Supplementary Material (ESI) for Organic & Biomolecular Chemistry This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Maren Pink' _publ_contact_author_address ; IUMSC, Dept. Chem. Indiana University 800 E. Kirkwood Bloomington, IN 47405 USA ; _publ_contact_author_phone '001 812 855 6821' _publ_contact_author_fax '001 812 855 8300' _publ_contact_author_email mpink@indiana.edu _publ_requested_coeditor_name ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; Photochemical preparation of Pyrrole Ring-Contracted Chlorins by the Wolff Rearrangement ; loop_ _publ_author_name _publ_author_address J.Zaleski ; Indiana University 800 E. Kirkwood Bloomington, IN 47405 USA ; T.Kopke ; Indiana University 800 E. Kirkwood Bloomington, IN 47405 USA ; 'Maren Pink' ; Indiana University 800 E. Kirkwood Bloomington, IN 47405 USA ; #======================================================================= data_05139 _database_code_depnum_ccdc_archive 'CCDC 605756' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H30 N4 Ni O2' _chemical_formula_sum 'C45 H30 N4 Ni O2' _chemical_formula_weight 717.44 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 orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.0768(12) _cell_length_b 14.1377(10) _cell_length_c 27.7514(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6699.9(8) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 6982 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 0.627 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8590 _exptl_absorpt_correction_T_max 0.8955 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 20 seconds each' _diffrn_measurement_method \w-scans _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_number 155 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 808 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 78224 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.09 _reflns_number_total 5956 _reflns_number_gt 5104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SIR-92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2003), XTEL (loc. libr.)' _computing_publication_material 'SHELXTL (Bruker, 2003)' _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^)+(0.0201P)^2^+11.4624P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5956 _refine_ls_number_parameters 500 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1073 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.229 _refine_ls_restrained_S_all 1.229 _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 Ni1 Ni 0.37986(2) 0.20242(3) 0.702908(12) 0.02510(11) Uani 1 1 d . . . N1 N 0.37071(13) 0.33102(18) 0.67929(8) 0.0265(5) Uani 1 1 d . . . N2 N 0.36091(13) 0.15109(17) 0.64072(8) 0.0263(5) Uani 1 1 d . . . N3 N 0.38725(13) 0.07835(17) 0.73252(8) 0.0254(5) Uani 1 1 d . . . N4 N 0.39901(14) 0.25260(18) 0.76241(8) 0.0278(5) Uani 1 1 d . . . C1 C 0.37018(16) 0.4151(2) 0.70495(10) 0.0278(6) Uani 1 1 d . . . C2 C 0.36187(17) 0.4933(2) 0.67314(11) 0.0321(7) Uani 1 1 d . . . H2 H 0.3590 0.5580 0.6821 0.040(9) Uiso 1 1 calc R . . C3 C 0.35884(17) 0.4588(2) 0.62792(11) 0.0307(7) Uani 1 1 d . . . H3 H 0.3543 0.4949 0.5992 0.035(9) Uiso 1 1 calc R . . C4 C 0.36368(16) 0.3587(2) 0.63108(10) 0.0275(6) Uani 1 1 d . . . C5 C 0.35535(16) 0.2968(2) 0.59278(10) 0.0287(6) Uani 1 1 d . . . C6 C 0.34935(17) 0.1990(2) 0.59793(10) 0.0281(6) Uani 1 1 d . . . C7 C 0.33300(18) 0.1343(2) 0.56006(10) 0.0316(7) Uani 1 1 d . . . H7 H 0.3223 0.1499 0.5274 0.028(8) Uiso 1 1 calc R . . C8 C 0.33554(17) 0.0460(2) 0.57912(10) 0.0308(7) Uani 1 1 d . . . H8 H 0.3258 -0.0117 0.5627 0.030(8) Uiso 1 1 calc R . . C9 C 0.35571(16) 0.0569(2) 0.62877(10) 0.0269(6) Uani 1 1 d . . . C10 C 0.37228(16) -0.0196(2) 0.65950(10) 0.0278(6) Uani 1 1 d . . . C11 C 0.38631(16) -0.0076(2) 0.70824(10) 0.0271(6) Uani 1 1 d . . . C12 C 0.40127(17) -0.0837(2) 0.74112(11) 0.0323(7) Uani 1 1 d . . . H12 H 0.4047 -0.1490 0.7334 0.046(10) Uiso 1 1 calc R . . C13 C 0.40958(18) -0.0449(2) 0.78491(11) 0.0321(7) Uani 1 1 d . . . H13 H 0.4196 -0.0780 0.8141 0.037(9) Uiso 1 1 calc R . . C14 C 0.40068(16) 0.0544(2) 0.77992(10) 0.0273(6) Uani 1 1 d . . . C15 C 0.40733(16) 0.1198(2) 0.81876(10) 0.0280(6) Uani 1 1 d . . . C16 C 0.40912(17) 0.2139(2) 0.80737(10) 0.0292(7) Uani 1 1 d . . . C17 C 0.41455(18) 0.3112(2) 0.83148(10) 0.0318(7) Uani 1 1 d . . . H17 H 0.4690 0.3272 0.8419 0.038(9) Uiso 1 1 calc R . . C18 C 0.39723(17) 0.3430(2) 0.78010(10) 0.0297(7) Uani 1 1 d . . . C19 C 0.38081(16) 0.4235(2) 0.75544(10) 0.0276(6) Uani 1 1 d . . . O20 O 0.38981(13) 0.34352(17) 0.91247(7) 0.0391(5) Uani 1 1 d . . . O21 O 0.28523(13) 0.33583(19) 0.86377(8) 0.0460(6) Uani 1 1 d . . . C20 C 0.35446(18) 0.3320(2) 0.86986(11) 0.0329(7) Uani 1 1 d . . . C21 C 0.3385(2) 0.3507(3) 0.95384(12) 0.0502(10) Uani 1 1 d . . . H21A H 0.3687 0.3398 0.9834 0.097(17) Uiso 1 1 calc R . . H21B H 0.2969 0.3032 0.9513 0.087(16) Uiso 1 1 calc R . . H21C H 0.3152 0.4140 0.9549 0.071(14) Uiso 1 1 calc R . . C22 C 0.35298(18) 0.3364(2) 0.54283(10) 0.0313(7) Uani 1 1 d . . . C23 C 0.4215(2) 0.3730(3) 0.52251(12) 0.0422(8) Uani 1 1 d . . . H23 H 0.4683 0.3759 0.5410 0.041(10) Uiso 1 1 calc R . . C24 C 0.4213(2) 0.4052(3) 0.47498(13) 0.0527(10) Uani 1 1 d . . . H24 H 0.4679 0.4299 0.4611 0.044(10) Uiso 1 1 calc R . . C25 C 0.3534(3) 0.4013(3) 0.44807(12) 0.0535(11) Uani 1 1 d . . . H25 H 0.3537 0.4223 0.4155 0.070(13) Uiso 1 1 calc R . . C26 C 0.2852(3) 0.3672(2) 0.46816(12) 0.0480(9) Uani 1 1 d . . . H26 H 0.2385 0.3654 0.4496 0.054(11) Uiso 1 1 calc R . . C27 C 0.2845(2) 0.3356(2) 0.51546(11) 0.0388(8) Uani 1 1 d . . . H27 H 0.2371 0.3132 0.5293 0.036(9) Uiso 1 1 calc R . . C28 C 0.37979(16) -0.1143(2) 0.63700(10) 0.0264(6) Uani 1 1 d . . . C29 C 0.43968(17) -0.1301(2) 0.60378(10) 0.0299(7) Uani 1 1 d . . . H29 H 0.4753 -0.0806 0.5964 0.034(9) Uiso 1 1 calc R . . C30 C 0.44792(19) -0.2171(2) 0.58140(11) 0.0341(7) Uani 1 1 d . . . H30 H 0.4891 -0.2269 0.5589 0.048(10) Uiso 1 1 calc R . . C31 C 0.39669(19) -0.2891(2) 0.59168(11) 0.0354(7) Uani 1 1 d . . . H31 H 0.4018 -0.3483 0.5759 0.032(8) Uiso 1 1 calc R . . C32 C 0.33740(18) -0.2755(2) 0.62514(12) 0.0374(8) Uani 1 1 d . . . H32 H 0.3024 -0.3256 0.6325 0.040(9) Uiso 1 1 calc R . . C33 C 0.32916(17) -0.1889(2) 0.64789(11) 0.0320(7) Uani 1 1 d . . . H33 H 0.2888 -0.1802 0.6710 0.033(9) Uiso 1 1 calc R . . C34 C 0.40985(17) 0.0880(2) 0.86963(10) 0.0304(7) Uani 1 1 d . . . C35 C 0.36199(18) 0.0148(2) 0.88622(11) 0.0360(7) Uani 1 1 d . . . H35 H 0.3263 -0.0149 0.8648 0.041(10) Uiso 1 1 calc R . . C36 C 0.3662(2) -0.0147(3) 0.93376(12) 0.0442(9) Uani 1 1 d . . . H36 H 0.3349 -0.0663 0.9443 0.046(10) Uiso 1 1 calc R . . C37 C 0.4154(2) 0.0299(3) 0.96585(12) 0.0469(10) Uani 1 1 d . . . H37 H 0.4181 0.0092 0.9984 0.048(10) Uiso 1 1 calc R . . C38 C 0.46091(19) 0.1052(3) 0.95045(11) 0.0417(9) Uani 1 1 d . . . H38 H 0.4935 0.1378 0.9727 0.041(9) Uiso 1 1 calc R . . C39 C 0.45888(18) 0.1330(2) 0.90261(10) 0.0337(7) Uani 1 1 d . . . H39 H 0.4914 0.1834 0.8921 0.021(7) Uiso 1 1 calc R . . C40 C 0.37612(17) 0.5164(2) 0.77960(10) 0.0277(6) Uani 1 1 d . . . C41 C 0.43877(19) 0.5515(3) 0.80552(12) 0.0421(8) Uani 1 1 d . . . H41 H 0.4849 0.5145 0.8087 0.056(11) Uiso 1 1 calc R . . C42 C 0.4351(2) 0.6403(3) 0.82703(13) 0.0500(10) Uani 1 1 d . . . H42 H 0.4790 0.6639 0.8443 0.052(11) Uiso 1 1 calc R . . C43 C 0.3684(2) 0.6939(3) 0.82343(12) 0.0420(8) Uani 1 1 d . . . H43 H 0.3657 0.7541 0.8386 0.031(8) Uiso 1 1 calc R . . C44 C 0.3052(2) 0.6600(3) 0.79767(14) 0.0476(9) Uani 1 1 d . . . H44 H 0.2590 0.6970 0.7949 0.068(13) Uiso 1 1 calc R . . C45 C 0.30921(19) 0.5720(3) 0.77580(13) 0.0430(8) Uani 1 1 d . . . H45 H 0.2656 0.5494 0.7579 0.066(12) 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 Ni1 0.02196(19) 0.0344(2) 0.01893(19) 0.00408(16) 0.00041(14) 0.00283(15) N1 0.0216(12) 0.0351(14) 0.0229(12) 0.0043(10) -0.0005(10) 0.0004(10) N2 0.0221(12) 0.0352(14) 0.0217(12) 0.0019(10) 0.0018(10) 0.0059(10) N3 0.0210(12) 0.0352(14) 0.0201(11) 0.0030(10) 0.0022(9) 0.0029(10) N4 0.0263(13) 0.0352(14) 0.0218(12) 0.0041(11) -0.0010(10) 0.0020(11) C1 0.0208(14) 0.0337(16) 0.0290(15) 0.0045(13) -0.0009(12) -0.0011(12) C2 0.0310(16) 0.0323(17) 0.0332(16) 0.0051(13) -0.0048(13) -0.0043(13) C3 0.0305(16) 0.0341(17) 0.0274(15) 0.0101(13) -0.0045(13) -0.0042(13) C4 0.0207(14) 0.0376(17) 0.0241(14) 0.0062(13) -0.0009(11) -0.0004(12) C5 0.0210(14) 0.0408(17) 0.0242(14) 0.0017(13) 0.0017(11) 0.0065(13) C6 0.0248(14) 0.0369(17) 0.0227(14) 0.0019(13) 0.0019(11) 0.0091(13) C7 0.0336(17) 0.0388(18) 0.0223(15) 0.0005(13) -0.0013(12) 0.0096(14) C8 0.0298(16) 0.0385(18) 0.0241(14) -0.0017(13) 0.0007(12) 0.0069(13) C9 0.0215(14) 0.0346(17) 0.0245(14) 0.0007(12) 0.0033(12) 0.0050(12) C10 0.0185(13) 0.0379(17) 0.0271(15) 0.0027(13) 0.0035(11) 0.0014(12) C11 0.0215(14) 0.0357(16) 0.0239(14) 0.0035(13) 0.0021(11) 0.0033(12) C12 0.0288(16) 0.0382(18) 0.0300(16) 0.0064(14) 0.0018(13) 0.0047(13) C13 0.0303(16) 0.0394(18) 0.0267(16) 0.0082(13) 0.0022(12) 0.0058(13) C14 0.0218(14) 0.0341(17) 0.0259(15) 0.0054(13) 0.0029(11) 0.0054(12) C15 0.0220(14) 0.0391(18) 0.0228(14) 0.0035(13) 0.0033(12) 0.0074(13) C16 0.0248(15) 0.0413(18) 0.0216(14) 0.0024(13) -0.0002(11) 0.0039(13) C17 0.0263(15) 0.0424(19) 0.0267(15) 0.0023(14) -0.0035(12) 0.0010(13) C18 0.0243(15) 0.0438(19) 0.0209(14) 0.0006(13) -0.0008(12) -0.0001(13) C19 0.0206(14) 0.0379(17) 0.0242(14) 0.0006(13) -0.0014(11) -0.0003(12) O20 0.0407(13) 0.0520(14) 0.0246(11) -0.0045(10) -0.0007(9) 0.0045(11) O21 0.0282(13) 0.0677(17) 0.0421(13) -0.0111(12) 0.0029(10) -0.0011(11) C20 0.0326(18) 0.0370(17) 0.0292(16) 0.0007(13) 0.0002(13) -0.0021(14) C21 0.062(2) 0.057(2) 0.0323(19) -0.0050(17) 0.0118(17) 0.001(2) C22 0.0380(17) 0.0313(16) 0.0245(15) 0.0050(13) 0.0024(13) 0.0104(14) C23 0.0404(19) 0.052(2) 0.0342(18) 0.0121(16) 0.0059(15) 0.0095(16) C24 0.064(3) 0.056(2) 0.039(2) 0.0166(18) 0.0212(19) 0.018(2) C25 0.088(3) 0.046(2) 0.0262(18) 0.0062(16) 0.0023(19) 0.023(2) C26 0.073(3) 0.0370(19) 0.0336(18) 0.0027(15) -0.0154(18) 0.0132(18) C27 0.047(2) 0.0384(18) 0.0315(17) 0.0023(14) -0.0067(15) 0.0075(16) C28 0.0256(15) 0.0299(16) 0.0237(14) 0.0042(12) -0.0039(12) 0.0025(12) C29 0.0295(16) 0.0311(16) 0.0292(16) 0.0051(13) 0.0023(12) 0.0017(13) C30 0.0388(18) 0.0344(18) 0.0291(16) 0.0023(13) 0.0035(14) 0.0062(14) C31 0.0414(18) 0.0309(17) 0.0340(17) 0.0005(14) -0.0105(14) 0.0039(14) C32 0.0295(17) 0.0397(19) 0.0429(19) 0.0108(15) -0.0109(14) -0.0033(14) C33 0.0236(15) 0.0409(19) 0.0314(16) 0.0077(14) -0.0027(12) 0.0004(13) C34 0.0270(15) 0.0406(18) 0.0238(15) 0.0051(13) 0.0043(12) 0.0135(13) C35 0.0285(16) 0.048(2) 0.0312(16) 0.0073(15) 0.0045(13) 0.0105(15) C36 0.0345(18) 0.062(2) 0.0362(18) 0.0220(17) 0.0116(15) 0.0124(17) C37 0.0368(19) 0.076(3) 0.0275(17) 0.0187(18) 0.0060(15) 0.0211(18) C38 0.0345(18) 0.065(2) 0.0253(16) -0.0014(16) -0.0019(14) 0.0191(17) C39 0.0291(16) 0.0455(19) 0.0265(16) 0.0054(14) 0.0024(12) 0.0127(14) C40 0.0274(15) 0.0334(16) 0.0224(14) 0.0019(12) 0.0016(12) -0.0020(13) C41 0.0296(17) 0.061(2) 0.0358(18) -0.0176(17) -0.0052(14) 0.0074(16) C42 0.039(2) 0.069(3) 0.041(2) -0.0242(19) -0.0072(16) -0.0034(18) C43 0.049(2) 0.0385(19) 0.0384(18) -0.0077(15) 0.0054(16) -0.0018(16) C44 0.0375(19) 0.047(2) 0.058(2) -0.0023(18) -0.0042(17) 0.0074(16) C45 0.0304(18) 0.045(2) 0.054(2) -0.0047(17) -0.0083(15) -0.0003(15) _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 N4 1.827(2) . ? Ni1 N2 1.900(2) . ? Ni1 N1 1.939(2) . ? Ni1 