# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. Christine McKenzie' _publ_contact_author_email chk@ifk.sdu.dk _publ_section_title ; Tunability of the MII2/MIIMIII and MIIMIII/MIII2 (M = Mn, Co) couples in bis-mu-O,O'- carboxylato-mu-OR bridged complexes ; loop_ _publ_author_name C.McKenzie R.Egdal F.Johanssen S.Veltze A.Bond E.Skou # Attachment '- submit_all.cif' ############################################################################## ## Redox control of the M(II)~2~/M(II)M(III) and M(II)M(III)/Mn(III)~2~ ## ## (M=Mn,Co) couples in bis-mu-O,O'-carboxylate-mu-OR bridged complexes ## ## R.K.Egdal,F.B.Johansson,S.Veltze,A.D.Bond & C.J.McKenzie ## ############################################################################## #TrackingRef '- submit_all.cif' #============================================================================== data_1_2.5MeCN _database_code_depnum_ccdc_archive 'CCDC 772400' #TrackingRef '- submit_all.cif' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C33 H31 Mn2 N6 O9 S2 +, Cl O4 -, 2.5(C2 H3 N) ; _chemical_formula_sum 'C38 H38.50 Cl Mn2 N8.50 O13 S2' _chemical_formula_weight 1031.72 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' S S 0.1246 0.1234 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5539(6) _cell_length_b 12.7614(8) _cell_length_c 17.0757(10) _cell_angle_alpha 100.751(2) _cell_angle_beta 94.365(2) _cell_angle_gamma 94.139(3) _cell_volume 2244.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7941 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 23.35 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1058 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.772 _exptl_absorpt_correction_T_max 0.891 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; One MeCN molecule is ordered and refined with anisotropic displacement parameters. A second MeCN is well resolved, but refined with 50% occupancy to obtain reasonable anisotropic displacement parameters. A third MeCN molecule is less well resolved and is refined in two orientations (each with 50% occupancy) with isotropic displacement parameters. All bond distances and 1,3-distances are restrained in all MeCN molecules: C---N = 1.15(1), C---C = 1.45(1), N...C = 2.60(1) \%A (12 restraints in total). ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 59774 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 25.13 _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_full 0.966 _reflns_number_total 7759 _reflns_number_gt 5964 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+2.3906P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7759 _refine_ls_number_parameters 592 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.898 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.066 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.85821(5) 0.22879(4) 0.17197(3) 0.02885(14) Uani 1 1 d . . . Mn2 Mn 0.55611(5) 0.24325(4) 0.23853(3) 0.03333(15) Uani 1 1 d . . . S1 S 0.80003(8) 0.44514(7) 0.08680(5) 0.0337(2) Uani 1 1 d . . . S2 S 0.69131(8) 0.43968(6) 0.39654(4) 0.0316(2) Uani 1 1 d . . . O1 O 0.7270(2) 0.33913(15) 0.22500(12) 0.0287(5) Uani 1 1 d . . . O2 O 0.8551(2) 0.12279(18) 0.25160(14) 0.0417(6) Uani 1 1 d . . . O3 O 0.6579(3) 0.13068(19) 0.28980(16) 0.0499(6) Uani 1 1 d . . . O4 O 0.7143(2) 0.14268(19) 0.08570(14) 0.0459(6) Uani 1 1 d . . . O5 O 0.5171(3) 0.1486(2) 0.12390(16) 0.0601(8) Uani 1 1 d . . . O11 O 0.8402(2) 0.52704(19) 0.04451(14) 0.0435(6) Uani 1 1 d . . . O12 O 0.6927(2) 0.37324(19) 0.05256(13) 0.0406(6) Uani 1 1 d . . . O21 O 0.6797(2) 0.52025(19) 0.46616(13) 0.0418(6) Uani 1 1 d . . . O22 O 0.7718(2) 0.35667(19) 0.40559(13) 0.0387(5) Uani 1 1 d . . . N1 N 0.9220(2) 0.3687(2) 0.09998(14) 0.0293(6) Uani 1 1 d . . . N2 N 1.0080(2) 0.34381(19) 0.25426(15) 0.0291(6) Uani 1 1 d . . . N3 N 1.0011(3) 0.1632(2) 0.09045(15) 0.0327(6) Uani 1 1 d . . . N4 N 0.5461(2) 0.3775(2) 0.36104(14) 0.0296(6) Uani 1 1 d . . . N5 N 0.4501(3) 0.3766(2) 0.20210(16) 0.0402(7) Uani 1 1 d . . . N6 N 0.3896(3) 0.1934(2) 0.30166(16) 0.0369(7) Uani 1 1 d . . . C1 C 0.7449(3) 0.4441(2) 0.24212(18) 0.0280(7) Uani 1 1 d . . . C2 C 0.7808(3) 0.5066(2) 0.18555(19) 0.0331(7) Uani 1 1 d . . . C3 C 0.7967(4) 0.6176(3) 0.2039(2) 0.0476(9) Uani 1 1 d . . . H3A H 0.8220 0.6559 0.1642 0.057 Uiso 1 1 calc R . . C4 C 0.7764(4) 0.6740(3) 0.2793(2) 0.0521(10) Uani 1 1 d . . . C5 C 0.7447(4) 0.6161(3) 0.3356(2) 0.0435(9) Uani 1 1 d . . . H5A H 0.7324 0.6527 0.3879 0.052 Uiso 1 1 calc R . . C6 C 0.7301(3) 0.5045(2) 0.31852(19) 0.0308(7) Uani 1 1 d . . . C7 C 0.7882(6) 0.7962(3) 0.2972(3) 0.0931(19) Uani 1 1 d . . . H7A H 0.7712 0.8220 0.3528 0.140 Uiso 1 1 calc R . . H7B H 0.7264 0.8222 0.2612 0.140 Uiso 1 1 calc R . . H7C H 0.8747 0.8229 0.2892 0.140 Uiso 1 1 calc R . . C8 C 1.0389(3) 0.4331(2) 0.14231(19) 0.0327(7) Uani 1 1 d . . . H8A H 1.0370 0.5078 0.1340 0.039 Uiso 1 1 calc R . . H8B H 1.1147 0.4039 0.1186 0.039 Uiso 1 1 calc R . . C9 C 1.0515(3) 0.4337(2) 0.23120(18) 0.0292(7) Uani 1 1 d . . . C10 C 1.1112(3) 0.5211(3) 0.2850(2) 0.0383(8) Uani 1 1 d . . . H10A H 1.1388 0.5846 0.2673 0.046 Uiso 1 1 calc R . . C11 C 1.1300(4) 0.5144(3) 0.3648(2) 0.0441(9) Uani 1 1 d . . . H11A H 1.1725 0.5727 0.4027 0.053 Uiso 1 1 calc R . . C12 C 1.0862(3) 0.4221(3) 0.3890(2) 0.0414(8) Uani 1 1 d . . . H12A H 1.0981 0.4157 0.4435 0.050 Uiso 1 1 calc R . . C13 C 1.0251(3) 0.3395(3) 0.33244(19) 0.0340(7) Uani 1 1 d . . . H13A H 0.9935 0.2765 0.3493 0.041 Uiso 1 1 calc R . . C14 C 0.9476(3) 0.3055(3) 0.02073(18) 0.0359(8) Uani 1 1 d . . . H14A H 0.9922 0.3531 -0.0100 0.043 Uiso 1 1 calc R . . H14B H 0.8658 0.2754 -0.0103 0.043 Uiso 1 1 calc R . . C15 C 1.0282(3) 0.2163(3) 0.03222(19) 0.0348(7) Uani 1 1 d . . . C16 C 1.1234(4) 0.1877(3) -0.0168(2) 0.0462(9) Uani 1 1 d . . . H16A H 1.1434 0.2280 -0.0564 0.055 Uiso 1 1 calc R . . C17 C 1.1888(4) 0.1008(3) -0.0080(2) 0.0520(10) Uani 1 1 d . . . H17A H 1.2537 0.0798 -0.0418 0.062 Uiso 1 1 calc R . . C18 C 1.1590(4) 0.0445(3) 0.0507(2) 0.0457(9) Uani 1 1 d . . . H18A H 1.2024 -0.0162 0.0579 0.055 Uiso 1 1 calc R . . C19 C 1.0649(3) 0.0780(3) 0.0985(2) 0.0380(8) Uani 1 1 d . . . H19A H 1.0442 0.0393 0.1389 0.046 Uiso 1 1 calc R . . C20 C 0.4527(3) 0.4547(3) 0.34338(19) 0.0349(7) Uani 1 1 d . . . H20A H 0.4799 0.5260 0.3769 0.042 Uiso 1 1 calc R . . H20B H 0.3681 0.4309 0.3584 0.042 Uiso 1 1 calc R . . C21 C 0.4403(3) 0.4648(3) 0.2565(2) 0.0375(8) Uani 1 1 d . . . C22 C 0.4122(4) 0.5608(3) 0.2356(3) 0.0538(10) Uani 1 1 d . . . H22A H 0.4078 0.6232 0.2753 0.065 Uiso 1 1 calc R . . C23 C 0.3907(4) 0.5629(5) 0.1546(3) 0.0743(15) Uani 1 1 d . . . H23A H 0.3704 0.6274 0.1382 0.089 Uiso 1 1 calc R . . C24 C 0.3985(4) 0.4731(5) 0.0988(3) 0.0694(14) Uani 1 1 d . . . H24A H 0.3834 0.4738 0.0434 0.083 Uiso 1 1 calc R . . C25 C 0.4285(3) 0.3819(4) 0.1241(2) 0.0525(10) Uani 1 1 d . . . H25A H 0.4344 0.3193 0.0850 0.063 Uiso 1 1 calc R . . C26 C 0.5007(3) 0.3111(3) 0.41863(18) 0.0355(8) Uani 1 1 d . . . H26A H 0.4756 0.3583 0.4668 0.043 Uiso 1 1 calc R . . H26B H 0.5705 0.2701 0.4356 0.043 Uiso 1 1 calc R . . C27 C 0.3885(3) 0.2351(3) 0.37966(19) 0.0333(7) Uani 1 1 d . . . C28 C 0.2908(3) 0.2066(3) 0.4231(2) 0.0409(8) Uani 1 1 d . . . H28A H 0.2918 0.2368 0.4784 0.049 Uiso 1 1 calc R . . C29 C 0.1916(4) 0.1339(3) 0.3854(2) 0.0463(9) Uani 1 1 d . . . H29A H 0.1241 0.1129 0.4145 0.056 Uiso 1 1 calc R . . C30 C 0.1919(4) 0.0925(3) 0.3054(2) 0.0466(9) Uani 1 1 d . . . H30A H 0.1239 0.0433 0.2779 0.056 Uiso 1 1 calc R . . C31 C 0.2921(4) 0.1233(3) 0.2657(2) 0.0457(9) Uani 1 1 d . . . H31A H 0.2926 0.0937 0.2104 0.055 Uiso 1 1 calc R . . C32 C 0.7647(4) 0.0965(3) 0.2887(2) 0.0424(9) Uani 1 1 d . . . H32A H 0.7795 0.0436 0.3200 0.051 Uiso 1 1 calc R . . C33 C 0.5978(4) 0.1264(3) 0.0751(2) 0.0553(11) Uani 1 1 d . . . H33A H 0.5644 0.0921 0.0226 0.066 Uiso 1 1 calc R . . Cl1 Cl 0.15128(12) 0.80061(7) 0.20417(6) 0.0592(3) Uani 1 1 d . . . O1A O 0.2076(5) 0.7966(4) 0.2750(2) 0.140(2) Uani 1 1 d . . . O1B O 0.1023(6) 0.6981(2) 0.16365(19) 0.126(2) Uani 1 1 d . . . O1C O 0.0555(6) 0.8634(4) 0.2113(7) 0.251(5) Uani 1 1 d . . . O1D O 0.2214(10) 0.8551(4) 0.1612(3) 0.242(5) Uani 1 1 d . . . N1S N 0.4822(5) 0.7656(4) 0.4119(2) 0.0928(15) Uani 1 1 d D . . C1S C 0.4752(5) 0.8474(4) 0.3959(3) 0.0683(13) Uani 1 1 d D . . C2S C 0.4651(6) 0.9506(4) 0.3745(5) 0.110(2) Uani 1 1 d D . . H21 H 0.4193 0.9951 0.4141 0.165 Uiso 1 1 d R . . H22 H 0.4183 0.9416 0.3215 0.165 Uiso 1 1 d R . . H23 H 0.5506 0.9853 0.3734 0.165 Uiso 1 1 d R . . N2S N 0.6006(13) 0.7405(9) 0.0821(7) 0.126(4) Uani 0.50 1 d PD . . C3S C 0.5464(13) 0.8073(9) 0.1156(9) 0.120(5) Uani 0.50 1 d PD . . C4S C 0.5020(14) 0.9013(8) 0.1620(8) 0.112(4) Uani 0.50 1 d PD . . H41 H 0.5420 0.9132 0.2170 0.168 Uiso 0.50 1 d PR . . H42 H 0.4091 0.8917 0.1624 0.168 Uiso 0.50 1 d PR . . H43 H 0.5250 0.9633 0.1380 0.168 Uiso 0.50 1 d PR . . N3S N 0.2318(11) 0.9812(8) 0.5253(7) 0.112(3) Uiso 0.50 1 d PD A 1 C5S C 0.1789(11) 0.9011(8) 0.4953(6) 0.073(3) Uiso 0.50 1 d PD A 1 C6S C 0.0848(14) 0.8087(10) 0.4600(9) 0.098(5) Uiso 0.50 1 d PD A 1 H61 H 0.0842 0.7572 0.4960 0.147 Uiso 0.50 1 d PR A 1 H62 H 0.1106 0.7747 0.4081 0.147 Uiso 0.50 1 d PR A 1 H63 H -0.0009 0.8323 0.4527 0.147 Uiso 0.50 1 d PR A 1 N3S' N 0.1309(13) 0.9944(8) 0.5230(7) 0.124(4) Uiso 0.50 1 d PD B 2 C5S' C 0.1139(12) 0.9051(8) 0.4925(7) 0.075(3) Uiso 0.50 1 d PD B 2 C6S' C 0.1305(15) 0.7944(8) 0.4614(9) 0.096(5) Uiso 0.50 1 d PD B 2 H64 H 0.1384 0.7841 0.4037 0.145 Uiso 0.50 1 d PR B 2 H65 H 0.0590 0.7468 0.4714 0.145 Uiso 0.50 1 d PR B 2 H66 H 0.2095 0.7778 0.4887 0.145 Uiso 0.50 1 d PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0374(3) 0.0249(2) 0.0246(2) 0.00531(19) 0.0053(2) 0.0012(2) Mn2 0.0385(3) 0.0340(3) 0.0264(3) 0.0029(2) 0.0067(2) -0.0004(2) S1 0.0403(5) 0.0373(4) 0.0277(4) 0.0154(3) 0.0030(4) 0.0064(4) S2 0.0346(5) 0.0367(4) 0.0223(4) 0.0031(3) 0.0000(3) 0.0041(4) O1 0.0373(12) 0.0242(11) 0.0254(11) 0.0062(9) 0.0043(9) 0.0030(9) O2 0.0496(15) 0.0352(13) 0.0456(14) 0.0183(11) 0.0107(12) 0.0042(11) O3 0.0546(17) 0.0405(14) 0.0625(17) 0.0226(12) 0.0197(14) 0.0099(13) O4 0.0458(16) 0.0463(14) 0.0387(14) -0.0072(11) 0.0043(12) -0.0021(12) O5 0.0497(16) 0.0728(19) 0.0437(15) -0.0207(14) 0.0110(13) -0.0127(14) O11 0.0548(16) 0.0454(14) 0.0383(13) 0.0260(11) 0.0069(12) 0.0078(12) O12 0.0388(14) 0.0528(14) 0.0301(12) 0.0121(11) -0.0039(11) 0.0004(12) O21 0.0446(14) 0.0499(14) 0.0253(12) -0.0047(10) 0.0001(11) 0.0000(11) O22 0.0378(13) 0.0485(14) 0.0325(12) 0.0140(11) 0.0014(10) 0.0085(11) N1 0.0374(15) 0.0292(13) 0.0222(13) 0.0071(11) 0.0035(12) 0.0024(12) N2 0.0324(15) 0.0278(13) 0.0276(13) 0.0066(11) -0.0002(12) 0.0045(11) N3 0.0400(16) 0.0307(14) 0.0258(13) 0.0023(11) 0.0037(12) 0.0002(12) N4 0.0333(15) 0.0328(14) 0.0230(13) 0.0052(11) 0.0025(11) 0.0045(12) N5 0.0346(16) 0.0604(19) 0.0273(14) 0.0149(14) -0.0008(13) 0.0031(14) N6 0.0397(17) 0.0392(16) 0.0302(15) 0.0023(12) 0.0062(13) 0.0002(14) C1 0.0267(16) 0.0282(16) 0.0292(16) 0.0064(13) -0.0013(13) 0.0040(13) C2 0.0400(19) 0.0298(17) 0.0311(17) 0.0088(14) 0.0021(15) 0.0081(14) C3 0.064(3) 0.0334(19) 0.053(2) 0.0195(17) 0.015(2) 0.0125(17) C4 0.078(3) 0.0246(17) 0.056(2) 0.0072(17) 0.018(2) 0.0084(18) C5 0.055(2) 0.0315(18) 0.043(2) -0.0001(16) 0.0132(18) 0.0048(16) C6 0.0308(17) 0.0307(16) 0.0305(16) 0.0052(13) 0.0013(14) 0.0030(14) C7 0.160(6) 0.030(2) 0.094(4) 0.007(2) 0.050(4) 0.011(3) C8 0.0383(19) 0.0283(16) 0.0317(17) 0.0093(14) 0.0017(15) -0.0024(14) C9 0.0295(17) 0.0273(16) 0.0313(17) 0.0077(13) 0.0003(14) 0.0041(13) C10 0.039(2) 0.0318(17) 0.043(2) 0.0083(15) -0.0041(16) 0.0019(15) C11 0.045(2) 0.040(2) 0.040(2) -0.0045(16) -0.0080(17) 0.0029(17) C12 0.045(2) 0.049(2) 0.0291(18) 0.0058(16) -0.0040(16) 0.0082(17) C13 0.0351(18) 0.0363(18) 0.0322(17) 0.0107(15) -0.0010(15) 0.0074(15) C14 0.047(2) 0.0376(18) 0.0246(16) 0.0095(14) 0.0079(15) 0.0012(16) C15 0.042(2) 0.0315(17) 0.0284(17) 0.0021(14) 0.0039(15) -0.0045(15) C16 0.057(2) 0.044(2) 0.039(2) 0.0055(16) 0.0182(18) 0.0015(18) C17 0.056(2) 0.046(2) 0.052(2) -0.0002(18) 0.019(2) 0.0061(19) C18 0.052(2) 0.0352(19) 0.047(2) -0.0011(17) 0.0033(19) 0.0082(17) C19 0.047(2) 0.0313(17) 0.0336(18) 0.0017(14) 0.0027(16) 0.0034(16) C20 0.0362(19) 0.0355(17) 0.0337(17) 0.0063(14) 0.0028(15) 0.0087(15) C21 0.0284(18) 0.049(2) 0.0381(19) 0.0159(17) 0.0013(15) 0.0034(15) C22 0.046(2) 0.056(2) 0.068(3) 0.030(2) 0.007(2) 0.0132(19) C23 0.057(3) 0.099(4) 0.090(4) 0.070(3) 0.009(3) 0.023(3) C24 0.044(2) 0.128(5) 0.051(3) 0.052(3) 0.000(2) 0.018(3) C25 0.036(2) 0.092(3) 0.0313(19) 0.020(2) -0.0027(17) 0.005(2) C26 0.043(2) 0.0412(19) 0.0235(16) 0.0085(14) 0.0056(15) 0.0028(16) C27 0.0384(19) 0.0331(17) 0.0313(17) 0.0103(14) 0.0060(15) 0.0082(15) C28 0.046(2) 0.045(2) 0.0358(19) 0.0121(16) 0.0118(17) 0.0080(18) C29 0.044(2) 0.044(2) 0.056(2) 0.0185(18) 0.0143(19) 0.0045(18) C30 0.043(2) 0.038(2) 0.056(2) 0.0066(17) 0.0062(19) -0.0035(17) C31 0.046(2) 0.049(2) 0.038(2) 0.0010(17) 0.0038(18) -0.0033(18) C32 0.055(2) 0.0317(18) 0.046(2) 0.0179(16) 0.0111(19) 0.0072(17) C33 0.050(3) 0.066(3) 0.036(2) -0.0209(19) 0.004(2) -0.010(2) Cl1 0.0995(9) 0.0299(5) 0.0448(5) 0.0099(4) -0.0143(5) -0.0024(5) O1A 0.207(5) 0.112(3) 0.085(3) 0.051(2) -0.082(3) -0.065(3) O1B 0.267(6) 0.0445(18) 0.0513(19) 0.0155(15) -0.041(3) -0.045(3) O1C 0.133(5) 0.062(3) 0.527(16) 0.011(5) -0.056(7) 0.016(3) O1D 0.489(14) 0.125(4) 0.093(4) 0.028(3) 0.060(5) -0.157(6) N1S 0.142(4) 0.083(3) 0.062(3) 0.035(2) -0.001(3) 0.027(3) C1S 0.083(3) 0.072(3) 0.054(3) 0.023(2) -0.003(2) 0.016(3) C2S 0.104(5) 0.076(4) 0.161(6) 0.057(4) -0.002(4) 0.010(3) N2S 0.148(11) 0.132(10) 0.120(9) 0.050(8) 0.071(8) 0.034(8) C3S 0.099(10) 0.140(14) 0.145(14) 0.082(12) 0.050(9) -0.002(9) C4S 0.143(12) 0.061(7) 0.121(10) -0.011(7) 0.005(9) 0.022(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 Mn1 Mn2 3.4712(7) . ? Mn1 O2 2.090(2) . ? Mn1 O4 2.121(3) . ? Mn1 O1 2.172(2) . ? Mn1 N3 2.232(3) . ? Mn1 N2 2.277(3) . ? Mn1 N1 2.434(2) . ? Mn2 O5 2.093(2) . ? Mn2 O3 2.129(3) . ? Mn2 O1 2.158(2) . ? Mn2 N6 2.244(3) . ? Mn2 N5 2.258(3) . ? Mn2 N4 2.459(2) . ? S1 O12 1.420(2) . ? S1 O11 1.434(2) . ? S1 N1 1.696(3) . ? S1 C2 1.755(3) . ? S2 O22 1.428(2) . ? S2 O21 1.439(2) . ? S2 N4 1.688(3) . ? S2 C6 1.753(3) . ? O1 C1 1.313(3) . ? O2 C32 1.245(4) . ? O3 C32 1.238(4) . ? O4 C33 1.227(5) . ? O5 C33 1.246(4) . ? N1 C8 1.489(4) . ? N1 C14 1.495(4) . ? N2 C9 1.342(4) . ? N2 C13 1.345(4) . ? N3 C15 1.340(4) . ? N3 C19 1.342(4) . ? N4 C20 1.496(4) . ? N4 C26 1.497(4) . ? N5 C21 1.336(5) . ? N5 C25 1.350(4) . ? N6 C27 1.340(4) . ? N6 C31 1.343(5) . ? C1 C6 1.412(4) . ? C1 C2 1.419(4) . ? C2 C3 1.387(5) . ? C3 C4 1.393(5) . ? C3 H3A 0.950 . ? C4 C5 1.365(5) . ? C4 C7 1.526(5) . ? C5 C6 1.394(4) . ? C5 H5A 0.950 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.512(4) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 C10 1.383(5) . ? C10 C11 1.383(5) . ? C10 H10A 0.950 . ? C11 C12 1.379(5) . ? C11 H11A 0.950 . ? C12 C13 1.373(5) . ? C12 H12A 0.950 . ? C13 H13A 0.950 . ? C14 C15 1.503(5) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.381(5) . ? C16 C17 1.374(5) . ? C16 H16A 0.950 . ? C17 C18 1.381(5) . ? C17 H17A 0.950 . ? C18 C19 1.374(5) . ? C18 H18A 0.950 . ? C19 H19A 0.950 . ? C20 C21 1.509(4) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C21 C22 1.384(5) . ? C22 C23 1.390(6) . ? C22 H22A 0.950 . ? C23 C24 1.360(7) . ? C23 H23A 0.950 . ? C24 C25 1.363(6) . ? C24 H24A 0.950 . ? C25 H25A 0.950 . ? C26 C27 1.503(5) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.382(5) . ? C28 C29 1.380(5) . ? C28 H28A 0.950 . ? C29 C30 1.371(5) . ? C29 H29A 0.950 . ? C30 C31 1.371(5) . ? C30 H30A 0.950 . ? C31 H31A 0.950 . ? C32 H32A 0.950 . ? C33 H33A 0.950 . ? Cl1 O1A 1.318(4) . ? Cl1 O1D 1.329(5) . ? Cl1 O1C 1.334(6) . ? Cl1 O1B 1.403(3) . ? N1S C1S 1.134(5) . ? C1S C2S 1.439(5) . ? C2S H21 0.980 . ? C2S H22 0.980 . ? C2S H23 0.980 . ? N2S C3S 1.148(8) . ? C3S C4S 1.439(8) . ? C4S H41 0.980 . ? C4S H42 0.980 . ? C4S H43 0.980 . ? N3S C5S 1.139(7) . ? C5S C6S 1.488(8) . ? C6S H61 0.980 . ? C6S H62 0.980 . ? C6S H63 0.980 . ? N3S' C5S' 1.156(8) . ? C5S' C6S' 1.441(8) . ? C6S' H64 0.980 . ? C6S' H65 0.980 . ? C6S' H66 0.980 . ? 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 O2 Mn1 O4 97.23(10) . . ? O2 Mn1 O1 99.44(8) . . ? O4 Mn1 O1 92.65(9) . . ? O2 Mn1 N3 101.91(9) . . ? O4 Mn1 N3 87.56(9) . . ? O1 Mn1 N3 158.45(9) . . ? O2 Mn1 N2 91.76(9) . . ? O4 Mn1 N2 170.70(9) . . ? O1 Mn1 N2 83.51(8) . . ? N3 Mn1 N2 92.92(9) . . ? O2 Mn1 N1 163.43(9) . . ? O4 Mn1 N1 98.37(9) . . ? O1 Mn1 N1 85.39(8) . . ? N3 Mn1 N1 73.28(9) . . ? N2 Mn1 N1 72.93(9) . . ? O5 Mn2 O3 96.56(12) . . ? O5 Mn2 O1 101.72(9) . . ? O3 Mn2 O1 93.67(9) . . ? O5 Mn2 N6 102.39(10) . . ? O3 Mn2 N6 86.89(10) . . ? O1 Mn2 N6 155.65(9) . . ? O5 Mn2 N5 91.56(11) . . ? O3 Mn2 N5 171.80(10) . . ? O1 Mn2 N5 85.68(9) . . ? N6 Mn2 N5 90.35(10) . . ? O5 Mn2 N4 163.37(10) . . ? O3 Mn2 N4 98.46(9) . . ? O1 Mn2 N4 84.41(8) . . ? N6 Mn2 N4 71.46(9) . . ? N5 Mn2 N4 73.34(9) . . ? O12 S1 O11 118.00(14) . . ? O12 S1 N1 106.39(14) . . ? O11 S1 N1 109.60(14) . . ? O12 S1 C2 111.52(15) . . ? O11 S1 C2 108.08(15) . . ? N1 S1 C2 102.06(14) . . ? O22 S2 O21 117.61(14) . . ? O22 S2 N4 105.99(14) . . ? O21 S2 N4 109.65(14) . . ? O22 S2 C6 112.54(14) . . ? O21 S2 C6 108.11(15) . . ? N4 S2 C6 101.72(14) . . ? C1 O1 Mn2 126.25(18) . . ? C1 O1 Mn1 127.06(19) . . ? Mn2 O1 Mn1 106.61(8) . . ? C32 O2 Mn1 127.9(2) . . ? C32 O3 Mn2 138.2(2) . . ? C33 O4 Mn1 139.9(2) . . ? C33 O5 Mn2 125.0(3) . . ? C8 N1 C14 111.7(2) . . ? C8 N1 S1 112.4(2) . . ? C14 N1 S1 109.3(2) . . ? C8 N1 Mn1 109.96(17) . . ? C14 N1 Mn1 102.23(17) . . ? S1 N1 Mn1 110.72(12) . . ? C9 N2 C13 118.1(3) . . ? C9 N2 Mn1 119.03(19) . . ? C13 N2 Mn1 120.1(2) . . ? C15 N3 C19 118.6(3) . . ? C15 N3 Mn1 117.0(2) . . ? C19 N3 Mn1 124.3(2) . . ? C20 N4 C26 112.3(2) . . ? C20 N4 S2 112.1(2) . . ? C26 N4 S2 109.2(2) . . ? C20 N4 Mn2 108.32(18) . . ? C26 N4 Mn2 102.69(18) . . ? S2 N4 Mn2 111.78(12) . . ? C21 N5 C25 118.0(3) . . ? C21 N5 Mn2 119.1(2) . . ? C25 N5 Mn2 120.4(3) . . ? C27 N6 C31 118.4(3) . . ? C27 N6 Mn2 118.0(2) . . ? C31 N6 Mn2 123.5(2) . . ? O1 C1 C6 122.9(3) . . ? O1 C1 C2 123.0(3) . . ? C6 C1 C2 114.2(3) . . ? C3 C2 C1 122.4(3) . . ? C3 C2 S1 117.1(3) . . ? C1 C2 S1 120.5(2) . . ? C2 C3 C4 121.4(3) . . ? C2 C3 H3A 119.3 . . ? C4 C3 H3A 119.3 . . ? C5 C4 C3 117.6(3) . . ? C5 C4 C7 121.7(4) . . ? C3 C4 C7 120.7(4) . . ? C4 C5 C6 121.7(3) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C5 C6 C1 122.7(3) . . ? C5 C6 S2 117.2(2) . . ? C1 C6 S2 120.2(2) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 112.9(2) . . ? N1 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? N1 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N2 C9 C10 122.3(3) . . ? N2 C9 C8 116.7(3) . . ? C10 C9 C8 120.9(3) . . ? C11 C10 C9 118.8(3) . . ? C11 C10 H10A 120.6 . . ? C9 C10 H10A 120.6 . . ? C12 C11 C10 119.3(3) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? C13 C12 C11 118.6(3) . . ? C13 C12 H12A 120.7 . . ? C11 C12 H12A 120.7 . . ? N2 C13 C12 123.0(3) . . ? N2 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? N1 C14 C15 110.3(3) . . ? N1 C14 H14A 109.6 . . ? C15 C14 H14A 109.6 . . ? N1 C14 H14B 109.6 . . ? C15 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? N3 C15 C16 121.3(3) . . ? N3 C15 C14 117.1(3) . . ? C16 C15 C14 121.5(3) . . ? C17 C16 C15 119.7(3) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C16 C17 C18 119.0(3) . . ? C16 C17 H17A 120.5 . . ? C18 C17 H17A 120.5 . . ? C19 C18 C17 118.5(3) . . ? C19 C18 H18A 120.7 . . ? C17 C18 H18A 120.7 . . ? N3 C19 C18 122.7(3) . . ? N3 C19 H19A 118.6 . . ? C18 C19 H19A 118.6 . . ? N4 C20 C21 113.2(3) . . ? N4 C20 H20A 108.9 . . ? C21 C20 H20A 108.9 . . ? N4 C20 H20B 108.9 . . ? C21 C20 H20B 108.9 . . ? H20A C20 H20B 107.8 . . ? N5 C21 C22 122.4(3) . . ? N5 C21 C20 117.2(3) . . ? C22 C21 C20 120.3(3) . . ? C21 C22 C23 117.8(4) . . ? C21 C22 H22A 121.1 . . ? C23 C22 H22A 121.1 . . ? C24 C23 C22 120.2(4) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C23 C24 C25 118.6(4) . . ? C23 C24 H24A 120.7 . . ? C25 C24 H24A 120.7 . . ? N5 C25 C24 123.0(4) . . ? N5 C25 H25A 118.5 . . ? C24 C25 H25A 118.5 . . ? N4 C26 C27 109.9(2) . . ? N4 C26 H26A 109.7 . . ? C27 C26 H26A 109.7 . . ? N4 C26 H26B 109.7 . . ? C27 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? N6 C27 C28 121.5(3) . . ? N6 C27 C26 117.1(3) . . ? C28 C27 C26 121.4(3) . . ? C29 C28 C27 119.4(3) . . ? C29 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? C30 C29 C28 119.1(3) . . ? C30 C29 H29A 120.5 . . ? C28 C29 H29A 120.5 . . ? C29 C30 C31 118.8(4) . . ? C29 C30 H30A 120.6 . . ? C31 C30 H30A 120.6 . . ? N6 C31 C30 122.8(3) . . ? N6 C31 H31A 118.6 . . ? C30 C31 H31A 118.6 . . ? O3 C32 O2 128.0(3) . . ? O3 C32 H32A 116.0 . . ? O2 C32 H32A 116.0 . . ? O4 C33 O5 128.8(3) . . ? O4 C33 H33A 115.6 . . ? O5 C33 H33A 115.6 . . ? O1A Cl1 O1D 113.9(4) . . ? O1A Cl1 O1C 110.8(5) . . ? O1D Cl1 O1C 97.8(6) . . ? O1A Cl1 O1B 110.8(2) . . ? O1D Cl1 O1B 114.3(3) . . ? O1C Cl1 O1B 108.4(4) . . ? N1S C1S C2S 179.1(6) . . ? C1S C2S H21 109.3 . . ? C1S C2S H22 109.5 . . ? H21 C2S H22 109.5 . . ? C1S C2S H23 109.5 . . ? H21 C2S H23 109.5 . . ? H22 C2S H23 109.5 . . ? N2S C3S C4S 169.2(17) . . ? C3S C4S H41 109.6 . . ? C3S C4S H42 109.7 . . ? H41 C4S H42 109.5 . . ? C3S C4S H43 109.1 . . ? H41 C4S H43 109.5 . . ? H42 C4S H43 109.5 . . ? N3S C5S C6S 167.6(15) . . ? C5S C6S H61 108.9 . . ? C5S C6S H62 108.7 . . ? H61 C6S H62 109.5 . . ? C5S C6S H63 110.8 . . ? H61 C6S H63 109.5 . . ? H62 C6S H63 109.5 . . ? N3S' C5S' C6S' 163.8(16) . . ? C5S' C6S' H64 109.8 . . ? C5S' C6S' H65 111.5 . . ? C5S' C6S' H66 107.1 . . ? H64 C6S' H65 109.5 . . ? H64 C6S' H66 109.5 . . ? H65 C6S' H66 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Mn2 O1 C1 126.4(2) . . . . ? O3 Mn2 O1 C1 -136.1(2) . . . . ? N6 Mn2 O1 C1 -45.5(3) . . . . ? N5 Mn2 O1 C1 35.7(2) . . . . ? N4 Mn2 O1 C1 -37.9(2) . . . . ? O5 Mn2 O1 Mn1 -50.63(12) . . . . ? O3 Mn2 O1 Mn1 46.86(10) . . . . ? N6 Mn2 O1 Mn1 137.4(2) . . . . ? N5 Mn2 O1 Mn1 -141.33(10) . . . . ? N4 Mn2 O1 Mn1 145.02(9) . . . . ? O2 Mn1 O1 C1 130.8(2) . . . . ? O4 Mn1 O1 C1 -131.4(2) . . . . ? N3 Mn1 O1 C1 -41.3(4) . . . . ? N2 Mn1 O1 C1 40.1(2) . . . . ? N1 Mn1 O1 C1 -33.2(2) . . . . ? O2 Mn1 O1 Mn2 -52.13(10) . . . . ? O4 Mn1 O1 Mn2 45.65(10) . . . . ? N3 Mn1 O1 Mn2 135.7(2) . . . . ? N2 Mn1 O1 Mn2 -142.85(10) . . . . ? N1 Mn1 O1 Mn2 143.84(10) . . . . ? O4 Mn1 O2 C32 -61.7(3) . . . . ? O1 Mn1 O2 C32 32.2(3) . . . . ? N3 Mn1 O2 C32 -150.7(3) . . . . ? N2 Mn1 O2 C32 115.9(3) . . . . ? N1 Mn1 O2 C32 138.1(3) . . . . ? O5 Mn2 O3 C32 76.2(4) . . . . ? O1 Mn2 O3 C32 -26.1(4) . . . . ? N6 Mn2 O3 C32 178.3(4) . . . . ? N4 Mn2 O3 C32 -111.0(4) . . . . ? O2 Mn1 O4 C33 78.1(4) . . . . ? O1 Mn1 O4 C33 -21.7(4) . . . . ? N3 Mn1 O4 C33 179.9(4) . . . . ? N1 Mn1 O4 C33 -107.4(4) . . . . ? O3 Mn2 O5 C33 -70.7(4) . . . . ? O1 Mn2 O5 C33 24.4(4) . . . . ? N6 Mn2 O5 C33 -159.0(4) . . . . ? N5 Mn2 O5 C33 110.3(4) . . . . ? N4 Mn2 O5 C33 134.7(4) . . . . ? O12 S1 N1 C8 -174.99(19) . . . . ? O11 S1 N1 C8 56.4(2) . . . . ? C2 S1 N1 C8 -58.0(2) . . . . ? O12 S1 N1 C14 60.3(2) . . . . ? O11 S1 N1 C14 -68.3(2) . . . . ? C2 S1 N1 C14 177.3(2) . . . . ? O12 S1 N1 Mn1 -51.55(15) . . . . ? O11 S1 N1 Mn1 179.83(13) . . . . ? C2 S1 N1 Mn1 65.44(16) . . . . ? O2 Mn1 N1 C8 -10.9(4) . . . . ? O4 Mn1 N1 C8 -171.07(19) . . . . ? O1 Mn1 N1 C8 96.92(19) . . . . ? N3 Mn1 N1 C8 -86.2(2) . . . . ? N2 Mn1 N1 C8 12.31(18) . . . . ? O2 Mn1 N1 C14 107.9(3) . . . . ? O4 Mn1 N1 C14 -52.3(2) . . . . ? O1 Mn1 N1 C14 -144.28(19) . . . . ? N3 Mn1 N1 C14 32.60(19) . . . . ? N2 Mn1 N1 C14 131.1(2) . . . . ? O2 Mn1 N1 S1 -135.7(3) . . . . ? O4 Mn1 N1 S1 64.08(14) . . . . ? O1 Mn1 N1 S1 -27.93(12) . . . . ? N3 Mn1 N1 S1 148.96(15) . . . . ? N2 Mn1 N1 S1 -112.54(14) . . . . ? O2 Mn1 N2 C9 179.0(2) . . . . ? O1 Mn1 N2 C9 -81.7(2) . . . . ? N3 Mn1 N2 C9 77.0(2) . . . . ? N1 Mn1 N2 C9 5.5(2) . . . . ? O2 Mn1 N2 C13 -20.3(2) . . . . ? O1 Mn1 N2 C13 79.0(2) . . . . ? N3 Mn1 N2 C13 -122.3(2) . . . . ? N1 Mn1 N2 C13 166.2(2) . . . . ? O2 Mn1 N3 C15 -178.3(2) . . . . ? O4 Mn1 N3 C15 84.9(2) . . . . ? O1 Mn1 N3 C15 -6.2(4) . . . . ? N2 Mn1 N3 C15 -85.9(2) . . . . ? N1 Mn1 N3 C15 -14.6(2) . . . . ? O2 Mn1 N3 C19 -1.5(3) . . . . ? O4 Mn1 N3 C19 -98.4(3) . . . . ? O1 Mn1 N3 C19 170.6(2) . . . . ? N2 Mn1 N3 C19 90.9(3) . . . . ? N1 Mn1 N3 C19 162.1(3) . . . . ? O22 S2 N4 C20 -176.3(2) . . . . ? O21 S2 N4 C20 55.8(2) . . . . ? C6 S2 N4 C20 -58.5(2) . . . . ? O22 S2 N4 C26 58.5(2) . . . . ? O21 S2 N4 C26 -69.4(2) . . . . ? C6 S2 N4 C26 176.3(2) . . . . ? O22 S2 N4 Mn2 -54.42(15) . . . . ? O21 S2 N4 Mn2 177.67(12) . . . . ? C6 S2 N4 Mn2 63.39(15) . . . . ? O5 Mn2 N4 C20 -13.1(4) . . . . ? O3 Mn2 N4 C20 -167.51(19) . . . . ? O1 Mn2 N4 C20 99.60(19) . . . . ? N6 Mn2 N4 C20 -83.7(2) . . . . ? N5 Mn2 N4 C20 12.45(19) . . . . ? O5 Mn2 N4 C26 105.9(4) . . . . ? O3 Mn2 N4 C26 -48.5(2) . . . . ? O1 Mn2 N4 C26 -141.40(19) . . . . ? N6 Mn2 N4 C26 35.30(19) . . . . ? N5 Mn2 N4 C26 131.4(2) . . . . ? O5 Mn2 N4 S2 -137.1(3) . . . . ? O3 Mn2 N4 S2 68.46(14) . . . . ? O1 Mn2 N4 S2 -24.43(12) . . . . ? N6 Mn2 N4 S2 152.27(15) . . . . ? N5 Mn2 N4 S2 -111.58(14) . . . . ? O5 Mn2 N5 C21 178.4(3) . . . . ? O1 Mn2 N5 C21 -79.9(2) . . . . ? N6 Mn2 N5 C21 76.0(3) . . . . ? N4 Mn2 N5 C21 5.5(2) . . . . ? O5 Mn2 N5 C25 -20.0(3) . . . . ? O1 Mn2 N5 C25 81.6(3) . . . . ? N6 Mn2 N5 C25 -122.4(3) . . . . ? N4 Mn2 N5 C25 167.1(3) . . . . ? O5 Mn2 N6 C27 176.0(2) . . . . ? O3 Mn2 N6 C27 80.0(2) . . . . ? O1 Mn2 N6 C27 -12.0(4) . . . . ? N5 Mn2 N6 C27 -92.3(2) . . . . ? N4 Mn2 N6 C27 -20.0(2) . . . . ? O5 Mn2 N6 C31 -3.1(3) . . . . ? O3 Mn2 N6 C31 -99.2(3) . . . . ? O1 Mn2 N6 C31 168.8(2) . . . . ? N5 Mn2 N6 C31 88.6(3) . . . . ? N4 Mn2 N6 C31 160.8(3) . . . . ? Mn2 O1 C1 C6 56.1(4) . . . . ? Mn1 O1 C1 C6 -127.4(3) . . . . ? Mn2 O1 C1 C2 -123.9(3) . . . . ? Mn1 O1 C1 C2 52.6(4) . . . . ? O1 C1 C2 C3 178.6(3) . . . . ? C6 C1 C2 C3 -1.4(5) . . . . ? O1 C1 C2 S1 1.4(4) . . . . ? C6 C1 C2 S1 -178.6(2) . . . . ? O12 S1 C2 C3 -126.7(3) . . . . ? O11 S1 C2 C3 4.6(3) . . . . ? N1 S1 C2 C3 120.1(3) . . . . ? O12 S1 C2 C1 50.6(3) . . . . ? O11 S1 C2 C1 -178.1(3) . . . . ? N1 S1 C2 C1 -62.6(3) . . . . ? C1 C2 C3 C4 -0.9(6) . . . . ? S1 C2 C3 C4 176.3(3) . . . . ? C2 C3 C4 C5 2.4(6) . . . . ? C2 C3 C4 C7 -177.1(4) . . . . ? C3 C4 C5 C6 -1.5(6) . . . . ? C7 C4 C5 C6 178.0(4) . . . . ? C4 C5 C6 C1 -1.0(6) . . . . ? C4 C5 C6 S2 179.2(3) . . . . ? O1 C1 C6 C5 -177.6(3) . . . . ? C2 C1 C6 C5 2.3(5) . . . . ? O1 C1 C6 S2 2.2(4) . . . . ? C2 C1 C6 S2 -177.8(2) . . . . ? O22 S2 C6 C5 -130.5(3) . . . . ? O21 S2 C6 C5 1.0(3) . . . . ? N4 S2 C6 C5 116.5(3) . . . . ? O22 S2 C6 C1 49.6(3) . . . . ? O21 S2 C6 C1 -178.8(2) . . . . ? N4 S2 C6 C1 -63.4(3) . . . . ? C14 N1 C8 C9 -139.8(3) . . . . ? S1 N1 C8 C9 96.9(3) . . . . ? Mn1 N1 C8 C9 -27.0(3) . . . . ? C13 N2 C9 C10 -0.8(4) . . . . ? Mn1 N2 C9 C10 160.3(2) . . . . ? C13 N2 C9 C8 175.9(3) . . . . ? Mn1 N2 C9 C8 -22.9(3) . . . . ? N1 C8 C9 N2 34.0(4) . . . . ? N1 C8 C9 C10 -149.2(3) . . . . ? N2 C9 C10 C11 2.0(5) . . . . ? C8 C9 C10 C11 -174.7(3) . . . . ? C9 C10 C11 C12 -1.5(5) . . . . ? C10 C11 C12 C13 0.0(5) . . . . ? C9 N2 C13 C12 -0.8(5) . . . . ? Mn1 N2 C13 C12 -161.7(3) . . . . ? C11 C12 C13 N2 1.2(5) . . . . ? C8 N1 C14 C15 70.5(3) . . . . ? S1 N1 C14 C15 -164.5(2) . . . . ? Mn1 N1 C14 C15 -47.1(3) . . . . ? C19 N3 C15 C16 -2.7(5) . . . . ? Mn1 N3 C15 C16 174.2(3) . . . . ? C19 N3 C15 C14 175.1(3) . . . . ? Mn1 N3 C15 C14 -7.9(4) . . . . ? N1 C14 C15 N3 40.7(4) . . . . ? N1 C14 C15 C16 -141.5(3) . . . . ? N3 C15 C16 C17 2.4(5) . . . . ? C14 C15 C16 C17 -175.3(3) . . . . ? C15 C16 C17 C18 -0.9(6) . . . . ? C16 C17 C18 C19 -0.3(6) . . . . ? C15 N3 C19 C18 1.5(5) . . . . ? Mn1 N3 C19 C18 -175.1(3) . . . . ? C17 C18 C19 N3 0.0(5) . . . . ? C26 N4 C20 C21 -140.1(3) . . . . ? S2 N4 C20 C21 96.4(3) . . . . ? Mn2 N4 C20 C21 -27.4(3) . . . . ? C25 N5 C21 C22 -1.7(5) . . . . ? Mn2 N5 C21 C22 160.3(3) . . . . ? C25 N5 C21 C20 174.4(3) . . . . ? Mn2 N5 C21 C20 -23.6(4) . . . . ? N4 C20 C21 N5 35.1(4) . . . . ? N4 C20 C21 C22 -148.7(3) . . . . ? N5 C21 C22 C23 1.7(6) . . . . ? C20 C21 C22 C23 -174.4(3) . . . . ? C21 C22 C23 C24 -0.6(6) . . . . ? C22 C23 C24 C25 -0.4(7) . . . . ? C21 N5 C25 C24 0.6(5) . . . . ? Mn2 N5 C25 C24 -161.1(3) . . . . ? C23 C24 C25 N5 0.4(6) . . . . ? C20 N4 C26 C27 68.7(3) . . . . ? S2 N4 C26 C27 -166.2(2) . . . . ? Mn2 N4 C26 C27 -47.4(3) . . . . ? C31 N6 C27 C28 0.6(5) . . . . ? Mn2 N6 C27 C28 -178.6(2) . . . . ? C31 N6 C27 C26 178.4(3) . . . . ? Mn2 N6 C27 C26 -0.8(4) . . . . ? N4 C26 C27 N6 36.1(4) . . . . ? N4 C26 C27 C28 -146.1(3) . . . . ? N6 C27 C28 C29 -0.2(5) . . . . ? C26 C27 C28 C29 -178.0(3) . . . . ? C27 C28 C29 C30 -0.7(5) . . . . ? C28 C29 C30 C31 1.2(5) . . . . ? C27 N6 C31 C30 -0.1(5) . . . . ? Mn2 N6 C31 C30 179.1(3) . . . . ? C29 C30 C31 N6 -0.8(6) . . . . ? Mn2 O3 C32 O2 0.0(7) . . . . ? Mn1 O2 C32 O3 -3.6(6) . . . . ? Mn1 O4 C33 O5 -11.5(8) . . . . ? Mn2 O5 C33 O4 9.4(7) . . . . ? #============================================================================== data_3_2MeCN _database_code_depnum_ccdc_archive 'CCDC 772401' #TrackingRef '- submit_all.cif' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C49 H47 Mn2 N6 O13 S2 +, Cl O4 -, 2(C2 H3 N) ; _chemical_formula_sum 'C53 H53 Cl Mn2 N8 O17 S2' _chemical_formula_weight 1283.48 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' S S 0.1246 0.1234 '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 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 16.1552(6) _cell_length_b 18.7603(7) _cell_length_c 18.8822(7) _cell_angle_alpha 90.00 _cell_angle_beta 104.151(2) _cell_angle_gamma 90.00 _cell_volume 5549.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 3820 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 22.02 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.974 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; SAME restraint applied to the geometry of one MeCN molecule, linking its geometry to the other MeCN molecule (3 restraints in total). ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 41786 _diffrn_reflns_av_R_equivalents 0.0891 _diffrn_reflns_av_sigmaI/netI 0.1055 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.57 _diffrn_reflns_theta_max 26.37 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 11323 _reflns_number_gt 6562 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+4.9660P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11323 _refine_ls_number_parameters 718 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1221 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1500 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.078 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.090 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.37047(4) 0.14307(3) 0.71875(3) 0.01997(17) Uani 1 1 d . . . Mn2 Mn 0.39908(4) 0.20625(3) 0.55619(3) 0.01944(16) Uani 1 1 d . . . S1 S 0.49629(7) 0.28263(6) 0.80379(6) 0.0222(3) Uani 1 1 d . . . S2 S 0.23254(7) 0.32102(6) 0.55829(6) 0.0226(3) Uani 1 1 d . . . O1 O 0.37439(17) 0.23877(15) 0.65922(14) 0.0200(6) Uani 1 1 d . . . O2 O 0.27989(18) 0.08407(16) 0.64721(15) 0.0254(7) Uani 1 1 d . . . O3 O 0.30802(19) 0.12404(16) 0.54373(16) 0.0281(7) Uani 1 1 d . . . O4 O 0.48604(18) 0.10928(17) 0.69218(17) 0.0292(7) Uani 1 1 d . . . O5 O 0.51613(18) 0.15407(17) 0.59245(16) 0.0294(7) Uani 1 1 d . . . O6 O 0.01580(19) -0.09585(17) 0.41137(16) 0.0315(8) Uani 1 1 d . . . O7 O 0.0884(2) -0.00320(17) 0.34510(16) 0.0326(8) Uani 1 1 d . . . O8 O 0.88569(18) 0.10228(18) 0.79957(17) 0.0331(8) Uani 1 1 d . . . O9 O 0.77585(19) 0.02933(17) 0.84730(16) 0.0307(8) Uani 1 1 d . . . O11 O 0.53057(19) 0.32358(17) 0.86841(15) 0.0307(8) Uani 1 1 d . . . O12 O 0.55443(17) 0.25593(17) 0.76389(16) 0.0282(7) Uani 1 1 d . . . O21 O 0.17968(19) 0.38002(17) 0.52643(16) 0.0326(8) Uani 1 1 d . . . O22 O 0.19195(18) 0.25736(17) 0.57292(15) 0.0285(7) Uani 1 1 d . . . N1 N 0.4452(2) 0.21038(19) 0.82693(18) 0.0224(8) Uani 1 1 d . . . N2 N 0.2686(2) 0.19873(19) 0.76469(18) 0.0228(8) Uani 1 1 d . . . N3 N 0.4111(2) 0.06558(19) 0.80744(18) 0.0236(8) Uani 1 1 d . . . N4 N 0.2951(2) 0.29785(19) 0.50204(18) 0.0213(8) Uani 1 1 d . . . N5 N 0.4718(2) 0.31200(19) 0.56273(18) 0.0219(8) Uani 1 1 d . . . N6 N 0.3724(2) 0.19763(19) 0.43338(18) 0.0225(8) Uani 1 1 d . . . C1 C 0.3655(2) 0.3043(2) 0.6801(2) 0.0192(9) Uani 1 1 d . . . C2 C 0.4150(3) 0.3330(2) 0.7461(2) 0.0202(9) Uani 1 1 d . . . C3 C 0.4097(3) 0.4048(2) 0.7644(2) 0.0230(10) Uani 1 1 d . . . H3A H 0.4449 0.4221 0.8090 0.028 Uiso 1 1 calc R . . C4 C 0.3548(3) 0.4510(2) 0.7195(2) 0.0255(10) Uani 1 1 d . . . C5 C 0.3015(3) 0.4231(2) 0.6553(2) 0.0234(10) Uani 1 1 d . . . H5A H 0.2615 0.4534 0.6240 0.028 Uiso 1 1 calc R . . C6 C 0.3065(3) 0.3521(2) 0.6372(2) 0.0203(9) Uani 1 1 d . . . C7 C 0.3527(3) 0.5302(2) 0.7371(3) 0.0319(11) Uani 1 1 d . . . H7A H 0.3939 0.5401 0.7834 0.048 Uiso 1 1 calc R . . H7B H 0.2953 0.5433 0.7410 0.048 Uiso 1 1 calc R . . H7C H 0.3675 0.5580 0.6980 0.048 Uiso 1 1 calc R . . C8 C 0.3817(3) 0.2294(3) 0.8692(2) 0.0273(11) Uani 1 1 d . . . H8A H 0.4017 0.2725 0.8987 0.033 Uiso 1 1 calc R . . H8B H 0.3784 0.1900 0.9033 0.033 Uiso 1 1 calc R . . C9 C 0.2944(3) 0.2432(2) 0.8218(2) 0.0244(10) Uani 1 1 d . . . C10 C 0.2426(3) 0.2964(3) 0.8371(3) 0.0326(11) Uani 1 1 d . . . H10A H 0.2631 0.3281 0.8767 0.039 Uiso 1 1 calc R . . C11 C 0.1605(3) 0.3031(3) 0.7941(3) 0.0371(12) Uani 1 1 d . . . H11A H 0.1238 0.3395 0.8035 0.045 Uiso 1 1 calc R . . C12 C 0.1327(3) 0.2558(3) 0.7368(3) 0.0342(12) Uani 1 1 d . . . H12A H 0.0762 0.2585 0.7069 0.041 Uiso 1 1 calc R . . C13 C 0.1882(3) 0.2052(3) 0.7244(2) 0.0275(11) Uani 1 1 d . . . H13A H 0.1689 0.1728 0.6852 0.033 Uiso 1 1 calc R . . C14 C 0.5104(3) 0.1580(2) 0.8670(2) 0.0259(10) Uani 1 1 d . . . H14A H 0.5299 0.1730 0.9187 0.031 Uiso 1 1 calc R . . H14B H 0.5604 0.1587 0.8454 0.031 Uiso 1 1 calc R . . C15 C 0.4757(3) 0.0828(2) 0.8640(2) 0.0234(10) Uani 1 1 d . . . C16 C 0.5152(3) 0.0334(3) 0.9146(2) 0.0291(11) Uani 1 1 d . . . H16A H 0.5595 0.0475 0.9552 0.035 Uiso 1 1 calc R . . C17 C 0.4900(3) -0.0370(3) 0.9059(2) 0.0336(12) Uani 1 1 d . . . H17A H 0.5178 -0.0722 0.9396 0.040 Uiso 1 1 calc R . . C18 C 0.4241(3) -0.0555(3) 0.8480(3) 0.0339(12) Uani 1 1 d . . . H18A H 0.4052 -0.1035 0.8409 0.041 Uiso 1 1 calc R . . C19 C 0.3858(3) -0.0027(3) 0.8001(2) 0.0278(11) Uani 1 1 d . . . H19A H 0.3396 -0.0153 0.7603 0.033 Uiso 1 1 calc R . . C20 C 0.3430(3) 0.3595(2) 0.4825(2) 0.0257(10) Uani 1 1 d . . . H20A H 0.3081 0.4032 0.4806 0.031 Uiso 1 1 calc R . . H20B H 0.3523 0.3517 0.4331 0.031 Uiso 1 1 calc R . . C21 C 0.4284(3) 0.3708(2) 0.5359(2) 0.0231(10) Uani 1 1 d . . . C22 C 0.4598(3) 0.4388(2) 0.5538(2) 0.0290(11) Uani 1 1 d . . . H22A H 0.4263 0.4794 0.5355 0.035 Uiso 1 1 calc R . . C23 C 0.5404(3) 0.4467(3) 0.5986(3) 0.0354(12) Uani 1 1 d . . . H23A H 0.5640 0.4928 0.6109 0.043 Uiso 1 1 calc R . . C24 C 0.5862(3) 0.3859(3) 0.6253(2) 0.0325(12) Uani 1 1 d . . . H24A H 0.6421 0.3896 0.6560 0.039 Uiso 1 1 calc R . . C25 C 0.5500(3) 0.3208(3) 0.6071(2) 0.0258(10) Uani 1 1 d . . . H25A H 0.5816 0.2796 0.6266 0.031 Uiso 1 1 calc R . . C26 C 0.2423(3) 0.2624(2) 0.4353(2) 0.0239(10) Uani 1 1 d . . . H26A H 0.2078 0.2986 0.4030 0.029 Uiso 1 1 calc R . . H26B H 0.2027 0.2281 0.4496 0.029 Uiso 1 1 calc R . . C27 C 0.2977(3) 0.2238(2) 0.3946(2) 0.0232(10) Uani 1 1 d . . . C28 C 0.2714(3) 0.2157(3) 0.3191(2) 0.0308(11) Uani 1 1 d . . . H28A H 0.2190 0.2356 0.2926 0.037 Uiso 1 1 calc R . . C29 C 0.3231(3) 0.1780(3) 0.2833(2) 0.0353(12) Uani 1 1 d . . . H29A H 0.3065 0.1718 0.2319 0.042 Uiso 1 1 calc R . . C30 C 0.3985(3) 0.1500(3) 0.3236(3) 0.0366(12) Uani 1 1 d . . . H30A H 0.4345 0.1231 0.3007 0.044 Uiso 1 1 calc R . . C31 C 0.4209(3) 0.1616(3) 0.3976(2) 0.0303(11) Uani 1 1 d . . . H31A H 0.4738 0.1431 0.4249 0.036 Uiso 1 1 calc R . . C32 C 0.2675(3) 0.0848(2) 0.5786(2) 0.0236(10) Uani 1 1 d . . . C33 C 0.2010(3) 0.0365(2) 0.5359(2) 0.0232(10) Uani 1 1 d . . . C34 C 0.1612(3) -0.0134(2) 0.5703(2) 0.0268(11) Uani 1 1 d . . . H34A H 0.1766 -0.0168 0.6220 0.032 Uiso 1 1 calc R . . C35 C 0.0998(3) -0.0582(2) 0.5305(2) 0.0274(11) Uani 1 1 d . . . H35A H 0.0736 -0.0924 0.5551 0.033 Uiso 1 1 calc R . . C36 C 0.0757(3) -0.0540(2) 0.4554(2) 0.0246(10) Uani 1 1 d . . . C37 C 0.1153(3) -0.0042(2) 0.4194(2) 0.0262(10) Uani 1 1 d . . . C38 C 0.1772(3) 0.0406(2) 0.4596(2) 0.0261(10) Uani 1 1 d . . . H38A H 0.2039 0.0746 0.4351 0.031 Uiso 1 1 calc R . . C39 C -0.0227(3) -0.1493(3) 0.4472(3) 0.0372(12) Uani 1 1 d . . . H39A H -0.0645 -0.1763 0.4107 0.056 Uiso 1 1 calc R . . H39B H -0.0514 -0.1264 0.4813 0.056 Uiso 1 1 calc R . . H39C H 0.0215 -0.1817 0.4741 0.056 Uiso 1 1 calc R . . C40 C 0.1343(3) 0.0415(3) 0.3071(2) 0.0361(12) Uani 1 1 d . . . H40A H 0.1094 0.0376 0.2544 0.054 Uiso 1 1 calc R . . H40B H 0.1942 0.0265 0.3181 0.054 Uiso 1 1 calc R . . H40C H 0.1309 0.0910 0.3225 0.054 Uiso 1 1 calc R . . C41 C 0.5372(3) 0.1273(2) 0.6558(2) 0.0241(10) Uani 1 1 d . . . C42 C 0.6312(3) 0.1172(2) 0.6896(2) 0.0238(10) Uani 1 1 d . . . C43 C 0.6911(3) 0.1503(2) 0.6609(3) 0.0281(11) Uani 1 1 d . . . H43A H 0.6733 0.1762 0.6165 0.034 Uiso 1 1 calc R . . C44 C 0.7777(3) 0.1466(3) 0.6954(3) 0.0307(11) Uani 1 1 d . . . H44A H 0.8186 0.1702 0.6752 0.037 Uiso 1 1 calc R . . C45 C 0.8035(3) 0.1081(2) 0.7596(2) 0.0251(10) Uani 1 1 d . . . C46 C 0.7427(3) 0.0706(2) 0.7868(2) 0.0243(10) Uani 1 1 d . . . C47 C 0.6569(3) 0.0767(2) 0.7528(2) 0.0247(10) Uani 1 1 d . . . H47A H 0.6156 0.0533 0.7726 0.030 Uiso 1 1 calc R . . C48 C 0.9494(3) 0.1402(3) 0.7737(3) 0.0406(13) Uani 1 1 d . . . H48A H 1.0056 0.1319 0.8068 0.061 Uiso 1 1 calc R . . H48B H 0.9365 0.1914 0.7719 0.061 Uiso 1 1 calc R . . H48C H 0.9498 0.1234 0.7246 0.061 Uiso 1 1 calc R . . C49 C 0.7175(3) -0.0103(3) 0.8773(3) 0.0387(13) Uani 1 1 d . . . H49A H 0.7491 -0.0372 0.9198 0.058 Uiso 1 1 calc R . . H49B H 0.6856 -0.0434 0.8404 0.058 Uiso 1 1 calc R . . H49C H 0.6777 0.0225 0.8923 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.34942(9) 0.20756(8) 0.07443(7) 0.0470(4) Uani 1 1 d . . . O1A O 0.4188(3) 0.2144(3) 0.1362(3) 0.0922(17) Uani 1 1 d . . . O1B O 0.3653(4) 0.1551(3) 0.0251(3) 0.100(2) Uani 1 1 d . . . O1C O 0.2750(3) 0.1867(2) 0.0988(2) 0.0606(12) Uani 1 1 d . . . O1D O 0.3318(3) 0.2738(2) 0.0360(3) 0.0691(13) Uani 1 1 d . . . N2S N 0.1369(5) 0.1012(4) 0.9418(4) 0.109(2) Uiso 1 1 d D . . C3S C 0.1250(5) 0.1613(4) 0.9480(4) 0.080(2) Uiso 1 1 d D . . C4S C 0.1226(5) 0.2358(4) 0.9591(4) 0.080(2) Uiso 1 1 d D . . H4SA H 0.0631 0.2520 0.9471 0.119 Uiso 1 1 d R . . H4SB H 0.1537 0.2601 0.9277 0.119 Uiso 1 1 d R . . H4SC H 0.1493 0.2468 1.0104 0.119 Uiso 1 1 d R . . N1S N 0.5933(5) 0.0629(4) 0.3854(4) 0.120(3) Uiso 1 1 d D . . C1S C 0.6095(5) 0.0522(5) 0.4493(5) 0.096(3) Uiso 1 1 d D . . C2S C 0.6134(6) 0.0204(5) 0.5192(5) 0.113(3) Uiso 1 1 d D . . H2SA H 0.6495 0.0497 0.5577 0.170 Uiso 1 1 d R . . H2SB H 0.6378 -0.0275 0.5206 0.170 Uiso 1 1 d R . . H2SC H 0.5558 0.0175 0.5271 0.170 Uiso 1 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 Mn1 0.0200(3) 0.0218(4) 0.0157(3) -0.0003(3) -0.0004(3) -0.0016(3) Mn2 0.0192(3) 0.0205(4) 0.0167(3) 0.0006(3) 0.0007(3) 0.0002(3) S1 0.0208(5) 0.0233(6) 0.0191(5) -0.0002(5) -0.0016(4) -0.0035(5) S2 0.0191(5) 0.0278(6) 0.0192(6) -0.0018(5) 0.0013(4) 0.0030(5) O1 0.0247(15) 0.0164(16) 0.0175(15) -0.0021(13) 0.0025(12) 0.0004(12) O2 0.0275(17) 0.0296(19) 0.0155(16) -0.0044(13) -0.0015(13) -0.0074(14) O3 0.0309(17) 0.0284(18) 0.0238(17) -0.0028(14) 