# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ; Structural Diversity in Manganese, Iron and Cobalt Complexes of the Ditopic 1,2-Bis(2,2'-bipyridyl-6-yl)ethyne Ligand and Observation of Epoxidation and Catalase Activity of Manganese Compounds ; _publ_contact_author_name 'Ronny Neumann' _publ_contact_author_email RONNY.NEUMANN@WEIZMANN.AC.IL loop_ _publ_author_name R.Neumann E.Balaraman Y.Diskin-Posner G.Leitus L.Shimon ; M.Vedichi ; # Attachment 'Cmpd_1-756141R2.cif' data_n167an _database_code_depnum_ccdc_archive 'CCDC 756141' #TrackingRef 'Cmpd_1-756141R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H23 Mn2 N4 O6, F6 P, O' _chemical_formula_sum 'C28 H23 F6 Mn2 N4 O7 P' _chemical_formula_weight 782.35 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 8.5423(1) _cell_length_b 12.9101(2) _cell_length_c 27.6759(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.0314(5) _cell_angle_gamma 90.00 _cell_volume 3051.66(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10533 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 31.51 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.970 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7595 _exptl_absorpt_correction_T_max 0.8296 _exptl_absorpt_process_details 'SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10533 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 29.13 _reflns_number_total 8160 _reflns_number_gt 5654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect package (Bruker Nonius)' _computing_cell_refinement HKL _computing_data_reduction HKL _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0824P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8160 _refine_ls_number_parameters 500 _refine_ls_number_restraints 145 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1268 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.98321(4) -0.07109(3) 0.130320(13) 0.02010(11) Uani 1 1 d . . . Mn2 Mn 0.78829(4) 0.00516(3) 0.229435(13) 0.01978(11) Uani 1 1 d . . . N1 N 1.1079(2) -0.08535(16) 0.06254(7) 0.0207(4) Uani 1 1 d . . . C1 C 1.1580(3) -0.0031(2) 0.03715(9) 0.0227(5) Uani 1 1 d . . . H1 H 1.1455 0.0643 0.0504 0.027 Uiso 1 1 calc R . . C2 C 1.2266(3) -0.0130(2) -0.00737(10) 0.0280(6) Uani 1 1 d . . . H2 H 1.2629 0.0461 -0.0243 0.034 Uiso 1 1 calc R . . C3 C 1.2408(3) -0.1105(2) -0.02652(10) 0.0329(7) Uani 1 1 d . . . H3 H 1.2850 -0.1191 -0.0575 0.040 Uiso 1 1 calc R . . C4 C 1.1913(3) -0.1966(2) -0.00099(10) 0.0316(6) Uani 1 1 d . . . H4 H 1.2012 -0.2643 -0.0140 0.038 Uiso 1 1 calc R . . C5 C 1.1269(3) -0.1812(2) 0.04415(9) 0.0227(5) Uani 1 1 d . . . C6 C 1.0744(3) -0.2690(2) 0.07499(9) 0.0220(5) Uani 1 1 d . . . C7 C 1.1077(3) -0.3724(2) 0.06456(10) 0.0282(6) Uani 1 1 d . . . H7 H 1.1642 -0.3901 0.0365 0.034 Uiso 1 1 calc R . . C8 C 1.0570(3) -0.4486(2) 0.09579(10) 0.0296(6) Uani 1 1 d . . . H8 H 1.0789 -0.5194 0.0893 0.036 Uiso 1 1 calc R . . C9 C 0.9749(3) -0.4219(2) 0.13628(10) 0.0268(6) Uani 1 1 d . . . H9 H 0.9383 -0.4734 0.1578 0.032 Uiso 1 1 calc R . . C10 C 0.9470(3) -0.31696(19) 0.14485(9) 0.0219(5) Uani 1 1 d . . . N2 N 0.9960(2) -0.24223(16) 0.11474(7) 0.0208(4) Uani 1 1 d . . . C11 C 0.8637(3) -0.28357(19) 0.18731(9) 0.0230(5) Uani 1 1 d . . . C12 C 0.7942(3) -0.2571(2) 0.22238(9) 0.0234(5) Uani 1 1 d . . . C13 C 0.7103(3) -0.2301(2) 0.26514(9) 0.0235(5) Uani 1 1 d . . . N3 N 0.6973(2) -0.12871(16) 0.27572(7) 0.0195(4) Uani 1 1 d . . . C14 C 0.6454(3) -0.3068(2) 0.29400(10) 0.0315(6) Uani 1 1 d . . . H14 H 0.6555 -0.3779 0.2858 0.038 Uiso 1 1 calc R . . C15 C 0.5662(4) -0.2770(2) 0.33485(11) 0.0356(7) Uani 1 1 d . . . H15 H 0.5199 -0.3278 0.3549 0.043 Uiso 1 1 calc R . . C16 C 0.5544(3) -0.1734(2) 0.34637(10) 0.0288(6) Uani 1 1 d . . . H16 H 0.5018 -0.1523 0.3747 0.035 Uiso 1 1 calc R . . C17 C 0.6203(3) -0.10059(19) 0.31610(9) 0.0204(5) Uani 1 1 d . . . C18 C 0.6090(3) 0.01328(18) 0.32497(9) 0.0202(5) Uani 1 1 d . . . C19 C 0.5284(3) 0.0548(2) 0.36359(10) 0.0262(6) Uani 1 1 d . . . H19 H 0.4777 0.0109 0.3860 0.031 Uiso 1 1 calc R . . C20 C 0.5233(3) 0.1622(2) 0.36881(10) 0.0315(6) Uani 1 1 d . . . H20 H 0.4665 0.1924 0.3944 0.038 Uiso 1 1 calc R . . C21 C 0.6006(3) 0.2238(2) 0.33691(11) 0.0332(6) Uani 1 1 d . . . H21 H 0.6013 0.2970 0.3406 0.040 Uiso 1 1 calc R . . C22 C 0.6783(3) 0.1768(2) 0.29899(10) 0.0286(6) Uani 1 1 d . . . H22 H 0.7316 0.2194 0.2766 0.034 Uiso 1 1 calc R . . N4 N 0.6810(2) 0.07404(15) 0.29278(8) 0.0210(4) Uani 1 1 d . . . C23 C 0.9685(4) 0.2710(2) 0.14454(11) 0.0333(6) Uani 1 1 d . . . H23A H 1.0589 0.2729 0.1232 0.050 Uiso 1 1 calc R . . H23B H 0.9903 0.3135 0.1732 0.050 Uiso 1 1 calc R . . H23C H 0.8762 0.2982 0.1273 0.050 Uiso 1 1 calc R . . C24 C 0.9381(3) 0.1610(2) 0.15976(10) 0.0249(5) Uani 1 1 d . . . O1 O 0.8545(2) 0.14612(14) 0.19624(7) 0.0319(5) Uani 1 1 d . . . O2 O 0.9950(2) 0.08995(14) 0.13449(7) 0.0333(5) Uani 1 1 d . . . C25 C 0.6172(3) -0.04393(19) 0.13812(9) 0.0216(5) Uani 1 1 d . . . C26 C 0.4758(3) -0.0382(2) 0.10495(10) 0.0276(6) Uani 1 1 d . . . H26A H 0.3809 -0.0339 0.1242 0.041 Uiso 1 1 calc R . . H26B H 0.4712 -0.1003 0.0846 0.041 Uiso 1 1 calc R . . H26C H 0.4833 0.0234 0.0844 0.041 Uiso 1 1 calc R . . O3 O 0.6014(2) -0.01975(15) 0.18157(7) 0.0295(4) Uani 1 1 d . . . O4 O 0.7437(2) -0.07112(16) 0.11971(7) 0.0338(5) Uani 1 1 d . . . C27 C 1.1339(3) -0.06756(18) 0.23108(9) 0.0200(5) Uani 1 1 d . . . C28 C 1.2802(3) -0.0759(2) 0.26184(10) 0.0270(6) Uani 1 1 d . . . H28A H 1.2894 -0.0148 0.2827 0.041 Uiso 1 1 calc R . . H28B H 1.3716 -0.0799 0.2410 0.041 Uiso 1 1 calc R . . H28C H 1.2751 -0.1384 0.2819 0.041 Uiso 1 1 calc R . . O5 O 1.0113(2) -0.03791(15) 0.25124(7) 0.0277(4) Uani 1 1 d . . . O6 O 1.1422(2) -0.09229(15) 0.18712(7) 0.0275(4) Uani 1 1 d . . . P1A P 0.6849(9) -0.3202(6) -0.0086(3) 0.0411(14) Uani 0.469(9) 1 d PD A 1 F1A F 0.8537(10) -0.2960(9) -0.0282(2) 0.106(3) Uani 0.469(9) 1 d PDU A 1 F2A F 0.5142(8) -0.3498(7) 0.01237(18) 0.063(2) Uani 0.469(9) 1 d PDU A 1 F3A F 0.7682(12) -0.4047(8) 0.0252(3) 0.111(4) Uani 0.469(9) 1 d PDU A 1 F4A F 0.6618(11) -0.4048(7) -0.0496(3) 0.053(2) Uani 0.469(9) 1 d PDU A 1 F5A F 0.7163(11) -0.2383(5) 0.03313(19) 0.073(2) Uani 0.469(9) 1 d PDU A 1 F6A F 0.6213(13) -0.2317(7) -0.0434(3) 0.088(3) Uani 0.469(9) 1 d PDU A 1 P1B P 0.6591(8) -0.3024(5) -0.0097(3) 0.0398(11) Uani 0.531(9) 1 d PD A 2 F1B F 0.8121(7) -0.2432(4) -0.0183(3) 0.083(2) Uani 0.531(9) 1 d PDU A 2 F5B F 0.6030(10) -0.2191(3) 0.02832(16) 0.066(2) Uani 0.531(9) 1 d PDU A 2 F3B F 0.7369(9) -0.3697(5) 0.0324(2) 0.074(2) Uani 0.531(9) 1 d PDU A 2 F4B F 0.7013(12) -0.3874(7) -0.0476(3) 0.097(4) Uani 0.531(9) 1 d PDU A 2 F6B F 0.5632(9) -0.2404(6) -0.0488(2) 0.070(2) Uani 0.531(9) 1 d PDU A 2 F2B F 0.5050(11) -0.3646(7) -0.0002(4) 0.129(4) Uani 0.531(9) 1 d PDU A 2 O7 O 0.2877(4) -0.4182(3) -0.06029(13) 0.0817(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0212(2) 0.0197(2) 0.01952(19) -0.00086(15) 0.00426(15) 0.00147(15) Mn2 0.0191(2) 0.0200(2) 0.02035(19) 0.00025(15) 0.00509(15) 0.00038(14) N1 0.0190(10) 0.0242(11) 0.0191(10) 0.0018(8) 0.0019(8) 0.0010(8) C1 0.0206(12) 0.0249(13) 0.0227(12) 0.0006(10) -0.0005(10) 0.0018(10) C2 0.0251(14) 0.0351(16) 0.0241(13) 0.0069(11) 0.0028(11) -0.0014(11) C3 0.0341(16) 0.0407(17) 0.0245(13) -0.0013(12) 0.0128(12) -0.0016(13) C4 0.0336(15) 0.0348(16) 0.0268(14) -0.0056(12) 0.0093(12) -0.0016(12) C5 0.0207(12) 0.0257(13) 0.0220(12) -0.0007(10) 0.0038(10) 0.0002(10) C6 0.0235(12) 0.0235(13) 0.0192(11) -0.0026(10) 0.0025(10) -0.0004(10) C7 0.0305(14) 0.0267(14) 0.0278(13) -0.0041(11) 0.0102(11) 0.0028(11) C8 0.0348(16) 0.0185(13) 0.0357(15) -0.0026(11) 0.0069(12) 0.0046(11) C9 0.0302(14) 0.0229(13) 0.0275(13) 0.0010(11) 0.0053(11) -0.0005(11) C10 0.0226(12) 0.0204(12) 0.0229(12) 0.0016(10) 0.0027(10) 0.0002(10) N2 0.0222(11) 0.0203(11) 0.0199(10) -0.0023(8) 0.0037(8) 0.0015(8) C11 0.0279(13) 0.0157(11) 0.0255(13) 0.0019(10) 0.0034(11) -0.0012(10) C12 0.0270(13) 0.0197(13) 0.0237(12) 0.0017(10) 0.0024(11) -0.0018(10) C13 0.0289(14) 0.0193(12) 0.0222(12) 0.0008(10) 0.0022(10) 0.0013(10) N3 0.0197(10) 0.0187(10) 0.0201(10) 0.0007(8) 0.0029(8) 0.0007(8) C14 0.0425(17) 0.0195(13) 0.0327(14) -0.0010(11) 0.0104(13) -0.0048(12) C15 0.0505(19) 0.0266(14) 0.0302(14) 0.0036(12) 0.0156(14) -0.0039(13) C16 0.0354(15) 0.0280(14) 0.0234(13) -0.0012(11) 0.0084(12) -0.0022(12) C17 0.0212(12) 0.0225(12) 0.0176(11) 0.0005(10) 0.0007(9) 0.0000(10) C18 0.0190(12) 0.0209(12) 0.0206(11) 0.0007(10) 0.0017(10) -0.0009(10) C19 0.0253(14) 0.0268(14) 0.0269(13) -0.0015(11) 0.0076(11) -0.0031(11) C20 0.0326(15) 0.0309(15) 0.0311(14) -0.0102(12) 0.0090(12) 0.0004(12) C21 0.0371(16) 0.0226(13) 0.0400(16) -0.0071(12) 0.0069(13) -0.0004(12) C22 0.0322(15) 0.0228(13) 0.0311(14) -0.0022(11) 0.0097(12) -0.0025(11) N4 0.0200(10) 0.0197(10) 0.0234(10) -0.0009(9) 0.0045(9) 0.0016(8) C23 0.0413(17) 0.0221(14) 0.0368(15) 0.0049(12) 0.0114(13) 0.0006(12) C24 0.0259(13) 0.0214(13) 0.0275(13) 0.0036(11) -0.0011(11) -0.0025(10) O1 0.0377(11) 0.0240(10) 0.0344(11) 0.0058(8) 0.0126(9) -0.0014(8) O2 0.0455(13) 0.0186(9) 0.0360(11) -0.0023(8) 0.0108(10) 0.0012(8) C25 0.0209(12) 0.0187(12) 0.0254(12) 0.0041(10) 0.0030(10) -0.0023(10) C26 0.0247(14) 0.0312(14) 0.0268(13) 0.0016(12) -0.0003(11) -0.0032(11) O3 0.0294(10) 0.0362(11) 0.0230(9) 0.0017(8) 0.0016(8) -0.0016(8) O4 0.0233(10) 0.0420(12) 0.0364(11) -0.0019(9) 0.0046(8) 0.0056(9) C27 0.0209(12) 0.0167(11) 0.0225(12) 0.0015(10) 0.0029(10) -0.0004(9) C28 0.0221(13) 0.0334(15) 0.0255(13) -0.0008(12) -0.0004(10) 0.0005(11) O5 0.0207(9) 0.0337(10) 0.0288(10) -0.0020(8) 0.0027(8) 0.0031(8) O6 0.0259(10) 0.0325(10) 0.0242(9) -0.0044(8) 0.0005(8) 0.0044(8) P1A 0.053(3) 0.040(3) 0.0294(15) -0.0021(17) -0.0022(15) -0.010(2) F1A 0.085(5) 0.165(8) 0.068(4) -0.024(5) 0.028(3) -0.051(5) F2A 0.042(3) 0.124(6) 0.021(2) -0.017(3) 0.0061(18) 0.000(3) F3A 0.122(6) 0.094(6) 0.114(6) 0.000(5) -0.067(5) 0.041(5) F4A 0.057(4) 0.048(3) 0.052(4) -0.012(3) -0.003(3) 0.001(3) F5A 0.099(5) 0.062(4) 0.059(3) -0.021(3) -0.014(3) -0.015(4) F6A 0.120(7) 0.062(4) 0.081(5) -0.003(3) -0.051(4) 0.008(4) P1B 0.054(2) 0.0280(16) 0.0378(17) -0.0043(12) 0.0059(15) -0.0011(14) F1B 0.056(3) 0.041(3) 0.152(6) 0.021(3) 0.011(3) -0.008(2) F5B 0.113(5) 0.043(2) 0.042(2) -0.0022(19) 0.026(3) 0.016(3) F3B 0.085(4) 0.067(4) 0.071(3) 0.030(3) 0.004(3) 0.023(3) F4B 0.110(7) 0.091(6) 0.088(5) -0.049(4) -0.009(4) 0.062(5) F6B 0.085(4) 0.087(4) 0.038(3) -0.013(3) -0.010(3) 0.056(4) F2B 0.089(5) 0.065(4) 0.234(9) -0.036(5) 0.029(6) -0.033(4) O7 0.074(2) 0.080(2) 0.091(2) -0.0062(19) 0.0085(18) 0.0089(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 Mn1 O4 2.061(2) . ? Mn1 O6 2.0767(19) . ? Mn1 O2 2.0846(19) . ? Mn1 N1 2.182(2) . ? Mn1 N2 2.254(2) . ? Mn2 O5 2.0645(18) . ? Mn2 O3 2.0813(19) . ? Mn2 O1 2.1199(19) . ? Mn2 N4 2.182(2) . ? Mn2 N3 2.295(2) . ? N1 C1 1.348(3) . ? N1 C5 1.349(3) . ? C1 C2 1.380(4) . ? C1 H1 0.9500 . ? C2 C3 1.372(4) . ? C2 H2 0.9500 . ? C3 C4 1.388(4) . ? C3 H3 0.9500 . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.493(4) . ? C6 N2 1.344(3) . ? C6 C7 1.396(4) . ? C7 C8 1.384(4) . ? C7 H7 0.9500 . ? C8 C9 1.377(4) . ? C8 H8 0.9500 . ? C9 C10 1.396(4) . ? C9 H9 0.9500 . ? C10 N2 1.346(3) . ? C10 C11 1.450(3) . ? C11 C12 1.196(3) . ? C12 C13 1.437(3) . ? C13 N3 1.346(3) . ? C13 C14 1.393(4) . ? N3 C17 1.357(3) . ? C14 C15 1.383(4) . ? C14 H14 0.9500 . ? C15 C16 1.379(4) . ? C15 H15 0.9500 . ? C16 C17 1.386(4) . ? C16 H16 0.9500 . ? C17 C18 1.494(3) . ? C18 N4 1.344(3) . ? C18 C19 1.390(4) . ? C19 C20 1.394(4) . ? C19 H19 0.9500 . ? C20 C21 1.367(4) . ? C20 H20 0.9500 . ? C21 C22 1.391(4) . ? C21 H21 0.9500 . ? C22 N4 1.338(3) . ? C22 H22 0.9500 . ? C23 C24 1.506(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 O2 1.256(3) . ? C24 O1 1.262(3) . ? C25 O3 1.252(3) . ? C25 O4 1.253(3) . ? C25 C26 1.505(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 O5 1.255(3) . ? C27 O6 1.261(3) . ? C27 C28 1.504(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? P1A F1A 1.581(8) . ? P1A F6A 1.584(9) . ? P1A F4A 1.584(9) . ? P1A F5A 1.586(8) . ? P1A F3A 1.596(9) . ? P1A F2A 1.624(8) . ? P1B F1B 1.537(8) . ? P1B F6B 1.565(8) . ? P1B F4B 1.565(8) . ? P1B F2B 1.567(9) . ? P1B F5B 1.586(8) . ? P1B F3B 1.589(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Mn1 O6 137.85(8) . . ? O4 Mn1 O2 93.15(8) . . ? O6 Mn1 O2 93.39(8) . . ? O4 Mn1 N1 112.10(8) . . ? O6 Mn1 N1 108.49(7) . . ? O2 Mn1 N1 96.19(8) . . ? O4 Mn1 N2 91.36(8) . . ? O6 Mn1 N2 89.00(8) . . ? O2 Mn1 N2 170.30(7) . . ? N1 Mn1 N2 74.15(8) . . ? O5 Mn2 O3 146.91(8) . . ? O5 Mn2 O1 96.08(8) . . ? O3 Mn2 O1 93.69(8) . . ? O5 Mn2 N4 105.89(8) . . ? O3 Mn2 N4 104.23(8) . . ? O1 Mn2 N4 96.75(8) . . ? O5 Mn2 N3 87.36(7) . . ? O3 Mn2 N3 88.59(7) . . ? O1 Mn2 N3 169.71(7) . . ? N4 Mn2 N3 72.97(7) . . ? C1 N1 C5 119.0(2) . . ? C1 N1 Mn1 123.11(17) . . ? C5 N1 Mn1 117.75(16) . . ? N1 C1 C2 122.4(2) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.2(3) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 C4 120.5(2) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 118.2(3) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? N1 C5 C4 121.5(2) . . ? N1 C5 C6 116.2(2) . . ? C4 C5 C6 122.3(2) . . ? N2 C6 C7 121.5(2) . . ? N2 C6 C5 115.6(2) . . ? C7 C6 C5 122.9(2) . . ? C8 C7 C6 118.9(2) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C9 C8 C7 119.9(2) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 118.2(2) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N2 C10 C9 122.3(2) . . ? N2 C10 C11 116.8(2) . . ? C9 C10 C11 120.9(2) . . ? C6 N2 C10 119.2(2) . . ? C6 N2 Mn1 115.81(16) . . ? C10 N2 Mn1 124.57(16) . . ? C12 C11 C10 179.3(3) . . ? C11 C12 C13 177.4(3) . . ? N3 C13 C14 122.1(2) . . ? N3 C13 C12 117.3(2) . . ? C14 C13 C12 120.6(2) . . ? C13 N3 C17 118.8(2) . . ? C13 N3 Mn2 125.51(16) . . ? C17 N3 Mn2 115.62(16) . . ? C15 C14 C13 118.5(3) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C16 C15 C14 119.8(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 119.1(2) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? N3 C17 C16 121.7(2) . . ? N3 C17 C18 115.6(2) . . ? C16 C17 C18 122.7(2) . . ? N4 C18 C19 121.6(2) . . ? N4 C18 C17 115.7(2) . . ? C19 C18 C17 122.7(2) . . ? C18 C19 C20 118.7(2) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? C21 C20 C19 119.7(2) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 118.4(3) . . ? C20 C21 H21 120.8 . . ? C22 C21 H21 120.8 . . ? N4 C22 C21 122.6(3) . . ? N4 C22 H22 118.7 . . ? C21 C22 H22 118.7 . . ? C22 N4 C18 119.0(2) . . ? C22 N4 Mn2 121.04(17) . . ? C18 N4 Mn2 119.90(16) . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O2 C24 O1 124.4(2) . . ? O2 C24 C23 117.5(2) . . ? O1 C24 C23 118.0(2) . . ? C24 O1 Mn2 129.52(18) . . ? C24 O2 Mn1 137.72(17) . . ? O3 C25 O4 124.7(2) . . ? O3 C25 C26 118.3(2) . . ? O4 C25 C26 117.0(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 O3 Mn2 123.72(18) . . ? C25 O4 Mn1 143.41(19) . . ? O5 C27 O6 124.6(2) . . ? O5 C27 C28 117.5(2) . . ? O6 C27 C28 117.9(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 O5 Mn2 136.47(17) . . ? C27 O6 Mn1 130.53(17) . . ? F1A P1A F6A 87.3(6) . . ? F1A P1A F4A 89.6(5) . . ? F6A P1A F4A 91.5(5) . . ? F1A P1A F5A 88.6(5) . . ? F6A P1A F5A 90.7(5) . . ? F4A P1A F5A 177.1(7) . . ? F1A P1A F3A 86.4(5) . . ? F6A P1A F3A 173.6(8) . . ? F4A P1A F3A 89.8(5) . . ? F5A P1A F3A 87.8(5) . . ? F1A P1A F2A 177.6(6) . . ? F6A P1A F2A 95.0(6) . . ? F4A P1A F2A 89.6(5) . . ? F5A P1A F2A 92.1(5) . . ? F3A P1A F2A 91.3(6) . . ? F1B P1B F6B 94.3(5) . . ? F1B P1B F4B 92.2(6) . . ? F6B P1B F4B 91.1(5) . . ? F1B P1B F2B 178.8(7) . . ? F6B P1B F2B 87.0(6) . . ? F4B P1B F2B 87.6(6) . . ? F1B P1B F5B 91.9(5) . . ? F6B P1B F5B 87.1(4) . . ? F4B P1B F5B 175.7(7) . . ? F2B P1B F5B 88.3(5) . . ? F1B P1B F3B 92.3(5) . . ? F6B P1B F3B 173.2(7) . . ? F4B P1B F3B 90.6(5) . . ? F2B P1B F3B 86.5(5) . . ? F5B P1B F3B 90.7(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 O4 Mn1 N1 C1 93.2(2) . . . . ? O6 Mn1 N1 C1 -98.4(2) . . . . ? O2 Mn1 N1 C1 -2.7(2) . . . . ? N2 Mn1 N1 C1 178.1(2) . . . . ? O4 Mn1 N1 C5 -82.74(19) . . . . ? O6 Mn1 N1 C5 85.62(19) . . . . ? O2 Mn1 N1 C5 -178.70(18) . . . . ? N2 Mn1 N1 C5 2.17(17) . . . . ? C5 N1 C1 C2 0.7(4) . . . . ? Mn1 N1 C1 C2 -175.19(19) . . . . ? N1 C1 C2 C3 1.3(4) . . . . ? C1 C2 C3 C4 -1.8(4) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C1 N1 C5 C4 -2.4(4) . . . . ? Mn1 N1 C5 C4 173.7(2) . . . . ? C1 N1 C5 C6 177.7(2) . . . . ? Mn1 N1 C5 C6 -6.1(3) . . . . ? C3 C4 C5 N1 2.0(4) . . . . ? C3 C4 C5 C6 -178.2(3) . . . . ? N1 C5 C6 N2 8.3(3) . . . . ? C4 C5 C6 N2 -171.6(2) . . . . ? N1 C5 C6 C7 -169.9(2) . . . . ? C4 C5 C6 C7 10.2(4) . . . . ? N2 C6 C7 C8 0.6(4) . . . . ? C5 C6 C7 C8 178.7(3) . . . . ? C6 C7 C8 C9 0.2(4) . . . . ? C7 C8 C9 C10 -0.8(4) . . . . ? C8 C9 C10 N2 0.7(4) . . . . ? C8 C9 C10 C11 -178.9(3) . . . . ? C7 C6 N2 C10 -0.7(4) . . . . ? C5 C6 N2 C10 -178.9(2) . . . . ? C7 C6 N2 Mn1 171.9(2) . . . . ? C5 C6 N2 Mn1 -6.3(3) . . . . ? C9 C10 N2 C6 0.0(4) . . . . ? C11 C10 N2 C6 179.7(2) . . . . ? C9 C10 N2 Mn1 -171.90(19) . . . . ? C11 C10 N2 Mn1 7.7(3) . . . . ? O4 Mn1 N2 C6 115.07(18) . . . . ? O6 Mn1 N2 C6 -107.09(18) . . . . ? N1 Mn1 N2 C6 2.46(17) . . . . ? O4 Mn1 N2 C10 -72.8(2) . . . . ? O6 Mn1 N2 C10 65.1(2) . . . . ? N1 Mn1 N2 C10 174.6(2) . . . . ? C14 C13 N3 C17 0.8(4) . . . . ? C12 C13 N3 C17 -179.3(2) . . . . ? C14 C13 N3 Mn2 -176.9(2) . . . . ? C12 C13 N3 Mn2 2.9(3) . . . . ? O5 Mn2 N3 C13 -72.0(2) . . . . ? O3 Mn2 N3 C13 75.1(2) . . . . ? O1 Mn2 N3 C13 178.1(4) . . . . ? N4 Mn2 N3 C13 -179.5(2) . . . . ? O5 Mn2 N3 C17 110.12(18) . . . . ? O3 Mn2 N3 C17 -102.73(18) . . . . ? O1 Mn2 N3 C17 0.3(5) . . . . ? N4 Mn2 N3 C17 2.62(17) . . . . ? N3 C13 C14 C15 -0.3(4) . . . . ? C12 C13 C14 C15 179.8(3) . . . . ? C13 C14 C15 C16 -0.7(5) . . . . ? C14 C15 C16 C17 1.1(5) . . . . ? C13 N3 C17 C16 -0.4(4) . . . . ? Mn2 N3 C17 C16 177.6(2) . . . . ? C13 N3 C17 C18 -179.2(2) . . . . ? Mn2 N3 C17 C18 -1.2(3) . . . . ? C15 C16 C17 N3 -0.6(4) . . . . ? C15 C16 C17 C18 178.1(3) . . . . ? N3 C17 C18 N4 -2.1(3) . . . . ? C16 C17 C18 N4 179.1(2) . . . . ? N3 C17 C18 C19 177.2(2) . . . . ? C16 C17 C18 C19 -1.6(4) . . . . ? N4 C18 C19 C20 -0.3(4) . . . . ? C17 C18 C19 C20 -179.6(2) . . . . ? C18 C19 C20 C21 -1.7(4) . . . . ? C19 C20 C21 C22 2.1(4) . . . . ? C20 C21 C22 N4 -0.4(5) . . . . ? C21 C22 N4 C18 -1.6(4) . . . . ? C21 C22 N4 Mn2 175.0(2) . . . . ? C19 C18 N4 C22 1.9(4) . . . . ? C17 C18 N4 C22 -178.7(2) . . . . ? C19 C18 N4 Mn2 -174.66(19) . . . . ? C17 C18 N4 Mn2 4.7(3) . . . . ? O5 Mn2 N4 C22 97.4(2) . . . . ? O3 Mn2 N4 C22 -96.5(2) . . . . ? O1 Mn2 N4 C22 -0.9(2) . . . . ? N3 Mn2 N4 C22 179.5(2) . . . . ? O5 Mn2 N4 C18 -86.08(19) . . . . ? O3 Mn2 N4 C18 80.0(2) . . . . ? O1 Mn2 N4 C18 175.60(19) . . . . ? N3 Mn2 N4 C18 -3.97(18) . . . . ? O2 C24 O1 Mn2 2.8(4) . . . . ? C23 C24 O1 Mn2 -178.94(19) . . . . ? O5 Mn2 O1 C24 64.9(2) . . . . ? O3 Mn2 O1 C24 -83.4(2) . . . . ? N4 Mn2 O1 C24 171.8(2) . . . . ? N3 Mn2 O1 C24 174.0(4) . . . . ? O1 C24 O2 Mn1 5.5(5) . . . . ? C23 C24 O2 Mn1 -172.8(2) . . . . ? O4 Mn1 O2 C24 58.2(3) . . . . ? O6 Mn1 O2 C24 -80.2(3) . . . . ? N1 Mn1 O2 C24 170.8(3) . . . . ? O4 C25 O3 Mn2 11.1(4) . . . . ? C26 C25 O3 Mn2 -167.51(17) . . . . ? O5 Mn2 O3 C25 -36.2(3) . . . . ? O1 Mn2 O3 C25 70.9(2) . . . . ? N4 Mn2 O3 C25 168.8(2) . . . . ? N3 Mn2 O3 C25 -119.2(2) . . . . ? O3 C25 O4 Mn1 -16.6(5) . . . . ? C26 C25 O4 Mn1 162.1(2) . . . . ? O6 Mn1 O4 C25 39.4(4) . . . . ? O2 Mn1 O4 C25 -59.2(3) . . . . ? N1 Mn1 O4 C25 -157.2(3) . . . . ? N2 Mn1 O4 C25 129.4(3) . . . . ? O6 C27 O5 Mn2 -10.1(4) . . . . ? C28 C27 O5 Mn2 171.07(18) . . . . ? O3 Mn2 O5 C27 36.8(3) . . . . ? O1 Mn2 O5 C27 -69.6(3) . . . . ? N4 Mn2 O5 C27 -168.4(2) . . . . ? N3 Mn2 O5 C27 120.1(3) . . . . ? O5 C27 O6 Mn1 12.1(4) . . . . ? C28 C27 O6 Mn1 -169.07(17) . . . . ? O4 Mn1 O6 C27 -35.2(3) . . . . ? O2 Mn1 O6 C27 63.3(2) . . . . ? N1 Mn1 O6 C27 161.0(2) . . . . ? N2 Mn1 O6 C27 -126.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.843 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.092 # Attachment 'Cmpd_2-756142R2.cif' data_n185 _database_code_depnum_ccdc_archive 'CCDC 756142' #TrackingRef 'Cmpd_2-756142R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H35 Mn2 N6 O7, C3 H7 N O, F6 P' _chemical_formula_sum 'C35 H42 F6 Mn2 N7 O8 P' _chemical_formula_weight 943.61 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m _symmetry_space_group_name_Hall -P2yb loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.94680(10) _cell_length_b 20.3942(2) _cell_length_c 12.6593(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.7040(9) _cell_angle_gamma 90.00 _cell_volume 2041.52(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10551 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 29.13 _exptl_crystal_description chunk _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9161 _exptl_absorpt_correction_T_max 0.9638 _exptl_absorpt_process_details 'SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Nonius Kappa CCD' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17465 _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4806 _reflns_number_gt 3920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect package Bruker-Nonius' _computing_cell_refinement HKL _computing_data_reduction HKL _computing_structure_solution 'SIR-97 (Altmore et al, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^+1.8822P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4806 _refine_ls_number_parameters 344 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1394 _refine_ls_wR_factor_gt 0.1296 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.74596(5) 0.167852(18) 0.58636(3) 0.04384(15) Uani 1 1 d . . . N1 N 0.8074(3) 0.05999(10) 0.59776(16) 0.0397(5) Uani 1 1 d . A . N2 N 0.6391(3) 0.12107(11) 0.4342(2) 0.0477(5) Uani 1 1 d . . . C1 C 0.9015(4) 0.03302(13) 0.6791(2) 0.0459(6) Uani 1 1 d . . . H1 H 0.9380 0.0599 0.7382 0.055 Uiso 1 1 calc R A . C2 C 0.9488(4) -0.03228(14) 0.6819(2) 0.0479(6) Uani 1 1 d . A . H2 H 1.0183 -0.0496 0.7407 0.057 Uiso 1 1 calc R . . C3 C 0.8925(4) -0.07135(13) 0.5970(2) 0.0484(6) Uani 1 1 d . . . H3 H 0.9228 -0.1164 0.5963 0.058 Uiso 1 1 calc R A . C4 C 0.7913(4) -0.04446(12) 0.5130(2) 0.0446(6) Uani 1 1 d . A . H4 H 0.7494 -0.0710 0.4545 0.053 Uiso 1 1 calc R . . C5 C 0.7516(3) 0.02192(11) 0.51488(19) 0.0375(5) Uani 1 1 d . . . C6 C 0.6503(3) 0.05548(12) 0.4254(2) 0.0410(5) Uani 1 1 d . . . C7 C 0.5751(4) 0.02253(17) 0.3382(2) 0.0556(7) Uani 1 1 d . . . H7 H 0.5823 -0.0238 0.3331 0.067 Uiso 1 1 calc R A . C8 C 0.4885(5) 0.0592(3) 0.2579(3) 0.0838(13) Uani 1 1 d . A . H8 H 0.4334 0.0379 0.1973 0.101 Uiso 1 1 calc R . . C9 C 0.4825(5) 0.1261(3) 0.2661(4) 0.1019(18) Uani 1 1 d . . . H9 H 0.4257 0.1515 0.2107 0.122 Uiso 1 1 calc R A . C10 C 0.5595(4) 0.15593(18) 0.3553(4) 0.0793(13) Uani 1 1 d . . . C11 C 0.5794(5) 0.2335(2) 0.4042(3) 0.0326(12) Uani 0.50 1 d P . -1 C12 C 0.5408(6) 0.2790(2) 0.3277(4) 0.0353(9) Uani 0.50 1 d P . -1 H12 H 0.5027 0.2500 0.2557 0.040(10) Uiso 1 2 d SR . -1 O1 O 0.6291(3) 0.2500 0.50492(16) 0.0341(5) Uani 1 2 d S . . O2 O 0.9830(2) 0.19564(9) 0.53419(17) 0.0499(5) Uani 1 1 d . A . C13 C 1.0502(4) 0.2500 0.5233(3) 0.0365(7) Uani 1 2 d S . . C14 C 1.2289(5) 0.2500 0.4945(5) 0.0658(13) Uani 1 2 d S A . H14A H 1.2737 0.2948 0.4989 0.099 Uiso 0.50 1 calc PR . . H14B H 1.2312 0.2335 0.4219 0.099 Uiso 0.50 1 calc PR . . H14C H 1.2986 0.2217 0.5438 0.099 Uiso 0.50 1 calc PR . . O3A O 0.8630(18) 0.1965(2) 0.7425(3) 0.051(2) Uani 0.65(4) 1 d P A 3 O3B O 0.800(4) 0.1972(5) 0.7399(8) 0.065(3) Uiso 0.35(4) 1 d P A 4 C15 C 0.8571(5) 0.2500 0.7869(3) 0.0454(8) Uani 1 2 d S . . C16 C 0.8861(7) 0.2500 0.9058(4) 0.0874(19) Uani 1 2 d S A . H16A H 0.7835 0.2651 0.9354 0.131 Uiso 0.50 1 calc PR . . H16B H 0.9802 0.2794 0.9287 0.131 Uiso 0.50 1 calc PR . . H16C H 0.9135 0.2055 0.9309 0.131 Uiso 0.50 1 calc PR . . O4 O 0.5170(3) 0.14515(11) 0.67332(19) 0.0636(6) Uani 1 1 d . A . N3 N 0.4250(3) 0.13265(14) 0.8356(2) 0.0584(7) Uani 1 1 d . . . C17A C 0.5466(4) 0.13236(17) 0.7735(3) 0.0470(9) Uani 0.785(5) 1 d P A 1 H17A H 0.661(5) 0.117(2) 0.804(3) 0.054(11) Uiso 0.785(5) 1 d P A 1 C18A C 0.4635(6) 0.1123(3) 0.9500(3) 0.0687(13) Uani 0.785(5) 1 d P A 1 H18A H 0.3890 0.0760 0.9657 0.103 Uiso 0.785(5) 1 calc PR A 1 H18B H 0.4450 0.1495 0.9964 0.103 Uiso 0.785(5) 1 calc PR A 1 H18C H 0.5817 0.0981 0.9622 0.103 Uiso 0.785(5) 1 calc PR A 1 C19A C 0.2529(5) 0.1479(3) 0.8011(4) 0.0828(16) Uani 0.785(5) 1 d P A 1 H19A H 0.2432 0.1602 0.7259 0.124 Uiso 0.785(5) 1 calc PR A 1 H19B H 0.2155 0.1846 0.8431 0.124 Uiso 0.785(5) 1 calc PR A 1 H19C H 0.1819 0.1095 0.8107 0.124 Uiso 0.785(5) 1 calc PR A 1 C17B C 0.4015(19) 0.1603(7) 0.7171(12) 0.055(4) Uani 0.215(5) 1 d P A 2 H17B H 0.3076 0.1852 0.6871 0.066 Uiso 0.215(5) 1 calc PR A 2 C18B C 0.540(3) 0.0950(10) 0.8644(15) 0.082(4) Uani 0.215(5) 1 d P A 2 H18D H 0.4962 0.0502 0.8661 0.122 Uiso 0.215(5) 1 calc PR A 2 H18E H 0.5901 0.1075 0.9354 0.122 Uiso 0.215(5) 1 calc PR A 2 H18F H 0.6269 0.0972 0.8145 0.122 Uiso 0.215(5) 1 calc PR A 2 C19B C 0.308(3) 0.1713(10) 0.8949(15) 0.082(4) Uani 0.215(5) 1 d P A 2 H19D H 0.2287 0.1416 0.9257 0.122 Uiso 0.215(5) 1 calc PR A 2 H19E H 0.2441 0.2020 0.8465 0.122 Uiso 0.215(5) 1 calc PR A 2 H19F H 0.3723 0.1958 0.9518 0.122 Uiso 0.215(5) 1 calc PR A 2 P1 P 0.0000 0.0000 1.0000 0.0506(3) Uani 1 2 d S . . F1 F 0.1349(2) -0.00894(13) 0.91622(14) 0.0773(6) Uani 1 1 d . . . F2 F 0.1374(3) 0.03736(14) 1.07701(15) 0.0917(8) Uani 1 1 d . . . F3 F -0.0567(4) 0.06689(13) 0.94405(19) 0.1006(8) Uani 1 1 d . . . O5 O 0.2690(4) 0.2500 0.1036(3) 0.0712(10) Uani 1 2 d SD . . C20 C 0.1468(7) 0.2896(3) 0.1197(4) 0.0535(13) Uani 0.50 1 d PD B -1 H20 H 0.1193 0.3301 0.1058 0.050(17) Uiso 0.50 1 d PR B -1 N4 N 0.0117(8) 0.2685(3) 0.1655(5) 0.0556(16) Uani 0.50 1 d P B -1 C21 C -0.1308(10) 0.3120(4) 0.1785(7) 0.0686(18) Uani 0.50 1 d P B -1 H21A H -0.2158 0.3072 0.1173 0.103 Uiso 0.50 1 calc PR B -1 H21B H -0.0911 0.3575 0.1831 0.103 Uiso 0.50 1 calc PR B -1 H21C H -0.1811 0.3004 0.2436 0.103 Uiso 0.50 1 calc PR B -1 C22 C -0.0039(14) 0.2016(5) 0.1967(9) 0.086(3) Uani 0.50 1 d P B -1 H22A H 0.1077 0.1808 0.2030 0.129 Uiso 0.50 1 calc PR B -1 H22B H -0.0793 0.1785 0.1431 0.129 Uiso 0.50 1 calc PR B -1 H22C H -0.0510 0.1998 0.2653 0.129 Uiso 0.50 1 calc PR B -1 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 0.0410(2) 0.0291(2) 0.0650(3) -0.00500(16) 0.02286(18) -0.00167(14) N1 0.0436(11) 0.0343(10) 0.0436(11) -0.0085(8) 0.0165(9) -0.0045(8) N2 0.0331(10) 0.0359(10) 0.0773(16) 0.0047(10) 0.0207(10) -0.0052(8) C1 0.0538(15) 0.0462(14) 0.0391(13) -0.0107(11) 0.0113(11) -0.0021(12) C2 0.0560(15) 0.0484(14) 0.0409(13) -0.0014(11) 0.0134(11) 0.0038(12) C3 0.0640(17) 0.0360(12) 0.0481(14) -0.0013(11) 0.0203(12) 0.0033(12) C4 0.0580(15) 0.0329(11) 0.0447(13) -0.0080(10) 0.0143(11) -0.0067(11) C5 0.0388(12) 0.0336(11) 0.0424(12) -0.0040(9) 0.0152(10) -0.0078(9) C6 0.0350(12) 0.0394(12) 0.0509(14) -0.0005(10) 0.0154(10) -0.0088(10) C7 0.0504(15) 0.0645(18) 0.0515(16) -0.0002(14) 0.0038(12) -0.0132(14) C8 0.055(2) 0.131(4) 0.064(2) 0.024(2) -0.0022(16) -0.018(2) C9 0.0429(18) 0.137(4) 0.126(4) 0.085(3) 0.009(2) 0.002(2) C10 0.0303(14) 0.067(2) 0.145(4) 0.048(2) 0.0324(19) 0.0057(14) C11 0.0214(16) 0.044(4) 0.033(2) -0.0014(16) 0.0060(14) -0.0015(14) C12 0.031(2) 0.047(2) 0.028(2) 0.0009(18) 0.0038(17) -0.0001(18) O1 0.0291(10) 0.0468(13) 0.0269(10) 0.000 0.0047(8) 0.000 O2 0.0339(9) 0.0338(9) 0.0848(14) -0.0118(9) 0.0199(9) -0.0023(7) C13 0.0259(14) 0.0424(17) 0.0422(17) 0.000 0.0081(12) 0.000 C14 0.0307(19) 0.062(3) 0.109(4) 0.000 0.029(2) 0.000 O3A 0.047(5) 0.049(2) 0.058(2) -0.0069(14) 0.0079(18) -0.0067(18) C15 0.0427(19) 0.062(2) 0.0314(17) 0.000 0.0010(14) 0.000 C16 0.064(3) 0.158(6) 0.040(2) 0.000 0.003(2) 0.000 O4 0.0627(13) 0.0539(12) 0.0814(15) 0.0155(11) 0.0437(12) 0.0122(10) N3 0.0487(13) 0.0673(16) 0.0631(15) -0.0194(13) 0.0254(11) -0.0104(12) C17A 0.0420(18) 0.0419(17) 0.060(2) 0.0001(15) 0.0198(15) -0.0042(14) C18A 0.064(3) 0.090(3) 0.054(2) -0.007(2) 0.0175(19) -0.019(2) C19A 0.045(2) 0.122(4) 0.085(3) 0.001(3) 0.024(2) 0.010(3) C17B 0.055(8) 0.050(7) 0.063(8) 0.004(6) 0.016(6) 0.022(6) C18B 0.096(10) 0.080(8) 0.075(8) 0.011(6) 0.037(7) 0.030(7) C19B 0.096(10) 0.080(8) 0.075(8) 0.011(6) 0.037(7) 0.030(7) P1 0.0493(5) 0.0665(7) 0.0361(5) -0.0030(4) 0.0048(4) -0.0088(5) F1 0.0608(11) 0.1239(18) 0.0493(10) -0.0142(10) 0.0161(8) -0.0159(12) F2 0.0804(14) 0.144(2) 0.0521(11) -0.0225(12) 0.0123(10) -0.0500(15) F3 0.130(2) 0.0951(17) 0.0794(15) 0.0220(13) 0.0216(14) 0.0199(16) O5 0.0399(16) 0.116(3) 0.0563(18) 0.000 -0.0013(13) 0.000 C20 0.047(3) 0.065(4) 0.048(3) 0.001(3) -0.001(2) -0.006(3) N4 0.055(3) 0.056(5) 0.056(3) 0.003(2) 0.008(2) -0.005(2) C21 0.060(4) 0.069(4) 0.080(5) -0.014(4) 0.024(3) -0.003(4) C22 0.080(6) 0.073(7) 0.105(7) 0.041(5) 0.010(5) 0.003(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 O3B 2.038(11) . ? Mn1 O2 2.1341(18) . ? Mn1 O1 2.1312(14) . ? Mn1 O3A 2.179(7) . ? Mn1 N2 2.239(3) . ? Mn1 N1 2.255(2) . ? Mn1 O4 2.266(2) . ? N1 C1 1.330(4) . ? N1 C5 1.345(3) . ? N2 C10 1.334(5) . ? N2 C6 1.346(3) . ? C1 C2 1.383(4) . ? C1 H1 0.9500 . ? C2 C3 1.376(4) . ? C2 H2 0.9500 . ? C3 C4 1.382(4) . ? C3 H3 0.9500 . ? C4 C5 1.391(3) . ? C4 H4 0.9500 . ? C5 C6 1.489(4) . ? C6 C7 1.377(4) . ? C7 C8 1.388(5) . ? C7 H7 0.9500 . ? C8 C9 1.368(7) . ? C8 H8 0.9500 . ? C9 C10 1.372(7) . ? C9 H9 0.9500 . ? C10 C12 1.376(6) 4_565 ? C10 C11 1.701(6) . ? C11 O1 1.340(5) . ? C11 C12 1.353(6) . ? C12 C10 1.377(6) 4_565 ? C12 H12 1.1043 . ? O1 C11 1.340(5) 4_565 ? O1 Mn1 2.1313(14) 4_565 ? O2 C13 1.244(2) . ? C13 O2 1.244(2) 4_565 ? C13 C14 1.501(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O3A C15 1.230(5) . ? O3B C15 1.291(15) . ? C15 O3A 1.230(5) 4_565 ? C15 O3B 1.291(15) 4_565 ? C15 C16 1.500(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O4 C17B 1.160(14) . ? O4 C17A 1.293(4) . ? N3 C18B 1.223(18) . ? N3 C17A 1.306(4) . ? N3 C19A 1.428(5) . ? N3 C19B 1.481(17) . ? N3 C18A 1.509(5) . ? N3 C17B 1.596(15) . ? C17A H17A 1.00(4) . ? C18A H18A 0.9800 . ? C18A H18B 0.9800 . ? C18A H18C 0.9800 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C17B H17B 0.9500 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? P1 F3 1.582(2) 3_557 ? P1 F3 1.582(2) . ? P1 F2 1.5849(19) . ? P1 F2 1.5849(19) 3_557 ? P1 F1 1.5916(18) 3_557 ? P1 F1 1.5916(18) . ? O5 C20 1.294(6) . ? O5 C20 1.294(6) 4_565 ? C20 N4 1.341(8) . ? C20 H20 0.8686 . ? N4 C22 1.428(11) . ? N4 C21 1.460(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 O3B Mn1 O2 96.3(8) . . ? O3B Mn1 O1 105.7(4) . . ? O2 Mn1 O1 89.85(8) . . ? O3B Mn1 O3A 13.1(5) . . ? O2 Mn1 O3A 84.2(3) . . ? O1 Mn1 O3A 110.74(19) . . ? O3B Mn1 N2 166.2(7) . . ? O2 Mn1 N2 96.78(8) . . ? O1 Mn1 N2 79.00(7) . . ? O3A Mn1 N2 170.24(18) . . ? O3B Mn1 N1 101.6(3) . . ? O2 Mn1 N1 94.97(7) . . ? O1 Mn1 N1 151.53(7) . . ? O3A Mn1 N1 97.67(19) . . ? N2 Mn1 N1 72.57(8) . . ? O3B Mn1 O4 72.5(8) . . ? O2 Mn1 O4 168.75(9) . . ? O1 Mn1 O4 93.62(8) . . ? O3A Mn1 O4 84.6(3) . . ? N2 Mn1 O4 94.39(9) . . ? N1 Mn1 O4 87.07(8) . . ? C1 N1 C5 118.8(2) . . ? C1 N1 Mn1 123.68(16) . . ? C5 N1 Mn1 117.45(17) . . ? C10 N2 C6 119.9(3) . . ? C10 N2 Mn1 121.9(3) . . ? C6 N2 Mn1 118.17(19) . . ? N1 C1 C2 123.3(2) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 118.1(3) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? C2 C3 C4 119.4(2) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.2(2) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.2(2) . . ? N1 C5 C6 116.1(2) . . ? C4 C5 C6 122.7(2) . . ? N2 C6 C7 121.6(3) . . ? N2 C6 C5 115.4(2) . . ? C7 C6 C5 123.0(2) . . ? C6 C7 C8 117.9(3) . . ? C6 C7 H7 121.0 . . ? C8 C7 H7 121.0 . . ? C9 C8 C7 120.0(4) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 119.2(4) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? N2 C10 C9 121.3(4) . . ? N2 C10 C12 137.3(5) . 