# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address P.J.Chmielewski ;Department of Chemistry University of Wroclaw 14 F. Joliot-Curie Wroclaw 50-383 ; J.Maciolek ;Department of Chemistry University of Wroclaw 14 F. Joliot-Curie Wroclaw 50-383 ; _publ_contact_author_address ;Department of Chemistry University of Wroclaw 14 F. Joliot-Curie Wroclaw 50-383 ; _publ_contact_author_email pjc@wchuwr.pl _publ_contact_author_name 'Piotr J. Chmielewski' data_chni3 _database_code_depnum_ccdc_archive 'CCDC 825666' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C200 H156 Cl8 N16 Ni4' _chemical_formula_weight 3301.85 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 13.3922(3) _cell_length_b 15.4736(3) _cell_length_c 23.0929(4) _cell_angle_alpha 100.664(2) _cell_angle_beta 102.767(2) _cell_angle_gamma 111.139(2) _cell_volume 4164.62(18) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24989 _cell_measurement_theta_min 4.7138 _cell_measurement_theta_max 38.5154 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 0.634 _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 100(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 'Xcalibur with Onyx CCD' _diffrn_measurement_method '\w and \p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94045 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.1401 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 4.73 _diffrn_reflns_theta_max 38.59 _reflns_number_total 45163 _reflns_number_gt 21181 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 45163 _refine_ls_number_parameters 1035 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 0.834 _refine_ls_restrained_S_all 0.834 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.000 341 44 ' ' 2 0.448 0.958 0.959 9 1 ' ' 3 0.557 0.045 0.045 9 1 ' ' _platon_squeeze_details ; ; 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 1.091986(17) 1.019829(14) 0.418666(9) 0.01263(4) Uani 1 1 d . . . C21 C 1.01246(13) 1.09382(11) 0.37872(7) 0.0130(3) Uani 1 1 d . . . N22 N 0.97211(11) 0.90045(10) 0.36080(6) 0.0141(2) Uani 1 1 d . . . N23 N 1.16205(11) 0.94695(9) 0.46008(6) 0.0134(2) Uani 1 1 d . . . N24 N 1.20098(11) 1.14070(9) 0.47986(6) 0.0139(2) Uani 1 1 d . . . C1 C 1.07968(13) 1.19503(11) 0.38275(7) 0.0137(3) Uani 1 1 d . . . N2 N 1.05567(11) 1.21630(10) 0.32795(6) 0.0144(2) Uani 1 1 d . . . C3 C 0.98209(13) 1.13277(11) 0.28549(7) 0.0129(3) Uani 1 1 d . . . C4 C 0.94970(13) 1.05439(11) 0.31167(7) 0.0134(3) Uani 1 1 d . . . C5 C 0.87469(13) 0.95816(11) 0.28260(7) 0.0143(3) Uani 1 1 d . . . C6 C 0.87994(13) 0.88801(11) 0.31292(7) 0.0147(3) Uani 1 1 d . . . C7 C 0.79605(14) 0.78953(12) 0.29296(8) 0.0172(3) Uani 1 1 d . . . H7A H 0.7260 0.7644 0.2627 0.021 Uiso 1 1 calc R . . C8 C 0.83830(14) 0.74072(12) 0.32644(8) 0.0177(3) Uani 1 1 d . . . H8A H 0.8027 0.6756 0.3239 0.021 Uiso 1 1 calc R . . C9 C 0.94849(13) 0.80822(11) 0.36671(7) 0.0148(3) Uani 1 1 d . . . C10 C 1.02509(14) 0.78159(11) 0.40211(7) 0.0157(3) Uani 1 1 d . . . C11 C 1.12946(14) 0.84836(12) 0.44292(7) 0.0152(3) Uani 1 1 d . . . C12 C 1.21352(14) 0.82443(12) 0.47761(8) 0.0179(3) Uani 1 1 d . . . H12A H 1.2115 0.7628 0.4735 0.022 Uiso 1 1 calc R . . C13 C 1.29628(14) 0.90839(12) 0.51745(8) 0.0178(3) Uani 1 1 d . . . H13A H 1.3623 0.9158 0.5458 0.021 Uiso 1 1 calc R . . C14 C 1.26205(13) 0.98380(12) 0.50737(7) 0.0145(3) Uani 1 1 d . . . C15 C 1.31455(13) 1.07908(12) 0.54568(7) 0.0152(3) Uani 1 1 d . . . C16 C 1.27911(13) 1.15015(11) 0.53396(7) 0.0143(3) Uani 1 1 d . . . C17 C 1.33182(14) 1.24865(12) 0.57349(7) 0.0171(3) Uani 1 1 d . . . H17A H 1.3846 1.2721 0.6128 0.021 Uiso 1 1 calc R . . C18 C 1.28995(14) 1.30027(12) 0.54251(7) 0.0169(3) Uani 1 1 d . . . H18A H 1.3082 1.3661 0.5565 0.020 Uiso 1 1 calc R . . C19 C 1.21171(13) 1.23411(11) 0.48374(7) 0.0143(3) Uani 1 1 d . . . C20 C 1.16436(13) 1.26392(11) 0.43505(7) 0.0135(3) Uani 1 1 d . . . C61 C 0.93596(14) 1.08562(13) 0.42067(8) 0.0179(3) Uani 1 1 d . . . H61A H 0.8877 1.1173 0.4098 0.027 Uiso 1 1 calc R . . H61B H 0.9819 1.1160 0.4633 0.027 Uiso 1 1 calc R . . H61C H 0.8907 1.0186 0.4149 0.027 Uiso 1 1 calc R . . Ni2 Ni 0.836335(18) 0.965084(15) 0.041973(9) 0.01423(5) Uani 1 1 d . . . C45 C 0.93421(13) 1.08456(12) 0.11426(7) 0.0148(3) Uani 1 1 d . . . N46 N 0.92183(12) 0.89934(10) 0.07881(6) 0.0149(3) Uani 1 1 d . . . N47 N 0.75022(12) 0.85284(10) -0.03123(6) 0.0167(3) Uani 1 1 d . . . N48 N 0.76566(12) 1.04045(10) 0.00528(6) 0.0160(3) Uani 1 1 d . . . C25 C 0.88676(13) 1.15313(11) 0.13326(7) 0.0142(3) Uani 1 1 d . . . N26 N 0.90343(11) 1.17956(10) 0.19575(6) 0.0149(3) Uani 1 1 d . . . C27 C 0.95679(13) 1.12881(11) 0.21944(7) 0.0131(3) Uani 1 1 d . . . C28 C 0.97946(13) 1.07091(11) 0.17383(7) 0.0139(3) Uani 1 1 d . . . C29 C 1.04006(13) 1.01477(11) 0.18159(7) 0.0139(3) Uani 1 1 d . . . C30 C 1.01574(13) 0.93658(12) 0.13139(7) 0.0156(3) Uani 1 1 d . . . C31 C 1.07331(15) 0.87395(13) 0.13091(8) 0.0204(3) Uani 1 1 d . . . H31A H 1.1411 0.8855 0.1594 0.024 Uiso 1 1 calc R . . C32 C 1.01048(15) 0.79574(13) 0.08157(8) 0.0215(3) Uani 1 1 d . . . H32A H 1.0257 0.7421 0.0700 0.026 Uiso 1 1 calc R . . C33 C 0.91525(15) 0.81033(12) 0.04990(7) 0.0175(3) Uani 1 1 d . . . C34 C 0.82939(15) 0.74130(12) -0.00190(7) 0.0170(3) Uani 1 1 d . . . C35 C 0.74804(15) 0.76157(12) -0.03896(7) 0.0179(3) Uani 1 1 d . . . C36 C 0.65960(16) 0.69424(13) -0.09415(8) 0.0224(4) Uani 1 1 d . . . H36A H 0.6394 0.6281 -0.1083 0.027 Uiso 1 1 calc R . . C37 C 0.61145(16) 0.74563(13) -0.12149(8) 0.0222(4) Uani 1 1 d . . . H37A H 0.5522 0.7216 -0.1584 0.027 Uiso 1 1 calc R . . C38 C 0.66846(14) 0.84393(12) -0.08315(7) 0.0180(3) Uani 1 1 d . . . C39 C 0.64933(14) 0.92137(12) -0.09729(7) 0.0173(3) Uani 1 1 d . . . C40 C 0.70022(14) 1.01411(12) -0.05600(7) 0.0170(3) Uani 1 1 d . . . C41 C 0.68278(14) 1.09522(12) -0.07057(8) 0.0187(3) Uani 1 1 d . . . H41A H 0.6428 1.0957 -0.1088 0.022 Uiso 1 1 calc R . . C42 C 0.73524(14) 1.17001(12) -0.01839(7) 0.0179(3) Uani 1 1 d . . . H42A H 0.7393 1.2322 -0.0141 0.022 Uiso 1 1 calc R . . C43 C 0.78399(14) 1.13623(11) 0.02957(7) 0.0155(3) Uani 1 1 d . . . C44 C 0.83163(13) 1.18960(11) 0.09228(7) 0.0151(3) Uani 1 1 d . . . C62 C 1.02550(14) 1.12425(12) 0.08285(8) 0.0187(3) Uani 1 1 d . . . H62A H 1.0843 1.1845 0.1103 0.028 Uiso 1 1 calc R . . H62B H 0.9919 1.1345 0.0450 0.028 Uiso 1 1 calc R . . H62C H 1.0567 1.0783 0.0739 0.028 Uiso 1 1 calc R . . C51 C 0.79043(13) 0.92463(12) 0.22039(7) 0.0160(3) Uani 1 1 d . . . C52 C 0.72069(14) 0.97127(13) 0.20550(8) 0.0192(3) Uani 1 1 d . . . H52A H 0.7274 1.0248 0.2348 0.023 Uiso 1 1 calc R . . C53 C 0.64083(15) 0.93795(14) 0.14683(8) 0.0244(4) Uani 1 1 d . . . H53A H 0.5954 0.9702 0.1375 0.029 Uiso 1 1 calc R . . C54 C 0.62780(15) 0.85840(15) 0.10238(8) 0.0246(4) Uani 1 1 d . . . C55 C 0.69717(15) 0.81196(14) 0.11685(8) 0.0222(3) Uani 1 1 d . . . H55A H 0.6898 0.7584 0.0872 0.027 Uiso 1 1 calc R . . C56 C 0.77731(14) 0.84402(12) 0.17470(8) 0.0186(3) Uani 1 1 d . . . H56A H 0.8229 0.8118 0.1834 0.022 Uiso 1 1 calc R . . C57 C 0.53966(17) 0.82206(18) 0.03925(9) 0.0355(5) Uani 1 1 d . . . H57A H 0.5316 0.8760 0.0272 0.053 Uiso 1 1 calc R . . H57B H 0.4688 0.7788 0.0412 0.053 Uiso 1 1 calc R . . H57C H 0.5627 0.7883 0.0093 0.053 Uiso 1 1 calc R . . C101 C 0.99120(14) 0.67566(12) 0.39499(8) 0.0168(3) Uani 1 1 d . . . C102 C 0.98579(17) 0.61416(13) 0.34123(8) 0.0245(4) Uani 1 1 d . . . H10A H 1.0082 0.6396 0.3104 0.029 Uiso 1 1 calc R . . C103 C 0.94735(17) 0.51535(13) 0.33297(9) 0.0260(4) Uani 1 1 d . . . H10B H 0.9452 0.4754 0.2968 0.031 Uiso 1 1 calc R . . C104 C 0.91203(15) 0.47496(12) 0.37780(9) 0.0216(3) Uani 1 1 d . . . C105 C 0.92069(16) 0.53710(13) 0.43203(9) 0.0243(4) Uani 1 1 d . . . H10C H 0.9000 0.5119 0.4633 0.029 Uiso 1 1 calc R . . C106 C 0.95949(16) 0.63581(13) 0.44067(8) 0.0227(4) Uani 1 1 d . . . H10D H 0.9644 0.6759 0.4775 0.027 Uiso 1 1 calc R . . C107 C 0.86207(17) 0.36703(13) 0.36610(10) 0.0293(4) Uani 1 1 d . . . H10E H 0.8683 0.3523 0.4050 0.044 Uiso 1 1 calc R . . H10F H 0.9019 0.3399 0.3441 0.044 Uiso 1 1 calc R . . H10G H 0.7840 0.3399 0.3417 0.044 Uiso 1 1 calc R . . C151 C 1.41423(14) 1.10698(11) 0.60142(7) 0.0164(3) Uani 1 1 d . . . C152 C 1.40382(15) 1.11717(13) 0.66070(8) 0.0221(3) Uani 1 1 d . . . H15A H 1.3334 1.1045 0.6658 0.027 Uiso 1 1 calc R . . C153 C 1.49708(16) 1.14599(14) 0.71210(8) 0.0256(4) Uani 1 1 d . . . H15B H 1.4882 1.1515 0.7512 0.031 Uiso 1 1 calc R . . C154 C 1.60403(16) 1.16691(13) 0.70630(9) 0.0249(4) Uani 1 1 d . . . C155 C 1.61370(15) 1.15532(13) 0.64704(9) 0.0233(4) Uani 1 1 d . . . H15C H 1.6841 1.1682 0.6420 0.028 Uiso 1 1 calc R . . C156 C 1.51971(14) 1.12477(13) 0.59491(8) 0.0205(3) Uani 1 1 d . . . H15D H 1.5279 1.1163 0.5556 0.025 Uiso 1 1 calc R . . C157 C 1.70636(19) 1.20227(17) 0.76262(10) 0.0389(5) Uani 1 1 d . . . H15E H 1.7652 1.1899 0.7505 0.058 Uiso 1 1 calc R . . H15F H 1.6870 1.1688 0.7924 0.058 Uiso 1 1 calc R . . H15G H 1.7320 1.2706 0.7808 0.058 Uiso 1 1 calc R . . C201 C 1.21743(14) 1.36760(11) 0.43747(7) 0.0149(3) Uani 1 1 d . . . C202 C 1.33174(14) 1.41194(12) 0.44385(8) 0.0186(3) Uani 1 1 d . . . H20A H 1.3746 1.3762 0.4467 0.022 Uiso 1 1 calc R . . C203 C 1.38244(15) 1.50847(13) 0.44605(8) 0.0213(3) Uani 1 1 d . . . H20B H 1.4585 1.5363 