6029 1.0096 0.4717 0.051 Uiso 1 1 calc R . . C17 C 0.4968(7) 0.9241(7) 0.3315(6) 0.0260(16) Uani 1 1 d . . . C18 C 0.9054(6) 0.6128(5) 0.2743(5) 0.0178(14) Uani 1 1 d . . . C19 C 0.9453(6) 0.4663(5) 0.1065(5) 0.0135(12) Uani 1 1 d . . . C20 C 0.7748(7) 0.6061(5) 0.0851(5) 0.0193(14) Uani 1 1 d . . . C21 C 0.8108(6) 0.4015(5) 0.2304(5) 0.0143(12) Uani 1 1 d . . . C22 C 0.8143(6) 0.2521(5) 0.2524(5) 0.0176(13) Uani 1 1 d . . . C23 C 0.8097(8) 0.1514(5) 0.2434(6) 0.0247(16) Uani 1 1 d . . . H23 H 0.7867 0.0980 0.1790 0.030 Uiso 1 1 calc R . . C24 C 0.8407(8) 0.1317(6) 0.3337(6) 0.0254(16) Uani 1 1 d . . . H24 H 0.8376 0.0634 0.3307 0.031 Uiso 1 1 calc R . . C25 C 0.8758(8) 0.2104(6) 0.4280(6) 0.0250(16) Uani 1 1 d . . . H25 H 0.8966 0.1945 0.4878 0.030 Uiso 1 1 calc R . . C26 C 0.8813(8) 0.3120(6) 0.4364(5) 0.0246(16) Uani 1 1 d . . . H26 H 0.9055 0.3661 0.5002 0.030 Uiso 1 1 calc R . . C27 C 0.8496(7) 0.3292(5) 0.3472(5) 0.0175(13) Uani 1 1 d . . . C28 C 0.6397(6) 0.5659(5) 0.2283(5) 0.0164(13) Uani 1 1 d . . . C29 C 0.4473(7) 0.6069(6) 0.2578(5) 0.0218(15) Uani 1 1 d . . . C30 C 0.3215(8) 0.6182(7) 0.2512(7) 0.0343(19) Uani 1 1 d . . . H30 H 0.2601 0.5845 0.1905 0.041 Uiso 1 1 calc R . . C31 C 0.2899(8) 0.6817(7) 0.3385(7) 0.0326(18) Uani 1 1 d . . . H31 H 0.2038 0.6915 0.3385 0.039 Uiso 1 1 calc R . . C32 C 0.3800(9) 0.7314(10) 0.4259(8) 0.051(3) Uani 1 1 d . . . H32 H 0.3540 0.7737 0.4846 0.062 Uiso 1 1 calc R . . C33 C 0.5079(9) 0.7216(9) 0.4308(8) 0.050(3) Uani 1 1 d . . . H33 H 0.5705 0.7580 0.4899 0.060 Uiso 1 1 calc R . . C34 C 0.5366(7) 0.6557(7) 0.3444(6) 0.0271(16) Uani 1 1 d . . . C35 C 0.5544(18) 0.6998(11) 0.7174(11) 0.055(3) Uani 0.50 1 d PDU A 1 H35 H 0.6387 0.6854 0.7012 0.065 Uiso 0.50 1 calc PR A 1 Cl1 Cl 0.4509(6) 0.6032(5) 0.6337(7) 0.0815(19) Uani 0.50 1 d PDU A 1 Cl2 Cl 0.5220(6) 0.8194(5) 0.7092(5) 0.0631(15) Uani 0.50 1 d PDU A 1 Cl3 Cl 0.5674(13) 0.7063(8) 0.8424(7) 0.121(3) Uani 0.50 1 d PDU A 1 C35A C 0.574(3) 0.9310(15) 0.9215(17) 0.051(5) Uani 0.25 1 d PDU B -2 H35A H 0.6660 0.9454 0.9520 0.061 Uiso 0.25 1 calc PR B -2 Cl1A Cl 0.5188(11) 0.8260(10) 0.9456(10) 0.068(3) Uani 0.25 1 d PDU B -2 Cl2A Cl 0.5503(10) 0.9043(9) 0.7913(9) 0.057(2) Uani 0.25 1 d PDU B -2 Cl3A Cl 0.4983(11) 1.0359(11) 0.9830(12) 0.074(3) Uani 0.25 1 d PDU B -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01630(19) 0.01154(19) 0.01001(18) 0.00303(13) 0.00117(12) -0.00086(12) Re2 0.01461(19) 0.01203(19) 0.00818(18) 0.00358(13) 0.00173(12) -0.00019(12) Br1 0.0288(4) 0.0217(4) 0.0094(3) 0.0041(3) 0.0029(3) 0.0021(3) Br2 0.0241(4) 0.0171(3) 0.0109(3) 0.0019(3) -0.0025(3) -0.0010(3) O1 0.044(3) 0.037(3) 0.018(3) 0.013(2) 0.013(2) -0.003(3) O2 0.022(3) 0.029(3) 0.049(4) 0.016(3) 0.002(3) 0.005(2) O3 0.028(3) 0.013(3) 0.035(3) 0.006(2) -0.001(2) -0.004(2) O4 0.022(2) 0.022(2) 0.014(2) 0.006(2) 0.0022(18) 0.0034(19) O5 0.025(3) 0.033(3) 0.015(2) -0.005(2) 0.001(2) -0.002(2) O6 0.023(3) 0.027(3) 0.021(3) 0.000(2) -0.004(2) -0.008(2) O7 0.026(3) 0.021(3) 0.024(3) 0.008(2) 0.010(2) 0.008(2) O8 0.043(3) 0.028(3) 0.034(3) 0.023(3) 0.018(3) 0.015(2) O9 0.030(3) 0.015(2) 0.010(2) 0.0051(18) 0.0000(19) 0.0025(19) O10 0.016(2) 0.047(3) 0.012(2) 0.003(2) 0.0002(19) 0.004(2) N1 0.027(3) 0.014(3) 0.013(3) 0.004(2) 0.000(2) -0.001(2) N2 0.019(3) 0.029(3) 0.010(3) -0.001(2) 0.000(2) -0.001(2) N3 0.028(3) 0.016(3) 0.009(3) 0.003(2) 0.000(2) -0.003(2) N4 0.023(3) 0.030(3) 0.013(3) 0.008(3) -0.001(2) 0.000(3) C1 0.027(4) 0.016(3) 0.024(4) 0.006(3) 0.000(3) -0.005(3) C2 0.014(3) 0.016(3) 0.022(3) 0.007(3) 0.001(3) 0.007(2) C3 0.016(3) 0.019(4) 0.015(3) 0.004(3) 0.000(2) -0.001(3) C4 0.010(3) 0.021(3) 0.013(3) 0.001(3) -0.002(2) -0.005(2) C5 0.022(4) 0.015(3) 0.020(3) 0.003(3) 0.002(3) -0.002(3) C6 0.033(4) 0.028(4) 0.042(5) 0.018(4) -0.003(4) -0.003(3) C7 0.028(4) 0.020(4) 0.055(6) 0.012(4) 0.002(4) 0.005(3) C8 0.029(4) 0.013(4) 0.049(5) -0.003(4) -0.003(4) 0.000(3) C9 0.026(4) 0.024(4) 0.029(4) -0.003(3) -0.002(3) 0.002(3) C10 0.017(3) 0.018(3) 0.021(3) 0.005(3) -0.001(3) -0.001(3) C11 0.018(3) 0.014(3) 0.012(3) 0.005(3) -0.001(2) -0.001(2) C12 0.024(4) 0.015(3) 0.014(3) 0.001(3) 0.000(3) -0.006(3) C13 0.018(4) 0.025(4) 0.029(4) 0.002(3) 0.003(3) 0.000(3) C14 0.019(4) 0.029(4) 0.034(4) 0.013(3) 0.002(3) 0.004(3) C15 0.025(4) 0.052(5) 0.024(4) 0.010(4) -0.003(3) -0.010(4) C16 0.027(4) 0.068(7) 0.015(4) -0.003(4) 0.000(3) -0.010(4) C17 0.014(3) 0.042(5) 0.016(3) 0.004(3) 0.004(3) 0.003(3) C18 0.015(3) 0.023(3) 0.019(3) 0.011(3) 0.003(3) 0.001(3) C19 0.024(3) 0.007(3) 0.009(3) 0.001(2) 0.006(2) 0.005(2) C20 0.023(4) 0.021(3) 0.013(3) 0.004(3) 0.006(3) 0.002(3) C21 0.016(3) 0.021(3) 0.008(3) 0.005(2) 0.005(2) 0.004(2) C22 0.020(3) 0.019(3) 0.014(3) 0.006(3) 0.004(3) 0.002(3) C23 0.041(4) 0.015(3) 0.019(4) 0.007(3) 0.007(3) -0.004(3) C24 0.036(4) 0.017(3) 0.028(4) 0.014(3) 0.009(3) 0.001(3) C25 0.038(4) 0.026(4) 0.017(3) 0.013(3) 0.011(3) 0.006(3) C26 0.040(4) 0.022(4) 0.009(3) 0.006(3) 0.001(3) 0.003(3) C27 0.024(4) 0.016(3) 0.014(3) 0.008(3) 0.006(3) 0.001(3) C28 0.018(3) 0.023(3) 0.015(3) 0.011(3) 0.009(3) 0.003(3) C29 0.023(4) 0.030(4) 0.017(3) 0.013(3) 0.006(3) 0.004(3) C30 0.022(4) 0.051(5) 0.033(4) 0.022(4) 0.001(3) -0.002(4) C31 0.023(4) 0.050(5) 0.039(5) 0.027(4) 0.017(3) 0.020(4) C32 0.035(5) 0.080(8) 0.038(5) 0.012(5) 0.021(4) 0.016(5) C33 0.030(5) 0.074(8) 0.034(5) 0.007(5) 0.003(4) 0.014(5) C34 0.019(4) 0.043(5) 0.020(4) 0.011(3) 0.005(3) 0.006(3) C35 0.057(8) 0.063(6) 0.052(6) 0.026(6) 0.021(6) 0.031(6) Cl1 0.050(3) 0.072(3) 0.137(5) 0.059(4) 0.016(3) 0.005(3) Cl2 0.086(4) 0.067(3) 0.065(3) 0.042(3) 0.043(3) 0.034(3) Cl3 0.216(11) 0.110(6) 0.086(4) 0.075(4) 0.068(5) 0.042(6) C35A 0.045(10) 0.049(8) 0.063(7) 0.023(7) 0.019(9) -0.014(7) Cl1A 0.060(6) 0.077(6) 0.072(7) 0.053(6) -0.017(5) -0.034(5) Cl2A 0.049(5) 0.061(6) 0.069(5) 0.044(5) -0.005(4) -0.018(4) Cl3A 0.045(6) 0.084(6) 0.104(8) 0.040(6) 0.031(6) 0.016(6) _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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 Br1 2.6551(7) . ? Re1 C1 1.888(8) . ? Re1 C2 1.972(7) . ? Re1 C3 1.945(7) . ? Re1 C4 2.118(7) . ? Re1 C11 2.136(7) . ? Re2 Br2 2.6545(7) . ? Re2 C18 1.894(7) . ? Re2 C19 1.973(6) . ? Re2 C20 1.972(7) . ? Re2 C21 2.137(6) . ? Re2 C28 2.145(6) . ? O1 C1 1.168(10) . ? O2 C2 1.137(9) . ? O3 C3 1.152(9) . ? O4 C4 1.353(8) . ? O4 C10 1.398(9) . ? O5 C11 1.357(8) . ? O5 C17 1.397(9) . ? O6 C18 1.147(9) . ? O7 C19 1.151(8) . ? O8 C20 1.138(9) . ? O9 C21 1.361(8) . ? O9 C27 1.390(8) . ? O10 C28 1.345(9) . ? O10 C34 1.399(9) . ? N1 H1 0.8800 . ? N1 C4 1.348(9) . ? N1 C5 1.390(9) . ? N2 H2 0.8800 . ? N2 C11 1.339(9) . ? N2 C12 1.403(9) . ? N3 H3 0.8800 . ? N3 C21 1.318(9) . ? N3 C22 1.372(9) . ? N4 H4 0.8800 . ? N4 C28 1.314(9) . ? N4 C29 1.425(10) . ? C5 C6 1.400(11) . ? C5 C10 1.368(10) . ? C6 H6 0.9500 . ? C6 C7 1.357(13) . ? C7 H7 0.9500 . ? C7 C8 1.408(14) . ? C8 H8 0.9500 . ? C8 C9 1.389(13) . ? C9 H9 0.9500 . ? C9 C10 1.383(11) . ? C12 C13 1.374(11) . ? C12 C17 1.372(10) . ? C13 H13 0.9500 . ? C13 C14 1.389(11) . ? C14 H14 0.9500 . ? C14 C15 1.377(12) . ? C15 H15 0.9500 . ? C15 C16 1.397(14) . ? C16 H16 0.9500 . ? C16 C17 1.375(11) . ? C22 C23 1.381(10) . ? C22 C27 1.390(10) . ? C23 H23 0.9500 . ? C23 C24 1.403(10) . ? C24 H24 0.9500 . ? C24 C25 1.395(11) . ? C25 H25 0.9500 . ? C25 C26 1.398(11) . ? C26 H26 0.9500 . ? C26 C27 1.368(10) . ? C29 C30 1.370(11) . ? C29 C34 1.366(11) . ? C30 H30 0.9500 . ? C30 C31 1.379(13) . ? C31 H31 0.9500 . ? C31 C32 1.378(14) . ? C32 H32 0.9500 . ? C32 C33 1.392(13) . ? C33 H33 0.9500 . ? C33 C34 1.367(13) . ? C35 H35 1.0000 . ? C35 Cl1 1.687(16) . ? C35 Cl2 1.768(15) . ? C35 Cl3 1.749(15) . ? C35A H35A 1.0000 . ? C35A Cl1A 1.765(18) . ? C35A Cl2A 1.744(19) . ? C35A Cl3A 1.748(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Re1 Br1 177.7(2) . . ? C1 Re1 C2 93.5(3) . . ? C1 Re1 C3 90.0(3) . . ? C1 Re1 C4 90.4(3) . . ? C1 Re1 C11 92.8(3) . . ? C2 Re1 Br1 87.4(2) . . ? C2 Re1 C4 91.2(3) . . ? C2 Re1 C11 173.8(3) . . ? C3 Re1 Br1 92.1(2) . . ? C3 Re1 C2 90.0(3) . . ? C3 Re1 C4 178.7(3) . . ? C3 Re1 C11 89.7(3) . . ? C4 Re1 Br1 87.46(18) . . ? C4 Re1 C11 89.1(2) . . ? C11 Re1 Br1 86.37(17) . . ? C18 Re2 Br2 176.1(2) . . ? C18 Re2 C19 88.3(3) . . ? C18 Re2 C20 91.7(3) . . ? C18 Re2 C21 94.0(3) . . ? C18 Re2 C28 89.7(3) . . ? C19 Re2 Br2 95.62(18) . . ? C19 Re2 C21 89.7(2) . . ? C19 Re2 C28 177.4(2) . . ? C20 Re2 Br2 88.4(2) . . ? C20 Re2 C19 89.3(3) . . ? C20 Re2 C21 174.2(3) . . ? C20 Re2 C28 92.4(3) . . ? C21 Re2 Br2 85.93(17) . . ? C21 Re2 C28 88.7(2) . . ? C28 Re2 Br2 86.32(19) . . ? C4 O4 C10 108.4(5) . . ? C11 O5 C17 109.1(5) . . ? C21 O9 C27 108.5(5) . . ? C28 O10 C34 109.0(5) . . ? C4 N1 H1 124.2 . . ? C4 N1 C5 111.6(6) . . ? C5 N1 H1 124.2 . . ? C11 N2 H2 123.8 . . ? C11 N2 C12 112.4(6) . . ? C12 N2 H2 123.8 . . ? C21 N3 H3 123.6 . . ? C21 N3 C22 112.8(6) . . ? C22 N3 H3 123.6 . . ? C28 N4 H4 124.2 . . ? C28 N4 C29 111.5(6) . . ? C29 N4 H4 124.2 . . ? O1 C1 Re1 178.3(7) . . ? O2 C2 Re1 177.4(7) . . ? O3 C3 Re1 178.2(6) . . ? O4 C4 Re1 123.2(5) . . ? N1 C4 Re1 130.1(5) . . ? N1 C4 O4 106.7(6) . . ? N1 C5 C6 134.1(7) . . ? C10 C5 N1 104.5(6) . . ? C10 C5 C6 121.3(7) . . ? C5 C6 H6 121.9 . . ? C7 C6 C5 116.3(8) . . ? C7 C6 H6 121.9 . . ? C6 C7 H7 119.0 . . ? C6 C7 C8 122.0(8) . . ? C8 C7 H7 119.0 . . ? C7 C8 H8 118.9 . . ? C9 C8 C7 122.2(8) . . ? C9 C8 H8 118.9 . . ? C8 C9 H9 122.8 . . ? C10 C9 C8 114.4(8) . . ? C10 C9 H9 122.8 . . ? C5 C10 O4 108.8(6) . . ? C5 C10 C9 123.9(7) . . ? C9 C10 O4 127.3(7) . . ? O5 C11 Re1 126.5(5) . . ? N2 C11 Re1 127.5(5) . . ? N2 C11 O5 106.0(6) . . ? C13 C12 N2 133.7(7) . . ? C17 C12 N2 103.8(6) . . ? C17 C12 C13 122.4(7) . . ? C12 C13 H13 122.0 . . ? C12 C13 C14 116.1(7) . . ? C14 C13 H13 122.0 . . ? C13 C14 H14 119.2 . . ? C15 C14 C13 121.7(8) . . ? C15 C14 H14 119.2 . . ? C14 C15 H15 119.2 . . ? C14 C15 C16 121.7(8) . . ? C16 C15 H15 119.2 . . ? C15 C16 H16 122.1 . . ? C17 C16 C15 115.8(8) . . ? C17 C16 H16 122.1 . . ? C12 C17 O5 108.6(6) . . ? C12 C17 C16 122.2(7) . . ? C16 C17 O5 129.2(7) . . ? O6 C18 Re2 178.2(6) . . ? O7 C19 Re2 175.0(6) . . ? O8 C20 Re2 178.7(7) . . ? O9 C21 Re2 125.1(5) . . ? N3 C21 Re2 128.1(5) . . ? N3 C21 O9 106.8(5) . . ? N3 C22 C23 134.8(7) . . ? N3 C22 C27 104.4(6) . . ? C23 C22 C27 120.8(6) . . ? C22 C23 H23 121.6 . . ? C22 C23 C24 116.9(7) . . ? C24 C23 H23 121.6 . . ? C23 C24 H24 119.3 . . ? C25 C24 C23 121.3(7) . . ? C25 C24 H24 119.3 . . ? C24 C25 H25 119.3 . . ? C24 C25 C26 121.4(7) . . ? C26 C25 H25 119.3 . . ? C25 C26 H26 121.9 . . ? C27 C26 C25 116.1(7) . . ? C27 C26 H26 121.9 . . ? C22 C27 O9 107.5(6) . . ? C26 C27 O9 129.0(6) . . ? C26 C27 C22 123.5(7) . . ? O10 C28 Re2 122.2(5) . . ? N4 C28 Re2 130.2(5) . . ? N4 C28 O10 107.4(6) . . ? C30 C29 N4 133.6(7) . . ? C34 C29 N4 103.7(6) . . ? C34 C29 C30 122.6(7) . . ? C29 C30 H30 122.2 . . ? C29 C30 C31 115.7(8) . . ? C31 C30 H30 122.2 . . ? C30 C31 H31 119.1 . . ? C32 C31 C30 121.7(8) . . ? C32 C31 H31 119.1 . . ? C31 C32 H32 118.9 . . ? C31 C32 C33 122.1(9) . . ? C33 