# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Yong Cui' _publ_contact_author_email YONGCUI@SJTU.EDU.CN _publ_section_title ; Homochiral Helical Coordination Polymers of Metallosalen Complexes with Tunable Pitches ; loop_ _publ_author_name 'Yong Cui' 'Taiwei Dong' 'Gao Li' 'Xiaobing Xi' 'Wei-Min Xuan' # Attachment 'Cif of 2.cif' data_2 #TrackingRef 'Cif of 2.cif' _database_code_depnum_ccdc_archive 'CCDC 761763' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H42 Co N4 O2' _chemical_formula_weight 645.69 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 16.561(3) _cell_length_b 12.656(3) _cell_length_c 17.176(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.54(3) _cell_angle_gamma 90.00 _cell_volume 3300.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24215 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 25.00 _exptl_crystal_description block-like _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1364 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.941 _exptl_absorpt_correction_T_max 0.962 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24215 _diffrn_reflns_av_R_equivalents 0.0956 _diffrn_reflns_av_sigmaI/netI 0.1212 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10387 _reflns_number_gt 6087 _reflns_threshold_expression >2sigma(I) _chemical_absolute_configuration ad _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _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 _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^)+(0.0866P)^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 geom _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 0.01(3) _refine_ls_number_reflns 10387 _refine_ls_number_parameters 811 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1186 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1825 _refine_ls_wR_factor_gt 0.1525 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.003 _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 0.36644(9) 0.27473(9) 0.23139(8) 0.0457(4) Uani 1 1 d . . . Co2 Co 0.86822(9) 0.55765(9) 0.73067(8) 0.0437(4) Uani 1 1 d . . . O1 O 0.4621(5) 0.2069(7) 0.3160(4) 0.055(2) Uani 1 1 d . . . O2 O 0.4134(5) 0.2264(6) 0.1552(4) 0.052(2) Uani 1 1 d . . . O3 O 0.9628(4) 0.6285(6) 0.8149(4) 0.0421(18) Uani 1 1 d . . . O4 O 0.9169(4) 0.6024(6) 0.6531(4) 0.047(2) Uani 1 1 d . . . N1 N 0.5656(5) -0.0791(7) 0.7405(5) 0.045(2) Uani 1 1 d . . . N2 N 0.3073(5) 0.2980(7) 0.3043(5) 0.043(2) Uani 1 1 d . . . N3 N 0.2649(5) 0.3263(8) 0.1444(5) 0.048(2) Uani 1 1 d . . . N4 N 0.3332(7) 0.3008(9) -0.3216(5) 0.068(3) Uani 1 1 d . . . N5 N 1.0661(5) 0.9104(8) 1.2367(5) 0.049(2) Uani 1 1 d . . . N6 N 0.8065(5) 0.5455(8) 0.8000(5) 0.045(2) Uani 1 1 d . . . N7 N 0.7704(6) 0.4961(8) 0.6465(5) 0.046(2) Uani 1 1 d . . . N8 N 0.8310(7) 0.5317(9) 0.1755(6) 0.074(3) Uani 1 1 d . . . C1 C 0.5430(8) -0.0234(10) 0.7940(6) 0.062(3) Uani 1 1 d . . . H1A H 0.5592 -0.0492 0.8502 0.074 Uiso 1 1 calc R . . C2 C 0.4997(7) 0.0651(10) 0.7732(6) 0.057(3) Uani 1 1 d . . . H2A H 0.4832 0.0989 0.8141 0.068 Uiso 1 1 calc R . . C3 C 0.4770(7) 0.1112(10) 0.6967(6) 0.055(3) Uani 1 1 d . . . H3A H 0.4447 0.1755 0.6833 0.067 Uiso 1 1 calc R . . C4 C 0.5018(7) 0.0622(10) 0.6392(6) 0.048(3) Uani 1 1 d . . . C5 C 0.5439(7) -0.0356(9) 0.6644(7) 0.047(3) Uani 1 1 d . . . H5A H 0.5580 -0.0739 0.6239 0.056 Uiso 1 1 calc R . . C6 C 0.4895(7) 0.1040(9) 0.5543(6) 0.041(3) Uani 1 1 d . . . C7 C 0.5591(7) 0.0983(9) 0.5270(6) 0.048(3) Uani 1 1 d . . . H7A H 0.6128 0.0665 0.5637 0.058 Uiso 1 1 calc R . . C8 C 0.5535(7) 0.1362(9) 0.4504(6) 0.043(3) Uani 1 1 d . . . C9 C 0.4713(7) 0.1794(9) 0.3959(5) 0.047(3) Uani 1 1 d . . . C10 C 0.4039(7) 0.1981(9) 0.4252(6) 0.043(3) Uani 1 1 d . . . C11 C 0.4164(7) 0.1600(8) 0.5036(6) 0.045(3) Uani 1 1 d . . . H11A H 0.3719 0.1730 0.5242 0.054 Uiso 1 1 calc R . . C12 C 0.6339(7) 0.1327(10) 0.4256(6) 0.052(3) Uani 1 1 d . . . C13 C 0.6544(8) 0.2424(10) 0.4054(7) 0.070(4) Uani 1 1 d . . . H13A H 0.7064 0.2404 0.3917 0.105 Uiso 1 1 calc R . . H13B H 0.6662 0.2882 0.4548 0.105 Uiso 1 1 calc R . . H13C H 0.6041 0.2701 0.3568 0.105 Uiso 1 1 calc R . . C14 C 0.7150(7) 0.0838(12) 0.4963(6) 0.074(4) Uani 1 1 d . . . H14A H 0.7647 0.0844 0.4791 0.112 Uiso 1 1 calc R . . H14B H 0.7018 0.0108 0.5063 0.112 Uiso 1 1 calc R . . H14C H 0.7301 0.1249 0.5486 0.112 Uiso 1 1 calc R . . C15 C 0.6158(6) 0.0605(12) 0.3464(5) 0.056(3) Uani 1 1 d . . . H15A H 0.6680 0.0593 0.3329 0.083 Uiso 1 1 calc R . . H15B H 0.5655 0.0883 0.2978 0.083 Uiso 1 1 calc R . . H15C H 0.6026 -0.0114 0.3590 0.083 Uiso 1 1 calc R . . C16 C 0.3288(7) 0.2570(10) 0.3766(6) 0.047(3) Uani 1 1 d . . . H16A H 0.2880 0.2675 0.4021 0.057 Uiso 1 1 calc R . . C17 C 0.2356(6) 0.3755(8) 0.2693(5) 0.056(3) Uani 1 1 d . . . H17A H 0.2640 0.4466 0.2763 0.068 Uiso 1 1 calc R . . C18 C 0.1694(7) 0.3831(10) 0.3048(6) 0.055(3) Uani 1 1 d . . . H18A H 0.1982 0.4009 0.3660 0.066 Uiso 1 1 calc R . . H18B H 0.1395 0.3141 0.2994 0.066 Uiso 1 1 calc R . . C19 C 0.1021(8) 0.4676(9) 0.2587(6) 0.062(3) Uani 1 1 d . . . H19A H 0.0560 0.4691 0.2817 0.075 Uiso 1 1 calc R . . H19B H 0.1314 0.5374 0.2696 0.075 Uiso 1 1 calc R . . C20 C 0.0600(6) 0.4491(7) 0.1655(5) 0.057(3) Uani 1 1 d . . . H20A H 0.0203 0.5089 0.1380 0.068 Uiso 1 1 calc R . . H20B H 0.0239 0.3840 0.1541 0.068 Uiso 1 1 calc R . . C21 C 0.1283(7) 0.4380(10) 0.1271(6) 0.059(3) Uani 1 1 d . . . H21A H 0.0991 0.4177 0.0666 0.071 Uiso 1 1 calc R . . H21B H 0.1589 0.5061 0.1307 0.071 Uiso 1 1 calc R . . C22 C 0.1937(5) 0.3541(7) 0.1759(5) 0.048(2) Uani 1 1 d . . . H22A H 0.1585 0.2881 0.1695 0.057 Uiso 1 1 calc R . . C23 C 0.2482(7) 0.3354(9) 0.0645(6) 0.046(3) Uani 1 1 d . . . H23A H 0.1943 0.3669 0.0279 0.055 Uiso 1 1 calc R . . C24 C 0.3095(7) 0.2989(10) 0.0288(6) 0.051(3) Uani 1 1 d . . . C25 C 0.3871(6) 0.2445(8) 0.0749(7) 0.046(3) Uani 1 1 d . . . C26 C 0.4377(7) 0.2069(9) 0.0271(6) 0.043(3) Uani 1 1 d . . . C27 C 0.4067(7) 0.2332(9) -0.0585(6) 0.051(3) Uani 1 1 d . . . H27A H 0.4413 0.2106 -0.0882 0.062 Uiso 1 1 calc R . . C28 C 0.3310(6) 0.2888(9) -0.1049(6) 0.045(3) Uani 1 1 d . . . C29 C 0.2783(7) 0.3237(9) -0.0607(5) 0.058(3) Uani 1 1 d . . . H29A H 0.2187 0.2930 -0.0895 0.070 Uiso 1 1 calc R . . H29B H 0.2720 0.4014 -0.0669 0.070 Uiso 1 1 calc R . . C30 C 0.5173(7) 0.1413(11) 0.0718(6) 0.054(3) Uani 1 1 d . . . C31 C 0.4958(6) 0.0420(11) 0.1103(6) 0.057(3) Uani 1 1 d . . . H31A H 0.4696 0.0622 0.1502 0.085 Uiso 1 1 calc R . . H31B H 0.5500 0.0018 0.1404 0.085 Uiso 1 1 calc R . . H31C H 0.4540 -0.0017 0.0650 0.085 Uiso 1 1 calc R . . C32 C 0.5906(7) 0.2073(11) 0.1438(6) 0.070(4) Uani 1 1 d . . . H32A H 0.5660 0.2367 0.1824 0.105 Uiso 1 1 calc R . . H32B H 0.6109 0.2649 0.1180 0.105 Uiso 1 1 calc R . . H32C H 0.6404 0.1611 0.1757 0.105 Uiso 1 1 calc R . . C33 C 0.5591(7) 0.1014(11) 0.0127(6) 0.064(4) Uani 1 1 d . . . H33A H 0.6114 0.0593 0.0453 0.096 Uiso 1 1 calc R . . H33B H 0.5761 0.1617 -0.0132 0.096 Uiso 1 1 calc R . . H33C H 0.5166 0.0575 -0.0319 0.096 Uiso 1 1 calc R . . C34 C 0.3003(7) 0.3079(9) -0.1978(6) 0.045(3) Uani 1 1 d . . . C35 C 0.3562(7) 0.2958(9) -0.2394(7) 0.055(3) Uani 1 1 d . . . H35A H 0.4166 0.2827 -0.2053 0.066 Uiso 1 1 calc R . . C36 C 0.2503(8) 0.3273(10) -0.3689(6) 0.054(3) Uani 1 1 d . . . H36A H 0.2320 0.3336 -0.4287 0.065 Uiso 1 1 calc R . . C37 C 0.1897(8) 0.3460(11) -0.3326(7) 0.078(4) Uani 1 1 d . . . H37A H 0.1305 0.3632 -0.3679 0.094 Uiso 1 1 calc R . . C38 C 0.2154(8) 0.3397(12) -0.2460(6) 0.087(5) Uani 1 1 d . . . H38A H 0.1757 0.3566 -0.2203 0.104 Uiso 1 1 calc R . . C39 C 1.0388(7) 0.8629(8) 1.2922(6) 0.051(3) Uani 1 1 d . . . H39A H 1.0509 0.8955 1.3455 0.061 Uiso 1 1 calc R . . C40 C 0.9919(7) 0.7644(11) 1.2728(7) 0.066(3) Uani 1 1 d . . . H40A H 1.0243 0.7130 1.3179 0.079 Uiso 1 1 calc R . . H40B H 0.9335 0.7755 1.2745 0.079 Uiso 1 1 calc R . . C41 C 0.9790(7) 0.7189(9) 1.1932(5) 0.053(3) Uani 1 1 d . . . H41A H 0.9502 0.6525 1.1775 0.064 Uiso 1 1 calc R . . C42 C 1.0084(6) 0.7710(10) 1.1377(6) 0.041(2) Uani 1 1 d . . . C43 C 1.0516(7) 0.8639(9) 1.1623(6) 0.047(3) Uani 1 1 d . . . H43A H 1.0729 0.8978 1.1249 0.057 Uiso 1 1 calc R . . C44 C 0.9973(7) 0.7203(9) 1.0568(6) 0.047(3) Uani 1 1 d . . . C45 C 1.0643(7) 0.7313(9) 1.0249(6) 0.047(3) Uani 1 1 d . . . H45A H 1.1165 0.7674 1.0598 0.057 Uiso 1 1 calc R . . C46 C 1.0597(7) 0.6939(10) 0.9473(7) 0.051(3) Uani 1 1 d . . . C47 C 0.9771(6) 0.6471(8) 0.8901(6) 0.037(2) Uani 1 1 d . . . C48 C 0.9119(7) 0.6321(9) 0.9253(6) 0.041(3) Uani 1 1 d . . . C49 C 0.9230(7) 0.6685(9) 1.0083(6) 0.047(3) Uani 1 1 d . . . H49A H 0.8783 0.6563 1.0287 0.056 Uiso 1 1 calc R . . C50 C 1.1376(7) 0.6966(11) 0.9226(7) 0.054(3) Uani 1 1 d . . . C51 C 1.1576(7) 0.5796(10) 0.9053(6) 0.066(3) Uani 1 1 d . . . H51A H 1.1056 0.5494 0.8598 0.099 Uiso 1 1 calc R . . H51B H 1.1722 0.5376 0.9571 0.099 Uiso 1 1 calc R . . H51C H 1.2074 0.5787 0.8882 0.099 Uiso 1 1 calc R . . C52 C 1.1196(7) 0.7615(11) 0.8445(6) 0.061(3) Uani 1 1 d . . . H52A H 1.1046 0.8339 0.8542 0.092 Uiso 1 1 calc R . . H52B H 1.0702 0.7306 0.7966 0.092 Uiso 1 1 calc R . . H52C H 1.1721 0.7626 0.8315 0.092 Uiso 1 1 calc R . . C53 C 1.2215(7) 0.7370(12) 0.9953(7) 0.072(4) Uani 1 1 d . . . H53A H 1.2121 0.8097 1.0096 0.108 Uiso 1 1 calc R . . H53B H 1.2708 0.7353 0.9775 0.108 Uiso 1 1 calc R . . H53C H 1.2351 0.6918 1.0453 0.108 Uiso 1 1 calc R . . C54 C 0.8277(7) 0.5800(9) 0.8779(6) 0.048(3) Uani 1 1 d . . . H54A H 0.7872 0.5709 0.9040 0.057 Uiso 1 1 calc R . . C55 C 0.7157(6) 0.5002(8) 0.7536(5) 0.051(3) Uani 1 1 d . . . H55A H 0.6750 0.5607 0.7276 0.061 Uiso 1 1 calc R . . C56 C 0.6775(7) 0.4376(10) 0.8093(6) 0.051(3) Uani 1 1 d . . . H56A H 0.7174 0.3785 0.8381 0.061 Uiso 1 1 calc R . . H56B H 0.6728 0.4847 0.8533 0.061 Uiso 1 1 calc R . . C57 C 0.5875(8) 0.3950(10) 0.7536(7) 0.071(4) Uani 1 1 d . . . H57A H 0.5455 0.4547 0.7348 0.086 Uiso 1 1 calc R . . H57B H 0.5676 0.3470 0.7878 0.086 Uiso 1 1 calc R . . C58 C 0.5850(6) 0.3355(8) 0.6754(5) 0.061(3) Uani 1 1 d . . . H58A H 0.5230 0.3189 0.6386 0.073 Uiso 1 1 calc R . . H58B H 0.6168 0.2678 0.6938 0.073 Uiso 1 1 calc R . . C59 C 0.6264(7) 0.3981(10) 0.6228(6) 0.052(3) Uani 1 1 d . . . H59A H 0.6294 0.3528 0.5770 0.062 Uiso 1 1 calc R . . H59B H 0.5897 0.4605 0.5963 0.062 Uiso 1 1 calc R . . C60 C 0.7182(6) 0.4330(8) 0.6813(5) 0.052(2) Uani 1 1 d . . . H60A H 0.7529 0.3679 0.7070 0.062 Uiso 1 1 calc R . . C61 C 0.7557(7) 0.4877(9) 0.5673(6) 0.050(3) Uani 1 1 d . . . H61A H 0.7046 0.4493 0.5330 0.060 Uiso 1 1 calc R . . C62 C 0.8077(6) 0.5298(9) 0.5250(5) 0.039(3) Uani 1 1 d . . . C63 C 0.8864(7) 0.5879(9) 0.5705(5) 0.047(3) Uani 1 1 d . . . C64 C 0.9342(7) 0.6296(10) 0.5250(6) 0.050(3) Uani 1 1 d . . . C65 C 0.9049(7) 0.6088(9) 0.4396(6) 0.050(3) Uani 1 1 d . . . H65A H 0.9373 0.6360 0.4093 0.060 Uiso 1 1 calc R . . C66 C 0.8281(7) 0.5484(11) 0.3949(5) 0.049(3) Uani 1 1 d . . . C67 C 0.7825(6) 0.5137(8) 0.4394(5) 0.046(3) Uani 1 1 d . . . H67A H 0.7295 0.4757 0.4098 0.055 Uiso 1 1 calc R . . C68 C 1.0181(7) 0.6979(10) 0.5692(6) 0.049(3) Uani 1 1 d . . . C69 C 1.0885(7) 0.6328(11) 0.6374(6) 0.064(3) Uani 1 1 d . . . H69A H 1.0667 0.6108 0.6802 0.096 Uiso 1 1 calc R . . H69B H 1.1418 0.6755 0.6644 0.096 Uiso 1 1 calc R . . H69C H 1.1022 0.5701 0.6114 0.096 Uiso 1 1 calc R . . C70 C 0.9942(7) 0.7959(11) 0.6074(6) 0.062(4) Uani 1 1 d . . . H70A H 0.9500 0.8374 0.5621 0.094 Uiso 1 1 calc R . . H70B H 1.0470 0.8390 0.6359 0.094 Uiso 1 1 calc R . . H70C H 0.9702 0.7743 0.6486 0.094 Uiso 1 1 calc R . . C71 C 1.0562(7) 0.7367(11) 0.5047(7) 0.069(4) Uani 1 1 d . . . H71A H 1.0129 0.7818 0.4619 0.104 Uiso 1 1 calc R . . H71B H 1.0695 0.6756 0.4767 0.104 Uiso 1 1 calc R . . H71C H 1.1103 0.7770 0.5348 0.104 Uiso 1 1 calc R . . C72 C 0.7979(8) 0.5291(10) 0.3024(7) 0.053(3) Uani 1 1 d . . . C73 C 0.8563(8) 0.5443(11) 0.2618(6) 0.070(4) Uani 1 1 d . . . H73A H 0.9154 0.5640 0.2953 0.084 Uiso 1 1 calc R . . C74 C 0.7477(9) 0.5113(11) 0.1297(7) 0.067(4) Uani 1 1 d . . . H74A H 0.7278 0.5106 0.0697 0.080 Uiso 1 1 calc R . . C75 C 0.6904(8) 0.4919(11) 0.1633(6) 0.070(4) Uani 1 1 d . . . H75A H 0.6323 0.4694 0.1286 0.084 Uiso 1 1 calc R . . C76 C 0.7160(8) 0.5047(10) 0.2503(7) 0.063(3) Uani 1 1 d . . . H76A H 0.6731 0.4956 0.2735 0.076 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 0.0505(10) 0.0495(10) 0.0410(8) -0.0009(7) 0.0225(7) 0.0004(8) Co2 0.0459(9) 0.0455(10) 0.0403(8) 0.0006(7) 0.0178(7) -0.0017(8) O1 0.053(5) 0.062(6) 