# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Thoi, V.' 'Chang, Chris' _publ_contact_author_name 'Chang, Chris' _publ_contact_author_email ChrisChang@berkeley.edu _publ_section_title ; Nickel N-Heterocyclic Carbene-Pyridine Complexes that Exhibit High Selectivity for Electrocatalytic Reduction of Carbon Dioxide Over Water ; # Attachment '- ethyl.cif' data_ethyl _database_code_depnum_ccdc_archive 'CCDC 809509' #TrackingRef '- ethyl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H16 F12 N6 Ni P2' _chemical_formula_sum 'C18 H16 F12 N6 Ni P2' _chemical_formula_weight 665.02 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 10.0790(7) _cell_length_b 19.0802(15) _cell_length_c 12.1281(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.4060(10) _cell_angle_gamma 90.00 _cell_volume 2294.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 119(2) _cell_measurement_reflns_used 12779 _cell_measurement_theta_min 2.315 _cell_measurement_theta_max 25.333 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.926 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 1.106 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7326 _exptl_absorpt_correction_T_max 0.8091 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 119(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 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 12525 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0117 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.33 _reflns_number_total 2099 _reflns_number_gt 2061 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2009.3' _computing_cell_refinement 'Bruker APEX2 v. 2009.3' _computing_data_reduction 'Bruker APEX2 v. 2009.3' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material CIFTAB _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^)+(0.0271P)^2^+2.8738P] 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 2099 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0220 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0572 _refine_ls_wR_factor_gt 0.0570 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 C1 C 0.12364(15) 0.14192(8) 0.35626(13) 0.0205(3) Uani 1 1 d . . . H1 H 0.0365 0.1212 0.3409 0.025 Uiso 1 1 calc R . . C2 C 0.23065(17) 0.10245(9) 0.41080(13) 0.0237(3) Uani 1 1 d . . . H2 H 0.2172 0.0555 0.4322 0.028 Uiso 1 1 calc R . . C3 C 0.35767(16) 0.13246(9) 0.43373(13) 0.0251(4) Uani 1 1 d . . . H3 H 0.4332 0.1055 0.4680 0.030 Uiso 1 1 calc R . . C4 C 0.37423(16) 0.20216(9) 0.40643(13) 0.0228(3) Uani 1 1 d . . . H4 H 0.4596 0.2245 0.4238 0.027 Uiso 1 1 calc R . . C5 C 0.26183(15) 0.23745(8) 0.35314(12) 0.0182(3) Uani 1 1 d . . . C8 C 0.13682(15) 0.33838(8) 0.28700(12) 0.0180(3) Uani 1 1 d . . . C6 C 0.36134(17) 0.35891(9) 0.33908(14) 0.0249(3) Uani 1 1 d . . . H7 H 0.4549 0.3515 0.3655 0.030 Uiso 1 1 calc R . . C7 C 0.30014(17) 0.41975(9) 0.30596(14) 0.0261(4) Uani 1 1 d . . . H8 H 0.3432 0.4639 0.3041 0.031 Uiso 1 1 calc R . . C9 C 0.06461(17) 0.46030(8) 0.22610(13) 0.0237(3) Uani 1 1 d . . . H9A H 0.0415 0.4527 0.1441 0.028 Uiso 1 1 calc R . . H9B H 0.1074 0.5070 0.2387 0.028 Uiso 1 1 calc R . . N1 N 0.13805(12) 0.20844(7) 0.32412(10) 0.0174(3) Uani 1 1 d . . . N2 N 0.25934(13) 0.30914(7) 0.32668(10) 0.0191(3) Uani 1 1 d . . . N3 N 0.16254(14) 0.40679(7) 0.27484(11) 0.0209(3) Uani 1 1 d . . . F1 F -0.33319(11) 0.57640(6) 0.12981(9) 0.0352(3) Uani 1 1 d . . . F2 F -0.15326(10) 0.54929(5) 0.04931(8) 0.0294(2) Uani 1 1 d . . . F3 F -0.16128(11) 0.65299(6) 0.13973(9) 0.0379(3) Uani 1 1 d . . . F4 F -0.18082(11) 0.65111(6) -0.04842(9) 0.0342(3) Uani 1 1 d . . . F5 F -0.36362(10) 0.67751(5) 0.03045(9) 0.0324(2) Uani 1 1 d . . . F6 F -0.35412(11) 0.57406(6) -0.05910(9) 0.0366(3) Uani 1 1 d . . . P2 P -0.25765(4) 0.61448(2) 0.04006(3) 0.01976(11) Uani 1 1 d . . . Ni1 Ni 0.0000 0.273491(14) 0.2500 0.01563(9) Uani 1 2 d S . . 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 0.0189(8) 0.0226(8) 0.0207(8) 0.0006(6) 0.0053(6) 0.0001(6) C2 0.0256(8) 0.0252(8) 0.0208(8) 0.0027(6) 0.0054(6) 0.0050(7) C3 0.0206(8) 0.0341(9) 0.0199(8) 0.0013(7) 0.0014(6) 0.0094(7) C4 0.0149(7) 0.0335(9) 0.0194(8) -0.0031(7) 0.0016(6) 0.0014(6) C5 0.0156(7) 0.0245(8) 0.0147(7) -0.0024(6) 0.0033(6) -0.0007(6) C8 0.0192(7) 0.0210(8) 0.0139(7) -0.0007(6) 0.0029(6) -0.0010(6) C6 0.0193(8) 0.0319(9) 0.0234(8) -0.0052(7) 0.0036(6) -0.0093(7) C7 0.0259(9) 0.0286(9) 0.0238(8) -0.0041(7) 0.0049(7) -0.0122(7) C9 0.0331(9) 0.0182(8) 0.0190(7) 0.0008(6) 0.0023(7) -0.0032(7) N1 0.0141(6) 0.0215(6) 0.0166(6) -0.0003(5) 0.0027(5) 0.0007(5) N2 0.0151(6) 0.0236(7) 0.0179(6) -0.0020(5) 0.0016(5) -0.0034(5) N3 0.0246(7) 0.0204(7) 0.0174(6) -0.0016(5) 0.0033(5) -0.0049(5) F1 0.0322(6) 0.0340(6) 0.0449(6) 0.0120(5) 0.0214(5) 0.0072(4) F2 0.0222(5) 0.0332(6) 0.0331(5) 0.0027(4) 0.0059(4) 0.0097(4) F3 0.0304(6) 0.0518(7) 0.0295(6) -0.0150(5) 0.0006(4) -0.0057(5) F4 0.0406(6) 0.0348(6) 0.0310(6) 0.0047(4) 0.0164(5) -0.0004(5) F5 0.0288(5) 0.0241(5) 0.0447(6) 0.0021(4) 0.0079(5) 0.0073(4) F6 0.0300(5) 0.0337(6) 0.0399(6) -0.0092(5) -0.0102(5) 0.0013(4) P2 0.0166(2) 0.0224(2) 0.0200(2) 0.00003(15) 0.00257(16) 0.00158(15) Ni1 0.01209(15) 0.01675(15) 0.01717(15) 0.000 0.00025(10) 0.000 _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 1.343(2) . ? C1 C2 1.382(2) . ? C1 H1 0.9500 . ? C2 C3 1.384(2) . ? C2 H2 0.9500 . ? C3 C4 1.388(3) . ? C3 H3 0.9500 . ? C4 C5 1.375(2) . ? C4 H4 0.9500 . ? C5 N1 1.352(2) . ? C5 N2 1.404(2) . ? C8 N3 1.344(2) . ? C8 N2 1.361(2) . ? C8 Ni1 1.8473(15) . ? C6 C7 1.342(3) . ? C6 N2 1.388(2) . ? C6 H7 0.9500 . ? C7 N3 1.392(2) . ? C7 H8 0.9500 . ? C9 N3 1.468(2) . ? C9 C9 1.518(3) 2 ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? N1 Ni1 1.9578(13) . ? F1 P2 1.6099(10) . ? F2 P2 1.6198(10) . ? F3 P2 1.5877(11) . ? F4 P2 1.5937(10) . ? F5 P2 1.5988(10) . ? F6 P2 1.6013(10) . ? Ni1 C8 1.8473(15) 2 ? Ni1 N1 1.9578(13) 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 122.53(15) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 118.96(15) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C2 C3 C4 119.69(15) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 117.20(15) . . ? C5 C4 H4 121.4 . . ? C3 C4 H4 121.4 . . ? N1 C5 C4 124.41(15) . . ? N1 C5 N2 111.21(13) . . ? C4 C5 N2 124.32(14) . . ? N3 C8 N2 104.85(13) . . ? N3 C8 Ni1 140.77(12) . . ? N2 C8 Ni1 113.63(11) . . ? C7 C6 N2 105.55(14) . . ? C7 C6 H7 127.2 . . ? N2 C6 H7 127.2 . . ? C6 C7 N3 108.01(14) . . ? C6 C7 H8 126.0 . . ? N3 C7 H8 126.0 . . ? N3 C9 C9 114.02(12) . 2 ? N3 C9 H9A 108.7 . . ? C9 C9 H9A 108.7 2 . ? N3 C9 H9B 108.7 . . ? C9 C9 H9B 108.7 2 . ? H9A C9 H9B 107.6 . . ? C1 N1 C5 117.02(13) . . ? C1 N1 Ni1 128.84(11) . . ? C5 N1 Ni1 113.94(10) . . ? C8 N2 C6 111.40(13) . . ? C8 N2 C5 117.24(13) . . ? C6 N2 C5 131.26(13) . . ? C8 N3 C7 110.20(14) . . ? C8 N3 C9 126.20(13) . . ? C7 N3 C9 123.37(13) . . ? F3 P2 F4 90.28(6) . . ? F3 P2 F5 90.92(6) . . ? F4 P2 F5 91.17(6) . . ? F3 P2 F6 178.77(7) . . ? F4 P2 F6 90.49(6) . . ? F5 P2 F6 90.03(6) . . ? F3 P2 F1 89.61(6) . . ? F4 P2 F1 178.97(6) . . ? F5 P2 F1 89.85(6) . . ? F6 P2 F1 89.61(6) . . ? F3 P2 F2 90.13(6) . . ? F4 P2 F2 89.71(6) . . ? F5 P2 F2 178.63(6) . . ? F6 P2 F2 88.91(6) . . ? F1 P2 F2 89.27(5) . . ? C8 Ni1 C8 95.83(10) . 2 ? C8 Ni1 N1 166.89(6) . 2 ? C8 Ni1 N1 82.87(6) 2 2 ? C8 Ni1 N1 82.87(6) . . ? C8 Ni1 N1 166.89(6) 2 . ? N1 Ni1 N1 101.31(8) 2 . ? 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 0.2(2) . . . . ? C1 C2 C3 C4 2.9(2) . . . . ? C2 C3 C4 C5 -2.4(2) . . . . ? C3 C4 C5 N1 -1.3(2) . . . . ? C3 C4 C5 N2 175.49(14) . . . . ? N2 C6 C7 N3 0.48(18) . . . . ? C2 C1 N1 C5 -3.7(2) . . . . ? C2 C1 N1 Ni1 -178.30(11) . . . . ? C4 C5 N1 C1 4.3(2) . . . . ? N2 C5 N1 C1 -172.81(13) . . . . ? C4 C5 N1 Ni1 179.70(12) . . . . ? N2 C5 N1 Ni1 2.56(15) . . . . ? N3 C8 N2 C6 -0.15(16) . . . . ? Ni1 C8 N2 C6 172.01(10) . . . . ? N3 C8 N2 C5 176.68(12) . . . . ? Ni1 C8 N2 C5 -11.16(16) . . . . ? C7 C6 N2 C8 -0.22(18) . . . . ? C7 C6 N2 C5 -176.46(15) . . . . ? N1 C5 N2 C8 5.38(18) . . . . ? C4 C5 N2 C8 -171.77(14) . . . . ? N1 C5 N2 C6 -178.56(15) . . . . ? C4 C5 N2 C6 4.3(3) . . . . ? N2 C8 N3 C7 0.45(16) . . . . ? Ni1 C8 N3 C7 -168.15(14) . . . . ? N2 C8 N3 C9 174.99(13) . . . . ? Ni1 C8 N3 C9 6.4(3) . . . . ? C6 C7 N3 C8 -0.61(18) . . . . ? C6 C7 N3 C9 -175.33(14) . . . . ? C9 C9 N3 C8 49.6(2) 2 . . . ? C9 C9 N3 C7 -136.57(15) 2 . . . ? N3 C8 Ni1 C8 -15.65(14) . . . 2 ? N2 C8 Ni1 C8 176.38(14) . . . 2 ? N3 C8 Ni1 N1 67.9(4) . . . 2 ? N2 C8 Ni1 N1 -100.0(3) . . . 2 ? N3 C8 Ni1 N1 177.48(19) . . . . ? N2 C8 Ni1 N1 9.52(10) . . . . ? C1 N1 Ni1 C8 167.89(14) . . . . ? C5 N1 Ni1 C8 -6.80(11) . . . . ? C1 N1 Ni1 C8 82.8(3) . . . 2 ? C5 N1 Ni1 C8 -91.9(3) . . . 2 ? C1 N1 Ni1 N1 -24.70(11) . . . 2 ? C5 N1 Ni1 N1 160.60(12) . . . 2 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.327 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.070 # Attachment '- ethyldimer.cif' data_ethyldimer _database_code_depnum_ccdc_archive 'CCDC 809510' #TrackingRef '- ethyldimer.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H28 N12 Ni2, 2(P F6), 2(C4 H10 O2)' _chemical_formula_sum 'C42 H48 F12 N12 Ni2 O4 P2' _chemical_formula_weight 1192.28 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 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 10.6550(15) _cell_length_b 21.779(3) _cell_length_c 21.880(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.063(2) _cell_angle_gamma 90.00 _cell_volume 5014.