C32 H32 118.9 . . ? C32 C33 H33 122.5 . . ? C34 C33 C32 115.1(9) . . ? C34 C33 H33 122.5 . . ? C29 C34 O10 108.3(6) . . ? C29 C34 C33 122.7(8) . . ? C33 C34 O10 129.0(7) . . ? Cl1 C35 H35 107.0 . . ? Cl1 C35 Cl2 113.9(10) . . ? Cl1 C35 Cl3 111.8(11) . . ? Cl2 C35 H35 107.0 . . ? Cl3 C35 H35 107.0 . . ? Cl3 C35 Cl2 109.7(9) . . ? Cl1A C35A H35A 108.3 . . ? Cl2A C35A H35A 108.3 . . ? Cl2A C35A Cl1A 110.9(13) . . ? Cl2A C35A Cl3A 113.0(16) . . ? Cl3A C35A H35A 108.3 . . ? Cl3A C35A Cl1A 107.9(14) . . ? #===END data_030912a_on _audit_creation_date 2012-03-30 _audit_creation_method ; Olex2 1.1 (compiled 2011.08.18 svn.r1932, GUI svn.r3819) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H18 N4 O4 Re, C H2 Cl2, F6 P' _chemical_formula_sum 'C27 H20 Cl2 F6 N4 O4 P Re' _chemical_formula_weight 866.54 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.0574(7) _cell_length_b 12.3624(8) _cell_length_c 14.8748(10) _cell_angle_alpha 70.632(6) _cell_angle_beta 74.249(6) _cell_angle_gamma 80.300(6) _cell_volume 1506.63(18) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7782 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 71.7210 _cell_measurement_theta_min 3.2348 _exptl_absorpt_coefficient_mu 10.739 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.55101 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 840 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.02 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_unetI/netI 0.0240 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 10728 _diffrn_reflns_theta_full 66.99 _diffrn_reflns_theta_max 66.99 _diffrn_reflns_theta_min 3.24 _diffrn_ambient_temperature 133(2) _diffrn_detector_area_resol_mean 16.1270 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator 'mirror' _diffrn_radiation_type 'CU K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_source_current n/a _diffrn_source_voltage n/a _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5244 _reflns_number_total 5328 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 0.925 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.099 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 470 _refine_ls_number_reflns 5328 _refine_ls_number_restraints 138 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0237 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+1.6407P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.0618 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re -0.035626(13) 0.543434(10) 0.739507(8) 0.01750(6) Uani 1 1 d . . . O1 O -0.3638(3) 0.4915(2) 0.86769(19) 0.0373(6) Uani 1 1 d . . . O2 O -0.0914(3) 0.4129(2) 0.6108(2) 0.0367(6) Uani 1 1 d . . . O3 O 0.0231(3) 0.8222(2) 0.4329(2) 0.0398(6) Uani 1 1 d . . . H3 H 0.0975 0.8231 0.4561 0.060 Uiso 1 1 calc R . . O4 O 0.3151(3) 0.5725(2) 0.66986(16) 0.0240(5) Uani 1 1 d . . . N1 N 0.0339(3) 0.6202(2) 0.83219(18) 0.0222(5) Uani 1 1 d . . . N2 N 0.0926(3) 0.4054(2) 0.82891(19) 0.0229(6) Uani 1 1 d . . . N3 N -0.1612(3) 0.7821(3) 0.6130(2) 0.0274(6) Uani 1 1 d . . . N4 N 0.2168(3) 0.6240(3) 0.5438(2) 0.0259(6) Uani 1 1 d . . . H4 H 0.1493 0.6383 0.5076 0.031 Uiso 1 1 calc R . . C1 C -0.2404(4) 0.5098(3) 0.8234(2) 0.0246(7) Uani 1 1 d . . . C2 C -0.0719(4) 0.4626(3) 0.6597(2) 0.0239(7) Uani 1 1 d . . . C3 C -0.1199(4) 0.6915(3) 0.6594(2) 0.0226(7) Uani 1 1 d . . . C4 C -0.0098(4) 0.7283(3) 0.8373(3) 0.0296(7) Uani 1 1 d . . . H4A H -0.0817 0.7744 0.8009 0.036 Uiso 1 1 calc R . . C5 C 0.0456(5) 0.7751(3) 0.8932(3) 0.0380(9) Uani 1 1 d . . . H5 H 0.0107 0.8510 0.8963 0.046 Uiso 1 1 calc R . . C6 C 0.1533(5) 0.7086(4) 0.9444(3) 0.0423(10) Uani 1 1 d . . . H6 H 0.1945 0.7388 0.9825 0.051 Uiso 1 1 calc R . . C7 C 0.1996(5) 0.5986(4) 0.9395(3) 0.0361(9) Uani 1 1 d . . . H7 H 0.2742 0.5526 0.9736 0.043 Uiso 1 1 calc R . . C8 C 0.1370(4) 0.5547(3) 0.8844(2) 0.0245(7) Uani 1 1 d . . . C9 C 0.1721(4) 0.4356(3) 0.8808(2) 0.0261(7) Uani 1 1 d . . . C10 C 0.2739(4) 0.3562(4) 0.9296(3) 0.0390(9) Uani 1 1 d . . . H10 H 0.3319 0.3794 0.9635 0.047 Uiso 1 1 calc R . . C11 C 0.2907(5) 0.2435(4) 0.9285(3) 0.0460(10) Uani 1 1 d . . . H11 H 0.3609 0.1887 0.9611 0.055 Uiso 1 1 calc R . . C12 C 0.2049(5) 0.2117(4) 0.8799(3) 0.0429(10) Uani 1 1 d . . . H12 H 0.2114 0.1340 0.8803 0.052 Uiso 1 1 calc R . . C13 C 0.1088(4) 0.2949(3) 0.8302(3) 0.0305(7) Uani 1 1 d . . . H13 H 0.0514 0.2730 0.7952 0.037 Uiso 1 1 calc R . . C14 C -0.1850(4) 0.8861(3) 0.5427(2) 0.0258(7) Uani 1 1 d . . . C15 C -0.3033(5) 0.9667(3) 0.5645(3) 0.0356(8) Uani 1 1 d . . . H15 H -0.3696 0.9511 0.6281 0.043 Uiso 1 1 calc R . . C16 C -0.3250(5) 1.0700(3) 0.4937(3) 0.0398(9) Uani 1 1 d . . . H16 H -0.4080 1.1246 0.5078 0.048 Uiso 1 1 calc R . . C17 C -0.2252(5) 1.0931(3) 0.4023(3) 0.0373(9) Uani 1 1 d . . . H17 H -0.2378 1.1648 0.3541 0.045 Uiso 1 1 calc R . . C18 C -0.1066(5) 1.0119(3) 0.3807(3) 0.0349(8) Uani 1 1 d . . . H18 H -0.0384 1.0286 0.3177 0.042 Uiso 1 1 calc R . . C19 C -0.0869(4) 0.9076(3) 0.4496(3) 0.0277(7) Uani 1 1 d . . . C20 C 0.1826(4) 0.5838(3) 0.6408(2) 0.0197(6) Uani 1 1 d . . . C21 C 0.3727(4) 0.6411(3) 0.5060(2) 0.0230(6) Uani 1 1 d . . . C22 C 0.4631(4) 0.6813(3) 0.4128(3) 0.0335(8) Uani 1 1 d . . . H22 H 0.4226 0.7031 0.3561 0.040 Uiso 1 1 calc R . . C23 C 0.6174(4) 0.6879(3) 0.4072(3) 0.0332(8) Uani 1 1 d . . . H23 H 0.6842 0.7157 0.3447 0.040 Uiso 1 1 calc R . . C24 C 0.6766(4) 0.6551(3) 0.4900(3) 0.0353(8) Uani 1 1 d . . . H24 H 0.7827 0.6609 0.4825 0.042 Uiso 1 1 calc R . . C25 C 0.5850(4) 0.6141(4) 0.5834(3) 0.0356(8) Uani 1 1 d . . . H25 H 0.6247 0.5915 0.6404 0.043 Uiso 1 1 calc R . . C26 C 0.4332(4) 0.6083(3) 0.5877(2) 0.0219(6) Uani 1 1 d . . . C27 C 0.4637(6) 0.9046(5) 0.8549(4) 0.0578(13) Uani 1 1 d . . . H27A H 0.4014 0.8969 0.9222 0.069 Uiso 1 1 calc R . . H27B H 0.5464 0.9547 0.8419 0.069 Uiso 1 1 calc R . . Cl1 Cl 0.34659(13) 0.96940(10) 0.77173(9) 0.0515(3) Uani 1 1 d . . . Cl2 Cl 0.54696(13) 0.76804(11) 0.84664(9) 0.0558(3) Uani 1 1 d . . . P1 P 0.7815(8) 0.1033(7) 0.8511(5) 0.0251(10) Uani 0.55 1 d PDU A 1 F1 F 0.8044(9) -0.0249(5) 0.8450(5) 0.0536(16) Uani 0.55 1 d PDU A 1 F2 F 0.7661(9) 0.2306(6) 0.8574(6) 0.0604(18) Uani 0.55 1 d PDU A 1 F3 F 0.6161(7) 0.0829(7) 0.9168(6) 0.0704(18) Uani 0.55 1 d PDU A 1 F4 F 0.7190(9) 0.1419(6) 0.7552(5) 0.0734(16) Uani 0.55 1 d PDU A 1 F5 F 0.9509(6) 0.1224(6) 0.7829(5) 0.0626(15) Uani 0.55 1 d PDU A 1 F6 F 0.8555(9) 0.0628(7) 0.9426(4) 0.0721(18) Uani 0.55 1 d PDU A 1 P1A P 0.7600(12) 0.1069(10) 0.8480(8) 0.0383(18) Uani 0.45 1 d PDU B 2 F1A F 0.7936(13) 0.0042(9) 0.8010(8) 0.081(3) Uani 0.45 1 d PDU B 2 F2A F 0.7242(13) 0.2088(8) 0.8935(7) 0.063(2) Uani 0.45 1 d PDU B 2 F3A F 0.6617(12) 0.0271(8) 0.9423(6) 0.075(2) Uani 0.45 1 d PDU B 2 F4A F 0.6123(10) 0.1466(6) 0.8059(7) 0.0746(19) Uani 0.45 1 d PDU B 2 F5A F 0.8564(14) 0.1870(9) 0.7532(6) 0.101(3) Uani 0.45 1 d PDU B 2 F6A F 0.9092(12) 0.0676(10) 0.8888(11) 0.104(3) Uani 0.45 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01612(9) 0.02299(9) 0.01435(9) -0.00524(6) -0.00444(6) -0.00359(5) O1 0.0218(13) 0.0551(16) 0.0301(13) -0.0070(12) -0.0004(11) -0.0111(11) O2 0.0427(15) 0.0435(15) 0.0378(15) -0.0230(12) -0.0206(12) 0.0000(12) O3 0.0392(15) 0.0454(15) 0.0262(13) -0.0092(11) -0.0055(11) 0.0125(12) O4 0.0177(11) 0.0373(12) 0.0157(10) -0.0045(9) -0.0044(9) -0.0053(9) N1 0.0219(13) 0.0319(14) 0.0127(12) -0.0057(10) -0.0008(10) -0.0095(11) N2 0.0210(13) 0.0278(14) 0.0165(12) -0.0031(10) -0.0022(10) -0.0039(10) N3 0.0276(15) 0.0292(15) 0.0226(14) -0.0037(12) -0.0068(12) -0.0012(12) N4 0.0180(13) 0.0435(16) 0.0167(13) -0.0070(11) -0.0061(10) -0.0049(11) C1 0.0249(18) 0.0287(16) 0.0209(15) -0.0054(13) -0.0078(14) -0.0042(13) C2 0.0219(16) 0.0299(16) 0.0211(15) -0.0065(13) -0.0071(13) -0.0045(13) C3 0.0164(15) 0.0325(18) 0.0213(15) -0.0106(14) -0.0051(12) -0.0019(13) C4 0.0330(19) 0.0315(18) 0.0233(16) -0.0096(14) 0.0023(14) -0.0120(14) C5 0.048(2) 0.041(2) 0.0287(18) -0.0183(16) 0.0061(17) -0.0215(17) C6 0.053(3) 0.058(3) 0.0243(18) -0.0161(17) -0.0009(17) -0.032(2) C7 0.036(2) 0.058(2) 0.0201(16) -0.0090(16) -0.0089(15) -0.0211(17) C8 0.0219(16) 0.0387(18) 0.0125(14) -0.0032(13) -0.0031(12) -0.0127(13) C9 0.0206(16) 0.0405(19) 0.0139(14) -0.0022(13) -0.0021(12) -0.0096(13) C10 0.0288(19) 0.058(2) 0.0245(18) -0.0025(17) -0.0113(15) -0.0003(17) C11 0.043(2) 0.052(2) 0.031(2) -0.0016(17) -0.0135(18) 0.0173(19) C12 0.051(3) 0.037(2) 0.0289(19) -0.0055(16) -0.0036(18) 0.0118(18) C13 0.0341(19) 0.0303(18) 0.0220(16) -0.0079(14) -0.0010(14) 0.0018(14) C14 0.0287(17) 0.0263(16) 0.0223(16) -0.0040(13) -0.0097(14) -0.0031(13) C15 0.036(2) 0.0349(19) 0.0280(18) -0.0074(15) 0.0005(15) 0.0015(15) C16 0.043(2) 0.0315(19) 0.040(2) -0.0111(16) -0.0080(18) 0.0079(16) C17 0.050(2) 0.0261(18) 0.0317(19) -0.0033(15) -0.0114(17) 0.0002(16) C18 0.042(2) 0.0349(19) 0.0226(17) -0.0047(15) -0.0031(15) -0.0049(16) C19 0.0278(17) 0.0320(17) 0.0239(16) -0.0105(14) -0.0060(14) 0.0002(13) C20 0.0191(15) 0.0217(15) 0.0204(15) -0.0075(12) -0.0068(12) -0.0019(11) C21 0.0202(15) 0.0290(16) 0.0203(15) -0.0093(12) -0.0037(12) -0.0019(12) C22 0.0308(19) 0.045(2) 0.0203(16) -0.0065(15) -0.0033(14) -0.0041(15) C23 0.0283(19) 0.0364(19) 0.0279(18) -0.0098(15) 0.0077(15) -0.0074(15) C24 0.0200(17) 0.047(2) 0.038(2) -0.0149(17) 0.0003(15) -0.0077(15) C25 0.0224(18) 0.054(2) 0.0300(19) -0.0106(16) -0.0072(15) -0.0048(16) C26 0.0190(15) 0.0273(16) 0.0181(15) -0.0062(12) -0.0024(12) -0.0031(12) C27 0.057(3) 0.072(3) 0.062(3) -0.041(3) -0.020(2) -0.001(2) Cl1 0.0440(6) 0.0572(6) 0.0538(6) -0.0216(5) -0.0089(5) 0.0004(5) Cl2 0.0422(6) 0.0667(7) 0.0553(7) -0.0189(5) -0.0108(5) 0.0036(5) P1 0.0301(18) 0.0270(16) 0.0170(16) -0.0073(11) -0.0007(12) -0.0055(12) F1 0.046(3) 0.032(2) 0.081(4) -0.020(2) -0.011(3) -0.0007(19) F2 0.056(4) 0.040(3) 0.092(5) -0.033(3) -0.013(3) -0.001(2) F3 0.036(2) 0.095(5) 0.090(4) -0.064(4) 0.028(3) -0.026(3) F4 0.098(4) 0.076(3) 0.055(3) -0.006(3) -0.051(3) -0.003(3) F5 0.044(2) 0.085(4) 0.073(3) -0.060(3) 0.025(2) -0.032(2) F6 0.091(4) 0.083(4) 0.049(3) -0.005(3) -0.043(3) -0.014(3) P1A 0.040(3) 0.039(3) 0.036(3) -0.0127(19) -0.0035(19) -0.009(2) F1A 0.054(4) 0.088(5) 0.118(7) -0.075(5) 0.013(4) -0.017(4) F2A 0.080(6) 0.062(4) 0.061(5) -0.035(4) -0.010(4) -0.019(3) F3A 0.105(5) 0.075(5) 0.044(3) -0.004(3) -0.008(3) -0.049(4) F4A 0.089(4) 0.053(3) 0.102(5) -0.022(3) -0.062(4) 0.002(3) F5A 0.136(6) 0.117(5) 0.053(3) -0.032(3) 0.027(4) -0.087(5) F6A 0.072(4) 0.084(5) 0.182(8) -0.043(5) -0.071(5) -0.004(4) _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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N1 2.177(3) . ? Re1 N2 2.166(3) . ? Re1 C1 1.957(3) . ? Re1 C2 1.904(3) . ? Re1 C3 1.982(3) . ? Re1 C20 2.141(3) . ? O1 C1 1.149(4) . ? O2 C2 1.158(4) . ? O3 H3 0.8400 . ? O3 C19 1.361(4) . ? O4 C20 1.353(4) . ? O4 C26 1.387(4) . ? N1 C4 1.349(5) . ? N1 C8 1.361(4) . ? N2 C9 1.355(4) . ? N2 C13 1.344(5) . ? N3 C3 1.165(5) . ? N3 C14 1.390(4) . ? N4 H4 0.8800 . ? N4 C20 1.326(4) . ? N4 C21 1.394(4) . ? C4 H4A 0.9500 . ? C4 C5 1.386(5) . ? C5 H5 0.9500 . ? C5 