# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ni-123 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C22 H26 Br2 Mn N4 O2), C8 N4 Ni S4 ' _chemical_formula_sum 'C52 H52 Br4 Mn2 N12 Ni O4 S4' _chemical_formula_weight 1525.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1908(9) _cell_length_b 9.9971(11) _cell_length_c 18.358(2) _cell_angle_alpha 78.0250(10) _cell_angle_beta 79.554(2) _cell_angle_gamma 83.196(2) _cell_volume 1441.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4743 _cell_measurement_theta_min 2.185 _cell_measurement_theta_max 27.5185 _exptl_crystal_description plate-like _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 3.729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2572 _exptl_absorpt_correction_T_max 0.7068 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11687 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_unetI/netI 0.0545 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5592 _reflns_number_gt 4774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0960P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5592 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.1329 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 Br1 Br 0.22755(5) 0.70843(4) 1.06611(2) 0.02407(14) Uani 1 1 d . . . Br2 Br 1.28205(5) 1.26396(4) 0.93838(2) 0.02180(14) Uani 1 1 d . . . C1 C 0.5807(4) 0.7587(4) 0.83188(19) 0.0136(7) Uani 1 1 d . . . C2 C 0.5000(5) 0.6384(4) 0.8611(2) 0.0187(8) Uani 1 1 d . . . H2 H 0.5158 0.5669 0.8329 0.022 Uiso 1 1 calc R . . C3 C 0.3975(5) 0.6226(4) 0.9306(2) 0.0197(8) Uani 1 1 d . . . H3 H 0.3466 0.5393 0.9506 0.024 Uiso 1 1 calc R . . C4 C 0.3690(4) 0.7283(4) 0.9710(2) 0.0179(8) Uani 1 1 d . . . C5 C 0.4393(4) 0.8509(4) 0.9417(2) 0.0160(7) Uani 1 1 d . . . H5 H 0.4153 0.9241 0.9688 0.019 Uiso 1 1 calc R . . C6 C 0.5464(4) 0.8674(4) 0.8720(2) 0.0153(7) Uani 1 1 d . . . C7 C 0.6009(4) 1.0017(4) 0.83918(19) 0.0149(7) Uani 1 1 d . . . H7 H 0.5443 1.0774 0.8598 0.018 Uiso 1 1 calc R . . C8 C 0.7303(5) 1.1695(4) 0.7430(2) 0.0180(8) Uani 1 1 d . . . H8A H 0.8449 1.1966 0.7375 0.022 Uiso 1 1 calc R . . H8B H 0.6538 1.2312 0.7720 0.022 Uiso 1 1 calc R . . C9 C 0.6818(5) 1.1826(4) 0.6657(2) 0.0219(8) Uani 1 1 d . . . H9A H 0.6709 1.2811 0.6424 0.026 Uiso 1 1 calc R . . H9B H 0.5711 1.1474 0.6723 0.026 Uiso 1 1 calc R . . C10 C 0.8032(5) 1.1073(4) 0.6117(2) 0.0215(8) Uani 1 1 d . . . H10A H 0.7680 1.1300 0.5614 0.026 Uiso 1 1 calc R . . H10B H 0.9154 1.1393 0.6063 0.026 Uiso 1 1 calc R . . C11 C 0.9338(5) 0.8850(4) 0.5849(2) 0.0227(8) Uani 1 1 d . . . H11A H 1.0418 0.9259 0.5748 0.027 Uiso 1 1 calc R . . H11B H 0.8921 0.8962 0.5364 0.027 Uiso 1 1 calc R . . C12 C 0.9564(5) 0.7360(4) 0.6190(2) 0.0228(8) Uani 1 1 d . . . H12A H 0.8510 0.6927 0.6247 0.027 Uiso 1 1 calc R . . H12B H 1.0435 0.6886 0.5861 0.027 Uiso 1 1 calc R . . C13 C 1.0061(5) 0.5814(4) 0.7363(2) 0.0226(8) Uani 1 1 d . . . H13A H 1.0828 0.5215 0.7062 0.027 Uiso 1 1 calc R . . H13B H 0.8927 0.5511 0.7430 0.027 Uiso 1 1 calc R . . C14 C 1.0585(5) 0.5643(4) 0.8133(2) 0.0206(8) Uani 1 1 d . . . H14A H 1.1707 0.5970 0.8065 0.025 Uiso 1 1 calc R . . H14B H 1.0667 0.4654 0.8361 0.025 Uiso 1 1 calc R . . C15 C 0.9401(5) 0.6408(4) 0.8678(2) 0.0182(8) Uani 1 1 d . . . H15A H 0.8255 0.6142 0.8724 0.022 Uiso 1 1 calc R . . H15B H 0.9737 0.6159 0.9184 0.022 Uiso 1 1 calc R . . C16 C 1.0193(4) 0.8551(4) 0.8763(2) 0.0166(7) Uani 1 1 d . . . H16 H 1.0401 0.8108 0.9252 0.020 Uiso 1 1 calc R . . C17 C 1.0747(4) 0.9897(4) 0.8477(2) 0.0145(7) Uani 1 1 d . . . C18 C 1.1303(4) 1.0579(4) 0.89701(19) 0.0148(7) Uani 1 1 d . . . H18 H 1.1153 1.0212 0.9496 0.018 Uiso 1 1 calc R . . C19 C 1.2058(4) 1.1766(4) 0.8696(2) 0.0149(7) Uani 1 1 d . . . C20 C 1.2358(4) 1.2303(4) 0.7928(2) 0.0169(7) Uani 1 1 d . . . H20 H 1.2918 1.3116 0.7745 0.020 Uiso 1 1 calc R . . C21 C 1.1830(5) 1.1639(4) 0.7430(2) 0.0167(7) Uani 1 1 d . . . H21 H 1.2036 1.2001 0.6904 0.020 Uiso 1 1 calc R . . C22 C 1.0993(4) 1.0434(4) 0.76930(19) 0.0142(7) Uani 1 1 d . . . C23 C 0.4849(5) 0.5908(4) 0.6534(2) 0.0230(8) Uani 1 1 d . . . C24 C 0.5137(5) 0.7051(4) 0.5922(2) 0.0186(8) Uani 1 1 d . . . C25 C 0.6121(5) 0.6911(4) 0.5255(2) 0.0197(8) Uani 1 1 d . . . C26 C 0.6889(5) 0.5604(4) 0.5115(2) 0.0241(9) Uani 1 1 d . . . Mn1 Mn 0.86746(6) 0.87631(5) 0.74331(3) 0.01265(15) Uani 1 1 d . . . N1 N 0.7213(4) 1.0260(3) 0.78366(16) 0.0146(6) Uani 1 1 d . . . N2 N 0.8123(4) 0.9556(3) 0.63815(16) 0.0166(6) Uani 1 1 d . . . H28 H 0.7081 0.9283 0.6373 0.020 Uiso 1 1 calc R . . N3 N 1.0068(4) 0.7250(3) 0.69410(16) 0.0174(6) Uani 1 1 d . . . H27 H 1.1168 0.7470 0.6850 0.021 Uiso 1 1 calc R . . N4 N 0.9432(4) 0.7899(3) 0.84051(16) 0.0144(6) Uani 1 1 d . . . N5 N 0.4605(5) 0.5017(4) 0.7025(2) 0.0325(9) Uani 1 1 d . . . N6 N 0.7490(5) 0.4568(4) 0.4992(2) 0.0380(10) Uani 1 1 d . . . Ni1 Ni 0.5000 1.0000 0.5000 0.01619(17) Uani 1 2 d S . . O1 O 0.6848(3) 0.7680(3) 0.76659(13) 0.0159(5) Uani 1 1 d . . . O2 O 1.0495(3) 0.9847(3) 0.72000(13) 0.0151(5) Uani 1 1 d . . . S1 S 0.64854(13) 0.83270(10) 0.45417(5) 0.0218(2) Uani 1 1 d . . . S2 S 0.42075(12) 0.86490(10) 0.60725(5) 0.0196(2) 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 Br1 0.0204(2) 0.0273(2) 0.0208(2) 0.00016(16) 0.00259(15) -0.00478(17) Br2 0.0240(2) 0.0222(2) 0.0232(2) -0.00684(16) -0.01035(16) -0.00339(16) C1 0.0088(16) 0.0158(18) 0.0160(16) 0.0001(13) -0.0066(13) 0.0014(14) C2 0.0160(19) 0.0154(19) 0.0254(19) -0.0037(15) -0.0050(15) -0.0024(15) C3 0.0154(18) 0.020(2) 0.0233(19) -0.0003(15) -0.0039(14) -0.0067(15) C4 0.0108(17) 0.023(2) 0.0188(18) -0.0009(14) -0.0031(13) 0.0004(15) C5 0.0116(17) 0.0155(18) 0.0201(17) -0.0008(14) -0.0064(13) 0.0029(14) C6 0.0126(17) 0.0166(19) 0.0173(17) -0.0009(14) -0.0075(13) -0.0006(14) C7 0.0157(18) 0.0161(18) 0.0144(17) -0.0043(13) -0.0068(13) 0.0014(14) C8 0.0185(19) 0.0131(18) 0.0210(18) 0.0017(14) -0.0055(14) -0.0010(15) C9 0.021(2) 0.021(2) 0.0215(19) 0.0025(15) -0.0071(15) 0.0031(16) C10 0.022(2) 0.025(2) 0.0164(18) 0.0017(15) -0.0059(14) -0.0042(17) C11 0.021(2) 0.033(2) 0.0146(18) -0.0046(15) -0.0049(14) 0.0005(17) C12 0.024(2) 0.030(2) 0.0168(18) -0.0095(16) -0.0037(15) -0.0034(17) C13 0.026(2) 0.018(2) 0.0242(19) -0.0058(15) -0.0055(16) 0.0016(16) C14 0.0187(19) 0.0169(19) 0.026(2) -0.0027(15) -0.0058(15) 0.0018(15) C15 0.0188(19) 0.0166(19) 0.0173(17) 0.0024(14) -0.0049(14) -0.0001(15) C16 0.0129(17) 0.022(2) 0.0131(17) 0.0014(14) -0.0024(13) -0.0002(15) C17 0.0094(17) 0.0140(18) 0.0199(18) -0.0011(14) -0.0048(13) -0.0006(14) C18 0.0111(17) 0.0198(19) 0.0138(16) -0.0010(13) -0.0058(13) -0.0003(14) C19 0.0096(16) 0.0173(18) 0.0207(17) -0.0082(14) -0.0060(13) 0.0014(14) C20 0.0128(17) 0.0139(18) 0.0229(18) -0.0013(14) -0.0045(14) 0.0020(14) C21 0.0144(18) 0.0207(19) 0.0132(16) 0.0005(14) -0.0024(13) -0.0009(15) C22 0.0086(16) 0.0160(18) 0.0178(17) -0.0021(13) -0.0051(13) 0.0027(14) C23 0.024(2) 0.024(2) 0.0219(19) -0.0060(17) -0.0022(15) -0.0029(17) C24 0.0170(19) 0.018(2) 0.0201(18) -0.0010(15) -0.0037(14) -0.0031(15) C25 0.0172(19) 0.025(2) 0.0183(18) -0.0055(15) -0.0051(14) -0.0003(16) C26 0.024(2) 0.027(2) 0.0205(19) -0.0038(16) -0.0002(15) -0.0043(18) Mn1 0.0107(3) 0.0147(3) 0.0127(3) -0.0011(2) -0.0040(2) -0.0009(2) N1 0.0161(15) 0.0134(15) 0.0153(14) -0.0011(11) -0.0066(12) -0.0018(12) N2 0.0158(15) 0.0219(17) 0.0127(14) -0.0018(12) -0.0053(11) -0.0022(13) N3 0.0141(15) 0.0216(17) 0.0180(15) -0.0044(12) -0.0040(12) -0.0047(13) N4 0.0117(15) 0.0141(15) 0.0168(14) -0.0015(11) -0.0031(11) 0.0000(12) N5 0.039(2) 0.0228(19) 0.032(2) -0.0038(16) 0.0056(16) -0.0074(16) N6 0.043(2) 0.026(2) 0.043(2) -0.0109(17) 0.0025(19) 0.0003(18) Ni1 0.0160(3) 0.0193(4) 0.0134(3) -0.0017(3) -0.0054(2) -0.0002(3) O1 0.0136(13) 0.0174(13) 0.0177(12) -0.0045(10) -0.0028(10) -0.0022(10) O2 0.0155(13) 0.0184(13) 0.0125(12) -0.0037(9) -0.0037(9) -0.0016(10) S1 0.0257(5) 0.0230(5) 0.0149(4) -0.0023(4) -0.0026(4) 0.0016(4) S2 0.0183(5) 0.0208(5) 0.0183(4) -0.0019(4) -0.0017(3) -0.0006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C4 1.899(4) . ? Br2 C19 1.902(3) . ? C1 O1 1.332(4) . ? C1 C2 1.401(5) . ? C1 C6 1.410(5) . ? C2 C3 1.385(5) . ? C2 H2 0.9500 . ? C3 C4 1.387(5) . ? C3 H3 0.9500 . ? C4 C5 1.380(5) . ? C5 C6 1.406(5) . ? C5 H5 0.9500 . ? C6 C7 1.439(5) . ? C7 N1 1.288(5) . ? C7 H7 0.9500 . ? C8 N1 1.477(4) . ? C8 C9 1.517(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.521(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.491(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N2 1.487(5) . ? C11 C12 1.495(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N3 1.489(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N3 1.483(5) . ? C13 C14 1.522(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.522(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N4 1.472(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N4 1.292(5) . ? C16 C17 1.434(5) . ? C16 H16 0.9500 . ? C17 C18 1.405(5) . ? C17 C22 1.414(5) . ? C18 C19 1.362(5) . ? C18 H18 0.9500 . ? C19 C20 1.389(5) . ? C20 C21 1.387(5) . ? C20 H20 0.9500 . ? C21 C22 1.410(5) . ? C21 H21 0.9500 . ? C22 O2 1.320(4) . ? C23 N5 1.135(5) . ? C23 C24 1.435(5) . ? C24 C25 1.362(5) . ? C24 S2 1.739(4) . ? C25 C26 1.434(6) . ? C25 S1 1.731(4) . ? C26 N6 1.141(6) . ? Mn1 O2 1.881(3) . ? Mn1 O1 1.885(2) . ? Mn1 N1 1.984(3) . ? Mn1 N4 1.987(3) . ? Mn1 N2 2.038(3) . ? Mn1 N3 2.048(3) . ? N2 H28 0.9300 . ? N3 H27 0.9300 . ? Ni1 S1 2.1716(10) . ? Ni1 S1 2.1716(10) 2_676 ? Ni1 S2 2.1824(9) 2_676 ? Ni1 S2 2.1824(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 119.2(3) . . ? O1 C1 C6 122.0(3) . . ? C2 C1 C6 118.8(3) . . ? C3 C2 C1 120.7(3) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C2 C3 C4 120.1(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.5(3) . . ? C5 C4 Br1 118.9(3) . . ? C3 C4 Br1 120.6(3) . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 119.7(3) . . ? C5 C6 C7 118.2(3) . . ? C1 C6 C7 121.6(3) . . ? N1 C7 C6 124.3(3) . . ? N1 C7 H7 117.9 . . ? C6 C7 H7 117.9 . . ? N1 C8 C9 109.4(3) . . ? N1 C8 H8A 109.8 . . ? C9 C8 H8A 109.8 . . ? N1 C8 H8B 109.8 . . ? C9 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C8 C9 C10 115.0(3) . . ? C8 C9 H9A 108.5 . . ? C10 C9 H9A 108.5 . . ? C8 C9 H9B 108.5 . . ? C10 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? N2 C10 C9 112.3(3) . . ? N2 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? N2 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N2 C11 C12 109.0(3) . . ? N2 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? N2 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N3 C12 C11 107.8(3) . . ? N3 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? N3 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.5 . . ? N3 C13 C14 112.8(3) . . ? N3 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? N3 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C13 C14 C15 114.1(3) . . ? C13 C14 H14A 108.7 . . ? C15 C14 H14A 108.7 . . ? C13 C14 H14B 108.7 . . ? C15 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? N4 C15 C14 110.0(3) . . ? N4 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? N4 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N4 C16 C17 124.7(3) . . ? N4 C16 H16 117.6 . . ? C17 C16 H16 117.6 . . ? C18 C17 C22 119.8(3) . . ? C18 C17 C16 118.7(3) . . ? C22 C17 C16 120.7(3) . . ? C19 C18 C17 120.2(3) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 121.5(3) . . ? C18 C19 Br2 118.7(3) . . ? C20 C19 Br2 119.8(3) . . ? C21 C20 C19 119.2(3) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C22 121.1(3) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? O2 C22 C21 119.0(3) . . ? O2 C22 C17 122.8(3) . . ? C21 C22 C17 118.2(3) . . ? N5 C23 C24 178.9(5) . . ? C25 C24 C23 122.0(4) . . ? C25 C24 S2 120.8(3) . . ? C23 C24 S2 117.1(3) . . ? C24 C25 C26 121.9(4) . . ? C24 C25 S1 120.5(3) . . ? C26 C25 S1 117.6(3) . . ? N6 C26 C25 178.8(5) . . ? O2 Mn1 O1 179.87(13) . . ? O2 Mn1 N1 90.67(12) . . ? O1 Mn1 N1 89.23(11) . . ? O2 Mn1 N4 89.02(11) . . ? O1 Mn1 N4 91.07(12) . . ? N1 Mn1 N4 95.30(12) . . ? O2 Mn1 N2 88.47(11) . . ? O1 Mn1 N2 91.45(12) . . ? N1 Mn1 N2 90.21(12) . . ? N4 Mn1 N2 173.98(12) . . ? O2 Mn1 N3 91.09(12) . . ? O1 Mn1 N3 89.00(11) . . ? N1 Mn1 N3 175.04(12) . . ? N4 Mn1 N3 89.37(12) . . ? N2 Mn1 N3 85.20(12) . . ? C7 N1 C8 117.0(3) . . ? C7 N1 Mn1 122.1(3) . . ? C8 N1 Mn1 120.2(2) . . ? C11 N2 C10 111.0(3) . . ? C11 N2 Mn1 106.6(2) . . ? C10 N2 Mn1 118.8(2) . . ? C11 N2 H28 106.6 . . ? C10 N2 H28 106.6 . . ? Mn1 N2 H28 106.6 . . ? C13 N3 C12 110.7(3) . . ? C13 N3 Mn1 118.7(2) . . ? C12 N3 Mn1 107.0(2) . . ? C13 N3 H27 106.6 . . ? C12 N3 H27 106.6 . . ? Mn1 N3 H27 106.6 . . ? C16 N4 C15 116.6(3) . . ? C16 N4 Mn1 122.5(3) . . ? C15 N4 Mn1 120.1(2) . . ? S1 Ni1 S1 180.0 . 2_676 ? S1 Ni1 S2 87.98(4) . 2_676 ? S1 Ni1 S2 92.02(4) 2_676 2_676 ? S1 Ni1 S2 92.02(4) . . ? S1 Ni1 S2 87.98(4) 2_676 . ? S2 Ni1 S2 180.000(1) 2_676 . ? C1 O1 Mn1 122.4(2) . . ? C22 O2 Mn1 123.7(2) . . ? C25 S1 Ni1 103.61(13) . . ? C24 S2 Ni1 102.94(13) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.040 _refine_diff_density_min -0.887 _refine_diff_density_rms 0.267 _database_code_depnum_ccdc_archive 'CCDC 969625' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Pt-123 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C22 H26 Br2 Mn N4 O2), C8 N4 Pt S4' _chemical_formula_sum 'C52 H52 Br4 Mn2 N12 O4 Pt S4' _chemical_formula_weight 1661.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1643(19) _cell_length_b 10.013(2) _cell_length_c 18.323(4) _cell_angle_alpha 78.223(3) _cell_angle_beta 79.349(4) _cell_angle_gamma 83.348(4) _cell_volume 1436.3(6) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2693 _cell_measurement_theta_min 2.547 _cell_measurement_theta_max 25.7215 _exptl_crystal_description plate-like _exptl_crystal_colour black _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 5.846 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.202 _exptl_absorpt_correction_T_max 0.496 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11599 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_unetI/netI 0.0716 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5576 _reflns_number_gt 4485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0955P)^2^+0.0122P] 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 5576 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Br1 Br 0.22653(7) 0.70672(6) 1.06666(3) 0.02367(15) Uani 1 1 d . . . Br2 Br 1.28108(7) 1.26349(6) 0.93930(3) 0.02167(14) Uani 1 1 d . . . C1 C 0.5822(7) 0.7577(5) 0.8314(3) 0.0157(13) Uani 1 1 d . . . C2 C 0.5001(7) 0.6368(5) 0.8633(3) 0.0165(13) Uani 1 1 d . . . H2 H 0.5181 0.5634 0.8363 0.020 Uiso 1 1 calc R . . C3 C 0.3986(7) 0.6224(6) 0.9299(3) 0.0188(14) Uani 1 1 d . . . H3 H 0.3464 0.5396 0.9497 0.023 Uiso 1 1 calc R . . C4 C 0.3686(7) 0.7299(5) 0.9711(3) 0.0158(13) Uani 1 1 d . . . C5 C 0.4388(7) 0.8480(5) 0.9425(3) 0.0147(12) Uani 1 1 d . . . H5 H 0.4146 0.9209 0.9699 0.018 Uiso 1 1 calc R . . C6 C 0.5463(6) 0.8658(5) 0.8736(3) 0.0129(12) Uani 1 1 d . . . C7 C 0.6023(7) 0.9990(5) 0.8397(3) 0.0139(12) Uani 1 1 d . . . H7 H 0.5454 1.0748 0.8601 0.017 Uiso 1 1 calc R . . C8 C 0.7310(7) 1.1666(5) 0.7428(3) 0.0169(13) Uani 1 1 d . . . H8A H 0.6556 1.2289 0.7720 0.020 Uiso 1 1 calc R . . H8B H 0.8465 1.1934 0.7365 0.020 Uiso 1 1 calc R . . C9 C 0.6818(8) 1.1793(6) 0.6677(3) 0.0202(14) Uani 1 1 d . . . H9A H 0.6693 1.2776 0.6446 0.024 Uiso 1 1 calc R . . H9B H 0.5714 1.1425 0.6746 0.024 Uiso 1 1 calc R . . C10 C 0.8064(8) 1.1047(6) 0.6130(3) 0.0216(14) Uani 1 1 d . . . H10A H 0.7733 1.1280 0.5624 0.026 Uiso 1 1 calc R . . H10B H 0.9191 1.1362 0.6086 0.026 Uiso 1 1 calc R . . C11 C 0.9352(7) 0.8849(6) 0.5848(3) 0.0220(15) Uani 1 1 d . . . H11A H 1.0436 0.9261 0.5744 0.026 Uiso 1 1 calc R . . H11B H 0.8929 0.8952 0.5365 0.026 Uiso 1 1 calc R . . C12 C 0.9570(8) 0.7368(6) 0.6198(3) 0.0213(14) Uani 1 1 d . . . H12A H 0.8503 0.6942 0.6267 0.026 Uiso 1 1 calc R . . H12B H 1.0425 0.6884 0.5864 0.026 Uiso 1 1 calc R . . C13 C 1.0076(8) 0.5816(5) 0.7370(3) 0.0200(14) Uani 1 1 d . . . H13A H 0.8929 0.5523 0.7451 0.024 Uiso 1 1 calc R . . H13B H 1.0821 0.5202 0.7069 0.024 Uiso 1 1 calc R . . C14 C 1.0621(7) 0.5660(6) 0.8116(3) 0.0202(14) Uani 1 1 d . . . H14A H 1.1743 0.6001 0.8037 0.024 Uiso 1 1 calc R . . H14B H 1.0722 0.4674 0.8344 0.024 Uiso 1 1 calc R . . C15 C 0.9427(7) 0.6424(5) 0.8675(3) 0.0145(12) Uani 1 1 d . . . H15A H 0.8278 0.6149 0.8728 0.017 Uiso 1 1 calc R . . H15B H 0.9776 0.6182 0.9178 0.017 Uiso 1 1 calc R . . C16 C 1.0214(6) 0.8555(5) 0.8764(3) 0.0135(12) Uani 1 1 d . . . H16 H 1.0418 0.8116 0.9253 0.016 Uiso 1 1 calc R . . C17 C 1.0760(6) 0.9877(5) 0.8479(3) 0.0129(12) Uani 1 1 d . . . C18 C 1.1303(7) 1.0575(5) 0.8980(3) 0.0142(13) Uani 1 1 d . . . H18 H 1.1136 1.0220 0.9507 0.017 Uiso 1 1 calc R . . C19 C 1.2066(7) 1.1760(6) 0.8700(3) 0.0189(13) Uani 1 1 d . . . C20 C 1.2352(7) 1.2294(5) 0.7937(3) 0.0149(13) Uani 1 1 d . . . H20 H 1.2897 1.3115 0.7754 0.018 Uiso 1 1 calc R . . C21 C 1.1840(7) 1.1623(6) 0.7440(3) 0.0167(13) Uani 1 1 d . . . H21 H 1.2057 1.1986 0.6913 0.020 Uiso 1 1 calc R . . C22 C 1.1011(7) 1.0425(5) 0.7690(3) 0.0132(12) Uani 1 1 d . . . C23 C 0.4891(7) 0.5845(6) 0.6551(3) 0.0209(14) Uani 1 1 d . . . C24 C 0.5175(7) 0.7014(5) 0.5943(3) 0.0175(13) Uani 1 1 d . . . C25 C 0.6119(7) 0.6819(6) 0.5276(3) 0.0184(14) Uani 1 1 d . . . C26 C 0.6891(8) 0.5545(6) 0.5159(3) 0.0215(14) Uani 1 1 d . . . Mn1 Mn 0.86876(10) 0.87570(8) 0.74369(4) 0.01162(19) Uani 1 1 d . . . N1 N 0.7217(6) 1.0233(4) 0.7848(3) 0.0136(11) Uani 1 1 d . . . N2 N 0.8130(6) 0.9545(5) 0.6391(3) 0.0153(11) Uani 1 1 d . . . H28 H 0.7081 0.9277 0.6383 0.018 Uiso 1 1 calc R . . N3 N 1.0095(6) 0.7259(5) 0.6925(3) 0.0155(11) Uani 1 1 d . . . H27 H 1.1198 0.7484 0.6827 0.019 Uiso 1 1 calc R . . N4 N 0.9449(5) 0.7895(4) 0.8401(2) 0.0121(10) Uani 1 1 d . . . N5 N 0.4673(7) 0.4958(6) 0.7055(3) 0.0337(15) Uani 1 1 d . . . N6 N 0.7516(8) 0.4480(6) 0.5029(3) 0.0390(17) Uani 1 1 d . . . O1 O 0.6857(5) 0.7663(4) 0.7680(2) 0.0149(9) Uani 1 1 d . . . O2 O 1.0518(5) 0.9847(4) 0.7201(2) 0.0149(9) Uani 1 1 d . . . Pt1 Pt 0.5000 1.0000 0.5000 0.01443(8) Uani 1 2 d S . . S1 S 0.65359(19) 