# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Wenbin Lin' 'Yong Cui' 'Helen L. Ngo' _publ_contact_author_name 'Prof Wenbin Lin' _publ_contact_author_address ; Dept of Chemistry Univ of North Carolina CB#3290 Chapel Hill NC 27599 UNITED STATES OF AMERICA ; _publ_contact_author_email WLIN@UNC.EDU _publ_section_title ; A homochiral triple helix constructed from an axially chiral bipyridine ; data_c02111m _database_code_CSD 200587 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47.50 H50 N2 Ni O8.50' _chemical_formula_weight 843.61 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 26.4314(7) _cell_length_b 11.4071(3) _cell_length_c 16.5957(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.379(2) _cell_angle_gamma 90.00 _cell_volume 4557.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 0.479 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15651 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.05 _reflns_number_total 8043 _reflns_number_gt 6327 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1076P)^2^+7.4282P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 8043 _refine_ls_number_parameters 520 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2004 _refine_ls_wR_factor_gt 0.1847 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.002 _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 -0.37393(3) -0.10570(6) -0.07234(5) 0.0438(2) Uani 1 1 d . . . O1 O -0.3657(3) 0.0293(4) -0.1458(5) 0.0793(19) Uani 1 1 d . . . O2 O -0.28974(19) -0.1069(7) -0.0004(4) 0.0827(17) Uani 1 1 d . . . O3 O -0.3831(2) -0.2453(4) -0.0050(3) 0.0555(13) Uani 1 1 d . . . O4 O -0.45771(14) -0.1005(4) -0.1451(2) 0.0405(8) Uani 1 1 d . . . O5 O -0.26912(17) 0.5170(3) 0.2921(3) 0.0442(10) Uani 1 1 d . . . O6 O -0.30086(16) 0.8345(3) 0.2827(2) 0.0381(9) Uani 1 1 d . . . N1 N -0.3817(2) 0.0163(5) 0.0172(4) 0.0516(15) Uani 1 1 d . . . N2 N -0.1371(2) 1.2766(4) 0.1627(4) 0.0409(13) Uani 1 1 d . . . C1 C -0.3084(2) 0.6298(4) 0.3722(4) 0.0318(11) Uani 1 1 d . . . C2 C -0.3121(2) 0.5373(5) 0.3177(4) 0.0384(13) Uani 1 1 d . . . C3 C -0.3610(3) 0.4645(5) 0.2796(4) 0.0418(14) Uani 1 1 d . . . C4 C -0.4037(3) 0.4874(5) 0.3032(4) 0.0431(14) Uani 1 1 d . . . H4A H -0.4351 0.4400 0.2810 0.052 Uiso 1 1 calc R . . C5 C -0.4475(3) 0.6072(6) 0.3822(5) 0.0556(17) Uani 1 1 d . . . H5A H -0.4791 0.5604 0.3603 0.067 Uiso 1 1 calc R . . C6 C -0.4449(3) 0.7004(7) 0.4350(5) 0.065(2) Uani 1 1 d . . . H6A H -0.4746 0.7155 0.4495 0.078 Uiso 1 1 calc R . . C7 C -0.3986(3) 0.7736(7) 0.4676(5) 0.0566(18) Uani 