Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'I. Dance' 'John C. McMurtrie' _publ_contact_author_name 'Prof I Dance' _publ_contact_author_address ; Department of Chemistry University of New South Wales KENSINGTON New South Wales 2052 AUSTRALIA ; _publ_contact_author_email I.DANCE@UNSW.EDU.AU _publ_requested_journal 'Cryst Eng. Comm.' _publ_section_title ; Engineering grids of metal complexes: development of the 2D M(terpy)2 embrace motif in crystals ; data_jcm28_crystal3 _database_code_depnum_ccdc_archive 'CCDC 260308' _audit_creation_method SHELXL-97 _chemical_name_common '[Ni(terpy)2](PF6)2.DMF' _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 N6 Ni, C3 H7 N O, 2(F6 P)' _chemical_formula_sum 'C33 H29 F12 N7 Ni O P2' _chemical_formula_weight 888.28 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8680(10) _cell_length_b 9.1230(10) _cell_length_c 45.055(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.4130(10) _cell_angle_gamma 90.00 _cell_volume 3634.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 994 _cell_measurement_theta_min 2.410 _cell_measurement_theta_max 27.933 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.732 _exptl_absorpt_correction_T_max 0.840 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 498 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.01 _diffrn_reflns_number 26371 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8629 _reflns_number_gt 7983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+7.4179P] 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_number_reflns 8629 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1491 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 C1 C 0.2738(3) 0.4899(3) 0.83768(7) 0.0287(6) Uani 1 1 d . . . H1 H 0.2322 0.4582 0.8187 0.034 Uiso 1 1 calc R . . C2 C 0.3353(4) 0.6299(4) 0.84047(8) 0.0370(7) Uani 1 1 d . . . H2 H 0.3361 0.6927 0.8237 0.044 Uiso 1 1 calc R . . C3 C 0.3950(4) 0.6760(3) 0.86805(9) 0.0408(8) Uani 1 1 d . . . H3 H 0.4387 0.7708 0.8704 0.049 Uiso 1 1 calc R . . C4 C 0.3908(3) 0.5836(3) 0.89218(8) 0.0346(7) Uani 1 1 d . . . H4 H 0.4300 0.6143 0.9114 0.042 Uiso 1 1 calc R . . C5 C 0.3282(3) 0.4447(3) 0.88792(7) 0.0264(6) Uani 1 1 d . . . C6 C 0.3175(3) 0.3377(3) 0.91250(7) 0.0277(6) Uani 1 1 d . . . C7 C 0.3761(4) 0.3561(4) 0.94183(7) 0.0381(7) Uani 1 1 d . . . H7 H 0.4280 0.4434 0.9479 0.046 Uiso 1 1 calc R . . C8 C 0.3567(4) 0.2436(4) 0.96189(7) 0.0440(8) Uani 1 1 d . . . H8 H 0.3957 0.2538 0.9820 0.053 Uiso 1 1 calc R . . C9 C 0.2811(4) 0.1168(4) 0.95281(7) 0.0364(7) Uani 1 1 d . . . H9 H 0.2668 0.0399 0.9665 0.044 Uiso 1 1 calc R . . C10 C 0.2265(3) 0.1048(3) 0.92317(6) 0.0273(6) Uani 1 1 d . . . C11 C 0.1481(3) -0.0247(3) 0.90919(6) 0.0252(5) Uani 1 1 d . . . C12 C 0.1086(4) -0.1480(4) 0.92506(7) 0.0339(7) Uani 1 1 d . . . H12 H 0.1303 -0.1524 0.9460 0.041 Uiso 1 1 calc R . . C13 C 0.0373(4) -0.2645(4) 0.90998(8) 0.0366(7) Uani 1 1 d . . . H13 H 0.0100 -0.3499 0.9204 0.044 Uiso 1 1 calc R . . C14 C 0.0068(3) -0.2541(3) 0.87962(7) 0.0326(6) Uani 1 1 d . . . H14 H -0.0417 -0.3323 0.8687 0.039 Uiso 1 1 calc R . . C15 C 0.0481(3) -0.1277(3) 0.86515(6) 0.0267(5) Uani 1 1 d . . . H15 H 0.0263 -0.1210 0.8442 0.032 Uiso 1 1 calc R . . C16 C -0.1139(4) 0.3310(4) 0.87573(9) 0.0389(7) Uani 1 1 d . . . H16 H -0.0717 0.3326 0.8958 0.047 Uiso 1 1 calc R . . C17 C -0.2540(4) 0.3957(4) 0.86891(11) 0.0540(11) Uani 1 1 d . . . H17 H -0.3066 0.4418 0.8840 0.065 Uiso 1 1 calc R . . C18 C -0.3148(4) 0.3917(5) 0.84003(12) 0.0604(12) Uani 1 1 d . . . H18 H -0.4104 0.4356 0.8349 0.072 Uiso 1 1 calc R . . C19 C -0.2377(4) 0.3239(4) 0.81814(10) 0.0496(10) Uani 1 1 d . . . H19 H -0.2799 0.3195 0.7981 0.059 Uiso 1 1 calc R . . C20 C -0.0959(3) 0.2622(3) 0.82640(7) 0.0326(7) Uani 1 1 d . . . C21 C 0.0013(4) 0.1929(3) 0.80518(7) 0.0322(6) Uani 1 1 d . . . C22 C -0.0358(5) 0.1723(4) 0.77483(8) 0.0471(9) Uani 1 1 d . . . H22 H -0.1310 0.2027 0.7658 0.057 Uiso 1 1 calc R . . C23 C 0.0699(5) 0.1065(5) 0.75835(8) 0.0552(11) Uani 1 1 d . . . H23 H 0.0462 0.0897 0.7377 0.066 Uiso 1 1 calc R . . C24 C 0.2106(5) 0.0639(4) 0.77130(7) 0.0451(9) Uani 1 1 d . . . H24 H 0.2835 0.0195 0.7598 0.054 Uiso 1 1 calc R . . C25 C 0.2412(4) 0.0883(3) 0.80151(6) 0.0301(6) Uani 1 1 d . . . C26 C 0.3848(3) 0.0523(3) 0.81923(6) 0.0282(6) Uani 1 1 d . . . C27 C 0.5070(4) -0.0163(4) 0.80750(8) 0.0401(8) Uani 1 1 d . . . H27 H 0.5025 -0.0432 0.7871 0.048 Uiso 1 1 calc R . . C28 C 0.6362(4) -0.0450(4) 0.82623(9) 0.0457(9) Uani 1 1 d . . . H28 H 0.7209 -0.0915 0.8186 0.055 Uiso 1 1 calc R . . C29 C 0.6408(4) -0.0056(4) 0.85588(8) 0.0381(7) Uani 1 1 d . . . H29 H 0.7277 -0.0249 0.8690 0.046 Uiso 1 1 calc R . . C30 C 0.5146(3) 0.0631(3) 0.86599(7) 0.0277(6) Uani 1 1 d . . . H30 H 0.5173 0.0917 0.8863 0.033 Uiso 1 1 calc R . . C31 C 0.8971(5) -0.5617(5) 0.96204(9) 0.0529(10) Uani 1 1 d . . . H31 H 0.8578 -0.4650 0.9626 0.064 Uiso 1 1 calc R . . C32 C 0.9055(5) -0.8068(4) 0.98209(9) 0.0528(10) Uani 1 1 d . . . H32A H 0.8578 -0.8624 0.9975 0.079 Uiso 1 1 calc R . . H32B H 1.0153 -0.8051 0.9867 0.079 Uiso 1 1 calc R . . H32C H 0.8823 -0.8536 0.9627 0.079 Uiso 1 1 calc R . . C33 C 0.7441(6) -0.6158(7) 1.00301(11) 0.0797(17) Uani 1 1 d . . . H33A H 0.7215 -0.7012 1.0151 0.120 Uiso 1 1 calc R . . H33B H 0.6503 -0.5786 0.9928 0.120 Uiso 1 1 calc R . . H33C H 0.7904 -0.5391 1.0159 0.120 Uiso 1 1 calc R . . N1 N 0.2713(2) 0.3985(3) 0.86083(5) 0.0239(5) Uani 1 1 d . . . N2 N 0.2448(3) 0.2145(3) 0.90395(5) 0.0229(4) Uani 1 1 d . . . N3 N 0.1172(2) -0.0153(2) 0.87938(5) 0.0221(4) Uani 1 1 d . . . N4 N -0.0365(3) 0.2663(3) 0.85493(6) 0.0288(5) Uani 1 1 d . . . N5 N 0.1371(3) 0.1507(3) 0.81759(5) 0.0250(5) Uani 1 1 d . . . N6 N 0.3893(3) 