# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email jingye@swu.edu.cn loop_ _publ_author_name 'Haiyan Chen' 'Dongrong Xiao' 'Jianghong He' 'Zhifu Li' 'Guangju Zhang' 'Dianzhen Sun' 'Ruo Yuan' 'Enbo Wang' 'Qun-Li Luo' data_c5b _database_code_depnum_ccdc_archive 'CCDC 808838' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H92 Mn4 N8 O26 S4' _chemical_formula_weight 2265.90 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 24.492(5) _cell_length_b 16.886(3) _cell_length_c 25.983(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10746(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 54713 _cell_measurement_theta_min 1.57 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4672 _exptl_absorpt_coefficient_mu 0.615 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7956 _exptl_absorpt_correction_T_max 0.8276 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX 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 54713 _diffrn_reflns_av_R_equivalents 0.1087 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9439 _reflns_number_gt 5261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^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 9439 _refine_ls_number_parameters 718 _refine_ls_number_restraints 172 _refine_ls_R_factor_all 0.1268 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1983 _refine_ls_wR_factor_gt 0.1582 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.59134(3) 0.02876(4) 0.51421(3) 0.0404(2) Uani 1 1 d . . . Mn2 Mn 0.56927(3) 0.24246(5) 0.51466(3) 0.0471(2) Uani 1 1 d . . . S1 S 0.78494(7) 0.27023(12) 0.75738(6) 0.0665(5) Uani 1 1 d . . . S2 S 0.38621(6) 0.51816(8) 0.29057(5) 0.0498(4) Uani 1 1 d . . . O1 O 0.64044(15) 0.0771(2) 0.57646(13) 0.0540(10) Uani 1 1 d . . . O2 O 0.59379(16) 0.1894(2) 0.58382(13) 0.0587(10) Uani 1 1 d . . . O3 O 0.64097(15) 0.4297(2) 0.95269(13) 0.0541(10) Uani 1 1 d . . . O4 O 0.63973(17) 0.3019(2) 0.97367(15) 0.0643(11) Uani 1 1 d . . . O5 O 0.80416(19) 0.3415(3) 0.73334(17) 0.0875(14) Uani 1 1 d . . . O6 O 0.82268(18) 0.2099(3) 0.77256(16) 0.0854(15) Uani 1 1 d . . . O7 O 0.53474(18) 0.2944(2) 0.44831(16) 0.0724(13) Uani 1 1 d . . . O8 O 0.48968(19) 0.1976(2) 0.40980(14) 0.0715(12) Uani 1 1 d . . . O9 O 0.53399(15) 0.4991(2) 0.07447(12) 0.0480(9) Uani 1 1 d . . . O10 O 0.45418(14) 0.45398(19) 0.04457(12) 0.0439(8) Uani 1 1 d . . . O11 O 0.40183(17) 0.5940(2) 0.31087(14) 0.0622(11) Uani 1 1 d . . . O12 O 0.32945(16) 0.4980(2) 0.28726(14) 0.0638(11) Uani 1 1 d . . . OW1 O 0.52904(15) 0.1280(2) 0.49145(14) 0.0430(8) Uani 1 1 d D . . HW1A H 0.5206(17) 0.142(3) 0.4611(8) 0.07(2) Uiso 1 1 d D . . HW1B H 0.5010(12) 0.110(3) 0.5061(15) 0.062(19) Uiso 1 1 d D . . N3 N 0.63778(19) -0.0831(3) 0.52663(17) 0.0535(12) Uani 1 1 d . . . N1 N 0.4980(2) 0.2930(3) 0.5621(2) 0.0706(15) Uani 1 1 d D . . C1 C 0.4958(5) 0.2812(7) 0.6141(3) 0.079(4) Uani 0.647(12) 1 d PDU A 1 H1A H 0.5208 0.2456 0.6279 0.095 Uiso 0.647(12) 1 calc PR A 1 C2 C 0.4601(5) 0.3168(7) 0.6482(5) 0.090(4) Uani 0.647(12) 1 d PDU A 1 H2A H 0.4617 0.3106 0.6838 0.108 Uiso 0.647(12) 1 calc PR A 1 C3 C 0.4212(8) 0.3633(11) 0.6229(5) 0.113(4) Uani 0.647(12) 1 d PDU A 1 C1A C 0.4744(9) 0.2542(11) 0.6003(7) 0.079(4) Uani 0.35 1 d PDU A 2 H1AA H 0.4839 0.2029 0.6097 0.095 Uiso 0.353(12) 1 calc PR A 2 C2A C 0.4344(9) 0.2972(13) 0.6248(9) 0.090(4) Uani 0.35 1 d PDU A 2 H2AA H 0.4125 0.2659 0.6458 0.108 Uiso 0.353(12) 1 calc PR A 2 C3A C 0.4191(18) 0.3764(15) 0.6256(7) 0.113(4) Uani 0.35 1 d PDU A 2 C4 C 0.4289(4) 0.3908(6) 0.5740(4) 0.126(4) Uani 1 1 d D . . H4A H 0.4087 0.4328 0.5608 0.126 Uiso 0.647(12) 1 calc PR A 1 H4B H 0.4075 0.4287 0.5576 0.126 Uiso 0.353(12) 1 calc PR A 2 C5 C 0.4682(3) 0.3531(5) 0.5451(3) 0.105(3) Uani 1 1 d D A . H5A H 0.4741 0.3708 0.5117 0.126 Uiso 1 1 calc R . . N2 N 0.4619(4) 0.7297(7) 0.7443(4) 0.148(3) Uani 1 1 d DU . . C8 C 0.3947(4) 0.6000(6) 0.7242(4) 0.108(3) Uani 1 1 d D . . C6 C 0.4636(5) 0.6632(8) 0.7716(4) 0.140(4) Uani 1 1 d DU . . H6A H 0.4882 0.6611 0.7989 0.167 Uiso 1 1 calc R A . C7 C 0.4332(5) 0.6000(7) 0.7633(4) 0.132(4) Uani 1 1 d U . . H7A H 0.4376 0.5552 0.7837 0.159 Uiso 1 1 calc R . . C9 C 0.3913(4) 0.6682(7) 0.6968(4) 0.120(3) Uani 1 1 d . . . H9A H 0.3663 0.6723 0.6700 0.144 Uiso 1 1 calc R . . C10 C 0.4239(5) 0.7296(7) 0.7081(4) 0.131(3) Uani 1 1 d DU . . H10A H 0.4194 0.7758 0.6890 0.157 Uiso 1 1 calc R A . C11 C 0.3731(5) 0.4079(8) 0.6474(6) 0.108(5) Uani 0.623(12) 1 d PDU A 1 H11A H 0.3481 0.4278 0.6215 0.130 Uiso 0.623(12) 1 calc PR A 1 H11B H 0.3532 0.3744 0.6713 0.130 Uiso 0.623(12) 1 calc PR A 1 C12 C 0.4023(6) 0.4756(9) 0.6754(6) 0.109(5) Uani 0.623(12) 1 d PDU A 1 H12A H 0.4161 0.5125 0.6498 0.131 Uiso 0.623(12) 1 calc PR A 1 H12B H 0.4335 0.4540 0.6935 0.131 Uiso 0.623(12) 1 calc PR A 1 C13 C 0.3670(7) 0.5217(8) 0.7139(7) 0.141(7) Uani 0.623(12) 1 d PDU A 1 H13A H 0.3308 0.5305 0.6998 0.170 Uiso 0.623(12) 1 calc PR A 1 H13B H 0.3633 0.4919 0.7457 0.170 Uiso 0.623(12) 1 calc PR A 1 C11A C 0.3950(11) 0.4118(14) 0.6756(7) 0.108(5) Uani 0.38 1 d PDU A 2 H11C H 0.3673 0.3776 0.6903 0.108 Uiso 0.377(12) 1 calc PR A 2 H11D H 0.4232 0.4213 0.7011 0.108 Uiso 0.377(12) 1 calc PR A 2 C12A C 0.3706(11) 0.4890(12) 0.6559(9) 0.109(5) Uani 0.38 1 d PDU A 2 H12C H 0.3396 0.4766 0.6342 0.109 Uiso 0.377(12) 1 calc PR A 2 H12D H 0.3976 0.5155 0.6347 0.109 Uiso 0.377(12) 1 calc PR A 2 C13A C 0.3520(9) 0.5464(16) 0.6979(11) 0.141(7) Uani 0.38 1 d PDU A 2 H13C H 0.3343 0.5155 0.7246 0.170 Uiso 0.377(12) 1 calc PR A 2 H13D H 0.3243 0.5806 0.6831 0.170 Uiso 0.377(12) 1 calc PR A 2 C14 C 0.6537(3) -0.1266(5) 0.4874(3) 0.097(3) Uani 1 1 d . . . H14A H 0.6434 -0.1102 0.4547 0.117 Uiso 1 1 calc R . . C15 C 0.6838(4) -0.1932(5) 0.4913(3) 0.105(3) Uani 1 1 d U . . H15A H 0.6950 -0.2199 0.4618 0.126 Uiso 1 1 calc R . . C16 C 0.6979(3) -0.2213(4) 0.5390(3) 0.090(2) Uani 1 1 d . . . C17 C 0.6796(3) -0.1793(4) 0.5801(3) 0.094(2) Uani 1 1 d . . . H17A H 0.6867 -0.1971 0.6132 0.112 Uiso 1 1 calc R . . C18 C 0.6506(3) -0.1105(4) 0.5729(3) 0.084(2) Uani 1 1 d . . . H18A H 0.6395 -0.0819 0.6016 0.100 Uiso 1 1 calc R . . N4 N 0.6179(2) -0.6435(3) 0.52190(18) 0.0625(14) Uani 1 1 d D . . C21 C 0.6917(3) -0.5165(4) 0.5266(3) 0.0717(18) Uani 1 1 d D . . C19 C 0.6413(3) -0.6123(4) 0.4790(3) 0.073(2) Uani 0.885(8) 1 d PD B 1 H19A H 0.6320 -0.6338 0.4472 0.087 Uiso 0.885(8) 1 calc PR B 1 C20 C 0.6783(3) -0.5507(4) 0.4801(3) 0.076(2) Uani 0.885(8) 1 d PD B 1 H20A H 0.6939 -0.5324 0.4497 0.091 Uiso 0.885(8) 1 calc PR B 1 C22 C 0.6693(3) -0.5489(4) 0.5690(3) 0.082(3) Uani 0.885(8) 1 d PD B 1 H22A H 0.6785 -0.5294 0.6013 0.099 Uiso 0.885(8) 1 calc PR B 1 C23 C 0.6330(4) -0.6102(4) 0.5651(3) 0.087(3) Uani 0.885(8) 1 d PD B 1 H23A H 0.6180 -0.6298 0.5954 0.104 Uiso 0.885(8) 1 calc PR B 1 C19A C 0.5991(17) -0.5686(10) 0.5269(14) 0.073(2) Uani 0.11 1 d PDU B 2 H19B H 0.5618 -0.5584 0.5253 0.087 Uiso 0.115(8) 1 calc PR B 2 C20A C 0.6358(6) -0.508(3) 0.5343(17) 0.076(2) Uani 0.11 1 d PDU B 2 H20B H 0.6226 -0.4585 0.5447 0.091 Uiso 0.115(8) 1 calc PR B 2 C22A C 0.7106(17) -0.5912(11) 0.5371(18) 0.082(3) Uani 0.11 1 d PDU B 2 H22B H 0.7463 -0.6016 0.5473 0.099 Uiso 0.115(8) 1 calc PR B 2 C23A C 0.6718(6) -0.649(3) 0.5313(18) 0.087(3) Uani 0.11 1 d PDU B 2 H23B H 0.6848 -0.7007 0.5343 0.104 Uiso 0.115(8) 1 calc PR B 2 C24 C 0.7319(3) -0.2955(4) 0.5438(3) 0.101(3) Uani 1 1 d D B . H24A H 0.7615 -0.2938 0.5191 0.122 Uiso 1 1 calc R . . H24B H 0.7477 -0.2981 0.5780 0.122 Uiso 1 1 calc R . . C25 C 0.6978(3) -0.3681(4) 0.5345(3) 0.103(2) Uani 1 1 d DU . . H25A H 0.6778 -0.3610 0.5026 0.124 Uiso 1 1 calc R B . H25B H 0.6712 -0.3726 0.5620 0.124 Uiso 1 1 calc R . . C26 C 0.7301(3) -0.4468(3) 0.5311(3) 0.094(2) Uani 1 1 d D B . H26A H 0.7541 -0.4454 0.5014 0.113 Uiso 1 1 calc R . . H26B H 0.7525 -0.4528 0.5616 0.113 Uiso 1 1 calc R . . C27 C 0.6948(3) 0.2737(4) 0.6970(2) 0.081(2) Uani 1 1 d . . . H27A H 0.6907 0.3254 0.7088 0.098 Uiso 1 1 calc R . . C28 C 0.6600(3) 0.2435(4) 0.6609(3) 0.081(2) Uani 1 1 d . . . H28A H 0.6316 0.2749 0.6486 0.097 Uiso 1 1 calc R . . C29 C 0.6660(2) 0.1680(3) 0.64225(19) 0.0502(14) Uani 1 1 d . . . C30 C 0.7050(2) 0.1201(3) 0.6637(2) 0.0550(15) Uani 1 1 d . . . H30A H 0.7076 0.0674 0.6534 0.066 Uiso 1 1 calc R . . C31 C 0.7404(2) 0.1489(4) 0.7003(2) 0.0593(15) Uani 1 1 d . . . H31A H 0.7671 0.1162 0.7144 0.071 Uiso 1 1 calc R . . C32 C 0.7361(2) 0.2263(4) 0.7158(2) 0.0595(16) Uani 1 1 d . . . C33 C 0.7469(2) 0.2980(3) 0.8128(2) 0.0525(14) Uani 1 1 d . . . C34 C 0.7420(3) 0.2449(4) 0.8521(2) 0.0671(17) Uani 1 1 d . . . H34A H 0.7588 0.1956 0.8500 0.080 Uiso 1 1 calc R . . C35 C 0.7118(2) 0.2650(3) 0.8952(2) 0.0599(16) Uani 1 1 d . . . H35A H 0.7082 0.2289 0.9220 0.072 Uiso 1 1 calc R . . C36 C 0.6871(2) 0.3386(3) 0.89872(19) 0.0467(13) Uani 1 1 d . . . C37 C 0.6942(2) 0.3910(3) 0.8595(2) 0.0574(15) Uani 1 1 d . . . H37A H 0.6790 0.4414 0.8622 0.069 Uiso 1 1 calc R . . C38 C 0.7231(2) 0.3714(3) 0.8161(2) 0.0601(16) Uani 1 1 d . . . H38A H 0.7266 0.4075 0.7892 0.072 Uiso 1 1 calc R . . C39 C 0.6307(2) 0.1411(3) 0.59759(19) 0.0464(13) Uani 1 1 d . . . C40 C 0.6528(2) 0.3586(4) 0.9453(2) 0.0495(14) Uani 1 1 d . . . C41 C 0.4059(2) 0.3660(3) 0.3213(2) 0.0593(16) Uani 1 1 d . . . H41A H 0.3791 0.3511 0.2979 0.071 Uiso 1 1 calc R . . C42 C 0.4322(3) 0.3095(3) 0.3501(2) 0.0585(16) Uani 1 1 d . . . H42A H 0.4230 0.2564 0.3460 0.070 Uiso 1 1 calc R . . C43 C 0.4716(2) 0.3305(3) 0.38463(19) 0.0488(13) Uani 1 1 d . . . C44 C 0.4848(3) 0.4088(3) 0.3901(2) 0.0639(17) Uani 1 1 d . . . H44A H 0.5115 0.4235 0.4137 0.077 Uiso 1 1 calc R . . C45 C 0.4591(3) 0.4659(3) 0.3612(2) 0.0623(16) Uani 1 1 d . . . H45A H 0.4688 0.5189 0.3647 0.075 Uiso 1 1 calc R . . C46 C 0.4189(2) 0.4440(3) 0.32694(18) 0.0446(13) Uani 1 1 d . . . C47 C 0.4155(2) 0.5085(3) 0.22854(19) 0.0442(13) Uani 1 1 d . . . C48 C 0.3949(2) 0.4505(3) 0.1958(2) 0.0533(14) Uani 1 1 d . . . H48A H 0.3668 0.4172 0.2061 0.064 Uiso 1 1 calc R . . C49 C 0.4179(2) 0.4442(3) 0.14733(19) 0.0518(14) Uani 1 1 d . . . H49A H 0.4046 0.4062 0.1247 0.062 Uiso 1 1 calc R . . C50 C 0.4598(2) 0.4925(3) 0.13185(18) 0.0422(12) Uani 1 1 d . . . C51 C 0.4796(2) 0.5494(3) 0.1654(2) 0.0520(14) Uani 1 1 d . . . H51A H 0.5086 0.5814 0.1555 0.062 Uiso 1 1 calc R . . C52 C 0.4563(2) 0.5588(3) 0.21368(19) 0.0517(14) Uani 1 1 d . . . H52A H 0.4682 0.5988 0.2356 0.062 Uiso 1 1 calc R . . C53 C 0.5008(2) 0.2680(4) 0.4158(2) 0.0522(14) Uani 1 1 d . . . C54 C 0.4849(2) 0.4814(3) 0.07979(18) 0.0403(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0418(5) 0.0433(5) 0.0360(4) 0.0027(3) 0.0012(3) 0.0003(4) Mn2 0.0533(5) 0.0427(5) 0.0454(5) 0.0013(4) -0.0065(4) 0.0001(4) S1 0.0494(10) 0.1021(13) 0.0480(9) -0.0278(9) -0.0011(7) 0.0086(9) S2 0.0586(10) 0.0541(9) 0.0366(7) 0.0061(6) 0.0068(6) 0.0119(7) O1 0.059(3) 0.058(2) 0.045(2) -0.0080(19) -0.0065(18) 0.001(2) O2 0.063(3) 0.074(3) 0.040(2) -0.0048(19) -0.0132(18) 0.018(2) O3 0.059(3) 0.054(2) 0.049(2) -0.0080(19) 0.0093(18) 0.0081(19) O4 0.068(3) 0.061(3) 0.063(3) 0.007(2) 0.014(2) 0.009(2) O5 0.078(3) 0.114(4) 0.070(3) -0.015(3) 0.022(2) -0.021(3) O6 0.058(3) 0.134(4) 0.064(3) -0.036(3) -0.009(2) 0.039(3) O7 0.090(3) 0.056(2) 0.071(3) 0.020(2) -0.039(2) -0.013(2) O8 0.117(4) 0.040(2) 0.057(3) 0.0028(19) -0.026(2) 0.001(2) O9 0.047(2) 0.059(2) 0.038(2) -0.0066(16) 0.0049(16) -0.0018(18) O10 0.046(2) 0.051(2) 0.034(2) -0.0019(16) 0.0017(16) 0.0000(17) O11 0.092(3) 0.047(2) 0.048(2) 0.0012(18) 0.013(2) 0.015(2) O12 0.048(3) 0.088(3) 0.055(2) 0.014(2) 0.0097(18) 0.015(2) OW1 0.049(2) 0.042(2) 0.038(2) 0.0068(17) -0.0006(18) -0.0044(17) N3 0.057(3) 0.060(3) 0.043(3) 0.004(2) 0.004(2) 0.011(2) N1 0.071(4) 0.062(3) 0.079(4) -0.001(3) -0.002(3) 0.018(3) C1 0.078(6) 0.071(6) 0.088(6) 0.010(5) 0.026(5) 0.008(5) C2 0.088(7) 0.096(6) 0.087(6) 0.012(5) 0.017(5) 0.007(5) C3 0.101(6) 0.100(6) 0.139(6) 0.005(5) 0.042(5) 0.022(5) C1A 0.078(6) 0.071(6) 0.088(6) 0.010(5) 0.026(5) 0.008(5) C2A 0.088(7) 0.096(6) 0.087(6) 0.012(5) 0.017(5) 0.007(5) C3A 0.101(6) 0.100(6) 0.139(6) 0.005(5) 0.042(5) 0.022(5) C4 0.102(7) 0.129(8) 0.148(9) -0.036(7) -0.025(6) 0.065(6) C5 0.119(7) 0.107(6) 0.091(6) -0.013(5) -0.015(5) 0.047(6) N2 0.126(6) 0.167(7) 0.151(7) -0.031(6) 0.018(5) 0.002(6) C8 0.107(7) 0.089(7) 0.129(8) -0.028(6) 0.031(6) 0.014(5) C6 0.137(7) 0.157(8) 0.125(7) -0.028(7) -0.024(6) 0.030(7) C7 0.154(8) 0.118(7) 0.124(7) 0.006(6) 0.003(6) 0.048(6) C9 0.129(9) 0.108(7) 0.125(8) -0.024(7) -0.024(6) 0.028(7) C10 0.148(8) 0.117(7) 0.127(7) -0.002(6) 0.001(6) 0.019(6) C11 0.093(7) 0.115(6) 0.118(8) -0.006(6) 0.014(6) 0.010(5) C12 0.105(8) 0.110(6) 0.113(7) -0.013(6) 0.014(6) 0.005(6) C13 0.149(8) 0.124(9) 0.151(9) -0.008(6) 0.026(6) -0.003(6) C11A 0.093(7) 0.115(6) 0.118(8) -0.006(6) 0.014(6) 0.010(5) C12A 0.105(8) 0.110(6) 0.113(7) -0.013(6) 0.014(6) 0.005(6) C13A 0.149(8) 0.124(9) 0.151(9) -0.008(6) 0.026(6) -0.003(6) C14 0.118(7) 0.117(6) 0.057(5) -0.003(4) -0.015(4) 0.070(5) C15 0.132(6) 0.106(5) 0.078(5) -0.018(4) -0.015(4) 0.056(5) C16 0.108(6) 0.073(5) 0.090(6) 0.002(4) -0.023(5) 0.037(4) C17 0.124(7) 0.087(5) 0.070(5) 0.011(4) -0.007(4) 0.040(5) C18 0.118(6) 0.073(5) 0.061(4) 0.004(4) 0.002(4) 0.035(4) N4 0.076(4) 0.052(3) 0.059(3) 0.001(2) 0.003(3) -0.011(3) C21 0.065(5) 0.057(4) 0.093(5) -0.004(4) -0.012(4) -0.008(3) C19 0.085(5) 0.069(4) 0.064(5) -0.007(4) 0.002(4) -0.009(4) C20 0.087(5) 0.059(4) 0.083(5) 0.000(4) 0.011(4) -0.015(4) C22 0.108(6) 0.077(5) 0.062(5) -0.013(4) -0.005(4) -0.031(4) C23 0.118(6) 0.083(5) 0.059(5) -0.001(4) 0.003(4) -0.034(5) C19A 0.085(5) 0.069(4) 0.064(5) -0.007(4) 0.002(4) -0.009(4) C20A 0.087(5) 0.059(4) 0.083(5) 0.000(4) 0.011(4) -0.015(4) C22A 0.108(6) 0.077(5) 0.062(5) -0.013(4) -0.005(4) -0.031(4) C23A 0.118(6) 0.083(5) 0.059(5) -0.001(4) 0.003(4) -0.034(5) C24 0.105(7) 0.062(5) 0.137(7) 0.011(5) -0.017(5) 0.008(4) C25 0.106(4) 0.080(4) 0.123(4) 0.015(4) -0.034(4) -0.010(3) C26 0.087(6) 0.055(4) 0.141(7) 0.004(4) -0.004(5) -0.012(4) C27 0.093(5) 0.075(4) 0.077(5) -0.039(4) -0.033(4) 0.028(4) C28 0.090(5) 0.073(4) 0.079(5) -0.034(4) -0.041(4) 0.033(4) C29 0.049(3) 0.061(4) 0.041(3) -0.007(3) -0.004(3) 0.014(3) C30 0.060(4) 0.056(4) 0.049(3) -0.006(3) -0.003(3) 0.010(3) C31 0.055(4) 0.074(4) 0.049(3) -0.005(3) -0.005(3) 0.010(3) C32 0.045(4) 0.088(4) 0.046(3) -0.022(3) -0.003(3) 0.014(3) C33 0.041(3) 0.074(4) 0.042(3) -0.020(3) -0.004(2) 0.004(3) C34 0.075(5) 0.059(4) 0.066(4) -0.007(3) 0.005(3) 0.015(3) C35 0.072(4) 0.062(4) 0.045(3) 0.004(3) 0.010(3) 0.011(3) C36 0.049(3) 0.051(3) 0.041(3) -0.004(3) -0.001(2) 0.005(3) C37 0.063(4) 0.057(4) 0.052(4) -0.005(3) 0.011(3) 0.009(3) C38 0.075(4) 0.060(4) 0.045(3) -0.004(3) 0.000(3) 0.008(3) C39 0.042(3) 0.062(4) 0.036(3) 0.002(3) 0.002(2) -0.002(3) C40 0.042(3) 0.061(4) 0.045(3) -0.001(3) -0.006(3) 0.008(3) C41 0.074(4) 0.050(4) 0.053(4) -0.002(3) -0.018(3) -0.006(3) C42 0.083(5) 0.042(3) 0.051(4) 0.009(3) -0.019(3) -0.008(3) C43 0.065(4) 0.045(3) 0.036(3) 0.011(2) -0.004(3) -0.002(3) C44 0.070(4) 0.050(4) 0.072(4) 0.010(3) -0.026(3) -0.005(3) C45 0.074(4) 0.044(3) 0.069(4) 0.005(3) -0.012(3) -0.008(3) C46 0.057(4) 0.046(3) 0.032(3) 0.004(2) 0.001(2) 0.003(3) C47 0.053(4) 0.042(3) 0.037(3) 0.007(2) 0.003(2) 0.004(3) C48 0.057(4) 0.055(3) 0.048(3) 0.006(3) 0.002(3) -0.010(3) C49 0.064(4) 0.059(3) 0.032(3) -0.004(2) 0.001(3) -0.012(3) C50 0.047(3) 0.043(3) 0.036(3) 0.003(2) 0.001(2) 0.005(2) C51 0.062(4) 0.053(3) 0.041(3) -0.002(3) 0.009(3) -0.011(3) C52 0.075(4) 0.044(3) 0.036(3) -0.006(2) 0.003(3) -0.005(3) C53 0.066(4) 0.055(4) 0.036(3) 0.007(3) -0.003(3) 0.002(3) C54 0.045(3) 0.039(3) 0.037(3) 0.004(2) 0.005(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O3 2.127(3) 7_565 ? Mn1 O9 2.156(3) 7_566 ? Mn1 O1 2.175(4) . ? Mn1 N3 2.229(5) . ? Mn1 O10 2.274(3) 3_645 ? Mn1 OW1 2.342(4) . ? Mn2 O2 2.096(4) . ? Mn2 O7 2.111(4) . ? Mn2 O4 2.162(4) 7_565 ? Mn2 OW1 2.252(4) . ? Mn2 N4 2.272(5) 1_565 ? Mn2 N1 2.301(5) . ? S1 O6 1.431(5) . ? S1 O5 1.435(5) . ? S1 C32 1.775(6) . ? S1 C33 1.778(5) . ? S2 O12 1.434(4) . ? S2 O11 1.437(4) . ? S2 C46 1.762(5) . ? S2 C47 1.772(5) . ? O1 C39 1.235(6) . ? O2 C39 1.270(6) . ? O3 C40 1.249(6) . ? O3 Mn1 2.127(3) 7_566 ? O4 C40 1.250(6) . ? O4 Mn2 2.162(4) 7_566 ? O7 C53 1.266(6) . ? O8 C53 1.230(6) . ? O9 C54 1.247(6) . ? O9 Mn1 2.156(3) 7_565 ? O10 C54 1.272(6) . ? O10 Mn1 2.274(3) 3_655 ? OW1 HW1A 0.847(10) . ? OW1 HW1B 0.840(10) . ? N3 C14 1.314(8) . ? N3 C18 1.324(7) . ? N1 C1A 1.323(10) . ? N1 C5 1.326(7) . ? N1 C1 1.366(8) . ? C1 C2 1.384(9) . ? C1 H1A 0.9300 . ? C2 C3 1.398(10) . ? C2 H2A 0.9300 . ? C3 C4 1.367(9) . ? C3 C11 1.537(9) . ? C1A C2A 1.376(10) . ? C1A H1AA 0.9300 . ? C2A C3A 1.389(10) . ? C2A H2AA 0.9300 . ? C3A C4 1.384(10) . ? C3A C11A 1.548(10) . ? C4 C5 1.375(7) . ? C4 H4A 0.9300 . ? C4 H4B 0.9300 . ? C5 H5A 0.9300 . ? N2 C6 1.329(8) . ? N2 C10 1.324(8) . ? C8 C7 1.384(13) . ? C8 C9 1.357(12) . ? C8 C13 1.511(9) . ? C8 C13A 1.544(10) . ? C6 C7 1.321(14) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C9 C10 1.341(13) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.533(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.536(9) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C11A C12A 1.524(10) . ? C11A H11C 0.9700 . ? C11A H11D 0.9700 . ? C12A C13A 1.529(10) . ? C12A H12C 0.9700 . ? C12A H12D 0.9700 . ? C13A H13C 0.9700 . ? C13A H13D 0.9700 . ? C14 C15 1.350(9) . ? C14 H14A 0.9300 . ? C15 C16 1.372(9) . ? C15 H15A 0.9300 . ? C16 C17 1.357(10) . ? C16 C24 1.509(9) . ? C17 C18 1.375(9) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? N4 C23 1.308(6) . ? N4 C23A 1.345(10) . ? N4 C19A 1.351(10) . ? N4 C19 1.359(6) . ? N4 Mn2 2.272(5) 1_545 ? C21 C22 1.346(7) . ? C21 C22A 1.370(10) . ? C21 C20 1.381(7) . ? C21 C20A 1.393(10) . ? C21 C26 1.511(8) . ? C19 C20 1.379(7) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C22 C23 1.367(7) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C19A C20A 1.382(10) . ? C19A H19B 0.9300 . ? C20A H20B 0.9300 . ? C22A C23A 1.374(11) . ? C22A H22B 0.9300 . ? C23A H23B 0.9300 . ? C24 C25 1.503(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.548(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.368(8) . ? C27 C32 1.378(8) . ? C27 H27A 0.9300 . ? C28 C29 1.371(8) . ? C28 H28A 0.9300 . ? C29 C30 1.371(7) . ? C29 C39 1.517(7) . ? C30 C31 1.376(7) . ? C30 H30A 0.9300 . ? C31 C32 1.372(8) . ? C31 H31A 0.9300 . ? C33 C34 1.364(8) . ? C33 C38 1.374(7) . ? C34 C35 1.383(8) . ? C34 H34A 0.9300 . ? C35 C36 1.387(7) . ? C35 H35A 0.9300 . ? C36 C37 1.360(7) . ? C36 C40 1.512(7) . ? C37 C38 1.373(7) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C41 C46 1.362(7) . ? C41 C42 1.374(7) . ? C41 H41A 0.9300 . ? C42 C43 1.365(7) . ? C42 H42A 0.9300 . ? C43 C44 1.368(7) . ? C43 C53 1.510(7) . ? C44 C45 1.375(7) . ? C44 H44A 0.9300 . ? C45 C46 1.377(7) . ? C45 H45A 0.9300 . ? C47 C52 1.368(7) . ? C47 C48 1.391(7) . ? C48 C49 1.383(7) . ? C48 H48A 0.9300 . ? C49 C50 1.371(7) . ? C49 H49A 0.9300 . ? C50 C51 1.384(7) . ? C50 C54 1.498(7) . ? C51 C52 1.388(7) . ? C51 H51A 0.9300 . ? C52 H52A 0.9300 . ? 