# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1917 #Neil G. Connelly, A.G. Orpen et al #Coordination chemistry of a bulky redox-active cyanomanganese carbonyl ligand: # N-bound tetrahedral complexes of 3d metals data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C56 H52 Cl2 Co Mn N O2 P4' _chemical_formula_weight 1079.72 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Co' 'Co' 0.3494 0.9721 '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 10.192(2) _cell_length_b 13.922(2) _cell_length_c 19.286(4) _cell_angle_alpha 91.22(2) _cell_angle_beta 97.58(2) _cell_angle_gamma 105.838(14) _cell_volume 2604.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 115 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 25.02 _exptl_crystal_description cubes _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method ? _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.827 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.618 _exptl_absorpt_correction_T_max 0.814 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16491 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.51 _reflns_number_total 11361 _reflns_number_observed 8416 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 10 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+5.6491P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11351 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_obs 0.0582 _refine_ls_wR_factor_all 0.1289 _refine_ls_wR_factor_obs 0.1033 _refine_ls_goodness_of_fit_all 1.226 _refine_ls_goodness_of_fit_obs 1.156 _refine_ls_restrained_S_all 1.231 _refine_ls_restrained_S_obs 1.156 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.21685(6) 0.55156(4) 0.37197(3) 0.02988(14) Uani 1 d . . Cl1 Cl 0.22550(14) 0.39555(8) 0.35121(7) 0.0500(3) Uani 1 d . . Cl2 Cl 0.00319(12) 0.57087(10) 0.35151(6) 0.0447(3) Uani 1 d . . Mn1 Mn 0.44809(6) 0.81612(4) 0.22193(3) 0.01921(12) Uani 1 d . . P1 P 0.59503(10) 0.74678(7) 0.17394(5) 0.0223(2) Uani 1 d . . P2 P 0.66015(10) 0.88327(7) 0.28509(5) 0.0220(2) Uani 1 d . . P3 P 0.23949(10) 0.74351(7) 0.15596(5) 0.0229(2) Uani 1 d . . P4 P 0.28942(10) 0.87116(7) 0.27185(5) 0.0213(2) Uani 1 d . . O1 O 0.5026(3) 0.9910(2) 0.13459(15) 0.0334(7) Uani 1 d . . O2 O 0.2836(3) 0.5933(3) 0.4734(2) 0.0470(9) Uani 1 d . . N1 N 0.3484(3) 0.6489(2) 0.3239(2) 0.0281(7) Uani 1 d . . C1 C 0.7538(4) 0.8336(3) 0.2228(2) 0.0275(9) Uani 1 d . . H1A H 0.8022(4) 0.8854(3) 0.1935(2) 0.033 Uiso 1 calc R . H1B H 0.8182(4) 0.7984(3) 0.2462(2) 0.033 Uiso 1 calc R . C2 C 0.6075(4) 0.7534(3) 0.0804(2) 0.0257(8) Uani 1 d . . C3 C 0.5546(5) 0.6673(3) 0.0356(2) 0.0400(11) Uani 1 d . . H3A H 0.5275(5) 0.6037(3) 0.0546(2) 0.048 Uiso 1 calc R . C4 C 0.5413(6) 0.6746(4) -0.0369(2) 0.0535(14) Uani 1 d . . H4A H 0.5035(6) 0.6158(4) -0.0669(2) 0.064 Uiso 1 calc R . C5 C 0.5821(5) 0.7652(4) -0.0650(2) 0.0508(13) Uani 1 d . . H5A H 0.5722(5) 0.7693(4) -0.1144(2) 0.061 Uiso 1 calc R . C6 C 0.6382(5) 0.8519(4) -0.0213(2) 0.0391(11) Uani 1 d . . H6A H 0.6677(5) 0.9150(4) -0.0408(2) 0.047 Uiso 1 calc R . C7 C 0.6507(4) 0.8455(3) 0.0507(2) 0.0310(9) Uani 1 d . . H7A H 0.6892(4) 0.9046(3) 0.0803(2) 0.037 Uiso 1 calc R . C8 C 0.6119(4) 0.6213(3) 0.1898(2) 0.0259(8) Uani 1 d . . C9 C 0.5002(5) 0.5463(3) 0.2055(2) 0.0341(10) Uani 1 d . . H9A H 0.4155(5) 0.5607(3) 0.2094(2) 0.041 Uiso 1 calc R . C10 C 0.5122(6) 0.4502(3) 0.2156(2) 0.0433(12) Uani 1 d . . H10A H 0.4360(6) 0.3995(3) 0.2270(2) 0.052 Uiso 1 calc R . C11 C 0.6341(6) 0.4280(4) 0.2091(3) 0.0491(13) Uani 1 d . . H11A H 0.6415(6) 0.3621(4) 0.2154(3) 0.059 Uiso 1 calc R . C12 C 0.7442(6) 0.5014(4) 0.1935(3) 0.0549(15) Uani 1 d . . H12A H 0.8283(6) 0.4862(4) 0.1894(3) 0.066 Uiso 1 calc R . C13 C 0.7345(5) 0.5979(3) 0.1838(3) 0.0430(12) Uani 1 d . . H13A H 0.8119(5) 0.6481(3) 0.1730(3) 0.052 Uiso 1 calc R . C14 C 0.7380(4) 1.0187(3) 0.2940(2) 0.0267(8) Uani 1 d . . C15 C 0.8804(5) 1.0620(3) 0.3061(2) 0.0397(11) Uani 1 d . . H15A H 0.9407(5) 1.0205(3) 0.3091(2) 0.048 Uiso 1 calc R . C16 C 0.9341(5) 1.1647(4) 0.3137(3) 0.0471(13) Uani 1 d . . H16A H 1.0311(5) 1.1931(4) 0.3227(3) 0.057 Uiso 1 calc R . C17 C 0.8482(5) 1.2265(3) 0.3084(2) 0.0446(12) Uani 1 d . . H17A H 0.8861(5) 1.2970(3) 0.3127(2) 0.054 Uiso 1 calc R . C18 C 0.7075(5) 1.1855(3) 0.2969(2) 0.0374(10) Uani 1 d . . H18A H 0.6478(5) 1.2275(3) 0.2936(2) 0.045 Uiso 1 calc R . C19 C 0.6534(4) 1.0817(3) 0.2902(2) 0.0295(9) Uani 1 d . . H19A H 0.5563(4) 1.0536(3) 0.2829(2) 0.035 Uiso 1 calc R . C20 C 0.7184(4) 0.8427(3) 0.3709(2) 0.0264(8) Uani 1 d . . C21 C 0.7226(5) 0.7447(3) 0.3784(2) 0.0381(10) Uani 1 d . . H21A H 0.7025(5) 0.6995(3) 0.3383(2) 0.046 Uiso 1 calc R . C22 C 0.7565(5) 0.7122(4) 0.4448(3) 0.0516(14) Uani 1 d . . H22A H 0.7599(5) 0.6451(4) 0.4495(3) 0.062 Uiso 1 calc R . C23 C 0.7848(5) 0.7768(4) 0.5033(3) 0.0486(13) Uani 1 d . . H23A H 0.8071(5) 0.7542(4) 0.5483(3) 0.058 Uiso 1 calc R . C24 C 0.7807(5) 0.8735(5) 0.4963(2) 0.0507(13) Uani 1 d . . H24A H 0.7999(5) 0.9180(5) 0.5367(2) 0.061 Uiso 1 calc R . C25 C 0.7488(5) 0.9073(4) 0.4306(2) 0.0392(11) Uani 1 d . . H25A H 0.7476(5) 0.9749(4) 0.4264(2) 0.047 Uiso 1 calc R . C26 C 0.1392(4) 0.7775(3) 0.2209(2) 0.0244(8) Uani 1 d . . H26A H 0.0985(4) 0.7207(3) 0.2486(2) 0.029 Uiso 1 calc R . H26B H 0.0670(4) 0.8076(3) 0.1997(2) 0.029 Uiso 1 calc R . C27 C 0.1732(4) 0.6093(3) 0.1315(2) 0.0279(9) Uani 1 d . . C28 C 0.1936(5) 0.5742(4) 0.0665(2) 0.0424(11) Uani 1 d . . H28A H 0.2316(5) 0.6204(4) 0.0340(2) 0.051 Uiso 1 calc R . C29 C 0.1583(6) 0.4720(4) 0.0492(3) 0.058(2) Uani 1 d . . H29A H 0.1720(6) 0.4487(4) 0.0048(3) 0.069 Uiso 1 calc R . C30 C 0.1033(6) 0.4039(4) 0.0965(3) 0.0572(15) Uani 1 d . . H30A H 0.0797(6) 0.3341(4) 0.0847(3) 0.069 Uiso 1 calc R . C31 C 0.0831(5) 0.4384(3) 0.1606(3) 0.0457(12) Uani 1 d . . H31A H 0.0453(5) 0.3921(3) 0.1931(3) 0.055 Uiso 1 calc R . C32 C 0.1174(4) 0.5402(3) 0.1782(2) 0.0348(10) Uani 1 d . . H32A H 0.1027(4) 0.5630(3) 0.2226(2) 0.042 Uiso 1 calc R . C33 C 0.1869(4) 0.7977(3) 0.0742(2) 0.0258(8) Uani 1 d . . C34 C 0.2813(4) 0.8271(3) 0.0277(2) 0.0329(9) Uani 1 d . . H34A H 0.3712(4) 0.8190(3) 0.0385(2) 0.039 Uiso 1 calc R . C35 C 0.2455(5) 0.8683(3) -0.0349(2) 0.0402(11) Uani 1 d . . H35A H 0.3102(5) 0.8870(3) -0.0669(2) 0.048 Uiso 1 calc R . C36 C 0.1161(5) 0.8820(4) -0.0502(2) 0.0435(12) Uani 1 d . . H36A H 0.0922(5) 0.9116(4) -0.0922(2) 0.052 Uiso 1 calc R . C37 C 0.0212(5) 0.8525(4) -0.0045(2) 0.0412(11) Uani 1 d . . H37A H -0.0679(5) 0.8620(4) -0.0152(2) 0.049 Uiso 1 calc R . C38 C 0.0548(4) 0.8092(3) 0.0570(2) 0.0339(10) Uani 1 d . . H38A H -0.0121(4) 0.7874(3) 0.0874(2) 0.041 Uiso 1 calc R . C39 C 0.2605(4) 0.9935(3) 0.2563(2) 0.0248(8) Uani 1 d . . C40 C 0.2985(4) 1.0690(3) 0.3097(2) 0.0312(9) Uani 1 d . . H40A H 0.3342(4) 1.0552(3) 0.3553(2) 0.037 Uiso 1 calc R . C41 C 0.2849(5) 1.1638(3) 0.2975(2) 0.0355(10) Uani 1 d . . H41A H 0.3116(5) 1.2143(3) 0.3346(2) 0.043 Uiso 1 calc R . C42 C 0.2326(5) 1.1852(3) 0.2315(2) 0.0359(10) Uani 1 d . . H42A H 0.2226(5) 1.2499(3) 0.2231(2) 0.043 Uiso 1 calc R . C43 C 0.1951(5) 1.1108(3) 0.1781(2) 0.0365(10) Uani 1 d . . H43A H 0.1591(5) 1.1248(3) 0.1326(2) 0.044 Uiso 1 calc R . C44 C 0.2095(4) 1.0166(3) 0.1900(2) 0.0308(9) Uani 1 d . . H44A H 0.1841(4) 0.9667(3) 0.1525(2) 0.037 Uiso 1 calc R . C45 C 0.2686(4) 0.8603(3) 0.3643(2) 0.0234(8) Uani 1 d . . C46 C 0.1404(5) 0.8374(4) 0.3864(2) 0.0430(12) Uani 1 d . . H46A H 0.0595(5) 0.8251(4) 0.3530(2) 0.052 Uiso 1 calc R . C47 C 0.1301(6) 0.8324(4) 0.4572(3) 0.0552(15) Uani 1 d . . H47A H 0.0418(6) 0.8166(4) 0.4720(3) 0.066 Uiso 1 calc R . C48 C 0.2468(6) 0.8503(3) 0.5063(2) 0.0444(12) Uani 1 d . . H48A H 0.2389(6) 0.8461(3) 0.5548(2) 0.053 Uiso 1 calc R . C49 C 0.3734(5) 0.8740(4) 0.4849(2) 0.0408(11) Uani 1 d . . H49A H 0.4541(5) 0.8874(4) 0.5186(2) 0.049 Uiso 1 calc R . C50 C 0.3847(4) 0.8784(3) 0.4140(2) 0.0321(9) Uani 1 d . . H50A H 0.4733(4) 0.8940(3) 0.3994(2) 0.039 Uiso 1 calc R . C51 C 0.4827(4) 0.9207(3) 0.1680(2) 0.0235(8) Uani 1 d . . C52 C 0.3942(4) 0.7094(3) 0.2859(2) 0.0227(8) Uani 1 d . . C53 C 0.2013(5) 0.5680(4) 0.5299(2) 0.0419(11) Uani 1 d . . H53A H 0.1401(5) 0.4988(4) 0.5220(2) 0.050 Uiso 1 calc R . H53B H 0.1442(5) 0.6146(4) 0.5337(2) 0.050 Uiso 1 calc R . C54 C 0.3052(6) 0.5778(4) 0.5951(3) 0.062(2) Uani 1 d . . H54A H 0.2727(6) 0.6032(4) 0.6360(3) 0.075 Uiso 1 calc R . H54B H 0.3223(6) 0.5125(4) 0.6053(3) 0.075 Uiso 1 calc R . C55 C 0.4331(6) 0.6511(5) 0.5781(3) 0.065(2) Uani 1 d . . H55A H 0.5167(6) 0.6404(5) 0.6053(3) 0.079 Uiso 1 calc R . H55B H 0.4313(6) 0.7208(5) 0.5877(3) 0.079 Uiso 1 calc R . C56 C 0.4286(5) 0.6290(4) 0.5011(3) 0.0502(13) Uani 1 d . . H56A H 0.4733(5) 0.6901(4) 0.4784(3) 0.060 Uiso 1 calc R . H56B H 0.4761(5) 0.5773(4) 0.4933(3) 0.060 Uiso 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 Co1 0.0332(3) 0.0258(3) 0.0271(3) 0.0031(2) 0.0085(2) 0.0001(2) Cl1 0.0588(8) 0.0219(5) 0.0645(8) 0.0044(5) 0.0047(6) 0.0048(5) Cl2 0.0330(6) 0.0640(8) 0.0376(6) 0.0054(5) 0.0121(5) 0.0111(5) Mn1 0.0193(3) 0.0197(3) 0.0176(3) -0.0004(2) 0.0052(2) 0.0027(2) P1 0.0227(5) 0.0232(5) 0.0211(5) -0.0005(4) 0.0068(4) 0.0049(4) P2 0.0202(5) 0.0228(5) 0.0214(5) -0.0012(4) 0.0044(4) 0.0031(4) P3 0.0209(5) 0.0248(5) 0.0212(5) -0.0020(4) 0.0038(4) 0.0032(4) P4 0.0209(5) 0.0224(5) 0.0202(5) -0.0013(4) 0.0053(4) 0.0047(4) O1 0.039(2) 0.031(2) 0.028(2) 0.0076(12) 0.0064(13) 0.0069(13) O2 0.032(2) 0.064(2) 0.031(2) -0.005(2) 0.0049(14) -0.008(2) N1 0.032(2) 0.023(2) 0.029(2) -0.0002(14) 0.0095(15) 0.0043(14) C1 0.024(2) 0.029(2) 0.027(2) -0.005(2) 0.007(2) 0.004(2) C2 0.030(2) 0.028(2) 0.020(2) 0.001(2) 0.008(2) 0.008(2) C3 0.053(3) 0.035(2) 0.030(2) -0.003(2) 0.010(2) 0.008(2) C4 0.074(4) 0.052(3) 0.026(2) -0.008(2) 0.012(2) 0.001(3) C5 0.055(3) 0.069(4) 0.023(2) 0.005(2) 0.010(2) 0.006(3) C6 0.044(3) 0.046(3) 0.032(2) 0.014(2) 0.016(2) 0.014(2) C7 0.031(2) 0.033(2) 0.030(2) 0.002(2) 0.011(2) 0.008(2) C8 0.029(2) 0.025(2) 0.024(2) 0.000(2) 0.003(2) 0.008(2) C9 0.041(3) 0.030(2) 0.031(2) -0.003(2) 0.010(2) 0.008(2) C10 0.065(3) 0.027(2) 0.035(3) 0.004(2) 0.014(2) 0.005(2) C11 0.074(4) 0.035(3) 0.039(3) 0.002(2) -0.008(3) 0.024(3) C12 0.046(3) 0.039(3) 0.079(4) -0.008(3) -0.012(3) 0.024(2) C13 0.029(2) 0.034(2) 0.065(3) -0.004(2) 0.002(2) 0.011(2) C14 0.026(2) 0.025(2) 0.025(2) -0.002(2) 0.005(2) -0.001(2) C15 0.031(2) 0.036(2) 0.049(3) -0.009(2) 0.011(2) 0.003(2) C16 0.033(3) 0.038(3) 0.060(3) -0.011(2) 0.016(2) -0.010(2) C17 0.058(3) 0.028(2) 0.040(3) -0.001(2) 0.015(2) -0.006(2) C18 0.045(3) 0.028(2) 0.035(2) 0.005(2) 0.003(2) 0.006(2) C19 0.030(2) 0.027(2) 0.028(2) -0.001(2) 0.004(2) 0.003(2) C20 0.019(2) 0.037(2) 0.023(2) 0.003(2) 0.0027(15) 0.006(2) C21 0.036(2) 0.034(2) 0.038(3) 0.002(2) -0.007(2) 0.004(2) C22 0.045(3) 0.043(3) 0.058(3) 0.018(2) -0.012(2) 0.005(2) C23 0.034(3) 0.073(4) 0.038(3) 0.019(3) 0.003(2) 0.014(3) C24 0.052(3) 0.080(4) 0.027(2) 0.001(2) 0.006(2) 0.030(3) C25 0.046(3) 0.050(3) 0.025(2) -0.003(2) 0.003(2) 0.022(2) C26 0.022(2) 0.027(2) 0.023(2) -0.0021(15) 0.006(2) 0.004(2) C27 0.024(2) 0.027(2) 0.029(2) -0.006(2) 0.000(2) 0.002(2) C28 0.055(3) 0.039(3) 0.033(2) -0.005(2) 0.010(2) 0.010(2) C29 0.090(4) 0.038(3) 0.044(3) -0.016(2) 0.010(3) 0.016(3) C30 0.076(4) 0.026(2) 0.063(4) -0.013(2) 0.001(3) 0.010(3) C31 0.044(3) 0.030(2) 0.057(3) 0.001(2) 0.008(2) 0.000(2) C32 0.034(2) 0.030(2) 0.034(2) -0.005(2) 0.005(2) -0.001(2) C33 0.026(2) 0.027(2) 0.023(2) -0.003(2) 0.000(2) 0.007(2) C34 0.028(2) 0.038(2) 0.031(2) 0.004(2) 0.004(2) 0.005(2) C35 0.041(3) 0.044(3) 0.030(2) 0.007(2) 0.006(2) 0.004(2) C36 0.041(3) 