0.4495 0.026 Uiso 1 1 calc R . . C204 C 1.32117(15) 1.56445(12) 0.44311(8) 0.0208(3) Uani 1 1 d . . . C205 C 1.20695(15) 1.51987(12) 0.43625(8) 0.0200(3) Uani 1 1 d . . . H20C H 1.1644 1.5559 0.4341 0.024 Uiso 1 1 calc R . . C206 C 1.15504(14) 1.42252(12) 0.43251(8) 0.0178(3) Uani 1 1 d . . . H20D H 1.0780 1.3938 0.4267 0.021 Uiso 1 1 calc R . . C207 C 1.37650(18) 1.66955(13) 0.44642(11) 0.0314(4) Uani 1 1 d . . . H20E H 1.3320 1.6823 0.4132 0.047 Uiso 1 1 calc R . . H20F H 1.4505 1.6845 0.4427 0.047 Uiso 1 1 calc R . . H20G H 1.3824 1.7090 0.4855 0.047 Uiso 1 1 calc R . . C291 C 1.12847(13) 1.03795(12) 0.24111(7) 0.0159(3) Uani 1 1 d . . . C292 C 1.20774(14) 1.13374(13) 0.26920(8) 0.0184(3) Uani 1 1 d . . . H29A H 1.2031 1.1815 0.2509 0.022 Uiso 1 1 calc R . . C293 C 1.29355(15) 1.15867(14) 0.32410(8) 0.0227(4) Uani 1 1 d . . . H29B H 1.3448 1.2231 0.3424 0.027 Uiso 1 1 calc R . . C294 C 1.30392(15) 1.08883(15) 0.35202(8) 0.0227(4) Uani 1 1 d . . . C295 C 1.22327(15) 0.99354(14) 0.32487(8) 0.0207(3) Uani 1 1 d . . . H29C H 1.2273 0.9461 0.3436 0.025 Uiso 1 1 calc R . . C296 C 1.13667(14) 0.96844(13) 0.27004(7) 0.0175(3) Uani 1 1 d . . . H29D H 1.0838 0.9045 0.2526 0.021 Uiso 1 1 calc R . . C297 C 1.40003(16) 1.11605(17) 0.41030(8) 0.0293(4) Uani 1 1 d . . . H29E H 1.3943 1.0593 0.4231 0.044 Uiso 1 1 calc R . . H29F H 1.3965 1.1628 0.4426 0.044 Uiso 1 1 calc R . . H29G H 1.4704 1.1434 0.4022 0.044 Uiso 1 1 calc R . . C341 C 0.83102(15) 0.64419(12) -0.02071(8) 0.0191(3) Uani 1 1 d . . . C342 C 0.81999(18) 0.58519(14) 0.01820(9) 0.0280(4) Uani 1 1 d . . . H34A H 0.8062 0.6043 0.0551 0.034 Uiso 1 1 calc R . . C343 C 0.82938(19) 0.49779(14) 0.00247(9) 0.0309(4) Uani 1 1 d . . . H34B H 0.8219 0.4591 0.0290 0.037 Uiso 1 1 calc R . . C344 C 0.84991(16) 0.46775(13) -0.05263(8) 0.0225(4) Uani 1 1 d . . . C345 C 0.86029(17) 0.52640(13) -0.09116(8) 0.0239(4) Uani 1 1 d . . . H34C H 0.8739 0.5073 -0.1282 0.029 Uiso 1 1 calc R . . C346 C 0.85083(17) 0.61407(13) -0.07565(8) 0.0236(4) Uani 1 1 d . . . H34D H 0.8579 0.6525 -0.1024 0.028 Uiso 1 1 calc R . . C347 C 0.8630(2) 0.37517(14) -0.06916(10) 0.0315(4) Uani 1 1 d . . . H34E H 0.9075 0.3789 -0.0967 0.047 Uiso 1 1 calc R . . H34F H 0.7900 0.3223 -0.0892 0.047 Uiso 1 1 calc R . . H34G H 0.8998 0.3648 -0.0321 0.047 Uiso 1 1 calc R . . C391 C 0.56667(14) 0.90369(12) -0.15860(7) 0.0170(3) Uani 1 1 d . . . C392 C 0.45211(15) 0.85529(13) -0.16916(8) 0.0223(4) Uani 1 1 d . . . H39A H 0.4271 0.8314 -0.1384 0.027 Uiso 1 1 calc R . . C393 C 0.37322(15) 0.84133(13) -0.22461(8) 0.0218(3) Uani 1 1 d . . . H39B H 0.2967 0.8077 -0.2308 0.026 Uiso 1 1 calc R . . C394 C 0.40895(15) 0.87775(12) -0.27079(8) 0.0188(3) Uani 1 1 d . . . C395 C 0.52395(15) 0.92578(13) -0.26024(8) 0.0211(3) Uani 1 1 d . . . H39C H 0.5491 0.9504 -0.2907 0.025 Uiso 1 1 calc R . . C396 C 0.60183(15) 0.93790(13) -0.20560(8) 0.0207(3) Uani 1 1 d . . . H39D H 0.6785 0.9692 -0.2001 0.025 Uiso 1 1 calc R . . C397 C 0.32569(17) 0.86637(13) -0.33058(8) 0.0257(4) Uani 1 1 d . . . H39E H 0.2510 0.8425 -0.3272 0.039 Uiso 1 1 calc R . . H39F H 0.3290 0.8214 -0.3640 0.039 Uiso 1 1 calc R . . H39G H 0.3440 0.9280 -0.3387 0.039 Uiso 1 1 calc R . . C441 C 0.82123(14) 1.28150(12) 0.11402(7) 0.0155(3) Uani 1 1 d . . . C442 C 0.71891(15) 1.28905(13) 0.09664(8) 0.0187(3) Uani 1 1 d . . . H44A H 0.6548 1.2351 0.0706 0.022 Uiso 1 1 calc R . . C443 C 0.71094(16) 1.37583(14) 0.11761(8) 0.0225(4) Uani 1 1 d . . . H44B H 0.6412 1.3785 0.1063 0.027 Uiso 1 1 calc R . . C444 C 0.90778(16) 1.45158(13) 0.17122(8) 0.0230(4) Uani 1 1 d . . . H44C H 0.9724 1.5066 0.1954 0.028 Uiso 1 1 calc R . . C445 C 0.80507(17) 1.45830(13) 0.15501(8) 0.0234(4) Uani 1 1 d . . . C446 C 0.91593(15) 1.36466(12) 0.15212(8) 0.0201(3) Uani 1 1 d . . . H44D H 0.9852 1.3617 0.1648 0.024 Uiso 1 1 calc R . . C447 C 0.7969(2) 1.55309(15) 0.17771(10) 0.0331(5) Uani 1 1 d . . . H44E H 0.7306 1.5525 0.1508 0.050 Uiso 1 1 calc R . . H44F H 0.8625 1.6058 0.1776 0.050 Uiso 1 1 calc R . . H44G H 0.7923 1.5610 0.2191 0.050 Uiso 1 1 calc R . . C1S C 0.5412(2) 0.3581(2) 0.30634(11) 0.0463(6) Uani 1 1 d . . . H1S H 0.5223 0.2897 0.2905 0.056 Uiso 1 1 calc R . . H2S H 0.4727 0.3672 0.2928 0.056 Uiso 1 1 calc R . . Cl1 Cl 0.58758(6) 0.39109(5) 0.38720(3) 0.05394(17) Uani 1 1 d . . . Cl2 Cl 0.63726(6) 0.42186(6) 0.27410(4) 0.0653(2) Uani 1 1 d . . . C2S C 0.1825(2) 0.41356(16) 0.28363(10) 0.0359(5) Uani 1 1 d . . . H3S H 0.1035 0.3716 0.2748 0.043 Uiso 1 1 calc R . . H4S H 0.2226 0.4188 0.3255 0.043 Uiso 1 1 calc R . . Cl3 Cl 0.19585(5) 0.52928(4) 0.27836(2) 0.03471(11) Uani 1 1 d . . . Cl4 Cl 0.23724(5) 0.36213(4) 0.23072(2) 0.03976(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01351(9) 0.01238(9) 0.01132(9) 0.00375(7) 0.00070(7) 0.00641(8) C21 0.0142(7) 0.0148(7) 0.0105(6) 0.0036(5) 0.0029(5) 0.0072(6) N22 0.0156(6) 0.0146(6) 0.0129(6) 0.0056(5) 0.0024(5) 0.0077(5) N23 0.0150(6) 0.0132(6) 0.0117(6) 0.0044(5) 0.0026(5) 0.0062(5) N24 0.0164(6) 0.0140(6) 0.0122(6) 0.0050(5) 0.0023(5) 0.0083(5) C1 0.0171(7) 0.0156(7) 0.0109(6) 0.0048(5) 0.0037(5) 0.0097(6) N2 0.0175(6) 0.0148(6) 0.0117(6) 0.0043(5) 0.0026(5) 0.0086(5) C3 0.0142(7) 0.0151(7) 0.0117(6) 0.0041(5) 0.0033(5) 0.0093(6) C4 0.0138(7) 0.0159(7) 0.0126(6) 0.0055(5) 0.0027(5) 0.0086(6) C5 0.0145(7) 0.0158(7) 0.0122(6) 0.0035(5) 0.0014(5) 0.0078(6) C6 0.0142(7) 0.0148(7) 0.0144(7) 0.0042(6) 0.0024(6) 0.0067(6) C7 0.0149(7) 0.0164(7) 0.0169(7) 0.0034(6) 0.0023(6) 0.0050(6) C8 0.0176(8) 0.0144(7) 0.0191(7) 0.0045(6) 0.0043(6) 0.0054(6) C9 0.0173(7) 0.0138(7) 0.0134(7) 0.0046(5) 0.0039(6) 0.0067(6) C10 0.0201(8) 0.0139(7) 0.0149(7) 0.0060(6) 0.0067(6) 0.0078(6) C11 0.0196(8) 0.0153(7) 0.0135(7) 0.0061(6) 0.0045(6) 0.0098(6) C12 0.0220(8) 0.0179(8) 0.0175(7) 0.0071(6) 0.0050(6) 0.0121(7) C13 0.0197(8) 0.0204(8) 0.0165(7) 0.0082(6) 0.0036(6) 0.0118(7) C14 0.0158(7) 0.0167(7) 0.0132(6) 0.0070(6) 0.0034(6) 0.0087(6) C15 0.0145(7) 0.0187(7) 0.0132(7) 0.0078(6) 0.0028(6) 0.0074(6) C16 0.0150(7) 0.0153(7) 0.0118(6) 0.0050(5) 0.0012(5) 0.0067(6) C17 0.0178(8) 0.0175(7) 0.0124(7) 0.0041(6) -0.0004(6) 0.0066(6) C18 0.0200(8) 0.0138(7) 0.0134(7) 0.0023(6) 0.0001(6) 0.0069(6) C19 0.0165(7) 0.0148(7) 0.0124(6) 0.0046(5) 0.0029(6) 0.0080(6) C20 0.0158(7) 0.0132(7) 0.0116(6) 0.0037(5) 0.0027(5) 0.0070(6) C61 0.0165(7) 0.0215(8) 0.0163(7) 0.0060(6) 0.0054(6) 0.0083(6) Ni2 0.01798(10) 0.01459(10) 0.01092(9) 0.00355(7) 0.00162(7) 0.00951(8) C45 0.0175(7) 0.0170(7) 0.0114(6) 0.0045(5) 0.0024(6) 0.0102(6) N46 0.0194(7) 0.0159(6) 0.0116(6) 0.0045(5) 0.0041(5) 0.0099(5) N47 0.0214(7) 0.0172(6) 0.0120(6) 0.0043(5) 0.0024(5) 0.0105(6) N48 0.0190(7) 0.0172(6) 0.0112(6) 0.0036(5) 0.0012(5) 0.0093(5) C25 0.0172(7) 0.0141(7) 0.0113(6) 0.0038(5) 0.0025(5) 0.0077(6) N26 0.0181(6) 0.0153(6) 0.0117(6) 0.0041(5) 0.0021(5) 0.0091(5) C27 0.0146(7) 0.0128(7) 0.0111(6) 0.0031(5) 0.0015(5) 0.0064(6) C28 0.0154(7) 0.0150(7) 0.0116(6) 0.0042(5) 0.0030(5) 0.0072(6) C29 0.0153(7) 0.0154(7) 0.0126(6) 0.0049(5) 0.0035(6) 0.0083(6) C30 0.0163(7) 0.0187(7) 0.0144(7) 0.0053(6) 0.0034(6) 0.0108(6) C31 0.0229(8) 0.0242(8) 0.0184(8) 0.0053(7) 0.0045(7) 0.0163(7) C32 0.0290(9) 0.0235(8) 0.0185(8) 0.0057(7) 0.0059(7) 0.0191(8) C33 0.0251(8) 0.0188(8) 0.0140(7) 0.0060(6) 0.0066(6) 0.0141(7) C34 0.0249(8) 0.0159(7) 0.0130(7) 0.0041(6) 0.0059(6) 0.0117(7) C35 0.0248(8) 0.0154(7) 0.0136(7) 0.0035(6) 0.0038(6) 0.0101(7) C36 0.0292(9) 0.0166(8) 0.0176(8) 0.0019(6) 0.0017(7) 0.0102(7) C37 0.0256(9) 0.0197(8) 0.0154(7) 0.0013(6) -0.0015(7) 0.0095(7) C38 0.0209(8) 0.0191(8) 0.0135(7) 0.0031(6) 0.0015(6) 0.0108(7) C39 0.0202(8) 0.0205(8) 0.0117(6) 0.0052(6) 0.0023(6) 0.0105(7) C40 0.0190(8) 0.0184(8) 0.0132(7) 0.0055(6) 0.0019(6) 0.0089(6) C41 0.0228(8) 0.0212(8) 0.0132(7) 0.0065(6) 0.0020(6) 0.0116(7) C42 0.0227(8) 0.0187(8) 0.0152(7) 0.0076(6) 0.0037(6) 0.0117(7) C43 0.0182(7) 0.0153(7) 0.0134(7) 0.0049(6) 0.0024(6) 0.0088(6) C44 0.0175(7) 0.0151(7) 0.0136(7) 0.0049(6) 0.0028(6) 0.0086(6) C62 0.0212(8) 0.0196(8) 0.0174(7) 0.0077(6) 0.0068(6) 0.0095(7) C51 0.0146(7) 0.0175(7) 0.0142(7) 0.0055(6) 0.0018(6) 0.0060(6) C52 0.0167(8) 0.0231(8) 0.0181(7) 0.0068(6) 0.0029(6) 0.0097(7) C53 0.0178(8) 0.0343(10) 0.0209(8) 0.0100(8) 0.0003(7) 0.0131(8) C54 0.0150(8) 0.0366(10) 0.0159(8) 0.0065(7) 0.0009(6) 0.0067(7) C55 0.0177(8) 0.0259(9) 0.0154(7) 0.0012(7) 0.0032(6) 0.0043(7) C56 0.0168(8) 0.0195(8) 0.0168(7) 0.0037(6) 0.0031(6) 0.0067(6) C57 0.0218(10) 0.0580(14) 0.0183(9) 0.0065(9) -0.0019(7) 0.0145(10) C101 0.0187(8) 0.0144(7) 0.0170(7) 0.0053(6) 0.0029(6) 0.0078(6) C102 0.0410(11) 0.0196(8) 0.0167(8) 0.0067(7) 0.0102(8) 0.0153(8) C103 0.0381(11) 0.0194(8) 0.0196(8) 0.0023(7) 0.0074(8) 0.0136(8) C104 0.0193(8) 0.0150(8) 0.0278(9) 0.0062(7) 0.0026(7) 0.0068(6) C105 0.0323(10) 0.0194(8) 0.0270(9) 0.0125(7) 0.0150(8) 0.0111(8) C106 0.0320(10) 0.0182(8) 0.0203(8) 0.0056(7) 0.0110(7) 0.0116(7) C107 0.0260(10) 0.0171(8) 0.0379(11) 0.0056(8) 0.0030(8) 0.0067(7) C151 0.0176(7) 0.0139(7) 0.0152(7) 0.0059(6) -0.0005(6) 0.0065(6) C152 0.0218(8) 0.0265(9) 0.0177(8) 0.0077(7) 0.0024(7) 0.0114(7) C153 0.0318(10) 0.0269(9) 0.0149(7) 0.0045(7) -0.0004(7) 0.0144(8) C154 0.0253(9) 0.0198(8) 0.0225(8) 0.0041(7) -0.0057(7) 0.0103(7) C155 0.0150(8) 0.0230(9) 0.0291(9) 