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 51586 _cell_measurement_theta_min 2.151 _cell_measurement_theta_max 25.45 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 0.916 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7108 _exptl_absorpt_correction_T_max 0.9730 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_reflns_number 51586 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.45 _reflns_number_total 9220 _reflns_number_gt 6045 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2009.3' _computing_cell_refinement 'Bruker APEX2 v. 2009.3' _computing_data_reduction 'Bruker APEX2 v. 2009.3' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material CIFTAB _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^)+(0.0353P)^2^+6.9898P] 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 9220 _refine_ls_number_parameters 661 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.006 _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 C30 C 0.9136(3) 0.09277(16) 0.07875(18) 0.0328(9) Uani 1 1 d . . . H30 H 0.9132 0.0622 0.0477 0.039 Uiso 1 1 calc R . . C44 C 0.1638(4) 0.0892(2) 0.3531(2) 0.0462(11) Uiso 1 1 d . . . H44A H 0.188(4) 0.0885(19) 0.399(2) 0.069 Uiso 1 1 d . . . H44B H 0.083(4) 0.067(2) 0.3338(19) 0.069 Uiso 1 1 d . . . H44C H 0.168(4) 0.138(2) 0.3404(19) 0.069 Uiso 1 1 d . . . C1 C 0.5296(3) 0.35184(14) 0.15923(15) 0.0216(7) Uani 1 1 d . . . C2 C 0.4136(3) 0.41033(16) 0.21725(18) 0.0364(9) Uani 1 1 d . . . H2 H 0.3778 0.4253 0.2515 0.044 Uiso 1 1 calc R . . C3 C 0.3937(4) 0.43172(17) 0.15958(18) 0.0369(9) Uani 1 1 d . . . H3 H 0.3401 0.4652 0.1449 0.044 Uiso 1 1 calc R . . C4 C 0.4681(3) 0.41179(15) 0.05983(16) 0.0278(8) Uani 1 1 d . . . H4A H 0.4633 0.4570 0.0549 0.033 Uiso 1 1 calc R . . H4B H 0.3920 0.3940 0.0341 0.033 Uiso 1 1 calc R . . C5 C 0.5852(3) 0.38889(14) 0.03618(16) 0.0256(8) Uani 1 1 d . . . H5A H 0.5928 0.4099 -0.0032 0.031 Uiso 1 1 calc R . . H5B H 0.6614 0.3991 0.0665 0.031 Uiso 1 1 calc R . . C6 C 0.4984(3) 0.29436(16) -0.02074(16) 0.0280(8) Uani 1 1 d . . . H6 H 0.4512 0.3141 -0.0557 0.034 Uiso 1 1 calc R . . C7 C 0.4971(3) 0.23465(16) -0.00866(16) 0.0279(8) Uani 1 1 d . . . H7 H 0.4492 0.2039 -0.0328 0.033 Uiso 1 1 calc R . . C8 C 0.6330(3) 0.28194(13) 0.07057(14) 0.0179(7) Uani 1 1 d . . . C9 C 0.5846(3) 0.17547(14) 0.08608(16) 0.0236(8) Uani 1 1 d . . . C10 C 0.5599(3) 0.11623(15) 0.06407(18) 0.0303(9) Uani 1 1 d . . . H10 H 0.5439 0.1079 0.0209 0.036 Uiso 1 1 calc R . . C11 C 0.5595(3) 0.07018(16) 0.1068(2) 0.0377(10) Uani 1 1 d . . . H11 H 0.5388 0.0293 0.0937 0.045 Uiso 1 1 calc R . . C12 C 0.5896(3) 0.08373(16) 0.1692(2) 0.0383(10) Uani 1 1 d . . . H12 H 0.5919 0.0522 0.1993 0.046 Uiso 1 1 calc R . . C13 C 0.6159(3) 0.14348(15) 0.18695(18) 0.0297(8) Uani 1 1 d . . . H13 H 0.6382 0.1522 0.2298 0.036 Uiso 1 1 calc R . . C14 C 0.5570(3) 0.32719(15) 0.26685(16) 0.0237(8) Uani 1 1 d . . . C15 C 0.5328(3) 0.33460(17) 0.32675(16) 0.0316(9) Uani 1 1 d . . . H15 H 0.4723 0.3638 0.3361 0.038 Uiso 1 1 calc R . . C16 C 0.5989(4) 0.29856(17) 0.37227(17) 0.0351(9) Uani 1 1 d . . . H16 H 0.5850 0.3025 0.4139 0.042 Uiso 1 1 calc R . . C17 C 0.6857(4) 0.25650(17) 0.35689(17) 0.0350(9) Uani 1 1 d . . . H17 H 0.7327 0.2314 0.3879 0.042 Uiso 1 1 calc R . . C18 C 0.7032(3) 0.25144(16) 0.29648(16) 0.0308(9) Uani 1 1 d . . . H18 H 0.7623 0.2220 0.2863 0.037 Uiso 1 1 calc R . . C19 C 0.9379(3) 0.36530(14) 0.09755(16) 0.0222(7) Uani 1 1 d . . . C20 C 1.0443(3) 0.43211(15) 0.04256(18) 0.0310(9) Uani 1 1 d . . . H20 H 1.0792 0.4499 0.0093 0.037 Uiso 1 1 calc R . . C21 C 1.0555(3) 0.45258(16) 0.10012(18) 0.0311(9) Uani 1 1 d . . . H21 H 1.1000 0.4885 0.1158 0.037 Uiso 1 1 calc R . . C22 C 0.9835(3) 0.42467(15) 0.19856(16) 0.0299(8) Uani 1 1 d . . . H22A H 0.9746 0.4695 0.2042 0.036 Uiso 1 1 calc R . . H22B H 1.0642 0.4117 0.2241 0.036 Uiso 1 1 calc R . . C23 C 0.8748(3) 0.39258(15) 0.22208(16) 0.0285(8) Uani 1 1 d . . . H23A H 0.8643 0.4100 0.2628 0.034 Uiso 1 1 calc R . . H23B H 0.7952 0.4001 0.1930 0.034 Uiso 1 1 calc R . . C24 C 0.9833(3) 0.29986(16) 0.27440(17) 0.0328(9) Uani 1 1 d . . . H24 H 1.0273 0.3200 0.3100 0.039 Uiso 1 1 calc R . . C25 C 0.9946(3) 0.24104(16) 0.26017(17) 0.0328(9) Uani 1 1 d . . . H25 H 1.0478 0.2114 0.2833 0.039 Uiso 1 1 calc R . . C26 C 0.8506(3) 0.28545(14) 0.18279(15) 0.0213(7) Uani 1 1 d . . . C27 C 0.9142(3) 0.18196(15) 0.16383(16) 0.0234(8) Uani 1 1 d . . . C28 C 0.9371(3) 0.12242(15) 0.18428(18) 0.0308(9) Uani 1 1 d . . . H28 H 0.9515 0.1131 0.2272 0.037 Uiso 1 1 calc R . . C29 C 0.9385(3) 0.07710(16) 0.14080(19) 0.0368(10) Uani 1 1 d . . . H29 H 0.9562 0.0358 0.1531 0.044 Uiso 1 1 calc R . . C31 C 0.8894(3) 0.15290(16) 0.06263(18) 0.0295(8) Uani 1 1 d . . . H31 H 0.8709 0.1629 0.0199 0.035 Uiso 1 1 calc R . . C32 C 0.9242(3) 0.34218(15) -0.00983(16) 0.0249(8) Uani 1 1 d . . . C33 C 0.9559(4) 0.35064(17) -0.06760(17) 0.0341(9) Uani 1 1 d . . . H33 H 1.0123 0.3825 -0.0753 0.041 Uiso 1 1 calc R . . C34 C 0.9035(4) 0.31147(18) -0.11410(18) 0.0391(10) Uani 1 1 d . . . H34 H 0.9241 0.3156 -0.1546 0.047 Uiso 1 1 calc R . . C35 C 0.8206(4) 0.26597(17) -0.10125(17) 0.0349(9) Uani 1 1 d . . . H35 H 0.7826 0.2389 -0.1329 0.042 Uiso 1 1 calc R . . C36 C 0.7942(3) 0.26077(16) -0.04218(16) 0.0270(8) Uani 1 1 d . . . H36 H 0.7374 0.2294 -0.0336 0.032 Uiso 1 1 calc R . . C37 C 1.2122(4) 0.27596(19) 0.0562(2) 0.0415(10) Uiso 1 1 d . . . C38 C 1.2192(4) 0.16816(16) 0.05378(17) 0.0349(9) Uiso 1 1 d . . . H38A H 1.1662 0.1637 0.0868 0.042 Uiso 1 1 calc R . . H38B H 1.3093 0.1705 0.0735 0.042 Uiso 1 1 calc R . . C39 C 1.2004(4) 0.11401(18) 0.01145(18) 0.0394(10) Uiso 1 1 d . . . H39A H 1.2157 0.0756 0.0357 0.047 Uiso 1 1 calc R . . H39B H 1.1119 0.1133 -0.0107 0.047 Uiso 1 1 calc R . . C40 C 1.2763(5) 0.0674(2) -0.0723(3) 0.0567(13) Uiso 1 1 d . . . C41 C 0.3090(5) 0.2178(2) 0.2237(2) 0.0514(12) Uiso 1 1 d . . . C42 C 0.3130(4) 0.11026(18) 0.2367(2) 0.0436(10) Uiso 1 1 d . . . H42A H 0.4026 0.1139 0.2569 0.052 Uiso 1 1 calc R . . H42B H 0.3122 0.1030 0.1920 0.052 Uiso 1 1 calc R . . C43 C 0.2521(4) 0.05732(18) 0.26386(18) 0.0397(10) Uiso 1 1 d . . . H43A H 0.1605 0.0567 0.2464 0.048 Uiso 1 1 calc R . . H43B H 0.2902 0.0188 0.2513 0.048 Uiso 1 1 calc R . . N1 N 0.4975(3) 0.36167(12) 0.21699(13) 0.0239(6) Uani 1 1 d . . . N2 N 0.4649(3) 0.39658(12) 0.12466(13) 0.0247(7) Uani 1 1 d . . . N3 N 0.5799(2) 0.32300(12) 0.02618(12) 0.0218(6) Uani 1 1 d . . . N4 N 0.5807(2) 0.22614(11) 0.04672(12) 0.0216(6) Uani 1 1 d . . . N5 N 0.6402(2) 0.28654(12) 0.25047(12) 0.0235(6) Uani 1 1 d . . . N6 N 0.6117(2) 0.19026(12) 0.14634(13) 0.0226(6) Uani 1 1 d . . . N7 N 0.9707(2) 0.37906(12) 0.04070(13) 0.0242(6) Uani 1 1 d . . . N8 N 0.9911(2) 0.41249(12) 0.13377(13) 0.0240(6) Uani 1 1 d . . . N9 N 0.8962(2) 0.32686(12) 0.22839(12) 0.0229(6) Uani 1 1 d . . . N10 N 0.9129(2) 0.23139(12) 0.20456(13) 0.0235(6) Uani 1 1 d . . . N11 N 0.8452(2) 0.29812(12) 0.00440(12) 0.0235(6) Uani 1 1 d . . . N12 N 0.8907(2) 0.19862(12) 0.10427(13) 0.0230(6) Uani 1 1 d . . . Ni1 Ni 0.64953(4) 0.285859(18) 0.158964(19) 0.01959(11) Uani 1 1 d . . . Ni2 Ni 0.83252(4) 0.293233(18) 0.094927(19) 0.02045(11) Uani 1 1 d . . . O1 O 0.2475(2) 0.16561(12) 0.24502(12) 0.0422(7) Uiso 1 1 d . . . O2 O 0.2650(2) 0.05891(11) 0.32951(12) 0.0375(6) Uiso 1 1 d . . . O3 O 1.2864(2) 0.11821(12) -0.03156(12) 0.0401(7) Uiso 1 1 d . . . O4 O 1.1850(2) 0.22231(11) 0.01963(12) 0.0364(6) Uiso 1 1 d . . . H37A H 1.200(4) 0.3111(19) 0.0256(18) 0.055 Uiso 1 1 d . . . H37B H 1.304(4) 0.2777(17) 0.0752(18) 0.055 Uiso 1 1 d . . . H37C H 1.157(4) 0.2750(17) 0.0891(19) 0.055 Uiso 1 1 d . . . H40A H 1.336(4) 0.0773(18) -0.1014(18) 0.055 Uiso 1 1 d . . . H40B H 1.198(4) 0.0639(18) -0.0932(18) 0.055 Uiso 1 1 d . . . H40C H 1.289(4) 0.0277(19) -0.0455(18) 0.055 Uiso 1 1 d . . . H41A H 0.251(4) 0.2515(19) 0.2264(18) 0.055 Uiso 1 1 d . . . H41B H 0.319(4) 0.2034(18) 0.181(2) 0.055 Uiso 1 1 d . . . H41C H 0.398(4) 0.2194(17) 0.2487(19) 0.055 Uiso 1 1 d . . . F7 F 0.8596(2) 0.57701(12) 0.16592(12) 0.0621(7) Uani 1 1 d . . . F8 F 0.58680(19) 0.55062(10) 0.08780(11) 0.0477(6) Uani 1 1 d . . . F9 F 0.7507(2) 0.61139(11) 0.07641(11) 0.0541(7) Uani 1 1 d . . . F10 F 0.6633(2) 0.61688(11) 0.16231(12) 0.0636(7) Uani 1 1 d . . . F11 F 0.6946(3) 0.51598(14) 0.17738(14) 0.0888(11) Uani 1 1 d . . . F12 F 0.7818(3) 0.51076(13) 0.09131(16) 0.0881(10) Uani 1 1 d . . . P2 P 0.72308(9) 0.56324(4) 0.12732(5) 0.0312(2) Uani 1 1 d . . . F1 F 0.4195(2) 0.94812(12) 0.15258(11) 0.0626(8) Uani 1 1 d . . . F2 F 0.1581(2) 0.90214(13) 0.07702(11) 0.0639(8) Uani 1 1 d . . . F3 F 0.3166(3) 0.96227(11) 0.05522(11) 0.0625(7) Uani 1 1 d . . . F4 F 0.3578(2) 0.86785(10) 0.09235(11) 0.0567(7) Uani 1 1 d . . . F5 F 0.2627(2) 0.88861(12) 0.17379(10) 0.0523(6) Uani 1 1 d . . . F6 F 0.2189(3) 0.98327(14) 0.13669(13) 0.0997(12) Uani 1 1 d . . . P1 P 0.28833(9) 0.92629(4) 0.11428(4) 0.0306(2) 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 C30 0.028(2) 0.0263(19) 0.044(3) -0.0116(18) 0.0063(18) 0.0033(15) C1 0.0201(18) 0.0216(17) 0.0233(19) -0.0027(14) 0.0043(14) -0.0028(14) C2 0.039(2) 0.033(2) 0.041(3) -0.0009(19) 0.0157(19) 0.0167(17) C3 0.039(2) 0.030(2) 0.043(3) 0.0027(19) 0.0117(19) 0.0192(17) C4 0.033(2) 0.0196(17) 0.029(2) 0.0040(15) -0.0016(16) 0.0059(15) C5 0.032(2) 0.0200(17) 0.024(2) 0.0048(15) 0.0013(16) -0.0018(14) C6 0.0266(19) 0.038(2) 0.0185(19) -0.0038(16) -0.0014(15) 0.0044(16) C7 0.0260(19) 0.0295(19) 0.026(2) -0.0101(16) -0.0017(16) 0.0003(15) C8 0.0172(16) 0.0175(16) 0.0200(18) -0.0018(14) 0.0056(13) 0.0013(13) C9 0.0164(17) 0.0215(17) 0.035(2) -0.0017(16) 0.0099(15) 0.0000(14) C10 0.0244(19) 0.0224(18) 0.046(2) -0.0095(17) 0.0101(17) -0.0013(15) C11 0.031(2) 0.0188(18) 0.067(3) -0.006(2) 0.022(2) -0.0018(15) C12 0.037(2) 0.024(2) 0.059(3) 0.0129(19) 0.024(2) 0.0033(16) C13 0.030(2) 0.0276(19) 0.034(2) 0.0072(17) 0.0118(17) -0.0008(15) C14 0.0238(19) 0.0249(18) 0.0227(19) -0.0014(15) 0.0048(15) -0.0018(14) C15 0.037(2) 0.035(2) 0.025(2) -0.0051(17) 0.0105(17) 0.0023(17) C16 0.042(2) 0.042(2) 0.022(2) -0.0026(18) 0.0070(17) -0.0073(18) C17 0.040(2) 0.041(2) 0.023(2) 0.0074(17) 0.0017(17) 0.0020(18) C18 0.032(2) 0.035(2) 0.024(2) 0.0042(17) 0.0034(17) 0.0042(16) C19 0.0189(17) 0.0201(17) 0.027(2) 0.0007(15) 0.0002(15) 0.0009(13) C20 0.029(2) 0.0228(18) 0.042(2) 0.0100(17) 0.0093(17) -0.0053(15) C21 0.029(2) 0.0218(18) 0.042(2) 0.0026(17) 0.0029(17) -0.0045(15) C22 0.032(2) 0.0247(18) 0.031(2) -0.0075(16) -0.0025(16) -0.0044(15) C23 0.034(2) 0.0252(18) 0.025(2) -0.0066(16) -0.0004(16) -0.0003(15) C24 0.033(2) 0.034(2) 0.027(2) -0.0031(17) -0.0072(16) -0.0003(16) C25 0.031(2) 0.033(2) 0.029(2) 0.0010(17) -0.0109(17) 0.0038(16) C26 0.0204(17) 0.0195(16) 0.0246(19) -0.0013(15) 0.0051(14) -0.0014(14) C27 0.0147(17) 0.0223(17) 0.033(2) -0.0051(16) 0.0047(15) -0.0011(13) C28 0.029(2) 0.0252(19) 0.036(2) 0.0009(17) -0.0024(17) 0.0027(15) C29 0.032(2) 0.0208(18) 0.056(3) -0.0001(19) 0.0002(19) 0.0051(15) C31 0.0250(19) 0.031(2) 0.034(2) -0.0063(17) 0.0073(16) 0.0033(15) C32 0.0219(18) 0.0268(18) 0.026(2) 0.0059(16) 0.0046(15) 0.0016(14) C33 0.038(2) 0.036(2) 0.029(2) 0.0062(18) 0.0077(18) -0.0040(17) C34 0.046(2) 0.047(2) 0.026(2) 