0.048(3) 0.036(3) 0.013(2) -0.006(2) 0.008(2) C37 0.035(3) 0.052(3) 0.036(3) 0.000(2) -0.007(2) 0.018(2) C38 0.027(2) 0.048(3) 0.024(2) -0.004(2) -0.001(2) 0.009(2) C39 0.021(2) 0.026(2) 0.028(2) 0.001(2) 0.006(2) 0.007(2) C40 0.034(2) 0.032(2) 0.027(2) -0.002(2) 0.000(2) 0.011(2) C41 0.041(3) 0.028(2) 0.039(2) -0.007(2) 0.002(2) 0.013(2) C42 0.035(2) 0.030(2) 0.046(3) 0.010(2) 0.011(2) 0.012(2) C43 0.037(2) 0.046(3) 0.031(2) 0.011(2) 0.007(2) 0.018(2) C44 0.034(2) 0.033(2) 0.027(2) 0.000(2) 0.005(2) 0.010(2) C45 0.027(2) 0.023(2) 0.022(2) -0.0009(15) 0.010(2) 0.008(2) C46 0.029(2) 0.062(3) 0.035(3) -0.006(2) 0.012(2) 0.005(2) C47 0.045(3) 0.074(4) 0.043(3) -0.004(3) 0.029(2) 0.002(3) C48 0.070(4) 0.038(3) 0.025(2) 0.002(2) 0.023(2) 0.009(2) C49 0.055(3) 0.045(3) 0.026(2) 0.001(2) 0.006(2) 0.021(2) C50 0.033(2) 0.041(2) 0.024(2) 0.002(2) 0.009(2) 0.011(2) C51 0.020(2) 0.028(2) 0.022(2) 0.000(2) 0.0055(15) 0.005(2) C52 0.019(2) 0.023(2) 0.025(2) -0.0060(15) 0.0026(15) 0.0033(15) C53 0.042(3) 0.049(3) 0.030(2) 0.003(2) 0.012(2) 0.003(2) C54 0.076(4) 0.061(4) 0.031(3) 0.001(2) -0.009(3) -0.004(3) C55 0.062(4) 0.071(4) 0.052(4) -0.004(3) -0.013(3) 0.009(3) C56 0.033(3) 0.060(3) 0.054(3) -0.006(3) 0.003(2) 0.010(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 Co1 N1 1.970(3) . ? Co1 O2 2.004(3) . ? Co1 Cl1 2.2276(13) . ? Co1 Cl2 2.2510(14) . ? Mn1 C51 1.791(4) . ? Mn1 C52 1.960(4) . ? Mn1 P1 2.2688(12) . ? Mn1 P2 2.2765(13) . ? Mn1 P4 2.2770(12) . ? Mn1 P3 2.2845(13) . ? P1 C2 1.828(4) . ? P1 C8 1.830(4) . ? P1 C1 1.857(4) . ? P2 C14 1.830(4) . ? P2 C20 1.837(4) . ? P2 C1 1.860(4) . ? P3 C27 1.833(4) . ? P3 C33 1.841(4) . ? P3 C26 1.848(4) . ? P4 C45 1.828(4) . ? P4 C39 1.830(4) . ? P4 C26 1.863(4) . ? O1 C51 1.168(4) . ? O2 C56 1.447(6) . ? O2 C53 1.452(5) . ? N1 C52 1.169(5) . ? C2 C3 1.398(6) . ? C2 C7 1.399(5) . ? C3 C4 1.394(6) . ? C4 C5 1.365(7) . ? C5 C6 1.395(7) . ? C6 C7 1.384(6) . ? C8 C9 1.391(6) . ? C8 C13 1.393(6) . ? C9 C10 1.392(6) . ? C10 C11 1.379(7) . ? C11 C12 1.366(8) . ? C12 C13 1.388(7) . ? C14 C19 1.384(6) . ? C14 C15 1.397(6) . ? C15 C16 1.382(6) . ? C16 C17 1.381(7) . ? C17 C18 1.376(7) . ? C18 C19 1.396(6) . ? C20 C21 1.387(6) . ? C20 C25 1.393(6) . ? C21 C22 1.398(6) . ? C22 C23 1.376(7) . ? C23 C24 1.367(7) . ? C24 C25 1.391(6) . ? C27 C32 1.391(6) . ? C27 C28 1.397(6) . ? C28 C29 1.391(6) . ? C29 C30 1.389(8) . ? C30 C31 1.378(7) . ? C31 C32 1.387(6) . ? C33 C34 1.388(5) . ? C33 C38 1.397(6) . ? C34 C35 1.395(6) . ? C35 C36 1.379(7) . ? C36 C37 1.381(7) . ? C37 C38 1.386(6) . ? C39 C44 1.393(6) . ? C39 C40 1.394(5) . ? C40 C41 1.386(6) . ? C41 C42 1.384(6) . ? C42 C43 1.383(6) . ? C43 C44 1.380(6) . ? C45 C50 1.382(6) . ? C45 C46 1.384(6) . ? C46 C47 1.385(6) . ? C47 C48 1.380(7) . ? C48 C49 1.363(7) . ? C49 C50 1.390(6) . ? C53 C54 1.511(7) . ? C54 C55 1.500(8) . ? C55 C56 1.501(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 N1 Co1 O2 102.95(14) . . ? N1 Co1 Cl1 111.98(11) . . ? O2 Co1 Cl1 109.47(12) . . ? N1 Co1 Cl2 112.00(11) . . ? O2 Co1 Cl2 105.59(11) . . ? Cl1 Co1 Cl2 114.03(6) . . ? C51 Mn1 C52 172.8(2) . . ? C51 Mn1 P1 92.29(12) . . ? C52 Mn1 P1 94.95(11) . . ? C51 Mn1 P2 88.16(13) . . ? C52 Mn1 P2 93.92(11) . . ? P1 Mn1 P2 73.57(4) . . ? C51 Mn1 P4 92.33(12) . . ? C52 Mn1 P4 80.44(11) . . ? P1 Mn1 P4 174.73(4) . . ? P2 Mn1 P4 109.13(4) . . ? C51 Mn1 P3 92.41(13) . . ? C52 Mn1 P3 85.84(11) . . ? P1 Mn1 P3 103.75(4) . . ? P2 Mn1 P3 177.29(5) . . ? P4 Mn1 P3 73.50(4) . . ? C2 P1 C8 101.5(2) . . ? C2 P1 C1 108.1(2) . . ? C8 P1 C1 105.2(2) . . ? C2 P1 Mn1 120.49(14) . . ? C8 P1 Mn1 124.55(13) . . ? C1 P1 Mn1 95.05(13) . . ? C14 P2 C20 102.8(2) . . ? C14 P2 C1 106.0(2) . . ? C20 P2 C1 104.9(2) . . ? C14 P2 Mn1 120.95(14) . . ? C20 P2 Mn1 124.49(13) . . ? C1 P2 Mn1 94.72(13) . . ? C27 P3 C33 101.4(2) . . ? C27 P3 C26 109.2(2) . . ? C33 P3 C26 105.7(2) . . ? C27 P3 Mn1 124.10(14) . . ? C33 P3 Mn1 120.37(13) . . ? C26 P3 Mn1 94.27(12) . . ? C45 P4 C39 101.2(2) . . ? C45 P4 C26 106.9(2) . . ? C39 P4 C26 106.0(2) . . ? C45 P4 Mn1 123.58(13) . . ? C39 P4 Mn1 122.67(13) . . ? C26 P4 Mn1 94.10(12) . . ? C56 O2 C53 110.6(4) . . ? C56 O2 Co1 122.5(3) . . ? C53 O2 Co1 125.1(3) . . ? C52 N1 Co1 162.0(3) . . ? P1 C1 P2 94.2(2) . . ? C3 C2 C7 118.3(4) . . ? C3 C2 P1 120.0(3) . . ? C7 C2 P1 121.0(3) . . ? C4 C3 C2 120.2(4) . . ? C5 C4 C3 120.7(5) . . ? C4 C5 C6 120.1(4) . . ? C7 C6 C5 119.6(4) . . ? C6 C7 C2 121.0(4) . . ? C9 C8 C13 118.7(4) . . ? C9 C8 P1 120.3(3) . . ? C13 C8 P1 121.0(3) . . ? C8 C9 C10 120.2(4) . . ? C11 C10 C9 120.4(5) . . ? C12 C11 C10 119.7(5) . . ? C11 C12 C13 120.8(5) . . ? C12 C13 C8 120.3(5) . . ? C19 C14 C15 118.0(4) . . ? C19 C14 P2 119.3(3) . . ? C15 C14 P2 122.7(3) . . ? C16 C15 C14 120.6(4) . . ? C17 C16 C15 120.6(4) . . ? C18 C17 C16 119.9(4) . . ? C17 C18 C19 119.4(4) . . ? C14 C19 C18 121.5(4) . . ? C21 C20 C25 118.6(4) . . ? C21 C20 P2 120.5(3) . . ? C25 C20 P2 120.8(3) . . ? C20 C21 C22 120.2(4) . . ? C23 C22 C21 120.4(5) . . ? C24 C23 C22 119.7(5) . . ? C23 C24 C25 120.6(5) . . ? C24 C25 C20 120.5(5) . . ? P3 C26 P4 94.7(2) . . ? C32 C27 C28 118.7(4) . . ? C32 C27 P3 122.3(3) . . ? C28 C27 P3 118.6(3) . . ? C29 C28 C27 120.3(5) . . ? C30 C29 C28 120.3(5) . . ? C31 C30 C29 119.5(4) . . ? C30 C31 C32 120.6(5) . . ? C31 C32 C27 120.6(4) . . ? C34 C33 C38 118.8(4) . . ? C34 C33 P3 118.9(3) . . ? C38 C33 P3 122.3(3) . . ? C33 C34 C35 120.7(4) . . ? C36 C35 C34 119.8(4) . . ? C35 C36 C37 119.9(4) . . ? C36 C37 C38 120.6(4) . . ? C37 C38 C33 120.1(4) . . ? C44 C39 C40 117.9(4) . . ? C44 C39 P4 121.4(3) . . ? C40 C39 P4 120.5(3) . . ? C41 C40 C39 121.1(4) . . ? C42 C41 C40 120.3(4) . . ? C43 C42 C41 119.0(4) . . ? C44 C43 C42 120.8(4) . . ? C43 C44 C39 120.9(4) . . ? C50 C45 C46 118.8(4) . . ? C50 C45 P4 119.0(3) . . ? C46 C45 P4 122.1(3) . . ? C45 C46 C47 120.0(5) . . ? C48 C47 C46 120.6(4) . . ? C49 C48 C47 119.6(4) . . ? C48 C49 C50 120.1(5) . . ? C45 C50 C49 120.7(4) . . ? O1 C51 Mn1 177.2(3) . . ? N1 C52 Mn1 172.3(3) . . ? O2 C53 C54 104.7(4) . . ? C55 C54 C53 104.5(4) . . ? C54 C55 C56 103.3(4) . . ? O2 C56 C55 105.3(4) . . ? _refine_diff_density_max 0.715 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.085 #=END data_2.thf _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C60 H60 Cl2 Mn2 N O3 P4' _chemical_formula_weight 1147.83 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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 13.3946(13) _cell_length_b 14.3660(8) _cell_length_c 16.995(2) _cell_angle_alpha 110.087(9) _cell_angle_beta 106.829(8) _cell_angle_gamma 99.213(8) _cell_volume 2814.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 85 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 24.98 _exptl_crystal_description 'square plates' _exptl_crystal_colour orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method ? _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 0.702 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.771 _exptl_absorpt_correction_T_max 0.819 _exptl_special_details ; ? ; _diffrn_ambient_temperature 73(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17706 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0141 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 27.49 _reflns_number_total 12194 _reflns_number_observed 11037 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 11 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+2.8684P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12183 _refine_ls_number_parameters 711 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_obs 0.0363 _refine_ls_wR_factor_all 0.0978 _refine_ls_wR_factor_obs 0.0885 _refine_ls_goodness_of_fit_all 1.072 _refine_ls_goodness_of_fit_obs 1.026 _refine_ls_restrained_S_all 1.075 _refine_ls_restrained_S_obs 1.026 _refine_ls_shift/esd_max 0.040 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.17121(2) 0.39671(2) 0.22804(2) 0.01953(7) Uani 1 d . . Mn2 Mn 0.38824(3) 0.77330(2) 0.35482(2) 0.03569(9) Uani 1 d . . Cl1 Cl 0.41055(7) 0.84560(5) 0.25655(5) 0.0627(2) Uani 1 d . . Cl2 Cl 0.53411(5) 0.77335(5) 0.46910(5) 0.0500(2) Uani 1 d . . P1 P 0.00619(4) 0.42790(4) 0.18712(3) 0.02215(10) Uani 1 d . . P2 P 0.12825(4) 0.38207(4) 0.08286(3) 0.02212(10) Uani 1 d . . P3 P 0.21983(4) 0.41997(4) 0.37551(3) 0.02149(10) Uani 1 d . . P4 P 0.34332(4) 0.38055(4) 0.27104(3) 0.02156(10) Uani 1 d . . N1 N 0.26598(15) 0.63456(13) 0.29523(13) 0.0332(4) Uani 1 d . . O1 O 0.08263(14) 0.17191(11) 0.17029(11) 0.0394(4) Uani 1 d . . C1 C 0.0171(2) 0.4431(2) 0.08568(13) 0.0264(4) Uani 1 d . . H1B H -0.0490(2) 0.4051(2) 0.03251(13) 0.032 Uiso 1 calc R . H1C H 0.0385(2) 0.5151(2) 0.09511(13) 0.032 Uiso 1 calc R . C2 C -0.12443(15) 0.3287(2) 0.14474(13) 0.0277(4) Uani 1 d . . C3 C -0.2086(2) 0.3479(2) 0.1744(2) 0.0363(5) Uani 1 d . . H3A H -0.1998(2) 0.4131(2) 0.2170(2) 0.044 Uiso 1 calc R . C4 C -0.3061(2) 0.2701(2) 0.1408(2) 0.0476(6) Uani 1 d . . H4A H -0.3617(2) 0.2834(2) 0.1615(2) 0.057 Uiso 1 calc R . C5 C -0.3203(2) 0.1733(2) 0.0769(2) 0.0530(7) Uani 1 d . . H5A H -0.3856(2) 0.1217(2) 0.0540(2) 0.064 Uiso 1 calc R . C6 C -0.2372(2) 0.1534(2) 0.0469(2) 0.0504(6) Uani 1 d . . H6A H -0.2468(2) 0.0882(2) 0.0038(2) 0.061 Uiso 1 calc R . C7 C -0.1394(2) 0.2302(2) 0.0810(2) 0.0382(5) Uani 1 d . . H7A H -0.0835(2) 0.2159(2) 0.0612(2) 0.046 Uiso 1 calc R . C8 C -0.02355(14) 0.54515(15) 0.24858(13) 0.0251(4) Uani 1 d . . C9 C -0.0029(2) 0.5756(2) 0.34044(14) 0.0313(4) Uani 1 d . . H9A H 0.0276(2) 0.5370(2) 0.36971(14) 0.038 Uiso 1 calc R . C10 C -0.0273(2) 0.6624(2) 0.38850(15) 0.0366(5) Uani 1 d . . H10A H -0.0147(2) 0.6809(2) 0.44936(15) 0.044 Uiso 1 calc R . C11 C -0.0705(2) 0.7219(2) 0.3461(2) 0.0366(5) Uani 1 d . . H11A H -0.0858(2) 0.7809(2) 0.3786(2) 0.044 Uiso 1 calc R . C12 C -0.0908(2) 0.6929(2) 0.2550(2) 0.0377(5) Uani 1 d . . H12A H -0.1193(2) 0.7328(2) 0.2264(2) 0.045 Uiso 1 calc R . C13 C -0.0687(2) 0.6043(2) 0.20632(14) 0.0324(4) Uani 1 d . . H13A H -0.0841(2) 0.5844(2) 0.14490(14) 0.039 Uiso 1 calc R . C14 C 0.0642(2) 0.2558(2) -0.01325(13) 0.0286(4) Uani 1 d . . C15 C 0.1018(2) 0.1714(2) -0.01077(15) 0.0363(5) Uani 1 d . . H15A H 0.1614(2) 0.1800(2) 0.03854(15) 0.044 Uiso 1 calc R . C16 C 0.0500(3) 0.0742(2) -0.0822(2) 0.0518(7) Uani 1 d . . H16A H 0.0753(3) 0.0181(2) -0.0803(2) 0.062 Uiso 1 calc R . C17 C -0.0383(3) 0.0604(2) -0.1558(2) 0.0600(8) Uani 1 d . . H17A H -0.0728(3) -0.0049(2) -0.2028(2) 0.072 Uiso 1 calc R . C18 C -0.0756(3) 0.1432(2) -0.1597(2) 0.0555(7) Uani 1 d . . H18A H -0.1350(3) 0.1339(2) -0.2094(2) 0.067 Uiso 1 calc R . C19 C -0.0242(2) 0.2409(2) -0.08913(15) 0.0410(5) Uani 1 d . . H19A H -0.0489(2) 0.2969(2) -0.09250(15) 0.049 Uiso 1 calc R . C20 C 0.21386(15) 0.4500(2) 0.04073(12) 0.0252(4) Uani 1 d . . C21 C 0.2661(2) 0.3960(2) -0.01171(14) 0.0335(4) Uani 1 d . . H21A H 0.2537(2) 0.3252(2) -0.02820(14) 0.040 Uiso 1 calc R . C22 C 0.3368(2) 0.4473(2) -0.0396(2) 0.0409(5) Uani 1 d . . H22A H 0.3718(2) 0.4107(2) -0.0739(2) 0.049 Uiso 1 calc R . C23 C 0.3551(2) 0.5524(2) -0.0164(2) 0.0414(5) Uani 1 d . . H23A H 0.4007(2) 0.5861(2) -0.0365(2) 0.050 Uiso 1 calc R . C24 C 0.3051(2) 0.6075(2) 0.0369(2) 0.0367(5) Uani 1 d . . H24A H 0.3178(2) 0.6783(2) 0.0531(2) 0.044 Uiso 1 calc R . C25 C 0.2360(2) 0.5571(2) 0.06621(14) 0.0288(4) Uani 1 d . . H25A H 0.2042(2) 0.5948(2) 0.10312(14) 0.035 Uiso 1 calc R . C26 C 0.36322(15) 0.4217(2) 0.39201(12) 0.0260(4) Uani 1 d . . H26A H 0.38508(15) 0.3723(2) 0.41541(12) 0.031 Uiso 1 calc R . H26B H 0.41398(15) 0.4902(2) 0.42968(12) 0.031 Uiso 1 calc R . C27 C 0.1592(2) 0.31341(15) 