4_565 ? C9 C10 C12 101.0(4) . 4_565 ? N2 C10 C11 101.7(4) . . ? C9 C10 C11 136.9(4) . . ? O1 C11 C12 122.2(4) . . ? O1 C11 C10 126.0(3) . . ? C12 C11 C10 111.8(4) . . ? C11 C12 C10 117.9(4) . 4_565 ? C11 C12 H12 104.3 . . ? C10 C12 H12 137.8 4_565 . ? C11 O1 Mn1 136.92(19) 4_565 . ? C11 O1 Mn1 109.67(18) . . ? C11 O1 Mn1 109.68(18) 4_565 4_565 ? C11 O1 Mn1 136.93(19) . 4_565 ? Mn1 O1 Mn1 103.64(9) . 4_565 ? C13 O2 Mn1 132.29(17) . . ? O2 C13 O2 126.0(3) . 4_565 ? O2 C13 C14 116.99(15) . . ? O2 C13 C14 116.99(15) 4_565 . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C15 O3A Mn1 128.3(7) . . ? C15 O3B Mn1 135.7(9) . . ? O3A C15 O3A 125.0(5) . 4_565 ? O3A C15 O3B 123.9(6) . 4_565 ? O3A C15 O3B 123.9(6) 4_565 . ? O3B C15 O3B 113.1(14) 4_565 . ? O3A C15 C16 116.7(3) . . ? O3A C15 C16 116.7(3) 4_565 . ? O3B C15 C16 118.3(5) 4_565 . ? O3B C15 C16 118.3(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17B O4 C17A 70.2(7) . . ? C17B O4 Mn1 152.8(7) . . ? C17A O4 Mn1 116.2(2) . . ? C18B N3 C17A 66.3(9) . . ? C18B N3 C19A 153.5(11) . . ? C17A N3 C19A 124.1(4) . . ? C18B N3 C19B 132.4(12) . . ? C17A N3 C19B 148.1(9) . . ? C19A N3 C19B 53.6(9) . . ? C18B N3 C18A 57.8(9) . . ? C17A N3 C18A 119.0(3) . . ? C19A N3 C18A 116.8(3) . . ? C19B N3 C18A 74.8(8) . . ? C18B N3 C17B 121.0(10) . . ? C17A N3 C17B 57.3(5) . . ? C19A N3 C17B 67.5(6) . . ? C19B N3 C17B 105.6(9) . . ? C18A N3 C17B 173.3(6) . . ? O4 C17A N3 121.1(3) . . ? O4 C17A H17A 121(2) . . ? N3 C17A H17A 118(2) . . ? N3 C18A H18A 109.5 . . ? N3 C18A H18B 109.5 . . ? N3 C18A H18C 109.5 . . ? N3 C19A H19A 109.5 . . ? N3 C19A H19B 109.5 . . ? N3 C19A H19C 109.5 . . ? O4 C17B N3 109.3(10) . . ? O4 C17B H17B 125.3 . . ? N3 C17B H17B 125.3 . . ? N3 C18B H17A 100(2) . . ? N3 C18B H18D 109.5 . . ? N3 C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? N3 C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? N3 C19B H19D 109.5 . . ? N3 C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? N3 C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? F3 P1 F3 179.998(1) 3_557 . ? F3 P1 F2 89.49(15) 3_557 . ? F3 P1 F2 90.51(15) . . ? F3 P1 F2 90.51(15) 3_557 3_557 ? F3 P1 F2 89.49(15) . 3_557 ? F2 P1 F2 180.00(18) . 3_557 ? F3 P1 F1 88.92(13) 3_557 3_557 ? F3 P1 F1 91.08(13) . 3_557 ? F2 P1 F1 90.20(10) . 3_557 ? F2 P1 F1 89.80(10) 3_557 3_557 ? F3 P1 F1 91.08(13) 3_557 . ? F3 P1 F1 88.92(13) . . ? F2 P1 F1 89.80(11) . . ? F2 P1 F1 90.20(10) 3_557 . ? F1 P1 F1 180.00(9) 3_557 . ? C20 O5 C20 77.2(6) . 4_565 ? O5 C20 N4 120.9(6) . . ? O5 C20 H20 137.8 . . ? N4 C20 H20 101.2 . . ? C20 N4 C22 121.4(7) . . ? C20 N4 C21 121.2(6) . . ? C22 N4 C21 117.3(7) . . ? N4 C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 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 O3B Mn1 N1 C1 -17.5(8) . . . . ? O2 Mn1 N1 C1 80.0(2) . . . . ? O1 Mn1 N1 C1 178.88(19) . . . . ? O3A Mn1 N1 C1 -4.8(4) . . . . ? N2 Mn1 N1 C1 175.5(2) . . . . ? O4 Mn1 N1 C1 -88.9(2) . . . . ? O3B Mn1 N1 C5 165.8(8) . . . . ? O2 Mn1 N1 C5 -96.79(17) . . . . ? O1 Mn1 N1 C5 2.1(3) . . . . ? O3A Mn1 N1 C5 178.4(4) . . . . ? N2 Mn1 N1 C5 -1.24(16) . . . . ? O4 Mn1 N1 C5 94.29(18) . . . . ? O3B Mn1 N2 C10 114(2) . . . . ? O2 Mn1 N2 C10 -85.4(2) . . . . ? O1 Mn1 N2 C10 3.2(2) . . . . ? N1 Mn1 N2 C10 -178.5(2) . . . . ? O4 Mn1 N2 C10 96.0(2) . . . . ? O3B Mn1 N2 C6 -63(2) . . . . ? O2 Mn1 N2 C6 97.53(18) . . . . ? O1 Mn1 N2 C6 -173.95(19) . . . . ? N1 Mn1 N2 C6 4.42(17) . . . . ? O4 Mn1 N2 C6 -81.11(18) . . . . ? C5 N1 C1 C2 1.6(4) . . . . ? Mn1 N1 C1 C2 -175.1(2) . . . . ? N1 C1 C2 C3 -1.4(4) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C2 C3 C4 C5 1.4(4) . . . . ? C1 N1 C5 C4 -0.3(3) . . . . ? Mn1 N1 C5 C4 176.62(18) . . . . ? C1 N1 C5 C6 -178.7(2) . . . . ? Mn1 N1 C5 C6 -1.7(3) . . . . ? C3 C4 C5 N1 -1.2(4) . . . . ? C3 C4 C5 C6 177.1(2) . . . . ? C10 N2 C6 C7 -2.8(4) . . . . ? Mn1 N2 C6 C7 174.4(2) . . . . ? C10 N2 C6 C5 176.1(2) . . . . ? Mn1 N2 C6 C5 -6.8(3) . . . . ? N1 C5 C6 N2 5.5(3) . . . . ? C4 C5 C6 N2 -172.8(2) . . . . ? N1 C5 C6 C7 -175.6(2) . . . . ? C4 C5 C6 C7 6.1(4) . . . . ? N2 C6 C7 C8 0.9(4) . . . . ? C5 C6 C7 C8 -177.8(3) . . . . ? C6 C7 C8 C9 1.2(5) . . . . ? C7 C8 C9 C10 -1.5(6) . . . . ? C6 N2 C10 C9 2.5(4) . . . . ? Mn1 N2 C10 C9 -174.6(3) . . . . ? C6 N2 C10 C12 -169.1(4) . . . 4_565 ? Mn1 N2 C10 C12 13.8(6) . . . 4_565 ? C6 N2 C10 C11 179.8(2) . . . . ? Mn1 N2 C10 C11 2.8(3) . . . . ? C8 C9 C10 N2 -0.4(6) . . . . ? C8 C9 C10 C12 173.9(4) . . . 4_565 ? C8 C9 C10 C11 -176.5(4) . . . . ? N2 C10 C11 O1 -13.0(4) . . . . ? C9 C10 C11 O1 163.7(4) . . . . ? C12 C10 C11 O1 179.6(6) 4_565 . . . ? N2 C10 C11 C12 166.1(3) . . . . ? C9 C10 C11 C12 -17.3(6) . . . . ? C12 C10 C11 C12 -1.40(17) 4_565 . . . ? O1 C11 C12 C10 2.1(6) . . . 4_565 ? C10 C11 C12 C10 -176.9(4) . . . 4_565 ? C12 C11 O1 C11 -0.3(4) . . . 4_565 ? C10 C11 O1 C11 178.6(3) . . . 4_565 ? C12 C11 O1 Mn1 -163.0(3) . . . . ? C10 C11 O1 Mn1 15.9(4) . . . . ? C12 C11 O1 Mn1 -24.5(5) . . . 4_565 ? C10 C11 O1 Mn1 154.4(2) . . . 4_565 ? O3B Mn1 O1 C11 171.8(8) . . . 4_565 ? O2 Mn1 O1 C11 75.3(3) . . . 4_565 ? O3A Mn1 O1 C11 159.1(4) . . . 4_565 ? N2 Mn1 O1 C11 -21.6(3) . . . 4_565 ? N1 Mn1 O1 C11 -24.9(4) . . . 4_565 ? O4 Mn1 O1 C11 -115.4(3) . . . 4_565 ? O3B Mn1 O1 C11 -176.1(8) . . . . ? O2 Mn1 O1 C11 87.5(2) . . . . ? O3A Mn1 O1 C11 171.2(4) . . . . ? N2 Mn1 O1 C11 -9.5(2) . . . . ? N1 Mn1 O1 C11 -12.7(3) . . . . ? O4 Mn1 O1 C11 -103.2(2) . . . . ? O3B Mn1 O1 Mn1 31.7(8) . . . 4_565 ? O2 Mn1 O1 Mn1 -64.78(9) . . . 4_565 ? O3A Mn1 O1 Mn1 19.0(4) . . . 4_565 ? N2 Mn1 O1 Mn1 -161.71(10) . . . 4_565 ? N1 Mn1 O1 Mn1 -164.96(12) . . . 4_565 ? O4 Mn1 O1 Mn1 104.52(10) . . . 4_565 ? O3B Mn1 O2 C13 -67.6(5) . . . . ? O1 Mn1 O2 C13 38.2(3) . . . . ? O3A Mn1 O2 C13 -72.7(3) . . . . ? N2 Mn1 O2 C13 117.1(3) . . . . ? N1 Mn1 O2 C13 -169.9(3) . . . . ? O4 Mn1 O2 C13 -69.9(5) . . . . ? Mn1 O2 C13 O2 -5.9(6) . . . 4_565 ? Mn1 O2 C13 C14 174.0(3) . . . . ? O3B Mn1 O3A C15 -64(2) . . . . ? O2 Mn1 O3A C15 93.2(9) . . . . ? O1 Mn1 O3A C15 5.5(11) . . . . ? N1 Mn1 O3A C15 -172.6(9) . . . . ? O4 Mn1 O3A C15 -86.3(10) . . . . ? O2 Mn1 O3B C15 51(3) . . . . ? O1 Mn1 O3B C15 -41(3) . . . . ? O3A Mn1 O3B C15 74(3) . . . . ? N2 Mn1 O3B C15 -148.9(8) . . . . ? N1 Mn1 O3B C15 147(2) . . . . ? O4 Mn1 O3B C15 -130(3) . . . . ? Mn1 O3A C15 O3A -39(2) . . . 4_565 ? Mn1 O3A C15 O3B -11(3) . . . 4_565 ? Mn1 O3A C15 O3B 56.1(19) . . . . ? Mn1 O3A C15 C16 156.1(6) . . . . ? Mn1 O3B C15 O3A -85(3) . . . . ? Mn1 O3B C15 O3A 15(4) . . . 4_565 ? Mn1 O3B C15 O3B 38(4) . . . 4_565 ? Mn1 O3B C15 C16 -177.3(17) . . . . ? O3B Mn1 O4 C17B 67.8(17) . . . . ? O2 Mn1 O4 C17B 70.2(18) . . . . ? O1 Mn1 O4 C17B -37.6(17) . . . . ? O3A Mn1 O4 C17B 72.9(17) . . . . ? N2 Mn1 O4 C17B -116.8(17) . . . . ? N1 Mn1 O4 C17B 170.9(17) . . . . ? O3B Mn1 O4 C17A -29.7(4) . . . . ? O2 Mn1 O4 C17A -27.3(5) . . . . ? O1 Mn1 O4 C17A -135.0(2) . . . . ? O3A Mn1 O4 C17A -24.5(3) . . . . ? N2 Mn1 O4 C17A 145.8(2) . . . . ? N1 Mn1 O4 C17A 73.5(2) . . . . ? C17B O4 C17A N3 13.8(8) . . . . ? Mn1 O4 C17A N3 165.0(2) . . . . ? C18B N3 C17A O4 150.7(12) . . . . ? C19A N3 C17A O4 -1.3(6) . . . . ? C19B N3 C17A O4 -75.8(18) . . . . ? C18A N3 C17A O4 175.3(3) . . . . ? C17B N3 C17A O4 -11.2(7) . . . . ? C17A O4 C17B N3 -10.2(6) . . . . ? Mn1 O4 C17B N3 -119.1(13) . . . . ? C18B N3 C17B O4 -8.1(19) . . . . ? C17A N3 C17B O4 11.3(7) . . . . ? C19A N3 C17B O4 -159.8(13) . . . . ? C19B N3 C17B O4 161.6(13) . . . . ? C20 O5 C20 N4 17.2(7) 4_565 . . . ? O5 C20 N4 C22 -1.1(11) . . . . ? O5 C20 N4 C21 -176.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.707 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.063 # Attachment 'Cmpd_3-756143R2.cif' data_n201a _database_code_depnum_ccdc_archive 'CCDC 756143' #TrackingRef 'Cmpd_3-756143R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H40 Mn4 N8 O11, 2(F6 P), 2(C2 H3 N)' _chemical_formula_sum 'C56 H46 F12 Mn4 N10 O11 P2' _chemical_formula_weight 1544.73 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 9.8849(3) _cell_length_b 11.0951(3) _cell_length_c 15.2615(4) _cell_angle_alpha 79.7990(10) _cell_angle_beta 73.9100(10) _cell_angle_gamma 66.6630(10) _cell_volume 1472.35(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17908 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.68 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 778 _exptl_absorpt_coefficient_mu 1.001 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9065 _exptl_absorpt_correction_T_max 0.9901 _exptl_absorpt_process_details 'Bruker Apex2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 KappaApex2 CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17908 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.67 _reflns_number_total 6781 _reflns_number_gt 5070 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2' _computing_cell_refinement 'Bruker Apex2' _computing_data_reduction 'Bruker Apex2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0834P)^2^+0.2765P] 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 6781 _refine_ls_number_parameters 482 _refine_ls_number_restraints 403 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1421 _refine_ls_wR_factor_gt 0.1326 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.085 _refine_ls_shift/su_mean 0.004 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 0.53692(5) 0.56563(4) 0.68221(3) 0.02167(13) Uani 1 1 d U . . Mn2 Mn 0.51659(5) 0.62149(4) 0.47223(3) 0.01696(13) Uani 1 1 d U . . O1 O 0.5488(2) 0.49250(18) 0.56713(13) 0.0177(4) Uani 1 1 d U . . N1 N 0.4720(3) 0.5061(2) 0.82840(17) 0.0229(5) Uani 1 1 d U . . N2 N 0.7415(3) 0.3947(2) 0.71750(17) 0.0229(5) Uani 1 1 d U . . N3 N 0.7519(3) 0.5526(2) 0.37367(16) 0.0198(5) Uani 1 1 d U . . N4 N 0.4875(3) 0.7385(2) 0.35010(16) 0.0179(5) Uani 1 1 d U . . C1 C 0.3302(4) 0.5527(3) 0.8793(2) 0.0282(7) Uani 1 1 d U . . H1 H 0.2579 0.6263 0.8542 0.034 Uiso 1 1 calc R . . C2 C 0.2830(4) 0.5005(3) 0.9658(2) 0.0320(7) Uani 1 1 d U . . H2 H 0.1811 0.5363 0.9991 0.038 Uiso 1 1 calc R . . C3 C 0.3887(4) 0.3944(3) 1.0024(2) 0.0322(7) Uani 1 1 d U . . H3 H 0.3605 0.3553 1.0618 0.039 Uiso 1 1 calc R . . C4 C 0.5349(4) 0.3460(3) 0.9521(2) 0.0310(7) Uani 1 1 d U . . H4 H 0.6081 0.2727 0.9767 0.037 Uiso 1 1 calc R . . C5 C 0.5764(3) 0.4031(3) 0.8661(2) 0.0242(6) Uani 1 1 d U . . C6 C 0.7287(3) 0.3516(3) 0.8070(2) 0.0219(6) Uani 1 1 d U . . C7 C 0.8541(4) 0.2613(3) 0.8392(2) 0.0297(7) Uani 1 1 d U . . H7 H 0.8441 0.2347 0.9026 0.036 Uiso 1 1 calc R . . C8 C 0.9900(4) 0.2120(3) 0.7799(2) 0.0338(8) Uani 1 1 d U . . H8 H 1.0749 0.1503 0.8017 0.041 Uiso 1 1 calc R . . C9 C 1.0048(4) 0.2523(3) 0.6864(2) 0.0287(7) Uani 1 1 d U . . H9 H 1.0986 0.2182 0.6436 0.034 Uiso 1 1 calc R . . C10 C 0.8781(3) 0.3434(3) 0.6588(2) 0.0232(6) Uani 1 1 d U . . C11 C 0.8854(3) 0.3876(3) 0.5628(2) 0.0248(7) Uani 1 1 d U . . C12 C 0.8868(3) 0.4207(3) 0.4846(2) 0.0192(6) Uani 1 1 d U . . C13 C 0.8826(3) 0.4622(3) 0.3913(2) 0.0209(6) Uani 1 1 d U . . C14 C 1.0099(3) 0.4125(3) 0.3214(2) 0.0262(7) Uani 1 1 d U . . H14 H 1.1008 0.3476 0.3346 0.031 Uiso 1 1 calc R . . C15 C 1.0005(4) 0.4604(3) 0.2315(2) 0.0281(7) Uani 1 1 d U . . H15 H 1.0845 0.4259 0.1824 0.034 Uiso 1 1 calc R . . C16 C 0.8685(3) 0.5583(3) 0.2139(2) 0.0256(6) Uani 1 1 d U . . H16 H 0.8619 0.5937 0.1532 0.031 Uiso 1 1 calc R . . C17 C 0.7466(3) 0.6035(3) 0.2866(2) 0.0212(6) Uani 1 1 d U . . C18 C 0.6010(3) 0.7114(3) 0.2743(2) 0.0190(6) Uani 1 1 d U . . C19 C 0.5835(4) 0.7811(3) 0.1916(2) 0.0249(6) Uani 1 1 d U . . H19 H 0.6649 0.7616 0.1391 0.030 Uiso 1 1 calc R . . C20 C 0.4442(4) 0.8809(3) 0.1858(2) 0.0283(7) Uani 1 1 d U . . H20 H 0.4296 0.9298 0.1292 0.034 Uiso 1 1 calc R . . C21 C 0.3291(3) 0.9073(3) 0.2625(2) 0.0270(7) Uani 1 1 d U . . H21 H 0.2334 0.9744 0.2600 0.032 Uiso 1 1 calc R . . C22 C 0.3550(3) 0.8339(3) 0.3443(2) 0.0231(6) Uani 1 1 d U . . H22 H 0.2755 0.8524 0.3978 0.028 Uiso 1 1 calc R . . O6 O 0.6454(2) 0.6995(2) 0.64267(15) 0.0277(5) Uani 1 1 d U . . O7 O 0.5993(2) 0.7433(2) 0.50320(14) 0.0248(5) Uani 1 1 d U . . C23 C 0.6442(3) 0.7639(3) 0.5665(2) 0.0217(6) Uani 1 1 d U . . C24 C 0.6983(4) 0.8773(3) 0.5496(2) 0.0302(7) Uani 1 1 d U . . H24A H 0.6346 0.9420 0.5946 0.045 Uiso 1 1 calc R . . H24B H 0.6921 0.9189 0.4878 0.045 Uiso 1 1 calc R . . H24C H 0.8035 0.8446 0.5553 0.045 Uiso 1 1 calc R . . O8 O 0.7385(8) 0.4619(7) 0.6146(5) 0.0674(18) Uani 0.50 1 d PU . . O4 O 0.3173(2) 0.7048(2) 0.69015(15) 0.0270(5) Uani 1 1 d U . . O5 O 0.2992(2) 0.75177(19) 0.54375(15) 0.0239(5) Uani 1 1 d U . . C25 C 0.2486(3) 0.7694(3) 0.6270(2) 0.0216(6) Uani 1 1 d U . . C26 C 0.0963(3) 0.8750(3) 0.6557(2) 0.0310(7) Uani 1 1 d U . . H26A H 0.1066 0.9611 0.6444 0.047 Uiso 1 1 calc R . . H26B H 0.0549 0.8594 0.7211 0.047 Uiso 1 1 calc R . . H26C H 0.0278 0.8737 0.6205 0.047 Uiso 1 1 calc R . . P1A P 0.8638(4) 0.8451(2) 0.95238(14) 0.0280(5) Uani 0.872(4) 1 d PDU A 1 F1A F 1.0405(5) 0.8140(4) 0.9209(4) 0.0685(15) Uani 0.872(4) 1 d PDU A 1 F2A F 0.6849(3) 0.8768(3) 0.9851(2) 0.0434(7) Uani 0.872(4) 1 d PDU A 1 F3A F 0.8650(5) 0.8665(4) 1.0518(3) 0.0605(10) Uani 0.872(4) 1 d PDU A 1 F4A F 0.8941(3) 0.6923(2) 0.9835(2) 0.0529(8) Uani 0.872(4) 1 d PDU A 1 F5A F 0.8310(4) 0.9961(3) 0.9202(3) 0.0470(8) Uani 0.872(4) 1 d PDU A 1 F6A F 0.8566(4) 0.8208(3) 0.85373(18) 0.0600(9) Uani 0.872(4) 1 d PDU A 1 P1B P 0.895(2) 0.8413(14) 0.9517(10) 0.051(8) Uani 0.128(4) 1 d PDU A 2 F1B F 1.064(2) 0.819(2) 0.9458(16) 0.047(8) Uani 0.128(4) 1 d PDU A 2 F2B F 0.726(2) 0.861(2) 0.9570(13) 0.0434(7) Uani 0.128(4) 1 d PDU A 2 F3B F 0.846(3) 0.932(2) 1.0310(13) 0.132(19) Uani 0.128(4) 1 d PDU A 2 F4B F 0.911(2) 0.7196(16) 1.0228(12) 0.0529(8) Uani 0.128(4) 1 d PDU A 2 F5B F 0.885(2) 0.9628(13) 0.8811(12) 0.038(5) Uani 0.128(4) 1 d PDU A 2 F6B F 0.955(2) 0.7503(15) 0.8721(10) 0.0600(9) Uani 0.128(4) 1 d PDU A 2 N5 N 0.3413(4) 1.0197(3) 0.6860(3) 0.0470(8) Uani 1 1 d U . . C27 C 0.3670(4) 0.9533(3) 0.7501(3) 0.0404(9) Uani 1 1 d U . . C28 C 0.3976(6) 0.8701(4) 0.8316(3) 0.0625(13) Uani 1 1 d U . . H28A H 0.3840 0.9242 0.8799 0.094 Uiso 1 1 calc R . . H28B H 0.5020 0.8066 0.8185 0.094 Uiso 1 1 calc R . . H28C H 0.3277 0.8227 0.8518 0.094 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0254(3) 0.0247(2) 0.0167(3) -0.00077(18) -0.00608(19) -0.01046(19) Mn2 0.0225(2) 0.0220(2) 0.0117(2) 0.00170(16) -0.00555(17) -0.01377(18) O1 0.0214(10) 0.0209(9) 0.0161(10) 0.0012(8) -0.0065(8) -0.0128(8) N1 0.0246(13) 0.0250(12) 0.0221(14) -0.0018(10) -0.0058(11) -0.0120(10) N2 0.0282(13) 0.0253(12) 0.0211(14) -0.0003(10) -0.0100(11) -0.0135(10) N3 0.0188(12) 0.0295(12) 0.0172(13) -0.0043(10) -0.0033(10) -0.0148(10) N4 0.0220(12) 0.0206(11) 0.0149(12) 0.0007(9) -0.0052(10) -0.0119(10) C1 0.0310(17) 0.0354(17) 0.0215(17) -0.0066(13) -0.0031(13) -0.0156(14) C2 0.0358(19) 0.0420(18) 0.0216(17) 0.0004(14) -0.0062(14) -0.0194(15) C3 0.0377(19) 0.0422(18) 0.0197(17) 0.0027(14) -0.0050(14) -0.0210(15) C4 0.045(2) 0.0338(17) 0.0210(17) 0.0052(13) -0.0137(15) -0.0204(15) C5 0.0321(17) 0.0261(14) 0.0214(16) -0.0003(12) -0.0105(13) -0.0157(13) C6 0.0346(17) 0.0189(13) 0.0179(15) 0.0010(11) -0.0140(13) -0.0114(12) C7 0.0372(19) 0.0315(16) 0.0234(17) 0.0005(13) -0.0134(15) -0.0126(14) C8 0.0347(18) 0.0298(16) 0.035(2) -0.0045(14) -0.0182(16) -0.0023(14) C9 0.0328(17) 0.0256(15) 0.0298(18) -0.0056(13) -0.0137(14) -0.0070(13) C10 0.0252(15) 0.0226(14) 0.0244(17) -0.0073(12) -0.0033(13) -0.0107(12) C11 0.0173(14) 0.0245(14) 0.0317(19) -0.0068(13) -0.0051(13) -0.0052(12) C12 0.0163(13) 0.0219(13) 0.0209(16) 0.0001(11) -0.0047(12) -0.0089(11) C13 0.0202(14) 0.0262(14) 0.0216(16) -0.0027(12) -0.0040(12) -0.0141(12) C14 0.0207(15) 0.0320(16) 0.0272(18) -0.0046(13) -0.0046(13) -0.0104(12) C15 0.0252(16) 0.0373(17) 0.0228(17) -0.0043(13) 0.0007(13) -0.0157(14) C16 0.0286(16) 0.0320(16) 0.0192(16) 0.0019(12) -0.0052(13) -0.0160(13) C17 0.0263(15) 0.0256(14) 0.0177(15) -0.0001(11) -0.0035(12) -0.0174(12) C18 0.0229(14) 0.0222(13) 0.0186(15) 0.0004(11) -0.0067(12) -0.0147(11) C19 0.0325(17) 0.0309(15) 0.0164(15) 0.0020(12) -0.0077(13) -0.0170(13) C20 0.0392(18) 0.0282(15) 0.0238(17) 0.0057(13) -0.0167(15) -0.0157(14) C21 0.0264(16) 0.0217(14) 0.0357(19) 0.0014(13) -0.0154(14) -0.0076(12) C22 0.0245(15) 0.0216(14) 0.0242(16) -0.0037(12) -0.0055(13) -0.0089(12) O6 0.0367(12) 0.0295(11) 0.0255(12) 0.0019(9) -0.0124(10) -0.0193(10) O7 0.0334(12) 0.0282(11) 0.0215(11) 0.0005(9) -0.0092(9) -0.0191(9) C23 0.0205(14) 0.0241(14) 0.0235(16) -0.0047(12) -0.0033(12) -0.0114(11) C24 0.0377(18) 0.0328(17) 0.0299(18) -0.0035(14) -0.0053(15) -0.0244(15) O8 0.071(4) 0.084(5) 0.067(5) 0.010(4) -0.031(4) -0.046(4) O4 0.0259(11) 0.0326(11) 0.0183(11) -0.0011(9) -0.0036(9) -0.0077(9) O5 0.0232(11) 0.0244(10) 0.0219(12) -0.0051(8) -0.0052(9) -0.0050(8) C25 0.0207(14) 0.0227(14) 0.0211(16) -0.0034(12) -0.0016(12) -0.0092(12) C26 0.0225(16) 0.0347(17) 0.0293(19) -0.0043(14) -0.0039(14) -0.0042(13) P1A 0.0277(9) 0.0247(9) 0.0227(10) 0.0063(6) -0.0035(6) -0.0055(5) F1A 0.0306(18) 0.064(3) 0.084(3) 0.020(2) 0.003(2) -0.0102(17) F2A 0.0308(17) 0.0612(15) 0.0295(18) 0.0125(13) -0.0057(12) -0.0152(13) F3A 0.060(2) 0.089(3) 0.0375(18) 0.0006(17) -0.0273(16) -0.0234(18) F4A 0.0598(17) 0.0302(13) 0.065(2) 0.0192(13) -0.0217(15) -0.0170(12) F5A 0.049(2) 0.0264(14) 0.066(2) 0.0095(14) -0.0234(17) -0.0136(14) F6A 0.095(2) 0.0465(16) 0.0305(15) -0.0056(12) -0.0075(15) -0.0206(16) P1B 0.047(12) 0.040(8) 0.049(10) 0.009(6) 0.006(6) -0.016(7) F1B 0.058(17) 0.053(13) 0.045(14) 0.010(10) -0.017(11) -0.037(12) F2B 0.0308(17) 0.0612(15) 0.0295(18) 0.0125(13) -0.0057(12) -0.0152(13) F3B 0.12(3) 0.18(4) 0.09(3) -0.10(3) 0.01(2) -0.05(3) F4B 0.0598(17) 0.0302(13) 0.065(2) 0.0192(13) -0.0217(15) -0.0170(12) F5B 0.032(10) 0.013(8) 0.048(13) 0.001(7) 0.009(8) -0.001(7) F6B 0.095(2) 0.0465(16) 0.0305(15) -0.0056(12) -0.0075(15) -0.0206(16) N5 0.0428(19) 0.0440(18) 0.049(2) 0.0009(16) -0.0134(16) -0.0102(15) C27 0.047(2) 0.0307(18) 0.043(2) -0.0063(17) -0.0111(18) -0.0127(16) C28 0.097(4) 0.037(2) 0.054(3) 0.003(2) -0.021(3) -0.026(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 O8 1.956(7) . ? Mn1 O1 2.0178(19) . ? Mn1 O6 2.075(2) . ? Mn1 O4 2.092(2) . ? Mn1 N1 2.201(3) . ? Mn1 N2 2.276(2) . ? Mn1 Mn2 3.2014(6) . ? Mn2 O1 1.8460(19) . ? Mn2 O1 1.8736(18) 2_666 ? Mn2 O7 2.0087(19) . ? Mn2 N4 2.094(2) . ? Mn2 O5 2.167(2) . ? Mn2 N3 2.305(2) . ? Mn2 Mn2 2.7985(8) 2_666 ? O1 Mn2 1.8736(18) 2_666 ? N1 C1 1.342(4) . ? N1 C5 1.365(4) . ? N2 C6 1.353(4) . ? N2 C10 1.360(4) . ? N3 C13 1.349(4) . ? N3 C17 1.355(4) . ? N4 C22 1.333(4) . ? N4 C18 1.350(4) . ? C1 C2 1.377(5) . ? C1 H1 0.9500 . ? C2 C3 1.381(5) . ? C2 H2 0.9500 . ? C3 C4 1.372(5) . ? C3 H3 0.9500 . ? C4 C5 1.381(4) . ? C4 H4 0.9500 . ? C5 C6 1.468(4) . ? C6 C7 1.401(4) . ? C7 C8 1.357(5) . ? C7 H7 0.9500 . ? C8 C9 1.403(5) . ? C8 H8 0.9500 . ? C9 C10 1.381(4) . ? C9 H9 0.9500 . ? C10 C11 1.452(5) . ? C11 C12 1.183(4) . ? C12 C13 1.423(4) . ? C13 C14 1.393(4) . ? C14 C15 1.394(4) . ? C14 H14 0.9500 . ? C15 C16 1.387(4) . ? C15 H15 0.9500 . ? C16 C17 1.382(4) . ? C16 H16 0.9500 . ? C17 C18 1.499(4) . ? C18 C19 1.375(4) . ? C19 C20 1.398(4) . ? C19 H19 0.9500 . ? C20 C21 1.367(5) . ? C20 H20 0.9500 . ? C21 C22 1.393(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? O6 C23 1.252(4) . ? O7 C23 1.256(3) . ? C23 C24 1.509(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? O4 C25 1.279(4) . ? O5 C25 1.250(4) . ? C25 C26 1.500(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? P1A F1A 1.586(4) . ? P1A F3A 1.581(4) . ? P1A F5A 1.587(3) . ? P1A F6A 1.601(3) . ? P1A F2A 1.606(4) . ? P1A F4A 1.607(3) . ? P1B F6B 1.552(13) . ? P1B F3B 1.558(13) . ? P1B F5B 1.559(13) . ? P1B F4B 1.560(13) . ? P1B F1B 1.571(12) . ? P1B F2B 1.577(12) . ? N5 C27 1.140(5) . ? C27 C28 1.438(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 O8 Mn1 O1 63.04(19) . . ? O8 Mn1 O6 76.53(19) . . ? O1 Mn1 O6 106.82(8) . . ? O8 Mn1 O4 152.8(2) . . ? O1 Mn1 O4 95.27(8) . . ? O6 Mn1 O4 96.12(9) . . ? O8 Mn1 N1 117.2(2) . . ? O1 Mn1 N1 132.72(8) . . ? O6 Mn1 N1 119.44(9) . . ? O4 Mn1 N1 89.36(9) . . ? O8 Mn1 N2 44.2(2) . . ? O1 Mn1 N2 94.52(8) . . ? O6 Mn1 N2 95.14(9) . . ? O4 Mn1 N2 162.27(9) . . ? N1 Mn1 N2 73.16(9) . . ? O8 Mn1 Mn2 75.17(19) . . ? O1 Mn1 Mn2 32.36(5) . . ? O6 Mn1 Mn2 81.72(6) . . ? O4 Mn1 Mn2 77.87(6) . . ? N1 Mn1 Mn2 156.65(6) . . ? N2 Mn1 Mn2 117.38(7) . . ? O1 Mn2 O1 82.41(9) . 2_666 ? O1 Mn2 O7 100.65(8) . . ? O1 Mn2 O7 174.83(9) 2_666 . ? O1 Mn2 N4 169.13(9) . . ? O1 Mn2 N4 88.02(8) 2_666 . ? O7 Mn2 N4 88.52(9) . . ? O1 Mn2 O5 96.36(8) . . ? O1 Mn2 O5 98.84(8) 2_666 . ? O7 Mn2 O5 85.02(8) . . ? N4 Mn2 O5 90.17(9) . . ? O1 Mn2 N3 100.47(9) . . ? O1 Mn2 N3 94.02(8) 2_666 . ? O7 Mn2 N3 81.36(8) . . ? N4 Mn2 N3 74.98(9) . . ? O5 Mn2 N3 160.01(8) . . ? O1 Mn2 Mn2 41.58(6) . 2_666 ? O1 Mn2 Mn2 40.83(6) 2_666 2_666 ? O7 Mn2 Mn2 142.07(7) . 2_666 ? N4 Mn2 Mn2 128.66(6) . 2_666 ? O5 Mn2 Mn2 100.14(6) . 2_666 ? N3 Mn2 Mn2 99.60(6) . 2_666 ? O1 Mn2 Mn1 35.81(6) . . ? O1 Mn2 Mn1 114.34(6) 2_666 . ? O7 Mn2 Mn1 69.84(6) . . ? N4 Mn2 Mn1 155.05(6) . . ? O5 Mn2 Mn1 76.11(6) . . ? N3 Mn2 Mn1 112.28(6) . . ? Mn2 Mn2 Mn1 74.989(18) 2_666 . ? Mn2 O1 Mn2 97.59(9) . 2_666 ? Mn2 O1 Mn1 111.82(9) . . ? Mn2 O1 Mn1 140.78(11) 2_666 . ? C1 N1 C5 117.6(3) . . ? C1 N1 Mn1 123.6(2) . . ? C5 N1 Mn1 118.0(2) . . ? C6 N2 C10 118.2(3) . . ? C6 N2 Mn1 115.8(2) . . ? C10 N2 Mn1 125.6(2) . . ? C13 N3 C17 119.5(2) . . ? C13 N3 Mn2 128.1(2) . . ? C17 N3 Mn2 112.13(18) . . ? C22 N4 C18 119.2(3) . . ? C22 N4 Mn2 120.9(2) . . ? C18 N4 Mn2 119.69(18) . . ? N1 C1 C2 124.0(3) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C1 C2 C3 117.8(3) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C4 C3 C2 119.2(3) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? N1 C5 C4 120.7(3) . . ? N1 C5 C6 116.0(3) . . ? C4 C5 C6 123.1(3) . . ? N2 C6 C7 121.0(3) . . ? N2 C6 C5 115.9(3) . . ? C7 C6 C5 123.1(3) . . ? C8 C7 C6 120.0(3) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 119.9(3) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 117.5(3) . . ? C10 C9 H9 121.2 . . ? C8 C9 H9 121.2 . . ? N2 C10 C9 123.3(3) . . ? N2 C10 C11 116.5(3) . . ? C9 C10 C11 120.2(3) . . ? C12 C11 C10 176.8(3) . . ? C11 C12 C13 177.9(3) . . ? N3 C13 C14 121.6(3) . . ? N3 C13 C12 117.4(3) . . ? C14 C13 C12 120.9(3) . . ? C15 C14 C13 118.3(3) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 118.6(3) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? N3 C17 C16 121.8(3) . . ? N3 C17 C18 115.9(3) . . ? C16 C17 C18 122.3(3) . . ? N4 C18 C19 121.5(3) . . ? N4 C18 C17 115.9(2) . . ? C19 C18 C17 122.6(3) . . ? C18 C19 C20 119.1(3) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 119.3(3) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C22 118.7(3) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? N4 C22 C21 122.3(3) . . ? N4 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C23 O6 Mn1 120.56(18) . . ? C23 O7 Mn2 141.2(2) . . ? O6 C23 O7 125.4(3) . . ? O6 C23 C24 117.6(3) . . ? O7 C23 C24 117.0(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 O4 Mn1 130.60(19) . . ? C25 O5 Mn2 130.17(19) . . ? O5 C25 O4 125.0(3) . . ? O5 C25 C26 117.9(3) . . ? O4 C25 C26 117.0(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? F1A P1A F3A 90.1(3) . . ? F1A P1A F5A 90.3(2) . . ? F3A P1A F5A 91.9(2) . . ? F1A P1A F6A 92.0(3) . . ? F3A P1A F6A 177.4(3) . . ? F5A P1A F6A 89.58(19) . . ? F1A P1A F2A 179.5(3) . . ? F3A P1A F2A 89.4(2) . . ? F5A P1A F2A 89.7(2) . . ? F6A P1A F2A 88.5(2) . . ? F1A P1A F4A 90.6(2) . . ? F3A P1A F4A 89.2(2) . . ? F5A P1A F4A 178.6(3) . . ? F6A P1A F4A 89.29(18) . . ? F2A P1A F4A 89.35(19) . . ? F6B P1B F3B 176.2(16) . . ? F6B P1B F5B 89.9(7) . . ? F3B P1B F5B 89.8(8) . . ? F6B P1B F4B 90.5(8) . . ? F3B P1B F4B 89.7(7) . . ? F5B P1B F4B 177.4(16) . . ? F6B P1B F1B 87.4(10) . . ? F3B P1B F1B 88.8(9) . . ? F5B P1B F1B 88.9(10) . . ? F4B P1B F1B 88.5(10) . . ? F6B P1B F2B 91.8(10) . . ? F3B P1B F2B 92.1(10) . . ? F5B P1B F2B 91.5(10) . . ? F4B P1B F2B 91.1(10) . . ? F1B P1B F2B 179.0(10) . . ? N5 C27 C28 179.3(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 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 O8 Mn1 Mn2 O1 62.7(2) . . . . ? O6 Mn1 Mn2 O1 140.88(12) . . . . ? O4 Mn1 Mn2 O1 -120.98(12) . . . . ? N1 Mn1 Mn2 O1 -62.77(19) . . . . ? N2 Mn1 Mn2 O1 49.36(12) . . . . ? O8 Mn1 Mn2 O1 91.7(2) . . . 