0.0052(19) 0.0125(19) 0.0058(19) C35 0.041(2) 0.040(2) 0.024(2) -0.0033(17) 0.0064(18) -0.0012(18) C36 0.0256(19) 0.0294(19) 0.026(2) -0.0063(16) 0.0037(16) -0.0049(15) N1 0.0258(16) 0.0233(15) 0.0239(17) -0.0004(13) 0.0078(13) 0.0055(12) N2 0.0262(16) 0.0216(14) 0.0262(17) 0.0019(13) 0.0040(13) 0.0064(12) N3 0.0233(15) 0.0233(14) 0.0181(15) 0.0012(12) 0.0014(12) 0.0007(12) N4 0.0208(15) 0.0190(14) 0.0248(16) -0.0046(12) 0.0031(12) -0.0021(11) N5 0.0206(15) 0.0272(15) 0.0230(16) 0.0013(13) 0.0040(12) 0.0024(12) N6 0.0203(15) 0.0213(14) 0.0276(17) 0.0021(13) 0.0087(12) 0.0021(11) N7 0.0244(16) 0.0217(15) 0.0268(17) 0.0027(13) 0.0050(13) -0.0033(12) N8 0.0239(15) 0.0197(14) 0.0274(17) 0.0001(13) 0.0008(13) -0.0031(12) N9 0.0250(15) 0.0233(15) 0.0185(16) -0.0024(12) -0.0022(12) -0.0007(12) N10 0.0214(15) 0.0234(15) 0.0240(16) 0.0008(12) -0.0019(12) 0.0028(12) N11 0.0202(15) 0.0272(15) 0.0238(16) -0.0001(13) 0.0054(12) -0.0019(12) N12 0.0186(15) 0.0236(15) 0.0268(17) -0.0026(13) 0.0039(12) 0.0014(11) Ni1 0.0212(2) 0.0195(2) 0.0183(2) 0.00082(18) 0.00397(17) 0.00405(17) Ni2 0.0204(2) 0.0218(2) 0.0194(2) -0.00203(19) 0.00384(17) -0.00322(18) F7 0.0370(14) 0.0858(19) 0.0568(17) 0.0123(14) -0.0134(12) -0.0110(13) F8 0.0300(12) 0.0517(14) 0.0575(16) -0.0019(12) -0.0046(11) -0.0091(10) F9 0.0432(14) 0.0697(17) 0.0480(16) 0.0211(13) 0.0023(12) -0.0117(12) F10 0.0593(17) 0.0609(16) 0.0749(19) -0.0314(14) 0.0240(14) -0.0076(13) F11 0.077(2) 0.087(2) 0.096(2) 0.0636(19) -0.0058(17) -0.0197(17) F12 0.0606(18) 0.0689(19) 0.132(3) -0.0457(19) 0.0072(18) 0.0230(15) P2 0.0284(5) 0.0282(5) 0.0354(6) 0.0029(5) 0.0000(4) -0.0002(4) F1 0.0612(16) 0.0752(18) 0.0453(15) 0.0133(13) -0.0104(13) -0.0376(14) F2 0.0465(15) 0.102(2) 0.0391(15) -0.0029(14) -0.0058(12) -0.0137(14) F3 0.095(2) 0.0509(15) 0.0391(15) 0.0202(12) 0.0035(14) -0.0123(14) F4 0.0762(18) 0.0436(14) 0.0535(16) -0.0011(12) 0.0202(14) 0.0181(12) F5 0.0404(14) 0.0865(18) 0.0310(13) 0.0132(12) 0.0091(11) -0.0113(12) F6 0.143(3) 0.083(2) 0.065(2) -0.0309(17) -0.0065(19) 0.068(2) P1 0.0384(6) 0.0298(5) 0.0227(5) -0.0017(4) 0.0017(4) 0.0013(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 C30 C31 1.370(5) . ? C30 C29 1.384(5) . ? C30 H30 0.9500 . ? C44 O2 1.428(5) . ? C44 H44A 0.99(4) . ? C44 H44B 1.01(4) . ? C44 H44C 1.09(4) . ? C1 N2 1.354(4) . ? C1 N1 1.377(4) . ? C1 Ni1 1.924(3) . ? C2 C3 1.330(5) . ? C2 N1 1.387(4) . ? C2 H2 0.9500 . ? C3 N2 1.388(4) . ? C3 H3 0.9500 . ? C4 N2 1.462(4) . ? C4 C5 1.509(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N3 1.451(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.328(5) . ? C6 N3 1.385(4) . ? C6 H6 0.9500 . ? C7 N4 1.398(4) . ? C7 H7 0.9500 . ? C8 N3 1.375(4) . ? C8 N4 1.403(4) . ? C8 Ni1 1.916(3) . ? C8 Ni2 2.123(3) . ? C9 N6 1.344(4) . ? C9 C10 1.388(4) . ? C9 N4 1.396(4) . ? C10 C11 1.371(5) . ? C10 H10 0.9500 . ? C11 C12 1.385(5) . ? C11 H11 0.9500 . ? C12 C13 1.374(5) . ? C12 H12 0.9500 . ? C13 N6 1.348(4) . ? C13 H13 0.9500 . ? C14 N5 1.341(4) . ? C14 C15 1.384(5) . ? C14 N1 1.392(4) . ? C15 C16 1.372(5) . ? C15 H15 0.9500 . ? C16 C17 1.381(5) . ? C16 H16 0.9500 . ? C17 C18 1.368(5) . ? C17 H17 0.9500 . ? C18 N5 1.355(4) . ? C18 H18 0.9500 . ? C19 N8 1.365(4) . ? C19 N7 1.377(4) . ? C19 Ni2 1.925(3) . ? C20 C21 1.324(5) . ? C20 N7 1.393(4) . ? C20 H20 0.9500 . ? C21 N8 1.392(4) . ? C21 H21 0.9500 . ? C22 N8 1.457(4) . ? C22 C23 1.511(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N9 1.453(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.328(5) . ? C24 N9 1.388(4) . ? C24 H24 0.9500 . ? C25 N10 1.396(4) . ? C25 H25 0.9500 . ? C26 N9 1.376(4) . ? C26 N10 1.398(4) . ? C26 Ni2 1.909(3) . ? C26 Ni1 2.123(3) . ? C27 N12 1.338(4) . ? C27 C28 1.381(5) . ? C27 N10 1.399(4) . ? C28 C29 1.373(5) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C31 N12 1.348(4) . ? C31 H31 0.9500 . ? C32 N11 1.345(4) . ? C32 C33 1.372(5) . ? C32 N7 1.393(4) . ? C33 C34 1.377(5) . ? C33 H33 0.9500 . ? C34 C35 1.386(5) . ? C34 H34 0.9500 . ? C35 C36 1.370(5) . ? C35 H35 0.9500 . ? C36 N11 1.350(4) . ? C36 H36 0.9500 . ? C37 O4 1.420(5) . ? C37 H37A 1.01(4) . ? C37 H37B 1.00(4) . ? C37 H37C 1.00(4) . ? C38 O4 1.413(4) . ? C38 C39 1.494(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 O3 1.416(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 O3 1.415(5) . ? C40 H40A 0.99(4) . ? C40 H40B 0.89(4) . ? C40 H40C 1.04(4) . ? C41 O1 1.426(5) . ? C41 H41A 0.96(4) . ? C41 H41B 1.01(4) . ? C41 H41C 1.02(4) . ? C42 O1 1.419(4) . ? C42 C43 1.491(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 O2 1.422(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? N5 Ni1 2.020(3) . ? N6 Ni1 2.130(3) . ? N11 Ni2 2.009(3) . ? N12 Ni2 2.152(3) . ? Ni1 Ni2 2.5790(6) . ? F7 P2 1.591(2) . ? F8 P2 1.593(2) . ? F9 P2 1.591(2) . ? F10 P2 1.584(2) . ? F11 P2 1.567(3) . ? F12 P2 1.573(3) . ? F1 P1 1.585(2) . ? F2 P1 1.584(2) . ? F3 P1 1.580(2) . ? F4 P1 1.584(2) . ? F5 P1 1.599(2) . ? F6 P1 1.563(3) . ? 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 C31 C30 C29 119.2(3) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? O2 C44 H44A 106(2) . . ? O2 C44 H44B 106(2) . . ? H44A C44 H44B 119(3) . . ? O2 C44 H44C 107(2) . . ? H44A C44 H44C 105(3) . . ? H44B C44 H44C 114(3) . . ? N2 C1 N1 102.9(3) . . ? N2 C1 Ni1 144.7(3) . . ? N1 C1 Ni1 112.3(2) . . ? C3 C2 N1 105.7(3) . . ? C3 C2 H2 127.2 . . ? N1 C2 H2 127.2 . . ? C2 C3 N2 108.0(3) . . ? C2 C3 H3 126.0 . . ? N2 C3 H3 126.0 . . ? N2 C4 C5 113.9(3) . . ? N2 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? N2 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? N3 C5 C4 111.3(3) . . ? N3 C5 H5A 109.4 . . ? C4 C5 H5A 109.4 . . ? N3 C5 H5B 109.4 . . ? C4 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C7 C6 N3 108.6(3) . . ? C7 C6 H6 125.7 . . ? N3 C6 H6 125.7 . . ? C6 C7 N4 106.1(3) . . ? C6 C7 H7 126.9 . . ? N4 C7 H7 126.9 . . ? N3 C8 N4 101.8(2) . . ? N3 C8 Ni1 130.2(2) . . ? N4 C8 Ni1 112.4(2) . . ? N3 C8 Ni2 112.8(2) . . ? N4 C8 Ni2 121.2(2) . . ? Ni1 C8 Ni2 79.19(11) . . ? N6 C9 C10 124.3(3) . . ? N6 C9 N4 113.4(3) . . ? C10 C9 N4 122.4(3) . . ? C11 C10 C9 117.7(4) . . ? C11 C10 H10 121.2 . . ? C9 C10 H10 121.2 . . ? C10 C11 C12 119.4(3) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C13 C12 C11 119.1(3) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? N6 C13 C12 123.0(4) . . ? N6 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? N5 C14 C15 124.0(3) . . ? N5 C14 N1 112.7(3) . . ? C15 C14 N1 123.3(3) . . ? C16 C15 C14 118.0(3) . . ? C16 C15 H15 121.0 . . ? C14 C15 H15 121.0 . . ? C15 C16 C17 119.3(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 119.2(3) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? N5 C18 C17 123.0(3) . . ? N5 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? N8 C19 N7 102.7(3) . . ? N8 C19 Ni2 144.9(3) . . ? N7 C19 Ni2 112.4(2) . . ? C21 C20 N7 105.9(3) . . ? C21 C20 H20 127.1 . . ? N7 C20 H20 127.1 . . ? C20 C21 N8 108.3(3) . . ? C20 C21 H21 125.9 . . ? N8 C21 H21 125.9 . . ? N8 C22 C23 114.2(3) . . ? N8 C22 H22A 108.7 . . ? C23 C22 H22A 108.7 . . ? N8 C22 H22B 108.7 . . ? C23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? N9 C23 C22 111.8(3) . . ? N9 C23 H23A 109.3 . . ? C22 C23 H23A 109.3 . . ? N9 C23 H23B 109.3 . . ? C22 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? C25 C24 N9 108.3(3) . . ? C25 C24 H24 125.9 . . ? N9 C24 H24 125.9 . . ? C24 C25 N10 106.4(3) . . ? C24 C25 H25 126.8 . . ? N10 C25 H25 126.8 . . ? N9 C26 N10 102.1(3) . . ? N9 C26 Ni2 129.8(2) . . ? N10 C26 Ni2 112.6(2) . . ? N9 C26 Ni1 113.8(2) . . ? N10 C26 Ni1 119.6(2) . . ? Ni2 C26 Ni1 79.32(12) . . ? N12 C27 C28 124.5(3) . . ? N12 C27 N10 113.1(3) . . ? C28 C27 N10 122.4(3) . . ? C29 C28 C27 118.1(4) . . ? C29 C28 H28 120.9 . . ? C27 C28 H28 120.9 . . ? C28 C29 C30 118.8(3) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? N12 C31 C30 123.4(4) . . ? N12 C31 H31 118.3 . . ? C30 C31 H31 118.3 . . ? N11 C32 C33 124.3(3) . . ? N11 C32 N7 112.6(3) . . ? C33 C32 N7 123.1(3) . . ? C32 C33 C34 117.9(3) . . ? C32 C33 H33 121.1 . . ? C34 C33 H33 121.1 . . ? C33 C34 C35 119.4(4) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C36 C35 C34 118.9(3) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? N11 C36 C35 123.0(3) . . ? N11 C36 H36 118.5 . . ? C35 C36 H36 118.5 . . ? O4 C37 H37A 105(2) . . ? O4 C37 H37B 111(2) . . ? H37A C37 H37B 105(3) . . ? O4 C37 H37C 107(2) . . ? H37A C37 H37C 118(3) . . ? H37B C37 H37C 110(3) . . ? O4 C38 C39 109.4(3) . . ? O4 C38 H38A 109.8 . . ? C39 C38 H38A 109.8 . . ? O4 C38 H38B 109.8 . . ? C39 C38 H38B 109.8 . . ? H38A C38 H38B 108.2 . . ? O3 C39 C38 108.9(3) . . ? O3 C39 H39A 109.9 . . ? C38 C39 H39A 109.9 . . ? O3 C39 H39B 109.9 . . ? C38 C39 H39B 109.9 . . ? H39A C39 H39B 108.3 . . ? O3 C40 H40A 104(2) . . ? O3 C40 H40B 111(3) . . ? H40A C40 H40B 110(3) . . ? O3 C40 H40C 108(2) . . ? H40A C40 H40C 120(3) . . ? H40B C40 H40C 104(3) . . ? O1 C41 H41A 105(2) . . ? O1 C41 H41B 100(2) . . ? H41A C41 H41B 117(3) . . ? O1 C41 H41C 107(2) . . ? H41A C41 H41C 119(3) . . ? H41B C41 H41C 106(3) . . ? O1 C42 C43 110.7(3) . . ? O1 C42 H42A 109.5 . . ? C43 C42 H42A 109.5 . . ? O1 C42 H42B 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? O2 C43 C42 113.8(3) . . ? O2 C43 H43A 108.8 . . ? C42 C43 H43A 108.8 . . ? O2 C43 H43B 108.8 . . ? C42 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? C1 N1 C2 112.1(3) . . ? C1 N1 C14 119.2(3) . . ? C2 N1 C14 128.5(3) . . ? C1 N2 C3 111.3(3) . . ? C1 N2 C4 128.1(3) . . ? C3 N2 C4 120.5(3) . . ? C8 N3 C6 111.8(3) . . ? C8 N3 C5 122.3(3) . . ? C6 N3 C5 124.2(3) . . ? C9 N4 C7 126.3(3) . . ? C9 N4 C8 118.9(3) . . ? C7 N4 C8 111.7(3) . . ? C14 N5 C18 116.4(3) . . ? C14 N5 Ni1 114.0(2) . . ? C18 N5 Ni1 129.5(2) . . ? C9 N6 C13 116.4(3) . . ? C9 N6 Ni1 111.6(2) . . ? C13 N6 Ni1 131.9(2) . . ? C19 N7 C32 118.8(3) . . ? C19 N7 C20 112.1(3) . . ? C32 N7 C20 129.0(3) . . ? C19 N8 C21 111.1(3) . . ? C19 N8 C22 128.3(3) . . ? C21 N8 C22 120.5(3) . . ? C26 N9 C24 111.6(3) . . ? C26 N9 C23 123.0(3) . . ? C24 N9 C23 124.3(3) . . ? C25 N10 C26 111.6(3) . . ? C25 N10 C27 127.2(3) . . ? C26 N10 C27 118.9(3) . . ? C32 N11 C36 116.6(3) . . ? C32 N11 Ni2 114.1(2) . . ? C36 N11 Ni2 129.1(2) . . ? C27 N12 C31 116.0(3) . . ? C27 N12 Ni2 111.0(2) . . ? C31 N12 Ni2 132.1(2) . . ? C8 Ni1 C1 94.64(13) . . ? C8 