0.39818(13) 0.0264(4) Uani 1 d . . C28 C 0.0486(2) 0.2612(2) 0.35089(14) 0.0323(4) Uani 1 d . . H28A H 0.0065(2) 0.2830(2) 0.31059(14) 0.039 Uiso 1 calc R . C29 C 0.0006(2) 0.1769(2) 0.3634(2) 0.0422(5) Uani 1 d . . H29A H -0.0734(2) 0.1429(2) 0.3321(2) 0.051 Uiso 1 calc R . C30 C 0.0635(2) 0.1437(2) 0.4227(2) 0.0470(6) Uani 1 d . . H30A H 0.0321(2) 0.0863(2) 0.4301(2) 0.056 Uiso 1 calc R . C31 C 0.1726(2) 0.1957(2) 0.4708(2) 0.0450(6) Uani 1 d . . H31A H 0.2142(2) 0.1735(2) 0.5110(2) 0.054 Uiso 1 calc R . C32 C 0.2208(2) 0.2810(2) 0.45960(15) 0.0344(4) Uani 1 d . . H32A H 0.2941(2) 0.3164(2) 0.49308(15) 0.041 Uiso 1 calc R . C33 C 0.2311(2) 0.53410(15) 0.47356(12) 0.0260(4) Uani 1 d . . C34 C 0.3089(2) 0.6279(2) 0.50161(14) 0.0336(4) Uani 1 d . . H34A H 0.3554(2) 0.6324(2) 0.47080(14) 0.040 Uiso 1 calc R . C35 C 0.3174(2) 0.7148(2) 0.5754(2) 0.0445(6) Uani 1 d . . H35A H 0.3705(2) 0.7765(2) 0.5946(2) 0.053 Uiso 1 calc R . C36 C 0.2469(3) 0.7093(2) 0.6202(2) 0.0503(6) Uani 1 d . . H36A H 0.2528(3) 0.7673(2) 0.6695(2) 0.060 Uiso 1 calc R . C37 C 0.1678(2) 0.6179(2) 0.5920(2) 0.0440(6) Uani 1 d . . H37A H 0.1196(2) 0.6149(2) 0.6216(2) 0.053 Uiso 1 calc R . C38 C 0.1600(2) 0.5301(2) 0.51922(14) 0.0321(4) Uani 1 d . . H38A H 0.1071(2) 0.4684(2) 0.50093(14) 0.039 Uiso 1 calc R . C39 C 0.3674(2) 0.25382(15) 0.23629(13) 0.0270(4) Uani 1 d . . C40 C 0.3545(2) 0.1901(2) 0.2809(2) 0.0406(5) Uani 1 d . . H40A H 0.3346(2) 0.2127(2) 0.3309(2) 0.049 Uiso 1 calc R . C41 C 0.3711(2) 0.0927(2) 0.2513(2) 0.0499(6) Uani 1 d . . H41A H 0.3627(2) 0.0509(2) 0.2817(2) 0.060 Uiso 1 calc R . C42 C 0.3998(2) 0.0581(2) 0.1773(2) 0.0519(7) Uani 1 d . . H42A H 0.4118(2) -0.0065(2) 0.1581(2) 0.062 Uiso 1 calc R . C43 C 0.4107(2) 0.1197(2) 0.1312(2) 0.0521(7) Uani 1 d . . H43A H 0.4289(2) 0.0957(2) 0.0805(2) 0.062 Uiso 1 calc R . C44 C 0.3947(2) 0.2172(2) 0.1605(2) 0.0390(5) Uani 1 d . . H44A H 0.4023(2) 0.2582(2) 0.1293(2) 0.047 Uiso 1 calc R . C45 C 0.46247(15) 0.46158(15) 0.26969(12) 0.0245(4) Uani 1 d . . C46 C 0.4479(2) 0.5266(2) 0.22517(14) 0.0305(4) Uani 1 d . . H46A H 0.3778(2) 0.5269(2) 0.19541(14) 0.037 Uiso 1 calc R . C47 C 0.5367(2) 0.5910(2) 0.2247(2) 0.0385(5) Uani 1 d . . H47A H 0.5259(2) 0.6341(2) 0.1948(2) 0.046 Uiso 1 calc R . C48 C 0.6409(2) 0.5909(2) 0.2687(2) 0.0401(5) Uani 1 d . . H48A H 0.7006(2) 0.6340(2) 0.2686(2) 0.048 Uiso 1 calc R . C49 C 0.6564(2) 0.5264(2) 0.3130(2) 0.0400(5) Uani 1 d . . H49A H 0.7267(2) 0.5263(2) 0.3426(2) 0.048 Uiso 1 calc R . C50 C 0.5682(2) 0.4620(2) 0.31378(15) 0.0336(4) Uani 1 d . . H50A H 0.5795(2) 0.4189(2) 0.34369(15) 0.040 Uiso 1 calc R . C51 C 0.1165(2) 0.26017(15) 0.19230(13) 0.0257(4) Uani 1 d . . C52 C 0.23065(15) 0.54573(15) 0.26997(12) 0.0243(4) Uani 1 d . . O2 O 0.3179(2) 0.8671(2) 0.4395(2) 0.0450(6) Uani 0.80 d P 1 C53 C 0.3754(4) 0.9598(3) 0.5213(3) 0.0635(12) Uani 0.80 d P 1 H53A H 0.4052(4) 1.0159(3) 0.5078(3) 0.076 Uiso 0.80 calc PR 1 H53B H 0.4347(4) 0.9480(3) 0.5618(3) 0.076 Uiso 0.80 calc PR 1 C54 C 0.2944(5) 0.9858(5) 0.5636(5) 0.078(2) Uani 0.80 d P 1 H54A H 0.3057(5) 0.9688(5) 0.6154(5) 0.094 Uiso 0.80 calc PR 1 H54B H 0.2996(5) 1.0589(5) 0.5827(5) 0.094 Uiso 0.80 calc PR 1 C56 C 0.2028(6) 0.8554(7) 0.4120(5) 0.109(3) Uani 0.80 d P 1 H56A H 0.1620(6) 0.7840(7) 0.3923(5) 0.131 Uiso 0.80 calc PR 1 H56B H 0.1783(6) 0.8768(7) 0.3632(5) 0.131 Uiso 0.80 calc PR 1 O2' O 0.2866(8) 0.8640(7) 0.3884(8) 0.046(2) Uani 0.20 d P 2 C53' C 0.3373(12) 0.9741(10) 0.4466(13) 0.058(4) Uani 0.20 d P 2 H53C H 0.3045(12) 1.0164(10) 0.4193(13) 0.070 Uiso 0.20 calc PR 2 H53D H 0.4150(12) 0.9933(10) 0.4596(13) 0.070 Uiso 0.20 calc PR 2 C54' C 0.3149(19) 0.9845(14) 0.5294(13) 0.060(5) Uani 0.20 d P 2 H54C H 0.3281(19) 1.0567(14) 0.5677(13) 0.072 Uiso 0.20 calc PR 2 H54D H 0.3601(19) 0.9544(14) 0.5634(13) 0.072 Uiso 0.20 calc PR 2 C56' C 0.2007(13) 0.8301(9) 0.4192(9) 0.019(2) Uiso 0.20 d P 2 H56C H 0.2183(13) 0.7800(9) 0.4432(9) 0.023 Uiso 0.20 calc PR 2 H56D H 0.1318(13) 0.7966(9) 0.3683(9) 0.023 Uiso 0.20 calc PR 2 C55 C 0.1893(3) 0.9225(3) 0.4924(4) 0.100(2) Uani 1 d . . H55A H 0.1471(3) 0.9671(3) 0.4773(4) 0.120 Uiso 1 calc R 1 H55B H 0.1495(3) 0.8806(3) 0.5139(4) 0.120 Uiso 1 calc R 1 O3 O 0.6722(6) 0.8219(4) 0.1785(5) 0.207(3) Uani 1 d . . C57 C 0.5862(6) 0.8286(5) 0.0999(5) 0.107(2) Uani 0.80 d P 1 H57A H 0.5883(6) 0.7832(5) 0.0433(5) 0.128 Uiso 0.80 calc PR 1 H57B H 0.5144(6) 0.8051(5) 0.1004(5) 0.128 Uiso 0.80 calc PR 1 C58 C 0.6040(5) 0.9286(4) 0.1058(4) 0.087(2) Uani 0.80 d P 1 H58A H 0.6168(5) 0.9311(4) 0.0531(4) 0.104 Uiso 0.80 calc PR 1 H58B H 0.5407(5) 0.9523(4) 0.1085(4) 0.104 Uiso 0.80 calc PR 1 C59 C 0.6905(11) 0.9888(7) 0.1800(7) 0.192(6) Uani 0.80 d P 1 H59A H 0.6671(11) 1.0295(7) 0.2262(7) 0.231 Uiso 0.80 calc PR 1 H59B H 0.7366(11) 1.0361(7) 0.1670(7) 0.231 Uiso 0.80 calc PR 1 C60 C 0.7580(8) 0.9199(7) 0.2161(6) 0.121(4) Uani 0.80 d P 1 H60A H 0.8158(8) 0.9117(7) 0.1930(6) 0.145 Uiso 0.80 calc PR 1 H60B H 0.7886(8) 0.9488(7) 0.2815(6) 0.145 Uiso 0.80 calc PR 1 C57' C 0.6359(18) 0.9079(18) 0.0940(15) 0.063(5) Uiso 0.20 d P 2 C58' C 0.7425(16) 0.9920(29) 0.2138(46) 0.186(28) Uani 0.20 d P 2 C59' C 0.7191(40) 0.9845(28) 0.2466(22) 0.138(16) Uani 0.20 d P 2 H59C H 0.6401(40) 0.9650(28) 0.2230(22) 0.165 Uiso 0.20 calc PR 2 H59D H 0.7482(40) 1.0442(28) 0.3042(22) 0.165 Uiso 0.20 calc PR 2 C60' C 0.7613(55) 0.8991(34) 0.2508(31) 0.201(29) Uani 0.20 d P 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01794(13) 0.01978(13) 0.01937(13) 0.00938(10) 0.00431(10) 0.00357(10) Mn2 0.0306(2) 0.0234(2) 0.0478(2) 0.01418(14) 0.01063(14) 0.00282(12) Cl1 0.0897(5) 0.0401(3) 0.0605(4) 0.0321(3) 0.0224(4) 0.0090(3) Cl2 0.0377(3) 0.0531(4) 0.0498(3) 0.0218(3) 0.0058(3) 0.0068(3) P1 0.0181(2) 0.0253(2) 0.0223(2) 0.0116(2) 0.0051(2) 0.0047(2) P2 0.0214(2) 0.0240(2) 0.0206(2) 0.0106(2) 0.0058(2) 0.0057(2) P3 0.0207(2) 0.0236(2) 0.0205(2) 0.0108(2) 0.0064(2) 0.0058(2) P4 0.0198(2) 0.0240(2) 0.0219(2) 0.0117(2) 0.0066(2) 0.0060(2) N1 0.0308(9) 0.0268(9) 0.0375(9) 0.0144(7) 0.0074(7) 0.0039(7) O1 0.0473(9) 0.0241(7) 0.0393(8) 0.0124(6) 0.0114(7) 0.0016(6) C1 0.0241(9) 0.0320(10) 0.0258(9) 0.0162(8) 0.0075(7) 0.0089(7) C2 0.0202(8) 0.0326(10) 0.0271(9) 0.0164(8) 0.0025(7) 0.0016(7) C3 0.0265(10) 0.0426(12) 0.0372(11) 0.0174(10) 0.0105(9) 0.0036(9) C4 0.0264(11) 0.059(2) 0.0564(15) 0.0266(13) 0.0165(10) 0.0023(10) C5 0.0284(11) 0.0494(15) 0.064(2) 0.0222(13) 0.0060(11) -0.0098(10) C6 0.0370(13) 0.0382(13) 0.0526(15) 0.0082(11) 0.0057(11) -0.0053(10) C7 0.0276(10) 0.0372(11) 0.0400(12) 0.0129(10) 0.0073(9) 0.0007(9) C8 0.0187(8) 0.0282(9) 0.0289(9) 0.0128(8) 0.0085(7) 0.0065(7) C9 0.0281(10) 0.0388(11) 0.0304(10) 0.0175(9) 0.0103(8) 0.0124(8) C10 0.0336(11) 0.0431(12) 0.0314(10) 0.0125(9) 0.0131(9) 0.0111(9) C11 0.0304(10) 0.0362(11) 0.0422(12) 0.0118(10) 0.0156(9) 0.0126(9) C12 0.0368(11) 0.0408(12) 0.0446(12) 0.0236(10) 0.0156(10) 0.0206(10) C13 0.0324(10) 0.0405(11) 0.0309(10) 0.0193(9) 0.0119(8) 0.0171(9) C14 0.0323(10) 0.0265(9) 0.0226(9) 0.0093(8) 0.0084(8) 0.0026(8) C15 0.0434(12) 0.0312(11) 0.0304(10) 0.0111(9) 0.0107(9) 0.0100(9) C16 0.074(2) 0.0305(12) 0.0407(13) 0.0099(10) 0.0139(13) 0.0125(12) C17 0.088(2) 0.0297(12) 0.0334(12) 0.0031(10) 0.0041(13) -0.0023(13) C18 0.065(2) 0.0427(14) 0.0299(12) 0.0105(11) -0.0076(11) -0.0017(12) C19 0.0494(13) 0.0336(11) 0.0286(10) 0.0137(9) 0.0012(10) 0.0053(10) C20 0.0219(8) 0.0323(10) 0.0215(8) 0.0141(8) 0.0053(7) 0.0068(7) C21 0.0332(10) 0.0381(11) 0.0320(10) 0.0158(9) 0.0138(9) 0.0109(9) C22 0.0351(11) 0.0550(14) 0.0372(12) 0.0194(11) 0.0198(10) 0.0123(10) C23 0.0325(11) 0.0569(15) 0.0432(12) 0.0307(12) 0.0167(10) 0.0070(10) C24 0.0322(11) 0.0393(11) 0.0412(12) 0.0261(10) 0.0083(9) 0.0055(9) C25 0.0246(9) 0.0330(10) 0.0306(10) 0.0175(8) 0.0069(8) 0.0089(8) C26 0.0228(9) 0.0319(10) 0.0221(8) 0.0121(8) 0.0060(7) 0.0069(7) C27 0.0309(10) 0.0254(9) 0.0268(9) 0.0128(8) 0.0141(8) 0.0075(7) C28 0.0324(10) 0.0341(10) 0.0325(10) 0.0152(9) 0.0144(9) 0.0071(8) C29 0.0403(12) 0.0370(12) 0.0475(13) 0.0155(10) 0.0217(11) 0.0008(10) C30 0.061(2) 0.0344(12) 0.064(2) 0.0284(12) 0.0390(14) 0.0137(11) C31 0.057(2) 0.0466(13) 0.0561(15) 0.0374(12) 0.0306(13) 0.0244(12) C32 0.0370(11) 0.0387(11) 0.0369(11) 0.0226(9) 0.0167(9) 0.0137(9) C33 0.0300(9) 0.0283(9) 0.0203(8) 0.0122(7) 0.0062(7) 0.0110(8) C34 0.0400(11) 0.0295(10) 0.0286(10) 0.0136(8) 0.0078(9) 0.0084(9) C35 0.058(2) 0.0270(11) 0.0359(12) 0.0095(9) 0.0064(11) 0.0088(10) C36 0.077(2) 0.0389(13) 0.0332(12) 0.0103(10) 0.0186(12) 0.0277(13) C37 0.061(2) 0.0474(14) 0.0344(11) 0.0178(10) 0.0239(11) 0.0283(12) C38 0.0364(11) 0.0364(11) 0.0281(10) 0.0158(9) 0.0126(8) 0.0151(9) C39 0.0230(9) 0.0259(9) 0.0293(9) 0.0109(8) 0.0061(7) 0.0075(7) C40 0.0536(14) 0.0363(11) 0.0413(12) 0.0219(10) 0.0206(11) 0.0185(10) C41 0.066(2) 0.0343(12) 0.0522(15) 0.0226(11) 0.0164(13) 0.0197(12) C42 0.057(2) 0.0301(12) 0.060(2) 0.0111(11) 0.0166(13) 0.0195(11) C43 0.060(2) 0.0389(13) 0.0524(15) 0.0059(11) 0.0295(13) 0.0156(12) C44 0.0448(13) 0.0337(11) 0.0375(11) 0.0115(9) 0.0183(10) 0.0104(10) C45 0.0204(8) 0.0283(9) 0.0234(8) 0.0109(7) 0.0069(7) 0.0055(7) C46 0.0214(9) 0.0407(11) 0.0318(10) 0.0212(9) 0.0070(8) 0.0069(8) C47 0.0304(11) 0.0492(13) 0.0416(12) 0.0302(11) 0.0111(9) 0.0049(9) C48 0.0233(10) 0.0537(14) 0.0418(12) 0.0238(11) 0.0111(9) 0.0004(9) C49 0.0188(9) 0.0560(14) 0.0451(13) 0.0253(11) 0.0071(9) 0.0089(9) C50 0.0256(10) 0.0414(11) 0.0367(11) 0.0218(9) 0.0077(8) 0.0118(9) C51 0.0249(9) 0.0276(9) 0.0231(8) 0.0112(7) 0.0070(7) 0.0055(7) C52 0.0205(8) 0.0279(9) 0.0240(8) 0.0130(7) 0.0055(7) 0.0055(7) O2 0.0309(12) 0.0398(12) 0.0530(15) 0.0094(12) 0.0135(11) 0.0071(9) C53 0.056(2) 0.035(2) 0.078(3) -0.003(2) 0.036(2) 0.000(2) C54 0.085(3) 0.056(3) 0.099(5) 0.013(3) 0.062(4) 0.024(2) C56 0.047(3) 0.202(9) 0.094(4) 0.066(5) 0.030(3) 0.057(4) O2' 0.033(5) 0.026(4) 0.065(7) 0.009(5) 0.014(5) 0.001(3) C53' 0.047(7) 0.031(6) 0.096(12) 0.018(7) 0.039(8) 0.009(5) C54' 0.076(15) 0.035(8) 0.050(10) 0.001(7) 0.022(9) 0.007(9) C55 0.066(2) 0.071(2) 0.140(4) 0.007(3) 0.055(3) 0.013(2) O3 0.276(8) 0.118(4) 0.186(6) 0.063(4) 0.070(5) -0.017(4) C57 0.100(4) 0.097(4) 0.103(5) 0.033(4) 0.032(4) 0.006(3) C58 0.080(4) 0.061(3) 0.098(4) 0.008(3) 0.035(3) 0.017(3) C59 0.232(12) 0.091(5) 0.149(8) 0.069(6) -0.061(8) -0.023(7) C60 0.108(6) 0.124(8) 0.105(6) 0.054(5) 0.025(4) -0.020(5) C58' 0.025(8) 0.136(25) 0.483(83) 0.239(44) 0.075(22) 0.028(12) C59' 0.274(47) 0.140(27) 0.114(21) 0.084(20) 0.137(29) 0.163(33) C60' 0.301(65) 0.103(26) 0.141(36) 0.002(24) 0.017(36) 0.140(37) _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 C51 1.794(2) . ? Mn1 C52 1.950(2) . ? Mn1 P1 2.2828(6) . ? Mn1 P4 2.2836(6) . ? Mn1 P3 2.2864(6) . ? Mn1 P2 2.2904(6) . ? Mn2 N1 2.071(2) . ? Mn2 O2' 2.093(10) . ? Mn2 O2 2.153(3) . ? Mn2 Cl1 2.3105(8) . ? Mn2 Cl2 2.3219(8) . ? P1 C8 1.826(2) . ? P1 C2 1.838(2) . ? P1 C1 1.854(2) . ? P2 C14 1.830(2) . ? P2 C20 1.837(2) . ? P2 C1 1.850(2) . ? P3 C27 1.828(2) . ? P3 C33 1.840(2) . ? P3 C26 1.854(2) . ? P4 C39 1.824(2) . ? P4 C45 1.830(2) . ? P4 C26 1.856(2) . ? N1 C52 1.162(3) . ? O1 C51 1.160(2) . ? C2 C3 1.391(3) . ? C2 C7 1.395(3) . ? C3 C4 1.394(3) . ? C4 C5 1.382(4) . ? C5 C6 1.382(4) . ? C6 C7 1.389(3) . ? C8 C13 1.391(3) . ? C8 C9 1.395(3) . ? C9 C10 1.384(3) . ? C10 C11 1.387(3) . ? C11 C12 1.387(3) . ? C12 C13 1.390(3) . ? C14 C15 1.394(3) . ? C14 C19 1.399(3) . ? C15 C16 1.395(3) . ? C16 C17 1.378(4) . ? C17 C18 1.376(4) . ? C18 C19 1.393(3) . ? C20 C21 1.395(3) . ? C20 C25 1.402(3) . ? C21 C22 1.393(3) . ? C22 C23 1.383(4) . ? C23 C24 