0.050(4) -0.004(4) 0.021(4) -0.001(4) O2 0.062(5) 0.054(6) 0.045(4) -0.008(4) 0.026(4) 0.004(4) O3 0.044(4) 0.054(5) 0.032(4) -0.011(4) 0.019(3) -0.013(4) O4 0.039(4) 0.063(6) 0.038(4) 0.001(3) 0.015(3) -0.004(3) N1 0.053(6) 0.044(6) 0.043(5) 0.001(5) 0.023(4) 0.004(5) N2 0.054(5) 0.037(5) 0.044(4) 0.006(4) 0.027(4) 0.004(4) N3 0.037(5) 0.069(7) 0.036(4) -0.001(4) 0.014(4) 0.009(4) N4 0.098(8) 0.080(9) 0.040(5) 0.014(5) 0.043(6) 0.033(7) N5 0.061(6) 0.050(6) 0.041(5) -0.002(5) 0.026(4) -0.003(5) N6 0.035(5) 0.055(6) 0.044(4) 0.005(4) 0.014(4) -0.004(4) N7 0.049(6) 0.044(5) 0.045(5) 0.008(4) 0.018(4) -0.001(4) N8 0.091(9) 0.071(9) 0.063(6) -0.018(6) 0.033(6) -0.012(7) C1 0.081(9) 0.083(10) 0.033(6) -0.005(6) 0.035(6) 0.004(7) C2 0.090(8) 0.067(9) 0.034(5) 0.003(6) 0.046(5) 0.026(7) C3 0.053(7) 0.057(8) 0.061(7) -0.001(6) 0.028(6) 0.005(6) C4 0.055(7) 0.046(7) 0.038(5) 0.000(6) 0.013(5) 0.003(6) C5 0.054(6) 0.050(7) 0.044(6) -0.013(5) 0.029(5) -0.003(5) C6 0.043(6) 0.040(6) 0.046(6) -0.003(5) 0.024(5) 0.000(5) C7 0.046(6) 0.053(8) 0.040(6) 0.000(5) 0.011(5) 0.015(5) C8 0.039(6) 0.053(8) 0.037(5) -0.004(5) 0.015(5) -0.003(5) C9 0.078(8) 0.046(7) 0.021(5) -0.003(4) 0.023(5) -0.017(5) C10 0.045(6) 0.046(7) 0.043(6) -0.004(5) 0.024(5) 0.002(5) C11 0.044(6) 0.042(7) 0.053(6) -0.006(5) 0.023(5) 0.006(5) C12 0.044(7) 0.064(9) 0.048(6) 0.005(6) 0.019(5) -0.001(6) C13 0.080(9) 0.076(10) 0.065(7) -0.019(6) 0.041(7) -0.026(7) C14 0.047(7) 0.127(13) 0.051(6) 0.004(7) 0.021(5) 0.010(7) C15 0.050(7) 0.079(8) 0.046(6) -0.001(6) 0.027(5) 0.004(6) C16 0.041(6) 0.045(8) 0.060(7) -0.013(6) 0.025(5) -0.008(6) C17 0.052(6) 0.067(7) 0.054(5) 0.006(4) 0.024(4) 0.000(5) C18 0.059(7) 0.054(8) 0.053(6) -0.006(5) 0.023(5) 0.003(5) C19 0.079(8) 0.076(8) 0.045(5) 0.015(5) 0.039(5) 0.026(6) C20 0.054(6) 0.067(7) 0.059(5) 0.002(5) 0.032(4) 0.019(5) C21 0.063(8) 0.072(9) 0.040(6) 0.003(6) 0.018(6) 0.004(7) C22 0.042(5) 0.047(6) 0.060(5) 0.005(4) 0.026(4) 0.005(4) C23 0.049(6) 0.036(6) 0.052(6) -0.008(5) 0.020(5) -0.010(5) C24 0.056(7) 0.055(9) 0.045(6) -0.008(6) 0.024(5) -0.009(6) C25 0.038(6) 0.025(7) 0.069(7) -0.010(5) 0.015(5) -0.003(5) C26 0.048(7) 0.044(7) 0.043(6) -0.008(5) 0.023(5) -0.010(6) C27 0.059(8) 0.065(8) 0.035(5) -0.006(5) 0.023(5) -0.014(6) C28 0.037(6) 0.040(7) 0.059(6) -0.007(5) 0.022(5) -0.002(5) C29 0.078(8) 0.059(8) 0.044(6) -0.014(5) 0.032(6) -0.034(6) C30 0.050(7) 0.079(9) 0.041(6) -0.011(6) 0.026(5) -0.009(7) C31 0.052(7) 0.060(8) 0.055(6) -0.006(6) 0.017(5) 0.002(6) C32 0.051(7) 0.091(10) 0.068(7) -0.012(7) 0.024(6) -0.015(7) C33 0.058(7) 0.095(11) 0.042(5) -0.013(6) 0.022(5) -0.005(7) C34 0.052(7) 0.056(8) 0.033(5) 0.000(5) 0.023(5) -0.008(6) C35 0.057(7) 0.043(7) 0.069(7) 0.013(6) 0.028(6) 0.027(6) C36 0.073(8) 0.051(8) 0.042(6) 0.004(5) 0.026(6) -0.001(6) C37 0.053(7) 0.102(11) 0.072(8) 0.001(7) 0.017(6) 0.030(7) C38 0.070(8) 0.154(14) 0.034(6) 0.006(7) 0.019(6) 0.032(9) C39 0.063(7) 0.036(7) 0.062(7) -0.013(5) 0.034(6) -0.013(6) C40 0.057(7) 0.056(8) 0.079(7) -0.003(7) 0.020(6) 0.001(6) C41 0.078(8) 0.052(8) 0.033(5) -0.010(5) 0.025(6) -0.016(6) C42 0.042(6) 0.048(7) 0.041(5) 0.000(6) 0.023(5) -0.004(6) C43 0.053(7) 0.057(8) 0.034(5) -0.007(5) 0.021(5) -0.010(6) C44 0.050(7) 0.053(7) 0.035(5) 0.004(5) 0.014(5) 0.000(5) C45 0.053(7) 0.049(8) 0.047(6) 0.001(5) 0.028(5) 0.009(5) C46 0.050(7) 0.056(8) 0.053(6) 0.003(6) 0.025(5) 0.002(6) C47 0.027(5) 0.034(6) 0.054(6) -0.001(4) 0.021(4) -0.013(4) C48 0.042(6) 0.043(7) 0.038(5) 0.004(5) 0.015(5) 0.004(5) C49 0.058(7) 0.046(7) 0.040(5) 0.005(5) 0.024(5) -0.002(6) C50 0.047(7) 0.077(9) 0.047(6) 0.000(6) 0.027(6) 0.001(7) C51 0.044(7) 0.084(10) 0.073(7) -0.010(7) 0.027(6) 0.004(6) C52 0.054(7) 0.066(8) 0.066(7) 0.005(7) 0.027(6) -0.008(6) C53 0.044(7) 0.108(12) 0.066(7) -0.019(7) 0.024(6) -0.010(7) C54 0.065(7) 0.048(8) 0.032(5) 0.001(5) 0.022(5) 0.000(6) C55 0.056(6) 0.064(7) 0.035(4) -0.002(4) 0.020(4) -0.013(5) C56 0.059(7) 0.056(7) 0.046(6) -0.010(5) 0.029(5) -0.010(5) C57 0.053(6) 0.084(9) 0.079(7) -0.020(6) 0.029(5) -0.019(6) C58 0.065(6) 0.060(7) 0.059(5) -0.011(5) 0.026(5) -0.015(5) C59 0.050(7) 0.053(8) 0.053(6) -0.004(6) 0.023(6) -0.015(6) C60 0.061(6) 0.058(7) 0.042(4) -0.009(4) 0.027(4) -0.010(5) C61 0.041(6) 0.055(8) 0.046(6) 0.001(5) 0.010(5) -0.007(5) C62 0.041(6) 0.041(7) 0.036(5) 0.002(5) 0.014(5) -0.002(5) C63 0.064(7) 0.067(9) 0.017(4) 0.000(4) 0.022(5) 0.005(6) C64 0.043(7) 0.065(8) 0.046(6) 0.007(6) 0.023(5) 0.006(6) C65 0.041(7) 0.053(7) 0.061(7) 0.005(6) 0.025(5) 0.004(5) C66 0.058(7) 0.064(8) 0.030(5) -0.004(5) 0.023(5) 0.008(7) C67 0.038(6) 0.043(7) 0.046(6) -0.004(5) 0.006(5) -0.020(5) C68 0.046(7) 0.058(8) 0.043(6) -0.008(5) 0.017(5) -0.016(6) C69 0.055(7) 0.086(10) 0.047(6) 0.001(6) 0.016(5) 0.001(7) C70 0.072(8) 0.076(10) 0.049(6) -0.008(6) 0.035(6) -0.023(7) C71 0.054(7) 0.093(11) 0.068(7) -0.016(6) 0.032(6) -0.036(7) C72 0.051(8) 0.050(8) 0.055(7) 0.000(6) 0.019(6) -0.004(6) C73 0.099(10) 0.079(9) 0.046(6) -0.015(7) 0.043(7) -0.012(8) C74 0.095(11) 0.067(9) 0.041(6) -0.003(6) 0.031(7) 0.011(8) C75 0.083(8) 0.102(10) 0.025(5) 0.004(6) 0.020(5) 0.030(7) C76 0.058(7) 0.073(8) 0.064(7) 0.012(6) 0.029(6) 0.017(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 1.866(8) . ? Co1 O2 1.871(6) . ? Co1 O1 1.877(8) . ? Co1 N2 1.896(7) . ? Co1 N1 2.118(9) 2_656 ? Co2 N7 1.857(9) . ? Co2 N6 1.859(7) . ? Co2 O3 1.882(7) . ? Co2 O4 1.899(6) . ? Co2 N5 2.118(9) 2_747 ? O1 C9 1.363(9) . ? O2 C25 1.291(10) . ? O3 C47 1.239(9) . ? O4 C63 1.314(8) . ? N1 C1 1.325(12) . ? N1 C5 1.329(12) . ? N1 Co1 2.118(9) 2_646 ? N2 C16 1.258(11) . ? N2 C17 1.472(12) . ? N3 C23 1.292(10) . ? N3 C22 1.521(10) . ? N4 C35 1.308(10) . ? N4 C36 1.328(13) . ? N5 C43 1.338(11) . ? N5 C39 1.348(12) . ? N5 Co2 2.118(9) 2_757 ? N6 C54 1.316(10) . ? N6 C55 1.506(11) . ? N7 C61 1.287(10) . ? N7 C60 1.468(11) . ? N8 C74 1.312(14) . ? N8 C73 1.379(11) . ? C1 C2 1.301(15) . ? C2 C3 1.347(12) . ? C3 C4 1.362(12) . ? C4 C5 1.402(15) . ? C4 C6 1.486(12) . ? C6 C11 1.373(14) . ? C6 C7 1.409(12) . ? C7 C8 1.368(11) . ? C8 C9 1.418(13) . ? C8 C12 1.552(12) . ? C9 C10 1.415(13) . ? C10 C11 1.365(12) . ? C10 C16 1.404(14) . ? C12 C13 1.502(16) . ? C12 C14 1.536(14) . ? C12 C15 1.565(14) . ? C17 C18 1.455(12) . ? C17 C22 1.496(11) . ? C18 C19 1.520(14) . ? C19 C20 1.487(12) . ? C20 C21 1.527(12) . ? C21 C22 1.509(13) . ? C23 C24 1.454(13) . ? C24 C25 1.392(14) . ? C24 C29 1.447(11) . ? C25 C26 1.468(12) . ? C26 C27 1.391(12) . ? C26 C30 1.485(15) . ? C27 C28 1.379(14) . ? C28 C29 1.436(12) . ? C28 C34 1.489(11) . ? C30 C33 1.525(12) . ? C30 C31 1.527(16) . ? C30 C32 1.582(14) . ? C34 C38 1.376(14) . ? C34 C35 1.386(11) . ? C36 C37 1.398(13) . ? C37 C38 1.377(12) . ? C39 C40 1.436(15) . ? C40 C41 1.418(12) . ? C41 C42 1.397(12) . ? C42 C43 1.353(15) . ? C42 C44 1.474(13) . ? C44 C49 1.349(14) . ? C44 C45 1.427(13) . ? C45 C46 1.387(12) . ? C46 C47 1.454(13) . ? C46 C50 1.511(13) . ? C47 C48 1.447(12) . ? C48 C49 1.437(12) . ? C48 C54 1.461(14) . ? C50 C52 1.498(14) . ? C50 C53 1.538(14) . ? C50 C51 1.571(17) . ? C55 C60 1.519(11) . ? C55 C56 1.556(11) . ? C56 C57 1.513(14) . ? C57 C58 1.525(12) . ? C58 C59 1.552(12) . ? C59 C60 1.515(12) . ? C61 C62 1.432(12) . ? C62 C67 1.375(10) . ? C62 C63 1.427(13) . ? C63 C64 1.418(12) . ? C64 C65 1.374(12) . ? C64 C68 1.553(14) . ? C65 C66 1.419(15) . ? C66 C67 1.344(12) . ? C66 C72 1.483(12) . ? C68 C69 1.523(15) . ? C68 C70 1.528(16) . ? C68 C71 1.557(12) . ? C72 C76 1.329(14) . ? C72 C73 1.414(13) . ? C74 C75 1.316(14) . ? C75 C76 1.390(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Co1 O2 92.7(3) . . ? N3 Co1 O1 173.1(4) . . ? O2 Co1 O1 86.2(3) . . ? N3 Co1 N2 86.3(3) . . ? O2 Co1 N2 168.8(4) . . ? O1 Co1 N2 93.3(3) . . ? N3 Co1 N1 95.9(4) . 2_656 ? O2 Co1 N1 96.5(3) . 2_656 ? O1 Co1 N1 90.9(3) . 2_656 ? N2 Co1 N1 94.7(4) . 2_656 ? N7 Co2 N6 86.1(4) . . ? N7 Co2 O3 176.1(4) . . ? N6 Co2 O3 92.8(3) . . ? N7 Co2 O4 93.6(3) . . ? N6 Co2 O4 165.9(4) . . ? O3 Co2 O4 86.6(3) . . ? N7 Co2 N5 91.9(4) . 2_747 ? N6 Co2 N5 96.5(4) . 2_747 ? O3 Co2 N5 91.9(3) . 2_747 ? O4 Co2 N5 97.5(3) . 2_747 ? C9 O1 Co1 128.1(7) . . ? C25 O2 Co1 129.2(7) . . ? C47 O3 Co2 130.2(6) . . ? C63 O4 Co2 128.8(6) . . ? C1 N1 C5 114.9(10) . . ? C1 N1 Co1 125.4(7) . 2_646 ? C5 N1 Co1 119.7(7) . 2_646 ? C16 N2 C17 122.9(8) . . ? C16 N2 Co1 124.7(8) . . ? C17 N2 Co1 112.3(6) . . ? C23 N3 C22 119.4(8) . . ? C23 N3 Co1 128.5(7) . . ? C22 N3 Co1 112.0(5) . . ? C35 N4 C36 117.2(8) . . ? C43 N5 C39 119.8(10) . . ? C43 N5 Co2 121.1(7) . 2_757 ? C39 N5 Co2 119.1(6) . 2_757 ? C54 N6 C55 117.9(8) . . ? C54 N6 Co2 129.2(7) . . ? C55 N6 Co2 112.4(5) . . ? C61 N7 C60 119.5(9) . . ? C61 N7 Co2 126.5(7) . . ? C60 N7 Co2 112.6(5) . . ? C74 N8 C73 117.5(10) . . ? C2 C1 N1 123.1(10) . . ? C1 C2 C3 123.3(10) . . ? C2 C3 C4 117.6(11) . . ? C3 C4 C5 115.7(10) . . ? C3 C4 C6 125.9(11) . . ? C5 C4 C6 118.3(9) . . ? N1 C5 C4 125.2(10) . . ? C11 C6 C7 116.5(9) . . ? C11 C6 C4 123.2(9) . . ? C7 C6 C4 119.9(9) . . ? C8 C7 C6 123.5(10) . . ? C7 C8 C9 116.6(8) . . ? C7 C8 C12 121.2(9) . . ? C9 C8 C12 122.1(9) . . ? O1 C9 C10 121.9(10) . . ? O1 C9 C8 117.1(9) . . ? C10 C9 C8 121.0(8) . . ? C11 C10 C16 121.5(9) . . ? C11 C10 C9 117.5(10) . . ? C16 C10 C9 120.9(9) . . ? C10 C11 C6 123.7(9) . . ? C13 C12 C14 110.3(10) . . ? C13 C12 C8 109.6(10) . . ? C14 C12 C8 111.7(8) . . ? C13 C12 C15 108.8(8) . . ? C14 C12 C15 104.8(10) . . ? C8 C12 C15 111.6(9) . . ? N2 C16 C10 129.8(9) . . ? C18 C17 N2 119.5(8) . . ? C18 C17 C22 111.0(8) . . ? N2 C17 C22 105.7(7) . . ? C17 C18 C19 110.2(8) . . ? C20 C19 C18 112.4(8) . . ? C19 C20 C21 111.7(8) . . ? C22 C21 C20 108.5(8) . . ? C17 C22 C21 112.9(8) . . ? C17 C22 N3 109.3(7) . . ? C21 C22 N3 116.8(7) . . ? N3 C23 C24 122.1(10) . . ? C25 C24 C29 124.6(9) . . ? C25 C24 C23 123.9(9) . . ? C29 C24 C23 111.4(10) . . ? O2 C25 C24 122.4(9) . . ? O2 C25 C26 121.0(9) . . ? C24 C25 C26 116.5(9) . . ? C27 C26 C25 117.5(10) . . ? C27 C26 C30 123.9(9) . . ? C25 C26 C30 118.6(8) . . ? C28 C27 C26 126.8(10) . . ? C27 C28 C29 117.2(9) . . ? C27 C28 C34 123.0(8) . . ? C29 C28 C34 119.8(9) . . ? C28 C29 C24 117.4(10) . . ? C26 C30 C33 112.7(9) . . ? C26 C30 C31 111.8(8) . . ? C33 C30 C31 105.2(10) . . ? C26 C30 C32 110.8(10) . . ? C33 C30 C32 106.6(8) . . ? C31 C30 C32 109.5(9) . . ? C38 C34 C35 117.1(9) . . ? C38 C34 C28 121.4(8) . . ? C35 C34 C28 121.5(9) . . ? N4 C35 C34 125.7(10) . . ? N4 C36 C37 121.3(9) . . ? C38 C37 C36 120.4(11) . . ? C34 C38 C37 117.8(10) . . ? N5 C39 C40 121.7(9) . . ? C41 C40 C39 115.9(10) . . ? C42 C41 C40 120.4(11) . . ? C43 C42 C41 118.8(10) . . ? C43 C42 C44 121.6(9) . . ? C41 C42 C44 119.4(11) . . ? N5 C43 C42 123.4(10) . . ? C49 C44 C45 117.9(9) . . ? C49 C44 C42 122.2(9) . . ? C45 C44 C42 119.8(10) . . ? C46 C45 C44 125.6(11) . . ? C45 C46 C47 117.7(9) . . ? C45 C46 C50 122.4(10) . . ? C47 C46 C50 119.9(9) . . ? O3 C47 C48 123.2(8) . . ? O3 C47 C46 121.2(7) . . ? C48 C47 C46 115.4(9) . . ? C49 C48 C47 123.4(9) . . ? C49 C48 C54 114.4(8) . . ? C47 C48 C54 122.1(8) . . ? C44 C49 C48 119.5(9) . . ? C52 C50 C46 112.1(9) . . ? C52 C50 C53 109.7(10) . . ? C46 C50 C53 112.0(9) . . ? C52 C50 C51 109.2(9) . . ? C46 C50 C51 107.4(10) . . ? C53 C50 C51 106.1(10) . . ? N6 C54 C48 121.7(9) . . ? N6 C55 C60 107.3(7) . . ? N6 C55 C56 115.7(7) . . ? C60 C55 C56 111.6(8) . . ? C57 C56 C55 109.4(8) . . ? C56 C57 C58 114.0(9) . . ? C57 C58 C59 113.4(9) . . ? C60 C59 C58 108.8(8) . . ? N7 C60 C59 119.1(7) . . ? N7 C60 C55 104.0(7) . . ? C59 C60 C55 111.0(8) . . ? N7 C61 C62 127.4(10) . . ? C67 C62 C63 118.9(8) . . ? C67 C62 C61 120.0(9) . . ? C63 C62 C61 121.1(8) . . ? O4 C63 C64 118.9(9) . . ? O4 C63 C62 122.5(8) . . ? C64 C63 C62 118.6(8) . . ? C65 C64 C63 118.7(10) . . ? C65 C64 C68 119.6(8) . . ? C63 C64 C68 121.8(9) . . ? C64 C65 C66 122.6(9) . . ? C67 C66 C65 117.0(8) . . ? C67 C66 C72 122.0(10) . . ? C65 C66 C72 120.9(9) . . ? C66 C67 C62 124.1(9) . . ? C69 C68 C70 111.0(8) . . ? C69 C68 C64 109.5(10) . . ? C70 C68 C64 109.1(8) . . ? C69 C68 C71 108.4(9) . . ? C70 C68 C71 107.4(10) . . ? C64 C68 C71 111.5(8) . . ? C76 C72 C73 114.5(10) . . ? C76 C72 C66 125.2(10) . . ? C73 C72 C66 120.2(10) . . ? N8 C73 C72 122.8(11) . . ? N8 C74 C75 123.0(11) . . ? C74 C75 C76 119.0(12) . . ? C72 C76 C75 122.9(11) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.763 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.066 # Attachment 'CIF of 4.cif' data_4 #TrackingRef 'CIF of 4.cif' _database_code_depnum_ccdc_archive 'CCDC 761764' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H43 Mn N4 O4' _chemical_formula_weight 686.