# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_eh10 #TrackingRef 'eh10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H20 N4 Ni' _chemical_formula_sum 'C17 H20 N4 Ni' _chemical_formula_weight 339.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 14.9461(4) _cell_length_b 7.3243(2) _cell_length_c 15.6793(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.463(2) _cell_angle_gamma 90.00 _cell_volume 1586.18(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4316 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 28.31 _exptl_crystal_description black _exptl_crystal_colour parallelepiped _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 1.225 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6401 _exptl_absorpt_correction_T_max 0.9413 _exptl_absorpt_process_details SADABS _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 X8 APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14568 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 28.42 _reflns_number_total 3949 _reflns_number_gt 3240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.0436P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3949 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 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 0.275695(11) 0.68861(2) 0.140394(12) 0.02050(5) Uani 1 1 d . . . N1 N 0.24613(8) 0.44506(16) 0.09496(8) 0.0226(3) Uani 1 1 d . . . N2 N 0.14733(8) 0.68996(16) 0.13093(8) 0.0227(3) Uani 1 1 d . . . N3 N 0.32050(8) 0.87108(17) 0.23076(8) 0.0233(3) Uani 1 1 d . . . N4 N 0.38715(8) 0.75144(17) 0.11585(8) 0.0217(3) Uani 1 1 d . . . C1 C 0.30143(11) 0.3186(2) 0.07464(11) 0.0257(3) Uani 1 1 d . . . C2 C 0.26680(12) 0.1554(2) 0.03362(11) 0.0296(4) Uani 1 1 d . . . C3 C 0.16941(12) 0.1110(2) 0.01130(11) 0.0314(4) Uani 1 1 d . . . C4 C 0.11186(11) 0.2328(2) 0.03272(11) 0.0292(4) Uani 1 1 d . . . C5 C 0.15087(10) 0.3993(2) 0.07529(10) 0.0240(3) Uani 1 1 d . . . C6 C 0.10039(10) 0.5350(2) 0.10279(10) 0.0237(3) Uani 1 1 d . . . C7 C 0.10665(10) 0.8243(2) 0.17480(11) 0.0265(3) Uani 1 1 d . . . C8 C 0.17513(11) 0.8641(2) 0.27502(11) 0.0307(4) Uani 1 1 d . . . C9 C 0.26482(11) 0.9663(2) 0.27660(11) 0.0303(4) Uani 1 1 d . . . C10 C 0.40229(10) 0.9505(2) 0.23617(10) 0.0255(3) Uani 1 1 d . . . C11 C 0.44447(10) 0.8808(2) 0.17639(10) 0.0232(3) Uani 1 1 d . . . C12 C 0.53203(11) 0.9394(2) 0.17242(11) 0.0286(3) Uani 1 1 d . . . C13 C 0.56133(11) 0.8706(2) 0.10641(11) 0.0313(4) Uani 1 1 d . . . C14 C 0.50304(11) 0.7409(2) 0.04422(11) 0.0294(3) Uani 1 1 d . . . C15 C 0.41944(11) 0.68536(19) 0.05174(11) 0.0243(3) Uani 1 1 d . . . C16 C 0.20211(13) 0.6874(3) 0.33055(12) 0.0415(5) Uani 1 1 d . . . H16A H 0.1430 0.6230 0.3262 0.062 Uiso 1 1 calc R . . H16B H 0.2408 0.7158 0.3953 0.062 Uiso 1 1 calc R . . H16C H 0.2399 0.6097 0.3058 0.062 Uiso 1 1 calc R . . C17 C 0.12058(13) 0.9915(3) 0.31631(13) 0.0509(5) Uani 1 1 d . . . H17A H 0.1009 1.1022 0.2786 0.076 Uiso 1 1 calc R . . H17B H 0.1630 1.0247 0.3794 0.076 Uiso 1 1 calc R . . H17C H 0.0630 0.9289 0.3173 0.076 Uiso 1 1 calc R . . H1 H 0.3704(11) 0.351(2) 0.0952(11) 0.025(4) Uiso 1 1 d . . . H15 H 0.3790(10) 0.601(2) 0.0123(10) 0.014(4) Uiso 1 1 d . . . H7B H 0.0448(11) 0.778(2) 0.1732(11) 0.020(4) Uiso 1 1 d . . . H10 H 0.4274(11) 1.055(2) 0.2730(11) 0.028(4) Uiso 1 1 d . . . H6 H 0.0376(11) 0.512(2) 0.1042(11) 0.024(4) Uiso 1 1 d . . . H7A H 0.0924(10) 0.942(2) 0.1376(10) 0.018(4) Uiso 1 1 d . . . H9B H 0.2431(10) 1.089(2) 0.2475(10) 0.023(4) Uiso 1 1 d . . . H13 H 0.6184(12) 0.900(2) 0.1042(12) 0.035(5) Uiso 1 1 d . . . H2 H 0.3087(11) 0.068(2) 0.0204(11) 0.028(4) Uiso 1 1 d . . . H12 H 0.5667(11) 1.023(2) 0.2095(11) 0.026(4) Uiso 1 1 d . . . H4 H 0.0425(13) 0.209(2) 0.0209(12) 0.031(5) Uiso 1 1 d . . . H14 H 0.5189(14) 0.698(2) -0.0025(15) 0.045(6) Uiso 1 1 d . . . H3 H 0.1425(13) -0.004(3) -0.0163(13) 0.045(6) Uiso 1 1 d . . . H9A H 0.3092(12) 0.987(2) 0.3402(13) 0.036(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01835(8) 0.02117(10) 0.02120(10) -0.00251(7) 0.00669(7) -0.00035(6) N1 0.0234(5) 0.0221(6) 0.0211(5) 0.0011(5) 0.0072(4) 0.0006(5) N2 0.0206(5) 0.0264(6) 0.0209(6) -0.0005(5) 0.0077(4) 0.0025(5) N3 0.0237(5) 0.0262(6) 0.0198(5) -0.0030(5) 0.0079(4) -0.0001(5) N4 0.0207(5) 0.0208(5) 0.0227(6) 0.0006(5) 0.0072(4) 0.0005(5) C1 0.0271(6) 0.0250(7) 0.0253(7) 0.0022(6) 0.0104(6) 0.0034(6) C2 0.0411(8) 0.0214(7) 0.0270(7) 0.0025(6) 0.0138(6) 0.0048(6) C3 0.0442(8) 0.0226(7) 0.0250(7) -0.0028(6) 0.0105(6) -0.0043(7) C4 0.0319(7) 0.0281(8) 0.0247(7) 0.0026(6) 0.0077(6) -0.0057(6) C5 0.0252(6) 0.0252(7) 0.0201(6) 0.0027(6) 0.0070(5) -0.0012(6) C6 0.0189(6) 0.0300(7) 0.0210(7) 0.0007(6) 0.0064(5) -0.0022(5) C7 0.0236(6) 0.0311(8) 0.0262(7) -0.0021(6) 0.0111(6) 0.0041(6) C8 0.0295(7) 0.0402(8) 0.0249(7) -0.0057(6) 0.0132(6) 0.0009(7) C9 0.0335(7) 0.0332(8) 0.0259(7) -0.0093(6) 0.0132(6) -0.0010(6) C10 0.0241(6) 0.0254(7) 0.0227(7) -0.0044(6) 0.0043(5) -0.0024(6) C11 0.0237(6) 0.0222(7) 0.0205(7) 0.0008(6) 0.0047(5) -0.0002(6) C12 0.0262(7) 0.0271(7) 0.0286(7) -0.0005(6) 0.0062(6) -0.0052(6) C13 0.0276(7) 0.0324(8) 0.0366(8) 0.0039(7) 0.0153(6) -0.0035(6) C14 0.0343(7) 0.0302(8) 0.0279(8) 0.0013(6) 0.0167(6) 0.0024(6) C15 0.0260(6) 0.0228(7) 0.0227(7) -0.0015(6) 0.0076(5) 0.0008(5) C16 0.0412(9) 0.0575(12) 0.0253(8) 0.0079(8) 0.0120(7) -0.0085(8) C17 0.0434(9) 0.0709(13) 0.0477(10) -0.0262(9) 0.0278(8) -0.0065(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.8670(12) . ? Ni1 N3 1.8754(12) . ? Ni1 N4 1.9038(12) . ? Ni1 N1 1.9091(12) . ? N1 C1 1.3577(19) . ? N1 C5 1.3780(18) . ? N2 C6 1.3186(18) . ? N2 C7 1.4599(19) . ? N3 C10 1.3269(19) . ? N3 C9 1.467(2) . ? N4 C15 1.360(2) . ? N4 C11 1.3827(18) . ? C1 C2 1.362(2) . ? C2 C3 1.399(2) . ? C3 C4 1.367(2) . ? C4 C5 1.405(2) . ? C5 C6 1.411(2) . ? C7 C8 1.540(2) . ? C8 C16 1.526(3) . ? C8 C9 1.527(2) . ? C8 C17 1.535(2) . ? C10 C11 1.410(2) . ? C11 C12 1.401(2) . ? C12 C13 1.365(2) . ? C13 C14 1.401(2) . ? C14 C15 1.361(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 N2 Ni1 N3 96.65(5) . . ? N2 Ni1 N4 159.17(5) . . ? N3 Ni1 N4 83.86(5) . . ? N2 Ni1 N1 83.74(5) . . ? N3 Ni1 N1 155.89(5) . . ? N4 Ni1 N1 104.25(5) . . ? C1 N1 C5 116.82(12) . . ? C1 N1 Ni1 130.54(10) . . ? C5 N1 Ni1 112.51(10) . . ? C6 N2 C7 118.29(13) . . ? C6 N2 Ni1 114.91(10) . . ? C7 N2 Ni1 124.51(9) . . ? C10 N3 C9 116.19(13) . . ? C10 N3 Ni1 114.53(10) . . ? C9 N3 Ni1 127.10(10) . . ? C15 N4 C11 116.73(12) . . ? C15 N4 Ni1 130.44(10) . . ? C11 N4 Ni1 112.79(10) . . ? N1 C1 C2 123.62(14) . . ? C1 C2 C3 119.57(15) . . ? C4 C3 C2 118.60(15) . . ? C3 C4 C5 119.80(15) . . ? N1 C5 C4 121.54(14) . . ? N1 C5 C6 112.81(12) . . ? C4 C5 C6 125.65(14) . . ? N2 C6 C5 115.49(13) . . ? N2 C7 C8 111.97(12) . . ? C16 C8 C9 111.56(13) . . ? C16 C8 C17 110.00(15) . . ? C9 C8 C17 107.45(14) . . ? C16 C8 C7 110.43(14) . . ? C9 C8 C7 110.26(13) . . ? C17 C8 C7 106.98(13) . . ? N3 C9 C8 114.71(13) . . ? N3 C10 C11 115.70(13) . . ? N4 C11 C12 121.58(14) . . ? N4 C11 C10 112.79(13) . . ? C12 C11 C10 125.54(14) . . ? C13 C12 C11 119.76(14) . . ? C12 C13 C14 118.93(15) . . ? C15 C14 C13 119.31(15) . . ? N4 C15 C14 123.68(14) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.42 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.489 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.065 _database_code_depnum_ccdc_archive 'CCDC 863631' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_vw6 #TrackingRef 'vw6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H40 N8 Ni2, 2(C F3 O3 S)' _chemical_formula_sum 'C36 H40 F6 N8 Ni2 O6 S2' _chemical_formula_weight 976.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0760(7) _cell_length_b 10.6657(7) _cell_length_c 19.6623(14) _cell_angle_alpha 90.050(3) _cell_angle_beta 97.940(3) _cell_angle_gamma 105.384(3) _cell_volume 2016.