0.82091(14) 0.45333(8) 0.0195(3) Uani 1 1 d . . . S2 S 0.41933(18) 0.85648(14) 0.61246(8) 0.0178(3) 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 Br1 0.0218(3) 0.0246(3) 0.0211(3) -0.0020(2) 0.0037(2) -0.0029(2) Br2 0.0255(3) 0.0208(3) 0.0228(3) -0.0085(2) -0.0095(2) -0.0017(2) C1 0.017(3) 0.013(2) 0.016(3) 0.000(2) -0.007(2) 0.006(2) C2 0.014(3) 0.013(2) 0.026(3) -0.008(2) -0.003(2) -0.005(2) C3 0.021(3) 0.013(3) 0.024(3) -0.003(2) -0.007(2) -0.001(2) C4 0.015(3) 0.017(3) 0.015(3) -0.002(2) -0.005(2) 0.001(2) C5 0.017(3) 0.018(3) 0.011(3) -0.007(2) -0.006(2) 0.008(2) C6 0.010(2) 0.010(2) 0.019(3) -0.003(2) -0.005(2) 0.002(2) C7 0.018(3) 0.012(2) 0.013(3) -0.005(2) -0.003(2) 0.004(2) C8 0.019(3) 0.013(3) 0.017(3) 0.001(2) -0.003(2) 0.003(2) C9 0.025(3) 0.013(3) 0.020(3) 0.000(2) -0.008(2) 0.009(2) C10 0.027(3) 0.022(3) 0.014(3) 0.002(2) -0.007(2) 0.001(2) C11 0.019(3) 0.034(3) 0.011(3) -0.002(2) 0.000(2) -0.001(3) C12 0.021(3) 0.024(3) 0.022(3) -0.014(2) -0.002(2) 0.000(2) C13 0.026(3) 0.012(3) 0.023(3) -0.009(2) -0.003(2) 0.001(2) C14 0.022(3) 0.014(3) 0.023(3) -0.001(2) -0.006(2) 0.006(2) C15 0.018(3) 0.009(2) 0.017(3) -0.004(2) -0.004(2) 0.001(2) C16 0.009(2) 0.023(3) 0.007(2) -0.004(2) 0.000(2) 0.002(2) C17 0.008(2) 0.015(2) 0.016(3) -0.002(2) -0.001(2) -0.004(2) C18 0.013(2) 0.015(3) 0.013(3) 0.001(2) -0.001(2) 0.000(2) C19 0.015(3) 0.017(3) 0.031(3) -0.017(2) -0.009(2) 0.003(2) C20 0.014(3) 0.011(2) 0.020(3) -0.006(2) -0.001(2) 0.000(2) C21 0.014(3) 0.023(3) 0.009(3) 0.002(2) 0.002(2) 0.000(2) C22 0.018(3) 0.011(2) 0.013(3) -0.0083(19) -0.004(2) 0.005(2) C23 0.021(3) 0.018(3) 0.021(3) -0.005(2) 0.002(2) 0.002(2) C24 0.017(3) 0.014(3) 0.021(3) -0.002(2) -0.001(2) -0.004(2) C25 0.020(3) 0.021(3) 0.014(3) -0.001(2) -0.006(2) 0.002(2) C26 0.029(3) 0.021(3) 0.014(3) -0.004(2) 0.000(2) -0.002(3) Mn1 0.0118(4) 0.0118(4) 0.0116(4) -0.0027(3) -0.0033(3) 0.0010(3) N1 0.014(2) 0.009(2) 0.019(2) -0.0042(17) -0.0060(19) 0.0015(17) N2 0.013(2) 0.015(2) 0.017(2) -0.0010(18) -0.0047(19) 0.0000(18) N3 0.012(2) 0.018(2) 0.015(2) -0.0034(18) -0.0005(18) 0.0052(18) N4 0.009(2) 0.012(2) 0.014(2) -0.0009(17) 0.0000(18) 0.0001(17) N5 0.036(3) 0.026(3) 0.031(3) 0.001(2) 0.009(3) -0.006(2) N6 0.047(4) 0.029(3) 0.034(3) -0.005(2) 0.005(3) 0.001(3) O1 0.0159(19) 0.0146(18) 0.0139(19) -0.0045(14) -0.0008(16) 0.0008(15) O2 0.0164(19) 0.0193(19) 0.0084(18) -0.0034(14) -0.0003(15) -0.0002(16) Pt1 0.01520(15) 0.01525(14) 0.01298(15) -0.00277(11) -0.00443(11) 0.00177(11) S1 0.0249(7) 0.0171(7) 0.0153(7) -0.0031(5) -0.0029(6) 0.0027(6) S2 0.0184(7) 0.0167(6) 0.0171(7) -0.0028(5) -0.0017(6) 0.0014(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 Br1 C4 1.900(5) . ? Br2 C19 1.900(6) . ? C1 O1 1.297(6) . ? C1 C2 1.418(7) . ? C1 C6 1.428(8) . ? C2 C3 1.334(8) . ? C2 H2 0.9500 . ? C3 C4 1.411(8) . ? C3 H3 0.9500 . ? C4 C5 1.339(8) . ? C5 C6 1.390(7) . ? C5 H5 0.9500 . ? C6 C7 1.439(7) . ? C7 N1 1.271(7) . ? C7 H7 0.9500 . ? C8 C9 1.481(9) . ? C8 N1 1.485(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.532(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.481(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N2 1.492(7) . ? C11 C12 1.495(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N3 1.453(8) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.488(9) . ? C13 N3 1.507(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.537(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N4 1.457(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N4 1.302(7) . ? C16 C17 1.412(7) . ? C16 H16 0.9500 . ? C17 C18 1.418(8) . ? C17 C22 1.423(7) . ? C18 C19 1.366(8) . ? C18 H18 0.9500 . ? C19 C20 1.378(8) . ? C20 C21 1.383(9) . ? C20 H20 0.9500 . ? C21 C22 1.399(8) . ? C21 H21 0.9500 . ? C22 O2 1.302(7) . ? C23 N5 1.146(8) . ? C23 C24 1.450(8) . ? C24 C25 1.356(8) . ? C24 S2 1.729(6) . ? C25 C26 1.395(8) . ? C25 S1 1.753(6) . ? C26 N6 1.178(8) . ? Mn1 O2 1.887(4) . ? Mn1 O1 1.889(4) . ? Mn1 N1 1.975(4) . ? Mn1 N4 1.978(5) . ? Mn1 N2 2.030(5) . ? Mn1 N3 2.055(4) . ? N2 H28 0.9300 . ? N3 H27 0.9300 . ? Pt1 S1 2.2865(14) . ? Pt1 S1 2.2865(14) 2_676 ? Pt1 S2 2.2922(14) 2_676 ? Pt1 S2 2.2922(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 120.8(5) . . ? O1 C1 C6 123.0(5) . . ? C2 C1 C6 116.1(5) . . ? C3 C2 C1 122.3(5) . . ? C3 C2 H2 118.8 . . ? C1 C2 H2 118.8 . . ? C2 C3 C4 120.2(5) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.0(5) . . ? C5 C4 Br1 120.3(4) . . ? C3 C4 Br1 119.6(4) . . ? C4 C5 C6 121.2(5) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 120.1(5) . . ? C5 C6 C7 119.8(5) . . ? C1 C6 C7 119.5(5) . . ? N1 C7 C6 125.3(5) . . ? N1 C7 H7 117.3 . . ? C6 C7 H7 117.3 . . ? C9 C8 N1 110.2(5) . . ? C9 C8 H8A 109.6 . . ? N1 C8 H8A 109.6 . . ? C9 C8 H8B 109.6 . . ? N1 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 114.1(5) . . ? C8 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? C8 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? N2 C10 C9 111.5(4) . . ? N2 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? N2 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? N2 C11 C12 107.8(4) . . ? N2 C11 H11A 110.1 . . ? C12 C11 H11A 110.1 . . ? N2 C11 H11B 110.1 . . ? C12 C11 H11B 110.1 . . ? H11A C11 H11B 108.5 . . ? N3 C12 C11 108.6(5) . . ? N3 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? N3 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? C14 C13 N3 113.5(5) . . ? C14 C13 H13A 108.9 . . ? N3 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? N3 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C14 C15 113.8(5) . . ? C13 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? C13 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? N4 C15 C14 109.7(4) . . ? N4 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? N4 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N4 C16 C17 124.4(5) . . ? N4 C16 H16 117.8 . . ? C17 C16 H16 117.8 . . ? C16 C17 C18 118.5(5) . . ? C16 C17 C22 121.3(5) . . ? C18 C17 C22 119.5(5) . . ? C19 C18 C17 119.7(5) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 121.7(6) . . ? C18 C19 Br2 118.0(5) . . ? C20 C19 Br2 120.2(4) . . ? C19 C20 C21 119.4(5) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C20 C21 C22 121.8(5) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? O2 C22 C21 119.6(5) . . ? O2 C22 C17 122.6(5) . . ? C21 C22 C17 117.8(5) . . ? N5 C23 C24 176.8(7) . . ? C25 C24 C23 119.0(5) . . ? C25 C24 S2 125.0(4) . . ? C23 C24 S2 116.0(4) . . ? C24 C25 C26 122.7(5) . . ? C24 C25 S1 120.5(4) . . ? C26 C25 S1 116.6(4) . . ? N6 C26 C25 177.0(7) . . ? O2 Mn1 O1 179.60(17) . . ? O2 Mn1 N1 90.93(17) . . ? O1 Mn1 N1 88.98(17) . . ? O2 Mn1 N4 89.05(18) . . ? O1 Mn1 N4 90.58(18) . . ? N1 Mn1 N4 95.45(19) . . ? O2 Mn1 N2 88.56(18) . . ? O1 Mn1 N2 91.83(18) . . ? N1 Mn1 N2 90.17(19) . . ? N4 Mn1 N2 173.93(18) . . ? O2 Mn1 N3 90.85(18) . . ? O1 Mn1 N3 89.28(18) . . ? N1 Mn1 N3 174.6(2) . . ? N4 Mn1 N3 89.71(18) . . ? N2 Mn1 N3 84.76(18) . . ? C7 N1 C8 117.7(4) . . ? C7 N1 Mn1 122.3(4) . . ? C8 N1 Mn1 119.3(3) . . ? C10 N2 C11 110.2(4) . . ? C10 N2 Mn1 118.5(4) . . ? C11 N2 Mn1 106.8(3) . . ? C10 N2 H28 106.9 . . ? C11 N2 H28 106.9 . . ? Mn1 N2 H28 106.9 . . ? C12 N3 C13 111.8(5) . . ? C12 N3 Mn1 106.8(3) . . ? C13 N3 Mn1 116.9(3) . . ? C12 N3 H27 107.0 . . ? C13 N3 H27 107.0 . . ? Mn1 N3 H27 107.0 . . ? C16 N4 C15 116.1(5) . . ? C16 N4 Mn1 122.4(4) . . ? C15 N4 Mn1 120.7(4) . . ? C1 O1 Mn1 123.1(4) . . ? C22 O2 Mn1 123.6(3) . . ? S1 Pt1 S1 180.000(1) . 2_676 ? S1 Pt1 S2 89.95(5) . 2_676 ? S1 Pt1 S2 90.05(5) 2_676 2_676 ? S1 Pt1 S2 90.05(5) . . ? S1 Pt1 S2 89.95(5) 2_676 . ? S2 Pt1 S2 180.000(1) 2_676 . ? C25 S1 Pt1 102.80(19) . . ? C24 S2 Pt1 101.54(19) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.356 _refine_diff_density_min -1.828 _refine_diff_density_rms 0.365 _database_code_depnum_ccdc_archive 'CCDC 969626' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_dmit _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H26 Br2 Mn N4 O2, C6 Ni S10, C2 H3 N' _chemical_formula_sum 'C30 H29 Br2 Mn N5 Ni O2 S10' _chemical_formula_weight 1085.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9060(9) _cell_length_b 12.1826(10) _cell_length_c 16.1265(13) _cell_angle_alpha 94.2340(10) _cell_angle_beta 104.1830(10) _cell_angle_gamma 92.672(2) _cell_volume 2067.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3717 _cell_measurement_theta_min 2.206 _cell_measurement_theta_max 24.823 _exptl_crystal_description long-strip _exptl_crystal_colour dark-green _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1086 _exptl_absorpt_coefficient_mu 3.235 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.325 _exptl_absorpt_correction_T_max 0.724 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11697 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_unetI/netI 0.0362 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7231 _reflns_number_gt 5470 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0426P)^2^+1.1345P] 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 7231 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.011 _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 Br1 Br -0.10847(5) 0.75145(4) 0.68707(3) 0.08358(17) Uani 1 1 d . . . Br2 Br -0.39655(4) -0.11344(4) 0.80005(4) 0.08011(16) Uani 1 1 d . . . C1 C 0.3222(3) 0.6804(3) -0.1082(2) 0.0438(8) Uani 1 1 d . . . C2 C 0.2521(4) 0.7647(3) -0.0913(2) 0.0509(9) Uani 1 1 d . . . C3 C 0.2767(4) 0.7877(3) -0.2454(3) 0.0547(10) Uani 1 1 d . . . C4 C 0.3532(4) 0.5444(3) 0.2411(2) 0.0530(9) Uani 1 1 d . . . C5 C 0.2757(4) 0.6246(3) 0.2540(2) 0.0531(9) Uani 1 1 d . . . C6 C 0.3208(4) 0.5239(4) 0.3948(2) 0.0648(11) Uani 1 1 d . . . C7 C 0.1285(3) 0.4392(3) 0.7161(2) 0.0446(8) Uani 1 1 d . . . C8 C 0.1134(4) 0.4974(3) 0.6424(2) 0.0544(10) Uani 1 1 d . . . H8 H 0.1522 0.4749 0.5992 0.065 Uiso 1 1 calc R . . C9 C 0.0409(4) 0.5882(3) 0.6340(3) 0.0596(10) Uani 1 1 d . . . H9 H 0.0290 0.6249 0.5843 0.071 Uiso 1 1 calc R . . C10 C -0.0130(4) 0.6241(3) 0.6978(3) 0.0572(10) Uani 1 1 d . . . C11 C 0.0023(4) 0.5708(3) 0.7711(2) 0.0538(10) Uani 1 1 d . . . H11 H -0.0333 0.5972 0.8149 0.065 Uiso 1 1 calc R . . C12 C 0.0713(3) 0.4767(3) 0.7803(2) 0.0453(8) Uani 1 1 d . . . C13 C 0.0852(4) 0.4224(3) 0.8588(2) 0.0497(9) Uani 1 1 d . . . H13 H 0.0657 0.4612 0.9053 0.060 Uiso 1 1 calc R . . C14 C 0.1447(4) 0.2871(3) 0.9556(2) 0.0623(11) Uani 1 1 d . . . H14A H 0.1014 0.2150 0.9526 0.075 Uiso 1 1 calc R . . H14B H 0.1100 0.3378 0.9918 0.075 Uiso 1 1 calc R . . C15 C 0.2860(5) 0.2805(3) 0.9953(3) 0.0735(14) Uani 1 1 d . . . H15A H 0.3283 0.3522 0.9946 0.088 Uiso 1 1 calc R . . H15B H 0.2972 0.2660 1.0550 0.088 Uiso 1 1 calc R . . C16 C 0.3513(4) 0.1954(3) 0.9532(3) 0.0695(12) Uani 1 1 d . . . H16A H 0.4373 0.1923 0.9876 0.083 Uiso 1 1 calc R . . H16B H 0.3074 0.1237 0.9510 0.083 Uiso 1 1 calc R . . C17 C 0.4308(4) 0.1416(4) 0.8289(3) 0.0775(14) Uani 1 1 d . . . H17A H 0.4026 0.0664 0.8345 0.093 Uiso 1 1 calc R . . H17B H 0.5192 0.1537 0.8599 0.093 Uiso 1 1 calc R . . C18 C 0.4167(4) 0.1585(4) 0.7362(3) 0.0784(14) Uani 1 1 d . . . H18A H 0.4467 0.2332 0.7307 0.094 Uiso 1 1 calc R . . H18B H 0.4672 0.1078 0.7118 0.094 Uiso 1 1 calc R . . C19 C 0.2596(5) 0.1651(4) 0.5992(3) 0.0775(14) Uani 1 1 d . . . H19A H 0.3173 0.1257 0.5725 0.093 Uiso 1 1 calc R . . H19B H 0.2785 0.2434 0.5979 0.093 Uiso 1 1 calc R . . C20 C 0.1257(5) 0.1348(4) 0.5481(3) 0.0770(14) Uani 1 1 d . . . H20A H 0.1062 0.0572 0.5523 0.092 Uiso 1 1 calc R . . H20B H 0.1209 0.1444 0.4882 0.092 Uiso 1 1 calc R . . C21 C 0.0250(4) 0.2005(3) 0.5754(2) 0.0635(11) Uani 1 1 d . . . H21A H 0.0474 0.2788 0.5770 0.076 Uiso 1 1 calc R . . H21B H -0.0558 0.1837 0.5339 0.076 Uiso 1 1 calc R . . C22 C -0.0805(4) 0.1085(3) 0.6637(2) 0.0471(9) Uani 1 1 d . . . H22 H -0.1432 0.0918 0.6131 0.057 Uiso 1 1 calc R . . C23 C -0.0975(3) 0.0598(3) 0.7390(2) 0.0394(8) Uani 1 1 d . . . C24 C -0.2165(3) 0.0094(3) 0.7367(2) 0.0478(9) Uani 1 1 d . . . H24 H -0.2832 0.0117 0.6884 0.057 Uiso 1 1 calc R . . C25 C -0.2353(3) -0.0432(3) 0.8054(2) 0.0490(9) Uani 1 1 d . . . C26 C -0.1372(4) -0.0486(3) 0.8768(2) 0.0481(9) Uani 1 1 d . . . H26 H -0.1505 -0.0846 0.9230 0.058 Uiso 1 1 calc R . . C27 C -0.0194(3) -0.0006(3) 0.8797(2) 0.0446(8) Uani 1 1 d . . . H27 H 0.0467 -0.0052 0.9280 0.053 Uiso 1 1 calc R . . C28 C 0.0032(3) 0.0547(2) 0.8116(2) 0.0378(8) Uani 1 1 d . . . C29 C 0.5677(5) 0.1390(5) 0.4935(3) 0.0859(15) Uani 1 1 d . . . C30 C 0.4829(6) 0.2149(5) 0.4520(4) 0.1072(19) Uani 1 1 d . . . H30A H 0.5279 0.2658 0.4255 0.161 Uiso 1 1 calc R . . H30B H 0.4482 0.2547 0.4936 0.161 Uiso 1 1 calc R . . H30C H 0.4155 0.1753 0.4090 0.161 Uiso 1 1 calc R . . H2 H 0.388(4) 0.272(3) 0.867(3) 0.060(14) Uiso 1 1 d . . . H3 H 0.269(4) 0.079(3) 0.691(3) 0.056(13) Uiso 1 1 d . . . Mn1 Mn 0.16530(5) 0.22392(4) 0.76984(3) 0.04184(14) Uani 1 1 d . . . N1 N 0.1222(3) 0.3248(2) 0.86891(18) 0.0487(7) Uani 1 1 d . . . N2 N 0.3550(4) 0.2189(3) 0.8653(3) 0.0634(10) Uani 1 1 d . . . N3 N 0.2816(3) 0.1391(3) 0.6894(3) 0.0607(10) Uani 1 1 d . . . N4 N 0.0141(3) 0.1731(2) 0.66093(17) 0.0454(7) Uani 1 1 d . . . N5 N 0.6356(6) 0.0776(5) 0.5242(4) 0.131(2) Uani 1 1 d . . . Ni1 Ni 0.29909(4) 0.64995(4) 0.07255(3) 0.04616(13) Uani 1 1 d . . . O1 O 0.2013(2) 0.35308(18) 0.72241(16) 0.0506(6) Uani 1 1 d . . . O2 O 0.1202(2) 0.09657(17) 0.81670(14) 0.0439(6) Uani 1 1 d . . . S1 S 0.37264(9) 0.58815(7) -0.03364(6) 0.0480(2) Uani 1 1 d . . . S2 S 0.20859(12) 0.78190(9) 0.00366(7) 0.0695(3) Uani 1 1 d . . . S3 S 0.35512(10) 0.67365(8) -0.20888(7) 0.0535(2) Uani 1 1 d . . . S4 S 0.20854(11) 0.85282(8) -0.17195(7) 0.0656(3) Uani 1 1 d . . . S5 S 0.26698(12) 0.83118(10) -0.34123(8) 0.0732(3) Uani 1 1 d . . . S6 S 0.39994(12) 0.52699(9) 0.14702(6) 0.0635(3) Uani 1 1 d . . . S7 S 0.21877(11) 0.70962(9) 0.17549(7) 0.0680(3) Uani 1 1 d . . . S8 S 0.40232(14) 0.46305(11) 0.32574(7) 0.0804(4) Uani 1 1 d . . . S9 S 0.23782(11) 0.63237(10) 0.35279(7) 0.0711(3) Uani 1 1 d . . . S10 S 0.32301(14) 0.48386(14) 0.48949(8) 0.0938(4) 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 Br1 0.0865(4) 0.0553(3) 0.1021(4) 0.0147(2) 0.0042(3) 0.0262(2) Br2 0.0478(3) 0.0917(3) 0.1038(4) 0.0245(3) 0.0225(2) -0.0093(2) C1 0.037(2) 0.0378(18) 0.056(2) 0.0093(16) 0.0093(16) 0.0027(15) C2 0.047(2) 0.043(2) 0.062(2) 0.0114(17) 0.0095(18) 0.0125(17) C3 0.046(2) 0.046(2) 0.073(3) 0.0207(19) 0.0114(19) 0.0000(16) C4 0.056(3) 0.056(2) 0.049(2) 0.0000(17) 0.0160(18) 0.0086(18) C5 0.048(2) 0.058(2) 0.053(2) -0.0081(18) 0.0168(18) 0.0040(18) C6 0.058(3) 0.087(3) 0.052(2) -0.003(2) 0.022(2) 0.003(2) C7 0.050(2) 0.0330(18) 0.053(2) 0.0078(15) 0.0158(17) -0.0033(15) C8 0.070(3) 0.041(2) 0.058(2) 0.0104(17) 0.024(2) 0.0032(18) C9 0.073(3) 0.046(2) 0.058(2) 0.0170(19) 0.008(2) 0.0027(19) C10 0.063(3) 0.0356(19) 0.069(3) 0.0079(18) 0.007(2) 0.0063(18) C11 0.062(3) 0.040(2) 0.060(2) 0.0000(18) 0.017(2) 0.0040(17) C12 0.052(2) 0.0366(18) 0.047(2) 0.0076(15) 0.0104(17) -0.0011(16) C13 0.055(2) 0.046(2) 0.050(2) -0.0004(17) 0.0181(18) 0.0000(17) C14 0.095(4) 0.049(2) 0.046(2) 0.0092(18) 0.023(2) -0.002(2) C15 0.097(4) 0.052(2) 0.054(2) 0.011(2) -0.011(2) -0.017(2) C16 0.064(3) 0.054(3) 0.074(3) 0.017(2) -0.013(2) -0.011(2) C17 0.045(3) 0.065(3) 0.117(4) 0.018(3) 0.009(3) 0.005(2) C18 0.054(3) 0.066(3) 0.125(4) 0.019(3) 0.038(3) 0.008(2) C19 0.103(4) 0.067(3) 0.083(3) 0.012(2) 0.059(3) 0.011(3) C20 0.112(4) 0.074(3) 0.053(3) 0.002(2) 0.037(3) -0.001(3) C21 0.083(3) 0.061(2) 0.046(2) 0.0123(19) 0.015(2) -0.006(2) C22 0.052(2) 0.0420(19) 0.045(2) 0.0064(16) 0.0047(17) 0.0060(17) C23 0.043(2) 0.0336(17) 0.0410(19) 0.0046(14) 0.0083(16) 0.0039(14) C24 0.038(2) 0.044(2) 0.059(2) 0.0067(17) 0.0043(17) 0.0066(16) C25 0.042(2) 0.044(2) 0.064(2) 0.0035(18) 0.0189(19) -0.0004(16) C26 0.055(2) 0.046(2) 0.046(2) 0.0075(16) 0.0177(18) -0.0036(17) C27 0.050(2) 0.0403(19) 0.0410(19) 0.0047(15) 0.0067(16) 0.0015(16) C28 0.041(2) 0.0259(16) 0.0468(19) 0.0026(14) 0.0110(16) 0.0018(14) C29 0.081(4) 0.096(4) 0.072(3) 0.028(3) 0.000(3) -0.016(3) C30 0.106(5) 0.123(5) 0.106(4) 0.035(4) 0.039(4) 0.031(4) Mn1 0.0454(3) 0.0325(3) 0.0485(3) 0.0081(2) 0.0126(2) 0.0004(2) N1 0.061(2) 0.0398(16) 0.0455(17) 0.0069(13) 0.0132(15) -0.0015(14) N2 0.055(2) 0.045(2) 0.084(3) 0.0137(19) 0.0046(19) -0.0110(18) N3 0.061(2) 0.041(2) 0.089(3) 0.0095(18) 0.034(2) 0.0044(17) N4 0.055(2) 0.0396(16) 0.0409(16) 0.0111(13) 0.0093(14) 0.0022(14) N5 0.113(5) 0.123(4) 0.130(4) 0.050(4) -0.030(4) -0.018(3) Ni1 0.0451(3) 0.0407(2) 0.0529(3) 0.0014(2) 0.0124(2) 0.0082(2) O1 0.0586(17) 0.0366(13) 0.0644(16) 0.0128(11) 0.0274(13) 0.0054(11) O2 0.0418(15) 0.0356(12) 0.0512(14) 0.0098(10) 0.0048(11) -0.0019(10) S1 0.0520(6) 0.0385(5) 0.0575(6) 0.0097(4) 0.0180(4) 0.0142(4) S2 0.0809(8) 0.0646(7) 0.0718(7) 0.0141(5) 0.0270(6) 0.0388(6) S3 0.0535(6) 0.0483(5) 0.0639(6) 0.0158(4) 0.0204(5) 0.0106(4) S4 0.0702(8) 0.0505(6) 0.0813(7) 0.0237(5) 0.0197(6) 0.0240(5) S5 0.0752(8) 0.0727(7) 0.0772(8) 0.0336(6) 0.0209(6) 0.0072(6) S6 0.0874(8) 0.0625(6) 0.0485(6) 0.0080(5) 0.0255(5) 0.0357(6) S7 0.0701(8) 0.0693(7) 0.0728(7) 0.0048(5) 0.0293(6) 0.0302(6) S8 0.1078(11) 0.0929(9) 0.0529(6) 0.0173(6) 0.0341(6) 0.0418(8) S9 0.0665(8) 0.0918(8) 0.0591(6) -0.0086(6) 0.0264(6) 0.0148(6) S10 0.0920(10) 0.1431(13) 0.0544(7) 0.0125(7) 0.0319(7) 0.0120(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 Br1 C10 1.903(4) . ? Br2 C25 1.899(4) . ? C1 C2 1.359(5) . ? C1 S1 1.716(3) . ? C1 S3 1.744(4) . ? C2 S2 1.713(4) . ? C2 S4 1.738(4) . ? C3 S5 1.651(4) . ? C3 S4 1.712(4) . ? C3 S3 1.730(4) . ? C4 C5 1.358(5) . ? C4 S6 1.717(4) . ? C4 S8 1.739(4) . ? C5 S7 1.711(4) . ? C5 S9 1.739(4) . ? C6 S10 1.632(4) . ? C6 S9 1.723(5) . ? C6 S8 1.733(4) . ? C7 O1 1.340(4) . ? C7 C12 1.394(5) . ? C7 C8 1.408(5) . ? C8 C9 1.384(5) . ? C8 H8 0.9300 . ? C9 C10 1.361(6) . ? C9 H9 0.9300 . ? C10 C11 1.369(5) . ? C11 C12 1.398(5) . ? C11 H11 0.9300 . ? C12 C13 1.451(5) . ? C13 N1 1.282(4) . ? C13 H13 0.9300 . ? C14 N1 1.471(4) . ? C14 C15 1.526(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.498(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N2 1.476(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N2 1.464(6) . ? C17 C18 1.497(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N3 1.481(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N3 1.475(6) . ? C19 C20 1.504(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.519(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N4 1.474(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N4 1.281(4) . ? C22 C23 1.437(5) . ? C22 H22 0.9300 . ? C23 C24 1.400(5) . ? C23 C28 1.403(5) . ? C24 C25 1.373(5) . ? C24 H24 0.9300 . ? C25 C26 1.374(5) . ? C26 C27 1.376(5) . ? C26 H26 0.9300 . ? C27 C28 1.395(4) . ? C27 H27 0.9300 . ? C28 O2 1.333(4) . ? C29 N5 1.131(7) . ? C29 C30 1.423(7) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? Mn1 O1 1.866(2) . ? Mn1 O2 1.872(2) . ? Mn1 N1 2.101(3) . ? Mn1 N4 2.124(3) . ? Mn1 N3 2.257(3) . ? Mn1 N2 2.262(4) . ? N2 H2 0.72(4) . ? N3 H3 0.75(4) . ? Ni1 S7 2.1553(11) . ? Ni1 S2 2.1603(11) . ? Ni1 S6 2.1605(11) . ? Ni1 S1 2.1637(10) . ? 