N3 1.941(2) . ? N1 C1 1.386(4) . ? N1 C4 1.399(4) . ? N2 C9 1.375(4) . ? N2 C6 1.381(4) . ? N3 C14 1.378(4) . ? N3 C11 1.390(4) . ? N4 C18 1.370(4) . ? N4 C16 1.373(4) . ? C1 C19 1.418(4) . ? C1 C2 1.421(4) . ? C2 C3 1.347(4) . ? C2 H2 0.9500 . ? C3 C4 1.420(4) . ? C3 H3 0.9500 . ? C4 C5 1.385(4) . ? C5 C6 1.393(4) . ? C5 C22 1.495(4) . ? C6 C7 1.422(4) . ? C7 C8 1.356(4) . ? C7 H7 0.9500 . ? C8 C9 1.429(4) . ? C8 H8 0.9500 . ? C9 C10 1.406(4) . ? C10 C11 1.384(4) . ? C10 C28 1.483(4) . ? C11 C12 1.434(4) . ? C12 C13 1.341(4) . ? C12 H12 0.9500 . ? C13 C14 1.419(4) . ? C13 H13 0.9500 . ? C14 C15 1.425(4) . ? C15 C16 1.368(4) . ? C15 C34 1.482(4) . ? C16 C17 1.532(4) . ? C16 C18 1.986(4) . ? C17 C20 1.508(4) . ? C17 C18 1.524(4) . ? C17 H17 1.0000 . ? C18 C19 1.356(4) . ? C19 C40 1.477(4) . ? O20 C20 1.337(4) . ? O20 C21 1.448(4) . ? O21 C20 1.195(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C27 1.395(4) . ? C22 C23 1.399(5) . ? C23 C24 1.396(5) . ? C23 H23 0.9500 . ? C24 C25 1.380(6) . ? C24 H24 0.9500 . ? C25 C26 1.378(6) . ? C25 H25 0.9500 . ? C26 C27 1.387(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.395(4) . ? C28 C33 1.397(4) . ? C29 C30 1.384(4) . ? C29 H29 0.9500 . ? C30 C31 1.372(5) . ? C30 H30 0.9500 . ? C31 C32 1.387(5) . ? C31 H31 0.9500 . ? C32 C33 1.384(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.394(4) . ? C34 C35 1.397(5) . ? C35 C36 1.386(4) . ? C35 H35 0.9500 . ? C36 C37 1.377(5) . ? C36 H36 0.9500 . ? C37 C38 1.386(5) . ? C37 H37 0.9500 . ? C38 C39 1.385(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.381(4) . ? C40 C45 1.391(4) . ? C41 C42 1.391(5) . ? C41 H41 0.9500 . ? C42 C43 1.372(5) . ? C42 H42 0.9500 . ? C43 C44 1.380(5) . ? C43 H43 0.9500 . ? C44 C45 1.386(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? 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 N4 Ni1 N2 179.33(11) . . ? N4 Ni1 N1 87.47(10) . . ? N2 Ni1 N1 92.14(10) . . ? N4 Ni1 N3 87.52(10) . . ? N2 Ni1 N3 92.90(10) . . ? N1 Ni1 N3 174.66(10) . . ? C1 N1 C4 104.5(2) . . ? C1 N1 Ni1 129.15(19) . . ? C4 N1 Ni1 126.4(2) . . ? C9 N2 C6 105.0(2) . . ? C9 N2 Ni1 126.86(19) . . ? C6 N2 Ni1 128.2(2) . . ? C14 N3 C11 104.5(2) . . ? C14 N3 Ni1 129.6(2) . . ? C11 N3 Ni1 125.75(18) . . ? C18 N4 C16 92.8(2) . . ? C18 N4 Ni1 133.0(2) . . ? C16 N4 Ni1 133.6(2) . . ? N1 C1 C19 125.3(3) . . ? N1 C1 C2 110.4(3) . . ? C19 C1 C2 124.2(3) . . ? C3 C2 C1 107.6(3) . . ? C3 C2 H2 126.2 . . ? C1 C2 H2 126.2 . . ? C2 C3 C4 107.5(3) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? C5 C4 N1 124.4(3) . . ? C5 C4 C3 125.2(3) . . ? N1 C4 C3 110.1(3) . . ? C4 C5 C6 123.8(3) . . ? C4 C5 C22 118.5(3) . . ? C6 C5 C22 117.7(3) . . ? N2 C6 C5 124.4(3) . . ? N2 C6 C7 110.3(3) . . ? C5 C6 C7 125.3(3) . . ? C8 C7 C6 107.3(3) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 106.5(3) . . ? C7 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? N2 C9 C10 125.9(3) . . ? N2 C9 C8 110.6(3) . . ? C10 C9 C8 123.4(3) . . ? C11 C10 C9 122.2(3) . . ? C11 C10 C28 120.5(3) . . ? C9 C10 C28 117.2(2) . . ? C10 C11 N3 125.7(3) . . ? C10 C11 C12 124.1(3) . . ? N3 C11 C12 110.2(2) . . ? C13 C12 C11 106.8(3) . . ? C13 C12 H12 126.6 . . ? C11 C12 H12 126.6 . . ? C12 C13 C14 107.7(3) . . ? C12 C13 H13 126.1 . . ? C14 C13 H13 126.1 . . ? N3 C14 C13 110.8(3) . . ? N3 C14 C15 125.2(3) . . ? C13 C14 C15 124.0(3) . . ? C16 C15 C14 117.3(3) . . ? C16 C15 C34 120.9(3) . . ? C14 C15 C34 121.8(3) . . ? C15 C16 N4 126.5(3) . . ? C15 C16 C17 140.7(3) . . ? N4 C16 C17 92.7(2) . . ? C15 C16 C18 168.4(3) . . ? N4 C16 C18 43.54(16) . . ? C17 C16 C18 49.28(16) . . ? C20 C17 C18 118.1(3) . . ? C20 C17 C16 116.3(3) . . ? C18 C17 C16 81.1(2) . . ? C20 C17 H17 112.6 . . ? C18 C17 H17 112.6 . . ? C16 C17 H17 112.6 . . ? C19 C18 N4 127.3(3) . . ? C19 C18 C17 139.4(3) . . ? N4 C18 C17 93.2(2) . . ? C19 C18 C16 169.6(3) . . ? N4 C18 C16 43.67(16) . . ? C17 C18 C16 49.65(17) . . ? C18 C19 C1 117.1(3) . . ? C18 C19 C40 121.9(3) . . ? C1 C19 C40 121.0(3) . . ? C20 O20 C21 115.9(3) . . ? O21 C20 O20 124.5(3) . . ? O21 C20 C17 125.6(3) . . ? O20 C20 C17 109.9(3) . . ? O20 C21 H21A 109.5 . . ? O20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 119.0(3) . . ? C27 C22 C5 121.6(3) . . ? C23 C22 C5 119.3(3) . . ? C24 C23 C22 119.9(3) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.1(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 120.3(3) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 120.2(4) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C22 120.4(3) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? C29 C28 C33 118.4(3) . . ? C29 C28 C10 119.1(3) . . ? C33 C28 C10 122.5(3) . . ? C30 C29 C28 120.9(3) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C31 C30 C29 120.1(3) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.1(3) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 120.2(3) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C28 120.4(3) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C39 C34 C35 118.2(3) . . ? C39 C34 C15 120.3(3) . . ? C35 C34 C15 121.4(3) . . ? C36 C35 C34 120.5(3) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 C35 120.6(3) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 119.7(3) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C39 C38 C37 119.9(3) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C34 121.0(3) . . ? C38 C39 H39 119.5 . . ? C34 C39 H39 119.5 . . ? C41 C40 C45 118.2(3) . . ? C41 C40 C19 120.9(3) . . ? C45 C40 C19 120.9(3) . . ? C40 C41 C42 120.9(3) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C43 C42 C41 120.3(3) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 119.7(3) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C43 C44 C45 120.0(3) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C40 121.0(3) . . ? C44 C45 H45 119.5 . . ? C40 C45 H45 119.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Ni1 N1 C1 -7.3(2) . . . . ? N2 Ni1 N1 C1 173.3(2) . . . . ? N3 Ni1 N1 C1 12.8(12) . . . . ? N4 Ni1 N1 C4 172.1(2) . . . . ? N2 Ni1 N1 C4 -7.3(2) . . . . ? N3 Ni1 N1 C4 -167.8(9) . . . . ? N4 Ni1 N2 C9 129(10) . . . . ? N1 Ni1 N2 C9 -177.7(2) . . . . ? N3 Ni1 N2 C9 0.5(2) . . . . ? N4 Ni1 N2 C6 -51(10) . . . . ? N1 Ni1 N2 C6 2.3(2) . . . . ? N3 Ni1 N2 C6 -179.5(2) . . . . ? N4 Ni1 N3 C14 0.8(2) . . . . ? N2 Ni1 N3 C14 -179.7(2) . . . . ? N1 Ni1 N3 C14 -19.3(12) . . . . ? N4 Ni1 N3 C11 -173.3(2) . . . . ? N2 Ni1 N3 C11 6.1(2) . . . . ? N1 Ni1 N3 C11 166.6(10) . . . . ? N2 Ni1 N4 C18 60(10) . . . . ? N1 Ni1 N4 C18 6.4(3) . . . . ? N3 Ni1 N4 C18 -171.8(3) . . . . ? N2 Ni1 N4 C16 -131(10) . . . . ? N1 Ni1 N4 C16 175.0(3) . . . . ? N3 Ni1 N4 C16 -3.2(3) . . . . ? C4 N1 C1 C19 -175.9(3) . . . . ? Ni1 N1 C1 C19 3.6(4) . . . . ? C4 N1 C1 C2 0.8(3) . . . . ? Ni1 N1 C1 C2 -179.7(2) . . . . ? N1 C1 C2 C3 -1.2(3) . . . . ? C19 C1 C2 C3 175.5(3) . . . . ? C1 C2 C3 C4 1.1(3) . . . . ? C1 N1 C4 C5 -174.6(3) . . . . ? Ni1 N1 C4 C5 5.9(4) . . . . ? C1 N1 C4 C3 -0.1(3) . . . . ? Ni1 N1 C4 C3 -179.63(19) . . . . ? C2 C3 C4 C5 173.7(3) . . . . ? C2 C3 C4 N1 -0.7(3) . . . . ? N1 C4 C5 C6 3.1(5) . . . . ? C3 C4 C5 C6 -170.5(3) . . . . ? N1 C4 C5 C22 -176.6(3) . . . . ? C3 C4 C5 C22 9.7(4) . . . . ? C9 N2 C6 C5 -175.2(3) . . . . ? Ni1 N2 C6 C5 4.8(4) . . . . ? C9 N2 C6 C7 3.0(3) . . . . ? Ni1 N2 C6 C7 -176.96(19) . . . . ? C4 C5 C6 N2 -8.7(5) . . . . ? C22 C5 C6 N2 171.0(3) . . . . ? C4 C5 C6 C7 173.4(3) . . . . ? C22 C5 C6 C7 -6.9(4) . . . . ? N2 C6 C7 C8 -0.9(3) . . . . ? C5 C6 C7 C8 177.3(3) . . . . ? C6 C7 C8 C9 -1.5(3) . . . . ? C6 N2 C9 C10 172.3(3) . . . . ? Ni1 N2 C9 C10 -7.7(4) . . . . ? C6 N2 C9 C8 -4.0(3) . . . . ? Ni1 N2 C9 C8 175.97(19) . . . . ? C7 C8 C9 N2 3.5(3) . . . . ? C7 C8 C9 C10 -172.9(3) . . . . ? N2 C9 C10 C11 8.7(5) . . . . ? C8 C9 C10 C11 -175.4(3) . . . . ? N2 C9 C10 C28 -167.1(3) . . . . ? C8 C9 C10 C28 8.8(4) . . . . ? C9 C10 C11 N3 -1.1(4) . . . . ? C28 C10 C11 N3 174.6(3) . . . . ? C9 C10 C11 C12 178.2(3) . . . . ? C28 C10 C11 C12 -6.1(4) . . . . ? C14 N3 C11 C10 177.9(3) . . . . ? Ni1 N3 C11 C10 -6.7(4) . . . . ? C14 N3 C11 C12 -1.5(3) . . . . ? Ni1 N3 C11 C12 173.87(19) . . . . ? C10 C11 C12 C13 -178.2(3) . . . . ? N3 C11 C12 C13 1.2(3) . . . . ? C11 C12 C13 C14 -0.5(3) . . . . ? C11 N3 C14 C13 1.2(3) . . . . ? Ni1 N3 C14 C13 -173.9(2) . . . . ? C11 N3 C14 C15 179.4(3) . . . . ? Ni1 N3 C14 C15 4.3(4) . . . . ? C12 C13 C14 N3 -0.5(4) . . . . ? C12 C13 C14 C15 -178.7(3) . . . . ? N3 C14 C15 C16 -7.6(4) . . . . ? C13 C14 C15 C16 170.3(3) . . . . ? N3 C14 C15 C34 170.6(3) . . . . ? C13 C14 C15 C34 -11.4(4) . . . . ? C14 C15 C16 N4 5.5(4) . . . . ? C34 C15 C16 N4 -172.8(3) . . . . ? C14 C15 C16 C17 179.4(3) . . . . ? C34 C15 C16 C17 1.2(6) . . . . ? C14 C15 C16 C18 33.6(14) . . . . ? C34 C15 C16 C18 -144.7(11) . . . . ? C18 N4 C16 C15 172.1(3) . . . . ? Ni1 N4 C16 C15 0.4(5) . . . . ? C18 N4 C16 C17 -4.1(2) . . . . ? Ni1 N4 C16 C17 -175.8(2) . . . . ? Ni1 N4 C16 C18 -171.7(3) . . . . ? C15 C16 C17 C20 -54.4(5) . . . . ? N4 C16 C17 C20 120.7(3) . . . . ? C18 C16 C17 C20 117.0(3) . . . . ? C15 C16 C17 C18 -171.4(4) . . . . ? N4 C16 C17 C18 3.7(2) . . . . ? C16 N4 C18 C19 -173.1(3) . . . . ? Ni1 N4 C18 C19 -1.3(5) . . . . ? C16 N4 C18 C17 4.1(2) . . . . ? Ni1 N4 C18 C17 175.9(2) . . . . ? Ni1 N4 C18 C16 171.8(3) . . . . ? C20 C17 C18 C19 57.8(5) . . . . ? C16 C17 C18 C19 172.9(4) . . . . ? C20 C17 C18 N4 -118.8(3) . . . . ? C16 C17 C18 N4 -3.7(2) . . . . ? C20 C17 C18 C16 -115.1(3) . . . . ? C15 C16 C18 C19 -1(2) . . . . ? N4 C16 C18 C19 32.0(14) . . . . ? C17 C16 C18 C19 -153.3(14) . . . . ? C15 C16 C18 N4 -33.4(12) . . . . ? C17 C16 C18 N4 174.6(3) . . . . ? C15 C16 C18 C17 152.0(13) . . . . ? N4 C16 C18 C17 -174.6(3) . . . . ? N4 C18 C19 C1 -5.4(5) . . . . ? C17 C18 C19 C1 178.9(3) . . . . ? C16 C18 C19 C1 -32.8(15) . . . . ? N4 C18 C19 C40 176.2(3) . . . . ? C17 C18 C19 C40 0.5(6) . . . . ? C16 C18 C19 C40 148.7(13) . . . . ? N1 C1 C19 C18 4.0(4) . . . . ? C2 C1 C19 C18 -172.3(3) . . . . ? N1 C1 C19 C40 -177.6(3) . . . . ? C2 C1 C19 C40 6.2(4) . . . . ? C21 O20 C20 O21 6.9(5) . . . . ? C21 O20 C20 C17 -171.6(3) . . . . ? C18 C17 C20 O21 31.5(5) . . . . ? C16 C17 C20 O21 -62.3(4) . . . . ? C18 C17 C20 O20 -150.0(3) . . . . ? C16 C17 C20 O20 116.1(3) . . . . ? C4 C5 C22 C27 -110.2(3) . . . . ? C6 C5 C22 C27 70.0(4) . . . . ? C4 C5 C22 C23 71.4(4) . . . . ? C6 C5 C22 C23 -108.3(4) . . . . ? C27 C22 C23 C24 -2.0(5) . . . . ? C5 C22 C23 C24 176.4(3) . . . . ? C22 C23 C24 C25 0.2(6) . . . . ? C23 C24 C25 C26 1.2(6) . . . . ? C24 C25 C26 C27 -0.7(6) . . . . ? C25 C26 C27 C22 -1.2(5) . . . . ? C23 C22 C27 C26 2.5(5) . . . . ? C5 C22 C27 C26 -175.8(3) . . . . ? C11 C10 C28 C29 -112.8(3) . . . . ? C9 C10 C28 C29 63.1(4) . . . . ? C11 C10 C28 C33 67.0(4) . . . . ? C9 C10 C28 C33 -117.1(3) . . . . ? C33 C28 C29 C30 1.2(4) . . . . ? C10 C28 C29 C30 -179.0(3) . . . . ? C28 C29 C30 C31 0.2(5) . . . . ? C29 C30 C31 C32 -1.2(5) . . . . ? C30 C31 C32 C33 0.7(5) . . . . ? C31 C32 C33 C28 0.7(4) . . . . ? C29 C28 C33 C32 -1.7(4) . . . . ? C10 C28 C33 C32 178.5(3) . . . . ? C16 C15 C34 C39 -40.3(4) . . . . ? C14 C15 C34 C39 141.6(3) . . . . ? C16 C15 C34 C35 137.8(3) . . . . ? C14 C15 C34 C35 -40.4(4) . . . . ? C39 C34 C35 C36 -2.9(4) . . . . ? C15 C34 C35 C36 179.0(3) . . . . ? C34 C35 C36 C37 2.5(5) . . . . ? C35 C36 C37 C38 0.2(5) . . . . ? C36 C37 C38 C39 -2.4(5) . . . . ? C37 C38 C39 C34 1.9(5) . . . . ? C35 C34 C39 C38 0.7(4) . . . . ? C15 C34 C39 C38 178.9(3) . . . . ? C18 C19 C40 C41 57.4(4) . . . . ? C1 C19 C40 C41 -121.0(3) . . . . ? C18 C19 C40 C45 -124.3(3) . . . . ? C1 C19 C40 C45 57.3(4) . . . . ? C45 C40 C41 C42 -0.3(5) . . . . ? C19 C40 C41 C42 178.0(3) . . . . ? C40 C41 C42 C43 1.1(6) . . . . ? C41 C42 C43 C44 -1.1(6) . . . . ? C42 C43 C44 C45 0.3(6) . . . . ? C43 C44 C45 C40 0.4(6) . . . . ? C41 C40 C45 C44 -0.4(5) . . . . ? C19 C40 C45 C44 -178.