2_666 ? O1 Mn1 Mn2 O1 29.00(16) . . . 2_666 ? O6 Mn1 Mn2 O1 169.88(9) . . . 2_666 ? O4 Mn1 Mn2 O1 -91.98(9) . . . 2_666 ? N1 Mn1 Mn2 O1 -33.77(18) . . . 2_666 ? N2 Mn1 Mn2 O1 78.35(10) . . . 2_666 ? O8 Mn1 Mn2 O7 -85.0(2) . . . . ? O1 Mn1 Mn2 O7 -147.71(12) . . . . ? O6 Mn1 Mn2 O7 -6.83(9) . . . . ? O4 Mn1 Mn2 O7 91.30(9) . . . . ? N1 Mn1 Mn2 O7 149.52(18) . . . . ? N2 Mn1 Mn2 O7 -98.36(9) . . . . ? O8 Mn1 Mn2 N4 -116.4(2) . . . . ? O1 Mn1 Mn2 N4 -179.07(18) . . . . ? O6 Mn1 Mn2 N4 -38.19(17) . . . . ? O4 Mn1 Mn2 N4 59.94(17) . . . . ? N1 Mn1 Mn2 N4 118.2(2) . . . . ? N2 Mn1 Mn2 N4 -129.72(17) . . . . ? O8 Mn1 Mn2 O5 -174.74(19) . . . . ? O1 Mn1 Mn2 O5 122.54(12) . . . . ? O6 Mn1 Mn2 O5 -96.57(8) . . . . ? O4 Mn1 Mn2 O5 1.56(8) . . . . ? N1 Mn1 Mn2 O5 59.77(17) . . . . ? N2 Mn1 Mn2 O5 171.90(9) . . . . ? O8 Mn1 Mn2 N3 -13.9(2) . . . . ? O1 Mn1 Mn2 N3 -76.57(12) . . . . ? O6 Mn1 Mn2 N3 64.31(9) . . . . ? O4 Mn1 Mn2 N3 162.45(9) . . . . ? N1 Mn1 Mn2 N3 -139.34(18) . . . . ? N2 Mn1 Mn2 N3 -27.22(9) . . . . ? O8 Mn1 Mn2 Mn2 80.54(19) . . . 2_666 ? O1 Mn1 Mn2 Mn2 17.83(10) . . . 2_666 ? O6 Mn1 Mn2 Mn2 158.71(7) . . . 2_666 ? O4 Mn1 Mn2 Mn2 -103.15(6) . . . 2_666 ? N1 Mn1 Mn2 Mn2 -44.94(17) . . . 2_666 ? N2 Mn1 Mn2 Mn2 67.18(7) . . . 2_666 ? O1 Mn2 O1 Mn2 0.0 2_666 . . 2_666 ? O7 Mn2 O1 Mn2 -175.78(9) . . . 2_666 ? N4 Mn2 O1 Mn2 -28.5(5) . . . 2_666 ? O5 Mn2 O1 Mn2 98.11(9) . . . 2_666 ? N3 Mn2 O1 Mn2 -92.71(9) . . . 2_666 ? Mn1 Mn2 O1 Mn2 153.54(14) . . . 2_666 ? O1 Mn2 O1 Mn1 -153.54(14) 2_666 . . . ? O7 Mn2 O1 Mn1 30.68(11) . . . . ? N4 Mn2 O1 Mn1 177.9(4) . . . . ? O5 Mn2 O1 Mn1 -55.43(10) . . . . ? N3 Mn2 O1 Mn1 113.75(10) . . . . ? Mn2 Mn2 O1 Mn1 -153.54(14) 2_666 . . . ? O8 Mn1 O1 Mn2 -105.4(2) . . . . ? O6 Mn1 O1 Mn2 -40.71(12) . . . . ? O4 Mn1 O1 Mn2 57.33(11) . . . . ? N1 Mn1 O1 Mn2 151.33(10) . . . . ? N2 Mn1 O1 Mn2 -137.48(10) . . . . ? O8 Mn1 O1 Mn2 118.9(3) . . . 2_666 ? O6 Mn1 O1 Mn2 -176.40(16) . . . 2_666 ? O4 Mn1 O1 Mn2 -78.37(17) . . . 2_666 ? N1 Mn1 O1 Mn2 15.6(2) . . . 2_666 ? N2 Mn1 O1 Mn2 86.83(17) . . . 2_666 ? Mn2 Mn1 O1 Mn2 -135.7(2) . . . 2_666 ? O8 Mn1 N1 C1 -168.1(3) . . . . ? O1 Mn1 N1 C1 -90.8(2) . . . . ? O6 Mn1 N1 C1 102.5(2) . . . . ? O4 Mn1 N1 C1 5.8(2) . . . . ? N2 Mn1 N1 C1 -171.1(2) . . . . ? Mn2 Mn1 N1 C1 -50.4(3) . . . . ? O8 Mn1 N1 C5 2.2(3) . . . . ? O1 Mn1 N1 C5 79.6(2) . . . . ? O6 Mn1 N1 C5 -87.2(2) . . . . ? O4 Mn1 N1 C5 176.2(2) . . . . ? N2 Mn1 N1 C5 -0.81(19) . . . . ? Mn2 Mn1 N1 C5 119.9(2) . . . . ? O8 Mn1 N2 C6 178.1(3) . . . . ? O1 Mn1 N2 C6 -139.16(19) . . . . ? O6 Mn1 N2 C6 113.47(19) . . . . ? O4 Mn1 N2 C6 -15.8(4) . . . . ? N1 Mn1 N2 C6 -5.76(18) . . . . ? Mn2 Mn1 N2 C6 -163.20(17) . . . . ? O8 Mn1 N2 C10 5.6(3) . . . . ? O1 Mn1 N2 C10 48.3(2) . . . . ? O6 Mn1 N2 C10 -59.0(2) . . . . ? O4 Mn1 N2 C10 171.7(3) . . . . ? N1 Mn1 N2 C10 -178.3(2) . . . . ? Mn2 Mn1 N2 C10 24.3(2) . . . . ? O1 Mn2 N3 C13 -13.5(2) . . . . ? O1 Mn2 N3 C13 -96.5(2) 2_666 . . . ? O7 Mn2 N3 C13 85.8(2) . . . . ? N4 Mn2 N3 C13 176.6(2) . . . . ? O5 Mn2 N3 C13 133.4(3) . . . . ? Mn2 Mn2 N3 C13 -55.8(2) 2_666 . . . ? Mn1 Mn2 N3 C13 21.8(2) . . . . ? O1 Mn2 N3 C17 159.44(18) . . . . ? O1 Mn2 N3 C17 76.43(18) 2_666 . . . ? O7 Mn2 N3 C17 -101.23(19) . . . . ? N4 Mn2 N3 C17 -10.44(18) . . . . ? O5 Mn2 N3 C17 -53.6(3) . . . . ? Mn2 Mn2 N3 C17 117.19(17) 2_666 . . . ? Mn1 Mn2 N3 C17 -165.20(16) . . . . ? O1 Mn2 N4 C22 117.1(5) . . . . ? O1 Mn2 N4 C22 88.8(2) 2_666 . . . ? O7 Mn2 N4 C22 -95.1(2) . . . . ? O5 Mn2 N4 C22 -10.0(2) . . . . ? N3 Mn2 N4 C22 -176.5(2) . . . . ? Mn2 Mn2 N4 C22 93.1(2) 2_666 . . . ? Mn1 Mn2 N4 C22 -65.8(3) . . . . ? O1 Mn2 N4 C18 -58.2(5) . . . . ? O1 Mn2 N4 C18 -86.5(2) 2_666 . . . ? O7 Mn2 N4 C18 89.6(2) . . . . ? O5 Mn2 N4 C18 174.7(2) . . . . ? N3 Mn2 N4 C18 8.18(19) . . . . ? Mn2 Mn2 N4 C18 -82.2(2) 2_666 . . . ? Mn1 Mn2 N4 C18 118.89(19) . . . . ? C5 N1 C1 C2 -2.0(4) . . . . ? Mn1 N1 C1 C2 168.4(2) . . . . ? N1 C1 C2 C3 0.6(5) . . . . ? C1 C2 C3 C4 0.3(5) . . . . ? C2 C3 C4 C5 0.4(5) . . . . ? C1 N1 C5 C4 2.6(4) . . . . ? Mn1 N1 C5 C4 -168.3(2) . . . . ? C1 N1 C5 C6 177.7(2) . . . . ? Mn1 N1 C5 C6 6.8(3) . . . . ? C3 C4 C5 N1 -1.8(5) . . . . ? C3 C4 C5 C6 -176.6(3) . . . . ? C10 N2 C6 C7 3.1(4) . . . . ? Mn1 N2 C6 C7 -170.0(2) . . . . ? C10 N2 C6 C5 -175.8(2) . . . . ? Mn1 N2 C6 C5 11.1(3) . . . . ? N1 C5 C6 N2 -11.9(4) . . . . ? C4 C5 C6 N2 163.1(3) . . . . ? N1 C5 C6 C7 169.3(3) . . . . ? C4 C5 C6 C7 -15.7(4) . . . . ? N2 C6 C7 C8 -2.5(4) . . . . ? C5 C6 C7 C8 176.3(3) . . . . ? C6 C7 C8 C9 0.5(5) . . . . ? C7 C8 C9 C10 0.8(5) . . . . ? C6 N2 C10 C9 -1.8(4) . . . . ? Mn1 N2 C10 C9 170.6(2) . . . . ? C6 N2 C10 C11 177.2(2) . . . . ? Mn1 N2 C10 C11 -10.4(3) . . . . ? C8 C9 C10 N2 -0.1(4) . . . . ? C8 C9 C10 C11 -179.1(3) . . . . ? C17 N3 C13 C14 -4.7(4) . . . . ? Mn2 N3 C13 C14 167.8(2) . . . . ? C17 N3 C13 C12 174.2(2) . . . . ? Mn2 N3 C13 C12 -13.3(3) . . . . ? N3 C13 C14 C15 1.2(4) . . . . ? C12 C13 C14 C15 -177.7(3) . . . . ? C13 C14 C15 C16 2.2(4) . . . . ? C14 C15 C16 C17 -2.0(4) . . . . ? C13 N3 C17 C16 4.9(4) . . . . ? Mn2 N3 C17 C16 -168.7(2) . . . . ? C13 N3 C17 C18 -175.0(2) . . . . ? Mn2 N3 C17 C18 11.3(3) . . . . ? C15 C16 C17 N3 -1.5(4) . . . . ? C15 C16 C17 C18 178.4(3) . . . . ? C22 N4 C18 C19 0.9(4) . . . . ? Mn2 N4 C18 C19 176.2(2) . . . . ? C22 N4 C18 C17 179.7(2) . . . . ? Mn2 N4 C18 C17 -5.0(3) . . . . ? N3 C17 C18 N4 -5.1(3) . . . . ? C16 C17 C18 N4 174.9(2) . . . . ? N3 C17 C18 C19 173.6(2) . . . . ? C16 C17 C18 C19 -6.3(4) . . . . ? N4 C18 C19 C20 -1.0(4) . . . . ? C17 C18 C19 C20 -179.7(2) . . . . ? C18 C19 C20 C21 0.4(4) . . . . ? C19 C20 C21 C22 0.3(4) . . . . ? C18 N4 C22 C21 -0.2(4) . . . . ? Mn2 N4 C22 C21 -175.5(2) . . . . ? C20 C21 C22 N4 -0.4(4) . . . . ? O8 Mn1 O6 C23 87.2(3) . . . . ? O1 Mn1 O6 C23 31.2(2) . . . . ? O4 Mn1 O6 C23 -66.2(2) . . . . ? N1 Mn1 O6 C23 -159.0(2) . . . . ? N2 Mn1 O6 C23 127.5(2) . . . . ? Mn2 Mn1 O6 C23 10.5(2) . . . . ? O1 Mn2 O7 C23 -10.8(3) . . . . ? N4 Mn2 O7 C23 175.0(3) . . . . ? O5 Mn2 O7 C23 84.7(3) . . . . ? N3 Mn2 O7 C23 -110.0(3) . . . . ? Mn2 Mn2 O7 C23 -15.4(4) 2_666 . . . ? Mn1 Mn2 O7 C23 7.7(3) . . . . ? Mn1 O6 C23 O7 -10.3(4) . . . . ? Mn1 O6 C23 C24 168.5(2) . . . . ? Mn2 O7 C23 O6 -1.6(5) . . . . ? Mn2 O7 C23 C24 179.6(2) . . . . ? O8 Mn1 O4 C25 3.1(5) . . . . ? O1 Mn1 O4 C25 -32.2(3) . . . . ? O6 Mn1 O4 C25 75.4(2) . . . . ? N1 Mn1 O4 C25 -165.0(2) . . . . ? N2 Mn1 O4 C25 -155.4(3) . . . . ? Mn2 Mn1 O4 C25 -4.7(2) . . . . ? O1 Mn2 O5 C25 30.2(2) . . . . ? O1 Mn2 O5 C25 113.5(2) 2_666 . . . ? O7 Mn2 O5 C25 -70.0(2) . . . . ? N4 Mn2 O5 C25 -158.5(2) . . . . ? N3 Mn2 O5 C25 -117.1(3) . . . . ? Mn2 Mn2 O5 C25 72.1(2) 2_666 . . . ? Mn1 Mn2 O5 C25 0.5(2) . . . . ? Mn2 O5 C25 O4 -4.0(4) . . . . ? Mn2 O5 C25 C26 175.41(19) . . . . ? Mn1 O4 C25 O5 6.9(4) . . . . ? Mn1 O4 C25 C26 -172.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.67 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.837 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.099 # Attachment 'Cmpd_4-756144R2.cif' data_n215 _database_code_depnum_ccdc_archive 'CCDC 756144' #TrackingRef 'Cmpd_4-756144R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H42 Fe2 N12, C0.80 H1.20 N0.40, C1.20 H1.80 N0.60, 4(C F3 O3 S)' _chemical_formula_sum 'C72 H45 F12 Fe2 N13 O12 S4' _chemical_formula_weight 1752.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe .3463 .8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c _symmetry_space_group_name_Hall -P2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 17.2541(7) _cell_length_b 10.5472(5) _cell_length_c 23.8490(8) _cell_angle_alpha 90.00 _cell_angle_beta 124.434(2) _cell_angle_gamma 90.00 _cell_volume 3579.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 28126 _cell_measurement_theta_min 2.404 _cell_measurement_theta_max 23.336 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 0.627 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9118 _exptl_absorpt_correction_T_max 0.9876 _exptl_absorpt_process_details 'SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 Kappa APEX II CCD' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27025 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 26.47 _reflns_number_total 7364 _reflns_number_gt 4394 _reflns_threshold_expression >2sigma(I) _computing_data_collection APEX2 _computing_cell_refinement APEX2 _computing_data_reduction APEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0511P)^2^+9.8961P] 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 7364 _refine_ls_number_parameters 592 _refine_ls_number_restraints 191 _refine_ls_R_factor_all 0.1152 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1558 _refine_ls_wR_factor_gt 0.1231 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.042 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.22241(4) 0.75841(6) 0.34373(3) 0.02525(16) Uani 1 1 d . . . N1 N 0.3093(2) 0.8050(4) 0.45178(18) 0.0337(9) Uani 1 1 d . . . N2 N 0.1564(2) 0.6579(3) 0.38661(16) 0.0218(7) Uani 1 1 d . . . N3 N 0.2992(2) 0.5877(4) 0.35585(18) 0.0347(9) Uani 1 1 d . . . N4 N 0.1657(2) 0.6933(3) 0.23790(17) 0.0277(8) Uani 1 1 d . . . N5 N 0.3091(2) 0.8775(3) 0.32470(16) 0.0279(8) Uani 1 1 d . . . C1 C 0.3829(3) 0.8840(5) 0.4810(2) 0.0501(14) Uani 1 1 d . . . H1 H 0.4021 0.9189 0.4540 0.060 Uiso 1 1 calc R . . C2 C 0.4321(3) 0.9168(5) 0.5492(2) 0.0509(14) Uani 1 1 d . . . H2 H 0.4843 0.9728 0.5686 0.061 Uiso 1 1 calc R . . C3 C 0.4037(3) 0.8664(5) 0.5880(2) 0.0408(12) Uani 1 1 d . . . H3 H 0.4358 0.8880 0.6347 0.049 Uiso 1 1 calc R . . C4 C 0.3287(3) 0.7846(4) 0.5587(2) 0.0328(10) Uani 1 1 d . . . H4 H 0.3089 0.7487 0.5851 0.039 Uiso 1 1 calc R . . C5 C 0.2818(3) 0.7547(4) 0.48993(19) 0.0245(8) Uani 1 1 d . . . C6 C 0.2009(3) 0.6673(4) 0.45502(19) 0.0238(9) Uani 1 1 d . . . C7 C 0.1715(3) 0.6012(4) 0.4898(2) 0.0288(9) Uani 1 1 d . . . H7 H 0.2038 0.6108 0.5376 0.035 Uiso 1 1 calc R . . C8 C 0.0953(3) 0.5216(4) 0.4551(2) 0.0312(10) Uani 1 1 d . . . H8 H 0.0741 0.4762 0.4784 0.037 Uiso 1 1 calc R . . C9 C 0.0500(3) 0.5086(4) 0.3854(2) 0.0269(9) Uani 1 1 d . . . H9 H -0.0015 0.4520 0.3603 0.032 Uiso 1 1 calc R . . C10 C 0.0813(3) 0.5798(4) 0.35329(19) 0.0226(8) Uani 1 1 d . . . C11 C 0.0272(3) 0.5777(4) 0.28016(19) 0.0224(8) Uani 1 1 d . . . C12 C 0.3572(3) 0.5268(5) 0.4153(2) 0.0461(13) Uani 1 1 d . . . H12 H 0.3638 0.5589 0.4550 0.055 Uiso 1 1 calc R . . C13 C 0.4073(4) 0.4200(6) 0.4209(3) 0.0567(15) Uani 1 1 d . . . H13 H 0.4473 0.3794 0.4636 0.068 Uiso 1 1 calc R . . C14 C 0.3983(3) 0.3736(5) 0.3638(3) 0.0532(14) Uani 1 1 d . . . H14 H 0.4336 0.3017 0.3668 0.064 Uiso 1 1 calc R . . C15 C 0.3373(3) 0.4324(5) 0.3016(3) 0.0424(12) Uani 1 1 d . . . H15 H 0.3288 0.3998 0.2614 0.051 Uiso 1 1 calc R . . C16 C 0.2890(3) 0.5391(4) 0.2993(2) 0.0325(10) Uani 1 1 d . . . C17 C 0.2230(3) 0.6091(4) 0.2357(2) 0.0297(10) Uani 1 1 d . . . C18 C 0.2221(3) 0.5895(4) 0.1772(2) 0.0398(11) Uani 1 1 d . . . H18 H 0.2640 0.5304 0.1776 0.048 Uiso 1 1 calc R . . C19 C 0.1603(4) 0.6562(5) 0.1197(2) 0.0468(13) Uani 1 1 d . . . H19 H 0.1599 0.6458 0.0800 0.056 Uiso 1 1 calc R . . C20 C 0.0984(3) 0.7387(4) 0.1198(2) 0.0382(11) Uani 1 1 d . . . H20 H 0.0537 0.7844 0.0798 0.046 Uiso 1 1 calc R . . C21 C 0.1026(3) 0.7540(4) 0.1792(2) 0.0294(9) Uani 1 1 d . . . C22 C 0.0355(3) 0.8361(4) 0.1782(2) 0.0305(10) Uani 1 1 d . . . C23 C -0.0277(3) 0.8994(4) 0.1698(2) 0.0352(11) Uani 1 1 d . . . N6 N 0.15795(19) 0.9519(2) 0.32414(15) 0.0329(8) Uani 1 1 d G . . C24 C 0.0894(2) 0.9890(3) 0.33427(19) 0.0432(12) Uani 1 1 d G . . C25 C 0.0736(3) 1.1171(3) 0.3377(3) 0.100(2) Uani 1 1 d G . . H25 H 0.0268 1.1425 0.3447 0.120 Uiso 1 1 calc R . . C26 C 0.1262(3) 1.2080(2) 0.3311(3) 0.100(2) Uani 1 1 d G . . H26 H 0.1153 1.2955 0.3335 0.120 Uiso 1 1 calc R . . C27 C 0.1947(3) 1.1709(2) 0.3210(3) 0.083(2) Uani 1 1 d G . . H27 H 0.2307 1.2330 0.3164 0.099 Uiso 1 1 calc R . . C28 C 0.2106(2) 1.0428(3) 0.31748(19) 0.0434(12) Uani 1 1 d G . . C29 C 0.2772(3) 0.9971(4) 0.3041(2) 0.0332(10) Uani 1 1 d . . . C30 C 0.3066(3) 1.0716(5) 0.2719(2) 0.0408(11) Uani 1 1 d . . . H30 H 0.2828 1.1552 0.2576 0.049 Uiso 1 1 calc R . . C31 C 0.3704(3) 1.0236(5) 0.2607(2) 0.0418(12) Uani 1 1 d . . . H31 H 0.3893 1.0724 0.2369 0.050 Uiso 1 1 calc R . . C32 C 0.4068(3) 0.9046(5) 0.2839(2) 0.0411(12) Uani 1 1 d . . . H32 H 0.4530 0.8712 0.2781 0.049 Uiso 1 1 calc R . . C33 C 0.3746(3) 0.8342(4) 0.3159(2) 0.0336(10) Uani 1 1 d . . . H33 H 0.4000 0.7520 0.3322 0.040 Uiso 1 1 calc R . . S1 S 0.13260(8) 0.27479(10) 0.12026(6) 0.0334(3) Uani 1 1 d D . . O1 O 0.0729(2) 0.3623(3) 0.06617(18) 0.0442(8) Uani 1 1 d D . . O2 O 0.2311(2) 0.2824(3) 0.14649(15) 0.0343(7) Uani 1 1 d D . . O3 O 0.1139(2) 0.2628(3) 0.17180(18) 0.0486(9) Uani 1 1 d D . . F1 F 0.0066(2) 0.1011(3) 0.04833(17) 0.0660(9) Uani 1 1 d D . . F2 F 0.11225(19) 0.1186(3) 0.02759(14) 0.0482(7) Uani 1 1 d D . . F3 F 0.1450(2) 0.0273(3) 0.11905(16) 0.0621(9) Uani 1 1 d D . . C34 C 0.0974(3) 0.1226(4) 0.0768(3) 0.0414(12) Uani 1 1 d D . . S2A S 0.6238(3) 0.6783(5) 0.4177(2) 0.0645(12) Uani 0.40 1 d PD A 1 O4A O 0.6675(13) 0.5630(14) 0.4138(9) 0.137(9) Uani 0.40 1 d PD A 1 O5A O 0.5503(7) 0.6551(16) 0.4243(6) 0.0645(12) Uani 0.40 1 d PD A 1 O6A O 0.6051(8) 0.7731(13) 0.3691(5) 0.070(4) Uani 0.40 1 d PD A 1 F4A F 0.7961(7) 0.7616(10) 0.4953(5) 0.071(3) Uani 0.40 1 d PD A 1 F5A F 0.7552(5) 0.6551(9) 0.5500(4) 0.058(2) Uani 0.40 1 d PD A 1 F6A F 0.7026(9) 0.8423(11) 0.5191(5) 0.114(5) Uani 0.40 1 d PD A 1 C35A C 0.7235(10) 0.7404(14) 0.4998(7) 0.114(5) Uani 0.40 1 d PD A 1 S2B S 0.6202(5) 0.6961(6) 0.4711(3) 0.0598(16) Uiso 0.24 1 d PD B 2 O4B O 0.5510(12) 0.6109(15) 0.4203(9) 0.058(6) Uiso 0.24 1 d PD B 2 O5B O 0.6975(11) 0.6209(16) 0.5257(8) 0.057(5) Uiso 0.24 1 d PD B 2 O6B O 0.5872(12) 0.7975(14) 0.4891(9) 0.074(5) Uiso 0.24 1 d PD B 2 F4B F 0.6167(12) 0.8431(16) 0.3806(8) 0.063(5) Uiso 0.24 1 d PD B 2 F5B F 0.7110(11) 0.6806(15) 0.4129(8) 0.086(5) Uiso 0.24 1 d PD B 2 F6B F 0.7463(10) 0.8429(15) 0.4759(8) 0.074(4) Uiso 0.24 1 d PD B 2 C35B C 0.6742(11) 0.7688(15) 0.4321(8) 0.047(6) Uiso 0.24 1 d PD B 2 S2C S 0.5942(4) 0.5903(5) 0.3884(3) 0.0469(12) Uiso 0.26 1 d PD C 3 O4C O 0.5050(8) 0.6319(14) 0.3326(7) 0.065(4) Uiso 0.26 1 d PD C 3 O5C O 0.6516(10) 0.5300(15) 0.3719(8) 0.056(4) Uiso 0.26 1 d PD C 3 O6C O 0.5983(11) 0.5291(14) 0.4431(6) 0.060(4) Uiso 0.26 1 d PD C 3 F4C F 0.6080(12) 0.8067(16) 0.4477(9) 0.107(5) Uiso 0.26 1 d PD C 3 F5C F 0.6593(14) 0.8084(19) 0.3829(9) 0.096(7) Uiso 0.26 1 d PD C 3 F6C F 0.7387(10) 0.7227(15) 0.4854(7) 0.076(4) Uiso 0.26 1 d PD C 3 C35C C 0.6534(13) 0.7399(16) 0.4281(9) 0.076(4) Uiso 0.26 1 d PD C 3 S2D S 0.6640(12) 0.6631(14) 0.4512(8) 0.057(4) Uiso 0.10 1 d PD D 4 O4D O 0.5757(18) 0.716(3) 0.4325(19) 0.060(12) Uiso 0.10 1 d PD D 4 O5D O 0.672(2) 0.584(2) 0.4059(14) 0.000(5) Uiso 0.10 1 d PD D 4 O6D O 0.724(3) 0.627(3) 0.5217(11) 0.043(13) Uiso 0.10 1 d PD D 4 F4D F 0.725(3) 0.896(3) 0.5040(17) 0.074(13) Uiso 0.10 1 d PD D 4 F5D F 0.671(3) 0.883(3) 0.4004(16) 0.098(14) Uiso 0.10 1 d PD D 4 F6D F 0.8088(19) 0.802(3) 0.4808(19) 0.068(11) Uiso 0.10 1 d PD D 4 C35D C 0.7204(19) 0.817(2) 0.4583(15) 0.068(11) Uiso 0.10 1 d PD D 4 N7A N 0.5000 0.2699(15) 0.2500 0.053(6) Uani 0.60 2 d SP E 5 C36A C 0.5000 0.3805(19) 0.2500 0.066(3) Uani 0.60 2 d SP E 5 C37A C 0.5000 0.5167(13) 0.2500 0.066(3) Uani 0.60 2 d SP E 5 H37A H 0.4769 0.5477 0.2043 0.098 Uiso 0.30 1 d PR E 5 H37B H 0.5641 0.5477 0.2824 0.098 Uiso 0.30 1 d PR E 5 H37C H 0.4590 0.5477 0.2633 0.098 Uiso 0.30 1 d PR E 5 N7B N 0.5000 0.243(3) 0.2500 0.070(14) Uiso 0.40 2 d SPD F 6 C36B C 0.5160(19) 0.338(2) 0.2708(13) 0.034(8) Uiso 0.20 1 d PD F 6 C37B C 0.5633(17) 0.470(2) 0.3051(12) 0.041(6) Uiso 0.20 1 d P F 6 H37D H 0.6188 0.4549 0.3513 0.061 Uiso 0.20 1 calc PR F 6 H37E H 0.5183 0.5225 0.3072 0.061 Uiso 0.20 1 calc PR F 6 H37F H 0.5821 0.5127 0.2782 0.061 Uiso 0.20 1 calc PR F 6 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 Fe1 0.0220(3) 0.0315(3) 0.0224(3) -0.0031(3) 0.0127(2) -0.0024(3) N1 0.031(2) 0.041(2) 0.0267(19) -0.0077(17) 0.0148(17) -0.0112(17) N2 0.0175(16) 0.0218(17) 0.0215(17) -0.0007(14) 0.0083(14) 0.0034(13) N3 0.0231(18) 0.045(2) 0.029(2) -0.0053(18) 0.0103(16) 0.0016(17) N4 0.0192(17) 0.0288(19) 0.031(2) -0.0041(16) 0.0114(15) -0.0068(15) N5 0.0235(17) 0.038(2) 0.0205(18) -0.0057(16) 0.0115(15) -0.0043(16) C1 0.044(3) 0.072(4) 0.032(3) -0.009(3) 0.020(2) -0.030(3) C2 0.037(3) 0.072(4) 0.035(3) -0.019(3) 0.016(2) -0.032(3) C3 0.035(3) 0.058(3) 0.031(2) -0.016(2) 0.019(2) -0.014(2) C4 0.028(2) 0.043(3) 0.030(2) -0.010(2) 0.017(2) -0.006(2) C5 0.0217(19) 0.028(2) 0.024(2) -0.0033(18) 0.0127(17) 0.0018(17) C6 0.024(2) 0.024(2) 0.021(2) -0.0014(17) 0.0110(18) 0.0062(17) C7 0.031(2) 0.028(2) 0.022(2) 0.0020(18) 0.0121(19) 0.0003(18) C8 0.031(2) 0.030(2) 0.025(2) 0.0066(19) 0.012(2) -0.0045(19) C9 0.024(2) 0.022(2) 0.026(2) 0.0018(17) 0.0092(18) -0.0003(17) C10 0.023(2) 0.019(2) 0.021(2) -0.0001(16) 0.0100(17) 0.0031(16) C11 0.020(2) 0.021(2) 0.0272(19) -0.0006(16) 0.0146(17) 0.0009(16) C12 0.032(3) 0.062(3) 0.032(3) 0.002(2) 0.011(2) 0.015(2) C13 0.040(3) 0.064(4) 0.040(3) -0.001(3) 0.007(2) 0.018(3) C14 0.032(3) 0.054(3) 0.052(3) -0.007(3) 0.011(3) 0.012(2) C15 0.032(3) 0.043(3) 0.045(3) -0.011(2) 0.017(2) 0.000(2) C16 0.021(2) 0.041(3) 0.032(2) -0.012(2) 0.0128(19) -0.0045(19) C17 0.025(2) 0.031(2) 0.030(2) -0.0091(19) 0.0136(19) -0.0085(18) C18 0.049(3) 0.033(3) 0.039(3) -0.014(2) 0.026(2) -0.006(2) C19 0.072(4) 0.035(3) 0.034(3) -0.014(2) 0.030(3) -0.005(3) C20 0.045(3) 0.034(3) 0.024(2) -0.006(2) 0.012(2) -0.011(2) C21 0.025(2) 0.027(2) 0.029(2) -0.0048(19) 0.0113(18) -0.0106(19) C22 0.023(2) 0.035(2) 0.030(2) 0.0028(19) 0.0128(19) -0.0087(19) C23 0.032(2) 0.036(3) 0.037(3) 0.005(2) 0.019(2) -0.007(2) N6 0.0292(19) 0.032(2) 0.036(2) -0.0077(17) 0.0179(17) -0.0032(16) C24 0.039(3) 0.037(3) 0.060(3) -0.011(2) 0.032(3) -0.001(2) C25 0.118(4) 0.035(2) 0.216(7) -0.018(3) 0.136(5) -0.003(3) C26 0.118(4) 0.035(2) 0.216(7) -0.018(3) 0.136(5) -0.003(3) C27 0.096(5) 0.036(3) 0.166(7) -0.015(4) 0.105(6) -0.010(3) C28 0.042(3) 0.037(3) 0.058(3) -0.008(2) 0.032(3) -0.004(2) C29 0.027(2) 0.035(3) 0.032(2) -0.005(2) 0.013(2) -0.0041(19) C30 0.034(3) 0.041(3) 0.045(3) 0.006(2) 0.021(2) 0.001(2) C31 0.041(3) 0.053(3) 0.031(3) 0.003(2) 0.020(2) -0.006(2) C32 0.032(2) 0.056(3) 0.041(3) -0.006(2) 0.025(2) -0.003(2) C33 0.029(2) 0.039(3) 0.029(2) -0.005(2) 0.014(2) -0.003(2) S1 0.0362(6) 0.0256(6) 0.0494(7) -0.0019(5) 0.0308(6) 0.0014(5) O1 0.046(2) 0.0319(18) 0.065(2) 0.0094(17) 0.0380(19) 0.0141(15) O2 0.0344(16) 0.0339(17) 0.0400(18) -0.0109(14) 0.0243(15) -0.0055(13) O3 0.058(2) 0.046(2) 0.068(2) 0.0017(18) 0.051(2) 0.0028(17) F1 0.0415(17) 0.072(2) 0.080(2) -0.0148(19) 0.0319(17) -0.0239(16) F2 0.0479(17) 0.0405(16) 0.0540(18) -0.0139(14) 0.0276(15) -0.0062(13) F3 0.075(2) 0.0245(15) 0.067(2) 0.0023(15) 0.0282(18) -0.0011(15) C34 0.036(3) 0.034(3) 0.050(3) -0.001(2) 0.022(2) -0.005(2) S2A 0.0321(18) 0.090(3) 0.048(2) 0.040(2) 0.0089(18) 0.014(2) O4A 0.087(12) 0.100(14) 0.090(13) 0.023(11) -0.030(9) 0.009(10) O5A 0.0321(18) 0.090(3) 0.048(2) 0.040(2) 0.0089(18) 0.014(2) O6A 0.065(8) 0.093(11) 0.049(6) 0.041(7) 0.031(6) 0.049(8) F4A 0.071(6) 0.085(7) 0.084(7) 0.011(6) 0.061(6) -0.002(6) F5A 0.035(5) 0.092(7) 0.033(5) 0.010(5) 0.012(4) 0.013(4) F6A 0.160(10) 0.110(8) 0.072(6) 0.001(6) 0.066(7) 0.085(8) C35A 0.160(10) 0.110(8) 0.072(6) 0.001(6) 0.066(7) 0.085(8) N7A 0.105(15) 0.007(6) 0.058(10) 0.000 0.054(9) 0.000 C36A 0.080(8) 0.052(6) 0.086(9) 0.000 0.061(7) 0.000 C37A 0.080(8) 0.052(6) 0.086(9) 0.000 0.061(7) 0.000 _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 Fe1 N3 2.155(4) . ? Fe1 N1 2.182(3) . ? Fe1 N2 2.188(3) . ? Fe1 N5 2.188(3) . ? Fe1 N4 2.237(3) . ? Fe1 N6 2.243(2) . ? N1 C1 1.338(6) . ? N1 C5 1.350(5) . ? N2 C10 1.350(5) . ? N2 C6 1.358(5) . ? N3 C12 1.348(6) . ? N3 C16 1.358(5) . ? N4 C21 1.352(5) . ? N4 C17 1.353(5) . ? N5 C33 1.342(5) . ? N5 C29 1.353(6) . ? C1 C2 1.387(7) . ? C1 H1 0.9500 . ? C2 C3 1.376(7) . ? C2 H2 0.9500 . ? C3 C4 1.372(6) . ? C3 H3 0.9500 . ? C4 C5 1.394(6) . ? C4 H4 0.9500 . ? C5 C6 1.476(5) . ? C6 C7 1.382(6) . ? C7 C8 1.373(6) . ? C7 H7 0.9500 . ? C8 C9 1.386(6) . ? C8 H8 0.9500 . ? C9 C10 1.382(6) . ? C9 H9 0.9500 . ? C10 C11 1.440(5) . ? C11 C11 1.193(8) 2 ? C12 C13 1.380(7) . ? C12 H12 0.9500 . ? C13 C14 1.372(7) . ? C13 H13 0.9500 . ? C14 C15 1.388(7) . ? C14 H14 0.9500 . ? C15 C16 1.382(6) . ? C15 H15 0.9500 . ? C16 C17 1.480(6) . ? C17 C18 1.400(6) . ? C18 C19 1.363(7) . ? C18 H18 0.9500 . ? C19 C20 1.379(7) . ? C19 H19 0.9500 . ? C20 C21 1.389(6) . ? C20 H20 0.9500 . ? C21 C22 1.435(6) . ? C22 C23 1.195(6) . ? C23 C24 1.386(10) 2 ? N6 C24 1.3900 . ? N6 C28 1.3900 . ? C24 C23 1.386(5) 2 ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C25 H25 0.9500 . ? C26 C27 1.3900 . ? C26 H26 0.9500 . ? C27 C28 1.3900 . ? C27 H27 0.9500 . ? C28 C29 1.438(5) . ? C29 C30 1.382(6) . ? C30 C31 1.368(7) . ? C30 H30 0.9500 . ? C31 C32 1.373(7) . ? C31 H31 0.9500 . ? C32 C33 1.385(6) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? S1 O1 1.440(3) . ? S1 O3 1.443(3) . ? S1 O2 1.444(3) . ? S1 C34 1.818(5) . ? F1 C34 1.328(5) . ? F2 C34 1.337(5) . ? F3 C34 1.329(5) . ? S2A O5A 1.385(11) . ? S2A O6A 1.422(10) . ? S2A O4A 1.462(13) . ? S2A C35A 1.847(13) . ? F4A C35A 1.336(15) . ? F5A C35A 1.342(14) . ? F6A C35A 1.297(13) . ? S2B O6B 1.389(12) . ? S2B O4B 1.437(13) . ? S2B O5B 1.462(13) . ? S2B C35B 1.817(14) . ? F4B C35B 1.316(15) . ? F5B C35B 1.346(15) . ? F6B C35B 1.334(15) . ? S2C O5C 1.407(12) . ? S2C O6C 1.421(12) . ? S2C O4C 1.420(12) . ? S2C C35C 1.827(15) . ? F4C C35C 1.320(16) . ? F5C C35C 1.349(16) . ? F6C C35C 1.338(16) . ? S2D O5D 1.430(15) . ? S2D O6D 1.441(15) . ? S2D O4D 1.436(16) . ? S2D C35D 1.849(16) . ? F4D C35D 1.336(18) . ? F5D C35D 1.337(17) . ? F6D C35D 1.308(18) . ? N7A C36A 1.17(2) . ? C36A C37A 1.44(2) . ? C37A H37A 0.9800 . ? C37A H37B 0.9800 . ? C37A H37C 0.9800 . ? N7B C36B 1.083(19) . ? C36B C37B 1.58(3) . ? C37B H37B 0.9911 . ? C37B H37D 0.9800 . ? C37B H37E 0.9800 . ? C37B H37F 0.9800 . ? 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 N3 Fe1 N1 94.01(14) . . ? N3 Fe1 N2 88.59(13) . . ? N1 Fe1 N2 75.46(13) . . ? N3 Fe1 N5 93.84(14) . . ? N1 Fe1 N5 91.24(13) . . ? N2 Fe1 N5 166.63(12) . . ? N3 Fe1 N4 74.86(13) . . ? N1 Fe1 N4 166.30(13) . . ? N2 Fe1 N4 111.55(12) . . ? N5 Fe1 N4 81.74(12) . . ? N3 Fe1 N6 169.26(13) . . ? N1 Fe1 N6 88.26(13) . . ? N2 Fe1 N6 102.13(11) . . ? N5 Fe1 N6 75.60(12) . . ? N4 Fe1 N6 101.24(12) . . ? C1 N1 C5 119.0(4) . . ? C1 N1 Fe1 124.9(3) . . ? C5 N1 Fe1 116.0(3) . . ? C10 N2 C6 117.1(3) . . ? C10 N2 Fe1 126.9(3) . . ? C6 N2 Fe1 115.8(3) . . ? C12 N3 C16 117.8(4) . . ? C12 N3 Fe1 125.0(3) . . ? C16 N3 Fe1 117.2(3) . . ? C21 N4 C17 116.6(4) . . ? C21 N4 Fe1 127.2(3) . . ? C17 N4 Fe1 112.5(3) . . ? C33 N5 C29 117.8(4) . . ? C33 N5 Fe1 125.0(3) . . ? C29 N5 Fe1 115.1(3) . . ? N1 C1 C2 122.5(4) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 118.5(4) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C4 C3 C2 119.5(4) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 120.8(4) . . ? N1 C5 C6 116.5(3) . . ? C4 C5 C6 122.7(4) . . ? N2 C6 C7 122.2(4) . . ? N2 C6 C5 115.9(3) . . ? C7 C6 C5 121.9(4) . . ? C8 C7 C6 119.8(4) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 118.8(4) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 118.6(4) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? N2 C10 C9 123.4(4) . . ? N2 C10 C11 118.1(3) . . ? C9 C10 C11 118.3(4) . . ? C11 C11 C10 171.7(5) 2 . ? N3 C12 C13 122.9(5) . . ? N3 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C14 C13 C12 118.8(5) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 119.5(5) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 118.9(5) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? N3 C16 C15 122.0(4) . . ? N3 C16 C17 115.0(4) . . ? C15 C16 C17 123.0(4) . . ? N4 C17 C18 122.7(4) . . ? N4 C17 C16 116.3(4) . . ? C18 C17 C16 121.0(4) . . ? C19 C18 C17 119.2(5) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 119.3(5) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C19 C20 C21 118.8(4) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? N4 C21 C20 123.3(4) . . ? N4 C21 C22 118.2(4) . . ? C20 C21 C22 118.5(4) . . ? C23 C22 C21 172.3(5) . . ? C22 C23 C24 170.1(5) . 2 ? C24 N6 C28 120.0 . . ? C24 N6 Fe1 126.20(15) . . ? C28 N6 Fe1 111.9(3) . . ? C23 C24 N6 119.4(3) 2 . ? C23 C24 C25 119.8(3) 2 . ? N6 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.0 . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 N6 120.0 . . ? C27 C28 C29 123.2(3) . . ? N6 C28 C29 116.7(3) . . ? N5 C29 C30 122.0(4) . . ? N5 C29 C28 116.4(4) . . ? C30 C29 C28 121.6(4) . . ? C31 C30 C29 119.2(5) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C30 C31 C32 119.7(5) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C31 C32 C33 118.5(4) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? N5 C33 C32 122.7(4) . . ? N5 C33 H33 118.7 . . ? C32 C33 H33 118.7 . . ? O1 S1 O3 115.4(2) . . ? O1 S1 O2 115.01(19) . . ? O3 S1 O2 114.3(2) . . ? O1 S1 C34 102.5(2) . . ? O3 S1 C34 104.2(2) . . ? O2 S1 C34 103.2(2) . . ? F1 C34 F3 107.7(4) . . ? F1 C34 F2 107.6(4) . . ? F3 C34 F2 107.3(4) . . ? F1 C34 S1 111.1(3) . . ? F3 C34 S1 111.8(3) . . ? F2 C34 S1 111.1(3) . . ? O5A S2A O6A 114.6(7) . . ? O5A S2A O4A 113.5(11) . . ? O6A S2A O4A 114.8(10) . . ? O5A S2A C35A 107.8(8) . . ? O6A S2A C35A 105.1(8) . . ? O4A S2A C35A 99.1(8) . . ? F6A C35A F4A 110.5(14) . . ? F6A C35A F5A 107.2(12) . . ? F4A C35A F5A 104.8(11) . . ? F6A C35A S2A 113.0(10) . . ? F4A C35A S2A 109.1(10) . . ? F5A C35A S2A 111.9(10) . . ? O6B S2B O4B 116.8(11) . . ? O6B S2B O5B 118.0(11) . . ? O4B S2B O5B 108.5(11) . . ? O6B S2B C35B 104.5(9) . . ? O4B S2B C35B 104.8(10) . . ? O5B S2B C35B 102.2(9) . . ? F4B C35B F6B 105.1(14) . . ? F4B C35B F5B 110.2(14) . . ? F6B C35B F5B 105.1(14) . . ? F4B C35B S2B 113.3(12) . . ? F6B C35B S2B 111.6(12) . . ? F5B C35B S2B 111.1(12) . . ? O5C S2C O6C 111.9(9) . . ? O5C S2C O4C 116.1(9) . . ? O6C S2C O4C 117.8(9) . . ? O5C S2C C35C 105.0(9) . . ? O6C S2C C35C 101.2(9) . . ? O4C S2C C35C 102.2(9) . . ? F4C C35C F6C 103.9(15) . . ? F4C C35C F5C 109.0(16) . . ? F6C C35C F5C 110.7(16) . . ? F4C C35C S2C 111.9(14) . . ? F6C C35C S2C 112.4(13) . . ? F5C C35C S2C 108.7(14) . . ? O5D S2D O6D 114.4(17) . . ? O5D S2D O4D 122.0(18) . . ? O6D S2D O4D 113.9(19) . . ? O5D S2D C35D 107.9(14) . . ? O6D S2D C35D 97.7(16) . . ? O4D S2D C35D 95.6(15) . . ? F6D C35D F4D 103(2) . . ? F6D C35D F5D 113(2) . . ? F4D C35D F5D 103(2) . . ? F6D C35D S2D 111.4(18) . . ? F4D C35D S2D 113.9(19) . . ? F5D C35D S2D 111.6(19) . . ? N7A C36A C37A 180.000(6) . . ? C36A C37A H37A 109.5 . . ? C36A C37A H37B 109.5 . . ? H37A C37A H37B 109.5 . . ? C36A C37A H37C 109.5 . . ? H37A C37A H37C 109.5 . . ? H37B C37A H37C 109.5 . . ? N7B C36B C37B 166(3) . . ? C36B C37B H37B 127.5 . . ? 