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 C2 C1 S1 120.8(3) . . ? C2 C1 S3 115.6(3) . . ? S1 C1 S3 123.6(2) . . ? C1 C2 S2 121.7(3) . . ? C1 C2 S4 116.1(3) . . ? S2 C2 S4 122.2(2) . . ? S5 C3 S4 122.4(2) . . ? S5 C3 S3 124.2(2) . . ? S4 C3 S3 113.4(2) . . ? C5 C4 S6 121.3(3) . . ? C5 C4 S8 115.9(3) . . ? S6 C4 S8 122.8(2) . . ? C4 C5 S7 120.8(3) . . ? C4 C5 S9 115.8(3) . . ? S7 C5 S9 123.4(2) . . ? S10 C6 S9 123.5(2) . . ? S10 C6 S8 123.9(3) . . ? S9 C6 S8 112.5(2) . . ? O1 C7 C12 123.3(3) . . ? O1 C7 C8 118.3(3) . . ? C12 C7 C8 118.4(3) . . ? C9 C8 C7 120.1(4) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 120.5(4) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.8(3) . . ? C9 C10 Br1 120.2(3) . . ? C11 C10 Br1 119.1(3) . . ? C10 C11 C12 120.1(4) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 120.0(3) . . ? C7 C12 C13 121.5(3) . . ? C11 C12 C13 118.4(3) . . ? N1 C13 C12 124.8(3) . . ? N1 C13 H13 117.6 . . ? C12 C13 H13 117.6 . . ? N1 C14 C15 111.1(3) . . ? N1 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N1 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 116.3(3) . . ? C16 C15 H15A 108.2 . . ? C14 C15 H15A 108.2 . . ? C16 C15 H15B 108.2 . . ? C14 C15 H15B 108.2 . . ? H15A C15 H15B 107.4 . . ? N2 C16 C15 112.5(3) . . ? N2 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? N2 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N2 C17 C18 109.4(4) . . ? N2 C17 H17A 109.8 . . ? C18 C17 H17A 109.8 . . ? N2 C17 H17B 109.8 . . ? C18 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? N3 C18 C17 109.4(4) . . ? N3 C18 H18A 109.8 . . ? C17 C18 H18A 109.8 . . ? N3 C18 H18B 109.8 . . ? C17 C18 H18B 109.8 . . ? H18A C18 H18B 108.2 . . ? N3 C19 C20 112.8(4) . . ? N3 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? N3 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C19 C20 C21 115.4(4) . . ? C19 C20 H20A 108.4 . . ? C21 C20 H20A 108.4 . . ? C19 C20 H20B 108.4 . . ? C21 C20 H20B 108.4 . . ? H20A C20 H20B 107.5 . . ? N4 C21 C20 110.1(3) . . ? N4 C21 H21A 109.6 . . ? C20 C21 H21A 109.6 . . ? N4 C21 H21B 109.6 . . ? C20 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? N4 C22 C23 125.2(3) . . ? N4 C22 H22 117.4 . . ? C23 C22 H22 117.4 . . ? C24 C23 C28 119.5(3) . . ? C24 C23 C22 118.4(3) . . ? C28 C23 C22 122.0(3) . . ? C25 C24 C23 120.4(3) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.5(3) . . ? C24 C25 Br2 119.7(3) . . ? C26 C25 Br2 119.8(3) . . ? C25 C26 C27 119.8(3) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C26 C27 C28 121.4(3) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? O2 C28 C27 118.8(3) . . ? O2 C28 C23 122.7(3) . . ? C27 C28 C23 118.4(3) . . ? N5 C29 C30 178.0(7) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 Mn1 O2 176.91(11) . . ? O1 Mn1 N1 87.34(11) . . ? O2 Mn1 N1 91.18(11) . . ? O1 Mn1 N4 91.69(11) . . ? O2 Mn1 N4 86.57(10) . . ? N1 Mn1 N4 117.15(12) . . ? O1 Mn1 N3 86.66(12) . . ? O2 Mn1 N3 95.64(12) . . ? N1 Mn1 N3 159.48(13) . . ? N4 Mn1 N3 82.64(13) . . ? O1 Mn1 N2 97.55(13) . . ? O2 Mn1 N2 84.97(12) . . ? N1 Mn1 N2 83.63(14) . . ? N4 Mn1 N2 157.73(13) . . ? N3 Mn1 N2 77.74(15) . . ? C13 N1 C14 117.6(3) . . ? C13 N1 Mn1 122.7(2) . . ? C14 N1 Mn1 119.5(2) . . ? C17 N2 C16 111.5(4) . . ? C17 N2 Mn1 108.5(3) . . ? C16 N2 Mn1 116.3(3) . . ? C17 N2 H2 104(4) . . ? C16 N2 H2 109(4) . . ? Mn1 N2 H2 106(4) . . ? C19 N3 C18 112.0(4) . . ? C19 N3 Mn1 117.2(3) . . ? C18 N3 Mn1 107.7(3) . . ? C19 N3 H3 110(3) . . ? C18 N3 H3 103(3) . . ? Mn1 N3 H3 106(3) . . ? C22 N4 C21 117.1(3) . . ? C22 N4 Mn1 123.3(2) . . ? C21 N4 Mn1 119.1(2) . . ? S7 Ni1 S2 86.14(4) . . ? S7 Ni1 S6 92.80(4) . . ? S2 Ni1 S6 175.79(5) . . ? S7 Ni1 S1 177.85(5) . . ? S2 Ni1 S1 93.04(4) . . ? S6 Ni1 S1 88.15(4) . . ? C7 O1 Mn1 123.7(2) . . ? C28 O2 Mn1 126.90(19) . . ? C1 S1 Ni1 102.30(12) . . ? C2 S2 Ni1 102.09(12) . . ? C3 S3 C1 97.25(18) . . ? C3 S4 C2 97.67(17) . . ? C4 S6 Ni1 102.24(13) . . ? C5 S7 Ni1 102.83(13) . . ? C6 S8 C4 97.76(19) . . ? C6 S9 C5 98.00(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.673 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.073 _database_code_depnum_ccdc_archive 'CCDC 969627' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_k _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C22 H26 Br2 Mn N4 O2), C8 N4 Ni S4 ' _chemical_formula_sum 'C52 H52 Br4 Mn2 N12 Ni O4 S4' _chemical_formula_weight 1525.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2849(5) _cell_length_b 10.0345(6) _cell_length_c 18.4775(10) _cell_angle_alpha 78.3540(10) _cell_angle_beta 79.2600(10) _cell_angle_gamma 84.2090(10) _cell_volume 1474.95(15) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2544 _cell_measurement_theta_min 2.284 _cell_measurement_theta_max 24.4335 _exptl_crystal_description plate-like _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 3.643 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2631 _exptl_absorpt_correction_T_max 0.7121 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10098 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_unetI/netI 0.0500 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6708 _reflns_number_gt 4678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6708 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1387 _refine_ls_wR_factor_gt 0.1130 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Br1 Br 0.22847(6) 0.71304(5) 1.06525(3) 0.06329(17) Uani 1 1 d . . . Br2 Br 1.28045(6) 1.26666(5) 0.93735(3) 0.05807(16) Uani 1 1 d . . . C1 C 0.5807(4) 0.7613(4) 0.8326(2) 0.0347(8) Uani 1 1 d . . . C2 C 0.5012(5) 0.6404(4) 0.8635(3) 0.0486(11) Uani 1 1 d . . . H2 H 0.5186 0.5688 0.8373 0.058 Uiso 1 1 calc R . . C3 C 0.3978(5) 0.6259(4) 0.9321(2) 0.0461(10) Uani 1 1 d . . . H3 H 0.3477 0.5444 0.9520 0.055 Uiso 1 1 calc R . . C4 C 0.3686(5) 0.7316(4) 0.9710(2) 0.0413(9) Uani 1 1 d . . . C5 C 0.4420(5) 0.8543(4) 0.9405(2) 0.0381(9) Uani 1 1 d . . . H5 H 0.4206 0.9265 0.9663 0.046 Uiso 1 1 calc R . . C6 C 0.5456(4) 0.8690(4) 0.8726(2) 0.0339(8) Uani 1 1 d . . . C7 C 0.6032(5) 1.0050(4) 0.8369(2) 0.0377(9) Uani 1 1 d . . . H7 H 0.5489 1.0794 0.8561 0.045 Uiso 1 1 calc R . . C8 C 0.7329(6) 1.1700(4) 0.7409(2) 0.0470(10) Uani 1 1 d . . . H8A H 0.8446 1.1961 0.7358 0.056 Uiso 1 1 calc R . . H8B H 0.6597 1.2317 0.7681 0.056 Uiso 1 1 calc R . . C9 C 0.6883(7) 1.1809(5) 0.6640(3) 0.0583(13) Uani 1 1 d . . . H9A H 0.6796 1.2765 0.6408 0.070 Uiso 1 1 calc R . . H9B H 0.5808 1.1458 0.6701 0.070 Uiso 1 1 calc R . . C10 C 0.8097(6) 1.1053(4) 0.6111(2) 0.0489(11) Uani 1 1 d . . . H10A H 0.7788 1.1269 0.5617 0.059 Uiso 1 1 calc R . . H10B H 0.9188 1.1364 0.6067 0.059 Uiso 1 1 calc R . . C11 C 0.9335(6) 0.8846(5) 0.5850(2) 0.0490(11) Uani 1 1 d . . . H11A H 1.0386 0.9255 0.5747 0.059 Uiso 1 1 calc R . . H11B H 0.8934 0.8941 0.5380 0.059 Uiso 1 1 calc R . . C12 C 0.9556(6) 0.7364(5) 0.6189(2) 0.0551(12) Uani 1 1 d . . . H12A H 0.8530 0.6932 0.6253 0.066 Uiso 1 1 calc R . . H12B H 1.0386 0.6909 0.5861 0.066 Uiso 1 1 calc R . . C13 C 1.0020(6) 0.5825(4) 0.7357(3) 0.0554(12) Uani 1 1 d . . . H13A H 1.0729 0.5227 0.7064 0.066 Uiso 1 1 calc R . . H13B H 0.8906 0.5541 0.7434 0.066 Uiso 1 1 calc R . . C14 C 1.0554(6) 0.5667(5) 0.8107(3) 0.0554(12) Uani 1 1 d . . . H14A H 1.1648 0.5991 0.8029 0.066 Uiso 1 1 calc R . . H14B H 1.0625 0.4704 0.8328 0.066 Uiso 1 1 calc R . . C15 C 0.9428(5) 0.6416(4) 0.8657(2) 0.0436(10) Uani 1 1 d . . . H15A H 0.8313 0.6146 0.8714 0.052 Uiso 1 1 calc R . . H15B H 0.9774 0.6168 0.9143 0.052 Uiso 1 1 calc R . . C16 C 1.0229(5) 0.8550(4) 0.8748(2) 0.0400(9) Uani 1 1 d . . . H16 H 1.0459 0.8112 0.9215 0.048 Uiso 1 1 calc R . . C17 C 1.0768(4) 0.9899(4) 0.8470(2) 0.0326(8) Uani 1 1 d . . . C18 C 1.1295(5) 1.0577(4) 0.8967(2) 0.0365(8) Uani 1 1 d . . . H18 H 1.1125 1.0226 0.9479 0.044 Uiso 1 1 calc R . . C19 C 1.2081(5) 1.1790(4) 0.8682(2) 0.0376(9) Uani 1 1 d . . . C20 C 1.2348(5) 1.2311(4) 0.7926(2) 0.0405(9) Uani 1 1 d . . . H20 H 1.2884 1.3113 0.7746 0.049 Uiso 1 1 calc R . . C21 C 1.1835(5) 1.1662(4) 0.7436(2) 0.0397(9) Uani 1 1 d . . . H21 H 1.2050 1.2017 0.6924 0.048 Uiso 1 1 calc R . . C22 C 1.0978(4) 1.0454(4) 0.7694(2) 0.0334(8) Uani 1 1 d . . . C23 C 0.4885(6) 0.5930(5) 0.6504(3) 0.0576(12) Uani 1 1 d . . . C24 C 0.5140(5) 0.7058(4) 0.5911(2) 0.0453(10) Uani 1 1 d . . . C25 C 0.6130(5) 0.6954(5) 0.5239(2) 0.0461(10) Uani 1 1 d . . . C26 C 0.6922(7) 0.5669(5) 0.5100(3) 0.0622(13) Uani 1 1 d . . . Mn1 Mn 0.86786(7) 0.87755(6) 0.74356(3) 0.03112(15) Uani 1 1 d . . . N1 N 0.7189(4) 1.0283(3) 0.78306(17) 0.0345(7) Uani 1 1 d . . . N2 N 0.8144(4) 0.9556(4) 0.63743(18) 0.0438(8) Uani 1 1 d . . . H28 H 0.7129 0.9290 0.6368 0.053 Uiso 1 1 calc R . . N3 N 1.0073(4) 0.7257(3) 0.69234(18) 0.0432(8) Uani 1 1 d . . . H27 H 1.1141 0.7475 0.6830 0.052 Uiso 1 1 calc R . . N4 N 0.9452(4) 0.7897(3) 0.84035(17) 0.0351(7) Uani 1 1 d . . . N5 N 0.4648(7) 0.5035(5) 0.6998(3) 0.0886(16) Uani 1 1 d . . . N6 N 0.7539(7) 0.4656(5) 0.4974(3) 0.0953(18) Uani 1 1 d . . . Ni1 Ni 0.5000 1.0000 0.5000 0.03954(19) Uani 1 2 d S . . O1 O 0.6865(3) 0.7690(3) 0.76778(15) 0.0391(6) Uani 1 1 d . . . O2 O 1.0474(3) 0.9865(3) 0.72073(13) 0.0355(6) Uani 1 1 d . . . S1 S 0.64786(15) 0.83622(12) 0.45360(6) 0.0526(3) Uani 1 1 d . . . S2 S 0.42105(14) 0.86326(12) 0.60640(6) 0.0482(3) 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 Br1 0.0543(3) 0.0722(4) 0.0540(3) -0.0055(2) 0.0118(2) -0.0117(3) Br2 0.0650(3) 0.0581(3) 0.0633(3) -0.0266(2) -0.0232(2) -0.0080(2) C1 0.0234(18) 0.040(2) 0.043(2) -0.0130(16) -0.0069(15) -0.0027(15) C2 0.044(3) 0.043(2) 0.065(3) -0.021(2) -0.011(2) -0.0060(19) C3 0.035(2) 0.045(2) 0.054(3) -0.003(2) 0.0018(19) -0.0149(19) C4 0.025(2) 0.046(2) 0.047(2) 0.0008(18) 0.0002(16) -0.0038(17) C5 0.033(2) 0.045(2) 0.039(2) -0.0140(17) -0.0059(16) 0.0005(17) C6 0.0264(19) 0.036(2) 0.037(2) -0.0033(16) -0.0049(15) -0.0021(15) C7 0.037(2) 0.037(2) 0.042(2) -0.0155(16) -0.0055(17) 0.0038(17) C8 0.054(3) 0.030(2) 0.054(3) -0.0047(18) -0.009(2) 0.0050(19) C9 0.071(3) 0.043(3) 0.059(3) -0.002(2) -0.023(3) 0.014(2) C10 0.054(3) 0.054(3) 0.036(2) 0.0018(19) -0.0096(19) -0.008(2) C11 0.044(3) 0.070(3) 0.036(2) -0.016(2) -0.0055(18) -0.006(2) C12 0.058(3) 0.067(3) 0.047(3) -0.031(2) -0.007(2) 0.004(2) C13 0.055(3) 0.044(3) 0.067(3) -0.023(2) -0.002(2) 0.006(2) C14 0.051(3) 0.039(2) 0.071(3) -0.007(2) -0.009(2) 0.008(2) C15 0.041(2) 0.034(2) 0.052(3) -0.0014(18) -0.0070(19) -0.0054(18) C16 0.045(2) 0.043(2) 0.031(2) -0.0025(16) -0.0111(17) 0.0003(18) C17 0.0253(18) 0.041(2) 0.0312(19) -0.0041(15) -0.0043(14) -0.0050(15) C18 0.031(2) 0.046(2) 0.033(2) -0.0079(16) -0.0046(15) -0.0033(17) C19 0.036(2) 0.040(2) 0.042(2) -0.0172(17) -0.0104(17) 0.0002(17) C20 0.032(2) 0.040(2) 0.048(2) -0.0086(18) 0.0003(17) -0.0063(17) C21 0.039(2) 0.044(2) 0.034(2) -0.0053(16) 0.0002(16) -0.0086(18) C22 0.0273(19) 0.038(2) 0.035(2) -0.0075(15) -0.0046(15) -0.0011(16) C23 0.055(3) 0.055(3) 0.060(3) -0.014(2) 0.008(2) -0.016(2) C24 0.042(2) 0.044(2) 0.050(3) -0.0116(19) -0.0023(19) -0.0067(19) C25 0.044(2) 0.050(3) 0.046(2) -0.0136(19) -0.0068(19) -0.002(2) C26 0.064(3) 0.058(3) 0.062(3) -0.019(2) 0.003(2) -0.002(3) Mn1 0.0296(3) 0.0341(3) 0.0305(3) -0.0095(2) -0.0048(2) 0.0000(2) N1 0.0358(18) 0.0327(17) 0.0341(17) -0.0054(13) -0.0045(13) -0.0026(13) N2 0.043(2) 0.051(2) 0.0389(19) -0.0122(15) -0.0105(15) -0.0006(16) N3 0.040(2) 0.046(2) 0.046(2) -0.0170(15) -0.0074(15) 0.0024(16) N4 0.0352(18) 0.0321(17) 0.0373(17) -0.0058(13) -0.0047(13) -0.0034(14) N5 0.116(5) 0.058(3) 0.076(3) -0.004(2) 0.017(3) -0.014(3) N6 0.105(5) 0.066(3) 0.106(4) -0.030(3) 0.008(3) 0.018(3) Ni1 0.0385(4) 0.0476(4) 0.0334(4) -0.0103(3) -0.0064(3) -0.0007(3) O1 0.0352(15) 0.0397(15) 0.0456(16) -0.0175(12) -0.0049(12) -0.0022(12) O2 0.0342(14) 0.0458(16) 0.0272(13) -0.0083(11) -0.0018(10) -0.0091(12) S1 0.0614(8) 0.0564(7) 0.0369(6) -0.0124(5) -0.0015(5) 0.0058(6) S2 0.0473(6) 0.0496(6) 0.0440(6) -0.0103(5) 0.0020(5) -0.0005(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 Br1 C4 1.890(4) . ? Br2 C19 1.900(4) . ? C1 O1 1.339(4) . ? C1 C2 1.405(5) . ? C1 C6 1.407(5) . ? C2 C3 1.381(6) . ? C2 H2 0.9300 . ? C3 C4 1.377(6) . ? C3 H3 0.9300 . ? C4 C5 1.395(5) . ? C5 C6 1.372(5) . ? C5 H5 0.9300 . ? C6 C7 1.475(5) . ? C7 N1 1.249(5) . ? C7 H7 0.9300 . ? C8 N1 1.481(5) . ? C8 C9 1.513(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.524(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.481(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.483(5) . ? C11 C12 1.499(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N3 1.479(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N3 1.498(5) . ? C13 C14 1.506(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.511(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N4 1.466(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N4 1.286(5) . ? C16 C17 1.432(5) . ? C16 H16 0.9300 . ? C17 C18 1.400(5) . ? C17 C22 1.414(5) . ? C18 C19 1.398(5) . ? C18 H18 0.9300 . ? C19 C20 1.374(5) . ? C20 C21 1.365(5) . ? C20 H20 0.9300 . ? C21 C22 1.420(5) . ? C21 H21 0.9300 . ? C22 O2 1.318(4) . ? C23 N5 1.148(6) . ? C23 C24 1.410(6) . ? C24 C25 1.371(6) . ? C24 S2 1.739(4) . ? C25 C26 1.435(7) . ? C25 S1 1.723(4) . ? C26 N6 1.138(7) . ? Mn1 O2 1.869(2) . ? Mn1 O1 1.878(3) . ? Mn1 N4 2.016(3) . ? Mn1 N1 2.020(3) . ? Mn1 N2 2.071(3) . ? Mn1 N3 2.091(3) . ? N2 H28 0.9100 . ? N3 H27 0.9100 . ? Ni1 S1 2.1697(12) . ? Ni1 S1 2.1697(12) 2_676 ? Ni1 S2 2.1882(11) 2_676 ? Ni1 S2 2.1882(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 119.5(4) . . ? O1 C1 C6 123.1(3) . . ? C2 C1 C6 117.4(4) . . ? C3 C2 C1 121.3(4) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 Br1 120.7(3) . . ? C5 C4 Br1 119.5(3) . . ? C6 C5 C4 120.3(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 121.1(3) . . ? C5 C6 C7 119.0(4) . . ? C1 C6 C7 119.5(3) . . ? N1 C7 C6 125.3(4) . . ? N1 C7 H7 117.4 . . ? C6 C7 H7 117.4 . . ? N1 C8 C9 110.0(3) . . ? N1 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? N1 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C8 C9 C10 114.9(4) . . ? C8 C9 H9A 108.5 . . ? C10 C9 H9A 108.5 . . ? C8 C9 H9B 108.5 . . ? C10 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? N2 C10 C9 112.2(4) . . ? N2 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? N2 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N2 C11 C12 109.9(4) . . ? N2 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? N2 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? N3 C12 C11 108.3(3) . . ? N3 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? N3 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? N3 C13 C14 113.0(4) . . ? N3 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? N3 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C13 C14 C15 114.6(4) . . ? C13 C14 H14A 108.6 . . ? C15 C14 H14A 108.6 . . ? C13 C14 H14B 108.6 . . ? C15 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? N4 C15 C14 111.3(3) . . ? N4 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? N4 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? N4 C16 C17 125.2(3) . . ? N4 C16 H16 117.4 . . ? C17 C16 H16 117.4 . . ? C18 C17 C22 120.6(3) . . ? C18 C17 C16 118.3(3) . . ? C22 C17 C16 120.6(3) . . ? C19 C18 C17 119.0(3) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C20 C19 C18 120.9(3) . . ? C20 C19 Br2 121.3(3) . . ? C18 C19 Br2 117.7(3) . . ? C21 C20 C19 120.7(4) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 121.0(4) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? O2 C22 C17 122.7(3) . . ? O2 C22 C21 119.5(3) . . ? C17 C22 C21 117.7(3) . . ? N5 C23 C24 178.2(6) . . ? C25 C24 C23 122.2(4) . . ? C25 C24 S2 119.9(3) . . ? C23 C24 S2 117.8(4) . . ? C24 C25 C26 121.1(4) . . ? C24 C25 S1 121.2(4) . . ? C26 C25 S1 117.7(4) . . ? N6 C26 C25 178.5(7) . . ? O2 Mn1 O1 179.18(11) . . ? O2 Mn1 N4 88.65(11) . . ? O1 Mn1 N4 90.90(12) . . ? O2 Mn1 N1 91.02(12) . . ? O1 Mn1 N1 88.36(12) . . ? N4 Mn1 N1 97.34(13) . . ? O2 Mn1 N2 88.74(12) . . ? O1 Mn1 N2 91.78(13) . . ? N4 Mn1 N2 172.80(14) . . ? N1 Mn1 N2 89.41(13) . . ? O2 Mn1 N3 91.20(13) . . ? O1 Mn1 N3 89.48(12) . . ? N4 Mn1 N3 88.90(13) . . ? N1 Mn1 N3 173.42(13) . . ? N2 Mn1 N3 84.44(13) . . ? C7 N1 C8 118.3(3) . . ? C7 N1 Mn1 122.3(3) . . ? C8 N1 Mn1 118.9(3) . . ? C10 N2 C11 111.1(3) . . ? C10 N2 Mn1 118.4(3) . . ? C11 N2 Mn1 106.3(3) . . ? C10 N2 H28 106.8 . . ? C11 N2 H28 106.8 . . ? Mn1 N2 H28 106.8 . . ? C12 N3 C13 111.3(3) . . ? C12 N3 Mn1 106.6(3) . . ? C13 N3 Mn1 117.1(3) . . ? C12 N3 H27 107.1 . . ? C13 N3 H27 107.1 . . ? Mn1 N3 H27 107.1 . . ? C16 N4 C15 117.2(3) . . ? C16 N4 Mn1 121.9(3) . . ? C15 N4 Mn1 119.9(2) . . ? S1 Ni1 S1 180.0 . 2_676 ? S1 Ni1 S2 88.14(4) . 2_676 ? S1 Ni1 S2 91.86(4) 2_676 2_676 ? S1 Ni1 S2 91.86(4) . . ? S1 Ni1 S2 88.14(4) 2_676 . ? S2 Ni1 S2 180.00(5) 2_676 . ? C1 O1 Mn1 122.9(2) . . ? C22 O2 Mn1 124.3(2) . . ? C25 S1 Ni1 103.69(16) . . ? C24 S2 Ni1 103.27(15) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.653 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.100 _database_code_depnum_ccdc_archive 'CCDC 976200' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ni-350 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C22 H26 Br2 Mn N4 O2), C8 N4 Ni S4 ' _chemical_formula_sum 'C52 H52 Br4 Mn2 N12 Ni O4 S4' _chemical_formula_weight 1525.