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.322 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.085 # Attachment '05155.cif' data_05155 _database_code_depnum_ccdc_archive 'CCDC 605757' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H30 Cu N4 O2' _chemical_formula_sum 'C45 H30 Cu N4 O2' _chemical_formula_weight 722.27 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_space_group_name_Hall '-P 2n 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 17.074(3) _cell_length_b 14.209(2) _cell_length_c 27.882(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6764.3(19) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 4312 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 26.2 _exptl_crystal_description block _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2984 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9032 _exptl_absorpt_correction_T_max 0.9339 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 60 seconds each' _diffrn_measurement_method \w-scans _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72376 _diffrn_reflns_av_R_equivalents 0.1183 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.43 _reflns_number_total 6870 _reflns_number_gt 4587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SIR-92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2003), XTEL (loc. libr.)' _computing_publication_material 'SHELXTL (Bruker, 2003)' _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. The data are weak and R(int) is somewhat large due to the small crystal size. ; _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^)+(0.0200P)^2^+16.1074P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6870 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1234 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Cu1 Cu 0.88167(2) 0.20242(3) 0.203495(15) 0.02861(12) Uani 1 1 d . . . N1 N 0.88705(16) 0.0758(2) 0.23464(10) 0.0293(7) Uani 1 1 d . . . N2 N 0.86227(16) 0.1512(2) 0.14076(10) 0.0292(7) Uani 1 1 d . . . N3 N 0.87180(16) 0.3350(2) 0.18018(10) 0.0280(6) Uani 1 1 d . . . N4 N 0.90278(17) 0.2539(2) 0.26460(11) 0.0315(7) Uani 1 1 d . . . C1 C 0.90133(19) 0.0531(3) 0.28135(13) 0.0310(8) Uani 1 1 d . . . C2 C 0.9101(2) -0.0471(3) 0.28625(13) 0.0354(9) Uani 1 1 d . . . H2A H 0.9203 -0.0803 0.3152 0.043 Uiso 1 1 calc R . . C3 C 0.9011(2) -0.0852(3) 0.24259(13) 0.0331(9) Uani 1 1 d . . . H3A H 0.9040 -0.1501 0.2348 0.040 Uiso 1 1 calc R . . C4 C 0.88613(19) -0.0090(3) 0.20974(13) 0.0304(8) Uani 1 1 d . . . C5 C 0.87305(19) -0.0188(3) 0.16077(12) 0.0293(8) Uani 1 1 d . . . C6 C 0.85694(19) 0.0575(3) 0.12918(13) 0.0291(8) Uani 1 1 d . . . C7 C 0.8372(2) 0.0475(3) 0.07976(13) 0.0328(8) Uani 1 1 d . . . H7A H 0.8277 -0.0100 0.0633 0.039 Uiso 1 1 calc R . . C8 C 0.8344(2) 0.1352(3) 0.06065(13) 0.0343(9) Uani 1 1 d . . . H8A H 0.8238 0.1507 0.0281 0.041 Uiso 1 1 calc R . . C9 C 0.85032(19) 0.1997(3) 0.09842(12) 0.0302(8) Uani 1 1 d . . . C10 C 0.85505(19) 0.2990(3) 0.09415(12) 0.0296(8) Uani 1 1 d . . . C11 C 0.86332(19) 0.3615(3) 0.13222(13) 0.0298(8) Uani 1 1 d . . . C12 C 0.8572(2) 0.4616(3) 0.12923(13) 0.0327(8) Uani 1 1 d . . . H12A H 0.8512 0.4975 0.1007 0.039 Uiso 1 1 calc R . . C13 C 0.8613(2) 0.4959(3) 0.17442(13) 0.0336(9) Uani 1 1 d . . . H13A H 0.8582 0.5602 0.1835 0.040 Uiso 1 1 calc R . . C14 C 0.87118(19) 0.4176(3) 0.20609(13) 0.0305(8) Uani 1 1 d . . . C15 C 0.88241(19) 0.4243(3) 0.25662(12) 0.0288(8) Uani 1 1 d . . . C16 C 0.8994(2) 0.3443(3) 0.28210(13) 0.0327(9) Uani 1 1 d . . . C17 C 0.9149(2) 0.3127(3) 0.33375(13) 0.0347(9) Uani 1 1 d . . . H17A H 0.9690 0.3290 0.3447 0.042 Uiso 1 1 calc R . . C18 C 0.91123(19) 0.2147(3) 0.30930(12) 0.0313(8) Uani 1 1 d . . . C19 C 0.90826(19) 0.1199(3) 0.31988(13) 0.0296(8) Uani 1 1 d . . . O20 O 0.88931(15) 0.3436(2) 0.41440(9) 0.0402(7) Uani 1 1 d . . . C20 C 0.8546(2) 0.3327(3) 0.37139(14) 0.0353(9) Uani 1 1 d . . . O21 O 0.78539(15) 0.3366(2) 0.36502(10) 0.0483(8) Uani 1 1 d . . . C21 C 0.8373(3) 0.3510(3) 0.45523(15) 0.0519(12) Uani 1 1 d . . . H21A H 0.8676 0.3444 0.4849 0.078 Uiso 1 1 calc R . . H21B H 0.7978 0.3011 0.4536 0.078 Uiso 1 1 calc R . . H21C H 0.8113 0.4125 0.4548 0.078 Uiso 1 1 calc R . . C22 C 0.8802(2) -0.1133(2) 0.13818(12) 0.0271(7) Uani 1 1 d . . . C23 C 0.8295(2) -0.1877(3) 0.14882(14) 0.0337(9) Uani 1 1 d . . . H23A H 0.7893 -0.1792 0.1720 0.040 Uiso 1 1 calc R . . C24 C 0.8372(2) -0.2737(3) 0.12599(14) 0.0385(10) Uani 1 1 d . . . H24A H 0.8017 -0.3233 0.1330 0.046 Uiso 1 1 calc R . . C25 C 0.8968(2) -0.2879(3) 0.09279(14) 0.0376(9) Uani 1 1 d . . . H25A H 0.9023 -0.3472 0.0774 0.045 Uiso 1 1 calc R . . C26 C 0.9481(2) -0.2154(3) 0.08228(14) 0.0352(9) Uani 1 1 d . . . H26A H 0.9889 -0.2247 0.0596 0.042 Uiso 1 1 calc R . . C27 C 0.9399(2) -0.1290(3) 0.10487(13) 0.0317(8) Uani 1 1 d . . . H27A H 0.9755 -0.0796 0.0976 0.038 Uiso 1 1 calc R . . C28 C 0.8524(2) 0.3376(3) 0.04432(13) 0.0329(8) Uani 1 1 d . . . C29 C 0.7838(2) 0.3368(3) 0.01733(14) 0.0393(9) Uani 1 1 d . . . H29A H 0.7364 0.3151 0.0313 0.047 Uiso 1 1 calc R . . C30 C 0.7843(3) 0.3674(3) -0.02994(15) 0.0469(11) Uani 1 1 d . . . H30A H 0.7375 0.3648 -0.0484 0.056 Uiso 1 1 calc R . . C31 C 0.8522(3) 0.4017(3) -0.05039(15) 0.0521(12) Uani 1 1 d . . . H31A H 0.8522 0.4224 -0.0828 0.063 Uiso 1 1 calc R . . C32 C 0.9203(3) 0.4058(3) -0.02346(15) 0.0509(12) Uani 1 1 d . . . H32A H 0.9670 0.4303 -0.0373 0.061 Uiso 1 1 calc R . . C33 C 0.9205(2) 0.3742(3) 0.02373(14) 0.0421(10) Uani 1 1 d . . . H33A H 0.9672 0.3776 0.0421 0.050 Uiso 1 1 calc R . . C34 C 0.8765(2) 0.5168(3) 0.28096(12) 0.0304(8) Uani 1 1 d . . . C35 C 0.8088(2) 0.5702(3) 0.27780(17) 0.0478(11) Uani 1 1 d . . . H35A H 0.7653 0.5466 0.2603 0.057 Uiso 1 1 calc R . . C36 C 0.8034(2) 0.6572(3) 0.29974(17) 0.0520(11) Uani 1 1 d . . . H36A H 0.7562 0.6924 0.2973 0.062 Uiso 1 1 calc R . . C37 C 0.8664(3) 0.6936(3) 0.32531(14) 0.0463(10) Uani 1 1 d . . . H37A H 0.8630 0.7533 0.3405 0.056 Uiso 1 1 calc R . . C38 C 0.9338(3) 0.6408(4) 0.32808(17) 0.0594(14) Uani 1 1 d . . . H38A H 0.9777 0.6649 0.3451 0.071 Uiso 1 1 calc R . . C39 C 0.9388(2) 0.5532(4) 0.30649(16) 0.0555(13) Uani 1 1 d . . . H39A H 0.9857 0.5177 0.3093 0.067 Uiso 1 1 calc R . . C40 C 0.9100(2) 0.0883(3) 0.37074(13) 0.0324(9) Uani 1 1 d . . . C41 C 0.9582(2) 0.1329(3) 0.40395(13) 0.0368(9) Uani 1 1 d . . . H41A H 0.9904 0.1836 0.3938 0.044 Uiso 1 1 calc R . . C42 C 0.9600(2) 0.1049(3) 0.45169(14) 0.0449(11) Uani 1 1 d . . . H42A H 0.9919 0.1376 0.4741 0.054 Uiso 1 1 calc R . . C43 C 0.9150(2) 0.0291(4) 0.46631(15) 0.0498(12) Uani 1 1 d . . . H43A H 0.9177 0.0079 0.4986 0.060 Uiso 1 1 calc R . . C44 C 0.8660(2) -0.0159(3) 0.43399(15) 0.0487(12) Uani 1 1 d . . . H44A H 0.8349 -0.0676 0.4442 0.058 Uiso 1 1 calc R . . C45 C 0.8623(2) 0.0144(3) 0.38677(14) 0.0372(9) Uani 1 1 d . . . H45A H 0.8271 -0.0152 0.3651 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0229(2) 0.0409(3) 0.0220(2) 0.0064(2) 0.00007(17) 0.00256(19) N1 0.0211(14) 0.0434(18) 0.0233(15) 0.0040(13) 0.0012(12) 0.0046(13) N2 0.0244(15) 0.0391(18) 0.0241(16) 0.0045(13) 0.0015(12) 0.0049(13) N3 0.0242(15) 0.0365(17) 0.0233(15) 0.0024(13) -0.0003(12) -0.0006(13) N4 0.0269(15) 0.0385(18) 0.0290(17) 0.0082(14) -0.0014(12) 0.0011(13) C1 0.0218(17) 0.044(2) 0.0274(19) 0.0089(17) 0.0031(14) 0.0076(15) C2 0.0300(18) 0.047(2) 0.030(2) 0.0097(17) 0.0044(15) 0.0081(17) C3 0.0309(19) 0.038(2) 0.030(2) 0.0063(17) 0.0004(15) 0.0062(16) C4 0.0214(16) 0.041(2) 0.029(2) 0.0039(16) 0.0021(15) 0.0049(15) C5 0.0210(16) 0.040(2) 0.0264(19) 0.0059(16) 0.0023(14) 0.0027(15) C6 0.0209(17) 0.040(2) 0.0268(19) 0.0027(16) 0.0043(14) 0.0039(15) C7 0.0301(19) 0.042(2) 0.027(2) -0.0008(17) 0.0013(15) 0.0069(16) C8 0.036(2) 0.044(2) 0.0232(19) 0.0029(17) 0.0016(15) 0.0123(17) C9 0.0247(16) 0.041(2) 0.0252(18) 0.0020(17) 0.0011(14) 0.0081(16) C10 0.0206(16) 0.042(2) 0.0261(18) 0.0050(17) 0.0008(13) 0.0061(16) C11 0.0234(17) 0.042(2) 0.0237(19) 0.0071(16) -0.0019(14) -0.0022(15) C12 0.0313(19) 0.037(2) 0.030(2) 0.0123(17) -0.0046(16) -0.0056(16) C13 0.0309(19) 0.036(2) 0.034(2) 0.0063(17) -0.0069(16) -0.0064(16) C14 0.0223(17) 0.037(2) 0.033(2) 0.0076(17) -0.0010(15) -0.0037(15) C15 0.0200(16) 0.038(2) 0.0285(19) 0.0025(16) -0.0016(15) -0.0006(15) C16 0.0232(18) 0.050(2) 0.0246(19) 0.0021(17) -0.0009(14) -0.0010(16) C17 0.0249(18) 0.050(3) 0.029(2) -0.0002(18) -0.0029(15) 0.0006(17) C18 0.0227(16) 0.048(2) 0.0233(19) 0.0047(16) 0.0003(13) 0.0035(16) C19 0.0216(16) 0.043(2) 0.0242(19) 0.0037(16) 0.0027(14) 0.0093(15) O20 0.0395(15) 0.0554(18) 0.0257(14) -0.0017(12) -0.0015(12) 0.0035(13) C20 0.031(2) 0.045(2) 0.030(2) 0.0016(17) -0.0012(16) -0.0005(17) O21 0.0278(14) 0.074(2) 0.0430(18) -0.0086(15) 0.0007(12) -0.0022(14) C21 0.058(3) 0.064(3) 0.034(2) -0.005(2) 0.009(2) 0.003(2) C22 0.0268(17) 0.0304(19) 0.0241(18) 0.0054(14) -0.0053(15) 0.0026(15) C23 0.0246(17) 0.043(2) 0.033(2) 0.0104(18) -0.0040(15) -0.0014(16) C24 0.031(2) 0.043(2) 0.042(2) 0.0105(18) -0.0096(17) -0.0036(17) C25 0.041(2) 0.035(2) 0.037(2) 0.0036(18) -0.0089(17) 0.0019(18) C26 0.037(2) 0.035(2) 0.034(2) 0.0030(17) 0.0019(16) 0.0058(17) C27 0.0318(19) 0.033(2) 0.031(2) 0.0088(16) 0.0022(16) 0.0033(16) C28 0.0343(19) 0.035(2) 0.029(2) 0.0056(16) 0.0012(16) 0.0092(16) C29 0.040(2) 0.044(2) 0.034(2) 0.0057(18) -0.0101(17) 0.0047(18) C30 0.065(3) 0.039(2) 0.037(2) 0.0031(19) -0.016(2) 0.010(2) C31 0.082(3) 0.048(3) 0.027(2) 0.0076(19) 0.002(2) 0.021(2) C32 0.059(3) 0.057(3) 0.037(3) 0.015(2) 0.017(2) 0.013(2) C33 0.038(2) 0.055(3) 0.034(2) 0.013(2) 0.0039(18) 0.0095(19) C34 0.0270(18) 0.039(2) 0.0249(18) 0.0026(15) 0.0004(15) -0.0017(16) C35 0.034(2) 0.045(3) 0.064(3) -0.006(2) -0.011(2) -0.0031(19) C36 0.038(2) 0.049(3) 0.069(3) -0.001(2) -0.006(2) 0.0033(19) C37 0.054(3) 0.049(3) 0.036(2) -0.007(2) 0.0011(19) -0.002(2) C38 0.039(2) 0.087(4) 0.052(3) -0.036(3) -0.010(2) 0.001(2) C39 0.027(2) 0.092(4) 0.047(3) -0.036(3) -0.0058(18) 0.011(2) C40 0.0232(17) 0.048(2) 0.026(2) 0.0085(17) 0.0046(14) 0.0145(16) C41 0.0300(19) 0.054(3) 0.026(2) 0.0065(18) 0.0035(15) 0.0158(18) C42 0.034(2) 0.072(3) 0.029(2) 0.002(2) -0.0015(17) 0.020(2) C43 0.037(2) 0.085(4) 0.028(2) 0.019(2) 0.0069(18) 0.019(2) C44 0.036(2) 0.069(3) 0.041(2) 0.026(2) 0.0160(19) 0.015(2) C45 0.0298(19) 0.051(3) 0.030(2) 0.0088(18) 0.0051(16) 0.0126(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N4 1.889(3) . ? Cu1 N2 1.923(3) . ? Cu1 N1 2.000(3) . ? Cu1 N3 2.000(3) . ? N1 C1 1.364(4) . ? N1 C4 1.391(5) . ? N2 C6 1.373(5) . ? N2 C9 1.382(4) . ? N3 C14 1.378(5) . ? N3 C11 1.397(4) . ? N4 C18 1.373(4) . ? N4 C16 1.375(5) . ? C1 C19 1.439(5) . ? C1 C2 1.439(5) . ? C2 C3 1.341(5) . ? C2 H2A 0.9500 . ? C3 C4 1.440(5) . ? C3 H3A 0.9500 . ? C4 C5 1.390(5) . ? C5 C6 1.424(5) . ? C5 C22 1.489(5) . ? C6 C7 1.426(5) . ? C7 C8 1.357(5) . ? C7 H7A 0.9500 . ? C8 C9 1.422(5) . ? C8 H8A 0.9500 . ? C9 C10 1.419(5) . ? C10 C11 1.392(5) . ? C10 C28 1.494(5) . ? C11 C12 1.427(5) . ? C12 C13 1.353(5) . ? C12 H12A 0.9500 . ? C13 C14 1.431(5) . ? C13 H13A 0.9500 . ? C14 C15 1.425(5) . ? C15 C16 1.371(5) . ? C15 C34 1.483(5) . ? C16 C17 1.532(5) . ? C16 C18 2.002(6) . ? C17 C20 1.498(5) . ? C17 C18 1.552(5) . ? C17 H17A 1.0000 . ? C18 C19 1.379(5) . ? C19 C40 1.488(5) . ? O20 C20 1.347(4) . ? O20 C21 1.448(5) . ? C20 O21 1.196(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C27 1.397(5) . ? C22 C23 1.398(5) . ? C23 C24 1.384(6) . ? C23 H23A 0.9500 . ? C24 C25 1.390(5) . ? C24 H24A 0.9500 . ? C25 C26 1.383(5) . ? C25 H25A 0.9500 . ? C26 C27 1.387(5) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C29 1.392(5) . ? C28 C33 1.397(5) . ? C29 C30 1.388(5) . ? C29 H29A 0.9500 . ? C30 C31 1.381(6) . ? C30 H30A 0.9500 . ? C31 C32 1.386(6) . ? C31 H31A 0.9500 . ? C32 C33 1.390(6) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 C39 1.381(5) . ? C34 C35 1.386(5) . ? C35 C36 1.383(6) . ? C35 H35A 0.9500 . ? C36 C37 1.391(6) . ? C36 H36A 0.9500 . ? C37 C38 1.376(6) . ? C37 H37A 0.9500 . ? C38 C39 1.386(6) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 C41 1.391(5) . ? C40 C45 1.402(5) . ? C41 C42 1.390(5) . ? C41 H41A 0.9500 . ? C42 C43 1.384(6) . ? C42 H42A 0.9500 . ? C43 C44 1.386(6) . ? C43 H43A 0.9500 . ? C44 C45 1.386(5) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? 