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 O3 Mn1 O9 172.00(14) 7_565 7_566 ? O3 Mn1 O1 96.84(14) 7_565 . ? O9 Mn1 O1 84.38(14) 7_566 . ? O3 Mn1 N3 95.57(15) 7_565 . ? O9 Mn1 N3 92.41(15) 7_566 . ? O1 Mn1 N3 85.89(16) . . ? O3 Mn1 O10 87.64(13) 7_565 3_645 ? O9 Mn1 O10 92.69(13) 7_566 3_645 ? O1 Mn1 O10 168.30(13) . 3_645 ? N3 Mn1 O10 82.91(15) . 3_645 ? O3 Mn1 OW1 86.93(14) 7_565 . ? O9 Mn1 OW1 85.14(13) 7_566 . ? O1 Mn1 OW1 106.23(13) . . ? N3 Mn1 OW1 167.28(15) . . ? O10 Mn1 OW1 84.74(12) 3_645 . ? O2 Mn2 O7 173.03(17) . . ? O2 Mn2 O4 92.62(15) . 7_565 ? O7 Mn2 O4 93.52(17) . 7_565 ? O2 Mn2 OW1 89.33(14) . . ? O7 Mn2 OW1 87.86(14) . . ? O4 Mn2 OW1 85.41(14) 7_565 . ? O2 Mn2 N4 98.10(17) . 1_565 ? O7 Mn2 N4 85.72(17) . 1_565 ? O4 Mn2 N4 85.18(17) 7_565 1_565 ? OW1 Mn2 N4 168.26(16) . 1_565 ? O2 Mn2 N1 85.21(17) . . ? O7 Mn2 N1 88.83(19) . . ? O4 Mn2 N1 176.35(18) 7_565 . ? OW1 Mn2 N1 97.48(17) . . ? N4 Mn2 N1 92.21(18) 1_565 . ? O6 S1 O5 120.3(3) . . ? O6 S1 C32 107.8(3) . . ? O5 S1 C32 107.8(3) . . ? O6 S1 C33 107.6(3) . . ? O5 S1 C33 107.7(3) . . ? C32 S1 C33 104.5(3) . . ? O12 S2 O11 119.5(2) . . ? O12 S2 C46 107.7(2) . . ? O11 S2 C46 108.4(2) . . ? O12 S2 C47 108.4(2) . . ? O11 S2 C47 108.0(2) . . ? C46 S2 C47 103.8(2) . . ? C39 O1 Mn1 123.5(3) . . ? C39 O2 Mn2 136.1(3) . . ? C40 O3 Mn1 124.4(4) . 7_566 ? C40 O4 Mn2 139.5(4) . 7_566 ? C53 O7 Mn2 131.5(4) . . ? C54 O9 Mn1 131.0(3) . 7_565 ? C54 O10 Mn1 124.8(3) . 3_655 ? Mn2 OW1 Mn1 105.15(14) . . ? Mn2 OW1 HW1A 97(4) . . ? Mn1 OW1 HW1A 126(4) . . ? Mn2 OW1 HW1B 123(4) . . ? Mn1 OW1 HW1B 99(4) . . ? HW1A OW1 HW1B 108.7(18) . . ? C14 N3 C18 116.0(5) . . ? C14 N3 Mn1 120.8(4) . . ? C18 N3 Mn1 123.2(4) . . ? C1A N1 C5 112.8(11) . . ? C1A N1 C1 33.7(11) . . ? C5 N1 C1 114.7(7) . . ? C1A N1 Mn2 123.4(9) . . ? C5 N1 Mn2 121.6(5) . . ? C1 N1 Mn2 120.4(6) . . ? N1 C1 C2 126.6(10) . . ? N1 C1 H1A 116.7 . . ? C2 C1 H1A 116.7 . . ? C3 C2 C1 111.9(11) . . ? C3 C2 H2A 124.1 . . ? C1 C2 H2A 124.1 . . ? C2 C3 C4 122.4(12) . . ? C2 C3 C11 127.0(11) . . ? C4 C3 C11 109.0(10) . . ? N1 C1A C2A 113.4(17) . . ? N1 C1A H1AA 123.3 . . ? C2A C1A H1AA 123.3 . . ? C3A C2A C1A 135(2) . . ? C3A C2A H2AA 112.5 . . ? C1A C2A H2AA 112.5 . . ? C4 C3A C2A 96.3(16) . . ? C4 C3A C11A 144.3(18) . . ? C2A C3A C11A 119.1(15) . . ? C3A C4 C5 124.6(13) . . ? C3A C4 C3 9.8(14) . . ? C5 C4 C3 116.5(9) . . ? C3A C4 H4A 113.4 . . ? C5 C4 H4A 121.8 . . ? C3 C4 H4A 121.8 . . ? C3A C4 H4B 117.7 . . ? C5 C4 H4B 117.7 . . ? C3 C4 H4B 125.4 . . ? H4A C4 H4B 6.9 . . ? N1 C5 C4 123.9(8) . . ? N1 C5 H5A 118.0 . . ? C4 C5 H5A 118.0 . . ? C6 N2 C10 113.7(11) . . ? C7 C8 C9 115.4(9) . . ? C7 C8 C13 115.8(13) . . ? C9 C8 C13 128.4(13) . . ? C7 C8 C13A 141.8(18) . . ? C9 C8 C13A 102.9(16) . . ? C13 C8 C13A 26.2(18) . . ? N2 C6 C7 125.2(11) . . ? N2 C6 H6A 117.4 . . ? C7 C6 H6A 117.4 . . ? C6 C7 C8 120.3(10) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C10 C9 C8 120.3(10) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? N2 C10 C9 125.1(11) . . ? N2 C10 H10A 117.5 . . ? C9 C10 H10A 117.5 . . ? C12 C11 C3 101.7(13) . . ? C12 C11 H11A 111.4 . . ? C3 C11 H11A 111.4 . . ? C12 C11 H11B 111.4 . . ? C3 C11 H11B 111.4 . . ? H11A C11 H11B 109.3 . . ? C11 C12 C13 115.1(10) . . ? C11 C12 H12A 108.5 . . ? C13 C12 H12A 108.5 . . ? C11 C12 H12B 108.5 . . ? C13 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C8 C13 C12 107.8(11) . . ? C8 C13 H13A 110.1 . . ? C12 C13 H13A 110.1 . . ? C8 C13 H13B 110.1 . . ? C12 C13 H13B 110.1 . . ? H13A C13 H13B 108.5 . . ? C12A C11A C3A 101.4(16) . . ? C12A C11A H11C 111.5 . . ? C3A C11A H11C 111.5 . . ? C12A C11A H11D 111.5 . . ? C3A C11A H11D 111.5 . . ? H11C C11A H11D 109.3 . . ? C11A C12A C13A 115(2) . . ? C11A C12A H12C 108.6 . . ? C13A C12A H12C 108.6 . . ? C11A C12A H12D 108.6 . . ? C13A C12A H12D 108.6 . . ? H12C C12A H12D 107.5 . . ? C12A C13A C8 119.0(19) . . ? C12A C13A H13C 107.6 . . ? C8 C13A H13C 107.6 . . ? C12A C13A H13D 107.6 . . ? C8 C13A H13D 107.6 . . ? H13C C13A H13D 107.0 . . ? N3 C14 C15 124.7(6) . . ? N3 C14 H14A 117.7 . . ? C15 C14 H14A 117.7 . . ? C14 C15 C16 119.6(7) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C17 C16 C15 116.4(7) . . ? C17 C16 C24 123.5(7) . . ? C15 C16 C24 120.0(7) . . ? C16 C17 C18 120.4(7) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? N3 C18 C17 122.7(6) . . ? N3 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? C23 N4 C23A 66(2) . . ? C23 N4 C19A 67.3(17) . . ? C23A N4 C19A 113(3) . . ? C23 N4 C19 114.6(6) . . ? C23A N4 C19 76(2) . . ? C19A N4 C19 82.0(15) . . ? C23 N4 Mn2 125.7(4) . 1_545 ? C23A N4 Mn2 118(2) . 1_545 ? C19A N4 Mn2 128.4(19) . 1_545 ? C19 N4 Mn2 118.8(4) . 1_545 ? C22 C21 C22A 66(2) . . ? C22 C21 C20 116.7(6) . . ? C22A C21 C20 83(2) . . ? C22 C21 C20A 61.7(18) . . ? C22A C21 C20A 114(3) . . ? C20 C21 C20A 86.3(19) . . ? C22 C21 C26 120.5(6) . . ? C22A C21 C26 119.5(19) . . ? C20 C21 C26 122.8(6) . . ? C20A C21 C26 121.0(19) . . ? N4 C19 C20 123.5(6) . . ? N4 C19 H19A 118.2 . . ? C20 C19 H19A 118.2 . . ? C19 C20 C21 119.3(7) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C21 C22 C23 120.8(7) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? N4 C23 C22 125.0(7) . . ? N4 C23 H23A 117.5 . . ? C22 C23 H23A 117.5 . . ? N4 C19A C20A 119(4) . . ? N4 C19A H19B 120.3 . . ? C20A C19A H19B 120.3 . . ? C19A C20A C21 123(4) . . ? C19A C20A H20B 118.7 . . ? C21 C20A H20B 118.7 . . ? C21 C22A C23A 114(4) . . ? C21 C22A H22B 123.2 . . ? C23A C22A H22B 123.2 . . ? N4 C23A C22A 130(4) . . ? N4 C23A H23B 114.8 . . ? C22A C23A H23B 114.8 . . ? C25 C24 C16 111.0(6) . . ? C25 C24 H24A 109.4 . . ? C16 C24 H24A 109.4 . . ? C25 C24 H24B 109.4 . . ? C16 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 115.2(6) . . ? C24 C25 H25A 108.5 . . ? C26 C25 H25A 108.5 . . ? C24 C25 H25B 108.5 . . ? C26 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? C21 C26 C25 110.8(6) . . ? C21 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C28 C27 C32 118.9(6) . . ? C28 C27 H27A 120.5 . . ? C32 C27 H27A 120.5 . . ? C27 C28 C29 121.5(6) . . ? C27 C28 H28A 119.3 . . ? C29 C28 H28A 119.3 . . ? C28 C29 C30 118.7(5) . . ? C28 C29 C39 119.2(5) . . ? C30 C29 C39 122.0(5) . . ? C29 C30 C31 120.7(5) . . ? C29 C30 H30A 119.7 . . ? C31 C30 H30A 119.7 . . ? C32 C31 C30 119.5(6) . . ? C32 C31 H31A 120.3 . . ? C30 C31 H31A 120.3 . . ? C31 C32 C27 120.4(6) . . ? C31 C32 S1 121.6(5) . . ? C27 C32 S1 117.9(5) . . ? C34 C33 C38 120.7(5) . . ? C34 C33 S1 118.7(4) . . ? C38 C33 S1 120.7(5) . . ? C33 C34 C35 119.5(5) . . ? C33 C34 H34A 120.3 . . ? C35 C34 H34A 120.3 . . ? C34 C35 C36 120.5(5) . . ? C34 C35 H35A 119.8 . . ? C36 C35 H35A 119.8 . . ? C37 C36 C35 118.5(5) . . ? C37 C36 C40 121.7(5) . . ? C35 C36 C40 119.7(5) . . ? C36 C37 C38 121.7(5) . . ? C36 C37 H37A 119.2 . . ? C38 C37 H37A 119.2 . . ? C33 C38 C37 119.2(5) . . ? C33 C38 H38A 120.4 . . ? C37 C38 H38A 120.4 . . ? O1 C39 O2 125.1(5) . . ? O1 C39 C29 119.5(5) . . ? O2 C39 C29 115.3(5) . . ? O3 C40 O4 125.9(5) . . ? O3 C40 C36 117.8(5) . . ? O4 C40 C36 116.3(5) . . ? C46 C41 C42 120.2(5) . . ? C46 C41 H41A 119.9 . . ? C42 C41 H41A 119.9 . . ? C43 C42 C41 120.6(5) . . ? C43 C42 H42A 119.7 . . ? C41 C42 H42A 119.7 . . ? C42 C43 C44 119.2(5) . . ? C42 C43 C53 120.4(5) . . ? C44 C43 C53 120.5(5) . . ? C43 C44 C45 120.8(5) . . ? C43 C44 H44A 119.6 . . ? C45 C44 H44A 119.6 . . ? C44 C45 C46 119.4(5) . . ? C44 C45 H45A 120.3 . . ? C46 C45 H45A 120.3 . . ? C41 C46 C45 119.8(5) . . ? C41 C46 S2 121.5(4) . . ? C45 C46 S2 118.7(4) . . ? C52 C47 C48 121.9(5) . . ? C52 C47 S2 119.7(4) . . ? C48 C47 S2 118.3(4) . . ? C49 C48 C47 117.7(5) . . ? C49 C48 H48A 121.2 . . ? C47 C48 H48A 121.2 . . ? C50 C49 C48 121.7(5) . . ? C50 C49 H49A 119.2 . . ? C48 C49 H49A 119.2 . . ? C49 C50 C51 119.4(5) . . ? C49 C50 C54 119.8(5) . . ? C51 C50 C54 120.8(5) . . ? C50 C51 C52 120.4(5) . . ? C50 C51 H51A 119.8 . . ? C52 C51 H51A 119.8 . . ? C47 C52 C51 118.9(5) . . ? C47 C52 H52A 120.5 . . ? C51 C52 H52A 120.5 . . ? O8 C53 O7 124.8(5) . . ? O8 C53 C43 120.2(5) . . ? O7 C53 C43 115.0(5) . . ? O9 C54 O10 125.3(4) . . ? O9 C54 C50 117.8(5) . . ? O10 C54 C50 116.9(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mn1 O1 C39 96.2(4) 7_565 . . . ? O9 Mn1 O1 C39 -75.8(4) 7_566 . . . ? N3 Mn1 O1 C39 -168.7(4) . . . . ? O10 Mn1 O1 C39 -151.8(6) 3_645 . . . ? OW1 Mn1 O1 C39 7.4(4) . . . . ? O7 Mn2 O2 C39 143.2(12) . . . . ? O4 Mn2 O2 C39 -8.4(5) 7_565 . . . ? OW1 Mn2 O2 C39 76.9(5) . . . . ? N4 Mn2 O2 C39 -93.9(5) 1_565 . . . ? N1 Mn2 O2 C39 174.5(5) . . . . ? O2 Mn2 O7 C53 -59.1(16) . . . . ? O4 Mn2 O7 C53 92.5(6) 7_565 . . . ? OW1 Mn2 O7 C53 7.2(5) . . . . ? N4 Mn2 O7 C53 177.4(6) 1_565 . . . ? N1 Mn2 O7 C53 -90.3(6) . . . . ? O2 Mn2 OW1 Mn1 -43.00(16) . . . . ? O7 Mn2 OW1 Mn1 143.38(18) . . . . ? O4 Mn2 OW1 Mn1 49.67(16) 7_565 . . . ? N4 Mn2 OW1 Mn1 86.5(8) 1_565 . . . ? N1 Mn2 OW1 Mn1 -128.09(18) . . . . ? O3 Mn1 OW1 Mn2 -70.73(16) 7_565 . . . ? O9 Mn1 OW1 Mn2 108.20(16) 7_566 . . . ? O1 Mn1 OW1 Mn2 25.50(18) . . . . ? N3 Mn1 OW1 Mn2 -172.5(6) . . . . ? O10 Mn1 OW1 Mn2 -158.63(16) 3_645 . . . ? O3 Mn1 N3 C14 -43.8(6) 7_565 . . . ? O9 Mn1 N3 C14 135.5(6) 7_566 . . . ? O1 Mn1 N3 C14 -140.3(6) . . . . ? O10 Mn1 N3 C14 43.1(6) 3_645 . . . ? OW1 Mn1 N3 C14 57.0(10) . . . . ? O3 Mn1 N3 C18 136.9(5) 7_565 . . . ? O9 Mn1 N3 C18 -43.8(5) 7_566 . . . ? O1 Mn1 N3 C18 40.4(5) . . . . ? O10 Mn1 N3 C18 -136.2(5) 3_645 . . . ? OW1 Mn1 N3 C18 -122.3(7) . . . . ? O2 Mn2 N1 C1A -34.8(14) . . . . ? O7 Mn2 N1 C1A 141.6(14) . . . . ? O4 Mn2 N1 C1A -88(3) 7_565 . . . ? OW1 Mn2 N1 C1A 53.9(14) . . . . ? N4 Mn2 N1 C1A -132.7(14) 1_565 . . . ? O2 Mn2 N1 C5 163.5(6) . . . . ? O7 Mn2 N1 C5 -20.1(6) . . . . ? O4 Mn2 N1 C5 110(3) 7_565 . . . ? OW1 Mn2 N1 C5 -107.8(6) . . . . ? N4 Mn2 N1 C5 65.6(6) 1_565 . . . ? O2 Mn2 N1 C1 5.1(7) . . . . ? O7 Mn2 N1 C1 -178.6(7) . . . . ? O4 Mn2 N1 C1 -49(3) 7_565 . . . ? OW1 Mn2 N1 C1 93.8(7) . . . . ? N4 Mn2 N1 C1 -92.9(7) 1_565 . . . ? C1A N1 C1 C2 -84(2) . . . . ? C5 N1 C1 C2 10.5(16) . . . . ? Mn2 N1 C1 C2 170.4(10) . . . . ? N1 C1 C2 C3 5(2) . . . . ? C1 C2 C3 C4 -20(3) . . . . ? C1 C2 C3 C11 176.2(18) . . . . ? C5 N1 C1A C2A -20(2) . . . . ? C1 N1 C1A C2A 81(2) . . . . ? Mn2 N1 C1A C2A 177.1(14) . . . . ? N1 C1A C2A C3A -14(5) . . . . ? C1A C2A C3A C4 38(5) . . . . ? C1A C2A C3A C11A -147(3) . . . . ? C2A C3A C4 C5 -31(4) . . . . ? C11A C3A C4 C5 157(5) . . . . ? C2A C3A C4 C3 6(14) . . . . ? C11A C3A C4 C3 -167(22) . . . . ? C2 C3 C4 C3A -129(18) . . . . ? C11 C3 C4 C3A 38(15) . . . . ? C2 C3 C4 C5 18(3) . . . . ? C11 C3 C4 C5 -175.5(12) . . . . ? C1A N1 C5 C4 23.4(16) . . . . ? C1 N1 C5 C4 -13.5(13) . . . . ? Mn2 N1 C5 C4 -173.0(7) . . . . ? C3A C4 C5 N1 7(3) . . . . ? C3 C4 C5 N1 0.0(18) . . . . ? C10 N2 C6 C7 3.4(18) . . . . ? N2 C6 C7 C8 -1.7(19) . . . . ? C9 C8 C7 C6 -0.2(15) . . . . ? C13 C8 C7 C6 173.0(11) . . . . ? C13A C8 C7 C6 178.0(17) . . . . ? C7 C8 C9 C10 0.1(14) . . . . ? C13 C8 C9 C10 -172.1(11) . . . . ? C13A C8 C9 C10 -178.8(13) . . . . ? C6 N2 C10 C9 -3.6(17) . . . . ? C8 C9 C10 N2 2.0(18) . . . . ? C2 C3 C11 C12 72(3) . . . . ? C4 C3 C11 C12 -93.5(19) . . . . ? C3 C11 C12 C13 -167.2(14) . . . . ? C7 C8 C13 C12 -87.4(16) . . . . ? C9 C8 C13 C12 84.7(17) . . . . ? C13A C8 C13 C12 100(3) . . . . ? C11 C12 C13 C8 -161.6(15) . . . . ? C4 C3A C11A C12A 6(7) . . . . ? C2A C3A C11A C12A -166(3) . . . . ? C3A C11A C12A C13A -170(2) . . . . ? C11A C12A C13A C8 82(4) . . . . ? C7 C8 C13A C12A -83(3) . . . . ? C9 C8 C13A C12A 95(3) . . . . ? C13 C8 C13A C12A -73(3) . . . . ? C18 N3 C14 C15 -3.5(12) . . . . ? Mn1 N3 C14 C15 177.1(7) . . . . ? N3 C14 C15 C16 2.8(15) . . . . ? C14 C15 C16 C17 0.6(13) . . . . ? C14 C15 C16 C24 -179.7(8) . . . . ? C15 C16 C17 C18 -2.8(13) . . . . ? C24 C16 C17 C18 177.5(8) . . . . ? C14 N3 C18 C17 1.1(11) . . . . ? Mn1 N3 C18 C17 -179.5(6) . . . . ? C16 C17 C18 N3 2.0(13) . . . . ? C23 N4 C19 C20 0.1(11) . . . . ? C23A N4 C19 C20 -55(2) . . . . ? C19A N4 C19 C20 60(2) . . . . ? Mn2 N4 C19 C20 -169.8(6) 1_545 . . . ? N4 C19 C20 C21 -1.7(12) . . . . ? C22 C21 C20 C19 3.1(11) . . . . ? C22A C21 C20 C19 62(2) . . . . ? C20A C21 C20 C19 -52.6(19) . . . . ? C26 C21 C20 C19 -177.6(7) . . . . ? C22A C21 C22 C23 -71(2) . . . . ? C20 C21 C22 C23 -3.0(12) . . . . ? C20A C21 C22 C23 66(2) . . . . ? C26 C21 C22 C23 177.7(7) . . . . ? C23A N4 C23 C22 61(2) . . . . ? C19A N4 C23 C22 -69(2) . . . . ? C19 N4 C23 C22 0.1(12) . . . . ? Mn2 N4 C23 C22 169.2(7) 1_545 . . . ? C21 C22 C23 N4 1.4(15) . . . . ? C23 N4 C19A C20A 57.2(13) . . . . ? C23A N4 C19A C20A 8(2) . . . . ? C19 N4 C19A C20A -63.8(13) . . . . ? Mn2 N4 C19A C20A 175.6(12) 1_545 . . . ? N4 C19A C20A C21 13(2) . . . . ? C22 C21 C20A C19A -74(2) . . . . ? C22A C21 C20A C19A -31(4) . . . . ? C20 C21 C20A C19A 49(2) . . . . ? C26 C21 C20A C19A 175.2(14) . . . . ? C22 C21 C22A C23A 67(4) . . . . ? C20 C21 C22A C23A -56(4) . . . . ? C20A C21 C22A C23A 27(5) . . . . ? C26 C21 C22A C23A -180(3) . . . . ? C23 N4 C23A C22A -61(5) . . . . ? C19A N4 C23A C22A -11(5) . . . . ? C19 N4 C23A C22A 64(5) . . . . ? Mn2 N4 C23A C22A 180(4) 1_545 . . . ? C21 C22A C23A N4 -7(7) . . . . ? C17 C16 C24 C25 102.8(10) . . . . ? C15 C16 C24 C25 -77.0(11) . . . . ? C16 C24 C25 C26 172.0(7) . . . . ? C22 C21 C26 C25 -83.8(9) . . . . ? C22A C21 C26 C25 -162(3) . . . . ? C20 C21 C26 C25 96.8(9) . . . . ? C20A C21 C26 C25 -11(2) . . . . ? C24 C25 C26 C21 174.8(7) . . . . ? C32 C27 C28 C29 -1.4(12) . . . . ? C27 C28 C29 C30 5.5(11) . . . . ? C27 C28 C29 C39 -172.5(6) . . . . ? C28 C29 C30 C31 -5.2(9) . . . . ? C39 C29 C30 C31 172.8(5) . . . . ? C29 C30 C31 C32 0.7(9) . . . . ? C30 C31 C32 C27 3.5(9) . . . . ? C30 C31 C32 S1 -172.9(5) . . . . ? C28 C27 C32 C31 -3.2(11) . . . . ? C28 C27 C32 S1 173.3(6) . . . . ? O6 S1 C32 C31 -4.6(6) . . . . ? O5 S1 C32 C31 126.7(5) . . . . ? C33 S1 C32 C31 -118.9(5) . . . . ? O6 S1 C32 C27 178.9(5) . . . . ? O5 S1 C32 C27 -49.8(6) . . . . ? C33 S1 C32 C27 64.6(6) . . . . ? O6 S1 C33 C34 -24.3(6) . . . . ? O5 S1 C33 C34 -155.4(5) . . . . ? C32 S1 C33 C34 90.1(5) . . . . ? O6 S1 C33 C38 155.5(5) . . . . ? O5 S1 C33 C38 24.4(6) . . . . ? C32 S1 C33 C38 -90.1(5) . . . . ? C38 C33 C34 C35 1.2(9) . . . . ? S1 C33 C34 C35 -179.0(5) . . . . ? C33 C34 C35 C36 -0.4(9) . . . . ? C34 C35 C36 C37 -1.5(9) . . . . ? C34 C35 C36 C40 178.1(5) . . . . ? C35 C36 C37 C38 2.8(9) . . . . ? C40 C36 C37 C38 -176.9(5) . . . . ? C34 C33 C38 C37 0.0(9) . . . . ? S1 C33 C38 C37 -179.9(4) . . . . ? C36 C37 C38 C33 -2.0(9) . . . . ? Mn1 O1 C39 O2 -5.3(7) . . . . ? Mn1 O1 C39 C29 177.4(3) . . . . ? Mn2 O2 C39 O1 -49.8(8) . . . . ? Mn2 O2 C39 C29 127.6(5) . . . . ? C28 C29 C39 O1 171.0(6) . . . . ? C30 C29 C39 O1 -7.0(8) . . . . ? C28 C29 C39 O2 -6.6(8) . . . . ? C30 C29 C39 O2 175.5(5) . . . . ? Mn1 O3 C40 O4 -3.3(8) 7_566 . . . ? Mn1 O3 C40 C36 178.0(3) 7_566 . . . ? Mn2 O4 C40 O3 44.6(9) 7_566 . . . ? Mn2 O4 C40 C36 -136.7(5) 7_566 . . . ? C37 C36 C40 O3 -15.4(8) . . . . ? C35 C36 C40 O3 165.0(5) . . . . ? C37 C36 C40 O4 165.8(5) . . . . ? C35 C36 C40 O4 -13.9(8) . . . . ? C46 C41 C42 C43 0.0(9) . . . . ? C41 C42 C43 C44 -0.3(9) . . . . ? C41 C42 C43 C53 -179.3(5) . . . . ? C42 C43 C44 C45 -0.3(9) . . . . ? C53 C43 C44 C45 178.7(6) . . . . ? C43 C44 C45 C46 1.2(10) . . . . ? C42 C41 C46 C45 0.9(9) . . . . ? C42 C41 C46 S2 179.9(5) . . . . ? C44 C45 C46 C41 -1.4(9) . . . . ? C44 C45 C46 S2 179.6(5) . . . . ? O12 S2 C46 C41 40.0(5) . . . . ? O11 S2 C46 C41 170.6(5) . . . . ? C47 S2 C46 C41 -74.9(5) . . . . ? O12 S2 C46 C45 -141.0(5) . . . . ? O11 S2 C46 C45 -10.4(5) . . . . ? C47 S2 C46 C45 104.2(5) . . . . ? O12 S2 C47 C52 145.9(4) . . . . ? O11 S2 C47 C52 15.2(5) . . . . ? C46 S2 C47 C52 -99.8(5) . . . . ? O12 S2 C47 C48 -32.4(5) . . . . ? O11 S2 C47 C48 -163.2(4) . . . . ? C46 S2 C47 C48 81.9(5) . . . . ? C52 C47 C48 C49 1.1(8) . . . . ? S2 C47 C48 C49 179.4(4) . . . . ? C47 C48 C49 C50 0.6(8) . . . . ? C48 C49 C50 C51 -0.3(8) . . . . ? C48 C49 C50 C54 177.5(5) . . . . ? C49 C50 C51 C52 -1.7(8) . . . . ? C54 C50 C51 C52 -179.5(5) . . . . ? C48 C47 C52 C51 -3.1(8) . . . . ? S2 C47 C52 C51 178.7(4) . . . . ? C50 C51 C52 C47 3.3(8) . . . . ? Mn2 O7 C53 O8 -17.6(9) . . . . ? Mn2 O7 C53 C43 159.9(4) . . . . ? C42 C43 C53 O8 0.8(8) . . . . ? C44 C43 C53 O8 -178.2(6) . . . . ? C42 C43 C53 O7 -176.8(5) . . . . ? C44 C43 C53 O7 4.1(8) . . . . ? Mn1 O9 C54 O10 -14.4(7) 7_565 . . . ? Mn1 O9 C54 C50 165.1(3) 7_565 . . . ? Mn1 O10 C54 O9 -84.4(6) 3_655 . . . ? Mn1 O10 C54 C50 96.0(4) 3_655 . . . ? C49 C50 C54 O9 -150.1(5) . . . . ? C51 C50 C54 O9 27.7(7) . . . . ? C49 C50 C54 O10 29.5(7) . . . . ? C51 C50 C54 O10 -152.7(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW1 HW1A O8 0.847(10) 1.80(2) 2.610(5) 159(5) . OW1 HW1A O7 0.847(10) 2.62(5) 3.029(5) 111(4) . OW1 HW1B O10 0.840(10) 1.869(18) 2.680(5) 162(5) 7_566 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.615 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.070 data_c4a _database_code_depnum_ccdc_archive 'CCDC 808839' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 Mn2 N3 O13 S2' _chemical_formula_weight 832.54 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 12.519(3) _cell_length_b 22.829(5) _cell_length_c 11.917(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.89(3) _cell_angle_gamma 90.00 _cell_volume 3275.