1 1 d . . . H7A H -0.3981 0.8383 0.5020 0.068 Uiso 1 1 calc R . . C8 C -0.3540(3) 0.7497(5) 0.4488(4) 0.0443(14) Uani 1 1 d . . . H8A H -0.3228 0.7976 0.4723 0.053 Uiso 1 1 calc R . . C9 C -0.3540(2) 0.6549(5) 0.3953(4) 0.0353(13) Uani 1 1 d . . . C10 C -0.4017(3) 0.5807(6) 0.3601(4) 0.0430(15) Uani 1 1 d . . . C11 C -0.2313(3) 0.4245(6) 0.3416(5) 0.064(2) Uani 1 1 d . . . H11A H -0.2027 0.4155 0.3205 0.096 Uiso 1 1 calc R . . H11B H -0.2514 0.3522 0.3336 0.096 Uiso 1 1 calc R . . H11C H -0.2148 0.4445 0.4032 0.096 Uiso 1 1 calc R . . C12 C -0.3615(3) 0.3726(5) 0.2169(4) 0.0503(17) Uani 1 1 d . . . H12A H -0.3338 0.3766 0.1963 0.060 Uiso 1 1 calc R . . C13 C -0.3972(3) 0.2852(5) 0.1867(5) 0.0506(16) Uani 1 1 d . . . H13A H -0.4269 0.2816 0.2030 0.061 Uiso 1 1 calc R . . C14 C -0.3919(3) 0.1916(6) 0.1273(5) 0.0512(16) Uani 1 1 d . . . C15 C -0.3475(4) 0.1873(7) 0.1042(7) 0.087(3) Uani 1 1 d . . . H15A H -0.3195 0.2432 0.1261 0.104 Uiso 1 1 calc R . . C16 C -0.3446(4) 0.1011(8) 0.0491(7) 0.086(3) Uani 1 1 d . . . H16A H -0.3148 0.1022 0.0330 0.103 Uiso 1 1 calc R . . C17 C -0.4230(3) 0.0161(5) 0.0434(4) 0.0457(14) Uani 1 1 d . . . H17A H -0.4485 -0.0451 0.0252 0.055 Uiso 1 1 calc R . . C18 C -0.4298(3) 0.1023(6) 0.0962(4) 0.0494(16) Uani 1 1 d . . . H18A H -0.4603 0.1000 0.1107 0.059 Uiso 1 1 calc R . . C19 C -0.2578(2) 0.7055(5) 0.4053(4) 0.0349(12) Uani 1 1 d . . . C20 C -0.2549(2) 0.7997(5) 0.3564(3) 0.0321(11) Uani 1 1 d . . . C21 C -0.2051(2) 0.8691(4) 0.3840(4) 0.0373(13) Uani 1 1 d . . . C22 C -0.1611(3) 0.8394(5) 0.4595(4) 0.0438(14) Uani 1 1 d . . . H22A H -0.1289 0.8842 0.4773 0.053 Uiso 1 1 calc R . . C23 C -0.1150(3) 0.7108(6) 0.5900(5) 0.0560(18) Uani 1 1 d . . . H23A H -0.0823 0.7538 0.6073 0.067 Uiso 1 1 calc R . . C24 C -0.1174(3) 0.6181(7) 0.6390(5) 0.0611(19) Uani 1 1 d . . . H24A H -0.0860 0.5964 0.6886 0.073 Uiso 1 1 calc R . . C25 C -0.1672(3) 0.5537(6) 0.6153(5) 0.0582(19) Uani 1 1 d . . . H25A H -0.1688 0.4919 0.6507 0.070 Uiso 1 1 calc R . . C26 C -0.2130(3) 0.5820(5) 0.5403(4) 0.0473(15) Uani 1 1 d . . . H26A H -0.2455 0.5386 0.5247 0.057 Uiso 1 1 calc R . . C27 C -0.2115(2) 0.6763(5) 0.4867(4) 0.0361(12) Uani 1 1 d . . . C28 C -0.1622(3) 0.7433(5) 0.5121(4) 0.0440(14) Uani 1 1 d . . . C29 C -0.3060(3) 0.7880(6) 0.2010(4) 0.0552(17) Uani 1 1 d . . . H29A H -0.3391 0.8182 0.1545 0.083 Uiso 1 1 calc R . . H29B H -0.3082 0.7041 0.2025 0.083 Uiso 1 1 calc R . . H29C H -0.2742 0.8101 0.1904 0.083 Uiso 1 1 calc R . . C30 C -0.2030(3) 0.9661(5) 0.3256(4) 0.0409(13) Uani 