Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr S Brooker' _publ_contact_author_address ; Chemistry Department University of Otago PO Box 56 Dunedin NEW ZEALAND ; _publ_contact_author_email SBROOKER@ALKALI.OTAGO.AC.NZ _publ_section_title ; Dimetallic complexes of a structurally versatile pyridazine-containing Schiff-base macrocyclic ligand with pendant pyridine arms ; loop_ _publ_author_name 'S. Brooker' 'Markus Weitzer' data_mw31 _database_code_depnum_ccdc_archive 'CCDC 269194' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H38 Ba2 Cl4 N12 O17' _chemical_formula_weight 1279.22 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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0103(4) _cell_length_b 12.6609(6) _cell_length_c 21.3721(10) _cell_angle_alpha 87.3140(10) _cell_angle_beta 84.3930(10) _cell_angle_gamma 69.8730(10) _cell_volume 2278.03(18) _cell_formula_units_Z 2 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 2.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 83(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 SMART area detector' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20467 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 25.37 _reflns_number_total 8308 _reflns_number_gt 7319 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. All non-H ANIS. No disorder. H's calc and ride except on water O50 where they were found and x,y,z and U refined freely. Both of these are involved in H-bonds to perchlorate counter ions. ; _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^)+(0.0186P)^2^+3.5236P] 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 8308 _refine_ls_number_parameters 612 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0544 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Ba1 Ba 0.340457(18) 0.661527(13) 0.173712(7) 0.01372(5) Uani 1 1 d . . . Ba2 Ba 0.514653(18) 0.343420(13) 0.324997(7) 0.01382(5) Uani 1 1 d . . . N1 N 0.2723(3) 0.43104(19) 0.18113(11) 0.0161(5) Uani 1 1 d . . . N2 N 0.2774(3) 0.36550(19) 0.23266(11) 0.0160(5) Uani 1 1 d . . . C2 C 0.2049(3) 0.2888(2) 0.23515(14) 0.0176(6) Uani 1 1 d . . . C3 C 0.1170(3) 0.2762(3) 0.18757(15) 0.0230(7) Uani 1 1 d . . . H3 H 0.0610 0.2246 0.1918 0.028 Uiso 1 1 calc R . . C4 C 0.1147(3) 0.3413(2) 0.13453(14) 0.0215(6) Uani 1 1 d . . . H4 H 0.0588 0.3354 0.1002 0.026 Uiso 1 1 calc R . . C5 C 0.1973(3) 0.4168(2) 0.13254(13) 0.0162(6) Uani 1 1 d . . . C6 C 0.2020(3) 0.4853(2) 0.07476(13) 0.0164(6) Uani 1 1 d . . . H6 H 0.1638 0.4680 0.0380 0.020 Uiso 1 1 calc R . . N3 N 0.2549(3) 0.5660(2) 0.07260(11) 0.0168(5) Uani 1 1 d . . . C7 C 0.2427(3) 0.6315(2) 0.01361(13) 0.0195(6) Uani 1 1 d . . . H7A H 0.2146 0.5919 -0.0198 0.023 Uiso 1 1 calc R . . H7B H 0.3456 0.6410 -0.0002 0.023 Uiso 1 1 calc R . . C8 C 0.1149(3) 0.7455(2) 0.02536(14) 0.0199(6) Uani 1 1 d . . . H8A H 0.0995 0.7890 -0.0147 0.024 Uiso 1 1 calc R . . H8B H 0.0136 0.7345 0.0402 0.024 Uiso 1 1 calc R . . N4 N 0.1562(3) 0.8107(2) 0.07269(11) 0.0174(5) Uani 1 1 d . . . C9 C 0.0123(3) 0.8955(2) 0.10230(14) 0.0207(6) Uani 1 1 d . . . H9A H -0.0527 0.9392 0.0689 0.025 Uiso 1 1 calc R . . H9B H 0.0442 0.9483 0.1260 0.025 Uiso 1 1 calc R . . C10 C -0.0879(3) 0.8451(3) 0.14636(14) 0.0218(6) Uani 1 1 d . . . H10A H -0.1807 0.9063 0.1653 0.026 Uiso 1 1 calc R . . H10B H -0.1279 0.7972 0.1222 0.026 Uiso 1 1 calc R . . N5 N 0.0027(3) 0.7772(2) 0.19668(11) 0.0178(5) Uani 1 1 d . . . C11 C -0.0743(3) 0.7723(2) 0.24877(14) 0.0206(6) Uani 1 1 d . . . H11 H -0.1850 0.8130 0.2531 0.025 Uiso 1 1 calc R . . N6 N 0.1465(3) 0.6293(2) 0.29287(11) 0.0168(5) Uani 1 1 d . . . N7 N 0.2180(3) 0.56619(19) 0.34092(11) 0.0157(5) Uani 1 1 d . . . C12 C 0.0003(3) 0.7059(2) 0.30341(13) 0.0167(6) Uani 1 1 d . . . C13 C -0.0804(3) 0.7270(2) 0.36319(14) 0.0198(6) Uani 1 1 d . . . H13 H -0.1840 0.7810 0.3693 0.024 Uiso 1 1 calc R . . C14 C -0.0041(3) 0.6666(2) 0.41275(14) 0.0193(6) Uani 1 1 d . . . H14 H -0.0508 0.6801 0.4547 0.023 Uiso 1 1 calc R . . C15 C 0.1440(3) 0.5850(2) 0.39932(13) 0.0161(6) Uani 1 1 d . . . C16 C 0.2225(3) 0.5121(2) 0.45094(13) 0.0168(6) Uani 1 1 d . . . H16 H 0.1776 0.5303 0.4928 0.020 Uiso 1 1 calc R . . N8 N 0.3460(3) 0.4270(2) 0.44226(11) 0.0178(5) Uani 1 1 d . . . C17 C 0.4070(3) 0.3587(2) 0.49787(13) 0.0198(6) Uani 1 1 d . . . H17A H 0.3390 0.3919 0.5362 0.024 Uiso 1 1 calc R . . H17B H 0.5161 0.3569 0.5026 0.024 Uiso 1 1 calc R . . C18 C 0.4074(3) 0.2400(2) 0.48961(13) 0.0191(6) Uani 1 1 d . . . H18A H 0.4391 0.1956 0.5285 0.023 Uiso 1 1 calc R . . H18B H 0.2984 0.2433 0.4833 0.023 Uiso 1 1 calc R . . N9 N 0.5169(3) 0.18202(19) 0.43535(11) 0.0158(5) Uani 1 1 d . . . C19 C 0.4729(3) 0.0880(2) 0.41384(14) 0.0185(6) Uani 1 1 d . . . H19A H 0.4660 0.0381 0.4502 0.022 Uiso 1 1 calc R . . H19B H 0.5580 0.0434 0.3830 0.022 Uiso 1 1 calc R . . C20 C 0.3166(3) 0.1262(2) 0.38398(14) 0.0197(6) Uani 1 1 d . . . H20A H 0.2981 0.0599 0.3682 0.024 Uiso 1 1 calc R . . H20B H 0.2290 0.1625 0.4161 0.024 Uiso 1 1 calc R . . N10 N 0.3169(3) 0.2063(2) 0.33155(11) 0.0177(5) Uani 1 1 d . . . C21 C 0.2222(3) 0.2122(2) 0.29063(13) 0.0181(6) Uani 1 1 d . . . H21 H 0.1590 0.1654 0.2957 0.022 Uiso 1 1 calc R . . C30 C 0.2601(4) 0.8676(3) 0.04013(14) 0.0214(6) Uani 1 1 d . . . H30A H 0.2007 0.9206 0.0083 0.026 Uiso 1 1 calc R . . H30B H 0.3517 0.8105 0.0175 0.026 Uiso 1 1 calc R . . C31 C 0.3214(3) 0.9312(2) 0.08277(14) 0.0197(6) Uani 1 1 d . . . C32 C 0.3491(4) 1.0287(3) 0.05986(15) 0.0246(7) Uani 1 1 d . . . H32 H 0.3201 1.0580 0.0193 0.029 Uiso 1 1 calc R . . C33 C 0.4191(4) 1.0822(3) 0.09676(16) 0.0288(7) Uani 1 1 d . . . H33 H 0.4411 1.1475 0.0817 0.035 Uiso 1 1 calc R . . C34 C 0.4560(4) 1.0383(3) 0.15595(16) 0.0279(7) Uani 1 1 d . . . H34 H 0.5040 1.0730 0.1824 0.034 Uiso 1 1 calc R . . C35 C 0.4220(4) 0.9428(3) 0.17610(16) 0.0248(7) Uani 1 1 d . . . H35 H 0.4465 0.9139 0.2171 0.030 Uiso 1 1 calc R . . N30 N 0.3556(3) 0.8890(2) 0.14040(12) 0.0213(5) Uani 1 1 d . . . C40 C 0.6799(3) 0.1376(2) 0.45498(13) 0.0184(6) Uani 1 1 d . . . H40A H 0.6841 0.0824 0.4897 0.022 Uiso 1 1 calc R . . H40B H 0.7068 0.2001 0.4712 0.022 Uiso 1 1 calc R . . C41 C 0.8020(3) 0.0817(2) 0.40230(14) 0.0181(6) Uani 1 1 d . . . C42 C 0.9350(4) -0.0099(3) 0.41519(15) 0.0232(7) Uani 1 1 d . . . H42 H 0.9465 -0.0396 0.4568 0.028 Uiso 1 1 calc R . . C43 C 1.0504(4) -0.0575(3) 0.36721(16) 0.0257(7) Uani 1 1 d . . . H43 H 1.1434 -0.1188 0.3755 0.031 Uiso 1 1 calc R . . C44 C 1.0274(4) -0.0140(3) 0.30716(16) 0.0244(7) Uani 1 1 d . . . H44 H 1.1034 -0.0454 0.2730 0.029 Uiso 1 1 calc R . . C45 C 0.8909(3) 0.0766(2) 0.29757(14) 0.0215(6) Uani 1 1 d . . . H45 H 0.8758 0.1061 0.2561 0.026 Uiso 1 1 calc R . . N40 N 0.7788(3) 0.1250(2) 0.34394(12) 0.0194(5) Uani 1 1 d . . . O50 O 0.5791(3) 0.50251(19) 0.24054(12) 0.0260(5) Uani 1 1 d . . . H50A H 0.644(4) 0.461(3) 0.2101(17) 0.026(9) Uiso 1 1 d . . . H50B H 0.656(6) 0.531(5) 0.255(3) 0.091(18) Uiso 1 1 d . . . Cl1 Cl 0.48087(8) 0.75091(6) 0.33363(3) 0.02336(16) Uani 1 1 d . . . O11 O 0.3818(2) 0.76250(17) 0.28233(9) 0.0227(5) Uani 1 1 d . . . O12 O 0.3951(3) 0.7352(2) 0.39112(10) 0.0345(6) Uani 1 1 d . . . O13 O 0.6260(3) 0.6576(2) 0.32235(12) 0.0401(6) Uani 1 1 d . . . O14 O 0.5188(3) 0.8525(2) 0.33646(12) 0.0373(6) Uani 1 1 d . . . Cl2 Cl 0.69730(8) 0.65682(6) 0.08752(3) 0.01832(14) Uani 1 1 d . . . O21 O 0.5745(2) 0.61681(18) 0.06987(10) 0.0234(5) Uani 1 1 d . . . O22 O 0.6636(2) 0.68456(18) 0.15369(9) 0.0246(5) Uani 1 1 d . . . O23 O 0.8500(2) 0.57052(19) 0.07724(11) 0.0283(5) Uani 1 1 d . . . O24 O 0.6947(3) 0.75485(19) 0.05036(11) 0.0308(5) Uani 1 1 d . . . Cl3 Cl 0.70692(9) 0.25057(6) 0.14925(3) 0.02422(16) Uani 1 1 d . . . O31 O 0.6325(2) 0.23798(18) 0.21138(9) 0.0253(5) Uani 1 1 d . . . O32 O 0.5972(3) 0.2620(2) 0.10368(10) 0.0369(6) Uani 1 1 d . . . O33 O 0.7515(3) 0.3500(2) 0.14746(11) 0.0371(6) Uani 1 1 d . . . O34 O 0.8491(3) 0.1557(2) 0.13791(12) 0.0521(8) Uani 1 1 d . . . Cl4 Cl 0.85983(8) 0.36912(6) 0.38225(3) 0.01951(15) Uani 1 1 d . . . O41 O 0.6966(2) 0.40236(18) 0.40997(10) 0.0229(5) Uani 1 1 d . . . O42 O 0.8605(3) 0.34209(19) 0.31715(10) 0.0274(5) Uani 1 1 d . . . O43 O 0.9541(3) 0.2722(2) 0.41595(11) 0.0330(5) Uani 1 1 d . . . O44 O 0.9188(3) 0.4595(2) 0.38657(11) 0.0318(5) 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 Ba1 0.01443(8) 0.01443(9) 0.01328(9) 0.00111(6) -0.00220(6) -0.00607(6) Ba2 0.01448(8) 0.01510(9) 0.01238(9) -0.00029(6) -0.00153(6) -0.00558(7) N1 0.0163(12) 0.0171(12) 0.0157(12) 0.0004(9) -0.0037(9) -0.0062(10) N2 0.0167(12) 0.0183(12) 0.0131(12) 0.0011(9) -0.0021(9) -0.0060(10) C2 0.0140(13) 0.0194(15) 0.0196(15) 0.0011(12) -0.0021(11) -0.0059(12) C3 0.0225(15) 0.0254(16) 0.0268(17) 0.0049(13) -0.0084(13) -0.0144(13) C4 0.0225(15) 0.0232(16) 0.0214(16) 0.0035(12) -0.0108(12) -0.0093(13) C5 0.0156(14) 0.0162(14) 0.0170(14) 0.0002(11) -0.0023(11) -0.0053(11) C6 0.0137(13) 0.0211(15) 0.0141(14) -0.0013(11) -0.0026(11) -0.0050(12) N3 0.0171(12) 0.0188(12) 0.0153(12) 0.0015(10) -0.0023(9) -0.0070(10) C7 0.0260(15) 0.0230(15) 0.0125(14) 0.0025(11) -0.0043(12) -0.0117(13) C8 0.0225(15) 0.0230(15) 0.0169(15) 0.0045(12) -0.0078(12) -0.0104(13) N4 0.0194(12) 0.0175(12) 0.0167(12) 0.0026(10) -0.0034(10) -0.0076(10) C9 0.0215(15) 0.0170(14) 0.0212(16) 0.0029(12) -0.0067(12) -0.0025(12) C10 0.0165(14) 0.0279(17) 0.0193(15) 0.0032(13) -0.0051(12) -0.0050(12) N5 0.0178(12) 0.0185(12) 0.0183(13) 0.0010(10) -0.0046(10) -0.0070(10) C11 0.0155(14) 0.0211(15) 0.0245(16) -0.0017(12) -0.0012(12) -0.0054(12) N6 0.0173(12) 0.0173(12) 0.0171(12) 0.0008(10) -0.0032(10) -0.0074(10) N7 0.0169(12) 0.0162(12) 0.0156(12) 0.0004(9) -0.0022(9) -0.0077(10) C12 0.0143(13) 0.0186(14) 0.0191(15) -0.0010(11) -0.0010(11) -0.0080(12) C13 0.0166(14) 0.0189(15) 0.0232(16) -0.0009(12) 0.0006(12) -0.0060(12) C14 0.0229(15) 0.0190(15) 0.0174(15) -0.0017(12) 0.0021(12) -0.0097(12) C15 0.0180(14) 0.0166(14) 0.0170(14) -0.0013(11) -0.0008(11) -0.0100(12) C16 0.0190(14) 0.0192(15) 0.0132(14) -0.0024(11) 0.0001(11) -0.0080(12) N8 0.0181(12) 0.0215(13) 0.0145(12) -0.0001(10) -0.0014(9) -0.0075(11) C17 0.0224(15) 0.0226(15) 0.0127(14) 0.0002(12) -0.0018(11) -0.0054(12) C18 0.0210(15) 0.0215(15) 0.0141(14) 0.0030(12) 0.0006(11) -0.0073(12) N9 0.0146(11) 0.0170(12) 0.0149(12) -0.0001(9) -0.0023(9) -0.0039(10) C19 0.0231(15) 0.0170(14) 0.0184(15) 0.0042(12) -0.0044(12) -0.0105(12) C20 0.0203(15) 0.0215(15) 0.0199(15) 0.0067(12) -0.0040(12) -0.0109(12) N10 0.0170(12) 0.0181(12) 0.0182(13) 0.0026(10) -0.0019(10) -0.0067(10) C21 0.0182(14) 0.0188(15) 0.0197(15) 0.0015(12) -0.0024(12) -0.0092(12) C30 0.0251(16) 0.0210(15) 0.0189(15) 0.0072(12) -0.0043(12) -0.0094(13) C31 0.0167(14) 0.0177(15) 0.0244(16) 0.0027(12) -0.0010(12) -0.0060(12) C32 0.0256(16) 0.0208(16) 0.0274(17) 0.0033(13) 0.0005(13) -0.0092(13) C33 0.0300(17) 0.0200(16) 0.0366(19) 0.0022(14) 0.0039(14) -0.0111(14) C34 0.0244(16) 0.0229(16) 0.039(2) -0.0075(14) -0.0010(14) -0.0110(14) C35 0.0248(16) 0.0205(16) 0.0298(18) -0.0003(13) -0.0058(13) -0.0077(13) N30 0.0220(13) 0.0196(13) 0.0238(14) 0.0018(10) -0.0054(10) -0.0085(11) C40 0.0186(14) 0.0190(15) 0.0184(15) 0.0036(12) -0.0064(11) -0.0066(12) C41 0.0172(14) 0.0176(14) 0.0232(16) -0.0002(12) -0.0046(12) -0.0096(12) C42 0.0244(16) 0.0192(15) 0.0277(17) 0.0015(13) -0.0086(13) -0.0084(13) C43 0.0180(15) 0.0209(16) 0.0378(19) -0.0005(14) -0.0043(13) -0.0057(13) C44 0.0201(15) 0.0197(15) 0.0343(18) -0.0058(13) 0.0041(13) -0.0091(13) C45 0.0231(15) 0.0207(15) 0.0213(16) -0.0010(12) 0.0014(12) -0.0090(13) N40 0.0187(12) 0.0182(12) 0.0217(13) -0.0001(10) -0.0022(10) -0.0066(10) O50 0.0231(11) 0.0202(11) 0.0353(14) 0.0064(10) -0.0047(10) -0.0085(10) Cl1 0.0205(4) 0.0258(4) 0.0219(4) -0.0030(3) -0.0063(3) -0.0040(3) O11 0.0249(11) 0.0259(11) 0.0197(11) -0.0010(9) -0.0075(9) -0.0102(9) O12 0.0332(13) 0.0485(15) 0.0203(12) 0.0072(11) -0.0084(10) -0.0113(11) O13 0.0283(13) 0.0349(14) 0.0493(16) -0.0101(12) -0.0118(11) 0.0025(11) O14 0.0420(14) 0.0319(13) 0.0450(15) -0.0053(11) -0.0147(12) -0.0178(11) Cl2 0.0165(3) 0.0216(4) 0.0184(3) 0.0008(3) -0.0011(3) -0.0088(3) O21 0.0169(10) 0.0317(12) 0.0257(12) -0.0044(9) -0.0016(8) -0.0129(9) O22 0.0255(11) 0.0325(13) 0.0183(11) -0.0026(9) -0.0004(9) -0.0130(10) O23 0.0173(11) 0.0327(13) 0.0340(13) -0.0051(10) -0.0013(9) -0.0068(9) O24 0.0347(13) 0.0320(13) 0.0306(13) 0.0129(10) -0.0065(10) -0.0185(11) Cl3 0.0277(4) 0.0272(4) 0.0154(3) -0.0021(3) 0.0005(3) -0.0067(3) O31 0.0286(12) 0.0278(12) 0.0156(11) -0.0014(9) 0.0034(9) -0.0059(10) O32 0.0486(15) 0.0561(16) 0.0193(12) 0.0022(11) -0.0082(11) -0.0339(13) O33 0.0412(14) 0.0499(16) 0.0323(14) -0.0028(11) 0.0011(11) -0.0320(13) O34 0.0548(17) 0.0443(16) 0.0315(15) -0.0001(12) 0.0134(13) 0.0112(13) Cl4 0.0170(3) 0.0223(4) 0.0208(4) -0.0031(3) -0.0011(3) -0.0086(3) O41 0.0156(10) 0.0292(12) 0.0246(11) -0.0072(9) 0.0017(8) -0.0086(9) O42 0.0307(12) 0.0325(13) 0.0201(11) -0.0071(9) 0.0007(9) -0.0121(10) O43 0.0249(12) 0.0338(13) 0.0377(14) 0.0083(11) -0.0088(10) -0.0061(10) O44 0.0304(12) 0.0340(13) 0.0391(14) -0.0071(11) 0.0001(10) -0.0215(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 Ba1 O11 2.817(2) . y Ba1 N3 2.818(2) . y Ba1 O50 2.841(2) . y Ba1 O21 2.842(2) . y Ba1 N5 2.891(2) . y Ba1 N30 2.980(2) . y Ba1 O22 3.013(2) . y Ba1 N4 3.024(2) . Y Ba1 N6 3.038(2) . Y Ba1 N1 3.176(2) . Y Ba1 Cl2 3.5292(7) . Y Ba2 O31 2.762(2) . Y Ba2 O50 2.813(2) . Y Ba2 O41 2.845(2) . Y Ba2 N8 2.847(2) . Y Ba2 N10 2.875(2) . Y Ba2 N2 2.984(2) . Y Ba2 N40 3.005(2) . Y Ba2 N9 3.044(2) . Y Ba2 O42 3.098(2) . Y Ba2 N7 3.153(2) . Y Ba2 Cl4 3.5711(7) . Y N1 N2 1.342(3) . ? N1 C5 1.344(4) . ? N2 C2 1.340(4) . ? C2 C3 1.395(4) . ? C2 C21 1.481(4) . ? C3 C4 1.368(4) . ? C4 C5 1.395(4) . ? C5 C6 1.481(4) . ? C6 N3 1.265(4) . ? N3 C7 1.468(4) . ? C7 C8 1.519(4) . ? C8 N4 1.485(4) . ? N4 C30 1.473(4) . ? N4 C9 1.476(4) . ? C9 C10 1.511(4) . ? C10 N5 1.471(4) . ? N5 C11 1.263(4) . ? C11 C12 1.481(4) . ? N6 N7 1.344(3) . ? N6 C12 1.346(4) . ? N7 C15 1.347(4) . ? C12 C13 1.396(4) . ? C13 C14 1.372(4) . ? C14 C15 1.391(4) . ? C15 C16 1.475(4) . ? C16 N8 1.260(4) . ? N8 C17 1.472(4) . ? C17 C18 1.519(4) . ? C18 N9 1.489(4) . ? N9 C40 1.476(3) . ? N9 C19 1.482(4) . ? C19 C20 1.517(4) . ? C20 N10 1.476(4) . ? N10 C21 1.263(4) . ? C30 C31 1.503(4) . ? C31 N30 1.341(4) . ? C31 C32 1.399(4) . ? C32 C33 1.386(5) . ? C33 C34 1.382(5) . ? C34 C35 1.386(4) . ? C35 N30 1.350(4) . ? C40 C41 1.509(4) . ? C41 N40 1.345(4) . ? C41 C42 1.390(4) . ? C42 C43 1.384(4) . ? C43 C44 1.379(5) . ? C44 C45 1.388(4) . ? C45 N40 1.346(4) . ? Cl1 O12 1.430(2) . ? Cl1 O13 1.438(2) . ? Cl1 O14 1.445(2) . ? Cl1 O11 1.451(2) . ? Cl2 O24 1.436(2) . ? Cl2 O23 1.437(2) . ? Cl2 O22 1.451(2) . ? Cl2 O21 1.452(2) . ? Cl3 O32 1.423(2) . ? Cl3 O34 1.432(3) . ? Cl3 O33 1.446(2) . ? Cl3 O31 1.455(2) . ? Cl4 O44 1.428(2) . ? Cl4 O43 1.437(2) . ? Cl4 O42 1.447(2) . ? Cl4 O41 1.455(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Ba1 N3 171.90(6) . . Y O11 Ba1 O50 70.76(7) . . Y N3 Ba1 O50 112.85(7) . . Y O11 Ba1 O21 120.24(6) . . Y N3 Ba1 O21 67.74(6) . . Y O50 Ba1 O21 85.56(6) . . Y O11 Ba1 N5 88.29(6) . . Y N3 Ba1 N5 84.21(7) . . Y O50 Ba1 N5 135.63(7) . . Y O21 Ba1 N5 137.80(6) . . Y O11 Ba1 N30 70.62(6) . . Y N3 Ba1 N30 111.66(7) . . Y O50 Ba1 N30 120.97(7) . . Y O21 Ba1 N30 77.42(6) . . Y N5 Ba1 N30 85.07(7) . . Y O11 Ba1 O22 73.33(6) . . Y N3 Ba1 O22 114.72(6) . . Y O50 Ba1 O22 64.84(6) . . Y O21 Ba1 O22 47.07(6) . . Y N5 Ba1 O22 146.23(6) . . Y N30 Ba1 O22 62.35(6) . . Y O11 Ba1 N4 118.65(6) . . Y N3 Ba1 N4 59.73(7) . . Y O50 Ba1 N4 164.16(7) . . Y O21 Ba1 N4 78.65(6) . . Y N5 Ba1 N4 59.76(6) . . Y N30 Ba1 N4 56.88(7) . . Y O22 Ba1 N4 104.28(6) . . Y O11 Ba1 N6 64.22(6) . . Y N3 Ba1 N6 108.76(6) . . Y O50 Ba1 N6 79.09(6) . . Y O21 Ba1 N6 161.43(6) . . Y N5 Ba1 N6 56.54(6) . . Y N30 Ba1 N6 119.56(7) . . Y O22 Ba1 N6 131.30(6) . . Y N4 Ba1 N6 116.14(6) . . Y O11 Ba1 N1 121.51(6) . . Y N3 Ba1 N1 55.30(6) . . Y O50 Ba1 N1 72.03(6) . . Y O21 Ba1 N1 99.75(6) . . Y N5 Ba1 N1 88.20(6) . . Y N30 Ba1 N1 165.99(6) . . Y O22 Ba1 N1 125.54(6) . . Y N4 Ba1 N1 109.15(6) . . Y N6 Ba1 N1 65.65(6) . . Y O11 Ba1 Cl2 96.94(4) . . Y N3 Ba1 Cl2 91.02(5) . . Y O50 Ba1 Cl2 76.37(5) . . Y O21 Ba1 Cl2 23.30(4) . . Y N5 Ba1 Cl2 146.63(5) . . Y N30 Ba1 Cl2 66.06(5) . . Y O22 Ba1 Cl2 24.00(4) . . Y N4 Ba1 Cl2 89.40(5) . . Y N6 Ba1 Cl2 153.06(4) . . Y N1 Ba1 Cl2 115.91(4) . . Y O31 Ba2 O50 72.48(7) . . Y O31 Ba2 O41 125.33(6) . . Y O50 Ba2 O41 87.24(7) . . Y O31 Ba2 N8 167.66(7) . . Y O50 Ba2 N8 116.39(7) . . Y O41 Ba2 N8 65.45(6) . . Y O31 Ba2 N10 83.53(7) . . Y O50 Ba2 N10 136.69(7) . . Y O41 Ba2 N10 135.52(6) . . Y N8 Ba2 N10 84.20(7) . . Y O31 Ba2 N2 63.90(6) . . Y O50 Ba2 N2 79.62(7) . . Y O41 Ba2 N2 160.70(6) . . Y N8 Ba2 N2 107.97(6) . . Y N10 Ba2 N2 57.34(6) . . Y O31 Ba2 N40 69.56(6) . . Y O50 Ba2 N40 117.83(7) . . Y O41 Ba2 N40 77.22(6) . . Y N8 Ba2 N40 110.51(7) . . Y N10 Ba2 N40 84.67(6) . . Y N2 Ba2 N40 121.46(7) . . Y O31 Ba2 N9 113.91(6) . . Y O50 Ba2 N9 163.96(7) . . Y O41 Ba2 N9 77.09(6) . . Y N8 Ba2 N9 60.06(6) . . Y N10 Ba2 N9 59.31(6) . . Y N2 Ba2 N9 116.41(6) . . Y N40 Ba2 N9 55.62(6) . . Y O31 Ba2 O42 79.52(6) . . Y O50 Ba2 O42 65.16(6) . . Y O41 Ba2 O42 46.20(5) . . Y N8 Ba2 O42 111.64(6) . . Y N10 Ba2 O42 145.17(6) . . Y N2 Ba2 O42 135.46(6) . . Y N40 Ba2 O42 60.94(6) . . Y N9 Ba2 O42 100.73(6) . . Y O31 Ba2 N7 123.80(6) . . Y O50 Ba2 N7 73.56(6) . . Y O41 Ba2 N7 95.91(6) . . Y N8 Ba2 N7 55.43(6) . . Y N10 Ba2 N7 92.05(6) . . Y N2 Ba2 N7 66.92(6) . . Y N40 Ba2 N7 165.88(6) . . Y N9 Ba2 N7 111.08(6) . . Y O42 Ba2 N7 122.65(6) . . Y O31 Ba2 Cl4 102.51(5) . . Y O50 Ba2 Cl4 78.03(5) . . Y O41 Ba2 Cl4 22.82(4) . . Y N8 Ba2 Cl4 88.17(5) . . Y N10 Ba2 Cl4 143.56(5) . . Y N2 Ba2 Cl4 156.63(5) . . Y N40 Ba2 Cl4 64.85(5) . . Y N9 Ba2 Cl4 86.11(4) . . Y O42 Ba2 Cl4 23.73(4) . . Y N7 Ba2 Cl4 112.51(4) . . Y N2 N1 C5 119.2(2) . . ? N2 N1 Ba1 125.49(16) . . ? C5 N1 Ba1 113.27(17) . . ? C2 N2 N1 119.4(2) . . ? C2 N2 Ba2 117.98(17) . . ? N1 N2 Ba2 120.56(16) . . ? N2 C2 C3 123.3(3) . . ? N2 C2 C21 118.2(2) . . ? C3 C2 C21 118.6(3) . . ? C4 C3 C2 117.2(3) . . ? C3 C4 C5 117.8(3) . . ? N1 C5 C4 122.9(3) . . ? N1 C5 C6 118.2(2) . . ? C4 C5 C6 119.0(3) . . ? N3 C6 C5 122.3(3) . . ? C6 N3 C7 116.5(2) . . ? C6 N3 Ba1 127.53(19) . . ? C7 N3 Ba1 114.84(17) . . ? N3 C7 C8 107.9(2) . . ? N4 C8 C7 112.1(2) . . ? C30 N4 C9 109.4(2) . . ? C30 N4 C8 107.9(2) . . ? C9 N4 C8 110.9(2) . . ? C30 N4 Ba1 106.76(16) . . ? C9 N4 Ba1 109.31(16) . . ? C8 N4 Ba1 112.37(16) . . ? N4 C9 C10 113.4(2) . . ? N5 C10 C9 111.7(2) . . ? C11 N5 C10 116.9(2) . . ? C11 N5 Ba1 123.07(19) . . ? C10 N5 Ba1 120.06(17) . . ? N5 C11 C12 123.0(3) . . ? N7 N6 C12 119.6(2) . . ? N7 N6 Ba1 120.58(16) . . ? C12 N6 Ba1 116.54(17) . . ? N6 N7 C15 118.9(2) . . ? N6 N7 Ba2 124.32(16) . . ? C15 N7 Ba2 115.56(17) . . ? N6 C12 C13 122.9(3) . . ? N6 C12 C11 117.6(2) . . ? C13 C12 C11 119.4(3) . . ? C14 C13 C12 117.4(3) . . ? C13 C14 C15 117.6(3) . . ? N7 C15 C14 123.3(3) . . ? N7 C15 C16 117.8(2) . . ? C14 C15 C16 118.8(3) . . ? N8 C16 C15 123.3(3) . . ? C16 N8 C17 117.5(2) . . ? C16 N8 Ba2 127.08(19) . . ? C17 N8 Ba2 115.37(16) . . ? N8 C17 C18 108.8(2) . . ? N9 C18 C17 112.6(2) . . ? C40 N9 C19 109.3(2) . . ? C40 N9 C18 108.7(2) . . ? C19 N9 C18 111.1(2) . . ? C40 N9 Ba2 107.76(16) . . ? C19 N9 Ba2 108.49(15) . . ? C18 N9 Ba2 111.46(16) . . ? N9 C19 C20 113.6(2) . . ? N10 C20 C19 111.2(2) . . ? C21 N10 C20 115.6(2) . . ? C21 N10 Ba2 122.36(19) . . ? C20 N10 Ba2 122.06(17) . . ? N10 C21 C2 123.1(3) . . ? N4 C30 C31 114.3(2) . . ? N30 C31 C32 122.3(3) . . ? N30 C31 C30 118.6(2) . . ? C32 C31 C30 119.0(3) . . ? C33 C32 C31 119.4(3) . . ? C34 C33 C32 118.4(3) . . ? C33 C34 C35 119.0(3) . . ? N30 C35 C34 123.3(3) . . ? C31 N30 C35 117.5(3) . . ? C31 N30 Ba1 118.66(19) . . ? C35 N30 Ba1 122.74(19) . . ? N9 C40 C41 113.0(2) . . ? N40 C41 C42 122.2(3) . . ? N40 C41 C40 117.8(2) . . ? C42 C41 C40 120.0(3) . . ? C43 C42 C41 119.8(3) . . ? C44 C43 C42 118.4(3) . . ? C43 C44 C45 118.7(3) . . ? N40 C45 C44 123.5(3) . . ? C41 N40 C45 117.3(2) . . ? C41 N40 Ba2 119.62(18) . . ? C45 N40 Ba2 122.27(19) . . ? Ba2 O50 Ba1 122.47(8) . . ? O12 Cl1 O13 111.06(15) . . ? O12 Cl1 O14 109.83(15) . . ? O13 Cl1 O14 108.69(15) . . ? O12 Cl1 O11 108.84(13) . . ? O13 Cl1 O11 109.82(14) . . ? O14 Cl1 O11 108.57(13) . . ? Cl1 O11 Ba1 145.17(12) . . ? O24 Cl2 O23 109.69(14) . . ? O24 Cl2 O22 110.31(14) . . ? O23 Cl2 O22 109.95(13) . . ? O24 Cl2 O21 109.26(13) . . ? O23 Cl2 O21 109.97(13) . . ? O22 Cl2 O21 107.63(12) . . ? O24 Cl2 Ba1 117.46(10) . . ? O23 Cl2 Ba1 132.65(10) . . ? O22 Cl2 Ba1 57.62(8) . . ? O21 Cl2 Ba1 50.72(8) . . ? Cl2 O21 Ba1 105.99(11) . . ? Cl2 O22 Ba1 98.39(10) . . ? O32 Cl3 O34 112.44(17) . . ? O32 Cl3 O33 109.28(15) . . ? O34 Cl3 O33 107.58(17) . . ? O32 Cl3 O31 109.20(14) . . ? O34 Cl3 O31 108.86(14) . . ? O33 Cl3 O31 109.45(14) . . ? Cl3 O31 Ba2 143.75(13) . . ? O44 Cl4 O43 109.88(14) . . ? O44 Cl4 O42 110.56(14) . . ? O43 Cl4 O42 110.44(14) . . ? O44 Cl4 O41 109.58(13) . . ? O43 Cl4 O41 108.66(13) . . ? O42 Cl4 O41 107.67(13) . . ? O44 Cl4 Ba2 134.62(10) . . ? O43 Cl4 Ba2 114.98(10) . . ? O42 Cl4 Ba2 59.48(9) . . ? O41 Cl4 Ba2 49.30(8) . . ? Cl4 O41 Ba2 107.87(10) . . ? Cl4 O42 Ba2 96.79(10) . . ? 