Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Vernon Gibson' 'Stuart McTavish' 'Carl Redshaw' 'Gregory A. Solan' 'Andrew J.P. White' 'David J. WIlliams' _publ_contact_author_name 'Prof Vernon Gibson' _publ_contact_author_address ; Department of Chemistry Imperial College Exhibition Rd London SW7 2AY UNITED KINGDOM ; _publ_contact_author_email 'V.GIBSON@IC.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; >From Monomeric to Polymeric Manganese Complexes Bearing Bis(imino)pyridine and Related Ligands ; data_VG0152 _database_code_CSD 190871 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C29 H34 N4 Br2 Mn' _chemical_formula_weight 653.36 _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' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.8419(4) _cell_length_b 15.1562(5) _cell_length_c 23.4306(15) _cell_angle_alpha 90.00 _cell_angle_beta 92.042(3) _cell_angle_gamma 90.00 _cell_volume 5977.1(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 10.96 _cell_measurement_theta_max 24.98 _exptl_crystal_description plates _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method ? _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 6.896 _exptl_absorpt_correction_type 'Lamina [0 0 1]' _exptl_absorpt_correction_T_min 0.3018 _exptl_absorpt_correction_T_max 0.7855 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8504 _diffrn_reflns_av_R_equivalents 0.0839 _diffrn_reflns_av_sigmaI/netI 0.0832 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 60.00 _reflns_number_total 8194 _reflns_number_observed 5248 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 897 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^)+(0.0713P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00011(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7297 _refine_ls_number_parameters 677 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_obs 0.0592 _refine_ls_wR_factor_all 0.1600 _refine_ls_wR_factor_obs 0.1330 _refine_ls_goodness_of_fit_all 1.012 _refine_ls_goodness_of_fit_obs 1.097 _refine_ls_restrained_S_all 1.027 _refine_ls_restrained_S_obs 1.084 _refine_ls_shift/esd_max 0.000 _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 Mn Mn 0.72066(7) 0.63851(8) 0.28563(5) 0.0425(3) Uani 1 d . . Br1 Br 0.85209(5) 0.65875(7) 0.33663(4) 0.0638(3) Uani 1 d . . Br2 Br 0.67298(6) 0.77539(6) 0.23711(4) 0.0583(2) Uani 1 d . . N1 N 0.6558(3) 0.5124(4) 0.2867(3) 0.0432(14) Uani 1 d . . C2 C 0.6681(4) 0.4519(5) 0.2470(3) 0.043(2) Uani 1 d . . C3 C 0.6319(5) 0.3717(6) 0.2474(4) 0.057(2) Uani 1 d . . H3A H 0.6417(5) 0.3305(6) 0.2191(4) 0.068 Uiso 1 calc R . C4 C 0.5807(6) 0.3520(6) 0.2899(4) 0.064(2) Uani 1 d . . H4A H 0.5560(6) 0.2972(6) 0.2913(4) 0.077 Uiso 1 calc R . C5 C 0.5668(6) 0.4157(7) 0.3307(4) 0.066(3) Uani 1 d . . H5A H 0.5313(6) 0.4048(7) 0.3594(4) 0.079 Uiso 1 calc R . C6 C 0.6056(4) 0.4950(6) 0.3286(3) 0.049(2) Uani 1 d . . C7 C 0.7243(4) 0.4795(6) 0.2015(3) 0.048(2) Uani 1 d . . N7 N 0.7574(4) 0.5544(4) 0.2077(3) 0.0431(14) Uani 1 d . . C8 C 0.7364(6) 0.4193(6) 0.1509(4) 0.061(2) Uani 1 d . . H8A H 0.6857(6) 0.4013(6) 0.1349(4) 0.092 Uiso 1 d R . H8B H 0.7660(6) 0.3682(6) 0.1632(4) 0.092 Uiso 1 d R . H8C H 0.7652(6) 0.4503(6) 0.1225(4) 0.092 Uiso 1 d R . C9 C 0.5942(5) 0.5692(6) 0.3702(3) 0.049(2) Uani 1 d . . N9 N 0.6373(3) 0.6386(4) 0.3629(3) 0.0438(14) Uani 1 d . . C10 C 0.5352(6) 0.5571(8) 0.4159(4) 0.077(3) Uani 1 d . . H10A H 0.5481(6) 0.5047(8) 0.4373(4) 0.115 Uiso 1 d R . H10B H 0.4829(6) 0.5515(8) 0.3987(4) 0.115 Uiso 1 d R . H10C H 0.5369(6) 0.6072(8) 0.4409(4) 0.115 Uiso 1 d R . C11 C 0.8113(5) 0.5884(6) 0.1665(4) 0.051(2) Uani 1 d . . C12 C 0.7834(5) 0.6385(6) 0.1215(4) 0.054(2) Uani 1 d . . C13 C 0.8375(7) 0.6804(7) 0.0880(4) 0.074(3) Uani 1 d . . H13A H 0.8190(7) 0.7165(7) 0.0584(4) 0.089 Uiso 1 calc R . C14 C 0.9180(7) 0.6702(7) 0.0973(5) 0.076(3) Uani 1 d . . C15 C 0.9448(6) 0.6154(7) 0.1399(5) 0.074(3) Uani 1 d . . H15A H 0.9993(6) 0.6064(7) 0.1450(5) 0.089 Uiso 1 calc R . C16 C 0.8937(5) 0.5723(6) 0.1762(4) 0.056(2) Uani 1 d . . C17 C 0.6948(6) 0.6471(8) 0.1072(4) 0.071(3) Uani 1 d . . H17A H 0.6870(6) 0.6809(8) 0.0728(4) 0.106 Uiso 1 d R . H17B H 0.6693(6) 0.6764(8) 0.1379(4) 0.106 Uiso 1 d R . H17C H 0.6721(6) 0.5895(8) 0.1018(4) 0.106 Uiso 1 d R . C18 C 0.9772(9) 0.7191(11) 0.0596(8) 0.132(6) Uani 1 d U . H18A H 0.9713(9) 0.7816(11) 0.0645(8) 0.198 Uiso 1 d R . H18B H 0.9666(9) 0.7040(11) 0.0203(8) 0.198 Uiso 1 d R . H18C H 1.0305(9) 0.7020(11) 0.0706(8) 0.198 Uiso 1 d R . C19 C 0.9241(5) 0.5082(7) 0.2209(5) 0.071(3) Uani 1 d . . H19A H 0.8991(5) 0.4519(7) 0.2146(5) 0.106 Uiso 1 d R . H19B H 0.9119(5) 0.5297(7) 0.2581(5) 0.106 Uiso 1 d R . H19C H 0.9806(5) 0.5020(7) 0.2183(5) 0.106 Uiso 1 d R . C20 C 0.6260(4) 0.7153(6) 0.3994(3) 0.044(2) Uani 1 d . . C21 C 0.6771(5) 0.7270(6) 0.4465(3) 0.051(2) Uani 1 d . . C22 C 0.6694(5) 0.8067(6) 0.4768(4) 0.058(2) Uani 1 d . . H22A H 0.7030(5) 0.8166(6) 0.5085(4) 0.069 Uiso 1 calc R . C23 C 0.6148(5) 0.8705(6) 0.4618(4) 0.059(2) Uani 1 d . . C24 C 0.5635(5) 0.8535(6) 0.4157(4) 0.055(2) Uani 1 d . . H24A H 0.5255(5) 0.8956(6) 0.4053(4) 0.065 Uiso 1 calc R . C25 C 0.5668(5) 0.7746(6) 0.3842(3) 0.052(2) Uani 1 d . . C26 C 0.7368(6) 0.6601(7) 0.4663(4) 0.065(2) Uani 1 d . . H26A H 0.7747(6) 0.6511(7) 0.4372(4) 0.097 Uiso 1 d R . H26B H 0.7103(6) 0.6055(7) 0.4738(4) 0.097 Uiso 1 d R . H26C H 0.7638(6) 0.6805(7) 0.5006(4) 0.097 Uiso 1 d R . C27 C 0.6107(7) 0.9570(8) 0.4939(6) 0.091(4) Uani 1 d . . H27A H 0.5563(7) 0.9711(8) 0.5005(6) 0.136 Uiso 1 d R . H27B H 0.6339(7) 1.0030(8) 0.4717(6) 0.136 Uiso 1 d R . H27C H 0.6395(7) 0.9517(8) 0.5298(6) 0.136 Uiso 1 d R . C28 C 0.5071(5) 0.7583(8) 0.3364(4) 0.070(3) Uani 1 d . . H28A H 0.5320(5) 0.7655(8) 0.3005(4) 0.105 Uiso 1 d R . H28B H 0.4641(5) 0.7995(8) 0.3389(4) 0.105 Uiso 1 d R . H28C H 0.4869(5) 0.6992(8) 0.3392(4) 0.105 Uiso 1 d R . Mn' Mn 0.20328(7) -0.03713(8) 0.27859(5) 0.0400(3) Uani 1 d . . Br1' Br 0.32676(5) -0.02339(7) 0.34024(4) 0.0576(2) Uani 1 d . . Br2' Br 0.17150(6) 0.10225(7) 0.22700(4) 0.0649(3) Uani 1 d . . N1' N 0.1407(3) -0.1651(4) 0.2782(3) 0.0396(13) Uani 1 d . . C2' C 0.1603(4) -0.2281(5) 0.2409(3) 0.045(2) Uani 1 d . . C3' C 0.1308(5) -0.3134(6) 0.2445(4) 0.055(2) Uani 1 d . . H3'A H 0.1458(5) -0.3573(6) 0.2193(4) 0.066 Uiso 1 calc R . C4' C 0.0777(5) -0.3304(6) 0.2876(4) 0.063(2) Uani 1 d . . H4'A H 0.0564(5) -0.3867(6) 0.2909(4) 0.076 Uiso 1 calc R . C5' C 0.0563(5) -0.2664(6) 0.3248(4) 0.054(2) Uani 1 d . . H5'A H 0.0203(5) -0.2779(6) 0.3530(4) 0.065 Uiso 1 calc R . C6' C 0.0900(4) -0.1831(5) 0.3193(3) 0.044(2) Uani 1 d . . C7' C 0.2164(5) -0.1993(6) 0.1969(3) 0.048(2) Uani 1 d . . N7' N 0.2445(4) -0.1218(4) 0.2025(3) 0.0426(14) Uani 1 d . . C8' C 0.2371(6) -0.2637(6) 0.1506(4) 0.066(2) Uani 1 d . . H8'1 H 0.1903(6) -0.2772(6) 0.1277(4) 0.098 Uiso 1 d R . H8'2 H 0.2578(6) -0.3169(6) 0.1677(4) 0.098 Uiso 1 d R . H8'3 H 0.2764(6) -0.2381(6) 0.1270(4) 0.098 Uiso 1 d R . C9' C 0.0697(4) -0.1063(5) 0.3566(3) 0.045(2) Uani 1 d . . N9' N 0.1082(3) -0.0348(4) 0.3493(3) 0.0391(13) Uani 1 d . . C10' C 0.0074(5) -0.1194(7) 0.4007(4) 0.064(2) Uani 1 d . . H10D H 0.0277(5) -0.1582(7) 0.4301(4) 0.096 Uiso 1 d R . H10E H -0.0394(5) -0.1448(7) 0.3828(4) 0.096 Uiso 1 d R . H10F H -0.0056(5) -0.0634(7) 0.4171(4) 0.096 Uiso 1 d R . C11' C 0.2974(4) -0.0849(5) 0.1623(3) 0.042(2) Uani 1 d . . C12' C 0.2668(5) -0.0386(6) 0.1156(3) 0.050(2) Uani 1 d . . C13' C 0.3189(6) 0.0090(6) 0.0827(4) 0.062(2) Uani 1 d . . H13B H 0.2988(6) 0.0436(6) 0.0527(4) 0.074 Uiso 1 calc R . C14' C 0.4009(6) 0.0059(6) 0.0937(4) 0.063(2) Uani 1 d . . C15' C 0.4289(5) -0.0441(6) 0.1380(4) 0.054(2) Uani 1 d . . H15B H 0.4835(5) -0.0457(6) 0.1456(4) 0.064 Uiso 1 calc R . C16' C 0.3799(5) -0.0935(5) 