0.0045(14) -0.0079(14) O4 0.0207(16) 0.0301(19) 0.0367(19) 0.0041(15) 0.0067(14) 0.0031(14) O5 0.0257(16) 0.0317(19) 0.0282(18) 0.0055(15) 0.0017(13) 0.0059(14) O6 0.0304(17) 0.033(2) 0.0263(17) -0.0024(15) -0.0032(14) -0.0125(15) O7 0.0427(19) 0.0301(19) 0.0196(17) 0.0014(14) -0.0027(14) -0.0064(16) O8 0.0195(16) 0.039(2) 0.0359(19) -0.0009(16) -0.0029(14) 0.0017(14) O9 0.0269(17) 0.039(2) 0.0237(17) 0.0045(15) 0.0005(14) 0.0057(15) O11 0.0360(18) 0.0291(18) 0.0207(16) -0.0029(14) -0.0052(13) -0.0063(15) O12 0.0207(16) 0.0311(19) 0.0328(18) 0.0022(15) 0.0064(13) 0.0016(14) O21 0.0293(17) 0.036(2) 0.0271(17) 0.0013(15) -0.0036(14) 0.0145(15) O22 0.0244(16) 0.038(2) 0.0229(16) -0.0014(15) 0.0062(13) -0.0071(15) N1 0.0225(18) 0.023(2) 0.0209(19) 0.0006(17) 0.0039(15) -0.0015(16) N2 0.0233(19) 0.023(2) 0.0205(19) 0.0014(17) 0.0023(15) -0.0009(16) N3 0.0244(19) 0.025(2) 0.0202(19) 0.0029(17) 0.0028(15) -0.0027(17) N4 0.0204(18) 0.024(2) 0.0177(18) 0.0009(16) 0.0018(14) 0.0012(16) N5 0.0215(18) 0.025(2) 0.0186(19) 0.0009(16) 0.0036(15) -0.0024(16) N6 0.0217(19) 0.027(2) 0.0176(18) 0.0000(17) 0.0028(15) -0.0022(16) C1 0.018(2) 0.022(3) 0.019(2) 0.0021(18) 0.0052(17) -0.0051(18) C2 0.020(2) 0.021(2) 0.020(2) -0.0015(19) 0.0061(18) -0.0015(18) C3 0.021(2) 0.025(3) 0.022(2) -0.003(2) 0.0030(18) -0.0030(19) C4 0.028(2) 0.020(2) 0.030(3) -0.001(2) 0.010(2) -0.0042(19) C5 0.022(2) 0.026(3) 0.022(2) 0.003(2) 0.0060(18) 0.0057(19) C6 0.021(2) 0.023(3) 0.017(2) -0.0009(19) 0.0058(17) 0.0018(19) C7 0.040(3) 0.023(3) 0.032(3) -0.003(2) 0.008(2) -0.001(2) C8 0.026(2) 0.037(3) 0.018(2) -0.006(2) 0.0028(19) -0.008(2) C9 0.024(2) 0.029(3) 0.022(2) -0.001(2) 0.0092(19) -0.004(2) C10 0.032(3) 0.037(3) 0.031(3) -0.001(2) 0.011(2) -0.002(2) C11 0.038(3) 0.037(3) 0.040(3) 0.007(3) 0.018(2) 0.011(2) C12 0.023(2) 0.047(3) 0.031(3) 0.010(3) 0.003(2) 0.004(2) C13 0.022(2) 0.036(3) 0.023(2) 0.000(2) 0.0031(19) 0.000(2) C14 0.023(2) 0.030(3) 0.021(2) 0.003(2) -0.0029(18) -0.003(2) C15 0.023(2) 0.027(3) 0.020(2) 0.000(2) 0.0060(19) -0.0020(19) C16 0.026(2) 0.035(3) 0.024(2) 0.006(2) 0.0012(19) 0.005(2) C17 0.040(3) 0.035(3) 0.024(3) 0.010(2) 0.004(2) 0.009(2) C18 0.040(3) 0.024(3) 0.038(3) 0.004(2) 0.009(2) -0.002(2) C19 0.025(2) 0.031(3) 0.026(3) 0.000(2) 0.004(2) -0.004(2) C20 0.027(2) 0.024(3) 0.023(2) 0.005(2) 0.0016(19) 0.002(2) C21 0.028(2) 0.022(3) 0.019(2) 0.0010(19) 0.0057(19) -0.0041(19) C22 0.036(3) 0.022(3) 0.029(3) 0.002(2) 0.007(2) -0.003(2) C23 0.043(3) 0.032(3) 0.032(3) -0.005(2) 0.011(2) -0.013(2) C24 0.026(2) 0.041(3) 0.029(3) -0.005(2) 0.003(2) -0.011(2) C25 0.021(2) 0.033(3) 0.023(2) 0.001(2) 0.0060(19) -0.002(2) C26 0.018(2) 0.033(3) 0.017(2) 0.001(2) -0.0035(17) 0.0003(19) C27 0.024(2) 0.023(3) 0.022(2) 0.0017(19) 0.0051(19) -0.0059(19) C28 0.028(2) 0.038(3) 0.023(2) 0.001(2) 0.000(2) 0.001(2) C29 0.043(3) 0.045(3) 0.018(2) -0.006(2) 0.007(2) -0.006(3) C30 0.041(3) 0.042(3) 0.032(3) -0.006(2) 0.018(2) 0.005(2) C31 0.029(2) 0.035(3) 0.027(3) 0.003(2) 0.008(2) 0.005(2) C32 0.023(2) 0.021(3) 0.027(3) -0.002(2) 0.0048(19) 0.0037(19) C33 0.024(2) 0.027(3) 0.016(2) -0.0040(19) 0.0003(18) -0.0021(19) C34 0.026(2) 0.033(3) 0.020(2) -0.003(2) 0.0023(19) -0.006(2) C35 0.034(3) 0.025(3) 0.022(2) -0.001(2) 0.006(2) -0.008(2) C36 0.025(2) 0.023(3) 0.021(2) -0.004(2) -0.0028(19) -0.0022(19) C37 0.028(2) 0.032(3) 0.016(2) 0.000(2) -0.0006(18) 0.003(2) C38 0.027(2) 0.028(3) 0.022(2) -0.002(2) 0.0033(19) -0.001(2) C39 0.028(3) 0.043(3) 0.035(3) -0.004(3) -0.002(2) -0.015(2) C40 0.052(3) 0.036(3) 0.020(2) 0.000(2) 0.008(2) -0.002(3) C41 0.024(2) 0.016(2) 0.030(3) -0.001(2) 0.003(2) 0.0043(19) C42 0.020(2) 0.024(2) 0.025(2) -0.002(2) 0.0030(18) 0.0027(19) C43 0.027(2) 0.027(3) 0.030(3) 0.003(2) 0.004(2) 0.001(2) C44 0.025(2) 0.032(3) 0.035(3) 0.003(2) 0.006(2) -0.002(2) C45 0.017(2) 0.024(3) 0.030(3) -0.008(2) -0.0032(19) 0.0033(19) C46 0.028(2) 0.020(2) 0.023(2) -0.002(2) 0.0018(19) 0.005(2) C47 0.019(2) 0.029(3) 0.027(2) -0.003(2) 0.0063(19) 0.0008(19) C48 0.019(2) 0.046(3) 0.053(3) -0.008(3) 0.003(2) -0.003(2) C49 0.039(3) 0.039(3) 0.035(3) 0.010(2) 0.003(2) -0.001(2) Cl1 0.0544(8) 0.0495(9) 0.0381(8) 0.0063(7) 0.0129(6) 0.0069(7) O1A 0.049(3) 0.150(5) 0.069(3) 0.019(3) -0.002(2) -0.012(3) O1B 0.149(5) 0.100(4) 0.062(3) 0.012(3) 0.045(3) 0.075(4) O1C 0.062(3) 0.074(3) 0.047(2) 0.006(2) 0.015(2) -0.022(2) O1D 0.068(3) 0.050(3) 0.090(3) 0.028(2) 0.021(3) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 Mn2 3.4255(9) . ? Mn1 O2 2.055(3) . ? Mn1 O1 2.127(3) . ? Mn1 O4 2.144(3) . ? Mn1 N3 2.193(3) . ? Mn1 N2 2.292(4) . ? Mn1 N1 2.453(3) . ? Mn2 O5 2.090(3) . ? Mn2 O3 2.104(3) . ? Mn2 O1 2.167(3) . ? Mn2 N6 2.259(3) . ? Mn2 N5 2.294(4) . ? Mn2 N4 2.446(3) . ? S1 O12 1.431(3) . ? S1 O11 1.434(3) . ? S1 N1 1.698(4) . ? S1 C2 1.761(4) . ? S2 O22 1.422(3) . ? S2 O21 1.437(3) . ? S2 N4 1.692(4) . ? S2 C6 1.766(4) . ? O1 C1 1.309(5) . ? O2 C32 1.262(5) . ? O3 C32 1.270(5) . ? O4 C41 1.244(5) . ? O5 C41 1.265(5) . ? O6 C36 1.361(5) . ? O6 C39 1.435(5) . ? O7 C37 1.364(5) . ? O7 C40 1.424(5) . ? O8 C45 1.362(5) . ? O8 C48 1.433(6) . ? O9 C46 1.374(5) . ? O9 C49 1.422(6) . ? N1 C8 1.489(5) . ? N1 C14 1.501(5) . ? N2 C13 1.339(5) . ? N2 C9 1.347(5) . ? N3 C15 1.338(5) . ? N3 C19 1.342(6) . ? N4 C20 1.488(5) . ? N4 C26 1.494(5) . ? N5 C21 1.339(5) . ? N5 C25 1.344(5) . ? N6 C31 1.336(6) . ? N6 C27 1.342(5) . ? C1 C6 1.411(6) . ? C1 C2 1.414(6) . ? C2 C3 1.399(6) . ? C3 C4 1.374(6) . ? C3 H3A 0.950 . ? C4 C5 1.406(6) . ? C4 C7 1.523(6) . ? C5 C6 1.383(6) . ? C5 H5A 0.950 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.497(6) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 C10 1.377(6) . ? C10 C11 1.381(6) . ? C10 H10A 0.950 . ? C11 C12 1.385(7) . ? C11 H11A 0.950 . ? C12 C13 1.366(6) . ? C12 H12A 0.950 . ? C13 H13A 0.950 . ? C14 C15 1.515(6) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.370(6) . ? C16 C17 1.381(7) . ? C16 H16A 0.950 . ? C17 C18 1.371(6) . ? C17 H17A 0.950 . ? C18 C19 1.381(6) . ? C18 H18A 0.950 . ? C19 H19A 0.950 . ? C20 C21 1.512(6) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C21 C22 1.384(6) . ? C22 C23 1.375(6) . ? C22 H22A 0.950 . ? C23 C24 1.387(7) . ? C23 H23A 0.950 . ? C24 C25 1.360(6) . ? C24 H24A 0.950 . ? C25 H25A 0.950 . ? C26 C27 1.500(6) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.391(6) . ? C28 C29 1.389(7) . ? C28 H28A 0.950 . ? C29 C30 1.374(7) . ? C29 H29A 0.950 . ? C30 C31 1.372(6) . ? C30 H30A 0.950 . ? C31 H31A 0.950 . ? C32 C33 1.485(6) . ? C33 C34 1.385(6) . ? C33 C38 1.400(6) . ? C34 C35 1.374(6) . ? C34 H34A 0.950 . ? C35 C36 1.378(6) . ? C35 H35A 0.950 . ? C36 C37 1.400(6) . ? C37 C38 1.381(6) . ? C38 H38A 0.950 . ? C39 H39A 0.980 . ? C39 H39B 0.980 . ? C39 H39C 0.980 . ? C40 H40A 0.980 . ? C40 H40B 0.980 . ? C40 H40C 0.980 . ? C41 C42 1.509(6) . ? C42 C43 1.369(6) . ? C42 C47 1.388(6) . ? C43 C44 1.394(6) . ? C43 H43A 0.950 . ? C44 C45 1.384(6) . ? C44 H44A 0.950 . ? C45 C46 1.405(6) . ? C46 C47 1.382(6) . ? C47 H47A 0.950 . ? C48 H48A 0.980 . ? C48 H48B 0.980 . ? C48 H48C 0.980 . ? C49 H49A 0.980 . ? C49 H49B 0.980 . ? C49 H49C 0.980 . ? Cl1 O1A 1.412(4) . ? Cl1 O1B 1.421(5) . ? Cl1 O1D 1.432(4) . ? Cl1 O1C 1.443(4) . ? N2S C3S 1.155(8) . ? C3S C4S 1.415(8) . ? C4S H4SA 0.980 . ? C4S H4SB 0.980 . ? C4S H4SC 0.980 . ? N1S C1S 1.187(8) . ? C1S C2S 1.436(8) . ? C2S H2SA 0.980 . ? C2S H2SB 0.980 . ? C2S H2SC 0.980 . ? 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 O2 Mn1 O1 102.45(11) . . ? O2 Mn1 O4 101.98(12) . . ? O1 Mn1 O4 89.18(11) . . ? O2 Mn1 N3 100.20(13) . . ? O1 Mn1 N3 157.03(12) . . ? O4 Mn1 N3 82.38(13) . . ? O2 Mn1 N2 91.85(12) . . ? O1 Mn1 N2 86.13(12) . . ? O4 Mn1 N2 166.06(12) . . ? N3 Mn1 N2 96.99(13) . . ? O2 Mn1 N1 161.96(12) . . ? O1 Mn1 N1 86.18(11) . . ? O4 Mn1 N1 93.86(12) . . ? N3 Mn1 N1 73.20(13) . . ? N2 Mn1 N1 72.74(12) . . ? O5 Mn2 O3 104.19(12) . . ? O5 Mn2 O1 100.85(11) . . ? O3 Mn2 O1 91.70(11) . . ? O5 Mn2 N6 103.47(12) . . ? O3 Mn2 N6 83.11(12) . . ? O1 Mn2 N6 155.67(12) . . ? O5 Mn2 N5 88.67(12) . . ? O3 Mn2 N5 167.11(12) . . ? O1 Mn2 N5 84.98(11) . . ? N6 Mn2 N5 94.81(12) . . ? O5 Mn2 N4 160.04(12) . . ? O3 Mn2 N4 94.49(12) . . ? O1 Mn2 N4 85.36(11) . . ? N6 Mn2 N4 71.45(12) . . ? N5 Mn2 N4 72.86(12) . . ? O12 S1 O11 117.98(19) . . ? O12 S1 N1 106.18(18) . . ? O11 S1 N1 108.64(18) . . ? O12 S1 C2 110.38(19) . . ? O11 S1 C2 108.25(19) . . ? N1 S1 C2 104.58(18) . . ? O22 S2 O21 118.25(19) . . ? O22 S2 N4 106.31(18) . . ? O21 S2 N4 108.67(18) . . ? O22 S2 C6 111.23(19) . . ? O21 S2 C6 108.0(2) . . ? N4 S2 C6 103.28(18) . . ? C1 O1 Mn1 127.9(2) . . ? C1 O1 Mn2 126.3(2) . . ? Mn1 O1 Mn2 105.82(12) . . ? C32 O2 Mn1 125.2(3) . . ? C32 O3 Mn2 143.2(3) . . ? C41 O4 Mn1 141.5(3) . . ? C41 O5 Mn2 120.6(3) . . ? C36 O6 C39 116.2(3) . . ? C37 O7 C40 116.9(4) . . ? C45 O8 C48 117.1(4) . . ? C46 O9 C49 117.6(3) . . ? C8 N1 C14 112.1(3) . . ? C8 N1 S1 112.8(3) . . ? C14 N1 S1 109.1(3) . . ? C8 N1 Mn1 107.8(2) . . ? C14 N1 Mn1 103.0(2) . . ? S1 N1 Mn1 111.58(17) . . ? C13 N2 C9 117.8(4) . . ? C13 N2 Mn1 120.8(3) . . ? C9 N2 Mn1 118.4(3) . . ? C15 N3 C19 118.2(4) . . ? C15 N3 Mn1 118.6(3) . . ? C19 N3 Mn1 121.8(3) . . ? C20 N4 C26 111.1(3) . . ? C20 N4 S2 112.5(3) . . ? C26 N4 S2 109.8(3) . . ? C20 N4 Mn2 107.7(2) . . ? C26 N4 Mn2 103.4(2) . . ? S2 N4 Mn2 111.89(16) . . ? C21 N5 C25 117.4(4) . . ? C21 N5 Mn2 118.6(3) . . ? C25 N5 Mn2 122.1(3) . . ? C31 N6 C27 118.0(4) . . ? C31 N6 Mn2 124.6(3) . . ? C27 N6 Mn2 117.0(3) . . ? O1 C1 C6 122.2(4) . . ? O1 C1 C2 122.9(4) . . ? C6 C1 C2 114.9(4) . . ? C3 C2 C1 121.9(4) . . ? C3 C2 S1 116.5(3) . . ? C1 C2 S1 121.1(3) . . ? C4 C3 C2 121.7(4) . . ? C4 C3 H3A 119.1 . . ? C2 C3 H3A 119.1 . . ? C3 C4 C5 117.6(4) . . ? C3 C4 C7 121.8(4) . . ? C5 C4 C7 120.6(4) . . ? C6 C5 C4 120.8(4) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C5 C6 C1 122.9(4) . . ? C5 C6 S2 117.3(3) . . ? C1 C6 S2 119.8(3) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 113.2(3) . . ? N1 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N1 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.8 . . ? N2 C9 C10 122.1(4) . . ? N2 C9 C8 115.7(4) . . ? C10 C9 C8 122.2(4) . . ? C9 C10 C11 119.2(5) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? C10 C11 C12 118.9(5) . . ? C10 C11 H11A 120.6 . . ? C12 C11 H11A 120.6 . . ? C13 C12 C11 118.5(4) . . ? C13 C12 H12A 120.7 . . ? C11 C12 H12A 120.7 . . ? N2 C13 C12 123.5(4) . . ? N2 C13 H13A 118.3 . . ? C12 C13 H13A 118.3 . . ? N1 C14 C15 112.6(3) . . ? N1 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N1 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? N3 C15 C16 122.1(4) . . ? N3 C15 C14 117.6(4) . . ? C16 C15 C14 120.0(4) . . ? C15 C16 C17 119.5(4) . . ? C15 C16 H16A 120.3 . . ? C17 C16 H16A 120.3 . . ? C18 C17 C16 118.9(4) . . ? C18 C17 H17A 120.5 . . ? C16 C17 H17A 120.5 . . ? C17 C18 C19 118.6(5) . . ? C17 C18 H18A 120.7 . . ? C19 C18 H18A 120.7 . . ? N3 C19 C18 122.7(4) . . ? N3 C19 H19A 118.7 . . ? C18 C19 H19A 118.7 . . ? N4 C20 C21 112.8(3) . . ? N4 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? N4 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? N5 C21 C22 122.7(4) . . ? N5 C21 C20 116.4(4) . . ? C22 C21 C20 120.9(4) . . ? C23 C22 C21 119.1(4) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C22 C23 C24 118.3(4) . . ? C22 C23 H23A 120.8 . . ? C24 C23 H23A 120.8 . . ? C25 C24 C23 119.2(4) . . ? C25 C24 H24A 120.4 . . ? C23 C24 H24A 120.4 . . ? N5 C25 C24 123.2(4) . . ? N5 C25 H25A 118.4 . . ? C24 C25 H25A 118.4 . . ? N4 C26 C27 111.0(3) . . ? N4 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? N4 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? N6 C27 C28 121.8(4) . . ? N6 C27 C26 117.8(4) . . ? C28 C27 C26 120.4(4) . . ? C29 C28 C27 119.0(4) . . ? C29 C28 H28A 120.5 . . ? C27 C28 H28A 120.5 . . ? C30 C29 C28 118.8(4) . . ? C30 C29 H29A 120.6 . . ? C28 C29 H29A 120.6 . . ? C31 C30 C29 118.7(4) . . ? C31 C30 H30A 120.6 . . ? C29 C30 H30A 120.6 . . ? N6 C31 C30 123.6(4) . . ? N6 C31 H31A 118.2 . . ? C30 C31 H31A 118.2 . . ? O2 C32 O3 124.5(4) . . ? O2 C32 C33 117.6(4) . . ? O3 C32 C33 117.9(4) . . ? C34 C33 C38 118.5(4) . . ? C34 C33 C32 121.1(4) . . ? C38 C33 C32 120.4(4) . . ? C35 C34 C33 120.9(4) . . ? C35 C34 H34A 119.6 . . ? C33 C34 H34A 119.6 . . ? C34 C35 C36 120.8(4) . . ? C34 C35 H35A 119.6 . . ? C36 C35 H35A 119.6 . . ? O6 C36 C35 125.2(4) . . ? O6 C36 C37 115.4(4) . . ? C35 C36 C37 119.4(4) . . ? O7 C37 C38 124.2(4) . . ? O7 C37 C36 116.1(4) . . ? C38 C37 C36 119.6(4) . . ? C37 C38 C33 120.8(4) . . ? C37 C38 H38A 119.6 . . ? C33 C38 H38A 119.6 . . ? O6 C39 H39A 109.5 . . ? O6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O7 C40 H40A 109.5 . . ? O7 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O7 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O4 C41 O5 124.6(4) . . ? O4 C41 C42 117.9(4) . . ? O5 C41 C42 117.5(4) . . ? C43 C42 C47 119.8(4) . . ? C43 C42 C41 120.7(4) . . ? C47 C42 C41 119.4(4) . . ? C42 C43 C44 121.2(4) . . ? C42 C43 H43A 119.4 . . ? C44 C43 H43A 119.4 . . ? C45 C44 C43 119.3(4) . . ? C45 C44 H44A 120.4 . . ? C43 C44 H44A 120.4 . . ? O8 C45 C44 124.8(4) . . ? O8 C45 C46 115.6(4) . . ? C44 C45 C46 119.6(4) . . ? O9 C46 C47 125.2(4) . . ? O9 C46 C45 114.9(4) . . ? C47 C46 C45 119.9(4) . . ? C46 C47 C42 120.1(4) . . ? C46 C47 H47A 120.0 . . ? C42 C47 H47A 120.0 . . ? O8 C48 H48A 109.5 . . ? O8 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O8 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O9 C49 H49A 109.5 . . ? O9 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O9 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O1A Cl1 O1B 111.8(3) . . ? O1A Cl1 O1D 111.0(3) . . ? O1B Cl1 O1D 108.3(3) . . ? O1A Cl1 O1C 108.5(3) . . ? O1B Cl1 O1C 108.6(3) . . ? O1D Cl1 O1C 108.6(3) . . ? N2S C3S C4S 172.2(9) . . ? C3S C4S H4SA 109.5 . . ? C3S C4S H4SB 109.5 . . ? H4SA C4S H4SB 109.5 . . ? C3S C4S H4SC 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? N1S C1S C2S 162.6(10) . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Mn1 O1 C1 126.5(3) . . . . ? O4 Mn1 O1 C1 -131.4(3) . . . . ? N3 Mn1 O1 C1 -63.4(5) . . . . ? N2 Mn1 O1 C1 35.4(3) . . . . ? N1 Mn1 O1 C1 -37.5(3) . . . . ? O2 Mn1 O1 Mn2 -54.71(14) . . . . ? O4 Mn1 O1 Mn2 47.38(13) . . . . ? N3 Mn1 O1 Mn2 115.5(3) . . . . ? N2 Mn1 O1 Mn2 -145.76(13) . . . . ? N1 Mn1 O1 Mn2 141.31(13) . . . . ? O5 Mn2 O1 C1 119.3(3) . . . . ? O3 Mn2 O1 C1 -136.0(3) . . . . ? N6 Mn2 O1 C1 -59.0(5) . . . . ? N5 Mn2 O1 C1 31.6(3) . . . . ? N4 Mn2 O1 C1 -41.6(3) . . . . ? O5 Mn2 O1 Mn1 -59.60(14) . . . . ? O3 Mn2 O1 Mn1 45.19(13) . . . . ? N6 Mn2 O1 Mn1 122.1(3) . . . . ? N5 Mn2 O1 Mn1 -147.28(13) . . . . ? N4 Mn2 O1 Mn1 139.56(13) . . . . ? O1 Mn1 O2 C32 34.3(4) . . . . ? O4 Mn1 O2 C32 -57.6(4) . . . . ? N3 Mn1 O2 C32 -141.8(3) . . . . ? N2 Mn1 O2 C32 120.7(3) . . . . ? N1 Mn1 O2 C32 151.5(4) . . . . ? O5 Mn2 O3 C32 80.3(5) . . . . ? O1 Mn2 O3 C32 -21.4(5) . . . . ? N6 Mn2 O3 C32 -177.5(5) . . . . ? N5 Mn2 O3 C32 -96.1(7) . . . . ? N4 Mn2 O3 C32 -106.8(5) . . . . ? O2 Mn1 O4 C41 97.9(5) . . . . ? O1 Mn1 O4 C41 -4.7(5) . . . . ? N3 Mn1 O4 C41 -163.2(5) . . . . ? N2 Mn1 O4 C41 -74.9(7) . . . . ? N1 Mn1 O4 C41 -90.8(5) . . . . ? O3 Mn2 O5 C41 -69.7(3) . . . . ? O1 Mn2 O5 C41 24.9(3) . . . . ? N6 Mn2 O5 C41 -155.8(3) . . . . ? N5 Mn2 O5 C41 109.5(3) . . . . ? N4 Mn2 O5 C41 131.5(4) . . . . ? O12 S1 N1 C8 -180.0(3) . . . . ? O11 S1 N1 C8 52.2(3) . . . . ? C2 S1 N1 C8 -63.2(3) . . . . ? O12 S1 N1 C14 54.7(3) . . . . ? O11 S1 N1 C14 -73.1(3) . . . . ? C2 S1 N1 C14 171.5(3) . . . . ? O12 S1 N1 Mn1 -58.4(2) . . . . ? O11 S1 N1 Mn1 173.78(17) . . . . ? C2 S1 N1 Mn1 58.4(2) . . . . ? O2 Mn1 N1 C8 -16.4(5) . . . . ? O1 Mn1 N1 C8 103.1(3) . . . . ? O4 Mn1 N1 C8 -168.0(3) . . . . ? N3 Mn1 N1 C8 -87.2(3) . . . . ? N2 Mn1 N1 C8 15.9(3) . . . . ? O2 Mn1 N1 C14 102.2(4) . . . . ? O1 Mn1 N1 C14 -138.3(2) . . . . ? O4 Mn1 N1 C14 -49.3(3) . . . . ? N3 Mn1 N1 C14 31.5(2) . . . . ? N2 Mn1 N1 C14 134.6(3) . . . . ? O2 Mn1 N1 S1 -140.9(3) . . . . ? O1 Mn1 N1 S1 -21.38(17) . . . . ? O4 Mn1 N1 S1 67.54(18) . . . . ? N3 Mn1 N1 S1 148.4(2) . . . . ? N2 Mn1 N1 S1 -108.51(19) . . . . ? O2 Mn1 N2 C13 -25.3(3) . . . . ? O1 Mn1 N2 C13 77.1(3) . . . . ? O4 Mn1 N2 C13 147.7(5) . . . . ? N3 Mn1 N2 C13 -125.8(3) . . . . ? N1 Mn1 N2 C13 164.3(4) . . . . ? O2 Mn1 N2 C9 174.9(3) . . . . ? O1 Mn1 N2 C9 -82.7(3) . . . . ? O4 Mn1 N2 C9 -12.1(7) . . . . ? N3 Mn1 N2 C9 74.4(3) . . . . ? N1 Mn1 N2 C9 4.5(3) . . . . ? O2 Mn1 N3 C15 175.4(3) . . . . ? O1 Mn1 N3 C15 5.2(5) . . . . ? O4 Mn1 N3 C15 74.5(3) . . . . ? N2 Mn1 N3 C15 -91.4(3) . . . . ? N1 Mn1 N3 C15 -21.9(3) . . . . ? O2 Mn1 N3 C19 9.2(4) . . . . ? O1 Mn1 N3 C19 -161.0(3) . . . . ? O4 Mn1 N3 C19 -91.6(3) . . . . ? N2 Mn1 N3 C19 102.4(3) . . . . ? N1 Mn1 N3 C19 172.0(4) . . . . ? O22 S2 N4 C20 -179.3(3) . . . . ? O21 S2 N4 C20 52.4(3) . . . . ? C6 S2 N4 C20 -62.1(3) . . . . ? O22 S2 N4 C26 56.3(3) . . . . ? O21 S2 N4 C26 -71.9(3) . . . . ? C6 S2 N4 C26 173.5(3) . . . . ? O22 S2 N4 Mn2 -57.8(2) . . . . ? O21 S2 N4 Mn2 173.87(17) . . . . ? C6 S2 N4 Mn2 59.3(2) . . . . ? O5 Mn2 N4 C20 -4.0(5) . . . . ? O3 Mn2 N4 C20 -163.4(3) . . . . ? O1 Mn2 N4 C20 105.3(3) . . . . ? N6 Mn2 N4 C20 -82.2(3) . . . . ? N5 Mn2 N4 C20 19.1(2) . . . . ? O5 Mn2 N4 C26 113.8(4) . . . . ? O3 Mn2 N4 C26 -45.7(2) . . . . ? O1 Mn2 N4 C26 -137.0(2) . . . . ? N6 Mn2 N4 C26 35.5(2) . . . . ? N5 Mn2 N4 C26 136.8(3) . . . . ? O5 Mn2 N4 S2 -128.2(3) . . . . ? O3 Mn2 N4 S2 72.43(18) . . . . ? O1 Mn2 N4 S2 -18.91(17) . . . . ? N6 Mn2 N4 S2 153.6(2) . . . . ? N5 Mn2 N4 S2 -105.08(19) . . . . ? O5 Mn2 N5 C21 172.0(3) . . . . ? O3 Mn2 N5 C21 -11.5(7) . . . . ? O1 Mn2 N5 C21 -87.0(3) . . . . ? N6 Mn2 N5 C21 68.6(3) . . . . ? N4 Mn2 N5 C21 -0.3(3) . . . . ? O5 Mn2 N5 C25 -24.5(3) . . . . ? O3 Mn2 N5 C25 152.1(5) . . . . ? O1 Mn2 N5 C25 76.6(3) . . . . ? N6 Mn2 N5 C25 -127.9(3) . . . . ? N4 Mn2 N5 C25 163.2(3) . . . . ? O5 Mn2 N6 C31 4.4(4) . . . . ? O3 Mn2 N6 C31 -98.6(4) . . . . ? O1 Mn2 N6 C31 -177.3(3) . . . . ? N5 Mn2 N6 C31 94.2(4) . . . . ? N4 Mn2 N6 C31 164.3(4) . . . . ? O5 Mn2 N6 C27 176.6(3) . . . . ? O3 Mn2 N6 C27 73.6(3) . . . . ? O1 Mn2 N6 C27 -5.1(5) . . . . ? N5 Mn2 N6 C27 -93.6(3) . . . . ? N4 Mn2 N6 C27 -23.5(3) . . . . ? Mn1 O1 C1 C6 -127.8(3) . . . . ? Mn2 O1 C1 C6 53.6(5) . . . . ? Mn1 O1 C1 C2 53.5(5) . . . . ? Mn2 O1 C1 C2 -125.1(4) . . . . ? O1 C1 C2 C3 174.4(4) . . . . ? C6 C1 C2 C3 -4.4(6) . . . . ? O1 C1 C2 S1 2.6(6) . . . . ? C6 C1 C2 S1 -176.2(3) . . . . ? O12 S1 C2 C3 -118.5(3) . . . . ? O11 S1 C2 C3 12.0(4) . . . . ? N1 S1 C2 C3 127.7(3) . . . . ? O12 S1 C2 C1 53.7(4) . . . . ? O11 S1 C2 C1 -175.8(3) . . . . ? N1 S1 C2 C1 -60.1(4) . . . . ? C1 C2 C3 C4 1.1(6) . . . . ? S1 C2 C3 C4 173.2(3) . . . . ? C2 C3 C4 C5 2.3(6) . . . . ? C2 C3 C4 C7 -176.3(4) . . . . ? C3 C4 C5 C6 -2.1(6) . . . . ? C7 C4 C5 C6 176.5(4) . . . . ? C4 C5 C6 C1 -1.5(6) . . . . ? C4 C5 C6 S2 176.4(3) . . . . ? O1 C1 C6 C5 -174.2(4) . . . . ? C2 C1 C6 C5 4.6(6) . . . . ? O1 C1 C6 S2 8.0(5) . . . . ? C2 C1 C6 S2 -173.2(3) . . . . ? O22 S2 C6 C5 -130.5(3) . . . . ? O21 S2 C6 C5 0.9(4) . . . . ? N4 S2 C6 C5 115.9(3) . . . . ? O22 S2 C6 C1 47.5(4) . . . . ? O21 S2 C6 C1 178.8(3) . . . . ? N4 S2 C6 C1 -66.2(4) . . . . ? C14 N1 C8 C9 -146.3(4) . . . . ? S1 N1 C8 C9 90.1(4) . . . . ? Mn1 N1 C8 C9 -33.6(4) . . . . ? C13 N2 C9 C10 -3.4(6) . . . . ? Mn1 N2 C9 C10 157.0(4) . . . . ? C13 N2 C9 C8 174.5(4) . . . . ? Mn1 N2 C9 C8 -25.1(5) . . . . ? N1 C8 C9 N2 40.6(5) . . . . ? N1 C8 C9 C10 -141.6(4) . . . . ? N2 C9 C10 C11 2.2(7) . . . . ? C8 C9 C10 C11 -175.5(4) . . . . ? C9 C10 C11 C12 0.2(7) . . . . ? C10 C11 C12 C13 -1.2(7) . . . . ? C9 N2 C13 C12 2.3(7) . . . . ? Mn1 N2 C13 C12 -157.6(4) . . . . ? C11 C12 C13 N2 0.0(7) . . . . ? C8 N1 C14 C15 76.6(4) . . . . ? S1 N1 C14 C15 -157.7(3) . . . . ? Mn1 N1 C14 C15 -39.0(4) . . . . ? C19 N3 C15 C16 -1.1(6) . . . . ? Mn1 N3 C15 C16 -167.8(3) . . . . ? C19 N3 C15 C14 173.2(4) . . . . ? Mn1 N3 C15 C14 6.5(5) . . . . ? N1 C14 C15 N3 25.9(5) . . . . ? N1 C14 C15 C16 -159.8(4) . . . . ? N3 C15 C16 C17 2.4(7) . . . . ? C14 C15 C16 C17 -171.7(4) . . . . ? C15 C16 C17 C18 -2.0(7) . . . . ? C16 C17 C18 C19 0.4(7) . . . . ? C15 N3 C19 C18 -0.6(6) . . . . ? Mn1 N3 C19 C18 165.7(3) . . . . ? C17 C18 C19 N3 0.9(7) . . . . ? C26 N4 C20 C21 -147.5(4) . . . . ? S2 N4 C20 C21 88.9(4) . . . . ? Mn2 N4 C20 C21 -34.9(4) . . . . ? C25 N5 C21 C22 -1.9(6) . . . . ? Mn2 N5 C21 C22 162.4(3) . . . . ? C25 N5 C21 C20 176.3(4) . . . . ? Mn2 N5 C21 C20 -19.4(5) . . . . ? N4 C20 C21 N5 37.9(5) . . . . ? N4 C20 C21 C22 -143.9(4) . . . . ? N5 C21 C22 C23 2.7(7) . . . . ? C20 C21 C22 C23 -175.4(4) . . . . ? C21 C22 C23 C24 -1.4(7) . . . . ? C22 C23 C24 C25 -0.5(7) . . . . ? C21 N5 C25 C24 -0.2(6) . . . . ? Mn2 N5 C25 C24 -163.9(3) . . . . ? C23 C24 C25 N5 1.4(7) . . . . ? C20 N4 C26 C27 70.4(4) . . . . ? S2 N4 C26 C27 -164.5(3) . . . . ? Mn2 N4 C26 C27 -45.0(4) . . . . ? C31 N6 C27 C28 -1.5(6) . . . . ? Mn2 N6 C27 C28 -174.2(3) . . . . ? C31 N6 C27 C26 178.3(4) . . . . ? Mn2 N6 C27 C26 5.6(5) . . . . ? N4 C26 C27 N6 29.9(5) . . . . ? N4 C26 C27 C28 -150.2(4) . . . . ? N6 C27 C28 C29 1.6(7) . . . . ? C26 C27 C28 C29 -178.3(4) . . . . ? C27 C28 C29 C30 -0.1(7) . . . . ? C28 C29 C30 C31 -1.4(8) . . . . ? C27 N6 C31 C30 0.0(7) . . . . ? Mn2 N6 C31 C30 172.1(4) . . . . ? C29 C30 C31 N6 1.5(8) . . . . ? Mn1 O2 C32 O3 -2.2(6) . . . . ? Mn1 O2 C32 C33 177.8(3) . . . . ? Mn2 O3 C32 O2 -5.3(8) . . . . ? Mn2 O3 C32 C33 174.7(3) . . . . ? O2 C32 C33 C34 -7.4(6) . . . . ? O3 C32 C33 C34 172.6(4) . . . . ? O2 C32 C33 C38 172.5(4) . . . . ? O3 C32 C33 C38 -7.5(6) . . . . ? C38 C33 C34 C35 0.2(7) . . . . ? C32 C33 C34 C35 -179.9(4) . . . . ? C33 C34 C35 C36 -0.6(7) . . . . ? C39 O6 C36 C35 -1.6(6) . . . . ? C39 O6 C36 C37 177.3(4) . . . . ? C34 C35 C36 O6 179.8(4) . . . . ? C34 C35 C36 C37 0.9(7) . . . . ? C40 O7 C37 C38 7.3(6) . . . . ? C40 O7 C37 C36 -173.3(4) . . . . ? O6 C36 C37 O7 0.8(6) . . . . ? C35 C36 C37 O7 179.8(4) . . . . ? O6 C36 C37 C38 -179.8(4) . . . . ? C35 C36 C37 C38 -0.8(7) . . . . ? O7 C37 C38 C33 179.7(4) . . . . ? C36 C37 C38 C33 0.3(7) . . . . ? C34 C33 C38 C37 0.0(7) . . . . ? C32 C33 C38 C37 -179.9(4) . . . . ? Mn1 O4 C41 O5 -40.4(7) . . . . ? Mn1 O4 C41 C42 139.2(4) . . . . ? Mn2 O5 C41 O4 23.3(6) . . . . ? Mn2 O5 C41 C42 -156.3(3) . . . . ? O4 C41 C42 C43 -164.8(4) . . . . ? O5 C41 C42 C43 14.8(6) . . . . ? O4 C41 C42 C47 11.9(6) . . . . ? O5 C41 C42 C47 -168.5(4) . . . . ? C47 C42 C43 C44 -2.6(7) . . . . ? C41 C42 C43 C44 174.0(4) . . . . ? C42 C43 C44 C45 0.7(7) . . . . ? C48 O8 C45 C44 1.4(6) . . . . ? C48 O8 C45 C46 -179.6(4) . . . . ? C43 C44 C45 O8 -177.9(4) . . . . ? C43 C44 C45 C46 3.1(7) . . . . ? C49 O9 C46 C47 0.1(6) . . . . ? C49 O9 C46 C45 -179.7(4) . . . . ? O8 C45 C46 O9 -4.3(6) . . . . ? C44 C45 C46 O9 174.7(4) . . . . ? O8 C45 C46 C47 175.9(4) . . . . ? C44 C45 C46 C47 -5.1(7) . . . . ? O9 C46 C47 C42 -176.6(4) . . . . ? C45 C46 C47 C42 3.2(7) . . . . ? C43 C42 C47 C46 0.6(7) . . . . ? C41 C42 C47 C46 -176.0(4) . . . . ? #============================================================================== data_4_2MeCN _database_code_depnum_ccdc_archive 'CCDC 772402' #TrackingRef '- submit_all.cif' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C33 H31 Co2 N6 O9 S2 +, Cl O4 -, 2(C2 H3 N) ; _chemical_formula_sum 'C37 H37 Cl Co2 N8 O13 S2' _chemical_formula_weight 1019.18 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' S S 0.1246 0.1234 '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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3915(3) _cell_length_b 13.2868(4) _cell_length_c 18.5255(8) _cell_angle_alpha 110.606(2) _cell_angle_beta 94.929(3) _cell_angle_gamma 97.080(2) _cell_volume 2126.37(13) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5690 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 24.75 _exptl_crystal_description lath _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 1.015 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; All bond distances and 1,3-distances are restrained in all MeCN molecules: C---N = 1.15(1), C---C = 1.45(1), N...C = 2.60(1) \%A (12 restraints in total). Residual electron density remains in the vicinity of N1S-C1S-C2S / N1S'-C1S'-C2S' ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 59834 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.92 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.92 _diffrn_measured_fraction_theta_full 0.980 _reflns_number_total 8133 _reflns_number_gt 6069 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+1.3766P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8133 _refine_ls_number_parameters 562 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.935 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.076 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.50286(4) 0.33399(3) 0.22011(2) 0.01853(11) Uani 1 1 d . . . Co2 Co 0.52712(4) 0.59605(3) 0.36052(2) 0.01864(12) Uani 1 1 d . . . S1 S 0.15261(8) 0.29956(6) 0.23725(5) 0.02275(18) Uani 1 1 d . . . S2 S 0.44917(8) 0.66945(6) 0.21262(4) 0.02073(17) Uani 1 1 d . . . O11 O 0.0117(2) 0.23522(18) 0.20664(14) 0.0336(6) Uani 1 1 d . . . O12 O 0.1973(2) 0.33731(17) 0.31902(12) 0.0278(5) Uani 1 1 d . . . O21 O 0.4112(2) 0.75076(17) 0.18402(12) 0.0287(5) Uani 1 1 d . . . O22 O 0.5654(2) 0.61447(17) 0.18320(11) 0.0242(5) Uani 1 1 d . . . O1 O 0.4140(2) 0.47359(15) 0.26147(11) 0.0178(4) Uani 1 1 d . . . O2 O 0.7061(2) 0.40565(17) 0.21965(12) 0.0272(5) Uani 1 1 d . . . O3 O 0.7226(2) 0.56694(17) 0.31863(12) 0.0265(5) Uani 1 1 d . . . O4 O 0.5451(2) 0.33760(17) 0.33435(12) 0.0279(5) Uani 1 1 d . . . O5 O 0.5493(2) 0.50397(17) 0.42505(12) 0.0275(5) Uani 1 1 d . . . N1 N 0.2803(3) 0.22733(19) 0.19491(14) 0.0204(5) Uani 1 1 d . . . N2 N 0.4321(3) 0.31225(19) 0.10298(14) 0.0222(6) Uani 1 1 d . . . N3 N 0.5471(3) 0.17466(19) 0.19406(14) 0.0226(6) Uani 1 1 d . . . N4 N 0.4952(3) 0.72570(19) 0.31120(14) 0.0199(5) Uani 1 1 d . . . N5 N 0.3252(3) 0.6373(2) 0.39476(14) 0.0230(6) Uani 1 1 d . . . N6 N 0.6606(3) 0.7379(2) 0.44181(14) 0.0227(6) Uani 1 1 d . . . C1 C 0.2963(3) 0.4850(2) 0.22342(16) 0.0176(6) Uani 1 1 d . . . C2 C 0.1675(3) 0.4087(2) 0.20303(17) 0.0201(6) Uani 1 1 d . . . C3 C 0.0449(3) 0.4196(2) 0.16043(17) 0.0229(7) Uani 1 1 d . . . H3A H -0.0388 0.3651 0.1466 0.027 Uiso 1 1 calc R . . C4 C 0.0425(3) 0.5090(3) 0.13765(17) 0.0244(7) Uani 1 1 d . . . C5 C 0.1668(3) 0.5864(3) 0.15834(17) 0.0237(7) Uani 1 1 d . . . H5A H 0.1675 0.6485 0.1442 0.028 Uiso 1 1 calc R . . C6 C 0.2910(3) 0.5747(2) 0.19959(16) 0.0194(6) Uani 1 1 d . . . C7 C -0.0920(3) 0.5220(3) 0.0931(2) 0.0350(8) Uani 1 1 d . . . H7A H -0.1450 0.4497 0.0600 0.052 Uiso 1 1 d R . . H7B H -0.0640 0.5633 0.0605 0.052 Uiso 1 1 d R . . H7C H -0.1540 0.5610 0.1296 0.052 Uiso 1 1 d R . . C8 C 0.2420(3) 0.1762(3) 0.10895(17) 0.0260(7) Uani 1 1 d . . . H8A H 0.1353 0.1639 0.0957 0.031 Uiso 1 1 calc R . . H8B H 0.2741 0.1043 0.0907 0.031 Uiso 1 1 calc R . . C9 C 0.3086(3) 0.2435(2) 0.06657(17) 0.0229(7) Uani 1 1 d . . . C10 C 0.2493(4) 0.2302(3) -0.00743(18) 0.0328(8) Uani 1 1 d . . . H10A H 0.1612 0.1816 -0.0314 0.039 Uiso 1 1 calc R . . C11 C 0.3203(4) 0.2889(3) -0.0464(2) 0.0380(9) Uani 1 1 d . . . H11A H 0.2816 0.2810 -0.0976 0.046 Uiso 1 1 calc R . . C12 C 0.4475(4) 0.3588(3) -0.0098(2) 0.0387(9) Uani 1 1 d . . . H12A H 0.4989 0.3989 -0.0356 0.046 Uiso 1 1 calc R . . C13 C 0.4990(4) 0.3694(3) 0.06479(18) 0.0300(8) Uani 1 1 d . . . H13A H 0.5853 0.4193 0.0904 0.036 Uiso 1 1 calc R . . C14 C 0.3082(3) 0.1450(2) 0.23044(19) 0.0256(7) Uani 1 1 d . . . H14A H 0.2267 0.0832 0.2120 0.031 Uiso 1 1 calc R . . H14B H 0.3166 0.1787 0.2879 0.031 Uiso 1 1 calc R . . C15 C 0.4471(3) 0.1045(2) 0.20730(17) 0.0241(7) Uani 1 1 d . . . C16 C 0.4708(4) 0.0016(3) 0.2021(2) 0.0329(8) Uani 1 1 d . . . H16A H 0.3981 -0.0472 0.2111 0.039 Uiso 1 1 calc R . . C17 C 0.6020(4) -0.0283(3) 0.1835(2) 0.0396(9) Uani 1 1 d . . . H17A H 0.6216 -0.0979 0.1806 0.048 Uiso 1 1 calc R . . C18 C 0.7041(4) 0.0425(3) 0.1692(2) 0.0367(8) Uani 1 1 d . . . H18A H 0.7945 0.0224 0.1555 0.044 Uiso 1 1 calc R . . C19 C 0.6733(3) 0.1437(3) 0.17494(19) 0.0288(7) Uani 1 1 d . . . H19A H 0.7440 0.1930 0.1650 0.035 Uiso 1 1 calc R . . C20 C 0.3826(3) 0.7869(2) 0.35028(18) 0.0251(7) Uani 1 1 d . . . H20A H 0.3303 0.8137 0.3138 0.030 Uiso 1 1 calc R . . H20B H 0.4304 0.8509 0.3962 0.030 Uiso 1 1 calc R . . C21 C 0.2756(3) 0.7167(2) 0.37598(17) 0.0223(7) Uani 1 1 d . . . C22 C 0.1347(3) 0.7362(3) 0.38167(18) 0.0312(8) Uani 1 1 d . . . H22A H 0.1024 0.7927 0.3676 0.037 Uiso 1 1 calc R . . C23 C 0.0418(4) 0.6719(3) 0.4082(2) 0.0385(9) Uani 1 1 d . . . H23A H -0.0554 0.6836 0.4127 0.046 Uiso 1 1 calc R . . C24 C 0.0921(4) 0.5907(3) 0.42800(19) 0.0363(9) Uani 1 1 d . . . H24A H 0.0302 0.5459 0.4465 0.044 Uiso 1 1 calc R . . C25 C 0.2336(3) 0.5752(3) 0.42066(17) 0.0281(7) Uani 1 1 d . . . H25A H 0.2677 0.5190 0.4343 0.034 Uiso 1 1 calc R . . C26 C 0.6402(3) 0.7977(3) 0.33229(18) 0.0254(7) Uani 1 1 d . . . H26A H 0.6305 0.8679 0.3264 0.031 Uiso 1 1 calc R . . H26B H 0.7079 0.7623 0.2971 0.031 Uiso 1 1 calc R . . C27 C 0.6987(3) 0.8178(2) 0.41559(18) 0.0253(7) Uani 1 1 d . . . C28 C 0.7908(4) 0.9127(3) 0.4615(2) 0.0366(8) Uani 1 1 d . . . H28A H 0.8159 0.9685 0.4417 0.044 Uiso 1 1 calc R . . C29 C 0.8460(4) 0.9257(3) 0.5362(2) 0.0413(9) Uani 1 1 d . . . H29A H 0.9089 0.9906 0.5688 0.050 Uiso 1 1 calc R . . C30 C 0.8080(4) 0.8427(3) 0.5628(2) 0.0367(8) Uani 1 1 d . . . H30A H 0.8455 0.8490 0.6137 0.044 Uiso 1 1 calc R . . C31 C 0.7150(3) 0.7507(3) 0.51443(18) 0.0291(7) Uani 1 1 d . . . H31A H 0.6883 0.6940 0.5332 0.035 Uiso 1 1 calc R . . C32 C 0.7704(3) 0.4965(3) 0.26661(18) 0.0269(7) Uani 1 1 d . . . H32A H 0.8694 0.5141 0.2618 0.032 Uiso 1 1 calc R . . C33 C 0.5530(3) 0.4043(3) 0.40199(18) 0.0253(7) Uani 1 1 d . . . H33A H 0.5634 0.3751 0.4418 0.030 Uiso 1 1 calc R . . Cl1 Cl 0.00547(9) 0.88887(7) 0.23611(5) 0.0358(2) Uani 1 1 d . . . O1A O 0.1514(3) 0.9039(3) 0.26902(19) 0.0657(9) Uani 1 1 d . . . O1B O -0.0034(4) 0.9132(4) 0.1684(2) 0.0969(13) Uani 1 1 d . . . O1C O -0.0615(5) 0.7794(3) 0.2180(3) 0.1177(15) Uani 1 1 d . . . O1D O -0.0729(4) 0.9561(4) 0.2912(2) 0.1064(15) Uani 1 1 d . . . N1S N 0.1050(15) 0.9291(10) -0.0108(7) 0.140(4) Uiso 0.50 1 d PD A -1 C1S C 0.1641(12) 0.8790(9) 0.0219(6) 0.074(3) Uiso 0.50 1 d PD A -1 C2S C 0.194(3) 0.7849(16) 0.0424(14) 0.228(12) Uiso 0.50 1 d PD A -1 H2S1 H 0.1326 0.7186 0.0053 0.343 Uiso 0.50 1 d PR A -1 H2S2 H 0.1721 0.7960 0.0952 0.343 Uiso 0.50 1 d PR A -1 H2S3 H 0.2960 0.7775 0.0399 0.343 Uiso 0.50 1 d PR A -1 N1S' N 0.2484(11) 0.8200(9) 0.0209(6) 0.088(3) Uiso 0.50 1 d PD B -2 C1S' C 0.3422(18) 0.8847(15) 0.0134(12) 0.181(8) Uiso 0.50 1 d PD B -2 C2S' C 0.4599(17) 0.9592(12) 0.0026(10) 0.134(6) Uiso 0.50 1 d PD B -2 H2S4 H 0.4795 1.0279 0.0477 0.202 Uiso 0.50 1 d PR B -2 H2S5 H 0.4301 0.9736 -0.0443 0.202 Uiso 0.50 1 d PR B -2 H2S6 H 0.5477 0.9260 -0.0035 0.202 Uiso 0.50 1 d PR B -2 N2S N 0.7661(11) 0.1780(8) 0.3811(5) 0.065(2) Uiso 0.50 1 d PD C 1 C3S C 0.6707(13) 0.1344(10) 0.4090(7) 0.062(3) Uiso 0.50 1 d PD C 1 C4S C 0.5547(11) 0.0848(9) 0.4372(6) 0.075(3) Uiso 0.50 1 d PD C 1 H7S H 0.5040 0.1414 0.4688 0.113 Uiso 0.50 1 d PR C 1 H8S H 0.5936 0.0466 0.4691 0.113 Uiso 0.50 1 d PR C 1 H9S H 0.4869 0.0328 0.3929 0.113 Uiso 0.50 1 d PR C 1 N2S' N 0.6197(11) 0.1180(7) 0.4234(5) 0.062(2) Uiso 0.50 1 d PD D 2 C3S' C 0.7153(15) 0.1622(12) 0.3980(9) 0.081(3) Uiso 0.50 1 d PD D 2 C4S' C 0.8261(11) 0.2153(9) 0.3652(6) 0.072(3) Uiso 0.50 1 d PD D 2 H10S H 0.8663 0.1591 0.3261 0.108 Uiso 0.50 1 d PR D 2 H11S H 0.9037 0.2607 0.4070 0.108 Uiso 0.50 1 d PR D 2 H12S H 0.7827 0.2609 0.3408 0.108 Uiso 0.50 1 d PR D 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 Co1 0.0177(2) 0.0175(2) 0.0216(2) 0.00819(17) 0.00380(16) 0.00358(16) Co2 0.0172(2) 0.0200(2) 0.0187(2) 0.00715(17) 0.00309(16) 0.00273(16) S1 0.0182(4) 0.0216(4) 0.0319(4) 0.0130(3) 0.0080(3) 0.0030(3) S2 0.0213(4) 0.0201(4) 0.0224(4) 0.0107(3) 0.0023(3) 0.0013(3) O11 0.0171(12) 0.0293(13) 0.0565(16) 0.0196(12) 0.0074(10) -0.0015(9) O12 0.0317(13) 0.0301(13) 0.0280(12) 0.0152(10) 0.0120(10) 0.0088(10) O21 0.0350(13) 0.0247(12) 0.0314(13) 0.0178(10) 0.0006(10) 0.0030(10) O22 0.0226(12) 0.0278(12) 0.0239(11) 0.0110(10) 0.0064(9) 0.0041(9) O1 0.0158(10) 0.0182(11) 0.0199(10) 0.0080(9) 0.0000(8) 0.0037(8) O2 0.0224(12) 0.0253(12) 0.0310(12) 0.0063(10) 0.0074(9) 0.0028(9) O3 0.0202(11) 0.0295(13) 0.0261(12) 0.0050(10) 0.0052(9) 0.0043(9) O4 0.0350(13) 0.0273(12) 0.0230(12) 0.0104(10) 0.0019(10) 0.0094(10) O5 0.0390(13) 0.0255(13) 0.0205(11) 0.0107(10) 0.0047(10) 0.0071(10) N1 0.0215(14) 0.0174(13) 0.0244(14) 0.0097(11) 0.0058(10) 0.0031(10) N2 0.0247(14) 0.0193(14) 0.0221(14) 0.0066(11) 0.0060(11) 0.0028(11) N3 0.0209(14) 0.0192(14) 0.0279(14) 0.0083(11) 0.0044(11) 0.0046(11) N4 0.0177(13) 0.0206(14) 0.0221(13) 0.0086(11) 0.0031(10) 0.0025(10) N5 0.0227(14) 0.0243(15) 0.0193(13) 0.0048(11) 0.0034(10) 0.0038(11) N6 0.0194(14) 0.0228(14) 0.0234(14) 0.0051(11) 0.0044(11) 0.0036(10) C1 0.0180(16) 0.0185(16) 0.0166(15) 0.0056(12) 0.0052(12) 0.0047(12) C2 0.0190(16) 0.0186(16) 0.0230(16) 0.0071(13) 0.0043(12) 0.0048(12) C3 0.0165(16) 0.0263(17) 0.0236(16) 0.0059(14) 0.0044(12) 0.0036(12) C4 0.0204(17) 0.0324(19) 0.0230(16) 0.0122(14) 0.0031(13) 0.0074(13) C5 0.0261(17) 0.0251(17) 0.0231(17) 0.0112(14) 0.0035(13) 0.0083(13) C6 0.0172(15) 0.0199(16) 0.0216(16) 0.0084(13) 0.0024(12) 0.0023(12) C7 0.0252(18) 0.042(2) 0.041(2) 0.0203(17) -0.0020(15) 0.0059(15) C8 0.0259(18) 0.0228(17) 0.0246(17) 0.0051(14) 0.0020(13) -0.0008(13) C9 0.0249(17) 0.0200(16) 0.0227(17) 0.0053(13) 0.0040(13) 0.0075(13) C10 0.0317(19) 0.036(2) 0.0260(18) 0.0057(16) -0.0002(14) 0.0078(15) C11 0.055(2) 0.041(2) 0.0209(18) 0.0115(16) 0.0049(16) 0.0199(19) C12 0.063(3) 0.031(2) 0.0280(19) 0.0144(16) 0.0178(18) 0.0123(18) C13 0.038(2) 0.0244(18) 0.0272(18) 0.0087(15) 0.0111(15) 0.0009(14) C14 0.0270(18) 0.0212(17) 0.0336(18) 0.0153(14) 0.0085(14) 0.0033(13) C15 0.0268(17) 0.0207(17) 0.0261(17) 0.0092(14) 0.0057(13) 0.0050(13) C16 0.038(2) 0.0219(18) 0.045(2) 0.0169(16) 0.0126(16) 0.0088(15) C17 0.043(2) 0.027(2) 0.056(2) 0.0197(18) 0.0132(18) 0.0166(16) C18 0.032(2) 0.031(2) 0.053(2) 0.0176(18) 0.0132(17) 0.0157(16) C19 0.0264(18) 0.0265(18) 0.0356(19) 0.0120(15) 0.0079(14) 0.0076(14) C20 0.0262(17) 0.0208(17) 0.0283(17) 0.0078(14) 0.0038(13) 0.0075(13) C21 0.0205(16) 0.0247(17) 0.0178(15) 0.0023(13) 0.0030(12) 0.0054(13) C22 0.0260(19) 0.039(2) 0.0265(18) 0.0076(16) 0.0038(14) 0.0124(15) C23 0.0213(18) 0.052(2) 0.038(2) 0.0103(18) 0.0051(15) 0.0081(16) C24 0.027(2) 0.045(2) 0.0315(19) 0.0091(17) 0.0121(15) -0.0029(16) C25 0.0293(19) 0.0277(18) 0.0249(17) 0.0074(14) 0.0080(14) -0.0005(14) C26 0.0204(17) 0.0230(17) 0.0321(18) 0.0114(14) 0.0026(13) -0.0029(13) C27 0.0199(16) 0.0248(18) 0.0280(18) 0.0062(14) 0.0040(13) 0.0021(13) C28 0.035(2) 0.0260(19) 0.041(2) 0.0085(16) -0.0009(16) -0.0070(15) C29 0.036(2) 0.038(2) 0.033(2) 0.0001(17) -0.0057(16) -0.0098(16) C30 0.030(2) 0.045(2) 0.0252(18) 0.0051(17) -0.0006(15) -0.0017(16) C31 0.0249(18) 0.036(2) 0.0252(18) 0.0091(15) 0.0057(14) 0.0038(14) C32 0.0155(16) 0.0319(19) 0.0301(18) 0.0077(16) 0.0060(13) 0.0016(14) C33 0.0256(18) 0.033(2) 0.0236(18) 0.0169(16) 0.0028(13) 0.0069(14) Cl1 0.0297(5) 0.0347(5) 0.0397(5) 0.0115(4) -0.0044(4) 0.0067(4) O1A 0.0310(16) 0.096(2) 0.084(2) 0.052(2) -0.0049(15) 0.0124(15) O1B 0.082(3) 0.162(4) 0.071(2) 0.068(3) 0.0042(19) 0.037(3) O1C 0.100(3) 0.061(3) 0.166(4) 0.029(3) -0.010(3) -0.021(2) O1D 0.086(3) 0.134(4) 0.075(2) -0.005(2) 0.008(2) 0.060(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 Co2 3.5028(6) . ? Co1 O2 2.028(2) . ? Co1 O1 2.0530(19) . ? Co1 O4 2.102(2) . ? Co1 N3 2.102(2) . ? Co1 N2 2.121(2) . ? Co1 N1 2.288(2) . ? Co2 O5 2.005(2) . ? Co2 O1 2.0689(19) . ? Co2 O3 2.081(2) . ? Co2 N6 2.118(2) . ? Co2 N5 2.125(2) . ? Co2 N4 2.254(2) . ? S1 O12 1.424(2) . ? S1 O11 1.433(2) . ? S1 N1 1.700(2) . ? S1 C2 1.771(3) . ? S2 O22 1.428(2) . ? S2 O21 1.429(2) . ? S2 N4 1.704(2) . ? S2 C6 1.765(3) . ? O1 C1 1.313(3) . ? O2 C32 1.253(4) . ? O3 C32 1.245(4) . ? O4 C33 1.244(4) . ? O5 C33 1.246(4) . ? N1 C8 1.485(4) . ? N1 C14 1.499(4) . ? N2 C9 1.343(4) . ? N2 C13 1.345(4) . ? N3 C19 1.338(4) . ? N3 C15 1.340(4) . ? N4 C20 1.494(4) . ? N4 C26 1.499(4) . ? N5 C21 1.343(4) . ? N5 C25 1.351(4) . ? N6 C27 1.338(4) . ? N6 C31 1.341(4) . ? C1 C2 1.408(4) . ? C1 C6 1.414(4) . ? C2 C3 1.391(4) . ? C3 C4 1.396(4) . ? C3 H3A 0.950 . ? C4 C5 1.384(4) . ? C4 C7 1.510(4) . ? C5 C6 1.394(4) . ? C5 H5A 0.950 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.499(4) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 C10 1.377(4) . ? C10 C11 1.388(5) . ? C10 H10A 0.950 . ? C11 C12 1.375(5) . ? C11 H11A 0.950 . ? C12 C13 1.377(5) . ? C12 H12A 0.950 . ? C13 H13A 0.950 . ? C14 C15 1.510(4) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.383(4) . ? C16 C17 1.375(5) . ? C16 H16A 0.950 . ? C17 C18 1.368(5) . ? C17 H17A 0.950 . ? C18 C19 1.379(4) . ? C18 H18A 0.950 . ? C19 H19A 0.950 . ? C20 C21 1.507(4) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C21 C22 1.385(4) . ? C22 C23 1.386(5) . ? C22 H22A 0.950 . ? C23 C24 1.377(5) . ? C23 H23A 0.950 . ? C24 C25 1.380(5) . ? C24 H24A 0.950 . ? C25 H25A 0.950 . ? C26 C27 1.511(4) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.383(4) . ? C28 C29 1.380(5) . ? C28 H28A 0.950 . ? C29 C30 1.379(5) . ? C29 H29A 0.950 . ? C30 C31 1.375(5) . ? C30 H30A 0.950 . ? C31 H31A 0.950 . ? C32 H32A 0.950 . ? C33 H33A 0.950 . ? Cl1 O1B 1.400(3) . ? Cl1 O1A 1.412(3) . ? Cl1 O1C 1.421(4) . ? Cl1 O1D 1.424(3) . ? N1S C1S 1.198(8) . ? C1S C2S 1.479(8) . ? C2S H2S1 0.980 . ? C2S H2S2 0.980 . ? C2S H2S3 0.980 . ? N1S' C1S' 1.205(8) . ? C1S' C2S' 1.466(8) . ? C2S' H2S4 0.980 . ? C2S' H2S5 0.980 . ? C2S' H2S6 0.980 . ? N2S C3S 1.252(8) . ? C3S C4S 1.434(8) . ? C4S H7S 0.980 . ? C4S H8S 0.980 . ? C4S H9S 0.980 . ? N2S' C3S' 1.228(8) . ? C3S' C4S' 1.477(8) . ? C4S' H10S 0.980 . ? C4S' H11S 0.980 . ? C4S' H12S 0.980 . ? 