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6957 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 28.34 _exptl_crystal_description block _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1692 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6686 _exptl_absorpt_correction_T_max 0.7332 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6957 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.34 _reflns_number_total 4035 _reflns_number_gt 3370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4035 _refine_ls_number_parameters 325 _refine_ls_number_restraints 170 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1474 _refine_ls_wR_factor_gt 0.1411 _refine_ls_goodness_of_fit_ref 1.639 _refine_ls_restrained_S_all 1.676 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.74385(7) 0.5000 1.11357(7) 0.0347(3) Uani 1 2 d S . . Mn2 Mn 0.80657(7) 0.5000 1.38151(7) 0.0304(3) Uani 1 2 d S . . S1 S 1.27691(10) 0.76129(6) 1.25056(10) 0.0440(3) Uani 1 1 d . . . O1 O 0.8681(3) 0.56447(18) 1.1657(3) 0.0541(10) Uani 1 1 d . . . OW1 O 0.8572(4) 0.5000 1.5629(3) 0.0374(11) Uani 1 2 d S . . O2 O 0.9225(3) 0.56120(18) 1.3579(3) 0.0528(10) Uani 1 1 d . . . O3 O 1.6376(10) 0.5718(6) 1.1583(10) 0.054(3) Uani 0.514(18) 1 d PDU . 1 O4 O 1.6930(6) 0.5757(4) 1.3502(8) 0.035(3) Uani 0.514(18) 1 d PDU . 1 O3A O 1.6193(8) 0.5565(5) 1.1129(10) 0.038(3) Uani 0.486(18) 1 d PDU . 2 O4A O 1.6697(7) 0.5474(5) 1.3019(9) 0.043(3) Uani 0.486(18) 1 d PDU . 2 O5 O 1.3115(3) 0.7924(2) 1.3593(3) 0.0676(14) Uani 1 1 d . . . O6 O 1.2428(3) 0.79359(17) 1.1445(3) 0.0469(9) Uani 1 1 d . . . C1 C 1.0907(4) 0.6968(3) 1.1534(3) 0.0420(13) Uani 1 1 d . . . H1 H 1.0914 0.7146 1.0834 0.042 Uiso 1 1 calc R . . C2 C 1.0125(4) 0.6557(2) 1.1573(4) 0.0366(11) Uani 1 1 d . . . H2 H 0.9601 0.6450 1.0887 0.037 Uiso 1 1 calc R . . C3 C 1.0098(3) 0.6296(2) 1.2620(4) 0.0348(11) Uani 1 1 d D . . C4 C 1.0854(3) 0.6457(2) 1.3646(4) 0.0336(10) Uani 1 1 d . . . H4 H 1.0834 0.6288 1.4349 0.034 Uiso 1 1 calc R . . C5 C 1.1654(4) 0.6880(2) 1.3613(4) 0.0389(12) Uani 1 1 d . . . H5 H 1.2158 0.7003 1.4300 0.039 Uiso 1 1 calc R . . C6 C 1.1691(3) 0.7112(2) 1.2567(3) 0.0347(12) Uani 1 1 d . . . C7 C 1.3846(3) 0.7153(3) 1.2435(3) 0.0498(17) Uani 1 1 d D . . C8 C 1.4671(10) 0.7127(6) 1.3486(9) 0.022(3) Uani 0.45(2) 1 d PDU . 1 H8A H 1.4668 0.7359 1.4127 0.027 Uiso 0.45(2) 1 calc PR . 1 C9 C 1.5498(10) 0.6724(6) 1.3490(10) 0.025(3) Uani 0.45(2) 1 d PDU . 1 H9A H 1.6064 0.6663 1.4171 0.030 Uiso 0.45(2) 1 calc PR . 1 C10 C 1.5496(8) 0.6407(6) 1.2493(9) 0.019(3) Uani 0.45(2) 1 d PDU . 1 C11 C 1.4733(9) 0.6534(7) 1.1445(10) 0.028(3) Uani 0.45(2) 1 d PDU . 1 H11A H 1.4884 0.6415 1.0757 0.033 Uiso 0.45(2) 1 calc PR . 1 C8A C 1.4703(10) 0.6916(7) 1.3328(10) 0.039(3) Uani 0.55(2) 1 d PDU . 2 H8AA H 1.4772 0.7062 1.4073 0.047 Uiso 0.55(2) 1 calc PR . 2 C9A C 1.5467(9) 0.6485(7) 1.3240(11) 0.040(3) Uani 0.55(2) 1 d PDU . 2 H9AA H 1.6073 0.6405 1.3873 0.049 Uiso 0.55(2) 1 calc PR . 2 C10A C 1.5321(9) 0.6177(6) 1.2208(10) 0.034(3) Uani 0.55(2) 1 d PDU . 2 C11A C 1.4447(9) 0.6355(5) 1.1273(9) 0.032(3) Uani 0.55(2) 1 d PDU . 2 H11B H 1.4313 0.6156 1.0567 0.038 Uiso 0.55(2) 1 calc PR . 2 C12 C 1.3765(4) 0.6828(3) 1.1373(4) 0.0489(15) Uani 1 1 d D . . H12A H 1.3142 0.6821 1.0732 0.049 Uiso 0.45(2) 1 calc PR . 1 H12B H 1.3220 0.6942 1.0707 0.049 Uiso 0.55(2) 1 calc PR . 2 C13 C 0.9265(3) 0.5817(2) 1.2607(4) 0.0386(11) Uani 1 1 d D . . C14 C 1.6357(9) 0.5934(6) 1.2532(8) 0.032(3) Uani 0.48(2) 1 d PDU . 1 C14A C 1.6123(9) 0.5698(6) 1.2110(9) 0.042(4) Uani 0.52(2) 1 d PDU . 2 N1 N 0.7288(4) 0.5000 0.9285(4) 0.0493(18) Uani 1 2 d SDU . . N2 N 0.6638(5) 0.5000 0.7438(4) 0.072(3) Uani 1 2 d SDU . . N3 N 0.7711(5) 0.5000 0.7599(5) 0.076(3) Uani 1 2 d SDU . . C15 C 0.8044(7) 0.5163(5) 0.8716(6) 0.055(3) Uani 0.50 1 d PDU . . C16 C 0.6374(6) 0.5000 0.8449(5) 0.063(2) Uani 1 2 d SDU . . H16A H 0.5659 0.5000 0.8538 0.075 Uiso 1 2 calc SR . . C17 C 0.6064(8) 0.5359(4) 0.6355(6) 0.050(3) Uani 0.50 1 d PD . . C18 C 0.5390(6) 0.4879(4) 0.5567(5) 0.048(3) Uani 0.50 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0271(5) 0.0589(8) 0.0190(4) 0.000 0.0076(3) 0.000 Mn2 0.0256(5) 0.0452(7) 0.0219(4) 0.000 0.0089(3) 0.000 S1 0.0345(6) 0.0657(9) 0.0347(5) -0.0050(7) 0.0143(4) -0.0211(7) O1 0.0409(18) 0.057(3) 0.058(2) -0.017(2) 0.0031(16) -0.010(2) OW1 0.044(2) 0.045(3) 0.027(2) 0.000 0.0152(18) 0.000 O2 0.056(2) 0.037(2) 0.055(2) 0.0103(18) -0.0020(16) -0.0166(19) O3 0.048(5) 0.061(6) 0.054(6) -0.021(5) 0.013(4) 0.006(5) O4 0.033(3) 0.024(5) 0.044(4) 0.004(4) 0.003(3) 0.012(3) O3A 0.027(4) 0.032(5) 0.056(6) 0.004(4) 0.016(4) 0.004(4) O4A 0.043(4) 0.036(6) 0.045(5) -0.002(4) 0.004(3) 0.007(4) O5 0.064(2) 0.091(4) 0.053(2) -0.030(2) 0.0244(18) -0.047(3) O6 0.049(2) 0.043(2) 0.0512(19) 0.0053(18) 0.0191(15) -0.0048(18) C1 0.031(2) 0.070(4) 0.025(2) -0.005(2) 0.0076(17) -0.006(3) C2 0.038(2) 0.038(3) 0.029(2) -0.003(2) 0.0013(17) -0.005(2) C3 0.031(2) 0.037(3) 0.038(2) -0.002(2) 0.0118(18) 0.004(2) C4 0.030(2) 0.038(3) 0.034(2) 0.002(2) 0.0116(17) 0.001(2) C5 0.040(2) 0.047(3) 0.030(2) -0.007(2) 0.0103(18) -0.005(2) C6 0.024(2) 0.050(3) 0.031(2) -0.007(2) 0.0085(16) 0.007(2) C7 0.028(2) 0.100(5) 0.026(2) 0.014(3) 0.0158(18) 0.011(3) C8 0.022(5) 0.023(6) 0.022(5) -0.003(4) 0.004(4) 0.001(4) C9 0.023(5) 0.022(6) 0.027(5) -0.014(4) 0.003(4) 0.001(5) C10 0.013(4) 0.027(6) 0.017(5) 0.001(5) 0.002(3) -0.004(4) C11 0.020(4) 0.032(5) 0.034(4) -0.004(4) 0.011(4) -0.011(4) C8A 0.037(5) 0.050(8) 0.030(4) -0.011(5) 0.011(4) 0.008(5) C9A 0.030(4) 0.047(7) 0.039(6) 0.001(6) 0.001(4) -0.003(5) C10A 0.028(5) 0.037(6) 0.035(5) -0.005(5) 0.008(4) 0.008(4) C11A 0.019(4) 0.038(6) 0.037(4) 0.014(4) 0.005(3) -0.009(4) C12 0.039(3) 0.073(4) 0.036(2) 0.021(3) 0.0134(19) 0.031(3) C13 0.027(2) 0.027(3) 0.058(3) -0.008(2) 0.005(2) 0.014(2) C14 0.027(4) 0.033(5) 0.036(5) -0.005(4) 0.005(3) 0.017(4) C14A 0.038(5) 0.046(7) 0.042(7) -0.005(6) 0.008(5) -0.005(5) N1 0.030(3) 0.093(6) 0.025(2) 0.000 0.008(2) 0.000 N2 0.048(3) 0.137(8) 0.030(3) 0.000 0.010(2) 0.000 N3 0.043(3) 0.160(8) 0.029(3) 0.000 0.018(3) 0.000 C15 0.055(4) 0.066(9) 0.048(4) 0.002(4) 0.020(3) -0.022(5) C16 0.047(4) 0.115(7) 0.025(3) 0.000 0.008(3) 0.000 C17 0.073(7) 0.041(7) 0.024(4) 0.016(4) -0.005(4) 0.018(6) C18 0.054(4) 0.053(9) 0.036(4) 0.013(4) 0.009(3) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O3A 2.022(10) 1_455 ? Mn1 O3A 2.022(10) 6_465 ? Mn1 O1 2.108(4) . ? Mn1 O1 2.108(4) 6_565 ? Mn1 N1 2.161(5) . ? Mn1 O3 2.264(11) 1_455 ? Mn1 O3 2.264(11) 6_465 ? Mn1 Mn2 3.0724(13) . ? Mn2 O4A 2.029(7) 6_465 ? Mn2 O4A 2.029(7) 1_455 ? Mn2 OW1 2.080(4) . ? Mn2 O2 2.088(4) . ? Mn2 O2 2.088(4) 6_565 ? Mn2 O4 2.203(7) 1_455 ? Mn2 O4 2.203(7) 6_465 ? S1 O6 1.424(4) . ? S1 O5 1.436(4) . ? S1 C7 1.729(5) . ? S1 C6 1.785(5) . ? O1 C13 1.232(6) . ? O2 C13 1.262(6) . ? O3 C14 1.240(9) . ? O3 Mn1 2.264(11) 1_655 ? O4 C14 1.250(8) . ? O4 Mn2 2.203(7) 1_655 ? O3A C14A 1.234(9) . ? O3A Mn1 2.022(10) 1_655 ? O4A C14A 1.235(8) . ? O4A Mn2 2.029(7) 1_655 ? C1 C2 1.365(7) . ? C1 C6 1.388(6) . ? C1 H1 0.9300 . ? C2 C3 1.391(6) . ? C2 H2 0.9300 . ? C3 C4 1.375(6) . ? C3 C13 1.510(6) . ? C4 C5 1.399(7) . ? C4 H4 0.9300 . ? C5 C6 1.366(6) . ? C5 H5 0.9300 . ? C7 C8 1.389(8) . ? C7 C8A 1.397(8) . ? C7 C12 1.447(7) . ? C8 C9 1.385(9) . ? C8 H8A 0.9300 . ? C9 C10 1.390(8) . ? C9 H9A 0.9300 . ? C10 C11 1.380(9) . ? C10 C14 1.517(9) . ? C11 C12 1.368(8) . ? C11 H11A 0.9300 . ? C8A C9A 1.395(9) . ? C8A H8AA 0.9300 . ? C9A C10A 1.386(8) . ? C9A H9AA 0.9300 . ? C10A C11A 1.391(8) . ? C10A C14A 1.510(9) . ? C11A C12 1.403(8) . ? C11A H11B 0.9300 . ? C12 H12A 0.9300 . ? C12 H12B 0.9300 . ? N1 C16 1.296(7) . ? N1 C15 1.358(7) . ? N1 C15 1.358(7) 6_565 ? N2 N3 1.303(7) . ? N2 C16 1.334(6) . ? N2 C17 1.532(7) 6_565 ? N2 C17 1.532(7) . ? N3 C15 1.334(7) . ? N3 C15 1.334(7) 6_565 ? C15 C15 0.74(2) 6_565 ? C16 H16A 0.9300 . ? C17 C18 1.206(10) 6_565 ? C17 C18 1.535(9) . ? C17 C17 1.637(18) 6_565 ? C18 C18 0.55(2) 6_565 ? C18 C17 1.206(10) 6_565 ? C18 C18 1.434(10) 2_656 ? C18 C18 1.536(9) 5_666 ? 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 O3A Mn1 O3A 79.3(6) 1_455 6_465 ? O3A Mn1 O1 93.5(3) 1_455 . ? O3A Mn1 O1 162.3(3) 6_465 . ? O3A Mn1 O1 162.3(3) 1_455 6_565 ? O3A Mn1 O1 93.5(3) 6_465 6_565 ? O1 Mn1 O1 88.6(2) . 6_565 ? O3A Mn1 N1 98.3(3) 1_455 . ? O3A Mn1 N1 98.3(3) 6_465 . ? O1 Mn1 N1 98.72(14) . . ? O1 Mn1 N1 98.72(14) 6_565 . ? O3A Mn1 O3 15.7(3) 1_455 1_455 ? O3A Mn1 O3 87.7(3) 6_465 1_455 ? O1 Mn1 O3 81.9(4) . 1_455 ? O1 Mn1 O3 150.4(3) 6_565 1_455 ? N1 Mn1 O3 110.3(3) . 1_455 ? O3A Mn1 O3 87.7(3) 1_455 6_465 ? O3A Mn1 O3 15.7(3) 6_465 6_465 ? O1 Mn1 O3 150.4(3) . 6_465 ? O1 Mn1 O3 81.9(4) 6_565 6_465 ? N1 Mn1 O3 110.3(3) . 6_465 ? O3 Mn1 O3 92.7(7) 1_455 6_465 ? O3A Mn1 Mn2 88.9(3) 1_455 . ? O3A Mn1 Mn2 88.9(3) 6_465 . ? O1 Mn1 Mn2 74.68(10) . . ? O1 Mn1 Mn2 74.68(10) 6_565 . ? N1 Mn1 Mn2 170.57(14) . . ? O3 Mn1 Mn2 75.8(3) 1_455 . ? O3 Mn1 Mn2 75.8(3) 6_465 . ? O4A Mn2 O4A 64.5(7) 6_465 1_455 ? O4A Mn2 OW1 117.7(3) 6_465 . ? O4A Mn2 OW1 117.7(3) 1_455 . ? O4A Mn2 O2 145.4(4) 6_465 . ? O4A Mn2 O2 96.3(3) 1_455 . ? OW1 Mn2 O2 96.59(14) . . ? O4A Mn2 O2 96.3(3) 6_465 6_565 ? O4A Mn2 O2 145.4(4) 1_455 6_565 ? OW1 Mn2 O2 96.59(13) . 6_565 ? O2 Mn2 O2 84.0(2) . 6_565 ? O4A Mn2 O4 85.2(6) 6_465 1_455 ? O4A Mn2 O4 23.0(2) 1_455 1_455 ? OW1 Mn2 O4 100.1(3) . 1_455 ? O2 Mn2 O4 83.8(2) . 1_455 ? O2 Mn2 O4 160.4(2) 6_565 1_455 ? O4A Mn2 O4 23.0(2) 6_465 6_465 ? O4A Mn2 O4 85.2(6) 1_455 6_465 ? OW1 Mn2 O4 100.1(3) . 6_465 ? O2 Mn2 O4 160.4(2) . 6_465 ? O2 Mn2 O4 83.8(2) 6_565 6_465 ? O4 Mn2 O4 103.3(5) 1_455 6_465 ? O4A Mn2 Mn1 64.6(3) 6_465 . ? O4A Mn2 Mn1 64.6(3) 1_455 . ? OW1 Mn2 Mn1 177.17(12) . . ? O2 Mn2 Mn1 81.33(10) . . ? O2 Mn2 Mn1 81.33(10) 6_565 . ? O4 Mn2 Mn1 81.6(2) 1_455 . ? O4 Mn2 Mn1 81.6(2) 6_465 . ? O6 S1 O5 119.2(3) . . ? O6 S1 C7 108.6(2) . . ? O5 S1 C7 107.3(2) . . ? O6 S1 C6 108.8(2) . . ? O5 S1 C6 108.9(2) . . ? C7 S1 C6 102.8(2) . . ? C13 O1 Mn1 134.2(4) . . ? C13 O2 Mn2 125.1(3) . . ? C14 O3 Mn1 131.5(9) . 1_655 ? C14 O4 Mn2 126.2(7) . 1_655 ? C14A O3A Mn1 114.0(8) . 1_655 ? C14A O4A Mn2 147.7(7) . 1_655 ? C2 C1 C6 118.2(4) . . ? C2 C1 H1 120.9 . . ? C6 C1 H1 120.9 . . ? C1 C2 C3 121.2(4) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 120.2(4) . . ? C4 C3 C13 120.5(4) . . ? C2 C3 C13 119.2(4) . . ? C3 C4 C5 118.9(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 119.8(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 121.6(5) . . ? C5 C6 S1 120.1(3) . . ? C1 C6 S1 118.3(4) . . ? C8 C7 C8A 21.7(6) . . ? C8 C7 C12 128.6(7) . . ? C8A C7 C12 108.8(7) . . ? C8 C7 S1 112.3(7) . . ? C8A C7 S1 130.2(6) . . ? C12 C7 S1 119.0(3) . . ? C9 C8 C7 113.7(10) . . ? C9 C8 H8A 123.2 . . ? C7 C8 H8A 123.2 . . ? C10 C9 C8 121.1(10) . . ? C10 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? C11 C10 C9 120.2(9) . . ? C11 C10 C14 119.1(9) . . ? C9 C10 C14 120.6(9) . . ? C10 C11 C12 122.8(9) . . ? C10 C11 H11A 118.6 . . ? C12 C11 H11A 118.6 . . ? C7 C8A C9A 128.0(10) . . ? C7 C8A H8AA 116.0 . . ? C9A C8A H8AA 116.0 . . ? C10A C9A C8A 119.9(9) . . ? C10A C9A H9AA 120.1 . . ? C8A C9A H9AA 120.1 . . ? C9A C10A C11A 116.5(9) . . ? C9A C10A C14A 120.5(9) . . ? C11A C10A C14A 122.9(9) . . ? C10A C11A C12 121.4(9) . . ? C10A C11A H11B 119.3 . . ? C12 C11A H11B 119.3 . . ? C11 C12 C11A 22.7(5) . . ? C11 C12 C7 110.4(7) . . ? C11A C12 C7 124.8(6) . . ? C11 C12 H12A 124.8 . . ? C11A C12 H12A 108.0 . . ? C7 C12 H12A 124.8 . . ? C11 C12 H12B 128.3 . . ? C11A C12 H12B 117.6 . . ? C7 C12 H12B 117.6 . . ? H12A C12 H12B 18.4 . . ? O1 C13 O2 124.3(5) . . ? O1 C13 C3 118.3(5) . . ? O2 C13 C3 117.4(4) . . ? O3 C14 O4 124.4(9) . . ? O3 C14 C10 116.5(9) . . ? O4 C14 C10 118.8(7) . . ? O4A C14A O3A 123.6(10) . . ? O4A C14A C10A 118.2(8) . . ? O3A C14A C10A 118.1(9) . . ? C16 N1 C15 101.8(6) . . ? C16 N1 C15 101.8(6) . 6_565 ? C15 N1 C15 31.8(10) . 6_565 ? C16 N1 Mn1 126.6(4) . . ? C15 N1 Mn1 129.2(5) . . ? C15 N1 Mn1 129.2(5) 6_565 . ? N3 N2 C16 111.6(5) . . ? N3 N2 C17 110.5(5) . 6_565 ? C16 N2 C17 125.9(6) . 6_565 ? N3 N2 C17 110.5(5) . . ? C16 N2 C17 125.9(5) . . ? C17 N2 C17 64.6(7) 6_565 . ? N2 N3 C15 100.1(5) . . ? N2 N3 C15 100.1(5) . 6_565 ? C15 N3 C15 32.4(10) . 6_565 ? C15 C15 N3 73.8(5) 6_565 . ? C15 C15 N1 74.1(5) 6_565 . ? N3 C15 N1 110.6(7) . . ? N1 C16 N2 108.0(6) . . ? N1 C16 H16A 126.0 . . ? N2 C16 H16A 126.0 . . ? C18 C17 N2 118.8(10) 6_565 . ? C18 C17 C18 18.7(8) 6_565 . ? N2 C17 C18 100.8(5) . . ? C18 C17 C17 63.2(7) 6_565 6_565 ? N2 C17 C17 57.7(4) . 6_565 ? C18 C17 C17 44.5(4) . 6_565 ? C18 C18 C17 116.8(7) 6_565 6_565 ? C18 C18 C18 90.000(2) 6_565 2_656 ? C17 C18 C18 152.1(7) 6_565 2_656 ? C18 C18 C18 69.0(8) 6_565 5_666 ? C17 C18 C18 170.6(13) 6_565 5_666 ? C18 C18 C18 21.0(8) 2_656 5_666 ? C18 C18 C17 44.5(4) 6_565 . ? C17 C18 C17 72.2(8) 6_565 . ? C18 C18 C17 134.0(4) 2_656 . ? C18 C18 C17 113.1(10) 5_666 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3A Mn1 Mn2 O4A 75.8(5) 1_455 . . 6_465 ? O3A Mn1 Mn2 O4A -3.5(4) 6_465 . . 6_465 ? O1 Mn1 Mn2 O4A 169.8(4) . . . 6_465 ? O1 Mn1 Mn2 O4A -97.4(4) 6_565 . . 6_465 ? N1 Mn1 Mn2 O4A -143.8(4) . . . 6_465 ? O3 Mn1 Mn2 O4A 84.5(6) 1_455 . . 6_465 ? O3 Mn1 Mn2 O4A -12.1(4) 6_465 . . 6_465 ? O3A Mn1 Mn2 O4A 3.5(4) 1_455 . . 1_455 ? O3A Mn1 Mn2 O4A -75.8(5) 6_465 . . 1_455 ? O1 Mn1 Mn2 O4A 97.4(4) . . . 1_455 ? O1 Mn1 Mn2 O4A -169.8(4) 6_565 . . 1_455 ? N1 Mn1 Mn2 O4A 143.8(4) . . . 1_455 ? O3 Mn1 Mn2 O4A 12.1(4) 1_455 . . 1_455 ? O3 Mn1 Mn2 O4A -84.5(6) 6_465 . . 1_455 ? O3A Mn1 Mn2 OW1 -140.3(3) 1_455 . . . ? O3A Mn1 Mn2 OW1 140.3(3) 6_465 . . . ? O1 Mn1 Mn2 OW1 -46.38(11) . . . . ? O1 Mn1 Mn2 OW1 46.38(11) 6_565 . . . ? N1 Mn1 Mn2 OW1 0.000(17) . . . . ? O3 Mn1 Mn2 OW1 -131.7(4) 1_455 . . . ? O3 Mn1 Mn2 OW1 131.7(4) 6_465 . . . ? O3A Mn1 Mn2 O2 -97.7(3) 1_455 . . . ? O3A Mn1 Mn2 O2 -177.1(3) 6_465 . . . ? O1 Mn1 Mn2 O2 -3.78(15) . . . . ? O1 Mn1 Mn2 O2 88.98(16) 6_565 . . . ? N1 Mn1 Mn2 O2 42.60(11) . . . . ? O3 Mn1 Mn2 O2 -89.1(4) 1_455 . . . ? O3 Mn1 Mn2 O2 174.3(4) 6_465 . . . ? O3A Mn1 Mn2 O2 177.1(3) 1_455 . . 6_565 ? O3A Mn1 Mn2 O2 97.7(3) 6_465 . . 6_565 ? O1 Mn1 Mn2 O2 -88.98(16) . . . 6_565 ? O1 Mn1 Mn2 O2 3.78(15) 6_565 . . 6_565 ? N1 Mn1 Mn2 O2 -42.60(11) . . . 6_565 ? O3 Mn1 Mn2 O2 -174.3(4) 1_455 . . 6_565 ? O3 Mn1 Mn2 O2 89.1(4) 6_465 . . 6_565 ? O3A Mn1 Mn2 O4 -12.8(3) 1_455 . . 1_455 ? O3A Mn1 Mn2 O4 -92.1(4) 6_465 . . 1_455 ? O1 Mn1 Mn2 O4 81.2(3) . . . 1_455 ? O1 Mn1 Mn2 O4 174.0(3) 6_565 . . 1_455 ? N1 Mn1 Mn2 O4 127.6(2) . . . 1_455 ? O3 Mn1 Mn2 O4 -4.1(4) 1_455 . . 1_455 ? O3 Mn1 Mn2 O4 -100.7(5) 6_465 . . 1_455 ? O3A Mn1 Mn2 O4 92.1(4) 1_455 . . 6_465 ? O3A Mn1 Mn2 O4 12.8(3) 6_465 . . 6_465 ? O1 Mn1 Mn2 O4 -174.0(3) . . . 6_465 ? O1 Mn1 Mn2 O4 -81.2(3) 6_565 . . 6_465 ? N1 Mn1 Mn2 O4 -127.6(2) . . . 6_465 ? O3 Mn1 Mn2 O4 100.7(5) 1_455 . . 6_465 ? O3 Mn1 Mn2 O4 4.1(4) 6_465 . . 6_465 ? O3A Mn1 O1 C13 91.6(6) 1_455 . . . ? O3A Mn1 O1 C13 26.3(13) 6_465 . . . ? O1 Mn1 O1 C13 -70.9(5) 6_565 . . . ? N1 Mn1 O1 C13 -169.5(5) . . . . ? O3 Mn1 O1 C13 81.0(6) 1_455 . . . ? O3 Mn1 O1 C13 -0.1(9) 6_465 . . . ? Mn2 Mn1 O1 C13 3.6(5) . . . . ? O4A Mn2 O2 C13 -3.7(7) 6_465 . . . ? O4A Mn2 O2 C13 -56.5(5) 1_455 . . . ? OW1 Mn2 O2 C13 -175.4(4) . . . . ? O2 Mn2 O2 C13 88.6(4) 6_565 . . . ? O4 Mn2 O2 C13 -75.9(5) 1_455 . . . ? O4 Mn2 O2 C13 36.7(11) 6_465 . . . ? Mn1 Mn2 O2 C13 6.5(4) . . . . ? C6 C1 C2 C3 1.1(8) . . . . ? C1 C2 C3 C4 1.2(8) . . . . ? C1 C2 C3 C13 -176.1(5) . . . . ? C2 C3 C4 C5 -0.8(7) . . . . ? C13 C3 C4 C5 176.4(4) . . . . ? C3 C4 C5 C6 -1.9(7) . . . . ? C4 C5 C6 C1 4.2(8) . . . . ? C4 C5 C6 S1 -175.5(4) . . . . ? C2 C1 C6 C5 -3.8(8) . . . . ? C2 C1 C6 S1 175.9(4) . . . . ? O6 S1 C6 C5 -160.5(4) . . . . ? O5 S1 C6 C5 -29.1(5) . . . . ? C7 S1 C6 C5 84.5(4) . . . . ? O6 S1 C6 C1 19.8(5) . . . . ? O5 S1 C6 C1 151.2(4) . . . . ? C7 S1 C6 C1 -95.2(4) . . . . ? O6 S1 C7 C8 139.7(8) . . . . ? O5 S1 C7 C8 9.6(8) . . . . ? C6 S1 C7 C8 -105.1(8) . . . . ? O6 S1 C7 C8A 154.2(11) . . . . ? O5 S1 C7 C8A 24.1(11) . . . . ? C6 S1 C7 C8A -90.6(11) . . . . ? O6 S1 C7 C12 -43.8(5) . . . . ? O5 S1 C7 C12 -173.9(4) . . . . ? C6 S1 C7 C12 71.4(5) . . . . ? C8A C7 C8 C9 26(2) . . . . ? C12 C7 C8 C9 -1.4(17) . . . . ? S1 C7 C8 C9 174.6(10) . . . . ? C7 C8 C9 C10 3.2(19) . . . . ? C8 C9 C10 C11 6.9(19) . . . . ? C8 C9 C10 C14 -175.5(13) . . . . ? C9 C10 C11 C12 -20.5(19) . . . . ? C14 C10 C11 C12 161.8(13) . . . . ? C8 C7 C8A C9A -151(4) . . . . ? C12 C7 C8A C9A 7.2(18) . . . . ? S1 C7 C8A C9A 170.6(10) . . . . ? C7 C8A C9A C10A -10(2) . . . . ? C8A C9A C10A C11A 5.1(16) . . . . ? C8A C9A C10A C14A -178.3(12) . . . . ? C9A C10A C11A C12 1.0(15) . . . . ? C14A C10A C11A C12 -175.5(11) . . . . ? C10 C11 C12 C11A -113(2) . . . . ? C10 C11 C12 C7 20.4(15) . . . . ? C10A C11A C12 C11 52.1(18) . . . . ? C10A C11A C12 C7 -3.5(14) . . . . ? C8 C7 C12 C11 -9.9(13) . . . . ? C8A C7 C12 C11 -20.1(11) . . . . ? S1 C7 C12 C11 174.3(8) . . . . ? C8 C7 C12 C11A 10.0(13) . . . . ? C8A C7 C12 C11A -0.3(11) . . . . ? S1 C7 C12 C11A -165.8(7) . . . . ? Mn1 O1 C13 O2 0.1(8) . . . . ? Mn1 O1 C13 C3 179.0(3) . . . . ? Mn2 O2 C13 O1 -6.5(7) . . . . ? Mn2 O2 C13 C3 174.6(3) . . . . ? C4 C3 C13 O1 -172.6(5) . . . . ? C2 C3 C13 O1 4.7(7) . . . . ? C4 C3 C13 O2 6.4(7) . . . . ? C2 C3 C13 O2 -176.3(4) . . . . ? Mn1 O3 C14 O4 -4.7(19) 1_655 . . . ? Mn1 O3 C14 C10 -178.5(10) 1_655 . . . ? Mn2 O4 C14 O3 -2.7(17) 1_655 . . . ? Mn2 O4 C14 C10 171.1(8) 1_655 . . . ? C11 C10 C14 O3 5.4(16) . . . . ? C9 C10 C14 O3 -172.3(12) . . . . ? C11 C10 C14 O4 -168.9(11) . . . . ? C9 C10 C14 O4 13.5(17) . . . . ? Mn2 O4A C14A O3A 17(3) 1_655 . . . ? Mn2 O4A C14A C10A -161.0(14) 1_655 . . . ? Mn1 O3A C14A O4A -5.5(16) 1_655 . . . ? Mn1 O3A C14A C10A 172.1(9) 1_655 . . . ? C9A C10A C14A O4A 20.5(17) . . . . ? C11A C10A C14A O4A -163.1(11) . . . . ? C9A C10A C14A O3A -157.2(11) . . . . ? C11A C10A C14A O3A 19.2(17) . . . . ? O3A Mn1 N1 C16 -40.2(3) 1_455 . . . ? O3A Mn1 N1 C16 40.2(3) 6_465 . . . ? O1 Mn1 N1 C16 -135.06(11) . . . . ? O1 Mn1 N1 C16 135.06(11) 6_565 . . . ? O3 Mn1 N1 C16 -50.5(4) 1_455 . . . ? O3 Mn1 N1 C16 50.5(4) 6_465 . . . ? Mn2 Mn1 N1 C16 180.000(4) . . . . ? O3A Mn1 N1 C15 119.2(7) 1_455 . . . ? O3A Mn1 N1 C15 -160.5(7) 6_465 . . . ? O1 Mn1 N1 C15 24.3(7) . . . . ? O1 Mn1 N1 C15 -65.6(7) 6_565 . . . ? O3 Mn1 N1 C15 108.8(7) 1_455 . . . ? O3 Mn1 N1 C15 -150.2(7) 6_465 . . . ? Mn2 Mn1 N1 C15 -20.7(6) . . . . ? O3A Mn1 N1 C15 160.5(7) 1_455 . . 