Ni1 N5 171.75(12) . . ? C1 Ni1 N5 81.67(12) . . ? C8 Ni1 C26 100.15(13) . . ? C1 Ni1 C26 130.35(13) . . ? N5 Ni1 C26 87.81(12) . . ? C8 Ni1 N6 80.81(12) . . ? C1 Ni1 N6 128.18(12) . . ? N5 Ni1 N6 95.62(11) . . ? C26 Ni1 N6 100.99(11) . . ? C8 Ni1 Ni2 53.94(9) . . ? C1 Ni1 Ni2 120.98(10) . . ? N5 Ni1 Ni2 134.21(8) . . ? C26 Ni1 Ni2 46.68(9) . . ? N6 Ni1 Ni2 97.71(7) . . ? C26 Ni2 C19 94.39(14) . . ? C26 Ni2 N11 170.27(12) . . ? C19 Ni2 N11 81.77(13) . . ? C26 Ni2 C8 100.40(13) . . ? C19 Ni2 C8 131.15(12) . . ? N11 Ni2 C8 88.78(11) . . ? C26 Ni2 N12 80.65(12) . . ? C19 Ni2 N12 128.31(12) . . ? N11 Ni2 N12 94.66(11) . . ? C8 Ni2 N12 100.07(11) . . ? C26 Ni2 Ni1 54.00(9) . . ? C19 Ni2 Ni1 121.44(10) . . ? N11 Ni2 Ni1 135.46(8) . . ? C8 Ni2 Ni1 46.87(9) . . ? N12 Ni2 Ni1 96.88(7) . . ? C42 O1 C41 112.0(3) . . ? C43 O2 C44 114.7(3) . . ? C40 O3 C39 112.1(3) . . ? C38 O4 C37 112.1(3) . . ? F11 P2 F12 90.5(2) . . ? F11 P2 F10 90.56(17) . . ? F12 P2 F10 178.83(18) . . ? F11 P2 F9 179.52(16) . . ? F12 P2 F9 89.78(17) . . ? F10 P2 F9 89.15(15) . . ? F11 P2 F7 90.81(15) . . ? F12 P2 F7 90.02(15) . . ? F10 P2 F7 90.46(15) . . ? F9 P2 F7 89.58(13) . . ? F11 P2 F8 90.34(14) . . ? F12 P2 F8 90.19(14) . . ? F10 P2 F8 89.32(13) . . ? F9 P2 F8 89.27(12) . . ? F7 P2 F8 178.83(15) . . ? F6 P1 F3 91.34(17) . . ? F6 P1 F2 90.32(17) . . ? F3 P1 F2 90.47(14) . . ? F6 P1 F4 179.07(19) . . ? F3 P1 F4 89.56(14) . . ? F2 P1 F4 89.47(15) . . ? F6 P1 F1 91.00(17) . . ? F3 P1 F1 91.03(14) . . ? F2 P1 F1 177.98(16) . . ? F4 P1 F1 89.19(15) . . ? F6 P1 F5 90.11(17) . . ? F3 P1 F5 178.46(16) . . ? F2 P1 F5 90.03(13) . . ? F4 P1 F5 88.98(14) . . ? F1 P1 F5 88.44(12) . . ? 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 C2 C3 N2 -0.2(4) . . . . ? N2 C4 C5 N3 74.2(4) . . . . ? N3 C6 C7 N4 -0.5(4) . . . . ? N6 C9 C10 C11 2.0(5) . . . . ? N4 C9 C10 C11 -176.5(3) . . . . ? C9 C10 C11 C12 -3.2(5) . . . . ? C10 C11 C12 C13 1.7(5) . . . . ? C11 C12 C13 N6 1.3(5) . . . . ? N5 C14 C15 C16 0.6(5) . . . . ? N1 C14 C15 C16 -179.0(3) . . . . ? C14 C15 C16 C17 -0.3(5) . . . . ? C15 C16 C17 C18 -0.4(6) . . . . ? C16 C17 C18 N5 0.9(6) . . . . ? N7 C20 C21 N8 0.6(4) . . . . ? N8 C22 C23 N9 71.4(4) . . . . ? N9 C24 C25 N10 -0.2(4) . . . . ? N12 C27 C28 C29 1.4(5) . . . . ? N10 C27 C28 C29 -178.9(3) . . . . ? C27 C28 C29 C30 -1.7(5) . . . . ? C31 C30 C29 C28 0.6(5) . . . . ? C29 C30 C31 N12 1.2(5) . . . . ? N11 C32 C33 C34 0.0(5) . . . . ? N7 C32 C33 C34 -179.7(3) . . . . ? C32 C33 C34 C35 0.7(5) . . . . ? C33 C34 C35 C36 -0.8(6) . . . . ? C34 C35 C36 N11 0.2(6) . . . . ? O4 C38 C39 O3 65.3(4) . . . . ? O1 C42 C43 O2 -68.0(4) . . . . ? N2 C1 N1 C2 1.2(4) . . . . ? Ni1 C1 N1 C2 178.4(2) . . . . ? N2 C1 N1 C14 -173.9(3) . . . . ? Ni1 C1 N1 C14 3.3(4) . . . . ? C3 C2 N1 C1 -0.6(4) . . . . ? C3 C2 N1 C14 173.8(3) . . . . ? N5 C14 N1 C1 -0.9(4) . . . . ? C15 C14 N1 C1 178.7(3) . . . . ? N5 C14 N1 C2 -175.1(3) . . . . ? C15 C14 N1 C2 4.6(5) . . . . ? N1 C1 N2 C3 -1.2(4) . . . . ? Ni1 C1 N2 C3 -176.8(3) . . . . ? N1 C1 N2 C4 175.7(3) . . . . ? Ni1 C1 N2 C4 0.1(6) . . . . ? C2 C3 N2 C1 0.9(4) . . . . ? C2 C3 N2 C4 -176.3(3) . . . . ? C5 C4 N2 C1 -20.9(5) . . . . ? C5 C4 N2 C3 155.8(3) . . . . ? N4 C8 N3 C6 1.3(3) . . . . ? Ni1 C8 N3 C6 -132.2(3) . . . . ? Ni2 C8 N3 C6 132.8(2) . . . . ? N4 C8 N3 C5 167.2(3) . . . . ? Ni1 C8 N3 C5 33.7(4) . . . . ? Ni2 C8 N3 C5 -61.4(3) . . . . ? C7 C6 N3 C8 -0.6(4) . . . . ? C7 C6 N3 C5 -166.1(3) . . . . ? C4 C5 N3 C8 -93.6(3) . . . . ? C4 C5 N3 C6 70.5(4) . . . . ? N6 C9 N4 C7 -143.3(3) . . . . ? C10 C9 N4 C7 35.4(5) . . . . ? N6 C9 N4 C8 15.1(4) . . . . ? C10 C9 N4 C8 -166.2(3) . . . . ? C6 C7 N4 C9 161.1(3) . . . . ? C6 C7 N4 C8 1.4(4) . . . . ? N3 C8 N4 C9 -163.1(3) . . . . ? Ni1 C8 N4 C9 -19.9(3) . . . . ? Ni2 C8 N4 C9 70.9(3) . . . . ? N3 C8 N4 C7 -1.7(3) . . . . ? Ni1 C8 N4 C7 141.5(2) . . . . ? Ni2 C8 N4 C7 -127.7(3) . . . . ? C15 C14 N5 C18 -0.2(5) . . . . ? N1 C14 N5 C18 179.4(3) . . . . ? C15 C14 N5 Ni1 178.5(3) . . . . ? N1 C14 N5 Ni1 -1.9(3) . . . . ? C17 C18 N5 C14 -0.5(5) . . . . ? C17 C18 N5 Ni1 -179.0(3) . . . . ? C10 C9 N6 C13 0.8(5) . . . . ? N4 C9 N6 C13 179.4(3) . . . . ? C10 C9 N6 Ni1 178.0(3) . . . . ? N4 C9 N6 Ni1 -3.4(3) . . . . ? C12 C13 N6 C9 -2.5(5) . . . . ? C12 C13 N6 Ni1 -178.9(3) . . . . ? N8 C19 N7 C32 -175.7(3) . . . . ? Ni2 C19 N7 C32 1.4(4) . . . . ? N8 C19 N7 C20 1.5(3) . . . . ? Ni2 C19 N7 C20 178.5(2) . . . . ? N11 C32 N7 C19 3.2(4) . . . . ? C33 C32 N7 C19 -177.1(3) . . . . ? N11 C32 N7 C20 -173.4(3) . . . . ? C33 C32 N7 C20 6.3(5) . . . . ? C21 C20 N7 C19 -1.4(4) . . . . ? C21 C20 N7 C32 175.4(3) . . . . ? N7 C19 N8 C21 -1.1(3) . . . . ? Ni2 C19 N8 C21 -176.3(3) . . . . ? N7 C19 N8 C22 176.9(3) . . . . ? Ni2 C19 N8 C22 1.7(6) . . . . ? C20 C21 N8 C19 0.3(4) . . . . ? C20 C21 N8 C22 -177.9(3) . . . . ? C23 C22 N8 C19 -19.3(5) . . . . ? C23 C22 N8 C21 158.5(3) . . . . ? N10 C26 N9 C24 1.3(4) . . . . ? Ni2 C26 N9 C24 -132.5(3) . . . . ? Ni1 C26 N9 C24 131.6(3) . . . . ? N10 C26 N9 C23 169.7(3) . . . . ? Ni2 C26 N9 C23 36.0(4) . . . . ? Ni1 C26 N9 C23 -59.9(4) . . . . ? C25 C24 N9 C26 -0.7(4) . . . . ? C25 C24 N9 C23 -169.0(3) . . . . ? C22 C23 N9 C26 -94.2(4) . . . . ? C22 C23 N9 C24 72.8(4) . . . . ? C24 C25 N10 C26 1.0(4) . . . . ? C24 C25 N10 C27 163.0(3) . . . . ? N9 C26 N10 C25 -1.4(4) . . . . ? Ni2 C26 N10 C25 141.6(2) . . . . ? Ni1 C26 N10 C25 -128.0(3) . . . . ? N9 C26 N10 C27 -165.1(3) . . . . ? Ni2 C26 N10 C27 -22.0(4) . . . . ? Ni1 C26 N10 C27 68.3(3) . . . . ? N12 C27 N10 C25 -140.6(3) . . . . ? C28 C27 N10 C25 39.7(5) . . . . ? N12 C27 N10 C26 20.2(4) . . . . ? C28 C27 N10 C26 -159.5(3) . . . . ? C33 C32 N11 C36 -0.6(5) . . . . ? N7 C32 N11 C36 179.1(3) . . . . ? C33 C32 N11 Ni2 174.3(3) . . . . ? N7 C32 N11 Ni2 -6.0(3) . . . . ? C35 C36 N11 C32 0.6(5) . . . . ? C35 C36 N11 Ni2 -173.5(3) . . . . ? C28 C27 N12 C31 0.3(5) . . . . ? N10 C27 N12 C31 -179.4(3) . . . . ? C28 C27 N12 Ni2 171.2(3) . . . . ? N10 C27 N12 Ni2 -8.5(3) . . . . ? C30 C31 N12 C27 -1.6(5) . . . . ? C30 C31 N12 Ni2 -170.1(3) . . . . ? N3 C8 Ni1 C1 14.7(3) . . . . ? N4 C8 Ni1 C1 -115.2(2) . . . . ? Ni2 C8 Ni1 C1 125.42(11) . . . . ? N3 C8 Ni1 N5 77.8(9) . . . . ? N4 C8 Ni1 N5 -52.0(9) . . . . ? Ni2 C8 Ni1 N5 -171.5(8) . . . . ? N3 C8 Ni1 C26 -117.7(3) . . . . ? N4 C8 Ni1 C26 112.4(2) . . . . ? Ni2 C8 Ni1 C26 -6.99(12) . . . . ? N3 C8 Ni1 N6 142.6(3) . . . . ? N4 C8 Ni1 N6 12.8(2) . . . . ? Ni2 C8 Ni1 N6 -106.62(10) . . . . ? N3 C8 Ni1 Ni2 -110.7(3) . . . . ? N4 C8 Ni1 Ni2 119.4(2) . . . . ? N2 C1 Ni1 C8 -15.3(4) . . . . ? N1 C1 Ni1 C8 169.3(2) . . . . ? N2 C1 Ni1 N5 172.1(4) . . . . ? N1 C1 Ni1 N5 -3.2(2) . . . . ? N2 C1 Ni1 C26 92.2(4) . . . . ? N1 C1 Ni1 C26 -83.1(3) . . . . ? N2 C1 Ni1 N6 -97.3(4) . . . . ? N1 C1 Ni1 N6 87.4(3) . . . . ? N2 C1 Ni1 Ni2 34.9(4) . . . . ? N1 C1 Ni1 Ni2 -140.45(19) . . . . ? C14 N5 Ni1 C8 -61.1(9) . . . . ? C18 N5 Ni1 C8 117.5(8) . . . . ? C14 N5 Ni1 C1 2.9(2) . . . . ? C18 N5 Ni1 C1 -178.6(3) . . . . ? C14 N5 Ni1 C26 134.2(2) . . . . ? C18 N5 Ni1 C26 -47.3(3) . . . . ? C14 N5 Ni1 N6 -124.9(2) . . . . ? C18 N5 Ni1 N6 53.6(3) . . . . ? C14 N5 Ni1 Ni2 128.59(19) . . . . ? C18 N5 Ni1 Ni2 -52.9(3) . . . . ? N9 C26 Ni1 C8 136.7(2) . . . . ? N10 C26 Ni1 C8 -102.3(3) . . . . ? Ni2 C26 Ni1 C8 7.77(13) . . . . ? N9 C26 Ni1 C1 31.7(3) . . . . ? N10 C26 Ni1 C1 152.6(2) . . . . ? Ni2 C26 Ni1 C1 -97.30(17) . . . . ? N9 C26 Ni1 N5 -45.5(2) . . . . ? N10 C26 Ni1 N5 75.5(3) . . . . ? Ni2 C26 Ni1 N5 -174.43(11) . . . . ? N9 C26 Ni1 N6 -140.8(2) . . . . ? N10 C26 Ni1 N6 -19.8(3) . . . . ? Ni2 C26 Ni1 N6 90.27(11) . . . . ? N9 C26 Ni1 Ni2 129.0(3) . . . . ? N10 C26 Ni1 Ni2 -110.1(3) . . . . ? C9 N6 Ni1 C8 -5.4(2) . . . . ? C13 N6 Ni1 C8 171.2(3) . . . . ? C9 N6 Ni1 C1 83.3(3) . . . . ? C13 N6 Ni1 C1 -100.2(3) . . . . ? C9 N6 Ni1 N5 167.1(2) . . . . ? C13 N6 Ni1 N5 -16.4(3) . . . . ? C9 N6 Ni1 C26 -104.1(2) . . . . ? C13 N6 Ni1 C26 72.5(3) . . . . ? C9 N6 Ni1 Ni2 -56.8(2) . . . . ? C13 N6 Ni1 Ni2 119.7(3) . . . . ? N9 C26 Ni2 C19 14.1(3) . . . . ? N10 C26 Ni2 C19 -116.0(2) . . . . ? Ni1 C26 Ni2 C19 126.22(11) . . . . ? N9 C26 Ni2 N11 80.4(8) . . . . ? N10 C26 Ni2 N11 -49.7(8) . . . . ? Ni1 C26 Ni2 N11 -167.5(7) . . . . ? N9 C26 Ni2 C8 -119.2(3) . . . . ? N10 C26 Ni2 C8 110.8(2) . . . . ? Ni1 C26 Ni2 C8 -7.02(12) . . . . ? N9 C26 Ni2 N12 142.2(3) . . . . ? N10 C26 Ni2 N12 12.1(2) . . . . ? Ni1 C26 Ni2 N12 -105.65(10) . . . . ? N9 C26 Ni2 Ni1 -112.1(3) . . . . ? N10 C26 Ni2 Ni1 117.8(2) . . . . ? N8 C19 Ni2 C26 -17.6(4) . . . . ? N7 C19 Ni2 C26 167.5(2) . . . . ? N8 C19 Ni2 N11 171.4(4) . . . . ? N7 C19 Ni2 N11 -3.6(2) . . . . ? N8 C19 Ni2 C8 90.4(4) . . . . ? N7 C19 Ni2 C8 -84.6(3) . . . . ? N8 C19 Ni2 N12 -99.1(4) . . . . ? N7 C19 Ni2 N12 85.9(3) . . . . ? N8 C19 Ni2 Ni1 32.3(4) . . . . ? N7 C19 Ni2 Ni1 -142.64(18) . . . . ? C32 N11 Ni2 C26 -61.9(8) . . . . ? C36 N11 Ni2 C26 112.3(7) . . . . ? C32 N11 Ni2 C19 5.5(2) . . . . ? C36 N11 Ni2 C19 179.6(3) . . . . ? C32 N11 Ni2 C8 137.4(2) . . . . ? C36 N11 Ni2 C8 -48.5(3) . . . . ? C32 N11 Ni2 N12 -122.6(2) . . . . ? C36 N11 Ni2 N12 51.5(3) . . . . ? C32 N11 Ni2 Ni1 132.65(19) . . . . ? C36 N11 Ni2 Ni1 -53.2(3) . . . . ? N3 C8 Ni2 C26 137.1(2) . . . . ? N4 C8 Ni2 C26 -102.0(3) . . . . ? Ni1 C8 Ni2 C26 7.78(13) . . . . ? N3 C8 Ni2 C19 31.8(3) . . . . ? N4 C8 Ni2 C19 152.7(2) . . . . ? Ni1 C8 Ni2 C19 -97.51(17) . . . . ? N3 C8 Ni2 N11 -46.2(2) . . . . ? N4 C8 Ni2 N11 74.7(3) . . . . ? Ni1 C8 Ni2 N11 -175.46(11) . . . . ? N3 C8 Ni2 N12 -140.7(2) . . . . ? N4 C8 Ni2 N12 -19.8(3) . . . . ? Ni1 C8 Ni2 N12 90.02(11) . . . . ? N3 C8 Ni2 Ni1 129.3(3) . . . . ? N4 C8 Ni2 Ni1 -109.8(3) . . . . ? C27 N12 Ni2 C26 -2.1(2) . . . . ? C31 N12 Ni2 C26 166.8(3) . . . . ? C27 N12 Ni2 C19 86.1(3) . . . . ? C31 N12 Ni2 C19 -104.9(3) . . . . ? C27 N12 Ni2 N11 169.3(2) . . . . ? C31 N12 Ni2 N11 -21.7(3) . . . . ? C27 N12 Ni2 C8 -101.1(2) . . . . ? C31 N12 Ni2 C8 67.8(3) . . . . ? C27 N12 Ni2 Ni1 -53.8(2) . . . . ? C31 N12 Ni2 Ni1 115.2(3) . . . . ? C8 Ni1 Ni2 C26 -170.52(16) . . . . ? C1 Ni1 Ni2 C26 118.16(16) . . . . ? N5 Ni1 Ni2 C26 7.77(16) . . . . ? N6 Ni1 Ni2 C26 -97.86(14) . . . . ? C8 Ni1 Ni2 C19 118.95(16) . . . . ? C1 Ni1 Ni2 C19 47.63(16) . . . . ? N5 Ni1 Ni2 C19 -62.76(16) . . . . ? C26 Ni1 Ni2 C19 -70.53(16) . . . . ? N6 Ni1 Ni2 C19 -168.39(13) . . . . ? C8 Ni1 Ni2 N11 6.48(15) . . . . ? C1 Ni1 Ni2 N11 -64.84(16) . . . . ? N5 Ni1 Ni2 N11 -175.23(15) . . . . ? C26 Ni1 Ni2 N11 177.00(16) . . . . ? N6 Ni1 Ni2 N11 79.14(13) . . . . ? C1 Ni1 Ni2 C8 -71.32(16) . . . . ? N5 Ni1 Ni2 C8 178.30(15) . . . . ? C26 Ni1 Ni2 C8 170.52(16) . . . . ? N6 Ni1 Ni2 C8 72.66(13) . . . . ? C8 Ni1 Ni2 N12 -97.38(13) . . . . ? C1 Ni1 Ni2 N12 -168.69(13) . . . . ? N5 Ni1 Ni2 N12 80.92(13) . . . . ? C26 Ni1 Ni2 N12 73.15(13) . . . . ? N6 Ni1 Ni2 N12 -24.71(10) . . . . ? C43 C42 O1 C41 175.6(3) . . . . ? C42 C43 O2 C44 91.2(4) . . . . ? C38 C39 O3 C40 178.4(3) . . . . ? C39 C38 O4 C37 -174.