1.387(4) . ? C24 C25 1.387(3) . ? C27 C28 1.394(3) . ? C27 C32 1.395(3) . ? C28 C29 1.390(3) . ? C29 C30 1.385(4) . ? C30 C31 1.378(4) . ? C31 C32 1.390(3) . ? C33 C34 1.397(3) . ? C33 C38 1.398(3) . ? C34 C35 1.393(3) . ? C35 C36 1.383(4) . ? C36 C37 1.379(4) . ? C37 C38 1.394(3) . ? C39 C44 1.393(3) . ? C39 C40 1.395(3) . ? C40 C41 1.393(3) . ? C41 C42 1.374(4) . ? C42 C43 1.384(4) . ? C43 C44 1.391(3) . ? C45 C46 1.394(3) . ? C45 C50 1.396(3) . ? C46 C47 1.389(3) . ? C47 C48 1.381(3) . ? C48 C49 1.386(3) . ? C49 C50 1.386(3) . ? O2 C56 1.439(7) . ? O2 C53 1.442(4) . ? C53 C54 1.493(5) . ? C54 C55 1.456(8) . ? C56 C55 1.458(9) . ? O2' C53' 1.46(2) . ? O2' C56' 1.48(2) . ? C53' C54' 1.49(3) . ? C54' C55 1.59(2) . ? C56' C55 1.541(14) . ? O3 C60' 1.40(5) . ? O3 C60 1.465(9) . ? O3 C57 1.533(9) . ? C57 C58 1.382(8) . ? C58 C59 1.328(10) . ? C59 C60 1.599(13) . ? C57' C58' 1.93(6) . ? C58' C59' 0.74(5) . ? C58' C60' 1.68(5) . ? C59' C60' 1.44(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 C51 Mn1 C52 178.53(8) . . ? C51 Mn1 P1 95.47(6) . . ? C52 Mn1 P1 84.56(6) . . ? C51 Mn1 P4 89.66(6) . . ? C52 Mn1 P4 90.33(6) . . ? P1 Mn1 P4 174.79(2) . . ? C51 Mn1 P3 90.10(6) . . ? C52 Mn1 P3 88.49(6) . . ? P1 Mn1 P3 107.07(2) . . ? P4 Mn1 P3 73.74(2) . . ? C51 Mn1 P2 92.83(6) . . ? C52 Mn1 P2 88.59(6) . . ? P1 Mn1 P2 73.39(2) . . ? P4 Mn1 P2 105.53(2) . . ? P3 Mn1 P2 176.98(2) . . ? N1 Mn2 O2' 94.3(3) . . ? N1 Mn2 O2 98.88(9) . . ? N1 Mn2 Cl1 114.53(6) . . ? O2' Mn2 Cl1 90.1(3) . . ? O2 Mn2 Cl1 107.73(8) . . ? N1 Mn2 Cl2 110.97(6) . . ? O2' Mn2 Cl2 119.4(3) . . ? O2 Mn2 Cl2 97.46(8) . . ? Cl1 Mn2 Cl2 122.72(3) . . ? C8 P1 C2 102.05(9) . . ? C8 P1 C1 104.36(9) . . ? C2 P1 C1 104.68(9) . . ? C8 P1 Mn1 124.54(6) . . ? C2 P1 Mn1 123.39(7) . . ? C1 P1 Mn1 93.87(6) . . ? C14 P2 C20 101.18(9) . . ? C14 P2 C1 104.96(9) . . ? C20 P2 C1 106.06(9) . . ? C14 P2 Mn1 121.16(7) . . ? C20 P2 Mn1 126.53(6) . . ? C1 P2 Mn1 93.73(6) . . ? C27 P3 C33 102.12(9) . . ? C27 P3 C26 107.54(9) . . ? C33 P3 C26 103.86(9) . . ? C27 P3 Mn1 117.33(7) . . ? C33 P3 Mn1 128.47(6) . . ? C26 P3 Mn1 94.82(6) . . ? C39 P4 C45 101.93(9) . . ? C39 P4 C26 105.39(9) . . ? C45 P4 C26 105.36(9) . . ? C39 P4 Mn1 121.13(6) . . ? C45 P4 Mn1 125.15(6) . . ? C26 P4 Mn1 94.86(6) . . ? C52 N1 Mn2 155.4(2) . . ? P2 C1 P1 95.11(9) . . ? C3 C2 C7 118.7(2) . . ? C3 C2 P1 122.5(2) . . ? C7 C2 P1 118.8(2) . . ? C2 C3 C4 120.6(2) . . ? C5 C4 C3 120.1(2) . . ? C4 C5 C6 119.9(2) . . ? C5 C6 C7 120.2(2) . . ? C6 C7 C2 120.5(2) . . ? C13 C8 C9 118.6(2) . . ? C13 C8 P1 122.1(2) . . ? C9 C8 P1 119.28(15) . . ? C10 C9 C8 120.8(2) . . ? C9 C10 C11 120.2(2) . . ? C10 C11 C12 119.6(2) . . ? C11 C12 C13 120.1(2) . . ? C12 C13 C8 120.7(2) . . ? C15 C14 C19 118.7(2) . . ? C15 C14 P2 119.9(2) . . ? C19 C14 P2 121.4(2) . . ? C14 C15 C16 120.0(2) . . ? C17 C16 C15 120.6(2) . . ? C18 C17 C16 120.1(2) . . ? C17 C18 C19 120.0(2) . . ? C18 C19 C14 120.7(2) . . ? C21 C20 C25 118.4(2) . . ? C21 C20 P2 119.6(2) . . ? C25 C20 P2 121.71(15) . . ? C22 C21 C20 120.6(2) . . ? C23 C22 C21 120.3(2) . . ? C22 C23 C24 119.8(2) . . ? C23 C24 C25 120.1(2) . . ? C24 C25 C20 120.7(2) . . ? P3 C26 P4 95.32(9) . . ? C28 C27 C32 119.0(2) . . ? C28 C27 P3 119.0(2) . . ? C32 C27 P3 122.0(2) . . ? C29 C28 C27 120.6(2) . . ? C30 C29 C28 119.7(2) . . ? C31 C30 C29 120.2(2) . . ? C30 C31 C32 120.4(2) . . ? C31 C32 C27 120.0(2) . . ? C34 C33 C38 118.7(2) . . ? C34 C33 P3 120.2(2) . . ? C38 C33 P3 121.1(2) . . ? C35 C34 C33 120.4(2) . . ? C36 C35 C34 120.1(2) . . ? C37 C36 C35 120.2(2) . . ? C36 C37 C38 120.1(2) . . ? C37 C38 C33 120.4(2) . . ? C44 C39 C40 118.7(2) . . ? C44 C39 P4 119.3(2) . . ? C40 C39 P4 122.0(2) . . ? C41 C40 C39 120.5(2) . . ? C42 C41 C40 120.3(2) . . ? C41 C42 C43 119.9(2) . . ? C42 C43 C44 120.3(2) . . ? C43 C44 C39 120.4(2) . . ? C46 C45 C50 118.8(2) . . ? C46 C45 P4 119.32(14) . . ? C50 C45 P4 121.9(2) . . ? C47 C46 C45 120.8(2) . . ? C48 C47 C46 119.9(2) . . ? C47 C48 C49 119.8(2) . . ? C50 C49 C48 120.6(2) . . ? C49 C50 C45 120.1(2) . . ? O1 C51 Mn1 178.9(2) . . ? N1 C52 Mn1 179.8(2) . . ? C56 O2 C53 109.5(4) . . ? C56 O2 Mn2 122.7(4) . . ? C53 O2 Mn2 126.9(2) . . ? O2 C53 C54 106.7(4) . . ? C55 C54 C53 104.3(4) . . ? O2 C56 C55 104.7(5) . . ? C53' O2' C56' 105.6(10) . . ? C53' O2' Mn2 117.8(8) . . ? C56' O2' Mn2 121.7(8) . . ? O2' C53' C54' 102.7(12) . . ? C53' C54' C55 104.2(13) . . ? O2' C56' C55 111.2(9) . . ? C54 C55 C56 111.1(4) . . ? C56' C55 C54' 92.9(9) . . ? C60 O3 C57 103.4(6) . . ? C58 C57 O3 111.3(5) . . ? C59 C58 C57 108.2(7) . . ? C58 C59 C60 110.2(7) . . ? O3 C60 C59 100.7(7) . . ? C59' C58' C60' 58.8(36) . . ? C59' C58' C57' 108.0(56) . . ? C60' C58' C57' 99.7(26) . . ? C58' C59' C60' 95.2(45) . . ? O3 C60' C59' 95.7(36) . . ? O3 C60' C58' 94.3(30) . . ? C59' C60' C58' 26.1(21) . . ? _refine_diff_density_max 0.791 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.056 data_3.thf _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C60 H60 Cl2 Mn N Ni O3 P4' _chemical_formula_weight 1151.59 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Ni' 'Ni' 0.3393 1.1124 '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 13.3705(12) _cell_length_b 14.325(2) _cell_length_c 17.179(2) _cell_angle_alpha 111.382(7) _cell_angle_beta 106.904(6) _cell_angle_gamma 98.725(10) _cell_volume 2806.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 94 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 25.01 _exptl_crystal_description 'parallelepipeds' _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method ? _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 0.815 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.688 _exptl_absorpt_correction_T_max 0.941 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17900 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.52 _reflns_number_total 12277 _reflns_number_observed 10285 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0907P)^2^+6.2849P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12268 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_obs 0.0657 _refine_ls_wR_factor_all 0.1914 _refine_ls_wR_factor_obs 0.1656 _refine_ls_goodness_of_fit_all 1.142 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 1.145 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.60802(4) 0.22436(4) 0.13689(4) 0.03357(15) Uani 1 d . . Cl1 Cl 0.61802(14) 0.15606(10) 0.23524(10) 0.0616(4) Uani 1 d . . Cl2 Cl 0.46687(9) 0.22924(9) 0.03123(8) 0.0463(3) Uani 1 d . . Mn1 Mn 0.82670(4) 0.59984(4) 0.27163(3) 0.01803(13) Uani 1 d . . P1 P 0.65494(7) 0.61789(7) 0.22854(6) 0.0202(2) Uani 1 d . . P2 P 0.77958(7) 0.57689(7) 0.12508(6) 0.0197(2) Uani 1 d . . P3 P 0.87038(7) 0.61467(7) 0.41622(6) 0.0211(2) Uani 1 d . . P4 P 0.99096(7) 0.56623(7) 0.31075(6) 0.0204(2) Uani 1 d . . O1 O 0.9161(2) 0.8272(2) 0.3348(2) 0.0355(6) Uani 1 d . . O2 O 0.6770(3) 0.1430(3) 0.0543(3) 0.0497(8) Uani 1 d . . N1 N 0.7191(3) 0.3597(3) 0.1950(2) 0.0320(7) Uani 1 d . . C1 C 0.6349(3) 0.5734(3) 0.1073(2) 0.0236(7) Uani 1 d . . H1B H 0.5839(3) 0.5021(3) 0.0687(2) 0.028 Uiso 1 calc R . H1C H 0.6116(3) 0.6230(3) 0.0833(2) 0.028 Uiso 1 calc R . C2 C 0.5351(3) 0.5376(3) 0.2296(2) 0.0233(7) Uani 1 d . . C3 C 0.5495(3) 0.4763(3) 0.2761(3) 0.0329(8) Uani 1 d . . H3A H 0.6213(3) 0.4780(3) 0.3083(3) 0.039 Uiso 1 calc R . C4 C 0.4601(3) 0.4123(4) 0.2764(3) 0.0425(10) Uani 1 d . . H4A H 0.4708(3) 0.3697(4) 0.3076(3) 0.051 Uiso 1 calc R . C5 C 0.3554(3) 0.4113(4) 0.2305(3) 0.0411(10) Uani 1 d . . H5A H 0.2942(3) 0.3692(4) 0.2317(3) 0.049 Uiso 1 calc R . C6 C 0.3397(3) 0.4712(4) 0.1833(3) 0.0366(9) Uani 1 d . . H6A H 0.2677(3) 0.4690(4) 0.1512(3) 0.044 Uiso 1 calc R . C7 C 0.4284(3) 0.5347(3) 0.1823(3) 0.0302(8) Uani 1 d . . H7A H 0.4170(3) 0.5760(3) 0.1499(3) 0.036 Uiso 1 calc R . C8 C 0.6317(3) 0.7474(3) 0.2631(3) 0.0261(7) Uani 1 d . . C9 C 0.6016(4) 0.7854(3) 0.3378(3) 0.0384(9) Uani 1 d . . H9A H 0.5914(4) 0.7438(3) 0.3687(3) 0.046 Uiso 1 calc R . C10 C 0.5866(4) 0.8847(4) 0.3664(4) 0.0542(13) Uani 1 d . . H10A H 0.5677(4) 0.9114(4) 0.4178(4) 0.065 Uiso 1 calc R . C11 C 0.5990(4) 0.9451(4) 0.3203(4) 0.0517(12) Uani 1 d . . H11A H 0.5854(4) 1.0115(4) 0.3386(4) 0.062 Uiso 1 calc R . C12 C 0.6310(4) 0.9086(4) 0.2482(4) 0.0497(12) Uani 1 d . . H12A H 0.6424(4) 0.9509(4) 0.2181(4) 0.060 Uiso 1 calc R . C13 C 0.6469(4) 0.8091(3) 0.2192(3) 0.0398(9) Uani 1 d . . H13A H 0.6682(4) 0.7837(3) 0.1690(3) 0.048 Uiso 1 calc R . C14 C 0.8404(3) 0.6861(3) 0.1062(2) 0.0237(7) Uani 1 d . . C15 C 0.7787(3) 0.7190(3) 0.0453(3) 0.0300(8) Uani 1 d . . H15A H 0.7038(3) 0.6820(3) 0.0102(3) 0.036 Uiso 1 calc R . C16 C 0.8271(4) 0.8054(4) 0.0363(3) 0.0395(10) Uani 1 d . . H16A H 0.7846(4) 0.8278(4) -0.0044(3) 0.047 Uiso 1 calc R . C17 C 0.9368(4) 0.8593(3) 0.0861(3) 0.0426(10) Uani 1 d . . H17A H 0.9688(4) 0.9192(3) 0.0806(3) 0.051 Uiso 1 calc R . C18 C 1.0001(3) 0.8251(3) 0.1446(3) 0.0366(9) Uani 1 d . . H18A H 1.0758(3) 0.8601(3) 0.1772(3) 0.044 Uiso 1 calc R . C19 C 0.9512(3) 0.7392(3) 0.1546(3) 0.0290(7) Uani 1 d . . H19A H 0.9940(3) 0.7166(3) 0.1949(3) 0.035 Uiso 1 calc R . C20 C 0.7701(3) 0.4626(3) 0.0256(2) 0.0249(7) Uani 1 d . . C21 C 0.6932(3) 0.3666(3) -0.0055(3) 0.0310(8) Uani 1 d . . H21A H 0.6455(3) 0.3604(3) 0.0250(3) 0.037 Uiso 1 calc R . C22 C 0.6856(4) 0.2804(3) -0.0804(3) 0.0417(10) Uani 1 d . . H22A H 0.6317(4) 0.2160(3) -0.1018(3) 0.050 Uiso 1 calc R . C23 C 0.7574(4) 0.2880(4) -0.1246(3) 0.0451(11) Uani 1 d . . H23A H 0.7525(4) 0.2288(4) -0.1758(3) 0.054 Uiso 1 calc R . C24 C 0.8350(4) 0.3815(4) -0.0933(3) 0.0416(10) Uani 1 d . . H24A H 0.8846(4) 0.3865(4) -0.1226(3) 0.050 Uiso 1 calc R . C25 C 0.8415(3) 0.4688(3) -0.0194(3) 0.0305(8) Uani 1 d . . H25A H 0.8947(3) 0.5332(3) 0.0010(3) 0.037 Uiso 1 calc R . C26 C 0.9809(3) 0.5519(3) 0.4120(2) 0.0255(7) Uani 1 d . . H26A H 0.9586(3) 0.4778(3) 0.4013(2) 0.031 Uiso 1 calc R . H26B H 1.0489(3) 0.5910(3) 0.4662(2) 0.031 Uiso 1 calc R . C27 C 0.7864(3) 0.5468(3) 0.4581(2) 0.0258(7) Uani 1 d . . C28 C 0.7373(3) 0.6017(3) 0.5141(3) 0.0344(8) Uani 1 d . . H28A H 0.7513(3) 0.6752(3) 0.5335(3) 0.041 Uiso 1 calc R . C29 C 0.6679(4) 0.5498(4) 0.5419(3) 0.0445(11) Uani 1 d . . H29A H 0.6348(4) 0.5883(4) 0.5798(3) 0.053 Uiso 1 calc R . C30 C 0.6469(4) 0.4432(4) 0.5148(3) 0.0423(10) Uani 1 d . . H30A H 0.6009(4) 0.4086(4) 0.5351(3) 0.051 Uiso 1 calc R . C31 C 0.6931(3) 0.3870(4) 0.4579(3) 0.0391(10) Uani 1 d . . H31A H 0.6779(3) 0.3134(4) 0.4384(3) 0.047 Uiso 1 calc R . C32 C 0.7616(3) 0.4376(3) 0.4292(3) 0.0300(8) Uani 1 d . . H32A H 0.7921(3) 0.3980(3) 0.3895(3) 0.036 Uiso 1 calc R . C33 C 0.9352(3) 0.7426(3) 0.5132(2) 0.0263(7) Uani 1 d . . C34 C 1.0254(4) 0.7598(3) 0.5882(3) 0.0363(9) Uani 1 d . . H34A H 1.0524(4) 0.7028(3) 0.5903(3) 0.044 Uiso 1 calc R . C35 C 1.0767(4) 0.8587(4) 0.6599(3) 0.0478(12) Uani 1 d . . H35A H 1.1380(4) 0.8688(4) 0.7103(3) 0.057 Uiso 1 calc R . C36 C 1.0379(5) 0.9425(4) 0.6573(3) 0.0517(13) Uani 1 d . . H36A H 1.0738(5) 1.0105(4) 0.7054(3) 0.062 Uiso 1 calc R . C37 C 0.9466(4) 0.9269(4) 0.5845(3) 0.0456(11) Uani 1 d . . H37A H 0.9190(4) 0.9840(4) 0.5837(3) 0.055 Uiso 1 calc R . C38 C 0.8952(3) 0.8277(3) 0.5125(3) 0.0342(8) Uani 1 d . . H38A H 0.8330(3) 0.8176(3) 0.4628(3) 0.041 Uiso 1 calc R . C39 C 1.0195(3) 0.4467(3) 0.2467(2) 0.0245(7) Uani 1 d . . C40 C 1.0022(3) 0.4187(3) 0.1563(3) 0.0298(8) Uani 1 d . . H40A H 0.9731(3) 0.4602(3) 0.1286(3) 0.036 Uiso 1 calc R . C41 C 1.0267(3) 0.3309(3) 0.1058(3) 0.0359(9) Uani 1 d . . H41A H 1.0156(3) 0.3131(3) 0.0444(3) 0.043 Uiso 1 calc R . C42 C 1.0678(3) 0.2690(3) 0.1469(3) 0.0352(9) Uani 1 d . . H42A H 1.0843(3) 0.2085(3) 0.1132(3) 0.042 Uiso 1 calc R . C43 C 1.0844(3) 0.2959(3) 0.2365(3) 0.0366(9) Uani 1 d . . H43A H 1.1113(3) 0.2532(3) 0.2638(3) 0.044 Uiso 1 calc R . C44 C 1.0619(3) 0.3854(3) 0.2873(3) 0.0318(8) Uani 1 d . . H44A H 1.0754(3) 0.4045(3) 0.3493(3) 0.038 Uiso 1 calc R . C45 C 1.1221(3) 0.6661(3) 0.3537(2) 0.0264(7) Uani 1 d . . C46 C 1.2062(3) 0.6460(3) 0.3233(3) 0.0344(8) Uani 1 d . . H46A H 1.1975(3) 0.5781(3) 0.2799(3) 0.041 Uiso 1 calc R . C47 C 1.3033(4) 0.7258(4) 0.3570(4) 0.0468(11) Uani 1 d . . H47A H 1.3597(4) 0.7118(4) 0.3354(4) 0.056 Uiso 1 calc R . C48 C 1.3182(4) 0.8236(4) 0.4205(4) 0.0516(13) Uani 1 d . . H48A H 1.3844(4) 0.8771(4) 0.4427(4) 0.062 Uiso 1 calc R . C49 C 1.2354(4) 0.8443(4) 0.4525(4) 0.0477(11) Uani 1 d . . H49A H 1.2457(4) 0.9117(4) 0.4976(4) 0.057 Uiso 1 calc R . C50 C 1.1382(3) 0.7664(3) 0.4185(3) 0.0363(9) Uani 1 d . . H50A H 1.0816(3) 0.7815(3) 0.4396(3) 0.044 Uiso 1 calc R . C51 C 0.8826(3) 0.7381(3) 0.3111(2) 0.0243(7) Uani 1 d . . C52 C 0.7609(3) 0.4489(3) 0.2248(2) 0.0237(7) Uani 1 d . . C53 C 0.6203(5) 0.0420(4) -0.0213(4) 0.061(2) Uani 1 d . . H53A H 0.5564(5) 0.0466(4) -0.0652(4) 0.074 Uiso 1 calc R . H53B H 0.5944(5) -0.0097(4) -0.0007(4) 0.074 Uiso 1 calc R . C54 C 0.6998(6) 0.0105(5) -0.0635(6) 0.084(2) Uani 1 d . . H54A H 0.6923(6) -0.0652(5) -0.0824(6) 0.100 Uiso 1 calc R . H54B H 0.6890(6) 0.0255(5) -0.1168(6) 0.100 Uiso 1 calc R . C55 C 0.8075(6) 0.0744(6) 0.0081(7) 0.108(3) Uani 1 d . . H55A H 0.8515(6) 0.1116(6) -0.0149(7) 0.130 Uiso 1 calc R . H55B H 0.8472(6) 0.0288(6) 0.0276(7) 0.130 Uiso 1 calc R . C56 C 0.7907(5) 0.1528(7) 0.0872(5) 0.077(2) Uani 1 d . . H56A H 0.8113(5) 0.1359(7) 0.1396(5) 0.093 Uiso 1 calc R . H56B H 0.8347(5) 0.2248(7) 0.1053(5) 0.093 Uiso 1 calc R . O3 O 0.6044(8) -0.0793(8) -0.4017(7) 0.171(4) Uani 1 d . . C57 C 0.5826(13) -0.1740(10) -0.3927(16) 0.195(9) Uani 1 d . . H57A H 0.5756(13) -0.2327(10) -0.4489(16) 0.234 Uiso 1 calc R . H57B H 0.5119(13) -0.1860(10) -0.3851(16) 0.234 Uiso 1 calc R . C58 C 0.7547(9) -0.0820(8) -0.2831(8) 0.119(4) Uani 1 d . . H58A H 0.8128(9) -0.0980(8) -0.3062(8) 0.142 Uiso 1 calc R . H58B H 0.7873(9) -0.0470(8) -0.2163(8) 0.142 Uiso 1 calc R . C59 C 0.6702(15) -0.1741(9) -0.3139(9) 0.150(6) Uani 1 d . . H59A H 0.6426(15) -0.1727(9) -0.2660(9) 0.180 Uiso 1 calc R . H59B H 0.6960(15) -0.2369(9) -0.3333(9) 0.180 Uiso 1 calc R . C60 C 0.7006(12) -0.0141(9) -0.3197(12) 0.176(7) Uani 1 d . . H60A H 0.6787(12) 0.0342(9) -0.2740(12) 0.211 Uiso 1 calc R . H60B H 0.7527(12) 0.0284(9) -0.3333(12) 0.211 Uiso 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 Ni1 0.0275(3) 0.0223(2) 0.0466(3) 0.0142(2) 0.0097(2) 0.0060(2) Cl1 0.0861(10) 0.0391(6) 0.0580(8) 0.0308(6) 0.0148(7) 0.0128(6) Cl2 0.0300(5) 0.0484(6) 0.0544(7) 0.0227(5) 0.0061(5) 0.0129(4) Mn1 0.0143(2) 0.0188(2) 0.0202(2) 0.0091(2) 0.0038(2) 0.0064(2) P1 0.0155(4) 0.0232(4) 0.0229(4) 0.0111(3) 0.0056(3) 0.0084(3) P2 0.0165(4) 0.0224(4) 0.0203(4) 0.0103(3) 0.0048(3) 0.0080(3) P3 0.0183(4) 0.0236(4) 0.0219(4) 0.0113(3) 0.0049(3) 0.0084(3) P4 0.0152(4) 0.0238(4) 0.0232(4) 0.0118(3) 0.0050(3) 0.0081(3) O1 0.040(2) 0.0234(13) 0.038(2) 0.0129(12) 0.0100(13) 0.0055(11) O2 0.029(2) 0.044(2) 0.062(2) 0.010(2) 0.0148(15) 0.0110(13) N1 0.029(2) 0.026(2) 0.038(2) 0.0147(14) 0.0083(14) 0.0061(13) C1 0.0177(15) 0.033(2) 0.022(2) 0.0136(14) 0.0054(13) 0.0109(13) C2 0.0171(15) 0.028(2) 0.026(2) 0.0119(14) 0.0080(13) 0.0095(13) C3 0.022(2) 0.047(2) 0.034(2) 0.024(2) 0.0068(15) 0.011(2) C4 0.029(2) 0.060(3) 0.052(3) 0.039(2) 0.015(2) 0.011(2) C5 0.022(2) 0.059(3) 0.045(2) 0.028(2) 0.012(2) 0.005(2) C6 0.016(2) 0.051(2) 0.043(2) 0.023(2) 0.008(2) 0.011(2) C7 0.023(2) 0.036(2) 0.036(2) 0.021(2) 0.0073(15) 0.0150(15) C8 0.019(2) 0.028(2) 0.030(2) 0.0120(15) 0.0066(14) 0.0124(13) C9 0.043(2) 0.032(2) 0.038(2) 0.009(2) 0.020(2) 0.013(2) C10 0.056(3) 0.037(2) 0.061(3) 0.004(2) 0.031(3) 0.014(2) C11 0.053(3) 0.029(2) 0.065(3) 0.011(2) 0.018(2) 0.021(2) C12 0.058(3) 0.030(2) 0.061(3) 0.022(2) 0.016(2) 0.020(2) C13 0.050(3) 0.032(2) 0.044(2) 0.020(2) 0.019(2) 0.022(2) C14 0.027(2) 0.024(2) 0.027(2) 0.0135(14) 0.0135(14) 0.0113(13) C15 0.030(2) 0.034(2) 0.034(2) 0.021(2) 0.014(2) 0.014(2) C16 0.049(2) 0.042(2) 0.050(3) 0.033(2) 0.026(2) 0.025(2) C17 0.053(3) 0.034(2) 0.057(3) 0.026(2) 0.033(2) 0.015(2) C18 0.031(2) 0.032(2) 0.046(2) 0.014(2) 0.019(2) 0.004(2) C19 0.028(2) 0.029(2) 0.031(2) 0.013(2) 0.0123(15) 0.0094(14) C20 0.025(2) 0.027(2) 0.023(2) 0.0131(14) 0.0055(13) 0.0120(13) C21 0.032(2) 0.028(2) 0.029(2) 0.012(2) 0.006(2) 0.0092(15) C22 0.049(3) 0.029(2) 0.035(2) 0.009(2) 0.005(2) 0.011(2) C23 0.065(3) 0.035(2) 0.033(2) 0.007(2) 0.019(2) 0.027(2) C24 0.051(3) 0.046(2) 0.033(2) 0.014(2) 0.021(2) 0.026(2) C25 0.033(2) 0.035(2) 0.028(2) 0.015(2) 0.012(2) 0.016(2) C26 0.026(2) 0.032(2) 0.027(2) 0.0183(15) 0.0112(14) 0.0139(14) C27 0.018(2) 0.037(2) 0.024(2) 0.0179(15) 0.0053(13) 0.0081(14) C28 0.033(2) 0.041(2) 0.029(2) 0.013(2) 0.014(2) 0.011(2) C29 0.037(2) 0.060(3) 0.040(2) 0.021(2) 0.022(2) 0.012(2) C30 0.031(2) 0.059(3) 0.045(2) 0.032(2) 0.015(2) 0.007(2) C31 0.029(2) 0.042(2) 0.048(2) 0.030(2) 0.006(2) 0.006(2) C32 0.023(2) 0.033(2) 0.036(2) 0.020(2) 0.0055(15) 0.0097(14) C33 0.028(2) 0.024(2) 0.024(2) 0.0089(14) 0.0085(14) 0.0056(13) C34 0.040(2) 0.035(2) 0.027(2) 0.015(2) 0.003(2) 0.008(2) C35 0.052(3) 0.041(2) 0.029(2) 0.012(2) -0.005(2) 0.001(2) C36 0.064(3) 0.034(2) 0.032(2) 0.004(2) 0.006(2) 0.001(2) C37 0.057(3) 0.033(2) 0.039(2) 0.010(2) 0.013(2) 0.015(2) C38 0.035(2) 0.033(2) 0.034(2) 0.014(2) 0.011(2) 0.014(2) C39 0.0173(15) 0.029(2) 0.028(2) 0.0132(14) 0.0082(13) 0.0097(13) C40 0.027(2) 0.034(2) 0.030(2) 0.016(2) 0.0078(15) 0.0135(15) C41 0.030(2) 0.043(2) 0.033(2) 0.014(2) 0.012(2) 0.015(2) C42 0.027(2) 0.036(2) 0.044(2) 0.013(2) 0.016(2) 0.015(2) C43 0.037(2) 0.038(2) 0.047(2) 0.024(2) 0.019(2) 0.024(2) C44 0.030(2) 0.041(2) 0.035(2) 0.021(2) 0.014(2) 0.021(2) C45 0.018(2) 0.032(2) 0.027(2) 0.0151(15) 0.0042(13) 0.0062(13) C46 0.020(2) 0.042(2) 0.040(2) 0.018(2) 0.011(2) 0.006(2) C47 0.025(2) 0.057(3) 0.057(3) 0.025(2) 0.016(2) 0.004(2) C48 0.025(2) 0.051(3) 0.065(3) 0.025(3) 0.008(2) -0.007(2) C49 0.034(2) 0.036(2) 0.051(3) 0.010(2) 0.004(2) -0.002(2) C50 0.025(2) 0.035(2) 0.041(2) 0.013(2) 0.007(2) 0.005(2) C51 0.023(2) 0.025(2) 0.025(2) 0.0126(14) 0.0049(13) 0.0082(13) C52 0.0191(15) 0.029(2) 0.026(2) 0.0147(14) 0.0069(13) 0.0100(13) C53 0.048(3) 0.044(3) 0.072(4) 0.002(3) 0.027(3) 0.007(2) C54 0.079(5) 0.058(4) 0.121(6) 0.026(4) 0.059(5) 0.028(3) C55 0.056(4) 0.069(5) 0.164(9) 0.010(5) 0.042(5) 0.026(3) C56 0.033(3) 0.114(6) 0.078(4) 0.033(4) 0.017(3) 0.035(3) O3 0.145(8) 0.140(8) 0.157(8) 0.041(6) 0.014(6) -0.009(6) C57 0.138(12) 0.074(7) 0.335(27) 0.047(12) 0.108(15) 0.000(7) C58 0.110(7) 0.107(7) 0.131(9) 0.057(7) 0.044(6) -0.002(6) C59 0.233(17) 0.079(7) 0.150(11) 0.057(7) 0.097(11) 0.006(9) C60 0.153(12) 0.085(7) 0.244(18) 0.069(10) 0.037(12) -0.007(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.953(3) . ? Ni1 O2 2.026(3) . ? Ni1 Cl1 2.2232(14) . ? Ni1 Cl2 2.2365(12) . ? Mn1 C51 1.794(4) . ? Mn1 C52 1.959(4) . ? Mn1 P4 2.2815(9) . ? Mn1 P1 2.2848(9) . ? Mn1 P2 2.2924(10) . ? Mn1 P3 2.3000(10) . ? P1 C2 1.835(4) . ? P1 C8 1.836(4) . ? P1 C1 1.863(4) . ? P2 C14 1.831(4) . ? P2 C20 1.841(4) . ? P2 C1 1.858(3) . ? P3 C33 1.827(4) . ? P3 C27 1.836(4) . ? P3 C26 1.849(4) . ? P4 C39 1.832(4) . ? P4 C45 1.839(4) . ? P4 C26 1.863(4) . ? O1 C51 1.155(4) . ? O2 C56 1.424(6) . ? O2 C53 1.441(6) . ? N1 C52 1.162(5) . ? C2 C3 1.385(5) . ? C2 C7 1.408(5) . ? C3 C4 1.393(6) . ? C4 C5 1.388(6) . ? C5 C6 1.379(6) . ? C6 C7 1.388(6) . ? C8 C13 1.382(6) . ? C8 C9 1.401(6) . ? C9 C10 1.392(6) . ? C10 C11 1.392(8) . ? C11 C12 1.377(8) . ? C12 C13 1.400(6) . ? C14 C19 1.395(5) . ? C14 C15 1.404(5) . ? C15 C16 1.390(6) . ? C16 C17 1.387(7) . ? C17 C18 1.397(7) . ? C18 C19 1.396(5) . ? C20 C21 1.396(5) . ? C20 C25 1.402(5) . ? C21 C22 1.385(6) . ? C22 C23 1.400(7) . ? C23 C24 1.376(7) . ? C24 C25 1.389(6) . ? C27 C28 1.396(5) . ? C27 C32 1.408(5) . ? C28 C29 1.397(6) . ? C29 C30 1.380(7) . ? C30 C31 1.383(7) . ? C31 C32 1.389(6) . ? C33 C34 1.396(5) . ? C33 C38 1.405(5) . ? C34 C35 1.391(6) . ? C35 C36 1.388(8) . ? C36 C37 1.389(7) . ? C37 C38 1.397(6) . ? C39 C40 1.390(5) . ? C39 C44 1.395(5) . ? C40 C41 1.392(6) . ? C41 C42 1.401(6) . ? C42 C43 1.382(6) . ? C43 C44 1.396(6) . ? C45 C46 1.396(5) . ? C45 C50 1.397(6) . ? C46 C47 1.400(6) . ? C47 C48 1.366(8) . ? C48 C49 1.398(7) . ? C49 C50 1.384(6) . ? C53 C54 1.489(8) . ? C54 C55 1.474(11) . ? C55 C56 1.516(11) . ? O3 C57 1.42(2) . ? O3 C60 1.46(2) . ? C57 C59 1.51(2) . ? C58 C59 1.410(14) . ? C58 C60 1.50(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 O2 97.90(14) . . ? N1 Ni1 Cl1 109.34(11) . . ? O2 Ni1 Cl1 104.92(12) . . ? N1 Ni1 Cl2 108.00(11) . . ? O2 Ni1 Cl2 97.83(11) . . ? Cl1 Ni1 Cl2 132.54(6) . . ? C51 Mn1 C52 177.72(14) . . ? C51 Mn1 P4 95.72(11) . . ? C52 Mn1 P4 86.18(10) . . ? C51 Mn1 P1 89.44(11) . . ? C52 Mn1 P1 88.66(10) . . ? P4 Mn1 P1 174.83(4) . . ? C51 Mn1 P2 90.42(12) . . ? C52 Mn1 P2 87.84(11) . . ? P4 Mn1 P2 106.49(4) . . ? P1 Mn1 P2 73.73(3) . . ? C51 Mn1 P3 92.23(12) . . ? C52 Mn1 P3 89.51(11) . . ? P4 Mn1 P3 73.33(3) . . ? P1 Mn1 P3 106.20(4) . . ? P2 Mn1 P3 177.35(4) . . ? C2 P1 C8 102.2(2) . . ? C2 P1 C1 105.6(2) . . ? C8 P1 C1 105.0(2) . . ? C2 P1 Mn1 124.68(12) . . ? C8 P1 Mn1 121.42(12) . . ? C1 P1 Mn1 94.79(11) . . ? C14 P2 C20 102.0(2) . . ? C14 P2 C1 107.6(2) . . ? C20 P2 C1 103.9(2) . . ? C14 P2 Mn1 117.13(12) . . ? C20 P2 Mn1 128.84(12) . . ? C1 P2 Mn1 94.67(11) . . ? C33 P3 C27 101.1(2) . . ? C33 P3 C26 105.2(2) . . ? C27 P3 C26 105.3(2) . . ? C33 P3 Mn1 120.72(12) . . ? C27 P3 Mn1 127.31(12) . . ? C26 P3 Mn1 93.87(12) . . ? C39 P4 C45 102.1(2) . . ? C39 P4 C26 104.8(2) . . ? C45 P4 C26 104.8(2) . . ? C39 P4 Mn1 124.64(12) . . ? C45 P4 Mn1 122.82(12) . . ? C26 P4 Mn1 94.09(11) . . ? C56 O2 C53 109.3(4) . . ? C56 O2 Ni1 120.7(4) . . ? C53 O2 Ni1 124.0(3) . . ? C52 N1 Ni1 162.0(3) . . ? P2 C1 P1 95.1(2) . . ? C3 C2 C7 119.1(3) . . ? C3 C2 P1 119.5(3) . . ? C7 C2 P1 121.5(3) . . ? C2 C3 C4 120.9(4) . . ? C5 C4 C3 119.4(4) . . ? C6 C5 C4 120.3(4) . . ? C5 C6 C7 120.6(4) . . ? C6 C7 C2 119.7(4) . . ? C13 C8 C9 119.7(4) . . ? C13 C8 P1 121.5(3) . . ? C9 C8 P1 118.7(3) . . ? C10 C9 C8 119.4(4) . . ? C11 C10 C9 120.6(5) . . ? C12 C11 C10 119.8(4) . . ? C11 C12 C13 120.0(5) . . ? C8 C13 C12 120.4(4) . . ? C19 C14 C15 118.9(3) . . ? C19 C14 P2 119.0(3) . . ? C15 C14 P2 122.1(3) . . ? C16 C15 C14 120.1(4) . . ? C17 C16 C15 120.6(4) . . ? C16 C17 C18 119.9(4) . . ? C19 C18 C17 119.5(4) . . ? C14 C19 C18 120.9(4) . . ? C21 C20 C25 118.3(4) . . ? C21 C20 P2 120.5(3) . . ? C25 C20 P2 121.1(3) . . ? C22 C21 C20 120.8(4) . . ? C21 C22 C23 120.0(4) . . ? C24 C23 C22 119.6(4) . . ? C23 C24 C25 120.5(4) . . ? C24 C25 C20 120.7(4) . . ? P3 C26 P4 95.0(2) . . ? C28 C27 C32 117.8(3) . . ? C28 C27 P3 120.1(3) . . ? C32 C27 P3 121.8(3) . . ? C27 C28 C29 120.7(4) . . ? C30 C29 C28 120.6(4) . . ? C29 C30 C31 119.6(4) . . ? C30 C31 C32 120.4(4) . . ? C31 C32 C27 120.9(4) . . ? C34 C33 C38 118.3(4) . . ? C34 C33 P3 122.1(3) . . ? C38 C33 P3 119.6(3) . . ? C35 C34 C33 121.5(4) . . ? C36 C35 C34 119.6(4) . . ? C35 C36 C37 120.0(4) . . ? C36 C37 C38 120.3(4) . . ? C37 C38 C33 120.3(4) . . ? C40 C39 C44 119.3(3) . . ? C40 C39 P4 119.1(3) . . ? C44 C39 P4 121.5(3) . . ? C39 C40 C41 121.2(4) . . ? C40 C41 C42 119.0(4) . . ? C43 C42 C41 120.1(4) . . ? C42 C43 C44 120.5(4) . . ? C39 C44 C43 119.8(4) . . ? C46 