C6 1.388(7) . ? C6 H6 0.9500 . ? C6 C7 1.374(6) . ? C7 H7 0.9500 . ? C7 C8 1.393(5) . ? C8 C9 1.468(5) . ? C9 C10 1.388(5) . ? C10 H10 0.9500 . ? C10 C11 1.381(7) . ? C11 H11 0.9500 . ? C11 C12 1.371(7) . ? C12 H12 0.9500 . ? C12 C13 1.380(6) . ? C13 H13 0.9500 . ? C14 C15 1.382(5) . ? C14 C19 1.395(5) . ? C15 H15 0.9500 . ? C15 C16 1.384(5) . ? C16 H16 0.9500 . ? C16 C17 1.382(6) . ? C17 H17 0.9500 . ? C17 C18 1.388(6) . ? C18 H18 0.9500 . ? C18 C19 1.375(5) . ? C21 C22 1.380(5) . ? C21 C26 1.378(5) . ? C22 H22 0.9500 . ? C22 C23 1.392(5) . ? C23 H23 0.9500 . ? C23 C24 1.386(6) . ? C24 H24 0.9500 . ? C24 C25 1.387(5) . ? C25 H25 0.9500 . ? C25 C26 1.372(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 Cl1 1.751(5) . ? C27 Cl2 1.758(5) . ? P1 F1 1.593(9) . ? P1 F2 1.588(9) . ? P1 F3 1.560(8) . ? P1 F4 1.574(8) . ? P1 F5 1.599(8) . ? P1 F6 1.576(8) . ? P1A F1A 1.593(13) . ? P1A F2A 1.568(13) . ? P1A F3A 1.561(12) . ? P1A F4A 1.566(11) . ? P1A F5A 1.557(12) . ? P1A F6A 1.568(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Re1 N1 74.62(11) . . ? C1 Re1 N1 96.22(12) . . ? C1 Re1 N2 96.75(12) . . ? C1 Re1 C3 91.30(14) . . ? C1 Re1 C20 176.80(11) . . ? C2 Re1 N1 172.27(12) . . ? C2 Re1 N2 98.62(13) . . ? C2 Re1 C1 88.22(14) . . ? C2 Re1 C3 91.69(14) . . ? C2 Re1 C20 89.75(13) . . ? C3 Re1 N1 94.52(12) . . ? C3 Re1 N2 167.08(12) . . ? C3 Re1 C20 86.28(13) . . ? C20 Re1 N1 86.07(11) . . ? C20 Re1 N2 86.01(11) . . ? C19 O3 H3 109.5 . . ? C20 O4 C26 108.8(2) . . ? C4 N1 Re1 125.4(2) . . ? C4 N1 C8 118.3(3) . . ? C8 N1 Re1 116.2(2) . . ? C9 N2 Re1 116.8(2) . . ? C13 N2 Re1 124.9(2) . . ? C13 N2 C9 118.1(3) . . ? C3 N3 C14 168.2(3) . . ? C20 N4 H4 124.1 . . ? C20 N4 C21 111.9(3) . . ? C21 N4 H4 124.1 . . ? O1 C1 Re1 175.9(3) . . ? O2 C2 Re1 178.9(3) . . ? N3 C3 Re1 175.2(3) . . ? N1 C4 H4A 118.6 . . ? N1 C4 C5 122.9(4) . . ? C5 C4 H4A 118.6 . . ? C4 C5 H5 120.8 . . ? C4 C5 C6 118.5(4) . . ? C6 C5 H5 120.8 . . ? C5 C6 H6 120.3 . . ? C7 C6 C5 119.3(3) . . ? C7 C6 H6 120.3 . . ? C6 C7 H7 120.1 . . ? C6 C7 C8 119.9(4) . . ? C8 C7 H7 120.1 . . ? N1 C8 C7 121.1(3) . . ? N1 C8 C9 115.6(3) . . ? C7 C8 C9 123.3(3) . . ? N2 C9 C8 115.2(3) . . ? N2 C9 C10 121.1(4) . . ? C10 C9 C8 123.7(3) . . ? C9 C10 H10 120.1 . . ? C11 C10 C9 119.7(4) . . ? C11 C10 H10 120.1 . . ? C10 C11 H11 120.4 . . ? C12 C11 C10 119.2(4) . . ? C12 C11 H11 120.4 . . ? C11 C12 H12 120.7 . . ? C11 C12 C13 118.6(4) . . ? C13 C12 H12 120.7 . . ? N2 C13 C12 123.2(4) . . ? N2 C13 H13 118.4 . . ? C12 C13 H13 118.4 . . ? N3 C14 C19 118.6(3) . . ? C15 C14 N3 120.7(3) . . ? C15 C14 C19 120.7(3) . . ? C14 C15 H15 120.0 . . ? C14 C15 C16 120.0(3) . . ? C16 C15 H15 120.0 . . ? C15 C16 H16 120.3 . . ? C17 C16 C15 119.5(4) . . ? C17 C16 H16 120.3 . . ? C16 C17 H17 119.9 . . ? C16 C17 C18 120.3(3) . . ? C18 C17 H17 119.9 . . ? C17 C18 H18 119.7 . . ? C19 C18 C17 120.7(3) . . ? C19 C18 H18 119.7 . . ? O3 C19 C14 117.1(3) . . ? O3 C19 C18 124.1(3) . . ? C18 C19 C14 118.8(3) . . ? O4 C20 Re1 123.9(2) . . ? N4 C20 Re1 129.1(2) . . ? N4 C20 O4 107.0(3) . . ? C22 C21 N4 134.2(3) . . ? C26 C21 N4 104.2(3) . . ? C26 C21 C22 121.6(3) . . ? C21 C22 H22 122.2 . . ? C21 C22 C23 115.7(3) . . ? C23 C22 H22 122.2 . . ? C22 C23 H23 119.0 . . ? C24 C23 C22 122.1(3) . . ? C24 C23 H23 119.0 . . ? C23 C24 H24 119.1 . . ? C23 C24 C25 121.8(3) . . ? C25 C24 H24 119.1 . . ? C24 C25 H25 122.3 . . ? C26 C25 C24 115.4(3) . . ? C26 C25 H25 122.3 . . ? C21 C26 O4 108.2(3) . . ? C25 C26 O4 128.4(3) . . ? C25 C26 C21 123.4(3) . . ? H27A C27 H27B 107.9 . . ? Cl1 C27 H27A 109.2 . . ? Cl1 C27 H27B 109.2 . . ? Cl1 C27 Cl2 112.1(3) . . ? Cl2 C27 H27A 109.2 . . ? Cl2 C27 H27B 109.2 . . ? F1 P1 F5 88.5(5) . . ? F2 P1 F1 177.6(7) . . ? F2 P1 F5 89.6(5) . . ? F3 P1 F1 90.5(5) . . ? F3 P1 F2 91.4(5) . . ? F3 P1 F4 91.4(6) . . ? F3 P1 F5 179.0(7) . . ? F3 P1 F6 92.3(6) . . ? F4 P1 F1 87.9(5) . . ? F4 P1 F2 93.5(6) . . ? F4 P1 F5 88.1(5) . . ? F4 P1 F6 176.0(7) . . ? F6 P1 F1 90.6(5) . . ? F6 P1 F2 87.8(6) . . ? F6 P1 F5 88.1(5) . . ? F2A P1A F1A 178.9(10) . . ? F2A P1A F6A 89.7(8) . . ? F3A P1A F1A 88.5(8) . . ? F3A P1A F2A 91.4(8) . . ? F3A P1A F4A 88.8(7) . . ? F3A P1A F6A 91.9(9) . . ? F4A P1A F1A 88.4(8) . . ? F4A P1A F2A 90.6(8) . . ? F4A P1A F6A 179.3(11) . . ? F5A P1A F1A 91.4(8) . . ? F5A P1A F2A 88.6(8) . . ? F5A P1A F3A 179.3(10) . . ? F5A P1A F4A 90.5(8) . . ? F5A P1A F6A 88.8(9) . . ? F6A P1A F1A 91.4(8) . . ? #===END data_062113a_on _audit_creation_date 2013-06-24 _audit_creation_method ; Olex2 1.1 (compiled 2011.08.18 svn.r1932, GUI svn.r3819) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H20 Cl2 N4 O3 Re, F6 P' _chemical_formula_sum 'C28 H20 Cl2 F6 N4 O3 P Re' _chemical_formula_weight 862.55 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.2810(12) _cell_length_b 17.0715(7) _cell_length_c 21.2735(18) _cell_angle_alpha 90.00 _cell_angle_beta 114.253(8) _cell_angle_gamma 90.00 _cell_volume 6053.2(7) _cell_formula_units_Z 8 _cell_measurement_reflns_used 8562 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 71.6981 _cell_measurement_theta_min 3.7032 _exptl_absorpt_coefficient_mu 10.663 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.53490 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.893 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 3344 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_unetI/netI 0.0400 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 17089 _diffrn_reflns_theta_full 66.97 _diffrn_reflns_theta_max 66.97 _diffrn_reflns_theta_min 3.71 _diffrn_ambient_temperature 133(2) _diffrn_detector_area_resol_mean 16.1270 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator 'mirror' _diffrn_radiation_type 'CU K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_source_current n/a _diffrn_source_voltage n/a _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4879 _reflns_number_total 5375 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 4.352 _refine_diff_density_min -3.932 _refine_diff_density_rms 0.487 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.235 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 406 _refine_ls_number_reflns 5375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0558 _refine_ls_restrained_S_all 1.235 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1950 _refine_ls_wR_factor_ref 0.2560 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.231404(17) 0.069476(17) 0.080000(15) 0.0192(3) Uani 1 1 d . . . Cl1 Cl -0.14497(12) 0.44278(12) -0.03054(10) 0.0293(5) Uani 1 1 d . . . Cl2 Cl -0.15844(11) 0.12871(13) 0.07751(11) 0.0372(5) Uani 1 1 d . . . P1 P 0.22719(16) 0.81709(13) 0.23848(12) 0.0325(5) Uani 1 1 d . . . F1 F 0.1749(5) 0.7372(6) 0.2308(5) 0.086(3) Uani 1 1 d . . . F2 F 0.2689(9) 0.8957(6) 0.2420(8) 0.123(4) Uani 1 1 d . . . F3 F 0.2776(5) 0.7933(5) 0.3152(4) 0.077(2) Uani 1 1 d . . . F4 F 0.1655(5) 0.8614(4) 0.2634(4) 0.077(2) Uani 1 1 d . . . F5 F 0.2808(6) 0.7711(5) 0.2104(5) 0.084(3) Uani 1 1 d . . . F6 F 0.1715(6) 0.8375(7) 0.1610(4) 0.108(3) Uani 1 1 d . . . O1 O 0.0928(4) -0.0484(4) 0.0382(3) 0.0360(14) Uani 1 1 d . . . O2 O 0.2202(5) 0.0714(3) -0.0695(3) 0.0352(16) Uani 1 1 d . . . O3 O 0.3180(4) 0.0620(3) 0.2352(3) 0.0255(12) Uani 1 1 d . . . N1 N 0.3371(4) 0.1435(5) 0.1163(4) 0.0294(16) Uani 1 1 d . . . N2 N 0.3310(5) -0.0115(5) 0.1181(4) 0.0284(16) Uani 1 1 d . . . N3 N 0.1090(5) 0.2079(5) 0.0301(4) 0.0381(19) Uani 1 1 d . . . N4 N 0.1911(5) 0.0708(3) 0.2138(4) 0.0214(17) Uani 1 1 d . . . C1 C 0.1454(5) -0.0041(5) 0.0527(4) 0.0243(17) Uani 1 1 d . . . C2 C 0.2247(6) 0.0691(4) -0.0127(5) 0.027(2) Uani 1 1 d . . . C3 C 0.1537(5) 0.1546(5) 0.0498(4) 0.0250(17) Uani 1 1 d . . . C4 C 0.2453(6) 0.0695(4) 0.1868(5) 0.021(2) Uani 1 1 d . . . C5 C 0.3158(6) 0.0576(5) 0.3042(4) 0.0310(19) Uani 1 1 d . . . H5A H 0.3468 0.1011 0.3340 0.037 Uiso 1 1 calc R . . H5B H 0.3382 0.0072 0.3270 0.037 Uiso 1 1 calc R . . C6 C 0.2271(5) 0.0642(5) 0.2898(5) 0.030(2) Uani 1 1 d . . . H6A H 0.2077 0.0170 0.3054 0.037 Uiso 1 1 calc R . . H6B H 0.2162 0.1112 0.3118 0.037 Uiso 1 1 calc R . . C7 C 0.1062(5) 0.0851(5) 0.1791(4) 0.0259(15) Uani 1 1 d . . . C8 C 0.0789(5) 0.1607(5) 0.1621(4) 0.0324(17) Uani 1 1 d . . . H8 H 0.1154 0.2032 0.1719 0.039 Uiso 1 1 calc R . . C9 C -0.0042(5) 0.1732(5) 0.1299(4) 0.0339(18) Uani 1 1 d . . . H9 H -0.0242 0.2247 0.1166 0.041 Uiso 1 1 calc R . . C10 C -0.0558(4) 0.1132(5) 0.1176(4) 0.0269(16) Uani 1 1 d . . . C11 C -0.0284(5) 0.0347(5) 0.1346(5) 0.0347(19) Uani 1 1 d . . . H11 H -0.0652 -0.0075 0.1251 0.042 Uiso 1 1 calc R . . C12 C 0.0528(5) 0.0218(5) 0.1650(5) 0.035(2) Uani 1 1 d . . . H12 H 0.0730 -0.0299 0.1766 0.041 Uiso 1 1 calc R . . C13 C 0.0496(5) 0.2650(5) 0.0131(5) 0.0307(18) Uani 1 1 d . . . C14 C 0.0694(4) 0.3398(5) 0.0380(4) 0.0264(15) Uani 1 1 d . . . H14 H 0.1239 0.3536 0.0644 0.032 Uiso 1 1 calc R . . C15 C 0.0092(5) 0.3948(4) 0.0242(4) 0.0257(16) Uani 1 1 d . . . H15 H 0.0217 0.4469 0.0409 0.031 Uiso 1 1 calc R . . C16 C -0.0694(5) 0.3728(5) -0.0142(4) 0.0261(16) Uani 1 1 d . . . C17 C -0.0900(5) 0.2995(5) -0.0407(4) 0.0318(18) Uani 1 1 d . . . H17 H -0.1444 0.2867 -0.0683 0.038 Uiso 1 1 calc R . . C18 C -0.0299(5) 0.2435(5) -0.0267(5) 0.0307(18) Uani 1 1 d . . . H18 H -0.0428 0.1916 -0.0439 0.037 Uiso 1 1 calc R . . C19 C 0.3375(6) 0.2234(6) 0.1156(5) 0.0315(19) Uani 1 1 d . . . H19 H 0.2875 0.2501 0.0979 0.038 Uiso 1 1 calc R . . C20 C 0.4054(6) 0.2661(6) 0.1388(5) 0.036(2) Uani 1 1 d . . . H20 H 0.4025 0.3217 0.1381 0.044 Uiso 1 1 calc R . . C21 C 0.4790(6) 0.2293(6) 0.1636(5) 0.042(2) Uani 1 1 d . . . H21 H 0.5272 0.2591 0.1796 0.050 Uiso 1 1 calc R . . C22 C 0.4815(5) 0.1494(7) 0.1649(5) 0.042(2) Uani 1 1 d . . . H22 H 0.5318 0.1233 0.1819 0.050 Uiso 1 1 calc R . . C23 C 0.4102(5) 0.1051(5) 0.1412(4) 0.0278(17) Uani 1 1 d . . . C24 C 0.4059(5) 0.0213(6) 0.1416(4) 0.0299(19) Uani 1 1 d . . . C25 C 0.4744(6) -0.0290(7) 0.1653(5) 0.037(2) Uani 1 1 d . . . H25 H 0.5266 -0.0070 0.1809 0.044 Uiso 1 1 calc R . . C26 C 0.4657(7) -0.1074(7) 0.1658(5) 0.042(3) Uani 1 1 d . . . H26 H 0.5115 -0.1405 0.1819 0.050 Uiso 1 1 calc R . . C27 C 0.3878(6) -0.1396(6) 0.1421(5) 0.040(2) Uani 1 1 d . . . H27 H 0.3802 -0.1946 0.1423 0.049 Uiso 1 1 calc R . . C28 C 0.3236(6) -0.0898(7) 0.1189(5) 0.033(2) Uani 1 1 d . . . H28 H 0.2713 -0.1116 0.1026 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0186(3) 0.0243(4) 0.0140(3) 0.00010(8) 0.0060(2) 0.00546(9) Cl1 0.0264(10) 0.0383(9) 0.0222(10) 0.0022(7) 0.0088(8) 0.0149(7) Cl2 0.0206(9) 0.0534(12) 0.0374(10) -0.0019(9) 0.0116(8) 0.0038(8) P1 0.0413(11) 0.0296(11) 0.0258(10) 0.0045(8) 0.0131(9) 0.0079(8) F1 0.084(6) 0.080(6) 0.100(7) -0.009(5) 0.043(5) -0.021(5) F2 0.182(11) 0.067(6) 0.191(11) -0.053(7) 0.149(10) -0.059(7) F3 0.063(4) 0.107(7) 0.053(4) 0.015(4) 0.016(4) 0.020(4) F4 0.102(6) 0.059(4) 0.087(5) 0.014(4) 0.056(5) 0.032(4) F5 0.124(7) 0.061(4) 0.113(7) 0.004(4) 0.094(6) 0.020(4) F6 0.114(7) 0.137(9) 0.055(5) 0.030(5) 0.017(5) 0.027(7) O1 0.040(3) 0.036(3) 0.033(3) -0.001(3) 0.016(3) -0.003(3) O2 0.043(4) 0.049(4) 0.015(3) 