data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H27 Mn O3 P2' _chemical_formula_weight 552.40 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' 'O' 'O' 0.0106 0.0060 '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' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.017(4) _cell_length_b 15.451(5) _cell_length_c 15.773(5) _cell_angle_alpha 95.888(6) _cell_angle_beta 90.886(6) _cell_angle_gamma 99.304(7) _cell_volume 2634.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 921 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 23.08 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.653 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11907 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0748 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 23.37 _reflns_number_total 7558 _reflns_number_gt 5330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1281P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7558 _refine_ls_number_parameters 657 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_gt 0.0798 _refine_ls_wR_factor_ref 0.2028 _refine_ls_wR_factor_gt 0.1833 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Mn1A Mn 0.47476(7) 0.74414(5) 0.83801(5) 0.0302(3) Uani 1 1 d D . . Mn1B Mn 0.12989(7) 0.74399(5) 0.33791(5) 0.0283(3) Uani 1 1 d . . . P1A P 0.46935(12) 0.77863(9) 0.70051(9) 0.0276(4) Uani 1 1 d . . . P2A P 0.29667(13) 0.64435(9) 0.81287(9) 0.0286(4) Uani 1 1 d . . . P1B P 0.26181(12) 0.64283(9) 0.31642(9) 0.0277(4) Uani 1 1 d . . . P2B P 0.16488(13) 0.78194(9) 0.20326(9) 0.0288(4) Uani 1 1 d . . . O1A O 0.6787(4) 0.8918(3) 0.8847(3) 0.0443(11) Uani 1 1 d . . . O2A O 0.6330(4) 0.6120(3) 0.7841(3) 0.0500(11) Uani 1 1 d . . . O3A O 0.4805(4) 0.7163(3) 1.0199(3) 0.0414(10) Uani 1 1 d . . . O1B O 0.1169(4) 0.7290(3) 0.5230(3) 0.0418(10) Uani 1 1 d . . . O2B O -0.0865(4) 0.6114(3) 0.2786(3) 0.0412(10) Uani 1 1 d . . . O3B O -0.0151(4) 0.8873(3) 0.3739(3) 0.0444(11) Uani 1 1 d . . . C1A C 0.5997(5) 0.8353(4) 0.8637(4) 0.0328(13) Uani 1 1 d . . . C2A C 0.5721(5) 0.6615(4) 0.8050(4) 0.0313(13) Uani 1 1 d . . . C3A C 0.4754(5) 0.7256(3) 0.9497(4) 0.0323(13) Uani 1 1 d . . . C4A C 0.4238(5) 0.6830(3) 0.6204(3) 0.0301(13) Uani 1 1 d . . . H4A1 H 0.4276 0.7032 0.5629 0.036 Uiso 1 1 calc R . . H4A2 H 0.4831 0.6415 0.6237 0.036 Uiso 1 1 calc R . . C5A C 0.2935(5) 0.6341(3) 0.6330(3) 0.0313(13) Uani 1 1 d . . . H5A1 H 0.2373 0.6778 0.6421 0.038 Uiso 1 1 calc R . . H5A2 H 0.2651 0.5951 0.5803 0.038 Uiso 1 1 calc R . . C6A C 0.2854(5) 0.5787(3) 0.7079(3) 0.0344(14) Uani 1 1 d . . . H6A1 H 0.3523 0.5429 0.7045 0.041 Uiso 1 1 calc R . . H6A2 H 0.2062 0.5375 0.7029 0.041 Uiso 1 1 calc R . . C7A C 0.3712(5) 0.8544(3) 0.6654(4) 0.0300(13) Uani 1 1 d . . . C8A C 0.2739(5) 0.8764(3) 0.7143(4) 0.0359(14) Uani 1 1 d . . . H8A H 0.2595 0.8535 0.7676 0.043 Uiso 1 1 calc R . . C9A C 0.1977(5) 0.9317(4) 0.6853(4) 0.0457(17) Uani 1 1 d . . . H9A H 0.1320 0.9470 0.7189 0.055 Uiso 1 1 calc R . . C10A C 0.2184(6) 0.9643(4) 0.6072(4) 0.0435(16) Uani 1 1 d . . . H10A H 0.1664 1.0020 0.5877 0.052 Uiso 1 1 calc R . . C11A C 0.3130(5) 0.9431(4) 0.5574(4) 0.0417(15) Uani 1 1 d . . . H11A H 0.3261 0.9655 0.5039 0.050 Uiso 1 1 calc R . . C12A C 0.3889(5) 0.8885(3) 0.5865(4) 0.0335(14) Uani 1 1 d . . . H12A H 0.4544 0.8737 0.5524 0.040 Uiso 1 1 calc R . . C13A C 0.6212(5) 0.8262(3) 0.6654(3) 0.0308(13) Uani 1 1 d . . . C14A C 0.6566(5) 0.9172(4) 0.6733(4) 0.0404(15) Uani 1 1 d . . . H14A H 0.6011 0.9540 0.6960 0.048 Uiso 1 1 calc R . . C15A C 0.7694(5) 0.9546(4) 0.6491(4) 0.0408(15) Uani 1 1 d . . . H15A H 0.7906 1.0170 0.6533 0.049 Uiso 1 1 calc R . . C16A C 0.8539(5) 0.9021(4) 0.6181(4) 0.0417(15) Uani 1 1 d . . . H16A H 0.9330 0.9282 0.6018 0.050 Uiso 1 1 calc R . . C17A C 0.8208(5) 0.8112(4) 0.6114(4) 0.0472(17) Uani 1 1 d . . . H17A H 0.8775 0.7746 0.5904 0.057 Uiso 1 1 calc R . . C18A C 0.7049(5) 0.7735(4) 0.6354(4) 0.0369(14) Uani 1 1 d . . . H18A H 0.6831 0.7111 0.6312 0.044 Uiso 1 1 calc R . . C19A C 0.1492(5) 0.6852(4) 0.8207(4) 0.0329(13) Uani 1 1 d . . . C20A C 0.1370(5) 0.7473(4) 0.8894(4) 0.0358(14) Uani 1 1 d . . . H20A H 0.2052 0.7697 0.9274 0.043 Uiso 1 1 calc R . . C21A C 0.0250(6) 0.7764(4) 0.9022(4) 0.0454(16) Uani 1 1 d . . . H21A H 0.0167 0.8186 0.9491 0.054 Uiso 1 1 calc R . . C22A C -0.0728(6) 0.7447(4) 0.8476(5) 0.0523(18) Uani 1 1 d . . . H22A H -0.1490 0.7649 0.8565 0.063 Uiso 1 1 calc R . . C23A C -0.0614(6) 0.6827(4) 0.7789(4) 0.0483(17) Uani 1 1 d . . . H23A H -0.1296 0.6609 0.7408 0.058 Uiso 1 1 calc R . . C24A C 0.0488(5) 0.6531(4) 0.7661(4) 0.0400(15) Uani 1 1 d . . . H24A H 0.0561 0.6104 0.7195 0.048 Uiso 1 1 calc R . . C25A C 0.2723(5) 0.5544(3) 0.8819(3) 0.0332(13) Uani 1 1 d . . . C26A C 0.3708(5) 0.5140(4) 0.9014(4) 0.0424(15) Uani 1 1 d . . . H26A H 0.4499 0.5351 0.8813 0.051 Uiso 1 1 calc R . . C27A C 0.3561(6) 0.4434(4) 0.9497(4) 0.0515(17) Uani 1 1 d . . . H27A H 0.4246 0.4156 0.9609 0.062 Uiso 1 1 calc R . . C28A C 0.2432(6) 0.4127(4) 0.9820(4) 0.0459(16) Uani 1 1 d . . . H28A H 0.2332 0.3649 1.0161 0.055 Uiso 1 1 calc R . . C29A C 0.1458(6) 0.4535(4) 0.9630(4) 0.0433(16) Uani 1 1 d . . . H29A H 0.0674 0.4336 0.9846 0.052 Uiso 1 1 calc R . . C30A C 0.1591(5) 0.5225(4) 0.9135(4) 0.0358(14) Uani 1 1 d . . . H30A H 0.0896 0.5487 0.9007 0.043 Uiso 1 1 calc R . . C1B C 0.1236(5) 0.7313(3) 0.4509(4) 0.0328(14) Uani 1 1 d . . . C2B C -0.0019(5) 0.6619(3) 0.3017(3) 0.0267(12) Uani 1 1 d . . . C3B C 0.0413(5) 0.8326(4) 0.3582(4) 0.0337(14) Uani 1 1 d . . . C4B C 0.2390(5) 0.5766(3) 0.2125(3) 0.0332(14) Uani 1 1 d . . . H4B1 H 0.2969 0.5337 0.2091 0.040 Uiso 1 1 calc R . . H4B2 H 0.1544 0.5427 0.2084 0.040 Uiso 1 1 calc R . . C5B C 0.2580(5) 0.6311(3) 0.1360(4) 0.0346(14) Uani 1 1 d . . . H5B1 H 0.3384 0.6706 0.1441 0.042 Uiso 1 1 calc R . . H5B2 H 0.2618 0.5903 0.0838 0.042 Uiso 1 1 calc R . . C6B C 0.1583(5) 0.6867(3) 0.1223(3) 0.0315(13) Uani 1 1 d . . . H6B1 H 0.0767 0.6491 0.1230 0.038 Uiso 1 1 calc R . . H6B2 H 0.1671 0.7081 0.0653 0.038 Uiso 1 1 calc R . . C7B C 0.2449(5) 0.5542(3) 0.3866(3) 0.0300(13) Uani 1 1 d . . . C8B C 0.3453(5) 0.5217(3) 0.4198(4) 0.0341(14) Uani 1 1 d . . . H8B H 0.4264 0.5470 0.4067 0.041 Uiso 1 1 calc R . . C9B C 0.3289(6) 0.4540(4) 0.4708(4) 0.0390(15) Uani 1 1 d . . . H9B H 0.3984 0.4338 0.4933 0.047 Uiso 1 1 calc R . . C10B C 0.2109(6) 0.4149(4) 0.4895(4) 0.0402(15) Uani 1 1 d . . . H10B H 0.1992 0.3685 0.5252 0.048 Uiso 1 1 calc R . . C11B C 0.1127(6) 0.4443(4) 0.4560(4) 0.0406(15) Uani 1 1 d . . . H11B H 0.0318 0.4170 0.4673 0.049 Uiso 1 1 calc R . . C12B C 0.1284(5) 0.5128(4) 0.4057(4) 0.0363(14) Uani 1 1 d . . . H12B H 0.0580 0.5323 0.3835 0.044 Uiso 1 1 calc R . . C13B C 0.4277(5) 0.6812(3) 0.3251(3) 0.0304(13) Uani 1 1 d . . . C14B C 0.5111(5) 0.6483(4) 0.2707(4) 0.0378(14) Uani 1 1 d . . . H14B H 0.4823 0.6044 0.2250 0.045 Uiso 1 1 calc R . . C15B C 0.6358(5) 0.6791(4) 0.2824(4) 0.0473(16) Uani 1 1 d . . . H15B H 0.6918 0.6557 0.2448 0.057 Uiso 1 1 calc R . . C16B C 0.6805(5) 0.7433(4) 0.3479(4) 0.0465(17) Uani 1 1 d . . . H16B H 0.7663 0.7647 0.3546 0.056 Uiso 1 1 calc R . . C17B C 0.5989(5) 0.7762(4) 0.4039(4) 0.0415(15) Uani 1 1 d . . . H17B H 0.6287 0.8190 0.4502 0.050 Uiso 1 1 calc R . . C18B C 0.4727(5) 0.7460(3) 0.3917(4) 0.0342(13) Uani 1 1 d . . . H18B H 0.4168 0.7698 0.4291 0.041 Uiso 1 1 calc R . . C19B C 0.3108(5) 0.8487(3) 0.1790(4) 0.0332(14) Uani 1 1 d . . . C20B C 0.3291(6) 0.8714(4) 0.0959(4) 0.0451(16) Uani 1 1 d . . . H20B H 0.2644 0.8554 0.0539 0.054 Uiso 1 1 calc R . . C21B C 0.4421(7) 0.9175(4) 0.0746(5) 0.0559(19) Uani 1 1 d . . . H21B H 0.4555 0.9329 0.0183 0.067 Uiso 1 1 calc R . . C22B C 0.5348(6) 0.9406(4) 0.1375(5) 0.0557(19) Uani 1 1 d . . . H22B H 0.6118 0.9724 0.1236 0.067 Uiso 1 1 calc R . . C23B C 0.5186(6) 0.9192(4) 0.2169(5) 0.0506(18) Uani 1 1 d . . . H23B H 0.5839 0.9355 0.2583 0.061 Uiso 1 1 calc R . . C24B C 0.4055(5) 0.8727(3) 0.2393(4) 0.0382(15) Uani 1 1 d . . . H24B H 0.3942 0.8578 0.2959 0.046 Uiso 1 1 calc R . . C25B C 0.0492(5) 0.8399(4) 0.1592(3) 0.0342(14) Uani 1 1 d . . . C26B C 0.0743(6) 0.9292(4) 0.1493(4) 0.0423(15) Uani 1 1 d . . . H26B H 0.1528 0.9622 0.1665 0.051 Uiso 1 1 calc R . . C27B C -0.0137(6) 0.9706(4) 0.1145(4) 0.0524(18) Uani 1 1 d . . . H27B H 0.0052 1.0314 0.1064 0.063 Uiso 1 1 calc R . . C28B C -0.1293(6) 0.9238(5) 0.0914(4) 0.0577(19) Uani 1 1 d . . . H28B H -0.1892 0.9516 0.0658 0.069 Uiso 1 1 calc R . . C29B C -0.1566(6) 0.8368(5) 0.1060(4) 0.0532(18) Uani 1 1 d . . . H29B H -0.2374 0.8053 0.0933 0.064 Uiso 1 1 calc R . . C30B C -0.0694(5) 0.7953(4) 0.1383(4) 0.0412(15) Uani 1 1 d . . . H30B H -0.0897 0.7347 0.1468 0.049 Uiso 1 1 calc R . . H1B H 0.255(5) 0.823(4) 0.364(3) 0.053(17) Uiso 1 1 d . . . H1A H 0.386(4) 0.825(2) 0.865(3) 0.022(12) Uiso 1 1 d 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 Mn1A 0.0236(5) 0.0258(5) 0.0377(5) -0.0020(4) 0.0015(4) -0.0032(4) Mn1B 0.0199(5) 0.0237(5) 0.0383(5) -0.0020(4) 0.0034(4) -0.0026(3) P1A 0.0221(8) 0.0209(7) 0.0371(9) -0.0026(6) 0.0029(6) -0.0007(6) P2A 0.0216(8) 0.0259(8) 0.0354(9) -0.0024(6) 0.0023(6) -0.0013(6) P1B 0.0201(7) 0.0246(8) 0.0351(9) -0.0028(6) 0.0031(6) -0.0021(6) P2B 0.0258(8) 0.0212(8) 0.0367(9) 0.0000(6) 0.0030(6) -0.0025(6) O1A 0.036(3) 0.036(2) 0.053(3) -0.006(2) -0.007(2) -0.011(2) O2A 0.035(3) 0.040(3) 0.073(3) 0.003(2) 0.009(2) 0.002(2) O3A 0.045(3) 0.038(2) 0.041(3) 0.001(2) 0.005(2) 0.0083(19) O1B 0.037(2) 0.041(3) 0.043(3) -0.002(2) 0.005(2) -0.0021(19) O2B 0.024(2) 0.036(2) 0.060(3) 0.002(2) 0.000(2) -0.004(2) O3B 0.031(2) 0.031(2) 0.071(3) -0.002(2) 0.014(2) 0.0061(19) C1A 0.031(3) 0.029(3) 0.038(3) 0.002(3) 