0.0907(2) 0.84831(5) 0.0234(4) Uani 1 1 d . . . N7 N 0.8477(3) -0.6578(4) 0.98120(6) 0.0411(7) Uani 1 1 d . . . F1 F 0.5730(3) -0.3018(2) 0.96129(5) 0.0476(5) Uani 1 1 d . . . F2 F 0.5944(3) -0.0614(3) 0.97345(5) 0.0526(6) Uani 1 1 d . . . F3 F 0.7121(3) -0.0194(3) 0.93142(5) 0.0677(8) Uani 1 1 d . . . F4 F 0.6909(2) -0.2608(3) 0.91980(5) 0.0492(5) Uani 1 1 d . . . F5 F 0.4836(2) -0.1302(2) 0.92841(5) 0.0483(5) Uani 1 1 d . . . F6 F 0.8016(3) -0.1898(3) 0.96452(5) 0.0554(6) Uani 1 1 d . . . F7 F -0.0156(5) 0.5141(3) 0.77082(7) 0.0978(13) Uani 1 1 d . . . F8 F -0.2259(3) 0.6447(5) 0.77971(7) 0.0932(12) Uani 1 1 d . . . F9 F -0.0738(4) 0.8380(3) 0.79198(7) 0.0805(10) Uani 1 1 d . . . F10 F 0.1265(3) 0.7063(4) 0.78252(6) 0.0705(8) Uani 1 1 d . . . F11 F -0.0585(3) 0.7278(3) 0.74685(5) 0.0662(7) Uani 1 1 d . . . F12 F -0.0390(3) 0.6213(3) 0.81449(5) 0.0553(6) Uani 1 1 d . . . P1 P 0.64310(9) -0.15876(9) 0.946446(18) 0.03210(18) Uani 1 1 d . . . P2 P -0.05109(10) 0.67541(9) 0.780414(18) 0.03257(18) Uani 1 1 d . . . Ni1 Ni 0.18470(4) 0.18353(4) 0.860904(7) 0.01943(10) Uani 1 1 d . . . O1 O 0.9886(4) -0.5868(3) 0.94370(7) 0.0606(8) 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 C1 0.0245(13) 0.0261(14) 0.0355(15) 0.0046(11) 0.0015(11) 0.0001(11) C2 0.0332(15) 0.0261(15) 0.0518(19) 0.0111(14) 0.0041(14) -0.0015(12) C3 0.0357(17) 0.0223(14) 0.064(2) -0.0026(14) 0.0032(15) -0.0064(12) C4 0.0308(15) 0.0285(15) 0.0442(18) -0.0083(13) 0.0007(13) -0.0045(12) C5 0.0193(12) 0.0236(13) 0.0362(15) -0.0035(11) 0.0018(10) 0.0010(10) C6 0.0262(13) 0.0271(14) 0.0297(14) -0.0060(11) 0.0019(11) 0.0011(11) C7 0.0450(18) 0.0367(17) 0.0318(16) -0.0101(13) -0.0024(13) -0.0037(14) C8 0.057(2) 0.050(2) 0.0229(14) -0.0066(14) -0.0060(14) -0.0012(17) C9 0.0467(18) 0.0397(18) 0.0229(14) 0.0028(12) 0.0029(12) 0.0007(14) C10 0.0283(13) 0.0302(14) 0.0238(13) -0.0002(11) 0.0054(10) 0.0035(11) C11 0.0245(12) 0.0270(14) 0.0248(13) 0.0024(10) 0.0057(10) 0.0034(10) C12 0.0401(16) 0.0332(16) 0.0294(14) 0.0084(12) 0.0092(12) 0.0000(13) C13 0.0406(17) 0.0308(16) 0.0403(17) 0.0086(13) 0.0149(13) -0.0041(13) C14 0.0310(14) 0.0275(15) 0.0399(16) 0.0008(12) 0.0073(12) -0.0058(12) C15 0.0265(13) 0.0262(14) 0.0278(13) -0.0002(11) 0.0040(10) -0.0024(11) C16 0.0278(15) 0.0297(16) 0.060(2) -0.0016(14) 0.0088(14) 0.0009(12) C17 0.0290(17) 0.040(2) 0.095(3) 0.007(2) 0.0155(19) 0.0085(15) C18 0.0230(16) 0.046(2) 0.111(4) 0.019(2) 0.003(2) 0.0077(15) C19 0.0310(17) 0.0392(19) 0.075(3) 0.0229(18) -0.0168(17) -0.0059(14) C20 0.0262(14) 0.0243(14) 0.0455(17) 0.0124(12) -0.0078(12) -0.0081(11) C21 0.0365(15) 0.0259(14) 0.0321(15) 0.0083(12) -0.0108(12) -0.0097(12) C22 0.057(2) 0.046(2) 0.0350(18) 0.0090(15) -0.0177(16) -0.0149(17) C23 0.085(3) 0.057(2) 0.0210(15) 0.0047(15) -0.0128(17) -0.022(2) C24 0.067(2) 0.045(2) 0.0245(15) -0.0023(14) 0.0086(15) -0.0139(17) C25 0.0420(16) 0.0264(14) 0.0222(13) 0.0024(11) 0.0052(11) -0.0084(12) C26 0.0366(15) 0.0220(13) 0.0273(13) 0.0024(11) 0.0112(11) -0.0040(11) C27 0.053(2) 0.0320(16) 0.0385(17) -0.0010(13) 0.0259(15) 0.0016(14) C28 0.0399(18) 0.0360(18) 0.065(2) 0.0028(16) 0.0288(17) 0.0076(14) C29 0.0272(14) 0.0308(16) 0.058(2) 0.0097(14) 0.0122(14) 0.0049(12) C30 0.0243(13) 0.0231(13) 0.0365(15) 0.0054(11) 0.0065(11) 0.0002(10) C31 0.069(3) 0.045(2) 0.046(2) 0.0123(17) 0.0121(19) 0.0101(19) C32 0.071(3) 0.041(2) 0.047(2) 0.0051(16) 0.0065(19) -0.0096(19) C33 0.070(3) 0.116(5) 0.056(3) 0.022(3) 0.028(2) 0.033(3) N1 0.0203(10) 0.0208(11) 0.0305(12) 0.0004(9) 0.0015(9) -0.0001(8) N2 0.0226(10) 0.0238(11) 0.0224(10) -0.0031(9) 0.0027(8) 0.0023(8) N3 0.0207(10) 0.0225(11) 0.0234(11) 0.0014(8) 0.0036(8) 0.0005(8) N4 0.0211(11) 0.0239(11) 0.0410(14) 0.0037(10) 0.0006(10) -0.0009(9) N5 0.0311(12) 0.0209(11) 0.0224(11) 0.0036(9) -0.0012(9) -0.0062(9) N6 0.0253(11) 0.0193(10) 0.0262(11) 0.0026(9) 0.0063(9) -0.0009(9) N7 0.0413(15) 0.0489(17) 0.0337(14) 0.0090(13) 0.0065(12) 0.0026(13) F1 0.0590(13) 0.0432(12) 0.0408(11) 0.0046(9) 0.0041(10) -0.0122(10) F2 0.0666(14) 0.0510(13) 0.0393(11) -0.0167(10) -0.0021(10) 0.0069(11) F3 0.096(2) 0.0600(16) 0.0449(13) 0.0106(11) -0.0095(13) -0.0398(14) F4 0.0373(10) 0.0705(15) 0.0404(11) -0.0194(11) 0.0072(8) -0.0031(10) F5 0.0454(11) 0.0465(12) 0.0501(12) -0.0108(10) -0.0161(9) 0.0100(10) F6 0.0401(11) 0.0702(16) 0.0528(13) -0.0081(11) -0.0164(10) -0.0011(11) F7 0.194(4) 0.0381(14) 0.0693(18) -0.0010(13) 0.060(2) 0.0079(19) F8 0.0491(15) 0.147(3) 0.080(2) 0.044(2) -0.0203(14) -0.0250(18) F9 0.123(3) 0.0427(14) 0.083(2) 0.0035(13) 0.0532(19) 0.0155(15) F10 0.0480(14) 0.104(2) 0.0597(16) 0.0153(15) 0.0040(11) -0.0063(14) F11 0.096(2) 0.0692(17) 0.0310(11) 0.0154(11) -0.0079(12) -0.0029(15) F12 0.0730(16) 0.0620(15) 0.0318(10) 0.0039(10) 0.0108(10) -0.0067(12) P1 0.0338(4) 0.0343(4) 0.0274(4) -0.0016(3) -0.0028(3) -0.0044(3) P2 0.0374(4) 0.0323(4) 0.0279(4) -0.0002(3) 0.0020(3) 0.0028(3) Ni1 0.01903(17) 0.01914(17) 0.01999(17) 0.00072(12) 0.00062(12) -0.00025(12) O1 0.078(2) 0.0561(18) 0.0508(16) 0.0164(14) 0.0259(15) 0.0024(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.337(4) . ? C1 C2 1.391(4) . ? C1 H1 0.9500 . ? C2 C3 1.378(5) . ? C2 H2 0.9500 . ? C3 C4 1.378(5) . ? C3 H3 0.9500 . ? C4 C5 1.391(4) . ? C4 H4 0.9500 . ? C5 N1 1.352(4) . ? C5 C6 1.485(4) . ? C6 N2 1.337(4) . ? C6 C7 1.392(4) . ? C7 C8 1.387(5) . ? C7 H7 0.9500 . ? C8 C9 1.383(5) . ? C8 H8 0.9500 . ? C9 C10 1.389(4) . ? C9 H9 0.9500 . ? C10 N2 1.342(4) . ? C10 C11 1.486(4) . ? C11 N3 1.353(3) . ? C11 C12 1.392(4) . ? C12 C13 1.388(5) . ? C12 H12 0.9500 . ? C13 C14 1.377(5) . ? C13 H13 0.9500 . ? C14 C15 1.388(4) . ? C14 H14 0.9500 . ? C15 N3 1.333(4) . ? C15 H15 0.9500 . ? C16 N4 1.341(4) . ? C16 C17 1.388(5) . ? C16 