0.006(2) 0.014(3) 0.009(2) O3 0.024(3) 0.038(3) 0.015(3) -0.0016(19) 0.009(2) 0.003(2) N1 0.028(4) 0.043(4) 0.012(3) 0.003(3) 0.003(3) 0.011(3) N2 0.033(4) 0.041(4) 0.010(3) 0.003(3) 0.007(3) 0.003(3) N3 0.034(4) 0.042(4) 0.037(4) 0.010(3) 0.013(3) 0.026(4) N4 0.021(4) 0.034(4) 0.011(3) 0.000(2) 0.009(3) 0.004(2) C1 0.022(4) 0.032(4) 0.018(4) -0.002(3) 0.007(3) 0.006(3) C2 0.021(4) 0.043(6) 0.024(5) 0.001(3) 0.016(4) 0.009(3) C3 0.027(4) 0.034(4) 0.020(4) -0.002(3) 0.016(3) -0.005(3) C4 0.015(4) 0.034(5) 0.016(4) -0.001(2) 0.008(3) 0.003(2) C5 0.041(5) 0.042(4) 0.011(4) -0.005(3) 0.012(4) -0.009(4) C6 0.030(5) 0.049(5) 0.017(4) 0.000(3) 0.014(4) 0.007(3) C7 0.021(4) 0.034(3) 0.030(4) -0.008(3) 0.018(3) -0.002(3) C8 0.028(4) 0.031(4) 0.040(4) -0.003(3) 0.016(3) -0.001(3) C9 0.027(4) 0.042(5) 0.037(4) -0.007(4) 0.017(3) 0.010(3) C10 0.021(4) 0.041(4) 0.023(3) 0.000(3) 0.013(3) 0.002(3) C11 0.027(4) 0.029(4) 0.043(5) -0.001(4) 0.010(4) -0.005(3) C12 0.029(4) 0.026(4) 0.039(5) 0.002(4) 0.004(4) 0.002(3) C13 0.028(4) 0.030(4) 0.035(4) 0.011(4) 0.013(4) 0.012(3) C14 0.019(3) 0.034(4) 0.024(4) 0.004(3) 0.007(3) 0.009(3) C15 0.026(4) 0.025(4) 0.022(3) -0.001(3) 0.005(3) 0.006(3) C16 0.020(3) 0.039(4) 0.018(3) 0.009(3) 0.007(3) 0.015(3) C17 0.026(4) 0.042(5) 0.025(4) 0.003(3) 0.008(3) 0.007(3) C18 0.038(4) 0.019(3) 0.036(4) 0.001(3) 0.015(4) 0.005(3) C19 0.028(4) 0.040(5) 0.024(4) 0.001(4) 0.009(3) 0.006(4) C20 0.040(5) 0.042(5) 0.027(4) -0.002(4) 0.013(4) -0.009(4) C21 0.037(5) 0.049(6) 0.039(5) -0.007(4) 0.015(4) -0.015(4) C22 0.022(4) 0.074(7) 0.027(4) -0.004(4) 0.009(3) -0.001(4) C23 0.025(4) 0.043(5) 0.018(3) 0.001(3) 0.011(3) 0.004(3) C24 0.027(4) 0.050(5) 0.015(3) 0.001(3) 0.011(3) 0.015(4) C25 0.031(4) 0.051(6) 0.025(4) 0.001(4) 0.008(4) 0.016(4) C26 0.046(6) 0.053(6) 0.029(5) 0.013(4) 0.019(4) 0.034(5) C27 0.052(6) 0.045(5) 0.031(4) 0.009(4) 0.024(4) 0.027(4) C28 0.041(5) 0.038(5) 0.021(4) -0.002(4) 0.013(4) 0.007(5) _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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N1 2.168(8) . ? Re1 N2 2.161(8) . ? Re1 C1 1.908(9) . ? Re1 C2 1.926(10) . ? Re1 C3 1.947(9) . ? Re1 C4 2.181(10) . ? Cl1 C16 1.749(7) . ? Cl2 C10 1.733(7) . ? P1 F1 1.635(9) . ? P1 F2 1.531(9) . ? P1 F3 1.563(7) . ? P1 F4 1.617(7) . ? P1 F5 1.555(7) . ? P1 F6 1.581(8) . ? O1 C1 1.161(11) . ? O2 C2 1.176(13) . ? O3 C4 1.310(11) . ? O3 C5 1.487(10) . ? N1 C19 1.364(13) . ? N1 C23 1.384(11) . ? N2 C24 1.370(12) . ? N2 C28 1.344(13) . ? N3 C3 1.180(12) . ? N3 C13 1.391(10) . ? N4 C4 1.334(13) . ? N4 C6 1.478(11) . ? N4 C7 1.441(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.525(13) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.377(12) . ? C7 C12 1.402(12) . ? C8 H8 0.9500 . ? C8 C9 1.403(11) . ? C9 H9 0.9500 . ? C9 C10 1.344(12) . ? C10 C11 1.424(12) . ? C11 H11 0.9500 . ? C11 C12 1.371(12) . ? C12 H12 0.9500 . ? C13 C14 1.373(13) . ? C13 C18 1.398(12) . ? C14 H14 0.9500 . ? C14 C15 1.384(10) . ? C15 H15 0.9500 . ? C15 C16 1.381(11) . ? C16 C17 1.360(12) . ? C17 H17 0.9500 . ? C17 C18 1.393(11) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C19 C20 1.346(14) . ? C20 H20 0.9500 . ? C20 C21 1.379(15) . ? C21 H21 0.9500 . ? C21 C22 1.366(16) . ? C22 H22 0.9500 . ? C22 C23 1.408(13) . ? C23 C24 1.432(15) . ? C24 C25 1.429(12) . ? C25 H25 0.9500 . ? C25 C26 1.347(18) . ? C26 H26 0.9500 . ? C26 C27 1.413(17) . ? C27 H27 0.9500 . ? C27 C28 1.366(14) . ? C28 H28 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Re1 C4 85.6(3) . . ? N2 Re1 N1 75.5(3) . . ? N2 Re1 C4 83.6(3) . . ? C1 Re1 N1 174.3(3) . . ? C1 Re1 N2 98.9(4) . . ? C1 Re1 C2 89.4(4) . . ? C1 Re1 C3 89.6(4) . . ? C1 Re1 C4 92.6(3) . . ? C2 Re1 N1 92.3(3) . . ? C2 Re1 N2 94.1(3) . . ? C2 Re1 C3 86.2(3) . . ? C2 Re1 C4 177.2(3) . . ? C3 Re1 N1 96.0(3) . . ? C3 Re1 N2 171.5(3) . . ? C3 Re1 C4 95.8(3) . . ? F2 P1 F1 174.8(7) . . ? F2 P1 F3 96.2(7) . . ? F2 P1 F4 88.5(5) . . ? F2 P1 F5 94.6(5) . . ? F2 P1 F6 87.3(8) . . ? F3 P1 F1 87.5(5) . . ? F3 P1 F4 88.3(4) . . ? F3 P1 F6 176.1(6) . . ? F4 P1 F1 88.0(5) . . ? F5 P1 F1 88.6(5) . . ? F5 P1 F3 94.3(5) . . ? F5 P1 F4 175.6(6) . . ? F5 P1 F6 87.0(6) . . ? F6 P1 F1 88.9(6) . . ? F6 P1 F4 90.1(5) . . ? C4 O3 C5 110.5(7) . . ? C19 N1 Re1 126.0(6) . . ? C19 N1 C23 117.9(8) . . ? C23 N1 Re1 116.1(6) . . ? C24 N2 Re1 115.9(6) . . ? C28 N2 Re1 124.6(7) . . ? C28 N2 C24 119.5(8) . . ? C3 N3 C13 170.3(10) . . ? C4 N4 C6 113.2(8) . . ? C4 N4 C7 128.1(8) . . ? C7 N4 C6 118.4(7) . . ? O1 C1 Re1 177.7(7) . . ? O2 C2 Re1 177.8(6) . . ? N3 C3 Re1 176.7(8) . . ? O3 C4 Re1 117.7(6) . . ? O3 C4 N4 110.9(8) . . ? N4 C4 Re1 131.3(7) . . ? O3 C5 H5A 110.8 . . ? O3 C5 H5B 110.8 . . ? O3 C5 C6 104.8(7) . . ? H5A C5 H5B 108.9 . . ? C6 C5 H5A 110.8 . . ? C6 C5 H5B 110.8 . . ? N4 C6 C5 100.6(7) . . ? N4 C6 H6A 111.7 . . ? N4 C6 H6B 111.7 . . ? C5 C6 H6A 111.7 . . ? C5 C6 H6B 111.7 . . ? H6A C6 H6B 109.4 . . ? C8 C7 N4 119.4(7) . . ? C8 C7 C12 121.4(8) . . ? C12 C7 N4 119.2(8) . . ? C7 C8 H8 120.9 . . ? C7 C8 C9 118.2(8) . . ? C9 C8 H8 120.9 . . ? C8 C9 H9 119.6 . . ? C10 C9 C8 120.8(8) . . ? C10 C9 H9 119.6 . . ? C9 C10 Cl2 120.7(7) . . ? C9 C10 C11 121.5(7) . . ? C11 C10 Cl2 117.8(6) . . ? C10 C11 H11 121.0 . . ? C12 C11 C10 118.1(8) . . ? C12 C11 H11 121.0 . . ? C7 C12 H12 120.0 . . ? C11 C12 C7 120.0(8) . . ? C11 C12 H12 120.0 . . ? N3 C13 C18 118.7(8) . . ? C14 C13 N3 119.8(8) . . ? C14 C13 C18 121.4(7) . . ? C13 C14 H14 120.4 . . ? C13 C14 C15 119.2(7) . . ? C15 C14 H14 120.4 . . ? C14 C15 H15 120.5 . . ? C16 C15 C14 119.0(7) . . ? C16 C15 H15 120.5 . . ? C15 C16 Cl1 118.5(6) . . ? C17 C16 Cl1 119.0(6) . . ? C17 C16 C15 122.5(7) . . ? C16 C17 H17 120.5 . . ? C16 C17 C18 118.9(8) . . ? C18 C17 H17 120.5 . . ? C13 C18 H18 120.6 . . ? C17 C18 C13 118.8(8) . . ? C17 C18 H18 120.6 . . ? N1 C19 H19 118.4 . . ? C20 C19 N1 123.2(9) . . ? C20 C19 H19 118.4 . . ? C19 C20 H20 120.0 . . ? C19 C20 C21 120.1(10) . . ? C21 C20 H20 120.0 . . ? C20 C21 H21 120.6 . . ? C22 C21 C20 118.8(9) . . ? C22 C21 H21 120.6 . . ? C21 C22 H22 119.6 . . ? C21 C22 C23 120.8(9) . . ? C23 C22 H22 119.6 . . ? N1 C23 C22 119.3(8) . . ? N1 C23 C24 115.3(7) . . ? C22 C23 C24 125.4(8) . . ? N2 C24 C23 117.1(7) . . ? N2 C24 C25 118.8(9) . . ? C25 C24 C23 124.1(8) . . ? C24 C25 H25 119.6 . . ? C26 C25 C24 120.7(9) . . ? C26 C25 H25 119.6 . . ? C25 C26 H26 120.4 . . ? C25 C26 C27 119.2(8) . . ? C27 C26 H26 120.4 . . ? C26 C27 H27 120.8 . . ? C28 C27 C26 118.5(10) . . ? C28 C27 H27 120.8 . . ? N2 C28 C27 123.2(10) . . ? N2 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? #===END data_042613a_on _audit_creation_date 2013-04-29 _audit_creation_method ; Olex2 1.1 (compiled 2011.08.18 svn.r1932, GUI svn.r3819) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H21 Cl2 N5 O2 Re, F6 P' _chemical_formula_sum 'C28 H21 Cl2 F6 N5 O2 P Re' _chemical_formula_weight 861.58 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 8.9611(3) _cell_length_b 11.5117(5) _cell_length_c 15.4666(7) _cell_angle_alpha 90.121(3) _cell_angle_beta 100.348(3) _cell_angle_gamma 107.215(3) _cell_volume 1496.63(11) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7464 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 71.6033 _cell_measurement_theta_min 4.0239 _exptl_absorpt_coefficient_mu 10.764 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.07260 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description rectangle _exptl_crystal_F_000 836 _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_unetI/netI 0.0386 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 9751 _diffrn_reflns_theta_full 66.98 _diffrn_reflns_theta_max 66.98 _diffrn_reflns_theta_min 4.03 _diffrn_ambient_temperature 133(2) _diffrn_detector_area_resol_mean 16.1270 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator 'mirror' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_source_current n/a _diffrn_source_voltage n/a _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5233 _reflns_number_total 5306 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 2.797 _refine_diff_density_min -1.937 _refine_diff_density_rms 0.230 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 406 _refine_ls_number_reflns 5306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0516 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1054P)^2^+5.9383P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1448 _refine_ls_wR_factor_ref 0.1454 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9639(9) 0.6953(6) 0.0850(4) 0.0258(14) Uani 1 1 d . . . C2 C 0.7487(8) 0.4820(6) 0.0793(4) 0.0243(14) Uani 1 1 d . . . C3 C 0.7293(8) 0.6673(6) 0.1834(4) 0.0213(13) Uani 1 1 d . . . C4 C 1.1051(9) 0.4249(7) 0.1402(5) 0.0313(15) Uani 1 1 d . . . H4 H 1.0208 0.3901 0.0921 0.038 Uiso 1 1 calc R . . C5 C 1.2351(10) 0.3823(7) 0.1530(6) 0.0364(17) Uani 1 1 d . . . H5 H 1.2411 0.3210 0.1137 0.044 Uiso 1 1 calc R . . C6 C 1.3565(10) 0.4303(7) 0.2239(6) 0.0408(18) Uani 1 1 d . . . H6 H 1.4471 0.4018 0.2346 0.049 Uiso 1 1 calc R . . C7 C 1.3447(9) 0.5199(7) 0.2789(5) 0.0312(15) Uani 1 1 d . . . H7 H 1.4255 0.5521 0.3291 0.037 Uiso 1 1 calc R . . C8 C 1.2148(8) 0.5624(6) 0.2606(4) 0.0263(14) Uani 1 1 d . . . C9 C 1.2003(8) 0.6658(6) 0.3127(4) 0.0251(13) Uani 1 1 d . . . C10 C 1.3142(9) 0.7278(7) 0.3843(5) 0.0318(15) Uani 1 1 d . . . H10 H 1.4050 0.7021 0.4052 0.038 Uiso 1 1 calc R . . C11 C 1.2925(10) 0.8282(7) 0.4244(5) 0.0370(17) Uani 1 1 d . . . H11 H 1.3693 0.8719 0.4732 0.044 Uiso 1 1 calc R . . C12 C 1.1604(10) 0.8646(7) 0.3939(5) 0.0360(17) Uani 1 1 d . . . H12 H 1.1452 0.9334 0.4209 0.043 Uiso 1 1 calc R . . C13 C 1.0488(9) 0.7978(6) 0.3222(5) 0.0314(15) Uani 1 1 d . . . H13 H 0.9581 0.8232 0.3003 0.038 Uiso 1 1 calc R . . C14 C 0.5593(9) 0.8054(6) 0.2045(5) 0.0276(15) Uani 1 1 d . . . C15 C 0.6181(9) 0.8882(6) 0.2762(5) 0.0309(15) Uani 1 1 d . . . H15 H 0.7103 0.8863 0.3169 0.037 Uiso 1 1 calc R . . C16 C 0.5428(9) 0.9734(6) 0.2884(5) 0.0308(15) Uani 1 1 d . . . H16 H 0.5818 1.0304 0.3378 0.037 Uiso 1 1 calc R . . C17 C 0.4122(9) 0.9752(6) 0.2293(5) 0.0311(15) Uani 1 1 d . . . C18 C 0.3482(9) 0.8904(6) 0.1566(5) 0.0330(15) Uani 1 1 d . . . H18 H 0.2556 0.8923 0.1163 0.040 Uiso 1 1 calc R . . C19 C 0.4232(9) 0.8045(6) 0.1453(5) 0.0310(15) Uani 1 1 d . . . H19 H 0.3820 0.7453 0.0974 0.037 Uiso 1 1 calc R . . C20 C 0.8099(8) 0.4713(6) 0.2813(4) 0.0219(13) Uani 1 1 d . . . C21 C 0.7471(12) 0.4287(7) 0.4216(5) 0.044(2) Uani 1 1 d . . . H21A H 0.6463 0.4291 0.4392 0.053 Uiso 1 1 calc R . . H21B H 0.8325 0.4453 0.4745 0.053 Uiso 1 1 calc R . . C22 C 0.7296(10) 0.3097(7) 0.3734(5) 0.0358(17) Uani 1 1 d . . . H22A H 0.8012 0.2668 0.4057 0.043 Uiso 1 1 calc R . . H22B H 0.6186 0.2557 0.3644 0.043 Uiso 1 1 calc R . . C23 C 0.7809(8) 0.2605(6) 0.2257(4) 0.0257(13) Uani 1 1 d . . . C24 C 0.6636(9) 0.2226(6) 0.1516(5) 0.0263(14) Uani 1 1 d . . . H24 H 0.5811 0.2598 0.1398 0.032 Uiso 1 1 calc R . . C25 C 0.6654(9) 0.1295(6) 0.0939(4) 0.0275(14) Uani 1 1 d . . . H25 H 0.5854 0.1034 0.0426 0.033 Uiso 1 1 calc R . . C26 C 