0.005(3) 0.002(3) C2A 0.022(3) 0.031(3) 0.037(3) 0.000(3) 0.005(2) -0.005(3) C3A 0.026(3) 0.022(3) 0.047(4) -0.003(3) -0.001(3) 0.004(2) C4A 0.030(3) 0.023(3) 0.034(3) -0.001(2) 0.007(2) -0.003(2) C5A 0.028(3) 0.030(3) 0.033(3) -0.004(3) 0.005(2) 0.001(2) C6A 0.023(3) 0.025(3) 0.048(4) -0.014(3) 0.003(3) -0.007(2) C7A 0.021(3) 0.020(3) 0.045(4) -0.004(2) -0.001(2) -0.005(2) C8A 0.028(3) 0.030(3) 0.049(4) 0.007(3) 0.008(3) -0.001(3) C9A 0.019(3) 0.040(4) 0.076(5) -0.001(3) 0.009(3) 0.001(3) C10A 0.035(4) 0.035(4) 0.060(4) 0.001(3) -0.007(3) 0.006(3) C11A 0.040(4) 0.032(3) 0.051(4) 0.000(3) -0.004(3) -0.001(3) C12A 0.029(3) 0.029(3) 0.039(4) 0.000(3) -0.005(3) -0.003(2) C13A 0.022(3) 0.030(3) 0.038(3) -0.001(3) 0.003(2) -0.002(2) C14A 0.027(3) 0.034(3) 0.057(4) -0.002(3) 0.005(3) -0.002(3) C15A 0.033(3) 0.035(3) 0.050(4) -0.001(3) 0.006(3) -0.005(3) C16A 0.024(3) 0.042(4) 0.055(4) 0.003(3) 0.003(3) -0.006(3) C17A 0.025(3) 0.045(4) 0.070(5) -0.001(3) 0.009(3) 0.006(3) C18A 0.026(3) 0.033(3) 0.051(4) 0.000(3) 0.007(3) 0.002(3) C19A 0.024(3) 0.032(3) 0.041(3) 0.005(3) 0.009(3) -0.001(2) C20A 0.032(3) 0.036(3) 0.040(4) 0.002(3) 0.006(3) 0.009(3) C21A 0.044(4) 0.047(4) 0.048(4) 0.008(3) 0.011(3) 0.016(3) C22A 0.028(4) 0.056(4) 0.078(5) 0.016(4) 0.015(3) 0.016(3) C23A 0.029(4) 0.060(4) 0.056(4) 0.007(3) 0.000(3) 0.009(3) C24A 0.033(4) 0.038(4) 0.046(4) 0.001(3) 0.008(3) -0.001(3) C25A 0.030(3) 0.031(3) 0.033(3) -0.004(3) 0.003(3) -0.007(3) C26A 0.031(3) 0.026(3) 0.069(4) 0.005(3) 0.011(3) 0.003(3) C27A 0.053(4) 0.033(4) 0.072(5) 0.010(3) 0.010(4) 0.012(3) C28A 0.054(4) 0.030(3) 0.050(4) 0.002(3) 0.003(3) -0.002(3) C29A 0.041(4) 0.036(4) 0.045(4) 0.002(3) 0.000(3) -0.016(3) C30A 0.029(3) 0.034(3) 0.041(4) 0.001(3) -0.005(3) -0.003(3) C1B 0.016(3) 0.025(3) 0.052(4) -0.011(3) 0.002(3) -0.004(2) C2B 0.022(3) 0.025(3) 0.031(3) 0.001(2) 0.001(2) -0.001(3) C3B 0.025(3) 0.026(3) 0.044(4) -0.001(3) 0.005(3) -0.011(3) C4B 0.025(3) 0.027(3) 0.046(4) -0.007(3) 0.003(3) 0.003(2) C5B 0.033(3) 0.029(3) 0.039(3) -0.003(3) 0.001(3) 0.000(3) C6B 0.033(3) 0.025(3) 0.034(3) -0.001(2) 0.001(3) -0.003(2) C7B 0.019(3) 0.027(3) 0.040(3) -0.006(2) 0.005(2) -0.004(2) C8B 0.033(3) 0.026(3) 0.042(4) 0.002(3) 0.006(3) 0.003(3) C9B 0.040(4) 0.038(4) 0.040(4) -0.003(3) 0.004(3) 0.012(3) C10B 0.050(4) 0.028(3) 0.043(4) 0.002(3) 0.007(3) 0.007(3) C11B 0.037(4) 0.034(3) 0.048(4) 0.008(3) 0.001(3) -0.004(3) C12B 0.030(3) 0.030(3) 0.047(4) 0.007(3) -0.003(3) -0.004(3) C13B 0.020(3) 0.026(3) 0.042(3) -0.001(3) -0.001(2) -0.004(2) C14B 0.026(3) 0.038(3) 0.047(4) -0.002(3) 0.004(3) 0.002(3) C15B 0.023(3) 0.059(4) 0.057(4) -0.004(3) 0.011(3) 0.005(3) C16B 0.016(3) 0.051(4) 0.069(5) 0.010(3) -0.003(3) -0.007(3) C17B 0.028(3) 0.035(3) 0.056(4) 0.002(3) -0.001(3) -0.007(3) C18B 0.026(3) 0.032(3) 0.043(4) 0.000(3) 0.000(3) 0.002(2) C19B 0.029(3) 0.023(3) 0.046(4) -0.002(3) 0.013(3) 0.000(2) C20B 0.051(4) 0.026(3) 0.052(4) -0.006(3) 0.010(3) -0.005(3) C21B 0.071(5) 0.030(4) 0.062(5) -0.002(3) 0.035(4) -0.004(3) C22B 0.035(4) 0.042(4) 0.085(6) -0.006(4) 0.033(4) -0.004(3) C23B 0.031(4) 0.030(3) 0.087(6) -0.003(3) 0.014(3) -0.001(3) C24B 0.026(3) 0.021(3) 0.066(4) 0.001(3) 0.011(3) -0.002(2) C25B 0.045(4) 0.030(3) 0.029(3) 0.006(2) 0.006(3) 0.006(3) C26B 0.041(4) 0.032(3) 0.052(4) 0.004(3) 0.002(3) 0.001(3) C27B 0.062(5) 0.039(4) 0.061(5) 0.017(3) 0.008(4) 0.015(4) C28B 0.048(4) 0.066(5) 0.069(5) 0.016(4) 0.002(4) 0.033(4) C29B 0.028(4) 0.065(5) 0.070(5) 0.013(4) 0.006(3) 0.013(3) C30B 0.033(4) 0.041(4) 0.046(4) 0.006(3) 0.002(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1A C1A 1.812(6) . ? Mn1A C3A 1.814(7) . ? Mn1A C2A 1.837(6) . ? Mn1A P1A 2.2881(18) . ? Mn1A P2A 2.2927(17) . ? Mn1A H1A 1.735(19) . ? Mn1B C2B 1.809(5) . ? Mn1B C3B 1.812(6) . ? Mn1B C1B 1.814(7) . ? Mn1B P2B 2.2828(18) . ? Mn1B P1B 2.3047(16) . ? Mn1B H1B 1.71(6) . ? P1A C13A 1.833(5) . ? P1A C7A 1.836(5) . ? P1A C4A 1.841(5) . ? P2A C19A 1.838(5) . ? P2A C25A 1.841(6) . ? P2A C6A 1.843(5) . ? P1B C13B 1.826(5) . ? P1B C4B 1.832(5) . ? P1B C7B 1.836(6) . ? P2B C19B 1.832(6) . ? P2B C6B 1.838(5) . ? P2B C25B 1.838(6) . ? O1A C1A 1.146(6) . ? O2A C2A 1.125(6) . ? O3A C3A 1.133(7) . ? O1B C1B 1.144(7) . ? O2B C2B 1.144(6) . ? O3B C3B 1.137(6) . ? C4A C5A 1.535(7) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C5A C6A 1.523(8) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7A C8A 1.396(7) . ? C7A C12A 1.404(8) . ? C8A C9A 1.395(8) . ? C8A H8A 0.9500 . ? C9A C10A 1.387(9) . ? C9A H9A 0.9500 . ? C10A C11A 1.376(8) . ? C10A H10A 0.9500 . ? C11A C12A 1.385(8) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A C18A 1.384(7) . ? C13A C14A 1.389(7) . ? C14A C15A 1.360(8) . ? C14A H14A 0.9500 . ? C15A C16A 1.393(8) . ? C15A H15A 0.9500 . ? C16A C17A 1.385(8) . ? C16A H16A 0.9500 . ? C17A C18A 1.390(8) . ? C17A H17A 0.9500 . ? C18A H18A 0.9500 . ? C19A C24A 1.384(8) . ? C19A C20A 1.395(7) . ? C20A C21A 1.391(8) . ? C20A H20A 0.9500 . ? C21A C22A 1.362(9) . ? C21A H21A 0.9500 . ? C22A C23A 1.392(9) . ? C22A H22A 0.9500 . ? C23A C24A 1.375(8) . ? C23A H23A 0.9500 . ? C24A H24A 0.9500 . ? C25A C26A 1.382(8) . ? C25A C30A 1.384(8) . ? C26A C27A 1.384(8) . ? C26A H26A 0.9500 . ? C27A C28A 1.382(9) . ? C27A H27A 0.9500 . ? C28A C29A 1.373(8) . ? C28A H28A 0.9500 . ? C29A C30A 1.376(8) . ? C29A H29A 0.9500 . ? C30A H30A 0.9500 . ? C4B C5B 1.538(8) . ? C4B H4B1 0.9900 . ? C4B H4B2 0.9900 . ? C5B C6B 1.526(7) . ? C5B H5B1 0.9900 . ? C5B H5B2 0.9900 . ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? C7B C12B 1.390(7) . ? C7B C8B 1.402(7) . ? C8B C9B 1.376(8) . ? C8B H8B 0.9500 . ? C9B C10B 1.391(8) . ? C9B H9B 0.9500 . ? C10B C11B 1.359(8) . ? C10B H10B 0.9500 . ? C11B C12B 1.378(8) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B C14B 1.388(8) . ? C13B C18B 1.400(7) . ? C14B C15B 1.383(8) . ? C14B H14B 0.9500 . ? C15B C16B 1.382(8) . ? C15B H15B 0.9500 . ? C16B C17B 1.387(8) . ? C16B H16B 0.9500 . ? C17B C18B 1.397(8) . ? C17B H17B 0.9500 . ? C18B H18B 0.9500 . ? C19B C24B 1.379(8) . ? C19B C20B 1.402(8) . ? C20B C21B 1.395(9) . ? C20B H20B 0.9500 . ? C21B C22B 1.390(10) . ? C21B H21B 0.9500 . ? C22B C23B 1.335(10) . ? C22B H22B 0.9500 . ? C23B C24B 1.404(8) . ? C23B H23B 0.9500 . ? C24B H24B 0.9500 . ? C25B C26B 1.389(7) . ? C25B C30B 1.393(8) . ? C26B C27B 1.381(8) . ? C26B H26B 0.9500 . ? C27B C28B 1.382(10) . ? C27B H27B 0.9500 . ? C28B C29B 1.373(9) . ? C28B H28B 0.9500 . ? C29B C30B 1.359(8) . ? C29B H29B 0.9500 . ? C30B H30B 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 C1A Mn1A C3A 88.2(2) . . ? C1A Mn1A C2A 96.2(2) . . ? C3A Mn1A C2A 95.2(2) . . ? C1A Mn1A P1A 89.70(18) . . ? C3A Mn1A P1A 175.28(17) . . ? C2A Mn1A P1A 89.19(18) . . ? C1A Mn1A P2A 170.90(17) . . ? C3A Mn1A P2A 90.54(18) . . ? C2A Mn1A P2A 92.87(17) . . ? P1A Mn1A P2A 90.85(6) . . ? C1A Mn1A H1A 82.4(15) . . ? C3A Mn1A H1A 87.1(14) . . ? C2A Mn1A H1A 177.3(15) . . ? P1A Mn1A H1A 88.5(14) . . ? P2A Mn1A H1A 88.5(15) . . ? C2B Mn1B C3B 94.6(2) . . ? C2B Mn1B C1B 98.2(2) . . ? C3B Mn1B C1B 87.6(2) . . ? C2B Mn1B P2B 92.24(17) . . ? C3B Mn1B P2B 90.01(19) . . ? C1B Mn1B P2B 169.46(17) . . ? C2B Mn1B P1B 91.83(16) . . ? C3B Mn1B P1B 173.59(17) . . ? C1B Mn1B P1B 91.81(17) . . ? P2B Mn1B P1B 89.42(6) . . ? C2B Mn1B H1B 175.4(19) . . ? C3B Mn1B H1B 85.3(18) . . ? C1B Mn1B H1B 86.4(19) . . ? P2B Mn1B H1B 83.2(19) . . ? P1B Mn1B H1B 88.3(18) . . ? C13A P1A C7A 102.3(2) . . ? C13A P1A C4A 102.4(2) . . ? C7A P1A C4A 100.4(2) . . ? C13A P1A Mn1A 112.51(18) . . ? C7A P1A Mn1A 122.35(19) . . ? C4A P1A Mn1A 114.28(18) . . ? C19A P2A C25A 101.4(3) . . ? C19A P2A C6A 104.0(3) . . ? C25A P2A C6A 99.5(2) . . ? C19A P2A Mn1A 118.34(19) . . ? C25A P2A Mn1A 116.42(18) . . ? C6A P2A Mn1A 114.59(18) . . ? C13B P1B C4B 103.9(2) . . ? C13B P1B C7B 101.3(2) . . ? C4B P1B C7B 99.7(2) . . ? C13B P1B Mn1B 119.23(18) . . ? C4B P1B Mn1B 113.79(18) . . ? C7B P1B Mn1B 116.26(17) . . ? C19B P2B C6B 101.0(2) . . ? C19B P2B C25B 103.1(3) . . ? C6B P2B C25B 101.0(2) . . ? C19B P2B Mn1B 120.5(2) . . ? C6B P2B Mn1B 113.65(19) . . ? C25B P2B Mn1B 115.01(19) . . ? O1A C1A Mn1A 176.1(5) . . ? O2A C2A Mn1A 178.8(5) . . ? O3A C3A Mn1A 177.1(5) . . ? C5A C4A P1A 112.6(4) . . ? C5A C4A H4A1 109.1 . . ? P1A C4A H4A1 109.1 . . ? C5A C4A H4A2 109.1 . . ? P1A C4A H4A2 109.1 . . ? H4A1 C4A H4A2 107.8 . . ? C6A C5A C4A 113.6(4) . . ? C6A C5A H5A1 108.9 . . ? C4A C5A H5A1 108.9 . . ? C6A C5A H5A2 108.9 . . ? C4A C5A H5A2 108.9 . . ? H5A1 C5A H5A2 107.7 . . ? C5A C6A P2A 113.7(4) . . ? C5A C6A H6A1 108.8 . . ? P2A C6A H6A1 108.8 . . ? C5A C6A H6A2 108.8 . . ? P2A C6A H6A2 108.8 . . ? H6A1 C6A H6A2 107.7 . . ? C8A C7A C12A 118.4(5) . . ? C8A C7A P1A 121.0(4) . . ? C12A C7A P1A 120.5(4) . . ? C9A C8A C7A 120.3(6) . . ? C9A C8A H8A 119.9 . . ? C7A C8A H8A 119.9 . . ? C10A C9A C8A 119.7(6) . . ? C10A C9A H9A 120.2 . . ? C8A C9A H9A 120.2 . . ? C11A C10A C9A 121.2(6) . . ? C11A C10A H10A 119.4 . . ? C9A C10A H10A 119.4 . . ? C10A C11A C12A 119.1(6) . . ? C10A C11A H11A 120.5 . . ? C12A C11A H11A 120.5 . . ? C11A C12A C7A 121.4(6) . . ? C11A C12A H12A 119.3 . . ? C7A C12A H12A 119.3 . . ? C18A C13A C14A 118.6(5) . . ? C18A C13A P1A 121.6(4) . . ? C14A C13A P1A 119.7(4) . . ? C15A C14A C13A 121.2(5) . . ? C15A C14A H14A 119.4 . . ? C13A C14A H14A 119.4 . . ? C14A C15A C16A 120.5(6) . . ? C14A C15A H15A 119.8 . . ? C16A C15A H15A 119.8 . . ? C17A C16A C15A 119.0(5) . . ? C17A C16A H16A 120.5 . . ? C15A C16A H16A 120.5 . . ? C16A C17A C18A 120.2(5) . . ? C16A C17A H17A 119.9 . . ? C18A C17A H17A 119.9 . . ? C13A C18A C17A 120.4(5) . . ? C13A C18A H18A 119.8 . . ? C17A C18A H18A 119.8 . . ? C24A C19A C20A 119.3(5) . . ? C24A C19A P2A 123.4(4) . . ? C20A C19A P2A 117.1(4) . . ? C21A C20A C19A 119.9(6) . . ? C21A C20A H20A 120.0 . . ? C19A C20A H20A 120.0 . . ? C22A C21A C20A 120.2(6) . . ? C22A C21A H21A 119.9 . . ? C20A C21A H21A 119.9 . . ? C21A C22A C23A 120.2(6) . . ? C21A C22A H22A 119.9 . . ? C23A C22A H22A 119.9 . . ? C24A C23A C22A 120.0(6) . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C23A C24A C19A 120.4(6) . . ? C23A C24A H24A 119.8 . . ? C19A C24A H24A 119.8 . . ? C26A C25A C30A 117.7(5) . . ? C26A C25A P2A 118.7(4) . . ? C30A C25A P2A 123.6(4) . . ? C25A C26A C27A 121.0(6) . . ? C25A C26A H26A 119.5 . . ? C27A C26A H26A 119.5 . . ? C28A C27A C26A 121.0(6) . . ? C28A C27A H27A 119.5 . . ? C26A C27A H27A 119.5 . . ? C29A C28A C27A 117.7(6) . . ? C29A C28A H28A 121.2 . . ? C27A C28A H28A 121.2 . . ? C28A C29A C30A 121.6(6) . . ? C28A C29A H29A 119.2 . . ? C30A C29A H29A 119.2 . . ? C29A C30A C25A 120.9(5) . . ? C29A C30A H30A 119.5 . . ? C25A C30A H30A 119.5 . . ? O1B C1B Mn1B 175.1(5) . . ? O2B C2B Mn1B 178.6(5) . . ? O3B C3B Mn1B 177.4(5) . . ? C5B C4B P1B 114.0(4) . . ? C5B C4B H4B1 108.7 . . ? P1B C4B H4B1 108.7 . . ? C5B C4B H4B2 108.7 . . ? P1B C4B H4B2 108.7 . . ? H4B1 C4B H4B2 107.6 . . ? C6B C5B C4B 114.7(5) . . ? C6B C5B H5B1 108.6 . . ? C4B C5B H5B1 108.6 . . ? C6B C5B H5B2 108.6 . . ? C4B C5B H5B2 108.6 . . ? H5B1 C5B H5B2 107.6 . . ? C5B C6B P2B 113.1(4) . . ? C5B C6B H6B1 109.0 . . ? P2B C6B H6B1 109.0 . . ? C5B C6B H6B2 109.0 . . ? P2B C6B H6B2 109.0 . . ? H6B1 C6B H6B2 107.8 . . ? C12B C7B C8B 116.8(5) . . ? C12B C7B P1B 120.2(4) . . ? C8B C7B P1B 123.0(4) . . ? C9B C8B C7B 121.3(5) . . ? C9B C8B H8B 119.3 . . ? C7B C8B H8B 119.3 . . ? C8B C9B C10B 120.3(5) . . ? C8B C9B H9B 119.8 . . ? C10B C9B H9B 119.8 . . ? C11B C10B C9B 118.9(6) . . ? C11B C10B H10B 120.6 . . ? C9B C10B H10B 120.6 . . ? C10B C11B C12B 121.2(6) . . ? C10B C11B H11B 119.4 . . ? C12B C11B H11B 119.4 . . ? C11B C12B C7B 121.5(5) . . ? C11B C12B H12B 119.3 . . ? C7B C12B H12B 119.3 . . ? C14B C13B C18B 118.6(5) . . ? C14B C13B P1B 123.6(4) . . ? C18B C13B P1B 117.8(4) . . ? C15B C14B C13B 120.4(5) . . ? C15B C14B H14B 119.8 . . ? C13B C14B H14B 119.8 . . ? C16B C15B C14B 121.2(6) . . ? C16B C15B H15B 119.4 . . ? C14B C15B H15B 119.4 . . ? C15B C16B C17B 119.4(5) . . ? C15B C16B H16B 120.3 . . ? C17B C16B H16B 120.3 . . ? C16B C17B C18B 119.7(6) . . ? C16B C17B H17B 120.2 . . ? C18B C17B H17B 120.2 . . ? C17B C18B C13B 120.8(5) . . ? C17B C18B H18B 119.6 . . ? C13B C18B H18B 119.6 . . ? C24B C19B C20B 119.2(5) . . ? C24B C19B P2B 121.6(5) . . ? C20B C19B P2B 119.1(4) . . ? C19B C20B C21B 120.2(6) . . ? C19B C20B H20B 119.9 . . ? C21B C20B H20B 119.9 . . ? C22B C21B C20B 118.6(7) . . ? C22B C21B H21B 120.7 . . ? C20B C21B H21B 120.7 . . ? C23B C22B C21B 121.8(6) . . ? C23B C22B H22B 119.1 . . ? C21B C22B H22B 119.1 . . ? C22B C23B C24B 120.3(7) . . ? C22B C23B H23B 119.8 . . ? C24B C23B H23B 119.8 . . ? C19B C24B C23B 119.9(6) . . ? C19B C24B H24B 120.0 . . ? C23B C24B H24B 120.0 . . ? C26B C25B C30B 117.9(5) . . ? C26B C25B P2B 121.9(4) . . ? C30B C25B P2B 120.1(4) . . ? C27B C26B C25B 120.6(6) . . ? C27B C26B H26B 119.7 . . ? C25B C26B H26B 119.7 . . ? C26B C27B C28B 120.1(6) . . ? C26B C27B H27B 119.9 . . ? C28B C27B H27B 119.9 . . ? C29B C28B C27B 119.3(6) . . ? C29B C28B H28B 120.3 . . ? C27B C28B H28B 120.3 . . ? C30B C29B C28B 120.7(6) . . ? C30B C29B H29B 119.7 . . ? C28B C29B H29B 119.7 . . ? C29B C30B C25B 121.2(6) . . ? C29B C30B H30B 119.4 . . ? C25B C30B H30B 119.4 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 23.37 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.224 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.184 #=====END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H33 Mn O6 P2 S' _chemical_formula_weight 722.57 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' 'O' 'O' 0.0106 0.0060 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.539(3) _cell_length_b 14.793(4) _cell_length_c 21.716(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.534(5) _cell_angle_gamma 90.00 _cell_volume 3385.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1015 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 23.28 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.592 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14890 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 23.32 _reflns_number_total 4885 _reflns_number_gt 4378 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+3.0794P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4885 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 Mn1 Mn 0.56700(4) 0.79101(3) 0.804135(19) 0.01539(16) Uani 1 1 d . . . P2 P 0.74285(7) 0.72857(5) 0.85587(3) 0.0168(2) Uani 1 1 d . . . S1 S 0.68481(7) 0.77664(5) 0.67119(3) 0.0183(2) Uani 1 1 d . . . P1 P 0.45861(7) 0.65245(5) 0.81747(3) 0.0160(2) Uani 1 1 d . . . O1 O 0.64530(19) 0.72654(13) 0.72764(9) 0.0184(5) Uani 1 1 d . . . O3 O 0.8046(2) 0.82071(14) 0.67972(10) 0.0274(5) Uani 1 1 d . . . O4 O 0.3517(2) 0.86519(14) 0.73082(10) 0.0248(5) Uani 1 1 d . . . O5 O 0.4671(2) 0.88757(14) 0.91108(10) 0.0283(5) Uani 1 1 d . . . C16 C 0.2980(3) 0.7019(2) 0.91172(14) 0.0235(7) Uani 1 1 d . . . H16 H 0.2857 0.7538 0.8882 0.028 Uiso 1 1 calc R . . O2 O 0.5841(2) 0.83290(14) 0.64759(9) 0.0266(5) Uani 1 1 d . . . C10 C 0.7463(3) 0.71268(19) 0.93950(14) 0.0212(7) Uani 1 1 d . . . C24 C 0.1238(3) 0.5718(2) 0.73581(17) 0.0300(8) Uani 1 1 d . . . H24 H 0.0472 0.5460 0.7475 0.036 Uiso 1 1 calc R . . C5 C 0.9698(3) 0.7675(2) 0.79539(14) 0.0234(7) Uani 1 1 d . . . H5 H 0.9541 0.7153 0.7727 0.028 Uiso 1 1 calc R . . C15 C 0.3795(3) 0.6350(2) 0.89087(13) 0.0192(7) Uani 1 1 d . . . C8 C 1.0749(3) 0.8195(2) 0.78238(16) 0.0284(7) Uani 1 1 d . . . H8 H 1.1297 0.8018 0.7513 0.034 Uiso 1 1 calc R . . C32 C 0.8442(3) 0.5841(2) 0.56692(15) 0.0315(8) Uani 1 1 d . . . H32 H 0.9246 0.5593 0.5621 0.038 Uiso 1 1 calc R . . C26 C 0.5051(3) 0.84536(19) 0.87017(14) 0.0200(7) Uani 1 1 d . . . C4 C 0.8875(3) 0.79207(19) 0.84164(14) 0.0199(7) Uani 1 1 d . . . C17 C 0.2353(3) 0.6925(2) 0.96675(16) 0.0310(8) Uani 1 1 d . . . H17 H 0.1811 0.7379 0.9801 0.037 Uiso 1 1 calc R . . C11 C 0.6384(3) 0.71747(19) 0.97520(14) 0.0228(7) Uani 1 1 d . . . H11 H 0.5613 0.7331 0.9569 0.027 Uiso 1 1 calc R . . C28 C 0.7073(3) 0.68889(19) 0.61705(13) 0.0194(7) Uani 1 1 d . . . C19 C 0.3311(3) 0.5479(2) 0.98131(14) 0.0286(8) Uani 1 1 d . . . H19 H 0.3416 0.4956 1.0046 0.034 Uiso 1 1 calc R . . C21 C 0.3493(3) 0.6499(2) 0.70065(14) 0.0245(7) Uani 1 1 d . . . H21 H 0.4251 0.6765 0.6886 0.029 Uiso 1 1 calc R . . C30 C 0.6265(3) 0.5902(2) 0.53898(14) 0.0257(7) Uani 1 1 d . . . H30 H 0.5588 0.5700 0.5149 0.031 Uiso 1 1 calc R . . C12 C 0.6435(4) 0.6992(2) 1.03789(15) 0.0317(8) Uani 1 1 d . . . H12 H 0.5704 0.7031 1.0614 0.038 Uiso 1 1 calc R . . C27 C 0.4345(3) 0.83499(19) 0.75779(14) 0.0197(7) Uani 1 1 d . . . C29 C 0.6071(3) 0.6583(2) 0.58173(14) 0.0236(7) Uani 1 1 d . . . H29 H 0.5268 0.6832 0.5865 0.028 Uiso 1 1 calc R . . C20 C 0.3302(3) 0.62970(18) 0.76245(14) 0.0189(6) Uani 1 1 d . . . C1 C 0.5579(3) 0.55272(19) 0.80520(13) 0.0188(6) Uani 1 1 d . . . H1A H 0.5065 0.4994 0.8124 0.023 Uiso 1 1 calc R . . H1B H 0.5826 0.5517 0.7623 0.023 Uiso 1 1 calc R . . C31 C 0.7454(3) 0.5520(2) 0.53167(14) 0.0247(7) Uani 1 1 d . . . C18 C 0.3943(3) 0.5568(2) 0.92605(14) 0.0225(7) Uani 1 1 d . . . H18 H 0.4467 0.5106 0.9124 0.027 Uiso 1 1 calc R . . C7 C 1.0172(3) 0.9229(2) 0.86090(16) 0.0310(8) Uani 1 1 d . . . H7 H 1.0326 0.9757 0.8830 0.037 Uiso 1 1 calc R . . C6 C 0.9122(3) 0.8709(2) 0.87438(15) 0.0285(8) Uani 1 1 d . . . H6 H 0.8578 0.8888 0.9055 0.034 Uiso 1 1 calc R . . C25 C 0.2162(3) 0.5903(2) 0.77982(15) 0.0246(7) Uani 1 1 d . . . H25 H 0.2019 0.5765 0.8209 0.030 Uiso 1 1 calc R . . C23 C 0.1448(3) 0.5914(2) 0.67500(16) 0.0315(8) Uani 1 1 d . . . H23 H 0.0829 0.5779 0.6456 0.038 Uiso 1 1 calc R . . C9 C 1.0992(3) 0.8974(2) 0.81518(14) 0.0247(7) Uani 1 1 d . . . H9 H 1.1703 0.9324 0.8065 0.030 Uiso 1 1 calc R . . C22 C 0.2571(3) 0.6309(2) 0.65725(15) 0.0293(8) Uani 1 1 d . . . H22 H 0.2705 0.6447 0.6160 0.035 Uiso 1 1 calc R . . C33 C 0.8267(3) 0.6525(2) 0.60953(15) 0.0278(7) Uani 1 1 d . . . H33 H 0.8948 0.6738 0.6329 0.033 Uiso 1 1 calc R . . C3 C 0.7801(3) 0.61468(19) 0.82889(14) 0.0200(7) Uani 1 1 d . . . H3A H 0.7906 0.6161 0.7846 0.024 Uiso 1 1 calc R . . H3B H 0.8601 0.5957 0.8471 0.024 Uiso 1 1 calc R . . C14 C 0.7571(4) 0.6754(2) 1.06523(15) 0.0363(9) Uani 1 1 d . . . H14 H 0.7606 0.6630 1.1072 0.044 Uiso 1 1 calc R . . C13 C 0.8606(3) 0.6885(2) 0.96810(15) 0.0289(8) Uani 1 1 d . . . H13 H 0.9342 0.6850 0.9449 0.035 Uiso 1 1 calc R . . C2 C 0.6779(3) 0.54512(19) 0.84471(14) 0.0193(6) Uani 1 1 d . . . H2A H 0.7131 0.4850 0.8398 0.023 Uiso 1 1 calc R . . H2B H 0.6552 0.5523 0.8876 0.023 Uiso 1 1 calc R . . O6 O 0.6982(2) 0.96650(14) 0.78607(10) 0.0270(5) Uani 1 1 d . . . C36 C 0.6532(3) 0.8969(2) 0.79111(13) 0.0198(7) Uani 1 1 d . . . C35 C 0.2528(3) 0.6157(2) 1.00233(15) 0.0322(8) Uani 1 1 d . . . H35 H 0.2122 0.6099 1.0400 0.039 Uiso 1 1 calc R . . C37 C 0.7657(3) 0.4779(2) 0.48480(16) 0.0333(8) Uani 1 1 d . . . H37A H 0.7776 0.5043 0.4449 0.050 Uiso 1 1 calc R . . H37B H 0.6928 0.4390 0.4837 0.050 Uiso 1 1 calc R . . H37C H 0.8395 0.4434 0.4961 0.050 Uiso 1 1 calc R . . C34 C 0.8656(4) 0.6698(2) 1.03042(16) 0.0363(9) Uani 1 1 d . . . H34 H 0.9422 0.6535 1.0489 0.044 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 Mn1 0.0182(3) 0.0135(3) 0.0145(3) -0.00084(17) 0.00001(19) -0.00078(17) P2 0.0187(4) 0.0157(4) 0.0160(4) -0.0021(3) -0.0015(3) -0.0005(3) S1 