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 N3 Fe1 N1 C1 95.6(4) . . . . ? N2 Fe1 N1 C1 -176.9(4) . . . . ? N5 Fe1 N1 C1 1.7(4) . . . . ? N4 Fe1 N1 C1 60.5(8) . . . . ? N6 Fe1 N1 C1 -73.9(4) . . . . ? N3 Fe1 N1 C5 -88.3(3) . . . . ? N2 Fe1 N1 C5 -0.8(3) . . . . ? N5 Fe1 N1 C5 177.7(3) . . . . ? N4 Fe1 N1 C5 -123.5(5) . . . . ? N6 Fe1 N1 C5 102.2(3) . . . . ? N3 Fe1 N2 C10 -82.6(3) . . . . ? N1 Fe1 N2 C10 -177.1(3) . . . . ? N5 Fe1 N2 C10 176.7(5) . . . . ? N4 Fe1 N2 C10 -9.5(3) . . . . ? N6 Fe1 N2 C10 98.0(3) . . . . ? N3 Fe1 N2 C6 91.5(3) . . . . ? N1 Fe1 N2 C6 -3.0(3) . . . . ? N5 Fe1 N2 C6 -9.3(7) . . . . ? N4 Fe1 N2 C6 164.6(3) . . . . ? N6 Fe1 N2 C6 -88.0(3) . . . . ? N1 Fe1 N3 C12 17.4(4) . . . . ? N2 Fe1 N3 C12 -58.0(4) . . . . ? N5 Fe1 N3 C12 108.9(4) . . . . ? N4 Fe1 N3 C12 -170.8(4) . . . . ? N6 Fe1 N3 C12 119.3(7) . . . . ? N1 Fe1 N3 C16 -161.7(3) . . . . ? N2 Fe1 N3 C16 123.0(3) . . . . ? N5 Fe1 N3 C16 -70.2(3) . . . . ? N4 Fe1 N3 C16 10.2(3) . . . . ? N6 Fe1 N3 C16 -59.7(8) . . . . ? N3 Fe1 N4 C21 -175.0(3) . . . . ? N1 Fe1 N4 C21 -138.5(5) . . . . ? N2 Fe1 N4 C21 102.7(3) . . . . ? N5 Fe1 N4 C21 -78.7(3) . . . . ? N6 Fe1 N4 C21 -5.3(3) . . . . ? N3 Fe1 N4 C17 -17.5(3) . . . . ? N1 Fe1 N4 C17 19.0(7) . . . . ? N2 Fe1 N4 C17 -99.8(3) . . . . ? N5 Fe1 N4 C17 78.8(3) . . . . ? N6 Fe1 N4 C17 152.3(3) . . . . ? N3 Fe1 N5 C33 8.0(3) . . . . ? N1 Fe1 N5 C33 102.1(3) . . . . ? N2 Fe1 N5 C33 108.2(6) . . . . ? N4 Fe1 N5 C33 -66.1(3) . . . . ? N6 Fe1 N5 C33 -170.0(3) . . . . ? N3 Fe1 N5 C29 171.1(3) . . . . ? N1 Fe1 N5 C29 -94.8(3) . . . . ? N2 Fe1 N5 C29 -88.8(6) . . . . ? N4 Fe1 N5 C29 97.0(3) . . . . ? N6 Fe1 N5 C29 -6.9(3) . . . . ? C5 N1 C1 C2 -0.2(8) . . . . ? Fe1 N1 C1 C2 175.7(4) . . . . ? N1 C1 C2 C3 -0.3(9) . . . . ? C1 C2 C3 C4 0.7(8) . . . . ? C2 C3 C4 C5 -0.6(7) . . . . ? C1 N1 C5 C4 0.3(7) . . . . ? Fe1 N1 C5 C4 -176.0(3) . . . . ? C1 N1 C5 C6 -179.4(4) . . . . ? Fe1 N1 C5 C6 4.3(5) . . . . ? C3 C4 C5 N1 0.1(7) . . . . ? C3 C4 C5 C6 179.8(4) . . . . ? C10 N2 C6 C7 -0.3(5) . . . . ? Fe1 N2 C6 C7 -175.0(3) . . . . ? C10 N2 C6 C5 -179.1(3) . . . . ? Fe1 N2 C6 C5 6.2(4) . . . . ? N1 C5 C6 N2 -7.0(5) . . . . ? C4 C5 C6 N2 173.3(4) . . . . ? N1 C5 C6 C7 174.1(4) . . . . ? C4 C5 C6 C7 -5.6(6) . . . . ? N2 C6 C7 C8 0.8(6) . . . . ? C5 C6 C7 C8 179.5(4) . . . . ? C6 C7 C8 C9 0.5(6) . . . . ? C7 C8 C9 C10 -2.2(6) . . . . ? C6 N2 C10 C9 -1.5(5) . . . . ? Fe1 N2 C10 C9 172.5(3) . . . . ? C6 N2 C10 C11 173.9(3) . . . . ? Fe1 N2 C10 C11 -12.1(5) . . . . ? C8 C9 C10 N2 2.8(6) . . . . ? C8 C9 C10 C11 -172.7(4) . . . . ? C16 N3 C12 C13 1.3(7) . . . . ? Fe1 N3 C12 C13 -177.8(4) . . . . ? N3 C12 C13 C14 0.3(9) . . . . ? C12 C13 C14 C15 -1.9(9) . . . . ? C13 C14 C15 C16 2.0(8) . . . . ? C12 N3 C16 C15 -1.2(7) . . . . ? Fe1 N3 C16 C15 177.9(3) . . . . ? C12 N3 C16 C17 178.9(4) . . . . ? Fe1 N3 C16 C17 -2.0(5) . . . . ? C14 C15 C16 N3 -0.4(7) . . . . ? C14 C15 C16 C17 179.5(4) . . . . ? C21 N4 C17 C18 3.6(6) . . . . ? Fe1 N4 C17 C18 -156.5(3) . . . . ? C21 N4 C17 C16 -177.4(3) . . . . ? Fe1 N4 C17 C16 22.5(4) . . . . ? N3 C16 C17 N4 -14.3(5) . . . . ? C15 C16 C17 N4 165.8(4) . . . . ? N3 C16 C17 C18 164.7(4) . . . . ? C15 C16 C17 C18 -15.2(7) . . . . ? N4 C17 C18 C19 -0.9(7) . . . . ? C16 C17 C18 C19 -179.8(4) . . . . ? C17 C18 C19 C20 -1.8(7) . . . . ? C18 C19 C20 C21 1.7(7) . . . . ? C17 N4 C21 C20 -3.8(6) . . . . ? Fe1 N4 C21 C20 153.0(3) . . . . ? C17 N4 C21 C22 175.0(4) . . . . ? Fe1 N4 C21 C22 -28.3(5) . . . . ? C19 C20 C21 N4 1.2(6) . . . . ? C19 C20 C21 C22 -177.5(4) . . . . ? N3 Fe1 N6 C24 179.5(6) . . . . ? N1 Fe1 N6 C24 -78.1(2) . . . . ? N2 Fe1 N6 C24 -3.3(2) . . . . ? N5 Fe1 N6 C24 -169.8(2) . . . . ? N4 Fe1 N6 C24 111.9(2) . . . . ? N3 Fe1 N6 C28 -16.6(7) . . . . ? N1 Fe1 N6 C28 85.90(19) . . . . ? N2 Fe1 N6 C28 160.63(18) . . . . ? N5 Fe1 N6 C28 -5.83(18) . . . . ? N4 Fe1 N6 C28 -84.17(19) . . . . ? C28 N6 C24 C23 169.9(4) . . . 2 ? Fe1 N6 C24 C23 -27.3(4) . . . 2 ? C28 N6 C24 C25 0.0 . . . . ? Fe1 N6 C24 C25 162.8(3) . . . . ? C23 C24 C25 C26 -169.9(4) 2 . . . ? N6 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 N6 0.0 . . . . ? C26 C27 C28 C29 177.2(4) . . . . ? C24 N6 C28 C27 0.0 . . . . ? Fe1 N6 C28 C27 -165.1(2) . . . . ? C24 N6 C28 C29 -177.4(4) . . . . ? Fe1 N6 C28 C29 17.6(3) . . . . ? C33 N5 C29 C30 3.3(6) . . . . ? Fe1 N5 C29 C30 -161.1(3) . . . . ? C33 N5 C29 C28 -176.9(3) . . . . ? Fe1 N5 C29 C28 18.7(5) . . . . ? C27 C28 C29 N5 158.0(3) . . . . ? N6 C28 C29 N5 -24.8(5) . . . . ? C27 C28 C29 C30 -22.2(6) . . . . ? N6 C28 C29 C30 155.0(4) . . . . ? N5 C29 C30 C31 -0.5(7) . . . . ? C28 C29 C30 C31 179.8(4) . . . . ? C29 C30 C31 C32 -2.5(7) . . . . ? C30 C31 C32 C33 2.5(7) . . . . ? C29 N5 C33 C32 -3.2(6) . . . . ? Fe1 N5 C33 C32 159.4(3) . . . . ? C31 C32 C33 N5 0.4(7) . . . . ? O1 S1 C34 F1 -59.3(4) . . . . ? O3 S1 C34 F1 61.2(4) . . . . ? O2 S1 C34 F1 -179.1(3) . . . . ? O1 S1 C34 F3 -179.7(3) . . . . ? O3 S1 C34 F3 -59.1(4) . . . . ? O2 S1 C34 F3 60.6(4) . . . . ? O1 S1 C34 F2 60.5(4) . . . . ? O3 S1 C34 F2 -179.0(3) . . . . ? O2 S1 C34 F2 -59.3(4) . . . . ? O5A S2A C35A F6A -57.7(15) . . . . ? O6A S2A C35A F6A 65.0(14) . . . . ? O4A S2A C35A F6A -176.1(14) . . . . ? O5A S2A C35A F4A 178.9(11) . . . . ? O6A S2A C35A F4A -58.4(11) . . . . ? O4A S2A C35A F4A 60.5(13) . . . . ? O5A S2A C35A F5A 63.4(12) . . . . ? O6A S2A C35A F5A -173.9(10) . . . . ? O4A S2A C35A F5A -54.9(13) . . . . ? O6B S2B C35B F4B -56.3(16) . . . . ? O4B S2B C35B F4B 67.1(16) . . . . ? O5B S2B C35B F4B -179.8(14) . . . . ? O6B S2B C35B F6B 62.1(15) . . . . ? O4B S2B C35B F6B -174.5(14) . . . . ? O5B S2B C35B F6B -61.4(15) . . . . ? O6B S2B C35B F5B 179.1(13) . . . . ? O4B S2B C35B F5B -57.5(15) . . . . ? O5B S2B C35B F5B 55.5(15) . . . . ? O5C S2C C35C F4C -178.7(14) . . . . ? O6C S2C C35C F4C -62.3(16) . . . . ? O4C S2C C35C F4C 59.7(16) . . . . ? O5C S2C C35C F6C -62.2(16) . . . . ? O6C S2C C35C F6C 54.3(16) . . . . ? O4C S2C C35C F6C 176.3(14) . . . . ? O5C S2C C35C F5C 60.8(16) . . . . ? O6C S2C C35C F5C 177.3(14) . . . . ? O4C S2C C35C F5C -60.8(16) . . . . ? O5D S2D C35D F6D -59(3) . . . . ? O6D S2D C35D F6D 60(3) . . . . ? O4D S2D C35D F6D 175(3) . . . . ? O5D S2D C35D F4D -174(2) . . . . ? O6D S2D C35D F4D -56(3) . . . . ? O4D S2D C35D F4D 59(3) . . . . ? O5D S2D C35D F5D 69(3) . . . . ? O6D S2D C35D F5D -172(3) . . . . ? O4D S2D C35D F5D -57(3) . . . . ? _diffrn_measured_fraction_theta_max .994 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full .994 _refine_diff_density_max 1.177 _refine_diff_density_min -.726 _refine_diff_density_rms .082 # Attachment 'Cmpd_5-756145R2.cif' data_n239 _database_code_depnum_ccdc_archive 'CCDC 756145' #TrackingRef 'Cmpd_5-756145R2.cif' # Structure solved and refined by Yael Diskin-Posner _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H42 Mn2 N12, 1.65(C4 H10 O), 1.7(C2 H3 N), 4(Cl O4)' _chemical_formula_sum 'C76 H63.60 Cl4 Mn2 N13.70 O17.65' _chemical_formula_weight 1702.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn .3368 .7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.8924(4) _cell_length_b 20.5718(7) _cell_length_c 28.9422(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.5220(10) _cell_angle_gamma 90.00 _cell_volume 7547.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 90854 _cell_measurement_theta_min 2.3645 _cell_measurement_theta_max 33.120 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3499 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7523 _exptl_absorpt_correction_T_max 0.8432 _exptl_absorpt_process_details 'SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX II Kappa CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 89382 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 33.30 _reflns_number_total 28961 _reflns_number_gt 20570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2' _computing_cell_refinement 'APEX 2' _computing_data_reduction 'APEX 2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0735P)^2^+4.9127P] 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 28961 _refine_ls_number_parameters 1052 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1534 _refine_ls_wR_factor_gt 0.1376 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.09136(2) 0.278259(13) 0.468880(9) 0.01352(6) Uani 1 1 d . . . Mn2 Mn 0.22399(2) 0.292396(13) 0.282312(9) 0.01435(6) Uani 1 1 d . . . N1 N 0.01958(13) 0.36396(8) 0.50004(5) 0.0172(3) Uani 1 1 d . . . N2 N -0.03970(12) 0.32029(8) 0.41231(5) 0.0158(3) Uani 1 1 d . . . C1 C 0.05560(16) 0.38533(10) 0.54375(7) 0.0213(4) Uani 1 1 d . . . H1 H 0.1164 0.3654 0.5616 0.026 Uiso 1 1 calc R . . C2 C 0.00734(17) 0.43556(10) 0.56386(7) 0.0238(4) Uani 1 1 d . . . H2 H 0.0351 0.4501 0.5948 0.029 Uiso 1 1 calc R . . C3 C -0.08142(17) 0.46387(10) 0.53812(8) 0.0255(4) Uani 1 1 d . . . H3 H -0.1170 0.4975 0.5515 0.031 Uiso 1 1 calc R . . C4 C -0.11846(16) 0.44303(10) 0.49262(8) 0.0225(4) Uani 1 1 d . . . H4 H -0.1792 0.4624 0.4742 0.027 Uiso 1 1 calc R . . C5 C -0.06524(14) 0.39314(9) 0.47423(7) 0.0174(3) Uani 1 1 d . . . C6 C -0.09843(14) 0.36857(9) 0.42554(6) 0.0178(3) Uani 1 1 d . . . C7 C -0.18475(16) 0.39454(11) 0.39515(7) 0.0255(4) Uani 1 1 d . . . H7 H -0.2234 0.4295 0.4051 0.031 Uiso 1 1 calc R . . C8 C -0.21396(17) 0.36926(13) 0.35037(8) 0.0312(5) Uani 1 1 d . . . H8 H -0.2727 0.3865 0.3293 0.037 Uiso 1 1 calc R . . C9 C -0.15627(17) 0.31855(12) 0.33684(7) 0.0267(4) Uani 1 1 d . . . H9 H -0.1758 0.2993 0.3067 0.032 Uiso 1 1 calc R . . C10 C -0.06847(15) 0.29613(10) 0.36845(6) 0.0187(3) Uani 1 1 d . . . C11 C -0.00016(15) 0.24787(10) 0.35448(6) 0.0195(3) Uani 1 1 d . . . C12 C 0.05992(15) 0.21131(9) 0.34112(6) 0.0188(3) Uani 1 1 d . . . C13 C 0.13196(15) 0.16472(9) 0.32821(6) 0.0180(3) Uani 1 1 d . . . C14 C 0.12239(17) 0.09952(10) 0.33940(7) 0.0235(4) Uani 1 1 d . . . H14 H 0.0677 0.0853 0.3550 0.028 Uiso 1 1 calc R . . C15 C 0.19450(19) 0.05586(10) 0.32729(8) 0.0270(4) Uani 1 1 d . . . H15 H 0.1902 0.0110 0.3345 0.032 Uiso 1 1 calc R . . C16 C 0.27284(18) 0.07817(10) 0.30455(7) 0.0241(4) Uani 1 1 d . . . H16 H 0.3224 0.0487 0.2956 0.029 Uiso 1 1 calc R . . C17 C 0.27842(15) 0.14426(9) 0.29486(6) 0.0186(3) Uani 1 1 d . . . C18 C 0.36152(16) 0.17063(9) 0.27076(7) 0.0204(3) Uani 1 1 d . . . C19 C 0.44516(19) 0.13289(11) 0.26222(9) 0.0323(5) Uani 1 1 d . . . H19 H 0.4515 0.0889 0.2724 0.039 Uiso 1 1 calc R . . C20 C 0.5193(2) 0.15980(13) 0.23880(10) 0.0385(6) Uani 1 1 d . . . H20 H 0.5769 0.1346 0.2325 0.046 Uiso 1 1 calc R . . C21 C 0.50826(19) 0.22399(12) 0.22469(10) 0.0361(5) Uani 1 1 d . . . H21 H 0.5576 0.2437 0.2084 0.043 Uiso 1 1 calc R . . C22 C 0.42328(18) 0.25891(11) 0.23497(9) 0.0288(4) Uani 1 1 d . . . H22 H 0.4161 0.3032 0.2255 0.035 Uiso 1 1 calc R . . N3 N 0.35094(13) 0.23348(8) 0.25747(6) 0.0203(3) Uani 1 1 d . . . N4 N 0.20932(12) 0.18753(8) 0.30641(5) 0.0161(3) Uani 1 1 d . . . N5 N -0.02874(13) 0.20436(8) 0.47910(6) 0.0183(3) Uani 1 1 d . . . N6 N 0.15145(12) 0.17903(7) 0.44702(5) 0.0154(3) Uani 1 1 d . . . C23 C -0.12475(16) 0.22008(10) 0.48732(7) 0.0231(4) Uani 1 1 d . . . H23 H -0.1369 0.2633 0.4966 0.028 Uiso 1 1 calc R . . C24 C -0.20646(17) 0.17596(11) 0.48286(8) 0.0283(4) Uani 1 1 d . . . H24 H -0.2733 0.1886 0.4892 0.034 Uiso 1 1 calc R . . C25 C -0.18974(18) 0.11304(12) 0.46897(9) 0.0309(5) Uani 1 1 d . . . H25 H -0.2452 0.0820 0.4652 0.037 Uiso 1 1 calc R . . C26 C -0.09079(17) 0.09602(10) 0.46066(8) 0.0261(4) Uani 1 1 d . . . H26 H -0.0773 0.0532 0.4510 0.031 Uiso 1 1 calc R . . C27 C -0.01175(15) 0.14273(9) 0.46669(7) 0.0185(3) Uani 1 1 d . . . C28 C 0.09707(15) 0.12841(9) 0.45974(6) 0.0175(3) Uani 1 1 d . . . C29 C 0.14025(17) 0.06613(10) 0.46703(8) 0.0236(4) Uani 1 1 d . . . H29 H 0.0993 0.0311 0.4754 0.028 Uiso 1 1 calc R . . C30 C 0.24351(18) 0.05645(10) 0.46189(8) 0.0278(4) Uani 1 1 d . . . H30 H 0.2755 0.0150 0.4681 0.033 Uiso 1 1 calc R . . C31 C 0.30013(17) 0.10760(10) 0.44766(8) 0.0247(4) Uani 1 1 d . . . H31 H 0.3711 0.1019 0.4438 0.030 Uiso 1 1 calc R . . C32 C 0.25039(15) 0.16751(9) 0.43922(6) 0.0170(3) Uani 1 1 d . . . C33 C 0.30086(14) 0.21966(9) 0.41876(6) 0.0176(3) Uani 1 1 d . . . C34 C 0.33961(14) 0.26064(9) 0.39790(6) 0.0174(3) Uani 1 1 d . . . C35 C 0.39382(14) 0.31351(9) 0.38058(6) 0.0176(3) Uani 1 1 d . . . C36 C 0.48188(16) 0.33898(11) 0.40995(7) 0.0244(4) Uani 1 1 d . . . H36 H 0.5067 0.3206 0.4400 0.029 Uiso 1 1 calc R . . C37 C 0.53231(17) 0.39157(12) 0.39435(8) 0.0285(4) Uani 1 1 d . . . H37 H 0.5927 0.4100 0.4137 0.034 Uiso 1 1 calc R . . C38 C 0.49430(16) 0.41719(11) 0.35051(7) 0.0246(4) Uani 1 1 d . . . H38 H 0.5284 0.4533 0.3392 0.030 Uiso 1 1 calc R . . C39 C 0.40505(14) 0.38948(9) 0.32285(6) 0.0175(3) Uani 1 1 d . . . C40 C 0.35810(15) 0.41741(9) 0.27630(6) 0.0175(3) Uani 1 1 d . . . C41 C 0.39666(17) 0.47389(10) 0.25912(7) 0.0239(4) Uani 1 1 d . . . H41 H 0.4570 0.4951 0.2763 0.029 Uiso 1 1 calc R . . C42 C 0.34537(18) 0.49864(11) 0.21642(7) 0.0270(4) Uani 1 1 d . . . H42 H 0.3699 0.5374 0.2041 0.032 Uiso 1 1 calc R . . C43 C 0.25825(17) 0.46647(10) 0.19194(7) 0.0242(4) Uani 1 1 d . . . H43 H 0.2215 0.4829 0.1628 0.029 Uiso 1 1 calc R . . C44 C 0.22583(16) 0.40984(10) 0.21082(7) 0.0210(4) Uani 1 1 d . . . H44 H 0.1663 0.3875 0.1939 0.025 Uiso 1 1 calc R . . N7 N 0.27473(12) 0.38513(8) 0.25194(5) 0.0171(3) Uani 1 1 d . . . N8 N 0.35532(12) 0.33789(8) 0.33756(5) 0.0161(3) Uani 1 1 d . . . N9 N 0.19545(13) 0.25161(8) 0.53846(5) 0.0172(3) Uani 1 1 d . . . N10 N 0.23997(12) 0.34056(7) 0.47558(5) 0.0139(3) Uani 1 1 d . . . C45 C 0.17807(17) 0.20065(10) 0.56496(7) 0.0223(4) Uani 1 1 d . . . H45 H 0.1092 0.1825 0.5606 0.027 Uiso 1 1 calc R . . C46 C 0.25657(19) 0.17349(11) 0.59848(7) 0.0280(4) Uani 1 1 d . . . H46 H 0.2416 0.1376 0.6169 0.034 Uiso 1 1 calc R . . C47 C 0.35684(19) 0.19950(12) 0.60473(8) 0.0296(5) Uani 1 1 d . . . H47 H 0.4123 0.1809 0.6269 0.036 Uiso 1 1 calc R . . C48 C 0.37584(17) 0.25292(11) 0.57835(7) 0.0240(4) Uani 1 1 d . . . H48 H 0.4440 0.2720 0.5824 0.029 Uiso 1 1 calc R . . C49 C 0.29286(15) 0.27789(9) 0.54596(6) 0.0167(3) Uani 1 1 d . . . C50 C 0.30569(14) 0.33586(9) 0.51724(6) 0.0157(3) Uani 1 1 d . . . C51 C 0.37949(15) 0.38372(10) 0.53385(7) 0.0210(4) Uani 1 1 d . . . H51 H 0.4248 0.3788 0.5634 0.025 Uiso 1 1 calc R . . C52 C 0.38605(16) 0.43837(10) 0.50685(7) 0.0228(4) Uani 1 1 d . . . H52 H 0.4337 0.4724 0.5182 0.027 Uiso 1 1 calc R . . C53 C 0.32218(15) 0.44283(9) 0.46296(7) 0.0199(3) Uani 1 1 d . . . H53 H 0.3267 0.4793 0.4433 0.024 Uiso 1 1 calc R . . C54 C 0.25115(14) 0.39265(9) 0.44830(6) 0.0148(3) Uani 1 1 d . . . C55 C 0.18630(14) 0.39501(9) 0.40265(6) 0.0157(3) Uani 1 1 d . . . C56 C 0.13676(15) 0.39785(9) 0.36334(6) 0.0168(3) Uani 1 1 d . . . C57 C 0.06670(15) 0.40102(9) 0.31883(6) 0.0169(3) Uani 1 1 d . . . C58 C -0.00860(17) 0.44980(10) 0.31034(7) 0.0230(4) Uani 1 1 d . . . H58 H -0.0103 0.4832 0.3329 0.028 Uiso 1 1 calc R . . C59 C -0.08093(18) 0.44931(11) 0.26887(7) 0.0264(4) Uani 1 1 d . . . H59 H -0.1324 0.4827 0.2621 0.032 Uiso 1 1 calc R . . C60 C -0.07700(16) 0.39894(11) 0.23727(7) 0.0232(4) Uani 1 1 d . . . H60 H -0.1265 0.3971 0.2086 0.028 Uiso 1 1 calc R . . C61 C 0.00018(14) 0.35127(9) 0.24803(6) 0.0167(3) Uani 1 1 d . . . C62 C 0.00558(15) 0.29521(9) 0.21628(6) 0.0179(3) Uani 1 1 d . . . C63 C -0.08307(17) 0.27314(11) 0.18577(7) 0.0265(4) Uani 1 1 d . . . H63 H -0.1498 0.2931 0.1850 0.032 Uiso 1 1 calc R . . C64 C -0.0723(2) 0.22132(13) 0.15634(8) 0.0339(5) Uani 1 1 d . . . H64 H -0.1316 0.2052 0.1351 0.041 Uiso 1 1 calc R . . C65 C 0.0255(2) 0.19377(12) 0.15848(8) 0.0318(5) Uani 1 1 d . . . H65 H 0.0349 0.1589 0.1381 0.038 Uiso 1 1 calc R . . C66 C 0.11028(18) 0.21726(10) 0.19057(7) 0.0248(4) Uani 1 1 d . . . H66 H 0.1774 0.1975 0.1922 0.030 Uiso 1 1 calc R . . N11 N 0.10056(13) 0.26712(8) 0.21946(5) 0.0184(3) Uani 1 1 d . . . N12 N 0.07378(12) 0.35258(7) 0.28770(5) 0.0148(3) Uani 1 1 d . . . Cl1 Cl -0.01245(4) 0.06899(2) 0.605161(17) 0.02351(9) Uani 1 1 d D . . O1 O -0.12455(16) 0.06921(12) 0.59389(11) 0.0669(8) Uani 1 1 d D . . O2 O 0.02727(16) 0.12827(9) 0.62775(6) 0.0395(4) Uani 1 1 d D . . O3 O 0.0307(2) 0.06145(10) 0.56357(8) 0.0578(7) Uani 1 1 d D . . O4 O 0.01986(19) 0.01527(12) 0.63520(9) 0.0666(8) Uani 1 1 d D . . Cl2 Cl 0.62741(11) 0.38042(11) 0.21739(7) 0.0244(3) Uani 0.463(4) 1 d PD A 1 O5 O 0.5350(3) 0.3702(2) 0.18307(15) 0.0244(3) Uani 0.463(4) 1 d PD A 1 O6 O 0.6953(4) 0.3272(2) 0.2139(3) 0.0570(15) Uani 0.463(4) 1 d PD A 1 O7 O 0.6777(3) 0.43895(19) 0.2098(2) 0.0570(15) Uani 0.463(4) 1 d PD A 1 O8 O 0.6000(4) 0.3801(3) 0.26241(14) 0.064(2) Uani 0.463(4) 1 d PD A 1 Cl2A Cl 0.62924(13) 0.39647(9) 0.21007(6) 0.0270(4) Uiso 0.537(4) 1 d PD A 2 O5A O 0.5198(3) 0.38079(18) 0.18976(12) 0.0272(8) Uiso 0.537(4) 1 d PD A 2 O6A O 0.6923(5) 0.3385(3) 0.2261(2) 0.0512(14) Uiso 0.537(4) 1 d PD A 2 O7A O 0.6801(3) 0.42782(17) 0.17654(13) 0.0339(8) Uiso 0.537(4) 1 d PD A 2 O8A O 0.6296(3) 0.43948(19) 0.24888(13) 0.0437(10) Uiso 0.537(4) 1 d PD A 2 Cl3 Cl 0.67376(4) 0.34355(2) 0.521065(17) 0.02182(9) Uani 1 1 d . . . O9 O 0.58774(13) 0.30210(8) 0.52729(6) 0.0339(4) Uani 1 1 d . . . O10 O 0.70333(13) 0.32861(9) 0.47651(6) 0.0329(4) Uani 1 1 d . . . O11 O 0.76340(13) 0.33254(10) 0.55767(6) 0.0358(4) Uani 1 1 d . . . O12 O 0.64117(14) 0.40995(8) 0.52028(7) 0.0375(4) Uani 1 1 d . . . Cl4 Cl 0.28086(4) 0.43288(3) 0.64819(2) 0.02822(11) Uani 1 1 d . . . O13 O 0.3657(2) 0.45891(13) 0.68117(10) 0.0732(8) Uani 1 1 d . . . O14 O 0.2774(2) 0.46314(11) 0.60327(8) 0.0638(7) Uani 1 1 d . . . O15 O 0.18429(17) 0.44614(12) 0.66457(8) 0.0529(6) Uani 1 1 d . . . O16 O 0.29134(18) 0.36440(9) 0.64325(8) 0.0487(5) Uani 1 1 d . . . C67 C 0.5977(3) 0.08501(19) 0.13036(11) 0.0553(6) Uani 1 1 d . . . H67A H 0.5477 0.0702 0.1499 0.083 Uiso 1 1 calc R . . H67B H 0.5792 0.0657 0.0990 0.083 Uiso 1 1 calc R . . H67C H 0.5946 0.1325 0.1278 0.083 Uiso 1 1 calc R . . C68 C 0.7064(3) 0.06476(19) 0.15233(11) 0.0553(6) Uani 1 1 d . . . H68A H 0.7089 0.0172 0.1578 0.066 Uiso 1 1 calc R . . H68B H 0.7566 0.0757 0.1314 0.066 Uiso 1 1 calc R . . O17 O 0.73417(18) 0.09867(13) 0.19601(10) 0.0622(5) Uani 1 1 d . C . C69 C 0.8333(3) 0.07991(19) 0.22067(14) 0.0622(5) Uani 1 1 d D . . H69A H 0.8884 0.0870 0.2014 0.075 Uiso 1 1 calc R B 6 H69B H 0.8333 0.0334 0.2296 0.075 Uiso 1 1 calc R B 6 C70A C 0.8524(5) 0.1224(3) 0.2636(2) 0.093(2) Uani 0.862(10) 1 d P C 6 H70A H 0.8171 0.1036 0.2878 0.140 Uiso 0.862(10) 1 calc PR C 6 H70B H 0.8241 0.1660 0.2554 0.140 Uiso 0.862(10) 1 calc PR C 6 H70C H 0.9284 0.1254 0.2757 0.140 Uiso 0.862(10) 1 calc PR C 6 C70B C 0.9198(14) 0.0812(12) 0.2605(6) 0.047(7) Uiso 0.138(10) 1 d PD C 7 H70D H 0.9818 0.1010 0.2510 0.071 Uiso 0.138(10) 1 calc PR C 7 H70E H 0.9367 0.0367 0.2714 0.071 Uiso 0.138(10) 1 calc PR C 7 H70F H 0.8993 0.1067 0.2859 0.071 Uiso 0.138(10) 1 calc PR C 7 N13 N 0.4205(4) 0.5953(3) 0.9766(2) 0.122(2) Uani 1 1 d . . . C71 C 0.3779(4) 0.6280(3) 0.9463(2) 0.0840(16) Uani 1 1 d . . . C72 C 0.3230(3) 0.6692(2) 0.90920(13) 0.0663(11) Uani 1 1 d . . . H72A H 0.2506 0.6534 0.8993 0.100 Uiso 1 1 calc R . . H72B H 0.3597 0.6681 0.8824 0.100 Uiso 1 1 calc R . . H72C H 0.3215 0.7139 0.9208 0.100 Uiso 1 1 calc R . . C73 C 0.4051(6) 0.4788(3) 0.0938(2) 0.0402(12) Uani 0.65 1 d P D 3 H73A H 0.4148 0.4584 0.1249 0.060 Uiso 0.65 1 calc PR D 3 H73B H 0.4403 0.4525 0.0729 0.060 Uiso 0.65 1 calc PR D 3 H73C H 0.3296 0.4817 0.0806 0.060 Uiso 0.65 1 calc PR D 3 C74 C 0.4520(5) 0.5458(4) 0.0981(2) 0.0460(13) Uani 0.65 1 d P D 3 H74A H 0.5252 0.5434 0.1159 0.055 Uiso 0.65 1 calc PR D 3 H74B H 0.4548 0.5628 0.0664 0.055 Uiso 0.65 1 calc PR D 3 O18 O 0.3932(3) 0.58960(17) 0.12134(11) 0.0454(7) Uani 0.65 1 d P D 3 C75 C 0.4226(4) 0.6549(3) 0.11723(18) 0.0580(15) Uani 0.65 1 d P D 3 H75A H 0.4179 0.6664 0.0837 0.070 Uiso 0.65 1 calc PR D 3 H75B H 0.4963 0.6615 0.1335 0.070 Uiso 0.65 1 calc PR D 3 C76 C 0.3493(7) 0.6979(3) 0.1391(3) 0.076(2) Uani 0.65 1 d P D 3 H76A H 0.2773 0.6939 0.1212 0.114 Uiso 0.65 1 calc PR D 3 H76B H 0.3725 0.7432 0.1385 0.114 Uiso 0.65 1 calc PR D 3 H76C H 0.3508 0.6844 0.1717 0.114 Uiso 0.65 1 calc PR D 3 N14B N 0.2427(9) 0.6383(6) 0.1518(4) 0.077(3) Uiso 0.35 1 d P E 4 C77 C 0.2989(11) 0.6780(7) 0.1436(5) 0.062(3) Uiso 0.35 1 d P E 4 C78 C 0.3750(11) 0.7282(7) 0.1357(5) 0.065(3) Uiso 0.35 1 d P E 4 H78A H 0.4432 0.7078 0.1346 0.098 Uiso 0.35 1 calc PR E 4 H78B H 0.3835 0.7598 0.1615 0.098 Uiso 0.35 1 calc PR E 4 H78C H 0.3490 0.7504 0.1059 0.098 Uiso 0.35 1 calc PR E 4 N15B N 0.4957(7) 0.5871(5) 0.1217(3) 0.062(2) Uiso 0.35 1 d P F 4 C79 C 0.4604(14) 0.5371(9) 0.1107(6) 0.062(2) Uiso 0.35 1 d P F 4 C80 C 0.421(3) 0.4784(16) 0.0947(11) 0.146(11) Uiso 0.35 1 d P F 4 H80A H 0.4496 0.4661 0.0669 0.219 Uiso 0.35 1 calc PR F 4 H80B H 0.3437 0.4812 0.0864 0.219 Uiso 0.35 1 calc PR F 4 H80C H 0.4403 0.4456 0.1193 0.219 Uiso 0.35 1 calc PR F 4 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 0.01263(11) 0.01271(12) 0.01518(11) 0.00018(9) 0.00246(9) -0.00014(9) Mn2 0.01369(12) 0.01294(12) 0.01672(12) -0.00047(9) 0.00357(9) -0.00009(9) N1 0.0183(7) 0.0160(7) 0.0176(6) 0.0008(5) 0.0045(5) 0.0017(6) N2 0.0141(7) 0.0173(7) 0.0161(6) 0.0018(5) 0.0031(5) -0.0003(5) C1 0.0245(9) 0.0197(9) 0.0200(8) -0.0005(7) 0.0050(7) 0.0034(7) C2 0.0294(10) 0.0197(9) 0.0236(9) -0.0025(7) 0.0084(8) 0.0030(8) C3 0.0243(10) 0.0199(9) 0.0347(11) -0.0062(8) 0.0116(8) 0.0025(7) C4 0.0171(8) 0.0181(9) 0.0331(10) -0.0009(7) 0.0067(7) 0.0037(7) C5 0.0148(8) 0.0158(8) 0.0227(8) 0.0011(6) 0.0059(6) 0.0000(6) C6 0.0147(8) 0.0180(8) 0.0213(8) 0.0035(6) 0.0048(6) 0.0011(6) C7 0.0177(9) 0.0322(11) 0.0265(9) 0.0049(8) 0.0042(7) 0.0077(8) C8 0.0197(9) 0.0467(14) 0.0256(10) 0.0066(9) -0.0006(8) 0.0071(9) C9 0.0200(9) 0.0399(12) 0.0191(8) 0.0013(8) 0.0006(7) 0.0023(9) C10 0.0144(8) 0.0234(9) 0.0184(8) 0.0021(7) 0.0035(6) -0.0018(7) C11 0.0201(8) 0.0234(9) 0.0147(7) -0.0003(6) 0.0024(6) -0.0050(7) C12 0.0198(8) 0.0200(8) 0.0170(7) -0.0003(6) 0.0041(6) -0.0062(7) C13 0.0195(8) 0.0179(8) 0.0164(7) -0.0016(6) 0.0031(6) -0.0045(7) C14 0.0303(10) 0.0188(9) 0.0219(8) -0.0006(7) 0.0062(8) -0.0084(8) C15 0.0372(12) 0.0145(8) 0.0291(10) -0.0010(7) 0.0058(9) -0.0051(8) C16 0.0289(10) 0.0157(8) 0.0276(9) -0.0010(7) 0.0047(8) 0.0006(7) C17 0.0206(8) 0.0166(8) 0.0181(8) -0.0012(6) 0.0024(6) -0.0002(7) C18 0.0203(9) 0.0175(8) 0.0238(8) 0.0004(7) 0.0053(7) 0.0029(7) C19 0.0322(12) 0.0238(10) 0.0438(13) 0.0067(9) 0.0144(10) 0.0115(9) C20 0.0297(12) 0.0332(12) 0.0577(16) 0.0046(11) 0.0216(11) 0.0119(10) C21 0.0273(11) 0.0317(12) 0.0554(15) 0.0024(11) 0.0239(11) 0.0039(9) C22 0.0250(10) 0.0200(9) 0.0457(12) 0.0002(9) 0.0177(9) 0.0012(8) N3 0.0179(7) 0.0158(7) 0.0290(8) -0.0004(6) 0.0091(6) 0.0008(6) N4 0.0183(7) 0.0143(7) 0.0153(6) -0.0009(5) 0.0024(5) -0.0017(5) N5 0.0163(7) 0.0168(7) 0.0227(7) 0.0020(6) 0.0060(6) -0.0002(6) N6 0.0161(7) 0.0139(7) 0.0161(6) -0.0007(5) 0.0028(5) -0.0009(5) C23 0.0183(9) 0.0222(9) 0.0305(10) 0.0017(7) 0.0088(7) -0.0003(7) C24 0.0166(9) 0.0313(11) 0.0387(11) 0.0032(9) 0.0097(8) -0.0031(8) C25 0.0214(10) 0.0291(11) 0.0429(12) -0.0001(9) 0.0082(9) -0.0096(8) C26 0.0248(10) 0.0193(9) 0.0351(11) -0.0018(8) 0.0076(8) -0.0059(8) C27 0.0178(8) 0.0172(8) 0.0209(8) 0.0019(6) 0.0047(6) -0.0017(7) C28 0.0179(8) 0.0154(8) 0.0194(8) -0.0012(6) 0.0036(6) -0.0012(6) C29 0.0254(10) 0.0154(8) 0.0312(10) 0.0009(7) 0.0084(8) -0.0009(7) C30 0.0287(11) 0.0168(9) 0.0386(11) 0.0028(8) 0.0082(9) 0.0053(8) C31 0.0205(9) 0.0186(9) 0.0359(11) 0.0001(8) 0.0073(8) 0.0041(7) C32 0.0169(8) 0.0159(8) 0.0182(7) -0.0006(6) 0.0035(6) 0.0009(6) C33 0.0160(8) 0.0183(8) 0.0183(7) -0.0027(6) 0.0026(6) 0.0009(6) C34 0.0129(7) 0.0215(8) 0.0172(7) -0.0014(6) 0.0015(6) 0.0013(6) C35 0.0124(7) 0.0210(8) 0.0196(8) 0.0002(6) 0.0031(6) -0.0007(6) C36 0.0168(8) 0.0322(11) 0.0226(9) 0.0030(8) -0.0006(7) -0.0054(8) C37 0.0167(9) 0.0382(12) 0.0281(10) 0.0027(9) -0.0025(7) -0.0093(8) C38 0.0178(9) 0.0273(10) 0.0279(9) 0.0031(8) 0.0018(7) -0.0074(8) C39 0.0148(8) 0.0179(8) 0.0205(8) -0.0005(6) 0.0048(6) -0.0012(6) C40 0.0164(8) 0.0166(8) 0.0202(8) -0.0016(6) 0.0049(6) -0.0018(6) C41 0.0265(10) 0.0210(9) 0.0241(9) 0.0001(7) 0.0047(7) -0.0070(8) C42 0.0338(11) 0.0212(9) 0.0265(9) 0.0047(7) 0.0066(8) -0.0069(8) C43 0.0292(10) 0.0217(9) 0.0214(8) 0.0042(7) 0.0039(7) -0.0025(8) C44 0.0222(9) 0.0194(9) 0.0210(8) -0.0009(7) 0.0030(7) -0.0040(7) N7 0.0178(7) 0.0157(7) 0.0185(7) -0.0004(5) 0.0048(6) -0.0007(6) N8 0.0134(6) 0.0165(7) 0.0189(7) -0.0006(5) 0.0046(5) -0.0007(5) N9 0.0177(7) 0.0175(7) 0.0164(6) 0.0016(5) 0.0032(5) 0.0003(6) N10 0.0130(6) 0.0134(6) 0.0153(6) -0.0001(5) 0.0022(5) 0.0008(5) C45 0.0253(9) 0.0220(9) 0.0197(8) 0.0047(7) 0.0042(7) -0.0018(7) C46 0.0346(11) 0.0266(10) 0.0223(9) 0.0114(8) 0.0040(8) 0.0016(9) C47 0.0302(11) 0.0319(11) 0.0244(9) 0.0090(8) -0.0015(8) 0.0056(9) C48 0.0207(9) 0.0270(10) 0.0222(8) 0.0038(7) -0.0019(7) 0.0017(8) C49 0.0173(8) 0.0170(8) 0.0155(7) 0.0011(6) 0.0019(6) 0.0016(6) C50 0.0140(7) 0.0163(8) 0.0166(7) -0.0010(6) 0.0020(6) 0.0013(6) C51 0.0161(8) 0.0224(9) 0.0225(8) -0.0005(7) -0.0014(7) -0.0021(7) C52 0.0183(9) 0.0207(9) 0.0276(9) -0.0012(7) -0.0005(7) -0.0058(7) C53 0.0189(8) 0.0163(8) 0.0244(8) 0.0021(7) 0.0038(7) -0.0034(7) C54 0.0136(7) 0.0143(7) 0.0165(7) 0.0003(6) 0.0027(6) 0.0002(6) C55 0.0164(8) 0.0132(7) 0.0183(7) 0.0010(6) 0.0052(6) 0.0004(6) C56 0.0186(8) 0.0155(8) 0.0172(7) -0.0011(6) 0.0061(6) 0.0014(6) C57 0.0176(8) 0.0179(8) 0.0153(7) 0.0005(6) 0.0037(6) 0.0026(6) C58 0.0267(10) 0.0230(9) 0.0192(8) -0.0011(7) 0.0043(7) 0.0085(8) C59 0.0271(10) 0.0277(10) 0.0236(9) 0.0019(8) 0.0028(8) 0.0146(8) C60 0.0202(9) 0.0280(10) 0.0198(8) 0.0013(7) -0.0001(7) 0.0069(8) C61 0.0160(8) 0.0195(8) 0.0145(7) 0.0001(6) 0.0027(6) 0.0009(6) C62 0.0193(8) 0.0201(8) 0.0141(7) -0.0003(6) 0.0022(6) -0.0006(7) C63 0.0222(9) 0.0309(11) 0.0234(9) -0.0022(8) -0.0033(7) -0.0021(8) C64 0.0355(12) 0.0351(12) 0.0266(10) -0.0088(9) -0.0062(9) -0.0059(10) C65 0.0426(13) 0.0268(11) 0.0238(9) -0.0102(8) 0.0006(9) -0.0023(10) C66 0.0324(11) 0.0218(9) 0.0197(8) -0.0055(7) 0.0033(8) 0.0020(8) N11 0.0209(7) 0.0176(7) 0.0165(6) -0.0024(5) 0.0030(6) 0.0006(6) N12 0.0149(7) 0.0159(7) 0.0140(6) 0.0006(5) 0.0035(5) 0.0004(5) Cl1 0.0224(2) 0.0231(2) 0.0247(2) -0.00041(17) 0.00341(17) -0.00408(17) O1 0.0226(9) 0.0488(13) 0.123(2) -0.0212(14) -0.0022(12) -0.0003(9) O2 0.0480(11) 0.0379(10) 0.0335(9) -0.0146(7) 0.0099(8) -0.0168(8) O3 0.0979(18) 0.0356(11) 0.0524(12) -0.0191(9) 0.0469(13) -0.0262(11) O4 0.0587(14) 0.0538(14) 0.0754(16) 0.0418(12) -0.0196(12) -0.0295(11) Cl2 0.0171(5) 0.0251(8) 0.0292(6) -0.0072(6) -0.0004(4) -0.0004(5) O5 0.0171(5) 0.0251(8) 0.0292(6) -0.0072(6) -0.0004(4) -0.0004(5) O6 0.0275(16) 0.0213(15) 0.121(5) 0.010(2) 0.012(2) -0.0069(12) O7 0.0275(16) 0.0213(15) 0.121(5) 0.010(2) 0.012(2) -0.0069(12) O8 0.038(2) 0.126(5) 0.0225(19) -0.020(2) -0.0058(16) 0.024(3) Cl3 0.0172(2) 0.0208(2) 0.0265(2) 0.00184(16) 0.00138(16) 0.00031(16) O9 0.0254(8) 0.0302(9) 0.0462(10) 0.0098(7) 0.0070(7) -0.0068(7) O10 0.0244(8) 0.0469(10) 0.0273(8) -0.0021(7) 0.0042(6) 0.0020(7) O11 0.0274(8) 0.0480(11) 0.0271(8) 0.0075(7) -0.0078(6) 0.0008(8) O12 0.0324(9) 0.0213(8) 0.0580(11) -0.0033(8) 0.0061(8) 0.0030(7) Cl4 0.0285(2) 0.0217(2) 0.0347(3) 0.00145(19) 0.0062(2) 0.00117(19) O13 0.0546(15) 0.0637(16) 0.0900(19) 0.0117(14) -0.0169(13) -0.0374(13) O14 0.105(2) 0.0479(13) 0.0483(12) 0.0195(10) 0.0388(13) 0.0382(13) O15 0.0453(12) 0.0661(15) 0.0511(12) -0.0102(10) 0.0186(10) 0.0170(11) O16 0.0623(13) 0.0207(8) 0.0716(14) -0.0022(9) 0.0348(11) -0.0008(8) C67 0.0548(13) 0.0711(16) 0.0404(11) 0.0018(10) 0.0095(10) -0.0017(12) C68 0.0548(13) 0.0711(16) 0.0404(11) 0.0018(10) 0.0095(10) -0.0017(12) O17 0.0405(10) 0.0636(13) 0.0781(14) 0.0142(11) -0.0007(9) 0.0003(9) C69 0.0405(10) 0.0636(13) 0.0781(14) 0.0142(11) -0.0007(9) 0.0003(9) C70A 0.076(4) 0.088(4) 0.095(4) 0.003(3) -0.040(3) -0.040(3) N13 0.071(3) 0.174(6) 0.125(4) -0.047(4) 0.029(3) 0.045(3) C71 0.047(2) 0.116(4) 0.097(4) -0.054(3) 0.034(2) -0.006(2) C72 0.083(3) 0.065(2) 0.056(2) -0.0253(18) 0.026(2) -0.029(2) C73 0.048(3) 0.036(2) 0.040(2) 0.0138(17) 0.0174(19) 0.0158(19) C74 0.029(2) 0.067(4) 0.046(3) 0.013(3) 0.018(2) 0.008(2) O18 0.0393(16) 0.0525(19) 0.0457(16) 0.0126(14) 0.0109(13) -0.0057(14) C75 0.054(3) 0.066(3) 0.048(3) 0.020(2) -0.008(2) -0.028(3) C76 0.095(6) 0.043(3) 0.077(4) 0.002(3) -0.019(4) -0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N5 2.2279(16) . ? Mn1 N1 2.2545(16) . ? Mn1 N9 2.2737(16) . ? Mn1 N10 2.2837(15) . ? Mn1 N2 2.2962(16) . ? Mn1 N6 2.3123(15) . ? Mn2 N7 2.2472(16) . ? Mn2 N11 2.2482(16) . ? Mn2 N3 2.2570(16) . ? Mn2 N4 2.2857(16) . ? Mn2 N8 2.3046(16) . ? Mn2 N12 2.3276(15) . ? N1 C1 1.340(2) . ? N1 C5 1.347(2) . ? N2 C6 1.346(2) . ? N2 C10 1.351(2) . ? C1 C2 1.388(3) . ? C1 H1 0.9500 . ? C2 C3 1.376(3) . ? C2 H2 0.9500 . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.393(3) . ? C4 H4 0.9500 . ? C5 C6 1.485(3) . ? C6 C7 1.393(3) . ? C7 C8 1.383(3) . ? C7 H7 0.9500 . ? C8 C9 1.379(3) . ? C8 H8 0.9500 . ? C9 C10 1.397(3) . ? C9 H9 0.9500 . ? C10 C11 1.433(3) . ? C11 C12 1.194(3) . ? C12 C13 1.431(3) . ? C13 N4 1.357(2) . ? C13 C14 1.391(3) . ? C14 C15 1.383(3) . ? C14 H14 0.9500 . ? C15 C16 1.381(3) . ? C15 H15 0.9500 . ? C16 C17 1.393(3) . ? C16 H16 0.9500 . ? C17 N4 1.344(2) . ? C17 C18 1.484(3) . ? C18 N3 1.349(2) . ? C18 C19 1.387(3) . ? C19 C20 1.384(3) . ? C19 H19 0.9500 . ? C20 C21 1.382(4) . ? C20 H20 0.9500 . ? C21 C22 1.387(3) . ? C21 H21 0.9500 . ? C22 N3 1.338(3) . ? C22 H22 0.9500 . ? N5 C23 1.342(2) . ? N5 C27 1.346(2) . ? N6 C28 1.344(2) . ? N6 C32 1.356(2) . ? C23 C24 1.379(3) . ? C23 H23 0.9500 . ? C24 C25 1.384(3) . ? C24 H24 0.9500 . ? C25 C26 1.386(3) . ? C25 H25 0.9500 . ? C26 C27 1.388(3) . ? C26 H26 0.9500 . ? C27 C28 1.483(3) . ? C28 C29 1.397(3) . ? C29 C30 1.381(3) . ? C29 H29 0.9500 . ? C30 C31 1.385(3) . ? C30 H30 0.9500 . ? C31 C32 1.390(3) . ? C31 H31 0.9500 . ? C32 C33 1.437(3) . ? C33 C34 1.198(3) . ? C34 C35 1.432(3) . ? C35 N8 1.350(2) . ? C35 C36 1.390(3) . ? C36 C37 1.380(3) . ? C36 H36 0.9500 . ? C37 C38 1.379(3) . ? C37 H37 0.9500 . ? C38 C39 1.398(3) . ? C38 H38 0.9500 . ? C39 N8 1.349(2) . ? C39 C40 1.488(3) . ? C40 N7 1.348(2) . ? C40 C41 1.391(3) . ? C41 C42 1.388(3) . ? C41 H41 0.9500 . ? C42 C43 1.382(3) . ? C42 H42 0.9500 . ? C43 C44 1.383(3) . ? C43 H43 0.9500 . ? C44 N7 1.341(2) . ? C44 H44 0.9500 . ? N9 C45 1.342(2) . ? N9 C49 1.348(2) . ? N10 C50 1.345(2) . ? N10 C54 1.354(2) . ? C45 C46 1.385(3) . ? C45 H45 0.9500 . ? C46 C47 1.380(3) . ? C46 H46 0.9500 . ? C47 C48 1.385(3) . ? C47 H47 0.9500 . ? C48 C49 1.386(3) . ? C48 H48 0.9500 . ? C49 C50 1.480(3) . ? C50 C51 1.393(3) . ? C51 C52 1.381(3) . ? C51 H51 0.9500 . ? C52 C53 1.385(3) . ? C52 H52 0.9500 . ? C53 C54 1.394(3) . ? C53 H53 0.9500 . ? C54 C55 1.430(3) . ? C55 C56 1.200(3) . ? C56 C57 1.433(3) . ? C57 N12 1.358(2) . ? C57 C58 1.387(3) . ? C58 C59 1.379(3) . ? C58 H58 0.9500 . ? C59 C60 1.389(3) . ? C59 H59 0.9500 . ? C60 C61 1.391(3) . ? C60 H60 0.9500 . ? C61 N12 1.349(2) . ? C61 C62 1.484(3) . ? C62 N11 1.342(2) . ? C62 C63 1.387(3) . ? C63 C64 1.387(3) . ? C63 H63 0.9500 . ? C64 C65 1.373(4) . ? C64 H64 0.9500 . ? C65 C66 1.386(3) . ? C65 H65 0.9500 . ? C66 N11 1.343(2) . ? C66 H66 0.9500 . ? Cl1 O4 1.421(2) . ? Cl1 O1 1.422(2) . ? Cl1 O3 1.4236(19) . ? Cl1 O2 1.4334(18) . ? Cl2 O7 1.404(4) . ? Cl2 O8 1.411(5) . ? Cl2 O6 1.417(6) . ? Cl2 O5 1.420(4) . ? Cl2A O7A 1.421(4) . ? Cl2A O8A 1.429(4) . ? Cl2A O5A 1.462(4) . ? Cl2A O6A 1.470(6) . ? Cl3 O12 1.4281(17) . ? Cl3 O11 1.4360(16) . ? Cl3 O9 1.4361(16) . ? Cl3 O10 1.4430(17) . ? Cl4 O13 1.419(2) . ? Cl4 O16 1.4248(19) . ? Cl4 O14 1.435(2) . ? Cl4 O15 1.437(2) . ? C67 C68 1.489(5) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 O17 1.431(4) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? O17 C69 1.400(4) . ? C69 C70B 1.449(9) . ? C69 C70A 1.503(7) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70A H70A 0.9800 . ? C70A H70B 0.9800 . ? C70A H70C 0.9800 . ? C70B H70D 0.9800 . ? C70B H70E 0.9800 . ? C70B H70F 0.9800 . ? N13 C71 1.161(7) . ? C71 C72 1.447(8) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.502(10) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 O18 1.423(7) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? O18 C75 1.407(6) . ? C75 C76 1.513(10) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? N14B C77 1.146(15) . ? C77 C78 1.470(18) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? N15B C79 1.15(2) . ? C79 C80 1.36(4) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? 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 N5 Mn1 N1 97.73(6) . . ? N5 Mn1 N9 91.72(6) . . ? N1 Mn1 N9 93.05(6) . . ? N5 Mn1 N10 164.65(6) . . ? N1 Mn1 N10 85.78(6) . . ? N9 Mn1 N10 73.13(5) . . ? N5 Mn1 N2 85.00(6) . . ? N1 Mn1 N2 71.84(6) . . ? N9 Mn1 N2 163.89(6) . . ? N10 Mn1 N2 110.24(5) . . ? N5 Mn1 N6 73.11(6) . . ? N1 Mn1 N6 169.21(5) . . ? N9 Mn1 N6 81.74(6) . . ? N10 Mn1 N6 101.59(5) . . ? N2 Mn1 N6 112.15(6) . . ? N7 Mn2 N11 95.37(6) . . ? N7 Mn2 N3 92.95(6) . . ? N11 Mn2 N3 93.75(6) . . ? N7 Mn2 N4 165.20(6) . . ? N11 Mn2 N4 86.72(6) . . ? N3 Mn2 N4 72.28(6) . . ? N7 Mn2 N8 72.37(6) . . ? N11 Mn2 N8 167.73(6) . . ? N3 Mn2 N8 87.45(6) . . ? N4 Mn2 N8 105.23(6) . . ? N7 Mn2 N12 83.10(5) . . ? N11 Mn2 N12 72.70(6) . . ? N3 Mn2 N12 165.36(6) . . ? N4 Mn2 N12 111.43(5) . . ? N8 Mn2 N12 104.62(5) . . ? C1 N1 C5 118.92(16) . . ? C1 N1 Mn1 122.51(13) . . ? C5 N1 Mn1 118.52(12) . . ? C6 N2 C10 117.81(16) . . ? C6 N2 Mn1 116.99(12) . . ? C10 N2 Mn1 124.87(13) . . ? N1 C1 C2 122.39(19) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.71(19) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 119.50(18) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 118.90(19) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.52(18) . . ? N1 C5 C6 116.01(16) . . ? C4 C5 C6 122.47(18) . . ? N2 C6 C7 121.96(18) . . ? N2 C6 C5 116.21(16) . . ? C7 C6 C5 121.83(17) . . ? C8 C7 C6 119.8(2) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C9 C8 C7 118.8(2) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C8 C9 C10 118.6(2) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? N2 C10 C9 122.99(18) . . ? N2 C10 C11 116.26(17) . . ? C9 C10 C11 120.66(18) . . ? C12 C11 C10 175.1(2) . . ? C11 C12 C13 175.7(2) . . ? N4 C13 C14 123.07(18) . . ? N4 C13 C12 117.17(16) . . ? C14 C13 C12 119.72(17) . . ? C15 C14 C13 118.36(18) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? C16 C15 C14 119.27(19) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 119.32(19) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? N4 C17 C16 122.37(18) . . ? N4 C17 C18 116.30(16) . . ? C16 C17 C18 121.33(17) . . ? N3 C18 C19 121.81(18) . . ? N3 C18 C17 116.14(16) . . ? C19 C18 C17 122.05(18) . . ? C20 C19 C18 119.5(2) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C21 C20 C19 118.9(2) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 118.3(2) . . ? C20 C21 H21 120.8 . . ? C22 C21 H21 120.8 . . ? N3 C22 C21 123.4(2) . . ? N3 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? C22 N3 C18 118.07(17) . . ? C22 N3 Mn2 123.77(14) . . ? C18 N3 Mn2 117.73(12) . . ? C17 N4 C13 117.60(16) . . ? C17 N4 Mn2 116.97(12) . . ? C13 N4 Mn2 125.23(13) . . ? C23 N5 C27 118.32(17) . . ? C23 N5 Mn1 123.02(13) . . ? C27 N5 Mn1 117.15(12) . . ? C28 N6 C32 117.63(16) . . ? C28 N6 Mn1 113.06(11) . . ? C32 N6 Mn1 124.89(12) . . ? N5 C23 C24 122.6(2) . . ? N5 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C23 C24 C25 119.1(2) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C24 C25 C26 118.9(2) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C25 C26 C27 118.8(2) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? N5 C27 C26 122.27(18) . . ? N5 C27 C28 115.30(16) . . ? C26 C27 C28 122.43(18) . . ? N6 C28 C29 122.58(17) . . ? N6 C28 C27 115.92(16) . . ? C29 C28 C27 121.49(17) . . ? C30 C29 C28 118.77(18) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? C29 C30 C31 119.55(19) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C30 C31 C32 118.32(19) . . ? C30 C31 H31 120.8 . . ? C32 C31 H31 120.8 . . ? N6 C32 C31 122.91(17) . . ? N6 C32 C33 116.65(16) . . ? C31 C32 C33 120.34(17) . . ? C34 C33 C32 174.2(2) . . ? C33 C34 C35 170.4(2) . . ? N8 C35 C36 123.05(18) . . ? N8 C35 C34 118.96(16) . . ? C36 C35 C34 117.94(17) . . ? C37 C36 C35 118.46(19) . . ? C37 C36 H36 120.8 . . ? C35 C36 H36 120.8 . . ? C36 C37 C38 119.42(19) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C37 C38 C39 119.24(19) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? N8 C39 C38 121.95(18) . . ? N8 C39 C40 116.84(16) . . ? C38 C39 C40 121.17(17) . . ? N7 C40 C41 121.84(18) . . ? N7 C40 C39 115.92(16) . . ? C41 C40 C39 122.23(17) . . ? C42 C41 C40 118.79(19) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? C43 C42 C41 119.43(19) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C42 C43 C44 118.46(19) . . ? C42 C43 H43 120.8 . . ? C44 C43 H43 120.8 . . ? N7 C44 C43 122.87(19) . . ? N7 C44 H44 118.6 . . ? C43 C44 H44 118.6 . . ? C44 N7 C40 118.57(16) . . ? C44 N7 Mn2 123.07(13) . . ? C40 N7 Mn2 118.36(12) . . ? C39 N8 C35 117.89(16) . . ? C39 N8 Mn2 115.59(12) . . ? C35 N8 Mn2 126.08(12) . . ? C45 N9 C49 117.98(17) . . ? C45 N9 Mn1 124.16(13) . . ? C49 N9 Mn1 115.33(12) . . ? C50 N10 C54 117.58(15) . . ? C50 N10 Mn1 114.66(11) . . ? C54 N10 Mn1 124.86(12) . . ? N9 C45 C46 122.6(2) . . ? N9 C45 H45 118.7 . . ? C46 C45 H45 118.7 . . ? C47 C46 C45 118.85(19) . . ? C47 C46 H46 120.6 . . ? C45 C46 H46 120.6 . . ? C46 C47 C48 119.4(2) . . ? C46 C47 H47 120.3 . . ? C48 C47 H47 120.3 . . ? C49 C48 C47 118.3(2) . . ? C49 C48 H48 120.8 . . ? C47 C48 H48 120.8 . . ? N9 C49 C48 122.81(17) . . ? N9 C49 C50 115.40(16) . . ? C48 C49 C50 121.79(17) . . ? N10 C50 C51 122.53(17) . . ? N10 C50 C49 116.41(16) . . ? C51 C50 C49 121.01(16) . . ? C52 C51 C50 119.27(18) . . ? C52 C51 H51 120.4 . . ? C50 C51 H51 120.4 . . ? C51 C52 C53 119.05(18) . . ? C51 C52 H52 120.5 . . ? C53 C52 H52 120.5 . . ? C52 C53 C54 118.55(17) . . ? C52 C53 H53 120.7 . . ? C54 C53 H53 120.7 . . ? N10 C54 C53 122.85(17) . . ? N10 C54 C55 117.33(16) . . ? C53 C54 C55 119.82(16) . . ? C56 C55 C54 176.37(19) . . ? C55 C56 C57 173.26(19) . . ? N12 C57 C58 122.91(17) . . ? N12 C57 C56 117.09(16) . . ? C58 C57 C56 119.87(16) . . ? C59 C58 C57 119.29(18) . . ? C59 C58 H58 120.4 . . ? C57 C58 H58 120.4 . . ? C58 C59 C60 118.58(18) . . ? C58 C59 H59 120.7 . . ? C60 C59 H59 120.7 . . ? C59 C60 C61 119.27(18) . . ? C59 C60 H60 120.4 . . ? C61 C60 H60 120.4 . . ? N12 C61 C60 122.64(17) . . ? N12 C61 C62 115.92(16) . . ? C60 C61 C62 121.43(17) . . ? N11 C62 C63 122.56(18) . . ? N11 C62 C61 115.95(16) . . ? C63 C62 C61 121.49(18) . . ? C64 C63 C62 118.6(2) . . ? C64 C63 H63 120.7 . . ? C62 C63 H63 120.7 . . ? C65 C64 C63 118.9(2) . . ? C65 C64 H64 120.5 . . ? C63 C64 H64 120.5 . . ? C64 C65 C66 119.4(2) . . ? C64 C65 H65 120.3 . . ? C66 C65 H65 120.3 . . ? N11 C66 C65 122.1(2) . . ? N11 C66 H66 118.9 . . ? C65 C66 H66 118.9 . . ? C62 N11 C66 118.28(17) . . ? C62 N11 Mn2 117.26(12) . . ? C66 N11 Mn2 123.19(14) . . ? C61 N12 C57 117.21(16) . . ? C61 N12 Mn2 113.37(11) . . ? C57 N12 Mn2 126.33(12) . . ? O4 Cl1 O1 108.36(15) . . ? O4 Cl1 O3 108.45(17) . . ? O1 Cl1 O3 110.12(17) . . ? O4 Cl1 O2 110.02(14) . . ? O1 Cl1 O2 111.42(13) . . ? O3 Cl1 O2 108.43(11) . . ? O7 Cl2 O8 110.4(4) . . ? O7 Cl2 O6 110.0(3) . . ? O8 Cl2 O6 108.9(5) . . ? O7 Cl2 O5 111.7(3) . . ? O8 Cl2 O5 109.0(3) . . ? O6 Cl2 O5 106.6(4) . . ? O7A Cl2A O8A 108.7(3) . . ? O7A Cl2A O5A 110.9(2) . . ? O8A Cl2A O5A 108.5(2) . . ? O7A Cl2A O6A 106.6(3) . . ? O8A Cl2A O6A 109.4(3) . . ? O5A Cl2A O6A 112.7(3) . . ? O12 Cl3 O11 110.94(12) . . ? O12 Cl3 O9 109.77(11) . . ? O11 Cl3 O9 110.47(11) . . ? O12 Cl3 O10 108.32(11) . . ? O11 Cl3 O10 108.50(10) . . ? O9 Cl3 O10 108.77(11) . . ? O13 Cl4 O16 111.40(16) . . ? O13 Cl4 O14 109.76(17) . . ? O16 Cl4 O14 109.01(13) . . ? O13 Cl4 O15 108.34(17) . . ? O16 Cl4 O15 108.94(14) . . ? O14 Cl4 O15 109.35(14) . . ? C68 C67 H67A 109.5 . . ? C68 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C68 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? O17 C68 C67 107.7(3) . . ? O17 C68 H68A 110.2 . . ? C67 C68 H68A 110.2 . . ? O17 C68 H68B 110.2 . . ? C67 C68 H68B 110.2 . . ? H68A C68 H68B 108.5 . . ? C68 O17 C69 111.9(3) . . ? C70B C69 O17 154.0(11) . . ? C70B C69 C70A 49.2(10) . . ? O17 C69 C70A 104.9(4) . . ? C70B C69 H69A 85.3 . . ? O17 C69 H69A 110.8 . . ? C70A C69 H69A 110.8 . . ? C70B C69 H69B 81.2 . . ? O17 C69 H69B 110.8 . . ? C70A C69 H69B 110.8 . . ? H69A C69 H69B 108.8 . . ? C69 C70A H70A 109.5 . . ? C69 C70A H70B 109.5 . . ? C69 C70A H70C 109.5 . . ? C69 C70B H70D 109.5 . . ? C69 C70B H70E 109.5 . . ? C69 C70B H70F 109.5 . . ? N13 C71 C72 178.7(4) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O18 C74 C73 112.3(4) . . ? O18 C74 H74A 109.1 . . ? C73 C74 H74A 109.1 . . ? O18 C74 H74B 109.1 . . ? C73 C74 H74B 109.1 . . ? H74A C74 H74B 107.9 . . ? C75 O18 C74 112.9(4) . . ? O18 C75 C76 108.9(5) . . ? O18 C75 H75A 109.9 . . ? C76 C75 H75A 109.9 . . ? O18 C75 H75B 109.9 . . ? C76 C75 H75B 109.9 . . ? H75A C75 H75B 108.3 . . ? N14B C77 C78 176.6(15) . . ? N15B C79 C80 176(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 N5 Mn1 N1 C1 100.75(15) . . . . ? N9 Mn1 N1 C1 8.60(15) . . . . ? N10 Mn1 N1 C1 -64.23(15) . . . . ? N2 Mn1 N1 C1 -177.14(16) . . . . ? N6 Mn1 N1 C1 69.4(4) . . . . ? N5 Mn1 N1 C5 -76.72(14) . . . . ? N9 Mn1 N1 C5 -168.87(13) . . . . ? N10 Mn1 N1 C5 118.30(13) . . . . ? N2 Mn1 N1 C5 5.40(13) . . . . ? N6 Mn1 N1 C5 -108.1(3) . . . . ? N5 Mn1 N2 C6 94.17(13) . . . . ? N1 Mn1 N2 C6 -5.66(12) . . . . ? N9 Mn1 N2 C6 15.4(3) . . . . ? N10 Mn1 N2 C6 -83.93(13) . . . . ? N6 Mn1 N2 C6 163.66(12) . . . . ? N5 Mn1 N2 C10 -79.09(14) . . . . ? N1 Mn1 N2 C10 -178.93(15) . . . . ? N9 Mn1 N2 C10 -157.87(19) . . . . ? N10 Mn1 N2 C10 102.81(14) . . . . ? N6 Mn1 N2 C10 -9.61(16) . . . . ? C5 N1 C1 C2 1.5(3) . . . . ? Mn1 N1 C1 C2 -176.00(15) . . . . ? N1 C1 C2 C3 0.8(3) . . . . ? C1 C2 C3 C4 -1.8(3) . . . . ? C2 C3 C4 C5 0.7(3) . . . . ? C1 N1 C5 C4 -2.6(3) . . . . ? Mn1 N1 C5 C4 174.94(14) . . . . ? C1 N1 C5 C6 177.84(16) . . . . ? Mn1 N1 C5 C6 -4.6(2) . . . . ? C3 C4 C5 N1 1.5(3) . . . . ? C3 C4 C5 C6 -178.96(18) . . . . ? C10 N2 C6 C7 -1.6(3) . . . . ? Mn1 N2 C6 C7 -175.33(15) . . . . ? C10 N2 C6 C5 179.13(16) . . . . ? Mn1 N2 C6 C5 5.4(2) . . . . ? N1 C5 C6 N2 -0.6(2) . . . . ? C4 C5 C6 N2 179.85(17) . . . . ? N1 C5 C6 C7 -179.92(18) . . . . ? C4 C5 C6 C7 0.5(3) . . . . ? N2 C6 C7 C8 1.9(3) . . . . ? C5 C6 C7 C8 -178.80(19) . . . . ? C6 C7 C8 C9 0.0(3) . . . . ? C7 C8 C9 C10 -2.1(3) . . . . ? C6 N2 C10 C9 -0.7(3) . . . . ? Mn1 N2 C10 C9 172.55(15) . . . . ? C6 N2 C10 C11 175.95(16) . . . . ? Mn1 N2 C10 C11 -10.8(2) . . . . ? C8 C9 C10 N2 2.5(3) . . . . ? C8 C9 C10 C11 -174.0(2) . . . . ? N4 C13 C14 C15 -0.7(3) . . . . ? C12 C13 C14 C15 -178.72(19) . . . . ? C13 C14 C15 C16 -0.2(3) . . . . ? C14 C15 C16 C17 0.9(3) . . . . ? C15 C16 C17 N4 -0.7(3) . . . . ? C15 C16 C17 C18 179.63(19) . . . . ? N4 C17 C18 N3 -8.4(3) . . . . ? C16 C17 C18 N3 171.26(19) . . . . ? N4 C17 C18 C19 171.8(2) . . . . ? C16 C17 C18 C19 -8.5(3) . . . . ? N3 C18 C19 C20 -1.0(4) . . . . ? C17 C18 C19 C20 178.8(2) . . . . ? C18 C19 C20 C21 0.3(4) . . . . ? C19 C20 C21 C22 0.4(4) . . . . ? C20 C21 C22 N3 -0.6(4) . . . . ? C21 C22 N3 C18 0.0(4) . . . . ? C21 C22 N3 Mn2 172.2(2) . . . . ? C19 C18 N3 C22 0.8(3) . . . . ? C17 C18 N3 C22 -178.97(19) . . . . ? C19 C18 N3 Mn2 -171.85(17) . . . . ? C17 C18 N3 Mn2 8.3(2) . . . . ? N7 Mn2 N3 C22 2.30(19) . . . . ? N11 Mn2 N3 C22 97.87(18) . . . . ? N4 Mn2 N3 C22 -176.78(19) . . . . ? N8 Mn2 N3 C22 -69.90(18) . . . . ? N12 Mn2 N3 C22 76.1(3) . . . . ? N7 Mn2 N3 C18 174.53(15) . . . . ? N11 Mn2 N3 C18 -89.89(15) . . . . ? N4 Mn2 N3 C18 -4.54(14) . . . . ? N8 Mn2 N3 C18 102.34(15) . . . . ? N12 Mn2 N3 C18 -111.7(2) . . . . ? C16 C17 N4 C13 -0.1(3) . . . . ? C18 C17 N4 C13 179.55(16) . . . . ? C16 C17 N4 Mn2 -175.29(15) . . . . ? C18 C17 N4 Mn2 4.4(2) . . . . ? C14 C13 N4 C17 0.8(3) . . . . ? C12 C13 N4 C17 178.91(17) . . . . ? C14 C13 N4 Mn2 175.56(14) . . . . ? C12 C13 N4 Mn2 -6.4(2) . . . . ? N7 Mn2 N4 C17 -3.8(3) . . . . ? N11 Mn2 N4 C17 94.82(13) . . . . ? N3 Mn2 N4 C17 -0.17(13) . . . . ? N8 Mn2 N4 C17 -82.39(14) . . . . ? N12 Mn2 N4 C17 164.79(13) . . . . ? N7 Mn2 N4 C13 -178.6(2) . . . . ? N11 Mn2 N4 C13 -79.93(15) . . . . ? N3 Mn2 N4 C13 -174.92(16) . . . . ? N8 Mn2 N4 C13 102.87(15) . . . . ? N12 Mn2 N4 C13 -9.95(16) . . . . ? N1 Mn1 N5 C23 17.59(16) . . . . ? N9 Mn1 N5 C23 110.90(16) . . . . ? N10 Mn1 N5 C23 120.0(2) . . . . ? N2 Mn1 N5 C23 -53.29(16) . . . . ? N6 Mn1 N5 C23 -168.26(17) . . . . ? N1 Mn1 N5 C27 -176.67(14) . . . . ? N9 Mn1 N5 C27 -83.35(14) . . . . ? N10 Mn1 N5 C27 -74.3(3) . . . . ? N2 Mn1 N5 C27 112.45(14) . . . . ? N6 Mn1 N5 C27 -2.51(13) . . . . ? N5 Mn1 N6 C28 -11.92(12) . . . . ? N1 Mn1 N6 C28 20.7(4) . . . . ? N9 Mn1 N6 C28 82.42(13) . . . . ? N10 Mn1 N6 C28 153.21(12) . . . . ? N2 Mn1 N6 C28 -89.10(13) . . . . ? N5 Mn1 N6 C32 -167.63(15) . . . . ? N1 Mn1 N6 C32 -135.0(3) . . . . ? N9 Mn1 N6 C32 -73.29(14) . . . . ? N10 Mn1 N6 C32 -2.50(15) . . . . ? N2 Mn1 N6 C32 115.20(14) . . . . ? C27 N5 C23 C24 -1.0(3) . . . . ? Mn1 N5 C23 C24 164.59(17) . . . . ? N5 C23 C24 C25 -0.6(3) . . . . ? C23 C24 C25 C26 1.0(4) . . . . ? C24 C25 C26 C27 0.2(3) . . . . ? C23 N5 C27 C26 2.2(3) . . . . ? Mn1 N5 C27 C26 -164.21(16) . . . . ? C23 N5 C27 C28 -178.04(17) . . . . ? Mn1 N5 C27 C28 15.5(2) . . . . ? C25 C26 C27 N5 -1.8(3) . . . . ? C25 C26 C27 C28 178.5(2) . . . . ? C32 N6 C28 C29 2.9(3) . . . . ? Mn1 N6 C28 C29 -154.75(16) . . . . ? C32 N6 C28 C27 -178.44(16) . . . . ? Mn1 N6 C28 C27 23.95(19) . . . . ? N5 C27 C28 N6 -26.9(2) . . . . ? C26 C27 C28 N6 152.81(19) . . . . ? N5 C27 C28 C29 151.80(19) . . . . ? C26 C27 C28 C29 -28.5(3) . . . . ? N6 C28 C29 C30 1.3(3) . . . . ? C27 C28 C29 C30 -177.32(19) . . . . ? C28 C29 C30 C31 -2.9(3) . . . . ? C29 C30 C31 C32 0.3(3) . . . . ? C28 N6 C32 C31 -5.6(3) . . . . ? Mn1 N6 C32 C31 149.07(16) . . . . ? C28 N6 C32 C33 170.68(16) . . . . ? Mn1 N6 C32 C33 -34.6(2) . . . . ? C30 C31 C32 N6 4.1(3) . . . . ? C30 C31 C32 C33 -172.1(2) . . . . ? N8 C35 C36 C37 -0.1(3) . . . . ? C34 C35 C36 C37 -177.5(2) . . . . ? C35 C36 C37 C38 0.0(3) . . . . ? C36 C37 C38 C39 0.3(3) . . . . ? C37 C38 C39 N8 -0.6(3) . . . . ? C37 C38 C39 C40 177.0(2) . . . . ? N8 C39 C40 N7 -4.8(2) . . . . ? C38 C39 C40 N7 177.46(18) . . . . ? N8 C39 C40 C41 174.34(18) . . . . ? C38 C39 C40 C41 -3.4(3) . . . . ? N7 C40 C41 C42 2.2(3) . . . . ? C39 C40 C41 C42 -176.87(19) . . . . ? C40 C41 C42 C43 -0.5(3) . . . . ? C41 C42 C43 C44 -0.8(3) . . . . ? C42 C43 C44 N7 0.5(3) . . . . ? C43 C44 N7 C40 1.1(3) . . . . ? C43 C44 N7 Mn2 -179.07(15) . . . . ? C41 C40 N7 C44 -2.4(3) . . . . ? C39 C40 N7 C44 176.67(16) . . . . ? C41 C40 N7 Mn2 177.70(14) . . . . ? C39 C40 N7 Mn2 -3.2(2) . . . . ? N11 Mn2 N7 C44 5.83(15) . . . . ? N3 Mn2 N7 C44 99.87(15) . . . . ? N4 Mn2 N7 C44 103.3(3) . . . . ? N8 Mn2 N7 C44 -173.75(16) . . . . ? N12 Mn2 N7 C44 -65.98(15) . . . . ? N11 Mn2 N7 C40 -174.31(13) . . . . ? N3 Mn2 N7 C40 -80.26(14) . . . . ? N4 Mn2 N7 C40 -76.8(3) . . . . ? N8 Mn2 N7 C40 6.12(13) . . . . ? N12 Mn2 N7 C40 113.89(13) . . . . ? C38 C39 N8 C35 0.6(3) . . . . ? C40 C39 N8 C35 -177.16(16) . . . . ? C38 C39 N8 Mn2 -172.22(15) . . . . ? C40 C39 N8 Mn2 10.0(2) . . . . ? C36 C35 N8 C39 -0.2(3) . . . . ? C34 C35 N8 C39 177.16(16) . . . . ? C36 C35 N8 Mn2 171.75(15) . . . . ? C34 C35 N8 Mn2 -10.9(2) . . . . ? N7 Mn2 N8 C39 -8.55(12) . . . . ? N11 Mn2 N8 C39 -10.5(3) . . . . ? N3 Mn2 N8 C39 85.36(13) . . . . ? N4 Mn2 N8 C39 156.22(12) . . . . ? N12 Mn2 N8 C39 -86.24(13) . . . . ? N7 Mn2 N8 C35 179.31(15) . . . . ? N11 Mn2 N8 C35 177.3(2) . . . . ? N3 Mn2 N8 C35 -86.78(15) . . . . ? N4 Mn2 N8 C35 -15.92(15) . . . . ? N12 Mn2 N8 C35 101.62(15) . . . . ? N5 Mn1 N9 C45 8.25(16) . . . . ? N1 Mn1 N9 C45 106.08(16) . . . . ? N10 Mn1 N9 C45 -169.26(16) . . . . ? N2 Mn1 N9 C45 86.1(3) . . . . ? N6 Mn1 N9 C45 -64.42(16) . . . . ? N5 Mn1 N9 C49 169.78(13) . . . . ? N1 Mn1 N9 C49 -92.39(13) . . . . ? N10 Mn1 N9 C49 -7.73(12) . . . . ? N2 Mn1 N9 C49 -112.4(2) . . . . ? N6 Mn1 N9 C49 97.11(13) . . . . ? N5 Mn1 N10 C50 -16.1(3) . . . . ? N1 Mn1 N10 C50 87.84(12) . . . . ? N9 Mn1 N10 C50 -6.65(12) . . . . ? N2 Mn1 N10 C50 156.72(12) . . . . ? N6 Mn1 N10 C50 -84.21(12) . . . . ? N5 Mn1 N10 C54 -176.28(19) . . . . ? N1 Mn1 N10 C54 -72.34(14) . . . . ? N9 Mn1 N10 C54 -166.82(15) . . . . ? N2 Mn1 N10 C54 -3.45(15) . . . . ? N6 Mn1 N10 C54 115.62(14) . . . . ? C49 N9 C45 C46 -1.7(3) . . . . ? Mn1 N9 C45 C46 159.41(16) . . . . ? N9 C45 C46 C47 -0.5(3) . . . . ? C45 C46 C47 C48 1.7(3) . . . . ? C46 C47 C48 C49 -0.8(3) . . . . ? C45 N9 C49 C48 2.6(3) . . . . ? Mn1 N9 C49 C48 -160.13(15) . . . . ? C45 N9 C49 C50 -177.19(16) . . . . ? Mn1 N9 C49 C50 20.1(2) . . . . ? C47 C48 C49 N9 -1.4(3) . . . . ? C47 C48 C49 C50 178.41(19) . . . . ? C54 N10 C50 C51 3.5(3) . . . . ? Mn1 N10 C50 C51 -158.23(14) . . . . ? C54 N10 C50 C49 -179.01(15) . . . . ? Mn1 N10 C50 C49 19.29(19) . . . . ? N9 C49 C50 N10 -26.7(2) . . . . ? C48 C49 C50 N10 153.46(18) . . . . ? N9 C49 C50 C51 150.82(17) . . . . ? C48 C49 C50 C51 -29.0(3) . . . . ? N10 C50 C51 C52 0.1(3) . . . . ? C49 C50 C51 C52 -177.31(18) . . . . ? C50 C51 C52 C53 -2.8(3) . . . . ? C51 C52 C53 C54 1.9(3) . . . . ? C50 N10 C54 C53 -4.4(3) . . . . ? Mn1 N10 C54 C53 155.22(14) . . . . ? C50 N10 C54 C55 175.58(15) . . . . ? Mn1 N10 C54 C55 -24.8(2) . . . . ? C52 C53 C54 N10 1.8(3) . . . . ? C52 C53 C54 C55 -178.24(17) . . . . ? N12 C57 C58 C59 0.9(3) . . . . ? C56 C57 C58 C59 -174.86(19) . . . . ? C57 C58 C59 C60 1.2(3) . . . . ? C58 C59 C60 C61 -0.9(3) . . . . ? C59 C60 C61 N12 -1.6(3) . . . . ? C59 C60 C61 C62 177.86(19) . . . . ? N12 C61 C62 N11 -25.2(2) . . . . ? C60 C61 C62 N11 155.32(18) . . . . ? N12 C61 C62 C63 154.03(18) . . . . ? C60 C61 C62 C63 -25.5(3) . . . . ? N11 C62 C63 C64 -2.1(3) . . . . ? C61 C62 C63 C64 178.7(2) . . . . ? C62 C63 C64 C65 0.0(4) . . . . ? C63 C64 C65 C66 1.5(4) . . . . ? C64 C65 C66 N11 -1.0(4) . . . . ? C63 C62 N11 C66 2.6(3) . . . . ? C61 C62 N11 C66 -178.23(17) . . . . ? C63 C62 N11 Mn2 -164.97(15) . . . . ? C61 C62 N11 Mn2 14.2(2) . . . . ? C65 C66 N11 C62 -1.0(3) . . . . ? C65 C66 N11 Mn2 165.79(17) . . . . ? N7 Mn2 N11 C62 -82.99(14) . . . . ? N3 Mn2 N11 C62 -176.30(14) . . . . ? N4 Mn2 N11 C62 111.71(14) . . . . ? N8 Mn2 N11 C62 -81.1(3) . . . . ? N12 Mn2 N11 C62 -1.94(13) . . . . ? N7 Mn2 N11 C66 110.11(16) . . . . ? N3 Mn2 N11 C66 16.79(16) . . . . ? N4 Mn2 N11 C66 -55.19(16) . . . . ? N8 Mn2 N11 C66 112.0(3) . . . . ? N12 Mn2 N11 C66 -168.85(17) . . . . ? C60 C61 N12 C57 3.6(3) . . . . ? C62 C61 N12 C57 -175.90(15) . . . . ? C60 C61 N12 Mn2 -157.82(15) . . . . ? C62 C61 N12 Mn2 22.66(19) . . . . ? C58 C57 N12 C61 -3.2(3) . . . . ? C56 C57 N12 C61 172.60(16) . . . . ? C58 C57 N12 Mn2 155.48(15) . . . . ? C56 C57 N12 Mn2 -28.7(2) . . . . ? N7 Mn2 N12 C61 86.33(13) . . . . ? N11 Mn2 N12 C61 -11.51(12) . . . . ? N3 Mn2 N12 C61 11.3(3) . . . . ? N4 Mn2 N12 C61 -90.75(13) . . . . ? N8 Mn2 N12 C61 156.04(12) . . . . ? N7 Mn2 N12 C57 -73.09(14) . . . . ? N11 Mn2 N12 C57 -170.93(15) . . . . ? N3 Mn2 N12 C57 -148.1(2) . . . . ? N4 Mn2 N12 C57 109.82(14) . . . . ? N8 Mn2 N12 C57 -3.39(15) . . . . ? C67 C68 O17 C69 176.6(3) . . . . ? C68 O17 C69 C70B -178(2) . . . . ? C68 O17 C69 C70A 176.8(3) . . . . ? C73 C74 O18 C75 -167.7(4) . . . . ? C74 O18 C75 C76 174.9(5) . . . . ? _diffrn_measured_fraction_theta_max .994 _diffrn_reflns_theta_full 33.30 _diffrn_measured_fraction_theta_full .994 _refine_diff_density_max 1.371 _refine_diff_density_min -1.122 _refine_diff_density_rms .091 # Attachment 'Cmpd_6-756146R2.cif' data_n224a _database_code_depnum_ccdc_archive 'CCDC 756146' #TrackingRef 'Cmpd_6-756146R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H42 Co2 N12, 2(C2 H3 N), 2(C4 H10 O), 4(Cl O4)' _chemical_formula_sum 'C78 H68 Cl4 Co2 N14 O18' _chemical_formula_weight 1749.12 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.0222(6) _cell_length_b 19.4232(6) _cell_length_c 25.1592(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.523(2) _cell_angle_gamma 90.00 _cell_volume 7829.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22777 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 25.68 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3600 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8826 _exptl_absorpt_correction_T_max 0.9748 _exptl_absorpt_process_details 'Bruker Apex2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 KappaApex2 CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22777 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.68 _reflns_number_total 7260 _reflns_number_gt 5238 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2' _computing_cell_refinement 'Bruker Apex2' _computing_data_reduction 'Bruker Apex2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0639P)^2^+3.8388P] 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 7260 _refine_ls_number_parameters 526 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1238 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.36146(2) 0.20372(2) 0.662241(16) 0.01685(13) Uani 1 1 d . . . N1 N 0.33637(14) 0.10734(13) 0.62455(10) 0.0219(6) Uani 1 1 d . . . N2 N 0.48634(14) 0.16747(12) 0.63410(10) 0.0183(5) Uani 1 1 d . . . N3 N 0.36934(14) 0.26269(13) 0.59096(10) 0.0207(6) Uani 1 1 d . . . N4 N 0.39215(13) 0.30726(12) 0.69136(9) 0.0169(5) Uani 1 1 d . . . N5 N 0.32721(13) 0.14980(12) 0.73481(9) 0.0169(5) Uani 1 1 d . . . N6 N 0.23460(14) 0.23219(13) 0.67416(10) 0.0191(6) Uani 1 1 d . . . C1 C 0.26377(18) 0.07319(16) 0.62700(13) 0.0252(7) Uani 1 1 d . . . H1 H 0.2169 0.0958 0.6419 0.030 Uiso 1 1 calc R . . C2 C 0.25430(19) 0.00646(17) 0.60869(13) 0.0275(8) Uani 1 1 d . . . H2 H 0.2019 -0.0161 0.6111 0.033 Uiso 1 1 calc R . . C3 C 0.32132(19) -0.02666(17) 0.58707(13) 0.0295(8) Uani 1 1 d . . . H3 H 0.3162 -0.0727 0.5747 0.035 Uiso 1 1 calc R . . C4 C 0.39682(19) 0.00796(16) 0.58343(13) 0.0259(7) Uani 1 1 d . . . H4 H 0.4443 -0.0140 0.5687 0.031 Uiso 1 1 calc R . . C5 C 0.40145(17) 0.07493(16) 0.60162(12) 0.0211(7) Uani 1 1 d . . . C6 C 0.47861(17) 0.11632(16) 0.59793(12) 0.0220(7) Uani 1 1 d . . . C7 C 0.53762(18) 0.10377(17) 0.55916(13) 0.0266(7) Uani 1 1 d . . . H7 H 0.5303 0.0670 0.5346 0.032 Uiso 1 1 calc R . . C8 C 0.60757(19) 0.14578(17) 0.55673(13) 0.0277(8) Uani 1 1 d . . . H8 H 0.6474 0.1396 0.5294 0.033 Uiso 1 1 calc R . . C9 C 0.61855(18) 0.19630(16) 0.59421(12) 0.0241(7) Uani 1 1 d . . . H9 H 0.6663 0.2253 0.5935 0.029 Uiso 1 1 calc R . . C10 C 0.55834(17) 0.20439(15) 0.63353(12) 0.0192(6) Uani 1 1 d . . . C11 C 0.57329(16) 0.25022(15) 0.67690(12) 0.0186(7) Uani 1 1 d . . . C12 C 0.40772(17) 0.28250(15) 0.78440(12) 0.0181(7) Uani 1 1 d . . . C13 C 0.39553(15) 0.33090(15) 0.74210(12) 0.0167(6) Uani 1 1 d . . . C14 C 0.39445(18) 0.40056(16) 0.75506(13) 0.0236(7) Uani 1 1 d . . . H14 H 0.3960 0.4149 0.7912 0.028 Uiso 1 1 calc R . . C15 C 0.39114(19) 0.44819(17) 0.71482(13) 0.0277(8) Uani 1 1 d . . . H15 H 0.3899 0.4960 0.7226 0.033 Uiso 1 1 calc R . . C16 C 0.38960(19) 0.42549(16) 0.66313(13) 0.0261(7) Uani 1 1 d . . . H16 H 0.3874 0.4576 0.6347 0.031 Uiso 1 1 calc R . . C17 C 0.39124(16) 0.35516(16) 0.65260(12) 0.0194(7) Uani 1 1 d . . . C18 C 0.39166(17) 0.32908(16) 0.59744(12) 0.0214(7) Uani 1 1 d . . . C19 C 0.4144(2) 0.37004(19) 0.55465(14) 0.0342(9) Uani 1 1 d . . . H19 H 0.4328 0.4160 0.5600 0.041 Uiso 1 1 calc R . . C20 C 0.4097(2) 0.3424(2) 0.50430(15) 0.0446(10) Uani 1 1 d . . . H20 H 0.4242 0.3695 0.4744 0.054 Uiso 1 1 calc R . . C21 C 0.3842(2) 0.2758(2) 0.49749(13) 0.0358(9) Uani 1 1 d . . . H21 H 0.3797 0.2566 0.4629 0.043 Uiso 1 1 calc R . . C22 C 0.36510(19) 0.23704(18) 0.54139(13) 0.0276(8) Uani 1 1 d . . . H22 H 0.3483 0.1905 0.5366 0.033 Uiso 1 1 calc R . . C23 C 0.19249(18) 0.27769(16) 0.64418(13) 0.0249(7) Uani 1 1 d . . . H23 H 0.2206 0.2992 0.6156 0.030 Uiso 1 1 calc R . . C24 C 0.11010(18) 0.29482(17) 0.65294(13) 0.0267(7) Uani 1 1 d . . . H24 H 0.0824 0.3279 0.6312 0.032 Uiso 1 1 calc R . . C25 C 0.06899(18) 0.26269(17) 0.69401(13) 0.0272(8) Uani 1 1 d . . . H25 H 0.0119 0.2727 0.7005 0.033 Uiso 1 1 calc R . . C26 C 0.11130(18) 0.21578(16) 0.72572(13) 0.0253(7) Uani 1 1 d . . . H26 H 0.0839 0.1934 0.7542 0.030 Uiso 1 1 calc R . . C27 C 0.19476(17) 0.20207(15) 0.71500(12) 0.0193(7) Uani 1 1 d . . . C28 C 0.24560(17) 0.15454(15) 0.74795(12) 0.0188(7) Uani 1 1 d . . . C29 C 0.21280(19) 0.11814(16) 0.79012(13) 0.0261(7) Uani 1 1 d . . . H29 H 0.1554 0.1228 0.7986 0.031 Uiso 1 1 calc R . . C30 C 0.26292(19) 0.07524(17) 0.81989(14) 0.0291(8) Uani 1 1 d . . . H30 H 0.2407 0.0499 0.8488 0.035 Uiso 1 1 calc R . . C31 C 0.34558(18) 0.06970(16) 0.80711(13) 0.0244(7) Uani 1 1 d . . . H31 H 0.3816 0.0404 0.8270 0.029 Uiso 1 1 calc R . . C32 C 0.37598(17) 0.10751(15) 0.76466(12) 0.0197(7) Uani 1 1 d . . . C33 C 0.46285(17) 0.10556(15) 0.75246(12) 0.0197(6) Uani 1 1 d . . . Cl3 Cl 0.03067(5) 0.06989(4) 0.63935(3) 0.0290(2) Uani 1 1 d . . . O3 O 0.07395(14) 0.12797(13) 0.61788(9) 0.0377(6) Uani 1 1 d . . . O4 O -0.05431(16) 0.08560(14) 0.64546(13) 0.0599(9) Uani 1 1 d . . . O2 O 0.0711(2) 0.05035(16) 0.68737(12) 0.0692(10) Uani 1 1 d . . . O1 O 0.03682(17) 0.01356(17) 0.60342(14) 0.0755(11) Uani 1 1 d . . . Cl2 Cl 0.33112(5) 0.05928(4) 0.44108(3) 0.0279(2) Uani 1 1 d . . . O5 O 0.30226(17) -0.00411(14) 0.46213(11) 0.0545(8) Uani 1 1 d . . . O6 O 0.3119(3) 0.06110(16) 0.38616(12) 0.0854(12) Uani 1 1 d . . . O7 O 0.41693(17) 0.06619(18) 0.45070(16) 0.0855(12) Uani 1 1 d . . . O8 O 0.2914(2) 0.11648(16) 0.46506(13) 0.0716(10) Uani 1 1 d . . . C100 C 0.1163(3) -0.0531(3) 0.49235(18) 0.0600(13) Uani 1 1 d . . . H10A H 0.1591 -0.0205 0.4806 0.090 Uiso 1 1 calc R . . H10B H 0.0795 -0.0304 0.5179 0.090 Uiso 1 1 calc R . . H10C H 0.0834 -0.0686 0.4616 0.090 Uiso 1 1 calc R . . C101 C 0.1549(3) -0.1100(3) 0.5167(2) 0.0657(14) Uani 1 1 d . . . N100 N 0.1874(3) -0.1556(2) 0.5345(2) 0.122(2) Uani 1 1 d . . . C102 C 0.0947(4) 0.2610(3) 0.9145(2) 0.0791(17) Uani 1 1 d U . . H10D H 0.0701 0.3018 0.9310 0.119 Uiso 1 1 calc R . . H10E H 0.1220 0.2328 0.9419 0.119 Uiso 1 1 calc R . . H10F H 0.0508 0.2341 0.8969 0.119 Uiso 1 1 calc R . . C103 C 0.1585(3) 0.2831(2) 0.8740(2) 0.0664(16) Uani 1 1 d U . . H10G H 0.2070 0.3045 0.8922 0.080 Uiso 1 1 calc R . . H10H H 0.1784 0.2425 0.8540 0.080 Uiso 1 1 calc R . . C104 C 0.1788(3) 0.3613(2) 0.80226(19) 0.0613(14) Uani 1 1 d U . . H10I H 0.2004 0.3255 0.7780 0.074 Uiso 1 1 calc R . . H10J H 0.2266 0.3812 0.8221 0.074 Uiso 1 1 calc R . . C105 C 0.1360(4) 0.4160(2) 0.7711(2) 0.0775(16) Uani 1 1 d U . . H10K H 0.0868 0.3966 0.7532 0.116 Uiso 1 1 calc R . . H10L H 0.1743 0.4344 0.7445 0.116 Uiso 1 1 calc R . . H10M H 0.1187 0.4530 0.7950 0.116 Uiso 1 1 calc R . . O100 O 0.12133(14) 0.33127(13) 0.83846(10) 0.0408(6) Uani 1 1 d U . . 