H16 0.9500 . ? C17 C18 1.370(7) . ? C17 H17 0.9500 . ? C18 C19 1.387(7) . ? C18 H18 0.9500 . ? C19 C20 1.401(4) . ? C19 H19 0.9500 . ? C20 N4 1.352(4) . ? C20 C21 1.478(5) . ? C21 N5 1.345(4) . ? C21 C22 1.394(5) . ? C22 C23 1.377(6) . ? C22 H22 0.9500 . ? C23 C24 1.392(6) . ? C23 H23 0.9500 . ? C24 C25 1.385(4) . ? C24 H24 0.9500 . ? C25 N5 1.344(4) . ? C25 C26 1.487(4) . ? C26 N6 1.354(4) . ? C26 C27 1.390(4) . ? C27 C28 1.395(6) . ? C27 H27 0.9500 . ? C28 C29 1.381(5) . ? C28 H28 0.9500 . ? C29 C30 1.389(4) . ? C29 H29 0.9500 . ? C30 N6 1.341(4) . ? C30 H30 0.9500 . ? C31 O1 1.224(5) . ? C31 N7 1.328(5) . ? C31 H31 0.9500 . ? C32 N7 1.452(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N7 1.448(5) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? N1 Ni1 2.106(2) . ? N2 Ni1 1.991(2) . ? N3 Ni1 2.102(2) . ? N4 Ni1 2.100(2) . ? N5 Ni1 1.987(2) . ? N6 Ni1 2.119(2) . ? F1 P1 1.612(2) . ? F2 P1 1.592(2) . ? F3 P1 1.586(2) . ? F4 P1 1.602(2) . ? F5 P1 1.598(2) . ? F6 P1 1.595(2) . ? F7 P2 1.572(3) . ? F8 P2 1.574(3) . ? F9 P2 1.590(3) . ? F10 P2 1.596(3) . ? F11 P2 1.583(2) . ? F12 P2 1.608(2) . ? 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 N1 C1 C2 122.2(3) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 118.9(3) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 119.5(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 118.9(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 115.3(2) . . ? C4 C5 C6 122.9(3) . . ? N2 C6 C7 120.8(3) . . ? N2 C6 C5 113.2(2) . . ? C7 C6 C5 126.0(3) . . ? C8 C7 C6 118.2(3) . . ? C8 C7 H7 120.9 . . ? C6 C7 H7 120.9 . . ? C9 C8 C7 120.5(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 118.4(3) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N2 C10 C9 120.7(3) . . ? N2 C10 C11 113.3(2) . . ? C9 C10 C11 126.0(3) . . ? N3 C11 C12 121.5(3) . . ? N3 C11 C10 115.0(2) . . ? C12 C11 C10 123.5(3) . . ? C13 C12 C11 119.4(3) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 118.8(3) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 119.0(3) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? N3 C15 C14 122.8(3) . . ? N3 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? N4 C16 C17 122.0(4) . . ? N4 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C18 C17 C16 118.6(4) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C17 C18 C19 120.5(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C20 118.1(4) . . ? C18 C19 H19 120.9 . . ? C20 C19 H19 120.9 . . ? N4 C20 C19 121.2(3) . . ? N4 C20 C21 115.0(3) . . ? C19 C20 C21 123.8(3) . . ? N5 C21 C22 120.4(3) . . ? N5 C21 C20 113.7(3) . . ? C22 C21 C20 125.9(3) . . ? C23 C22 C21 117.9(4) . . ? C23 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? C22 C23 C24 121.4(3) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C25 C24 C23 118.0(4) . . ? C25 C24 H24 121.0 . . ? C23 C24 H24 121.0 . . ? N5 C25 C24 120.5(3) . . ? N5 C25 C26 113.5(2) . . ? C24 C25 C26 126.0(3) . . ? N6 C26 C27 121.3(3) . . ? N6 C26 C25 115.0(3) . . ? C27 C26 C25 123.7(3) . . ? C26 C27 C28 118.8(3) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C29 C28 C27 119.9(3) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 118.0(3) . . ? C28 C29 H29 121.0 . . ? C30 C29 H29 121.0 . . ? N6 C30 C29 122.8(3) . . ? N6 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? O1 C31 N7 125.8(4) . . ? O1 C31 H31 117.1 . . ? N7 C31 H31 117.1 . . ? N7 C32 H32A 109.5 . . ? N7 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N7 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N7 C33 H33A 109.5 . . ? N7 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N7 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C1 N1 C5 118.8(3) . . ? C1 N1 Ni1 127.6(2) . . ? C5 N1 Ni1 113.58(19) . . ? C6 N2 C10 121.4(2) . . ? C6 N2 Ni1 119.1(2) . . ? C10 N2 Ni1 119.10(19) . . ? C15 N3 C11 118.6(2) . . ? C15 N3 Ni1 127.41(19) . . ? C11 N3 Ni1 113.96(18) . . ? C16 N4 C20 119.6(3) . . ? C16 N4 Ni1 126.3(2) . . ? C20 N4 Ni1 113.8(2) . . ? C25 N5 C21 121.8(3) . . ? C25 N5 Ni1 119.4(2) . . ? C21 N5 Ni1 118.8(2) . . ? C30 N6 C26 119.2(2) . . ? C30 N6 Ni1 127.17(19) . . ? C26 N6 Ni1 113.62(19) . . ? C31 N7 C33 121.6(4) . . ? C31 N7 C32 120.2(3) . . ? C33 N7 C32 118.0(4) . . ? F3 P1 F2 90.88(15) . . ? F3 P1 F6 90.35(15) . . ? F2 P1 F6 89.36(13) . . ? F3 P1 F5 90.44(14) . . ? F2 P1 F5 90.93(12) . . ? F6 P1 F5 179.16(15) . . ? F3 P1 F4 90.75(14) . . ? F2 P1 F4 178.34(15) . . ? F6 P1 F4 90.35(13) . . ? F5 P1 F4 89.34(12) . . ? F3 P1 F1 179.17(14) . . ? F2 P1 F1 89.92(13) . . ? F6 P1 F1 89.86(14) . . ? F5 P1 F1 89.35(13) . . ? F4 P1 F1 88.45(13) . . ? F7 P2 F8 92.6(2) . . ? F7 P2 F11 90.82(16) . . ? F8 P2 F11 93.80(16) . . ? F7 P2 F9 175.0(2) . . ? F8 P2 F9 91.4(2) . . ? F11 P2 F9 91.97(16) . . ? F7 P2 F10 87.9(2) . . ? F8 P2 F10 177.74(16) . . ? F11 P2 F10 88.38(15) . . ? F9 P2 F10 87.98(19) . . ? F7 P2 F12 88.56(15) . . ? F8 P2 F12 87.57(15) . . ? F11 P2 F12 178.52(16) . . ? F9 P2 F12 88.54(15) . . ? F10 P2 F12 90.25(14) . . ? N5 Ni1 N2 176.72(10) . . ? N5 Ni1 N4 78.61(10) . . ? N2 Ni1 N4 104.55(10) . . ? N5 Ni1 N3 102.34(9) . . ? N2 Ni1 N3 78.45(9) . . ? N4 Ni1 N3 93.98(9) . . ? N5 Ni1 N1 100.87(9) . . ? N2 Ni1 N1 78.41(10) . . ? N4 Ni1 N1 90.12(9) . . ? N3 Ni1 N1 156.79(9) . . ? N5 Ni1 N6 78.37(10) . . ? N2 Ni1 N6 98.45(9) . . ? N4 Ni1 N6 156.94(10) . . ? N3 Ni1 N6 92.12(9) . . ? N1 Ni1 N6 92.97(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.3(5) . . . . ? C1 C2 C3 C4 -0.8(5) . . . . ? C2 C3 C4 C5 1.0(5) . . . . ? C3 C4 C5 N1 -0.2(4) . . . . ? C3 C4 C5 C6 -179.6(3) . . . . ? N1 C5 C6 N2 -3.5(4) . . . . ? C4 C5 C6 N2 175.9(3) . . . . ? N1 C5 C6 C7 175.8(3) . . . . ? C4 C5 C6 C7 -4.8(5) . . . . ? N2 C6 C7 C8 -0.1(5) . . . . ? C5 C6 C7 C8 -179.4(3) . . . . ? C6 C7 C8 C9 0.0(5) . . . . ? C7 C8 C9 C10 0.5(5) . . . . ? C8 C9 C10 N2 -1.0(5) . . . . ? C8 C9 C10 C11 177.5(3) . . . . ? N2 C10 C11 N3 4.1(3) . . . . ? C9 C10 C11 N3 -174.5(3) . . . . ? N2 C10 C11 C12 -176.1(3) . . . . ? C9 C10 C11 C12 5.4(5) . . . . ? N3 C11 C12 C13 0.6(5) . . . . ? C10 C11 C12 C13 -179.2(3) . . . . ? C11 C12 C13 C14 -0.4(5) . . . . ? C12 C13 C14 C15 -0.1(5) . . . . ? C13 C14 C15 N3 0.4(5) . . . . ? N4 C16 C17 C18 0.6(6) . . . . ? C16 C17 C18 C19 0.2(6) . . . . ? C17 C18 C19 C20 -0.9(6) . . . . ? C18 C19 C20 N4 1.0(5) . . . . ? C18 C19 C20 C21 -177.1(3) . . . . ? N4 C20 C21 N5 -2.8(4) . . . . ? C19 C20 C21 N5 175.3(3) . . . . ? N4 C20 C21 C22 178.3(3) . . . . ? C19 C20 C21 C22 -3.5(5) . . . . ? N5 C21 C22 C23 0.7(5) . . . . ? C20 C21 C22 C23 179.5(3) . . . . ? C21 C22 C23 C24 -1.1(6) . . . . ? C22 C23 C24 C25 0.7(6) . . . . ? C23 C24 C25 N5 0.2(5) . . . . ? C23 C24 C25 C26 -179.2(3) . . . . ? N5 C25 C26 N6 -1.4(4) . . . . ? C24 C25 C26 N6 178.1(3) . . . . ? N5 C25 C26 C27 178.3(3) . . . . ? C24 C25 C26 C27 -2.3(5) . . . . ? N6 C26 C27 C28 -0.3(5) . . . . ? C25 C26 C27 C28 -179.9(3) . . . . ? C26 C27 C28 C29 0.2(5) . . . . ? C27 C28 C29 C30 -0.4(5) . . . . ? C28 C29 C30 N6 0.8(5) . . . . ? C2 C1 N1 C5 1.1(4) . . . . ? C2 C1 N1 Ni1 -179.7(2) . . . . ? C4 C5 N1 C1 -0.9(4) . . . . ? C6 C5 N1 C1 178.6(2) . . . . ? C4 C5 N1 Ni1 179.8(2) . . . . ? C6 C5 N1 Ni1 -0.7(3) . . . . ? C7 C6 N2 C10 -0.3(4) . . . . ? C5 C6 N2 C10 179.1(2) . . . . ? C7 C6 N2 Ni1 -172.8(2) . . . . ? C5 C6 N2 Ni1 6.6(3) . . . . ? C9 C10 N2 C6 0.9(4) . . . . ? C11 C10 N2 C6 -177.8(2) . . . . ? C9 C10 N2 Ni1 173.4(2) . . . . ? C11 C10 N2 Ni1 -5.3(3) . . . . ? C14 C15 N3 C11 -0.1(4) . . . . ? C14 C15 N3 Ni1 -179.3(2) . . . . ? C12 C11 N3 C15 -0.4(4) . . . . ? C10 C11 N3 C15 179.4(2) . . . . ? C12 C11 N3 Ni1 178.9(2) . . . . ? C10 C11 N3 Ni1 -1.3(3) . . . . ? C17 C16 N4 C20 -0.6(5) . . . . ? C17 C16 N4 Ni1 173.3(3) . . . . ? C19 C20 N4 C16 -0.3(4) . . . . ? C21 C20 N4 C16 178.0(3) . . . . ? C19 C20 N4 Ni1 -174.8(2) . . . . ? C21 C20 N4 Ni1 3.4(3) . . . . ? C24 C25 N5 C21 -0.6(4) . . . . ? C26 C25 N5 C21 178.9(2) . . . . ? C24 C25 N5 Ni1 179.8(2) . . . . ? C26 C25 N5 Ni1 -0.7(3) . . . . ? C22 C21 N5 C25 0.1(4) . . . . ? C20 C21 N5 C25 -178.7(2) . . . . ? C22 C21 N5 Ni1 179.7(2) . . . . ? C20 C21 N5 Ni1 0.8(3) . . . . ? C29 C30 N6 C26 -0.9(4) . . . . ? C29 C30 N6 Ni1 176.4(2) . . . . ? C27 C26 N6 C30 0.7(4) . . . . ? C25 C26 N6 C30 -179.7(2) . . . . ? C27 C26 N6 Ni1 -177.0(2) . . . . ? C25 C26 N6 Ni1 2.6(3) . . . . ? O1 C31 N7 C33 177.2(5) . . . . ? O1 C31 N7 C32 1.5(7) . . . . ? C25 N5 Ni1 N4 -179.7(2) . . . . ? C21 N5 Ni1 N4 0.7(2) . . . . ? C25 N5 Ni1 N3 -88.1(2) . . . . ? C21 N5 Ni1 N3 92.4(2) . . . . ? C25 N5 Ni1 N1 92.4(2) . . . . ? C21 N5 Ni1 N1 -87.2(2) . . . . ? C25 N5 Ni1 N6 1.6(2) . . . . ? C21 N5 Ni1 N6 -178.0(2) . . . . ? C6 N2 Ni1 N4 -92.5(2) . . . . ? C10 N2 Ni1 N4 94.8(2) . . . . ? C6 N2 Ni1 N3 176.3(2) . . . . ? C10 N2 Ni1 N3 3.6(2) . . . . ? C6 N2 Ni1 N1 -5.5(2) . . . . ? C10 N2 Ni1 N1 -178.1(2) . . . . ? C6 N2 Ni1 N6 85.9(2) . . . . ? C10 N2 Ni1 N6 -86.8(2) . . . . ? C16 N4 Ni1 N5 -176.4(3) . . . . ? C20 N4 Ni1 N5 -2.3(2) . . . . ? C16 N4 Ni1 N2 2.7(3) . . . . ? C20 N4 Ni1 N2 176.8(2) . . . . ? C16 N4 Ni1 N3 81.8(3) . . . . ? C20 N4 Ni1 N3 -104.1(2) . . . . ? C16 N4 Ni1 N1 -75.4(3) . . . . ? C20 N4 Ni1 N1 98.8(2) . . . . ? C16 N4 Ni1 N6 -173.3(2) . . . . ? C20 N4 Ni1 N6 0.8(4) . . . . ? C15 N3 Ni1 N5 -5.1(2) . . . . ? C11 N3 Ni1 N5 175.66(18) . . . . ? C15 N3 Ni1 N2 178.1(2) . . . . ? C11 N3 Ni1 N2 -1.08(18) . . . . ? C15 N3 Ni1 N4 74.1(2) . . . . ? C11 N3 Ni1 N4 -105.14(19) . . . . ? C15 N3 Ni1 N1 173.8(2) . . . . ? C11 N3 Ni1 N1 -5.5(3) . . . . ? C15 N3 Ni1 N6 -83.7(2) . . . . ? C11 N3 Ni1 N6 97.11(19) . . . . ? C1 N1 Ni1 N5 7.2(2) . . . . ? C5 N1 Ni1 N5 -173.62(19) . . . . ? C1 N1 Ni1 N2 -176.1(2) . . . . ? C5 N1 Ni1 N2 3.12(18) . . . . ? C1 N1 Ni1 N4 -71.3(2) . . . . ? C5 N1 Ni1 N4 107.96(19) . . . . ? C1 N1 Ni1 N3 -171.7(2) . . . . ? C5 N1 Ni1 N3 7.5(3) . . . . ? C1 N1 Ni1 N6 85.9(2) . . . . ? C5 N1 Ni1 N6 -94.90(19) . . . . ? C30 N6 Ni1 N5 -179.7(2) . . . . ? C26 N6 Ni1 N5 -2.26(19) . . . . ? C30 N6 Ni1 N2 1.1(2) . . . . ? C26 N6 Ni1 N2 178.53(19) . . . . ? C30 N6 Ni1 N4 177.1(2) . . . . ? C26 N6 Ni1 N4 -5.4(4) . . . . ? C30 N6 Ni1 N3 -77.6(2) . . . . ? C26 N6 Ni1 N3 99.90(19) . . . . ? C30 N6 Ni1 N1 79.8(2) . . . . ? C26 N6 Ni1 N1 -102.75(19) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.727 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.085 data_jcm20_crystal2 _database_code_depnum_ccdc_archive 'CCDC 260309' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 N6 Ni, (P F6)2, C3 H6 O' _chemical_formula_sum 'C33 H28 F12 N6 Ni O P2' _chemical_formula_weight 873.26 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.7687(17) _cell_length_b 8.9641(18) _cell_length_c 44.959(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3533.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 982 _cell_measurement_theta_min 2.691 _cell_measurement_theta_max 27.583 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour orange _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 0.742 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 0.881 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 445 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.13 _diffrn_reflns_number 30804 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -57 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8183 _reflns_number_gt 7979 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT and XPREP (Siemens, 1995)' _computing_structure_solution 'SIR97 (Altomare, et. al. 