0.0237(4) 0.0162(4) 0.0150(4) 0.0005(3) 0.0007(3) 0.0013(3) P1 0.0190(4) 0.0152(4) 0.0139(4) -0.0002(3) -0.0009(3) -0.0016(3) O1 0.0253(11) 0.0161(10) 0.0137(10) -0.0004(8) 0.0008(9) 0.0003(8) O3 0.0288(12) 0.0240(12) 0.0294(12) -0.0023(9) 0.0036(10) -0.0067(9) O4 0.0197(12) 0.0244(12) 0.0300(12) 0.0012(10) -0.0034(10) 0.0034(9) O5 0.0360(13) 0.0244(12) 0.0245(12) -0.0057(10) 0.0068(10) 0.0016(10) C16 0.0256(17) 0.0221(16) 0.0228(17) -0.0003(13) 0.0020(14) -0.0041(13) O2 0.0358(13) 0.0252(12) 0.0189(11) 0.0019(9) 0.0003(10) 0.0106(10) C10 0.0282(18) 0.0167(15) 0.0184(16) -0.0025(12) -0.0055(14) -0.0026(12) C24 0.0196(17) 0.0196(17) 0.051(2) -0.0115(15) -0.0064(16) 0.0007(13) C5 0.0210(16) 0.0208(16) 0.0284(18) -0.0070(13) 0.0014(14) -0.0008(13) C15 0.0200(16) 0.0206(16) 0.0171(15) -0.0024(12) -0.0017(12) -0.0062(12) C8 0.0221(17) 0.0298(18) 0.0334(19) -0.0041(15) 0.0066(14) 0.0016(14) C32 0.0282(18) 0.038(2) 0.0288(19) -0.0051(15) -0.0004(15) 0.0109(15) C26 0.0222(16) 0.0172(15) 0.0207(17) 0.0022(13) -0.0020(13) -0.0021(13) C4 0.0196(16) 0.0195(16) 0.0206(16) 0.0005(12) -0.0059(13) 0.0013(12) C17 0.0317(19) 0.0307(19) 0.0309(19) -0.0088(15) 0.0091(15) -0.0027(15) C11 0.0320(18) 0.0171(16) 0.0193(16) -0.0032(12) -0.0022(14) -0.0032(13) C28 0.0274(17) 0.0161(15) 0.0147(15) 0.0025(12) 0.0014(13) 0.0009(13) C19 0.0359(19) 0.0302(18) 0.0198(17) 0.0051(14) 0.0014(14) -0.0062(15) C21 0.0308(18) 0.0201(16) 0.0225(17) -0.0023(13) -0.0048(14) -0.0020(13) C30 0.0276(17) 0.0273(17) 0.0221(17) -0.0015(14) -0.0004(13) -0.0078(14) C12 0.047(2) 0.0261(18) 0.0217(18) -0.0031(14) 0.0017(16) -0.0027(15) C27 0.0272(18) 0.0122(15) 0.0197(16) -0.0027(12) 0.0054(14) -0.0047(13) C29 0.0227(17) 0.0258(17) 0.0224(17) -0.0003(13) 0.0031(13) -0.0017(13) C20 0.0226(16) 0.0123(14) 0.0217(16) -0.0019(12) -0.0046(13) 0.0007(12) C1 0.0241(16) 0.0157(15) 0.0164(15) -0.0022(12) -0.0002(13) -0.0031(12) C31 0.0335(18) 0.0228(16) 0.0178(16) 0.0012(13) 0.0033(14) -0.0036(14) C18 0.0243(16) 0.0222(16) 0.0209(16) 0.0006(13) 0.0002(13) -0.0024(13) C7 0.0355(19) 0.0228(17) 0.035(2) -0.0070(14) 0.0003(16) -0.0082(15) C6 0.0309(18) 0.0268(18) 0.0278(18) -0.0090(14) 0.0061(15) -0.0056(14) C25 0.0245(17) 0.0200(16) 0.0294(18) -0.0048(13) 0.0011(14) 0.0001(13) C23 0.0326(19) 0.0239(17) 0.038(2) -0.0122(15) -0.0200(16) 0.0105(15) C9 0.0196(16) 0.0230(17) 0.0316(18) 0.0031(14) -0.0017(14) -0.0045(13) C22 0.043(2) 0.0203(17) 0.0240(18) -0.0027(14) -0.0118(15) 0.0029(15) C33 0.0271(18) 0.0330(19) 0.0233(17) -0.0054(14) -0.0046(14) 0.0046(14) C3 0.0197(16) 0.0188(16) 0.0215(16) -0.0024(12) -0.0024(13) 0.0023(12) C14 0.062(3) 0.0291(19) 0.0175(18) -0.0011(14) -0.0085(17) -0.0040(18) C13 0.0305(18) 0.0295(18) 0.0265(18) -0.0001(14) -0.0067(14) -0.0038(15) C2 0.0240(16) 0.0149(15) 0.0192(16) -0.0009(12) -0.0017(13) 0.0021(12) O6 0.0333(12) 0.0183(12) 0.0293(13) 0.0008(9) 0.0020(10) -0.0060(10) C36 0.0214(16) 0.0231(18) 0.0149(15) -0.0025(12) -0.0004(12) 0.0028(14) C35 0.037(2) 0.040(2) 0.0194(17) -0.0019(15) 0.0096(15) -0.0094(16) C37 0.042(2) 0.0293(19) 0.0289(19) -0.0066(15) 0.0068(16) -0.0022(16) C34 0.046(2) 0.0318(19) 0.031(2) 0.0014(15) -0.0190(17) -0.0035(16) _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 Mn1 C26 1.774(3) . ? Mn1 C27 1.833(3) . ? Mn1 C36 1.834(3) . ? Mn1 O1 2.092(2) . ? Mn1 P2 2.3477(10) . ? Mn1 P1 2.3658(10) . ? P2 C4 1.820(3) . ? P2 C3 1.828(3) . ? P2 C10 1.831(3) . ? S1 O3 1.431(2) . ? S1 O2 1.439(2) . ? S1 O1 1.495(2) . ? S1 C28 1.769(3) . ? P1 C15 1.824(3) . ? P1 C20 1.828(3) . ? P1 C1 1.830(3) . ? O4 C27 1.138(4) . ? O5 C26 1.160(4) . ? C16 C17 1.378(5) . ? C16 C15 1.390(4) . ? C10 C11 1.384(5) . ? C10 C13 1.396(5) . ? C24 C23 1.372(5) . ? C24 C25 1.385(4) . ? C5 C8 1.380(5) . ? C5 C4 1.382(4) . ? C15 C18 1.394(4) . ? C8 C9 1.378(5) . ? C32 C31 1.372(5) . ? C32 C33 1.385(5) . ? C4 C6 1.389(4) . ? C17 C35 1.386(5) . ? C11 C12 1.388(5) . ? C28 C29 1.376(4) . ? C28 C33 1.380(4) . ? C19 C35 1.379(5) . ? C19 C18 1.384(4) . ? C21 C22 1.377(4) . ? C21 C20 1.391(4) . ? C30 C31 1.385(5) . ? C30 C29 1.386(4) . ? C12 C14 1.377(5) . ? C20 C25 1.391(4) . ? C1 C2 1.526(4) . ? C31 C37 1.512(4) . ? C7 C9 1.375(5) . ? C7 C6 1.381(5) . ? C23 C22 1.378(5) . ? C3 C2 1.531(4) . ? C14 C34 1.379(5) . ? C13 C34 1.382(5) . ? O6 C36 1.139(4) . ? 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 C26 Mn1 C27 89.94(13) . . ? C26 Mn1 C36 85.63(13) . . ? C27 Mn1 C36 89.30(13) . . ? C26 Mn1 O1 178.27(11) . . ? C27 Mn1 O1 91.71(11) . . ? C36 Mn1 O1 93.87(11) . . ? C26 Mn1 P2 94.94(10) . . ? C27 Mn1 P2 175.12(9) . . ? C36 Mn1 P2 91.15(9) . . ? O1 Mn1 P2 83.40(6) . . ? C26 Mn1 P1 96.43(10) . . ? C27 Mn1 P1 90.49(9) . . ? C36 Mn1 P1 177.92(9) . . ? O1 Mn1 P1 84.07(6) . . ? P2 Mn1 P1 88.88(3) . . ? C4 P2 C3 103.81(14) . . ? C4 P2 C10 103.05(14) . . ? C3 P2 C10 101.38(14) . . ? C4 P2 Mn1 111.99(10) . . ? C3 P2 Mn1 112.35(10) . . ? C10 P2 Mn1 122.23(11) . . ? O3 S1 O2 115.42(14) . . ? O3 S1 O1 111.83(12) . . ? O2 S1 O1 111.64(13) . . ? O3 S1 C28 107.26(14) . . ? O2 S1 C28 106.89(14) . . ? O1 S1 C28 102.78(12) . . ? C15 P1 C20 101.75(14) . . ? C15 P1 C1 106.24(14) . . ? C20 P1 C1 100.22(13) . . ? C15 P1 Mn1 117.06(10) . . ? C20 P1 Mn1 115.78(10) . . ? C1 P1 Mn1 113.78(10) . . ? S1 O1 Mn1 122.69(11) . . ? C17 C16 C15 120.9(3) . . ? C11 C10 C13 118.3(3) . . ? C11 C10 P2 122.7(2) . . ? C13 C10 P2 118.9(2) . . ? C23 C24 C25 120.2(3) . . ? C8 C5 C4 120.9(3) . . ? C16 C15 C18 118.6(3) . . ? C16 C15 P1 118.2(2) . . ? C18 C15 P1 123.2(2) . . ? C9 C8 C5 120.4(3) . . ? C31 C32 C33 121.3(3) . . ? O5 C26 Mn1 174.4(3) . . ? C5 C4 C6 118.5(3) . . ? C5 C4 P2 121.4(2) . . ? C6 C4 P2 120.0(2) . . ? C16 C17 C35 120.3(3) . . ? C10 C11 C12 121.0(3) . . ? C29 C28 C33 120.1(3) . . ? C29 C28 S1 120.3(2) . . ? C33 C28 S1 119.5(2) . . ? C35 C19 C18 120.8(3) . . ? C22 C21 C20 120.6(3) . . ? C31 C30 C29 120.8(3) . . ? C14 C12 C11 119.9(3) . . ? O4 C27 Mn1 177.1(3) . . ? C28 C29 C30 119.7(3) . . ? C21 C20 C25 119.0(3) . . ? C21 C20 P1 118.5(2) . . ? C25 C20 P1 122.4(2) . . ? C2 C1 P1 116.7(2) . . ? C32 C31 C30 118.6(3) . . ? C32 C31 C37 121.0(3) . . ? C30 C31 C37 120.5(3) . . ? C19 C18 C15 120.1(3) . . ? C9 C7 C6 120.7(3) . . ? C7 C6 C4 120.4(3) . . ? C24 C25 C20 119.9(3) . . ? C24 C23 C22 120.4(3) . . ? C8 C9 C7 119.2(3) . . ? C21 C22 C23 119.9(3) . . ? C28 C33 C32 119.4(3) . . ? C2 C3 P2 113.2(2) . . ? C12 C14 C34 120.0(3) . . ? C34 C13 C10 120.8(3) . . ? C1 C2 C3 113.9(2) . . ? O6 C36 Mn1 173.7(3) . . ? C19 C35 C17 119.2(3) . . ? C14 C34 C13 120.0(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.266 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.188 #=====END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H31 Mn O4 P2' _chemical_formula_weight 596.45 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' 'O' 'O' 0.0106 0.0060 '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' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.921(4) _cell_length_b 10.031(5) _cell_length_c 18.271(9) _cell_angle_alpha 94.634(8) _cell_angle_beta 93.541(9) _cell_angle_gamma 91.340(9) _cell_volume 1443.7(12) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 679 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 22.64 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6428 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0831 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 23.30 _reflns_number_total 4098 _reflns_number_gt 2902 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1123P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4098 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1871 _refine_ls_wR_factor_gt 0.1671 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Mn1 Mn 0.56813(10) 0.67712(8) 0.77703(4) 0.0238(3) Uani 1 1 d . . . P1 P 0.56184(18) 0.54927(14) 0.66456(7) 0.0243(4) Uani 1 1 d . . . P2 P 0.32404(18) 0.56112(14) 0.80912(7) 0.0234(4) Uani 1 1 d . . . O1 O 0.8538(5) 0.8456(4) 0.7340(2) 0.0342(10) Uani 1 1 d . . . O4 O 0.3891(5) 0.7716(4) 0.71698(19) 0.0268(9) Uani 1 1 d . . . C3 C 0.7204(7) 0.5810(5) 0.8246(3) 0.0255(13) Uani 1 1 d . . . O3 O 0.8240(5) 0.5230(4) 0.8557(2) 0.0349(10) Uani 1 1 d . . . C11 C 0.7512(7) 0.1925(5) 0.5812(3) 0.0289(13) Uani 1 1 d . . . H11 H 0.7735 0.1530 0.5351 0.035 Uiso 1 1 calc R . . C7 C 0.6531(7) 0.3819(5) 0.6555(3) 0.0246(13) Uani 1 1 d . . . C4 C 0.3510(7) 0.5153(5) 0.6189(3) 0.0251(13) Uani 1 1 d . . . H4A H 0.3029 0.5994 0.6068 0.030 Uiso 1 1 calc R . . H4B H 0.3624 0.4611 0.5731 0.030 Uiso 1 1 calc R . . C14 C 0.8379(7) 0.6175(6) 0.5825(3) 0.0313(14) Uani 1 1 d . . . H14 H 0.8940 0.5494 0.6047 0.038 Uiso 1 1 calc R . . C15 C 0.9246(7) 0.6939(6) 0.5353(3) 0.0338(15) Uani 1 1 d . . . H15 H 1.0370 0.6776 0.5266 0.041 Uiso 1 1 calc R . . C18 C 0.5892(7) 0.7439(5) 0.5632(3) 0.0281(14) Uani 1 1 d . . . H18 H 0.4777 0.7625 0.5725 0.034 Uiso 1 1 calc R . . C10 C 0.7802(7) 0.1233(6) 0.6428(3) 0.0339(15) Uani 1 1 d . . . H10 H 0.8261 0.0388 0.6385 0.041 Uiso 1 1 calc R . . C13 C 0.6709(7) 0.6403(5) 0.5970(3) 0.0243(13) Uani 1 1 d . . . C5 C 0.2283(7) 0.4432(5) 0.6651(3) 0.0258(13) Uani 1 1 d . . . H5A H 0.2837 0.3666 0.6840 0.031 Uiso 1 1 calc R . . H5B H 0.1307 0.4100 0.6337 0.031 Uiso 1 1 calc R . . C6 C 0.1670(7) 0.5334(5) 0.7306(3) 0.0252(13) Uani 1 1 d . . . H6A H 0.0654 0.4928 0.7472 0.030 Uiso 1 1 calc R . . H6B H 0.1373 0.6194 0.7135 0.030 Uiso 1 1 calc R . . C17 C 0.6759(7) 0.8193(5) 0.5156(3) 0.0298(14) Uani 1 1 d . . . H17 H 0.6208 0.8874 0.4929 0.036 Uiso 1 1 calc R . . C16 C 0.8404(8) 0.7943(6) 0.5019(3) 0.0307(14) Uani 1 1 d . . . H16 H 0.8959 0.8450 0.4698 0.037 Uiso 1 1 calc R . . C8 C 0.6775(8) 0.3087(6) 0.7174(3) 0.0325(14) Uani 1 1 d . . . H8 H 0.6510 0.3463 0.7633 0.039 Uiso 1 1 calc R . . C9 C 0.7410(8) 0.1801(6) 0.7107(3) 0.0385(16) Uani 1 1 d . . . H9 H 0.7569 0.1325 0.7521 0.046 Uiso 1 1 calc R . . C12 C 0.6886(7) 0.3208(6) 0.5877(3) 0.0310(14) Uani 1 1 d . . . H12 H 0.6703 0.3666 0.5458 0.037 Uiso 1 1 calc R . . O2 O 0.5712(5) 0.8633(4) 0.9125(2) 0.0369(10) Uani 1 1 d . . . C25 C 0.2033(7) 0.6555(5) 0.8773(3) 0.0241(13) Uani 1 1 d . . . C30 C 0.1376(7) 0.7779(5) 0.8596(3) 0.0263(13) Uani 1 1 d . . . H30 H 0.1595 0.8111 0.8150 0.032 Uiso 1 1 calc R . . C26 C 0.1700(7) 0.6101(5) 0.9454(3) 0.0245(13) Uani 1 1 d . . . H26 H 0.2118 0.5286 0.9580 0.029 Uiso 1 1 calc R . . C19 C 0.3383(7) 0.3972(6) 0.8449(3) 0.0267(13) Uani 1 1 d . . . C28 C 0.0088(7) 0.8043(6) 0.9754(3) 0.0306(14) Uani 1 1 d . . . H28 H -0.0567 0.8538 1.0075 0.037 Uiso 1 1 calc R . . C1 C 0.7425(8) 0.7811(6) 0.7480(3) 0.0278(14) Uani 1 1 d . . . C27 C 0.0751(7) 0.6850(6) 0.9949(3) 0.0311(14) Uani 1 1 d . . . H27 H 0.0566 0.6548 1.0406 0.037 Uiso 1 1 calc R . . C24 C 0.2205(8) 0.2921(5) 0.8229(3) 0.0308(14) Uani 1 1 d . . . H24 H 0.1328 0.3056 0.7883 0.037 Uiso 1 1 calc R . . C2 C 0.5619(7) 0.7919(6) 0.8600(3) 0.0262(13) Uani 1 1 d . . . C22 C 0.3611(8) 0.1475(6) 0.9044(3) 0.0365(15) Uani 1 1 d . . . H22 H 0.3695 0.0646 0.9235 0.044 Uiso 1 1 calc R . . C31 C 0.4103(7) 0.9091(6) 0.7133(3) 0.0295(14) Uani 1 1 d . . . H31A H 0.5157 0.9280 0.6914 0.035 Uiso 1 1 calc R . . H31B H 0.4159 0.9536 0.7626 0.035 Uiso 1 1 calc R . . C29 C 0.0400(7) 0.8499(6) 0.9082(3) 0.0315(14) Uani 1 1 d . . . H29 H -0.0052 0.9301 0.8953 0.038 Uiso 1 1 calc R . . C20 C 0.4660(7) 0.3731(6) 0.8984(3) 0.0300(14) Uani 1 1 d . . . H20 H 0.5454 0.4405 0.9145 0.036 Uiso 1 1 calc R . . C32 C 0.2625(8) 0.9630(6) 0.6673(3) 0.0360(15) Uani 1 1 d . . . H32A H 0.2586 0.9203 0.6182 0.054 Uiso 1 1 calc R . . H32B H 0.2781 1.0579 0.6656 0.054 Uiso 1 1 calc R . . H32C H 0.1583 0.9446 0.6892 0.054 Uiso 1 1 calc R . . C21 C 0.4757(8) 0.2491(6) 0.9279(3) 0.0362(15) Uani 1 1 d . . . H21 H 0.5604 0.2353 0.9638 0.043 Uiso 1 1 calc R . . C23 C 0.2327(8) 0.1690(6) 0.8519(3) 0.0359(15) Uani 1 1 d . . . H23 H 0.1545 0.1005 0.8360 0.043 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 Mn1 0.0243(5) 0.0293(5) 0.0184(5) 0.0076(4) -0.0026(4) 0.0026(4) P1 0.0248(9) 0.0311(9) 0.0180(7) 0.0078(6) -0.0006(6) 0.0038(6) P2 0.0245(9) 0.0274(8) 0.0185(8) 0.0056(6) -0.0021(6) 0.0025(6) O1 0.029(2) 0.041(3) 0.032(2) 0.0125(19) -0.0039(19) -0.003(2) O4 0.031(2) 0.028(2) 0.022(2) 0.0085(16) -0.0031(17) 0.0059(17) C3 0.027(3) 0.027(3) 0.024(3) 0.007(3) 0.006(3) 0.001(3) O3 0.030(2) 0.038(2) 0.037(2) 0.015(2) -0.0090(19) 0.0011(19) C11 0.033(4) 0.026(3) 0.028(3) 0.002(2) 0.010(3) 0.004(3) C7 0.018(3) 0.032(3) 0.024(3) 0.008(2) -0.003(2) -0.001(2) C4 0.028(3) 0.029(3) 0.018(3) 0.005(2) -0.006(2) 0.004(2) C14 0.030(4) 0.037(4) 0.027(3) 0.011(3) -0.007(3) 0.006(3) C15 0.024(3) 0.049(4) 0.027(3) 0.007(3) -0.007(3) -0.003(3) C18 0.024(3) 0.033(3) 0.026(3) 0.002(3) -0.005(3) 0.006(3) C10 0.035(4) 0.024(3) 0.045(4) 0.011(3) 0.003(3) 0.005(3) C13 0.024(3) 0.027(3) 0.021(3) 0.003(2) -0.004(2) 0.003(2) C5 0.027(3) 0.028(3) 0.022(3) 0.002(2) -0.003(2) 0.004(2) C6 0.025(3) 0.030(3) 0.022(3) 0.008(2) 0.000(2) 0.004(2) C17 0.038(4) 0.026(3) 0.027(3) 0.009(3) 0.001(3) 0.003(3) C16 0.037(4) 0.032(3) 0.025(3) 0.009(3) 0.006(3) -0.004(3) C8 0.049(4) 0.029(3) 0.020(3) 0.005(2) 0.002(3) 0.004(3) C9 0.053(4) 0.033(4) 0.031(4) 0.011(3) 0.002(3) 0.003(3) C12 0.025(3) 0.045(4) 0.024(3) 0.011(3) -0.001(2) 0.004(3) O2 0.040(3) 0.040(3) 0.029(2) 0.001(2) -0.0061(19) 0.005(2) C25 0.018(3) 0.028(3) 0.026(3) 0.004(2) -0.002(2) 0.000(2) C30 0.029(3) 0.025(3) 0.025(3) 0.001(2) 0.001(2) -0.004(2) C26 0.023(3) 0.028(3) 0.023(3) 0.006(2) -0.003(2) -0.001(2) C19 0.026(3) 0.035(3) 0.020(3) 0.009(2) 0.003(2) 0.004(3) C28 0.027(3) 0.032(3) 0.033(3) 0.000(3) 0.003(3) 0.000(3) C1 0.039(4) 0.027(3) 0.016(3) 0.002(2) -0.008(3) 0.011(3) C27 0.031(4) 0.041(4) 0.022(3) 0.006(3) 0.005(3) -0.002(3) C24 0.040(4) 0.031(3) 0.022(3) 0.006(3) 0.002(3) 0.000(3) C2 0.020(3) 0.028(3) 0.033(4) 0.015(3) 0.000(3) 0.002(2) C22 0.047(4) 0.031(4) 0.034(4) 0.013(3) 0.011(3) 0.010(3) C31 0.030(3) 0.036(4) 0.024(3) 0.006(3) 0.001(3) 0.005(3) C29 0.035(4) 0.031(3) 0.029(3) 0.007(3) -0.001(3) 0.004(3) C20 0.026(3) 0.038(4) 0.028(3) 0.015(3) 0.000(3) -0.004(3) C32 0.040(4) 0.040(4) 0.029(3) 0.015(3) -0.002(3) 0.003(3) C21 0.034(4) 0.044(4) 0.034(4) 0.021(3) 0.003(3) 0.007(3) C23 0.056(4) 0.026(3) 0.027(3) 0.004(3) 0.008(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C3 1.789(6) . ? Mn1 C2 1.832(6) . ? Mn1 C1 1.841(7) . ? Mn1 O4 2.037(3) . ? Mn1 P1 2.3299(18) . ? Mn1 P2 2.3624(19) . ? P1 C4 1.832(6) . ? P1 C13 1.838(6) . ? P1 C7 1.843(5) . ? P2 C19 1.821(6) . ? P2 C25 1.834(5) . ? P2 C6 1.839(5) . ? O1 C1 1.136(7) . ? O4 C31 1.394(7) . ? C3 O3 1.163(6) . ? C11 C10 1.379(8) . ? C11 C12 1.389(8) . ? C7 C12 1.385(8) . ? C7 C8 1.403(7) . ? C4 C5 1.533(8) . ? C14 C13 1.386(8) . ? C14 C15 1.399(8) . ? C15 C16 1.383(8) . ? C18 C17 1.399(8) . ? C18 C13 1.403(7) . ? C10 C9 1.379(8) . ? C5 C6 1.551(7) . ? C17 C16 1.367(8) . ? C8 C9 1.395(8) . ? O2 C2 1.148(7) . ? C25 C26 1.398(7) . ? C25 C30 1.399(7) . ? C30 C29 1.383(7) . ? C26 C27 1.394(8) . ? C19 C20 1.402(8) . ? C19 C24 1.408(8) . ? C28 C29 1.378(8) . ? C28 C27 1.382(8) . ? C24 C23 1.385(8) . ? C22 C21 1.373(9) . ? C22 C23 1.387(8) . ? C31 C32 1.534(8) . ? C20 C21 1.396(8) . ? 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 C3 Mn1 C2 89.3(2) . . ? C3 Mn1 C1 89.1(2) . . ? C2 Mn1 C1 88.6(2) . . ? C3 Mn1 O4 174.9(2) . . ? C2 Mn1 O4 95.37(19) . . ? C1 Mn1 O4 93.1(2) . . ? C3 Mn1 P1 96.74(18) . . ? C2 Mn1 P1 173.76(16) . . ? C1 Mn1 P1 89.78(17) . . ? O4 Mn1 P1 78.71(11) . . ? C3 Mn1 P2 97.11(18) . . ? C2 Mn1 P2 90.44(18) . . ? C1 Mn1 P2 173.70(17) . . ? O4 Mn1 P2 80.77(12) . . ? P1 Mn1 P2 90.54(6) . . ? C4 P1 C13 102.6(2) . . ? C4 P1 C7 101.2(2) . . ? C13 P1 C7 103.3(2) . . ? C4 P1 Mn1 115.34(18) . . ? C13 P1 Mn1 110.19(18) . . ? C7 P1 Mn1 121.95(18) . . ? C19 P2 C25 102.9(2) . . ? C19 P2 C6 103.6(3) . . ? C25 P2 C6 101.8(2) . . ? C19 P2 Mn1 121.06(19) . . ? C25 P2 Mn1 113.83(19) . . ? C6 P2 Mn1 111.52(19) . . ? C31 O4 Mn1 117.7(3) . . ? O3 C3 Mn1 177.2(5) . . ? C10 C11 C12 120.2(5) . . ? C12 C7 C8 118.0(5) . . ? C12 C7 P1 121.7(4) . . ? C8 C7 P1 120.2(4) . . ? C5 C4 P1 114.0(4) . . ? C13 C14 C15 121.9(5) . . ? C16 C15 C14 118.9(6) . . ? C17 C18 C13 119.9(5) . . ? C9 C10 C11 119.8(5) . . ? C14 C13 C18 118.0(5) . . ? C14 C13 P1 122.1(4) . . ? C18 C13 P1 119.7(4) . . ? C4 C5 C6 113.5(5) . . ? C5 C6 P2 114.0(4) . . ? C16 C17 C18 120.9(5) . . ? C17 C16 C15 120.4(5) . . ? C9 C8 C7 120.6(5) . . ? C10 C9 C8 120.1(5) . . ? C7 C12 C11 121.2(5) . . ? C26 C25 C30 118.1(5) . . ? C26 C25 P2 123.5(4) . . ? C30 C25 P2 118.4(4) . . ? C29 C30 C25 120.3(5) . . ? C27 C26 C25 121.1(5) . . ? C20 C19 C24 117.3(5) . . ? C20 C19 P2 120.3(4) . . ? C24 C19 P2 122.4(4) . . ? C29 C28 C27 120.0(5) . . ? O1 C1 Mn1 176.3(5) . . ? C28 C27 C26 119.5(5) . . ? C23 C24 C19 121.3(6) . . ? O2 C2 Mn1 174.8(5) . . ? C21 C22 C23 119.7(6) . . ? O4 C31 C32 110.3(5) . . ? C28 C29 C30 120.9(5) . . ? C21 C20 C19 120.9(6) . . ? C22 C21 C20 120.5(6) . . ? C24 C23 C22 120.2(6) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.567 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.150 #====END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H26 Cl Mn O3 P2' _chemical_formula_weight 586.84 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' 'O' 'O' 0.0106 0.0060 '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' 'Mn' 'Mn' 0.3368 0.7283 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9382(18) _cell_length_b 20.643(3) _cell_length_c 13.666(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.871(3) _cell_angle_gamma 90.00 _cell_volume 2696.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 711 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 20.72 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12136 _diffrn_reflns_av_R_equivalents 0.1100 _diffrn_reflns_av_sigmaI/netI 0.1341 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 23.31 _reflns_number_total 3879 _reflns_number_gt 2149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3879 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1430 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.1861 _refine_ls_wR_factor_gt 0.1526 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Mn1 Mn 0.03178(11) 0.11154(6) 0.26615(8) 0.0318(4) Uani 1 1 d . . . P1 P 0.1861(2) 0.13446(10) 0.42508(15) 0.0317(5) Uani 1 1 d . . . P2 P 0.1321(2) 0.00804(9) 0.27028(14) 0.0298(5) Uani 1 1 d . . . Cl1 Cl -0.1117(2) 0.06916(10) 0.36464(15) 0.0418(6) Uani 1 1 d . . . O1 O -0.1242(6) 0.2342(3) 0.2606(4) 0.0532(16) Uani 1 1 d . . . O2 O 0.1991(6) 0.1773(3) 0.1509(4) 0.0480(15) Uani 1 1 d . . . O3 O -0.1717(6) 0.0751(3) 0.0728(4) 0.0433(14) Uani 1 1 d . . . C1 C -0.0604(8) 0.1876(4) 0.2639(5) 0.036(2) Uani 1 1 d . . . C2 C 0.1363(8) 0.1495(4) 0.1983(6) 0.039(2) Uani 1 1 d . . . C3 C -0.0942(8) 0.0887(4) 0.1493(7) 0.037(2) Uani 1 1 d . . . C4 C 0.3694(8) 0.1564(3) 0.4387(6) 0.0317(19) Uani 1 1 d . . . C5 C 0.4347(8) 0.1434(4) 0.3637(6) 0.036(2) Uani 1 1 d . . . H5 H 0.3801 0.1281 0.2995 0.043 Uiso 1 1 calc R . . C6 C 0.5768(8) 0.1521(4) 0.3790(7) 0.044(2) Uani 1 1 d . . . H6 H 0.6195 0.1430 0.3262 0.052 Uiso 1 1 calc R . . C7 C 0.6559(9) 0.1744(4) 0.4725(7) 0.045(2) Uani 1 1 d . . . H7 H 0.7538 0.1805 0.4842 0.054 Uiso 1 1 calc R . . C8 C 0.5938(8) 0.1877(3) 0.5490(6) 0.039(2) Uani 1 1 d . . . H8 H 0.6493 0.2023 0.6133 0.046 Uiso 1 1 calc R . . C9 C 0.4508(8) 0.1799(4) 0.5322(6) 