0.0097(7) -0.0010(7) 0.0082(7) C156 0.0208(8) 0.0235(8) 0.0191(8) 0.0098(7) 0.0031(6) 0.0116(7) C157 0.0352(12) 0.0381(12) 0.0304(11) 0.0031(9) -0.0121(9) 0.0175(10) C201 0.0197(8) 0.0145(7) 0.0100(6) 0.0037(5) 0.0013(6) 0.0085(6) C202 0.0188(8) 0.0186(8) 0.0184(7) 0.0067(6) 0.0024(6) 0.0093(6) C203 0.0164(8) 0.0195(8) 0.0245(8) 0.0080(7) 0.0024(7) 0.0054(6) C204 0.0225(8) 0.0148(7) 0.0216(8) 0.0059(6) 0.0026(7) 0.0060(7) C205 0.0234(8) 0.0166(8) 0.0230(8) 0.0066(6) 0.0054(7) 0.0122(7) C206 0.0176(8) 0.0169(7) 0.0196(7) 0.0065(6) 0.0044(6) 0.0082(6) C207 0.0295(10) 0.0169(8) 0.0424(12) 0.0103(8) 0.0056(9) 0.0062(8) C291 0.0154(7) 0.0210(8) 0.0135(7) 0.0044(6) 0.0034(6) 0.0111(6) C292 0.0187(8) 0.0205(8) 0.0186(7) 0.0060(6) 0.0055(6) 0.0111(7) C293 0.0173(8) 0.0262(9) 0.0198(8) 0.0014(7) 0.0035(6) 0.0080(7) C294 0.0172(8) 0.0398(11) 0.0145(7) 0.0067(7) 0.0036(6) 0.0170(8) C295 0.0215(8) 0.0316(9) 0.0166(7) 0.0099(7) 0.0063(6) 0.0178(7) C296 0.0185(8) 0.0219(8) 0.0160(7) 0.0062(6) 0.0046(6) 0.0128(7) C297 0.0207(9) 0.0477(12) 0.0158(8) 0.0065(8) 0.0000(7) 0.0149(9) C341 0.0264(9) 0.0169(8) 0.0157(7) 0.0044(6) 0.0044(6) 0.0122(7) C342 0.0500(12) 0.0267(9) 0.0192(8) 0.0107(7) 0.0174(8) 0.0235(9) C343 0.0556(13) 0.0263(10) 0.0245(9) 0.0151(8) 0.0184(9) 0.0250(10) C344 0.0322(10) 0.0164(8) 0.0212(8) 0.0058(6) 0.0080(7) 0.0128(7) C345 0.0367(10) 0.0186(8) 0.0198(8) 0.0042(7) 0.0119(8) 0.0141(8) C346 0.0397(11) 0.0185(8) 0.0185(8) 0.0084(6) 0.0121(8) 0.0155(8) C347 0.0512(13) 0.0219(9) 0.0303(10) 0.0099(8) 0.0155(10) 0.0223(9) C391 0.0214(8) 0.0156(7) 0.0131(7) 0.0028(6) 0.0017(6) 0.0099(6) C392 0.0231(9) 0.0245(9) 0.0177(8) 0.0111(7) 0.0035(7) 0.0074(7) C393 0.0187(8) 0.0215(8) 0.0197(8) 0.0073(7) -0.0002(6) 0.0053(7) C394 0.0239(8) 0.0158(7) 0.0147(7) 0.0037(6) 0.0012(6) 0.0094(7) C395 0.0266(9) 0.0248(9) 0.0147(7) 0.0074(6) 0.0072(7) 0.0126(7) C396 0.0198(8) 0.0253(9) 0.0181(8) 0.0050(7) 0.0061(6) 0.0114(7) C397 0.0322(10) 0.0204(8) 0.0177(8) 0.0056(7) -0.0027(7) 0.0097(8) C441 0.0205(8) 0.0168(7) 0.0122(6) 0.0062(6) 0.0038(6) 0.0106(6) C442 0.0213(8) 0.0212(8) 0.0156(7) 0.0079(6) 0.0044(6) 0.0109(7) C443 0.0267(9) 0.0290(9) 0.0210(8) 0.0119(7) 0.0096(7) 0.0183(8) C444 0.0306(9) 0.0170(8) 0.0181(8) 0.0020(6) 0.0034(7) 0.0104(7) C445 0.0393(11) 0.0239(9) 0.0158(7) 0.0070(7) 0.0095(7) 0.0217(8) C446 0.0231(8) 0.0206(8) 0.0176(7) 0.0047(6) 0.0035(6) 0.0123(7) C447 0.0524(13) 0.0274(10) 0.0286(10) 0.0061(8) 0.0125(9) 0.0276(10) C1S 0.0398(13) 0.0634(17) 0.0396(13) 0.0165(12) 0.0118(11) 0.0255(13) Cl1 0.0478(4) 0.0616(4) 0.0439(3) 0.0113(3) 0.0136(3) 0.0162(3) Cl2 0.0544(4) 0.0718(5) 0.0532(4) 0.0236(4) 0.0111(3) 0.0091(4) C2S 0.0528(14) 0.0308(11) 0.0236(10) 0.0132(8) 0.0130(10) 0.0136(10) Cl3 0.0427(3) 0.0375(3) 0.0331(3) 0.0170(2) 0.0141(2) 0.0224(2) Cl4 0.0633(4) 0.0309(3) 0.0282(2) 0.0115(2) 0.0143(3) 0.0218(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N24 1.9408(13) . ? Ni1 N22 1.9429(14) . ? Ni1 N23 1.9577(13) . ? Ni1 C21 2.0327(15) . ? C21 C1 1.471(2) . ? C21 C4 1.477(2) . ? C21 C61 1.547(2) . ? N22 C9 1.386(2) . ? N22 C6 1.3892(19) . ? N23 C14 1.372(2) . ? N23 C11 1.376(2) . ? N24 C19 1.384(2) . ? N24 C16 1.3862(19) . ? C1 N2 1.3652(19) . ? C1 C20 1.388(2) . ? N2 C3 1.337(2) . ? C3 C4 1.426(2) . ? C3 C27 1.472(2) . ? C4 C5 1.389(2) . ? C5 C6 1.410(2) . ? C5 C51 1.480(2) . ? C6 C7 1.440(2) . ? C7 C8 1.349(2) . ? C7 H7A 0.9300 . ? C8 C9 1.434(2) . ? C8 H8A 0.9300 . ? C9 C10 1.396(2) . ? C10 C11 1.387(2) . ? C10 C101 1.500(2) . ? C11 C12 1.435(2) . ? C12 C13 1.353(2) . ? C12 H12A 0.9300 . ? C13 C14 1.437(2) . ? C13 H13A 0.9300 . ? C14 C15 1.395(2) . ? C15 C16 1.392(2) . ? C15 C151 1.498(2) . ? C16 C17 1.442(2) . ? C17 C18 1.350(2) . ? C17 H17A 0.9300 . ? C18 C19 1.439(2) . ? C18 H18A 0.9300 . ? C19 C20 1.402(2) . ? C20 C201 1.486(2) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? Ni2 N48 1.9446(13) . ? Ni2 N46 1.9491(13) . ? Ni2 N47 1.9522(14) . ? Ni2 C45 2.0163(16) . ? C45 C28 1.461(2) . ? C45 C25 1.470(2) . ? C45 C62 1.554(2) . ? N46 C33 1.377(2) . ? N46 C30 1.390(2) . ? N47 C35 1.379(2) . ? N47 C38 1.380(2) . ? N48 C40 1.385(2) . ? N48 C43 1.393(2) . ? C25 N26 1.369(2) . ? C25 C44 1.396(2) . ? N26 C27 1.3481(19) . ? C27 C28 1.412(2) . ? C28 C29 1.395(2) . ? C29 C30 1.394(2) . ? C29 C291 1.487(2) . ? C30 C31 1.440(2) . ? C31 C32 1.343(2) . ? C31 H31A 0.9300 . ? C32 C33 1.438(2) . ? C32 H32A 0.9300 . ? C33 C34 1.388(2) . ? C34 C35 1.397(2) . ? C34 C341 1.494(2) . ? C35 C36 1.437(2) . ? C36 C37 1.350(2) . ? C36 H36A 0.9300 . ? C37 C38 1.430(2) . ? C37 H37A 0.9300 . ? C38 C39 1.392(2) . ? C39 C40 1.391(2) . ? C39 C391 1.500(2) . ? C40 C41 1.441(2) . ? C41 C42 1.345(2) . ? C41 H41A 0.9300 . ? C42 C43 1.438(2) . ? C42 H42A 0.9300 . ? C43 C44 1.398(2) . ? C44 C441 1.484(2) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C51 C52 1.395(2) . ? C51 C56 1.405(2) . ? C52 C53 1.396(2) . ? C52 H52A 0.9300 . ? C53 C54 1.378(3) . ? C53 H53A 0.9300 . ? C54 C55 1.387(3) . ? C54 C57 1.514(2) . ? C55 C56 1.385(2) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C101 C106 1.387(2) . ? C101 C102 1.388(2) . ? C102 C103 1.386(3) . ? C102 H10A 0.9300 . ? C103 C104 1.389(3) . ? C103 H10B 0.9300 . ? C104 C105 1.384(3) . ? C104 C107 1.502(2) . ? C105 C106 1.383(2) . ? C105 H10C 0.9300 . ? C106 H10D 0.9300 . ? C107 H10E 0.9600 . ? C107 H10F 0.9600 . ? C107 H10G 0.9600 . ? C151 C156 1.387(2) . ? C151 C152 1.392(2) . ? C152 C153 1.384(2) . ? C152 H15A 0.9300 . ? C153 C154 1.393(3) . ? C153 H15B 0.9300 . ? C154 C155 1.388(3) . ? C154 C157 1.509(3) . ? C155 C156 1.396(2) . ? C155 H15C 0.9300 . ? C156 H15D 0.9300 . ? C157 H15E 0.9600 . ? C157 H15F 0.9600 . ? C157 H15G 0.9600 . ? C201 C206 1.393(2) . ? C201 C202 1.393(2) . ? C202 C203 1.386(2) . ? C202 H20A 0.9300 . ? C203 C204 1.392(2) . ? C203 H20B 0.9300 . ? C204 C205 1.390(3) . ? C204 C207 1.503(3) . ? C205 C206 1.389(2) . ? C205 H20C 0.9300 . ? C206 H20D 0.9300 . ? C207 H20E 0.9600 . ? C207 H20F 0.9600 . ? C207 H20G 0.9600 . ? C291 C296 1.391(2) . ? C291 C292 1.396(2) . ? C292 C293 1.390(2) . ? C292 H29A 0.9300 . ? C293 C294 1.389(3) . ? C293 H29B 0.9300 . ? C294 C295 1.394(3) . ? C294 C297 1.510(2) . ? C295 C296 1.394(2) . ? C295 H29C 0.9300 . ? C296 H29D 0.9300 . ? C297 H29E 0.9600 . ? C297 H29F 0.9600 . ? C297 H29G 0.9600 . ? C341 C346 1.384(2) . ? C341 C342 1.388(2) . ? C342 C343 1.392(3) . ? C342 H34A 0.9300 . ? C343 C344 1.392(3) . ? C343 H34B 0.9300 . ? C344 C345 1.377(3) . ? C344 C347 1.495(2) . ? C345 C346 1.396(2) . ? C345 H34C 0.9300 . ? C346 H34D 0.9300 . ? C347 H34E 0.9600 . ? C347 H34F 0.9600 . ? C347 H34G 0.9600 . ? C391 C392 1.383(3) . ? C391 C396 1.392(2) . ? C392 C393 1.392(2) . ? C392 H39A 0.9300 . ? C393 C394 1.392(3) . ? C393 H39B 0.9300 . ? C394 C395 1.388(3) . ? C394 C397 1.506(2) . ? C395 C396 1.380(2) . ? C395 H39C 0.9300 . ? C396 H39D 0.9300 . ? C397 H39E 0.9600 . ? C397 H39F 0.9600 . ? C397 H39G 0.9600 . ? C441 C442 1.394(2) . ? C441 C446 1.396(2) . ? C442 C443 1.391(2) . ? C442 H44A 0.9300 . ? C443 C445 1.383(3) . ? C443 H44B 0.9300 . ? C444 C446 1.387(2) . ? C444 C445 1.390(3) . ? C444 H44C 0.9300 . ? C445 C447 1.515(2) . ? C446 H44D 0.9300 . ? C447 H44E 0.9600 . ? C447 H44F 0.9600 . ? C447 H44G 0.9600 . ? C1S Cl2 1.721(3) . ? C1S Cl1 1.743(3) . ? C1S H1S 0.9700 . ? C1S H2S 0.9700 . ? C2S Cl3 1.764(2) . ? C2S Cl4 1.767(2) . ? C2S H3S 0.9700 . ? C2S H4S 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N24 Ni1 N22 174.53(6) . . ? N24 Ni1 N23 90.98(5) . . ? N22 Ni1 N23 90.98(5) . . ? N24 Ni1 C21 89.29(6) . . ? N22 Ni1 C21 88.44(6) . . ? N23 Ni1 C21 176.47(6) . . ? C1 C21 C4 100.58(12) . . ? C1 C21 C61 112.22(13) . . ? C4 C21 C61 113.81(13) . . ? C1 C21 Ni1 118.60(10) . . ? C4 C21 Ni1 118.36(10) . . ? C61 C21 Ni1 93.99(9) . . ? C9 N22 C6 104.14(13) . . ? C9 N22 Ni1 125.75(10) . . ? C6 N22 Ni1 129.00(11) . . ? C14 N23 C11 104.97(12) . . ? C14 N23 Ni1 127.27(10) . . ? C11 N23 Ni1 127.28(10) . . ? C19 N24 C16 104.38(12) . . ? C19 N24 Ni1 129.26(10) . . ? C16 N24 Ni1 126.05(10) . . ? N2 C1 C20 120.93(14) . . ? N2 C1 C21 113.55(13) . . ? C20 C1 C21 125.44(13) . . ? C3 N2 C1 106.26(13) . . ? N2 C3 C4 112.55(13) . . ? N2 C3 C27 118.77(14) . . ? C4 C3 C27 128.11(14) . . ? C5 C4 C3 129.11(14) . . ? C5 C4 C21 124.05(14) . . ? C3 C4 C21 106.84(13) . . ? C4 C5 C6 118.81(14) . . ? C4 C5 C51 123.32(14) . . ? C6 C5 C51 117.85(14) . . ? N22 C6 C5 124.86(14) . . ? N22 C6 C7 110.63(13) . . ? C5 C6 C7 124.06(14) . . ? C8 C7 C6 106.98(14) . . ? C8 C7 H7A 126.5 . . ? C6 C7 H7A 126.5 . . ? C7 C8 C9 107.01(14) . . ? C7 C8 H8A 126.5 . . ? C9 C8 H8A 126.5 . . ? N22 C9 C10 124.95(14) . . ? N22 C9 C8 111.00(13) . . ? C10 C9 C8 123.74(15) . . ? C11 C10 C9 122.94(14) . . ? C11 C10 C101 119.50(14) . . ? C9 C10 C101 117.56(14) . . ? N23 C11 C10 124.19(14) . . ? N23 C11 C12 110.51(14) . . ? C10 C11 C12 125.03(15) . . ? C13 C12 C11 107.06(14) . . ? C13 C12 H12A 126.5 . . ? C11 C12 H12A 126.5 . . ? C12 C13 C14 106.42(14) . . ? C12 C13 H13A 126.8 . . ? C14 C13 H13A 126.8 . . ? N23 C14 C15 123.95(14) . . ? N23 C14 C13 110.91(14) . . ? C15 C14 C13 124.59(14) . . ? C16 C15 C14 122.74(14) . . ? C16 C15 C151 118.29(14) . . ? C14 C15 C151 118.96(14) . . ? N24 C16 C15 125.39(14) . . ? N24 C16 C17 110.70(13) . . ? C15 C16 C17 123.35(14) . . ? C18 