0.1729(3) 0.049(2) Uani 1 d . . C17' C 0.1780(6) -0.0366(8) 0.1016(4) 0.070(3) Uani 1 d . . H17D H 0.1667(6) 0.0079(8) 0.0733(4) 0.105 Uiso 1 d R . H17E H 0.1500(6) -0.0232(8) 0.1355(4) 0.105 Uiso 1 d R . H17F H 0.1612(6) -0.0931(8) 0.0871(4) 0.105 Uiso 1 d R . C18' C 0.4551(8) 0.0619(8) 0.0586(5) 0.095(4) Uani 1 d . . H18D H 0.4456(8) 0.1232(8) 0.0663(5) 0.142 Uiso 1 d R . H18E H 0.4447(8) 0.0503(8) 0.0188(5) 0.142 Uiso 1 d R . H18F H 0.5095(8) 0.0479(8) 0.0685(5) 0.142 Uiso 1 d R . C19' C 0.4129(5) -0.1506(6) 0.2197(4) 0.059(2) Uani 1 d . . H19D H 0.3919(5) -0.2092(6) 0.2153(4) 0.088 Uiso 1 d R . H19E H 0.3982(5) -0.1271(6) 0.2558(4) 0.088 Uiso 1 d R . H19F H 0.4697(5) -0.1524(6) 0.2180(4) 0.088 Uiso 1 d R . C20' C 0.0913(4) 0.0423(5) 0.3829(3) 0.043(2) Uani 1 d . . C21' C 0.1285(4) 0.0546(5) 0.4356(3) 0.045(2) Uani 1 d . . C22' C 0.1135(5) 0.1334(6) 0.4648(4) 0.055(2) Uani 1 d . . H22B H 0.1391(5) 0.1433(6) 0.5001(4) 0.066 Uiso 1 calc R . C23' C 0.0623(5) 0.1964(6) 0.4432(4) 0.055(2) Uani 1 d . . C24' C 0.0248(5) 0.1806(6) 0.3901(4) 0.053(2) Uani 1 d . . H24B H -0.0097(5) 0.2229(6) 0.3746(4) 0.063 Uiso 1 calc R . C25' C 0.0375(5) 0.1042(6) 0.3599(4) 0.048(2) Uani 1 d . . C26' C 0.1826(6) -0.0141(7) 0.4637(4) 0.065(2) Uani 1 d . . H26D H 0.2048(6) 0.0088(7) 0.4990(4) 0.098 Uiso 1 d R . H26E H 0.2247(6) -0.0282(7) 0.4387(4) 0.098 Uiso 1 d R . H26F H 0.1524(6) -0.0663(7) 0.4711(4) 0.098 Uiso 1 d R . C27' C 0.0473(7) 0.2809(8) 0.4754(5) 0.086(3) Uani 1 d . . H27D H 0.0859(7) 0.3244(8) 0.4655(5) 0.129 Uiso 1 d R . H27E H 0.0514(7) 0.2697(8) 0.5158(5) 0.129 Uiso 1 d R . H27F H -0.0051(7) 0.3023(8) 0.4655(5) 0.129 Uiso 1 d R . C28' C -0.0085(5) 0.0876(7) 0.3044(4) 0.062(2) Uani 1 d . . H28D H -0.0393(5) 0.1389(7) 0.2942(4) 0.093 Uiso 1 d R . H28E H -0.0433(5) 0.0381(7) 0.3089(4) 0.093 Uiso 1 d R . H28F H 0.0279(5) 0.0751(7) 0.2748(4) 0.093 Uiso 1 d R . N30 N 0.6720(24) 0.4084(31) 0.4649(12) 0.092(10) Uani 0.50 d PU 1 C31 C 0.7263(25) 0.4063(32) 0.4358(22) 0.069(10) Uani 0.50 d PU 1 C32 C 0.7950(24) 0.4020(31) 0.4050(19) 0.109(12) Uani 0.50 d PU 1 H32A H 0.8042(24) 0.4581(31) 0.3875(19) 0.163 Uiso 0.50 d PR 1 H32B H 0.7887(24) 0.3576(31) 0.3760(19) 0.163 Uiso 0.50 d PR 1 H32C H 0.8393(24) 0.3872(31) 0.4301(19) 0.163 Uiso 0.50 d PR 1 N30' N 0.6969(23) 0.4089(31) 0.4474(16) 0.082(12) Uani 0.50 d PU 2 C31' C 0.7576(21) 0.4121(28) 0.4272(18) 0.076(9) Uani 0.50 d PU 2 C32' C 0.8307(21) 0.4196(27) 0.3969(21) 0.116(12) Uani 0.50 d PU 2 H32D H 0.8711(21) 0.3845(27) 0.4159(21) 0.174 Uiso 0.50 d PR 2 H32E H 0.8472(21) 0.4802(27) 0.3964(21) 0.174 Uiso 0.50 d PR 2 H32F H 0.8223(21) 0.3990(27) 0.3584(21) 0.174 Uiso 0.50 d PR 2 N40 N 0.1714(8) -0.2508(8) 0.4601(6) 0.112(4) Uani 1 d . . C41 C 0.2284(9) -0.2556(8) 0.4366(5) 0.085(3) Uani 1 d . . C42 C 0.3016(11) -0.2599(12) 0.4073(8) 0.137(6) Uani 1 d . . H42A H 0.2949(11) -0.2978(12) 0.3746(8) 0.205 Uiso 1 d R . H42B H 0.3426(11) -0.2830(12) 0.4325(8) 0.205 Uiso 1 d R . H42C H 0.3161(11) -0.2018(12) 0.3951(8) 0.205 Uiso 1 d 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 Mn 0.0403(6) 0.0422(7) 0.0450(6) 0.0014(5) 0.0017(5) -0.0038(5) Br1 0.0455(4) 0.0753(7) 0.0700(5) 0.0076(5) -0.0053(4) -0.0091(4) Br2 0.0679(5) 0.0475(5) 0.0590(5) 0.0041(4) -0.0037(4) 0.0022(4) N1 0.038(3) 0.050(4) 0.040(3) 0.001(3) -0.003(3) -0.001(3) C2 0.038(4) 0.042(4) 0.049(4) 0.002(3) -0.006(3) 0.005(3) C3 0.056(5) 0.047(5) 0.066(5) -0.007(4) -0.004(4) 0.001(4) C4 0.068(5) 0.051(5) 0.075(6) -0.003(5) 0.004(5) -0.019(4) C5 0.076(6) 0.060(6) 0.063(5) 0.000(4) 0.018(5) -0.032(5) C6 0.043(4) 0.056(5) 0.046(4) 0.003(4) -0.003(4) -0.002(3) C7 0.049(4) 0.046(5) 0.048(4) -0.003(4) -0.003(4) 0.003(4) N7 0.039(3) 0.041(4) 0.050(3) 0.002(3) 0.006(3) 0.002(3) C8 0.068(5) 0.050(5) 0.065(5) -0.005(4) -0.006(5) 0.015(4) C9 0.052(4) 0.050(5) 0.045(4) 0.005(4) -0.004(4) -0.006(4) N9 0.039(3) 0.049(4) 0.043(3) 0.004(3) -0.002(3) -0.007(3) C10 0.071(6) 0.096(8) 0.065(6) -0.015(6) 0.028(5) -0.028(6) C11 0.047(4) 0.045(5) 0.062(5) -0.003(4) 0.010(4) 0.006(3) C12 0.059(5) 0.057(5) 0.047(4) -0.005(4) 0.009(4) 0.016(4) C13 0.099(8) 0.066(6) 0.061(6) 0.008(5) 0.041(6) 0.011(6) C14 0.086(7) 0.066(6) 0.078(7) -0.010(5) 0.044(6) 0.000(5) C15 0.054(5) 0.073(7) 0.097(8) -0.009(6) 0.029(5) 0.011(5) C16 0.054(5) 0.045(5) 0.068(5) -0.005(4) 0.018(4) 0.002(4) C17 0.068(6) 0.093(8) 0.052(5) -0.001(5) 0.011(5) 0.022(5) C18 0.140(12) 0.102(11) 0.160(14) 0.015(10) 0.097(12) -0.005(9) C19 0.043(4) 0.075(7) 0.094(7) 0.003(6) 0.001(5) 0.014(4) C20 0.039(4) 0.055(5) 0.038(3) 0.005(3) 0.007(3) 0.000(3) C21 0.051(4) 0.063(5) 0.039(4) 0.004(4) 0.007(4) -0.003(4) C22 0.062(5) 0.068(6) 0.042(4) -0.006(4) -0.001(4) -0.016(4) C23 0.058(5) 0.061(6) 0.058(5) -0.007(4) 0.018(4) -0.005(4) C24 0.048(4) 0.059(5) 0.058(5) 0.002(4) 0.018(4) 0.002(4) C25 0.044(4) 0.069(6) 0.043(4) 0.002(4) 0.000(4) 0.002(4) C26 0.071(6) 0.071(6) 0.050(5) 0.014(4) -0.016(4) 0.016(5) C27 0.085(7) 0.079(8) 0.108(9) -0.026(7) 0.013(7) -0.003(6) C28 0.057(5) 0.100(8) 0.052(5) -0.013(5) -0.006(4) 0.022(5) Mn' 0.0445(6) 0.0345(6) 0.0413(6) -0.0008(5) 0.0045(5) -0.0037(5) Br1' 0.0542(5) 0.0609(5) 0.0571(5) -0.0019(4) -0.0047(4) -0.0045(4) Br2' 0.0830(6) 0.0490(5) 0.0631(5) 0.0123(4) 0.0060(5) 0.0117(5) N1' 0.046(3) 0.031(3) 0.042(3) -0.001(3) 0.004(3) -0.003(3) C2' 0.049(4) 0.038(4) 0.047(4) 0.002(3) -0.001(3) -0.002(3) C3' 0.055(5) 0.042(5) 0.068(5) -0.007(4) 0.003(4) -0.007(4) C4' 0.068(5) 0.047(5) 0.076(6) -0.002(5) 0.007(5) -0.018(4) C5' 0.053(4) 0.045(5) 0.064(5) -0.003(4) 0.007(4) -0.009(4) C6' 0.042(4) 0.043(4) 0.046(4) 0.006(3) 0.000(3) -0.002(3) C7' 0.053(4) 0.045(5) 0.045(4) -0.006(3) 0.002(4) 0.002(3) N7' 0.051(3) 0.037(3) 0.041(3) -0.001(3) 0.005(3) -0.004(3) C8' 0.089(6) 0.047(5) 0.062(5) -0.014(4) 0.012(5) -0.002(5) C9' 0.040(4) 0.048(5) 0.046(4) -0.001(3) 0.000(3) -0.001(3) N9' 0.038(3) 0.037(3) 0.042(3) -0.003(3) 0.008(3) 0.003(3) C10' 0.064(5) 0.068(6) 0.062(5) 0.003(5) 0.028(5) -0.009(4) C11' 0.050(4) 0.046(4) 0.031(3) -0.002(3) 0.008(3) 0.010(3) C12' 0.055(4) 0.054(5) 0.041(4) -0.004(4) -0.003(4) 0.011(4) C13' 0.088(6) 0.054(5) 0.045(4) 0.004(4) 0.011(5) 0.001(5) C14' 0.079(6) 0.051(5) 0.061(5) 0.005(4) 0.027(5) -0.011(4) C15' 0.053(4) 0.053(5) 0.055(5) -0.014(4) 0.014(4) -0.003(4) C16' 0.056(4) 0.041(4) 0.049(4) -0.006(3) 0.006(4) 0.003(4) C17' 0.074(6) 0.083(7) 0.052(5) 0.001(5) 0.000(5) 0.020(5) C18' 0.134(10) 0.067(7) 0.088(7) -0.005(6) 0.071(8) -0.021(7) C19' 0.060(5) 0.061(6) 0.056(5) 0.007(4) 0.004(4) 0.013(4) C20' 0.043(4) 0.045(4) 0.041(4) -0.006(3) 0.009(3) -0.002(3) C21' 0.045(4) 0.045(4) 0.045(4) 0.003(3) 0.012(3) 0.003(3) C22' 0.057(5) 0.064(6) 0.046(4) -0.010(4) 0.007(4) -0.012(4) C23' 0.054(5) 0.051(5) 0.062(5) -0.009(4) 0.023(4) -0.007(4) C24' 0.044(4) 0.059(5) 0.056(5) 0.005(4) 0.012(4) 0.006(4) C25' 0.045(4) 0.049(5) 0.051(4) -0.004(4) 0.005(4) 0.001(3) C26' 0.074(6) 0.072(6) 0.049(4) 0.007(4) -0.008(4) 0.016(5) C27' 0.106(8) 0.062(7) 0.092(8) -0.018(6) 0.018(7) 0.009(6) C28' 0.042(4) 0.072(6) 0.071(6) 0.002(5) 0.001(4) 0.007(4) N30 0.127(24) 0.096(16) 0.052(14) -0.016(13) -0.001(14) 0.000(17) C31 0.073(19) 0.061(12) 0.073(16) -0.013(11) 0.004(15) -0.006(15) C32 0.129(26) 0.110(22) 0.089(17) -0.007(17) 0.027(20) -0.018(21) N30' 0.096(24) 0.079(15) 0.073(23) 0.010(17) 0.006(18) 0.012(18) C31' 0.076(17) 0.081(14) 0.071(15) -0.003(12) -0.010(14) 0.002(14) C32' 0.119(23) 0.096(20) 0.133(24) -0.037(18) 0.005(21) -0.023(18) N40 0.124(9) 0.087(8) 0.125(10) -0.019(7) -0.006(9) 0.014(7) C41 0.124(11) 0.068(7) 0.062(6) -0.006(5) -0.008(7) 0.000(7) C42 0.185(17) 0.105(12) 0.125(13) 0.013(10) 0.053(13) 0.014(12) _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 Mn N1 2.202(7) . ? Mn N9 2.330(6) . ? Mn N7 2.330(7) . ? Mn