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9892 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 29.37 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5527 _exptl_absorpt_correction_T_max 0.9725 _exptl_absorpt_process_details SADABS _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 X8 APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33779 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 28.28 _reflns_number_total 9861 _reflns_number_gt 8200 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+1.0061P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9861 _refine_ls_number_parameters 545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.96115(2) -0.14850(2) 0.257309(10) 0.01714(6) Uani 1 1 d . . . Ni2 Ni 0.83946(2) 0.073871(19) 0.231001(10) 0.01487(5) Uani 1 1 d . . . N1 N 1.03878(15) -0.24408(14) 0.33260(7) 0.0214(3) Uani 1 1 d . . . N2 N 1.01880(15) -0.26590(13) 0.20052(7) 0.0213(3) Uani 1 1 d . . . N3 N 1.00880(14) 0.00869(13) 0.20360(7) 0.0165(3) Uani 1 1 d . . . N4 N 0.99488(14) 0.16322(13) 0.30992(7) 0.0182(3) Uani 1 1 d . . . N5 N 0.82406(14) 0.23452(13) 0.17427(7) 0.0171(3) Uani 1 1 d . . . N6 N 0.68907(14) 0.12812(13) 0.27616(7) 0.0185(3) Uani 1 1 d . . . N7 N 0.80215(14) -0.09426(13) 0.28287(7) 0.0170(3) Uani 1 1 d . . . N8 N 0.71031(14) -0.05327(13) 0.15252(7) 0.0178(3) Uani 1 1 d . . . C1 C 1.05911(19) -0.22229(19) 0.40063(9) 0.0264(4) Uani 1 1 d . . . H1A H 1.0231 -0.1578 0.4189 0.032 Uiso 1 1 calc R . . C2 C 1.1306(2) -0.2898(2) 0.44572(10) 0.0303(4) Uani 1 1 d . . . H2A H 1.1453 -0.2698 0.4937 0.036 Uiso 1 1 calc R . . C3 C 1.1801(2) -0.3862(2) 0.42010(10) 0.0338(4) Uani 1 1 d . . . H3A H 1.2283 -0.4343 0.4502 0.041 Uiso 1 1 calc R . . C4 C 1.1584(2) -0.41179(19) 0.34995(10) 0.0323(4) Uani 1 1 d . . . H4A H 1.1906 -0.4784 0.3310 0.039 Uiso 1 1 calc R . . C5 C 1.08881(19) -0.33863(17) 0.30759(9) 0.0246(4) Uani 1 1 d . . . C6 C 1.0738(2) -0.34767(17) 0.23290(10) 0.0273(4) Uani 1 1 d . . . H6A H 1.1033 -0.4111 0.2094 0.033 Uiso 1 1 calc R . . C7 C 1.02024(19) -0.25153(17) 0.12680(9) 0.0238(4) Uani 1 1 d . . . H7A H 0.9241 -0.2645 0.1030 0.029 Uiso 1 1 calc R . . H7B H 1.0594 -0.3181 0.1083 0.029 Uiso 1 1 calc R . . C8 C 1.10878(18) -0.11493(17) 0.11368(8) 0.0207(3) Uani 1 1 d . . . C9 C 1.04076(17) -0.00826(16) 0.13335(8) 0.0187(3) Uani 1 1 d . . . H9A H 1.1018 0.0761 0.1221 0.022 Uiso 1 1 calc R . . H9B H 0.9522 -0.0218 0.1018 0.022 Uiso 1 1 calc R . . C10 C 1.11007(17) 0.02640(15) 0.25858(8) 0.0187(3) Uani 1 1 d . . . H10A H 1.2049 0.0241 0.2500 0.022 Uiso 1 1 calc R . . C11 C 1.10090(17) 0.10682(16) 0.31715(8) 0.0184(3) Uani 1 1 d . . . C12 C 1.19791(18) 0.12691(18) 0.37677(9) 0.0253(4) Uani 1 1 d . . . H12A H 1.2703 0.0844 0.3816 0.030 Uiso 1 1 calc R . . C13 C 1.1873(2) 0.20961(19) 0.42888(9) 0.0287(4) Uani 1 1 d . . . H13A H 1.2517 0.2241 0.4700 0.034 Uiso 1 1 calc R . . C14 C 1.08137(19) 0.27090(18) 0.42013(9) 0.0271(4) Uani 1 1 d . . . H14A H 1.0732 0.3296 0.4547 0.032 Uiso 1 1 calc R . . C15 C 0.98782(18) 0.24518(16) 0.36030(9) 0.0228(3) Uani 1 1 d . . . H15A H 0.9152 0.2874 0.3545 0.027 Uiso 1 1 calc R . . C16 C 0.88926(17) 0.28370(16) 0.12172(9) 0.0203(3) Uani 1 1 d . . . H16A H 0.9666 0.2546 0.1126 0.024 Uiso 1 1 calc R . . C17 C 0.84871(19) 0.37587(17) 0.07979(9) 0.0253(4) Uani 1 1 d . . . H17A H 0.8969 0.4084 0.0425 0.030 Uiso 1 1 calc R . . C18 C 0.7376(2) 0.41909(19) 0.09325(10) 0.0306(4) Uani 1 1 d . . . H18A H 0.7065 0.4806 0.0648 0.037 Uiso 1 1 calc R . . C19 C 0.6715(2) 0.37155(19) 0.14897(10) 0.0305(4) Uani 1 1 d . . . H19A H 0.5964 0.4021 0.1601 0.037 Uiso 1 1 calc R . . C20 C 0.71646(17) 0.27914(16) 0.18813(9) 0.0198(3) Uani 1 1 d . . . C21 C 0.65080(18) 0.22192(17) 0.24718(9) 0.0221(3) Uani 1 1 d . . . H21A H 0.5812 0.2543 0.2634 0.027 Uiso 1 1 calc R . . C22 C 0.63913(18) 0.08115(17) 0.34066(9) 0.0228(3) Uani 1 1 d . . . H22A H 0.5475 0.0983 0.3414 0.027 Uiso 1 1 calc R . . H22B H 0.7041 0.1328 0.3793 0.027 Uiso 1 1 calc R . . C23 C 0.62402(18) -0.06349(17) 0.35326(9) 0.0219(3) Uani 1 1 d . . . C24 C 0.76241(18) -0.10146(17) 0.35206(8) 0.0207(3) Uani 1 1 d . . . H24A H 0.8373 -0.0421 0.3841 0.025 Uiso 1 1 calc R . . H24B H 0.7516 -0.1911 0.3681 0.025 Uiso 1 1 calc R . . C25 C 0.74902(17) -0.20109(16) 0.23976(9) 0.0193(3) Uani 1 1 d . . . H25A H 0.7002 -0.2833 0.2602 0.023 Uiso 1 1 calc R . . C26 C 0.69648(17) -0.17893(16) 0.16892(8) 0.0189(3) Uani 1 1 d . . . C27 C 0.62895(19) -0.28060(17) 0.12170(10) 0.0256(4) Uani 1 1 d . . . H27A H 0.6182 -0.3682 0.1345 0.031 Uiso 1 1 calc R . . C28 C 0.5776(2) -0.25386(18) 0.05628(10) 0.0297(4) Uani 1 1 d . . . H28A H 0.5321 -0.3225 0.0234 0.036 Uiso 1 1 calc R . . C29 C 0.59337(19) -0.12561(18) 0.03927(9) 0.0276(4) Uani 1 1 d . . . H29A H 0.5596 -0.1044 -0.0056 0.033 Uiso 1 1 calc R . . C30 C 0.65910(18) -0.02874(17) 0.08871(9) 0.0219(3) Uani 1 1 d . . . H30A H 0.6685 0.0593 0.0770 0.026 Uiso 1 1 calc R . . C31 C 1.25975(19) -0.0951(2) 0.14740(10) 0.0297(4) Uani 1 1 d . . . H31A H 1.3014 -0.1546 0.1252 0.045 Uiso 1 1 calc R . . H31B H 1.2618 -0.1129 0.1964 0.045 Uiso 1 1 calc R . . H31C H 1.3126 -0.0050 0.1422 0.045 Uiso 1 1 calc R . . C32 C 1.1080(2) -0.10742(19) 0.03568(9) 0.0288(4) Uani 1 1 d . . . H32A H 1.1535 -0.1705 0.0200 0.043 Uiso 1 1 calc R . . H32B H 1.1583 -0.0195 0.0247 0.043 Uiso 1 1 calc R . . H32C H 1.0118 -0.1274 0.0126 0.043 Uiso 1 1 calc R . . C33 C 0.50568(19) -0.14747(19) 0.30219(10) 0.0296(4) Uani 1 1 d . . . H33A H 0.4174 -0.1315 0.3100 0.044 Uiso 1 1 calc R . . H33B H 0.5012 -0.2395 0.3086 0.044 Uiso 1 1 calc R . . H33C H 0.5225 -0.1252 0.2552 0.044 Uiso 1 1 calc R . . C34 C 0.5870(2) -0.0863(2) 0.42635(10) 0.0324(4) Uani 1 1 d . . . H34A H 0.6652 -0.0376 0.4597 0.049 Uiso 1 1 calc R . . H34B H 0.5679 -0.1793 0.4352 0.049 Uiso 1 1 calc R . . H34C H 0.5045 -0.0564 0.4307 0.049 Uiso 1 1 calc R . . S1 S 0.71189(5) -0.50932(4) 0.38575(2) 0.02325(9) Uani 1 1 d . . . S2 S 0.26688(5) -0.57934(5) 0.09182(2) 0.02682(10) Uani 1 1 d . . . F1 F 0.46363(16) -0.47561(17) 0.38605(9) 0.0648(4) Uani 1 1 d . . . F2 F 0.51454(15) -0.61084(16) 0.45879(7) 0.0550(4) Uani 1 1 d . . . F3 F 0.46276(13) -0.66586(13) 0.35113(7) 0.0482(3) Uani 1 1 d . . . F4 F 0.38896(16) -0.51381(16) 0.21798(7) 0.0627(4) Uani 1 1 d . . . F5 F 0.34704(15) -0.71573(15) 0.19259(8) 0.0579(4) Uani 1 1 d . . . F6 F 0.18094(13) -0.63582(15) 0.21169(6) 0.0475(3) Uani 1 1 d . . . O1 O 0.70675(17) -0.48124(14) 0.31413(7) 0.0400(4) Uani 1 1 d . . . O2 O 0.76416(15) -0.61877(14) 0.40469(7) 0.0352(3) Uani 1 1 d . . . O3 O 0.76122(16) -0.39881(14) 0.43311(8) 0.0416(4) Uani 1 1 d . . . O4 O 0.40415(13) -0.54699(13) 0.07253(7) 0.0304(3) Uani 1 1 d . . . O5 O 0.20329(19) -0.47413(18) 0.09230(9) 0.0568(5) Uani 1 1 d . . . O6 O 0.17656(16) -0.70000(17) 0.06257(8) 0.0509(4) Uani 1 1 d . . . C1S C 0.5296(2) -0.5676(2) 0.39599(10) 0.0333(4) Uani 1 1 d . . . C2S C 0.2974(2) -0.6114(2) 0.18278(10) 0.0339(4) 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 0.02031(11) 0.01741(10) 0.01615(11) 0.00282(8) 0.00228(8) 0.00949(8) Ni2 0.01615(10) 0.01428(10) 0.01531(10) 0.00105(7) 0.00153(8) 0.00638(8) N1 0.0214(7) 0.0232(7) 0.0217(7) 0.0055(6) 0.0033(6) 0.0095(6) N2 0.0269(8) 0.0187(7) 0.0204(7) 0.0012(5) 0.0032(6) 0.0099(6) N3 0.0190(7) 0.0168(6) 0.0147(6) 0.0016(5) 0.0017(5) 0.0068(5) N4 0.0182(7) 0.0187(7) 0.0177(7) -0.0006(5) 0.0024(5) 0.0051(5) N5 0.0174(7) 0.0150(6) 0.0192(7) 0.0005(5) 0.0016(5) 0.0056(5) N6 0.0191(7) 0.0187(7) 0.0190(7) 0.0018(5) 0.0040(5) 0.0068(5) N7 0.0181(7) 0.0184(7) 0.0164(7) 0.0032(5) 0.0027(5) 0.0079(5) N8 0.0169(7) 0.0171(6) 0.0191(7) 0.0009(5) 0.0015(5) 0.0048(5) C1 0.0274(9) 0.0343(10) 0.0214(9) 0.0065(7) 0.0051(7) 0.0143(8) C2 0.0295(10) 0.0409(11) 0.0222(9) 0.0100(8) 0.0021(8) 0.0133(8) C3 0.0359(11) 0.0388(11) 0.0311(10) 0.0153(8) 0.0009(8) 0.0197(9) C4 0.0381(11) 0.0322(10) 0.0332(11) 0.0093(8) 0.0036(9) 0.0217(9) C5 0.0267(9) 0.0240(9) 0.0263(9) 0.0072(7) 0.0044(7) 0.0118(7) C6 0.0361(10) 0.0226(9) 0.0283(10) 0.0019(7) 0.0043(8) 0.0167(8) C7 0.0325(10) 0.0234(8) 0.0185(8) -0.0004(6) 0.0028(7) 0.0132(7) C8 0.0234(8) 0.0254(8) 0.0164(8) -0.0001(6) 0.0034(6) 0.0118(7) C9 0.0222(8) 0.0212(8) 0.0152(8) 0.0031(6) 0.0037(6) 0.0095(6) C10 0.0182(8) 0.0205(8) 0.0186(8) 0.0025(6) 0.0033(6) 0.0073(6) C11 0.0180(8) 0.0193(8) 0.0173(8) 0.0015(6) 0.0024(6) 0.0039(6) C12 0.0218(9) 0.0301(9) 0.0228(9) 0.0009(7) -0.0012(7) 0.0068(7) C13 0.0276(9) 0.0332(10) 0.0198(9) -0.0023(7) -0.0041(7) 0.0025(8) C14 0.0293(10) 0.0275(9) 0.0220(9) -0.0057(7) 0.0047(7) 0.0029(7) C15 0.0234(9) 0.0212(8) 0.0237(9) -0.0026(7) 0.0044(7) 0.0054(7) C16 0.0198(8) 0.0193(8) 0.0224(8) 0.0006(6) 0.0040(7) 0.0059(6) C17 0.0309(10) 0.0216(8) 0.0247(9) 0.0063(7) 0.0076(7) 0.0073(7) C18 0.0386(11) 0.0282(10) 0.0315(10) 0.0132(8) 0.0083(8) 0.0184(8) C19 0.0335(10) 0.0316(10) 0.0354(11) 0.0127(8) 0.0128(8) 0.0205(8) C20 0.0208(8) 0.0182(8) 0.0228(8) 0.0034(6) 0.0041(7) 0.0087(6) C21 0.0209(8) 0.0248(8) 0.0247(9) 0.0022(7) 0.0070(7) 0.0114(7) C22 0.0257(9) 0.0265(9) 0.0211(8) 0.0051(7) 0.0103(7) 0.0120(7) C23 0.0232(8) 0.0260(9) 0.0190(8) 0.0069(7) 0.0069(7) 0.0090(7) C24 0.0235(9) 0.0240(8) 0.0169(8) 0.0057(6) 0.0038(6) 0.0101(7) C25 0.0189(8) 0.0160(7) 0.0235(8) 0.0027(6) 0.0034(6) 0.0054(6) C26 0.0181(8) 0.0182(8) 0.0216(8) 0.0012(6) 0.0034(6) 0.0064(6) C27 0.0284(9) 0.0164(8) 0.0306(10) -0.0023(7) 0.0024(7) 0.0045(7) C28 0.0314(10) 0.0275(9) 0.0259(9) -0.0080(7) -0.0015(8) 0.0033(8) C29 0.0281(9) 0.0319(10) 0.0196(9) -0.0012(7) -0.0041(7) 0.0066(8) C30 0.0228(8) 0.0211(8) 0.0212(8) 0.0029(6) 0.0005(7) 0.0065(7) C31 0.0244(9) 0.0394(11) 0.0299(10) -0.0030(8) 0.0040(8) 0.0167(8) C32 0.0369(11) 0.0354(10) 0.0183(9) 0.0004(7) 0.0077(8) 0.0149(8) C33 0.0225(9) 0.0316(10) 0.0342(10) 0.0059(8) 0.0047(8) 0.0064(8) C34 0.0357(11) 0.0435(11) 0.0248(10) 0.0134(8) 0.0141(8) 0.0173(9) S1 0.0272(2) 0.0205(2) 0.0216(2) 0.00142(16) 0.00149(17) 0.00660(17) S2 0.0228(2) 0.0328(2) 0.0249(2) 0.00111(18) 0.00341(17) 0.00747(18) F1 0.0491(9) 0.0819(11) 0.0762(11) -0.0134(9) -0.0035(8) 0.0460(8) F2 0.0495(8) 0.0789(10) 0.0354(7) 0.0010(7) 0.0217(6) 0.0071(7) F3 0.0328(7) 0.0559(8) 0.0458(8) -0.0178(6) 0.0078(6) -0.0067(6) F4 0.0590(10) 0.0766(11) 0.0321(7) -0.0086(7) -0.0051(7) -0.0116(8) F5 0.0553(9) 0.0668(10) 0.0640(10) 0.0337(8) 0.0177(7) 0.0330(8) F6 0.0396(7) 0.0730(10) 0.0342(7) 