C17 C16 106.87(14) . . ? C18 C17 H17A 126.6 . . ? C16 C17 H17A 126.6 . . ? C17 C18 C19 106.97(14) . . ? C17 C18 H18A 126.5 . . ? C19 C18 H18A 126.5 . . ? N24 C19 C20 125.35(14) . . ? N24 C19 C18 110.85(13) . . ? C20 C19 C18 123.39(14) . . ? C1 C20 C19 119.56(14) . . ? C1 C20 C201 121.59(13) . . ? C19 C20 C201 118.31(13) . . ? C21 C61 H61A 109.5 . . ? C21 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C21 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N48 Ni2 N46 174.13(6) . . ? N48 Ni2 N47 91.31(6) . . ? N46 Ni2 N47 91.47(6) . . ? N48 Ni2 C45 88.47(6) . . ? N46 Ni2 C45 88.37(6) . . ? N47 Ni2 C45 175.59(7) . . ? C28 C45 C25 100.85(13) . . ? C28 C45 C62 113.00(13) . . ? C25 C45 C62 113.18(13) . . ? C28 C45 Ni2 117.68(11) . . ? C25 C45 Ni2 118.48(11) . . ? C62 C45 Ni2 94.38(10) . . ? C33 N46 C30 104.59(13) . . ? C33 N46 Ni2 125.15(10) . . ? C30 N46 Ni2 128.99(11) . . ? C35 N47 C38 104.83(13) . . ? C35 N47 Ni2 127.19(11) . . ? C38 N47 Ni2 127.56(11) . . ? C40 N48 C43 104.80(12) . . ? C40 N48 Ni2 125.51(11) . . ? C43 N48 Ni2 128.82(10) . . ? N26 C25 C44 122.75(14) . . ? N26 C25 C45 113.38(13) . . ? C44 C25 C45 123.86(14) . . ? C27 N26 C25 105.69(13) . . ? N26 C27 C28 112.52(13) . . ? N26 C27 C3 121.68(13) . . ? C28 C27 C3 125.75(13) . . ? C29 C28 C27 128.67(14) . . ? C29 C28 C45 123.68(14) . . ? C27 C28 C45 107.52(13) . . ? C30 C29 C28 117.75(14) . . ? C30 C29 C291 120.99(13) . . ? C28 C29 C291 121.26(14) . . ? N46 C30 C29 124.33(14) . . ? N46 C30 C31 110.25(14) . . ? C29 C30 C31 124.72(14) . . ? C32 C31 C30 106.98(15) . . ? C32 C31 H31A 126.5 . . ? C30 C31 H31A 126.5 . . ? C31 C32 C33 107.22(15) . . ? C31 C32 H32A 126.4 . . ? C33 C32 H32A 126.4 . . ? N46 C33 C34 126.46(14) . . ? N46 C33 C32 110.62(14) . . ? C34 C33 C32 122.91(15) . . ? C33 C34 C35 122.66(15) . . ? C33 C34 C341 117.62(14) . . ? C35 C34 C341 119.55(14) . . ? N47 C35 C34 123.80(15) . . ? N47 C35 C36 110.59(14) . . ? C34 C35 C36 125.21(15) . . ? C37 C36 C35 106.67(15) . . ? C37 C36 H36A 126.7 . . ? C35 C36 H36A 126.7 . . ? C36 C37 C38 107.27(15) . . ? C36 C37 H37A 126.4 . . ? C38 C37 H37A 126.4 . . ? N47 C38 C39 124.14(15) . . ? N47 C38 C37 110.52(14) . . ? C39 C38 C37 125.26(15) . . ? C40 C39 C38 122.84(15) . . ? C40 C39 C391 118.21(14) . . ? C38 C39 C391 118.89(15) . . ? N48 C40 C39 126.02(14) . . ? N48 C40 C41 110.43(14) . . ? C39 C40 C41 123.34(14) . . ? C42 C41 C40 107.08(14) . . ? C42 C41 H41A 126.5 . . ? C40 C41 H41A 126.5 . . ? C41 C42 C43 107.51(14) . . ? C41 C42 H42A 126.2 . . ? C43 C42 H42A 126.2 . . ? N48 C43 C44 125.76(14) . . ? N48 C43 C42 110.05(13) . . ? C44 C43 C42 123.86(14) . . ? C25 C44 C43 118.20(14) . . ? C25 C44 C441 121.62(14) . . ? C43 C44 C441 120.17(13) . . ? C45 C62 H62A 109.5 . . ? C45 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C45 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C52 C51 C56 117.90(15) . . ? C52 C51 C5 121.16(15) . . ? C56 C51 C5 120.93(14) . . ? C51 C52 C53 120.37(16) . . ? C51 C52 H52A 119.8 . . ? C53 C52 H52A 119.8 . . ? C54 C53 C52 121.44(16) . . ? C54 C53 H53A 119.3 . . ? C52 C53 H53A 119.3 . . ? C53 C54 C55 118.44(16) . . ? C53 C54 C57 120.94(18) . . ? C55 C54 C57 120.62(18) . . ? C56 C55 C54 121.09(17) . . ? C56 C55 H55A 119.5 . . ? C54 C55 H55A 119.5 . . ? C55 C56 C51 120.75(16) . . ? C55 C56 H56A 119.6 . . ? C51 C56 H56A 119.6 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C106 C101 C102 118.21(15) . . ? C106 C101 C10 120.94(15) . . ? C102 C101 C10 120.78(15) . . ? C103 C102 C101 120.75(17) . . ? C103 C102 H10A 119.6 . . ? C101 C102 H10A 119.6 . . ? C102 C103 C104 121.08(17) . . ? C102 C103 H10B 119.5 . . ? C104 C103 H10B 119.5 . . ? C105 C104 C103 117.78(16) . . ? C105 C104 C107 121.69(18) . . ? C103 C104 C107 120.48(17) . . ? C106 C105 C104 121.37(17) . . ? C106 C105 H10C 119.3 . . ? C104 C105 H10C 119.3 . . ? C105 C106 C101 120.75(16) . . ? C105 C106 H10D 119.6 . . ? C101 C106 H10D 119.6 . . ? C104 C107 H10E 109.5 . . ? C104 C107 H10F 109.5 . . ? H10E C107 H10F 109.5 . . ? C104 C107 H10G 109.5 . . ? H10E C107 H10G 109.5 . . ? H10F C107 H10G 109.5 . . ? C156 C151 C152 118.56(15) . . ? C156 C151 C15 120.29(15) . . ? C152 C151 C15 121.14(15) . . ? C153 C152 C151 120.70(17) . . ? C153 C152 H15A 119.7 . . ? C151 C152 H15A 119.7 . . ? C152 C153 C154 121.24(18) . . ? C152 C153 H15B 119.4 . . ? C154 C153 H15B 119.4 . . ? C155 C154 C153 117.83(16) . . ? C155 C154 C157 120.99(19) . . ? C153 C154 C157 121.17(19) . . ? C154 C155 C156 121.23(17) . . ? C154 C155 H15C 119.4 . . ? C156 C155 H15C 119.4 . . ? C151 C156 C155 120.41(17) . . ? C151 C156 H15D 119.8 . . ? C155 C156 H15D 119.8 . . ? C154 C157 H15E 109.5 . . ? C154 C157 H15F 109.5 . . ? H15E C157 H15F 109.5 . . ? C154 C157 H15G 109.5 . . ? H15E C157 H15G 109.5 . . ? H15F C157 H15G 109.5 . . ? C206 C201 C202 118.24(15) . . ? C206 C201 C20 121.53(15) . . ? C202 C201 C20 120.22(14) . . ? C203 C202 C201 120.94(15) . . ? C203 C202 H20A 119.5 . . ? C201 C202 H20A 119.5 . . ? C202 C203 C204 120.99(16) . . ? C202 C203 H20B 119.5 . . ? C204 C203 H20B 119.5 . . ? C205 C204 C203 117.96(15) . . ? C205 C204 C207 121.02(16) . . ? C203 C204 C207 121.02(17) . . ? C206 C205 C204 121.32(15) . . ? C206 C205 H20C 119.3 . . ? C204 C205 H20C 119.3 . . ? C205 C206 C201 120.50(16) . . ? C205 C206 H20D 119.7 . . ? C201 C206 H20D 119.7 . . ? C204 C207 H20E 109.5 . . ? C204 C207 H20F 109.5 . . ? H20E C207 H20F 109.5 . . ? C204 C207 H20G 109.5 . . ? H20E C207 H20G 109.5 . . ? H20F C207 H20G 109.5 . . ? C296 C291 C292 118.21(15) . . ? C296 C291 C29 123.07(15) . . ? C292 C291 C29 118.71(15) . . ? C293 C292 C291 120.87(16) . . ? C293 C292 H29A 119.6 . . ? C291 C292 H29A 119.6 . . ? C294 C293 C292 120.97(17) . . ? C294 C293 H29B 119.5 . . ? C292 C293 H29B 119.5 . . ? C293 C294 C295 118.21(15) . . ? C293 C294 C297 120.56(18) . . ? C295 C294 C297 121.23(17) . . ? C296 C295 C294 120.90(16) . . ? C296 C295 H29C 119.6 . . ? C294 C295 H29C 119.6 . . ? C291 C296 C295 120.78(16) . . ? C291 C296 H29D 119.6 . . ? C295 C296 H29D 119.6 . . ? C294 C297 H29E 109.5 . . ? C294 C297 H29F 109.5 . . ? H29E C297 H29F 109.5 . . ? C294 C297 H29G 109.5 . . ? H29E C297 H29G 109.5 . . ? H29F C297 H29G 109.5 . . ? C346 C341 C342 118.66(15) . . ? C346 C341 C34 120.38(15) . . ? C342 C341 C34 120.83(15) . . ? C341 C342 C343 120.67(17) . . ? C341 C342 H34A 119.7 . . ? C343 C342 H34A 119.7 . . ? C342 C343 C344 120.66(17) . . ? C342 C343 H34B 119.7 . . ? C344 C343 H34B 119.7 . . ? C345 C344 C343 118.40(16) . . ? C345 C344 C347 120.55(17) . . ? C343 C344 C347 121.04(16) . . ? C344 C345 C346 121.18(17) . . ? C344 C345 H34C 119.4 . . ? C346 C345 H34C 119.4 . . ? C341 C346 C345 120.43(16) . . ? C341 C346 H34D 119.8 . . ? C345 C346 H34D 119.8 . . ? C344 C347 H34E 109.5 . . ? C344 C347 H34F 109.5 . . ? H34E C347 H34F 109.5 . . ? C344 C347 H34G 109.5 . . ? H34E C347 H34G 109.5 . . ? H34F C347 H34G 109.5 . . ? C392 C391 C396 117.97(15) . . ? C392 C391 C39 120.41(15) . . ? C396 C391 C39 121.58(16) . . ? C391 C392 C393 121.71(17) . . ? C391 C392 H39A 119.1 . . ? C393 C392 H39A 119.1 . . ? C394 C393 C392 119.96(17) . . ? C394 C393 H39B 120.0 . . ? C392 C393 H39B 120.0 . . ? C395 C394 C393 118.22(15) . . ? C395 C394 C397 120.48(16) . . ? C393 C394 C397 121.30(16) . . ? C396 C395 C394 121.54(17) . . ? C396 C395 H39C 119.2 . . ? C394 C395 H39C 119.2 . . ? C395 C396 C391 120.56(17) . . ? C395 C396 H39D 119.7 . . ? C391 C396 H39D 119.7 . . ? C394 C397 H39E 109.5 . . ? C394 C397 H39F 109.5 . . ? H39E C397 H39F 109.5 . . ? C394 C397 H39G 109.5 . . ? H39E C397 H39G 109.5 . . ? H39F C397 H39G 109.5 . . ? C442 C441 C446 117.64(15) . . ? C442 C441 C44 122.08(15) . . ? C446 C441 C44 120.27(14) . . ? C443 C442 C441 121.17(16) . . ? C443 C442 H44A 119.4 . . ? C441 C442 H44A 119.4 . . ? C445 C443 C442 121.05(16) . . ? C445 C443 H44B 119.5 . . ? C442 C443 H44B 119.5 . . ? C446 C444 C445 121.45(17) . . ? C446 C444 H44C 119.3 . . ? C445 C444 H44C 119.3 . . ? C443 C445 C444 117.90(16) . . ? C443 C445 C447 121.22(17) . . ? C444 C445 C447 120.87(18) . . ? C444 C446 C441 120.74(16) . . ? C444 C446 H44D 119.6 . . ? C441 C446 H44D 119.6 . . ? C445 C447 H44E 109.5 . . ? C445 C447 H44F 109.5 . . ? H44E C447 H44F 109.5 . . ? C445 C447 H44G 109.5 . . ? H44E C447 H44G 109.5 . . ? H44F C447 H44G 109.5 . . ? Cl2 C1S Cl1 114.50(15) . . ? Cl2 C1S H1S 108.6 . . ? Cl1 C1S H1S 108.6 . . ? Cl2 C1S H2S 108.6 . . ? Cl1 C1S H2S 108.6 . . ? H1S C1S H2S 107.6 . . ? Cl3 C2S Cl4 110.90(12) . . ? Cl3 C2S H3S 109.5 . . ? Cl4 C2S H3S 109.5 . . ? Cl3 C2S H4S 109.5 . . ? Cl4 C2S H4S 109.5 . . ? H3S C2S H4S 108.0 . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.476 _refine_diff_density_min -1.575 _refine_diff_density_rms 0.099 # Attachment '7324_web_deposit_cif_file_1_PiotrJ.Chmielewski_1316792793.P3.cif' data_chni22 _database_code_depnum_ccdc_archive 'CCDC 825667' #TrackingRef '7324_web_deposit_cif_file_1_PiotrJ.Chmielewski_1316792793.P3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C98 H74 N8 Ni2' _chemical_formula_sum 'C98 H74 N8 Ni2' _chemical_formula_weight 1481.07 _chemical_absolute_configuration S 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 14.485(1) _cell_length_b 14.485(1) _cell_length_c 35.711(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7492.