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.308(2) _cell_length_b 10.025(2) _cell_length_c 18.528(5) _cell_angle_alpha 78.414(4) _cell_angle_beta 79.045(4) _cell_angle_gamma 84.969(4) _cell_volume 1482.3(6) _cell_formula_units_Z 1 _cell_measurement_temperature 350(2) _cell_measurement_reflns_used 2332 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 24.101 _exptl_crystal_description plate-like _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 3.625 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2644 _exptl_absorpt_correction_T_max 0.7132 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 350(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11045 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_unetI/netI 0.0822 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5141 _reflns_number_gt 3608 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0989P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5141 _refine_ls_number_parameters 358 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1777 _refine_ls_wR_factor_gt 0.1416 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.037 _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 Br1 Br 0.22848(6) 0.71707(5) 1.06577(3) 0.07705(17) Uani 1 1 d . . . Br2 Br 1.27896(6) 1.26809(5) 0.93769(3) 0.07219(14) Uani 1 1 d . . . C1 C 0.5824(4) 0.7608(4) 0.8339(2) 0.0407(9) Uani 1 1 d . . . C2 C 0.5023(5) 0.6416(4) 0.8653(2) 0.0555(12) Uani 1 1 d . . . H2 H 0.5183 0.5693 0.8397 0.067 Uiso 1 1 calc R . . C3 C 0.3989(5) 0.6286(4) 0.9341(2) 0.0550(12) Uani 1 1 d . . . H3 H 0.3489 0.5469 0.9551 0.066 Uiso 1 1 calc R . . C4 C 0.3703(4) 0.7353(4) 0.9711(2) 0.0461(10) Uani 1 1 d . . . C5 C 0.4404(4) 0.8561(4) 0.9408(2) 0.0462(10) Uani 1 1 d . . . H5 H 0.4169 0.9285 0.9662 0.055 Uiso 1 1 calc R . . C6 C 0.5472(4) 0.8732(4) 0.8717(2) 0.0439(10) Uani 1 1 d . . . C7 C 0.5996(4) 1.0051(4) 0.8367(2) 0.0455(10) Uani 1 1 d . . . H7 H 0.5431 1.0790 0.8551 0.055 Uiso 1 1 calc R . . C8 C 0.7344(5) 1.1710(4) 0.7395(2) 0.0516(11) Uani 1 1 d . . . H8A H 0.8464 1.1976 0.7335 0.062 Uiso 1 1 calc R . . H8B H 0.6627 1.2324 0.7670 0.062 Uiso 1 1 calc R . . C9 C 0.6885(5) 1.1808(4) 0.6642(2) 0.0646(14) Uani 1 1 d . . . H9A H 0.6787 1.2763 0.6411 0.078 Uiso 1 1 calc R . . H9B H 0.5816 1.1435 0.6709 0.078 Uiso 1 1 calc R . . C10 C 0.8132(6) 1.1050(4) 0.6099(2) 0.0627(13) Uani 1 1 d . . . H10A H 0.7840 1.1267 0.5605 0.075 Uiso 1 1 calc R . . H10B H 0.9223 1.1362 0.6061 0.075 Uiso 1 1 calc R . . C11 C 0.9308(5) 0.8819(5) 0.5852(2) 0.0626(13) Uani 1 1 d . . . H11A H 1.0364 0.9228 0.5741 0.075 Uiso 1 1 calc R . . H11B H 0.8905 0.8906 0.5386 0.075 Uiso 1 1 calc R . . C12 C 0.9513(6) 0.7345(4) 0.6191(2) 0.0633(13) Uani 1 1 d . . . H12A H 0.8480 0.6910 0.6267 0.076 Uiso 1 1 calc R . . H12B H 1.0324 0.6887 0.5860 0.076 Uiso 1 1 calc R . . C13 C 1.0022(6) 0.5826(4) 0.7335(3) 0.0641(13) Uani 1 1 d . . . H13A H 1.0748 0.5249 0.7038 0.077 Uiso 1 1 calc R . . H13B H 0.8920 0.5514 0.7408 0.077 Uiso 1 1 calc R . . C14 C 1.0541(6) 0.5664(4) 0.8091(3) 0.0688(15) Uani 1 1 d . . . H14A H 1.0601 0.4700 0.8307 0.083 Uiso 1 1 calc R . . H14B H 1.1637 0.5990 0.8012 0.083 Uiso 1 1 calc R . . C15 C 0.9443(5) 0.6393(4) 0.8652(2) 0.0568(12) Uani 1 1 d . . . H15A H 0.8324 0.6123 0.8715 0.068 Uiso 1 1 calc R . . H15B H 0.9798 0.6139 0.9132 0.068 Uiso 1 1 calc R . . C16 C 1.0252(4) 0.8538(4) 0.8740(2) 0.0433(10) Uani 1 1 d . . . H16 H 1.0476 0.8100 0.9205 0.052 Uiso 1 1 calc R . . C17 C 1.0782(4) 0.9891(4) 0.84693(19) 0.0410(10) Uani 1 1 d . . . C18 C 1.1346(4) 1.0597(4) 0.8955(2) 0.0462(10) Uani 1 1 d . . . H18 H 1.1212 1.0230 0.9464 0.055 Uiso 1 1 calc R . . C19 C 1.2068(4) 1.1783(4) 0.8695(2) 0.0476(10) Uani 1 1 d . . . C20 C 1.2358(4) 1.2333(4) 0.7940(2) 0.0480(11) Uani 1 1 d . . . H20 H 1.2904 1.3138 0.7765 0.058 Uiso 1 1 calc R . . C21 C 1.1826(5) 1.1672(4) 0.7444(2) 0.0488(11) Uani 1 1 d . . . H21 H 1.2021 1.2040 0.6935 0.059 Uiso 1 1 calc R . . C22 C 1.1001(4) 1.0462(4) 0.76988(19) 0.0393(9) Uani 1 1 d . . . C23 C 0.4906(6) 0.5953(5) 0.6491(3) 0.0686(14) Uani 1 1 d . . . C24 C 0.5159(5) 0.7049(4) 0.5896(2) 0.0538(12) Uani 1 1 d . . . C25 C 0.6096(5) 0.6963(4) 0.5241(2) 0.0559(12) Uani 1 1 d . . . C26 C 0.6918(6) 0.5695(5) 0.5082(3) 0.0714(15) Uani 1 1 d . . . Mn1 Mn 0.86853(6) 0.87782(5) 0.74370(3) 0.03757(14) Uani 1 1 d U . . N1 N 0.7198(3) 1.0305(3) 0.78127(17) 0.0433(8) Uani 1 1 d . . . N2 N 0.8144(4) 0.9546(3) 0.63679(17) 0.0501(9) Uani 1 1 d . . . H28 H 0.7123 0.9283 0.6368 0.060 Uiso 1 1 calc R . . N3 N 1.0053(4) 0.7252(3) 0.69134(18) 0.0521(9) Uani 1 1 d U . . H27 H 1.1119 0.7482 0.6807 0.063 Uiso 1 1 calc R . . N4 N 0.9497(4) 0.7876(3) 0.83969(16) 0.0421(8) Uani 1 1 d . . . N5 N 0.4669(7) 0.5043(5) 0.6985(3) 0.1078(19) Uani 1 1 d . . . N6 N 0.7564(6) 0.4729(5) 0.4940(3) 0.114(2) Uani 1 1 d . . . Ni1 Ni 0.5000 1.0000 0.5000 0.04668(19) Uani 1 2 d S . . O1 O 0.6852(3) 0.7686(3) 0.76942(14) 0.0465(7) Uani 1 1 d . . . O2 O 1.0500(3) 0.9882(2) 0.72044(13) 0.0430(6) Uani 1 1 d U . . S1 S 0.64792(14) 0.83854(12) 0.45309(6) 0.0617(3) Uani 1 1 d . . . S2 S 0.42188(14) 0.86227(12) 0.60562(6) 0.0586(3) 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 Br1 0.0655(3) 0.0895(4) 0.0628(3) -0.0044(3) 0.0161(2) -0.0141(3) Br2 0.0802(3) 0.0727(3) 0.0787(3) -0.0318(2) -0.0305(2) -0.0093(2) C1 0.0289(16) 0.0463(19) 0.051(2) -0.0178(16) -0.0080(15) 0.0002(15) C2 0.054(2) 0.043(2) 0.071(3) -0.0213(19) -0.002(2) -0.0078(19) C3 0.050(2) 0.052(2) 0.060(2) -0.002(2) -0.0021(19) -0.0162(19) C4 0.0409(19) 0.057(2) 0.0377(18) -0.0061(17) -0.0016(16) -0.0083(18) C5 0.0357(18) 0.060(2) 0.0442(19) -0.0194(17) -0.0041(15) 0.0038(17) C6 0.0344(18) 0.0412(19) 0.056(2) -0.0077(17) -0.0102(16) -0.0004(16) C7 0.0433(19) 0.047(2) 0.048(2) -0.0117(17) -0.0113(16) 0.0022(17) C8 0.058(2) 0.0374(19) 0.054(2) -0.0023(17) -0.0064(19) 0.0001(18) C9 0.059(2) 0.057(2) 0.071(3) 0.007(2) -0.016(2) 0.005(2) C10 0.070(3) 0.072(3) 0.045(2) 0.000(2) -0.017(2) -0.009(2) C11 0.058(2) 0.090(3) 0.042(2) -0.022(2) -0.0058(19) -0.001(2) C12 0.063(3) 0.076(3) 0.055(2) -0.032(2) 0.003(2) -0.007(2) C13 0.065(3) 0.049(2) 0.077(3) -0.020(2) -0.006(2) 0.008(2) C14 0.069(3) 0.048(2) 0.082(3) -0.004(2) -0.010(2) 0.007(2) C15 0.056(2) 0.050(2) 0.061(2) 0.001(2) -0.013(2) -0.007(2) C16 0.0412(19) 0.049(2) 0.0386(18) -0.0037(16) -0.0092(15) 0.0001(17) C17 0.0389(18) 0.045(2) 0.0373(18) -0.0042(16) -0.0057(15) -0.0022(16) C18 0.046(2) 0.052(2) 0.0423(19) -0.0095(17) -0.0129(16) -0.0009(18) C19 0.043(2) 0.0428(19) 0.061(2) -0.0178(17) -0.0134(17) 0.0025(17) C20 0.042(2) 0.0427(19) 0.057(2) -0.0093(18) -0.0005(18) -0.0074(17) C21 0.044(2) 0.054(2) 0.043(2) -0.0030(18) 0.0014(17) -0.0078(18) C22 0.0329(17) 0.0438(19) 0.0393(18) -0.0080(16) -0.0025(15) -0.0001(16) C23 0.061(3) 0.060(3) 0.080(3) -0.010(2) 0.004(2) -0.019(2) C24 0.050(2) 0.045(2) 0.065(3) -0.0071(19) -0.0043(19) -0.0097(18) C25 0.055(2) 0.060(2) 0.054(2) -0.0140(19) -0.0098(19) 0.000(2) C26 0.073(3) 0.065(3) 0.073(3) -0.015(2) -0.001(3) -0.006(3) Mn1 0.0350(3) 0.0406(3) 0.0374(3) -0.0091(2) -0.0057(2) -0.0010(2) N1 0.0396(16) 0.0445(16) 0.0469(16) -0.0132(13) -0.0059(13) -0.0007(14) N2 0.0455(17) 0.0587(19) 0.0477(17) -0.0107(15) -0.0115(14) -0.0029(16) N3 0.0397(16) 0.0585(16) 0.0592(19) -0.0208(13) -0.0012(14) -0.0019(14) N4 0.0421(16) 0.0396(16) 0.0426(16) -0.0024(13) -0.0063(13) -0.0068(14) N5 0.136(4) 0.066(3) 0.105(4) 0.002(3) 0.011(3) -0.028(3) N6 0.119(4) 0.083(3) 0.135(4) -0.042(3) 0.001(4) 0.013(3) Ni1 0.0452(4) 0.0559(4) 0.0391(3) -0.0095(3) -0.0080(3) -0.0008(3) O1 0.0438(13) 0.0528(14) 0.0439(13) -0.0150(12) -0.0032(11) -0.0048(12) O2 0.0424(12) 0.0508(14) 0.0349(12) -0.0054(11) -0.0057(10) -0.0067(9) S1 0.0700(7) 0.0660(6) 0.0442(5) -0.0115(5) -0.0016(5) 0.0062(6) S2 0.0546(6) 0.0612(6) 0.0535(6) -0.0091(5) 0.0042(5) -0.0013(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 Br1 C4 1.903(3) . ? Br2 C19 1.898(4) . ? C1 O1 1.323(4) . ? C1 C2 1.386(5) . ? C1 C6 1.425(5) . ? C2 C3 1.384(6) . ? C2 H2 0.9300 . ? C3 C4 1.363(6) . ? C3 H3 0.9300 . ? C4 C5 1.359(5) . ? C5 C6 1.400(5) . ? C5 H5 0.9300 . ? C6 C7 1.417(5) . ? C7 N1 1.291(4) . ? C7 H7 0.9300 . ? C8 N1 1.468(4) . ? C8 C9 1.497(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.560(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.490(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.478(5) . ? C11 C12 1.494(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N3 1.474(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N3 1.485(5) . ? C13 C14 1.517(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.508(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N4 1.468(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N4 1.278(5) . ? C16 C17 1.426(5) . ? C16 H16 0.9300 . ? C17 C22 1.411(5) . ? C17 C18 1.415(5) . ? C18 C19 1.339(5) . ? C18 H18 0.9300 . ? C19 C20 1.379(5) . ? C20 C21 1.389(6) . ? C20 H20 0.9300 . ? C21 C22 1.399(5) . ? C21 H21 0.9300 . ? C22 O2 1.324(4) . ? C23 N5 1.156(6) . ? C23 C24 1.391(6) . ? C24 C25 1.326(6) . ? C24 S2 1.752(4) . ? C25 C26 1.446(6) . ? C25 S1 1.742(4) . ? C26 N6 1.119(6) . ? Mn1 O2 1.881(3) . ? Mn1 O1 1.885(3) . ? Mn1 N1 2.031(3) . ? Mn1 N4 2.034(3) . ? Mn1 N2 2.094(3) . ? Mn1 N3 2.108(3) . ? N2 H28 0.9100 . ? N3 H27 0.9100 . ? Ni1 S1 2.1670(12) 2_676 ? Ni1 S1 2.1670(12) . ? Ni1 S2 2.1786(11) 2_676 ? Ni1 S2 2.1786(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 119.8(3) . . ? O1 C1 C6 121.9(3) . . ? C2 C1 C6 118.3(3) . . ? C3 C2 C1 121.0(4) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 120.8(3) . . ? C5 C4 Br1 119.1(3) . . ? C3 C4 Br1 120.1(3) . . ? C4 C5 C6 121.0(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 119.5(3) . . ? C5 C6 C1 118.6(3) . . ? C7 C6 C1 121.3(3) . . ? N1 C7 C6 125.0(3) . . ? N1 C7 H7 117.5 . . ? C6 C7 H7 117.5 . . ? N1 C8 C9 109.7(3) . . ? N1 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? N1 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C8 C9 C10 114.2(3) . . ? C8 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? C8 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? N2 C10 C9 111.3(3) . . ? N2 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? N2 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N2 C11 C12 110.7(3) . . ? N2 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N3 C12 C11 108.0(4) . . ? N3 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? N3 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? N3 C13 C14 113.3(4) . . ? N3 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? N3 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C15 C14 C13 115.9(4) . . ? C15 C14 H14A 108.3 . . ? C13 C14 H14A 108.3 . . ? C15 C14 H14B 108.3 . . ? C13 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? N4 C15 C14 110.4(3) . . ? N4 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? N4 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N4 C16 C17 125.5(3) . . ? N4 C16 H16 117.2 . . ? C17 C16 H16 117.2 . . ? C22 C17 C18 118.6(3) . . ? C22 C17 C16 120.9(3) . . ? C18 C17 C16 119.8(3) . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 121.3(4) . . ? C18 C19 Br2 119.1(3) . . ? C20 C19 Br2 119.6(3) . . ? C19 C20 C21 119.3(4) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C20 C21 C22 121.0(3) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? O2 C22 C21 118.7(3) . . ? O2 C22 C17 122.8(3) . . ? C21 C22 C17 118.5(4) . . ? N5 C23 C24 178.9(6) . . ? C25 C24 C23 123.6(4) . . ? C25 C24 S2 119.9(3) . . ? C23 C24 S2 116.5(3) . . ? C24 C25 C26 122.2(4) . . ? C24 C25 S1 122.0(3) . . ? C26 C25 S1 115.8(3) . . ? N6 C26 C25 178.2(6) . . ? O2 Mn1 O1 178.52(11) . . ? O2 Mn1 N1 90.97(12) . . ? O1 Mn1 N1 88.02(12) . . ? O2 Mn1 N4 88.16(11) . . ? O1 Mn1 N4 90.95(12) . . ? N1 Mn1 N4 99.75(12) . . ? O2 Mn1 N2 89.30(12) . . ? O1 Mn1 N2 91.74(12) . . ? N1 Mn1 N2 88.45(12) . . ? N4 Mn1 N2 171.46(12) . . ? O2 Mn1 N3 91.57(12) . . ? O1 Mn1 N3 89.59(12) . . ? N1 Mn1 N3 171.72(13) . . ? N4 Mn1 N3 88.22(13) . . ? N2 Mn1 N3 83.70(13) . . ? C7 N1 C8 118.4(3) . . ? C7 N1 Mn1 121.2(3) . . ? C8 N1 Mn1 119.9(2) . . ? C11 N2 C10 111.6(3) . . ? C11 N2 Mn1 106.0(2) . . ? C10 N2 Mn1 117.9(3) . . ? C11 N2 H28 106.9 . . ? C10 N2 H28 106.9 . . ? Mn1 N2 H28 106.9 . . ? C12 N3 C13 110.6(3) . . ? C12 N3 Mn1 106.9(2) . . ? C13 N3 Mn1 118.1(2) . . ? C12 N3 H27 106.9 . . ? C13 N3 H27 106.9 . . ? Mn1 N3 H27 106.9 . . ? C16 N4 C15 117.8(3) . . ? C16 N4 Mn1 121.5(2) . . ? C15 N4 Mn1 120.1(3) . . ? S1 Ni1 S1 180.000(1) 2_676 . ? S1 Ni1 S2 91.84(4) 2_676 2_676 ? S1 Ni1 S2 88.16(4) . 2_676 ? S1 Ni1 S2 88.16(4) 2_676 . ? S1 Ni1 S2 91.84(4) . . ? S2 Ni1 S2 180.00(5) 2_676 . ? C1 O1 Mn1 122.9(2) . . ? C22 O2 Mn1 123.5(2) . . ? C25 S1 Ni1 102.96(14) . . ? C24 S2 Ni1 103.25(14) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.957 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.204 _database_code_depnum_ccdc_archive 'CCDC 976201' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ni-400 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C22 H26 Br2 Mn N4 O2), C8 N4 Ni S4 ' _chemical_formula_sum 'C52 H52 Br4 Mn2 N12 Ni O4 S4' _chemical_formula_weight 1525.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3414(15) _cell_length_b 10.0287(18) _cell_length_c 18.604(3) _cell_angle_alpha 78.537(3) _cell_angle_beta 78.887(3) _cell_angle_gamma 85.589(3) _cell_volume 1495.4(5) _cell_formula_units_Z 1 _cell_measurement_temperature 400(2) _cell_measurement_reflns_used 2108 _cell_measurement_theta_min 2.169 _cell_measurement_theta_max 23.3045 _exptl_crystal_description plate-like _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 3.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2667 _exptl_absorpt_correction_T_max 0.7152 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 400(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10930 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_unetI/netI 0.1089 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5165 _reflns_number_gt 3306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0005P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5165 _refine_ls_number_parameters 358 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1228 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.22867(5) 0.72001(5) 1.06628(2) 0.09141(16) Uani 1 1 d . . . Br2 Br 1.27804(5) 1.26904(5) 0.93774(3) 0.08673(14) Uani 1 1 d . . . C1 C 0.5813(3) 0.7626(3) 0.83425(18) 0.0503(9) Uani 1 1 d . . . C2 C 0.5017(4) 0.6427(4) 0.8674(2) 0.0654(11) Uani 1 1 d . . . H2 H 0.5184 0.5693 0.8428 0.078 Uiso 1 1 calc R . . C3 C 0.3989(4) 0.6296(4) 0.9357(2) 0.0673(12) Uani 1 1 d . . . H3 H 0.3488 0.5478 0.9570 0.081 Uiso 1 1 calc R . . C4 C 0.3707(4) 0.7377(4) 0.97204(19) 0.0588(11) Uani 1 1 d . . . C5 C 0.4394(4) 0.8580(3) 0.94020(18) 0.0537(10) Uani 1 1 d . . . H5 H 0.4145 0.9318 0.9643 0.064 Uiso 1 1 calc R . . C6 C 0.5462(3) 0.8737(3) 0.87234(18) 0.0480(9) Uani 1 1 d . . . C7 C 0.6005(4) 1.0077(3) 0.83521(18) 0.0543(10) Uani 1 1 d . . . H7 H 0.5434 1.0818 0.8527 0.065 Uiso 1 1 calc R . . C8 C 0.7332(4) 1.1735(3) 0.73784(19) 0.0618(10) Uani 1 1 d U . . H8A H 0.8435 1.2026 0.7332 0.074 Uiso 1 1 calc R . . H8B H 0.6585 1.2346 0.7638 0.074 Uiso 1 1 calc R . . C9 C 0.6942(5) 1.1804(4) 0.6612(2) 0.0783(13) Uani 1 1 d . . . H9A H 0.6896 1.2752 0.6370 0.094 Uiso 1 1 calc R . . H9B H 0.5863 1.1455 0.6670 0.094 Uiso 1 1 calc R . . C10 C 0.8132(5) 1.1031(4) 0.6103(2) 0.0736(13) Uani 1 1 d . . . H10A H 0.7847 1.1235 0.5610 0.088 Uiso 1 1 calc R . . H10B H 0.9223 1.1347 0.6059 0.088 Uiso 1 1 calc R . . C11 C 0.9310(5) 0.8821(4) 0.5853(2) 0.0766(11) Uani 1 1 d U . . H11A H 1.0361 0.9240 0.5742 0.092 Uiso 1 1 calc R . . H11B H 0.8911 0.8903 0.5389 0.092 Uiso 1 1 calc R . . C12 C 0.9515(5) 0.7346(4) 0.6189(2) 0.0755(11) Uani 1 1 d U . . H12A H 0.8486 0.6904 0.6262 0.091 Uiso 1 1 calc R . . H12B H 1.0322 0.6901 0.5855 0.091 Uiso 1 1 calc R . . C13 C 0.9992(5) 0.5814(4) 0.7337(2) 0.0779(13) Uani 1 1 d . . . H13A H 0.8881 0.5514 0.7426 0.094 Uiso 1 1 calc R . . H13B H 1.0680 0.5225 0.7039 0.094 Uiso 1 1 calc R . . C14 C 1.0536(5) 0.5654(4) 0.8065(2) 0.0795(14) Uani 1 1 d . . . H14A H 1.1631 0.5988 0.7974 0.095 Uiso 1 1 calc R . . H14B H 1.0600 0.4690 0.8276 0.095 Uiso 1 1 calc R . . C15 C 0.9458(4) 0.6379(3) 0.8642(2) 0.0655(11) Uani 1 1 d . . . H15A H 0.8336 0.6115 0.8711 0.079 Uiso 1 1 calc R . . H15B H 0.9823 0.6116 0.9117 0.079 Uiso 1 1 calc R . . C16 C 1.0264(4) 0.8528(3) 0.87405(18) 0.0527(10) Uani 1 1 d . . . H16 H 1.0460 0.8100 0.9209 0.063 Uiso 1 1 calc R . . C17 C 1.0803(3) 0.9903(3) 0.84606(17) 0.0469(9) Uani 1 1 d . . . C18 C 1.1340(4) 1.0595(4) 0.89531(18) 0.0554(10) Uani 1 1 d . . . H18 H 1.1200 1.0218 0.9459 0.066 Uiso 1 1 calc R . . C19 C 1.2051(3) 1.1798(3) 0.86988(18) 0.0505(9) Uani 1 1 d . . . C20 C 1.2345(4) 1.2348(3) 0.7944(2) 0.0571(10) Uani 1 1 d . . . H20 H 1.2888 1.3157 0.7771 0.068 Uiso 1 1 calc R . . C21 C 1.1826(4) 1.1689(4) 0.74495(19) 0.0560(10) Uani 1 1 d . . . H21 H 1.2027 1.2057 0.6942 0.067 Uiso 1 1 calc R . . C22 C 1.1008(3) 1.0482(3) 0.77025(17) 0.0468(8) Uani 1 1 d U . . C23 C 0.4905(5) 0.5928(4) 0.6481(2) 0.0811(14) Uani 1 1 d . . . C24 C 0.5165(4) 0.7066(4) 0.5880(2) 0.0633(11) Uani 1 1 d . . . C25 C 0.6130(4) 0.6982(4) 0.5227(2) 0.0623(11) Uani 1 1 d . . . C26 C 0.6912(5) 0.5721(5) 0.5080(2) 0.0838(14) Uani 1 1 d . . . Mn1 Mn 0.86883(5) 0.87838(5) 0.74392(3) 0.04494(13) Uani 1 1 d U . . N1 N 0.7184(3) 1.0334(3) 0.78119(14) 0.0505(7) Uani 1 1 d U . . N2 N 0.8151(3) 0.9537(3) 0.63661(15) 0.0576(8) Uani 1 1 d U . . H28 H 0.7136 0.9261 0.6369 0.069 Uiso 1 1 calc R . . N3 N 1.0044(3) 0.7231(3) 0.69046(15) 0.0599(8) Uani 1 1 d U . . H27 H 1.1110 0.7460 0.6799 0.072 Uiso 1 1 calc R . . N4 N 0.9542(3) 0.7868(3) 0.83901(15) 0.0512(8) Uani 1 1 d . . . N5 N 0.4701(6) 0.5045(4) 0.6971(2) 0.1230(17) Uani 1 1 d . . . N6 N 0.7586(5) 0.4750(4) 0.4953(3) 0.1322(19) Uani 1 1 d . . . Ni1 Ni 0.5000 1.0000 0.5000 0.05505(18) Uani 1 2 d S . . O1 O 0.6848(2) 0.7686(2) 0.77052(12) 0.0529(6) Uani 1 1 d . . . O2 O 1.0498(2) 0.9890(2) 0.72117(11) 0.0506(6) Uani 1 1 d U . . S1 S 0.64719(13) 0.83997(11) 0.45249(5) 0.0724(3) Uani 1 1 d . . . S2 S 0.42221(11) 0.86123(10) 0.60538(5) 0.0674(3) 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 Br1 