0.0089(6) 0.0163(6) 0.0168(7) O1 0.0520(9) 0.0361(8) 0.0263(7) 0.0102(6) 0.0059(7) 0.0022(7) O2 0.0408(8) 0.0374(8) 0.0360(8) 0.0070(6) 0.0063(6) 0.0248(6) O3 0.0459(9) 0.0311(8) 0.0410(9) -0.0115(6) -0.0041(7) 0.0039(6) O4 0.0239(7) 0.0316(7) 0.0335(7) 0.0015(6) 0.0080(6) 0.0018(5) O5 0.0678(12) 0.0656(12) 0.0583(11) 0.0213(9) 0.0202(9) 0.0491(10) O6 0.0338(8) 0.0620(11) 0.0427(9) -0.0179(8) 0.0104(7) -0.0142(7) C1S 0.0294(10) 0.0425(12) 0.0289(10) -0.0069(8) 0.0035(8) 0.0117(9) C2S 0.0295(10) 0.0420(12) 0.0300(10) 0.0048(9) 0.0051(8) 0.0085(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.9274(14) . ? Ni1 N3 1.9679(13) . ? Ni1 N7 1.9666(13) . ? Ni1 N1 1.9871(14) . ? Ni1 C25 2.0401(16) . ? Ni1 C10 2.0582(16) . ? Ni1 Ni2 2.9607(3) . ? Ni2 N7 2.0368(13) . ? Ni2 N6 2.0629(13) . ? Ni2 N5 2.0738(13) . ? Ni2 N4 2.0743(14) . ? Ni2 N8 2.1021(14) . ? Ni2 N3 2.1373(13) . ? N1 C1 1.336(2) . ? N1 C5 1.360(2) . ? N2 C6 1.278(2) . ? N2 C7 1.459(2) . ? N3 C10 1.356(2) . ? N3 C9 1.4824(19) . ? N4 C15 1.342(2) . ? N4 C11 1.350(2) . ? N5 C16 1.334(2) . ? N5 C20 1.353(2) . ? N6 C21 1.273(2) . ? N6 C22 1.468(2) . ? N7 C25 1.361(2) . ? N7 C24 1.467(2) . ? N8 C30 1.342(2) . ? N8 C26 1.354(2) . ? C1 C2 1.387(2) . ? C2 C3 1.379(3) . ? C3 C4 1.382(3) . ? C4 C5 1.387(2) . ? C5 C6 1.456(3) . ? C7 C8 1.536(2) . ? C8 C31 1.533(2) . ? C8 C32 1.535(2) . ? C8 C9 1.549(2) . ? C10 C11 1.463(2) . ? C11 C12 1.395(2) . ? C12 C13 1.385(3) . ? C13 C14 1.384(3) . ? C14 C15 1.380(2) . ? C16 C17 1.391(2) . ? C17 C18 1.376(3) . ? C18 C19 1.387(3) . ? C19 C20 1.383(2) . ? C20 C21 1.469(2) . ? C22 C23 1.533(2) . ? C23 C33 1.528(3) . ? C23 C34 1.537(2) . ? C23 C24 1.555(2) . ? C25 C26 1.463(2) . ? C26 C27 1.390(2) . ? C27 C28 1.378(3) . ? C28 C29 1.381(3) . ? C29 C30 1.381(2) . ? S1 O2 1.4323(14) . ? S1 O3 1.4364(14) . ? S1 O1 1.4367(14) . ? S1 C1S 1.815(2) . ? S2 O6 1.4310(16) . ? S2 O5 1.4328(16) . ? S2 O4 1.4380(13) . ? S2 C2S 1.821(2) . ? F1 C1S 1.324(2) . ? F2 C1S 1.333(2) . ? F3 C1S 1.338(2) . ? F4 C2S 1.314(2) . ? F5 C2S 1.339(2) . ? F6 C2S 1.338(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 N2 Ni1 N3 98.81(6) . . ? N2 Ni1 N7 145.50(6) . . ? N3 Ni1 N7 89.39(5) . . ? N2 Ni1 N1 82.54(6) . . ? N3 Ni1 N1 142.50(6) . . ? N7 Ni1 N1 110.66(6) . . ? N2 Ni1 C25 105.95(6) . . ? N3 Ni1 C25 102.50(6) . . ? N7 Ni1 C25 39.66(6) . . ? N1 Ni1 C25 113.21(6) . . ? N2 Ni1 C10 105.34(6) . . ? N3 Ni1 C10 39.28(6) . . ? N7 Ni1 C10 102.11(6) . . ? N1 Ni1 C10 103.93(6) . . ? C25 Ni1 C10 133.71(6) . . ? N2 Ni1 Ni2 134.83(4) . . ? N3 Ni1 Ni2 46.16(4) . . ? N7 Ni1 Ni2 43.23(4) . . ? N1 Ni1 Ni2 142.43(4) . . ? C25 Ni1 Ni2 66.37(5) . . ? C10 Ni1 Ni2 67.36(4) . . ? N7 Ni2 N6 89.52(5) . . ? N7 Ni2 N5 165.76(5) . . ? N6 Ni2 N5 80.13(5) . . ? N7 Ni2 N4 90.18(5) . . ? N6 Ni2 N4 92.27(5) . . ? N5 Ni2 N4 99.91(5) . . ? N7 Ni2 N8 80.66(5) . . ? N6 Ni2 N8 99.16(5) . . ? N5 Ni2 N8 91.28(5) . . ? N4 Ni2 N8 165.24(5) . . ? N7 Ni2 N3 83.01(5) . . ? N6 Ni2 N3 169.07(5) . . ? N5 Ni2 N3 108.51(5) . . ? N4 Ni2 N3 79.83(5) . . ? N8 Ni2 N3 87.54(5) . . ? N7 Ni2 Ni1 41.40(4) . . ? N6 Ni2 Ni1 130.33(4) . . ? N5 Ni2 Ni1 149.47(4) . . ? N4 Ni2 Ni1 82.83(4) . . ? N8 Ni2 Ni1 82.65(4) . . ? N3 Ni2 Ni1 41.62(4) . . ? C1 N1 C5 117.66(15) . . ? C1 N1 Ni1 130.54(12) . . ? C5 N1 Ni1 111.50(11) . . ? C6 N2 C7 120.95(14) . . ? C6 N2 Ni1 115.39(12) . . ? C7 N2 Ni1 123.03(11) . . ? C10 N3 C9 120.47(13) . . ? C10 N3 Ni1 73.96(9) . . ? C9 N3 Ni1 117.14(10) . . ? C10 N3 Ni2 109.18(10) . . ? C9 N3 Ni2 127.06(10) . . ? Ni1 N3 Ni2 92.22(5) . . ? C15 N4 C11 118.50(14) . . ? C15 N4 Ni2 127.96(12) . . ? C11 N4 Ni2 111.83(10) . . ? C16 N5 C20 118.28(14) . . ? C16 N5 Ni2 129.33(11) . . ? C20 N5 Ni2 111.55(10) . . ? C21 N6 C22 119.53(14) . . ? C21 N6 Ni2 113.48(11) . . ? C22 N6 Ni2 126.50(10) . . ? C25 N7 C24 117.71(13) . . ? C25 N7 Ni1 73.08(9) . . ? C24 N7 Ni1 124.60(10) . . ? C25 N7 Ni2 112.10(10) . . ? C24 N7 Ni2 122.53(10) . . ? Ni1 N7 Ni2 95.37(6) . . ? C30 N8 C26 118.23(14) . . ? C30 N8 Ni2 130.18(11) . . ? C26 N8 Ni2 110.89(11) . . ? N1 C1 C2 122.80(17) . . ? C3 C2 C1 119.26(18) . . ? C2 C3 C4 118.92(17) . . ? C3 C4 C5 118.89(17) . . ? N1 C5 C4 122.45(17) . . ? N1 C5 C6 114.03(14) . . ? C4 C5 C6 123.30(16) . . ? N2 C6 C5 116.52(15) . . ? N2 C7 C8 109.53(14) . . ? C31 C8 C32 107.83(14) . . ? C31 C8 C7 110.59(15) . . ? C32 C8 C7 106.78(14) . . ? C31 C8 C9 114.52(14) . . ? C32 C8 C9 105.19(13) . . ? C7 C8 C9 111.43(13) . . ? N3 C9 C8 122.60(13) . . ? N3 C10 C11 118.15(14) . . ? N3 C10 Ni1 66.77(9) . . ? C11 C10 Ni1 108.47(11) . . ? N4 C11 C12 121.54(15) . . ? N4 C11 C10 116.34(14) . . ? C12 C11 C10 122.10(15) . . ? C13 C12 C11 119.12(17) . . ? C14 C13 C12 119.07(17) . . ? C13 C14 C15 118.79(16) . . ? N4 C15 C14 122.91(16) . . ? N5 C16 C17 122.70(15) . . ? C18 C17 C16 118.81(16) . . ? C17 C18 C19 119.03(16) . . ? C20 C19 C18 119.09(16) . . ? N5 C20 C19 122.05(15) . . ? N5 C20 C21 115.31(14) . . ? C19 C20 C21 122.64(15) . . ? N6 C21 C20 118.63(14) . . ? N6 C22 C23 115.90(13) . . ? C33 C23 C22 110.20(15) . . ? C33 C23 C34 108.90(15) . . ? C22 C23 C34 106.52(14) . . ? C33 C23 C24 111.85(14) . . ? C22 C23 C24 112.51(14) . . ? C34 C23 C24 106.60(14) . . ? N7 C24 C23 111.53(13) . . ? N7 C25 C26 116.94(14) . . ? N7 C25 Ni1 67.26(9) . . ? C26 C25 Ni1 111.58(11) . . ? N8 C26 C27 121.30(16) . . ? N8 C26 C25 116.27(14) . . ? C27 C26 C25 122.33(15) . . ? C28 C27 C26 119.78(17) . . ? C29 C28 C27 118.90(17) . . ? C28 C29 C30 118.75(17) . . ? N8 C30 C29 123.02(16) . . ? O2 S1 O3 115.04(9) . . ? O2 S1 O1 114.58(9) . . ? O3 S1 O1 115.95(9) . . ? O2 S1 C1S 102.63(9) . . ? O3 S1 C1S 102.82(9) . . ? O1 S1 C1S 103.16(9) . . ? O6 S2 O5 114.90(12) . . ? O6 S2 O4 114.93(9) . . ? O5 S2 O4 115.61(10) . . ? O6 S2 C2S 103.19(10) . . ? O5 S2 C2S 102.34(10) . . ? O4 S2 C2S 103.25(9) . . ? F1 C1S F3 106.93(17) . . ? F1 C1S F2 107.36(16) . . ? F3 C1S F2 107.30(18) . . ? F1 C1S S1 112.24(16) . . ? F3 C1S S1 111.34(13) . . ? F2 C1S S1 111.41(14) . . ? F4 C2S F6 107.65(17) . . ? F4 C2S F5 106.54(18) . . ? F6 C2S F5 106.43(17) . . ? F4 C2S S2 112.23(15) . . ? F6 C2S S2 112.34(14) . . ? F5 C2S S2 111.29(14) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.406 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.057 _database_code_depnum_ccdc_archive 'CCDC 863632' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_vw10 #TrackingRef 'vw10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H36 K N4 Ni O2' _chemical_formula_sum 'C25 H36 K N4 Ni O2' _chemical_formula_weight 522.39 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' K K 0.2009 0.2494 '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 10.5982(8) _cell_length_b 12.3634(8) _cell_length_c 19.8165(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.155(3) _cell_angle_gamma 90.00 _cell_volume 2586.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8955 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 28.53 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6509 _exptl_absorpt_correction_T_max 0.9634 _exptl_absorpt_process_details SADABS _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 X8 APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25673 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6390 _reflns_number_gt 5049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+1.1380P] 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 6390 _refine_ls_number_parameters 366 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.079 _refine_ls_shift/su_mean 0.003 _iucr_refine_instructions_details ; TITL vw10 in P2(1)/n CELL 0.71073 10.5982 12.3634 19.8165 90.000 95.155 90.000 ZERR 4.00 0.0008 0.0008 0.0013 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N K NI O UNIT 100 144 16 4 4 8 TEMP -100 SIZE 0.04 0.30 0.50 SHEL 100 .75 SIMU c23 c23' DELU c23 c23' ACTA OMIT 0 1 1 L.S. 10 WPDB WGHT 0.046400 1.138000 FVAR 0.16618 0.59443 0.66724 0.73558 K1 4 0.673223 0.701745 0.223741 11.00000 0.04017 0.02879 = 0.04059 0.00057 0.00727 -0.00446 NI1 5 0.701970 0.443083 0.225606 11.00000 0.03116 0.02404 = 0.02303 0.00264 -0.00091 -0.00154 O1 6 0.540510 0.693482 0.331562 11.00000 0.08096 0.04331 = 0.04029 0.00337 0.01793 -0.01508 O2 6 0.437913 0.743006 0.167716 11.00000 0.05065 0.06611 = 0.04074 0.00405 0.00449 0.01631 N1 3 0.751345 0.440226 0.320137 11.00000 0.03144 0.02603 = 0.02411 0.00138 0.00137 -0.00048 N2 3 0.582184 0.339599 0.246153 11.00000 0.03318 0.02602 = 0.02941 0.00085 -0.00194 -0.00350 N3 3 0.616739 0.491931 0.144575 11.00000 0.03984 0.03016 = 0.03119 0.00546 -0.00509 -0.00066 N4 3 0.850460 0.491889 0.185755 11.00000 0.03707 0.02558 = 0.02937 0.00046 0.00375 -0.00026 C1 1 0.840100 0.498416 0.358219 11.00000 0.03740 0.02660 = 0.03035 0.00029 0.00002 -0.00296 AFIX 43 H1A 2 0.885566 0.551854 0.335905 11.00000 -1.20000 AFIX 0 C2 1 0.868569 0.485549 0.426249 11.00000 0.04807 0.03614 = 0.02932 -0.00133 -0.00453 -0.00475 AFIX 43 H2A 2 0.929582 0.530670 0.450384 11.00000 -1.20000 AFIX 0 C3 1 0.805183 0.403277 0.460408 11.00000 0.05241 0.04001 = 0.02358 0.00338 -0.00005 0.00070 AFIX 43 H3A 2 0.825791 0.390624 0.507392 11.00000 -1.20000 AFIX 