Br2 2.485(2) . ? Mn Br1 2.4965(15) . ? N1 C2 1.328(10) . ? N1 C6 1.344(10) . ? C2 C3 1.359(12) . ? C2 C7 1.510(11) . ? C3 C4 1.374(13) . ? C4 C5 1.384(14) . ? C5 C6 1.370(12) . ? C6 C9 1.506(12) . ? C7 N7 1.270(10) . ? C7 C8 1.516(12) . ? N7 C11 1.442(10) . ? C9 N9 1.292(10) . ? C9 C10 1.496(12) . ? N9 C20 1.461(10) . ? C11 C12 1.369(12) . ? C11 C16 1.419(12) . ? C12 C13 1.378(13) . ? C12 C17 1.524(12) . ? C13 C14 1.38(2) . ? C14 C15 1.36(2) . ? C14 C18 1.54(2) . ? C15 C16 1.394(14) . ? C16 C19 1.504(14) . ? C20 C25 1.380(11) . ? C20 C21 1.387(11) . ? C21 C22 1.409(13) . ? C21 C26 1.490(12) . ? C22 C23 1.371(13) . ? C23 C24 1.383(13) . ? C23 C27 1.513(14) . ? C24 C25 1.409(13) . ? C25 C28 1.499(12) . ? Mn' N1' 2.207(6) . ? Mn' N7' 2.322(6) . ? Mn' N9' 2.345(6) . ? Mn' Br2' 2.483(2) . ? Mn' Br1' 2.4982(15) . ? N1' C6' 1.338(10) . ? N1' C2' 1.343(10) . ? C2' C3' 1.389(11) . ? C2' C7' 1.489(11) . ? C3' C4' 1.396(13) . ? C4' C5' 1.361(13) . ? C5' C6' 1.391(11) . ? C6' C9' 1.502(11) . ? C7' N7' 1.272(10) . ? C7' C8' 1.510(11) . ? N7' C11' 1.434(10) . ? C9' N9' 1.277(10) . ? C9' C10' 1.511(11) . ? N9' C20' 1.445(9) . ? C11' C12' 1.384(11) . ? C11' C16' 1.409(11) . ? C12' C13' 1.390(13) . ? C12' C17' 1.521(12) . ? C13' C14' 1.396(14) . ? C14' C15' 1.356(13) . ? C14' C18' 1.512(12) . ? C15' C16' 1.399(12) . ? C16' C19' 1.489(12) . ? C20' C21' 1.378(11) . ? C20' C25' 1.398(11) . ? C21' C22' 1.404(12) . ? C21' C26' 1.517(12) . ? C22' C23' 1.371(13) . ? C23' C24' 1.397(13) . ? C23' C27' 1.512(13) . ? C24' C25' 1.376(12) . ? C25' C28' 1.512(12) . ? N30 C31 1.16(6) . ? C31 C32 1.39(5) . ? N30' C31' 1.14(5) . ? C31' C32' 1.45(5) . ? N40 C41 1.13(2) . ? C41 C42 1.43(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 Mn N9 71.2(2) . . ? N1 Mn N7 71.3(2) . . ? N9 Mn N7 142.6(2) . . ? N1 Mn Br2 125.3(2) . . ? N9 Mn Br2 99.3(2) . . ? N7 Mn Br2 100.9(2) . . ? N1 Mn Br1 122.2(2) . . ? N9 Mn Br1 100.2(2) . . ? N7 Mn Br1 100.8(2) . . ? Br2 Mn Br1 112.51(6) . . ? C2 N1 C6 119.6(7) . . ? C2 N1 Mn 120.1(5) . . ? C6 N1 Mn 120.3(5) . . ? N1 C2 C3 122.1(8) . . ? N1 C2 C7 114.8(7) . . ? C3 C2 C7 123.1(8) . . ? C2 C3 C4 119.5(8) . . ? C3 C4 C5 118.3(8) . . ? C6 C5 C4 119.6(8) . . ? N1 C6 C5 120.8(8) . . ? N1 C6 C9 115.1(7) . . ? C5 C6 C9 124.0(8) . . ? N7 C7 C2 116.8(7) . . ? N7 C7 C8 123.8(8) . . ? C2 C7 C8 119.4(7) . . ? C7 N7 C11 121.8(7) . . ? C7 N7 Mn 116.7(5) . . ? C11 N7 Mn 121.3(5) . . ? N9 C9 C10 125.9(8) . . ? N9 C9 C6 115.8(7) . . ? C10 C9 C6 118.3(8) . . ? C9 N9 C20 118.9(7) . . ? C9 N9 Mn 117.4(6) . . ? C20 N9 Mn 123.4(5) . . ? C12 C11 C16 121.7(8) . . ? C12 C11 N7 120.4(7) . . ? C16 C11 N7 117.8(8) . . ? C11 C12 C13 118.5(9) . . ? C11 C12 C17 121.6(8) . . ? C13 C12 C17 119.8(9) . . ? C14 C13 C12 121.9(10) . . ? C15 C14 C13 118.8(10) . . ? C15 C14 C18 120.5(12) . . ? C13 C14 C18 120.7(12) . . ? C14 C15 C16 122.5(9) . . ? C15 C16 C11 116.4(9) . . ? C15 C16 C19 121.6(8) . . ? C11 C16 C19 121.9(8) . . ? C25 C20 C21 123.0(8) . . ? C25 C20 N9 118.4(7) . . ? C21 C20 N9 118.6(7) . . ? C20 C21 C22 116.4(8) . . ? C20 C21 C26 123.5(8) . . ? C22 C21 C26 120.0(8) . . ? C23 C22 C21 123.3(8) . . ? C22 C23 C24 117.6(9) . . ? C22 C23 C27 121.7(9) . . ? C24 C23 C27 120.7(10) . . ? C23 C24 C25 122.2(8) . . ? C20 C25 C24 117.3(8) . . ? C20 C25 C28 123.0(9) . . ? C24 C25 C28 119.6(8) . . ? N1' Mn' N7' 70.6(2) . . ? N1' Mn' N9' 71.2(2) . . ? N7' Mn' N9' 141.3(2) . . ? N1' Mn' Br2' 130.6(2) . . ? N7' Mn' Br2' 99.3(2) . . ? N9' Mn' Br2' 101.0(2) . . ? N1' Mn' Br1' 117.6(2) . . ? N7' Mn' Br1' 103.0(2) . . ? N9' Mn' Br1' 99.5(2) . . ? Br2' Mn' Br1' 111.79(6) . . ? C6' N1' C2' 120.1(6) . . ? C6' N1' Mn' 119.5(5) . . ? C2' N1' Mn' 119.9(5) . . ? N1' C2' C3' 121.7(7) . . ? N1' C2' C7' 114.8(7) . . ? C3' C2' C7' 123.5(8) . . ? C2' C3' C4' 117.1(8) . . ? C5' C4' C3' 121.5(8) . . ? C4' C5' C6' 118.0(8) . . ? N1' C6' C5' 121.6(7) . . ? N1' C6' C9' 115.1(7) . . ? C5' C6' C9' 123.2(7) . . ? N7' C7' C2' 116.2(7) . . ? N7' C7' C8' 125.3(8) . . ? C2' C7' C8' 118.5(7) . . ? C7' N7' C11' 121.9(7) . . ? C7' N7' Mn' 118.1(5) . . ? C11' N7' Mn' 120.0(5) . . ? N9' C9' C6' 116.9(7) . . ? N9' C9' C10' 124.8(8) . . ? C6' C9' C10' 118.3(7) . . ? C9' N9' C20' 120.2(6) . . ? C9' N9' Mn' 116.4(5) . . ? C20' N9' Mn' 123.4(4) . . ? C12' C11' C16' 121.5(7) . . ? C12' C11' N7' 119.7(7) . . ? C16' C11' N7' 118.7(7) . . ? C11' C12' C13' 118.5(8) . . ? C11' C12' C17' 121.1(8) . . ? C13' C12' C17' 120.4(8) . . ? C12' C13' C14' 121.2(9) . . ? C15' C14' C13' 118.5(8) . . ? C15' C14' C18' 121.9(10) . . ? C13' C14' C18' 119.5(10) . . ? C14' C15' C16' 123.3(8) . . ? C15' C16' C11' 116.5(8) . . ? C15' C16' C19' 121.9(8) . . ? C11' C16' C19' 121.5(7) . . ? C21' C20' C25' 121.5(7) . . ? C21' C20' N9' 120.4(7) . . ? C25' C20' N9' 118.1(7) . . ? C20' C21' C22' 117.8(8) . . ? C20' C21' C26' 122.9(8) . . ? C22' C21' C26' 119.3(8) . . ? C23' C22' C21' 122.3(8) . . ? C22' C23' C24' 117.9(8) . . ? C22' C23' C27' 121.3(9) . . ? C24' C23' C27' 120.8(9) . . ? C25' C24' C23' 121.8(8) . . ? C24' C25' C20' 118.5(8) . . ? C24' C25' C28' 119.8(8) . . ? C20' C25' C28' 121.7(8) . . ? N30 C31 C32 175.4(57) . . ? N30' C31' C32' 174.5(43) . . ? N40 C41 C42 178.8(15) . . ? _refine_diff_density_max 0.546 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.082 data_VG9761 _database_code_CSD 190872 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C25 H28 N6 Cl2 Mn' _chemical_formula_weight 538.37 _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' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7366(9) _cell_length_b 13.2107(10) _cell_length_c 15.1806(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.911(6) _cell_angle_gamma 90.00 _cell_volume 2695.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 19 _cell_measurement_theta_min 11.01 _cell_measurement_theta_max 19.97 _exptl_crystal_description plates _exptl_crystal_colour Orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method ? _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 5.993 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.5472 _exptl_absorpt_correction_T_max 0.7682 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4169 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0843 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 59.98 _reflns_number_total 3982 _reflns_number_observed 2650 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0464P)^2^+2.1364P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00111(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3982 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_obs 0.0589 _refine_ls_wR_factor_all 0.1461 _refine_ls_wR_factor_obs 0.1213 _refine_ls_goodness_of_fit_all 1.051 _refine_ls_goodness_of_fit_obs 1.087 _refine_ls_restrained_S_all 1.051 _refine_ls_restrained_S_obs 1.087 _refine_ls_shift/esd_max 0.000 _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 Mn Mn 0.23474(7) 0.17275(6) 0.01356(6) 0.0395(2) Uani 1 d . . Cl1 Cl 0.27745(12) 0.03474(12) -0.06882(10) 0.0561(4) Uani 1 d . . Cl2 Cl 0.2629(2) 0.34426(11) -0.00778(14) 0.0767(5) Uani 1 d . . N1 N 0.1577(3) 0.1175(3) 0.1155(3) 0.0373(9) Uani 1 d . . C2 C 0.0593(4) 0.1020(4) 0.0954(3) 0.0374(11) Uani 1 d . . C3 C 0.0105(5) 0.0536(4) 0.1542(4) 0.0466(13) Uani 1 d . . H3A H -0.0580(5) 0.0438(4) 0.1395(4) 0.056 Uiso 1 calc R . C4 C 0.0661(5) 0.0197(4) 0.2357(4) 0.0501(14) Uani 1 d . . H4A H 0.0349(5) -0.0132(4) 0.2764(4) 0.060 Uiso 1 calc R . C5 C 0.1659(4) 0.0344(4) 0.2562(4) 0.0460(12) Uani 1 d . . H5A H 0.2032(4) 0.0117(4) 0.3109(4) 0.055 Uiso 1 calc R . C6 C 0.2124(4) 0.0840(4) 0.1947(3) 0.0385(11) Uani 1 d . . C7 C 0.0071(4) 0.1396(3) 0.0054(4) 0.0391(11) Uani 1 d . . N8 N 0.0643(3) 0.1709(3) -0.0464(3) 0.0409(9) Uani 1 d . . N9 N 0.0189(4) 0.2045(4) -0.1323(3) 