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16418 _cell_measurement_theta_min 4.7589 _cell_measurement_theta_max 38.5679 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3096 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 48854 48836 48912 48834 73301 65107 65139 97649 N (int>3sigma) = 0 13852 13807 14163 13791 20911 18332 18412 27655 Mean intensity = 0.0 21.2 20.9 21.8 21.9 21.3 21.3 21.5 21.8 Mean int/sigma = 0.0 4.7 4.7 4.9 4.8 4.8 4.8 4.8 4.8 Crystal system T and Lattice type P selected Mean |E*E-1| = 0.688 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: 41/43 42 n-- -b- -c- -n- -21- --c N 65 44 832 2896 2850 2850 36 2429 N I>3s 1 1 255 1363 1290 1217 0 943 1.0 1.3 31.3 59.8 65.1 56.3 1.6 32.8 0.6 0.8 6.4 12.5 12.6 11.7 0.4 7.6 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] P4(1)2(1)2 # 92 chiral 1 245 0.125 48438 0.8 / 4.8 10.83 [B] P4(3)2(1)2 # 96 chiral 1 245 0.125 48438 0.8 / 4.8 10.83 Option [A] chosen The structure can be solved and satisfactorily refined within both space groups. Within P4(1)2(1)2 the Flack parameter x = -0.016(12), while in the case of inverted structure in P4(3)2(1)2 x = 1.009(12). ; _diffrn_ambient_temperature 100(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 'Xcalibur with Onyx CCD' _diffrn_measurement_method '\w and \p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 64868 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 4.77 _diffrn_reflns_theta_max 26.99 _reflns_number_total 8141 _reflns_number_gt 5762 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881; 3476 Friedel pairs' _refine_ls_abs_structure_Flack -0.016(12) _refine_ls_number_reflns 8141 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _refine_ls_shift/su_max 0.004 _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 0.57135(2) 0.69898(2) 0.113050(9) 0.02951(10) Uani 1 1 d . . . C21 C 0.68075(18) 0.73490(18) 0.08198(7) 0.0264(6) Uani 1 1 d . . . N22 N 0.58967(14) 0.57108(14) 0.09728(6) 0.0289(5) Uani 1 1 d . . . N24 N 0.56020(15) 0.82765(14) 0.12898(5) 0.0296(5) Uani 1 1 d . . . N23 N 0.47371(16) 0.66019(15) 0.14786(6) 0.0375(6) Uani 1 1 d . . . C1 C 0.69076(18) 0.82972(17) 0.06780(6) 0.0261(6) Uani 1 1 d . . . N2 N 0.72134(14) 0.83349(15) 0.03167(5) 0.0275(5) Uani 1 1 d . . . C3 C 0.72639(17) 0.74601(18) 0.01986(7) 0.0250(6) Uani 1 1 d . . . C4 C 0.70298(18) 0.68155(17) 0.04783(7) 0.0275(6) Uani 1 1 d . . . C5 C 0.70068(19) 0.58611(18) 0.04528(7) 0.0310(6) Uani 1 1 d . . . C6 C 0.6541(2) 0.53525(19) 0.07240(7) 0.0307(6) Uani 1 1 d . . . C7 C 0.65900(19) 0.43720(19) 0.07537(7) 0.0335(6) Uani 1 1 d . . . H7A H 0.6977 0.3984 0.0618 0.040 Uiso 1 1 calc R . . C8 C 0.5974(2) 0.41150(19) 0.10139(7) 0.0353(7) Uani 1 1 d . . . H8A H 0.5861 0.3516 0.1096 0.042 Uiso 1 1 calc R . . C9 C 0.55188(19) 0.49426(19) 0.11422(8) 0.0347(7) Uani 1 1 d . . . C10 C 0.4794(2) 0.4937(2) 0.13924(9) 0.0449(8) Uani 1 1 d . . . C11 C 0.4400(2) 0.5728(2) 0.15320(9) 0.0476(7) Uani 1 1 d . . . C12 C 0.3617(2) 0.5752(2) 0.17816(11) 0.0666(11) Uani 1 1 d . . . H12A H 0.3258 0.5252 0.1855 0.080 Uiso 1 1 calc R . . C13 C 0.3504(2) 0.6638(2) 0.18874(11) 0.0647(11) Uani 1 1 d . . . H13A H 0.3058 0.6867 0.2050 0.078 Uiso 1 1 calc R . . C14 C 0.4209(2) 0.71591(19) 0.16995(8) 0.0443(7) Uani 1 1 d . . . C15 C 0.4370(2) 0.8096(2) 0.17560(8) 0.0463(8) Uani 1 1 d . . . C16 C 0.5036(2) 0.8595(2) 0.15730(8) 0.0378(7) Uani 1 1 d . . . C17 C 0.5232(2) 0.9548(2) 0.16483(8) 0.0428(8) Uani 1 1 d . . . H17A H 0.4954 0.9908 0.1832 0.051 Uiso 1 1 calc R . . C18 C 0.5876(2) 0.98250(18) 0.14103(8) 0.0378(7) Uani 1 1 d . . . H18A H 0.6128 1.0414 0.1395 0.045 Uiso 1 1 calc R . . C19 C 0.61136(18) 0.90465(18) 0.11799(7) 0.0300(6) Uani 1 1 d . . . C20 C 0.66908(17) 0.90989(17) 0.08669(7) 0.0272(6) Uani 1 1 d . . . C31 C 0.75295(18) 0.71596(18) 0.11348(7) 0.0312(6) Uani 1 1 d . . . H31A H 0.8138 0.7293 0.1043 0.047 Uiso 1 1 calc R . . H31B H 0.7497 0.6523 0.1209 0.047 Uiso 1 1 calc R . . H31C H 0.7398 0.7546 0.1347 0.047 Uiso 1 1 calc R . . C51 C 0.7470(2) 0.53517(19) 0.01395(7) 0.0395(7) Uani 1 1 d . . . C52 C 0.8424(3) 0.5364(2) 0.01047(9) 0.0498(9) Uani 1 1 d . . . H52A H 0.8777 0.5711 0.0270 0.060 Uiso 1 1 calc R . . C53 C 0.8855(3) 0.4858(3) -0.01768(10) 0.0656(12) Uani 1 1 d . . . H53A H 0.9495 0.4872 -0.0197 0.079 Uiso 1 1 calc R . . C54 C 0.8350(4) 0.4335(3) -0.04270(10) 0.0744(14) Uani 1 1 d . . . C55 C 0.7400(4) 0.4352(2) -0.03964(9) 0.0711(13) Uani 1 1 d . . . H55A H 0.7046 0.4027 -0.0569 0.085 Uiso 1 1 calc R . . C56 C 0.6963(3) 0.4842(2) -0.01145(8) 0.0527(9) Uani 1 1 d . . . H56A H 0.6323 0.4828 -0.0096 0.063 Uiso 1 1 calc R . . C57 C 0.8834(5) 0.3778(3) -0.07275(10) 0.122(2) Uani 1 1 d . . . H57A H 0.9345 0.4125 -0.0824 0.184 Uiso 1 1 calc R . . H57B H 0.8408 0.3646 -0.0926 0.184 Uiso 1 1 calc R . . H57C H 0.9055 0.3210 -0.0622 0.184 Uiso 1 1 calc R . . C101 C 0.4431(3) 0.4013(2) 0.15239(12) 0.0652(11) Uani 1 1 d . . . C102 C 0.4663(4) 0.3668(3) 0.18713(13) 0.0912(17) Uani 1 1 d . . . H10A H 0.5041 0.4012 0.2029 0.109 Uiso 1 1 calc R . . C103 C 0.4341(4) 0.2815(3) 0.19890(16) 0.113(2) Uani 1 1 d . . . H10B H 0.4526 0.2584 0.2220 0.136 Uiso 1 1 calc R . . C104 C 0.3770(5) 0.2319(3) 0.1776(2) 0.116(2) Uani 1 1 d . . . C105 C 0.3531(4) 0.2644(4) 0.1420(3) 0.132(2) Uani 1 1 d . . . H10C H 0.3146 0.2295 0.1268 0.158 Uiso 1 1 calc R . . C106 C 0.3883(3) 0.3517(3) 0.12908(17) 0.1001(17) Uani 1 1 d . . . H10D H 0.3737 0.3736 0.1053 0.120 Uiso 1 1 calc R . . C107 C 0.3389(4) 0.1377(3) 0.1907(2) 0.176(3) Uani 1 1 d . . . H10E H 0.3861 0.1049 0.2041 0.264 Uiso 1 1 calc R . . H10F H 0.3200 0.1022 0.1694 0.264 Uiso 1 1 calc R . . H10G H 0.2868 0.1475 0.2069 0.264 Uiso 1 1 calc R . . C151 C 0.3745(3) 0.8580(2) 0.20240(12) 0.0640(11) Uani 1 1 d . . . C152 C 0.3896(4) 0.8529(3) 0.23969(13) 0.112(2) Uani 1 1 d . . . H15A H 0.4408 0.8215 0.2489 0.134 Uiso 1 1 calc R . . C153 C 0.3245(6) 0.8971(4) 0.26570(18) 0.131(3) Uani 1 1 d . . . H15B H 0.3336 0.8948 0.2915 0.158 Uiso 1 1 calc R . . C154 C 0.2494(5) 0.9422(4) 0.2505(2) 0.119(3) Uani 1 1 d . . . C155 C 0.2344(4) 0.9453(3) 0.2131(2) 0.114(2) Uani 1 1 d . . . H15C H 0.1826 0.9752 0.2037 0.137 Uiso 1 1 calc R . . C156 C 0.2962(3) 0.9041(3) 0.18894(14) 0.0843(14) Uani 1 1 d . . . H15D H 0.2857 0.9068 0.1633 0.101 Uiso 1 1 calc R . . C157 C 0.1790(5) 0.9852(4) 0.2777(2) 0.217(5) Uani 1 1 d . . . H15E H 0.1714 1.0495 0.2719 0.325 Uiso 1 1 calc R . . H15F H 0.2009 0.9788 0.3029 0.325 Uiso 1 1 calc R . . H15G H 0.1208 0.9542 0.2751 0.325 Uiso 1 1 calc R . . C201 C 0.7042(2) 0.99890(17) 0.07232(7) 0.0295(6) Uani 1 1 d . . . C202 C 0.6464(2) 1.0727(2) 0.06310(7) 0.0379(7) Uani 1 1 d . . . H20A H 0.5833 1.0684 0.0674 0.045 Uiso 1 1 calc R . . C203 C 0.6832(2) 1.1521(2) 0.04760(8) 0.0452(8) Uani 1 1 d . . . H20B H 0.6437 1.2006 0.0417 0.054 Uiso 1 1 calc R . . C204 C 0.7768(2) 1.1619(2) 0.04060(8) 0.0422(8) Uani 1 1 d . . . C205 C 0.8339(2) 1.0884(2) 0.04992(7) 0.0395(7) Uani 1 1 d . . . H20C H 0.8972 1.0932 0.0460 0.047 Uiso 1 1 calc R . . C206 C 0.7981(2) 1.00855(19) 0.06493(7) 0.0337(6) Uani 1 1 d . . . H20D H 0.8376 0.9597 0.0703 0.040 Uiso 1 1 calc R . . C207 C 0.8170(3) 1.2490(2) 0.02427(9) 0.0589(10) Uani 1 1 d . . . H20E H 0.7683 1.2860 0.0139 0.088 Uiso 1 1 calc R . . H20F H 0.8603 1.2334 0.0049 0.088 Uiso 1 1 calc R . . H20G H 0.8479 1.2832 0.0436 0.088 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0292(2) 0.02358(18) 0.03569(18) 0.00006(16) 0.00447(16) -0.00273(15) C21 0.0293(15) 0.0251(14) 0.0250(14) -0.0001(11) 0.0017(12) -0.0009(11) N22 0.0312(12) 0.0227(11) 0.0329(11) 0.0002(10) 0.0009(10) -0.0032(10) N24 0.0335(13) 0.0233(12) 0.0321(12) 0.0011(9) 0.0031(10) -0.0028(9) N23 0.0348(14) 0.0259(13) 0.0518(15) 0.0034(11) 0.0128(12) -0.0012(10) C1 0.0245(14) 0.0270(15) 0.0267(13) -0.0006(11) -0.0033(12) -0.0037(11) N2 0.0278(13) 0.0307(13) 0.0240(11) -0.0003(10) -0.0006(9) -0.0036(9) C3 0.0223(14) 0.0266(15) 0.0262(13) 0.0005(11) -0.0017(11) -0.0029(10) C4 0.0252(14) 0.0296(15) 0.0277(14) -0.0014(11) -0.0032(12) -0.0004(12) C5 0.0373(16) 0.0282(16) 0.0276(13) -0.0030(12) -0.0026(13) 0.0016(12) C6 0.0362(17) 0.0279(16) 0.0282(14) -0.0010(12) -0.0063(13) -0.0018(12) C7 0.0453(17) 0.0257(15) 0.0294(14) -0.0024(12) -0.0018(13) 0.0025(13) C8 0.0430(17) 0.0243(15) 0.0384(16) 0.0015(12) -0.0071(14) -0.0039(12) C9 0.0351(16) 0.0293(15) 0.0397(17) -0.0028(14) -0.0026(15) -0.0043(12) C10 0.0422(19) 0.0291(16) 0.063(2) -0.0005(16) 0.0153(17) -0.0086(13) C11 0.0369(17) 0.0312(17) 0.075(2) -0.0004(16) 0.0191(16) -0.0028(14) C12 0.057(2) 0.0326(19) 0.110(3) 0.003(2) 0.044(2) -0.0032(17) C13 0.055(2) 0.043(2) 0.096(3) 0.001(2) 0.040(2) -0.0006(17) C14 0.047(2) 0.0294(17) 0.0560(18) 0.0017(14) 0.0138(16) -0.0032(14) C15 0.050(2) 0.0376(18) 0.0518(18) -0.0015(15) 0.0211(16) 0.0010(16) C16 0.0404(18) 0.0318(16) 0.0411(17) 0.0004(14) 0.0142(15) 0.0029(14) C17 0.050(2) 0.0316(17) 0.0464(18) -0.0065(14) 0.0152(16) -0.0012(14) C18 0.0514(19) 0.0244(14) 0.0376(15) -0.0027(13) 0.0086(15) -0.0065(13) C19 0.0339(15) 0.0288(15) 0.0272(14) -0.0015(12) 0.0000(12) -0.0023(12) C20 0.0291(14) 0.0242(15) 0.0283(14) -0.0004(11) -0.0007(11) -0.0011(11) C31 0.0330(15) 0.0308(15) 0.0297(14) -0.0035(13) -0.0008(13) -0.0009(12) C51 0.066(2) 0.0255(16) 0.0271(15) 