0 C4 1 0.715249 0.343398 0.425057 11.00000 0.04210 0.03404 = 0.02740 0.00427 0.00685 0.00233 AFIX 43 H4A 2 0.673320 0.287703 0.447374 11.00000 -1.20000 AFIX 0 C5 1 0.682451 0.362710 0.354695 11.00000 0.03225 0.02570 = 0.02807 0.00212 0.00561 0.00195 C6 1 0.587004 0.314405 0.313518 11.00000 0.03256 0.02705 = 0.03220 0.00445 0.00580 -0.00135 AFIX 43 H6A 2 0.527935 0.266359 0.330921 11.00000 -1.20000 AFIX 0 C7 1 0.461152 0.316272 0.207511 11.00000 0.03463 0.03816 = 0.03650 0.00008 -0.00105 -0.00626 AFIX 23 H7A 2 0.393606 0.356781 0.227984 11.00000 -1.20000 H7B 2 0.442640 0.238219 0.211840 11.00000 -1.20000 AFIX 0 C8 1 0.455675 0.344673 0.132282 11.00000 0.03463 0.03327 = 0.03023 -0.00331 -0.00529 0.00093 C9 1 0.485964 0.464128 0.122618 11.00000 0.03884 0.03618 = 0.03503 0.00103 -0.00851 0.00296 AFIX 23 H9A 2 0.468623 0.482755 0.074083 11.00000 -1.20000 H9B 2 0.428965 0.508315 0.148412 11.00000 -1.20000 AFIX 0 C10 1 0.694268 0.522804 0.097534 11.00000 0.05427 0.03007 = 0.02376 0.00304 -0.00203 0.00010 AFIX 13 H10A 2 0.661102 0.539495 0.049832 11.00000 -1.20000 AFIX 0 C11 1 0.822570 0.529197 0.118797 11.00000 0.05072 0.02389 = 0.02807 0.00055 0.00774 0.00019 C12 1 0.922331 0.562360 0.079698 11.00000 0.06263 0.03040 = 0.03545 0.00137 0.01822 0.00057 AFIX 43 H12A 2 0.903194 0.586049 0.034327 11.00000 -1.20000 AFIX 0 C13 1 1.044452 0.560269 0.106937 11.00000 0.05878 0.03390 = 0.05705 -0.00150 0.03143 -0.00251 AFIX 43 H13A 2 1.111032 0.581827 0.080816 11.00000 -1.20000 AFIX 0 C14 1 1.071534 0.525311 0.175246 11.00000 0.04154 0.03537 = 0.05654 -0.00340 0.01448 0.00094 AFIX 43 H14A 2 1.156161 0.524724 0.195627 11.00000 -1.20000 AFIX 0 C15 1 0.974029 0.492717 0.210884 11.00000 0.03900 0.03069 = 0.03863 -0.00097 0.00656 0.00172 AFIX 43 H15A 2 0.993794 0.469060 0.256214 11.00000 -1.20000 AFIX 0 C16 1 0.319607 0.323501 0.101252 11.00000 0.04262 0.04373 = 0.04710 -0.00457 -0.01262 -0.00335 AFIX 137 H16A 2 0.295905 0.248657 0.110405 11.00000 -1.50000 H16B 2 0.314918 0.335314 0.052189 11.00000 -1.50000 H16C 2 0.261324 0.373044 0.121397 11.00000 -1.50000 AFIX 0 C17 1 0.546666 0.273404 0.096138 11.00000 0.05638 0.04097 = 0.03864 -0.00967 -0.00471 0.00819 AFIX 137 H17A 2 0.633087 0.283021 0.117341 11.00000 -1.50000 H17B 2 0.543420 0.294146 0.048282 11.00000 -1.50000 H17C 2 0.521742 0.197422 0.099651 11.00000 -1.50000 AFIX 0 PART 1 C18 1 0.550942 0.749132 0.394850 31.00000 0.04153 0.04397 = 0.05695 -0.00805 0.00414 0.00135 AFIX 23 H18A 2 0.475589 0.794590 0.400202 31.00000 -1.20000 H18B 2 0.628100 0.794567 0.400349 31.00000 -1.20000 AFIX 0 PART 2 C18' 1 0.597591 0.730492 0.398985 -31.00000 0.05813 0.05110 = 0.05143 -0.00225 0.00695 -0.00137 AFIX 23 H18C 2 0.682149 0.697736 0.410092 -31.00000 -1.20000 H18D 2 0.605629 0.810251 0.400515 -31.00000 -1.20000 AFIX 0 PART 1 C19 1 0.559108 0.653096 0.444573 21.00000 0.04548 0.08020 = 0.03706 0.00699 0.00401 0.01932 AFIX 23 H19A 2 0.645291 0.621505 0.448928 21.00000 -1.20000 H19B 2 0.536894 0.675774 0.489934 21.00000 -1.20000 AFIX 0 PART 2 C19' 1 0.505127 0.691620 0.446238 -21.00000 0.04019 0.06485 = 0.03762 -0.00004 0.00671 0.00571 AFIX 23 H19C 2 0.430770 0.740144 0.445925 -21.00000 -1.20000 H19D 2 0.545045 0.684604 0.493152 -21.00000 -1.20000 AFIX 0 PART 0 C20 1 0.467560 0.576784 0.414132 11.00000 0.07359 0.05278 = 0.05305 0.01277 0.02336 0.00411 C21 1 0.464731 0.598955 0.339519 11.00000 0.05427 0.03758 = 0.05087 0.00192 0.01335 -0.00118 C22 1 0.327202 0.777001 0.197573 11.00000 0.04175 0.05097 = 0.04354 0.00738 0.00556 0.00107 PART 1 C23 1 0.274090 0.870596 0.152866 41.00000 0.04932 0.05077 = 0.06172 0.01944 -0.00757 0.00846 AFIX 23 H23C 2 0.318135 0.939652 0.164430 41.00000 -1.20000 H23D 2 0.181743 0.879874 0.154970 41.00000 -1.20000 AFIX 0 PART 2 C23' 1 0.260517 0.846556 0.148753 -41.00000 0.07298 0.08169 = 0.10715 0.01734 0.04762 0.01376 AFIX 23 H23A 2 0.179103 0.812097 0.132468 -41.00000 -1.20000 H23B 2 0.241001 0.915420 0.171093 -41.00000 -1.20000 AFIX 0 PART 1 C24 1 0.307037 0.824879 0.081739 31.00000 0.09245 0.07132 = 0.04917 0.02185 -0.01608 -0.00131 AFIX 23 H24C 2 0.233975 0.784824 0.059340 31.00000 -1.20000 H24D 2 0.329017 0.884665 0.051691 31.00000 -1.20000 AFIX 0 PART 2 C24' 1 0.329800 0.869516 0.092051 -31.00000 0.05100 AFIX 23 H24A 2 0.384311 0.934277 0.099177 -31.00000 -1.20000 H24B 2 0.274395 0.876657 0.049326 -31.00000 -1.20000 AFIX 0 PART 0 C25 1 0.412960 0.754227 0.095876 11.00000 0.07619 0.07159 = 0.04039 0.00172 0.00741 -0.00146 H22 2 0.497651 0.538724 0.313105 11.00000 0.04513 H21 2 0.377038 0.618415 0.320183 11.00000 0.06338 H20B 2 0.380116 0.579129 0.429341 11.00000 0.08345 H20A 2 0.510021 0.508461 0.422989 11.00000 0.11837 H22B 2 0.267802 0.715916 0.199429 11.00000 0.06275 H22A 2 0.350807 0.798994 0.242601 11.00000 0.05438 H25B 2 0.489021 0.771742 0.075871 11.00000 0.06491 H25A 2 0.373366 0.687316 0.076788 11.00000 0.08228 HKLF 4 REM vw10 in P2(1)/n REM R1 = 0.0355 for 5049 Fo > 4sig(Fo) and 0.0511 for all 6390 data REM 366 parameters refined using 6 restraints END WGHT 0.0392 1.2596 REM Highest difference peak 1.227, deepest hole -0.548, 1-sigma level 0.057 Q1 1 0.7555 0.4186 0.2013 11.00000 0.05 1.23 Q2 1 0.6654 0.4551 0.1213 11.00000 0.05 0.43 Q3 1 0.7198 0.3966 0.3392 11.00000 0.05 0.33 Q4 1 0.4000 0.4626 0.1875 11.00000 0.05 0.33 Q5 1 0.6386 0.3132 0.2242 11.00000 0.05 0.32 Q6 1 0.5088 0.2856 0.1731 11.00000 0.05 0.31 Q7 1 0.8830 0.5237 0.0980 11.00000 0.05 0.30 Q8 1 0.4750 0.3970 0.1273 11.00000 0.05 0.30 Q9 1 0.7592 0.5021 0.0745 11.00000 0.05 0.29 Q10 1 0.5388 0.5766 0.4306 11.00000 0.05 0.28 Q11 1 0.3984 0.3369 0.1095 11.00000 0.05 0.26 Q12 1 0.6052 0.6704 0.3530 11.00000 0.05 0.26 Q13 1 0.7459 0.4242 0.2855 11.00000 0.05 0.25 Q14 1 0.7975 0.4146 0.3099 11.00000 0.05 0.25 Q15 1 0.7633 0.5011 0.0966 11.00000 0.05 0.25 Q16 1 0.8214 0.4534 0.4452 11.00000 0.05 0.25 Q17 1 0.9150 0.4837 0.1911 11.00000 0.05 0.24 Q18 1 0.6820 0.3716 0.3894 11.00000 0.05 0.24 Q19 1 0.7303 0.3995 0.4413 11.00000 0.05 0.24 Q20 1 0.8259 0.4901 0.3972 11.00000 0.05 0.24 ; 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 K1 K 0.67322(4) 0.70174(4) 0.22374(2) 0.03630(11) Uani 1 1 d . . . Ni1 Ni 0.70197(2) 0.443083(18) 0.225606(11) 0.02628(8) Uani 1 1 d . . . O1 O 0.54051(18) 0.69348(13) 0.33156(8) 0.0541(4) Uani 1 1 d . . . O2 O 0.43791(15) 0.74301(15) 0.16772(8) 0.0525(4) Uani 1 1 d . . . N1 N 0.75134(14) 0.44023(12) 0.32014(8) 0.0273(3) Uani 1 1 d . . . N2 N 0.58218(14) 0.33960(13) 0.24615(8) 0.0298(3) Uani 1 1 d . . . N3 N 0.61674(15) 0.49193(13) 0.14458(8) 0.0342(4) Uani 1 1 d . . . N4 N 0.85046(15) 0.49189(13) 0.18575(8) 0.0306(3) Uani 1 1 d . . . C1 C 0.84010(18) 0.49842(16) 0.35822(10) 0.0316(4) Uani 1 1 d . . . H1A H 0.8856 0.5519 0.3359 0.038 Uiso 1 1 calc R . . C2 C 0.8686(2) 0.48555(18) 0.42625(10) 0.0383(5) Uani 1 1 d . . . H2A H 0.9296 0.5307 0.4504 0.046 Uiso 1 1 calc R . . C3 C 0.8052(2) 0.40328(18) 0.46041(10) 0.0389(5) Uani 1 1 d . . . H3A H 0.8258 0.3906 0.5074 0.047 Uiso 1 1 calc R . . C4 C 0.71525(19) 0.34340(17) 0.42506(10) 0.0343(4) Uani 1 1 d . . . H4A H 0.6733 0.2877 0.4474 0.041 Uiso 1 1 calc R . . C5 C 0.68245(17) 0.36271(15) 0.35469(9) 0.0285(4) Uani 1 1 d . . . C6 C 0.58700(17) 0.31441(15) 0.31352(10) 0.0304(4) Uani 1 1 d . . . H6A H 0.5279 0.2664 0.3309 0.037 Uiso 1 1 calc R . . C7 C 0.46115(18) 0.31627(18) 0.20751(10) 0.0367(5) Uani 1 1 d . A . H7A H 0.3936 0.3568 0.2280 0.044 Uiso 1 1 calc R . . H7B H 0.4426 0.2382 0.2118 0.044 Uiso 1 1 calc R . . C8 C 0.45567(18) 0.34467(16) 0.13228(10) 0.0332(4) Uani 1 1 d . . . C9 C 0.48596(19) 0.46413(17) 0.12262(11) 0.0374(5) Uani 1 1 d . A . H9A H 0.4686 0.4828 0.0741 0.045 Uiso 1 1 calc R . . H9B H 0.4290 0.5083 0.1484 0.045 Uiso 1 1 calc R . . C10 C 0.6943(2) 0.52280(17) 0.09753(10) 0.0364(4) Uani 1 1 d . A . H10A H 0.6611 0.5395 0.0498 0.044 Uiso 1 1 calc R . . C11 C 0.8226(2) 0.52920(16) 0.11880(10) 0.0340(4) Uani 1 1 d . A . C12 C 0.9223(2) 0.56236(17) 0.07970(12) 0.0420(5) Uani 1 1 d . . . H12A H 0.9032 0.5860 0.0343 0.050 Uiso 1 1 calc R A . C13 C 1.0445(2) 0.56027(18) 0.10694(14) 0.0483(6) Uani 1 1 d . A . H13A H 1.1110 0.5818 0.0808 0.058 Uiso 1 1 calc R . . C14 C 1.0715(2) 0.52531(18) 0.17525(12) 0.0439(5) Uani 1 1 d . . . H14A H 1.1562 0.5247 0.1956 0.053 Uiso 1 1 calc R A . C15 C 0.97403(19) 0.49272(17) 0.21088(11) 0.0359(4) Uani 1 1 d . A . H15A H 0.9938 0.4691 0.2562 0.043 Uiso 1 1 calc R . . C16 C 0.3196(2) 0.32350(19) 0.10125(12) 0.0455(5) Uani 1 1 d . A . H16A H 0.2959 0.2487 0.1104 0.068 Uiso 1 1 calc R . . H16B H 0.3149 0.3353 0.0522 0.068 Uiso 1 1 calc R . . H16C H 0.2613 0.3730 0.1214 0.068 Uiso 1 1 calc R . . C17 C 0.5467(2) 0.27340(19) 0.09614(11) 0.0459(5) Uani 1 1 d . A . H17A H 0.6331 0.2830 0.1173 0.069 Uiso 1 1 calc R . . H17B H 0.5434 0.2941 0.0483 0.069 Uiso 1 1 calc R . . H17C H 0.5217 0.1974 0.0997 0.069 Uiso 1 1 calc R . . C18 C 0.5509(7) 0.7491(7) 0.3949(4) 0.0475(14) Uani 0.667(16) 1 d P A 1 H18A H 0.4756 0.7946 0.4002 0.057 Uiso 0.667(16) 1 calc PR A 1 H18B H 0.6281 0.7946 0.4003 0.057 Uiso 0.667(16) 1 calc PR A 1 C18' C 0.5976(17) 0.7305(14) 0.3990(8) 