0.0818(3) 0.1067(4) 0.0712(3) -0.0068(2) 0.0161(2) -0.0151(2) Br2 0.1005(3) 0.0878(3) 0.0905(3) -0.0394(2) -0.0385(2) -0.0071(2) C1 0.0410(15) 0.058(2) 0.0521(19) -0.0108(16) -0.0074(14) -0.0012(14) C2 0.0611(19) 0.053(2) 0.085(3) -0.0237(19) -0.0057(19) -0.0086(16) C3 0.0552(18) 0.056(2) 0.087(3) -0.006(2) -0.0068(19) -0.0156(16) C4 0.0523(17) 0.069(2) 0.050(2) -0.0023(17) -0.0027(16) -0.0100(17) C5 0.0501(16) 0.059(2) 0.054(2) -0.0173(16) -0.0103(15) 0.0042(16) C6 0.0430(15) 0.0472(19) 0.0558(19) -0.0139(15) -0.0097(14) -0.0002(14) C7 0.0544(17) 0.053(2) 0.056(2) -0.0174(16) -0.0091(16) 0.0065(15) C8 0.0665(19) 0.0483(15) 0.066(2) -0.0037(15) -0.0088(18) 0.0020(16) C9 0.084(2) 0.066(3) 0.077(3) 0.004(2) -0.021(2) 0.013(2) C10 0.082(2) 0.084(3) 0.053(2) -0.001(2) -0.0215(19) 0.003(2) C11 0.076(2) 0.1066(17) 0.050(2) -0.0263(18) -0.0066(19) -0.005(2) C12 0.077(2) 0.0977(18) 0.061(2) -0.0400(17) -0.0075(19) -0.004(2) C13 0.087(2) 0.065(2) 0.084(3) -0.030(2) -0.008(2) 0.006(2) C14 0.077(2) 0.062(3) 0.090(3) -0.004(2) -0.008(2) 0.0141(19) C15 0.072(2) 0.051(2) 0.070(2) -0.0024(18) -0.0140(19) -0.0050(17) C16 0.0516(16) 0.061(2) 0.0483(19) -0.0069(16) -0.0162(15) -0.0070(15) C17 0.0451(15) 0.054(2) 0.0411(17) -0.0085(15) -0.0087(14) -0.0007(14) C18 0.0546(17) 0.069(2) 0.0424(18) -0.0119(16) -0.0089(15) 0.0018(16) C19 0.0475(16) 0.053(2) 0.0582(19) -0.0207(16) -0.0188(15) 0.0027(14) C20 0.0541(17) 0.050(2) 0.067(2) -0.0139(17) -0.0068(17) -0.0041(15) C21 0.0552(18) 0.059(2) 0.0463(19) -0.0013(16) 0.0010(16) -0.0070(16) C22 0.0426(14) 0.0524(19) 0.0461(15) -0.0098(12) -0.0109(12) 0.0024(13) C23 0.091(3) 0.069(3) 0.079(3) -0.013(2) 0.000(2) -0.018(2) C24 0.0597(18) 0.063(2) 0.066(2) -0.0080(19) -0.0108(18) -0.0076(17) C25 0.0627(19) 0.060(2) 0.069(2) -0.0172(18) -0.0168(18) -0.0072(17) C26 0.085(3) 0.082(3) 0.085(3) -0.022(2) -0.007(2) -0.004(2) Mn1 0.0462(2) 0.0480(3) 0.0417(3) -0.0114(2) -0.0086(2) 0.0009(2) N1 0.0568(14) 0.0470(13) 0.0461(15) -0.0064(11) -0.0087(13) -0.0005(12) N2 0.0580(14) 0.0674(19) 0.0488(12) -0.0092(13) -0.0144(12) -0.0044(14) N3 0.0568(15) 0.0626(16) 0.0619(18) -0.0219(13) -0.0057(14) 0.0016(12) N4 0.0561(14) 0.0409(16) 0.0561(16) -0.0023(13) -0.0133(13) -0.0077(12) N5 0.156(4) 0.082(3) 0.108(3) 0.003(2) 0.019(3) -0.023(3) N6 0.137(4) 0.103(3) 0.158(4) -0.057(3) -0.009(3) 0.027(3) Ni1 0.0553(3) 0.0662(4) 0.0453(3) -0.0125(3) -0.0119(3) -0.0001(3) O1 0.0539(11) 0.0531(13) 0.0552(13) -0.0193(10) -0.0075(10) -0.0059(10) O2 0.0532(11) 0.0628(14) 0.0361(11) -0.0086(9) -0.0083(9) -0.0053(10) S1 0.0863(6) 0.0786(7) 0.0487(5) -0.0152(5) -0.0051(5) 0.0095(5) S2 0.0680(5) 0.0716(6) 0.0565(6) -0.0108(5) 0.0016(5) -0.0006(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 Br1 C4 1.902(3) . ? Br2 C19 1.896(4) . ? C1 O1 1.319(3) . ? C1 C2 1.392(5) . ? C1 C6 1.419(5) . ? C2 C3 1.377(5) . ? C2 H2 0.9300 . ? C3 C4 1.371(5) . ? C3 H3 0.9300 . ? C4 C5 1.352(5) . ? C5 C6 1.386(4) . ? C5 H5 0.9300 . ? C6 C7 1.447(4) . ? C7 N1 1.264(4) . ? C7 H7 0.9300 . ? C8 N1 1.475(4) . ? C8 C9 1.509(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.515(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.481(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.473(5) . ? C11 C12 1.497(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N3 1.463(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.484(6) . ? C13 N3 1.487(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.526(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N4 1.476(4) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N4 1.269(4) . ? C16 C17 1.447(5) . ? C16 H16 0.9300 . ? C17 C22 1.397(4) . ? C17 C18 1.408(5) . ? C18 C19 1.343(5) . ? C18 H18 0.9300 . ? C19 C20 1.384(5) . ? C20 C21 1.382(5) . ? C20 H20 0.9300 . ? C21 C22 1.389(4) . ? C21 H21 0.9300 . ? C22 O2 1.330(4) . ? C23 N5 1.135(5) . ? C23 C24 1.427(5) . ? C24 C25 1.335(5) . ? C24 S2 1.744(4) . ? C25 C26 1.429(6) . ? C25 S1 1.729(4) . ? C26 N6 1.130(6) . ? Mn1 O2 1.875(2) . ? Mn1 O1 1.888(2) . ? Mn1 N4 2.054(3) . ? Mn1 N1 2.065(3) . ? Mn1 N2 2.109(3) . ? Mn1 N3 2.145(3) . ? N2 H28 0.9100 . ? N3 H27 0.9100 . ? Ni1 S1 2.1695(11) 2_676 ? Ni1 S1 2.1695(11) . ? Ni1 S2 2.1829(10) 2_676 ? Ni1 S2 2.1829(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 119.9(3) . . ? O1 C1 C6 123.1(3) . . ? C2 C1 C6 117.0(3) . . ? C3 C2 C1 121.9(3) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C4 C3 C2 119.8(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 120.3(3) . . ? C5 C4 Br1 119.9(3) . . ? C3 C4 Br1 119.8(3) . . ? C4 C5 C6 121.4(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 119.6(3) . . ? C5 C6 C7 119.8(3) . . ? C1 C6 C7 119.8(3) . . ? N1 C7 C6 125.9(3) . . ? N1 C7 H7 117.0 . . ? C6 C7 H7 117.0 . . ? N1 C8 C9 110.5(3) . . ? N1 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 115.8(3) . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9B 108.3 . . ? C10 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? N2 C10 C9 113.5(3) . . ? N2 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? N2 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? N2 C11 C12 110.9(3) . . ? N2 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.0 . . ? N3 C12 C11 109.1(3) . . ? N3 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? N3 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? C14 C13 N3 114.1(3) . . ? C14 C13 H13A 108.7 . . ? N3 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? N3 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 C14 C15 115.8(3) . . ? C13 C14 H14A 108.3 . . ? C15 C14 H14A 108.3 . . ? C13 C14 H14B 108.3 . . ? C15 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? N4 C15 C14 109.9(3) . . ? N4 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? N4 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N4 C16 C17 124.4(3) . . ? N4 C16 H16 117.8 . . ? C17 C16 H16 117.8 . . ? C22 C17 C18 119.3(3) . . ? C22 C17 C16 121.8(3) . . ? C18 C17 C16 118.4(3) . . ? C19 C18 C17 120.6(3) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 120.8(3) . . ? C18 C19 Br2 119.3(3) . . ? C20 C19 Br2 119.8(3) . . ? C21 C20 C19 119.7(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 120.6(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? O2 C22 C21 119.0(3) . . ? O2 C22 C17 122.2(3) . . ? C21 C22 C17 118.8(3) . . ? N5 C23 C24 178.2(5) . . ? C25 C24 C23 122.5(4) . . ? C25 C24 S2 121.0(3) . . ? C23 C24 S2 116.4(3) . . ? C24 C25 C26 121.5(3) . . ? C24 C25 S1 121.1(3) . . ? C26 C25 S1 117.4(3) . . ? N6 C26 C25 177.3(5) . . ? O2 Mn1 O1 177.80(10) . . ? O2 Mn1 N4 87.25(10) . . ? O1 Mn1 N4 91.35(10) . . ? O2 Mn1 N1 90.93(10) . . ? O1 Mn1 N1 87.69(10) . . ? N4 Mn1 N1 101.34(11) . . ? O2 Mn1 N2 89.88(10) . . ? O1 Mn1 N2 91.78(10) . . ? N4 Mn1 N2 170.06(11) . . ? N1 Mn1 N2 88.22(11) . . ? O2 Mn1 N3 92.19(10) . . ? O1 Mn1 N3 89.43(10) . . ? N4 Mn1 N3 87.47(11) . . ? N1 Mn1 N3 170.79(11) . . ? N2 Mn1 N3 83.12(11) . . ? C7 N1 C8 118.9(3) . . ? C7 N1 Mn1 120.9(2) . . ? C8 N1 Mn1 119.60(19) . . ? C11 N2 C10 111.9(3) . . ? C11 N2 Mn1 106.1(2) . . ? C10 N2 Mn1 117.6(2) . . ? C11 N2 H28 106.9 . . ? C10 N2 H28 106.9 . . ? Mn1 N2 H28 106.9 . . ? C12 N3 C13 112.5(3) . . ? C12 N3 Mn1 106.5(2) . . ? C13 N3 Mn1 117.2(2) . . ? C12 N3 H27 106.7 . . ? C13 N3 H27 106.7 . . ? Mn1 N3 H27 106.7 . . ? C16 N4 C15 118.2(3) . . ? C16 N4 Mn1 121.9(2) . . ? C15 N4 Mn1 119.7(2) . . ? S1 Ni1 S1 180.000(1) 2_676 . ? S1 Ni1 S2 91.86(4) 2_676 2_676 ? S1 Ni1 S2 88.14(4) . 2_676 ? S1 Ni1 S2 88.14(4) 2_676 . ? S1 Ni1 S2 91.86(4) . . ? S2 Ni1 S2 180.00(5) 2_676 . ? C1 O1 Mn1 123.1(2) . . ? C22 O2 Mn1 124.18(17) . . ? C25 S1 Ni1 103.38(13) . . ? C24 S2 Ni1 102.60(12) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.591 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.084 _database_code_depnum_ccdc_archive 'CCDC 976202' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ni-473 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C22 H26 Br2 Mn N4 O2), C8 N4 Ni S4 ' _chemical_formula_sum 'C52 H52 Br4 Mn2 N12 Ni O4 S4' _chemical_formula_weight 1525.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.381(3) _cell_length_b 10.044(3) _cell_length_c 18.692(6) _cell_angle_alpha 78.624(6) _cell_angle_beta 78.750(6) _cell_angle_gamma 86.181(6) _cell_volume 1512.2(9) _cell_formula_units_Z 1 _cell_measurement_temperature 473(2) _cell_measurement_reflns_used 1514 _cell_measurement_theta_min 2.764 _cell_measurement_theta_max 19.0885 _exptl_crystal_description plate-like _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 762 _exptl_absorpt_coefficient_mu 3.553 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2696 _exptl_absorpt_correction_T_max 0.7177 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 473(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11203 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_unetI/netI 0.1127 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5233 _reflns_number_gt 2668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5233 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1222 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _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 Br1 Br 0.22951(10) 0.72322(9) 1.06574(4) 0.1129(3) Uani 1 1 d . . . Br2 Br 1.27660(11) 1.26996(8) 0.93773(5) 0.1087(3) Uani 1 1 d . . . C1 C 0.5818(7) 0.7626(6) 0.8348(3) 0.0631(15) Uani 1 1 d . . . C2 C 0.5010(8) 0.6432(7) 0.8690(4) 0.085(2) Uani 1 1 d . . . H2 H 0.5171 0.5691 0.8452 0.102 Uiso 1 1 calc R . . C3 C 0.3988(8) 0.6316(7) 0.9365(4) 0.0822(19) Uani 1 1 d . . . H3 H 0.3476 0.5501 0.9581 0.099 Uiso 1 1 calc R . . C4 C 0.3717(7) 0.7401(7) 0.9723(3) 0.0708(17) Uani 1 1 d . . . C5 C 0.4392(7) 0.8605(7) 0.9401(3) 0.0686(17) Uani 1 1 d . . . H5 H 0.4146 0.9345 0.9638 0.082 Uiso 1 1 calc R . . C6 C 0.5455(7) 0.8758(6) 0.8717(3) 0.0610(15) Uani 1 1 d . . . C7 C 0.5973(7) 1.0080(6) 0.8355(3) 0.0674(16) Uani 1 1 d . . . H7 H 0.5404 1.0813 0.8531 0.081 Uiso 1 1 calc R . . C8 C 0.7331(8) 1.1732(6) 0.7364(3) 0.0748(18) Uani 1 1 d . . . H8A H 0.8432 1.2026 0.7317 0.090 Uiso 1 1 calc R . . H8B H 0.6592 1.2348 0.7618 0.090 Uiso 1 1 calc R . . C9 C 0.6951(9) 1.1785(7) 0.6599(4) 0.095(2) Uani 1 1 d . . . H9A H 0.6900 1.2729 0.6355 0.113 Uiso 1 1 calc R . . H9B H 0.5882 1.1418 0.6657 0.113 Uiso 1 1 calc R . . C10 C 0.8156(9) 1.1020(8) 0.6100(4) 0.094(2) Uani 1 1 d . . . H10A H 0.7896 1.1217 0.5606 0.112 Uiso 1 1 calc R . . H10B H 0.9239 1.1346 0.6063 0.112 Uiso 1 1 calc R . . C11 C 0.9304(9) 0.8812(9) 0.5860(3) 0.095(2) Uani 1 1 d . . . H11A H 1.0359 0.9225 0.5750 0.114 Uiso 1 1 calc R . . H11B H 0.8914 0.8901 0.5396 0.114 Uiso 1 1 calc R . . C12 C 0.9482(9) 0.7352(8) 0.6184(4) 0.100(2) Uani 1 1 d . . . H12A H 1.0266 0.6906 0.5847 0.120 Uiso 1 1 calc R . . H12B H 0.8446 0.6916 0.6267 0.120 Uiso 1 1 calc R . . C13 C 0.9998(9) 0.5820(7) 0.7321(4) 0.098(2) Uani 1 1 d . . . H13A H 1.0701 0.5246 0.7024 0.118 Uiso 1 1 calc R . . H13B H 0.8898 0.5500 0.7404 0.118 Uiso 1 1 calc R . . C14 C 1.0527(9) 0.5679(7) 0.8060(4) 0.099(2) Uani 1 1 d . . . H14A H 1.0597 0.4719 0.8272 0.119 Uiso 1 1 calc R . . H14B H 1.1614 0.6029 0.7971 0.119 Uiso 1 1 calc R . . C15 C 0.9457(8) 0.6380(6) 0.8627(4) 0.0830(19) Uani 1 1 d . . . H15A H 0.8342 0.6109 0.8690 0.100 Uiso 1 1 calc R . . H15B H 0.9806 0.6112 0.9101 0.100 Uiso 1 1 calc R . . C16 C 1.0294(7) 0.8525(6) 0.8724(3) 0.0668(16) Uani 1 1 d . . . H16 H 1.0534 0.8085 0.9179 0.080 Uiso 1 1 calc R . . C17 C 1.0799(7) 0.9901(6) 0.8459(3) 0.0582(14) Uani 1 1 d . . . C18 C 1.1345(7) 1.0608(7) 0.8946(3) 0.0680(16) Uani 1 1 d . . . H18 H 1.1203 1.0235 0.9450 0.082 Uiso 1 1 calc R . . C19 C 1.2067(7) 1.1812(7) 0.8691(4) 0.0670(16) Uani 1 1 d . . . C20 C 1.2349(7) 1.2362(6) 0.7945(4) 0.0688(16) Uani 1 1 d . . . H20 H 1.2898 1.3172 0.7772 0.083 Uiso 1 1 calc R . . C21 C 1.1818(7) 1.1712(6) 0.7457(3) 0.0690(16) Uani 1 1 d . . . H21 H 1.2001 1.2095 0.6954 0.083 Uiso 1 1 calc R . . C22 C 1.1009(7) 1.0488(6) 0.7702(3) 0.0570(14) Uani 1 1 d . . . C23 C 0.4899(10) 0.5934(9) 0.6474(5) 0.099(2) Uani 1 1 d . . . C24 C 0.5160(8) 0.7064(7) 0.5892(4) 0.0778(18) Uani 1 1 d . . . C25 C 0.6108(8) 0.7009(7) 0.5222(4) 0.0784(18) Uani 1 1 d . . . C26 C 0.6907(10) 0.5754(9) 0.5082(5) 0.106(3) Uani 1 1 d . . . Mn1 Mn 0.86877(10) 0.87913(8) 0.74409(4) 0.0574(3) Uani 1 1 d . . . N1 N 0.7167(6) 1.0351(5) 0.7801(3) 0.0624(12) Uani 1 1 d . . . N2 N 0.8167(6) 0.9535(6) 0.6365(3) 0.0777(15) Uani 1 1 d . . . H28 H 0.7152 0.9257 0.6370 0.093 Uiso 1 1 calc R . . N3 N 1.0045(6) 0.7242(5) 0.6901(3) 0.0768(14) Uani 1 1 d . . . H27 H 1.1107 0.7480 0.6788 0.092 Uiso 1 1 calc R . . N4 N 0.9544(6) 0.7864(4) 0.8387(2) 0.0596(12) Uani 1 1 d . . . N5 N 0.4701(11) 0.5070(8) 0.6960(4) 0.153(3) Uani 1 1 d . . . N6 N 0.7541(9) 0.4776(7) 0.4940(5) 0.155(3) Uani 1 1 d . . . Ni1 Ni 0.5000 1.0000 0.5000 0.0700(3) Uani 1 2 d S . . O1 O 0.6851(5) 0.7696(4) 0.7711(2) 0.0686(11) Uani 1 1 d . . . O2 O 1.0503(4) 0.9907(4) 0.72123(18) 0.0624(10) Uani 1 1 d . . . S1 S 0.6461(2) 0.84126(19) 0.45251(9) 0.0892(6) Uani 1 1 d . . . S2 S 0.4231(2) 0.86030(18) 0.60471(9) 0.0861(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 Br1 0.0960(6) 0.1293(7) 0.0951(6) -0.0104(5) 0.0198(4) -0.0159(5) Br2 0.1163(7) 0.1086(6) 0.1238(7) -0.0502(5) -0.0464(5) -0.0086(5) C1 0.048(4) 0.063(4) 0.083(4) -0.020(4) -0.020(3) 0.006(3) C2 0.075(5) 0.065(5) 0.112(6) -0.023(4) -0.003(4) -0.012(4) C3 0.067(5) 0.077(5) 0.097(5) -0.006(4) -0.006(4) -0.021(4) C4 0.060(4) 0.076(5) 0.070(4) -0.003(4) -0.007(3) 0.000(4) C5 0.059(4) 0.074(5) 0.071(4) -0.022(4) -0.004(3) 0.009(4) C6 0.046(4) 0.048(4) 0.084(4) -0.004(3) -0.010(3) 0.004(3) C7 0.059(4) 0.069(4) 0.074(4) -0.020(3) -0.009(3) 0.019(3) C8 0.076(5) 0.059(4) 0.079(4) 0.003(3) -0.008(3) 0.003(3) C9 0.093(6) 0.083(5) 0.099(5) 0.004(4) -0.027(4) 0.018(4) C10 0.095(6) 0.108(6) 0.075(5) 0.002(4) -0.025(4) -0.010(5) C11 0.093(6) 0.138(7) 0.056(4) -0.027(5) -0.010(4) -0.011(5) C12 0.102(6) 0.119(7) 0.087(5) -0.054(5) -0.004(4) 0.005(5) C13 0.099(6) 0.075(5) 0.120(6) -0.040(5) 0.003(5) 0.001(4) C14 0.097(6) 0.072(5) 0.126(6) -0.016(5) -0.018(5) 0.004(4) C15 0.078(5) 0.070(5) 0.098(5) -0.007(4) -0.019(4) -0.001(4) C16 0.053(4) 0.074(4) 0.070(4) -0.003(3) -0.014(3) 0.001(3) C17 0.054(4) 0.063(4) 0.057(4) -0.008(3) -0.009(3) -0.007(3) C18 0.062(4) 0.084(5) 0.058(4) -0.013(4) -0.016(3) 0.006(4) C19 0.058(4) 0.072(4) 0.078(5) -0.026(4) -0.019(3) 0.009(3) C20 0.062(4) 0.057(4) 0.085(5) -0.012(4) -0.005(3) -0.008(3) C21 0.066(4) 0.075(4) 0.061(4) -0.011(3) -0.001(3) -0.007(4) C22 0.046(4) 0.059(4) 0.065(4) -0.012(3) -0.009(3) 0.004(3) C23 0.096(6) 0.086(6) 0.104(6) -0.004(5) 0.002(5) -0.016(5) C24 0.068(4) 0.084(5) 0.081(5) -0.014(4) -0.012(4) -0.007(4) C25 0.080(5) 0.075(5) 0.087(5) -0.024(4) -0.023(4) -0.004(4) C26 0.097(6) 0.094(6) 0.126(7) -0.036(5) 0.000(5) -0.001(5) Mn1 0.0535(6) 0.0591(6) 0.0597(5) -0.0135(4) -0.0094(4) 0.0011(4) N1 0.063(3) 0.056(3) 0.068(3) -0.012(3) -0.012(3) 0.003(3) N2 0.068(4) 0.105(4) 0.062(3) -0.019(3) -0.012(3) -0.010(3) N3 0.061(3) 0.089(4) 0.082(4) -0.028(3) -0.007(3) 0.000(3) N4 0.057(3) 0.050(3) 0.070(3) -0.005(2) -0.014(2) -0.006(2) N5 0.184(8) 0.102(6) 0.135(6) 0.025(5) 0.015(6) -0.017(6) N6 0.148(8) 0.126(7) 0.189(8) -0.069(6) 0.004(6) 0.024(6) Ni1 0.0625(8) 0.0846(8) 0.0638(7) -0.0158(6) -0.0127(5) -0.0004(6) O1 0.060(3) 0.074(3) 0.077(3) -0.032(2) -0.005(2) -0.003(2) O2 0.064(3) 0.072(2) 0.051(2) -0.011(2) -0.0103(18) -0.002(2) S1 0.0950(14) 0.0981(14) 0.0709(11) -0.0195(10) -0.0071(9) 0.0099(11) S2 0.0782(13) 0.0902(13) 0.0799(11) -0.0108(10) 0.0038(9) -0.0021(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C4 1.897(6) . ? Br2 C19 1.898(6) . ? C1 O1 1.321(6) . ? C1 C2 1.394(8) . ? C1 C6 1.429(7) . ? C2 C3 1.369(8) . ? C2 H2 0.9300 . ? C3 C4 1.372(8) . ? C3 H3 0.9300 . ? C4 C5 1.348(8) . ? C5 C6 1.396(7) . ? C5 H5 0.9300 . ? C6 C7 1.421(8) . ? C7 N1 1.292(7) . ? C7 H7 0.9300 . ? C8 N1 1.465(7) . ? C8 C9 1.514(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.515(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.477(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.468(7) . ? C11 C12 1.482(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N3 1.486(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N3 1.487(8) . ? C13 C14 1.509(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.504(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N4 1.471(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N4 1.268(6) . ? C16 C17 1.436(7) . ? C16 H16 0.9300 . ? C17 C22 1.403(7) . ? C17 C18 1.415(7) . ? C18 C19 1.346(8) . ? C18 H18 0.9300 . ? C19 C20 1.374(8) . ? C20 C21 1.375(8) . ? C20 H20 0.9300 . ? C21 C22 1.396(7) . ? C21 H21 0.9300 . ? C22 O2 1.324(6) . ? C23 N5 1.120(9) . ? C23 C24 1.406(9) . ? C24 C25 1.354(8) . ? C24 S2 1.734(7) . ? C25 C26 1.434(10) . ? C25 S1 1.718(7) . ? C26 N6 1.139(9) . ? Mn1 O2 1.881(4) . ? Mn1 O1 1.881(4) . ? Mn1 N4 2.065(5) . ? Mn1 N1 2.084(4) . ? Mn1 N2 2.122(5) . ? Mn1 N3 2.162(5) . ? N2 H28 0.9100 . ? N3 H27 0.9100 . ? Ni1 S1 2.1686(17) . ? Ni1 S1 2.1686(17) 2_676 ? Ni1 S2 2.1818(18) 2_676 ? Ni1 S2 2.1818(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 121.0(5) . . ? O1 C1 C6 122.4(6) . . ? C2 C1 C6 116.6(6) . . ? C3 C2 C1 122.1(6) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C2 C3 C4 120.0(7) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.6(6) . . ? C5 C4 Br1 119.6(5) . . ? C3 C4 Br1 119.8(5) . . ? C4 C5 C6 121.0(6) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 118.9(5) . . ? C5 C6 C1 119.6(6) . . ? C7 C6 C1 120.9(5) . . ? N1 C7 C6 125.5(5) . . ? N1 C7 H7 117.3 . . ? C6 C7 H7 117.3 . . ? N1 C8 C9 110.6(5) . . ? N1 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 115.2(5) . . ? C8 C9 H9A 108.5 . . ? C10 C9 H9A 108.5 . . ? C8 C9 H9B 108.5 . . ? C10 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? N2 C10 C9 113.3(5) . . ? N2 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? N2 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? N2 C11 C12 111.7(5) . . ? N2 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? N2 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C11 C12 N3 108.3(5) . . ? C11 C12 H12A 110.0 . . ? N3 C12 H12A 110.0 . . ? C11 C12 H12B 110.0 . . ? N3 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? N3 C13 C14 112.9(5) . . ? N3 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? N3 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C13 116.3(6) . . ? C15 C14 H14A 108.2 . . ? C13 C14 H14A 108.2 . . ? C15 C14 H14B 108.2 . . ? C13 C14 H14B 108.2 . . ? H14A C14 H14B 107.4 . . ? N4 C15 C14 110.3(5) . . ? N4 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? N4 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N4 C16 C17 125.1(6) . . ? N4 C16 H16 117.5 . . ? C17 C16 H16 117.5 . . ? C22 C17 C18 118.6(5) . . ? C22 C17 C16 121.3(5) . . ? C18 C17 C16 119.3(5) . . ? C19 C18 C17 121.0(5) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 120.8(6) . . ? C18 C19 Br2 118.6(5) . . ? C20 C19 Br2 120.5(5) . . ? C19 C20 C21 119.7(6) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C22 121.3(6) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? O2 C22 C21 119.1(5) . . ? O2 C22 C17 122.4(5) . . ? C21 C22 C17 118.4(5) . . ? N5 C23 C24 176.8(9) . . ? C25 C24 C23 123.2(6) . . ? C25 C24 S2 118.8(6) . . ? C23 C24 S2 118.0(5) . . ? C24 C25 C26 120.0(7) . . ? C24 C25 S1 122.6(5) . . ? C26 C25 S1 117.4(6) . . ? N6 C26 C25 177.2(10) . . ? O2 Mn1 O1 177.51(15) . . ? O2 Mn1 N4 87.25(17) . . ? O1 Mn1 N4 91.22(18) . . ? O2 Mn1 N1 91.25(17) . . ? O1 Mn1 N1 87.17(17) . . ? N4 Mn1 N1 102.82(18) . . ? O2 Mn1 N2 89.91(18) . . ? O1 Mn1 N2 91.95(19) . . ? N4 Mn1 N2 169.25(19) . . ? N1 Mn1 N2 87.6(2) . . ? O2 Mn1 N3 91.98(18) . . ? O1 Mn1 N3 89.91(18) . . ? N4 Mn1 N3 87.04(19) . . ? N1 Mn1 N3 169.77(19) . . ? N2 Mn1 N3 82.7(2) . . ? C7 N1 C8 119.8(5) . . ? C7 N1 Mn1 120.3(4) . . ? C8 N1 Mn1 119.4(4) . . ? C11 N2 C10 112.4(5) . . ? C11 N2 Mn1 106.1(4) . . ? C10 N2 Mn1 117.6(4) . . ? C11 N2 H28 106.7 . . ? C10 N2 H28 106.7 . . ? Mn1 N2 H28 106.7 . . ? C12 N3 C13 111.7(5) . . ? C12 N3 Mn1 106.0(4) . . ? C13 N3 Mn1 117.9(4) . . ? C12 N3 H27 106.9 . . ? C13 N3 H27 106.9 . . ? Mn1 N3 H27 106.9 . . ? C16 N4 C15 118.8(5) . . ? C16 N4 Mn1 121.3(4) . . ? C15 N4 Mn1 119.5(4) . . ? S1 Ni1 S1 180.000(1) . 