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 O11 Ba1 N1 N2 -7.9(2) . . . . ? N3 Ba1 N1 N2 -179.0(2) . . . . ? O50 Ba1 N1 N2 44.89(19) . . . . ? O21 Ba1 N1 N2 126.94(19) . . . . ? N5 Ba1 N1 N2 -94.8(2) . . . . ? N30 Ba1 N1 N2 -156.0(2) . . . . ? O22 Ba1 N1 N2 83.5(2) . . . . ? N4 Ba1 N1 N2 -151.78(19) . . . . ? N6 Ba1 N1 N2 -41.00(19) . . . . ? Cl2 Ba1 N1 N2 109.23(19) . . . . ? O11 Ba1 N1 C5 155.82(17) . . . . ? N3 Ba1 N1 C5 -15.28(17) . . . . ? O50 Ba1 N1 C5 -151.43(19) . . . . ? O21 Ba1 N1 C5 -69.38(19) . . . . ? N5 Ba1 N1 C5 68.93(18) . . . . ? N30 Ba1 N1 C5 7.7(4) . . . . ? O22 Ba1 N1 C5 -112.78(18) . . . . ? N4 Ba1 N1 C5 11.90(19) . . . . ? N6 Ba1 N1 C5 122.68(19) . . . . ? Cl2 Ba1 N1 C5 -87.09(18) . . . . ? C5 N1 N2 C2 -1.4(4) . . . . ? Ba1 N1 N2 C2 161.42(19) . . . . ? C5 N1 N2 Ba2 161.96(19) . . . . ? Ba1 N1 N2 Ba2 -35.2(2) . . . . ? O31 Ba2 N2 C2 91.5(2) . . . . ? O50 Ba2 N2 C2 167.0(2) . . . . ? O41 Ba2 N2 C2 -145.2(2) . . . . ? N8 Ba2 N2 C2 -78.5(2) . . . . ? N10 Ba2 N2 C2 -7.98(18) . . . . ? N40 Ba2 N2 C2 50.6(2) . . . . ? N9 Ba2 N2 C2 -13.6(2) . . . . ? O42 Ba2 N2 C2 129.64(19) . . . . ? N7 Ba2 N2 C2 -116.6(2) . . . . ? Cl4 Ba2 N2 C2 149.80(16) . . . . ? O31 Ba2 N2 N1 -72.04(18) . . . . ? O50 Ba2 N2 N1 3.42(18) . . . . ? O41 Ba2 N2 N1 51.3(3) . . . . ? N8 Ba2 N2 N1 117.98(18) . . . . ? N10 Ba2 N2 N1 -171.5(2) . . . . ? N40 Ba2 N2 N1 -112.96(18) . . . . ? N9 Ba2 N2 N1 -177.15(17) . . . . ? O42 Ba2 N2 N1 -33.9(2) . . . . ? N7 Ba2 N2 N1 79.85(19) . . . . ? Cl4 Ba2 N2 N1 -13.8(3) . . . . ? N1 N2 C2 C3 -3.0(4) . . . . ? Ba2 N2 C2 C3 -166.7(2) . . . . ? N1 N2 C2 C21 175.7(2) . . . . ? Ba2 N2 C2 C21 12.0(3) . . . . ? N2 C2 C3 C4 4.3(5) . . . . ? C21 C2 C3 C4 -174.4(3) . . . . ? C2 C3 C4 C5 -1.3(4) . . . . ? N2 N1 C5 C4 4.3(4) . . . . ? Ba1 N1 C5 C4 -160.5(2) . . . . ? N2 N1 C5 C6 -176.3(2) . . . . ? Ba1 N1 C5 C6 18.9(3) . . . . ? C3 C4 C5 N1 -2.9(4) . . . . ? C3 C4 C5 C6 177.7(3) . . . . ? N1 C5 C6 N3 -9.6(4) . . . . ? C4 C5 C6 N3 169.9(3) . . . . ? C5 C6 N3 C7 -176.1(2) . . . . ? C5 C6 N3 Ba1 -8.7(4) . . . . ? O11 Ba1 N3 C6 -57.0(6) . . . . ? O50 Ba1 N3 C6 58.0(2) . . . . ? O21 Ba1 N3 C6 132.7(2) . . . . ? N5 Ba1 N3 C6 -79.5(2) . . . . ? N30 Ba1 N3 C6 -161.8(2) . . . . ? O22 Ba1 N3 C6 129.7(2) . . . . ? N4 Ba1 N3 C6 -137.7(2) . . . . ? N6 Ba1 N3 C6 -27.8(2) . . . . ? N1 Ba1 N3 C6 12.3(2) . . . . ? Cl2 Ba1 N3 C6 133.6(2) . . . . ? O11 Ba1 N3 C7 110.6(4) . . . . ? O50 Ba1 N3 C7 -134.44(17) . . . . ? O21 Ba1 N3 C7 -59.70(18) . . . . ? N5 Ba1 N3 C7 88.08(18) . . . . ? N30 Ba1 N3 C7 5.73(19) . . . . ? O22 Ba1 N3 C7 -62.74(19) . . . . ? N4 Ba1 N3 C7 29.88(17) . . . . ? N6 Ba1 N3 C7 139.79(17) . . . . ? N1 Ba1 N3 C7 179.9(2) . . . . ? Cl2 Ba1 N3 C7 -58.82(18) . . . . ? C6 N3 C7 C8 108.1(3) . . . . ? Ba1 N3 C7 C8 -60.9(2) . . . . ? N3 C7 C8 N4 62.9(3) . . . . ? C7 C8 N4 C30 83.3(3) . . . . ? C7 C8 N4 C9 -156.8(2) . . . . ? C7 C8 N4 Ba1 -34.1(3) . . . . ? O11 Ba1 N4 C30 74.08(18) . . . . ? N3 Ba1 N4 C30 -115.04(18) . . . . ? O50 Ba1 N4 C30 -49.3(3) . . . . ? O21 Ba1 N4 C30 -44.33(17) . . . . ? N5 Ba1 N4 C30 143.12(19) . . . . ? N30 Ba1 N4 C30 37.95(16) . . . . ? O22 Ba1 N4 C30 -4.50(18) . . . . ? N6 Ba1 N4 C30 147.58(16) . . . . ? N1 Ba1 N4 C30 -140.82(17) . . . . ? Cl2 Ba1 N4 C30 -23.51(17) . . . . ? O11 Ba1 N4 C9 -44.21(19) . . . . ? N3 Ba1 N4 C9 126.67(19) . . . . ? O50 Ba1 N4 C9 -167.5(2) . . . . ? O21 Ba1 N4 C9 -162.62(18) . . . . ? N5 Ba1 N4 C9 24.83(16) . . . . ? N30 Ba1 N4 C9 -80.34(18) . . . . ? O22 Ba1 N4 C9 -122.79(17) . . . . ? N6 Ba1 N4 C9 29.29(19) . . . . ? N1 Ba1 N4 C9 100.89(18) . . . . ? Cl2 Ba1 N4 C9 -141.80(17) . . . . ? O11 Ba1 N4 C8 -167.84(16) . . . . ? N3 Ba1 N4 C8 3.04(16) . . . . ? O50 Ba1 N4 C8 68.8(3) . . . . ? O21 Ba1 N4 C8 73.75(17) . . . . ? N5 Ba1 N4 C8 -98.80(18) . . . . ? N30 Ba1 N4 C8 156.0(2) . . . . ? O22 Ba1 N4 C8 113.58(17) . . . . ? N6 Ba1 N4 C8 -94.34(18) . . . . ? N1 Ba1 N4 C8 -22.74(18) . . . . ? Cl2 Ba1 N4 C8 94.57(17) . . . . ? C30 N4 C9 C10 -169.7(2) . . . . ? C8 N4 C9 C10 71.3(3) . . . . ? Ba1 N4 C9 C10 -53.1(3) . . . . ? N4 C9 C10 N5 57.6(3) . . . . ? C9 C10 N5 C11 149.9(3) . . . . ? C9 C10 N5 Ba1 -30.5(3) . . . . ? O11 Ba1 N5 C11 -52.4(2) . . . . ? N3 Ba1 N5 C11 124.5(2) . . . . ? O50 Ba1 N5 C11 7.5(3) . . . . ? O21 Ba1 N5 C11 171.8(2) . . . . ? N30 Ba1 N5 C11 -123.1(2) . . . . ? O22 Ba1 N5 C11 -108.3(2) . . . . ? N4 Ba1 N5 C11 -177.3(3) . . . . ? N6 Ba1 N5 C11 7.5(2) . . . . ? N1 Ba1 N5 C11 69.2(2) . . . . ? Cl2 Ba1 N5 C11 -152.47(19) . . . . ? O11 Ba1 N5 C10 128.0(2) . . . . ? N3 Ba1 N5 C10 -55.1(2) . . . . ? O50 Ba1 N5 C10 -172.13(18) . . . . ? O21 Ba1 N5 C10 -7.8(2) . . . . ? N30 Ba1 N5 C10 57.3(2) . . . . ? O22 Ba1 N5 C10 72.1(2) . . . . ? N4 Ba1 N5 C10 3.07(19) . . . . ? N6 Ba1 N5 C10 -172.1(2) . . . . ? N1 Ba1 N5 C10 -110.4(2) . . . . ? Cl2 Ba1 N5 C10 27.9(2) . . . . ? C10 N5 C11 C12 179.1(3) . . . . ? Ba1 N5 C11 C12 -0.5(4) . . . . ? O11 Ba1 N6 N7 -67.90(18) . . . . ? N3 Ba1 N6 N7 116.48(18) . . . . ? O50 Ba1 N6 N7 5.86(18) . . . . ? O21 Ba1 N6 N7 40.7(3) . . . . ? N5 Ba1 N6 N7 -174.1(2) . . . . ? N30 Ba1 N6 N7 -113.68(18) . . . . ? O22 Ba1 N6 N7 -35.9(2) . . . . ? N4 Ba1 N6 N7 -178.76(17) . . . . ? N1 Ba1 N6 N7 80.93(19) . . . . ? Cl2 Ba1 N6 N7 -18.7(3) . . . . ? O11 Ba1 N6 C12 91.7(2) . . . . ? N3 Ba1 N6 C12 -83.9(2) . . . . ? O50 Ba1 N6 C12 165.5(2) . . . . ? O21 Ba1 N6 C12 -159.72(19) . . . . ? N5 Ba1 N6 C12 -14.52(18) . . . . ? N30 Ba1 N6 C12 45.9(2) . . . . ? O22 Ba1 N6 C12 123.69(18) . . . . ? N4 Ba1 N6 C12 -19.1(2) . . . . ? N1 Ba1 N6 C12 -119.5(2) . . . . ? Cl2 Ba1 N6 C12 140.87(16) . . . . ? C12 N6 N7 C15 -3.1(4) . . . . ? Ba1 N6 N7 C15 155.91(19) . . . . ? C12 N6 N7 Ba2 163.74(18) . . . . ? Ba1 N6 N7 Ba2 -37.3(2) . . . . ? O31 Ba2 N7 N6 -9.2(2) . . . . ? O50 Ba2 N7 N6 45.72(19) . . . . ? O41 Ba2 N7 N6 131.08(19) . . . . ? N8 Ba2 N7 N6 -174.3(2) . . . . ? N10 Ba2 N7 N6 -92.75(19) . . . . ? N2 Ba2 N7 N6 -39.78(18) . . . . ? N40 Ba2 N7 N6 -168.9(2) . . . . ? N9 Ba2 N7 N6 -150.50(18) . . . . ? O42 Ba2 N7 N6 90.55(19) . . . . ? Cl4 Ba2 N7 N6 114.85(18) . . . . ? O31 Ba2 N7 C15 158.05(17) . . . . ? O50 Ba2 N7 C15 -147.1(2) . . . . ? O41 Ba2 N7 C15 -61.70(19) . . . . ? N8 Ba2 N7 C15 -7.05(17) . . . . ? N10 Ba2 N7 C15 74.47(19) . . . . ? N2 Ba2 N7 C15 127.4(2) . . . . ? N40 Ba2 N7 C15 -1.7(4) . . . . ? N9 Ba2 N7 C15 16.7(2) . . . . ? O42 Ba2 N7 C15 -102.23(19) . . . . ? Cl4 Ba2 N7 C15 -77.93(19) . . . . ? N7 N6 C12 C13 2.7(4) . . . . ? Ba1 N6 C12 C13 -157.2(2) . . . . ? N7 N6 C12 C11 -179.2(2) . . . . ? Ba1 N6 C12 C11 21.0(3) . . . . ? N5 C11 C12 N6 -14.9(4) . . . . ? N5 C11 C12 C13 163.3(3) . . . . ? N6 C12 C13 C14 0.7(4) . . . . ? C11 C12 C13 C14 -177.5(3) . . . . ? C12 C13 C14 C15 -3.3(4) . . . . ? N6 N7 C15 C14 0.3(4) . . . . ? Ba2 N7 C15 C14 -167.7(2) . . . . ? N6 N7 C15 C16 178.0(2) . . . . ? Ba2 N7 C15 C16 10.1(3) . . . . ? C13 C14 C15 N7 3.0(4) . . . . ? C13 C14 C15 C16 -174.7(3) . . . . ? N7 C15 C16 N8 -7.3(4) . . . . ? C14 C15 C16 N8 170.5(3) . . . . ? C15 C16 N8 C17 -177.0(2) . . . . ? C15 C16 N8 Ba2 -0.5(4) . . . . ? O31 Ba2 N8 C16 -86.8(4) . . . . ? O50 Ba2 N8 C16 47.3(3) . . . . ? O41 Ba2 N8 C16 120.7(2) . . . . ? N10 Ba2 N8 C16 -92.7(2) . . . . ? N2 Ba2 N8 C16 -39.8(2) . . . . ? N40 Ba2 N8 C16 -174.8(2) . . . . ? N9 Ba2 N8 C16 -150.4(3) . . . . ? O42 Ba2 N8 C16 119.4(2) . . . . ? N7 Ba2 N8 C16 3.8(2) . . . . ? Cl4 Ba2 N8 C16 123.0(2) . . . . ? O31 Ba2 N8 C17 89.8(3) . . . . ? O50 Ba2 N8 C17 -136.11(18) . . . . ? O41 Ba2 N8 C17 -62.71(18) . . . . ? N10 Ba2 N8 C17 83.89(19) . . . . ? N2 Ba2 N8 C17 136.79(18) . . . . ? N40 Ba2 N8 C17 1.8(2) . . . . ? N9 Ba2 N8 C17 26.13(17) . . . . ? O42 Ba2 N8 C17 -64.03(19) . . . . ? N7 Ba2 N8 C17 -179.6(2) . . . . ? Cl4 Ba2 N8 C17 -60.43(18) . . . . ? C16 N8 C17 C18 119.7(3) . . . . ? Ba2 N8 C17 C18 -57.2(3) . . . . ? N8 C17 C18 N9 63.8(3) . . . . ? C17 C18 N9 C40 80.9(3) . . . . ? C17 C18 N9 C19 -158.8(2) . . . . ? C17 C18 N9 Ba2 -37.7(3) . . . . ? O31 Ba2 N9 C40 79.47(17) . . . . ? O50 Ba2 N9 C40 -31.0(3) . . . . ? O41 Ba2 N9 C40 -43.71(16) . . . . ? N8 Ba2 N9 C40 -112.62(18) . . . . ? N10 Ba2 N9 C40 145.48(18) . . . . ? N2 Ba2 N9 C40 150.98(16) . . . . ? N40 Ba2 N9 C40 39.50(16) . . . . ? O42 Ba2 N9 C40 -3.72(17) . . . . ? N7 Ba2 N9 C40 -135.14(16) . . . . ? Cl4 Ba2 N9 C40 -22.49(16) . . . . ? O31 Ba2 N9 C19 -38.77(18) . . . . ? O50 Ba2 N9 C19 -149.3(2) . . . . ? O41 Ba2 N9 C19 -161.96(17) . . . . ? N8 Ba2 N9 C19 129.14(18) . . . . ? N10 Ba2 N9 C19 27.24(16) . . . . ? N2 Ba2 N9 C19 32.74(18) . . . . ? N40 Ba2 N9 C19 -78.74(17) . . . . ? O42 Ba2 N9 C19 -121.96(16) . . . . ? N7 Ba2 N9 C19 106.62(16) . . . . ? Cl4 Ba2 N9 C19 -140.74(16) . . . . ? O31 Ba2 N9 C18 -161.35(17) . . . . ? O50 Ba2 N9 C18 88.1(3) . . . . ? O41 Ba2 N9 C18 75.47(17) . . . . ? N8 Ba2 N9 C18 6.56(16) . . . . ? N10 Ba2 N9 C18 -95.34(18) . . . . ? N2 Ba2 N9 C18 -89.84(18) . . . . ? N40 Ba2 N9 C18 158.7(2) . . . . ? O42 Ba2 N9 C18 115.46(17) . . . . ? N7 Ba2 N9 C18 -15.95(19) . . . . ? Cl4 Ba2 N9 C18 96.69(17) . . . . ? C40 N9 C19 C20 -171.8(2) . . . . ? C18 N9 C19 C20 68.2(3) . . . . ? Ba2 N9 C19 C20 -54.6(2) . . . . ? N9 C19 C20 N10 55.3(3) . . . . ? C19 C20 N10 C21 155.9(3) . . . . ? C19 C20 N10 Ba2 -25.6(3) . . . . ? O31 Ba2 N10 C21 -59.6(2) . . . . ? O50 Ba2 N10 C21 -3.8(3) . . . . ? O41 Ba2 N10 C21 164.8(2) . . . . ? N8 Ba2 N10 C21 119.2(2) . . . . ? N2 Ba2 N10 C21 3.5(2) . . . . ? N40 Ba2 N10 C21 -129.5(2) . . . . ? N9 Ba2 N10 C21 177.6(2) . . . . ? O42 Ba2 N10 C21 -120.6(2) . . . . ? N7 Ba2 N10 C21 64.2(2) . . . . ? Cl4 Ba2 N10 C21 -161.87(18) . . . . ? O31 Ba2 N10 C20 122.0(2) . . . . ? O50 Ba2 N10 C20 177.84(18) . . . . ? O41 Ba2 N10 C20 -13.6(2) . . . . ? N8 Ba2 N10 C20 -59.2(2) . . . . ? N2 Ba2 N10 C20 -174.9(2) . . . . ? N40 Ba2 N10 C20 52.1(2) . . . . ? N9 Ba2 N10 C20 -0.77(19) . . . . ? O42 Ba2 N10 C20 61.0(2) . . . . ? N7 Ba2 N10 C20 -114.2(2) . . . . ? Cl4 Ba2 N10 C20 19.7(2) . . . . ? C20 N10 C21 C2 179.3(3) . . . . ? Ba2 N10 C21 C2 0.8(4) . . . . ? N2 C2 C21 N10 -9.1(4) . . . . ? C3 C2 C21 N10 169.7(3) . . . . ? C9 N4 C30 C31 63.1(3) . . . . ? C8 N4 C30 C31 -176.1(2) . . . . ? Ba1 N4 C30 C31 -55.1(3) . . . . ? N4 C30 C31 N30 35.5(4) . . . . ? N4 C30 C31 C32 -148.0(3) . . . . ? N30 C31 C32 C33 2.2(5) . . . . ? C30 C31 C32 C33 -174.2(3) . . . . ? C31 C32 C33 C34 -1.5(5) . . . . ? C32 C33 C34 C35 0.0(5) . . . . ? C33 C34 C35 N30 0.8(5) . . . . ? C32 C31 N30 C35 -1.4(4) . . . . ? C30 C31 N30 C35 175.0(3) . . . . ? C32 C31 N30 Ba1 -169.9(2) . . . . ? C30 C31 N30 Ba1 6.5(3) . . . . ? C34 C35 N30 C31 -0.2(4) . . . . ? C34 C35 N30 Ba1 167.8(2) . . . . ? O11 Ba1 N30 C31 -171.1(2) . . . . ? N3 Ba1 N30 C31 0.6(2) . . . . ? O50 Ba1 N30 C31 137.1(2) . . . . ? O21 Ba1 N30 C31 60.2(2) . . . . ? N5 Ba1 N30 C31 -81.2(2) . . . . ? O22 Ba1 N30 C31 108.1(2) . . . . ? N4 Ba1 N30 C31 -24.34(19) . . . . ? N6 Ba1 N30 C31 -127.9(2) . . . . ? N1 Ba1 N30 C31 -19.6(4) . . . . ? Cl2 Ba1 N30 C31 81.7(2) . . . . ? O11 Ba1 N30 C35 21.0(2) . . . . ? N3 Ba1 N30 C35 -167.3(2) . . . . ? O50 Ba1 N30 C35 -30.7(2) . . . . ? O21 Ba1 N30 C35 -107.7(2) . . . . ? N5 Ba1 N30 C35 111.0(2) . . . . ? O22 Ba1 N30 C35 -59.8(2) . . . . ? N4 Ba1 N30 C35 167.8(2) . . . . ? N6 Ba1 N30 C35 64.2(2) . . . . ? N1 Ba1 N30 C35 172.6(2) . . . . ? Cl2 Ba1 N30 C35 -86.2(2) . . . . ? C19 N9 C40 C41 61.4(3) . . . . ? C18 N9 C40 C41 -177.2(2) . . . . ? Ba2 N9 C40 C41 -56.3(2) . . . . ? N9 C40 C41 N40 34.8(3) . . . . ? N9 C40 C41 C42 -146.6(3) . . . . ? N40 C41 C42 C43 1.6(4) . . . . ? C40 C41 C42 C43 -176.9(3) . . . . ? C41 C42 C43 C44 -1.8(4) . . . . ? C42 C43 C44 C45 1.0(4) . . . . ? C43 C44 C45 N40 0.1(5) . . . . ? C42 C41 N40 C45 -0.5(4) . . . . ? C40 C41 N40 C45 178.0(3) . . . . ? C42 C41 N40 Ba2 -170.6(2) . . . . ? C40 C41 N40 Ba2 7.9(3) . . . . ? C44 C45 N40 C41 -0.3(4) . . . . ? C44 C45 N40 Ba2 169.5(2) . . . . ? O31 Ba2 N40 C41 -167.0(2) . . . . ? O50 Ba2 N40 C41 137.04(19) . . . . ? O41 Ba2 N40 C41 57.2(2) . . . . ? N8 Ba2 N40 C41 -0.2(2) . . . . ? N10 Ba2 N40 C41 -82.0(2) . . . . ? N2 Ba2 N40 C41 -128.13(19) . . . . ? N9 Ba2 N40 C41 -25.82(18) . . . . ? O42 Ba2 N40 C41 103.8(2) . . . . ? N7 Ba2 N40 C41 -4.9(4) . . . . ? Cl4 Ba2 N40 C41 77.50(19) . . . . ? O31 Ba2 N40 C45 23.4(2) . . . . ? O50 Ba2 N40 C45 -32.5(2) . . . . ? O41 Ba2 N40 C45 -112.4(2) . . . . ? N8 Ba2 N40 C45 -169.8(2) . . . . ? N10 Ba2 N40 C45 108.5(2) . . . . ? N2 Ba2 N40 C45 62.3(2) . . . . ? N9 Ba2 N40 C45 164.6(2) . . . . ? O42 Ba2 N40 C45 -65.7(2) . . . . ? N7 Ba2 N40 C45 -174.5(2) . . . . ? Cl4 Ba2 N40 C45 -92.1(2) . . . . ? O31 Ba2 O50 Ba1 97.51(11) . . . . ? O41 Ba2 O50 Ba1 -134.01(11) . . . . ? N8 Ba2 O50 Ba1 -73.23(12) . . . . ? N10 Ba2 O50 Ba1 37.99(16) . . . . ? N2 Ba2 O50 Ba1 31.79(10) . . . . ? N40 Ba2 O50 Ba1 152.00(9) . . . . ? N9 Ba2 O50 Ba1 -146.36(19) . . . . ? O42 Ba2 O50 Ba1 -176.16(13) . . . . ? N7 Ba2 O50 Ba1 -37.02(10) . . . . ? Cl4 Ba2 O50 Ba1 -155.09(11) . . . . ? O11 Ba1 O50 Ba2 96.31(11) . . . . ? N3 Ba1 O50 Ba2 -75.91(12) . . . . ? O21 Ba1 O50 Ba2 -139.49(11) . . . . ? N5 Ba1 O50 Ba2 30.01(16) . . . . ? N30 Ba1 O50 Ba2 148.05(9) . . . . ? O22 Ba1 O50 Ba2 176.43(13) . . . . ? N4 Ba1 O50 Ba2 -134.6(2) . . . . ? N6 Ba1 O50 Ba2 30.01(10) . . . . ? N1 Ba1 O50 Ba2 -37.73(9) . . . . ? Cl2 Ba1 O50 Ba2 -161.19(11) . . . . ? O12 Cl1 O11 Ba1 -111.5(2) . . . . ? O13 Cl1 O11 Ba1 10.3(3) . . . . ? O14 Cl1 O11 Ba1 129.0(2) . . . . ? N3 Ba1 O11 Cl1 129.0(4) . . . . ? O50 Ba1 O11 Cl1 11.3(2) . . . . ? O21 Ba1 O11 Cl1 -61.4(2) . . . . ? N5 Ba1 O11 Cl1 151.4(2) . . . . ? N30 Ba1 O11 Cl1 -123.2(2) . . . . ? O22 Ba1 O11 Cl1 -57.3(2) . . . . ? N4 Ba1 O11 Cl1 -154.8(2) . . . . ? N6 Ba1 O11 Cl1 98.2(2) . . . . ? N1 Ba1 O11 Cl1 64.6(2) . . . . ? Cl2 Ba1 O11 Cl1 -61.6(2) . . . . ? O11 Ba1 Cl2 O24 -87.40(12) . . . . ? N3 Ba1 Cl2 O24 91.10(12) . . . . ? O50 Ba1 Cl2 O24 -155.61(13) . . . . ? O21 Ba1 Cl2 O24 93.16(16) . . . . ? N5 Ba1 Cl2 O24 10.09(15) . . . . ? N30 Ba1 Cl2 O24 -22.22(12) . . . . ? O22 Ba1 Cl2 O24 -97.67(15) . . . . ? N4 Ba1 Cl2 O24 31.40(12) . . . . ? N6 Ba1 Cl2 O24 -130.73(15) . . . . ? N1 Ba1 Cl2 O24 142.47(12) . . . . ? O11 Ba1 Cl2 O23 98.28(14) . . . . ? N3 Ba1 Cl2 O23 -83.22(14) . . . . ? O50 Ba1 Cl2 O23 30.06(14) . . . . ? O21 Ba1 Cl2 O23 -81.16(17) . . . . ? N5 Ba1 Cl2 O23 -164.23(15) . . . . ? N30 Ba1 Cl2 O23 163.46(14) . . . . ? O22 Ba1 Cl2 O23 88.00(17) . . . . ? N4 Ba1 Cl2 O23 -142.93(14) . . . . ? N6 Ba1 Cl2 O23 54.94(17) . . . . ? N1 Ba1 Cl2 O23 -31.85(14) . . . . ? O11 Ba1 Cl2 O22 10.28(11) . . . . ? N3 Ba1 Cl2 O22 -171.22(11) . . . . ? O50 Ba1 Cl2 O22 -57.94(12) . . . . ? O21 Ba1 Cl2 O22 -169.16(16) . . . . ? N5 Ba1 Cl2 O22 107.77(13) . . . . ? N30 Ba1 Cl2 O22 75.46(12) . . . . ? N4 Ba1 Cl2 O22 129.07(11) . . . . ? N6 Ba1 Cl2 O22 -33.06(15) . . . . ? N1 Ba1 Cl2 O22 -119.85(11) . . . . ? O11 Ba1 Cl2 O21 179.44(12) . . . . ? N3 Ba1 Cl2 O21 -2.06(12) . . . . ? O50 Ba1 Cl2 O21 111.22(13) . . . . ? N5 Ba1 Cl2 O21 -83.07(14) . . . . ? N30 Ba1 Cl2 O21 -115.38(13) . . . . ? O22 Ba1 Cl2 O21 169.16(16) . . . . ? N4 Ba1 Cl2 O21 -61.77(12) . . . . ? N6 Ba1 Cl2 O21 136.10(15) . . . . ? N1 Ba1 Cl2 O21 49.31(12) . . . . ? O24 Cl2 O21 Ba1 -110.20(13) . . . . ? O23 Cl2 O21 Ba1 129.35(12) . . . . ? O22 Cl2 O21 Ba1 9.59(14) . . . . ? O11 Ba1 O21 Cl2 -0.65(14) . . . . ? N3 Ba1 O21 Cl2 177.77(13) . . . . ? O50 Ba1 O21 Cl2 -65.32(11) . . . . ? N5 Ba1 O21 Cl2 125.63(11) . . . . ? N30 Ba1 O21 Cl2 57.78(11) . . . . ? O22 Ba1 O21 Cl2 -5.99(9) . . . . ? N4 Ba1 O21 Cl2 116.03(12) . . . . ? N6 Ba1 O21 Cl2 -99.5(2) . . . . ? N1 Ba1 O21 Cl2 -136.21(11) . . . . ? O24 Cl2 O22 Ba1 110.34(11) . . . . ? O23 Cl2 O22 Ba1 -128.56(11) . . . . ? O21 Cl2 O22 Ba1 -8.78(13) . . . . ? O11 Ba1 O22 Cl2 -169.35(12) . . . . ? N3 Ba1 O22 Cl2 9.67(13) . . . . ? O50 Ba1 O22 Cl2 114.51(12) . . . . ? O21 Ba1 O22 Cl2 5.83(9) . . . . ? N5 Ba1 O22 Cl2 -109.58(13) . . . . ? N30 Ba1 O22 Cl2 -92.89(11) . . . . ? N4 Ba1 O22 Cl2 -53.23(11) . . . . ? N6 Ba1 O22 Cl2 160.79(9) . . . . ? N1 Ba1 O22 Cl2 73.48(12) . . . . ? O32 Cl3 O31 Ba2 -110.4(2) . . . . ? O34 Cl3 O31 Ba2 126.5(2) . . . . ? O33 Cl3 O31 Ba2 9.2(3) . . . . ? O50 Ba2 O31 Cl3 9.3(2) . . . . ? O41 Ba2 O31 Cl3 -64.1(2) . . . . ? N8 Ba2 O31 Cl3 146.9(3) . . . . ? N10 Ba2 O31 Cl3 152.8(2) . . . . ? N2 Ba2 O31 Cl3 96.1(2) . . . . ? N40 Ba2 O31 Cl3 -120.5(2) . . . . ? N9 Ba2 O31 Cl3 -154.9(2) . . . . ? O42 Ba2 O31 Cl3 -57.8(2) . . . . ? N7 Ba2 O31 Cl3 64.7(2) . . . . ? Cl4 Ba2 O31 Cl3 -63.7(2) . . . . ? O31 Ba2 Cl4 O44 104.06(15) . . . . ? O50 Ba2 Cl4 O44 35.29(15) . . . . ? O41 Ba2 Cl4 O44 -76.85(18) . . . . ? N8 Ba2 Cl4 O44 -82.19(15) . . . . ? N10 Ba2 Cl4 O44 -159.85(16) . . . . ? N2 Ba2 Cl4 O44 52.57(19) . . . . ? N40 Ba2 Cl4 O44 164.10(15) . . . . ? N9 Ba2 Cl4 O44 -142.30(15) . . . . ? O42 Ba2 Cl4 O44 89.49(18) . . . . ? N7 Ba2 Cl4 O44 -31.07(15) . . . . ? O31 Ba2 Cl4 O43 -85.37(12) . . . . ? O50 Ba2 Cl4 O43 -154.13(13) . . . . ? O41 Ba2 Cl4 O43 93.73(16) . . . . ? N8 Ba2 Cl4 O43 88.39(12) . . . . ? N10 Ba2 Cl4 O43 10.72(14) . . . . ? N2 Ba2 Cl4 O43 -136.86(16) . . . . ? N40 Ba2 Cl4 O43 -25.33(12) . . . . ? N9 Ba2 Cl4 O43 28.28(12) . . . . ? O42 Ba2 Cl4 O43 -99.94(16) . . . . ? N7 Ba2 Cl4 O43 139.50(12) . . . . ? O31 Ba2 Cl4 O42 14.57(12) . . . . ? O50 Ba2 Cl4 O42 -54.19(12) . . . . ? O41 Ba2 Cl4 O42 -166.33(16) . . . . ? N8 Ba2 Cl4 O42 -171.67(12) . . . . ? N10 Ba2 Cl4 O42 110.66(13) . . . . ? N2 Ba2 Cl4 O42 -36.92(16) . . . . ? N40 Ba2 Cl4 O42 74.61(12) . . . . ? N9 Ba2 Cl4 O42 128.21(12) . . . . ? N7 Ba2 Cl4 O42 -120.56(12) . . . . ? O31 Ba2 Cl4 O41 -179.10(12) . . . . ? O50 Ba2 Cl4 O41 112.14(13) . . . . ? N8 Ba2 Cl4 O41 -5.34(12) . . . . ? N10 Ba2 Cl4 O41 -83.01(14) . . . . ? N2 Ba2 Cl4 O41 129.41(16) . . . . ? N40 Ba2 Cl4 O41 -119.06(13) . . . . ? N9 Ba2 Cl4 O41 -65.45(12) . . . . ? O42 Ba2 Cl4 O41 166.33(16) . . . . ? N7 Ba2 Cl4 O41 45.78(12) . . . . ? O44 Cl4 O41 Ba2 132.63(12) . . . . ? O43 Cl4 O41 Ba2 -107.30(13) . . . . ? O42 Cl4 O41 Ba2 12.33(15) . . . . ? O31 Ba2 O41 Cl4 1.08(15) . . . . ? O50 Ba2 O41 Cl4 -65.12(12) . . . . ? N8 Ba2 O41 Cl4 174.13(14) . . . . ? N10 Ba2 O41 Cl4 122.71(11) . . . . ? N2 Ba2 O41 Cl4 -112.02(18) . . . . ? N40 Ba2 O41 Cl4 54.23(11) . . . . ? N9 Ba2 O41 Cl4 111.40(12) . . . . ? O42 Ba2 O41 Cl4 -7.57(9) . . . . ? N7 Ba2 O41 Cl4 -138.27(11) . . . . ? O44 Cl4 O42 Ba2 -130.52(11) . . . . ? O43 Cl4 O42 Ba2 107.66(12) . . . . ? O41 Cl4 O42 Ba2 -10.84(13) . . . . ? O31 Ba2 O42 Cl4 -165.54(12) . . . . ? O50 Ba2 O42 Cl4 119.04(12) . . . . ? O41 Ba2 O42 Cl4 7.29(9) . . . . ? N8 Ba2 O42 Cl4 8.96(13) . . . . ? N10 Ba2 O42 Cl4 -103.35(13) . . . . ? N2 Ba2 O42 Cl4 160.14(9) . . . . ? N40 Ba2 O42 Cl4 -93.21(12) . . . . ? N9 Ba2 O42 Cl4 -52.93(11) . . . . ? N7 Ba2 O42 Cl4 70.87(12) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.365 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.085 data_mw38a _database_code_depnum_ccdc_archive 'CCDC 269195' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H42 Cl4 Cu2 N14 O16' _chemical_formula_weight 1195.