0.0499(12) Uani 1 d . . C10 C 0.3203(4) 0.1037(4) 0.2102(3) 0.0437(12) Uani 1 d . . N11 N 0.3523(3) 0.1449(3) 0.1449(3) 0.0402(10) Uani 1 d . . N12 N 0.4532(3) 0.1656(4) 0.1571(3) 0.0516(12) Uani 1 d . . C13 C -0.1037(4) 0.1356(4) -0.0192(4) 0.0514(14) Uani 1 d . . H13A H -0.1308(4) 0.1955(4) 0.0024(4) 0.077 Uiso 1 d R . H13B H -0.1270(4) 0.0770(4) 0.0077(4) 0.077 Uiso 1 d R . H13C H -0.1247(4) 0.1319(4) -0.0835(4) 0.077 Uiso 1 d R . C14 C 0.3850(5) 0.0715(6) 0.2974(4) 0.061(2) Uani 1 d . . H14A H 0.3630(5) 0.0070(6) 0.3149(4) 0.092 Uiso 1 d R . H14B H 0.3810(5) 0.1207(6) 0.3431(4) 0.092 Uiso 1 d R . H14C H 0.4527(5) 0.0661(6) 0.2903(4) 0.092 Uiso 1 d R . C15 C 0.0900(6) 0.2061(5) -0.1922(4) 0.063(2) Uani 1 d . . H15A H 0.1300(6) 0.1459(5) -0.1830(4) 0.094 Uiso 1 calc R . H15B H 0.1321(6) 0.2645(5) -0.1791(4) 0.094 Uiso 1 calc R . H15C H 0.0545(6) 0.2089(5) -0.2536(4) 0.094 Uiso 1 calc R . C16 C -0.0409(3) 0.3601(3) -0.0702(3) 0.068(2) Uani 1 d G . H16A H 0.0039(3) 0.3508(3) -0.0159(3) 0.081 Uiso 1 calc R . C17 C -0.1038(4) 0.4437(3) -0.0821(4) 0.092(3) Uani 1 d G . H17A H -0.1010(6) 0.4903(4) -0.0357(5) 0.111 Uiso 1 calc R . C18 C -0.1709(4) 0.4575(3) -0.1633(5) 0.109(4) Uani 1 d G . H18A H -0.2129(5) 0.5134(4) -0.1712(6) 0.131 Uiso 1 calc R . C19 C -0.1750(3) 0.3879(4) -0.2326(3) 0.101(4) Uani 1 d G . H19A H -0.2199(4) 0.3972(6) -0.2869(4) 0.122 Uiso 1 calc R . C20 C -0.1122(3) 0.3043(4) -0.2207(3) 0.072(2) Uani 1 d G . H20A H -0.1150(5) 0.2577(5) -0.2671(3) 0.086 Uiso 1 calc R . C21 C -0.0451(3) 0.2905(3) -0.1395(3) 0.0507(14) Uani 1 d G . C22 C 0.4847(5) 0.1710(7) 0.0712(5) 0.073(2) Uani 1 d . . H22A H 0.4535(5) 0.1178(7) 0.0324(5) 0.109 Uiso 1 calc R . H22B H 0.5557(5) 0.1636(7) 0.0812(5) 0.109 Uiso 1 calc R . H22C H 0.4658(5) 0.2353(7) 0.0434(5) 0.109 Uiso 1 calc R . C23 C 0.5972(3) 0.2422(4) 0.2497(3) 0.078(2) Uani 1 d G . H23A H 0.6358(3) 0.1979(4) 0.2237(3) 0.093 Uiso 1 calc R . C24 C 0.6426(3) 0.3094(4) 0.3160(4) 0.087(3) Uani 1 d G . H24A H 0.7115(3) 0.3101(6) 0.3344(5) 0.105 Uiso 1 calc R . C25 C 0.5849(4) 0.3756(4) 0.3549(3) 0.082(2) Uani 1 d G . H25A H 0.6153(5) 0.4205(5) 0.3993(4) 0.099 Uiso 1 calc R . C26 C 0.4819(4) 0.3745(4) 0.3275(3) 0.086(3) Uani 1 d G . H26A H 0.4434(5) 0.4187(5) 0.3535(5) 0.104 Uiso 1 calc R . C27 C 0.4366(2) 0.3072(4) 0.2612(3) 0.068(2) Uani 1 d G . H27A H 0.3677(2) 0.3065(5) 0.2428(5) 0.082 Uiso 1 calc R . C28 C 0.4942(3) 0.2411(3) 0.2223(3) 0.0474(13) Uani 1 d G . N30 N 0.7636(10) 0.3319(9) 0.0874(6) 0.137(4) Uani 1 d . . C31 C 0.6995(9) 0.3640(7) 0.0368(7) 0.092(3) Uani 1 d . . C32 C 0.6228(9) 0.4036(9) -0.0298(8) 0.124(4) Uani 1 d . . H32A H 0.6419(9) 0.4690(9) -0.0479(8) 0.186 Uiso 1 d R . H32B H 0.5634(9) 0.4098(9) -0.0063(8) 0.186 Uiso 1 d R . H32C H 0.6107(9) 0.3590(9) -0.0808(8) 0.186 Uiso 1 d 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 Mn 0.0454(5) 0.0350(4) 0.0376(4) 0.0014(4) 0.0073(3) -0.0071(4) Cl1 0.0585(8) 0.0529(8) 0.0562(8) -0.0155(6) 0.0104(6) -0.0046(7) Cl2 0.1021(13) 0.0406(8) 0.0848(11) 0.0081(8) 0.0128(9) -0.0184(9) N1 0.043(2) 0.032(2) 0.036(2) 0.001(2) 0.006(2) -0.001(2) C2 0.040(3) 0.028(2) 0.044(3) -0.003(2) 0.007(2) -0.004(2) C3 0.052(3) 0.042(3) 0.049(3) -0.004(2) 0.018(3) -0.009(2) C4 0.060(4) 0.047(3) 0.048(3) 0.007(2) 0.020(3) -0.009(3) C5 0.056(3) 0.045(3) 0.039(3) 0.003(2) 0.013(2) -0.003(3) C6 0.046(3) 0.034(2) 0.035(2) 0.001(2) 0.006(2) 0.001(2) C7 0.048(3) 0.025(2) 0.043(3) 0.001(2) 0.006(2) 0.000(2) N8 0.043(2) 0.036(2) 0.040(2) 0.002(2) 0.000(2) -0.003(2) N9 0.059(3) 0.041(2) 0.045(2) 0.009(2) 0.000(2) 0.000(2) C10 0.045(3) 0.046(3) 0.037(3) -0.001(2) 0.001(2) -0.002(2) N11 0.037(2) 0.044(2) 0.039(2) -0.003(2) 0.004(2) -0.003(2) N12 0.037(2) 0.070(3) 0.045(2) -0.015(2) 0.004(2) -0.009(2) C13 0.042(3) 0.043(3) 0.067(4) 0.004(3) 0.008(3) -0.001(2) C14 0.055(4) 0.079(5) 0.044(3) 0.007(3) -0.004(3) -0.003(3) C15 0.085(5) 0.058(4) 0.045(3) 0.007(3) 0.012(3) 0.004(3) C16 0.058(4) 0.041(3) 0.095(5) 0.010(3) -0.006(4) 0.005(3) C17 0.087(6) 0.051(4) 0.136(8) 0.012(5) 0.018(6) 0.011(4) C18 0.059(5) 0.075(6) 0.190(12) 0.074(7) 0.019(6) 0.014(4) C19 0.049(4) 0.114(8) 0.130(8) 0.085(7) -0.006(5) -0.005(5) C20 0.049(4) 0.088(5) 0.072(4) 0.039(4) -0.003(3) -0.005(3) C21 0.042(3) 0.046(3) 0.059(3) 0.020(3) -0.001(3) 0.000(2) C22 0.053(4) 0.111(6) 0.058(4) -0.021(4) 0.022(3) -0.015(4) C23 0.049(4) 0.083(5) 0.092(5) -0.023(4) -0.006(4) -0.007(4) C24 0.067(5) 0.091(6) 0.093(6) -0.024(5) -0.007(4) -0.020(4) C25 0.094(6) 0.086(5) 0.061(4) -0.015(4) 0.004(4) -0.044(5) C26 0.111(7) 0.073(5) 0.084(5) -0.033(4) 0.041(5) -0.016(5) C27 0.058(4) 0.072(5) 0.076(4) -0.023(4) 0.017(3) -0.011(3) C28 0.042(3) 0.053(3) 0.045(3) -0.009(2) 0.006(2) -0.010(3) N30 0.194(12) 0.121(8) 0.085(5) -0.007(6) 0.002(6) 0.043(8) C31 0.130(9) 0.068(5) 0.080(6) -0.010(4) 0.026(6) -0.005(5) C32 0.126(10) 0.099(8) 0.131(10) 0.004(7) -0.008(8) -0.012(7) _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 Mn N1 2.173(4) . ? Mn N11 2.321(4) . ? Mn N8 2.330(4) . ? Mn Cl2 2.332(2) . ? Mn Cl1 2.353(2) . ? N1 C2 1.338(7) . ? N1 C6 1.354(7) . ? C2 C3 1.379(8) . ? C2 C7 1.491(7) . ? C3 C4 1.387(8) . ? C4 C5 1.356(9) . ? C5 C6 1.399(7) . ? C6 C10 1.475(8) . ? C7 N8 1.290(7) . ? C7 C13 1.491(8) . ? N8 N9 1.396(6) . ? N9 C21 1.426(6) . ? N9 C15 1.465(8) . ? C10 N11 1.285(7) . ? C10 C14 1.497(8) . ? N11 N12 1.387(6) . ? N12 C28 1.436(6) . ? N12 C22 1.458(8) . ? C16 C17 1.39 . ? C16 C21 1.39 . ? C17 C18 1.39 . ? C18 C19 1.39 . ? C19 C20 1.39 . ? C20 C21 1.39 . ? C23 C24 1.39 . ? C23 C28 1.39 . ? C24 C25 1.39 . ? C25 C26 1.39 . ? C26 C27 1.39 . ? C27 C28 1.39 . ? N30 C31 1.125(14) . ? C31 C32 1.402(15) . ? 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 Mn N11 71.9(2) . . ? N1 Mn N8 71.2(2) . . ? N11 Mn N8 143.0(2) . . ? N1 Mn Cl2 122.96(13) . . ? N11 Mn Cl2 99.65(12) . . ? N8 Mn Cl2 97.91(13) . . ? N1 Mn Cl1 109.25(12) . . ? N11 Mn Cl1 97.35(12) . . ? N8 Mn Cl1 97.18(12) . . ? Cl2 Mn Cl1 127.77(7) . . ? C2 N1 C6 120.1(5) . . ? C2 N1 Mn 120.4(3) . . ? C6 N1 Mn 118.6(4) . . ? N1 C2 C3 121.8(5) . . ? N1 C2 C7 115.5(5) . . ? C3 C2 C7 122.7(5) . . ? C2 C3 C4 118.3(5) . . ? C5 C4 C3 120.2(5) . . ? C4 C5 C6 119.5(5) . . ? N1 C6 C5 120.0(5) . . ? N1 C6 C10 116.1(5) . . ? C5 C6 C10 123.9(5) . . ? N8 C7 C2 115.3(5) . . ? N8 C7 C13 125.3(5) . . ? C2 C7 C13 119.4(5) . . ? C7 N8 N9 117.4(5) . . ? C7 N8 Mn 117.1(3) . . ? N9 N8 Mn 125.5(3) . . ? N8 N9 C21 118.3(4) . . ? N8 N9 C15 110.9(5) . . ? C21 N9 C15 114.8(4) . . ? N11 C10 C6 116.3(5) . . ? N11 C10 C14 124.6(5) . . ? C6 C10 C14 119.0(5) . . ? C10 N11 N12 118.1(5) . . ? C10 N11 Mn 116.2(4) . . ? N12 N11 Mn 125.6(3) . . ? N11 N12 C28 117.9(4) . . ? N11 N12 C22 111.3(4) . . ? C28 N12 C22 115.8(5) . . ? C17 C16 C21 120.0 . . ? C16 C17 C18 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C20 120.0 . . ? C21 C20 C19 120.0 . . ? C20 C21 C16 120.0 . . ? C20 C21 N9 117.3(3) . . ? C16 C21 N9 122.7(3) . . ? C24 C23 C28 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C27 C26 C25 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C28 C23 120.0 . . ? C27 C28 N12 123.5(3) . . ? C23 C28 N12 116.4(3) . . ? N30 C31 C32 176.8(13) . . ? _refine_diff_density_max 0.323 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.065 data_VG9809 _database_code_CSD 190873 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H43 N3 Cl2 Mn' _chemical_formula_weight 595.53 _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' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.4629(9) _cell_length_b 13.5585(6) _cell_length_c 18.6936(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3412.