0.7865(10) 0.0762(6) 0.1132(5) 0.0329(16) Uani 1 1 d . . . C27 C 0.9042(10) 0.1136(8) 0.1871(6) 0.0425(19) Uani 1 1 d . . . H27 H 0.9854 0.0752 0.1997 0.051 Uiso 1 1 calc R . . C28 C 0.9035(9) 0.2068(7) 0.2426(5) 0.0370(17) Uani 1 1 d . . . H28 H 0.9863 0.2348 0.2925 0.044 Uiso 1 1 calc R . . N1 N 1.0908(7) 0.5153(5) 0.1934(4) 0.0214(11) Uani 1 1 d . . . N2 N 1.0657(7) 0.6996(5) 0.2834(4) 0.0234(11) Uani 1 1 d . . . N3 N 0.6386(8) 0.7208(6) 0.1914(4) 0.0328(14) Uani 1 1 d . . . N4 N 0.7888(8) 0.5168(5) 0.3551(4) 0.0344(14) Uani 1 1 d . . . H4A H 0.7991 0.5946 0.3636 0.041 Uiso 1 1 calc R . . N5 N 0.7763(8) 0.3496(5) 0.2875(4) 0.0303(13) Uani 1 1 d . . . O1 O 0.9986(7) 0.7586(5) 0.0313(3) 0.0358(12) Uani 1 1 d . . . O2 O 0.6669(8) 0.4259(5) 0.0190(4) 0.0430(14) Uani 1 1 d . . . Cl1 Cl 0.3190(3) 1.08533(17) 0.24317(17) 0.0477(5) Uani 1 1 d . . . Cl2 Cl 0.7876(3) -0.04196(17) 0.04311(16) 0.0517(6) Uani 1 1 d . . . Re1 Re 0.89091(3) 0.58638(2) 0.176127(15) 0.02025(15) Uani 1 1 d . . . F1 F 0.3467(7) 0.1593(5) 0.4905(3) 0.0524(13) Uani 1 1 d . . . F2 F 0.1278(7) 0.3347(6) 0.4562(4) 0.0583(15) Uani 1 1 d . . . F3 F 0.2642(11) 0.2596(8) 0.3756(4) 0.091(2) Uani 1 1 d . . . F4 F 0.3860(8) 0.3638(6) 0.5032(6) 0.079(2) Uani 1 1 d . . . F5 F 0.2157(12) 0.2459(7) 0.5718(4) 0.094(3) Uani 1 1 d . . . F6 F 0.0850(9) 0.1356(5) 0.4407(6) 0.090(2) Uani 1 1 d . . . P1 P 0.2367(2) 0.24531(18) 0.47265(12) 0.0330(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.042(4) 0.020(3) 0.017(3) 0.002(3) 0.004(3) 0.011(3) C2 0.029(3) 0.014(3) 0.023(3) -0.002(3) -0.006(3) 0.003(3) C3 0.024(3) 0.019(3) 0.026(3) 0.007(2) 0.012(2) 0.010(3) C4 0.036(4) 0.024(3) 0.036(4) -0.003(3) 0.003(3) 0.014(3) C5 0.044(4) 0.026(4) 0.044(4) -0.003(3) 0.011(3) 0.017(3) C6 0.036(4) 0.034(4) 0.058(5) 0.007(4) 0.006(4) 0.022(3) C7 0.034(4) 0.031(4) 0.031(3) 0.008(3) 0.005(3) 0.013(3) C8 0.032(3) 0.021(3) 0.024(3) 0.010(2) 0.008(3) 0.005(3) C9 0.031(3) 0.018(3) 0.025(3) 0.007(2) 0.008(3) 0.003(3) C10 0.030(4) 0.033(4) 0.026(3) 0.002(3) 0.002(3) 0.003(3) C11 0.042(4) 0.030(4) 0.030(4) -0.006(3) 0.008(3) -0.004(3) C12 0.044(4) 0.025(3) 0.035(4) -0.006(3) 0.015(3) 0.002(3) C13 0.039(4) 0.017(3) 0.040(4) -0.002(3) 0.016(3) 0.006(3) C14 0.036(4) 0.020(3) 0.036(4) 0.009(3) 0.019(3) 0.014(3) C15 0.037(4) 0.029(3) 0.028(3) 0.009(3) 0.006(3) 0.012(3) C16 0.042(4) 0.023(3) 0.029(3) 0.002(3) 0.011(3) 0.010(3) C17 0.040(4) 0.018(3) 0.044(4) 0.008(3) 0.021(3) 0.013(3) C18 0.028(4) 0.023(3) 0.045(4) 0.004(3) 0.003(3) 0.006(3) C19 0.036(4) 0.020(3) 0.035(4) 0.000(3) 0.006(3) 0.006(3) C20 0.033(3) 0.020(3) 0.015(3) 0.005(2) 0.009(2) 0.009(3) C21 0.070(6) 0.030(4) 0.027(4) 0.006(3) 0.020(4) -0.001(4) C22 0.053(5) 0.026(3) 0.023(3) 0.008(3) 0.012(3) 0.002(3) C23 0.030(3) 0.015(3) 0.030(3) 0.005(2) 0.008(3) 0.003(2) C24 0.035(4) 0.013(3) 0.030(3) 0.005(2) 0.006(3) 0.007(3) C25 0.039(4) 0.020(3) 0.025(3) 0.003(3) 0.009(3) 0.009(3) C26 0.049(4) 0.014(3) 0.043(4) 0.009(3) 0.025(3) 0.012(3) C27 0.040(4) 0.035(4) 0.063(5) 0.017(4) 0.019(4) 0.020(3) C28 0.032(4) 0.030(4) 0.043(4) 0.011(3) -0.001(3) 0.006(3) N1 0.033(3) 0.015(2) 0.021(3) 0.005(2) 0.013(2) 0.010(2) N2 0.029(3) 0.015(3) 0.022(3) 0.000(2) 0.003(2) 0.003(2) N3 0.041(4) 0.024(3) 0.040(3) 0.009(3) 0.011(3) 0.018(3) N4 0.051(4) 0.018(3) 0.034(3) 0.003(2) 0.013(3) 0.008(3) N5 0.053(4) 0.016(3) 0.019(3) 0.008(2) 0.011(3) 0.003(3) O1 0.053(3) 0.024(2) 0.028(3) 0.007(2) 0.009(2) 0.007(2) O2 0.065(4) 0.022(2) 0.033(3) 0.002(2) -0.001(3) 0.006(3) Cl1 0.0483(11) 0.0264(9) 0.0818(15) 0.0077(9) 0.0283(10) 0.0222(8) Cl2 0.0845(16) 0.0231(8) 0.0641(13) 0.0080(8) 0.0420(12) 0.0249(9) Re1 0.0288(2) 0.01191(19) 0.0217(2) 0.00194(12) 0.00638(13) 0.00772(13) F1 0.060(3) 0.044(3) 0.050(3) -0.009(2) -0.010(2) 0.023(2) F2 0.055(3) 0.063(4) 0.058(3) -0.017(3) -0.008(3) 0.029(3) F3 0.148(7) 0.108(6) 0.049(3) 0.012(4) 0.033(4) 0.080(6) F4 0.055(4) 0.050(4) 0.125(6) -0.004(4) 0.013(4) 0.008(3) F5 0.180(8) 0.101(5) 0.039(3) 0.019(3) 0.036(4) 0.092(6) F6 0.071(4) 0.038(3) 0.141(7) -0.014(4) -0.021(4) 0.011(3) P1 0.0347(10) 0.0374(10) 0.0250(9) -0.0052(7) 0.0023(7) 0.0100(8) _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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.132(9) . ? C1 Re1 1.959(7) . ? C2 O2 1.139(9) . ? C2 Re1 1.926(6) . ? C3 N3 1.178(9) . ? C3 Re1 1.958(6) . ? C4 H4 0.9500 . ? C4 C5 1.376(11) . ? C4 N1 1.375(9) . ? C5 H5 0.9500 . ? C5 C6 1.381(12) . ? C6 H6 0.9500 . ? C6 C7 1.376(11) . ? C7 H7 0.9500 . ? C7 C8 1.377(10) . ? C8 C9 1.486(9) . ? C8 N1 1.354(9) . ? C9 C10 1.391(10) . ? C9 N2 1.377(9) . ? C10 H10 0.9500 . ? C10 C11 1.390(11) . ? C11 H11 0.9500 . ? C11 C12 1.376(12) . ? C12 H12 0.9500 . ? C12 C13 1.402(11) . ? C13 H13 0.9500 . ? C13 N2 1.338(9) . ? C14 C15 1.379(11) . ? C14 C19 1.385(11) . ? C14 N3 1.398(9) . ? C15 H15 0.9500 . ? C15 C16 1.375(11) . ? C16 H16 0.9500 . ? C16 C17 1.355(11) . ? C17 C18 1.407(11) . ? C17 Cl1 1.744(7) . ? C18 H18 0.9500 . ? C18 C19 1.375(11) . ? C19 H19 0.9500 . ? C20 N4 1.322(9) . ? C20 N5 1.350(9) . ? C20 Re1 2.189(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.511(11) . ? C21 N4 1.465(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 N5 1.497(8) . ? C23 C24 1.379(10) . ? C23 C28 1.398(11) . ? C23 N5 1.414(9) . ? C24 H24 0.9500 . ? C24 C25 1.399(9) . ? C25 H25 0.9500 . ? C25 C26 1.387(11) . ? C26 C27 1.379(13) . ? C26 Cl2 1.740(7) . ? C27 H27 0.9500 . ? C27 C28 1.375(13) . ? C28 H28 0.9500 . ? N1 Re1 2.155(6) . ? N2 Re1 2.180(5) . ? N4 H4A 0.8800 . ? F1 P1 1.585(6) . ? F2 P1 1.607(6) . ? F3 P1 1.566(7) . ? F4 P1 1.602(6) . ? F5 P1 1.579(6) . ? F6 P1 1.557(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Re1 176.6(7) . . ? O2 C2 Re1 175.9(6) . . ? N3 C3 Re1 176.1(6) . . ? C5 C4 H4 118.3 . . ? N1 C4 H4 118.3 . . ? N1 C4 C5 123.4(7) . . ? C4 C5 H5 120.6 . . ? C4 C5 C6 118.7(7) . . ? C6 C5 H5 120.6 . . ? C5 C6 H6 120.4 . . ? C7 C6 C5 119.1(7) . . ? C7 C6 H6 120.4 . . ? C6 C7 H7 120.3 . . ? C6 C7 C8 119.4(7) . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 122.4(6) . . ? N1 C8 C7 123.3(6) . . ? N1 C8 C9 114.3(6) . . ? C10 C9 C8 123.9(7) . . ? N2 C9 C8 114.8(6) . . ? N2 C9 C10 121.3(6) . . ? C9 C10 H10 120.7 . . ? C11 C10 C9 118.6(7) . . ? C11 C10 H10 120.7 . . ? C10 C11 H11 119.8 . . ? C12 C11 C10 120.4(7) . . ? C12 C11 H11 119.8 . . ? C11 C12 H12 120.8 . . ? C11 C12 C13 118.4(7) . . ? C13 C12 H12 120.8 . . ? C12 C13 H13 118.8 . . ? N2 C13 C12 122.3(7) . . ? N2 C13 H13 118.8 . . ? C15 C14 C19 121.3(7) . . ? C15 C14 N3 119.4(7) . . ? C19 C14 N3 119.3(7) . . ? C14 C15 H15 120.2 . . ? C16 C15 C14 119.7(7) . . ? C16 C15 H15 120.2 . . ? C15 C16 H16 120.3 . . ? C17 C16 C15 119.3(7) . . ? C17 C16 H16 120.3 . . ? C16 C17 C18 122.1(7) . . ? C16 C17 Cl1 119.4(6) . . ? C18 C17 Cl1 118.5(6) . . ? C17 C18 H18 120.8 . . ? C19 C18 C17 118.3(7) . . ? C19 C18 H18 120.8 . . ? C14 C19 H19 120.3 . . ? C18 C19 C14 119.3(7) . . ? C18 C19 H19 120.3 . . ? N4 C20 N5 107.3(5) . . ? N4 C20 Re1 122.2(5) . . ? N5 C20 Re1 130.4(5) . . ? H21A C21 H21B 109.2 . . ? C22 C21 H21A 111.4 . . ? C22 C21 H21B 111.4 . . ? N4 C21 H21A 111.4 . . ? N4 C21 H21B 111.4 . . ? N4 C21 C22 102.0(6) . . ? C21 C22 H22A 111.2 . . ? C21 C22 H22B 111.2 . . ? H22A C22 H22B 109.1 . . ? N5 C22 C21 102.9(5) . . ? N5 C22 H22A 111.2 . . ? N5 C22 H22B 111.2 . . ? C24 C23 C28 119.9(7) . . ? C24 C23 N5 121.2(6) . . ? C28 C23 N5 118.9(6) . . ? C23 C24 H24 119.9 . . ? C23 C24 C25 120.3(7) . . ? C25 C24 H24 119.9 . . ? C24 C25 H25 120.7 . . ? C26 C25 C24 118.7(7) . . ? C26 C25 H25 120.7 . . ? C25 C26 Cl2 119.0(6) . . ? C27 C26 C25 121.3(7) . . ? C27 C26 Cl2 119.6(6) . . ? C26 C27 H27 120.2 . . ? C28 C27 C26 119.7(7) . . ? C28 C27 H27 120.2 . . ? C23 C28 H28 119.9 . . ? C27 C28 C23 120.1(7) . . ? C27 C28 H28 119.9 . . ? C4 N1 Re1 125.0(5) . . ? C8 N1 C4 115.9(6) . . ? C8 N1 Re1 119.1(4) . . ? C9 N2 Re1 117.0(4) . . ? C13 N2 C9 118.9(6) . . ? C13 N2 Re1 124.1(5) . . ? C3 N3 C14 168.0(7) . . ? C20 N4 C21 115.3(6) . . ? C20 N4 H4A 122.3 . . ? C21 N4 H4A 122.3 . . ? C20 N5 C22 112.2(6) . . ? C20 N5 C23 129.1(5) . . ? C23 N5 C22 118.7(5) . . ? C1 Re1 C20 177.6(2) . . ? C1 Re1 N1 94.3(3) . . ? C1 Re1 N2 94.2(2) . . ? C2 Re1 C1 85.0(3) . . ? C2 Re1 C3 89.5(3) . . ? C2 Re1 C20 96.8(3) . . ? C2 Re1 N1 101.5(3) . . ? C2 Re1 N2 175.8(2) . . ? C3 Re1 C1 89.4(3) . . ? C3 Re1 C20 89.1(3) . . ? C3 Re1 N1 168.6(2) . . ? C3 Re1 N2 94.6(3) . . ? N1 Re1 C20 86.8(2) . . ? N1 Re1 N2 74.4(2) . . ? N2 Re1 C20 84.1(2) . . ? F1 P1 F2 178.7(3) . . ? F1 P1 F4 91.3(3) . . ? F3 P1 F1 91.4(4) . . ? F3 P1 F2 89.2(4) . . ? F3 P1 F4 89.4(5) . . ? F3 P1 F5 174.0(5) . . ? F4 P1 F2 87.6(3) . . ? F5 P1 F1 91.9(4) . . ? F5 P1 F2 87.4(4) . . ? F5 P1 F4 85.5(5) . . ? F6 P1 F1 92.3(3) . . ? F6 P1 F2 88.8(3) . . ? F6 P1 F3 89.8(5) . . ? F6 P1 F4 176.3(4) . . ? F6 P1 F5 95.0(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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 C5 C6 C7 -0.7(12) . . . . ? C4 N1 Re1 C1 -81.2(6) . . . . ? C4 N1 Re1 C2 4.6(6) . . . . ? C4 N1 Re1 C3 170.1(10) . . . . ? C4 N1 Re1 C20 100.9(6) . . . . ? C4 N1 Re1 N2 -174.3(6) . . . . ? C5 C4 N1 C8 0.5(10) . . . . ? C5 C4 N1 Re1 179.6(6) . . . . ? C5 C6 C7 C8 -2.1(12) . . . . ? C6 C7 C8 C9 -174.9(7) . . . . ? C6 C7 C8 N1 4.3(11) . . . . ? C7 C8 C9 C10 -0.5(10) . . . . ? C7 C8 C9 N2 177.7(6) . . . . ? C7 C8 N1 C4 -3.4(9) . . . . ? C7 C8 N1 Re1 177.4(5) . . . . ? C8 C9 C10 C11 175.9(6) . . . . ? C8 C9 N2 C13 -174.9(6) . . . . ? C8 C9 N2 Re1 5.7(7) . . . . ? C8 N1 Re1 C1 97.9(5) . . . . ? C8 N1 Re1 C2 -176.3(5) . . . . ? C8 N1 Re1 C3 -10.8(13) . . . . ? C8 N1 Re1 C20 -80.0(5) . . . . ? C8 N1 Re1 N2 4.8(4) . . . . ? C9 C8 N1 C4 175.8(6) . . . . ? C9 C8 N1 Re1 -3.3(7) . . . . ? C9 C10 C11 C12 0.3(11) . . . . ? C9 N2 Re1 C1 -98.9(5) . . . . ? C9 N2 Re1 C2 -20(3) . . . . ? C9 N2 Re1 C3 171.4(5) . . . . ? C9 N2 Re1 C20 82.8(5) . . . . ? C9 N2 Re1 N1 -5.6(4) . . . . ? C10 C9 N2 C13 3.3(9) . . . . ? C10 C9 N2 Re1 -176.1(5) . . . . ? C10 C11 C12 C13 0.4(11) . . . . ? C11 C12 C13 N2 0.8(11) . . . . ? C12 C13 N2 C9 -2.6(10) . . . . ? C12 C13 N2 Re1 176.7(5) . . . . ? C13 N2 Re1 C1 81.7(6) . . . . ? C13 N2 Re1 C2 161(3) . . . . ? C13 N2 Re1 C3 -8.0(6) . . . . ? C13 N2 Re1 C20 -96.6(6) . . . . ? C13 N2 Re1 N1 175.0(6) . . . . ? C14 C15 C16 C17 -0.5(10) . . . . ? C15 C14 C19 C18 2.1(11) . . . . ? C15 C14 N3 C3 -46(4) . . . . ? C15 C16 C17 C18 1.7(11) . . . . ? C15 C16 C17 Cl1 -178.5(5) . . . . ? C16 C17 C18 C19 -0.9(11) . . . . ? C17 C18 C19 C14 -0.9(11) . . . . ? C19 C14 C15 C16 -1.4(11) . . . . ? C19 C14 N3 C3 134(3) . . . . ? C21 C22 N5 C20 -2.5(9) . . . . ? C21 C22 N5 C23 177.2(7) . . . . ? C22 C21 N4 C20 -5.0(10) . . . . ? C23 C24 C25 C26 0.4(10) . . . . ? C24 C23 C28 C27 -2.2(10) . . . . ? C24 C23 N5 C20 -75.4(10) . . . . ? C24 C23 N5 C22 105.0(8) . . . . ? C24 C25 C26 C27 -0.4(10) . . . . ? C24 C25 C26 Cl2 178.6(5) . . . . ? C25 C26 C27 C28 -0.9(11) . . . . ? C26 C27 C28 C23 2.2(11) . . . . ? C28 C23 C24 C25 0.9(10) . . . . ? C28 C23 N5 C20 107.3(9) . . . . ? C28 C23 N5 C22 -72.3(9) . . . . ? N1 C4 C5 C6 1.5(12) . . . . ? N1 