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3739(1) _cell_length_b 14.3390(3) _cell_length_c 16.5674(2) _cell_angle_alpha 99.648(1) _cell_angle_beta 101.602(1) _cell_angle_gamma 112.359(1) _cell_volume 2357.25(6) _cell_formula_units_Z 2 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue-purple _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 1.214 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 83(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 SMART area detector' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22850 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.42 _reflns_number_total 9556 _reflns_number_gt 7452 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. All non-H ANIS. All H's calc and ride. Two of the four ClO4 anions disordered. One, Cl3, is twirling about the Cl3-O31 bond (0.59:0.41) and is restrained by EADP and SAME. The other, Cl4, has two complete sets of O's (0.68:0.32). Two reflections, 0 0 1 and 0 1 0, omitted as obscured by beamstop. ; _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^)+(0.0510P)^2^+3.9005P] 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 9556 _refine_ls_number_parameters 696 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.048 _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 Cu1 Cu 0.30236(4) 0.80966(3) 0.14411(3) 0.01864(11) Uani 1 1 d . . . Cu2 Cu 0.42148(4) 1.25107(3) 0.30240(3) 0.02009(11) Uani 1 1 d . . . N1 N 0.1996(3) 0.8977(2) 0.15089(18) 0.0193(6) Uani 1 1 d . . . N2 N 0.2379(3) 0.9932(2) 0.14000(19) 0.0215(6) Uani 1 1 d . . . C2 C 0.1542(4) 1.0379(3) 0.1389(2) 0.0226(8) Uani 1 1 d . . . C3 C 0.0298(4) 0.9907(3) 0.1527(3) 0.0297(9) Uani 1 1 d . . . H3 H -0.0261 1.0258 0.1539 0.036 Uiso 1 1 calc R . . C4 C -0.0083(4) 0.8921(3) 0.1643(3) 0.0308(9) Uani 1 1 d . . . H4 H -0.0911 0.8567 0.1745 0.037 Uiso 1 1 calc R . . C5 C 0.0787(4) 0.8457(3) 0.1606(2) 0.0239(8) Uani 1 1 d . . . C6 C 0.0487(4) 0.7363(3) 0.1619(2) 0.0267(8) Uani 1 1 d . . . H6 H -0.0333 0.6904 0.1677 0.032 Uiso 1 1 calc R . . N3 N 0.1392(3) 0.7076(2) 0.15479(19) 0.0232(7) Uani 1 1 d . . . C7 C 0.1295(4) 0.6015(3) 0.1460(3) 0.0303(9) Uani 1 1 d . . . H7A H 0.0359 0.5492 0.1206 0.036 Uiso 1 1 calc R . . H7B H 0.1640 0.5925 0.2025 0.036 Uiso 1 1 calc R . . C8 C 0.2131(4) 0.5882(3) 0.0874(3) 0.0302(9) Uani 1 1 d . . . H8A H 0.2281 0.5250 0.0900 0.036 Uiso 1 1 calc R . . H8B H 0.1657 0.5794 0.0276 0.036 Uiso 1 1 calc R . . N4 N 0.3436(3) 0.6831(2) 0.11566(19) 0.0224(7) Uani 1 1 d . . . C30 C 0.4089(4) 0.6988(3) 0.0459(2) 0.0236(8) Uani 1 1 d . . . H30A H 0.3403 0.6710 -0.0102 0.028 Uiso 1 1 calc R . . H30B H 0.4651 0.6604 0.0456 0.028 Uiso 1 1 calc R . . C31 C 0.4933(4) 0.8140(3) 0.0603(2) 0.0200(7) Uani 1 1 d . . . C32 C 0.6103(4) 0.8527(3) 0.0376(2) 0.0237(8) Uani 1 1 d . . . H32 H 0.6427 0.8062 0.0131 0.028 Uiso 1 1 calc R . . C33 C 0.6789(4) 0.9594(3) 0.0508(2) 0.0259(8) Uani 1 1 d . . . H33 H 0.7583 0.9867 0.0349 0.031 Uiso 1 1 calc R . . C34 C 0.6311(4) 1.0264(3) 0.0876(2) 0.0228(8) Uani 1 1 d . . . H34 H 0.6771 1.1000 0.0972 0.027 Uiso 1 1 calc R . . C35 C 0.5158(4) 0.9840(3) 0.1099(2) 0.0231(8) Uani 1 1 d . . . H35 H 0.4836 1.0296 0.1363 0.028 Uiso 1 1 calc R . . N30 N 0.4469(3) 0.8799(2) 0.09566(18) 0.0188(6) Uani 1 1 d . . . C9 C 0.4339(4) 0.6819(3) 0.1942(2) 0.0272(9) Uani 1 1 d . . . H9A H 0.4849 0.6435 0.1770 0.033 Uiso 1 1 calc R . . H9B H 0.3794 0.6435 0.2279 0.033 Uiso 1 1 calc R . . C10 C 0.5299(4) 0.7900(3) 0.2504(2) 0.0262(8) Uani 1 1 d . . . H10A H 0.5785 0.7848 0.3049 0.031 Uiso 1 1 calc R . . H10B H 0.5955 0.8249 0.2213 0.031 Uiso 1 1 calc R . . N5 N 0.4551(3) 0.8514(3) 0.26748(19) 0.0247(7) Uani 1 1 d . . . C11 C 0.4852(4) 0.9082(3) 0.3417(2) 0.0284(9) Uani 1 1 d . . . H11 H 0.5530 0.9091 0.3864 0.034 Uiso 1 1 calc R . . N6 N 0.4399(3) 1.0534(2) 0.32279(19) 0.0250(7) Uani 1 1 d . . . N7 N 0.3807(3) 1.1159(2) 0.33646(18) 0.0220(6) Uani 1 1 d . . . C12 C 0.4143(4) 0.9738(3) 0.3594(2) 0.0252(8) Uani 1 1 d . . . C13 C 0.3277(4) 0.9537(3) 0.4103(2) 0.0273(8) Uani 1 1 d . . . H13 H 0.3146 0.8984 0.4371 0.033 Uiso 1 1 calc R . . C14 C 0.2626(4) 1.0156(3) 0.4204(2) 0.0270(8) Uani 1 1 d . . . H14 H 0.1991 1.0027 0.4516 0.032 Uiso 1 1 calc R . . C15 C 0.2934(4) 1.0984(3) 0.3830(2) 0.0225(8) Uani 1 1 d . . . C16 C 0.2400(4) 1.1774(3) 0.3920(2) 0.0251(8) Uani 1 1 d . . . H16 H 0.1793 1.1757 0.4243 0.030 Uiso 1 1 calc R . . N8 N 0.2804(3) 1.2476(2) 0.35397(19) 0.0242(7) Uani 1 1 d . . . C17 C 0.2510(4) 1.3388(3) 0.3591(3) 0.0297(9) Uani 1 1 d . . . H17A H 0.2212 1.3524 0.4102 0.036 Uiso 1 1 calc R . . H17B H 0.1802 1.3274 0.3075 0.036 Uiso 1 1 calc R . . C18 C 0.3805(4) 1.4308(3) 0.3651(2) 0.0273(8) Uani 1 1 d . . . H18A H 0.3623 1.4907 0.3549 0.033 Uiso 1 1 calc R . . H18B H 0.4428 1.4532 0.4232 0.033 Uiso 1 1 calc R . . N9 N 0.4422(3) 1.3990(2) 0.30005(19) 0.0217(6) Uani 1 1 d . . . C40 C 0.5872(4) 1.4653(3) 0.3226(3) 0.0272(8) Uani 1 1 d . . . H40A H 0.6226 1.4968 0.3852 0.033 Uiso 1 1 calc R . . H40B H 0.6028 1.5229 0.2945 0.033 Uiso 1 1 calc R . . C41 C 0.6604(4) 1.4029(3) 0.2952(2) 0.0263(8) Uani 1 1 d . . . C42 C 0.7819(4) 1.4483(3) 0.2801(3) 0.0320(9) Uani 1 1 d . . . H42 H 0.8196 1.5205 0.2820 0.038 Uiso 1 1 calc R . . C43 C 0.8481(4) 1.3878(3) 0.2622(3) 0.0348(10) Uani 1 1 d . . . H43 H 0.9316 1.4179 0.2513 0.042 Uiso 1 1 calc R . . C44 C 0.7913(4) 1.2822(3) 0.2602(3) 0.0316(9) Uani 1 1 d . . . H44 H 0.8358 1.2395 0.2491 0.038 Uiso 1 1 calc R . . C45 C 0.6691(4) 1.2413(3) 0.2745(2) 0.0269(8) Uani 1 1 d . . . H45 H 0.6295 1.1691 0.2725 0.032 Uiso 1 1 calc R . . N40 N 0.6033(3) 1.2998(2) 0.29139(18) 0.0221(6) Uani 1 1 d . . . C19 C 0.3693(4) 1.3971(3) 0.2131(2) 0.0246(8) Uani 1 1 d . . . H19A H 0.4122 1.4666 0.2028 0.029 Uiso 1 1 calc R . . H19B H 0.2768 1.3838 0.2117 0.029 Uiso 1 1 calc R . . C20 C 0.3675(4) 1.3135(3) 0.1420(2) 0.0254(8) Uani 1 1 d . . . H20A H 0.3088 1.3083 0.0868 0.030 Uiso 1 1 calc R . . H20B H 0.4582 1.3323 0.1364 0.030 Uiso 1 1 calc R . . N10 N 0.3181(3) 1.2126(2) 0.16358(19) 0.0237(7) Uani 1 1 d . . . C21 C 0.2037(4) 1.1418(3) 0.1195(2) 0.0255(8) Uani 1 1 d . . . H21 H 0.1504 1.1548 0.0747 0.031 Uiso 1 1 calc R . . Cl1 Cl 0.56594(9) 1.29664(7) 0.54667(5) 0.02302(19) Uani 1 1 d . . . O11 O 0.5832(3) 1.3608(2) 0.48772(17) 0.0309(6) Uani 1 1 d D . . O12 O 0.5726(3) 1.2006(2) 0.51072(17) 0.0287(6) Uani 1 1 d D . . O13 O 0.4375(3) 1.2725(2) 0.56128(18) 0.0371(7) Uani 1 1 d D . . O14 O 0.6692(3) 1.3513(2) 0.62689(16) 0.0303(6) Uani 1 1 d D . . Cl2 Cl 0.68651(9) 0.58655(7) 0.11555(5) 0.02241(19) Uani 1 1 d . . . O21 O 0.7383(3) 0.6460(2) 0.20431(19) 0.0450(8) Uani 1 1 d . . . O22 O 0.5510(3) 0.5134(2) 0.09924(19) 0.0341(7) Uani 1 1 d . . . O23 O 0.6953(3) 0.6590(2) 0.0644(2) 0.0443(8) Uani 1 1 d . . . O24 O 0.7655(3) 0.5316(2) 0.0991(2) 0.0416(8) Uani 1 1 d . . . Cl3 Cl 1.02939(9) 0.73411(7) -0.07933(6) 0.0265(2) Uani 1 1 d . . . O31 O 1.1545(3) 0.7340(3) -0.0447(2) 0.0606(10) Uani 1 1 d D A . O32 O 1.0409(6) 0.8081(5) -0.1283(5) 0.0577(16) Uani 0.59 1 d PD A 1 O33 O 0.9549(6) 0.6329(4) -0.1414(5) 0.0590(14) Uani 0.59 1 d PD A 1 O34 O 0.9576(7) 0.7437(7) -0.0213(4) 0.0610(17) Uani 0.59 1 d PD A 1 O35 O 1.0634(8) 0.8461(6) -0.0472(7) 0.0590(14) Uani 0.41 1 d PD A 2 O36 O 0.9708(9) 0.6988(10) -0.1662(5) 0.0610(17) Uani 0.41 1 d PD A 2 O37 O 0.9343(10) 0.6834(7) -0.0369(8) 0.0577(16) Uani 0.41 1 d PD A 2 Cl4 Cl 0.87645(10) 0.05427(8) 0.34775(7) 0.0362(2) Uani 1 1 d . . . O41 O 0.7888(7) 0.0254(6) 0.2670(4) 0.086(3) Uani 0.68 1 d P B 1 O42 O 0.9533(5) 0.1647(4) 0.3779(4) 0.0498(14) Uani 0.68 1 d P B 1 O43 O 0.8072(6) 0.0177(5) 0.4069(3) 0.0657(16) Uani 0.68 1 d P B 1 O44 O 0.9687(6) 0.0066(4) 0.3435(4) 0.0633(16) Uani 0.68 1 d P B 1 O45 O 0.9558(12) 0.1443(10) 0.3165(11) 0.064(4) Uani 0.32 1 d P B 2 O46 O 0.8228(12) -0.0364(9) 0.2764(7) 0.050(3) Uani 0.32 1 d P B 2 O47 O 0.7549(13) 0.0635(11) 0.3573(15) 0.105(7) Uani 0.32 1 d P B 2 O48 O 0.9490(13) 0.0451(10) 0.4211(8) 0.078(4) Uani 0.32 1 d P B 2 N50 N 0.8765(4) 0.5865(3) 0.4847(2) 0.0444(10) Uani 1 1 d . . . C50 C 0.9892(4) 0.6211(3) 0.4948(3) 0.0336(9) Uani 1 1 d . . . C51 C 1.1309(4) 0.6649(4) 0.5053(3) 0.0411(11) Uani 1 1 d . . . H51A H 1.1464 0.6635 0.4491 0.049 Uiso 1 1 calc R . . H51B H 1.1691 0.6233 0.5329 0.049 Uiso 1 1 calc R . . H51C H 1.1730 0.7373 0.5410 0.049 Uiso 1 1 calc R . . N60 N 1.0470(4) 0.7640(3) 0.3412(3) 0.0494(10) Uani 1 1 d . . . C60 C 0.9636(4) 0.7741(3) 0.3648(3) 0.0358(10) Uani 1 1 d . . . C61 C 0.8587(5) 0.7871(4) 0.3957(3) 0.0424(11) Uani 1 1 d . . . H61A H 0.8216 0.7322 0.4236 0.051 Uiso 1 1 calc R . . H61B H 0.7886 0.7821 0.3474 0.051 Uiso 1 1 calc R . . H61C H 0.8951 0.8559 0.4369 0.051 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 Cu1 0.0195(2) 0.0188(2) 0.0199(2) 0.00777(18) 0.00846(18) 0.00820(18) Cu2 0.0296(3) 0.0205(2) 0.0178(2) 0.00808(18) 0.01113(19) 0.0154(2) N1 0.0187(15) 0.0190(15) 0.0194(15) 0.0068(12) 0.0061(12) 0.0063(13) N2 0.0215(16) 0.0230(16) 0.0214(15) 0.0077(13) 0.0059(13) 0.0105(13) C2 0.0204(18) 0.0245(19) 0.0192(18) 0.0028(15) 0.0000(15) 0.0098(16) C3 0.0207(19) 0.034(2) 0.036(2) 0.0061(18) 0.0057(17) 0.0154(18) C4 0.021(2) 0.036(2) 0.037(2) 0.0115(19) 0.0116(18) 0.0124(18) C5 0.0177(18) 0.027(2) 0.0253(19) 0.0069(16) 0.0082(16) 0.0068(16) C6 0.0219(19) 0.029(2) 0.029(2) 0.0128(17) 0.0098(17) 0.0079(17) N3 0.0252(16) 0.0230(16) 0.0211(16) 0.0089(13) 0.0099(13) 0.0074(14) C7 0.038(2) 0.022(2) 0.038(2) 0.0132(17) 0.023(2) 0.0117(18) C8 0.038(2) 0.0180(19) 0.035(2) 0.0062(17) 0.0177(19) 0.0087(17) N4 0.0278(17) 0.0232(16) 0.0207(16) 0.0094(13) 0.0130(14) 0.0113(14) C30 0.028(2) 0.0230(19) 0.0214(19) 0.0052(15) 0.0132(16) 0.0095(16) C31 0.0230(18) 0.0236(19) 0.0118(16) 0.0050(14) 0.0036(14) 0.0091(16) C32 0.029(2) 0.028(2) 0.0174(18) 0.0069(15) 0.0099(16) 0.0129(17) C33 0.0209(19) 0.032(2) 0.0218(19) 0.0090(16) 0.0085(16) 0.0068(17) C34 0.0219(18) 0.0220(19) 0.0217(18) 0.0107(15) 0.0042(15) 0.0055(16) C35 0.0227(19) 0.0238(19) 0.0238(19) 0.0080(16) 0.0057(16) 0.0108(16) N30 0.0197(15) 0.0211(15) 0.0156(14) 0.0066(12) 0.0041(12) 0.0084(13) C9 0.037(2) 0.036(2) 0.028(2) 0.0208(18) 0.0201(18) 0.0257(19) C10 0.028(2) 0.039(2) 0.025(2) 0.0148(17) 0.0127(17) 0.0242(19) N5 0.0246(16) 0.0319(18) 0.0196(16) 0.0047(14) 0.0069(13) 0.0149(15) C11 0.034(2) 0.0201(19) 0.026(2) 0.0038(16) -0.0004(17) 0.0114(17) N6 0.0365(19) 0.0267(17) 0.0164(15) 0.0058(13) 0.0059(14) 0.0193(15) N7 0.0307(17) 0.0226(16) 0.0149(15) 0.0046(12) 0.0055(13) 0.0147(14) C12 0.032(2) 0.0170(18) 0.0169(18) -0.0006(15) -0.0075(16) 0.0105(16) C13 0.028(2) 0.023(2) 0.025(2) 0.0104(16) 0.0005(17) 0.0071(17) C14 0.026(2) 0.028(2) 0.025(2) 0.0102(16) 0.0059(17) 0.0077(17) C15 0.0261(19) 0.025(2) 0.0156(17) 0.0060(15) 0.0037(15) 0.0116(16) C16 0.029(2) 0.033(2) 0.0181(18) 0.0079(16) 0.0086(16) 0.0164(18) N8 0.0317(18) 0.0253(17) 0.0226(16) 0.0088(13) 0.0099(14) 0.0173(15) C17 0.046(3) 0.035(2) 0.025(2) 0.0130(17) 0.0179(19) 0.030(2) C18 0.042(2) 0.025(2) 0.0237(19) 0.0046(16) 0.0117(18) 0.0241(19) N9 0.0307(17) 0.0204(16) 0.0184(15) 0.0062(12) 0.0080(13) 0.0147(14) C40 0.031(2) 0.0198(19) 0.028(2) 0.0057(16) 0.0052(17) 0.0100(17) C41 0.032(2) 0.028(2) 0.0191(18) 0.0059(16) 0.0054(16) 0.0131(18) C42 0.034(2) 0.030(2) 0.029(2) 0.0102(18) 0.0089(18) 0.0094(19) C43 0.033(2) 0.045(3) 0.028(2) 0.0124(19) 0.0147(19) 0.014(2) C44 0.031(2) 0.043(2) 0.026(2) 0.0073(18) 0.0115(18) 0.021(2) C45 0.034(2) 0.029(2) 0.0210(19) 0.0055(16) 0.0073(17) 0.0183(18) N40 0.0269(17) 0.0239(16) 0.0156(15) 0.0053(12) 0.0050(13) 0.0117(14) C19 0.031(2) 0.025(2) 0.0233(19) 0.0110(16) 0.0079(17) 0.0154(17) C20 0.036(2) 0.025(2) 0.0201(19) 0.0102(16) 0.0097(17) 0.0147(17) N10 0.0330(18) 0.0247(17) 0.0168(15) 0.0082(13) 0.0111(14) 0.0132(15) C21 0.028(2) 0.027(2) 0.0243(19) 0.0090(16) 0.0050(17) 0.0160(18) Cl1 0.0312(5) 0.0252(5) 0.0187(4) 0.0088(4) 0.0095(4) 0.0160(4) O11 0.0473(18) 0.0338(16) 0.0261(14) 0.0183(12) 0.0173(13) 0.0248(14) O12 0.0354(16) 0.0216(14) 0.0289(15) 0.0044(11) 0.0074(12) 0.0140(12) O13 0.0339(16) 0.057(2) 0.0312(16) 0.0173(14) 0.0178(13) 0.0248(15) O14 0.0376(16) 0.0324(15) 0.0204(14) 0.0057(12) 0.0034(12) 0.0176(13) Cl2 0.0228(4) 0.0192(4) 0.0217(4) 0.0045(3) 0.0057(4) 0.0062(4) O21 0.051(2) 0.0429(19) 0.0267(16) -0.0066(14) -0.0022(15) 0.0178(16) O22 0.0273(15) 0.0290(15) 0.0401(17) 0.0086(13) 0.0155(13) 0.0034(12) O23 0.0426(18) 0.0418(18) 0.051(2) 0.0302(16) 0.0153(16) 0.0127(15) O24 0.0364(17) 0.0295(16) 0.060(2) 0.0036(15) 0.0197(16) 0.0157(14) Cl3 0.0219(4) 0.0330(5) 0.0254(5) 0.0119(4) 0.0081(4) 0.0102(4) O31 0.044(2) 0.110(3) 0.046(2) 0.029(2) 0.0123(17) 0.050(2) O32 0.062(3) 0.057(3) 0.086(4) 0.051(3) 0.048(3) 0.032(3) O33 0.035(3) 0.028(2) 0.099(4) 0.004(3) 0.010(3) 0.008(2) O34 0.057(3) 0.140(6) 0.020(2) 0.030(3) 0.021(2) 0.070(4) O35 0.035(3) 0.028(2) 0.099(4) 0.004(3) 0.010(3) 0.008(2) O36 0.057(3) 0.140(6) 0.020(2) 0.030(3) 0.021(2) 0.070(4) O37 0.062(3) 0.057(3) 0.086(4) 0.051(3) 0.048(3) 0.032(3) Cl4 0.0349(6) 0.0291(5) 0.0376(6) 0.0083(4) 0.0023(5) 0.0107(4) O41 0.076(5) 0.070(5) 0.043(3) 0.026(3) -0.026(3) -0.021(4) O42 0.034(3) 0.026(3) 0.077(4) 0.001(3) 0.003(3) 0.013(2) O43 0.065(4) 0.106(5) 0.043(3) 0.030(3) 0.037(3) 0.039(4) O44 0.069(4) 0.037(3) 0.106(5) 0.022(3) 0.054(4) 0.030(3) O45 0.033(6) 0.052(8) 0.096(11) 0.023(8) 0.000(8) 0.016(6) O46 0.059(7) 0.039(6) 0.036(6) 0.003(5) 0.020(6) 0.004(6) O47 0.053(8) 0.059(9) 0.23(2) 0.045(11) 0.061(11) 0.038(7) O48 0.058(8) 0.058(8) 0.064(8) 0.020(7) -0.039(7) -0.004(6) N50 0.038(2) 0.053(3) 0.036(2) 0.0036(18) 0.0147(18) 0.015(2) C50 0.037(3) 0.041(2) 0.024(2) 0.0084(18) 0.0118(19) 0.016(2) C51 0.032(2) 0.058(3) 0.035(2) 0.016(2) 0.011(2) 0.021(2) N60 0.033(2) 0.060(3) 0.043(2) 0.014(2) 0.0115(19) 0.008(2) C60 0.032(2) 0.036(2) 0.026(2) 0.0079(18) 0.0031(19) 0.0041(19) C61 0.049(3) 0.044(3) 0.039(3) 0.011(2) 0.015(2) 0.023(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 Cu1 N3 1.942(3) . y Cu1 N30 1.976(3) . y Cu1 N1 2.025(3) . y Cu1 N4 2.045(3) . y Cu1 N5 2.219(3) . y Cu2 N8 1.953(3) . y Cu2 N40 1.973(3) . y Cu2 N7 2.019(3) . y Cu2 N9 2.051(3) . y Cu2 N10 2.229(3) . y N1 N2 1.326(4) . ? N1 C5 1.350(4) . ? N2 C2 1.333(4) . ? C2 C3 1.401(5) . ? C2 C21 1.495(5) . ? C3 C4 1.373(6) . ? C4 C5 1.391(5) . ? C5 C6 1.479(5) . ? C6 N3 1.264(5) . ? N3 C7 1.462(5) . ? C7 C8 1.527(5) . ? C8 N4 1.498(5) . ? N4 C9 1.494(5) . ? N4 C30 1.497(4) . ? C30 C31 1.508(5) . ? C31 N30 1.354(4) . ? C31 C32 1.390(5) . ? C32 C33 1.381(5) . ? C33 C34 1.387(5) . ? C34 C35 1.375(5) . ? C35 N30 1.348(5) . ? C9 C10 1.510(6) . ? C10 N5 1.471(4) . ? N5 C11 1.256(5) . ? C11 C12 1.484(5) . ? N6 N7 1.328(4) . ? N6 C12 1.344(5) . ? N7 C15 1.351(5) . ? C12 C13 1.401(6) . ? C13 C14 1.366(5) . ? C14 C15 1.391(5) . ? C15 C16 1.476(5) . ? C16 N8 1.265(5) . ? N8 C17 1.461(5) . ? C17 C18 1.529(6) . ? C18 N9 1.498(4) . ? N9 C40 1.484(5) . ? N9 C19 1.501(5) . ? C40 C41 1.510(5) . ? C41 N40 1.355(5) . ? C41 C42 1.380(5) . ? C42 C43 1.382(6) . ? C43 C44 1.393(6) . ? C44 C45 1.375(5) . ? C45 N40 1.351(5) . ? C19 C20 1.524(5) . ? C20 N10 1.474(5) . ? N10 C21 1.274(5) . ? Cl1 O11 1.442(3) . ? Cl1 O12 1.442(3) . ? Cl1 O14 1.443(3) . ? Cl1 O13 1.448(3) . ? Cl2 O22 1.434(3) . ? Cl2 O23 1.435(3) . ? Cl2 O24 1.438(3) . ? Cl2 O21 1.444(3) . ? Cl3 O36 1.373(7) . ? Cl3 O34 1.403(5) . ? Cl3 O32 1.423(5) . ? Cl3 O31 1.424(3) . ? Cl3 O37 1.439(9) . ? Cl3 O33 1.447(6) . ? Cl3 O35 1.473(8) . ? Cl4 O48 1.382(11) . ? Cl4 O41 1.386(5) . ? Cl4 O43 1.423(5) . ? Cl4 O42 1.424(5) . ? Cl4 O46 1.432(10) . ? Cl4 O44 1.460(5) . ? Cl4 O47 1.475(12) . ? Cl4 O45 1.508(13) . ? N50 C50 1.148(5) . ? C50 C51 1.451(6) . ? N60 C60 1.144(6) . ? C60 C61 1.450(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N30 160.92(12) . . y N3 Cu1 N1 80.42(12) . . y N30 Cu1 N1 106.81(11) . . y N3 Cu1 N4 83.82(12) . . y N30 Cu1 N4 85.10(12) . . y N1 Cu1 N4 160.79(12) . . y N3 Cu1 N5 105.67(12) . . y N30 Cu1 N5 88.45(12) . . y N1 Cu1 N5 111.08(12) . . y N4 Cu1 N5 83.69(12) . . y N8 Cu2 N40 157.49(13) . . y N8 Cu2 N7 80.15(12) . . y N40 Cu2 N7 106.70(12) . . y N8 Cu2 N9 83.90(12) . . y N40 Cu2 N9 85.19(12) . . y N7 Cu2 N9 161.94(12) . . y N8 Cu2 N10 101.79(12) . . y N40 Cu2 N10 96.34(12) . . y N7 Cu2 N10 108.44(12) . . y N9 Cu2 N10 83.03(11) . . y N2 N1 C5 121.4(3) . . ? N2 N1 Cu1 125.5(2) . . ? C5 N1 Cu1 112.8(2) . . ? N1 N2 C2 118.6(3) . . ? N2 C2 C3 123.1(3) . . ? N2 C2 C21 113.9(3) . . ? C3 C2 C21 123.0(3) . . ? C4 C3 C2 117.6(3) . . ? C3 C4 C5 117.6(3) . . ? N1 C5 C4 121.4(3) . . ? N1 C5 C6 113.2(3) . . ? C4 C5 C6 125.2(3) . . ? N3 C6 C5 115.7(3) . . ? C6 N3 C7 126.3(3) . . ? C6 N3 Cu1 117.8(3) . . ? C7 N3 Cu1 115.7(2) . . ? N3 C7 C8 106.2(3) . . ? N4 C8 C7 109.1(3) . . ? C9 N4 C30 112.0(3) . . ? C9 N4 C8 111.1(3) . . ? C30 N4 C8 113.0(3) . . ? C9 N4 Cu1 108.7(2) . . ? C30 N4 Cu1 105.2(2) . . ? C8 N4 Cu1 106.4(2) . . ? N4 C30 C31 109.6(3) . . ? N30 C31 C32 120.6(3) . . ? N30 C31 C30 115.9(3) . . ? C32 C31 C30 123.5(3) . . ? C33 C32 C31 119.4(3) . . ? C32 C33 C34 119.7(3) . . ? C35 C34 C33 118.6(3) . . ? N30 C35 C34 122.1(3) . . ? C35 N30 C31 119.7(3) . . ? C35 N30 Cu1 126.3(2) . . ? C31 N30 Cu1 112.5(2) . . ? N4 C9 C10 113.3(3) . . ? N5 C10 C9 108.9(3) . . ? C11 N5 C10 119.0(3) . . ? C11 N5 Cu1 136.1(3) . . ? C10 N5 Cu1 104.9(2) . . ? N5 C11 C12 119.7(3) . . ? N7 N6 C12 117.9(3) . . ? N6 N7 C15 121.5(3) . . ? N6 N7 Cu2 125.3(2) . . ? C15 N7 Cu2 113.0(2) . . ? N6 C12 C13 123.1(3) . . ? N6 C12 C11 114.6(3) . . ? C13 C12 C11 122.3(3) . . ? C14 C13 C12 118.3(3) . . ? C13 C14 C15 117.0(4) . . ? N7 C15 C14 122.2(3) . . ? N7 C15 C16 113.3(3) . . ? C14 C15 C16 124.5(3) . . ? N8 C16 C15 115.6(3) . . ? C16 N8 C17 125.9(3) . . ? C16 N8 Cu2 117.3(3) . . ? C17 N8 Cu2 115.7(2) . . ? N8 C17 C18 106.0(3) . . ? N9 C18 C17 109.9(3) . . ? C40 N9 C18 112.7(3) . . ? C40 N9 C19 112.3(3) . . ? C18 N9 C19 109.6(3) . . ? C40 N9 Cu2 106.1(2) . . ? C18 N9 Cu2 106.0(2) . . ? C19 N9 Cu2 109.9(2) . . ? N9 C40 C41 111.7(3) . . ? N40 C41 C42 121.5(4) . . ? N40 C41 C40 115.7(3) . . ? C42 C41 C40 122.7(4) . . ? C41 C42 C43 119.4(4) . . ? C42 C43 C44 119.3(4) . . ? C45 C44 C43 118.5(4) . . ? N40 C45 C44 122.5(4) . . ? C45 N40 C41 118.8(3) . . ? C45 N40 Cu2 127.6(3) . . ? C41 N40 Cu2 113.4(2) . . ? N9 C19 C20 112.4(3) . . ? N10 C20 C19 108.4(3) . . ? C21 N10 C20 118.7(3) . . ? C21 N10 Cu2 129.6(2) . . ? C20 N10 Cu2 104.6(2) . . ? N10 C21 C2 119.2(3) . . ? O11 Cl1 O12 109.35(16) . . ? O11 Cl1 O14 110.08(17) . . ? O12 Cl1 O14 109.17(16) . . ? O11 Cl1 O13 109.43(17) . . ? O12 Cl1 O13 109.32(18) . . ? O14 Cl1 O13 109.47(17) . . ? O22 Cl2 O23 110.63(18) . . ? O22 Cl2 O24 110.05(17) . . ? O23 Cl2 O24 110.7(2) . . ? O22 Cl2 O21 109.18(19) . . ? O23 Cl2 O21 107.7(2) . . ? O24 Cl2 O21 108.5(2) . . ? O36 Cl3 O34 122.2(4) . . ? O36 Cl3 O32 60.8(5) . . ? O34 Cl3 O32 111.4(4) . . ? O36 Cl3 O31 119.5(4) . . ? O34 Cl3 O31 116.1(3) . . ? O32 Cl3 O31 111.5(3) . . ? O36 Cl3 O37 109.2(6) . . ? O34 Cl3 O37 31.8(4) . . ? O32 Cl3 O37 134.2(5) . . ? O31 Cl3 O37 111.4(5) . . ? O36 Cl3 O33 44.1(5) . . ? O34 Cl3 O33 108.7(4) . . ? O32 Cl3 O33 104.9(4) . . ? O31 Cl3 O33 103.4(3) . . ? O37 Cl3 O33 80.1(5) . . ? O36 Cl3 O35 111.5(6) . . ? O34 Cl3 O35 72.1(5) . . ? O32 Cl3 O35 53.1(5) . . ? O31 Cl3 O35 100.1(4) . . ? O37 Cl3 O35 103.9(6) . . ? O33 Cl3 O35 152.9(5) . . ? O48 Cl4 O41 159.6(6) . . ? O48 Cl4 O43 63.0(7) . . ? O41 Cl4 O43 110.7(4) . . ? O48 Cl4 O42 88.3(6) . . ? O41 Cl4 O42 111.8(4) . . ? O43 Cl4 O42 109.9(4) . . ? O48 Cl4 O46 114.1(8) . . ? O41 Cl4 O46 46.5(5) . . ? O43 Cl4 O46 103.2(5) . . ? O42 Cl4 O46 146.0(5) . . ? O48 Cl4 O44 59.3(7) . . ? O41 Cl4 O44 108.8(5) . . ? O43 Cl4 O44 108.1(4) . . ? O42 Cl4 O44 107.4(3) . . ? O46 Cl4 O44 68.1(6) . . ? O48 Cl4 O47 112.8(11) . . ? O41 Cl4 O47 71.6(9) . . ? O43 Cl4 O47 54.2(8) . . ? O42 Cl4 O47 92.0(6) . . ? O46 Cl4 O47 101.4(9) . . ? O44 Cl4 O47 158.1(6) . . ? O48 Cl4 O45 113.3(7) . . ? O41 Cl4 O45 82.2(6) . . ? O43 Cl4 O45 149.3(7) . . ? O42 Cl4 O45 40.5(5) . . ? O46 Cl4 O45 105.5(8) . . ? O44 Cl4 O45 92.7(5) . . ? O47 Cl4 O45 108.9(8) . . ? N50 C50 C51 178.6(5) . . ? N60 C60 C61 179.3(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 Cu1 N1 N2 -173.2(3) . . . . ? N30 Cu1 N1 N2 -11.4(3) . . . . ? N4 Cu1 N1 N2 -138.0(3) . . . . ? N5 Cu1 N1 N2 83.6(3) . . . . ? N3 Cu1 N1 C5 1.3(3) . . . . ? N30 Cu1 N1 C5 163.1(2) . . . . ? N4 Cu1 N1 C5 36.5(5) . . . . ? N5 Cu1 N1 C5 -101.9(3) . . . . ? C5 N1 N2 C2 0.1(5) . . . . ? Cu1 N1 N2 C2 174.2(2) . . . . ? N1 N2 C2 C3 3.0(5) . . . . ? N1 N2 C2 C21 -175.5(3) . . . . ? N2 C2 C3 C4 -2.7(6) . . . . ? C21 C2 C3 C4 175.7(4) . . . . ? C2 C3 C4 C5 -0.7(6) . . . . ? N2 N1 C5 C4 -3.5(5) . . . . ? Cu1 N1 C5 C4 -178.3(3) . . . . ? N2 N1 C5 C6 173.3(3) . . . . ? Cu1 N1 C5 C6 -1.4(4) . . . . ? C3 C4 C5 N1 3.7(6) . . . . ? C3 C4 C5 C6 -172.7(4) . . . . ? N1 C5 C6 N3 0.8(5) . . . . ? C4 C5 C6 N3 177.4(4) . . . . ? C5 C6 N3 C7 -173.7(3) . . . . ? C5 C6 N3 Cu1 0.4(4) . . . . ? N30 Cu1 N3 C6 -115.1(4) . . . . ? N1 Cu1 N3 C6 -0.9(3) . . . . ? N4 Cu1 N3 C6 -169.9(3) . . . . ? N5 Cu1 N3 C6 108.5(3) . . . . ? N30 Cu1 N3 C7 59.6(5) . . . . ? N1 Cu1 N3 C7 173.8(3) . . . . ? N4 Cu1 N3 C7 4.8(3) . . . . ? N5 Cu1 N3 C7 -76.8(3) . . . . ? C6 N3 C7 C8 145.4(4) . . . . ? Cu1 N3 C7 C8 -28.8(4) . . . . ? N3 C7 C8 N4 46.0(4) . . . . ? C7 C8 N4 C9 76.1(4) . . . . ? C7 C8 N4 C30 -157.0(3) . . . . ? C7 C8 N4 Cu1 -42.1(3) . . . . ? N3 Cu1 N4 C9 -98.8(2) . . . . ? N30 Cu1 N4 C9 96.7(2) . . . . ? N1 Cu1 N4 C9 -133.8(3) . . . . ? N5 Cu1 N4 C9 