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.492 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.076 # Attachment '- methyldimer.cif' data_methyldimer _database_code_depnum_ccdc_archive 'CCDC 809511' #TrackingRef '- methyldimer.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H28 N12 Ni2, 2(C F3 O3 S)' _chemical_formula_sum 'C36 H28 F6 N12 Ni2 O6 S2' _chemical_formula_weight 1020.24 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' S S 0.1246 0.1234 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.4040(17) _cell_length_b 31.424(7) _cell_length_c 16.616(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.615(4) _cell_angle_gamma 90.00 _cell_volume 3822.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 32966 _cell_measurement_theta_min 2.480 _cell_measurement_theta_max 25.181 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 1.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6947 _exptl_absorpt_correction_T_max 0.9539 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 32458 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6961 _reflns_number_gt 4608 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2009.3' _computing_cell_refinement 'Bruker APEX2 v. 2009.3' _computing_data_reduction 'Bruker APEX2 v. 2009.3' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material CIFTAB _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^)+(0.0528P)^2^+2.2201P] 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 6961 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 C1 C 0.6215(6) 0.30506(16) 0.1515(3) 0.0333(12) Uani 1 1 d . . . H1 H 0.6442 0.3276 0.1162 0.040 Uiso 1 1 calc R . . C2 C 0.6450(6) 0.26400(16) 0.1275(3) 0.0385(13) Uani 1 1 d . . . H2 H 0.6850 0.2585 0.0768 0.046 Uiso 1 1 calc R . . C3 C 0.6103(6) 0.23056(17) 0.1772(3) 0.0413(13) Uani 1 1 d . . . H3 H 0.6242 0.2019 0.1607 0.050 Uiso 1 1 calc R . . C4 C 0.5555(6) 0.23948(15) 0.2508(3) 0.0377(12) Uani 1 1 d . . . H4 H 0.5298 0.2173 0.2862 0.045 Uiso 1 1 calc R . . C5 C 0.5389(6) 0.28179(14) 0.2720(3) 0.0263(10) Uani 1 1 d . . . C6 C 0.4626(6) 0.27224(15) 0.4147(3) 0.0315(11) Uani 1 1 d . . . H6 H 0.4723 0.2423 0.4216 0.038 Uiso 1 1 calc R . . C7 C 0.4208(6) 0.30035(14) 0.4688(3) 0.0308(11) Uani 1 1 d . . . H7 H 0.3940 0.2942 0.5218 0.037 Uiso 1 1 calc R . . C8 C 0.4649(5) 0.33837(14) 0.3570(2) 0.0253(10) Uani 1 1 d . . . C9 C 0.3835(6) 0.37826(14) 0.4788(3) 0.0326(11) Uani 1 1 d . . . H9A H 0.4942 0.3862 0.5170 0.039 Uiso 1 1 calc R . . H9B H 0.2864 0.3712 0.5116 0.039 Uiso 1 1 calc R . . C10 C 0.3535(6) 0.45606(14) 0.4560(3) 0.0282(10) Uani 1 1 d . . . H10 H 0.4139 0.4641 0.5084 0.034 Uiso 1 1 calc R . . C11 C 0.2808(6) 0.48265(14) 0.3970(3) 0.0298(11) Uani 1 1 d . . . H11 H 0.2791 0.5129 0.3990 0.036 Uiso 1 1 calc R . . C12 C 0.2350(5) 0.41397(14) 0.3498(2) 0.0246(10) Uani 1 1 d . . . C13 C 0.1136(6) 0.46774(14) 0.2556(3) 0.0261(10) Uani 1 1 d . . . C14 C 0.0940(6) 0.50885(15) 0.2260(3) 0.0335(11) Uani 1 1 d . . . H14 H 0.1468 0.5323 0.2572 0.040 Uiso 1 1 calc R . . C15 C -0.0050(7) 0.51465(16) 0.1497(3) 0.0411(13) Uani 1 1 d . . . H15 H -0.0217 0.5424 0.1272 0.049 Uiso 1 1 calc R . . C16 C -0.0796(6) 0.47982(16) 0.1063(3) 0.0396(13) Uani 1 1 d . . . H16 H -0.1507 0.4835 0.0543 0.047 Uiso 1 1 calc R . . C17 C -0.0503(6) 0.43976(15) 0.1388(3) 0.0321(11) Uani 1 1 d . . . H17 H -0.1003 0.4160 0.1078 0.039 Uiso 1 1 calc R . . C18 C 0.7365(6) 0.42890(15) 0.3795(3) 0.0301(11) Uani 1 1 d . . . H18 H 0.7615 0.4052 0.4149 0.036 Uiso 1 1 calc R . . C19 C 0.8089(6) 0.46793(15) 0.4049(3) 0.0316(11) Uani 1 1 d . . . H19 H 0.8836 0.4710 0.4563 0.038 Uiso 1 1 calc R . . C20 C 0.7705(6) 0.50242(15) 0.3540(3) 0.0351(12) Uani 1 1 d . . . H20 H 0.8173 0.5297 0.3706 0.042 Uiso 1 1 calc R . . C21 C 0.6641(6) 0.49732(15) 0.2792(3) 0.0335(11) Uani 1 1 d . . . H21 H 0.6350 0.5208 0.2437 0.040 Uiso 1 1 calc R . . C22 C 0.6015(6) 0.45711(14) 0.2578(3) 0.0256(10) Uani 1 1 d . . . C23 C 0.4425(6) 0.47161(16) 0.1136(3) 0.0356(12) Uani 1 1 d . . . H23 H 0.4674 0.5009 0.1068 0.043 Uiso 1 1 calc R . . C24 C 0.3486(6) 0.44542(16) 0.0593(3) 0.0352(12) Uani 1 1 d . . . H24 H 0.2953 0.4529 0.0055 0.042 Uiso 1 1 calc R . . C25 C 0.4314(6) 0.40560(14) 0.1723(3) 0.0279(11) Uani 1 1 d . . . C26 C 0.2514(7) 0.37030(16) 0.0489(3) 0.0428(13) Uani 1 1 d . . . H26A H 0.3354 0.3581 0.0139 0.051 Uiso 1 1 calc R . . H26B H 0.1429 0.3813 0.0128 0.051 Uiso 1 1 calc R . . C27 C 0.1744(6) 0.29523(16) 0.0713(3) 0.0352(12) Uani 1 1 d . . . H27 H 0.1968 0.2854 0.0197 0.042 Uiso 1 1 calc R . . C28 C 0.1189(6) 0.27132(16) 0.1297(3) 0.0368(12) Uani 1 1 d . . . H28 H 0.0948 0.2416 0.1277 0.044 Uiso 1 1 calc R . . C29 C 0.1513(6) 0.33978(14) 0.1763(3) 0.0262(10) Uani 1 1 d . . . C30 C 0.0509(5) 0.29122(14) 0.2702(3) 0.0264(10) Uani 1 1 d . . . C31 C 0.0131(6) 0.25144(16) 0.2983(3) 0.0383(12) Uani 1 1 d . . . H31 H 0.0256 0.2268 0.2665 0.046 Uiso 1 1 calc R . . C32 C -0.0433(6) 0.24803(16) 0.3735(3) 0.0379(12) Uani 1 1 d . . . H32 H -0.0713 0.2211 0.3944 0.045 Uiso 1 1 calc R . . C33 C -0.0581(6) 0.28468(16) 0.4176(3) 0.0343(12) Uani 1 1 d . . . H33 H -0.0989 0.2833 0.4691 0.041 Uiso 1 1 calc R . . C34 C -0.0136(6) 0.32331(15) 0.3866(3) 0.0312(11) Uani 1 1 d . . . H34 H -0.0221 0.3481 0.4184 0.037 Uiso 1 1 calc R . . C35 C 1.0398(8) 0.36979(17) 0.6902(3) 0.0474(14) Uani 1 1 d . . . C36 C 0.5673(8) 0.38793(19) -0.1464(3) 0.0506(15) Uani 1 1 d . . . N1 N 0.6317(4) 0.42278(11) 0.3067(2) 0.0250(8) Uani 1 1 d . . . N2 N 0.4964(5) 0.44650(12) 0.1826(2) 0.0270(9) Uani 1 1 d . . . N3 N 0.3418(5) 0.40548(12) 0.0946(2) 0.0278(9) Uani 1 1 d . . . N4 N 0.1937(5) 0.33665(12) 0.0993(2) 0.0302(9) Uani 1 1 d . . . N5 N 0.1038(5) 0.29890(12) 0.1939(2) 0.0283(9) Uani 1 1 d . . . N6 N 0.0415(4) 0.32753(11) 0.3133(2) 0.0261(9) Uani 1 1 d . . . N7 N 0.5673(5) 0.31486(12) 0.2234(2) 0.0271(9) Uani 1 1 d . . . N8 N 0.4892(5) 0.29530(11) 0.3458(2) 0.0260(8) Uani 1 1 d . . . N9 N 0.4236(5) 0.34059(11) 0.43363(19) 0.0247(8) Uani 1 1 d . . . N10 N 0.3250(5) 0.41473(11) 0.42734(19) 0.0241(8) Uani 1 1 d . . . N11 N 0.2084(4) 0.45687(11) 0.3321(2) 0.0236(8) Uani 1 1 d . . . N12 N 0.0469(5) 0.43289(12) 0.2131(2) 0.0275(9) Uani 1 1 d . . . F1 F 1.1665(5) 0.34205(11) 0.6756(2) 0.0735(11) Uani 1 1 d . . . F2 F 1.1253(5) 0.40359(10) 0.72621(19) 0.0771(12) Uani 1 1 d . . . F3 F 0.9448(6) 0.35183(12) 0.7427(2) 0.0821(12) Uani 1 1 d . . . F4 F 0.5593(5) 0.36600(11) -0.21398(18) 0.0711(10) Uani 1 1 d . . . F5 F 0.6403(7) 0.42506(12) -0.1606(2) 0.1056(15) Uani 1 1 d . . . F6 F 0.4013(5) 0.39624(18) -0.1325(2) 0.1178(18) Uani 1 1 d . . . Ni1 Ni 0.48717(8) 0.371136(18) 0.26452(3) 0.02723(17) Uani 1 1 d . . . Ni2 Ni 0.14918(8) 0.377981(18) 0.26324(3) 0.02763(17) Uani 1 1 d . . . S1 S 0.89442(17) 0.38429(4) 0.59650(7) 0.0370(3) Uani 1 1 d . . . S2 S 0.69881(18) 0.36188(4) -0.05907(7) 0.0406(3) Uani 1 1 d . . . O1 O 0.7634(5) 0.41389(11) 0.6227(2) 0.0477(9) Uani 1 1 d . . . O2 O 0.8153(5) 0.34462(12) 0.5662(2) 0.0561(11) Uani 1 1 d . . . O3 O 1.0198(5) 0.40282(12) 0.5487(2) 0.0503(10) Uani 1 1 d . . . O4 O 0.6758(5) 0.38902(12) 0.0072(2) 0.0573(11) Uani 1 1 d . . . O5 O 0.8789(5) 0.35954(16) -0.0795(2) 0.0826(15) Uani 1 1 d . . . O6 O 0.6045(8) 0.32225(13) -0.0579(2) 0.0951(17) 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 0.035(3) 0.035(3) 0.028(2) -0.002(2) 0.000(2) 0.000(2) C2 0.039(3) 0.038(3) 0.036(3) -0.013(2) -0.003(2) 0.009(3) C3 0.045(3) 0.030(3) 0.043(3) -0.014(3) -0.012(2) 0.016(3) C4 0.045(3) 0.019(3) 0.044(3) -0.007(2) -0.009(2) 0.007(2) C5 0.026(2) 0.020(3) 0.030(2) -0.005(2) -0.0059(19) 0.004(2) C6 0.034(3) 0.021(3) 0.037(3) 0.008(2) -0.004(2) 0.001(2) C7 0.038(3) 0.026(3) 0.027(2) 0.009(2) 0.001(2) -0.001(2) C8 0.024(2) 0.018(3) 0.031(2) -0.001(2) -0.0037(19) 0.002(2) C9 0.044(3) 0.024(3) 0.027(2) 0.000(2) -0.002(2) 0.007(2) C10 0.034(2) 0.021(3) 0.030(2) -0.007(2) 0.0047(19) -0.001(2) C11 0.034(3) 0.018(3) 0.036(3) -0.006(2) 0.003(2) -0.001(2) C12 0.024(2) 0.019(3) 0.030(2) 0.0013(19) 0.0013(18) 0.001(2) C13 0.024(2) 0.021(3) 0.034(2) 0.000(2) 0.0059(18) 0.002(2) C14 0.037(3) 0.022(3) 0.040(3) -0.001(2) 0.002(2) 0.004(2) C15 0.051(3) 0.028(3) 0.042(3) 0.009(2) 0.003(2) 0.010(3) C16 0.039(3) 0.039(3) 0.037(3) 0.004(2) -0.004(2) 0.012(3) C17 0.037(3) 0.023(3) 0.035(3) -0.001(2) -0.002(2) 0.005(2) C18 0.030(2) 0.030(3) 0.029(2) -0.004(2) 0.0010(19) 0.002(2) C19 0.027(2) 0.030(3) 0.036(3) -0.009(2) 0.001(2) -0.002(2) C20 0.042(3) 0.020(3) 0.044(3) -0.003(2) 0.009(2) -0.011(2) C21 0.043(3) 0.018(3) 0.040(3) 0.002(2) 0.008(2) -0.001(2) C22 0.025(2) 0.021(3) 0.031(2) 0.003(2) 0.0040(18) 0.001(2) C23 0.044(3) 0.024(3) 0.038(3) 0.011(2) 0.003(2) 0.004(2) C24 0.040(3) 0.033(3) 0.030(3) 0.010(2) -0.002(2) 0.008(2) C25 0.028(2) 0.024(3) 0.030(2) 0.000(2) 0.0008(19) -0.005(2) C26 0.054(3) 0.046(4) 0.025(2) -0.003(2) -0.003(2) -0.017(3) C27 0.036(3) 0.033(3) 0.034(3) -0.012(2) -0.001(2) 0.000(2) C28 0.040(3) 0.027(3) 0.040(3) -0.011(2) -0.006(2) 0.001(2) C29 0.026(2) 0.015(3) 0.034(2) -0.001(2) -0.0065(19) 0.000(2) C30 0.024(2) 0.021(3) 0.031(2) 0.001(2) -0.0045(19) 0.000(2) C31 0.043(3) 0.026(3) 0.042(3) -0.003(2) -0.006(2) 0.000(2) C32 0.041(3) 0.026(3) 0.044(3) 0.008(2) -0.001(2) -0.012(2) C33 0.030(3) 0.036(3) 0.036(3) 0.006(2) 0.001(2) -0.004(2) C34 0.033(2) 0.023(3) 0.034(3) -0.002(2) -0.005(2) -0.002(2) C35 0.065(4) 0.027(3) 0.047(3) 0.007(3) -0.001(3) 0.004(3) C36 0.051(4) 0.043(4) 0.056(4) -0.001(3) -0.001(3) 0.000(3) N1 0.0284(19) 0.017(2) 0.0277(19) 0.0002(16) -0.0018(15) 0.0010(17) N2 0.032(2) 0.020(2) 0.029(2) 0.0034(17) 0.0051(16) -0.0005(17) N3 0.034(2) 0.025(2) 0.0237(19) -0.0009(17) 0.0013(16) 0.0006(18) N4 0.036(2) 0.027(2) 0.026(2) -0.0026(17) -0.0020(16) -0.0037(18) N5 0.031(2) 0.019(2) 0.032(2) -0.0041(17) -0.0036(16) -0.0008(17) N6 