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.312(7) _cell_length_b 12.191(5) _cell_length_c 18.927(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.983(7) _cell_angle_gamma 90.00 _cell_volume 3507(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 15045 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 23.00 _exptl_crystal_description block-like _exptl_crystal_colour brown _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.422 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.955 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15045 _diffrn_reflns_av_R_equivalents 0.1017 _diffrn_reflns_av_sigmaI/netI 0.1645 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 23.00 _reflns_number_total 8873 _reflns_number_gt 5566 _reflns_threshold_expression >2sigma(I) _chemical_absolute_configuration ad _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _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 _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^)+(0.1008P)^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 geom _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 0.06(4) _refine_ls_number_reflns 8873 _refine_ls_number_parameters 865 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1303 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.2325 _refine_ls_wR_factor_gt 0.1964 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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 0.19667(11) 0.11845(12) 0.82139(8) 0.0363(5) Uani 1 1 d . . . Mn2 Mn 0.79795(10) 0.83814(12) 0.68060(8) 0.0370(5) Uani 1 1 d . . . N1 N 0.0693(6) 0.1573(7) 0.8057(4) 0.029(2) Uani 1 1 d . . . N2 N 0.2026(6) 0.2241(8) 0.7439(5) 0.038(2) Uani 1 1 d . . . N3 N -0.1993(6) -0.2364(8) 1.0784(5) 0.041(2) Uani 1 1 d . . . N4 N 0.7369(9) 0.4016(14) 0.7190(9) 0.111(6) Uani 1 1 d . . . N5 N 0.7949(6) 0.7096(8) 0.7444(5) 0.038(2) Uani 1 1 d . . . N6 N 0.9277(6) 0.8209(8) 0.7061(5) 0.037(2) Uani 1 1 d . . . N7 N 0.3521(12) 0.5067(17) 0.8743(9) 0.159(9) Uani 1 1 d . . . N8 N 1.1926(6) 1.2059(9) 0.4201(5) 0.046(3) Uani 1 1 d . . . O1 O 0.1814(5) 0.0246(7) 0.8959(4) 0.046(2) Uani 1 1 d . . . O2 O 0.3209(5) 0.1133(8) 0.8377(4) 0.0385(19) Uani 1 1 d . . . O3 O 0.1781(5) -0.0072(7) 0.7443(4) 0.050(2) Uani 1 1 d . . . O4 O 0.2132(6) -0.1571(9) 0.6908(4) 0.078(3) Uani 1 1 d . . . O5 O 0.6736(5) 0.8390(8) 0.6602(4) 0.044(2) Uani 1 1 d . . . O6 O 0.8134(5) 0.9447(7) 0.6111(4) 0.041(2) Uani 1 1 d . . . O7 O 0.7968(6) 0.9455(7) 0.7669(4) 0.058(2) Uani 1 1 d . . . O8 O 0.7838(6) 1.1143(9) 0.8096(5) 0.075(3) Uani 1 1 d . . . C1 C 0.1093(8) -0.0169(10) 0.9169(5) 0.042(3) Uani 1 1 d . . . C2 C 0.1139(8) -0.1015(11) 0.9703(6) 0.040(3) Uani 1 1 d . . . C3 C 0.0367(8) -0.1408(12) 0.9898(6) 0.053(4) Uani 1 1 d . . . H3A H 0.0404 -0.1959 1.0240 0.063 Uiso 1 1 calc R . . C4 C -0.0469(7) -0.1052(10) 0.9626(6) 0.035(3) Uani 1 1 d . . . C5 C -0.0517(8) -0.0225(10) 0.9124(5) 0.043(3) Uani 1 1 d . . . H5A H -0.1066 0.0037 0.8934 0.051 Uiso 1 1 calc R . . C6 C 0.0238(8) 0.0231(10) 0.8893(6) 0.039(3) Uani 1 1 d . . . C7 C 0.2060(8) -0.1443(11) 1.0015(7) 0.050(3) Uani 1 1 d . . . C8 C 0.2614(9) -0.0548(14) 1.0396(8) 0.073(5) Uani 1 1 d . . . H8A H 0.2310 -0.0242 1.0764 0.110 Uiso 1 1 calc R . . H8B H 0.2718 0.0016 1.0063 0.110 Uiso 1 1 calc R . . H8C H 0.3166 -0.0850 1.0602 0.110 Uiso 1 1 calc R . . C9 C 0.2557(8) -0.1935(12) 0.9433(7) 0.066(4) Uani 1 1 d . . . H9A H 0.3120 -0.2201 0.9643 0.099 Uiso 1 1 calc R . . H9B H 0.2641 -0.1381 0.9087 0.099 Uiso 1 1 calc R . . H9C H 0.2223 -0.2530 0.9205 0.099 Uiso 1 1 calc R . . C10 C 0.1938(9) -0.2381(16) 1.0545(8) 0.101(7) Uani 1 1 d . . . H10A H 0.1634 -0.2108 1.0923 0.151 Uiso 1 1 calc R . . H10B H 0.2504 -0.2657 1.0739 0.151 Uiso 1 1 calc R . . H10C H 0.1601 -0.2962 1.0301 0.151 Uiso 1 1 calc R . . C11 C -0.1273(8) -0.1512(11) 0.9859(6) 0.043(3) Uani 1 1 d . . . C12 C -0.2070(7) -0.1576(11) 0.9395(6) 0.044(3) Uani 1 1 d . . . H12A H -0.2101 -0.1302 0.8934 0.053 Uiso 1 1 calc R . . C13 C -0.2794(10) -0.2041(12) 0.9630(7) 0.060(4) Uani 1 1 d . . . H13A H -0.3310 -0.2130 0.9320 0.072 Uiso 1 1 calc R . . C14 C -0.2755(8) -0.2384(11) 1.0340(7) 0.053(4) Uani 1 1 d . . . H14A H -0.3265 -0.2632 1.0510 0.064 Uiso 1 1 calc R . . C15 C -0.1302(7) -0.1952(8) 1.0540(6) 0.034(3) Uani 1 1 d . . . H15A H -0.0780 -0.1949 1.0847 0.041 Uiso 1 1 calc R . . C16 C 0.0109(7) 0.1069(10) 0.8373(5) 0.033(3) Uani 1 1 d . . . H16A H -0.0471 0.1284 0.8242 0.040 Uiso 1 1 calc R . . C17 C 0.0496(7) 0.2483(9) 0.7558(5) 0.040(3) Uani 1 1 d . . . H17A H 0.0602 0.3167 0.7828 0.048 Uiso 1 1 calc R . . C18 C -0.0468(8) 0.2528(12) 0.7173(7) 0.054(4) Uani 1 1 d . . . H18A H -0.0604 0.1849 0.6915 0.065 Uiso 1 1 calc R . . H18B H -0.0878 0.2609 0.7522 0.065 Uiso 1 1 calc R . . C19 C -0.0563(7) 0.3478(12) 0.6664(6) 0.058(4) Uani 1 1 d . . . H19A H -0.0509 0.4155 0.6936 0.069 Uiso 1 1 calc R . . H19B H -0.1147 0.3461 0.6402 0.069 Uiso 1 1 calc R . . C20 C 0.0112(7) 0.3483(10) 0.6138(5) 0.055(3) Uani 1 1 d . . . H20A H 0.0047 0.4151 0.5857 0.066 Uiso 1 1 calc R . . H20B H 0.0002 0.2867 0.5815 0.066 Uiso 1 1 calc R . . C21 C 0.1063(7) 0.3412(10) 0.6517(5) 0.047(3) Uani 1 1 d . . . H21A H 0.1472 0.3330 0.6167 0.056 Uiso 1 1 calc R . . H21B H 0.1210 0.4081 0.6782 0.056 Uiso 1 1 calc R . . C22 C 0.1141(6) 0.2446(9) 0.7015(5) 0.040(2) Uani 1 1 d . . . H22A H 0.0999 0.1791 0.6723 0.047 Uiso 1 1 calc R . . C23 C 0.2715(9) 0.2678(13) 0.7242(6) 0.055(4) Uani 1 1 d . . . H23A H 0.2634 0.3181 0.6870 0.066 Uiso 1 1 calc R . . C24 C 0.3627(8) 0.2454(11) 0.7554(6) 0.043(3) Uani 1 1 d . . . C25 C 0.3824(7) 0.1650(9) 0.8095(5) 0.032(3) Uani 1 1 d . . . C26 C 0.4731(8) 0.1434(11) 0.8312(6) 0.049(4) Uani 1 1 d . . . C27 C 0.5366(8) 0.2075(11) 0.7999(6) 0.046(3) Uani 1 1 d . . . H27A H 0.5957 0.1963 0.8162 0.055 Uiso 1 1 calc R . . C28 C 0.5164(8) 0.2838(10) 0.7479(6) 0.047(3) Uani 1 1 d . . . C29 C 0.4281(8) 0.3029(10) 0.7258(7) 0.047(3) Uani 1 1 d . . . H29A H 0.4122 0.3549 0.6906 0.057 Uiso 1 1 calc R . . C30 C 0.5016(7) 0.0552(11) 0.8878(6) 0.045(3) Uani 1 1 d . . . C31 C 0.4628(8) 0.0749(14) 0.9564(6) 0.079(5) Uani 1 1 d . . . H31A H 0.4813 0.0176 0.9897 0.118 Uiso 1 1 calc R . . H31B H 0.3998 0.0752 0.9470 0.118 Uiso 1 1 calc R . . H31C H 0.4828 0.1444 0.9761 0.118 Uiso 1 1 calc R . . C32 C 0.4739(9) -0.0561(11) 0.8586(7) 0.075(4) Uani 1 1 d . . . H32A H 0.4922 -0.1113 0.8935 0.113 Uiso 1 1 calc R . . H32B H 0.5009 -0.0699 0.8163 0.113 Uiso 1 1 calc R . . H32C H 0.4111 -0.0581 0.8475 0.113 Uiso 1 1 calc R . . C33 C 0.6018(8) 0.0495(13) 0.9076(8) 0.086(5) Uani 1 1 d . . . H33A H 0.6160 -0.0081 0.9416 0.129 Uiso 1 1 calc R . . H33B H 0.6228 0.1182 0.9278 0.129 Uiso 1 1 calc R . . H33C H 0.6294 0.0348 0.8656 0.129 Uiso 1 1 calc R . . C34 C 0.5862(8) 0.3469(11) 0.7158(6) 0.045(3) Uani 1 1 d . . . C35 C 0.6708(10) 0.3479(14) 0.7452(9) 0.101(6) Uani 1 1 d . . . H35A H 0.6848 0.3082 0.7870 0.121 Uiso 1 1 calc R . . C36 C 0.7172(10) 0.4546(14) 0.6588(8) 0.077(5) Uani 1 1 d . . . H36A H 0.7614 0.4910 0.6385 0.093 Uiso 1 1 calc R . . C37 C 0.6346(10) 0.4573(17) 0.6261(7) 0.098(6) Uani 1 1 d . . . H37A H 0.6223 0.4964 0.5838 0.118 Uiso 1 1 calc R . . C38 C 0.5673(10) 0.4031(16) 0.6539(9) 0.100(7) Uani 1 1 d . . . H38A H 0.5102 0.4050 0.6308 0.120 Uiso 1 1 calc R . . C39 C 0.2245(8) -0.0893(11) 0.7361(6) 0.041(3) Uani 1 1 d . . . C40 C 0.5668(8) 0.6526(11) 0.7745(7) 0.052(4) Uani 1 1 d . . . H40A H 0.5811 0.5973 0.8078 0.063 Uiso 1 1 calc R . . C41 C 0.6364(8) 0.7082(11) 0.7453(6) 0.041(3) Uani 1 1 d . . . C42 C 0.6119(8) 0.7892(11) 0.6917(6) 0.045(3) Uani 1 1 d . . . C43 C 0.5233(8) 0.8153(11) 0.6705(6) 0.045(3) Uani 1 1 d . . . C44 C 0.4949(8) 0.9049(12) 0.6151(7) 0.053(4) Uani 1 1 d . . . C45 C 0.5252(10) 0.8798(15) 0.5450(7) 0.096(6) Uani 1 1 d . . . H45A H 0.4981 0.8132 0.5264 0.144 Uiso 1 1 calc R . . H45B H 0.5880 0.8713 0.5510 0.144 Uiso 1 1 calc R . . H45C H 0.5090 0.9389 0.5125 0.144 Uiso 1 1 calc R . . C46 C 0.5382(10) 1.0164(12) 0.6410(8) 0.087(5) Uani 1 1 d . . . H46A H 0.6010 1.0076 0.6495 0.130 Uiso 1 1 calc R . . H46B H 0.5164 1.0385 0.6842 0.130 Uiso 1 1 calc R . . H46C H 0.5240 1.0714 0.6051 0.130 Uiso 1 1 calc R . . C47 C 0.3951(9) 0.9156(16) 0.6021(9) 0.128(8) Uani 1 1 d . . . H47A H 0.3699 0.8472 0.5848 0.192 Uiso 1 1 calc R . . H47B H 0.3794 0.9720 0.5675 0.192 Uiso 1 1 calc R . . H47C H 0.3730 0.9344 0.6459 0.192 Uiso 1 1 calc R . . C48 C 0.4619(8) 0.7613(11) 0.7040(6) 0.048(3) Uani 1 1 d . . . H48A H 0.4033 0.7811 0.6923 0.058 Uiso 1 1 calc R . . C49 C 0.4809(8) 0.6773(11) 0.7554(6) 0.048(4) Uani 1 1 d . . . C50 C 0.4083(8) 0.6186(11) 0.7865(6) 0.051(3) Uani 1 1 d . . . C51 C 0.4187(11) 0.5668(17) 0.8484(8) 0.102(7) Uani 1 1 d . . . H51A H 0.4732 0.5708 0.8759 0.122 Uiso 1 1 calc R . . C52 C 0.2750(10) 0.4991(13) 0.8309(10) 0.077(5) Uani 1 1 d . . . H52A H 0.2289 0.4601 0.8465 0.092 Uiso 1 1 calc R . . C53 C 0.2635(9) 0.5435(13) 0.7697(8) 0.072(5) Uani 1 1 d . . . H53A H 0.2101 0.5369 0.7407 0.086 Uiso 1 1 calc R . . C54 C 0.3282(10) 0.5982(16) 0.7488(9) 0.098(6) Uani 1 1 d . . . H54A H 0.3191 0.6267 0.7029 0.118 Uiso 1 1 calc R . . C55 C 0.7247(8) 0.6730(11) 0.7642(6) 0.050(3) Uani 1 1 d . . . H55A H 0.7318 0.6143 0.7957 0.060 Uiso 1 1 calc R . . C56 C 0.8804(6) 0.6585(8) 0.7653(5) 0.039(2) Uani 1 1 d . . . H56A H 0.8927 0.6113 0.7258 0.047 Uiso 1 1 calc R . . C57 C 0.8888(8) 0.5875(11) 0.8319(6) 0.053(3) Uani 1 1 d . . . H57A H 0.8494 0.5251 0.8247 0.064 Uiso 1 1 calc R . . H57B H 0.8730 0.6296 0.8719 0.064 Uiso 1 1 calc R . . C58 C 0.9849(7) 0.5474(9) 0.8475(6) 0.060(3) Uani 1 1 d . . . H58A H 0.9914 0.5051 0.8912 0.072 Uiso 1 1 calc R . . H58B H 0.9980 0.4995 0.8093 0.072 Uiso 1 1 calc R . . C59 C 1.0499(8) 0.6410(11) 0.8546(6) 0.061(4) Uani 1 1 d . . . H59A H 1.1093 0.6124 0.8640 0.074 Uiso 1 1 calc R . . H59B H 1.0390 0.6876 0.8942 0.074 Uiso 1 1 calc R . . C60 C 1.0402(8) 0.7095(11) 0.7842(6) 0.055(4) Uani 1 1 d . . . H60A H 1.0815 0.7701 0.7885 0.066 Uiso 1 1 calc R . . H60B H 1.0528 0.6637 0.7447 0.066 Uiso 1 1 calc R . . C61 C 0.9492(7) 0.7516(9) 0.7710(5) 0.041(3) Uani 1 1 d . . . H61A H 0.9392 0.7967 0.8122 0.049 Uiso 1 1 calc R . . C62 C 0.9861(8) 0.8639(10) 0.6744(6) 0.046(3) Uani 1 1 d . . . H62A H 1.0441 0.8457 0.6905 0.055 Uiso 1 1 calc R . . C63 C 0.9719(7) 0.9407(10) 0.6138(5) 0.034(3) Uani 1 1 d . . . C64 C 0.8856(8) 0.9769(10) 0.5852(6) 0.038(3) Uani 1 1 d . . . C65 C 0.8786(8) 1.0559(11) 0.5312(6) 0.042(3) Uani 1 1 d . . . C66 C 0.9566(7) 1.0948(10) 0.5066(5) 0.034(3) Uani 1 1 d . . . H66A H 0.9517 1.1476 0.4709 0.041 Uiso 1 1 calc R . . C67 C 1.0432(7) 1.0572(10) 0.5340(6) 0.038(3) Uani 1 1 d . . . C68 C 1.0481(7) 0.9763(10) 0.5867(5) 0.040(3) Uani 1 1 d . . . H68A H 1.1023 0.9460 0.6038 0.048 Uiso 1 1 calc R . . C69 C 0.7903(8) 1.1032(13) 0.4983(6) 0.051(4) Uani 1 1 d . . . C70 C 0.7306(9) 1.0103(12) 0.4626(7) 0.070(5) Uani 1 1 d . . . H70A H 0.7208 0.9562 0.4976 0.105 Uiso 1 1 calc R . . H70B H 0.7589 0.9767 0.4256 0.105 Uiso 1 1 calc R . . H70C H 0.6752 1.0408 0.4426 0.105 Uiso 1 1 calc R . . C71 C 0.7444(9) 1.1590(14) 0.5565(7) 0.080(5) Uani 1 1 d . . . H71A H 0.7813 1.2164 0.5783 0.120 Uiso 1 1 calc R . . H71B H 0.7338 1.1059 0.5920 0.120 Uiso 1 1 calc R . . H71C H 0.6894 1.1896 0.5358 0.120 Uiso 1 1 calc R . . C72 C 0.7995(9) 1.1889(13) 0.4397(8) 0.089(6) Uani 1 1 d . . . H72A H 0.8366 1.2477 0.4591 0.134 Uiso 1 1 calc R . . H72B H 0.7425 1.2173 0.4222 0.134 Uiso 1 1 calc R . . H72C H 0.8252 1.1549 0.4014 0.134 Uiso 1 1 calc R . . C73 C 1.1214(7) 1.1051(10) 0.5098(6) 0.036(3) Uani 1 1 d . . . C74 C 1.1226(8) 1.1555(10) 0.4439(5) 0.046(3) Uani 1 1 d . . . H74A H 1.0704 1.1546 0.4132 0.055 Uiso 1 1 calc R . . C75 C 1.2653(8) 1.2053(11) 0.4659(7) 0.050(3) Uani 1 1 d . . . H75A H 1.3141 1.2419 0.4528 0.060 Uiso 1 1 calc R . . C76 C 1.2742(8) 1.1540(11) 0.5320(7) 0.052(4) Uani 1 1 d . . . H76A H 1.3280 1.1524 0.5607 0.062 Uiso 1 1 calc R . . C77 C 1.2006(8) 1.1057(12) 0.5536(7) 0.055(4) Uani 1 1 d . . . H77A H 1.2041 1.0730 0.5982 0.066 Uiso 1 1 calc R . . C78 C 0.7700(9) 1.0410(14) 0.7652(7) 0.058(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0357(10) 0.0411(12) 0.0311(9) 0.0073(9) 0.0007(8) 0.0039(9) Mn2 0.0375(11) 0.0435(12) 0.0300(9) 0.0060(9) 0.0032(8) 0.0009(9) N1 0.032(5) 0.028(5) 