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 10.63 _cell_measurement_theta_max 24.99 _exptl_crystal_description prisms _exptl_crystal_colour Orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method ? _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 4.748 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.1594 _exptl_absorpt_correction_T_max 0.2988 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3176 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 63.94 _reflns_number_total 3176 _reflns_number_observed 2691 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 107 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^)+(0.0435P)^2^+0.0591P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00102(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 3069 _refine_ls_number_parameters 348 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_obs 0.0406 _refine_ls_wR_factor_all 0.1046 _refine_ls_wR_factor_obs 0.0902 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.053 _refine_ls_restrained_S_all 1.113 _refine_ls_restrained_S_obs 1.052 _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 Mn Mn 0.15729(5) 0.12594(5) 0.89762(3) 0.0429(2) Uani 1 d . . Cl1 Cl -0.00434(13) 0.1806(2) 0.91690(11) 0.0940(5) Uani 1 d . . Cl2 Cl 0.18962(12) 0.10967(11) 0.77756(6) 0.0703(4) Uani 1 d . . N1 N 0.2120(3) 0.0896(3) 1.0057(2) 0.0454(8) Uani 1 d . . C2 C 0.2682(4) 0.1584(4) 1.0385(2) 0.0506(10) Uani 1 d . . C3 C 0.3019(4) 0.1477(4) 1.1077(3) 0.0656(13) Uani 1 d . . H3A H 0.3387(4) 0.1973(4) 1.1296(3) 0.079 Uiso 1 calc R . C4 C 0.2796(5) 0.0615(5) 1.1436(3) 0.073(2) Uani 1 d . . H4A H 0.3023(5) 0.0512(5) 1.1900(3) 0.088 Uiso 1 calc R . C5 C 0.2233(5) -0.0089(4) 1.1094(3) 0.0682(14) Uani 1 d . . H5A H 0.2089(5) -0.0680(4) 1.1325(3) 0.082 Uiso 1 calc R . C6 C 0.1874(4) 0.0077(4) 1.0401(2) 0.0513(11) Uani 1 d . . C7 C 0.1218(5) -0.0659(4) 1.0017(3) 0.0661(15) Uani 1 d . . H7A H 0.1553(5) -0.1300(4) 1.0026(3) 0.079 Uiso 1 calc R . N7 N 0.1062(3) -0.0380(3) 0.9260(2) 0.0511(9) Uani 1 d D . H7 H 0.0450(21) -0.0115(48) 0.9287(36) 0.080(21) Uiso 1 d D . C8 C 0.0226(7) -0.0765(9) 1.0415(4) 0.137(5) Uani 1 d . . H8A H -0.0187(7) -0.1232(9) 1.0170(4) 0.206 Uiso 1 calc R . H8B H -0.0102(7) -0.0137(9) 1.0432(4) 0.206 Uiso 1 calc R . H8C H 0.0348(7) -0.0991(9) 1.0894(4) 0.206 Uiso 1 calc R . C9 C 0.2909(4) 0.2462(4) 0.9954(3) 0.0530(11) Uani 1 d . . H9A H 0.3285(4) 0.2970(4) 1.0150(3) 0.064 Uiso 1 calc R . N9 N 0.2593(3) 0.2530(3) 0.9317(2) 0.0449(8) Uani 1 d . . C10 C 0.1192(4) -0.1167(4) 0.8745(2) 0.0548(11) Uani 1 d . . C11 C 0.2158(5) -0.1508(4) 0.8599(3) 0.0665(15) Uani 1 d . . C12 C 0.2249(7) -0.2267(5) 0.8093(4) 0.085(2) Uani 1 d . . H12A H 0.2876(7) -0.2511(5) 0.7981(4) 0.103 Uiso 1 calc R . C13 C 0.1423(8) -0.2659(4) 0.7756(4) 0.099(3) Uani 1 d . . H13A H 0.1502(8) -0.3173(4) 0.7432(4) 0.119 Uiso 1 calc R . C14 C 0.0499(7) -0.2306(5) 0.7891(3) 0.083(2) Uani 1 d . . H14A H -0.0042(7) -0.2570(5) 0.7648(3) 0.100 Uiso 1 calc R . C15 C 0.0346(5) -0.1551(4) 0.8388(3) 0.0675(15) Uani 1 d . . C16 C 0.3066(5) -0.1091(4) 0.8944(4) 0.078(2) Uani 1 d . . H16A H 0.2859(5) -0.0542(4) 0.9251(4) 0.094 Uiso 1 calc R . C17 C 0.3804(6) -0.0679(7) 0.8377(5) 0.109(3) Uani 1 d . . H17A H 0.4379(6) -0.0417(7) 0.8614(5) 0.163 Uiso 1 calc R . H17B H 0.3485(6) -0.0166(7) 0.8108(5) 0.163 Uiso 1 calc R . H17C H 0.4002(6) -0.1200(7) 0.8060(5) 0.163 Uiso 1 calc R . C18 C 0.3596(8) -0.1855(7) 0.9417(6) 0.140(4) Uani 1 d . . H18A H 0.4174(8) -0.1561(7) 0.9629(6) 0.210 Uiso 1 calc R . H18B H 0.3791(8) -0.2409(7) 0.9131(6) 0.210 Uiso 1 calc R . H18C H 0.3153(8) -0.2072(7) 0.9788(6) 0.210 Uiso 1 calc R . C19 C -0.0702(6) -0.1179(6) 0.8509(4) 0.088(2) Uani 1 d . . H19A H -0.0688(6) -0.0768(6) 0.8941(4) 0.106 Uiso 1 calc R . C20 C -0.1450(9) -0.1972(9) 0.8636(6) 0.159(5) Uani 1 d . . H20A H -0.2092(9) -0.1680(9) 0.8708(6) 0.239 Uiso 1 calc R . H20B H -0.1267(9) -0.2343(9) 0.9053(6) 0.239 Uiso 1 calc R . H20C H -0.1472(9) -0.2402(9) 0.8229(6) 0.239 Uiso 1 calc R . C21 C -0.1003(9) -0.0511(12) 0.7888(7) 0.185(7) Uani 1 d . . H21A H -0.0507(9) -0.0011(12) 0.7821(7) 0.278 Uiso 1 calc R . H21B H -0.1629(9) -0.0205(12) 0.7993(7) 0.278 Uiso 1 calc R . H21C H -0.1061(9) -0.0896(12) 0.7459(7) 0.278 Uiso 1 calc R . C22 C 0.2853(4) 0.3409(3) 0.8917(3) 0.0508(10) Uani 1 d . . C23 C 0.2334(4) 0.4283(4) 0.9046(3) 0.0617(12) Uani 1 d . . C24 C 0.2606(6) 0.5114(5) 0.8642(4) 0.080(2) Uani 1 d . . H24A H 0.2271(6) 0.5707(5) 0.8707(4) 0.096 Uiso 1 calc R . C25 C 0.3360(6) 0.5056(5) 0.8155(4) 0.084(2) Uani 1 d . . H25A H 0.3546(6) 0.5618(5) 0.7903(4) 0.100 Uiso 1 calc R . C26 C 0.3840(5) 0.4201(5) 0.8032(4) 0.078(2) Uani 1 d . . H26A H 0.4333(5) 0.4181(5) 0.7684(4) 0.094 Uiso 1 calc R . C27 C 0.3615(4) 0.3338(4) 0.8417(3) 0.0605(13) Uani 1 d . . C28 C 0.1492(6) 0.4356(5) 0.9590(4) 0.083(2) Uani 1 d . . H28A H 0.1342(6) 0.3686(5) 0.9754(4) 0.100 Uiso 1 calc R . C29 C 0.0553(7) 0.4776(8) 0.9269(6) 0.130(4) Uani 1 d . . H29A H 0.0046(7) 0.4808(8) 0.9630(6) 0.195 Uiso 1 calc R . H29B H 0.0334(7) 0.4360(8) 0.8885(6) 0.195 Uiso 1 calc R . H29C H 0.0683(7) 0.5427(8) 0.9089(6) 0.195 Uiso 1 calc R . C30 C 0.1832(10) 0.4949(10) 1.0241(5) 0.156(5) Uani 1 d . . H30A H 0.2429(10) 0.4662(10) 1.0431(5) 0.234 Uiso 1 calc R . H30B H 0.1322(10) 0.4937(10) 1.0599(5) 0.234 Uiso 1 calc R . H30C H 0.1960(10) 0.5618(10) 1.0101(5) 0.234 Uiso 1 calc R . C31 C 0.4199(5) 0.2393(5) 0.8312(4) 0.072(2) Uani 1 d . . H31A H 0.3816(5) 0.1853(5) 0.8525(4) 0.087 Uiso 1 calc R . C32 C 0.4360(6) 0.2150(6) 0.7516(4) 0.098(2) Uani 1 d . . H32A H 0.4731(6) 0.1548(6) 0.7475(4) 0.146 Uiso 1 calc R . H32B H 0.4722(6) 0.2677(6) 0.7293(4) 0.146 Uiso 1 calc R . H32C H 0.3728(6) 0.2074(6) 0.7285(4) 0.146 Uiso 1 calc R . C33 C 0.5194(6) 0.2457(8) 0.8706(6) 0.122(3) Uani 1 d . . H33A H 0.5558(6) 0.1855(8) 0.8636(6) 0.182 Uiso 1 calc R . H33B H 0.5077(6) 0.2554(8) 0.9207(6) 0.182 Uiso 1 calc R . H33C H 0.5572(6) 0.3000(8) 0.8520(6) 0.182 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 Mn 0.0479(3) 0.0446(3) 0.0361(3) -0.0005(3) -0.0009(3) 0.0018(3) Cl1 0.0629(8) 0.1062(12) 0.1129(13) 0.0043(10) 0.0174(8) 0.0313(9) Cl2 0.0988(10) 0.0720(8) 0.0401(5) -0.0053(5) 0.0077(5) 0.0026(7) N1 0.051(2) 0.047(2) 0.038(2) 0.0025(14) -0.0016(15) -0.007(2) C2 0.055(3) 0.054(2) 0.042(2) 0.004(2) -0.006(2) -0.008(2) C3 0.075(3) 0.072(3) 0.050(2) 0.009(2) -0.017(3) -0.021(3) C4 0.090(4) 0.082(4) 0.049(3) 0.015(3) -0.023(3) -0.020(4) C5 0.091(4) 0.065(3) 0.049(3) 0.017(2) -0.005(3) -0.018(3) C6 0.059(3) 0.052(2) 0.043(2) 0.005(2) 0.001(2) -0.012(2) C7 0.094(4) 0.057(3) 0.047(2) 0.010(2) -0.006(3) -0.026(3) N7 0.065(3) 0.043(2) 0.045(2) -0.002(2) -0.001(2) -0.005(2) C8 0.137(8) 0.206(11) 0.068(4) 0.003(5) 0.011(4) -0.122(8) C9 0.051(3) 0.052(2) 0.056(2) 0.004(2) -0.008(2) -0.015(2) N9 0.050(2) 0.043(2) 0.041(2) 0.0020(15) -0.002(2) -0.007(2) C10 0.082(3) 0.037(2) 0.046(2) 0.000(2) -0.001(2) -0.004(2) C11 0.091(4) 0.045(3) 0.064(3) 0.003(2) -0.002(3) 0.005(3) C12 0.122(6) 0.053(3) 0.082(4) -0.008(3) -0.001(4) 0.016(4) C13 0.181(9) 0.046(3) 0.070(4) -0.012(3) 0.008(5) -0.005(5) C14 0.125(6) 0.059(3) 0.066(3) -0.012(3) -0.015(4) -0.016(4) C15 0.093(4) 0.050(3) 0.060(3) -0.002(2) -0.013(3) -0.012(3) C16 0.077(3) 0.061(3) 0.097(4) 0.001(4) 0.000(4) 0.016(3) C17 0.079(5) 0.108(6) 0.139(7) -0.001(6) 0.031(5) 0.026(5) C18 0.128(8) 0.110(7) 0.181(10) 0.041(7) -0.046(8) 0.031(6) C19 0.086(4) 0.087(4) 0.091(4) -0.018(4) -0.024(3) -0.010(4) C20 0.140(9) 0.170(11) 0.167(10) -0.063(8) 0.062(8) -0.068(9) C21 0.111(9) 0.241(17) 0.204(14) 0.087(13) -0.031(9) 0.037(11) C22 0.059(3) 0.045(2) 0.048(2) 0.006(2) -0.007(2) -0.010(2) C23 0.064(3) 0.053(2) 0.068(3) 0.006(2) -0.001(3) -0.005(2) C24 0.086(5) 0.051(3) 0.103(5) 0.020(3) -0.001(4) -0.002(3) C25 0.088(5) 0.066(3) 0.098(4) 0.035(3) 0.000(4) -0.014(4) C26 0.080(4) 0.079(4) 0.075(3) 0.026(3) 