# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Robert Grubbs' 'Eric F. Connor' 'Jason I. Henderson' 'Andrew W. Waltman' 'Todd R. Younkin' _publ_contact_author_address ; Chemistry and Chemical Engineering California Institute of Technology 1200 E. California Blvd. MC 164-30 Pasadena CA 91125 UNITED STATES OF AMERICA ; _publ_contact_author_email RHG@ITS.CALTECH.EDU _publ_contact_author_name 'Prof Robert Grubbs' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Synthesis of neutral nickel catalysts for ethylene polymerization the influence of ligand size on catalyst stability ; #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Michael W. Day Beckman Institute California Institute of Technology Pasadena, CA 91125 USA ; _publ_contact_author_fax '(818) 449 4159' _publ_contact_author_phone '(818) 395 2734' _publ_contact_letter ; Please consider this CIF submission for deposition in the Cambridge Structural Database. ; _publ_requested_coeditor_name ? data_9 _audit_creation_method SHELXL-97 _database_code_CSD 161495 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H52 N4 Ni O2' _chemical_formula_weight 919.77 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.8013(6) _cell_length_b 19.2789(6) _cell_length_c 27.0247(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9274.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 33100 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 27.01 _exptl_crystal_description Needle _exptl_crystal_colour 'Greenish yellow' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3872 _exptl_absorpt_coefficient_mu 0.469 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8471 _exptl_absorpt_correction_T_max 0.9183 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans at 6 f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 154074 _diffrn_reflns_av_R_equivalents 0.0780 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.59 _reflns_number_total 11208 _reflns_number_gt 7057 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT v6.2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Difference Fourier map' _refine_ls_hydrogen_treatment Unrestrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11208 _refine_ls_number_parameters 812 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.0589 _refine_ls_wR_factor_gt 0.0566 _refine_ls_goodness_of_fit_ref 1.805 _refine_ls_restrained_S_all 1.805 _refine_ls_shift/su_max 0.005 _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 0.725425(12) 0.153820(11) 0.382572(8) 0.03310(7) Uani 1 1 d . . . O1 O 0.81321(6) 0.15828(6) 0.42841(4) 0.0343(3) Uani 1 1 d . . . O2 O 0.63913(6) 0.16207(6) 0.33560(4) 0.0361(3) Uani 1 1 d . . . N1 N 0.65209(8) 0.09922(7) 0.43110(5) 0.0331(4) Uani 1 1 d . . . N2 N 0.77392(8) 0.06160(7) 0.35237(5) 0.0360(4) Uani 1 1 d . . . N3 N 0.69394(8) 0.25596(7) 0.41724(6) 0.0410(4) Uani 1 1 d . . . N4 N 0.78215(9) 0.22143(8) 0.32722(5) 0.0442(4) Uani 1 1 d . . . C1 C 0.58193(11) 0.08701(9) 0.42139(7) 0.0340(5) Uani 1 1 d . . . C2 C 0.54084(9) 0.10102(8) 0.37675(6) 0.0320(4) Uani 1 1 d . . . C3 C 0.46808(10) 0.07297(9) 0.37303(7) 0.0386(5) Uani 1 1 d . . . C4 C 0.42468(12) 0.08271(10) 0.33205(8) 0.0453(5) Uani 1 1 d . . . C5 C 0.45237(12) 0.12440(10) 0.29398(8) 0.0447(5) Uani 1 1 d . . . C6 C 0.52262(10) 0.15350(9) 0.29553(6) 0.0344(4) Uani 1 1 d . . . C7 C 0.57136(10) 0.13931(8) 0.33648(6) 0.0323(4) Uani 1 1 d . . . C8 C 0.67606(10) 0.07299(9) 0.47822(6) 0.0339(4) Uani 1 1 d . . . C9 C 0.73450(11) 0.02570(10) 0.47969(7) 0.0420(5) Uani 1 1 d . . . C10 C 0.75431(12) -0.00582(11) 0.52371(8) 0.0482(6) Uani 1 1 d . . . C11 C 0.71673(13) 0.01024(11) 0.56679(8) 0.0507(6) Uani 1 1 d . . . C12 C 0.66046(13) 0.05889(11) 0.56593(8) 0.0488(6) Uani 1 1 d . . . C13 C 0.64012(12) 0.09006(10) 0.52177(7) 0.0408(5) Uani 1 1 d . . . C14 C 0.54985(9) 0.20123(10) 0.25589(6) 0.0361(5) Uani 1 1 d . . . C15 C 0.58298(10) 0.17519(10) 0.21259(7) 0.0410(5) Uani 1 1 d . . . C16 C 0.59059(13) 0.10285(12) 0.20365(9) 0.0535(6) Uani 1 1 d . . . C17 C 0.62092(15) 0.07953(15) 0.16071(10) 0.0708(7) Uani 1 1 d . . . C18 C 0.64600(15) 0.12627(17) 0.12420(10) 0.0757(8) Uani 1 1 d . . . C19 C 0.64194(13) 0.19453(16) 0.13147(8) 0.0641(7) Uani 1 1 d . . . C20 C 0.61096(10) 0.22207(11) 0.17591(7) 0.0461(5) Uani 1 1 d . . . C21 C 0.60793(11) 0.29292(12) 0.18483(8) 0.0502(6) Uani 1 1 d . . . C22 C 0.57474(10) 0.31994(10) 0.22694(7) 0.0431(5) Uani 1 1 d . . . C23 C 0.56918(13) 0.39282(12) 0.23574(10) 0.0544(6) Uani 1 1 d . . . C24 C 0.53520(13) 0.41803(13) 0.27643(10) 0.0582(6) Uani 1 1 d . . . C25 C 0.50377(12) 0.37275(12) 0.31111(9) 0.0518(6) Uani 1 1 d . . . C26 C 0.50732(11) 0.30317(11) 0.30471(8) 0.0432(5) Uani 1 1 d . . . C27 C 0.54367(10) 0.27373(10) 0.26284(7) 0.0373(5) Uani 1 1 d . . . C28 C 0.83884(11) 0.03718(10) 0.36578(6) 0.0371(5) Uani 1 1 d . . . C29 C 0.88948(10) 0.06249(9) 0.40301(6) 0.0336(4) Uani 1 1 d . . . C30 C 0.95599(11) 0.02497(10) 0.41097(7) 0.0427(5) Uani 1 1 d . . . C31 C 1.00737(12) 0.04395(11) 0.44551(7) 0.0479(6) Uani 1 1 d . . . C32 C 0.99400(11) 0.10348(10) 0.47346(7) 0.0429(5) Uani 1 1 d . . . C33 C 0.92998(10) 0.14225(9) 0.46775(6) 0.0328(4) Uani 1 1 d . . . C34 C 0.87420(10) 0.12241(9) 0.43219(6) 0.0321(4) Uani 1 1 d . . . C35 C 0.73723(10) 0.02056(9) 0.31516(7) 0.0374(5) Uani 1 1 d . . . C36 C 0.77065(13) 0.00682(12) 0.27026(7) 0.0535(6) Uani 1 1 d . . . C37 C 0.73514(14) -0.03592(12) 0.23637(8) 0.0616(7) Uani 1 1 d . . . C38 C 0.66700(13) -0.06472(11) 0.24685(8) 0.0537(6) Uani 1 1 d . . . C39 C 0.63334(13) -0.05094(10) 0.29149(8) 0.0480(5) Uani 1 1 d . . . C40 C 0.66859(11) -0.00853(10) 0.32544(8) 0.0422(5) Uani 1 1 d . . . C41 C 0.91580(9) 0.20646(9) 0.49749(6) 0.0335(4) Uani 1 1 d . . . C42 C 0.93169(10) 0.27162(9) 0.47665(7) 0.0355(4) Uani 1 1 d . . . C43 C 0.96853(11) 0.27920(11) 0.43021(7) 0.0401(5) Uani 1 1 d . . . C44 C 0.97725(11) 0.34234(11) 0.40870(8) 0.0464(5) Uani 1 1 d . . . C45 C 0.95072(12) 0.40222(11) 0.43262(9) 0.0497(6) Uani 1 1 d . . . C46 C 0.91867(11) 0.39843(11) 0.47775(8) 0.0465(5) Uani 1 1 d . . . C47 C 0.90784(10) 0.33332(9) 0.50178(7) 0.0372(5) Uani 1 1 d . . . C48 C 0.87382(11) 0.32781(10) 0.54763(7) 0.0430(5) Uani 1 1 d . . . C49 C 0.86202(10) 0.26426(10) 0.57048(7) 0.0394(5) Uani 1 1 d . . . C50 C 0.82919(11) 0.25825(12) 0.61828(8) 0.0490(5) Uani 1 1 d . . . C51 C 0.81546(12) 0.19636(12) 0.63910(8) 0.0518(6) Uani 1 1 d . . . C52 C 0.83333(12) 0.13505(11) 0.61286(8) 0.0504(6) Uani 1 1 d . . . C53 C 0.86525(11) 0.13775(10) 0.56773(7) 0.0440(5) Uani 1 1 d . . . C54 C 0.88226(10) 0.20214(9) 0.54438(6) 0.0353(4) Uani 1 1 d . . . C55 C 0.7453(2) 0.30418(13) 0.39062(11) 0.0848(10) Uani 1 1 d . . . C56 C 0.75330(19) 0.29043(13) 0.33809(11) 0.0848(9) Uani 1 1 d . . . C57 C 0.71197(16) 0.26112(15) 0.47004(9) 0.0569(7) Uani 1 1 d . . . C58 C 0.61564(16) 0.27448(16) 0.41115(13) 0.0743(9) Uani 1 1 d . . . C59 C 0.86440(13) 0.21836(17) 0.33002(10) 0.0591(7) Uani 1 1 d . . . C60 C 0.76277(18) 0.2053(2) 0.27545(9) 0.0711(9) Uani 1 1 d . . . H1 H 0.5523(8) 0.0637(7) 0.4469(5) 0.026(4) Uiso 1 1 d . . . H3 H 0.4493(8) 0.0456(7) 0.4010(5) 0.024(4) Uiso 1 1 d . . . H4 H 0.3762(9) 0.0637(8) 0.3302(6) 0.043(5) Uiso 1 1 d . . . H5 H 0.4226(8) 0.1347(7) 0.2673(5) 0.034(5) Uiso 1 1 d . . . H9 H 0.7604(8) 0.0133(7) 0.4500(5) 0.025(4) Uiso 1 1 d . . . H10 H 0.7927(9) -0.0398(8) 0.5230(6) 0.039(5) Uiso 1 1 d . . . H11 H 0.7309(9) -0.0109(8) 0.5973(6) 0.049(5) Uiso 1 1 d . . . H12 H 0.6343(9) 0.0707(8) 0.5946(6) 0.037(5) Uiso 1 1 d . . . H13 H 0.6025(8) 0.1229(7) 0.5212(5) 0.029(5) Uiso 1 1 d . . . H16 H 0.5746(9) 0.0714(9) 0.2281(6) 0.048(6) Uiso 1 1 d . . . H17 H 0.6262(10) 0.0304(10) 0.1560(7) 0.067(7) Uiso 1 1 d . . . H18 H 0.6659(11) 0.1106(10) 0.0947(7) 0.078(8) Uiso 1 1 d . . . H19 H 0.6550(11) 0.2276(9) 0.1075(7) 0.062(7) Uiso 1 1 d . . . H21 H 0.6281(9) 0.3239(8) 0.1619(6) 0.041(5) Uiso 1 1 d . . . H23 H 0.5890(9) 0.4214(8) 0.2128(6) 0.045(6) Uiso 1 1 d . . . H24 H 0.5325(10) 0.4666(9) 0.2813(6) 0.060(6) Uiso 1 1 d . . . H25 H 0.4783(9) 0.3880(8) 0.3398(6) 0.041(6) Uiso 1 1 d . . . H26 H 0.4861(8) 0.2733(8) 0.3281(5) 0.033(5) Uiso 1 1 d . . . H28 H 0.8552(8) -0.0049(8) 0.3500(5) 0.036(5) Uiso 1 1 d . . . H30 H 0.9627(8) -0.0147(8) 0.3920(6) 0.038(5) Uiso 1 1 d . . . H31 H 1.0507(9) 0.0170(8) 0.4516(5) 0.035(5) Uiso 1 1 d . . . H32 H 1.0286(9) 0.1179(8) 0.4970(6) 0.038(5) Uiso 1 1 d . . . H36 H 0.8175(10) 0.0268(8) 0.2633(6) 0.052(6) Uiso 1 1 d . . . H37 H 0.7600(10) -0.0443(9) 0.2044(7) 0.067(6) Uiso 1 1 d . . . H38 H 0.6445(10) -0.0932(9) 0.2242(6) 0.057(6) Uiso 1 1 d . . . H39 H 0.5858(9) -0.0699(8) 0.2997(6) 0.048(6) Uiso 1 1 d . . . H40 H 0.6449(8) -0.0020(7) 0.3558(5) 0.030(5) Uiso 1 1 d . . . H43 H 0.9859(8) 0.2401(7) 0.4135(5) 0.024(4) Uiso 1 1 d . . . H44 H 1.0003(9) 0.3456(8) 0.3749(6) 0.045(5) Uiso 1 1 d . . . H45 H 0.9560(9) 0.4435(8) 0.4168(6) 0.038(5) Uiso 1 1 d . . . H46 H 0.9004(8) 0.4382(8) 0.4944(5) 0.038(5) Uiso 1 1 d . . . H48 H 0.8575(9) 0.3676(8) 0.5636(5) 0.037(5) Uiso 1 1 d . . . H50 H 0.8172(9) 0.2988(8) 0.6348(6) 0.042(5) Uiso 1 1 d . . . H51 H 0.7922(9) 0.1928(8) 0.6710(6) 0.045(5) Uiso 1 1 d . . . H52 H 0.8219(9) 0.0930(9) 0.6273(6) 0.051(6) Uiso 1 1 d . . . H53 H 0.8771(8) 0.0960(8) 0.5501(5) 0.030(5) Uiso 1 1 d . . . H55A H 0.7216(10) 0.3542(10) 0.3969(6) 0.065(6) Uiso 1 1 d . . . H55B H 0.7985(18) 0.2984(17) 0.4049(12) 0.187(18) Uiso 1 1 d . . . H56A H 0.7829(10) 0.3267(10) 0.3227(6) 0.063(6) Uiso 1 1 d . . . H56B H 0.6900(17) 0.2991(14) 0.3401(11) 0.158(12) Uiso 1 1 d . . . H57A H 0.7615(12) 0.2498(10) 0.4756(7) 