0.025(4) 0.000(4) -0.006(4) -0.004(4) N2 0.035(5) 0.047(6) 0.034(5) 0.004(4) 0.007(4) 0.006(5) N3 0.046(6) 0.039(6) 0.036(5) 0.008(5) -0.001(5) -0.001(5) N4 0.056(9) 0.124(13) 0.153(14) 0.072(12) 0.011(9) -0.007(8) N5 0.037(5) 0.048(6) 0.031(5) 0.005(4) 0.013(4) 0.003(5) N6 0.046(6) 0.034(5) 0.033(5) -0.001(4) 0.008(4) -0.010(5) N7 0.134(16) 0.22(2) 0.128(15) 0.058(16) 0.032(13) -0.058(16) N8 0.036(6) 0.056(7) 0.048(6) 0.012(5) 0.013(5) 0.001(5) O1 0.045(5) 0.045(5) 0.047(5) 0.007(4) 0.008(4) -0.013(4) O2 0.033(4) 0.052(5) 0.031(4) 0.005(5) 0.008(3) -0.001(4) O3 0.045(5) 0.059(6) 0.044(4) -0.008(4) -0.006(4) 0.002(4) O4 0.079(7) 0.080(8) 0.068(6) -0.041(7) -0.023(5) 0.020(7) O5 0.040(5) 0.057(6) 0.036(4) 0.010(5) 0.003(4) 0.004(5) O6 0.040(5) 0.052(5) 0.030(4) 0.024(4) -0.002(4) 0.000(4) O7 0.076(6) 0.050(5) 0.046(5) 0.001(4) -0.001(4) 0.015(5) O8 0.081(7) 0.067(7) 0.073(7) -0.016(7) -0.001(6) 0.016(7) C1 0.059(8) 0.035(8) 0.025(6) 0.001(6) -0.020(6) 0.003(7) C2 0.042(7) 0.052(8) 0.027(6) 0.002(6) 0.007(5) -0.003(6) C3 0.055(9) 0.070(10) 0.036(7) 0.009(7) 0.015(6) 0.003(8) C4 0.039(7) 0.039(7) 0.028(6) 0.001(6) 0.014(5) -0.015(6) C5 0.043(7) 0.044(8) 0.037(7) -0.008(7) -0.011(6) 0.000(6) C6 0.045(8) 0.037(8) 0.034(6) 0.005(6) 0.007(6) 0.002(6) C7 0.046(8) 0.052(9) 0.051(7) 0.003(7) 0.005(6) -0.003(7) C8 0.041(8) 0.118(14) 0.058(9) -0.002(10) -0.004(7) 0.007(9) C9 0.055(8) 0.065(10) 0.078(10) -0.006(8) 0.009(7) 0.032(8) C10 0.055(9) 0.161(18) 0.088(11) 0.080(12) 0.016(9) 0.036(11) C11 0.051(8) 0.037(8) 0.039(7) -0.010(7) 0.005(6) -0.008(7) C12 0.031(6) 0.061(8) 0.038(6) 0.012(7) -0.002(5) -0.008(7) C13 0.072(10) 0.064(10) 0.042(7) 0.018(7) 0.000(7) -0.005(8) C14 0.036(7) 0.047(8) 0.080(9) 0.008(7) 0.020(7) 0.003(6) C15 0.032(6) 0.029(7) 0.042(7) -0.005(6) 0.009(5) -0.010(5) C16 0.034(6) 0.034(6) 0.031(5) -0.006(5) 0.001(5) 0.001(5) C17 0.044(6) 0.035(6) 0.036(6) 0.001(5) -0.015(5) 0.004(5) C18 0.043(8) 0.066(10) 0.052(7) 0.011(8) -0.003(6) 0.016(7) C19 0.035(6) 0.087(10) 0.048(7) -0.003(7) -0.008(5) 0.000(7) C20 0.058(7) 0.058(8) 0.047(6) 0.021(6) -0.005(6) -0.002(6) C21 0.042(6) 0.053(8) 0.042(6) 0.028(6) -0.009(5) -0.008(6) C22 0.033(6) 0.057(7) 0.030(5) 0.009(5) 0.006(4) 0.007(5) C23 0.067(9) 0.071(9) 0.027(6) 0.006(6) 0.006(6) 0.013(8) C24 0.040(7) 0.046(8) 0.043(7) 0.003(7) 0.007(6) 0.004(6) C25 0.035(7) 0.030(7) 0.027(6) -0.005(5) -0.004(5) -0.004(6) C26 0.043(8) 0.062(10) 0.040(7) 0.009(7) -0.002(6) 0.020(7) C27 0.032(7) 0.056(9) 0.051(7) -0.006(7) 0.006(6) -0.004(6) C28 0.054(9) 0.032(8) 0.054(8) -0.007(6) 0.006(7) -0.020(7) C29 0.038(8) 0.048(9) 0.055(8) 0.015(7) 0.000(6) -0.007(6) C30 0.030(7) 0.051(9) 0.055(8) 0.002(7) 0.007(6) 0.003(6) C31 0.071(9) 0.120(15) 0.044(7) 0.019(9) 0.003(7) 0.035(9) C32 0.091(12) 0.059(10) 0.072(10) -0.003(8) -0.007(8) 0.004(8) C33 0.057(10) 0.086(11) 0.107(12) 0.012(10) -0.024(8) -0.008(9) C34 0.041(7) 0.053(8) 0.045(7) -0.002(7) 0.016(6) 0.000(7) C35 0.063(10) 0.096(13) 0.146(15) 0.080(13) 0.018(10) 0.026(10) C36 0.068(11) 0.087(12) 0.083(11) 0.019(10) 0.030(9) -0.009(10) C37 0.064(10) 0.171(18) 0.055(9) 0.033(11) -0.017(8) -0.037(11) C38 0.053(9) 0.156(18) 0.084(11) 0.048(12) -0.023(8) -0.051(11) C39 0.037(7) 0.041(8) 0.047(8) -0.017(7) 0.009(6) -0.011(6) C40 0.049(9) 0.061(10) 0.045(7) 0.003(7) 0.001(6) 0.002(7) C41 0.039(7) 0.054(9) 0.029(6) 0.003(6) -0.005(5) 0.002(7) C42 0.048(8) 0.050(9) 0.039(7) -0.003(7) 0.016(6) 0.012(7) C43 0.043(8) 0.049(9) 0.044(7) -0.012(7) 0.008(6) -0.019(7) C44 0.043(8) 0.065(10) 0.047(8) 0.017(7) -0.013(6) 0.018(7) C45 0.110(14) 0.111(15) 0.065(10) 0.013(11) 0.001(9) 0.021(11) C46 0.102(13) 0.059(11) 0.099(13) 0.021(10) 0.008(10) 0.004(9) C47 0.053(10) 0.154(18) 0.181(18) 0.124(15) 0.024(11) 0.031(11) C48 0.046(8) 0.046(8) 0.050(7) -0.001(7) -0.007(6) -0.007(7) C49 0.044(8) 0.068(10) 0.033(7) 0.003(7) 0.009(6) 0.014(7) C50 0.055(8) 0.047(8) 0.047(7) 0.006(7) -0.006(6) -0.018(7) C51 0.060(10) 0.17(2) 0.070(11) 0.042(12) 0.005(8) -0.034(11) C52 0.048(9) 0.064(11) 0.121(15) -0.005(11) 0.019(10) -0.019(8) C53 0.045(9) 0.087(11) 0.077(10) 0.031(9) -0.018(7) -0.036(8) C54 0.071(11) 0.122(15) 0.100(12) 0.008(12) 0.000(9) -0.048(11) C55 0.055(8) 0.040(7) 0.054(7) 0.012(6) 0.005(6) 0.013(7) C56 0.045(6) 0.043(6) 0.030(5) 0.008(5) 0.007(5) 0.018(5) C57 0.055(7) 0.054(8) 0.050(7) 0.005(6) 0.009(6) -0.003(6) C58 0.068(8) 0.046(7) 0.063(8) 0.012(6) -0.004(6) 0.025(7) C59 0.045(7) 0.080(11) 0.058(8) 0.044(7) 0.002(6) 0.013(7) C60 0.049(8) 0.065(10) 0.051(8) 0.022(7) 0.007(6) 0.008(7) C61 0.053(7) 0.039(6) 0.028(5) 0.014(5) -0.009(5) -0.005(5) C62 0.052(8) 0.042(8) 0.039(7) -0.003(6) -0.005(6) 0.011(6) C63 0.034(7) 0.044(8) 0.022(6) 0.003(5) -0.008(5) 0.013(6) C64 0.046(8) 0.043(8) 0.028(6) -0.004(6) 0.019(6) 0.000(6) C65 0.041(7) 0.045(8) 0.039(7) 0.005(6) -0.001(6) 0.002(6) C66 0.046(7) 0.034(7) 0.020(5) 0.003(5) -0.004(5) 0.008(6) C67 0.043(7) 0.040(7) 0.028(6) 0.000(6) -0.009(5) 0.009(6) C68 0.031(7) 0.060(9) 0.032(6) 0.006(7) 0.015(5) 0.008(6) C69 0.049(8) 0.070(10) 0.036(6) 0.033(8) 0.012(6) 0.025(8) C70 0.074(11) 0.070(11) 0.058(9) -0.004(8) -0.021(8) 0.013(9) C71 0.077(11) 0.094(13) 0.064(9) 0.025(9) -0.013(8) 0.010(10) C72 0.061(9) 0.102(14) 0.105(12) 0.078(11) 0.013(9) 0.019(9) C73 0.037(7) 0.038(7) 0.037(6) 0.017(6) 0.015(5) 0.015(6) C74 0.050(8) 0.059(9) 0.025(6) 0.002(6) -0.011(5) -0.006(7) C75 0.037(7) 0.053(9) 0.060(8) 0.022(7) 0.011(6) 0.002(6) C76 0.035(7) 0.063(10) 0.053(8) 0.017(7) -0.016(6) -0.008(7) C77 0.057(8) 0.055(9) 0.054(8) 0.027(8) 0.006(7) 0.001(8) C78 0.069(10) 0.059(10) 0.045(8) 0.006(8) -0.005(7) 0.017(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.852(8) . ? Mn1 O2 1.891(7) . ? Mn1 N2 1.962(10) . ? Mn1 N1 1.994(9) . ? Mn1 O3 2.111(8) . ? Mn2 O6 1.884(7) . ? Mn2 O5 1.896(8) . ? Mn2 N5 1.982(9) . ? Mn2 N6 1.997(10) . ? Mn2 O7 2.095(9) . ? Mn2 N8 2.514(10) 2_746 ? N1 C16 1.290(12) . ? N1 C17 1.465(13) . ? N2 C23 1.277(15) . ? N2 C22 1.509(13) . ? N3 C15 1.305(13) . ? N3 C14 1.352(15) . ? N4 C36 1.312(19) . ? N4 C35 1.351(17) . ? N5 C55 1.262(14) . ? N5 C56 1.460(12) . ? N6 C62 1.251(13) . ? N6 C61 1.495(12) . ? N7 C52 1.36(2) . ? N7 C51 1.393(19) . ? N8 C75 1.324(14) . ? N8 C74 1.359(14) . ? N8 Mn2 2.514(10) 2_756 ? O1 C1 1.318(13) . ? O2 C25 1.300(12) . ? O3 C39 1.248(14) . ? O4 C39 1.188(14) . ? O5 C42 1.324(13) . ? O6 C64 1.322(12) . ? O7 C78 1.234(16) . ? O8 C78 1.227(16) . ? C1 C6 1.434(15) . ? C1 C2 1.441(16) . ? C2 C3 1.366(15) . ? C2 C7 1.551(17) . ? C3 C4 1.390(15) . ? C4 C5 1.382(15) . ? C4 C11 1.469(14) . ? C5 C6 1.399(14) . ? C6 C16 1.417(15) . ? C7 C8 1.509(19) . ? C7 C9 1.537(16) . ? C7 C10 1.547(18) . ? C11 C15 1.402(14) . ? C11 C12 1.416(16) . ? C12 C13 1.367(16) . ? C13 C14 1.402(17) . ? C17 C22 1.510(13) . ? C17 C18 1.566(16) . ? C18 C19 1.502(17) . ? C19 C20 1.520(14) . ? C20 C21 1.546(14) . ? C21 C22 1.504(14) . ? C23 C24 1.475(17) . ? C24 C29 1.395(15) . ? C24 C25 1.422(15) . ? C25 C26 1.424(15) . ? C26 C27 1.431(16) . ? C26 C30 1.543(16) . ? C27 C28 1.363(16) . ? C28 C29 1.386(15) . ? C28 C34 1.503(15) . ? C30 C32 1.506(17) . ? C30 C31 1.511(14) . ? C30 C33 1.536(15) . ? C34 C35 1.345(18) . ? C34 C38 1.358(18) . ? C36 C37 1.341(19) . ? C37 C38 1.381(18) . ? C40 C49 1.355(15) . ? C40 C41 1.428(16) . ? C41 C55 1.422(16) . ? C41 C42 1.434(16) . ? C42 C43 1.403(16) . ? C43 C48 1.366(15) . ? C43 C44 1.540(17) . ? C44 C45 1.488(17) . ? C44 C47 1.524(16) . ? C44 C46 1.565(19) . ? C48 C49 1.418(17) . ? C49 C50 1.502(16) . ? C50 C51 1.322(19) . ? C50 C54 1.365(18) . ? C52 C53 1.27(2) . ? C53 C54 1.296(17) . ? C56 C57 1.521(14) . ? C56 C61 1.544(14) . ? C57 C58 1.544(15) . ? C58 C59 1.510(16) . ? C59 C60 1.564(15) . ? C60 C61 1.478(15) . ? C62 C63 1.475(15) . ? C63 C68 1.400(14) . ? C63 C64 1.435(15) . ? C64 C65 1.399(16) . ? C65 C66 1.416(14) . ? C65 C69 1.531(16) . ? C66 C67 1.439(13) . ? C67 C68 1.398(15) . ? C67 C73 1.455(15) . ? C69 C71 1.536(17) . ? C69 C72 1.542(16) . ? C69 C70 1.558(19) . ? C73 C77 1.383(16) . ? C73 C74 1.391(14) . ? C75 C76 1.392(16) . ? C76 C77 1.377(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O2 94.2(3) . . ? O1 Mn1 N2 174.7(4) . . ? O2 Mn1 N2 90.4(4) . . ? O1 Mn1 N1 92.7(3) . . ? O2 Mn1 N1 168.2(4) . . ? N2 Mn1 N1 82.3(4) . . ? O1 Mn1 O3 93.4(3) . . ? O2 Mn1 O3 97.9(3) . . ? N2 Mn1 O3 88.5(3) . . ? N1 Mn1 O3 91.3(3) . . ? O6 Mn2 O5 93.6(4) . . ? O6 Mn2 N5 169.9(4) . . ? O5 Mn2 N5 91.8(4) . . ? O6 Mn2 N6 92.0(3) . . ? O5 Mn2 N6 173.9(4) . . ? N5 Mn2 N6 82.3(4) . . ? O6 Mn2 O7 97.3(4) . . ? O5 Mn2 O7 93.0(4) . . ? N5 Mn2 O7 90.9(4) . . ? N6 Mn2 O7 88.8(4) . . ? O6 Mn2 N8 83.6(3) . 2_746 ? O5 Mn2 N8 89.9(4) . 2_746 ? N5 Mn2 N8 87.9(4) . 2_746 ? N6 Mn2 N8 88.2(3) . 2_746 ? O7 Mn2 N8 176.9(4) . 2_746 ? C16 N1 C17 124.0(9) . . ? C16 N1 Mn1 122.6(8) . . ? C17 N1 Mn1 113.4(6) . . ? C23 N2 C22 119.7(10) . . ? C23 N2 Mn1 127.4(9) . . ? C22 N2 Mn1 112.7(7) . . ? C15 N3 C14 117.5(10) . . ? C36 N4 C35 117.0(15) . . ? C55 N5 C56 122.4(10) . . ? C55 N5 Mn2 123.0(9) . . ? C56 N5 Mn2 114.6(7) . . ? C62 N6 C61 122.2(10) . . ? C62 N6 Mn2 126.0(9) . . ? C61 N6 Mn2 111.8(6) . . ? C52 N7 C51 116.2(16) . . ? C75 N8 C74 114.5(10) . . ? C75 N8 Mn2 112.2(8) . 2_756 ? C74 N8 Mn2 131.5(8) . 2_756 ? C1 O1 Mn1 130.9(7) . . ? C25 O2 Mn1 132.9(8) . . ? C39 O3 Mn1 129.6(8) . . ? C42 O5 Mn2 131.2(8) . . ? C64 O6 Mn2 130.2(7) . . ? C78 O7 Mn2 127.2(9) . . ? O1 C1 C6 121.3(11) . . ? O1 C1 C2 121.0(11) . . ? C6 C1 C2 117.6(11) . . ? C3 C2 C1 118.0(12) . . ? C3 C2 C7 123.7(12) . . ? C1 C2 C7 118.2(10) . . ? C2 C3 C4 125.4(13) . . ? C5 C4 C3 116.8(10) . . ? C5 C4 C11 120.6(11) . . ? C3 C4 C11 122.6(11) . . ? C4 C5 C6 121.8(11) . . ? C5 C6 C16 116.9(11) . . ? C5 C6 C1 120.3(11) . . ? C16 C6 C1 122.9(11) . . ? C8 C7 C9 109.0(11) . . ? C8 C7 C10 109.3(12) . . ? C9 C7 C10 106.6(12) . . ? C8 C7 C2 111.8(12) . . ? C9 C7 C2 111.4(11) . . ? C10 C7 C2 108.7(10) . . ? C15 C11 C12 115.3(11) . . ? C15 C11 C4 122.9(11) . . ? C12 C11 C4 121.7(10) . . ? C13 C12 C11 119.6(11) . . ? C12 C13 C14 119.5(13) . . ? N3 C14 C13 121.6(12) . . ? N3 C15 C11 126.1(11) . . ? N1 C16 C6 128.3(11) . . ? N1 C17 C22 108.4(8) . . ? N1 C17 C18 115.8(9) . . ? C22 C17 C18 110.0(8) . . ? C19 C18 C17 109.7(10) . . ? C18 C19 C20 113.8(11) . . ? C19 C20 C21 111.9(9) . . ? C22 C21 C20 109.5(9) . . ? C21 C22 N2 117.4(9) . . ? C21 C22 C17 113.2(9) . . ? N2 C22 C17 105.2(7) . . ? N2 C23 C24 125.5(12) . . ? C29 C24 C25 122.5(11) . . ? C29 C24 C23 115.9(11) . . ? C25 C24 C23 121.5(11) . . ? O2 C25 C24 122.0(10) . . ? O2 C25 C26 121.4(11) . . ? C24 C25 C26 116.7(10) . . ? C25 C26 C27 117.9(11) . . ? C25 C26 C30 120.9(11) . . ? C27 C26 C30 121.2(11) . . ? C28 C27 C26 124.5(11) . . ? C27 C28 C29 117.4(11) . . ? C27 C28 C34 122.1(12) . . ? C29 C28 C34 120.5(12) . . ? C28 C29 C24 121.0(12) . . ? C32 C30 C31 109.6(12) . . ? C32 C30 C33 106.1(11) . . ? C31 C30 C33 106.5(11) . . ? C32 C30 C26 109.2(11) . . ? C31 C30 C26 112.2(11) . . ? C33 C30 C26 113.0(10) . . ? C35 C34 C38 116.5(13) . . ? C35 C34 C28 122.2(12) . . ? C38 C34 C28 121.2(12) . . ? C34 C35 N4 125.4(14) . . ? N4 C36 C37 121.2(15) . . ? C36 C37 C38 121.2(15) . . ? C34 C38 C37 118.7(14) . . ? O4 C39 O3 127.8(13) . . ? C49 C40 C41 122.5(12) . . ? C55 C41 C40 119.4(12) . . ? C55 C41 C42 123.0(11) . . ? C40 C41 C42 117.2(11) . . ? O5 C42 C43 119.1(11) . . ? O5 C42 C41 119.7(11) . . ? C43 C42 C41 121.2(11) . . ? C48 C43 C42 117.0(12) . . ? C48 C43 C44 120.3(11) . . ? C42 C43 C44 122.5(11) . . ? C45 C44 C47 106.8(13) . . ? C45 C44 C43 111.7(12) . . ? C47 C44 C43 111.4(11) . . ? C45 C44 C46 106.9(13) . . ? C47 C44 C46 110.8(13) . . ? C43 C44 C46 109.2(10) . . ? C43 C48 C49 124.8(12) . . ? C40 C49 C48 117.1(12) . . ? C40 C49 C50 122.0(12) . . ? C48 C49 C50 120.9(11) . . ? C51 C50 C54 112.4(14) . . ? C51 C50 C49 124.1(12) . . ? C54 C50 C49 122.8(12) . . ? C50 C51 N7 123.3(16) . . ? C53 C52 N7 122.5(15) . . ? C52 C53 C54 118.1(15) . . ? C53 C54 C50 127.3(16) . . ? N5 C55 C41 129.6(12) . . ? N5 C56 C57 116.8(8) . . ? N5 C56 C61 106.7(8) . . ? C57 C56 C61 111.8(9) . . ? C56 C57 C58 108.7(9) . . ? C59 C58 C57 112.4(10) . . ? C58 C59 C60 109.5(10) . . ? C61 C60 C59 108.6(9) . . ? C60 C61 N6 116.4(8) . . ? C60 C61 C56 112.2(9) . . ? N6 C61 C56 106.1(8) . . ? N6 C62 C63 126.3(11) . . ? C68 C63 C64 122.4(10) . . ? C68 C63 C62 115.6(10) . . ? C64 C63 C62 122.0(10) . . ? O6 C64 C65 118.8(11) . . ? O6 C64 C63 122.8(10) . . ? C65 C64 C63 118.2(10) . . ? C64 C65 C66 118.5(11) . . ? C64 C65 C69 122.8(11) . . ? C66 C65 C69 118.6(11) . . ? C65 C66 C67 123.5(11) . . ? C68 C67 C66 116.7(10) . . ? C68 C67 C73 122.2(10) . . ? C66 C67 C73 121.0(11) . . ? C67 C68 C63 120.4(11) . . ? C65 C69 C71 109.5(11) . . ? C65 C69 C72 113.2(10) . . ? C71 C69 C72 107.8(12) . . ? C65 C69 C70 110.2(12) . . ? C71 C69 C70 109.7(11) . . ? C72 C69 C70 106.3(11) . . ? C77 C73 C74 115.4(11) . . ? C77 C73 C67 120.5(10) . . ? C74 C73 C67 124.1(11) . . ? N8 C74 C73 126.4(11) . . ? N8 C75 C76 125.0(12) . . ? C77 C76 C75 117.7(12) . . ? C76 C77 C73 120.9(11) . . ? O8 C78 O7 129.8(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.493 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.086 # Attachment 'CIF of 3.cif' data_3 #TrackingRef 'CIF of 3.cif' _database_code_depnum_ccdc_archive 'CCDC 761765' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H88 N8 Ni2 O6' _chemical_formula_weight 1326.