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;ORTEP-3 (Farrugia, 1997) WINGX-32 (Farrugia, 1999) ; _computing_publication_material 'enCIFer 1.0 (CCDC, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+15.6632P] 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 0.26(2) _chemical_absolute_configuration ad _refine_ls_number_reflns 8183 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.1816 _refine_ls_wR_factor_gt 0.1807 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.88946(7) 0.26479(6) 0.638039(13) 0.01683(14) Uani 1 1 d . . . P1A P 0.4278(4) 0.1284(4) 0.54958(7) 0.0356(4) Uiso 0.50 1 d PG A 1 F1A F 0.5354(6) 0.1803(6) 0.52303(10) 0.0563(7) Uiso 0.50 1 d PG A 1 F2A F 0.5632(7) 0.0252(6) 0.56229(14) 0.0563(7) Uiso 0.50 1 d PG A 1 F3A F 0.3693(7) -0.0092(5) 0.53025(12) 0.0563(7) Uiso 0.50 1 d PG A 1 F4A F 0.4900(6) 0.2638(6) 0.56942(11) 0.0563(7) Uiso 0.50 1 d PG A 1 F5A F 0.2955(5) 0.2310(6) 0.53700(13) 0.0563(7) Uiso 0.50 1 d PG A 1 F6A F 0.3224(7) 0.0741(7) 0.57648(10) 0.0563(7) Uiso 0.50 1 d PG A 1 P1B P 0.4370(4) 0.1067(4) 0.54767(7) 0.0356(4) Uiso 0.50 1 d PG B 2 F1B F 0.2952(5) 0.1709(6) 0.52970(13) 0.0563(7) Uiso 0.50 1 d PG B 2 F2B F 0.3796(7) -0.0606(4) 0.54091(13) 0.0563(7) Uiso 0.50 1 d PG B 2 F3B F 0.3391(7) 0.1059(7) 0.57752(10) 0.0563(7) Uiso 0.50 1 d PG B 2 F4B F 0.5343(6) 0.1028(7) 0.51753(10) 0.0563(7) Uiso 0.50 1 d PG B 2 F5B F 0.4931(6) 0.2717(4) 0.55406(12) 0.0563(7) Uiso 0.50 1 d PG B 2 F6B F 0.5782(6) 0.0388(7) 0.56561(13) 0.0563(7) Uiso 0.50 1 d PG B 2 P2A P 0.6711(5) 0.7497(5) 0.71817(10) 0.0318(4) Uiso 0.35 1 d PG C 1 F7A F 0.8097(7) 0.6608(7) 0.70378(16) 0.0423(7) Uiso 0.35 1 d PG C 1 F8A F 0.7729(7) 0.8992(6) 0.71851(17) 0.0423(7) Uiso 0.35 1 d PG C 1 F9A F 0.7319(8) 0.7110(9) 0.75066(11) 0.0423(7) Uiso 0.35 1 d PG C 1 F10A F 0.6122(8) 0.7928(8) 0.68556(11) 0.0423(7) Uiso 0.35 1 d PG C 1 F11A F 0.5714(8) 0.6023(6) 0.71758(16) 0.0423(7) Uiso 0.35 1 d PG C 1 F12A F 0.5339(7) 0.8419(8) 0.73265(16) 0.0423(7) Uiso 0.35 1 d PG C 1 P2B P 0.6726(5) 0.7681(5) 0.71542(11) 0.0318(4) Uiso 0.35 1 d PG D 2 F7B F 0.6851(10) 0.7152(9) 0.74912(12) 0.0423(7) Uiso 0.35 1 d PG D 2 F8B F 0.6082(9) 0.6061(6) 0.70634(19) 0.0423(7) Uiso 0.35 1 d PG D 2 F9B F 0.8413(6) 0.7101(9) 0.7091(2) 0.0423(7) Uiso 0.35 1 d PG D 2 F10B F 0.5013(6) 0.8222(8) 0.72141(18) 0.0423(7) Uiso 0.35 1 d PG D 2 F11B F 0.7352(9) 0.9274(6) 0.72460(19) 0.0423(7) Uiso 0.35 1 d PG D 2 F12B F 0.6590(10) 0.8179(9) 0.68139(12) 0.0423(7) Uiso 0.35 1 d PG D 2 P2C P 0.6773(6) 0.7606(6) 0.71793(13) 0.0318(4) Uiso 0.30 1 d PG E 3 F7C F 0.7044(11) 0.6872(10) 0.74972(15) 0.0423(7) Uiso 0.30 1 d PG E 3 F8C F 0.6682(10) 0.5968(7) 0.7033(2) 0.0423(7) Uiso 0.30 1 d PG E 3 F9C F 0.8564(6) 0.7619(11) 0.7119(2) 0.0423(7) Uiso 0.30 1 d PG E 3 F10C F 0.4970(6) 0.7551(11) 0.7235(2) 0.0423(7) Uiso 0.30 1 d PG E 3 F11C F 0.6854(11) 0.9213(7) 0.7325(2) 0.0423(7) Uiso 0.30 1 d PG E 3 F12C F 0.6501(11) 0.8310(10) 0.68571(14) 0.0423(7) Uiso 0.30 1 d PG E 3 N1 N 0.8068(5) 0.4648(5) 0.61927(10) 0.0218(9) Uani 1 1 d . . . N2 N 0.9000(5) 0.2184(5) 0.59488(9) 0.0213(8) Uani 1 1 d . . . N3 N 0.9736(4) 0.0448(5) 0.63842(10) 0.0198(8) Uani 1 1 d . . . N4 N 1.1124(5) 0.3550(5) 0.64374(9) 0.0234(8) Uani 1 1 d . . . N5 N 0.8920(5) 0.3129(5) 0.68141(9) 0.0198(8) Uani 1 1 d . . . N6 N 0.6715(5) 0.1882(5) 0.65148(10) 0.0228(9) Uani 1 1 d . . . C1 C 0.7568(6) 0.5860(6) 0.63284(13) 0.0242(11) Uani 1 1 d . . . H1 H 0.7628 0.5902 0.6539 0.029 Uiso 1 1 calc R . . C2 C 0.6960(7) 0.7073(7) 0.61791(14) 0.0327(13) Uani 1 1 d . . . H2 H 0.6605 0.7919 0.6286 0.039 Uiso 1 1 calc R . . C3 C 0.6879(8) 0.7032(7) 0.58758(15) 0.0362(14) Uani 1 1 d . . . H3 H 0.6469 0.7855 0.5769 0.043 Uiso 1 1 calc R . . C4 C 0.7390(7) 0.5798(7) 0.57250(14) 0.0326(13) Uani 1 1 d . . . H4 H 0.7340 0.5757 0.5514 0.039 Uiso 1 1 calc R . . C5 C 0.7988(6) 0.4600(6) 0.58882(12) 0.0239(11) Uani 1 1 d . . . C6 C 0.8587(6) 0.3213(6) 0.57520(12) 0.0234(11) Uani 1 1 d . . . C7 C 0.8755(7) 0.2977(7) 0.54453(12) 0.0309(12) Uani 1 1 d . . . H7 H 0.8477 0.3723 0.5305 0.037 Uiso 1 1 calc R . . C8 C 0.9338(7) 0.1621(7) 0.53543(13) 0.0339(13) Uani 1 1 d . . . H8 H 0.9465 0.1426 0.5148 0.041 Uiso 1 1 calc R . . C9 C 0.9740(7) 0.0543(7) 0.55596(13) 0.0311(13) Uani 1 1 d . . . H9 H 1.0114 -0.0400 0.5497 0.037 Uiso 1 1 calc R . . C10 C 0.9582(5) 0.0874(6) 0.58632(11) 0.0213(10) Uani 1 1 d . . . C11 C 1.0023(6) -0.0108(6) 0.61108(12) 0.0213(10) Uani 1 1 d . . . C12 C 1.0678(7) -0.1519(7) 0.60686(13) 0.0296(12) Uani 1 1 d . . . H12 H 1.0883 -0.1889 0.5875 0.035 Uiso 1 1 calc R . . C13 C 1.1020(7) -0.2361(6) 0.63217(13) 0.0345(12) Uani 1 1 d . . . H13 H 1.1466 -0.3322 0.6302 0.041 Uiso 1 1 calc R . . C14 C 1.0705(7) -0.1791(7) 0.66032(14) 0.0321(13) Uani 1 1 d . . . H14 H 1.0927 -0.2349 0.6778 0.038 Uiso 1 1 calc R . . C15 C 1.0057(7) -0.0381(7) 0.66209(13) 0.0284(12) Uani 1 1 d . . . H15 H 0.9831 0.0011 0.6812 0.034 Uiso 1 1 calc R . . C16 C 1.2217(6) 0.3703(6) 0.62277(13) 0.0267(11) Uani 1 1 d . . . H16 H 1.2017 0.3348 0.6033 0.032 Uiso 1 1 calc R . . C17 C 1.3621(6) 0.4358(6) 0.62855(15) 0.0310(13) Uani 1 1 d . . . H17 H 1.4374 0.4445 0.6135 0.037 Uiso 1 1 calc R . . C18 C 1.3887(7) 0.4886(7) 0.65745(16) 0.0388(14) Uani 1 1 d . . . H18 H 1.4814 0.5384 0.6620 0.047 Uiso 1 1 calc R . . C19 C 1.2801(7) 0.4682(7) 0.67913(16) 0.0341(14) Uani 1 1 d . . . H19 H 1.2989 0.4996 0.6990 0.041 Uiso 1 1 calc R . . C20 C 1.1413(6) 0.4006(7) 0.67156(13) 0.0280(12) Uani 1 1 d . . . C21 C 1.0169(6) 0.3736(7) 0.69360(12) 0.0266(11) Uani 1 1 d . . . C22 C 1.0248(8) 0.4054(9) 0.72373(14) 0.0418(16) Uani 1 1 d . . . H22 H 1.1132 0.4496 0.7322 0.050 Uiso 1 1 calc R . . C23 C 0.8995(9) 0.3704(9) 0.74101(13) 0.0472(17) Uani 1 1 d . . . H23 H 