0.013(3) -0.015(3) C27 0.060(3) 0.063(3) 0.059(3) 0.015(2) 0.003(2) -0.009(2) C28 0.089(5) 0.066(4) 0.094(4) -0.002(3) 0.019(4) 0.012(4) C29 0.089(6) 0.119(7) 0.182(11) 0.015(7) 0.020(7) 0.029(6) C30 0.167(12) 0.188(12) 0.112(7) -0.061(8) 0.031(8) -0.007(10) C31 0.060(3) 0.077(4) 0.080(4) 0.004(3) 0.018(3) -0.001(3) C32 0.100(6) 0.098(5) 0.094(5) -0.011(4) 0.036(4) -0.009(5) C33 0.087(6) 0.116(7) 0.162(9) -0.010(6) -0.009(6) 0.035(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn N1 2.206(4) . ? Mn N9 2.294(4) . ? Mn Cl2 2.2967(12) . ? Mn Cl1 2.327(2) . ? Mn N7 2.386(4) . ? N1 C6 1.326(6) . ? N1 C2 1.348(6) . ? C2 C3 1.378(7) . ? C2 C9 1.470(7) . ? C3 C4 1.381(8) . ? C4 C5 1.377(8) . ? C5 C6 1.400(7) . ? C6 C7 1.514(7) . ? C7 N7 1.480(6) . ? C7 C8 1.537(10) . ? N7 C10 1.448(6) . ? C9 N9 1.268(6) . ? N9 C22 1.449(6) . ? C10 C11 1.408(9) . ? C10 C15 1.419(8) . ? C11 C12 1.404(8) . ? C11 C16 1.493(9) . ? C12 C13 1.384(12) . ? C13 C14 1.356(13) . ? C14 C15 1.398(9) . ? C15 C19 1.515(10) . ? C16 C18 1.537(10) . ? C16 C17 1.556(11) . ? C19 C20 1.491(12) . ? C19 C21 1.528(13) . ? C22 C27 1.391(8) . ? C22 C23 1.397(7) . ? C23 C24 1.404(8) . ? C23 C28 1.526(9) . ? C24 C25 1.366(11) . ? C25 C26 1.347(10) . ? C26 C27 1.406(8) . ? C27 C31 1.517(9) . ? C28 C29 1.509(11) . ? C28 C30 1.528(12) . ? C31 C33 1.531(11) . ? C31 C32 1.538(9) . ? 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 Mn N9 73.35(13) . . ? N1 Mn Cl2 144.11(12) . . ? N9 Mn Cl2 103.30(10) . . ? N1 Mn Cl1 103.98(12) . . ? N9 Mn Cl1 106.12(12) . . ? Cl2 Mn Cl1 111.05(7) . . ? N1 Mn N7 71.63(14) . . ? N9 Mn N7 144.16(14) . . ? Cl2 Mn N7 100.51(10) . . ? Cl1 Mn N7 89.58(12) . . ? C6 N1 C2 119.8(4) . . ? C6 N1 Mn 123.3(3) . . ? C2 N1 Mn 116.8(3) . . ? N1 C2 C3 122.7(4) . . ? N1 C2 C9 115.3(4) . . ? C3 C2 C9 122.1(4) . . ? C2 C3 C4 118.2(5) . . ? C5 C4 C3 118.8(5) . . ? C4 C5 C6 120.5(5) . . ? N1 C6 C5 119.9(5) . . ? N1 C6 C7 117.8(4) . . ? C5 C6 C7 122.3(4) . . ? N7 C7 C6 111.6(4) . . ? N7 C7 C8 111.3(6) . . ? C6 C7 C8 109.7(5) . . ? C10 N7 C7 115.4(4) . . ? C10 N7 Mn 120.3(3) . . ? C7 N7 Mn 114.2(3) . . ? N9 C9 C2 120.3(4) . . ? C9 N9 C22 117.6(4) . . ? C9 N9 Mn 114.0(3) . . ? C22 N9 Mn 128.3(3) . . ? C11 C10 C15 122.1(5) . . ? C11 C10 N7 118.8(5) . . ? C15 C10 N7 119.1(5) . . ? C12 C11 C10 116.9(6) . . ? C12 C11 C16 119.8(7) . . ? C10 C11 C16 123.3(5) . . ? C13 C12 C11 121.2(8) . . ? C14 C13 C12 121.2(6) . . ? C13 C14 C15 121.2(7) . . ? C14 C15 C10 117.5(7) . . ? C14 C15 C19 118.7(6) . . ? C10 C15 C19 123.7(5) . . ? C11 C16 C18 111.9(6) . . ? C11 C16 C17 111.4(7) . . ? C18 C16 C17 109.8(7) . . ? C20 C19 C15 114.4(8) . . ? C20 C19 C21 111.7(9) . . ? C15 C19 C21 109.3(7) . . ? C27 C22 C23 122.9(5) . . ? C27 C22 N9 117.9(4) . . ? C23 C22 N9 119.2(4) . . ? C22 C23 C24 117.2(5) . . ? C22 C23 C28 122.8(5) . . ? C24 C23 C28 120.0(6) . . ? C25 C24 C23 120.4(7) . . ? C26 C25 C24 121.4(6) . . ? C25 C26 C27 121.7(6) . . ? C22 C27 C26 116.5(6) . . ? C22 C27 C31 121.8(5) . . ? C26 C27 C31 121.7(5) . . ? C29 C28 C23 112.4(6) . . ? C29 C28 C30 111.7(8) . . ? C23 C28 C30 110.0(7) . . ? C27 C31 C33 110.1(6) . . ? C27 C31 C32 112.3(6) . . ? C33 C31 C32 110.7(6) . . ? _refine_diff_density_max 0.247 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.040 data_VG9830 _database_code_CSD 190874 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C108 H108 N20 Cl10 Mn5' _chemical_formula_weight 2315.34 _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' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 12.7957(13) _cell_length_b 17.2978(9) _cell_length_c 25.1666(14) _cell_angle_alpha 90.00 _cell_angle_beta 94.434(8) _cell_angle_gamma 90.00 _cell_volume 5553.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 10.93 _cell_measurement_theta_max 28.01 _exptl_crystal_description prisms _exptl_crystal_colour Orange _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method ? _exptl_crystal_F_000 2382 _exptl_absorpt_coefficient_mu 7.154 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.1220 _exptl_absorpt_correction_T_max 0.5910 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8646 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 60.00 _reflns_number_total 8230 _reflns_number_observed 5746 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 686 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^)+(0.0588P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00006(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7544 _refine_ls_number_parameters 674 _refine_ls_number_restraints 118 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_obs 0.0515 _refine_ls_wR_factor_all 0.1260 _refine_ls_wR_factor_obs 0.1081 _refine_ls_goodness_of_fit_all 1.029 _refine_ls_goodness_of_fit_obs 1.100 _refine_ls_restrained_S_all 1.057 _refine_ls_restrained_S_obs 1.103 _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 Mn1 Mn 0.19622(6) 0.47129(4) 0.74060(3) 0.0227(2) Uani 1 d . . Mn2 Mn 0.5000 0.32636(6) 0.7500 0.0263(3) Uani 1 d S . Cl1 Cl 0.0000 0.50156(10) 0.7500 0.0272(3) Uani 1 d S . Cl2 Cl 0.25510(9) 0.59955(6) 0.75004(5) 0.0305(3) Uani 1 d . . Cl3 Cl 0.37820(9) 0.41488(8) 0.70735(6) 0.0431(3) Uani 1 d . . Cl4 Cl 0.57132(10) 0.24348(7) 0.68814(5) 0.0373(3) Uani 1 d . . N1 N 0.1565(3) 0.3495(2) 0.73494(15) 0.0202(8) Uani 1 d . . C2 C 0.1642(3) 0.3049(3) 0.7786(2) 0.0210(10) Uani 1 d . . C3 C 0.1442(4) 0.2263(3) 0.7762(2) 0.0275(11) Uani 1 d . . H3A H 0.1498(4) 0.1954(3) 0.8075(2) 0.033 Uiso 1 calc R . C4 C 0.1158(4) 0.1938(3) 0.7268(2) 0.0310(11) Uani 1 d . . H4A H 0.1003(4) 0.1401(3) 0.7240(2) 0.037 Uiso 1 calc R . C5 C 0.1100(4) 0.2393(3) 0.6816(2) 0.0279(11) Uani 1 d . . H5A H 0.0912(4) 0.2174(3) 0.6476(2) 0.033 Uiso 1 calc R . C6 C 0.1320(3) 0.3176(3) 0.6868(2) 0.0230(10) Uani 1 d . . C7 C 0.2034(3) 0.3460(3) 0.8287(2) 0.0236(10) Uani 1 d . . N7 N 0.2302(3) 0.4174(2) 0.82347(15) 0.0231(8) Uani 1 d . . C8 C 0.2108(4) 0.3011(3) 0.8800(2) 0.0326(12) Uani 1 d . . H8A H 0.2676(4) 0.2631(3) 0.8796(2) 0.049 Uiso 1 d R . H8B H 0.1443(4) 0.2742(3) 0.8837(2) 0.049 Uiso 1 d R . H8C H 0.2249(4) 0.3365(3) 0.9101(2) 0.049 Uiso 1 d R . C9 C 0.1298(3) 0.3739(3) 0.6418(2) 0.0257(10) Uani 1 d . . N9 N 0.1440(3) 0.4443(2) 0.65329(15) 0.0220(8) Uani 1 d . . C10 C 0.1142(4) 0.3410(3) 0.5865(2) 0.0361(13) Uani 1 d . . H10A H 0.0441(4) 0.3182(3) 0.5810(2) 0.054 Uiso 1 d R . H10B H 0.1671(4) 0.3012(3) 0.5817(2) 0.054 Uiso 1 d R . H10C H 0.1213(4) 0.3826(3) 0.5606(2) 0.054 Uiso 1 d R . C11 C 0.2877(4) 0.4562(3) 0.8672(2) 0.0252(10) Uani 1 d . . C12 C 0.3917(4) 0.4345(3) 0.8790(2) 0.0365(13) Uani 1 d . . H12A H 0.4197(4) 0.3923(3) 0.8606(2) 0.044 Uiso 1 calc R . C13 C 0.4541(4) 0.4736(4) 0.9169(2) 0.048(2) Uani 1 d . . H13A H 0.5252(4) 0.4589(4) 0.9246(2) 0.058 Uiso 1 calc R . C14 C 0.4125(4) 0.5341(4) 0.9437(2) 0.049(2) Uani 1 d . . H14A H 0.4548(4) 0.5604(4) 0.9705(2) 0.059 Uiso 1 calc R . C15 C 0.3105(4) 0.5569(3) 0.9321(2) 0.0401(13) Uani 1 d . . H15A H 0.2834(4) 0.5992(3) 0.9508(2) 0.048 Uiso 1 calc R . C16 C 0.2453(4) 0.5184(3) 0.8927(2) 0.0301(11) Uani 1 d . . C17 C 0.1335(4) 0.5433(3) 0.8827(2) 0.0285(11) Uani 1 d . . H17A H 0.1152(4) 0.5454(3) 0.8438(2) 0.034 Uiso 1 calc R . H17B H 0.1256(4) 0.5961(3) 0.8971(2) 0.034 Uiso 1 calc R . C18 C 0.1419(4) 0.5025(3) 0.6133(2) 0.0267(10) Uani 1 d . . C19 C 0.2355(4) 0.5401(3) 0.6052(2) 0.0365(12) Uani 1 d . . H19A H 0.2980(4) 0.5251(3) 0.6255(2) 0.044 Uiso 1 calc R . C20 C 0.2389(5) 0.5986(4) 0.5685(2) 0.0441(14) Uani 1 d . . H20A H 0.3037(5) 0.6229(4) 0.5627(2) 0.053 Uiso 1 calc R . C21 C 0.1469(5) 0.6223(4) 0.5399(2) 0.0452(14) Uani 1 d . . H21A H 0.1480(5) 0.6630(4) 0.5146(2) 0.054 Uiso 1 calc R . C22 C 0.0546(4) 0.5858(3) 0.5488(2) 0.0374(13) Uani 1 d . . H22A H -0.0079(4) 0.6025(3) 0.5293(2) 