0.043(2) Uani 1 1 d . . . H9 H 0.4080 0.1906 0.5842 0.051 Uiso 1 1 calc R . . C10 C 0.1255(7) 0.1992(4) 0.4929(6) 0.035(2) Uani 1 1 d . . . C11 C 0.1325(8) 0.2630(4) 0.4605(6) 0.044(2) Uani 1 1 d . . . H11 H 0.1752 0.2719 0.4077 0.053 Uiso 1 1 calc R . . C12 C 0.0780(8) 0.3132(4) 0.5044(7) 0.047(2) Uani 1 1 d . . . H12 H 0.0790 0.3562 0.4798 0.056 Uiso 1 1 calc R . . C13 C 0.0213(9) 0.3002(4) 0.5857(7) 0.051(2) Uani 1 1 d . . . H13 H -0.0133 0.3346 0.6182 0.061 Uiso 1 1 calc R . . C14 C 0.0158(9) 0.2380(5) 0.6179(6) 0.050(2) Uani 1 1 d . . . H14 H -0.0231 0.2293 0.6728 0.060 Uiso 1 1 calc R . . C15 C 0.0657(8) 0.1878(4) 0.5724(6) 0.038(2) Uani 1 1 d . . . H15 H 0.0594 0.1447 0.5952 0.046 Uiso 1 1 calc R . . C16 C 0.2143(8) 0.0672(3) 0.5154(5) 0.0332(19) Uani 1 1 d . . . H16A H 0.2716 0.0825 0.5825 0.040 Uiso 1 1 calc R . . H16B H 0.1229 0.0529 0.5235 0.040 Uiso 1 1 calc R . . C17 C 0.2878(7) 0.0091(3) 0.4818(5) 0.0316(18) Uani 1 1 d . . . H17A H 0.3679 0.0249 0.4585 0.038 Uiso 1 1 calc R . . H17B H 0.3251 -0.0197 0.5410 0.038 Uiso 1 1 calc R . . C18 C 0.1894(8) -0.0300(4) 0.3958(5) 0.0335(19) Uani 1 1 d . . . H18A H 0.1050 -0.0412 0.4174 0.040 Uiso 1 1 calc R . . H18B H 0.2368 -0.0712 0.3884 0.040 Uiso 1 1 calc R . . C19 C 0.2818(8) 0.0051(3) 0.2186(5) 0.0325(19) Uani 1 1 d . . . C20 C 0.2690(8) 0.0313(3) 0.1226(5) 0.0295(18) Uani 1 1 d . . . H20 H 0.1807 0.0465 0.0831 0.035 Uiso 1 1 calc R . . C21 C 0.3830(8) 0.0353(4) 0.0848(5) 0.0328(19) Uani 1 1 d . . . H21 H 0.3721 0.0527 0.0187 0.039 Uiso 1 1 calc R . . C22 C 0.5134(8) 0.0145(4) 0.1407(6) 0.037(2) Uani 1 1 d . . . H22 H 0.5921 0.0187 0.1145 0.044 Uiso 1 1 calc R . . C23 C 0.5273(8) -0.0119(4) 0.2342(6) 0.036(2) Uani 1 1 d . . . H23 H 0.6167 -0.0263 0.2731 0.044 Uiso 1 1 calc R . . C24 C 0.4139(8) -0.0184(4) 0.2738(6) 0.0343(19) Uani 1 1 d . . . H24 H 0.4251 -0.0385 0.3380 0.041 Uiso 1 1 calc R . . C25 C 0.0220(8) -0.0573(3) 0.2018(5) 0.0309(19) Uani 1 1 d . . . C26 C -0.1145(8) -0.0646(4) 0.2093(6) 0.037(2) Uani 1 1 d . . . H26 H -0.1504 -0.0334 0.2467 0.045 Uiso 1 1 calc R . . C27 C -0.1990(8) -0.1154(4) 0.1646(5) 0.0340(19) Uani 1 1 d . . . H27 H -0.2905 -0.1197 0.1727 0.041 Uiso 1 1 calc R . . C28 C -0.1486(8) -0.1601(4) 0.1076(6) 0.037(2) Uani 1 1 d . . . H28 H -0.2065 -0.1948 0.0749 0.045 Uiso 1 1 calc R . . C29 C -0.0140(8) -0.1541(4) 0.0985(6) 0.042(2) Uani 1 1 d . . . H29 H 0.0202 -0.1850 0.0596 0.050 Uiso 1 1 calc R . . C30 C 0.0709(8) -0.1043(4) 0.1445(6) 0.039(2) Uani 1 1 d . . . H30 H 0.1635 -0.1014 0.1380 0.047 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 Mn1 0.0291(7) 0.0322(8) 0.0327(7) 0.0009(6) 0.0059(5) 0.0009(5) P1 0.0301(12) 0.0293(12) 0.0331(11) 0.0022(9) 0.0040(10) 0.0015(9) P2 0.0283(12) 0.0321(13) 0.0284(11) 0.0006(9) 0.0068(9) 0.0006(9) Cl1 0.0404(12) 0.0457(14) 0.0411(11) -0.0016(10) 0.0139(10) 0.0009(10) O1 0.053(4) 0.039(4) 0.061(4) 0.000(3) 0.005(3) 0.018(3) O2 0.048(4) 0.047(4) 0.051(4) 0.006(3) 0.019(3) 0.004(3) O3 0.044(4) 0.042(4) 0.039(3) -0.002(3) 0.003(3) 0.003(3) C1 0.038(5) 0.037(5) 0.029(4) -0.002(4) 0.003(4) -0.002(4) C2 0.032(5) 0.036(5) 0.042(5) -0.003(4) -0.003(4) 0.000(4) C3 0.024(5) 0.035(5) 0.054(6) 0.004(4) 0.013(4) -0.004(4) C4 0.034(5) 0.020(4) 0.042(5) 0.001(4) 0.011(4) -0.001(3) C5 0.022(5) 0.037(5) 0.042(5) 0.003(4) -0.001(4) -0.002(4) C6 0.032(5) 0.036(5) 0.065(6) 0.003(5) 0.017(5) 0.000(4) C7 0.029(5) 0.032(5) 0.070(6) 0.005(5) 0.006(5) -0.002(4) C8 0.025(5) 0.028(5) 0.049(5) 0.003(4) -0.015(4) -0.003(4) C9 0.048(6) 0.026(5) 0.048(5) -0.001(4) 0.001(5) 0.003(4) C10 0.028(5) 0.032(5) 0.040(5) 0.000(4) 0.001(4) 0.002(4) C11 0.036(5) 0.046(6) 0.050(5) -0.008(5) 0.012(4) 0.001(4) C12 0.043(5) 0.030(5) 0.055(6) 0.006(4) -0.008(5) 0.003(4) C13 0.048(6) 0.043(6) 0.058(6) -0.011(5) 0.010(5) 0.016(4) C14 0.046(6) 0.059(7) 0.044(5) -0.009(5) 0.007(5) 0.009(5) C15 0.033(5) 0.034(5) 0.042(5) -0.001(4) 0.001(4) 0.007(4) C16 0.035(5) 0.036(5) 0.026(4) -0.001(4) 0.005(4) 0.003(4) C17 0.021(4) 0.035(5) 0.037(4) -0.001(4) 0.005(4) 0.007(3) C18 0.037(5) 0.034(5) 0.033(4) -0.001(4) 0.015(4) -0.002(4) C19 0.036(5) 0.027(5) 0.034(4) -0.006(4) 0.008(4) -0.006(4) C20 0.029(5) 0.028(5) 0.028(4) 0.001(4) 0.002(4) 0.000(3) C21 0.039(5) 0.034(5) 0.026(4) 0.005(4) 0.011(4) 0.000(4) C22 0.029(5) 0.047(5) 0.037(5) 0.004(4) 0.015(4) -0.003(4) C23 0.027(5) 0.038(5) 0.042(5) -0.008(4) 0.005(4) -0.002(4) C24 0.028(5) 0.043(5) 0.031(4) 0.004(4) 0.006(4) -0.002(4) C25 0.031(5) 0.034(5) 0.028(4) 0.000(4) 0.008(4) 0.000(4) C26 0.038(5) 0.037(5) 0.035(4) 0.000(4) 0.007(4) 0.005(4) C27 0.029(5) 0.034(5) 0.033(4) 0.000(4) 0.000(4) -0.006(4) C28 0.033(5) 0.031(5) 0.041(5) -0.002(4) -0.001(4) -0.001(4) C29 0.035(5) 0.045(6) 0.044(5) -0.015(4) 0.007(4) 0.002(4) C30 0.033(5) 0.048(6) 0.039(5) -0.005(4) 0.014(4) 0.001(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 Mn1 C2 1.754(9) . ? Mn1 C3 1.802(9) . ? Mn1 C1 1.814(9) . ? Mn1 P1 2.339(2) . ? Mn1 P2 2.352(2) . ? Mn1 Cl1 2.379(2) . ? P1 C10 1.820(8) . ? P1 C16 1.828(7) . ? P1 C4 1.837(8) . ? P2 C19 1.815(8) . ? P2 C25 1.826(7) . ? P2 C18 1.830(7) . ? O1 C1 1.146(8) . ? O2 C2 1.166(9) . ? O3 C3 1.150(8) . ? C4 C5 1.381(10) . ? C4 C9 1.399(10) . ? C5 C6 1.382(10) . ? C6 C7 1.383(11) . ? C7 C8 1.379(11) . ? C8 C9 1.386(10) . ? C10 C15 1.393(10) . ? C10 C11 1.397(10) . ? C11 C12 1.381(11) . ? C12 C13 1.403(11) . ? C13 C14 1.364(11) . ? C14 C15 1.369(10) . ? C16 C17 1.539(9) . ? C17 C18 1.537(9) . ? C19 C20 1.391(9) . ? C19 C24 1.410(10) . ? C20 C21 1.370(9) . ? C21 C22 1.380(10) . ? C22 C23 1.361(10) . ? C23 C24 1.383(10) . ? C25 C26 1.396(10) . ? C25 C30 1.414(10) . ? C26 C27 1.377(10) . ? C27 C28 1.387(10) . ? C28 C29 1.383(10) . ? C29 C30 1.368(10) . ? 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 C2 Mn1 C3 91.0(3) . . ? C2 Mn1 C1 88.5(4) . . ? C3 Mn1 C1 89.2(3) . . ? C2 Mn1 P1 93.9(2) . . ? C3 Mn1 P1 174.9(2) . . ? C1 Mn1 P1 92.3(2) . . ? C2 Mn1 P2 96.3(3) . . ? C3 Mn1 P2 88.3(3) . . ? C1 Mn1 P2 174.6(3) . . ? P1 Mn1 P2 89.75(8) . . ? C2 Mn1 Cl1 174.9(3) . . ? C3 Mn1 Cl1 91.5(2) . . ? C1 Mn1 Cl1 87.1(3) . . ? P1 Mn1 Cl1 83.75(8) . . ? P2 Mn1 Cl1 88.17(8) . . ? C10 P1 C16 103.0(3) . . ? C10 P1 C4 103.0(3) . . ? C16 P1 C4 98.8(3) . . ? C10 P1 Mn1 113.4(2) . . ? C16 P1 Mn1 114.5(2) . . ? C4 P1 Mn1 121.6(3) . . ? C19 P2 C25 102.5(3) . . ? C19 P2 C18 105.8(3) . . ? C25 P2 C18 98.8(3) . . ? C19 P2 Mn1 114.1(2) . . ? C25 P2 Mn1 117.9(2) . . ? C18 P2 Mn1 115.7(2) . . ? O1 C1 Mn1 176.9(7) . . ? O2 C2 Mn1 175.8(7) . . ? O3 C3 Mn1 177.5(7) . . ? C5 C4 C9 118.2(7) . . ? C5 C4 P1 122.1(6) . . ? C9 C4 P1 119.2(6) . . ? C4 C5 C6 122.0(8) . . ? C5 C6 C7 118.9(8) . . ? C8 C7 C6 120.5(8) . . ? C7 C8 C9 120.2(8) . . ? C8 C9 C4 120.2(8) . . ? C15 C10 C11 118.3(7) . . ? C15 C10 P1 123.0(6) . . ? C11 C10 P1 118.6(6) . . ? C12 C11 C10 120.8(8) . . ? C11 C12 C13 119.4(8) . . ? C14 C13 C12 119.7(8) . . ? C13 C14 C15 120.9(9) . . ? C14 C15 C10 120.8(8) . . ? C17 C16 P1 112.9(5) . . ? C18 C17 C16 112.5(6) . . ? C17 C18 P2 117.5(5) . . ? C20 C19 C24 118.0(7) . . ? C20 C19 P2 118.7(6) . . ? C24 C19 P2 123.1(6) . . ? C21 C20 C19 120.5(7) . . ? C20 C21 C22 121.3(7) . . ? C23 C22 C21 118.9(7) . . ? C22 C23 C24 121.4(7) . . ? C23 C24 C19 119.8(7) . . ? C26 C25 C30 117.1(7) . . ? C26 C25 P2 120.0(6) . . ? C30 C25 P2 122.8(6) . . ? C27 C26 C25 122.4(7) . . ? C26 C27 C28 119.1(7) . . ? C29 C28 C27 119.8(7) . . ? C30 C29 C28 121.1(7) . . ? C29 C30 C25 120.5(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.945 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.121 #====END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H26 Br Mn O3 P2' _chemical_formula_weight 631.30 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' 'O' 'O' 0.0106 0.0060 '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' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.073(4) _cell_length_b 20.612(8) _cell_length_c 13.765(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.551(7) _cell_angle_gamma 90.00 _cell_volume 2739.4(19) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 850 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 23.26 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 2.088 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12140 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 23.31 _reflns_number_total 3954 _reflns_number_gt 3233 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0978P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3954 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1545 _refine_ls_wR_factor_gt 0.1359 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.159 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.002 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 Mn1 Mn 0.46166(7) 0.11297(4) 0.23633(6) 0.0225(3) Uani 1 1 d . . . Br1 Br 0.61874(5) 0.07219(2) 0.13635(4) 0.0272(2) Uani 1 1 d . . . P1 P 0.31009(13) 0.13484(6) 0.07551(10) 0.0227(3) Uani 1 1 d . . . P2 P 0.36453(13) 0.00863(6) 0.23193(10) 0.0217(3) Uani 1 1 d . . . O1 O 0.6681(4) 0.07623(18) 0.4279(3) 0.0367(10) Uani 1 1 d . . . O2 O 0.2939(4) 0.17764(17) 0.3501(3) 0.0329(9) Uani 1 1 d . . . O3 O 0.6107(4) 0.23784(19) 0.2441(3) 0.0411(10) Uani 1 1 d . . . C1 C 0.5892(6) 0.0896(3) 0.3534(4) 0.0270(12) Uani 1 1 d . . . C2 C 0.3556(5) 0.1502(2) 0.3044(4) 0.0268(12) Uani 1 1 d . . . C3 C 0.5512(5) 0.1900(3) 0.2384(4) 0.0277(12) Uani 1 1 d . . . C4 C 0.3058(5) -0.0297(2) 0.1071(4) 0.0248(12) Uani 1 1 d . . . H4A H 0.3870 -0.0412 0.0863 0.030 Uiso 1 1 calc R . . H4B H 0.2592 -0.0698 0.1144 0.030 Uiso 1 1 calc R . . C5 C 0.2088(5) 0.0095(2) 0.0215(4) 0.0272(12) Uani 1 1 d . . . H5A H 0.1327 0.0259 0.0445 0.033 Uiso 1 1 calc R . . H5B