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.564(2) _cell_length_b 18.821(4) _cell_length_c 17.117(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.68(3) _cell_angle_gamma 90.00 _cell_volume 3661.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28652 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 25.00 _exptl_crystal_description block-like _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.569 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.915 _exptl_absorpt_correction_T_max 0.945 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28652 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12013 _reflns_number_gt 8231 _reflns_threshold_expression >2sigma(I) _chemical_absolute_configuration ad _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _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 _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^)+(0.0719P)^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 geom _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 -0.036(19) _refine_ls_number_reflns 12013 _refine_ls_number_parameters 829 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1414 _refine_ls_wR_factor_gt 0.1249 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 0.68329(7) 0.68513(3) 1.13424(4) 0.0340(2) Uani 1 1 d . . . Ni2 Ni 0.17659(7) 0.40267(3) 0.63752(4) 0.0336(2) Uani 1 1 d . . . C1 C 0.1586(9) 0.9243(6) 0.9476(6) 0.084(3) Uani 1 1 d . . . H1A H 0.2177 0.9483 0.9818 0.101 Uiso 1 1 calc R . . C2 C 0.1609(8) 0.8525(6) 0.9469(5) 0.066(2) Uani 1 1 d . . . C3 C 0.0677(11) 0.8241(7) 0.8952(6) 0.093(3) Uani 1 1 d . . . H3A H 0.0655 0.7747 0.8933 0.112 Uiso 1 1 calc R . . C4 C -0.0120(14) 0.8536(11) 0.8517(9) 0.133(6) Uani 1 1 d . . . H4A H -0.0713 0.8268 0.8210 0.160 Uiso 1 1 calc R . . C5 C -0.0153(14) 0.9213(15) 0.8477(9) 0.177(11) Uani 1 1 d . . . H5A H -0.0741 0.9433 0.8113 0.212 Uiso 1 1 calc R . . C6 C 0.2532(7) 0.8102(5) 0.9955(4) 0.057(2) Uani 1 1 d . . . C7 C 0.3637(7) 0.8326(5) 1.0148(4) 0.056(2) Uani 1 1 d . . . H7A H 0.3821 0.8776 0.9984 0.067 Uiso 1 1 calc R . . C8 C 0.4549(7) 0.7911(4) 1.0593(4) 0.0434(18) Uani 1 1 d . . . C9 C 0.4294(7) 0.7207(4) 1.0837(4) 0.049(2) Uani 1 1 d . . . C10 C 0.3116(7) 0.6977(5) 1.0663(4) 0.052(2) Uani 1 1 d . . . C11 C 0.2293(7) 0.7423(6) 1.0226(4) 0.067(2) Uani 1 1 d . . . H11A H 0.1521 0.7262 1.0102 0.081 Uiso 1 1 calc R . . C12 C 0.5705(8) 0.8236(4) 1.0780(4) 0.052(2) Uani 1 1 d . . . H12A H 0.5754 0.8712 1.0645 0.062 Uiso 1 1 calc R . . C13 C 0.2762(8) 0.6258(5) 1.0941(5) 0.063(2) Uani 1 1 d . . . C14 C 0.3065(10) 0.6219(7) 1.1840(5) 0.110(4) Uani 1 1 d . . . H14A H 0.2637 0.6578 1.2065 0.164 Uiso 1 1 calc R . . H14B H 0.3895 0.6294 1.2012 0.164 Uiso 1 1 calc R . . H14C H 0.2856 0.5759 1.2013 0.164 Uiso 1 1 calc R . . C15 C 0.3416(10) 0.5672(6) 1.0586(6) 0.092(3) Uani 1 1 d . . . H15A H 0.4249 0.5744 1.0742 0.137 Uiso 1 1 calc R . . H15B H 0.3203 0.5685 1.0017 0.137 Uiso 1 1 calc R . . H15C H 0.3208 0.5219 1.0777 0.137 Uiso 1 1 calc R . . C16 C 0.1462(8) 0.6101(6) 1.0702(5) 0.089(3) Uani 1 1 d . . . H16A H 0.1019 0.6454 1.0924 0.133 Uiso 1 1 calc R . . H16B H 0.1298 0.5640 1.0897 0.133 Uiso 1 1 calc R . . H16C H 0.1243 0.6108 1.0133 0.133 Uiso 1 1 calc R . . C17 C 0.7761(6) 0.8356(3) 1.1313(4) 0.0464(15) Uani 1 1 d . . . H17A H 0.7820 0.8517 1.1864 0.056 Uiso 1 1 calc R . . C18 C 0.7864(8) 0.9022(5) 1.0805(5) 0.066(2) Uani 1 1 d . . . H18A H 0.7768 0.8891 1.0249 0.079 Uiso 1 1 calc R . . H18B H 0.7251 0.9359 1.0863 0.079 Uiso 1 1 calc R . . C19 C 0.9064(7) 0.9360(4) 1.1077(5) 0.067(2) Uani 1 1 d . . . H19A H 0.9139 0.9765 1.0740 0.081 Uiso 1 1 calc R . . H19B H 0.9116 0.9533 1.1616 0.081 Uiso 1 1 calc R . . C20 C 1.0064(7) 0.8858(4) 1.1054(4) 0.066(2) Uani 1 1 d . . . H20A H 1.0804 0.9101 1.1235 0.079 Uiso 1 1 calc R . . H20B H 1.0045 0.8704 1.0511 0.079 Uiso 1 1 calc R . . C21 C 0.9983(7) 0.8202(4) 1.1588(4) 0.054(2) Uani 1 1 d . . . H21A H 1.0616 0.7873 1.1551 0.065 Uiso 1 1 calc R . . H21B H 1.0053 0.8348 1.2138 0.065 Uiso 1 1 calc R . . C22 C 0.8791(5) 0.7846(3) 1.1300(3) 0.0436(14) Uani 1 1 d . . . H22A H 0.8764 0.7713 1.0744 0.052 Uiso 1 1 calc R . . C23 C 0.9326(7) 0.6907(4) 1.2258(3) 0.0441(17) Uani 1 1 d . . . H23A H 1.0040 0.7143 1.2405 0.053 Uiso 1 1 calc R . . C24 C 0.9185(7) 0.6247(4) 1.2654(4) 0.0441(18) Uani 1 1 d . . . C25 C 0.8101(8) 0.5861(4) 1.2559(4) 0.0459(19) Uani 1 1 d . . . C26 C 0.8129(8) 0.5185(4) 1.2937(4) 0.0488(19) Uani 1 1 d . . . C27 C 0.9157(7) 0.4980(4) 1.3438(4) 0.0479(18) Uani 1 1 d . . . H27A H 0.9157 0.4549 1.3705 0.058 Uiso 1 1 calc R . . C28 C 1.0178(8) 0.5375(5) 1.3566(4) 0.054(2) Uani 1 1 d . . . C29 C 1.0188(8) 0.5990(5) 1.3155(4) 0.062(2) Uani 1 1 d . . . H29A H 1.0884 0.6248 1.3209 0.074 Uiso 1 1 calc R . . C30 C 0.7056(7) 0.4699(4) 1.2797(4) 0.0500(18) Uani 1 1 d . . . C31 C 0.6098(9) 0.4991(5) 1.3203(6) 0.090(3) Uani 1 1 d . . . H31A H 0.6410 0.5065 1.3757 0.135 Uiso 1 1 calc R . . H31B H 0.5460 0.4657 1.3149 0.135 Uiso 1 1 calc R . . H31C H 0.5818 0.5433 1.2961 0.135 Uiso 1 1 calc R . . C32 C 0.6623(10) 0.4572(7) 1.1921(5) 0.108(4) Uani 1 1 d . . . H32A H 0.6410 0.5017 1.1660 0.162 Uiso 1 1 calc R . . H32B H 0.5948 0.4266 1.1850 0.162 Uiso 1 1 calc R . . H32C H 0.7235 0.4353 1.1696 0.162 Uiso 1 1 calc R . . C33 C 0.7321(9) 0.3954(5) 1.3128(7) 0.111(4) Uani 1 1 d . . . H33A H 0.7612 0.3981 1.3691 0.167 Uiso 1 1 calc R . . H33B H 0.7905 0.3737 1.2874 0.167 Uiso 1 1 calc R . . H33C H 0.6615 0.3674 1.3030 0.167 Uiso 1 1 calc R . . C34 C 1.1247(7) 0.5107(4) 1.4099(4) 0.050(2) Uani 1 1 d . . . C35 C 1.1150(7) 0.4768(4) 1.4806(4) 0.051(2) Uani 1 1 d . . . H35A H 1.0404 0.4717 1.4929 0.062 Uiso 1 1 calc R . . C36 C 1.3142(7) 0.4597(6) 1.5134(5) 0.072(3) Uani 1 1 d . . . H36A H 1.3792 0.4412 1.5476 0.087 Uiso 1 1 calc R . . C37 C 1.3314(9) 0.4946(6) 1.4465(5) 0.093(4) Uani 1 1 d . . . H37A H 1.4072 0.5041 1.4384 0.111 Uiso 1 1 calc R . . C38 C 1.2389(8) 0.5146(6) 1.3933(5) 0.075(3) Uani 1 1 d . . . H38A H 1.2498 0.5315 1.3441 0.090 Uiso 1 1 calc R . . C39 C 0.6154(7) 0.6157(4) 0.9733(4) 0.0471(18) Uani 1 1 d . . . H39A H 0.5404 0.6246 0.9833 0.056 Uiso 1 1 calc R . . C40 C 0.6241(8) 0.5812(5) 0.9032(5) 0.064(2) Uani 1 1 d . . . C41 C 0.7319(9) 0.5665(6) 0.8895(5) 0.087(4) Uani 1 1 d . . . H41A H 0.7418 0.5398 0.8455 0.105 Uiso 1 1 calc R . . C42 C 0.8286(9) 0.5922(6) 0.9425(6) 0.100(4) Uani 1 1 d . . . H42A H 0.9039 0.5874 0.9312 0.120 Uiso 1 1 calc R . . C43 C 0.8127(9) 0.6244(5) 1.0113(5) 0.072(3) Uani 1 1 d . . . H43A H 0.8784 0.6381 1.0483 0.086 Uiso 1 1 calc R . . C44 C 0.5187(7) 0.5571(4) 0.8483(4) 0.051(2) Uani 1 1 d . . . C45 C 0.4132(7) 0.5995(4) 0.8283(4) 0.0510(19) Uani 1 1 d . . . H45A H 0.4147 0.6451 0.8495 0.061 Uiso 1 1 calc R . . C46 C 0.3138(7) 0.5783(4) 0.7817(4) 0.0445(17) Uani 1 1 d . . . C47 C 0.3085(7) 0.5077(4) 0.7509(4) 0.0453(19) Uani 1 1 d . . . C48 C 0.4092(7) 0.4634(4) 0.7661(4) 0.049(2) Uani 1 1 d . . . C49 C 0.5123(7) 0.4893(4) 0.8158(4) 0.0468(19) Uani 1 1 d . . . H49A H 0.5778 0.4598 0.8271 0.056 Uiso 1 1 calc R . . C50 C 0.2088(7) 0.6305(4) 0.7606(4) 0.054(2) Uani 1 1 d . . . C51 C 0.1101(9) 0.6064(5) 0.8018(5) 0.077(3) Uani 1 1 d . . . H51A H 0.0873 0.5588 0.7855 0.115 Uiso 1 1 calc R . . H51B H 0.0438 0.6376 0.7876 0.115 Uiso 1 1 calc R . . H51C H 0.1368 0.6076 0.8584 0.115 Uiso 1 1 calc R . . C52 C 0.2443(10) 0.7054(5) 0.7888(7) 0.103(4) Uani 1 1 d . . . H52A H 0.2741 0.7048 0.8450 0.154 Uiso 1 1 calc R . . H52B H 0.1770 0.7361 0.7776 0.154 Uiso 1 1 calc R . . H52C H 0.3043 0.7225 0.7615 0.154 Uiso 1 1 calc R . . C53 C 0.1589(9) 0.6305(6) 0.6703(5) 0.087(3) Uani 1 1 d . . . H53A H 0.1350 0.5832 0.6534 0.131 Uiso 1 1 calc R . . H53B H 0.2183 0.6466 0.6420 0.131 Uiso 1 1 calc R . . H53C H 0.0922 0.6618 0.6593 0.131 Uiso 1 1 calc R . . C54 C 0.4162(6) 0.3912(4) 0.7376(4) 0.0436(17) Uani 1 1 d . . . H54A H 0.4843 0.3658 0.7576 0.052 Uiso 1 1 calc R . . C55 C 0.3550(5) 0.2843(3) 0.6683(3) 0.0414(13) Uani 1 1 d . . . H55A H 0.3316 0.2554 0.7104 0.050 Uiso 1 1 calc R . . C56 C 0.4800(7) 0.2624(4) 0.6616(5) 0.059(2) Uani 1 1 d . . . H56A H 0.5074 0.2921 0.6225 0.071 Uiso 1 1 calc R . . H56B H 0.5318 0.2699 0.7124 0.071 Uiso 1 1 calc R . . C57 C 0.4864(7) 0.1854(4) 0.6379(4) 0.0653(19) Uani 1 1 d . . . H57A H 0.5651 0.1750 0.6290 0.078 Uiso 1 1 calc R . . H57B H 0.4714 0.1554 0.6810 0.078 Uiso 1 1 calc R . . C58 C 0.3996(6) 0.1683(3) 0.5643(4) 0.0556(17) Uani 1 1 d . . . H58A H 0.4017 0.1176 0.5541 0.067 Uiso 1 1 calc R . . H58B H 0.4218 0.1929 0.5195 0.067 Uiso 1 1 calc R . . C59 C 0.2757(6) 0.1894(4) 0.5711(4) 0.0473(17) Uani 1 1 d . . . H59A H 0.2229 0.1798 0.5212 0.057 Uiso 1 1 calc R . . H59B H 0.2501 0.1613 0.6122 0.057 Uiso 1 1 calc R . . C60 C 0.2698(5) 0.2671(3) 0.5909(3) 0.0426(14) Uani 1 1 d . . . H60A H 0.2981 0.2932 0.5486 0.051 Uiso 1 1 calc R . . C61 C 0.0603(7) 0.2655(4) 0.5709(4) 0.049(2) Uani 1 1 d . . . H61A H 0.0639 0.2190 0.5533 0.059 Uiso 1 1 calc R . . C62 C -0.0558(7) 0.2967(5) 0.5666(4) 0.054(2) Uani 1 1 d . . . C63 C -0.0758(7) 0.3648(4) 0.5951(4) 0.0429(18) Uani 1 1 d . . . C64 C -0.1964(6) 0.3904(4) 0.5829(4) 0.0437(17) Uani 1 1 d . . . C65 C -0.2840(7) 0.3475(4) 0.5409(4) 0.0502(18) Uani 1 1 d . . . H65A H -0.3611 0.3641 0.5322 0.060 Uiso 1 1 calc R . . C66 C -0.2630(7) 0.2805(5) 0.5108(5) 0.061(2) Uani 1 1 d . . . C67 C -0.1480(7) 0.2552(4) 0.5261(5) 0.058(2) Uani 1 1 d . . . H67A H -0.1322 0.2099 0.5090 0.070 Uiso 1 1 calc R . . C68 C -0.2255(7) 0.4631(5) 0.6148(4) 0.057(2) Uani 1 1 d . . . C69 C -0.1667(8) 0.5238(4) 0.5748(6) 0.076(3) Uani 1 1 d . . . H69A H -0.1859 0.5687 0.5957 0.113 Uiso 1 1 calc R . . H69B H -0.1950 0.5227 0.5184 0.113 Uiso 1 1 calc R . . H69C H -0.0829 0.5174 0.5855 0.113 Uiso 1 1 calc R . . C70 C -0.3594(8) 0.4774(5) 0.5984(6) 0.089(3) Uani 1 1 d . . . H70A H -0.3744 0.5234 0.6187 0.134 Uiso 1 1 calc R . . H70B H -0.3983 0.4418 0.6242 0.134 Uiso 1 1 calc R . . H70C H -0.3888 0.4761 0.5422 0.134 Uiso 1 1 calc R . . C71 C -0.1855(8) 0.4675(5) 0.7043(5) 0.079(3) Uani 1 1 d . . . H71A H -0.2039 0.5136 0.7226 0.119 Uiso 1 1 calc R . . H71B H -0.1020 0.4599 0.7174 0.119 Uiso 1 1 calc R . . H71C H -0.2252 0.4318 0.7295 0.119 Uiso 1 1 calc R . . C72 C -0.3626(7) 0.2409(5) 0.4584(5) 0.063(2) Uani 1 1 d . . . C73 C -0.4501(9) 0.2774(6) 0.4096(6) 0.083(3) Uani 1 1 d . . . H73A H -0.4530 0.3268 0.4109 0.100 Uiso 1 1 calc R . . C74 C -0.5275(12) 0.1674(7) 0.3568(7) 0.105(4) Uani 1 1 d . . . H74A H -0.5845 0.1427 0.3217 0.126 Uiso 1 1 calc R . . C75 C -0.4413(11) 0.1299(7) 0.4045(8) 0.109(5) Uani 1 1 d . . . H75A H -0.4393 0.0806 0.4019 0.131 Uiso 1 1 calc R . . C76 C -0.3580(9) 0.1662(6) 0.4560(6) 0.085(3) Uani 1 1 d . . . H76A H -0.2986 0.1418 0.4894 0.102 Uiso 1 1 calc R . . N3 N 0.6659(6) 0.7940(3) 1.1110(4) 0.0477(16) Uani 1 1 d . . . N2 N 0.8552(5) 0.7200(3) 1.1719(3) 0.0437(15) Uani 1 1 d . . . N1 N 1.2073(6) 0.4511(4) 1.5319(4) 0.0537(17) Uani 1 1 d . . . N4 N 0.0713(13) 0.9645(7) 0.8991(8) 0.139(5) Uani 1 1 d . . . N6 N 0.3387(5) 0.3596(3) 0.6884(3) 0.0419(14) Uani 1 1 d . . . N7 N 0.1584(5) 0.2972(3) 0.5971(3) 0.0426(14) Uani 1 1 d . . . N5 N 0.7059(6) 0.6367(3) 1.0268(3) 0.0461(16) Uani 1 1 d . . . N8 N -0.5337(8) 0.2393(7) 0.3585(5) 0.111(3) Uani 1 1 d . . . O1 O 0.5110(4) 0.6798(3) 1.1223(3) 0.0565(13) Uani 1 1 d . . . O2 O 0.7136(5) 0.6101(3) 1.2154(3) 0.0554(15) Uani 1 1 d . . . O3 O 0.2074(5) 0.4828(3) 0.7120(3) 0.0589(15) Uani 1 1 d . . . O4 O 0.0062(4) 0.4059(3) 0.6311(3) 0.0516(12) Uani 1 1 d . . . O5 O 0.1248(15) 0.3031(7) 0.3603(6) 0.286(8) Uani 1 1 d . . . O6 