C8 C9 C10 -179.7(6) . . . . ? N1 C8 C9 N2 -1.6(8) . . . . ? N2 C9 C10 C11 -2.1(10) . . . . ? N3 C3 Re1 C1 -87(9) . . . . ? N3 C3 Re1 C2 -172(9) . . . . ? N3 C3 Re1 C20 91(9) . . . . ? N3 C3 Re1 N1 22(9) . . . . ? N3 C3 Re1 N2 7(9) . . . . ? N3 C14 C15 C16 178.5(6) . . . . ? N3 C14 C19 C18 -177.8(7) . . . . ? N4 C20 N5 C22 -0.5(9) . . . . ? N4 C20 N5 C23 179.9(7) . . . . ? N4 C20 Re1 C1 1(6) . . . . ? N4 C20 Re1 C2 -138.1(6) . . . . ? N4 C20 Re1 C3 -48.7(6) . . . . ? N4 C20 Re1 N1 120.7(6) . . . . ? N4 C20 Re1 N2 46.0(6) . . . . ? N4 C21 C22 N5 4.0(9) . . . . ? N5 C20 N4 C21 3.6(9) . . . . ? N5 C20 Re1 C1 -177(6) . . . . ? N5 C20 Re1 C2 43.5(7) . . . . ? N5 C20 Re1 C3 132.9(7) . . . . ? N5 C20 Re1 N1 -57.7(7) . . . . ? N5 C20 Re1 N2 -132.3(7) . . . . ? N5 C23 C24 C25 -176.4(6) . . . . ? N5 C23 C28 C27 175.1(7) . . . . ? O1 C1 Re1 C2 61(10) . . . . ? O1 C1 Re1 C3 -28(10) . . . . ? O1 C1 Re1 C20 -78(12) . . . . ? O1 C1 Re1 N1 162(10) . . . . ? O1 C1 Re1 N2 -123(10) . . . . ? O2 C2 Re1 C1 -13(10) . . . . ? O2 C2 Re1 C3 77(10) . . . . ? O2 C2 Re1 C20 166(10) . . . . ? O2 C2 Re1 N1 -106(10) . . . . ? O2 C2 Re1 N2 -92(10) . . . . ? Cl1 C17 C18 C19 179.2(6) . . . . ? Cl2 C26 C27 C28 -179.9(6) . . . . ? Re1 C3 N3 C14 30(11) . . . . ? Re1 C20 N4 C21 -175.1(6) . . . . ? Re1 C20 N5 C22 178.1(5) . . . . ? Re1 C20 N5 C23 -1.5(12) . . . . ? #===END data_070913a_on _audit_creation_date 2013-07-17 _audit_creation_method ; Olex2 1.1 (compiled 2011.08.18 svn.r1932, GUI svn.r3819) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H20 Cl2 N4 O2 Re S, C0.25 Cl0.5, F6 P' _chemical_formula_sum 'C28.25 H20.50 Cl2.50 F6 N4 O2 P Re S' _chemical_formula_weight 899.84 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 17.2744(7) _cell_length_b 9.8309(3) _cell_length_c 20.7285(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.302(4) _cell_angle_gamma 90.00 _cell_volume 3256.9(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6872 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 71.5173 _cell_measurement_theta_min 4.2163 _exptl_absorpt_coefficient_mu 10.868 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.21895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1746 _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.01 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_unetI/netI 0.0314 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 13664 _diffrn_reflns_theta_full 71.65 _diffrn_reflns_theta_max 71.65 _diffrn_reflns_theta_min 4.39 _diffrn_ambient_temperature 133(2) _diffrn_detector_area_resol_mean 16.1270 _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -20.00 23.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 37.0000 150.0000 43 #__ type_ start__ end____ width___ exp.time_ 2 omega 39.00 66.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 37.0000 150.0000 27 #__ type_ start__ end____ width___ exp.time_ 3 omega -24.00 31.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 -99.0000 0.0000 55 #__ type_ start__ end____ width___ exp.time_ 4 omega 98.00 125.00 1.0000 16.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 125.0000 -150.0000 27 #__ type_ start__ end____ width___ exp.time_ 5 omega -9.00 75.00 1.0000 16.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 -57.0000 120.0000 84 #__ type_ start__ end____ width___ exp.time_ 6 omega 90.00 117.00 1.0000 16.0000 omega____ theta____ kappa____ phi______ frames - 55.0000 88.0000 -110.0000 27 #__ type_ start__ end____ width___ exp.time_ 7 omega -71.00 7.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 25.0000 -30.0000 78 #__ type_ start__ end____ width___ exp.time_ 8 omega -137.00 -30.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - -64.0000 -25.0000 -30.0000 107 #__ type_ start__ end____ width___ exp.time_ 9 omega 53.00 90.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -111.0000 150.0000 37 #__ type_ start__ end____ width___ exp.time_ 10 omega 38.00 66.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -37.0000 60.0000 28 #__ type_ start__ end____ width___ exp.time_ 11 omega 37.00 69.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 0.0000 32 #__ type_ start__ end____ width___ exp.time_ 12 omega 41.00 68.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 60.0000 27 #__ type_ start__ end____ width___ exp.time_ 13 omega 38.00 65.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -37.0000 -60.0000 27 #__ type_ start__ end____ width___ exp.time_ 14 omega 41.00 69.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -37.0000 150.0000 28 #__ type_ start__ end____ width___ exp.time_ 15 omega 38.00 65.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 120.0000 27 #__ type_ start__ end____ width___ exp.time_ 16 omega 45.00 80.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 -90.0000 35 #__ type_ start__ end____ width___ exp.time_ 17 omega 90.00 125.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 63.0000 30.0000 35 #__ type_ start__ end____ width___ exp.time_ 18 omega 37.00 62.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 -150.0000 25 #__ type_ start__ end____ width___ exp.time_ 19 omega 135.00 178.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 63.0000 30.0000 43 #__ type_ start__ end____ width___ exp.time_ 20 omega 53.00 78.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -111.0000 0.0000 25 #__ type_ start__ end____ width___ exp.time_ 21 omega 38.00 67.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -37.0000 -120.0000 29 #__ type_ start__ end____ width___ exp.time_ 22 omega 37.00 70.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -25.0000 90.0000 33 #__ type_ start__ end____ width___ exp.time_ 23 omega 44.00 80.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -50.0000 -30.0000 36 #__ type_ start__ end____ width___ exp.time_ 24 omega 42.00 130.00 1.0000 32.0000 omega____ theta____ kappa____ phi______ frames - 110.0000 -63.0000 120.0000 88 ; _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0565268000 _diffrn_orient_matrix_UB_12 -0.0564194000 _diffrn_orient_matrix_UB_13 -0.0718016000 _diffrn_orient_matrix_UB_21 -0.0778380000 _diffrn_orient_matrix_UB_22 0.0279785000 _diffrn_orient_matrix_UB_23 0.0172884000 _diffrn_orient_matrix_UB_31 -0.0071700000 _diffrn_orient_matrix_UB_32 0.1433167000 _diffrn_orient_matrix_UB_33 -0.0316435000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_source_current n/a _diffrn_source_voltage n/a _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 5759 _reflns_number_total 6230 _reflns_odcompleteness_completeness 99.91 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 3.686 _refine_diff_density_min -1.690 _refine_diff_density_rms 0.162 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 414 _refine_ls_number_reflns 6230 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0541 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+25.0248P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1416 _refine_ls_wR_factor_ref 0.1450 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.304668(17) 0.26909(3) 0.244728(15) 0.03144(13) Uani 1 1 d . . . Cl1 Cl -0.09496(14) -0.2874(3) -0.02960(12) 0.0591(6) Uani 1 1 d . . . Cl1S Cl 0.4750(4) 0.1233(7) 0.4649(4) 0.0881(17) Uiso 0.50 1 d PD . . Cl2 Cl 0.40363(19) 0.8651(4) 0.10078(16) 0.1092(15) Uani 1 1 d . . . S1 S 0.10581(11) 0.33057(19) 0.22240(10) 0.0391(4) Uani 1 1 d . . . P1 P 0.17550(14) 0.7497(2) 0.37257(11) 0.0455(5) Uani 1 1 d . . . F1 F 0.0830(4) 0.6909(8) 0.3461(4) 0.089(2) Uani 1 1 d . . . F2 F 0.2014(3) 0.6339(6) 0.3306(3) 0.0574(13) Uani 1 1 d . . . F3 F 0.1485(4) 0.8646(6) 0.4149(3) 0.0674(15) Uani 1 1 d . . . F4 F 0.1493(5) 0.8474(7) 0.3075(3) 0.083(2) Uani 1 1 d . . . F5 F 0.2670(4) 0.8068(9) 0.4005(4) 0.102(3) Uani 1 1 d . . . F6 F 0.2013(5) 0.6533(8) 0.4389(3) 0.096(2) Uani 1 1 d . . . O1 O 0.4495(4) 0.0606(7) 0.2983(4) 0.067(2) Uani 1 1 d . . . O2 O 0.3536(5) 0.3082(10) 0.1187(3) 0.079(2) Uani 1 1 d . . . N1 N 0.2868(4) 0.2623(6) 0.3431(3) 0.0376(14) Uani 1 1 d . . . N2 N 0.3747(3) 0.4393(6) 0.3040(3) 0.0355(13) Uani 1 1 d . . . N3 N 0.1787(4) 0.0380(7) 0.1654(4) 0.0473(17) Uani 1 1 d . . . N4 N 0.1752(3) 0.5181(6) 0.1828(3) 0.0319(12) Uani 1 1 d . . . C1 C 0.3974(4) 0.1394(9) 0.2796(4) 0.046(2) Uani 1 1 d . . . C1S C 0.5616(16) 0.011(3) 0.4982(18) 0.052(8) Uiso 0.25 1 d PD . . C2 C 0.3321(5) 0.2942(11) 0.1648(5) 0.057(2) Uani 1 1 d . . . C3 C 0.2270(4) 0.1199(7) 0.1954(4) 0.0372(16) Uani 1 1 d . . . C4 C 0.1927(4) 0.3962(7) 0.2108(3) 0.0275(13) Uani 1 1 d . . . C5 C 0.0442(5) 0.4857(9) 0.1975(5) 0.050(2) Uani 1 1 d . . . H5A H -0.0135 0.4656 0.1647 0.059 Uiso 1 1 calc R . . H5B H 0.0415 0.5321 0.2390 0.059 Uiso 1 1 calc R . . C6 C 0.0895(5) 0.5719(9) 0.1632(5) 0.0462(19) Uani 1 1 d . . . H6A H 0.0598 0.5690 0.1119 0.055 Uiso 1 1 calc R . . H6B H 0.0915 0.6675 0.1786 0.055 Uiso 1 1 calc R . . C7 C 0.2446(5) 0.1665(9) 0.3612(4) 0.0481(19) Uani 1 1 d . . . H7 H 0.2234 0.0905 0.3314 0.058 Uiso 1 1 calc R . . C8 C 0.2310(6) 0.1759(12) 0.4235(5) 0.064(3) Uani 1 1 d . . . H8 H 0.2012 0.1066 0.4362 0.077 Uiso 1 1 calc R . . C9 C 0.2613(8) 0.2872(13) 0.4659(5) 0.071(3) Uani 1 1 d . . . H9 H 0.2513 0.2955 0.5077 0.086 Uiso 1 1 calc R . . C10 C 0.3042(7) 0.3826(12) 0.4490(5) 0.063(3) Uani 1 1 d . . . H10 H 0.3251 0.4595 0.4783 0.076 Uiso 1 1 calc R . . C11 C 0.3185(5) 0.3680(8) 0.3866(4) 0.0399(17) Uani 1 1 d . . . C12 C 0.3684(5) 0.4663(8) 0.3663(4) 0.0406(17) Uani 1 1 d . . . C13 C 0.4107(6) 0.5769(11) 0.4062(6) 0.067(3) Uani 1 1 d . . . H13 H 0.4067 0.5962 0.4497 0.080 Uiso 1 1 calc R . . C14 C 0.4595(6) 0.6594(10) 0.3810(7) 0.076(4) Uani 1 1 d . . . H14 H 0.4881 0.7359 0.4073 0.091 Uiso 1 1 calc R . . C15 C 0.4657(5) 0.6303(10) 0.3192(6) 0.066(3) Uani 1 1 d . . . H15 H 0.4990 0.6853 0.3022 0.079 Uiso 1 1 calc R . . C16 C 0.4232(5) 0.5205(9) 0.2816(5) 0.053(2) Uani 1 1 d . . . H16 H 0.4278 0.5004 0.2384 0.064 Uiso 1 1 calc R . . C17 C 0.1133(5) -0.0402(7) 0.1201(4) 0.0398(17) Uani 1 1 d . . . C18 C 0.1237(5) -0.1014(8) 0.0627(4) 0.0436(18) Uani 1 1 d . . . H18 H 0.1745 -0.0911 0.0554 0.052 Uiso 1 1 calc R . . C19 C 0.0580(5) -0.1778(8) 0.0169(4) 0.0425(17) Uani 1 1 d . . . H19 H 0.0632 -0.2206 -0.0223 0.051 Uiso 1 1 calc R . . C20 C -0.0141(5) -0.1905(8) 0.0288(4) 0.0412(17) Uani 1 1 d . . . C21 C -0.0250(5) -0.1287(9) 0.0839(4) 0.0432(17) Uani 1 1 d . . . H21 H -0.0764 -0.1376 0.0903 0.052 Uiso 1 1 calc R . . C22 C 0.0398(5) -0.0532(8) 0.1301(4) 0.0452(19) Uani 1 1 d . . . H22 H 0.0333 -0.0102 0.1688 0.054 Uiso 1 1 calc R . . C23 C 0.2326(4) 0.6008(8) 0.1639(4) 0.0369(16) Uani 1 1 d . . . C24 C 0.2704(5) 0.7113(8) 0.2052(5) 0.0456(19) Uani 1 1 d . . . H24 H 0.2608 0.7308 0.2464 0.055 Uiso 1 1 calc R . . C25 C 0.3233(6) 0.7938(9) 0.1844(5) 0.059(3) Uani 1 1 d . . . H25 H 0.3501 0.8704 0.2118 0.070 Uiso 1 1 calc R . . C26 C 0.3358(6) 0.7637(11) 0.1252(5) 0.065(3) Uani 1 1 d . . . C27 C 0.2969(6) 0.6557(13) 0.0836(5) 0.067(3) Uani 1 1 d . . . H27 H 0.3063 0.6369 0.0422 0.080 Uiso 1 1 calc R . . C28 C 0.2442(5) 0.5753(10) 0.1028(4) 0.049(2) Uani 1 1 d . . . H28 H 0.2156 0.5017 0.0738 