0.9013 0.3928 0.7617 0.057 Uiso 1 1 calc R . . C24 C 0.7708(8) 0.3034(8) 0.72891(14) 0.0397(15) Uani 1 1 d . . . H24 H 0.6857 0.2777 0.7409 0.048 Uiso 1 1 calc R . . C25 C 0.7716(6) 0.2750(7) 0.69808(12) 0.0278(11) Uani 1 1 d . . . C26 C 0.6465(6) 0.2061(6) 0.68124(12) 0.0249(11) Uani 1 1 d . . . C27 C 0.5140(7) 0.1587(8) 0.69477(15) 0.0376(15) Uani 1 1 d . . . H27 H 0.4975 0.1733 0.7154 0.045 Uiso 1 1 calc R . . C28 C 0.4053(7) 0.0889(8) 0.67708(18) 0.0470(18) Uani 1 1 d . . . H28 H 0.3133 0.0539 0.6858 0.056 Uiso 1 1 calc R . . C29 C 0.4295(6) 0.0701(7) 0.64731(16) 0.0352(15) Uani 1 1 d . . . H29 H 0.3552 0.0225 0.6352 0.042 Uiso 1 1 calc R . . C30 C 0.5679(6) 0.1232(6) 0.63482(14) 0.0289(11) Uani 1 1 d . . . H30 H 0.5860 0.1115 0.6141 0.035 Uiso 1 1 calc R . . O1A O 0.5572(12) -0.2037(13) 0.4608(3) 0.0474(11) Uiso 0.50 1 d PG F 1 C32A C 0.6689(10) -0.1648(9) 0.47413(19) 0.0474(11) Uiso 0.50 1 d PG F 1 C33A C 0.7747(14) -0.0529(14) 0.4617(3) 0.0474(11) Uiso 0.50 1 d PG F 1 C31A C 0.7037(16) -0.2262(16) 0.5041(2) 0.0474(11) Uiso 0.50 1 d PG F 1 H31A H 0.6317 -0.3043 0.5086 0.057 Uiso 0.50 1 d PG F 1 H31B H 0.8052 -0.2667 0.5039 0.057 Uiso 0.50 1 d PG F 1 H31C H 0.6972 -0.1447 0.5210 0.057 Uiso 0.50 1 d PG F 1 H33A H 0.8676 -0.0890 0.4587 0.057 Uiso 0.50 1 d PG F 1 H33B H 0.7812 0.0289 0.4753 0.057 Uiso 0.50 1 d PG F 1 H33C H 0.7348 -0.0187 0.4431 0.057 Uiso 0.50 1 d PG F 1 O1B O 0.5578(11) -0.1720(14) 0.4583(3) 0.0474(11) Uiso 0.50 1 d PG G 2 C32B C 0.6805(10) -0.1522(9) 0.46951(19) 0.0474(11) Uiso 0.50 1 d PG G 2 C33B C 0.8134(12) -0.1056(17) 0.4516(3) 0.0474(11) Uiso 0.50 1 d PG G 2 C31B C 0.7028(16) -0.1711(17) 0.50212(19) 0.0474(11) Uiso 0.50 1 d PG G 2 H31D H 0.6103 -0.2108 0.5106 0.057 Uiso 0.50 1 d PG G 2 H31E H 0.7851 -0.2401 0.5053 0.057 Uiso 0.50 1 d PG G 2 H31F H 0.7290 -0.0700 0.5129 0.057 Uiso 0.50 1 d PG G 2 H33D H 0.8882 -0.1721 0.4519 0.057 Uiso 0.50 1 d PG G 2 H33E H 0.8511 -0.0133 0.4595 0.057 Uiso 0.50 1 d PG G 2 H33F H 0.7810 -0.0914 0.4315 0.057 Uiso 0.50 1 d PG G 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0142(2) 0.0177(3) 0.0186(3) 0.0008(2) -0.0002(2) 0.0020(2) N1 0.0134(19) 0.026(2) 0.026(2) 0.0027(18) -0.0032(16) 0.0009(17) N2 0.0149(17) 0.026(2) 0.0227(19) 0.0002(16) 0.0008(16) -0.0031(18) N3 0.0138(18) 0.0242(19) 0.0213(19) 0.0036(19) 0.0010(16) 0.0013(15) N4 0.0172(19) 0.024(2) 0.029(2) -0.0009(16) -0.0004(18) 0.0022(17) N5 0.0174(19) 0.023(2) 0.0186(18) 0.0023(15) -0.0003(17) 0.0085(18) N6 0.019(2) 0.025(2) 0.025(2) 0.0081(17) -0.0013(17) 0.0041(17) C1 0.016(2) 0.025(3) 0.032(3) 0.002(2) 0.000(2) 0.0010(19) C2 0.033(3) 0.026(3) 0.039(3) 0.002(2) 0.002(2) 0.006(2) C3 0.038(3) 0.027(3) 0.044(3) 0.012(3) -0.002(3) 0.014(3) C4 0.030(3) 0.038(3) 0.029(3) 0.011(3) -0.003(2) 0.008(3) C5 0.017(2) 0.025(3) 0.030(3) 0.005(2) 0.002(2) 0.000(2) C6 0.018(3) 0.027(2) 0.025(2) 0.002(2) -0.0016(19) -0.0048(19) C7 0.027(3) 0.047(3) 0.019(2) 0.007(2) 0.003(2) 0.002(3) C8 0.036(3) 0.043(3) 0.023(3) -0.003(2) 0.005(2) 0.000(3) C9 0.026(3) 0.039(3) 0.028(3) -0.008(2) 0.000(2) 0.001(2) C10 0.012(2) 0.028(3) 0.024(2) -0.002(2) 0.0030(18) -0.0019(19) C11 0.013(2) 0.027(3) 0.024(2) -0.002(2) 0.0019(18) -0.0018(19) C12 0.025(3) 0.029(3) 0.035(3) -0.001(2) 0.006(2) 0.004(2) C13 0.038(3) 0.021(2) 0.045(3) 0.001(2) 0.001(3) 0.009(3) C14 0.032(3) 0.031(3) 0.033(3) 0.009(2) -0.005(2) 0.006(2) C15 0.029(3) 0.029(3) 0.027(3) 0.002(2) 0.004(2) 0.000(2) C16 0.025(3) 0.021(3) 0.034(3) 0.002(2) 0.001(2) 0.004(2) C17 0.019(3) 0.023(3) 0.051(4) 0.004(2) 0.010(2) 0.003(2) C18 0.018(3) 0.031(3) 0.067(4) -0.008(3) -0.006(3) 0.002(3) C19 0.022(3) 0.032(3) 0.048(4) -0.001(3) -0.015(3) -0.002(2) C20 0.016(2) 0.034(3) 0.035(3) 0.001(2) -0.008(2) 0.006(2) C21 0.022(3) 0.033(3) 0.025(3) -0.004(2) -0.006(2) 0.004(2) C22 0.041(4) 0.059(4) 0.026(3) -0.013(3) -0.014(3) 0.010(3) C23 0.057(4) 0.067(5) 0.018(3) 0.004(3) -0.005(3) 0.003(4) C24 0.042(4) 0.048(4) 0.030(3) 0.010(3) 0.012(3) 0.005(3) C25 0.022(2) 0.028(3) 0.034(3) 0.007(2) 0.005(2) 0.009(2) C26 0.019(2) 0.030(3) 0.027(2) 0.004(2) 0.0044(19) 0.0070(19) C27 0.025(3) 0.048(4) 0.040(3) 0.014(3) 0.009(3) 0.007(3) C28 0.019(3) 0.048(4) 0.075(5) 0.024(4) 0.010(3) -0.001(3) C29 0.012(2) 0.030(3) 0.063(4) 0.009(3) -0.008(2) 0.000(2) C30 0.019(2) 0.030(3) 0.038(3) 0.006(2) -0.004(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.987(4) . ? Ni1 N5 1.997(4) . ? Ni1 N3 2.106(4) . ? Ni1 N1 2.110(5) . ? Ni1 N6 2.119(5) . ? Ni1 N4 2.131(5) . ? P1A F5A 1.5848 . ? P1A F1A 1.5912 . ? P1A F3A 1.5934 . ? P1A F6A 1.5979 . ? P1A F4A 1.6015 . ? P1A F2A 1.6101 . ? P1B F5B 1.5848 . ? P1B F1B 1.5912 . ? P1B F3B 1.5933 . ? P1B F6B 1.5980 . ? P1B F4B 1.6016 . ? P1B F2B 1.6102 . ? P2A F11A 1.5847 . ? P2A F7A 1.5910 . ? P2A F9A 1.5934 . ? P2A F12A 1.5981 . ? P2A F10A 1.6016 . ? P2A F8A 1.6102 . ? P2B F11B 1.5848 . ? P2B F7B 1.5911 . ? P2B F9B 1.5933 . ? P2B F12B 1.5982 . ? P2B F10B 1.6016 . ? P2B F8B 1.6102 . ? P2C F11C 1.5848 . ? P2C F7C 1.5912 . ? P2C F9C 1.5933 . ? P2C F12C 1.5981 . ? P2C F10C 1.6016 . ? P2C F8C 1.6102 . ? N1 C1 1.322(7) . ? N1 C5 1.371(7) . ? N2 C6 1.329(7) . ? N2 C10 1.337(7) . ? N3 C15 1.328(7) . ? N3 C11 1.350(7) . ? N4 C20 1.340(7) . ? N4 C16 1.352(7) . ? N5 C25 1.339(7) . ? N5 C21 1.339(7) . ? N6 C30 1.313(7) . ? N6 C26 1.365(7) . ? C1 C2 1.384(8) . ? C1 H1 0.9500 . ? C2 C3 1.366(9) . ? C2 H2 0.9500 . ? C3 C4 1.372(9) . ? C3 H3 0.9500 . ? C4 C5 1.402(8) . ? C4 H4 0.9500 . ? C5 C6 1.482(8) . ? C6 C7 1.403(7) . ? C7 C8 1.381(9) . ? C7 H7 0.9500 . ? C8 C9 1.382(9) . ? C8 H8 0.9500 . ? C9 C10 1.404(7) . ? C9 H9 0.9500 . ? C10 C11 1.471(7) . ? C11 C12 1.402(8) . ? C12 C13 1.398(8) . ? C12 H12 0.9500 . ? C13 C14 1.393(8) . ? C13 H13 0.9500 . ? C14 C15 