O 0.6383(10) 0.8493(7) 0.8285(11) 0.333(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0287(5) 0.0381(5) 0.0319(4) 0.0004(4) -0.0032(4) -0.0048(4) Ni2 0.0275(5) 0.0381(5) 0.0317(4) -0.0021(4) -0.0033(4) 0.0034(4) C1 0.063(7) 0.091(8) 0.102(7) 0.035(6) 0.022(6) 0.026(5) C2 0.039(5) 0.097(7) 0.064(5) 0.008(5) 0.013(4) 0.016(4) C3 0.073(8) 0.116(8) 0.083(6) -0.002(6) -0.006(6) 0.040(6) C4 0.097(11) 0.175(15) 0.107(10) 0.001(11) -0.034(8) 0.056(11) C5 0.078(10) 0.35(3) 0.089(9) 0.043(15) -0.010(8) 0.087(17) C6 0.044(5) 0.073(5) 0.051(4) 0.002(4) 0.005(4) 0.012(4) C7 0.043(5) 0.069(5) 0.056(4) 0.000(4) 0.011(4) 0.012(4) C8 0.036(4) 0.043(4) 0.049(4) 0.006(3) 0.004(3) -0.001(3) C9 0.042(5) 0.065(5) 0.041(4) -0.001(3) 0.004(3) 0.013(4) C10 0.042(5) 0.068(5) 0.046(4) 0.002(4) 0.005(3) -0.002(4) C11 0.036(5) 0.111(7) 0.054(4) -0.008(5) 0.008(4) -0.004(5) C12 0.056(6) 0.044(5) 0.057(4) 0.009(4) 0.013(4) -0.006(4) C13 0.050(5) 0.081(6) 0.056(4) 0.007(4) 0.004(4) -0.018(4) C14 0.090(8) 0.159(11) 0.079(6) 0.052(7) 0.013(6) -0.022(7) C15 0.094(9) 0.089(7) 0.092(6) 0.015(6) 0.020(6) -0.021(6) C16 0.042(5) 0.124(8) 0.096(6) 0.017(6) 0.001(4) -0.021(5) C17 0.042(4) 0.046(3) 0.051(4) -0.002(3) 0.008(3) -0.008(3) C18 0.062(6) 0.046(4) 0.090(5) 0.011(5) 0.013(4) -0.005(5) C19 0.072(6) 0.055(4) 0.077(5) 0.004(4) 0.019(5) -0.019(4) C20 0.057(5) 0.075(5) 0.070(5) 0.002(4) 0.020(4) -0.021(4) C21 0.050(5) 0.052(5) 0.060(4) 0.001(4) 0.007(4) -0.019(4) C22 0.036(4) 0.053(4) 0.043(3) 0.000(3) 0.010(3) -0.005(3) C23 0.042(4) 0.051(4) 0.036(3) 0.002(3) -0.003(3) -0.002(3) C24 0.040(5) 0.054(5) 0.034(3) 0.000(4) -0.004(3) -0.004(4) C25 0.048(5) 0.049(4) 0.041(4) 0.003(3) 0.007(4) -0.006(4) C26 0.053(5) 0.044(4) 0.049(4) 0.003(3) 0.007(4) -0.001(4) C27 0.054(5) 0.043(4) 0.043(4) 0.012(3) 0.000(3) -0.002(3) C28 0.046(5) 0.066(5) 0.047(4) 0.017(4) -0.002(4) -0.010(4) C29 0.041(5) 0.078(6) 0.063(5) 0.023(5) 0.002(4) 0.006(4) C30 0.053(5) 0.045(4) 0.051(4) -0.001(3) 0.007(3) 0.001(3) C31 0.060(6) 0.093(7) 0.128(8) -0.012(6) 0.045(6) -0.010(5) C32 0.120(9) 0.136(9) 0.062(5) -0.029(5) -0.001(5) -0.074(7) C33 0.076(7) 0.055(5) 0.192(11) 0.034(7) -0.003(7) -0.032(5) C34 0.043(5) 0.058(5) 0.047(4) 0.014(4) 0.006(4) 0.010(4) C35 0.040(5) 0.064(5) 0.048(4) 0.013(4) 0.005(4) 0.008(4) C36 0.026(5) 0.110(8) 0.077(6) 0.038(6) 0.000(4) 0.003(5) C37 0.038(6) 0.156(11) 0.086(6) 0.058(7) 0.016(5) 0.015(6) C38 0.051(6) 0.107(8) 0.063(5) 0.038(5) 0.002(5) -0.006(5) C39 0.035(5) 0.054(4) 0.048(4) -0.009(4) -0.004(4) 0.004(4) C40 0.042(6) 0.085(6) 0.059(5) -0.023(5) -0.003(4) 0.013(5) C41 0.052(6) 0.127(9) 0.083(7) -0.064(6) 0.015(5) -0.020(6) C42 0.047(6) 0.127(9) 0.122(8) -0.081(8) 0.008(6) 0.010(6) C43 0.059(7) 0.073(6) 0.075(6) -0.028(5) -0.010(5) -0.002(5) C44 0.044(5) 0.058(5) 0.050(4) -0.015(4) 0.005(4) -0.012(4) C45 0.047(5) 0.056(4) 0.049(4) -0.002(3) 0.004(3) 0.000(4) C46 0.042(5) 0.042(4) 0.047(4) -0.001(3) 0.001(3) -0.001(3) C47 0.038(5) 0.055(5) 0.038(4) -0.007(3) -0.005(3) 0.000(4) C48 0.048(5) 0.051(5) 0.045(4) -0.016(4) 0.003(4) 0.001(4) C49 0.040(5) 0.051(5) 0.042(4) -0.005(3) -0.010(3) 0.015(4) C50 0.055(5) 0.047(4) 0.062(4) 0.010(3) 0.016(4) 0.012(3) C51 0.080(7) 0.071(5) 0.085(5) 0.011(4) 0.029(5) 0.022(5) C52 0.084(8) 0.052(5) 0.161(9) -0.005(5) -0.008(7) -0.003(4) C53 0.082(7) 0.106(7) 0.065(5) 0.014(5) -0.011(4) 0.022(6) C54 0.038(4) 0.049(4) 0.041(3) 0.003(3) 0.000(3) 0.005(3) C55 0.045(4) 0.034(3) 0.045(3) 0.004(3) 0.006(3) 0.003(3) C56 0.034(4) 0.057(5) 0.079(5) -0.017(4) -0.008(4) 0.005(3) C57 0.053(5) 0.065(4) 0.072(4) -0.017(4) -0.004(4) 0.012(4) C58 0.055(5) 0.054(4) 0.058(4) -0.005(3) 0.014(4) 0.008(3) C59 0.045(4) 0.047(4) 0.050(3) -0.011(3) 0.009(3) 0.005(4) C60 0.038(4) 0.050(4) 0.039(3) 0.002(3) 0.005(3) 0.002(3) C61 0.038(5) 0.050(5) 0.057(4) -0.006(4) 0.004(4) -0.015(4) C62 0.040(5) 0.067(6) 0.057(4) -0.002(4) 0.014(4) -0.005(4) C63 0.033(4) 0.048(4) 0.046(4) 0.001(3) 0.003(3) 0.006(3) C64 0.031(4) 0.056(5) 0.044(3) 0.003(3) 0.008(3) 0.001(3) C65 0.036(4) 0.056(4) 0.059(4) -0.004(3) 0.009(3) -0.004(3) C66 0.038(5) 0.070(5) 0.075(5) -0.008(4) 0.013(4) -0.005(4) C67 0.042(5) 0.057(5) 0.077(5) -0.022(4) 0.011(4) -0.008(4) C68 0.030(4) 0.069(5) 0.070(5) -0.020(4) 0.008(4) 0.008(4) C69 0.060(6) 0.049(5) 0.115(7) 0.012(5) 0.012(5) 0.007(4) C70 0.058(6) 0.077(6) 0.131(8) -0.011(5) 0.015(5) 0.032(5) C71 0.070(6) 0.094(6) 0.069(5) -0.036(5) 0.000(4) 0.023(5) C72 0.039(5) 0.082(6) 0.070(5) -0.015(4) 0.013(4) -0.022(4) C73 0.049(6) 0.108(7) 0.085(6) 0.006(5) -0.010(5) -0.022(5) C74 0.099(10) 0.134(11) 0.080(7) -0.037(7) 0.009(7) -0.070(9) C75 0.060(8) 0.113(9) 0.159(12) -0.074(9) 0.034(8) -0.054(7) C76 0.052(6) 0.098(8) 0.107(7) -0.019(6) 0.018(5) -0.030(5) N3 0.035(4) 0.052(4) 0.056(3) 0.000(3) 0.008(3) -0.004(3) N2 0.041(3) 0.049(3) 0.038(3) 0.006(2) 0.002(3) -0.008(3) N1 0.035(4) 0.067(5) 0.055(4) 0.008(3) -0.004(3) -0.002(3) N4 0.118(11) 0.166(11) 0.143(10) 0.038(9) 0.047(8) 0.064(9) N6 0.042(4) 0.040(3) 0.039(3) -0.005(2) -0.004(3) 0.002(2) N7 0.039(4) 0.046(3) 0.042(3) -0.009(3) 0.006(3) 0.003(3) N5 0.041(4) 0.045(4) 0.050(3) -0.014(3) 0.003(3) -0.006(3) N8 0.057(5) 0.158(9) 0.102(6) 0.019(7) -0.025(5) -0.052(6) O1 0.039(3) 0.065(3) 0.064(3) 0.017(3) 0.005(2) 0.011(3) O2 0.038(3) 0.070(4) 0.054(3) 0.021(3) -0.002(3) -0.005(3) O3 0.049(4) 0.051(3) 0.067(3) -0.015(3) -0.011(3) 0.012(3) O4 0.037(3) 0.053(3) 0.061(3) -0.011(3) -0.001(2) 0.014(3) O5 0.52(2) 0.208(11) 0.123(7) 0.019(7) 0.048(11) 0.039(14) O6 0.153(11) 0.270(15) 0.53(3) -0.171(16) -0.058(13) 0.104(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 1.966(5) . ? Ni1 O1 1.968(5) . ? Ni1 N2 2.079(6) . ? Ni1 N3 2.089(7) . ? Ni1 N5 2.112(5) . ? Ni2 O4 1.954(5) . ? Ni2 O3 1.965(5) . ? Ni2 N6 2.079(6) . ? Ni2 N7 2.100(6) . ? Ni2 N1 2.114(6) 1_454 ? C1 C2 1.353(13) . ? C1 N4 1.403(15) . ? C2 C3 1.371(14) . ? C2 C6 1.461(12) . ? C3 C4 1.207(16) . ? C4 C5 1.28(3) . ? C5 N4 1.45(2) . ? C6 C7 1.329(11) . ? C6 C11 1.404(12) . ? C7 C8 1.415(10) . ? C8 C9 1.436(10) . ? C8 C12 1.452(11) . ? C9 O1 1.299(9) . ? C9 C10 1.408(11) . ? C10 C11 1.381(11) . ? C10 C13 1.515(12) . ? C12 N3 1.271(10) . ? C13 C16 1.513(12) . ? C13 C14 1.517(11) . ? C13 C15 1.526(14) . ? C17 N3 1.482(8) . ? C17 C22 1.533(8) . ? C17 C18 1.543(10) . ? C18 C19 1.518(11) . ? C19 C20 1.499(10) . ? C20 C21 1.548(10) . ? C21 C22 1.530(9) . ? C22 N2 1.464(7) . ? C23 N2 1.283(8) . ? C23 C24 1.439(11) . ? C24 C29 1.395(10) . ? C24 C25 1.432(10) . ? C25 O2 1.282(10) . ? C25 C26 1.424(11) . ? C26 C27 1.386(11) . ? C26 C30 1.524(11) . ? C27 C28 1.378(11) . ? C28 C29 1.356(11) . ? C28 C34 1.482(11) . ? C30 C32 1.510(10) . ? C30 C31 1.515(11) . ? C30 C33 1.523(12) . ? C34 C35 1.390(9) . ? C34 C38 1.404(11) . ? C35 N1 1.341(9) . ? C36 N1 1.341(9) . ? C36 C37 1.366(11) . ? C37 C38 1.325(13) . ? C39 N5 1.318(9) . ? C39 C40 1.384(10) . ? C40 C41 1.339(12) . ? C40 C44 1.466(11) . ? C41 C42 1.389(13) . ? C42 C43 1.368(11) . ? C43 N5 1.331(10) . ? C44 C49 1.389(10) . ? C44 C45 1.445(11) . ? C45 C46 1.333(11) . ? C46 C47 1.426(11) . ? C46 C50 1.551(10) . ? C47 O3 1.319(9) . ? C47 C48 1.416(11) . ? C48 C49 1.416(10) . ? C48 C54 1.451(11) . ? C50 C51 1.518(10) . ? C50 C52 1.522(12) . ? C50 C53 1.547(10) . ? C54 N6 1.260(9) . ? C55 N6 1.478(7) . ? C55 C56 1.529(9) . ? C55 C60 1.531(8) . ? C56 C57 1.510(11) . ? C57 C58 1.493(9) . ? C58 C59 1.512(9) . ? C59 C60 1.506(10) . ? C60 N7 1.430(8) . ? C61 N7 1.286(9) . ? C61 C62 1.454(11) . ? C62 C67 1.397(11) . ? C62 C63 1.407(11) . ? C63 O4 1.289(9) . ? C63 C64 1.454(10) . ? C64 C65 1.388(10) . ? C64 C68 1.533(11) . ? C65 C66 1.399(11) . ? C66 C67 1.392(11) . ? C66 C72 1.517(11) . ? C68 C71 1.519(10) . ? C68 C70 1.546(11) . ? C68 C69 1.551(12) . ? C72 C73 1.371(13) . ? C72 C76 1.408(14) . ? C73 N8 1.378(12) . ? C74 N8 1.356(16) . ? C74 C75 1.363(17) . ? C75 C76 1.363(14) . ? N1 Ni2 2.114(6) 1_656 ? 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 Ni1 O1 94.6(2) . . ? O2 Ni1 N2 88.4(2) . . ? O1 Ni1 N2 160.0(2) . . ? O2 Ni1 N3 146.8(2) . . ? O1 Ni1 N3 88.3(2) . . ? N2 Ni1 N3 78.6(2) . . ? O2 Ni1 N5 105.7(2) . . ? O1 Ni1 N5 100.0(2) . . ? N2 Ni1 N5 98.1(2) . . ? N3 Ni1 N5 106.3(2) . . ? O4 Ni2 O3 94.1(2) . . ? O4 Ni2 N6 149.0(2) . . ? O3 Ni2 N6 89.2(2) . . ? O4 Ni2 N7 88.4(2) . . ? O3 Ni2 N7 159.2(2) . . ? N6 Ni2 N7 78.3(2) . . ? O4 Ni2 N1 105.5(2) . 1_454 ? O3 Ni2 N1 100.7(2) . 1_454 ? N6 Ni2 N1 104.2(2) . 1_454 ? N7 Ni2 N1 98.5(2) . 1_454 ? C2 C1 N4 123.1(13) . . ? C1 C2 C3 112.4(10) . . ? C1 C2 C6 123.6(10) . . ? C3 C2 C6 124.0(10) . . ? C4 C3 C2 129.7(15) . . ? C3 C4 C5 120(2) . . ? C4 C5 N4 121.1(17) . . ? C7 C6 C11 116.4(8) . . ? C7 C6 C2 122.4(9) . . ? C11 C6 C2 121.1(9) . . ? C6 C7 C8 123.0(8) . . ? C7 C8 C9 119.6(7) . . ? C7 C8 C12 116.7(7) . . ? C9 C8 C12 123.7(7) . . ? O1 C9 C10 120.5(8) . . ? O1 C9 C8 121.7(8) . . ? C10 C9 C8 117.7(7) . . ? C11 C10 C9 118.0(8) . . ? C11 C10 C13 120.9(8) . . ? C9 C10 C13 121.0(7) . . ? C10 C11 C6 125.1(8) . . ? N3 C12 C8 126.9(7) . . ? C16 C13 C10 113.8(8) . . ? C16 C13 C14 107.2(7) . . ? C10 C13 C14 109.8(8) . . ? C16 C13 C15 107.0(8) . . ? C10 C13 C15 109.7(7) . . ? C14 C13 C15 109.3(9) . . ? N3 C17 C22 107.6(5) . . ? N3 C17 C18 116.8(6) . . ? C22 C17 C18 111.1(5) . . ? C19 C18 C17 109.2(7) . . ? C20 C19 C18 113.2(7) . . ? C19 C20 C21 110.8(6) . . ? C22 C21 C20 108.0(6) . . ? N2 C22 C21 116.6(5) . . ? N2 C22 C17 107.2(5) . . ? C21 C22 C17 112.1(5) . . ? N2 C23 C24 125.7(7) . . ? C29 C24 C25 120.2(7) . . ? C29 C24 C23 115.8(7) . . ? C25 C24 C23 124.0(7) . . ? O2 C25 C26 120.3(8) . . ? O2 C25 C24 122.5(7) . . ? C26 C25 C24 117.2(8) . . ? C27 C26 C25 118.4(8) . . ? C27 C26 C30 120.6(7) . . ? C25 C26 C30 121.0(7) . . ? C28 C27 C26 123.9(7) . . ? C29 C28 C27 117.9(8) . . ? C29 C28 C34 121.6(8) . . ? C27 C28 C34 120.4(7) . . ? C28 C29 C24 121.9(8) . . ? C32 C30 C31 112.2(8) . . ? C32 C30 C33 103.3(9) . . ? C31 C30 C33 106.0(7) . . ? C32 C30 C26 111.2(6) . . ? C31 C30 C26 110.7(7) . . ? C33 C30 C26 113.1(7) . . ? C35 C34 C38 115.5(7) . . ? C35 C34 C28 120.0(7) . . ? C38 C34 C28 124.5(7) . . ? N1 C35 C34 123.6(7) . . ? N1 C36 C37 122.6(8) . . ? C38 C37 C36 119.2(9) . . ? C37 C38 C34 121.1(8) . . ? N5 C39 C40 124.5(7) . . ? C41 C40 C39 117.9(8) . . ? C41 C40 C44 120.9(8) . . ? C39 C40 C44 121.0(8) . . ? C40 C41 C42 118.5(8) . . ? C43 C42 C41 119.7(9) . . ? N5 C43 C42 121.8(9) . . ? C49 C44 C45 115.6(7) . . ? C49 C44 C40 121.2(8) . . ? C45 C44 C40 123.1(8) . . ? C46 C45 C44 124.9(8) . . ? C45 C46 C47 118.3(8) . . ? C45 C46 C50 120.0(7) . . ? C47 C46 C50 121.7(7) . . ? O3 C47 C48 120.4(7) . . ? O3 C47 C46 119.3(7) . . ? C48 C47 C46 120.2(7) . . ? C47 C48 C49 118.7(7) . . ? C47 C48 C54 125.8(7) . . ? C49 C48 C54 115.5(7) . . ? C44 C49 C48 122.2(7) . . ? C51 C50 C52 108.1(7) . . ? C51 C50 C53 106.9(8) . . ? C52 C50 C53 110.2(8) . . ? C51 C50 C46 109.0(6) . . ? C52 C50 C46 111.1(8) . . ? C53 C50 C46 111.4(6) . . ? N6 C54 C48 126.1(7) . . ? N6 C55 C56 116.1(5) . . ? N6 C55 C60 108.4(5) . . ? C56 C55 C60 110.1(5) . . ? C57 C56 C55 112.0(6) . . ? C58 C57 C56 112.0(6) . . ? C57 C58 C59 112.2(5) . . ? C60 C59 C58 110.8(6) . . ? N7 C60 C59 118.7(6) . . ? N7 C60 C55 107.2(5) . . ? C59 C60 C55 110.6(5) . . ? N7 C61 C62 125.3(8) . . ? C67 C62 C63 121.5(8) . . ? C67 C62 C61 114.4(8) . . ? C63 C62 C61 124.0(8) . . ? O4 C63 C62 124.0(7) . . ? O4 C63 C64 118.1(6) . . ? C62 C63 C64 117.9(7) . . ? C65 C64 C63 118.0(7) . . ? C65 C64 C68 121.2(7) . . ? C63 C64 C68 120.8(7) . . ? C64 C65 C66 123.8(8) . . ? C67 C66 C65 117.7(8) . . ? C67 C66 C72 122.5(8) . . ? C65 C66 C72 119.7(8) . . ? C66 C67 C62 121.1(8) . . ? C71 C68 C64 111.2(7) . . ? C71 C68 C70 106.3(6) . . ? C64 C68 C70 111.7(7) . . ? C71 C68 C69 109.2(8) . . ? C64 C68 C69 110.9(6) . . ? C70 C68 C69 107.3(7) . . ? C73 C72 C76 120.6(10) . . ? C73 C72 C66 120.5(9) . . ? C76 C72 C66 118.7(10) . . ? C72 C73 N8 118.6(10) . . ? N8 C74 C75 122.7(11) . . ? C76 C75 C74 118.6(13) . . ? C75 C76 C72 119.6(12) . . ? C12 N3 C17 120.6(7) . . ? C12 N3 Ni1 124.1(6) . . ? C17 N3 Ni1 115.2(5) . . ? C23 N2 C22 122.6(6) . . ? C23 N2 Ni1 125.9(5) . . ? C22 N2 Ni1 111.5(4) . . ? C36 N1 C35 117.3(7) . . ? C36 N1 Ni2 124.2(6) . 1_656 ? C35 N1 Ni2 118.4(5) . 