0.045 Uiso 1 calc R . C23 C 0.0481(4) 0.5256(3) 0.5849(2) 0.0306(11) Uani 1 d . . C24 C -0.0574(4) 0.4890(3) 0.5919(2) 0.0316(11) Uani 1 d . . H24A H -0.0468(4) 0.4423(3) 0.6145(2) 0.038 Uiso 1 calc R . H24B H -0.0891(4) 0.4723(3) 0.5567(2) 0.038 Uiso 1 calc R . Mn3 Mn 0.02896(5) 0.03003(4) 0.34914(3) 0.0222(2) Uani 1 d . . Cl5 Cl 0.0000 0.00428(10) 0.2500 0.0270(3) Uani 1 d S . Cl6 Cl 0.06481(9) -0.09743(6) 0.37899(5) 0.0295(3) Uani 1 d . . N31 N -0.0020(3) 0.1538(2) 0.3350(2) 0.0240(9) Uani 1 d . . C32 C 0.0777(4) 0.2016(3) 0.3267(2) 0.0270(11) Uani 1 d . . C33 C 0.0611(4) 0.2794(3) 0.3164(2) 0.0328(12) Uani 1 d . . H33A H 0.1176(4) 0.3122(3) 0.3089(2) 0.039 Uiso 1 calc R . C34 C -0.0402(4) 0.3085(3) 0.3172(2) 0.0336(12) Uani 1 d . . H34A H -0.0534(4) 0.3619(3) 0.3113(2) 0.040 Uiso 1 calc R . C35 C -0.1210(4) 0.2594(3) 0.3268(2) 0.0315(11) Uani 1 d . . H35A H -0.1904(4) 0.2785(3) 0.3278(2) 0.038 Uiso 1 calc R . C36 C -0.0996(4) 0.1809(3) 0.3350(2) 0.0240(10) Uani 1 d . . C37 C 0.1843(4) 0.1656(3) 0.3329(2) 0.0284(11) Uani 1 d . . N37 N 0.1890(3) 0.0944(2) 0.3468(2) 0.0255(9) Uani 1 d . . C38 C 0.2756(4) 0.2160(3) 0.3238(3) 0.0432(15) Uani 1 d . . H38A H 0.2884(4) 0.2508(3) 0.3543(3) 0.065 Uiso 1 d R . H38B H 0.2609(4) 0.2465(3) 0.2913(3) 0.065 Uiso 1 d R . H38C H 0.3377(4) 0.1838(3) 0.3202(3) 0.065 Uiso 1 d R . C39 C -0.1814(4) 0.1215(3) 0.3436(2) 0.0283(11) Uani 1 d . . N39 N -0.1484(3) 0.0517(2) 0.3480(2) 0.0232(8) Uani 1 d . . C40 C -0.2930(4) 0.1472(3) 0.3466(2) 0.0363(13) Uani 1 d . . H40A H -0.3196(4) 0.1676(3) 0.3118(2) 0.054 Uiso 1 d R . H40B H -0.2965(4) 0.1876(3) 0.3737(2) 0.054 Uiso 1 d R . H40C H -0.3359(4) 0.1030(3) 0.3560(2) 0.054 Uiso 1 d R . C41 C 0.2889(4) 0.0619(3) 0.3649(2) 0.0267(10) Uani 1 d . . C42 C 0.3418(4) 0.0951(3) 0.4101(2) 0.0384(13) Uani 1 d . . H42A H 0.3120(4) 0.1379(3) 0.4271(2) 0.046 Uiso 1 calc R . C43 C 0.4381(5) 0.0655(4) 0.4302(2) 0.046(2) Uani 1 d . . H43A H 0.4753(5) 0.0894(4) 0.4599(2) 0.055 Uiso 1 calc R . C44 C 0.4791(4) 0.0014(4) 0.4067(2) 0.0436(14) Uani 1 d . . H44A H 0.5442(4) -0.0198(4) 0.4206(2) 0.052 Uiso 1 calc R . C45 C 0.4248(4) -0.0320(3) 0.3629(2) 0.0349(12) Uani 1 d . . H45A H 0.4536(4) -0.0762(3) 0.3471(2) 0.042 Uiso 1 calc R . C46 C 0.3298(4) -0.0031(3) 0.3412(2) 0.0277(11) Uani 1 d . . C47 C 0.2797(3) -0.0393(3) 0.2910(2) 0.0266(10) Uani 1 d . . H47A H 0.2027(3) -0.0406(3) 0.2928(2) 0.032 Uiso 1 calc R . H47B H 0.3047(3) -0.0931(3) 0.2882(2) 0.032 Uiso 1 calc R . C48 C -0.2170(3) -0.0127(3) 0.3526(2) 0.0266(10) Uani 1 d . . C49 C -0.2035(4) -0.0547(3) 0.4001(2) 0.0330(12) Uani 1 d . . H49A H -0.1542(4) -0.0380(3) 0.4279(2) 0.040 Uiso 1 calc R . C50 C -0.2623(4) -0.1205(3) 0.4063(2) 0.0373(13) Uani 1 d . . H50A H -0.2557(4) -0.1480(3) 0.4390(2) 0.045 Uiso 1 calc R . C51 C -0.3307(4) -0.1465(3) 0.3650(2) 0.0354(12) Uani 1 d . . H51A H -0.3696(4) -0.1927(3) 0.3690(2) 0.042 Uiso 1 calc R . C52 C -0.3423(4) -0.1052(3) 0.3178(2) 0.0323(12) Uani 1 d . . H52A H -0.3891(4) -0.1239(3) 0.2896(2) 0.039 Uiso 1 calc R . C53 C -0.2873(4) -0.0370(3) 0.3104(2) 0.0280(10) Uani 1 d . . C54 C -0.3061(4) 0.0064(3) 0.2587(2) 0.0288(11) Uani 1 d . . H54A H -0.2635(4) 0.0543(3) 0.2609(2) 0.035 Uiso 1 calc R . H54B H -0.3807(4) 0.0219(3) 0.2544(2) 0.035 Uiso 1 calc R . N60 N 0.0364(4) 0.0754(3) 0.4390(2) 0.0434(12) Uani 1 d . . C61 C 0.0372(4) 0.1257(3) 0.4673(2) 0.0380(13) Uani 1 d . . C62 C 0.0387(5) 0.1913(4) 0.5027(3) 0.054(2) Uani 1 d . . H62A H 0.0300(5) 0.1734(4) 0.5390(3) 0.081 Uiso 1 d R . H62B H -0.0185(5) 0.2267(4) 0.4913(3) 0.081 Uiso 1 d R . H62C H 0.1059(5) 0.2183(4) 0.5018(3) 0.081 Uiso 1 d R . N63 N 0.3144(6) 0.2631(4) 0.5013(3) 0.076(2) Uani 1 d . . C64 C 0.4020(7) 0.2628(4) 0.5163(3) 0.062(2) Uani 1 d . . C65 C 0.5089(7) 0.2603(6) 0.5351(4) 0.096(3) Uani 1 d . . H65A H 0.5181(7) 0.2893(6) 0.5686(4) 0.143 Uiso 1 d R . H65B H 0.5526(7) 0.2834(6) 0.5090(4) 0.143 Uiso 1 d R . H65C H 0.5298(7) 0.2064(6) 0.5414(4) 0.143 Uiso 1 d R . N66 N 0.2291(10) -0.1972(6) 0.5169(5) 0.162(6) Uani 1 d . . C67 C 0.2444(6) -0.1394(5) 0.5012(3) 0.066(2) Uani 1 d . . C68 C 0.2624(7) -0.0638(5) 0.4818(3) 0.073(2) Uani 1 d . . H68A H 0.2799(7) -0.0659(5) 0.4446(3) 0.109 Uiso 1 d R . H68B H 0.3205(7) -0.0401(5) 0.5037(3) 0.109 Uiso 1 d R . H68C H 0.1988(7) -0.0328(5) 0.4843(3) 0.109 Uiso 1 d R . N69 N 0.5222(9) 0.7253(7) 0.9005(5) 0.056(3) Uani 0.50 d PDU 1 C70 C 0.5168(9) 0.6816(8) 0.8682(5) 0.050(2) Uani 0.50 d PDU 1 C71 C 0.5060(15) 0.6140(9) 0.8210(6) 0.055(3) Uani 0.50 d PDU 1 H71A H 0.4678(15) 0.5671(9) 0.8297(6) 0.083 Uiso 0.50 d PR 1 H71B H 0.5788(15) 0.6008(9) 0.8156(6) 0.083 Uiso 0.50 d PR 1 H71C H 0.4728(15) 0.6372(9) 0.7885(6) 0.083 Uiso 0.50 d PR 1 N72 N 0.5128(13) 0.7625(9) 0.7757(6) 0.092(3) Uani 0.50 d PDU 2 C73 C 0.5135(15) 0.7044(9) 0.7965(7) 0.083(3) Uani 0.50 d PDU 2 C74 C 0.5075(17) 0.6329(10) 0.8300(8) 0.070(4) Uani 0.50 d PDU 2 H74A H 0.5095(17) 0.6393(10) 0.8688(8) 0.106 Uiso 0.50 d PR 2 H74B H 0.5610(17) 0.5955(10) 0.8212(8) 0.106 Uiso 0.50 d PR 2 H74C H 0.4382(17) 0.6141(10) 0.8166(8) 0.106 Uiso 0.50 d PR 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 0.0287(4) 0.0207(4) 0.0179(4) -0.0001(3) -0.0025(3) -0.0014(3) Mn2 0.0185(5) 0.0269(6) 0.0335(6) 0.000 0.0020(4) 0.000 Cl1 0.0197(7) 0.0339(8) 0.0280(8) 0.000 0.0008(6) 0.000 Cl2 0.0272(5) 0.0240(6) 0.0401(6) -0.0021(5) 0.0018(5) -0.0024(4) Cl3 0.0251(6) 0.0511(8) 0.0535(8) 0.0183(7) 0.0066(5) 0.0116(5) Cl4 0.0346(6) 0.0356(7) 0.0428(7) -0.0074(6) 0.0099(5) -0.0018(5) N1 0.018(2) 0.021(2) 0.022(2) -0.002(2) 0.0016(15) 0.0012(14) C2 0.014(2) 0.022(2) 0.026(2) 0.000(2) -0.001(2) 0.005(2) C3 0.027(2) 0.026(3) 0.030(3) 0.003(2) 0.005(2) 0.001(2) C4 0.028(2) 0.024(2) 0.040(3) 0.000(2) 0.001(2) -0.003(2) C5 0.022(2) 0.028(3) 0.032(3) -0.008(2) -0.001(2) 0.003(2) C6 0.021(2) 0.023(2) 0.023(2) -0.003(2) -0.003(2) 0.002(2) C7 0.019(2) 0.031(3) 0.021(2) 0.002(2) 0.002(2) 0.005(2) N7 0.024(2) 0.028(2) 0.016(2) -0.001(2) 0.001(2) 0.004(2) C8 0.035(3) 0.037(3) 0.025(3) 0.010(2) 0.003(2) 0.002(2) C9 0.022(2) 0.035(3) 0.019(2) -0.003(2) 0.001(2) 0.003(2) N9 0.018(2) 0.027(2) 0.021(2) 0.001(2) 0.001(2) -0.0002(15) C10 0.051(3) 0.038(3) 0.019(3) -0.010(2) 0.002(2) 0.007(2) C11 0.027(2) 0.033(3) 0.016(2) -0.001(2) -0.002(2) -0.003(2) C12 0.030(3) 0.052(3) 0.026(3) -0.006(2) -0.002(2) 0.005(2) C13 0.028(3) 0.071(4) 0.044(3) -0.012(3) -0.011(2) 0.000(3) C14 0.035(3) 0.071(4) 0.039(3) -0.014(3) -0.011(3) -0.010(3) C15 0.039(3) 0.045(3) 0.035(3) -0.012(3) -0.003(2) -0.001(2) C16 0.029(2) 0.038(3) 0.022(2) -0.001(2) -0.002(2) -0.004(2) C17 0.033(3) 0.029(3) 0.023(2) -0.002(2) -0.002(2) 0.001(2) C18 0.027(2) 0.033(3) 0.020(2) 0.002(2) 0.002(2) 0.001(2) C19 0.027(2) 0.047(3) 0.034(3) 0.006(3) -0.002(2) -0.007(2) C20 0.044(3) 0.052(4) 0.037(3) 0.010(3) 0.008(3) -0.015(3) C21 0.058(4) 0.045(3) 0.034(3) 0.015(3) 0.009(3) -0.001(3) C22 0.041(3) 0.043(3) 0.027(3) 0.003(2) -0.003(2) 0.005(2) C23 0.030(2) 0.038(3) 0.024(2) 0.001(2) 0.000(2) 0.004(2) C24 0.028(2) 0.034(3) 0.032(3) -0.001(2) -0.001(2) 0.000(2) Mn3 0.0223(3) 0.0208(4) 0.0234(4) -0.0016(3) 0.0013(3) 0.0002(3) Cl5 0.0282(8) 0.0338(8) 0.0186(7) 0.000 -0.0008(6) 0.000 Cl6 0.0362(6) 0.0242(6) 0.0282(6) -0.0008(5) 0.0023(5) 0.0025(5) N31 0.024(2) 0.025(2) 0.023(2) -0.001(2) 0.000(2) 0.001(2) C32 0.027(2) 0.030(3) 0.024(3) 0.000(2) -0.001(2) -0.003(2) C33 0.034(3) 0.023(3) 0.040(3) 0.003(2) -0.003(2) -0.003(2) C34 0.040(3) 0.021(2) 0.038(3) -0.003(2) -0.007(2) 0.003(2) C35 0.030(2) 0.030(3) 0.035(3) -0.002(2) 0.000(2) 0.007(2) C36 0.027(2) 0.024(2) 0.021(2) -0.001(2) 0.001(2) 0.001(2) C37 0.025(2) 0.029(3) 0.031(3) -0.003(2) 0.002(2) -0.003(2) N37 0.025(2) 0.026(2) 0.026(2) -0.006(2) -0.002(2) 0.001(2) C38 0.028(3) 0.031(3) 0.070(4) 0.003(3) 