0.0272(19) 0.019(2) 0.031(2) -0.0034(17) -0.0014(16) -0.0014(17) N7 0.030(2) 0.022(2) 0.027(2) -0.0044(17) -0.0010(16) 0.0013(17) N8 0.030(2) 0.016(2) 0.030(2) 0.0042(16) -0.0016(16) 0.0027(17) N9 0.033(2) 0.018(2) 0.0214(18) -0.0006(16) 0.0010(15) 0.0010(17) N10 0.0312(19) 0.017(2) 0.0230(18) -0.0033(15) 0.0009(15) 0.0020(17) N11 0.0248(18) 0.016(2) 0.0285(19) -0.0056(16) 0.0002(15) -0.0016(16) N12 0.029(2) 0.020(2) 0.032(2) -0.0021(17) -0.0003(16) -0.0001(17) F1 0.071(2) 0.047(2) 0.095(3) 0.005(2) -0.0106(19) 0.0262(19) F2 0.107(3) 0.041(2) 0.065(2) -0.0064(17) -0.044(2) -0.001(2) F3 0.132(3) 0.063(3) 0.056(2) 0.0257(19) 0.027(2) 0.016(2) F4 0.101(3) 0.072(3) 0.0370(18) -0.0029(17) -0.0026(17) 0.000(2) F5 0.164(4) 0.044(2) 0.104(3) 0.029(2) 0.002(3) -0.007(3) F6 0.056(2) 0.222(6) 0.073(3) 0.011(3) 0.001(2) 0.049(3) Ni1 0.0373(3) 0.0173(3) 0.0253(3) 0.0004(2) -0.0010(2) -0.0020(3) Ni2 0.0370(3) 0.0169(3) 0.0266(3) -0.0022(3) -0.0028(2) -0.0015(3) S1 0.0449(7) 0.0293(8) 0.0353(7) -0.0037(6) 0.0009(5) -0.0057(6) S2 0.0532(8) 0.0318(8) 0.0348(7) -0.0050(6) 0.0001(6) 0.0015(6) O1 0.053(2) 0.033(2) 0.057(2) -0.0065(18) 0.0082(18) 0.0065(18) O2 0.060(2) 0.040(2) 0.068(3) -0.024(2) 0.011(2) -0.0132(19) O3 0.050(2) 0.057(3) 0.044(2) 0.0136(19) 0.0105(17) -0.0057(19) O4 0.067(2) 0.058(3) 0.046(2) -0.028(2) 0.0041(18) -0.004(2) O5 0.049(2) 0.131(4) 0.066(3) -0.011(3) 0.003(2) 0.029(3) O6 0.186(5) 0.034(3) 0.060(3) 0.005(2) 0.003(3) -0.044(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 C1 N7 1.352(5) . ? C1 C2 1.369(6) . ? C1 H1 0.9500 . ? C2 C3 1.385(7) . ? C2 H2 0.9500 . ? C3 C4 1.374(7) . ? C3 H3 0.9500 . ? C4 C5 1.386(6) . ? C4 H4 0.9500 . ? C5 N7 1.352(5) . ? C5 N8 1.398(5) . ? C6 C7 1.330(6) . ? C6 N8 1.393(5) . ? C6 H6 0.9500 . ? C7 N9 1.395(5) . ? C7 H7 0.9500 . ? C8 N9 1.355(5) . ? C8 N8 1.382(5) . ? C8 Ni1 1.878(4) . ? C9 N9 1.456(5) . ? C9 N10 1.456(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.339(6) . ? C10 N10 1.389(5) . ? C10 H10 0.9500 . ? C11 N11 1.390(5) . ? C11 H11 0.9500 . ? C12 N10 1.359(5) . ? C12 N11 1.388(5) . ? C12 Ni2 1.865(4) . ? C13 N12 1.355(5) . ? C13 C14 1.382(6) . ? C13 N11 1.399(5) . ? C14 C15 1.378(6) . ? C14 H14 0.9500 . ? C15 C16 1.380(6) . ? C15 H15 0.9500 . ? C16 C17 1.374(6) . ? C16 H16 0.9500 . ? C17 N12 1.350(5) . ? C17 H17 0.9500 . ? C18 N1 1.350(5) . ? C18 C19 1.379(6) . ? C18 H18 0.9500 . ? C19 C20 1.378(6) . ? C19 H19 0.9500 . ? C20 C21 1.378(6) . ? C20 H20 0.9500 . ? C21 C22 1.375(6) . ? C21 H21 0.9500 . ? C22 N1 1.349(5) . ? C22 N2 1.409(5) . ? C23 C24 1.337(6) . ? C23 N2 1.400(5) . ? C23 H23 0.9500 . ? C24 N3 1.389(6) . ? C24 H24 0.9500 . ? C25 N3 1.361(5) . ? C25 N2 1.374(5) . ? C25 Ni1 1.871(4) . ? C26 N3 1.447(6) . ? C26 N4 1.452(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.339(6) . ? C27 N4 1.382(6) . ? C27 H27 0.9500 . ? C28 N5 1.392(5) . ? C28 H28 0.9500 . ? C29 N4 1.365(5) . ? C29 N5 1.375(5) . ? C29 Ni2 1.881(4) . ? C30 N6 1.354(5) . ? C30 C31 1.378(6) . ? C30 N5 1.402(5) . ? C31 C32 1.380(6) . ? C31 H31 0.9500 . ? C32 C33 1.378(6) . ? C32 H32 0.9500 . ? C33 C34 1.378(6) . ? C33 H33 0.9500 . ? C34 N6 1.348(5) . ? C34 H34 0.9500 . ? C35 F3 1.326(6) . ? C35 F1 1.329(6) . ? C35 F2 1.331(6) . ? C35 S1 1.814(5) . ? C36 F4 1.311(6) . ? C36 F6 1.311(6) . ? C36 F5 1.322(6) . ? C36 S2 1.817(6) . ? N1 Ni1 2.011(3) . ? N6 Ni2 2.010(4) . ? N7 Ni1 2.017(4) . ? N12 Ni2 2.014(4) . ? Ni1 Ni2 2.5087(10) . ? S1 O3 1.432(3) . ? S1 O2 1.436(4) . ? S1 O1 1.456(3) . ? S2 O4 1.423(3) . ? S2 O5 1.426(4) . ? S2 O6 1.429(4) . ? 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 N7 C1 C2 122.6(5) . . ? N7 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 119.9(5) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 118.8(5) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 118.1(5) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? N7 C5 C4 123.9(4) . . ? N7 C5 N8 112.1(4) . . ? C4 C5 N8 124.0(4) . . ? C7 C6 N8 106.6(4) . . ? C7 C6 H6 126.7 . . ? N8 C6 H6 126.7 . . ? C6 C7 N9 107.4(4) . . ? C6 C7 H7 126.3 . . ? N9 C7 H7 126.3 . . ? N9 C8 N8 103.2(4) . . ? N9 C8 Ni1 143.2(3) . . ? N8 C8 Ni1 113.5(3) . . ? N9 C9 N10 113.8(3) . . ? N9 C9 H9A 108.8 . . ? N10 C9 H9A 108.8 . . ? N9 C9 H9B 108.8 . . ? N10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C11 C10 N10 108.0(4) . . ? C11 C10 H10 126.0 . . ? N10 C10 H10 126.0 . . ? C10 C11 N11 105.7(4) . . ? C10 C11 H11 127.2 . . ? N11 C11 H11 127.2 . . ? N10 C12 N11 102.6(3) . . ? N10 C12 Ni2 143.5(3) . . ? N11 C12 Ni2 113.8(3) . . ? N12 C13 C14 124.0(4) . . ? N12 C13 N11 111.7(4) . . ? C14 C13 N11 124.2(4) . . ? C15 C14 C13 117.6(4) . . ? C15 C14 H14 121.2 . . ? C13 C14 H14 121.2 . . ? C14 C15 C16 119.5(5) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 119.6(4) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? N12 C17 C16 122.5(4) . . ? N12 C17 H17 118.8 . . ? C16 C17 H17 118.8 . . ? N1 C18 C19 123.1(4) . . ? N1 C18 H18 118.4 . . ? C19 C18 H18 118.4 . . ? C20 C19 C18 118.4(4) . . ? C20 C19 H19 120.8 . . ? C18 C19 H19 120.8 . . ? C21 C20 C19 120.0(4) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 117.8(4) . . ? C22 C21 H21 121.1 . . ? C20 C21 H21 121.1 . . ? N1 C22 C21 124.0(4) . . ? N1 C22 N2 111.4(4) . . ? C21 C22 N2 124.6(4) . . ? C24 C23 N2 105.2(4) . . ? C24 C23 H23 127.4 . . ? N2 C23 H23 127.4 . . ? C23 C24 N3 108.6(4) . . ? C23 C24 H24 125.7 . . ? N3 C24 H24 125.7 . . ? N3 C25 N2 103.4(4) . . ? N3 C25 Ni1 142.4(4) . . ? N2 C25 Ni1 114.2(3) . . ? N3 C26 N4 114.0(4) . . ? N3 C26 H26A 108.7 . . ? N4 C26 H26A 108.7 . . ? N3 C26 H26B 108.7 . . ? N4 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C28 C27 N4 108.2(4) . . ? C28 C27 H27 125.9 . . ? N4 C27 H27 125.9 . . ? C27 C28 N5 105.9(4) . . ? C27 C28 H28 127.0 . . ? N5 C28 H28 127.0 . . ? N4 C29 N5 103.5(4) . . ? N4 C29 Ni2 142.7(3) . . ? N5 C29 Ni2 113.6(3) . . ? N6 C30 C31 123.7(4) . . ? N6 C30 N5 112.1(4) . . ? C31 C30 N5 124.1(4) . . ? C30 C31 C32 118.8(5) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? C33 C32 C31 118.4(5) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C34 C33 C32 119.7(5) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? N6 C34 C33 123.1(4) . . ? N6 C34 H34 118.5 . . ? C33 C34 H34 118.5 . . ? F3 C35 F1 107.4(4) . . ? F3 C35 F2 107.9(5) . . ? F1 C35 F2 107.7(5) . . ? F3 C35 S1 111.5(4) . . ? F1 C35 S1 110.6(4) . . ? F2 C35 S1 111.5(4) . . ? F4 C36 F6 109.4(5) . . ? F4 C36 F5 106.2(5) . . ? F6 C36 F5 105.9(5) . . ? F4 C36 S2 113.4(4) . . ? F6 C36 S2 110.7(4) . . ? F5 C36 S2 110.8(4) . . ? C22 N1 C18 116.6(4) . . ? C22 N1 Ni1 113.8(3) . . ? C18 N1 Ni1 129.2(3) . . ? C25 N2 C23 112.0(4) . . ? C25 N2 C22 117.9(3) . . ? C23 N2 C22 130.1(4) . . ? C25 N3 C24 110.8(4) . . ? C25 N3 C26 128.4(4) . . ? C24 N3 C26 120.8(4) . . ? C29 N4 C27 110.9(4) . . ? C29 N4 C26 128.0(4) . . ? C27 N4 C26 121.1(4) . . ? C29 N5 C28 111.5(4) . . ? C29 N5 C30 117.9(4) . . ? C28 N5 C30 130.6(4) . . ? C34 N6 C30 116.2(4) . . ? C34 N6 Ni2 130.1(3) . . ? C30 N6 Ni2 113.0(3) . . ? C5 N7 C1 116.5(4) . . ? C5 N7 Ni1 113.1(3) . . ? C1 N7 Ni1 129.8(3) . . ? C8 N8 C6 111.2(4) . . ? C8 N8 C5 118.2(4) . . ? C6 N8 C5 130.6(4) . . ? C8 N9 C7 111.5(4) . . ? C8 N9 C9 128.2(4) . . ? C7 N9 C9 120.3(4) . . ? C12 N10 C10 111.7(4) . . ? C12 N10 C9 127.1(4) . . ? C10 N10 C9 121.2(3) . . ? C12 N11 C11 112.1(3) . . ? C12 N11 C13 117.8(3) . . ? C11 N11 C13 130.2(4) . . ? C17 N12 C13 116.7(4) . . ? C17 N12 Ni2 129.1(3) . . ? C13 N12 Ni2 113.1(3) . . ? C25 Ni1 C8 162.17(18) . . ? C25 Ni1 N1 81.88(16) . . ? C8 Ni1 N1 105.37(16) . . ? C25 Ni1 N7 105.67(17) . . ? C8 Ni1 N7 82.11(17) . . ? N1 Ni1 N7 131.08(14) . . ? C25 Ni1 Ni2 81.14(13) . . ? C8 Ni1 Ni2 81.03(12) . . ? N1 Ni1 Ni2 114.33(10) . . ? N7 Ni1 Ni2 114.59(10) . . ? C12 Ni2 C29 159.82(18) . . ? C12 Ni2 N6 105.65(16) . . ? C29 Ni2 N6 82.17(17) . . ? C12 Ni2 N12 82.13(16) . . ? C29 Ni2 N12 105.97(16) . . ? N6 Ni2 N12 134.36(14) . . ? C12 Ni2 Ni1 79.69(13) . . ? C29 Ni2 Ni1 80.13(13) . . ? N6 Ni2 Ni1 112.70(10) . . ? N12 Ni2 Ni1 112.94(10) . . ? O3 S1 O2 115.0(2) . . ? O3 S1 O1 114.9(2) . . ? O2 S1 O1 113.8(2) . . ? O3 S1 C35 103.1(2) . . ? O2 S1 C35 104.0(2) . . ? O1 S1 C35 103.9(2) . . ? O4 S2 O5 116.1(2) . . ? O4 S2 O6 113.4(3) . . ? O5 S2 O6 115.7(3) . . ? O4 S2 C36 103.7(3) . . ? O5 S2 C36 104.0(3) . . ? O6 S2 C36 101.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 C1 C2 C3 0.9(7) . . . . ? C1 C2 C3 C4 -1.1(7) . . . . ? C2 C3 C4 C5 -0.5(6) . . . . ? C3 C4 C5 N7 2.3(6) . . . . ? C3 C4 C5 N8 -178.2(4) . . . . ? N8 C6 C7 N9 -0.6(5) . . . . ? N10 C10 C11 N11 -0.1(5) . . . . ? N12 C13 C14 C15 2.3(7) . . . . ? N11 C13 C14 C15 -179.3(4) . . . . ? C13 C14 C15 C16 0.0(7) . . . . ? C14 C15 C16 C17 -1.7(7) . . . . ? C15 C16 C17 N12 1.3(7) . . . . ? N1 C18 C19 C20 0.9(7) . . . . ? C18 C19 C20 C21 -0.9(7) . . . . ? C19 C20 C21 C22 -0.8(7) . . . . ? C20 C21 C22 N1 2.7(7) . . . . ? C20 C21 C22 N2 -177.9(4) . . . . ? N2 C23 C24 N3 1.1(5) . . . . ? N4 C27 C28 N5 0.2(5) . . . . ? N6 C30 C31 C32 2.1(7) . . . . ? N5 C30 C31 C32 -178.0(4) . . . . ? C30 C31 C32 C33 -0.5(6) . . . . ? C31 C32 C33 C34 -1.2(6) . . . . ? C32 C33 C34 N6 1.4(6) . . . . ? C21 C22 N1 C18 -2.8(6) . . . . ? N2 C22 N1 C18 177.9(4) . . . . ? C21 C22 N1 Ni1 170.3(4) . . . . ? N2 C22 N1 Ni1 -9.1(4) . . . . ? C19 C18 N1 C22 0.9(6) . . . . ? C19 C18 N1 Ni1 -171.0(3) . . . . ? N3 C25 N2 C23 2.1(5) . . . . ? Ni1 C25 N2 C23 -176.7(3) . . . . ? N3 C25 N2 C22 -178.5(3) . . . . ? Ni1 C25 N2 C22 2.7(5) . . . . ? C24 C23 N2 C25 -2.1(5) . . . . ? C24 C23 N2 C22 178.6(4) . . . . ? N1 C22 N2 C25 4.5(5) . . . . ? C21 C22 N2 C25 -174.9(4) . . . . ? N1 C22 N2 C23 -176.3(4) . . . . ? C21 C22 N2 C23 4.3(7) . . . . ? N2 C25 N3 C24 -1.4(5) . . . . ? Ni1 C25 N3 C24 176.8(4) . . . . ? N2 C25 N3 C26 177.4(4) . . . . ? Ni1 C25 N3 C26 -4.5(8) . . . . ? C23 C24 N3 C25 0.1(5) . . . . ? C23 C24 N3 C26 -178.7(4) . . . . ? N4 C26 N3 C25 23.9(7) . . . . ? N4 C26 N3 C24 -157.5(4) . . . . ? N5 C29 N4 C27 -0.6(4) . . . . ? Ni2 C29 N4 C27 174.6(4) . . . . ? N5 C29 N4 C26 179.2(4) . . . . ? Ni2 C29 N4 C26 -5.6(8) . . . . ? C28 C27 N4 C29 0.3(5) . . . . ? C28 C27 N4 C26 -179.5(4) . . . . ? N3 C26 N4 C29 26.5(7) . . . . ? N3 C26 N4 C27 -153.8(4) . . . . ? N4 C29 N5 C28 0.8(4) . . . . ? Ni2 C29 N5 C28 -176.1(3) . . . . ? N4 C29 N5 C30 -179.7(3) . . . . ? Ni2 C29 N5 C30 3.5(5) . . . . ? C27 