1_656 ? C1 N4 C5 113.3(14) . . ? C54 N6 C55 120.2(6) . . ? C54 N6 Ni2 124.8(5) . . ? C55 N6 Ni2 114.8(4) . . ? C61 N7 C60 122.7(6) . . ? C61 N7 Ni2 125.5(6) . . ? C60 N7 Ni2 111.2(4) . . ? C39 N5 C43 117.2(6) . . ? C39 N5 Ni1 121.6(5) . . ? C43 N5 Ni1 121.2(6) . . ? C74 N8 C73 119.9(11) . . ? C9 O1 Ni1 130.4(5) . . ? C25 O2 Ni1 131.2(5) . . ? C47 O3 Ni2 129.6(5) . . ? C63 O4 Ni2 130.7(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.463 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.060 # Attachment 'CIF of 1.cif' data_1 #TrackingRef 'CIF of 1.cif' _database_code_depnum_ccdc_archive 'CCDC 761766' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H42 N4 O2 Zn' _chemical_formula_weight 652.13 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.7901(11) _cell_length_b 10.4305(12) _cell_length_c 32.683(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.7400(10) _cell_angle_gamma 90.00 _cell_volume 3307.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 20890 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 27.52 _exptl_crystal_description block-like _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.782 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.910 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20890 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0671 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.52 _reflns_number_total 11116 _reflns_number_gt 7761 _reflns_threshold_expression >2sigma(I) _chemical_absolute_configuration ad _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _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 _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^)+(0.0393P)^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 geom _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 0.009(12) _refine_ls_number_reflns 11116 _refine_ls_number_parameters 811 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _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 Zn1 Zn 0.09791(6) 0.16081(5) 0.635535(13) 0.03969(17) Uani 1 1 d . . . Zn2 Zn 0.39808(5) 0.85358(4) 0.867672(12) 0.03484(15) Uani 1 1 d . . . C1 C 0.1022(6) -0.1279(7) 0.34978(13) 0.0514(15) Uani 1 1 d . . . H1A H 0.0882 -0.1587 0.3228 0.062 Uiso 1 1 calc R . . C2 C 0.1961(6) -0.0353(6) 0.35986(14) 0.0630(18) Uani 1 1 d . . . H2A H 0.2463 -0.0029 0.3400 0.076 Uiso 1 1 calc R . . C3 C 0.2181(6) 0.0113(6) 0.39924(14) 0.0580(17) Uani 1 1 d . . . H3A H 0.2859 0.0730 0.4061 0.070 Uiso 1 1 calc R . . C4 C 0.1418(5) -0.0311(6) 0.42882(12) 0.0390(13) Uani 1 1 d . . . C5 C 0.0476(5) -0.1274(7) 0.41617(12) 0.0486(15) Uani 1 1 d . . . H5A H -0.0054 -0.1598 0.4354 0.058 Uiso 1 1 calc R . . C6 C 0.1567(5) 0.0211(5) 0.47140(12) 0.0388(13) Uani 1 1 d . . . C7 C 0.2645(5) 0.1051(6) 0.48564(12) 0.0444(15) Uani 1 1 d . . . H7A H 0.3273 0.1251 0.4676 0.053 Uiso 1 1 calc R . . C8 C 0.2844(4) 0.1604(6) 0.52442(11) 0.0383(12) Uani 1 1 d . . . C9 C 0.1903(5) 0.1278(6) 0.55293(12) 0.0387(14) Uani 1 1 d . . . C10 C 0.0814(5) 0.0397(6) 0.53921(12) 0.0421(14) Uani 1 1 d . . . C11 C 0.0674(5) -0.0103(6) 0.49872(13) 0.0458(14) Uani 1 1 d . . . H11A H -0.0047 -0.0664 0.4903 0.055 Uiso 1 1 calc R . . C12 C 0.4076(5) 0.2477(6) 0.53811(14) 0.0479(16) Uani 1 1 d . . . C13 C 0.4970(7) 0.2682(8) 0.50384(18) 0.086(3) Uani 1 1 d . . . H13A H 0.5310 0.1870 0.4957 0.128 Uiso 1 1 calc R . . H13B H 0.5732 0.3229 0.5137 0.128 Uiso 1 1 calc R . . H13C H 0.4429 0.3076 0.4805 0.128 Uiso 1 1 calc R . . C14 C 0.3581(6) 0.3812(6) 0.54974(18) 0.075(2) Uani 1 1 d . . . H14A H 0.3029 0.3731 0.5718 0.113 Uiso 1 1 calc R . . H14B H 0.3041 0.4193 0.5262 0.113 Uiso 1 1 calc R . . H14C H 0.4365 0.4346 0.5586 0.113 Uiso 1 1 calc R . . C15 C 0.4983(5) 0.1877(9) 0.57521(15) 0.081(2) Uani 1 1 d . . . H15A H 0.4448 0.1763 0.5975 0.121 Uiso 1 1 calc R . . H15B H 0.5748 0.2433 0.5839 0.121 Uiso 1 1 calc R . . H15C H 0.5319 0.1061 0.5674 0.121 Uiso 1 1 calc R . . C16 C -0.0106(5) -0.0155(5) 0.56575(12) 0.0443(14) Uani 1 1 d . . . H16A H -0.0710 -0.0787 0.5542 0.053 Uiso 1 1 calc R . . C17 C -0.1010(4) -0.0607(4) 0.62878(12) 0.0376(10) Uani 1 1 d . . . H17A H -0.0433 -0.1308 0.6413 0.045 Uiso 1 1 calc R . . C18 C -0.2321(5) -0.1210(6) 0.60591(13) 0.0504(14) Uani 1 1 d . . . H18A H -0.2896 -0.0545 0.5918 0.061 Uiso 1 1 calc R . . H18B H -0.2077 -0.1806 0.5853 0.061 Uiso 1 1 calc R . . C19 C -0.3127(5) -0.1916(6) 0.63594(14) 0.0595(15) Uani 1 1 d . . . H19A H -0.3982 -0.2236 0.6210 0.071 Uiso 1 1 calc R . . H19B H -0.2593 -0.2648 0.6473 0.071 Uiso 1 1 calc R . . C20 C -0.3450(5) -0.1073(5) 0.67086(14) 0.0583(14) Uani 1 1 d . . . H20A H -0.3910 -0.1575 0.6899 0.070 Uiso 1 1 calc R . . H20B H -0.4068 -0.0391 0.6600 0.070 Uiso 1 1 calc R . . C21 C -0.2125(5) -0.0491(6) 0.69383(13) 0.0465(13) Uani 1 1 d . . . H21A H -0.2353 0.0073 0.7155 0.056 Uiso 1 1 calc R . . H21B H -0.1537 -0.1169 0.7065 0.056 Uiso 1 1 calc R . . C22 C -0.1369(4) 0.0256(4) 0.66434(11) 0.0375(10) Uani 1 1 d . . . H22A H -0.1994 0.0926 0.6520 0.045 Uiso 1 1 calc R . . C23 C 0.0318(5) 0.0938(5) 0.72090(12) 0.0412(13) Uani 1 1 d . . . H23A H -0.0211 0.0513 0.7382 0.049 Uiso 1 1 calc R . . C24 C 0.1530(5) 0.1608(6) 0.73985(12) 0.0381(12) Uani 1 1 d . . . C25 C 0.1648(5) 0.1753(6) 0.78323(11) 0.0397(13) Uani 1 1 d . . . H25A H 0.0988 0.1372 0.7972 0.048 Uiso 1 1 calc R . . C26 C 0.2690(5) 0.2426(5) 0.80536(12) 0.0375(13) Uani 1 1 d . . . C27 C 0.3656(5) 0.3013(6) 0.78270(12) 0.0418(13) Uani 1 1 d . . . H27A H 0.4356 0.3505 0.7970 0.050 Uiso 1 1 calc R . . C28 C 0.3613(5) 0.2892(6) 0.74036(12) 0.0382(13) Uani 1 1 d . . . C29 C 0.2521(5) 0.2172(6) 0.71771(12) 0.0403(14) Uani 1 1 d . . . C30 C 0.4682(5) 0.3557(7) 0.71708(12) 0.0436(13) Uani 1 1 d . . . C31 C 0.5487(5) 0.2526(6) 0.69603(14) 0.0576(18) Uani 1 1 d . . . H31A H 0.5909 0.1936 0.7165 0.086 Uiso 1 1 calc R . . H31B H 0.6186 0.2933 0.6826 0.086 Uiso 1 1 calc R . . H31C H 0.4863 0.2070 0.6759 0.086 Uiso 1 1 calc R . . C32 C 0.3974(6) 0.4477(6) 0.68440(15) 0.0656(18) Uani 1 1 d . . . H32A H 0.3473 0.5114 0.6975 0.098 Uiso 1 1 calc R . . H32B H 0.3349 0.4006 0.6648 0.098 Uiso 1 1 calc R . . H32C H 0.4657 0.4888 0.6704 0.098 Uiso 1 1 calc R . . C33 C 0.5737(6) 0.4350(7) 0.74542(15) 0.082(2) Uani 1 1 d . . . H33A H 0.6208 0.3806 0.7665 0.123 Uiso 1 1 calc R . . H33B H 0.5271 0.5022 0.7581 0.123 Uiso 1 1 calc R . . H33C H 0.6393 0.4718 0.7295 0.123 Uiso 1 1 calc R . . C34 C 0.2772(5) 0.2594(5) 0.85118(12) 0.0348(12) Uani 1 1 d . . . C35 C 0.2265(4) 0.1675(6) 0.87545(12) 0.0400(12) Uani 1 1 d . . . H35A H 0.1893 0.0917 0.8638 0.048 Uiso 1 1 calc R . . C36 C 0.2320(5) 0.1899(6) 0.91732(13) 0.0507(15) Uani 1 1 d . . . H36A H 0.1954 0.1308 0.9342 0.061 Uiso 1 1 calc R . . C37 C 0.2912(6) 0.2989(7) 0.93340(14) 0.0624(18) Uani 1 1 d . . . H37A H 0.2953 0.3114 0.9617 0.075 Uiso 1 1 calc R . . C38 C 0.3358(5) 0.3656(7) 0.87094(12) 0.0510(15) Uani 1 1 d . . . H38A H 0.3731 0.4264 0.8548 0.061 Uiso 1 1 calc R . . C39 C 0.2300(7) 0.7257(8) 0.57023(16) 0.076(2) Uani 1 1 d . . . H39A H 0.2296 0.7125 0.5421 0.091 Uiso 1 1 calc R . . C40 C 0.2976(5) 0.8315(7) 0.58786(14) 0.0570(17) Uani 1 1 d . . . H40A H 0.3458 0.8859 0.5724 0.068 Uiso 1 1 calc R . . C41 C 0.2923(5) 0.8546(8) 0.62898(12) 0.0542(15) Uani 1 1 d . . . H41A H 0.3331 0.9283 0.6411 0.065 Uiso 1 1 calc R . . C42 C 0.2274(5) 0.7704(6) 0.65257(13) 0.0395(14) Uani 1 1 d . . . C43 C 0.1647(5) 0.6627(8) 0.63189(13) 0.0555(16) Uani 1 1 d . . . H43A H 0.1212 0.6037 0.6471 0.067 Uiso 1 1 calc R . . C44 C 0.2274(5) 0.7861(6) 0.69801(12) 0.0361(13) Uani 1 1 d . . . C45 C 0.3235(4) 0.8623(6) 0.72100(11) 0.0385(12) Uani 1 1 d . . . H45A H 0.3835 0.9102 0.7073 0.046 Uiso 1 1 calc R . . C46 C 0.3351(5) 0.8707(6) 0.76409(11) 0.0367(12) Uani 1 1 d . . . C47 C 0.2391(4) 0.8056(5) 0.78573(12) 0.0341(12) Uani 1 1 d . . . C48 C 0.1323(5) 0.7311(6) 0.76167(13) 0.0374(13) Uani 1 1 d . . . C49 C 0.1326(5) 0.7247(6) 0.71949(13) 0.0386(13) Uani 1 1 d . . . H49A H 0.0643 0.6758 0.7043 0.046 Uiso 1 1 calc R . . C50 C 0.0211(5) 0.6675(7) 0.78387(12) 0.0466(14) Uani 1 1 d . . . C51 C -0.0812(6) 0.5917(7) 0.75327(14) 0.072(2) Uani 1 1 d . . . H51A H -0.1491 0.5522 0.7678 0.108 Uiso 1 1 calc R . . H51B H -0.0326 0.5267 0.7403 0.108 Uiso 1 1 calc R . . H51C H -0.1259 0.6488 0.7326 0.108 Uiso 1 1 calc R . . C52 C 0.0897(6) 0.5709(7) 0.81598(15) 0.0664(19) Uani 1 1 d . . . H52A H 0.0203 0.5305 0.8297 0.100 Uiso 1 1 calc R . . H52B H 0.1538 0.6151 0.8359 0.100 Uiso 1 1 calc R . . H52C H 0.1378 0.5070 0.8023 0.100 Uiso 1 1 calc R . . C53 C -0.0558(5) 0.7695(6) 0.80409(14) 0.0617(19) Uani 1 1 d . . . H53A H -0.1254 0.7301 0.8180 0.093 Uiso 1 1 calc R . . H53B H -0.0985 0.8276 0.7834 0.093 Uiso 1 1 calc R . . H53C H 0.0074 0.8158 0.8237 0.093 Uiso 1 1 calc R . . C54 C 0.4406(4) 0.9539(5) 0.78430(12) 0.0381(12) Uani 1 1 d . . . H54A H 0.4831 1.0083 0.7673 0.046 Uiso 1 1 calc R . . C55 C 0.5833(4) 1.0592(4) 0.83940(11) 0.0325(9) Uani 1 1 d . . . H55A H 0.5320 1.1381 0.8430 0.039 Uiso 1 1 calc R . . C56 C 0.6496(4) 1.0150(4) 0.88295(11) 0.0364(10) Uani 1 1 d . . . H56A H 0.7068 0.9400 0.8791 0.044 Uiso 1 1 calc R . . C57 C 0.7443(5) 1.1174(6) 0.90353(13) 0.0434(14) Uani 1 1 d . . . H57A H 0.7881 1.0864 0.9301 0.052 Uiso 1 1 calc R . . H57B H 0.6907 1.1929 0.9083 0.052 Uiso 1 1 calc R . . C58 C 0.8544(4) 1.1535(5) 0.87687(12) 0.0509(13) Uani 1 1 d . . . H58A H 0.9145 1.0805 0.8748 0.061 Uiso 1 1 calc R . . H58B H 0.9098 1.2230 0.8899 0.061 Uiso 1 1 calc R . . C59 C 0.7908(4) 1.1946(5) 0.83371(12) 0.0485(12) Uani 1 1 d . . . H59A H 0.7397 1.2735 0.8356 0.058 Uiso 1 1 calc R . . H59B H 0.8637 1.2112 0.8170 0.058 Uiso 1 1 calc R . . C60 C 0.6949(5) 1.0922(5) 0.81291(12) 0.0453(13) Uani 1 1 d . . . H60A H 0.7476 1.0158 0.8085 0.054 Uiso 1 1 calc R . . H60B H 0.6525 1.1230 0.7862 0.054 Uiso 1 1 calc R . . C61 C 0.5314(4) 0.9968(5) 0.94271(12) 0.0388(12) Uani 1 1 d . . . H61A H 0.6039 1.0452 0.9561 0.047 Uiso 1 1 calc R . . C62 C 0.4259(4) 0.9594(5) 0.96710(12) 0.0346(12) Uani 1 1 d . . . C63 C 0.4379(5) 1.0071(5) 1.00697(12) 0.0386(12) Uani 1 1 d . . . H63A H 0.5152 1.0558 1.0166 0.046 Uiso 1 1 calc R . . C64 C 0.3409(5) 0.9859(5) 1.03309(12) 0.0358(12) Uani 1 1 d . . . C65 C 0.2273(5) 0.9087(5) 1.01770(12) 0.0356(13) Uani 1 1 d . . . H65A H 0.1610 0.8927 1.0349 0.043 Uiso 1 1 calc R . . C66 C 0.2086(4) 0.8559(6) 0.97911(11) 0.0331(10) Uani 1 1 d . . . C67 C 0.3109(5) 0.8812(5) 0.95169(11) 0.0331(12) Uani 1 1 d . . . C68 C 0.0823(5) 0.7699(6) 0.96412(13) 0.0384(13) Uani 1 1 d . . . C69 C 0.1304(6) 0.6373(6) 0.95332(15) 0.0604(17) Uani 1 1 d . . . H69A H 0.1820 0.5992 0.9773 0.091 Uiso 1 1 calc R . . H69B H 0.1878 0.6442 0.9318 0.091 Uiso 1 1 calc R . . H69C H 0.0518 0.5848 0.9440 0.091 Uiso 1 1 calc R . . C70 C -0.0011(5) 0.8318(7) 0.92594(13) 0.0625(19) Uani 1 1 d . . . H70A H -0.0311 0.9156 0.9330 0.094 Uiso 1 1 calc R . . H70B H -0.0800 0.7796 0.9167 0.094 Uiso 1 1 calc R . . H70C H 0.0557 0.8388 0.9043 0.094 Uiso 1 1 calc R . . C71 C -0.0140(6) 0.7561(6) 0.99721(15) 0.0572(17) Uani 1 1 d . . . H71A H 0.0344 0.7149 1.0212 0.086 Uiso 1 1 calc R . . H71B H -0.0925 0.7053 0.9865 0.086 Uiso 1 1 calc R . . H71C H -0.0442 0.8394 1.0047 0.086 Uiso 1 1 calc R . . C72 C 0.3565(5) 1.0408(5) 1.07547(13) 0.0349(12) Uani 1 1 d . . . C73 C 0.2849(5) 0.9954(6) 1.10604(12) 0.0423(13) Uani 1 1 d . . . H73A H 0.2212 0.9296 1.1002 0.051 Uiso 1 1 calc R . . C74 C 0.3077(6) 1.0483(6) 1.14590(13) 0.0508(15) Uani 1 1 d . . . H74A H 0.2587 1.0194 1.1666 0.061 Uiso 1 1 calc R . . C75 C 0.4048(5) 1.1440(6) 1.15358(12) 0.0433(14) Uani 1 1 d . . . H75A H 0.4228 1.1771 1.1802 0.052 Uiso 1 1 calc R . . C76 C 0.4485(5) 1.1391(6) 1.08696(12) 0.0404(13) Uani 1 1 d . . . H76A H 0.4971 1.1720 1.0668 0.048 Uiso 1 1 calc R . . N1 N -0.0084(4) 0.0886(4) 0.68201(10) 0.0376(10) Uani 1 1 d . . . N2 N -0.0168(4) 0.0146(4) 0.60382(10) 0.0399(11) Uani 1 1 d . . . N3 N 0.0282(4) -0.1768(4) 0.37778(10) 0.0434(12) Uani 1 1 d . . . N4 N 0.3442(5) 0.3897(6) 0.91160(12) 0.0612(15) Uani 1 1 d . . . N5 N 0.4822(4) 0.9612(4) 0.82306(9) 0.0357(9) Uani 1 1 d . . . N6 N 0.5362(4) 0.9707(4) 0.90490(10) 0.0354(10) Uani 1 1 d . . . N7 N 0.1643(5) 0.6403(7) 0.59137(13) 0.0802(19) Uani 1 1 d . . . N8 N 0.4734(4) 1.1908(4) 1.12477(10) 0.0385(11) Uani 1 1 d . . . O1 O 0.2061(3) 0.1763(5) 0.58933(8) 0.0508(11) Uani 1 1 d . . . O2 O 0.2512(3) 0.2010(4) 0.67826(8) 0.0506(11) Uani 1 1 d . . . O3 O 0.2435(3) 0.8114(4) 0.82578(8) 0.0478(11) Uani 1 1 d . . . O4 O 0.2930(3) 0.8349(4) 0.91452(8) 0.0418(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0446(4) 0.0494(4) 0.0250(2) -0.0009(3) 0.0044(2) -0.0042(3) Zn2 0.0398(3) 0.0410(4) 0.0240(2) 0.0015(3) 0.0053(2) -0.0035(3) C1 0.077(4) 0.049(4) 