0.076(8) Uiso 1 1 d . . . H57B H 0.6767(13) 0.2323(12) 0.4888(8) 0.110(11) Uiso 1 1 d . . . H57C H 0.7045(9) 0.3090(10) 0.4824(6) 0.054(6) Uiso 1 1 d . . . H58A H 0.6063(10) 0.3215(10) 0.4236(6) 0.061(6) Uiso 1 1 d . . . H58B H 0.5840(10) 0.2409(9) 0.4287(7) 0.055(8) Uiso 1 1 d . . . H58C H 0.6020(12) 0.2725(11) 0.3762(8) 0.090(9) Uiso 1 1 d . . . H59A H 0.8862(10) 0.2505(9) 0.3065(6) 0.058(6) Uiso 1 1 d . . . H59B H 0.8836(12) 0.1724(11) 0.3246(8) 0.091(10) Uiso 1 1 d . . . H59C H 0.8774(10) 0.2322(9) 0.3625(7) 0.064(7) Uiso 1 1 d . . . H60A H 0.7102(13) 0.2109(11) 0.2725(8) 0.092(9) Uiso 1 1 d . . . H60B H 0.7807(17) 0.1586(15) 0.2686(11) 0.164(16) Uiso 1 1 d . . . H60C H 0.7879(9) 0.2389(9) 0.2529(6) 0.055(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.03271(12) 0.03465(13) 0.03192(12) -0.00021(12) -0.00160(12) -0.00044(12) O1 0.0336(7) 0.0331(7) 0.0361(7) -0.0060(6) -0.0045(5) 0.0042(6) O2 0.0308(7) 0.0431(8) 0.0343(7) 0.0052(6) -0.0035(6) -0.0040(6) N1 0.0370(9) 0.0313(9) 0.0309(9) 0.0004(7) -0.0008(7) 0.0022(7) N2 0.0367(9) 0.0412(9) 0.0300(8) -0.0046(7) -0.0007(8) -0.0015(8) N3 0.0420(10) 0.0357(9) 0.0454(10) -0.0012(8) -0.0045(8) 0.0047(8) N4 0.0387(10) 0.0513(11) 0.0425(10) 0.0043(8) -0.0004(8) -0.0070(8) C1 0.0379(12) 0.0274(11) 0.0368(12) 0.0009(9) 0.0077(10) 0.0000(9) C2 0.0322(10) 0.0300(10) 0.0338(11) -0.0003(9) -0.0011(9) 0.0015(8) C3 0.0377(12) 0.0353(11) 0.0429(13) 0.0024(10) 0.0033(10) 0.0003(9) C4 0.0347(13) 0.0445(13) 0.0567(14) 0.0024(11) -0.0069(11) -0.0096(10) C5 0.0419(13) 0.0467(13) 0.0456(14) 0.0036(11) -0.0122(11) 0.0000(10) C6 0.0364(11) 0.0318(10) 0.0349(11) -0.0007(9) -0.0052(8) 0.0015(10) C7 0.0340(11) 0.0275(11) 0.0355(11) -0.0057(8) -0.0011(9) 0.0021(8) C8 0.0359(11) 0.0340(11) 0.0320(11) 0.0040(9) -0.0022(9) -0.0070(9) C9 0.0421(13) 0.0464(13) 0.0374(12) 0.0046(10) 0.0027(11) -0.0013(10) C10 0.0447(14) 0.0487(14) 0.0511(14) 0.0142(12) -0.0081(11) 0.0004(11) C11 0.0585(15) 0.0551(15) 0.0386(13) 0.0114(12) -0.0132(12) -0.0154(13) C12 0.0613(16) 0.0540(14) 0.0310(13) -0.0024(11) 0.0024(12) -0.0124(12) C13 0.0444(13) 0.0393(13) 0.0386(12) -0.0009(10) 0.0004(11) -0.0014(10) C14 0.0331(11) 0.0393(12) 0.0357(11) 0.0024(9) -0.0110(9) 0.0011(9) C15 0.0396(12) 0.0467(13) 0.0366(12) -0.0003(10) -0.0093(9) 0.0043(10) C16 0.0628(16) 0.0515(16) 0.0463(15) -0.0044(13) -0.0051(12) 0.0043(12) C17 0.085(2) 0.0627(19) 0.0646(18) -0.0176(16) -0.0035(15) 0.0164(16) C18 0.0766(19) 0.101(2) 0.0493(18) -0.0168(18) 0.0048(15) 0.0181(17) C19 0.0625(17) 0.085(2) 0.0450(16) 0.0052(16) 0.0032(12) 0.0070(16) C20 0.0397(12) 0.0624(15) 0.0361(13) 0.0013(11) -0.0052(10) 0.0050(11) C21 0.0442(14) 0.0586(16) 0.0479(14) 0.0207(13) -0.0034(11) -0.0030(12) C22 0.0374(12) 0.0445(13) 0.0475(13) 0.0083(11) -0.0087(10) -0.0001(10) C23 0.0481(15) 0.0463(16) 0.0687(18) 0.0191(14) -0.0095(13) -0.0046(12) C24 0.0519(15) 0.0375(15) 0.085(2) -0.0024(15) -0.0157(14) 0.0029(12) C25 0.0451(14) 0.0490(15) 0.0613(16) -0.0096(13) -0.0077(12) 0.0064(11) C26 0.0363(13) 0.0443(14) 0.0488(14) 0.0021(12) -0.0064(10) -0.0012(11) C27 0.0323(11) 0.0401(12) 0.0395(12) 0.0044(10) -0.0092(9) 0.0017(9) C28 0.0401(12) 0.0357(12) 0.0356(12) -0.0077(9) 0.0055(9) 0.0008(10) C29 0.0354(11) 0.0349(11) 0.0304(10) -0.0056(9) -0.0007(8) 0.0012(9) C30 0.0472(13) 0.0351(12) 0.0458(13) -0.0128(10) -0.0003(10) 0.0073(10) C31 0.0435(13) 0.0416(13) 0.0585(15) -0.0073(11) -0.0108(11) 0.0165(11) C32 0.0434(13) 0.0410(13) 0.0444(13) -0.0074(10) -0.0127(11) 0.0042(10) C33 0.0366(11) 0.0305(11) 0.0315(10) 0.0002(9) -0.0029(9) 0.0027(9) C34 0.0345(11) 0.0303(10) 0.0316(11) 0.0010(9) 0.0014(9) -0.0003(9) C35 0.0385(12) 0.0384(11) 0.0354(11) -0.0060(9) -0.0045(9) 0.0043(9) C36 0.0431(14) 0.0748(16) 0.0426(13) -0.0168(11) 0.0000(12) -0.0083(13) C37 0.0558(16) 0.0869(18) 0.0421(14) -0.0254(13) -0.0030(13) 0.0013(14) C38 0.0530(15) 0.0561(15) 0.0521(15) -0.0230(12) -0.0170(12) 0.0030(12) C39 0.0415(14) 0.0433(13) 0.0591(15) -0.0081(11) -0.0058(12) -0.0027(11) C40 0.0430(13) 0.0416(12) 0.0420(13) -0.0092(10) 0.0010(11) 0.0030(10) C41 0.0335(11) 0.0309(11) 0.0362(11) -0.0052(9) -0.0100(9) 0.0033(9) C42 0.0344(11) 0.0341(11) 0.0379(11) -0.0019(9) -0.0095(9) -0.0003(9) C43 0.0406(12) 0.0336(13) 0.0460(13) -0.0066(11) -0.0022(10) 0.0008(10) C44 0.0434(13) 0.0477(14) 0.0481(14) -0.0005(12) 0.0025(10) -0.0061(11) C45 0.0521(14) 0.0352(14) 0.0618(16) 0.0087(13) -0.0040(12) -0.0035(11) C46 0.0481(14) 0.0338(13) 0.0576(15) -0.0074(12) -0.0030(12) 0.0035(10) C47 0.0367(11) 0.0311(12) 0.0437(12) -0.0046(9) -0.0083(9) -0.0002(9) C48 0.0461(13) 0.0357(13) 0.0472(14) -0.0135(11) -0.0060(10) 0.0049(10) C49 0.0401(12) 0.0404(12) 0.0379(12) -0.0069(10) -0.0072(9) 0.0013(10) C50 0.0545(14) 0.0472(14) 0.0455(14) -0.0130(13) 0.0000(11) 0.0024(11) C51 0.0593(15) 0.0596(16) 0.0364(13) -0.0039(12) 0.0015(11) -0.0048(12) C52 0.0630(15) 0.0483(15) 0.0401(13) 0.0051(12) -0.0049(12) -0.0085(11) C53 0.0560(14) 0.0371(13) 0.0387(12) -0.0054(10) -0.0064(11) 0.0025(10) C54 0.0368(11) 0.0348(11) 0.0342(11) -0.0036(9) -0.0086(9) 0.0000(9) C55 0.141(3) 0.0331(15) 0.080(2) 0.0020(14) 0.018(2) -0.0116(17) C56 0.114(3) 0.0415(16) 0.099(2) 0.0201(15) 0.0449(19) 0.0001(16) C57 0.0594(19) 0.0571(17) 0.0541(16) -0.0220(13) -0.0109(14) 0.0180(15) C58 0.065(2) 0.064(2) 0.094(2) -0.0327(19) -0.0306(18) 0.0259(16) C59 0.0447(15) 0.085(2) 0.0472(16) 0.0159(16) -0.0021(12) -0.0188(15) C60 0.0551(18) 0.119(3) 0.0391(15) 0.0289(16) -0.0050(13) -0.0293(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 1.9959(11) . yes Ni1 O2 1.9991(11) . yes Ni1 N1 2.1289(14) . yes Ni1 N2 2.1383(14) . yes Ni1 N4 2.2263(14) . yes Ni1 N3 2.2517(14) . yes O1 C34 1.2913(18) . ? O2 C7 1.2839(18) . ? N1 C1 1.298(2) . ? N1 C8 1.435(2) . ? N2 C28 1.299(2) . ? N2 C35 1.437(2) . ? N3 C58 1.448(3) . ? N3 C57 1.466(3) . ? N3 C55 1.489(3) . ? N4 C56 1.456(3) . ? N4 C59 1.467(3) . ? N4 C60 1.474(3) . ? C1 C2 1.436(2) . ? C1 H1 0.978(13) . ? C2 C3 1.407(2) . ? C2 C7 1.423(2) . ? C3 C4 1.363(2) . ? C3 H3 0.981(13) . ? C4 C5 1.396(3) . ? C4 H4 0.939(15) . ? C5 C6 1.371(2) . ? C5 H5 0.916(14) . ? C6 C7 1.433(2) . ? C6 C14 1.493(2) . ? C8 C13 1.379(2) . ? C8 C9 1.384(2) . ? C9 C10 1.382(2) . ? C9 H9 0.955(14) . ? C10 C11 1.378(3) . ? C10 H10 0.948(15) . ? C11 C12 1.372(3) . ? C11 H11 0.953(16) . ? C12 C13 1.384(3) . ? C12 H12 0.933(15) . ? C13 H13 0.921(14) . ? C14 C15 1.403(2) . ? C14 C27 1.415(2) . ? C15 C16 1.422(3) . ? C15 C20 1.431(2) . ? C16 C17 1.357(3) . ? C16 H16 0.942(16) . ? C17 C18 1.409(3) . ? C17 H17 0.961(18) . ? C18 C19 1.332(3) . ? C18 H18 0.924(19) . ? C19 C20 1.424(3) . ? C19 H19 0.937(17) . ? C20 C21 1.388(3) . ? C21 C22 1.384(3) . ? C21 H21 0.933(15) . ? C22 C23 1.428(3) . ? C22 C27 1.429(2) . ? C23 C24 1.346(3) . ? C23 H23 0.901(16) . ? C24 C25 1.398(3) . ? C24 H24 0.946(17) . ? C25 C26 1.354(3) . ? C25 H25 0.946(15) . ? C26 C27 1.422(2) . ? C26 H26 0.934(14) . ? C28 C29 1.436(2) . ? C28 H28 0.962(14) . ? C29 C30 1.404(2) . ? C29 C34 1.425(2) . ? C30 C31 1.357(2) . ? C30 H30 0.929(15) . ? C31 C32 1.394(2) . ? C31 H31 0.945(15) . ? C32 C33 1.372(2) . ? C32 H32 0.929(15) . ? C33 C34 1.434(2) . ? C33 C41 1.497(2) . ? C35 C40 1.373(2) . ? C35 C36 1.377(2) . ? C36 C37 1.385(3) . ? C36 H36 0.937(16) . ? C37 C38 1.364(3) . ? C37 H37 0.985(18) . ? C38 C39 1.373(3) . ? C38 H38 0.915(17) . ? C39 C40 1.380(2) . ? C39 H39 0.948(16) . ? C40 H40 0.930(14) . ? C41 C54 1.403(2) . ? C41 C42 1.405(2) . ? C42 C43 1.424(2) . ? C42 C47 1.434(2) . ? C43 C44 1.358(2) . ? C43 H43 0.931(13) . ? C44 C45 1.405(3) . ? C44 H44 1.003(15) . ? C45 C46 1.348(3) . ? C45 H45 0.908(15) . ? C46 C47 1.426(2) . ? C46 H46 0.946(15) . ? C47 C48 1.383(2) . ? C48 C49 1.388(2) . ? C48 H48 0.927(15) . ? C49 C50 1.423(2) . ? C49 C54 1.436(2) . ? C50 C51 1.342(3) . ? C50 H50 0.925(15) . ? C51 C52 1.415(3) . ? C51 H51 0.958(15) . ? C52 C53 1.346(3) . ? C52 H52 0.923(16) . ? C53 C54 1.425(2) . ? C53 H53 0.958(14) . ? C55 C56 1.451(4) . ? C55 H55A 1.066(18) . ? C55 H55B 1.03(3) . ? C56 H56A 0.969(19) . ? C56 H56B 1.14(3) . ? C57 H57A 0.92(2) . ? C57 H57B 0.98(2) . ? C57 H57C 0.990(18) . ? C58 H58A 0.981(18) . ? C58 H58B 0.980(17) . ? C58 H58C 0.98(2) . ? C59 H59A 0.968(17) . ? C59 H59B 0.96(2) . ? C59 H59C 0.946(18) . ? C60 H60A 0.95(2) . ? C60 H60B 0.97(3) . ? C60 H60C 0.997(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O2 172.87(5) . . yes O1 Ni1 N1 96.84(5) . . yes O2 Ni1 N1 87.67(5) . . yes O1 Ni1 N2 87.51(5) . . yes O2 Ni1 N2 97.70(5) . . yes N1 Ni1 N2 94.10(5) . . yes O1 Ni1 N4 92.10(5) . . yes O2 Ni1 N4 82.84(5) . . yes N1 Ni1 N4 168.98(6) . . yes N2 Ni1 N4 92.71(6) . . yes O1 Ni1 N3 84.20(5) . . yes O2 Ni1 N3 90.19(5) . . yes N1 Ni1 N3 91.34(5) . . yes N2 Ni1 N3 170.57(6) . . yes N4 Ni1 N3 83.13(6) . . yes C34 O1 Ni1 133.18(11) . . ? C7 O2 Ni1 133.09(11) . . ? C1 N1 C8 113.69(15) . . ? C1 N1 Ni1 123.72(12) . . ? C8 N1 Ni1 122.59(11) . . ? C28 N2 C35 113.57(15) . . ? C28 N2 Ni1 123.64(12) . . ? C35 N2 Ni1 122.79(11) . . ? C58 N3 C57 107.7(2) . . ? C58 N3 C55 112.4(2) . . ? C57 N3 C55 107.1(2) . . ? C58 N3 Ni1 114.07(14) . . ? C57 N3 Ni1 114.20(13) . . ? C55 N3 Ni1 101.08(13) . . ? C56 N4 C59 112.2(2) . . ? C56 N4 C60 107.6(2) . . ? C59 N4 C60 105.9(2) . . ? C56 N4 Ni1 103.85(14) . . ? C59 N4 Ni1 113.22(13) . . ? C60 N4 Ni1 114.06(14) . . ? N1 C1 C2 128.74(17) . . ? N1 C1 H1 117.4(8) . . ? C2 C1 H1 113.8(8) . . ? C3 C2 C7 119.75(16) . . ? C3 C2 C1 117.16(16) . . ? C7 C2 C1 123.06(16) . . ? C4 C3 C2 121.78(19) . . ? C4 C3 H3 120.4(8) . . ? C2 C3 H3 117.8(8) . . ? C3 C4 C5 118.57(19) . . ? C3 C4 H4 120.8(10) . . ? C5 