0.053(3) Uani 0.333(16) 1 d P A 2 H18C H 0.6821 0.6977 0.4101 0.064 Uiso 0.333(16) 1 calc PR A 2 H18D H 0.6056 0.8103 0.4005 0.064 Uiso 0.333(16) 1 calc PR A 2 C19 C 0.5591(7) 0.6531(6) 0.4446(2) 0.0542(17) Uani 0.594(16) 1 d P A 1 H19A H 0.6453 0.6215 0.4489 0.065 Uiso 0.594(16) 1 calc PR A 1 H19B H 0.5369 0.6758 0.4899 0.065 Uiso 0.594(16) 1 calc PR A 1 C19' C 0.5051(10) 0.6916(8) 0.4462(3) 0.047(2) Uani 0.406(16) 1 d P A 2 H19C H 0.4308 0.7401 0.4459 0.057 Uiso 0.406(16) 1 calc PR A 2 H19D H 0.5450 0.6846 0.4932 0.057 Uiso 0.406(16) 1 calc PR A 2 C20 C 0.4676(3) 0.5768(2) 0.41413(15) 0.0587(7) Uani 1 1 d . . . C21 C 0.4647(2) 0.5990(2) 0.33952(13) 0.0471(5) Uani 1 1 d . A . C22 C 0.3272(2) 0.7770(2) 0.19757(13) 0.0453(5) Uani 1 1 d . A . C23 C 0.2741(9) 0.8706(9) 0.1529(5) 0.0547(19) Uani 0.74(4) 1 d PU A 1 H23C H 0.3181 0.9397 0.1644 0.066 Uiso 0.74(4) 1 calc PR A 1 H23D H 0.1817 0.8799 0.1550 0.066 Uiso 0.74(4) 1 calc PR A 1 C23' C 0.261(3) 0.847(4) 0.1488(18) 0.085(9) Uani 0.26(4) 1 d PU A 2 H23A H 0.1791 0.8121 0.1325 0.102 Uiso 0.26(4) 1 calc PR A 2 H23B H 0.2410 0.9154 0.1711 0.102 Uiso 0.26(4) 1 calc PR A 2 C24 C 0.3070(6) 0.8249(8) 0.0817(3) 0.0723(18) Uani 0.667(16) 1 d P A 1 H24C H 0.2340 0.7848 0.0593 0.087 Uiso 0.667(16) 1 calc PR A 1 H24D H 0.3290 0.8847 0.0517 0.087 Uiso 0.667(16) 1 calc PR A 1 C24' C 0.3298(10) 0.8695(11) 0.0921(6) 0.051(3) Uiso 0.333(16) 1 d P A 2 H24A H 0.3843 0.9343 0.0992 0.061 Uiso 0.333(16) 1 calc PR A 2 H24B H 0.2744 0.8767 0.0493 0.061 Uiso 0.333(16) 1 calc PR A 2 C25 C 0.4130(3) 0.7542(3) 0.09588(14) 0.0626(7) Uani 1 1 d . A . H22 H 0.498(2) 0.539(2) 0.3131(12) 0.045(6) Uiso 1 1 d . . . H21 H 0.377(3) 0.618(2) 0.3202(13) 0.063(8) Uiso 1 1 d . . . H20B H 0.380(3) 0.579(2) 0.4293(16) 0.083(10) Uiso 1 1 d . . . H20A H 0.510(4) 0.508(4) 0.4230(19) 0.118(14) Uiso 1 1 d . . . H22B H 0.268(3) 0.716(2) 0.1994(13) 0.063(8) Uiso 1 1 d . . . H22A H 0.351(2) 0.799(2) 0.2426(14) 0.054(7) Uiso 1 1 d . . . H25B H 0.489(3) 0.772(2) 0.0759(14) 0.065(8) Uiso 1 1 d . . . H25A H 0.373(3) 0.687(3) 0.0768(15) 0.082(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0402(2) 0.0288(2) 0.0406(3) 0.00057(18) 0.00727(18) -0.00446(17) Ni1 0.03116(13) 0.02404(13) 0.02303(13) 0.00264(9) -0.00091(9) -0.00154(9) O1 0.0810(12) 0.0433(10) 0.0403(9) 0.0034(7) 0.0179(8) -0.0151(8) O2 0.0506(9) 0.0661(12) 0.0407(9) 0.0040(8) 0.0045(7) 0.0163(8) N1 0.0314(7) 0.0260(8) 0.0241(8) 0.0014(6) 0.0014(6) -0.0005(6) N2 0.0332(8) 0.0260(8) 0.0294(8) 0.0008(7) -0.0019(6) -0.0035(6) N3 0.0398(9) 0.0302(9) 0.0312(9) 0.0055(7) -0.0051(7) -0.0007(7) N4 0.0371(8) 0.0256(8) 0.0294(8) 0.0005(7) 0.0037(6) -0.0003(6) C1 0.0374(9) 0.0266(10) 0.0304(10) 0.0003(8) 0.0000(8) -0.0030(8) C2 0.0481(11) 0.0361(11) 0.0293(10) -0.0013(9) -0.0045(8) -0.0047(9) C3 0.0524(12) 0.0400(12) 0.0236(10) 0.0034(9) -0.0001(8) 0.0007(9) C4 0.0421(10) 0.0340(11) 0.0274(10) 0.0043(8) 0.0069(8) 0.0023(8) C5 0.0322(9) 0.0257(9) 0.0281(9) 0.0021(8) 0.0056(7) 0.0019(7) C6 0.0326(9) 0.0271(10) 0.0322(10) 0.0045(8) 0.0058(7) -0.0014(7) C7 0.0346(10) 0.0382(12) 0.0365(11) 0.0001(9) -0.0011(8) -0.0063(8) C8 0.0346(9) 0.0333(11) 0.0302(10) -0.0033(8) -0.0053(7) 0.0009(8) C9 0.0388(10) 0.0362(11) 0.0350(11) 0.0010(9) -0.0085(8) 0.0030(8) C10 0.0543(12) 0.0301(10) 0.0238(10) 0.0030(8) -0.0020(8) 0.0001(9) C11 0.0507(11) 0.0239(10) 0.0281(10) 0.0005(8) 0.0077(8) 0.0002(8) C12 0.0626(14) 0.0304(11) 0.0355(11) 0.0014(9) 0.0182(10) 0.0006(9) C13 0.0588(14) 0.0339(12) 0.0570(15) -0.0015(11) 0.0314(12) -0.0025(10) C14 0.0415(11) 0.0354(12) 0.0565(15) -0.0034(11) 0.0145(10) 0.0009(9) C15 0.0390(10) 0.0307(11) 0.0386(11) -0.0010(9) 0.0066(8) 0.0017(8) C16 0.0426(11) 0.0437(13) 0.0471(13) -0.0046(10) -0.0126(9) -0.0034(10) C17 0.0564(13) 0.0410(13) 0.0386(12) -0.0097(10) -0.0047(10) 0.0082(10) C18 0.042(3) 0.044(3) 0.057(3) -0.008(2) 0.004(3) 0.001(2) C18' 0.058(8) 0.051(7) 0.051(6) -0.002(5) 0.007(7) -0.001(6) C19 0.045(3) 0.080(4) 0.037(2) 0.007(2) 0.004(2) 0.019(3) C19' 0.040(4) 0.065(5) 0.038(3) 0.000(3) 0.007(3) 0.006(3) C20 0.0736(18) 0.0528(17) 0.0530(16) 0.0128(13) 0.0234(14) 0.0041(14) C21 0.0543(14) 0.0376(13) 0.0509(14) 0.0019(11) 0.0133(11) -0.0012(11) C22 0.0418(12) 0.0510(15) 0.0435(14) 0.0074(12) 0.0056(10) 0.0011(10) C23 0.049(3) 0.051(3) 0.062(3) 0.019(2) -0.008(3) 0.008(2) C23' 0.073(12) 0.082(19) 0.107(17) 0.017(12) 0.048(13) 0.014(11) C24 0.092(4) 0.071(5) 0.049(3) 0.022(3) -0.016(3) -0.001(3) C25 0.0762(19) 0.072(2) 0.0404(14) 0.0017(14) 0.0074(13) -0.0015(16) _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 K1 O1 2.6634(17) . ? K1 O2 2.6860(16) . ? K1 C5 3.0238(19) 2_655 ? K1 C6 3.0463(19) 2_655 ? K1 N3 3.0626(17) . ? K1 N2 3.1149(16) 2_655 ? K1 N1 3.1958(16) 2_655 ? K1 Ni1 3.2123(5) . ? K1 N4 3.3288(16) . ? K1 C10 3.361(2) . ? K1 Ni1 3.3795(5) 2_655 ? K1 C11 3.460(2) . ? Ni1 N3 1.8704(15) . ? Ni1 N2 1.8728(15) . ? Ni1 N1 1.8995(15) . ? Ni1 N4 1.9203(16) . ? Ni1 K1 3.3795(5) 2_645 ? O1 C18 1.426(8) . ? O1 C21 1.435(3) . ? O1 C18' 1.488(17) . ? O2 C22 1.424(3) . ? O2 C25 1.431(3) . ? N1 C1 1.358(2) . ? N1 C5 1.418(2) . ? N1 K1 3.1958(16) 2_645 ? N2 C6 1.367(2) . ? N2 C7 1.462(2) . ? N2 K1 3.1148(16) 2_645 ? N3 C10 1.352(3) . ? N3 C9 1.456(2) . ? N4 C15 1.359(2) . ? N4 C11 1.411(2) . ? C1 C2 1.364(3) . ? C2 C3 1.423(3) . ? C3 C4 1.352(3) . ? C4 C5 1.427(3) . ? C5 C6 1.377(3) . ? C5 K1 3.0237(19) 2_645 ? C6 K1 3.0462(19) 2_645 ? C7 C8 1.528(3) . ? C8 C9 1.527(3) . ? C8 C17 1.531(3) . ? C8 C16 1.538(3) . ? C10 C11 1.389(3) . ? C11 C12 1.426(3) . ? C12 C13 1.357(4) . ? C13 C14 1.425(4) . ? C14 C15 1.364(3) . ? C18 C19 1.540(11) . ? C18' C19' 1.494(19) . ? C19 C20 1.446(6) . ? C19' C20 1.592(9) . ? C20 C21 1.501(4) . ? C22 C23 1.533(9) . ? C22 C23' 1.43(3) . ? C23 C24 1.586(14) . ? C23' C24' 1.42(3) . ? C24 C25 1.430(6) . ? C24' C25 1.674(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 K1 O2 78.54(5) . . ? O1 K1 C5 139.96(5) . 2_655 ? O2 K1 C5 98.99(5) . 2_655 ? O1 K1 C6 136.40(5) . 2_655 ? O2 K1 C6 125.22(5) . 2_655 ? C5 K1 C6 26.23(5) 2_655 2_655 ? O1 K1 N3 106.58(5) . . ? O2 K1 N3 79.49(5) . . ? C5 K1 N3 112.26(5) 2_655 . ? C6 K1 N3 113.08(5) 2_655 . ? O1 K1 N2 110.96(5) . 2_655 ? O2 K1 N2 134.51(5) . 2_655 ? C5 K1 N2 44.57(4) 2_655 2_655 ? C6 K1 N2 25.61(4) 2_655 2_655 ? N3 K1 N2 133.04(5) . 2_655 ? O1 K1 N1 114.62(5) . 2_655 ? O2 K1 N1 87.59(5) . 2_655 ? C5 K1 N1 26.17(4) 2_655 2_655 ? C6 K1 N1 43.76(5) 2_655 2_655 ? N3 K1 N1 133.17(4) . 2_655 ? N2 K1 N1 47.40(4) 2_655 2_655 ? O1 K1 Ni1 90.51(4) . . ? O2 K1 Ni1 106.11(4) . . ? C5 K1 Ni1 127.54(4) 2_655 . ? C6 K1 Ni1 112.19(4) 2_655 . ? N3 K1 Ni1 34.58(3) . . ? N2 K1 Ni1 117.78(3) 2_655 . ? N1 K1 Ni1 153.61(3) 2_655 . ? O1 K1 N4 120.06(5) . . ? O2 K1 N4 125.20(5) . . ? C5 K1 N4 94.30(5) 2_655 . ? C6 K1 N4 78.56(5) 2_655 . ? N3 K1 N4 46.55(4) . . ? N2 K1 N4 89.60(4) 2_655 . ? N1 K1 N4 119.84(4) 2_655 . ? Ni1 K1 N4 34.09(3) . . ? O1 K1 C10 130.30(5) . . ? O2 K1 C10 86.48(5) . . ? C5 K1 C10 88.87(5) 2_655 . ? C6 K1 C10 90.46(5) 2_655 . ? N3 K1 C10 23.71(5) . . ? N2 K1 C10 113.13(5) 2_655 . ? N1 K1 C10 111.71(5) 2_655 . ? Ni1 K1 C10 48.76(4) . . ? N4 K1 C10 40.73(4) . . ? O1 K1 Ni1 90.94(4) . 2_655 ? O2 K1 Ni1 106.21(4) . 2_655 ? C5 K1 Ni1 50.88(4) 2_655 2_655 ? C6 K1 Ni1 49.88(4) 2_655 2_655 ? N3 K1 Ni1 162.40(4) . 2_655 ? N2 K1 Ni1 33.20(3) 2_655 2_655 ? N1 K1 Ni1 33.43(3) 2_655 2_655 ? Ni1 K1 Ni1 147.282(15) . 2_655 ? N4 K1 Ni1 122.79(3) . 2_655 ? C10 K1 Ni1 138.74(4) . 2_655 ? O1 K1 C11 139.60(5) . . ? O2 K1 C11 109.06(5) . . ? C5 K1 C11 79.45(5) 2_655 . ? C6 K1 C11 72.52(5) 2_655 . ? N3 K1 C11 41.31(5) . . ? N2 K1 C11 91.99(5) 2_655 . ? N1 K1 C11 105.44(4) 2_655 . ? Ni1 K1 C11 49.09(3) . . ? N4 K1 C11 23.89(4) . . ? C10 K1 C11 23.44(5) . . ? Ni1 K1 C11 122.33(4) 2_655 . ? N3 Ni1 N2 97.05(7) . . ? N3 Ni1 N1 157.17(7) . . ? N2 Ni1 N1 84.54(7) . . ? N3 Ni1 N4 84.03(7) . . ? N2 Ni1 N4 154.25(7) . . ? N1 Ni1 N4 104.36(7) . . ? N3 Ni1 K1 68.33(5) . . ? N2 Ni1 K1 128.11(5) . . ? N1 Ni1 K1 92.71(5) . . ? N4 Ni1 K1 76.28(5) . . ? N3 Ni1 K1 133.31(5) . 2_645 ? N2 Ni1 K1 65.61(5) . 2_645 ? N1 Ni1 K1 67.97(5) . 2_645 ? N4 Ni1 K1 94.95(5) . 2_645 ? K1 Ni1 K1 156.425(9) . 2_645 ? C18 O1 C21 107.2(4) . . ? C18 O1 C18' 21.4(5) . . ? C21 O1 C18' 109.8(7) . . ? C18 O1 K1 133.0(3) . . ? C21 O1 K1 117.42(14) . . ? C18' O1 K1 120.5(7) . . ? C22 O2 C25 107.41(19) . . ? C22 O2 K1 130.79(14) . . ? C25 O2 K1 120.75(16) . . ? C1 N1 C5 116.79(16) . . ? C1 N1 Ni1 130.83(13) . . ? C5 N1 Ni1 112.38(11) . . ? C1 N1 K1 117.53(11) . 2_645 ? C5 N1 K1 70.13(9) . 2_645 ? Ni1 N1 K1 78.60(5) . 2_645 ? C6 N2 C7 114.86(15) . . ? C6 N2 Ni1 113.66(12) . . ? C7 N2 Ni1 126.92(13) . . ? C6 N2 K1 74.39(10) . 2_645 ? C7 N2 K1 131.92(12) . 2_645 ? Ni1 N2 K1 81.18(5) . 2_645 ? C10 N3 C9 118.80(17) . . ? C10 N3 Ni1 113.99(13) . . ? C9 N3 Ni1 123.62(13) . . ? C10 N3 K1 90.64(12) . . ? C9 N3 K1 119.34(13) . . ? Ni1 N3 K1 77.09(5) . . ? C15 N4 C11 117.12(17) . . ? C15 N4 Ni1 130.56(14) . . ? C11 N4 Ni1 112.29(13) . . ? C15 N4 K1 117.14(12) . . ? C11 N4 K1 83.28(11) . . ? Ni1 N4 K1 69.63(5) . . ? N1 C1 C2 124.62(18) . . ? C1 C2 C3 118.78(18) . . ? C4 C3 C2 119.07(18) . . ? C3 C4 C5 120.89(19) . . ? C6 C5 N1 112.93(16) . . ? C6 C5 C4 127.44(18) . . ? N1 C5 C4 119.63(17) . . ? C6 C5 K1 77.80(11) . 