2_676 ? S1 Ni1 S2 88.47(7) . 2_676 ? S1 Ni1 S2 91.53(7) 2_676 2_676 ? S1 Ni1 S2 91.53(7) . . ? S1 Ni1 S2 88.47(7) 2_676 . ? S2 Ni1 S2 180.000(1) 2_676 . ? C1 O1 Mn1 123.5(4) . . ? C22 O2 Mn1 123.9(3) . . ? C25 S1 Ni1 103.1(2) . . ? C24 S2 Ni1 103.9(2) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.473 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.068 _database_code_depnum_ccdc_archive 'CCDC 976203' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Pt-296 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C22 H26 Br2 Mn N4 O2), C8 N4 Pt S4' _chemical_formula_sum 'C52 H52 Br4 Mn2 N12 O4 Pt S4' _chemical_formula_weight 1661.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2697(4) _cell_length_b 10.0679(5) _cell_length_c 18.4929(10) _cell_angle_alpha 78.6030(10) _cell_angle_beta 79.1010(10) _cell_angle_gamma 84.2880(10) _cell_volume 1479.01(13) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2459 _cell_measurement_theta_min 2.538 _cell_measurement_theta_max 24.127 _exptl_crystal_description plate-like _exptl_crystal_colour black _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 5.677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.213 _exptl_absorpt_correction_T_max 0.506 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9037 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_unetI/netI 0.0482 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5784 _reflns_number_gt 4629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0487P)^2^+0.0122P] 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 5784 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Br1 Br 0.22833(8) 0.71147(7) 1.06535(4) 0.0643(2) Uani 1 1 d . . . Br2 Br 1.27927(8) 1.26564(6) 0.93849(4) 0.05867(19) Uani 1 1 d . . . C1 C 0.5835(6) 0.7597(5) 0.8321(3) 0.0358(12) Uani 1 1 d . . . C2 C 0.5033(7) 0.6395(5) 0.8624(3) 0.0461(14) Uani 1 1 d . . . H2 H 0.5198 0.5684 0.8359 0.055 Uiso 1 1 calc R . . C3 C 0.3997(7) 0.6258(5) 0.9313(3) 0.0483(14) Uani 1 1 d . . . H3 H 0.3483 0.5452 0.9507 0.058 Uiso 1 1 calc R . . C4 C 0.3717(6) 0.7298(6) 0.9715(3) 0.0428(13) Uani 1 1 d . . . C5 C 0.4401(6) 0.8523(6) 0.9409(3) 0.0400(12) Uani 1 1 d . . . H5 H 0.4147 0.9248 0.9663 0.048 Uiso 1 1 calc R . . C6 C 0.5473(6) 0.8686(5) 0.8719(3) 0.0354(12) Uani 1 1 d . . . C7 C 0.6010(6) 1.0030(5) 0.8374(3) 0.0372(12) Uani 1 1 d . . . H7 H 0.5438 1.0766 0.8563 0.045 Uiso 1 1 calc R . . C8 C 0.7308(7) 1.1686(5) 0.7412(3) 0.0436(13) Uani 1 1 d . . . H8A H 0.8416 1.1970 0.7364 0.052 Uiso 1 1 calc R . . H8B H 0.6552 1.2286 0.7687 0.052 Uiso 1 1 calc R . . C9 C 0.6884(7) 1.1796(6) 0.6649(3) 0.0509(15) Uani 1 1 d . . . H9A H 0.6808 1.2748 0.6420 0.061 Uiso 1 1 calc R . . H9B H 0.5802 1.1454 0.6706 0.061 Uiso 1 1 calc R . . C10 C 0.8084(8) 1.1047(6) 0.6121(3) 0.0514(15) Uani 1 1 d . . . H10A H 0.7765 1.1256 0.5631 0.062 Uiso 1 1 calc R . . H10B H 0.9177 1.1364 0.6071 0.062 Uiso 1 1 calc R . . C11 C 0.9334(7) 0.8844(6) 0.5848(3) 0.0484(14) Uani 1 1 d . . . H11A H 1.0390 0.9246 0.5743 0.058 Uiso 1 1 calc R . . H11B H 0.8924 0.8947 0.5381 0.058 Uiso 1 1 calc R . . C12 C 0.9545(8) 0.7378(6) 0.6175(3) 0.0528(15) Uani 1 1 d . . . H12A H 1.0375 0.6927 0.5844 0.063 Uiso 1 1 calc R . . H12B H 0.8514 0.6952 0.6238 0.063 Uiso 1 1 calc R . . C13 C 1.0051(8) 0.5846(6) 0.7330(3) 0.0547(16) Uani 1 1 d . . . H13A H 1.0786 0.5269 0.7032 0.066 Uiso 1 1 calc R . . H13B H 0.8946 0.5540 0.7402 0.066 Uiso 1 1 calc R . . C14 C 1.0578(7) 0.5691(6) 0.8088(3) 0.0525(15) Uani 1 1 d . . . H14A H 1.0665 0.4731 0.8302 0.063 Uiso 1 1 calc R . . H14B H 1.1669 0.6026 0.8011 0.063 Uiso 1 1 calc R . . C15 C 0.9446(7) 0.6414(5) 0.8650(3) 0.0428(13) Uani 1 1 d . . . H15A H 0.8328 0.6144 0.8708 0.051 Uiso 1 1 calc R . . H15B H 0.9797 0.6164 0.9133 0.051 Uiso 1 1 calc R . . C16 C 1.0240(6) 0.8532(5) 0.8744(3) 0.0392(12) Uani 1 1 d . . . H16 H 1.0464 0.8093 0.9210 0.047 Uiso 1 1 calc R . . C17 C 1.0778(6) 0.9899(5) 0.8465(3) 0.0347(11) Uani 1 1 d . . . C18 C 1.1314(6) 1.0582(5) 0.8964(3) 0.0365(12) Uani 1 1 d . . . H18 H 1.1167 1.0220 0.9473 0.044 Uiso 1 1 calc R . . C19 C 1.2050(6) 1.1778(5) 0.8695(3) 0.0381(12) Uani 1 1 d . . . C20 C 1.2340(6) 1.2303(5) 0.7936(3) 0.0419(13) Uani 1 1 d . . . H20 H 1.2883 1.3100 0.7761 0.050 Uiso 1 1 calc R . . C21 C 1.1834(7) 1.1659(5) 0.7444(3) 0.0403(12) Uani 1 1 d . . . H21 H 1.2041 1.2024 0.6935 0.048 Uiso 1 1 calc R . . C22 C 1.0998(6) 1.0445(5) 0.7689(3) 0.0344(11) Uani 1 1 d . . . C23 C 0.4929(8) 0.5874(6) 0.6520(4) 0.0546(16) Uani 1 1 d . . . C24 C 0.5186(7) 0.7012(5) 0.5928(3) 0.0443(13) Uani 1 1 d . . . C25 C 0.6148(7) 0.6881(6) 0.5262(3) 0.0429(13) Uani 1 1 d . . . C26 C 0.6919(8) 0.5585(7) 0.5135(4) 0.0575(16) Uani 1 1 d . . . Mn1 Mn 0.86927(9) 0.87704(7) 0.74364(4) 0.03079(18) Uani 1 1 d . . . N1 N 0.7208(5) 1.0272(4) 0.7833(2) 0.0338(9) Uani 1 1 d . . . N2 N 0.8152(5) 0.9550(4) 0.6381(2) 0.0399(10) Uani 1 1 d . . . H28 H 0.7135 0.9280 0.6379 0.048 Uiso 1 1 calc R . . N3 N 1.0070(5) 0.7259(4) 0.6916(2) 0.0430(11) Uani 1 1 d . . . H27 H 1.1139 0.7482 0.6818 0.052 Uiso 1 1 calc R . . N4 N 0.9482(5) 0.7895(4) 0.8394(2) 0.0346(9) Uani 1 1 d . . . N5 N 0.4728(9) 0.4986(6) 0.7022(4) 0.086(2) Uani 1 1 d . . . N6 N 0.7556(9) 0.4580(6) 0.5016(4) 0.089(2) Uani 1 1 d . . . O1 O 0.6875(4) 0.7680(3) 0.76755(19) 0.0374(8) Uani 1 1 d . . . O2 O 1.0498(4) 0.9861(3) 0.72044(17) 0.0342(8) Uani 1 1 d . . . Pt1 Pt 0.5000 1.0000 0.5000 0.03750(11) Uani 1 2 d S . . S1 S 0.65335(19) 0.82395(15) 0.45312(8) 0.0486(4) Uani 1 1 d . . . S2 S 0.42014(18) 0.85533(14) 0.61129(8) 0.0452(3) 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 Br1 0.0573(4) 0.0717(4) 0.0534(4) -0.0033(3) 0.0118(3) -0.0113(3) Br2 0.0677(4) 0.0576(4) 0.0629(4) -0.0255(3) -0.0249(3) -0.0078(3) C1 0.027(3) 0.038(3) 0.046(3) -0.012(2) -0.012(2) 0.001(2) C2 0.048(3) 0.037(3) 0.052(4) -0.010(3) -0.002(3) -0.006(3) C3 0.046(3) 0.033(3) 0.063(4) -0.003(3) -0.005(3) -0.010(3) C4 0.031(3) 0.054(3) 0.039(3) 0.000(3) -0.003(2) -0.006(3) C5 0.031(3) 0.046(3) 0.043(3) -0.007(3) -0.009(2) 0.000(2) C6 0.026(3) 0.036(3) 0.046(3) -0.011(2) -0.007(2) -0.001(2) C7 0.040(3) 0.031(3) 0.041(3) -0.010(2) -0.007(2) 0.004(2) C8 0.045(3) 0.031(3) 0.051(3) -0.007(2) -0.002(3) 0.004(2) C9 0.052(4) 0.044(3) 0.055(4) 0.001(3) -0.022(3) 0.006(3) C10 0.057(4) 0.056(4) 0.041(3) 0.001(3) -0.016(3) -0.008(3) C11 0.049(3) 0.063(4) 0.036(3) -0.017(3) -0.007(3) 0.002(3) C12 0.057(4) 0.065(4) 0.045(3) -0.030(3) -0.011(3) 0.000(3) C13 0.058(4) 0.042(3) 0.064(4) -0.022(3) -0.002(3) 0.006(3) C14 0.049(4) 0.041(3) 0.065(4) -0.009(3) -0.008(3) 0.010(3) C15 0.044(3) 0.030(3) 0.052(3) 0.002(2) -0.012(3) -0.004(2) C16 0.038(3) 0.044(3) 0.032(3) -0.001(2) -0.003(2) -0.003(2) C17 0.033(3) 0.035(3) 0.037(3) -0.008(2) -0.005(2) -0.003(2) C18 0.036(3) 0.041(3) 0.032(3) -0.009(2) -0.006(2) 0.003(2) C19 0.036(3) 0.035(3) 0.047(3) -0.017(2) -0.009(2) -0.001(2) C20 0.038(3) 0.035(3) 0.052(3) -0.007(3) -0.004(3) -0.005(2) C21 0.047(3) 0.039(3) 0.033(3) -0.004(2) -0.003(2) -0.010(2) C22 0.027(3) 0.036(3) 0.038(3) -0.007(2) -0.004(2) 0.003(2) C23 0.056(4) 0.046(4) 0.058(4) -0.015(3) 0.006(3) -0.005(3) C24 0.044(3) 0.041(3) 0.045(3) -0.004(3) -0.005(3) -0.005(3) C25 0.044(3) 0.045(3) 0.041(3) -0.013(3) -0.006(3) -0.001(3) C26 0.061(4) 0.051(4) 0.055(4) -0.010(3) 0.001(3) 0.000(3) Mn1 0.0312(4) 0.0311(4) 0.0307(4) -0.0086(3) -0.0054(3) 0.0009(3) N1 0.035(2) 0.030(2) 0.035(2) -0.0028(18) -0.008(2) 0.0006(18) N2 0.037(2) 0.049(3) 0.033(2) -0.007(2) -0.007(2) -0.002(2) N3 0.037(3) 0.046(3) 0.046(3) -0.016(2) -0.001(2) -0.001(2) N4 0.035(2) 0.031(2) 0.038(2) -0.0071(19) -0.0063(19) -0.0013(18) N5 0.119(6) 0.051(3) 0.071(4) -0.001(3) 0.017(4) -0.016(4) N6 0.098(5) 0.057(4) 0.097(5) -0.018(4) 0.014(4) 0.011(4) O1 0.035(2) 0.0381(19) 0.041(2) -0.0128(16) -0.0044(16) -0.0047(16) O2 0.0371(19) 0.0422(19) 0.0247(17) -0.0078(15) -0.0048(15) -0.0063(16) Pt1 0.03829(18) 0.04225(18) 0.03274(17) -0.00808(13) -0.00818(13) 0.00002(13) S1 0.0595(9) 0.0483(8) 0.0345(7) -0.0098(6) -0.0017(7) 0.0046(7) S2 0.0470(8) 0.0452(8) 0.0389(8) -0.0061(6) 0.0004(6) 0.0012(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C4 1.895(5) . ? Br2 C19 1.907(5) . ? C1 O1 1.327(6) . ? C1 C2 1.403(7) . ? C1 C6 1.415(7) . ? C2 C3 1.384(8) . ? C2 H2 0.9300 . ? C3 C4 1.378(8) . ? C3 H3 0.9300 . ? C4 C5 1.380(7) . ? C5 C6 1.401(7) . ? C5 H5 0.9300 . ? C6 C7 1.451(7) . ? C7 N1 1.272(6) . ? C7 H7 0.9300 . ? C8 N1 1.483(6) . ? C8 C9 1.498(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.511(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.488(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.485(7) . ? C11 C12 1.486(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N3 1.493(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N3 1.476(7) . ? C13 C14 1.520(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.511(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N4 1.474(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N4 1.274(6) . ? C16 C17 1.453(7) . ? C16 H16 0.9300 . ? C17 C18 1.409(7) . ? C17 C22 1.416(7) . ? C18 C19 1.364(7) . ? C18 H18 0.9300 . ? C19 C20 1.383(7) . ? C20 C21 1.362(7) . ? C20 H20 0.9300 . ? C21 C22 1.417(7) . ? C21 H21 0.9300 . ? C22 O2 1.310(6) . ? C23 N5 1.154(8) . ? C23 C24 1.421(8) . ? C24 C25 1.357(7) . ? C24 S2 1.744(6) . ? C25 C26 1.436(8) . ? C25 S1 1.730(6) . ? C26 N6 1.135(8) . ? Mn1 O2 1.876(3) . ? Mn1 O1 1.883(3) . ? Mn1 N4 2.011(4) . ? Mn1 N1 2.015(4) . ? Mn1 N2 2.069(4) . ? Mn1 N3 2.088(4) . ? N2 H28 0.9100 . ? N3 H27 0.9100 . ? Pt1 S1 2.2903(14) . ? Pt1 S1 2.2903(14) 2_676 ? Pt1 S2 2.2992(14) . ? Pt1 S2 2.2992(14) 2_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 119.4(5) . . ? O1 C1 C6 122.6(5) . . ? C2 C1 C6 118.0(5) . . ? C3 C2 C1 120.6(5) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 121.0(5) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.6(5) . . ? C3 C4 Br1 121.0(4) . . ? C5 C4 Br1 119.3(4) . . ? C4 C5 C6 120.6(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 120.0(5) . . ? C5 C6 C7 118.8(5) . . ? C1 C6 C7 120.7(5) . . ? N1 C7 C6 124.7(5) . . ? N1 C7 H7 117.7 . . ? C6 C7 H7 117.7 . . ? N1 C8 C9 111.0(4) . . ? N1 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? N1 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C10 115.4(5) . . ? C8 C9 H9A 108.4 . . ? C10 C9 H9A 108.4 . . ? C8 C9 H9B 108.4 . . ? C10 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? N2 C10 C9 112.7(5) . . ? N2 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? N2 C10 H10B 109.0 . . ? C9 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? N2 C11 C12 109.9(5) . . ? N2 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? N2 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C11 C12 N3 108.3(4) . . ? C11 C12 H12A 110.0 . . ? N3 C12 H12A 110.0 . . ? C11 C12 H12B 110.0 . . ? N3 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? N3 C13 C14 112.8(5) . . ? N3 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? N3 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C13 115.5(5) . . ? C15 C14 H14A 108.4 . . ? C13 C14 H14A 108.4 . . ? C15 C14 H14B 108.4 . . ? C13 C14 H14B 108.4 . . ? H14A C14 H14B 107.5 . . ? N4 C15 C14 109.8(5) . . ? N4 C15 H15A 109.7 . . ? C14 C15 H15A 109.7 . . ? N4 C15 H15B 109.7 . . ? C14 C15 H15B 109.7 . . ? H15A C15 H15B 108.2 . . ? N4 C16 C17 124.4(5) . . ? N4 C16 H16 117.8 . . ? C17 C16 H16 117.8 . . ? C18 C17 C22 120.4(4) . . ? C18 C17 C16 118.4(5) . . ? C22 C17 C16 120.5(4) . . ? C19 C18 C17 119.7(5) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 120.9(5) . . ? C18 C19 Br2 118.4(4) . . ? C20 C19 Br2 120.5(4) . . ? C21 C20 C19 120.3(5) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 121.5(5) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? O2 C22 C17 122.8(4) . . ? O2 C22 C21 120.2(4) . . ? C17 C22 C21 117.0(5) . . ? N5 C23 C24 177.0(7) . . ? C25 C24 C23 120.9(5) . . ? C25 C24 S2 122.9(4) . . ? C23 C24 S2 116.2(4) . . ? C24 C25 C26 120.8(5) . . ? C24 C25 S1 122.7(4) . . ? C26 C25 S1 116.5(4) . . ? N6 C26 C25 178.0(8) . . ? O2 Mn1 O1 179.60(15) . . ? O2 Mn1 N4 88.58(15) . . ? O1 Mn1 N4 91.20(16) . . ? O2 Mn1 N1 90.91(15) . . ? O1 Mn1 N1 88.79(15) . . ? N4 Mn1 N1 97.75(16) . . ? O2 Mn1 N2 88.61(16) . . ? O1 Mn1 N2 91.64(16) . . ? N4 Mn1 N2 172.58(18) . . ? N1 Mn1 N2 89.16(17) . . ? O2 Mn1 N3 91.52(16) . . ? O1 Mn1 N3 88.81(16) . . ? N4 Mn1 N3 88.92(17) . . ? N1 Mn1 N3 172.95(17) . . ? N2 Mn1 N3 84.28(17) . . ? C7 N1 C8 117.5(4) . . ? C7 N1 Mn1 121.9(3) . . ? C8 N1 Mn1 119.7(3) . . ? C11 N2 C10 111.4(4) . . ? C11 N2 Mn1 106.6(3) . . ? C10 N2 Mn1 118.7(3) . . ? C11 N2 H28 106.4 . . ? C10 N2 H28 106.4 . . ? Mn1 N2 H28 106.4 . . ? C13 N3 C12 111.5(4) . . ? C13 N3 Mn1 118.3(4) . . ? C12 N3 Mn1 106.7(3) . . ? C13 N3 H27 106.6 . . ? C12 N3 H27 106.6 . . ? Mn1 N3 H27 106.6 . . ? C16 N4 C15 116.6(4) . . ? C16 N4 Mn1 122.6(3) . . ? C15 N4 Mn1 120.0(3) . . ? C1 O1 Mn1 122.5(3) . . ? C22 O2 Mn1 124.0(3) . . ? S1 Pt1 S1 180.0 . 2_676 ? S1 Pt1 S2 89.75(5) . . ? S1 Pt1 S2 90.25(5) 2_676 . ? S1 Pt1 S2 90.25(5) . 2_676 ? S1 Pt1 S2 89.75(5) 2_676 2_676 ? S2 Pt1 S2 180.000(1) . 2_676 ? C25 S1 Pt1 102.68(19) . . ? C24 S2 Pt1 101.95(19) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.839 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.129 _database_code_depnum_ccdc_archive 'CCDC 976204' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pt-350 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C22 H26 Br2 Mn N4 O2), C8 N4 Pt S4' _chemical_formula_sum 'C52 H52 Br4 Mn2 N12 O4 Pt S4' _chemical_formula_weight 1661.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2884(16) _cell_length_b 10.0517(19) _cell_length_c 18.518(4) _cell_angle_alpha 78.811(3) _cell_angle_beta 79.000(3) _cell_angle_gamma 84.998(3) _cell_volume 1483.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 350(2) _cell_measurement_reflns_used 4196 _cell_measurement_theta_min 2.2785 _cell_measurement_theta_max 25.8425 _exptl_crystal_description plate-like _exptl_crystal_colour black _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 5.