7.7(2) . . . . ? N3 Cu1 N4 C30 141.1(2) . . . . ? N30 Cu1 N4 C30 -23.4(2) . . . . ? N1 Cu1 N4 C30 106.1(4) . . . . ? N5 Cu1 N4 C30 -112.4(2) . . . . ? N3 Cu1 N4 C8 20.9(2) . . . . ? N30 Cu1 N4 C8 -143.5(2) . . . . ? N1 Cu1 N4 C8 -14.0(5) . . . . ? N5 Cu1 N4 C8 127.5(2) . . . . ? C9 N4 C30 C31 -82.7(4) . . . . ? C8 N4 C30 C31 150.9(3) . . . . ? Cu1 N4 C30 C31 35.2(3) . . . . ? N4 C30 C31 N30 -34.0(4) . . . . ? N4 C30 C31 C32 147.6(3) . . . . ? N30 C31 C32 C33 -0.3(5) . . . . ? C30 C31 C32 C33 178.0(3) . . . . ? C31 C32 C33 C34 0.8(5) . . . . ? C32 C33 C34 C35 0.0(5) . . . . ? C33 C34 C35 N30 -1.3(5) . . . . ? C34 C35 N30 C31 1.8(5) . . . . ? C34 C35 N30 Cu1 166.9(3) . . . . ? C32 C31 N30 C35 -0.9(5) . . . . ? C30 C31 N30 C35 -179.4(3) . . . . ? C32 C31 N30 Cu1 -167.9(3) . . . . ? C30 C31 N30 Cu1 13.6(4) . . . . ? N3 Cu1 N30 C35 145.6(4) . . . . ? N1 Cu1 N30 C35 35.6(3) . . . . ? N4 Cu1 N30 C35 -159.7(3) . . . . ? N5 Cu1 N30 C35 -75.9(3) . . . . ? N3 Cu1 N30 C31 -48.4(5) . . . . ? N1 Cu1 N30 C31 -158.4(2) . . . . ? N4 Cu1 N30 C31 6.2(2) . . . . ? N5 Cu1 N30 C31 90.0(2) . . . . ? C30 N4 C9 C10 81.9(4) . . . . ? C8 N4 C9 C10 -150.6(3) . . . . ? Cu1 N4 C9 C10 -33.9(3) . . . . ? N4 C9 C10 N5 51.9(4) . . . . ? C9 C10 N5 C11 137.7(4) . . . . ? C9 C10 N5 Cu1 -40.3(3) . . . . ? N3 Cu1 N5 C11 -77.4(4) . . . . ? N30 Cu1 N5 C11 115.6(4) . . . . ? N1 Cu1 N5 C11 8.2(4) . . . . ? N4 Cu1 N5 C11 -159.1(4) . . . . ? N3 Cu1 N5 C10 100.2(2) . . . . ? N30 Cu1 N5 C10 -66.8(2) . . . . ? N1 Cu1 N5 C10 -174.3(2) . . . . ? N4 Cu1 N5 C10 18.4(2) . . . . ? C10 N5 C11 C12 177.7(3) . . . . ? Cu1 N5 C11 C12 -5.0(6) . . . . ? C12 N6 N7 C15 -2.4(5) . . . . ? C12 N6 N7 Cu2 171.2(3) . . . . ? N8 Cu2 N7 N6 179.3(3) . . . . ? N40 Cu2 N7 N6 -22.7(3) . . . . ? N9 Cu2 N7 N6 -152.4(4) . . . . ? N10 Cu2 N7 N6 80.1(3) . . . . ? N8 Cu2 N7 C15 -6.6(3) . . . . ? N40 Cu2 N7 C15 151.3(2) . . . . ? N9 Cu2 N7 C15 21.7(6) . . . . ? N10 Cu2 N7 C15 -105.9(3) . . . . ? N7 N6 C12 C13 0.6(5) . . . . ? N7 N6 C12 C11 -179.5(3) . . . . ? N5 C11 C12 N6 -68.5(5) . . . . ? N5 C11 C12 C13 111.5(4) . . . . ? N6 C12 C13 C14 2.5(6) . . . . ? C11 C12 C13 C14 -177.4(4) . . . . ? C12 C13 C14 C15 -3.6(5) . . . . ? N6 N7 C15 C14 1.2(5) . . . . ? Cu2 N7 C15 C14 -173.1(3) . . . . ? N6 N7 C15 C16 179.1(3) . . . . ? Cu2 N7 C15 C16 4.8(4) . . . . ? C13 C14 C15 N7 1.9(6) . . . . ? C13 C14 C15 C16 -175.7(4) . . . . ? N7 C15 C16 N8 1.5(5) . . . . ? C14 C15 C16 N8 179.4(4) . . . . ? C15 C16 N8 C17 -174.5(3) . . . . ? C15 C16 N8 Cu2 -7.5(4) . . . . ? N40 Cu2 N8 C16 -102.2(4) . . . . ? N7 Cu2 N8 C16 7.9(3) . . . . ? N9 Cu2 N8 C16 -163.6(3) . . . . ? N10 Cu2 N8 C16 114.9(3) . . . . ? N40 Cu2 N8 C17 66.2(4) . . . . ? N7 Cu2 N8 C17 176.3(3) . . . . ? N9 Cu2 N8 C17 4.8(3) . . . . ? N10 Cu2 N8 C17 -76.8(3) . . . . ? C16 N8 C17 C18 138.9(4) . . . . ? Cu2 N8 C17 C18 -28.4(4) . . . . ? N8 C17 C18 N9 45.9(4) . . . . ? C17 C18 N9 C40 -157.6(3) . . . . ? C17 C18 N9 C19 76.6(4) . . . . ? C17 C18 N9 Cu2 -41.9(3) . . . . ? N8 Cu2 N9 C40 140.7(2) . . . . ? N40 Cu2 N9 C40 -19.5(2) . . . . ? N7 Cu2 N9 C40 112.7(4) . . . . ? N10 Cu2 N9 C40 -116.6(2) . . . . ? N8 Cu2 N9 C18 20.7(2) . . . . ? N40 Cu2 N9 C18 -139.6(2) . . . . ? N7 Cu2 N9 C18 -7.4(5) . . . . ? N10 Cu2 N9 C18 123.4(2) . . . . ? N8 Cu2 N9 C19 -97.7(2) . . . . ? N40 Cu2 N9 C19 102.0(2) . . . . ? N7 Cu2 N9 C19 -125.7(4) . . . . ? N10 Cu2 N9 C19 5.0(2) . . . . ? C18 N9 C40 C41 145.1(3) . . . . ? C19 N9 C40 C41 -90.6(4) . . . . ? Cu2 N9 C40 C41 29.5(3) . . . . ? N9 C40 C41 N40 -27.9(5) . . . . ? N9 C40 C41 C42 156.1(4) . . . . ? N40 C41 C42 C43 -1.2(6) . . . . ? C40 C41 C42 C43 174.6(4) . . . . ? C41 C42 C43 C44 -0.4(6) . . . . ? C42 C43 C44 C45 1.3(6) . . . . ? C43 C44 C45 N40 -0.8(6) . . . . ? C44 C45 N40 C41 -0.7(5) . . . . ? C44 C45 N40 Cu2 173.6(3) . . . . ? C42 C41 N40 C45 1.7(5) . . . . ? C40 C41 N40 C45 -174.4(3) . . . . ? C42 C41 N40 Cu2 -173.4(3) . . . . ? C40 C41 N40 Cu2 10.6(4) . . . . ? N8 Cu2 N40 C45 129.8(4) . . . . ? N7 Cu2 N40 C45 24.9(3) . . . . ? N9 Cu2 N40 C45 -169.0(3) . . . . ? N10 Cu2 N40 C45 -86.6(3) . . . . ? N8 Cu2 N40 C41 -55.7(4) . . . . ? N7 Cu2 N40 C41 -160.6(2) . . . . ? N9 Cu2 N40 C41 5.5(2) . . . . ? N10 Cu2 N40 C41 88.0(3) . . . . ? C40 N9 C19 C20 86.2(4) . . . . ? C18 N9 C19 C20 -147.7(3) . . . . ? Cu2 N9 C19 C20 -31.6(4) . . . . ? N9 C19 C20 N10 52.2(4) . . . . ? C19 C20 N10 C21 109.9(4) . . . . ? C19 C20 N10 Cu2 -43.4(3) . . . . ? N8 Cu2 N10 C21 -45.3(3) . . . . ? N40 Cu2 N10 C21 148.1(3) . . . . ? N7 Cu2 N10 C21 38.1(4) . . . . ? N9 Cu2 N10 C21 -127.5(3) . . . . ? N8 Cu2 N10 C20 104.0(2) . . . . ? N40 Cu2 N10 C20 -62.6(2) . . . . ? N7 Cu2 N10 C20 -172.6(2) . . . . ? N9 Cu2 N10 C20 21.7(2) . . . . ? C20 N10 C21 C2 178.1(3) . . . . ? Cu2 N10 C21 C2 -36.3(5) . . . . ? N2 C2 C21 N10 -53.0(5) . . . . ? C3 C2 C21 N10 128.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.302 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.089 data_mw52a _database_code_depnum_ccdc_archive 'CCDC 269196' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H51 Cl4 Fe2 N17 O16' _chemical_formula_weight 1303.50 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.496 _cell_length_b 17.8357(3) _cell_length_c 21.1804(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.4170(10) _cell_angle_gamma 90.00 _cell_volume 5279.14(13) _cell_formula_units_Z 4 _cell_measurement_temperature 84(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular fragment' _exptl_crystal_colour dark _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.546 _exptl_absorpt_correction_T_max 0.867 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 84(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 SMART area detector' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29034 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.0906 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.62 _reflns_number_total 9844 _reflns_number_gt 6854 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. In view of the severely disordered anions (2 ClO4- of the 4 ClO4- per Fe2 macrocycle) and solvent (2-3 MeCN in total per Fe2, but spread over many partial occupancy sites), and the fact that the best attempt to model this gave an R1 on observed data of 0.1338, cf R(int) = 0.0681, the structure was subjected to the SQUEEZE procedure of the PLATON suite (P. van der Sluis, A. L. Spek, Acta Crystallogr., Section A, 1990, 46, 194-201). A total potential solvent/anion accessible volume of 1459 A^3^ per cell containing 680 electrons was calculated. The electron count is close to that calculated (664 electrons) for 8ClO4- and 12MeCN per cell. The final value for R1 on observed data on reincorporation of electron density in the void volume was 0.087. The chemical formulae, electron count, absorption coefficient and other derived parameters reported above and below are based on the presence of 2ClO4- and 3MeCN in the void space per Fe2 macrocycle. ; _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^)+(0.0551P)^2^+27.5277P] 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 9844 _refine_ls_number_parameters 572 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.1963 _refine_ls_wR_factor_gt 0.1842 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.059 _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 Fe1 Fe 0.74164(5) 0.82916(5) -0.00635(4) 0.0273(2) Uani 1 1 d . . . Fe2 Fe 0.56309(6) 0.73249(5) 0.19129(4) 0.0242(2) Uani 1 1 d . . . N1 N 0.7794(3) 0.7535(3) 0.0625(2) 0.0251(11) Uani 1 1 d . . . N2 N 0.7200(3) 0.7123(3) 0.0877(2) 0.0282(12) Uani 1 1 d . . . C2 C 0.7579(4) 0.6605(4) 0.1333(3) 0.0313(14) Uani 1 1 d . . . C3 C 0.8571(5) 0.6478(4) 0.1562(3) 0.0369(16) Uani 1 1 d . . . H3 H 0.8816 0.6124 0.1901 0.044 Uiso 1 1 calc R . . C4 C 0.9172(5) 0.6869(4) 0.1290(3) 0.0360(16) Uani 1 1 d . . . H4 H 0.9844 0.6789 0.1424 0.043 Uiso 1 1 calc R . . C5 C 0.8762(4) 0.7394(3) 0.0804(3) 0.0291(14) Uani 1 1 d . . . C6 C 0.9268(4) 0.7806(4) 0.0405(3) 0.0293(14) Uani 1 1 d . . . H6 H 0.9944 0.7791 0.0481 0.035 Uiso 1 1 calc R . . N3 N 0.8724(3) 0.8192(3) -0.0056(2) 0.0255(11) Uani 1 1 d . . . C7 C 0.9082(4) 0.8664(4) -0.0529(3) 0.0344(16) Uani 1 1 d . . . H7A H 0.9574 0.8390 -0.0684 0.041 Uiso 1 1 calc R . . H7B H 0.9363 0.9137 -0.0320 0.041 Uiso 1 1 calc R . . C8 C 0.8202(4) 0.8820(4) -0.1096(3) 0.0347(15) Uani 1 1 d . . . H8A H 0.8074 0.8385 -0.1397 0.042 Uiso 1 1 calc R . . H8B H 0.8321 0.9263 -0.1345 0.042 Uiso 1 1 calc R . . N4 N 0.7336(3) 0.8965(3) -0.0830(3) 0.0345(13) Uani 1 1 d . . . C30 C 0.6457(4) 0.8711(4) -0.1360(3) 0.0382(17) Uani 1 1 d . . . H30A H 0.5866 0.8901 -0.1266 0.046 Uiso 1 1 calc R . . H30B H 0.6485 0.8904 -0.1793 0.046 Uiso 1 1 calc R . . C31 C 0.6462(5) 0.7873(5) -0.1359(3) 0.047(2) Uani 1 1 d . . . C32 C 0.6024(5) 0.7425(6) -0.1908(4) 0.060(3) Uani 1 1 d . . . H32 H 0.5713 0.7653 -0.2314 0.072 Uiso 1 1 calc R . . C33 C 0.6052(6) 0.6657(7) -0.1850(4) 0.072(3) Uani 1 1 d . . . H33 H 0.5769 0.6355 -0.2221 0.086 Uiso 1 1 calc R . . C34 C 0.6491(5) 0.6313(6) -0.1251(4) 0.062(2) Uani 1 1 d . . . H34 H 0.6504 0.5783 -0.1204 0.074 Uiso 1 1 calc R . . C35 C 0.6911(5) 0.6783(4) -0.0723(3) 0.0390(16) Uani 1 1 d . . . H35 H 0.7220 0.6559 -0.0314 0.047 Uiso 1 1 calc R . . N30 N 0.6898(3) 0.7543(3) -0.0766(2) 0.0326(13) Uani 1 1 d . . . C9 C 0.7258(5) 0.9764(4) -0.0630(3) 0.0394(17) Uani 1 1 d . . . H9A H 0.6582 0.9885 -0.0658 0.047 Uiso 1 1 calc R . . H9B H 0.7480 1.0104 -0.0929 0.047 Uiso 1 1 calc R . . C10 C 0.7871(4) 0.9872(4) 0.0073(3) 0.0348(15) Uani 1 1 d . . . H10A H 0.8556 0.9906 0.0079 0.042 Uiso 1 1 calc R . . H10B H 0.7688 1.0342 0.0256 0.042 Uiso 1 1 calc R . . N5 N 0.7716(3) 0.9220(3) 0.0472(2) 0.0258(11) Uani 1 1 d . . . C11 C 0.7763(4) 0.9375(3) 0.1077(3) 0.0242(13) Uani 1 1 d . . . H11 H 0.7879 0.9886 0.1200 0.029 Uiso 1 1 calc R . . C12 C 0.7657(4) 0.8857(3) 0.1607(3) 0.0239(12) Uani 1 1 d . . . C13 C 0.8340(4) 0.8864(4) 0.2205(3) 0.0321(14) Uani 1 1 d . . . H13 H 0.8894 0.9170 0.2270 0.039 Uiso 1 1 calc R . . C14 C 0.8202(4) 0.8416(4) 0.2706(3) 0.0387(17) Uani 1 1 d . . . H14 H 0.8657 0.8400 0.3122 0.046 Uiso 1 1 calc R . . C15 C 0.7369(4) 0.7991(3) 0.2575(3) 0.0254(13) Uani 1 1 d . . . N6 N 0.6871(3) 0.8412(3) 0.1480(2) 0.0249(11) Uani 1 1 d . . . N7 N 0.6740(3) 0.7968(3) 0.1963(2) 0.0216(10) Uani 1 1 d . . . C16 C 0.7041(4) 0.7544(3) 0.3047(3) 0.0256(13) Uani 1 1 d . . . H16 H 0.7399 0.7490 0.3491 0.031 Uiso 1 1 calc R . . N8 N 0.6217(3) 0.7224(2) 0.2812(2) 0.0217(10) Uani 1 1 d . . . C17 C 0.5761(4) 0.6744(4) 0.3204(3) 0.0324(14) Uani 1 1 d . . . H17A H 0.5834 0.6964 0.3643 0.039 Uiso 1 1 calc R . . H17B H 0.6057 0.6240 0.3257 0.039 Uiso 1 1 calc R . . C18 C 0.4696(4) 0.6690(4) 0.2832(3) 0.0281(13) Uani 1 1 d . . . H18A H 0.4428 0.6215 0.2948 0.034 Uiso 1 1 calc R . . H18B H 0.4343 0.7110 0.2965 0.034 Uiso 1 1 calc R . . N9 N 0.4561(3) 0.6719(3) 0.2095(2) 0.0276(11) Uani 1 1 d . . . C40 C 0.3658(4) 0.7160(4) 0.1813(3) 0.0344(15) Uani 1 1 d . . . H40A H 0.3443 0.7088 0.1333 0.041 Uiso 1 1 calc R . . H40B H 0.3144 0.6985 0.2005 0.041 Uiso 1 1 calc R . . C41 C 0.3867(4) 0.7966(4) 0.1969(3) 0.0313(14) Uani 1 1 d . . . C42 C 0.3192(4) 0.8494(4) 0.2054(3) 0.0373(17) Uani 1 1 d . . . H42 H 0.2547 0.8346 0.2003 0.045 Uiso 1 1 calc R . . C43 C 0.3461(5) 0.9236(5) 0.2211(3) 0.0468(19) Uani 1 1 d . . . H43 H 0.3008 0.9596 0.2269 0.056 Uiso 1 1 calc R . . C44 C 0.4429(5) 0.9438(4) 0.2283(3) 0.0387(16) Uani 1 1 d . . . H44 H 0.4639 0.9937 0.2395 0.046 Uiso 1 1 calc R . . C45 C 0.5067(5) 0.8893(4) 0.2186(3) 0.0350(15) Uani 1 1 d . . . H45 H 0.5713 0.9032 0.2229 0.042 Uiso 1 1 calc R . . N40 N 0.4802(3) 0.8171(3) 0.2034(2) 0.0273(11) Uani 1 1 d . . . C19 C 0.4560(5) 0.5972(4) 0.1804(3) 0.0390(17) Uani 1 1 d . . . H19A H 0.4243 0.5993 0.1328 0.047 Uiso 1 1 calc R . . H19B H 0.4203 0.5615 0.2008 0.047 Uiso 1 1 calc R . . C20 C 0.5574(5) 0.5718(3) 0.1916(3) 0.0310(14) Uani 1 1 d . . . H20A H 0.5834 0.5571 0.2380 0.037 Uiso 1 1 calc R . . H20B H 0.5598 0.5274 0.1640 0.037 Uiso 1 1 calc R . . N10 N 0.6165(4) 0.6327(3) 0.1752(2) 0.0268(11) Uani 1 1 d . . . C21 C 0.6885(5) 0.6114(4) 0.1559(3) 0.0330(15) Uani 1 1 d . . . H21 H 0.6995 0.5589 0.1559 0.040 Uiso 1 1 calc R . . N200 N 0.6104(3) 0.8492(3) -0.0016(2) 0.0293(12) Uani 1 1 d . . . C200 C 0.5419(4) 0.8741(4) 0.0110(3) 0.0285(14) Uani 1 1 d . . . C201 C 0.4608(4) 0.9050(3) 0.0290(3) 0.0259(13) Uani 1 1 d . . . H20A' H 0.4036 0.8755 0.0086 0.031 Uiso 1 1 calc R . . H20B' H 0.4511 0.9571 0.0139 0.031 Uiso 1 1 calc R . . H20C H 0.4725 0.9035 0.0767 0.031 Uiso 1 1 calc R . . N210 N 0.5045(3) 0.7329(3) 0.0955(2) 0.0282(11) Uani 1 1 d . . . C210 C 0.4775(4) 0.7220(3) 0.0399(3) 0.0274(13) Uani 1 1 d . . . C211 C 0.4461(5) 0.7094(4) -0.0303(3) 0.0405(17) Uani 1 1 d . . . H21A H 0.4269 0.7572 -0.0528 0.049 Uiso 1 1 calc R . . H21B H 0.3916 0.6748 -0.0403 0.049 Uiso 1 1 calc R . . H21C H 0.4987 0.6877 -0.0453 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.04157(10) 0.94538(9) 0.14623(7) 0.0314(3) Uani 1 1 d D . . O11 O 0.0073(4) 0.8712(2) 0.1565(2) 0.0457(12) Uani 1 1 d D . . O12 O -0.0250(4) 1.0007(3) 0.1571(3) 0.0650(17) Uani 1 1 d D . . O13 O 0.1316(4) 0.9600(4) 0.1923(3) 0.083(2) Uani 1 1 d D . . O14 O 0.0493(6) 0.9533(3) 0.0812(3) 0.079(2) Uani 1 1 d D . . Cl2 Cl 0.86449(12) 0.58396(11) 0.33547(10) 0.0519(5) Uani 1 1 d D . . O21 O 0.9029(4) 0.6527(3) 0.3211(3) 0.0667(17) Uani 1 1 d D A . O22 O 0.8065(7) 0.6127(6) 0.3819(5) 0.077(3) Uani 0.60 1 d PD A 1 O23 O 0.8019(7) 0.5489(6) 0.2855(4) 0.073(3) Uani 0.60 1 d PD A 1 O24 O 0.9386(5) 0.5416(4) 0.3780(4) 0.0395(18) Uani 0.60 1 d PD A 1 O25 O 0.7592(7) 0.5805(6) 0.3147(6) 0.0395(18) Uani 0.40 1 d PD A 2 O26 O 0.8818(12) 0.5370(8) 0.2770(6) 0.077(3) Uani 0.40 1 d PD A 2 O27 O 0.8986(11) 0.5305(9) 0.3857(7) 0.073(3) Uani 0.40 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0127(4) 0.0445(5) 0.0222(5) 0.0024(4) 0.0004(3) 0.0069(4) Fe2 0.0209(4) 0.0287(5) 0.0202(4) 0.0002(4) 0.0007(3) -0.0024(4) N1 0.014(2) 0.034(3) 0.025(3) -0.005(2) 0.0010(19) 0.003(2) N2 0.025(3) 0.036(3) 0.024(3) -0.011(2) 0.007(2) -0.007(2) C2 0.033(3) 0.038(4) 0.023(3) -0.005(3) 0.008(3) 0.004(3) C3 0.036(4) 0.024(3) 0.048(4) 0.002(3) 0.006(3) 0.010(3) C4 0.025(3) 0.047(4) 0.032(4) 0.004(3) 0.001(3) 0.004(3) C5 0.021(3) 0.030(3) 0.033(3) -0.008(3) 0.001(3) 0.002(3) C6 0.013(3) 0.048(4) 0.024(3) -0.004(3) -0.001(2) 0.005(3) N3 0.017(2) 0.035(3) 0.024(3) -0.001(2) 0.002(2) 0.002(2) C7 0.014(3) 0.060(5) 0.032(4) 0.009(3) 0.011(3) 0.010(3) C8 0.020(3) 0.059(5) 0.025(3) 0.007(3) 0.004(3) 0.006(3) N4 0.019(3) 0.053(4) 0.031(3) 0.006(3) 0.006(2) 0.004(2) C30 0.026(3) 0.061(5) 0.023(3) 0.011(3) -0.001(3) 0.015(3) C31 0.022(3) 0.095(7) 0.022(3) -0.003(4) 0.003(3) 0.004(4) C32 0.030(4) 0.113(9) 0.029(4) -0.003(5) -0.004(3) 0.005(5) C33 0.043(5) 0.120(10) 0.044(5) -0.022(6) -0.003(4) -0.002(5) C34 0.043(4) 0.089(7) 0.048(5) -0.033(5) 0.002(4) -0.026(4) C35 0.030(3) 0.047(4) 0.038(4) -0.006(3) 0.006(3) -0.004(3) N30 0.010(2) 0.063(4) 0.024(3) -0.007(3) 0.002(2) 0.001(2) C9 0.031(3) 0.059(5) 0.032(4) 0.019(3) 0.014(3) 0.017(3) C10 0.029(3) 0.044(4) 0.032(4) 0.009(3) 0.009(3) 0.008(3) N5 0.012(2) 0.038(3) 0.027(3) 0.010(2) 0.004(2) 0.010(2) C11 0.014(3) 0.021(3) 0.034(3) 0.010(3) 0.002(2) 0.005(2) C12 0.025(3) 0.019(3) 0.026(3) -0.001(2) 0.005(2) 0.005(2) C13 0.024(3) 0.036(4) 0.034(4) -0.007(3) 0.003(3) -0.009(3) C14 0.023(3) 0.060(5) 0.026(3) 0.003(3) -0.006(3) -0.011(3) C15 0.024(3) 0.028(3) 0.023(3) -0.003(2) 0.006(2) 0.005(2) N6 0.023(2) 0.028(3) 0.022(3) 0.002(2) 0.005(2) 0.000(2) N7 0.022(2) 0.020(2) 0.020(2) 0.0020(19) 0.001(2) 0.0031(19) C16 0.027(3) 0.024(3) 0.022(3) 0.001(2) 0.001(2) 0.006(2) N8 0.022(2) 0.014(2) 0.027(3) 0.0019(19) 0.004(2) -0.0018(19) C17 0.030(3) 0.041(4) 0.024(3) 0.005(3) 0.002(3) -0.004(3) C18 0.023(3) 0.028(3) 0.032(3) 0.002(3) 0.005(3) -0.005(3) N9 0.024(2) 0.029(3) 0.026(3) -0.003(2) 0.000(2) -0.006(2) C40 0.020(3) 0.052(4) 0.028(3) 0.003(3) 0.002(3) -0.006(3) C41 0.020(3) 0.044(4) 0.028(3) 0.017(3) 0.003(3) 0.013(3) C42 0.026(3) 0.061(5) 0.025(3) 0.020(3) 0.007(3) 0.011(3) C43 0.028(4) 0.070(6) 0.038(4) 0.009(4) 0.000(3) 0.022(4) C44 0.032(4) 0.048(4) 0.036(4) 0.012(3) 0.009(3) 0.013(3) C45 0.028(3) 0.041(4) 0.037(4) 0.006(3) 0.009(3) -0.001(3) N40 0.013(2) 0.043(3) 0.023(3) 0.010(2) 0.0004(19) 0.004(2) C19 0.040(4) 0.045(4) 0.034(4) -0.011(3) 0.015(3) -0.022(3) C20 0.045(4) 0.010(3) 0.041(4) -0.001(3) 0.016(3) -0.008(3) N10 0.035(3) 0.020(3) 0.024(3) 0.001(2) 0.005(2) 0.000(2) C21 0.042(4) 0.027(3) 0.025(3) -0.004(3) 0.002(3) -0.003(3) N200 0.015(2) 0.051(3) 0.019(3) 0.004(2) 0.001(2) 0.004(2) C200 0.017(3) 0.033(3) 0.030(3) 0.000(3) -0.004(2) -0.004(3) C201 0.021(3) 0.024(3) 0.035(3) -0.003(3) 0.010(3) -0.002(2) N210 0.023(3) 0.037(3) 0.024(3) -0.003(2) 0.004(2) -0.003(2) C210 0.023(3) 0.030(3) 0.029(3) 0.003(3) 0.005(3) 0.005(3) C211 0.046(4) 0.047(4) 0.021(3) -0.009(3) -0.004(3) 0.003(3) Cl1 0.0261(7) 0.0367(8) 0.0307(8) 0.0076(7) 0.0061(6) 0.0109(6) O11 0.070(3) 0.026(2) 0.039(3) 0.000(2) 0.010(2) 0.006(2) O12 0.036(3) 0.044(3) 0.117(5) -0.022(3) 0.026(3) 0.006(2) O13 0.028(3) 0.091(5) 0.105(5) 0.058(4) -0.026(3) -0.010(3) O14 0.160(7) 0.048(4) 0.043(3) 0.001(3) 0.050(4) -0.004(4) Cl2 0.0251(8) 0.0620(12) 0.0654(13) 0.0405(10) 0.0066(8) 0.0036(8) O21 0.041(3) 0.045(3) 0.104(5) 0.012(3) 0.000(3) -0.018(3) O22 0.079(6) 0.075(6) 0.091(7) 0.045(5) 0.048(5) 0.042(5) O23 0.055(6) 0.083(7) 0.059(5) 0.035(5) -0.021(5) -0.025(5) O24 0.040(4) 0.029(4) 0.043(4) 0.005(3) 0.000(3) 0.018(3) O25 0.040(4) 0.029(4) 0.043(4) 0.005(3) 0.000(3) 0.018(3) O26 0.079(6) 0.075(6) 0.091(7) 0.045(5) 0.048(5) 0.042(5) O27 0.055(6) 0.083(7) 0.059(5) 0.035(5) -0.021(5) -0.025(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 Fe1 N3 1.899(5) . Y Fe1 N1 1.956(5) . Y Fe1 N200 1.965(5) . Y Fe1 N5 1.988(5) . Y Fe1 N30 1.992(5) . Y Fe1 N4 1.998(5) . Y Fe2 N8 1.876(5) . Y Fe2 N7 1.955(5) . Y Fe2 N210 1.981(5) . Y Fe2 N40 1.988(5) . Y Fe2 N10 2.006(5) . Y Fe2 N9 2.010(5) . Y N1 N2 1.346(7) . ? N1 C5 1.376(7) . ? N2 C2 1.342(8) . ? C2 C3 1.409(9) . ? C2 C21 1.506(9) . ? C3 C4 1.358(9) . ? C3 H3 0.9500 . ? C4 C5 1.402(9) . ? C4 H4 0.9500 . ? C5 C6 1.457(9) . ? C6 N3 1.280(7) . ? C6 H6 0.9500 . ? N3 C7 1.503(8) . ? C7 C8 1.527(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N4 1.529(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N4 C9 1.498(9) . ? N4 C30 1.527(8) . ? C30 C31 1.494(11) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N30 1.379(9) . ? C31 C32 1.414(11) . ? C32 C33 1.375(14) . ? C32 H32 0.9500 . ? C33 C34 1.401(13) . ? C33 H33 0.9500 . ? C34 C35 1.400(10) . ? C34 H34 0.9500 . ? C35 N30 1.359(9) . ? C35 H35 0.9500 . ? C9 C10 1.530(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N5 1.490(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? N5 C11 1.297(7) . ? C11 C12 1.492(8) . ? C11 H11 0.9500 . ? C12 N6 1.355(7) . ? C12 C13 1.386(8) . ? C13 C14 1.384(9) . ? C13 H13 0.9500 . ? C14 C15 1.390(8) . ? C14 H14 0.9500 . ? C15 N7 1.373(7) . ? C15 C16 1.454(8) . ? N6 N7 1.347(6) . ? C16 N8 1.297(7) . ? C16 H16 0.9500 . ? N8 C17 1.468(7) . ? C17 C18 1.538(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N9 1.521(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? N9 C19 1.467(8) . ? N9 C40 1.508(8) . ? C40 C41 1.489(10) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 N40 1.375(7) . ? C41 C42 1.404(9) . ? C42 C43 1.393(11) . ? C42 H42 0.9500 . ? C43 C44 1.417(9) . ? C43 H43 0.9500 . ? C44 C45 1.395(9) . ? C44 H44 0.9500 . ? C45 N40 1.357(8) . ? C45 H45 0.9500 . ? C19 C20 1.496(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N10 1.481(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N10 C21 1.275(8) . ? C21 H21 0.9500 . ? N200 C200 1.181(7) . ? C200 C201 1.438(8) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? N210 C210 1.154(7) . ? C210 C211 1.453(8) . ? C211 H21A 0.9800 . ? C211 H21B 0.9800 . ? C211 H21C 0.9800 . ? Cl1 O14 1.419(5) . ? Cl1 O13 1.430(5) . ? Cl1 O12 1.441(5) . ? Cl1 O11 1.450(5) . ? Cl2 O23 1.350(8) . ? Cl2 O21 1.413(5) . ? Cl2 O27 1.416(11) . ? Cl2 O24 1.422(7) . ? Cl2 O25 1.474(10) . ? Cl2 O22 1.541(9) . ? Cl2 O26 1.569(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 N3 Fe1 N1 81.3(2) . . Y N3 Fe1 N200 173.9(2) . . Y N1 Fe1 N200 99.8(2) . . Y N3 Fe1 N5 90.4(2) . . Y N1 Fe1 N5 100.02(19) . . Y N200 Fe1 N5 83.5(2) . . Y N3 Fe1 N30 96.9(2) . . Y N1 Fe1 N30 94.0(2) . . Y N200 Fe1 N30 89.0(2) . . Y N5 Fe1 N30 165.0(2) . . Y N3 Fe1 N4 84.6(2) . . Y N1 Fe1 N4 164.9(2) . . Y N200 Fe1 N4 94.8(2) . . Y N5 Fe1 N4 85.4(2) . . Y