2_645 ? N1 C5 K1 83.70(10) . 2_645 ? C4 C5 K1 107.59(12) . 2_645 ? N2 C6 C5 116.14(16) . . ? N2 C6 K1 80.00(10) . 2_645 ? C5 C6 K1 75.97(11) . 2_645 ? N2 C7 C8 114.86(16) . . ? C9 C8 C7 110.78(16) . . ? C9 C8 C17 110.46(18) . . ? C7 C8 C17 110.73(17) . . ? C9 C8 C16 108.33(16) . . ? C7 C8 C16 107.64(17) . . ? C17 C8 C16 108.80(17) . . ? N3 C9 C8 113.33(16) . . ? N3 C10 C11 116.48(17) . . ? N3 C10 K1 65.65(11) . . ? C11 C10 K1 82.27(12) . . ? C10 C11 N4 112.54(17) . . ? C10 C11 C12 127.22(19) . . ? N4 C11 C12 120.14(19) . . ? C10 C11 K1 74.29(12) . . ? N4 C11 K1 72.83(10) . . ? C12 C11 K1 123.42(13) . . ? C13 C12 C11 120.4(2) . . ? C12 C13 C14 119.1(2) . . ? C15 C14 C13 119.0(2) . . ? N4 C15 C14 124.2(2) . . ? O1 C18 C19 100.7(5) . . ? C19' C18' O1 103.1(11) . . ? C20 C19 C18 103.8(4) . . ? C18' C19' C20 101.0(8) . . ? C19 C20 C21 104.2(3) . . ? C19 C20 C19' 28.0(2) . . ? C21 C20 C19' 102.3(3) . . ? O1 C21 C20 107.2(2) . . ? O2 C22 C23 104.8(4) . . ? O2 C22 C23' 105.8(13) . . ? C23 C22 C23' 12(2) . . ? C22 C23 C24 98.4(7) . . ? C24' C23' C22 113(2) . . ? C25 C24 C23 106.0(4) . . ? C23' C24' C25 95.8(16) . . ? O2 C25 C24 109.0(3) . . ? O2 C25 C24' 100.2(4) . . ? C24 C25 C24' 21.6(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.227 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.057 _database_code_depnum_ccdc_archive 'CCDC 921476' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_vw11 #TrackingRef 'vw11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H26 N6 Ni, 2(F6 P), C2 H3 N' _chemical_formula_sum 'C23 H29 F12 N7 Ni P2' _chemical_formula_weight 752.18 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 Cc 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' _cell_length_a 9.2230(4) _cell_length_b 23.7522(8) _cell_length_c 15.2139(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.3500(10) _cell_angle_gamma 90.00 _cell_volume 3181.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9986 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 33.34 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.808 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6427 _exptl_absorpt_correction_T_max 0.7935 _exptl_absorpt_process_details SADABS _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 X8 APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15695 _diffrn_reflns_av_R_equivalents 0.0143 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 29.13 _reflns_number_total 7932 _reflns_number_gt 7539 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+0.4646P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.003(7) _refine_ls_number_reflns 7932 _refine_ls_number_parameters 448 _refine_ls_number_restraints 158 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 2.966 _refine_ls_shift/su_mean 0.188 _iucr_refine_instructions_details ; TITL vw11 in Cc CELL 0.71073 9.2230 23.7522 15.2139 90.000 107.350 90.000 ZERR 4.00 0.0004 0.0008 0.0006 0.000 0.001 0.000 LATT -7 SYMM X, -Y, 0.5+Z SFAC C H N F P NI UNIT 92 116 28 48 8 4 TEMP -100 SIZE 0.30 0.40 0.60 SADI p1 f1 p1 f2 p1 f3 p1 f4 p1 f5 p1 f6 p2 f7 p2 f8 p2 f9 p2 f10 p2 f11 = P2 F12 P2 F9' P2 F10' P2 F11' P2 F12' SIMU f7 > f12' SHEL 100 .73 L.S. 8 ACTA WPDB WGHT 0.043100 0.464600 FVAR 0.17327 0.43368 NI1 6 0.101994 0.861341 0.919825 11.00000 0.02846 0.02140 = 0.02995 0.00023 0.00565 -0.00045 P1 5 -0.571991 1.037875 1.161756 11.00000 0.03901 0.04220 = 0.03655 -0.00253 0.01375 -0.00589 P2 5 0.094328 0.803469 1.281030 11.00000 0.04312 0.03839 = 0.04511 0.00334 0.00759 0.00356 N1 3 -0.030655 0.907056 0.986762 11.00000 0.04617 0.02572 = 0.04002 0.00136 0.01864 -0.00054 N2 3 -0.103081 0.861307 0.820120 11.00000 0.02782 0.02647 = 0.03730 0.00100 0.00893 -0.00203 N3 3 0.203416 0.824007 0.832449 11.00000 0.02928 0.03017 = 0.03279 0.00102 0.00363 0.00570 N4 3 0.323610 0.851825 1.009064 11.00000 0.04016 0.02532 = 0.03417 0.00317 -0.00230 -0.00414 N5 3 0.177150 0.942086 0.889371 11.00000 0.03618 0.02803 = 0.03251 0.00045 0.00671 -0.00146 N6 3 0.040806 0.784780 0.965839 11.00000 0.04419 0.02814 = 0.03589 0.00267 0.00864 -0.00239 C1 1 0.008552 0.932045 1.068663 11.00000 0.06703 0.03365 = 0.04255 -0.00182 0.02020 0.00367 AFIX 43 H1A 2 0.109627 0.927888 1.107826 11.00000 -1.20000 AFIX 0 C2 1 -0.093929 0.964225 1.099087 11.00000 0.10617 0.03571 = 0.05495 -0.00260 0.04530 0.00614 AFIX 43 H2A 2 -0.063238 0.980967 1.158492 11.00000 -1.20000 AFIX 0 C3 1 -0.239127 0.971390 1.042380 11.00000 0.08770 0.04017 = 0.07537 0.00399 0.05763 0.01343 AFIX 43 H3A 2 -0.309635 0.993740 1.061524 11.00000 -1.20000 AFIX 0 C4 1 -0.281802 0.945656 0.956848 11.00000 0.05728 0.04093 = 0.07221 0.00534 0.03728 0.01054 AFIX 43 H4A 2 -0.382287 0.949532 0.916735 11.00000 -1.20000 AFIX 0 C5 1 -0.174534 0.914027 0.930893 11.00000 0.03957 0.03020 = 0.05070 0.00412 0.02381 0.00162 C6 1 -0.209314 0.885544 0.841479 11.00000 0.02896 0.03536 = 0.04851 0.00353 0.01100 0.00076 AFIX 43 H6A 2 -0.309798 0.885376 0.800547 11.00000 -1.20000 AFIX 0 C7 1 -0.136932 0.828139 0.735211 11.00000 0.03210 0.03462 = 0.03864 -0.00508 0.00434 -0.00641 AFIX 23 H7A 2 -0.235848 0.840570 0.693212 11.00000 -1.20000 H7B 2 -0.147164 0.788082 0.750344 11.00000 -1.20000 AFIX 0 C8 1 -0.016418 0.832939 0.684870 11.00000 0.03534 0.03046 = 0.03260 -0.00061 0.00371 0.00261 C9 1 0.132800 0.803660 0.738164 11.00000 0.04763 0.05495 = 0.03492 -0.01055 0.00146 0.02013 AFIX 23 H9A 2 0.112716 0.762851 0.740882 11.00000 -1.20000 H9B 2 0.206603 0.808334 0.702953 11.00000 -1.20000 AFIX 0 C10 1 0.346675 0.818609 0.866297 11.00000 0.03243 0.04218 = 0.04667 0.00705 0.01075 0.00763 AFIX 43 H10A 2 0.406231 0.805784 0.828994 11.00000 -1.20000 AFIX 0 C11 1 0.418450 0.832374 0.963234 11.00000 0.03101 0.03082 = 0.04565 0.00967 0.00099 -0.00359 C12 1 0.572169 0.823708 1.005016 11.00000 0.03103 0.04655 = 0.07346 0.02007 -0.00049 -0.00292 AFIX 43 H12A 2 0.635386 0.810106 0.970510 11.00000 -1.20000 AFIX 0 C13 1 0.632023 0.835288 1.098280 11.00000 0.04571 0.04727 = 0.07630 0.01686 -0.02134 -0.01068 AFIX 43 H13A 2 0.737055 0.829852 1.128818 11.00000 -1.20000 AFIX 0 C14 1 0.537010 0.854642 1.145280 11.00000 0.07988 0.04107 = 0.05002 0.00423 -0.02888 -0.01100 AFIX 43 H14A 2 0.575781 0.863043 1.209067 11.00000 -1.20000 AFIX 0 C15 1 0.381500 0.862127 1.099053 11.00000 0.06289 0.03287 = 0.03971 -0.00192 -0.00668 -0.00221 AFIX 43 H15A 2 0.316059 0.874833 1.132739 11.00000 -1.20000 AFIX 0 C16 1 0.009277 0.894082 0.665375 11.00000 0.05298 0.04082 = 0.03840 0.00252 0.00727 -0.01235 AFIX 137 H16A 2 -0.086551 0.910723 0.628061 11.00000 -1.50000 H16B 2 0.084755 0.896425 0.631813 11.00000 -1.50000 H16C 2 0.046250 0.914650 0.723638 11.00000 -1.50000 AFIX 0 C17 1 -0.079104 0.800951 0.593273 11.00000 0.05483 0.04494 = 0.03759 -0.00761 0.00020 0.00571 AFIX 137 H17A 2 -0.173631 0.818741 0.556535 11.00000 -1.50000 H17B 2 -0.099238 0.761733 0.605906 11.00000 -1.50000 H17C 2 -0.004323 0.802028 0.559105 11.00000 -1.50000 AFIX 0 C18 1 0.235041 0.983780 0.884732 11.00000 0.03837 0.02728 = 0.02875 -0.00205 0.00855 0.00009 C19 1 0.308508 1.037620 0.878217 11.00000 0.06590 0.02926 = 0.03932 -0.00228 0.01853 -0.01472 AFIX 137 H19A 2 0.242849 1.059826 0.827568 11.00000 -1.50000 H19B 2 0.405935 1.030697 0.866601 11.00000 -1.50000 H19C 2 0.325908 1.058367 0.936123 11.00000 -1.50000 AFIX 0 C20 1 0.003104 0.744224 0.991884 11.00000 0.03694 0.02785 = 0.02971 0.00257 0.00107 -0.00186 C21 1 -0.043672 0.692358 1.026282 11.00000 0.05042 0.03434 = 0.04640 0.00886 0.00440 -0.01053 AFIX 137 H21A 2 0.009423 0.660442 1.008999 11.00000 -1.50000 H21B 2 -0.153546 0.687409 0.999528 11.00000 -1.50000 H21C 2 -0.018433 0.694250 1.093512 11.00000 -1.50000 AFIX 0 F1 4 -0.574170 1.083576 1.237569 11.00000 0.05329 0.10687 = 0.07159 -0.04849 0.02474 -0.00735 F2 4 -0.569513 0.991765 1.086025 11.00000 0.07781 0.04714 = 0.05744 -0.01625 0.01402 -0.00007 F3 4 -0.433169 1.069353 1.140788 11.00000 0.06904 0.05885 = 0.09987 -0.01605 0.05459 -0.01802 F4 4 -0.686572 1.075497 1.084620 11.00000 0.07814 0.06990 = 0.05509 0.01635 0.02708 0.02493 F5 4 -0.713334 1.007975 1.181594 11.00000 0.05301 0.08870 = 0.06896 0.01336 0.01898 -0.02416 F6 4 -0.455869 1.001813 1.238113 11.00000 0.06910 0.09928 = 0.05489 0.01743 0.00013 0.02193 F7 4 0.047434 0.864789 1.242628 11.00000 0.13738 0.06455 = 0.10807 0.04100 0.05613 0.04016 F8 4 0.144528 0.742970 1.323141 11.00000 0.07415 0.05451 = 0.16776 0.04457 0.05713 0.01996 PART 1 F9 4 0.019611 0.773137 1.194328 21.00000 0.17739 0.41993 = 0.18458 -0.24720 0.02709 -0.00924 F10 4 0.245669 0.810470 1.264159 21.00000 0.13761 0.09615 = 0.30998 0.08717 0.18255 0.04558 F11 4 0.140341 0.832916 1.376351 21.00000 0.16214 0.16699 = 0.11394 -0.05769 -0.09597 0.01941 F12 4 -0.070467 0.797660 1.294586 21.00000 0.06366 0.05132 = 0.23644 -0.00644 0.06755 0.01237 PART 2 F9' 4 0.116935 0.786593 1.184734 -21.00000 0.15745 0.08770 = 0.04007 -0.01382 0.03309 0.00847 F10' 4 0.271095 0.818524 1.308833 -21.00000 0.05092 0.09814 = 0.07696 0.00414 0.00640 -0.02484 F11' 4 0.096394 0.822603 1.379994 -21.00000 0.15213 0.15760 = 0.04614 0.02183 0.05640 0.08609 F12' 4 -0.072581 0.787201 1.254283 -21.00000 0.03025 0.15932 = 0.21415 0.11508 -0.04927 -0.02795 PART 0 N1S 3 -0.342838 0.892100 1.412294 11.00000 0.07452 0.09091 = 0.09056 0.02737 0.01643 0.00070 C1S 1 -0.243395 0.911117 1.395809 11.00000 0.06504 0.05897 = 0.06304 0.00296 0.01976 0.00719 C2S 1 -0.116682 0.936784 1.376986 11.00000 0.11336 0.07112 = 0.17037 -0.02130 0.09840 0.00238 AFIX 137 H2S1 2 -0.148916 0.971916 1.342999 11.00000 -1.50000 H2S2 2 -0.075464 0.911183 1.339907 11.00000 -1.50000 H2S3 2 -0.038273 0.944955 1.435071 11.00000 -1.50000 HKLF 4 REM vw11 in Cc REM R1 = 0.0282 for 7539 Fo > 4sig(Fo) and 0.0303 for all 7932 data REM 448 parameters refined using 158 restraints END WGHT 0.0375 0.6991 REM Highest difference peak 0.421, deepest hole -0.295, 1-sigma level 0.043 Q1 1 0.0749 0.7392 1.2623 11.00000 0.05 0.42 Q2 1 -0.6544 0.9784 1.1925 11.00000 0.05 0.35 Q3 1 -0.0050 0.8064 1.3469 11.00000 0.05 0.33 Q4 1 -0.3772 1.0424 1.1855 11.00000 0.05 0.29 Q5 1 -0.7276 1.0430 1.0974 11.00000 0.05 0.27 Q6 1 0.1248 0.7959 1.3779 11.00000 0.05 0.27 Q7 1 0.0529 0.8002 1.2293 11.00000 0.05 0.26 Q8 1 0.1097 0.8610 1.2934 11.00000 0.05 0.26 Q9 1 0.0542 0.8116 1.1698 11.00000 0.05 0.25 Q10 1 -0.0362 0.7606 1.2181 11.00000 0.05 0.24 Q11 1 0.3777 0.8247 0.9192 11.00000 0.05 0.22 Q12 1 0.1155 0.7568 1.3674 11.00000 0.05 0.22 Q13 1 0.1118 0.8615 0.8683 11.00000 0.05 0.22 Q14 1 0.1209 0.8635 0.9707 11.00000 0.05 0.22 Q15 1 0.0757 0.7705 1.2011 11.00000 0.05 0.21 Q16 1 0.6285 0.7619 1.0786 11.00000 0.05 0.21 Q17 1 -0.5953 1.0810 1.1200 11.00000 0.05 0.20 Q18 1 0.1958 0.8122 1.2824 11.00000 0.05 0.20 Q19 1 -0.0773 0.7697 1.2035 11.00000 0.05 0.20 Q20 1 -0.4276 1.0831 1.1437 11.00000 0.05 0.20 ; 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 0.10199(2) 0.861341(8) 0.919825(17) 0.02727(6) Uani 1 1 d . . . P1 P -0.57199(7) 1.03787(3) 1.16176(4) 0.03871(12) Uani 1 1 d D . . P2 P 0.09433(7) 0.80347(3) 1.28103(4) 0.04342(14) Uani 1 1 d D . . N1 N -0.0307(2) 0.90706(7) 0.98676(12) 0.0360(4) Uani 1 1 d . . . N2 N -0.1031(2) 0.86131(6) 0.82012(14) 0.0307(4) Uani 1 1 d . . . N3 N 0.2034(2) 0.82401(7) 0.83245(11) 0.0320(3) Uani 1 1 d . . . N4 N 0.3236(2) 0.85182(8) 1.00906(13) 0.0361(4) Uani 1 1 d . . . N5 N 0.1772(2) 0.94209(7) 0.88937(12) 0.0330(3) Uani 1 1 d . . . N6 N 0.0408(2) 0.78478(7) 0.96584(12) 0.0368(4) Uani 1 1 d . . . C1 C 0.0086(4) 0.93204(9) 1.06866(17) 0.0469(5) Uani 1 1 d . . . H1A H 0.1096 0.9279 1.1078 0.056 Uiso 1 1 calc R . . C2 C -0.0939(5) 0.96422(10) 1.0991(2) 0.0610(8) Uani 1 1 d . . . H2A H -0.0632 0.9810 1.1585 0.073 Uiso 1 1 calc R . . C3 C -0.2391(4) 0.97139(11) 1.0424(2) 0.0605(8) Uani 1 1 d . . . H3A H -0.3096 0.9937 1.0615 0.073 Uiso 1 1 calc R . . C4 C -0.2818(4) 0.94566(11) 0.9568(2) 0.0529(6) Uani 1 1 d . . . H4A H -0.3823 0.9495 0.9167 0.063 Uiso 1 1 calc R . . C5 C -0.1745(3) 0.91403(9) 0.93089(16) 0.0379(4) Uani 1 1 d . . . C6 C -0.2093(3) 0.88554(9) 0.84148(16) 0.0377(4) Uani 1 1 d . . . H6A H -0.3098 0.8854 0.8005 0.045 Uiso 1 1 calc R . . C7 C -0.1369(3) 0.82814(9) 0.73521(15) 0.0365(4) Uani 1 1 d . . . H7A H -0.2358 0.8406 0.6932 0.044 Uiso 1 1 calc R . . H7B H -0.1472 0.7881 0.7503 0.044 Uiso 1 1 calc R . . C8 C -0.0164(2) 0.83294(8) 0.68487(14) 0.0342(4) Uani 1 1 d . . . C9 C 0.1328(3) 0.80366(11) 0.73816(16) 0.0482(6) Uani 1 1 d . . . H9A H 0.1127 0.7629 0.7409 0.058 Uiso 1 1 calc R . . H9B H 0.2066 0.8083 0.7030 0.058 Uiso 1 1 calc R . . C10 C 0.3467(3) 0.81861(9) 0.86630(17) 0.0407(5) Uani 1 1 d . . . H10A H 0.4062 0.8058 0.8290 0.049 Uiso 1 1 calc R . . C11 C 0.4185(3) 0.83237(9) 0.96323(16) 0.0381(4) Uani 1 1 d . . . C12 C 0.5722(3) 0.82371(11) 1.0050(2) 0.0539(7) Uani 1 1 d . . . H12A H 0.6354 0.8101 0.9705 0.065 Uiso 1 1 calc R . . C13 C 0.6320(4) 0.83529(12) 1.0983(3) 0.0650(9) Uani 1 1 d . . . H13A H 0.7371 0.8299 1.1288 0.078 Uiso 1 1 calc R . . C14 C 0.5370(5) 0.85464(11) 1.1453(2) 0.0675(10) Uani 1 1 d . . . H14A H 0.5758 0.8630 1.2091 0.081 Uiso 1 1 calc R . . C15 C 0.3815(4) 0.86213(9) 1.09905(18) 0.0500(6) Uani 1 1 d . . . H15A H 0.3161 0.8748 1.1327 0.060 Uiso 1 1 calc R . . C16 C 0.0093(3) 0.89408(10) 0.66537(16) 0.0455(5) Uani 1 1 d . . . H16A H -0.0866 0.9107 0.6281 0.068 Uiso 1 1 calc R . . H16B H 0.0848 0.8964 0.6318 0.068 Uiso 1 1 calc R . . H16C H 0.0462 0.9147 0.7236 0.068 Uiso 1 1 calc R . . C17 C -0.0791(3) 0.80095(11) 0.59327(17) 0.0488(6) Uani 1 1 d . . . H17A H -0.1736 0.8187 0.5565 0.073 Uiso 1 1 calc R . . H17B H -0.0992 0.7617 0.6059 0.073 Uiso 1 1 calc R . . H17C H -0.0043 0.8020 0.5591 0.073 Uiso 1 1 calc R . . C18 C 0.2350(2) 0.98378(8) 0.88473(13) 0.0318(4) Uani 1 1 d . . . C19 C 0.3085(3) 1.03762(9) 0.87822(16) 0.0442(5) Uani 1 1 d . . . H19A H 0.2428 1.0598 0.8276 0.066 Uiso 1 1 calc R . . H19B H 0.4059 1.0307 0.8666 0.066 Uiso 1 1 calc R . . H19C H 0.3259 1.0584 0.9361 0.066 Uiso 1 1 calc R . . C20 C 0.0031(2) 0.74422(8) 0.99188(13) 0.0334(4) Uani 1 1 d . . . C21 C -0.0437(3) 0.69236(9) 1.02628(17) 0.0459(5) Uani 1 1 d . . . H21A H 0.0094 0.6604 1.0090 0.069 Uiso 1 1 calc R . . H21B H -0.1535 0.6874 0.9995 0.069 Uiso 1 1 calc R . . H21C H -0.0184 0.6943 1.0935 0.069 Uiso 1 1 calc R . . F1 F -0.5742(2) 1.08358(10) 1.23757(14) 0.0759(6) Uani 1 1 d D . . F2 F -0.5695(2) 0.99177(7) 1.08602(12) 0.0621(4) Uani 1 1 d D . . F3 F -0.4332(2) 1.06935(8) 1.14079(15) 0.0695(5) Uani 1 1 d D . . F4 F -0.6866(2) 1.07550(8) 1.08462(12) 0.0661(5) Uani 1 1 d D . . F5 F -0.7133(2) 1.00797(9) 1.18159(13) 0.0701(5) Uani 1 1 d D . . F6 F -0.4559(3) 1.00181(10) 1.23811(14) 0.0784(6) Uani 1 1 d D . . F7 F 0.0474(4) 0.86479(9) 1.2426(2) 0.0991(9) Uani 1 1 d D A . F8 F 0.1445(3) 0.74297(9) 1.3231(2) 0.0942(8) Uani 1 1 d D A . F9 F 0.0196(19) 0.7731(9) 1.1943(9) 0.267(10) Uani 0.434(11) 1 d PDU A 1 F10 F 0.2457(14) 0.8105(5) 1.2642(15) 0.156(7) Uani 0.434(11) 1 d PDU A 1 F11 F 0.1403(16) 0.8329(6) 1.3764(7) 0.178(7) Uani 0.434(11) 1 d PDU A 1 F12 F -0.0705(9) 0.7977(3) 1.2946(10) 0.112(4) Uani 0.434(11) 1 d PDU A 1 F9' F 0.1169(10) 0.7866(2) 1.1847(3) 0.094(2) Uani 0.566(11) 1 d PDU A 2 F10' F 0.2711(7) 0.8185(4) 1.3088(4) 0.0781(19) Uani 0.566(11) 1 d PDU A 2 F11' F 0.0964(10) 0.8226(4) 1.3800(3) 0.113(3) Uani 0.566(11) 1 d PDU A 2 F12' F -0.0726(6) 0.7872(5) 1.2543(9) 0.153(5) Uani 0.566(11) 1 d PDU A 2 N1S N -0.3428(4) 0.89210(16) 1.4123(3) 0.0871(10) Uani 1 1 d . . . C1S C -0.2434(4) 0.91112(14) 1.3958(2) 0.0622(7) Uani 1 1 d . . . C2S C -0.1167(6) 0.93678(18) 1.3770(5) 0.1060(18) Uani 1 1 d . . . H2S1 H -0.1489 0.9719 1.3430 0.159 Uiso 1 1 calc R . . H2S2 H -0.0755 0.9112 1.3399 0.159 Uiso 1 1 calc R . . H2S3 H -0.0383 0.9450 1.4351 0.159 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02846(11) 0.02140(9) 0.02995(10) 0.00023(8) 0.00565(8) -0.00045(9) P1 0.0390(3) 0.0422(3) 0.0365(2) -0.0025(2) 0.0138(2) -0.0059(2) P2 0.0431(3) 0.0384(3) 0.0451(3) 0.0033(2) 0.0076(3) 0.0036(2) N1 0.0462(11) 0.0257(7) 0.0400(9) 0.0014(6) 0.0186(8) -0.0005(7) N2 0.0278(9) 0.0265(8) 0.0373(9) 0.0010(6) 0.0089(7) -0.0020(6) N3 0.0293(8) 0.0302(7) 0.0328(8) 0.0010(6) 0.0036(7) 0.0057(6) N4 0.0402(11) 0.0253(7) 0.0342(9) 0.0032(6) -0.0023(8) -0.0041(7) N5 0.0362(9) 0.0280(7) 0.0325(8) 0.0004(6) 0.0067(7) -0.0015(6) N6 0.0442(10) 0.0281(7) 0.0359(8) 0.0027(6) 0.0086(7) -0.0024(7) C1 0.0670(17) 0.0336(10) 0.0425(11) -0.0018(8) 0.0202(11) 0.0037(10) C2 0.106(3) 0.0357(11) 0.0550(14) -0.0026(10) 0.0453(17) 0.0061(13) C3 0.088(2) 0.0402(11) 0.0754(18) 0.0040(11) 0.0576(19) 0.0134(13) C4 0.0573(16) 0.0409(12) 0.0722(16) 0.0053(11) 0.0373(14) 0.0105(11) C5 0.0396(12) 0.0302(9) 0.0507(12) 0.0041(8) 0.0238(10) 0.0016(8) C6 0.0290(10) 0.0354(10) 0.0485(11) 0.0035(8) 0.0110(8) 0.0008(8) C7 0.0321(10) 0.0346(9) 0.0386(10) -0.0051(8) 0.0043(8) -0.0064(8) C8 0.0353(10) 0.0305(8) 0.0326(9) -0.0006(7) 0.0037(8) 0.0026(7) C9 0.0476(14) 0.0550(13) 0.0349(10) -0.0105(9) 0.0015(10) 0.0201(11) C10 0.0324(11) 0.0422(11) 0.0467(12) 0.0071(9) 0.0107(9) 0.0076(8) C11 0.0310(10) 0.0308(9) 0.0457(11) 0.0097(8) 0.0010(8) -0.0036(7) C12 0.0310(12) 0.0466(12) 0.0735(17) 0.0201(12) -0.0005(12) -0.0029(9) C13 0.0457(16) 0.0473(14) 0.0763(19) 0.0169(13) -0.0213(14) -0.0107(12) C14 0.080(2) 0.0411(12) 0.0500(15) 0.0042(10) -0.0289(16) -0.0110(13) C15 0.0629(17) 0.0329(11) 0.0397(11) -0.0019(8) -0.0067(11) -0.0022(9) C16 0.0530(14) 0.0408(11) 0.0384(10) 0.0025(8) 0.0073(10) -0.0124(10) C17 0.0548(16) 0.0449(12) 0.0376(11) -0.0076(9) 0.0002(10) 0.0057(11) C18 0.0384(11) 0.0273(8) 0.0288(8) -0.0020(6) 0.0085(7) 0.0001(7) C19 0.0659(16) 0.0293(9) 0.0393(10) -0.0023(7) 0.0185(10) -0.0147(9) C20 0.0369(10) 0.0279(8) 0.0297(8) 0.0026(6) 0.0011(7) -0.0019(7) C21 0.0504(14) 0.0343(10) 0.0464(12) 0.0089(8) 0.0044(10) -0.0105(9) F1 0.0533(10) 0.1069(16) 0.0716(11) -0.0485(11) 0.0247(9) -0.0073(10) F2 0.0778(13) 0.0471(8) 0.0574(9) -0.0163(7) 0.0140(9) -0.0001(8) F3 0.0690(12) 0.0589(10) 0.0999(14) -0.0160(9) 0.0546(11) -0.0180(9) F4 0.0781(13) 0.0699(11) 0.0551(9) 