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 O2 Co1 O1 97.58(8) . . ? O2 Co1 O4 94.43(9) . . ? O1 Co1 O4 89.66(8) . . ? O2 Co1 N3 97.20(9) . . ? O1 Co1 N3 163.21(9) . . ? O4 Co1 N3 81.30(9) . . ? O2 Co1 N2 93.97(9) . . ? O1 Co1 N2 91.83(8) . . ? O4 Co1 N2 171.20(9) . . ? N3 Co1 N2 95.04(9) . . ? O2 Co1 N1 167.60(8) . . ? O1 Co1 N1 91.45(8) . . ? O4 Co1 N1 94.10(8) . . ? N3 Co1 N1 75.24(9) . . ? N2 Co1 N1 77.20(9) . . ? O5 Co2 O1 97.01(8) . . ? O5 Co2 O3 91.81(9) . . ? O1 Co2 O3 90.73(8) . . ? O5 Co2 N6 95.46(9) . . ? O1 Co2 N6 165.83(9) . . ? O3 Co2 N6 82.15(9) . . ? O5 Co2 N5 95.13(9) . . ? O1 Co2 N5 88.36(8) . . ? O3 Co2 N5 173.06(9) . . ? N6 Co2 N5 97.23(9) . . ? O5 Co2 N4 168.18(9) . . ? O1 Co2 N4 92.26(8) . . ? O3 Co2 N4 95.41(8) . . ? N6 Co2 N4 76.33(9) . . ? N5 Co2 N4 77.76(9) . . ? O12 S1 O11 118.33(14) . . ? O12 S1 N1 106.04(12) . . ? O11 S1 N1 109.41(13) . . ? O12 S1 C2 111.27(13) . . ? O11 S1 C2 107.93(14) . . ? N1 S1 C2 102.73(12) . . ? O22 S2 O21 118.17(13) . . ? O22 S2 N4 105.96(12) . . ? O21 S2 N4 109.64(12) . . ? O22 S2 C6 110.56(13) . . ? O21 S2 C6 107.97(13) . . ? N4 S2 C6 103.56(13) . . ? C1 O1 Co1 120.62(17) . . ? C1 O1 Co2 122.88(17) . . ? Co1 O1 Co2 116.38(9) . . ? C32 O2 Co1 126.45(19) . . ? C32 O3 Co2 139.3(2) . . ? C33 O4 Co1 138.0(2) . . ? C33 O5 Co2 127.85(19) . . ? C8 N1 C14 111.8(2) . . ? C8 N1 S1 111.92(19) . . ? C14 N1 S1 110.96(18) . . ? C8 N1 Co1 107.34(17) . . ? C14 N1 Co1 102.38(17) . . ? S1 N1 Co1 112.04(12) . . ? C9 N2 C13 117.9(3) . . ? C9 N2 Co1 118.54(19) . . ? C13 N2 Co1 123.4(2) . . ? C19 N3 C15 118.7(3) . . ? C19 N3 Co1 124.5(2) . . ? C15 N3 Co1 116.20(19) . . ? C20 N4 C26 110.8(2) . . ? C20 N4 S2 111.99(19) . . ? C26 N4 S2 110.50(18) . . ? C20 N4 Co2 108.50(17) . . ? C26 N4 Co2 103.97(17) . . ? S2 N4 Co2 110.75(12) . . ? C21 N5 C25 118.2(3) . . ? C21 N5 Co2 117.54(19) . . ? C25 N5 Co2 123.1(2) . . ? C27 N6 C31 118.6(3) . . ? C27 N6 Co2 115.9(2) . . ? C31 N6 Co2 125.5(2) . . ? O1 C1 C2 122.5(3) . . ? O1 C1 C6 122.0(3) . . ? C2 C1 C6 115.5(3) . . ? C3 C2 C1 122.1(3) . . ? C3 C2 S1 117.4(2) . . ? C1 C2 S1 120.4(2) . . ? C2 C3 C4 121.3(3) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C5 C4 C3 117.8(3) . . ? C5 C4 C7 121.1(3) . . ? C3 C4 C7 121.2(3) . . ? C4 C5 C6 121.2(3) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C5 C6 C1 122.2(3) . . ? C5 C6 S2 117.1(2) . . ? C1 C6 S2 120.4(2) . . ? C4 C7 H7A 109.2 . . ? C4 C7 H7B 109.3 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.9 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 113.4(2) . . ? N1 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N1 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? N2 C9 C10 122.5(3) . . ? N2 C9 C8 116.4(3) . . ? C10 C9 C8 121.0(3) . . ? C9 C10 C11 119.0(3) . . ? C9 C10 H10A 120.5 . . ? C11 C10 H10A 120.5 . . ? C12 C11 C10 118.9(3) . . ? C12 C11 H11A 120.5 . . ? C10 C11 H11A 120.5 . . ? C11 C12 C13 118.9(3) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? N2 C13 C12 122.8(3) . . ? N2 C13 H13A 118.6 . . ? C12 C13 H13A 118.6 . . ? N1 C14 C15 109.0(2) . . ? N1 C14 H14A 109.9 . . ? C15 C14 H14A 109.9 . . ? N1 C14 H14B 109.9 . . ? C15 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? N3 C15 C16 122.0(3) . . ? N3 C15 C14 116.3(3) . . ? C16 C15 C14 121.6(3) . . ? C17 C16 C15 118.5(3) . . ? C17 C16 H16A 120.8 . . ? C15 C16 H16A 120.8 . . ? C18 C17 C16 119.8(3) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C17 C18 C19 118.7(3) . . ? C17 C18 H18A 120.6 . . ? C19 C18 H18A 120.6 . . ? N3 C19 C18 122.2(3) . . ? N3 C19 H19A 118.9 . . ? C18 C19 H19A 118.9 . . ? N4 C20 C21 111.8(2) . . ? N4 C20 H20A 109.3 . . ? C21 C20 H20A 109.3 . . ? N4 C20 H20B 109.3 . . ? C21 C20 H20B 109.3 . . ? H20A C20 H20B 107.9 . . ? N5 C21 C22 122.4(3) . . ? N5 C21 C20 116.6(3) . . ? C22 C21 C20 120.9(3) . . ? C21 C22 C23 118.8(3) . . ? C21 C22 H22A 120.6 . . ? C23 C22 H22A 120.6 . . ? C24 C23 C22 119.1(3) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? C23 C24 C25 119.2(3) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? N5 C25 C24 122.2(3) . . ? N5 C25 H25A 118.9 . . ? C24 C25 H25A 118.9 . . ? N4 C26 C27 109.1(2) . . ? N4 C26 H26A 109.9 . . ? C27 C26 H26A 109.9 . . ? N4 C26 H26B 109.9 . . ? C27 C26 H26B 109.9 . . ? H26A C26 H26B 108.3 . . ? N6 C27 C28 121.8(3) . . ? N6 C27 C26 116.7(3) . . ? C28 C27 C26 121.4(3) . . ? C29 C28 C27 119.4(3) . . ? C29 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? C30 C29 C28 118.6(3) . . ? C30 C29 H29A 120.7 . . ? C28 C29 H29A 120.7 . . ? C31 C30 C29 119.1(3) . . ? C31 C30 H30A 120.5 . . ? C29 C30 H30A 120.5 . . ? N6 C31 C30 122.5(3) . . ? N6 C31 H31A 118.8 . . ? C30 C31 H31A 118.8 . . ? O3 C32 O2 129.0(3) . . ? O3 C32 H32A 115.5 . . ? O2 C32 H32A 115.5 . . ? O4 C33 O5 129.3(3) . . ? O4 C33 H33A 115.4 . . ? O5 C33 H33A 115.4 . . ? O1B Cl1 O1A 110.6(2) . . ? O1B Cl1 O1C 109.4(3) . . ? O1A Cl1 O1C 110.0(2) . . ? O1B Cl1 O1D 110.1(2) . . ? O1A Cl1 O1D 109.9(2) . . ? O1C Cl1 O1D 106.6(3) . . ? N1S C1S C2S 158.5(15) . . ? C1S C2S H2S1 109.0 . . ? C1S C2S H2S2 109.7 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.7 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C1S' N1S' H2S3 105.0 . . ? N1S' C1S' C2S' 177(2) . . ? C1S' C2S' H2S4 109.9 . . ? C1S' C2S' H2S5 108.5 . . ? H2S4 C2S' H2S5 109.5 . . ? C1S' C2S' H2S6 109.9 . . ? H2S4 C2S' H2S6 109.5 . . ? H2S5 C2S' H2S6 109.5 . . ? C3S N2S H10S 145.4 . . ? C3S N2S H11S 140.3 . . ? H10S N2S H11S 66.0 . . ? N2S C3S C4S 176.3(11) . . ? C3S C4S H7S 109.3 . . ? C3S C4S H8S 109.8 . . ? H7S C4S H8S 109.5 . . ? C3S C4S H9S 109.3 . . ? H7S C4S H9S 109.5 . . ? H8S C4S H9S 109.5 . . ? C3S' N2S' H7S 141.6 . . ? C3S' N2S' H8S 142.9 . . ? H7S N2S' H8S 66.5 . . ? C3S' N2S' H9S 138.7 . . ? H7S N2S' H9S 66.3 . . ? H8S N2S' H9S 64.8 . . ? N2S' C3S' C4S' 177.9(13) . . ? C3S' C4S' H10S 109.1 . . ? C3S' C4S' H11S 109.3 . . ? H10S C4S' H11S 109.5 . . ? C3S' C4S' H12S 110.1 . . ? H10S C4S' H12S 109.5 . . ? H11S C4S' H12S 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Co1 O1 C1 126.0(2) . . . . ? O4 Co1 O1 C1 -139.6(2) . . . . ? N3 Co1 O1 C1 -82.5(4) . . . . ? N2 Co1 O1 C1 31.8(2) . . . . ? N1 Co1 O1 C1 -45.5(2) . . . . ? O2 Co1 O1 Co2 -50.10(11) . . . . ? O4 Co1 O1 Co2 44.33(10) . . . . ? N3 Co1 O1 Co2 101.4(3) . . . . ? N2 Co1 O1 Co2 -144.34(11) . . . . ? N1 Co1 O1 Co2 138.43(10) . . . . ? O5 Co2 O1 C1 133.0(2) . . . . ? O3 Co2 O1 C1 -135.1(2) . . . . ? N6 Co2 O1 C1 -75.6(4) . . . . ? N5 Co2 O1 C1 38.0(2) . . . . ? N4 Co2 O1 C1 -39.7(2) . . . . ? O5 Co2 O1 Co1 -51.03(11) . . . . ? O3 Co2 O1 Co1 40.89(10) . . . . ? N6 Co2 O1 Co1 100.4(3) . . . . ? N5 Co2 O1 Co1 -145.99(11) . . . . ? N4 Co2 O1 Co1 136.33(10) . . . . ? O1 Co1 O2 C32 33.0(3) . . . . ? O4 Co1 O2 C32 -57.2(3) . . . . ? N3 Co1 O2 C32 -139.0(3) . . . . ? N2 Co1 O2 C32 125.4(3) . . . . ? N1 Co1 O2 C32 169.4(4) . . . . ? O5 Co2 O3 C32 83.4(3) . . . . ? O1 Co2 O3 C32 -13.6(3) . . . . ? N6 Co2 O3 C32 178.7(3) . . . . ? N4 Co2 O3 C32 -106.0(3) . . . . ? O2 Co1 O4 C33 80.4(3) . . . . ? O1 Co1 O4 C33 -17.2(3) . . . . ? N3 Co1 O4 C33 177.0(3) . . . . ? N1 Co1 O4 C33 -108.6(3) . . . . ? O1 Co2 O5 C33 27.3(3) . . . . ? O3 Co2 O5 C33 -63.6(3) . . . . ? N6 Co2 O5 C33 -145.9(3) . . . . ? N5 Co2 O5 C33 116.3(3) . . . . ? N4 Co2 O5 C33 168.7(4) . . . . ? O12 S1 N1 C8 176.07(19) . . . . ? O11 S1 N1 C8 47.4(2) . . . . ? C2 S1 N1 C8 -67.1(2) . . . . ? O12 S1 N1 C14 50.5(2) . . . . ? O11 S1 N1 C14 -78.2(2) . . . . ? C2 S1 N1 C14 167.3(2) . . . . ? O12 S1 N1 Co1 -63.30(15) . . . . ? O11 S1 N1 Co1 168.03(12) . . . . ? C2 S1 N1 Co1 53.57(15) . . . . ? O2 Co1 N1 C8 -26.5(5) . . . . ? O1 Co1 N1 C8 110.36(18) . . . . ? O4 Co1 N1 C8 -159.87(18) . . . . ? N3 Co1 N1 C8 -79.99(18) . . . . ? N2 Co1 N1 C8 18.81(18) . . . . ? O2 Co1 N1 C14 91.3(4) . . . . ? O1 Co1 N1 C14 -131.84(17) . . . . ? O4 Co1 N1 C14 -42.07(17) . . . . ? N3 Co1 N1 C14 37.81(17) . . . . ? N2 Co1 N1 C14 136.61(18) . . . . ? O2 Co1 N1 S1 -149.8(3) . . . . ? O1 Co1 N1 S1 -12.89(13) . . . . ? O4 Co1 N1 S1 76.87(13) . . . . ? N3 Co1 N1 S1 156.75(15) . . . . ? N2 Co1 N1 S1 -104.44(13) . . . . ? O2 Co1 N2 C9 164.8(2) . . . . ? O1 Co1 N2 C9 -97.5(2) . . . . ? N3 Co1 N2 C9 67.2(2) . . . . ? N1 Co1 N2 C9 -6.4(2) . . . . ? O2 Co1 N2 C13 -20.0(2) . . . . ? O1 Co1 N2 C13 77.7(2) . . . . ? N3 Co1 N2 C13 -117.6(2) . . . . ? N1 Co1 N2 C13 168.8(3) . . . . ? O2 Co1 N3 C19 -7.1(3) . . . . ? O1 Co1 N3 C19 -158.7(3) . . . . ? O4 Co1 N3 C19 -100.5(3) . . . . ? N2 Co1 N3 C19 87.5(2) . . . . ? N1 Co1 N3 C19 162.9(3) . . . . ? O2 Co1 N3 C15 164.3(2) . . . . ? O1 Co1 N3 C15 12.8(5) . . . . ? O4 Co1 N3 C15 70.9(2) . . . . ? N2 Co1 N3 C15 -101.0(2) . . . . ? N1 Co1 N3 C15 -25.7(2) . . . . ? O22 S2 N4 C20 179.79(19) . . . . ? O21 S2 N4 C20 51.2(2) . . . . ? C6 S2 N4 C20 -63.8(2) . . . . ? O22 S2 N4 C26 55.7(2) . . . . ? O21 S2 N4 C26 -72.9(2) . . . . ? C6 S2 N4 C26 172.12(19) . . . . ? O22 S2 N4 Co2 -58.95(14) . . . . ? O21 S2 N4 Co2 172.48(12) . . . . ? C6 S2 N4 Co2 57.46(14) . . . . ? O5 Co2 N4 C20 -36.7(5) . . . . ? O1 Co2 N4 C20 104.96(18) . . . . ? O3 Co2 N4 C20 -164.09(18) . . . . ? N6 Co2 N4 C20 -83.54(18) . . . . ? N5 Co2 N4 C20 17.14(18) . . . . ? O5 Co2 N4 C26 81.3(5) . . . . ? O1 Co2 N4 C26 -137.03(17) . . . . ? O3 Co2 N4 C26 -46.09(18) . . . . ? N6 Co2 N4 C26 34.46(17) . . . . ? N5 Co2 N4 C26 135.14(18) . . . . ? O5 Co2 N4 S2 -160.0(4) . . . . ? O1 Co2 N4 S2 -18.34(12) . . . . ? O3 Co2 N4 S2 72.61(12) . . . . ? N6 Co2 N4 S2 153.16(14) . . . . ? N5 Co2 N4 S2 -106.16(13) . . . . ? O5 Co2 N5 C21 168.5(2) . . . . ? O1 Co2 N5 C21 -94.6(2) . . . . ? N6 Co2 N5 C21 72.3(2) . . . . ? N4 Co2 N5 C21 -1.9(2) . . . . ? O5 Co2 N5 C25 -24.3(2) . . . . ? O1 Co2 N5 C25 72.6(2) . . . . ? N6 Co2 N5 C25 -120.5(2) . . . . ? N4 Co2 N5 C25 165.2(2) . . . . ? O5 Co2 N6 C27 168.0(2) . . . . ? O1 Co2 N6 C27 16.5(5) . . . . ? O3 Co2 N6 C27 77.0(2) . . . . ? N5 Co2 N6 C27 -96.1(2) . . . . ? N4 Co2 N6 C27 -20.6(2) . . . . ? O5 Co2 N6 C31 -8.0(2) . . . . ? O1 Co2 N6 C31 -159.5(3) . . . . ? O3 Co2 N6 C31 -99.1(2) . . . . ? N5 Co2 N6 C31 87.9(2) . . . . ? N4 Co2 N6 C31 163.4(2) . . . . ? Co1 O1 C1 C2 54.9(3) . . . . ? Co2 O1 C1 C2 -129.3(2) . . . . ? Co1 O1 C1 C6 -124.6(2) . . . . ? Co2 O1 C1 C6 51.2(3) . . . . ? O1 C1 C2 C3 -177.8(3) . . . . ? C6 C1 C2 C3 1.7(4) . . . . ? O1 C1 C2 S1 6.7(4) . . . . ? C6 C1 C2 S1 -173.8(2) . . . . ? O12 S1 C2 C3 -126.4(2) . . . . ? O11 S1 C2 C3 5.0(3) . . . . ? N1 S1 C2 C3 120.5(2) . . . . ? O12 S1 C2 C1 49.3(3) . . . . ? O11 S1 C2 C1 -179.3(2) . . . . ? N1 S1 C2 C1 -63.7(3) . . . . ? C1 C2 C3 C4 -1.9(4) . . . . ? S1 C2 C3 C4 173.7(2) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C2 C3 C4 C7 -178.5(3) . . . . ? C3 C4 C5 C6 0.9(4) . . . . ? C7 C4 C5 C6 179.9(3) . . . . ? C4 C5 C6 C1 -1.0(5) . . . . ? C4 C5 C6 S2 172.6(2) . . . . ? O1 C1 C6 C5 179.2(3) . . . . ? C2 C1 C6 C5 -0.3(4) . . . . ? O1 C1 C6 S2 5.8(4) . . . . ? C2 C1 C6 S2 -173.7(2) . . . . ? O22 S2 C6 C5 -124.0(2) . . . . ? O21 S2 C6 C5 6.7(3) . . . . ? N4 S2 C6 C5 122.9(2) . . . . ? O22 S2 C6 C1 49.8(3) . . . . ? O21 S2 C6 C1 -179.5(2) . . . . ? N4 S2 C6 C1 -63.3(3) . . . . ? C14 N1 C8 C9 -140.2(3) . . . . ? S1 N1 C8 C9 94.7(3) . . . . ? Co1 N1 C8 C9 -28.7(3) . . . . ? C13 N2 C9 C10 -0.1(4) . . . . ? Co1 N2 C9 C10 175.3(2) . . . . ? C13 N2 C9 C8 176.4(3) . . . . ? Co1 N2 C9 C8 -8.1(3) . . . . ? N1 C8 C9 N2 26.0(4) . . . . ? N1 C8 C9 C10 -157.4(3) . . . . ? N2 C9 C10 C11 0.8(5) . . . . ? C8 C9 C10 C11 -175.6(3) . . . . ? C9 C10 C11 C12 -0.2(5) . . . . ? C10 C11 C12 C13 -1.0(5) . . . . ? C9 N2 C13 C12 -1.2(5) . . . . ? Co1 N2 C13 C12 -176.4(2) . . . . ? C11 C12 C13 N2 1.8(5) . . . . ? C8 N1 C14 C15 69.3(3) . . . . ? S1 N1 C14 C15 -165.0(2) . . . . ? Co1 N1 C14 C15 -45.3(3) . . . . ? C19 N3 C15 C16 0.3(5) . . . . ? Co1 N3 C15 C16 -171.7(2) . . . . ? C19 N3 C15 C14 178.7(3) . . . . ? Co1 N3 C15 C14 6.7(3) . . . . ? N1 C14 C15 N3 29.2(4) . . . . ? N1 C14 C15 C16 -152.4(3) . . . . ? N3 C15 C16 C17 0.7(5) . . . . ? C14 C15 C16 C17 -177.6(3) . . . . ? C15 C16 C17 C18 -1.3(5) . . . . ? C16 C17 C18 C19 1.0(6) . . . . ? C15 N3 C19 C18 -0.6(5) . . . . ? Co1 N3 C19 C18 170.6(3) . . . . ? C17 C18 C19 N3 0.0(5) . . . . ? C26 N4 C20 C21 -142.5(3) . . . . ? S2 N4 C20 C21 93.6(3) . . . . ? Co2 N4 C20 C21 -29.0(3) . . . . ? C25 N5 C21 C22 -0.5(4) . . . . ? Co2 N5 C21 C22 167.3(2) . . . . ? C25 N5 C21 C20 177.7(3) . . . . ? Co2 N5 C21 C20 -14.5(3) . . . . ? N4 C20 C21 N5 29.9(4) . . . . ? N4 C20 C21 C22 -151.8(3) . . . . ? N5 C21 C22 C23 0.4(5) . . . . ? C20 C21 C22 C23 -177.7(3) . . . . ? C21 C22 C23 C24 -0.1(5) . . . . ? C22 C23 C24 C25 -0.2(5) . . . . ? C21 N5 C25 C24 0.2(4) . . . . ? Co2 N5 C25 C24 -166.9(2) . . . . ? C23 C24 C25 N5 0.1(5) . . . . ? C20 N4 C26 C27 72.7(3) . . . . ? S2 N4 C26 C27 -162.5(2) . . . . ? Co2 N4 C26 C27 -43.7(3) . . . . ? C31 N6 C27 C28 -0.7(4) . . . . ? Co2 N6 C27 C28 -177.0(2) . . . . ? C31 N6 C27 C26 177.3(3) . . . . ? Co2 N6 C27 C26 1.0(3) . . . . ? N4 C26 C27 N6 31.0(4) . . . . ? N4 C26 C27 C28 -150.9(3) . . . . ? N6 C27 C28 C29 0.4(5) . . . . ? C26 C27 C28 C29 -177.5(3) . . . . ? C27 C28 C29 C30 0.4(5) . . . . ? C28 C29 C30 C31 -0.9(5) . . . . ? C27 N6 C31 C30 0.1(4) . . . . ? Co2 N6 C31 C30 176.1(2) . . . . ? C29 C30 C31 N6 0.7(5) . . . . ? Co2 O3 C32 O2 -5.1(6) . . . . ? Co1 O2 C32 O3 -7.2(5) . . . . ? Co1 O4 C33 O5 -7.4(5) . . . . ? Co2 O5 C33 O4 0.5(5) . . . . ? #============================================================================== data_7_2Acetone _database_code_depnum_ccdc_archive 'CCDC 772403' #TrackingRef '- submit_all.cif' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C49 H47 Co2 N6 O13 S2 +, Cl O4 -, 2(C3 H6 O) ; _chemical_formula_sum 'C55 H59 Cl Co2 N6 O19 S2' _chemical_formula_weight 1325.51 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' S S 0.1246 0.1234 '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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 16.2647(13) _cell_length_b 19.8095(16) _cell_length_c 18.7038(14) _cell_angle_alpha 90.00 _cell_angle_beta 106.037(3) _cell_angle_gamma 90.00 _cell_volume 5791.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5249 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 22.49 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2744 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 0.927 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ? _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 85764 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 25.05 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.994 _reflns_number_total 10210 _reflns_number_gt 6958 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+1.9048P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10210 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.515 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.061 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.38425(2) 0.156692(19) 0.72220(2) 0.02141(11) Uani 1 1 d . . . Co2 Co 0.40605(2) 0.220035(19) 0.555219(19) 0.02079(11) Uani 1 1 d . . . S1 S 0.51171(4) 0.28149(4) 0.80689(4) 0.02444(18) Uani 1 1 d . . . S2 S 0.24078(4) 0.31922(4) 0.55749(4) 0.02401(18) Uani 1 1 d . . . O11 O 0.54798(12) 0.31897(10) 0.87365(10) 0.0329(5) Uani 1 1 d . . . O12 O 0.56841(11) 0.25617(9) 0.76718(10) 0.0283(5) Uani 1 1 d . . . O21 O 0.18763(11) 0.37522(10) 0.52523(10) 0.0310(5) Uani 1 1 d . . . O22 O 0.20102(11) 0.25808(10) 0.57001(10) 0.0282(5) Uani 1 1 d . . . O1 O 0.38682(11) 0.24114(9) 0.65957(9) 0.0206(4) Uani 1 1 d . . . O2 O 0.30303(11) 0.10084(9) 0.64518(10) 0.0261(5) Uani 1 1 d . . . O3 O 0.31931(12) 0.14151(9) 0.53774(10) 0.0256(5) Uani 1 1 d . . . O4 O 0.49310(12) 0.12346(10) 0.69622(10) 0.0287(5) Uani 1 1 d . . . O5 O 0.51694(11) 0.16766(9) 0.59326(10) 0.0248(5) Uani 1 1 d . . . O6 O 0.02979(12) -0.07520(10) 0.41355(10) 0.0327(5) Uani 1 1 d . . . O7 O 0.09848(12) 0.00880(10) 0.34168(10) 0.0334(5) Uani 1 1 d . . . O8 O 0.88994(12) 0.09478(10) 0.80086(11) 0.0341(5) Uani 1 1 d . . . O9 O 0.77535(12) 0.03012(10) 0.84482(10) 0.0327(5) Uani 1 1 d . . . N1 N 0.45801(13) 0.21322(11) 0.82725(11) 0.0220(5) Uani 1 1 d . . . N2 N 0.28451(14) 0.19962(12) 0.75995(12) 0.0253(6) Uani 1 1 d . . . N3 N 0.41911(14) 0.07923(11) 0.80159(12) 0.0226(5) Uani 1 1 d . . . N4 N 0.30433(13) 0.29882(11) 0.50174(12) 0.0210(5) Uani 1 1 d . . . N5 N 0.47849(13) 0.31095(11) 0.56503(12) 0.0226(5) Uani 1 1 d . . . N6 N 0.38777(14) 0.20943(11) 0.43874(12) 0.0237(6) Uani 1 1 d . . . C1 C 0.37748(16) 0.30274(14) 0.68128(14) 0.0201(6) Uani 1 1 d . . . C2 C 0.42938(16) 0.32982(14) 0.74882(14) 0.0210(6) Uani 1 1 d . . . C3 C 0.42249(17) 0.39675(14) 0.76942(15) 0.0252(7) Uani 1 1 d . . . H3A H 0.4587 0.4127 0.8153 0.030 Uiso 1 1 calc R . . C4 C 0.36431(17) 0.44048(14) 0.72480(15) 0.0245(7) Uani 1 1 d . . . C5 C 0.31044(17) 0.41449(14) 0.65950(15) 0.0246(7) Uani 1 1 d . . . H5A H 0.2688 0.4431 0.6283 0.029 Uiso 1 1 calc R . . C6 C 0.31605(16) 0.34794(13) 0.63889(14) 0.0209(6) Uani 1 1 d . . . C7 C 0.3619(2) 0.51435(14) 0.74445(16) 0.0334(8) Uani 1 1 d . . . H7A H 0.4028 0.5228 0.7930 0.050 Uiso 1 1 calc R . . H7B H 0.3042 0.5263 0.7466 0.050 Uiso 1 1 calc R . . H7C H 0.3772 0.5419 0.7065 0.050 Uiso 1 1 calc R . . C8 C 0.39559(18) 0.23413(15) 0.86858(15) 0.0283(7) Uani 1 1 d . . . H8A H 0.4144 0.2775 0.8941 0.034 Uiso 1 1 calc R . . H8B H 0.3954 0.1999 0.9071 0.034 Uiso 1 1 calc R . . C9 C 0.30622(18) 0.24200(15) 0.81862(16) 0.0270(7) Uani 1 1 d . . . C10 C 0.2490(2) 0.28663(16) 0.83413(18) 0.0385(8) Uani 1 1 d . . . H10A H 0.2663 0.3169 0.8749 0.046 Uiso 1 1 calc R . . C11 C 0.1655(2) 0.28672(18) 0.7891(2) 0.0494(9) Uani 1 1 d . . . H11A H 0.1246 0.3172 0.7985 0.059 Uiso 1 1 calc R . . C12 C 0.1426(2) 0.24209(18) 0.73052(18) 0.0436(9) Uani 1 1 d . . . H12A H 0.0854 0.2405 0.6998 0.052 Uiso 1 1 calc R . . C13 C 0.20313(18) 0.20038(16) 0.71723(16) 0.0314(8) Uani 1 1 d . . . H13A H 0.1872 0.1705 0.6760 0.038 Uiso 1 1 calc R . . C14 C 0.52076(17) 0.16272(13) 0.86949(15) 0.0269(7) Uani 1 1 d . . . H14A H 0.5396 0.1759 0.9226 0.032 Uiso 1 1 calc R . . H14B H 0.5717 0.1624 0.8503 0.032 Uiso 1 1 calc R . . C15 C 0.48247(17) 0.09286(14) 0.86278(15) 0.0224(7) Uani 1 1 d . . . C16 C 0.51751(18) 0.04320(15) 0.91421(15) 0.0278(7) Uani 1 1 d . . . H16A H 0.5611 0.0541 0.9582 0.033 Uiso 1 1 calc R . . C17 C 0.48845(19) -0.02235(16) 0.90094(16) 0.0329(8) Uani 1 1 d . . . H17A H 0.5122 -0.0572 0.9353 0.039 Uiso 1 1 calc R . . C18 C 0.42468(19) -0.03648(15) 0.83738(17) 0.0338(8) Uani 1 1 d . . . H18A H 0.4041 -0.0813 0.8269 0.041 Uiso 1 1 calc R . . C19 C 0.39112(18) 0.01541(15) 0.78909(16) 0.0285(7) Uani 1 1 d . . . H19A H 0.3466 0.0057 0.7454 0.034 Uiso 1 1 calc R . . C20 C 0.34929(17) 0.35931(14) 0.48358(16) 0.0267(7) Uani 1 1 d . . . H20A H 0.3153 0.4001 0.4864 0.032 Uiso 1 1 calc R . . H20B H 0.3533 0.3553 0.4319 0.032 Uiso 1 1 calc R . . C21 C 0.43815(17) 0.36744(14) 0.53558(14) 0.0210(6) Uani 1 1 d . . . C22 C 0.47528(18) 0.43018(15) 0.55000(15) 0.0288(7) Uani 1 1 d . . . H22A H 0.4440 0.4695 0.5298 0.035 Uiso 1 1 calc R . . C23 C 0.55831(19) 0.43527(15) 0.59411(16) 0.0317(7) Uani 1 1 d . . . H23A H 0.5854 0.4781 0.6044 0.038 Uiso 1 1 calc R . . C24 C 0.60109(18) 0.37737(15) 0.62296(16) 0.0308(7) Uani 1 1 d . . . H24A H 0.6586 0.3795 0.6530 0.037 Uiso 1 1 calc R . . C25 C 0.55993(17) 0.31655(15) 0.60795(15) 0.0259(7) Uani 1 1 d . . . H25A H 0.5898 0.2768 0.6285 0.031 Uiso 1 1 calc R . . C26 C 0.25239(17) 0.26376(14) 0.43305(14) 0.0240(7) Uani 1 1 d . . . H26A H 0.2161 0.2970 0.3989 0.029 Uiso 1 1 calc R . . H26B H 0.2145 0.2299 0.4465 0.029 Uiso 1 1 calc R . . C27 C 0.31139(17) 0.22959(14) 0.39503(15) 0.0233(7) Uani 1 1 d . . . C28 C 0.28756(18) 0.21941(15) 0.31894(15) 0.0297(7) Uani 1 1 d . . . H28A H 0.2334 0.2345 0.2892 0.036 Uiso 1 1 calc R . . C29 C 0.3437(2) 0.18700(16) 0.28686(17) 0.0378(8) Uani 1 1 d . . . H29A H 0.3283 0.1789 0.2348 0.045 Uiso 1 1 calc R . . C30 C 0.4225(2) 0.16652(16) 0.33129(17) 0.0389(8) Uani 1 1 d . . . H30A H 0.4624 0.1445 0.3105 0.047 Uiso 1 1 calc R . . C31 C 0.44149(19) 0.17880(15) 0.40606(17) 0.0332(8) Uani 1 1 d . . . H31A H 0.4958 0.1649 0.4366 0.040 Uiso 1 1 calc R . . C32 C 0.28527(17) 0.10323(14) 0.57490(15) 0.0229(7) Uani 1 1 d . . . C33 C 0.21827(16) 0.05473(14) 0.53355(14) 0.0211(6) Uani 1 1 d . . . C34 C 0.18291(18) 0.00786(14) 0.57106(15) 0.0272(7) Uani 1 1 d . . . H34A H 0.2022 0.0059 0.6238 0.033 Uiso 1 1 calc R . . C35 C 0.11973(18) -0.03638(15) 0.53317(16) 0.0290(7) Uani 1 1 d . . . H35A H 0.0957 -0.0679 0.5600 0.035 Uiso 1 1 calc R . . C36 C 0.09169(17) -0.03471(14) 0.45642(15) 0.0253(7) Uani 1 1 d . . . C37 C 0.12873(17) 0.01146(14) 0.41748(14) 0.0228(7) Uani 1 1 d . . . C38 C 0.19046(17) 0.05603(14) 0.45601(15) 0.0232(7) Uani 1 1 d . . . H38A H 0.2143 0.0879 0.4294 0.028 Uiso 1 1 calc R . . C39 C -0.0055(2) -0.12525(16) 0.45141(18) 0.0392(8) Uani 1 1 d . . . H39A H -0.0479 -0.1520 0.4150 0.059 Uiso 1 1 calc R . . H39B H -0.0331 -0.1032 0.4856 0.059 Uiso 1 1 calc R . . H39C H 0.0403 -0.1549 0.4796 0.059 Uiso 1 1 calc R . . C40 C 0.1439(2) 0.04679(16) 0.30056(16) 0.0385(8) Uani 1 1 d . . . H40A H 0.1200 0.0377 0.2473 0.058 Uiso 1 1 calc R . . H40B H 0.2044 0.0338 0.3159 0.058 Uiso 1 1 calc R . . H40C H 0.1387 0.0950 0.3101 0.058 Uiso 1 1 calc R . . C41 C 0.54098(17) 0.14014(14) 0.65706(16) 0.0236(7) Uani 1 1 d . . . C42 C 0.63482(17) 0.12639(14) 0.68908(15) 0.0226(7) Uani 1 1 d . . . C43 C 0.69668(17) 0.15608(14) 0.66236(15) 0.0256(7) Uani 1 1 d . . . H43A H 0.6801 0.1837 0.6192 0.031 Uiso 1 1 calc R . . C44 C 0.78308(18) 0.14642(14) 0.69740(16) 0.0278(7) Uani 1 1 d . . . H44A H 0.8252 0.1674 0.6784 0.033 Uiso 1 1 calc R . . C45 C 0.80738(17) 0.10613(14) 0.76007(16) 0.0258(7) Uani 1 1 d . . . C46 C 0.74518(18) 0.07280(14) 0.78541(15) 0.0257(7) Uani 1 1 d . . . C47 C 0.65955(17) 0.08357(14) 0.75085(15) 0.0244(7) Uani 1 1 d . . . H47A H 0.6173 0.0619 0.7690 0.029 Uiso 1 1 calc R . . C48 C 0.95544(18) 0.12757(17) 0.77582(19) 0.0420(9) Uani 1 1 d . . . H48A H 1.0116 0.1158 0.8089 0.063 Uiso 1 1 calc R . . H48B H 0.9474 0.1766 0.7763 0.063 Uiso 1 1 calc R . . H48C H 0.9521 0.1127 0.7251 0.063 Uiso 1 1 calc R . . C49 C 0.7136(2) -0.00765(18) 0.86857(19) 0.0513(10) Uani 1 1 d . . . H49A H 0.7427 -0.0396 0.9074 0.077 Uiso 1 1 calc R . . H49B H 0.6773 -0.0326 0.8262 0.077 Uiso 1 1 calc R . . H49C H 0.6781 0.0231 0.8885 0.077 Uiso 1 1 calc R . . Cl1 Cl 0.39033(5) 0.21010(4) 0.08610(5) 0.0433(2) Uani 1 1 d . . . O1A O 0.43312(15) 0.24604(14) 0.15076(13) 0.0640(8) Uani 1 1 d . . . O1B O 0.44989(18) 0.18342(13) 0.05010(14) 0.0675(8) Uani 1 1 d . . . O1C O 0.3377(2) 0.15874(14) 0.10164(14) 0.0829(10) Uani 1 1 d . . . O1D O 0.33741(17) 0.25689(14) 0.03363(17) 0.0807(9) Uani 1 1 d . . . O1S O 0.6207(2) 0.08294(14) 0.36236(17) 0.0795(9) Uani 1 1 d . . . C1S C 0.6110(3) 0.06204(19) 0.4189(2) 0.0539(10) Uani 1 1 d . . . C2S C 0.5478(3) 0.0088(2) 0.4167(3) 0.1045(18) Uani 1 1 d . . . H2SA H 0.5331 -0.0132 0.3679 0.157 Uiso 1 1 calc R . . H2SB H 0.4962 0.0286 0.4255 0.157 Uiso 1 1 calc R . . H2SC H 0.5718 -0.0247 0.4554 0.157 Uiso 1 1 calc R . . C3S C 0.6603(3) 0.0885(3) 0.4915(2) 0.1025(19) Uani 1 1 d . . . H3SA H 0.6895 0.1302 0.4842 0.154 Uiso 1 1 calc R . . H3SB H 0.7028 0.0550 0.5167 0.154 Uiso 1 1 calc R . . H3SC H 0.6215 0.0981 0.5221 0.154 Uiso 1 1 calc R . . O2S O 0.1607(2) 0.04305(17) 0.95691(16) 0.0966(11) Uani 1 1 d . . . C4S C 0.1962(3) 0.0929(3) 0.9444(2) 0.0693(13) Uani 1 1 d . . . C5S C 0.1560(3) 0.1590(3) 0.9431(2) 0.0935(17) Uani 1 1 d . . . H5SA H 0.0982 0.1533 0.9485 0.140 Uiso 1 1 calc R . . H5SB H 0.1529 0.1815 0.8958 0.140 Uiso 1 1 calc R . . H5SC H 0.1901 0.1865 0.9843 0.140 Uiso 1 1 calc R . . C6S C 0.2815(3) 0.0888(3) 0.9299(2) 0.0963(18) Uani 1 1 d . . . H6SA H 0.3014 0.0419 0.9350 0.145 Uiso 1 1 calc R . . H6SB H 0.3223 0.1171 0.9659 0.145 Uiso 1 1 calc R . . H6SC H 0.2770 0.1048 0.8794 0.145 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0171(2) 0.0280(2) 0.0159(2) 0.00046(17) -0.00082(16) -0.00194(17) Co2 0.0162(2) 0.0255(2) 0.0173(2) 0.00224(16) -0.00105(16) 0.00050(17) S1 0.0191(4) 0.0283(4) 0.0203(4) 0.0034(3) -0.0040(3) -0.0050(3) S2 0.0172(4) 0.0326(5) 0.0182(4) -0.0014(3) -0.0018(3) 0.0035(3) O11 0.0329(12) 0.0335(12) 0.0226(11) 0.0008(9) -0.0085(9) -0.0092(10) O12 0.0191(10) 0.0334(12) 0.0293(12) 0.0068(9) 0.0016(9) -0.0020(9) O21 0.0215(11) 0.0393(13) 0.0251(11) -0.0013(9) -0.0054(9) 0.0120(10) O22 0.0214(11) 0.0364(13) 0.0253(11) -0.0035(9) 0.0040(9) -0.0056(9) O1 0.0200(10) 0.0226(11) 0.0157(10) 0.0005(8) -0.0009(8) 0.0001(8) O2 0.0251(11) 0.0312(12) 0.0167(11) -0.0029(9) -0.0029(9) -0.0046(9) O3 0.0241(11) 0.0302(12) 0.0205(11) -0.0002(9) 0.0029(9) -0.0050(9) O4 0.0200(11) 0.0368(12) 0.0282(11) 0.0077(9) 0.0049(10) 0.0038(9) O5 0.0189(10) 0.0305(12) 0.0225(11) 0.0045(9) 0.0017(9) 0.0037(9) O6 0.0312(12) 0.0328(12) 0.0270(11) -0.0050(9) -0.0037(10) -0.0102(10) O7 0.0405(13) 0.0350(12) 0.0179(11) -0.0005(9) -0.0031(10) -0.0047(10) O8 0.0170(11) 0.0431(13) 0.0352(12) 0.0010(10) -0.0047(9) 0.0036(10) O9 0.0246(11) 0.0416(13) 0.0283(12) 0.0104(10) 0.0011(9) 0.0066(10) N1 0.0175(12) 0.0273(14) 0.0179(12) 0.0031(10) -0.0007(10) -0.0038(10) N2 0.0200(13) 0.0351(15) 0.0190(13) 0.0003(11) 0.0024(11) -0.0023(11) N3 0.0194(13) 0.0278(14) 0.0193(13) 0.0003(10) 0.0031(11) -0.0033(11) N4 0.0169(12) 0.0251(13) 0.0176(12) 0.0019(10) -0.0010(10) -0.0020(10) N5 0.0191(13) 0.0284(14) 0.0180(13) 0.0044(11) 0.0010(10) -0.0005(11) N6 0.0205(13) 0.0285(14) 0.0202(13) 0.0024(11) 0.0026(11) 0.0012(11) C1 0.0164(15) 0.0270(17) 0.0165(15) 0.0014(13) 0.0039(12) -0.0033(13) C2 0.0168(15) 0.0261(18) 0.0188(15) 0.0040(12) 0.0028(12) -0.0018(12) C3 0.0226(16) 0.0346(19) 0.0175(15) -0.0003(13) 0.0039(13) -0.0089(14) C4 0.0233(16) 0.0273(17) 0.0243(16) 0.0011(13) 0.0089(14) -0.0031(13) C5 0.0232(16) 0.0292(18) 0.0211(16) 0.0036(13) 0.0058(13) 0.0033(13) C6 0.0171(15) 0.0272(17) 0.0155(15) -0.0009(13) -0.0001(12) 0.0011(13) C7 0.0383(19) 0.0323(19) 0.0268(17) -0.0038(14) 0.0041(15) -0.0002(15) C8 0.0301(17) 0.0348(19) 0.0192(16) -0.0027(13) 0.0055(14) -0.0075(14) C9 0.0262(17) 0.0313(18) 0.0243(17) 0.0024(14) 0.0085(14) -0.0049(14) C10 0.040(2) 0.038(2) 0.038(2) -0.0081(16) 0.0116(17) 0.0026(17) C11 0.038(2) 0.060(3) 0.054(2) 0.000(2) 0.0200(19) 0.0162(18) C12 0.0244(18) 0.067(3) 0.037(2) 0.0045(18) 0.0040(16) 0.0084(18) C13 0.0191(16) 0.048(2) 0.0250(17) 0.0006(14) 0.0025(14) -0.0028(15) C14 0.0225(16) 0.0312(18) 0.0200(15) 0.0074(13) -0.0058(13) -0.0048(14) C15 0.0174(15) 0.0324(18) 0.0168(15) 0.0018(13) 0.0038(13) -0.0005(13) C16 0.0249(16) 0.036(2) 0.0177(15) 0.0030(14) -0.0014(13) -0.0041(14) C17 0.0357(18) 0.037(2) 0.0256(18) 0.0075(14) 0.0075(15) 0.0039(16) C18 0.0395(19) 0.0267(18) 0.0348(19) -0.0002(15) 0.0098(16) -0.0059(15) C19 0.0270(17) 0.0342(19) 0.0226(16) -0.0020(14) 0.0042(13) -0.0051(15) C20 0.0231(16) 0.0306(18) 0.0239(16) 0.0062(13) 0.0024(13) 0.0040(14) C21 0.0215(15) 0.0261(17) 0.0154(15) 0.0016(13) 0.0055(12) -0.0014(14) C22 0.0314(18) 0.0289(18) 0.0264(17) 0.0043(14) 0.0088(14) 0.0003(14) C23 0.0344(19) 0.0275(18) 0.0310(18) -0.0013(14) 0.0055(15) -0.0094(15) C24 0.0208(16) 0.043(2) 0.0247(17) 0.0023(15) -0.0008(13) -0.0069(15) C25 0.0198(16) 0.0331(18) 0.0217(16) 0.0052(13) 0.0007(13) -0.0008(14) C26 0.0156(15) 0.0341(18) 0.0176(15) -0.0004(13) -0.0031(12) 0.0037(13) C27 0.0222(16) 0.0265(17) 0.0195(16) 0.0039(13) 0.0028(13) -0.0025(13) C28 0.0252(17) 0.0410(19) 0.0197(16) 0.0019(14) 0.0008(14) -0.0010(15) C29 0.043(2) 0.050(2) 0.0202(17) -0.0001(15) 0.0080(16) 0.0004(17) C30 0.0356(19) 0.050(2) 0.034(2) -0.0026(16) 0.0148(16) 0.0079(17) C31 0.0264(17) 0.041(2) 0.0302(19) 0.0019(15) 0.0044(15) 0.0065(15) C32 0.0178(15) 0.0268(17) 0.0204(17) -0.0031(13) -0.0009(13) 0.0053(13) C33 0.0154(14) 0.0263(17) 0.0188(15) -0.0026(13) 0.0002(12) 0.0010(13) C34 0.0296(17) 0.0343(18) 0.0155(15) -0.0038(13) 0.0028(13) -0.0027(15) C35 0.0297(17) 0.0327(18) 0.0244(17) 0.0003(14) 0.0071(14) -0.0059(14) C36 0.0222(16) 0.0225(16) 0.0272(17) -0.0066(13) 0.0001(14) -0.0027(13) C37 0.0236(16) 0.0261(17) 0.0146(15) -0.0023(13) -0.0015(13) 0.0043(13) C38 0.0210(15) 0.0258(16) 0.0211(16) 0.0016(13) 0.0030(13) -0.0005(13) C39 0.0347(19) 0.0345(19) 0.042(2) -0.0082(16) 0.0000(16) -0.0135(16) C40 0.056(2) 0.037(2) 0.0212(17) -0.0019(15) 0.0084(16) 0.0013(17) C41 0.0208(16) 0.0236(17) 0.0241(17) -0.0007(13) 0.0025(14) 0.0011(13) C42 0.0201(15) 0.0228(16) 0.0220(16) -0.0002(13) 0.0013(13) 0.0023(13) C43 0.0245(16) 0.0281(17) 0.0229(16) 0.0034(13) 0.0044(13) 0.0043(14) C44 0.0215(16) 0.0313(18) 0.0308(18) -0.0003(14) 0.0074(14) 0.0011(13) C45 0.0179(16) 0.0283(17) 0.0288(17) -0.0058(14) 0.0021(14) 0.0031(13) C46 0.0282(17) 0.0240(17) 0.0214(16) 0.0025(13) 0.0012(14) 0.0092(14) C47 0.0192(16) 0.0310(17) 0.0229(16) 0.0018(13) 0.0055(13) 0.0028(13) C48 0.0149(16) 0.053(2) 0.053(2) -0.0065(18) 0.0010(16) -0.0005(16) C49 0.040(2) 0.060(2) 0.052(2) 0.0322(19) 0.0091(18) 0.0069(19) Cl1 0.0486(5) 0.0437(5) 0.0376(5) -0.0082(4) 0.0119(4) -0.0117(4) O1A 0.0439(15) 0.098(2) 0.0481(16) -0.0349(14) 0.0086(13) -0.0186(14) O1B 0.093(2) 0.0629(17) 0.0586(17) -0.0041(14) 0.0418(16) 0.0113(16) O1C 0.113(2) 0.091(2) 0.0492(17) -0.0057(15) 0.0291(17) -0.0662(19) O1D 0.0628(18) 0.075(2) 0.087(2) 0.0280(17) -0.0079(16) 0.0031(16) O1S 0.107(2) 0.070(2) 0.061(2) 0.0189(16) 0.0235(18) 0.0149(17) C1S 0.071(3) 0.041(2) 0.048(2) 0.0022(19) 0.014(2) 0.027(2) C2S 0.143(5) 0.045(3) 0.153(5) -0.006(3) 0.086(4) -0.013(3) C3S 0.089(4) 0.139(4) 0.058(3) -0.042(3) -0.015(3) 0.066(3) O2S 0.120(3) 0.104(3) 0.080(2) -0.0212(18) 0.052(2) -0.076(2) C4S 0.088(3) 0.087(4) 0.030(2) -0.014(2) 0.013(2) -0.058(3) C5S 0.091(4) 0.121(5) 0.052(3) 0.011(3) -0.007(3) -0.039(3) C6S 0.104(4) 0.131(4) 0.065(3) -0.047(3) 0.042(3) -0.085(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 Co2 3.4737(6) . ? Co1 O2 1.9983(17) . ? Co1 O1 2.0493(18) . ? Co1 O4 2.0688(19) . ? Co1 N3 2.101(2) . ? Co1 N2 2.118(2) . ? Co1 N1 2.292(2) . ? Co2 O5 2.0314(17) . ? Co2 O3 2.0646(19) . ? Co2 O1 2.1023(18) . ? Co2 N6 2.126(2) . ? Co2 N5 2.132(2) . ? Co2 N4 2.293(2) . ? S1 O12 1.426(2) . ? S1 O11 1.4323(19) . ? S1 N1 1.709(2) . ? S1 C2 1.757(3) . ? S2 O22 1.422(2) . ? S2 O21 1.4332(19) . ? S2 N4 1.707(2) . ? S2 C6 1.764(3) . ? O1 C1 1.308(3) . ? O2 C32 1.266(3) . ? O3 C32 1.256(3) . ? O4 C41 1.252(3) . ? O5 C41 1.271(3) . ? O6 C36 1.361(3) . ? O6 C39 1.428(3) . ? O7 C37 1.367(3) . ? O7 C40 1.421(3) . ? O8 C45 1.367(3) . ? O8 C48 1.432(4) . ? O9 C46 1.374(3) . ? O9 C49 1.419(4) . ? N1 C14 1.490(3) . ? N1 C8 1.494(3) . ? N2 C13 1.344(3) . ? N2 C9 1.349(4) . ? N3 C15 1.339(3) . ? N3 C19 1.342(3) . ? N4 C20 1.491(3) . ? N4 C26 1.499(3) . ? N5 C21 1.337(3) . ? N5 C25 1.351(3) . ? N6 C31 1.342(4) . ? N6 C27 1.345(3) . ? C1 C6 1.411(4) . ? C1 C2 1.417(4) . ? C2 C3 1.394(4) . ? C3 C4 1.381(4) . ? C3 H3A 0.950 . ? C4 C5 1.390(4) . ? C4 C7 1.512(4) . ? C5 C6 1.384(4) . ? C5 H5A 0.950 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.503(4) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 C10 1.371(4) . ? C10 C11 1.387(4) . ? C10 H10A 0.950 . ? C11 C12 1.377(5) . ? C11 H11A 0.950 . ? C12 C13 1.360(4) . ? C12 H12A 0.950 . ? C13 H13A 0.950 . ? C14 C15 1.509(4) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 C16 1.384(4) . ? C16 C17 1.381(4) . ? C16 H16A 0.950 . ? C17 C18 1.373(4) . ? C17 H17A 0.950 . ? C18 C19 1.378(4) . ? C18 H18A 0.950 . ? C19 H19A 0.950 . ? C20 C21 1.511(4) . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C21 C22 1.376(4) . ? C22 C23 1.378(4) . ? C22 H22A 0.950 . ? C23 C24 1.372(4) . ? C23 H23A 0.950 . ? C24 C25 1.369(4) . ? C24 H24A 0.950 . ? C25 H25A 0.950 . ? C26 C27 1.504(4) . ? C26 H26A 0.990 . ? C26 H26B 0.990 . ? C27 C28 1.383(4) . ? C28 C29 1.382(4) . ? C28 H28A 0.950 . ? C29 C30 1.382(4) . ? C29 H29A 0.950 . ? C30 C31 1.368(4) . ? C30 H30A 0.950 . ? C31 H31A 0.950 . ? C32 C33 1.498(4) . ? C33 C34 1.381(4) . ? C33 C38 1.395(4) . ? C34 C35 1.387(4) . ? C34 H34A 0.950 . ? C35 C36 1.381(4) . ? C35 H35A 0.950 . ? C36 C37 1.405(4) . ? C37 C38 1.381(4) . ? C38 H38A 0.950 . ? C39 H39A 0.980 . ? C39 H39B 0.980 . ? C39 H39C 0.980 . ? C40 H40A 0.980 . ? C40 H40B 0.980 . ? C40 H40C 0.980 . ? C41 C42 1.502(4) . ? C42 C43 1.373(4) . ? C42 C47 1.400(4) . ? C43 C44 1.390(4) . ? C43 H43A 0.950 . ? C44 C45 1.383(4) . ? C44 H44A 0.950 . ? C45 C46 1.396(4) . ? C46 C47 1.380(4) . ? C47 H47A 0.950 . ? C48 H48A 0.980 . ? C48 H48B 0.980 . ? C48 H48C 0.980 . ? C49 H49A 0.980 . ? C49 H49B 0.980 . ? C49 H49C 0.980 . ? Cl1 O1A 1.410(2) . ? Cl1 O1C 1.411(2) . ? Cl1 O1B 1.425(3) . ? Cl1 O1D 1.448(3) . ? O1S C1S 1.186(4) . ? C1S C2S 1.467(6) . ? C1S C3S 1.470(5) . ? C2S H2SA 0.980 . ? C2S H2SB 0.980 . ? C2S H2SC 0.980 . ? C3S H3SA 0.980 . ? C3S H3SB 0.980 . ? C3S H3SC 0.980 . ? O2S C4S 1.199(4) . ? C4S C5S 1.461(6) . ? C4S C6S 1.487(6) . ? C5S H5SA 0.980 . ? C5S H5SB 0.980 . ? C5S H5SC 0.980 . ? C6S H6SA 0.980 . ? C6S H6SB 0.980 . ? C6S H6SC 0.980 . ? 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 O2 Co1 O1 98.84(7) . . ? O2 Co1 O4 95.31(8) . . ? O1 Co1 O4 88.37(7) . . ? O2 Co1 N3 95.78(8) . . ? O1 Co1 N3 162.92(8) . . ? O4 Co1 N3 81.51(8) . . ? O2 Co1 N2 92.75(8) . . ? O1 Co1 N2 90.07(8) . . ? O4 Co1 N2 171.93(8) . . ? N3 Co1 N2 98.02(9) . . ? O2 Co1 N1 166.89(8) . . ? O1 Co1 N1 90.15(7) . . ? O4 Co1 N1 94.45(8) . . ? N3 Co1 N1 77.05(8) . . ? N2 Co1 N1 77.63(8) . . ? O5 Co2 O3 99.93(7) . . ? O5 Co2 O1 97.00(7) . . ? O3 Co2 O1 91.51(7) . . ? O5 Co2 N6 99.66(8) . . ? O3 Co2 N6 82.38(8) . . ? O1 Co2 N6 163.01(8) . . ? O5 Co2 N5 89.15(8) . . ? O3 Co2 N5 170.85(8) . . ? O1 Co2 N5 88.43(8) . . ? N6 Co2 N5 95.11(8) . . ? O5 Co2 N4 164.60(8) . . ? O3 Co2 N4 93.70(7) . . ? O1 Co2 N4 89.72(7) . . ? N6 Co2 N4 74.96(8) . . ? N5 Co2 N4 77.15(8) . . ? O12 S1 O11 117.82(12) . . ? O12 S1 N1 106.37(11) . . ? O11 S1 N1 109.19(11) . . ? O12 S1 C2 111.22(12) . . ? O11 S1 C2 108.45(13) . . ? N1 S1 C2 102.70(12) . . ? O22 S2 O21 118.65(12) . . ? O22 S2 N4 106.18(11) . . ? O21 S2 N4 108.82(11) . . ? O22 S2 C6 111.80(12) . . ? O21 S2 C6 107.92(12) . . ? N4 S2 C6 102.16(12) . . ? C1 O1 Co1 124.17(16) . . ? C1 O1 Co2 122.24(15) . . ? Co1 O1 Co2 113.59(8) . . ? C32 O2 Co1 130.05(18) . . ? C32 O3 Co2 138.92(17) . . ? C41 O4 Co1 139.86(18) . . ? C41 O5 Co2 124.12(18) . . ? C36 O6 C39 116.8(2) . . ? C37 O7 C40 116.7(2) . . ? C45 O8 C48 116.6(2) . . ? C46 O9 C49 116.9(2) . . ? C14 N1 C8 112.1(2) . . ? C14 N1 S1 109.39(16) . . ? C8 N1 S1 110.98(18) . . ? C14 N1 Co1 104.25(16) . . ? C8 N1 Co1 108.02(15) . . ? S1 N1 Co1 111.99(10) . . ? C13 N2 C9 118.0(3) . . ? C13 N2 Co1 121.70(19) . . ? C9 N2 Co1 117.94(18) . . ? C15 N3 C19 118.9(2) . . ? C15 N3 Co1 116.76(18) . . ? C19 N3 Co1 123.53(18) . . ? C20 N4 C26 111.9(2) . . ? C20 N4 S2 111.52(17) . . ? C26 N4 S2 109.89(16) . . ? C20 N4 Co2 107.83(15) . . ? C26 N4 Co2 103.08(15) . . ? S2 N4 Co2 112.34(11) . . ? C21 N5 C25 117.7(2) . . ? C21 N5 Co2 118.36(17) . . ? C25 N5 Co2 123.26(19) . . ? C31 N6 C27 117.8(2) . . ? C31 N6 Co2 125.95(18) . . ? C27 N6 Co2 115.95(18) . . ? O1 C1 C6 122.9(2) . . ? O1 C1 C2 122.6(2) . . ? C6 C1 C2 114.6(2) . . ? C3 C2 C1 122.2(2) . . ? C3 C2 S1 117.0(2) . . ? C1 C2 S1 120.6(2) . . ? C4 C3 C2 121.6(3) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 117.3(3) . . ? C3 C4 C7 121.3(3) . . ? C5 C4 C7 121.3(3) . . ? C6 C5 C4 121.6(3) . . ? C6 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? C5 C6 C1 122.6(2) . . ? C5 C6 S2 117.7(2) . . ? C1 C6 S2 119.7(2) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C9 112.7(2) . . ? N1 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N1 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? N2 C9 C10 122.2(3) . . ? N2 C9 C8 115.6(3) . . ? C10 C9 C8 122.1(3) . . ? C9 C10 C11 118.7(3) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? C12 C11 C10 119.1(3) . . ? C12 C11 H11A 120.5 . . ? C10 C11 H11A 120.5 . . ? C13 C12 C11 119.1(3) . . ? C13 C12 H12A 120.5 . . ? C11 C12 H12A 120.5 . . ? N2 C13 C12 122.8(3) . . ? N2 C13 H13A 118.6 . . ? C12 C13 H13A 118.6 . . ? N1 C14 C15 111.4(2) . . ? N1 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? N1 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? N3 C15 C16 121.5(3) . . ? N3 C15 C14 117.3(2) . . ? C16 C15 C14 120.9(2) . . ? C17 C16 C15 119.3(3) . . ? C17 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? C18 C17 C16 119.1(3) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C17 C18 C19 118.9(3) . . ? C17 C18 H18A 120.6 . . ? C19 C18 H18A 120.6 . . ? N3 C19 C18 122.3(3) . . ? N3 C19 H19A 118.8 . . ? C18 C19 H19A 118.8 . . ? N4 C20 C21 112.4(2) . . ? N4 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? N4 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? N5 C21 C22 122.5(2) . . ? N5 C21 C20 116.7(2) . . ? C22 C21 C20 120.8(2) . . ? C21 C22 C23 119.2(3) . . ? C21 C22 H22A 120.4 . . ? C23 C22 H22A 120.4 . . ? C24 C23 C22 118.7(3) . . ? C24 C23 H23A 120.6 . . ? C22 C23 H23A 120.6 . . ? C25 C24 C23 119.3(3) . . ? C25 C24 H24A 120.4 . . ? C23 C24 H24A 120.4 . . ? N5 C25 C24 122.5(3) . . ? N5 C25 H25A 118.7 . . ? C24 C25 H25A 118.7 . . ? N4 C26 C27 109.4(2) . . ? N4 C26 H26A 109.8 . . ? C27 C26 H26A 109.8 . . ? N4 C26 H26B 109.8 . . ? C27 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? N6 C27 C28 122.1(3) . . ? N6 C27 C26 116.7(2) . . ? C28 C27 C26 121.2(2) . . ? C29 C28 C27 118.9(3) . . ? C29 C28 H28A 120.5 . . ? C27 C28 H28A 120.5 . . ? C28 C29 C30 119.3(3) . . ? C28 C29 H29A 120.3 . . ? C30 C29 H29A 120.3 . . ? C31 C30 C29 118.2(3) . . ? C31 C30 H30A 120.9 . . ? C29 C30 H30A 120.9 . . ? N6 C31 C30 123.7(3) . . ? N6 C31 H31A 118.2 . . ? C30 C31 H31A 118.2 . . ? O3 C32 O2 126.0(2) . . ? O3 C32 C33 118.1(2) . . ? O2 C32 C33 115.9(3) . . ? C34 C33 C38 118.7(2) . . ? C34 C33 C32 121.0(2) . . ? C38 C33 C32 120.4(3) . . ? C33 C34 C35 121.2(3) . . ? C33 C34 H34A 119.4 . . ? C35 C34 H34A 119.4 . . ? C36 C35 C34 120.1(3) . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? O6 C36 C35 125.2(3) . . ? O6 C36 C37 115.6(2) . . ? C35 C36 C37 119.2(2) . . ? O7 C37 C38 124.6(3) . . ? O7 C37 C36 115.4(2) . . ? C38 C37 C36 120.0(2) . . ? C37 C38 C33 120.7(3) . . ? C37 C38 H38A 119.6 . . ? C33 C38 H38A 119.6 . . ? O6 C39 H39A 109.5 . . ? O6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O7 C40 H40A 109.5 . . ? O7 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O7 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O4 C41 O5 125.6(2) . . ? O4 C41 C42 116.5(2) . . ? O5 C41 C42 117.8(3) . . ? C43 C42 C47 119.2(2) . . ? C43 C42 C41 122.9(2) . . ? C47 C42 C41 117.9(3) . . ? C42 C43 C44 121.1(3) . . ? C42 C43 H43A 119.5 . . ? C44 C43 H43A 119.5 . . ? C45 C44 C43 119.6(3) . . ? C45 C44 H44A 120.2 . . ? C43 C44 H44A 120.2 . . ? O8 C45 C44 125.1(3) . . ? O8 C45 C46 115.1(3) . . ? C44 C45 C46 119.8(2) . . ? O9 C46 C47 124.2(3) . . ? O9 C46 C45 115.8(2) . . ? C47 C46 C45 120.0(3) . . ? C46 C47 C42 120.2(3) . . ? C46 C47 H47A 119.9 . . ? C42 C47 H47A 119.9 . . ? O8 C48 H48A 109.5 . . ? O8 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O8 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O9 C49 H49A 109.5 . . ? O9 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? O9 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? O1A Cl1 O1C 111.78(16) . . ? O1A Cl1 O1B 110.71(16) . . ? O1C Cl1 O1B 111.12(18) . . ? O1A Cl1 O1D 108.55(18) . . ? O1C Cl1 O1D 108.68(18) . . ? O1B Cl1 O1D 105.76(17) . . ? O1S C1S C2S 119.4(4) . . ? O1S C1S C3S 121.8(4) . . ? C2S C1S C3S 118.8(4) . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C1S C3S H3SA 109.5 . . ? C1S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? C1S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? O2S C4S C5S 120.2(5) . . ? O2S C4S C6S 121.0(5) . . ? C5S C4S C6S 118.8(4) . . ? C4S C5S H5SA 109.5 . . ? C4S C5S H5SB 109.5 . . ? H5SA C5S H5SB 109.5 . . ? C4S C5S H5SC 109.5 . . ? H5SA C5S H5SC 109.5 . . ? H5SB C5S H5SC 109.5 . . ? C4S C6S H6SA 109.5 . . ? C4S C6S H6SB 109.5 . . ? H6SA C6S H6SB 109.5 . . ? C4S C6S H6SC 109.5 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Co1 O1 C1 131.68(19) . . . . ? O4 Co1 O1 C1 -133.19(19) . . . . ? N3 Co1 O1 C1 -79.8(3) . . . . ? N2 Co1 O1 C1 38.89(19) . . . . ? N1 Co1 O1 C1 -38.74(19) . . . . ? O2 Co1 O1 Co2 -48.28(9) . . . . ? O4 Co1 O1 Co2 46.84(9) . . . . ? N3 Co1 O1 Co2 100.3(3) . . . . ? N2 Co1 O1 Co2 -141.07(9) . . . . ? N1 Co1 O1 Co2 141.30(9) . . . . ? O5 Co2 O1 C1 124.11(18) . . . . ? O3 Co2 O1 C1 -135.70(18) . . . . ? N6 Co2 O1 C1 -67.3(3) . . . . ? N5 Co2 O1 C1 35.15(19) . . . . ? N4 Co2 O1 C1 -42.00(18) . . . . ? O5 Co2 O1 Co1 -55.93(9) . . . . ? O3 Co2 O1 Co1 44.26(9) . . . . ? N6 Co2 O1 Co1 112.7(3) . . . . ? N5 Co2 O1 Co1 -144.89(9) . . . . ? N4 Co2 O1 Co1 137.96(9) . . . . ? O1 Co1 O2 C32 24.6(2) . . . . ? O4 Co1 O2 C32 -64.6(2) . . . . ? N3 Co1 O2 C32 -146.6(2) . . . . ? N2 Co1 O2 C32 115.1(2) . . . . ? N1 Co1 O2 C32 157.4(3) . . . . ? O5 Co2 O3 C32 76.8(3) . . . . ? O1 Co2 O3 C32 -20.6(3) . . . . ? N6 Co2 O3 C32 175.3(3) . . . . ? N4 Co2 O3 C32 -110.4(3) . . . . ? O2 Co1 O4 C41 94.3(3) . . . . ? O1 Co1 O4 C41 -4.5(3) . . . . ? N3 Co1 O4 C41 -170.7(3) . . . . ? N1 Co1 O4 C41 -94.5(3) . . . . ? O3 Co2 O5 C41 -72.0(2) . . . . ? O1 Co2 O5 C41 20.8(2) . . . . ? N6 Co2 O5 C41 -155.9(2) . . . . ? N5 Co2 O5 C41 109.1(2) . . . . ? N4 Co2 O5 C41 136.0(3) . . . . ? O12 S1 N1 C14 56.43(19) . . . . ? O11 S1 N1 C14 -71.7(2) . . . . ? C2 S1 N1 C14 173.36(18) . . . . ? O12 S1 N1 C8 -179.42(16) . . . . ? O11 S1 N1 C8 52.47(19) . . . . ? C2 S1 N1 C8 -62.49(19) . . . . ? O12 S1 N1 Co1 -58.62(13) . . . . ? O11 S1 N1 Co1 173.27(11) . . . . ? C2 S1 N1 Co1 58.31(14) . . . . ? O2 Co1 N1 C14 87.5(4) . . . . ? O1 Co1 N1 C14 -138.97(16) . . . . ? O4 Co1 N1 C14 -50.59(16) . . . . ? N3 Co1 N1 C14 29.62(16) . . . . ? N2 Co1 N1 C14 130.99(17) . . . . ? O2 Co1 N1 C8 -31.9(4) . . . . ? O1 Co1 N1 C8 101.69(16) . . . . ? O4 Co1 N1 C8 -169.94(16) . . . . ? N3 Co1 N1 C8 -89.72(17) . . . . ? N2 Co1 N1 C8 11.65(16) . . . . ? O2 Co1 N1 S1 -154.4(3) . . . . ? O1 Co1 N1 S1 -20.82(12) . . . . ? O4 Co1 N1 S1 67.56(12) . . . . ? N3 Co1 N1 S1 147.78(13) . . . . ? N2 Co1 N1 S1 -110.86(12) . . . . ? O2 Co1 N2 C13 -20.9(2) . . . . ? O1 Co1 N2 C13 78.0(2) . . . . ? N3 Co1 N2 C13 -117.1(2) . . . . ? N1 Co1 N2 C13 168.1(2) . . . . ? O2 Co1 N2 C9 176.7(2) . . . . ? O1 Co1 N2 C9 -84.4(2) . . . . ? N3 Co1 N2 C9 80.5(2) . . . . ? N1 Co1 N2 C9 5.7(2) . . . . ? O2 Co1 N3 C15 173.09(19) . . . . ? O1 Co1 N3 C15 24.3(4) . . . . ? O4 Co1 N3 C15 78.56(19) . . . . ? N2 Co1 N3 C15 -93.30(19) . . . . ? N1 Co1 N3 C15 -18.04(19) . . . . ? O2 Co1 N3 C19 3.7(2) . . . . ? O1 Co1 N3 C19 -145.1(3) . . . . ? O4 Co1 N3 C19 -90.8(2) . . . . ? N2 Co1 N3 C19 97.3(2) . . . . ? N1 Co1 N3 C19 172.6(2) . . . . ? O22 S2 N4 C20 179.33(16) . . . . ? O21 S2 N4 C20 50.55(19) . . . . ? C6 S2 N4 C20 -63.41(19) . . . . ? O22 S2 N4 C26 54.66(19) . . . . ? O21 S2 N4 C26 -74.12(19) . . . . ? C6 S2 N4 C26 171.92(17) . . . . ? O22 S2 N4 Co2 -59.48(13) . . . . ? O21 S2 N4 Co2 171.74(10) . . . . ? C6 S2 N4 Co2 57.78(13) . . . . ? O5 Co2 N4 C20 -10.2(4) . . . . ? O3 Co2 N4 C20 -162.57(16) . . . . ? O1 Co2 N4 C20 105.93(16) . . . . ? N6 Co2 N4 C20 -81.49(17) . . . . ? N5 Co2 N4 C20 17.48(16) . . . . ? O5 Co2 N4 C26 108.2(3) . . . . ? O3 Co2 N4 C26 -44.09(16) . . . . ? O1 Co2 N4 C26 -135.58(15) . . . . ? N6 Co2 N4 C26 36.99(15) . . . . ? N5 Co2 N4 C26 135.96(17) . . . . ? O5 Co2 N4 S2 -133.5(3) . . . . ? O3 Co2 N4 S2 74.15(11) . . . . ? O1 Co2 N4 S2 -17.35(11) . . . . ? N6 Co2 N4 S2 155.22(13) . . . . ? N5 Co2 N4 S2 -105.80(12) . . . . ? O5 Co2 N5 C21 169.91(19) . . . . ? O1 Co2 N5 C21 -93.07(19) . . . . ? N6 Co2 N5 C21 70.3(2) . . . . ? N4 Co2 N5 C21 -2.99(19) . . . . ? O5 Co2 N5 C25 -19.5(2) . . . . ? O1 Co2 N5 C25 77.6(2) . . . . ? N6 Co2 N5 C25 -119.1(2) . . . . ? N4 Co2 N5 C25 167.6(2) . . . . ? O5 Co2 N6 C31 -3.2(2) . . . . ? O3 Co2 N6 C31 -102.0(2) . . . . ? O1 Co2 N6 C31 -171.7(2) . . . . ? N5 Co2 N6 C31 86.8(2) . . . . ? N4 Co2 N6 C31 162.0(2) . . . . ? O5 Co2 N6 C27 169.82(19) . . . . ? O3 Co2 N6 C27 70.98(19) . . . . ? O1 Co2 N6 C27 1.3(4) . . . . ? N5 Co2 N6 C27 -100.17(19) . . . . ? N4 Co2 N6 C27 -24.96(18) . . . . ? Co1 O1 C1 C6 -126.3(2) . . . . ? Co2 O1 C1 C6 53.7(3) . . . . ? Co1 O1 C1 C2 54.8(3) . . . . ? Co2 O1 C1 C2 -125.2(2) . . . . ? O1 C1 C2 C3 176.0(2) . . . . ? C6 C1 C2 C3 -2.9(4) . . . . ? O1 C1 C2 S1 1.3(4) . . . . ? C6 C1 C2 S1 -177.7(2) . . . . ? O12 S1 C2 C3 -121.0(2) . . . . ? O11 S1 C2 C3 10.1(2) . . . . ? N1 S1 C2 C3 125.6(2) . . . . ? O12 S1 C2 C1 54.1(2) . . . . ? O11 S1 C2 C1 -174.8(2) . . . . ? N1 S1 C2 C1 -59.3(2) . . . . ? C1 C2 C3 C4 0.0(4) . . . . ? S1 C2 C3 C4 175.0(2) . . . . ? C2 C3 C4 C5 2.3(4) . . . . ? C2 C3 C4 C7 -175.1(3) . . . . ? C3 C4 C5 C6 -1.6(4) . . . . ? C7 C4 C5 C6 175.8(3) . . . . ? C4 C5 C6 C1 -1.6(4) . . . . ? C4 C5 C6 S2 176.7(2) . . . . ? O1 C1 C6 C5 -175.3(2) . . . . ? C2 C1 C6 C5 3.7(4) . . . . ? O1 C1 C6 S2 6.5(4) . . . . ? C2 C1 C6 S2 -174.53(19) . . . . ? O22 S2 C6 C5 -129.7(2) . . . . ? O21 S2 C6 C5 2.6(3) . . . . ? N4 S2 C6 C5 117.2(2) . . . . ? O22 S2 C6 C1 48.6(3) . . . . ? O21 S2 C6 C1 -179.1(2) . . . . ? N4 S2 C6 C1 -64.5(2) . . . . ? C14 N1 C8 C9 -140.2(2) . . . . ? S1 N1 C8 C9 97.2(2) . . . . ? Co1 N1 C8 C9 -26.0(3) . . . . ? C13 N2 C9 C10 -2.1(4) . . . . ? Co1 N2 C9 C10 160.9(2) . . . . ? C13 N2 C9 C8 174.2(2) . . . . ? Co1 N2 C9 C8 -22.7(3) . . . . ? N1 C8 C9 N2 33.1(3) . . . . ? N1 C8 C9 C10 -150.6(3) . . . . ? N2 C9 C10 C11 1.9(5) . . . . ? C8 C9 C10 C11 -174.3(3) . . . . ? C9 C10 C11 C12 0.1(5) . . . . ? C10 C11 C12 C13 -1.7(5) . . . . ? C9 N2 C13 C12 0.4(4) . . . . ? Co1 N2 C13 C12 -162.0(2) . . . . ? C11 C12 C13 N2 1.5(5) . . . . ? C8 N1 C14 C15 79.1(3) . . . . ? S1 N1 C14 C15 -157.43(19) . . . . ? Co1 N1 C14 C15 -37.5(2) . . . . ? C19 N3 C15 C16 -2.1(4) . . . . ? Co1 N3 C15 C16 -172.0(2) . . . . ? C19 N3 C15 C14 171.5(2) . . . . ? Co1 N3 C15 C14 1.5(3) . . . . ? N1 C14 C15 N3 26.9(3) . . . . ? N1 C14 C15 C16 -159.5(2) . . . . ? N3 C15 C16 C17 2.2(4) . . . . ? C14 C15 C16 C17 -171.2(3) . . . . ? C15 C16 C17 C18 -0.8(4) . . . . ? C16 C17 C18 C19 -0.6(4) . . . . ? C15 N3 C19 C18 0.7(4) . . . . ? Co1 N3 C19 C18 169.9(2) . . . . ? C17 C18 C19 N3 0.7(4) . . . . ? C26 N4 C20 C21 -141.5(2) . . . . ? S2 N4 C20 C21 95.0(2) . . . . ? Co2 N4 C20 C21 -28.8(3) . . . . ? C25 N5 C21 C22 -2.7(4) . . . . ? Co2 N5 C21 C22 168.4(2) . . . . ? C25 N5 C21 C20 176.0(2) . . . . ? Co2 N5 C21 C20 -12.9(3) . . . . ? N4 C20 C21 N5 29.1(3) . . . . ? N4 C20 C21 C22 -152.2(2) . . . . ? N5 C21 C22 C23 2.5(4) . . . . ? C20 C21 C22 C23 -176.1(3) . . . . ? C21 C22 C23 C24 -0.7(4) . . . . ? C22 C23 C24 C25 -0.8(4) . . . . ? C21 N5 C25 C24 1.1(4) . . . . ? Co2 N5 C25 C24 -169.5(2) . . . . ? C23 C24 C25 N5 0.6(4) . . . . ? C20 N4 C26 C27 70.9(3) . . . . ? S2 N4 C26 C27 -164.68(18) . . . . ? Co2 N4 C26 C27 -44.7(2) . . . . ? C31 N6 C27 C28 0.2(4) . . . . ? Co2 N6 C27 C28 -173.4(2) . . . . ? C31 N6 C27 C26 180.0(2) . . . . ? Co2 N6 C27 C26 6.3(3) . . . . ? N4 C26 C27 N6 28.7(3) . . . . ? N4 C26 C27 C28 -151.5(3) . . . . ? N6 C27 C28 C29 0.6(4) . . . . ? C26 C27 C28 C29 -179.2(3) . . . . ? C27 C28 C29 C30 -0.9(5) . . . . ? C28 C29 C30 C31 0.6(5) . . . . ? C27 N6 C31 C30 -0.6(4) . . . . ? Co2 N6 C31 C30 172.3(2) . . . . ? C29 C30 C31 N6 0.2(5) . . . . ? Co2 O3 C32 O2 -5.2(4) . . . . ? Co2 O3 C32 C33 175.81(18) . . . . ? Co1 O2 C32 O3 3.0(4) . . . . ? Co1 O2 C32 C33 -177.98(16) . . . . ? O3 C32 C33 C34 175.2(2) . . . . ? O2 C32 C33 C34 -3.9(4) . . . . ? O3 C32 C33 C38 -4.7(4) . . . . ? O2 C32 C33 C38 176.2(2) . . . . ? C38 C33 C34 C35 -1.3(4) . . . . ? C32 C33 C34 C35 178.8(2) . . . . ? C33 C34 C35 C36 0.8(4) . . . . ? C39 O6 C36 C35 -3.1(4) . . . . ? C39 O6 C36 C37 176.5(2) . . . . ? C34 C35 C36 O6 -179.4(3) . . . . ? C34 C35 C36 C37 0.9(4) . . . . ? C40 O7 C37 C38 10.8(4) . . . . ? C40 O7 C37 C36 -170.0(2) . . . . ? O6 C36 C37 O7 -0.9(4) . . . . ? C35 C36 C37 O7 178.7(2) . . . . ? O6 C36 C37 C38 178.2(2) . . . . ? C35 C36 C37 C38 -2.1(4) . . . . ? O7 C37 C38 C33 -179.3(2) . . . . ? C36 C37 C38 C33 1.6(4) . . . . ? C34 C33 C38 C37 0.1(4) . . . . ? C32 C33 C38 C37 180.0(2) . . . . ? Co1 O4 C41 O5 -36.2(5) . . . . ? Co1 O4 C41 C42 143.5(2) . . . . ? Co2 O5 C41 O4 22.3(4) . . . . ? Co2 O5 C41 C42 -157.46(18) . . . . ? O4 C41 C42 C43 -163.5(3) . . . . ? O5 C41 C42 C43 16.3(4) . . . . ? O4 C41 C42 C47 13.8(4) . . . . ? O5 C41 C42 C47 -166.5(2) . . . . ? C47 C42 C43 C44 -2.6(4) . . . . ? C41 C42 C43 C44 174.6(3) . . . . ? C42 C43 C44 C45 0.2(4) . . . . ? C48 O8 C45 C44 0.0(4) . . . . ? C48 O8 C45 C46 179.2(2) . . . . ? C43 C44 C45 O8 -177.5(3) . . . . ? C43 C44 C45 C46 3.2(4) . . . . ? C49 O9 C46 C47 3.7(4) . . . . ? C49 O9 C46 C45 -176.1(3) . . . . ? O8 C45 C46 O9 -3.8(4) . . . . ? C44 C45 C46 O9 175.5(2) . . . . ? O8 C45 C46 C47 176.4(2) . . . . ? C44 C45 C46 C47 -4.2(4) . . . . ? O9 C46 C47 C42 -177.9(2) . . . . ? C45 C46 C47 C42 1.8(4) . . . . ? C43 C42 C47 C46 1.6(4) . . . . ? C41 C42 C47 C46 -175.7(2) . . . . ? #============================================================================== data_8_MeCN _database_code_depnum_ccdc_archive 'CCDC 772404' #TrackingRef '- submit_all.cif' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H41 Mn2 N6 O5 +, Cl O4 -, C2 H3 N' _chemical_formula_sum 'C40 H44 Cl Mn2 N7 O9' _chemical_formula_weight 912.15 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' 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 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8414(14) _cell_length_b 25.087(4) _cell_length_c 16.780(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.605(3) _cell_angle_gamma 90.00 _cell_volume 4072.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 11930 _cell_measurement_theta_min 3.59 _cell_measurement_theta_max 30.61 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ? _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 46988 _diffrn_reflns_av_R_equivalents 0.0947 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 30.61 _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 11930 _reflns_number_gt 7682 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0567P)^2^] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11930 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1158 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.395 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.089 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.59110(3) 0.153854(13) 0.71965(2) 0.01575(8) Uani 1 1 d . . . Mn2 Mn 0.28631(3) 0.170529(13) 0.79119(2) 0.01531(8) Uani 1 1 d . . . O1 O 0.43249(15) 0.11511(6) 0.76567(9) 0.0167(3) Uani 1 1 d . . . O2 O 0.64095(17) 0.21348(6) 0.80907(10) 0.0245(4) Uani 1 1 d . . . O3 O 0.45100(18) 0.21669(7) 0.86517(11) 0.0275(4) Uani 1 1 d . . . O4 O 0.44216(17) 0.20313(7) 0.64059(10) 0.0228(4) Uani 1 1 d . . . O5 O 0.24722(17) 0.21974(6) 0.68752(10) 0.0230(4) Uani 1 1 d . . . N1 N 0.59319(19) 0.07804(7) 0.64119(11) 0.0165(4) Uani 1 1 d . . . N2 N 0.73467(19) 0.09620(7) 0.80135(11) 0.0184(4) Uani 1 1 d . . . N3 N 0.73353(19) 0.17099(7) 0.63129(11) 0.0193(4) Uani 1 1 d . . . N4 N 0.25978(19) 0.11360(7) 0.89647(11) 0.0160(4) Uani 1 1 d . . . N5 N 0.12987(19) 0.10738(7) 0.73253(11) 0.0177(4) Uani 1 1 d . . . N6 N 0.14203(19) 0.21085(7) 0.86001(11) 0.0181(4) Uani 1 1 d . . . C1 C 0.4251(2) 0.06230(8) 0.77705(13) 0.0158(4) Uani 1 1 d . . . C2 C 0.4394(2) 0.02677(9) 0.71479(13) 0.0163(4) Uani 1 1 d . . . C3 C 0.4297(2) -0.02753(9) 0.72767(14) 0.0175(4) Uani 1 1 d . . . H3A H 0.4390 -0.0512 0.6848 0.021 Uiso 1 1 calc R . . C4 C 0.4070(2) -0.04906(9) 0.80071(14) 0.0169(4) Uani 1 1 d . . . C5 C 0.3946(2) -0.01297(9) 0.86164(13) 0.0168(4) Uani 1 1 d . . . H5A H 0.3803 -0.0262 0.9125 0.020 Uiso 1 1 calc R . . C6 C 0.4022(2) 0.04198(9) 0.85116(13) 0.0160(4) Uani 1 1 d . . . C7 C 0.3978(2) -0.10945(8) 0.81038(14) 0.0184(5) Uani 1 1 d . . . C8 C 0.5412(2) -0.13352(9) 0.80838(15) 0.0229(5) Uani 1 1 d . . . H8A H 0.6091 -0.1187 0.8530 0.034 Uiso 1 1 calc R . . H8B H 0.5685 -0.1248 0.7566 0.034 Uiso 1 1 calc R . . H8C H 0.5373 -0.1723 0.8142 0.034 Uiso 1 1 calc R . . C9 C 0.2908(3) -0.13261(9) 0.74053(15) 0.0254(5) Uani 1 1 d . . . H9A H 0.2021 -0.1144 0.7382 0.038 Uiso 1 1 calc R . . H9B H 0.2792 -0.1708 0.7497 0.038 Uiso 1 1 calc R . . H9C H 0.3230 -0.1274 0.6892 0.038 Uiso 1 1 calc R . . C10 C 0.3548(3) -0.12542(9) 0.88963(15) 0.0247(5) Uani 1 1 d . . . H10A H 0.2625 -0.1113 0.8910 0.037 Uiso 1 1 calc R . . H10B H 0.4211 -0.1109 0.9353 0.037 Uiso 1 1 calc R . . H10C H 0.3533 -0.1644 0.8937 0.037 Uiso 1 1 calc R . . C11 C 0.4611(2) 0.04806(9) 0.63452(13) 0.0178(5) Uani 1 1 d . . . H11A H 0.4612 0.0180 0.5963 0.021 Uiso 1 1 calc R . . H11B H 0.3832 0.0719 0.6121 0.021 Uiso 1 1 calc R . . C12 C 0.7122(2) 0.04451(9) 0.67838(13) 0.0195(5) Uani 1 1 d . . . H12A H 0.7958 0.0564 0.6585 0.023 Uiso 1 1 calc R . . H12B H 0.6938 0.0071 0.6611 0.023 Uiso 1 1 calc R . . C13 C 0.7391(2) 0.04713(9) 0.76955(14) 0.0186(5) Uani 1 1 d . . . C14 C 0.7731(2) 0.00236(10) 0.81706(15) 0.0236(5) Uani 1 1 d . . . H14A H 0.7741 -0.0319 0.7929 0.028 Uiso 1 1 calc R . . C15 C 0.8054(3) 0.00820(11) 0.89999(15) 0.0283(6) Uani 1 1 d . . . H15A H 0.8301 -0.0219 0.9339 0.034 Uiso 1 1 calc R . . C16 C 0.8015(3) 0.05831(11) 0.93324(15) 0.0275(6) Uani 1 1 d . . . H16A H 0.8234 0.0632 0.9903 0.033 Uiso 1 1 calc R . . C17 C 0.7653(2) 0.10113(10) 0.88240(14) 0.0239(5) Uani 1 1 d . . . H17A H 0.7620 0.1355 0.9056 0.029 Uiso 1 1 calc R . . C18 C 0.6102(2) 0.09628(9) 0.56053(13) 0.0201(5) Uani 1 1 d . . . H18A H 0.5211 0.1105 0.5311 0.024 Uiso 1 1 calc R . . H18B H 0.6364 0.0657 0.5293 0.024 Uiso 1 1 calc R . . C19 C 0.7195(2) 0.13892(9) 0.56624(13) 0.0185(5) Uani 1 1 d . . . C20 C 0.7972(3) 0.14575(10) 0.50634(15) 0.0240(5) Uani 1 1 d . . . H20A H 0.7861 0.1222 0.4612 0.029 Uiso 1 1 calc R . . C21 C 0.8916(3) 0.18726(11) 0.51270(16) 0.0289(6) Uani 1 1 d . . . H21A H 0.9449 0.1930 0.4717 0.035 Uiso 1 1 calc R . . C22 C 0.9067(3) 0.22003(10) 0.57940(16) 0.0274(6) Uani 1 1 d . . . H22A H 0.9711 0.2486 0.5856 0.033 Uiso 1 1 calc R . . C23 C 0.8266(2) 0.21051(10) 0.63714(15) 0.0232(5) Uani 1 1 d . . . H23A H 0.8378 0.2331 0.6834 0.028 Uiso 1 1 calc R . . C24 C 0.3854(2) 0.07992(9) 0.91831(13) 0.0176(5) Uani 1 1 d . . . H24A H 0.3793 0.0593 0.9678 0.021 Uiso 1 1 calc R . . H24B H 0.4678 0.1032 0.9306 0.021 Uiso 1 1 calc R . . C25 C 0.1347(2) 0.08120(9) 0.87108(14) 0.0195(5) Uani 1 1 d . . . H25A H 0.0534 0.1012 0.8821 0.023 Uiso 1 1 calc R . . H25B H 0.1427 0.0480 0.9035 0.023 Uiso 1 1 calc R . . C26 C 0.1126(2) 0.06710(9) 0.78256(14) 0.0177(5) Uani 1 1 d . . . C27 C 0.0757(2) 0.01613(9) 0.75407(15) 0.0227(5) Uani 1 1 d . . . H27A H 0.0649 -0.0117 0.7908 0.027 Uiso 1 1 calc R . . C28 C 0.0549(2) 0.00644(10) 0.67230(16) 0.0263(5) Uani 1 1 d . . . H28A H 0.0294 -0.0281 0.6517 0.032 Uiso 1 1 calc R . . C29 C 0.0717(2) 0.04769(10) 0.62032(15) 0.0256(5) Uani 1 1 d . . . H29A H 0.0576 0.0420 0.5634 0.031 Uiso 1 1 calc R . . C30 C 0.1092(2) 0.09724(10) 0.65252(14) 0.0219(5) Uani 1 1 d . . . H30A H 0.1209 0.1255 0.6166 0.026 Uiso 1 1 calc R . . C31 C 0.2453(2) 0.14898(9) 0.96440(13) 0.0194(5) Uani 1 1 d . . . H31A H 0.3372 0.1633 0.9891 0.023 Uiso 1 1 calc R . . H31B H 0.2095 0.1283 1.0063 0.023 Uiso 1 1 calc R . . C32 C 0.1484(2) 0.19455(9) 0.93633(14) 0.0181(5) Uani 1 1 d . . . C33 C 0.0738(2) 0.21998(9) 0.98782(14) 0.0227(5) Uani 1 1 d . . . H33A H 0.0796 0.2081 1.0421 0.027 Uiso 1 1 calc R . . C34 C -0.0091(3) 0.26286(9) 0.95916(15) 0.0248(5) Uani 1 1 d . . . H34A H -0.0601 0.2810 0.9937 0.030 Uiso 1 1 calc R . . C35 C -0.0171(3) 0.27899(9) 0.88053(15) 0.0239(5) Uani 1 1 d . . . H35A H -0.0742 0.3081 0.8595 0.029 Uiso 1 1 calc R . . C36 C 0.0594(2) 0.25208(9) 0.83268(14) 0.0204(5) Uani 1 1 d . . . H36A H 0.0535 0.2631 0.7780 0.025 Uiso 1 1 calc R . . C37 C 0.5718(3) 0.22899(9) 0.86024(15) 0.0236(5) Uani 1 1 d . . . H37A H 0.6170 0.2531 0.9002 0.028 Uiso 1 1 calc R . . C38 C 0.3242(2) 0.22191(9) 0.63617(14) 0.0222(5) Uani 1 1 d . . . H38A H 0.2878 0.2403 0.5874 0.027 Uiso 1 1 calc R . . Cl1 Cl 0.21112(6) 0.10290(2) 0.42295(3) 0.02243(13) Uani 1 1 d . . . O1A O 0.2230(2) 0.05066(7) 0.45841(11) 0.0352(5) Uani 1 1 d . . . O1B O 0.06774(18) 0.11497(8) 0.39299(12) 0.0372(5) Uani 1 1 d . . . O1C O 0.2858(2) 0.10438(8) 0.35710(12) 0.0399(5) Uani 1 1 d . . . O1D O 0.2671(2) 0.14215(8) 0.48237(12) 0.0422(5) Uani 1 1 d . . . N1S N 0.0196(3) 0.10156(10) 0.11387(16) 0.0430(6) Uani 1 1 d . . . C1S C 0.0457(3) 0.13392(11) 0.16153(16) 0.0291(6) Uani 1 1 d . . . C2S C 0.0786(3) 0.17603(11) 0.22092(17) 0.0381(7) Uani 1 1 d . . . H2S1 H 0.0574 0.2107 0.1946 0.057 Uiso 1 1 d R . . H2S2 H 0.1772 0.1745 0.2449 0.057 Uiso 1 1 d R . . H2S3 H 0.0236 0.1714 0.2636 0.057 Uiso 1 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 Mn1 0.01525(17) 0.01570(16) 0.01761(18) -0.00122(13) 0.00644(13) -0.00052(13) Mn2 0.01599(17) 0.01491(16) 0.01644(17) 0.00016(13) 0.00665(13) 0.00197(13) O1 0.0161(8) 0.0137(8) 0.0220(8) 0.0006(6) 0.0078(6) 0.0019(6) O2 0.0243(9) 0.0245(9) 0.0251(9) -0.0062(7) 0.0055(7) -0.0020(7) O3 0.0250(9) 0.0277(9) 0.0310(10) -0.0090(7) 0.0086(8) -0.0034(7) O4 0.0216(9) 0.0253(9) 0.0222(9) 0.0030(7) 0.0059(7) 0.0031(7) O5 0.0250(9) 0.0241(9) 0.0219(9) 0.0057(7) 0.0099(7) 0.0046(7) N1 0.0159(9) 0.0178(9) 0.0166(10) 0.0021(7) 0.0050(8) 0.0009(7) N2 0.0127(9) 0.0230(10) 0.0203(10) -0.0024(8) 0.0048(8) -0.0011(8) N3 0.0180(9) 0.0200(9) 0.0208(10) 0.0001(8) 0.0061(8) -0.0007(8) N4 0.0170(9) 0.0166(9) 0.0156(9) -0.0008(7) 0.0060(7) 0.0028(7) N5 0.0138(9) 0.0208(10) 0.0188(10) -0.0002(8) 0.0039(7) -0.0001(7) N6 0.0187(9) 0.0189(9) 0.0172(10) 0.0005(7) 0.0051(8) 0.0025(8) C1 0.0112(10) 0.0145(10) 0.0220(12) 0.0004(9) 0.0041(9) -0.0001(8) C2 0.0124(10) 0.0192(11) 0.0177(11) 0.0009(9) 0.0036(8) 0.0015(8) C3 0.0150(10) 0.0178(11) 0.0198(11) -0.0028(9) 0.0038(9) 0.0001(8) C4 0.0139(10) 0.0167(11) 0.0200(11) 0.0009(9) 0.0029(9) 0.0013(8) C5 0.0153(10) 0.0188(11) 0.0171(11) 0.0030(9) 0.0051(9) 0.0015(9) C6 0.0133(10) 0.0177(11) 0.0175(11) 0.0006(9) 0.0043(8) 0.0029(8) C7 0.0205(11) 0.0138(10) 0.0210(12) -0.0010(9) 0.0042(9) -0.0002(9) C8 0.0243(12) 0.0181(11) 0.0259(13) 0.0008(10) 0.0037(10) 0.0053(9) C9 0.0281(13) 0.0179(12) 0.0287(14) -0.0014(10) 0.0015(11) -0.0035(10) C10 0.0338(14) 0.0168(11) 0.0258(13) 0.0021(10) 0.0119(11) -0.0016(10) C11 0.0189(11) 0.0181(11) 0.0169(11) -0.0019(9) 0.0049(9) -0.0028(9) C12 0.0188(11) 0.0217(11) 0.0192(12) -0.0004(9) 0.0064(9) 0.0049(9) C13 0.0128(10) 0.0248(12) 0.0197(12) -0.0003(9) 0.0070(9) 0.0034(9) C14 0.0203(12) 0.0263(12) 0.0253(13) 0.0035(10) 0.0071(10) 0.0056(10) C15 0.0247(13) 0.0342(14) 0.0269(14) 0.0110(11) 0.0072(11) 0.0064(11) C16 0.0219(12) 0.0427(16) 0.0181(12) 0.0021(11) 0.0039(10) 0.0044(11) C17 0.0167(11) 0.0315(13) 0.0238(13) -0.0048(10) 0.0040(10) 0.0012(10) C18 0.0226(12) 0.0237(12) 0.0155(11) -0.0002(9) 0.0074(9) -0.0019(9) C19 0.0189(11) 0.0204(11) 0.0165(11) 0.0016(9) 0.0043(9) 0.0027(9) C20 0.0264(13) 0.0278(13) 0.0199(12) 0.0024(10) 0.0096(10) 0.0009(10) C21 0.0250(13) 0.0360(14) 0.0294(14) 0.0069(11) 0.0147(11) -0.0008(11) C22 0.0235(13) 0.0239(13) 0.0373(15) 0.0024(11) 0.0119(11) -0.0053(10) C23 0.0196(12) 0.0235(12) 0.0274(13) -0.0019(10) 0.0065(10) -0.0044(10) C24 0.0175(11) 0.0176(11) 0.0185(11) 0.0013(9) 0.0053(9) 0.0041(9) C25 0.0152(11) 0.0227(12) 0.0220(12) 0.0029(9) 0.0075(9) 0.0005(9) C26 0.0101(10) 0.0207(11) 0.0233(12) 0.0004(9) 0.0055(9) 0.0002(8) C27 0.0147(11) 0.0210(12) 0.0328(14) 0.0001(10) 0.0055(10) -0.0008(9) C28 0.0170(11) 0.0250(13) 0.0361(15) -0.0078(11) 0.0029(10) -0.0040(10) C29 0.0178(12) 0.0330(14) 0.0255(13) -0.0086(11) 0.0024(10) -0.0026(10) C30 0.0179(11) 0.0273(13) 0.0205(12) 0.0013(10) 0.0035(9) 0.0018(10) C31 0.0252(12) 0.0207(11) 0.0134(11) 0.0000(9) 0.0067(9) 0.0069(9) C32 0.0197(11) 0.0188(11) 0.0173(11) 0.0000(9) 0.0072(9) 0.0029(9) C33 0.0274(13) 0.0250(12) 0.0185(12) 0.0011(9) 0.0114(10) 0.0046(10) C34 0.0272(13) 0.0233(12) 0.0275(13) -0.0010(10) 0.0142(11) 0.0060(10) C35 0.0257(13) 0.0189(11) 0.0291(13) 0.0015(10) 0.0106(10) 0.0068(10) C36 0.0214(12) 0.0213(12) 0.0199(12) 0.0000(9) 0.0073(9) 0.0025(9) C37 0.0250(13) 0.0217(12) 0.0236(13) -0.0081(10) 0.0035(10) -0.0011(10) C38 0.0247(12) 0.0228(12) 0.0194(12) 0.0049(9) 0.0049(10) 0.0028(10) Cl1 0.0239(3) 0.0219(3) 0.0221(3) -0.0028(2) 0.0056(2) -0.0059(2) O1A 0.0517(12) 0.0253(10) 0.0295(10) 0.0037(8) 0.0096(9) -0.0023(9) O1B 0.0227(10) 0.0354(11) 0.0521(13) -0.0066(9) 0.0031(9) -0.0013(8) O1C 0.0470(12) 0.0404(11) 0.0396(12) 0.0052(9) 0.0274(10) -0.0008(9) O1D 0.0477(13) 0.0351(11) 0.0405(12) -0.0154(9) -0.0008(10) -0.0143(9) N1S 0.0454(15) 0.0359(14) 0.0468(16) -0.0029(12) 0.0064(13) 0.0044(12) C1S 0.0275(14) 0.0267(13) 0.0332(15) 0.0072(12) 0.0059(12) 0.0032(11) C2S 0.0494(18) 0.0292(15) 0.0332(16) 0.0039(12) 0.0011(13) 0.0005(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 Mn2 3.4553(6) . ? Mn1 O1 2.1027(15) . ? Mn1 O2 2.1115(16) . ? Mn1 O4 2.1727(16) . ? Mn1 N3 2.2612(19) . ? Mn1 N2 2.2923(19) . ? Mn1 N1 2.3154(19) . ? Mn2 O1 2.1006(15) . ? Mn2 O5 2.1100(16) . ? Mn2 O3 2.1837(17) . ? Mn2 N6 2.2308(19) . ? Mn2 N5 2.3003(19) . ? Mn2 N4 2.3234(18) . ? O1 C1 1.343(3) . ? O2 C37 1.252(3) . ? O3 C37 1.246(3) . ? O4 C38 1.242(3) . ? O5 C38 1.249(3) . ? N1 C18 1.467(3) . ? N1 C12 1.483(3) . ? N1 C11 1.488(3) . ? N2 C17 1.343(3) . ? N2 C13 1.346(3) . ? N3 C23 1.341(3) . ? N3 C19 1.343(3) . ? N4 C25 1.471(3) . ? N4 C31 1.472(3) . ? N4 C24 1.486(3) . ? N5 C26 1.345(3) . ? N5 C30 1.345(3) . ? N6 C32 1.335(3) . ? N6 C36 1.343(3) . ? C1 C2 1.400(3) . ? C1 C6 1.400(3) . ? C2 C3 1.385(3) . ? C2 C11 1.500(3) . ? C3 C4 1.394(3) . ? C3 H3A 0.950 . ? C4 C5 1.388(3) . ? C4 C7 1.528(3) . ? C5 C6 1.393(3) . ? C5 H5A 0.950 . ? C6 C24 1.507(3) . ? C7 C10 1.521(3) . ? C7 C9 1.538(3) . ? C7 C8 1.542(3) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 C13 1.505(3) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.382(3) . ? C14 C15 1.377(3) . ? C14 H14A 0.950 . ? C15 C16 1.378(4) . ? C15 H15A 0.950 . ? C16 C17 1.377(3) . ? C16 H16A 0.950 . ? C17 H17A 0.950 . ? C18 C19 1.508(3) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 C20 1.381(3) . ? C20 C21 1.387(3) . ? C20 H20A 0.950 . ? C21 C22 1.375(4) . ? C21 H21A 0.950 . ? C22 C23 1.378(3) . ? C22 H22A 0.950 . ? C23 H23A 0.950 . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 C26 1.503(3) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.390(3) . ? C27 C28 1.371(3) . ? C27 H27A 0.950 . ? C28 C29 1.383(4) . ? C28 H28A 0.950 . ? C29 C30 1.378(3) . ? C29 H29A 0.950 . ? C30 H30A 0.950 . ? C31 C32 1.508(3) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 C33 1.388(3) . ? C33 C34 1.382(3) . ? C33 H33A 0.950 . ? C34 C35 1.369(3) . ? C34 H34A 0.950 . ? C35 C36 1.374(3) . ? C35 H35A 0.950 . ? C36 H36A 0.950 . ? C37 H37A 0.950 . ? C38 H38A 0.950 . ? Cl1 O1A 1.4351(18) . ? Cl1 O1C 1.4356(18) . ? Cl1 O1D 1.4373(19) . ? Cl1 O1B 1.4403(19) . ? N1S C1S 1.135(3) . ? C1S C2S 1.448(4) . ? C2S H2S1 0.980 . ? C2S H2S2 0.980 . ? C2S H2S3 0.980 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O2 99.06(6) . . ? O1 Mn1 O4 91.39(6) . . ? O2 Mn1 O4 94.20(7) . . ? O1 Mn1 N3 156.98(7) . . ? O2 Mn1 N3 103.90(7) . . ? O4 Mn1 N3 85.49(7) . . ? O1 Mn1 N2 84.62(6) . . ? O2 Mn1 N2 89.13(7) . . ? O4 Mn1 N2 175.16(6) . . ? N3 Mn1 N2 97.12(7) . . ? O1 Mn1 N1 85.07(6) . . ? O2 Mn1 N1 163.89(7) . . ? O4 Mn1 N1 101.29(6) . . ? N3 Mn1 N1 73.26(7) . . ? N2 Mn1 N1 75.69(7) . . ? O1 Mn2 O5 104.29(6) . . ? O1 Mn2 O3 90.14(6) . . ? O5 Mn2 O3 99.32(7) . . ? O1 Mn2 N6 158.54(6) . . ? O5 Mn2 N6 97.16(7) . . ? O3 Mn2 N6 86.66(7) . . ? O1 Mn2 N5 83.48(6) . . ? O5 Mn2 N5 92.52(7) . . ? O3 Mn2 N5 167.64(7) . . ? N6 Mn2 N5 95.40(7) . . ? O1 Mn2 N4 85.71(6) . . ? O5 Mn2 N4 163.25(7) . . ? O3 Mn2 N4 93.97(7) . . ? N6 Mn2 N4 73.37(6) . . ? N5 Mn2 N4 75.05(7) . . ? C1 O1 Mn2 124.55(13) . . ? C1 O1 Mn1 124.87(13) . . ? Mn2 O1 Mn1 110.58(7) . . ? C37 O2 Mn1 128.56(15) . . ? C37 O3 Mn2 135.34(16) . . ? C38 O4 Mn1 140.37(16) . . ? C38 O5 Mn2 123.56(15) . . ? C18 N1 C12 110.48(17) . . ? C18 N1 C11 109.54(17) . . ? C12 N1 C11 110.86(17) . . ? C18 N1 Mn1 106.43(13) . . ? C12 N1 Mn1 108.40(13) . . ? C11 N1 Mn1 111.02(13) . . ? C17 N2 C13 117.9(2) . . ? C17 N2 Mn1 123.11(15) . . ? C13 N2 Mn1 113.67(15) . . ? C23 N3 C19 118.0(2) . . ? C23 N3 Mn1 126.15(16) . . ? C19 N3 Mn1 115.83(15) . . ? C25 N4 C31 111.27(17) . . ? C25 N4 C24 111.75(17) . . ? C31 N4 C24 110.26(17) . . ? C25 N4 Mn2 108.93(13) . . ? C31 N4 Mn2 104.99(13) . . ? C24 N4 Mn2 109.40(13) . . ? C26 N5 C30 117.9(2) . . ? C26 N5 Mn2 113.71(14) . . ? C30 N5 Mn2 121.60(15) . . ? C32 N6 C36 118.82(19) . . ? C32 N6 Mn2 115.82(14) . . ? C36 N6 Mn2 125.14(15) . . ? O1 C1 C2 120.44(19) . . ? O1 C1 C6 120.49(19) . . ? C2 C1 C6 119.1(2) . . ? C3 C2 C1 119.4(2) . . ? C3 C2 C11 121.0(2) . . ? C1 C2 C11 119.59(19) . . ? C2 C3 C4 123.0(2) . . ? C2 C3 H3A 118.5 . . ? C4 C3 H3A 118.5 . . ? C5 C4 C3 116.4(2) . . ? C5 C4 C7 123.6(2) . . ? C3 C4 C7 120.0(2) . . ? C4 C5 C6 122.6(2) . . ? C4 C5 H5A 118.7 . . ? C6 C5 H5A 118.7 . . ? C5 C6 C1 119.6(2) . . ? C5 C6 C24 121.0(2) . . ? C1 C6 C24 119.47(19) . . ? C10 C7 C4 112.67(18) . . ? C10 C7 C9 107.79(19) . . ? C4 C7 C9 109.85(19) . . ? C10 C7 C8 108.58(19) . . ? C4 C7 C8 108.26(18) . . ? C9 C7 C8 109.66(19) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C2 112.27(18) . . ? N1 C11 H11A 109.2 . . ? C2 C11 H11A 109.2 . . ? N1 C11 H11B 109.2 . . ? C2 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N1 C12 C13 112.37(18) . . ? N1 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? N1 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? N2 C13 C14 122.5(2) . . ? N2 C13 C12 115.5(2) . . ? C14 C13 C12 122.0(2) . . ? C15 C14 C13 118.9(2) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? C14 C15 C16 119.2(2) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? C17 C16 C15 118.9(2) . . ? C17 C16 H16A 120.5 . . ? C15 C16 H16A 120.5 . . ? N2 C17 C16 122.7(2) . . ? N2 C17 H17A 118.7 . . ? C16 C17 H17A 118.7 . . ? N1 C18 C19 111.33(18) . . ? N1 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? N1 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? N3 C19 C20 122.0(2) . . ? N3 C19 C18 116.25(19) . . ? C20 C19 C18 121.7(2) . . ? C19 C20 C21 119.3(2) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C22 C21 C20 118.8(2) . . ? C22 C21 H21A 120.6 . . ? C20 C21 H21A 120.6 . . ? C21 C22 C23 118.6(2) . . ? C21 C22 H22A 120.7 . . ? C23 C22 H22A 120.7 . . ? N3 C23 C22 123.2(2) . . ? N3 C23 H23A 118.4 . . ? C22 C23 H23A 118.4 . . ? N4 C24 C6 112.06(18) . . ? N4 C24 H24A 109.2 . . ? C6 C24 H24A 109.2 . . ? N4 C24 H24B 109.2 . . ? C6 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? N4 C25 C26 112.20(17) . . ? N4 C25 H25A 109.2 . . ? C26 C25 H25A 109.2 . . ? N4 C25 H25B 109.2 . . ? C26 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? N5 C26 C27 122.1(2) . . ? N5 C26 C25 115.35(19) . . ? C27 C26 C25 122.5(2) . . ? C28 C27 C26 119.2(2) . . ? C28 C27 H27A 120.4 . . ? C26 C27 H27A 120.4 . . ? C27 C28 C29 119.0(2) . . ? C27 C28 H28A 120.5 . . ? C29 C28 H28A 120.5 . . ? C30 C29 C28 118.8(2) . . ? C30 C29 H29A 120.6 . . ? C28 C29 H29A 120.6 . . ? N5 C30 C29 122.8(2) . . ? N5 C30 H30A 118.6 . . ? C29 C30 H30A 118.6 . . ? N4 C31 C32 111.16(18) . . ? N4 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? N4 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? N6 C32 C33 121.3(2) . . ? N6 C32 C31 116.58(19) . . ? C33 C32 C31 122.1(2) . . ? C34 C33 C32 119.2(2) . . ? C34 C33 H33A 120.4 . . ? C32 C33 H33A 120.4 . . ? C35 C34 C33 119.4(2) . . ? C35 C34 H34A 120.3 . . ? C33 C34 H34A 120.3 . . ? C34 C35 C36 118.5(2) . . ? C34 C35 H35A 120.7 . . ? C36 C35 H35A 120.7 . . ? N6 C36 C35 122.8(2) . . ? N6 C36 H36A 118.6 . . ? C35 C36 H36A 118.6 . . ? O3 C37 O2 127.9(2) . . ? O3 C37 H37A 116.0 . . ? O2 C37 H37A 116.0 . . ? O4 C38 O5 128.4(2) . . ? O4 C38 H38A 115.8 . . ? O5 C38 H38A 115.8 . . ? O1A Cl1 O1C 109.18(12) . . ? O1A Cl1 O1D 110.27(12) . . ? O1C Cl1 O1D 109.33(12) . . ? O1A Cl1 O1B 109.67(12) . . ? O1C Cl1 O1B 109.47(12) . . ? O1D Cl1 O1B 108.91(12) . . ? N1S C1S C2S 178.8(3) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.4 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Mn2 O1 C1 -133.39(16) . . . . ? O3 Mn2 O1 C1 126.95(16) . . . . ? N6 Mn2 O1 C1 45.8(3) . . . . ? N5 Mn2 O1 C1 -42.43(16) . . . . ? N4 Mn2 O1 C1 32.98(16) . . . . ? O5 Mn2 O1 Mn1 46.45(8) . . . . ? O3 Mn2 O1 Mn1 -53.21(8) . . . . ? N6 Mn2 O1 Mn1 -134.40(16) . . . . ? N5 Mn2 O1 Mn1 137.41(8) . . . . ? N4 Mn2 O1 Mn1 -147.18(8) . . . . ? O2 Mn1 O1 C1 -129.88(16) . . . . ? O4 Mn1 O1 C1 135.64(16) . . . . ? N3 Mn1 O1 C1 53.9(3) . . . . ? N2 Mn1 O1 C1 -41.63(16) . . . . ? N1 Mn1 O1 C1 34.43(16) . . . . ? O2 Mn1 O1 Mn2 50.28(8) . . . . ? O4 Mn1 O1 Mn2 -44.20(8) . . . . ? N3 Mn1 O1 Mn2 -125.92(15) . . . . ? N2 Mn1 O1 Mn2 138.54(8) . . . . ? N1 Mn1 O1 Mn2 -145.41(8) . . . . ? O1 Mn1 O2 C37 -16.5(2) . . . . ? O4 Mn1 O2 C37 75.6(2) . . . . ? N3 Mn1 O2 C37 162.0(2) . . . . ? N2 Mn1 O2 C37 -100.9(2) . . . . ? N1 Mn1 O2 C37 -120.3(3) . . . . ? O1 Mn2 O3 C37 38.6(2) . . . . ? O5 Mn2 O3 C37 -65.9(2) . . . . ? N6 Mn2 O3 C37 -162.6(2) . . . . ? N5 Mn2 O3 C37 97.3(4) . . . . ? N4 Mn2 O3 C37 124.3(2) . . . . ? O1 Mn1 O4 C38 26.6(3) . . . . ? O2 Mn1 O4 C38 -72.6(3) . . . . ? N3 Mn1 O4 C38 -176.2(3) . . . . ? N1 Mn1 O4 C38 111.8(2) . . . . ? O1 Mn2 O5 C38 -16.7(2) . . . . ? O3 Mn2 O5 C38 75.82(19) . . . . ? N6 Mn2 O5 C38 163.59(19) . . . . ? N5 Mn2 O5 C38 -100.64(19) . . . . ? N4 Mn2 O5 C38 -142.1(2) . . . . ? O1 Mn1 N1 C18 139.40(14) . . . . ? O2 Mn1 N1 C18 -114.9(2) . . . . ? O4 Mn1 N1 C18 48.97(14) . . . . ? N3 Mn1 N1 C18 -32.77(13) . . . . ? N2 Mn1 N1 C18 -134.90(14) . . . . ? O1 Mn1 N1 C12 -101.74(14) . . . . ? O2 Mn1 N1 C12 4.0(3) . . . . ? O4 Mn1 N1 C12 167.82(13) . . . . ? N3 Mn1 N1 C12 86.09(14) . . . . ? N2 Mn1 N1 C12 -16.05(13) . . . . ? O1 Mn1 N1 C11 20.26(13) . . . . ? O2 Mn1 N1 C11 126.0(2) . . . . ? O4 Mn1 N1 C11 -70.17(14) . . . . ? N3 Mn1 N1 C11 -151.91(15) . . . . ? N2 Mn1 N1 C11 105.95(14) . . . . ? O1 Mn1 N2 C17 -73.67(18) . . . . ? O2 Mn1 N2 C17 25.51(18) . . . . ? N3 Mn1 N2 C17 129.42(18) . . . . ? N1 Mn1 N2 C17 -159.94(19) . . . . ? O1 Mn1 N2 C13 79.95(15) . . . . ? O2 Mn1 N2 C13 179.13(15) . . . . ? N3 Mn1 N2 C13 -76.96(15) . . . . ? N1 Mn1 N2 C13 -6.32(14) . . . . ? O1 Mn1 N3 C23 176.14(17) . . . . ? O2 Mn1 N3 C23 0.0(2) . . . . ? O4 Mn1 N3 C23 93.23(19) . . . . ? N2 Mn1 N3 C23 -90.86(19) . . . . ? N1 Mn1 N3 C23 -163.5(2) . . . . ? O1 Mn1 N3 C19 -2.1(3) . . . . ? O2 Mn1 N3 C19 -178.24(15) . . . . ? O4 Mn1 N3 C19 -85.02(16) . . . . ? N2 Mn1 N3 C19 90.89(16) . . . . ? N1 Mn1 N3 C19 18.21(15) . . . . ? O1 Mn2 N4 C25 -100.21(13) . . . . ? O5 Mn2 N4 C25 27.4(3) . . . . ? O3 Mn2 N4 C25 169.95(13) . . . . ? N6 Mn2 N4 C25 84.63(14) . . . . ? N5 Mn2 N4 C25 -15.83(13) . . . . ? O1 Mn2 N4 C31 140.53(14) . . . . ? O5 Mn2 N4 C31 -91.9(3) . . . . ? O3 Mn2 N4 C31 50.69(14) . . . . ? N6 Mn2 N4 C31 -34.63(13) . . . . ? N5 Mn2 N4 C31 -135.09(14) . . . . ? O1 Mn2 N4 C24 22.21(13) . . . . ? O5 Mn2 N4 C24 149.8(2) . . . . ? O3 Mn2 N4 C24 -67.63(14) . . . . ? N6 Mn2 N4 C24 -152.95(15) . . . . ? N5 Mn2 N4 C24 106.60(14) . . . . ? O1 Mn2 N5 C26 80.24(15) . . . . ? O5 Mn2 N5 C26 -175.65(15) . . . . ? O3 Mn2 N5 C26 20.9(4) . . . . ? N6 Mn2 N5 C26 -78.22(15) . . . . ? N4 Mn2 N5 C26 -7.05(14) . . . . ? O1 Mn2 N5 C30 -70.27(17) . . . . ? O5 Mn2 N5 C30 33.84(17) . . . . ? O3 Mn2 N5 C30 -129.6(3) . . . . ? N6 Mn2 N5 C30 131.28(17) . . . . ? N4 Mn2 N5 C30 -157.55(18) . . . . ? O1 Mn2 N6 C32 8.4(3) . . . . ? O5 Mn2 N6 C32 -172.39(16) . . . . ? O3 Mn2 N6 C32 -73.40(17) . . . . ? N5 Mn2 N6 C32 94.37(17) . . . . ? N4 Mn2 N6 C32 21.75(16) . . . . ? O1 Mn2 N6 C36 -176.94(17) . . . . ? O5 Mn2 N6 C36 2.22(19) . . . . ? O3 Mn2 N6 C36 101.21(19) . . . . ? N5 Mn2 N6 C36 -91.02(19) . . . . ? N4 Mn2 N6 C36 -163.6(2) . . . . ? Mn2 O1 C1 C2 129.62(18) . . . . ? Mn1 O1 C1 C2 -50.2(3) . . . . ? Mn2 O1 C1 C6 -50.0(3) . . . . ? Mn1 O1 C1 C6 130.18(17) . . . . ? O1 C1 C2 C3 -179.22(19) . . . . ? C6 C1 C2 C3 0.4(3) . . . . ? O1 C1 C2 C11 -0.9(3) . . . . ? C6 C1 C2 C11 178.75(19) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C11 C2 C3 C4 -178.8(2) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? C2 C3 C4 C7 -179.9(2) . . . . ? C3 C4 C5 C6 0.8(3) . . . . ? C7 C4 C5 C6 -179.4(2) . . . . ? C4 C5 C6 C1 -0.9(3) . . . . ? C4 C5 C6 C24 178.8(2) . . . . ? O1 C1 C6 C5 179.86(19) . . . . ? C2 C1 C6 C5 0.2(3) . . . . ? O1 C1 C6 C24 0.2(3) . . . . ? C2 C1 C6 C24 -179.45(19) . . . . ? C5 C4 C7 C10 7.5(3) . . . . ? C3 C4 C7 C10 -172.7(2) . . . . ? C5 C4 C7 C9 127.7(2) . . . . ? C3 C4 C7 C9 -52.6(3) . . . . ? C5 C4 C7 C8 -112.6(2) . . . . ? C3 C4 C7 C8 67.2(3) . . . . ? C18 N1 C11 C2 178.22(18) . . . . ? C12 N1 C11 C2 56.0(2) . . . . ? Mn1 N1 C11 C2 -64.5(2) . . . . ? C3 C2 C11 N1 -118.2(2) . . . . ? C1 C2 C11 N1 63.5(3) . . . . ? C18 N1 C12 C13 151.62(19) . . . . ? C11 N1 C12 C13 -86.7(2) . . . . ? Mn1 N1 C12 C13 35.4(2) . . . . ? C17 N2 C13 C14 0.3(3) . . . . ? Mn1 N2 C13 C14 -154.78(18) . . . . ? C17 N2 C13 C12 -176.47(19) . . . . ? Mn1 N2 C13 C12 28.4(2) . . . . ? N1 C12 C13 N2 -44.4(3) . . . . ? N1 C12 C13 C14 138.8(2) . . . . ? N2 C13 C14 C15 -0.9(3) . . . . ? C12 C13 C14 C15 175.7(2) . . . . ? C13 C14 C15 C16 0.7(4) . . . . ? C14 C15 C16 C17 0.0(4) . . . . ? C13 N2 C17 C16 0.4(3) . . . . ? Mn1 N2 C17 C16 153.00(18) . . . . ? C15 C16 C17 N2 -0.6(4) . . . . ? C12 N1 C18 C19 -73.3(2) . . . . ? C11 N1 C18 C19 164.27(18) . . . . ? Mn1 N1 C18 C19 44.2(2) . . . . ? C23 N3 C19 C20 -0.2(3) . . . . ? Mn1 N3 C19 C20 178.23(17) . . . . ? C23 N3 C19 C18 -177.9(2) . . . . ? Mn1 N3 C19 C18 0.5(2) . . . . ? N1 C18 C19 N3 -31.6(3) . . . . ? N1 C18 C19 C20 150.8(2) . . . . ? N3 C19 C20 C21 -0.7(4) . . . . ? C18 C19 C20 C21 176.8(2) . . . . ? C19 C20 C21 C22 1.0(4) . . . . ? C20 C21 C22 C23 -0.4(4) . . . . ? C19 N3 C23 C22 0.8(4) . . . . ? Mn1 N3 C23 C22 -177.42(18) . . . . ? C21 C22 C23 N3 -0.5(4) . . . . ? C25 N4 C24 C6 54.2(2) . . . . ? C31 N4 C24 C6 178.50(18) . . . . ? Mn2 N4 C24 C6 -66.52(19) . . . . ? C5 C6 C24 N4 -115.2(2) . . . . ? C1 C6 C24 N4 64.4(3) . . . . ? C31 N4 C25 C26 150.76(18) . . . . ? C24 N4 C25 C26 -85.5(2) . . . . ? Mn2 N4 C25 C26 35.5(2) . . . . ? C30 N5 C26 C27 0.6(3) . . . . ? Mn2 N5 C26 C27 -151.12(17) . . . . ? C30 N5 C26 C25 -178.96(19) . . . . ? Mn2 N5 C26 C25 29.4(2) . . . . ? N4 C25 C26 N5 -45.0(3) . . . . ? N4 C25 C26 C27 135.5(2) . . . . ? N5 C26 C27 C28 -0.6(3) . . . . ? C25 C26 C27 C28 178.9(2) . . . . ? C26 C27 C28 C29 0.2(3) . . . . ? C27 C28 C29 C30 0.2(3) . . . . ? C26 N5 C30 C29 -0.2(3) . . . . ? Mn2 N5 C30 C29 149.17(18) . . . . ? C28 C29 C30 N5 -0.2(4) . . . . ? C25 N4 C31 C32 -73.3(2) . . . . ? C24 N4 C31 C32 162.12(18) . . . . ? Mn2 N4 C31 C32 44.4(2) . . . . ? C36 N6 C32 C33 -1.3(3) . . . . ? Mn2 N6 C32 C33 173.70(18) . . . . ? C36 N6 C32 C31 -178.6(2) . . . . ? Mn2 N6 C32 C31 -3.6(3) . . . . ? N4 C31 C32 N6 -29.5(3) . . . . ? N4 C31 C32 C33 153.1(2) . . . . ? N6 C32 C33 C34 0.3(4) . . . . ? C31 C32 C33 C34 177.5(2) . . . . ? C32 C33 C34 C35 0.7(4) . . . . ? C33 C34 C35 C36 -0.7(4) . . . . ? C32 N6 C36 C35 1.3(3) . . . . ? Mn2 N6 C36 C35 -173.13(18) . . . . ? C34 C35 C36 N6 -0.4(4) . . . . ? Mn2 O3 C37 O2 -5.9(4) . . . . ? Mn1 O2 C37 O3 -8.0(4) . . . . ? Mn1 O4 C38 O5 5.3(4) . . . . ? Mn2 O5 C38 O4 -11.1(4) . . . . ? #============================================================================== data_8_1.5H2O _database_code_depnum_ccdc_archive 'CCDC 772405' #TrackingRef '- submit_all.cif' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H41 Mn2 N6 O5 +, Cl O4 -, 1.5(H2 O)' _chemical_formula_sum 'C38 H44 Cl Mn2 N6 O10.50' _chemical_formula_weight 898.12 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' 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 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.5344(4) _cell_length_b 23.6857(10) _cell_length_c 17.8475(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.634(1) _cell_angle_gamma 90.00 _cell_volume 4017.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6982 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 30.24 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.746 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; The geometry of both perchlorate anions is restrained to be tetrahedral. All Cl---O distances are restrained to a common free variable, while the O...O distances are restrained to 1.633 times that free variable, all with an su of 0.01 \%A. [Refined free variable = 1.421(3)]. One solvent water molecule is included with 50% site occupancy to provide reasonable atomic displacement parameters. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 52998 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 30.51 _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 11716 _reflns_number_gt 8154 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+3.9873P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11716 _refine_ls_number_parameters 527 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1603 _refine_ls_wR_factor_gt 0.1404 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.602 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.114 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.50035(4) 0.681064(17) 0.47707(2) 0.01700(10) Uani 1 1 d . . . Mn2 Mn 0.51487(4) 0.827691(16) 0.46134(2) 0.01450(10) Uani 1 1 d . . . O1 O 0.4199(2) 0.75283(7) 0.41800(10) 0.0170(4) Uani 1 1 d . . . O2 O 0.7167(2) 0.69841(9) 0.46664(12) 0.0259(4) Uani 1 1 d . . . O3 O 0.7192(2) 0.79181(9) 0.44485(12) 0.0256(4) Uani 1 1 d . . . O4 O 0.4724(3) 0.72109(9) 0.58429(11) 0.0290(5) Uani 1 1 d . . . O5 O 0.5145(2) 0.81385(8) 0.57767(11) 0.0240(4) Uani 1 1 d . . . N1 N 0.2730(2) 0.64668(9) 0.46510(12) 0.0175(4) Uani 1 1 d . . . N2 N 0.4841(2) 0.63337(9) 0.36553(13) 0.0185(5) Uani 1 1 d . . . N3 N 0.5022(3) 0.60255(10) 0.54950(13) 0.0226(5) Uani 1 1 d . . . N4 N 0.4765(2) 0.86284(9) 0.34024(12) 0.0164(4) Uani 1 1 d . . . N5 N 0.2923(2) 0.86457(9) 0.45572(13) 0.0186(5) Uani 1 1 d . . . N6 N 0.6336(3) 0.91021(10) 0.46071(13) 0.0202(5) Uani 1 1 d . . . C1 C 0.3125(3) 0.75270(10) 0.36479(14) 0.0153(5) Uani 1 1 d . . . C2 C 0.1874(3) 0.72321(11) 0.37594(14) 0.0160(5) Uani 1 1 d . . . C3 C 0.0762(3) 0.72433(12) 0.32067(15) 0.0188(5) Uani 1 1 d . . . H3A H -0.0068 0.7038 0.3287 0.023 Uiso 1 1 calc R . . C4 C 0.0818(3) 0.75449(12) 0.25390(15) 0.0201(5) Uani 1 1 d . . . C5 C 0.2062(3) 0.78308(12) 0.24372(15) 0.0192(5) Uani 1 1 d . . . H5A H 0.2134 0.8036 0.1984 0.023 Uiso 1 1 calc R . . C6 C 0.3210(3) 0.78279(11) 0.29766(14) 0.0162(5) Uani 1 1 d . . . C7 C -0.0472(3) 0.75665(14) 0.19643(17) 0.0269(6) Uani 1 1 d . . . C8 C -0.0946(5) 0.6957(2) 0.1748(3) 0.0573(12) Uani 1 1 d . . . H8A H -0.1717 0.6972 0.1350 0.086 Uiso 1 1 calc R . . H8B H -0.1268 0.6766 0.2190 0.086 Uiso 1 1 calc R . . H8C H -0.0152 0.6748 0.1567 0.086 Uiso 1 1 calc R . . C9 C -0.1677(4) 0.7853(3) 0.2316(2) 0.0656(15) Uani 1 1 d . . . H9A H -0.1444 0.8251 0.2411 0.098 Uiso 1 1 calc R . . H9B H -0.1838 0.7666 0.2791 0.098 Uiso 1 1 calc R . . H9C H -0.2531 0.7827 0.1973 0.098 Uiso 1 1 calc R . . C10 C -0.0179(5) 0.7870(2) 0.1245(2) 0.0596(13) Uani 1 1 d . . . H10A H 0.0052 0.8265 0.1357 0.089 Uiso 1 1 calc R . . H10B H -0.1014 0.7851 0.0888 0.089 Uiso 1 1 calc R . . H10C H 0.0616 0.7688 0.1024 0.089 Uiso 1 1 calc R . . C11 C 0.1729(3) 0.69427(11) 0.44991(15) 0.0185(5) Uani 1 1 d . . . H11A H 0.1879 0.7224 0.4908 0.022 Uiso 1 1 calc R . . H11B H 0.0756 0.6798 0.4507 0.022 Uiso 1 1 calc R . . C12 C 0.2577(3) 0.60391(11) 0.40467(15) 0.0207(5) Uani 1 1 d . . . H12A H 0.1592 0.6039 0.3824 0.025 Uiso 1 1 calc R . . H12B H 0.2780 0.5661 0.4266 0.025 Uiso 1 1 calc R . . C13 C 0.3547(3) 0.61468(11) 0.34345(15) 0.0180(5) Uani 1 1 d . . . C14 C 0.3144(3) 0.60163(12) 0.26851(15) 0.0220(6) Uani 1 1 d . . . H14A H 0.2211 0.5896 0.2539 0.026 Uiso 1 1 calc R . . C15 C 0.4129(3) 0.60652(12) 0.21586(16) 0.0250(6) Uani 1 1 d . . . H15A H 0.3883 0.5977 0.1645 0.030 Uiso 1 1 calc R . . C16 C 0.5479(3) 0.62439(12) 0.23907(16) 0.0232(6) Uani 1 1 d . . . H16A H 0.6180 0.6271 0.2043 0.028 Uiso 1 1 calc R . . C17 C 0.5785(3) 0.63811(12) 0.31342(16) 0.0208(5) Uani 1 1 d . . . H17A H 0.6702 0.6515 0.3288 0.025 Uiso 1 1 calc R . . C18 C 0.2497(3) 0.62093(12) 0.53815(16) 0.0242(6) Uani 1 1 d . . . H18A H 0.1658 0.5962 0.5322 0.029 Uiso 1 1 calc R . . H18B H 0.2306 0.6511 0.5744 0.029 Uiso 1 1 calc R . . C19 C 0.3750(3) 0.58670(12) 0.56911(15) 0.0235(6) Uani 1 1 d . . . C20 C 0.3575(4) 0.54276(13) 0.61940(17) 0.0305(7) Uani 1 1 d . . . H20A H 0.2661 0.5314 0.6308 0.037 Uiso 1 1 calc R . . C21 C 0.4759(4) 0.51595(13) 0.65245(18) 0.0342(8) Uani 1 1 d . . . H21A H 0.4670 0.4864 0.6878 0.041 Uiso 1 1 calc R . . C22 C 0.6074(4) 0.53274(13) 0.63325(18) 0.0328(8) Uani 1 1 d . . . H22A H 0.6901 0.5153 0.6556 0.039 Uiso 1 1 calc R . . C23 C 0.6163(4) 0.57566(12) 0.58058(17) 0.0284(7) Uani 1 1 d . . . H23A H 0.7064 0.5863 0.5661 0.034 Uiso 1 1 calc R . . C24 C 0.4527(3) 0.81571(11) 0.28561(14) 0.0177(5) Uani 1 1 d . . . H24A H 0.5346 0.7899 0.2905 0.021 Uiso 1 1 calc R . . H24B H 0.4454 0.8312 0.2339 0.021 Uiso 1 1 calc R . . C25 C 0.3553(3) 0.90218(11) 0.33668(16) 0.0205(5) Uani 1 1 d . . . H25A H 0.3133 0.9045 0.2842 0.025 Uiso 1 1 calc R . . H25B H 0.3887 0.9403 0.3521 0.025 Uiso 1 1 calc R . . C26 C 0.2443(3) 0.88312(11) 0.38718(16) 0.0192(5) Uani 1 1 d . . . C27 C 0.1015(3) 0.88690(12) 0.36501(18) 0.0244(6) Uani 1 1 d . . . H27A H 0.0701 0.9010 0.3167 0.029 Uiso 1 1 calc R . . C28 C 0.0060(3) 0.86967(13) 0.41468(19) 0.0280(7) Uani 1 1 d . . . H28A H -0.0921 0.8707 0.4003 0.034 Uiso 1 1 calc R . . C29 C 0.0544(3) 0.85102(13) 0.48517(18) 0.0272(6) Uani 1 1 d . . . H29A H -0.0098 0.8398 0.5204 0.033 Uiso 1 1 calc R . . C30 C 0.1969(3) 0.84890(12) 0.50368(17) 0.0231(6) Uani 1 1 d . . . H30A H 0.2298 0.8359 0.5523 0.028 Uiso 1 1 calc R . . C31 C 0.6067(3) 0.89352(12) 0.32571(15) 0.0204(5) Uani 1 1 d . . . H31A H 0.5876 0.9184 0.2815 0.024 Uiso 1 1 calc R . . H31B H 0.6798 0.8660 0.3138 0.024 Uiso 1 1 calc R . . C32 C 0.6615(3) 0.92881(11) 0.39248(16) 0.0197(5) Uani 1 1 d . . . C33 C 0.7477(3) 0.97533(12) 0.38320(18) 0.0260(6) Uani 1 1 d . . . H33A H 0.7642 0.9882 0.3343 0.031 Uiso 1 1 calc R . . C34 C 0.8089(4) 1.00255(13) 0.4464(2) 0.0323(7) Uani 1 1 d . . . H34A H 0.8692 1.0340 0.4414 0.039 Uiso 1 1 calc R . . C35 C 0.7811(4) 0.98324(13) 0.5165(2) 0.0323(7) Uani 1 1 d . . . H35A H 0.8221 1.0011 0.5607 0.039 Uiso 1 1 calc R . . C36 C 0.6922(3) 0.93748(13) 0.52149(18) 0.0274(6) Uani 1 1 d . . . H36A H 0.6718 0.9248 0.5699 0.033 Uiso 1 1 calc R . . C37 C 0.7738(3) 0.74423(12) 0.45033(16) 0.0218(6) Uani 1 1 d . . . H37A H 0.8704 0.7422 0.4411 0.026 Uiso 1 1 calc R . . C38 C 0.4862(3) 0.76933(12) 0.61125(15) 0.0235(6) Uani 1 1 d . . . H38A H 0.4738 0.7729 0.6633 0.028 Uiso 1 1 calc R . . Cl1 Cl 0.07982(10) 0.46736(4) 0.75267(5) 0.0413(2) Uani 1 1 d D . . O1A O 0.0866(3) 0.42198(12) 0.70022(15) 0.0526(8) Uani 1 1 d D . . O1B O 0.2161(3) 0.48326(13) 0.78102(18) 0.0564(8) Uani 1 1 d D . . O1C O 0.0014(4) 0.45048(18) 0.81298(19) 0.0834(13) Uani 1 1 d D . . O1D O 0.0109(6) 0.51443(19) 0.7154(2) 0.137(3) Uani 1 1 d D . . O1W O 0.1120(5) 0.4025(2) 0.5374(4) 0.132(2) Uani 1 1 d . . . H1W H 0.1040 0.4083 0.5839 0.197 Uiso 1 1 d R . . H2W H 0.1620 0.3729 0.5355 0.197 Uiso 1 1 d R . . O2W O 0.0491(10) 0.4935(4) 0.4531(5) 0.104(3) Uani 0.50 1 d P . . H3W H 0.0701 0.4647 0.4801 0.156 Uiso 0.50 1 d PR . . H4W H 0.0322 0.4913 0.4057 0.156 Uiso 0.50 1 d PR . . 