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02598(18) 0.0352(2) 0.02928(18) -0.00569(11) 0.00615(12) 0.00290(11) Cl1 0.0535(12) 0.0669(14) 0.0483(11) -0.0223(10) 0.0093(9) -0.0191(10) Cl2 0.0735(17) 0.144(3) 0.0766(18) 0.058(2) -0.0095(14) -0.063(2) S1 0.0310(8) 0.0402(10) 0.0483(10) 0.0074(8) 0.0177(7) 0.0015(7) P1 0.0409(11) 0.0532(12) 0.0408(10) -0.0040(9) 0.0136(9) 0.0077(9) F1 0.058(4) 0.096(5) 0.118(6) -0.034(4) 0.041(4) -0.010(3) F2 0.060(3) 0.066(3) 0.050(3) -0.009(2) 0.024(2) 0.012(3) F3 0.070(3) 0.073(4) 0.059(3) -0.015(3) 0.025(3) 0.016(3) F4 0.117(5) 0.080(4) 0.058(3) 0.015(3) 0.039(4) 0.028(4) F5 0.047(3) 0.124(6) 0.128(6) -0.058(5) 0.026(4) -0.008(4) F6 0.146(7) 0.092(5) 0.056(3) 0.013(3) 0.046(4) 0.047(5) O1 0.053(4) 0.072(5) 0.061(4) -0.016(3) 0.003(3) 0.029(3) O2 0.069(4) 0.144(7) 0.036(3) 0.011(4) 0.034(3) 0.031(5) N1 0.036(3) 0.036(3) 0.036(3) 0.009(2) 0.008(3) 0.004(2) N2 0.025(3) 0.033(3) 0.041(3) 0.000(2) 0.004(2) 0.001(2) N3 0.043(4) 0.040(4) 0.048(4) -0.012(3) 0.004(3) 0.005(3) N4 0.028(3) 0.034(3) 0.032(3) 0.002(2) 0.010(2) 0.001(2) C1 0.025(3) 0.056(5) 0.048(4) -0.012(4) 0.002(3) 0.018(3) C2 0.038(4) 0.074(6) 0.048(5) -0.003(4) 0.005(4) 0.018(4) C3 0.029(3) 0.034(4) 0.039(4) -0.015(3) 0.002(3) 0.005(3) C4 0.022(3) 0.034(3) 0.025(3) -0.003(3) 0.008(2) 0.001(2) C5 0.034(4) 0.045(5) 0.068(6) 0.010(4) 0.018(4) 0.008(3) C6 0.037(4) 0.041(4) 0.057(5) 0.009(4) 0.014(4) 0.010(3) C7 0.050(5) 0.050(5) 0.046(4) 0.014(4) 0.020(4) 0.004(4) C8 0.061(6) 0.074(7) 0.064(6) 0.035(5) 0.030(5) 0.012(5) C9 0.078(7) 0.095(9) 0.043(5) 0.010(5) 0.026(5) 0.018(6) C10 0.070(6) 0.082(7) 0.038(4) -0.001(5) 0.021(4) 0.018(5) C11 0.039(4) 0.048(4) 0.031(3) -0.003(3) 0.011(3) 0.011(3) C12 0.036(4) 0.035(4) 0.042(4) -0.009(3) 0.004(3) 0.006(3) C13 0.056(5) 0.056(6) 0.070(6) -0.027(5) 0.004(5) 0.004(5) C14 0.046(5) 0.042(5) 0.109(9) -0.020(6) -0.004(6) -0.011(4) C15 0.035(4) 0.047(5) 0.101(8) 0.005(5) 0.010(5) -0.010(4) C16 0.025(4) 0.051(5) 0.076(6) 0.012(4) 0.011(4) -0.006(3) C17 0.040(4) 0.031(4) 0.036(4) -0.007(3) 0.001(3) 0.005(3) C18 0.039(4) 0.041(4) 0.046(4) -0.006(3) 0.010(3) -0.001(3) C19 0.047(4) 0.039(4) 0.033(4) -0.011(3) 0.005(3) 0.000(3) C20 0.039(4) 0.038(4) 0.036(4) -0.005(3) 0.003(3) -0.003(3) C21 0.036(4) 0.051(5) 0.037(4) -0.003(3) 0.009(3) 0.002(3) C22 0.045(4) 0.043(4) 0.040(4) -0.010(3) 0.007(3) 0.010(3) C23 0.031(3) 0.038(4) 0.036(4) 0.007(3) 0.006(3) -0.001(3) C24 0.044(4) 0.028(4) 0.051(5) 0.002(3) 0.003(4) -0.004(3) C25 0.050(5) 0.039(5) 0.064(6) 0.009(4) -0.005(4) -0.010(4) C26 0.045(5) 0.079(7) 0.049(5) 0.032(5) -0.004(4) -0.024(5) C27 0.045(5) 0.104(9) 0.041(5) 0.020(5) 0.004(4) -0.024(5) C28 0.041(4) 0.065(6) 0.035(4) 0.002(4) 0.007(3) -0.019(4) _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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N1 2.176(7) . ? Re1 N2 2.155(6) . ? Re1 C1 1.958(7) . ? Re1 C2 1.905(10) . ? Re1 C3 1.989(7) . ? Re1 C4 2.183(6) . ? Cl1 C20 1.744(7) . ? Cl1S C1S 1.777(10) . ? Cl1S C1S 1.76(4) 3_656 ? Cl2 C26 1.753(9) . ? S1 C4 1.732(7) . ? S1 C5 1.819(8) . ? P1 F1 1.588(7) . ? P1 F2 1.596(5) . ? P1 F3 1.603(6) . ? P1 F4 1.576(6) . ? P1 F5 1.567(7) . ? P1 F6 1.588(7) . ? O1 C1 1.139(9) . ? O2 C2 1.157(12) . ? N1 C7 1.329(10) . ? N1 C11 1.348(10) . ? N2 C12 1.363(10) . ? N2 C16 1.359(10) . ? N3 C3 1.157(10) . ? N3 C17 1.394(9) . ? N4 C4 1.316(9) . ? N4 C6 1.476(9) . ? N4 C23 1.448(9) . ? C1S Cl1S 1.76(4) 3_656 ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.503(12) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7 0.9500 . ? C7 C8 1.401(13) . ? C8 H8 0.9500 . ? C8 C9 1.377(17) . ? C9 H9 0.9500 . ? C9 C10 1.323(16) . ? C10 H10 0.9500 . ? C10 C11 1.413(11) . ? C11 C12 1.459(12) . ? C12 C13 1.393(12) . ? C13 H13 0.9500 . ? C13 C14 1.405(17) . ? C14 H14 0.9500 . ? C14 C15 1.355(17) . ? C15 H15 0.9500 . ? C15 C16 1.370(13) . ? C16 H16 0.9500 . ? C17 C18 1.403(11) . ? C17 C22 1.369(12) . ? C18 H18 0.9500 . ? C18 C19 1.392(10) . ? C19 H19 0.9500 . ? C19 C20 1.365(12) . ? C20 C21 1.367(11) . ? C21 H21 0.9500 . ? C21 C22 1.381(11) . ? C22 H22 0.9500 . ? C23 C24 1.383(11) . ? C23 C28 1.378(11) . ? C24 H24 0.9500 . ? C24 C25 1.406(13) . ? C25 H25 0.9500 . ? C25 C26 1.358(16) . ? C26 C27 1.372(15) . ? C27 H27 0.9500 . ? C27 C28 1.374(12) . ? C28 H28 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Re1 C4 84.0(2) . . ? N2 Re1 N1 74.8(2) . . ? N2 Re1 C4 88.6(2) . . ? C1 Re1 N1 91.2(3) . . ? C1 Re1 N2 95.2(3) . . ? C1 Re1 C3 90.4(3) . . ? C1 Re1 C4 172.9(3) . . ? C2 Re1 N1 171.8(4) . . ? C2 Re1 N2 97.1(4) . . ? C2 Re1 C1 88.1(4) . . ? C2 Re1 C3 89.5(4) . . ? C2 Re1 C4 97.4(3) . . ? C3 Re1 N1 98.7(3) . . ? C3 Re1 N2 171.4(3) . . ? C3 Re1 C4 85.1(3) . . ? C1S Cl1S C1S 75.7(16) 3_656 . ? C4 S1 C5 95.4(4) . . ? F1 P1 F2 90.3(3) . . ? F1 P1 F3 89.0(4) . . ? F1 P1 F6 89.8(5) . . ? F2 P1 F3 179.2(4) . . ? F4 P1 F1 90.1(4) . . ? F4 P1 F2 91.0(3) . . ? F4 P1 F3 89.5(3) . . ? F4 P1 F6 178.9(4) . . ? F5 P1 F1 178.6(5) . . ? F5 P1 F2 90.3(3) . . ? F5 P1 F3 90.4(4) . . ? F5 P1 F4 91.2(5) . . ? F5 P1 F6 88.9(5) . . ? F6 P1 F2 90.1(3) . . ? F6 P1 F3 89.5(3) . . ? C7 N1 Re1 125.0(6) . . ? C7 N1 C11 119.0(7) . . ? C11 N1 Re1 115.9(5) . . ? C12 N2 Re1 117.5(5) . . ? C16 N2 Re1 123.2(6) . . ? C16 N2 C12 119.3(7) . . ? C3 N3 C17 168.8(8) . . ? C4 N4 C6 119.1(6) . . ? C4 N4 C23 124.3(6) . . ? C23 N4 C6 116.3(6) . . ? O1 C1 Re1 177.6(8) . . ? Cl1S C1S Cl1S 104.3(16) 3_656 . ? O2 C2 Re1 176.0(8) . . ? N3 C3 Re1 176.6(7) . . ? S1 C4 Re1 116.8(3) . . ? N4 C4 Re1 133.7(5) . . ? N4 C4 S1 109.5(5) . . ? S1 C5 H5A 110.8 . . ? S1 C5 H5B 110.8 . . ? H5A C5 H5B 108.9 . . ? C6 C5 S1 104.6(5) . . ? C6 C5 H5A 110.8 . . ? C6 C5 H5B 110.8 . . ? N4 C6 C5 108.4(6) . . ? N4 C6 H6A 110.0 . . ? N4 C6 H6B 110.0 . . ? C5 C6 H6A 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? N1 C7 H7 119.5 . . ? N1 C7 C8 121.0(9) . . ? C8 C7 H7 119.5 . . ? C7 C8 H8 120.5 . . ? C9 C8 C7 119.0(10) . . ? C9 C8 H8 120.5 . . ? C8 C9 H9 119.7 . . ? C10 C9 C8 120.7(10) . . ? C10 C9 H9 119.7 . . ? C9 C10 H10 120.7 . . ? C9 C10 C11 118.7(10) . . ? C11 C10 H10 120.7 . . ? N1 C11 C10 121.6(9) . . ? N1 C11 C12 116.8(6) . . ? C10 C11 C12 121.6(8) . . ? N2 C12 C11 114.4(6) . . ? N2 C12 C13 120.1(9) . . ? C13 C12 C11 125.4(9) . . ? C12 C13 H13 120.5 . . ? C12 C13 C14 118.9(10) . . ? C14 C13 H13 120.5 . . ? C13 C14 H14 119.9 . . ? C15 C14 C13 120.2(9) . . ? C15 C14 H14 119.9 . . ? C14 C15 H15 120.5 . . ? C14 C15 C16 119.1(10) . . ? C16 C15 H15 120.5 . . ? N2 C16 C15 122.4(10) . . ? N2 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? N3 C17 C18 118.4(7) . . ? C22 C17 N3 120.7(7) . . ? C22 C17 C18 120.9(7) . . ? C17 C18 H18 120.8 . . ? C19 C18 C17 118.4(8) . . ? C19 C18 H18 120.8 . . ? C18 C19 H19 120.3 . . ? C20 C19 C18 119.3(7) . . ? C20 C19 H19 120.3 . . ? C19 C20 Cl1 118.0(6) . . ? C19 C20 C21 122.3(7) . . ? C21 C20 Cl1 119.7(6) . . ? C20 C21 H21 120.5 . . ? C20 C21 C22 119.0(8) . . ? C22 C21 H21 120.5 . . ? C17 C22 C21 120.0(7) . . ? C17 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 N4 118.9(7) . . ? C28 C23 N4 120.1(7) . . ? C28 C23 C24 120.8(8) . . ? C23 C24 H24 120.9 . . ? C23 C24 C25 118.2(9) . . ? C25 C24 H24 120.9 . . ? C24 C25 H25 120.2 . . ? C26 C25 C24 119.7(9) . . ? C26 C25 H25 120.2 . . ? C25 C26 Cl2 119.4(8) . . ? C25 C26 C27 122.0(9) . . ? C27 C26 Cl2 118.7(9) . . ? C26 C27 H27 120.6 . . ? C26 C27 C28 118.9(10) . . ? C28 C27 H27 120.6 . . ? C23 C28 H28 119.8 . . ? C27 C28 C23 120.3(9) . . ? C27 C28 H28 119.8 . . ? #===END data_052213a_on _audit_creation_date 2013-05-24 _audit_creation_method ; Olex2 1.1 (compiled 2011.08.18 svn.r1932, GUI svn.r3819) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H19 Cl2 N5 O2 Re, F6 P' _chemical_formula_sum 'C28 H19 Cl2 F6 N5 O2 P Re' _chemical_formula_weight 859.55 _chemical_melting_point ? _chemical_oxdiff_formula 'C11 H10 S O2' 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.796(2) _cell_length_b 14.7810(5) _cell_length_c 18.781(3) _cell_angle_alpha 90.00 _cell_angle_beta 119.867(15) _cell_angle_gamma 90.00 _cell_volume 5969.4(11) _cell_formula_units_Z 8 _cell_measurement_reflns_used 6626 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 29.0897 _cell_measurement_theta_min 2.8228 _exptl_absorpt_coefficient_mu 4.379 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.21558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.913 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 3328 _exptl_crystal_size_max 0.81 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.02 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_unetI/netI 0.0320 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 13785 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.83 _diffrn_ambient_temperature 133(2) _diffrn_detector_area_resol_mean 16.1270 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -95.00 -37.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -18.4430 178.0000 150.0000 58 #__ type_ start__ end____ width___ exp.time_ 2 omega -72.00 -42.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -18.4430 -57.0000 30.0000 30 #__ type_ start__ end____ width___ exp.time_ 3 omega -92.00 -51.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -18.4430 -178.0000 90.0000 41 #__ type_ start__ end____ width___ exp.time_ 4 omega -38.00 49.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -18.4430 57.0000 0.0000 87 #__ type_ start__ end____ width___ exp.time_ 5 omega -4.00 48.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -18.4430 57.0000 120.0000 52 #__ type_ start__ end____ width___ exp.time_ 6 omega -16.00 9.