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 N4 Cu1 N2 178.74(13) . . ? N4 Cu1 N1 87.01(13) . . ? N2 Cu1 N1 93.60(12) . . ? N4 Cu1 N3 86.82(12) . . ? N2 Cu1 N3 92.64(12) . . ? N1 Cu1 N3 172.93(12) . . ? C1 N1 C4 105.9(3) . . ? C1 N1 Cu1 129.5(3) . . ? C4 N1 Cu1 124.2(2) . . ? C6 N2 C9 105.8(3) . . ? C6 N2 Cu1 126.3(2) . . ? C9 N2 Cu1 127.9(3) . . ? C14 N3 C11 105.7(3) . . ? C14 N3 Cu1 129.2(2) . . ? C11 N3 Cu1 125.0(2) . . ? C18 N4 C16 93.5(3) . . ? C18 N4 Cu1 133.0(3) . . ? C16 N4 Cu1 132.3(2) . . ? N1 C1 C19 124.9(3) . . ? N1 C1 C2 110.1(3) . . ? C19 C1 C2 125.0(3) . . ? C3 C2 C1 107.5(3) . . ? C3 C2 H2A 126.2 . . ? C1 C2 H2A 126.2 . . ? C2 C3 C4 107.2(3) . . ? C2 C3 H3A 126.4 . . ? C4 C3 H3A 126.4 . . ? C5 C4 N1 125.3(3) . . ? C5 C4 C3 125.3(4) . . ? N1 C4 C3 109.4(3) . . ? C4 C5 C6 124.2(3) . . ? C4 C5 C22 119.5(3) . . ? C6 C5 C22 116.2(3) . . ? N2 C6 C5 125.5(3) . . ? N2 C6 C7 109.9(3) . . ? C5 C6 C7 124.5(3) . . ? C8 C7 C6 107.2(3) . . ? C8 C7 H7A 126.4 . . ? C6 C7 H7A 126.4 . . ? C7 C8 C9 107.1(3) . . ? C7 C8 H8A 126.4 . . ? C9 C8 H8A 126.4 . . ? N2 C9 C10 124.0(3) . . ? N2 C9 C8 109.9(3) . . ? C10 C9 C8 126.1(3) . . ? C11 C10 C9 125.2(3) . . ? C11 C10 C28 118.6(3) . . ? C9 C10 C28 116.2(3) . . ? C10 C11 N3 124.6(3) . . ? C10 C11 C12 125.7(3) . . ? N3 C11 C12 109.4(3) . . ? C13 C12 C11 107.5(3) . . ? C13 C12 H12A 126.3 . . ? C11 C12 H12A 126.3 . . ? C12 C13 C14 107.5(3) . . ? C12 C13 H13A 126.3 . . ? C14 C13 H13A 126.3 . . ? N3 C14 C15 125.0(3) . . ? N3 C14 C13 109.9(3) . . ? C15 C14 C13 125.0(3) . . ? C16 C15 C14 119.0(3) . . ? C16 C15 C34 120.8(3) . . ? C14 C15 C34 120.2(3) . . ? C15 C16 N4 126.8(3) . . ? C15 C16 C17 140.0(4) . . ? N4 C16 C17 93.0(3) . . ? C15 C16 C18 168.6(3) . . ? N4 C16 C18 43.2(2) . . ? C17 C16 C18 50.0(2) . . ? C20 C17 C16 118.9(3) . . ? C20 C17 C18 116.7(3) . . ? C16 C17 C18 81.0(3) . . ? C20 C17 H17A 112.3 . . ? C16 C17 H17A 112.3 . . ? C18 C17 H17A 112.3 . . ? N4 C18 C19 125.9(3) . . ? N4 C18 C17 92.2(3) . . ? C19 C18 C17 141.6(3) . . ? N4 C18 C16 43.3(2) . . ? C19 C18 C16 167.2(3) . . ? C17 C18 C16 49.1(2) . . ? C18 C19 C1 119.2(3) . . ? C18 C19 C40 119.9(3) . . ? C1 C19 C40 120.9(3) . . ? C20 O20 C21 116.0(3) . . ? O21 C20 O20 124.2(4) . . ? O21 C20 C17 125.7(4) . . ? O20 C20 C17 110.0(3) . . ? O20 C21 H21A 109.5 . . ? O20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 118.2(3) . . ? C27 C22 C5 119.0(3) . . ? C23 C22 C5 122.8(3) . . ? C24 C23 C22 120.8(4) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 C25 120.2(4) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C26 C25 C24 119.8(4) . . ? C26 C25 H25A 120.1 . . ? C24 C25 H25A 120.1 . . ? C25 C26 C27 120.0(4) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C26 C27 C22 121.1(3) . . ? C26 C27 H27A 119.4 . . ? C22 C27 H27A 119.4 . . ? C29 C28 C33 118.7(3) . . ? C29 C28 C10 121.7(3) . . ? C33 C28 C10 119.6(3) . . ? C30 C29 C28 120.4(4) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C31 C30 C29 120.5(4) . . ? C31 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? C30 C31 C32 119.8(4) . . ? C30 C31 H31A 120.1 . . ? C32 C31 H31A 120.1 . . ? C31 C32 C33 120.0(4) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C32 C33 C28 120.5(4) . . ? C32 C33 H33A 119.7 . . ? C28 C33 H33A 119.7 . . ? C39 C34 C35 118.1(4) . . ? C39 C34 C15 121.0(3) . . ? C35 C34 C15 120.9(3) . . ? C36 C35 C34 121.1(4) . . ? C36 C35 H35A 119.4 . . ? C34 C35 H35A 119.4 . . ? C35 C36 C37 120.5(4) . . ? C35 C36 H36A 119.8 . . ? C37 C36 H36A 119.8 . . ? C38 C37 C36 118.3(4) . . ? C38 C37 H37A 120.8 . . ? C36 C37 H37A 120.8 . . ? C37 C38 C39 121.1(4) . . ? C37 C38 H38A 119.5 . . ? C39 C38 H38A 119.5 . . ? C34 C39 C38 120.9(4) . . ? C34 C39 H39A 119.5 . . ? C38 C39 H39A 119.5 . . ? C41 C40 C45 118.2(3) . . ? C41 C40 C19 120.6(3) . . ? C45 C40 C19 121.2(4) . . ? C42 C41 C40 121.4(4) . . ? C42 C41 H41A 119.3 . . ? C40 C41 H41A 119.3 . . ? C43 C42 C41 119.5(4) . . ? C43 C42 H42A 120.3 . . ? C41 C42 H42A 120.3 . . ? C42 C43 C44 120.2(4) . . ? C42 C43 H43A 119.9 . . ? C44 C43 H43A 119.9 . . ? C43 C44 C45 120.1(4) . . ? C43 C44 H44A 120.0 . . ? C45 C44 H44A 120.0 . . ? C44 C45 C40 120.6(4) . . ? C44 C45 H45A 119.7 . . ? C40 C45 H45A 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cu1 N1 C1 -0.3(3) . . . . ? N2 Cu1 N1 C1 178.6(3) . . . . ? N3 Cu1 N1 C1 -29.5(11) . . . . ? N4 Cu1 N1 C4 -171.7(3) . . . . ? N2 Cu1 N1 C4 7.2(3) . . . . ? N3 Cu1 N1 C4 159.1(8) . . . . ? N4 Cu1 N2 C6 118(6) . . . . ? N1 Cu1 N2 C6 -0.5(3) . . . . ? N3 Cu1 N2 C6 -177.2(3) . . . . ? N4 Cu1 N2 C9 -62(6) . . . . ? N1 Cu1 N2 C9 179.0(3) . . . . ? N3 Cu1 N2 C9 2.3(3) . . . . ? N4 Cu1 N3 C14 -8.0(3) . . . . ? N2 Cu1 N3 C14 173.2(3) . . . . ? N1 Cu1 N3 C14 21.3(11) . . . . ? N4 Cu1 N3 C11 172.6(3) . . . . ? N2 Cu1 N3 C11 -6.3(3) . . . . ? N1 Cu1 N3 C11 -158.2(8) . . . . ? N2 Cu1 N4 C18 -123(6) . . . . ? N1 Cu1 N4 C18 -4.1(3) . . . . ? N3 Cu1 N4 C18 172.4(3) . . . . ? N2 Cu1 N4 C16 73(6) . . . . ? N1 Cu1 N4 C16 -168.5(3) . . . . ? N3 Cu1 N4 C16 8.1(3) . . . . ? C4 N1 C1 C19 179.1(3) . . . . ? Cu1 N1 C1 C19 6.5(5) . . . . ? C4 N1 C1 C2 0.3(4) . . . . ? Cu1 N1 C1 C2 -172.3(2) . . . . ? N1 C1 C2 C3 0.0(4) . . . . ? C19 C1 C2 C3 -178.8(3) . . . . ? C1 C2 C3 C4 -0.3(4) . . . . ? C1 N1 C4 C5 179.6(3) . . . . ? Cu1 N1 C4 C5 -7.3(5) . . . . ? C1 N1 C4 C3 -0.5(4) . . . . ? Cu1 N1 C4 C3 172.6(2) . . . . ? C2 C3 C4 C5 -179.6(3) . . . . ? C2 C3 C4 N1 0.5(4) . . . . ? N1 C4 C5 C6 -1.4(6) . . . . ? C3 C4 C5 C6 178.8(3) . . . . ? N1 C4 C5 C22 175.0(3) . . . . ? C3 C4 C5 C22 -4.8(5) . . . . ? C9 N2 C6 C5 173.4(3) . . . . ? Cu1 N2 C6 C5 -7.0(5) . . . . ? C9 N2 C6 C7 -3.3(4) . . . . ? Cu1 N2 C6 C7 176.3(2) . . . . ? C4 C5 C6 N2 9.2(5) . . . . ? C22 C5 C6 N2 -167.3(3) . . . . ? C4 C5 C6 C7 -174.6(3) . . . . ? C22 C5 C6 C7 8.8(5) . . . . ? N2 C6 C7 C8 3.1(4) . . . . ? C5 C6 C7 C8 -173.6(3) . . . . ? C6 C7 C8 C9 -1.6(4) . . . . ? C6 N2 C9 C10 -176.6(3) . . . . ? Cu1 N2 C9 C10 3.8(5) . . . . ? C6 N2 C9 C8 2.3(4) . . . . ? Cu1 N2 C9 C8 -177.3(2) . . . . ? C7 C8 C9 N2 -0.4(4) . . . . ? C7 C8 C9 C10 178.5(3) . . . . ? N2 C9 C10 C11 -7.7(5) . . . . ? C8 C9 C10 C11 173.6(3) . . . . ? N2 C9 C10 C28 171.0(3) . . . . ? C8 C9 C10 C28 -7.7(5) . . . . ? C9 C10 C11 N3 3.1(5) . . . . ? C28 C10 C11 N3 -175.6(3) . . . . ? C9 C10 C11 C12 -170.6(3) . . . . ? C28 C10 C11 C12 10.7(5) . . . . ? C14 N3 C11 C10 -174.9(3) . . . . ? Cu1 N3 C11 C10 4.7(5) . . . . ? C14 N3 C11 C12 -0.2(4) . . . . ? Cu1 N3 C11 C12 179.3(2) . . . . ? C10 C11 C12 C13 174.2(3) . . . . ? N3 C11 C12 C13 -0.3(4) . . . . ? C11 C12 C13 C14 0.8(4) . . . . ? C11 N3 C14 C15 -176.5(3) . . . . ? Cu1 N3 C14 C15 3.9(5) . . . . ? C11 N3 C14 C13 0.7(4) . . . . ? Cu1 N3 C14 C13 -178.8(2) . . . . ? C12 C13 C14 N3 -1.0(4) . . . . ? C12 C13 C14 C15 176.3(3) . . . . ? N3 C14 C15 C16 3.7(5) . . . . ? C13 C14 C15 C16 -173.2(3) . . . . ? N3 C14 C15 C34 -176.9(3) . . . . ? C13 C14 C15 C34 6.3(5) . . . . ? C14 C15 C16 N4 -4.0(5) . . . . ? C34 C15 C16 N4 176.5(3) . . . . ? C14 C15 C16 C17 -178.9(4) . . . . ? C34 C15 C16 C17 1.6(7) . . . . ? C14 C15 C16 C18 -30.8(17) . . . . ? C34 C15 C16 C18 149.7(14) . . . . ? C18 N4 C16 C15 -172.5(4) . . . . ? Cu1 N4 C16 C15 -3.9(6) . . . . ? C18 N4 C16 C17 4.2(3) . . . . ? Cu1 N4 C16 C17 172.9(3) . . . . ? Cu1 N4 C16 C18 168.6(4) . . . . ? C15 C16 C17 C20 56.5(6) . . . . ? N4 C16 C17 C20 -119.4(4) . . . . ? C18 C16 C17 C20 -115.6(4) . . . . ? C15 C16 C17 C18 172.1(5) . . . . ? N4 C16 C17 C18 -3.8(2) . . . . ? C16 N4 C18 C19 170.9(3) . . . . ? Cu1 N4 C18 C19 2.4(5) . . . . ? C16 N4 C18 C17 -4.2(3) . . . . ? Cu1 N4 C18 C17 -172.7(3) . . . . ? Cu1 N4 C18 C16 -168.5(4) . . . . ? C20 C17 C18 N4 121.7(3) . . . . ? C16 C17 C18 N4 3.8(2) . . . . ? C20 C17 C18 C19 -51.9(6) . . . . ? C16 C17 C18 C19 -169.8(5) . . . . ? C20 C17 C18 C16 117.9(4) . . . . ? C15 C16 C18 N4 31.9(15) . . . . ? C17 C16 C18 N4 -174.5(4) . . . . ? C15 C16 C18 C19 -4(3) . . . . ? N4 C16 C18 C19 -35.4(13) . . . . ? C17 C16 C18 C19 150.1(14) . . . . ? C15 C16 C18 C17 -153.7(16) . . . . ? N4 C16 C18 C17 174.5(4) . . . . ? N4 C18 C19 C1 4.8(5) . . . . ? C17 C18 C19 C1 176.9(4) . . . . ? C16 C18 C19 C1 34.1(15) . . . . ? N4 C18 C19 C40 -173.6(3) . . . . ? C17 C18 C19 C40 -1.5(7) . . . . ? C16 C18 C19 C40 -144.2(12) . . . . ? N1 C1 C19 C18 -9.1(5) . . . . ? C2 C1 C19 C18 169.6(3) . . . . ? N1 C1 C19 C40 169.3(3) . . . . ? C2 C1 C19 C40 -12.1(5) . . . . ? C21 O20 C20 O21 6.3(6) . . . . ? C21 O20 C20 C17 -172.2(3) . . . . ? C16 C17 C20 O21 31.3(6) . . . . ? C18 C17 C20 O21 -63.2(5) . . . . ? C16 C17 C20 O20 -150.3(3) . . . . ? C18 C17 C20 O20 115.2(4) . . . . ? C4 C5 C22 C27 -114.3(4) . . . . ? C6 C5 C22 C27 62.5(4) . . . . ? C4 C5 C22 C23 65.7(5) . . . . ? C6 C5 C22 C23 -117.5(4) . . . . ? C27 C22 C23 C24 -1.6(5) . . . . ? C5 C22 C23 C24 178.4(3) . . . . ? C22 C23 C24 C25 1.4(5) . . . . ? C23 C24 C25 C26 -0.6(6) . . . . ? C24 C25 C26 C27 0.0(6) . . . . ? C25 C26 C27 C22 -0.3(5) . . . . ? C23 C22 C27 C26 1.1(5) . . . . ? C5 C22 C27 C26 -178.9(3) . . . . ? C11 C10 C28 C29 -109.7(4) . . . . ? C9 C10 C28 C29 71.5(5) . . . . ? C11 C10 C28 C33 71.3(5) . . . . ? C9 C10 C28 C33 -107.5(4) . . . . ? C33 C28 C29 C30 3.2(6) . . . . ? C10 C28 C29 C30 -175.8(4) . . . . ? C28 C29 C30 C31 -1.9(6) . . . . ? C29 C30 C31 C32 -0.2(7) . . . . ? C30 C31 C32 C33 0.9(7) . . . . ? C31 C32 C33 C28 0.4(7) . . . . ? C29 C28 C33 C32 -2.5(6) . . . . ? C10 C28 C33 C32 176.5(4) . . . . ? C16 C15 C34 C39 58.7(5) . . . . ? C14 C15 C34 C39 -120.8(4) . . . . ? C16 C15 C34 C35 -122.9(4) . . . . ? C14 C15 C34 C35 57.7(5) . . . . ? C39 C34 C35 C36 -0.3(7) . . . . ? C15 C34 C35 C36 -178.9(4) . . . . ? C34 C35 C36 C37 0.5(7) . . . . ? C35 C36 C37 C38 0.1(7) . . . . ? C36 C37 C38 C39 -0.8(7) . . . . ? C35 C34 C39 C38 -0.4(7) . . . . ? C15 C34 C39 C38 178.2(4) . . . . ? C37 C38 C39 C34 0.9(8) . . . . ? C18 C19 C40 C41 -39.3(5) . . . . ? C1 C19 C40 C41 142.4(3) . . . . ? C18 C19 C40 C45 139.3(4) . . . . ? C1 C19 C40 C45 -39.0(5) . . . . ? C45 C40 C41 C42 0.7(5) . . . . ? C19 C40 C41 C42 179.3(3) . . . . ? C40 C41 C42 C43 2.1(6) . . . . ? C41 C42 C43 C44 -2.7(6) . . . . ? C42 C43 C44 C45 0.5(6) . . . . ? C43 C44 C45 C40 2.4(6) . . . . ? C41 C40 C45 C44 -3.0(5) . . . . ? C19 C40 C45 C44 178.