H 0.1703 -0.0190 -0.0356 0.033 Uiso 1 1 calc R . . C6 C 0.2805(6) 0.0668(2) -0.0141(4) 0.0271(12) Uani 1 1 d . . . H6A H 0.2236 0.0814 -0.0798 0.033 Uiso 1 1 calc R . . H6B H 0.3686 0.0525 -0.0219 0.033 Uiso 1 1 calc R . . C7 C 0.1289(5) 0.1574(2) 0.0587(4) 0.0244(12) Uani 1 1 d . . . C8 C 0.0643(5) 0.1449(2) 0.1336(4) 0.0289(12) Uani 1 1 d . . . H8 H 0.1161 0.1299 0.1967 0.035 Uiso 1 1 calc R . . C9 C -0.0762(5) 0.1547(3) 0.1150(5) 0.0341(14) Uani 1 1 d . . . H9 H -0.1183 0.1474 0.1660 0.041 Uiso 1 1 calc R . . C10 C -0.1548(6) 0.1756(3) 0.0201(5) 0.0377(15) Uani 1 1 d . . . H10 H -0.2499 0.1811 0.0069 0.045 Uiso 1 1 calc R . . C11 C -0.0921(5) 0.1879(2) -0.0538(5) 0.0338(14) Uani 1 1 d . . . H11 H -0.1449 0.2020 -0.1173 0.041 Uiso 1 1 calc R . . C12 C 0.0494(5) 0.1797(2) -0.0352(4) 0.0317(13) Uani 1 1 d . . . H12 H 0.0914 0.1891 -0.0856 0.038 Uiso 1 1 calc R . . C13 C 0.3696(5) 0.1992(2) 0.0074(4) 0.0266(12) Uani 1 1 d . . . C14 C 0.4280(5) 0.1864(3) -0.0711(4) 0.0318(13) Uani 1 1 d . . . H14 H 0.4332 0.1439 -0.0922 0.038 Uiso 1 1 calc R . . C15 C 0.4786(6) 0.2364(3) -0.1182(4) 0.0381(15) Uani 1 1 d . . . H15 H 0.5160 0.2272 -0.1710 0.046 Uiso 1 1 calc R . . C16 C 0.4734(6) 0.2992(3) -0.0868(5) 0.0417(15) Uani 1 1 d . . . H16 H 0.5074 0.3326 -0.1184 0.050 Uiso 1 1 calc R . . C17 C 0.4169(6) 0.3129(3) -0.0074(5) 0.0371(15) Uani 1 1 d . . . H17 H 0.4144 0.3555 0.0144 0.045 Uiso 1 1 calc R . . C18 C 0.3648(6) 0.2636(3) 0.0388(4) 0.0337(13) Uani 1 1 d . . . H18 H 0.3263 0.2731 0.0910 0.040 Uiso 1 1 calc R . . C19 C 0.4751(5) -0.0568(2) 0.3016(4) 0.0243(12) Uani 1 1 d . . . C20 C 0.6086(6) -0.0645(3) 0.2941(4) 0.0312(13) Uani 1 1 d . . . H20 H 0.6437 -0.0345 0.2574 0.037 Uiso 1 1 calc R . . C21 C 0.6901(6) -0.1157(3) 0.3399(4) 0.0320(13) Uani 1 1 d . . . H21 H 0.7789 -0.1203 0.3330 0.038 Uiso 1 1 calc R . . C22 C 0.6413(6) -0.1603(3) 0.3958(4) 0.0367(14) Uani 1 1 d . . . H22 H 0.6968 -0.1948 0.4270 0.044 Uiso 1 1 calc R . . C23 C 0.5095(6) -0.1534(3) 0.4051(5) 0.0383(14) Uani 1 1 d . . . H23 H 0.4764 -0.1830 0.4436 0.046 Uiso 1 1 calc R . . C24 C 0.4265(6) -0.1030(3) 0.3579(4) 0.0344(14) Uani 1 1 d . . . H24 H 0.3369 -0.0996 0.3633 0.041 Uiso 1 1 calc R . . C25 C 0.2164(5) 0.0057(2) 0.2826(4) 0.0221(11) Uani 1 1 d . . . C26 C 0.2290(5) 0.0318(2) 0.3791(4) 0.0247(12) Uani 1 1 d . . . H26 H 0.3146 0.0470 0.4182 0.030 Uiso 1 1 calc R . . C27 C 0.1165(5) 0.0352(3) 0.4166(4) 0.0289(12) Uani 1 1 d . . . H27 H 0.1275 0.0516 0.4813 0.035 Uiso 1 1 calc R . . C28 C -0.0116(6) 0.0148(3) 0.3599(4) 0.0323(13) Uani 1 1 d . . . H28 H -0.0883 0.0196 0.3841 0.039 Uiso 1 1 calc R . . C29 C -0.0251(5) -0.0129(3) 0.2663(4) 0.0324(13) Uani 1 1 d . . . H29 H -0.1111 -0.0285 0.2288 0.039 Uiso 1 1 calc R . . C30 C 0.0860(5) -0.0180(3) 0.2272(4) 0.0287(12) Uani 1 1 d . . . H30 H 0.0748 -0.0372 0.1642 0.034 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 Mn1 0.0204(4) 0.0237(5) 0.0229(5) -0.0006(3) 0.0055(4) -0.0010(3) Br1 0.0238(3) 0.0304(4) 0.0296(4) 0.0007(2) 0.0111(2) 0.0009(2) P1 0.0215(7) 0.0221(7) 0.0243(7) -0.0004(6) 0.0063(6) -0.0003(5) P2 0.0202(7) 0.0234(7) 0.0220(7) -0.0012(5) 0.0067(6) 0.0001(5) O1 0.031(2) 0.043(3) 0.030(2) -0.0023(18) 0.000(2) -0.0030(18) O2 0.034(2) 0.031(2) 0.037(2) -0.0074(18) 0.0148(19) 0.0017(17) O3 0.039(2) 0.035(2) 0.043(3) 0.0021(19) 0.002(2) -0.008(2) C1 0.026(3) 0.028(3) 0.030(3) -0.004(2) 0.013(3) -0.002(2) C2 0.025(3) 0.023(3) 0.027(3) 0.002(2) -0.002(2) -0.005(2) C3 0.026(3) 0.035(3) 0.022(3) -0.003(2) 0.006(2) -0.003(3) C4 0.029(3) 0.022(3) 0.024(3) 0.003(2) 0.009(2) 0.000(2) C5 0.028(3) 0.026(3) 0.027(3) -0.002(2) 0.005(2) -0.005(2) C6 0.027(3) 0.026(3) 0.028(3) 0.003(2) 0.007(2) 0.005(2) C7 0.021(3) 0.018(3) 0.035(3) -0.004(2) 0.009(2) -0.001(2) C8 0.029(3) 0.023(3) 0.031(3) -0.002(2) 0.003(2) 0.000(2) C9 0.027(3) 0.027(3) 0.051(4) -0.007(3) 0.014(3) -0.004(2) C10 0.019(3) 0.029(3) 0.060(4) -0.007(3) 0.002(3) 0.000(2) C11 0.024(3) 0.022(3) 0.047(4) 0.003(3) -0.004(3) 0.004(2) C12 0.031(3) 0.024(3) 0.036(3) 0.001(2) 0.003(3) -0.004(2) C13 0.026(3) 0.025(3) 0.028(3) 0.001(2) 0.006(2) -0.004(2) C14 0.029(3) 0.035(3) 0.033(3) 0.005(3) 0.010(3) 0.000(2) C15 0.034(3) 0.050(4) 0.032(3) 0.010(3) 0.011(3) -0.004(3) C16 0.035(3) 0.037(4) 0.052(4) 0.015(3) 0.009(3) -0.008(3) C17 0.031(3) 0.026(3) 0.049(4) 0.005(3) 0.003(3) -0.003(2) C18 0.031(3) 0.031(3) 0.039(3) 0.005(3) 0.011(3) 0.004(2) C19 0.023(3) 0.026(3) 0.022(3) -0.004(2) 0.004(2) 0.001(2) C20 0.035(3) 0.027(3) 0.033(3) 0.005(2) 0.012(3) 0.001(2) C21 0.025(3) 0.036(3) 0.033(3) 0.000(3) 0.005(3) 0.004(2) C22 0.038(3) 0.029(3) 0.037(3) 0.004(3) -0.001(3) 0.008(3) C23 0.040(3) 0.033(3) 0.044(4) 0.008(3) 0.015(3) -0.002(3) C24 0.030(3) 0.035(3) 0.039(3) 0.006(3) 0.010(3) 0.000(3) C25 0.024(3) 0.018(3) 0.024(3) 0.004(2) 0.007(2) 0.000(2) C26 0.021(3) 0.024(3) 0.027(3) 0.001(2) 0.004(2) -0.001(2) C27 0.036(3) 0.031(3) 0.018(3) -0.004(2) 0.007(2) -0.002(2) C28 0.027(3) 0.036(3) 0.039(3) 0.001(3) 0.017(3) 0.001(2) C29 0.021(3) 0.041(3) 0.034(3) 0.006(3) 0.006(2) -0.002(2) C30 0.027(3) 0.037(3) 0.023(3) 0.001(2) 0.008(2) -0.003(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 Mn1 C2 1.783(6) . ? Mn1 C1 1.816(6) . ? Mn1 C3 1.821(6) . ? Mn1 P1 2.3471(17) . ? Mn1 P2 2.3563(17) . ? Mn1 Br1 2.5189(11) . ? P1 C13 1.822(5) . ? P1 C7 1.833(5) . ? P1 C6 1.835(5) . ? P2 C25 1.819(5) . ? P2 C4 1.829(5) . ? P2 C19 1.836(5) . ? O1 C1 1.138(6) . ? O2 C2 1.151(6) . ? O3 C3 1.146(6) . ? C4 C5 1.530(7) . ? C5 C6 1.536(7) . ? C7 C12 1.391(7) . ? C7 C8 1.391(7) . ? C8 C9 1.379(7) . ? C9 C10 1.389(8) . ? C10 C11 1.366(8) . ? C11 C12 1.385(7) . ? C13 C14 1.394(8) . ? C13 C18 1.400(7) . ? C14 C15 1.388(8) . ? C15 C16 1.370(8) . ? C16 C17 1.398(8) . ? C17 C18 1.380(8) . ? C19 C20 1.388(8) . ? C19 C24 1.400(8) . ? C20 C21 1.375(7) . ? C21 C22 1.377(8) . ? C22 C23 1.377(8) . ? C23 C24 1.375(8) . ? C25 C30 1.405(7) . ? C25 C26 1.406(7) . ? C26 C27 1.374(7) . ? C27 C28 1.370(7) . ? C28 C29 1.381(8) . ? C29 C30 1.377(7) . ? 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 C2 Mn1 C1 91.5(2) . . ? C2 Mn1 C3 89.2(2) . . ? C1 Mn1 C3 89.7(2) . . ? C2 Mn1 P1 94.99(17) . . ? C1 Mn1 P1 173.33(17) . . ? C3 Mn1 P1 91.91(16) . . ? C2 Mn1 P2 95.71(17) . . ? C1 Mn1 P2 87.97(17) . . ? C3 Mn1 P2 174.66(17) . . ? P1 Mn1 P2 89.84(5) . . ? C2 Mn1 Br1 174.02(17) . . ? C1 Mn1 Br1 90.02(17) . . ? C3 Mn1 Br1 85.06(17) . . ? P1 Mn1 Br1 83.68(5) . . ? P2 Mn1 Br1 90.13(5) . . ? C13 P1 C7 102.3(2) . . ? C13 P1 C6 103.0(2) . . ? C7 P1 C6 98.3(2) . . ? C13 P1 Mn1 113.85(17) . . ? C7 P1 Mn1 121.62(18) . . ? C6 P1 Mn1 115.13(17) . . ? C25 P2 C4 105.3(2) . . ? C25 P2 C19 102.5(2) . . ? C4 P2 C19 99.1(2) . . ? C25 P2 Mn1 113.63(16) . . ? C4 P2 Mn1 116.06(17) . . ? C19 P2 Mn1 118.14(17) . . ? O1 C1 Mn1 178.3(5) . . ? O2 C2 Mn1 175.2(4) . . ? O3 C3 Mn1 176.9(5) . . ? C5 C4 P2 117.4(4) . . ? C4 C5 C6 113.4(4) . . ? C5 C6 P1 112.0(4) . . ? C12 C7 C8 118.9(5) . . ? C12 C7 P1 119.3(4) . . ? C8 C7 P1 121.3(4) . . ? C9 C8 C7 120.4(5) . . ? C8 C9 C10 120.0(6) . . ? C11 C10 C9 119.9(5) . . ? C10 C11 C12 120.6(5) . . ? C11 C12 C7 120.2(5) . . ? C14 C13 C18 118.5(5) . . ? C14 C13 P1 122.3(4) . . ? C18 C13 P1 119.0(4) . . ? C15 C14 C13 120.9(5) . . ? C16 C15 C14 120.1(6) . . ? C15 C16 C17 119.9(5) . . ? C18 C17 C16 120.2(6) . . ? C17 C18 C13 120.4(5) . . ? C20 C19 C24 117.6(5) . . ? C20 C19 P2 120.1(4) . . ? C24 C19 P2 122.2(4) . . ? C21 C20 C19 121.2(5) . . ? C20 C21 C22 120.5(5) . . ? C21 C22 C23 119.4(5) . . ? C24 C23 C22 120.4(5) . . ? C23 C24 C19 120.9(5) . . ? C30 C25 C26 117.7(5) . . ? C30 C25 P2 123.1(4) . . ? C26 C25 P2 119.1(4) . . ? C27 C26 C25 120.8(5) . . ? C28 C27 C26 121.0(5) . . ? C27 C28 C29 119.0(5) . . ? C30 C29 C28 121.4(5) . . ? C29 C30 C25 120.0(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.975 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.191 #====END data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H32 Mn N3 O3 P2' _chemical_formula_weight 671.53 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.826(3) _cell_length_b 17.209(4) _cell_length_c 15.102(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.727(4) _cell_angle_gamma 90.00 _cell_volume 3208.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 817 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 22.93 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.552 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14172 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 23.31 _reflns_number_total 4611 _reflns_number_gt 3401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0935P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4611 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1557 _refine_ls_wR_factor_gt 0.1407 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Mn1 Mn 0.17532(5) 0.03145(3) 0.94395(4) 0.0241(2) Uani 1 1 d . . . P1 P 0.29832(9) 0.13401(6) 0.98999(8) 0.0245(3) Uani 1 1 d . . . P2 P 0.18771(9) 0.04432(6) 0.79291(8) 0.0238(3) Uani 1 1 d . . . O1 O 0.0146(2) -0.09330(17) 0.8731(2) 0.0342(7) Uani 1 1 d . . . O2 O 0.1830(2) -0.01019(17) 1.1368(2) 0.0352(8) Uani 1 1 d . . . O3 O -0.0116(2) 0.13396(16) 0.9351(2) 0.0304(7) Uani 1 1 d . . . N1 N 0.3176(3) -0.0373(2) 0.9637(2) 0.0252(8) Uani 1 1 d . . . N2 N 0.3214(3) -0.0947(3) 1.0052(3) 0.0362(10) Uani 1 1 d . . . N3 N 0.3317(4) -0.1552(2) 1.0462(3) 0.0552(13) Uani 1 1 d . . . C1 C 0.0801(4) -0.0470(2) 0.9020(3) 0.0260(10) Uani 1 1 d . . . C2 C 0.1806(3) 0.0085(2) 1.0636(3) 0.0281(10) Uani 1 1 d . . . C3 C 0.0620(4) 0.0953(2) 0.9359(3) 0.0276(10) Uani 1 1 d . . . C4 C 0.4113(3) 0.1331(2) 0.9375(3) 0.0281(10) Uani 1 1 d . . . H4A H 0.4628 0.1749 0.9652 0.034 Uiso 