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 0.0220(2) 0.01340(18) 0.01524(19) 0.00054(14) -0.00082(15) 0.00123(15) Mn2 0.0157(2) 0.01348(18) 0.01430(18) 0.00113(14) 0.00073(14) -0.00051(14) O1 0.0187(9) 0.0145(8) 0.0173(9) 0.0007(7) -0.0023(7) 0.0005(7) O2 0.0213(11) 0.0260(11) 0.0293(11) 0.0020(9) -0.0052(8) 0.0014(8) O3 0.0192(10) 0.0248(10) 0.0330(11) 0.0012(9) 0.0034(9) 0.0021(8) O4 0.0497(14) 0.0186(10) 0.0185(10) -0.0015(8) 0.0022(9) 0.0000(9) O5 0.0332(12) 0.0215(10) 0.0172(9) 0.0004(7) 0.0022(8) -0.0029(8) N1 0.0232(12) 0.0135(10) 0.0162(10) 0.0007(8) 0.0046(9) 0.0012(9) N2 0.0219(12) 0.0150(10) 0.0188(11) -0.0010(8) 0.0022(9) 0.0002(9) N3 0.0343(14) 0.0152(11) 0.0181(11) -0.0002(8) 0.0007(10) 0.0032(10) N4 0.0147(11) 0.0160(10) 0.0186(11) 0.0023(8) 0.0016(8) -0.0010(8) N5 0.0179(11) 0.0146(10) 0.0237(11) -0.0023(9) 0.0045(9) 0.0002(8) N6 0.0209(12) 0.0178(11) 0.0218(11) -0.0001(9) 0.0018(9) -0.0018(9) C1 0.0177(13) 0.0150(11) 0.0134(11) -0.0020(9) 0.0009(10) 0.0027(9) C2 0.0172(13) 0.0153(12) 0.0161(12) 0.0002(9) 0.0046(10) 0.0012(9) C3 0.0140(13) 0.0218(13) 0.0212(13) -0.0010(10) 0.0045(10) -0.0007(10) C4 0.0165(13) 0.0288(14) 0.0147(12) -0.0021(10) -0.0008(10) -0.0010(11) C5 0.0168(13) 0.0252(13) 0.0160(12) 0.0020(10) 0.0028(10) -0.0012(10) C6 0.0149(12) 0.0189(12) 0.0151(11) 0.0007(9) 0.0023(9) 0.0009(10) C7 0.0155(14) 0.0456(19) 0.0190(13) 0.0021(12) -0.0022(11) -0.0039(12) C8 0.052(3) 0.071(3) 0.046(2) -0.008(2) -0.013(2) -0.017(2) C9 0.030(2) 0.129(5) 0.037(2) -0.002(3) -0.0006(17) 0.023(3) C10 0.040(2) 0.105(4) 0.032(2) 0.015(2) -0.0091(17) -0.018(2) C11 0.0187(13) 0.0179(12) 0.0195(12) 0.0010(10) 0.0053(10) 0.0012(10) C12 0.0233(14) 0.0168(12) 0.0222(13) -0.0025(10) 0.0040(11) -0.0018(10) C13 0.0231(14) 0.0112(11) 0.0195(12) -0.0004(9) -0.0002(10) -0.0003(10) C14 0.0270(15) 0.0176(12) 0.0207(13) 0.0017(10) -0.0022(11) -0.0018(11) C15 0.0387(18) 0.0211(13) 0.0150(12) 0.0005(10) 0.0002(12) -0.0021(12) C16 0.0304(16) 0.0205(13) 0.0193(13) 0.0020(10) 0.0066(11) -0.0007(11) C17 0.0215(14) 0.0191(13) 0.0219(13) -0.0007(10) 0.0033(11) -0.0003(10) C18 0.0309(16) 0.0223(14) 0.0204(13) 0.0063(11) 0.0089(12) 0.0014(12) C19 0.0377(17) 0.0162(12) 0.0169(13) -0.0003(10) 0.0035(12) 0.0032(12) C20 0.048(2) 0.0200(14) 0.0244(15) 0.0044(11) 0.0051(14) -0.0011(13) C21 0.060(2) 0.0184(14) 0.0248(15) 0.0029(11) 0.0037(15) 0.0081(14) C22 0.052(2) 0.0203(14) 0.0254(15) 0.0000(12) -0.0036(14) 0.0156(14) C23 0.0399(18) 0.0201(14) 0.0247(14) -0.0006(11) -0.0004(13) 0.0037(13) C24 0.0170(13) 0.0224(13) 0.0136(11) 0.0002(10) 0.0018(9) -0.0010(10) C25 0.0173(13) 0.0182(12) 0.0255(14) 0.0068(10) -0.0007(11) 0.0007(10) C26 0.0197(14) 0.0124(11) 0.0256(13) 0.0010(10) 0.0037(11) 0.0016(10) C27 0.0203(14) 0.0196(13) 0.0332(15) 0.0028(11) 0.0010(12) 0.0050(11) C28 0.0152(14) 0.0272(15) 0.0419(18) -0.0003(13) 0.0030(12) 0.0034(11) C29 0.0221(15) 0.0275(15) 0.0334(16) -0.0036(12) 0.0102(12) -0.0019(12) C30 0.0232(15) 0.0241(14) 0.0230(14) -0.0030(11) 0.0073(11) -0.0015(11) C31 0.0175(13) 0.0243(13) 0.0197(13) 0.0052(10) 0.0032(10) -0.0046(10) C32 0.0163(13) 0.0159(12) 0.0269(14) 0.0031(10) 0.0012(10) 0.0010(10) C33 0.0241(15) 0.0173(13) 0.0367(17) 0.0046(12) 0.0037(12) -0.0022(11) C34 0.0294(17) 0.0180(14) 0.050(2) -0.0036(13) 0.0047(15) -0.0070(12) C35 0.0342(18) 0.0229(15) 0.0394(18) -0.0093(13) 0.0014(14) -0.0056(13) C36 0.0297(17) 0.0246(14) 0.0282(15) -0.0052(12) 0.0028(12) -0.0036(12) C37 0.0177(13) 0.0270(14) 0.0205(13) -0.0030(11) 0.0010(11) 0.0008(11) C38 0.0332(16) 0.0228(13) 0.0145(12) -0.0008(10) 0.0019(11) 0.0019(12) Cl1 0.0349(5) 0.0486(5) 0.0405(5) -0.0211(4) 0.0031(4) -0.0015(4) O1A 0.0623(19) 0.0506(17) 0.0454(16) -0.0274(13) 0.0078(14) -0.0075(14) O1B 0.0396(16) 0.0608(19) 0.070(2) -0.0237(16) 0.0085(14) -0.0237(14) O1C 0.057(2) 0.129(3) 0.069(2) -0.046(2) 0.0355(18) -0.043(2) O1D 0.212(6) 0.102(4) 0.086(3) -0.033(3) -0.058(4) 0.100(4) O1W 0.106(4) 0.092(4) 0.205(6) 0.001(4) 0.064(4) 0.016(3) O2W 0.133(8) 0.087(6) 0.086(6) 0.052(5) -0.027(5) -0.037(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 Mn1 Mn2 3.4879(6) . ? Mn1 O1 2.1114(18) . ? Mn1 O2 2.126(2) . ? Mn1 O4 2.171(2) . ? Mn1 N3 2.264(2) . ? Mn1 N2 2.283(2) . ? Mn1 N1 2.309(2) . ? Mn2 O5 2.102(2) . ? Mn2 O1 2.1091(19) . ? Mn2 O3 2.167(2) . ? Mn2 N6 2.259(2) . ? Mn2 N5 2.290(2) . ? Mn2 N4 2.317(2) . ? O1 C1 1.339(3) . ? O2 C37 1.259(4) . ? O3 C37 1.242(3) . ? O4 C38 1.243(4) . ? O5 C38 1.253(3) . ? N1 C18 1.472(3) . ? N1 C12 1.478(3) . ? N1 C11 1.488(3) . ? N2 C13 1.340(4) . ? N2 C17 1.350(4) . ? N3 C23 1.342(4) . ? N3 C19 1.343(4) . ? N4 C31 1.479(3) . ? N4 C25 1.482(3) . ? N4 C24 1.487(3) . ? N5 C26 1.345(4) . ? N5 C30 1.350(4) . ? N6 C32 1.342(4) . ? N6 C36 1.345(4) . ? C1 C6 1.402(4) . ? C1 C2 1.410(4) . ? C2 C3 1.388(4) . ? C2 C11 1.504(4) . ? C3 C4 1.394(4) . ? C3 H3A 0.950 . ? C4 C5 1.390(4) . ? C4 C7 1.537(4) . ? C5 C6 1.399(4) . ? C5 H5A 0.950 . ? C6 C24 1.508(4) . ? C7 C9 1.514(5) . ? C7 C10 1.517(5) . ? C7 C8 1.553(5) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 C13 1.509(4) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.396(4) . ? C14 C15 1.387(4) . ? C14 H14A 0.950 . ? C15 C16 1.386(4) . ? C15 H15A 0.950 . ? C16 C17 1.374(4) . ? C16 H16A 0.950 . ? C17 H17A 0.950 . ? C18 C19 1.511(4) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 C20 1.393(4) . ? C20 C21 1.384(5) . ? C20 H20A 0.950 . ? C21 C22 1.385(5) . ? C21 H21A 0.950 . ? C22 C23 1.392(4) . ? C22 H22A 0.950 . ? C23 H23A 0.950 . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 C26 1.514(4) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.390(4) . ? C27 C28 1.382(4) . ? C27 H27A 0.950 . ? C28 C29 1.377(5) . ? C28 H28A 0.950 . ? C29 C30 1.373(4) . ? C29 H29A 0.950 . ? C30 H30A 0.950 . ? C31 C32 1.514(4) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 C33 1.392(4) . ? C33 C34 1.386(5) . ? C33 H33A 0.950 . ? C34 C35 1.379(5) . ? C34 H34A 0.950 . ? C35 C36 1.383(4) . ? C35 H35A 0.950 . ? C36 H36A 0.950 . ? C37 H37A 0.950 . ? C38 H38A 0.950 . ? Cl1 O1B 1.407(3) . ? Cl1 O1C 1.417(3) . ? Cl1 O1A 1.430(2) . ? Cl1 O1D 1.431(4) . ? O1W H1W 0.850 . ? O1W H2W 0.850 . ? O2W H3W 0.850 . ? O2W H4W 0.850 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O2 96.69(8) . . ? O1 Mn1 O4 91.33(8) . . ? O2 Mn1 O4 100.47(9) . . ? O1 Mn1 N3 158.76(9) . . ? O2 Mn1 N3 104.23(9) . . ? O4 Mn1 N3 81.44(8) . . ? O1 Mn1 N2 88.09(8) . . ? O2 Mn1 N2 90.99(8) . . ? O4 Mn1 N2 168.52(9) . . ? N3 Mn1 N2 95.07(8) . . ? O1 Mn1 N1 86.41(8) . . ? O2 Mn1 N1 165.96(8) . . ? O4 Mn1 N1 93.12(9) . . ? N3 Mn1 N1 74.16(9) . . ? N2 Mn1 N1 75.39(8) . . ? O5 Mn2 O1 101.32(8) . . ? O5 Mn2 O3 98.40(8) . . ? O1 Mn2 O3 89.11(8) . . ? O5 Mn2 N6 100.40(8) . . ? O1 Mn2 N6 157.80(8) . . ? O3 Mn2 N6 83.23(8) . . ? O5 Mn2 N5 91.56(8) . . ? O1 Mn2 N5 86.32(8) . . ? O3 Mn2 N5 169.69(8) . . ? N6 Mn2 N5 97.64(8) . . ? O5 Mn2 N4 164.67(8) . . ? O1 Mn2 N4 85.95(8) . . ? O3 Mn2 N4 95.16(8) . . ? N6 Mn2 N4 74.10(8) . . ? N5 Mn2 N4 75.31(8) . . ? C1 O1 Mn2 122.88(15) . . ? C1 O1 Mn1 125.32(15) . . ? Mn2 O1 Mn1 111.47(9) . . ? C37 O2 Mn1 128.84(19) . . ? C37 O3 Mn2 136.1(2) . . ? C38 O4 Mn1 136.56(19) . . ? C38 O5 Mn2 128.39(18) . . ? C18 N1 C12 110.4(2) . . ? C18 N1 C11 109.5(2) . . ? C12 N1 C11 111.2(2) . . ? C18 N1 Mn1 105.79(18) . . ? C12 N1 Mn1 110.23(16) . . ? C11 N1 Mn1 109.48(16) . . ? C13 N2 C17 118.3(2) . . ? C13 N2 Mn1 114.58(17) . . ? C17 N2 Mn1 123.88(19) . . ? C23 N3 C19 118.6(3) . . ? C23 N3 Mn1 126.5(2) . . ? C19 N3 Mn1 114.40(19) . . ? C31 N4 C25 110.2(2) . . ? C31 N4 C24 109.9(2) . . ? C25 N4 C24 111.5(2) . . ? C31 N4 Mn2 105.59(16) . . ? C25 N4 Mn2 109.24(16) . . ? C24 N4 Mn2 110.24(15) . . ? C26 N5 C30 118.0(2) . . ? C26 N5 Mn2 114.23(17) . . ? C30 N5 Mn2 122.46(19) . . ? C32 N6 C36 118.3(3) . . ? C32 N6 Mn2 115.12(18) . . ? C36 N6 Mn2 126.0(2) . . ? O1 C1 C6 120.7(2) . . ? O1 C1 C2 120.5(2) . . ? C6 C1 C2 118.7(2) . . ? C3 C2 C1 119.7(2) . . ? C3 C2 C11 120.9(2) . . ? C1 C2 C11 119.2(2) . . ? C2 C3 C4 122.5(3) . . ? C2 C3 H3A 118.7 . . ? C4 C3 H3A 118.7 . . ? C5 C4 C3 116.9(3) . . ? C5 C4 C7 122.8(3) . . ? C3 C4 C7 120.2(3) . . ? C4 C5 C6 122.4(2) . . ? C4 C5 H5A 118.8 . . ? C6 C5 H5A 118.8 . . ? C5 C6 C1 119.6(2) . . ? C5 C6 C24 120.9(2) . . ? C1 C6 C24 119.4(2) . . ? C9 C7 C10 109.7(4) . . ? C9 C7 C4 109.4(3) . . ? C10 C7 C4 112.9(3) . . ? C9 C7 C8 107.7(4) . . ? C10 C7 C8 107.4(3) . . ? C4 C7 C8 109.7(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C2 113.7(2) . . ? N1 C11 H11A 108.8 . . ? C2 C11 H11A 108.8 . . ? N1 C11 H11B 108.8 . . ? C2 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? N1 C12 C13 112.5(2) . . ? N1 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? N1 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? N2 C13 C14 122.1(3) . . ? N2 C13 C12 116.5(2) . . ? C14 C13 C12 121.2(3) . . ? C15 C14 C13 118.8(3) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? C16 C15 C14 119.1(3) . . ? C16 C15 H15A 120.4 . . ? C14 C15 H15A 120.4 . . ? C17 C16 C15 118.7(3) . . ? C17 C16 H16A 120.7 . . ? C15 C16 H16A 120.7 . . ? N2 C17 C16 123.0(3) . . ? N2 C17 H17A 118.5 . . ? C16 C17 H17A 118.5 . . ? N1 C18 C19 112.0(2) . . ? N1 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? N1 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N3 C19 C20 122.3(3) . . ? N3 C19 C18 117.3(2) . . ? C20 C19 C18 120.3(3) . . ? C21 C20 C19 118.8(3) . . ? C21 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? C20 C21 C22 119.1(3) . . ? C20 C21 H21A 120.5 . . ? C22 C21 H21A 120.5 . . ? C21 C22 C23 118.9(3) . . ? C21 C22 H22A 120.6 . . ? C23 C22 H22A 120.6 . . ? N3 C23 C22 122.3(3) . . ? N3 C23 H23A 118.9 . . ? C22 C23 H23A 118.9 . . ? N4 C24 C6 112.3(2) . . ? N4 C24 H24A 109.1 . . ? C6 C24 H24A 109.1 . . ? N4 C24 H24B 109.1 . . ? C6 C24 H24B 109.1 . . ? H24A C24 H24B 107.9 . . ? N4 C25 C26 111.6(2) . . ? N4 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? N4 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? N5 C26 C27 122.2(3) . . ? N5 C26 C25 115.9(2) . . ? C27 C26 C25 121.8(3) . . ? C28 C27 C26 118.6(3) . . ? C28 C27 H27A 120.7 . . ? C26 C27 H27A 120.7 . . ? C29 C28 C27 119.4(3) . . ? C29 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? C30 C29 C28 118.9(3) . . ? C30 C29 H29A 120.6 . . ? C28 C29 H29A 120.6 . . ? N5 C30 C29 122.8(3) . . ? N5 C30 H30A 118.6 . . ? C29 C30 H30A 118.6 . . ? N4 C31 C32 112.0(2) . . ? N4 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? N4 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? N6 C32 C33 122.0(3) . . ? N6 C32 C31 116.9(2) . . ? C33 C32 C31 120.9(3) . . ? C34 C33 C32 119.0(3) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? C35 C34 C33 119.0(3) . . ? C35 C34 H34A 120.5 . . ? C33 C34 H34A 120.5 . . ? C34 C35 C36 118.8(3) . . ? C34 C35 H35A 120.6 . . ? C36 C35 H35A 120.6 . . ? N6 C36 C35 122.8(3) . . ? N6 C36 H36A 118.6 . . ? C35 C36 H36A 118.6 . . ? O3 C37 O2 128.0(3) . . ? O3 C37 H37A 116.0 . . ? O2 C37 H37A 116.0 . . ? O4 C38 O5 127.5(3) . . ? O4 C38 H38A 116.2 . . ? O5 C38 H38A 116.2 . . ? O1B Cl1 O1C 109.3(2) . . ? O1B Cl1 O1A 110.33(18) . . ? O1C Cl1 O1A 109.8(2) . . ? O1B Cl1 O1D 109.6(3) . . ? O1C Cl1 O1D 108.8(3) . . ? O1A Cl1 O1D 108.9(2) . . ? H1W O1W H2W 105.4 . . ? H3W O2W H4W 122.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Mn2 O1 C1 130.18(19) . . . . ? O3 Mn2 O1 C1 -131.4(2) . . . . ? N6 Mn2 O1 C1 -61.9(3) . . . . ? N5 Mn2 O1 C1 39.32(19) . . . . ? N4 Mn2 O1 C1 -36.19(19) . . . . ? O5 Mn2 O1 Mn1 -43.59(11) . . . . ? O3 Mn2 O1 Mn1 54.80(10) . . . . ? N6 Mn2 O1 Mn1 124.3(2) . . . . ? N5 Mn2 O1 Mn1 -134.45(10) . . . . ? N4 Mn2 O1 Mn1 150.04(10) . . . . ? O2 Mn1 O1 C1 134.0(2) . . . . ? O4 Mn1 O1 C1 -125.3(2) . . . . ? N3 Mn1 O1 C1 -55.9(3) . . . . ? N2 Mn1 O1 C1 43.2(2) . . . . ? N1 Mn1 O1 C1 -32.3(2) . . . . ? O2 Mn1 O1 Mn2 -52.43(10) . . . . ? O4 Mn1 O1 Mn2 48.28(10) . . . . ? N3 Mn1 O1 Mn2 117.7(2) . . . . ? N2 Mn1 O1 Mn2 -143.19(10) . . . . ? N1 Mn1 O1 Mn2 141.33(10) . . . . ? O1 Mn1 O2 C37 17.8(2) . . . . ? O4 Mn1 O2 C37 -74.8(2) . . . . ? N3 Mn1 O2 C37 -158.5(2) . . . . ? N2 Mn1 O2 C37 106.0(2) . . . . ? N1 Mn1 O2 C37 119.9(4) . . . . ? O5 Mn2 O3 C37 64.9(3) . . . . ? O1 Mn2 O3 C37 -36.4(3) . . . . ? N6 Mn2 O3 C37 164.5(3) . . . . ? N5 Mn2 O3 C37 -100.0(5) . . . . ? N4 Mn2 O3 C37 -122.2(3) . . . . ? O1 Mn1 O4 C38 -38.1(3) . . . . ? O2 Mn1 O4 C38 59.0(3) . . . . ? N3 Mn1 O4 C38 162.0(3) . . . . ? N2 Mn1 O4 C38 -125.0(4) . . . . ? N1 Mn1 O4 C38 -124.6(3) . . . . ? O1 Mn2 O5 C38 10.1(3) . . . . ? O3 Mn2 O5 C38 -80.7(3) . . . . ? N6 Mn2 O5 C38 -165.3(3) . . . . ? N5 Mn2 O5 C38 96.6(3) . . . . ? N4 Mn2 O5 C38 127.3(3) . . . . ? O1 Mn1 N1 C18 -138.36(17) . . . . ? O2 Mn1 N1 C18 118.3(3) . . . . ? O4 Mn1 N1 C18 -47.23(17) . . . . ? N3 Mn1 N1 C18 32.96(16) . . . . ? N2 Mn1 N1 C18 132.68(18) . . . . ? O1 Mn1 N1 C12 102.24(17) . . . . ? O2 Mn1 N1 C12 -1.1(4) . . . . ? O4 Mn1 N1 C12 -166.62(17) . . . . ? N3 Mn1 N1 C12 -86.43(17) . . . . ? N2 Mn1 N1 C12 13.28(16) . . . . ? O1 Mn1 N1 C11 -20.42(16) . . . . ? O2 Mn1 N1 C11 -123.8(3) . . . . ? O4 Mn1 N1 C11 70.71(16) . . . . ? N3 Mn1 N1 C11 150.90(17) . . . . ? N2 Mn1 N1 C11 -109.38(17) . . . . ? O1 Mn1 N2 C13 -80.14(19) . . . . ? O2 Mn1 N2 C13 -176.81(19) . . . . ? O4 Mn1 N2 C13 7.1(5) . . . . ? N3 Mn1 N2 C13 78.81(19) . . . . ? N1 Mn1 N2 C13 6.65(18) . . . . ? O1 Mn1 N2 C17 79.1(2) . . . . ? O2 Mn1 N2 C17 -17.6(2) . . . . ? O4 Mn1 N2 C17 166.4(4) . . . . ? N3 Mn1 N2 C17 -122.0(2) . . . . ? N1 Mn1 N2 C17 165.9(2) . . . . ? O1 Mn1 N3 C23 -167.3(2) . . . . ? O2 Mn1 N3 C23 2.6(2) . . . . ? O4 Mn1 N3 C23 -96.1(2) . . . . ? N2 Mn1 N3 C23 94.9(2) . . . . ? N1 Mn1 N3 C23 168.2(2) . . . . ? O1 Mn1 N3 C19 4.4(3) . . . . ? O2 Mn1 N3 C19 174.32(19) . . . . ? O4 Mn1 N3 C19 75.6(2) . . . . ? N2 Mn1 N3 C19 -93.4(2) . . . . ? N1 Mn1 N3 C19 -20.13(19) . . . . ? O5 Mn2 N4 C31 103.4(3) . . . . ? O1 Mn2 N4 C31 -137.57(17) . . . . ? O3 Mn2 N4 C31 -48.83(17) . . . . ? N6 Mn2 N4 C31 32.61(16) . . . . ? N5 Mn2 N4 C31 135.17(18) . . . . ? O5 Mn2 N4 C25 -15.2(4) . . . . ? O1 Mn2 N4 C25 103.90(17) . . . . ? O3 Mn2 N4 C25 -167.36(17) . . . . ? N6 Mn2 N4 C25 -85.92(17) . . . . ? N5 Mn2 N4 C25 16.64(16) . . . . ? O5 Mn2 N4 C24 -138.0(3) . . . . ? O1 Mn2 N4 C24 -18.96(17) . . . . ? O3 Mn2 N4 C24 69.77(17) . . . . ? N6 Mn2 N4 C24 151.21(18) . . . . ? N5 Mn2 N4 C24 -106.22(17) . . . . ? O5 Mn2 N5 C26 177.42(19) . . . . ? O1 Mn2 N5 C26 -81.34(19) . . . . ? O3 Mn2 N5 C26 -17.4(6) . . . . ? N6 Mn2 N5 C26 76.71(19) . . . . ? N4 Mn2 N5 C26 5.43(18) . . . . ? O5 Mn2 N5 C30 -28.9(2) . . . . ? O1 Mn2 N5 C30 72.4(2) . . . . ? O3 Mn2 N5 C30 136.2(4) . . . . ? N6 Mn2 N5 C30 -129.6(2) . . . . ? N4 Mn2 N5 C30 159.1(2) . . . . ? O5 Mn2 N6 C32 175.1(2) . . . . ? O1 Mn2 N6 C32 7.2(4) . . . . ? O3 Mn2 N6 C32 77.8(2) . . . . ? N5 Mn2 N6 C32 -91.9(2) . . . . ? N4 Mn2 N6 C32 -19.58(19) . . . . ? O5 Mn2 N6 C36 3.9(3) . . . . ? O1 Mn2 N6 C36 -164.0(2) . . . . ? O3 Mn2 N6 C36 -93.4(2) . . . . ? N5 Mn2 N6 C36 97.0(2) . . . . ? N4 Mn2 N6 C36 169.2(3) . . . . ? Mn2 O1 C1 C6 52.0(3) . . . . ? Mn1 O1 C1 C6 -135.1(2) . . . . ? Mn2 O1 C1 C2 -126.6(2) . . . . ? Mn1 O1 C1 C2 46.3(3) . . . . ? O1 C1 C2 C3 178.9(2) . . . . ? C6 C1 C2 C3 0.2(4) . . . . ? O1 C1 C2 C11 3.1(4) . . . . ? C6 C1 C2 C11 -175.6(2) . . . . ? C1 C2 C3 C4 -1.0(4) . . . . ? C11 C2 C3 C4 174.8(3) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C2 C3 C4 C7 -176.9(3) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C7 C4 C5 C6 177.3(3) . . . . ? C4 C5 C6 C1 0.1(4) . . . . ? C4 C5 C6 C24 -178.2(3) . . . . ? O1 C1 C6 C5 -178.5(2) . . . . ? C2 C1 C6 C5 0.2(4) . . . . ? O1 C1 C6 C24 -0.1(4) . . . . ? C2 C1 C6 C24 178.5(2) . . . . ? C5 C4 C7 C9 -115.4(4) . . . . ? C3 C4 C7 C9 62.7(4) . . . . ? C5 C4 C7 C10 6.9(5) . . . . ? C3 C4 C7 C10 -175.0(3) . . . . ? C5 C4 C7 C8 126.6(3) . . . . ? C3 C4 C7 C8 -55.3(4) . . . . ? C18 N1 C11 C2 -179.5(2) . . . . ? C12 N1 C11 C2 -57.1(3) . . . . ? Mn1 N1 C11 C2 64.9(2) . . . . ? C3 C2 C11 N1 118.9(3) . . . . ? C1 C2 C11 N1 -65.3(3) . . . . ? C18 N1 C12 C13 -146.6(2) . . . . ? C11 N1 C12 C13 91.6(3) . . . . ? Mn1 N1 C12 C13 -30.1(3) . . . . ? C17 N2 C13 C14 -1.8(4) . . . . ? Mn1 N2 C13 C14 158.7(2) . . . . ? C17 N2 C13 C12 173.5(2) . . . . ? Mn1 N2 C13 C12 -26.1(3) . . . . ? N1 C12 C13 N2 38.6(3) . . . . ? N1 C12 C13 C14 -146.1(3) . . . . ? N2 C13 C14 C15 2.1(4) . . . . ? C12 C13 C14 C15 -173.0(3) . . . . ? C13 C14 C15 C16 -0.3(4) . . . . ? C14 C15 C16 C17 -1.7(4) . . . . ? C13 N2 C17 C16 -0.3(4) . . . . ? Mn1 N2 C17 C16 -158.8(2) . . . . ? C15 C16 C17 N2 2.1(4) . . . . ? C12 N1 C18 C19 76.5(3) . . . . ? C11 N1 C18 C19 -160.7(2) . . . . ? Mn1 N1 C18 C19 -42.8(3) . . . . ? C23 N3 C19 C20 -1.2(4) . . . . ? Mn1 N3 C19 C20 -173.6(2) . . . . ? C23 N3 C19 C18 175.0(3) . . . . ? Mn1 N3 C19 C18 2.6(3) . . . . ? N1 C18 C19 N3 28.7(4) . . . . ? N1 C18 C19 C20 -155.0(3) . . . . ? N3 C19 C20 C21 2.5(4) . . . . ? C18 C19 C20 C21 -173.6(3) . . . . ? C19 C20 C21 C22 -1.5(5) . . . . ? C20 C21 C22 C23 -0.7(5) . . . . ? C19 N3 C23 C22 -1.2(4) . . . . ? Mn1 N3 C23 C22 170.2(2) . . . . ? C21 C22 C23 N3 2.1(5) . . . . ? C31 N4 C24 C6 -180.0(2) . . . . ? C25 N4 C24 C6 -57.5(3) . . . . ? Mn2 N4 C24 C6 64.1(2) . . . . ? C5 C6 C24 N4 113.9(3) . . . . ? C1 C6 C24 N4 -64.4(3) . . . . ? C31 N4 C25 C26 -150.7(2) . . . . ? C24 N4 C25 C26 87.0(3) . . . . ? Mn2 N4 C25 C26 -35.1(3) . . . . ? C30 N5 C26 C27 0.5(4) . . . . ? Mn2 N5 C26 C27 155.4(2) . . . . ? C30 N5 C26 C25 177.8(2) . . . . ? Mn2 N5 C26 C25 -27.2(3) . . . . ? N4 C25 C26 N5 43.1(3) . . . . ? N4 C25 C26 C27 -139.6(3) . . . . ? N5 C26 C27 C28 -1.6(4) . . . . ? C25 C26 C27 C28 -178.8(3) . . . . ? C26 C27 C28 C29 2.0(4) . . . . ? C27 C28 C29 C30 -1.4(5) . . . . ? C26 N5 C30 C29 0.2(4) . . . . ? Mn2 N5 C30 C29 -152.6(2) . . . . ? C28 C29 C30 N5 0.3(5) . . . . ? C25 N4 C31 C32 75.0(3) . . . . ? C24 N4 C31 C32 -161.7(2) . . . . ? Mn2 N4 C31 C32 -42.8(2) . . . . ? C36 N6 C32 C33 -0.5(4) . . . . ? Mn2 N6 C32 C33 -172.4(2) . . . . ? C36 N6 C32 C31 173.7(3) . . . . ? Mn2 N6 C32 C31 1.8(3) . . . . ? N4 C31 C32 N6 29.4(3) . . . . ? N4 C31 C32 C33 -156.4(3) . . . . ? N6 C32 C33 C34 1.4(5) . . . . ? C31 C32 C33 C34 -172.5(3) . . . . ? C32 C33 C34 C35 -0.9(5) . . . . ? C33 C34 C35 C36 -0.3(5) . . . . ? C32 N6 C36 C35 -0.9(5) . . . . ? Mn2 N6 C36 C35 170.1(2) . . . . ? C34 C35 C36 N6 1.3(5) . . . . ? Mn2 O3 C37 O2 2.7(5) . . . . ? Mn1 O2 C37 O3 9.1(5) . . . . ? Mn1 O4 C38 O5 5.9(5) . . . . ? Mn2 O5 C38 O4 11.8(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W O1A 0.85 2.12 2.971(7) 179.2 . O1W H2W O2 0.85 2.05 2.900(5) 178.8 3_666 O2W H3W O1W 0.85 1.82 2.669(9) 179.0 . O2W H4W O1D 0.85 2.17 3.020(9) 179.9 3_566 #============================================================================== data_9_MeCN _database_code_depnum_ccdc_archive 'CCDC 772406' #TrackingRef '- submit_all.cif' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C40 H45 Mn2 N6 O5, 1.15(Cl O4), 0.85(C2 H3 N) ; _chemical_formula_sum ; C41.70 H47.55 Cl1.15 Mn2 N6.85 O9.60 ; _chemical_formula_weight 948.96 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' 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 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 12.1472(5) _cell_length_b 22.0062(10) _cell_length_c 16.9073(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.2780(10) _cell_angle_gamma 90.00 _cell_volume 4492.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9165 _cell_measurement_theta_min 3.53 _cell_measurement_theta_max 26.37 _exptl_crystal_description block _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.692 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.759 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; The perchlorate anion containing Cl2 is partially occupied. Where the perchlorate anion is absent, the site is occupied by MeCN. This implies that the complex is partially oxidised from Mn(II) to Mn(III). This suggestion is consistent with the green colour of the crystal; the pure Mn(II)-Mn(II) crystal is known to be colourless. The geometry of both perchlorate anions is restrained to be tetrahedral. All Cl---O distances are restrained to a common free variable, while the O...O distances are restrained to 1.633 times that free variable, all with an su of 0.01 \%A. [Refined free variable = 1.437(3)]. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 65338 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.03 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 7904 _reflns_number_gt 5285 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+12.2416P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7904 _refine_ls_number_parameters 577 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1564 _refine_ls_wR_factor_gt 0.1378 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.863 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.085 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.44937(6) 0.18543(3) 0.59184(4) 0.02118(19) Uani 1 1 d . . . Mn2 Mn 0.54477(6) 0.25725(3) 0.76413(4) 0.02373(19) Uani 1 1 d . . . O1 O 0.5475(3) 0.25801(13) 0.64164(18) 0.0254(7) Uani 1 1 d . . . O2 O 0.3062(3) 0.18843(15) 0.65225(19) 0.0328(8) Uani 1 1 d . . . O3 O 0.3678(3) 0.25301(17) 0.7493(2) 0.0443(10) Uani 1 1 d . . . O4 O 0.5286(3) 0.11947(14) 0.67317(19) 0.0327(8) Uani 1 1 d . . . O5 O 0.5721(3) 0.16612(16) 0.7894(2) 0.0415(9) Uani 1 1 d . . . N1 N 0.5721(3) 0.18715(16) 0.4940(2) 0.0248(9) Uani 1 1 d . . . N2 N 0.3795(3) 0.25870(17) 0.5022(2) 0.0281(9) Uani 1 1 d . . . N3 N 0.4024(3) 0.10771(17) 0.5090(2) 0.0277(9) Uani 1 1 d . . . N4 N 0.5480(3) 0.36097(17) 0.7589(2) 0.0257(9) Uani 1 1 d . . . N5 N 0.7271(3) 0.28118(16) 0.7672(2) 0.0228(9) Uani 1 1 d . . . N6 N 0.5248(3) 0.28810(19) 0.8866(2) 0.0301(10) Uani 1 1 d . . . C1 C 0.5986(4) 0.29989(18) 0.6011(3) 0.0223(10) Uani 1 1 d . . . C2 C 0.6646(4) 0.2825(2) 0.5429(3) 0.0246(10) Uani 1 1 d . . . C3 C 0.7170(4) 0.3270(2) 0.5017(3) 0.0282(11) Uani 1 1 d . . . H3A H 0.7642 0.3146 0.4634 0.034 Uiso 1 1 calc R . . C4 C 0.7030(4) 0.3884(2) 0.5143(3) 0.0292(11) Uani 1 1 d . . . C5 C 0.6368(4) 0.40493(19) 0.5724(3) 0.0246(11) Uani 1 1 d . . . H5A H 0.6277 0.4469 0.5831 0.030 Uiso 1 1 calc R . . C6 C 0.5829(4) 0.3626(2) 0.6159(3) 0.0251(11) Uani 1 1 d . . . C7 C 0.7595(4) 0.4384(2) 0.4685(3) 0.0349(12) Uani 1 1 d . . . C8 C 0.6687(5) 0.4781(2) 0.4230(3) 0.0465(15) Uani 1 1 d . . . H8A H 0.7034 0.5109 0.3953 0.070 Uiso 1 1 calc R . . H8B H 0.6216 0.4955 0.4606 0.070 Uiso 1 1 calc R . . H8C H 0.6236 0.4530 0.3840 0.070 Uiso 1 1 calc R . . C9 C 0.8315(6) 0.4117(3) 0.4079(4) 0.0570(17) Uani 1 1 d . . . H9A H 0.8671 0.4447 0.3813 0.086 Uiso 1 1 calc R . . H9B H 0.7850 0.3879 0.3683 0.086 Uiso 1 1 calc R . . H9C H 0.8885 0.3854 0.4355 0.086 Uiso 1 1 calc R . . C10 C 0.8318(5) 0.4779(3) 0.5277(3) 0.0489(16) Uani 1 1 d . . . H10A H 0.8676 0.5096 0.4988 0.073 Uiso 1 1 calc R . . H10B H 0.8884 0.4526 0.5574 0.073 Uiso 1 1 calc R . . H10C H 0.7855 0.4969 0.5648 0.073 Uiso 1 1 calc R . . C11 C 0.6785(4) 0.2161(2) 0.5249(3) 0.0277(11) Uani 1 1 d . . . H11A H 0.7319 0.2118 0.4850 0.033 Uiso 1 1 calc R . . H11B H 0.7095 0.1949 0.5739 0.033 Uiso 1 1 calc R . . C12 C 0.5180(4) 0.2200(2) 0.4231(3) 0.0283(11) Uani 1 1 d . . . H12A H 0.4736 0.1908 0.3884 0.034 Uiso 1 1 calc R . . H12B H 0.5759 0.2368 0.3925 0.034 Uiso 1 1 calc R . . C13 C 0.4441(4) 0.2709(2) 0.4445(3) 0.0255(11) Uani 1 1 d . . . C14 C 0.4387(5) 0.3264(2) 0.4051(3) 0.0356(13) Uani 1 1 d . . . H14A H 0.4854 0.3341 0.3647 0.043 Uiso 1 1 calc R . . C15 C 0.3661(5) 0.3697(2) 0.4247(3) 0.0398(14) Uani 1 1 d . . . H15A H 0.3618 0.4079 0.3983 0.048 Uiso 1 1 calc R . . C16 C 0.2992(5) 0.3574(2) 0.4833(4) 0.0437(15) Uani 1 1 d . . . H16A H 0.2472 0.3866 0.4973 0.052 Uiso 1 1 calc R . . C17 C 0.3088(4) 0.3014(2) 0.5217(3) 0.0346(12) Uani 1 1 d . . . H17A H 0.2638 0.2933 0.5630 0.042 Uiso 1 1 calc R . . C18 C 0.5895(4) 0.1231(2) 0.4754(3) 0.0304(11) Uani 1 1 d . . . H18A H 0.6386 0.1042 0.5191 0.036 Uiso 1 1 calc R . . H18B H 0.6263 0.1201 0.4261 0.036 Uiso 1 1 calc R . . C19 C 0.4800(4) 0.0889(2) 0.4642(3) 0.0263(11) Uani 1 1 d . . . C20 C 0.4619(5) 0.0401(2) 0.4121(3) 0.0344(12) Uani 1 1 d . . . H20A H 0.5177 0.0276 0.3804 0.041 Uiso 1 1 calc R . . C21 C 0.3615(5) 0.0100(2) 0.4075(3) 0.0372(14) Uani 1 1 d . . . H21A H 0.3480 -0.0238 0.3728 0.045 Uiso 1 1 calc R . . C22 C 0.2814(5) 0.0292(2) 0.4529(3) 0.0364(13) Uani 1 1 d . . . H22A H 0.2119 0.0091 0.4503 0.044 Uiso 1 1 calc R . . C23 C 0.3045(4) 0.0786(2) 0.5028(3) 0.0312(12) Uani 1 1 d . . . H23A H 0.2490 0.0924 0.5339 0.037 Uiso 1 1 calc R . . C24 C 0.5086(4) 0.3821(2) 0.6761(3) 0.0295(11) Uani 1 1 d . . . H24A H 0.4334 0.3658 0.6606 0.035 Uiso 1 1 calc R . . H24B H 0.5036 0.4270 0.6759 0.035 Uiso 1 1 calc R . . C25 C 0.6622(4) 0.3829(2) 0.7846(3) 0.0292(11) Uani 1 1 d . . . H25A H 0.6721 0.3869 0.8432 0.035 Uiso 1 1 calc R . . H25B H 0.6721 0.4237 0.7616 0.035 Uiso 1 1 calc R . . C26 C 0.7489(4) 0.3410(2) 0.7594(3) 0.0235(10) Uani 1 1 d . . . C27 C 0.8458(4) 0.3613(2) 0.7319(3) 0.0316(12) Uani 1 1 d . . . H27A H 0.8594 0.4036 0.7277 0.038 Uiso 1 1 calc R . . C28 C 0.9221(4) 0.3198(2) 0.7106(3) 0.0366(13) Uani 1 1 d . . . H28A H 0.9893 0.3328 0.6920 0.044 Uiso 1 1 calc R . . C29 C 0.8982(4) 0.2582(2) 0.7170(3) 0.0335(12) Uani 1 1 d . . . H29A H 0.9484 0.2283 0.7020 0.040 Uiso 1 1 calc R . . C30 C 0.8012(4) 0.2412(2) 0.7452(3) 0.0265(11) Uani 1 1 d . . . H30A H 0.7857 0.1990 0.7493 0.032 Uiso 1 1 calc R . . C31 C 0.4717(4) 0.3811(2) 0.8154(3) 0.0360(13) Uani 1 1 d . . . H31A H 0.3943 0.3748 0.7918 0.043 Uiso 1 1 calc R . . H31B H 0.4823 0.4251 0.8261 0.043 Uiso 1 1 calc R . . C32 C 0.4922(4) 0.3462(3) 0.8924(3) 0.0368(13) Uani 1 1 d . . . C33 C 0.4786(5) 0.3714(3) 0.9661(4) 0.0584(18) Uani 1 1 d . . . H33A H 0.4580 0.4128 0.9702 0.070 Uiso 1 1 calc R . . C34 C 0.4952(7) 0.3359(4) 1.0328(4) 0.078(2) Uani 1 1 d . . . H34A H 0.4840 0.3523 1.0833 0.094 Uiso 1 1 calc R . . C35 C 0.5286(6) 0.2756(4) 1.0267(4) 0.069(2) Uani 1 1 d . . . H35A H 0.5422 0.2505 1.0724 0.083 Uiso 1 1 calc R . . C36 C 0.5410(5) 0.2541(3) 0.9524(3) 0.0497(15) Uani 1 1 d . . . H36A H 0.5621 0.2128 0.9472 0.060 Uiso 1 1 calc R . . C37 C 0.2942(4) 0.2201(2) 0.7133(3) 0.0273(11) Uani 1 1 d . . . C38 C 0.1861(4) 0.2188(3) 0.7458(4) 0.0458(15) Uani 1 1 d . . . H38A H 0.1972 0.2074 0.8021 0.069 Uiso 1 1 calc R . . H38B H 0.1376 0.1891 0.7163 0.069 Uiso 1 1 calc R . . H38C H 0.1519 0.2592 0.7405 0.069 Uiso 1 1 calc R . . C39 C 0.5608(4) 0.1198(2) 0.7457(3) 0.0291(11) Uani 1 1 d . . . C40 C 0.5910(5) 0.0597(2) 0.7861(3) 0.0384(13) Uani 1 1 d . . . H40A H 0.5470 0.0271 0.7588 0.058 Uiso 1 1 calc R . . H40B H 0.5759 0.0617 0.8418 0.058 Uiso 1 1 calc R . . H40C H 0.6699 0.0515 0.7838 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.91217(10) 0.06622(5) 0.70339(8) 0.0347(3) Uani 1 1 d D . . O1A O 0.9958(3) 0.10945(16) 0.7326(2) 0.0457(10) Uani 1 1 d D . . O1B O 0.8839(4) 0.02900(16) 0.7678(2) 0.0574(12) Uani 1 1 d D . . O1C O 0.9532(3) 0.02864(16) 0.6433(2) 0.0485(10) Uani 1 1 d D . . O1D O 0.8151(3) 0.09807(16) 0.6699(2) 0.0480(10) Uani 1 1 d D . . Cl2 Cl 0.1572(10) 0.4023(6) 0.7106(7) 0.067(4) Uiso 0.15 1 d PD A 1 O2A O 0.160(2) 0.3588(10) 0.6485(12) 0.088(11) Uiso 0.15 1 d PD A 1 O2B O 0.156(2) 0.3712(11) 0.7855(10) 0.070(9) Uiso 0.15 1 d PD A 1 O2C O 0.2535(18) 0.4406(12) 0.7145(18) 0.130(16) Uiso 0.15 1 d PD A 1 O2D O 0.0593(17) 0.4395(11) 0.6969(15) 0.087(11) Uiso 0.15 1 d PD A 1 N1S N 0.1581(8) 0.4315(5) 0.7567(8) 0.121(4) Uani 0.85 1 d P B 2 C1S C 0.2034(8) 0.4748(5) 0.7748(6) 0.073(3) Uani 0.85 1 d P B 2 C2S C 0.2601(7) 0.5339(4) 0.8004(5) 0.073(3) Uani 0.85 1 d P B 2 H2S1 H 0.3011 0.5490 0.7577 0.110 Uiso 0.85 1 calc PR B 2 H2S2 H 0.3115 0.5270 0.8484 0.110 Uiso 0.85 1 calc PR B 2 H2S3 H 0.2044 0.5639 0.8118 0.110 Uiso 0.85 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0266(4) 0.0171(3) 0.0181(4) -0.0022(3) -0.0055(3) -0.0033(3) Mn2 0.0279(4) 0.0215(4) 0.0205(4) -0.0036(3) -0.0033(3) -0.0048(3) O1 0.0293(18) 0.0192(16) 0.0263(17) -0.0009(13) -0.0031(14) -0.0058(14) O2 0.0283(19) 0.038(2) 0.0312(19) -0.0043(17) -0.0015(15) -0.0041(16) O3 0.035(2) 0.051(2) 0.047(2) -0.0184(19) 0.0053(18) -0.0116(18) O4 0.046(2) 0.0250(18) 0.0243(18) 0.0043(14) -0.0070(16) 0.0030(16) O5 0.065(3) 0.033(2) 0.0249(19) 0.0010(16) -0.0046(18) -0.0101(18) N1 0.034(2) 0.0158(19) 0.024(2) -0.0018(16) -0.0029(17) -0.0015(17) N2 0.028(2) 0.023(2) 0.031(2) 0.0007(17) -0.0074(18) 0.0003(17) N3 0.034(2) 0.023(2) 0.024(2) -0.0005(17) -0.0055(18) -0.0041(18) N4 0.024(2) 0.026(2) 0.027(2) -0.0069(17) 0.0005(17) 0.0025(17) N5 0.023(2) 0.020(2) 0.023(2) -0.0028(16) -0.0103(16) 0.0006(16) N6 0.028(2) 0.035(2) 0.026(2) -0.0028(19) -0.0020(18) -0.0033(18) C1 0.025(2) 0.012(2) 0.026(2) 0.0003(18) -0.013(2) -0.0064(18) C2 0.024(3) 0.019(2) 0.030(3) -0.005(2) -0.001(2) 0.0015(19) C3 0.026(3) 0.027(3) 0.030(3) -0.002(2) -0.005(2) -0.005(2) C4 0.029(3) 0.023(3) 0.034(3) 0.000(2) -0.009(2) -0.004(2) C5 0.030(3) 0.012(2) 0.029(3) 0.0017(19) -0.010(2) -0.0031(19) C6 0.025(3) 0.021(2) 0.027(3) -0.005(2) -0.010(2) 0.0016(19) C7 0.044(3) 0.017(2) 0.042(3) 0.004(2) -0.003(2) -0.007(2) C8 0.061(4) 0.034(3) 0.042(3) 0.013(3) -0.008(3) -0.007(3) C9 0.068(4) 0.038(3) 0.067(4) 0.006(3) 0.020(4) -0.012(3) C10 0.052(4) 0.038(3) 0.053(4) 0.009(3) -0.009(3) -0.022(3) C11 0.028(3) 0.022(2) 0.033(3) -0.002(2) 0.001(2) -0.001(2) C12 0.041(3) 0.024(3) 0.019(2) 0.003(2) 0.000(2) -0.005(2) C13 0.028(3) 0.023(2) 0.022(2) -0.0020(19) -0.011(2) -0.006(2) C14 0.050(3) 0.027(3) 0.027(3) 0.001(2) -0.012(2) -0.004(2) C15 0.052(4) 0.027(3) 0.038(3) 0.011(2) -0.010(3) 0.001(3) C16 0.041(3) 0.029(3) 0.055(4) 0.000(3) -0.019(3) 0.007(2) C17 0.027(3) 0.036(3) 0.039(3) 0.003(2) -0.007(2) 0.003(2) C18 0.045(3) 0.019(2) 0.027(3) -0.006(2) 0.006(2) 0.001(2) C19 0.041(3) 0.016(2) 0.020(2) 0.0041(19) -0.005(2) 0.000(2) C20 0.051(3) 0.024(3) 0.027(3) -0.005(2) -0.003(2) 0.002(2) C21 0.063(4) 0.018(3) 0.026(3) -0.002(2) -0.015(3) -0.008(3) C22 0.046(3) 0.023(3) 0.036(3) 0.004(2) -0.016(3) -0.011(2) C23 0.042(3) 0.025(3) 0.023(3) 0.002(2) -0.010(2) -0.006(2) C24 0.032(3) 0.020(2) 0.033(3) -0.002(2) -0.010(2) 0.004(2) C25 0.029(3) 0.023(3) 0.033(3) -0.012(2) -0.006(2) -0.003(2) C26 0.028(3) 0.020(2) 0.019(2) -0.0052(19) -0.012(2) 0.002(2) C27 0.030(3) 0.028(3) 0.035(3) -0.001(2) -0.007(2) -0.003(2) C28 0.030(3) 0.035(3) 0.044(3) 0.002(2) -0.002(2) -0.003(2) C29 0.023(3) 0.037(3) 0.039(3) 0.001(2) -0.005(2) 0.009(2) C30 0.031(3) 0.020(2) 0.025(3) -0.002(2) -0.011(2) 0.007(2) C31 0.035(3) 0.032(3) 0.039(3) -0.010(2) -0.007(2) 0.010(2) C32 0.025(3) 0.050(3) 0.035(3) -0.014(3) 0.002(2) -0.001(2) C33 0.055(4) 0.071(5) 0.048(4) -0.028(3) 0.003(3) 0.017(3) C34 0.096(6) 0.109(7) 0.031(4) -0.019(4) 0.013(4) 0.023(5) C35 0.087(5) 0.097(6) 0.024(3) 0.004(3) 0.009(3) 0.025(4) C36 0.055(4) 0.063(4) 0.031(3) -0.002(3) 0.002(3) -0.001(3) C37 0.024(3) 0.023(2) 0.033(3) 0.007(2) -0.005(2) 0.000(2) C38 0.031(3) 0.053(4) 0.054(4) -0.017(3) 0.005(3) -0.008(3) C39 0.033(3) 0.027(3) 0.027(3) 0.003(2) 0.003(2) 0.000(2) C40 0.041(3) 0.035(3) 0.038(3) 0.012(2) 0.001(2) 0.003(2) Cl1 0.0395(7) 0.0199(6) 0.0423(7) -0.0063(5) -0.0066(6) -0.0012(5) O1A 0.047(2) 0.038(2) 0.051(2) -0.0174(18) -0.0038(19) -0.0183(18) O1B 0.086(3) 0.029(2) 0.055(3) 0.0036(19) 0.001(2) -0.009(2) O1C 0.048(2) 0.037(2) 0.057(3) -0.0263(19) -0.009(2) 0.0055(18) O1D 0.039(2) 0.033(2) 0.068(3) 0.0003(19) -0.010(2) 0.0069(17) N1S 0.080(7) 0.113(9) 0.177(12) 0.062(9) 0.039(7) -0.002(6) C1S 0.057(6) 0.083(7) 0.082(7) 0.029(6) 0.015(5) 0.001(5) C2S 0.080(6) 0.102(7) 0.038(4) 0.005(4) 0.010(4) 0.026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 Mn2 3.4041(9) . ? Mn1 O2 2.112(3) . ? Mn1 O1 2.113(3) . ? Mn1 O4 2.153(3) . ? Mn1 N3 2.245(4) . ? Mn1 N2 2.310(4) . ? Mn1 N1 2.345(4) . ? Mn2 O5 2.070(4) . ? Mn2 O1 2.075(3) . ? Mn2 O3 2.139(4) . ? Mn2 N6 2.218(4) . ? Mn2 N5 2.272(4) . ? Mn2 N4 2.285(4) . ? O1 C1 1.340(5) . ? O2 C37 1.267(6) . ? O3 C37 1.255(6) . ? O4 C39 1.246(5) . ? O5 C39 1.259(6) . ? N1 C18 1.465(6) . ? N1 C11 1.485(6) . ? N1 C12 1.489(6) . ? N2 C17 1.339(6) . ? N2 C13 1.343(6) . ? N3 C19 1.337(6) . ? N3 C23 1.345(6) . ? N4 C31 1.470(6) . ? N4 C25 1.488(6) . ? N4 C24 1.503(6) . ? N5 C30 1.341(6) . ? N5 C26 1.353(6) . ? N6 C36 1.337(7) . ? N6 C32 1.345(7) . ? C1 C2 1.390(7) . ? C1 C6 1.418(6) . ? C2 C3 1.395(7) . ? C2 C11 1.506(6) . ? C3 C4 1.382(7) . ? C3 H3A 0.950 . ? C4 C5 1.385(7) . ? C4 C7 1.549(7) . ? C5 C6 1.394(6) . ? C5 H5A 0.950 . ? C6 C24 1.495(7) . ? C7 C10 1.527(7) . ? C7 C9 1.535(8) . ? C7 C8 1.545(7) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 C13 1.503(7) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.389(6) . ? C14 C15 1.365(7) . ? C14 H14A 0.950 . ? C15 C16 1.375(8) . ? C15 H15A 0.950 . ? C16 C17 1.390(7) . ? C16 H16A 0.950 . ? C17 H17A 0.950 . ? C18 C19 1.521(7) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 C20 1.392(6) . ? C20 C21 1.382(7) . ? C20 H20A 0.950 . ? C21 C22 1.371(8) . ? C21 H21A 0.950 . ? C22 C23 1.385(7) . ? C22 H22A 0.950 . ? C23 H23A 0.950 . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 C26 1.496(6) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.385(7) . ? C27 C28 1.378(7) . ? C27 H27A 0.950 . ? C28 C29 1.393(7) . ? C28 H28A 0.950 . ? C29 C30 1.370(7) . ? C29 H29A 0.950 . ? C30 H30A 0.950 . ? C31 C32 1.509(7) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 C33 1.391(7) . ? C33 C34 1.368(10) . ? C33 H33A 0.950 . ? C34 C35 1.394(10) . ? C34 H34A 0.950 . ? C35 C36 1.367(8) . ? C35 H35A 0.950 . ? C36 H36A 0.950 . ? C37 C38 1.477(7) . ? C38 H38A 0.980 . ? C38 H38B 0.980 . ? C38 H38C 0.980 . ? C39 C40 1.514(7) . ? C40 H40A 0.980 . ? C40 H40B 0.980 . ? C40 H40C 0.980 . ? Cl1 O1D 1.433(3) . ? Cl1 O1B 1.434(4) . ? Cl1 O1A 1.439(3) . ? Cl1 O1C 1.441(3) . ? Cl2 O2A 1.423(9) . ? Cl2 O2C 1.437(9) . ? Cl2 O2D 1.442(9) . ? Cl2 O2B 1.443(9) . ? N1S C1S 1.125(13) . ? C1S C2S 1.512(14) . ? C2S H2S1 0.980 . ? C2S H2S2 0.980 . ? C2S H2S3 0.980 . ? 