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 0.0148(2) 0.0178(2) 0.0179(2) -0.00036(18) -0.00240(16) -0.00166(15) N1 0.0200(12) 0.0235(14) 0.0220(15) -0.0021(12) -0.0029(11) -0.0044(10) N2 0.0188(12) 0.0172(13) 0.0190(14) -0.0001(11) -0.0037(10) -0.0004(10) N3 0.0183(12) 0.0265(15) 0.0172(14) 0.0010(12) -0.0024(11) -0.0003(10) N4 0.0129(11) 0.0191(14) 0.0185(14) 0.0005(11) -0.0011(10) -0.0005(9) N5 0.0155(12) 0.0166(13) 0.0185(14) -0.0019(11) -0.0013(10) -0.0018(9) N6 0.0164(12) 0.0187(14) 0.0223(15) -0.0012(11) -0.0016(11) -0.0029(10) C1 0.0200(15) 0.0285(19) 0.0270(19) -0.0038(15) -0.0005(14) -0.0057(13) C2 0.0238(16) 0.0295(19) 0.0292(19) -0.0019(15) -0.0010(14) -0.0093(14) C3 0.0339(18) 0.0229(18) 0.032(2) -0.0036(15) -0.0032(15) -0.0062(14) C4 0.0268(16) 0.0249(18) 0.0261(18) -0.0035(15) 0.0000(14) -0.0020(13) C5 0.0215(15) 0.0238(17) 0.0181(17) -0.0015(14) -0.0017(13) -0.0020(12) C6 0.0213(15) 0.0229(17) 0.0217(18) -0.0028(14) -0.0033(13) -0.0005(12) C7 0.0274(16) 0.0271(18) 0.0254(19) -0.0076(15) 0.0020(14) -0.0034(13) C8 0.0267(16) 0.034(2) 0.0221(18) -0.0057(16) 0.0053(14) -0.0030(14) C9 0.0205(15) 0.0272(18) 0.0246(18) 0.0006(15) 0.0005(13) -0.0034(13) C10 0.0168(14) 0.0204(16) 0.0204(17) 0.0000(14) -0.0026(12) -0.0024(12) C11 0.0136(14) 0.0198(16) 0.0222(18) 0.0047(14) -0.0016(13) -0.0009(12) C12 0.0150(14) 0.0172(16) 0.0221(18) -0.0025(14) -0.0014(13) 0.0010(11) C13 0.0101(13) 0.0192(16) 0.0209(17) 0.0016(13) -0.0028(12) -0.0003(11) C14 0.0244(16) 0.0213(17) 0.0250(19) -0.0030(15) -0.0017(14) 0.0036(13) C15 0.0323(17) 0.0182(17) 0.033(2) 0.0001(15) -0.0028(15) 0.0009(13) C16 0.0271(16) 0.0212(18) 0.030(2) 0.0076(15) -0.0068(15) -0.0007(13) C17 0.0113(13) 0.0246(17) 0.0221(17) 0.0041(14) -0.0033(12) -0.0007(12) C18 0.0170(14) 0.0262(18) 0.0209(17) 0.0032(14) -0.0024(13) -0.0008(12) C19 0.040(2) 0.033(2) 0.030(2) 0.0067(17) -0.0032(16) -0.0095(15) C20 0.055(2) 0.053(3) 0.027(2) 0.0110(19) 0.0015(18) -0.011(2) C21 0.043(2) 0.052(2) 0.0122(18) -0.0007(17) -0.0040(16) 0.0015(17) C22 0.0305(17) 0.032(2) 0.0197(19) -0.0049(16) -0.0050(14) 0.0014(14) C23 0.0200(15) 0.0238(17) 0.031(2) 0.0036(15) -0.0053(14) -0.0014(12) C24 0.0213(15) 0.0266(18) 0.032(2) -0.0005(15) -0.0083(14) 0.0032(13) C25 0.0160(15) 0.034(2) 0.032(2) -0.0039(16) -0.0024(14) 0.0012(13) C26 0.0194(15) 0.0305(19) 0.0259(19) -0.0017(15) 0.0016(14) 0.0003(13) C27 0.0163(14) 0.0187(16) 0.0228(17) -0.0056(14) -0.0009(13) -0.0012(12) C28 0.0188(14) 0.0164(16) 0.0212(17) -0.0033(13) -0.0019(13) -0.0025(12) C29 0.0215(15) 0.0251(18) 0.032(2) -0.0014(15) 0.0038(14) -0.0035(13) C30 0.0272(17) 0.031(2) 0.029(2) 0.0065(16) 0.0016(15) -0.0053(14) C31 0.0233(16) 0.0215(17) 0.0284(19) 0.0020(15) -0.0043(14) -0.0012(13) C32 0.0173(14) 0.0185(16) 0.0232(17) -0.0042(14) -0.0032(13) -0.0007(12) C33 0.0246(13) 0.0141(15) 0.0203(16) 0.0022(13) -0.0056(14) -0.0003(12) Cl3 0.0285(4) 0.0314(5) 0.0272(5) -0.0022(4) -0.0005(3) -0.0018(3) O3 0.0357(13) 0.0477(16) 0.0298(14) 0.0113(12) 0.0008(11) -0.0099(11) O4 0.0373(15) 0.0440(17) 0.099(3) 0.0183(16) 0.0332(15) 0.0096(12) O2 0.088(2) 0.063(2) 0.056(2) 0.0303(17) -0.0228(18) -0.0222(17) O1 0.0413(16) 0.072(2) 0.114(3) -0.060(2) 0.0249(17) -0.0120(15) Cl2 0.0277(4) 0.0255(4) 0.0305(5) -0.0013(4) -0.0041(3) 0.0025(3) O5 0.0614(17) 0.0428(17) 0.060(2) 0.0103(14) 0.0148(15) -0.0114(13) O6 0.183(4) 0.0373(18) 0.0351(18) -0.0006(14) -0.035(2) -0.018(2) O7 0.0286(15) 0.076(2) 0.151(4) 0.029(2) -0.0060(18) -0.0028(15) O8 0.080(2) 0.051(2) 0.083(2) -0.0327(18) 0.0018(18) 0.0130(17) C100 0.046(2) 0.079(4) 0.056(3) 0.017(3) 0.003(2) 0.010(2) C101 0.072(3) 0.051(3) 0.073(3) 0.014(3) -0.044(3) -0.021(2) N100 0.125(4) 0.057(3) 0.181(6) 0.035(3) -0.102(4) -0.032(3) C102 0.106(4) 0.060(3) 0.071(4) 0.025(3) -0.047(3) -0.026(3) C103 0.064(3) 0.035(2) 0.100(4) -0.022(3) -0.052(3) 0.014(2) C104 0.047(2) 0.056(3) 0.081(3) -0.038(3) 0.023(2) -0.023(2) C105 0.127(5) 0.046(3) 0.060(3) -0.003(3) 0.020(3) -0.022(3) O100 0.0285(12) 0.0375(15) 0.0562(18) -0.0055(13) -0.0083(12) -0.0002(11) _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 N6 2.130(2) . ? Co1 N3 2.133(3) . ? Co1 N1 2.135(3) . ? Co1 N5 2.179(2) . ? Co1 N4 2.194(2) . ? Co1 N2 2.242(2) . ? N1 C1 1.341(4) . ? N1 C5 1.352(4) . ? N2 C6 1.352(4) . ? N2 C10 1.359(4) . ? N3 C22 1.344(4) . ? N3 C18 1.348(4) . ? N4 C17 1.348(4) . ? N4 C13 1.357(4) . ? N5 C28 1.355(4) . ? N5 C32 1.356(4) . ? N6 C23 1.340(4) . ? N6 C27 1.348(4) . ? C1 C2 1.383(4) . ? C1 H1 0.9500 . ? C2 C3 1.369(4) . ? C2 H2 0.9500 . ? C3 C4 1.388(4) . ? C3 H3 0.9500 . ? C4 C5 1.381(4) . ? C4 H4 0.9500 . ? C5 C6 1.478(4) . ? C6 C7 1.386(4) . ? C7 C8 1.388(4) . ? C7 H7 0.9500 . ? C8 C9 1.371(4) . ? C8 H8 0.9500 . ? C9 C10 1.397(4) . ? C9 H9 0.9500 . ? C10 C11 1.427(4) . ? C11 C12 1.195(4) 2_656 ? C12 C11 1.195(4) 2_656 ? C12 C13 1.432(4) . ? C13 C14 1.392(4) . ? C14 C15 1.372(4) . ? C14 H14 0.9500 . ? C15 C16 1.373(5) . ? C15 H15 0.9500 . ? C16 C17 1.392(4) . ? C16 H16 0.9500 . ? C17 C18 1.477(4) . ? C18 C19 1.390(4) . ? C19 C20 1.378(5) . ? C19 H19 0.9500 . ? C20 C21 1.366(5) . ? C20 H20 0.9500 . ? C21 C22 1.374(5) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.381(4) . ? C23 H23 0.9500 . ? C24 C25 1.380(5) . ? C24 H24 0.9500 . ? C25 C26 1.384(4) . ? C25 H25 0.9500 . ? C26 C27 1.392(4) . ? C26 H26 0.9500 . ? C27 C28 1.480(4) . ? C28 C29 1.383(4) . ? C29 C30 1.374(4) . ? C29 H29 0.9500 . ? C30 C31 1.370(4) . ? C30 H30 0.9500 . ? C31 C32 1.388(4) . ? C31 H31 0.9500 . ? C32 C33 1.429(4) . ? C33 C33 1.198(6) 2_656 ? Cl3 O4 1.405(3) . ? Cl3 O2 1.417(3) . ? Cl3 O1 1.423(3) . ? Cl3 O3 1.432(2) . ? Cl2 O7 1.400(3) . ? Cl2 O6 1.413(3) . ? Cl2 O8 1.418(3) . ? Cl2 O5 1.419(3) . ? C100 C101 1.405(6) . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? C101 N100 1.119(6) . ? C102 C103 1.512(7) . ? C102 H10D 0.9800 . ? C102 H10E 0.9800 . ? C102 H10F 0.9800 . ? C103 O100 1.421(5) . ? C103 H10G 0.9900 . ? C103 H10H 0.9900 . ? C104 O100 1.426(5) . ? C104 C105 1.484(7) . ? C104 H10I 0.9900 . ? C104 H10J 0.9900 . ? C105 H10K 0.9800 . ? C105 H10L 0.9800 . ? C105 H10M 0.9800 . ? 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 N6 Co1 N3 92.46(9) . . ? N6 Co1 N1 96.55(9) . . ? N3 Co1 N1 96.31(10) . . ? N6 Co1 N5 76.05(9) . . ? N3 Co1 N5 168.49(9) . . ? N1 Co1 N5 84.42(9) . . ? N6 Co1 N4 85.77(9) . . ? N3 Co1 N4 76.93(9) . . ? N1 Co1 N4 172.96(9) . . ? N5 Co1 N4 102.59(9) . . ? N6 Co1 N2 168.93(9) . . ? N3 Co1 N2 80.98(9) . . ? N1 Co1 N2 75.48(9) . . ? N5 Co1 N2 110.23(9) . . ? N4 Co1 N2 101.27(8) . . ? C1 N1 C5 117.5(3) . . ? C1 N1 Co1 125.0(2) . . ? C5 N1 Co1 117.07(19) . . ? C6 N2 C10 117.0(2) . . ? C6 N2 Co1 111.52(18) . . ? C10 N2 Co1 126.72(19) . . ? C22 N3 C18 118.6(3) . . ? C22 N3 Co1 125.3(2) . . ? C18 N3 Co1 115.5(2) . . ? C17 N4 C13 116.6(3) . . ? C17 N4 Co1 112.96(19) . . ? C13 N4 Co1 129.12(19) . . ? C28 N5 C32 117.3(2) . . ? C28 N5 Co1 115.01(19) . . ? C32 N5 Co1 127.37(19) . . ? C23 N6 C27 118.4(2) . . ? C23 N6 Co1 124.6(2) . . ? C27 N6 Co1 116.98(19) . . ? N1 C1 C2 122.7(3) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.3(3) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 119.1(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 118.6(3) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 122.7(3) . . ? N1 C5 C6 115.0(3) . . ? C4 C5 C6 122.3(3) . . ? N2 C6 C7 122.9(3) . . ? N2 C6 C5 115.4(3) . . ? C7 C6 C5 121.6(3) . . ? C6 C7 C8 118.9(3) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C9 C8 C7 119.3(3) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 118.8(3) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N2 C10 C9 122.7(3) . . ? N2 C10 C11 117.3(3) . . ? C9 C10 C11 120.0(3) . . ? C12 C11 C10 171.9(3) 2_656 . ? C11 C12 C13 169.1(3) 2_656 . ? N4 C13 C14 123.3(3) . . ? N4 C13 C12 118.7(3) . . ? C14 C13 C12 117.8(3) . . ? C15 C14 C13 118.9(3) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C14 C15 C16 118.9(3) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C15 C16 C17 119.7(3) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? N4 C17 C16 122.7(3) . . ? N4 C17 C18 116.3(3) . . ? C16 C17 C18 121.0(3) . . ? N3 C18 C19 121.7(3) . . ? N3 C18 C17 116.0(3) . . ? C19 C18 C17 122.3(3) . . ? C20 C19 C18 118.4(3) . . ? C20 C19 H19 120.8 . . ? C18 C19 H19 120.8 . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 119.1(3) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? N3 C22 C21 122.2(3) . . ? N3 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? N6 C23 C24 123.1(3) . . ? N6 C23 H23 118.5 . . ? C24 C23 H23 118.5 . . ? C25 C24 C23 118.3(3) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? C24 C25 C26 119.6(3) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 118.7(3) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? N6 C27 C26 121.8(3) . . ? N6 C27 C28 115.8(2) . . ? C26 C27 C28 122.4(3) . . ? N5 C28 C29 121.8(3) . . ? N5 C28 C27 115.7(3) . . ? C29 C28 C27 122.5(3) . . ? C30 C29 C28 120.3(3) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 118.7(3) . . ? C31 C30 H30 120.6 . . ? C29 C30 H30 120.6 . . ? C30 C31 C32 119.1(3) . . ? C30 C31 H31 120.5 . . ? C32 C31 H31 120.5 . . ? N5 C32 C31 122.8(3) . . ? N5 C32 C33 117.0(3) . . ? C31 C32 C33 120.0(3) . . ? C33 C33 C32 173.3(4) 2_656 . ? O4 Cl3 O2 113.6(2) . . ? O4 Cl3 O1 108.00(18) . . ? O2 Cl3 O1 107.6(2) . . ? O4 Cl3 O3 110.07(16) . . ? O2 Cl3 O3 108.27(16) . . ? O1 Cl3 O3 109.23(18) . . ? O7 Cl2 O6 111.8(3) . . ? O7 Cl2 O8 107.2(2) . . ? O6 Cl2 O8 107.6(2) . . ? O7 Cl2 O5 109.97(19) . . ? O6 Cl2 O5 108.53(18) . . ? O8 Cl2 O5 111.83(19) . . ? C101 C100 H10A 109.5 . . ? C101 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C101 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? N100 C101 C100 177.5(7) . . ? C103 C102 H10D 109.5 . . ? C103 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C103 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? O100 C103 C102 109.3(4) . . ? O100 C103 H10G 109.8 . . ? C102 C103 H10G 109.8 . . ? O100 C103 H10H 109.8 . . ? C102 C103 H10H 109.8 . . ? H10G C103 H10H 108.3 . . ? O100 C104 C105 109.4(4) . . ? O100 C104 H10I 109.8 . . ? C105 C104 H10I 109.8 . . ? O100 C104 H10J 109.8 . . ? C105 C104 H10J 109.8 . . ? H10I C104 H10J 108.2 . . ? C104 C105 H10K 109.5 . . ? C104 C105 H10L 109.5 . . ? H10K C105 H10L 109.5 . . ? C104 C105 H10M 109.5 . . ? H10K C105 H10M 109.5 . . ? H10L C105 H10M 109.5 . . ? C103 O100 C104 113.7(3) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.964 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.073 # Attachment 'Cmpd_7-756147R2.cif' data_n259 _database_code_depnum_ccdc_archive 'CCDC 756147' #TrackingRef 'Cmpd_7-756147R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H44 Co2 N12 O2, 2(Cl O4), O' _chemical_formula_sum 'C66 H44 Cl2 Co2 N12 O11' _chemical_formula_weight 1369.89 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 P2(1)/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 10.2991(5) _cell_length_b 23.2804(10) _cell_length_c 12.4289(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.073(2) _cell_angle_gamma 90.00 _cell_volume 2877.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21210 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 26.02 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8961 _exptl_absorpt_correction_T_max 0.9707 _exptl_absorpt_process_details 'Bruker Apex2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 KappaApex2 CCD' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21210 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 26.02 _reflns_number_total 5652 _reflns_number_gt 3369 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2' _computing_cell_refinement 'Bruker Apex2' _computing_data_reduction 'Bruker Apex2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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.Partial disorder near ClO4 has been left unmodeled ; _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^)+(0.1472P)^2^+4.9323P] 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 5652 _refine_ls_number_parameters 426 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.1399 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.2541 _refine_ls_wR_factor_gt 0.2122 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.44040(9) 0.03898(4) 0.15017(7) 0.0318(3) Uani 1 1 d . . . N1 N 0.6144(6) 0.0087(2) 0.1872(4) 0.0339(12) Uani 1 1 d . . . N2 N 0.4908(6) 0.0567(2) 0.3178(4) 0.0384(14) Uani 1 1 d . . . N3 N 0.4923(6) 0.1146(2) 0.1178(4) 0.0394(14) Uani 1 1 d . . . N4 N 0.2657(6) 0.0718(2) 0.1233(4) 0.0356(13) Uani 1 1 d . . . N5 N 0.1333(7) -0.1383(3) 0.1661(5) 0.0469(15) Uani 1 1 d . . . N6 N -0.0396(8) -0.2715(3) 0.1194(6) 0.068(2) Uani 1 1 d . . . O1 O 0.3881(5) -0.03580(19) 0.1796(4) 0.0398(11) Uani 1 1 d . . . C0 C 0.4418(7) 0.0134(3) 0.0005(5) 0.0337(15) Uani 1 1 d . . . C1 C 0.6588(7) -0.0183(3) 0.1069(5) 0.0335(15) Uani 1 1 d . . . C2 C 0.7826(7) -0.0442(3) 0.1353(6) 0.0442(18) Uani 1 1 d . . . H2 H 0.8144 -0.0641 0.0804 0.053 Uiso 1 1 calc R . . C3 C 0.8621(8) -0.0413(4) 0.2452(6) 0.052(2) Uani 1 1 d . . . H3 H 0.9490 -0.0582 0.2646 0.062 Uiso 1 1 calc R . . C4 C 0.8144(8) -0.0139(3) 0.3251(6) 0.0485(19) Uani 1 1 d . . . H4 H 0.8676 -0.0115 0.3999 0.058 Uiso 1 1 calc R . . C5 C 0.6879(7) 0.0102(3) 0.2946(5) 0.0387(16) Uani 1 1 d . . . C6 C 0.6175(8) 0.0382(3) 0.3688(5) 0.0418(17) Uani 1 1 d . . . C7 C 0.6730(9) 0.0454(4) 0.4822(6) 0.058(2) Uani 1 1 d . . . H7 H 0.7625 0.0337 0.5168 0.069 Uiso 1 1 calc R . . C8 C 0.5918(10) 0.0705(4) 0.5432(6) 0.067(3) Uani 1 1 d . . . H8 H 0.6261 0.0762 0.6211 0.080 Uiso 1 1 calc R . . C9 C 0.4661(10) 0.0866(4) 0.4930(7) 0.062(2) Uani 1 1 d . . . H9 H 0.4103 0.1026 0.5354 0.075 Uiso 1 1 calc R . . C10 C 0.4173(8) 0.0799(3) 0.3781(6) 0.0463(18) Uani 1 1 d . . . H10 H 0.3287 0.0924 0.3426 0.056 Uiso 1 1 calc R . . C11 C 0.6123(9) 0.1313(3) 0.1065(7) 0.053(2) Uani 1 1 d . . . H11 H 0.6828 0.1041 0.1145 0.064 Uiso 1 1 calc R . . C12 C 0.6347(10) 0.1887(4) 0.0829(7) 0.061(2) Uani 1 1 d . . . H12 H 0.7201 0.2000 0.0743 0.073 Uiso 1 1 calc R . . C13 C 0.5359(10) 0.2283(4) 0.0723(7) 0.063(2) Uani 1 1 d . . . H13 H 0.5517 0.2672 0.0567 0.076 Uiso 1 1 calc R . . C14 C 0.4126(10) 0.2116(4) 0.0844(7) 0.061(2) Uani 1 1 d . . . H14 H 0.3431 0.2392 0.0786 0.073 Uiso 1 1 calc R . . C15 C 0.3898(8) 0.1546(3) 0.1049(6) 0.0439(18) Uani 1 1 d . . . C16 C 0.2619(8) 0.1304(3) 0.1110(5) 0.0410(17) Uani 1 1 d . . . C17 C 0.1448(8) 0.1608(3) 0.1007(6) 0.0469(19) Uani 1 1 d . . . H17 H 0.1433 0.2013 0.0910 0.056 Uiso 1 1 calc R . . C18 C 0.0306(8) 0.1319(3) 0.1046(6) 0.0483(19) Uani 1 1 d . . . H18 H -0.0510 0.1521 0.0988 0.058 Uiso 1 1 calc R . . C19 C 0.0350(8) 0.0733(3) 0.1169(6) 0.0442(17) Uani 1 1 d . . . H19 H -0.0446 0.0533 0.1190 0.053 Uiso 1 1 calc R . . C20 C 0.1530(7) 0.0426(3) 0.1265(5) 0.0355(15) Uani 1 1 d . . . C21 C 0.1563(8) -0.0190(3) 0.1372(6) 0.0440(17) Uani 1 1 d . . . H21 H 0.0719 -0.0377 0.1266 0.053 Uiso 1 1 calc R . . C22 C 0.2663(7) -0.0531(3) 0.1608(5) 0.0375(16) Uani 1 1 d . . . C23 C 0.2535(8) -0.1172(3) 0.1697(5) 0.0419(17) Uani 1 1 d . . . C24 C 0.3685(9) -0.1509(3) 0.1858(7) 0.056(2) Uani 1 1 d . . . H24 H 0.4536 -0.1336 0.1915 0.067 Uiso 1 1 calc R . . C25 C 0.3568(11) -0.2095(4) 0.1932(9) 0.071(3) Uani 1 1 d . . . H25 H 0.4340 -0.2334 0.2069 0.085 Uiso 1 1 calc R . . C26 C 0.2307(11) -0.2325(4) 0.1804(8) 0.066(3) Uani 1 1 d . . . H26 H 0.2188 -0.2730 0.1788 0.079 Uiso 1 1 calc R . . C27 C 0.1204(9) -0.1961(3) 0.1699(6) 0.052(2) Uani 1 1 d . . . C28 C -0.0151(10) -0.2192(4) 0.1633(7) 0.062(2) Uani 1 1 d . . . C29 C -0.1075(9) -0.1878(4) 0.2014(9) 0.073(3) Uani 1 1 d . . . H29 H -0.0862 -0.1500 0.2294 0.087 Uiso 1 1 calc R . . C30 C -0.2326(11) -0.2116(5) 0.1990(11) 0.093(4) Uani 1 1 d . . . H30 H -0.2977 -0.1911 0.2256 0.112 Uiso 1 1 calc R . . C31 C -0.2577(13) -0.2670(5) 0.1555(11) 0.106(5) Uani 1 1 d . . . H31 H -0.3406 -0.2856 0.1528 0.127 Uiso 1 1 calc R . . C32 C -0.1604(14) -0.2942(5) 0.1168(10) 0.088(3) Uani 1 1 d . . . H32 H -0.1798 -0.3315 0.0860 0.105 Uiso 1 1 calc R . . Cl1 Cl 0.5425(3) 0.38527(10) 0.9245(2) 0.0844(9) Uani 1 1 d D . . O4 O 0.5985(6) 0.4381(2) 0.9040(5) 0.0656(15) Uani 1 1 d DU . . O7 O 0.4800(7) 0.3863(3) 1.0075(6) 0.0877(19) Uani 1 1 d DU . . O5 O 0.5975(8) 0.3391(3) 0.8924(7) 0.104(2) Uani 1 1 d DU . . O6 O 0.4057(8) 0.3827(4) 0.8233(7) 0.120(2) Uani 1 1 d DU . . O3 O 0.3820(12) 0.2200(5) 0.5651(9) 0.063(3) Uani 0.50 1 d P . . 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 0.0442(6) 0.0306(5) 0.0198(4) 0.0001(3) 0.0067(4) -0.0038(4) N1 0.047(3) 0.033(3) 0.020(3) 0.002(2) 0.005(2) -0.001(3) N2 0.055(4) 0.038(3) 0.023(3) -0.003(2) 0.011(3) -0.006(3) N3 0.052(4) 0.039(3) 0.028(3) -0.004(2) 0.012(3) -0.010(3) N4 0.056(4) 0.032(3) 0.020(3) 0.000(2) 0.012(3) 0.001(3) N5 0.060(4) 0.040(3) 0.037(3) 0.003(3) 0.004(3) -0.004(3) N6 0.087(6) 0.035(4) 0.061(5) 0.005(3) -0.016(4) -0.015(4) O1 0.053(3) 0.037(3) 0.031(2) 0.002(2) 0.012(2) -0.004(2) C0 0.046(4) 0.032(3) 0.022(3) 0.004(3) 0.008(3) -0.007(3) C1 0.040(4) 0.036(3) 0.023(3) -0.003(3) 0.007(3) -0.006(3) C2 0.046(4) 0.051(5) 0.033(4) 0.000(3) 0.005(3) 0.006(4) C3 0.049(5) 0.066(5) 0.036(4) 0.008(4) 0.003(3) 0.004(4) C4 0.054(5) 0.061(5) 0.024(3) 0.004(3) -0.002(3) -0.006(4) C5 0.046(4) 0.040(4) 0.025(3) 0.002(3) -0.001(3) -0.002(3) C6 0.055(4) 0.045(4) 0.022(3) -0.003(3) 0.004(3) -0.005(4) C7 0.067(6) 0.070(6) 0.027(4) -0.002(4) -0.004(4) -0.002(4) C8 0.088(7) 0.081(7) 0.023(4) -0.016(4) 0.000(4) 0.008(5) C9 0.090(7) 0.064(6) 0.037(4) -0.007(4) 0.024(5) 0.007(5) C10 0.065(5) 0.048(4) 0.031(4) -0.001(3) 0.020(4) 0.003(4) C11 0.060(5) 0.044(4) 0.052(5) 0.000(4) 0.010(4) -0.011(4) C12 0.066(6) 0.057(5) 0.058(5) 0.013(4) 0.012(4) -0.020(5) C13 0.081(7) 0.057(5) 0.054(5) 0.001(4) 0.022(5) -0.014(5) C14 0.078(6) 0.048(5) 0.054(5) 0.004(4) 0.013(5) 0.006(4) C15 0.070(5) 0.034(4) 0.027(4) 0.003(3) 0.011(3) -0.004(4) C16 0.060(5) 0.041(4) 0.022(3) -0.004(3) 0.011(3) -0.001(4) C17 0.067(5) 0.035(4) 0.037(4) -0.003(3) 0.010(4) 0.005(4) C18 0.046(5) 0.053(5) 0.042(4) -0.003(4) 0.003(3) 0.010(4) C19 0.046(4) 0.046(4) 0.038(4) -0.002(3) 0.006(3) -0.005(3) C20 0.041(4) 0.043(4) 0.024(3) -0.003(3) 0.010(3) -0.004(3) C21 0.054(5) 0.043(4) 0.034(4) -0.003(3) 0.009(3) -0.004(4) C22 0.049(5) 0.042(4) 0.021(3) -0.001(3) 0.008(3) -0.004(3) C23 0.065(5) 0.039(4) 0.022(3) -0.001(3) 0.011(3) -0.006(4) C24 0.067(6) 0.044(4) 0.063(5) 0.008(4) 0.029(4) -0.002(4) C25 0.086(7) 0.048(5) 0.096(7) 0.020(5) 0.052(6) 0.011(5) C26 0.102(8) 0.036(4) 0.067(6) 0.010(4) 0.035(5) 0.006(5) C27 0.081(6) 0.037(4) 0.037(4) 0.003(3) 0.015(4) -0.005(4) C28 0.077(6) 0.041(4) 0.055(5) 0.014(4) -0.007(5) -0.013(4) C29 0.053(6) 0.055(6) 0.099(8) 0.012(5) 0.000(5) -0.010(5) C30 0.067(7) 0.073(7) 0.127(10) 0.034(7) 0.004(6) -0.005(6) C31 0.087(9) 0.082(8) 0.112(10) 0.035(7) -0.038(7) -0.046(7) C32 0.100(9) 0.048(6) 0.096(9) 0.006(5) -0.008(7) -0.008(6) Cl1 0.126(2) 0.0477(13) 0.107(2) -0.0193(12) 0.0786(19) -0.0291(14) O4 0.085(4) 0.047(3) 0.069(3) -0.001(3) 0.028(3) -0.023(3) O7 0.106(4) 0.082(4) 0.093(4) -0.012(3) 0.060(4) -0.031(3) O5 0.134(5) 0.070(4) 0.123(5) -0.011(4) 0.061(4) -0.002(4) O6 0.121(5) 0.117(5) 0.114(5) -0.013(4) 0.016(4) -0.040(4) O3 0.087(9) 0.051(6) 0.050(6) 0.006(5) 0.018(6) 0.040(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 Co1 N1 1.869(6) . ? Co1 O1 1.886(5) . ? Co1 N4 1.903(6) . ? Co1 N3 1.914(6) . ? Co1 C0 1.957(6) . ? Co1 N2 2.054(5) . ? N1 C5 1.354(8) . ? N1 C1 1.355(8) . ? N2 C10 1.312(9) . ? N2 C6 1.364(10) . ? N3 C11 1.337(10) . ? N3 C15 1.384(10) . ? N4 C20 1.354(9) . ? N4 C16 1.373(9) . ? N5 C23 1.321(10) . ? N5 C27 1.355(9) . ? N6 C28 1.333(11) . ? N6 C32 1.344(14) . ? O1 C22 1.280(8) . ? C0 C0 1.355(14) 3_655 ? C0 C1 1.466(9) 3_655 ? C1 C2 1.371(10) . ? C1 C0 1.466(9) 3_655 ? C2 C3 1.400(10) . ? C2 H2 0.9500 . ? C3 C4 1.374(11) . ? C3 H3 0.9500 . ? C4 C5 1.377(10) . ? C4 H4 0.9500 . ? C5 C6 1.466(10) . ? C6 C7 1.386(10) . ? C7 C8 1.396(12) . ? C7 H7 0.9500 . ? C8 C9 1.337(13) . ? C8 H8 0.9500 . ? C9 C10 1.394(11) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.400(11) . ? C11 H11 0.9500 . ? C12 C13 1.354(13) . ? C12 H12 0.9500 . ? C13 C14 1.373(12) . ? C13 H13 0.9500 . ? C14 C15 1.385(11) . ? C14 H14 0.9500 . ? C15 C16 1.452(11) . ? C16 C17 1.375(11) . ? C17 C18 1.368(11) . ? C17 H17 0.9500 . ? C18 C19 1.372(10) . ? C18 H18 0.9500 . ? C19 C20 1.389(10) . ? C19 H19 0.9500 . ? C20 C21 1.439(10) . ? C21 C22 1.352(10) . ? C21 H21 0.9500 . ? C22 C23 1.505(10) . ? C23 C24 1.390(11) . ? C24 C25 1.375(11) . ? C24 H24 0.9500 . ? C25 C26 1.375(13) . ? C25 H25 0.9500 . ? C26 C27 1.396(12) . ? C26 H26 0.9500 . ? C27 C28 1.478(12) . ? C28 C29 1.377(14) . ? C29 C30 1.396(14) . ? C29 H29 0.9500 . ? C30 C31 1.396(17) . ? C30 H30 0.9500 . ? C31 C32 1.374(18) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? Cl1 O5 1.324(7) . ? Cl1 O7 1.351(6) . ? Cl1 O4 1.409(5) . ? Cl1 O6 1.627(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 O1 84.7(2) . . ? N1 Co1 N4 175.8(2) . . ? O1 Co1 N4 95.7(2) . . ? N1 Co1 N3 95.5(3) . . ? O1 Co1 N3 179.1(2) . . ? N4 Co1 N3 84.1(3) . . ? N1 Co1 C0 82.9(3) . . ? O1 Co1 C0 88.7(2) . . ? N4 Co1 C0 101.3(2) . . ? N3 Co1 C0 90.5(2) . . ? N1 Co1 N2 81.5(2) . . ? O1 Co1 N2 89.9(2) . . ? N4 Co1 N2 94.3(2) . . ? N3 Co1 N2 91.0(2) . . ? C0 Co1 N2 164.4(3) . . ? C5 N1 C1 121.9(6) . . ? C5 N1 Co1 119.2(5) . . ? C1 N1 Co1 118.6(4) . . ? C10 N2 C6 119.3(6) . . ? C10 N2 Co1 129.1(5) . . ? C6 N2 Co1 111.5(4) . . ? C11 N3 C15 119.4(6) . . ? C11 N3 Co1 127.3(5) . . ? C15 N3 Co1 113.4(5) . . ? C20 N4 C16 120.2(6) . . ? C20 N4 Co1 124.9(5) . . ? C16 N4 Co1 114.6(5) . . ? C23 N5 C27 117.9(7) . . ? C28 N6 C32 116.4(10) . . ? C22 O1 Co1 124.8(5) . . ? C0 C0 C1 116.4(7) 3_655 3_655 ? C0 C0 Co1 112.0(6) 3_655 . ? C1 C0 Co1 131.6(5) 3_655 . ? N1 C1 C2 118.9(6) . . ? N1 C1 C0 109.9(6) . 3_655 ? C2 C1 C0 131.1(6) . 3_655 ? C1 C2 C3 119.9(7) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 119.9(7) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 118.7(7) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 120.5(6) . . ? N1 C5 C6 113.0(6) . . ? C4 C5 C6 126.5(6) . . ? N2 C6 C7 121.7(7) . . ? N2 C6 C5 114.7(6) . . ? C7 C6 C5 123.5(7) . . ? C6 C7 C8 117.2(8) . . ? C6 C7 H7 121.4 . . ? C8 C7 H7 121.4 . . ? C9 C8 C7 120.6(7) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 119.6(8) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 121.6(8) . . ? N2 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? N3 C11 C12 120.5(8) . . ? N3 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 120.6(8) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 119.4(8) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C13 C14 C15 119.8(9) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? N3 C15 C14 120.4(7) . . ? N3 C15 C16 114.1(6) . . ? C14 C15 C16 125.5(8) . . ? N4 C16 C17 121.4(7) . . ? N4 C16 C15 113.0(6) . . ? C17 C16 C15 125.5(7) . . ? C18 C17 C16 119.0(7) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C19 119.3(7) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 121.7(7) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? N4 C20 C19 118.4(6) . . ? N4 C20 C21 120.2(6) . . ? C19 C20 C21 121.3(7) . . ? C22 C21 C20 127.1(7) . . ? C22 C21 H21 116.5 . . ? C20 C21 H21 116.5 . . ? O1 C22 C21 125.6(7) . . ? O1 C22 C23 113.6(6) . . ? C21 C22 C23 120.9(7) . . ? N5 C23 C24 123.4(7) . . ? N5 C23 C22 117.8(7) . . ? C24 C23 C22 118.7(7) . . ? C25 C24 C23 118.8(8) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C24 C25 C26 118.5(9) . . ? C24 C25 H25 120.8 . . ? C26 C25 H25 120.8 . . ? C25 C26 C27 119.6(8) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? N5 C27 C26 121.4(8) . . ? N5 C27 C28 117.3(8) . . ? C26 C27 C28 121.3(7) . . ? N6 C28 C29 123.5(9) . . ? N6 C28 C27 115.4(9) . . ? C29 C28 C27 121.1(8) . . ? C28 C29 C30 119.9(10) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C29 C30 C31 116.9(12) . . ? C29 C30 H30 121.5 . . ? C31 C30 H30 121.5 . . ? C32 C31 C30 118.8(11) . . ? C32 C31 H31 120.6 . . ? C30 C31 H31 120.6 . . ? N6 C32 C31 124.5(10) . . ? N6 C32 H32 117.7 . . ? C31 C32 H32 117.7 . . ? O5 Cl1 O7 124.8(5) . . ? O5 Cl1 O4 115.2(4) . . ? O7 Cl1 O4 115.0(4) . . ? O5 Cl1 O6 95.1(5) . . ? O7 Cl1 O6 95.9(5) . . ? O4 Cl1 O6 101.8(4) . . ? 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 O1 Co1 N1 C5 -89.4(5) . . . . ? N3 Co1 N1 C5 91.5(5) . . . . ? C0 Co1 N1 C5 -178.7(5) . . . . ? N2 Co1 N1 C5 1.3(5) . . . . ? O1 Co1 N1 C1 85.2(5) . . . . ? N3 Co1 N1 C1 -93.9(5) . . . . ? C0 Co1 N1 C1 -4.2(5) . . . . ? N2 Co1 N1 C1 175.8(5) . . . . ? N1 Co1 N2 C10 -177.2(6) . . . . ? O1 Co1 N2 C10 -92.5(6) . . . . ? N4 Co1 N2 C10 3.2(6) . . . . ? N3 Co1 N2 C10 87.3(6) . . . . ? C0 Co1 N2 C10 -177.2(8) . . . . ? N1 Co1 N2 C6 -0.5(5) . . . . ? O1 Co1 N2 C6 84.2(5) . . . . ? N4 Co1 N2 C6 179.9(5) . . . . ? N3 Co1 N2 C6 -95.9(5) . . . . ? C0 Co1 N2 C6 -0.5(11) . . . . ? N1 Co1 N3 C11 11.3(6) . . . . ? N4 Co1 N3 C11 -172.8(6) . . . . ? C0 Co1 N3 C11 -71.5(6) . . . . ? N2 Co1 N3 C11 92.9(6) . . . . ? N1 Co1 N3 C15 -169.1(4) . . . . ? N4 Co1 N3 C15 6.8(4) . . . . ? C0 Co1 N3 C15 108.1(5) . . . . ? N2 Co1 N3 C15 -87.5(5) . . . . ? O1 Co1 N4 C20 -1.1(5) . . . . ? N3 Co1 N4 C20 178.0(5) . . . . ? C0 Co1 N4 C20 88.7(5) . . . . ? N2 Co1 N4 C20 -91.5(5) . . . . ? O1 Co1 N4 C16 172.3(4) . . . . ? N3 Co1 N4 C16 -8.6(4) . . . . ? C0 Co1 N4 C16 -97.9(4) . . . . ? N2 Co1 N4 C16 82.0(4) . . . . ? N1 Co1 O1 C22 -172.5(5) . . . . ? N4 Co1 O1 C22 11.7(5) . . . . ? C0 Co1 O1 C22 -89.5(5) . . . . ? N2 Co1 O1 C22 106.0(5) . . . . ? N1 Co1 C0 C0 2.2(6) . . . 3_655 ? O1 Co1 C0 C0 -82.7(7) . . . 3_655 ? N4 Co1 C0 C0 -178.2(6) . . . 3_655 ? N3 Co1 C0 C0 97.7(7) . . . 3_655 ? N2 Co1 C0 C0 2.2(14) . . . 3_655 ? N1 Co1 C0 C1 -178.0(6) . . . 