C45 C50 118.4(4) . . ? C46 C45 P4 122.5(3) . . ? C50 C45 P4 119.0(3) . . ? C45 C46 C47 120.0(4) . . ? C48 C47 C46 121.0(4) . . ? C47 C48 C49 119.6(4) . . ? C50 C49 C48 119.9(5) . . ? C49 C50 C45 121.1(4) . . ? O1 C51 Mn1 178.2(3) . . ? N1 C52 Mn1 177.8(3) . . ? O2 C53 C54 106.7(5) . . ? C55 C54 C53 104.4(6) . . ? C54 C55 C56 108.7(6) . . ? O2 C56 C55 104.3(5) . . ? C57 O3 C60 101.5(12) . . ? O3 C57 C59 113.2(11) . . ? C59 C58 C60 104.9(11) . . ? C58 C59 C57 104.3(10) . . ? O3 C60 C58 110.0(10) . . ? _refine_diff_density_max 1.686 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.127 #=END data_11 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C104 H88 Cl2 Co Mn2 N2 O2 P8' _chemical_formula_weight 1885.38 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.332(3) _cell_length_b 11.742(2) _cell_length_c 37.409(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.516(15) _cell_angle_gamma 90.00 _cell_volume 9360.9(24) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 77 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 25.00 _exptl_crystal_description plates _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method ? _exptl_crystal_F_000 4136 _exptl_absorpt_coefficient_mu 0.915 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 0.867 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21388 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8178 _reflns_number_observed 7013 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+22.9185P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00015(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8171 _refine_ls_number_parameters 547 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_obs 0.0383 _refine_ls_wR_factor_all 0.0878 _refine_ls_wR_factor_obs 0.0786 _refine_ls_goodness_of_fit_all 1.167 _refine_ls_goodness_of_fit_obs 1.140 _refine_ls_restrained_S_all 1.174 _refine_ls_restrained_S_obs 1.140 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.5000 0.89770(4) 0.2500 0.02224(12) Uani 1 d S . Cl1 Cl 0.58592(3) 1.01228(6) 0.24963(2) 0.0373(2) Uani 1 d . . Mn1 Mn 0.44662(2) 0.71220(3) 0.128994(10) 0.01862(10) Uani 1 d . . P1 P 0.34764(3) 0.78302(6) 0.13710(2) 0.02035(15) Uani 1 d . . P2 P 0.44471(3) 0.90017(6) 0.11221(2) 0.02025(15) Uani 1 d . . P3 P 0.44365(3) 0.52907(6) 0.14886(2) 0.0231(2) Uani 1 d . . P4 P 0.54511(3) 0.64268(6) 0.12387(2) 0.0226(2) Uani 1 d . . C1 C 0.37553(12) 0.9329(2) 0.13822(7) 0.0225(5) Uani 1 d . . H1A H 0.34658(12) 0.9851(2) 0.12606(7) 0.027 Uiso 1 calc R . H1B H 0.38639(12) 0.9597(2) 0.16222(7) 0.027 Uiso 1 calc R . C2 C 0.29963(12) 0.7607(2) 0.17591(7) 0.0254(6) Uani 1 d . . C3 C 0.31248(15) 0.8183(3) 0.20780(8) 0.0417(8) Uani 1 d . . H3A H 0.34320(15) 0.8745(3) 0.20893(8) 0.050 Uiso 1 calc R . C4 C 0.2797(2) 0.7923(4) 0.23806(9) 0.0554(10) Uani 1 d . . H4A H 0.2885(2) 0.8314(4) 0.25931(9) 0.066 Uiso 1 calc R . C5 C 0.2341(2) 0.7086(3) 0.23669(8) 0.0466(9) Uani 1 d . . H5A H 0.2125(2) 0.6909(3) 0.25705(8) 0.056 Uiso 1 calc R . C6 C 0.22056(14) 0.6516(3) 0.20527(8) 0.0381(7) Uani 1 d . . H6A H 0.18955(14) 0.5959(3) 0.20426(8) 0.046 Uiso 1 calc R . C7 C 0.25351(13) 0.6774(3) 0.17473(8) 0.0333(7) Uani 1 d . . H7A H 0.24438(13) 0.6384(3) 0.15350(8) 0.040 Uiso 1 calc R . C8 C 0.28628(12) 0.7863(2) 0.10084(7) 0.0238(6) Uani 1 d . . C9 C 0.28220(12) 0.7042(2) 0.07397(7) 0.0280(6) Uani 1 d . . H9A H 0.30967(12) 0.6427(2) 0.07465(7) 0.034 Uiso 1 calc R . C10 C 0.23691(13) 0.7141(3) 0.04597(8) 0.0359(7) Uani 1 d . . H10A H 0.23466(13) 0.6593(3) 0.02801(8) 0.043 Uiso 1 calc R . C11 C 0.19567(14) 0.8042(3) 0.04478(8) 0.0392(7) Uani 1 d . . H11A H 0.16608(14) 0.8109(3) 0.02590(8) 0.047 Uiso 1 calc R . C12 C 0.19840(15) 0.8852(3) 0.07194(9) 0.0407(8) Uani 1 d . . H12A H 0.17039(15) 0.9459(3) 0.07137(9) 0.049 Uiso 1 calc R . C13 C 0.24289(13) 0.8751(3) 0.09980(8) 0.0336(7) Uani 1 d . . H13A H 0.24388(13) 0.9286(3) 0.11815(8) 0.040 Uiso 1 calc R . C14 C 0.42114(13) 0.9259(2) 0.06505(7) 0.0247(6) Uani 1 d . . C15 C 0.36721(14) 0.9858(2) 0.05425(7) 0.0300(6) Uani 1 d . . H15A H 0.34190(14) 1.0166(2) 0.07140(7) 0.036 Uiso 1 calc R . C16 C 0.35067(15) 1.0000(3) 0.01796(8) 0.0387(7) Uani 1 d . . H16A H 0.31445(15) 1.0397(3) 0.01099(8) 0.046 Uiso 1 calc R . C17 C 0.3885(2) 0.9547(3) -0.00748(8) 0.0407(8) Uani 1 d . . H17A H 0.3780(2) 0.9652(3) -0.03165(8) 0.049 Uiso 1 calc R . C18 C 0.4417(2) 0.8939(3) 0.00264(8) 0.0387(7) Uani 1 d . . H18A H 0.4668(2) 0.8633(3) -0.01466(8) 0.046 Uiso 1 calc R . C19 C 0.45781(14) 0.8785(2) 0.03888(7) 0.0312(6) Uani 1 d . . H19A H 0.49326(14) 0.8363(2) 0.04564(7) 0.037 Uiso 1 calc R . C20 C 0.50070(12) 1.0169(2) 0.12217(7) 0.0224(5) Uani 1 d . . C21 C 0.53920(14) 1.0580(3) 0.09591(8) 0.0358(7) Uani 1 d . . H21A H 0.53505(14) 1.0291(3) 0.07279(8) 0.043 Uiso 1 calc R . C22 C 0.58347(15) 1.1414(3) 0.10379(9) 0.0427(8) Uani 1 d . . H22A H 0.60856(15) 1.1681(3) 0.08588(9) 0.051 Uiso 1 calc R . C23 C 0.59087(14) 1.1856(3) 0.13801(8) 0.0354(7) Uani 1 d . . H23A H 0.62067(14) 1.2417(3) 0.14321(8) 0.042 Uiso 1 calc R . C24 C 0.55310(14) 1.1449(2) 0.16445(8) 0.0348(7) Uani 1 d . . H24A H 0.55779(14) 1.1736(2) 0.18758(8) 0.042 Uiso 1 calc R . C25 C 0.50851(14) 1.0618(2) 0.15669(7) 0.0300(6) Uani 1 d . . H25A H 0.48344(14) 1.0355(2) 0.17467(7) 0.036 Uiso 1 calc R . C26 C 0.52941(13) 0.5045(2) 0.14601(7) 0.0278(6) Uani 1 d . . H26A H 0.55080(13) 0.4977(2) 0.16934(7) 0.033 Uiso 1 calc R . H26B H 0.53897(13) 0.4395(2) 0.13123(7) 0.033 Uiso 1 calc R . C27 C 0.40279(13) 0.4232(2) 0.11999(7) 0.0270(6) Uani 1 d . . C28 C 0.4314(2) 0.3312(3) 0.10386(9) 0.0393(7) Uani 1 d . . H28A H 0.4740(2) 0.3180(3) 0.10823(9) 0.047 Uiso 1 calc R . C29 C 0.3965(2) 0.2589(3) 0.08122(9) 0.0456(8) Uani 1 d . . H29A H 0.4161(2) 0.1982(3) 0.07032(9) 0.055 Uiso 1 calc R . C30 C 0.3329(2) 0.2766(3) 0.07476(9) 0.0427(8) Uani 1 d . . H30A H 0.3098(2) 0.2282(3) 0.05954(9) 0.051 Uiso 1 calc R . C31 C 0.3040(2) 0.3666(3) 0.09112(9) 0.0421(8) Uani 1 d . . H31A H 0.2612(2) 0.3784(3) 0.08716(9) 0.051 Uiso 1 calc R . C32 C 0.33866(14) 0.4395(2) 0.11342(8) 0.0339(7) Uani 1 d . . H32A H 0.31877(14) 0.5002(2) 0.12416(8) 0.041 Uiso 1 calc R . C33 C 0.42376(13) 0.4780(2) 0.19326(7) 0.0288(6) Uani 1 d . . C34 C 0.4311(2) 0.3636(3) 0.20244(9) 0.0445(8) Uani 1 d . . H34A H 0.4463(2) 0.3125(3) 0.18591(9) 0.053 Uiso 1 calc R . C35 C 0.4158(2) 0.3254(3) 0.23602(9) 0.0545(10) Uani 1 d . . H35A H 0.4210(2) 0.2490(3) 0.24197(9) 0.065 Uiso 1 calc R . C36 C 0.3929(2) 0.4002(3) 0.26057(9) 0.0492(9) Uani 1 d . . H36A H 0.3826(2) 0.3741(3) 0.28303(9) 0.059 Uiso 1 calc R . C37 C 0.3853(2) 0.5139(3) 0.25201(8) 0.0478(9) Uani 1 d . . H37A H 0.3696(2) 0.5642(3) 0.26861(8) 0.057 Uiso 1 calc R . C38 C 0.40107(15) 0.5529(3) 0.21833(8) 0.0376(7) Uani 1 d . . H38A H 0.39638(15) 0.6297(3) 0.21265(8) 0.045 Uiso 1 calc R . C40 C 0.54983(13) 0.5159(3) 0.05942(7) 0.0328(7) Uani 1 d . . H40A H 0.52323(13) 0.4643(3) 0.06996(7) 0.039 Uiso 1 calc R . C41 C 0.56727(14) 0.4979(3) 0.02435(8) 0.0389(8) Uani 1 d . . H41A H 0.55264(14) 0.4341(3) 0.01183(8) 0.047 Uiso 1 calc R . C42 C 0.6060(2) 0.5740(3) 0.00826(8) 0.0475(9) Uani 1 d . . H42A H 0.6175(2) 0.5619(3) -0.01513(8) 0.057 Uiso 1 calc R . C43 C 0.6277(2) 0.6686(3) 0.02701(9) 0.0565(10) Uani 1 d . . H43A H 0.6537(2) 0.7204(3) 0.01610(9) 0.068 Uiso 1 calc R . C44 C 0.6108(2) 0.6869(3) 0.06233(8) 0.0430(8) Uani 1 d . . H44A H 0.6258(2) 0.7507(3) 0.07473(8) 0.052 Uiso 1 calc R . C39 C 0.57168(12) 0.6104(2) 0.07897(7) 0.0275(6) Uani 1 d . . C46 C 0.62804(14) 0.8099(3) 0.15097(8) 0.0371(7) Uani 1 d . . H46A H 0.59507(14) 0.8607(3) 0.14685(8) 0.045 Uiso 1 calc R . C47 C 0.6870(2) 0.8501(3) 0.16301(9) 0.0481(9) Uani 1 d . . H47A H 0.6934(2) 0.9278(3) 0.16633(9) 0.058 Uiso 1 calc R . C48 C 0.7358(2) 0.7749(3) 0.16997(8) 0.0479(9) Uani 1 d . . H48A H 0.7750(2) 0.8020(3) 0.17778(8) 0.058 Uiso 1 calc R . C49 C 0.72640(15) 0.6592(3) 0.16536(9) 0.0461(8) Uani 1 d . . H49A H 0.75895(15) 0.6084(3) 0.17069(9) 0.055 Uiso 1 calc R . C50 C 0.66830(13) 0.6187(3) 0.15275(8) 0.0367(7) Uani 1 d . . H50A H 0.66236(13) 0.5409(3) 0.14932(8) 0.044 Uiso 1 calc R . C51 C 0.42921(11) 0.6629(2) 0.08431(7) 0.0219(5) Uani 1 d . . C45 C 0.61874(12) 0.6941(2) 0.14518(7) 0.0268(6) Uani 1 d . . C52 C 0.47202(12) 0.7688(2) 0.17752(7) 0.0215(5) Uani 1 d . . N1 N 0.48741(10) 0.8061(2) 0.20546(6) 0.0244(5) Uani 1 d . . O1 O 0.41980(9) 0.6292(2) 0.05517(5) 0.0305(4) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0299(3) 0.0220(3) 0.0146(2) 0.000 -0.0014(2) 0.000 Cl1 0.0344(4) 0.0324(4) 0.0445(4) 0.0117(3) -0.0048(3) -0.0087(3) Mn1 0.0223(2) 0.0197(2) 0.0138(2) -0.0022(2) 0.00134(14) 0.0004(2) P1 0.0209(3) 0.0230(3) 0.0171(3) -0.0026(3) 0.0010(3) -0.0006(3) P2 0.0243(3) 0.0211(3) 0.0154(3) -0.0004(3) 0.0012(3) -0.0008(3) P3 0.0283(4) 0.0201(3) 0.0210(3) -0.0001(3) 0.0007(3) 0.0000(3) P4 0.0238(3) 0.0256(4) 0.0184(3) -0.0036(3) 0.0009(3) 0.0024(3) C1 0.0255(14) 0.0221(13) 0.0199(13) -0.0031(10) 0.0012(10) 0.0011(11) C2 0.0230(13) 0.0333(15) 0.0202(13) -0.0007(11) 0.0032(11) 0.0015(12) C3 0.042(2) 0.055(2) 0.029(2) -0.0106(15) 0.0085(13) -0.020(2) C4 0.060(2) 0.080(3) 0.026(2) -0.017(2) 0.012(2) -0.024(2) C5 0.042(2) 0.068(2) 0.031(2) -0.001(2) 0.0154(14) -0.012(2) C6 0.031(2) 0.046(2) 0.038(2) 0.0003(15) 0.0098(13) -0.0088(14) C7 0.033(2) 0.039(2) 0.028(2) -0.0047(13) 0.0066(12) -0.0066(13) C8 0.0229(13) 0.0292(14) 0.0194(13) -0.0014(11) 0.0023(10) -0.0020(11) C9 0.0243(14) 0.034(2) 0.0264(14) -0.0019(12) 0.0025(11) -0.0005(12) C10 0.032(2) 0.049(2) 0.0261(15) -0.0093(14) 0.0012(12) -0.0060(15) C11 0.029(2) 0.055(2) 0.033(2) 0.005(2) -0.0097(13) 0.0006(15) C12 0.036(2) 0.039(2) 0.047(2) -0.0003(15) -0.0052(14) 0.0071(14) C13 0.030(2) 0.036(2) 0.034(2) -0.0075(13) -0.0038(13) 0.0040(13) C14 0.035(2) 0.0216(13) 0.0178(13) 0.0006(11) -0.0016(11) -0.0058(12) C15 0.036(2) 0.0288(15) 0.0252(14) 0.0032(12) -0.0013(12) -0.0050(13) C16 0.040(2) 0.041(2) 0.033(2) 0.0062(14) -0.0120(14) -0.0062(15) C17 0.050(2) 0.049(2) 0.0223(15) 0.0030(14) -0.0065(14) -0.013(2) C18 0.049(2) 0.046(2) 0.0216(15) -0.0018(14) 0.0061(13) -0.009(2) C19 0.037(2) 0.033(2) 0.0239(14) 0.0032(12) 0.0015(12) -0.0038(13) C20 0.0248(13) 0.0200(13) 0.0224(13) 0.0007(11) 0.0005(10) -0.0005(11) C21 0.040(2) 0.042(2) 0.0260(15) -0.0055(13) 0.0091(13) -0.0099(14) C22 0.040(2) 0.049(2) 0.040(2) -0.002(2) 0.0126(14) -0.020(2) C23 0.030(2) 0.029(2) 0.047(2) -0.0012(14) -0.0058(13) -0.0075(13) C24 0.045(2) 0.032(2) 0.0265(15) -0.0014(13) -0.0067(13) -0.0043(14) C25 0.039(2) 0.0280(15) 0.0226(14) 0.0016(12) -0.0003(12) -0.0053(13) C26 0.0298(15) 0.0275(14) 0.0255(14) 0.0001(12) -0.0037(11) 0.0041(12) C27 0.036(2) 0.0226(14) 0.0224(13) -0.0005(11) -0.0002(12) -0.0029(12) C28 0.040(2) 0.030(2) 0.048(2) -0.0084(14) -0.0042(15) 0.0026(14) C29 0.056(2) 0.031(2) 0.050(2) -0.0141(15) 0.002(2) -0.001(2) C30 0.053(2) 0.034(2) 0.041(2) -0.0081(14) -0.010(2) -0.012(2) C31 0.038(2) 0.039(2) 0.049(2) -0.003(2) -0.0060(15) -0.0048(15) C32 0.035(2) 0.028(2) 0.038(2) -0.0045(13) 0.0004(13) -0.0013(13) C33 0.032(2) 0.0281(15) 0.0263(14) 0.0049(12) -0.0015(12) -0.0047(12) C34 0.063(2) 0.032(2) 0.039(2) 0.0064(14) 0.004(2) 0.001(2) C35 0.080(3) 0.038(2) 0.045(2) 0.016(2) 0.002(2) -0.006(2) C36 0.070(2) 0.051(2) 0.027(2) 0.015(2) 0.001(2) -0.015(2) C37 0.068(2) 0.049(2) 0.027(2) -0.0011(15) 0.010(2) -0.008(2) C38 0.054(2) 0.030(2) 0.029(2) 0.0051(13) 0.0048(14) -0.0032(14) C40 0.0251(14) 0.047(2) 0.0262(15) -0.0081(13) -0.0016(11) 0.0076(13) C41 0.033(2) 0.054(2) 0.029(2) -0.0158(15) -0.0091(13) 0.016(2) C42 0.059(2) 0.061(2) 0.023(2) -0.006(2) 0.0053(15) 