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 O2 Mn1 O1 104.03(13) . . ? O2 Mn1 O4 92.65(13) . . ? O1 Mn1 O4 93.55(12) . . ? O2 Mn1 N3 99.16(14) . . ? O1 Mn1 N3 156.74(14) . . ? O4 Mn1 N3 87.15(13) . . ? O2 Mn1 N2 91.88(14) . . ? O1 Mn1 N2 83.38(12) . . ? O4 Mn1 N2 175.04(14) . . ? N3 Mn1 N2 94.13(14) . . ? O2 Mn1 N1 163.98(13) . . ? O1 Mn1 N1 83.94(12) . . ? O4 Mn1 N1 100.80(13) . . ? N3 Mn1 N1 73.12(14) . . ? N2 Mn1 N1 75.04(14) . . ? O5 Mn2 O1 101.20(13) . . ? O5 Mn2 O3 96.80(15) . . ? O1 Mn2 O3 90.53(13) . . ? O5 Mn2 N6 97.76(15) . . ? O1 Mn2 N6 160.90(14) . . ? O3 Mn2 N6 84.95(14) . . ? O5 Mn2 N5 94.92(14) . . ? O1 Mn2 N5 84.20(13) . . ? O3 Mn2 N5 167.89(14) . . ? N6 Mn2 N5 96.50(14) . . ? O5 Mn2 N4 166.63(14) . . ? O1 Mn2 N4 87.20(13) . . ? O3 Mn2 N4 93.47(14) . . ? N6 Mn2 N4 74.60(15) . . ? N5 Mn2 N4 75.43(13) . . ? C1 O1 Mn2 125.1(3) . . ? C1 O1 Mn1 126.1(3) . . ? Mn2 O1 Mn1 108.76(14) . . ? C37 O2 Mn1 125.8(3) . . ? C37 O3 Mn2 137.4(3) . . ? C39 O4 Mn1 134.1(3) . . ? C39 O5 Mn2 131.3(3) . . ? C18 N1 C11 110.4(4) . . ? C18 N1 C12 110.8(4) . . ? C11 N1 C12 111.4(4) . . ? C18 N1 Mn1 104.7(3) . . ? C11 N1 Mn1 110.8(3) . . ? C12 N1 Mn1 108.5(3) . . ? C17 N2 C13 118.7(4) . . ? C17 N2 Mn1 121.9(3) . . ? C13 N2 Mn1 114.4(3) . . ? C19 N3 C23 118.7(4) . . ? C19 N3 Mn1 116.2(3) . . ? C23 N3 Mn1 125.0(3) . . ? C31 N4 C25 110.3(4) . . ? C31 N4 C24 110.7(4) . . ? C25 N4 C24 111.3(4) . . ? C31 N4 Mn2 105.2(3) . . ? C25 N4 Mn2 109.4(3) . . ? C24 N4 Mn2 109.8(3) . . ? C30 N5 C26 117.9(4) . . ? C30 N5 Mn2 121.6(3) . . ? C26 N5 Mn2 115.1(3) . . ? C36 N6 C32 119.4(5) . . ? C36 N6 Mn2 125.7(4) . . ? C32 N6 Mn2 114.9(3) . . ? O1 C1 C2 120.5(4) . . ? O1 C1 C6 120.0(4) . . ? C2 C1 C6 119.4(4) . . ? C1 C2 C3 119.4(4) . . ? C1 C2 C11 119.8(4) . . ? C3 C2 C11 120.8(4) . . ? C4 C3 C2 122.5(5) . . ? C4 C3 H3A 118.7 . . ? C2 C3 H3A 118.7 . . ? C3 C4 C5 117.2(4) . . ? C3 C4 C7 123.3(5) . . ? C5 C4 C7 119.5(4) . . ? C4 C5 C6 122.8(4) . . ? C4 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? C5 C6 C1 118.6(4) . . ? C5 C6 C24 121.3(4) . . ? C1 C6 C24 120.1(4) . . ? C10 C7 C9 109.1(5) . . ? C10 C7 C8 109.4(4) . . ? C9 C7 C8 108.2(5) . . ? C10 C7 C4 109.4(4) . . ? C9 C7 C4 112.2(4) . . ? C8 C7 C4 108.6(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C2 112.1(4) . . ? N1 C11 H11A 109.2 . . ? C2 C11 H11A 109.2 . . ? N1 C11 H11B 109.2 . . ? C2 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N1 C12 C13 113.0(4) . . ? N1 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? N1 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? N2 C13 C14 121.5(5) . . ? N2 C13 C12 116.0(4) . . ? C14 C13 C12 122.5(5) . . ? C15 C14 C13 119.7(5) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 119.0(5) . . ? C14 C15 H15A 120.5 . . ? C16 C15 H15A 120.5 . . ? C15 C16 C17 119.0(5) . . ? C15 C16 H16A 120.5 . . ? C17 C16 H16A 120.5 . . ? N2 C17 C16 122.0(5) . . ? N2 C17 H17A 119.0 . . ? C16 C17 H17A 119.0 . . ? N1 C18 C19 110.9(4) . . ? N1 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? N1 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.0 . . ? N3 C19 C20 121.6(5) . . ? N3 C19 C18 116.0(4) . . ? C20 C19 C18 122.4(5) . . ? C21 C20 C19 118.9(5) . . ? C21 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? C22 C21 C20 119.8(5) . . ? C22 C21 H21A 120.1 . . ? C20 C21 H21A 120.1 . . ? C21 C22 C23 118.3(5) . . ? C21 C22 H22A 120.9 . . ? C23 C22 H22A 120.9 . . ? N3 C23 C22 122.7(5) . . ? N3 C23 H23A 118.7 . . ? C22 C23 H23A 118.7 . . ? C6 C24 N4 113.0(4) . . ? C6 C24 H24A 109.0 . . ? N4 C24 H24A 109.0 . . ? C6 C24 H24B 109.0 . . ? N4 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? N4 C25 C26 112.3(4) . . ? N4 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? N4 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.9 . . ? N5 C26 C27 122.0(4) . . ? N5 C26 C25 114.9(4) . . ? C27 C26 C25 123.1(4) . . ? C28 C27 C26 119.6(5) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C27 C28 C29 118.2(5) . . ? C27 C28 H28A 120.9 . . ? C29 C28 H28A 120.9 . . ? C30 C29 C28 119.2(5) . . ? C30 C29 H29A 120.4 . . ? C28 C29 H29A 120.4 . . ? N5 C30 C29 123.1(4) . . ? N5 C30 H30A 118.4 . . ? C29 C30 H30A 118.4 . . ? N4 C31 C32 110.5(4) . . ? N4 C31 H31A 109.6 . . ? C32 C31 H31A 109.6 . . ? N4 C31 H31B 109.6 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? N6 C32 C33 120.5(5) . . ? N6 C32 C31 116.4(4) . . ? C33 C32 C31 123.1(5) . . ? C34 C33 C32 119.3(6) . . ? C34 C33 H33A 120.3 . . ? C32 C33 H33A 120.3 . . ? C33 C34 C35 120.0(6) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C36 C35 C34 117.4(6) . . ? C36 C35 H35A 121.3 . . ? C34 C35 H35A 121.3 . . ? N6 C36 C35 123.3(6) . . ? N6 C36 H36A 118.3 . . ? C35 C36 H36A 118.3 . . ? O3 C37 O2 124.9(5) . . ? O3 C37 C38 116.5(5) . . ? O2 C37 C38 118.6(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O4 C39 O5 125.8(4) . . ? O4 C39 C40 118.3(4) . . ? O5 C39 C40 115.9(4) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O1D Cl1 O1B 108.9(2) . . ? O1D Cl1 O1A 109.3(2) . . ? O1B Cl1 O1A 109.6(2) . . ? O1D Cl1 O1C 109.6(2) . . ? O1B Cl1 O1C 109.7(2) . . ? O1A Cl1 O1C 109.6(2) . . ? O2A Cl2 O2C 110.2(8) . . ? O2A Cl2 O2D 110.4(8) . . ? O2C Cl2 O2D 109.1(8) . . ? O2A Cl2 O2B 109.3(8) . . ? O2C Cl2 O2B 109.0(8) . . ? O2D Cl2 O2B 108.7(8) . . ? N1S C1S C2S 177.8(12) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Mn2 O1 C1 -137.1(3) . . . . ? O3 Mn2 O1 C1 125.9(3) . . . . ? N6 Mn2 O1 C1 49.9(6) . . . . ? N5 Mn2 O1 C1 -43.2(3) . . . . ? N4 Mn2 O1 C1 32.5(3) . . . . ? O5 Mn2 O1 Mn1 46.29(17) . . . . ? O3 Mn2 O1 Mn1 -50.75(16) . . . . ? N6 Mn2 O1 Mn1 -126.7(4) . . . . ? N5 Mn2 O1 Mn1 140.17(15) . . . . ? N4 Mn2 O1 Mn1 -144.20(15) . . . . ? O2 Mn1 O1 C1 -132.9(3) . . . . ? O4 Mn1 O1 C1 133.4(3) . . . . ? N3 Mn1 O1 C1 42.4(5) . . . . ? N2 Mn1 O1 C1 -42.7(3) . . . . ? N1 Mn1 O1 C1 32.9(3) . . . . ? O2 Mn1 O1 Mn2 43.66(17) . . . . ? O4 Mn1 O1 Mn2 -49.96(16) . . . . ? N3 Mn1 O1 Mn2 -141.0(3) . . . . ? N2 Mn1 O1 Mn2 133.95(16) . . . . ? N1 Mn1 O1 Mn2 -150.46(15) . . . . ? O1 Mn1 O2 C37 -10.9(4) . . . . ? O4 Mn1 O2 C37 83.4(4) . . . . ? N3 Mn1 O2 C37 170.9(4) . . . . ? N2 Mn1 O2 C37 -94.6(4) . . . . ? N1 Mn1 O2 C37 -129.3(5) . . . . ? O5 Mn2 O3 C37 -47.3(5) . . . . ? O1 Mn2 O3 C37 54.0(5) . . . . ? N6 Mn2 O3 C37 -144.5(5) . . . . ? N5 Mn2 O3 C37 118.0(7) . . . . ? N4 Mn2 O3 C37 141.3(5) . . . . ? O2 Mn1 O4 C39 -63.3(5) . . . . ? O1 Mn1 O4 C39 40.9(5) . . . . ? N3 Mn1 O4 C39 -162.4(5) . . . . ? N1 Mn1 O4 C39 125.4(5) . . . . ? O1 Mn2 O5 C39 -19.6(5) . . . . ? O3 Mn2 O5 C39 72.3(5) . . . . ? N6 Mn2 O5 C39 158.1(5) . . . . ? N5 Mn2 O5 C39 -104.6(5) . . . . ? N4 Mn2 O5 C39 -147.7(6) . . . . ? O2 Mn1 N1 C18 -97.7(5) . . . . ? O1 Mn1 N1 C18 141.4(3) . . . . ? O4 Mn1 N1 C18 48.9(3) . . . . ? N3 Mn1 N1 C18 -34.7(3) . . . . ? N2 Mn1 N1 C18 -133.8(3) . . . . ? O2 Mn1 N1 C11 143.3(4) . . . . ? O1 Mn1 N1 C11 22.4(3) . . . . ? O4 Mn1 N1 C11 -70.1(3) . . . . ? N3 Mn1 N1 C11 -153.7(3) . . . . ? N2 Mn1 N1 C11 107.1(3) . . . . ? O2 Mn1 N1 C12 20.7(6) . . . . ? O1 Mn1 N1 C12 -100.2(3) . . . . ? O4 Mn1 N1 C12 167.3(3) . . . . ? N3 Mn1 N1 C12 83.7(3) . . . . ? N2 Mn1 N1 C12 -15.5(3) . . . . ? O2 Mn1 N2 C17 29.0(4) . . . . ? O1 Mn1 N2 C17 -75.0(4) . . . . ? N3 Mn1 N2 C17 128.3(4) . . . . ? N1 Mn1 N2 C17 -160.4(4) . . . . ? O2 Mn1 N2 C13 -176.5(3) . . . . ? O1 Mn1 N2 C13 79.6(3) . . . . ? N3 Mn1 N2 C13 -77.1(3) . . . . ? N1 Mn1 N2 C13 -5.8(3) . . . . ? O2 Mn1 N3 C19 -174.6(3) . . . . ? O1 Mn1 N3 C19 9.9(5) . . . . ? O4 Mn1 N3 C19 -82.4(3) . . . . ? N2 Mn1 N3 C19 92.8(3) . . . . ? N1 Mn1 N3 C19 19.8(3) . . . . ? O2 Mn1 N3 C23 3.8(4) . . . . ? O1 Mn1 N3 C23 -171.6(3) . . . . ? O4 Mn1 N3 C23 96.0(4) . . . . ? N2 Mn1 N3 C23 -88.8(4) . . . . ? N1 Mn1 N3 C23 -161.8(4) . . . . ? O5 Mn2 N4 C31 -90.5(7) . . . . ? O1 Mn2 N4 C31 140.0(3) . . . . ? O3 Mn2 N4 C31 49.7(3) . . . . ? N6 Mn2 N4 C31 -34.1(3) . . . . ? N5 Mn2 N4 C31 -135.2(3) . . . . ? O5 Mn2 N4 C25 27.9(8) . . . . ? O1 Mn2 N4 C25 -101.5(3) . . . . ? O3 Mn2 N4 C25 168.1(3) . . . . ? N6 Mn2 N4 C25 84.3(3) . . . . ? N5 Mn2 N4 C25 -16.8(3) . . . . ? O5 Mn2 N4 C24 150.4(6) . . . . ? O1 Mn2 N4 C24 20.9(3) . . . . ? O3 Mn2 N4 C24 -69.4(3) . . . . ? N6 Mn2 N4 C24 -153.2(3) . . . . ? N5 Mn2 N4 C24 105.7(3) . . . . ? O5 Mn2 N5 C30 31.8(3) . . . . ? O1 Mn2 N5 C30 -69.0(3) . . . . ? O3 Mn2 N5 C30 -133.5(6) . . . . ? N6 Mn2 N5 C30 130.2(3) . . . . ? N4 Mn2 N5 C30 -157.6(4) . . . . ? O5 Mn2 N5 C26 -174.8(3) . . . . ? O1 Mn2 N5 C26 84.4(3) . . . . ? O3 Mn2 N5 C26 19.8(8) . . . . ? N6 Mn2 N5 C26 -76.4(3) . . . . ? N4 Mn2 N5 C26 -4.2(3) . . . . ? O5 Mn2 N6 C36 6.6(5) . . . . ? O1 Mn2 N6 C36 179.6(4) . . . . ? O3 Mn2 N6 C36 102.8(4) . . . . ? N5 Mn2 N6 C36 -89.3(4) . . . . ? N4 Mn2 N6 C36 -162.2(5) . . . . ? O5 Mn2 N6 C32 -172.5(3) . . . . ? O1 Mn2 N6 C32 0.5(6) . . . . ? O3 Mn2 N6 C32 -76.3(3) . . . . ? N5 Mn2 N6 C32 91.6(3) . . . . ? N4 Mn2 N6 C32 18.7(3) . . . . ? Mn2 O1 C1 C2 133.6(3) . . . . ? Mn1 O1 C1 C2 -50.3(5) . . . . ? Mn2 O1 C1 C6 -48.1(5) . . . . ? Mn1 O1 C1 C6 127.9(4) . . . . ? O1 C1 C2 C3 -179.9(4) . . . . ? C6 C1 C2 C3 1.9(6) . . . . ? O1 C1 C2 C11 0.4(6) . . . . ? C6 C1 C2 C11 -177.9(4) . . . . ? C1 C2 C3 C4 -2.3(7) . . . . ? C11 C2 C3 C4 177.4(4) . . . . ? C2 C3 C4 C5 2.2(7) . . . . ? C2 C3 C4 C7 -179.4(4) . . . . ? C3 C4 C5 C6 -1.8(7) . . . . ? C7 C4 C5 C6 179.8(4) . . . . ? C4 C5 C6 C1 1.4(7) . . . . ? C4 C5 C6 C24 -177.7(4) . . . . ? O1 C1 C6 C5 -179.7(4) . . . . ? C2 C1 C6 C5 -1.4(6) . . . . ? O1 C1 C6 C24 -0.6(6) . . . . ? C2 C1 C6 C24 177.6(4) . . . . ? C3 C4 C7 C10 -120.8(5) . . . . ? C5 C4 C7 C10 57.6(6) . . . . ? C3 C4 C7 C9 0.3(7) . . . . ? C5 C4 C7 C9 178.7(5) . . . . ? C3 C4 C7 C8 119.8(5) . . . . ? C5 C4 C7 C8 -61.8(6) . . . . ? C18 N1 C11 C2 178.6(4) . . . . ? C12 N1 C11 C2 55.0(5) . . . . ? Mn1 N1 C11 C2 -65.8(4) . . . . ? C1 C2 C11 N1 62.8(6) . . . . ? C3 C2 C11 N1 -116.9(5) . . . . ? C18 N1 C12 C13 148.4(4) . . . . ? C11 N1 C12 C13 -88.2(5) . . . . ? Mn1 N1 C12 C13 34.0(4) . . . . ? C17 N2 C13 C14 -0.1(6) . . . . ? Mn1 N2 C13 C14 -155.5(3) . . . . ? C17 N2 C13 C12 -177.5(4) . . . . ? Mn1 N2 C13 C12 27.1(5) . . . . ? N1 C12 C13 N2 -42.5(5) . . . . ? N1 C12 C13 C14 140.1(4) . . . . ? N2 C13 C14 C15 -0.3(7) . . . . ? C12 C13 C14 C15 176.9(4) . . . . ? C13 C14 C15 C16 -0.1(7) . . . . ? C14 C15 C16 C17 1.0(8) . . . . ? C13 N2 C17 C16 1.0(7) . . . . ? Mn1 N2 C17 C16 154.6(4) . . . . ? C15 C16 C17 N2 -1.5(7) . . . . ? C11 N1 C18 C19 165.5(4) . . . . ? C12 N1 C18 C19 -70.6(5) . . . . ? Mn1 N1 C18 C19 46.2(4) . . . . ? C23 N3 C19 C20 -0.4(6) . . . . ? Mn1 N3 C19 C20 178.2(3) . . . . ? C23 N3 C19 C18 -178.8(4) . . . . ? Mn1 N3 C19 C18 -0.2(5) . . . . ? N1 C18 C19 N3 -33.2(5) . . . . ? N1 C18 C19 C20 148.4(4) . . . . ? N3 C19 C20 C21 -0.6(7) . . . . ? C18 C19 C20 C21 177.7(4) . . . . ? C19 C20 C21 C22 0.9(7) . . . . ? C20 C21 C22 C23 -0.2(7) . . . . ? C19 N3 C23 C22 1.1(7) . . . . ? Mn1 N3 C23 C22 -177.3(3) . . . . ? C21 C22 C23 N3 -0.8(7) . . . . ? C5 C6 C24 N4 -118.4(5) . . . . ? C1 C6 C24 N4 62.5(5) . . . . ? C31 N4 C24 C6 -179.7(4) . . . . ? C25 N4 C24 C6 57.3(5) . . . . ? Mn2 N4 C24 C6 -64.0(4) . . . . ? C31 N4 C25 C26 150.1(4) . . . . ? C24 N4 C25 C26 -86.6(5) . . . . ? Mn2 N4 C25 C26 34.9(5) . . . . ? C30 N5 C26 C27 -2.0(6) . . . . ? Mn2 N5 C26 C27 -156.4(3) . . . . ? C30 N5 C26 C25 179.5(4) . . . . ? Mn2 N5 C26 C25 25.1(5) . . . . ? N4 C25 C26 N5 -41.0(5) . . . . ? N4 C25 C26 C27 140.5(4) . . . . ? N5 C26 C27 C28 1.0(7) . . . . ? C25 C26 C27 C28 179.3(4) . . . . ? C26 C27 C28 C29 0.5(7) . . . . ? C27 C28 C29 C30 -1.0(7) . . . . ? C26 N5 C30 C29 1.5(6) . . . . ? Mn2 N5 C30 C29 154.2(4) . . . . ? C28 C29 C30 N5 0.0(7) . . . . ? C25 N4 C31 C32 -72.2(5) . . . . ? C24 N4 C31 C32 164.2(4) . . . . ? Mn2 N4 C31 C32 45.6(4) . . . . ? C36 N6 C32 C33 2.0(8) . . . . ? Mn2 N6 C32 C33 -178.9(4) . . . . ? C36 N6 C32 C31 -177.9(5) . . . . ? Mn2 N6 C32 C31 1.3(6) . . . . ? N4 C31 C32 N6 -33.4(6) . . . . ? N4 C31 C32 C33 146.8(5) . . . . ? N6 C32 C33 C34 -2.1(9) . . . . ? C31 C32 C33 C34 177.7(6) . . . . ? C32 C33 C34 C35 1.9(11) . . . . ? C33 C34 C35 C36 -1.5(12) . . . . ? C32 N6 C36 C35 -1.6(9) . . . . ? Mn2 N6 C36 C35 179.3(5) . . . . ? C34 C35 C36 N6 1.3(11) . . . . ? Mn2 O3 C37 O2 -24.3(8) . . . . ? Mn2 O3 C37 C38 155.5(4) . . . . ? Mn1 O2 C37 O3 -3.0(7) . . . . ? Mn1 O2 C37 C38 177.2(4) . . . . ? Mn1 O4 C39 O5 -14.0(8) . . . . ? Mn1 O4 C39 C40 167.0(3) . . . . ? Mn2 O5 C39 O4 0.1(8) . . . . ? Mn2 O5 C39 C40 179.2(3) . . . . ? #============================================================================== data_10_MeCN _database_code_depnum_ccdc_archive 'CCDC 772407' #TrackingRef '- submit_all.cif' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H39 F6 Mn2 N6 O5 +, Cl O4 -, C2 H3 N' _chemical_formula_sum 'C42 H42 Cl F6 Mn2 N7 O9' _chemical_formula_weight 1048.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0416(13) _cell_length_b 11.1647(15) _cell_length_c 20.987(3) _cell_angle_alpha 81.088(6) _cell_angle_beta 84.150(5) _cell_angle_gamma 77.758(5) _cell_volume 2265.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9637 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.74 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ? _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 66975 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 26.00 _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.975 _reflns_number_total 8464 _reflns_number_gt 7020 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.8689P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8464 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.347 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.046 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.45105(2) 0.72534(2) 0.190805(12) 0.01954(7) Uani 1 1 d . . . Mn2 Mn 0.14001(2) 0.64964(2) 0.164239(12) 0.01858(7) Uani 1 1 d . . . F4 F 0.02731(12) 1.09818(11) 0.10369(7) 0.0558(4) Uani 1 1 d . . . F1 F 0.30608(13) 0.73771(13) -0.04810(6) 0.0544(4) Uani 1 1 d . . . F5 F 0.23248(14) 1.11172(11) 0.10730(8) 0.0623(4) Uani 1 1 d . . . F2 F 0.47289(18) 0.81502(16) -0.03234(6) 0.0745(5) Uani 1 1 d . . . F3 F 0.50205(17) 0.62496(16) -0.04006(6) 0.0788(5) Uani 1 1 d . . . F6 F 0.1804(2) 1.02025(14) 0.03496(7) 0.0825(5) Uani 1 1 d . . . O1 O 0.30496(11) 0.61612(10) 0.22336(5) 0.0206(3) Uani 1 1 d . . . O2 O 0.47702(13) 0.70773(13) 0.08946(6) 0.0337(3) Uani 1 1 d . . . O3 O 0.28551(13) 0.64473(13) 0.07542(6) 0.0335(3) Uani 1 1 d . . . O4 O 0.28908(14) 0.88464(12) 0.16595(8) 0.0429(4) Uani 1 1 d . . . O5 O 0.09343(13) 0.84688(11) 0.13941(7) 0.0330(3) Uani 1 1 d . . . N1 N 0.48643(14) 0.72439(12) 0.29777(7) 0.0200(3) Uani 1 1 d . . . N2 N 0.60742(14) 0.54976(13) 0.21598(7) 0.0208(3) Uani 1 1 d . . . N3 N 0.57944(14) 0.86662(13) 0.19006(7) 0.0234(3) Uani 1 1 d . . . N4 N 0.13358(14) 0.44394(12) 0.19227(6) 0.0187(3) Uani 1 1 d . . . N5 N 0.01023(14) 0.64552(13) 0.25899(7) 0.0213(3) Uani 1 1 d . . . N6 N -0.00601(14) 0.60880(13) 0.09966(7) 0.0219(3) Uani 1 1 d . . . C1 C 0.31807(16) 0.53163(15) 0.27697(8) 0.0188(3) Uani 1 1 d . . . C2 C 0.34877(16) 0.56309(15) 0.33513(8) 0.0197(3) Uani 1 1 d . . . C3 C 0.36548(17) 0.47379(16) 0.38937(8) 0.0225(4) Uani 1 1 d . . . H3A H 0.3853 0.4968 0.4286 0.027 Uiso 1 1 calc R . . C4 C 0.35431(17) 0.35235(16) 0.38837(8) 0.0233(4) Uani 1 1 d . . . C5 C 0.32060(17) 0.32384(16) 0.33055(8) 0.0225(4) Uani 1 1 d . . . H5A H 0.3097 0.2420 0.3288 0.027 Uiso 1 1 calc R . . C6 C 0.30232(16) 0.40994(15) 0.27550(8) 0.0200(4) Uani 1 1 d . . . C7 C 0.3799(2) 0.25064(18) 0.44640(9) 0.0319(4) Uani 1 1 d . . . C8 C 0.4194(3) 0.2994(2) 0.50452(10) 0.0481(6) Uani 1 1 d . . . H8A H 0.4346 0.2320 0.5406 0.072 Uiso 1 1 calc R . . H8B H 0.3456 0.3658 0.5175 0.072 Uiso 1 1 calc R . . H8C H 0.5034 0.3317 0.4928 0.072 Uiso 1 1 calc R . . C9 C 0.2511(3) 0.1986(2) 0.46698(11) 0.0501(6) Uani 1 1 d . . . H9A H 0.2271 0.1618 0.4313 0.075 Uiso 1 1 calc R . . H9B H 0.1758 0.2654 0.4781 0.075 Uiso 1 1 calc R . . H9C H 0.2675 0.1351 0.5047 0.075 Uiso 1 1 calc R . . C10 C 0.4982(3) 0.1487(2) 0.42678(12) 0.0567(7) Uani 1 1 d . . . H10A H 0.4712 0.1099 0.3926 0.085 Uiso 1 1 calc R . . H10B H 0.5209 0.0862 0.4644 0.085 Uiso 1 1 calc R . . H10C H 0.5782 0.1848 0.4108 0.085 Uiso 1 1 calc R . . C11 C 0.36546(17) 0.69292(16) 0.33871(8) 0.0227(4) Uani 1 1 d . . . H11A H 0.2823 0.7521 0.3244 0.027 Uiso 1 1 calc R . . H11B H 0.3754 0.7013 0.3842 0.027 Uiso 1 1 calc R . . C12 C 0.61342(17) 0.63479(16) 0.31456(8) 0.0230(4) Uani 1 1 d . . . H12A H 0.6083 0.6061 0.3616 0.028 Uiso 1 1 calc R . . H12B H 0.6922 0.6765 0.3042 0.028 Uiso 1 1 calc R . . C13 C 0.63590(16) 0.52460(15) 0.27841(8) 0.0204(4) Uani 1 1 d . . . C14 C 0.68637(17) 0.40554(16) 0.30734(9) 0.0252(4) Uani 1 1 d . . . H14A H 0.7063 0.3905 0.3515 0.030 Uiso 1 1 calc R . . C15 C 0.70734(19) 0.30925(17) 0.27122(9) 0.0301(4) Uani 1 1 d . . . H15A H 0.7423 0.2269 0.2900 0.036 Uiso 1 1 calc R . . C16 C 0.67674(19) 0.33440(17) 0.20721(9) 0.0307(4) Uani 1 1 d . . . H16A H 0.6897 0.2696 0.1813 0.037 Uiso 1 1 calc R . . C17 C 0.62720(18) 0.45477(16) 0.18165(9) 0.0255(4) Uani 1 1 d . . . H17A H 0.6060 0.4715 0.1377 0.031 Uiso 1 1 calc R . . C18 C 0.50005(18) 0.85152(16) 0.30280(8) 0.0250(4) Uani 1 1 d . . . H18A H 0.5366 0.8532 0.3447 0.030 Uiso 1 1 calc R . . H18B H 0.4091 0.9072 0.3013 0.030 Uiso 1 1 calc R . . C19 C 0.59474(17) 0.89654(15) 0.24804(8) 0.0229(4) Uani 1 1 d . . . C20 C 0.69046(18) 0.96454(16) 0.25630(9) 0.0276(4) Uani 1 1 d . . . H20A H 0.7007 0.9834 0.2979 0.033 Uiso 1 1 calc R . . C21 C 0.77096(19) 1.00459(16) 0.20326(10) 0.0308(4) Uani 1 1 d . . . H21A H 0.8389 1.0495 0.2081 0.037 Uiso 1 1 calc R . . C22 C 0.75143(19) 0.97851(17) 0.14342(10) 0.0310(4) Uani 1 1 d . . . H22A H 0.8034 1.0075 0.1060 0.037 Uiso 1 1 calc R . . C23 C 0.65477(18) 0.90938(17) 0.13869(9) 0.0281(4) Uani 1 1 d . . . H23A H 0.6413 0.8915 0.0973 0.034 Uiso 1 1 calc R . . C24 C 0.26765(17) 0.37324(15) 0.21419(8) 0.0219(4) Uani 1 1 d . . . H24A H 0.3400 0.3870 0.1797 0.026 Uiso 1 1 calc R . . H24B H 0.2659 0.2838 0.2213 0.026 Uiso 1 1 calc R . . C25 C 0.02181(17) 0.43333(16) 0.24349(8) 0.0220(4) Uani 1 1 d . . . H25A H 0.0417 0.3504 0.2694 0.026 Uiso 1 1 calc R . . H25B H -0.0647 0.4409 0.2230 0.026 Uiso 1 1 calc R . . C26 C 0.00370(16) 0.53006(15) 0.28760(8) 0.0205(4) Uani 1 1 d . . . C27 C -0.02370(18) 0.50303(17) 0.35357(9) 0.0264(4) Uani 1 1 d . . . H27A H -0.0274 0.4208 0.3726 0.032 Uiso 1 1 calc R . . C28 C -0.0456(2) 0.59690(18) 0.39124(9) 0.0331(4) Uani 1 1 d . . . H28A H -0.0649 0.5804 0.4366 0.040 Uiso 1 1 calc R . . C29 C -0.0390(2) 0.71549(18) 0.36209(9) 0.0325(4) Uani 1 1 d . . . H29A H -0.0544 0.7819 0.3870 0.039 Uiso 1 1 calc R . . C30 C -0.00960(18) 0.73550(16) 0.29649(9) 0.0255(4) Uani 1 1 d . . . H30A H -0.0030 0.8168 0.2768 0.031 Uiso 1 1 calc R . . C31 C 0.10320(18) 0.39726(16) 0.13481(8) 0.0230(4) Uani 1 1 d . . . H31A H 0.0730 0.3176 0.1480 0.028 Uiso 1 1 calc R . . H31B H 0.1870 0.3823 0.1056 0.028 Uiso 1 1 calc R . . C32 C -0.00708(17) 0.48879(16) 0.09946(8) 0.0207(4) Uani 1 1 d . . . C33 C -0.10078(17) 0.45099(17) 0.06703(8) 0.0243(4) Uani 1 1 d . . . H33A H -0.1001 0.3655 0.0680 0.029 Uiso 1 1 calc R . . C34 C -0.19543(18) 0.53988(18) 0.03320(8) 0.0275(4) Uani 1 1 d . . . H34A H -0.2610 0.5162 0.0107 0.033 Uiso 1 1 calc R . . C35 C -0.19358(18) 0.66332(18) 0.03246(8) 0.0278(4) Uani 1 1 d . . . H35A H -0.2571 0.7259 0.0092 0.033 Uiso 1 1 calc R . . C36 C -0.09747(18) 0.69393(17) 0.06627(8) 0.0253(4) Uani 1 1 d . . . H36A H -0.0962 0.7789 0.0658 0.030 Uiso 1 1 calc R . . C37 C 0.38901(17) 0.68728(16) 0.05725(8) 0.0232(4) Uani 1 1 d . . . C38 C 0.4169(2) 0.71803(18) -0.01640(9) 0.0312(4) Uani 1 1 d . . . C39 C 0.18159(18) 0.91030(16) 0.13922(9) 0.0261(4) Uani 1 1 d . . . C40 C 0.1543(2) 1.03617(18) 0.09625(10) 0.0360(5) Uani 1 1 d . . . Cl1 Cl 0.03598(5) 0.07303(4) 0.32402(2) 0.03359(12) Uani 1 1 d . . . O1A O 0.02417(19) 0.18006(14) 0.35465(7) 0.0534(4) Uani 1 1 d . . . O1B O 0.03601(18) 0.10819(16) 0.25554(7) 0.0565(4) Uani 1 1 d . . . O1C O -0.08039(18) 0.01857(15) 0.34621(9) 0.0617(5) Uani 1 1 d . . . O1D O 0.1565(2) -0.0129(2) 0.34051(10) 0.0837(7) Uani 1 1 d . . . N1S N 0.7861(3) 0.3736(2) 0.47682(11) 0.0709(7) Uani 1 1 d . . . C1S C 0.8221(2) 0.2704(2) 0.48845(10) 0.0453(5) Uani 1 1 d . . . C2S C 0.8662(3) 0.1389(2) 0.50232(14) 0.0669(7) Uani 1 1 d . . . H2S1 H 0.8425 0.1124 0.5480 0.100 Uiso 1 1 d R . . H2S2 H 0.9654 0.1165 0.4933 0.100 Uiso 1 1 d R . . H2S3 H 0.8206 0.0980 0.4754 0.100 Uiso 1 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 Mn1 0.02101(14) 0.02020(14) 0.01896(14) -0.00043(11) -0.00553(10) -0.00722(10) Mn2 0.02058(14) 0.01706(14) 0.01933(14) 0.00012(10) -0.00511(10) -0.00663(10) F4 0.0374(7) 0.0296(7) 0.0906(11) 0.0167(7) -0.0119(6) 0.0006(5) F1 0.0483(8) 0.0880(10) 0.0311(7) 0.0135(6) -0.0211(5) -0.0300(7) F5 0.0517(8) 0.0277(7) 0.1073(12) 0.0130(7) -0.0153(8) -0.0192(6) F2 0.1043(13) 0.1016(12) 0.0361(8) 0.0225(8) -0.0192(7) -0.0781(10) F3 0.0846(11) 0.1045(13) 0.0286(7) -0.0180(8) 0.0047(7) 0.0250(10) F6 0.1495(17) 0.0504(9) 0.0362(9) 0.0087(7) 0.0069(9) -0.0117(9) O1 0.0227(6) 0.0206(6) 0.0192(6) 0.0029(5) -0.0069(5) -0.0075(5) O2 0.0331(7) 0.0527(9) 0.0199(7) -0.0033(6) -0.0045(5) -0.0186(6) O3 0.0316(7) 0.0489(9) 0.0247(7) -0.0066(6) 0.0011(5) -0.0187(6) O4 0.0315(8) 0.0248(7) 0.0714(11) 0.0039(7) -0.0179(7) -0.0045(6) O5 0.0341(8) 0.0206(7) 0.0453(8) 0.0029(6) -0.0112(6) -0.0089(5) N1 0.0214(7) 0.0179(7) 0.0220(8) -0.0037(6) -0.0034(5) -0.0054(5) N2 0.0198(7) 0.0226(8) 0.0200(8) -0.0030(6) -0.0015(5) -0.0045(6) N3 0.0242(8) 0.0221(8) 0.0252(8) -0.0013(6) -0.0044(6) -0.0074(6) N4 0.0216(7) 0.0184(7) 0.0173(7) -0.0032(6) -0.0031(5) -0.0054(5) N5 0.0198(7) 0.0190(8) 0.0255(8) -0.0034(6) -0.0024(6) -0.0043(6) N6 0.0230(8) 0.0228(8) 0.0209(8) -0.0027(6) -0.0035(6) -0.0057(6) C1 0.0169(8) 0.0197(9) 0.0186(9) 0.0014(7) -0.0019(6) -0.0040(6) C2 0.0190(8) 0.0201(9) 0.0201(9) -0.0027(7) -0.0010(6) -0.0042(6) C3 0.0229(9) 0.0288(10) 0.0167(9) -0.0029(7) -0.0024(6) -0.0069(7) C4 0.0235(9) 0.0252(10) 0.0198(9) 0.0019(7) -0.0031(7) -0.0050(7) C5 0.0237(9) 0.0170(9) 0.0260(10) 0.0000(7) -0.0038(7) -0.0039(7) C6 0.0190(9) 0.0208(9) 0.0198(9) -0.0016(7) -0.0032(6) -0.0033(6) C7 0.0421(11) 0.0303(11) 0.0231(10) 0.0070(8) -0.0081(8) -0.0115(8) C8 0.0676(16) 0.0503(14) 0.0296(12) 0.0128(10) -0.0229(10) -0.0232(12) C9 0.0660(16) 0.0574(15) 0.0319(12) 0.0140(11) -0.0080(10) -0.0353(12) C10 0.0708(17) 0.0408(14) 0.0440(14) 0.0160(11) -0.0105(12) 0.0081(12) C11 0.0236(9) 0.0257(10) 0.0199(9) -0.0041(7) -0.0002(7) -0.0074(7) C12 0.0231(9) 0.0251(10) 0.0221(9) -0.0014(7) -0.0066(7) -0.0065(7) C13 0.0165(8) 0.0239(9) 0.0212(9) -0.0023(7) -0.0020(6) -0.0052(6) C14 0.0220(9) 0.0279(10) 0.0245(10) 0.0008(8) -0.0051(7) -0.0041(7) C15 0.0297(10) 0.0214(10) 0.0362(11) 0.0000(8) -0.0023(8) -0.0018(7) C16 0.0333(11) 0.0269(10) 0.0320(11) -0.0107(8) 0.0014(8) -0.0028(8) C17 0.0264(10) 0.0290(10) 0.0214(9) -0.0060(8) 0.0002(7) -0.0055(7) C18 0.0310(10) 0.0221(9) 0.0250(10) -0.0068(8) -0.0038(7) -0.0092(7) C19 0.0239(9) 0.0172(9) 0.0282(10) -0.0030(7) -0.0058(7) -0.0034(7) C20 0.0308(10) 0.0203(9) 0.0343(11) -0.0055(8) -0.0078(8) -0.0067(7) C21 0.0263(10) 0.0216(10) 0.0466(12) -0.0034(9) -0.0057(8) -0.0091(7) C22 0.0293(10) 0.0253(10) 0.0381(12) -0.0012(9) 0.0024(8) -0.0095(8) C23 0.0308(10) 0.0271(10) 0.0271(10) -0.0013(8) -0.0027(8) -0.0088(8) C24 0.0243(9) 0.0182(9) 0.0229(9) -0.0020(7) -0.0049(7) -0.0024(7) C25 0.0245(9) 0.0215(9) 0.0216(9) -0.0007(7) -0.0017(7) -0.0098(7) C26 0.0166(8) 0.0218(9) 0.0243(10) -0.0034(7) -0.0018(6) -0.0058(6) C27 0.0296(10) 0.0251(10) 0.0249(10) -0.0007(8) -0.0003(7) -0.0089(7) C28 0.0392(11) 0.0380(12) 0.0229(10) -0.0072(9) 0.0017(8) -0.0094(9) C29 0.0368(11) 0.0304(11) 0.0323(11) -0.0135(9) 0.0003(8) -0.0058(8) C30 0.0251(9) 0.0199(9) 0.0319(11) -0.0053(8) -0.0024(7) -0.0039(7) C31 0.0285(10) 0.0203(9) 0.0221(9) -0.0057(7) -0.0051(7) -0.0056(7) C32 0.0222(9) 0.0242(9) 0.0165(9) -0.0030(7) 0.0006(6) -0.0070(7) C33 0.0269(9) 0.0287(10) 0.0204(9) -0.0058(8) 0.0002(7) -0.0118(7) C34 0.0237(10) 0.0412(12) 0.0209(9) -0.0047(8) -0.0036(7) -0.0127(8) C35 0.0235(9) 0.0355(11) 0.0230(10) -0.0010(8) -0.0058(7) -0.0031(7) C36 0.0265(9) 0.0238(10) 0.0247(10) -0.0010(8) -0.0045(7) -0.0037(7) C37 0.0243(9) 0.0228(9) 0.0224(9) -0.0033(7) -0.0031(7) -0.0034(7) C38 0.0327(11) 0.0394(12) 0.0239(10) -0.0001(9) -0.0070(8) -0.0129(9) C39 0.0268(10) 0.0180(9) 0.0316(10) -0.0033(8) 0.0004(8) -0.0018(7) C40 0.0372(12) 0.0251(11) 0.0430(13) 0.0030(9) -0.0014(9) -0.0067(8) Cl1 0.0372(3) 0.0256(2) 0.0390(3) -0.0021(2) -0.0110(2) -0.00624(19) O1A 0.0881(13) 0.0364(9) 0.0456(9) -0.0081(7) -0.0110(8) -0.0299(8) O1B 0.0736(12) 0.0632(11) 0.0349(9) -0.0075(8) -0.0118(8) -0.0141(9) O1C 0.0655(12) 0.0522(10) 0.0783(13) -0.0081(9) -0.0047(9) -0.0366(9) O1D 0.0578(12) 0.0850(15) 0.0827(14) 0.0103(11) -0.0115(10) 0.0301(10) N1S 0.0960(19) 0.0590(16) 0.0511(14) -0.0066(12) 0.0219(12) -0.0139(13) C1S 0.0503(14) 0.0545(17) 0.0304(12) -0.0032(11) 0.0056(10) -0.0147(11) C2S 0.083(2) 0.0538(17) 0.0583(17) 0.0022(13) -0.0070(14) -0.0087(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 Mn2 3.5214(5) . ? Mn1 O1 2.0981(11) . ? Mn1 O2 2.1506(13) . ? Mn1 O4 2.1770(13) . ? Mn1 N3 2.2363(14) . ? Mn1 N2 2.2650(14) . ? Mn1 N1 2.3063(14) . ? Mn2 O1 2.1060(11) . ? Mn2 O5 2.1440(13) . ? Mn2 O3 2.2483(13) . ? Mn2 N6 2.2528(14) . ? Mn2 N5 2.2635(14) . ? Mn2 N4 2.2937(14) . ? F4 C40 1.322(2) . ? F1 C38 1.316(2) . ? F5 C40 1.327(2) . ? F2 C38 1.307(2) . ? F3 C38 1.324(2) . ? F6 C40 1.318(3) . ? O1 C1 1.3497(19) . ? O2 C37 1.243(2) . ? O3 C37 1.234(2) . ? O4 C39 1.227(2) . ? O5 C39 1.245(2) . ? N1 C18 1.475(2) . ? N1 C12 1.481(2) . ? N1 C11 1.487(2) . ? N2 C17 1.342(2) . ? N2 C13 1.344(2) . ? N3 C23 1.338(2) . ? N3 C19 1.342(2) . ? N4 C31 1.468(2) . ? N4 C25 1.483(2) . ? N4 C24 1.487(2) . ? N5 C30 1.340(2) . ? N5 C26 1.347(2) . ? N6 C36 1.339(2) . ? N6 C32 1.343(2) . ? C1 C2 1.401(2) . ? C1 C6 1.406(2) . ? C2 C3 1.391(2) . ? C2 C11 1.508(2) . ? C3 C4 1.387(2) . ? C3 H3A 0.950 . ? C4 C5 1.392(2) . ? C4 C7 1.533(2) . ? C5 C6 1.385(2) . ? C5 H5A 0.950 . ? C6 C24 1.503(2) . ? C7 C9 1.525(3) . ? C7 C8 1.529(3) . ? C7 C10 1.532(3) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 C13 1.509(2) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.385(2) . ? C14 C15 1.378(3) . ? C14 H14A 0.950 . ? C15 C16 1.381(3) . ? C15 H15A 0.950 . ? C16 C17 1.374(3) . ? C16 H16A 0.950 . ? C17 H17A 0.950 . ? C18 C19 1.509(2) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 C20 1.384(2) . ? C20 C21 1.381(3) . ? C20 H20A 0.950 . ? C21 C22 1.374(3) . ? C21 H21A 0.950 . ? C22 C23 1.382(3) . ? C22 H22A 0.950 . ? C23 H23A 0.950 . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 C26 1.500(2) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.383(2) . ? C27 C28 1.377(3) . ? C27 H27A 0.950 . ? C28 C29 1.382(3) . ? C28 H28A 0.950 . ? C29 C30 1.372(3) . ? C29 H29A 0.950 . ? C30 H30A 0.950 . ? C31 C32 1.508(2) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 C33 1.384(2) . ? C33 C34 1.383(3) . ? C33 H33A 0.950 . ? C34 C35 1.380(3) . ? C34 H34A 0.950 . ? C35 C36 1.381(2) . ? C35 H35A 0.950 . ? C36 H36A 0.950 . ? C37 C38 1.541(3) . ? C39 C40 1.535(3) . ? Cl1 O1D 1.4122(17) . ? Cl1 O1A 1.4204(15) . ? Cl1 O1B 1.4299(16) . ? Cl1 O1C 1.4334(16) . ? N1S C1S 1.128(3) . ? C1S C2S 1.433(4) . ? C2S H2S1 0.980 . ? C2S H2S2 0.980 . ? C2S H2S3 0.980 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O2 101.31(5) . . ? O1 Mn1 O4 90.26(5) . . ? O2 Mn1 O4 86.69(6) . . ? O1 Mn1 N3 159.24(5) . . ? O2 Mn1 N3 98.45(5) . . ? O4 Mn1 N3 84.56(5) . . ? O1 Mn1 N2 85.48(5) . . ? O2 Mn1 N2 92.35(5) . . ? O4 Mn1 N2 175.36(5) . . ? N3 Mn1 N2 100.07(5) . . ? O1 Mn1 N1 87.62(5) . . ? O2 Mn1 N1 164.40(5) . . ? O4 Mn1 N1 106.21(5) . . ? N3 Mn1 N1 74.65(5) . . ? N2 Mn1 N1 75.48(5) . . ? O1 Mn2 O5 104.47(5) . . ? O1 Mn2 O3 90.49(5) . . ? O5 Mn2 O3 87.21(5) . . ? O1 Mn2 N6 158.26(5) . . ? O5 Mn2 N6 96.35(5) . . ? O3 Mn2 N6 84.28(5) . . ? O1 Mn2 N5 84.46(5) . . ? O5 Mn2 N5 95.62(5) . . ? O3 Mn2 N5 174.69(5) . . ? N6 Mn2 N5 99.83(5) . . ? O1 Mn2 N4 86.48(5) . . ? O5 Mn2 N4 166.14(5) . . ? O3 Mn2 N4 101.38(5) . . ? N6 Mn2 N4 73.97(5) . . ? N5 Mn2 N4 76.73(5) . . ? C1 O1 Mn1 122.31(9) . . ? C1 O1 Mn2 123.90(9) . . ? Mn1 O1 Mn2 113.78(5) . . ? C37 O2 Mn1 125.33(11) . . ? C37 O3 Mn2 134.64(11) . . ? C39 O4 Mn1 139.31(13) . . ? C39 O5 Mn2 121.27(11) . . ? C18 N1 C12 110.75(13) . . ? C18 N1 C11 110.48(13) . . ? C12 N1 C11 111.76(13) . . ? C18 N1 Mn1 105.45(10) . . ? C12 N1 Mn1 109.37(10) . . ? C11 N1 Mn1 108.82(10) . . ? C17 N2 C13 117.89(15) . . ? C17 N2 Mn1 121.80(11) . . ? C13 N2 Mn1 114.95(11) . . ? C23 N3 C19 118.46(15) . . ? C23 N3 Mn1 125.12(12) . . ? C19 N3 Mn1 115.77(11) . . ? C31 N4 C25 109.32(13) . . ? C31 N4 C24 109.30(13) . . ? C25 N4 C24 111.66(13) . . ? C31 N4 Mn2 107.88(10) . . ? C25 N4 Mn2 108.11(10) . . ? C24 N4 Mn2 110.49(10) . . ? C30 N5 C26 118.08(15) . . ? C30 N5 Mn2 123.21(11) . . ? C26 N5 Mn2 113.21(11) . . ? C36 N6 C32 118.43(14) . . ? C36 N6 Mn2 125.18(11) . . ? C32 N6 Mn2 116.16(11) . . ? O1 C1 C2 120.69(14) . . ? O1 C1 C6 120.70(14) . . ? C2 C1 C6 118.61(15) . . ? C3 C2 C1 119.79(15) . . ? C3 C2 C11 120.07(15) . . ? C1 C2 C11 120.13(15) . . ? C4 C3 C2 122.45(15) . . ? C4 C3 H3A 118.8 . . ? C2 C3 H3A 118.8 . . ? C3 C4 C5 116.78(15) . . ? C3 C4 C7 123.43(16) . . ? C5 C4 C7 119.78(16) . . ? C6 C5 C4 122.67(16) . . ? C6 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? C5 C6 C1 119.65(15) . . ? C5 C6 C24 120.24(15) . . ? C1 C6 C24 120.11(15) . . ? C9 C7 C8 107.93(17) . . ? C9 C7 C10 110.54(19) . . ? C8 C7 C10 108.11(19) . . ? C9 C7 C4 109.96(16) . . ? C8 C7 C4 111.86(16) . . ? C10 C7 C4 108.43(16) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C2 112.00(13) . . ? N1 C11 H11A 109.2 . . ? C2 C11 H11A 109.2 . . ? N1 C11 H11B 109.2 . . ? C2 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N1 C12 C13 111.83(13) . . ? N1 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? N1 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? N2 C13 C14 122.20(16) . . ? N2 C13 C12 115.74(14) . . ? C14 C13 C12 122.03(15) . . ? C15 C14 C13 119.14(16) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C14 C15 C16 118.90(17) . . ? C14 C15 H15A 120.6 . . ? C16 C15 H15A 120.6 . . ? C17 C16 C15 118.84(17) . . ? C17 C16 H16A 120.6 . . ? C15 C16 H16A 120.6 . . ? N2 C17 C16 123.02(17) . . ? N2 C17 H17A 118.5 . . ? C16 C17 H17A 118.5 . . ? N1 C18 C19 110.30(14) . . ? N1 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? N1 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? N3 C19 C20 121.81(16) . . ? N3 C19 C18 115.29(15) . . ? C20 C19 C18 122.90(16) . . ? C21 C20 C19 119.16(17) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C22 C21 C20 119.09(17) . . ? C22 C21 H21A 120.5 . . ? C20 C21 H21A 120.5 . . ? C21 C22 C23 118.73(18) . . ? C21 C22 H22A 120.6 . . ? C23 C22 H22A 120.6 . . ? N3 C23 C22 122.65(17) . . ? N3 C23 H23A 118.7 . . ? C22 C23 H23A 118.7 . . ? N4 C24 C6 112.65(13) . . ? N4 C24 H24A 109.1 . . ? C6 C24 H24A 109.1 . . ? N4 C24 H24B 109.1 . . ? C6 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? N4 C25 C26 112.63(13) . . ? N4 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? N4 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? N5 C26 C27 122.01(15) . . ? N5 C26 C25 116.18(14) . . ? C27 C26 C25 121.76(15) . . ? C28 C27 C26 119.12(17) . . ? C28 C27 H27A 120.4 . . ? C26 C27 H27A 120.4 . . ? C27 C28 C29 119.06(17) . . ? C27 C28 H28A 120.5 . . ? C29 C28 H28A 120.5 . . ? C30 C29 C28 118.76(17) . . ? C30 C29 H29A 120.6 . . ? C28 C29 H29A 120.6 . . ? N5 C30 C29 122.94(17) . . ? N5 C30 H30A 118.5 . . ? C29 C30 H30A 118.5 . . ? N4 C31 C32 110.75(13) . . ? N4 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? N4 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? N6 C32 C33 122.17(16) . . ? N6 C32 C31 115.99(14) . . ? C33 C32 C31 121.80(15) . . ? C34 C33 C32 118.80(17) . . ? C34 C33 H33A 120.6 . . ? C32 C33 H33A 120.6 . . ? C35 C34 C33 119.29(16) . . ? C35 C34 H34A 120.4 . . ? C33 C34 H34A 120.4 . . ? C34 C35 C36 118.59(16) . . ? C34 C35 H35A 120.7 . . ? C36 C35 H35A 120.7 . . ? N6 C36 C35 122.71(17) . . ? N6 C36 H36A 118.6 . . ? C35 C36 H36A 118.6 . . ? O3 C37 O2 129.80(17) . . ? O3 C37 C38 116.17(15) . . ? O2 C37 C38 114.02(15) . . ? F2 C38 F1 107.51(16) . . ? F2 C38 F3 106.56(18) . . ? F1 C38 F3 105.84(16) . . ? F2 C38 C37 112.69(15) . . ? F1 C38 C37 113.00(15) . . ? F3 C38 C37 110.80(15) . . ? O4 C39 O5 129.48(17) . . ? O4 C39 C40 115.76(16) . . ? O5 C39 C40 114.68(16) . . ? F6 C40 F4 108.14(18) . . ? F6 C40 F5 106.48(18) . . ? F4 C40 F5 105.41(16) . . ? F6 C40 C39 109.74(16) . . ? F4 C40 C39 113.55(16) . . ? F5 C40 C39 113.14(17) . . ? O1D Cl1 O1A 110.19(13) . . ? O1D Cl1 O1B 110.76(12) . . ? O1A Cl1 O1B 109.39(10) . . ? O1D Cl1 O1C 109.44(13) . . ? O1A Cl1 O1C 107.90(10) . . ? O1B Cl1 O1C 109.11(11) . . ? N1S C1S C2S 178.9(3) . . ? C1S C2S H2S1 109.1 . . ? C1S C2S H2S2 109.7 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.6 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Mn1 O1 C1 133.27(12) . . . . ? O4 Mn1 O1 C1 -140.06(12) . . . . ? N3 Mn1 O1 C1 -64.86(19) . . . . ? N2 Mn1 O1 C1 41.77(12) . . . . ? N1 Mn1 O1 C1 -33.85(12) . . . . ? O2 Mn1 O1 Mn2 -46.02(7) . . . . ? O4 Mn1 O1 Mn2 40.65(6) . . . . ? N3 Mn1 O1 Mn2 115.85(13) . . . . ? N2 Mn1 O1 Mn2 -137.51(6) . . . . ? N1 Mn1 O1 Mn2 146.87(6) . . . . ? O5 Mn2 O1 C1 139.45(12) . . . . ? O3 Mn2 O1 C1 -133.30(12) . . . . ? N6 Mn2 O1 C1 -57.66(19) . . . . ? N5 Mn2 O1 C1 45.06(12) . . . . ? N4 Mn2 O1 C1 -31.93(12) . . . . ? O5 Mn2 O1 Mn1 -41.27(7) . . . . ? O3 Mn2 O1 Mn1 45.97(6) . . . . ? N6 Mn2 O1 Mn1 121.62(12) . . . . ? N5 Mn2 O1 Mn1 -135.67(6) . . . . ? N4 Mn2 O1 Mn1 147.34(6) . . . . ? O1 Mn1 O2 C37 27.47(15) . . . . ? O4 Mn1 O2 C37 -62.13(15) . . . . ? N3 Mn1 O2 C37 -146.13(15) . . . . ? N2 Mn1 O2 C37 113.32(15) . . . . ? N1 Mn1 O2 C37 151.47(17) . . . . ? O1 Mn2 O3 C37 -43.08(17) . . . . ? O5 Mn2 O3 C37 61.38(17) . . . . ? N6 Mn2 O3 C37 158.06(17) . . . . ? N4 Mn2 O3 C37 -129.59(17) . . . . ? O1 Mn1 O4 C39 -44.6(2) . . . . ? O2 Mn1 O4 C39 56.7(2) . . . . ? N3 Mn1 O4 C39 155.5(2) . . . . ? N1 Mn1 O4 C39 -132.2(2) . . . . ? O1 Mn2 O5 C39 25.25(15) . . . . ? O3 Mn2 O5 C39 -64.54(14) . . . . ? N6 Mn2 O5 C39 -148.46(14) . . . . ? N5 Mn2 O5 C39 110.96(14) . . . . ? N4 Mn2 O5 C39 166.62(18) . . . . ? O1 Mn1 N1 C18 -138.90(10) . . . . ? O2 Mn1 N1 C18 95.5(2) . . . . ? O4 Mn1 N1 C18 -49.33(11) . . . . ? N3 Mn1 N1 C18 30.18(10) . . . . ? N2 Mn1 N1 C18 135.16(11) . . . . ? O1 Mn1 N1 C12 101.97(10) . . . . ? O2 Mn1 N1 C12 -23.6(2) . . . . ? O4 Mn1 N1 C12 -168.45(10) . . . . ? N3 Mn1 N1 C12 -88.94(10) . . . . ? N2 Mn1 N1 C12 16.03(10) . . . . ? O1 Mn1 N1 C11 -20.36(10) . . . . ? O2 Mn1 N1 C11 -145.92(17) . . . . ? O4 Mn1 N1 C11 69.21(11) . . . . ? N3 Mn1 N1 C11 148.72(11) . . . . ? N2 Mn1 N1 C11 -106.30(10) . . . . ? O1 Mn1 N2 C17 69.99(13) . . . . ? O2 Mn1 N2 C17 -31.17(13) . . . . ? N3 Mn1 N2 C17 -130.18(13) . . . . ? N1 Mn1 N2 C17 158.70(13) . . . . ? O1 Mn1 N2 C13 -83.59(11) . . . . ? O2 Mn1 N2 C13 175.24(11) . . . . ? N3 Mn1 N2 C13 76.23(12) . . . . ? N1 Mn1 N2 C13 5.12(11) . . . . ? O1 Mn1 N3 C23 -167.52(13) . . . . ? O2 Mn1 N3 C23 -5.48(15) . . . . ? O4 Mn1 N3 C23 -91.30(15) . . . . ? N2 Mn1 N3 C23 88.44(14) . . . . ? N1 Mn1 N3 C23 160.22(15) . . . . ? O1 Mn1 N3 C19 21.9(2) . . . . ? O2 Mn1 N3 C19 -176.06(12) . . . . ? O4 Mn1 N3 C19 98.11(13) . . . . ? N2 Mn1 N3 C19 -82.14(12) . . . . ? N1 Mn1 N3 C19 -10.37(12) . . . . ? O1 Mn2 N4 C31 -141.42(10) . . . . ? O5 Mn2 N4 C31 75.9(2) . . . . ? O3 Mn2 N4 C31 -51.63(11) . . . . ? N6 Mn2 N4 C31 28.96(10) . . . . ? N5 Mn2 N4 C31 133.45(11) . . . . ? O1 Mn2 N4 C25 100.47(10) . . . . ? O5 Mn2 N4 C25 -42.3(3) . . . . ? O3 Mn2 N4 C25 -169.74(10) . . . . ? N6 Mn2 N4 C25 -89.16(10) . . . . ? N5 Mn2 N4 C25 15.34(10) . . . . ? O1 Mn2 N4 C24 -21.99(10) . . . . ? O5 Mn2 N4 C24 -164.72(19) . . . . ? O3 Mn2 N4 C24 67.80(10) . . . . ? N6 Mn2 N4 C24 148.38(11) . . . . ? N5 Mn2 N4 C24 -107.13(10) . . . . ? O1 Mn2 N5 C30 71.51(13) . . . . ? O5 Mn2 N5 C30 -32.54(13) . . . . ? N6 Mn2 N5 C30 -130.00(13) . . . . ? N4 Mn2 N5 C30 159.19(14) . . . . ? O1 Mn2 N5 C26 -81.71(11) . . . . ? O5 Mn2 N5 C26 174.24(11) . . . . ? N6 Mn2 N5 C26 76.78(11) . . . . ? N4 Mn2 N5 C26 5.97(11) . . . . ? O1 Mn2 N6 C36 -170.41(13) . . . . ? O5 Mn2 N6 C36 -7.06(14) . . . . ? O3 Mn2 N6 C36 -93.60(14) . . . . ? N5 Mn2 N6 C36 89.79(14) . . . . ? N4 Mn2 N6 C36 162.80(14) . . . . ? O1 Mn2 N6 C32 15.2(2) . . . . ? O5 Mn2 N6 C32 178.53(12) . . . . ? O3 Mn2 N6 C32 91.99(12) . . . . ? N5 Mn2 N6 C32 -84.62(12) . . . . ? N4 Mn2 N6 C32 -11.61(11) . . . . ? Mn1 O1 C1 C2 49.34(19) . . . . ? Mn2 O1 C1 C2 -131.44(13) . . . . ? Mn1 O1 C1 C6 -130.13(13) . . . . ? Mn2 O1 C1 C6 49.08(19) . . . . ? O1 C1 C2 C3 -178.27(14) . . . . ? C6 C1 C2 C3 1.2(2) . . . . ? O1 C1 C2 C11 0.9(2) . . . . ? C6 C1 C2 C11 -179.58(15) . . . . ? C1 C2 C3 C4 0.7(3) . . . . ? C11 C2 C3 C4 -178.53(15) . . . . ? C2 C3 C4 C5 -2.1(2) . . . . ? C2 C3 C4 C7 176.56(16) . . . . ? C3 C4 C5 C6 1.8(3) . . . . ? C7 C4 C5 C6 -176.97(16) . . . . ? C4 C5 C6 C1 0.1(3) . . . . ? C4 C5 C6 C24 179.25(16) . . . . ? O1 C1 C6 C5 177.92(14) . . . . ? C2 C1 C6 C5 -1.6(2) . . . . ? O1 C1 C6 C24 -1.3(2) . . . . ? C2 C1 C6 C24 179.24(15) . . . . ? C3 C4 C7 C9 119.6(2) . . . . ? C5 C4 C7 C9 -61.7(2) . . . . ? C3 C4 C7 C8 -0.3(3) . . . . ? C5 C4 C7 C8 178.38(18) . . . . ? C3 C4 C7 C10 -119.4(2) . . . . ? C5 C4 C7 C10 59.3(2) . . . . ? C18 N1 C11 C2 -179.62(14) . . . . ? C12 N1 C11 C2 -55.82(18) . . . . ? Mn1 N1 C11 C2 65.06(15) . . . . ? C3 C2 C11 N1 113.42(17) . . . . ? C1 C2 C11 N1 -65.8(2) . . . . ? C18 N1 C12 C13 -149.52(14) . . . . ? C11 N1 C12 C13 86.83(16) . . . . ? Mn1 N1 C12 C13 -33.73(15) . . . . ? C17 N2 C13 C14 1.1(2) . . . . ? Mn1 N2 C13 C14 155.75(13) . . . . ? C17 N2 C13 C12 179.32(14) . . . . ? Mn1 N2 C13 C12 -26.01(17) . . . . ? N1 C12 C13 N2 41.1(2) . . . . ? N1 C12 C13 C14 -140.69(16) . . . . ? N2 C13 C14 C15 -0.5(3) . . . . ? C12 C13 C14 C15 -178.60(16) . . . . ? C13 C14 C15 C16 -0.3(3) . . . . ? C14 C15 C16 C17 0.4(3) . . . . ? C13 N2 C17 C16 -1.0(2) . . . . ? Mn1 N2 C17 C16 -153.81(14) . . . . ? C15 C16 C17 N2 0.2(3) . . . . ? C12 N1 C18 C19 72.06(17) . . . . ? C11 N1 C18 C19 -163.57(14) . . . . ? Mn1 N1 C18 C19 -46.14(15) . . . . ? C23 N3 C19 C20 -3.3(3) . . . . ? Mn1 N3 C19 C20 167.94(13) . . . . ? C23 N3 C19 C18 176.34(15) . . . . ? Mn1 N3 C19 C18 -12.42(19) . . . . ? N1 C18 C19 N3 41.1(2) . . . . ? N1 C18 C19 C20 -139.23(16) . . . . ? N3 C19 C20 C21 1.1(3) . . . . ? C18 C19 C20 C21 -178.50(16) . . . . ? C19 C20 C21 C22 1.6(3) . . . . ? C20 C21 C22 C23 -2.1(3) . . . . ? C19 N3 C23 C22 2.8(3) . . . . ? Mn1 N3 C23 C22 -167.56(14) . . . . ? C21 C22 C23 N3 -0.1(3) . . . . ? C31 N4 C24 C6 -176.33(14) . . . . ? C25 N4 C24 C6 -55.25(18) . . . . ? Mn2 N4 C24 C6 65.10(15) . . . . ? C5 C6 C24 N4 118.79(17) . . . . ? C1 C6 C24 N4 -62.0(2) . . . . ? C31 N4 C25 C26 -150.92(14) . . . . ? C24 N4 C25 C26 88.01(16) . . . . ? Mn2 N4 C25 C26 -33.73(15) . . . . ? C30 N5 C26 C27 0.6(2) . . . . ? Mn2 N5 C26 C27 155.27(13) . . . . ? C30 N5 C26 C25 177.99(14) . . . . ? Mn2 N5 C26 C25 -27.30(17) . . . . ? N4 C25 C26 N5 42.6(2) . . . . ? N4 C25 C26 C27 -139.94(16) . . . . ? N5 C26 C27 C28 0.3(3) . . . . ? C25 C26 C27 C28 -177.02(16) . . . . ? C26 C27 C28 C29 -0.3(3) . . . . ? C27 C28 C29 C30 -0.5(3) . . . . ? C26 N5 C30 C29 -1.4(2) . . . . ? Mn2 N5 C30 C29 -153.45(14) . . . . ? C28 C29 C30 N5 1.4(3) . . . . ? C25 N4 C31 C32 74.77(17) . . . . ? C24 N4 C31 C32 -162.74(13) . . . . ? Mn2 N4 C31 C32 -42.56(15) . . . . ? C36 N6 C32 C33 -1.2(2) . . . . ? Mn2 N6 C32 C33 173.58(12) . . . . ? C36 N6 C32 C31 176.72(15) . . . . ? Mn2 N6 C32 C31 -8.48(18) . . . . ? N4 C31 C32 N6 35.3(2) . . . . ? N4 C31 C32 C33 -146.75(16) . . . . ? N6 C32 C33 C34 0.7(3) . . . . ? C31 C32 C33 C34 -177.15(15) . . . . ? C32 C33 C34 C35 0.3(3) . . . . ? C33 C34 C35 C36 -0.6(3) . . . . ? C32 N6 C36 C35 0.9(3) . . . . ? Mn2 N6 C36 C35 -173.44(13) . . . . ? C34 C35 C36 N6 0.1(3) . . . . ? Mn2 O3 C37 O2 30.5(3) . . . . ? Mn2 O3 C37 C38 -150.87(13) . . . . ? Mn1 O2 C37 O3 -19.0(3) . . . . ? Mn1 O2 C37 C38 162.33(12) . . . . ? O3 C37 C38 F2 145.52(18) . . . . ? O2 C37 C38 F2 -35.6(2) . . . . ? O3 C37 C38 F1 23.4(2) . . . . ? O2 C37 C38 F1 -157.74(16) . . . . ? O3 C37 C38 F3 -95.2(2) . . . . ? O2 C37 C38 F3 83.7(2) . . . . ? Mn1 O4 C39 O5 35.3(3) . . . . ? Mn1 O4 C39 C40 -141.11(17) . . . . ? Mn2 O5 C39 O4 -19.8(3) . . . . ? Mn2 O5 C39 C40 156.70(12) . . . . ? O4 C39 C40 F6 102.3(2) . . . . ? O5 C39 C40 F6 -74.7(2) . . . . ? O4 C39 C40 F4 -136.56(19) . . . . ? O5 C39 C40 F4 46.5(2) . . . . ? O4 C39 C40 F5 -16.5(3) . . . . ? O5 C39 C40 F5 166.57(17) . . . . ? #============================================================================== data_12_MeCN _database_code_depnum_ccdc_archive 'CCDC 772408' #TrackingRef '- submit_all.cif' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H45 Co2 N6 O5 +, Cl O4 -, C2 H3 N' _chemical_formula_sum 'C42 H48 Cl Co2 N7 O9' _chemical_formula_weight 948.18 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' Cl Cl 0.1484 0.1585 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 12.0489(5) _cell_length_b 21.8143(10) _cell_length_c 16.8981(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.195(2) _cell_angle_gamma 90.00 _cell_volume 4415.