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2567 _exptl_absorpt_correction_T_max 0.5500 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 350(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12031 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_unetI/netI 0.0484 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5759 _reflns_number_gt 4808 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0970P)^2^+0.0122P] 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 5759 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.1369 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Br1 Br 0.22872(7) 0.71510(7) 1.06583(3) 0.07487(18) Uani 1 1 d . . . Br2 Br 1.27791(7) 1.26665(6) 0.93884(3) 0.06870(15) Uani 1 1 d . . . C1 C 0.5832(5) 0.7608(4) 0.8339(3) 0.0410(10) Uani 1 1 d . . . C2 C 0.5033(6) 0.6403(5) 0.8647(3) 0.0518(12) Uani 1 1 d . . . H2 H 0.5193 0.5685 0.8387 0.062 Uiso 1 1 calc R . . C3 C 0.3997(5) 0.6272(5) 0.9342(3) 0.0543(13) Uani 1 1 d . . . H3 H 0.3495 0.5459 0.9548 0.065 Uiso 1 1 calc R . . C4 C 0.3714(5) 0.7323(5) 0.9724(3) 0.0487(12) Uani 1 1 d . . . C5 C 0.4402(5) 0.8543(5) 0.9410(3) 0.0436(11) Uani 1 1 d . . . H5 H 0.4153 0.9273 0.9660 0.052 Uiso 1 1 calc R . . C6 C 0.5472(5) 0.8707(4) 0.8721(2) 0.0385(10) Uani 1 1 d . . . C7 C 0.6030(5) 1.0046(4) 0.8376(3) 0.0431(11) Uani 1 1 d . . . H7 H 0.5490 1.0784 0.8572 0.052 Uiso 1 1 calc R . . C8 C 0.7349(6) 1.1688(4) 0.7411(3) 0.0499(12) Uani 1 1 d . . . H8A H 0.8469 1.1957 0.7353 0.060 Uiso 1 1 calc R . . H8B H 0.6624 1.2297 0.7688 0.060 Uiso 1 1 calc R . . C9 C 0.6884(7) 1.1788(5) 0.6641(3) 0.0622(15) Uani 1 1 d . . . H9A H 0.6792 1.2737 0.6408 0.075 Uiso 1 1 calc R . . H9B H 0.5817 1.1413 0.6701 0.075 Uiso 1 1 calc R . . C10 C 0.8160(7) 1.1025(6) 0.6123(3) 0.0626(15) Uani 1 1 d . . . H10A H 0.7912 1.1243 0.5620 0.075 Uiso 1 1 calc R . . H10B H 0.9245 1.1337 0.6104 0.075 Uiso 1 1 calc R . . C11 C 0.9326(6) 0.8839(6) 0.5845(3) 0.0560(13) Uani 1 1 d . . . H11A H 1.0389 0.9239 0.5737 0.067 Uiso 1 1 calc R . . H11B H 0.8913 0.8945 0.5380 0.067 Uiso 1 1 calc R . . C12 C 0.9512(7) 0.7372(6) 0.6168(3) 0.0647(15) Uani 1 1 d . . . H12A H 1.0320 0.6918 0.5832 0.078 Uiso 1 1 calc R . . H12B H 0.8471 0.6949 0.6238 0.078 Uiso 1 1 calc R . . C13 C 1.0008(7) 0.5837(5) 0.7328(3) 0.0624(15) Uani 1 1 d . . . H13A H 1.0701 0.5251 0.7024 0.075 Uiso 1 1 calc R . . H13B H 0.8889 0.5552 0.7412 0.075 Uiso 1 1 calc R . . C14 C 1.0577(6) 0.5665(5) 0.8082(3) 0.0621(15) Uani 1 1 d . . . H14A H 1.0650 0.4705 0.8294 0.074 Uiso 1 1 calc R . . H14B H 1.1672 0.6001 0.7999 0.074 Uiso 1 1 calc R . . C15 C 0.9449(6) 0.6401(5) 0.8644(3) 0.0519(13) Uani 1 1 d . . . H15A H 0.8328 0.6135 0.8697 0.062 Uiso 1 1 calc R . . H15B H 0.9785 0.6147 0.9128 0.062 Uiso 1 1 calc R . . C16 C 1.0260(5) 0.8531(5) 0.8742(2) 0.0421(10) Uani 1 1 d . . . H16 H 1.0486 0.8098 0.9206 0.050 Uiso 1 1 calc R . . C17 C 1.0783(5) 0.9900(4) 0.8467(2) 0.0376(10) Uani 1 1 d . . . C18 C 1.1340(5) 1.0571(5) 0.8958(2) 0.0442(11) Uani 1 1 d . . . H18 H 1.1218 1.0192 0.9464 0.053 Uiso 1 1 calc R . . C19 C 1.2067(5) 1.1785(4) 0.8698(3) 0.0433(10) Uani 1 1 d . . . C20 C 1.2332(5) 1.2325(5) 0.7948(3) 0.0477(11) Uani 1 1 d . . . H20 H 1.2859 1.3136 0.7775 0.057 Uiso 1 1 calc R . . C21 C 1.1819(5) 1.1671(5) 0.7453(3) 0.0448(11) Uani 1 1 d . . . H21 H 1.2009 1.2043 0.6945 0.054 Uiso 1 1 calc R . . C22 C 1.1013(4) 1.0451(4) 0.7700(2) 0.0352(9) Uani 1 1 d . . . C23 C 0.4926(7) 0.5867(6) 0.6511(3) 0.0640(15) Uani 1 1 d . . . C24 C 0.5177(5) 0.7007(5) 0.5920(3) 0.0466(11) Uani 1 1 d . . . C25 C 0.6126(6) 0.6914(5) 0.5251(3) 0.0499(12) Uani 1 1 d . . . C26 C 0.6934(7) 0.5602(6) 0.5121(3) 0.0670(16) Uani 1 1 d . . . Mn1 Mn 0.86957(7) 0.87730(6) 0.74367(3) 0.03443(14) Uani 1 1 d . . . N1 N 0.7209(4) 1.0285(4) 0.7824(2) 0.0392(8) Uani 1 1 d . . . N2 N 0.8181(4) 0.9535(4) 0.6374(2) 0.0455(9) Uani 1 1 d . . . H28 H 0.7157 0.9276 0.6372 0.055 Uiso 1 1 calc R . . N3 N 1.0069(5) 0.7250(4) 0.6916(2) 0.0496(10) Uani 1 1 d . . . H27 H 1.1141 0.7470 0.6816 0.060 Uiso 1 1 calc R . . N4 N 0.9513(4) 0.7875(4) 0.8395(2) 0.0407(9) Uani 1 1 d . . . N5 N 0.4717(9) 0.4985(6) 0.7003(4) 0.102(2) Uani 1 1 d . . . N6 N 0.7566(8) 0.4601(6) 0.5007(4) 0.100(2) Uani 1 1 d . . . O1 O 0.6867(3) 0.7674(3) 0.76897(17) 0.0434(7) Uani 1 1 d . . . O2 O 1.0517(3) 0.9866(3) 0.72155(15) 0.0399(7) Uani 1 1 d . . . Pt1 Pt 0.5000 1.0000 0.5000 0.04131(7) Uani 1 2 d S . . S1 S 0.65285(16) 0.82617(14) 0.45262(7) 0.0542(3) Uani 1 1 d . . . S2 S 0.42136(15) 0.85436(13) 0.61092(7) 0.0507(3) 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 Br1 0.0657(3) 0.0871(4) 0.0589(3) -0.0022(3) 0.0145(3) -0.0147(3) Br2 0.0787(3) 0.0701(3) 0.0718(3) -0.0287(3) -0.0304(3) -0.0098(3) C1 0.0313(17) 0.046(2) 0.048(2) -0.0095(19) -0.0116(16) -0.0009(16) C2 0.049(2) 0.047(2) 0.061(3) -0.015(2) -0.006(2) -0.008(2) C3 0.041(2) 0.047(3) 0.070(3) -0.002(2) -0.004(2) -0.010(2) C4 0.0357(19) 0.061(3) 0.046(3) -0.002(2) -0.0053(18) -0.0050(19) C5 0.041(2) 0.048(2) 0.043(2) -0.0114(19) -0.0086(17) 0.0026(18) C6 0.0320(17) 0.043(2) 0.039(2) -0.0016(18) -0.0094(16) 0.0005(16) C7 0.044(2) 0.037(2) 0.047(2) -0.0110(19) -0.0077(18) 0.0062(18) C8 0.060(3) 0.033(2) 0.051(3) 0.000(2) -0.005(2) -0.001(2) C9 0.069(3) 0.049(3) 0.060(3) 0.006(3) -0.011(3) 0.007(2) C10 0.075(3) 0.067(3) 0.047(3) 0.001(3) -0.022(2) -0.008(3) C11 0.049(2) 0.082(3) 0.041(2) -0.020(2) -0.0079(19) -0.003(2) C12 0.063(3) 0.084(4) 0.053(3) -0.034(3) -0.003(2) -0.006(3) C13 0.065(3) 0.046(3) 0.076(4) -0.018(3) -0.009(3) 0.007(2) C14 0.057(3) 0.042(3) 0.080(4) -0.001(3) -0.011(3) 0.009(2) C15 0.052(2) 0.042(2) 0.058(3) 0.003(2) -0.012(2) -0.004(2) C16 0.0413(19) 0.048(2) 0.034(2) 0.0038(18) -0.0086(16) -0.0063(18) C17 0.0372(18) 0.039(2) 0.036(2) -0.0064(17) -0.0063(16) -0.0012(16) C18 0.042(2) 0.055(3) 0.036(2) -0.008(2) -0.0081(17) -0.0025(19) C19 0.0395(19) 0.047(2) 0.049(2) -0.0198(19) -0.0108(17) -0.0023(18) C20 0.047(2) 0.044(2) 0.054(3) -0.009(2) -0.007(2) -0.0107(19) C21 0.044(2) 0.047(2) 0.040(2) -0.0020(19) -0.0027(18) -0.0078(19) C22 0.0294(17) 0.043(2) 0.033(2) -0.0061(17) -0.0071(15) 0.0028(16) C23 0.063(3) 0.058(3) 0.068(3) -0.016(3) 0.006(3) -0.013(2) C24 0.043(2) 0.051(3) 0.044(2) -0.001(2) -0.0088(18) -0.0041(19) C25 0.047(2) 0.054(3) 0.049(3) -0.011(2) -0.009(2) -0.003(2) C26 0.073(3) 0.058(3) 0.067(4) -0.014(3) -0.001(3) -0.007(3) Mn1 0.0341(3) 0.0367(3) 0.0330(3) -0.0074(2) -0.0068(2) -0.0003(2) N1 0.0400(16) 0.0372(18) 0.0394(19) -0.0040(15) -0.0092(14) 0.0019(14) N2 0.0418(17) 0.055(2) 0.0402(19) -0.0071(17) -0.0097(15) -0.0037(16) N3 0.0398(18) 0.055(2) 0.055(2) -0.0173(18) -0.0051(16) 0.0000(16) N4 0.0449(17) 0.0357(18) 0.0391(19) 0.0010(15) -0.0088(15) -0.0033(15) N5 0.140(5) 0.058(3) 0.084(4) 0.003(3) 0.030(4) -0.021(3) N6 0.110(4) 0.066(3) 0.120(5) -0.037(3) 0.004(4) 0.017(3) O1 0.0388(14) 0.0489(17) 0.0453(16) -0.0146(13) -0.0064(12) -0.0058(12) O2 0.0422(14) 0.0470(16) 0.0302(14) -0.0060(12) -0.0053(11) -0.0055(12) Pt1 0.04129(12) 0.04891(14) 0.03419(12) -0.00655(10) -0.00936(9) -0.00114(10) S1 0.0638(7) 0.0580(7) 0.0375(6) -0.0100(5) -0.0033(5) 0.0052(6) S2 0.0517(6) 0.0528(7) 0.0418(6) -0.0041(5) 0.0001(5) 0.0000(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 Br1 C4 1.888(5) . ? Br2 C19 1.894(5) . ? C1 O1 1.331(5) . ? C1 C2 1.400(6) . ? C1 C6 1.405(6) . ? C2 C3 1.394(7) . ? C2 H2 0.9300 . ? C3 C4 1.361(7) . ? C3 H3 0.9300 . ? C4 C5 1.374(7) . ? C5 C6 1.398(6) . ? C5 H5 0.9300 . ? C6 C7 1.448(6) . ? C7 N1 1.274(5) . ? C7 H7 0.9300 . ? C8 N1 1.471(5) . ? C8 C9 1.529(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.544(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.480(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.465(6) . ? C11 C12 1.486(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N3 1.523(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N3 1.476(7) . ? C13 C14 1.531(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.520(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N4 1.466(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N4 1.273(6) . ? C16 C17 1.445(6) . ? C16 H16 0.9300 . ? C17 C18 1.395(6) . ? C17 C22 1.405(6) . ? C18 C19 1.369(6) . ? C18 H18 0.9300 . ? C19 C20 1.371(7) . ? C20 C21 1.374(7) . ? C20 H20 0.9300 . ? C21 C22 1.403(6) . ? C21 H21 0.9300 . ? C22 O2 1.305(5) . ? C23 N5 1.139(8) . ? C23 C24 1.422(7) . ? C24 C25 1.350(6) . ? C24 S2 1.742(5) . ? C25 C26 1.467(7) . ? C25 S1 1.718(5) . ? C26 N6 1.131(8) . ? Mn1 O2 1.880(3) . ? Mn1 O1 1.886(3) . ? Mn1 N1 2.025(3) . ? Mn1 N4 2.038(4) . ? Mn1 N2 2.078(4) . ? Mn1 N3 2.102(4) . ? N2 H28 0.9100 . ? N3 H27 0.9100 . ? Pt1 S1 2.2831(13) 2_676 ? Pt1 S1 2.2831(13) . ? Pt1 S2 2.2968(12) 2_676 ? Pt1 S2 2.2968(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 O1 C1 C2 118.7(4) . . ? O1 C1 C6 122.9(4) . . ? C2 C1 C6 118.4(4) . . ? C3 C2 C1 120.4(5) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C4 C3 C2 120.7(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 Br1 120.6(4) . . ? C5 C4 Br1 119.5(4) . . ? C4 C5 C6 121.1(4) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 119.3(4) . . ? C5 C6 C7 119.0(4) . . ? C1 C6 C7 121.3(4) . . ? N1 C7 C6 124.5(4) . . ? N1 C7 H7 117.7 . . ? C6 C7 H7 117.7 . . ? N1 C8 C9 109.8(4) . . ? N1 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? N1 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C8 C9 C10 112.2(4) . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? N2 C10 C9 112.7(4) . . ? N2 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? N2 C10 H10B 109.0 . . ? C9 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? N2 C11 C12 109.9(4) . . ? N2 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 . . ? N2 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C11 C12 N3 108.1(4) . . ? C11 C12 H12A 110.1 . . ? N3 C12 H12A 110.1 . . ? C11 C12 H12B 110.1 . . ? N3 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? N3 C13 C14 112.8(5) . . ? N3 C13 H13A 109.0 . . ? C14 C13 H13A 109.0 . . ? N3 C13 H13B 109.0 . . ? C14 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C13 113.7(4) . . ? C15 C14 H14A 108.8 . . ? C13 C14 H14A 108.8 . . ? C15 C14 H14B 108.8 . . ? C13 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? N4 C15 C14 110.3(4) . . ? N4 C15 H15A 109.6 . . ? C14 C15 H15A 109.6 . . ? N4 C15 H15B 109.6 . . ? C14 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? N4 C16 C17 124.8(4) . . ? N4 C16 H16 117.6 . . ? C17 C16 H16 117.6 . . ? C18 C17 C22 119.9(4) . . ? C18 C17 C16 118.2(4) . . ? C22 C17 C16 120.8(4) . . ? C19 C18 C17 120.2(4) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.6(4) . . ? C18 C19 Br2 118.6(3) . . ? C20 C19 Br2 120.7(3) . . ? C19 C20 C21 120.1(4) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 121.0(4) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? O2 C22 C21 119.5(4) . . ? O2 C22 C17 122.5(4) . . ? C21 C22 C17 118.0(4) . . ? N5 C23 C24 177.5(7) . . ? C25 C24 C23 122.1(5) . . ? C25 C24 S2 121.5(4) . . ? C23 C24 S2 116.3(4) . . ? C24 C25 C26 119.6(5) . . ? C24 C25 S1 124.3(4) . . ? C26 C25 S1 116.0(4) . . ? N6 C26 C25 178.8(7) . . ? O2 Mn1 O1 178.26(13) . . ? O2 Mn1 N1 91.00(14) . . ? O1 Mn1 N1 88.35(13) . . ? O2 Mn1 N4 87.63(13) . . ? O1 Mn1 N4 90.88(14) . . ? N1 Mn1 N4 99.40(15) . . ? O2 Mn1 N2 89.28(14) . . ? O1 Mn1 N2 92.32(14) . . ? N1 Mn1 N2 89.07(15) . . ? N4 Mn1 N2 171.02(15) . . ? O2 Mn1 N3 91.62(14) . . ? O1 Mn1 N3 89.22(14) . . ? N1 Mn1 N3 172.46(16) . . ? N4 Mn1 N3 87.77(16) . . ? N2 Mn1 N3 83.90(16) . . ? C7 N1 C8 117.9(4) . . ? C7 N1 Mn1 121.9(3) . . ? C8 N1 Mn1 119.8(3) . . ? C11 N2 C10 111.3(4) . . ? C11 N2 Mn1 107.6(3) . . ? C10 N2 Mn1 117.4(3) . . ? C11 N2 H28 106.6 . . ? C10 N2 H28 106.6 . . ? Mn1 N2 H28 106.6 . . ? C13 N3 C12 111.0(4) . . ? C13 N3 Mn1 118.1(3) . . ? C12 N3 Mn1 105.8(3) . . ? C13 N3 H27 107.2 . . ? C12 N3 H27 107.2 . . ? Mn1 N3 H27 107.2 . . ? C16 N4 C15 118.0(4) . . ? C16 N4 Mn1 121.7(3) . . ? C15 N4 Mn1 119.8(3) . . ? C1 O1 Mn1 122.3(3) . . ? C22 O2 Mn1 124.4(2) . . ? S1 Pt1 S1 180.000(1) 2_676 . ? S1 Pt1 S2 89.71(4) 2_676 2_676 ? S1 Pt1 S2 90.29(5) . 2_676 ? S1 Pt1 S2 90.29(5) 2_676 . ? S1 Pt1 S2 89.71(4) . . ? S2 Pt1 S2 180.0 2_676 . ? C25 S1 Pt1 102.13(17) . . ? C24 S2 Pt1 102.23(16) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.972 _refine_diff_density_min -1.527 _refine_diff_density_rms 0.255 _database_code_depnum_ccdc_archive 'CCDC 976205' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pt400 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C22 H26 Br2 Mn N4 O2), C8 N4 Pt S4' _chemical_formula_sum 'C52 H52 Br4 Mn2 N12 O4 Pt S4' _chemical_formula_weight 1661.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3184(11) _cell_length_b 10.0509(13) _cell_length_c 18.595(2) _cell_angle_alpha 78.835(2) _cell_angle_beta 78.768(2) _cell_angle_gamma 85.630(2) _cell_volume 1494.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 400(2) _cell_measurement_reflns_used 3333 _cell_measurement_theta_min 2.4985 _cell_measurement_theta_max 23.666 _exptl_crystal_description plate-like _exptl_crystal_colour black _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 5.617 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2586 _exptl_absorpt_correction_T_max 0.5521 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 400(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12122 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_unetI/netI 0.0569 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5813 _reflns_number_gt 4449 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1009P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5813 _refine_ls_number_parameters 358 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1647 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.22910(9) 0.71838(8) 1.06611(4) 0.0894(2) Uani 1 1 d . . . Br2 Br 1.27603(9) 1.26728(7) 0.93933(4) 0.08414(19) Uani 1 1 d . . . C1 C 0.5816(6) 0.7608(5) 0.8351(3) 0.0498(12) Uani 1 1 d . . . C2 C 0.5033(7) 0.6408(5) 0.8670(3) 0.0624(15) Uani 1 1 d . . . H2 H 0.5207 0.5673 0.8424 0.075 Uiso 1 1 calc R . . C3 C 0.3998(7) 0.6306(6) 0.9351(4) 0.0667(17) Uani 1 1 d . . . H3 H 0.3492 0.5492 0.9560 0.080 Uiso 1 1 calc R . . C4 C 0.3694(6) 0.7352(5) 0.9726(3) 0.0568(14) Uani 1 1 d . . . C5 C 0.4408(6) 0.8581(5) 0.9403(3) 0.0513(13) Uani 1 1 d . . . H5 H 0.4174 0.9310 0.9653 0.062 Uiso 1 1 calc R . . C6 C 0.5463(5) 0.8751(5) 0.8716(3) 0.0466(12) Uani 1 1 d . . . C7 C 0.5978(6) 1.0055(4) 0.8366(3) 0.0477(12) Uani 1 1 d . . . H7 H 0.5412 1.0788 0.8552 0.057 Uiso 1 1 calc R . . C8 C 0.7331(7) 1.1710(5) 0.7391(3) 0.0600(15) Uani 1 1 d . . . H8A H 0.8444 1.1987 0.7345 0.072 Uiso 1 1 calc R . . H8B H 0.6594 1.2323 0.7656 0.072 Uiso 1 1 calc R . . C9 C 0.6931(8) 1.1792(6) 0.6622(4) 0.0710(18) Uani 1 1 d . . . H9A H 0.6879 1.2738 0.6385 0.085 Uiso 1 1 calc R . . H9B H 0.5853 1.1436 0.6677 0.085 Uiso 1 1 calc R . . C10 C 0.8152(7) 1.1024(6) 0.6113(3) 0.0662(16) Uani 1 1 d . . . H10A H 0.7889 1.1231 0.5617 0.079 Uiso 1 1 calc R . . H10B H 0.9242 1.1339 0.6081 0.079 Uiso 1 1 calc R . . C11 C 0.9360(7) 0.8849(6) 0.5841(3) 0.0678(16) Uani 1 1 d . . . H11A H 1.0428 0.9237 0.5754 0.081 Uiso 1 1 calc R . . H11B H 0.8997 0.8957 0.5367 0.081 Uiso 1 1 calc R . . C12 C 0.9467(8) 0.7340(6) 0.6192(3) 0.0720(17) Uani 1 1 d . . . H12A H 0.8399 0.6952 0.6276 0.086 Uiso 1 1 calc R . . H12B H 1.0230 0.6853 0.5860 0.086 Uiso 1 1 calc R . . C13 C 1.0036(8) 0.5839(6) 0.7323(4) 0.0744(19) Uani 1 1 d . . . H13A H 1.0748 0.5269 0.7020 0.089 Uiso 1 1 calc R . . H13B H 0.8934 0.5511 0.7413 0.089 Uiso 1 1 calc R . . C14 C 1.0593(8) 0.5697(6) 0.8060(4) 0.0756(19) Uani 1 1 d . . . H14A H 1.1680 0.6053 0.7967 0.091 Uiso 1 1 calc R . . H14B H 1.0686 0.4738 0.8269 0.091 Uiso 1 1 calc R . . C15 C 0.9495(7) 0.6401(5) 0.8640(3) 0.0634(16) Uani 1 1 d . . . H15A H 0.8378 0.6113 0.8713 0.076 Uiso 1 1 calc R . . H15B H 0.9870 0.6156 0.9112 0.076 Uiso 1 1 calc R . . C16 C 1.0298(6) 0.8505(5) 0.8744(3) 0.0519(12) Uani 1 1 d U . . H16 H 1.0539 0.8065 0.9200 0.062 Uiso 1 1 calc R . . C17 C 1.0797(5) 0.9895(5) 0.8467(3) 0.0448(10) Uani 1 1 d U . . C18 C 1.1325(6) 1.0555(5) 0.8963(3) 0.0518(11) Uani 1 1 d U . . H18 H 1.1177 1.0176 0.9467 0.062 Uiso 1 1 calc R . . C19 C 1.2079(6) 1.1791(5) 0.8698(3) 0.0499(11) Uani 1 1 d U . . C20 C 1.2314(6) 1.2302(5) 0.7973(3) 0.0544(12) Uani 1 1 d U . . H20 H 1.2837 1.3120 0.7806 0.065 Uiso 1 1 calc R . . C21 C 1.1832(6) 1.1693(5) 0.7462(3) 0.0524(13) Uani 1 1 d . . . H21 H 1.2038 1.2082 0.6959 0.063 Uiso 1 1 calc R . . C22 C 1.0999(5) 1.0440(5) 0.7713(3) 0.0441(12) Uani 1 1 d . . . C23 C 0.4958(8) 0.5896(7) 0.6506(4) 0.080(2) Uani 1 1 d . . . C24 C 0.5178(6) 0.7011(5) 0.5913(3) 0.0578(14) Uani 1 1 d . . . C25 C 0.6124(7) 0.6881(6) 0.5246(3) 0.0620(14) Uani 1 1 d U . . C26 C 0.6889(8) 0.5660(6) 0.5110(4) 0.0720(17) Uani 1 1 d U . . Mn1 Mn 0.86968(8) 0.87747(7) 0.74395(4) 0.04165(17) Uani 1 1 d . . . N1 N 0.7164(5) 1.0319(4) 0.7814(2) 0.0491(10) Uani 1 1 d . . . N2 N 0.8163(5) 0.9547(5) 0.6369(2) 0.0592(12) Uani 1 1 d . . . H28 H 0.7148 0.9271 0.6365 0.071 Uiso 1 1 calc R . . N3 N 1.0038(5) 0.7220(4) 0.6910(3) 0.0600(12) Uani 1 1 d . . . H27 H 1.1104 0.7459 0.6793 0.072 Uiso 1 1 calc R . . N4 N 0.9539(5) 0.7853(4) 0.8389(2) 0.0491(10) Uani 1 1 d . . . N5 N 0.4701(10) 0.4976(6) 0.6989(4) 0.121(3) Uani 1 1 d . . . N6 N 0.7582(9) 0.4677(6) 0.4988(4) 0.110(2) Uani 1 1 d U . . O1 O 0.6869(4) 0.7683(3) 0.7703(2) 0.0537(9) Uani 1 1 d . . . O2 O 1.0514(4) 0.9887(3) 0.72149(17) 0.0475(8) Uani 1 1 d . . . Pt1 Pt 0.5000 1.0000 0.5000 0.04956(8) Uani 1 2 d S . . S1 S 0.6521(2) 0.82739(15) 0.45220(8) 0.0645(4) Uani 1 1 d . . . S2 S 0.42139(18) 0.85284(14) 0.61046(8) 0.0610(4) 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 Br1 0.0781(4) 0.1026(5) 0.0717(4) -0.0060(4) 0.0185(4) -0.0139(4) Br2 0.0962(4) 0.0852(4) 0.0886(4) -0.0386(3) -0.0348(3) -0.0094(3) C1 0.046(2) 0.053(2) 0.053(3) -0.017(2) -0.012(2) 0.000(2) C2 0.057(3) 0.052(3) 0.079(4) -0.020(3) -0.003(3) -0.010(2) C3 0.055(3) 0.059(3) 0.080(4) -0.003(3) -0.003(3) -0.016(2) C4 0.043(2) 0.060(3) 0.063(3) -0.005(2) -0.004(2) -0.006(2) C5 0.042(2) 0.054(3) 0.056(3) -0.012(2) -0.007(2) 0.006(2) C6 0.040(2) 0.053(2) 0.046(2) -0.010(2) -0.008(2) 0.004(2) C7 0.050(2) 0.039(2) 0.053(3) -0.014(2) -0.006(2) 0.007(2) C8 0.068(3) 0.041(2) 0.067(3) -0.004(2) -0.009(3) -0.001(2) C9 0.072(3) 0.055(3) 0.077(4) 0.004(3) -0.013(3) 0.007(3) C10 0.072(3) 0.070(3) 0.051(3) 0.006(3) -0.013(3) -0.003(3) C11 0.066(3) 0.096(4) 0.047(3) -0.026(3) -0.014(2) 0.007(3) C12 0.072(3) 0.088(4) 0.064(3) -0.046(3) -0.001(3) -0.004(3) C13 0.071(3) 0.062(3) 0.087(4) -0.029(3) 0.002(3) 0.017(3) C14 0.080(4) 0.051(3) 0.093(5) -0.005(3) -0.021(3) 0.009(3) C15 0.065(3) 0.045(3) 0.078(4) -0.001(3) -0.021(3) 0.003(2) C16 0.051(2) 0.056(2) 0.046(2) -0.0043(19) -0.0091(19) -0.001(2) C17 0.0450(18) 0.0470(19) 0.0427(19) -0.0047(17) -0.0098(17) -0.0077(17) C18 0.051(2) 0.058(2) 0.047(2) -0.0077(19) -0.0135(18) 0.0021(19) C19 0.0483(19) 0.049(2) 0.053(2) -0.0115(18) -0.0062(18) -0.0060(18) C20 0.052(2) 0.049(2) 0.062(2) -0.011(2) -0.005(2) -0.0104(19) C21 0.056(3) 0.054(3) 0.043(3) -0.003(2) 0.000(2) -0.013(2) C22 0.043(2) 0.045(2) 0.043(2) -0.0100(19) -0.005(2) 0.0046(19) C23 0.074(4) 0.077(4) 0.088(5) -0.029(3) -0.005(4) 0.006(3) C24 0.056(3) 0.059(3) 0.055(3) -0.008(2) -0.001(2) -0.010(2) C25 0.061(3) 0.061(3) 0.064(3) -0.015(2) -0.009(2) -0.001(2) C26 0.073(3) 0.056(3) 0.081(4) -0.017(3) 0.001(3) 0.000(3) Mn1 0.0414(3) 0.0431(3) 0.0407(4) -0.0115(3) -0.0056(3) 0.0015(3) N1 0.049(2) 0.048(2) 0.049(2) -0.0095(18) -0.0078(18) 0.0050(17) N2 0.057(2) 0.073(3) 0.052(2) -0.016(2) -0.018(2) 0.000(2) N3 0.048(2) 0.065(2) 0.067(3) -0.021(2) 0.002(2) -0.008(2) N4 0.056(2) 0.0409(18) 0.048(2) -0.0023(17) -0.0088(19) -0.0074(17) N5 0.156(6) 0.061(3) 0.109(5) 0.020(3) 0.028(5) -0.017(4) N6 0.111(4) 0.081(3) 0.125(5) -0.020(4) 0.016(4) -0.008(3) O1 0.0472(16) 0.0584(18) 0.058(2) -0.0223(16) -0.0057(16) -0.0008(15) O2 0.0508(16) 0.0542(17) 0.0373(16) -0.0069(14) -0.0056(14) -0.0114(14) Pt1 0.04898(13) 0.05745(15) 0.04254(14) -0.00960(11) -0.00905(11) -0.00108(12) S1 0.0760(8) 0.0685(8) 0.0451(7) -0.0125(6) -0.0031(7) 0.0061(7) S2 0.0604(7) 0.0643(7) 0.0519(7) -0.0078(6) 0.0010(6) 0.0018(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C4 1.881(5) . ? Br2 C19 1.892(5) . ? C1 O1 1.337(6) . ? C1 C2 1.387(7) . ? C1 C6 1.428(7) . ? C2 