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.306 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.070 # Attachment '05168.cif' data_05168 _database_code_depnum_ccdc_archive 'CCDC 605758' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H52 N8 Ni2 O2, 3(C H2 Cl2)' _chemical_formula_sum 'C91 H58 Cl6 N8 Ni2 O2' _chemical_formula_weight 1625.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.111(4) _cell_length_b 14.986(4) _cell_length_c 27.852(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.635(5) _cell_angle_gamma 90.00 _cell_volume 7376(3) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2367 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 22.1 _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 0.787 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9254 _exptl_absorpt_correction_T_max 0.9844 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 50 seconds each' _diffrn_measurement_method \w-scans _diffrn_measurement_device 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49219 _diffrn_reflns_av_R_equivalents 0.1224 _diffrn_reflns_av_sigmaI/netI 0.1125 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.15 _reflns_number_total 13121 _reflns_number_gt 7141 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SIR-92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2003), XTEL (loc. libr.)' _computing_publication_material 'SHELXTL (Bruker, 2003)' _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. The data are weak and R(int) is somewhat large due to the small crystal size. ; _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^)+(0.1018P)^2^+19.2797P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13121 _refine_ls_number_parameters 992 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1465 _refine_ls_R_factor_gt 0.0715 _refine_ls_wR_factor_ref 0.2276 _refine_ls_wR_factor_gt 0.1805 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.012 _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 Ni1A Ni 0.82593(4) 0.80725(5) 0.53432(3) 0.0229(2) Uani 1 1 d . . . O1A O 0.9278(2) 0.8137(3) 0.36964(16) 0.0329(11) Uani 1 1 d . . . N1A N 0.8962(3) 0.8792(3) 0.57824(19) 0.0259(12) Uani 1 1 d . . . N2A N 0.7680(3) 0.7926(3) 0.58279(19) 0.0267(12) Uani 1 1 d . . . N3A N 0.7541(3) 0.7388(3) 0.48999(19) 0.0249(12) Uani 1 1 d . . . N4A N 0.8861(3) 0.8158(3) 0.48664(18) 0.0230(11) Uani 1 1 d . . . C1A C 0.9684(3) 0.9021(4) 0.5745(2) 0.0269(14) Uani 1 1 d . . . C2A C 0.9981(4) 0.9694(4) 0.6096(2) 0.0297(15) Uani 1 1 d . . . H2AA H 1.0469 0.9957 0.6144 0.036 Uiso 1 1 calc R . . C3A C 0.9444(4) 0.9887(5) 0.6345(2) 0.0344(16) Uani 1 1 d . . . H3AA H 0.9475 1.0331 0.6592 0.041 Uiso 1 1 calc R . . C4A C 0.8817(3) 0.9303(4) 0.6170(2) 0.0270(14) Uani 1 1 d . . . C5A C 0.8218(3) 0.9154(4) 0.6386(2) 0.0285(15) Uani 1 1 d . . . C6A C 0.7715(3) 0.8437(4) 0.6249(2) 0.0295(15) Uani 1 1 d . . . C7A C 0.7233(4) 0.8061(5) 0.6535(2) 0.0334(16) Uani 1 1 d . . . H7AA H 0.7146 0.8293 0.6835 0.040 Uiso 1 1 calc R . . C8A C 0.6925(4) 0.7320(5) 0.6304(2) 0.0319(16) Uani 1 1 d . . . H8AA H 0.6592 0.6922 0.6417 0.038 Uiso 1 1 calc R . . C9A C 0.7187(3) 0.7238(4) 0.5861(2) 0.0275(14) Uani 1 1 d . . . C10A C 0.6900(3) 0.6646(4) 0.5475(2) 0.0292(15) Uani 1 1 d . . . C11A C 0.7026(3) 0.6778(4) 0.5010(2) 0.0276(14) Uani 1 1 d . . . C12A C 0.6578(4) 0.6402(5) 0.4570(3) 0.0380(17) Uani 1 1 d . . . H12A H 0.6207 0.5947 0.4547 0.046 Uiso 1 1 calc R . . C13A C 0.6788(4) 0.6827(5) 0.4192(3) 0.0386(17) Uani 1 1 d . . . H13A H 0.6565 0.6756 0.3853 0.046 Uiso 1 1 calc R . . C14A C 0.7405(3) 0.7399(5) 0.4396(2) 0.0283(15) Uani 1 1 d . . . C15A C 0.7894(3) 0.7795(4) 0.4130(2) 0.0267(14) Uani 1 1 d . . . C16A C 0.8613(3) 0.8051(4) 0.4368(2) 0.0220(13) Uani 1 1 d . . . C17A C 0.9267(3) 0.8072(4) 0.4128(2) 0.0251(13) Uani 1 1 d . . . C18A C 0.9957(3) 0.7951(4) 0.4552(2) 0.0250(14) Uani 1 1 d . . . H18A H 1.0389 0.8335 0.4509 0.030 Uiso 1 1 calc R . . C19A C 0.9636(3) 0.8254(4) 0.4973(2) 0.0241(14) Uani 1 1 d . . . C20A C 1.0054(3) 0.8670(4) 0.5390(2) 0.0242(14) Uani 1 1 d . . . C21A C 0.8124(4) 0.9678(5) 0.6835(3) 0.0350(16) Uani 1 1 d . . . C22A C 0.8641(4) 0.9568(6) 0.7282(3) 0.052(2) Uani 1 1 d . . . H22A H 0.9070 0.9196 0.7300 0.062 Uiso 1 1 calc R . . C23A C 0.8528(5) 1.0001(7) 0.7699(3) 0.062(3) Uani 1 1 d . . . H23A H 0.8880 0.9927 0.8004 0.075 Uiso 1 1 calc R . . C24A C 0.7906(5) 1.0538(7) 0.7670(3) 0.064(3) Uani 1 1 d . . . H24A H 0.7833 1.0841 0.7955 0.077 Uiso 1 1 calc R . . C25A C 0.7383(5) 1.0645(5) 0.7230(3) 0.051(2) Uani 1 1 d . . . H25A H 0.6952 1.1014 0.7214 0.062 Uiso 1 1 calc R . . C26A C 0.7495(4) 1.0210(5) 0.6813(3) 0.0394(17) Uani 1 1 d . . . H26A H 0.7137 1.0278 0.6510 0.047 Uiso 1 1 calc R . . C27A C 0.6395(3) 0.5897(4) 0.5572(2) 0.0287(15) Uani 1 1 d . . . C28A C 0.5635(4) 0.5969(5) 0.5476(4) 0.060(3) Uani 1 1 d . . . H28A H 0.5403 0.6499 0.5328 0.072 Uiso 1 1 calc R . . C29A C 0.5181(4) 0.5283(6) 0.5590(4) 0.070(3) Uani 1 1 d . . . H29A H 0.4647 0.5355 0.5523 0.083 Uiso 1 1 calc R . . C30A C 0.5497(4) 0.4517(5) 0.5794(3) 0.0413(18) Uani 1 1 d . . . H30A H 0.5187 0.4042 0.5862 0.050 Uiso 1 1 calc R . . C31A C 0.6253(5) 0.4435(6) 0.5898(4) 0.067(3) Uani 1 1 d . . . H31A H 0.6480 0.3902 0.6047 0.081 Uiso 1 1 calc R . . C32A C 0.6707(5) 0.5126(6) 0.5791(4) 0.075(3) Uani 1 1 d . . . H32A H 0.7242 0.5061 0.5872 0.091 Uiso 1 1 calc R . . C33A C 0.7654(4) 0.7832(5) 0.3581(2) 0.0354(17) Uani 1 1 d . . . C34A C 0.7431(4) 0.8640(6) 0.3354(3) 0.055(2) Uani 1 1 d . . . H34A H 0.7468 0.9175 0.3541 0.065 Uiso 1 1 calc R . . C35A C 0.7150(5) 0.8656(9) 0.2845(4) 0.077(3) Uani 1 1 d . . . H35A H 0.6989 0.9207 0.2687 0.093 Uiso 1 1 calc R . . C36A C 0.7102(5) 0.7895(10) 0.2568(4) 0.080(4) Uani 1 1 d . . . H36A H 0.6916 0.7921 0.2222 0.096 Uiso 1 1 calc R . . C37A C 0.7321(5) 0.7099(8) 0.2792(3) 0.073(3) Uani 1 1 d . . . H37A H 0.7295 0.6566 0.2604 0.088 Uiso 1 1 calc R . . C38A C 0.7585(5) 0.7082(6) 0.3301(3) 0.051(2) Uani 1 1 d . . . H38A H 0.7723 0.6525 0.3457 0.062 Uiso 1 1 calc R . . C39A C 1.0892(4) 0.8838(4) 0.5463(3) 0.0338(16) Uani 1 1 d . . . C40A C 1.1195(4) 0.9357(5) 0.5148(3) 0.0433(19) Uani 1 1 d . . . H40A H 1.0864 0.9603 0.4867 0.052 Uiso 1 1 calc R . . C41A C 1.1957(4) 0.9535(5) 0.5223(3) 0.0452(19) Uani 1 1 d . . . H41A H 1.2147 0.9891 0.4995 0.054 Uiso 1 1 calc R . . C42A C 1.2448(4) 0.9183(5) 0.5641(3) 0.049(2) Uani 1 1 d . . . H42A H 1.2975 0.9302 0.5698 0.059 Uiso 1 1 calc R . . C43A C 1.2159(4) 0.8658(5) 0.5972(3) 0.047(2) Uani 1 1 d . . . H43A H 1.2488 0.8416 0.6255 0.056 Uiso 1 1 calc R . . C44A C 1.1384(4) 0.8493(5) 0.5882(3) 0.0374(17) Uani 1 1 d . . . H44A H 1.1185 0.8142 0.6109 0.045 Uiso 1 1 calc R . . Ni1B Ni 1.25220(4) 0.69089(6) 0.52717(3) 0.0263(2) Uani 1 1 d . . . O1B O 1.0196(2) 0.6364(3) 0.37851(17) 0.0351(11) Uani 1 1 d . . . N1B N 1.2120(3) 0.6359(4) 0.57944(19) 0.0283(12) Uani 1 1 d . . . N2B N 1.3503(3) 0.6971(4) 0.5694(2) 0.0338(13) Uani 1 1 d . . . N3B N 1.2910(3) 0.7393(4) 0.4736(2) 0.0307(13) Uani 1 1 d . . . N4B N 1.1548(3) 0.6904(3) 0.48469(19) 0.0251(11) Uani 1 1 d . . . C1B C 1.1369(4) 0.6179(4) 0.5806(2) 0.0298(15) Uani 1 1 d . . . C2B C 1.1333(4) 0.5644(5) 0.6222(2) 0.0330(16) Uani 1 1 d . . . H2BA H 1.0888 0.5435 0.6314 0.040 Uiso 1 1 calc R . . C3B C 1.2053(4) 0.5492(5) 0.6460(2) 0.0350(16) Uani 1 1 d . . . H3BA H 1.2207 0.5144 0.6750 0.042 Uiso 1 1 calc R . . C4B C 1.2539(4) 0.5935(5) 0.6207(2) 0.0316(15) Uani 1 1 d . . . C5B C 1.3322(4) 0.5997(5) 0.6372(2) 0.0346(16) Uani 1 1 d . . . C6B C 1.3745(4) 0.6540(5) 0.6140(3) 0.0383(17) Uani 1 1 d . . . C7B C 1.4518(4) 0.6780(6) 0.6349(3) 0.052(2) Uani 1 1 d . . . H7BA H 1.4823 0.6556 0.6646 0.063 Uiso 1 1 calc R . . C8B C 1.4730(4) 0.7387(6) 0.6044(3) 0.050(2) Uani 1 1 d . . . H8BA H 1.5205 0.7683 0.6094 0.061 Uiso 1 1 calc R . . C9B C 1.4107(4) 0.7498(5) 0.5630(3) 0.0378(17) Uani 1 1 d . . . C10B C 1.4162(4) 0.7924(4) 0.5196(3) 0.0330(16) Uani 1 1 d . . . C11B C 1.3602(3) 0.7833(4) 0.4768(3) 0.0313(16) Uani 1 1 d . . . C12B C 1.3665(4) 0.8116(5) 0.4290(3) 0.0358(16) Uani 1 1 d . . . H12B H 1.4071 0.8445 0.4212 0.043 Uiso 1 1 calc R . . C13B C 1.3046(4) 0.7831(4) 0.3973(3) 0.0346(16) Uani 1 1 d . . . H13B H 1.2940 0.7903 0.3626 0.042 Uiso 1 1 calc R . . C14B C 1.2575(4) 0.7400(4) 0.4249(2) 0.0283(15) Uani 1 1 d . . . C15B C 1.1829(3) 0.7095(4) 0.4040(2) 0.0254(14) Uani 1 1 d . . . C16B C 1.1356(3) 0.6903(4) 0.4339(2) 0.0239(13) Uani 1 1 d . . . C17B C 1.0525(3) 0.6676(4) 0.4173(2) 0.0272(14) Uani 1 1 d . . . C18B C 1.0195(3) 0.6922(4) 0.4615(2) 0.0255(13) Uani 1 1 d . . . C19B C 1.0895(3) 0.6830(4) 0.5011(2) 0.0224(13) Uani 1 1 d . . . C20B C 1.0770(3) 0.6450(4) 0.5435(2) 0.0257(14) Uani 1 1 d . . . C21B C 1.3689(4) 0.5471(5) 0.6812(3) 0.0381(17) Uani 1 1 d . . . C22B C 1.3612(4) 0.5707(7) 0.7281(3) 0.055(2) Uani 1 1 d . . . H22B H 1.3354 0.6241 0.7328 0.067 Uiso 1 1 calc R . . C23B C 1.3906(4) 0.5174(6) 0.7679(3) 0.055(2) Uani 1 1 d . . . H23B H 1.3856 0.5349 0.7998 0.066 Uiso 1 1 calc R . . C24B C 1.4269(4) 0.4395(6) 0.7620(3) 0.050(2) Uani 1 1 d . . . H24B H 1.4445 0.4014 0.7894 0.061 Uiso 1 1 calc R . . C25B C 1.4377(4) 0.4170(6) 0.7164(3) 0.056(2) Uani 1 1 d . . . H25B H 1.4645 0.3640 0.7124 0.067 Uiso 1 1 calc R . . C26B C 1.4098(4) 0.4712(5) 0.6758(3) 0.0426(18) Uani 1 1 d . . . H26B H 1.4188 0.4560 0.6445 0.051 Uiso 1 1 calc R . . C27B C 1.4854(4) 0.8457(5) 0.5209(3) 0.0400(18) Uani 1 1 d . . . C28B C 1.5048(4) 0.9147(5) 0.5553(3) 0.049(2) Uani 1 1 d . . . H28B H 1.4716 0.9297 0.5762 0.058 Uiso 1 1 calc R . . C29B C 1.5717(5) 0.9611(6) 0.5592(4) 0.062(3) Uani 1 1 d . . . H29B H 1.5846 1.0068 0.5832 0.075 Uiso 1 1 calc R . . C30B C 1.6195(4) 0.9419(6) 0.5289(4) 0.062(3) Uani 1 1 d . . . H30B H 1.6654 0.9743 0.5319 0.075 Uiso 1 1 calc R . . C31B C 1.6017(4) 0.8768(6) 0.4946(4) 0.060(3) Uani 1 1 d . . . H31B H 1.6348 0.8648 0.4732 0.073 Uiso 1 1 calc R . . C32B C 1.5350(4) 0.8268(5) 0.4902(3) 0.050(2) Uani 1 1 d . . . H32B H 1.5236 0.7804 0.4664 0.060 Uiso 1 1 calc R . . C33B C 1.1569(3) 0.7104(4) 0.3496(2) 0.0284(15) Uani 1 1 d . . . C34B C 1.1786(4) 0.6442(5) 0.3204(3) 0.0393(17) Uani 1 1 d . . . H34B H 1.2105 0.5970 0.3352 0.047 Uiso 1 1 calc R . . C35B C 1.1538(4) 0.6470(5) 0.2699(3) 0.0442(19) Uani 1 1 d . . . H35B H 1.1691 0.6016 0.2503 0.053 Uiso 1 1 calc R . . C36B C 1.1075(4) 0.7138(6) 0.2477(3) 0.045(2) Uani 1 1 d . . . H36B H 1.0900 0.7143 0.2129 0.054 Uiso 1 1 calc R . . C37B C 1.0864(5) 0.7802(6) 0.2757(3) 0.051(2) Uani 1 1 d . . . H37B H 1.0547 0.8274 0.2604 0.061 Uiso 1 1 calc R . . C38B C 1.1117(4) 0.7782(5) 0.3267(3) 0.0431(19) Uani 1 1 d . . . H38B H 1.0973 0.8247 0.3460 0.052 Uiso 1 1 calc R . . C39B C 0.9957(4) 0.6164(4) 0.5325(3) 0.0342(16) Uani 1 1 d . . . C40B C 0.9523(4) 0.5699(5) 0.5587(3) 0.0357(16) Uani 1 1 d . . . H40B H 0.9720 0.5566 0.5924 0.043 Uiso 1 1 calc R . . C41B C 0.8809(4) 0.5425(4) 0.5365(3) 0.0319(16) Uani 1 1 d . . . H41B H 0.8506 0.5135 0.5557 0.038 Uiso 1 1 calc R . . C42B C 0.8517(4) 0.5561(5) 0.4869(3) 0.0389(17) Uani 1 1 d . . . H42B H 0.8033 0.5329 0.4720 0.047 Uiso 1 1 calc R . . C43B C 0.8930(4) 0.6038(4) 0.4586(3) 0.0336(16) Uani 1 1 d . . . H43B H 0.8731 0.6146 0.4246 0.040 Uiso 1 1 calc R . . C44B C 0.9640(4) 0.6348(4) 0.4817(2) 0.0312(15) Uani 1 1 d . . . Cl1 Cl 1.11181(14) 0.41903(18) 0.32290(9) 0.0714(7) Uani 1 1 d . . . Cl2 Cl 0.99247(14) 0.28695(17) 0.31863(10) 0.0695(7) Uani 1 1 d . . . C1S C 1.0908(5) 0.3089(6) 0.3389(4) 0.062(2) Uani 1 1 d . . . H1S1 H 1.1059 0.3013 0.3750 0.074 Uiso 1 1 calc R . . H1S2 H 1.1200 0.2657 0.3235 0.074 Uiso 1 1 calc R . . Cl3 Cl 0.8970(2) 0.6880(3) 