1 1 d . . . H30A H -0.2341 0.9768 0.2728 0.049 Uiso 1 1 calc R . . C31 C -0.1604(3) 1.0391(6) 0.3420(4) 0.0507(16) Uani 1 1 d . . . H31A H -0.1319 1.0365 0.3985 0.061 Uiso 1 1 calc R . . C32 C -0.1544(3) 1.1215(6) 0.2807(4) 0.0452(15) Uani 1 1 d . . . C33 C -0.1891(3) 1.1239(7) 0.1912(5) 0.066(2) Uani 1 1 d . . . H33A H -0.2197 1.0743 0.1681 0.079 Uiso 1 1 calc R . . C34 C -0.1776(3) 1.2009(7) 0.1370(5) 0.064(2) Uani 1 1 d . . . H34A H -0.2006 1.1985 0.0770 0.076 Uiso 1 1 calc R . . C35 C -0.1046(3) 1.2786(7) 0.2485(5) 0.0599(19) Uani 1 1 d . . . H35A H -0.0760 1.3333 0.2694 0.072 Uiso 1 1 calc R . . C36 C -0.1113(3) 1.2030(7) 0.3082(5) 0.067(2) Uani 1 1 d . . . H36A H -0.0867 1.2064 0.3676 0.080 Uiso 1 1 calc R . . C37 C -0.3286(7) 0.1434(12) -0.2273(15) 0.214(12) Uani 1 1 d . . . H37A H -0.3673 0.1626 -0.2560 0.321 Uiso 1 1 calc R . . H37B H -0.3169 0.1082 -0.2694 0.321 Uiso 1 1 calc R . . H37C H -0.3075 0.2135 -0.2041 0.321 Uiso 1 1 calc R . . C38 C -0.3190(5) 0.0570(8) -0.1514(10) 0.112(5) Uani 1 1 d . . . C39 C -0.2698(6) 0.0153(12) -0.1007(13) 0.139(6) Uani 1 1 d . . . H39A H -0.2408 0.0369 -0.1155 0.167 Uiso 1 1 calc R . . C40 C -0.2557(4) -0.0592(12) -0.0259(10) 0.116(5) Uani 1 1 d . . . C41 C -0.1965(4) -0.0911(17) 0.0258(13) 0.200(9) Uani 1 1 d . . . H41A H -0.1932 -0.1390 0.0753 0.299 Uiso 1 1 calc R . . H41B H -0.1749 -0.0211 0.0468 0.299 Uiso 1 1 calc R . . H41C H -0.1831 -0.1337 -0.0113 0.299 Uiso 1 1 calc R . . C42 C -0.4176(5) -0.4218(7) 0.0231(7) 0.096(3) Uani 1 1 d . . . H42A H -0.3803 -0.4264 0.0680 0.144 Uiso 1 1 calc R . . H42B H -0.4249 -0.4886 -0.0154 0.144 Uiso 1 1 calc R . . H42C H -0.4433 -0.4211 0.0503 0.144 Uiso 1 1 calc R . . C43 C -0.4243(4) -0.3097(6) -0.0307(5) 0.0552(18) Uani 1 1 d . . . C44 C -0.4749(3) -0.2855(6) -0.0987(5) 0.0625(19) Uani 1 1 d . . . H44A H -0.5020 -0.3434 -0.1119 0.075 Uiso 1 1 calc R . . C45 C -0.4904(2) -0.1836(6) -0.1505(4) 0.0429(14) Uani 1 1 d . . . C46 C -0.5499(3) -0.1698(8) -0.2153(6) 0.071(2) Uani 1 1 d . . . H46A H -0.5544 -0.0963 -0.2456 0.106 Uiso 1 1 calc R . . H46B H -0.5735 -0.1716 -0.1842 0.106 Uiso 1 1 calc R . . H46C H -0.5598 -0.2327 -0.2574 0.106 Uiso 1 1 calc R . . O7 O -0.4739(7) 0.1508(17) -0.1950(12) 0.254(7) Uiso 1 1 d D . . C47 C -0.4753(8) 0.0790(16) -0.2697(12) 0.171(7) Uiso 1 1 d D . . O8 O -0.4871(12) 0.376(2) -0.4646(16) 0.207(11) Uiso 0.50 1 d PD . . C48 C -0.462(2) 0.348(5) -0.371(2) 0.24(2) Uiso 0.50 1 d PD . . O9 O -0.4864(8) 0.3159(17) -0.2639(13) 0.136(6) Uiso 0.50 1 d P . . O10 O -0.4741(10) -0.036(2) -0.4416(15) 0.177(9) Uiso 0.50 1 d P . . 