C4 H4 120.6(10) . . ? C6 C5 C4 122.35(19) . . ? C6 C5 H5 117.6(10) . . ? C4 C5 H5 120.0(10) . . ? C5 C6 C7 119.86(17) . . ? C5 C6 C14 121.74(16) . . ? C7 C6 C14 118.38(15) . . ? O2 C7 C2 123.38(15) . . ? O2 C7 C6 119.31(16) . . ? C2 C7 C6 117.30(16) . . ? C13 C8 C9 118.76(18) . . ? C13 C8 N1 122.36(17) . . ? C9 C8 N1 118.77(16) . . ? C10 C9 C8 120.4(2) . . ? C10 C9 H9 119.3(9) . . ? C8 C9 H9 120.2(9) . . ? C11 C10 C9 120.3(2) . . ? C11 C10 H10 121.6(10) . . ? C9 C10 H10 118.1(10) . . ? C12 C11 C10 119.6(2) . . ? C12 C11 H11 120.1(10) . . ? C10 C11 H11 120.3(10) . . ? C11 C12 C13 120.2(2) . . ? C11 C12 H12 121.1(10) . . ? C13 C12 H12 118.7(10) . . ? C8 C13 C12 120.7(2) . . ? C8 C13 H13 119.1(10) . . ? C12 C13 H13 120.2(10) . . ? C15 C14 C27 119.79(17) . . ? C15 C14 C6 120.95(16) . . ? C27 C14 C6 119.24(16) . . ? C14 C15 C16 122.19(19) . . ? C14 C15 C20 119.87(18) . . ? C16 C15 C20 117.94(19) . . ? C17 C16 C15 120.6(2) . . ? C17 C16 H16 120.6(11) . . ? C15 C16 H16 118.9(11) . . ? C16 C17 C18 120.9(3) . . ? C16 C17 H17 118.7(12) . . ? C18 C17 H17 120.4(12) . . ? C19 C18 C17 120.7(3) . . ? C19 C18 H18 118.1(13) . . ? C17 C18 H18 121.1(13) . . ? C18 C19 C20 120.9(3) . . ? C18 C19 H19 123.8(12) . . ? C20 C19 H19 115.1(12) . . ? C21 C20 C19 121.9(2) . . ? C21 C20 C15 119.20(19) . . ? C19 C20 C15 118.9(2) . . ? C22 C21 C20 122.0(2) . . ? C22 C21 H21 118.1(10) . . ? C20 C21 H21 120.0(10) . . ? C21 C22 C23 122.5(2) . . ? C21 C22 C27 119.28(19) . . ? C23 C22 C27 118.3(2) . . ? C24 C23 C22 121.5(2) . . ? C24 C23 H23 121.1(11) . . ? C22 C23 H23 117.4(11) . . ? C23 C24 C25 120.1(2) . . ? C23 C24 H24 119.6(11) . . ? C25 C24 H24 120.3(11) . . ? C26 C25 C24 121.0(2) . . ? C26 C25 H25 115.7(10) . . ? C24 C25 H25 123.3(10) . . ? C25 C26 C27 121.2(2) . . ? C25 C26 H26 120.3(10) . . ? C27 C26 H26 118.5(10) . . ? C14 C27 C26 122.37(18) . . ? C14 C27 C22 119.73(18) . . ? C26 C27 C22 117.89(18) . . ? N2 C28 C29 129.08(18) . . ? N2 C28 H28 116.8(9) . . ? C29 C28 H28 114.1(9) . . ? C30 C29 C34 119.59(17) . . ? C30 C29 C28 117.49(17) . . ? C34 C29 C28 122.91(17) . . ? C31 C30 C29 122.33(19) . . ? C31 C30 H30 121.0(10) . . ? C29 C30 H30 116.6(10) . . ? C30 C31 C32 118.7(2) . . ? C30 C31 H31 121.4(9) . . ? C32 C31 H31 119.9(9) . . ? C33 C32 C31 121.97(19) . . ? C33 C32 H32 117.7(10) . . ? C31 C32 H32 120.3(10) . . ? C32 C33 C34 120.36(17) . . ? C32 C33 C41 122.02(16) . . ? C34 C33 C41 117.62(15) . . ? O1 C34 C29 123.43(16) . . ? O1 C34 C33 119.50(15) . . ? C29 C34 C33 117.07(16) . . ? C40 C35 C36 118.97(19) . . ? C40 C35 N2 119.20(17) . . ? C36 C35 N2 121.75(18) . . ? C35 C36 C37 120.0(2) . . ? C35 C36 H36 118.7(10) . . ? C37 C36 H36 121.3(11) . . ? C38 C37 C36 120.7(2) . . ? C38 C37 H37 121.0(11) . . ? C36 C37 H37 118.3(11) . . ? C37 C38 C39 119.5(2) . . ? C37 C38 H38 119.7(11) . . ? C39 C38 H38 120.8(11) . . ? C38 C39 C40 120.0(2) . . ? C38 C39 H39 121.4(10) . . ? C40 C39 H39 118.6(10) . . ? C35 C40 C39 120.8(2) . . ? C35 C40 H40 121.7(9) . . ? C39 C40 H40 117.5(9) . . ? C54 C41 C42 120.03(16) . . ? C54 C41 C33 120.49(16) . . ? C42 C41 C33 119.34(16) . . ? C41 C42 C43 122.52(17) . . ? C41 C42 C47 119.48(17) . . ? C43 C42 C47 117.95(17) . . ? C44 C43 C42 121.47(19) . . ? C44 C43 H43 118.6(9) . . ? C42 C43 H43 119.9(9) . . ? C43 C44 C45 120.1(2) . . ? C43 C44 H44 119.6(10) . . ? C45 C44 H44 120.3(10) . . ? C46 C45 C44 120.9(2) . . ? C46 C45 H45 121.1(10) . . ? C44 C45 H45 118.0(10) . . ? C45 C46 C47 121.1(2) . . ? C45 C46 H46 122.1(9) . . ? C47 C46 H46 116.7(9) . . ? C48 C47 C46 122.31(18) . . ? C48 C47 C42 119.35(18) . . ? C46 C47 C42 118.32(18) . . ? C47 C48 C49 122.18(18) . . ? C47 C48 H48 119.4(10) . . ? C49 C48 H48 118.4(10) . . ? C48 C49 C50 122.56(18) . . ? C48 C49 C54 118.67(17) . . ? C50 C49 C54 118.76(18) . . ? C51 C50 C49 121.9(2) . . ? C51 C50 H50 120.5(10) . . ? C49 C50 H50 117.7(10) . . ? C50 C51 C52 119.5(2) . . ? C50 C51 H51 121.3(10) . . ? C52 C51 H51 119.2(10) . . ? C53 C52 C51 121.1(2) . . ? C53 C52 H52 120.6(11) . . ? C51 C52 H52 118.2(11) . . ? C52 C53 C54 121.6(2) . . ? C52 C53 H53 120.7(9) . . ? C54 C53 H53 117.7(9) . . ? C41 C54 C53 122.82(17) . . ? C41 C54 C49 120.05(17) . . ? C53 C54 C49 117.11(17) . . ? C56 C55 N3 114.8(2) . . ? C56 C55 H55A 111.0(10) . . ? N3 C55 H55A 104.2(10) . . ? C56 C55 H55B 104.8(19) . . ? N3 C55 H55B 108.4(18) . . ? H55A C55 H55B 114(2) . . ? C55 C56 N4 113.5(2) . . ? C55 C56 H56A 110.0(11) . . ? N4 C56 H56A 112.4(11) . . ? C55 C56 H56B 80.1(15) . . ? N4 C56 H56B 119.5(14) . . ? H56A C56 H56B 116.9(18) . . ? N3 C57 H57A 110.7(12) . . ? N3 C57 H57B 109.0(14) . . ? H57A C57 H57B 113.2(19) . . ? N3 C57 H57C 111.2(10) . . ? H57A C57 H57C 107.1(16) . . ? H57B C57 H57C 105.6(17) . . ? N3 C58 H58A 110.5(11) . . ? N3 C58 H58B 109.6(12) . . ? H58A C58 H58B 110.3(16) . . ? N3 C58 H58C 109.8(13) . . ? H58A C58 H58C 109.1(17) . . ? H58B C58 H58C 107.4(18) . . ? N4 C59 H59A 109.9(11) . . ? N4 C59 H59B 112.6(14) . . ? H59A C59 H59B 110.4(17) . . ? N4 C59 H59C 106.3(12) . . ? H59A C59 H59C 109.4(15) . . ? H59B C59 H59C 108.3(18) . . ? N4 C60 H60A 106.7(14) . . ? N4 C60 H60B 107.5(18) . . ? H60A C60 H60B 114(2) . . ? N4 C60 H60C 109.8(10) . . ? H60A C60 H60C 108.5(17) . . ? H60B C60 H60C 110(2) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 28.59 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 1.016 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.049 #============================================================================== data_8 _audit_creation_method SHELXL-97 _database_code_CSD 162674 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H44 N2 Ni O2' _chemical_formula_weight 619.46 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0050(5) _cell_length_b 10.1054(6) _cell_length_c 11.0123(7) _cell_angle_alpha 113.5190(10) _cell_angle_beta 97.4260(10) _cell_angle_gamma 97.6730(10) _cell_volume 793.01(8) _cell_formula_units_Z 1 _cell_measurement_temperature 93 _cell_measurement_reflns_used 7378 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.73 _exptl_crystal_description Rhomboid _exptl_crystal_colour 'Olive green' _exptl_crystal_size_max 0.370 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.185 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 330 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8648 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.73 _reflns_number_total 3382 _reflns_number_gt 3260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT v. 6.2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Direct methods' _atom_sites_solution_hydrogens 'Difference Fourier map' _refine_ls_hydrogen_treatment Unrestrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3382 _refine_ls_number_parameters 284 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0713 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 2.406 _refine_ls_restrained_S_all 2.406 _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 Ni Ni 0.5000 0.5000 0.5000 0.01128(9) Uani 1 2 d S . . O O 0.59964(12) 0.34782(10) 0.40598(10) 0.0157(2) Uani 1 1 d . . . N N 0.54624(14) 0.47327(12) 0.66225(11) 0.0121(2) Uani 1 1 d . . . C1 C 0.65023(17) 0.24594(14) 0.43835(14) 0.0127(3) Uani 1 1 d . . . C2 C 0.70566(19) 0.12999(15) 0.33922(15) 0.0169(3) Uani 1 1 d . . . C3 C 0.75939(19) 0.01951(15) 0.36754(15) 0.0183(3) Uani 1 1 d . . . C4 C 0.76203(19) 0.01881(15) 0.49498(16) 0.0189(3) Uani 1 1 d . . . C5 C 0.70919(19) 0.13048(15) 0.59264(15) 0.0165(3) Uani 1 1 d . . . C6 C 0.65323(17) 0.24604(14) 0.56711(14) 0.0130(3) Uani 1 1 d . . . C7 C 0.60673(17) 0.36351(14) 0.67273(14) 0.0134(3) Uani 1 1 d . . . C8 C 0.51712(18) 0.58212(14) 0.78765(13) 0.0127(3) Uani 1 1 d . . . C9 C 0.37350(18) 0.54994(14) 0.83977(14) 0.0145(3) Uani 1 1 d . . . C10 C 0.35205(19) 0.65904(16) 0.96086(14) 0.0174(3) Uani 1 1 d . . . C11 C 0.4663(2) 0.79392(16) 1.02521(15) 0.0192(3) Uani 1 1 d . . . C12 C 0.6048(2) 0.82347(16) 0.97055(15) 0.0183(3) Uani 1 1 d . . . C13 C 0.63310(18) 0.71821(14) 0.84999(14) 0.0146(3) Uani 1 1 d . . . C14 C 0.24281(19) 0.40456(15) 0.76460(15) 0.0176(3) Uani 1 1 d . . . C15 C 0.1258(2) 0.40338(19) 0.64258(17) 0.0259(4) Uani 1 1 d . . . C16 C 0.1350(2) 0.36640(18) 0.85581(18) 0.0235(3) Uani 1 1 d . . . C17 C 0.78783(19) 0.75176(15) 0.79206(15) 0.0176(3) Uani 1 1 d . . . C18 C 0.7925(2) 0.89347(18) 0.77123(19) 0.0256(4) Uani 1 1 d . . . C19 C 0.9548(2) 0.7598(2) 0.88099(19) 0.0275(4) Uani 1 1 d . . . H2 H 0.7036(19) 0.1304(15) 0.2525(16) 0.016(4) Uiso 1 1 d . . . H3 H 0.7919(19) -0.0536(17) 0.3013(16) 0.020(4) Uiso 1 1 d . . . H4 H 0.799(2) -0.0584(19) 0.5158(19) 0.037(5) Uiso 1 1 d . . . H5 H 0.7125(19) 0.1345(15) 0.6814(16) 0.019(4) Uiso 1 1 d . . . H7 H 0.6250(19) 0.3639(16) 0.7614(16) 0.016(4) Uiso 1 1 d . . . H10 H 0.257(2) 0.6430(16) 0.9975(16) 0.019(4) Uiso 1 1 d . . . H11 H 0.448(2) 0.8650(17) 1.1004(16) 0.020(4) Uiso 1 1 d . . . H12 H 0.681(2) 0.9168(18) 1.0145(17) 0.028(5) Uiso 1 1 d . . . H14 H 0.3091(18) 0.3300(15) 0.7336(15) 0.012(4) Uiso 1 1 d . . . H17 H 0.778(2) 0.6721(18) 0.7053(17) 0.027(4) Uiso 1 1 d . . . H15A H 0.190(2) 0.4208(19) 0.5825(18) 0.036(5) Uiso 1 1 d . . . H16A H 0.058(2) 0.4346(18) 0.8864(17) 0.027(4) Uiso 1 1 d . . . H18A H 0.896(2) 0.9117(18) 0.7321(17) 0.031(5) Uiso 1 1 d . . . H19A H 1.056(2) 0.7816(18) 0.8458(17) 0.030(4) Uiso 1 1 d . . . H15B H 0.058(2) 0.4791(18) 0.6708(16) 0.023(4) Uiso 1 1 d . . . H16B H 0.060(2) 0.268(2) 0.8029(18) 0.033(5) Uiso 1 1 d . . . H18B H 0.689(3) 0.8841(19) 0.7092(19) 0.041(5) Uiso 1 1 d . . . H19B H 0.966(2) 0.838(2) 0.978(2) 0.040(5) Uiso 1 1 d . . . H15C H 0.042(2) 