0.21312(11) 0.1107(11) Uani 1 1 d . . . Cl4 Cl 0.9151(3) 0.5354(2) 0.27713(12) 0.1268(15) Uani 1 1 d . . . C2S C 0.9200(9) 0.6465(7) 0.2731(3) 0.109(5) Uani 1 1 d . . . H2S1 H 0.9720 0.6658 0.2887 0.131 Uiso 1 1 calc R . . H2S2 H 0.8853 0.6734 0.2921 0.131 Uiso 1 1 calc R . . Cl5 Cl 1.0595(3) 0.2807(3) 0.1952(2) 0.1119(17) Uani 0.782(4) 1 d PD A 1 Cl6 Cl 0.9519(3) 0.3995(5) 0.1342(2) 0.171(3) Uani 0.782(4) 1 d PD A 1 C3S C 0.9769(17) 0.3533(14) 0.1911(10) 0.121(8) Uani 0.782(4) 1 d PD A 1 H3S1 H 0.9340 0.3181 0.1979 0.146 Uiso 0.782(4) 1 calc PR A 1 H3S2 H 0.9889 0.4011 0.2161 0.146 Uiso 0.782(4) 1 calc PR A 1 Cl5D Cl 1.0168(11) 0.2841(12) 0.1571(8) 0.1119(17) Uani 0.218(4) 1 d PD A 2 Cl6D Cl 1.0212(12) 0.4837(16) 0.1718(7) 0.171(3) Uani 0.218(4) 1 d PD A 2 C3D C 0.995(9) 0.3829(19) 0.191(4) 0.121(8) Uani 0.218(4) 1 d PD A 2 H3D1 H 0.9397 0.3842 0.1886 0.146 Uiso 0.218(4) 1 calc PR A 2 H3D2 H 1.0198 0.3754 0.2259 0.146 Uiso 0.218(4) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1A 0.0183(4) 0.0251(4) 0.0257(4) -0.0014(4) 0.0057(3) -0.0001(3) O1A 0.030(2) 0.044(3) 0.025(3) 0.006(2) 0.0061(19) -0.002(2) N1A 0.018(3) 0.026(3) 0.035(3) -0.003(2) 0.009(2) -0.001(2) N2A 0.022(3) 0.029(3) 0.030(3) -0.002(2) 0.007(2) 0.000(2) N3A 0.020(3) 0.026(3) 0.030(3) 0.000(2) 0.009(2) 0.000(2) N4A 0.019(2) 0.020(3) 0.029(3) -0.002(2) 0.003(2) -0.004(2) C1A 0.023(3) 0.027(4) 0.029(4) 0.000(3) 0.003(3) 0.001(3) C2A 0.024(3) 0.035(4) 0.029(4) -0.008(3) 0.001(3) -0.006(3) C3A 0.035(4) 0.030(4) 0.035(4) -0.012(3) 0.001(3) 0.000(3) C4A 0.021(3) 0.035(4) 0.025(3) -0.003(3) 0.005(3) 0.004(3) C5A 0.024(3) 0.037(4) 0.024(3) -0.003(3) 0.004(3) 0.009(3) C6A 0.025(3) 0.035(4) 0.031(4) 0.000(3) 0.011(3) 0.007(3) C7A 0.029(3) 0.046(4) 0.028(4) 0.000(3) 0.011(3) 0.004(3) C8A 0.025(3) 0.038(4) 0.034(4) 0.009(3) 0.011(3) 0.003(3) C9A 0.022(3) 0.028(4) 0.033(4) 0.006(3) 0.005(3) 0.003(3) C10A 0.019(3) 0.029(4) 0.041(4) 0.002(3) 0.011(3) 0.003(3) C11A 0.016(3) 0.032(4) 0.036(4) -0.001(3) 0.007(3) -0.001(3) C12A 0.028(4) 0.042(4) 0.046(4) -0.005(4) 0.012(3) -0.018(3) C13A 0.028(4) 0.056(5) 0.029(4) -0.002(4) 0.000(3) -0.015(3) C14A 0.020(3) 0.038(4) 0.026(4) 0.001(3) 0.004(3) -0.001(3) C15A 0.022(3) 0.029(4) 0.026(3) 0.002(3) 0.000(3) 0.001(3) C16A 0.019(3) 0.019(3) 0.027(3) 0.006(3) 0.003(2) 0.000(2) C17A 0.024(3) 0.020(3) 0.032(4) 0.002(3) 0.007(3) -0.004(3) C18A 0.018(3) 0.024(3) 0.031(4) 0.000(3) 0.003(3) -0.002(2) C19A 0.023(3) 0.020(3) 0.027(3) -0.002(3) 0.001(3) 0.000(2) C20A 0.022(3) 0.022(3) 0.028(3) 0.003(3) 0.003(3) -0.002(3) C21A 0.030(4) 0.036(4) 0.041(4) -0.010(3) 0.011(3) 0.000(3) C22A 0.036(4) 0.081(6) 0.036(4) -0.013(4) 0.001(3) 0.009(4) C23A 0.052(5) 0.105(8) 0.029(4) -0.021(5) 0.005(4) -0.010(5) C24A 0.059(6) 0.080(7) 0.062(6) -0.032(5) 0.033(5) -0.018(5) C25A 0.056(5) 0.044(5) 0.063(6) -0.009(4) 0.030(4) 0.006(4) C26A 0.044(4) 0.032(4) 0.045(4) -0.007(3) 0.015(3) 0.005(3) C27A 0.025(3) 0.029(4) 0.034(4) 0.002(3) 0.010(3) 0.001(3) C28A 0.027(4) 0.041(5) 0.116(8) 0.027(5) 0.026(5) 0.004(3) C29A 0.025(4) 0.052(5) 0.135(9) 0.038(6) 0.022(5) 0.001(4) C30A 0.032(4) 0.033(4) 0.060(5) 0.006(4) 0.014(4) -0.007(3) C31A 0.048(5) 0.042(5) 0.120(8) 0.033(5) 0.034(5) 0.007(4) C32A 0.034(5) 0.047(5) 0.152(10) 0.042(6) 0.034(5) 0.006(4) C33A 0.022(3) 0.055(5) 0.028(4) 0.005(3) 0.002(3) -0.011(3) C34A 0.045(5) 0.069(6) 0.053(5) 0.022(5) 0.018(4) 0.014(4) C35A 0.053(6) 0.124(10) 0.055(6) 0.050(7) 0.014(5) 0.027(6) C36A 0.042(5) 0.156(12) 0.035(5) 0.014(7) -0.008(4) -0.035(6) C37A 0.068(6) 0.120(10) 0.033(5) -0.013(6) 0.011(4) -0.054(6) C38A 0.062(5) 0.063(6) 0.027(4) -0.002(4) 0.006(4) -0.025(4) C39A 0.028(4) 0.024(4) 0.050(5) -0.010(3) 0.010(3) -0.003(3) C40A 0.027(4) 0.046(5) 0.056(5) 0.011(4) 0.009(3) 0.001(3) C41A 0.027(4) 0.049(5) 0.059(5) -0.003(4) 0.009(4) -0.009(3) C42A 0.027(4) 0.044(5) 0.078(6) -0.007(4) 0.011(4) -0.006(3) C43A 0.031(4) 0.044(5) 0.059(5) -0.012(4) 0.000(4) -0.004(3) C44A 0.032(4) 0.035(4) 0.043(4) -0.001(3) 0.004(3) 0.001(3) Ni1B 0.0209(4) 0.0272(5) 0.0297(5) -0.0003(4) 0.0029(3) 0.0004(3) O1B 0.030(2) 0.046(3) 0.030(3) -0.008(2) 0.007(2) -0.001(2) N1B 0.024(3) 0.032(3) 0.028(3) -0.002(2) 0.003(2) 0.001(2) N2B 0.029(3) 0.032(3) 0.041(3) 0.002(3) 0.009(2) 0.001(3) N3B 0.028(3) 0.025(3) 0.039(3) -0.001(3) 0.007(2) -0.003(2) N4B 0.023(3) 0.018(3) 0.036(3) 0.001(2) 0.010(2) 0.002(2) C1B 0.034(4) 0.026(4) 0.029(4) -0.005(3) 0.006(3) 0.003(3) C2B 0.031(4) 0.038(4) 0.031(4) -0.001(3) 0.009(3) -0.004(3) C3B 0.038(4) 0.038(4) 0.027(4) 0.005(3) 0.003(3) 0.005(3) C4B 0.031(4) 0.033(4) 0.030(4) -0.007(3) 0.005(3) 0.003(3) C5B 0.030(4) 0.036(4) 0.033(4) 0.003(3) -0.005(3) 0.005(3) C6B 0.029(4) 0.044(4) 0.039(4) 0.008(4) 0.000(3) -0.005(3) C7B 0.037(4) 0.066(6) 0.047(5) 0.010(4) -0.008(4) -0.015(4) C8B 0.029(4) 0.054(5) 0.058(5) 0.008(4) -0.012(4) -0.012(4) C9B 0.024(4) 0.032(4) 0.054(5) 0.001(4) 0.003(3) -0.003(3) C10B 0.025(3) 0.030(4) 0.043(4) 0.000(3) 0.005(3) -0.002(3) C11B 0.025(3) 0.022(3) 0.048(4) -0.003(3) 0.010(3) -0.005(3) C12B 0.029(4) 0.031(4) 0.050(4) 0.003(4) 0.015(3) -0.001(3) C13B 0.037(4) 0.035(4) 0.034(4) 0.003(3) 0.013(3) -0.001(3) C14B 0.030(4) 0.020(3) 0.035(4) 0.001(3) 0.007(3) 0.003(3) C15B 0.030(3) 0.020(3) 0.027(3) 0.005(3) 0.008(3) 0.004(3) C16B 0.022(3) 0.025(3) 0.027(3) -0.003(3) 0.008(3) 0.003(3) C17B 0.027(3) 0.031(4) 0.024(4) 0.000(3) 0.006(3) -0.001(3) C18B 0.020(3) 0.027(3) 0.030(3) -0.001(3) 0.004(2) -0.004(3) C19B 0.018(3) 0.020(3) 0.027(3) -0.008(3) 0.003(2) 0.000(2) C20B 0.024(3) 0.028(4) 0.027(4) -0.004(3) 0.010(3) -0.002(3) C21B 0.028(4) 0.049(5) 0.033(4) 0.008(3) -0.001(3) -0.004(3) C22B 0.041(4) 0.083(7) 0.043(5) 0.010(5) 0.010(4) 0.020(4) C23B 0.040(5) 0.082(7) 0.040(5) 0.012(5) 0.005(4) 0.014(4) C24B 0.042(5) 0.053(5) 0.043(5) 0.008(4) -0.019(4) -0.008(4) C25B 0.050(5) 0.037(5) 0.063(6) -0.005(4) -0.025(4) -0.004(4) C26B 0.044(4) 0.038(4) 0.038(4) -0.005(3) -0.009(3) -0.005(3) C27B 0.029(4) 0.028(4) 0.060(5) 0.011(4) 0.003(4) 0.000(3) C28B 0.037(4) 0.034(4) 0.065(5) 0.000(4) -0.009(4) -0.001(3) C29B 0.046(5) 0.040(5) 0.088(7) 0.016(5) -0.013(5) -0.010(4) C30B 0.026(4) 0.049(6) 0.105(8) 0.030(6) 0.001(5) -0.003(4) C31B 0.030(4) 0.052(6) 0.101(8) 0.032(6) 0.017(5) 0.017(4) C32B 0.034(4) 0.042(5) 0.073(6) 0.016(4) 0.009(4) 0.007(3) C33B 0.025(3) 0.032(4) 0.031(4) -0.002(3) 0.010(3) -0.004(3) C34B 0.042(4) 0.038(4) 0.041(4) 0.003(3) 0.016(3) 0.012(3) C35B 0.054(5) 0.050(5) 0.034(4) -0.003(4) 0.020(4) 0.008(4) C36B 0.042(4) 0.070(6) 0.026(4) 0.002(4) 0.015(3) -0.002(4) C37B 0.060(5) 0.049(5) 0.041(5) 0.008(4) 0.003(4) 0.016(4) C38B 0.053(5) 0.035(4) 0.039(4) 0.005(3) 0.006(4) 0.009(4) C39B 0.033(4) 0.025(4) 0.046(4) 0.003(3) 0.012(3) 0.007(3) C40B 0.031(4) 0.030(4) 0.046(4) 0.002(3) 0.008(3) 0.003(3) C41B 0.028(4) 0.026(4) 0.045(4) 0.004(3) 0.014(3) 0.000(3) C42B 0.034(4) 0.034(4) 0.048(5) -0.002(4) 0.009(3) 0.002(3) C43B 0.035(4) 0.025(4) 0.040(4) -0.005(3) 0.005(3) -0.009(3) C44B 0.030(4) 0.029(4) 0.035(4) -0.003(3) 0.009(3) 0.002(3) Cl1 0.0664(15) 0.0833(18) 0.0690(16) 0.0056(13) 0.0250(12) -0.0154(13) Cl2 0.0633(14) 0.0643(16) 0.0815(17) -0.0032(13) 0.0172(12) -0.0105(11) C1S 0.046(5) 0.062(6) 0.076(6) 0.007(5) 0.011(4) 0.011(4) Cl3 0.120(3) 0.139(3) 0.0687(18) 0.028(2) 0.0093(17) 0.023(2) Cl4 0.205(4) 0.096(2) 0.076(2) 0.0034(18) 0.023(2) -0.068(3) C2S 0.231(16) 0.057(7) 0.037(6) 0.009(5) 0.022(7) 0.015(8) Cl5 0.119(4) 0.110(3) 0.130(4) -0.015(3) 0.077(3) -0.035(3) Cl6 0.145(5) 0.260(8) 0.117(4) 0.073(5) 0.051(3) -0.025(5) C3S 0.12(2) 0.163(17) 0.098(10) 0.020(15) 0.059(11) -0.003(16) Cl5D 0.119(4) 0.110(3) 0.130(4) -0.015(3) 0.077(3) -0.035(3) Cl6D 0.145(5) 0.260(8) 0.117(4) 0.073(5) 0.051(3) -0.025(5) C3D 0.12(2) 0.163(17) 0.098(10) 0.020(15) 0.059(11) -0.003(16) _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 Ni1A N3A 1.889(5) . ? Ni1A N2A 1.896(5) . ? Ni1A N1A 1.896(5) . ? Ni1A N4A 1.897(5) . ? O1A C17A 1.210(7) . ? N1A C1A 1.377(8) . ? N1A C4A 1.395(8) . ? N2A C9A 1.379(8) . ? N2A C6A 1.389(8) . ? N3A C14A 1.370(8) . ? N3A C11A 1.388(8) . ? N4A C16A 1.371(8) . ? N4A C19A 1.378(7) . ? C1A C20A 1.412(9) . ? C1A C2A 1.424(9) . ? C2A C3A 1.345(9) . ? C2A H2AA 0.9500 . ? C3A C4A 1.432(9) . ? C3A H3AA 0.9500 . ? C4A C5A 1.369(9) . ? C5A C6A 1.407(9) . ? C5A C21A 1.517(9) . ? C6A C7A 1.419(9) . ? C7A C8A 1.342(10) . ? C7A H7AA 0.9500 . ? C8A C9A 1.422(9) . ? C8A H8AA 0.9500 . ? C9A C10A 1.402(9) . ? C10A C11A 1.378(9) . ? C10A C27A 1.508(9) . ? C11A C12A 1.430(9) . ? C12A C13A 1.354(10) . ? C12A H12A 0.9500 . ? C13A C14A 1.425(9) . ? C13A H13A 0.9500 . ? C14A C15A 1.404(9) . ? C15A C16A 1.380(8) . ? C15A C33A 1.499(9) . ? C16A C17A 1.482(8) . ? C17A C18A 1.530(8) . ? C18A C19A 1.489(9) . ? C18A C18B 1.600(9) . ? C18A H18A 1.0000 . ? C19A C20A 1.389(8) . ? C20A C39A 1.507(9) . ? C21A C26A 1.381(9) . ? C21A C22A 1.395(10) . ? C22A C23A 1.384(11) . ? C22A H22A 0.9500 . ? C23A C24A 1.373(12) . ? C23A H23A 0.9500 . ? C24A C25A 1.384(12) . ? C24A H24A 0.9500 . ? C25A C26A 1.384(10) . ? C25A H25A 0.9500 . ? C26A H26A 0.9500 . ? C27A C28A 1.348(9) . ? C27A C32A 1.371(10) . ? C28A C29A 1.395(10) . ? C28A H28A 0.9500 . ? C29A C30A 1.351(11) . ? C29A H29A 0.9500 . ? C30A C31A 1.342(10) . ? C30A H30A 0.9500 . ? C31A C32A 1.394(11) . ? C31A H31A 0.9500 . ? C32A H32A 0.9500 . ? C33A C38A 1.359(11) . ? C33A C34A 1.384(11) . ? C34A C35A 1.398(12) . ? C34A H34A 0.9500 . ? C35A C36A 1.368(16) . ? C35A H35A 0.9500 . ? C36A C37A 1.364(16) . ? C36A H36A 0.9500 . ? C37A C38A 1.393(11) . ? C37A H37A 0.9500 . ? C38A H38A 0.9500 . ? C39A C40A 1.373(10) . ? C39A C44A 1.404(10) . ? C40A C41A 1.376(9) . ? C40A H40A 0.9500 . ? C41A C42A 1.404(11) . ? C41A H41A 0.9500 . ? C42A C43A 1.399(11) . ? C42A H42A 0.9500 . ? C43A C44A 1.393(10) . ? C43A H43A 0.9500 . ? C44A H44A 0.9500 . ? Ni1B N4B 1.897(5) . ? Ni1B N2B 1.906(5) . ? Ni1B N3B 1.924(6) . ? Ni1B N1B 1.947(5) . ? O1B C17B 1.208(7) . ? N1B C4B 1.385(8) . ? N1B C1B 1.395(8) . ? N2B C6B 1.383(9) . ? N2B C9B 1.392(8) . ? N3B C14B 1.361(8) . ? N3B C11B 1.401(8) . ? N4B C19B 1.362(7) . ? N4B C16B 1.382(8) . ? C1B C20B 1.386(9) . ? C1B C2B 1.421(9) . ? C2B C3B 1.347(9) . ? C2B H2BA 0.9500 . ? C3B C4B 1.410(10) . ? C3B H3BA 0.9500 . ? C4B C5B 1.394(9) . ? C5B C6B 1.373(10) . ? C5B C21B 1.487(9) . ? C6B C7B 1.439(10) . ? C7B C8B 1.357(11) . ? C7B H7BA 0.9500 . ? C8B C9B 1.435(10) . ? C8B H8BA 0.9500 . ? C9B C10B 1.389(10) . ? C10B C11B 1.394(9) . ? C10B C27B 1.481(9) . ? C11B C12B 1.423(10) . ? C12B C13B 1.336(9) . ? C12B H12B 0.9500 . ? C13B C14B 1.422(9) . ? C13B H13B 0.9500 . ? C14B C15B 1.424(9) . ? C15B C16B 1.348(8) . ? C15B C33B 1.486(9) . ? C16B C17B 1.515(8) . ? C17B C18B 1.527(9) . ? C18B C19B 1.493(8) . ? C18B C44B 1.521(9) . ? C19B C20B 1.375(9) . ? C20B C39B 1.499(9) . ? C21B C26B 1.385(10) . ? C21B C22B 1.388(10) . ? C22B C23B 1.375(11) . ? C22B H22B 0.9500 . ? C23B C24B 1.366(12) . ? C23B H23B 0.9500 . ? C24B C25B 1.369(12) . ? C24B H24B 0.9500 . ? C25B C26B 1.394(11) . ? C25B H25B 0.9500 . ? C26B H26B 0.9500 . ? C27B C32B 1.398(11) . ? C27B C28B 1.402(11) . ? C28B C29B 1.379(11) . ? C28B H28B 0.9500 . ? C29B C30B 1.366(13) . ? C29B H29B 0.9500 . ? C30B C31B 1.354(13) . ? C30B H30B 0.9500 . ? C31B C32B 1.404(11) . ? C31B H31B 0.9500 . ? C32B H32B 0.9500 . ? C33B C38B 1.371(9) . ? C33B C34B 1.394(9) . ? C34B C35B 1.380(10) . ? C34B H34B 0.9500 . ? C35B C36B 1.365(11) . ? C35B H35B 0.9500 . ? C36B C37B 1.369(11) . ? C36B H36B 0.9500 . ? C37B C38B 1.395(10) . ? C37B H37B 0.9500 . ? C38B H38B 0.9500 . ? C39B C40B 1.374(10) . ? C39B C44B 1.433(9) . ? C40B C41B 1.369(9) . ? C40B H40B 0.9500 . ? C41B C42B 1.383(10) . ? C41B H41B 0.9500 . ? C42B C43B 1.396(10) . ? C42B H42B 0.9500 . ? C43B C44B 1.386(9) . ? C43B H43B 0.9500 . ? Cl1 C1S 1.772(9) . ? Cl2 C1S 1.777(9) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? Cl3 C2S 1.746(9) . ? Cl4 C2S 1.672(11) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? Cl5 C3S 1.83(3) . ? Cl6 C3S 1.70(3) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? Cl5D C3D 1.84(3) . ? Cl6D C3D 1.70(3) . ? C3D H3D1 0.9900 . ? C3D H3D2 0.9900 . ? 