6_565 ? O3A Mn1 N1 C15 -119.2(7) 6_465 . . 6_565 ? O1 Mn1 N1 C15 65.6(7) . . . 6_565 ? O1 Mn1 N1 C15 -24.3(7) 6_565 . . 6_565 ? O3 Mn1 N1 C15 150.2(7) 1_455 . . 6_565 ? O3 Mn1 N1 C15 -108.8(8) 6_465 . . 6_565 ? Mn2 Mn1 N1 C15 20.7(7) . . . 6_565 ? C16 N2 N3 C15 -16.5(5) . . . . ? C17 N2 N3 C15 -161.6(6) 6_565 . . . ? C17 N2 N3 C15 128.7(7) . . . . ? C16 N2 N3 C15 16.5(5) . . . 6_565 ? C17 N2 N3 C15 -128.7(7) 6_565 . . 6_565 ? C17 N2 N3 C15 161.6(6) . . . 6_565 ? N2 N3 C15 C15 92.96(17) . . . 6_565 ? N2 N3 C15 N1 27.4(8) . . . . ? C15 N3 C15 N1 -65.6(8) 6_565 . . . ? C16 N1 C15 C15 -93.42(18) . . . 6_565 ? Mn1 N1 C15 C15 103.4(5) . . . 6_565 ? C16 N1 C15 N3 -28.1(8) . . . . ? C15 N1 C15 N3 65.4(8) 6_565 . . . ? Mn1 N1 C15 N3 168.8(4) . . . . ? C15 N1 C16 N2 16.2(5) . . . . ? C15 N1 C16 N2 -16.2(5) 6_565 . . . ? Mn1 N1 C16 N2 180.000(2) . . . . ? N3 N2 C16 N1 0.000(2) . . . . ? C17 N2 C16 N1 138.7(5) 6_565 . . . ? C17 N2 C16 N1 -138.7(5) . . . . ? N3 N2 C17 C18 120.7(9) . . . 6_565 ? C16 N2 C17 C18 -100.2(10) . . . 6_565 ? C17 N2 C17 C18 17.0(12) 6_565 . . 6_565 ? N3 N2 C17 C18 115.5(6) . . . . ? C16 N2 C17 C18 -105.4(7) . . . . ? C17 N2 C17 C18 11.8(8) 6_565 . . . ? N3 N2 C17 C17 103.7(4) . . . 6_565 ? C16 N2 C17 C17 -117.2(6) . . . 6_565 ? N2 C17 C18 C18 165.7(10) . . . 6_565 ? C17 C17 C18 C18 180.000(8) 6_565 . . 6_565 ? C18 C17 C18 C17 180.000(7) 6_565 . . 6_565 ? N2 C17 C18 C17 -14.3(10) . . . 6_565 ? C18 C17 C18 C18 11.3(18) 6_565 . . 2_656 ? N2 C17 C18 C18 177.0(12) . . . 2_656 ? C17 C17 C18 C18 -168.7(18) 6_565 . . 2_656 ? C18 C17 C18 C18 8.2(13) 6_565 . . 5_666 ? N2 C17 C18 C18 173.9(8) . . . 5_666 ? C17 C17 C18 C18 -171.8(13) 6_565 . . 5_666 ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.374 _refine_diff_density_min -1.132 _refine_diff_density_rms 0.094 data_c1a _database_code_depnum_ccdc_archive 'CCDC 808840' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H58 Mn4 N4 O30 S4' _chemical_formula_weight 1735.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.401(3) _cell_length_b 12.606(3) _cell_length_c 13.664(3) _cell_angle_alpha 70.84(3) _cell_angle_beta 69.99(3) _cell_angle_gamma 62.04(3) _cell_volume 1736.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10629 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 886 _exptl_absorpt_coefficient_mu 0.925 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6919 _exptl_absorpt_correction_T_max 0.7500 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10629 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7397 _reflns_number_gt 6437 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+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 7397 _refine_ls_number_parameters 511 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.90797(3) 0.10254(3) 0.14070(2) 0.02084(10) Uani 1 1 d . . . Mn2 Mn 0.81207(3) 0.02948(3) 0.42879(2) 0.02351(10) Uani 1 1 d . . . S1 S 1.67019(5) -0.43706(5) 0.17526(5) 0.02815(14) Uani 1 1 d . . . S2 S 0.10718(5) 0.58974(5) 0.26443(4) 0.02262(13) Uani 1 1 d . . . OW1 O 0.93030(17) 0.27595(15) 0.04543(13) 0.0345(4) Uani 1 1 d D . . O1 O 1.10400(14) -0.00748(15) 0.12016(14) 0.0349(4) Uani 1 1 d . . . OW2 O 1.00083(17) -0.11383(16) 0.41041(15) 0.0402(4) Uani 1 1 d D . . O2 O 1.14213(16) -0.10071(18) -0.00809(14) 0.0452(5) Uani 1 1 d . . . OW3 O 0.5996(3) 0.3697(3) 0.5111(2) 0.0743(7) Uani 1 1 d DU . . O3 O 1.87794(18) -0.05817(16) 0.22942(15) 0.0428(4) Uani 1 1 d . . . O4 O 1.75450(19) -0.08209(19) 0.38808(15) 0.0470(5) Uani 1 1 d . . . O5 O 1.65635(17) -0.52768(15) 0.26946(15) 0.0420(4) Uani 1 1 d . . . O6 O 1.75699(15) -0.47588(16) 0.07912(15) 0.0408(4) Uani 1 1 d . . . O7 O 0.66090(15) 0.18693(16) 0.37664(13) 0.0364(4) Uani 1 1 d . . . O8 O 0.71105(15) 0.21031(17) 0.19924(14) 0.0404(4) Uani 1 1 d . . . O9 O -0.06568(16) 0.15402(15) 0.26977(13) 0.0356(4) Uani 1 1 d . . . O10 O -0.11961(16) 0.15548(15) 0.44118(12) 0.0328(4) Uani 1 1 d . . . O11 O 0.10786(15) 0.66321(15) 0.15884(13) 0.0337(4) Uani 1 1 d . . . O12 O 0.04791(14) 0.64959(14) 0.35401(13) 0.0300(3) Uani 1 1 d . . . N1 N 0.7220(2) -0.0170(2) 0.59766(15) 0.0376(5) Uani 1 1 d . . . N2 N 0.6514(2) -0.0536(2) 0.77163(15) 0.0360(5) Uani 1 1 d . . . C1 C 1.5110(2) -0.3073(2) 0.03930(17) 0.0261(4) Uani 1 1 d . . . H1A H 1.5809 -0.3361 -0.0143 0.031 Uiso 1 1 calc R . . C2 C 1.3948(2) -0.2291(2) 0.01556(16) 0.0257(4) Uani 1 1 d . . . H2A H 1.3860 -0.2079 -0.0540 0.031 Uiso 1 1 calc R . . C3 C 1.29177(19) -0.18262(18) 0.09557(16) 0.0218(4) Uani 1 1 d . . . C4 C 1.3033(2) -0.2195(2) 0.20038(17) 0.0263(4) Uani 1 1 d . . . H4A H 1.2338 -0.1895 0.2539 0.032 Uiso 1 1 calc R . . C5 C 1.4178(2) -0.3008(2) 0.22598(17) 0.0279(5) Uani 1 1 d . . . H5A H 1.4250 -0.3272 0.2964 0.033 Uiso 1 1 calc R . . C6 C 1.52119(19) -0.34188(19) 0.14495(17) 0.0239(4) Uani 1 1 d . . . C7 C 1.7103(2) -0.3370(2) 0.20750(18) 0.0260(4) Uani 1 1 d . . . C8 C 1.6635(3) -0.3163(3) 0.3098(2) 0.0415(6) Uani 1 1 d . . . H8A H 1.6131 -0.3544 0.3599 0.050 Uiso 1 1 calc R . . C9 C 1.6931(3) -0.2379(3) 0.3364(2) 0.0432(6) Uani 1 1 d . . . H9A H 1.6626 -0.2237 0.4053 0.052 Uiso 1 1 calc R . . C10 C 1.7675(2) -0.1804(2) 0.26175(17) 0.0264(4) Uani 1 1 d . . . C11 C 1.8131(2) -0.2011(2) 0.15904(17) 0.0280(5) Uani 1 1 d . . . H11A H 1.8626 -0.1621 0.1087 0.034 Uiso 1 1 calc R . . C12 C 1.7846(2) -0.2804(2) 0.13129(17) 0.0283(5) Uani 1 1 d . . . H12A H 1.8151 -0.2950 0.0626 0.034 Uiso 1 1 calc R . . C13 C 1.16825(19) -0.08987(19) 0.06649(16) 0.0237(4) Uani 1 1 d . . . C14 C 1.8014(2) -0.0996(2) 0.29484(19) 0.0307(5) Uani 1 1 d . . . C15 C 0.2921(2) 0.4266(3) 0.36826(19) 0.0451(7) Uani 1 1 d . . . H15A H 0.2297 0.4371 0.4304 0.054 Uiso 1 1 calc R . . C16 C 0.4141(2) 0.3455(3) 0.37255(19) 0.0429(7) Uani 1 1 d . . . H16A H 0.4342 0.3022 0.4380 0.052 Uiso 1 1 calc R . . C17 C 0.50678(19) 0.3283(2) 0.28001(17) 0.0248(4) Uani 1 1 d . . . C18 C 0.4774(2) 0.3977(2) 0.18330(17) 0.0266(4) Uani 1 1 d . . . H18A H 0.5400 0.3891 0.1212 0.032 Uiso 1 1 calc R . . C19 C 0.3557(2) 0.4798(2) 0.17815(17) 0.0257(4) Uani 1 1 d . . . H19A H 0.3361 0.5261 0.1131 0.031 Uiso 1 1 calc R . . C20 C 0.26406(19) 0.49194(19) 0.27079(16) 0.0239(4) Uani 1 1 d . . . C21 C 0.04152(19) 0.48489(19) 0.28262(16) 0.0231(4) Uani 1 1 d . . . C22 C 0.0746(2) 0.4227(2) 0.20240(18) 0.0338(5) Uani 1 1 d . . . H22A H 0.1240 0.4421 0.1365 0.041 Uiso 1 1 calc R . . C23 C 0.0330(2) 0.3317(2) 0.22224(18) 0.0331(5) Uani 1 1 d . . . H23A H 0.0542 0.2898 0.1692 0.040 Uiso 1 1 calc R . . C24 C -0.0403(2) 0.30257(19) 0.32094(17) 0.0244(4) Uani 1 1 d . . . C25 C -0.0771(2) 0.3688(2) 0.39892(18) 0.0307(5) Uani 1 1 d . . . H25A H -0.1299 0.3522 0.4637 0.037 Uiso 1 1 calc R . . C26 C -0.0349(2) 0.4596(2) 0.37988(18) 0.0298(5) Uani 1 1 d . . . H26A H -0.0579 0.5032 0.4322 0.036 Uiso 1 1 calc R . . C27 C 0.6374(2) 0.2341(2) 0.28583(18) 0.0273(5) Uani 1 1 d . . . C28 C -0.0779(2) 0.1976(2) 0.34413(17) 0.0258(4) Uani 1 1 d . . . C29 C 0.6248(4) -0.0512(4) 0.6216(2) 0.0707(11) Uani 1 1 d . . . H29A H 0.5929 -0.0568 0.5719 0.085 Uiso 1 1 calc R . . C30 C 0.5821(4) -0.0757(4) 0.7279(2) 0.0753(12) Uani 1 1 d . . . H30A H 0.5179 -0.1025 0.7642 0.090 Uiso 1 1 calc R . . C31 C 0.7340(2) -0.0187(2) 0.69109(17) 0.0319(5) Uani 1 1 d . . . H31A H 0.7928 0.0018 0.6995 0.038 Uiso 1 1 calc R . . C32 C 0.6385(2) -0.0689(2) 0.88623(17) 0.0355(5) Uani 1 1 d . . . H32A H 0.6996 -0.0478 0.8957 0.043 Uiso 1 1 calc R . . H32B H 0.6562 -0.1542 0.9202 0.043 Uiso 1 1 calc R . . C33 C 0.5075(2) 0.0111(2) 0.94001(17) 0.0341(5) Uani 1 1 d . . . H33A H 0.4459 -0.0063 0.9269 0.041 Uiso 1 1 calc R . . H33C H 0.4917 0.0968 0.9092 0.041 Uiso 1 1 calc R . . HW2A H 1.011(3) -0.1741(18) 0.389(2) 0.056(9) Uiso 1 1 d D . . HW2B H 1.042(3) -0.141(2) 0.457(2) 0.065(10) Uiso 1 1 d D . . HW1A H 0.922(3) 0.295(2) -0.0166(11) 0.052(9) Uiso 1 1 d D . . HW1B H 0.880(2) 0.3348(19) 0.0768(18) 0.051(9) Uiso 1 1 d D . . HW3A H 0.625(5) 0.305(3) 0.489(4) 0.14(2) Uiso 1 1 d D . . HW3B H 0.617(6) 0.423(4) 0.460(3) 0.16(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01889(17) 0.02242(18) 0.02081(17) -0.00742(12) -0.00476(12) -0.00578(13) Mn2 0.02807(19) 0.02419(18) 0.02260(17) -0.00496(12) -0.00790(13) -0.01228(14) S1 0.0255(3) 0.0221(3) 0.0434(3) -0.0121(2) -0.0165(2) -0.0053(2) S2 0.0195(3) 0.0225(3) 0.0265(3) -0.00506(19) -0.00672(19) -0.0078(2) OW1 0.0440(10) 0.0283(9) 0.0260(8) -0.0056(7) -0.0082(7) -0.0102(7) O1 0.0222(8) 0.0369(9) 0.0457(10) -0.0223(8) -0.0095(7) -0.0016(7) OW2 0.0416(10) 0.0373(10) 0.0453(10) -0.0160(8) -0.0230(8) -0.0046(8) O2 0.0367(10) 0.0586(12) 0.0387(10) -0.0216(9) -0.0218(8) -0.0011(8) OW3 0.0826(18) 0.0713(17) 0.0524(14) -0.0247(13) -0.0050(13) -0.0167(15) O3 0.0479(11) 0.0344(10) 0.0566(11) -0.0044(8) -0.0124(9) -0.0275(8) O4 0.0624(13) 0.0572(12) 0.0449(11) -0.0228(9) -0.0066(9) -0.0383(10) O5 0.0490(11) 0.0258(9) 0.0620(12) 0.0029(8) -0.0331(10) -0.0173(8) O6 0.0282(9) 0.0395(10) 0.0595(12) -0.0312(9) -0.0133(8) -0.0012(7) O7 0.0275(8) 0.0399(10) 0.0327(9) -0.0058(7) -0.0103(7) -0.0049(7) O8 0.0236(8) 0.0507(11) 0.0367(9) -0.0225(8) -0.0069(7) 0.0020(7) O9 0.0436(10) 0.0371(9) 0.0379(9) -0.0165(7) -0.0148(8) -0.0160(8) O10 0.0452(10) 0.0358(9) 0.0297(8) -0.0030(7) -0.0125(7) -0.0255(8) O11 0.0316(9) 0.0345(9) 0.0333(8) 0.0039(7) -0.0139(7) -0.0145(7) O12 0.0261(8) 0.0284(8) 0.0376(9) -0.0162(7) -0.0044(7) -0.0084(6) N1 0.0464(12) 0.0470(13) 0.0256(10) -0.0108(9) -0.0014(9) -0.0260(10) N2 0.0455(12) 0.0446(12) 0.0241(10) -0.0127(8) 0.0022(8) -0.0262(10) C1 0.0219(10) 0.0285(11) 0.0294(11) -0.0127(8) -0.0046(8) -0.0077(9) C2 0.0266(11) 0.0293(11) 0.0237(10) -0.0081(8) -0.0073(8) -0.0103(9) C3 0.0216(10) 0.0215(10) 0.0257(10) -0.0078(8) -0.0078(8) -0.0078(8) C4 0.0239(11) 0.0299(11) 0.0261(10) -0.0104(8) -0.0048(8) -0.0091(9) C5 0.0325(12) 0.0300(11) 0.0245(10) -0.0060(8) -0.0118(9) -0.0111(9) C6 0.0234(10) 0.0209(10) 0.0327(11) -0.0085(8) -0.0120(9) -0.0071(8) C7 0.0260(11) 0.0265(11) 0.0327(11) -0.0104(8) -0.0114(9) -0.0101(9) C8 0.0548(16) 0.0591(17) 0.0324(12) -0.0126(11) 0.0001(11) -0.0449(14) C9 0.0643(18) 0.0622(17) 0.0261(12) -0.0163(11) 0.0022(11) -0.0473(15) C10 0.0288(11) 0.0287(11) 0.0290(11) -0.0069(8) -0.0090(9) -0.0150(9) C11 0.0260(11) 0.0333(12) 0.0280(11) -0.0063(9) -0.0036(9) -0.0161(9) C12 0.0267(11) 0.0352(12) 0.0262(10) -0.0131(9) -0.0037(8) -0.0122(9) C13 0.0210(10) 0.0267(10) 0.0238(10) -0.0068(8) -0.0046(8) -0.0092(8) C14 0.0336(12) 0.0259(11) 0.0405(13) -0.0084(9) -0.0144(10) -0.0131(10) C15 0.0227(12) 0.0637(18) 0.0233(11) -0.0055(11) 0.0000(9) -0.0028(11) C16 0.0256(12) 0.0579(17) 0.0232(11) 0.0000(11) -0.0066(9) -0.0039(11) C17 0.0196(10) 0.0279(11) 0.0286(11) -0.0103(8) -0.0064(8) -0.0072(8) C18 0.0245(11) 0.0321(12) 0.0228(10) -0.0111(8) 0.0004(8) -0.0113(9) C19 0.0254(11) 0.0275(11) 0.0228(10) -0.0047(8) -0.0060(8) -0.0093(9) C20 0.0170(10) 0.0269(11) 0.0279(10) -0.0088(8) -0.0048(8) -0.0070(8) C21 0.0223(10) 0.0234(10) 0.0268(10) -0.0060(8) -0.0062(8) -0.0107(8) C22 0.0366(13) 0.0468(14) 0.0252(11) -0.0128(10) 0.0014(9) -0.0246(11) C23 0.0376(13) 0.0416(13) 0.0287(11) -0.0177(10) -0.0028(10) -0.0190(11) C24 0.0260(11) 0.0239(10) 0.0272(10) -0.0072(8) -0.0087(8) -0.0102(8) C25 0.0356(12) 0.0349(12) 0.0257(11) -0.0118(9) 0.0013(9) -0.0194(10) C26 0.0314(12) 0.0326(12) 0.0303(11) -0.0152(9) -0.0005(9) -0.0153(10) C27 0.0217(10) 0.0288(11) 0.0346(12) -0.0122(9) -0.0073(9) -0.0083(9) C28 0.0251(11) 0.0268(11) 0.0306(11) -0.0093(8) -0.0104(9) -0.0094(9) C29 0.088(3) 0.134(4) 0.0324(15) -0.0272(18) 0.0061(15) -0.085(3) C30 0.096(3) 0.145(4) 0.0335(15) -0.0273(18) 0.0133(16) -0.101(3) C31 0.0381(13) 0.0364(13) 0.0257(11) -0.0117(9) -0.0007(9) -0.0194(10) C32 0.0476(15) 0.0364(13) 0.0226(11) -0.0078(9) -0.0025(10) -0.0196(11) C33 0.0454(14) 0.0325(12) 0.0234(12) -0.0066(9) -0.0037(10) -0.0171(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O2 2.1169(16) 2_755 ? Mn1 O3 2.1210(19) 1_455 ? Mn1 O1 2.1304(17) . ? Mn1 O8 2.1712(19) . ? Mn1 O9 2.2321(16) 1_655 ? Mn1 OW1 2.2368(19) . ? Mn2 O7 2.1115(19) . ? Mn2 O4 2.1268(18) 1_455 ? Mn2 OW2 2.176(2) . ? Mn2 O10 2.1921(16) 1_655 ? Mn2 N1 2.209(2) . ? S1 O5 1.4349(19) . ? S1 O6 1.4437(19) . ? S1 C7 1.771(2) . ? S1 C6 1.773(2) . ? S2 O11 1.4359(17) . ? S2 O12 1.4414(16) . ? S2 C20 1.763(2) . ? S2 C21 1.768(2) . ? OW1 HW1A 0.832(10) . ? OW1 HW1B 0.845(10) . ? O1 C13 1.255(3) . ? OW2 HW2A 0.845(10) . ? OW2 HW2B 0.842(10) . ? O2 C13 1.233(3) . ? O2 Mn1 2.1169(16) 2_755 ? OW3 HW3A 0.842(10) . ? OW3 HW3B 0.84(5) . ? O3 C14 1.246(3) . ? O3 Mn1 2.1210(19) 1_655 ? O4 C14 1.252(3) . ? O4 Mn2 2.1268(18) 1_655 ? O7 C27 1.257(3) . ? O8 C27 1.249(3) . ? O9 C28 1.241(3) . ? O9 Mn1 2.2321(16) 1_455 ? O10 C28 1.278(3) . ? O10 Mn2 2.1921(16) 1_455 ? N1 C31 1.327(3) . ? N1 C29 1.367(4) . ? N2 C31 1.337(3) . ? N2 C30 1.364(4) . ? N2 C32 1.474(3) . ? C1 C2 1.389(3) . ? C1 C6 1.396(3) . ? C1 H1A 0.9300 . ? C2 C3 1.391(3) . ? C2 H2A 0.9300 . ? C3 C4 1.389(3) . ? C3 C13 1.518(3) . ? C4 C5 1.389(3) . ? C4 H4A 0.9300 . ? C5 C6 1.386(3) . ? C5 H5A 0.9300 . ? C7 C8 1.378(3) . ? C7 C12 1.384(3) . ? C8 C9 1.381(3) . ? C8 H8A 0.9300 . ? C9 C10 1.384(3) . ? C9 H9A 0.9300 . ? C10 C11 1.384(3) . ? C10 C14 1.500(3) . ? C11 C12 1.392(3) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C15 C20 1.379(3) . ? C15 C16 1.382(3) . ? C15 H15A 0.9300 . ? C16 C17 1.385(3) . ? C16 H16A 0.9300 . ? C17 C18 1.385(3) . ? C17 C27 1.504(3) . ? C18 C19 1.383(3) . ? C18 H18A 0.9300 . ? C19 C20 1.377(3) . ? C19 H19A 0.9300 . ? C21 C26 1.382(3) . ? C21 C22 1.392(3) . ? C22 C23 1.382(3) . ? C22 H22A 0.9300 . ? C23 C24 1.389(3) . ? C23 H23A 0.9300 . ? C24 C25 1.390(3) . ? C24 C28 1.507(3) . ? C25 C26 1.388(3) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C29 C30 1.347(4) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 C33 1.526(3) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C33 1.530(4) 2_657 ? C33 H33A 0.9700 . ? C33 H33C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn1 O3 91.99(8) 2_755 1_455 ? O2 Mn1 O1 105.60(7) 2_755 . ? O3 Mn1 O1 87.76(8) 1_455 . ? O2 Mn1 O8 87.54(7) 2_755 . ? O3 Mn1 O8 88.72(8) 1_455 . ? O1 Mn1 O8 166.50(6) . . ? O2 Mn1 O9 165.90(7) 2_755 1_655 ? O3 Mn1 O9 98.82(7) 1_455 1_655 ? O1 Mn1 O9 83.97(7) . 1_655 ? O8 Mn1 O9 83.70(7) . 1_655 ? O2 Mn1 OW1 86.22(8) 2_755 . ? O3 Mn1 OW1 177.18(7) 1_455 . ? O1 Mn1 OW1 94.82(8) . . ? O8 Mn1 OW1 89.02(8) . . ? O9 Mn1 OW1 82.61(7) 1_655 . ? O7 Mn2 O4 89.84(8) . 1_455 ? O7 Mn2 OW2 155.44(7) . . ? O4 Mn2 OW2 88.37(8) 1_455 . ? O7 Mn2 O10 86.78(7) . 1_655 ? O4 Mn2 O10 170.14(7) 1_455 1_655 ? OW2 Mn2 O10 90.86(7) . 1_655 ? O7 Mn2 N1 99.94(9) . . ? O4 Mn2 N1 90.46(8) 1_455 . ? OW2 Mn2 N1 104.56(9) . . ? O10 Mn2 N1 99.23(7) 1_655 . ? O5 S1 O6 119.39(12) . . ? O5 S1 C7 107.56(11) . . ? O6 S1 C7 108.58(11) . . ? O5 S1 C6 108.83(11) . . ? O6 S1 C6 107.63(11) . . ? C7 S1 C6 103.77(10) . . ? O11 S2 O12 119.15(10) . . ? O11 S2 C20 107.50(11) . . ? O12 S2 C20 108.86(10) . . ? O11 S2 C21 109.42(10) . . ? O12 S2 C21 108.29(10) . . ? C20 S2 C21 102.31(10) . . ? Mn1 OW1 HW1A 115(2) . . ? Mn1 OW1 HW1B 110(2) . . ? HW1A OW1 HW1B 109.3(15) . . ? C13 O1 Mn1 127.40(14) . . ? Mn2 OW2 HW2A 116(2) . . ? Mn2 OW2 HW2B 122(2) . . ? HW2A OW2 HW2B 108.2(16) . . ? C13 O2 Mn1 175.00(18) . 2_755 ? HW3A OW3 HW3B 108.5(17) . . ? C14 O3 Mn1 145.58(17) . 1_655 ? C14 O4 Mn2 114.98(16) . 1_655 ? C27 O7 Mn2 130.90(15) . . ? C27 O8 Mn1 138.35(15) . . ? C28 O9 Mn1 166.48(16) . 1_455 ? C28 O10 Mn2 103.14(13) . 1_455 ? C31 N1 C29 104.8(2) . . ? C31 N1 Mn2 136.60(17) . . ? C29 N1 Mn2 118.60(17) . . ? C31 N2 C30 106.8(2) . . ? C31 N2 C32 127.2(2) . . ? C30 N2 C32 125.9(2) . . ? C2 C1 C6 119.0(2) . . ? C2 C1 H1A 120.5 . . ? C6 C1 H1A 120.5 . . ? C1 C2 C3 120.20(19) . . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? C4 C3 C2 119.93(18) . . ? C4 C3 C13 120.81(19) . . ? C2 C3 C13 119.25(18) . . ? C3 C4 C5 120.6(2) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C6 C5 C4 118.95(19) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? C5 C6 C1 121.29(19) . . ? C5 C6 S1 119.48(16) . . ? C1 C6 S1 119.22(17) . . ? C8 C7 C12 121.6(2) . . ? C8 C7 S1 117.86(18) . . ? C12 C7 S1 120.53(16) . . ? C9 C8 C7 118.8(2) . . ? C9 C8 H8A 120.6 . . ? C7 C8 H8A 120.6 . . ? C8 C9 C10 120.7(2) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C11 C10 C9 119.9(2) . . ? C11 C10 C14 120.9(2) . . ? C9 C10 C14 119.1(2) . . ? C10 C11 C12 119.9(2) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C7 C12 C11 119.0(2) . . ? C7 C12 H12A 120.5 . . ? C11 C12 H12A 120.5 . . ? O2 C13 O1 126.5(2) . . ? O2 C13 C3 117.59(19) . . ? O1 C13 C3 115.86(18) . . ? O3 C14 O4 124.1(2) . . ? O3 C14 C10 118.1(2) . . ? O4 C14 C10 117.8(2) . . ? C20 C15 C16 119.2(2) . . ? C20 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? C15 C16 C17 120.5(2) . . ? C15 C16 H16A 119.8 . . ? C17 C16 H16A 119.8 . . ? C18 C17 C16 119.35(19) . . ? C18 C17 C27 121.0(2) . . ? C16 C17 C27 119.7(2) . . ? C19 C18 C17 120.6(2) . . ? C19 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? C20 C19 C18 119.0(2) . . ? C20 C19 H19A 120.5 . . ? C18 C19 H19A 120.5 . . ? C19 C20 C15 121.27(19) . . ? C19 C20 S2 119.40(16) . . ? C15 C20 S2 119.31(17) . . ? C26 C21 C22 121.1(2) . . ? C26 C21 S2 118.84(16) . . ? C22 C21 S2 119.85(17) . . ? C23 C22 C21 119.0(2) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C22 C23 C24 120.4(2) . . ? C22 C23 H23A 119.8 . . ? C24 C23 H23A 119.8 . . ? C25 C24 C23 120.0(2) . . ? C25 C24 C28 120.0(2) . . ? C23 C24 C28 119.94(19) . . ? C26 C25 C24 119.8(2) . . ? C26 C25 H25A 120.1 . . ? C24 C25 H25A 120.1 . . ? C21 C26 C25 119.5(2) . . ? C21 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? O8 C27 O7 126.8(2) . . ? O8 C27 C17 116.1(2) . . ? O7 C27 C17 117.1(2) . . ? O9 C28 O10 122.5(2) . . ? O9 C28 C24 119.6(2) . . ? O10 C28 C24 117.93(18) . . ? C30 C29 N1 110.1(3) . . ? C30 C29 H29A 125.0 . . ? N1 C29 H29A 125.0 . . ? C29 C30 N2 106.6(3) . . ? C29 C30 H30A 126.7 . . ? N2 C30 H30A 126.7 . . ? N1 C31 N2 111.8(2) . . ? N1 C31 H31A 124.1 . . ? N2 C31 H31A 124.1 . . ? N2 C32 C33 112.1(2) . . ? N2 C32 H32A 109.2 . . ? C33 C32 H32A 109.2 . . ? N2 C32 H32B 109.2 . . ? C33 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C33 111.8(3) . 