C28 N5 C29 -0.6(5) . . . . ? C27 C28 N5 C30 179.9(4) . . . . ? N6 C30 N5 C29 5.0(5) . . . . ? C31 C30 N5 C29 -174.9(4) . . . . ? N6 C30 N5 C28 -175.5(4) . . . . ? C31 C30 N5 C28 4.6(7) . . . . ? C33 C34 N6 C30 0.2(6) . . . . ? C33 C34 N6 Ni2 -169.4(3) . . . . ? C31 C30 N6 C34 -1.9(6) . . . . ? N5 C30 N6 C34 178.1(3) . . . . ? C31 C30 N6 Ni2 169.4(3) . . . . ? N5 C30 N6 Ni2 -10.5(4) . . . . ? C4 C5 N7 C1 -2.5(6) . . . . ? N8 C5 N7 C1 178.0(3) . . . . ? C4 C5 N7 Ni1 169.5(3) . . . . ? N8 C5 N7 Ni1 -10.0(4) . . . . ? C2 C1 N7 C5 0.8(6) . . . . ? C2 C1 N7 Ni1 -169.6(3) . . . . ? N9 C8 N8 C6 0.1(4) . . . . ? Ni1 C8 N8 C6 -177.1(3) . . . . ? N9 C8 N8 C5 -178.4(3) . . . . ? Ni1 C8 N8 C5 4.4(4) . . . . ? C7 C6 N8 C8 0.3(5) . . . . ? C7 C6 N8 C5 178.6(4) . . . . ? N7 C5 N8 C8 4.0(5) . . . . ? C4 C5 N8 C8 -175.5(4) . . . . ? N7 C5 N8 C6 -174.1(4) . . . . ? C4 C5 N8 C6 6.4(7) . . . . ? N8 C8 N9 C7 -0.4(4) . . . . ? Ni1 C8 N9 C7 175.2(4) . . . . ? N8 C8 N9 C9 -180.0(4) . . . . ? Ni1 C8 N9 C9 -4.3(8) . . . . ? C6 C7 N9 C8 0.7(5) . . . . ? C6 C7 N9 C9 -179.8(4) . . . . ? N10 C9 N9 C8 21.1(6) . . . . ? N10 C9 N9 C7 -158.4(4) . . . . ? N11 C12 N10 C10 -0.3(5) . . . . ? Ni2 C12 N10 C10 176.2(4) . . . . ? N11 C12 N10 C9 177.8(4) . . . . ? Ni2 C12 N10 C9 -5.6(8) . . . . ? C11 C10 N10 C12 0.3(5) . . . . ? C11 C10 N10 C9 -178.0(4) . . . . ? N9 C9 N10 C12 29.2(6) . . . . ? N9 C9 N10 C10 -152.8(4) . . . . ? N10 C12 N11 C11 0.2(5) . . . . ? Ni2 C12 N11 C11 -177.5(3) . . . . ? N10 C12 N11 C13 -178.6(3) . . . . ? Ni2 C12 N11 C13 3.7(5) . . . . ? C10 C11 N11 C12 0.0(5) . . . . ? C10 C11 N11 C13 178.6(4) . . . . ? N12 C13 N11 C12 5.9(5) . . . . ? C14 C13 N11 C12 -172.7(4) . . . . ? N12 C13 N11 C11 -172.7(4) . . . . ? C14 C13 N11 C11 8.8(7) . . . . ? C16 C17 N12 C13 0.9(7) . . . . ? C16 C17 N12 Ni2 -166.4(4) . . . . ? C14 C13 N12 C17 -2.7(6) . . . . ? N11 C13 N12 C17 178.7(4) . . . . ? C14 C13 N12 Ni2 166.6(4) . . . . ? N11 C13 N12 Ni2 -12.0(4) . . . . ? N3 C25 Ni1 C8 -68.5(9) . . . . ? N2 C25 Ni1 C8 109.6(6) . . . . ? N3 C25 Ni1 N1 176.0(6) . . . . ? N2 C25 Ni1 N1 -5.9(3) . . . . ? N3 C25 Ni1 N7 45.6(6) . . . . ? N2 C25 Ni1 N7 -136.4(3) . . . . ? N3 C25 Ni1 Ni2 -67.6(5) . . . . ? N2 C25 Ni1 Ni2 110.4(3) . . . . ? N9 C8 Ni1 C25 -65.6(9) . . . . ? N8 C8 Ni1 C25 109.8(6) . . . . ? N9 C8 Ni1 N1 46.5(5) . . . . ? N8 C8 Ni1 N1 -138.1(3) . . . . ? N9 C8 Ni1 N7 177.0(5) . . . . ? N8 C8 Ni1 N7 -7.6(3) . . . . ? N9 C8 Ni1 Ni2 -66.4(5) . . . . ? N8 C8 Ni1 Ni2 109.0(3) . . . . ? C22 N1 Ni1 C25 8.6(3) . . . . ? C18 N1 Ni1 C25 -179.4(4) . . . . ? C22 N1 Ni1 C8 -154.7(3) . . . . ? C18 N1 Ni1 C8 17.3(4) . . . . ? C22 N1 Ni1 N7 112.4(3) . . . . ? C18 N1 Ni1 N7 -75.6(4) . . . . ? C22 N1 Ni1 Ni2 -67.8(3) . . . . ? C18 N1 Ni1 Ni2 104.2(4) . . . . ? C5 N7 Ni1 C25 -153.6(3) . . . . ? C1 N7 Ni1 C25 17.1(4) . . . . ? C5 N7 Ni1 C8 10.0(3) . . . . ? C1 N7 Ni1 C8 -179.3(4) . . . . ? C5 N7 Ni1 N1 113.6(3) . . . . ? C1 N7 Ni1 N1 -75.8(4) . . . . ? C5 N7 Ni1 Ni2 -66.3(3) . . . . ? C1 N7 Ni1 Ni2 104.4(3) . . . . ? N10 C12 Ni2 C29 -68.8(8) . . . . ? N11 C12 Ni2 C29 107.5(5) . . . . ? N10 C12 Ni2 N6 41.8(6) . . . . ? N11 C12 Ni2 N6 -141.9(3) . . . . ? N10 C12 Ni2 N12 175.8(6) . . . . ? N11 C12 Ni2 N12 -7.9(3) . . . . ? N10 C12 Ni2 Ni1 -69.0(5) . . . . ? N11 C12 Ni2 Ni1 107.3(3) . . . . ? N4 C29 Ni2 C12 -67.5(8) . . . . ? N5 C29 Ni2 C12 107.4(6) . . . . ? N4 C29 Ni2 N6 177.9(5) . . . . ? N5 C29 Ni2 N6 -7.1(3) . . . . ? N4 C29 Ni2 N12 43.9(5) . . . . ? N5 C29 Ni2 N12 -141.2(3) . . . . ? N4 C29 Ni2 Ni1 -67.3(5) . . . . ? N5 C29 Ni2 Ni1 107.6(3) . . . . ? C34 N6 Ni2 C12 18.9(4) . . . . ? C30 N6 Ni2 C12 -150.9(3) . . . . ? C34 N6 Ni2 C29 179.9(4) . . . . ? C30 N6 Ni2 C29 10.1(3) . . . . ? C34 N6 Ni2 N12 -75.4(4) . . . . ? C30 N6 Ni2 N12 114.8(3) . . . . ? C34 N6 Ni2 Ni1 104.1(3) . . . . ? C30 N6 Ni2 Ni1 -65.7(3) . . . . ? C17 N12 Ni2 C12 179.0(4) . . . . ? C13 N12 Ni2 C12 11.4(3) . . . . ? C17 N12 Ni2 C29 17.9(4) . . . . ? C13 N12 Ni2 C29 -149.7(3) . . . . ? C17 N12 Ni2 N6 -76.8(4) . . . . ? C13 N12 Ni2 N6 115.6(3) . . . . ? C17 N12 Ni2 Ni1 103.8(4) . . . . ? C13 N12 Ni2 Ni1 -63.9(3) . . . . ? C25 Ni1 Ni2 C12 -105.58(19) . . . . ? C8 Ni1 Ni2 C12 74.16(19) . . . . ? N1 Ni1 Ni2 C12 -28.73(17) . . . . ? N7 Ni1 Ni2 C12 151.16(17) . . . . ? C25 Ni1 Ni2 C29 74.51(19) . . . . ? C8 Ni1 Ni2 C29 -105.75(19) . . . . ? N1 Ni1 Ni2 C29 151.36(17) . . . . ? N7 Ni1 Ni2 C29 -28.75(18) . . . . ? C25 Ni1 Ni2 N6 151.64(17) . . . . ? C8 Ni1 Ni2 N6 -28.62(17) . . . . ? N1 Ni1 Ni2 N6 -131.50(15) . . . . ? N7 Ni1 Ni2 N6 48.38(16) . . . . ? C25 Ni1 Ni2 N12 -28.77(18) . . . . ? C8 Ni1 Ni2 N12 150.98(17) . . . . ? N1 Ni1 Ni2 N12 48.09(15) . . . . ? N7 Ni1 Ni2 N12 -132.03(16) . . . . ? F3 C35 S1 O3 180.0(4) . . . . ? F1 C35 S1 O3 -60.5(4) . . . . ? F2 C35 S1 O3 59.3(5) . . . . ? F3 C35 S1 O2 -59.6(4) . . . . ? F1 C35 S1 O2 59.8(4) . . . . ? F2 C35 S1 O2 179.7(4) . . . . ? F3 C35 S1 O1 59.7(4) . . . . ? F1 C35 S1 O1 179.2(4) . . . . ? F2 C35 S1 O1 -60.9(5) . . . . ? F4 C36 S2 O4 -175.1(4) . . . . ? F6 C36 S2 O4 -51.7(5) . . . . ? F5 C36 S2 O4 65.6(5) . . . . ? F4 C36 S2 O5 63.1(5) . . . . ? F6 C36 S2 O5 -173.4(5) . . . . ? F5 C36 S2 O5 -56.2(5) . . . . ? F4 C36 S2 O6 -57.3(5) . . . . ? F6 C36 S2 O6 66.1(5) . . . . ? F5 C36 S2 O6 -176.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.569 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.089 # Attachment '- propyl.cif' data_propyl _database_code_depnum_ccdc_archive 'CCDC 809512' #TrackingRef '- propyl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H18 N6 Ni, 2(P F6)' _chemical_formula_sum 'C19 H18 F12 N6 Ni P2' _chemical_formula_weight 679.04 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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 33.730(4) _cell_length_b 33.730(4) _cell_length_c 13.4121(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 13215(3) _cell_formula_units_Z 18 _cell_measurement_temperature 119(2) _cell_measurement_reflns_used 95329 _cell_measurement_theta_min 2.389 _cell_measurement_theta_max 25.279 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6120 _exptl_absorpt_coefficient_mu 0.866 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7812 _exptl_absorpt_correction_T_max 0.9184 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 119(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 'Bruker APEX-I CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 94483 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.37 _reflns_number_total 5384 _reflns_number_gt 4630 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v. 2009.3' _computing_cell_refinement 'Bruker APEX2 v. 2009.3' _computing_data_reduction 'Bruker APEX2 v. 2009.3' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-32 _computing_publication_material CIFTAB _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^)+(0.0580P)^2^+24.9130P] 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 5384 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 0.162984(11) 0.793307(11) 0.04008(2) 0.02711(11) Uani 1 1 d . . . N2 N 0.11355(7) 0.81308(7) -0.08928(14) 0.0268(4) Uani 1 1 d . . . N1 N 0.10987(7) 0.74736(7) -0.03459(15) 0.0283(5) Uani 1 1 d . . . N3 N 0.16725(7) 0.87853(7) -0.04021(15) 0.0282(5) Uani 1 1 d . . . N6 N 0.19481(7) 0.76063(7) 0.07851(15) 0.0309(5) Uani 1 1 d . . . N4 N 0.19607(7) 0.86385(7) 0.20247(15) 0.0304(5) Uani 1 1 d . . . N5 N 0.22068(7) 0.81621(7) 0.19739(15) 0.0320(5) Uani 1 1 d . . . C5 C 0.08915(8) 0.76481(9) -0.09072(17) 0.0286(5) Uani 1 1 d . . . C8 C 0.14924(8) 0.83353(8) -0.02487(17) 0.0273(5) Uani 1 1 d . . . C1 C 0.08751(9) 0.70156(9) -0.0232(2) 0.0353(6) Uani 1 1 d . . . H1 H 0.1005 0.6882 0.0181 0.042 Uiso 1 1 calc R . . C12 C 0.22190(9) 0.87013(10) 0.28870(19) 0.0344(6) Uani 1 1 d . . . H12 H 0.2276 0.8917 0.3402 0.041 Uiso 1 1 calc R . . C15 C 0.22315(9) 0.77916(9) 0.1572(2) 0.0340(6) Uani 1 1 d . . . C13 C 0.23707(9) 0.84055(10) 0.28558(19) 0.0372(6) Uani 1 1 d . . . H13 H 0.2555 0.8368 0.3341 0.045 Uiso 1 1 calc R . . C19 C 0.19633(10) 0.72691(9) 0.0280(2) 0.0373(6) Uani 1 1 d . . . H19 H 0.1772 0.7140 -0.0287 0.045 Uiso 1 1 calc R . . C7 C 0.14172(9) 0.88610(9) -0.11115(18) 0.0328(6) Uani 1 1 d . . . H7 H 0.1471 0.9151 -0.1331 0.039 Uiso 1 1 calc R . . C6 C 0.10816(9) 0.84524(9) -0.14329(19) 0.0337(6) Uani 1 1 d . . . H6 H 0.0856 0.8396 -0.1924 0.040 Uiso 1 1 calc R . . C14 C 0.19555(8) 0.83075(8) 0.14610(18) 0.0288(5) Uani 1 1 d . . . C11 C 0.17126(9) 0.88833(9) 0.18116(19) 0.0321(6) Uani 1 1 d . . . H11A H 0.1657 0.8998 0.2445 0.039 Uiso 1 1 calc R . . H11B H 0.1411 0.8666 0.1519 0.039 Uiso 1 1 calc R . . C16 C 0.25169(10) 0.76412(10) 0.1913(2) 0.0466(7) Uani 1 1 d . . . H16 H 0.2704 0.7774 0.2484 0.056 Uiso 1 1 calc R . . C4 C 0.04862(9) 0.73933(9) -0.1410(2) 0.0353(6) Uani 1 1 d . . . H4 H 0.0360 0.7534 -0.1813 0.042 Uiso 1 1 calc R . . C3 C 0.02708(10) 0.69246(10) -0.1304(2) 0.0414(7) Uani 1 1 d . . . H3 H -0.0007 0.6734 -0.1648 0.050 Uiso 1 1 calc R . . C9 C 0.20824(9) 0.91468(9) 0.01043(19) 0.0329(6) Uani 1 1 d . . . H9A H 0.2232 0.9420 -0.0332 0.039 Uiso 1 1 calc R . . H9B H 0.2302 0.9037 0.0216 0.039 Uiso 1 1 calc R . . C10 C 0.19679(10) 0.92827(9) 0.11017(19) 0.0358(6) Uani 1 1 d . . . H10A H 0.2256 0.9514 0.1424 0.043 Uiso 1 1 calc R . . H10B H 0.1779 0.9427 0.0978 0.043 Uiso 1 1 calc R . . C18 C 0.22505(11) 0.71060(11) 0.0564(3) 0.0475(7) Uani 1 1 d . . . H18 H 0.2260 0.6871 0.0192 0.057 Uiso 1 1 calc R . . C2 C 0.04602(10) 0.67339(10) -0.0698(2) 0.0427(7) Uani 1 1 d . . . H2 H 0.0308 0.6412 -0.0600 0.051 Uiso 1 1 calc R . . C17 C 0.25237(11) 0.72897(11) 0.1398(3) 0.0554(9) Uani 1 1 d . . . H17 H 0.2715 0.7175 0.1616 0.066 Uiso 1 1 calc R . . P2 P 0.00475(2) 0.23862(2) 0.40208(5) 0.03267(18) Uani 1 1 d . . . F11 F -0.00588(6) 0.20350(6) 0.49109(12) 0.0469(4) Uani 1 1 d . . . F12 F -0.02783(7) 0.25421(6) 0.45216(15) 0.0579(5) Uani 1 1 d . . . F8 F -0.03801(7) 0.20048(6) 0.34144(13) 0.0595(5) Uani 1 1 d . . . F10 F 0.04729(6) 0.27777(6) 0.46221(14) 0.0615(6) Uani 1 1 d . . . F9 F 0.01594(6) 0.27462(6) 0.31338(12) 0.0488(4) Uani 1 1 d . . . F7 F 0.03753(8) 0.22330(8) 0.35339(18) 0.0777(7) Uani 1 1 d . . . P1 P 0.16946(4) 0.20230(4) 0.11027(6) 0.0542(3) Uani 1 1 d . . . F3 F 0.21451(8) 0.20323(8) 0.15092(16) 0.0718(6) Uani 1 1 d . . . F6 F 0.19177(7) 0.25533(7) 0.13724(19) 0.0724(6) Uani 1 1 d . . . F4 F 