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 N3A Ni1A N2A 89.6(2) . . ? N3A Ni1A N1A 178.2(2) . . ? N2A Ni1A N1A 90.3(2) . . ? N3A Ni1A N4A 89.9(2) . . ? N2A Ni1A N4A 177.0(2) . . ? N1A Ni1A N4A 90.4(2) . . ? C1A N1A C4A 105.3(5) . . ? C1A N1A Ni1A 127.4(4) . . ? C4A N1A Ni1A 126.8(4) . . ? C9A N2A C6A 105.5(5) . . ? C9A N2A Ni1A 126.9(4) . . ? C6A N2A Ni1A 127.3(4) . . ? C14A N3A C11A 104.8(5) . . ? C14A N3A Ni1A 127.3(4) . . ? C11A N3A Ni1A 127.8(4) . . ? C16A N4A C19A 108.8(5) . . ? C16A N4A Ni1A 126.1(4) . . ? C19A N4A Ni1A 124.8(4) . . ? N1A C1A C20A 124.3(6) . . ? N1A C1A C2A 110.4(5) . . ? C20A C1A C2A 125.2(6) . . ? C3A C2A C1A 107.4(6) . . ? C3A C2A H2AA 126.3 . . ? C1A C2A H2AA 126.3 . . ? C2A C3A C4A 107.6(6) . . ? C2A C3A H3AA 126.2 . . ? C4A C3A H3AA 126.2 . . ? C5A C4A N1A 123.5(6) . . ? C5A C4A C3A 126.6(6) . . ? N1A C4A C3A 109.2(5) . . ? C4A C5A C6A 122.3(6) . . ? C4A C5A C21A 121.3(6) . . ? C6A C5A C21A 115.9(6) . . ? N2A C6A C5A 123.9(6) . . ? N2A C6A C7A 109.6(6) . . ? C5A C6A C7A 126.2(6) . . ? C8A C7A C6A 107.5(6) . . ? C8A C7A H7AA 126.2 . . ? C6A C7A H7AA 126.2 . . ? C7A C8A C9A 107.8(6) . . ? C7A C8A H8AA 126.1 . . ? C9A C8A H8AA 126.1 . . ? N2A C9A C10A 124.1(6) . . ? N2A C9A C8A 109.6(6) . . ? C10A C9A C8A 125.5(6) . . ? C11A C10A C9A 121.2(6) . . ? C11A C10A C27A 120.4(6) . . ? C9A C10A C27A 118.2(6) . . ? C10A C11A N3A 124.1(6) . . ? C10A C11A C12A 124.7(6) . . ? N3A C11A C12A 110.6(6) . . ? C13A C12A C11A 106.2(6) . . ? C13A C12A H12A 126.9 . . ? C11A C12A H12A 126.9 . . ? C12A C13A C14A 107.6(6) . . ? C12A C13A H13A 126.2 . . ? C14A C13A H13A 126.2 . . ? N3A C14A C15A 123.5(6) . . ? N3A C14A C13A 110.5(6) . . ? C15A C14A C13A 125.1(6) . . ? C16A C15A C14A 120.1(6) . . ? C16A C15A C33A 120.9(6) . . ? C14A C15A C33A 118.6(5) . . ? N4A C16A C15A 125.7(5) . . ? N4A C16A C17A 109.7(5) . . ? C15A C16A C17A 123.5(6) . . ? O1A C17A C16A 129.7(5) . . ? O1A C17A C18A 126.0(5) . . ? C16A C17A C18A 104.3(5) . . ? C19A C18A C17A 100.2(5) . . ? C19A C18A C18B 110.4(5) . . ? C17A C18A C18B 110.8(5) . . ? C19A C18A H18A 111.6 . . ? C17A C18A H18A 111.6 . . ? C18B C18A H18A 111.6 . . ? N4A C19A C20A 124.8(6) . . ? N4A C19A C18A 110.7(5) . . ? C20A C19A C18A 124.2(5) . . ? C19A C20A C1A 119.9(5) . . ? C19A C20A C39A 122.4(6) . . ? C1A C20A C39A 117.6(5) . . ? C26A C21A C22A 119.6(7) . . ? C26A C21A C5A 120.3(6) . . ? C22A C21A C5A 120.0(6) . . ? C23A C22A C21A 120.1(8) . . ? C23A C22A H22A 120.0 . . ? C21A C22A H22A 120.0 . . ? C24A C23A C22A 119.6(8) . . ? C24A C23A H23A 120.2 . . ? C22A C23A H23A 120.2 . . ? C23A C24A C25A 120.9(8) . . ? C23A C24A H24A 119.5 . . ? C25A C24A H24A 119.5 . . ? C26A C25A C24A 119.4(8) . . ? C26A C25A H25A 120.3 . . ? C24A C25A H25A 120.3 . . ? C21A C26A C25A 120.4(7) . . ? C21A C26A H26A 119.8 . . ? C25A C26A H26A 119.8 . . ? C28A C27A C32A 117.3(7) . . ? C28A C27A C10A 122.6(6) . . ? C32A C27A C10A 120.0(6) . . ? C27A C28A C29A 121.6(7) . . ? C27A C28A H28A 119.2 . . ? C29A C28A H28A 119.2 . . ? C30A C29A C28A 120.3(7) . . ? C30A C29A H29A 119.8 . . ? C28A C29A H29A 119.8 . . ? C31A C30A C29A 119.2(7) . . ? C31A C30A H30A 120.4 . . ? C29A C30A H30A 120.4 . . ? C30A C31A C32A 120.4(8) . . ? C30A C31A H31A 119.8 . . ? C32A C31A H31A 119.8 . . ? C27A C32A C31A 121.1(8) . . ? C27A C32A H32A 119.4 . . ? C31A C32A H32A 119.4 . . ? C38A C33A C34A 118.7(7) . . ? C38A C33A C15A 121.7(7) . . ? C34A C33A C15A 119.3(7) . . ? C33A C34A C35A 118.9(9) . . ? C33A C34A H34A 120.6 . . ? C35A C34A H34A 120.6 . . ? C36A C35A C34A 121.4(10) . . ? C36A C35A H35A 119.3 . . ? C34A C35A H35A 119.3 . . ? C37A C36A C35A 119.6(9) . . ? C37A C36A H36A 120.2 . . ? C35A C36A H36A 120.2 . . ? C36A C37A C38A 118.8(10) . . ? C36A C37A H37A 120.6 . . ? C38A C37A H37A 120.6 . . ? C33A C38A C37A 122.4(9) . . ? C33A C38A H38A 118.8 . . ? C37A C38A H38A 118.8 . . ? C40A C39A C44A 118.1(6) . . ? C40A C39A C20A 122.7(6) . . ? C44A C39A C20A 119.2(6) . . ? C39A C40A C41A 122.8(7) . . ? C39A C40A H40A 118.6 . . ? C41A C40A H40A 118.6 . . ? C40A C41A C42A 119.0(7) . . ? C40A C41A H41A 120.5 . . ? C42A C41A H41A 120.5 . . ? C43A C42A C41A 119.8(7) . . ? C43A C42A H42A 120.1 . . ? C41A C42A H42A 120.1 . . ? C44A C43A C42A 119.3(7) . . ? C44A C43A H43A 120.3 . . ? C42A C43A H43A 120.3 . . ? C43A C44A C39A 121.0(7) . . ? C43A C44A H44A 119.5 . . ? C39A C44A H44A 119.5 . . ? N4B Ni1B N2B 177.4(2) . . ? N4B Ni1B N3B 88.0(2) . . ? N2B Ni1B N3B 90.6(2) . . ? N4B Ni1B N1B 90.9(2) . . ? N2B Ni1B N1B 90.6(2) . . ? N3B Ni1B N1B 176.9(2) . . ? C4B N1B C1B 104.6(5) . . ? C4B N1B Ni1B 126.0(4) . . ? C1B N1B Ni1B 128.7(4) . . ? C6B N2B C9B 106.0(5) . . ? C6B N2B Ni1B 127.0(4) . . ? C9B N2B Ni1B 127.0(5) . . ? C14B N3B C11B 104.8(5) . . ? C14B N3B Ni1B 128.1(4) . . ? C11B N3B Ni1B 127.1(5) . . ? C19B N4B C16B 107.5(5) . . ? C19B N4B Ni1B 123.2(4) . . ? C16B N4B Ni1B 129.1(4) . . ? C20B C1B N1B 122.3(6) . . ? C20B C1B C2B 127.3(6) . . ? N1B C1B C2B 110.3(5) . . ? C3B C2B C1B 106.6(6) . . ? C3B C2B H2BA 126.7 . . ? C1B C2B H2BA 126.7 . . ? C2B C3B C4B 108.5(6) . . ? C2B C3B H3BA 125.8 . . ? C4B C3B H3BA 125.8 . . ? N1B C4B C5B 125.2(6) . . ? N1B C4B C3B 110.0(6) . . ? C5B C4B C3B 124.6(6) . . ? C6B C5B C4B 121.1(6) . . ? C6B C5B C21B 120.5(6) . . ? C4B C5B C21B 118.4(6) . . ? C5B C6B N2B 126.8(6) . . ? C5B C6B C7B 123.5(7) . . ? N2B C6B C7B 109.7(6) . . ? C8B C7B C6B 107.3(7) . . ? C8B C7B H7BA 126.4 . . ? C6B C7B H7BA 126.4 . . ? C7B C8B C9B 107.4(6) . . ? C7B C8B H8BA 126.3 . . ? C9B C8B H8BA 126.3 . . ? C10B C9B N2B 125.4(6) . . ? C10B C9B C8B 123.9(6) . . ? N2B C9B C8B 109.5(6) . . ? C9B C10B C11B 121.6(6) . . ? C9B C10B C27B 116.7(6) . . ? C11B C10B C27B 121.8(6) . . ? C10B C11B N3B 124.9(6) . . ? C10B C11B C12B 125.4(6) . . ? N3B C11B C12B 109.6(6) . . ? C13B C12B C11B 107.2(6) . . ? C13B C12B H12B 126.4 . . ? C11B C12B H12B 126.4 . . ? C12B C13B C14B 107.6(6) . . ? C12B C13B H13B 126.2 . . ? C14B C13B H13B 126.2 . . ? N3B C14B C13B 110.7(6) . . ? N3B C14B C15B 125.5(6) . . ? C13B C14B C15B 123.6(6) . . ? C16B C15B C14B 119.4(6) . . ? C16B C15B C33B 121.9(6) . . ? C14B C15B C33B 118.3(5) . . ? C15B C16B N4B 125.4(5) . . ? C15B C16B C17B 125.7(6) . . ? N4B C16B C17B 108.8(5) . . ? O1B C17B C16B 128.4(6) . . ? O1B C17B C18B 127.8(6) . . ? C16B C17B C18B 103.8(5) . . ? C19B C18B C44B 101.5(5) . . ? C19B C18B C17B 98.8(5) . . ? C44B C18B C17B 124.6(5) . . ? C19B C18B C18A 109.6(5) . . ? C44B C18B C18A 113.7(5) . . ? C17B C18B C18A 106.7(5) . . ? N4B C19B C20B 129.8(5) . . ? N4B C19B C18B 113.9(5) . . ? C20B C19B C18B 113.5(5) . . ? C19B C20B C1B 120.9(6) . . ? C19B C20B C39B 106.4(5) . . ? C1B C20B C39B 129.9(6) . . ? C26B C21B C22B 118.5(7) . . ? C26B C21B C5B 119.9(7) . . ? C22B C21B C5B 121.6(7) . . ? C23B C22B C21B 120.6(8) . . ? C23B C22B H22B 119.7 . . ? C21B C22B H22B 119.7 . . ? C24B C23B C22B 120.8(8) . . ? C24B C23B H23B 119.6 . . ? C22B C23B H23B 119.6 . . ? C23B C24B C25B 119.4(8) . . ? C23B C24B H24B 120.3 . . ? C25B C24B H24B 120.3 . . ? C24B C25B C26B 120.6(8) . . ? C24B C25B H25B 119.7 . . ? C26B C25B H25B 119.7 . . ? C21B C26B C25B 119.9(8) . . ? C21B C26B H26B 120.1 . . ? C25B C26B H26B 120.1 . . ? C32B C27B C28B 118.0(7) . . ? C32B C27B C10B 122.0(7) . . ? C28B C27B C10B 119.9(7) . . ? C29B C28B C27B 120.6(9) . . ? C29B C28B H28B 119.7 . . ? C27B C28B H28B 119.7 . . ? C30B C29B C28B 120.7(9) . . ? C30B C29B H29B 119.6 . . ? C28B C29B H29B 119.6 . . ? C31B C30B C29B 120.0(8) . . ? C31B C30B H30B 120.0 . . ? C29B C30B H30B 120.0 . . ? C30B C31B C32B 121.0(9) . . ? C30B C31B H31B 119.5 . . ? C32B C31B H31B 119.5 . . ? C27B C32B C31B 119.5(9) . . ? C27B C32B H32B 120.2 . . ? C31B C32B H32B 120.2 . . ? C38B C33B C34B 118.1(6) . . ? C38B C33B C15B 120.4(6) . . ? C34B C33B C15B 121.5(6) . . ? C35B C34B C33B 120.3(7) . . ? C35B C34B H34B 119.9 . . ? C33B C34B H34B 119.9 . . ? C36B C35B C34B 120.9(7) . . ? C36B C35B H35B 119.5 . . ? C34B C35B H35B 119.5 . . ? C35B C36B C37B 119.7(7) . . ? C35B C36B H36B 120.1 . . ? C37B C36B H36B 120.1 . . ? C36B C37B C38B 119.7(7) . . ? C36B C37B H37B 120.2 . . ? C38B C37B H37B 120.2 . . ? C33B C38B C37B 121.3(7) . . ? C33B C38B H38B 119.4 . . ? C37B C38B H38B 119.4 . . ? C40B C39B C44B 118.0(6) . . ? C40B C39B C20B 133.4(6) . . ? C44B C39B C20B 108.1(6) . . ? C41B C40B C39B 120.4(7) . . ? C41B C40B H40B 119.8 . . ? C39B C40B H40B 119.8 . . ? C40B C41B C42B 121.6(6) . . ? C40B C41B H41B 119.2 . . ? C42B C41B H41B 119.2 . . ? C41B C42B C43B 120.3(7) . . ? C41B C42B H42B 119.8 . . ? C43B C42B H42B 119.8 . . ? C44B C43B C42B 117.8(7) . . ? C44B C43B H43B 121.1 . . ? C42B C43B H43B 121.1 . . ? C43B C44B C39B 121.7(6) . . ? C43B C44B C18B 129.7(6) . . ? C39B C44B C18B 108.6(5) . . ? Cl1 C1S Cl2 110.4(5) . . ? Cl1 C1S H1S1 109.6 . . ? Cl2 C1S H1S1 109.6 . . ? Cl1 C1S H1S2 109.6 . . ? Cl2 C1S H1S2 109.6 . . ? H1S1 C1S H1S2 108.1 . . ? Cl4 C2S Cl3 114.4(6) . . ? Cl4 C2S H2S1 108.7 . . ? Cl3 C2S H2S1 108.7 . . ? Cl4 C2S H2S2 108.7 . . ? Cl3 C2S H2S2 108.7 . . ? H2S1 C2S H2S2 107.6 . . ? Cl6 C3S Cl5 110.3(8) . . ? Cl6 C3S H3S1 109.6 . . ? Cl5 C3S H3S1 109.6 . . ? Cl6 C3S H3S2 109.6 . . ? Cl5 C3S H3S2 109.6 . . ? H3S1 C3S H3S2 108.1 . . ? Cl6D C3D Cl5D 117(2) . . ? Cl6D C3D H3D1 108.1 . . ? Cl5D C3D H3D1 108.1 . . ? Cl6D C3D H3D2 108.1 . . ? Cl5D C3D H3D2 108.1 . . ? H3D1 C3D H3D2 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3A Ni1A N1A C1A -111(7) . . . . ? N2A Ni1A N1A C1A 163.6(5) . . . . ? N4A Ni1A N1A C1A -13.4(5) . . . . ? N3A Ni1A N1A C4A 59(7) . . . . ? N2A Ni1A N1A C4A -26.4(5) . . . . ? N4A Ni1A N1A C4A 156.6(5) . . . . ? N3A Ni1A N2A C9A 25.5(5) . . . . ? N1A Ni1A N2A C9A -156.3(5) . . . . ? N4A Ni1A N2A C9A -55(4) . . . . ? N3A Ni1A N2A C6A -161.2(5) . . . . ? N1A Ni1A N2A C6A 17.0(5) . . . . ? N4A Ni1A N2A C6A 119(4) . . . . ? N2A Ni1A N3A C14A 156.9(5) . . . . ? N1A Ni1A N3A C14A 71(7) . . . . ? N4A Ni1A N3A C14A -26.1(5) . . . . ? N2A Ni1A N3A C11A -21.7(5) . . . . ? N1A Ni1A N3A C11A -107(7) . . . . ? N4A Ni1A N3A C11A 155.3(5) . . . . ? N3A Ni1A N4A C16A 21.8(5) . . . . ? N2A Ni1A N4A C16A 102(4) . . . . ? N1A Ni1A N4A C16A -156.5(5) . . . . ? N3A Ni1A N4A C19A -151.6(5) . . . . ? N2A Ni1A N4A C19A -72(4) . . . . ? N1A Ni1A N4A C19A 30.1(5) . . . . ? C4A N1A C1A C20A -178.7(6) . . . . ? Ni1A N1A C1A C20A -7.0(9) . . . . ? C4A N1A C1A C2A -2.1(7) . . . . ? Ni1A N1A C1A C2A 169.6(4) . . . . ? N1A C1A C2A C3A -0.6(8) . . . . ? C20A C1A C2A C3A 176.0(6) . . . . ? C1A C2A C3A C4A 2.9(8) . . . . ? C1A N1A C4A C5A -167.2(6) . . . . ? Ni1A N1A C4A C5A 21.0(9) . . . . ? C1A N1A C4A C3A 3.9(7) . . . . ? Ni1A N1A C4A C3A -167.9(4) . . . . ? C2A C3A C4A C5A 166.4(7) . . . . ? C2A C3A C4A N1A -4.3(8) . . . . ? N1A C4A C5A C6A 3.2(10) . . . . ? C3A C4A C5A C6A -166.3(6) . . . . ? N1A C4A C5A C21A 174.8(6) . . . . ? C3A C4A C5A C21A 5.3(10) . . . . ? C9A N2A C6A C5A 172.9(6) . . . . ? Ni1A N2A C6A C5A -1.5(9) . . . . ? C9A