2_657 ? C32 C33 H33A 109.3 . . ? C33 C33 H33A 109.3 2_657 . ? C32 C33 H33C 109.3 . . ? C33 C33 H33C 109.3 2_657 . ? H33A C33 H33C 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Mn1 O1 C13 -23.0(2) 2_755 . . . ? O3 Mn1 O1 C13 68.4(2) 1_455 . . . ? O8 Mn1 O1 C13 143.4(3) . . . . ? O9 Mn1 O1 C13 167.5(2) 1_655 . . . ? OW1 Mn1 O1 C13 -110.5(2) . . . . ? O4 Mn2 O7 C27 -64.4(2) 1_455 . . . ? OW2 Mn2 O7 C27 21.3(3) . . . . ? O10 Mn2 O7 C27 106.3(2) 1_655 . . . ? N1 Mn2 O7 C27 -154.9(2) . . . . ? O2 Mn1 O8 C27 157.2(3) 2_755 . . . ? O3 Mn1 O8 C27 65.2(3) 1_455 . . . ? O1 Mn1 O8 C27 -9.8(5) . . . . ? O9 Mn1 O8 C27 -33.9(3) 1_655 . . . ? OW1 Mn1 O8 C27 -116.5(3) . . . . ? O7 Mn2 N1 C31 -113.0(3) . . . . ? O4 Mn2 N1 C31 157.0(3) 1_455 . . . ? OW2 Mn2 N1 C31 68.6(3) . . . . ? O10 Mn2 N1 C31 -24.7(3) 1_655 . . . ? O7 Mn2 N1 C29 64.8(3) . . . . ? O4 Mn2 N1 C29 -25.1(3) 1_455 . . . ? OW2 Mn2 N1 C29 -113.6(3) . . . . ? O10 Mn2 N1 C29 153.1(3) 1_655 . . . ? C6 C1 C2 C3 2.5(3) . . . . ? C1 C2 C3 C4 -3.5(3) . . . . ? C1 C2 C3 C13 175.3(2) . . . . ? C2 C3 C4 C5 1.3(3) . . . . ? C13 C3 C4 C5 -177.5(2) . . . . ? C3 C4 C5 C6 1.8(3) . . . . ? C4 C5 C6 C1 -2.8(3) . . . . ? C4 C5 C6 S1 175.57(17) . . . . ? C2 C1 C6 C5 0.6(3) . . . . ? C2 C1 C6 S1 -177.73(16) . . . . ? O5 S1 C6 C5 43.5(2) . . . . ? O6 S1 C6 C5 174.24(17) . . . . ? C7 S1 C6 C5 -70.80(19) . . . . ? O5 S1 C6 C1 -138.11(18) . . . . ? O6 S1 C6 C1 -7.4(2) . . . . ? C7 S1 C6 C1 107.58(18) . . . . ? O5 S1 C7 C8 -31.7(2) . . . . ? O6 S1 C7 C8 -162.2(2) . . . . ? C6 S1 C7 C8 83.5(2) . . . . ? O5 S1 C7 C12 149.26(19) . . . . ? O6 S1 C7 C12 18.8(2) . . . . ? C6 S1 C7 C12 -95.5(2) . . . . ? C12 C7 C8 C9 -0.6(4) . . . . ? S1 C7 C8 C9 -179.6(2) . . . . ? C7 C8 C9 C10 0.5(4) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? C8 C9 C10 C14 -177.7(2) . . . . ? C9 C10 C11 C12 -0.4(4) . . . . ? C14 C10 C11 C12 177.4(2) . . . . ? C8 C7 C12 C11 0.3(3) . . . . ? S1 C7 C12 C11 179.25(16) . . . . ? C10 C11 C12 C7 0.2(3) . . . . ? Mn1 O2 C13 O1 42(2) 2_755 . . . ? Mn1 O2 C13 C3 -136.6(19) 2_755 . . . ? Mn1 O1 C13 O2 22.7(4) . . . . ? Mn1 O1 C13 C3 -159.06(14) . . . . ? C4 C3 C13 O2 -146.9(2) . . . . ? C2 C3 C13 O2 34.3(3) . . . . ? C4 C3 C13 O1 34.7(3) . . . . ? C2 C3 C13 O1 -144.1(2) . . . . ? Mn1 O3 C14 O4 -63.1(4) 1_655 . . . ? Mn1 O3 C14 C10 119.9(3) 1_655 . . . ? Mn2 O4 C14 O3 1.3(3) 1_655 . . . ? Mn2 O4 C14 C10 178.36(15) 1_655 . . . ? C11 C10 C14 O3 -4.5(3) . . . . ? C9 C10 C14 O3 173.3(2) . . . . ? C11 C10 C14 O4 178.2(2) . . . . ? C9 C10 C14 O4 -4.0(3) . . . . ? C20 C15 C16 C17 -1.2(5) . . . . ? C15 C16 C17 C18 3.3(4) . . . . ? C15 C16 C17 C27 -176.4(3) . . . . ? C16 C17 C18 C19 -2.8(3) . . . . ? C27 C17 C18 C19 176.8(2) . . . . ? C17 C18 C19 C20 0.3(3) . . . . ? C18 C19 C20 C15 1.9(3) . . . . ? C18 C19 C20 S2 -176.40(17) . . . . ? C16 C15 C20 C19 -1.5(4) . . . . ? C16 C15 C20 S2 176.8(2) . . . . ? O11 S2 C20 C19 -12.9(2) . . . . ? O12 S2 C20 C19 -143.20(17) . . . . ? C21 S2 C20 C19 102.34(19) . . . . ? O11 S2 C20 C15 168.8(2) . . . . ? O12 S2 C20 C15 38.5(2) . . . . ? C21 S2 C20 C15 -76.0(2) . . . . ? O11 S2 C21 C26 -141.83(18) . . . . ? O12 S2 C21 C26 -10.5(2) . . . . ? C20 S2 C21 C26 104.39(19) . . . . ? O11 S2 C21 C22 42.9(2) . . . . ? O12 S2 C21 C22 174.27(17) . . . . ? C20 S2 C21 C22 -70.9(2) . . . . ? C26 C21 C22 C23 -2.0(3) . . . . ? S2 C21 C22 C23 173.16(18) . . . . ? C21 C22 C23 C24 -0.3(4) . . . . ? C22 C23 C24 C25 3.0(4) . . . . ? C22 C23 C24 C28 -175.9(2) . . . . ? C23 C24 C25 C26 -3.4(3) . . . . ? C28 C24 C25 C26 175.4(2) . . . . ? C22 C21 C26 C25 1.5(3) . . . . ? S2 C21 C26 C25 -173.68(17) . . . . ? C24 C25 C26 C21 1.2(4) . . . . ? Mn1 O8 C27 O7 -6.6(4) . . . . ? Mn1 O8 C27 C17 174.11(17) . . . . ? Mn2 O7 C27 O8 -13.8(4) . . . . ? Mn2 O7 C27 C17 165.44(15) . . . . ? C18 C17 C27 O8 -10.1(3) . . . . ? C16 C17 C27 O8 169.5(2) . . . . ? C18 C17 C27 O7 170.6(2) . . . . ? C16 C17 C27 O7 -9.8(3) . . . . ? Mn1 O9 C28 O10 80.6(7) 1_455 . . . ? Mn1 O9 C28 C24 -100.7(7) 1_455 . . . ? Mn2 O10 C28 O9 -10.2(2) 1_455 . . . ? Mn2 O10 C28 C24 171.05(15) 1_455 . . . ? C25 C24 C28 O9 166.5(2) . . . . ? C23 C24 C28 O9 -14.6(3) . . . . ? C25 C24 C28 O10 -14.7(3) . . . . ? C23 C24 C28 O10 164.2(2) . . . . ? C31 N1 C29 C30 -1.5(5) . . . . ? Mn2 N1 C29 C30 -179.9(3) . . . . ? N1 C29 C30 N2 1.5(5) . . . . ? C31 N2 C30 C29 -1.0(4) . . . . ? C32 N2 C30 C29 -179.5(3) . . . . ? C29 N1 C31 N2 0.8(3) . . . . ? Mn2 N1 C31 N2 178.87(19) . . . . ? C30 N2 C31 N1 0.1(3) . . . . ? C32 N2 C31 N1 178.5(2) . . . . ? C31 N2 C32 C33 122.3(3) . . . . ? C30 N2 C32 C33 -59.5(4) . . . . ? N2 C32 C33 C33 176.5(3) . . . 2_657 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW3 HW3A O7 0.842(10) 2.28(2) 3.072(3) 158(5) . OW2 HW2A O12 0.845(10) 2.227(11) 3.065(2) 171(3) 1_645 OW2 HW2B O10 0.842(10) 1.858(11) 2.679(2) 164(3) 2_656 OW1 HW1A O11 0.832(10) 1.955(10) 2.786(2) 176(3) 2_665 OW1 HW1B O6 0.845(10) 2.152(16) 2.929(3) 153(2) 1_465 OW3 HW3B O5 0.84(5) 2.40(4) 3.087(3) 139(5) 1_465 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.555 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.106 data_c2b _database_code_depnum_ccdc_archive 'CCDC 808841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 N4 Ni O10 S' _chemical_formula_weight 625.29 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2542(19) _cell_length_b 12.022(2) _cell_length_c 13.235(3) _cell_angle_alpha 80.84(3) _cell_angle_beta 79.36(3) _cell_angle_gamma 86.47(3) _cell_volume 1427.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8066 _cell_measurement_theta_min 1.58 _cell_measurement_theta_max 26.50 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 0.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6681 _exptl_absorpt_correction_T_max 0.7266 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8066 _diffrn_reflns_av_R_equivalents 0.0214 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 26.50 _reflns_number_total 5751 _reflns_number_gt 4990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1700P)^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 5751 _refine_ls_number_parameters 385 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.2130 _refine_ls_wR_factor_gt 0.2047 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni -0.47784(4) 0.34180(3) -0.18773(3) 0.02482(19) Uani 1 1 d . . . S1 S 0.22863(10) -0.11754(8) -0.42763(6) 0.0377(3) Uani 1 1 d . . . O1 O -0.3022(2) 0.2447(2) -0.24866(18) 0.0326(5) Uani 1 1 d . . . OW1 O -0.6482(3) 0.4471(2) -0.12667(19) 0.0334(5) Uani 1 1 d D . . O2 O -0.1077(3) 0.3381(2) -0.2345(2) 0.0437(6) Uani 1 1 d . . . OW2 O -0.3439(3) 0.4835(2) -0.22458(18) 0.0322(5) Uani 1 1 d D . . OW3 O -0.9222(4) 0.3623(4) 0.0968(3) 0.0834(12) Uani 1 1 d . . . O3 O 0.6127(2) -0.3791(2) -0.06759(17) 0.0356(5) Uani 1 1 d . . . OW4 O 0.0552(4) 0.4219(5) -0.1162(4) 0.0832(13) Uani 1 1 d DU . . O4 O 0.4133(3) -0.3172(2) 0.03592(17) 0.0339(5) Uani 1 1 d . . . O5 O 0.1356(3) -0.1996(2) -0.4495(2) 0.0495(7) Uani 1 1 d . . . O6 O 0.3447(3) -0.0696(3) -0.5076(2) 0.0504(7) Uani 1 1 d . . . N1 N -0.5906(3) 0.1925(2) -0.1412(2) 0.0316(6) Uani 1 1 d . . . N2 N -0.7152(4) 0.0534(3) -0.0423(3) 0.0461(8) Uani 1 1 d . . . N3 N -0.5516(3) 0.3751(2) -0.3295(2) 0.0300(6) Uani 1 1 d . . . N4 N -0.6831(3) 0.4493(3) -0.4483(2) 0.0333(6) Uani 1 1 d . . . C1 C 0.1771(4) 0.0896(3) -0.3651(3) 0.0393(8) Uani 1 1 d . . . H1A H 0.2784 0.0974 -0.3825 0.047 Uiso 1 1 calc R . . C2 C 0.0864(4) 0.1743(3) -0.3241(3) 0.0362(8) Uani 1 1 d . . . H2A H 0.1275 0.2391 -0.3131 0.043 Uiso 1 1 calc R . . C3 C -0.0658(4) 0.1626(3) -0.2993(2) 0.0293(7) Uani 1 1 d . . . C4 C -0.1264(4) 0.0663(3) -0.3163(3) 0.0342(7) Uani 1 1 d . . . H4A H -0.2279 0.0594 -0.3016 0.041 Uiso 1 1 calc R . . C5 C -0.0379(4) -0.0201(3) -0.3549(3) 0.0367(8) Uani 1 1 d . . . H5A H -0.0785 -0.0858 -0.3641 0.044 Uiso 1 1 calc R . . C6 C 0.1139(4) -0.0060(3) -0.3796(3) 0.0323(7) Uani 1 1 d . . . C7 C 0.3077(4) -0.1800(3) -0.3182(3) 0.0343(7) Uani 1 1 d . . . C8 C 0.2146(4) -0.2340(3) -0.2314(3) 0.0372(8) Uani 1 1 d . . . H8A H 0.1148 -0.2387 -0.2321 0.045 Uiso 1 1 calc R . . C9 C 0.2732(4) -0.2807(3) -0.1440(3) 0.0325(7) Uani 1 1 d . . . H9A H 0.2117 -0.3130 -0.0841 0.039 Uiso 1 1 calc R . . C10 C 0.4245(4) -0.2791(3) -0.1464(2) 0.0288(7) Uani 1 1 d . . . C11 C 0.5161(4) -0.2284(3) -0.2357(3) 0.0384(8) Uani 1 1 d . . . H11A H 0.6172 -0.2299 -0.2379 0.046 Uiso 1 1 calc R . . C12 C 0.4576(4) -0.1759(3) -0.3213(3) 0.0388(8) Uani 1 1 d . . . H12A H 0.5180 -0.1389 -0.3794 0.047 Uiso 1 1 calc R . . C13 C -0.1647(3) 0.2567(3) -0.2569(2) 0.0279(6) Uani 1 1 d . . . C14 C 0.4877(4) -0.3297(3) -0.0513(2) 0.0298(7) Uani 1 1 d . . . C15 C -0.6814(4) 0.1610(3) -0.0525(3) 0.0427(9) Uani 1 1 d . . . H15A H -0.7170 0.2083 -0.0036 0.051 Uiso 1 1 calc R . . C16 C -0.5676(5) 0.1003(3) -0.1887(3) 0.0507(11) Uani 1 1 d . . . H16A H -0.5090 0.0969 -0.2533 0.061 Uiso 1 1 calc R . . C17 C -0.6423(5) 0.0134(4) -0.1284(4) 0.0657(14) Uani 1 1 d . . . H17A H -0.6435 -0.0596 -0.1432 0.079 Uiso 1 1 calc R . . C18 C -0.8117(6) -0.0114(5) 0.0469(4) 0.0690(15) Uani 1 1 d . . . H18A H -0.8391 0.0346 0.1018 0.083 Uiso 1 1 calc R . . H18B H -0.7576 -0.0777 0.0740 0.083 Uiso 1 1 calc R . . C19 C -0.9510(6) -0.0479(5) 0.0163(4) 0.0721(15) Uani 1 1 d . . . H19A H -0.9231 -0.0916 -0.0403 0.087 Uiso 1 1 calc R . . H19B H -1.0049 -0.0964 0.0750 0.087 Uiso 1 1 calc R . . C20 C -0.6510(4) 0.4539(3) -0.3539(3) 0.0338(7) Uani 1 1 d . . . H20A H -0.6933 0.5059 -0.3112 0.041 Uiso 1 1 calc R . . C21 C -0.5197(4) 0.3175(3) -0.4129(3) 0.0356(7) Uani 1 1 d . . . H21A H -0.4529 0.2568 -0.4184 0.043 Uiso 1 1 calc R . . C22 C -0.6007(4) 0.3627(3) -0.4863(3) 0.0386(8) Uani 1 1 d . . . H22A H -0.5999 0.3389 -0.5499 0.046 Uiso 1 1 calc R . . C23 C -0.7949(4) 0.5201(3) -0.4974(3) 0.0410(8) Uani 1 1 d . . . H23A H -0.7607 0.5356 -0.5719 0.049 Uiso 1 1 calc R . . H23B H -0.8082 0.5915 -0.4709 0.049 Uiso 1 1 calc R . . C24 C -0.9409(4) 0.4626(3) -0.4759(3) 0.0452(9) Uani 1 1 d . . . H24A H -0.9736 0.4450 -0.4013 0.054 Uiso 1 1 calc R . . H24B H -0.9281 0.3923 -0.5041 0.054 Uiso 1 1 calc R . . HW2A H -0.363(5) 0.531(3) -0.183(3) 0.078(18) Uiso 1 1 d D . . HW1B H -0.7358(18) 0.440(4) -0.134(2) 0.041(11) Uiso 1 1 d D . . HW2B H -0.259(2) 0.456(4) -0.223(4) 0.063(15) Uiso 1 1 d D . . HW1A H -0.643(4) 0.430(3) -0.0632(11) 0.040(11) Uiso 1 1 d D . . HW4B H 0.028(8) 0.4904(17) -0.126(6) 0.12(3) Uiso 1 1 d D . . HW4A H 0.012(7) 0.386(4) -0.150(5) 0.11(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0197(3) 0.0263(3) 0.0279(3) -0.00250(17) -0.00482(17) 0.00102(17) S1 0.0408(5) 0.0415(5) 0.0308(5) -0.0074(4) -0.0106(4) 0.0172(4) O1 0.0203(11) 0.0336(13) 0.0433(13) -0.0079(10) -0.0035(9) 0.0029(9) OW1 0.0260(12) 0.0376(13) 0.0360(13) -0.0050(10) -0.0067(9) 0.0068(10) O2 0.0262(12) 0.0447(15) 0.0638(17) -0.0211(13) -0.0073(12) 0.0016(11) OW2 0.0317(13) 0.0312(12) 0.0345(12) -0.0107(10) -0.0039(10) 0.0009(10) OW3 0.0471(19) 0.106(3) 0.096(3) -0.023(2) 0.0020(19) -0.018(2) O3 0.0269(12) 0.0492(14) 0.0327(12) -0.0106(10) -0.0101(9) 0.0106(10) OW4 0.0456(19) 0.119(4) 0.105(3) -0.056(3) -0.034(2) 0.005(2) O4 0.0289(12) 0.0421(14) 0.0293(12) -0.0033(10) -0.0051(9) 0.0046(10) O5 0.0608(18) 0.0473(16) 0.0477(15) -0.0198(12) -0.0243(13) 0.0186(13) O6 0.0494(16) 0.0633(18) 0.0306(13) 0.0025(12) -0.0021(11) 0.0208(14) N1 0.0275(14) 0.0266(14) 0.0400(15) -0.0074(11) -0.0022(11) -0.0001(11) N2 0.0447(18) 0.0446(18) 0.0453(17) 0.0043(14) -0.0031(14) -0.0158(15) N3 0.0251(13) 0.0348(15) 0.0302(13) -0.0052(11) -0.0054(10) -0.0003(11) N4 0.0263(14) 0.0412(16) 0.0319(14) 0.0018(12) -0.0097(11) -0.0012(12) C1 0.0247(16) 0.040(2) 0.050(2) -0.0039(16) -0.0037(14) 0.0049(14) C2 0.0275(17) 0.0332(18) 0.048(2) -0.0070(15) -0.0065(14) 0.0016(13) C3 0.0265(15) 0.0341(17) 0.0255(14) 0.0013(12) -0.0070(11) 0.0061(12) C4 0.0238(15) 0.044(2) 0.0345(17) -0.0055(14) -0.0079(12) 0.0036(13) C5 0.0343(18) 0.0381(19) 0.0397(18) -0.0038(14) -0.0149(14) 0.0016(14) C6 0.0299(17) 0.0330(17) 0.0318(16) -0.0030(13) -0.0062(13) 0.0143(13) C7 0.0353(18) 0.0355(18) 0.0321(17) -0.0066(13) -0.0092(13) 0.0132(14) C8 0.0287(16) 0.0395(19) 0.0440(19) -0.0013(15) -0.0128(14) 0.0014(14) C9 0.0284(16) 0.0315(17) 0.0362(17) -0.0018(13) -0.0055(13) 0.0011(13) C10 0.0286(16) 0.0280(16) 0.0301(16) -0.0045(12) -0.0077(12) 0.0048(12) C11 0.0268(16) 0.052(2) 0.0341(17) -0.0049(15) -0.0026(13) 0.0071(15) C12 0.0335(18) 0.046(2) 0.0319(17) 0.0002(14) -0.0009(13) 0.0067(15) C13 0.0244(15) 0.0313(16) 0.0269(15) -0.0008(12) -0.0063(11) 0.0043(12) C14 0.0298(16) 0.0306(16) 0.0309(16) -0.0026(12) -0.0117(12) -0.0021(13) C15 0.043(2) 0.046(2) 0.0385(19) -0.0097(16) 0.0017(15) -0.0108(17) C16 0.047(2) 0.043(2) 0.059(2) -0.0227(19) 0.0132(19) -0.0141(18) C17 0.057(3) 0.037(2) 0.096(4) -0.017(2) 0.016(3) -0.011(2) C18 0.067(3) 0.077(3) 0.053(3) 0.027(2) -0.008(2) -0.034(3) C19 0.063(3) 0.063(3) 0.076(3) 0.011(3) 0.010(3) -0.023(3) C20 0.0330(17) 0.0370(18) 0.0314(16) -0.0048(13) -0.0078(13) 0.0043(14) C21 0.0316(17) 0.0396(19) 0.0356(17) -0.0090(14) -0.0057(13) 0.0075(14) C22 0.0388(19) 0.050(2) 0.0291(16) -0.0115(15) -0.0092(14) 0.0025(16) C23 0.0312(18) 0.046(2) 0.0430(19) 0.0122(15) -0.0144(14) -0.0004(15) C24 0.0334(19) 0.049(2) 0.050(2) 0.0114(17) -0.0156(16) -0.0028(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.059(2) . ? Ni1 N1 2.081(3) . ? Ni1 N3 2.084(3) . ? Ni1 OW1 2.086(2) . ? Ni1 OW2 2.109(2) . ? Ni1 O4 2.171(2) 2 ? S1 O6 1.438(3) . ? S1 O5 1.444(3) . ? S1 C7 1.781(3) . ? S1 C6 1.783(3) . ? O1 C13 1.271(4) . ? OW1 HW1B 0.843(10) . ? OW1 HW1A 0.842(10) . ? O2 C13 1.241(4) . ? OW2 HW2A 0.843(10) . ? OW2 HW2B 0.837(10) . ? O3 C14 1.265(4) . ? OW4 HW4B 0.845(10) . ? OW4 HW4A 0.83(6) . ? O4 C14 1.256(4) . ? O4 Ni1 2.171(2) 2 ? N1 C15 1.327(4) . ? N1 C16 1.347(5) . ? N2 C15 1.330(5) . ? N2 C17 1.355(6) . ? N2 C18 1.484(5) . ? N3 C20 1.323(4) . ? N3 C21 1.373(4) . ? N4 C20 1.347(4) . ? N4 C22 1.359(5) . ? N4 C23 1.477(4) . ? C1 C6 1.375(5) . ? C1 C2 1.393(5) . ? C1 H1A 0.9300 . ? C2 C3 1.397(5) . ? C2 H2A 0.9300 . ? C3 C4 1.384(5) . ? C3 C13 1.521(5) . ? C4 C5 1.385(5) . ? C4 H4A 0.9300 . ? C5 C6 1.397(5) . ? C5 H5A 0.9300 . ? C7 C12 1.384(5) . ? C7 C8 1.397(5) . ? C8 C9 1.391(5) . ? C8 H8A 0.9300 . ? C9 C10 1.396(5) . ? C9 H9A 0.9300 . ? C10 C11 1.397(5) . ? C10 C14 1.511(4) . ? C11 C12 1.390(5) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.351(6) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.529(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C19 1.481(11) 2_355 ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9300 . ? C21 C22 1.360(5) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 C24 1.515(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C24 1.538(7) 2_364 ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? 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 Ni1 N1 86.60(10) . . ? O1 Ni1 N3 91.86(10) . . ? N1 Ni1 N3 93.35(12) . . ? O1 Ni1 OW1 176.98(9) . . ? N1 Ni1 OW1 96.31(11) . . ? N3 Ni1 OW1 88.77(11) . . ? O1 Ni1 OW2 89.45(9) . . ? N1 Ni1 OW2 172.99(10) . . ? N3 Ni1 OW2 92.57(10) . . ? OW1 Ni1 OW2 87.57(10) . . ? O1 Ni1 O4 92.54(9) . 2 ? N1 Ni1 O4 87.75(11) . 2 ? N3 Ni1 O4 175.52(9) . 2 ? OW1 Ni1 O4 86.79(10) . 2 ? OW2 Ni1 O4 86.64(10) . 2 ? O6 S1 O5 119.80(18) . . ? O6 S1 C7 108.19(17) . . ? O5 S1 C7 107.56(17) . . ? O6 S1 C6 108.72(17) . . ? O5 S1 C6 108.22(17) . . ? C7 S1 C6 103.09(16) . . ? C13 O1 Ni1 130.2(2) . . ? Ni1 OW1 HW1B 121(3) . . ? Ni1 OW1 HW1A 99(3) . . ? HW1B OW1 HW1A 108.4(16) . . ? Ni1 OW2 HW2A 115(4) . . ? Ni1 OW2 HW2B 104(3) . . ? HW2A OW2 HW2B 109.0(17) . . ? HW4B OW4 HW4A 108.8(18) . . ? C14 O4 Ni1 129.9(2) . 2 ? C15 N1 C16 105.2(3) . . ? C15 N1 Ni1 128.1(2) . . ? C16 N1 Ni1 126.0(2) . . ? C15 N2 C17 106.8(3) . . ? C15 N2 C18 126.8(4) . . ? C17 N2 C18 126.4(4) . . ? C20 N3 C21 105.1(3) . . ? C20 N3 Ni1 125.6(2) . . ? C21 N3 Ni1 129.0(2) . . ? C20 N4 C22 107.1(3) . . ? C20 N4 C23 126.1(3) . . ? C22 N4 C23 126.6(3) . . ? C6 C1 C2 118.7(3) . . ? C6 C1 H1A 120.6 . . ? C2 C1 H1A 120.6 . . ? C1 C2 C3 120.4(3) . . ? C1 C2 H2A 119.8 . . ? C3 C2 H2A 119.8 . . ? C4 C3 C2 119.5(3) . . ? C4 C3 C13 120.2(3) . . ? C2 C3 C13 120.2(3) . . ? C3 C4 C5 121.0(3) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C4 C5 C6 118.3(3) . . ? C4 C5 H5A 120.8 . . ? C6 C5 H5A 120.8 . . ? C1 C6 C5 122.0(3) . . ? C1 C6 S1 119.4(3) . . ? C5 C6 S1 118.6(3) . . ? C12 C7 C8 121.8(3) . . ? C12 C7 S1 120.2(3) . . ? C8 C7 S1 118.0(3) . . ? C9 C8 C7 119.0(3) . . ? C9 C8 H8A 120.5 . . ? C7 C8 H8A 120.5 . . ? C8 C9 C10 119.8(3) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C9 C10 C11 120.0(3) . . ? C9 C10 C14 119.7(3) . . ? C11 C10 C14 120.3(3) . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C7 C12 C11 118.6(3) . . ? C7 C12 H12A 120.7 . . ? C11 C12 H12A 120.7 . . ? O2 C13 O1 125.2(3) . . ? O2 C13 C3 119.1(3) . . ? O1 C13 C3 115.7(3) . . ? O4 C14 O3 126.2(3) . . ? O4 C14 C10 117.4(3) . . ? O3 C14 C10 116.4(3) . . ? N1 C15 N2 111.5(3) . . ? N1 C15 H15A 124.2 . . ? N2 C15 H15A 124.2 . . ? N1 C16 C17 109.9(4) . . ? N1 C16 H16A 125.0 . . ? C17 C16 H16A 125.0 . . ? C16 C17 N2 106.6(4) . . ? C16 C17 H17A 126.7 . . ? N2 C17 H17A 126.7 . . ? N2 C18 C19 112.1(4) . . ? N2 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? N2 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C19 C19 C18 113.4(6) 2_355 . ? C19 C19 H19A 108.9 2_355 . ? C18 C19 H19A 108.9 . . ? C19 C19 H19B 108.9 2_355 . ? C18 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? N3 C20 N4 111.6(3) . . ? N3 C20 H20A 124.2 . . ? N4 C20 H20A 124.2 . . ? C22 C21 N3 109.7(3) . . ? C22 C21 H21A 125.2 . . ? N3 C21 H21A 125.2 . . ? N4 C22 C21 106.5(3) . . ? N4 C22 H22A 126.8 . . ? C21 C22 H22A 126.8 . . ? N4 C23 C24 111.4(3) . . ? N4 C23 H23A 109.4 . . ? C24 C23 H23A 109.4 . . ? N4 C23 H23B 109.4 . . ? C24 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C23 C24 C24 111.6(4) . 2_364 ? C23 C24 H24A 109.3 . . ? C24 C24 H24A 109.3 2_364 . ? C23 C24 H24B 109.3 . . ? C24 C24 H24B 109.3 2_364 . ? H24A C24 H24B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 O1 C13 -147.1(3) . . . . ? N3 Ni1 O1 C13 119.6(3) . . . . ? OW1 Ni1 O1 C13 17.5(18) . . . . ? OW2 Ni1 O1 C13 27.1(3) . . . . ? O4 Ni1 O1 C13 -59.5(3) 2 . . . ? O1 Ni1 N1 C15 139.8(3) . . . . ? N3 Ni1 N1 C15 -128.5(3) . . . . ? OW1 Ni1 N1 C15 -39.4(3) . . . . ? OW2 Ni1 N1 C15 84.0(8) . . . . ? O4 Ni1 N1 C15 47.1(3) 2 . . . ? O1 Ni1 N1 C16 -28.8(3) . . . . ? N3 Ni1 N1 C16 62.9(3) . . . . ? OW1 Ni1 N1 C16 152.0(3) . . . . ? OW2 Ni1 N1 C16 -84.6(8) . . . . ? O4 Ni1 N1 C16 -121.5(3) 2 . . . ? O1 Ni1 N3 C20 -166.1(3) . . . . ? N1 Ni1 N3 C20 107.2(3) . . . . ? OW1 Ni1 N3 C20 11.0(3) . . . . ? OW2 Ni1 N3 C20 -76.6(3) . . . . ? O4 Ni1 N3 C20 3.1(13) 2 . . . ? O1 Ni1 N3 C21 19.7(3) . . . . ? N1 Ni1 N3 C21 -67.0(3) . . . . ? OW1 Ni1 N3 C21 -163.2(3) . . . . ? OW2 Ni1 N3 C21 109.3(3) . . . . ? O4 Ni1 N3 C21 -171.1(11) 2 . . . ? C6 C1 C2 C3 -0.7(5) . . . . ? C1 C2 C3 C4 -0.3(5) . . . . ? C1 C2 C3 C13 -178.5(3) . . . . ? C2 C3 C4 C5 1.8(5) . . . . ? C13 C3 C4 C5 179.9(3) . . . . ? C3 C4 C5 C6 -2.1(5) . . . . ? C2 C1 C6 C5 0.3(5) . . . . ? C2 C1 C6 S1 -177.7(3) . . . . ? C4 C5 C6 C1 1.1(5) . . . . ? C4 C5 C6 S1 179.1(3) . . . . ? O6 S1 C6 C1 -40.4(3) . . . . ? O5 S1 C6 C1 -172.0(3) . . . . ? C7 S1 C6 C1 74.3(3) . . . . ? O6 S1 C6 C5 141.5(3) . . . . ? O5 S1 C6 C5 9.9(3) . . . . ? C7 S1 C6 C5 -103.8(3) . . . . ? O6 S1 C7 C12 0.1(4) . . . . ? O5 S1 C7 C12 130.9(3) . . . . ? C6 S1 C7 C12 -114.9(3) . . . . ? O6 S1 C7 C8 -178.7(3) . . . . ? O5 S1 C7 C8 -48.0(3) . . . . ? C6 S1 C7 C8 66.2(3) . . . . ? C12 C7 C8 C9 2.9(5) . . . . ? S1 C7 C8 C9 -178.3(3) . . . . ? C7 C8 C9 C10 -3.9(5) . . . . ? C8 C9 C10 C11 1.4(5) . . . . ? C8 C9 C10 C14 179.9(3) . . . . ? C9 C10 C11 C12 2.3(5) . . . . ? C14 C10 C11 C12 -176.2(3) . . . . ? C8 C7 C12 C11 0.7(6) . . . . ? S1 C7 C12 C11 -178.1(3) . . . . ? C10 C11 C12 C7 -3.3(6) . . . . ? Ni1 O1 C13 O2 -5.2(5) . . . . ? Ni1 O1 C13 C3 175.57(19) . . . . ? C4 C3 C13 O2 174.3(3) . . . . ? C2 C3 C13 O2 -7.5(5) . . . . ? C4 C3 C13 O1 -6.5(4) . . . . ? C2 C3 C13 O1 171.7(3) . . . . ? Ni1 O4 C14 O3 13.4(5) 2 . . . ? Ni1 O4 C14 C10 -165.2(2) 2 . . . ? C9 C10 C14 O4 -37.0(4) . . . . ? C11 C10 C14 O4 141.5(3) . . . . ? C9 C10 C14 O3 144.2(3) . . . . ? C11 C10 C14 O3 -37.2(5) . . . . ? C16 N1 C15 N2 0.4(5) . . . . ? Ni1 N1 C15 N2 -170.0(3) . . . . ? C17 N2 C15 N1 0.2(5) . . . . ? C18 N2 C15 N1 179.1(4) . . . . ? C15 N1 C16 C17 -0.9(5) . . . . ? Ni1 N1 C16 C17 169.9(3) . . . . ? N1 C16 C17 N2 1.0(6) . . . . ? C15 N2 C17 C16 -0.7(6) . . . . ? C18 N2 C17 C16 -179.6(4) . . . . ? C15 N2 C18 C19 114.8(5) . . . . ? C17 N2 C18 C19 -66.4(7) . . . . ? N2 C18 C19 C19 -64.6(8) . . . 2_355 ? C21 N3 C20 N4 -0.2(4) . . . . ? Ni1 N3 C20 N4 -175.5(2) . . . . ? C22 N4 C20 N3 0.4(4) . . . . ? C23 N4 C20 N3 176.3(3) . . . . ? C20 N3 C21 C22 0.0(4) . . . . ? Ni1 N3 C21 C22 175.1(2) . . . . ? C20 N4 C22 C21 -0.4(4) . . . . ? C23 N4 C22 C21 -176.3(3) . . . . ? N3 C21 C22 N4 0.2(4) . . . . ? C20 N4 C23 C24 -93.5(4) . . . . ? C22 N4 C23 C24 81.7(5) . . . . ? N4 C23 C24 C24 178.3(4) . . . 2_364 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OW2 HW2B O2 0.837(10) 1.93(2) 2.711(4) 154(4) . OW4 HW4A O2 0.83(6) 1.88(2) 2.702(5) 166(6) . OW2 HW2A O3 0.843(10) 1.980(14) 2.813(3) 169(4) 1_465 OW1 HW1B OW4 0.843(10) 1.927(14) 2.755(4) 167(3) 1_455 OW1 HW1A O3 0.842(10) 1.809(11) 2.645(3) 172(4) 2 OW1 HW1A O4 0.842(10) 2.50(3) 2.925(4) 112(3) 2 _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.345 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.141 data_c24b _database_code_depnum_ccdc_archive 'CCDC 808842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H46 N8 Ni2 O11' _chemical_formula_weight 1052.37 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 9.1045(3) _cell_length_b 19.8708(6) _cell_length_c 26.5094(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.067(2) _cell_angle_gamma 90.00 _cell_volume 4759.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 17765 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 27.56 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.862 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7029 _exptl_absorpt_correction_T_max 0.7409 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _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 'Bruker APEX 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 17765 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.56 _reflns_number_total 8836 _reflns_number_gt 7295 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0930P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(13) _refine_ls_number_reflns 8836 _refine_ls_number_parameters 650 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1386 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.71875(6) 0.14802(3) 0.13731(2) 0.04022(16) Uani 1 1 d . . . Ni2 Ni 0.85598(5) 0.10906(3) -0.54108(2) 0.03775(15) Uani 1 1 d . . . C1 C 0.5370(5) 0.0452(2) -0.01974(18) 0.0401(10) Uani 1 1 d . . . H1A H 0.5889 0.0121 -0.0002 0.048 Uiso 1 1 calc R . . C2 C 0.4812(6) 0.0311(2) -0.06913(18) 0.0432(11) Uani 1 1 d . . . H2A H 0.4978 -0.0110 -0.0827 0.052 Uiso 1 1 calc R . . C3 C 0.4002(6) 0.0788(2) -0.09907(18) 0.0416(10) Uani 1 1 d . . . C4 C 0.3785(6) 0.1428(2) -0.0776(2) 0.0474(12) Uani 1 1 d . . . H4A H 0.3238 0.1754 -0.0968 0.057 Uiso 1 1 calc R . . C5 C 0.4375(6) 0.1569(3) -0.0288(2) 0.0470(12) Uani 1 1 d . . . H5A H 0.4248 0.1995 -0.0154 0.056 Uiso 1 1 calc R . . C6 C 0.5172(5) 0.1077(2) 0.00137(18) 0.0411(10) Uani 1 1 d . . . C7 C 0.5858(5) 0.1227(2) 0.05359(18) 0.0399(10) Uani 1 1 d . . . C8 C 0.3338(6) 0.0641(3) -0.15098(19) 0.0492(12) Uani 1 1 d . . . C9 C 0.4021(6) 0.0112(2) -0.18192(16) 0.0400(10) Uani 1 1 d . . . C10 C 0.3181(6) -0.0357(3) -0.21065(19) 0.0502(12) Uani 1 1 d . . . H10A H 0.2184 -0.0409 -0.2070 0.060 Uiso 1 1 calc R . . C11 C 0.3823(6) -0.0753(3) -0.24512(19) 0.0488(12) Uani 1 1 d . . . H11A H 0.3254 -0.1072 -0.2644 0.059 Uiso 1 1 calc R . . C12 C 0.5302(6) -0.0677(2) -0.25092(16) 0.0407(10) Uani 1 1 d . . . C13 C 0.6144(6) -0.0214(3) -0.22072(19) 0.0473(12) Uani 1 1 d . . . H13A H 0.7140 -0.0159 -0.2244 0.057 Uiso 1 1 calc R . . C14 C 0.5525(7) 0.0164(3) -0.1856(2) 0.0543(14) Uani 1 1 d . . . H14A H 0.6111 0.0455 -0.1642 0.065 Uiso 1 1 calc R . . C15 C 0.5983(6) -0.1030(2) -0.29181(18) 0.0458(12) Uani 1 1 d . . . C16 C 0.8713(8) 0.2533(4) 0.2114(2) 0.0715(18) Uani 1 1 d . . . H16A H 0.9344 0.2228 0.2296 0.086 Uiso 1 1 calc R . . C17 C 0.7064(7) 0.2938(3) 0.1566(2) 0.0570(14) Uani 1 1 d . . . H17A H 0.6347 0.2979 0.1287 0.068 Uiso 1 1 calc R . . C18 C 0.8601(10) 0.3192(4) 0.2226(3) 0.085(2) Uani 1 1 d . . . H18A H 0.9169 0.3425 0.2485 0.103 Uiso 1 1 calc R . . C19 C 0.6852(15) 0.4092(5) 0.1937(5) 0.132(4) Uani 1 1 d DU . . H19A H 0.6872 0.4193 0.2295 0.132 Uiso 0.58(2) 1 calc PR A 1 H19B H 0.5822 0.4070 0.1791 0.132 Uiso 0.58(2) 1 calc PR A 1 H19C H 0.5929 0.4028 0.2078 0.132 Uiso 0.42(2) 1 d PR A 2 H19D H 0.7511 0.4336 0.2188 0.132 Uiso 0.42(2) 1 d PR A 2 C20 C 0.7583(17) 0.4666(5) 0.1688(4) 0.078(5) Uani 0.58(2) 1 d PDU A 1 H20A H 0.7047 0.5069 0.1761 0.078 Uiso 0.58(2) 1 calc PR A 1 H20B H 0.8567 0.4709 0.1872 0.078 Uiso 0.58(2) 1 calc PR A 1 C20A C 0.6533(19) 0.4502(11) 0.1470(7) 0.098(8) Uani 0.42(2) 1 d PDU A 2 H20C H 0.6078 0.4916 0.1567 0.098 Uiso 0.42(2) 1 calc PR A 2 H20D H 0.5786 0.4262 0.1246 0.098 Uiso 0.42(2) 1 calc PR A 2 C21 C 0.7769(12) 0.4702(5) 0.1147(3) 0.114(3) Uani 1 1 d DU . . H21A H 0.8766 0.4870 0.1137 0.114 Uiso 0.58(2) 1 calc PR A 1 H21B H 0.7776 0.4239 0.1032 0.114 Uiso 0.58(2) 1 calc PR A 1 H21C H 0.8545 0.4985 0.1319 0.114 Uiso 0.42(2) 1 d PR A 2 H21D H 0.8205 0.4301 0.1019 0.114 Uiso 0.42(2) 1 d PR A 2 C22 C 0.6852(7) 0.5064(4) 0.0746(2) 0.0679(17) Uani 1 1 d . A . H22A H 0.6148 0.4752 0.0569 0.081 Uiso 1 1 calc R . . H22B H 0.7479 0.5229 0.0502 0.081 Uiso 1 1 calc R . . C23 C 0.4595(6) 0.5670(3) 0.09678(19) 0.0496(12) Uani 1 1 d . A . H23A H 0.3927 0.5327 0.0867 0.059 Uiso 1 1 calc R . . C24 C 0.6652(6) 0.6225(3) 0.1129(2) 0.0611(15) Uani 1 1 d . A . H24A H 0.7648 0.6341 0.1158 0.073 Uiso 1 1 calc R . . C25 C 0.5542(6) 0.6599(3) 0.1274(2) 0.0513(13) Uani 1 1 d . A . H25A H 0.5647 0.7023 0.1422 0.062 Uiso 1 1 calc R . . C26 C 0.7885(5) 0.1472(2) -0.39912(17) 0.0373(10) Uani 1 1 d . . . C27 C 0.8313(5) 0.2094(2) -0.37804(18) 0.0417(10) Uani 1 1 d . . . H27A H 0.8601 0.2437 -0.3986 0.050 Uiso 1 1 calc R . . C28 C 0.8310(5) 0.2204(2) -0.32715(18) 0.0408(10) Uani 1 1 d . . . H28A H 0.8663 0.2609 -0.3128 0.049 Uiso 1 1 calc R . . C29 C 0.7778(6) 0.1709(2) -0.29656(18) 0.0438(11) Uani 1 1 d . . . C30 C 0.7283(6) 0.1102(3) -0.3182(2) 0.0479(12) Uani 1 1 d . . . H30A H 0.6899 0.0775 -0.2983 0.058 Uiso 1 1 calc R . . C31 C 0.7360(6) 0.0981(3) -0.36899(19) 0.0462(12) Uani 1 1 d . . . H31A H 0.7058 0.0568 -0.3831 0.055 Uiso 1 1 calc R . . C32 C 0.8061(5) 0.1339(2) -0.45404(18) 0.0384(10) Uani 1 1 d . . . C33 C 0.7684(6) 0.1826(3) -0.24143(18) 0.0476(12) Uani 1 1 d . . . C34 C 0.8739(6) 0.2297(2) -0.21121(17) 0.0430(11) Uani 1 1 d . . . C35 C 1.0232(6) 0.2308(3) -0.21649(19) 0.0485(12) Uani 1 1 d . . . H35A H 1.0574 0.2069 -0.2428 0.058 Uiso 1 1 calc R . . C36 C 1.1222(6) 0.2668(3) -0.18336(18) 0.0462(11) Uani 1 1 d . . . H36A H 1.2229 0.2649 -0.1862 0.055 Uiso 1 1 calc R . . C37 C 1.0717(6) 0.3059(3) -0.14577(16) 0.0415(11) Uani 1 1 d . . . C38 C 0.9215(6) 0.3071(3) -0.14142(19) 0.0509(12) Uani 1 1 d . . . H38A H 0.8864 0.3343 -0.1170 0.061 Uiso 1 1 calc R . . C39 C 0.8232(6) 0.2682(3) -0.1731(2) 0.0572(14) Uani 1 1 d . . . H39A H 0.7233 0.2677 -0.1688 0.069 Uiso 1 1 calc R . . C40 C 1.1786(6) 0.3426(2) -0.10812(17) 0.0421(11) Uani 1 1 d . . . C41 C 1.1416(6) 0.1725(2) -0.49437(18) 0.0419(11) Uani 1 1 d . . . H41A H 1.0903 0.2052 -0.4785 0.050 Uiso 1 1 calc R . . C42 C 1.1927(6) 0.0885(3) -0.5399(2) 0.0461(11) Uani 1 1 d . . . H42A H 1.1815 0.0515 -0.5615 0.055 Uiso 1 1 calc R . . C43 C 1.3240(6) 0.1147(3) -0.5195(2) 0.0504(12) Uani 1 1 d . . . H43A H 1.4180 0.0998 -0.5243 0.061 Uiso 1 1 calc R . . C44 C 1.3993(6) 0.2109(3) -0.4611(2) 0.0560(14) Uani 1 1 d . . . H44A H 1.4655 0.1831 -0.4385 0.067 Uiso 1 1 calc R . . H44B H 1.3494 0.2416 -0.4404 0.067 Uiso 1 1 calc R . . C45 C 1.4882(7) 0.2509(3) -0.4943(3) 0.0623(15) Uani 1 1 d . . . H45A H 1.5219 0.2212 -0.5196 0.075 Uiso 1 1 calc R . . H45B H 1.5750 0.2686 -0.4737 0.075 Uiso 1 1 calc R . . C46 C 1.4023(7) 0.3089(3) -0.5212(2) 0.0607(15) Uani 1 1 d . . . H46A H 1.3150 0.2919 -0.5420 0.073 Uiso 1 1 calc R . . H46B H 1.3706 0.3398 -0.4964 0.073 Uiso 1 1 calc R . . C47 C 1.4998(8) 0.3445(3) -0.5538(3) 0.080(2) Uani 1 1 d . . . H47A H 1.5133 0.3160 -0.5825 0.096 Uiso 1 1 calc R . . H47B H 1.5961 0.3511 -0.5343 0.096 Uiso 1 1 calc R . . C48 C 1.4073(7) 0.4623(3) -0.5448(2) 0.0545(14) Uani 1 1 d . . . H48A H 1.4015 0.4593 -0.5101 0.065 Uiso 1 1 calc R . . C49 C 1.4383(10) 0.4337(4) -0.6210(3) 0.083(2) Uani 1 1 d . . . H49A H 1.4560 0.4084 -0.6491 0.100 Uiso 1 1 calc R . . C50 C 1.4045(9) 0.4995(4) -0.6203(2) 0.0754(19) Uani 1 1 d . . . H50A H 1.3972 0.5283 -0.6482 0.090 Uiso 1 1 calc R . . N1 N 0.7763(5) 0.2387(2) 0.16940(16) 0.0468(10) Uani 1 1 d . . . N2 N 0.7499(8) 0.3449(3) 0.1889(2) 0.0752(17) Uani 1 1 d . A . N3 N 0.6024(5) 0.5643(2) 0.09296(16) 0.0501(10) Uani 1 1 d . . . N4 N 0.4229(5) 0.62546(19) 0.11707(15) 0.0440(9) Uani 1 1 d . . . N5 N 1.0783(5) 0.1248(2) -0.52380(15) 0.0406(9) Uani 1 1 d . . . N6 N 1.2891(4) 0.1680(2) -0.49015(15) 0.0415(9) Uani 1 1 d . . . N7 N 1.4413(6) 0.4119(2) -0.5735(2) 0.0638(13) Uani 1 1 d . . . N8 N 1.3826(5) 0.5172(2) -0.57192(16) 0.0460(9) Uani 1 1 d . . . O1 O 0.6111(4) 0.18310(16) 0.06750(12) 0.0471(8) Uani 1 1 d . . . OW1 O 1.4679(9) 0.3745(4) -0.2049(3) 0.138(3) Uani 1 1 d . . . O2 O 0.6216(4) 0.07434(16) 0.08397(13) 0.0467(8) Uani 1 1 d . . . O3 O 0.5203(4) -0.13947(18) -0.32351(13) 0.0484(8) Uani 1 1 d . . . O4 O 0.7345(5) -0.0947(2) -0.29528(14) 0.0554(10) Uani 1 1 d . . . O5 O 0.2210(6) 0.0930(2) -0.17013(17) 0.0736(12) Uani 1 1 d . . . O6 O 0.8183(4) 0.18232(16) -0.48353(12) 0.0428(7) Uani 1 1 d . . . O7 O 0.8165(4) 0.07324(16) -0.46882(12) 0.0458(8) Uani 1 1 d . . . O8 O 1.3155(4) 0.3362(2) -0.10955(13) 0.0512(9) Uani 1 1 d . . . O9 O 1.1298(4) 0.37767(18) -0.07425(12) 0.0444(8) Uani 1 1 d . . . O10 O 0.6741(6) 0.1540(2) -0.22033(16) 0.0747(13) 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 Ni1 0.0463(4) 0.0335(3) 0.0408(3) 0.0010(2) 0.0053(2) 0.0006(3) Ni2 0.0417(3) 0.0330(3) 0.0374(3) 0.0019(2) 0.0001(2) 0.0003(3) C1 0.044(3) 0.029(2) 0.048(3) 0.0031(19) 0.006(2) 0.0058(19) C2 0.054(3) 0.034(2) 0.042(2) 0.0006(19) 0.007(2) 0.009(2) C3 0.046(3) 0.033(2) 0.046(3) 0.0013(19) 0.008(2) 0.009(2) C4 0.056(3) 0.037(3) 0.048(3) 0.001(2) 0.000(2) 0.017(2) C5 0.050(3) 0.033(2) 0.058(3) -0.004(2) 0.005(2) 0.013(2) C6 0.041(3) 0.037(2) 0.045(2) -0.0006(19) 0.008(2) 0.003(2) C7 0.041(3) 0.033(2) 0.046(2) 0.0036(19) 0.006(2) 0.0047(19) C8 0.049(3) 0.051(3) 0.049(3) 0.004(2) 0.009(2) 0.016(2) C9 0.049(3) 0.032(2) 0.038(2) 0.0028(18) 0.003(2) 0.003(2) C10 0.045(3) 0.063(3) 0.043(3) 0.002(2) 0.008(2) 0.000(2) C11 0.057(3) 0.043(3) 0.046(3) -0.005(2) 0.004(2) -0.004(2) C12 0.047(3) 0.040(3) 0.035(2) 0.0047(19) 0.0067(19) -0.001(2) C13 0.046(3) 0.048(3) 0.049(3) -0.004(2) 0.008(2) -0.009(2) C14 0.066(4) 0.049(3) 0.049(3) -0.010(2) 0.011(3) -0.012(3) C15 0.053(3) 0.043(3) 0.043(3) -0.001(2) 0.011(2) -0.007(2) C16 0.084(5) 0.072(4) 0.055(3) -0.018(3) -0.008(3) 0.013(4) C17 0.063(4) 0.042(3) 0.068(3) -0.007(2) 0.017(3) -0.002(3) C18 0.090(6) 0.092(6) 0.076(4) -0.037(4) 0.016(4) -0.031(5) C19 0.156(8) 0.087(6) 0.161(7) -0.041(6) 0.054(6) 0.006(6) C20 0.112(9) 0.060(6) 0.060(6) -0.002(5) 0.000(6) 0.028(6) C20A 0.092(11) 0.083(10) 0.122(11) -0.013(8) 0.018(8) 0.018(8) C21 0.126(7) 0.091(6) 0.124(6) -0.002(5) 0.012(5) 0.038(5) C22 0.066(4) 0.069(4) 0.070(4) -0.015(3) 0.012(3) 0.016(3) C23 0.052(3) 0.043(3) 0.052(3) -0.003(2) 0.005(2) -0.001(2) C24 0.039(3) 0.071(4) 0.073(4) 0.000(3) 0.003(3) -0.008(3) C25 0.041(3) 0.040(3) 0.071(3) -0.003(2) 0.001(2) -0.002(2) C26 0.035(2) 0.034(2) 0.042(2) -0.0001(18) -0.0020(19) 0.0035(18) C27 0.045(3) 0.034(2) 0.046(2) 0.0099(19) 0.001(2) -0.0021(19) C28 0.041(3) 0.033(2) 0.047(3) -0.0028(19) 0.000(2) -0.0047(19) C29 0.050(3) 0.039(2) 0.041(2) -0.0018(19) 0.000(2) -0.012(2) C30 0.049(3) 0.046(3) 0.048(3) 0.004(2) 0.001(2) -0.014(2) C31 0.047(3) 0.037(2) 0.053(3) -0.008(2) -0.001(2) -0.010(2) C32 0.030(2) 0.041(2) 0.043(2) 0.001(2) -0.0005(18) 0.0003(19) C33 0.047(3) 0.053(3) 0.040(3) 0.004(2) -0.006(2) -0.012(2) C34 0.047(3) 0.042(3) 0.038(2) 0.001(2) -0.002(2) -0.010(2) C35 0.050(3) 0.052(3) 0.041(3) -0.010(2) -0.003(2) 0.004(2) C36 0.044(3) 0.049(3) 0.044(3) -0.006(2) 0.000(2) 0.003(2) C37 0.050(3) 0.040(3) 0.033(2) -0.0014(18) -0.001(2) 0.001(2) C38 0.050(3) 0.059(3) 0.043(3) -0.012(2) 0.002(2) 0.002(2) C39 0.048(3) 0.076(4) 0.047(3) -0.012(3) 0.003(2) -0.007(3) C40 0.044(3) 0.044(3) 0.036(2) -0.0015(19) 0.001(2) 0.007(2) C41 0.041(3) 0.035(2) 0.050(3) -0.002(2) 0.007(2) 0.007(2) C42 0.041(3) 0.043(3) 0.057(3) -0.011(2) 0.015(2) -0.007(2) C43 0.048(3) 0.044(3) 0.060(3) -0.002(2) 0.010(2) 0.012(2) C44 0.039(3) 0.058(3) 0.067(3) -0.013(3) -0.007(2) 0.001(2) C45 0.043(3) 0.050(3) 0.092(4) -0.019(3) 0.004(3) -0.004(3) C46 0.051(3) 0.042(3) 0.092(4) -0.014(3) 0.018(3) 0.003(2) C47 0.069(4) 0.043(3) 0.137(6) -0.014(4) 0.046(4) 0.003(3) C48 0.065(4) 0.041(3) 0.059(3) -0.007(2) 0.015(3) 0.004(2) C49 0.121(6) 0.065(4) 0.067(4) -0.033(3) 0.025(4) -0.019(4) C50 0.104(5) 0.074(4) 0.050(3) -0.014(3) 0.014(3) -0.020(4) N1 0.047(3) 0.038(2) 0.055(2) -0.0050(18) 0.0069(19) -0.0046(18) N2 0.100(5) 0.043(3) 0.088(4) -0.018(3) 0.033(4) -0.013(3) N3 0.046(3) 0.053(3) 0.050(2) -0.003(2) 0.0038(19) 0.003(2) N4 0.051(3) 0.034(2) 0.047(2) -0.0004(18) 0.0093(19) -0.0007(18) N5 0.043(2) 0.037(2) 0.041(2) 0.0019(16) 0.0042(17) 0.0014(17) N6 0.036(2) 0.041(2) 0.047(2) -0.0059(17) 0.0022(17) 0.0013(17) N7 0.068(3) 0.043(2) 0.085(4) -0.015(2) 0.028(3) -0.010(2) N8 0.048(2) 0.038(2) 0.050(2) -0.0051(19) -0.0004(18) -0.0019(18) O1 0.064(2) 0.0334(18) 0.0438(17) -0.0015(14) 0.0044(15) -0.0026(15) OW1 0.107(5) 0.134(6) 0.171(7) -0.057(5) 0.014(5) -0.007(4) O2 0.052(2) 0.0337(17) 0.0532(19) 0.0030(15) 0.0023(15) 0.0023(15) O3 0.054(2) 0.046(2) 0.0456(18) -0.0084(16) 0.0074(16) -0.0065(16) O4 0.058(3) 0.061(2) 0.049(2) -0.0148(17) 0.0121(18) -0.0098(19) O5 0.082(3) 0.071(3) 0.065(3) -0.008(2) -0.004(2) 0.028(3) O6 0.049(2) 0.0365(18) 0.0422(17) 0.0020(14) 0.0034(14) 0.0040(15) O7 0.061(2) 0.0341(18) 0.0417(17) -0.0019(13) 0.0014(15) 0.0025(15) O8 0.048(2) 0.055(2) 0.049(2) -0.0164(17) 0.0002(16) 0.0025(18) O9 0.051(2) 0.0417(18) 0.0403(18) -0.0076(14) 0.0039(15) 0.0027(15) O10 0.095(4) 0.078(3) 