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 0.0408(4) 0.0360(4) 0.0541(5) -0.0174(4) 0.0191(3) -0.0058(4) O1 0.095(4) 0.039(3) 0.141(6) -0.006(3) 0.086(4) -0.008(3) O2 0.045(3) 0.091(4) 0.102(4) -0.057(4) 0.020(3) -0.010(4) O3 0.081(4) 0.048(3) 0.037(3) -0.004(2) 0.023(3) 0.007(3) O4 0.0401(19) 0.0388(18) 0.043(2) -0.007(2) 0.0172(17) -0.003(2) O5 0.044(2) 0.038(2) 0.055(3) -0.0100(19) 0.025(2) -0.0010(19) O6 0.042(2) 0.038(2) 0.030(2) -0.0005(17) 0.0113(18) 0.0002(18) N1 0.041(3) 0.046(3) 0.062(4) -0.026(3) 0.014(3) -0.005(3) N2 0.043(3) 0.036(3) 0.038(3) 0.010(2) 0.012(3) 0.001(2) C1 0.038(3) 0.027(2) 0.029(3) 0.000(2) 0.012(2) -0.005(2) C2 0.046(3) 0.031(3) 0.044(3) -0.003(2) 0.024(3) -0.002(2) C3 0.047(3) 0.033(3) 0.043(4) -0.010(3) 0.017(3) -0.007(3) C4 0.042(3) 0.036(3) 0.049(4) -0.010(3) 0.016(3) -0.015(3) C5 0.052(4) 0.067(4) 0.056(4) -0.008(4) 0.031(4) -0.016(3) C6 0.062(5) 0.087(5) 0.063(5) -0.017(4) 0.044(4) -0.001(4) C7 0.066(5) 0.063(4) 0.051(4) -0.019(3) 0.034(4) -0.009(4) C8 0.050(3) 0.046(3) 0.040(3) -0.014(3) 0.022(3) -0.008(3) C9 0.043(3) 0.035(3) 0.025(3) -0.004(2) 0.011(3) -0.007(3) C10 0.049(4) 0.046(3) 0.040(4) -0.002(3) 0.023(3) -0.004(3) C11 0.064(4) 0.056(5) 0.070(5) -0.007(3) 0.026(4) 0.017(3) C12 0.062(4) 0.034(4) 0.060(4) -0.019(3) 0.030(3) -0.011(3) C13 0.055(4) 0.042(3) 0.056(4) -0.023(3) 0.025(3) -0.012(3) C14 0.052(4) 0.044(3) 0.058(4) -0.016(3) 0.022(3) -0.007(3) C15 0.071(5) 0.070(5) 0.136(8) -0.066(6) 0.059(6) -0.033(4) C16 0.063(5) 0.086(6) 0.124(8) -0.062(6) 0.054(5) -0.028(5) C17 0.046(4) 0.035(3) 0.050(4) -0.008(3) 0.014(3) -0.008(3) C18 0.049(4) 0.050(4) 0.051(4) -0.015(3) 0.022(3) -0.005(3) C19 0.040(3) 0.031(3) 0.037(3) -0.002(2) 0.020(3) 0.002(2) C20 0.035(3) 0.032(3) 0.028(3) -0.002(2) 0.012(2) -0.001(2) C21 0.043(3) 0.028(3) 0.040(3) -0.002(2) 0.017(3) -0.004(2) C22 0.040(3) 0.040(3) 0.046(4) 0.002(3) 0.011(3) -0.011(3) C23 0.051(4) 0.052(4) 0.051(4) 0.002(3) 0.007(4) -0.008(3) C24 0.062(5) 0.062(4) 0.042(4) 0.004(3) 0.005(4) -0.001(4) C25 0.079(5) 0.045(4) 0.044(4) 0.009(3) 0.018(4) -0.003(4) C26 0.058(4) 0.040(3) 0.037(4) 0.000(3) 0.013(3) -0.011(3) C27 0.048(3) 0.031(3) 0.029(3) 0.000(2) 0.016(3) -0.004(3) C28 0.045(4) 0.036(3) 0.044(4) 0.002(3) 0.011(3) 0.000(3) C29 0.059(4) 0.058(4) 0.042(4) -0.006(3) 0.014(3) -0.010(3) C30 0.041(3) 0.036(3) 0.037(3) 0.005(2) 0.008(3) -0.002(3) C31 0.048(4) 0.058(4) 0.036(4) 0.013(3) 0.007(3) -0.007(3) C32 0.050(4) 0.041(3) 0.046(4) 0.001(3) 