N30 Fe1 N4 82.4(2) . . Y N8 Fe2 N7 81.77(19) . . Y N8 Fe2 N210 174.5(2) . . Y N7 Fe2 N210 100.1(2) . . Y N8 Fe2 N40 93.92(19) . . Y N7 Fe2 N40 93.7(2) . . Y N210 Fe2 N40 91.1(2) . . Y N8 Fe2 N10 89.8(2) . . Y N7 Fe2 N10 100.4(2) . . Y N210 Fe2 N10 84.8(2) . . Y N40 Fe2 N10 165.8(2) . . Y N8 Fe2 N9 85.31(19) . . Y N7 Fe2 N9 166.07(19) . . Y N210 Fe2 N9 93.2(2) . . Y N40 Fe2 N9 82.0(2) . . Y N10 Fe2 N9 84.7(2) . . Y N2 N1 C5 120.2(5) . . ? N2 N1 Fe1 126.3(4) . . ? C5 N1 Fe1 113.2(4) . . ? C2 N2 N1 118.6(5) . . ? N2 C2 C3 122.9(6) . . ? N2 C2 C21 116.7(5) . . ? C3 C2 C21 120.3(6) . . ? C4 C3 C2 118.8(6) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 117.4(6) . . ? C3 C4 H4 121.3 . . ? C5 C4 H4 121.3 . . ? N1 C5 C4 121.8(6) . . ? N1 C5 C6 112.4(5) . . ? C4 C5 C6 125.6(5) . . ? N3 C6 C5 114.2(5) . . ? N3 C6 H6 122.9 . . ? C5 C6 H6 122.9 . . ? C6 N3 C7 123.9(5) . . ? C6 N3 Fe1 117.9(4) . . ? C7 N3 Fe1 117.5(3) . . ? N3 C7 C8 105.2(5) . . ? N3 C7 H7A 110.7 . . ? C8 C7 H7A 110.7 . . ? N3 C7 H7B 110.7 . . ? C8 C7 H7B 110.7 . . ? H7A C7 H7B 108.8 . . ? C7 C8 N4 109.7(5) . . ? C7 C8 H8A 109.7 . . ? N4 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? N4 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C9 N4 C30 112.3(5) . . ? C9 N4 C8 113.3(5) . . ? C30 N4 C8 106.6(5) . . ? C9 N4 Fe1 109.6(4) . . ? C30 N4 Fe1 106.0(4) . . ? C8 N4 Fe1 108.7(4) . . ? C31 C30 N4 107.1(5) . . ? C31 C30 H30A 110.3 . . ? N4 C30 H30A 110.3 . . ? C31 C30 H30B 110.3 . . ? N4 C30 H30B 110.3 . . ? H30A C30 H30B 108.6 . . ? N30 C31 C32 120.3(8) . . ? N30 C31 C30 115.4(6) . . ? C32 C31 C30 124.3(7) . . ? C33 C32 C31 119.6(8) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 120.8(8) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C35 C34 C33 117.3(9) . . ? C35 C34 H34 121.3 . . ? C33 C34 H34 121.3 . . ? N30 C35 C34 123.2(7) . . ? N30 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? C35 N30 C31 118.9(6) . . ? C35 N30 Fe1 128.5(4) . . ? C31 N30 Fe1 112.6(5) . . ? N4 C9 C10 109.1(5) . . ? N4 C9 H9A 109.9 . . ? C10 C9 H9A 109.9 . . ? N4 C9 H9B 109.9 . . ? C10 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N5 C10 C9 108.5(5) . . ? N5 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? N5 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C11 N5 C10 114.7(5) . . ? C11 N5 Fe1 133.5(4) . . ? C10 N5 Fe1 111.7(4) . . ? N5 C11 C12 128.5(5) . . ? N5 C11 H11 115.8 . . ? C12 C11 H11 115.8 . . ? N6 C12 C13 123.1(5) . . ? N6 C12 C11 117.5(5) . . ? C13 C12 C11 119.4(5) . . ? C14 C13 C12 118.8(6) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 117.2(5) . . ? C13 C14 H14 121.4 . . ? C15 C14 H14 121.4 . . ? N7 C15 C14 121.9(5) . . ? N7 C15 C16 112.1(5) . . ? C14 C15 C16 126.0(5) . . ? N7 N6 C12 118.3(5) . . ? N6 N7 C15 120.5(5) . . ? N6 N7 Fe2 125.7(3) . . ? C15 N7 Fe2 113.5(4) . . ? N8 C16 C15 114.4(5) . . ? N8 C16 H16 122.8 . . ? C15 C16 H16 122.8 . . ? C16 N8 C17 123.1(5) . . ? C16 N8 Fe2 118.1(4) . . ? C17 N8 Fe2 118.7(4) . . ? N8 C17 C18 106.7(5) . . ? N8 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? N8 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? N9 C18 C17 111.2(5) . . ? N9 C18 H18A 109.4 . . ? C17 C18 H18A 109.4 . . ? N9 C18 H18B 109.4 . . ? C17 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C19 N9 C40 113.8(5) . . ? C19 N9 C18 112.7(5) . . ? C40 N9 C18 106.6(5) . . ? C19 N9 Fe2 108.8(4) . . ? C40 N9 Fe2 106.0(4) . . ? C18 N9 Fe2 108.6(3) . . ? C41 C40 N9 108.2(5) . . ? C41 C40 H40A 110.1 . . ? N9 C40 H40A 110.1 . . ? C41 C40 H40B 110.1 . . ? N9 C40 H40B 110.1 . . ? H40A C40 H40B 108.4 . . ? N40 C41 C42 120.8(6) . . ? N40 C41 C40 114.6(5) . . ? C42 C41 C40 124.7(6) . . ? C43 C42 C41 120.4(6) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 118.3(7) . . ? C42 C43 H43 120.8 . . ? C44 C43 H43 120.8 . . ? C45 C44 C43 118.8(7) . . ? C45 C44 H44 120.6 . . ? C43 C44 H44 120.6 . . ? N40 C45 C44 122.7(6) . . ? N40 C45 H45 118.7 . . ? C44 C45 H45 118.7 . . ? C45 N40 C41 119.0(5) . . ? C45 N40 Fe2 127.5(4) . . ? C41 N40 Fe2 113.5(4) . . ? N9 C19 C20 108.5(5) . . ? N9 C19 H19A 110.0 . . ? C20 C19 H19A 110.0 . . ? N9 C19 H19B 110.0 . . ? C20 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? N10 C20 C19 110.3(5) . . ? N10 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? N10 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C21 N10 C20 115.4(5) . . ? C21 N10 Fe2 134.9(4) . . ? C20 N10 Fe2 109.7(4) . . ? N10 C21 C2 126.9(6) . . ? N10 C21 H21 116.5 . . ? C2 C21 H21 116.5 . . ? C200 N200 Fe1 164.5(5) . . ? N200 C200 C201 177.6(6) . . ? C200 C201 H20A 109.5 . . ? C200 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C200 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C210 N210 Fe2 168.9(5) . . ? N210 C210 C211 178.2(7) . . ? C210 C211 H21A 109.5 . . ? C210 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C210 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? O14 Cl1 O13 110.6(4) . . ? O14 Cl1 O12 108.4(4) . . ? O13 Cl1 O12 107.2(4) . . ? O14 Cl1 O11 110.8(3) . . ? O13 Cl1 O11 110.5(3) . . ? O12 Cl1 O11 109.3(3) . . ? O23 Cl2 O21 117.0(5) . . ? O23 Cl2 O27 107.8(8) . . ? O21 Cl2 O27 131.8(7) . . ? O23 Cl2 O24 119.2(6) . . ? O21 Cl2 O24 108.8(4) . . ? O27 Cl2 O24 27.4(6) . . ? O23 Cl2 O25 47.1(6) . . ? O21 Cl2 O25 114.1(5) . . ? O27 Cl2 O25 108.8(8) . . ? O24 Cl2 O25 135.6(6) . . ? O23 Cl2 O22 106.7(7) . . ? O21 Cl2 O22 99.3(5) . . ? O27 Cl2 O22 83.4(9) . . ? O24 Cl2 O22 102.7(5) . . ? O25 Cl2 O22 60.4(6) . . ? O23 Cl2 O26 49.4(7) . . ? O21 Cl2 O26 98.0(6) . . ? O27 Cl2 O26 97.8(9) . . ? O24 Cl2 O26 88.0(6) . . ? O25 Cl2 O26 96.4(8) . . ? O22 Cl2 O26 155.4(8) . . ? 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 N2 -167.2(5) . . . . ? N200 Fe1 N1 N2 18.9(5) . . . . ? N5 Fe1 N1 N2 104.0(4) . . . . ? N30 Fe1 N1 N2 -70.8(5) . . . . ? N4 Fe1 N1 N2 -146.2(7) . . . . ? N3 Fe1 N1 C5 6.9(4) . . . . ? N200 Fe1 N1 C5 -167.0(4) . . . . ? N5 Fe1 N1 C5 -82.0(4) . . . . ? N30 Fe1 N1 C5 103.3(4) . . . . ? N4 Fe1 N1 C5 27.9(10) . . . . ? C5 N1 N2 C2 3.8(8) . . . . ? Fe1 N1 N2 C2 177.5(4) . . . . ? N1 N2 C2 C3 0.5(9) . . . . ? N1 N2 C2 C21 -175.1(5) . . . . ? N2 C2 C3 C4 -3.2(10) . . . . ? C21 C2 C3 C4 172.1(6) . . . . ? C2 C3 C4 C5 1.6(10) . . . . ? N2 N1 C5 C4 -5.5(9) . . . . ? Fe1 N1 C5 C4 -179.9(5) . . . . ? N2 N1 C5 C6 170.5(5) . . . . ? Fe1 N1 C5 C6 -4.0(6) . . . . ? C3 C4 C5 N1 2.6(10) . . . . ? C3 C4 C5 C6 -172.8(6) . . . . ? N1 C5 C6 N3 -3.3(8) . . . . ? C4 C5 C6 N3 172.5(6) . . . . ? C5 C6 N3 C7 179.8(5) . . . . ? C5 C6 N3 Fe1 9.5(7) . . . . ? N1 Fe1 N3 C6 -9.3(5) . . . . ? N200 Fe1 N3 C6 91(2) . . . . ? N5 Fe1 N3 C6 90.8(5) . . . . ? N30 Fe1 N3 C6 -102.3(5) . . . . ? N4 Fe1 N3 C6 176.1(5) . . . . ? N1 Fe1 N3 C7 179.8(5) . . . . ? N200 Fe1 N3 C7 -80(2) . . . . ? N5 Fe1 N3 C7 -80.2(5) . . . . ? N30 Fe1 N3 C7 86.8(5) . . . . ? N4 Fe1 N3 C7 5.1(5) . . . . ? C6 N3 C7 C8 163.5(6) . . . . ? Fe1 N3 C7 C8 -26.1(7) . . . . ? N3 C7 C8 N4 39.4(7) . . . . ? C7 C8 N4 C9 85.2(7) . . . . ? C7 C8 N4 C30 -150.8(6) . . . . ? C7 C8 N4 Fe1 -36.9(7) . . . . ? N3 Fe1 N4 C9 -106.6(4) . . . . ? N1 Fe1 N4 C9 -127.5(8) . . . . ? N200 Fe1 N4 C9 67.3(4) . . . . ? N5 Fe1 N4 C9 -15.8(4) . . . . ? N30 Fe1 N4 C9 155.6(4) . . . . ? N3 Fe1 N4 C30 132.0(4) . . . . ? N1 Fe1 N4 C30 111.2(8) . . . . ? N200 Fe1 N4 C30 -54.1(4) . . . . ? N5 Fe1 N4 C30 -137.2(4) . . . . ? N30 Fe1 N4 C30 34.2(4) . . . . ? N3 Fe1 N4 C8 17.7(4) . . . . ? N1 Fe1 N4 C8 -3.1(11) . . . . ? N200 Fe1 N4 C8 -168.4(4) . . . . ? N5 Fe1 N4 C8 108.6(4) . . . . ? N30 Fe1 N4 C8 -80.0(4) . . . . ? C9 N4 C30 C31 -161.6(5) . . . . ? C8 N4 C30 C31 73.7(6) . . . . ? Fe1 N4 C30 C31 -42.0(6) . . . . ? N4 C30 C31 N30 28.3(7) . . . . ? N4 C30 C31 C32 -154.4(6) . . . . ? N30 C31 C32 C33 -1.3(11) . . . . ? C30 C31 C32 C33 -178.5(7) . . . . ? C31 C32 C33 C34 1.3(13) . . . . ? C32 C33 C34 C35 -1.1(12) . . . . ? C33 C34 C35 N30 0.8(11) . . . . ? C34 C35 N30 C31 -0.8(9) . . . . ? C34 C35 N30 Fe1 177.8(5) . . . . ? C32 C31 N30 C35 1.0(9) . . . . ? C30 C31 N30 C35 178.5(6) . . . . ? C32 C31 N30 Fe1 -177.8(5) . . . . ? C30 C31 N30 Fe1 -0.4(7) . . . . ? N3 Fe1 N30 C35 77.7(5) . . . . ? N1 Fe1 N30 C35 -4.0(5) . . . . ? N200 Fe1 N30 C35 -103.7(5) . . . . ? N5 Fe1 N30 C35 -163.5(7) . . . . ? N4 Fe1 N30 C35 161.3(5) . . . . ? N3 Fe1 N30 C31 -103.6(4) . . . . ? N1 Fe1 N30 C31 174.7(4) . . . . ? N200 Fe1 N30 C31 75.0(4) . . . . ? N5 Fe1 N30 C31 15.2(10) . . . . ? N4 Fe1 N30 C31 -20.0(4) . . . . ? C30 N4 C9 C10 153.9(5) . . . . ? C8 N4 C9 C10 -85.3(6) . . . . ? Fe1 N4 C9 C10 36.4(6) . . . . ? N4 C9 C10 N5 -43.4(6) . . . . ? C9 C10 N5 C11 -146.8(5) . . . . ? C9 C10 N5 Fe1 30.4(6) . . . . ? N3 Fe1 N5 C11 -107.5(5) . . . . ? N1 Fe1 N5 C11 -26.3(5) . . . . ? N200 Fe1 N5 C11 72.6(5) . . . . ? N30 Fe1 N5 C11 133.0(7) . . . . ? N4 Fe1 N5 C11 168.0(5) . . . . ? N3 Fe1 N5 C10 76.0(4) . . . . ? N1 Fe1 N5 C10 157.2(4) . . . . ? N200 Fe1 N5 C10 -104.0(4) . . . . ? N30 Fe1 N5 C10 -43.6(9) . . . . ? N4 Fe1 N5 C10 -8.6(4) . . . . ? C10 N5 C11 C12 -179.0(5) . . . . ? Fe1 N5 C11 C12 4.5(9) . . . . ? N5 C11 C12 N6 -51.8(8) . . . . ? N5 C11 C12 C13 129.9(6) . . . . ? N6 C12 C13 C14 -2.3(9) . . . . ? C11 C12 C13 C14 175.8(6) . . . . ? C12 C13 C14 C15 -0.8(10) . . . . ? C13 C14 C15 N7 4.8(10) . . . . ? C13 C14 C15 C16 -173.6(6) . . . . ? C13 C12 N6 N7 1.4(8) . . . . ? C11 C12 N6 N7 -176.8(5) . . . . ? C12 N6 N7 C15 2.7(7) . . . . ? C12 N6 N7 Fe2 176.3(4) . . . . ? C14 C15 N7 N6 -5.9(8) . . . . ? C16 C15 N7 N6 172.7(5) . . . . ? C14 C15 N7 Fe2 179.8(5) . . . . ? C16 C15 N7 Fe2 -1.6(6) . . . . ? N8 Fe2 N7 N6 -171.0(5) . . . . ? N210 Fe2 N7 N6 14.3(5) . . . . ? N40 Fe2 N7 N6 -77.6(4) . . . . ? N10 Fe2 N7 N6 100.7(4) . . . . ? N9 Fe2 N7 N6 -148.8(7) . . . . ? N8 Fe2 N7 C15 3.0(4) . . . . ? N210 Fe2 N7 C15 -171.8(4) . . . . ? N40 Fe2 N7 C15 96.4(4) . . . . ? N10 Fe2 N7 C15 -85.3(4) . . . . ? N9 Fe2 N7 C15 25.1(10) . . . . ? N7 C15 C16 N8 -1.5(7) . . . . ? C14 C15 C16 N8 177.0(6) . . . . ? C15 C16 N8 C17 179.4(5) . . . . ? C15 C16 N8 Fe2 4.2(7) . . . . ? N7 Fe2 N8 C16 -4.1(4) . . . . ? N210 Fe2 N8 C16 107(2) . . . . ? N40 Fe2 N8 C16 -97.2(4) . . . . ? N10 Fe2 N8 C16 96.5(4) . . . . ? N9 Fe2 N8 C16 -178.8(4) . . . . ? N7 Fe2 N8 C17 -179.5(5) . . . . ? N210 Fe2 N8 C17 -69(2) . . . . ? N40 Fe2 N8 C17 87.4(4) . . . . ? N10 Fe2 N8 C17 -79.0(4) . . . . ? N9 Fe2 N8 C17 5.7(4) . . . . ? C16 N8 C17 C18 162.0(5) . . . . ? Fe2 N8 C17 C18 -22.9(6) . . . . ? N8 C17 C18 N9 32.9(7) . . . . ? C17 C18 N9 C19 91.4(6) . . . . ? C17 C18 N9 C40 -143.1(5) . . . . ? C17 C18 N9 Fe2 -29.3(6) . . . . ? N8 Fe2 N9 C19 -109.6(4) . . . . ? N7 Fe2 N9 C19 -131.6(8) . . . . ? N210 Fe2 N9 C19 65.1(4) . . . . ? N40 Fe2 N9 C19 155.8(4) . . . . ? N10 Fe2 N9 C19 -19.3(4) . . . . ? N8 Fe2 N9 C40 127.7(4) . . . . ? N7 Fe2 N9 C40 105.7(8) . . . . ? N210 Fe2 N9 C40 -57.6(4) . . . . ? N40 Fe2 N9 C40 33.0(4) . . . . ? N10 Fe2 N9 C40 -142.1(4) . . . . ? N8 Fe2 N9 C18 13.5(4) . . . . ? N7 Fe2 N9 C18 -8.5(11) . . . . ? N210 Fe2 N9 C18 -171.8(4) . . . . ? N40 Fe2 N9 C18 -81.1(4) . . . . ? N10 Fe2 N9 C18 103.7(4) . . . . ? C19 N9 C40 C41 -160.9(5) . . . . ? C18 N9 C40 C41 74.2(6) . . . . ? Fe2 N9 C40 C41 -41.4(5) . . . . ? N9 C40 C41 N40 28.5(7) . . . . ? N9 C40 C41 C42 -151.0(6) . . . . ? N40 C41 C42 C43 -0.6(9) . . . . ? C40 C41 C42 C43 178.8(6) . . . . ? C41 C42 C43 C44 0.0(10) . . . . ? C42 C43 C44 C45 0.7(10) . . . . ? C43 C44 C45 N40 -0.8(10) . . . . ? C44 C45 N40 C41 0.2(9) . . . . ? C44 C45 N40 Fe2 -177.6(5) . . . . ? C42 C41 N40 C45 0.6(8) . . . . ? C40 C41 N40 C45 -178.9(5) . . . . ? C42 C41 N40 Fe2 178.6(4) . . . . ? C40 C41 N40 Fe2 -0.9(6) . . . . ? N8 Fe2 N40 C45 74.2(5) . . . . ? N7 Fe2 N40 C45 -7.8(5) . . . . ? N210 Fe2 N40 C45 -108.0(5) . . . . ? N10 Fe2 N40 C45 179(58) . . . . ? N9 Fe2 N40 C45 158.9(5) . . . . ? N8 Fe2 N40 C41 -103.7(4) . . . . ? N7 Fe2 N40 C41 174.3(4) . . . . ? N210 Fe2 N40 C41 74.1(4) . . . . ? N10 Fe2 N40 C41 1.2(10) . . . . ? N9 Fe2 N40 C41 -19.0(4) . . . . ? C40 N9 C19 C20 158.3(5) . . . . ? C18 N9 C19 C20 -80.3(6) . . . . ? Fe2 N9 C19 C20 40.3(6) . . . . ? N9 C19 C20 N10 -46.4(7) . . . . ? C19 C20 N10 C21 -151.5(5) . . . . ? C19 C20 N10 Fe2 29.8(6) . . . . ? N8 Fe2 N10 C21 -98.9(6) . . . . ? N7 Fe2 N10 C21 -17.4(6) . . . . ? N210 Fe2 N10 C21 82.0(6) . . . . ? N40 Fe2 N10 C21 155.7(7) . . . . ? N9 Fe2 N10 C21 175.7(6) . . . . ? N8 Fe2 N10 C20 79.5(4) . . . . ? N7 Fe2 N10 C20 161.0(4) . . . . ? N210 Fe2 N10 C20 -99.6(4) . . . . ? N40 Fe2 N10 C20 -25.9(10) . . . . ? N9 Fe2 N10 C20 -5.9(4) . . . . ? C20 N10 C21 C2 177.0(6) . . . . ? Fe2 N10 C21 C2 -4.7(10) . . . . ? N2 C2 C21 N10 -50.0(9) . . . . ? C3 C2 C21 N10 134.3(7) . . . . ? N3 Fe1 N200 C200 -6(3) . . . . ? N1 Fe1 N200 C200 93.0(19) . . . . ? N5 Fe1 N200 C200 -6.1(19) . . . . ? N30 Fe1 N200 C200 -173.1(19) . . . . ? N4 Fe1 N200 C200 -90.9(19) . . . . ? Fe1 N200 C200 C201 -37(18) . . . . ? N8 Fe2 N210 C210 -10(4) . . . . ? N7 Fe2 N210 C210 100(2) . . . . ? N40 Fe2 N210 C210 -166(2) . . . . ? N10 Fe2 N210 C210 0(2) . . . . ? N9 Fe2 N210 C210 -84(2) . . . . ? Fe2 N210 C210 C211 -91(23) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.62 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.803 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.106 data_mw64 _database_code_depnum_ccdc_archive 'CCDC 269197' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H50.50 Cl4 Mn2 N14.50 O17.50' _chemical_formula_weight 1254.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.9488(2) _cell_length_b 13.7829(2) _cell_length_c 22.1623(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.9540(10) _cell_angle_gamma 90.00 _cell_volume 5296.97(12) _cell_formula_units_Z 4 _cell_measurement_temperature 84(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 0.762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 84(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 SMART area detector' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29250 _diffrn_reflns_av_R_equivalents 0.0819 _diffrn_reflns_av_sigmaI/netI 0.1015 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.64 _reflns_number_total 9923 _reflns_number_gt 6038 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. Half occupancy diethylether molecule shares two carbon atoms (C233 and C234) with half occupancy acetonitrile molecule (N230). The latter is restrained by SAME to have similar bond lengths and angles to the full occupancy MeCN of solvation. The two hydrogen atoms on the coordinated water molecule were found from a difference map and their coordinates allowed to freely refine. All other hydrogen atoms were inserted at calculated positions and rode on the atoms to which they were attached. All hydrogen atoms had U(iso)=1.2 times that of the attached non-H atom. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+9.2919P] 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 9923 _refine_ls_number_parameters 722 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1307 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.1855 _refine_ls_wR_factor_gt 0.1569 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.035 _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 0.45308(5) 0.18833(6) 0.72531(4) 0.0238(2) Uani 1 1 d . . . Mn2 Mn 0.53702(5) 0.49879(6) 0.74122(4) 0.0226(2) Uani 1 1 d . . . N1 N 0.5809(2) 0.2653(3) 0.7899(2) 0.0252(11) Uani 1 1 d . . . N2 N 0.6097(2) 0.3555(3) 0.7868(2) 0.0220(10) Uani 1 1 d . . . C2 C 0.6815(3) 0.3756(4) 0.8193(3) 0.0233(12) Uani 1 1 d . . . C3 C 0.7294(3) 0.3082(4) 0.8587(3) 0.0263(13) Uani 1 1 d . . . H3 H 0.7801 0.3250 0.8816 0.032 Uiso 1 1 calc R . . C4 C 0.6998(3) 0.2174(4) 0.8627(3) 0.0252(13) Uani 1 1 d . . . H4 H 0.7294 0.1687 0.8885 0.030 Uiso 1 1 calc R . . C5 C 0.6251(3) 0.1992(4) 0.8278(3) 0.0228(12) Uani 1 1 d . . . C6 C 0.5885(3) 0.1030(4) 0.8292(3) 0.0240(13) Uani 1 1 d . . . H6 H 0.6150 0.0543 0.8568 0.029 Uiso 1 1 calc R . . N3 N 0.5224(2) 0.0849(3) 0.7941(2) 0.0220(10) Uani 1 1 d . . . C7 C 0.4891(3) -0.0128(4) 0.7937(3) 0.0264(13) Uani 1 1 d . . . H7A H 0.4470 -0.0118 0.8150 0.032 Uiso 1 1 calc R . . H7B H 0.5291 -0.0589 0.8159 0.032 Uiso 1 1 calc R . . C8 C 0.4581(3) -0.0439(4) 0.7261(3) 0.0260(13) Uani 1 1 d . . . H8A H 0.5022 -0.0596 0.7087 0.031 Uiso 1 1 calc R . . H8B H 0.4276 -0.1040 0.7251 0.031 Uiso 1 1 calc R . . N4 N 0.4088(2) 0.0299(3) 0.6849(2) 0.0243(11) Uani 1 1 d . . . C30 C 0.4193(3) 0.0248(4) 0.6216(3) 0.0266(13) Uani 1 1 d . . . H30A H 0.3778 0.0620 0.5929 0.032 Uiso 1 1 calc R . . H30B H 0.4152 -0.0436 0.6076 0.032 Uiso 1 1 calc R . . C31 C 0.4961(3) 0.0646(4) 0.6187(3) 0.0251(13) Uani 1 1 d . . . C32 C 0.5395(3) 0.0249(4) 0.5814(3) 0.0309(14) Uani 1 1 d . . . H32 H 0.5230 -0.0336 0.5594 0.037 Uiso 1 1 calc R . . C33 C 0.6063(3) 0.0691(4) 0.5757(3) 0.0280(13) Uani 1 1 d . . . H33 H 0.6355 0.0424 0.5495 0.034 Uiso 1 1 calc R . . C34 C 0.6300(3) 0.1543(4) 0.6095(3) 0.0295(14) Uani 1 1 d . . . H34 H 0.6749 0.1877 0.6060 0.035 Uiso 1 1 calc R . . C35 C 0.5865(3) 0.1891(4) 0.6484(3) 0.0254(13) Uani 1 1 d . . . H35 H 0.6039 0.2455 0.6725 0.030 Uiso 1 1 calc R . . N30 N 0.5207(3) 0.1465(3) 0.6536(2) 0.0254(11) Uani 1 1 d . . . C9 C 0.3260(3) 0.0208(4) 0.6836(3) 0.0286(14) Uani 1 1 d . . . H9A H 0.3095 -0.0474 0.6746 0.034 Uiso 1 1 calc R . . H9B H 0.2950 0.0618 0.6496 0.034 Uiso 1 1 calc R . . C10 C 0.3109(3) 0.0515(4) 0.7453(3) 0.0297(14) Uani 1 1 d . . . H10A H 0.2548 0.0582 0.7407 0.036 Uiso 1 1 calc R . . H10B H 0.3315 0.0023 0.7779 0.036 Uiso 1 1 calc R . . N5 N 0.3500(3) 0.1456(3) 0.7630(2) 0.0258(11) Uani 1 1 d . . . C11 C 0.3301(3) 0.1979(4) 0.8034(3) 0.0298(14) Uani 1 1 d . . . H11 H 0.2917 0.1755 0.8226 0.036 Uiso 1 1 calc R . . N6 N 0.4176(3) 0.3209(3) 0.7888(2) 0.0266(11) Uani 1 1 d . . . N7 N 0.4513(3) 0.4096(3) 0.7998(2) 0.0257(11) Uani 1 1 d . . . C12 C 0.3664(3) 0.2935(4) 0.8206(3) 0.0248(13) Uani 1 1 d . . . C13 C 0.3476(3) 0.3498(4) 0.8660(3) 0.0304(14) Uani 1 1 d . . . H13 H 0.3116 0.3281 0.8878 0.036 Uiso 1 1 calc R . . C14 C 0.3835(4) 0.4396(4) 0.8786(3) 0.0330(14) Uani 1 1 d . . . H14 H 0.3730 0.4815 0.9095 0.040 Uiso 1 1 calc R . . C15 C 0.4347(3) 0.4655(4) 0.8450(3) 0.0276(13) Uani 1 1 d . . . C16 C 0.4745(3) 0.5610(4) 0.8545(3) 0.0299(14) Uani 1 1 d . . . H16 H 0.4667 0.6038 0.8859 0.036 Uiso 1 1 calc R . . N8 N 0.5184(3) 0.5854(3) 0.8210(2) 0.0253(11) Uani 1 1 d . . . C17 C 0.5530(3) 0.6836(4) 0.8276(3) 0.0282(13) Uani 1 1 d . . . H17A H 0.6094 0.6797 0.8458 0.034 Uiso 1 1 calc R . . H17B H 0.5303 0.7241 0.8553 0.034 Uiso 1 1 calc R . . C18 C 0.5350(3) 0.7270(4) 0.7618(3) 0.0265(13) Uani 1 1 d . . . H18A H 0.4790 0.7408 0.7479 0.032 Uiso 1 1 calc R . . H18B H 0.5626 0.7895 0.7637 0.032 Uiso 1 1 calc R . . N9 N 0.5565(2) 0.6636(3) 0.7142(2) 0.0232(10) Uani 1 1 d . . . C40 C 0.5047(3) 0.6825(4) 0.6518(3) 0.0273(13) Uani 1 1 d . . . H40A H 0.5283 0.6560 0.6196 0.033 Uiso 1 1 calc R . . H40B H 0.4992 0.7535 0.6453 0.033 Uiso 1 1 calc R . . C41 C 0.4258(3) 0.6382(4) 0.6436(3) 0.0298(14) Uani 1 1 d . . . C42 C 0.3619(3) 0.6741(5) 0.6004(3) 0.0351(15) Uani 1 1 d . . . H42 H 0.3662 0.7316 0.5779 0.042 Uiso 1 1 calc R . . C43 C 0.2912(4) 0.6264(5) 0.5899(3) 0.0434(17) Uani 1 1 d . . . H43 H 0.2468 0.6500 0.5601 0.052 Uiso 1 1 calc R . . C44 C 0.2877(3) 0.5419(5) 0.6248(3) 0.0375(16) Uani 1 1 d . . . H44 H 0.2409 0.5067 0.6186 0.045 Uiso 1 1 calc R . . C45 C 0.3523(3) 0.5115(4) 0.6674(3) 0.0299(14) Uani 1 1 d . . . H45 H 0.3481 0.4560 0.6918 0.036 Uiso 1 1 calc R . . N40 N 0.4221(3) 0.5548(3) 0.6777(2) 0.0276(11) Uani 1 1 d . . . C19 C 0.6385(3) 0.6761(4) 0.7115(3) 0.0258(13) Uani 1 1 d . . . H19A H 0.6498 0.7461 0.7094 0.031 Uiso 1 1 calc R . . H19B H 0.6455 0.6450 0.6730 0.031 Uiso 1 1 calc R . . C20 C 0.6945(3) 0.6320(4) 0.7676(3) 0.0273(13) Uani 1 1 d . . . H20A H 0.7462 0.6264 0.7599 0.033 Uiso 1 1 calc R . . H20B H 0.6986 0.6734 0.8048 0.033 Uiso 1 1 calc R . . N10 N 0.6649(3) 0.5341(3) 0.7780(2) 0.0244(11) Uani 1 1 d . . . C21 C 0.7110(3) 0.4744(4) 0.8110(3) 0.0233(13) Uani 1 1 d . . . H21 H 0.7629 0.4918 0.8301 0.028 Uiso 1 1 calc R . . N200 N 0.5560(3) 0.4473(3) 0.6517(2) 0.0264(11) Uani 1 1 d . . . C200 C 0.5764(4) 0.4376(5) 0.6070(4) 0.0453(18) Uani 1 1 d . . . C201 C 0.6039(5) 0.4203(6) 0.5493(4) 0.059(2) Uani 1 1 d . . . H20C H 0.6507 0.3806 0.5600 0.071 Uiso 1 1 calc R . . H20D H 0.6150 0.4826 0.5323 0.071 Uiso 1 1 calc R . . H20E H 0.5637 0.3863 0.5181 0.071 Uiso 1 1 calc R . . O210 O 0.3738(3) 0.2611(3) 0.6492(2) 0.0368(11) Uani 1 1 d . . . H21A H 0.382(4) 0.278(5) 0.617(3) 0.044 Uiso 1 1 d . . . H21B H 0.328(4) 0.278(5) 0.649(3) 0.044 Uiso 1 1 d . . . Cl1 Cl 0.41360(10) 0.26290(15) 0.49199(8) 