0.14839(8) 0.18988(7) 0.21924(15) 0.0709(6) Uani 1 1 d . . . F1 F 0.12541(9) 0.20199(9) 0.07087(17) 0.0802(7) Uani 1 1 d . . . F5 F 0.14794(11) 0.14931(9) 0.0863(2) 0.1040(10) Uani 1 1 d . . . F2 F 0.19132(12) 0.21482(13) 0.00266(17) 0.1127(11) 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 0.02655(19) 0.02622(19) 0.02536(18) 0.00113(12) -0.00307(12) 0.01079(14) N2 0.0268(11) 0.0238(11) 0.0256(10) 0.0020(8) -0.0017(8) 0.0095(9) N1 0.0279(11) 0.0262(11) 0.0273(10) 0.0015(8) -0.0010(8) 0.0109(9) N3 0.0262(11) 0.0272(11) 0.0262(10) 0.0021(8) 0.0003(8) 0.0095(9) N6 0.0278(11) 0.0282(11) 0.0323(11) 0.0070(9) 0.0021(9) 0.0107(9) N4 0.0258(11) 0.0295(11) 0.0254(10) 0.0020(8) 0.0002(8) 0.0059(9) N5 0.0239(11) 0.0343(12) 0.0299(11) 0.0062(9) -0.0029(8) 0.0086(10) C5 0.0284(13) 0.0292(13) 0.0242(12) 0.0026(9) 0.0025(10) 0.0113(11) C8 0.0251(13) 0.0277(13) 0.0239(12) 0.0006(9) 0.0012(9) 0.0091(11) C1 0.0371(15) 0.0296(14) 0.0355(14) 0.0039(11) -0.0007(11) 0.0139(12) C12 0.0262(13) 0.0383(15) 0.0250(12) 0.0002(10) -0.0036(10) 0.0060(12) C15 0.0226(13) 0.0301(14) 0.0397(14) 0.0097(11) -0.0002(10) 0.0061(11) C13 0.0253(13) 0.0400(16) 0.0295(13) 0.0066(11) -0.0041(10) 0.0037(12) C19 0.0358(15) 0.0337(15) 0.0393(15) 0.0074(11) 0.0065(11) 0.0152(13) C7 0.0366(15) 0.0288(14) 0.0291(13) 0.0065(10) 0.0003(11) 0.0135(12) C6 0.0347(14) 0.0368(15) 0.0279(13) 0.0058(11) -0.0036(10) 0.0165(12) C14 0.0247(13) 0.0280(13) 0.0272(12) 0.0061(10) -0.0005(9) 0.0084(11) C11 0.0267(13) 0.0333(14) 0.0306(13) -0.0037(10) -0.0005(10) 0.0109(11) C16 0.0318(16) 0.0385(17) 0.0618(19) 0.0089(14) -0.0116(13) 0.0118(14) C4 0.0293(14) 0.0319(14) 0.0378(15) 0.0000(11) -0.0060(11) 0.0101(12) C3 0.0293(15) 0.0362(16) 0.0469(16) -0.0019(12) -0.0065(12) 0.0074(13) C9 0.0263(13) 0.0246(13) 0.0347(14) 0.0013(10) -0.0008(10) 0.0030(11) C10 0.0369(15) 0.0276(14) 0.0338(14) -0.0030(10) -0.0035(11) 0.0092(12) C18 0.0426(17) 0.0342(16) 0.067(2) 0.0106(14) 0.0070(15) 0.0202(14) C2 0.0384(16) 0.0260(14) 0.0521(17) 0.0015(12) -0.0054(13) 0.0074(13) C17 0.0396(18) 0.0455(19) 0.084(2) 0.0136(17) -0.0054(16) 0.0233(16) P2 0.0295(4) 0.0358(4) 0.0297(3) 0.0054(3) 0.0006(3) 0.0141(3) F11 0.0394(9) 0.0456(10) 0.0465(9) 0.0165(8) -0.0009(7) 0.0145(8) F12 0.0556(12) 0.0460(11) 0.0751(13) 0.0092(9) 0.0226(10) 0.0277(9) F8 0.0638(12) 0.0442(10) 0.0443(10) -0.0007(8) -0.0161(9) 0.0074(9) F10 0.0449(11) 0.0528(11) 0.0501(11) 0.0156(8) -0.0178(8) -0.0030(9) F9 0.0490(10) 0.0485(10) 0.0355(9) 0.0127(7) -0.0065(7) 0.0143(8) F7 0.0779(15) 0.0770(15) 0.0970(17) 0.0289(12) 0.0482(13) 0.0529(13) P1 0.0875(7) 0.0778(6) 0.0330(4) -0.0037(4) -0.0026(4) 0.0682(6) F3 0.1004(17) 0.0950(17) 0.0650(13) -0.0068(11) -0.0121(12) 0.0826(15) F6 0.0642(13) 0.0593(13) 0.1114(18) 0.0143(12) 0.0177(12) 0.0442(11) F4 0.0995(17) 0.0668(14) 0.0462(11) 0.0005(9) 0.0088(11) 0.0413(13) F1 0.0945(17) 0.1087(19) 0.0691(14) -0.0206(13) -0.0235(12) 0.0746(16) F5 0.158(3) 0.0900(19) 0.0983(19) -0.0491(15) -0.0431(18) 0.087(2) F2 0.167(3) 0.208(3) 0.0472(13) 0.0280(16) 0.0281(15) 0.157(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 C14 1.854(3) . ? Ni1 C8 1.856(3) . ? Ni1 N6 1.953(2) . ? Ni1 N1 1.959(2) . ? N2 C8 1.357(3) . ? N2 C6 1.390(3) . ? N2 C5 1.410(3) . ? N1 C5 1.347(3) . ? N1 C1 1.347(3) . ? N3 C8 1.339(3) . ? N3 C7 1.390(3) . ? N3 C9 1.474(3) . ? N6 C19 1.347(3) . ? N6 C15 1.349(3) . ? N4 C14 1.341(3) . ? N4 C12 1.399(3) . ? N4 C11 1.468(3) . ? N5 C14 1.359(3) . ? N5 C13 1.387(3) . ? N5 C15 1.402(4) . ? C5 C4 1.373(4) . ? C1 C2 1.387(4) . ? C1 H1 0.9500 . ? C12 C13 1.331(4) . ? C12 H12 0.9500 . ? C15 C16 1.372(4) . ? C13 H13 0.9500 . ? C19 C18 1.385(4) . ? C19 H19 0.9500 . ? C7 C6 1.344(4) . ? C7 H7 0.9500 . ? C6 H6 0.9500 . ? C11 C10 1.518(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C16 C17 1.382(5) . ? C16 H16 0.9500 . ? C4 C3 1.378(4) . ? C4 H4 0.9500 . ? C3 C2 1.376(4) . ? C3 H3 0.9500 . ? C9 C10 1.525(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C18 C17 1.383(5) . ? C18 H18 0.9500 . ? C2 H2 0.9500 . ? C17 H17 0.9500 . ? P2 F7 1.577(2) . ? P2 F12 1.5854(19) . ? P2 F11 1.5915(17) . ? P2 F8 1.5941(18) . ? P2 F10 1.5995(18) . ? P2 F9 1.6042(17) . ? P1 F1 1.572(2) . ? P1 F2 1.579(2) . ? P1 F4 1.587(2) . ? P1 F5 1.590(3) . ? P1 F6 1.597(2) . ? P1 F3 1.600(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 C14 Ni1 C8 98.13(11) . . ? C14 Ni1 N6 82.90(10) . . ? C8 Ni1 N6 160.92(10) . . ? C14 Ni1 N1 157.99(10) . . ? C8 Ni1 N1 82.79(10) . . ? N6 Ni1 N1 103.39(9) . . ? C8 N2 C6 111.3(2) . . ? C8 N2 C5 116.9(2) . . ? C6 N2 C5 131.7(2) . . ? C5 N1 C1 116.7(2) . . ? C5 N1 Ni1 114.16(17) . . ? C1 N1 Ni1 127.99(18) . . ? C8 N3 C7 110.0(2) . . ? C8 N3 C9 125.0(2) . . ? C7 N3 C9 125.1(2) . . ? C19 N6 C15 117.9(2) . . ? C19 N6 Ni1 127.40(19) . . ? C15 N6 Ni1 114.03(18) . . ? C14 N4 C12 109.9(2) . . ? C14 N4 C11 125.8(2) . . ? C12 N4 C11 124.3(2) . . ? C14 N5 C13 110.7(2) . . ? C14 N5 C15 116.9(2) . . ? C13 N5 C15 132.2(2) . . ? N1 C5 C4 124.9(2) . . ? N1 C5 N2 111.5(2) . . ? C4 C5 N2 123.6(2) . . ? N3 C8 N2 105.2(2) . . ? N3 C8 Ni1 139.75(19) . . ? N2 C8 Ni1 114.17(17) . . ? N1 C1 C2 122.0(3) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C13 C12 N4 107.7(2) . . ? C13 C12 H12 126.1 . . ? N4 C12 H12 126.1 . . ? N6 C15 C16 123.8(3) . . ? N6 C15 N5 111.7(2) . . ? C16 C15 N5 124.5(3) . . ? C12 C13 N5 106.3(2) . . ? C12 C13 H13 126.8 . . ? N5 C13 H13 126.8 . . ? N6 C19 C18 121.7(3) . . ? N6 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C6 C7 N3 108.2(2) . . ? C6 C7 H7 125.9 . . ? N3 C7 H7 125.9 . . ? C7 C6 N2 105.2(2) . . ? C7 C6 H6 127.4 . . ? N2 C6 H6 127.4 . . ? N4 C14 N5 105.3(2) . . ? N4 C14 Ni1 139.14(19) . . ? N5 C14 Ni1 113.97(19) . . ? N4 C11 C10 113.1(2) . . ? N4 C11 H11A 109.0 . . ? C10 C11 H11A 109.0 . . ? N4 C11 H11B 109.0 . . ? C10 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C15 C16 C17 117.8(3) . . ? C15 C16 H16 121.1 . . ? C17 C16 H16 121.1 . . ? C5 C4 C3 117.2(3) . . ? C5 C4 H4 121.4 . . ? C3 C4 H4 121.4 . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? N3 C9 C10 112.3(2) . . ? N3 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? N3 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 113.6(2) . . ? C11 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C17 C18 C19 119.1(3) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C3 C2 C1 119.4(3) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C16 C17 C18 119.7(3) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? F7 P2 F12 179.32(14) . . ? F7 P2 F11 90.02(11) . . ? F12 P2 F11 89.64(10) . . ? F7 P2 F8 91.37(13) . . ? F12 P2 F8 89.22(12) . . ? F11 P2 F8 90.33(10) . . ? F7 P2 F10 89.59(13) . . ? F12 P2 F10 89.83(12) . . ? F11 P2 F10 90.66(9) . . ? F8 P2 F10 178.62(12) . . ? F7 P2 F9 90.16(11) . . ? F12 P2 F9 90.17(10) . . ? F11 P2 F9 179.19(12) . . ? F8 P2 F9 90.46(9) . . ? F10 P2 F9 88.54(9) . . ? F1 P1 F2 90.44(14) . . ? F1 P1 F4 90.63(14) . . ? F2 P1 F4 178.92(15) . . ? F1 P1 F5 91.48(15) . . ? F2 P1 F5 90.30(18) . . ? F4 P1 F5 89.84(15) . . ? F1 P1 F6 89.89(13) . . ? F2 P1 F6 90.68(17) . . ? F4 P1 F6 89.15(12) . . ? F5 P1 F6 178.31(15) . . ? F1 P1 F3 179.30(14) . . ? F2 P1 F3 89.68(14) . . ? F4 P1 F3 89.25(13) . . ? F5 P1 F3 89.22(14) . . ? F6 P1 F3 89.41(12) . . ? 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 C14 Ni1 N1 C5 92.0(3) . . . . ? C8 Ni1 N1 C5 -1.87(18) . . . . ? N6 Ni1 N1 C5 -163.52(17) . . . . ? C14 Ni1 N1 C1 -75.3(4) . . . . ? C8 Ni1 N1 C1 -169.1(2) . . . . ? N6 Ni1 N1 C1 29.2(2) . . . . ? C14 Ni1 N6 C19 -170.1(2) . . . . ? C8 Ni1 N6 C19 -75.8(4) . . . . ? N1 Ni1 N6 C19 31.3(2) . . . . ? C14 Ni1 N6 C15 -0.16(18) . . . . ? C8 Ni1 N6 C15 94.2(3) . . . . ? N1 Ni1 N6 C15 -158.71(17) . . . . ? C1 N1 C5 C4 -3.8(4) . . . . ? Ni1 N1 C5 C4 -172.6(2) . . . . ? C1 N1 C5 N2 174.3(2) . . . . ? Ni1 N1 C5 N2 5.5(3) . . . . ? C8 N2 C5 N1 -7.7(3) . . . . ? C6 N2 C5 N1 172.0(2) . . . . ? C8 N2 C5 C4 170.4(2) . . . . ? C6 N2 C5 C4 -9.9(4) . . . . ? C7 N3 C8 N2 2.4(3) . . . . ? C9 N3 C8 N2 -177.4(2) . . . . ? C7 N3 C8 Ni1 170.6(2) . . . . ? C9 N3 C8 Ni1 -9.2(4) . . . . ? C6 N2 C8 N3 -1.8(3) . . . . ? C5 N2 C8 N3 178.0(2) . . . . ? C6 N2 C8 Ni1 -173.48(17) . . . . ? C5 N2 C8 Ni1 6.3(3) . . . . ? C14 Ni1 C8 N3 32.3(3) . . . . ? N6 Ni1 C8 N3 -59.5(5) . . . . ? N1 Ni1 C8 N3 -169.9(3) . . . . ? C14 Ni1 C8 N2 -160.21(18) . . . . ? N6 Ni1 C8 N2 108.0(3) . . . . ? N1 Ni1 C8 N2 -2.41(17) . . . . ? C5 N1 C1 C2 2.4(4) . . . . ? Ni1 N1 C1 C2 169.4(2) . . . . ? C14 N4 C12 C13 -0.4(3) . . . . ? C11 N4 C12 C13 176.3(2) . . . . ? C19 N6 C15 C16 -3.3(4) . . . . ? Ni1 N6 C15 C16 -174.3(2) . . . . ? C19 N6 C15 N5 175.0(2) . . . . ? Ni1 N6 C15 N5 4.1(3) . . . . ? C14 N5 C15 N6 -7.5(3) . . . . ? C13 N5 C15 N6 167.9(2) . . . . ? C14 N5 C15 C16 170.8(3) . . . . ? C13 N5 C15 C16 -13.8(4) . . . . ? N4 C12 C13 N5 0.2(3) . . . . ? C14 N5 C13 C12 0.1(3) . . . . ? C15 N5 C13 C12 -175.5(3) . . . . ? C15 N6 C19 C18 1.6(4) . . . . ? Ni1 N6 C19 C18 171.3(2) . . . . ? C8 N3 C7 C6 -2.1(3) . . . . ? C9 N3 C7 C6 177.6(2) . . . . ? N3 C7 C6 N2 0.9(3) . . . . ? C8 N2 C6 C7 0.5(3) . . . . ? C5 N2 C6 C7 -179.2(2) . . . . ? C12 N4 C14 N5 0.4(3) . . . . ? C11 N4 C14 N5 -176.2(2) . . . . ? C12 N4 C14 Ni1 164.2(2) . . . . ? C11 N4 C14 Ni1 -12.4(4) . . . . ? C13 N5 C14 N4 -0.4(3) . . . . ? C15 N5 C14 N4 176.0(2) . . . . ? C13 N5 C14 Ni1 -168.83(17) . . . . ? C15 N5 C14 Ni1 7.6(3) . . . . ? C8 Ni1 C14 N4 32.4(3) . . . . ? N6 Ni1 C14 N4 -166.8(3) . . . . ? N1 Ni1 C14 N4 -58.5(4) . . . . ? C8 Ni1 C14 N5 -164.74(18) . . . . ? N6 Ni1 C14 N5 -3.96(18) . . . . ? N1 Ni1 C14 N5 104.4(3) . . . . ? C14 N4 C11 C10 -84.0(3) . . . . ? C12 N4 C11 C10 99.8(3) . . . . ? N6 C15 C16 C17 2.2(4) . . . . ? N5 C15 C16 C17 -175.9(3) . . . . ? N1 C5 C4 C3 2.0(4) . . . . ? N2 C5 C4 C3 -175.9(2) . . . . ? C5 C4 C3 C2 1.3(4) . . . . ? C8 N3 C9 C10 -86.2(3) . . . . ? C7 N3 C9 C10 94.1(3) . . . . ? N4 C11 C10 C9 57.2(3) . . . . ? N3 C9 C10 C11 55.7(3) . . . . ? N6 C19 C18 C17 1.0(4) . . . . ? C4 C3 C2 C1 -2.5(5) . . . . ? N1 C1 C2 C3 0.6(5) . . . . ? C15 C16 C17 C18 0.5(5) . . . . ? C19 C18 C17 C16 -2.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.676 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.061 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.000 -0.001 931 282 ' ' 2 0.333 0.667 0.736 926 282 ' ' 3 0.667 0.333 0.403 926 282 ' ' _platon_squeeze_details ; ;