N2A C6A C7A -0.7(7) . . . . ? Ni1A N2A C6A C7A -175.1(4) . . . . ? C4A C5A C6A N2A -13.0(10) . . . . ? C21A C5A C6A N2A 175.0(6) . . . . ? C4A C5A C6A C7A 159.5(6) . . . . ? C21A C5A C6A C7A -12.5(10) . . . . ? N2A C6A C7A C8A 1.8(7) . . . . ? C5A C6A C7A C8A -171.6(6) . . . . ? C6A C7A C8A C9A -2.1(7) . . . . ? C6A N2A C9A C10A 169.6(6) . . . . ? Ni1A N2A C9A C10A -15.9(9) . . . . ? C6A N2A C9A C8A -0.6(7) . . . . ? Ni1A N2A C9A C8A 173.9(4) . . . . ? C7A C8A C9A N2A 1.7(7) . . . . ? C7A C8A C9A C10A -168.3(6) . . . . ? N2A C9A C10A C11A -7.6(9) . . . . ? C8A C9A C10A C11A 161.1(6) . . . . ? N2A C9A C10A C27A 177.1(6) . . . . ? C8A C9A C10A C27A -14.2(9) . . . . ? C9A C10A C11A N3A 11.8(10) . . . . ? C27A C10A C11A N3A -173.1(6) . . . . ? C9A C10A C11A C12A -159.0(6) . . . . ? C27A C10A C11A C12A 16.1(10) . . . . ? C14A N3A C11A C10A -171.1(6) . . . . ? Ni1A N3A C11A C10A 7.7(9) . . . . ? C14A N3A C11A C12A 0.8(7) . . . . ? Ni1A N3A C11A C12A 179.7(4) . . . . ? C10A C11A C12A C13A 168.1(7) . . . . ? N3A C11A C12A C13A -3.8(8) . . . . ? C11A C12A C13A C14A 5.0(8) . . . . ? C11A N3A C14A C15A -167.2(6) . . . . ? Ni1A N3A C14A C15A 13.9(9) . . . . ? C11A N3A C14A C13A 2.4(7) . . . . ? Ni1A N3A C14A C13A -176.5(5) . . . . ? C12A C13A C14A N3A -4.8(8) . . . . ? C12A C13A C14A C15A 164.6(7) . . . . ? N3A C14A C15A C16A 12.2(10) . . . . ? C13A C14A C15A C16A -155.8(7) . . . . ? N3A C14A C15A C33A -175.0(6) . . . . ? C13A C14A C15A C33A 16.9(10) . . . . ? C19A N4A C16A C15A 169.0(6) . . . . ? Ni1A N4A C16A C15A -5.2(9) . . . . ? C19A N4A C16A C17A 0.4(7) . . . . ? Ni1A N4A C16A C17A -173.9(4) . . . . ? C14A C15A C16A N4A -16.6(10) . . . . ? C33A C15A C16A N4A 170.7(6) . . . . ? C14A C15A C16A C17A 150.6(6) . . . . ? C33A C15A C16A C17A -22.1(9) . . . . ? N4A C16A C17A O1A -167.4(6) . . . . ? C15A C16A C17A O1A 23.6(10) . . . . ? N4A C16A C17A C18A 14.9(6) . . . . ? C15A C16A C17A C18A -154.0(6) . . . . ? O1A C17A C18A C19A 159.7(6) . . . . ? C16A C17A C18A C19A -22.5(6) . . . . ? O1A C17A C18A C18B -83.7(8) . . . . ? C16A C17A C18A C18B 94.1(6) . . . . ? C16A N4A C19A C20A 156.6(6) . . . . ? Ni1A N4A C19A C20A -29.0(8) . . . . ? C16A N4A C19A C18A -16.5(7) . . . . ? Ni1A N4A C19A C18A 157.9(4) . . . . ? C17A C18A C19A N4A 24.5(6) . . . . ? C18B C18A C19A N4A -92.4(6) . . . . ? C17A C18A C19A C20A -148.7(6) . . . . ? C18B C18A C19A C20A 94.4(7) . . . . ? N4A C19A C20A C1A 0.9(9) . . . . ? C18A C19A C20A C1A 173.1(6) . . . . ? N4A C19A C20A C39A -173.7(6) . . . . ? C18A C19A C20A C39A -1.5(10) . . . . ? N1A C1A C20A C19A 17.6(10) . . . . ? C2A C1A C20A C19A -158.5(6) . . . . ? N1A C1A C20A C39A -167.6(6) . . . . ? C2A C1A C20A C39A 16.3(9) . . . . ? C4A C5A C21A C26A 118.3(7) . . . . ? C6A C5A C21A C26A -69.6(9) . . . . ? C4A C5A C21A C22A -66.9(10) . . . . ? C6A C5A C21A C22A 105.2(8) . . . . ? C26A C21A C22A C23A -1.0(13) . . . . ? C5A C21A C22A C23A -175.8(8) . . . . ? C21A C22A C23A C24A 0.0(14) . . . . ? C22A C23A C24A C25A 0.8(15) . . . . ? C23A C24A C25A C26A -0.6(14) . . . . ? C22A C21A C26A C25A 1.1(11) . . . . ? C5A C21A C26A C25A 175.9(7) . . . . ? C24A C25A C26A C21A -0.3(12) . . . . ? C11A C10A C27A C28A -82.4(9) . . . . ? C9A C10A C27A C28A 92.9(9) . . . . ? C11A C10A C27A C32A 101.7(9) . . . . ? C9A C10A C27A C32A -83.0(9) . . . . ? C32A C27A C28A C29A -0.9(14) . . . . ? C10A C27A C28A C29A -176.9(9) . . . . ? C27A C28A C29A C30A -1.0(16) . . . . ? C28A C29A C30A C31A 1.9(15) . . . . ? C29A C30A C31A C32A -1.0(16) . . . . ? C28A C27A C32A C31A 1.8(15) . . . . ? C10A C27A C32A C31A 178.0(9) . . . . ? C30A C31A C32A C27A -0.9(17) . . . . ? C16A C15A C33A C38A 105.4(8) . . . . ? C14A C15A C33A C38A -67.3(9) . . . . ? C16A C15A C33A C34A -80.5(8) . . . . ? C14A C15A C33A C34A 106.8(8) . . . . ? C38A C33A C34A C35A -0.6(11) . . . . ? C15A C33A C34A C35A -174.9(7) . . . . ? C33A C34A C35A C36A -0.9(13) . . . . ? C34A C35A C36A C37A 0.9(15) . . . . ? C35A C36A C37A C38A 0.5(14) . . . . ? C34A C33A C38A C37A 2.1(12) . . . . ? C15A C33A C38A C37A 176.2(7) . . . . ? C36A C37A C38A C33A -2.0(13) . . . . ? C19A C20A C39A C40A 60.7(9) . . . . ? C1A C20A C39A C40A -114.0(8) . . . . ? C19A C20A C39A C44A -123.0(7) . . . . ? C1A C20A C39A C44A 62.3(8) . . . . ? C44A C39A C40A C41A 1.3(11) . . . . ? C20A C39A C40A C41A 177.7(7) . . . . ? C39A C40A C41A C42A -0.8(12) . . . . ? C40A C41A C42A C43A 0.2(12) . . . . ? C41A C42A C43A C44A -0.2(12) . . . . ? C42A C43A C44A C39A 0.7(11) . . . . ? C40A C39A C44A C43A -1.3(11) . . . . ? C20A C39A C44A C43A -177.8(6) . . . . ? N4B Ni1B N1B C4B 162.6(5) . . . . ? N2B Ni1B N1B C4B -19.5(5) . . . . ? N3B Ni1B N1B C4B 93(4) . . . . ? N4B Ni1B N1B C1B -6.4(6) . . . . ? N2B Ni1B N1B C1B 171.4(6) . . . . ? N3B Ni1B N1B C1B -76(4) . . . . ? N4B Ni1B N2B C6B 138(5) . . . . ? N3B Ni1B N2B C6B -163.7(6) . . . . ? N1B Ni1B N2B C6B 13.5(6) . . . . ? N4B Ni1B N2B C9B -38(5) . . . . ? N3B Ni1B N2B C9B 20.1(6) . . . . ? N1B Ni1B N2B C9B -162.7(6) . . . . ? N4B Ni1B N3B C14B -16.9(5) . . . . ? N2B Ni1B N3B C14B 165.3(5) . . . . ? N1B Ni1B N3B C14B 53(4) . . . . ? N4B Ni1B N3B C11B 161.8(5) . . . . ? N2B Ni1B N3B C11B -16.0(5) . . . . ? N1B Ni1B N3B C11B -128(4) . . . . ? N2B Ni1B N4B C19B -105(5) . . . . ? N3B Ni1B N4B C19B -163.2(5) . . . . ? N1B Ni1B N4B C19B 19.6(5) . . . . ? N2B Ni1B N4B C16B 81(5) . . . . ? N3B Ni1B N4B C16B 22.0(5) . . . . ? N1B Ni1B N4B C16B -155.1(5) . . . . ? C4B N1B C1B C20B -176.3(6) . . . . ? Ni1B N1B C1B C20B -5.4(9) . . . . ? C4B N1B C1B C2B -0.3(7) . . . . ? Ni1B N1B C1B C2B 170.6(4) . . . . ? C20B C1B C2B C3B 175.2(7) . . . . ? N1B C1B C2B C3B -0.5(8) . . . . ? C1B C2B C3B C4B 1.1(8) . . . . ? C1B N1B C4B C5B -174.0(6) . . . . ? Ni1B N1B C4B C5B 14.8(10) . . . . ? C1B N1B C4B C3B 1.0(7) . . . . ? Ni1B N1B C4B C3B -170.2(4) . . . . ? C2B C3B C4B N1B -1.3(8) . . . . ? C2B C3B C4B C5B 173.7(7) . . . . ? N1B C4B C5B C6B 3.2(11) . . . . ? C3B C4B C5B C6B -171.1(7) . . . . ? N1B C4B C5B C21B -177.9(6) . . . . ? C3B C4B C5B C21B 7.8(11) . . . . ? C4B C5B C6B N2B -10.3(12) . . . . ? C21B C5B C6B N2B 170.8(7) . . . . ? C4B C5B C6B C7B 166.2(7) . . . . ? C21B C5B C6B C7B -12.7(12) . . . . ? C9B N2B C6B C5B 175.2(8) . . . . ? Ni1B N2B C6B C5B -1.7(11) . . . . ? C9B N2B C6B C7B -1.7(8) . . . . ? Ni1B N2B C6B C7B -178.5(5) . . . . ? C5B C6B C7B C8B -174.2(8) . . . . ? N2B C6B C7B C8B 2.8(10) . . . . ? C6B C7B C8B C9B -2.7(10) . . . . ? C6B N2B C9B C10B 168.1(7) . . . . ? Ni1B N2B C9B C10B -15.0(10) . . . . ? C6B N2B C9B C8B 0.0(8) . . . . ? Ni1B N2B C9B C8B 176.8(5) . . . . ? C7B C8B C9B C10B -166.6(8) . . . . ? C7B C8B C9B N2B 1.8(10) . . . . ? N2B C9B C10B C11B -2.1(11) . . . . ? C8B C9B C10B C11B 164.4(7) . . . . ? N2B C9B C10B C27B 179.7(6) . . . . ? C8B C9B C10B C27B -13.8(11) . . . . ? C9B C10B C11B N3B 6.5(11) . . . . ? C27B C10B C11B N3B -175.3(6) . . . . ? C9B C10B C11B C12B -168.8(7) . . . . ? C27B C10B C11B C12B 9.3(11) . . . . ? C14B N3B C11B C10B -174.9(6) . . . . ? Ni1B N3B C11B C10B 6.1(9) . . . . ? C14B N3B C11B C12B 1.0(7) . . . . ? Ni1B N3B C11B C12B -177.9(4) . . . . ? C10B C11B C12B C13B 173.8(7) . . . . ? N3B C11B C12B C13B -2.2(8) . . . . ? C11B C12B C13B C14B 2.4(8) . . . . ? C11B N3B C14B C13B 0.4(7) . . . . ? Ni1B N3B C14B C13B 179.4(4) . . . . ? C11B N3B C14B C15B -174.3(6) . . . . ? Ni1B N3B C14B C15B 4.7(9) . . . . ? C12B C13B C14B N3B -1.8(8) . . . . ? C12B C13B C14B C15B 173.0(6) . . . . ? N3B C14B C15B C16B 10.7(9) . . . . ? C13B C14B C15B C16B -163.4(6) . . . . ? N3B C14B C15B C33B -176.6(6) . . . . ? C13B C14B C15B C33B 9.3(9) . . . . ? C14B C15B C16B N4B -5.7(9) . . . . ? C33B C15B C16B N4B -178.1(6) . . . . ? C14B C15B C16B C17B 172.5(6) . . . . ? C33B C15B C16B C17B 0.1(10) . . . . ? C19B N4B C16B C15B 169.7(6) . . . . ? Ni1B N4B C16B C15B -14.9(9) . . . . ? C19B N4B C16B C17B -8.8(7) . . . . ? Ni1B N4B C16B C17B 166.6(4) . . . . ? C15B C16B C17B O1B 24.8(11) . . . . ? N4B C16B C17B O1B -156.7(7) . . . . ? C15B C16B C17B C18B -155.9(6) . . . . ? N4B C16B C17B C18B 22.6(6) . . . . ? O1B C17B C18B C19B 154.1(7) . . . . ? C16B C17B C18B C19B -25.2(6) . . . . ? O1B C17B C18B C44B 43.5(10) . . . . ? C16B C17B C18B C44B -135.8(6) . . . . ? O1B C17B C18B C18A -92.2(8) . . . . ? C16B C17B C18B C18A 88.4(5) . . . . ? C19A C18A C18B C19B -73.2(6) . . . . ? C17A C18A C18B C19B 176.7(5) . . . . ? C19A C18A C18B C44B 39.6(7) . . . . ? C17A C18A C18B C44B -70.6(7) . . . . ? C19A C18A C18B C17B -179.3(5) . . . . ? C17A C18A C18B C17B 70.6(6) . . . . ? C16B N4B C19B C20B 150.3(6) . . . . ? Ni1B N4B C19B C20B -25.5(9) . . . . ? C16B N4B C19B C18B -9.4(7) . . . . ? Ni1B N4B C19B C18B 174.9(4) . . . . ? C44B C18B C19B N4B 150.7(5) . . . . ? C17B C18B C19B N4B 22.5(6) . . . . ? C18A C18B C19B N4B -88.8(6) . . . . ? C44B C18B C19B C20B -12.4(7) . . . . ? C17B C18B C19B C20B -140.6(5) . . . . ? C18A C18B C19B C20B 108.2(6) . . . . ? N4B C19B C20B C1B 9.3(10) . . . . ? C18B C19B C20B C1B 169.0(6) . . . . ? N4B C19B C20B C39B -153.5(6) . . . . ? C18B C19B C20B C39B 6.2(7) . . . . ? N1B C1B C20B C19B 7.0(10) . . . . ? C2B C1B C20B C19B -168.2(6) . . . . ? N1B C1B C20B C39B 165.3(6) . . . . ? C2B C1B C20B C39B -9.9(11) . . . . ? C6B C5B C21B C26B -75.7(10) . . . . ? C4B C5B C21B C26B 105.4(8) . . . . ? C6B C5B C21B C22B 106.4(9) . . . . ? C4B C5B C21B C22B -72.5(10) . . . . ? C26B C21B C22B C23B -3.0(12) . . . . ? C5B C21B C22B C23B 174.9(7) . . . . ? C21B C22B C23B C24B -1.0(13) . . . . ? C22B C23B C24B C25B 3.6(13) . . . . ? C23B C24B C25B C26B -2.2(12) . . . . ? C22B C21B C26B C25B 4.4(11) . . . . ? C5B C21B C26B C25B -173.6(7) . . . . ? C24B C25B C26B C21B -1.8(11) . . . . ? C9B C10B C27B C32B 120.0(8) . . . . ? C11B C10B C27B C32B -58.2(10) . . . . ? C9B C10B C27B C28B -56.8(9) . . . . ? C11B C10B C27B C28B 125.0(8) . . . . ? C32B C27B C28B C29B -1.3(11) . . . . ? C10B C27B C28B C29B 175.6(7) . . . . ? C27B C28B C29B C30B 1.4(12) . . . . ? C28B C29B C30B C31B 0.0(13) . . . . ? C29B C30B C31B C32B -1.3(12) . . . . ? C28B C27B C32B C31B 0.0(11) . . . . ? C10B C27B C32B C31B -176.9(7) . . . . ? C30B C31B C32B C27B 1.4(12) . . . . ? C16B C15B C33B C38B 72.7(9) . . . . ? C14B C15B C33B C38B -99.8(7) . . . . ? C16B C15B C33B C34B -108.6(7) . . . . ? C14B C15B C33B C34B 78.9(8) . . . . ? C38B C33B C34B C35B -1.0(10) . . . . ? C15B C33B C34B C35B -179.7(6) . . . . ? C33B C34B C35B C36B -0.3(12) . . . . ? C34B C35B C36B C37B 1.2(12) . . . . ? C35B C36B C37B C38B -0.8(12) . . . . ? C34B C33B C38B C37B 1.5(11) . . . . ? C15B C33B C38B C37B -179.8(7) . . . . ? C36B C37B C38B C33B -0.6(12) . . . . ? C19B C20B C39B C40B 174.8(7) . . . . ? C1B C20B C39B C40B 14.1(12) . . . . ? C19B C20B C39B C44B 3.2(7) . . . . ? C1B C20B C39B C44B -157.5(7) . . . . ? C44B C39B C40B C41B -0.2(10) . . . . ? C20B C39B C40B C41B -171.1(7) . . . . ? C39B C40B C41B C42B 3.6(10) . . . . ? C40B C41B C42B C43B -4.3(10) . . . . ? C41B C42B C43B C44B 1.3(10) . . . . ? C42B C43B C44B C39B 2.2(10) . . . . ? C42B C43B C44B C18B -176.2(6) . . . . ? C40B C39B C44B C43B -2.8(10) . . . . ? C20B C39B C44B C43B 170.3(6) . . . . ? C40B C39B C44B C18B 175.9(6) . . . . ? C20B C39B C44B C18B -11.0(7) . . . . ? C19B C18B C44B C43B -167.7(7) . . . . ? C17B C18B C44B C43B -58.4(10) . . . . ? C18A C18B C44B C43B 74.7(9) . . . . ? C19B C18B C44B C39B 13.8(7) . . . . ? C17B C18B C44B C39B 123.1(6) . . . . ? C18A C18B C44B C39B -103.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.545 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.106