0.052(2) -0.006(2) 0.009(2) -0.041(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.033(4) . ? Ni1 N4 2.046(4) 3_545 ? Ni1 O4 2.067(3) 2 ? Ni1 O1 2.104(3) . ? Ni1 O2 2.149(3) . ? Ni1 O3 2.199(4) 2 ? Ni1 C7 2.446(5) . ? Ni1 C15 2.458(5) 2 ? Ni2 N8 2.027(4) 3_445 ? Ni2 N5 2.043(4) . ? Ni2 O8 2.109(3) 4_454 ? Ni2 O7 2.115(3) . ? Ni2 O9 2.153(4) 4_454 ? Ni2 O6 2.166(3) . ? Ni2 C40 2.446(5) 4_454 ? Ni2 C32 2.456(5) . ? C1 C2 1.374(7) . ? C1 C6 1.383(7) . ? C1 H1A 0.9300 . ? C2 C3 1.389(7) . ? C2 H2A 0.9300 . ? C3 C4 1.416(7) . ? C3 C8 1.463(7) . ? C4 C5 1.367(8) . ? C4 H4A 0.9300 . ? C5 C6 1.408(7) . ? C5 H5A 0.9300 . ? C6 C7 1.478(7) . ? C7 O1 1.268(6) . ? C7 O2 1.271(6) . ? C8 O5 1.230(7) . ? C8 C9 1.513(7) . ? C9 C10 1.375(7) . ? C9 C14 1.388(8) . ? C10 C11 1.388(7) . ? C10 H10A 0.9300 . ? C11 C12 1.382(7) . ? C11 H11A 0.9300 . ? C12 C13 1.388(7) . ? C12 C15 1.489(7) . ? C13 C14 1.371(7) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 O3 1.261(6) . ? C15 O4 1.265(7) . ? C15 Ni1 2.458(5) 2_554 ? C16 C18 1.348(10) . ? C16 N1 1.354(8) . ? C16 H16A 0.9300 . ? C17 N1 1.291(7) . ? C17 N2 1.355(8) . ? C17 H17A 0.9300 . ? C18 N2 1.360(11) . ? C18 H18A 0.9300 . ? C19 N2 1.418(11) . ? C19 C20A 1.479(10) . ? C19 C20 1.511(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C19 H19D 0.9700 . ? C20 C21 1.467(8) . ? C20 H19D 1.4874 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H21C 1.5292 . ? C20A C21 1.548(10) . ? C20A H20C 0.9700 . ? C20A H20D 0.9700 . ? C21 C22 1.459(11) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9699 . ? C21 H21D 0.9699 . ? C22 N3 1.490(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N3 1.319(7) . ? C23 N4 1.339(6) . ? C23 H23A 0.9300 . ? C24 C25 1.348(8) . ? C24 N3 1.367(7) . ? C24 H24A 0.9300 . ? C25 N4 1.375(7) . ? C25 H25A 0.9300 . ? C26 C31 1.382(7) . ? C26 C27 1.393(7) . ? C26 C32 1.507(7) . ? C27 C28 1.367(7) . ? C27 H27A 0.9300 . ? C28 C29 1.398(6) . ? C28 H28A 0.9300 . ? C29 C30 1.387(7) . ? C29 C33 1.493(7) . ? C30 C31 1.379(7) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 O6 1.253(6) . ? C32 O7 1.275(6) . ? C33 O10 1.221(7) . ? C33 C34 1.500(7) . ? C34 C35 1.384(7) . ? C34 C39 1.391(7) . ? C35 C36 1.378(7) . ? C35 H35A 0.9300 . ? C36 C37 1.385(7) . ? C36 H36A 0.9300 . ? C37 C38 1.386(8) . ? C37 C40 1.496(7) . ? C38 C39 1.385(8) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C40 O8 1.258(6) . ? C40 O9 1.260(6) . ? C40 Ni2 2.446(5) 4 ? C41 N5 1.315(6) . ? C41 N6 1.337(6) . ? C41 H41A 0.9300 . ? C42 C43 1.354(8) . ? C42 N5 1.377(6) . ? C42 H42A 0.9300 . ? C43 N6 1.373(6) . ? C43 H43A 0.9300 . ? C44 N6 1.462(7) . ? C44 C45 1.495(9) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C46 1.521(9) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.491(9) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 N7 1.510(9) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 N8 1.311(7) . ? C48 N7 1.317(7) . ? C48 H48A 0.9300 . ? C49 N7 1.329(9) . ? C49 C50 1.345(10) . ? C49 H49A 0.9300 . ? C50 N8 1.368(7) . ? C50 H50A 0.9300 . ? N4 Ni1 2.046(4) 3_455 ? N8 Ni2 2.027(4) 3 ? O3 Ni1 2.199(4) 2_554 ? O4 Ni1 2.067(3) 2_554 ? O8 Ni2 2.109(3) 4 ? O9 Ni2 2.153(4) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N4 96.21(17) . 3_545 ? N1 Ni1 O4 96.04(18) . 2 ? N4 Ni1 O4 98.39(16) 3_545 2 ? N1 Ni1 O1 98.21(16) . . ? N4 Ni1 O1 100.48(15) 3_545 . ? O4 Ni1 O1 154.90(15) 2 . ? N1 Ni1 O2 160.58(16) . . ? N4 Ni1 O2 89.52(15) 3_545 . ? O4 Ni1 O2 101.47(15) 2 . ? O1 Ni1 O2 62.45(12) . . ? N1 Ni1 O3 93.16(15) . 2 ? N4 Ni1 O3 158.83(14) 3_545 2 ? O4 Ni1 O3 61.67(14) 2 2 ? O1 Ni1 O3 96.90(14) . 2 ? O2 Ni1 O3 87.86(14) . 2 ? N1 Ni1 C7 129.43(17) . . ? N4 Ni1 C7 94.65(16) 3_545 . ? O4 Ni1 C7 130.78(17) 2 . ? O1 Ni1 C7 31.22(14) . . ? O2 Ni1 C7 31.27(14) . . ? O3 Ni1 C7 93.97(15) 2 . ? N1 Ni1 C15 96.83(17) . 2 ? N4 Ni1 C15 128.72(17) 3_545 2 ? O4 Ni1 C15 30.96(17) 2 2 ? O1 Ni1 C15 126.14(17) . 2 ? O2 Ni1 C15 93.94(16) . 2 ? O3 Ni1 C15 30.78(15) 2 2 ? C7 Ni1 C15 113.66(17) . 2 ? N8 Ni2 N5 93.67(17) 3_445 . ? N8 Ni2 O8 97.70(16) 3_445 4_454 ? N5 Ni2 O8 100.22(15) . 4_454 ? N8 Ni2 O7 95.99(15) 3_445 . ? N5 Ni2 O7 97.03(15) . . ? O8 Ni2 O7 157.18(14) 4_454 . ? N8 Ni2 O9 95.80(16) 3_445 4_454 ? N5 Ni2 O9 160.70(14) . 4_454 ? O8 Ni2 O9 61.87(13) 4_454 4_454 ? O7 Ni2 O9 98.66(13) . 4_454 ? N8 Ni2 O6 157.88(15) 3_445 . ? N5 Ni2 O6 88.73(15) . . ? O8 Ni2 O6 103.51(14) 4_454 . ? O7 Ni2 O6 61.91(12) . . ? O9 Ni2 O6 88.79(13) 4_454 . ? N8 Ni2 C40 99.28(17) 3_445 4_454 ? N5 Ni2 C40 130.54(16) . 4_454 ? O8 Ni2 C40 30.96(15) 4_454 4_454 ? O7 Ni2 C40 128.29(15) . 4_454 ? O9 Ni2 C40 30.97(14) 4_454 4_454 ? O6 Ni2 C40 95.76(14) . 4_454 ? N8 Ni2 C32 127.24(16) 3_445 . ? N5 Ni2 C32 92.94(15) . . ? O8 Ni2 C32 132.23(16) 4_454 . ? O7 Ni2 C32 31.26(14) . . ? O9 Ni2 C32 94.64(14) 4_454 . ? O6 Ni2 C32 30.65(14) . . ? C40 Ni2 C32 114.95(16) 4_454 . ? C2 C1 C6 121.2(4) . . ? C2 C1 H1A 119.4 . . ? C6 C1 H1A 119.4 . . ? C1 C2 C3 120.9(4) . . ? C1 C2 H2A 119.6 . . ? C3 C2 H2A 119.6 . . ? C2 C3 C4 118.3(4) . . ? C2 C3 C8 122.0(4) . . ? C4 C3 C8 119.7(4) . . ? C5 C4 C3 120.4(4) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C6 120.7(4) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C1 C6 C5 118.5(4) . . ? C1 C6 C7 120.0(4) . . ? C5 C6 C7 121.4(4) . . ? O1 C7 O2 120.6(4) . . ? O1 C7 C6 120.3(4) . . ? O2 C7 C6 119.1(4) . . ? O1 C7 Ni1 59.3(2) . . ? O2 C7 Ni1 61.4(2) . . ? C6 C7 Ni1 175.3(3) . . ? O5 C8 C3 121.5(5) . . ? O5 C8 C9 118.6(5) . . ? C3 C8 C9 119.9(4) . . ? C10 C9 C14 119.9(4) . . ? C10 C9 C8 122.2(5) . . ? C14 C9 C8 117.4(4) . . ? C9 C10 C11 119.9(5) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C12 C11 C10 120.4(5) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C11 C12 C13 119.0(4) . . ? C11 C12 C15 121.9(5) . . ? C13 C12 C15 118.8(4) . . ? C14 C13 C12 120.7(5) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C9 119.9(5) . . ? C13 C14 H14A 120.1 . . ? C9 C14 H14A 120.1 . . ? O3 C15 O4 120.2(4) . . ? O3 C15 C12 120.3(5) . . ? O4 C15 C12 119.5(4) . . ? O3 C15 Ni1 63.2(3) . 2_554 ? O4 C15 Ni1 57.2(2) . 2_554 ? C12 C15 Ni1 173.3(4) . 2_554 ? C18 C16 N1 109.5(7) . . ? C18 C16 H16A 125.3 . . ? N1 C16 H16A 125.3 . . ? N1 C17 N2 112.0(6) . . ? N1 C17 H17A 124.0 . . ? N2 C17 H17A 124.0 . . ? C16 C18 N2 106.8(6) . . ? C16 C18 H18A 126.6 . . ? N2 C18 H18A 126.6 . . ? N2 C19 C20A 117.5(11) . . ? N2 C19 C20 115.5(9) . . ? C20A C19 C20 43.3(9) . . ? N2 C19 H19A 108.4 . . ? C20A C19 H19A 133.2 . . ? C20 C19 H19A 108.4 . . ? N2 C19 H19B 108.4 . . ? C20A C19 H19B 67.1 . . ? C20 C19 H19B 108.4 . . ? H19A C19 H19B 107.5 . . ? N2 C19 H19C 107.8 . . ? C20A C19 H19C 107.7 . . ? C20 C19 H19C 135.7 . . ? H19A C19 H19C 63.9 . . ? H19B C19 H19C 46.1 . . ? N2 C19 H19D 106.5 . . ? C20A C19 H19D 109.9 . . ? C20 C19 H19D 69.8 . . ? H19A C19 H19D 44.5 . . ? H19B C19 H19D 141.4 . . ? H19C C19 H19D 106.9 . . ? C21 C20 C19 125.0(10) . . ? C21 C20 H19D 156.4 . . ? C19 C20 H19D 37.7 . . ? C21 C20 H20A 106.1 . . ? C19 C20 H20A 106.1 . . ? H19D C20 H20A 96.1 . . ? C21 C20 H20B 106.1 . . ? C19 C20 H20B 106.1 . . ? H19D C20 H20B 74.3 . . ? H20A C20 H20B 106.3 . . ? C21 C20 H21C 37.7 . . ? C19 C20 H21C 155.4 . . ? H19D C20 H21C 147.6 . . ? H20A C20 H21C 97.3 . . ? H20B C20 H21C 73.7 . . ? C19 C20A C21 121.5(11) . . ? C19 C20A H20C 106.9 . . ? C21 C20A H20C 106.9 . . ? C19 C20A H20D 106.9 . . ? C21 C20A H20D 106.9 . . ? H20C C20A H20D 106.7 . . ? C22 C21 C20 127.8(9) . . ? C22 C21 C20A 98.1(9) . . ? C20 C21 C20A 42.8(9) . . ? C22 C21 H21A 105.4 . . ? C20 C21 H21A 105.4 . . ? C20A C21 H21A 148.2 . . ? C22 C21 H21B 105.4 . . ? C20 C21 H21B 105.4 . . ? C20A C21 H21B 87.8 . . ? H21A C21 H21B 106.0 . . ? C22 C21 H21C 112.1 . . ? C20 C21 H21C 74.6 . . ? C20A C21 H21C 115.2 . . ? H21A C21 H21C 35.4 . . ? H21B C21 H21C 131.6 . . ? C22 C21 H21D 111.9 . . ? C20 C21 H21D 113.7 . . ? C20A C21 H21D 109.7 . . ? H21A C21 H21D 81.3 . . ? H21B C21 H21D 24.7 . . ? H21C C21 H21D 109.5 . . ? C21 C22 N3 114.1(6) . . ? C21 C22 H22A 108.7 . . ? N3 C22 H22A 108.7 . . ? C21 C22 H22B 108.7 . . ? N3 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? N3 C23 N4 111.3(5) . . ? N3 C23 H23A 124.4 . . ? N4 C23 H23A 124.4 . . ? C25 C24 N3 106.5(5) . . ? C25 C24 H24A 126.8 . . ? N3 C24 H24A 126.8 . . ? C24 C25 N4 109.5(5) . . ? C24 C25 H25A 125.3 . . ? N4 C25 H25A 125.3 . . ? C31 C26 C27 119.6(4) . . ? C31 C26 C32 121.3(4) . . ? C27 C26 C32 119.1(4) . . ? C28 C27 C26 120.2(4) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C27 C28 C29 120.2(4) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C30 C29 C28 119.4(4) . . ? C30 C29 C33 119.0(4) . . ? C28 C29 C33 121.6(4) . . ? C31 C30 C29 120.1(4) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C26 120.3(4) . . ? C30 C31 H31A 119.8 . . ? C26 C31 H31A 119.8 . . ? O6 C32 O7 121.2(4) . . ? O6 C32 C26 119.7(4) . . ? O7 C32 C26 118.9(4) . . ? O6 C32 Ni2 61.8(2) . . ? O7 C32 Ni2 59.4(2) . . ? C26 C32 Ni2 175.2(3) . . ? O10 C33 C29 120.3(5) . . ? O10 C33 C34 119.1(4) . . ? C29 C33 C34 120.7(4) . . ? C35 C34 C39 118.9(5) . . ? C35 C34 C33 121.9(5) . . ? C39 C34 C33 118.8(5) . . ? C36 C35 C34 121.1(5) . . ? C36 C35 H35A 119.4 . . ? C34 C35 H35A 119.4 . . ? C35 C36 C37 120.0(5) . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C36 C37 C38 119.2(5) . . ? C36 C37 C40 120.5(5) . . ? C38 C37 C40 120.2(4) . . ? C39 C38 C37 120.7(5) . . ? C39 C38 H38A 119.6 . . ? C37 C38 H38A 119.6 . . ? C38 C39 C34 119.9(5) . . ? C38 C39 H39A 120.0 . . ? C34 C39 H39A 120.0 . . ? O8 C40 O9 121.0(4) . . ? O8 C40 C37 119.8(4) . . ? O9 C40 C37 119.2(4) . . ? O8 C40 Ni2 59.6(2) . 4 ? O9 C40 Ni2 61.6(3) . 4 ? C37 C40 Ni2 173.5(4) . 4 ? N5 C41 N6 111.3(4) . . ? N5 C41 H41A 124.3 . . ? N6 C41 H41A 124.3 . . ? C43 C42 N5 109.8(4) . . ? C43 C42 H42A 125.1 . . ? N5 C42 H42A 125.1 . . ? C42 C43 N6 105.6(5) . . ? C42 C43 H43A 127.2 . . ? N6 C43 H43A 127.2 . . ? N6 C44 C45 112.7(5) . . ? N6 C44 H44A 109.0 . . ? C45 C44 H44A 109.0 . . ? N6 C44 H44B 109.0 . . ? C45 C44 H44B 109.0 . . ? H44A C44 H44B 107.8 . . ? C44 C45 C46 113.2(5) . . ? C44 C45 H45A 108.9 . . ? C46 C45 H45A 108.9 . . ? C44 C45 H45B 108.9 . . ? C46 C45 H45B 108.9 . . ? H45A C45 H45B 107.8 . . ? C47 C46 C45 108.8(5) . . ? C47 C46 H46A 109.9 . . ? C45 C46 H46A 109.9 . . ? C47 C46 H46B 109.9 . . ? C45 C46 H46B 109.9 . . ? H46A C46 H46B 108.3 . . ? C46 C47 N7 114.3(5) . . ? C46 C47 H47A 108.7 . . ? N7 C47 H47A 108.7 . . ? C46 C47 H47B 108.7 . . ? N7 C47 H47B 108.7 . . ? H47A C47 H47B 107.6 . . ? N8 C48 N7 110.7(5) . . ? N8 C48 H48A 124.6 . . ? N7 C48 H48A 124.6 . . ? N7 C49 C50 106.5(5) . . ? N7 C49 H49A 126.8 . . ? C50 C49 H49A 126.8 . . ? C49 C50 N8 108.8(6) . . ? C49 C50 H50A 125.6 . . ? N8 C50 H50A 125.6 . . ? C17 N1 C16 106.0(5) . . ? C17 N1 Ni1 123.3(4) . . ? C16 N1 Ni1 129.8(4) . . ? C18 N2 C17 105.5(6) . . ? C18 N2 C19 124.1(8) . . ? C17 N2 C19 129.7(9) . . ? C23 N3 C24 107.8(4) . . ? C23 N3 C22 126.9(5) . . ? C24 N3 C22 125.2(5) . . ? C23 N4 C25 105.0(4) . . ? C23 N4 Ni1 125.1(4) . 3_455 ? C25 N4 Ni1 129.3(3) . 3_455 ? C41 N5 C42 105.6(4) . . ? C41 N5 Ni2 126.4(3) . . ? C42 N5 Ni2 128.1(3) . . ? C41 N6 C43 107.7(4) . . ? C41 N6 C44 128.4(4) . . ? C43 N6 C44 123.8(4) . . ? C48 N7 C49 108.6(5) . . ? C48 N7 C47 125.0(6) . . ? C49 N7 C47 125.6(6) . . ? C48 N8 C50 105.4(5) . . ? C48 N8 Ni2 123.4(3) . 3 ? C50 N8 Ni2 130.4(4) . 3 ? C7 O1 Ni1 89.4(3) . . ? C7 O2 Ni1 87.4(3) . . ? C15 O3 Ni1 86.1(3) . 2_554 ? C15 O4 Ni1 91.8(3) . 2_554 ? C32 O6 Ni2 87.6(3) . . ? C32 O7 Ni2 89.3(3) . . ? C40 O8 Ni2 89.5(3) . 4 ? C40 O9 Ni2 87.4(3) . 4 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.4(8) . . . . ? C1 C2 C3 C4 0.9(8) . . . . ? C1 C2 C3 C8 -177.1(5) . . . . ? C2 C3 C4 C5 0.7(8) . . . . ? C8 C3 C4 C5 178.7(5) . . . . ? C3 C4 C5 C6 -1.7(8) . . . . ? C2 C1 C6 C5 0.4(7) . . . . ? C2 C1 C6 C7 -176.4(5) . . . . ? C4 C5 C6 C1 1.2(8) . . . . ? C4 C5 C6 C7 178.0(5) . . . . ? C1 C6 C7 O1 156.8(5) . . . . ? C5 C6 C7 O1 -19.9(7) . . . . ? C1 C6 C7 O2 -21.9(7) . . . . ? C5 C6 C7 O2 161.4(5) . . . . ? C1 C6 C7 Ni1 72(4) . . . . ? C5 C6 C7 Ni1 -104(4) . . . . ? N1 Ni1 C7 O1 -0.6(4) . . . . ? N4 Ni1 C7 O1 -102.6(3) 3_545 . . . ? O4 Ni1 C7 O1 152.1(3) 2 . . . ? O2 Ni1 C7 O1 176.0(4) . . . . ? O3 Ni1 C7 O1 96.8(3) 2 . . . ? C15 Ni1 C7 O1 121.3(3) 2 . . . ? N1 Ni1 C7 O2 -176.7(3) . . . . ? N4 Ni1 C7 O2 81.4(3) 3_545 . . . ? O4 Ni1 C7 O2 -23.9(4) 2 . . . ? O1 Ni1 C7 O2 -176.0(4) . . . . ? O3 Ni1 C7 O2 -79.3(3) 2 . . . ? C15 Ni1 C7 O2 -54.8(3) 2 . . . ? N1 Ni1 C7 C6 87(4) . . . . ? N4 Ni1 C7 C6 -15(4) 3_545 . . . ? O4 Ni1 C7 C6 -121(4) 2 . . . ? O1 Ni1 C7 C6 87(4) . . . . ? O2 Ni1 C7 C6 -97(4) . . . . ? O3 Ni1 C7 C6 -176(4) 2 . . . ? C15 Ni1 C7 C6 -152(4) 2 . . . ? C2 C3 C8 O5 151.4(6) . . . . ? C4 C3 C8 O5 -26.6(8) . . . . ? C2 C3 C8 C9 -27.3(8) . . . . ? C4 C3 C8 C9 154.7(5) . . . . ? O5 C8 C9 C10 -42.7(8) . . . . ? C3 C8 C9 C10 136.1(5) . . . . ? O5 C8 C9 C14 129.5(6) . . . . ? C3 C8 C9 C14 -51.7(7) . . . . ? C14 C9 C10 C11 -3.3(7) . . . . ? C8 C9 C10 C11 168.7(5) . . . . ? C9 C10 C11 C12 -0.3(8) . . . . ? C10 C11 C12 C13 1.9(8) . . . . ? C10 C11 C12 C15 -172.2(5) . . . . ? C11 C12 C13 C14 0.1(8) . . . . ? C15 C12 C13 C14 174.4(5) . . . . ? C12 C13 C14 C9 -3.7(8) . . . . ? C10 C9 C14 C13 5.3(8) . . . . ? C8 C9 C14 C13 -167.1(5) . . . . ? C11 C12 C15 O3 2.2(7) . . . . ? C13 C12 C15 O3 -171.9(4) . . . . ? C11 C12 C15 O4 -179.5(5) . . . . ? C13 C12 C15 O4 6.4(7) . . . . ? C11 C12 C15 Ni1 122(3) . . . 2_554 ? C13 C12 C15 Ni1 -52(4) . . . 2_554 ? N1 C16 C18 N2 3.7(8) . . . . ? N2 C19 C20 C21 58.2(17) . . . . ? C20A C19 C20 C21 -45.6(13) . . . . ? N2 C19 C20A C21 -58(2) . . . . ? C20 C19 C20A C21 40.6(12) . . . . ? C19 C20 C21 C22 98.4(15) . . . . ? C19 C20 C21 C20A 43.5(12) . . . . ? C19 C20A C21 C22 178.2(16) . . . . ? C19 C20A C21 C20 -42.5(12) . . . . ? C20 C21 C22 N3 24.4(14) . . . . ? C20A C21 C22 N3 58.6(12) . . . . ? N3 C24 C25 N4 0.3(7) . . . . ? C31 C26 C27 C28 4.4(7) . . . . ? C32 C26 C27 C28 -173.2(4) . . . . ? C26 C27 C28 C29 -4.6(7) . . . . ? C27 C28 C29 C30 1.4(8) . . . . ? C27 C28 C29 C33 -176.7(5) . . . . ? C28 C29 C30 C31 2.0(8) . . . . ? C33 C29 C30 C31 -179.9(5) . . . . ? C29 C30 C31 C26 -2.1(8) . . . . ? C27 C26 C31 C30 -1.1(8) . . . . ? C32 C26 C31 C30 176.5(5) . . . . ? C31 C26 C32 O6 162.6(5) . . . . ? C27 C26 C32 O6 -19.9(7) . . . . ? C31 C26 C32 O7 -21.3(7) . . . . ? C27 C26 C32 O7 156.3(4) . . . . ? C31 C26 C32 Ni2 -90(4) . . . . ? C27 C26 C32 Ni2 87(4) . . . . ? N8 Ni2 C32 O6 179.4(3) 3_445 . . . ? N5 Ni2 C32 O6 82.5(3) . . . . ? O8 Ni2 C32 O6 -24.1(4) 4_454 . . . ? O7 Ni2 C32 O6 -178.8(4) . . . . ? O9 Ni2 C32 O6 -79.7(3) 4_454 . . . ? C40 Ni2 C32 O6 -55.4(3) 4_454 . . . ? N8 Ni2 C32 O7 -1.9(3) 3_445 . . . ? N5 Ni2 C32 O7 -98.7(3) . . . . ? O8 Ni2 C32 O7 154.6(3) 4_454 . . . ? O9 Ni2 C32 O7 99.0(3) 4_454 . . . ? O6 Ni2 C32 O7 178.8(4) . . . . ? C40 Ni2 C32 O7 123.4(3) 4_454 . . . ? N8 Ni2 C32 C26 70(4) 3_445 . . . ? N5 Ni2 C32 C26 -27(4) . . . . ? O8 Ni2 C32 C26 -134(4) 4_454 . . . ? O7 Ni2 C32 C26 71(4) . . . . ? O9 Ni2 C32 C26 171(4) 4_454 . . . ? O6 Ni2 C32 C26 -110(4) . . . . ? C40 Ni2 C32 C26 -165(4) 4_454 . . . ? C30 C29 C33 O10 -27.3(8) . . . . ? C28 C29 C33 O10 150.8(6) . . . . ? C30 C29 C33 C34 152.9(5) . . . . ? C28 C29 C33 C34 -29.0(8) . . . . ? O10 C33 C34 C35 138.0(6) . . . . ? C29 C33 C34 C35 -42.2(7) . . . . ? O10 C33 C34 C39 -35.0(8) . . . . ? C29 C33 C34 C39 144.8(5) . . . . ? C39 C34 C35 C36 2.9(8) . . . . ? C33 C34 C35 C36 -170.2(5) . . . . ? C34 C35 C36 C37 -3.8(8) . . . . ? C35 C36 C37 C38 1.3(8) . . . . ? C35 C36 C37 C40 177.2(5) . . . . ? C36 C37 C38 C39 2.1(8) . . . . ? C40 C37 C38 C39 -173.8(5) . . . . ? C37 C38 C39 C34 -3.0(9) . . . . ? C35 C34 C39 C38 0.5(8) . . . . ? C33 C34 C39 C38 173.8(5) . . . . ? C36 C37 C40 O8 -2.4(7) . . . . ? C38 C37 C40 O8 173.5(5) . . . . ? C36 C37 C40 O9 -179.9(4) . . . . ? C38 C37 C40 O9 -4.0(7) . . . . ? C36 C37 C40 Ni2 -85(3) . . . 4 ? C38 C37 C40 Ni2 91(3) . . . 4 ? N5 C42 C43 N6 0.2(6) . . . . ? N6 C44 C45 C46 73.9(6) . . . . ? C44 C45 C46 C47 -179.1(5) . . . . ? C45 C46 C47 N7 -167.0(6) . . . . ? N7 C49 C50 N8 -1.8(9) . . . . ? N2 C17 N1 C16 -0.6(7) . . . . ? N2 C17 N1 Ni1 169.9(4) . . . . ? C18 C16 N1 C17 -1.9(7) . . . . ? C18 C16 N1 Ni1 -171.6(5) . . . . ? N4 Ni1 N1 C17 126.3(4) 3_545 . . . ? O4 Ni1 N1 C17 -134.5(4) 2 . . . ? O1 Ni1 N1 C17 24.7(4) . . . . ? O2 Ni1 N1 C17 19.8(8) . . . . ? O3 Ni1 N1 C17 -72.7(4) 2 . . . ? C7 Ni1 N1 C17 25.1(5) . . . . ? C15 Ni1 N1 C17 -103.4(4) 2 . . . ? N4 Ni1 N1 C16 -65.6(5) 3_545 . . . ? O4 Ni1 N1 C16 33.5(5) 2 . . . ? O1 Ni1 N1 C16 -167.2(5) . . . . ? O2 Ni1 N1 C16 -172.1(5) . . . . ? O3 Ni1 N1 C16 95.4(5) 2 . . . ? C7 Ni1 N1 C16 -166.9(5) . . . . ? C15 Ni1 N1 C16 64.7(5) 2 . . . ? C16 C18 N2 C17 -3.9(8) . . . . ? C16 C18 N2 C19 167.7(8) . . . . ? N1 C17 N2 C18 2.9(7) . . . . ? N1 C17 N2 C19 -168.1(7) . . . . ? C20A C19 N2 C18 138.7(11) . . . . ? C20 C19 N2 C18 90.1(12) . . . . ? C20A C19 N2 C17 -51.9(15) . . . . ? C20 C19 N2 C17 -100.5(12) . . . . ? N4 C23 N3 C24 1.8(6) . . . . ? N4 C23 N3 C22 177.0(5) . . . . ? C25 C24 N3 C23 -1.3(6) . . . . ? C25 C24 N3 C22 -176.5(5) . . . . ? C21 C22 N3 C23 -105.9(8) . . . . ? C21 C22 N3 C24 68.4(9) . . . . ? N3 C23 N4 C25 -1.6(6) . . . . ? N3 C23 N4 Ni1 -173.0(3) . . . 3_455 ? C24 C25 N4 C23 0.7(6) . . . . ? C24 C25 N4 Ni1 171.7(4) . . . 3_455 ? N6 C41 N5 C42 -1.1(5) . . . . ? N6 C41 N5 Ni2 178.8(3) . . . . ? C43 C42 N5 C41 0.5(6) . . . . ? C43 C42 N5 Ni2 -179.4(3) . . . . ? N8 Ni2 N5 C41 -167.8(4) 3_445 . . . ? O8 Ni2 N5 C41 93.7(4) 4_454 . . . ? O7 Ni2 N5 C41 -71.3(4) . . . . ? O9 Ni2 N5 C41 72.9(6) 4_454 . . . ? O6 Ni2 N5 C41 -9.8(4) . . . . ? C40 Ni2 N5 C41 86.7(4) 4_454 . . . ? C32 Ni2 N5 C41 -40.2(4) . . . . ? N8 Ni2 N5 C42 12.0(4) 3_445 . . . ? O8 Ni2 N5 C42 -86.5(4) 4_454 . . . ? O7 Ni2 N5 C42 108.5(4) . . . . ? O9 Ni2 N5 C42 -107.3(5) 4_454 . . . ? O6 Ni2 N5 C42 170.0(4) . . . . ? C40 Ni2 N5 C42 -93.5(4) 4_454 . . . ? C32 Ni2 N5 C42 139.6(4) . . . . ? N5 C41 N6 C43 1.2(6) . . . . ? N5 C41 N6 C44 -179.9(5) . . . . ? C42 C43 N6 C41 -0.9(6) . . . . ? C42 C43 N6 C44 -179.8(5) . . . . ? C45 C44 N6 C41 -113.3(6) . . . . ? C45 C44 N6 C43 65.4(7) . . . . ? N8 C48 N7 C49 -0.4(8) . . . . ? N8 C48 N7 C47 169.8(6) . . . . ? C50 C49 N7 C48 1.4(9) . . . . ? C50 C49 N7 C47 -168.8(6) . . . . ? C46 C47 N7 C48 56.9(9) . . . . ? C46 C47 N7 C49 -134.5(7) . . . . ? N7 C48 N8 C50 -0.7(7) . . . . ? N7 C48 N8 Ni2 -170.9(4) . . . 