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5679 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 22.60 _exptl_crystal_description plate _exptl_crystal_colour pink _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.958 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ? _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 70379 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0508 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 25.83 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.83 _diffrn_measured_fraction_theta_full 0.976 _reflns_number_total 8318 _reflns_number_gt 5766 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+1.7662P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8318 _refine_ls_number_parameters 555 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.527 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.063 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.45203(3) 0.192116(16) 0.58168(2) 0.02521(11) Uani 1 1 d . . . Co2 Co 0.54909(3) 0.262084(16) 0.75531(2) 0.02574(11) Uani 1 1 d . . . O1 O 0.54454(14) 0.25951(8) 0.63630(10) 0.0258(4) Uani 1 1 d . . . O2 O 0.31888(15) 0.19208(9) 0.64596(11) 0.0345(5) Uani 1 1 d . . . O3 O 0.37372(16) 0.25772(10) 0.74394(12) 0.0429(5) Uani 1 1 d . . . O4 O 0.53399(15) 0.12446(8) 0.65827(10) 0.0333(5) Uani 1 1 d . . . O5 O 0.56867(16) 0.17113(8) 0.77627(10) 0.0348(5) Uani 1 1 d . . . N1 N 0.56904(19) 0.18846(9) 0.49114(12) 0.0276(5) Uani 1 1 d . . . N2 N 0.38380(19) 0.26134(10) 0.49939(13) 0.0309(5) Uani 1 1 d . . . N3 N 0.39477(19) 0.11544(10) 0.51100(12) 0.0308(5) Uani 1 1 d . . . N4 N 0.54817(17) 0.36225(10) 0.75326(12) 0.0283(5) Uani 1 1 d . . . N5 N 0.72317(18) 0.28112(10) 0.75787(12) 0.0255(5) Uani 1 1 d . . . N6 N 0.52689(19) 0.28477(11) 0.87445(13) 0.0320(5) Uani 1 1 d . . . C1 C 0.5982(2) 0.30159(11) 0.59611(15) 0.0252(6) Uani 1 1 d . . . C2 C 0.6668(2) 0.28345(12) 0.53896(15) 0.0268(6) Uani 1 1 d . . . C3 C 0.7223(2) 0.32732(12) 0.49867(16) 0.0312(6) Uani 1 1 d . . . H3A H 0.7695 0.3143 0.4604 0.037 Uiso 1 1 calc R . . C4 C 0.7110(2) 0.38996(12) 0.51251(16) 0.0315(6) Uani 1 1 d . . . C5 C 0.6405(2) 0.40659(12) 0.56911(16) 0.0307(6) Uani 1 1 d . . . H5A H 0.6305 0.4490 0.5793 0.037 Uiso 1 1 calc R . . C6 C 0.5845(2) 0.36449(11) 0.61118(15) 0.0264(6) Uani 1 1 d . . . C7 C 0.7716(3) 0.43978(13) 0.46901(18) 0.0400(7) Uani 1 1 d . . . C8 C 0.6849(3) 0.48018(15) 0.4215(2) 0.0518(9) Uani 1 1 d . . . H8A H 0.7228 0.5128 0.3950 0.078 Uiso 1 1 calc R . . H8B H 0.6356 0.4984 0.4576 0.078 Uiso 1 1 calc R . . H8C H 0.6406 0.4553 0.3815 0.078 Uiso 1 1 calc R . . C9 C 0.8487(3) 0.41230(16) 0.4126(2) 0.0626(10) Uani 1 1 d . . . H9A H 0.8859 0.4454 0.3864 0.094 Uiso 1 1 calc R . . H9B H 0.8048 0.3874 0.3723 0.094 Uiso 1 1 calc R . . H9C H 0.9048 0.3865 0.4428 0.094 Uiso 1 1 calc R . . C10 C 0.8421(3) 0.47880(15) 0.5304(2) 0.0530(9) Uani 1 1 d . . . H10A H 0.8806 0.5107 0.5030 0.080 Uiso 1 1 calc R . . H10B H 0.8974 0.4528 0.5611 0.080 Uiso 1 1 calc R . . H10C H 0.7937 0.4979 0.5664 0.080 Uiso 1 1 calc R . . C11 C 0.6783(2) 0.21607(12) 0.52175(16) 0.0298(6) Uani 1 1 d . . . H11A H 0.7319 0.2105 0.4819 0.036 Uiso 1 1 calc R . . H11B H 0.7083 0.1946 0.5711 0.036 Uiso 1 1 calc R . . C12 C 0.5188(2) 0.22099(13) 0.41875(15) 0.0336(7) Uani 1 1 d . . . H12A H 0.4747 0.1916 0.3835 0.040 Uiso 1 1 calc R . . H12B H 0.5790 0.2375 0.3894 0.040 Uiso 1 1 calc R . . C13 C 0.4446(2) 0.27262(12) 0.43924(15) 0.0302(6) Uani 1 1 d . . . C14 C 0.4365(3) 0.32745(13) 0.39718(17) 0.0403(8) Uani 1 1 d . . . H14A H 0.4821 0.3348 0.3557 0.048 Uiso 1 1 calc R . . C15 C 0.3613(3) 0.37093(14) 0.4166(2) 0.0491(9) Uani 1 1 d . . . H15A H 0.3540 0.4087 0.3884 0.059 Uiso 1 1 calc R . . C16 C 0.2970(3) 0.35907(14) 0.4772(2) 0.0495(9) Uani 1 1 d . . . H16A H 0.2437 0.3882 0.4908 0.059 Uiso 1 1 calc R . . C17 C 0.3107(2) 0.30463(13) 0.51782(18) 0.0384(7) Uani 1 1 d . . . H17A H 0.2671 0.2971 0.5604 0.046 Uiso 1 1 calc R . . C18 C 0.5824(2) 0.12253(12) 0.47481(17) 0.0331(7) Uani 1 1 d . . . H18A H 0.6317 0.1035 0.5187 0.040 Uiso 1 1 calc R . . H18B H 0.6177 0.1173 0.4250 0.040 Uiso 1 1 calc R . . C19 C 0.4697(3) 0.09130(12) 0.46696(16) 0.0337(7) Uani 1 1 d . . . C20 C 0.4454(3) 0.04039(13) 0.41896(17) 0.0401(7) Uani 1 1 d . . . H20A H 0.4998 0.0239 0.3882 0.048 Uiso 1 1 calc R . . C21 C 0.3414(3) 0.01417(13) 0.41671(17) 0.0445(8) Uani 1 1 d . . . H21A H 0.3231 -0.0207 0.3842 0.053 Uiso 1 1 calc R . . C22 C 0.2639(3) 0.03869(14) 0.46191(17) 0.0426(8) Uani 1 1 d . . . H22A H 0.1918 0.0209 0.4613 0.051 Uiso 1 1 calc R . . C23 C 0.2932(2) 0.08993(13) 0.50838(16) 0.0357(7) Uani 1 1 d . . . H23A H 0.2397 0.1074 0.5392 0.043 Uiso 1 1 calc R . . C24 C 0.5089(2) 0.38415(12) 0.67186(15) 0.0307(6) Uani 1 1 d . . . H24A H 0.5044 0.4295 0.6723 0.037 Uiso 1 1 calc R . . H24B H 0.4329 0.3681 0.6562 0.037 Uiso 1 1 calc R . . C25 C 0.6625(2) 0.38417(12) 0.77982(16) 0.0310(6) Uani 1 1 d . . . H25A H 0.6714 0.3883 0.8385 0.037 Uiso 1 1 calc R . . H25B H 0.6734 0.4252 0.7567 0.037 Uiso 1 1 calc R . . C26 C 0.7499(2) 0.34111(12) 0.75533(15) 0.0280(6) Uani 1 1 d . . . C27 C 0.8501(2) 0.36102(13) 0.73272(16) 0.0337(7) Uani 1 1 d . . . H27A H 0.8667 0.4036 0.7313 0.040 Uiso 1 1 calc R . . C28 C 0.9263(2) 0.31817(14) 0.71215(17) 0.0373(7) Uani 1 1 d . . . H28A H 0.9964 0.3307 0.6969 0.045 Uiso 1 1 calc R . . C29 C 0.8991(2) 0.25704(14) 0.71405(16) 0.0351(7) Uani 1 1 d . . . H29A H 0.9500 0.2268 0.6997 0.042 Uiso 1 1 calc R . . C30 C 0.7979(2) 0.24036(12) 0.73676(15) 0.0296(6) Uani 1 1 d . . . H30A H 0.7797 0.1980 0.7376 0.036 Uiso 1 1 calc R . . C31 C 0.4706(2) 0.38028(13) 0.81062(16) 0.0355(7) Uani 1 1 d . . . H31A H 0.3927 0.3745 0.7865 0.043 Uiso 1 1 calc R . . H31B H 0.4812 0.4242 0.8241 0.043 Uiso 1 1 calc R . . C32 C 0.4908(2) 0.34224(13) 0.88513(16) 0.0342(7) Uani 1 1 d . . . C33 C 0.4709(3) 0.36318(16) 0.95947(18) 0.0457(8) Uani 1 1 d . . . H33A H 0.4468 0.4041 0.9663 0.055 Uiso 1 1 calc R . . C34 C 0.4866(3) 0.32399(18) 1.0234(2) 0.0604(10) Uani 1 1 d . . . H34A H 0.4733 0.3377 1.0749 0.072 Uiso 1 1 calc R . . C35 C 0.5215(3) 0.26467(18) 1.01250(19) 0.0561(9) Uani 1 1 d . . . H35A H 0.5316 0.2367 1.0558 0.067 Uiso 1 1 calc R . . C36 C 0.5414(3) 0.24703(15) 0.93686(17) 0.0424(8) Uani 1 1 d . . . H36A H 0.5664 0.2064 0.9289 0.051 Uiso 1 1 calc R . . C37 C 0.3038(2) 0.22356(13) 0.70626(16) 0.0304(6) Uani 1 1 d . . . C38 C 0.1911(3) 0.22078(18) 0.7353(2) 0.0568(10) Uani 1 1 d . . . H38A H 0.1616 0.2624 0.7391 0.085 Uiso 1 1 calc R . . H38B H 0.1972 0.2013 0.7878 0.085 Uiso 1 1 calc R . . H38C H 0.1406 0.1968 0.6979 0.085 Uiso 1 1 calc R . . C39 C 0.5634(2) 0.12485(12) 0.73168(16) 0.0270(6) Uani 1 1 d . . . C40 C 0.5963(3) 0.06465(13) 0.77147(16) 0.0366(7) Uani 1 1 d . . . H40A H 0.5485 0.0319 0.7471 0.055 Uiso 1 1 calc R . . H40B H 0.5874 0.0673 0.8283 0.055 Uiso 1 1 calc R . . H40C H 0.6745 0.0556 0.7648 0.055 Uiso 1 1 calc R . . Cl1 Cl 0.92759(6) 0.06696(3) 0.69299(5) 0.0418(2) Uani 1 1 d . . . O1A O 1.01145(19) 0.10976(10) 0.72257(15) 0.0604(7) Uani 1 1 d . . . O1B O 0.8983(3) 0.02911(11) 0.75658(16) 0.0751(8) Uani 1 1 d . . . O1C O 0.9682(2) 0.02973(11) 0.63241(14) 0.0619(7) Uani 1 1 d . . . O1D O 0.83103(19) 0.09984(11) 0.65951(16) 0.0646(7) Uani 1 1 d . . . N1S N 0.1485(4) 0.4296(2) 0.7560(4) 0.138(2) Uani 1 1 d . . . C1S C 0.1890(4) 0.4740(3) 0.7761(3) 0.0786(13) Uani 1 1 d . . . C2S C 0.2404(4) 0.5318(2) 0.7999(2) 0.0886(14) Uani 1 1 d . . . H2S1 H 0.1825 0.5615 0.8102 0.133 Uiso 1 1 d R . . H2S2 H 0.2917 0.5260 0.8484 0.133 Uiso 1 1 d R . . H2S3 H 0.2819 0.5473 0.7573 0.133 Uiso 1 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 Co1 0.0307(2) 0.01967(19) 0.02436(19) -0.00271(15) -0.00112(15) -0.00220(16) Co2 0.0304(2) 0.0220(2) 0.02465(19) -0.00521(15) 0.00189(15) -0.00180(16) O1 0.0315(10) 0.0215(9) 0.0241(9) -0.0024(8) 0.0014(8) -0.0032(8) O2 0.0330(11) 0.0354(11) 0.0354(11) -0.0068(9) 0.0048(9) -0.0065(9) O3 0.0330(12) 0.0481(13) 0.0484(12) -0.0192(10) 0.0084(10) -0.0063(10) O4 0.0455(12) 0.0242(10) 0.0287(11) -0.0019(8) -0.0036(9) 0.0025(9) O5 0.0530(13) 0.0230(10) 0.0281(10) -0.0030(8) 0.0024(9) -0.0037(9) N1 0.0381(13) 0.0172(11) 0.0267(12) -0.0045(9) 0.0000(10) -0.0005(10) N2 0.0342(13) 0.0242(12) 0.0320(13) -0.0018(10) -0.0070(11) -0.0016(11) N3 0.0392(14) 0.0256(13) 0.0254(12) -0.0003(10) -0.0063(10) -0.0037(11) N4 0.0291(12) 0.0252(12) 0.0302(12) -0.0065(10) 0.0012(10) 0.0011(10) N5 0.0303(13) 0.0201(12) 0.0245(11) -0.0040(9) -0.0037(9) 0.0022(10) N6 0.0360(14) 0.0314(13) 0.0285(13) -0.0060(10) 0.0029(10) -0.0024(11) C1 0.0273(14) 0.0238(14) 0.0228(13) 0.0011(11) -0.0045(11) -0.0021(12) C2 0.0281(15) 0.0217(14) 0.0297(14) -0.0029(11) -0.0010(12) -0.0008(12) C3 0.0343(16) 0.0296(16) 0.0299(15) -0.0028(12) 0.0044(12) -0.0009(13) C4 0.0344(16) 0.0263(15) 0.0331(15) 0.0021(12) 0.0003(13) -0.0035(12) C5 0.0364(16) 0.0194(14) 0.0349(16) 0.0003(12) -0.0033(13) 0.0012(12) C6 0.0285(15) 0.0204(14) 0.0285(14) -0.0030(11) -0.0047(11) 0.0020(11) C7 0.0458(19) 0.0289(17) 0.0459(18) 0.0065(14) 0.0086(14) -0.0056(14) C8 0.067(2) 0.040(2) 0.048(2) 0.0134(15) 0.0044(17) -0.0079(17) C9 0.077(3) 0.040(2) 0.077(3) 0.0093(18) 0.038(2) -0.0099(19) C10 0.050(2) 0.0381(19) 0.070(2) 0.0042(17) 0.0020(17) -0.0166(16) C11 0.0348(16) 0.0257(14) 0.0290(14) -0.0008(12) 0.0039(12) -0.0003(12) C12 0.0493(19) 0.0277(16) 0.0228(14) 0.0002(12) -0.0005(13) -0.0051(14) C13 0.0407(17) 0.0239(15) 0.0237(14) -0.0024(11) -0.0077(13) -0.0038(13) C14 0.054(2) 0.0307(17) 0.0325(16) 0.0030(13) -0.0103(14) -0.0056(15) C15 0.062(2) 0.0269(17) 0.053(2) 0.0088(15) -0.0162(18) 0.0025(16) C16 0.050(2) 0.0326(18) 0.063(2) 0.0019(16) -0.0104(18) 0.0114(15) C17 0.0337(17) 0.0355(17) 0.0439(18) -0.0008(14) -0.0055(14) 0.0013(14) C18 0.0466(18) 0.0194(14) 0.0335(15) -0.0065(12) 0.0054(13) 0.0017(13) C19 0.0523(19) 0.0220(15) 0.0254(14) 0.0019(12) -0.0017(13) -0.0006(13) C20 0.061(2) 0.0234(16) 0.0339(16) -0.0032(13) -0.0042(14) -0.0002(15) C21 0.074(2) 0.0222(16) 0.0335(17) -0.0023(13) -0.0134(16) -0.0047(16) C22 0.054(2) 0.0310(17) 0.0379(17) 0.0054(14) -0.0166(15) -0.0142(15) C23 0.0417(18) 0.0272(16) 0.0354(16) 0.0036(12) -0.0081(13) -0.0062(13) C24 0.0356(16) 0.0202(14) 0.0356(16) -0.0024(12) 0.0006(13) 0.0042(12) C25 0.0356(16) 0.0212(14) 0.0349(15) -0.0083(12) -0.0018(12) -0.0023(12) C26 0.0309(15) 0.0279(16) 0.0231(14) -0.0035(11) -0.0063(11) 0.0003(12) C27 0.0322(16) 0.0321(16) 0.0353(16) -0.0007(13) -0.0033(13) -0.0084(13) C28 0.0286(16) 0.044(2) 0.0386(17) 0.0025(14) 0.0016(13) -0.0039(14) C29 0.0313(16) 0.0369(17) 0.0360(16) -0.0042(13) -0.0006(13) 0.0082(14) C30 0.0351(17) 0.0240(14) 0.0280(14) -0.0007(12) -0.0044(12) 0.0030(13) C31 0.0384(17) 0.0299(16) 0.0384(16) -0.0102(13) 0.0044(13) 0.0045(13) C32 0.0310(16) 0.0372(18) 0.0349(16) -0.0100(13) 0.0058(13) -0.0015(13) C33 0.049(2) 0.048(2) 0.0409(18) -0.0150(15) 0.0096(15) 0.0058(16) C34 0.076(3) 0.076(3) 0.0310(18) -0.0140(18) 0.0162(17) 0.005(2) C35 0.073(3) 0.065(2) 0.0313(17) 0.0014(16) 0.0090(16) 0.002(2) C36 0.050(2) 0.0447(19) 0.0328(17) -0.0016(14) 0.0064(14) 0.0000(15) C37 0.0273(15) 0.0275(15) 0.0361(16) 0.0017(13) 0.0015(13) 0.0017(13) C38 0.039(2) 0.065(2) 0.070(2) -0.0185(19) 0.0179(17) -0.0111(17) C39 0.0250(15) 0.0251(15) 0.0308(15) 0.0004(12) 0.0026(12) -0.0013(12) C40 0.0498(19) 0.0273(16) 0.0317(15) 0.0013(12) -0.0005(13) 0.0023(14) Cl1 0.0471(5) 0.0216(4) 0.0554(5) -0.0048(3) -0.0002(4) -0.0035(3) O1A 0.0615(15) 0.0435(14) 0.0746(17) -0.0189(12) -0.0003(13) -0.0181(12) O1B 0.113(2) 0.0362(14) 0.0777(18) 0.0143(13) 0.0164(16) -0.0089(14) O1C 0.0678(16) 0.0476(15) 0.0684(16) -0.0247(12) -0.0024(13) 0.0074(12) O1D 0.0526(15) 0.0425(14) 0.0955(19) 0.0039(13) -0.0064(13) 0.0097(12) N1S 0.107(4) 0.096(4) 0.214(6) 0.026(4) 0.035(4) -0.025(3) C1S 0.060(3) 0.094(4) 0.085(3) 0.021(3) 0.021(2) 0.002(3) C2S 0.091(3) 0.120(4) 0.055(3) -0.013(3) 0.009(2) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 Co2 3.4008(5) . ? Co1 O1 2.0084(17) . ? Co1 O2 2.0322(19) . ? Co1 N3 2.127(2) . ? Co1 O4 2.1336(18) . ? Co1 N2 2.155(2) . ? Co1 N1 2.191(2) . ? Co2 O1 2.0067(17) . ? Co2 O5 2.0247(18) . ? Co2 O3 2.103(2) . ? Co2 N6 2.118(2) . ? Co2 N5 2.134(2) . ? Co2 N4 2.185(2) . ? O1 C1 1.348(3) . ? O2 C37 1.258(3) . ? O3 C37 1.247(3) . ? O4 C39 1.253(3) . ? O5 C39 1.257(3) . ? N1 C18 1.477(3) . ? N1 C12 1.485(3) . ? N1 C11 1.488(3) . ? N2 C13 1.338(3) . ? N2 C17 1.351(4) . ? N3 C19 1.338(4) . ? N3 C23 1.341(3) . ? N4 C31 1.471(3) . ? N4 C25 1.482(3) . ? N4 C24 1.484(3) . ? N5 C30 1.341(3) . ? N5 C26 1.349(3) . ? N6 C36 1.334(4) . ? N6 C32 1.345(4) . ? C1 C2 1.395(4) . ? C1 C6 1.408(3) . ? C2 C3 1.387(4) . ? C2 C11 1.508(4) . ? C3 C4 1.395(4) . ? C3 H3A 0.950 . ? C4 C5 1.394(4) . ? C4 C7 1.540(4) . ? C5 C6 1.381(4) . ? C5 H5A 0.950 . ? C6 C24 1.505(4) . ? C7 C9 1.524(4) . ? C7 C8 1.527(4) . ? C7 C10 1.527(4) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 C13 1.502(4) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.389(4) . ? C14 C15 1.375(4) . ? C14 H14A 0.950 . ? C15 C16 1.374(5) . ? C15 H15A 0.950 . ? C16 C17 1.373(4) . ? C16 H16A 0.950 . ? C17 H17A 0.950 . ? C18 C19 1.513(4) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 C20 1.388(4) . ? C20 C21 1.374(4) . ? C20 H20A 0.950 . ? C21 C22 1.377(5) . ? C21 H21A 0.950 . ? C22 C23 1.389(4) . ? C22 H22A 0.950 . ? C23 H23A 0.950 . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 C26 1.502(4) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.376(4) . ? C27 C28 1.380(4) . ? C27 H27A 0.950 . ? C28 C29 1.374(4) . ? C28 H28A 0.950 . ? C29 C30 1.366(4) . ? C29 H29A 0.950 . ? C30 H30A 0.950 . ? C31 C32 1.506(4) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 C33 1.382(4) . ? C33 C34 1.375(5) . ? C33 H33A 0.950 . ? C34 C35 1.379(5) . ? C34 H34A 0.950 . ? C35 C36 1.380(4) . ? C35 H35A 0.950 . ? C36 H36A 0.950 . ? C37 C38 1.494(4) . ? C38 H38A 0.980 . ? C38 H38B 0.980 . ? C38 H38C 0.980 . ? C39 C40 1.509(4) . ? C40 H40A 0.980 . ? C40 H40B 0.980 . ? C40 H40C 0.980 . ? Cl1 O1A 1.426(2) . ? Cl1 O1B 1.430(3) . ? Cl1 O1D 1.430(2) . ? Cl1 O1C 1.434(2) . ? N1S C1S 1.122(6) . ? C1S C2S 1.442(7) . ? C2S H2S1 0.980 . ? C2S H2S2 0.980 . ? C2S H2S3 0.980 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 100.70(7) . . ? O1 Co1 N3 164.62(8) . . ? O2 Co1 N3 94.18(8) . . ? O1 Co1 O4 91.71(7) . . ? O2 Co1 O4 90.91(8) . . ? N3 Co1 O4 84.12(7) . . ? O1 Co1 N2 86.43(7) . . ? O2 Co1 N2 94.41(9) . . ? N3 Co1 N2 96.36(8) . . ? O4 Co1 N2 174.60(8) . . ? O1 Co1 N1 88.88(7) . . ? O2 Co1 N1 167.92(8) . . ? N3 Co1 N1 76.91(8) . . ? O4 Co1 N1 96.19(8) . . ? N2 Co1 N1 78.72(8) . . ? O1 Co2 O5 97.93(7) . . ? O1 Co2 O3 89.35(8) . . ? O5 Co2 O3 93.93(8) . . ? O1 Co2 N6 165.15(8) . . ? O5 Co2 N6 94.99(8) . . ? O3 Co2 N6 82.46(8) . . ? O1 Co2 N5 86.92(7) . . ? O5 Co2 N5 95.25(8) . . ? O3 Co2 N5 170.48(8) . . ? N6 Co2 N5 99.21(8) . . ? O1 Co2 N4 90.72(7) . . ? O5 Co2 N4 169.37(8) . . ? O3 Co2 N4 92.32(8) . . ? N6 Co2 N4 77.32(8) . . ? N5 Co2 N4 78.99(8) . . ? C1 O1 Co2 121.55(15) . . ? C1 O1 Co1 122.65(15) . . ? Co2 O1 Co1 115.78(8) . . ? C37 O2 Co1 128.60(17) . . ? C37 O3 Co2 133.66(19) . . ? C39 O4 Co1 131.22(17) . . ? C39 O5 Co2 133.20(17) . . ? C18 N1 C12 110.8(2) . . ? C18 N1 C11 110.4(2) . . ? C12 N1 C11 111.1(2) . . ? C18 N1 Co1 104.92(16) . . ? C12 N1 Co1 108.78(16) . . ? C11 N1 Co1 110.74(15) . . ? C13 N2 C17 118.1(2) . . ? C13 N2 Co1 114.65(18) . . ? C17 N2 Co1 123.64(19) . . ? C19 N3 C23 119.1(2) . . ? C19 N3 Co1 115.12(18) . . ? C23 N3 Co1 125.8(2) . . ? C31 N4 C25 110.5(2) . . ? C31 N4 C24 111.3(2) . . ? C25 N4 C24 111.7(2) . . ? C31 N4 Co2 105.04(16) . . ? C25 N4 Co2 108.36(15) . . ? C24 N4 Co2 109.70(15) . . ? C30 N5 C26 117.7(2) . . ? C30 N5 Co2 123.54(18) . . ? C26 N5 Co2 115.16(17) . . ? C36 N6 C32 119.1(2) . . ? C36 N6 Co2 126.0(2) . . ? C32 N6 Co2 114.89(18) . . ? O1 C1 C2 120.5(2) . . ? O1 C1 C6 120.0(2) . . ? C2 C1 C6 119.4(2) . . ? C3 C2 C1 119.8(2) . . ? C3 C2 C11 121.3(2) . . ? C1 C2 C11 118.9(2) . . ? C2 C3 C4 122.2(3) . . ? C2 C3 H3A 118.9 . . ? C4 C3 H3A 118.9 . . ? C5 C4 C3 116.6(3) . . ? C5 C4 C7 119.9(2) . . ? C3 C4 C7 123.5(3) . . ? C6 C5 C4 123.2(2) . . ? C6 C5 H5A 118.4 . . ? C4 C5 H5A 118.4 . . ? C5 C6 C1 118.8(2) . . ? C5 C6 C24 121.7(2) . . ? C1 C6 C24 119.5(2) . . ? C9 C7 C8 109.1(3) . . ? C9 C7 C10 108.2(3) . . ? C8 C7 C10 109.5(3) . . ? C9 C7 C4 111.9(2) . . ? C8 C7 C4 109.0(2) . . ? C10 C7 C4 109.1(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C2 111.4(2) . . ? N1 C11 H11A 109.3 . . ? C2 C11 H11A 109.3 . . ? N1 C11 H11B 109.3 . . ? C2 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? N1 C12 C13 111.6(2) . . ? N1 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? N1 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? N2 C13 C14 122.2(3) . . ? N2 C13 C12 115.2(2) . . ? C14 C13 C12 122.6(3) . . ? C15 C14 C13 118.9(3) . . ? C15 C14 H14A 120.5 . . ? C13 C14 H14A 120.5 . . ? C16 C15 C14 119.1(3) . . ? C16 C15 H15A 120.4 . . ? C14 C15 H15A 120.4 . . ? C17 C16 C15 119.3(3) . . ? C17 C16 H16A 120.4 . . ? C15 C16 H16A 120.4 . . ? N2 C17 C16 122.3(3) . . ? N2 C17 H17A 118.8 . . ? C16 C17 H17A 118.8 . . ? N1 C18 C19 109.9(2) . . ? N1 C18 H18A 109.7 . . ? C19 C18 H18A 109.7 . . ? N1 C18 H18B 109.7 . . ? C19 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? N3 C19 C20 121.9(3) . . ? N3 C19 C18 115.3(2) . . ? C20 C19 C18 122.8(3) . . ? C21 C20 C19 118.9(3) . . ? C21 C20 H20A 120.5 . . ? C19 C20 H20A 120.5 . . ? C20 C21 C22 119.6(3) . . ? C20 C21 H21A 120.2 . . ? C22 C21 H21A 120.2 . . ? C21 C22 C23 118.7(3) . . ? C21 C22 H22A 120.7 . . ? C23 C22 H22A 120.7 . . ? N3 C23 C22 121.8(3) . . ? N3 C23 H23A 119.1 . . ? C22 C23 H23A 119.1 . . ? N4 C24 C6 112.6(2) . . ? N4 C24 H24A 109.1 . . ? C6 C24 H24A 109.1 . . ? N4 C24 H24B 109.1 . . ? C6 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? N4 C25 C26 111.8(2) . . ? N4 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? N4 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? N5 C26 C27 122.3(3) . . ? N5 C26 C25 114.9(2) . . ? C27 C26 C25 122.8(2) . . ? C26 C27 C28 118.9(3) . . ? C26 C27 H27A 120.5 . . ? C28 C27 H27A 120.5 . . ? C29 C28 C27 119.0(3) . . ? C29 C28 H28A 120.5 . . ? C27 C28 H28A 120.5 . . ? C30 C29 C28 119.1(3) . . ? C30 C29 H29A 120.4 . . ? C28 C29 H29A 120.4 . . ? N5 C30 C29 122.9(3) . . ? N5 C30 H30A 118.5 . . ? C29 C30 H30A 118.5 . . ? N4 C31 C32 110.3(2) . . ? N4 C31 H31A 109.6 . . ? C32 C31 H31A 109.6 . . ? N4 C31 H31B 109.6 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? N6 C32 C33 121.3(3) . . ? N6 C32 C31 115.3(2) . . ? C33 C32 C31 123.4(3) . . ? C34 C33 C32 119.1(3) . . ? C34 C33 H33A 120.4 . . ? C32 C33 H33A 120.4 . . ? C33 C34 C35 119.7(3) . . ? C33 C34 H34A 120.1 . . ? C35 C34 H34A 120.1 . . ? C34 C35 C36 118.1(3) . . ? C34 C35 H35A 120.9 . . ? C36 C35 H35A 120.9 . . ? N6 C36 C35 122.6(3) . . ? N6 C36 H36A 118.7 . . ? C35 C36 H36A 118.7 . . ? O3 C37 O2 126.3(3) . . ? O3 C37 C38 116.4(3) . . ? O2 C37 C38 117.3(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O4 C39 O5 126.1(2) . . ? O4 C39 C40 117.9(2) . . ? O5 C39 C40 116.0(2) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O1A Cl1 O1B 109.74(16) . . ? O1A Cl1 O1D 109.01(15) . . ? O1B Cl1 O1D 109.30(17) . . ? O1A Cl1 O1C 109.73(15) . . ? O1B Cl1 O1C 109.92(16) . . ? O1D Cl1 O1C 109.13(15) . . ? N1S C1S C2S 178.4(6) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Co2 O1 C1 -138.31(18) . . . . ? O3 Co2 O1 C1 127.81(18) . . . . ? N6 Co2 O1 C1 71.5(4) . . . . ? N5 Co2 O1 C1 -43.44(18) . . . . ? N4 Co2 O1 C1 35.50(18) . . . . ? O5 Co2 O1 Co1 43.36(10) . . . . ? O3 Co2 O1 Co1 -50.52(10) . . . . ? N6 Co2 O1 Co1 -106.8(3) . . . . ? N5 Co2 O1 Co1 138.23(10) . . . . ? N4 Co2 O1 Co1 -142.83(10) . . . . ? O2 Co1 O1 C1 -138.39(18) . . . . ? N3 Co1 O1 C1 56.5(4) . . . . ? O4 Co1 O1 C1 130.36(18) . . . . ? N2 Co1 O1 C1 -44.57(19) . . . . ? N1 Co1 O1 C1 34.20(18) . . . . ? O2 Co1 O1 Co2 39.92(10) . . . . ? N3 Co1 O1 Co2 -125.2(3) . . . . ? O4 Co1 O1 Co2 -51.33(10) . . . . ? N2 Co1 O1 Co2 133.74(10) . . . . ? N1 Co1 O1 Co2 -147.49(10) . . . . ? O1 Co1 O2 C37 -3.8(2) . . . . ? N3 Co1 O2 C37 172.3(2) . . . . ? O4 Co1 O2 C37 88.1(2) . . . . ? N2 Co1 O2 C37 -91.0(2) . . . . ? N1 Co1 O2 C37 -145.8(3) . . . . ? O1 Co2 O3 C37 50.0(3) . . . . ? O5 Co2 O3 C37 -47.9(3) . . . . ? N6 Co2 O3 C37 -142.4(3) . . . . ? N4 Co2 O3 C37 140.7(3) . . . . ? O1 Co1 O4 C39 41.5(2) . . . . ? O2 Co1 O4 C39 -59.3(2) . . . . ? N3 Co1 O4 C39 -153.4(2) . . . . ? N1 Co1 O4 C39 130.5(2) . . . . ? O1 Co2 O5 C39 -9.6(2) . . . . ? O3 Co2 O5 C39 80.2(2) . . . . ? N6 Co2 O5 C39 163.0(2) . . . . ? N5 Co2 O5 C39 -97.3(2) . . . . ? N4 Co2 O5 C39 -153.9(4) . . . . ? O1 Co1 N1 C18 139.76(16) . . . . ? O2 Co1 N1 C18 -77.5(4) . . . . ? N3 Co1 N1 C18 -34.31(16) . . . . ? O4 Co1 N1 C18 48.16(16) . . . . ? N2 Co1 N1 C18 -133.66(17) . . . . ? O1 Co1 N1 C12 -101.69(16) . . . . ? O2 Co1 N1 C12 41.0(4) . . . . ? N3 Co1 N1 C12 84.24(16) . . . . ? O4 Co1 N1 C12 166.71(15) . . . . ? N2 Co1 N1 C12 -15.10(16) . . . . ? O1 Co1 N1 C11 20.63(16) . . . . ? O2 Co1 N1 C11 163.4(3) . . . . ? N3 Co1 N1 C11 -153.44(17) . . . . ? O4 Co1 N1 C11 -70.97(16) . . . . ? N2 Co1 N1 C11 107.22(17) . . . . ? O1 Co1 N2 C13 84.84(18) . . . . ? O2 Co1 N2 C13 -174.69(18) . . . . ? N3 Co1 N2 C13 -79.98(18) . . . . ? N1 Co1 N2 C13 -4.73(17) . . . . ? O1 Co1 N2 C17 -73.2(2) . . . . ? O2 Co1 N2 C17 27.2(2) . . . . ? N3 Co1 N2 C17 122.0(2) . . . . ? N1 Co1 N2 C17 -162.8(2) . . . . ? O1 Co1 N3 C19 -3.2(4) . . . . ? O2 Co1 N3 C19 -168.50(18) . . . . ? O4 Co1 N3 C19 -78.01(18) . . . . ? N2 Co1 N3 C19 96.58(19) . . . . ? N1 Co1 N3 C19 19.76(18) . . . . ? O1 Co1 N3 C23 175.9(2) . . . . ? O2 Co1 N3 C23 10.5(2) . . . . ? O4 Co1 N3 C23 101.0(2) . . . . ? N2 Co1 N3 C23 -84.4(2) . . . . ? N1 Co1 N3 C23 -161.2(2) . . . . ? O1 Co2 N4 C31 137.68(16) . . . . ? O5 Co2 N4 C31 -77.7(5) . . . . ? O3 Co2 N4 C31 48.31(16) . . . . ? N6 Co2 N4 C31 -33.43(16) . . . . ? N5 Co2 N4 C31 -135.60(16) . . . . ? O1 Co2 N4 C25 -104.18(16) . . . . ? O5 Co2 N4 C25 40.4(5) . . . . ? O3 Co2 N4 C25 166.44(16) . . . . ? N6 Co2 N4 C25 84.70(17) . . . . ? N5 Co2 N4 C25 -17.47(16) . . . . ? O1 Co2 N4 C24 17.99(17) . . . . ? O5 Co2 N4 C24 162.6(4) . . . . ? O3 Co2 N4 C24 -71.39(17) . . . . ? N6 Co2 N4 C24 -153.12(17) . . . . ? N5 Co2 N4 C24 104.71(17) . . . . ? O1 Co2 N5 C30 -68.2(2) . . . . ? O5 Co2 N5 C30 29.5(2) . . . . ? N6 Co2 N5 C30 125.4(2) . . . . ? N4 Co2 N5 C30 -159.6(2) . . . . ? O1 Co2 N5 C26 89.93(17) . . . . ? O5 Co2 N5 C26 -172.38(17) . . . . ? N6 Co2 N5 C26 -76.45(18) . . . . ? N4 Co2 N5 C26 -1.40(17) . . . . ? O1 Co2 N6 C36 159.0(3) . . . . ? O5 Co2 N6 C36 8.6(2) . . . . ? O3 Co2 N6 C36 102.0(2) . . . . ? N5 Co2 N6 C36 -87.5(2) . . . . ? N4 Co2 N6 C36 -163.9(2) . . . . ? O1 Co2 N6 C32 -18.4(4) . . . . ? O5 Co2 N6 C32 -168.75(19) . . . . ? O3 Co2 N6 C32 -75.43(19) . . . . ? N5 Co2 N6 C32 95.1(2) . . . . ? N4 Co2 N6 C32 18.67(19) . . . . ? Co2 O1 C1 C2 131.0(2) . . . . ? Co1 O1 C1 C2 -50.7(3) . . . . ? Co2 O1 C1 C6 -49.5(3) . . . . ? Co1 O1 C1 C6 128.7(2) . . . . ? O1 C1 C2 C3 -179.4(2) . . . . ? C6 C1 C2 C3 1.1(4) . . . . ? O1 C1 C2 C11 1.2(4) . . . . ? C6 C1 C2 C11 -178.3(2) . . . . ? C1 C2 C3 C4 -0.8(4) . . . . ? C11 C2 C3 C4 178.6(2) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C2 C3 C4 C7 179.8(3) . . . . ? C3 C4 C5 C6 0.8(4) . . . . ? C7 C4 C5 C6 -179.2(2) . . . . ? C4 C5 C6 C1 -0.4(4) . . . . ? C4 C5 C6 C24 -179.9(2) . . . . ? O1 C1 C6 C5 180.0(2) . . . . ? C2 C1 C6 C5 -0.5(4) . . . . ? O1 C1 C6 C24 -0.5(4) . . . . ? C2 C1 C6 C24 179.0(2) . . . . ? C5 C4 C7 C9 177.3(3) . . . . ? C3 C4 C7 C9 -2.7(4) . . . . ? C5 C4 C7 C8 -62.0(3) . . . . ? C3 C4 C7 C8 118.1(3) . . . . ? C5 C4 C7 C10 57.6(3) . . . . ? C3 C4 C7 C10 -122.4(3) . . . . ? C18 N1 C11 C2 -180.0(2) . . . . ? C12 N1 C11 C2 56.8(3) . . . . ? Co1 N1 C11 C2 -64.2(2) . . . . ? C3 C2 C11 N1 -118.0(3) . . . . ? C1 C2 C11 N1 61.4(3) . . . . ? C18 N1 C12 C13 146.3(2) . . . . ? C11 N1 C12 C13 -90.7(3) . . . . ? Co1 N1 C12 C13 31.4(3) . . . . ? C17 N2 C13 C14 1.6(4) . . . . ? Co1 N2 C13 C14 -157.8(2) . . . . ? C17 N2 C13 C12 -176.3(2) . . . . ? Co1 N2 C13 C12 24.3(3) . . . . ? N1 C12 C13 N2 -38.1(3) . . . . ? N1 C12 C13 C14 144.0(2) . . . . ? N2 C13 C14 C15 -1.8(4) . . . . ? C12 C13 C14 C15 176.0(3) . . . . ? C13 C14 C15 C16 0.4(4) . . . . ? C14 C15 C16 C17 1.1(5) . . . . ? C13 N2 C17 C16 0.0(4) . . . . ? Co1 N2 C17 C16 157.4(2) . . . . ? C15 C16 C17 N2 -1.4(5) . . . . ? C12 N1 C18 C19 -72.8(3) . . . . ? C11 N1 C18 C19 163.7(2) . . . . ? Co1 N1 C18 C19 44.4(2) . . . . ? C23 N3 C19 C20 -0.4(4) . . . . ? Co1 N3 C19 C20 178.7(2) . . . . ? C23 N3 C19 C18 -179.1(2) . . . . ? Co1 N3 C19 C18 0.0(3) . . . . ? N1 C18 C19 N3 -31.3(3) . . . . ? N1 C18 C19 C20 150.0(2) . . . . ? N3 C19 C20 C21 0.0(4) . . . . ? C18 C19 C20 C21 178.6(3) . . . . ? C19 C20 C21 C22 -0.1(4) . . . . ? C20 C21 C22 C23 0.5(4) . . . . ? C19 N3 C23 C22 0.8(4) . . . . ? Co1 N3 C23 C22 -178.22(19) . . . . ? C21 C22 C23 N3 -0.8(4) . . . . ? C31 N4 C24 C6 -178.0(2) . . . . ? C25 N4 C24 C6 58.0(3) . . . . ? Co2 N4 C24 C6 -62.2(2) . . . . ? C5 C6 C24 N4 -117.6(3) . . . . ? C1 C6 C24 N4 62.9(3) . . . . ? C31 N4 C25 C26 147.4(2) . . . . ? C24 N4 C25 C26 -88.1(3) . . . . ? Co2 N4 C25 C26 32.8(2) . . . . ? C30 N5 C26 C27 -0.5(4) . . . . ? Co2 N5 C26 C27 -160.0(2) . . . . ? C30 N5 C26 C25 -179.9(2) . . . . ? Co2 N5 C26 C25 20.6(3) . . . . ? N4 C25 C26 N5 -36.5(3) . . . . ? N4 C25 C26 C27 144.1(2) . . . . ? N5 C26 C27 C28 -0.2(4) . . . . ? C25 C26 C27 C28 179.1(2) . . . . ? C26 C27 C28 C29 0.7(4) . . . . ? C27 C28 C29 C30 -0.5(4) . . . . ? C26 N5 C30 C29 0.8(4) . . . . ? Co2 N5 C30 C29 158.4(2) . . . . ? C28 C29 C30 N5 -0.3(4) . . . . ? C25 N4 C31 C32 -72.9(3) . . . . ? C24 N4 C31 C32 162.4(2) . . . . ? Co2 N4 C31 C32 43.8(2) . . . . ? C36 N6 C32 C33 1.4(4) . . . . ? Co2 N6 C32 C33 179.0(2) . . . . ? C36 N6 C32 C31 -176.6(3) . . . . ? Co2 N6 C32 C31 1.0(3) . . . . ? N4 C31 C32 N6 -31.5(3) . . . . ? N4 C31 C32 C33 150.5(3) . . . . ? N6 C32 C33 C34 -1.2(5) . . . . ? C31 C32 C33 C34 176.7(3) . . . . ? C32 C33 C34 C35 -0.1(5) . . . . ? C33 C34 C35 C36 1.0(6) . . . . ? C32 N6 C36 C35 -0.4(5) . . . . ? Co2 N6 C36 C35 -177.7(2) . . . . ? C34 C35 C36 N6 -0.8(5) . . . . ? Co2 O3 C37 O2 -22.0(5) . . . . ? Co2 O3 C37 C38 158.9(2) . . . . ? Co1 O2 C37 O3 -7.4(4) . . . . ? Co1 O2 C37 C38 171.7(2) . . . . ? Co1 O4 C39 O5 -13.8(4) . . . . ? Co1 O4 C39 C40 166.43(18) . . . . ? Co2 O5 C39 O4 -6.3(4) . . . . ? Co2 O5 C39 C40 173.51(18) . . . . ? #============================================================================== data_13_H2O _database_code_depnum_ccdc_archive 'CCDC 772409' #TrackingRef '- submit_all.cif' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C40 H45 Co2 N6 O5 2+, 2(Cl O4 -), H2 O ; _chemical_formula_sum 'C40 H47 Cl2 Co2 N6 O14' _chemical_formula_weight 1024.60 # H atoms are omitted from disordered water molecule # H atom sites in CIF sum to 8 H atoms per unit cell fewer than stated formula 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' Cl Cl 0.1484 0.1585 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 12.2490(4) _cell_length_b 21.8499(8) _cell_length_c 16.4739(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.346(2) _cell_angle_gamma 90.00 _cell_volume 4396.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6082 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 23.13 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2116 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Isostructural with Mn(II)/Mn(III) analogue (CSD: FOSCAR) and Fe(II)/Fe(III) analogue (CSD: LEQZAI). Water molecule is poorly resolved: modelled as disordered over three partially occupied sites. H atoms are omitted from these water molecules so that the atom sites are 8 x H per cell short of the stated formula. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 77742 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 26.37 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 8973 _reflns_number_gt 6094 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+2.1733P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8973 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1120 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.727 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.070 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.45825(4) 0.187161(17) 0.58877(2) 0.02712(12) Uani 1 1 d . . . Co2 Co 0.52917(3) 0.263051(18) 0.76839(2) 0.02452(12) Uani 1 1 d . . . O1 O 0.53642(16) 0.25633(8) 0.65374(11) 0.0238(4) Uani 1 1 d . . . O2 O 0.32956(19) 0.18846(10) 0.65962(13) 0.0384(6) Uani 1 1 d . . . O3 O 0.37241(17) 0.25601(10) 0.76120(12) 0.0315(5) Uani 1 1 d . . . O4 O 0.53883(19) 0.12641(9) 0.67026(12) 0.0359(5) Uani 1 1 d . . . O5 O 0.54418(18) 0.17765(9) 0.78979(12) 0.0309(5) Uani 1 1 d . . . N1 N 0.5832(2) 0.18771(10) 0.50327(14) 0.0280(6) Uani 1 1 d . . . N2 N 0.3940(2) 0.25602(11) 0.50679(15) 0.0291(6) Uani 1 1 d . . . N3 N 0.4152(2) 0.11033(12) 0.51530(16) 0.0372(7) Uani 1 1 d . . . N4 N 0.5200(2) 0.35299(11) 0.76662(14) 0.0266(6) Uani 1 1 d . . . N5 N 0.6852(2) 0.27524(11) 0.77378(14) 0.0259(6) Uani 1 1 d . . . N6 N 0.5150(2) 0.27663(12) 0.88418(15) 0.0302(6) Uani 1 1 d . . . C1 C 0.5888(2) 0.30002(12) 0.61276(17) 0.0233(6) Uani 1 1 d . . . C2 C 0.6647(2) 0.28324(13) 0.55823(17) 0.0253(7) Uani 1 1 d . . . C3 C 0.7159(3) 0.32921(14) 0.51590(18) 0.0305(7) Uani 1 1 d . . . H3A H 0.7680 0.3179 0.4787 0.037 Uiso 1 1 calc R . . C4 C 0.6932(3) 0.39096(14) 0.52638(18) 0.0323(7) Uani 1 1 d . . . C5 C 0.6171(3) 0.40581(13) 0.58125(18) 0.0288(7) Uani 1 1 d . . . H5A H 0.6007 0.4477 0.5899 0.035 Uiso 1 1 calc R . . C6 C 0.5641(2) 0.36144(13) 0.62397(17) 0.0251(7) Uani 1 1 d . . . C7 C 0.7483(3) 0.44189(15) 0.4795(2) 0.0412(9) Uani 1 1 d . . . C8 C 0.6573(4) 0.48089(19) 0.4337(3) 0.0633(12) Uani 1 1 d . . . H8A H 0.6907 0.5155 0.4071 0.095 Uiso 1 1 calc R . . H8B H 0.6071 0.4962 0.4726 0.095 Uiso 1 1 calc R . . H8C H 0.6167 0.4556 0.3927 0.095 Uiso 1 1 calc R . . C9 C 0.8215(4) 0.41698(19) 0.4171(3) 0.0820(16) Uani 1 1 d . . . H9A H 0.8827 0.3946 0.4450 0.123 Uiso 1 1 calc R . . H9B H 0.8498 0.4510 0.3861 0.123 Uiso 1 1 calc R . . H9C H 0.7792 0.3893 0.3800 0.123 Uiso 1 1 calc R . . C10 C 0.8141(3) 0.48279(18) 0.5403(3) 0.0608(11) Uani 1 1 d . . . H10A H 0.8730 0.4589 0.5686 0.091 Uiso 1 1 calc R . . H10B H 0.7658 0.4990 0.5799 0.091 Uiso 1 1 calc R . . H10C H 0.8458 0.5168 0.5112 0.091 Uiso 1 1 calc R . . C11 C 0.6848(3) 0.21687(14) 0.54008(18) 0.0292(7) Uani 1 1 d . . . H11A H 0.7433 0.2135 0.5021 0.035 Uiso 1 1 calc R . . H11B H 0.7095 0.1953 0.5910 0.035 Uiso 1 1 calc R . . C12 C 0.5400(3) 0.22070(14) 0.42886(17) 0.0316(7) Uani 1 1 d . . . H12A H 0.5031 0.1912 0.3903 0.038 Uiso 1 1 calc R . . H12B H 0.6016 0.2393 0.4021 0.038 Uiso 1 1 calc R . . C13 C 0.4608(3) 0.26962(14) 0.44832(17) 0.0304(7) Uani 1 1 d . . . C14 C 0.4527(3) 0.32509(14) 0.40685(19) 0.0368(8) Uani 1 1 d . . . H14A H 0.5012 0.3343 0.3662 0.044 Uiso 1 1 calc R . . C15 C 0.3737(3) 0.36647(15) 0.4255(2) 0.0416(9) Uani 1 1 d . . . H15A H 0.3671 0.4046 0.3980 0.050 Uiso 1 1 calc R . . C16 C 0.3041(3) 0.35193(15) 0.4848(2) 0.0406(8) Uani 1 1 d . . . H16A H 0.2480 0.3795 0.4980 0.049 Uiso 1 1 calc R . . C17 C 0.3177(3) 0.29663(15) 0.5243(2) 0.0348(8) Uani 1 1 d . . . H17A H 0.2708 0.2869 0.5658 0.042 Uiso 1 1 calc R . . C18 C 0.6029(3) 0.12256(13) 0.48478(19) 0.0359(8) Uani 1 1 d . . . H18A H 0.6460 0.1031 0.5311 0.043 Uiso 1 1 calc R . . H18B H 0.6450 0.1192 0.4360 0.043 Uiso 1 1 calc R . . C19 C 0.4941(3) 0.09064(14) 0.46968(18) 0.0365(8) Uani 1 1 d . . . C20 C 0.4759(4) 0.04393(15) 0.4130(2) 0.0451(9) Uani 1 1 d . . . H20A H 0.5324 0.0311 0.3804 0.054 Uiso 1 1 calc R . . C21 C 0.3743(4) 0.01668(16) 0.4053(2) 0.0530(11) Uani 1 1 d . . . H21A H 0.3597 -0.0151 0.3667 0.064 Uiso 1 1 calc R . . C22 C 0.2947(4) 0.03550(16) 0.4530(2) 0.0524(11) Uani 1 1 d . . . H22A H 0.2250 0.0163 0.4491 0.063 Uiso 1 1 calc R . . C23 C 0.3167(3) 0.08298(16) 0.5075(2) 0.0457(9) Uani 1 1 d . . . H23A H 0.2607 0.0966 0.5401 0.055 Uiso 1 1 calc R . . C24 C 0.4823(3) 0.37718(14) 0.68401(17) 0.0294(7) Uani 1 1 d . . . H24A H 0.4735 0.4222 0.6867 0.035 Uiso 1 1 calc R . . H24B H 0.4103 0.3592 0.6661 0.035 Uiso 1 1 calc R . . C25 C 0.6307(2) 0.37851(14) 0.79318(18) 0.0298(7) Uani 1 1 d . . . H25A H 0.6414 0.4180 0.7655 0.036 Uiso 1 1 calc R . . H25B H 0.6360 0.3859 0.8527 0.036 Uiso 1 1 calc R . . C26 C 0.7166(3) 0.33437(14) 0.77238(17) 0.0286(7) Uani 1 1 d . . . C27 C 0.8207(3) 0.35081(15) 0.75365(19) 0.0359(8) Uani 1 1 d . . . H27A H 0.8415 0.3927 0.7529 0.043 Uiso 1 1 calc R . . C28 C 0.8941(3) 0.30541(16) 0.7361(2) 0.0400(8) Uani 1 1 d . . . H28A H 0.9655 0.3157 0.7217 0.048 Uiso 1 1 calc R . . C29 C 0.8624(3) 0.24519(15) 0.73964(19) 0.0348(8) Uani 1 1 d . . . H29A H 0.9123 0.2134 0.7294 0.042 Uiso 1 1 calc R . . C30 C 0.7585(3) 0.23159(14) 0.75805(18) 0.0301(7) Uani 1 1 d . . . H30A H 0.7370 0.1899 0.7599 0.036 Uiso 1 1 calc R . . C31 C 0.4420(3) 0.37021(15) 0.82830(18) 0.0343(8) Uani 1 1 d . . . H31A H 0.4498 0.4141 0.8425 0.041 Uiso 1 1 calc R . . H31B H 0.3656 0.3625 0.8068 0.041 Uiso 1 1 calc R . . C32 C 0.4708(3) 0.33132(15) 0.90095(19) 0.0335(8) Uani 1 1 d . . . C33 C 0.4568(3) 0.34855(18) 0.9801(2) 0.0440(9) Uani 1 1 d . . . H33A H 0.4267 0.3874 0.9914 0.053 Uiso 1 1 calc R . . C34 C 0.4872(3) 0.30863(19) 1.0424(2) 0.0515(10) Uani 1 1 d . . . H34A H 0.4792 0.3200 1.0973 0.062 Uiso 1 1 calc R . . C35 C 0.5291(3) 0.25249(19) 1.0249(2) 0.0474(10) Uani 1 1 d . . . H35A H 0.5481 0.2241 1.0672 0.057 Uiso 1 1 calc R . . C36 C 0.5433(3) 0.23764(16) 0.94458(19) 0.0376(8) Uani 1 1 d . . . H36A H 0.5737 0.1990 0.9323 0.045 Uiso 1 1 calc R . . C37 C 0.3065(3) 0.21972(14) 0.72034(18) 0.0300(7) Uani 1 1 d . . . C38 C 0.1945(3) 0.21637(19) 0.7474(2) 0.0505(10) Uani 1 1 d . . . H38A H 0.1509 0.1876 0.7127 0.076 Uiso 1 1 calc R . . H38B H 0.1607 0.2570 0.7435 0.076 Uiso 1 1 calc R . . H38C H 0.1976 0.2023 0.8040 0.076 Uiso 1 1 calc R . . C39 C 0.5496(3) 0.12900(14) 0.74545(19) 0.0314(7) Uani 1 1 d . . . C40 C 0.5761(3) 0.07129(15) 0.7928(2) 0.0458(9) Uani 1 1 d . . . H40A H 0.5236 0.0393 0.7752 0.069 Uiso 1 1 calc R . . H40B H 0.5717 0.0792 0.8510 0.069 Uiso 1 1 calc R . . H40C H 0.6503 0.0578 0.7831 0.069 Uiso 1 1 calc R . . Cl1 Cl 0.90526(8) 0.06262(4) 0.70367(5) 0.0431(2) Uani 1 1 d . . . O1A O 0.9917(2) 0.10359(12) 0.73027(17) 0.0619(8) Uani 1 1 d . . . O1B O 0.8717(3) 0.02719(13) 0.76931(18) 0.0851(11) Uani 1 1 d . . . O1C O 0.9415(3) 0.02140(14) 0.64417(18) 0.0761(9) Uani 1 1 d . . . O1D O 0.8167(3) 0.09700(14) 0.6683(2) 0.0913(11) Uani 1 1 d . . . Cl2 Cl 0.14336(7) 0.40256(4) 0.71220(6) 0.0490(2) Uani 1 1 d . . . O2A O 0.0439(3) 0.43177(17) 0.7000(3) 0.1021(13) Uani 1 1 d . . . O2B O 0.1595(4) 0.3631(2) 0.6489(2) 0.1330(17) Uani 1 1 d . . . O2C O 0.2296(3) 0.44491(19) 0.7203(3) 0.1248(16) Uani 1 1 d . . . O2D O 0.1448(3) 0.36752(14) 0.78570(17) 0.0729(9) Uani 1 1 d . . . O1W O 0.1757(10) -0.0004(5) 0.6177(7) 0.157(3) Uiso 0.50 1 d P A 1 O2W O 0.2735(18) 0.0439(10) 0.6858(13) 0.157(3) Uiso 0.25 1 d P B 2 O3W O 0.1115(19) 0.0063(10) 0.5611(14) 0.157(3) Uiso 0.25 1 d P C 3 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 0.0364(3) 0.0216(2) 0.0224(2) -0.00108(17) -0.00363(18) -0.00459(18) Co2 0.0296(2) 0.0239(2) 0.0194(2) -0.00059(16) -0.00188(17) -0.00152(18) O1 0.0326(12) 0.0199(10) 0.0184(10) -0.0005(8) -0.0007(9) -0.0044(9) O2 0.0426(14) 0.0406(13) 0.0324(12) -0.0076(11) 0.0053(11) -0.0123(11) O3 0.0302(12) 0.0368(12) 0.0271(11) -0.0024(10) 0.0004(10) -0.0032(10) O4 0.0558(15) 0.0229(11) 0.0279(12) 0.0016(9) -0.0044(11) 0.0018(10) O5 0.0414(13) 0.0263(11) 0.0244(11) 0.0029(9) -0.0010(10) -0.0028(10) N1 0.0431(16) 0.0179(13) 0.0222(13) -0.0015(10) -0.0025(12) 0.0020(11) N2 0.0334(15) 0.0264(14) 0.0259(14) -0.0025(11) -0.0076(12) -0.0023(12) N3 0.0476(18) 0.0268(14) 0.0350(15) 0.0005(12) -0.0109(14) -0.0054(13) N4 0.0311(14) 0.0267(13) 0.0218(13) -0.0043(10) 0.0001(11) 0.0024(11) N5 0.0319(14) 0.0250(14) 0.0198(12) 0.0000(10) -0.0045(11) -0.0008(11) N6 0.0298(15) 0.0361(15) 0.0240(13) -0.0006(12) -0.0017(12) -0.0002(12) C1 0.0288(16) 0.0201(15) 0.0197(14) -0.0002(12) -0.0061(13) -0.0029(13) C2 0.0306(17) 0.0236(15) 0.0209(15) -0.0010(12) -0.0033(14) -0.0020(13) C3 0.0359(18) 0.0311(17) 0.0246(15) -0.0025(13) 0.0033(14) -0.0029(14) C4 0.043(2) 0.0250(17) 0.0289(17) 0.0022(14) 0.0007(16) -0.0065(15) C5 0.0368(18) 0.0190(15) 0.0298(16) -0.0007(13) -0.0026(15) -0.0009(13) C6 0.0298(17) 0.0251(16) 0.0193(14) 0.0018(12) -0.0045(13) 0.0025(13) C7 0.055(2) 0.0301(18) 0.0397(19) 0.0051(15) 0.0129(18) -0.0104(17) C8 0.072(3) 0.056(3) 0.061(3) 0.026(2) 0.001(2) -0.010(2) C9 0.114(4) 0.045(2) 0.096(4) 0.015(2) 0.070(3) -0.011(3) C10 0.058(3) 0.045(2) 0.079(3) 0.007(2) 0.002(2) -0.019(2) C11 0.0335(18) 0.0257(16) 0.0281(16) 0.0008(13) 0.0010(15) 0.0021(14) C12 0.047(2) 0.0268(17) 0.0205(15) -0.0021(13) 0.0005(15) 0.0008(15) C13 0.0417(19) 0.0298(17) 0.0178(15) -0.0023(13) -0.0104(15) -0.0029(15) C14 0.057(2) 0.0306(18) 0.0218(16) 0.0030(14) -0.0057(16) -0.0004(17) C15 0.058(2) 0.0266(18) 0.0375(19) 0.0014(15) -0.0129(19) 0.0062(17) C16 0.043(2) 0.0335(19) 0.043(2) -0.0048(16) -0.0090(18) 0.0081(16) C17 0.0296(18) 0.040(2) 0.0335(18) 0.0006(15) -0.0080(15) -0.0049(15) C18 0.055(2) 0.0230(17) 0.0292(17) -0.0017(14) 0.0009(16) 0.0046(16) C19 0.062(2) 0.0222(17) 0.0233(16) 0.0004(13) -0.0079(17) 0.0019(16) C20 0.078(3) 0.0256(18) 0.0296(18) -0.0009(14) -0.0099(18) 0.0002(19) C21 0.095(3) 0.0260(19) 0.034(2) 0.0003(16) -0.020(2) -0.008(2) C22 0.064(3) 0.032(2) 0.056(2) 0.0047(18) -0.029(2) -0.0124(19) C23 0.052(2) 0.036(2) 0.046(2) 0.0011(17) -0.0121(18) -0.0086(18) C24 0.0351(18) 0.0259(16) 0.0266(16) 0.0014(13) -0.0006(14) 0.0019(14) C25 0.0351(18) 0.0273(17) 0.0266(16) -0.0052(13) -0.0012(14) -0.0054(14) C26 0.0362(19) 0.0271(17) 0.0214(15) -0.0019(13) -0.0048(14) -0.0025(14) C27 0.039(2) 0.0350(19) 0.0321(18) -0.0055(15) -0.0060(16) -0.0093(16) C28 0.0297(18) 0.052(2) 0.0378(19) -0.0034(17) -0.0031(16) -0.0042(17) C29 0.0343(19) 0.0382(19) 0.0309(17) -0.0028(15) -0.0048(15) 0.0071(15) C30 0.0354(18) 0.0294(17) 0.0244(16) 0.0011(13) -0.0047(14) 0.0018(15) C31 0.0371(19) 0.0362(19) 0.0296(17) -0.0052(14) 0.0029(15) 0.0060(15) C32 0.0289(17) 0.043(2) 0.0285(17) -0.0054(15) 0.0010(15) -0.0026(15) C33 0.044(2) 0.055(2) 0.0332(19) -0.0100(17) 0.0062(17) 0.0041(18) C34 0.052(2) 0.077(3) 0.0253(18) -0.0063(19) 0.0073(18) 0.005(2) C35 0.045(2) 0.071(3) 0.0247(18) 0.0084(18) -0.0014(16) 0.001(2) C36 0.0359(19) 0.047(2) 0.0293(17) 0.0045(16) -0.0029(15) -0.0003(16) C37 0.0371(19) 0.0267(16) 0.0255(16) 0.0062(14) -0.0033(15) -0.0072(14) C38 0.043(2) 0.057(2) 0.052(2) -0.0091(19) 0.0072(19) -0.0111(19) C39 0.0346(19) 0.0265(17) 0.0328(18) 0.0050(14) 0.0017(15) -0.0028(14) C40 0.066(3) 0.0307(19) 0.041(2) 0.0085(16) 0.0054(19) 0.0022(18) Cl1 0.0537(6) 0.0293(4) 0.0451(5) -0.0038(4) -0.0035(4) -0.0026(4) O1A 0.0631(18) 0.0504(16) 0.0693(19) -0.0149(14) -0.0126(15) -0.0140(14) O1B 0.148(3) 0.0454(17) 0.0640(19) 0.0061(15) 0.021(2) -0.0157(19) O1C 0.089(2) 0.068(2) 0.071(2) -0.0355(16) 0.0083(18) -0.0091(17) O1D 0.069(2) 0.0534(19) 0.145(3) 0.015(2) -0.033(2) 0.0077(16) Cl2 0.0436(5) 0.0454(5) 0.0595(6) 0.0097(5) 0.0138(5) 0.0009(4) O2A 0.059(2) 0.090(3) 0.157(4) 0.030(2) 0.004(2) 0.0325(19) O2B 0.215(5) 0.127(3) 0.061(2) -0.026(2) 0.040(3) 0.052(3) O2C 0.097(3) 0.130(3) 0.143(4) 0.072(3) -0.019(3) -0.064(3) O2D 0.091(2) 0.071(2) 0.0576(18) 0.0189(15) 0.0130(17) -0.0124(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 Co2 3.4454(5) . ? Co1 O2 2.031(2) . ? Co1 O1 2.0474(19) . ? Co1 O4 2.083(2) . ? Co1 N3 2.113(3) . ? Co1 N2 2.132(2) . ? Co1 N1 2.157(3) . ? Co2 O1 1.9032(18) . ? Co2 O5 1.905(2) . ? Co2 O3 1.921(2) . ? Co2 N5 1.925(3) . ? Co2 N6 1.951(2) . ? Co2 N4 1.968(2) . ? O1 C1 1.358(3) . ? O2 C37 1.261(4) . ? O3 C37 1.285(4) . ? O4 C39 1.237(4) . ? O5 C39 1.294(4) . ? N1 C18 1.480(4) . ? N1 C12 1.484(4) . ? N1 C11 1.486(4) . ? N2 C17 1.336(4) . ? N2 C13 1.344(4) . ? N3 C19 1.340(4) . ? N3 C23 1.343(4) . ? N4 C31 1.494(4) . ? N4 C24 1.500(4) . ? N4 C25 1.501(4) . ? N5 C30 1.349(4) . ? N5 C26 1.349(4) . ? N6 C36 1.335(4) . ? N6 C32 1.349(4) . ? C1 C2 1.390(4) . ? C1 C6 1.391(4) . ? C2 C3 1.398(4) . ? C2 C11 1.505(4) . ? C3 C4 1.391(4) . ? C3 H3A 0.950 . ? C4 C5 1.385(4) . ? C4 C7 1.539(4) . ? C5 C6 1.388(4) . ? C5 H5A 0.950 . ? C6 C24 1.501(4) . ? C7 C9 1.515(5) . ? C7 C10 1.526(5) . ? C7 C8 1.552(5) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 C13 1.495(4) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.391(4) . ? C14 C15 1.377(5) . ? C14 H14A 0.950 . ? C15 C16 1.381(5) . ? C15 H15A 0.950 . ? C16 C17 1.377(5) . ? C16 H16A 0.950 . ? C17 H17A 0.950 . ? C18 C19 1.508(5) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 C20 1.390(4) . ? C20 C21 1.377(6) . ? C20 H20A 0.950 . ? C21 C22 1.362(6) . ? C21 H21A 0.950 . ? C22 C23 1.384(5) . ? C22 H22A 0.950 . ? C23 H23A 0.950 . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 C26 1.486(4) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.381(4) . ? C27 C28 1.384(5) . ? C27 H27A 0.950 . ? C28 C29 1.375(5) . ? C28 H28A 0.950 . ? C29 C30 1.362(4) . ? C29 H29A 0.950 . ? C30 H30A 0.950 . ? C31 C32 1.488(4) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 C33 1.380(4) . ? C33 C34 1.377(5) . ? C33 H33A 0.950 . ? C34 C35 1.369(5) . ? C34 H34A 0.950 . ? C35 C36 1.386(5) . ? C35 H35A 0.950 . ? C36 H36A 0.950 . ? C37 C38 1.476(5) . ? C38 H38A 0.980 . ? C38 H38B 0.980 . ? C38 H38C 0.980 . ? C39 C40 1.505(4) . ? C40 H40A 0.980 . ? C40 H40B 0.980 . ? C40 H40C 0.980 . ? Cl1 O1D 1.409(3) . ? Cl1 O1B 1.416(3) . ? Cl1 O1C 1.426(3) . ? Cl1 O1A 1.429(3) . ? Cl2 O2A 1.376(3) . ? Cl2 O2B 1.379(3) . ? Cl2 O2C 1.403(3) . ? Cl2 O2D 1.432(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 O2 Co1 O1 92.40(8) . . ? O2 Co1 O4 89.37(9) . . ? O1 Co1 O4 87.33(8) . . ? O2 Co1 N3 99.74(10) . . ? O1 Co1 N3 166.56(10) . . ? O4 Co1 N3 87.05(9) . . ? O2 Co1 N2 95.09(10) . . ? O1 Co1 N2 86.89(8) . . ? O4 Co1 N2 172.84(10) . . ? N3 Co1 N2 97.68(10) . . ? O2 Co1 N1 174.21(9) . . ? O1 Co1 N1 90.60(8) . . ? O4 Co1 N1 95.71(9) . . ? N3 Co1 N1 77.83(10) . . ? N2 Co1 N1 80.13(10) . . ? O1 Co2 O5 95.56(8) . . ? O1 Co2 O3 93.11(9) . . ? O5 Co2 O3 90.86(9) . . ? O1 Co2 N5 86.30(9) . . ? O5 Co2 N5 92.60(10) . . ? O3 Co2 N5 176.53(10) . . ? O1 Co2 N6 175.03(10) . . ? O5 Co2 N6 89.00(10) . . ? O3 Co2 N6 84.84(10) . . ? N5 Co2 N6 95.48(10) . . ? O1 Co2 N4 93.97(9) . . ? O5 Co2 N4 170.09(9) . . ? O3 Co2 N4 91.33(10) . . ? N5 Co2 N4 85.31(10) . . ? N6 Co2 N4 81.58(10) . . ? C1 O1 Co2 119.91(16) . . ? C1 O1 Co1 118.61(16) . . ? Co2 O1 Co1 121.37(9) . . ? C37 O2 Co1 133.9(2) . . ? C37 O3 Co2 131.8(2) . . ? C39 O4 Co1 128.7(2) . . ? C39 O5 Co2 135.09(19) . . ? C18 N1 C12 110.5(2) . . ? C18 N1 C11 110.6(2) . . ? C12 N1 C11 111.3(2) . . ? C18 N1 Co1 105.32(18) . . ? C12 N1 Co1 108.43(19) . . ? C11 N1 Co1 110.45(17) . . ? C17 N2 C13 118.8(3) . . ? C17 N2 Co1 124.2(2) . . ? C13 N2 Co1 113.2(2) . . ? C19 N3 C23 119.0(3) . . ? C19 N3 Co1 114.6(2) . . ? C23 N3 Co1 126.3(3) . . ? C31 N4 C24 111.1(2) . . ? C31 N4 C25 108.5(2) . . ? C24 N4 C25 110.1(2) . . ? C31 N4 Co2 106.27(18) . . ? C24 N4 Co2 112.26(17) . . ? C25 N4 Co2 108.49(18) . . ? C30 N5 C26 118.6(3) . . ? C30 N5 Co2 124.5(2) . . ? C26 N5 Co2 114.5(2) . . ? C36 N6 C32 119.9(3) . . ? C36 N6 Co2 126.5(2) . . ? C32 N6 Co2 113.7(2) . . ? O1 C1 C2 120.0(2) . . ? O1 C1 C6 119.8(3) . . ? C2 C1 C6 120.2(3) . . ? C1 C2 C3 118.7(3) . . ? C1 C2 C11 120.7(3) . . ? C3 C2 C11 120.5(3) . . ? C4 C3 C2 122.2(3) . . ? C4 C3 H3A 118.9 . . ? C2 C3 H3A 118.9 . . ? C5 C4 C3 117.3(3) . . ? C5 C4 C7 120.0(3) . . ? C3 C4 C7 122.7(3) . . ? C4 C5 C6 122.1(3) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C1 119.5(3) . . ? C5 C6 C24 122.4(3) . . ? C1 C6 C24 118.1(3) . . ? C9 C7 C10 110.2(4) . . ? C9 C7 C4 112.7(3) . . ? C10 C7 C4 109.0(3) . . ? C9 C7 C8 107.9(3) . . ? C10 C7 C8 108.7(3) . . ? C4 C7 C8 108.3(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C2 110.5(2) . . ? N1 C11 H11A 109.6 . . ? C2 C11 H11A 109.6 . . ? N1 C11 H11B 109.6 . . ? C2 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? N1 C12 C13 111.5(2) . . ? N1 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? N1 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? N2 C13 C14 121.4(3) . . ? N2 C13 C12 115.9(3) . . ? C14 C13 C12 122.7(3) . . ? C15 C14 C13 119.1(3) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C14 C15 C16 119.3(3) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C17 C16 C15 118.5(3) . . ? C17 C16 H16A 120.8 . . ? C15 C16 H16A 120.8 . . ? N2 C17 C16 122.9(3) . . ? N2 C17 H17A 118.6 . . ? C16 C17 H17A 118.6 . . ? N1 C18 C19 108.8(3) . . ? N1 C18 H18A 109.9 . . ? C19 C18 H18A 109.9 . . ? N1 C18 H18B 109.9 . . ? C19 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? N3 C19 C20 121.8(3) . . ? N3 C19 C18 115.2(3) . . ? C20 C19 C18 123.1(3) . . ? C21 C20 C19 118.5(4) . . ? C21 C20 H20A 120.7 . . ? C19 C20 H20A 120.7 . . ? C22 C21 C20 119.8(3) . . ? C22 C21 H21A 120.1 . . ? C20 C21 H21A 120.1 . . ? C21 C22 C23 119.2(4) . . ? C21 C22 H22A 120.4 . . ? C23 C22 H22A 120.4 . . ? N3 C23 C22 121.6(4) . . ? N3 C23 H23A 119.2 . . ? C22 C23 H23A 119.2 . . ? N4 C24 C6 110.0(2) . . ? N4 C24 H24A 109.7 . . ? C6 C24 H24A 109.7 . . ? N4 C24 H24B 109.7 . . ? C6 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C26 C25 N4 109.4(2) . . ? C26 C25 H25A 109.8 . . ? N4 C25 H25A 109.8 . . ? C26 C25 H25B 109.8 . . ? N4 C25 H25B 109.8 . . ? H25A C25 H25B 108.2 . . ? N5 C26 C27 121.5(3) . . ? N5 C26 C25 114.2(3) . . ? C27 C26 C25 124.3(3) . . ? C26 C27 C28 119.1(3) . . ? C26 C27 H27A 120.5 . . ? C28 C27 H27A 120.5 . . ? C29 C28 C27 119.1(3) . . ? C29 C28 H28A 120.4 . . ? C27 C28 H28A 120.4 . . ? C30 C29 C28 119.3(3) . . ? C30 C29 H29A 120.3 . . ? C28 C29 H29A 120.3 . . ? N5 C30 C29 122.4(3) . . ? N5 C30 H30A 118.8 . . ? C29 C30 H30A 118.8 . . ? C32 C31 N4 106.2(2) . . ? C32 C31 H31A 110.5 . . ? N4 C31 H31A 110.5 . . ? C32 C31 H31B 110.5 . . ? N4 C31 H31B 110.5 . . ? H31A C31 H31B 108.7 . . ? N6 C32 C33 121.0(3) . . ? N6 C32 C31 114.5(3) . . ? C33 C32 C31 124.4(3) . . ? C34 C33 C32 119.1(3) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? C35 C34 C33 119.7(3) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C34 C35 C36 119.2(3) . . ? C34 C35 H35A 120.4 . . ? C36 C35 H35A 120.4 . . ? N6 C36 C35 121.2(3) . . ? N6 C36 H36A 119.4 . . ? C35 C36 H36A 119.4 . . ? O2 C37 O3 125.5(3) . . ? O2 C37 C38 118.8(3) . . ? O3 C37 C38 115.7(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O4 C39 O5 126.6(3) . . ? O4 C39 C40 118.9(3) . . ? O5 C39 C40 114.4(3) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O1D Cl1 O1B 110.3(2) . . ? O1D Cl1 O1C 108.8(2) . . ? O1B Cl1 O1C 107.64(19) . . ? O1D Cl1 O1A 108.79(18) . . ? O1B Cl1 O1A 111.07(19) . . ? O1C Cl1 O1A 110.16(18) . . ? O2A Cl2 O2B 110.8(3) . . ? O2A Cl2 O2C 111.1(3) . . ? O2B Cl2 O2C 109.6(3) . . ? O2A Cl2 O2D 109.0(2) . . ? O2B Cl2 O2D 108.2(2) . . ? O2C Cl2 O2D 108.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Co2 O1 C1 -143.0(2) . . . . ? O3 Co2 O1 C1 125.8(2) . . . . ? N5 Co2 O1 C1 -50.8(2) . . . . ? N4 Co2 O1 C1 34.2(2) . . . . ? O5 Co2 O1 Co1 40.93(12) . . . . ? O3 Co2 O1 Co1 -50.23(12) . . . . ? N5 Co2 O1 Co1 133.19(12) . . . . ? N4 Co2 O1 Co1 -141.78(12) . . . . ? O2 Co1 O1 C1 -140.0(2) . . . . ? O4 Co1 O1 C1 130.7(2) . . . . ? N3 Co1 O1 C1 65.4(4) . . . . ? N2 Co1 O1 C1 -45.0(2) . . . . ? N1 Co1 O1 C1 35.0(2) . . . . ? O2 Co1 O1 Co2 36.05(13) . . . . ? O4 Co1 O1 Co2 -53.21(12) . . . . ? N3 Co1 O1 Co2 -118.6(4) . . . . ? N2 Co1 O1 Co2 131.02(13) . . . . ? N1 Co1 O1 Co2 -148.90(12) . . . . ? O1 Co1 O2 C37 -0.1(3) . . . . ? O4 Co1 O2 C37 87.2(3) . . . . ? N3 Co1 O2 C37 174.1(3) . . . . ? N2 Co1 O2 C37 -87.2(3) . . . . ? O1 Co2 O3 C37 44.7(3) . . . . ? O5 Co2 O3 C37 -50.9(3) . . . . ? N6 Co2 O3 C37 -139.9(3) . . . . ? N4 Co2 O3 C37 138.7(3) . . . . ? O2 Co1 O4 C39 -46.1(3) . . . . ? O1 Co1 O4 C39 46.3(3) . . . . ? N3 Co1 O4 C39 -145.9(3) . . . . ? N1 Co1 O4 C39 136.7(3) . . . . ? O1 Co2 O5 C39 -4.6(3) . . . . ? O3 Co2 O5 C39 88.6(3) . . . . ? N5 Co2 O5 C39 -91.2(3) . . . . ? N6 Co2 O5 C39 173.4(3) . . . . ? O1 Co1 N1 C18 139.91(19) . . . . ? O4 Co1 N1 C18 52.53(19) . . . . ? N3 Co1 N1 C18 -33.20(19) . . . . ? N2 Co1 N1 C18 -133.3(2) . . . . ? O1 Co1 N1 C12 -101.74(18) . . . . ? O4 Co1 N1 C12 170.88(18) . . . . ? N3 Co1 N1 C12 85.15(19) . . . . ? N2 Co1 N1 C12 -15.00(18) . . . . ? O1 Co1 N1 C11 20.49(18) . . . . ? O4 Co1 N1 C11 -66.88(18) . . . . ? N3 Co1 N1 C11 -152.61(19) . . . . ? N2 Co1 N1 C11 107.24(18) . . . . ? O2 Co1 N2 C17 20.9(3) . . . . ? O1 Co1 N2 C17 -71.2(2) . . . . ? N3 Co1 N2 C17 121.5(2) . . . . ? N1 Co1 N2 C17 -162.4(3) . . . . ? O2 Co1 N2 C13 178.8(2) . . . . ? O1 Co1 N2 C13 86.7(2) . . . . ? N3 Co1 N2 C13 -80.6(2) . . . . ? N1 Co1 N2 C13 -4.5(2) . . . . ? O2 Co1 N3 C19 -169.4(2) . . . . ? O1 Co1 N3 C19 -15.2(5) . . . . ? O4 Co1 N3 C19 -80.6(2) . . . . ? N2 Co1 N3 C19 94.0(2) . . . . ? N1 Co1 N3 C19 15.9(2) . . . . ? O2 Co1 N3 C23 14.6(3) . . . . ? O1 Co1 N3 C23 168.8(3) . . . . ? O4 Co1 N3 C23 103.4(3) . . . . ? N2 Co1 N3 C23 -82.0(3) . . . . ? N1 Co1 N3 C23 -160.1(3) . . . . ? O1 Co2 N4 C31 142.06(18) . . . . ? O3 Co2 N4 C31 48.85(19) . . . . ? N5 Co2 N4 C31 -131.98(19) . . . . ? N6 Co2 N4 C31 -35.73(19) . . . . ? O1 Co2 N4 C24 20.4(2) . . . . ? O3 Co2 N4 C24 -72.77(19) . . . . ? N5 Co2 N4 C24 106.4(2) . . . . ? N6 Co2 N4 C24 -157.4(2) . . . . ? O1 Co2 N4 C25 -101.40(18) . . . . ? O3 Co2 N4 C25 165.39(18) . . . . ? N5 Co2 N4 C25 -15.44(18) . . . . ? N6 Co2 N4 C25 80.81(18) . . . . ? O1 Co2 N5 C30 -69.3(2) . . . . ? O5 Co2 N5 C30 26.1(2) . . . . ? N6 Co2 N5 C30 115.3(2) . . . . ? N4 Co2 N5 C30 -163.6(2) . . . . ? O1 Co2 N5 C26 93.1(2) . . . . ? O5 Co2 N5 C26 -171.5(2) . . . . ? N6 Co2 N5 C26 -82.3(2) . . . . ? N4 Co2 N5 C26 -1.2(2) . . . . ? O5 Co2 N6 C36 17.2(3) . . . . ? O3 Co2 N6 C36 108.2(3) . . . . ? N5 Co2 N6 C36 -75.3(3) . . . . ? N4 Co2 N6 C36 -159.7(3) . . . . ? O5 Co2 N6 C32 -162.1(2) . . . . ? O3 Co2 N6 C32 -71.1(2) . . . . ? N5 Co2 N6 C32 105.4(2) . . . . ? N4 Co2 N6 C32 21.0(2) . . . . ? Co2 O1 C1 C2 131.4(2) . . . . ? Co1 O1 C1 C2 -52.5(3) . . . . ? Co2 O1 C1 C6 -50.3(3) . . . . ? Co1 O1 C1 C6 125.9(2) . . . . ? O1 C1 C2 C3 178.9(3) . . . . ? C6 C1 C2 C3 0.6(4) . . . . ? O1 C1 C2 C11 3.7(4) . . . . ? C6 C1 C2 C11 -174.6(3) . . . . ? C1 C2 C3 C4 -0.2(5) . . . . ? C11 C2 C3 C4 175.0(3) . . . . ? C2 C3 C4 C5 0.2(5) . . . . ? C2 C3 C4 C7 -179.4(3) . . . . ? C3 C4 C5 C6 -0.6(5) . . . . ? C7 C4 C5 C6 179.0(3) . . . . ? C4 C5 C6 C1 1.0(4) . . . . ? C4 C5 C6 C24 179.5(3) . . . . ? O1 C1 C6 C5 -179.3(3) . . . . ? C2 C1 C6 C5 -1.0(4) . . . . ? O1 C1 C6 C24 2.1(4) . . . . ? C2 C1 C6 C24 -179.5(3) . . . . ? C5 C4 C7 C9 -175.0(4) . . . . ? C3 C4 C7 C9 4.6(5) . . . . ? C5 C4 C7 C10 62.4(4) . . . . ? C3 C4 C7 C10 -118.0(4) . . . . ? C5 C4 C7 C8 -55.8(4) . . . . ? C3 C4 C7 C8 123.9(4) . . . . ? C18 N1 C11 C2 179.6(2) . . . . ? C12 N1 C11 C2 56.3(3) . . . . ? Co1 N1 C11 C2 -64.2(3) . . . . ? C1 C2 C11 N1 61.7(3) . . . . ? C3 C2 C11 N1 -113.4(3) . . . . ? C18 N1 C12 C13 146.0(3) . . . . ? C11 N1 C12 C13 -90.7(3) . . . . ? Co1 N1 C12 C13 31.1(3) . . . . ? C17 N2 C13 C14 0.8(4) . . . . ? Co1 N2 C13 C14 -158.4(2) . . . . ? C17 N2 C13 C12 -176.8(3) . . . . ? Co1 N2 C13 C12 24.0(3) . . . . ? N1 C12 C13 N2 -37.8(4) . . . . ? N1 C12 C13 C14 144.6(3) . . . . ? N2 C13 C14 C15 -0.9(5) . . . . ? C12 C13 C14 C15 176.6(3) . . . . ? C13 C14 C15 C16 -0.2(5) . . . . ? C14 C15 C16 C17 1.2(5) . . . . ? C13 N2 C17 C16 0.3(4) . . . . ? Co1 N2 C17 C16 157.0(2) . . . . ? C15 C16 C17 N2 -1.2(5) . . . . ? C12 N1 C18 C19 -71.6(3) . . . . ? C11 N1 C18 C19 164.7(2) . . . . ? Co1 N1 C18 C19 45.3(3) . . . . ? C23 N3 C19 C20 1.8(5) . . . . ? Co1 N3 C19 C20 -174.5(2) . . . . ? C23 N3 C19 C18 -177.9(3) . . . . ? Co1 N3 C19 C18 5.8(3) . . . . ? N1 C18 C19 N3 -35.4(4) . . . . ? N1 C18 C19 C20 144.8(3) . . . . ? N3 C19 C20 C21 -1.3(5) . . . . ? C18 C19 C20 C21 178.4(3) . . . . ? C19 C20 C21 C22 -0.5(5) . . . . ? C20 C21 C22 C23 1.6(5) . . . . ? C19 N3 C23 C22 -0.6(5) . . . . ? Co1 N3 C23 C22 175.2(2) . . . . ? C21 C22 C23 N3 -1.1(5) . . . . ? C31 N4 C24 C6 177.7(2) . . . . ? C25 N4 C24 C6 57.5(3) . . . . ? Co2 N4 C24 C6 -63.4(3) . . . . ? C5 C6 C24 N4 -120.2(3) . . . . ? C1 C6 C24 N4 58.3(3) . . . . ? C31 N4 C25 C26 143.0(2) . . . . ? C24 N4 C25 C26 -95.2(3) . . . . ? Co2 N4 C25 C26 28.0(3) . . . . ? C30 N5 C26 C27 1.4(4) . . . . ? Co2 N5 C26 C27 -162.1(2) . . . . ? C30 N5 C26 C25 -178.1(2) . . . . ? Co2 N5 C26 C25 18.4(3) . . . . ? N4 C25 C26 N5 -30.8(3) . . . . ? N4 C25 C26 C27 149.8(3) . . . . ? N5 C26 C27 C28 -0.1(5) . . . . ? C25 C26 C27 C28 179.3(3) . . . . ? C26 C27 C28 C29 -1.6(5) . . . . ? C27 C28 C29 C30 1.9(5) . . . . ? C26 N5 C30 C29 -1.0(4) . . . . ? Co2 N5 C30 C29 160.7(2) . . . . ? C28 C29 C30 N5 -0.6(5) . . . . ? C24 N4 C31 C32 165.8(2) . . . . ? C25 N4 C31 C32 -73.1(3) . . . . ? Co2 N4 C31 C32 43.4(3) . . . . ? C36 N6 C32 C33 1.8(5) . . . . ? Co2 N6 C32 C33 -178.9(3) . . . . ? C36 N6 C32 C31 -179.5(3) . . . . ? Co2 N6 C32 C31 -0.1(3) . . . . ? N4 C31 C32 N6 -28.9(4) . . . . ? N4 C31 C32 C33 149.8(3) . . . . ? N6 C32 C33 C34 -1.0(5) . . . . ? C31 C32 C33 C34 -179.6(3) . . . . ? C32 C33 C34 C35 -0.9(6) . . . . ? C33 C34 C35 C36 2.0(6) . . . . ? C32 N6 C36 C35 -0.6(5) . . . . ? Co2 N6 C36 C35 -179.9(3) . . . . ? C34 C35 C36 N6 -1.3(5) . . . . ? Co1 O2 C37 O3 -10.4(5) . . . . ? Co1 O2 C37 C38 168.3(2) . . . . ? Co2 O3 C37 O2 -17.8(5) . . . . ? Co2 O3 C37 C38 163.5(2) . . . . ? Co1 O4 C39 O5 -23.3(5) . . . . ? Co1 O4 C39 C40 159.3(2) . . . . ? Co2 O5 C39 O4 -4.9(5) . . . . ? Co2 O5 C39 C40 172.6(2) . . . . ? #============================================================================== data_14_MeOH _database_code_depnum_ccdc_archive 'CCDC 772410' #TrackingRef '- submit_all.cif' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H39 Co2 F6 N6 O5 +, Cl O4 -, C H4 O' _chemical_formula_sum 'C41 H43 Cl Co2 F6 N6 O10' _chemical_formula_weight 1047.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 12.6557(12) _cell_length_b 21.836(2) _cell_length_c 17.0944(15) _cell_angle_alpha 90.00 _cell_angle_beta 98.764(3) _cell_angle_gamma 90.00 _cell_volume 4668.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9022 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 24.38 _exptl_crystal_description plat _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ? _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 89141 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 25.50 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.990 _reflns_number_total 8621 _reflns_number_gt 6984 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+14.9420P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8621 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1570 _refine_ls_wR_factor_gt 0.1479 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.905 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.088 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.47268(4) 0.19810(3) 0.57557(3) 0.02376(15) Uani 1 1 d . . . Co2 Co 0.58546(4) 0.27047(2) 0.75169(3) 0.02437(15) Uani 1 1 d . . . F1 F 0.1668(3) 0.1968(3) 0.7015(3) 0.122(2) Uani 1 1 d . . . F2 F 0.2343(3) 0.2483(3) 0.7997(2) 0.116(2) Uani 1 1 d . . . F3 F 0.1841(3) 0.2888(3) 0.6871(3) 0.1163(19) Uani 1 1 d . . . F4 F 0.5666(3) 0.08080(14) 0.85354(17) 0.0634(9) Uani 1 1 d . . . F5 F 0.5022(3) 0.03535(16) 0.7493(2) 0.0810(12) Uani 1 1 d . . . F6 F 0.6691(3) 0.04427(17) 0.7803(3) 0.0895(14) Uani 1 1 d . . . O1 O 0.5637(2) 0.26485(12) 0.63288(15) 0.0236(6) Uani 1 1 d . . . O2 O 0.3455(2) 0.20432(15) 0.63887(17) 0.0353(7) Uani 1 1 d . . . O3 O 0.4140(2) 0.26035(17) 0.74457(18) 0.0411(8) Uani 1 1 d . . . O4 O 0.5437(3) 0.13089(14) 0.66117(17) 0.0351(7) Uani 1 1 d . . . O5 O 0.6060(3) 0.17905(13) 0.77515(17) 0.0359(7) Uani 1 1 d . . . N1 N 0.5823(3) 0.19156(16) 0.4889(2) 0.0283(8) Uani 1 1 d . . . N2 N 0.4047(3) 0.26493(16) 0.4915(2) 0.0290(8) Uani 1 1 d . . . N3 N 0.4181(3) 0.11871(16) 0.5114(2) 0.0300(8) Uani 1 1 d . . . N4 N 0.5781(3) 0.36938(16) 0.74661(19) 0.0265(7) Uani 1 1 d . . . N5 N 0.7486(3) 0.29074(16) 0.7500(2) 0.0269(7) Uani 1 1 d . . . N6 N 0.5669(3) 0.29372(17) 0.8687(2) 0.0310(8) Uani 1 1 d . . . C1 C 0.6119(3) 0.30677(18) 0.5917(2) 0.0246(8) Uani 1 1 d . . . C2 C 0.6740(3) 0.2877(2) 0.5348(2) 0.0280(9) Uani 1 1 d . . . C3 C 0.7195(3) 0.3314(2) 0.4916(3) 0.0322(10) Uani 1 1 d . . . H3A H 0.7615 0.3180 0.4533 0.039 Uiso 1 1 calc R . . C4 C 0.7066(3) 0.3936(2) 0.5017(3) 0.0333(10) Uani 1 1 d . . . C5 C 0.6465(3) 0.4115(2) 0.5596(3) 0.0327(10) Uani 1 1 d . . . H5A H 0.6373 0.4539 0.5687 0.039 Uiso 1 1 calc R . . C6 C 0.5995(3) 0.36926(19) 0.6043(2) 0.0273(9) Uani 1 1 d . . . C7 C 0.7541(4) 0.4425(2) 0.4525(3) 0.0476(13) Uani 1 1 d . . . C8 C 0.6655(5) 0.4857(3) 0.4132(4) 0.0643(16) Uani 1 1 d . . . H8A H 0.6129 0.4622 0.3772 0.096 Uiso 1 1 calc R . . H8B H 0.6969 0.5173 0.3833 0.096 Uiso 1 1 calc R . . H8C H 0.6302 0.5050 0.4540 0.096 Uiso 1 1 calc R . . C9 C 0.8052(6) 0.4139(3) 0.3862(4) 0.077(2) Uani 1 1 d . . . H9A H 0.7510 0.3910 0.3507 0.115 Uiso 1 1 calc R . . H9B H 0.8625 0.3860 0.4088 0.115 Uiso 1 1 calc R . . H9C H 0.8349 0.4462 0.3563 0.115 Uiso 1 1 calc R . . C10 C 0.8358(5) 0.4799(3) 0.5085(4) 0.078(2) Uani 1 1 d . . . H10A H 0.8927 0.4527 0.5337 0.116 Uiso 1 1 calc R . . H10B H 0.8003 0.4991 0.5493 0.116 Uiso 1 1 calc R . . H10C H 0.8667 0.5116 0.4784 0.116 Uiso 1 1 calc R . . C11 C 0.6865(3) 0.2204(2) 0.5207(3) 0.0298(9) Uani 1 1 d . . . H11A H 0.7374 0.2142 0.4828 0.036 Uiso 1 1 calc R . . H11B H 0.7165 0.2002 0.5711 0.036 Uiso 1 1 calc R . . C12 C 0.5319(4) 0.2220(2) 0.4156(2) 0.0319(10) Uani 1 1 d . . . H12A H 0.4890 0.1917 0.3813 0.038 Uiso 1 1 calc R . . H12B H 0.5884 0.2376 0.3866 0.038 Uiso 1 1 calc R . . C13 C 0.4613(3) 0.2740(2) 0.4316(2) 0.0304(9) Uani 1 1 d . . . C14 C 0.4496(4) 0.3265(2) 0.3856(3) 0.0394(11) Uani 1 1 d . . . H14A H 0.4919 0.3327 0.3449 0.047 Uiso 1 1 calc R . . C15 C 0.3749(4) 0.3699(2) 0.4000(3) 0.0483(13) Uani 1 1 d . . . H15A H 0.3636 0.4058 0.3683 0.058 Uiso 1 1 calc R . . C16 C 0.3172(4) 0.3603(2) 0.4609(3) 0.0473(13) Uani 1 1 d . . . H16A H 0.2660 0.3895 0.4722 0.057 Uiso 1 1 calc R . . C17 C 0.3347(4) 0.3080(2) 0.5050(3) 0.0371(11) Uani 1 1 d . . . H17A H 0.2951 0.3020 0.5474 0.044 Uiso 1 1 calc R . . C18 C 0.5947(4) 0.1255(2) 0.4763(3) 0.0335(10) Uani 1 1 d . . . H18A H 0.6426 0.1078 0.5218 0.040 Uiso 1 1 calc R . . H18B H 0.6277 0.1188 0.4281 0.040 Uiso 1 1 calc R . . C19 C 0.4884(4) 0.0942(2) 0.4674(2) 0.0316(10) Uani 1 1 d . . . C20 C 0.4618(4) 0.0442(2) 0.4192(3) 0.0388(11) Uani 1 1 d . . . H20A H 0.5109 0.0287 0.3873 0.047 Uiso 1 1 calc R . . C21 C 0.3631(4) 0.0168(2) 0.4176(3) 0.0422(12) Uani 1 1 d . . . H21A H 0.3440 -0.0178 0.3850 0.051 Uiso 1 1 calc R . . C22 C 0.2926(4) 0.0404(2) 0.4641(3) 0.0414(12) Uani 1 1 d . . . H22A H 0.2247 0.0220 0.4647 0.050 Uiso 1 1 calc R . . C23 C 0.3234(4) 0.0913(2) 0.5095(3) 0.0376(11) Uani 1 1 d . . . H23A H 0.2747 0.1078 0.5411 0.045 Uiso 1 1 calc R . . C24 C 0.5326(3) 0.3901(2) 0.6652(2) 0.0288(9) Uani 1 1 d . . . H24A H 0.5280 0.4354 0.6644 0.035 Uiso 1 1 calc R . . H24B H 0.4592 0.3737 0.6512 0.035 Uiso 1 1 calc R . . C25 C 0.6879(3) 0.39290(19) 0.7709(3) 0.0309(9) Uani 1 1 d . . . H25A H 0.7015 0.3979 0.8291 0.037 Uiso 1 1 calc R . . H25B H 0.6946 0.4336 0.7467 0.037 Uiso 1 1 calc R . . C26 C 0.7695(3) 0.35058(19) 0.7461(2) 0.0281(9) Uani 1 1 d . . . C27 C 0.8634(3) 0.3717(2) 0.7221(3) 0.0369(10) Uani 1 1 d . . . H27A H 0.8777 0.4144 0.7204 0.044 Uiso 1 1 calc R . . C28 C 0.9351(4) 0.3298(2) 0.7009(3) 0.0446(12) Uani 1 1 d . . . H28A H 0.9992 0.3433 0.6838 0.054 Uiso 1 1 calc R . . C29 C 0.9132(4) 0.2682(2) 0.7046(3) 0.0411(11) Uani 1 1 d . . . H29A H 0.9621 0.2385 0.6907 0.049 Uiso 1 1 calc R . . C30 C 0.8194(3) 0.2505(2) 0.7288(2) 0.0306(9) Uani 1 1 d . . . H30A H 0.8037 0.2080 0.7306 0.037 Uiso 1 1 calc R . . C31 C 0.5088(4) 0.3886(2) 0.8042(3) 0.0323(10) Uani 1 1 d . . . H31A H 0.4329 0.3847 0.7800 0.039 Uiso 1 1 calc R . . H31B H 0.5227 0.4322 0.8182 0.039 Uiso 1 1 calc R . . C32 C 0.5294(3) 0.3499(2) 0.8779(3) 0.0327(10) Uani 1 1 d . . . C33 C 0.5045(4) 0.3699(3) 0.9499(3) 0.0488(13) Uani 1 1 d . . . H33A H 0.4766 0.4099 0.9552 0.059 Uiso 1 1 calc R . . C34 C 0.5212(6) 0.3306(3) 1.0136(3) 0.0670(19) Uani 1 1 d . . . H34A H 0.5072 0.3436 1.0641 0.080 Uiso 1 1 calc R . . C35 C 0.5580(5) 0.2726(3) 1.0038(3) 0.0609(17) Uani 1 1 d . . . H35A H 0.5680 0.2446 1.0469 0.073 Uiso 1 1 calc R . . C36 C 0.5804(4) 0.2553(2) 0.9303(3) 0.0452(12) Uani 1 1 d . . . H36A H 0.6062 0.2151 0.9234 0.054 Uiso 1 1 calc R . . C37 C 0.3436(3) 0.2342(2) 0.7006(2) 0.0291(9) Uani 1 1 d . . . C38 C 0.2321(4) 0.2413(3) 0.7239(3) 0.0539(15) Uani 1 1 d . . . C39 C 0.5756(3) 0.13416(19) 0.7333(2) 0.0256(9) Uani 1 1 d . . . C40 C 0.5786(4) 0.0735(2) 0.7788(3) 0.0324(10) Uani 1 1 d . . . Cl1 Cl 0.90357(9) 0.07472(5) 0.68083(7) 0.0362(3) Uani 1 1 d . . . O1A O 0.9808(3) 0.12174(17) 0.7015(2) 0.0532(10) Uani 1 1 d . . . O1B O 0.9036(3) 0.03431(17) 0.7461(2) 0.0593(10) Uani 1 1 d . . . O1C O 0.9301(3) 0.04064(19) 0.6144(2) 0.0592(10) Uani 1 1 d . . . O1D O 0.8002(3) 0.10155(19) 0.6602(3) 0.0693(12) Uani 1 1 d . . . O1S O 0.1470(5) 0.0129(3) 0.6048(4) 0.115(2) Uani 1 1 d . . . H1S H 0.0820 0.0211 0.6075 0.172 Uiso 1 1 d R . . C1S C 0.2097(8) 0.0252(8) 0.6756(6) 0.187(7) Uani 1 1 d . . . H1S1 H 0.2726 -0.0016 0.6828 0.280 Uiso 1 1 d R . . H1S2 H 0.1686 0.0186 0.7190 0.280 Uiso 1 1 d R . . H1S3 H 0.2328 0.0680 0.6755 0.280 Uiso 1 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 Co1 0.0235(3) 0.0297(3) 0.0179(3) -0.0025(2) 0.0026(2) -0.0033(2) Co2 0.0254(3) 0.0279(3) 0.0193(3) -0.0046(2) 0.0018(2) 0.0005(2) F1 0.054(2) 0.181(5) 0.144(4) -0.057(4) 0.052(3) -0.062(3) F2 0.055(2) 0.253(6) 0.048(2) -0.026(3) 0.0324(19) -0.002(3) F3 0.060(3) 0.162(5) 0.132(4) 0.019(4) 0.030(3) 0.063(3) F4 0.105(3) 0.0512(19) 0.0377(17) 0.0066(14) 0.0232(17) -0.0013(18) F5 0.111(3) 0.059(2) 0.065(2) 0.0127(17) -0.016(2) -0.046(2) F6 0.075(2) 0.070(2) 0.137(4) 0.056(2) 0.059(3) 0.041(2) O1 0.0231(14) 0.0298(15) 0.0178(13) -0.0015(11) 0.0034(11) -0.0011(11) O2 0.0305(16) 0.0510(19) 0.0253(16) -0.0072(14) 0.0066(13) -0.0096(14) O3 0.0296(17) 0.063(2) 0.0322(17) -0.0165(16) 0.0101(14) -0.0094(15) O4 0.0446(18) 0.0323(17) 0.0262(16) -0.0027(13) -0.0021(14) -0.0010(14) O5 0.052(2) 0.0287(16) 0.0257(16) -0.0035(13) 0.0012(14) -0.0014(14) N1 0.0294(19) 0.0299(19) 0.0250(18) -0.0043(14) 0.0028(15) -0.0021(15) N2 0.0240(18) 0.036(2) 0.0251(18) -0.0021(15) -0.0012(14) -0.0013(15) N3 0.0326(19) 0.035(2) 0.0208(17) -0.0007(15) -0.0007(15) -0.0083(16) N4 0.0249(17) 0.0305(18) 0.0240(17) -0.0069(14) 0.0030(14) 0.0023(14) N5 0.0240(17) 0.0313(19) 0.0239(17) -0.0056(14) -0.0014(14) 0.0035(14) N6 0.033(2) 0.037(2) 0.0225(18) -0.0055(15) 0.0008(15) 0.0029(16) C1 0.022(2) 0.030(2) 0.021(2) -0.0024(16) 0.0006(16) -0.0029(16) C2 0.022(2) 0.034(2) 0.027(2) -0.0038(17) 0.0029(17) -0.0023(17) C3 0.025(2) 0.042(3) 0.031(2) -0.0022(19) 0.0090(18) -0.0053(19) C4 0.026(2) 0.039(3) 0.034(2) 0.001(2) 0.0039(18) -0.0078(19) C5 0.034(2) 0.028(2) 0.036(2) -0.0005(18) 0.0037(19) -0.0020(18) C6 0.023(2) 0.034(2) 0.025(2) 0.0000(17) 0.0024(16) 0.0013(17) C7 0.048(3) 0.047(3) 0.051(3) 0.004(2) 0.016(2) -0.013(2) C8 0.075(4) 0.063(4) 0.057(4) 0.022(3) 0.017(3) -0.002(3) C9 0.097(5) 0.061(4) 0.085(5) 0.017(3) 0.058(4) -0.003(4) C10 0.067(4) 0.071(4) 0.093(5) 0.016(4) 0.008(4) -0.035(4) C11 0.026(2) 0.037(2) 0.028(2) -0.0065(18) 0.0081(18) -0.0021(18) C12 0.040(2) 0.039(2) 0.018(2) -0.0040(17) 0.0090(18) -0.005(2) C13 0.034(2) 0.036(2) 0.019(2) -0.0008(17) -0.0034(17) -0.0078(19) C14 0.047(3) 0.042(3) 0.028(2) 0.003(2) 0.001(2) -0.010(2) C15 0.053(3) 0.042(3) 0.045(3) 0.011(2) -0.011(2) 0.001(2) C16 0.043(3) 0.047(3) 0.050(3) 0.002(2) 0.000(2) 0.009(2) C17 0.029(2) 0.045(3) 0.036(3) 0.002(2) 0.0004(19) 0.006(2) C18 0.039(2) 0.031(2) 0.032(2) -0.0090(19) 0.0096(19) 0.0000(19) C19 0.038(2) 0.031(2) 0.024(2) -0.0001(18) -0.0008(18) -0.0015(19) C20 0.052(3) 0.033(2) 0.029(2) -0.0040(19) -0.002(2) -0.002(2) C21 0.056(3) 0.032(2) 0.033(2) -0.003(2) -0.010(2) -0.007(2) C22 0.043(3) 0.039(3) 0.037(3) 0.004(2) -0.009(2) -0.015(2) C23 0.042(3) 0.041(3) 0.029(2) 0.001(2) 0.002(2) -0.010(2) C24 0.029(2) 0.030(2) 0.027(2) -0.0023(17) 0.0002(17) 0.0063(17) C25 0.031(2) 0.027(2) 0.033(2) -0.0094(18) -0.0001(18) -0.0016(18) C26 0.025(2) 0.031(2) 0.026(2) -0.0050(17) -0.0038(17) 0.0023(17) C27 0.028(2) 0.039(3) 0.042(3) 0.000(2) 0.002(2) -0.0024(19) C28 0.027(2) 0.054(3) 0.054(3) 0.005(2) 0.008(2) 0.003(2) C29 0.032(2) 0.050(3) 0.040(3) -0.003(2) 0.003(2) 0.014(2) C30 0.028(2) 0.031(2) 0.029(2) -0.0015(18) -0.0055(18) 0.0088(18) C31 0.035(2) 0.031(2) 0.033(2) -0.0064(18) 0.0096(19) 0.0087(19) C32 0.031(2) 0.039(3) 0.026(2) -0.0081(19) 0.0007(18) 0.0029(19) C33 0.060(3) 0.056(3) 0.030(3) -0.010(2) 0.010(2) 0.019(3) C34 0.107(5) 0.075(4) 0.021(3) -0.007(3) 0.016(3) 0.027(4) C35 0.088(5) 0.075(4) 0.020(2) 0.004(2) 0.007(3) 0.024(3) C36 0.059(3) 0.049(3) 0.025(2) 0.000(2) -0.001(2) 0.014(3) C37 0.026(2) 0.039(2) 0.024(2) 0.0043(18) 0.0078(18) 0.0001(18) C38 0.034(3) 0.086(4) 0.045(3) -0.011(3) 0.016(2) -0.001(3) C39 0.021(2) 0.029(2) 0.027(2) -0.0044(17) 0.0044(17) 0.0036(16) C40 0.037(2) 0.029(2) 0.032(2) -0.0034(18) 0.0072(19) -0.0013(19) Cl1 0.0387(6) 0.0294(5) 0.0408(6) -0.0031(5) 0.0067(5) -0.0071(4) O1A 0.061(2) 0.052(2) 0.048(2) -0.0148(17) 0.0136(18) -0.0292(18) O1B 0.079(3) 0.041(2) 0.062(2) 0.0127(18) 0.025(2) -0.0003(19) O1C 0.065(3) 0.063(3) 0.050(2) -0.0239(19) 0.0115(19) -0.012(2) O1D 0.054(2) 0.057(3) 0.091(3) -0.002(2) -0.009(2) 0.014(2) O1S 0.090(4) 0.163(6) 0.100(4) -0.009(4) 0.043(4) -0.002(4) C1S 0.086(7) 0.40(2) 0.073(6) 0.011(10) -0.004(5) -0.058(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 Co1 Co2 3.5056(8) . ? Co1 O1 2.017(3) . ? Co1 O2 2.076(3) . ? Co1 N3 2.111(3) . ? Co1 N2 2.135(4) . ? Co1 O4 2.168(3) . ? Co1 N1 2.184(3) . ? Co2 O1 2.011(3) . ? Co2 O5 2.045(3) . ? Co2 N6 2.112(3) . ? Co2 N5 2.116(4) . ? Co2 N4 2.163(4) . ? Co2 O3 2.166(3) . ? F1 C38 1.295(7) . ? F2 C38 1.300(6) . ? F3 C38 1.314(8) . ? F4 C40 1.319(5) . ? F5 C40 1.317(5) . ? F6 C40 1.308(5) . ? O1 C1 1.355(5) . ? O2 C37 1.244(5) . ? O3 C37 1.217(5) . ? O4 C39 1.239(5) . ? O5 C39 1.240(5) . ? N1 C18 1.469(5) . ? N1 C12 1.475(5) . ? N1 C11 1.487(5) . ? N2 C17 1.336(6) . ? N2 C13 1.350(6) . ? N3 C23 1.336(6) . ? N3 C19 1.359(6) . ? N4 C31 1.475(5) . ? N4 C25 1.481(5) . ? N4 C24 1.493(5) . ? N5 C26 1.337(5) . ? N5 C30 1.344(5) . ? N6 C32 1.333(6) . ? N6 C36 1.337(6) . ? C1 C6 1.394(6) . ? C1 C2 1.404(6) . ? C2 C3 1.384(6) . ? C2 C11 1.503(6) . ? C3 C4 1.382(6) . ? C3 H3A 0.950 . ? C4 C5 1.393(6) . ? C4 C7 1.536(6) . ? C5 C6 1.387(6) . ? C5 H5A 0.950 . ? C6 C24 1.510(6) . ? C7 C9 1.523(8) . ? C7 C10 1.533(8) . ? C7 C8 1.540(8) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 C13 1.495(6) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.387(6) . ? C14 C15 1.387(7) . ? C14 H14A 0.950 . ? C15 C16 1.376(8) . ? C15 H15A 0.950 . ? C16 C17 1.367(7) . ? C16 H16A 0.950 . ? C17 H17A 0.950 . ? C18 C19 1.495(6) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 C20 1.378(6) . ? C20 C21 1.381(7) . ? C20 H20A 0.950 . ? C21 C22 1.381(7) . ? C21 H21A 0.950 . ? C22 C23 1.379(7) . ? C22 H22A 0.950 . ? C23 H23A 0.950 . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 C26 1.494(6) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.394(6) . ? C27 C28 1.376(7) . ? C27 H27A 0.950 . ? C28 C29 1.377(7) . ? C28 H28A 0.950 . ? C29 C30 1.371(7) . ? C29 H29A 0.950 . ? C30 H30A 0.950 . ? C31 C32 1.508(6) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 C33 1.387(6) . ? C33 C34 1.378(8) . ? C33 H33A 0.950 . ? C34 C35 1.369(8) . ? C34 H34A 0.950 . ? C35 C36 1.382(7) . ? C35 H35A 0.950 . ? C36 H36A 0.950 . ? C37 C38 1.532(6) . ? C39 C40 1.534(6) . ? Cl1 O1B 1.423(4) . ? Cl1 O1A 1.424(3) . ? Cl1 O1D 1.427(4) . ? Cl1 O1C 1.439(4) . ? O1S C1S 1.369(10) . ? O1S H1S 0.850 . ? C1S H1S1 0.980 . ? C1S H1S2 0.980 . ? C1S H1S3 0.980 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 97.49(11) . . ? O1 Co1 N3 164.47(13) . . ? O2 Co1 N3 96.12(13) . . ? O1 Co1 N2 88.55(12) . . ? O2 Co1 N2 92.38(13) . . ? N3 Co1 N2 98.35(13) . . ? O1 Co1 O4 90.81(11) . . ? O2 Co1 O4 88.10(12) . . ? N3 Co1 O4 82.19(12) . . ? N2 Co1 O4 179.24(13) . . ? O1 Co1 N1 90.11(12) . . ? O2 Co1 N1 168.87(12) . . ? N3 Co1 N1 77.57(13) . . ? N2 Co1 N1 79.64(13) . . ? O4 Co1 N1 99.97(13) . . ? O1 Co2 O5 97.60(11) . . ? O1 Co2 N6 162.47(13) . . ? O5 Co2 N6 94.47(13) . . ? O1 Co2 N5 89.02(12) . . ? O5 Co2 N5 96.43(13) . . ? N6 Co2 N5 102.25(14) . . ? O1 Co2 N4 91.26(12) . . ? O5 Co2 N4 170.42(12) . . ? N6 Co2 N4 77.74(13) . . ? N5 Co2 N4 80.03(13) . . ? O1 Co2 O3 87.44(11) . . ? O5 Co2 O3 90.43(14) . . ? N6 Co2 O3 79.78(13) . . ? N5 Co2 O3 172.65(14) . . ? N4 Co2 O3 93.60(13) . . ? C1 O1 Co2 118.7(2) . . ? C1 O1 Co1 120.3(2) . . ? Co2 O1 Co1 120.98(13) . . ? C37 O2 Co1 126.4(3) . . ? C37 O3 Co2 135.7(3) . . ? C39 O4 Co1 132.1(3) . . ? C39 O5 Co2 129.7(3) . . ? C18 N1 C12 111.1(3) . . ? C18 N1 C11 111.1(3) . . ? C12 N1 C11 111.4(3) . . ? C18 N1 Co1 104.9(3) . . ? C12 N1 Co1 108.0(3) . . ? C11 N1 Co1 110.1(2) . . ? C17 N2 C13 118.1(4) . . ? C17 N2 Co1 125.1(3) . . ? C13 N2 Co1 113.9(3) . . ? C23 N3 C19 118.1(4) . . ? C23 N3 Co1 127.0(3) . . ? C19 N3 Co1 114.9(3) . . ? C31 N4 C25 110.0(3) . . ? C31 N4 C24 110.6(3) . . ? C25 N4 C24 111.6(3) . . ? C31 N4 Co2 106.5(3) . . ? C25 N4 Co2 107.6(2) . . ? C24 N4 Co2 110.4(2) . . ? C26 N5 C30 118.8(4) . . ? C26 N5 Co2 113.9(3) . . ? C30 N5 Co2 124.0(3) . . ? C32 N6 C36 119.3(4) . . ? C32 N6 Co2 115.2(3) . . ? C36 N6 Co2 125.2(3) . . ? O1 C1 C6 120.8(4) . . ? O1 C1 C2 120.2(4) . . ? C6 C1 C2 119.0(4) . . ? C3 C2 C1 119.2(4) . . ? C3 C2 C11 121.8(4) . . ? C1 C2 C11 119.0(4) . . ? C4 C3 C2 123.0(4) . . ? C4 C3 H3A 118.5 . . ? C2 C3 H3A 118.5 . . ? C3 C4 C5 116.9(4) . . ? C3 C4 C7 123.4(4) . . ? C5 C4 C7 119.7(4) . . ? C6 C5 C4 122.1(4) . . ? C6 C5 H5A 119.0 . . ? C4 C5 H5A 119.0 . . ? C5 C6 C1 119.9(4) . . ? C5 C6 C24 120.8(4) . . ? C1 C6 C24 119.3(4) . . ? C9 C7 C10 111.2(5) . . ? C9 C7 C4 111.6(4) . . ? C10 C7 C4 108.1(4) . . ? C9 C7 C8 106.8(5) . . ? C10 C7 C8 108.9(5) . . ? C4 C7 C8 110.2(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C2 111.3(3) . . ? N1 C11 H11A 109.4 . . ? C2 C11 H11A 109.4 . . ? N1 C11 H11B 109.4 . . ? C2 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N1 C12 C13 112.3(3) . . ? N1 C12 H12A 109.1 . . ? C13 C12 H12A 109.1 . . ? N1 C12 H12B 109.1 . . ? C13 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? N2 C13 C14 121.9(4) . . ? N2 C13 C12 115.4(4) . . ? C14 C13 C12 122.6(4) . . ? C13 C14 C15 118.7(5) . . ? C13 C14 H14A 120.6 . . ? C15 C14 H14A 120.6 . . ? C16 C15 C14 119.0(5) . . ? C16 C15 H15A 120.5 . . ? C14 C15 H15A 120.5 . . ? C17 C16 C15 119.0(5) . . ? C17 C16 H16A 120.5 . . ? C15 C16 H16A 120.5 . . ? N2 C17 C16 123.3(5) . . ? N2 C17 H17A 118.4 . . ? C16 C17 H17A 118.4 . . ? N1 C18 C19 110.5(4) . . ? N1 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? N1 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? N3 C19 C20 121.4(4) . . ? N3 C19 C18 114.7(4) . . ? C20 C19 C18 123.9(4) . . ? C19 C20 C21 119.5(5) . . ? C19 C20 H20A 120.2 . . ? C21 C20 H20A 120.2 . . ? C20 C21 C22 119.3(4) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C23 C22 C21 118.2(5) . . ? C23 C22 H22A 120.9 . . ? C21 C22 H22A 120.9 . . ? N3 C23 C22 123.4(5) . . ? N3 C23 H23A 118.3 . . ? C22 C23 H23A 118.3 . . ? N4 C24 C6 112.0(3) . . ? N4 C24 H24A 109.2 . . ? C6 C24 H24A 109.2 . . ? N4 C24 H24B 109.2 . . ? C6 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? N4 C25 C26 111.4(3) . . ? N4 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? N4 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? N5 C26 C27 121.5(4) . . ? N5 C26 C25 116.1(4) . . ? C27 C26 C25 122.4(4) . . ? C28 C27 C26 118.9(4) . . ? C28 C27 H27A 120.6 . . ? C26 C27 H27A 120.6 . . ? C27 C28 C29 119.6(5) . . ? C27 C28 H28A 120.2 . . ? C29 C28 H28A 120.2 . . ? C30 C29 C28 118.6(4) . . ? C30 C29 H29A 120.7 . . ? C28 C29 H29A 120.7 . . ? N5 C30 C29 122.7(4) . . ? N5 C30 H30A 118.6 . . ? C29 C30 H30A 118.6 . . ? N4 C31 C32 110.7(3) . . ? N4 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? N4 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? N6 C32 C33 121.9(4) . . ? N6 C32 C31 115.9(4) . . ? C33 C32 C31 122.1(4) . . ? C34 C33 C32 118.4(5) . . ? C34 C33 H33A 120.8 . . ? C32 C33 H33A 120.8 . . ? C35 C34 C33 119.6(5) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C34 C35 C36 119.0(5) . . ? C34 C35 H35A 120.5 . . ? C36 C35 H35A 120.5 . . ? N6 C36 C35 121.6(5) . . ? N6 C36 H36A 119.2 . . ? C35 C36 H36A 119.2 . . ? O3 C37 O2 131.5(4) . . ? O3 C37 C38 114.1(4) . . ? O2 C37 C38 114.4(4) . . ? F1 C38 F2 107.5(5) . . ? F1 C38 F3 102.9(6) . . ? F2 C38 F3 108.8(6) . . ? F1 C38 C37 114.7(5) . . ? F2 C38 C37 112.9(5) . . ? F3 C38 C37 109.3(5) . . ? O4 C39 O5 130.2(4) . . ? O4 C39 C40 115.7(4) . . ? O5 C39 C40 114.1(4) . . ? F6 C40 F5 106.7(4) . . ? F6 C40 F4 105.6(4) . . ? F5 C40 F4 105.1(4) . . ? F6 C40 C39 112.7(4) . . ? F5 C40 C39 113.1(4) . . ? F4 C40 C39 112.9(4) . . ? O1B Cl1 O1A 109.5(2) . . ? O1B Cl1 O1D 109.9(3) . . ? O1A Cl1 O1D 109.5(3) . . ? O1B Cl1 O1C 109.0(2) . . ? O1A Cl1 O1C 109.6(2) . . ? O1D Cl1 O1C 109.4(3) . . ? C1S O1S H1S 110.2 . . ? O1S C1S H1S1 110.2 . . ? O1S C1S H1S2 109.7 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 108.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Co2 O1 C1 -137.8(3) . . . . ? N6 Co2 O1 C1 89.1(5) . . . . ? N5 Co2 O1 C1 -41.5(3) . . . . ? N4 Co2 O1 C1 38.5(3) . . . . ? O3 Co2 O1 C1 132.1(3) . . . . ? O5 Co2 O1 Co1 41.93(17) . . . . ? N6 Co2 O1 Co1 -91.2(4) . . . . ? N5 Co2 O1 Co1 138.28(16) . . . . ? N4 Co2 O1 Co1 -141.71(16) . . . . ? O3 Co2 O1 Co1 -48.16(16) . . . . ? O2 Co1 O1 C1 -135.1(3) . . . . ? N3 Co1 O1 C1 73.9(5) . . . . ? N2 Co1 O1 C1 -42.9(3) . . . . ? O4 Co1 O1 C1 136.7(3) . . . . ? N1 Co1 O1 C1 36.7(3) . . . . ? O2 Co1 O1 Co2 45.12(17) . . . . ? N3 Co1 O1 Co2 -105.9(4) . . . . ? N2 Co1 O1 Co2 137.33(17) . . . . ? O4 Co1 O1 Co2 -43.07(16) . . . . ? N1 Co1 O1 Co2 -143.04(16) . . . . ? O1 Co1 O2 C37 -10.4(4) . . . . ? N3 Co1 O2 C37 162.1(4) . . . . ? N2 Co1 O2 C37 -99.3(4) . . . . ? O4 Co1 O2 C37 80.1(4) . . . . ? N1 Co1 O2 C37 -143.2(6) . . . . ? O1 Co2 O3 C37 31.5(5) . . . . ? O5 Co2 O3 C37 -66.1(5) . . . . ? N6 Co2 O3 C37 -160.5(5) . . . . ? N4 Co2 O3 C37 122.6(5) . . . . ? O1 Co1 O4 C39 34.7(4) . . . . ? O2 Co1 O4 C39 -62.8(4) . . . . ? N3 Co1 O4 C39 -159.2(4) . . . . ? N1 Co1 O4 C39 124.9(4) . . . . ? O1 Co2 O5 C39 -23.5(4) . . . . ? N6 Co2 O5 C39 143.7(4) . . . . ? N5 Co2 O5 C39 -113.4(4) . . . . ? O3 Co2 O5 C39 63.9(4) . . . . ? O1 Co1 N1 C18 137.6(3) . . . . ? O2 Co1 N1 C18 -89.1(7) . . . . ? N3 Co1 N1 C18 -32.8(3) . . . . ? N2 Co1 N1 C18 -133.9(3) . . . . ? O4 Co1 N1 C18 46.8(3) . . . . ? O1 Co1 N1 C12 -103.8(3) . . . . ? O2 Co1 N1 C12 29.4(8) . . . . ? N3 Co1 N1 C12 85.7(3) . . . . ? N2 Co1 N1 C12 -15.3(3) . . . . ? O4 Co1 N1 C12 165.3(2) . . . . ? O1 Co1 N1 C11 18.0(3) . . . . ? O2 Co1 N1 C11 151.3(6) . . . . ? N3 Co1 N1 C11 -152.4(3) . . . . ? N2 Co1 N1 C11 106.5(3) . . . . ? O4 Co1 N1 C11 -72.8(3) . . . . ? O1 Co1 N2 C17 -73.5(4) . . . . ? O2 Co1 N2 C17 24.0(4) . . . . ? N3 Co1 N2 C17 120.5(4) . . . . ? N1 Co1 N2 C17 -163.8(4) . . . . ? O1 Co1 N2 C13 86.4(3) . . . . ? O2 Co1 N2 C13 -176.2(3) . . . . ? N3 Co1 N2 C13 -79.6(3) . . . . ? N1 Co1 N2 C13 -4.0(3) . . . . ? O1 Co1 N3 C23 159.1(4) . . . . ? O2 Co1 N3 C23 8.1(4) . . . . ? N2 Co1 N3 C23 -85.3(4) . . . . ? O4 Co1 N3 C23 95.3(4) . . . . ? N1 Co1 N3 C23 -162.6(4) . . . . ? O1 Co1 N3 C19 -21.4(6) . . . . ? O2 Co1 N3 C19 -172.4(3) . . . . ? N2 Co1 N3 C19 94.2(3) . . . . ? O4 Co1 N3 C19 -85.2(3) . . . . ? N1 Co1 N3 C19 16.9(3) . . . . ? O1 Co2 N4 C31 135.3(3) . . . . ? N6 Co2 N4 C31 -31.0(3) . . . . ? N5 Co2 N4 C31 -136.0(3) . . . . ? O3 Co2 N4 C31 47.7(3) . . . . ? O1 Co2 N4 C25 -106.8(3) . . . . ? N6 Co2 N4 C25 87.0(3) . . . . ? N5 Co2 N4 C25 -18.0(3) . . . . ? O3 Co2 N4 C25 165.7(3) . . . . ? O1 Co2 N4 C24 15.2(3) . . . . ? N6 Co2 N4 C24 -151.0(3) . . . . ? N5 Co2 N4 C24 104.0(3) . . . . ? O3 Co2 N4 C24 -72.3(3) . . . . ? O1 Co2 N5 C26 90.9(3) . . . . ? O5 Co2 N5 C26 -171.6(3) . . . . ? N6 Co2 N5 C26 -75.6(3) . . . . ? N4 Co2 N5 C26 -0.6(3) . . . . ? O1 Co2 N5 C30 -68.1(3) . . . . ? O5 Co2 N5 C30 29.4(3) . . . . ? N6 Co2 N5 C30 125.4(3) . . . . ? N4 Co2 N5 C30 -159.6(3) . . . . ? O1 Co2 N6 C32 -33.5(6) . . . . ? O5 Co2 N6 C32 -167.0(3) . . . . ? N5 Co2 N6 C32 95.5(3) . . . . ? N4 Co2 N6 C32 18.7(3) . . . . ? O3 Co2 N6 C32 -77.3(3) . . . . ? O1 Co2 N6 C36 140.2(4) . . . . ? O5 Co2 N6 C36 6.8(4) . . . . ? N5 Co2 N6 C36 -90.8(4) . . . . ? N4 Co2 N6 C36 -167.6(4) . . . . ? O3 Co2 N6 C36 96.4(4) . . . . ? Co2 O1 C1 C6 -52.4(4) . . . . ? Co1 O1 C1 C6 127.9(3) . . . . ? Co2 O1 C1 C2 128.4(3) . . . . ? Co1 O1 C1 C2 -51.3(4) . . . . ? O1 C1 C2 C3 177.9(4) . . . . ? C6 C1 C2 C3 -1.3(6) . . . . ? O1 C1 C2 C11 -0.3(6) . . . . ? C6 C1 C2 C11 -179.5(4) . . . . ? C1 C2 C3 C4 -0.1(6) . . . . ? C11 C2 C3 C4 178.0(4) . . . . ? C2 C3 C4 C5 1.4(7) . . . . ? C2 C3 C4 C7 -178.2(4) . . . . ? C3 C4 C5 C6 -1.2(7) . . . . ? C7 C4 C5 C6 178.3(4) . . . . ? C4 C5 C6 C1 -0.1(6) . . . . ? C4 C5 C6 C24 -178.5(4) . . . . ? O1 C1 C6 C5 -177.8(4) . . . . ? C2 C1 C6 C5 1.4(6) . . . . ? O1 C1 C6 C24 0.6(6) . . . . ? C2 C1 C6 C24 179.8(4) . . . . ? C3 C4 C7 C9 6.5(7) . . . . ? C5 C4 C7 C9 -173.1(5) . . . . ? C3 C4 C7 C10 -116.1(6) . . . . ? C5 C4 C7 C10 64.4(6) . . . . ? C3 C4 C7 C8 125.0(5) . . . . ? C5 C4 C7 C8 -54.5(6) . . . . ? C18 N1 C11 C2 -179.2(3) . . . . ? C12 N1 C11 C2 56.3(4) . . . . ? Co1 N1 C11 C2 -63.5(4) . . . . ? C3 C2 C11 N1 -114.0(4) . . . . ? C1 C2 C11 N1 64.1(5) . . . . ? C18 N1 C12 C13 145.9(4) . . . . ? C11 N1 C12 C13 -89.6(4) . . . . ? Co1 N1 C12 C13 31.4(4) . . . . ? C17 N2 C13 C14 1.0(6) . . . . ? Co1 N2 C13 C14 -160.4(3) . . . . ? C17 N2 C13 C12 -175.4(4) . . . . ? Co1 N2 C13 C12 23.2(4) . . . . ? N1 C12 C13 N2 -37.6(5) . . . . ? N1 C12 C13 C14 146.0(4) . . . . ? N2 C13 C14 C15 -2.2(7) . . . . ? C12 C13 C14 C15 173.9(4) . . . . ? C13 C14 C15 C16 1.9(7) . . . . ? C14 C15 C16 C17 -0.5(8) . . . . ? C13 N2 C17 C16 0.5(7) . . . . ? Co1 N2 C17 C16 159.6(4) . . . . ? C15 C16 C17 N2 -0.7(8) . . . . ? C12 N1 C18 C19 -71.9(4) . . . . ? C11 N1 C18 C19 163.5(3) . . . . ? Co1 N1 C18 C19 44.6(4) . . . . ? C23 N3 C19 C20 3.0(6) . . . . ? Co1 N3 C19 C20 -176.6(3) . . . . ? C23 N3 C19 C18 -176.8(4) . . . . ? Co1 N3 C19 C18 3.7(5) . . . . ? N1 C18 C19 N3 -33.9(5) . . . . ? N1 C18 C19 C20 146.4(4) . . . . ? N3 C19 C20 C21 -2.5(7) . . . . ? C18 C19 C20 C21 177.2(4) . . . . ? C19 C20 C21 C22 0.5(7) . . . . ? C20 C21 C22 C23 1.0(7) . . . . ? C19 N3 C23 C22 -1.4(7) . . . . ? Co1 N3 C23 C22 178.1(3) . . . . ? C21 C22 C23 N3 -0.6(7) . . . . ? C31 N4 C24 C6 -178.0(3) . . . . ? C25 N4 C24 C6 59.2(4) . . . . ? Co2 N4 C24 C6 -60.4(4) . . . . ? C5 C6 C24 N4 -119.0(4) . . . . ? C1 C6 C24 N4 62.6(5) . . . . ? C31 N4 C25 C26 148.6(4) . . . . ? C24 N4 C25 C26 -88.3(4) . . . . ? Co2 N4 C25 C26 33.0(4) . . . . ? C30 N5 C26 C27 -1.3(6) . . . . ? Co2 N5 C26 C27 -161.4(3) . . . . ? C30 N5 C26 C25 -179.7(4) . . . . ? Co2 N5 C26 C25 20.1(4) . . . . ? N4 C25 C26 N5 -36.7(5) . . . . ? N4 C25 C26 C27 144.9(4) . . . . ? N5 C26 C27 C28 1.0(7) . . . . ? C25 C26 C27 C28 179.4(4) . . . . ? C26 C27 C28 C29 -0.7(7) . . . . ? C27 C28 C29 C30 0.6(7) . . . . ? C26 N5 C30 C29 1.2(6) . . . . ? Co2 N5 C30 C29 159.3(3) . . . . ? C28 C29 C30 N5 -0.9(7) . . . . ? C25 N4 C31 C32 -77.1(4) . . . . ? C24 N4 C31 C32 159.2(4) . . . . ? Co2 N4 C31 C32 39.2(4) . . . . ? C36 N6 C32 C33 0.4(7) . . . . ? Co2 N6 C32 C33 174.5(4) . . . . ? C36 N6 C32 C31 -175.6(4) . . . . ? Co2 N6 C32 C31 -1.5(5) . . . . ? N4 C31 C32 N6 -26.5(5) . . . . ? N4 C31 C32 C33 157.5(4) . . . . ? N6 C32 C33 C34 1.2(8) . . . . ? C31 C32 C33 C34 176.9(5) . . . . ? C32 C33 C34 C35 -2.2(10) . . . . ? C33 C34 C35 C36 1.7(11) . . . . ? C32 N6 C36 C35 -0.9(8) . . . . ? Co2 N6 C36 C35 -174.4(5) . . . . ? C34 C35 C36 N6 -0.1(10) . . . . ? Co2 O3 C37 O2 -3.4(8) . . . . ? Co2 O3 C37 C38 179.0(4) . . . . ? Co1 O2 C37 O3 -10.0(7) . . . . ? Co1 O2 C37 C38 167.5(3) . . . . ? O3 C37 C38 F1 -152.9(5) . . . . ? O2 C37 C38 F1 29.1(7) . . . . ? O3 C37 C38 F2 -29.3(7) . . . . ? O2 C37 C38 F2 152.8(5) . . . . ? O3 C37 C38 F3 92.1(6) . . . . ? O2 C37 C38 F3 -85.9(6) . . . . ? Co1 O4 C39 O5 -23.8(7) . . . . ? Co1 O4 C39 C40 156.2(3) . . . . ? Co2 O5 C39 O4 16.2(7) . . . . ? Co2 O5 C39 C40 -163.9(3) . . . . ? O4 C39 C40 F6 88.3(5) . . . . ? O5 C39 C40 F6 -91.6(5) . . . . ? O4 C39 C40 F5 -32.9(5) . . . . ? O5 C39 C40 F5 147.2(4) . . . . ? O4 C39 C40 F4 -152.1(4) . . . . ? O5 C39 C40 F4 28.0(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1S H1S O1C 0.85 1.99 2.840(7) 179.7 1_455 #===END