0.015(2) C43 0.082(3) 0.056(2) 0.034(2) 0.000(2) 0.024(2) -0.003(2) C44 0.060(2) 0.042(2) 0.028(2) -0.0054(14) 0.0097(15) -0.005(2) C39 0.0276(14) 0.035(2) 0.0200(13) -0.0043(12) 0.0011(11) 0.0093(12) C46 0.036(2) 0.039(2) 0.036(2) -0.0054(14) 0.0001(13) -0.0019(14) C47 0.048(2) 0.052(2) 0.044(2) -0.007(2) -0.001(2) -0.015(2) C48 0.032(2) 0.082(3) 0.031(2) -0.009(2) 0.0007(13) -0.017(2) C49 0.029(2) 0.071(2) 0.038(2) -0.009(2) -0.0001(14) 0.007(2) C50 0.030(2) 0.047(2) 0.033(2) -0.0088(14) -0.0006(13) 0.0052(14) C51 0.0186(13) 0.0228(13) 0.0248(14) 0.0005(11) 0.0041(10) 0.0029(11) C45 0.0252(14) 0.038(2) 0.0176(13) -0.0027(12) 0.0025(11) -0.0010(12) C52 0.0250(13) 0.0186(13) 0.0211(14) 0.0018(11) 0.0042(11) 0.0010(11) N1 0.0315(12) 0.0247(12) 0.0171(12) -0.0017(9) 0.0001(9) 0.0002(10) O1 0.0328(11) 0.0392(11) 0.0194(10) -0.0096(9) -0.0010(8) 0.0028(9) _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 Co1 N1 1.991(2) 2_655 ? Co1 N1 1.991(2) . ? Co1 Cl1 2.2742(8) . ? Co1 Cl1 2.2743(8) 2_655 ? Mn1 C51 1.792(3) . ? Mn1 C52 1.986(3) . ? Mn1 P4 2.2700(8) . ? Mn1 P3 2.2768(9) . ? Mn1 P2 2.2945(8) . ? Mn1 P1 2.3018(8) . ? P1 C2 1.832(3) . ? P1 C8 1.844(3) . ? P1 C1 1.857(3) . ? P2 C14 1.838(3) . ? P2 C1 1.843(3) . ? P2 C20 1.845(3) . ? P3 C33 1.833(3) . ? P3 C27 1.841(3) . ? P3 C26 1.860(3) . ? P4 C45 1.832(3) . ? P4 C39 1.836(3) . ? P4 C26 1.859(3) . ? C2 C7 1.387(4) . ? C2 C3 1.388(4) . ? C3 C4 1.390(4) . ? C4 C5 1.383(5) . ? C5 C6 1.372(4) . ? C6 C7 1.400(4) . ? C8 C9 1.392(4) . ? C8 C13 1.394(4) . ? C9 C10 1.398(4) . ? C10 C11 1.375(4) . ? C11 C12 1.391(4) . ? C12 C13 1.383(4) . ? C14 C15 1.393(4) . ? C14 C19 1.396(4) . ? C15 C16 1.398(4) . ? C16 C17 1.381(5) . ? C17 C18 1.380(5) . ? C18 C19 1.395(4) . ? C20 C21 1.394(4) . ? C20 C25 1.398(4) . ? C21 C22 1.383(4) . ? C22 C23 1.384(4) . ? C23 C24 1.388(4) . ? C24 C25 1.385(4) . ? C27 C28 1.391(4) . ? C27 C32 1.393(4) . ? C28 C29 1.392(4) . ? C29 C30 1.383(5) . ? C30 C31 1.380(5) . ? C31 C32 1.386(4) . ? C33 C38 1.388(4) . ? C33 C34 1.394(4) . ? C34 C35 1.386(5) . ? C35 C36 1.376(5) . ? C36 C37 1.380(5) . ? C37 C38 1.396(4) . ? C40 C41 1.396(4) . ? C40 C39 1.397(4) . ? C41 C42 1.373(5) . ? C42 C43 1.383(5) . ? C43 C44 1.401(4) . ? C44 C39 1.392(4) . ? C46 C45 1.390(4) . ? C46 C47 1.400(4) . ? C47 C48 1.380(5) . ? C48 C49 1.383(5) . ? C49 C50 1.390(4) . ? C50 C45 1.398(4) . ? C51 O1 1.169(3) . ? C52 N1 1.167(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 114.63(13) 2_655 . ? N1 Co1 Cl1 104.21(7) 2_655 . ? N1 Co1 Cl1 113.17(7) . . ? N1 Co1 Cl1 113.18(7) 2_655 2_655 ? N1 Co1 Cl1 104.20(7) . 2_655 ? Cl1 Co1 Cl1 107.46(5) . 2_655 ? C51 Mn1 C52 175.98(11) . . ? C51 Mn1 P4 87.70(8) . . ? C52 Mn1 P4 88.92(8) . . ? C51 Mn1 P3 89.54(9) . . ? C52 Mn1 P3 91.61(7) . . ? P4 Mn1 P3 74.17(3) . . ? C51 Mn1 P2 93.13(8) . . ? C52 Mn1 P2 85.93(7) . . ? P4 Mn1 P2 109.16(3) . . ? P3 Mn1 P2 175.80(3) . . ? C51 Mn1 P1 94.92(8) . . ? C52 Mn1 P1 88.49(8) . . ? P4 Mn1 P1 177.27(3) . . ? P3 Mn1 P1 105.03(3) . . ? P2 Mn1 P1 71.53(3) . . ? C2 P1 C8 100.52(12) . . ? C2 P1 C1 107.91(12) . . ? C8 P1 C1 102.33(12) . . ? C2 P1 Mn1 126.91(9) . . ? C8 P1 Mn1 122.43(9) . . ? C1 P1 Mn1 92.89(8) . . ? C14 P2 C1 106.31(12) . . ? C14 P2 C20 102.67(12) . . ? C1 P2 C20 105.36(12) . . ? C14 P2 Mn1 114.93(9) . . ? C1 P2 Mn1 93.49(8) . . ? C20 P2 Mn1 130.96(9) . . ? C33 P3 C27 100.86(12) . . ? C33 P3 C26 105.58(12) . . ? C27 P3 C26 107.66(13) . . ? C33 P3 Mn1 127.98(10) . . ? C27 P3 Mn1 117.75(9) . . ? C26 P3 Mn1 94.94(9) . . ? C45 P4 C39 99.96(12) . . ? C45 P4 C26 105.15(13) . . ? C39 P4 C26 107.26(13) . . ? C45 P4 Mn1 128.59(9) . . ? C39 P4 Mn1 118.40(9) . . ? C26 P4 Mn1 95.20(9) . . ? P2 C1 P1 93.09(12) . . ? C7 C2 C3 118.9(3) . . ? C7 C2 P1 119.8(2) . . ? C3 C2 P1 121.0(2) . . ? C2 C3 C4 120.4(3) . . ? C5 C4 C3 120.3(3) . . ? C6 C5 C4 120.0(3) . . ? C5 C6 C7 120.0(3) . . ? C2 C7 C6 120.5(3) . . ? C9 C8 C13 118.5(2) . . ? C9 C8 P1 122.5(2) . . ? C13 C8 P1 119.0(2) . . ? C8 C9 C10 120.2(3) . . ? C11 C10 C9 120.5(3) . . ? C10 C11 C12 119.7(3) . . ? C13 C12 C11 119.8(3) . . ? C12 C13 C8 121.2(3) . . ? C15 C14 C19 118.6(2) . . ? C15 C14 P2 123.3(2) . . ? C19 C14 P2 118.0(2) . . ? C14 C15 C16 120.8(3) . . ? C17 C16 C15 119.6(3) . . ? C18 C17 C16 120.6(3) . . ? C17 C18 C19 119.9(3) . . ? C14 C19 C18 120.5(3) . . ? C21 C20 C25 118.0(2) . . ? C21 C20 P2 120.8(2) . . ? C25 C20 P2 121.1(2) . . ? C22 C21 C20 120.9(3) . . ? C21 C22 C23 120.8(3) . . ? C22 C23 C24 118.9(3) . . ? C25 C24 C23 120.6(3) . . ? C24 C25 C20 120.8(3) . . ? P4 C26 P3 95.01(12) . . ? C28 C27 C32 118.4(3) . . ? C28 C27 P3 125.0(2) . . ? C32 C27 P3 116.5(2) . . ? C27 C28 C29 120.3(3) . . ? C30 C29 C28 120.6(3) . . ? C31 C30 C29 119.4(3) . . ? C30 C31 C32 120.2(3) . . ? C31 C32 C27 121.0(3) . . ? C38 C33 C34 118.9(3) . . ? C38 C33 P3 120.4(2) . . ? C34 C33 P3 120.7(2) . . ? C35 C34 C33 120.4(3) . . ? C36 C35 C34 120.2(3) . . ? C35 C36 C37 120.3(3) . . ? C36 C37 C38 119.7(3) . . ? C33 C38 C37 120.4(3) . . ? C41 C40 C39 121.1(3) . . ? C42 C41 C40 120.2(3) . . ? C41 C42 C43 119.7(3) . . ? C42 C43 C44 120.5(3) . . ? C39 C44 C43 120.4(3) . . ? C44 C39 C40 118.1(3) . . ? C44 C39 P4 119.4(2) . . ? C40 C39 P4 122.2(2) . . ? C45 C46 C47 120.0(3) . . ? C48 C47 C46 120.3(3) . . ? C47 C48 C49 120.1(3) . . ? C48 C49 C50 120.0(3) . . ? C49 C50 C45 120.5(3) . . ? O1 C51 Mn1 177.8(2) . . ? C46 C45 C50 119.1(3) . . ? C46 C45 P4 120.3(2) . . ? C50 C45 P4 120.4(2) . . ? N1 C52 Mn1 177.4(2) . . ? C52 N1 Co1 167.0(2) . . ? _refine_diff_density_max 0.350 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.057 #=END data_13.CH2Cl2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C53 H46 Cl5 Mn2 N O P4' _chemical_formula_weight 1124.0 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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 'P 1 2(1)/c 1' 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 12.629(3) _cell_length_b 23.525(4) _cell_length_c 18.306(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.31(2) _cell_angle_gamma 90.00 _cell_volume 5270.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 219 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 24.00 _exptl_crystal_description Plates _exptl_crystal_colour Red _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method ? _exptl_crystal_F_000 2296 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_T_max 0.803 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25042 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 24.00 _reflns_number_total 8253 _reflns_number_observed 5433 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 38 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+8.1546P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8215 _refine_ls_number_parameters 610 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0932 _refine_ls_R_factor_obs 0.0521 _refine_ls_wR_factor_all 0.1416 _refine_ls_wR_factor_obs 0.1193 _refine_ls_goodness_of_fit_all 1.017 _refine_ls_goodness_of_fit_obs 1.088 _refine_ls_restrained_S_all 1.029 _refine_ls_restrained_S_obs 1.088 _refine_ls_shift/esd_max -0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mn1 Mn 0.75892(5) 0.25039(3) 0.47199(4) 0.0228(2) Uani 1 d . . Mn2 Mn 0.67377(6) 0.42165(3) 0.28784(4) 0.0305(2) Uani 1 d . . Cl1 Cl 0.6322(2) 0.51145(7) 0.32245(12) 0.0869(7) Uani 1 d . . Cl2 Cl 0.80771(12) 0.41646(7) 0.22103(9) 0.0566(4) Uani 1 d . . Cl3 Cl 0.51358(11) 0.37191(6) 0.22081(7) 0.0391(3) Uani 1 d . . P1 P 0.85071(9) 0.29785(5) 0.58251(7) 0.0250(3) Uani 1 d . . P2 P 0.94631(10) 0.23971(5) 0.48535(7) 0.0256(3) Uani 1 d . . P3 P 0.57037(9) 0.26229(5) 0.45393(7) 0.0237(3) Uani 1 d . . P4 P 0.66875(10) 0.20385(5) 0.35971(7) 0.0249(3) Uani 1 d . . N1 N 0.7264(3) 0.3624(2) 0.3781(2) 0.0294(9) Uani 1 d . . O1 O 0.7716(3) 0.14324(15) 0.5582(2) 0.0429(9) Uani 1 d . . C1 C 0.9748(4) 0.2552(2) 0.5874(3) 0.0282(11) Uani 1 d . . H1A H 0.9771(4) 0.2204(2) 0.6182(3) 0.034 Uiso 1 calc R . H1B H 1.0427(4) 0.2774(2) 0.6058(3) 0.034 Uiso 1 calc R . C2 C 0.8013(4) 0.2879(2) 0.6672(3) 0.0296(11) Uani 1 d . . C3 C 0.7509(4) 0.3329(2) 0.6947(3) 0.0399(13) Uani 1 d . . H3A H 0.7539(4) 0.3701(2) 0.6751(3) 0.048 Uiso 1 calc R . C4 C 0.6960(5) 0.3236(3) 0.7510(3) 0.050(2) Uani 1 d . . H4A H 0.6615(5) 0.3544(3) 0.7696(3) 0.060 Uiso 1 calc R . C5 C 0.6918(4) 0.2700(3) 0.7795(3) 0.048(2) Uani 1 d . . H5A H 0.6523(4) 0.2633(3) 0.8166(3) 0.058 Uiso 1 calc R . C6 C 0.7449(4) 0.2261(2) 0.7542(3) 0.0422(14) Uani 1 d . . H6A H 0.7445(4) 0.1894(2) 0.7758(3) 0.051 Uiso 1 calc R . C7 C 0.7984(4) 0.2341(2) 0.6986(3) 0.0341(12) Uani 1 d . . H7A H 0.8336(4) 0.2030(2) 0.6813(3) 0.041 Uiso 1 calc R . C8 C 0.8911(4) 0.3718(2) 0.5836(3) 0.0318(12) Uani 1 d . . C9 C 0.8158(4) 0.4131(2) 0.5490(3) 0.0394(13) Uani 1 d . . H9A H 0.7433(4) 0.4022(2) 0.5245(3) 0.047 Uiso 1 calc R . C10 C 0.8454(5) 0.4692(2) 0.5500(4) 0.056(2) Uani 1 d . . H10A H 0.7936(5) 0.4967(2) 0.5257(4) 0.067 Uiso 1 calc R . C11 C 0.9500(6) 0.4859(3) 0.5860(4) 0.068(2) Uani 1 d . . H11A H 0.9696(6) 0.5249(3) 0.5873(4) 0.081 Uiso 1 calc R . C12 C 1.0257(6) 0.4459(3) 0.6200(5) 0.077(2) Uani 1 d . . H12A H 1.0981(6) 0.4571(3) 0.6443(5) 0.093 Uiso 1 calc R . C13 C 0.9957(5) 0.3891(2) 0.6186(4) 0.055(2) Uani 1 d . . H13A H 1.0482(5) 0.3616(2) 0.6422(4) 0.066 Uiso 1 calc R . C14 C 0.9977(4) 0.1699(2) 0.4704(3) 0.0299(12) Uani 1 d . . C15 C 1.0403(4) 0.1325(2) 0.5286(3) 0.0426(14) Uani 1 d . . H15A H 1.0509(4) 0.1442(2) 0.5795(3) 0.051 Uiso 1 calc R . C16 C 1.0676(5) 0.0774(3) 0.5117(4) 0.060(2) Uani 1 d . . H16A H 1.0965(5) 0.0514(3) 0.5514(4) 0.072 Uiso 1 calc R . C17 C 1.0532(5) 0.0605(3) 0.4387(5) 0.063(2) Uani 1 d . . H17A H 1.0723(5) 0.0229(3) 0.4281(5) 0.076 Uiso 1 calc R . C18 C 1.0110(5) 0.0974(3) 0.3801(4) 0.054(2) Uani 1 d . . H18A H 1.0003(5) 0.0852(3) 0.3293(4) 0.065 Uiso 1 calc R . C19 C 0.9844(4) 0.1526(2) 0.3960(3) 0.0408(14) Uani 1 d . . H19A H 0.9572(4) 0.1786(2) 0.3560(3) 0.049 Uiso 1 calc R . C20 C 1.0297(4) 0.2887(2) 0.4462(3) 0.0269(11) Uani 1 d . . C21 C 0.9870(4) 0.3196(2) 0.3822(3) 0.0361(13) Uani 1 d . . H21A H 0.9125(4) 0.3150(2) 0.3562(3) 0.043 Uiso 1 calc R . C22 C 1.0530(4) 0.3577(2) 0.3552(3) 0.0396(13) Uani 1 d . . H22A H 1.0236(4) 0.3789(2) 0.3107(3) 0.048 Uiso 1 calc R . C23 C 1.1608(4) 0.3646(2) 0.3932(3) 0.0405(14) Uani 1 d . . H23A H 1.2051(4) 0.3914(2) 0.3757(3) 0.049 Uiso 1 calc R . C24 C 1.2040(4) 0.3332(2) 0.4555(3) 0.0441(14) Uani 1 d . . H24A H 1.2787(4) 0.3377(2) 0.4810(3) 0.053 Uiso 1 calc R . C25 C 1.1392(4) 0.2942(2) 0.4824(3) 0.0417(14) Uani 1 d . . H25A H 1.1701(4) 0.2716(2) 0.5254(3) 0.050 Uiso 1 calc R . C26 C 0.5453(4) 0.2479(2) 0.3524(3) 0.0250(11) Uani 1 d . . H26A H 0.5458(4) 0.2828(2) 0.3224(3) 0.030 Uiso 1 calc R . H26B H 0.4769(4) 0.2264(2) 0.3325(3) 0.030 Uiso 1 calc R . C27 C 0.4887(4) 0.2118(2) 0.4915(3) 0.0282(11) Uani 1 d . . C28 C 0.5257(4) 0.1890(2) 0.5626(3) 0.0359(13) Uani 1 d . . H28A H 0.5963(4) 0.1986(2) 0.5922(3) 0.043 Uiso 1 calc R . C29 C 0.4600(5) 0.1520(2) 0.5913(3) 0.0452(15) Uani 1 d . . H29A H 0.4861(5) 0.1362(2) 0.6402(3) 0.054 Uiso 1 calc R . C30 C 0.3577(4) 0.1385(2) 0.5489(3) 0.0414(14) Uani 1 d . . H30A H 0.3133(4) 0.1128(2) 0.5682(3) 0.050 Uiso 1 calc R . C31 C 0.3194(5) 0.1618(3) 0.4793(3) 0.050(2) Uani 1 d . . H31A H 0.2478(5) 0.1527(3) 0.4506(3) 0.060 Uiso 1 calc R . C32 C 0.3834(4) 0.1984(2) 0.4502(3) 0.0418(14) Uani 1 d . . H32A H 0.3557(4) 0.2146(2) 0.4017(3) 0.050 Uiso 1 calc R . C33 C 0.5154(4) 0.3310(2) 0.4712(3) 0.0253(11) Uani 1 d . . C34 C 0.4760(4) 0.3706(2) 0.4158(3) 0.0328(12) Uani 1 d . . H34A H 0.4736(4) 0.3622(2) 0.3646(3) 