0.312(2) 0.5939(18) 0.036(5) Uiso 1 1 d . . . H16C H 0.209(2) 0.3736(18) 0.9366(18) 0.028(5) Uiso 1 1 d . . . H18C H 0.796(2) 0.977(2) 0.8558(19) 0.033(5) Uiso 1 1 d . . . H19C H 0.954(2) 0.669(2) 0.8891(18) 0.039(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.01522(15) 0.00985(13) 0.00967(14) 0.00424(10) 0.00318(10) 0.00447(10) O 0.0235(6) 0.0144(5) 0.0115(5) 0.0059(4) 0.0051(4) 0.0087(4) N 0.0140(6) 0.0105(5) 0.0108(6) 0.0035(5) 0.0027(5) 0.0023(5) C1 0.0109(7) 0.0109(6) 0.0146(7) 0.0046(6) 0.0006(6) 0.0014(5) C2 0.0200(8) 0.0158(7) 0.0146(8) 0.0052(6) 0.0054(6) 0.0047(6) C3 0.0206(8) 0.0133(7) 0.0190(8) 0.0031(6) 0.0065(7) 0.0072(6) C4 0.0204(8) 0.0143(7) 0.0253(8) 0.0107(6) 0.0048(7) 0.0065(6) C5 0.0180(8) 0.0156(7) 0.0180(8) 0.0090(6) 0.0043(6) 0.0039(6) C6 0.0113(7) 0.0119(6) 0.0152(7) 0.0061(6) 0.0014(6) 0.0010(5) C7 0.0131(7) 0.0147(7) 0.0130(7) 0.0072(6) 0.0020(6) 0.0016(6) C8 0.0173(7) 0.0133(6) 0.0084(7) 0.0051(6) 0.0009(6) 0.0059(6) C9 0.0167(7) 0.0150(6) 0.0136(7) 0.0074(6) 0.0022(6) 0.0057(6) C10 0.0187(8) 0.0217(7) 0.0150(7) 0.0088(6) 0.0063(6) 0.0086(6) C11 0.0252(8) 0.0187(7) 0.0107(7) 0.0014(6) 0.0032(6) 0.0100(6) C12 0.0215(8) 0.0135(7) 0.0151(8) 0.0026(6) -0.0005(6) 0.0033(6) C13 0.0168(7) 0.0145(6) 0.0123(7) 0.0061(6) 0.0001(6) 0.0041(6) C14 0.0184(8) 0.0150(7) 0.0196(8) 0.0059(6) 0.0080(6) 0.0043(6) C15 0.0221(9) 0.0294(9) 0.0213(9) 0.0096(7) 0.0021(7) -0.0051(8) C16 0.0256(9) 0.0220(8) 0.0283(9) 0.0139(7) 0.0118(8) 0.0059(7) C17 0.0201(8) 0.0140(7) 0.0149(8) 0.0035(6) 0.0022(6) 0.0002(6) C18 0.0243(9) 0.0245(8) 0.0326(10) 0.0179(8) 0.0046(8) 0.0016(7) C19 0.0203(9) 0.0360(10) 0.0343(10) 0.0224(9) 0.0062(8) 0.0070(7) _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 Ni O 1.8285(9) . yes Ni O 1.8285(9) 2_666 yes Ni N 1.9087(11) . yes Ni N 1.9087(11) 2_666 yes O C1 1.3107(15) . ? N C7 1.3074(16) . ? N C8 1.4528(16) . ? C1 C6 1.4147(19) . ? C1 C2 1.4159(18) . ? C2 C3 1.3785(19) . ? C2 H2 0.955(15) . ? C3 C4 1.404(2) . ? C3 H3 0.903(16) . ? C4 C5 1.373(2) . ? C4 H4 0.967(18) . ? C5 C6 1.4187(18) . ? C5 H5 0.959(15) . ? C6 C7 1.4242(18) . ? C7 H7 0.967(16) . ? C8 C13 1.4019(19) . ? C8 C9 1.4059(19) . ? C9 C10 1.3998(19) . ? C9 C14 1.528(2) . ? C10 C11 1.387(2) . ? C10 H10 0.932(16) . ? C11 C12 1.381(2) . ? C11 H11 0.897(16) . ? C12 C13 1.4003(19) . ? C12 H12 0.949(17) . ? C13 C17 1.5235(19) . ? C14 C15 1.531(2) . ? C14 C16 1.5319(19) . ? C14 H14 0.956(14) . ? C15 H15A 0.945(19) . ? C15 H15B 0.969(17) . ? C15 H15C 0.968(18) . ? C16 H16A 0.972(17) . ? C16 H16B 0.989(18) . ? C16 H16C 0.972(18) . ? C17 C19 1.524(2) . ? C17 C18 1.5345(19) . ? C17 H17 0.957(17) . ? C18 H18A 1.009(18) . ? C18 H18B 0.97(2) . ? C18 H18C 0.969(18) . ? C19 H19A 0.977(17) . ? C19 H19B 1.03(2) . ? C19 H19C 0.955(19) . ? 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 O Ni O 180.0 . 2_666 yes O Ni N 93.03(4) . . yes O Ni N 86.97(4) 2_666 . yes O Ni N 86.97(4) . 2_666 yes O Ni N 93.03(4) 2_666 2_666 yes N Ni N 180.0 . 2_666 yes C1 O Ni 130.01(9) . . ? C7 N C8 114.96(11) . . ? C7 N Ni 125.34(9) . . ? C8 N Ni 119.69(8) . . ? O C1 C6 123.54(12) . . ? O C1 C2 118.18(12) . . ? C6 C1 C2 118.28(12) . . ? C3 C2 C1 120.63(13) . . ? C3 C2 H2 121.3(9) . . ? C1 C2 H2 118.0(9) . . ? C2 C3 C4 121.31(13) . . ? C2 C3 H3 118.1(10) . . ? C4 C3 H3 120.6(10) . . ? C5 C4 C3 118.98(13) . . ? C5 C4 H4 119.0(11) . . ? C3 C4 H4 122.0(11) . . ? C4 C5 C6 121.26(13) . . ? C4 C5 H5 120.9(9) . . ? C6 C5 H5 117.8(9) . . ? C1 C6 C5 119.54(12) . . ? C1 C6 C7 120.75(11) . . ? C5 C6 C7 119.67(12) . . ? N C7 C6 126.27(12) . . ? N C7 H7 116.8(9) . . ? C6 C7 H7 116.9(9) . . ? C13 C8 C9 122.60(12) . . ? C13 C8 N 117.70(12) . . ? C9 C8 N 119.68(12) . . ? C10 C9 C8 117.13(13) . . ? C10 C9 C14 121.45(12) . . ? C8 C9 C14 121.37(12) . . ? C11 C10 C9 121.28(13) . . ? C11 C10 H10 118.9(10) . . ? C9 C10 H10 119.8(10) . . ? C12 C11 C10 120.35(13) . . ? C12 C11 H11 118.9(10) . . ? C10 C11 H11 120.7(10) . . ? C11 C12 C13 120.85(14) . . ? C11 C12 H12 119.7(10) . . ? C13 C12 H12 119.5(10) . . ? C12 C13 C8 117.77(13) . . ? C12 C13 C17 120.19(13) . . ? C8 C13 C17 122.03(12) . . ? C9 C14 C15 111.35(12) . . ? C9 C14 C16 113.14(13) . . ? C15 C14 C16 110.38(13) . . ? C9 C14 H14 105.7(9) . . ? C15 C14 H14 109.0(9) . . ? C16 C14 H14 107.0(8) . . ? C14 C15 H15A 111.3(11) . . ? C14 C15 H15B 111.0(10) . . ? H15A C15 H15B 107.7(14) . . ? C14 C15 H15C 112.2(11) . . ? H15A C15 H15C 109.3(15) . . ? H15B C15 H15C 105.1(14) . . ? C14 C16 H16A 111.4(10) . . ? C14 C16 H16B 109.0(10) . . ? H16A C16 H16B 106.1(14) . . ? C14 C16 H16C 110.7(10) . . ? H16A C16 H16C 106.5(14) . . ? H16B C16 H16C 113.1(14) . . ? C13 C17 C19 110.84(12) . . ? C13 C17 C18 111.98(12) . . ? C19 C17 C18 110.84(13) . . ? C13 C17 H17 107.7(10) . . ? C19 C17 H17 107.7(10) . . ? C18 C17 H17 107.5(10) . . ? C17 C18 H18A 109.8(10) . . ? C17 C18 H18B 110.0(11) . . ? H18A C18 H18B 108.8(15) . . ? C17 C18 H18C 110.6(10) . . ? H18A C18 H18C 110.4(14) . . ? H18B C18 H18C 107.2(15) . . ? C17 C19 H19A 112.2(10) . . ? C17 C19 H19B 110.3(11) . . ? H19A C19 H19B 109.3(15) . . ? C17 C19 H19C 110.5(11) . . ? H19A C19 H19C 108.8(15) . . ? H19B C19 H19C 105.4(15) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 27.73 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 0.471 _refine_diff_density_min -0.267 _refine_diff_density_rms 0.053 #===END #===END data_7 _audit_creation_method SHELXL-97 _database_code_CSD 212728 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 N2 Ni O' _chemical_formula_weight 571.38 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.0982(13) _cell_length_b 14.4000(10) _cell_length_c 22.3830(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5833.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 5843 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 23.30 _exptl_crystal_description Blade _exptl_crystal_colour 'Dichroic yellow/brown' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans at 4 phi settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47311 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0276 _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 -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 23.32 _reflns_number_total 4213 _reflns_number_gt 3431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT v 6.01' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary direct _atom_sites_solution_secondary direct _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment unrestrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4213 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0527 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 1.913 _refine_ls_restrained_S_all 1.913 _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 Ni Ni 0.184162(14) 0.054172(17) 0.427685(12) 0.02187(9) Uani 1 1 d . . . N1 N 0.25793(9) 0.02802(10) 0.37052(8) 0.0196(4) Uani 1 1 d . . . N2 N 0.10882(10) 0.08221(12) 0.48116(8) 0.0262(5) Uani 1 1 d . . . O O 0.10477(7) 0.01676(9) 0.37682(6) 0.0217(3) Uani 1 1 d . . . C1 C 0.25497(13) 0.09966(18) 0.48520(11) 0.0273(6) Uani 1 1 d . . . C2 C 0.05834(13) 0.10305(15) 0.50817(10) 0.0261(5) Uani 1 1 d . . . C3 C -0.00594(15) 0.1325(2) 0.54195(13) 0.0343(6) Uani 1 1 d . . . C4 C 0.33637(10) 0.03505(14) 0.38413(9) 0.0213(5) Uani 1 1 d . . . C5 C 0.37383(11) 0.11569(14) 0.36713(9) 0.0215(5) Uani 1 1 d . . . C6 C 0.44840(12) 0.12267(16) 0.38305(10) 0.0263(6) Uani 1 1 d . . . C7 C 0.48272(12) 0.05366(16) 0.41505(9) 0.0279(6) Uani 1 1 d . . . C8 C 0.44451(12) -0.02507(15) 0.43119(10) 0.0255(5) Uani 1 1 d . . . C9 C 0.37044(11) -0.03641(14) 0.41617(9) 0.0231(5) Uani 1 1 d . . . C10 C 0.33653(13) 0.19507(15) 0.33462(10) 0.0265(6) Uani 1 1 d . . . C11 C 0.35879(17) 0.1992(2) 0.26948(12) 0.0362(7) Uani 1 1 d . . . C12 C 0.35155(15) 0.28794(16) 0.36517(13) 0.0309(6) Uani 1 1 d . . . C13 C 0.32911(12) -0.12440(14) 0.43248(10) 0.0287(6) Uani 1 1 d . . . C14 C 0.34025(16) -0.19721(19) 0.38389(15) 0.0407(7) Uani 1 1 d . . . C15 C 0.34984(16) -0.1624(2) 0.49368(13) 0.0406(7) Uani 1 1 d . . . C16 C 0.24326(12) 0.00975(14) 0.31495(11) 0.0219(5) Uani 1 1 d . . . C17 C 0.17303(10) 0.00344(13) 0.28627(9) 0.0194(5) Uani 1 1 d . . . C18 C 0.17110(13) -0.01042(14) 0.22435(10) 0.0237(5) Uani 1 1 d . . . C19 C 0.10608(12) -0.01888(15) 0.19415(11) 0.0261(6) Uani 1 1 d . . . C20 C 0.03980(13) -0.01583(14) 0.22637(10) 0.0247(6) Uani 1 1 d . . . C21 C 0.03780(11) -0.00389(13) 0.28729(9) 0.0201(5) Uani 1 1 d . . . C22 C 0.10575(11) 0.00648(13) 0.31940(10) 0.0204(5) Uani 1 1 d . . . C23 C -0.03437(11) -0.00532(14) 0.31978(9) 0.0206(5) Uani 1 1 d . . . C24 C -0.05987(11) 0.07424(14) 0.35053(9) 0.0214(5) Uani 1 1 d . . . C25 C -0.02008(13) 0.15991(15) 0.35218(10) 0.0264(6) Uani 1 1 d . . . C26 C -0.04733(13) 0.23592(17) 0.37982(11) 0.0307(6) Uani 1 1 d . . . C27 C -0.11616(13) 0.23255(17) 0.41011(11) 0.0334(6) Uani 1 1 d . . . C28 C -0.15561(13) 0.15315(16) 0.41051(10) 0.0300(6) Uani 1 1 d . . . C29 C -0.13011(11) 0.07174(14) 0.38063(9) 0.0236(5) Uani 1 1 d . . . C30 C -0.17174(12) -0.00894(15) 0.37880(10) 0.0245(5) Uani 1 1 d . . . C31 C -0.14794(11) -0.08810(14) 0.34916(9) 0.0228(5) Uani 1 1 d . . . C32 C -0.19101(14) -0.17118(16) 0.34769(11) 0.0291(6) Uani 1 1 d . . . C33 C -0.16708(12) -0.24880(17) 0.32030(11) 0.0320(6) Uani 1 1 d . . . C34 C -0.09746(13) -0.24854(17) 0.29168(11) 0.0289(6) Uani 1 1 d . . . C35 C -0.05467(13) -0.17121(15) 0.29072(10) 0.0255(6) Uani 1 1 d . . . C36 C -0.07779(11) -0.08673(14) 0.31911(9) 0.0213(5) Uani 1 1 d . . . H1A H 0.2292(10) 0.1248(13) 0.5190(9) 0.021(6) Uiso 1 1 d . . . H1B H 0.2877(11) 0.0485(15) 0.5012(9) 0.038(6) Uiso 1 1 d . . . H1C H 0.2868(11) 0.1464(13) 0.4663(8) 0.026(6) Uiso 1 1 d . . . H3A H -0.0275(12) 0.0836(16) 0.5655(11) 0.055(8) Uiso 1 1 d . . . H3B H 0.0129(12) 0.1825(16) 0.5660(11) 0.049(8) Uiso 1 1 d . . . H3C H -0.0440(13) 0.1538(16) 0.5127(11) 0.057(8) Uiso 1 1 d . . . H6 H 0.4755(10) 0.1771(12) 0.3717(8) 0.019(5) Uiso 1 1 d . . . H7 H 0.5347(11) 0.0592(12) 0.4260(8) 0.025(5) Uiso 1 1 d . . . H8 H 0.4678(10) -0.0731(12) 0.4536(8) 0.018(5) Uiso 1 1 d . . . H10 H 0.2875(10) 0.1849(11) 0.3374(7) 0.006(5) Uiso 1 1 d . . . H11A H 0.3442(11) 0.1428(16) 0.2457(9) 0.041(7) Uiso 1 1 d . . . H11B H 0.4093(12) 0.2060(14) 0.2664(9) 0.033(7) Uiso 1 1 d . . . H11C H 0.3377(10) 0.2515(15) 0.2492(9) 0.030(6) Uiso 1 1 d . . . H12A H 0.4034(12) 0.3044(13) 0.3593(8) 0.029(6) Uiso 1 1 d . . . H12B H 0.3198(11) 0.3370(13) 0.3489(8) 0.022(5) Uiso 1 1 d . . . H12C H 0.3424(11) 0.2876(14) 0.4087(10) 0.039(7) Uiso 1 1 d . . . H13 H 0.2776(10) -0.1120(12) 0.4346(8) 0.017(5) Uiso 1 1 d . . . H14A H 0.3917(15) -0.2118(16) 0.3793(10) 0.057(8) Uiso 1 1 d . . . H14B H 0.3143(12) -0.2530(15) 0.3917(9) 0.034(6) Uiso 1 1 d . . . H14C H 0.3244(12) -0.1755(15) 0.3427(10) 0.042(7) Uiso 1 1 d . . . H15A H 0.4002(13) -0.1849(15) 0.4922(9) 0.043(7) Uiso 1 1 d . . . H15B H 0.3446(12) -0.1145(17) 0.5279(11) 0.056(8) Uiso 1 1 d . . . H15C H 0.3190(13) -0.2147(17) 0.5033(10) 0.053(7) Uiso 1 1 d . . . H16 H 0.2841(10) 0.0015(11) 0.2904(8) 0.013(5) Uiso 1 1 d . . . H18 H 0.2153(10) -0.0136(12) 0.2029(8) 0.021(6) Uiso 1 1 d . . . H19 H 0.1051(10) -0.0295(12) 0.1538(9) 0.018(6) Uiso 1 1 d . . . H20 H -0.0045(10) -0.0233(12) 0.2060(8) 0.019(6) Uiso 1 1 d . . . H25 H 0.0249(10) 0.1630(11) 0.3332(8) 0.014(5) Uiso 1 1 d . . . H26 H -0.0204(11) 0.2913(13) 0.3792(8) 0.023(6) Uiso 1 1 d . . . H27 H -0.1346(11) 0.2862(14) 0.4315(9) 0.029(6) Uiso 1 1 d . . . H28 H -0.2010(11) 0.1477(13) 0.4307(8) 0.026(6) Uiso 1 1 d . . . H30 H -0.2162(10) -0.0113(12) 0.3987(8) 0.014(5) Uiso 1 1 d . . . H32 H -0.2334(11) -0.1700(13) 0.3664(9) 0.024(6) Uiso 1 1 d . . . H33 H -0.1959(10) -0.3062(13) 0.3214(8) 0.026(6) Uiso 1 1 d . . . H34 H -0.0815(10) -0.3014(13) 0.2748(8) 0.018(6) Uiso 1 1 d . . . H35 H -0.0097(10) -0.1718(11) 0.2711(8) 0.013(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.01759(15) 0.02427(15) 0.02374(16) -0.00125(13) 0.00065(13) 0.00068(12) N1 0.0177(10) 0.0168(10) 0.0243(11) -0.0006(8) -0.0015(8) -0.0013(7) N2 0.0245(11) 0.0297(11) 0.0245(11) 0.0001(9) -0.0033(9) -0.0010(9) O 0.0190(8) 0.0254(8) 0.0205(9) -0.0017(7) 0.0011(7) 0.0008(6) C1 0.0241(14) 0.0323(15) 0.0255(16) -0.0008(13) 0.0044(12) 0.0002(12) C2 0.0274(14) 0.0273(14) 0.0237(14) 0.0018(11) -0.0027(12) -0.0015(11) C3 0.0311(16) 0.0388(18) 0.0328(17) 0.0008(15) 0.0079(14) 0.0040(13) C4 0.0155(12) 0.0258(13) 0.0225(12) -0.0070(10) 0.0021(9) -0.0003(9) C5 0.0171(12) 0.0257(13) 0.0215(13) -0.0051(10) 0.0026(10) -0.0004(10) C6 0.0247(14) 0.0253(13) 0.0288(14) -0.0076(12) 0.0055(11) -0.0057(11) C7 0.0180(13) 0.0382(14) 0.0277(15) -0.0105(12) -0.0034(11) -0.0005(12) C8 0.0233(13) 0.0257(14) 0.0276(14) -0.0032(12) -0.0041(11) 0.0047(10) C9 0.0173(12) 0.0253(13) 0.0265(14) -0.0064(11) -0.0006(10) 0.0015(9) C10 0.0179(14) 0.0291(14) 0.0324(15) -0.0001(11) 0.0024(11) -0.0053(10) C11 0.0368(18) 0.0405(18) 0.0312(17) 0.0048(14) -0.0012(14) -0.0070(14) C12 0.0277(16) 0.0252(15) 0.0398(19) 0.0018(13) -0.0007(14) -0.0033(12) C13 0.0194(14) 0.0249(13) 0.0417(15) 0.0000(12) -0.0052(12) 0.0016(10) C14 0.0289(17) 0.0293(16) 0.064(2) -0.0112(15) -0.0055(15) 0.0003(13) C15 0.0328(17) 0.0339(17) 0.055(2) 0.0089(15) -0.0091(15) -0.0054(14) C16 0.0184(13) 0.0162(12) 0.0312(16) -0.0002(11) 0.0059(12) -0.0006(10) C17 0.0175(13) 0.0166(11) 0.0241(13) 0.0016(10) 0.0010(10) 0.0013(9) C18 0.0200(14) 0.0239(12) 0.0272(15) 0.0020(11) 0.0054(11) -0.0004(10) C19 0.0285(15) 0.0306(14) 0.0193(15) -0.0004(11) -0.0012(12) 0.0017(10) C20 0.0201(14) 0.0237(13) 0.0303(16) 0.0014(11) -0.0057(12) -0.0003(10) C21 0.0204(13) 0.0154(11) 0.0245(14) 0.0022(10) -0.0001(10) 0.0009(9) C22 0.0219(13) 0.0140(12) 0.0254(14) 0.0010(10) -0.0010(11) 0.0015(9) C23 0.0163(12) 0.0246(12) 0.0209(13) 0.0035(10) -0.0050(10) 0.0029(10) C24 0.0179(12) 0.0253(13) 0.0211(13) 0.0029(10) -0.0053(10) 0.0019(10) C25 0.0182(14) 0.0295(14) 0.0315(15) 0.0015(11) -0.0015(12) 0.0019(11) C26 0.0243(14) 0.0250(14) 0.0429(16) -0.0021(13) -0.0056(12) 0.0027(12) C27 0.0300(15) 0.0323(15) 0.0378(16) -0.0070(12) -0.0027(12) 0.0104(12) C28 0.0219(14) 0.0376(16) 0.0303(15) 0.0004(12) 0.0013(12) 0.0065(12) C29 0.0197(12) 0.0293(14) 0.0217(13) 0.0015(11) -0.0026(10) 0.0057(10) C30 0.0137(13) 0.0382(15) 0.0217(13) 0.0054(11) 0.0005(10) 0.0001(11) C31 0.0189(12) 0.0265(13) 0.0230(13) 0.0042(11) -0.0037(10) 0.0013(10) C32 0.0199(14) 0.0359(15) 0.0313(15) 0.0064(12) 0.0015(12) -0.0043(12) C33 0.0299(15) 0.0285(14) 0.0374(15) 0.0045(12) -0.0012(13) -0.0085(12) C34 0.0293(15) 0.0236(14) 0.0338(16) -0.0015(12) -0.0018(12) 0.0024(12) C35 0.0189(14) 0.0306(15) 0.0271(14) 0.0016(11) -0.0015(11) 0.0013(11) C36 0.0169(12) 0.0264(13) 0.0206(13) 0.0034(10) -0.0052(10) 0.0023(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N2 1.8588(19) . yes Ni N1 1.8872(16) . yes Ni O 1.9107(13) . yes Ni C1 1.931(2) . yes N1 C16 1.299(3) . ? N1 C4 1.455(2) . ? N2 C2 1.136(3) . ? O C22 1.294(2) . ? C1 H1A 0.96(2) . ? C1 H1B 1.01(2) . ? C1 H1C 0.98(2) . ? C2 C3 1.451(3) . ? C3 H3A 0.96(2) . ? C3 H3B 0.96(2) . ? C3 H3C 1.00(2) . ? C4 C9 1.398(3) . ? C4 C5 1.397(3) . ? C5 C6 1.399(3) . ? C5 C10 1.514(3) . ? C6 C7 1.373(3) . ? C6 H6 0.958(18) . ? C7 C8 1.376(3) . ? C7 H7 0.976(18) . ? C8 C9 1.392(3) . ? C8 H8 0.953(18) . ? C9 C13 1.516(3) . ? C10 C12 1.526(3) . ? C10 C11 1.514(3) . ? C10 H10 0.902(17) . ? C11 H11A 1.01(2) . ? C11 H11B 0.92(2) . ? C11 H11C 0.96(2) . ? C12 H12A 0.98(2) . ? C12 H12B 0.981(19) . ? C12 H12C 0.99(2) . ? C13 C15 1.522(3) . ? C13 C14 1.524(3) . ? C13 H13 0.950(18) . ? C14 H14A 0.96(3) . ? C14 H14B 0.95(2) . ? C14 H14C 1.01(2) . ? C15 H15A 0.97(2) . ? C15 H15B 1.03(2) . ? C15 H15C 0.96(2) . ? C16 C17 1.427(3) . ? C16 H16 0.928(18) . ? C17 C18 1.401(3) . ? C17 C22 1.426(3) . ? C18 C19 1.362(3) . ? C18 H18 0.934(18) . ? C19 C20 1.400(3) . ? C19 H19 0.916(19) . ? C20 C21 1.375(3) . ? C20 H20 0.928(18) . ? C21 C22 1.432(3) . ? C21 C23 1.495(3) . ? C23 C24 1.414(3) . ? C23 C36 1.411(3) . ? C24 C29 1.439(3) . ? C24 C25 1.429(3) . ? C25 C26 1.351(3) . ? C25 H25 0.919(18) . ? C26 C27 1.419(3) . ? C26 H26 0.935(19) . ? C27 C28 1.348(3) . ? C27 H27 0.97(2) . ? C28 C29 1.426(3) . ? C28 H28 0.940(19) . ? C29 C30 1.385(3) . ? C30 C31 1.387(3) . ? C30 H30 0.920(18) . ? C31 C36 1.437(3) . ? C31 C32 1.428(3) . ? C32 C33 1.346(3) . ? C32 H32 0.87(2) . ? C33 C34 1.414(3) . ? C33 H33 0.978(19) . ? C34 C35 1.357(3) . ? C34 H34 0.898(18) . ? C35 C36 1.435(3) . ? C35 H35 0.926(17) . ? 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 N2 Ni N1 177.34(7) . . yes N2 Ni O 83.87(6) . . yes N1 Ni O 94.12(6) . . yes N2 Ni C1 89.07(9) . . yes N1 Ni C1 92.88(9) . . yes O Ni C1 172.72(9) . . yes C16 N1 C4 114.45(17) . . ? C16 N1 Ni 123.03(15) . . ? C4 N1 Ni 122.29(13) . . ? C2 N2 Ni 171.95(18) . . ? C22 O Ni 127.87(13) . . ? Ni C1 H1A 109.3(11) . . ? Ni C1 H1B 112.2(12) . . ? H1A C1 H1B 106.3(16) . . ? Ni C1 H1C 109.5(11) . . ? H1A C1 H1C 111.5(16) . . ? H1B C1 H1C 108.0(16) . . ? N2 C2 C3 178.3(3) . . ? C2 C3 H3A 113.4(13) . . ? C2 C3 H3B 103.1(14) . . ? H3A C3 H3B 113(2) . . ? C2 C3 H3C 107.5(14) . . ? H3A C3 H3C 107.8(19) . . ? H3B C3 H3C 112.4(19) . . ? C9 C4 C5 122.51(19) . . ? C9 C4 N1 119.11(17) . . ? C5 C4 N1 118.30(18) . . ? C6 C5 C4 117.3(2) . . ? C6 C5 C10 119.88(19) . . ? C4 C5 C10 122.82(18) . . ? C7 C6 C5 121.1(2) . . ? C7 C6 H6 119.8(11) . . ? C5 C6 H6 119.1(11) . . ? C6 C7 C8 120.4(2) . . ? C6 C7 H7 120.6(11) . . ? C8 C7 H7 119.0(11) . . ? C7 C8 C9 121.1(2) . . ? C7 C8 H8 120.9(11) . . ? C9 C8 H8 117.9(11) . . ? C4 C9 C8 117.55(19) . . ? C4 C9 C13 121.42(18) . . ? C8 C9 C13 121.01(19) . . ? C5 C10 C12 111.52(19) . . ? C5 C10 C11 112.0(2) . . ? C12 C10 C11 110.4(2) . . ? C5 C10 H10 106.5(11) . . ? C12 C10 H10 106.6(11) . . ? C11 C10 H10 109.6(11) . . ? C10 C11 H11A 114.1(12) . . ? C10 C11 H11B 109.9(13) . . ? H11A C11 H11B 107.8(18) . . ? C10 C11 H11C 112.4(12) . . ? H11A C11 H11C 106.2(17) . . ? H11B C11 H11C 106.1(17) . . ? C10 C12 H12A 108.9(11) . . ? C10 C12 H12B 111.1(11) . . ? H12A C12 H12B 109.7(16) . . ? C10 C12 H12C 114.0(12) . . ? H12A C12 H12C 107.2(17) . . ? H12B C12 H12C 105.8(17) . . ? C9 C13 C15 113.29(19) . . ? C9 C13 C14 109.7(2) . . ? C15 C13 C14 111.3(2) . . ? C9 C13 H13 109.8(10) . . ? C15 C13 H13 105.4(11) . . ? C14 C13 H13 107.1(11) . . ? C13 C14 H14A 110.8(14) . . ? C13 C14 H14B 112.7(13) . . ? H14A C14 H14B 108.4(19) . . ? C13 C14 H14C 113.5(12) . . ? H14A C14 H14C 104.2(19) . . ? H14B C14 H14C 106.9(18) . . ? C13 C15 H15A 108.8(13) . . ? C13 C15 H15B 113.9(13) . . ? H15A C15 H15B 109.6(18) . . ? C13 C15 H15C 109.9(14) . . ? H15A C15 H15C 106.9(19) . . ? H15B C15 H15C 107.6(19) . . ? N1 C16 C17 128.7(2) . . ? N1 C16 H16 115.4(11) . . ? C17 C16 H16 115.8(11) . . ? C18 C17 C22 119.83(19) . . ? C18 C17 C16 118.5(2) . . ? C22 C17 C16 121.65(19) . . ? C19 C18 C17 121.7(2) . . ? C19 C18 H18 118.7(12) . . ? C17 C18 H18 119.6(12) . . ? C20 C19 C18 118.8(2) . . ? C20 C19 H19 119.8(12) . . ? C18 C19 H19 121.4(12) . . ? C21 C20 C19 122.5(2) . . ? C21 C20 H20 118.6(12) . . ? C19 C20 H20 118.9(12) . . ? C20 C21 C22 119.2(2) . . ? C20 C21 C23 120.25(19) . . ? C22 C21 C23 120.50(18) . . ? O