3_655 ? O1 Co1 C0 C1 97.1(6) . . . 3_655 ? N4 Co1 C0 C1 1.6(7) . . . 3_655 ? N3 Co1 C0 C1 -82.5(6) . . . 3_655 ? N2 Co1 C0 C1 -178.0(7) . . . 3_655 ? C5 N1 C1 C2 -1.0(10) . . . . ? Co1 N1 C1 C2 -175.4(5) . . . . ? C5 N1 C1 C0 179.3(6) . . . 3_655 ? Co1 N1 C1 C0 4.9(7) . . . 3_655 ? N1 C1 C2 C3 -1.5(11) . . . . ? C0 C1 C2 C3 178.2(7) 3_655 . . . ? C1 C2 C3 C4 1.8(12) . . . . ? C2 C3 C4 C5 0.2(12) . . . . ? C1 N1 C5 C4 3.0(10) . . . . ? Co1 N1 C5 C4 177.4(5) . . . . ? C1 N1 C5 C6 -176.1(6) . . . . ? Co1 N1 C5 C6 -1.7(8) . . . . ? C3 C4 C5 N1 -2.6(11) . . . . ? C3 C4 C5 C6 176.5(7) . . . . ? C10 N2 C6 C7 -2.7(11) . . . . ? Co1 N2 C6 C7 -179.8(6) . . . . ? C10 N2 C6 C5 176.8(6) . . . . ? Co1 N2 C6 C5 -0.3(7) . . . . ? N1 C5 C6 N2 1.2(9) . . . . ? C4 C5 C6 N2 -177.8(7) . . . . ? N1 C5 C6 C7 -179.2(7) . . . . ? C4 C5 C6 C7 1.7(12) . . . . ? N2 C6 C7 C8 2.4(12) . . . . ? C5 C6 C7 C8 -177.1(8) . . . . ? C6 C7 C8 C9 0.0(14) . . . . ? C7 C8 C9 C10 -1.9(15) . . . . ? C6 N2 C10 C9 0.7(11) . . . . ? Co1 N2 C10 C9 177.2(6) . . . . ? C8 C9 C10 N2 1.7(13) . . . . ? C15 N3 C11 C12 0.6(11) . . . . ? Co1 N3 C11 C12 -179.8(6) . . . . ? N3 C11 C12 C13 0.7(13) . . . . ? C11 C12 C13 C14 -0.3(13) . . . . ? C12 C13 C14 C15 -1.3(13) . . . . ? C11 N3 C15 C14 -2.2(10) . . . . ? Co1 N3 C15 C14 178.1(6) . . . . ? C11 N3 C15 C16 175.7(6) . . . . ? Co1 N3 C15 C16 -3.9(7) . . . . ? C13 C14 C15 N3 2.6(12) . . . . ? C13 C14 C15 C16 -175.1(7) . . . . ? C20 N4 C16 C17 -0.6(9) . . . . ? Co1 N4 C16 C17 -174.4(5) . . . . ? C20 N4 C16 C15 -177.7(5) . . . . ? Co1 N4 C16 C15 8.5(7) . . . . ? N3 C15 C16 N4 -2.9(8) . . . . ? C14 C15 C16 N4 174.9(7) . . . . ? N3 C15 C16 C17 -179.9(6) . . . . ? C14 C15 C16 C17 -2.0(11) . . . . ? N4 C16 C17 C18 1.0(10) . . . . ? C15 C16 C17 C18 177.8(6) . . . . ? C16 C17 C18 C19 -1.0(11) . . . . ? C17 C18 C19 C20 0.5(11) . . . . ? C16 N4 C20 C19 0.1(9) . . . . ? Co1 N4 C20 C19 173.2(5) . . . . ? C16 N4 C20 C21 178.8(6) . . . . ? Co1 N4 C20 C21 -8.0(8) . . . . ? C18 C19 C20 N4 0.0(10) . . . . ? C18 C19 C20 C21 -178.8(7) . . . . ? N4 C20 C21 C22 10.1(10) . . . . ? C19 C20 C21 C22 -171.1(7) . . . . ? Co1 O1 C22 C21 -13.2(9) . . . . ? Co1 O1 C22 C23 168.2(4) . . . . ? C20 C21 C22 O1 1.2(11) . . . . ? C20 C21 C22 C23 179.8(6) . . . . ? C27 N5 C23 C24 -5.1(10) . . . . ? C27 N5 C23 C22 177.6(6) . . . . ? O1 C22 C23 N5 171.4(6) . . . . ? C21 C22 C23 N5 -7.4(9) . . . . ? O1 C22 C23 C24 -6.1(9) . . . . ? C21 C22 C23 C24 175.2(7) . . . . ? N5 C23 C24 C25 3.1(12) . . . . ? C22 C23 C24 C25 -179.6(7) . . . . ? C23 C24 C25 C26 2.3(13) . . . . ? C24 C25 C26 C27 -5.4(14) . . . . ? C23 N5 C27 C26 1.8(11) . . . . ? C23 N5 C27 C28 -178.8(6) . . . . ? C25 C26 C27 N5 3.5(13) . . . . ? C25 C26 C27 C28 -176.0(8) . . . . ? C32 N6 C28 C29 -2.1(13) . . . . ? C32 N6 C28 C27 177.4(8) . . . . ? N5 C27 C28 N6 151.9(7) . . . . ? C26 C27 C28 N6 -28.7(11) . . . . ? N5 C27 C28 C29 -28.6(11) . . . . ? C26 C27 C28 C29 150.9(9) . . . . ? N6 C28 C29 C30 2.5(15) . . . . ? C27 C28 C29 C30 -177.1(9) . . . . ? C28 C29 C30 C31 -0.8(15) . . . . ? C29 C30 C31 C32 -1.0(16) . . . . ? C28 N6 C32 C31 0.2(15) . . . . ? C30 C31 C32 N6 1.3(18) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.192 _refine_diff_density_min -1.346 _refine_diff_density_rms 0.121 # Attachment 'Cmpd_8-756148R2.cif' data_n186p _database_code_depnum_ccdc_archive 'CCDC 756148' #TrackingRef 'Cmpd_8-756148R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C88 H56 Co4 N16 O4, 4(Cl O4)' _symmetry_space_group_name_Hall -P4bc _chemical_formula_sum 'C88 H56 Cl4 Co4 N16 O20' _chemical_formula_weight 2035.01 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 Tetragonal _symmetry_space_group_name_H-M P4(2)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 35.107(5) _cell_length_b 35.107(5) _cell_length_c 14.585(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17976(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 126603 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 27.53 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8256 _exptl_absorpt_coefficient_mu 0.924 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9215 _exptl_absorpt_correction_T_max 0.9818 _exptl_absorpt_process_details 'Bruker Apex2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 KappaApexII CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20616 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.0726 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.53 _reflns_number_total 20616 _reflns_number_gt 10752 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2' _computing_cell_refinement 'Bruker Apex2' _computing_data_reduction 'Bruker Apex2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All possibilities of twinning was checked. They didn't improve the model. In addition to big Co contained complex the structure model also contains some solvent molecules:4 independent molecules ClO4 which disordered and distributed along 5 places, 1 acetonitrile molecule distributed in 2 places with occupancy 0.5 and several water molecules. Other disordered water molecules can be also be in the structure and solvent accessible voids in the structure confirms this state. The ClO4 molecule containing Cl1 atom has occupancy factor 0.95257 .....................Cl2................................................0.93503 .....................Cl3................................................0.77537 .....................Cl4................................................0.90951 .....................Cl5................................................0.42752 As a result of several experiments and many attempts to process data applying different symmetry (both translational and point group symmetry) allow to conclude that the most of moieties surrounding Co-complex don't form periodical structure strictly enough and some of them form the periodical structure with lower symmetry. The presented structural model is determined by symmetry of Co-complex strongly dominating by its weight and number of variable parameters. The natural vagueness in the moiety's positions leads to the low quality of the structure model: (high R-factors, acetonitrile molecule isn't straight enough etc.). Nevertheless we consider that the model is sufficiently exactly confirms the structure of Co-contained complex which was the main purpose of the study. SQUEEZE was used with removing acetonitrile molecule, water molecules and 1 of positions (contained Cl5 atom) of ClO4. Because the ClO4 are counterpartners for the complex we have to remain 4 molecules of ClO4 fixing their occupancy to be equal 1. # SQUEEZE RESULTS ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.002 -0.002 -0.001 2552.6 308.5 2 0.075 0.689 0.854 10.1 1.6 3 0.189 0.925 0.354 10.1 1.7 4 0.311 0.575 0.354 10.1 1.7 5 0.425 0.811 0.854 10.0 1.6 6 0.575 0.189 0.146 10.0 1.6 7 0.689 0.425 0.646 10.1 1.6 8 0.811 0.075 0.646 10.1 1.6 9 0.925 0.311 0.146 10.0 1.7 _platon_squeeze_details ; ? ; _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^)+(0.0023P)^2^+55.0819P] 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 20616 _refine_ls_number_parameters 1189 _refine_ls_number_restraints 117 _refine_ls_R_factor_all 0.1686 _refine_ls_R_factor_gt 0.0971 _refine_ls_wR_factor_ref 0.1774 _refine_ls_wR_factor_gt 0.1641 _refine_ls_goodness_of_fit_ref 1.273 _refine_ls_restrained_S_all 1.347 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.82930(4) 0.22894(4) 0.01691(11) 0.0472(4) Uani 1 1 d . . . O5 O 0.86391(12) 0.24276(12) -0.0218(3) 0.0609(12) Uani 1 1 d . . . O6 O 0.83257(13) 0.18942(12) 0.0362(4) 0.0726(15) Uani 1 1 d . . . O7 O 0.79892(12) 0.23528(13) -0.0473(3) 0.0624(12) Uani 1 1 d . . . O8 O 0.82101(14) 0.24985(14) 0.0996(3) 0.0726(14) Uani 1 1 d . . . Cl2 Cl 0.51243(8) 1.10433(7) 0.0470(2) 0.1003(8) Uani 1 1 d DU . . O9 O 0.5077(2) 1.07093(17) 0.0001(5) 0.124(3) Uani 1 1 d DU . . O10 O 0.4861(3) 1.1310(2) 0.0177(7) 0.172(4) Uani 1 1 d DU . . O11 O 0.5026(4) 1.1004(3) 0.1419(7) 0.213(5) Uani 1 1 d DU . . O12 O 0.5464(3) 1.1190(3) 0.0426(11) 0.262(6) Uani 1 1 d DU . . Cl3 Cl 0.10912(12) 0.27866(18) 0.1841(2) 0.1682(16) Uani 1 1 d DU . . O13 O 0.0871(5) 0.2461(4) 0.1791(9) 0.276(7) Uani 1 1 d DU . . O14 O 0.0853(4) 0.3071(5) 0.1460(9) 0.260(6) Uani 1 1 d DU . . O15 O 0.1143(4) 0.2851(4) 0.2749(8) 0.291(7) Uani 1 1 d DU . . O16 O 0.1389(5) 0.2784(6) 0.1326(15) 0.397(11) Uani 1 1 d DU . . Cl4 Cl 0.95434(10) 1.18368(15) 0.16252(18) 0.1692(18) Uani 1 1 d DU . . O17 O 0.9386(3) 1.2273(4) 0.1713(7) 0.201(5) Uani 1 1 d DU . . O18 O 0.9423(2) 1.1763(2) 0.0745(5) 0.144(3) Uani 1 1 d DU . . O19 O 0.9360(2) 1.1615(2) 0.2329(4) 0.143(3) Uani 1 1 d DU . . O20 O 0.99367(19) 1.1867(2) 0.1772(4) 0.131(3) Uani 1 1 d DU . . Co1 Co 0.73599(2) 0.42778(2) 0.02945(6) 0.0513(2) Uani 1 1 d . . . N1 N 0.67763(15) 0.41523(16) 0.0180(4) 0.0573(15) Uani 1 1 d . . . C1 C 0.6580(2) 0.3938(2) 0.0768(6) 0.070(2) Uani 1 1 d . . . H1 H 0.6715 0.3818 0.1252 0.084 Uiso 1 1 calc R . . C2 C 0.6196(2) 0.3880(2) 0.0719(7) 0.080(3) Uani 1 1 d . . . H2 H 0.6068 0.3724 0.1154 0.097 Uiso 1 1 calc R . . C3 C 0.6005(2) 0.4051(2) 0.0032(7) 0.081(3) Uani 1 1 d . . . H3 H 0.5738 0.4014 -0.0025 0.097 Uiso 1 1 calc R . . C4 C 0.6192(2) 0.4278(2) -0.0584(6) 0.077(2) Uani 1 1 d . . . H4 H 0.6059 0.4402 -0.1067 0.092 Uiso 1 1 calc R . . C5 C 0.6584(2) 0.4321(2) -0.0478(5) 0.062(2) Uani 1 1 d . . . C6 C 0.6808(2) 0.4562(2) -0.1084(5) 0.067(2) Uani 1 1 d . . . C7 C 0.6673(3) 0.4714(3) -0.1919(6) 0.091(3) Uani 1 1 d . . . H7 H 0.6426 0.4651 -0.2133 0.109 Uiso 1 1 calc R . . C8 C 0.6904(3) 0.4958(3) -0.2429(6) 0.098(3) Uani 1 1 d . . . H8 H 0.6807 0.5074 -0.2969 0.118 Uiso 1 1 calc R . . C9 C 0.7266(3) 0.5031(2) -0.2160(5) 0.081(3) Uani 1 1 d . . . H9 H 0.7428 0.5192 -0.2511 0.097 Uiso 1 1 calc R . . C10 C 0.7393(2) 0.4863(2) -0.1355(5) 0.064(2) Uani 1 1 d . . . N2 N 0.71738(16) 0.46352(16) -0.0822(4) 0.0565(15) Uani 1 1 d . . . N3 N 0.75560(16) 0.38765(16) -0.0706(4) 0.0596(15) Uani 1 1 d . . . C11 C 0.7606(2) 0.3946(2) -0.1603(5) 0.075(2) Uani 1 1 d . . . H11 H 0.7584 0.4201 -0.1813 0.090 Uiso 1 1 calc R . . C12 C 0.7688(2) 0.3662(2) -0.2237(5) 0.077(2) Uani 1 1 d . . . H12 H 0.7724 0.3722 -0.2867 0.093 Uiso 1 1 calc R . . C13 C 0.7716(2) 0.3295(2) -0.1935(5) 0.068(2) Uani 1 1 d . . . H13 H 0.7761 0.3093 -0.2355 0.081 Uiso 1 1 calc R . . C14 C 0.76765(17) 0.32196(19) -0.1002(5) 0.0593(19) Uani 1 1 d . . . H14 H 0.7704 0.2967 -0.0777 0.071 Uiso 1 1 calc R . . C15 C 0.75964(15) 0.35172(19) -0.0400(4) 0.0471(16) Uani 1 1 d . . . C16 C 0.75607(15) 0.34669(17) 0.0588(4) 0.0435(15) Uani 1 1 d . . . C17 C 0.76178(16) 0.31108(17) 0.1009(5) 0.0502(17) Uani 1 1 d . . . H17 H 0.7669 0.2892 0.0647 0.060 Uiso 1 1 calc R . . C18 C 0.75996(17) 0.3083(2) 0.1947(6) 0.0598(19) Uani 1 1 d . . . H18 H 0.7643 0.2845 0.2241 0.072 Uiso 1 1 calc R . . C19 C 0.75196(17) 0.3396(2) 0.2447(5) 0.0591(19) Uani 1 1 d . . . H19 H 0.7505 0.3378 0.3096 0.071 Uiso 1 1 calc R . . C20 C 0.74571(16) 0.37479(19) 0.2018(5) 0.0505(16) Uani 1 1 d . . . N4 N 0.74795(12) 0.37802(13) 0.1085(4) 0.0421(12) Uani 1 1 d . . . Co2 Co 0.84622(2) 0.45546(2) 0.10270(7) 0.0556(3) Uani 1 1 d . . . N5 N 0.85355(15) 0.40527(14) 0.0244(4) 0.0553(14) Uani 1 1 d . . . C21 C 0.8569(2) 0.4034(2) -0.0668(5) 0.066(2) Uani 1 1 d . . . H21 H 0.8555 0.4265 -0.1006 0.079 Uiso 1 1 calc R . . C22 C 0.8624(2) 0.3698(2) -0.1147(5) 0.0643(19) Uani 1 1 d . . . H22 H 0.8642 0.3697 -0.1797 0.077 Uiso 1 1 calc R . . C23 C 0.86510(17) 0.33699(18) -0.0659(5) 0.0560(18) Uani 1 1 d . . . H23 H 0.8694 0.3135 -0.0965 0.067 Uiso 1 1 calc R . . C24 C 0.86164(16) 0.33799(17) 0.0279(5) 0.0482(15) Uani 1 1 d . . . H24 H 0.8635 0.3152 0.0628 0.058 Uiso 1 1 calc R . . C25 C 0.85543(15) 0.37250(16) 0.0708(4) 0.0426(14) Uani 1 1 d . . . C26 C 0.84900(14) 0.37587(16) 0.1715(4) 0.0397(14) Uani 1 1 d . . . C27 C 0.85022(16) 0.34461(17) 0.2295(5) 0.0481(16) Uani 1 1 d . . . H27 H 0.8567 0.3201 0.2065 0.058 Uiso 1 1 calc R . . C28 C 0.84207(17) 0.34948(19) 0.3200(5) 0.0556(17) Uani 1 1 d . . . H28 H 0.8429 0.3284 0.3607 0.067 Uiso 1 1 calc R . . C29 C 0.83268(16) 0.38475(19) 0.3524(5) 0.0501(16) Uani 1 1 d . . . H29 H 0.8261 0.3882 0.4150 0.060 Uiso 1 1 calc R . . C30 C 0.83291(15) 0.41570(17) 0.2923(5) 0.0440(15) Uani 1 1 d . . . N6 N 0.84084(12) 0.41106(13) 0.2021(4) 0.0428(12) Uani 1 1 d . . . N7 N 0.90306(15) 0.46741(16) 0.1497(5) 0.0667(17) Uani 1 1 d . . . C31 C 0.9175(2) 0.4581(2) 0.2347(6) 0.073(2) Uani 1 1 d . . . H31 H 0.9019 0.4441 0.2759 0.087 Uiso 1 1 calc R . . C32 C 0.9530(2) 0.4682(2) 0.2618(7) 0.077(2) Uani 1 1 d . . . H32 H 0.9625 0.4609 0.3203 0.093 Uiso 1 1 calc R . . C33 C 0.9754(2) 0.4894(2) 0.2016(8) 0.083(3) Uani 1 1 d . . . H33 H 1.0004 0.4968 0.2187 0.100 Uiso 1 1 calc R . . C34 C 0.9608(2) 0.49978(19) 0.1161(7) 0.073(2) Uani 1 1 d . . . H34 H 0.9758 0.5145 0.0750 0.087 Uiso 1 1 calc R . . C35 C 0.92424(18) 0.48844(17) 0.0912(6) 0.060(2) Uani 1 1 d . . . C36 C 0.9065(2) 0.49889(18) 0.0046(6) 0.065(2) Uani 1 1 d . . . C37 C 0.9271(3) 0.5168(2) -0.0640(8) 0.092(3) Uani 1 1 d . . . H37 H 0.9534 0.5221 -0.0554 0.111 Uiso 1 1 calc R . . C38 C 0.9098(3) 0.5266(3) -0.1430(9) 0.111(4) Uani 1 1 d . . . H38 H 0.9240 0.5384 -0.1907 0.133 Uiso 1 1 calc R . . C39 C 0.8723(3) 0.5196(3) -0.1537(6) 0.099(3) Uani 1 1 d . . . H39 H 0.8596 0.5265 -0.2088 0.119 Uiso 1 1 calc R . . C40 C 0.8523(2) 0.5019(2) -0.0826(6) 0.073(2) Uani 1 1 d . . . N8 N 0.86949(17) 0.49115(14) -0.0053(4) 0.0610(16) Uani 1 1 d . . . Co3 Co 0.80522(2) 0.55437(3) 0.18414(7) 0.0596(3) Uani 1 1 d . . . N9 N 0.86336(15) 0.57010(15) 0.1913(5) 0.0618(16) Uani 1 1 d . . . C41 C 0.8860(2) 0.5654(2) 0.2633(7) 0.078(2) Uani 1 1 d . . . H41 H 0.8752 0.5557 0.3184 0.093 Uiso 1 1 calc R . . C42 C 0.9248(2) 0.5740(2) 0.2620(8) 0.091(3) Uani 1 1 d . . . H42 H 0.9401 0.5705 0.3150 0.110 Uiso 1 1 calc R . . C43 C 0.9401(2) 0.5878(2) 0.1826(8) 0.088(3) Uani 1 1 d . . . H43 H 0.9663 0.5943 0.1792 0.105 Uiso 1 1 calc R . . C44 C 0.9172(2) 0.59189(19) 0.1091(7) 0.078(3) Uani 1 1 d . . . H44 H 0.9277 0.6009 0.0531 0.094 Uiso 1 1 calc R . . C45 C 0.87863(19) 0.58317(18) 0.1133(7) 0.066(2) Uani 1 1 d . . . C46 C 0.8523(2) 0.58873(19) 0.0371(6) 0.071(2) Uani 1 1 d . . . C47 C 0.8628(3) 0.6061(3) -0.0448(8) 0.106(4) Uani 1 1 d . . . H47 H 0.8881 0.6149 -0.0537 0.128 Uiso 1 1 calc R . . C48 C 0.8359(5) 0.6104(3) -0.1125(9) 0.138(5) Uani 1 1 d . . . H48 H 0.8427 0.6227 -0.1681 0.165 Uiso 1 1 calc R . . C49 C 0.7995(4) 0.5971(3) -0.1012(7) 0.109(3) Uani 1 1 d . . . H49 H 0.7810 0.5995 -0.1486 0.130 Uiso 1 1 calc R . . C50 C 0.7905(2) 0.5802(2) -0.0183(6) 0.075(2) Uani 1 1 d . . . N10 N 0.81626(16) 0.57560(14) 0.0492(4) 0.0577(15) Uani 1 1 d . . . N11 N 0.78258(15) 0.60933(16) 0.2223(5) 0.0623(16) Uani 1 1 d . . . C51 C 0.77171(18) 0.63716(19) 0.1664(6) 0.069(2) Uani 1 1 d . . . H51 H 0.7715 0.6324 0.1023 0.083 Uiso 1 1 calc R . . C52 C 0.7607(2) 0.6728(2) 0.1973(8) 0.084(3) Uani 1 1 d . . . H52 H 0.7536 0.6921 0.1550 0.101 Uiso 1 1 calc R . . C53 C 0.7603(2) 0.6797(2) 0.2870(9) 0.088(3) Uani 1 1 d . . . H53 H 0.7524 0.7038 0.3096 0.106 Uiso 1 1 calc R . . C54 C 0.77127(18) 0.6514(2) 0.3467(7) 0.078(3) Uani 1 1 d . . . H54 H 0.7718 0.6559 0.4109 0.093 Uiso 1 1 calc R . . C55 C 0.78152(18) 0.61632(19) 0.3116(7) 0.064(2) Uani 1 1 d . . . C56 C 0.7927(2) 0.5845(2) 0.3710(6) 0.072(2) Uani 1 1 d . . . C57 C 0.7933(3) 0.5875(3) 0.4647(8) 0.100(3) Uani 1 1 d . . . H57 H 0.7859 0.6106 0.4936 0.120 Uiso 1 1 calc R . . C58 C 0.8046(3) 0.5574(3) 0.5157(7) 0.109(3) Uani 1 1 d . . . H58 H 0.8057 0.5596 0.5805 0.131 Uiso 1 1 calc R . . C59 C 0.8146(3) 0.5233(3) 0.4734(7) 0.097(3) Uani 1 1 d . . . H59 H 0.8231 0.5021 0.5084 0.116 Uiso 1 1 calc R . . C60 C 0.8118(2) 0.5212(2) 0.3779(6) 0.068(2) Uani 1 1 d . . . N12 N 0.80148(15) 0.55113(15) 0.3295(4) 0.0560(14) Uani 1 1 d . . . Co4 Co 0.70001(3) 0.50791(3) 0.19765(7) 0.0618(3) Uani 1 1 d . . . N13 N 0.64442(16) 0.48386(15) 0.2206(5) 0.0657(17) Uani 1 1 d . . . C61 C 0.6335(2) 0.4646(2) 0.2940(7) 0.078(2) Uani 1 1 d . . . H61 H 0.6512 0.4610 0.3426 0.094 Uiso 1 1 calc R . . C62 C 0.5968(2) 0.4492(2) 0.3022(8) 0.092(3) Uani 1 1 d . . . H62 H 0.5896 0.4358 0.3560 0.111 Uiso 1 1 calc R . . C63 C 0.5721(3) 0.4539(2) 0.2337(9) 0.093(3) Uani 1 1 d . . . H63 H 0.5474 0.4429 0.2375 0.112 Uiso 1 1 calc R . . C64 C 0.5824(2) 0.4744(2) 0.1574(8) 0.085(3) Uani 1 1 d . . . H64 H 0.5646 0.4784 0.1093 0.102 Uiso 1 1 calc R . . C65 C 0.6195(2) 0.4896(2) 0.1510(6) 0.068(2) Uani 1 1 d . . . C66 C 0.6322(2) 0.5124(2) 0.0730(6) 0.073(2) Uani 1 1 d . . . C67 C 0.6093(3) 0.5217(3) -0.0014(7) 0.095(3) Uani 1 1 d . . . H67 H 0.5836 0.5133 -0.0035 0.114 Uiso 1 1 calc R . . C68 C 0.6236(4) 0.5426(4) -0.0703(8) 0.121(4) Uani 1 1 d . . . H68 H 0.6078 0.5488 -0.1211 0.145 Uiso 1 1 calc R . . C69 C 0.6601(3) 0.5549(3) -0.0687(7) 0.097(3) Uani 1 1 d . . . H69 H 0.6703 0.5699 -0.1171 0.116 Uiso 1 1 calc R . . C70 C 0.6823(2) 0.5446(2) 0.0071(6) 0.071(2) Uani 1 1 d . . . N14 N 0.66896(18) 0.52431(17) 0.0766(4) 0.0634(16) Uani 1 1 d . . . N15 N 0.69010(15) 0.56079(14) 0.2623(4) 0.0530(14) Uani 1 1 d . . . C71 C 0.67843(19) 0.59263(19) 0.2214(5) 0.0617(19) Uani 1 1 d . . . H71 H 0.6736 0.5921 0.1573 0.074 Uiso 1 1 calc R . . C72 C 0.67307(18) 0.62660(18) 0.2684(6) 0.062(2) Uani 1 1 d . . . H72 H 0.6649 0.6489 0.2370 0.074 Uiso 1 1 calc R . . C73 C 0.67969(17) 0.62746(19) 0.3597(6) 0.059(2) Uani 1 1 d . . . H73 H 0.6763 0.6504 0.3932 0.071 Uiso 1 1 calc R . . C74 C 0.69134(16) 0.59466(17) 0.4039(5) 0.0541(17) Uani 1 1 d . . . H74 H 0.6957 0.5948 0.4682 0.065 Uiso 1 1 calc R . . C75 C 0.69659(17) 0.56178(17) 0.3540(5) 0.0497(16) Uani 1 1 d . . . C76 C 0.70961(17) 0.52567(17) 0.3938(5) 0.0483(15) Uani 1 1 d . . . C77 C 0.7159(2) 0.5215(2) 0.4866(5) 0.068(2) Uani 1 1 d . . . H77 H 0.7115 0.5422 0.5271 0.082 Uiso 1 1 calc R . . C78 C 0.7288(2) 0.4868(2) 0.5206(6) 0.079(2) Uani 1 1 d . . . H78 H 0.7334 0.4838 0.5844 0.094 Uiso 1 1 calc R . . C79 C 0.7349(2) 0.4569(2) 0.4616(5) 0.066(2) Uani 1 1 d . . . H79 H 0.7436 0.4329 0.4835 0.079 Uiso 1 1 calc R . . C80 C 0.72793(17) 0.46273(17) 0.3699(5) 0.0494(16) Uani 1 1 d . . . C81 C 0.73362(17) 0.43222(18) 0.3086(5) 0.0557(17) Uani 1 1 d . . . C82 C 0.73780(18) 0.4084(2) 0.2524(5) 0.0620(19) Uani 1 1 d . . . N16 N 0.71589(13) 0.49646(14) 0.3352(3) 0.0472(13) Uani 1 1 d . . . C83 C 0.82525(18) 0.4534(2) 0.3252(5) 0.0578(18) Uani 1 1 d . . . C84 C 0.8207(2) 0.4860(2) 0.3325(7) 0.088(3) Uani 1 1 d . . . C85 C 0.7789(3) 0.4916(2) -0.1090(5) 0.064(2) Uani 1 1 d . . . C86 C 0.8115(3) 0.4946(2) -0.0928(6) 0.073(2) Uani 1 1 d . . . C87 C 0.7520(3) 0.5666(2) -0.0039(7) 0.082(3) Uani 1 1 d . . . C88 C 0.7207(3) 0.5566(2) 0.0074(6) 0.082(3) Uani 1 1 d . . . O1 O 0.78347(13) 0.45984(17) 0.0866(4) 0.093(2) Uani 1 1 d D . . O2 O 0.8120(3) 0.49925(19) 0.1482(6) 0.176(3) Uani 1 1 d DU . . O4 O 0.7330(3) 0.4719(2) 0.1225(5) 0.167(3) Uani 1 1 d DU . . O3 O 0.76089(14) 0.51341(17) 0.1617(4) 0.0890(18) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0437(8) 0.0513(9) 0.0467(9) 0.0107(7) 0.0058(7) 0.0078(7) O5 0.052(3) 0.057(3) 0.074(3) -0.001(2) 0.010(2) -0.003(2) O6 0.070(3) 0.047(3) 0.101(4) 0.023(3) 0.027(3) 0.013(2) O7 0.053(3) 0.074(3) 0.061(3) 0.009(3) -0.010(2) 0.001(2) O8 0.077(3) 0.088(4) 0.053(3) -0.002(3) 0.004(3) 0.031(3) Cl2 0.1107(19) 0.0709(15) 0.119(2) 0.0219(14) -0.0603(16) -0.0198(13) O9 0.182(7) 0.069(4) 0.122(5) 0.015(4) -0.079(5) -0.036(4) O10 0.200(8) 0.102(5) 0.214(9) 0.014(6) -0.108(7) 0.009(5) O11 0.376(14) 0.116(7) 0.147(8) -0.008(6) -0.059(9) 0.031(8) O12 0.138(7) 0.249(11) 0.398(15) -0.087(11) -0.066(9) -0.084(8) Cl3 0.123(3) 0.292(5) 0.090(2) 0.019(3) -0.020(2) -0.059(3) O13 0.311(13) 0.306(14) 0.213(11) -0.078(10) -0.007(10) -0.126(12) O14 0.249(12) 0.332(15) 0.198(11) 0.029(10) -0.070(10) 0.008(11) O15 0.374(15) 0.344(14) 0.156(9) -0.050(9) -0.131(10) -0.035(12) O16 0.252(13) 0.53(2) 0.411(18) 0.082(15) 0.163(14) -0.008(14) Cl4 0.127(2) 0.329(5) 0.0511(14) -0.036(2) 0.0224(15) -0.135(3) O17 0.201(9) 0.269(11) 0.134(8) -0.027(8) 0.012(7) -0.085(9) O18 0.130(6) 0.211(8) 0.092(5) 0.004(5) -0.006(4) -0.098(5) O19 0.146(6) 0.201(7) 0.083(5) -0.022(5) 0.024(4) -0.104(6) O20 0.111(5) 0.209(7) 0.072(4) -0.014(4) 0.005(4) -0.086(5) Co1 0.0458(5) 0.0498(5) 0.0583(6) -0.0052(4) -0.0098(4) 0.0125(4) N1 0.047(3) 0.058(4) 0.067(4) -0.009(3) -0.010(3) 0.012(3) C1 0.059(5) 0.056(4) 0.094(6) -0.008(4) -0.005(4) 0.010(4) C2 0.047(4) 0.061(5) 0.134(8) -0.018(5) -0.003(5) 0.000(4) C3 0.049(5) 0.072(6) 0.121(8) -0.053(6) -0.017(5) 0.004(4) C4 0.064(5) 0.071(5) 0.096(7) -0.030(5) -0.026(5) 0.027(4) C5 0.055(4) 0.064(5) 0.068(5) -0.029(4) -0.011(4) 0.018(4) C6 0.070(5) 0.077(5) 0.055(5) -0.018(4) -0.021(4) 0.048(4) C7 0.089(6) 0.120(8) 0.063(6) -0.022(5) -0.019(5) 0.061(6) C8 0.129(9) 0.115(8) 0.051(5) 0.010(5) -0.008(6) 0.067(7) C9 0.110(7) 0.083(6) 0.050(5) 0.009(4) 0.008(5) 0.051(5) C10 0.079(5) 0.065(5) 0.048(4) -0.005(4) 0.005(4) 0.043(4) N2 0.061(4) 0.063(4) 0.046(3) -0.004(3) -0.003(3) 0.030(3) N3 0.062(4) 0.056(4) 0.061(4) -0.012(3) -0.012(3) 0.022(3) C11 0.106(6) 0.062(5) 0.058(5) -0.012(4) -0.002(5) 0.037(4) C12 0.090(6) 0.093(6) 0.049(5) -0.021(4) -0.007(4) 0.037(5) C13 0.062(5) 0.073(5) 0.069(5) -0.031(4) -0.014(4) 0.018(4) C14 0.041(4) 0.053(4) 0.084(6) -0.024(4) -0.010(4) 0.012(3) C15 0.030(3) 0.064(4) 0.047(4) -0.020(3) -0.017(3) 0.013(3) C16 0.024(3) 0.046(4) 0.061(4) -0.014(3) -0.013(3) 0.002(2) C17 0.033(3) 0.043(4) 0.075(5) -0.009(3) -0.023(3) 0.001(3) C18 0.044(4) 0.051(4) 0.085(6) 0.001(4) -0.013(4) -0.006(3) C19 0.041(4) 0.079(5) 0.058(4) 0.019(4) -0.016(3) -0.020(3) C20 0.027(3) 0.068(4) 0.057(4) -0.012(4) -0.005(3) -0.013(3) N4 0.026(2) 0.042(3) 0.058(3) -0.013(3) -0.007(2) 0.003(2) Co2 0.0519(5) 0.0350(5) 0.0799(7) 0.0030(5) 0.0058(5) 0.0040(4) N5 0.061(4) 0.044(3) 0.061(4) 0.005(3) 0.009(3) 0.003(3) C21 0.080(5) 0.046(4) 0.073(5) 0.010(4) 0.010(4) 0.002(4) C22 0.068(5) 0.069(5) 0.056(5) -0.009(4) 0.013(4) 0.000(4) C23 0.045(4) 0.042(4) 0.081(5) -0.008(4) 0.005(4) 0.000(3) C24 0.044(4) 0.044(4) 0.056(4) -0.003(3) 0.002(3) 0.006(3) C25 0.031(3) 0.037(3) 0.059(4) 0.001(3) 0.003(3) -0.002(2) C26 0.022(3) 0.043(3) 0.054(4) -0.001(3) -0.005(3) 0.000(2) C27 0.041(3) 0.040(3) 0.064(5) 0.006(3) -0.009(3) 0.002(3) C28 0.045(4) 0.058(4) 0.064(5) 0.008(4) -0.014(3) -0.005(3) C29 0.033(3) 0.066(4) 0.051(4) -0.001(4) -0.010(3) -0.010(3) C30 0.026(3) 0.048(4) 0.057(4) -0.002(3) -0.003(3) -0.006(2) N6 0.027(2) 0.035(3) 0.066(4) -0.003(3) 0.000(2) -0.0019(19) N7 0.041(3) 0.051(3) 0.108(5) 0.000(4) 0.020(4) -0.003(3) C31 0.045(4) 0.073(5) 0.100(7) 0.015(5) -0.002(4) -0.005(4) C32 0.048(4) 0.069(5) 0.115(7) 0.002(5) -0.003(5) -0.001(4) C33 0.053(5) 0.049(5) 0.147(9) -0.015(5) 0.012(6) 0.005(4) C34 0.057(5) 0.038(4) 0.123(7) -0.029(5) 0.040(5) -0.010(3) C35 0.047(4) 0.030(3) 0.102(6) -0.010(4) 0.024(4) 0.006(3) C36 0.059(5) 0.038(4) 0.098(6) 0.001(4) 0.033(5) 0.008(3) C37 0.090(7) 0.061(5) 0.125(9) 0.007(6) 0.044(7) 0.009(5) C38 0.092(8) 0.090(7) 0.152(11) 0.040(7) 0.069(8) 0.014(6) C39 0.114(8) 0.096(7) 0.088(7) 0.036(5) 0.045(6) 0.032(6) C40 0.086(6) 0.046(4) 0.087(6) 0.011(4) 0.032(5) 0.020(4) N8 0.068(4) 0.039(3) 0.076(4) 0.008(3) 0.025(3) 0.011(3) Co3 0.0456(5) 0.0541(6) 0.0791(7) -0.0066(5) 0.0160(5) -0.0106(4) N9 0.041(3) 0.049(3) 0.096(5) -0.004(3) 0.003(4) 0.001(3) C41 0.047(4) 0.062(5) 0.125(8) -0.015(5) 0.006(5) -0.002(4) C42 0.042(4) 0.070(5) 0.162(10) -0.048(6) -0.014(5) 0.004(4) C43 0.045(5) 0.057(5) 0.161(10) -0.056(6) 0.028(6) -0.013(4) C44 0.063(5) 0.040(4) 0.132(8) -0.030(5) 0.037(5) -0.003(4) C45 0.043(4) 0.033(3) 0.120(7) -0.018(4) 0.028(5) 0.002(3) C46 0.067(5) 0.042(4) 0.105(7) 0.006(4) 0.042(5) 0.005(3) C47 0.111(8) 0.074(6) 0.134(10) 0.024(7) 0.055(8) -0.003(6) C48 0.189(15) 0.111(9) 0.113(10) 0.056(8) 0.053(10) 0.011(10) C49 0.131(9) 0.098(8) 0.097(8) 0.028(6) 0.003(7) 0.023(7) C50 0.080(6) 0.062(5) 0.083(6) 0.007(5) 0.012(5) 0.021(4) N10 0.050(3) 0.047(3) 0.076(4) 0.004(3) 0.019(3) 0.010(3) N11 0.044(3) 0.049(3) 0.094(5) -0.005(3) 0.016(3) 0.005(3) C51 0.045(4) 0.052(4) 0.111(7) -0.006(5) 0.012(4) 0.010(3) C52 0.040(4) 0.055(5) 0.158(10) 0.002(6) 0.026(6) 0.009(3) C53 0.040(4) 0.043(4) 0.181(11) -0.023(6) 0.026(6) -0.003(3) C54 0.040(4) 0.063(5) 0.130(8) -0.037(5) 0.020(4) -0.011(3) C55 0.037(4) 0.044(4) 0.111(7) -0.008(5) 0.020(4) -0.009(3) C56 0.058(5) 0.077(6) 0.082(6) -0.030(5) 0.021(4) -0.022(4) C57 0.113(8) 0.074(6) 0.113(9) -0.021(6) 0.019(7) -0.002(5) C58 0.149(10) 0.100(8) 0.078(7) -0.019(6) 0.027(7) -0.006(7) C59 0.123(8) 0.073(6) 0.094(7) 0.005(6) -0.004(6) -0.014(5) C60 0.074(5) 0.057(5) 0.072(6) -0.006(4) 0.006(4) -0.019(4) N12 0.051(3) 0.046(3) 0.072(4) -0.013(3) 0.008(3) -0.009(3) Co4 0.0614(6) 0.0661(6) 0.0578(6) -0.0162(5) 0.0060(5) 0.0160(5) N13 0.059(4) 0.045(3) 0.093(5) -0.007(3) 0.005(4) 0.016(3) C61 0.057(5) 0.066(5) 0.111(7) 0.024(5) 0.021(5) 0.022(4) C62 0.054(5) 0.053(5) 0.170(10) 0.008(6) 0.020(6) 0.013(4) C63 0.065(6) 0.057(5) 0.158(10) -0.023(6) 0.010(7) 0.014(4) C64 0.056(5) 0.066(5) 0.132(9) -0.044(6) -0.017(5) 0.021(4) C65 0.062(5) 0.053(4) 0.089(6) -0.024(4) 0.004(5) 0.020(4) C66 0.061(5) 0.062(5) 0.096(7) -0.027(5) -0.005(5) 0.027(4) C67 0.078(6) 0.111(8) 0.096(7) -0.023(6) -0.013(6) 0.046(6) C68 0.127(10) 0.157(11) 0.079(7) 0.000(7) -0.016(7) 0.083(9) C69 0.095(7) 0.108(7) 0.087(7) 0.006(6) -0.003(6) 0.057(6) C70 0.066(5) 0.071(5) 0.076(6) -0.019(5) 0.014(5) 0.033(4) N14 0.066(4) 0.062(4) 0.063(4) -0.011(3) 0.005(3) 0.019(3) N15 0.054(3) 0.041(3) 0.064(4) -0.002(3) 0.019(3) 0.001(2) C71 0.058(4) 0.051(4) 0.076(5) 0.008(4) 0.008(4) 0.001(3) C72 0.040(4) 0.040(4) 0.106(7) -0.002(4) 0.012(4) 0.004(3) C73 0.034(3) 0.044(4) 0.099(6) -0.023(4) 0.011(4) 0.001(3) C74 0.038(3) 0.048(4) 0.076(5) -0.019(4) 0.010(3) -0.001(3) C75 0.036(3) 0.045(4) 0.068(5) -0.005(3) 0.015(3) 0.000(3) C76 0.044(4) 0.045(4) 0.055(4) -0.004(3) 0.013(3) 0.003(3) C77 0.084(5) 0.062(5) 0.058(5) -0.014(4) 0.016(4) 0.016(4) C78 0.101(6) 0.078(6) 0.056(5) -0.006(4) 0.016(5) 0.027(5) C79 0.070(5) 0.056(4) 0.071(5) 0.010(4) 0.018(4) 0.010(4) C80 0.043(4) 0.044(4) 0.061(5) -0.002(3) 0.011(3) 0.005(3) C81 0.040(4) 0.045(4) 0.082(5) -0.014(4) 0.004(4) -0.002(3) C82 0.040(4) 0.089(5) 0.057(4) -0.016(4) 0.006(3) -0.025(4) N16 0.044(3) 0.047(3) 0.051(3) -0.007(3) 0.012(2) 0.000(2) C83 0.049(4) 0.057(4) 0.067(5) -0.013(4) 0.008(3) -0.006(3) C84 0.070(5) 0.048(5) 0.147(9) 0.003(5) -0.036(5) -0.009(4) C85 0.084(6) 0.060(5) 0.049(4) 0.000(4) 0.023(4) 0.031(4) C86 0.094(7) 0.060(5) 0.065(5) 0.007(4) 0.020(5) 0.026(5) C87 0.066(5) 0.075(6) 0.105(7) -0.017(5) -0.004(5) 0.027(5) C88 0.115(8) 0.066(5) 0.064(5) 0.002(4) 0.021(6) 0.040(5) O1 0.052(3) 0.137(5) 0.088(4) 0.068(4) -0.027(3) -0.040(3) O2 0.274(8) 0.079(4) 0.175(7) -0.014(4) 0.099(6) 0.047(5) O4 0.282(8) 0.123(5) 0.097(5) -0.043(4) -0.011(5) 0.136(5) O3 0.060(3) 0.122(5) 0.084(4) 0.033(4) -0.002(3) -0.021(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 Cl1 O6 1.420(4) . ? Cl1 O5 1.425(4) . ? Cl1 O7 1.437(4) . ? Cl1 O8 1.442(5) . ? Cl2 O12 1.300(9) . ? Cl2 O9 1.368(6) . ? Cl2 O10 1.385(7) . ? Cl2 O11 1.432(11) . ? Cl3 O16 1.287(14) . ? Cl3 O15 1.356(11) . ? Cl3 O13 1.383(12) . ? Cl3 O14 1.417(13) . ? Cl4 O18 1.376(7) . ? Cl4 O20 1.402(7) . ? Cl4 O19 1.441(7) . ? Cl4 O17 1.633(12) . ? Co1 O4 2.060(6) . ? Co1 N1 2.102(5) . ? Co1 N4 2.135(5) . ? Co1 N3 2.142(5) . ? Co1 N2 2.157(5) . ? Co1 O1 2.177(5) . ? N1 C5 1.315(9) . ? N1 C1 1.334(9) . ? C1 C2 1.364(10) . ? C1 H1 0.9500 . ? C2 C3 1.348(11) . ? C2 H2 0.9500 . ? C3 C4 1.368(11) . ? C3 H3 0.9500 . ? C4 C5 1.393(10) . ? C4 H4 0.9500 . ? C5 C6 1.455(11) . ? C6 N2 1.364(9) . ? C6 C7 1.412(10) . ? C7 C8 1.393(13) . ? C7 H7 0.9500 . ? C8 C9 1.355(12) . ? C8 H8 0.9500 . ? C9 C10 1.387(10) . ? C9 H9 0.9500 . ? C10 N2 1.355(9) . ? C10 C85 1.456(11) . ? N3 C11 1.342(9) . ? N3 C15 1.345(8) . ? C11 C12 1.390(9) . ? C11 H11 0.9500 . ? C12 C13 1.368(10) . ? C12 H12 0.9500 . ? C13 C14 1.392(10) . ? C13 H13 0.9500 . ? C14 C15 1.393(8) . ? C14 H14 