0.0516(5) Uani 1 1 d . . . O12 O 0.3723(2) 0.3233(4) 0.4406(2) 0.0532(14) Uani 1 1 d . . . O11 O 0.4266(3) 0.3210(4) 0.5470(3) 0.0626(15) Uani 1 1 d . . . O13 O 0.4867(3) 0.2340(4) 0.4824(3) 0.0645(15) Uani 1 1 d . . . O14 O 0.3682(3) 0.1771(4) 0.4973(3) 0.0675(16) Uani 1 1 d . . . Cl2 Cl 0.17180(8) 0.27698(10) 0.68623(7) 0.0319(4) Uani 1 1 d . . . O24 O 0.1018(2) 0.3233(3) 0.6513(2) 0.0469(12) Uani 1 1 d . . . O22 O 0.1725(3) 0.2734(4) 0.7511(2) 0.0480(12) Uani 1 1 d . . . O23 O 0.1762(3) 0.1794(3) 0.6632(2) 0.0457(12) Uani 1 1 d . . . O21 O 0.2384(2) 0.3312(3) 0.6793(2) 0.0483(13) Uani 1 1 d . . . Cl3 Cl 0.29998(9) 0.39492(13) 0.01825(7) 0.0404(4) Uani 1 1 d . . . O31 O 0.2910(3) 0.4377(4) 0.0733(2) 0.0643(16) Uani 1 1 d . . . O32 O 0.3797(3) 0.3869(4) 0.0194(2) 0.0620(15) Uani 1 1 d . . . O33 O 0.2595(4) 0.4425(7) -0.0353(3) 0.119(3) Uani 1 1 d . . . O34 O 0.2687(5) 0.2980(6) 0.0160(5) 0.141(4) Uani 1 1 d . . . Cl4 Cl 0.28556(8) 0.08796(9) 0.18603(7) 0.0286(3) Uani 1 1 d . . . O41 O 0.3398(2) 0.0686(3) 0.2450(2) 0.0369(10) Uani 1 1 d . . . O42 O 0.2289(2) 0.1567(3) 0.1950(2) 0.0404(11) Uani 1 1 d . . . O43 O 0.2474(2) -0.0016(3) 0.1610(2) 0.0338(10) Uani 1 1 d . . . O44 O 0.3261(2) 0.1271(3) 0.1429(2) 0.0378(11) Uani 1 1 d . . . N220 N 0.9150(4) 0.4207(6) 0.4167(3) 0.069(2) Uani 1 1 d D . . C220 C 0.9320(4) 0.3912(5) 0.4670(3) 0.0435(17) Uani 1 1 d D . . C221 C 0.9518(6) 0.3520(7) 0.5286(4) 0.083(3) Uani 1 1 d D . . H22A H 0.9183 0.3803 0.5526 0.100 Uiso 1 1 calc R . . H22B H 1.0057 0.3674 0.5490 0.100 Uiso 1 1 calc R . . H22C H 0.9449 0.2814 0.5265 0.100 Uiso 1 1 calc R . . C230 C 0.7894(13) 0.5516(12) 0.5159(8) 0.077(6) Uani 0.50 1 d P A 1 H23A H 0.8183 0.5479 0.5599 0.093 Uiso 0.50 1 calc PR A 1 H23B H 0.8055 0.4987 0.4926 0.093 Uiso 0.50 1 calc PR A 1 H23C H 0.7341 0.5457 0.5128 0.093 Uiso 0.50 1 calc PR A 1 C231 C 0.8050(15) 0.648(3) 0.4889(9) 0.149(14) Uani 0.50 1 d P A 1 H23D H 0.8169 0.6350 0.4484 0.179 Uiso 0.50 1 calc PR A 1 H23E H 0.7570 0.6864 0.4802 0.179 Uiso 0.50 1 calc PR A 1 O232 O 0.8655(8) 0.7048(10) 0.5260(6) 0.087(4) Uani 0.50 1 d P A 1 N230 N 0.8071(8) 0.8118(19) 0.4846(7) 0.113(9) Uani 0.50 1 d PD A 2 C233 C 0.8729(8) 0.8102(8) 0.5170(7) 0.133(6) Uani 1 1 d D . . H23F H 0.8740 0.8268 0.4738 0.160 Uiso 0.50 1 calc PR A 1 H23G H 0.8320 0.8480 0.5291 0.160 Uiso 0.50 1 calc PR A 1 C234 C 0.9428(6) 0.8207(10) 0.5584(5) 0.124(6) Uani 1 1 d D A . H23H H 0.9556 0.8898 0.5639 0.149 Uiso 0.50 1 calc PR B 1 H23I H 0.9820 0.7873 0.5425 0.149 Uiso 0.50 1 calc PR B 1 H23J H 0.9412 0.7924 0.5986 0.149 Uiso 0.50 1 calc PR B 1 H23K H 0.9655 0.7566 0.5701 0.149 Uiso 0.50 1 calc PR B 2 H23L H 0.9365 0.8543 0.5957 0.149 Uiso 0.50 1 calc PR B 2 H23M H 0.9767 0.8586 0.5391 0.149 Uiso 0.50 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0258(5) 0.0101(4) 0.0382(5) -0.0022(4) 0.0130(4) 0.0008(4) Mn2 0.0245(4) 0.0109(4) 0.0342(5) -0.0029(4) 0.0109(4) 0.0001(4) N1 0.023(2) 0.016(2) 0.039(3) -0.007(2) 0.014(2) -0.002(2) N2 0.025(2) 0.011(2) 0.033(3) -0.007(2) 0.014(2) -0.0017(19) C2 0.021(3) 0.019(3) 0.032(3) -0.008(3) 0.011(2) 0.003(2) C3 0.019(3) 0.025(3) 0.035(3) -0.007(3) 0.007(2) -0.002(2) C4 0.023(3) 0.021(3) 0.033(3) -0.005(3) 0.009(2) 0.002(2) C5 0.020(3) 0.012(3) 0.038(3) -0.006(3) 0.011(2) 0.001(2) C6 0.030(3) 0.011(3) 0.035(3) -0.004(2) 0.015(3) 0.002(2) N3 0.021(2) 0.011(2) 0.036(3) -0.004(2) 0.011(2) -0.0046(19) C7 0.025(3) 0.013(3) 0.041(4) 0.005(3) 0.010(3) -0.001(2) C8 0.026(3) 0.009(3) 0.045(4) -0.003(3) 0.013(3) -0.002(2) N4 0.021(2) 0.017(2) 0.034(3) -0.003(2) 0.007(2) -0.0021(19) C30 0.032(3) 0.011(3) 0.036(3) -0.005(2) 0.008(3) 0.003(2) C31 0.026(3) 0.016(3) 0.033(3) -0.002(3) 0.006(3) 0.000(2) C32 0.035(3) 0.022(3) 0.034(3) -0.002(3) 0.004(3) 0.008(3) C33 0.029(3) 0.027(3) 0.031(3) -0.001(3) 0.012(3) 0.007(3) C34 0.026(3) 0.027(3) 0.034(3) -0.004(3) 0.006(3) -0.002(3) C35 0.025(3) 0.013(3) 0.038(3) -0.003(3) 0.008(3) -0.001(2) N30 0.026(2) 0.015(2) 0.038(3) -0.002(2) 0.012(2) 0.002(2) C9 0.025(3) 0.017(3) 0.044(4) -0.004(3) 0.010(3) -0.003(2) C10 0.027(3) 0.016(3) 0.045(4) -0.002(3) 0.009(3) -0.004(2) N5 0.025(3) 0.015(2) 0.039(3) 0.000(2) 0.012(2) 0.001(2) C11 0.023(3) 0.023(3) 0.049(4) 0.005(3) 0.020(3) 0.003(3) N6 0.027(3) 0.016(2) 0.039(3) -0.002(2) 0.012(2) 0.003(2) N7 0.027(3) 0.015(2) 0.037(3) 0.000(2) 0.011(2) 0.000(2) C12 0.027(3) 0.012(3) 0.040(3) 0.001(2) 0.017(3) 0.004(2) C13 0.031(3) 0.022(3) 0.043(4) -0.001(3) 0.020(3) 0.000(3) C14 0.041(4) 0.022(3) 0.042(4) -0.002(3) 0.022(3) 0.002(3) C15 0.035(3) 0.014(3) 0.039(4) 0.000(3) 0.021(3) 0.001(2) C16 0.038(3) 0.015(3) 0.040(4) 0.000(3) 0.015(3) 0.002(3) N8 0.036(3) 0.011(2) 0.033(3) 0.001(2) 0.017(2) -0.001(2) C17 0.039(3) 0.010(3) 0.036(3) -0.007(3) 0.011(3) -0.003(2) C18 0.030(3) 0.009(3) 0.043(4) -0.005(3) 0.013(3) -0.004(2) N9 0.026(2) 0.013(2) 0.035(3) -0.004(2) 0.015(2) -0.0034(19) C40 0.032(3) 0.018(3) 0.035(3) 0.003(3) 0.014(3) -0.001(3) C41 0.032(3) 0.025(3) 0.038(4) 0.000(3) 0.020(3) 0.001(3) C42 0.032(3) 0.030(4) 0.044(4) 0.012(3) 0.011(3) 0.004(3) C43 0.033(4) 0.043(4) 0.054(4) 0.019(4) 0.010(3) 0.007(3) C44 0.022(3) 0.040(4) 0.050(4) 0.008(3) 0.009(3) -0.005(3) C45 0.026(3) 0.026(3) 0.040(4) 0.009(3) 0.013(3) 0.000(3) N40 0.028(3) 0.022(3) 0.037(3) 0.001(2) 0.015(2) -0.001(2) C19 0.028(3) 0.018(3) 0.035(3) -0.003(3) 0.015(3) -0.003(2) C20 0.027(3) 0.012(3) 0.046(4) -0.007(3) 0.016(3) -0.010(2) N10 0.029(3) 0.011(2) 0.037(3) -0.003(2) 0.015(2) -0.001(2) C21 0.022(3) 0.016(3) 0.034(3) -0.008(3) 0.010(2) -0.002(2) N200 0.026(3) 0.026(3) 0.030(3) -0.005(2) 0.012(2) 0.004(2) C200 0.046(4) 0.025(4) 0.060(5) 0.000(4) 0.006(4) 0.000(3) C201 0.068(5) 0.052(5) 0.058(5) -0.007(4) 0.018(4) 0.003(4) O210 0.033(2) 0.039(3) 0.042(3) 0.005(2) 0.017(2) 0.016(2) Cl1 0.0392(9) 0.0735(13) 0.0414(10) 0.0157(10) 0.0092(8) -0.0034(9) O12 0.032(2) 0.074(4) 0.050(3) 0.031(3) 0.004(2) 0.004(2) O11 0.037(3) 0.061(4) 0.079(4) 0.007(3) -0.005(3) -0.013(3) O13 0.041(3) 0.084(4) 0.069(4) 0.019(3) 0.015(3) 0.006(3) O14 0.073(4) 0.065(4) 0.066(4) 0.017(3) 0.020(3) -0.026(3) Cl2 0.0285(7) 0.0220(8) 0.0483(9) -0.0006(7) 0.0158(7) 0.0053(6) O24 0.034(2) 0.042(3) 0.063(3) 0.007(2) 0.011(2) 0.012(2) O22 0.044(3) 0.059(3) 0.047(3) -0.002(3) 0.022(2) 0.012(2) O23 0.046(3) 0.020(2) 0.070(3) -0.011(2) 0.014(2) 0.003(2) O21 0.037(3) 0.027(2) 0.090(4) 0.009(3) 0.034(3) 0.001(2) Cl3 0.0419(9) 0.0486(10) 0.0327(9) -0.0021(8) 0.0130(7) 0.0031(8) O31 0.057(3) 0.092(4) 0.050(3) -0.024(3) 0.026(3) -0.001(3) O32 0.043(3) 0.092(4) 0.057(3) 0.015(3) 0.023(3) 0.019(3) O33 0.086(4) 0.229(9) 0.052(4) 0.057(5) 0.037(3) 0.105(6) O34 0.120(6) 0.081(5) 0.233(10) -0.064(6) 0.068(7) -0.049(5) Cl4 0.0333(8) 0.0115(7) 0.0436(9) -0.0004(6) 0.0145(7) -0.0018(6) O41 0.038(2) 0.030(2) 0.041(3) 0.006(2) 0.008(2) -0.006(2) O42 0.046(3) 0.016(2) 0.067(3) 0.000(2) 0.028(2) 0.0072(19) O43 0.035(2) 0.013(2) 0.054(3) -0.009(2) 0.012(2) -0.0050(18) O44 0.044(3) 0.027(2) 0.047(3) 0.007(2) 0.021(2) -0.005(2) N220 0.052(4) 0.105(6) 0.049(4) 0.013(4) 0.010(3) -0.008(4) C220 0.042(4) 0.042(4) 0.042(4) 0.005(3) 0.002(3) -0.010(3) C221 0.115(8) 0.078(7) 0.046(5) 0.015(5) 0.001(5) -0.019(6) C230 0.135(17) 0.042(10) 0.049(10) -0.029(9) 0.012(11) -0.012(11) C231 0.13(2) 0.28(4) 0.047(12) -0.066(19) 0.035(13) -0.11(2) O232 0.095(10) 0.082(10) 0.091(10) -0.010(8) 0.037(8) -0.010(8) N230 0.049(9) 0.22(3) 0.056(10) 0.033(13) -0.013(8) -0.021(13) C233 0.210(17) 0.060(7) 0.194(17) -0.001(9) 0.168(15) -0.035(10) C234 0.097(8) 0.189(14) 0.111(9) -0.086(9) 0.071(7) -0.086(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O210 2.153(5) . y Mn1 N3 2.219(5) . y Mn1 N5 2.295(5) . y Mn1 N30 2.309(5) . y Mn1 N4 2.416(4) . y Mn1 N6 2.487(5) . y Mn1 N1 2.597(4) . y Mn2 N200 2.215(5) . y Mn2 N8 2.229(5) . y Mn2 N10 2.281(5) . y Mn2 N40 2.310(5) . y Mn2 N9 2.398(4) . y Mn2 N2 2.439(4) . y Mn2 N7 2.568(5) . y N1 C5 1.348(7) . ? N1 N2 1.355(6) . ? N2 C2 1.332(7) . ? C2 C3 1.405(8) . ? C2 C21 1.490(8) . ? C3 C4 1.371(8) . ? C3 H3 0.9500 . ? C4 C5 1.388(7) . ? C4 H4 0.9500 . ? C5 C6 1.484(7) . ? C6 N3 1.264(7) . ? C6 H6 0.9500 . ? N3 C7 1.472(6) . ? C7 C8 1.519(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N4 1.495(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N4 C30 1.465(7) . ? N4 C9 1.484(7) . ? C30 C31 1.501(8) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N30 1.375(7) . ? C31 C32 1.387(8) . ? C32 C33 1.379(8) . ? C32 H32 0.9500 . ? C33 C34 1.399(8) . ? C33 H33 0.9500 . ? C34 C35 1.388(8) . ? C34 H34 0.9500 . ? C35 N30 1.350(7) . ? C35 H35 0.9500 . ? C9 C10 1.522(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N5 1.477(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? N5 C11 1.271(7) . ? C11 C12 1.475(8) . ? C11 H11 0.9500 . ? N6 C12 1.349(7) . ? N6 N7 1.358(6) . ? N7 C15 1.357(7) . ? C12 C13 1.381(8) . ? C13 C14 1.390(8) . ? C13 H13 0.9500 . ? C14 C15 1.371(8) . ? C14 H14 0.9500 . ? C15 C16 1.485(8) . ? C16 N8 1.260(7) . ? C16 H16 0.9500 . ? N8 C17 1.479(7) . ? C17 C18 1.533(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N9 1.494(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? N9 C40 1.477(7) . ? N9 C19 1.497(7) . ? C40 C41 1.511(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.382(8) . ? C41 N40 1.385(7) . ? C42 C43 1.396(9) . ? C42 H42 0.9500 . ? C43 C44 1.408(9) . ? C43 H43 0.9500 . ? C44 C45 1.360(8) . ? C44 H44 0.9500 . ? C45 N40 1.352(7) . ? C45 H45 0.9500 . ? C19 C20 1.510(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N10 1.489(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N10 C21 1.259(7) . ? C21 H21 0.9500 . ? N200 C200 1.150(8) . ? C200 C201 1.502(11) . ? C201 H20C 0.9800 . ? C201 H20D 0.9800 . ? C201 H20E 0.9800 . ? O210 H21A 0.80(7) . ? O210 H21B 0.85(7) . ? Cl1 O11 1.428(6) . ? Cl1 O13 1.437(5) . ? Cl1 O12 1.450(5) . ? Cl1 O14 1.457(5) . ? Cl2 O22 1.435(5) . ? Cl2 O24 1.443(4) . ? Cl2 O23 1.447(4) . ? Cl2 O21 1.451(4) . ? Cl3 O33 1.386(6) . ? Cl3 O31 1.402(5) . ? Cl3 O32 1.429(5) . ? Cl3 O34 1.445(7) . ? Cl4 O41 1.439(4) . ? Cl4 O42 1.440(4) . ? Cl4 O44 1.447(4) . ? Cl4 O43 1.452(4) . ? N220 C220 1.150(8) . ? C220 C221 1.426(10) . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? C230 C231 1.51(3) . ? C230 H23A 0.9800 . ? C230 H23B 0.9800 . ? C230 H23C 0.9800 . ? C231 O232 1.42(2) . ? C231 H23D 0.9900 . ? C231 H23E 0.9900 . ? O232 C233 1.478(16) . ? N230 C233 1.214(14) . ? C233 C234 1.357(14) . ? C233 H23F 0.9900 . ? C233 H23G 0.9900 . ? C234 H23H 0.9800 . ? C234 H23I 0.9800 . ? C234 H23J 0.9800 . ? C234 H23K 0.9800 . ? C234 H23L 0.9800 . ? C234 H23M 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 O210 Mn1 N3 167.72(17) . . y O210 Mn1 N5 88.47(18) . . y N3 Mn1 N5 86.95(16) . . y O210 Mn1 N30 86.26(17) . . y N3 Mn1 N30 90.65(16) . . y N5 Mn1 N30 143.42(17) . . y O210 Mn1 N4 92.45(17) . . y N3 Mn1 N4 75.29(16) . . y N5 Mn1 N4 71.55(16) . . y N30 Mn1 N4 72.56(16) . . y O210 Mn1 N6 83.54(17) . . y N3 Mn1 N6 105.30(16) . . y N5 Mn1 N6 68.58(16) . . y N30 Mn1 N6 146.08(16) . . y N4 Mn1 N6 140.00(15) . . y O210 Mn1 N1 123.57(17) . . y N3 Mn1 N1 67.97(15) . . y N5 Mn1 N1 125.80(16) . . y N30 Mn1 N1 86.27(15) . . y N4 Mn1 N1 137.13(15) . . y N6 Mn1 N1 72.95(14) . . y N200 Mn2 N8 166.27(17) . . y N200 Mn2 N10 90.88(17) . . y N8 Mn2 N10 86.82(17) . . y N200 Mn2 N40 83.17(17) . . y N8 Mn2 N40 90.66(17) . . y N10 Mn2 N40 143.56(17) . . y N200 Mn2 N9 90.79(17) . . y N8 Mn2 N9 75.63(16) . . y N10 Mn2 N9 71.86(16) . . y N40 Mn2 N9 72.32(16) . . y N200 Mn2 N2 85.54(16) . . y N8 Mn2 N2 106.17(16) . . y N10 Mn2 N2 69.11(15) . . y N40 Mn2 N2 145.26(16) . . y N9 Mn2 N2 140.71(15) . . y N200 Mn2 N7 123.40(17) . . y N8 Mn2 N7 67.88(16) . . y N10 Mn2 N7 126.88(16) . . y N40 Mn2 N7 84.87(16) . . y N9 Mn2 N7 136.44(15) . . y N2 Mn2 N7 74.28(14) . . y C5 N1 N2 118.7(4) . . ? C5 N1 Mn1 111.2(3) . . ? N2 N1 Mn1 129.9(3) . . ? C2 N2 N1 119.5(5) . . ? C2 N2 Mn2 113.3(3) . . ? N1 N2 Mn2 126.4(3) . . ? N2 C2 C3 123.3(5) . . ? N2 C2 C21 116.6(5) . . ? C3 C2 C21 120.0(5) . . ? C4 C3 C2 117.3(5) . . ? C4 C3 H3 121.4 . . ? C2 C3 H3 121.4 . . ? C3 C4 C5 117.6(5) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? N1 C5 C4 123.6(5) . . ? N1 C5 C6 115.1(5) . . ? C4 C5 C6 121.3(5) . . ? N3 C6 C5 120.9(5) . . ? N3 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 N3 C7 119.9(5) . . ? C6 N3 Mn1 124.5(4) . . ? C7 N3 Mn1 115.4(3) . . ? N3 C7 C8 108.0(5) . . ? N3 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? N3 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? N4 C8 C7 114.7(4) . . ? N4 C8 H8A 108.6 . . ? C7 C8 H8A 108.6 . . ? N4 C8 H8B 108.6 . . ? C7 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C30 N4 C9 110.7(4) . . ? C30 N4 C8 110.5(4) . . ? C9 N4 C8 112.8(4) . . ? C30 N4 Mn1 106.7(3) . . ? C9 N4 Mn1 108.4(3) . . ? C8 N4 Mn1 107.6(3) . . ? N4 C30 C31 111.8(5) . . ? N4 C30 H30A 109.3 . . ? C31 C30 H30A 109.3 . . ? N4 C30 H30B 109.3 . . ? C31 C30 H30B 109.3 . . ? H30A C30 H30B 107.9 . . ? N30 C31 C32 120.8(5) . . ? N30 C31 C30 116.1(5) . . ? C32 C31 C30 123.1(5) . . ? C33 C32 C31 121.0(6) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 118.2(5) . . ? C32 C33 H33 120.9 . . ? C34 C33 H33 120.9 . . ? C35 C34 C33 118.8(5) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? N30 C35 C34 123.1(5) . . ? N30 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? C35 N30 C31 118.0(5) . . ? C35 N30 Mn1 125.2(4) . . ? C31 N30 Mn1 116.3(4) . . ? N4 C9 C10 111.6(5) . . ? N4 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? N4 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? N5 C10 C9 107.5(5) . . ? N5 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? N5 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? C11 N5 C10 119.0(5) . . ? C11 N5 Mn1 120.7(4) . . ? C10 N5 Mn1 120.1(3) . . ? N5 C11 C12 120.2(5) . . ? N5 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C12 N6 N7 119.4(5) . . ? C12 N6 Mn1 113.4(3) . . ? N7 N6 Mn1 126.6(3) . . ? C15 N7 N6 118.1(5) . . ? C15 N7 Mn2 112.1(3) . . ? N6 N7 Mn2 129.6(3) . . ? N6 C12 C13 123.4(5) . . ? N6 C12 C11 115.5(5) . . ? C13 C12 C11 121.1(5) . . ? C12 C13 C14 117.4(5) . . ? C12 C13 H13 121.3 . . ? C14 C13 H13 121.3 . . ? C15 C14 C13 117.6(5) . . ? C15 C14 H14 121.2 . . ? C13 C14 H14 121.2 . . ? N7 C15 C14 124.0(5) . . ? N7 C15 C16 114.7(5) . . ? C14 C15 C16 121.3(5) . . ? N8 C16 C15 120.4(5) . . ? N8 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 N8 C17 119.7(5) . . ? C16 N8 Mn2 124.6(4) . . ? C17 N8 Mn2 115.1(3) . . ? N8 C17 C18 106.4(4) . . ? N8 C17 H17A 110.5 . . ? C18 C17 H17A 110.5 . . ? N8 C17 H17B 110.5 . . ? C18 C17 H17B 110.5 . . ? H17A C17 H17B 108.6 . . ? N9 C18 C17 114.5(4) . . ? N9 C18 H18A 108.6 . . ? C17 C18 H18A 108.6 . . ? N9 C18 H18B 108.6 . . ? C17 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C40 N9 C18 110.0(4) . . ? C40 N9 C19 109.2(4) . . ? C18 N9 C19 113.4(4) . . ? C40 N9 Mn2 107.7(3) . . ? C18 N9 Mn2 107.2(3) . . ? C19 N9 Mn2 109.1(3) . . ? N9 C40 C41 112.7(5) . . ? N9 C40 H40A 109.1 . . ? C41 C40 H40A 109.1 . . ? N9 C40 H40B 109.1 . . ? C41 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? C42 C41 N40 121.8(5) . . ? C42 C41 C40 121.5(5) . . ? N40 C41 C40 116.5(5) . . ? C41 C42 C43 120.2(6) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C42 C43 C44 117.7(6) . . ? C42 C43 H43 121.1 . . ? C44 C43 H43 121.1 . . ? C45 C44 C43 119.1(6) . . ? C45 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? N40 C45 C44 124.6(6) . . ? N40 C45 H45 117.7 . . ? C44 C45 H45 117.7 . . ? C45 N40 C41 116.6(5) . . ? C45 N40 Mn2 126.7(4) . . ? C41 N40 Mn2 116.6(4) . . ? N9 C19 C20 111.9(4) . . ? N9 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N9 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? N10 C20 C19 107.7(4) . . ? N10 C20 H20A 110.2 . . ? C19 C20 H20A 110.2 . . ? N10 C20 H20B 110.2 . . ? C19 C20 H20B 110.2 . . ? H20A C20 H20B 108.5 . . ? C21 N10 C20 118.4(5) . . ? C21 N10 Mn2 121.2(4) . . ? C20 N10 Mn2 120.3(3) . . ? N10 C21 C2 118.0(5) . . ? N10 C21 H21 121.0 . . ? C2 C21 H21 121.0 . . ? C200 N200 Mn2 165.2(5) . . ? N200 C200 C201 177.4(7) . . ? C200 C201 H20C 109.5 . . ? C200 C201 H20D 109.5 . . ? H20C C201 H20D 109.5 . . ? C200 C201 H20E 109.5 . . ? H20C C201 H20E 109.5 . . ? H20D C201 H20E 109.5 . . ? Mn1 O210 H21A 127(5) . . ? Mn1 O210 H21B 124(5) . . ? H21A O210 H21B 109(7) . . ? O11 Cl1 O13 109.1(3) . . ? O11 Cl1 O12 106.6(3) . . ? O13 Cl1 O12 110.1(3) . . ? O11 Cl1 O14 110.9(3) . . ? O13 Cl1 O14 109.7(4) . . ? O12 Cl1 O14 110.3(3) . . ? O22 Cl2 O24 109.5(3) . . ? O22 Cl2 O23 109.5(3) . . ? O24 Cl2 O23 110.0(3) . . ? O22 Cl2 O21 109.2(3) . . ? O24 Cl2 O21 110.0(3) . . ? O23 Cl2 O21 108.6(3) . . ? O33 Cl3 O31 113.2(4) . . ? O33 Cl3 O32 110.8(4) . . ? O31 Cl3 O32 110.9(3) . . ? O33 Cl3 O34 107.1(6) . . ? O31 Cl3 O34 106.8(5) . . ? O32 Cl3 O34 107.9(4) . . ? O41 Cl4 O42 109.5(3) . . ? O41 Cl4 O44 109.3(3) . . ? O42 Cl4 O44 109.8(3) . . ? O41 Cl4 O43 109.4(3) . . ? O42 Cl4 O43 109.4(2) . . ? O44 Cl4 O43 109.5(3) . . ? N220 C220 C221 178.3(9) . . ? C220 C221 H22A 109.5 . . ? C220 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C220 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? O232 C231 C230 117(2) . . ? O232 C231 H23D 108.1 . . ? C230 C231 H23D 108.1 . . ? O232 C231 H23E 108.1 . . ? C230 C231 H23E 108.1 . . ? H23D C231 H23E 107.3 . . ? C231 O232 C233 123.3(19) . . ? N230 C233 C234 170.7(18) . . ? N230 C233 O232 89.4(16) . . ? C234 C233 O232 96.4(12) . . ? N230 C233 H23F 71.5 . . ? C234 C233 H23F 112.5 . . ? O232 C233 H23F 112.5 . . ? N230 C233 H23G 58.4 . . ? C234 C233 H23G 112.5 . . ? O232 C233 H23G 112.5 . . ? H23F C233 H23G 110.0 . . ? C233 C234 H23H 109.5 . . ? C233 C234 H23I 109.5 . . ? C233 C234 H23J 109.5 . . ? C233 C234 H23K 109.5 . . ? C233 C234 H23L 109.5 . . ? H23K C234 H23L 109.5 . . ? C233 C234 H23M 109.5 . . ? H23K C234 H23M 109.5 . . ? H23L C234 H23M 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 O210 Mn1 N1 C5 -170.2(3) . . . . ? N3 Mn1 N1 C5 5.0(3) . . . . ? N5 Mn1 N1 C5 73.8(4) . . . . ? N30 Mn1 N1 C5 -87.2(4) . . . . ? N4 Mn1 N1 C5 -28.0(5) . . . . ? N6 Mn1 N1 C5 120.0(4) . . . . ? O210 Mn1 N1 N2 4.1(5) . . . . ? N3 Mn1 N1 N2 179.3(5) . . . . ? N5 Mn1 N1 N2 -112.0(4) . . . . ? N30 Mn1 N1 N2 87.1(4) . . . . ? N4 Mn1 N1 N2 146.3(4) . . . . ? N6 Mn1 N1 N2 -65.8(4) . . . . ? C5 N1 N2 C2 2.4(7) . . . . ? Mn1 N1 N2 C2 -171.5(4) . . . . ? C5 N1 N2 Mn2 -166.3(4) . . . . ? Mn1 N1 N2 Mn2 19.8(6) . . . . ? N200 Mn2 N2 C2 104.6(4) . . . . ? N8 Mn2 N2 C2 -68.1(4) . . . . ? N10 Mn2 N2 C2 11.9(4) . . . . ? N40 Mn2 N2 C2 175.8(3) . . . . ? N9 Mn2 N2 C2 18.8(5) . . . . ? N7 Mn2 N2 C2 -128.9(4) . . . . ? N200 Mn2 N2 N1 -86.2(4) . . . . ? N8 Mn2 N2 N1 101.1(4) . . . . ? N10 Mn2 N2 N1 -178.8(4) . . . . ? N40 Mn2 N2 N1 -14.9(6) . . . . ? N9 Mn2 N2 N1 -172.0(4) . . . . ? N7 Mn2 N2 N1 40.4(4) . . . . ? N1 N2 C2 C3 -1.8(8) . . . . ? Mn2 N2 C2 C3 168.3(4) . . . . ? N1 N2 C2 C21 176.7(4) . . . . ? Mn2 N2 C2 C21 -13.2(6) . . . . ? N2 C2 C3 C4 0.7(8) . . . . ? C21 C2 C3 C4 -177.8(5) . . . . ? C2 C3 C4 C5 -0.2(8) . . . . ? N2 N1 C5 C4 -2.0(8) . . . . ? Mn1 N1 C5 C4 173.0(4) . . . . ? N2 N1 C5 C6 178.9(4) . . . . ? Mn1 N1 C5 C6 -6.1(6) . . . . ? C3 C4 C5 N1 0.9(8) . . . . ? C3 C4 C5 C6 179.9(5) . . . . ? N1 C5 C6 N3 3.9(8) . . . . ? C4 C5 C6 N3 -175.2(5) . . . . ? C5 C6 N3 C7 176.5(5) . . . . ? C5 C6 N3 Mn1 1.4(7) . . . . ? O210 Mn1 N3 C6 157.6(7) . . . . ? N5 Mn1 N3 C6 -134.2(5) . . . . ? N30 Mn1 N3 C6 82.3(5) . . . . ? N4 Mn1 N3 C6 154.1(5) . . . . ? N6 Mn1 N3 C6 -67.4(5) . . . . ? N1 Mn1 N3 C6 -3.4(4) . . . . ? O210 Mn1 N3 C7 -17.8(10) . . . . ? N5 Mn1 N3 C7 50.5(4) . . . . ? N30 Mn1 N3 C7 -93.0(4) . . . . ? N4 Mn1 N3 C7 -21.2(4) . . . . ? N6 Mn1 N3 C7 117.3(4) . . . . ? N1 Mn1 N3 C7 -178.7(4) . . . . ? C6 N3 C7 C8 -132.4(5) . . . . ? Mn1 N3 C7 C8 43.2(5) . . . . ? N3 C7 C8 N4 -48.5(6) . . . . ? C7 C8 N4 C30 146.1(5) . . . . ? C7 C8 N4 C9 -89.5(5) . . . . ? C7 C8 N4 Mn1 30.1(5) . . . . ? O210 Mn1 N4 C30 57.2(3) . . . . ? N3 Mn1 N4 C30 -123.5(3) . . . . ? N5 Mn1 N4 C30 144.8(4) . . . . ? N30 Mn1 N4 C30 -28.1(3) . . . . ? N6 Mn1 N4 C30 140.1(3) . . . . ? N1 Mn1 N4 C30 -92.1(4) . . . . ? O210 Mn1 N4 C9 -62.0(4) . . . . ? N3 Mn1 N4 C9 117.3(4) . . . . ? N5 Mn1 N4 C9 25.6(3) . . . . ? N30 Mn1 N4 C9 -147.3(4) . . . . ? N6 Mn1 N4 C9 20.9(5) . . . . ? N1 Mn1 N4 C9 148.8(3) . . . . ? O210 Mn1 N4 C8 175.8(3) . . . . ? N3 Mn1 N4 C8 -5.0(3) . . . . ? N5 Mn1 N4 C8 -96.7(3) . . . . ? N30 Mn1 N4 C8 90.5(3) . . . . ? N6 Mn1 N4 C8 -101.4(4) . . . . ? N1 Mn1 N4 C8 26.5(4) . . . . ? C9 N4 C30 C31 161.8(4) . . . . ? C8 N4 C30 C31 -72.6(5) . . . . ? Mn1 N4 C30 C31 44.1(5) . . . . ? N4 C30 C31 N30 -39.9(7) . . . . ? N4 C30 C31 C32 142.6(5) . . . . ? N30 C31 C32 C33 -3.4(9) . . . . ? C30 C31 C32 C33 174.0(5) . . . . ? C31 C32 C33 C34 1.1(9) . . . . ? C32 C33 C34 C35 1.7(8) . . . . ? C33 C34 C35 N30 -2.4(9) . . . . ? C34 C35 N30 C31 0.2(8) . . . . ? C34 C35 N30 Mn1 172.2(4) . . . . ? C32 C31 N30 C35 2.7(8) . . . . ? C30 C31 N30 C35 -174.9(5) . . . . ? C32 C31 N30 Mn1 -170.0(4) . . . . ? C30 C31 N30 Mn1 12.4(6) . . . . ? O210 Mn1 N30 C35 103.1(5) . . . . ? N3 Mn1 N30 C35 -88.8(4) . . . . ? N5 Mn1 N30 C35 -174.6(4) . . . . ? N4 Mn1 N30 C35 -163.2(5) . . . . ? N6 Mn1 N30 C35 30.5(6) . . . . ? N1 Mn1 N30 C35 -21.0(4) . . . . ? O210 Mn1 N30 C31 -84.8(4) . . . . ? N3 Mn1 N30 C31 83.3(4) . . . . ? N5 Mn1 N30 C31 -2.5(5) . . . . ? N4 Mn1 N30 C31 8.9(4) . . . . ? N6 Mn1 N30 C31 -157.4(4) . . . . ? N1 Mn1 N30 C31 151.2(4) . . . . ? C30 N4 C9 C10 -165.3(5) . . . . ? C8 N4 C9 C10 70.4(6) . . . . ? Mn1 N4 C9 C10 -48.6(5) . . . . ? N4 C9 C10 N5 48.0(6) . . . . ? C9 C10 N5 C11 162.0(5) . . . . ? C9 C10 N5 Mn1 -24.2(6) . . . . ? O210 Mn1 N5 C11 -93.5(5) . . . . ? N3 Mn1 N5 C11 97.9(5) . . . . ? N30 Mn1 N5 C11 -175.1(4) . . . . ? N4 Mn1 N5 C11 173.4(5) . . . . ? N6 Mn1 N5 C11 -9.8(4) . . . . ? N1 Mn1 N5 C11 38.0(5) . . . . ? O210 Mn1 N5 C10 92.8(4) . . . . ? N3 Mn1 N5 C10 -75.8(4) . . . . ? N30 Mn1 N5 C10 11.1(5) . . . . ? N4 Mn1 N5 C10 -0.3(4) . . . . ? N6 Mn1 N5 C10 176.4(4) . . . . ? N1 Mn1 N5 C10 -135.7(4) . . . . ? C10 N5 C11 C12 -178.2(5) . . . . ? Mn1 N5 C11 C12 8.0(7) . . . . ? O210 Mn1 N6 C12 101.6(4) . . . . ? N3 Mn1 N6 C12 -69.7(4) . . . . ? N5 Mn1 N6 C12 10.7(4) . . . . ? N30 Mn1 N6 C12 175.0(4) . . . . ? N4 Mn1 N6 C12 15.5(5) . . . . ? N1 Mn1 N6 C12 -130.3(4) . . . . ? O210 Mn1 N6 N7 -87.3(4) . . . . ? N3 Mn1 N6 N7 101.4(4) . . . . ? N5 Mn1 N6 N7 -178.2(5) . . . . ? N30 Mn1 N6 N7 -13.9(6) . . . . ? N4 Mn1 N6 N7 -173.4(4) . . . . ? N1 Mn1 N6 N7 40.8(4) . . . . ? C12 N6 N7 C15 3.3(7) . . . . ? Mn1 N6 N7 C15 -167.4(4) . . . . ? C12 N6 N7 Mn2 -171.3(4) . . . . ? Mn1 N6 N7 Mn2 18.1(6) . . . . ? N200 Mn2 N7 C15 -166.0(4) . . . . ? N8 Mn2 N7 C15 5.1(4) . . . . ? N10 Mn2 N7 C15 72.8(4) . . . . ? N40 Mn2 N7 C15 -87.7(4) . . . . ? N9 Mn2 N7 C15 -30.1(5) . . . . ? N2 Mn2 N7 C15 120.4(4) . . . . ? N200 Mn2 N7 N6 8.8(5) . . . . ? N8 Mn2 N7 N6 180.0(5) . . . . ? N10 Mn2 N7 N6 -112.4(4) . . . . ? N40 Mn2 N7 N6 87.2(4) . . . . ? N9 Mn2 N7 N6 144.7(4) . . . . ? N2 Mn2 N7 N6 -64.8(4) . . . . ? N7 N6 C12 C13 -2.3(8) . . . . ? Mn1 N6 C12 C13 169.5(5) . . . . ? N7 N6 C12 C11 177.3(5) . . . . ? Mn1 N6 C12 C11 -11.0(6) . . . . ? N5 C11 C12 N6 2.9(8) . . . . ? N5 C11 C12 C13 -177.5(6) . . . . ? N6 C12 C13 C14 0.6(9) . . . . ? C11 C12 C13 C14 -178.9(5) . . . . ? C12 C13 C14 C15 0.1(9) . . . . ? N6 N7 C15 C14 -2.8(9) . . . . ? Mn2 N7 C15 C14 172.7(5) . . . . ? N6 N7 C15 C16 179.5(5) . . . . ? Mn2 N7 C15 C16 -5.0(6) . . . . ? C13 C14 C15 N7 1.1(9) . . . . ? C13 C14 C15 C16 178.7(6) . . . . ? N7 C15 C16 N8 1.3(8) . . . . ? C14 C15 C16 N8 -176.5(6) . . . . ? C15 C16 N8 C17 175.4(5) . . . . ? C15 C16 N8 Mn2 4.4(8) . . . . ? N200 Mn2 N8 C16 142.1(7) . . . . ? N10 Mn2 N8 C16 -137.2(5) . . . . ? N40 Mn2 N8 C16 79.1(5) . . . . ? N9 Mn2 N8 C16 150.7(5) . . . . ? N2 Mn2 N8 C16 -70.1(5) . . . . ? N7 Mn2 N8 C16 -5.0(5) . . . . ? N200 Mn2 N8 C17 -29.2(9) . . . . ? N10 Mn2 N8 C17 51.4(4) . . . . ? N40 Mn2 N8 C17 -92.2(4) . . . . ? N9 Mn2 N8 C17 -20.7(4) . . . . ? N2 Mn2 N8 C17 118.6(4) . . . . ? N7 Mn2 N8 C17 -176.4(4) . . . . ? C16 N8 C17 C18 -128.2(6) . . . . ? Mn2 N8 C17 C18 43.7(5) . . . . ? N8 C17 C18 N9 -51.5(6) . . . . ? C17 C18 N9 C40 150.7(5) . . . . ? C17 C18 N9 C19 -86.6(5) . . . . ? C17 C18 N9 Mn2 33.9(5) . . . . ? N200 Mn2 N9 C40 52.4(3) . . . . ? N8 Mn2 N9 C40 -125.5(3) . . . . ? N10 Mn2 N9 C40 143.1(4) . . . . ? N40 Mn2 N9 C40 -30.1(3) . . . . ? N2 Mn2 N9 C40 136.4(3) . . . . ? N7 Mn2 N9 C40 -92.0(4) . . . . ? N200 Mn2 N9 C18 170.8(3) . . . . ? N8 Mn2 N9 C18 -7.2(3) . . . . ? N10 Mn2 N9 C18 -98.6(3) . . . . ? N40 Mn2 N9 C18 88.2(3) . . . . ? N2 Mn2 N9 C18 -105.3(4) . . . . ? N7 Mn2 N9 C18 26.3(4) . . . . ? N200 Mn2 N9 C19 -66.0(3) . . . . ? N8 Mn2 N9 C19 116.0(4) . . . . ? N10 Mn2 N9 C19 24.7(3) . . . . ? N40 Mn2 N9 C19 -148.6(4) . . . . ? N2 Mn2 N9 C19 17.9(5) . . . . ? N7 Mn2 N9 C19 149.6(3) . . . . ? C18 N9 C40 C41 -75.5(6) . . . . ? C19 N9 C40 C41 159.3(5) . . . . ? Mn2 N9 C40 C41 41.0(5) . . . . ? N9 C40 C41 C42 156.2(5) . . . . ? N9 C40 C41 N40 -29.2(7) . . . . ? N40 C41 C42 C43 -0.2(10) . . . . ? C40 C41 C42 C43 174.2(6) . . . . ? C41 C42 C43 C44 0.4(10) . . . . ? C42 C43 C44 C45 0.9(10) . . . . ? C43 C44 C45 N40 -2.7(10) . . . . ? C44 C45 N40 C41 2.8(9) . . . . ? C44 C45 N40 Mn2 -172.9(5) . . . . ? C42 C41 N40 C45 -1.4(8) . . . . ? C40 C41 N40 C45 -175.9(5) . . . . ? C42 C41 N40 Mn2 174.8(5) . . . . ? C40 C41 N40 Mn2 0.2(6) . . . . ? N200 Mn2 N40 C45 99.4(5) . . . . ? N8 Mn2 N40 C45 -92.9(5) . . . . ? N10 Mn2 N40 C45 -178.5(4) . . . . ? N9 Mn2 N40 C45 -167.6(5) . . . . ? N2 Mn2 N40 C45 27.4(6) . . . . ? N7 Mn2 N40 C45 -25.2(5) . . . . ? N200 Mn2 N40 C41 -76.4(4) . . . . ? N8 Mn2 N40 C41 91.3(4) . . . . ? N10 Mn2 N40 C41 5.8(6) . . . . ? N9 Mn2 N40 C41 16.7(4) . . . . ? N2 Mn2 N40 C41 -148.3(4) . . . . ? N7 Mn2 N40 C41 159.1(4) . . . . ? C40 N9 C19 C20 -164.3(4) . . . . ? C18 N9 C19 C20 72.5(6) . . . . ? Mn2 N9 C19 C20 -46.9(5) . . . . ? N9 C19 C20 N10 45.8(6) . . . . ? C19 C20 N10 C21 161.5(5) . . . . ? C19 C20 N10 Mn2 -23.2(6) . . . . ? N200 Mn2 N10 C21 -94.9(4) . . . . ? N8 Mn2 N10 C21 98.6(4) . . . . ? N40 Mn2 N10 C21 -174.6(4) . . . . ? N9 Mn2 N10 C21 174.6(5) . . . . ? N2 Mn2 N10 C21 -10.0(4) . . . . ? N7 Mn2 N10 C21 39.5(5) . . . . ? N200 Mn2 N10 C20 90.0(4) . . . . ? N8 Mn2 N10 C20 -76.5(4) . . . . ? N40 Mn2 N10 C20 10.3(5) . . . . ? N9 Mn2 N10 C20 -0.6(4) . . . . ? N2 Mn2 N10 C20 174.8(4) . . . . ? N7 Mn2 N10 C20 -135.6(4) . . . . ? C20 N10 C21 C2 -177.9(5) . . . . ? Mn2 N10 C21 C2 6.9(7) . . . . ? N2 C2 C21 N10 5.2(7) . . . . ? C3 C2 C21 N10 -176.2(5) . . . . ? N8 Mn2 N200 C200 40(2) . . . . ? N10 Mn2 N200 C200 -40(2) . . . . ? N40 Mn2 N200 C200 104(2) . . . . ? N9 Mn2 N200 C200 32(2) . . . . ? N2 Mn2 N200 C200 -109(2) . . . . ? N7 Mn2 N200 C200 -176.9(19) . . . . ? Mn2 N200 C200 C201 129(16) . . . . ? C230 C231 O232 C233 -160.1(19) . . . . ? C231 O232 C233 N230 14(2) . . . . ? C231 O232 C233 C234 -173.0(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O210 H21A O11 0.80(7) 2.00(7) 2.794(7) 168(7) . O210 H21B O21 0.85(7) 2.04(7) 2.851(6) 160(6) . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.64 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.749 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.108 data_mw64n _database_code_depnum_ccdc_archive 'CCDC 269198' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H50 Cl4 Mn2 N16 O17' _chemical_formula_weight 1278.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0752(3) _cell_length_b 18.0620(3) _cell_length_c 20.9482(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.4380(10) _cell_angle_gamma 90.00 _cell_volume 5267.93(17) _cell_formula_units_Z 4 _cell_measurement_temperature 84(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 0.904 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 84(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 SMART area detector' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31477 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 26.40 _reflns_number_total 10740 _reflns_number_gt 8020 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. All non-H ANIS. One perchlorate disordered: twirling about Cl4-O41 such that O42, O43, O44 are 0.6 occupancy and O45, O46, O47 are 0.4 occupancy. All H inserted at calc positions and ride, except for those on the coordinated water molecule: those two H were found from a difference map and their coordinates fixed (AFIX 01) and their U = 1.2U(attached oxygen atom). ; _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^)+(0.0380P)^2^+17.6280P] 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 10740 _refine_ls_number_parameters 726 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1416 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 0.61857(4) 0.44393(3) 0.23432(3) 0.02117(15) Uani 1 1 d . . . Mn2 Mn 0.91499(4) 0.37058(3) 0.23675(3) 0.01767(14) Uani 1 1 d . . . N1 N 0.6977(2) 0.33978(17) 0.29353(16) 0.0201(7) Uani 1 1 d . . . N2 N 0.7850(2) 0.31264(17) 0.28807(16) 0.0189(7) Uani 1 1 d . . . C2 C 0.8124(3) 0.2482(2) 0.31731(19) 0.0185(8) Uani 1 1 d . . . C3 C 0.7563(3) 0.2090(2) 0.3553(2) 0.0237(9) Uani 1 1 d . . . H3 H 0.7782 0.1640 0.3760 0.028 Uiso 1 1 calc R . . C4 C 0.6682(3) 0.2380(2) 0.3616(2) 0.0261(9) Uani 1 1 d . . . H4 H 0.6273 0.2144 0.3877 0.031 Uiso 1 1 calc R . . C5 C 0.6405(3) 0.3034(2) 0.3284(2) 0.0223(9) Uani 1 1 d . . . C6 C 0.5438(3) 0.3342(2) 0.3275(2) 0.0271(9) Uani 1 1 d . . . H6 H 0.4998 0.3114 0.3517 0.033 Uiso 1 1 calc R . . N3 N 0.5195(2) 0.39130(19) 0.29433(18) 0.0262(8) Uani 1 1 d . . . C7 C 0.4209(3) 0.4195(3) 0.2864(2) 0.0334(11) Uani 1 1 d . . . H7A H 0.4178 0.4650 0.3124 0.040 Uiso 1 1 calc R . . H7B H 0.3776 0.3820 0.3012 0.040 Uiso 1 1 calc R . . C8 C 0.3900(3) 0.4363(2) 0.2153(2) 0.0345(11) Uani 1 1 d . . . H8A H 0.3791 0.3890 0.1914 0.041 Uiso 1 1 calc R . . H8B H 0.3283 0.4634 0.2102 0.041 Uiso 1 1 calc R . . N4 N 0.4621(2) 0.48114(19) 0.18618(19) 0.0273(8) Uani 1 1 d . . . C30 C 0.4574(3) 0.4634(2) 0.1172(2) 0.0333(11) Uani 1 1 d . . . H30A H 0.4925 0.5018 0.0963 0.040 Uiso 1 1 calc R . . H30B H 0.3895 0.4644 0.0965 0.040 Uiso 1 1 calc R . . C31 C 0.4999(3) 0.3883(2) 0.1065(2) 0.0288(10) Uani 1 1 d . . . C32 C 0.4739(3) 0.3512(3) 0.0488(2) 0.0359(11) Uani 1 1 d . . . H32 H 0.4321 0.3739 0.0147 0.043 Uiso 1 1 calc R . . C33 C 0.5093(3) 0.2807(3) 0.0412(2) 0.0382(12) Uani 1 1 d . . . H33 H 0.4928 0.2546 0.0018 0.046 Uiso 1 1 calc R . . C34 C 0.5691(3) 0.2490(3) 0.0923(2) 0.0353(11) Uani 1 1 d . . . H34 H 0.5918 0.1997 0.0894 0.042 Uiso 1 1 calc R . . C35 C 0.5951(3) 0.2905(2) 0.1472(2) 0.0313(10) Uani 1 1 d . . . H35 H 0.6382 0.2693 0.1815 0.038 Uiso 1 1 calc R . . N30 N 0.5626(2) 0.35977(19) 0.15490(18) 0.0289(8) Uani 1 1 d . . . C9 C 0.4498(3) 0.5619(2) 0.1958(2) 0.0322(11) Uani 1 1 d . . . H9A H 0.3804 0.5739 0.1890 0.039 Uiso 1 1 calc R . . H9B H 0.4800 0.5893 0.1631 0.039 Uiso 1 1 calc R . . C10 C 0.4937(3) 0.5877(2) 0.2625(2) 0.0296(10) Uani 1 1 d . . . H10A H 0.4975 0.6424 0.2637 0.036 Uiso 1 1 calc R . . H10B H 0.4534 0.5713 0.2948 0.036 Uiso 1 1 calc R . . N5 N 0.5904(2) 0.55555(18) 0.27738(17) 0.0245(8) Uani 1 1 d . . . C11 C 0.6546(3) 0.5916(2) 0.3130(2) 0.0238(9) Uani 1 1 d . . . H11 H 0.6401 0.6382 0.3303 0.029 Uiso 1 1 calc R . . N6 N 0.7684(2) 0.49844(17) 0.29523(16) 0.0190(7) Uani 1 1 d . . . N7 N 0.8566(2) 0.46862(17) 0.30240(15) 0.0167(7) Uani 1 1 d . . . C12 C 0.7527(3) 0.5603(2) 0.32740(19) 0.0201(8) Uani 1 1 d . . . C13 C 0.8237(3) 0.5941(2) 0.3711(2) 0.0234(9) Uani 1 1 d . . . H13 H 0.8107 0.6376 0.3937 0.028 Uiso 1 1 calc R . . C14 C 0.9133(3) 0.5622(2) 0.38021(19) 0.0219(8) Uani 1 1 d . . . H14 H 0.9641 0.5822 0.4102 0.026 Uiso 1 1 calc R . . C15 C 0.9271(3) 0.4997(2) 0.34418(19) 0.0185(8) Uani 1 1 d . . . C16 C 1.0223(3) 0.4644(2) 0.34731(19) 0.0205(8) Uani 1 1 d . . . H16 H 1.0748 0.4809 0.3777 0.025 Uiso 1 1 calc R . . N8 N 1.0332(2) 0.41188(18) 0.30908(16) 0.0215(7) Uani 1 1 d . . . C17 C 1.1277(3) 0.3787(2) 0.3088(2) 0.0247(9) Uani 1 1 d . . . H17A H 1.1304 0.3295 0.3298 0.030 Uiso 1 1 calc R . . H17B H 1.1779 0.4105 0.3329 0.030 Uiso 1 1 calc R . . C18 C 1.1446(3) 0.3710(2) 0.2391(2) 0.0259(9) Uani 1 1 d . . . H18A H 1.1582 0.4205 0.2223 0.031 Uiso 1 1 calc R . . H18B H 1.2020 0.3397 0.2378 0.031 Uiso 1 1 calc R . . N9 N 1.0616(2) 0.33777(18) 0.19598(16) 0.0221(7) Uani 1 1 d . . . C40 C 1.0553(3) 0.3704(2) 0.1309(2) 0.0306(10) Uani 1 1 d . . . H40A H 1.0146 0.3385 0.0996 0.037 Uiso 1 1 calc R . . H40B H 1.1203 0.3723 0.1181 0.037 Uiso 1 1 calc R . . C41 C 1.0134(3) 0.4477(2) 0.1285(2) 0.0276(9) Uani 1 1 d . . . C42 C 1.0398(3) 0.4990(2) 0.0852(2) 0.0287(10) Uani 1 1 d . . . H42 H 1.0871 0.4872 0.0588 0.034 Uiso 1 1 calc R . . C43 C 0.9960(3) 0.5680(2) 0.0810(2) 0.0271(9) Uani 1 1 d . . . H43 H 1.0125 0.6039 0.0514 0.033 Uiso 1 1 calc R . . C44 C 0.9284(3) 0.5837(2) 0.12014(19) 0.0248(9) Uani 1 1 d . . . H44 H 0.8967 0.6303 0.1177 0.030 Uiso 1 1 calc R . . C45 C 0.9076(3) 0.5302(2) 0.16323(19) 0.0230(9) Uani 1 1 d . . . H45 H 0.8622 0.5419 0.1910 0.028 Uiso 1 1 calc R . . N40 N 0.9481(2) 0.46255(19) 0.16804(16) 0.0241(8) Uani 1 1 d . . . C19 C 1.0678(3) 0.2560(2) 0.1926(2) 0.0249(9) Uani 1 1 d . . . H19A H 1.1336 0.2416 0.1862 0.030 Uiso 1 1 calc R . . H19B H 1.0227 0.2380 0.1550 0.030 Uiso 1 1 calc R . . C20 C 1.0435(3) 0.2196(2) 0.2535(2) 0.0233(9) Uani 1 1 d . . . H20A H 1.0334 0.1658 0.2464 0.028 Uiso 1 1 calc R . . H20B H 1.0971 0.2265 0.2893 0.028 Uiso 1 1 calc R . . N10 N 0.9554(2) 0.25394(18) 0.27025(16) 0.0201(7) Uani 1 1 d . . . C21 C 0.9037(3) 0.2170(2) 0.3030(2) 0.0207(8) Uani 1 1 d . . . H21 H 0.9236 0.1692 0.3184 0.025 Uiso 1 1 calc R . . O210 O 0.6785(2) 0.49686(16) 0.15661(14) 0.0311(7) Uani 1 1 d . . . H21X H 0.6756 0.5522 0.1575 0.037 Uiso 1 1 d . . . H21Y H 0.6922 0.4817 0.1208 0.037 Uiso 1 1 d . . . N200 N 0.8335(3) 0.3194(2) 0.15133(17) 0.0282(8) Uani 1 1 d . . . C200 C 0.8185(4) 0.2871(3) 0.1066(3) 0.0548(15) Uani 1 1 d . . . C201 C 0.7985(6) 0.2377(4) 0.0479(3) 0.079(2) Uani 1 1 d . . . H20C H 0.8070 0.1858 0.0612 0.095 Uiso 1 1 calc R . . H20D H 0.8432 0.2498 0.0177 0.095 Uiso 1 1 calc R . . H20E H 0.7324 0.2455 0.0268 0.095 Uiso 1 1 calc R . . Cl1 Cl 0.66862(7) 0.70486(6) 0.16342(5) 0.0269(2) Uani 1 1 d . . . O11 O 0.7356(2) 0.64538(19) 0.1774(2) 0.0514(10) Uani 1 1 d . . . O12 O 0.7144(3) 0.76601(18) 0.13661(18) 0.0437(9) Uani 1 1 d . . . O13 O 0.5885(3) 0.6818(2) 0.11764(18) 0.0491(9) Uani 1 1 d . . . O14 O 0.6341(3) 0.7276(2) 0.22093(18) 0.0551(11) Uani 1 1 d . . . Cl2 Cl 0.78700(8) 0.09081(6) 0.19417(5) 0.0301(2) Uani 1 1 d . . . O21 O 0.8162(3) 0.0615(2) 0.25723(19) 0.0588(11) Uani 1 1 d . . . O22 O 0.7337(2) 0.03531(19) 0.15476(18) 0.0461(9) Uani 1 1 d . . . O23 O 0.7280(3) 0.1540(2) 0.1995(2) 0.0539(11) Uani 1 1 d . . . O24 O 0.8704(3) 0.1111(2) 0.1671(2) 0.0529(10) Uani 1 1 d . . . Cl3 Cl 0.96852(10) 0.82255(6) 0.03042(5) 0.0393(3) Uani 1 1 d . . . O31 O 0.8770(3) 0.8602(2) 0.03094(19) 0.0648(12) Uani 1 1 d . . . O32 O 0.9681(3) 0.78990(19) -0.03203(16) 0.0452(9) Uani 1 1 d . . . O33 O 0.9747(3) 0.7675(2) 0.07820(18) 0.0610(11) Uani 1 1 d . . . O34 O 1.0423(4) 0.8747(3) 0.0423(3) 0.119(3) Uani 1 1 d . . . Cl4 Cl 0.74213(8) 0.43385(7) -0.00466(6) 0.0398(3) Uani 1 1 d . . . O41 O 0.8352(3) 0.4042(3) 0.0086(2) 0.0796(17) Uani 1 1 d . A . O42 O 0.6997(4) 0.4093(4) 0.0564(3) 0.0525(14) Uani 0.60 1 d P A 1 O43 O 0.6797(6) 0.4049(4) -0.0559(3) 0.0621(19) Uani 0.60 1 d P A 1 O44 O 0.7488(4) 0.5096(4) -0.0035(4) 0.0525(15) Uani 0.60 1 d P A 1 O45 O 0.7509(7) 0.4687(6) -0.0745(4) 0.0525(14) Uani 0.40 1 d P A 2 O46 O 0.7059(9) 0.4951(6) 0.0248(5) 0.0621(19) Uani 0.40 1 d P A 2 O47 O 0.6799(7) 0.3782(6) -0.0203(6) 0.0525(15) Uani 0.40 1 d P A 2 N210 N 0.3673(5) 0.8729(3) 0.0382(3) 0.0772(18) Uani 1 1 d . . . C210 C 0.3029(5) 0.9135(4) 0.0236(3) 0.0660(19) Uani 1 1 d . . . C211 C 0.2255(5) 0.9617(4) 0.0004(4) 0.074(2) Uani 1 1 d . . . H21A H 0.2195 0.9654 -0.0466 0.089 Uiso 1 1 calc R . . H21B H 0.2379 1.0109 0.0196 0.089 Uiso 1 1 calc R . . H21C H 0.1658 0.9419 0.0125 0.089 Uiso 1 1 calc R . . N220 N 0.2863(3) 0.2621(2) 0.1146(2) 0.0435(11) Uani 1 1 d . . . C220 C 0.2600(3) 0.2856(2) 0.0648(2) 0.0297(10) Uani 1 1 d . . . C221 C 0.2252(4) 0.3167(3) 0.0022(2) 0.0446(13) Uani 1 1 d . . . H22A H 0.1550 0.3134 -0.0059 0.054 Uiso 1 1 calc R . . H22B H 0.2524 0.2892 -0.0311 0.054 Uiso 1 1 calc R . . H22C H 0.2447 0.3688 0.0013 0.054 Uiso 1 1 calc R . . N230 N 0.5386(4) 0.5597(3) 0.4259(3) 0.0723(16) Uani 1 1 d . . . C230 C 0.5714(5) 0.5748(3) 0.4773(3) 0.0549(15) Uani 1 1 d . . . C231 C 0.6097(6) 0.5940(5) 0.5425(4) 0.089(3) Uani 1 1 d . . . H23A H 0.6515 0.6374 0.5424 0.107 Uiso 1 1 calc R . . H23B H 0.6468 0.5523 0.5630 0.107 Uiso 1 1 calc R . . H23C H 0.5568 0.6054 0.5665 0.107 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 0.0169(3) 0.0153(3) 0.0300(4) 0.0030(3) -0.0012(2) -0.0009(2) Mn2 0.0179(3) 0.0162(3) 0.0188(3) 0.0004(2) 0.0023(2) 0.0005(2) N1 0.0180(16) 0.0162(16) 0.0257(18) -0.0003(14) 0.0020(14) -0.0032(13) N2 0.0184(16) 0.0154(16) 0.0217(17) -0.0016(13) -0.0013(13) -0.0022(13) C2 0.0178(19) 0.0157(19) 0.021(2) -0.0011(15) -0.0017(15) -0.0040(15) C3 0.025(2) 0.0153(19) 0.031(2) 0.0059(17) 0.0031(18) 0.0006(16) C4 0.026(2) 0.022(2) 0.032(2) 0.0016(18) 0.0071(18) -0.0041(17) C5 0.0192(19) 0.0159(19) 0.031(2) 0.0025(17) 0.0009(17) -0.0020(16) C6 0.021(2) 0.023(2) 0.038(3) 0.0039(19) 0.0058(19) -0.0043(17) N3 0.0182(17) 0.0204(18) 0.039(2) 0.0019(16) 0.0016(15) -0.0002(14) C7 0.020(2) 0.027(2) 0.054(3) 0.008(2) 0.008(2) -0.0031(18) C8 0.021(2) 0.023(2) 0.057(3) 0.004(2) -0.002(2) -0.0027(18) N4 0.0200(17) 0.0182(18) 0.042(2) 0.0049(16) -0.0010(16) -0.0021(14) C30 0.029(2) 0.030(2) 0.035(3) 0.008(2) -0.013(2) -0.0016(19) C31 0.021(2) 0.030(2) 0.033(3) 0.0016(19) -0.0035(18) -0.0063(18) C32 0.027(2) 0.045(3) 0.034(3) 0.003(2) 0.000(2) -0.006(2) C33 0.031(3) 0.045(3) 0.037(3) -0.008(2) 0.000(2) -0.008(2) C34 0.035(3) 0.029(2) 0.041(3) -0.006(2) 0.003(2) -0.004(2) C35 0.027(2) 0.026(2) 0.039(3) -0.001(2) -0.004(2) -0.0035(18) N30 0.0249(18) 0.0211(18) 0.037(2) 0.0012(16) -0.0085(16) -0.0028(15) C9 0.021(2) 0.022(2) 0.052(3) 0.010(2) -0.001(2) 0.0037(17) C10 0.019(2) 0.018(2) 0.051(3) 0.002(2) 0.004(2) 0.0043(17) N5 0.0198(17) 0.0186(17) 0.035(2) 0.0041(15) 0.0019(15) 0.0001(14) C11 0.024(2) 0.019(2) 0.030(2) 0.0035(17) 0.0084(18) 0.0013(17) N6 0.0192(16) 0.0167(16) 0.0216(18) 0.0004(13) 0.0044(14) -0.0010(13) N7 0.0168(16) 0.0138(15) 0.0196(17) 0.0015(13) 0.0032(13) -0.0020(12) C12 0.024(2) 0.0151(19) 0.022(2) 0.0022(16) 0.0058(16) 0.0001(16) C13 0.028(2) 0.016(2) 0.026(2) -0.0033(16) 0.0060(18) 0.0014(17) C14 0.027(2) 0.0181(19) 0.020(2) -0.0047(16) -0.0002(17) -0.0027(16) C15 0.0191(19) 0.0178(19) 0.019(2) 0.0030(15) 0.0029(16) -0.0010(15) C16 0.021(2) 0.020(2) 0.020(2) 0.0017(16) 0.0029(16) -0.0023(16) N8 0.0196(16) 0.0179(17) 0.0272(19) 0.0009(14) 0.0038(14) 0.0001(13) C17 0.0159(19) 0.026(2) 0.032(2) -0.0050(18) 0.0022(17) 0.0006(16) C18 0.022(2) 0.022(2) 0.036(2) 0.0014(18) 0.0104(18) 0.0005(17) N9 0.0268(18) 0.0189(17) 0.0221(18) 0.0000(14) 0.0082(15) 0.0017(14) C40 0.043(3) 0.024(2) 0.028(2) 0.0047(19) 0.016(2) 0.006(2) C41 0.038(2) 0.024(2) 0.022(2) 0.0014(17) 0.0084(19) 0.0030(19) C42 0.040(3) 0.028(2) 0.021(2) 0.0042(18) 0.0115(19) -0.0005(19) C43 0.037(2) 0.024(2) 0.020(2) 0.0039(17) 0.0040(18) -0.0044(18) C44 0.033(2) 0.021(2) 0.019(2) 0.0016(16) -0.0012(18) -0.0017(18) C45 0.025(2) 0.024(2) 0.020(2) -0.0014(17) 0.0037(17) 0.0011(17) N40 0.0300(19) 0.0219(18) 0.0212(18) 0.0024(14) 0.0070(15) 0.0038(15) C19 0.028(2) 0.018(2) 0.030(2) -0.0029(17) 0.0081(18) 0.0036(17) C20 0.024(2) 0.0177(19) 0.029(2) 0.0002(17) 0.0063(17) 0.0018(16) N10 0.0204(16) 0.0178(16) 0.0219(18) -0.0009(14) 0.0025(14) 0.0007(13) C21 0.0175(19) 0.0161(19) 0.027(2) 0.0009(16) -0.0026(16) 0.0021(15) O210 0.0406(18) 0.0272(16) 0.0256(16) -0.0021(13) 0.0056(14) -0.0066(14) N200 0.033(2) 0.035(2) 0.0149(18) -0.0076(16) -0.0023(15) -0.0049(17) C200 0.048(3) 0.053(4) 0.062(4) 0.016(3) 0.004(3) 0.002(3) C201 0.093(5) 0.072(5) 0.068(5) -0.017(4) 0.000(4) -0.010(4) Cl1 0.0249(5) 0.0238(5) 0.0320(6) -0.0020(4) 0.0044(4) -0.0032(4) O11 0.0298(18) 0.0311(19) 0.094(3) 0.0068(19) 0.0125(19) 0.0069(15) O12 0.047(2) 0.0314(18) 0.053(2) 0.0043(16) 0.0108(17) -0.0129(16) O13 0.046(2) 0.050(2) 0.048(2) 0.0034(18) -0.0060(17) -0.0147(18) O14 0.088(3) 0.040(2) 0.042(2) 0.0093(17) 0.026(2) 0.021(2) Cl2 0.0296(5) 0.0254(5) 0.0352(6) -0.0066(4) 0.0040(5) 0.0018(4) O21 0.083(3) 0.039(2) 0.048(2) 0.0069(18) -0.014(2) -0.010(2) O22 0.042(2) 0.041(2) 0.053(2) -0.0200(17) -0.0012(17) -0.0067(16) O23 0.043(2) 0.044(2) 0.071(3) -0.024(2) -0.0044(19) 0.0197(17) O24 0.056(2) 0.039(2) 0.071(3) -0.0163(19) 0.034(2) -0.0101(18) Cl3 0.0627(8) 0.0330(6) 0.0246(6) -0.0042(5) 0.0146(5) -0.0162(6) O31 0.090(3) 0.060(3) 0.046(2) -0.002(2) 0.013(2) 0.032(2) O32 0.073(3) 0.0350(19) 0.0295(18) -0.0024(15) 0.0154(18) 0.0033(18) O33 0.080(3) 0.067(3) 0.032(2) 0.0184(19) -0.007(2) 0.000(2) O34 0.135(5) 0.134(5) 0.108(4) -0.085(4) 0.082(4) -0.109(4) Cl4 0.0290(6) 