1.388(8) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.388(8) . ? C16 H16 0.9500 . ? C17 C18 1.402(9) . ? C17 H17 0.9500 . ? C18 C19 1.375(10) . ? C18 H18 0.9500 . ? C19 C20 1.402(8) . ? C19 H19 0.9500 . ? C20 C21 1.494(8) . ? C21 C22 1.386(8) . ? C22 C23 1.382(10) . ? C22 H22 0.9500 . ? C23 C24 1.389(11) . ? C23 H23 0.9500 . ? C24 C25 1.409(9) . ? C24 H24 0.9500 . ? C25 C26 1.469(8) . ? C26 C27 1.379(8) . ? C27 C28 1.390(10) . ? C27 H27 0.9500 . ? C28 C29 1.366(10) . ? C28 H28 0.9500 . ? C29 C30 1.420(8) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? O1A C32A 1.2008 . ? C32A C33A 1.4757 . ? C32A C31A 1.4890 . ? C33A H33A 0.8866 . ? C33A H33B 0.9572 . ? C33A H33C 0.9593 . ? C31A H31A 0.9640 . ? C31A H31B 0.9613 . ? C31A H31C 1.0533 . ? O1B C32B 1.2009 . ? C32B C33B 1.4758 . ? C32B C31B 1.4889 . ? C33B H33D 0.8866 . ? C33B H33E 0.9572 . ? C33B H33F 0.9593 . ? C31B H31D 0.9641 . ? C31B H31E 0.9613 . ? C31B H31F 1.0534 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N5 176.68(19) . . ? N2 Ni1 N3 78.21(18) . . ? N5 Ni1 N3 100.97(17) . . ? N2 Ni1 N1 78.65(18) . . ? N5 Ni1 N1 102.17(17) . . ? N3 Ni1 N1 156.85(18) . . ? N2 Ni1 N6 104.62(18) . . ? N5 Ni1 N6 78.57(18) . . ? N3 Ni1 N6 90.59(16) . . ? N1 Ni1 N6 94.56(17) . . ? N2 Ni1 N4 98.88(17) . . ? N5 Ni1 N4 77.89(18) . . ? N3 Ni1 N4 91.88(16) . . ? N1 Ni1 N4 92.34(17) . . ? N6 Ni1 N4 156.37(17) . . ? F5A P1A F1A 89.8 . . ? F5A P1A F3A 91.1 . . ? F1A P1A F3A 90.4 . . ? F5A P1A F6A 91.3 . . ? F1A P1A F6A 178.9 . . ? F3A P1A F6A 89.5 . . ? F5A P1A F4A 90.5 . . ? F1A P1A F4A 89.7 . . ? F3A P1A F4A 178.5 . . ? F6A P1A F4A 90.3 . . ? F5A P1A F2A 179.5 . . ? F1A P1A F2A 89.8 . . ? F3A P1A F2A 89.2 . . ? F6A P1A F2A 89.0 . . ? F4A P1A F2A 89.2 . . ? F5B P1B F1B 89.8 . . ? F5B P1B F3B 91.1 . . ? F1B P1B F3B 90.5 . . ? F5B P1B F6B 91.3 . . ? F1B P1B F6B 178.9 . . ? F3B P1B F6B 89.5 . . ? F5B P1B F4B 90.5 . . ? F1B P1B F4B 89.7 . . ? F3B P1B F4B 178.5 . . ? F6B P1B F4B 90.3 . . ? F5B P1B F2B 179.5 . . ? F1B P1B F2B 89.8 . . ? F3B P1B F2B 89.2 . . ? F6B P1B F2B 89.0 . . ? F4B P1B F2B 89.2 . . ? F11A P2A F7A 89.8 . . ? F11A P2A F9A 91.1 . . ? F7A P2A F9A 90.5 . . ? F11A P2A F12A 91.3 . . ? F7A P2A F12A 178.9 . . ? F9A P2A F12A 89.5 . . ? F11A P2A F10A 90.5 . . ? F7A P2A F10A 89.7 . . ? F9A P2A F10A 178.5 . . ? F12A P2A F10A 90.3 . . ? F11A P2A F8A 179.5 . . ? F7A P2A F8A 89.8 . . ? F9A P2A F8A 89.2 . . ? F12A P2A F8A 89.0 . . ? F10A P2A F8A 89.2 . . ? F11B P2B F7B 89.8 . . ? F11B P2B F9B 91.1 . . ? F7B P2B F9B 90.5 . . ? F11B P2B F12B 91.3 . . ? F7B P2B F12B 178.9 . . ? F9B P2B F12B 89.5 . . ? F11B P2B F10B 90.5 . . ? F7B P2B F10B 89.7 . . ? F9B P2B F10B 178.5 . . ? F12B P2B F10B 90.3 . . ? F11B P2B F8B 179.5 . . ? F7B P2B F8B 89.8 . . ? F9B P2B F8B 89.2 . . ? F12B P2B F8B 89.0 . . ? F10B P2B F8B 89.2 . . ? F11C P2C F7C 89.8 . . ? F11C P2C F9C 91.1 . . ? F7C P2C F9C 90.5 . . ? F11C P2C F12C 91.3 . . ? F7C P2C F12C 178.9 . . ? F9C P2C F12C 89.5 . . ? F11C P2C F10C 90.5 . . ? F7C P2C F10C 89.7 . . ? F9C P2C F10C 178.5 . . ? F12C P2C F10C 90.3 . . ? F11C P2C F8C 179.5 . . ? F7C P2C F8C 89.8 . . ? F9C P2C F8C 89.2 . . ? F12C P2C F8C 89.0 . . ? F10C P2C F8C 89.2 . . ? C1 N1 C5 118.0(5) . . ? C1 N1 Ni1 128.9(4) . . ? C5 N1 Ni1 113.0(4) . . ? C6 N2 C10 121.5(4) . . ? C6 N2 Ni1 119.5(4) . . ? C10 N2 Ni1 118.9(3) . . ? C15 N3 C11 118.9(5) . . ? C15 N3 Ni1 127.2(4) . . ? C11 N3 Ni1 113.8(3) . . ? C20 N4 C16 119.0(5) . . ? C20 N4 Ni1 113.7(4) . . ? C16 N4 Ni1 127.3(4) . . ? C25 N5 C21 121.2(5) . . ? C25 N5 Ni1 118.9(4) . . ? C21 N5 Ni1 119.8(4) . . ? C30 N6 C26 120.0(5) . . ? C30 N6 Ni1 127.2(4) . . ? C26 N6 Ni1 112.7(4) . . ? N1 C1 C2 123.3(5) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 118.9(6) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 119.9(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 118.7(6) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 121.2(5) . . ? N1 C5 C6 114.9(5) . . ? C4 C5 C6 124.0(5) . . ? N2 C6 C7 121.4(5) . . ? N2 C6 C5 113.8(5) . . ? C7 C6 C5 124.8(5) . . ? C8 C7 C6 117.6(5) . . ? C8 C7 H7 121.2 . . ? C6 C7 H7 121.2 . . ? C7 C8 C9 120.8(5) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C8 C9 C10 118.5(6) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N2 C10 C9 120.2(5) . . ? N2 C10 C11 114.1(4) . . ? C9 C10 C11 125.7(5) . . ? N3 C11 C12 122.2(5) . . ? N3 C11 C10 114.8(5) . . ? C12 C11 C10 123.0(5) . . ? C13 C12 C11 117.7(5) . . ? C13 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? C14 C13 C12 119.9(5) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 117.9(5) . . ? C15 C14 H14 121.1 . . ? C13 C14 H14 121.1 . . ? N3 C15 C14 123.4(5) . . ? N3 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? N4 C16 C17 122.8(6) . . ? N4 C16 H16 118.6 . . ? C17 C16 H16 118.6 . . ? C16 C17 C18 117.6(6) . . ? C16 C17 H17 121.2 . . ? C18 C17 H17 121.2 . . ? C19 C18 C17 119.8(6) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 119.1(6) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? N4 C20 C19 121.6(6) . . ? N4 C20 C21 115.5(5) . . ? C19 C20 C21 122.9(6) . . ? N5 C21 C22 121.6(6) . . ? N5 C21 C20 113.0(5) . . ? C22 C21 C20 125.3(6) . . ? C23 C22 C21 117.6(6) . . ? C23 C22 H22 121.2 . . ? C21 C22 H22 121.2 . . ? C22 C23 C24 121.6(6) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C23 C24 C25 117.3(6) . . ? C23 C24 H24 121.3 . . ? C25 C24 H24 121.3 . . ? N5 C25 C24 120.6(6) . . ? N5 C25 C26 114.0(5) . . ? C24 C25 C26 125.4(5) . . ? N6 C26 C27 122.1(6) . . ? N6 C26 C25 115.8(5) . . ? C27 C26 C25 122.1(5) . . ? C26 C27 C28 117.7(6) . . ? C26 C27 H27 121.2 . . ? C28 C27 H27 121.2 . . ? C29 C28 C27 120.6(6) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 118.6(6) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? N6 