0.021(3) -0.009(3) C33 0.059(5) 0.062(4) 0.059(5) 0.017(4) 0.006(4) -0.024(4) C34 0.064(5) 0.064(5) 0.045(4) 0.019(4) 0.004(4) -0.020(4) C35 0.054(4) 0.069(5) 0.055(5) -0.002(4) 0.021(4) -0.031(4) C36 0.066(5) 0.091(5) 0.038(4) 0.001(4) 0.016(4) -0.042(4) C37 0.226(19) 0.107(10) 0.44(3) 0.116(16) 0.27(2) 0.044(11) C38 0.107(9) 0.051(5) 0.229(15) 0.008(7) 0.120(10) 0.008(5) C39 0.103(10) 0.098(9) 0.27(2) -0.019(11) 0.128(13) -0.020(8) C40 0.040(5) 0.121(10) 0.192(13) -0.081(9) 0.055(7) -0.021(5) C41 0.049(5) 0.181(14) 0.33(2) -0.093(18) 0.037(9) 0.002(9) C42 0.139(9) 0.053(4) 0.129(9) 0.031(5) 0.088(8) 0.026(5) C43 0.086(6) 0.041(3) 0.051(4) 0.002(3) 0.040(4) 0.005(4) C44 0.067(5) 0.051(4) 0.074(5) -0.008(4) 0.034(4) -0.015(4) C45 0.038(3) 0.052(4) 0.039(3) -0.021(3) 0.017(3) -0.009(3) C46 0.048(4) 0.086(5) 0.068(5) -0.016(4) 0.014(4) -0.001(4) _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 O3 2.017(5) . ? Ni1 O1 2.031(6) . ? Ni1 O4 2.039(4) . ? Ni1 O2 2.046(5) . ? Ni1 N1 2.106(5) . ? Ni1 N2 2.121(5) 4_435 ? O1 C38 1.314(11) . ? O2 C40 1.263(14) . ? O3 C43 1.235(9) . ? O4 C45 1.261(7) . ? O5 C2 1.386(7) . ? O5 C11 1.452(8) . ? O6 C20 1.380(7) . ? O6 C29 1.409(7) . ? N1 C16 1.322(9) . ? N1 C17 1.333(9) . ? N2 C34 1.301(9) . ? N2 C35 1.326(9) . ? N2 Ni1 2.121(5) 4_465 ? C1 C2 1.368(8) . ? C1 C9 1.436(8) . ? C1 C19 1.492(8) . ? C2 C3 1.445(8) . ? C3 C4 1.362(9) . ? C3 C12 1.473(8) . ? C4 C10 1.409(8) . ? C5 C6 1.361(10) . ? C5 C10 1.433(9) . ? C6 C7 1.392(10) . ? C7 C8 1.366(9) . ? C8 C9 1.400(8) . ? C9 C10 1.429(9) . ? C12 C13 1.321(8) . ? C13 C14 1.499(9) . ? C14 C18 1.372(9) . ? C14 C15 1.379(10) . ? C15 C16 1.366(10) . ? C17 C18 1.376(9) . ? C19 C20 1.368(8) . ? C19 C27 1.438(8) . ? C20 C21 1.439(8) . ? C21 C22 1.355(8) . ? C21 C30 1.488(7) . ? C22 C28 1.409(8) . ? C23 C24 1.350(10) . ? C23 C28 1.427(9) . ? C24 C25 1.414(11) . ? C25 C26 1.370(10) . ? C26 C27 1.407(8) . ? C27 C28 1.417(8) . ? C30 C31 1.334(9) . ? C31 C32 1.442(9) . ? C32 C33 1.387(10) . ? C32 C36 1.394(9) . ? C33 C34 1.378(10) . ? C35 C36 1.379(9) . ? C37 C38 1.536(19) . ? C38 C39 1.311(19) . ? C39 C40 1.422(19) . ? C40 C41 1.488(16) . ? C42 C43 1.527(10) . ? C43 C44 1.376(11) . ? C44 C45 1.402(10) . ? C45 C46 1.501(10) . ? O7 C47 1.473(15) . ? O8 O8 1.09(5) 2_454 ? O8 C48 1.447(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 O3 Ni1 O1 176.9(2) . . ? O3 Ni1 O4 90.1(2) . . ? O1 Ni1 O4 89.0(2) . . ? O3 Ni1 O2 91.2(3) . . ? O1 Ni1 O2 89.7(3) . . ? O4 Ni1 O2 178.6(3) . . ? O3 Ni1 N1 93.6(2) . . ? O1 Ni1 N1 89.4(3) . . ? O4 Ni1 N1 90.0(2) . . ? O2 Ni1 N1 89.5(2) . . ? O3 Ni1 N2 88.6(2) . 