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 18.9899 102.0000 146.0000 25 ; _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0033675000 _diffrn_orient_matrix_UB_12 0.0460501000 _diffrn_orient_matrix_UB_13 -0.0059099000 _diffrn_orient_matrix_UB_21 -0.0375901000 _diffrn_orient_matrix_UB_22 0.0075215000 _diffrn_orient_matrix_UB_23 -0.0205844000 _diffrn_orient_matrix_UB_31 0.0112113000 _diffrn_orient_matrix_UB_32 0.0112185000 _diffrn_orient_matrix_UB_33 0.0379386000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_source_current n/a _diffrn_source_voltage n/a _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4590 _reflns_number_total 5265 _reflns_odcompleteness_completeness 99.72 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 25.30 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.278 _refine_diff_density_min -1.513 _refine_diff_density_rms 0.127 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 406 _refine_ls_number_reflns 5265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0283 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+19.8567P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.0792 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.069696(7) 0.206974(12) 0.149455(10) 0.02198(8) Uani 1 1 d . . . Cl1 Cl 0.14080(6) 0.03305(9) -0.15795(7) 0.0356(3) Uani 1 1 d . . . Cl2 Cl 0.22941(7) 0.28975(12) 0.69306(8) 0.0543(4) Uani 1 1 d . . . P1 P 0.14601(5) 0.56543(9) 0.30890(7) 0.0258(3) Uani 1 1 d . . . F1 F 0.11910(13) 0.46436(19) 0.30229(16) 0.0369(7) Uani 1 1 d . . . F2 F 0.16889(13) 0.5661(2) 0.40478(16) 0.0387(7) Uani 1 1 d . . . F3 F 0.08046(12) 0.6067(2) 0.28915(17) 0.0386(7) Uani 1 1 d . . . F4 F 0.17285(13) 0.6639(2) 0.31432(17) 0.0385(7) Uani 1 1 d . . . F5 F 0.12273(13) 0.5612(2) 0.21230(15) 0.0370(7) Uani 1 1 d . . . F6 F 0.21063(13) 0.5208(2) 0.32708(17) 0.0405(7) Uani 1 1 d . . . O1 O -0.02539(19) 0.0828(3) 0.1616(3) 0.0588(12) Uani 1 1 d . . . O2 O 0.15246(17) 0.0396(3) 0.1886(2) 0.0416(9) Uani 1 1 d . . . N1 N 0.01725(17) 0.1939(3) 0.0171(2) 0.0244(8) Uani 1 1 d . . . N2 N 0.00887(16) 0.3250(3) 0.1050(2) 0.0236(8) Uani 1 1 d . . . N3 N 0.13214(19) 0.2482(3) 0.3385(2) 0.0356(10) Uani 1 1 d . . . N4 N 0.15936(16) 0.3732(3) 0.1852(2) 0.0247(8) Uani 1 1 d . . . H4 H 0.1502 0.3917 0.2224 0.030 Uiso 1 1 calc R . . N5 N 0.16134(17) 0.2973(2) 0.0907(2) 0.0240(8) Uani 1 1 d . . . C1 C 0.0098(2) 0.1315(4) 0.1585(3) 0.0332(11) Uani 1 1 d . . . C2 C 0.1217(2) 0.1029(3) 0.1747(3) 0.0290(10) Uani 1 1 d . . . C3 C 0.1092(2) 0.2319(4) 0.2683(3) 0.0305(11) Uani 1 1 d . . . C4 C 0.13533(19) 0.2970(3) 0.1397(2) 0.0198(9) Uani 1 1 d . . . C5 C 0.1993(2) 0.4184(4) 0.1671(3) 0.0338(11) Uani 1 1 d . . . H5 H 0.2216 0.4723 0.1920 0.041 Uiso 1 1 calc R . . C6 C 0.2005(2) 0.3705(4) 0.1069(3) 0.0341(11) Uani 1 1 d . . . H6 H 0.2238 0.3843 0.0807 0.041 Uiso 1 1 calc R . . C7 C 0.1522(2) 0.2306(3) 0.0300(3) 0.0249(10) Uani 1 1 d . . . C8 C 0.1812(2) 0.1474(3) 0.0552(3) 0.0281(10) Uani 1 1 d . . . H8 H 0.2042 0.1329 0.1120 0.034 Uiso 1 1 calc R . . C9 C 0.1764(2) 0.0855(3) -0.0031(3) 0.0300(10) Uani 1 1 d . . . H9 H 0.1957 0.0278 0.0132 0.036 Uiso 1 1 calc R . . C10 C 0.1432(2) 0.1089(3) -0.0851(3) 0.0259(10) Uani 1 1 d . . . C11 C 0.1135(3) 0.1908(4) -0.1106(3) 0.0362(12) Uani 1 1 d . . . H11 H 0.0900 0.2049 -0.1675 0.043 Uiso 1 1 calc R . . C12 C 0.1183(2) 0.2527(4) -0.0520(3) 0.0332(11) Uani 1 1 d . . . H12 H 0.0983 0.3099 -0.0684 0.040 Uiso 1 1 calc R . . C13 C 0.1561(2) 0.2580(4) 0.4232(3) 0.0310(11) Uani 1 1 d . . . C14 C 0.1517(2) 0.1860(4) 0.4672(3) 0.0379(12) Uani 1 1 d . . . H14 H 0.1329 0.1307 0.4404 0.046 Uiso 1 1 calc R . . C15 C 0.1753(3) 0.1960(4) 0.5515(3) 0.0420(14) Uani 1 1 d . . . H15 H 0.1730 0.1475 0.5830 0.050 Uiso 1 1 calc R . . C16 C 0.2019(2) 0.2768(4) 0.5884(3) 0.0351(12) Uani 1 1 d . . . C17 C 0.2074(2) 0.3464(4) 0.5448(3) 0.0414(13) Uani 1 1 d . . . H17 H 0.2272 0.4010 0.5719 0.050 Uiso 1 1 calc R . . C18 C 0.1842(2) 0.3376(4) 0.4616(3) 0.0386(12) Uani 1 1 d . . . H18 H 0.1876 0.3861 0.4309 0.046 Uiso 1 1 calc R . . C19 C 0.0190(2) 0.1198(3) -0.0245(3) 0.0324(11) Uani 1 1 d . . . H19 H 0.0483 0.0735 0.0051 0.039 Uiso 1 1 calc R . . C20 C -0.0198(3) 0.1091(4) -0.1075(3) 0.0433(13) Uani 1 1 d . . . H20 H -0.0175 0.0562 -0.1346 0.052 Uiso 1 1 calc R . . C21 C -0.0620(3) 0.1764(4) -0.1508(3) 0.0424(14) Uani 1 1 d . . . H21 H -0.0897 0.1702 -0.2081 0.051 Uiso 1 1 calc R . . C22 C -0.0635(2) 0.2524(4) -0.1100(3) 0.0336(11) Uani 1 1 d . . . H22 H -0.0918 0.2999 -0.1391 0.040 Uiso 1 1 calc R . . C23 C -0.0237(2) 0.2594(3) -0.0263(3) 0.0250(10) Uani 1 1 d . . . C24 C -0.02543(19) 0.3363(3) 0.0227(3) 0.0239(9) Uani 1 1 d . . . C25 C -0.0607(2) 0.4128(4) -0.0118(3) 0.0323(11) Uani 1 1 d . . . H25 H -0.0846 0.4191 -0.0697 0.039 Uiso 1 1 calc R . . C26 C -0.0609(2) 0.4801(4) 0.0390(3) 0.0384(12) Uani 1 1 d . . . H26 H -0.0846 0.5336 0.0165 0.046 Uiso 1 1 calc R . . C27 C -0.0263(2) 0.4688(4) 0.1229(3) 0.0366(12) Uani 1 1 d . . . H27 H -0.0258 0.5141 0.1591 0.044 Uiso 1 1 calc R . . C28 C 0.0073(2) 0.3906(4) 0.1529(3) 0.0294(11) Uani 1 1 d . . . H28 H 0.0307 0.3827 0.2107 0.035 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.02386(11) 0.02335(13) 0.02161(11) 0.00058(7) 0.01350(8) -0.00053(7) Cl1 0.0510(7) 0.0319(7) 0.0329(6) -0.0081(5) 0.0277(6) -0.0052(5) Cl2 0.0427(8) 0.0931(14) 0.0212(6) -0.0026(6) 0.0114(6) 0.0170(7) P1 0.0322(6) 0.0225(7) 0.0242(6) -0.0036(5) 0.0151(5) -0.0034(5) F1 0.0491(17) 0.0237(16) 0.0340(15) -0.0019(12) 0.0176(13) -0.0098(13) F2 0.0512(17) 0.0388(19) 0.0255(14) -0.0057(12) 0.0186(13) -0.0006(14) F3 0.0331(15) 0.0388(19) 0.0465(17) 0.0013(14) 0.0217(13) 0.0017(13) F4 0.0494(17) 0.0264(17) 0.0500(17) -0.0081(13) 0.0326(15) -0.0105(13) F5 0.0539(18) 0.0314(17) 0.0267(14) -0.0005(12) 0.0208(13) 0.0002(13) F6 0.0340(15) 0.042(2) 0.0424(16) -0.0110(14) 0.0168(13) 0.0024(13) O1 0.055(2) 0.048(3) 0.094(3) 0.009(2) 0.053(2) -0.008(2) O2 0.052(2) 0.032(2) 0.050(2) 0.0158(17) 0.0325(19) 0.0143(18) N1 0.030(2) 0.021(2) 0.0253(19) -0.0018(15) 0.0156(17) -0.0030(16) N2 0.0213(18) 0.028(2) 0.0211(18) -0.0053(16) 0.0105(15) -0.0027(16) N3 0.038(2) 0.044(3) 0.027(2) 0.0028(19) 0.0182(19) 0.010(2) N4 0.0290(19) 0.023(2) 0.0251(18) -0.0049(16) 0.0161(16) -0.0027(16) N5 0.029(2) 0.020(2) 0.028(2) -0.0054(15) 0.0186(17) -0.0038(15) C1 0.039(3) 0.028(3) 0.041(3) 0.002(2) 0.027(2) 0.002(2) C2 0.035(2) 0.027(3) 0.030(2) 0.008(2) 0.020(2) 0.003(2) C3 0.028(2) 0.041(3) 0.027(3) 0.007(2) 0.018(2) 0.007(2) C4 0.020(2) 0.019(2) 0.019(2) -0.0005(16) 0.0092(17) 0.0016(16) C5 0.038(3) 0.028(3) 0.041(3) -0.008(2) 0.024(2) -0.011(2) C6 0.035(3) 0.037(3) 0.040(3) -0.007(2) 0.025(2) -0.011(2) C7 0.029(2) 0.026(3) 0.028(2) -0.0048(19) 0.020(2) -0.0038(19) C8 0.028(2) 0.031(3) 0.025(2) -0.0020(19) 0.0131(19) 0.003(2) C9 0.029(2) 0.028(3) 0.033(3) 0.000(2) 0.015(2) 0.005(2) C10 0.036(2) 0.023(3) 0.028(2) -0.0040(19) 0.023(2) -0.0069(19) C11 0.052(3) 0.034(3) 0.026(2) 0.005(2) 0.023(2) 0.001(2) C12 0.052(3) 0.023(3) 0.031(3) 0.004(2) 0.025(2) 0.006(2) C13 0.031(2) 0.043(3) 0.022(2) 0.006(2) 0.016(2) 0.013(2) C14 0.045(3) 0.043(3) 0.032(3) -0.003(2) 0.023(2) 0.002(2) C15 0.047(3) 0.058(4) 0.030(3) 0.015(2) 0.026(2) 0.015(3) C16 0.029(2) 0.054(4) 0.021(2) 0.003(2) 0.011(2) 0.017(2) C17 0.037(3) 0.042(4) 0.036(3) -0.002(2) 0.011(2) 0.011(2) C18 0.041(3) 0.038(3) 0.032(3) 0.007(2) 0.014(2) 0.012(2) C19 0.038(3) 0.018(3) 0.042(3) -0.006(2) 0.021(2) -0.006(2) C20 0.059(3) 0.035(3) 0.040(3) -0.017(2) 0.027(3) -0.013(3) C21 0.057(3) 0.043(4) 0.025(3) -0.009(2) 0.019(3) -0.010(3) C22 0.039(3) 0.036(3) 0.024(2) 0.000(2) 0.015(2) -0.004(2) C23 0.028(2) 0.024(3) 0.026(2) -0.0032(19) 0.0152(19) -0.0050(19) C24 0.024(2) 0.023(3) 0.025(2) -0.0057(18) 0.0130(18) -0.0062(18) C25 0.027(2) 0.035(3) 0.029(2) -0.002(2) 0.010(2) 0.002(2) C26 0.031(3) 0.033(3) 0.049(3) -0.004(2) 0.018(2) 0.010(2) C27 0.025(2) 0.040(3) 0.041(3) -0.018(2) 0.015(2) 0.002(2) C28 0.023(2) 0.036(3) 0.030(2) -0.011(2) 0.0130(19) 0.001(2) _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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N1 2.165(4) . ? Re1 N2 2.181(4) . ? Re1 C1 1.931(5) . ? Re1 C2 1.910(5) . ? Re1 C3 1.975(5) . ? Re1 C4 2.179(4) . ? Cl1 C10 1.747(4) . ? Cl2 C16 1.741(5) . ? P1 F1 1.616(3) . ? P1 F2 1.596(3) . ? P1 F3 1.597(3) . ? P1 F4 1.582(3) . ? P1 F5 1.608(3) . ? P1 F6 1.605(3) . ? O1 C1 1.155(6) . ? O2 C2 1.151(6) . ? N1 C19 1.359(6) . ? N1 C23 1.345(6) . ? N2 C24 1.354(5) . ? N2 C28 1.336(6) . ? N3 C3 1.173(6) . ? N3 C13 1.401(6) . ? N4 H4 0.8800 . ? N4 C4 1.359(6) . ? N4 C5 1.371(6) . ? N5 C4 1.362(6) . ? N5 C6 1.382(6) . ? N5 C7 1.437(6) . ? C5 H5 0.9500 . ? C5 C6 1.346(7) . ? C6 H6 0.9500 . ? C7 C8 1.383(7) . ? C7 C12 1.377(6) . ? C8 H8 0.9500 . ? C8 C9 1.387(7) . ? C9 H9 0.9500 . ? C9 C10 1.381(6) . ? C10 C11 1.374(7) . ? C11 H11 0.9500 . ? C11 C12 1.391(7) . ? C12 H12 0.9500 . ? C13 C14 1.384(8) . ? C13 C18 1.375(8) . ? C14 H14 0.9500 . ? C14 C15 1.395(7) . ? C15 H15 0.9500 . ? C15 C16 1.373(8) . ? C16 C17 1.363(8) . ? C17 H17 0.9500 . ? C17 C18 1.377(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C19 C20 1.374(7) . ? C20 H20 0.9500 . ? C20 C21 1.378(8) . ? C21 H21 0.9500 . ? C21 C22 1.369(8) . ? C22 H22 0.9500 . ? C22 C23 1.382(6) . ? C23 C24 1.477(6) . ? C24 C25 1.377(7) . ? C25 H25 0.9500 . ? C25 C26 1.380(7) . ? C26 H26 0.9500 . ? C26 C27 1.378(7) . ? C27 H27 0.9500 . ? C27 C28 1.371(7) . ? C28 H28 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Re1 N2 74.13(13) . . ? N1 Re1 C4 90.29(15) . . ? C1 Re1 N1 90.03(18) . . ? C1 Re1 N2 94.58(18) . . ? C1 Re1 C3 88.8(2) . . ? C1 Re1 C4 177.66(18) . . ? C2 Re1 N1 99.11(17) . . ? C2 Re1 N2 172.69(16) . . ? C2 Re1 C1 88.1(2) . . ? C2 Re1 C3 88.6(2) . . ? C2 Re1 C4 94.13(18) . . ? C3 Re1 N1 172.12(17) . . ? C3 Re1 N2 98.20(17) . . ? C3 Re1 C4 90.60(18) . . ? C4 Re1 N2 83.27(15) . . ? F2 P1 F1 89.63(16) . . ? F2 P1 F3 90.49(16) . . ? F2 P1 F5 178.12(18) . . ? F2 P1 F6 90.36(16) . . ? F3 P1 F1 90.07(17) . . ? F3 P1 F5 90.04(16) . . ? F3 P1 F6 177.96(18) . . ? F4 P1 F1 178.96(17) . . ? F4 P1 F2 91.13(16) . . ? F4 P1 F3 90.62(17) . . ? F4 P1 F5 90.67(16) . . ? F4 P1 F6 91.22(17) . . ? F5 P1 F1 88.56(15) . . ? F6 P1 F1 88.08(17) . . ? F6 P1 F5 89.06(16) . . ? C19 N1 Re1 124.0(3) . . ? C23 N1 Re1 118.2(3) . . ? C23 N1 C19 117.5(4) . . ? C24 N2 Re1 117.2(3) . . ? C28 N2 Re1 124.7(3) . . ? C28 N2 C24 117.8(4) . . ? C3 N3 C13 172.9(6) . . ? C4 N4 H4 123.4 . . ? C4 N4 C5 113.2(4) . . ? C5 N4 H4 123.4 . . ? C4 N5 C6 111.8(4) . . ? C4 N5 C7 126.3(4) . . ? C6 N5 C7 121.9(4) . . ? O1 C1 Re1 176.3(5) . . ? O2 C2 Re1 178.8(5) . . ? N3 C3 Re1 178.7(5) . . ? N4 C4 Re1 124.5(3) . . ? N4 C4 N5 102.4(4) . . ? N5 C4 Re1 133.2(3) . . ? N4 C5 H5 127.1 . . ? C6 C5 N4 105.8(4) . . ? C6 C5 H5 127.1 . . ? N5 C6 H6 126.6 . . ? C5 C6 N5 106.9(4) . . ? C5 C6 H6 126.6 . . ? C8 C7 N5 119.2(4) . . ? C12 C7 N5 119.5(4) . . ? C12 C7 C8 121.1(4) . . ? C7 C8 H8 120.3 . . ? C7 C8 C9 119.5(4) . . ? C9 C8 H8 120.3 . . ? C8 C9 H9 120.6 . . ? C10 C9 C8 118.9(5) . . ? C10 C9 H9 120.6 . . ? C9 C10 Cl1 118.8(4) . . ? C11 C10 Cl1 119.2(3) . . ? C11 C10 C9 122.0(4) . . ? C10 C11 H11 120.5 . . ? C10 C11 C12 118.9(4) . . ? C12 C11 H11 120.5 . . ? C7 C12 C11 119.6(5) . . ? C7 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 N3 118.9(5) . . ? C18 C13 N3 120.1(5) . . ? C18 C13 C14 121.0(4) . . ? C13 C14 H14 120.6 . . ? C13 C14 C15 118.8(5) . . ? C15 C14 H14 120.6 . . ? C14 C15 H15 120.3 . . ? C16 C15 C14 119.4(5) . . ? C16 C15 H15 120.3 . . ? C15 C16 Cl2 119.0(4) . . ? C17 C16 Cl2 119.7(5) . . ? C17 C16 C15 121.3(5) . . ? C16 C17 H17 120.0 . . ? C16 C17 C18 120.0(6) . . ? C18 C17 H17 120.0 . . ? C13 C18 C17 119.5(5) . . ? C13 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? N1 C19 H19 118.6 . . ? N1 C19 C20 122.7(5) . . ? C20 C19 H19 118.6 . . ? C19 C20 H20 120.6 . . ? C19 C20 C21 118.9(5) . . ? C21 C20 H20 120.6 . . ? C20 C21 H21 120.4 . . ? C22 C21 C20 119.1(5) . . ? C22 C21 H21 120.4 . . ? C21 C22 H22 120.2 . . ? C21 C22 C23 119.6(5) . . ? C23 C22 H22 120.2 . . ? N1 C23 C22 122.1(4) . . ? N1 C23 C24 115.1(4) . . ? C22 C23 C24 122.7(4) . . ? N2 C24 C23 114.8(4) . . ? N2 C24 C25 121.9(4) . . ? C25 C24 C23 123.2(4) . . ? C24 C25 H25 120.4 . . ? C24 C25 C26 119.1(4) . . ? C26 C25 H25 120.4 . . ? C25 C26 H26 120.4 . . ? C27 C26 C25 119.3(5) . . ? C27 C26 H26 120.4 . . ? C26 C27 H27 120.8 . . ? C28 C27 C26 118.5(5) . . ? C28 C27 H27 120.8 . . ? N2 C28 C27 123.4(4) . . ? N2 C28 H28 118.3 . . ? C27 C28 H28 118.3 . . ? #===END