1 1 calc R . . H4B H 0.4501 0.0829 0.9515 0.034 Uiso 1 1 calc R . . C5 C 0.3747(4) 0.1443(2) 0.8326(3) 0.0303(10) Uani 1 1 d . . . H5A H 0.3235 0.1885 0.8183 0.036 Uiso 1 1 calc R . . H5B H 0.4387 0.1582 0.8110 0.036 Uiso 1 1 calc R . . C6 C 0.3206(3) 0.0734(2) 0.7795(3) 0.0258(10) Uani 1 1 d . . . H6A H 0.3706 0.0288 0.7977 0.031 Uiso 1 1 calc R . . H6B H 0.3123 0.0831 0.7133 0.031 Uiso 1 1 calc R . . C7 C 0.3641(3) 0.1334(2) 1.1137(3) 0.0228(9) Uani 1 1 d . . . C8 C 0.3020(4) 0.1532(2) 1.1719(3) 0.0306(11) Uani 1 1 d . . . H8 H 0.2277 0.1661 1.1471 0.037 Uiso 1 1 calc R . . C9 C 0.3474(4) 0.1546(2) 1.2673(3) 0.0302(10) Uani 1 1 d . . . H9 H 0.3042 0.1679 1.3072 0.036 Uiso 1 1 calc R . . C10 C 0.4551(4) 0.1366(2) 1.3027(3) 0.0332(11) Uani 1 1 d . . . H10 H 0.4864 0.1386 1.3674 0.040 Uiso 1 1 calc R . . C11 C 0.5184(4) 0.1158(2) 1.2456(3) 0.0333(11) Uani 1 1 d . . . H11 H 0.5927 0.1035 1.2708 0.040 Uiso 1 1 calc R . . C12 C 0.4722(3) 0.1131(2) 1.1509(3) 0.0282(10) Uani 1 1 d . . . H12 H 0.5147 0.0972 1.1115 0.034 Uiso 1 1 calc R . . C13 C 0.2541(3) 0.2359(2) 0.9715(3) 0.0250(10) Uani 1 1 d . . . C14 C 0.3191(3) 0.2952(2) 1.0226(3) 0.0304(10) Uani 1 1 d . . . H14 H 0.3833 0.2819 1.0686 0.036 Uiso 1 1 calc R . . C15 C 0.2905(4) 0.3723(2) 1.0068(3) 0.0345(11) Uani 1 1 d . . . H15 H 0.3356 0.4115 1.0417 0.041 Uiso 1 1 calc R . . C16 C 0.1972(4) 0.3931(2) 0.9407(3) 0.0337(11) Uani 1 1 d . . . H16 H 0.1777 0.4463 0.9306 0.040 Uiso 1 1 calc R . . C17 C 0.1326(4) 0.3357(2) 0.8894(3) 0.0303(11) Uani 1 1 d . . . H17 H 0.0683 0.3496 0.8438 0.036 Uiso 1 1 calc R . . C18 C 0.1614(3) 0.2576(2) 0.9042(3) 0.0286(10) Uani 1 1 d . . . H18 H 0.1170 0.2188 0.8679 0.034 Uiso 1 1 calc R . . C19 C 0.0885(3) 0.1116(2) 0.7236(3) 0.0256(10) Uani 1 1 d . . . C20 C -0.0205(3) 0.1004(2) 0.7232(3) 0.0262(10) Uani 1 1 d . . . H20 H -0.0399 0.0573 0.7547 0.031 Uiso 1 1 calc R . . C21 C -0.0986(3) 0.1516(2) 0.6775(3) 0.0296(10) Uani 1 1 d . . . H21 H -0.1717 0.1440 0.6784 0.036 Uiso 1 1 calc R . . C22 C -0.0725(4) 0.2144(2) 0.6300(3) 0.0339(11) Uani 1 1 d . . . H22 H -0.1268 0.2503 0.5999 0.041 Uiso 1 1 calc R . . C23 C 0.0338(4) 0.2242(2) 0.6270(3) 0.0282(10) Uani 1 1 d . . . H23 H 0.0516 0.2661 0.5928 0.034 Uiso 1 1 calc R . . C24 C 0.1145(3) 0.1735(2) 0.6733(3) 0.0276(10) Uani 1 1 d . . . H24 H 0.1871 0.1808 0.6708 0.033 Uiso 1 1 calc R . . C25 C 0.1666(3) -0.0425(2) 0.7200(3) 0.0261(10) Uani 1 1 d . . . C26 C 0.1920(3) -0.1165(2) 0.7567(3) 0.0281(10) Uani 1 1 d . . . H26 H 0.2152 -0.1229 0.8215 0.034 Uiso 1 1 calc R . . C27 C 0.1843(3) -0.1811(2) 0.7004(3) 0.0287(10) Uani 1 1 d . . . H27 H 0.2026 -0.2312 0.7266 0.034 Uiso 1 1 calc R . . C28 C 0.1498(4) -0.1723(3) 0.6064(3) 0.0364(12) Uani 1 1 d . . . H28 H 0.1435 -0.2166 0.5677 0.044 Uiso 1 1 calc R . . C29 C 0.1245(4) -0.1001(3) 0.5680(3) 0.0396(12) Uani 1 1 d . . . H29 H 0.1022 -0.0943 0.5030 0.048 Uiso 1 1 calc R . . C30 C 0.1317(4) -0.0356(2) 0.6244(3) 0.0328(11) Uani 1 1 d . . . H30 H 0.1126 0.0141 0.5975 0.039 Uiso 1 1 calc R . . C1S C 0.6127(4) 0.0500(3) 0.6135(4) 0.0444(13) Uani 1 1 d . . . H1S H 0.6106 -0.0052 0.6120 0.053 Uiso 1 1 calc R . . C2S C 0.6000(4) 0.0895(3) 0.6901(4) 0.0485(14) Uani 1 1 d . . . H2S H 0.5890 0.0616 0.7411 0.058 Uiso 1 1 calc R . . C3S C 0.6036(4) 0.1699(3) 0.6914(4) 0.0451(13) Uani 1 1 d . . . H3S H 0.5958 0.1972 0.7439 0.054 Uiso 1 1 calc R . . C4S C 0.6183(3) 0.2102(3) 0.6173(3) 0.0381(12) Uani 1 1 d . . . H4S H 0.6195 0.2654 0.6182 0.046 Uiso 1 1 calc R . . C5S C 0.6316(3) 0.1705(3) 0.5409(3) 0.0371(12) Uani 1 1 d . . . H5S H 0.6428 0.1982 0.4899 0.045 Uiso 1 1 calc R . . C6S C 0.6283(4) 0.0906(3) 0.5399(3) 0.0405(12) Uani 1 1 d . . . H6S H 0.6369 0.0633 0.4877 0.049 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 Mn1 0.0244(4) 0.0244(4) 0.0240(4) -0.0002(3) 0.0076(3) -0.0003(3) P1 0.0245(6) 0.0253(6) 0.0244(6) -0.0007(5) 0.0077(5) 0.0001(5) P2 0.0252(6) 0.0234(6) 0.0239(6) 0.0001(5) 0.0084(5) 0.0010(4) O1 0.0358(18) 0.0318(17) 0.0377(19) -0.0044(15) 0.0144(15) -0.0066(15) O2 0.0368(19) 0.0394(19) 0.031(2) 0.0027(16) 0.0119(15) -0.0045(14) O3 0.0291(18) 0.0294(17) 0.0348(18) -0.0033(14) 0.0123(14) 0.0012(14) N1 0.029(2) 0.0221(19) 0.026(2) 0.0040(17) 0.0094(16) -0.0006(15) N2 0.023(2) 0.046(3) 0.042(3) -0.010(2) 0.0129(19) -0.0028(18) N3 0.059(3) 0.035(2) 0.082(4) 0.024(3) 0.036(3) 0.013(2) C1 0.032(3) 0.027(2) 0.020(2) 0.0018(19) 0.008(2) 0.006(2) C2 0.024(2) 0.029(2) 0.031(3) 0.003(2) 0.005(2) 0.0003(18) C3 0.030(3) 0.030(2) 0.024(2) -0.009(2) 0.009(2) -0.007(2) C4 0.034(3) 0.025(2) 0.026(2) -0.0015(19) 0.009(2) -0.0028(19) C5 0.037(3) 0.028(2) 0.027(3) 0.002(2) 0.011(2) -0.0034(19) C6 0.025(2) 0.031(2) 0.023(2) 0.0039(19) 0.0096(19) 0.0057(18) C7 0.029(2) 0.018(2) 0.021(2) -0.0004(18) 0.006(2) -0.0018(17) C8 0.029(2) 0.027(2) 0.034(3) 0.001(2) 0.008(2) 0.0039(19) C9 0.038(3) 0.029(2) 0.025(3) -0.004(2) 0.012(2) -0.002(2) C10 0.044(3) 0.031(3) 0.021(2) -0.001(2) 0.003(2) -0.004(2) C11 0.028(3) 0.033(3) 0.035(3) 0.000(2) 0.002(2) 0.0006(19) C12 0.028(3) 0.026(2) 0.032(3) 0.001(2) 0.011(2) -0.0026(18) C13 0.029(2) 0.023(2) 0.026(2) -0.0021(19) 0.014(2) -0.0035(18) C14 0.029(3) 0.031(3) 0.033(3) -0.002(2) 0.011(2) -0.0013(19) C15 0.041(3) 0.029(3) 0.036(3) -0.006(2) 0.015(2) -0.009(2) C16 0.046(3) 0.023(2) 0.037(3) 0.004(2) 0.019(2) 0.004(2) C17 0.033(3) 0.028(2) 0.033(3) 0.005(2) 0.013(2) 0.006(2) C18 0.027(2) 0.026(2) 0.035(3) -0.007(2) 0.011(2) -0.0051(18) C19 0.028(2) 0.024(2) 0.023(2) -0.0042(19) 0.0039(19) 0.0007(18) C20 0.031(3) 0.022(2) 0.026(2) -0.0003(19) 0.008(2) -0.0029(18) C21 0.026(2) 0.037(3) 0.027(2) -0.002(2) 0.008(2) 0.0018(19) C22 0.038(3) 0.031(3) 0.029(3) -0.003(2) 0.004(2) 0.007(2) C23 0.042(3) 0.021(2) 0.021(2) 0.0015(19) 0.008(2) 0.0015(19) C24 0.028(2) 0.027(2) 0.029(2) 0.000(2) 0.010(2) -0.0018(19) C25 0.029(2) 0.025(2) 0.025(3) -0.0006(19) 0.009(2) 0.0015(18) C26 0.026(2) 0.027(2) 0.032(3) 0.005(2) 0.009(2) 0.0032(18) C27 0.029(2) 0.023(2) 0.033(3) 0.002(2) 0.007(2) 0.0023(18) C28 0.047(3) 0.030(3) 0.035(3) -0.013(2) 0.015(2) -0.002(2) C29 0.062(3) 0.034(3) 0.025(3) -0.001(2) 0.016(2) 0.002(2) C30 0.047(3) 0.025(2) 0.026(3) 0.004(2) 0.009(2) 0.002(2) C1S 0.046(3) 0.037(3) 0.046(3) 0.002(3) 0.006(3) 0.000(2) C2S 0.041(3) 0.056(4) 0.048(3) 0.009(3) 0.013(3) -0.003(2) C3S 0.026(3) 0.058(4) 0.051(3) -0.004(3) 0.010(2) -0.002(2) C4S 0.026(3) 0.035(3) 0.048(3) -0.005(2) 0.000(2) 0.005(2) C5S 0.030(3) 0.034(3) 0.039(3) 0.005(2) -0.005(2) 0.000(2) C6S 0.040(3) 0.043(3) 0.033(3) -0.003(2) -0.001(2) 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 Mn1 C3 1.799(5) . ? Mn1 C1 1.816(5) . ? Mn1 C2 1.832(5) . ? Mn1 N1 2.126(3) . ? Mn1 P2 2.3396(14) . ? Mn1 P1 2.3437(13) . ? P1 C7 1.830(4) . ? P1 C4 1.831(4) . ? P1 C13 1.841(4) . ? P2 C19 1.826(4) . ? P2 C25 1.832(4) . ? P2 C6 1.841(4) . ? O1 C1 1.154(5) . ? O2 C2 1.144(5) . ? O3 C3 1.153(5) . ? N1 N2 1.164(5) . ? N2 N3 1.200(6) . ? C4 C5 1.538(6) . ? C5 C6 1.520(6) . ? C7 C8 1.380(6) . ? C7 C12 1.392(6) . ? C8 C9 1.400(6) . ? C9 C10 1.374(6) . ? C10 C11 1.383(6) . ? C11 C12 1.392(6) . ? C13 C18 1.390(6) . ? C13 C14 1.408(6) . ? C14 C15 1.380(6) . ? C15 C16 1.382(6) . ? C16 C17 1.384(6) . ? C17 C18 1.397(6) . ? C19 C24 1.400(6) . ? C19 C20 1.409(6) . ? C20 C21 1.372(6) . ? C21 C22 1.387(6) . ? C22 C23 1.386(6) . ? C23 C24 1.389(6) . ? C25 C26 1.391(6) . ? C25 C30 1.396(6) . ? C26 C27 1.387(6) . ? C27 C28 1.377(6) . ? C28 C29 1.372(6) . ? C29 C30 1.387(6) . ? C1S C6S 1.372(7) . ? C1S C2S 1.389(7) . ? C2S C3S 1.384(7) . ? C3S C4S 1.374(7) . ? C4S C5S 1.390(6) . ? C5S C6S 1.375(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 C3 Mn1 C1 88.62(18) . . ? C3 Mn1 C2 90.69(19) . . ? C1 Mn1 C2 91.45(19) . . ? C3 Mn1 N1 174.65(16) . . ? C1 Mn1 N1 96.06(16) . . ? C2 Mn1 N1 86.61(16) . . ? C3 Mn1 P2 98.22(14) . . ? C1 Mn1 P2 86.99(13) . . ? C2 Mn1 P2 170.90(14) . . ? N1 Mn1 P2 84.65(10) . . ? C3 Mn1 P1 91.53(13) . . ? C1 Mn1 P1 176.96(14) . . ? C2 Mn1 P1 91.58(14) . . ? N1 Mn1 P1 83.94(10) . . ? P2 Mn1 P1 89.99(4) . . ? C7 P1 C4 104.01(19) . . ? C7 P1 C13 101.39(18) . . ? C4 P1 C13 100.99(18) . . ? C7 P1 Mn1 112.71(13) . . ? C4 P1 Mn1 114.39(14) . . ? C13 P1 Mn1 121.16(14) . . ? C19 P2 C25 101.88(19) . . ? C19 P2 C6 106.66(19) . . ? C25 P2 C6 98.42(19) . . ? C19 P2 Mn1 113.46(14) . . ? C25 P2 Mn1 118.06(14) . . ? C6 P2 Mn1 116.31(14) . . ? N2 N1 Mn1 117.2(3) . . ? N1 N2 N3 175.4(4) . . ? O1 C1 Mn1 175.6(4) . . ? O2 C2 Mn1 176.1(4) . . ? O3 C3 Mn1 176.0(4) . . ? C5 C4 P1 112.9(3) . . ? C6 C5 C4 114.2(3) . . ? C5 C6 P2 117.7(3) . . ? C8 C7 C12 119.2(4) . . ? C8 C7 P1 117.6(3) . . ? C12 C7 P1 123.2(3) . . ? C7 C8 C9 120.6(4) . . ? C10 C9 C8 119.4(4) . . ? C9 C10 C11 120.9(4) . . ? C10 C11 C12 119.4(4) . . ? C7 C12 C11 120.4(4) . . ? C18 C13 C14 117.9(4) . . ? C18 C13 P1 122.3(3) . . ? C14 C13 P1 119.7(3) . . ? C15 C14 C13 120.8(4) . . ? C14 C15 C16 120.8(4) . . ? C15 C16 C17 119.4(4) . . ? C16 C17 C18 120.3(4) . . ? C13 C18 C17 120.9(4) . . ? C24 C19 C20 118.9(4) . . ? C24 C19 P2 124.2(3) . . ? C20 C19 P2 116.9(3) . . ? C21 C20 C19 120.2(4) . . ? C20 C21 C22 121.0(4) . . ? C23 C22 C21 119.3(4) . . ? C22 C23 C24 120.9(4) . . ? C23 C24 C19 119.7(4) . . ? C26 C25 C30 117.7(4) . . ? C26 C25 P2 121.8(3) . . ? C30 C25 P2 120.4(3) . . ? C27 C26 C25 121.3(4) . . ? C28 C27 C26 119.5(4) . . ? C29 C28 C27 120.6(4) . . ? C28 C29 C30 119.8(4) . . ? C29 C30 C25 121.1(4) . . ? C6S C1S C2S 120.0(5) . . ? C3S C2S C1S 119.4(5) . . ? C4S C3S C2S 120.3(5) . . ? C3S C4S C5S 120.2(5) . . ? C6S C5S C4S 119.4(5) . . ? C1S C6S C5S 120.7(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.601 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.111