0.031(2) -0.001(3) 0.018(2) -0.010(4) C2 0.097(5) 0.060(4) 0.040(3) -0.006(3) 0.036(3) -0.025(4) C3 0.080(4) 0.052(4) 0.046(3) -0.012(3) 0.024(3) -0.017(3) C4 0.047(3) 0.042(4) 0.029(2) 0.002(2) 0.010(2) 0.000(3) C5 0.057(3) 0.061(4) 0.032(2) -0.005(3) 0.016(2) -0.009(4) C6 0.047(3) 0.042(4) 0.028(2) -0.008(2) 0.007(2) -0.005(3) C7 0.046(3) 0.059(4) 0.029(2) 0.001(2) 0.009(2) 0.001(3) C8 0.039(3) 0.047(3) 0.0297(19) 0.003(3) 0.0061(19) -0.003(3) C9 0.040(3) 0.047(4) 0.028(2) -0.001(2) 0.002(2) -0.001(3) C10 0.045(3) 0.058(4) 0.024(2) -0.008(2) 0.006(2) -0.006(3) C11 0.046(3) 0.056(4) 0.036(2) -0.007(3) 0.009(2) -0.004(3) C12 0.046(3) 0.063(5) 0.036(2) -0.002(3) 0.010(2) -0.012(3) C13 0.074(4) 0.124(7) 0.066(3) -0.032(4) 0.034(3) -0.052(4) C14 0.080(5) 0.050(5) 0.098(5) -0.024(4) 0.019(4) -0.017(4) C15 0.051(4) 0.119(8) 0.068(4) 0.005(5) -0.012(3) -0.005(5) C16 0.043(3) 0.058(4) 0.032(2) -0.007(2) 0.007(2) -0.008(3) C17 0.032(2) 0.046(3) 0.036(2) -0.001(2) 0.0084(18) -0.003(2) C18 0.051(3) 0.055(4) 0.045(2) -0.011(3) 0.005(2) -0.008(3) C19 0.050(3) 0.067(4) 0.064(3) -0.016(3) 0.019(3) -0.020(3) C20 0.045(3) 0.070(4) 0.065(3) -0.018(3) 0.025(2) -0.012(3) C21 0.041(3) 0.060(4) 0.041(2) -0.005(2) 0.014(2) -0.009(3) C22 0.033(2) 0.046(3) 0.033(2) 0.003(2) 0.0059(18) 0.005(2) C23 0.042(3) 0.052(3) 0.031(2) 0.004(2) 0.011(2) -0.003(2) C24 0.036(3) 0.047(3) 0.032(2) 0.002(3) 0.0054(19) -0.003(3) C25 0.035(3) 0.054(4) 0.031(2) 0.003(2) 0.0077(19) 0.006(3) C26 0.041(3) 0.043(3) 0.029(2) 0.000(2) 0.006(2) 0.004(3) C27 0.039(3) 0.053(4) 0.031(2) -0.001(3) -0.001(2) -0.002(3) C28 0.038(3) 0.046(4) 0.030(2) 0.005(2) 0.005(2) 0.003(3) C29 0.043(3) 0.049(4) 0.027(2) -0.003(2) 0.001(2) 0.001(3) C30 0.051(3) 0.049(3) 0.031(2) -0.005(3) 0.007(2) -0.013(3) C31 0.050(3) 0.081(5) 0.043(3) 0.006(3) 0.010(2) -0.003(3) C32 0.078(4) 0.058(5) 0.062(3) 0.017(3) 0.014(3) -0.002(4) C33 0.081(5) 0.119(7) 0.046(3) 0.002(4) 0.010(3) -0.047(5) C34 0.033(3) 0.044(3) 0.028(2) 0.000(2) 0.006(2) 0.001(2) C35 0.036(2) 0.045(3) 0.039(2) 0.003(3) 0.0037(19) 0.003(3) C36 0.046(3) 0.072(5) 0.034(2) 0.006(3) 0.007(2) 0.000(3) C37 0.066(4) 0.091(5) 0.030(2) -0.003(3) 0.008(2) -0.011(4) C38 0.050(3) 0.068(4) 0.035(2) -0.009(3) 0.008(2) -0.008(4) C39 0.089(5) 0.106(7) 0.036(3) -0.008(4) 0.019(3) 0.022(5) C40 0.055(3) 0.083(5) 0.037(2) 0.012(3) 0.019(2) 0.005(3) C41 0.047(3) 0.081(4) 0.035(2) -0.003(3) 0.006(2) 0.001(4) C42 0.030(3) 0.058(4) 0.029(2) -0.004(2) -0.003(2) 0.005(3) C43 0.060(4) 0.072(5) 0.037(2) -0.007(3) 0.012(2) -0.009(4) C44 0.030(3) 0.051(4) 0.027(2) -0.002(2) 0.002(2) 0.002(3) C45 0.039(3) 0.046(3) 0.032(2) 0.002(2) 0.0108(19) -0.007(3) C46 0.037(2) 0.044(3) 0.0276(19) -0.002(2) 0.0002(18) -0.002(3) C47 0.031(3) 0.040(3) 0.031(2) 0.009(2) 0.0046(19) 0.001(2) C48 0.036(3) 0.044(4) 0.032(2) -0.001(2) 0.004(2) -0.001(3) C49 0.037(3) 0.044(4) 0.034(2) -0.005(2) 0.003(2) -0.003(3) C50 0.035(3) 0.069(4) 0.035(2) 0.014(3) 0.001(2) -0.011(3) C51 0.068(4) 0.100(6) 0.049(3) -0.009(3) 0.013(3) -0.049(4) C52 0.075(4) 0.068(5) 0.056(3) 0.020(3) 0.008(3) -0.012(4) C53 0.049(3) 0.092(6) 0.049(3) 0.009(3) 0.021(3) 0.003(4) C54 0.042(3) 0.044(3) 0.030(2) 0.007(2) 0.0110(19) -0.002(2) C55 0.031(2) 0.033(3) 0.035(2) 0.0024(19) 0.0099(18) -0.0005(19) C56 0.032(2) 0.043(3) 0.036(2) -0.002(2) 0.0097(18) 0.003(2) C57 0.035(3) 0.058(4) 0.037(2) -0.003(2) 0.0074(19) -0.010(2) C58 0.041(3) 0.063(4) 0.050(2) 0.001(3) 0.011(2) -0.009(3) C59 0.049(3) 0.054(4) 0.046(2) 0.003(2) 0.017(2) -0.012(2) C60 0.053(3) 0.048(3) 0.035(2) 0.004(2) 0.009(2) -0.012(3) C61 0.034(2) 0.048(3) 0.034(2) -0.003(2) 0.0021(19) -0.007(2) C62 0.033(2) 0.043(3) 0.030(2) 0.002(2) 0.0104(18) 0.005(2) C63 0.036(3) 0.049(3) 0.030(2) -0.005(2) 0.0019(19) -0.011(2) C64 0.040(3) 0.040(3) 0.028(2) 0.002(2) 0.006(2) 0.006(3) C65 0.037(3) 0.039(3) 0.033(2) 0.000(2) 0.012(2) -0.006(2) C66 0.034(2) 0.036(3) 0.0309(19) 0.000(3) 0.0086(18) 0.006(3) C67 0.035(3) 0.037(4) 0.0264(19) -0.002(2) 0.0024(18) 0.001(2) C68 0.040(3) 0.042(4) 0.034(2) -0.004(2) 0.007(2) -0.009(3) C69 0.060(4) 0.059(5) 0.062(3) -0.003(3) 0.010(3) -0.016(3) C70 0.052(3) 0.079(6) 0.053(3) 0.011(4) -0.007(2) -0.020(4) C71 0.050(3) 0.072(5) 0.051(3) -0.006(3) 0.015(2) -0.022(3) C72 0.038(3) 0.035(3) 0.032(2) -0.004(2) 0.005(2) 0.002(3) C73 0.056(3) 0.039(3) 0.033(2) -0.003(2) 0.013(2) -0.007(3) C74 0.080(4) 0.045(4) 0.032(2) -0.004(2) 0.023(2) -0.007(3) C75 0.062(4) 0.043(4) 0.026(2) -0.007(3) 0.011(2) 0.001(3) C76 0.051(3) 0.046(4) 0.027(2) 0.003(2) 0.014(2) 0.000(3) N1 0.037(2) 0.048(3) 0.0280(17) -0.0003(17) 0.0026(15) -0.0061(19) N2 0.040(2) 0.050(3) 0.0313(18) -0.0020(18) 0.0094(16) -0.0026(19) N3 0.053(3) 0.047(4) 0.0311(18) -0.005(2) 0.0109(18) -0.005(2) N4 0.069(3) 0.077(4) 0.038(2) -0.011(2) 0.009(2) -0.014(3) N5 0.040(2) 0.037(2) 0.0302(17) 0.0002(17) 0.0030(15) -0.0048(18) N6 0.035(2) 0.044(3) 0.0275(17) -0.0024(17) 0.0079(15) -0.0034(18) N7 0.093(4) 0.107(6) 0.043(2) -0.021(3) 0.016(3) -0.007(4) N8 0.051(3) 0.039(3) 0.0269(17) -0.0004(19) 0.0106(17) 0.004(2) O1 0.055(2) 0.070(3) 0.0286(15) -0.0126(19) 0.0106(14) -0.015(2) O2 0.049(2) 0.077(3) 0.0254(15) -0.0027(18) 0.0057(14) -0.021(2) O3 0.045(2) 0.075(3) 0.0237(14) 0.0040(17) 0.0054(14) -0.014(2) O4 0.047(2) 0.051(3) 0.0289(14) -0.0074(17) 0.0105(14) -0.014(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 Zn1 O2 1.953(3) . ? Zn1 O1 1.965(3) . ? Zn1 N2 2.085(4) . ? Zn1 N1 2.094(3) . ? Zn1 N3 2.107(4) 2_556 ? Zn2 O3 1.949(3) . ? Zn2 O4 1.966(3) . ? Zn2 N6 2.088(4) . ? Zn2 N5 2.094(4) . ? Zn2 N8 2.108(4) 2_647 ? C1 N3 1.342(6) . ? C1 C2 1.343(8) . ? C2 C3 1.366(6) . ? C3 C4 1.372(6) . ? C4 C5 1.389(8) . ? C4 C6 1.483(6) . ? C5 N3 1.346(5) . ? C6 C11 1.371(6) . ? C6 C7 1.402(7) . ? C7 C8 1.382(6) . ? C8 C9 1.436(6) . ? C8 C12 1.529(7) . ? C9 O1 1.283(5) . ? C9 C10 1.434(7) . ? C10 C11 1.412(6) . ? C10 C16 1.450(6) . ? C12 C13 1.526(7) . ? C12 C15 1.536(7) . ? C12 C14 1.539(8) . ? C16 N2 1.292(5) . ? C17 N2 1.464(5) . ? C17 C18 1.530(6) . ? C17 C22 1.547(5) . ? C18 C19 1.529(7) . ? C19 C20 1.508(6) . ? C20 C21 1.533(6) . ? C21 C22 1.509(6) . ? C22 N1 1.466(5) . ? C23 N1 1.280(5) . ? C23 C24 1.443(6) . ? C24 C29 1.414(6) . ? C24 C25 1.415(5) . ? C25 C26 1.363(7) . ? C26 C27 1.416(6) . ? C26 C34 1.499(5) . ? C27 C28 1.385(5) . ? C28 C29 1.429(7) . ? C28 C30 1.539(6) . ? C29 O2 1.299(4) . ? C30 C32 1.530(7) . ? C30 C33 1.534(7) . ? C30 C31 1.548(7) . ? C34 C38 1.369(8) . ? C34 C35 1.379(7) . ? C35 C36 1.382(5) . ? C36 C37 1.350(9) . ? C37 N4 1.332(8) . ? C38 N4 1.344(5) . ? C39 N7 1.344(9) . ? C39 C40 1.373(9) . ? C40 C41 1.373(6) . ? C41 C42 1.379(7) . ? C42 C43 1.409(8) . ? C42 C44 1.494(5) . ? C43 N7 1.344(5) . ? C44 C45 1.375(7) . ? C44 C49 1.393(6) . ? C45 C46 1.400(5) . ? C46 C47 1.423(6) . ? C46 C54 1.439(7) . ? C47 O3 1.305(4) . ? C47 C48 1.448(7) . ? C48 C49 1.381(5) . ? C48 C50 1.537(6) . ? C50 C53 1.507(8) . ? C50 C51 1.536(7) . ? C50 C52 1.542(7) . ? C54 N5 1.280(5) . ? C55 N5 1.472(5) . ? C55 C60 1.522(6) . ? C55 C56 1.553(5) . ? C56 N6 1.474(5) . ? C56 C57 1.512(7) . ? C57 C58 1.521(6) . ? C58 C59 1.524(5) . ? C59 C60 1.521(6) . ? C61 N6 1.273(5) . ? C61 C62 1.441(6) . ? C62 C63 1.385(5) . ? C62 C67 1.427(7) . ? C63 C64 1.378(6) . ? C64 C65 1.409(6) . ? C64 C72 1.487(6) . ? C65 C66 1.366(6) . ? C66 C67 1.455(6) . ? C66 C68 1.553(7) . ? C67 O4 1.297(5) . ? C68 C69 1.518(8) . ? C68 C71 1.534(6) . ? C68 C70 1.538(7) . ? C72 C73 1.379(6) . ? C72 C76 1.383(7) . ? C73 C74 1.404(6) . ? C74 C75 1.378(8) . ? C75 N8 1.321(6) . ? C76 N8 1.340(5) . ? N3 Zn1 2.107(4) 2_546 ? N8 Zn2 2.108(4) 2_657 ? 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 Zn1 O1 95.16(12) . . ? O2 Zn1 N2 145.38(17) . . ? O1 Zn1 N2 89.32(14) . . ? O2 Zn1 N1 88.16(13) . . ? O1 Zn1 N1 163.63(18) . . ? N2 Zn1 N1 79.07(14) . . ? O2 Zn1 N3 110.35(17) . 2_556 ? O1 Zn1 N3 97.86(16) . 2_556 ? N2 Zn1 N3 102.95(15) . 2_556 ? N1 Zn1 N3 95.98(15) . 2_556 ? O3 Zn2 O4 94.96(12) . . ? O3 Zn2 N6 157.23(16) . . ? O4 Zn2 N6 88.30(13) . . ? O3 Zn2 N5 88.44(13) . . ? O4 Zn2 N5 153.05(16) . . ? N6 Zn2 N5 78.90(14) . . ? O3 Zn2 N8 107.16(16) . 2_647 ? O4 Zn2 N8 101.28(15) . 2_647 ? N6 Zn2 N8 94.21(15) . 2_647 ? N5 Zn2 N8 103.22(15) . 2_647 ? N3 C1 C2 121.3(5) . . ? C1 C2 C3 120.2(5) . . ? C2 C3 C4 121.2(5) . . ? C3 C4 C5 115.2(4) . . ? C3 C4 C6 123.3(5) . . ? C5 C4 C6 121.5(4) . . ? N3 C5 C4 124.0(4) . . ? C11 C6 C7 116.8(4) . . ? C11 C6 C4 122.2(5) . . ? C7 C6 C4 121.0(4) . . ? C8 C7 C6 124.9(4) . . ? C7 C8 C9 118.2(5) . . ? C7 C8 C12 121.7(4) . . ? C9 C8 C12 120.0(4) . . ? O1 C9 C10 122.3(4) . . ? O1 C9 C8 120.0(5) . . ? C10 C9 C8 117.7(4) . . ? C11 C10 C9 120.2(4) . . ? C11 C10 C16 115.1(5) . . ? C9 C10 C16 124.3(4) . . ? C6 C11 C10 122.2(5) . . ? C13 C12 C8 112.1(4) . . ? C13 C12 C15 108.0(5) . . ? C8 C12 C15 109.7(5) . . ? C13 C12 C14 106.6(5) . . ? C8 C12 C14 110.4(5) . . ? C15 C12 C14 109.9(5) . . ? N2 C16 C10 126.4(5) . . ? N2 C17 C18 116.5(4) . . ? N2 C17 C22 108.0(4) . . ? C18 C17 C22 110.2(3) . . ? C19 C18 C17 110.8(4) . . ? C20 C19 C18 112.6(4) . . ? C19 C20 C21 110.6(4) . . ? C22 C21 C20 110.3(4) . . ? N1 C22 C21 116.6(3) . . ? N1 C22 C17 106.7(3) . . ? C21 C22 C17 111.1(4) . . ? N1 C23 C24 124.9(4) . . ? C29 C24 C25 119.9(5) . . ? C29 C24 C23 124.3(4) . . ? C25 C24 C23 115.7(4) . . ? C26 C25 C24 122.8(4) . . ? C25 C26 C27 116.7(4) . . ? C25 C26 C34 121.7(4) . . ? C27 C26 C34 121.5(4) . . ? C28 C27 C26 123.4(5) . . ? C27 C28 C29 119.0(4) . . ? C27 C28 C30 121.5(4) . . ? C29 C28 C30 119.5(4) . . ? O2 C29 C24 122.7(4) . . ? O2 C29 C28 119.1(4) . . ? C24 C29 C28 118.1(4) . . ? C32 C30 C33 106.7(5) . . ? C32 C30 C28 110.7(4) . . ? C33 C30 C28 113.1(4) . . ? C32 C30 C31 109.6(4) . . ? C33 C30 C31 107.5(4) . . ? C28 C30 C31 109.1(5) . . ? C38 C34 C35 116.9(4) . . ? C38 C34 C26 121.9(5) . . ? C35 C34 C26 121.2(5) . . ? C34 C35 C36 118.9(5) . . ? C37 C36 C35 119.0(5) . . ? N4 C37 C36 124.7(5) . . ? N4 C38 C34 125.7(6) . . ? N7 C39 C40 123.7(5) . . ? C39 C40 C41 118.2(6) . . ? C40 C41 C42 121.1(6) . . ? C41 C42 C43 116.3(4) . . ? C41 C42 C44 123.2(5) . . ? C43 C42 C44 120.4(5) . . ? N7 C43 C42 123.7(6) . . ? C45 C44 C49 116.4(4) . . ? C45 C44 C42 121.0(4) . . ? C49 C44 C42 122.6(4) . . ? C44 C45 C46 122.9(4) . . ? C45 C46 C47 120.0(4) . . ? C45 C46 C54 117.1(4) . . ? C47 C46 C54 122.7(4) . . ? O3 C47 C46 122.8(4) . . ? O3 C47 C48 119.6(4) . . ? C46 C47 C48 117.6(4) . . ? C49 C48 C47 118.0(4) . . ? C49 C48 C50 123.2(4) . . ? C47 C48 C50 118.7(4) . . ? C48 C49 C44 124.9(5) . . ? C53 C50 C51 109.2(4) . . ? C53 C50 C48 109.2(5) . . ? C51 C50 C48 110.9(4) . . ? C53 C50 C52 111.1(4) . . ? C51 C50 C52 107.0(6) . . ? C48 C50 C52 109.4(4) . . ? N5 C54 C46 127.1(4) . . ? N5 C55 C60 116.7(3) . . ? N5 C55 C56 107.7(3) . . ? C60 C55 C56 110.2(3) . . ? N6 C56 C57 117.5(3) . . ? N6 C56 C55 106.9(3) . . ? C57 C56 C55 110.7(4) . . ? C56 C57 C58 111.0(4) . . ? C57 C58 C59 111.5(4) . . ? C60 C59 C58 111.5(4) . . ? C59 C60 C55 110.6(4) . . ? N6 C61 C62 127.0(4) . . ? C63 C62 C67 120.0(4) . . ? C63 C62 C61 116.6(4) . . ? C67 C62 C61 123.4(4) . . ? C64 C63 C62 123.2(5) . . ? C63 C64 C65 116.5(4) . . ? C63 C64 C72 121.5(5) . . ? C65 C64 C72 122.0(4) . . ? C66 C65 C64 124.2(4) . . ? C65 C66 C67 118.6(4) . . ? C65 C66 C68 121.8(4) . . ? C67 C66 C68 119.7(4) . . ? O4 C67 C62 123.0(4) . . ? O4 C67 C66 119.5(4) . . ? C62 C67 C66 117.5(4) . . ? C69 C68 C71 108.5(5) . . ? C69 C68 C70 109.9(4) . . ? C71 C68 C70 107.6(4) . . ? C69 C68 C66 109.9(4) . . ? C71 C68 C66 111.8(4) . . ? C70 C68 C66 109.1(5) . . ? C73 C72 C76 115.7(4) . . ? C73 C72 C64 123.0(5) . . ? C76 C72 C64 121.3(4) . . ? C72 C73 C74 120.3(5) . . ? C75 C74 C73 118.2(5) . . ? N8 C75 C74 122.8(4) . . ? N8 C76 C72 125.4(4) . . ? C23 N1 C22 122.9(4) . . ? C23 N1 Zn1 126.0(3) . . ? C22 N1 Zn1 111.1(2) . . ? C16 N2 C17 120.6(4) . . ? C16 N2 Zn1 124.3(3) . . ? C17 N2 Zn1 114.9(2) . . ? C1 N3 C5 118.0(5) . . ? C1 N3 Zn1 121.3(3) . 2_546 ? C5 N3 Zn1 120.3(4) . 2_546 ? C37 N4 C38 114.8(6) . . ? C54 N5 C55 120.6(4) . . ? C54 N5 Zn2 123.7(3) . . ? C55 N5 Zn2 115.3(2) . . ? C61 N6 C56 122.3(4) . . ? C61 N6 Zn2 125.8(3) . . ? C56 N6 Zn2 111.8(2) . . ? C39 N7 C43 116.9(6) . . ? C75 N8 C76 117.5(5) . . ? C75 N8 Zn2 124.5(3) . 2_657 ? C76 N8 Zn2 117.6(3) . 2_657 ? C9 O1 Zn1 132.1(3) . . ? C29 O2 Zn1 129.7(3) . . ? C47 O3 Zn2 129.3(3) . . ? C67 O4 Zn2 132.3(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.307 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.052