0.0040(13) 0.0048(15) 0.0038(14) C52 0.075(3) 0.0334(18) 0.0408(18) 0.0068(14) 0.0210(18) 0.0114(17) C53 0.099(3) 0.042(2) 0.055(2) 0.0156(19) 0.046(2) 0.021(2) C54 0.152(5) 0.037(2) 0.034(2) 0.0071(17) 0.029(2) 0.037(3) C55 0.152(4) 0.0318(19) 0.0298(18) -0.0046(16) -0.009(2) 0.014(2) C56 0.092(3) 0.0307(17) 0.0350(17) -0.0027(14) -0.0073(19) 0.0054(18) C57 0.257(7) 0.061(3) 0.049(2) 0.001(2) 0.052(3) 0.071(4) C101 0.062(2) 0.0297(18) 0.104(3) -0.006(2) 0.047(2) -0.0081(17) C102 0.136(4) 0.046(2) 0.091(3) 0.007(2) 0.071(3) -0.018(2) C103 0.164(6) 0.049(3) 0.127(4) 0.003(3) 0.103(4) -0.017(3) C104 0.116(5) 0.038(3) 0.193(6) 0.003(4) 0.099(5) -0.006(3) C105 0.090(4) 0.058(3) 0.248(8) -0.025(4) 0.046(5) -0.033(3) C106 0.063(3) 0.052(3) 0.185(5) -0.003(3) 0.018(3) -0.030(2) C107 0.165(6) 0.040(3) 0.323(9) 0.016(4) 0.163(6) -0.021(3) C151 0.082(3) 0.0279(19) 0.082(3) -0.0042(18) 0.055(2) -0.0101(18) C152 0.190(6) 0.056(3) 0.090(3) -0.013(2) 0.086(4) -0.008(3) C153 0.210(8) 0.055(3) 0.129(5) -0.003(3) 0.105(5) -0.029(4) C154 0.189(7) 0.048(3) 0.120(5) -0.020(3) 0.109(5) -0.038(4) C155 0.092(4) 0.048(3) 0.203(6) -0.015(3) 0.083(4) -0.011(2) C156 0.072(3) 0.043(2) 0.139(4) -0.012(2) 0.061(3) 0.000(2) C157 0.235(8) 0.085(4) 0.330(10) -0.066(5) 0.244(8) -0.046(5) C201 0.0392(16) 0.0248(14) 0.0246(13) -0.0024(11) 0.0035(12) -0.0038(13) C202 0.0461(18) 0.0298(16) 0.0378(15) -0.0035(14) 0.0042(14) -0.0012(14) C203 0.069(3) 0.0291(17) 0.0370(16) 0.0006(13) 0.0030(16) 0.0070(16) C204 0.071(3) 0.0293(16) 0.0260(15) 0.0008(13) 0.0083(15) -0.0066(15) C205 0.0483(19) 0.0339(18) 0.0363(16) -0.0065(13) 0.0072(14) -0.0152(14) C206 0.0417(17) 0.0285(15) 0.0309(15) -0.0028(12) -0.0007(14) -0.0032(13) C207 0.086(3) 0.040(2) 0.051(2) 0.0033(16) 0.021(2) -0.0125(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 N22 1.955(2) . ? Ni1 N24 1.955(2) . ? Ni1 N23 1.965(2) . ? Ni1 C21 2.003(3) . ? C21 C1 1.471(4) . ? C21 C4 1.479(3) . ? C21 C31 1.560(3) . ? N22 C9 1.380(3) . ? N22 C6 1.389(3) . ? N24 C16 1.381(3) . ? N24 C19 1.396(3) . ? N23 C14 1.364(3) . ? N23 C11 1.370(4) . ? C1 N2 1.365(3) . ? C1 C20 1.379(3) . ? N2 C3 1.337(3) . ? C3 C4 1.409(3) . ? C3 C3 1.475(5) 7 ? C4 C5 1.386(3) . ? C5 C6 1.391(4) . ? C5 C51 1.499(4) . ? C6 C7 1.426(4) . ? C7 C8 1.341(4) . ? C7 H7A 0.9300 . ? C8 C9 1.443(4) . ? C8 H8A 0.9300 . ? C9 C10 1.379(4) . ? C10 C11 1.373(4) . ? C10 C101 1.514(4) . ? C11 C12 1.444(4) . ? C12 C13 1.347(5) . ? C12 H12A 0.9300 . ? C13 C14 1.436(4) . ? C13 H13A 0.9300 . ? C14 C15 1.392(4) . ? C15 C16 1.371(4) . ? C15 C151 1.492(4) . ? C16 C17 1.434(4) . ? C17 C18 1.325(4) . ? C17 H17A 0.9300 . ? C18 C19 1.438(4) . ? C18 H18A 0.9300 . ? C19 C20 1.398(3) . ? C20 C201 1.478(3) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C51 C56 1.380(4) . ? C51 C52 1.388(5) . ? C52 C53 1.392(4) . ? C52 H52A 0.9300 . ? C53 C54 1.381(6) . ? C53 H53A 0.9300 . ? C54 C55 1.380(6) . ? C54 C57 1.515(5) . ? C55 C56 1.385(5) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C101 C106 1.356(6) . ? C101 C102 1.379(6) . ? C102 C103 1.386(5) . ? C102 H10A 0.9300 . ? C103 C104 1.333(8) . ? C103 H10B 0.9300 . ? C104 C105 1.397(9) . ? C104 C107 1.545(6) . ? C105 C106 1.440(7) . ? C105 H10C 0.9300 . ? C106 H10D 0.9300 . ? C107 H10E 0.9600 . ? C107 H10F 0.9600 . ? C107 H10G 0.9600 . ? C151 C152 1.351(6) . ? C151 C156 1.401(6) . ? C152 C153 1.471(7) . ? C152 H15A 0.9300 . ? C153 C154 1.378(9) . ? C153 H15B 0.9300 . ? C154 C155 1.356(8) . ? C154 C157 1.539(7) . ? C155 C156 1.378(6) . ? C155 H15C 0.9300 . ? C156 H15D 0.9300 . ? C157 H15E 0.9600 . ? C157 H15F 0.9600 . ? C157 H15G 0.9600 . ? C201 C206 1.392(4) . ? C201 C202 1.397(4) . ? C202 C203 1.383(4) . ? C202 H20A 0.9300 . ? C203 C204 1.385(4) . ? C203 H20B 0.9300 . ? C204 C205 1.389(4) . ? C204 C207 1.508(4) . ? C205 C206 1.376(4) . ? C205 H20C 0.9300 . ? C206 H20D 0.9300 . ? C207 H20E 0.9600 . ? C207 H20F 0.9600 . ? C207 H20G 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 N22 Ni1 N24 176.94(9) . . ? N22 Ni1 N23 90.51(9) . . ? N24 Ni1 N23 91.66(9) . . ? N22 Ni1 C21 88.81(9) . . ? N24 Ni1 C21 88.80(10) . . ? N23 Ni1 C21 173.73(10) . . ? C1 C21 C4 100.51(19) . . ? C1 C21 C31 110.3(2) . . ? C4 C21 C31 110.9(2) . . ? C1 C21 Ni1 120.74(18) . . ? C4 C21 Ni1 119.55(18) . . ? C31 C21 Ni1 94.89(15) . . ? C9 N22 C6 104.2(2) . . ? C9 N22 Ni1 125.74(18) . . ? C6 N22 Ni1 129.03(17) . . ? C16 N24 C19 104.7(2) . . ? C16 N24 Ni1 125.50(18) . . ? C19 N24 Ni1 129.50(18) . . ? C14 N23 C11 105.4(2) . . ? C14 N23 Ni1 126.92(19) . . ? C11 N23 Ni1 127.50(19) . . ? N2 C1 C20 120.2(2) . . ? N2 C1 C21 113.2(2) . . ? C20 C1 C21 126.5(2) . . ? C3 N2 C1 106.1(2) . . ? N2 C3 C4 113.0(2) . . ? N2 C3 C3 119.8(2) . 7 ? C4 C3 C3 126.9(2) . 7 ? C5 C4 C3 128.4(2) . . ? C5 C4 C21 124.7(2) . . ? C3 C4 C21 106.9(2) . . ? C4 C5 C6 119.6(2) . . ? C4 C5 C51 122.0(2) . . ? C6 C5 C51 118.4(2) . . ? N22 C6 C5 125.0(2) . . ? N22 C6 C7 111.0(2) . . ? C5 C6 C7 123.7(3) . . ? C8 C7 C6 107.2(3) . . ? C8 C7 H7A 126.4 . . ? C6 C7 H7A 126.4 . . ? C7 C8 C9 107.1(2) . . ? C7 C8 H8A 126.5 . . ? C9 C8 H8A 126.5 . . ? C10 C9 N22 126.2(3) . . ? C10 C9 C8 123.3(3) . . ? N22 C9 C8 110.5(2) . . ? C11 C10 C9 123.1(3) . . ? C11 C10 C101 118.8(3) . . ? C9 C10 C101 118.1(3) . . ? N23 C11 C10 124.9(3) . . ? N23 C11 C12 110.1(3) . . ? C10 C11 C12 124.8(3) . . ? C13 C12 C11 106.9(3) . . ? C13 C12 H12A 126.5 . . ? C11 C12 H12A 126.5 . . ? C12 C13 C14 106.5(3) . . ? C12 C13 H13A 126.8 . . ? C14 C13 H13A 126.8 . . ? N23 C14 C15 124.5(3) . . ? N23 C14 C13 111.0(3) . . ? C15 C14 C13 124.3(3) . . ? C16 C15 C14 124.2(3) . . ? C16 C15 C151 119.0(3) . . ? C14 C15 C151 116.7(3) . . ? C15 C16 N24 126.2(3) . . ? C15 C16 C17 123.8(3) . . ? N24 C16 C17 110.0(2) . . ? C18 C17 C16 108.1(3) . . ? C18 C17 H17A 125.9 . . ? C16 C17 H17A 125.9 . . ? C17 C18 C19 107.3(2) . . ? C17 C18 H18A 126.3 . . ? C19 C18 H18A 126.3 . . ? N24 C19 C20 125.9(2) . . ? N24 C19 C18 109.8(2) . . ? C20 C19 C18 123.9(2) . . ? C1 C20 C19 118.8(2) . . ? C1 C20 C201 119.1(2) . . ? C19 C20 C201 122.1(2) . . ? C21 C31 H31A 109.5 . . ? C21 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C21 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C56 C51 C52 118.5(3) . . ? C56 C51 C5 121.1(3) . . ? C52 C51 C5 120.4(3) . . ? C51 C52 C53 120.3(4) . . ? C51 C52 H52A 119.8 . . ? C53 C52 H52A 119.8 . . ? C54 C53 C52 121.2(4) . . ? C54 C53 H53A 119.4 . . ? C52 C53 H53A 119.4 . . ? C55 C54 C53 117.9(3) . . ? C55 C54 C57 121.8(5) . . ? C53 C54 C57 120.3(5) . . ? C54 C55 C56 121.5(4) . . ? C54 C55 H55A 119.3 . . ? C56 C55 H55A 119.3 . . ? C51 C56 C55 120.6(4) . . ? C51 C56 H56A 119.7 . . ? C55 C56 H56A 119.7 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C106 C101 C102 120.2(4) . . ? C106 C101 C10 118.8(4) . . ? C102 C101 C10 121.0(4) . . ? C101 C102 C103 120.9(5) . . ? C101 C102 H10A 119.5 . . ? C103 C102 H10A 119.5 . . ? C104 C103 C102 121.0(6) . . ? C104 C103 H10B 119.5 . . ? C102 C103 H10B 119.5 . . ? C103 C104 C105 119.4(5) . . ? C103 C104 C107 121.6(7) . . ? C105 C104 C107 119.0(7) . . ? C104 C105 C106 120.0(6) . . ? C104 C105 H10C 120.0 . . ? C106 C105 H10C 120.0 . . ? C101 C106 C105 118.3(6) . . ? C101 C106 H10D 120.8 . . ? C105 C106 H10D 120.8 . . ? C104 C107 H10E 109.5 . . ? C104 C107 H10F 109.5 . . ? H10E C107 H10F 109.5 . . ? C104 C107 H10G 109.5 . . ? H10E C107 H10G 109.5 . . ? H10F C107 H10G 109.5 . . ? C152 C151 C156 119.7(4) . . ? C152 C151 C15 120.5(4) . . ? C156 C151 C15 119.6(4) . . ? C151 C152 C153 119.6(6) . . ? C151 C152 H15A 120.2 . . ? C153 C152 H15A 120.2 . . ? C154 C153 C152 117.6(6) . . ? C154 C153 H15B 121.2 . . ? C152 C153 H15B 121.2 . . ? C155 C154 C153 122.0(6) . . ? C155 C154 C157 120.1(8) . . ? C153 C154 C157 117.8(7) . . ? C154 C155 C156 119.9(6) . . ? C154 C155 H15C 120.1 . . ? C156 C155 H15C 120.1 . . ? C155 C156 C151 121.1(5) . . ? C155 C156 H15D 119.4 . . ? C151 C156 H15D 119.4 . . ? C154 C157 H15E 109.5 . . ? C154 C157 H15F 109.5 . . ? H15E C157 H15F 109.5 . . ? C154 C157 H15G 109.5 . . ? H15E C157 H15G 109.5 . . ? H15F C157 H15G 109.5 . . ? C206 C201 C202 117.6(3) . . ? C206 C201 C20 119.3(2) . . ? C202 C201 C20 122.9(3) . . ? C203 C202 C201 120.0(3) . . ? C203 C202 H20A 120.0 . . ? C201 C202 H20A 120.0 . . ? C202 C203 C204 122.3(3) . . ? C202 C203 H20B 118.9 . . ? C204 C203 H20B 118.9 . . ? C203 C204 C205 117.5(3) . . ? C203 C204 C207 122.3(3) . . ? C205 C204 C207 120.3(3) . . ? C206 C205 C204 120.8(3) . . ? C206 C205 H20C 119.6 . . ? C204 C205 H20C 119.6 . . ? C205 C206 C201 121.8(3) . . ? C205 C206 H20D 119.1 . . ? C201 C206 H20D 119.1 . . ? C204 C207 H20E 109.5 . . ? C204 C207 H20F 109.5 . . ? H20E C207 H20F 109.5 . . ? C204 C207 H20G 109.5 . . ? H20E C207 H20G 109.5 . . ? H20F C207 H20G 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.785 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.047 # Attachment '7325_web_deposit_cif_file_2_PiotrJ.Chmielewski_1316792793.5.cif' data_chni1s _database_code_depnum_ccdc_archive 'CCDC 825668' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H77 I N8 Ni2' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour brown _diffrn_ambient_temperature 100(2) _chemical_formula_weight 1623.01 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_int_tables_number 15 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.8601(7) _cell_length_b 24.5782(10) _cell_length_c 17.3598(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.971(4) _cell_angle_gamma 90.00 _cell_volume 8920.