3 ? C49 C50 N8 C48 1.5(8) . . . . ? C49 C50 N8 Ni2 170.8(5) . . . 3 ? O2 C7 O1 Ni1 4.0(5) . . . . ? C6 C7 O1 Ni1 -174.6(4) . . . . ? N1 Ni1 O1 C7 179.5(3) . . . . ? N4 Ni1 O1 C7 81.6(3) 3_545 . . . ? O4 Ni1 O1 C7 -56.5(5) 2 . . . ? O2 Ni1 O1 C7 -2.3(3) . . . . ? O3 Ni1 O1 C7 -86.3(3) 2 . . . ? C15 Ni1 O1 C7 -75.8(3) 2 . . . ? O1 C7 O2 Ni1 -4.0(4) . . . . ? C6 C7 O2 Ni1 174.7(4) . . . . ? N1 Ni1 O2 C7 7.8(6) . . . . ? N4 Ni1 O2 C7 -99.8(3) 3_545 . . . ? O4 Ni1 O2 C7 161.8(3) 2 . . . ? O1 Ni1 O2 C7 2.3(3) . . . . ? O3 Ni1 O2 C7 101.2(3) 2 . . . ? C15 Ni1 O2 C7 131.4(3) 2 . . . ? O4 C15 O3 Ni1 -4.8(5) . . . 2_554 ? C12 C15 O3 Ni1 173.5(4) . . . 2_554 ? O3 C15 O4 Ni1 5.1(5) . . . 2_554 ? C12 C15 O4 Ni1 -173.2(4) . . . 2_554 ? O7 C32 O6 Ni2 -1.2(4) . . . . ? C26 C32 O6 Ni2 174.8(4) . . . . ? N8 Ni2 O6 C32 -1.3(6) 3_445 . . . ? N5 Ni2 O6 C32 -97.9(3) . . . . ? O8 Ni2 O6 C32 161.9(3) 4_454 . . . ? O7 Ni2 O6 C32 0.7(3) . . . . ? O9 Ni2 O6 C32 101.2(3) 4_454 . . . ? C40 Ni2 O6 C32 131.4(3) 4_454 . . . ? O6 C32 O7 Ni2 1.3(5) . . . . ? C26 C32 O7 Ni2 -174.8(4) . . . . ? N8 Ni2 O7 C32 178.5(3) 3_445 . . . ? N5 Ni2 O7 C32 84.1(3) . . . . ? O8 Ni2 O7 C32 -54.9(5) 4_454 . . . ? O9 Ni2 O7 C32 -84.7(3) 4_454 . . . ? O6 Ni2 O7 C32 -0.7(3) . . . . ? C40 Ni2 O7 C32 -74.7(3) 4_454 . . . ? O9 C40 O8 Ni2 4.8(5) . . . 4 ? C37 C40 O8 Ni2 -172.6(4) . . . 4 ? O8 C40 O9 Ni2 -4.7(5) . . . 4 ? C37 C40 O9 Ni2 172.7(4) . . . 4 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.182 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.076 data_x20b _database_code_depnum_ccdc_archive 'CCDC 808844' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H50 Co3 N4 O24 S4' _chemical_formula_weight 1708.23 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.502(2) _cell_length_b 13.122(3) _cell_length_c 13.598(3) _cell_angle_alpha 95.81(3) _cell_angle_beta 108.69(3) _cell_angle_gamma 109.68(3) _cell_volume 1779.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15461 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 871 _exptl_absorpt_coefficient_mu 0.895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7389 _exptl_absorpt_correction_T_max 0.7814 _exptl_absorpt_process_details 'SADABS(Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku RAXIS RAPID IP' _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15461 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.1071 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6950 _reflns_number_gt 4273 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _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^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6950 _refine_ls_number_parameters 502 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1350 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.15446(6) -0.17998(5) 0.02465(4) 0.02910(17) Uani 1 1 d . . . Co2 Co 0.0000 0.0000 0.0000 0.0245(2) Uani 1 2 d S . . S1 S 0.50343(12) 0.25826(11) -0.33608(8) 0.0392(3) Uani 1 1 d . . . S2 S -0.67481(12) -0.44476(11) -0.37689(9) 0.0393(3) Uani 1 1 d . . . O1 O 0.2559(3) -0.0868(3) -0.0538(2) 0.0388(8) Uani 1 1 d . . . O2 O 0.1678(3) 0.0397(3) -0.0393(2) 0.0359(8) Uani 1 1 d . . . O3 O 0.0988(3) 0.0105(3) -0.8427(2) 0.0355(8) Uani 1 1 d . . . O4 O 0.2515(3) -0.0627(3) -0.8320(2) 0.0384(8) Uani 1 1 d . . . O5 O 0.4846(4) 0.3611(3) -0.3294(3) 0.0575(11) Uani 1 1 d . . . O6 O 0.6363(3) 0.2597(3) -0.3077(2) 0.0511(10) Uani 1 1 d . . . O7 O -0.0335(3) -0.1703(2) -0.0384(2) 0.0315(7) Uani 1 1 d . . . O8 O -0.0117(3) -0.2885(3) -0.1500(3) 0.0476(9) Uani 1 1 d . . . O9 O -0.9627(5) -0.1010(4) -0.5697(3) 0.0783(13) Uani 1 1 d . . . O10 O -0.9333(5) -0.0523(4) -0.3994(3) 0.0759(13) Uani 1 1 d . . . O11 O -0.7235(3) -0.4952(3) -0.3019(3) 0.0540(10) Uani 1 1 d . . . O12 O -0.7001(3) -0.5113(3) -0.4775(3) 0.0540(10) Uani 1 1 d . . . N1 N 0.2404(3) -0.2989(3) 0.0250(2) 0.0306(9) Uani 1 1 d . . . N2 N 0.0658(4) -0.2912(3) 0.1076(3) 0.0360(9) Uani 1 1 d . . . C1 C 0.3072(4) 0.0649(4) -0.1353(3) 0.0302(10) Uani 1 1 d . . . C2 C 0.2676(5) 0.1445(4) -0.1765(4) 0.0440(13) Uani 1 1 d . . . H2A H 0.2001 0.1591 -0.1623 0.053 Uiso 1 1 calc R . . C3 C 0.3261(5) 0.2034(5) -0.2385(4) 0.0466(13) Uani 1 1 d . . . H3A H 0.2975 0.2562 -0.2669 0.056 Uiso 1 1 calc R . . C4 C 0.4278(4) 0.1825(4) -0.2577(3) 0.0328(11) Uani 1 1 d . . . C5 C 0.4721(5) 0.1055(4) -0.2153(3) 0.0352(11) Uani 1 1 d . . . H5A H 0.5420 0.0935 -0.2275 0.042 Uiso 1 1 calc R . . C6 C 0.4120(4) 0.0461(4) -0.1545(3) 0.0342(11) Uani 1 1 d . . . H6A H 0.4411 -0.0066 -0.1261 0.041 Uiso 1 1 calc R . . C7 C 0.4105(4) 0.1778(4) -0.4686(3) 0.0316(10) Uani 1 1 d . . . C8 C 0.2902(5) 0.1794(4) -0.5256(3) 0.0452(13) Uani 1 1 d . . . H8A H 0.2540 0.2202 -0.4939 0.054 Uiso 1 1 calc R . . C9 C 0.2219(5) 0.1201(4) -0.6310(3) 0.0392(12) Uani 1 1 d . . . H9A H 0.1398 0.1213 -0.6703 0.047 Uiso 1 1 calc R . . C10 C 0.2758(4) 0.0588(4) -0.6782(3) 0.0310(10) Uani 1 1 d . . . C11 C 0.3983(5) 0.0592(5) -0.6193(3) 0.0481(14) Uani 1 1 d . . . H11A H 0.4357 0.0196 -0.6511 0.058 Uiso 1 1 calc R . . C12 C 0.4665(5) 0.1173(4) -0.5138(3) 0.0474(14) Uani 1 1 d . . . H12A H 0.5482 0.1159 -0.4739 0.057 Uiso 1 1 calc R . . C13 C 0.2383(4) 0.0013(4) -0.0710(3) 0.0313(10) Uani 1 1 d . . . C14 C 0.2027(4) -0.0022(4) -0.7944(3) 0.0335(11) Uani 1 1 d . . . C15 C -0.2282(4) -0.2862(4) -0.1913(3) 0.0320(10) Uani 1 1 d . . . C16 C -0.2810(4) -0.3575(4) -0.2910(3) 0.0379(11) Uani 1 1 d . . . H16A H -0.2248 -0.3771 -0.3181 0.045 Uiso 1 1 calc R . . C17 C -0.4150(5) -0.3995(4) -0.3500(3) 0.0395(12) Uani 1 1 d . . . H17A H -0.4492 -0.4463 -0.4174 0.047 Uiso 1 1 calc R . . C18 C -0.4996(4) -0.3729(4) -0.3102(3) 0.0330(10) Uani 1 1 d . . . C19 C -0.4477(5) -0.2989(4) -0.2112(3) 0.0409(12) Uani 1 1 d . . . H19A H -0.5040 -0.2788 -0.1847 0.049 Uiso 1 1 calc R . . C20 C -0.3134(5) -0.2560(4) -0.1531(3) 0.0394(12) Uani 1 1 d . . . H20A H -0.2786 -0.2061 -0.0873 0.047 Uiso 1 1 calc R . . C21 C -0.7420(5) -0.3419(4) -0.4025(3) 0.0404(12) Uani 1 1 d . . . C22 C -0.7619(5) -0.3130(5) -0.5003(4) 0.0494(14) Uani 1 1 d . . . H22A H -0.7371 -0.3446 -0.5504 0.059 Uiso 1 1 calc R . . C23 C -0.8194(5) -0.2366(5) -0.5219(4) 0.0541(15) Uani 1 1 d . . . H23A H -0.8323 -0.2157 -0.5867 0.065 Uiso 1 1 calc R . . C24 C -0.8581(5) -0.1908(4) -0.4469(4) 0.0464(13) Uani 1 1 d . . . C25 C -0.8363(6) -0.2196(5) -0.3494(4) 0.0527(14) Uani 1 1 d . . . H25A H -0.8600 -0.1877 -0.2987 0.063 Uiso 1 1 calc R . . C26 C -0.7792(5) -0.2957(4) -0.3282(4) 0.0457(13) Uani 1 1 d . . . H26A H -0.7656 -0.3162 -0.2632 0.055 Uiso 1 1 calc R . . C27 C -0.0835(4) -0.2455(4) -0.1257(3) 0.0326(10) Uani 1 1 d . . . C28 C -0.9200(5) -0.1082(5) -0.4715(5) 0.0553(15) Uani 1 1 d . . . C29 C 0.3285(5) -0.2977(4) -0.0184(3) 0.0411(12) Uani 1 1 d . . . H29A H 0.3551 -0.2404 -0.0516 0.049 Uiso 1 1 calc R . . C30 C 0.3827(6) -0.3760(5) -0.0173(4) 0.0610(16) Uani 1 1 d . . . H30A H 0.4443 -0.3725 -0.0488 0.073 Uiso 1 1 calc R . . C31 C 0.3430(6) -0.4596(5) 0.0319(5) 0.0644(17) Uani 1 1 d . . . H31A H 0.3780 -0.5141 0.0345 0.077 Uiso 1 1 calc R . . C32 C 0.2523(6) -0.4634(4) 0.0771(4) 0.0495(14) Uani 1 1 d . . . H32A H 0.2249 -0.5202 0.1106 0.059 Uiso 1 1 calc R . . C33 C 0.2012(4) -0.3814(4) 0.0725(3) 0.0332(10) Uani 1 1 d . . . C34 C 0.1034(4) -0.3772(4) 0.1203(3) 0.0342(10) Uani 1 1 d . . . C35 C 0.0546(5) -0.4529(4) 0.1755(4) 0.0451(12) Uani 1 1 d . . . H35A H 0.0805 -0.5125 0.1828 0.054 Uiso 1 1 calc R . . C36 C -0.0325(5) -0.4390(5) 0.2192(4) 0.0520(14) Uani 1 1 d . . . H36A H -0.0657 -0.4888 0.2571 0.062 Uiso 1 1 calc R . . C37 C -0.0705(6) -0.3516(5) 0.2068(5) 0.0596(16) Uani 1 1 d . . . H37A H -0.1296 -0.3411 0.2361 0.071 Uiso 1 1 calc R . . C38 C -0.0201(5) -0.2804(5) 0.1510(4) 0.0494(14) Uani 1 1 d . . . H38B H -0.0466 -0.2212 0.1425 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0276(3) 0.0308(4) 0.0303(3) 0.0082(3) 0.0101(3) 0.0136(3) Co2 0.0216(4) 0.0282(5) 0.0213(4) 0.0043(3) 0.0056(3) 0.0098(4) S1 0.0387(7) 0.0383(7) 0.0254(5) 0.0035(5) 0.0100(5) 0.0002(6) S2 0.0275(6) 0.0394(7) 0.0408(6) 0.0044(5) 0.0087(5) 0.0063(6) O1 0.045(2) 0.037(2) 0.0456(17) 0.0164(15) 0.0254(16) 0.0203(17) O2 0.0341(18) 0.0381(19) 0.0399(17) 0.0062(14) 0.0210(15) 0.0135(16) O3 0.0317(19) 0.045(2) 0.0259(14) 0.0053(14) 0.0028(13) 0.0184(16) O4 0.0359(19) 0.044(2) 0.0306(15) -0.0010(14) 0.0061(14) 0.0188(17) O5 0.089(3) 0.030(2) 0.0426(18) 0.0036(16) 0.024(2) 0.013(2) O6 0.0259(19) 0.071(3) 0.0345(16) 0.0060(17) 0.0076(14) -0.0009(18) O7 0.0297(17) 0.0277(17) 0.0286(14) 0.0065(13) 0.0022(13) 0.0095(15) O8 0.036(2) 0.046(2) 0.054(2) -0.0017(17) 0.0059(16) 0.0228(18) O9 0.101(4) 0.084(3) 0.068(3) 0.025(2) 0.031(3) 0.056(3) O10 0.084(3) 0.077(3) 0.082(3) 0.019(2) 0.031(3) 0.050(3) O11 0.041(2) 0.054(2) 0.065(2) 0.0189(19) 0.0284(18) 0.0072(19) O12 0.037(2) 0.054(2) 0.0474(19) -0.0159(17) 0.0017(16) 0.0112(18) N1 0.030(2) 0.037(2) 0.0218(16) 0.0024(16) 0.0084(15) 0.0117(18) N2 0.030(2) 0.038(2) 0.041(2) 0.0135(18) 0.0147(17) 0.0130(19) C1 0.030(2) 0.033(3) 0.028(2) 0.0074(19) 0.0111(19) 0.013(2) C2 0.046(3) 0.062(4) 0.056(3) 0.029(3) 0.036(3) 0.038(3) C3 0.053(3) 0.059(4) 0.052(3) 0.033(3) 0.030(3) 0.036(3) C4 0.029(3) 0.043(3) 0.0208(19) 0.0009(19) 0.0055(18) 0.013(2) C5 0.034(3) 0.043(3) 0.036(2) 0.011(2) 0.017(2) 0.019(2) C6 0.031(3) 0.041(3) 0.040(2) 0.015(2) 0.016(2) 0.021(2) C7 0.027(2) 0.034(3) 0.026(2) 0.0062(19) 0.0065(18) 0.007(2) C8 0.044(3) 0.058(4) 0.031(2) 0.000(2) 0.012(2) 0.023(3) C9 0.032(3) 0.048(3) 0.029(2) 0.004(2) 0.004(2) 0.015(2) C10 0.028(2) 0.034(3) 0.025(2) 0.0105(19) 0.0037(18) 0.011(2) C11 0.047(3) 0.063(4) 0.031(2) -0.003(2) 0.002(2) 0.034(3) C12 0.042(3) 0.067(4) 0.029(2) 0.003(2) 0.003(2) 0.029(3) C13 0.027(2) 0.031(3) 0.027(2) 0.0011(19) 0.0055(19) 0.006(2) C14 0.032(3) 0.032(3) 0.025(2) 0.0045(19) 0.0043(19) 0.005(2) C15 0.028(3) 0.023(2) 0.037(2) 0.0050(19) 0.009(2) 0.005(2) C16 0.027(3) 0.037(3) 0.042(2) 0.000(2) 0.011(2) 0.009(2) C17 0.038(3) 0.040(3) 0.033(2) -0.003(2) 0.010(2) 0.013(2) C18 0.026(2) 0.034(3) 0.033(2) 0.011(2) 0.0071(19) 0.007(2) C19 0.034(3) 0.048(3) 0.039(2) 0.001(2) 0.016(2) 0.015(2) C20 0.035(3) 0.038(3) 0.037(2) 0.002(2) 0.011(2) 0.008(2) C21 0.030(3) 0.049(3) 0.037(2) 0.003(2) 0.011(2) 0.013(2) C22 0.042(3) 0.070(4) 0.041(3) 0.014(3) 0.016(2) 0.027(3) C23 0.052(4) 0.069(4) 0.051(3) 0.027(3) 0.022(3) 0.030(3) C24 0.037(3) 0.043(3) 0.061(3) 0.011(3) 0.019(3) 0.018(3) C25 0.056(4) 0.059(4) 0.048(3) 0.006(3) 0.022(3) 0.028(3) C26 0.046(3) 0.056(3) 0.037(2) 0.016(2) 0.014(2) 0.023(3) C27 0.031(3) 0.022(2) 0.035(2) 0.0084(19) 0.004(2) 0.006(2) C28 0.041(3) 0.052(4) 0.068(4) 0.012(3) 0.017(3) 0.016(3) C29 0.042(3) 0.055(3) 0.036(2) 0.009(2) 0.018(2) 0.027(3) C30 0.070(4) 0.073(4) 0.067(4) 0.022(3) 0.040(3) 0.045(4) C31 0.080(5) 0.070(4) 0.072(4) 0.028(3) 0.035(4) 0.055(4) C32 0.067(4) 0.041(3) 0.057(3) 0.022(3) 0.027(3) 0.034(3) C33 0.029(3) 0.033(3) 0.029(2) 0.0012(19) 0.0042(19) 0.009(2) C34 0.030(3) 0.031(3) 0.035(2) 0.005(2) 0.007(2) 0.010(2) C35 0.049(3) 0.034(3) 0.053(3) 0.016(2) 0.021(3) 0.013(3) C36 0.049(3) 0.049(3) 0.059(3) 0.027(3) 0.028(3) 0.010(3) C37 0.060(4) 0.066(4) 0.074(4) 0.026(3) 0.045(3) 0.028(3) C38 0.045(3) 0.058(4) 0.068(3) 0.029(3) 0.034(3) 0.031(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.024(3) . ? Co1 O4 2.062(3) 1_556 ? Co1 O7 2.108(3) . ? Co1 N1 2.110(4) . ? Co1 N2 2.124(4) . ? Co2 O3 2.041(3) 1_556 ? Co2 O3 2.041(3) 2_554 ? Co2 O2 2.080(3) . ? Co2 O2 2.080(3) 2 ? Co2 O7 2.114(3) 2 ? Co2 O7 2.114(3) . ? S1 O5 1.435(4) . ? S1 O6 1.444(3) . ? S1 C4 1.762(5) . ? S1 C7 1.767(4) . ? S2 O11 1.429(3) . ? S2 O12 1.432(3) . ? S2 C18 1.774(5) . ? S2 C21 1.780(5) . ? O1 C13 1.270(5) . ? O2 C13 1.245(5) . ? O3 C14 1.241(5) . ? O3 Co2 2.041(3) 1_554 ? O4 C14 1.269(5) . ? O4 Co1 2.062(3) 1_554 ? O7 C27 1.288(5) . ? O8 C27 1.250(5) . ? O9 C28 1.292(7) . ? O10 C28 1.244(6) . ? N1 C29 1.323(5) . ? N1 C33 1.338(6) . ? N2 C38 1.340(5) . ? N2 C34 1.346(6) . ? C1 C2 1.375(6) . ? C1 C6 1.404(6) . ? C1 C13 1.495(6) . ? C2 C3 1.380(6) . ? C2 H2A 0.9300 . ? C3 C4 1.382(6) . ? C3 H3A 0.9300 . ? C4 C5 1.375(6) . ? C5 C6 1.379(6) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.360(6) . ? C7 C12 1.387(6) . ? C8 C9 1.385(6) . ? C8 H8A 0.9300 . ? C9 C10 1.389(6) . ? C9 H9A 0.9300 . ? C10 C11 1.378(6) . ? C10 C14 1.510(5) . ? C11 C12 1.382(6) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C15 C16 1.384(6) . ? C15 C20 1.390(6) . ? C15 C27 1.484(6) . ? C16 C17 1.367(6) . ? C16 H16A 0.9300 . ? C17 C18 1.374(6) . ? C17 H17A 0.9300 . ? C18 C19 1.394(6) . ? C19 C20 1.366(6) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C26 1.379(6) . ? C21 C22 1.389(7) . ? C22 C23 1.382(7) . ? C22 H22A 0.9300 . ? C23 C24 1.396(6) . ? C23 H23A 0.9300 . ? C24 C25 1.384(7) . ? C24 C28 1.495(7) . ? C25 C26 1.375(7) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C29 C30 1.369(7) . ? C29 H29A 0.9300 . ? C30 C31 1.366(8) . ? C30 H30A 0.9300 . ? C31 C32 1.360(7) . ? C31 H31A 0.9300 . ? C32 C33 1.387(6) . ? C32 H32A 0.9300 . ? C33 C34 1.481(6) . ? C34 C35 1.383(6) . ? C35 C36 1.368(6) . ? C35 H35A 0.9300 . ? C36 C37 1.364(7) . ? C36 H36A 0.9300 . ? C37 C38 1.359(7) . ? C37 H37A 0.9300 . ? C38 H38B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O4 95.25(13) . 1_556 ? O1 Co1 O7 102.33(12) . . ? O4 Co1 O7 103.98(11) 1_556 . ? O1 Co1 N1 95.23(13) . . ? O4 Co1 N1 110.52(13) 1_556 . ? O7 Co1 N1 139.45(13) . . ? O1 Co1 N2 171.63(13) . . ? O4 Co1 N2 86.90(14) 1_556 . ? O7 Co1 N2 84.94(13) . . ? N1 Co1 N2 76.47(14) . . ? O3 Co2 O3 180.00(8) 1_556 2_554 ? O3 Co2 O2 95.42(12) 1_556 . ? O3 Co2 O2 84.58(12) 2_554 . ? O3 Co2 O2 84.58(12) 1_556 2 ? O3 Co2 O2 95.42(12) 2_554 2 ? O2 Co2 O2 180.0(2) . 2 ? O3 Co2 O7 89.45(12) 1_556 2 ? O3 Co2 O7 90.55(12) 2_554 2 ? O2 Co2 O7 90.73(12) . 2 ? O2 Co2 O7 89.27(12) 2 2 ? O3 Co2 O7 90.55(12) 1_556 . ? O3 Co2 O7 89.45(12) 2_554 . ? O2 Co2 O7 89.27(12) . . ? O2 Co2 O7 90.73(12) 2 . ? O7 Co2 O7 180.00(15) 2 . ? O5 S1 O6 119.9(2) . . ? O5 S1 C4 107.7(2) . . ? O6 S1 C4 108.2(2) . . ? O5 S1 C7 108.1(2) . . ? O6 S1 C7 106.9(2) . . ? C4 S1 C7 105.1(2) . . ? O11 S2 O12 120.3(2) . . ? O11 S2 C18 106.8(2) . . ? O12 S2 C18 108.0(2) . . ? O11 S2 C21 106.2(2) . . ? O12 S2 C21 108.0(2) . . ? C18 S2 C21 106.8(2) . . ? C13 O1 Co1 118.6(3) . . ? C13 O2 Co2 144.9(3) . . ? C14 O3 Co2 132.7(3) . 1_554 ? C14 O4 Co1 125.4(3) . 1_554 ? C27 O7 Co1 98.3(2) . . ? C27 O7 Co2 134.9(3) . . ? Co1 O7 Co2 106.55(13) . . ? C29 N1 C33 118.5(4) . . ? C29 N1 Co1 124.8(3) . . ? C33 N1 Co1 116.7(3) . . ? C38 N2 C34 117.9(4) . . ? C38 N2 Co1 125.5(3) . . ? C34 N2 Co1 116.6(3) . . ? C2 C1 C6 118.8(4) . . ? C2 C1 C13 119.3(4) . . ? C6 C1 C13 121.9(4) . . ? C1 C2 C3 121.3(4) . . ? C1 C2 H2A 119.4 . . ? C3 C2 H2A 119.4 . . ? C2 C3 C4 119.0(5) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C3 121.1(4) . . ? C5 C4 S1 119.8(3) . . ? C3 C4 S1 119.0(4) . . ? C4 C5 C6 119.5(4) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C5 C6 C1 120.2(4) . . ? C5 C6 H6A 119.9 . . ? C1 C6 H6A 119.9 . . ? C8 C7 C12 121.3(4) . . ? C8 C7 S1 120.7(3) . . ? C12 C7 S1 118.0(3) . . ? C7 C8 C9 119.8(4) . . ? C7 C8 H8A 120.1 . . ? C9 C8 H8A 120.1 . . ? C8 C9 C10 120.1(4) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 119.2(4) . . ? C11 C10 C14 121.2(4) . . ? C9 C10 C14 119.6(4) . . ? C10 C11 C12 121.1(4) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C11 C12 C7 118.6(4) . . ? C11 C12 H12A 120.7 . . ? C7 C12 H12A 120.7 . . ? O2 C13 O1 125.7(4) . . ? O2 C13 C1 116.6(4) . . ? O1 C13 C1 117.7(4) . . ? O3 C14 O4 126.6(4) . . ? O3 C14 C10 116.1(4) . . ? O4 C14 C10 117.2(4) . . ? C16 C15 C20 118.9(4) . . ? C16 C15 C27 120.1(4) . . ? C20 C15 C27 121.0(4) . . ? C17 C16 C15 120.6(4) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C16 C17 C18 120.4(4) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C17 C18 C19 119.7(4) . . ? C17 C18 S2 120.0(3) . . ? C19 C18 S2 119.8(3) . . ? C20 C19 C18 119.6(4) . . ? C20 C19 H19A 120.2 . . ? C18 C19 H19A 120.2 . . ? C19 C20 C15 120.7(4) . . ? C19 C20 H20A 119.6 . . ? C15 C20 H20A 119.6 . . ? C26 C21 C22 120.8(5) . . ? C26 C21 S2 120.2(4) . . ? C22 C21 S2 118.9(3) . . ? C23 C22 C21 118.9(4) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? C22 C23 C24 120.2(5) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C25 C24 C23 120.2(5) . . ? C25 C24 C28 120.3(5) . . ? C23 C24 C28 119.5(5) . . ? C26 C25 C24 119.5(4) . . ? C26 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? C25 C26 C21 120.4(5) . . ? C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? O8 C27 O7 119.4(4) . . ? O8 C27 C15 121.0(4) . . ? O7 C27 C15 119.4(4) . . ? O10 C28 O9 122.4(5) . . ? O10 C28 C24 120.1(5) . . ? O9 C28 C24 117.5(5) . . ? N1 C29 C30 123.7(5) . . ? N1 C29 H29A 118.2 . . ? C30 C29 H29A 118.2 . . ? C31 C30 C29 117.6(5) . . ? C31 C30 H30A 121.2 . . ? C29 C30 H30A 121.2 . . ? C32 C31 C30 120.2(5) . . ? C32 C31 H31A 119.9 . . ? C30 C31 H31A 119.9 . . ? C31 C32 C33 119.1(5) . . ? C31 C32 H32A 120.5 . . ? C33 C32 H32A 120.5 . . ? N1 C33 C32 121.0(4) . . ? N1 C33 C34 115.7(4) . . ? C32 C33 C34 123.3(4) . . ? N2 C34 C35 121.4(4) . . ? N2 C34 C33 114.5(4) . . ? C35 C34 C33 124.1(4) . . ? C36 C35 C34 119.1(5) . . ? C36 C35 H35A 120.5 . . ? C34 C35 H35A 120.5 . . ? C37 C36 C35 119.7(5) . . ? C37 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? C38 C37 C36 118.7(5) . . ? C38 C37 H37A 120.7 . . ? C36 C37 H37A 120.7 . . ? N2 C38 C37 123.3(5) . . ? N2 C38 H38B 118.4 . . ? C37 C38 H38B 118.4 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.603 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.087