C22 C17 122.11(18) . . ? O C22 C21 119.91(18) . . ? C17 C22 C21 117.97(19) . . ? C24 C23 C36 119.76(18) . . ? C24 C23 C21 120.72(18) . . ? C36 C23 C21 119.52(18) . . ? C23 C24 C29 119.74(18) . . ? C23 C24 C25 123.20(19) . . ? C29 C24 C25 117.04(19) . . ? C26 C25 C24 121.8(2) . . ? C26 C25 H25 119.7(11) . . ? C24 C25 H25 118.4(11) . . ? C25 C26 C27 120.8(2) . . ? C25 C26 H26 119.6(12) . . ? C27 C26 H26 119.6(12) . . ? C28 C27 C26 119.8(2) . . ? C28 C27 H27 119.5(12) . . ? C26 C27 H27 120.7(12) . . ? C27 C28 C29 121.5(2) . . ? C27 C28 H28 122.4(12) . . ? C29 C28 H28 116.1(12) . . ? C30 C29 C24 119.18(19) . . ? C30 C29 C28 121.8(2) . . ? C24 C29 C28 119.0(2) . . ? C31 C30 C29 122.3(2) . . ? C31 C30 H30 118.2(11) . . ? C29 C30 H30 119.5(11) . . ? C30 C31 C36 119.13(19) . . ? C30 C31 C32 122.0(2) . . ? C36 C31 C32 118.9(2) . . ? C33 C32 C31 122.0(2) . . ? C33 C32 H32 121.1(13) . . ? C31 C32 H32 116.8(13) . . ? C32 C33 C34 119.4(2) . . ? C32 C33 H33 121.2(11) . . ? C34 C33 H33 119.3(11) . . ? C35 C34 C33 121.2(2) . . ? C35 C34 H34 120.4(12) . . ? C33 C34 H34 118.4(12) . . ? C34 C35 C36 121.5(2) . . ? C34 C35 H35 120.1(11) . . ? C36 C35 H35 118.4(11) . . ? C23 C36 C35 123.12(19) . . ? C23 C36 C31 119.90(19) . . ? C35 C36 C31 116.96(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.274 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.044 #===END data_10 _audit_creation_method SHELXL-97 _database_code_CSD 212729 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H66 N4 Ni O2' _chemical_formula_weight 1053.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8701(8) _cell_length_b 28.890(2) _cell_length_c 18.3122(14) _cell_angle_alpha 90.00 _cell_angle_beta 97.8390(10) _cell_angle_gamma 90.00 _cell_volume 5697.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 93 _cell_measurement_reflns_used 5769 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.39 _exptl_crystal_description 'Thin chunk' _exptl_crystal_colour 'Dark brown' _exptl_crystal_size_max 0.259 _exptl_crystal_size_mid 0.185 _exptl_crystal_size_min 0.148 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 0.390 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 104083 _diffrn_reflns_av_R_equivalents 0.0967 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.58 _reflns_number_total 13770 _reflns_number_gt 8132 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT v 6.2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details w=1/s^2^(Fo^2^) _atom_sites_solution_primary 'Patterson method' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Difference Fourier map' _refine_ls_hydrogen_treatment Unrestrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13770 _refine_ls_number_parameters 901 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0985 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.0818 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.499 _refine_ls_restrained_S_all 2.662 _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 Ni Ni 0.74724(5) 0.825232(17) 0.78152(3) 0.02041(15) Uani 1 1 d . . . O1 O 0.6917(2) 0.88461(8) 0.75968(15) 0.0228(7) Uani 1 1 d . . . O2 O 0.7619(2) 0.76744(8) 0.82352(14) 0.0204(7) Uani 1 1 d . . . N1 N 0.6575(3) 0.79926(11) 0.69525(19) 0.0229(8) Uani 1 1 d . . . N2 N 0.8919(3) 0.84877(10) 0.83905(18) 0.0204(8) Uani 1 1 d . . . C1 C 0.6389(4) 0.90097(14) 0.6967(2) 0.0224(10) Uani 1 1 d . . . C2 C 0.6038(4) 0.94854(14) 0.6908(2) 0.0243(10) Uani 1 1 d . . . C3 C 0.5568(4) 0.96609(17) 0.6227(3) 0.0344(12) Uani 1 1 d . . . C4 C 0.5387(5) 0.93923(18) 0.5590(3) 0.0450(14) Uani 1 1 d . . . C5 C 0.5646(5) 0.89270(17) 0.5655(3) 0.0416(14) Uani 1 1 d . . . C6 C 0.6120(4) 0.87331(14) 0.6333(2) 0.0277(11) Uani 1 1 d . . . C7 C 0.6219(4) 0.82394(16) 0.6371(2) 0.0277(10) Uani 1 1 d . . . C8 C 0.6443(4) 0.74955(13) 0.6831(2) 0.0239(10) Uani 1 1 d . A . C9 C 0.5275(4) 0.72958(15) 0.6819(2) 0.0306(11) Uani 1 1 d . . . C10 C 0.5168(5) 0.68236(16) 0.6662(3) 0.0361(12) Uani 1 1 d . A . C11 C 0.6170(5) 0.65698(16) 0.6513(3) 0.0344(13) Uani 1 1 d . . . C12 C 0.7311(5) 0.67774(16) 0.6529(2) 0.0323(12) Uani 1 1 d . A . C13 C 0.7486(4) 0.72419(14) 0.6697(2) 0.0260(11) Uani 1 1 d . . . C14 C 0.6089(4) 0.97865(14) 0.7572(2) 0.0257(11) Uani 1 1 d . . . C15 C 0.6844(4) 1.01818(14) 0.7653(3) 0.0298(11) Uani 1 1 d . . . C16 C 0.7617(4) 1.03179(16) 0.7118(3) 0.0381(13) Uani 1 1 d . . . C17 C 0.8242(5) 1.07241(18) 0.7173(4) 0.0470(15) Uani 1 1 d . . . C18 C 0.8191(5) 1.1018(2) 0.7783(4) 0.0567(19) Uani 1 1 d . . . C19 C 0.7515(5) 1.09007(18) 0.8317(4) 0.0482(16) Uani 1 1 d . . . C20 C 0.6777(4) 1.04870(15) 0.8266(3) 0.0374(13) Uani 1 1 d . . . C21 C 0.5978(5) 1.03858(17) 0.8768(3) 0.0374(13) Uani 1 1 d . . . C22 C 0.5178(4) 1.00097(15) 0.8678(2) 0.0313(12) Uani 1 1 d . . . C23 C 0.4238(5) 0.99396(19) 0.9138(3) 0.0395(14) Uani 1 1 d . . . C24 C 0.3395(5) 0.95985(19) 0.9009(3) 0.0425(14) Uani 1 1 d . . . C25 C 0.3436(5) 0.92951(18) 0.8406(3) 0.0375(13) Uani 1 1 d . . . C26 C 0.4327(4) 0.93419(15) 0.7961(3) 0.0300(11) Uani 1 1 d . . . C27 C 0.5236(4) 0.97024(14) 0.8072(2) 0.0267(11) Uani 1 1 d . . . C28 C 0.4171(4) 0.75711(18) 0.6942(3) 0.0559(19) Uani 0.693(8) 1 d PD A 1 H28 H 0.4310 0.7852 0.6664 0.084 Uiso 0.693(8) 1 calc PR A 1 C29 C 0.4190(5) 0.7771(2) 0.7702(3) 0.036(2) Uani 0.693(8) 1 d PD A 1 H29A H 0.3374 0.7877 0.7763 0.043 Uiso 0.693(8) 1 calc PR A 1 H29B H 0.4761 0.8026 0.7766 0.043 Uiso 0.693(8) 1 calc PR A 1 H29C H 0.4449 0.7537 0.8064 0.043 Uiso 0.693(8) 1 calc PR A 1 C30 C 0.2959(5) 0.7426(3) 0.6557(4) 0.064(3) Uani 0.693(8) 1 d PD A 1 H30A H 0.2352 0.7660 0.6611 0.077 Uiso 0.693(8) 1 calc PR A 1 H30B H 0.2715 0.7141 0.6764 0.077 Uiso 0.693(8) 1 calc PR A 1 H30C H 0.3018 0.7382 0.6043 0.077 Uiso 0.693(8) 1 calc PR A 1 C28B C 0.4171(4) 0.75711(18) 0.6942(3) 0.0559(19) Uani 0.31 1 d PD A 2 H28B H 0.4519 0.7879 0.7062 0.084 Uiso 0.307(8) 1 calc PR A 2 C29B C 0.3715(13) 0.7424(7) 0.7650(6) 0.068(7) Uiso 0.307(8) 1 d PD A 2 H29D H 0.3002 0.7605 0.7723 0.081 Uiso 0.307(8) 1 calc PR A 2 H29E H 0.4361 0.7472 0.8055 0.081 Uiso 0.307(8) 1 calc PR A 2 H29F H 0.3494 0.7102 0.7620 0.081 Uiso 0.307(8) 1 calc PR A 2 C30B C 0.3205(10) 0.7663(6) 0.6314(5) 0.033(5) Uiso 0.307(8) 1 d PD A 2 H30D H 0.3590 0.7744 0.5890 0.050 Uiso 0.307(8) 1 calc PR A 2 H30E H 0.2689 0.7913 0.6433 0.050 Uiso 0.307(8) 1 calc PR A 2 H30F H 0.2707 0.7390 0.6208 0.050 Uiso 0.307(8) 1 calc PR A 2 C31 C 0.8767(4) 0.74694(15) 0.6693(2) 0.0287(11) Uani 1 1 d D A . C32 C 0.9806(5) 0.71613(19) 0.7045(3) 0.0368(13) Uani 1 1 d D . . C33 C 0.8899(6) 0.7643(2) 0.5950(3) 0.0439(14) Uani 1 1 d D . . C34 C 0.8554(4) 0.74962(13) 0.8668(2) 0.0175(9) Uani 1 1 d . . . C35 C 0.8479(4) 0.70281(13) 0.8922(2) 0.0196(10) Uani 1 1 d . . . C36 C 0.9499(4) 0.68331(14) 0.9338(2) 0.0217(10) Uani 1 1 d . . . C37 C 1.0602(4) 0.70733(15) 0.9527(3) 0.0265(11) Uani 1 1 d . . . C38 C 1.0683(4) 0.75250(15) 0.9319(2) 0.0256(11) Uani 1 1 d . . . C39 C 0.9663(4) 0.77422(13) 0.8896(2) 0.0190(10) Uani 1 1 d . . . C40 C 0.9768(4) 0.82249(14) 0.8739(2) 0.0204(9) Uani 1 1 d . . . C41 C 0.9256(3) 0.89759(13) 0.8371(2) 0.0201(10) Uani 1 1 d . . . C42 C 0.9671(4) 0.91532(14) 0.7740(2) 0.0222(10) Uani 1 1 d . . . C43 C 1.0048(4) 0.96153(15) 0.7765(3) 0.0274(11) Uani 1 1 d . . . C44 C 0.9988(4) 0.98849(16) 0.8380(3) 0.0281(11) Uani 1 1 d . . . C45 C 0.9545(4) 0.97019(14) 0.8987(3) 0.0243(11) Uani 1 1 d . . . C46 C 0.9168(4) 0.92387(13) 0.9002(2) 0.0210(10) Uani 1 1 d . . . C47 C 0.7316(3) 0.67509(14) 0.8736(2) 0.0195(9) Uani 1 1 d . . . C48 C 0.6219(4) 0.68891(13) 0.8996(2) 0.0215(10) Uani 1 1 d . . . C49 C 0.6157(4) 0.72844(14) 0.9457(2) 0.0224(10) Uani 1 1 d . . . C50 C 0.5098(4) 0.73982(16) 0.9730(3) 0.0289(11) Uani 1 1 d . . . C51 C 0.4004(5) 0.71382(17) 0.9542(3) 0.0389(13) Uani 1 1 d . . . C52 C 0.4004(4) 0.67612(18) 0.9109(3) 0.0377(12) Uani 1 1 d . . . C53 C 0.5113(4) 0.66148(14) 0.8828(2) 0.0267(11) Uani 1 1 d . . . C54 C 0.5152(4) 0.62099(15) 0.8428(3) 0.0308(12) Uani 1 1 d . . . C55 C 0.6247(4) 0.60601(14) 0.8189(2) 0.0265(11) Uani 1 1 d . . . C56 C 0.6300(5) 0.56390(15) 0.7793(3) 0.0341(13) Uani 1 1 d . . . C57 C 0.7346(5) 0.54960(16) 0.7551(3) 0.0356(13) Uani 1 1 d . . . C58 C 0.8431(5) 0.57604(16) 0.7691(3) 0.0328(12) Uani 1 1 d . . . C59 C 0.8432(4) 0.61679(15) 0.8065(2) 0.0266(11) Uani 1 1 d . . . C60 C 0.7351(4) 0.63354(13) 0.8341(2) 0.0216(10) Uani 1 1 d . . . C61 C 0.9748(4) 0.88613(15) 0.7062(2) 0.0287(11) Uani 1 1 d . . . C62 C 0.9396(6) 0.9123(2) 0.6340(3) 0.0422(14) Uani 1 1 d . . . C63 C 1.1019(6) 0.8640(2) 0.7083(4) 0.0487(16) Uani 1 1 d . . . C64 C 0.8724(4) 0.90449(15) 0.9687(2) 0.0245(11) Uani 1 1 d . . . C65 C 0.7822(5) 0.93651(17) 1.0001(3) 0.0315(12) Uani 1 1 d . . . C66 C 0.9822(5) 0.89395(19) 1.0282(3) 0.0325(12) Uani 1 1 d . . . C101 C 0.5317(5) 0.8561(2) 0.9464(4) 0.0536(18) Uani 1 1 d . B 3 H10A H 0.594(5) 0.8492(18) 0.995(3) 0.10(2) Uiso 1 1 d . C 3 H10B H 0.534(4) 0.8885(18) 0.933(3) 0.071(18) Uiso 1 1 d . D 3 H10C H 0.545(5) 0.830(2) 0.905(3) 0.10(2) Uiso 1 1 d . E 3 C100 C 0.4044(5) 0.84906(16) 0.9625(3) 0.0461(15) Uani 1 1 d . B 3 N100 N 0.3053(4) 0.84369(14) 0.9742(3) 0.0596(14) Uani 1 1 d . B 3 N200 N 0.7895 1.0019 0.4474 0.112 Uiso 0.24 1 d PD F 4 C200 C 0.8384 1.0296 0.4862 0.169 Uiso 0.24 1 d PD F 4 C201 C 0.9062 1.0615 0.5379 0.131 Uiso 0.24 1 d PD F 4 H20A H 0.9859 1.0486 0.5560 0.158 Uiso 0.24 1 d P F 4 H20B H 0.8603 1.0667 0.5783 0.158 Uiso 0.24 1 d P F 4 H20C H 0.9173 1.0903 0.5135 0.158 Uiso 0.24 1 d P F 4 N300 N 0.8898 1.0441 0.5371 0.116 Uiso 0.76 1 d PD F 5 C300 C 0.8496 1.0130 0.5025 