0.003(3) -0.004(2) C39 0.027(2) 0.034(3) 0.024(2) -0.003(2) 0.000(2) 0.002(2) N39 0.023(2) 0.026(2) 0.022(2) -0.002(2) 0.006(2) 0.003(2) C40 0.028(3) 0.035(3) 0.047(3) -0.005(2) 0.003(2) 0.004(2) C41 0.024(2) 0.027(2) 0.029(3) 0.001(2) 0.001(2) -0.002(2) C42 0.036(3) 0.034(3) 0.043(3) -0.010(3) -0.008(2) -0.003(2) C43 0.041(3) 0.049(3) 0.045(3) -0.013(3) -0.015(3) -0.005(3) C44 0.030(3) 0.051(3) 0.048(3) -0.004(3) -0.012(3) 0.006(2) C45 0.030(3) 0.039(3) 0.036(3) -0.001(2) -0.001(2) 0.005(2) C46 0.023(2) 0.031(3) 0.030(3) -0.001(2) 0.003(2) -0.002(2) C47 0.021(2) 0.027(2) 0.031(3) -0.002(2) -0.001(2) 0.002(2) C48 0.020(2) 0.030(3) 0.030(3) -0.001(2) 0.007(2) 0.001(2) C49 0.026(2) 0.045(3) 0.028(3) 0.006(2) 0.000(2) -0.003(2) C50 0.032(3) 0.047(3) 0.034(3) 0.015(2) 0.009(2) -0.003(2) C51 0.025(2) 0.038(3) 0.044(3) 0.011(2) 0.013(2) -0.006(2) C52 0.021(2) 0.040(3) 0.036(3) -0.002(2) 0.001(2) -0.002(2) C53 0.025(2) 0.032(3) 0.028(3) 0.005(2) 0.004(2) 0.000(2) C54 0.032(2) 0.030(3) 0.024(3) -0.002(2) -0.001(2) 0.002(2) N60 0.055(3) 0.040(3) 0.034(3) -0.010(2) 0.001(2) 0.003(2) C61 0.041(3) 0.042(3) 0.029(3) 0.001(3) -0.004(2) 0.000(2) C62 0.069(4) 0.050(4) 0.044(4) -0.022(3) 0.003(3) 0.008(3) N63 0.086(5) 0.065(4) 0.077(5) 0.026(4) 0.011(4) -0.003(4) C64 0.086(6) 0.054(4) 0.051(4) 0.009(3) 0.025(4) -0.005(4) C65 0.089(7) 0.110(8) 0.086(7) 0.004(6) -0.002(5) -0.019(6) N66 0.203(12) 0.111(8) 0.160(10) 0.080(8) -0.067(9) -0.072(8) C67 0.070(5) 0.071(5) 0.055(4) 0.010(4) -0.011(4) -0.013(4) C68 0.084(5) 0.075(5) 0.057(5) 0.002(4) -0.011(4) -0.014(4) N69 0.049(5) 0.057(6) 0.063(6) 0.004(5) 0.005(5) 0.000(5) C70 0.037(4) 0.060(5) 0.054(5) 0.010(5) 0.006(4) 0.004(4) C71 0.055(3) 0.056(3) 0.055(3) -0.0003(10) 0.0040(11) 0.0004(10) N72 0.092(3) 0.092(3) 0.092(3) -0.0002(10) 0.0073(10) 0.0000(10) C73 0.083(3) 0.083(3) 0.083(3) 0.0000(10) 0.0066(10) 0.0001(10) C74 0.070(4) 0.071(4) 0.071(4) 0.0000(10) 0.0054(11) 0.0004(10) _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 N1 2.168(4) . ? Mn1 N9 2.295(4) . ? Mn1 N7 2.295(4) . ? Mn1 Cl2 2.3491(13) . ? Mn1 Cl1 2.5935(9) . ? Mn1 Cl3 2.716(2) . ? Mn2 Cl4 2.3519(15) . ? Mn2 Cl4 2.3519(15) 2_656 ? Mn2 Cl3 2.3806(14) 2_656 ? Mn2 Cl3 2.3806(14) . ? Cl1 Mn1 2.5935(9) 2_556 ? N1 C2 1.340(6) . ? N1 C6 1.346(6) . ? C2 C3 1.385(7) . ? C2 C7 1.501(6) . ? C3 C4 1.387(7) . ? C4 C5 1.379(7) . ? C5 C6 1.388(7) . ? C6 C9 1.494(7) . ? C7 N7 1.291(6) . ? C7 C8 1.503(6) . ? N7 C11 1.442(6) . ? C9 N9 1.262(6) . ? C9 C10 1.502(6) . ? N9 C18 1.422(6) . ? C11 C16 1.384(7) . ? C11 C12 1.392(7) . ? C12 C13 1.375(7) . ? C13 C14 1.373(9) . ? C14 C15 1.374(8) . ? C15 C16 1.412(7) . ? C16 C17 1.498(7) . ? C17 C24 1.528(7) 2_556 ? C18 C19 1.392(7) . ? C18 C23 1.407(6) . ? C19 C20 1.374(8) . ? C20 C21 1.394(8) . ? C21 C22 1.373(8) . ? C22 C23 1.388(8) . ? C23 C24 1.513(7) . ? C24 C17 1.528(7) 2_556 ? Mn3 N31 2.201(4) . ? Mn3 N39 2.298(4) . ? Mn3 N37 2.336(4) . ? Mn3 Cl6 2.3627(13) . ? Mn3 N60 2.388(5) . ? Mn3 Cl5 2.5333(8) . ? Cl5 Mn3 2.5333(8) 2 ? N31 C36 1.334(6) . ? N31 C32 1.341(6) . ? C32 C33 1.383(7) . ? C32 C37 1.497(7) . ? C33 C34 1.392(7) . ? C34 C35 1.373(8) . ? C35 C36 1.397(7) . ? C36 C39 1.495(7) . ? C37 N37 1.280(6) . ? C37 C38 1.489(7) . ? N37 C41 1.438(6) . ? C39 N39 1.280(6) . ? C39 C40 1.504(7) . ? N39 C48 1.429(6) . ? C41 C46 1.394(7) . ? C41 C42 1.401(7) . ? C42 C43 1.392(8) . ? C43 C44 1.380(8) . ? C44 C45 1.384(7) . ? C45 C46 1.386(7) . ? C46 C47 1.508(6) . ? C47 C54 1.540(7) 2 ? C48 C49 1.398(7) . ? C48 C53 1.402(6) . ? C49 C50 1.380(8) . ? C50 C51 1.381(8) . ? C51 C52 1.385(7) . ? C52 C53 1.393(7) . ? C53 C54 1.505(7) . ? C54 C47 1.540(7) 2 ? N60 C61 1.124(7) . ? C61 C62 1.442(8) . ? N63 C64 1.155(10) . ? C64 C65 1.413(12) . ? N66 C67 1.098(11) . ? C67 C68 1.421(11) . ? N69 C70 1.107(13) . ? C70 C71 1.664(15) . ? N72 C73 1.132(15) . ? N72 N72 1.31(3) 2_656 ? C73 C74 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 Mn1 N9 71.96(14) . . ? N1 Mn1 N7 72.06(14) . . ? N9 Mn1 N7 143.92(14) . . ? N1 Mn1 Cl2 174.58(10) . . ? N9 Mn1 Cl2 110.87(11) . . ? N7 Mn1 Cl2 104.78(10) . . ? N1 Mn1 Cl1 88.76(10) . . ? N9 Mn1 Cl1 85.19(10) . . ? N7 Mn1 Cl1 96.65(10) . . ? Cl2 Mn1 Cl1 96.04(5) . . ? N1 Mn1 Cl3 80.39(11) . . ? N9 Mn1 Cl3 79.93(10) . . ? N7 Mn1 Cl3 91.56(10) . . ? Cl2 Mn1 Cl3 95.43(5) . . ? Cl1 Mn1 Cl3 163.70(5) . . ? Cl4 Mn2 Cl4 104.89(8) . 2_656 ? Cl4 Mn2 Cl3 114.61(5) . 2_656 ? Cl4 Mn2 Cl3 111.57(5) 2_656 2_656 ? Cl4 Mn2 Cl3 111.57(5) . . ? Cl4 Mn2 Cl3 114.61(5) 2_656 . ? Cl3 Mn2 Cl3 99.94(8) 2_656 . ? Mn1 Cl1 Mn1 156.71(8) 2_556 . ? Mn2 Cl3 Mn1 129.74(6) . . ? C2 N1 C6 119.8(4) . . ? C2 N1 Mn1 120.3(3) . . ? C6 N1 Mn1 119.7(3) . . ? N1 C2 C3 121.9(4) . . ? N1 C2 C7 114.5(4) . . ? C3 C2 C7 123.4(4) . . ? C2 C3 C4 118.2(5) . . ? C5 C4 C3 120.0(5) . . ? C4 C5 C6 118.8(5) . . ? N1 C6 C5 121.2(4) . . ? N1 C6 C9 113.8(4) . . ? C5 C6 C9 125.0(4) . . ? N7 C7 C2 116.2(4) . . ? N7 C7 C8 125.7(4) . . ? C2 C7 C8 118.1(4) . . ? C7 N7 C11 119.4(4) . . ? C7 N7 Mn1 116.7(3) . . ? C11 N7 Mn1 123.6(3) . . ? N9 C9 C6 117.5(4) . . ? N9 C9 C10 125.8(5) . . ? C6 C9 C10 116.7(4) . . ? C9 N9 C18 121.7(4) . . ? C9 N9 Mn1 116.2(3) . . ? C18 N9 Mn1 121.5(3) . . ? C16 C11 C12 120.9(4) . . ? C16 C11 N7 121.4(4) . . ? C12 C11 N7 117.3(4) . . ? C13 C12 C11 120.6(5) . . ? C14 C13 C12 119.2(5) . . ? C13 C14 C15 120.9(5) . . ? C14 C15 C16 120.8(6) . . ? C11 C16 C15 117.5(5) . . ? C11 C16 C17 123.3(4) . . ? C15 C16 C17 119.1(5) . . ? C16 C17 C24 112.6(4) . 2_556 ? C19 C18 C23 120.2(5) . . ? C19 C18 N9 117.7(4) . . ? C23 C18 N9 122.0(4) . . ? C20 C19 C18 121.0(5) . . ? C19 C20 C21 119.6(5) . . ? C22 C21 C20 118.9(5) . . ? C21 C22 C23 123.2(5) . . ? C22 C23 C18 117.0(5) . . ? C22 C23 C24 119.3(4) . . ? C18 C23 C24 123.7(5) . . ? C23 C24 C17 113.2(4) . 2_556 ? N31 Mn3 N39 71.00(14) . . ? N31 Mn3 N37 71.27(14) . . ? N39 Mn3 N37 142.06(14) . . ? N31 Mn3 Cl6 170.79(11) . . ? N39 Mn3 Cl6 108.87(11) . . ? N37 Mn3 Cl6 107.70(10) . . ? N31 Mn3 N60 80.1(2) . . ? N39 Mn3 N60 85.7(2) . . ? N37 Mn3 N60 84.1(2) . . ? Cl6 Mn3 N60 90.74(12) . . ? N31 Mn3 Cl5 90.05(11) . . ? N39 Mn3 Cl5 86.97(10) . . ? N37 Mn3 Cl5 96.92(10) . . ? Cl6 Mn3 Cl5 99.15(5) . . ? N60 Mn3 Cl5 169.20(12) . . ? Mn3 Cl5 Mn3 159.75(8) 2 . ? C36 N31 C32 120.4(4) . . ? C36 N31 Mn3 119.9(3) . . ? C32 N31 Mn3 119.7(3) . . ? N31 C32 C33 121.5(5) . . ? N31 C32 C37 115.1(4) . . ? C33 C32 C37 123.3(5) . . ? C32 C33 C34 118.5(5) . . ? C35 C34 C33 119.6(5) . . ? C34 C35 C36 119.0(5) . . ? N31 C36 C35 120.9(5) . . ? N31 C36 C39 115.1(4) . . ? C35 C36 C39 124.0(4) . . ? N37 C37 C38 125.7(5) . . ? N37 C37 C32 116.9(4) . . ? C38 C37 C32 117.4(4) . . ? C37 N37 C41 119.0(4) . . ? C37 N37 Mn3 116.3(3) . . ? C41 N37 Mn3 124.4(3) . . ? N39 C39 C36 115.5(4) . . ? N39 C39 C40 125.6(5) . . ? C36 C39 C40 118.8(4) . . ? C39 N39 C48 122.8(4) . . ? C39 N39 Mn3 118.3(3) . . ? C48 N39 Mn3 119.0(3) . . ? C46 C41 C42 120.2(4) . . ? C46 C41 N37 122.3(4) . . ? C42 C41 N37 117.4(5) . . ? C43 C42 C41 120.2(5) . . ? C44 C43 C42 119.7(5) . . ? C43 C44 C45 119.5(5) . . ? C44 C45 C46 122.3(5) . . ? C45 C46 C41 118.0(4) . . ? C45 C46 C47 118.9(5) . . ? C41 C46 C47 122.9(4) . . ? C46 C47 C54 111.3(4) . 2 ? C49 C48 C53 121.5(5) . . ? C49 C48 N39 116.0(4) . . ? C53 C48 N39 122.3(4) . . ? C50 C49 C48 119.4(5) . . ? C49 C50 C51 120.3(5) . . ? C50 C51 C52 119.7(5) . . ? C51 C52 C53 122.0(5) . . ? C52 C53 C48 117.0(4) . . ? C52 C53 C54 119.3(4) . . ? C48 C53 C54 123.8(5) . . ? C53 C54 C47 114.6(4) . 2 ? C61 N60 Mn3 148.4(5) . . ? N60 C61 C62 178.8(7) . . ? N63 C64 C65 178.4(9) . . ? N66 C67 C68 178.6(13) . . ? N69 C70 C71 177.9(15) . . ? C73 N72 N72 116.6(13) . 2_656 ? N72 C73 C74 172.2(22) . . ? _refine_diff_density_max 0.516 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.072