0.9500 . ? C15 C16 1.458(9) . ? C16 N4 1.347(7) . ? C16 C17 1.407(8) . ? C17 C18 1.373(9) . ? C17 H17 0.9500 . ? C18 C19 1.350(9) . ? C18 H18 0.9500 . ? C19 C20 1.402(9) . ? C19 H19 0.9500 . ? C20 N4 1.369(8) . ? C20 C82 1.418(10) . ? Co2 O2 2.060(6) . ? Co2 N5 2.115(5) . ? Co2 N6 2.137(5) . ? Co2 N7 2.151(6) . ? Co2 N8 2.172(6) . ? Co2 O1 2.221(5) . ? N5 C21 1.336(9) . ? N5 C25 1.336(7) . ? C21 C22 1.386(9) . ? C21 H21 0.9500 . ? C22 C23 1.357(9) . ? C22 H22 0.9500 . ? C23 C24 1.375(9) . ? C23 H23 0.9500 . ? C24 C25 1.381(8) . ? C24 H24 0.9500 . ? C25 C26 1.490(8) . ? C26 N6 1.345(7) . ? C26 C27 1.387(8) . ? C27 C28 1.362(9) . ? C27 H27 0.9500 . ? C28 C29 1.365(9) . ? C28 H28 0.9500 . ? C29 C30 1.395(8) . ? C29 H29 0.9500 . ? C30 N6 1.355(8) . ? C30 C83 1.433(9) . ? N7 C35 1.351(8) . ? N7 C31 1.378(9) . ? C31 C32 1.357(10) . ? C31 H31 0.9500 . ? C32 C33 1.394(11) . ? C32 H32 0.9500 . ? C33 C34 1.396(12) . ? C33 H33 0.9500 . ? C34 C35 1.392(10) . ? C34 H34 0.9500 . ? C35 C36 1.454(11) . ? C36 N8 1.336(9) . ? C36 C37 1.386(11) . ? C37 C38 1.346(13) . ? C37 H37 0.9500 . ? C38 C39 1.352(13) . ? C38 H38 0.9500 . ? C39 C40 1.397(11) . ? C39 H39 0.9500 . ? C40 N8 1.334(10) . ? C40 C86 1.460(12) . ? Co3 O2 2.019(7) . ? Co3 N9 2.117(6) . ? Co3 N12 2.127(6) . ? Co3 N10 2.140(6) . ? Co3 O3 2.144(5) . ? Co3 N11 2.160(6) . ? N9 C41 1.327(10) . ? N9 C45 1.339(9) . ? C41 C42 1.396(10) . ? C41 H41 0.9500 . ? C42 C43 1.365(13) . ? C42 H42 0.9500 . ? C43 C44 1.348(12) . ? C43 H43 0.9500 . ? C44 C45 1.389(10) . ? C44 H44 0.9500 . ? C45 C46 1.460(11) . ? C46 N10 1.357(9) . ? C46 C47 1.390(12) . ? C47 C48 1.375(15) . ? C47 H47 0.9500 . ? C48 C49 1.372(15) . ? C48 H48 0.9500 . ? C49 C50 1.383(12) . ? C49 H49 0.9500 . ? C50 N10 1.346(10) . ? C50 C87 1.450(12) . ? N11 C55 1.326(9) . ? N11 C51 1.329(9) . ? C51 C52 1.386(10) . ? C51 H51 0.9500 . ? C52 C53 1.331(12) . ? C52 H52 0.9500 . ? C53 C54 1.377(12) . ? C53 H53 0.9500 . ? C54 C55 1.380(9) . ? C54 H54 0.9500 . ? C55 C56 1.466(11) . ? C56 N12 1.356(9) . ? C56 C57 1.370(12) . ? C57 C58 1.351(13) . ? C57 H57 0.9500 . ? C58 C59 1.391(12) . ? C58 H58 0.9500 . ? C59 C60 1.399(11) . ? C59 H59 0.9500 . ? C60 N12 1.317(9) . ? C60 C84 1.438(11) . ? Co4 O4 2.036(6) . ? Co4 N15 2.111(5) . ? Co4 N16 2.121(5) . ? Co4 N13 2.153(6) . ? Co4 N14 2.153(6) . ? Co4 O3 2.209(5) . ? N13 C61 1.323(9) . ? N13 C65 1.355(9) . ? C61 C62 1.404(10) . ? C61 H61 0.9500 . ? C62 C63 1.332(13) . ? C62 H62 0.9500 . ? C63 C64 1.374(12) . ? C63 H63 0.9500 . ? C64 C65 1.410(11) . ? C64 H64 0.9500 . ? C65 C66 1.461(11) . ? C66 N14 1.359(9) . ? C66 C67 1.389(11) . ? C67 C68 1.340(14) . ? C67 H67 0.9500 . ? C68 C69 1.354(14) . ? C68 H68 0.9500 . ? C69 C70 1.401(11) . ? C69 H69 0.9500 . ? C70 N14 1.325(10) . ? C70 C88 1.412(13) . ? N15 C71 1.332(8) . ? N15 C75 1.357(8) . ? C71 C72 1.389(9) . ? C71 H71 0.9500 . ? C72 C73 1.352(10) . ? C72 H72 0.9500 . ? C73 C74 1.382(9) . ? C73 H73 0.9500 . ? C74 C75 1.378(8) . ? C74 H74 0.9500 . ? C75 C76 1.467(9) . ? C76 N16 1.353(7) . ? C76 C77 1.379(9) . ? C77 C78 1.390(10) . ? C77 H77 0.9500 . ? C78 C79 1.375(10) . ? C78 H78 0.9500 . ? C79 C80 1.375(9) . ? C79 H79 0.9500 . ? C80 N16 1.356(8) . ? C80 C81 1.410(9) . ? C81 C82 1.181(9) . ? C83 C84 1.159(9) . ? C85 C86 1.173(11) . ? C87 C88 1.164(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Cl1 O5 110.0(3) . . ? O6 Cl1 O7 109.9(3) . . ? O5 Cl1 O7 108.8(3) . . ? O6 Cl1 O8 110.4(3) . . ? O5 Cl1 O8 109.3(3) . . ? O7 Cl1 O8 108.5(3) . . ? O12 Cl2 O9 115.2(7) . . ? O12 Cl2 O10 109.2(7) . . ? O9 Cl2 O10 110.1(5) . . ? O12 Cl2 O11 107.9(8) . . ? O9 Cl2 O11 111.8(5) . . ? O10 Cl2 O11 101.7(7) . . ? O16 Cl3 O15 117.6(12) . . ? O16 Cl3 O13 114.7(13) . . ? O15 Cl3 O13 105.3(9) . . ? O16 Cl3 O14 104.7(11) . . ? O15 Cl3 O14 110.1(10) . . ? O13 Cl3 O14 103.5(9) . . ? O18 Cl4 O20 117.3(5) . . ? O18 Cl4 O19 115.1(4) . . ? O20 Cl4 O19 112.0(5) . . ? O18 Cl4 O17 98.4(6) . . ? O20 Cl4 O17 104.5(5) . . ? O19 Cl4 O17 107.5(6) . . ? O4 Co1 N1 99.2(3) . . ? O4 Co1 N4 105.6(2) . . ? N1 Co1 N4 93.6(2) . . ? O4 Co1 N3 163.5(3) . . ? N1 Co1 N3 96.9(2) . . ? N4 Co1 N3 76.5(2) . . ? O4 Co1 N2 92.6(2) . . ? N1 Co1 N2 76.5(2) . . ? N4 Co1 N2 160.6(2) . . ? N3 Co1 N2 88.0(2) . . ? O4 Co1 O1 53.0(3) . . ? N1 Co1 O1 152.2(2) . . ? N4 Co1 O1 93.76(18) . . ? N3 Co1 O1 110.8(2) . . ? N2 Co1 O1 102.7(2) . . ? C5 N1 C1 117.2(6) . . ? C5 N1 Co1 117.7(5) . . ? C1 N1 Co1 124.9(5) . . ? N1 C1 C2 124.2(8) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C3 C2 C1 117.5(9) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? C2 C3 C4 120.7(8) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 117.6(8) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? N1 C5 C4 122.7(8) . . ? N1 C5 C6 115.2(6) . . ? C4 C5 C6 122.1(8) . . ? N2 C6 C7 119.1(9) . . ? N2 C6 C5 116.7(6) . . ? C7 C6 C5 124.2(8) . . ? C8 C7 C6 119.8(9) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C9 C8 C7 120.5(8) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 117.7(9) . . ? C8 C9 H9 121.1 . . ? C10 C9 H9 121.1 . . ? N2 C10 C9 123.7(8) . . ? N2 C10 C85 117.8(6) . . ? C9 C10 C85 118.4(8) . . ? C10 N2 C6 119.0(6) . . ? C10 N2 Co1 127.2(5) . . ? C6 N2 Co1 112.8(5) . . ? C11 N3 C15 118.7(6) . . ? C11 N3 Co1 125.9(5) . . ? C15 N3 Co1 115.2(5) . . ? N3 C11 C12 123.1(7) . . ? N3 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C13 C12 C11 118.4(7) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C12 C13 C14 119.1(7) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C15 119.6(7) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N3 C15 C14 121.1(6) . . ? N3 C15 C16 115.6(5) . . ? C14 C15 C16 123.3(6) . . ? N4 C16 C17 121.4(6) . . ? N4 C16 C15 116.8(6) . . ? C17 C16 C15 121.8(6) . . ? C18 C17 C16 119.5(6) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C19 C18 C17 119.3(7) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 120.7(7) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.6 . . ? N4 C20 C19 120.5(6) . . ? N4 C20 C82 117.4(6) . . ? C19 C20 C82 122.1(7) . . ? C16 N4 C20 118.7(5) . . ? C16 N4 Co1 114.8(4) . . ? C20 N4 Co1 126.4(4) . . ? O2 Co2 N5 150.0(3) . . ? O2 Co2 N6 105.9(3) . . ? N5 Co2 N6 76.7(2) . . ? O2 Co2 N7 107.0(3) . . ? N5 Co2 N7 102.8(2) . . ? N6 Co2 N7 90.5(2) . . ? O2 Co2 N8 91.3(3) . . ? N5 Co2 N8 92.5(2) . . ? N6 Co2 N8 161.06(19) . . ? N7 Co2 N8 76.7(3) . . ? O2 Co2 O1 53.5(3) . . ? N5 Co2 O1 97.0(2) . . ? N6 Co2 O1 91.98(17) . . ? N7 Co2 O1 160.1(2) . . ? N8 Co2 O1 104.9(2) . . ? C21 N5 C25 117.2(6) . . ? C21 N5 Co2 126.0(5) . . ? C25 N5 Co2 116.7(5) . . ? N5 C21 C22 123.8(7) . . ? N5 C21 H21 118.1 . . ? C22 C21 H21 118.1 . . ? C23 C22 C21 117.9(7) . . ? C23 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? C22 C23 C24 119.6(6) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C23 C24 C25 119.2(6) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? N5 C25 C24 122.2(6) . . ? N5 C25 C26 115.0(5) . . ? C24 C25 C26 122.7(6) . . ? N6 C26 C27 122.0(6) . . ? N6 C26 C25 115.7(5) . . ? C27 C26 C25 122.3(5) . . ? C28 C27 C26 119.1(6) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 120.0(6) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C30 119.2(6) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? N6 C30 C29 121.1(6) . . ? N6 C30 C83 118.3(6) . . ? C29 C30 C83 120.5(6) . . ? C26 N6 C30 118.5(5) . . ? C26 N6 Co2 115.2(4) . . ? C30 N6 Co2 126.1(4) . . ? C35 N7 C31 119.7(6) . . ? C35 N7 Co2 114.6(6) . . ? C31 N7 Co2 125.5(5) . . ? C32 C31 N7 122.6(8) . . ? C32 C31 H31 118.7 . . ? N7 C31 H31 118.7 . . ? C31 C32 C33 118.2(9) . . ? C31 C32 H32 120.9 . . ? C33 C32 H32 120.9 . . ? C32 C33 C34 119.8(8) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C35 C34 C33 119.7(8) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? N7 C35 C34 120.0(8) . . ? N7 C35 C36 116.8(6) . . ? C34 C35 C36 123.3(7) . . ? N8 C36 C37 121.4(9) . . ? N8 C36 C35 117.3(7) . . ? C37 C36 C35 121.3(8) . . ? C38 C37 C36 120.0(10) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 119.4(9) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C38 C39 C40 119.1(10) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? N8 C40 C39 121.7(8) . . ? N8 C40 C86 118.7(7) . . ? C39 C40 C86 119.6(9) . . ? C40 N8 C36 118.4(7) . . ? C40 N8 Co2 127.3(5) . . ? C36 N8 Co2 113.9(5) . . ? O2 Co3 N9 98.5(3) . . ? O2 Co3 N12 102.4(3) . . ? N9 Co3 N12 91.4(2) . . ? O2 Co3 N10 94.2(3) . . ? N9 Co3 N10 77.3(3) . . ? N12 Co3 N10 161.2(2) . . ? O2 Co3 O3 53.4(3) . . ? N9 Co3 O3 151.9(2) . . ? N12 Co3 O3 94.1(2) . . ? N10 Co3 O3 103.0(2) . . ? O2 Co3 N11 165.2(3) . . ? N9 Co3 N11 96.3(2) . . ? N12 Co3 N11 76.6(2) . . ? N10 Co3 N11 89.6(2) . . ? O3 Co3 N11 111.8(2) . . ? C41 N9 C45 118.4(7) . . ? C41 N9 Co3 125.7(5) . . ? C45 N9 Co3 115.7(5) . . ? N9 C41 C42 123.1(9) . . ? N9 C41 H41 118.4 . . ? C42 C41 H41 118.4 . . ? C43 C42 C41 118.2(9) . . ? C43 C42 H42 120.9 . . ? C41 C42 H42 120.9 . . ? C44 C43 C42 118.6(8) . . ? C44 C43 H43 120.7 . . ? C42 C43 H43 120.7 . . ? C43 C44 C45 121.4(9) . . ? C43 C44 H44 119.3 . . ? C45 C44 H44 119.3 . . ? N9 C45 C44 120.2(9) . . ? N9 C45 C46 116.1(6) . . ? C44 C45 C46 123.7(8) . . ? N10 C46 C47 120.6(9) . . ? N10 C46 C45 116.5(7) . . ? C47 C46 C45 122.9(8) . . ? C48 C47 C46 118.8(10) . . ? C48 C47 H47 120.6 . . ? C46 C47 H47 120.6 . . ? C49 C48 C47 121.2(10) . . ? C49 C48 H48 119.4 . . ? C47 C48 H48 119.4 . . ? C48 C49 C50 117.5(11) . . ? C48 C49 H49 121.3 . . ? C50 C49 H49 121.3 . . ? N10 C50 C49 122.6(9) . . ? N10 C50 C87 118.7(8) . . ? C49 C50 C87 118.6(9) . . ? C50 N10 C46 119.3(7) . . ? C50 N10 Co3 126.4(5) . . ? C46 N10 Co3 114.0(6) . . ? C55 N11 C51 117.3(7) . . ? C55 N11 Co3 115.4(5) . . ? C51 N11 Co3 127.2(6) . . ? N11 C51 C52 123.0(9) . . ? N11 C51 H51 118.5 . . ? C52 C51 H51 118.5 . . ? C53 C52 C51 119.1(9) . . ? C53 C52 H52 120.5 . . ? C51 C52 H52 120.5 . . ? C52 C53 C54 119.2(8) . . ? C52 C53 H53 120.4 . . ? C54 C53 H53 120.4 . . ? C53 C54 C55 118.9(9) . . ? C53 C54 H54 120.6 . . ? C55 C54 H54 120.6 . . ? N11 C55 C54 122.4(8) . . ? N11 C55 C56 115.6(7) . . ? C54 C55 C56 122.0(9) . . ? N12 C56 C57 120.4(9) . . ? N12 C56 C55 117.1(7) . . ? C57 C56 C55 122.4(8) . . ? C58 C57 C56 119.7(9) . . ? C58 C57 H57 120.2 . . ? C56 C57 H57 120.2 . . ? C57 C58 C59 120.2(10) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? C58 C59 C60 118.0(9) . . ? C58 C59 H59 121.0 . . ? C60 C59 H59 121.0 . . ? N12 C60 C59 120.7(8) . . ? N12 C60 C84 120.0(8) . . ? C59 C60 C84 119.3(8) . . ? C60 N12 C56 121.0(7) . . ? C60 N12 Co3 124.1(5) . . ? C56 N12 Co3 114.4(5) . . ? O4 Co4 N15 151.8(3) . . ? O4 Co4 N16 104.0(2) . . ? N15 Co4 N16 77.7(2) . . ? O4 Co4 N13 110.8(3) . . ? N15 Co4 N13 97.2(2) . . ? N16 Co4 N13 91.0(2) . . ? O4 Co4 N14 90.7(3) . . ? N15 Co4 N14 92.7(2) . . ? N16 Co4 N14 163.6(2) . . ? N13 Co4 N14 76.9(3) . . ? O4 Co4 O3 51.4(3) . . ? N15 Co4 O3 100.9(2) . . ? N16 Co4 O3 89.23(19) . . ? N13 Co4 O3 161.5(2) . . ? N14 Co4 O3 105.8(2) . . ? C61 N13 C65 119.7(7) . . ? C61 N13 Co4 126.0(6) . . ? C65 N13 Co4 114.3(6) . . ? N13 C61 C62 122.1(9) . . ? N13 C61 H61 119.0 . . ? C62 C61 H61 119.0 . . ? C63 C62 C61 119.1(10) . . ? C63 C62 H62 120.5 . . ? C61 C62 H62 120.5 . . ? C62 C63 C64 120.1(9) . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C63 C64 C65 119.6(9) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? N13 C65 C64 119.4(9) . . ? N13 C65 C66 117.9(7) . . ? C64 C65 C66 122.7(9) . . ? N14 C66 C67 120.5(9) . . ? N14 C66 C65 115.3(7) . . ? C67 C66 C65 124.2(9) . . ? C68 C67 C66 119.9(10) . . ? C68 C67 H67 120.1 . . ? C66 C67 H67 120.1 . . ? C67 C68 C69 121.1(10) . . ? C67 C68 H68 119.5 . . ? C69 C68 H68 119.5 . . ? C68 C69 C70 117.3(10) . . ? C68 C69 H69 121.4 . . ? C70 C69 H69 121.4 . . ? N14 C70 C69 123.0(9) . . ? N14 C70 C88 119.8(8) . . ? C69 C70 C88 117.2(9) . . ? C70 N14 C66 118.2(7) . . ? C70 N14 Co4 126.2(6) . . ? C66 N14 Co4 115.6(6) . . ? C71 N15 C75 118.1(6) . . ? C71 N15 Co4 126.1(5) . . ? C75 N15 Co4 115.8(4) . . ? N15 C71 C72 122.8(7) . . ? N15 C71 H71 118.6 . . ? C72 C71 H71 118.6 . . ? C73 C72 C71 118.8(7) . . ? C73 C72 H72 120.6 . . ? C71 C72 H72 120.6 . . ? C72 C73 C74 119.5(6) . . ? C72 C73 H73 120.3 . . ? C74 C73 H73 120.3 . . ? C75 C74 C73 119.4(7) . . ? C75 C74 H74 120.3 . . ? C73 C74 H74 120.3 . . ? N15 C75 C74 121.3(6) . . ? N15 C75 C76 114.9(6) . . ? C74 C75 C76 123.8(7) . . ? N16 C76 C77 120.8(6) . . ? N16 C76 C75 117.1(6) . . ? C77 C76 C75 122.1(6) . . ? C76 C77 C78 119.8(7) . . ? C76 C77 H77 120.1 . . ? C78 C77 H77 120.1 . . ? C79 C78 C77 119.8(7) . . ? C79 C78 H78 120.1 . . ? C77 C78 H78 120.1 . . ? C80 C79 C78 117.8(7) . . ? C80 C79 H79 121.1 . . ? C78 C79 H79 121.1 . . ? N16 C80 C79 123.3(6) . . ? N16 C80 C81 118.1(6) . . ? C79 C80 C81 118.6(6) . . ? C82 C81 C80 175.4(8) . . ? C81 C82 C20 167.1(8) . . ? C76 N16 C80 118.5(6) . . ? C76 N16 Co4 114.3(4) . . ? C80 N16 Co4 126.9(4) . . ? C84 C83 C30 165.2(9) . . ? C83 C84 C60 156.9(11) . . ? C86 C85 C10 175.5(8) . . ? C85 C86 C40 172.5(9) . . ? C88 C87 C50 178.3(9) . . ? C87 C88 C70 171.7(10) . . ? Co1 O1 Co2 139.8(3) . . ? Co3 O2 Co2 150.2(5) . . ? Co4 O4 Co1 148.3(5) . . ? Co3 O3 Co4 136.5(3) . . ? 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 O4 Co1 N1 C5 92.6(5) . . . . ? N4 Co1 N1 C5 -160.9(5) . . . . ? N3 Co1 N1 C5 -84.1(5) . . . . ? N2 Co1 N1 C5 2.2(5) . . . . ? O1 Co1 N1 C5 93.9(6) . . . . ? O4 Co1 N1 C1 -81.6(6) . . . . ? N4 Co1 N1 C1 24.9(6) . . . . ? N3 Co1 N1 C1 101.7(6) . . . . ? N2 Co1 N1 C1 -172.1(6) . . . . ? O1 Co1 N1 C1 -80.3(7) . . . . ? C5 N1 C1 C2 1.2(11) . . . . ? Co1 N1 C1 C2 175.4(6) . . . . ? N1 C1 C2 C3 -0.2(12) . . . . ? C1 C2 C3 C4 -0.6(11) . . . . ? C2 C3 C4 C5 0.6(11) . . . . ? C1 N1 C5 C4 -1.2(10) . . . . ? Co1 N1 C5 C4 -175.9(5) . . . . ? C1 N1 C5 C6 178.0(6) . . . . ? Co1 N1 C5 C6 3.3(7) . . . . ? C3 C4 C5 N1 0.4(11) . . . . ? C3 C4 C5 C6 -178.8(6) . . . . ? N1 C5 C6 N2 -10.3(9) . . . . ? C4 C5 C6 N2 168.9(6) . . . . ? N1 C5 C6 C7 168.4(6) . . . . ? C4 C5 C6 C7 -12.4(11) . . . . ? N2 C6 C7 C8 -4.6(11) . . . . ? C5 C6 C7 C8 176.8(7) . . . . ? C6 C7 C8 C9 4.2(13) . . . . ? C7 C8 C9 C10 -1.5(12) . . . . ? C8 C9 C10 N2 -0.9(11) . . . . ? C8 C9 C10 C85 175.8(7) . . . . ? C9 C10 N2 C6 0.5(10) . . . . ? C85 C10 N2 C6 -176.2(6) . . . . ? C9 C10 N2 Co1 167.9(5) . . . . ? C85 C10 N2 Co1 -8.8(9) . . . . ? C7 C6 N2 C10 2.3(9) . . . . ? C5 C6 N2 C10 -179.0(6) . . . . ? C7 C6 N2 Co1 -166.9(5) . . . . ? C5 C6 N2 Co1 11.8(7) . . . . ? O4 Co1 N2 C10 85.5(6) . . . . ? N1 Co1 N2 C10 -175.7(6) . . . . ? N4 Co1 N2 C10 -114.8(7) . . . . ? N3 Co1 N2 C10 -78.0(5) . . . . ? O1 Co1 N2 C10 32.8(6) . . . . ? O4 Co1 N2 C6 -106.4(5) . . . . ? N1 Co1 N2 C6 -7.6(4) . . . . ? N4 Co1 N2 C6 53.3(8) . . . . ? N3 Co1 N2 C6 90.1(4) . . . . ? O1 Co1 N2 C6 -159.0(4) . . . . ? O4 Co1 N3 C11 -77.3(11) . . . . ? N1 Co1 N3 C11 91.2(7) . . . . ? N4 Co1 N3 C11 -176.7(7) . . . . ? N2 Co1 N3 C11 15.1(7) . . . . ? O1 Co1 N3 C11 -87.8(6) . . . . ? O4 Co1 N3 C15 109.1(9) . . . . ? N1 Co1 N3 C15 -82.4(5) . . . . ? N4 Co1 N3 C15 9.7(4) . . . . ? N2 Co1 N3 C15 -158.6(5) . . . . ? O1 Co1 N3 C15 98.6(5) . . . . ? C15 N3 C11 C12 1.7(12) . . . . ? Co1 N3 C11 C12 -171.7(6) . . . . ? N3 C11 C12 C13 0.6(13) . . . . ? C11 C12 C13 C14 -2.6(11) . . . . ? C12 C13 C14 C15 2.3(10) . . . . ? C11 N3 C15 C14 -2.0(9) . . . . ? Co1 N3 C15 C14 172.1(4) . . . . ? C11 N3 C15 C16 176.5(6) . . . . ? Co1 N3 C15 C16 -9.4(7) . . . . ? C13 C14 C15 N3 0.1(9) . . . . ? C13 C14 C15 C16 -178.3(6) . . . . ? N3 C15 C16 N4 2.0(8) . . . . ? C14 C15 C16 N4 -179.5(5) . . . . ? N3 C15 C16 C17 -176.3(5) . . . . ? C14 C15 C16 C17 2.1(9) . . . . ? N4 C16 C17 C18 -1.6(8) . . . . ? C15 C16 C17 C18 176.7(5) . . . . ? C16 C17 C18 C19 1.3(9) . . . . ? C17 C18 C19 C20 -0.3(9) . . . . ? C18 C19 C20 N4 -0.6(9) . . . . ? C18 C19 C20 C82 -179.1(6) . . . . ? C17 C16 N4 C20 0.7(8) . . . . ? C15 C16 N4 C20 -177.7(5) . . . . ? C17 C16 N4 Co1 -175.2(4) . . . . ? C15 C16 N4 Co1 6.4(6) . . . . ? C19 C20 N4 C16 0.3(8) . . . . ? C82 C20 N4 C16 178.9(5) . . . . ? C19 C20 N4 Co1 175.8(4) . . . . ? C82 C20 N4 Co1 -5.7(7) . . . . ? O4 Co1 N4 C16 -171.6(4) . . . . ? N1 Co1 N4 C16 87.8(4) . . . . ? N3 Co1 N4 C16 -8.5(4) . . . . ? N2 Co1 N4 C16 29.5(8) . . . . ? O1 Co1 N4 C16 -118.9(4) . . . . ? O4 Co1 N4 C20 12.9(5) . . . . ? N1 Co1 N4 C20 -87.7(5) . . . . ? N3 Co1 N4 C20 176.0(5) . . . . ? N2 Co1 N4 C20 -146.1(6) . . . . ? O1 Co1 N4 C20 65.5(5) . . . . ? O2 Co2 N5 C21 75.4(8) . . . . ? N6 Co2 N5 C21 174.3(6) . . . . ? N7 Co2 N5 C21 -98.3(6) . . . . ? N8 Co2 N5 C21 -21.4(6) . . . . ? O1 Co2 N5 C21 83.9(6) . . . . ? O2 Co2 N5 C25 -105.4(6) . . . . ? N6 Co2 N5 C25 -6.6(4) . . . . ? N7 Co2 N5 C25 80.8(5) . . . . ? N8 Co2 N5 C25 157.7(5) . . . . ? O1 Co2 N5 C25 -97.0(4) . . . . ? C25 N5 C21 C22 -0.4(11) . . . . ? Co2 N5 C21 C22 178.7(5) . . . . ? N5 C21 C22 C23 -1.1(11) . . . . ? C21 C22 C23 C24 1.2(10) . . . . ? C22 C23 C24 C25 0.0(10) . . . . ? C21 N5 C25 C24 1.8(9) . . . . ? Co2 N5 C25 C24 -177.4(4) . . . . ? C21 N5 C25 C26 -176.2(6) . . . . ? Co2 N5 C25 C26 4.6(6) . . . . ? C23 C24 C25 N5 -1.6(9) . . . . ? C23 C24 C25 C26 176.2(5) . . . . ? N5 C25 C26 N6 2.3(7) . . . . ? C24 C25 C26 N6 -175.7(5) . . . . ? N5 C25 C26 C27 -179.6(5) . . . . ? C24 C25 C26 C27 2.4(8) . . . . ? N6 C26 C27 C28 1.5(8) . . . . ? C25 C26 C27 C28 -176.5(5) . . . . ? C26 C27 C28 C29 0.3(9) . . . . ? C27 C28 C29 C30 -2.3(9) . . . . ? C28 C29 C30 N6 2.6(8) . . . . ? C28 C29 C30 C83 -176.5(5) . . . . ? C27 C26 N6 C30 -1.2(8) . . . . ? C25 C26 N6 C30 176.9(5) . . . . ? C27 C26 N6 Co2 174.0(4) . . . . ? C25 C26 N6 Co2 -7.8(6) . . . . ? C29 C30 N6 C26 -0.8(8) . . . . ? C83 C30 N6 C26 178.3(5) . . . . ? C29 C30 N6 Co2 -175.5(4) . . . . ? C83 C30 N6 Co2 3.7(7) . . . . ? O2 Co2 N6 C26 156.9(5) . . . . ? N5 Co2 N6 C26 7.7(4) . . . . ? N7 Co2 N6 C26 -95.3(4) . . . . ? N8 Co2 N6 C26 -48.7(8) . . . . ? O1 Co2 N6 C26 104.4(4) . . . . ? O2 Co2 N6 C30 -28.3(5) . . . . ? N5 Co2 N6 C30 -177.4(5) . . . . ? N7 Co2 N6 C30 79.5(5) . . . . ? N8 Co2 N6 C30 126.2(7) . . . . ? O1 Co2 N6 C30 -80.7(5) . . . . ? O2 Co2 N7 C35 -89.7(5) . . . . ? N5 Co2 N7 C35 87.1(5) . . . . ? N6 Co2 N7 C35 163.5(4) . . . . ? N8 Co2 N7 C35 -2.4(4) . . . . ? O1 Co2 N7 C35 -99.4(8) . . . . ? O2 Co2 N7 C31 85.0(6) . . . . ? N5 Co2 N7 C31 -98.3(6) . . . . ? N6 Co2 N7 C31 -21.9(6) . . . . ? N8 Co2 N7 C31 172.2(6) . . . . ? O1 Co2 N7 C31 75.3(9) . . . . ? C35 N7 C31 C32 -2.2(11) . . . . ? Co2 N7 C31 C32 -176.6(6) . . . . ? N7 C31 C32 C33 1.4(12) . . . . ? C31 C32 C33 C34 0.1(11) . . . . ? C32 C33 C34 C35 -0.7(11) . . . . ? C31 N7 C35 C34 1.6(9) . . . . ? Co2 N7 C35 C34 176.5(4) . . . . ? C31 N7 C35 C36 -176.9(6) . . . . ? Co2 N7 C35 C36 -1.9(7) . . . . ? C33 C34 C35 N7 -0.2(9) . . . . ? C33 C34 C35 C36 178.2(6) . . . . ? N7 C35 C36 N8 8.3(9) . . . . ? C34 C35 C36 N8 -170.2(6) . . . . ? N7 C35 C36 C37 -172.9(6) . . . . ? C34 C35 C36 C37 8.7(10) . . . . ? N8 C36 C37 C38 -0.3(12) . . . . ? C35 C36 C37 C38 -179.1(8) . . . . ? C36 C37 C38 C39 1.3(15) . . . . ? C37 C38 C39 C40 -0.5(15) . . . . ? C38 C39 C40 N8 -1.3(13) . . . . ? C38 C39 C40 C86 179.1(8) . . . . ? C39 C40 N8 C36 2.3(10) . . . . ? C86 C40 N8 C36 -178.1(6) . . . . ? C39 C40 N8 Co2 -169.2(6) . . . . ? C86 C40 N8 Co2 10.4(9) . . . . ? C37 C36 N8 C40 -1.5(10) . . . . ? C35 C36 N8 C40 177.3(6) . . . . ? C37 C36 N8 Co2 171.1(5) . . . . ? C35 C36 N8 Co2 -10.1(7) . . . . ? O2 Co2 N8 C40 -74.2(6) . . . . ? N5 Co2 N8 C40 76.0(6) . . . . ? N6 Co2 N8 C40 130.2(7) . . . . ? N7 Co2 N8 C40 178.6(6) . . . . ? O1 Co2 N8 C40 -21.9(6) . . . . ? O2 Co2 N8 C36 113.9(5) . . . . ? N5 Co2 N8 C36 -95.8(5) . . . . ? N6 Co2 N8 C36 -41.6(9) . . . . ? N7 Co2 N8 C36 6.8(4) . . . . ? O1 Co2 N8 C36 166.3(5) . . . . ? O2 Co3 N9 C41 -84.9(6) . . . . ? N12 Co3 N9 C41 17.8(6) . . . . ? N10 Co3 N9 C41 -177.4(6) . . . . ? O3 Co3 N9 C41 -83.5(8) . . . . ? N11 Co3 N9 C41 94.5(6) . . . . ? O2 Co3 N9 C45 89.7(5) . . . . ? N12 Co3 N9 C45 -167.5(5) . . . . ? N10 Co3 N9 C45 -2.7(4) . . . . ? O3 Co3 N9 C45 91.2(6) . . . . ? N11 Co3 N9 C45 -90.8(5) . . . . ? C45 N9 C41 C42 1.0(10) . . . . ? Co3 N9 C41 C42 175.6(5) . . . . ? N9 C41 C42 C43 -0.3(11) . . . . ? C41 C42 C43 C44 -0.8(11) . . . . ? C42 C43 C44 C45 1.2(11) . . . . ? C41 N9 C45 C44 -0.6(9) . . . . ? Co3 N9 C45 C44 -175.7(5) . . . . ? C41 N9 C45 C46 -178.4(6) . . . . ? Co3 N9 C45 C46 6.5(7) . . . . ? C43 C44 C45 N9 -0.5(10) . . . . ? C43 C44 C45 C46 177.1(7) . . . . ? N9 C45 C46 N10 -8.1(9) . . . . ? C44 C45 C46 N10 174.1(6) . . . . ? N9 C45 C46 C47 172.5(7) . . . . ? C44 C45 C46 C47 -5.2(11) . . . . ? N10 C46 C47 C48 1.2(14) . . . . ? C45 C46 C47 C48 -179.5(9) . . . . ? C46 C47 C48 C49 -1.4(18) . . . . ? C47 C48 C49 C50 1.6(18) . . . . ? C48 C49 C50 N10 -1.6(14) . . . . ? C48 C49 C50 C87 178.8(9) . . . . ? C49 C50 N10 C46 1.4(11) . . . . ? C87 C50 N10 C46 -179.0(6) . . . . ? C49 C50 N10 Co3 174.4(6) . . . . ? C87 C50 N10 Co3 -6.0(10) . . . . ? C47 C46 N10 C50 -1.2(10) . . . . ? C45 C46 N10 C50 179.4(6) . . . . ? C47 C46 N10 Co3 -175.0(6) . . . . ? C45 C46 N10 Co3 5.7(7) . . . . ? O2 Co3 N10 C50 87.2(6) . . . . ? N9 Co3 N10 C50 -175.0(6) . . . . ? N12 Co3 N10 C50 -120.8(8) . . . . ? O3 Co3 N10 C50 33.8(6) . . . . ? N11 Co3 N10 C50 -78.5(6) . . . . ? O2 Co3 N10 C46 -99.6(5) . . . . ? N9 Co3 N10 C46 -1.8(4) . . . . ? N12 Co3 N10 C46 52.5(8) . . . . ? O3 Co3 N10 C46 -152.9(4) . . . . ? N11 Co3 N10 C46 94.8(5) . . . . ? O2 Co3 N11 C55 95.3(13) . . . . ? N9 Co3 N11 C55 -82.5(5) . . . . ? N12 Co3 N11 C55 7.4(5) . . . . ? N10 Co3 N11 C55 -159.7(5) . . . . ? O3 Co3 N11 C55 96.5(5) . . . . ? O2 Co3 N11 C51 -88.6(14) . . . . ? N9 Co3 N11 C51 93.6(6) . . . . ? N12 Co3 N11 C51 -176.5(6) . . . . ? N10 Co3 N11 C51 16.4(6) . . . . ? O3 Co3 N11 C51 -87.4(6) . . . . ? C55 N11 C51 C52 2.0(10) . . . . ? Co3 N11 C51 C52 -174.0(5) . . . . ? N11 C51 C52 C53 -1.2(11) . . . . ? C51 C52 C53 C54 1.0(12) . . . . ? C52 C53 C54 C55 -1.7(11) . . . . ? C51 N11 C55 C54 -2.8(10) . . . . ? Co3 N11 C55 C54 173.7(5) . . . . ? C51 N11 C55 C56 178.3(6) . . . . ? Co3 N11 C55 C56 -5.2(7) . . . . ? C53 C54 C55 N11 2.7(10) . . . . ? C53 C54 C55 C56 -178.5(6) . . . . ? N11 C55 C56 N12 -2.3(9) . . . . ? C54 C55 C56 N12 178.7(6) . . . . ? N11 C55 C56 C57 179.4(7) . . . . ? C54 C55 C56 C57 0.5(11) . . . . ? N12 C56 C57 C58 3.1(14) . . . . ? C55 C56 C57 C58 -178.7(8) . . . . ? C56 C57 C58 C59 -1.5(16) . . . . ? C57 C58 C59 C60 -1.4(15) . . . . ? C58 C59 C60 N12 2.8(13) . . . . ? C58 C59 C60 C84 -178.1(8) . . . . ? C59 C60 N12 C56 -1.3(11) . . . . ? C84 C60 N12 C56 179.6(6) . . . . ? C59 C60 N12 Co3 169.1(6) . . . . ? C84 C60 N12 Co3 -10.0(9) . . . . ? C57 C56 N12 C60 -1.7(11) . . . . ? C55 C56 N12 C60 -180.0(6) . . . . ? C57 C56 N12 Co3 -173.0(6) . . . . ? C55 C56 N12 Co3 8.7(7) . . . . ? O2 Co3 N12 C60 15.7(6) . . . . ? N9 Co3 N12 C60 -83.3(5) . . . . ? N10 Co3 N12 C60 -135.7(7) . . . . ? O3 Co3 N12 C60 69.1(6) . . . . ? N11 Co3 N12 C60 -179.5(6) . . . . ? O2 Co3 N12 C56 -173.3(5) . . . . ? N9 Co3 N12 C56 87.6(5) . . . . ? N10 Co3 N12 C56 35.3(9) . . . . ? O3 Co3 N12 C56 -119.9(5) . . . . ? N11 Co3 N12 C56 -8.5(5) . . . . ? O4 Co4 N13 C61 95.5(6) . . . . ? N15 Co4 N13 C61 -87.6(6) . . . . ? N16 Co4 N13 C61 -9.9(6) . . . . ? N14 Co4 N13 C61 -178.7(6) . . . . ? O3 Co4 N13 C61 80.6(10) . . . . ? O4 Co4 N13 C65 -83.9(5) . . . . ? N15 Co4 N13 C65 92.9(5) . . . . ? N16 Co4 N13 C65 170.7(4) . . . . ? N14 Co4 N13 C65 1.8(4) . . . . ? O3 Co4 N13 C65 -98.8(8) . . . . ? C65 N13 C61 C62 0.7(11) . . . . ? Co4 N13 C61 C62 -178.7(5) . . . . ? N13 C61 C62 C63 0.8(12) . . . . ? C61 C62 C63 C64 -2.1(12) . . . . ? C62 C63 C64 C65 2.0(12) . . . . ? C61 N13 C65 C64 -0.7(10) . . . . ? Co4 N13 C65 C64 178.7(5) . . . . ? C61 N13 C65 C66 177.4(6) . . . . ? Co4 N13 C65 C66 -3.2(7) . . . . ? C63 C64 C65 N13 -0.6(10) . . . . ? C63 C64 C65 C66 -178.6(7) . . . . ? N13 C65 C66 N14 3.0(9) . . . . ? C64 C65 C66 N14 -178.9(6) . . . . ? N13 C65 C66 C67 -177.6(7) . . . . ? C64 C65 C66 C67 0.5(11) . . . . ? N14 C66 C67 C68 0.1(12) . . . . ? C65 C66 C67 C68 -179.3(8) . . . . ? C66 C67 C68 C69 -0.1(15) . . . . ? C67 C68 C69 C70 0.7(15) . . . . ? C68 C69 C70 N14 -1.2(12) . . . . ? C68 C69 C70 C88 178.3(8) . . . . ? C69 C70 N14 C66 1.2(10) . . . . ? C88 C70 N14 C66 -178.3(6) . . . . ? C69 C70 N14 Co4 -178.6(5) . . . . ? C88 C70 N14 Co4 1.9(9) . . . . ? C67 C66 N14 C70 -0.6(10) . . . . ? C65 C66 N14 C70 178.9(6) . . . . ? C67 C66 N14 Co4 179.3(5) . . . . ? C65 C66 N14 Co4 -1.3(7) . . . . ? O4 Co4 N14 C70 -69.2(6) . . . . ? N15 Co4 N14 C70 82.8(6) . . . . ? N16 Co4 N14 C70 136.4(8) . . . . ? N13 Co4 N14 C70 179.6(6) . . . . ? O3 Co4 N14 C70 -19.3(6) . . . . ? O4 Co4 N14 C66 111.0(5) . . . . ? N15 Co4 N14 C66 -97.1(5) . . . . ? N16 Co4 N14 C66 -43.4(10) . . . . ? N13 Co4 N14 C66 -0.2(4) . . . . ? O3 Co4 N14 C66 160.9(5) . . . . ? O4 Co4 N15 C71 80.4(8) . . . . ? N16 Co4 N15 C71 177.3(6) . . . . ? N13 Co4 N15 C71 -93.3(5) . . . . ? N14 Co4 N15 C71 -16.1(6) . . . . ? O3 Co4 N15 C71 90.5(5) . . . . ? O4 Co4 N15 C75 -99.2(6) . . . . ? N16 Co4 N15 C75 -2.4(4) . . . . ? N13 Co4 N15 C75 87.1(5) . . . . ? N14 Co4 N15 C75 164.2(5) . . . . ? O3 Co4 N15 C75 -89.2(4) . . . . ? C75 N15 C71 C72 0.7(9) . . . . ? Co4 N15 C71 C72 -179.0(5) . . . . ? N15 C71 C72 C73 -0.5(10) . . . . ? C71 C72 C73 C74 -0.4(10) . . . . ? C72 C73 C74 C75 1.0(9) . . . . ? C71 N15 C75 C74 0.0(9) . . . . ? Co4 N15 C75 C74 179.7(4) . . . . ? C71 N15 C75 C76 -179.6(5) . . . . ? Co4 N15 C75 C76 0.1(7) . . . . ? C73 C74 C75 N15 -0.8(9) . . . . ? C73 C74 C75 C76 178.8(6) . . . . ? N15 C75 C76 N16 3.9(8) . . . . ? C74 C75 C76 N16 -175.7(5) . . . . ? N15 C75 C76 C77 -177.2(6) . . . . ? C74 C75 C76 C77 3.2(10) . . . . ? N16 C76 C77 C78 -0.2(11) . . . . ? C75 C76 C77 C78 -179.0(7) . . . . ? C76 C77 C78 C79 -0.5(12) . . . . ? C77 C78 C79 C80 0.3(12) . . . . ? C78 C79 C80 N16 0.7(11) . . . . ? C78 C79 C80 C81 -179.4(7) . . . . ? N4 C20 C82 C81 -165(3) . . . . ? C19 C20 C82 C81 14(3) . . . . ? C77 C76 N16 C80 1.1(9) . . . . ? C75 C76 N16 C80 -180.0(5) . . . . ? C77 C76 N16 Co4 175.3(5) . . . . ? C75 C76 N16 Co4 -5.8(7) . . . . ? C79 C80 N16 C76 -1.4(9) . . . . ? C81 C80 N16 C76 178.7(5) . . . . ? C79 C80 N16 Co4 -174.7(5) . . . . ? C81 C80 N16 Co4 5.3(8) . . . . ? O4 Co4 N16 C76 155.5(5) . . . . ? N15 Co4 N16 C76 4.4(4) . . . . ? N13 Co4 N16 C76 -92.8(4) . . . . ? N14 Co4 N16 C76 -51.0(9) . . . . ? O3 Co4 N16 C76 105.7(4) . . . . ? O4 Co4 N16 C80 -31.0(6) . . . . ? N15 Co4 N16 C80 178.0(5) . . . . ? N13 Co4 N16 C80 80.8(5) . . . . ? N14 Co4 N16 C80 122.5(8) . . . . ? O3 Co4 N16 C80 -80.7(5) . . . . ? N6 C30 C83 C84 -3(3) . . . . ? C29 C30 C83 C84 176(3) . . . . ? N12 C60 C84 C83 -158.9(18) . . . . ? C59 C60 C84 C83 22(2) . . . . ? O4 Co1 O1 Co2 162.9(5) . . . . ? N1 Co1 O1 Co2 161.2(4) . . . . ? N4 Co1 O1 Co2 56.1(4) . . . . ? N3 Co1 O1 Co2 -20.8(4) . . . . ? N2 Co1 O1 Co2 -113.6(4) . . . . ? O2 Co2 O1 Co1 -179.3(5) . . . . ? N5 Co2 O1 Co1 5.9(4) . . . . ? N6 Co2 O1 Co1 -70.9(4) . . . . ? N7 Co2 O1 Co1 -167.7(5) . . . . ? N8 Co2 O1 Co1 100.4(4) . . . . ? N9 Co3 O2 Co2 -12.3(11) . . . . ? N12 Co3 O2 Co2 -105.6(10) . . . . ? N10 Co3 O2 Co2 65.5(10) . . . . ? O3 Co3 O2 Co2 168.6(12) . . . . ? N11 Co3 O2 Co2 169.9(8) . . . . ? N5 Co2 O2 Co3 -144.1(8) . . . . ? N6 Co2 O2 Co3 125.0(10) . . . . ? N7 Co2 O2 Co3 29.5(11) . . . . ? N8 Co2 O2 Co3 -46.9(10) . . . . ? O1 Co2 O2 Co3 -154.6(12) . . . . ? N15 Co4 O4 Co1 -149.1(6) . . . . ? N16 Co4 O4 Co1 120.8(7) . . . . ? N13 Co4 O4 Co1 24.2(9) . . . . ? N14 Co4 O4 Co1 -52.0(8) . . . . ? O3 Co4 O4 Co1 -161.8(9) . . . . ? N1 Co1 O4 Co4 -5.1(8) . . . . ? N4 Co1 O4 Co4 -101.5(7) . . . . ? N3 Co1 O4 Co4 163.4(6) . . . . ? N2 Co1 O4 Co4 71.7(8) . . . . ? O1 Co1 O4 Co4 175.7(9) . . . . ? O2 Co3 O3 Co4 161.6(5) . . . . ? N9 Co3 O3 Co4 159.8(4) . . . . ? N12 Co3 O3 Co4 59.2(4) . . . . ? N10 Co3 O3 Co4 -112.9(4) . . . . ? N11 Co3 O3 Co4 -18.0(5) . . . . ? O4 Co4 O3 Co3 178.0(5) . . . . ? N15 Co4 O3 Co3 4.1(4) . . . . ? N16 Co4 O3 Co3 -73.3(4) . . . . ? N13 Co4 O3 Co3 -164.1(6) . . . . ? N14 Co4 O3 Co3 100.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.872 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.096