0.102 Uiso 0.76 1 d PD F 5 C301 C 0.8044 0.9740 0.4568 0.083 Uiso 0.76 1 d PD F 5 H30D' H 0.7176 0.9696 0.4593 0.100 Uiso 0.76 1 d P F 5 H30E' H 0.8493 0.9466 0.4741 0.100 Uiso 0.76 1 d P F 5 H30F' H 0.8164 0.9799 0.4066 0.100 Uiso 0.76 1 d P F 5 H3 H 0.535(3) 0.9987(13) 0.619(2) 0.035(13) Uiso 1 1 d . . . H4 H 0.500(4) 0.9511(13) 0.513(2) 0.034(13) Uiso 1 1 d . . . H5 H 0.549(3) 0.8725(13) 0.523(2) 0.031(12) Uiso 1 1 d . . . H7 H 0.593(3) 0.8072(11) 0.591(2) 0.020(11) Uiso 1 1 d . . . H10 H 0.434(4) 0.6677(13) 0.665(2) 0.034(12) Uiso 1 1 d . . . H11 H 0.609(3) 0.6253(13) 0.642(2) 0.032(12) Uiso 1 1 d . . . H12 H 0.798(3) 0.6610(13) 0.642(2) 0.028(12) Uiso 1 1 d . . . H16 H 0.767(3) 1.0130(13) 0.671(2) 0.030(14) Uiso 1 1 d . . . H17 H 0.869(4) 1.0801(13) 0.677(2) 0.030(14) Uiso 1 1 d . . . H18 H 0.862(4) 1.1272(15) 0.780(2) 0.041(15) Uiso 1 1 d . . . H19 H 0.743(4) 1.1084(14) 0.875(2) 0.036(14) Uiso 1 1 d . . . H21 H 0.598(3) 1.0570(13) 0.919(2) 0.029(12) Uiso 1 1 d . . . H23 H 0.427(4) 1.0159(14) 0.955(2) 0.045(14) Uiso 1 1 d . . . H24 H 0.275(4) 0.9543(16) 0.933(3) 0.068(18) Uiso 1 1 d . . . H25 H 0.287(4) 0.9041(14) 0.831(2) 0.044(14) Uiso 1 1 d . . . H26 H 0.435(3) 0.9116(13) 0.754(2) 0.036(13) Uiso 1 1 d . . . H31 H 0.870(3) 0.7723(10) 0.7029(17) 0.002(9) Uiso 1 1 d . . . H32A H 0.972(4) 0.7007(16) 0.756(3) 0.071(17) Uiso 1 1 d . . . H32B H 1.054(4) 0.7320(13) 0.705(2) 0.029(13) Uiso 1 1 d . . . H32C H 0.995(4) 0.6924(13) 0.670(2) 0.033(13) Uiso 1 1 d . . . H33A H 0.827(4) 0.7891(17) 0.568(3) 0.071(17) Uiso 1 1 d . . . H33B H 0.891(3) 0.7375(13) 0.561(2) 0.030(13) Uiso 1 1 d . . . H33C H 0.968(4) 0.7764(13) 0.593(2) 0.026(13) Uiso 1 1 d . . . H36 H 0.943(3) 0.6530(12) 0.9491(19) 0.020(11) Uiso 1 1 d . . . H37 H 1.122(3) 0.6934(11) 0.981(2) 0.019(11) Uiso 1 1 d . . . H38 H 1.143(3) 0.7719(12) 0.9453(19) 0.027(12) Uiso 1 1 d . . . H40 H 1.058(3) 0.8366(11) 0.8952(17) 0.010(9) Uiso 1 1 d . . . H43 H 1.034(3) 0.9758(12) 0.7357(19) 0.017(11) Uiso 1 1 d . . . H44 H 1.024(3) 1.0205(12) 0.8369(18) 0.017(10) Uiso 1 1 d . . . H45 H 0.950(3) 0.9889(11) 0.9389(18) 0.008(10) Uiso 1 1 d . . . H49 H 0.691(3) 0.7471(11) 0.9577(18) 0.016(10) Uiso 1 1 d . . . H50 H 0.512(3) 0.7659(12) 1.006(2) 0.022(11) Uiso 1 1 d . . . H51 H 0.328(4) 0.7220(14) 0.976(2) 0.045(14) Uiso 1 1 d . . . H52 H 0.326(4) 0.6551(13) 0.896(2) 0.038(13) Uiso 1 1 d . . . H54 H 0.434(4) 0.6032(13) 0.829(2) 0.035(12) Uiso 1 1 d . . . H56 H 0.558(3) 0.5466(12) 0.773(2) 0.026(12) Uiso 1 1 d . . . H57 H 0.739(3) 0.5224(12) 0.728(2) 0.023(11) Uiso 1 1 d . . . H58 H 0.920(4) 0.5642(13) 0.754(2) 0.032(12) Uiso 1 1 d . . . H59 H 0.920(3) 0.6353(12) 0.815(2) 0.028(12) Uiso 1 1 d . . . H61 H 0.914(3) 0.8609(12) 0.706(2) 0.027(12) Uiso 1 1 d . . . H62A H 0.857(4) 0.9292(15) 0.630(2) 0.058(16) Uiso 1 1 d . . . H62B H 0.937(4) 0.8914(14) 0.592(2) 0.044(14) Uiso 1 1 d . . . H62C H 1.004(4) 0.9370(14) 0.621(2) 0.039(13) Uiso 1 1 d . . . H63A H 1.126(4) 0.8440(15) 0.752(3) 0.056(17) Uiso 1 1 d . . . H63B H 1.165(4) 0.8887(16) 0.707(2) 0.057(17) Uiso 1 1 d . . . H63C H 1.102(4) 0.8457(14) 0.664(2) 0.044(15) Uiso 1 1 d . . . H64 H 0.834(3) 0.8781(13) 0.958(2) 0.029(12) Uiso 1 1 d . . . H65A H 0.718(3) 0.9444(12) 0.962(2) 0.018(11) Uiso 1 1 d . . . H65B H 0.827(3) 0.9669(13) 1.023(2) 0.031(12) Uiso 1 1 d . . . H65C H 0.748(4) 0.9217(13) 1.043(2) 0.040(14) Uiso 1 1 d . . . H66A H 1.037(4) 0.8684(14) 1.011(2) 0.046(14) Uiso 1 1 d . . . H66B H 0.952(4) 0.8810(13) 1.073(2) 0.036(13) Uiso 1 1 d . . . H66C H 1.034(4) 0.9199(14) 1.042(2) 0.043(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0209(3) 0.0162(3) 0.0233(3) -0.0026(3) 0.0003(2) 0.0013(3) O1 0.0242(17) 0.0188(16) 0.0243(17) -0.0008(13) -0.0006(14) 0.0036(13) O2 0.0187(16) 0.0185(15) 0.0228(17) -0.0003(13) -0.0020(13) -0.0003(12) N1 0.020(2) 0.021(2) 0.026(2) -0.0034(17) -0.0001(17) 0.0030(16) N2 0.021(2) 0.0157(18) 0.024(2) 0.0001(16) 0.0034(16) 0.0016(15) C1 0.019(2) 0.022(2) 0.026(3) 0.000(2) 0.003(2) 0.0021(19) C2 0.025(3) 0.020(2) 0.027(3) 0.000(2) 0.001(2) 0.0046(19) C3 0.044(3) 0.024(3) 0.034(3) 0.003(2) 0.002(3) 0.006(2) C4 0.067(4) 0.036(3) 0.030(3) 0.006(3) -0.003(3) 0.012(3) C5 0.065(4) 0.034(3) 0.024(3) -0.004(3) -0.001(3) 0.009(3) C6 0.037(3) 0.021(2) 0.024(3) 0.001(2) 0.002(2) 0.008(2) C7 0.031(3) 0.029(3) 0.022(3) -0.005(2) -0.002(2) 0.004(2) C8 0.028(3) 0.019(2) 0.023(3) -0.0070(19) -0.005(2) 0.002(2) C9 0.023(3) 0.029(3) 0.037(3) -0.010(2) -0.007(2) 0.006(2) C10 0.033(3) 0.032(3) 0.041(3) -0.007(2) -0.004(2) -0.006(2) C11 0.046(3) 0.020(3) 0.035(3) -0.009(2) -0.003(3) 0.001(2) C12 0.038(3) 0.027(3) 0.031(3) -0.009(2) 0.003(2) 0.011(3) C13 0.032(3) 0.024(3) 0.022(3) -0.004(2) 0.002(2) 0.005(2) C14 0.025(3) 0.019(2) 0.031(3) 0.000(2) -0.005(2) 0.008(2) C15 0.022(3) 0.023(3) 0.042(3) 0.001(2) -0.007(2) 0.006(2) C16 0.026(3) 0.024(3) 0.061(4) 0.003(3) -0.006(3) 0.007(2) C17 0.026(3) 0.034(3) 0.078(5) 0.013(3) -0.006(3) 0.002(3) C18 0.031(4) 0.026(3) 0.103(6) 0.003(4) -0.027(4) -0.003(3) C19 0.030(3) 0.031(3) 0.076(5) -0.014(3) -0.019(3) 0.007(3) C20 0.027(3) 0.021(3) 0.058(4) -0.007(3) -0.017(3) 0.007(2) C21 0.039(3) 0.031(3) 0.037(3) -0.013(3) -0.012(3) 0.016(2) C22 0.033(3) 0.029(3) 0.029(3) -0.003(2) -0.008(2) 0.015(2) C23 0.045(4) 0.040(3) 0.032(3) -0.002(3) -0.001(3) 0.023(3) C24 0.043(4) 0.047(4) 0.038(4) 0.009(3) 0.009(3) 0.019(3) C25 0.037(3) 0.034(3) 0.042(3) 0.010(3) 0.005(3) 0.008(3) C26 0.035(3) 0.023(3) 0.032(3) 0.002(2) 0.003(2) 0.007(2) C27 0.028(3) 0.022(2) 0.029(3) 0.000(2) -0.004(2) 0.010(2) C28 0.031(3) 0.055(4) 0.080(5) -0.026(3) 0.001(3) -0.003(3) C29 0.029(4) 0.038(5) 0.045(5) 0.015(4) 0.017(3) 0.011(3) C30 0.035(5) 0.090(8) 0.069(7) 0.007(6) 0.011(5) 0.012(5) C28B 0.031(3) 0.055(4) 0.080(5) -0.026(3) 0.001(3) -0.003(3) C31 0.033(3) 0.027(3) 0.027(3) -0.003(2) 0.007(2) 0.006(2) C32 0.031(3) 0.037(3) 0.043(4) -0.001(3) 0.006(3) 0.009(3) C33 0.047(4) 0.055(4) 0.031(3) 0.005(3) 0.011(3) -0.003(3) C34 0.016(2) 0.018(2) 0.019(2) -0.0052(18) 0.0053(19) 0.0013(18) C35 0.018(2) 0.020(2) 0.021(2) -0.0047(19) 0.0043(19) -0.0015(19) C36 0.020(2) 0.016(3) 0.030(3) -0.001(2) 0.004(2) 0.0008(19) C37 0.017(3) 0.023(3) 0.038(3) 0.002(2) -0.003(2) 0.004(2) C38 0.017(2) 0.021(3) 0.038(3) -0.003(2) 0.003(2) -0.001(2) C39 0.015(2) 0.016(2) 0.027(3) -0.0022(19) 0.0044(19) 0.0024(18) C40 0.017(2) 0.019(2) 0.025(2) -0.004(2) 0.0019(19) -0.003(2) C41 0.015(2) 0.015(2) 0.029(3) 0.000(2) 0.000(2) -0.0016(18) C42 0.020(2) 0.020(2) 0.027(3) 0.001(2) 0.003(2) 0.0014(19) C43 0.030(3) 0.025(3) 0.028(3) 0.008(2) 0.007(2) -0.005(2) C44 0.031(3) 0.019(3) 0.034(3) 0.001(2) 0.002(2) -0.006(2) C45 0.029(3) 0.016(2) 0.027(3) -0.004(2) 0.003(2) -0.001(2) C46 0.016(2) 0.020(2) 0.027(3) 0.001(2) 0.0022(19) 0.0002(18) C47 0.017(2) 0.018(2) 0.023(2) 0.002(2) 0.0009(18) -0.0002(19) C48 0.018(2) 0.018(2) 0.028(3) 0.0062(19) 0.002(2) 0.0005(18) C49 0.021(3) 0.020(2) 0.026(3) 0.007(2) 0.005(2) 0.004(2) C50 0.029(3) 0.024(3) 0.036(3) 0.007(2) 0.009(2) 0.008(2) C51 0.024(3) 0.034(3) 0.061(4) 0.007(3) 0.017(3) 0.011(2) C52 0.018(3) 0.035(3) 0.060(4) 0.008(3) 0.004(2) 0.000(2) C53 0.018(2) 0.022(3) 0.039(3) 0.007(2) 0.002(2) 0.0019(19) C54 0.017(3) 0.027(3) 0.046(3) 0.003(2) -0.004(2) -0.005(2) C55 0.025(3) 0.018(2) 0.034(3) -0.001(2) -0.002(2) -0.003(2) C56 0.028(3) 0.022(3) 0.050(3) -0.004(2) -0.005(3) -0.007(2) C57 0.040(3) 0.020(3) 0.044(3) -0.013(2) -0.007(3) 0.001(2) C58 0.029(3) 0.028(3) 0.041(3) -0.011(2) 0.004(2) 0.003(2) C59 0.023(3) 0.024(3) 0.033(3) -0.004(2) 0.003(2) -0.002(2) C60 0.020(2) 0.019(2) 0.025(3) 0.0001(19) 0.000(2) -0.0001(19) C61 0.034(3) 0.025(3) 0.028(3) -0.002(2) 0.009(2) -0.001(2) C62 0.054(4) 0.044(4) 0.031(3) -0.001(3) 0.014(3) -0.003(3) C63 0.048(4) 0.051(4) 0.049(4) -0.014(4) 0.013(3) 0.008(3) C64 0.029(3) 0.015(2) 0.030(3) -0.003(2) 0.004(2) -0.003(2) C65 0.031(3) 0.030(3) 0.035(3) -0.003(3) 0.009(3) -0.002(2) C66 0.036(3) 0.029(3) 0.033(3) 0.002(3) 0.007(3) 0.002(3) C101 0.033(4) 0.040(4) 0.084(5) 0.022(4) -0.005(3) -0.007(3) C100 0.041(4) 0.029(3) 0.064(4) 0.012(3) -0.010(3) 0.001(3) N100 0.044(3) 0.043(3) 0.090(4) 0.015(3) 0.001(3) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O2 1.836(3) . yes Ni O1 1.844(2) . yes Ni N1 1.895(3) . yes Ni N2 1.896(3) . yes O1 C1 1.305(4) . ? O2 C34 1.306(4) . ? N1 C7 1.295(5) . ? N1 C8 1.457(5) . ? N2 C40 1.294(5) . ? N2 C41 1.459(4) . ? C1 C6 1.407(5) . ? C1 C2 1.427(5) . ? C2 C3 1.379(6) . ? C2 C14 1.490(5) . ? C3 C4 1.392(6) . ? C3 H3 0.97(4) . ? C4 C5 1.375(6) . ? C4 H4 0.95(4) . ? C5 C6 1.394(6) . ? C5 H5 0.97(4) . ? C6 C7 1.431(6) . ? C7 H7 0.99(3) . ? C8 C9 1.392(5) . ? C8 C13 1.399(5) . ? C9 C10 1.396(6) . ? C9 C28 1.483(6) . ? C10 C11 1.371(6) . ? C10 H10 0.99(4) . ? C11 C12 1.374(6) . ? C11 H11 0.93(4) . ? C12 C13 1.384(6) . ? C12 H12 0.92(4) . ? C13 C31 1.541(6) . ? C14 C15 1.403(5) . ? C14 C27 1.410(6) . ? C15 C16 1.430(7) . ? C15 C20 1.436(6) . ? C16 C17 1.353(6) . ? C16 H16 0.93(4) . ? C17 C18 1.411(8) . ? C17 H17 0.96(4) . ? C18 C19 1.344(8) . ? C18 H18 0.87(4) . ? C19 C20 1.436(7) . ? C19 H19 0.97(4) . ? C20 C21 1.380(7) . ? C21 C22 1.387(6) . ? C21 H21 0.94(4) . ? C22 C23 1.424(6) . ? C22 C27 1.430(6) . ? C23 C24 1.344(7) . ? C23 H23 0.98(4) . ? C24 C25 1.415(7) . ? C24 H24 0.98(5) . ? C25 C26 1.354(6) . ? C25 H25 0.96(4) . ? C26 C27 1.430(6) . ? C26 H26 1.02(4) . ? C28 C30 1.468(5) . ? C28 C29 1.505(5) . ? C28 H28 0.9800 . ? C28B C30B 1.4719(47) . ? C28B C29B 1.5095(47) . ? C28B H28B 0.9800 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C29B H29D 0.9600 . ? C29B H29E 0.9600 . ? C29B H29F 0.9600 . ? C30B H30D 0.9600 . ? C30B H30E 0.9600 . ? C30B H30F 0.9600 . ? C31 C33 1.476(5) . ? C31 C32 1.511(5) . ? C31 H31 0.97(3) . ? C32 H32A 1.06(5) . ? C32 H32B 0.92(4) . ? C32 H32C 0.95(4) . ? C33 H33A 1.06(5) . ? C33 H33B 1.00(4) . ? C33 H33C 0.92(4) . ? C34 C39 1.413(5) . ? C34 C35 1.436(5) . ? C35 C36 1.377(5) . ? C35 C47 1.496(5) . ? C36 C37 1.388(5) . ? C36 H36 0.93(3) . ? C37 C38 1.366(5) . ? C37 H37 0.89(3) . ? C38 C39 1.410(5) . ? C38 H38 0.99(3) . ? C39 C40 1.431(5) . ? C40 H40 1.00(3) . ? C41 C42 1.394(5) . ? C41 C46 1.396(5) . ? C42 C43 1.396(5) . ? C42 C61 1.513(6) . ? C43 C44 1.377(6) . ? C43 H43 0.95(3) . ? C44 C45 1.376(6) . ? C44 H44 0.97(3) . ? C45 C46 1.401(5) . ? C45 H45 0.92(3) . ? C46 C64 1.512(6) . ? C47 C48 1.401(5) . ? C47 C60 1.405(5) . ? C48 C49 1.427(5) . ? C48 C53 1.438(5) . ? C49 C50 1.356(5) . ? C49 H49 0.98(3) . ? C50 C51 1.409(6) . ? C50 H50 0.96(3) . ? C51 C52 1.347(6) . ? C51 H51 0.96(4) . ? C52 C53 1.438(6) . ? C52 H52 1.02(4) . ? C53 C54 1.384(6) . ? C54 C55 1.392(6) . ? C54 H54 1.02(4) . ? C55 C56 1.422(6) . ? C55 C60 1.435(5) . ? C56 C57 1.341(6) . ? C56 H56 0.92(4) . ? C57 C58 1.399(6) . ? C57 H57 0.94(3) . ? C58 C59 1.362(6) . ? C58 H58 0.98(4) . ? C59 C60 1.426(5) . ? C59 H59 0.98(4) . ? C61 C63 1.519(7) . ? C61 C62 1.526(6) . ? C61 H61 0.98(4) . ? C62 H62A 1.01(5) . ? C62 H62B 0.98(4) . ? C62 H62C 1.05(4) . ? C63 H63A 1.00(5) . ? C63 H63B 0.99(5) . ? C63 H63C 0.97(4) . ? C64 C65 1.517(6) . ? C64 C66 1.532(6) . ? C64 H64 0.88(4) . ? C65 H65A 0.95(3) . ? C65 H65B 1.06(4) . ? C65 H65C 1.01(4) . ? C66 H66A 1.02(4) . ? C66 H66B 1.00(4) . ? C66 H66C 0.95(4) . ? C101 C100 1.467(7) . ? C101 H10A 1.05(6) . ? C101 H10B 0.97(5) . ? C101 H10C 1.09(6) . ? C100 N100 1.136(6) . ? N200 C200 1.1514 . ? N200 H30D 1.2557 . ? N200 H30F 1.0507 . ? C200 C201 1.4491 . ? C201 H20A 0.9600 . ? C201 H20B 0.9600 . ? C201 H20C 0.9600 . ? N300 C300 1.1500 . ? N300 H20A 1.0623 . ? N300 H20B 1.0809 . ? N300 H20C 1.4475 . ? C300 C301 1.4500 . ? C301 H30D 0.9600 . ? C301 H30E 0.9600 . ? C301 H30F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ni O1 160.71(12) . . yes O2 Ni N1 89.69(13) . . yes O1 Ni N1 94.10(13) . . yes O2 Ni N2 94.32(12) . . yes O1 Ni N2 90.52(12) . . yes N1 Ni N2 154.05(14) . . yes C1 O1 Ni 128.3(3) . . ? C34 O2 Ni 128.9(2) . . ? C7 N1 C8 113.9(4) . . ? C7 N1 Ni 121.9(3) . . ? C8 N1 Ni 123.1(3) . . ? C40 N2 C41 114.5(3) . . ? C40 N2 Ni 123.0(3) . . ? C41 N2 Ni 121.7(2) . . ? O1 C1 C6 122.7(4) . . ? O1 C1 C2 119.8(4) . . ? C6 C1 C2 117.5(4) . . ? C3 C2 C1 119.0(4) . . ? C3 C2 C14 119.4(4) . . ? C1 C2 C14 121.4(4) . . ? C2 C3 C4 123.1(5) . . ? C2 C3 H3 118(2) . . ? C4 C3 H3 119(2) . . ? C5 C4 C3 117.9(5) . . ? C5 C4 H4 119(2) . . ? C3 C4 H4 122(2) . . ? C4 C5 C6 121.1(5) . . ? C4 C5 H5 121(2) . . ? C6 C5 H5 118(2) . . ? C5 C6 C1 121.1(4) . . ? C5 C6 C7 117.4(4) . . ? C1 C6 C7 121.3(4) . . ? N1 C7 C6 127.0(4) . . ? N1 C7 H7 117(2) . . ? C6 C7 H7 116(2) . . ? C9 C8 C13 122.6(4) . . ? C9 C8 N1 118.8(4) . . ? C13 C8 N1 118.5(4) . . ? C8 C9 C10 117.3(4) . . ? C8 C9 C28 122.1(4) . . ? C10 C9 C28 120.6(4) . . ? C11 C10 C9 121.2(5) . . ? C11 C10 H10 121(2) . . ? C9 C10 H10 118(2) . . ? C10 C11 C12 120.1(5) . . ? C10 C11 H11 120(2) . . ? C12 C11 H11 120(2) . . ? C11 C12 C13 121.6(5) . . ? C11 C12 H12 120(2) . . ? C13 C12 H12 118(2) . . ? C12 C13 C8 117.1(4) . . ? C12 C13 C31 120.6(4) . . ? C8 C13 C31 122.1(4) . . ? C15 C14 C27 119.9(4) . . ? C15 C14 C2 121.2(4) . . ? C27 C14 C2 118.4(4) . . ? C14 C15 C16 122.8(4) . . ? C14 C15 C20 119.4(5) . . ? C16 C15 C20 117.6(4) . . ? C17 C16 C15 121.6(6) . . ? C17 C16 H16 119(3) . . ? C15 C16 H16 120(3) . . ? C16 C17 C18 120.4(6) . . ? C16 C17 H17 116(3) . . ? C18 C17 H17 123(3) . . ? C19 C18 C17 120.6(6) . . ? C19 C18 H18 122(3) . . ? C17 C18 H18 118(3) . . ? C18 C19 C20 121.2(6) . . ? C18 C19 H19 126(3) . . ? C20 C19 H19 113(3) . . ? C21 C20 C19 122.0(5) . . ? C21 C20 C15 119.6(4) . . ? C19 C20 C15 118.3(5) . . ? C20 C21 C22 121.9(5) . . ? C20 C21 H21 120(2) . . ? C22 C21 H21 118(2) . . ? C21 C22 C23 122.0(5) . . ? C21 C22 C27 119.0(5) . . ? C23 C22 C27 118.8(5) . . ? C24 C23 C22 121.8(5) . . ? C24 C23 H23 124(3) . . ? C22 C23 H23 114(3) . . ? C23 C24 C25 119.9(6) . . ? C23 C24 H24 123(3) . . ? C25 C24 H24 118(3) . . ? C26 C25 C24 120.5(5) . . ? C26 C25 H25 117(3) . . ? C24 C25 H25 122(3) . . ? C25 C26 C27 121.6(5) . . ? C25 C26 H26 119(2) . . ? C27 C26 H26 119(2) . . ? C14 C27 C22 120.0(4) . . ? C14 C27 C26 122.4(4) . . ? C22 C27 C26 117.4(4) . . ? C30 C28 C9 117.7(4) . . ? C30 C28 C29 117.0(4) . . ? C9 C28 C29 115.9(4) . . ? C30 C28 H28 100.3 . . ? C9 C28 H28 100.3 . . ? C29 C28 H28 100.3 . . ? C30B C28B C9 118.87(69) . . ? C30B C28B C29B 116.07(39) . . ? C9 C28B C29B 110.29(74) . . ? C30B C28B H28B 103.00 . . ? C9 C28B H28B 103.00 . . ? C29B C28B H28B 103.00 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? H29D C29B H29E 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? H30D C30B H30E 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C33 C31 C32 115.6(4) . . ? C33 C31 C13 110.5(4) . . ? C32 C31 C13 111.7(4) . . ? C33 C31 H31 110.8(18) . . ? C32 C31 H31 107.0(18) . . ? C13 C31 H31 100.1(18) . . ? C31 C32 H32A 118(3) . . ? C31 C32 H32B 108(2) . . ? H32A C32 H32B 112(4) . . ? C31 C32 H32C 109(2) . . ? H32A C32 H32C 109(3) . . ? H32B C32 H32C 99(3) . . ? C31 C33 H33A 122(3) . . ? C31 C33 H33B 109(2) . . ? H33A C33 H33B 107(3) . . ? C31 C33 H33C 112(2) . . ? H33A C33 H33C 105(4) . . ? H33B C33 H33C 100(3) . . ? O2 C34 C39 122.9(3) . . ? O2 C34 C35 119.6(3) . . ? C39 C34 C35 117.5(3) . . ? C36 C35 C34 119.1(4) . . ? C36 C35 C47 119.9(4) . . ? C34 C35 C47 120.9(3) . . ? C35 C36 C37 122.5(4) . . ? C35 C36 H36 117(2) . . ? C37 C36 H36 120(2) . . ? C38 C37 C36 119.6(4) . . ? C38 C37 H37 122(2) . . ? C36 C37 H37 119(2) . . ? C37 C38 C39 120.2(4) . . ? C37 C38 H38 123(2) . . ? C39 C38 H38 116(2) . . ? C38 C39 C34 120.9(4) . . ? C38 C39 C40 117.8(4) . . ? C34 C39 C40 121.2(4) . . ? N2 C40 C39 126.9(4) . . ? N2 C40 H40 119.0(18) . . ? C39 C40 H40 114.0(18) . . ? C42 C41 C46 123.5(4) . . ? C42 C41 N2 119.1(4) . . ? C46 C41 N2 117.4(4) . . ? C41 C42 C43 116.8(4) . . ? C41 C42 C61 122.4(4) . . ? C43 C42 C61 120.7(4) . . ? C44 C43 C42 121.4(4) . . ? C44 C43 H43 117(2) . . ? C42 C43 H43 121(2) . . ? C45 C44 C43 120.2(4) . . ? C45 C44 H44 121(2) . . ? C43 C44 H44 119(2) . . ? C44 C45 C46 121.3(4) . . ? C44 C45 H45 119(2) . . ? C46 C45 H45 120(2) . . ? C41 C46 C45 116.7(4) . . ? C41 C46 C64 123.4(4) . . ? C45 C46 C64 119.9(4) . . ? C48 C47 C60 120.2(4) . . ? C48 C47 C35 120.1(4) . . ? C60 C47 C35 119.5(3) . . ? C47 C48 C49 122.7(4) . . ? C47 C48 C53 119.7(4) . . ? C49 C48 C53 117.5(4) . . ? C50 C49 C48 121.5(4) . . ? C50 C49 H49 121(2) . . ? C48 C49 H49 118(2) . . ? C49 C50 C51 120.8(5) . . ? C49 C50 H50 118(2) . . ? C51 C50 H50 121(2) . . ? C52 C51 C50 120.4(5) . . ? C52 C51 H51 120(3) . . ? C50 C51 H51 119(3) . . ? C51 C52 C53 121.1(5) . . ? C51 C52 H52 125(2) . . ? C53 C52 H52 113(2) . . ? C54 C53 C52 121.7(4) . . ? C54 C53 C48 119.6(4) . . ? C52 C53 C48 118.6(4) . . ? C53 C54 C55 121.2(4) . . ? C53 C54 H54 118(2) . . ? C55 C54 H54 121(2) . . ? C54 C55 C56 121.5(4) . . ? C54 C55 C60 119.7(4) . . ? C56 C55 C60 118.8(4) . . ? C57 C56 C55 121.8(4) . . ? C57 C56 H56 123(2) . . ? C55 C56 H56 116(2) . . ? C56 C57 C58 120.3(5) . . ? C56 C57 H57 123(2) . . ? C58 C57 H57 117(2) . . ? C59 C58 C57 120.4(5) . . ? C59 C58 H58 120(2) . . ? C57 C58 H58 119(2) . . ? C58 C59 C60 121.9(4) . . ? C58 C59 H59 120(2) . . ? C60 C59 H59 118(2) . . ? C47 C60 C59 123.7(4) . . ? C47 C60 C55 119.5(4) . . ? C59 C60 C55 116.8(4) . . ? C42 C61 C63 111.5(4) . . ? C42 C61 C62 113.6(4) . . ? C63 C61 C62 110.5(5) . . ? C42 C61 H61 107(2) . . ? C63 C61 H61 107(2) . . ? C62 C61 H61 106(2) . . ? C61 C62 H62A 114(3) . . ? C61 C62 H62B 111(3) . . ? H62A C62 H62B 108(4) . . ? C61 C62 H62C 116(2) . . ? H62A C62 H62C 106(3) . . ? H62B C62 H62C 101(3) . . ? C61 C63 H63A 114(3) . . ? C61 C63 H63B 109(3) . . ? H63A C63 H63B 109(4) . . ? C61 C63 H63C 108(3) . . ? H63A C63 H63C 109(4) . . ? H63B C63 H63C 107(4) . . ? C46 C64 C65 112.6(4) . . ? C46 C64 C66 111.0(4) . . ? C65 C64 C66 109.5(4) . . ? C46 C64 H64 110(3) . . ? C65 C64 H64 107(3) . . ? C66 C64 H64 107(3) . . ? C64 C65 H65A 108(2) . . ? C64 C65 H65B 112(2) . . ? H65A C65 H65B 110(3) . . ? C64 C65 H65C 111(2) . . ? H65A C65 H65C 112(3) . . ? H65B C65 H65C 104(3) . . ? C64 C66 H66A 111(2) . . ? C64 C66 H66B 110(2) . . ? H66A C66 H66B 104(3) . . ? C64 C66 H66C 114(3) . . ? H66A C66 H66C 107(3) . . ? H66B C66 H66C 109(3) . . ? C100 C101 H10A 109(3) . . ? C100 C101 H10B 104(3) . . ? H10A C101 H10B 111(4) . . ? C100 C101 H10C 106(3) . . ? H10A C101 H10C 109(4) . . ? H10B C101 H10C 117(4) . . ? N100 C100 C101 179.2(7) . . ? C200 N200 H30D 131.0 . . ? C200 N200 H30F 135.0 . . ? H30D N200 H30F 85.2 . . ? N200 C200 C201 175.4 . . ? C200 C201 H20A 109.5 . . ? C200 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C200 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C300 N300 H20A 124.0 . . ? C300 N300 H20B 137.0 . . ? H20A N300 H20B 94.0 . . ? C300 N300 H20C 129.4 . . ? H20A N300 H20C 75.6 . . ? H20B N300 H20C 75.1 . . ? N300 C300 C301 177.0 . . ? C300 C301 H30D 109.5 . . ? C300 C301 H30E 109.5 . . ? H30D C301 H30E 109.5 . . ? C300 C301 H30F 109.5 . . ? H30D C301 H30F 109.5 . . ? H30E C301 H30F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 28.58 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.689 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.064 #===END