0.039 Uiso 1 calc R . C35 C 0.4398(4) 0.4231(2) 0.4354(3) 0.0413(14) Uani 1 d . . H35A H 0.4118(4) 0.4505(2) 0.3975(3) 0.050 Uiso 1 calc R . C36 C 0.4444(4) 0.4352(2) 0.5098(4) 0.0432(15) Uani 1 d . . H36A H 0.4201(4) 0.4712(2) 0.5229(4) 0.052 Uiso 1 calc R . C37 C 0.4840(4) 0.3958(2) 0.5653(3) 0.0397(14) Uani 1 d . . H37A H 0.4867(4) 0.4044(2) 0.6164(3) 0.048 Uiso 1 calc R . C38 C 0.5202(4) 0.3432(2) 0.5466(3) 0.0323(12) Uani 1 d . . H38A H 0.5478(4) 0.3158(2) 0.5847(3) 0.039 Uiso 1 calc R . C39 C 0.6252(4) 0.1309(2) 0.3639(3) 0.0340(12) Uani 1 d . . C40 C 0.7005(5) 0.0902(2) 0.3977(3) 0.0470(15) Uani 1 d . . H40A H 0.7740(5) 0.1010(2) 0.4196(3) 0.056 Uiso 1 calc R . C41 C 0.6698(6) 0.0340(3) 0.3999(5) 0.076(2) Uani 1 d . . H41A H 0.7218(6) 0.0063(3) 0.4237(5) 0.092 Uiso 1 calc R . C42 C 0.5638(6) 0.0182(3) 0.3675(7) 0.115(4) Uani 1 d . . H42A H 0.5417(6) -0.0202(3) 0.3705(7) 0.138 Uiso 1 calc R . C43 C 0.4897(6) 0.0582(3) 0.3307(6) 0.113(4) Uani 1 d . . H43A H 0.4171(6) 0.0470(3) 0.3067(6) 0.135 Uiso 1 calc R . C44 C 0.5206(5) 0.1143(2) 0.3287(4) 0.067(2) Uani 1 d . . H44A H 0.4694(5) 0.1416(2) 0.3028(4) 0.080 Uiso 1 calc R . C45 C 0.7180(4) 0.2077(2) 0.2745(3) 0.0275(11) Uani 1 d . . C46 C 0.7535(4) 0.1583(2) 0.2446(3) 0.0371(13) Uani 1 d . . H46A H 0.7427(4) 0.1220(2) 0.2642(3) 0.045 Uiso 1 calc R . C47 C 0.8045(4) 0.1633(3) 0.1857(3) 0.0437(14) Uani 1 d . . H47A H 0.8269(4) 0.1300(3) 0.1644(3) 0.052 Uiso 1 calc R . C48 C 0.8230(4) 0.2152(3) 0.1581(3) 0.0431(14) Uani 1 d . . H48A H 0.8612(4) 0.2180(3) 0.1195(3) 0.052 Uiso 1 calc R . C49 C 0.7856(4) 0.2639(2) 0.1865(3) 0.0410(14) Uani 1 d . . H49A H 0.7959(4) 0.3000(2) 0.1661(3) 0.049 Uiso 1 calc R . C50 C 0.7655(4) 0.1850(2) 0.5249(3) 0.0296(12) Uani 1 d . . C51 C 0.7436(3) 0.3214(2) 0.4132(3) 0.0240(11) Uani 1 d . . C52 C 0.7339(4) 0.2601(2) 0.2442(3) 0.0333(12) Uani 1 d . . H52A H 0.7088(4) 0.2936(2) 0.2634(3) 0.040 Uiso 1 calc R . C53 C 0.7219(14) 0.5340(5) 0.8261(11) 0.145(8) Uani 0.80 d PD 1 H53A H 0.6586(14) 0.5558(5) 0.8338(11) 0.174 Uiso 0.80 calc PR 1 H53B H 0.7629(14) 0.5174(5) 0.8745(11) 0.174 Uiso 0.80 calc PR 1 Cl4 Cl 0.6777(3) 0.4752(2) 0.7455(3) 0.183(2) Uani 0.80 d PD 1 Cl5 Cl 0.8015(2) 0.57273(11) 0.7854(2) 0.0965(8) Uani 0.80 d PD 1 C53' C 0.6969(26) 0.5248(13) 0.7957(16) 0.016(6) Uani 0.20 d PDU 2 H53C H 0.7096(26) 0.5662(13) 0.8026(16) 0.020 Uiso 0.20 calc PR 2 H53D H 0.6174(26) 0.5180(13) 0.7865(16) 0.020 Uiso 0.20 calc PR 2 Cl4' Cl 0.7451(13) 0.5003(7) 0.7086(14) 0.183(2) Uani 0.20 d PD 2 Cl5' Cl 0.7668(9) 0.4882(5) 0.8818(7) 0.0965(8) Uani 0.20 d PD 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0180(3) 0.0265(4) 0.0243(4) -0.0002(3) 0.0058(3) -0.0014(3) Mn2 0.0392(5) 0.0237(4) 0.0309(4) -0.0001(3) 0.0132(4) -0.0005(3) Cl1 0.152(2) 0.0289(8) 0.102(2) -0.0101(9) 0.0740(15) 0.0136(10) Cl2 0.0559(9) 0.0727(11) 0.0508(9) 0.0087(8) 0.0315(8) 0.0067(8) Cl3 0.0372(7) 0.0446(8) 0.0340(7) -0.0044(6) 0.0060(6) -0.0024(6) P1 0.0206(6) 0.0298(7) 0.0248(7) -0.0003(6) 0.0058(5) -0.0006(5) P2 0.0192(6) 0.0301(7) 0.0281(7) -0.0002(6) 0.0071(5) -0.0011(5) P3 0.0195(6) 0.0272(7) 0.0255(7) -0.0005(5) 0.0080(5) -0.0006(5) P4 0.0229(6) 0.0237(7) 0.0285(7) -0.0039(5) 0.0072(6) -0.0009(5) N1 0.030(2) 0.031(2) 0.027(2) 0.002(2) 0.007(2) -0.004(2) O1 0.048(2) 0.032(2) 0.046(2) 0.014(2) 0.007(2) 0.000(2) C1 0.021(2) 0.032(3) 0.030(3) 0.003(2) 0.004(2) -0.001(2) C2 0.025(3) 0.038(3) 0.026(3) -0.002(2) 0.007(2) -0.002(2) C3 0.043(3) 0.047(3) 0.033(3) -0.005(3) 0.015(3) 0.005(3) C4 0.048(4) 0.068(4) 0.037(3) -0.007(3) 0.016(3) 0.014(3) C5 0.038(3) 0.076(5) 0.033(3) 0.002(3) 0.016(3) -0.008(3) C6 0.041(3) 0.051(4) 0.035(3) 0.004(3) 0.011(3) -0.013(3) C7 0.031(3) 0.041(3) 0.030(3) -0.003(2) 0.007(2) -0.006(2) C8 0.033(3) 0.033(3) 0.030(3) -0.004(2) 0.009(2) -0.005(2) C9 0.039(3) 0.036(3) 0.042(3) -0.003(3) 0.008(3) 0.002(3) C10 0.064(4) 0.036(3) 0.067(4) 0.002(3) 0.014(4) 0.005(3) C11 0.073(5) 0.035(4) 0.099(6) 0.003(4) 0.030(5) -0.010(3) C12 0.057(4) 0.046(4) 0.118(7) -0.005(4) 0.001(4) -0.014(4) C13 0.039(3) 0.036(3) 0.081(5) 0.000(3) -0.003(3) -0.004(3) C14 0.019(3) 0.030(3) 0.043(3) -0.001(2) 0.012(2) -0.003(2) C15 0.044(3) 0.040(3) 0.052(4) 0.005(3) 0.026(3) 0.005(3) C16 0.066(4) 0.039(4) 0.087(5) 0.023(4) 0.040(4) 0.016(3) C17 0.064(4) 0.038(4) 0.102(6) -0.009(4) 0.048(4) 0.004(3) C18 0.042(4) 0.056(4) 0.068(5) -0.023(4) 0.022(3) -0.003(3) C19 0.030(3) 0.046(3) 0.046(4) -0.011(3) 0.009(3) -0.003(3) C20 0.019(2) 0.033(3) 0.030(3) -0.003(2) 0.009(2) 0.000(2) C21 0.021(3) 0.050(3) 0.038(3) 0.004(3) 0.007(2) 0.000(2) C22 0.036(3) 0.047(3) 0.039(3) 0.010(3) 0.016(3) 0.004(3) C23 0.035(3) 0.045(3) 0.047(4) 0.000(3) 0.022(3) -0.010(3) C24 0.025(3) 0.060(4) 0.047(4) -0.001(3) 0.009(3) -0.016(3) C25 0.025(3) 0.057(4) 0.040(3) 0.006(3) 0.003(2) -0.006(3) C26 0.019(2) 0.029(3) 0.028(3) 0.000(2) 0.007(2) -0.002(2) C27 0.026(3) 0.026(3) 0.036(3) 0.001(2) 0.015(2) 0.000(2) C28 0.027(3) 0.044(3) 0.037(3) 0.002(3) 0.009(2) -0.001(2) C29 0.048(4) 0.048(4) 0.045(4) 0.017(3) 0.020(3) 0.005(3) C30 0.042(3) 0.035(3) 0.057(4) -0.002(3) 0.030(3) -0.010(3) C31 0.035(3) 0.069(4) 0.045(4) 0.002(3) 0.011(3) -0.020(3) C32 0.030(3) 0.053(4) 0.039(3) 0.010(3) 0.003(3) -0.010(3) C33 0.019(2) 0.028(3) 0.032(3) -0.003(2) 0.012(2) -0.003(2) C34 0.033(3) 0.031(3) 0.038(3) -0.002(2) 0.015(2) 0.000(2) C35 0.042(3) 0.033(3) 0.055(4) 0.005(3) 0.023(3) 0.000(3) C36 0.041(3) 0.025(3) 0.071(4) -0.012(3) 0.028(3) -0.007(2) C37 0.037(3) 0.041(3) 0.044(3) -0.018(3) 0.016(3) -0.013(3) C38 0.026(3) 0.039(3) 0.036(3) -0.007(2) 0.016(2) -0.005(2) C39 0.035(3) 0.024(3) 0.045(3) -0.007(2) 0.012(3) -0.003(2) C40 0.036(3) 0.033(3) 0.071(4) -0.007(3) 0.011(3) -0.001(3) C41 0.059(5) 0.026(3) 0.140(7) 0.000(4) 0.016(5) 0.008(3) C42 0.063(5) 0.035(4) 0.246(12) 0.002(6) 0.038(7) -0.008(4) C43 0.040(4) 0.039(4) 0.247(12) -0.023(6) 0.015(6) -0.016(3) C44 0.039(4) 0.029(3) 0.124(6) -0.009(4) 0.004(4) -0.007(3) C45 0.019(2) 0.036(3) 0.025(3) -0.007(2) 0.001(2) 0.002(2) C46 0.035(3) 0.036(3) 0.040(3) -0.007(3) 0.009(3) 0.006(2) C47 0.046(3) 0.052(4) 0.037(3) -0.014(3) 0.017(3) 0.014(3) C48 0.038(3) 0.061(4) 0.035(3) -0.007(3) 0.017(3) 0.002(3) C49 0.044(3) 0.044(3) 0.036(3) -0.001(3) 0.013(3) -0.001(3) C50 0.022(3) 0.036(3) 0.030(3) 0.000(2) 0.006(2) 0.000(2) C51 0.016(2) 0.035(3) 0.021(3) -0.005(2) 0.004(2) -0.003(2) C52 0.037(3) 0.035(3) 0.030(3) -0.004(2) 0.012(2) 0.001(2) C53 0.168(16) 0.062(8) 0.256(23) -0.045(11) 0.150(16) 0.013(9) Cl4 0.106(3) 0.101(3) 0.308(6) 0.010(3) -0.014(3) -0.023(2) Cl5 0.097(2) 0.069(2) 0.130(2) 0.028(2) 0.040(2) 0.0077(14) C53' 0.018(7) 0.011(8) 0.022(7) 0.001(5) 0.008(5) -0.001(5) Cl4' 0.106(3) 0.101(3) 0.308(6) 0.010(3) -0.014(3) -0.023(2) Cl5' 0.097(2) 0.069(2) 0.130(2) 0.028(2) 0.040(2) 0.0077(14) _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 C50 1.808(5) . ? Mn1 C51 1.970(5) . ? Mn1 P2 2.3318(14) . ? Mn1 P3 2.3386(14) . ? Mn1 P1 2.3503(15) . ? Mn1 P4 2.3587(15) . ? Mn2 N1 2.138(4) . ? Mn2 Cl1 2.303(2) . ? Mn2 Cl2 2.323(2) . ? Mn2 Cl3 2.396(2) . ? P1 C8 1.813(5) . ? P1 C2 1.825(5) . ? P1 C1 1.844(5) . ? P2 C14 1.812(5) . ? P2 C20 1.823(5) . ? P2 C1 1.850(5) . ? P3 C27 1.816(5) . ? P3 C33 1.817(5) . ? P3 C26 1.837(5) . ? P4 C39 1.808(5) . ? P4 C45 1.818(5) . ? P4 C26 1.849(4) . ? N1 C51 1.150(6) . ? O1 C50 1.149(6) . ? C2 C3 1.391(7) . ? C2 C7 1.395(7) . ? C3 C4 1.394(7) . ? C4 C5 1.370(8) . ? C5 C6 1.372(8) . ? C6 C7 1.367(7) . ? C8 C13 1.380(7) . ? C8 C9 1.396(7) . ? C9 C10 1.369(8) . ? C10 C11 1.379(9) . ? C11 C12 1.376(9) . ? C12 C13 1.387(8) . ? C14 C15 1.383(7) . ? C14 C19 1.390(7) . ? C15 C16 1.396(8) . ? C16 C17 1.361(9) . ? C17 C18 1.382(9) . ? C18 C19 1.390(8) . ? C20 C21 1.371(7) . ? C20 C25 1.383(6) . ? C21 C22 1.396(7) . ? C22 C23 1.376(7) . ? C23 C24 1.356(7) . ? C24 C25 1.397(7) . ? C27 C28 1.379(7) . ? C27 C32 1.394(7) . ? C28 C29 1.391(7) . ? C29 C30 1.371(8) . ? C30 C31 1.362(8) . ? C31 C32 1.375(7) . ? C33 C34 1.377(7) . ? C33 C38 1.395(7) . ? C34 C35 1.396(7) . ? C35 C36 1.378(8) . ? C36 C37 1.375(8) . ? C37 C38 1.390(7) . ? C39 C44 1.376(7) . ? C39 C40 1.384(7) . ? C40 C41 1.381(8) . ? C41 C42 1.374(10) . ? C42 C43 1.380(11) . ? C43 C44 1.381(9) . ? C45 C52 1.386(7) . ? C45 C46 1.405(7) . ? C46 C47 1.390(7) . ? C47 C48 1.364(8) . ? C48 C49 1.389(7) . ? C49 C52 1.374(7) . ? C53 Cl5 1.66(2) . ? C53 Cl4 1.998(15) . ? C53' Cl5' 1.82(3) . ? C53' Cl4' 1.93(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 C50 Mn1 C51 177.1(2) . . ? C50 Mn1 P2 86.6(2) . . ? C51 Mn1 P2 96.24(13) . . ? C50 Mn1 P3 95.1(2) . . ? C51 Mn1 P3 82.08(13) . . ? P2 Mn1 P3 177.83(6) . . ? C50 Mn1 P1 89.7(2) . . ? C51 Mn1 P1 91.63(13) . . ? P2 Mn1 P1 71.88(5) . . ? P3 Mn1 P1 109.46(5) . . ? C50 Mn1 P4 91.2(2) . . ? C51 Mn1 P4 87.51(14) . . ? P2 Mn1 P4 107.48(5) . . ? P3 Mn1 P4 71.15(5) . . ? P1 Mn1 P4 178.87(5) . . ? N1 Mn2 Cl1 115.71(12) . . ? N1 Mn2 Cl2 104.16(12) . . ? Cl1 Mn2 Cl2 115.99(7) . . ? N1 Mn2 Cl3 98.02(11) . . ? Cl1 Mn2 Cl3 111.58(8) . . ? Cl2 Mn2 Cl3 109.72(6) . . ? C8 P1 C2 105.5(2) . . ? C8 P1 C1 106.8(2) . . ? C2 P1 C1 110.7(2) . . ? C8 P1 Mn1 122.9(2) . . ? C2 P1 Mn1 118.1(2) . . ? C1 P1 Mn1 90.9(2) . . ? C14 P2 C20 104.5(2) . . ? C14 P2 C1 110.1(2) . . ? C20 P2 C1 106.6(2) . . ? C14 P2 Mn1 118.3(2) . . ? C20 P2 Mn1 124.1(2) . . ? C1 P2 Mn1 91.36(15) . . ? C27 P3 C33 103.8(2) . . ? C27 P3 C26 106.8(2) . . ? C33 P3 C26 111.3(2) . . ? C27 P3 Mn1 121.5(2) . . ? C33 P3 Mn1 120.07(15) . . ? C26 P3 Mn1 92.05(14) . . ? C39 P4 C45 104.8(2) . . ? C39 P4 C26 106.0(2) . . ? C45 P4 C26 111.8(2) . . ? C39 P4 Mn1 119.3(2) . . ? C45 P4 Mn1 122.0(2) . . ? C26 P4 Mn1 91.12(15) . . ? C51 N1 Mn2 163.4(4) . . ? P1 C1 P2 96.1(2) . . ? C3 C2 C7 118.7(5) . . ? C3 C2 P1 119.6(4) . . ? C7 C2 P1 121.0(4) . . ? C2 C3 C4 120.2(5) . . ? C5 C4 C3 120.0(5) . . ? C4 C5 C6 119.7(5) . . ? C7 C6 C5 121.3(5) . . ? C6 C7 C2 120.0(5) . . ? C13 C8 C9 118.2(5) . . ? C13 C8 P1 121.5(4) . . ? C9 C8 P1 120.3(4) . . ? C10 C9 C8 120.7(5) . . ? C9 C10 C11 120.5(6) . . ? C12 C11 C10 119.8(6) . . ? C11 C12 C13 119.6(6) . . ? C8 C13 C12 121.1(6) . . ? C15 C14 C19 119.9(5) . . ? C15 C14 P2 123.0(4) . . ? C19 C14 P2 116.9(4) . . ? C14 C15 C16 119.4(6) . . ? C17 C16 C15 120.5(6) . . ? C16 C17 C18 120.7(6) . . ? C17 C18 C19 119.4(6) . . ? C18 C19 C14 120.1(6) . . ? C21 C20 C25 119.7(5) . . ? C21 C20 P2 121.8(4) . . ? C25 C20 P2 118.5(4) . . ? C20 C21 C22 120.0(5) . . ? C23 C22 C21 120.0(5) . . ? C24 C23 C22 120.2(5) . . ? C23 C24 C25 120.4(5) . . ? C20 C25 C24 119.7(5) . . ? P3 C26 P4 95.7(2) . . ? C28 C27 C32 118.6(4) . . ? C28 C27 P3 121.4(4) . . ? C32 C27 P3 119.9(4) . . ? C27 C28 C29 120.4(5) . . ? C30 C29 C28 119.8(5) . . ? C31 C30 C29 120.3(5) . . ? C30 C31 C32 120.5(5) . . ? C31 C32 C27 120.3(5) . . ? C34 C33 C38 120.6(4) . . ? C34 C33 P3 123.9(4) . . ? C38 C33 P3 115.5(4) . . ? C33 C34 C35 119.4(5) . . ? C36 C35 C34 120.1(5) . . ? C37 C36 C35 120.6(5) . . ? C36 C37 C38 120.0(5) . . ? C37 C38 C33 119.3(5) . . ? C44 C39 C40 119.1(5) . . ? C44 C39 P4 121.1(4) . . ? C40 C39 P4 119.6(4) . . ? C41 C40 C39 120.7(5) . . ? C42 C41 C40 119.8(6) . . ? C41 C42 C43 119.9(7) . . ? C42 C43 C44 120.2(7) . . ? C39 C44 C43 120.3(6) . . ? C52 C45 C46 119.1(5) . . ? C52 C45 P4 120.2(4) . . ? C46 C45 P4 120.2(4) . . ? C47 C46 C45 119.1(5) . . ? C48 C47 C46 121.2(5) . . ? C47 C48 C49 119.6(5) . . ? C52 C49 C48 120.2(5) . . ? O1 C50 Mn1 178.7(4) . . ? N1 C51 Mn1 174.9(4) . . ? C49 C52 C45 120.7(5) . . ? Cl5 C53 Cl4 98.0(8) . . ? Cl5' C53' Cl4' 113.0(18) . . ? _refine_diff_density_max 1.014 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.078 #=END