4_435 ? O1 Ni1 N2 88.6(2) . 4_435 ? O4 Ni1 N2 91.89(19) . 4_435 ? O2 Ni1 N2 88.5(2) . 4_435 ? N1 Ni1 N2 177.1(2) . 4_435 ? C38 O1 Ni1 124.2(7) . . ? C40 O2 Ni1 123.7(8) . . ? C43 O3 Ni1 124.7(5) . . ? C45 O4 Ni1 124.5(4) . . ? C2 O5 C11 114.1(5) . . ? C20 O6 C29 116.4(5) . . ? C16 N1 C17 116.3(6) . . ? C16 N1 Ni1 119.6(5) . . ? C17 N1 Ni1 124.1(4) . . ? C34 N2 C35 116.4(6) . . ? C34 N2 Ni1 121.5(5) . 4_465 ? C35 N2 Ni1 122.1(4) . 4_465 ? C2 C1 C9 119.4(5) . . ? C2 C1 C19 119.9(5) . . ? C9 C1 C19 120.6(5) . . ? C1 C2 O5 119.2(5) . . ? C1 C2 C3 122.7(5) . . ? O5 C2 C3 117.9(5) . . ? C4 C3 C2 117.5(5) . . ? C4 C3 C12 124.9(5) . . ? C2 C3 C12 117.6(5) . . ? C3 C4 C10 122.1(5) . . ? C6 C5 C10 120.3(6) . . ? C5 C6 C7 121.5(6) . . ? C8 C7 C6 119.6(6) . . ? C7 C8 C9 121.7(6) . . ? C8 C9 C10 119.1(5) . . ? C8 C9 C1 122.9(5) . . ? C10 C9 C1 118.0(5) . . ? C4 C10 C9 120.2(5) . . ? C4 C10 C5 122.0(6) . . ? C9 C10 C5 117.8(6) . . ? C13 C12 C3 127.0(6) . . ? C12 C13 C14 122.8(6) . . ? C18 C14 C15 116.3(6) . . ? C18 C14 C13 121.6(6) . . ? C15 C14 C13 122.0(6) . . ? C16 C15 C14 120.1(7) . . ? N1 C16 C15 123.9(7) . . ? N1 C17 C18 123.1(6) . . ? C14 C18 C17 120.2(6) . . ? C20 C19 C27 120.3(5) . . ? C20 C19 C1 119.8(5) . . ? C27 C19 C1 119.9(5) . . ? C19 C20 O6 120.5(5) . . ? C19 C20 C21 120.7(5) . . ? O6 C20 C21 118.6(5) . . ? C22 C21 C20 118.7(5) . . ? C22 C21 C30 122.6(5) . . ? C20 C21 C30 118.5(5) . . ? C21 C22 C28 122.5(5) . . ? C24 C23 C28 120.6(7) . . ? C23 C24 C25 120.6(7) . . ? C26 C25 C24 120.2(6) . . ? C25 C26 C27 120.6(6) . . ? C26 C27 C28 119.2(6) . . ? C26 C27 C19 122.3(5) . . ? C28 C27 C19 118.5(5) . . ? C22 C28 C27 119.2(6) . . ? C22 C28 C23 122.0(6) . . ? C27 C28 C23 118.8(6) . . ? C31 C30 C21 125.9(6) . . ? C30 C31 C32 126.3(6) . . ? C33 C32 C36 115.3(6) . . ? C33 C32 C31 123.5(6) . . ? C36 C32 C31 121.2(6) . . ? C34 C33 C32 119.0(7) . . ? N2 C34 C33 125.6(7) . . ? N2 C35 C36 122.8(6) . . ? C35 C36 C32 120.8(6) . . ? C39 C38 O1 125.3(12) . . ? C39 C38 C37 122.9(12) . . ? O1 C38 C37 111.7(11) . . ? C38 C39 C40 127.6(11) . . ? O2 C40 C39 125.7(10) . . ? O2 C40 C41 115.3(16) . . ? C39 C40 C41 118.9(14) . . ? O3 C43 C44 125.8(6) . . ? O3 C43 C42 115.0(8) . . ? C44 C43 C42 119.1(8) . . ? C43 C44 C45 127.4(7) . . ? O4 C45 C44 124.1(6) . . ? O4 C45 C46 117.2(6) . . ? C44 C45 C46 118.7(7) . . ? O8 O8 C48 164(4) 2_454 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.894 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.090