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3471 _cell_measurement_theta_min 4.7113 _cell_measurement_theta_max 38.4759 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 0.817 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; SPACE GROUP DETERMINATION #------------------------------------------------------------------------------ Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 28124 28124 0 28168 28124 37493 37477 56240 N (int>3sigma) = 0 2838 2838 0 2810 2838 3765 3768 5663 Mean intensity = 0.0 9.8 9.8 0.0 9.2 9.8 9.8 9.6 9.6 Mean int/sigma = 0.0 1.8 1.8 0.0 1.7 1.8 1.8 1.8 1.8 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.647 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 543 N I>3s 0 2.3 0.3 Identical indices and Friedel opposites combined before calculating R(sym) Option Space Group No. Type Axes CSD R(sym) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.286 13406 0.3 / 1.8 17.11 [B] Cc # 9 non-cen 1 566 0.286 13406 0.3 / 1.8 7.75 Option [A] chosen The structure can be solved either in centrosymmetric or non-centrosymmetric space group but due to molecule's disorder only within C2/c can be satisfactorily refined. #------------------------------------------------------------------------------ ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur with Onyx CCD' _diffrn_measurement_method '\w and \p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29582 _diffrn_reflns_av_R_equivalents 0.1276 _diffrn_reflns_av_sigmaI/netI 0.2914 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.72 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9688 _reflns_number_gt 3066 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9688 _refine_ls_number_parameters 504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2017 _refine_ls_R_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.2541 _refine_ls_wR_factor_gt 0.2359 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 -0.019 591 202 ' ' 2 0.500 1.000 0.072 591 202 ' ' 3 0.500 0.641 0.250 102 34 ' ' 4 1.000 0.141 0.250 102 34 ' ' 5 0.500 0.359 0.750 102 33 ' ' 6 1.000 0.859 0.750 102 33 ' ' _platon_squeeze_details ; ; 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 0.30336(4) 0.28236(4) 1.14185(7) 0.0316(3) Uani 1 1 d . . . C21 C 0.3727(3) 0.3345(3) 1.1290(5) 0.032(2) Uani 1 1 d . . . N22 N 0.3617(3) 0.2215(3) 1.1400(4) 0.0319(16) Uani 1 1 d . . . N23 N 0.2362(3) 0.2316(3) 1.1455(4) 0.0332(18) Uani 1 1 d . . . N24 N 0.2463(3) 0.3437(3) 1.1335(4) 0.0342(17) Uani 1 1 d . . . C1 C 0.3707(3) 0.3875(3) 1.1617(5) 0.032(2) Uani 1 1 d . . . N2 N 0.4269(3) 0.4009(3) 1.2158(4) 0.0389(18) Uani 1 1 d . . . C3 C 0.4674(3) 0.3577(3) 1.2207(5) 0.035(2) Uani 1 1 d . . . C4 C 0.4381(3) 0.3177(3) 1.1662(5) 0.0275(19) Uani 1 1 d . . . C5 C 0.4637(3) 0.2691(3) 1.1473(5) 0.030(2) Uani 1 1 d . . . C6 C 0.4230(3) 0.2241(4) 1.1263(5) 0.034(2) Uani 1 1 d . . . C7 C 0.4390(3) 0.1713(3) 1.1023(5) 0.032(2) Uani 1 1 d . . . H7A H 0.4747 0.1622 1.0863 0.038 Uiso 1 1 calc R . . C8 C 0.3914(4) 0.1372(4) 1.1077(5) 0.040(2) Uani 1 1 d . . . H8A H 0.3892 0.1001 1.0969 0.048 Uiso 1 1 calc R . . C9 C 0.3456(3) 0.1684(4) 1.1327(5) 0.035(2) Uani 1 1 d . . . C10 C 0.2918(4) 0.1452(4) 1.1486(5) 0.043(2) Uani 1 1 d . . . C11 C 0.2417(3) 0.1767(4) 1.1593(5) 0.035(2) Uani 1 1 d . . . C12 C 0.1864(4) 0.1562(4) 1.1783(5) 0.043(2) Uani 1 1 d . . . H12A H 0.1798 0.1206 1.1921 0.052 Uiso 1 1 calc R . . C13 C 0.1463(4) 0.1976(4) 1.1728(5) 0.044(2) Uani 1 1 d . . . H13A H 0.1067 0.1965 1.1825 0.053 Uiso 1 1 calc R . . C14 C 0.1761(4) 0.2448(4) 1.1486(5) 0.041(2) Uani 1 1 d . . . C15 C 0.1472(3) 0.2960(3) 1.1272(5) 0.034(2) Uani 1 1 d . . . C16 C 0.1798(3) 0.3403(4) 1.1143(5) 0.037(2) Uani 1 1 d . . . C17 C 0.1509(3) 0.3913(4) 1.0852(5) 0.040(2) Uani 1 1 d . . . H17A H 0.1072 0.3985 1.0691 0.047 Uiso 1 1 calc R . . C18 C 0.1975(3) 0.4275(4) 1.0849(5) 0.041(2) Uani 1 1 d . . . H18A H 0.1921 0.4633 1.0669 0.049 Uiso 1 1 calc R . . C19 C 0.2582(3) 0.3988(4) 1.1187(5) 0.037(2) Uani 1 1 d . . . C20 C 0.3172(3) 0.4229(3) 1.1406(5) 0.034(2) Uani 1 1 d . . . C51 C 0.5318(3) 0.2662(3) 1.1484(5) 0.033(2) Uani 1 1 d . . . C52 C 0.5585(3) 0.3119(3) 1.1224(5) 0.035(2) Uani 1 1 d . . . H52A H 0.5334 0.3426 1.1048 0.042 Uiso 1 1 calc R . . C53 C 0.6215(4) 0.3120(3) 1.1224(5) 0.041(2) Uani 1 1 d . . . H53A H 0.6387 0.3432 1.1066 0.049 Uiso 1 1 calc R . . C54 C 0.6599(3) 0.2658(3) 1.1458(5) 0.037(2) Uani 1 1 d . . . C55 C 0.6337(3) 0.2203(4) 1.1701(5) 0.036(2) Uani 1 1 d . . . H55A H 0.6587 0.1893 1.1850 0.044 Uiso 1 1 calc R . . C56 C 0.5700(3) 0.2198(3) 1.1730(4) 0.0322(19) Uani 1 1 d . . . H56A H 0.5535 0.1891 1.1911 0.039 Uiso 1 1 calc R . . C57 C 0.7285(3) 0.2656(3) 1.1439(6) 0.047(3) Uani 1 1 d . . . H57A H 0.7441 0.2289 1.1481 0.070 Uiso 1 1 calc R . . H57B H 0.7543 0.2866 1.1883 0.070 Uiso 1 1 calc R . . H57C H 0.7309 0.2813 1.0942 0.070 Uiso 1 1 calc R . . C101 C 0.2889(4) 0.0848(4) 1.1561(5) 0.043(2) Uani 1 1 d . . . C102 C 0.2396(5) 0.0550(4) 1.1057(6) 0.074(4) Uani 1 1 d . . . H10A H 0.2071 0.0728 1.0672 0.089 Uiso 1 1 calc R . . C103 C 0.2380(5) -0.0005(5) 1.1119(7) 0.090(4) Uani 1 1 d . . . H10B H 0.2062 -0.0199 1.0746 0.108 Uiso 1 1 calc R . . C104 C 0.2821(4) -0.0286(4) 1.1718(5) 0.043(2) Uani 1 1 d . . . C105 C 0.3293(4) 0.0013(4) 1.2238(6) 0.044(2) Uani 1 1 d . . . H10C H 0.3593 -0.0166 1.2653 0.053 Uiso 1 1 calc R . . C106 C 0.3341(3) 0.0571(4) 1.2169(5) 0.039(2) Uani 1 1 d . . . H10D H 0.3672 0.0760 1.2527 0.047 Uiso 1 1 calc R . . C107 C 0.2757(4) -0.0894(4) 1.1809(6) 0.049(2) Uani 1 1 d . . . H10E H 0.3150 -0.1037 1.2155 0.073 Uiso 1 1 calc R . . H10F H 0.2663 -0.1065 1.1290 0.073 Uiso 1 1 calc R . . H10G H 0.2416 -0.0967 1.2040 0.073 Uiso 1 1 calc R . . C151 C 0.0759(3) 0.3003(4) 1.1189(5) 0.046(3) Uani 1 1 d . . . C152 C 0.0335(3) 0.2649(3) 1.0640(5) 0.037(2) Uani 1 1 d . . . H15A H 0.0490 0.2395 1.0347 0.045 Uiso 1 1 calc R . . C153 C -0.0312(3) 0.2686(4) 1.0547(5) 0.043(2) Uani 1 1 d . . . H15B H -0.0588 0.2444 1.0202 0.052 Uiso 1 1 calc R . . C154 C -0.0562(4) 0.3066(5) 1.0944(6) 0.062(3) Uani 1 1 d . . . C155 C -0.0137(4) 0.3400(5) 1.1465(7) 0.085(4) Uani 1 1 d . . . H15C H -0.0295 0.3654 1.1756 0.103 Uiso 1 1 calc R . . C156 C 0.0520(4) 0.3380(5) 1.1581(7) 0.071(3) Uani 1 1 d . . . H15D H 0.0791 0.3625 1.1926 0.085 Uiso 1 1 calc R . . C157 C -0.1275(4) 0.3088(4) 1.0851(7) 0.075(4) Uani 1 1 d . . . H15E H -0.1428 0.3453 1.0720 0.113 Uiso 1 1 calc R . . H15F H -0.1350 0.2979 1.1346 0.113 Uiso 1 1 calc R . . H15G H -0.1497 0.2846 1.0427 0.113 Uiso 1 1 calc R . . C201 C 0.3249(3) 0.4826(3) 1.1338(5) 0.0278(19) Uani 1 1 d . . . C202 C 0.2882(3) 0.5200(3) 1.1601(5) 0.034(2) Uani 1 1 d . . . H20A H 0.2599 0.5083 1.1877 0.040 Uiso 1 1 calc R . . C203 C 0.2936(3) 0.5742(4) 1.1455(5) 0.039(2) Uani 1 1 d . . . H20B H 0.2674 0.5986 1.1619 0.047 Uiso 1 1 calc R . . C204 C 0.3367(4) 0.5944(4) 1.1073(5) 0.044(2) Uani 1 1 d . . . C205 C 0.3744(4) 0.5573(3) 1.0814(5) 0.036(2) Uani 1 1 d . . . H20C H 0.4028 0.5695 1.0543 0.044 Uiso 1 1 calc R . . C206 C 0.3699(3) 0.5026(3) 1.0954(5) 0.036(2) Uani 1 1 d . . . H20D H 0.3965 0.4783 1.0797 0.044 Uiso 1 1 calc R . . C207 C 0.3403(5) 0.6543(3) 1.0912(6) 0.063(3) Uani 1 1 d . . . H20E H 0.3744 0.6609 1.0679 0.094 Uiso 1 1 calc R . . H20F H 0.3482 0.6741 1.1408 0.094 Uiso 1 1 calc R . . H20G H 0.3006 0.6661 1.0545 0.094 Uiso 1 1 calc R . . C25 C 0.4384(7) 0.4505(6) 1.2852(10) 0.040(4) Uiso 0.50 1 d P . . H25A H 0.4040 0.4763 1.2695 0.060 Uiso 0.50 1 calc PR . . H25B H 0.4782 0.4686 1.2895 0.060 Uiso 0.50 1 calc PR . . H25C H 0.4396 0.4350 1.3364 0.060 Uiso 0.50 1 calc PR . . C26 C 0.3498(4) 0.3309(3) 1.0361(5) 0.041(2) Uani 1 1 d . . . H26A H 0.3765 0.3533 1.0140 0.062 Uiso 1 1 calc R . . H26B H 0.3063 0.3432 1.0167 0.062 Uiso 1 1 calc R . . H26C H 0.3523 0.2938 1.0198 0.062 Uiso 1 1 calc R . . I1 I 0.46554(9) 0.42792(10) 0.96290(15) 0.1369(9) Uani 0.50 1 d P A -1 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 0.0140(5) 0.0396(7) 0.0375(6) 0.0068(6) 0.0016(4) -0.0003(5) C21 0.015(4) 0.038(6) 0.041(6) 0.015(4) 0.004(4) 0.008(4) N22 0.021(3) 0.035(4) 0.036(4) 0.007(4) 0.003(3) 0.002(3) N23 0.013(3) 0.050(5) 0.038(4) 0.014(4) 0.009(3) -0.002(3) N24 0.019(3) 0.042(5) 0.041(4) -0.002(4) 0.008(3) 0.001(3) C1 0.018(4) 0.033(5) 0.042(6) 0.009(4) 0.006(4) 0.003(4) N2 0.019(3) 0.034(4) 0.058(5) 0.006(4) 0.002(4) -0.002(3) C3 0.019(4) 0.026(5) 0.059(6) -0.002(5) 0.012(4) -0.004(4) C4 0.018(4) 0.026(5) 0.039(5) 0.007(4) 0.008(4) 0.000(3) C5 0.018(4) 0.029(5) 0.038(5) 0.013(4) 0.000(4) -0.004(3) C6 0.022(4) 0.047(6) 0.026(5) 0.006(4) -0.004(4) 0.006(4) C7 0.020(4) 0.027(5) 0.042(5) -0.003(4) -0.002(4) -0.001(4) C8 0.039(5) 0.038(6) 0.032(5) 0.002(4) -0.006(4) 0.000(4) C9 0.022(4) 0.036(6) 0.042(6) -0.001(4) 0.001(4) -0.004(4) C10 0.034(5) 0.045(6) 0.038(6) 0.016(5) -0.011(4) -0.013(4) C11 0.013(4) 0.050(6) 0.033(5) 0.006(5) -0.009(4) -0.004(4) C12 0.028(4) 0.058(6) 0.040(6) 0.018(5) 0.004(4) -0.008(5) C13 0.020(4) 0.065(7) 0.044(6) 0.020(5) 0.003(4) -0.010(4) C14 0.022(4) 0.066(7) 0.034(5) 0.004(5) 