C30 C29 121.0(6) . . ? N6 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? O1A C32A C33A 121.4 . . ? O1A C32A C31A 120.9 . . ? C33A C32A C31A 117.7 . . ? H33D C33A H33E 73.5 . . ? H33D C33A H33F 61.4 . . ? H33E C33A H33F 87.2 . . ? H31D C31A H31E 156.6 . . ? H31D C31A H31F 84.4 . . ? H31E C31A H31F 89.8 . . ? O1B C32B C33B 121.4 . . ? O1B C32B C31B 120.9 . . ? C33B C32B C31B 117.7 . . ? C32B C33B H33A 114.4 . . ? C32B C33B H33C 84.1 . . ? C32B C33B H33D 112.8 . . ? C32B C33B H33E 108.5 . . ? H33D C33B H33E 108.8 . . ? C32B C33B H33F 108.6 . . ? H33D C33B H33F 108.6 . . ? H33E C33B H33F 109.6 . . ? C32B C31B H31A 104.3 . . ? C32B C31B H31B 103.7 . . ? C32B C31B H31C 155.4 . . ? C32B C31B H31D 108.8 . . ? C32B C31B H31E 108.6 . . ? H31D C31B H31E 109.6 . . ? C32B C31B H31F 112.6 . . ? H31D C31B H31F 108.6 . . ? H31E C31B H31F 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N1 C1 178.0(5) . . . . ? N5 Ni1 N1 C1 -5.3(5) . . . . ? N3 Ni1 N1 C1 176.2(4) . . . . ? N6 Ni1 N1 C1 73.9(5) . . . . ? N4 Ni1 N1 C1 -83.4(5) . . . . ? N2 Ni1 N1 C5 1.6(4) . . . . ? N5 Ni1 N1 C5 178.3(4) . . . . ? N3 Ni1 N1 C5 -0.1(6) . . . . ? N6 Ni1 N1 C5 -102.4(4) . . . . ? N4 Ni1 N1 C5 100.2(4) . . . . ? N3 Ni1 N2 C6 -179.4(4) . . . . ? N1 Ni1 N2 C6 1.3(4) . . . . ? N6 Ni1 N2 C6 93.1(4) . . . . ? N4 Ni1 N2 C6 -89.4(4) . . . . ? N3 Ni1 N2 C10 -3.9(4) . . . . ? N1 Ni1 N2 C10 176.8(4) . . . . ? N6 Ni1 N2 C10 -91.4(4) . . . . ? N4 Ni1 N2 C10 86.2(4) . . . . ? N2 Ni1 N3 C15 -178.4(5) . . . . ? N5 Ni1 N3 C15 4.9(5) . . . . ? N1 Ni1 N3 C15 -176.7(4) . . . . ? N6 Ni1 N3 C15 -73.6(5) . . . . ? N4 Ni1 N3 C15 82.9(5) . . . . ? N2 Ni1 N3 C11 4.6(3) . . . . ? N5 Ni1 N3 C11 -172.1(3) . . . . ? N1 Ni1 N3 C11 6.3(6) . . . . ? N6 Ni1 N3 C11 109.4(4) . . . . ? N4 Ni1 N3 C11 -94.1(4) . . . . ? N2 Ni1 N4 C20 179.1(4) . . . . ? N5 Ni1 N4 C20 -1.7(4) . . . . ? N3 Ni1 N4 C20 -102.5(4) . . . . ? N1 Ni1 N4 C20 100.2(4) . . . . ? N6 Ni1 N4 C20 -6.7(6) . . . . ? N2 Ni1 N4 C16 -0.5(5) . . . . ? N5 Ni1 N4 C16 178.7(5) . . . . ? N3 Ni1 N4 C16 77.8(4) . . . . ? N1 Ni1 N4 C16 -79.4(4) . . . . ? N6 Ni1 N4 C16 173.6(4) . . . . ? N3 Ni1 N5 C25 -86.1(4) . . . . ? N1 Ni1 N5 C25 94.5(4) . . . . ? N6 Ni1 N5 C25 2.2(4) . . . . ? N4 Ni1 N5 C25 -175.7(4) . . . . ? N3 Ni1 N5 C21 89.7(4) . . . . ? N1 Ni1 N5 C21 -89.7(4) . . . . ? N6 Ni1 N5 C21 178.1(4) . . . . ? N4 Ni1 N5 C21 0.1(4) . . . . ? N2 Ni1 N6 C30 0.6(5) . . . . ? N5 Ni1 N6 C30 -178.4(5) . . . . ? N3 Ni1 N6 C30 -77.3(5) . . . . ? N1 Ni1 N6 C30 80.1(5) . . . . ? N4 Ni1 N6 C30 -173.4(4) . . . . ? N2 Ni1 N6 C26 177.6(3) . . . . ? N5 Ni1 N6 C26 -1.5(3) . . . . ? N3 Ni1 N6 C26 99.6(4) . . . . ? N1 Ni1 N6 C26 -103.0(4) . . . . ? N4 Ni1 N6 C26 3.6(6) . . . . ? C5 N1 C1 C2 0.5(8) . . . . ? Ni1 N1 C1 C2 -175.7(4) . . . . ? N1 C1 C2 C3 -0.5(9) . . . . ? C1 C2 C3 C4 0.3(10) . . . . ? C2 C3 C4 C5 0.1(10) . . . . ? C1 N1 C5 C4 -0.1(8) . . . . ? Ni1 N1 C5 C4 176.6(4) . . . . ? C1 N1 C5 C6 179.3(5) . . . . ? Ni1 N1 C5 C6 -3.9(6) . . . . ? C3 C4 C5 N1 -0.1(9) . . . . ? C3 C4 C5 C6 -179.5(6) . . . . ? C10 N2 C6 C7 -0.5(8) . . . . ? Ni1 N2 C6 C7 175.0(4) . . . . ? C10 N2 C6 C5 -179.1(4) . . . . ? Ni1 N2 C6 C5 -3.7(6) . . . . ? N1 C5 C6 N2 5.0(7) . . . . ? C4 C5 C6 N2 -175.6(5) . . . . ? N1 C5 C6 C7 -173.6(5) . . . . ? C4 C5 C6 C7 5.8(9) . . . . ? N2 C6 C7 C8 1.2(8) . . . . ? C5 C6 C7 C8 179.7(5) . . . . ? C6 C7 C8 C9 0.0(9) . . . . ? C7 C8 C9 C10 -1.8(9) . . . . ? C6 N2 C10 C9 -1.4(7) . . . . ? Ni1 N2 C10 C9 -176.9(4) . . . . ? C6 N2 C10 C11 178.0(4) . . . . ? Ni1 N2 C10 C11 2.6(6) . . . . ? C8 C9 C10 N2 2.6(8) . . . . ? C8 C9 C10 C11 -176.8(5) . . . . ? C15 N3 C11 C12 -1.4(7) . . . . ? Ni1 N3 C11 C12 175.9(4) . . . . ? C15 N3 C11 C10 178.1(5) . . . . ? Ni1 N3 C11 C10 -4.6(5) . . . . ? N2 C10 C11 N3 1.6(6) . . . . ? C9 C10 C11 N3 -179.0(5) . . . . ? N2 C10 C11 C12 -178.9(5) . . . . ? C9 C10 C11 C12 0.5(8) . . . . ? N3 C11 C12 C13 0.7(8) . . . . ? C10 C11 C12 C13 -178.7(5) . . . . ? C11 C12 C13 C14 0.1(9) . . . . ? C12 C13 C14 C15 -0.2(9) . . . . ? C11 N3 C15 C14 1.3(8) . . . . ? Ni1 N3 C15 C14 -175.6(4) . . . . ? C13 C14 C15 N3 -0.5(9) . . . . ? C20 N4 C16 C17 -2.0(8) . . . . ? Ni1 N4 C16 C17 177.6(4) . . . . ? N4 C16 C17 C18 -0.6(8) . . . . ? C16 C17 C18 C19 3.0(9) . . . . ? C17 C18 C19 C20 -2.9(9) . . . . ? C16 N4 C20 C19 2.2(8) . . . . ? Ni1 N4 C20 C19 -177.5(4) . . . . ? C16 N4 C20 C21 -177.5(5) . . . . ? Ni1 N4 C20 C21 2.9(6) . . . . ? C18 C19 C20 N4 0.2(9) . . . . ? C18 C19 C20 C21 179.9(6) . . . . ? C25 N5 C21 C22 -2.7(9) . . . . ? Ni1 N5 C21 C22 -178.4(5) . . . . ? C25 N5 C21 C20 177.0(5) . . . . ? Ni1 N5 C21 C20 1.3(6) . . . . ? N4 C20 C21 N5 -2.8(7) . . . . ? C19 C20 C21 N5 177.6(5) . . . . ? N4 C20 C21 C22 176.9(6) . . . . ? C19 C20 C21 C22 -2.7(10) . . . . ? N5 C21 C22 C23 0.8(10) . . . . ? C20 C21 C22 C23 -178.8(6) . . . . ? C21 C22 C23 C24 1.1(11) . . . . ? C22 C23 C24 C25 -1.3(11) . . . . ? C21 N5 C25 C24 2.5(8) . . . . ? Ni1 N5 C25 C24 178.3(4) . . . . ? C21 N5 C25 C26 -178.3(5) . . . . ? Ni1 N5 C25 C26 -2.5(6) . . . . ? C23 C24 C25 N5 -0.5(9) . . . . ? C23 C24 C25 C26 -179.6(6) . . . . ? C30 N6 C26 C27 -0.5(8) . . . . ? Ni1 N6 C26 C27 -177.7(5) . . . . ? C30 N6 C26 C25 177.8(5) . . . . ? Ni1 N6 C26 C25 0.6(6) . . . . ? N5 C25 C26 N6 1.1(7) . . . . ? C24 C25 C26 N6 -179.7(6) . . . . ? N5 C25 C26 C27 179.4(5) . . . . ? C24 C25 C26 C27 -1.4(9) . . . . ? N6 C26 C27 C28 1.0(9) . . . . ? C25 C26 C27 C28 -177.2(6) . . . . ? C26 C27 C28 C29 -0.8(10) . . . . ? C27 C28 C29 C30 0.1(10) . . . . ? C26 N6 C30 C29 -0.3(8) . . . . ? Ni1 N6 C30 C29 176.5(4) . . . . ? C28 C29 C30 N6 0.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.011 _refine_diff_density_min -0.968 _refine_diff_density_rms 0.122