C3 1.376(8) . ? C2 H2 0.9300 . ? C3 C4 1.353(9) . ? C3 H3 0.9300 . ? C4 C5 1.388(7) . ? C5 C6 1.391(7) . ? C5 H5 0.9300 . ? C6 C7 1.404(6) . ? C7 N1 1.280(6) . ? C7 H7 0.9300 . ? C8 N1 1.467(6) . ? C8 C9 1.516(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.520(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.468(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.493(7) . ? C11 C12 1.533(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N3 1.483(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N3 1.450(7) . ? C13 C14 1.508(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.520(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N4 1.444(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N4 1.286(7) . ? C16 C17 1.454(6) . ? C16 H16 0.9300 . ? C17 C22 1.385(6) . ? C17 C18 1.386(7) . ? C18 C19 1.394(7) . ? C18 H18 0.9300 . ? C19 C20 1.329(7) . ? C20 C21 1.359(8) . ? C20 H20 0.9300 . ? C21 C22 1.437(6) . ? C21 H21 0.9300 . ? C22 O2 1.308(6) . ? C23 N5 1.158(9) . ? C23 C24 1.407(8) . ? C24 C25 1.356(8) . ? C24 S2 1.735(6) . ? C25 C26 1.383(8) . ? C25 S1 1.746(6) . ? C26 N6 1.144(9) . ? Mn1 O1 1.874(3) . ? Mn1 O2 1.882(3) . ? Mn1 N4 2.054(4) . ? Mn1 N1 2.071(4) . ? Mn1 N2 2.111(4) . ? Mn1 N3 2.135(5) . ? N2 H28 0.9100 . ? N3 H27 0.9100 . ? Pt1 S1 2.2859(16) 2_676 ? Pt1 S1 2.2859(16) . ? Pt1 S2 2.2982(14) . ? Pt1 S2 2.2982(14) 2_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 119.6(5) . . ? O1 C1 C6 121.1(4) . . ? C2 C1 C6 119.2(5) . . ? C3 C2 C1 119.9(5) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 122.2(5) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C3 C4 C5 118.9(5) . . ? C3 C4 Br1 121.4(4) . . ? C5 C4 Br1 119.6(4) . . ? C4 C5 C6 121.7(5) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C7 119.4(5) . . ? C5 C6 C1 117.9(4) . . ? C7 C6 C1 122.2(4) . . ? N1 C7 C6 125.3(4) . . ? N1 C7 H7 117.3 . . ? C6 C7 H7 117.3 . . ? N1 C8 C9 110.2(5) . . ? N1 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? N1 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 114.5(5) . . ? C8 C9 H9A 108.6 . . ? C10 C9 H9A 108.6 . . ? C8 C9 H9B 108.6 . . ? C10 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? N2 C10 C9 113.3(4) . . ? N2 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? N2 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? N2 C11 C12 107.9(4) . . ? N2 C11 H11A 110.1 . . ? C12 C11 H11A 110.1 . . ? N2 C11 H11B 110.1 . . ? C12 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? N3 C12 C11 108.4(5) . . ? N3 C12 H12A 110.0 . . ? C11 C12 H12A 110.0 . . ? N3 C12 H12B 110.0 . . ? C11 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? N3 C13 C14 113.7(5) . . ? N3 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? N3 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C13 C14 C15 115.8(5) . . ? C13 C14 H14A 108.3 . . ? C15 C14 H14A 108.3 . . ? C13 C14 H14B 108.3 . . ? C15 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? N4 C15 C14 109.4(4) . . ? N4 C15 H15A 109.8 . . ? C14 C15 H15A 109.8 . . ? N4 C15 H15B 109.8 . . ? C14 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? N4 C16 C17 123.4(5) . . ? N4 C16 H16 118.3 . . ? C17 C16 H16 118.3 . . ? C22 C17 C18 121.4(4) . . ? C22 C17 C16 120.6(5) . . ? C18 C17 C16 117.0(4) . . ? C17 C18 C19 119.4(5) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 119.4(5) . . ? C20 C19 Br2 122.3(4) . . ? C18 C19 Br2 118.2(4) . . ? C19 C20 C21 123.6(5) . . ? C19 C20 H20 118.2 . . ? C21 C20 H20 118.2 . . ? C20 C21 C22 118.9(5) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.6 . . ? O2 C22 C17 124.9(4) . . ? O2 C22 C21 117.9(4) . . ? C17 C22 C21 117.2(5) . . ? N5 C23 C24 176.7(8) . . ? C25 C24 C23 120.8(5) . . ? C25 C24 S2 123.5(4) . . ? C23 C24 S2 115.7(5) . . ? C24 C25 C26 122.4(5) . . ? C24 C25 S1 121.5(4) . . ? C26 C25 S1 116.0(5) . . ? N6 C26 C25 177.2(7) . . ? O1 Mn1 O2 177.64(16) . . ? O1 Mn1 N4 90.81(16) . . ? O2 Mn1 N4 87.64(15) . . ? O1 Mn1 N1 87.41(15) . . ? O2 Mn1 N1 91.16(15) . . ? N4 Mn1 N1 101.76(17) . . ? O1 Mn1 N2 92.32(17) . . ? O2 Mn1 N2 89.48(16) . . ? N4 Mn1 N2 170.46(17) . . ? N1 Mn1 N2 87.38(17) . . ? O1 Mn1 N3 88.82(16) . . ? O2 Mn1 N3 92.88(16) . . ? N4 Mn1 N3 87.13(18) . . ? N1 Mn1 N3 170.38(18) . . ? N2 Mn1 N3 83.93(18) . . ? C7 N1 C8 119.5(4) . . ? C7 N1 Mn1 120.7(3) . . ? C8 N1 Mn1 119.4(3) . . ? C10 N2 C11 110.9(4) . . ? C10 N2 Mn1 117.9(4) . . ? C11 N2 Mn1 106.0(3) . . ? C10 N2 H28 107.2 . . ? C11 N2 H28 107.2 . . ? Mn1 N2 H28 107.2 . . ? C13 N3 C12 112.9(5) . . ? C13 N3 Mn1 118.8(4) . . ? C12 N3 Mn1 105.5(3) . . ? C13 N3 H27 106.3 . . ? C12 N3 H27 106.3 . . ? Mn1 N3 H27 106.3 . . ? C16 N4 C15 116.2(4) . . ? C16 N4 Mn1 122.0(3) . . ? C15 N4 Mn1 121.3(4) . . ? C1 O1 Mn1 123.5(3) . . ? C22 O2 Mn1 122.9(3) . . ? S1 Pt1 S1 180.00(7) 2_676 . ? S1 Pt1 S2 90.45(5) 2_676 . ? S1 Pt1 S2 89.55(5) . . ? S1 Pt1 S2 89.55(5) 2_676 2_676 ? S1 Pt1 S2 90.45(5) . 2_676 ? S2 Pt1 S2 180.000(1) . 2_676 ? C25 S1 Pt1 103.0(2) . . ? C24 S2 Pt1 102.25(18) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.225 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.283 _database_code_depnum_ccdc_archive 'CCDC 976206' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pt-473 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C22 H26 Br2 Mn N4 O2), C8 N4 Pt S4' _chemical_formula_sum 'C52 H52 Br4 Mn2 N12 O4 Pt S4' _chemical_formula_weight 1661.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.356(2) _cell_length_b 10.057(3) _cell_length_c 18.676(5) _cell_angle_alpha 78.942(4) _cell_angle_beta 78.639(4) _cell_angle_gamma 86.212(4) _cell_volume 1509.7(6) _cell_formula_units_Z 1 _cell_measurement_temperature 473(2) _cell_measurement_reflns_used 1954 _cell_measurement_theta_min 2.487 _cell_measurement_theta_max 21.0425 _exptl_crystal_description plate-like _exptl_crystal_colour black _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 5.562 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2612 _exptl_absorpt_correction_T_max 0.5550 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 473(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11120 _diffrn_reflns_av_R_equivalents 0.0584 _diffrn_reflns_av_unetI/netI 0.0934 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5249 _reflns_number_gt 3264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0630P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5249 _refine_ls_number_parameters 352 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1255 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.006 _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 Br1 Br 0.22973(9) 0.72067(8) 1.06577(4) 0.1100(3) Uani 1 1 d . . . Br2 Br 1.27506(9) 1.26820(7) 0.93930(4) 0.1057(2) Uani 1 1 d . . . C1 C 0.5810(5) 0.7640(5) 0.8362(3) 0.0589(14) Uani 1 1 d U . . C2 C 0.5043(7) 0.6410(5) 0.8679(3) 0.0782(19) Uani 1 1 d . . . H2 H 0.5240 0.5673 0.8436 0.094 Uiso 1 1 calc R . . C3 C 0.3985(6) 0.6309(5) 0.9361(3) 0.0771(19) Uani 1 1 d . . . H3 H 0.3449 0.5505 0.9570 0.092 Uiso 1 1 calc R . . C4 C 0.3728(6) 0.7375(5) 0.9722(3) 0.0730(18) Uani 1 1 d . . . C5 C 0.4410(6) 0.8581(5) 0.9398(3) 0.0625(16) Uani 1 1 d . . . H5 H 0.4165 0.9318 0.9640 0.075 Uiso 1 1 calc R . . C6 C 0.5460(5) 0.8744(5) 0.8721(3) 0.0554(14) Uani 1 1 d U . . C7 C 0.5994(6) 1.0093(5) 0.8351(3) 0.0672(17) Uani 1 1 d U . . H7 H 0.5444 1.0832 0.8529 0.081 Uiso 1 1 calc R . . C8 C 0.7292(7) 1.1724(5) 0.7378(3) 0.0774(19) Uani 1 1 d U . . H8A H 0.8378 1.2048 0.7344 0.093 Uiso 1 1 calc R . . H8B H 0.6509 1.2311 0.7634 0.093 Uiso 1 1 calc R . . C9 C 0.6961(8) 1.1769(6) 0.6610(3) 0.086(2) Uani 1 1 d U . . H9A H 0.6913 1.2710 0.6367 0.103 Uiso 1 1 calc R . . H9B H 0.5892 1.1403 0.6657 0.103 Uiso 1 1 calc R . . C10 C 0.8182(8) 1.1012(6) 0.6108(3) 0.087(2) Uani 1 1 d U . . H10A H 0.7940 1.1213 0.5611 0.104 Uiso 1 1 calc R . . H10B H 0.9269 1.1326 0.6082 0.104 Uiso 1 1 calc R . . C11 C 0.9321(7) 0.8842(6) 0.5837(3) 0.086(2) Uani 1 1 d . . . H11A H 1.0376 0.9261 0.5722 0.103 Uiso 1 1 calc R . . H11B H 0.8912 0.8920 0.5378 0.103 Uiso 1 1 calc R . . C12 C 0.9496(8) 0.7364(6) 0.6181(3) 0.095(2) Uani 1 1 d . . . H12A H 0.8455 0.6933 0.6262 0.114 Uiso 1 1 calc R . . H12B H 1.0281 0.6909 0.5846 0.114 Uiso 1 1 calc R . . C13 C 0.9993(8) 0.5834(6) 0.7318(4) 0.094(2) Uani 1 1 d . . . H13A H 1.0675 0.5251 0.7017 0.113 Uiso 1 1 calc R . . H13B H 0.8882 0.5526 0.7412 0.113 Uiso 1 1 calc R . . C14 C 1.0551(8) 0.5686(6) 0.8044(4) 0.093(2) Uani 1 1 d U . . H14A H 1.1638 0.6044 0.7948 0.112 Uiso 1 1 calc R . . H14B H 1.0639 0.4727 0.8247 0.112 Uiso 1 1 calc R . . C15 C 0.9483(7) 0.6371(5) 0.8628(3) 0.0732(17) Uani 1 1 d U . . H15A H 0.8365 0.6090 0.8704 0.088 Uiso 1 1 calc R . . H15B H 0.9862 0.6117 0.9096 0.088 Uiso 1 1 calc R . . C16 C 1.0310(6) 0.8502(5) 0.8722(3) 0.0632(16) Uani 1 1 d . . . H16 H 1.0554 0.8053 0.9173 0.076 Uiso 1 1 calc R . . C17 C 1.0806(5) 0.9896(4) 0.8463(3) 0.0537(14) Uani 1 1 d . . . C18 C 1.1341(6) 1.0563(5) 0.8952(3) 0.0651(16) Uani 1 1 d . . . H18 H 1.1216 1.0171 0.9452 0.078 Uiso 1 1 calc R . . C19 C 1.2053(6) 1.1792(5) 0.8704(3) 0.0663(16) Uani 1 1 d . . . C20 C 1.2323(6) 1.2323(5) 0.7962(3) 0.0648(16) Uani 1 1 d U . . H20 H 1.2866 1.3134 0.7791 0.078 Uiso 1 1 calc R . . C21 C 1.1818(6) 1.1698(5) 0.7470(3) 0.0664(16) Uani 1 1 d U . . H21 H 1.2004 1.2088 0.6969 0.080 Uiso 1 1 calc R . . C22 C 1.1015(5) 1.0463(5) 0.7711(3) 0.0529(14) Uani 1 1 d . . . C23 C 0.4910(8) 0.5878(6) 0.6494(4) 0.094(2) Uani 1 1 d . . . C24 C 0.5193(6) 0.7019(5) 0.5907(3) 0.0666(16) Uani 1 1 d . . . C25 C 0.6118(6) 0.6917(5) 0.5244(3) 0.0651(16) Uani 1 1 d . . . C26 C 0.6912(8) 0.5656(7) 0.5112(4) 0.095(2) Uani 1 1 d . . . Mn1 Mn 0.87004(8) 0.87827(7) 0.74383(4) 0.0540(2) Uani 1 1 d U . . N1 N 0.7167(5) 1.0320(4) 0.7800(2) 0.0561(12) Uani 1 1 d U . . N2 N 0.8158(5) 0.9541(5) 0.6373(2) 0.0745(14) Uani 1 1 d . . . H28 H 0.7137 0.9272 0.6377 0.089 Uiso 1 1 calc R . . N3 N 1.0045(5) 0.7237(4) 0.6894(3) 0.0740(11) Uani 1 1 d U . . H27 H 1.1111 0.7471 0.6783 0.089 Uiso 1 1 calc R . . N4 N 0.9565(5) 0.7858(4) 0.8373(2) 0.0615(13) Uani 1 1 d . . . N5 N 0.4735(10) 0.5022(6) 0.6983(4) 0.143(3) Uani 1 1 d . . . N6 N 0.7548(9) 0.4701(7) 0.4978(4) 0.144(3) Uani 1 1 d . . . O1 O 0.6851(4) 0.7681(3) 0.7714(2) 0.0681(11) Uani 1 1 d . . . O2 O 1.0505(4) 0.9901(3) 0.72179(18) 0.0627(10) Uani 1 1 d . . . Pt1 Pt 0.5000 1.0000 0.5000 0.06314(9) Uani 1 2 d S . . S1 S 0.65204(16) 0.82870(14) 0.45200(7) 0.06314(9) Uani 1 1 d . . . S2 S 0.42150(18) 0.85244(15) 0.60955(9) 0.0769(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 Br1 0.0961(4) 0.1262(5) 0.0882(5) -0.0060(4) 0.0205(4) -0.0169(4) Br2 0.1200(5) 0.1062(4) 0.1117(5) -0.0467(4) -0.0426(4) -0.0117(4) C1 0.048(2) 0.070(3) 0.061(3) -0.016(2) -0.011(2) -0.007(2) C2 0.074(3) 0.067(3) 0.095(4) -0.024(3) -0.008(3) -0.010(3) C3 0.069(3) 0.062(3) 0.092(4) -0.009(3) 0.003(3) -0.011(3) C4 0.057(3) 0.071(3) 0.084(4) -0.002(3) -0.009(3) -0.010(3) C5 0.059(3) 0.062(3) 0.070(3) -0.021(3) -0.013(3) 0.008(3) C6 0.044(2) 0.055(2) 0.067(3) -0.016(2) -0.005(2) 0.002(2) C7 0.077(3) 0.054(3) 0.069(3) -0.015(3) -0.012(3) 0.013(3) C8 0.081(3) 0.064(3) 0.082(4) -0.013(3) -0.003(3) -0.003(3) C9 0.098(4) 0.071(3) 0.081(4) -0.002(3) -0.015(3) 0.006(3) C10 0.101(4) 0.091(4) 0.061(3) 0.004(3) -0.018(3) 0.003(3) C11 0.080(3) 0.132(5) 0.050(3) -0.035(3) -0.005(3) -0.006(4) C12 0.088(4) 0.114(5) 0.083(4) -0.043(4) 0.002(4) 0.002(4) C13 0.099(4) 0.079(4) 0.109(5) -0.045(4) -0.011(4) 0.020(4) C14 0.090(4) 0.056(3) 0.129(5) -0.008(3) -0.026(4) 0.017(3) C15 0.083(3) 0.055(3) 0.079(4) 0.003(3) -0.027(3) 0.000(3) C16 0.065(3) 0.061(3) 0.059(3) -0.003(3) -0.010(3) 0.001(3) C17 0.051(2) 0.053(3) 0.055(3) -0.003(2) -0.011(2) -0.002(2) C18 0.067(3) 0.079(3) 0.050(3) -0.010(3) -0.015(3) 0.001(3) C19 0.057(3) 0.071(3) 0.078(3) -0.025(3) -0.019(3) -0.002(3) C20 0.055(3) 0.056(3) 0.080(3) -0.004(2) -0.013(3) 0.005(2) C21 0.071(3) 0.060(3) 0.064(3) -0.008(2) -0.003(3) -0.009(3) C22 0.052(2) 0.055(3) 0.049(3) -0.013(2) -0.002(2) 0.000(2) C23 0.102(4) 0.087(4) 0.083(4) -0.022(3) 0.018(4) -0.015(4) C24 0.059(3) 0.078(3) 0.061(3) -0.016(3) -0.005(3) -0.004(3) C25 0.062(3) 0.069(3) 0.066(3) -0.022(3) -0.009(3) 0.001(3) C26 0.106(4) 0.092(4) 0.090(4) -0.036(3) -0.006(4) -0.014(4) Mn1 0.0540(4) 0.0549(4) 0.0526(4) -0.0117(3) -0.0079(3) 0.0006(3) N1 0.055(2) 0.051(2) 0.061(2) -0.0109(19) -0.0086(19) 0.0030(19) N2 0.064(2) 0.096(3) 0.066(3) -0.013(2) -0.019(2) -0.009(2) N3 0.055(2) 0.0819(13) 0.086(3) -0.0338(12) -0.0001(18) 0.0069(15) N4 0.056(2) 0.049(2) 0.075(3) 0.000(2) -0.012(2) -0.0058(19) N5 0.181(6) 0.087(4) 0.126(5) 0.019(4) 0.024(5) -0.016(4) N6 0.162(6) 0.105(4) 0.160(7) -0.042(5) -0.007(5) 0.016(5) O1 0.0682(19) 0.070(2) 0.067(2) -0.0238(17) -0.0026(18) -0.0080(18) O2 0.0699(19) 0.0663(19) 0.0496(19) -0.0132(16) -0.0020(17) -0.0069(17) Pt1 0.06176(15) 0.07303(18) 0.05431(16) -0.01085(14) -0.01100(13) -0.00179(14) S1 0.06176(15) 0.07303(18) 0.05431(16) -0.01085(14) -0.01100(13) -0.00179(14) S2 0.0736(8) 0.0798(9) 0.0677(9) -0.0073(7) 0.0033(8) 0.0002(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C4 1.898(6) . ? Br2 C19 1.899(6) . ? C1 O1 1.340(6) . ? C1 C6 1.390(7) . ? C1 C2 1.402(7) . ? C2 C3 1.390(8) . ? C2 H2 0.9300 . ? C3 C4 1.357(8) . ? C3 H3 0.9300 . ? C4 C5 1.355(7) . ? C5 C6 1.379(7) . ? C5 H5 0.9300 . ? C6 C7 1.454(6) . ? C7 N1 1.271(6) . ? C7 H7 0.9300 . ? C8 N1 1.478(6) . ? C8 C9 1.505(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.513(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.467(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.497(7) . ? C11 C12 1.512(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N3 1.471(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N3 1.478(7) . ? C13 C14 1.496(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.512(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N4 1.482(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N4 1.268(7) . ? C16 C17 1.451(6) . ? C16 H16 0.9300 . ? C17 C18 1.385(7) . ? C17 C22 1.392(6) . ? C18 C19 1.366(7) . ? C18 H18 0.9300 . ? C19 C20 1.365(7) . ? C20 C21 1.351(8) . ? C20 H20 0.9300 . ? C21 C22 1.404(6) . ? C21 H21 0.9300 . ? C22 O2 1.318(6) . ? C23 N5 1.122(8) . ? C23 C24 1.422(8) . ? C24 C25 1.343(7) . ? C24 S2 1.735(6) . ? C25 C26 1.433(8) . ? C25 S1 1.735(5) . ? C26 N6 1.114(9) . ? Mn1 O2 1.874(3) . ? Mn1 O1 1.891(3) . ? Mn1 N4 2.054(4) . ? Mn1 N1 2.071(4) . ? Mn1 N2 2.115(4) . ? Mn1 N3 2.154(5) . ? N2 H28 0.9100 . ? N3 H27 0.9100 . ? Pt1 S1 2.2892(15) 2_676 ? Pt1 S1 2.2892(15) . ? Pt1 S2 2.2922(15) . ? Pt1 S2 2.2922(15) 2_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 123.4(4) . . ? O1 C1 C2 117.0(5) . . ? C6 C1 C2 119.7(5) . . ? C3 C2 C1 119.0(5) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 120.4(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 120.3(5) . . ? C5 C4 Br1 119.9(4) . . ? C3 C4 Br1 119.7(4) . . ? C4 C5 C6 121.6(5) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 118.8(4) . . ? C5 C6 C7 119.5(5) . . ? C1 C6 C7 121.2(4) . . ? N1 C7 C6 123.9(5) . . ? N1 C7 H7 118.0 . . ? C6 C7 H7 118.0 . . ? N1 C8 C9 110.0(5) . . ? N1 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? N1 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C8 C9 C10 116.2(5) . . ? C8 C9 H9A 108.2 . . ? C10 C9 H9A 108.2 . . ? C8 C9 H9B 108.2 . . ? C10 C9 H9B 108.2 . . ? H9A C9 H9B 107.4 . . ? N2 C10 C9 112.2(4) . . ? N2 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? N2 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N2 C11 C12 108.9(4) . . ? N2 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? N2 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N3 C12 C11 110.3(5) . . ? N3 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 . . ? N3 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? N3 C13 C14 113.8(5) . . ? N3 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? N3 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C13 C14 C15 116.2(5) . . ? C13 C14 H14A 108.2 . . ? C15 C14 H14A 108.2 . . ? C13 C14 H14B 108.2 . . ? C15 C14 H14B 108.2 . . ? H14A C14 H14B 107.4 . . ? N4 C15 C14 108.6(4) . . ? N4 C15 H15A 110.0 . . ? C14 C15 H15A 110.0 . . ? N4 C15 H15B 110.0 . . ? C14 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? N4 C16 C17 124.2(5) . . ? N4 C16 H16 117.9 . . ? C17 C16 H16 117.9 . . ? C18 C17 C22 120.2(4) . . ? C18 C17 C16 118.5(4) . . ? C22 C17 C16 120.3(5) . . ? C19 C18 C17 120.4(5) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C18 119.5(5) . . ? C20 C19 Br2 121.3(4) . . ? C18 C19 Br2 119.1(4) . . ? C21 C20 C19 121.5(5) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 120.5(5) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? O2 C22 C17 123.5(4) . . ? O2 C22 C21 118.7(4) . . ? C17 C22 C21 117.8(5) . . ? N5 C23 C24 175.5(8) . . ? C25 C24 C23 121.7(5) . . ? C25 C24 S2 122.5(4) . . ? C23 C24 S2 115.8(4) . . ? C24 C25 C26 120.9(5) . . ? C24 C25 S1 123.1(4) . . ? C26 C25 S1 115.9(4) . . ? N6 C26 C25 177.1(8) . . ? O2 Mn1 O1 176.82(16) . . ? O2 Mn1 N4 87.08(15) . . ? O1 Mn1 N4 91.01(15) . . ? O2 Mn1 N1 91.24(15) . . ? O1 Mn1 N1 86.73(15) . . ? N4 Mn1 N1 103.31(17) . . ? O2 Mn1 N2 90.11(16) . . ? O1 Mn1 N2 92.20(16) . . ? N4 Mn1 N2 169.71(17) . . ? N1 Mn1 N2 86.64(17) . . ? O2 Mn1 N3 92.80(16) . . ? O1 Mn1 N3 89.63(16) . . ? N4 Mn1 N3 86.88(18) . . ? N1 Mn1 N3 169.23(18) . . ? N2 Mn1 N3 83.37(18) . . ? C7 N1 C8 116.7(4) . . ? C7 N1 Mn1 122.2(3) . . ? C8 N1 Mn1 120.8(3) . . ? C10 N2 C11 109.9(4) . . ? C10 N2 Mn1 118.0(4) . . ? C11 N2 Mn1 106.8(3) . . ? C10 N2 H28 107.2 . . ? C11 N2 H28 107.2 . . ? Mn1 N2 H28 107.2 . . ? C12 N3 C13 113.1(5) . . ? C12 N3 Mn1 105.8(3) . . ? C13 N3 Mn1 117.3(4) . . ? C12 N3 H27 106.6 . . ? C13 N3 H27 106.6 . . ? Mn1 N3 H27 106.6 . . ? C16 N4 C15 116.7(4) . . ? C16 N4 Mn1 122.1(3) . . ? C15 N4 Mn1 120.9(4) . . ? C1 O1 Mn1 122.5(3) . . ? C22 O2 Mn1 124.0(3) . . ? S1 Pt1 S1 180.00(6) 2_676 . ? S1 Pt1 S2 90.50(5) 2_676 . ? S1 Pt1 S2 89.50(5) . . ? S1 Pt1 S2 89.50(5) 2_676 2_676 ? S1 Pt1 S2 90.50(5) . 2_676 ? S2 Pt1 S2 180.000(1) . 2_676 ? C25 S1 Pt1 102.28(19) . . ? C24 S2 Pt1 102.46(18) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.938 _refine_diff_density_min -2.109 _refine_diff_density_rms 0.100 _database_code_depnum_ccdc_archive 'CCDC 976207'