0.005(4) -0.002(4) C15 0.020(4) 0.053(6) 0.026(5) -0.003(4) 0.003(4) -0.002(4) C16 0.018(4) 0.048(6) 0.040(6) -0.002(5) 0.001(4) -0.009(4) C17 0.014(4) 0.050(6) 0.044(6) -0.009(5) -0.007(4) 0.008(4) C18 0.016(4) 0.062(6) 0.037(5) -0.005(5) -0.004(4) 0.004(4) C19 0.019(4) 0.048(6) 0.037(5) 0.000(5) -0.002(4) 0.007(4) C20 0.016(4) 0.046(6) 0.035(5) 0.013(4) -0.002(4) 0.004(4) C51 0.022(4) 0.040(6) 0.034(5) 0.004(4) 0.004(4) 0.000(4) C52 0.020(4) 0.043(6) 0.042(6) 0.003(4) 0.007(4) 0.009(4) C53 0.031(5) 0.030(5) 0.057(6) -0.004(5) 0.006(5) -0.001(4) C54 0.014(4) 0.045(6) 0.043(6) -0.007(4) -0.004(4) 0.001(4) C55 0.022(4) 0.044(5) 0.035(5) 0.005(5) -0.005(4) 0.009(4) C56 0.029(4) 0.036(5) 0.025(4) -0.003(4) -0.001(4) 0.002(4) C57 0.020(4) 0.051(6) 0.069(7) 0.005(5) 0.013(5) 0.000(4) C101 0.036(5) 0.044(6) 0.042(6) 0.006(5) 0.000(5) -0.010(4) C102 0.071(7) 0.052(7) 0.059(7) 0.024(6) -0.043(6) -0.021(6) C103 0.101(9) 0.068(9) 0.057(7) 0.014(6) -0.048(7) -0.040(7) C104 0.039(5) 0.045(6) 0.040(6) 0.013(5) 0.004(5) 0.007(4) C105 0.035(5) 0.039(6) 0.049(6) 0.015(5) 0.000(5) -0.002(4) C106 0.020(4) 0.051(6) 0.039(5) 0.016(5) -0.002(4) 0.003(4) C107 0.045(5) 0.052(6) 0.052(6) 0.009(5) 0.019(5) 0.002(5) C151 0.015(4) 0.083(8) 0.038(6) 0.000(5) 0.006(4) 0.002(4) C152 0.022(4) 0.050(6) 0.040(5) -0.002(4) 0.008(4) -0.001(4) C153 0.017(4) 0.059(7) 0.047(6) 0.004(5) -0.002(4) -0.010(4) C154 0.024(5) 0.108(9) 0.053(7) -0.024(6) 0.010(5) -0.003(5) C155 0.039(6) 0.137(11) 0.079(9) -0.063(8) 0.015(6) 0.000(6) C156 0.016(4) 0.112(10) 0.082(8) -0.045(7) 0.012(5) -0.008(5) C157 0.019(4) 0.089(8) 0.118(10) -0.030(7) 0.022(6) -0.007(5) C201 0.019(4) 0.029(5) 0.030(5) 0.002(4) -0.002(4) 0.005(3) C202 0.032(4) 0.034(5) 0.034(5) -0.008(4) 0.008(4) -0.001(4) C203 0.023(4) 0.052(6) 0.040(5) -0.014(5) 0.006(4) 0.012(4) C204 0.045(5) 0.039(6) 0.036(5) 0.011(5) -0.005(5) 0.005(4) C205 0.036(5) 0.036(6) 0.043(6) 0.002(4) 0.019(4) 0.005(4) C206 0.022(4) 0.033(5) 0.049(6) -0.006(4) 0.003(4) 0.006(4) C207 0.083(7) 0.023(5) 0.079(8) -0.003(5) 0.020(7) 0.004(5) C26 0.031(4) 0.046(6) 0.044(6) 0.006(5) 0.007(4) 0.008(4) I1 0.0773(12) 0.188(2) 0.161(2) 0.0263(18) 0.0603(14) 0.0077(13) _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 N24 1.935(6) . ? Ni1 N23 1.943(6) . ? Ni1 N22 1.972(6) . ? Ni1 C21 2.047(7) . ? C21 C1 1.426(11) . ? C21 C4 1.447(9) . ? C21 C26 1.547(11) . ? N22 C9 1.349(10) . ? N22 C6 1.429(9) . ? N23 C14 1.368(9) . ? N23 C11 1.369(10) . ? N24 C16 1.396(9) . ? N24 C19 1.416(10) . ? C1 N2 1.352(9) . ? C1 C20 1.417(10) . ? N2 C3 1.370(9) . ? N2 C25 1.681(16) . ? C3 C4 1.385(10) . ? C3 C3 1.488(14) 2_657 ? C4 C5 1.398(10) . ? C5 C6 1.400(10) . ? C5 C51 1.485(10) . ? C6 C7 1.437(10) . ? C7 C8 1.358(10) . ? C7 H7A 0.9300 . ? C8 C9 1.427(11) . ? C8 H8A 0.9300 . ? C9 C10 1.405(11) . ? C10 C11 1.397(11) . ? C10 C101 1.493(11) . ? C11 C12 1.434(10) . ? C12 C13 1.326(11) . ? C12 H12A 0.9300 . ? C13 C14 1.452(11) . ? C13 H13A 0.9300 . ? C14 C15 1.409(11) . ? C15 C16 1.355(10) . ? C15 C151 1.526(10) . ? C16 C17 1.428(11) . ? C17 C18 1.354(11) . ? C17 H17A 0.9300 . ? C18 C19 1.466(10) . ? C18 H18A 0.9300 . ? C19 C20 1.368(10) . ? C20 C201 1.488(11) . ? C51 C52 1.399(10) . ? C51 C56 1.404(10) . ? C52 C53 1.376(10) . ? C52 H52A 0.9300 . ? C53 C54 1.399(10) . ? C53 H53A 0.9300 . ? C54 C55 1.378(11) . ? C54 C57 1.511(9) . ? C55 C56 1.408(10) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C101 C102 1.383(11) . ? C101 C106 1.395(10) . ? C102 C103 1.371(13) . ? C102 H10A 0.9300 . ? C103 C104 1.379(12) . ? C103 H10B 0.9300 . ? C104 C105 1.369(11) . ? C104 C107 1.515(11) . ? C105 C106 1.383(11) . ? C105 H10C 0.9300 . ? C106 H10D 0.9300 . ? C107 H10E 0.9600 . ? C107 H10F 0.9600 . ? C107 H10G 0.9600 . ? C151 C156 1.342(12) . ? C151 C152 1.418(11) . ? C152 C153 1.379(10) . ? C152 H15A 0.9300 . ? C153 C154 1.365(12) . ? C153 H15B 0.9300 . ? C154 C155 1.365(12) . ? C154 C157 1.521(11) . ? C155 C156 1.393(11) . ? C155 H15C 0.9300 . ? C156 H15D 0.9300 . ? C157 H15E 0.9600 . ? C157 H15F 0.9600 . ? C157 H15G 0.9600 . ? C201 C202 1.383(10) . ? C201 C206 1.424(10) . ? C202 C203 1.369(11) . ? C202 H20A 0.9300 . ? C203 C204 1.393(11) . ? C203 H20B 0.9300 . ? C204 C205 1.390(11) . ? C204 C207 1.505(11) . ? C205 C206 1.375(10) . ? C205 H20C 0.9300 . ? C206 H20D 0.9300 . ? C207 H20E 0.9600 . ? C207 H20F 0.9600 . ? C207 H20G 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 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 N24 Ni1 N23 91.5(3) . . ? N24 Ni1 N22 174.6(3) . . ? N23 Ni1 N22 90.7(3) . . ? N24 Ni1 C21 89.2(3) . . ? N23 Ni1 C21 175.7(3) . . ? N22 Ni1 C21 88.3(3) . . ? C1 C21 C4 103.0(7) . . ? C1 C21 C26 115.4(7) . . ? C4 C21 C26 115.2(7) . . ? C1 C21 Ni1 114.8(5) . . ? C4 C21 Ni1 116.1(5) . . ? C26 C21 Ni1 93.0(5) . . ? C9 N22 C6 105.0(7) . . ? C9 N22 Ni1 125.6(5) . . ? C6 N22 Ni1 127.8(6) . . ? C14 N23 C11 105.4(6) . . ? C14 N23 Ni1 126.2(6) . . ? C11 N23 Ni1 127.6(5) . . ? C16 N24 C19 104.3(6) . . ? C16 N24 Ni1 125.1(6) . . ? C19 N24 Ni1 127.6(5) . . ? N2 C1 C20 123.0(8) . . ? N2 C1 C21 111.8(6) . . ? C20 C1 C21 125.2(7) . . ? C1 N2 C3 107.1(7) . . ? C1 N2 C25 126.2(8) . . ? C3 N2 C25 124.0(8) . . ? N2 C3 C4 110.2(6) . . ? N2 C3 C3 121.0(6) . 2_657 ? C4 C3 C3 128.7(5) . 2_657 ? C3 C4 C5 129.1(7) . . ? C3 C4 C21 107.6(7) . . ? C5 C4 C21 123.4(7) . . ? C4 C5 C6 118.0(7) . . ? C4 C5 C51 120.4(7) . . ? C6 C5 C51 121.6(7) . . ? C5 C6 N22 123.1(8) . . ? C5 C6 C7 126.9(7) . . ? N22 C6 C7 109.1(7) . . ? C8 C7 C6 106.4(7) . . ? C8 C7 H7A 126.8 . . ? C6 C7 H7A 126.8 . . ? C7 C8 C9 108.0(7) . . ? C7 C8 H8A 126.0 . . ? C9 C8 H8A 126.0 . . ? N22 C9 C10 125.9(7) . . ? N22 C9 C8 111.1(7) . . ? C10 C9 C8 123.0(8) . . ? C11 C10 C9 122.3(8) . . ? C11 C10 C101 119.0(7) . . ? C9 C10 C101 118.7(8) . . ? N23 C11 C10 123.8(7) . . ? N23 C11 C12 110.4(7) . . ? C10 C11 C12 125.6(8) . . ? C13 C12 C11 107.3(8) . . ? C13 C12 H12A 126.3 . . ? C11 C12 H12A 126.3 . . ? C12 C13 C14 107.0(7) . . ? C12 C13 H13A 126.5 . . ? C14 C13 H13A 126.5 . . ? N23 C14 C15 124.4(8) . . ? N23 C14 C13 109.7(8) . . ? C15 C14 C13 125.9(7) . . ? C16 C15 C14 123.0(7) . . ? C16 C15 C151 120.0(8) . . ? C14 C15 C151 117.0(7) . . ? C15 C16 N24 124.7(8) . . ? C15 C16 C17 124.4(7) . . ? N24 C16 C17 110.8(7) . . ? C18 C17 C16 108.8(7) . . ? C18 C17 H17A 125.6 . . ? C16 C17 H17A 125.6 . . ? C17 C18 C19 106.0(8) . . ? C17 C18 H18A 127.0 . . ? C19 C18 H18A 127.0 . . ? C20 C19 N24 124.8(7) . . ? C20 C19 C18 124.9(8) . . ? N24 C19 C18 109.9(6) . . ? C19 C20 C1 116.5(7) . . ? C19 C20 C201 121.7(7) . . ? C1 C20 C201 121.4(6) . . ? C52 C51 C56 118.9(7) . . ? C52 C51 C5 118.0(7) . . ? C56 C51 C5 123.2(7) . . ? C53 C52 C51 120.9(8) . . ? C53 C52 H52A 119.6 . . ? C51 C52 H52A 119.6 . . ? C52 C53 C54 120.9(8) . . ? C52 C53 H53A 119.5 . . ? C54 C53 H53A 119.5 . . ? C55 C54 C53 118.7(7) . . ? C55 C54 C57 120.5(7) . . ? C53 C54 C57 120.8(8) . . ? C54 C55 C56 121.5(8) . . ? C54 C55 H55A 119.3 . . ? C56 C55 H55A 119.3 . . ? C51 C56 C55 119.2(8) . . ? C51 C56 H56A 120.4 . . ? C55 C56 H56A 120.4 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C102 C101 C106 118.0(8) . . ? C102 C101 C10 121.1(8) . . ? C106 C101 C10 120.8(7) . . ? C103 C102 C101 120.7(9) . . ? C103 C102 H10A 119.7 . . ? C101 C102 H10A 119.7 . . ? C102 C103 C104 121.9(9) . . ? C102 C103 H10B 119.0 . . ? C104 C103 H10B 119.0 . . ? C105 C104 C103 117.2(8) . . ? C105 C104 C107 122.4(8) . . ? C103 C104 C107 120.4(8) . . ? C104 C105 C106 122.4(8) . . ? C104 C105 H10C 118.8 . . ? C106 C105 H10C 118.8 . . ? C105 C106 C101 119.7(8) . . ? C105 C106 H10D 120.2 . . ? C101 C106 H10D 120.2 . . ? C104 C107 H10E 109.5 . . ? C104 C107 H10F 109.5 . . ? H10E C107 H10F 109.5 . . ? C104 C107 H10G 109.5 . . ? H10E C107 H10G 109.5 . . ? H10F C107 H10G 109.5 . . ? C156 C151 C152 119.2(7) . . ? C156 C151 C15 122.5(8) . . ? C152 C151 C15 118.1(8) . . ? C153 C152 C151 119.0(8) . . ? C153 C152 H15A 120.5 . . ? C151 C152 H15A 120.5 . . ? C154 C153 C152 122.3(8) . . ? C154 C153 H15B 118.9 . . ? C152 C153 H15B 118.9 . . ? C155 C154 C153 116.8(8) . . ? C155 C154 C157 121.8(9) . . ? C153 C154 C157 121.3(9) . . ? C154 C155 C156 123.2(9) . . ? C154 C155 H15C 118.4 . . ? C156 C155 H15C 118.4 . . ? C151 C156 C155 119.3(9) . . ? C151 C156 H15D 120.3 . . ? C155 C156 H15D 120.3 . . ? C154 C157 H15E 109.5 . . ? C154 C157 H15F 109.5 . . ? H15E C157 H15F 109.5 . . ? C154 C157 H15G 109.5 . . ? H15E C157 H15G 109.5 . . ? H15F C157 H15G 109.5 . . ? C202 C201 C206 118.2(7) . . ? C202 C201 C20 122.5(7) . . ? C206 C201 C20 119.2(7) . . ? C203 C202 C201 119.6(7) . . ? C203 C202 H20A 120.2 . . ? C201 C202 H20A 120.2 . . ? C202 C203 C204 122.9(7) . . ? C202 C203 H20B 118.5 . . ? C204 C203 H20B 118.5 . . ? C205 C204 C203 117.8(8) . . ? C205 C204 C207 120.9(8) . . ? C203 C204 C207 121.2(8) . . ? C206 C205 C204 120.3(8) . . ? C206 C205 H20C 119.8 . . ? C204 C205 H20C 119.8 . . ? C205 C206 C201 121.0(7) . . ? C205 C206 H20D 119.5 . . ? C201 C206 H20D 119.5 . . ? C204 C207 H20E 109.5 . . ? C204 C207 H20F 109.5 . . ? H20E C207 H20F 109.5 . . ? C204 C207 H20G 109.5 . . ? H20E C207 H20G 109.5 . . ? H20F C207 H20G 109.5 . . ? N2 C25 H25A 109.5 . . ? N2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.301 _refine_diff_density_min -1.125 _refine_diff_density_rms 0.121