0.0484(7) 0.0393(7) -0.0161(6) -0.0035(5) 0.0039(5) O41 0.028(2) 0.127(4) 0.085(3) 0.074(3) 0.013(2) 0.019(2) O42 0.055(3) 0.068(4) 0.043(3) -0.016(3) 0.034(3) -0.016(3) O43 0.089(5) 0.050(4) 0.038(3) -0.025(3) -0.020(3) 0.030(3) O44 0.039(3) 0.056(4) 0.064(4) -0.026(3) 0.014(3) -0.015(3) O45 0.055(3) 0.068(4) 0.043(3) -0.016(3) 0.034(3) -0.016(3) O46 0.089(5) 0.050(4) 0.038(3) -0.025(3) -0.020(3) 0.030(3) O47 0.039(3) 0.056(4) 0.064(4) -0.026(3) 0.014(3) -0.015(3) N210 0.084(4) 0.073(4) 0.069(4) 0.016(3) -0.011(3) -0.026(4) C210 0.065(4) 0.055(4) 0.069(5) 0.016(3) -0.018(4) -0.010(3) C211 0.079(5) 0.076(5) 0.070(5) -0.015(4) 0.023(4) -0.003(4) N220 0.041(2) 0.042(2) 0.047(3) 0.016(2) 0.002(2) -0.008(2) C220 0.024(2) 0.028(2) 0.038(3) 0.003(2) 0.009(2) -0.0017(18) C221 0.044(3) 0.054(3) 0.035(3) 0.011(2) 0.003(2) -0.011(3) N230 0.091(4) 0.074(4) 0.050(3) 0.018(3) 0.008(3) 0.023(3) C230 0.065(4) 0.053(4) 0.047(4) 0.011(3) 0.008(3) 0.017(3) C231 0.103(6) 0.090(6) 0.068(5) -0.012(4) -0.012(4) 0.024(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 O210 2.163(3) . y Mn1 N3 2.223(4) . y Mn1 N5 2.267(3) . y Mn1 N30 2.305(4) . y Mn1 N4 2.380(3) . y Mn1 N1 2.432(3) . y Mn1 N6 2.501(3) . y Mn2 N200 2.184(4) . y Mn2 N8 2.209(3) . y Mn2 N10 2.267(3) . y Mn2 N40 2.290(3) . y Mn2 N9 2.420(3) . y Mn2 N7 2.456(3) . y Mn2 N2 2.485(3) . y N1 C5 1.337(5) . ? N1 N2 1.343(4) . ? N2 C2 1.345(5) . ? C2 C3 1.394(5) . ? C2 C21 1.474(5) . ? C3 C4 1.370(6) . ? C3 H3 0.9500 . ? C4 C5 1.397(6) . ? C4 H4 0.9500 . ? C5 C6 1.468(6) . ? C6 N3 1.262(5) . ? C6 H6 0.9500 . ? N3 C7 1.465(5) . ? C7 C8 1.520(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N4 1.497(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N4 C30 1.472(6) . ? N4 C9 1.487(5) . ? C30 C31 1.513(6) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N30 1.344(5) . ? C31 C32 1.383(7) . ? C32 C33 1.385(7) . ? C32 H32 0.9500 . ? C33 C34 1.384(7) . ? C33 H33 0.9500 . ? C34 C35 1.378(6) . ? C34 H34 0.9500 . ? C35 N30 1.350(6) . ? C35 H35 0.9500 . ? C9 C10 1.515(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N5 1.470(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? N5 C11 1.265(5) . ? C11 C12 1.481(5) . ? C11 H11 0.9500 . ? N6 C12 1.341(5) . ? N6 N7 1.341(4) . ? N7 C15 1.345(5) . ? C12 C13 1.392(6) . ? C13 C14 1.374(6) . ? C13 H13 0.9500 . ? C14 C15 1.387(5) . ? C14 H14 0.9500 . ? C15 C16 1.477(5) . ? C16 N8 1.265(5) . ? C16 H16 0.9500 . ? N8 C17 1.460(5) . ? C17 C18 1.519(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N9 1.493(5) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? N9 C40 1.476(5) . ? N9 C19 1.482(5) . ? C40 C41 1.515(6) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 N40 1.350(5) . ? C41 C42 1.386(6) . ? C42 C43 1.386(6) . ? C42 H42 0.9500 . ? C43 C44 1.374(6) . ? C43 H43 0.9500 . ? C44 C45 1.382(6) . ? C44 H44 0.9500 . ? C45 N40 1.346(5) . ? C45 H45 0.9500 . ? C19 C20 1.519(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N10 1.474(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? N10 C21 1.261(5) . ? C21 H21 0.9500 . ? O210 H21X 1.0006 . ? O210 H21Y 0.8469 . ? N200 C200 1.097(7) . ? C200 C201 1.511(9) . ? C201 H20C 0.9800 . ? C201 H20D 0.9800 . ? C201 H20E 0.9800 . ? Cl1 O14 1.424(4) . ? Cl1 O11 1.431(3) . ? Cl1 O13 1.431(4) . ? Cl1 O12 1.434(3) . ? Cl2 O24 1.424(4) . ? Cl2 O23 1.425(3) . ? Cl2 O21 1.427(4) . ? Cl2 O22 1.438(3) . ? Cl3 O34 1.397(4) . ? Cl3 O33 1.404(4) . ? Cl3 O32 1.434(3) . ? Cl3 O31 1.458(4) . ? Cl4 O47 1.342(10) . ? Cl4 O44 1.371(7) . ? Cl4 O43 1.387(6) . ? Cl4 O46 1.399(9) . ? Cl4 O41 1.405(4) . ? Cl4 O42 1.553(6) . ? Cl4 O45 1.614(9) . ? N210 C210 1.171(8) . ? C210 C211 1.422(10) . ? C211 H21A 0.9800 . ? C211 H21B 0.9800 . ? C211 H21C 0.9800 . ? N220 C220 1.137(6) . ? C220 C221 1.444(7) . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? N230 C230 1.141(8) . ? C230 C231 1.434(9) . ? C231 H23A 0.9800 . ? C231 H23B 0.9800 . ? C231 H23C 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 O210 Mn1 N3 163.91(13) . . y O210 Mn1 N5 90.96(12) . . y N3 Mn1 N5 89.68(13) . . y O210 Mn1 N30 83.01(12) . . y N3 Mn1 N30 87.12(13) . . y N5 Mn1 N30 144.30(12) . . y O210 Mn1 N4 89.72(12) . . y N3 Mn1 N4 75.08(13) . . y N5 Mn1 N4 73.29(12) . . y N30 Mn1 N4 71.54(12) . . y O210 Mn1 N1 121.72(12) . . y N3 Mn1 N1 70.06(12) . . y N5 Mn1 N1 125.36(12) . . y N30 Mn1 N1 86.59(12) . . y N4 Mn1 N1 139.52(11) . . y O210 Mn1 N6 79.46(11) . . y N3 Mn1 N6 115.57(12) . . y N5 Mn1 N6 68.33(11) . . y N30 Mn1 N6 143.24(12) . . y N4 Mn1 N6 139.77(11) . . y N1 Mn1 N6 75.84(10) . . y N200 Mn2 N8 163.13(13) . . y N200 Mn2 N10 86.46(13) . . y N8 Mn2 N10 88.39(12) . . y N200 Mn2 N40 85.57(13) . . y N8 Mn2 N40 89.07(12) . . y N10 Mn2 N40 143.48(12) . . y N200 Mn2 N9 88.83(13) . . y N8 Mn2 N9 74.30(12) . . y N10 Mn2 N9 72.14(11) . . y N40 Mn2 N9 72.12(12) . . y N200 Mn2 N7 125.83(12) . . y N8 Mn2 N7 69.67(11) . . y N10 Mn2 N7 125.87(11) . . y N40 Mn2 N7 86.83(11) . . y N9 Mn2 N7 138.31(11) . . y N200 Mn2 N2 81.09(12) . . y N8 Mn2 N2 111.93(12) . . y N10 Mn2 N2 69.02(11) . . y N40 Mn2 N2 143.91(12) . . y N9 Mn2 N2 140.32(11) . . y N7 Mn2 N2 74.54(10) . . y C5 N1 N2 119.9(3) . . ? C5 N1 Mn1 113.1(2) . . ? N2 N1 Mn1 126.5(2) . . ? N1 N2 C2 118.8(3) . . ? N1 N2 Mn2 128.6(2) . . ? C2 N2 Mn2 112.4(2) . . ? N2 C2 C3 123.4(4) . . ? N2 C2 C21 115.9(3) . . ? C3 C2 C21 120.5(3) . . ? C4 C3 C2 117.2(4) . . ? C4 C3 H3 121.4 . . ? C2 C3 H3 121.4 . . ? C3 C4 C5 117.7(4) . . ? C3 C4 H4 121.1 . . ? C5 C4 H4 121.1 . . ? N1 C5 C4 122.8(4) . . ? N1 C5 C6 116.0(3) . . ? C4 C5 C6 121.2(4) . . ? N3 C6 C5 119.5(4) . . ? N3 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 N3 C7 121.4(4) . . ? C6 N3 Mn1 121.3(3) . . ? C7 N3 Mn1 116.7(3) . . ? N3 C7 C8 108.1(4) . . ? N3 C7 H7A 110.1 . . ? C8 C7 H7A 110.1 . . ? N3 C7 H7B 110.1 . . ? C8 C7 H7B 110.1 . . ? H7A C7 H7B 108.4 . . ? N4 C8 C7 113.2(4) . . ? N4 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? N4 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C30 N4 C9 110.9(3) . . ? C30 N4 C8 110.3(3) . . ? C9 N4 C8 112.1(3) . . ? C30 N4 Mn1 105.1(3) . . ? C9 N4 Mn1 109.8(2) . . ? C8 N4 Mn1 108.3(2) . . ? N4 C30 C31 112.3(4) . . ? N4 C30 H30A 109.2 . . ? C31 C30 H30A 109.2 . . ? N4 C30 H30B 109.2 . . ? C31 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? N30 C31 C32 122.2(4) . . ? N30 C31 C30 117.5(4) . . ? C32 C31 C30 120.3(4) . . ? C31 C32 C33 119.5(5) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C34 C33 C32 118.6(5) . . ? C34 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? C35 C34 C33 118.5(4) . . ? C35 C34 H34 120.7 . . ? C33 C34 H34 120.7 . . ? N30 C35 C34 123.4(4) . . ? N30 C35 H35 118.3 . . ? C34 C35 H35 118.3 . . ? C31 N30 C35 117.5(4) . . ? C31 N30 Mn1 114.1(3) . . ? C35 N30 Mn1 127.6(3) . . ? N4 C9 C10 112.7(4) . . ? N4 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? N4 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N5 C10 C9 108.3(3) . . ? N5 C10 H10A 110.0 . . ? C9 C10 H10A 110.0 . . ? N5 C10 H10B 110.0 . . ? C9 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C11 N5 C10 118.8(4) . . ? C11 N5 Mn1 122.8(3) . . ? C10 N5 Mn1 118.5(3) . . ? N5 C11 C12 119.2(4) . . ? N5 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C12 N6 N7 119.8(3) . . ? C12 N6 Mn1 113.3(2) . . ? N7 N6 Mn1 126.6(2) . . ? N6 N7 C15 119.2(3) . . ? N6 N7 Mn2 127.4(2) . . ? C15 N7 Mn2 112.9(2) . . ? N6 C12 C13 122.6(4) . . ? N6 C12 C11 115.7(3) . . ? C13 C12 C11 121.6(4) . . ? C14 C13 C12 117.7(4) . . ? C14 C13 H13 121.2 . . ? C12 C13 H13 121.2 . . ? C13 C14 C15 117.6(4) . . ? C13 C14 H14 121.2 . . ? C15 C14 H14 121.2 . . ? N7 C15 C14 123.0(4) . . ? N7 C15 C16 115.2(3) . . ? C14 C15 C16 121.7(4) . . ? N8 C16 C15 119.3(4) . . ? N8 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 N8 C17 120.4(3) . . ? C16 N8 Mn2 122.6(3) . . ? C17 N8 Mn2 117.0(2) . . ? N8 C17 C18 108.3(3) . . ? N8 C17 H17A 110.0 . . ? C18 C17 H17A 110.0 . . ? N8 C17 H17B 110.0 . . ? C18 C17 H17B 110.0 . . ? H17A C17 H17B 108.4 . . ? N9 C18 C17 113.5(3) . . ? N9 C18 H18A 108.9 . . ? C17 C18 H18A 108.9 . . ? N9 C18 H18B 108.9 . . ? C17 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C40 N9 C19 110.5(3) . . ? C40 N9 C18 109.5(3) . . ? C19 N9 C18 112.6(3) . . ? C40 N9 Mn2 106.8(2) . . ? C19 N9 Mn2 108.6(2) . . ? C18 N9 Mn2 108.6(2) . . ? N9 C40 C41 111.7(3) . . ? N9 C40 H40A 109.3 . . ? C41 C40 H40A 109.3 . . ? N9 C40 H40B 109.3 . . ? C41 C40 H40B 109.3 . . ? H40A C40 H40B 108.0 . . ? N40 C41 C42 122.8(4) . . ? N40 C41 C40 117.4(4) . . ? C42 C41 C40 119.8(4) . . ? C41 C42 C43 118.9(4) . . ? C41 C42 H42 120.6 . . ? C43 C42 H42 120.6 . . ? C44 C43 C42 119.2(4) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C43 C44 C45 118.5(4) . . ? C43 C44 H44 120.8 . . ? C45 C44 H44 120.8 . . ? N40 C45 C44 123.7(4) . . ? N40 C45 H45 118.1 . . ? C44 C45 H45 118.1 . . ? C45 N40 C41 116.9(4) . . ? C45 N40 Mn2 125.6(3) . . ? C41 N40 Mn2 117.5(3) . . ? N9 C19 C20 111.7(3) . . ? N9 C19 H19A 109.3 . . ? C20 C19 H19A 109.3 . . ? N9 C19 H19B 109.3 . . ? C20 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? N10 C20 C19 108.6(3) . . ? N10 C20 H20A 110.0 . . ? C19 C20 H20A 110.0 . . ? N10 C20 H20B 110.0 . . ? C19 C20 H20B 110.0 . . ? H20A C20 H20B 108.4 . . ? C21 N10 C20 118.7(3) . . ? C21 N10 Mn2 121.4(3) . . ? C20 N10 Mn2 119.9(2) . . ? N10 C21 C2 120.0(4) . . ? N10 C21 H21 120.0 . . ? C2 C21 H21 120.0 . . ? Mn1 O210 H21X 113.9 . . ? Mn1 O210 H21Y 133.5 . . ? H21X O210 H21Y 110.8 . . ? C200 N200 Mn2 159.5(4) . . ? N200 C200 C201 176.0(6) . . ? C200 C201 H20C 109.5 . . ? C200 C201 H20D 109.5 . . ? H20C C201 H20D 109.5 . . ? C200 C201 H20E 109.5 . . ? H20C C201 H20E 109.5 . . ? H20D C201 H20E 109.5 . . ? O14 Cl1 O11 109.8(2) . . ? O14 Cl1 O13 108.5(2) . . ? O11 Cl1 O13 110.4(2) . . ? O14 Cl1 O12 109.8(2) . . ? O11 Cl1 O12 109.8(2) . . ? O13 Cl1 O12 108.5(2) . . ? O24 Cl2 O23 110.4(2) . . ? O24 Cl2 O21 108.7(3) . . ? O23 Cl2 O21 108.5(3) . . ? O24 Cl2 O22 110.0(2) . . ? O23 Cl2 O22 110.0(2) . . ? O21 Cl2 O22 109.2(2) . . ? O34 Cl3 O33 112.5(4) . . ? O34 Cl3 O32 110.1(3) . . ? O33 Cl3 O32 110.5(2) . . ? O34 Cl3 O31 108.6(4) . . ? O33 Cl3 O31 106.7(3) . . ? O32 Cl3 O31 108.2(2) . . ? O47 Cl4 O44 142.4(6) . . ? O47 Cl4 O43 37.9(5) . . ? O44 Cl4 O43 115.1(4) . . ? O47 Cl4 O46 115.6(7) . . ? O44 Cl4 O46 39.8(5) . . ? O43 Cl4 O46 114.2(5) . . ? O47 Cl4 O41 108.6(5) . . ? O44 Cl4 O41 108.6(4) . . ? O43 Cl4 O41 118.4(4) . . ? O46 Cl4 O41 127.2(5) . . ? O47 Cl4 O42 70.8(5) . . ? O44 Cl4 O42 107.6(4) . . ? O43 Cl4 O42 104.6(5) . . ? O46 Cl4 O42 69.7(6) . . ? O41 Cl4 O42 100.9(3) . . ? O47 Cl4 O45 101.8(6) . . ? O44 Cl4 O45 67.3(5) . . ? O43 Cl4 O45 64.5(5) . . ? O46 Cl4 O45 100.0(6) . . ? O41 Cl4 O45 97.8(4) . . ? O42 Cl4 O45 161.3(4) . . ? N210 C210 C211 175.4(8) . . ? C210 C211 H21A 109.5 . . ? C210 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C210 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? N220 C220 C221 178.5(6) . . ? C220 C221 H22A 109.5 . . ? C220 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? C220 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? N230 C230 C231 178.2(8) . . ? C230 C231 H23A 109.5 . . ? C230 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? C230 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 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 O210 Mn1 N1 C5 -164.9(3) . . . . ? N3 Mn1 N1 C5 2.9(3) . . . . ? N5 Mn1 N1 C5 77.6(3) . . . . ? N30 Mn1 N1 C5 -85.2(3) . . . . ? N4 Mn1 N1 C5 -29.2(4) . . . . ? N6 Mn1 N1 C5 127.3(3) . . . . ? O210 Mn1 N1 N2 7.1(3) . . . . ? N3 Mn1 N1 N2 174.9(3) . . . . ? N5 Mn1 N1 N2 -110.5(3) . . . . ? N30 Mn1 N1 N2 86.7(3) . . . . ? N4 Mn1 N1 N2 142.7(3) . . . . ? N6 Mn1 N1 N2 -60.7(3) . . . . ? C5 N1 N2 C2 1.1(5) . . . . ? Mn1 N1 N2 C2 -170.4(3) . . . . ? C5 N1 N2 Mn2 -173.5(3) . . . . ? Mn1 N1 N2 Mn2 15.0(4) . . . . ? N200 Mn2 N2 N1 -85.8(3) . . . . ? N8 Mn2 N2 N1 105.3(3) . . . . ? N10 Mn2 N2 N1 -175.5(3) . . . . ? N40 Mn2 N2 N1 -16.2(4) . . . . ? N9 Mn2 N2 N1 -163.1(3) . . . . ? N7 Mn2 N2 N1 45.3(3) . . . . ? N200 Mn2 N2 C2 99.3(3) . . . . ? N8 Mn2 N2 C2 -69.6(3) . . . . ? N10 Mn2 N2 C2 9.7(2) . . . . ? N40 Mn2 N2 C2 168.9(2) . . . . ? N9 Mn2 N2 C2 22.1(3) . . . . ? N7 Mn2 N2 C2 -129.6(3) . . . . ? N1 N2 C2 C3 -2.5(6) . . . . ? Mn2 N2 C2 C3 172.9(3) . . . . ? N1 N2 C2 C21 172.8(3) . . . . ? Mn2 N2 C2 C21 -11.7(4) . . . . ? N2 C2 C3 C4 1.2(6) . . . . ? C21 C2 C3 C4 -174.0(4) . . . . ? C2 C3 C4 C5 1.5(6) . . . . ? N2 N1 C5 C4 1.7(6) . . . . ? Mn1 N1 C5 C4 174.2(3) . . . . ? N2 N1 C5 C6 -175.5(3) . . . . ? Mn1 N1 C5 C6 -2.9(4) . . . . ? C3 C4 C5 N1 -3.0(6) . . . . ? C3 C4 C5 C6 174.0(4) . . . . ? N1 C5 C6 N3 0.8(6) . . . . ? C4 C5 C6 N3 -176.4(4) . . . . ? C5 C6 N3 C7 173.4(4) . . . . ? C5 C6 N3 Mn1 2.3(6) . . . . ? O210 Mn1 N3 C6 136.8(4) . . . . ? N5 Mn1 N3 C6 -130.9(4) . . . . ? N30 Mn1 N3 C6 84.7(4) . . . . ? N4 Mn1 N3 C6 156.3(4) . . . . ? N1 Mn1 N3 C6 -2.7(3) . . . . ? N6 Mn1 N3 C6 -65.2(4) . . . . ? O210 Mn1 N3 C7 -34.8(6) . . . . ? N5 Mn1 N3 C7 57.5(3) . . . . ? N30 Mn1 N3 C7 -86.9(3) . . . . ? N4 Mn1 N3 C7 -15.2(3) . . . . ? N1 Mn1 N3 C7 -174.3(3) . . . . ? N6 Mn1 N3 C7 123.2(3) . . . . ? C6 N3 C7 C8 -133.3(4) . . . . ? Mn1 N3 C7 C8 38.3(4) . . . . ? N3 C7 C8 N4 -48.8(5) . . . . ? C7 C8 N4 C30 150.1(4) . . . . ? C7 C8 N4 C9 -85.7(4) . . . . ? C7 C8 N4 Mn1 35.6(4) . . . . ? O210 Mn1 N4 C30 45.7(3) . . . . ? N3 Mn1 N4 C30 -129.0(3) . . . . ? N5 Mn1 N4 C30 136.8(3) . . . . ? N30 Mn1 N4 C30 -37.0(2) . . . . ? N1 Mn1 N4 C30 -97.9(3) . . . . ? N6 Mn1 N4 C30 118.9(3) . . . . ? O210 Mn1 N4 C9 -73.7(3) . . . . ? N3 Mn1 N4 C9 111.6(3) . . . . ? N5 Mn1 N4 C9 17.4(3) . . . . ? N30 Mn1 N4 C9 -156.4(3) . . . . ? N1 Mn1 N4 C9 142.8(3) . . . . ? N6 Mn1 N4 C9 -0.5(4) . . . . ? O210 Mn1 N4 C8 163.5(3) . . . . ? N3 Mn1 N4 C8 -11.1(3) . . . . ? N5 Mn1 N4 C8 -105.4(3) . . . . ? N30 Mn1 N4 C8 80.8(3) . . . . ? N1 Mn1 N4 C8 20.0(4) . . . . ? N6 Mn1 N4 C8 -123.3(3) . . . . ? C9 N4 C30 C31 161.9(3) . . . . ? C8 N4 C30 C31 -73.3(4) . . . . ? Mn1 N4 C30 C31 43.3(4) . . . . ? N4 C30 C31 N30 -21.9(6) . . . . ? N4 C30 C31 C32 157.8(4) . . . . ? N30 C31 C32 C33 3.3(7) . . . . ? C30 C31 C32 C33 -176.3(4) . . . . ? C31 C32 C33 C34 0.7(7) . . . . ? C32 C33 C34 C35 -3.4(7) . . . . ? C33 C34 C35 N30 2.4(7) . . . . ? C32 C31 N30 C35 -4.4(6) . . . . ? C30 C31 N30 C35 175.3(4) . . . . ? C32 C31 N30 Mn1 166.4(3) . . . . ? C30 C31 N30 Mn1 -13.9(5) . . . . ? C34 C35 N30 C31 1.5(7) . . . . ? C34 C35 N30 Mn1 -167.9(3) . . . . ? O210 Mn1 N30 C31 -63.7(3) . . . . ? N3 Mn1 N30 C31 103.6(3) . . . . ? N5 Mn1 N30 C31 18.2(4) . . . . ? N4 Mn1 N30 C31 28.4(3) . . . . ? N1 Mn1 N30 C31 173.8(3) . . . . ? N6 Mn1 N30 C31 -125.5(3) . . . . ? O210 Mn1 N30 C35 106.1(4) . . . . ? N3 Mn1 N30 C35 -86.6(4) . . . . ? N5 Mn1 N30 C35 -172.1(3) . . . . ? N4 Mn1 N30 C35 -161.9(4) . . . . ? N1 Mn1 N30 C35 -16.5(4) . . . . ? N6 Mn1 N30 C35 44.2(5) . . . . ? C30 N4 C9 C10 -156.1(4) . . . . ? C8 N4 C9 C10 80.1(4) . . . . ? Mn1 N4 C9 C10 -40.4(4) . . . . ? N4 C9 C10 N5 46.6(5) . . . . ? C9 C10 N5 C11 148.5(4) . . . . ? C9 C10 N5 Mn1 -30.7(4) . . . . ? O210 Mn1 N5 C11 -82.0(3) . . . . ? N3 Mn1 N5 C11 114.1(3) . . . . ? N30 Mn1 N5 C11 -161.3(3) . . . . ? N4 Mn1 N5 C11 -171.4(4) . . . . ? N1 Mn1 N5 C11 49.0(4) . . . . ? N6 Mn1 N5 C11 -3.8(3) . . . . ? O210 Mn1 N5 C10 97.1(3) . . . . ? N3 Mn1 N5 C10 -66.8(3) . . . . ? N30 Mn1 N5 C10 17.8(4) . . . . ? N4 Mn1 N5 C10 7.7(3) . . . . ? N1 Mn1 N5 C10 -131.8(3) . . . . ? N6 Mn1 N5 C10 175.4(3) . . . . ? C10 N5 C11 C12 -179.0(4) . . . . ? Mn1 N5 C11 C12 0.2(5) . . . . ? O210 Mn1 N6 C12 102.4(3) . . . . ? N3 Mn1 N6 C12 -71.6(3) . . . . ? N5 Mn1 N6 C12 7.1(3) . . . . ? N30 Mn1 N6 C12 165.2(3) . . . . ? N4 Mn1 N6 C12 25.5(4) . . . . ? N1 Mn1 N6 C12 -130.9(3) . . . . ? O210 Mn1 N6 N7 -83.7(3) . . . . ? N3 Mn1 N6 N7 102.3(3) . . . . ? N5 Mn1 N6 N7 -179.0(3) . . . . ? N30 Mn1 N6 N7 -20.9(4) . . . . ? N4 Mn1 N6 N7 -160.6(3) . . . . ? N1 Mn1 N6 N7 43.0(3) . . . . ? C12 N6 N7 C15 2.9(5) . . . . ? Mn1 N6 N7 C15 -170.6(3) . . . . ? C12 N6 N7 Mn2 -168.0(3) . . . . ? Mn1 N6 N7 Mn2 18.5(4) . . . . ? N200 Mn2 N7 N6 3.6(3) . . . . ? N8 Mn2 N7 N6 176.0(3) . . . . ? N10 Mn2 N7 N6 -111.7(3) . . . . ? N40 Mn2 N7 N6 85.8(3) . . . . ? N9 Mn2 N7 N6 144.2(3) . . . . ? N2 Mn2 N7 N6 -62.9(3) . . . . ? N200 Mn2 N7 C15 -167.8(2) . . . . ? N8 Mn2 N7 C15 4.6(2) . . . . ? N10 Mn2 N7 C15 76.9(3) . . . . ? N40 Mn2 N7 C15 -85.6(3) . . . . ? N9 Mn2 N7 C15 -27.2(3) . . . . ? N2 Mn2 N7 C15 125.7(3) . . . . ? N7 N6 C12 C13 -3.1(6) . . . . ? Mn1 N6 C12 C13 171.2(3) . . . . ? N7 N6 C12 C11 176.2(3) . . . . ? Mn1 N6 C12 C11 -9.5(4) . . . . ? N5 C11 C12 N6 6.9(5) . . . . ? N5 C11 C12 C13 -173.8(4) . . . . ? N6 C12 C13 C14 0.8(6) . . . . ? C11 C12 C13 C14 -178.4(4) . . . . ? C12 C13 C14 C15 1.5(6) . . . . ? N6 N7 C15 C14 -0.6(5) . . . . ? Mn2 N7 C15 C14 171.5(3) . . . . ? N6 N7 C15 C16 -178.2(3) . . . . ? Mn2 N7 C15 C16 -6.0(4) . . . . ? C13 C14 C15 N7 -1.6(6) . . . . ? C13 C14 C15 C16 175.8(4) . . . . ? N7 C15 C16 N8 4.3(5) . . . . ? C14 C15 C16 N8 -173.3(4) . . . . ? C15 C16 N8 C17 176.6(3) . . . . ? C15 C16 N8 Mn2 0.3(5) . . . . ? N200 Mn2 N8 C16 155.8(4) . . . . ? N10 Mn2 N8 C16 -132.0(3) . . . . ? N40 Mn2 N8 C16 84.4(3) . . . . ? N9 Mn2 N8 C16 156.1(3) . . . . ? N7 Mn2 N8 C16 -2.6(3) . . . . ? N2 Mn2 N8 C16 -65.5(3) . . . . ? N200 Mn2 N8 C17 -20.7(6) . . . . ? N10 Mn2 N8 C17 51.5(3) . . . . ? N40 Mn2 N8 C17 -92.1(3) . . . . ? N9 Mn2 N8 C17 -20.4(3) . . . . ? N7 Mn2 N8 C17 -179.0(3) . . . . ? N2 Mn2 N8 C17 118.1(3) . . . . ? C16 N8 C17 C18 -134.0(4) . . . . ? Mn2 N8 C17 C18 42.5(4) . . . . ? N8 C17 C18 N9 -47.4(4) . . . . ? C17 C18 N9 C40 146.5(3) . . . . ? C17 C18 N9 C19 -90.2(4) . . . . ? C17 C18 N9 Mn2 30.2(4) . . . . ? N200 Mn2 N9 C40 56.0(3) . . . . ? N8 Mn2 N9 C40 -123.9(3) . . . . ? N10 Mn2 N9 C40 142.6(3) . . . . ? N40 Mn2 N9 C40 -29.7(3) . . . . ? N7 Mn2 N9 C40 -93.0(3) . . . . ? N2 Mn2 N9 C40 130.5(3) . . . . ? N200 Mn2 N9 C19 -63.2(3) . . . . ? N8 Mn2 N9 C19 116.9(3) . . . . ? N10 Mn2 N9 C19 23.5(3) . . . . ? N40 Mn2 N9 C19 -148.9(3) . . . . ? N7 Mn2 N9 C19 147.8(2) . . . . ? N2 Mn2 N9 C19 11.3(3) . . . . ? N200 Mn2 N9 C18 174.0(3) . . . . ? N8 Mn2 N9 C18 -5.9(2) . . . . ? N10 Mn2 N9 C18 -99.3(3) . . . . ? N40 Mn2 N9 C18 88.3(3) . . . . ? N7 Mn2 N9 C18 25.0(3) . . . . ? N2 Mn2 N9 C18 -111.5(3) . . . . ? C19 N9 C40 C41 159.2(4) . . . . ? C18 N9 C40 C41 -76.3(4) . . . . ? Mn2 N9 C40 C41 41.2(4) . . . . ? N9 C40 C41 N40 -31.7(6) . . . . ? N9 C40 C41 C42 150.7(4) . . . . ? N40 C41 C42 C43 -1.5(7) . . . . ? C40 C41 C42 C43 176.0(4) . . . . ? C41 C42 C43 C44 0.5(7) . . . . ? C42 C43 C44 C45 1.0(6) . . . . ? C43 C44 C45 N40 -1.7(6) . . . . ? C44 C45 N40 C41 0.8(6) . . . . ? C44 C45 N40 Mn2 -178.7(3) . . . . ? C42 C41 N40 C45 0.9(6) . . . . ? C40 C41 N40 C45 -176.7(4) . . . . ? C42 C41 N40 Mn2 -179.6(3) . . . . ? C40 C41 N40 Mn2 2.8(5) . . . . ? N200 Mn2 N40 C45 104.4(3) . . . . ? N8 Mn2 N40 C45 -91.6(3) . . . . ? N10 Mn2 N40 C45 -177.6(3) . . . . ? N9 Mn2 N40 C45 -165.4(4) . . . . ? N7 Mn2 N40 C45 -21.9(3) . . . . ? N2 Mn2 N40 C45 36.2(4) . . . . ? N200 Mn2 N40 C41 -75.0(3) . . . . ? N8 Mn2 N40 C41 88.9(3) . . . . ? N10 Mn2 N40 C41 2.9(4) . . . . ? N9 Mn2 N40 C41 15.1(3) . . . . ? N7 Mn2 N40 C41 158.6(3) . . . . ? N2 Mn2 N40 C41 -143.3(3) . . . . ? C40 N9 C19 C20 -162.4(3) . . . . ? C18 N9 C19 C20 74.8(4) . . . . ? Mn2 N9 C19 C20 -45.5(4) . . . . ? N9 C19 C20 N10 46.6(4) . . . . ? C19 C20 N10 C21 154.6(4) . . . . ? C19 C20 N10 Mn2 -25.0(4) . . . . ? N200 Mn2 N10 C21 -88.6(3) . . . . ? N8 Mn2 N10 C21 107.5(3) . . . . ? N40 Mn2 N10 C21 -166.2(3) . . . . ? N9 Mn2 N10 C21 -178.5(3) . . . . ? N7 Mn2 N10 C21 44.2(4) . . . . ? N2 Mn2 N10 C21 -6.7(3) . . . . ? N200 Mn2 N10 C20 91.1(3) . . . . ? N8 Mn2 N10 C20 -72.8(3) . . . . ? N40 Mn2 N10 C20 13.5(4) . . . . ? N9 Mn2 N10 C20 1.2(3) . . . . ? N7 Mn2 N10 C20 -136.1(3) . . . . ? N2 Mn2 N10 C20 172.9(3) . . . . ? C20 N10 C21 C2 -176.5(3) . . . . ? Mn2 N10 C21 C2 3.2(5) . . . . ? N2 C2 C21 N10 6.7(5) . . . . ? C3 C2 C21 N10 -177.8(4) . . . . ? N8 Mn2 N200 C200 10.5(15) . . . . ? N10 Mn2 N200 C200 -62.0(12) . . . . ? N40 Mn2 N200 C200 82.4(12) . . . . ? N9 Mn2 N200 C200 10.2(12) . . . . ? N7 Mn2 N200 C200 165.2(12) . . . . ? N2 Mn2 N200 C200 -131.3(13) . . . . ? Mn2 N200 C200 C201 78(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O210 H21X O11 1.00 1.90 2.816(5) 150.5 . O210 H21Y O42 0.85 1.89 2.680(6) 154.0 . O210 H21Y O46 0.85 2.06 2.843(12) 153.1 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.034 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.091