0.0163(8) 0.0271(9) 0.0249(9) F5 0.0530(10) 0.0887(13) 0.0690(11) 0.0134(10) 0.0190(8) -0.0242(9) F6 0.0691(13) 0.0993(15) 0.0549(9) 0.0174(10) 0.0001(9) 0.0219(11) F7 0.137(2) 0.0646(13) 0.1081(18) 0.0410(12) 0.0561(18) 0.0402(13) F8 0.0742(14) 0.0545(10) 0.168(2) 0.0446(13) 0.0571(16) 0.0200(10) F9 0.177(13) 0.42(2) 0.185(11) -0.247(14) 0.027(9) -0.009(12) F10 0.138(9) 0.096(7) 0.310(19) 0.087(10) 0.183(11) 0.046(6) F11 0.162(9) 0.167(9) 0.114(8) -0.058(7) -0.096(7) 0.019(8) F12 0.064(5) 0.051(3) 0.236(13) -0.006(5) 0.068(7) 0.012(3) F9' 0.157(6) 0.088(3) 0.0401(18) -0.0138(19) 0.033(3) 0.008(3) F10' 0.051(2) 0.098(4) 0.077(3) 0.004(2) 0.006(2) -0.025(2) F11' 0.152(7) 0.158(6) 0.046(3) 0.022(3) 0.056(4) 0.086(5) F12' 0.030(3) 0.159(8) 0.214(10) 0.115(7) -0.049(4) -0.028(3) N1S 0.075(2) 0.091(2) 0.091(2) 0.0274(19) 0.0164(18) 0.0007(18) C1S 0.065(2) 0.0590(16) 0.0630(17) 0.0030(13) 0.0198(15) 0.0072(14) C2S 0.113(4) 0.071(2) 0.170(5) -0.021(3) 0.098(4) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 2.041(2) . ? Ni1 N3 2.0421(17) . ? Ni1 N6 2.0859(17) . ? Ni1 N4 2.102(2) . ? Ni1 N1 2.1109(18) . ? Ni1 N5 2.1366(17) . ? P1 F6 1.577(2) . ? P1 F1 1.5884(17) . ? P1 F5 1.5904(18) . ? P1 F3 1.5949(18) . ? P1 F2 1.5947(16) . ? P1 F4 1.5978(18) . ? P2 F10 1.502(8) . ? P2 F9 1.480(7) . ? P2 F12' 1.520(6) . ? P2 F11' 1.567(4) . ? P2 F7 1.5808(19) . ? P2 F8 1.585(2) . ? P2 F12 1.600(8) . ? P2 F11 1.551(8) . ? P2 F9' 1.591(4) . ? P2 F10' 1.598(6) . ? N1 C1 1.329(3) . ? N1 C5 1.356(3) . ? N2 C6 1.260(3) . ? N2 C7 1.465(3) . ? N3 C10 1.273(3) . ? N3 C9 1.469(3) . ? N4 C15 1.335(3) . ? N4 C11 1.352(4) . ? N5 C18 1.137(3) . ? N6 C20 1.135(3) . ? C1 C2 1.397(4) . ? C2 C3 1.370(5) . ? C3 C4 1.384(5) . ? C4 C5 1.390(3) . ? C5 C6 1.467(3) . ? C7 C8 1.531(3) . ? C8 C16 1.515(3) . ? C8 C9 1.539(3) . ? C8 C17 1.540(3) . ? C10 C11 1.462(3) . ? C11 C12 1.385(3) . ? C12 C13 1.388(5) . ? C13 C14 1.365(6) . ? C14 C15 1.408(5) . ? C18 C19 1.464(3) . ? C20 C21 1.453(3) . ? N1S C1S 1.116(5) . ? C1S C2S 1.421(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N3 91.08(7) . . ? N2 Ni1 N6 88.03(7) . . ? N3 Ni1 N6 93.57(7) . . ? N2 Ni1 N4 170.78(8) . . ? N3 Ni1 N4 80.08(8) . . ? N6 Ni1 N4 89.87(8) . . ? N2 Ni1 N1 79.45(8) . . ? N3 Ni1 N1 168.91(7) . . ? N6 Ni1 N1 91.88(7) . . ? N4 Ni1 N1 109.61(8) . . ? N2 Ni1 N5 97.34(7) . . ? N3 Ni1 N5 90.42(7) . . ? N6 Ni1 N5 173.25(7) . . ? N4 Ni1 N5 85.45(7) . . ? N1 Ni1 N5 85.13(7) . . ? F6 P1 F1 89.38(13) . . ? F6 P1 F5 91.87(12) . . ? F1 P1 F5 88.78(11) . . ? F6 P1 F3 89.58(13) . . ? F1 P1 F3 90.55(11) . . ? F5 P1 F3 178.40(13) . . ? F6 P1 F2 90.36(11) . . ? F1 P1 F2 179.72(13) . . ? F5 P1 F2 91.12(11) . . ? F3 P1 F2 89.55(10) . . ? F6 P1 F4 178.65(14) . . ? F1 P1 F4 90.13(11) . . ? F5 P1 F4 89.38(11) . . ? F3 P1 F4 89.17(12) . . ? F2 P1 F4 90.13(10) . . ? F10 P2 F9 96.4(9) . . ? F10 P2 F12' 154.3(9) . . ? F9 P2 F12' 58.2(7) . . ? F10 P2 F11' 112.7(9) . . ? F9 P2 F11' 150.0(9) . . ? F12' P2 F11' 93.0(6) . . ? F10 P2 F7 90.0(4) . . ? F9 P2 F7 96.6(9) . . ? F12' P2 F7 89.5(3) . . ? F11' P2 F7 90.7(3) . . ? F10 P2 F8 89.7(4) . . ? F9 P2 F8 85.5(9) . . ? F12' P2 F8 91.6(3) . . ? F11' P2 F8 87.5(3) . . ? F7 P2 F8 177.87(19) . . ? F10 P2 F12 177.3(8) . . ? F9 P2 F12 82.3(8) . . ? F12' P2 F12 24.1(7) . . ? F11' P2 F12 69.0(5) . . ? F7 P2 F12 87.8(4) . . ? F8 P2 F12 92.5(4) . . ? F10 P2 F11 95.8(9) . . ? F9 P2 F11 167.8(9) . . ? F12' P2 F11 109.7(8) . . ? F11' P2 F11 18.1(8) . . ? F7 P2 F11 84.2(6) . . ? F8 P2 F11 93.8(6) . . ? F12 P2 F11 85.6(7) . . ? F10 P2 F9' 59.1(8) . . ? F9 P2 F9' 37.9(7) . . ? F12' P2 F9' 95.2(6) . . ? F11' P2 F9' 171.9(5) . . ? F7 P2 F9' 89.3(2) . . ? F8 P2 F9' 92.4(2) . . ? F12 P2 F9' 119.2(5) . . ? F11 P2 F9' 154.2(7) . . ? F10 P2 F10' 25.0(9) . . ? F9 P2 F10' 120.8(8) . . ? F12' P2 F10' 178.2(6) . . ? F11' P2 F10' 87.8(4) . . ? F7 P2 F10' 92.1(4) . . ? F8 P2 F10' 86.8(3) . . ? F12 P2 F10' 156.8(5) . . ? F11 P2 F10' 71.2(7) . . ? F9' P2 F10' 84.1(4) . . ? C1 N1 C5 118.4(2) . . ? C1 N1 Ni1 130.33(19) . . ? C5 N1 Ni1 111.11(13) . . ? C6 N2 C7 119.7(2) . . ? C6 N2 Ni1 115.32(17) . . ? C7 N2 Ni1 124.20(15) . . ? C10 N3 C9 117.78(19) . . ? C10 N3 Ni1 113.70(15) . . ? C9 N3 Ni1 128.52(14) . . ? C15 N4 C11 118.0(2) . . ? C15 N4 Ni1 131.1(2) . . ? C11 N4 Ni1 110.96(15) . . ? C18 N5 Ni1 169.68(17) . . ? C20 N6 Ni1 177.26(19) . . ? N1 C1 C2 122.2(3) . . ? C3 C2 C1 119.3(3) . . ? C2 C3 C4 119.2(2) . . ? C3 C4 C5 118.6(3) . . ? N1 C5 C4 122.3(2) . . ? N1 C5 C6 115.32(18) . . ? C4 C5 C6 122.4(2) . . ? N2 C6 C5 118.6(2) . . ? N2 C7 C8 113.93(17) . . ? C16 C8 C7 110.41(18) . . ? C16 C8 C9 111.6(2) . . ? C7 C8 C9 111.80(18) . . ? C16 C8 C17 109.52(18) . . ? C7 C8 C17 106.46(19) . . ? C9 C8 C17 106.80(18) . . ? N3 C9 C8 115.60(17) . . ? N3 C10 C11 119.2(2) . . ? N4 C11 C12 123.0(2) . . ? N4 C11 C10 115.4(2) . . ? C12 C11 C10 121.5(2) . . ? C11 C12 C13 118.7(3) . . ? C14 C13 C12 118.7(3) . . ? C13 C14 C15 119.9(3) . . ? N4 C15 C14 121.7(3) . . ? N5 C18 C19 179.6(3) . . ? N6 C20 C21 179.3(2) . . ? N1S C1S C2S 178.1(4) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.421 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.043 _database_code_depnum_ccdc_archive 'CCDC 921477' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_vw13 #TrackingRef 'vw13.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H56 K N6 Ni O6' _chemical_formula_sum 'C35 H56 K N6 Ni O6' _chemical_formula_weight 754.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7277(11) _cell_length_b 21.000(2) _cell_length_c 28.837(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.126(4) _cell_angle_gamma 90.00 _cell_volume 7610.2(13) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4274 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 23.21 _exptl_crystal_description parallelorgam _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3224 _exptl_absorpt_coefficient_mu 0.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7755 _exptl_absorpt_correction_T_max 0.9867 _exptl_absorpt_process_details SADABS _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 X8 APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35129 _diffrn_reflns_av_R_equivalents 0.0896 _diffrn_reflns_av_sigmaI/netI 0.0839 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 21.26 _reflns_number_total 8405 _reflns_number_gt 4964 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1290P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8405 _refine_ls_number_parameters 883 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1258 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.2094 _refine_ls_wR_factor_gt 0.1682 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 K2 K 0.17661(12) 0.76018(8) -0.10461(6) 0.0261(5) Uani 1 1 d . . . Ni2 Ni 0.08218(7) 0.66726(5) 0.13906(3) 0.0224(3) Uani 1 1 d . . . O7 O -0.0183(4) 0.7319(3) -0.15831(18) 0.0404(15) Uani 1 1 d . . . O8 O 0.0600(4) 0.8569(3) -0.1564(2) 0.0452(16) Uani 1 1 d . . . O9 O 0.2101(4) 0.8016(3) -0.01007(17) 0.0340(14) Uani 1 1 d . . . O10 O 0.1971(4) 0.6688(2) -0.02807(17) 0.0306(13) Uani 1 1 d . . . O11 O 0.2868(4) 0.6895(3) -0.16599(17) 0.0333(14) Uani 1 1 d . . . O12 O 0.3679(4) 0.8063(2) -0.12955(17) 0.0298(13) Uani 1 1 d . . . N7 N 0.0906(5) 0.7574(3) 0.1403(2) 0.0302(17) Uani 1 1 d . . . N8 N 0.1310(4) 0.6723(3) 0.2038(2) 0.0245(16) Uani 1 1 d . . . N9 N 0.1231(4) 0.5830(3) 0.1329(2) 0.0251(16) Uani 1 1 d . . . N10 N -0.0151(4) 0.6508(3) 0.0822(2) 0.0245(16) Uani 1 1 d . . . N11 N 0.1195(5) 0.6250(3) -0.1245(2) 0.0318(17) Uani 1 1 d . . . N12 N 0.2395(5) 0.8939(3) -0.0813(2) 0.0364(18) Uani 1 1 d . . . C36 C 0.0685(6) 0.8032(4) 0.1067(3) 0.031(2) Uani 1 1 d . . . H36A H 0.0457 0.7895 0.0754 0.037 Uiso 1 1 calc R . . C37 C 0.0765(6) 0.8669(4) 0.1145(3) 0.039(2) Uani 1 1 d . . . H37A H 0.0607 0.8957 0.0890 0.047 Uiso 1 1 calc R . . C38 C 0.1077(7) 0.8902(4) 0.1597(3) 0.044(2) Uani 1 1 d . . . H38A H 0.1117 0.9347 0.1655 0.053 Uiso 1 1 calc R . . C39 C 0.1326(6) 0.8474(4) 0.1959(3) 0.034(2) Uani 1 1 d . . . H39A H 0.1552 0.8626 0.2269 0.041 Uiso 1 1 calc R . . C40 C 0.1250(5) 0.7813(4) 0.1873(3) 0.026(2) Uani 1 1 d . . . C41 C 0.1507(5) 0.7325(4) 0.2186(3) 0.026(2) Uani 1 1 d . . . H41A H 0.1818 0.7410 0.2502 0.031 Uiso 1 1 calc R . . C42 C 0.1841(6) 0.6228(4) 0.2341(3) 0.031(2) Uani 1 1 d . . . H42A H 0.1667 0.6288 0.2661 0.038 Uiso 1 1 calc R . . H42B H 0.2619 0.6283 0.2360 0.038 Uiso 1 1 calc R . . C43 C 0.1552(5) 0.5549(4) 0.2183(2) 0.027(2) Uani 1 1 d . . . C44 C 0.1841(6) 0.5439(4) 0.1687(2) 0.027(2) Uani 1 1 d . . . H44A H 0.2607 0.5530 0.1696 0.032 Uiso 1 1 calc R . . H44B H 0.1721 0.4985 0.1602 0.032 Uiso 1 1 calc R . . C45 C 0.0659(6) 0.5525(4) 0.0954(2) 0.0230(19) Uani 1 1 d . . . H45A H 0.0756 0.5085 0.0896 0.028 Uiso 1 1 calc R . . C46 C -0.0064(5) 0.5889(4) 0.0667(2) 0.0205(18) Uani 1 1 d . . . C47 C -0.0733(6) 0.5686(4) 0.0253(3) 0.035(2) Uani 1 1 d . . . H47A H -0.0665 0.5263 0.0144 0.042 Uiso 1 1 calc R . . C48 C -0.1461(7) 0.6074(5) 0.0011(3) 0.041(2) Uani 1 1 d . . . H48A H -0.1903 0.5931 -0.0266 0.049 Uiso 1 1 calc R . . C49 C -0.1554(6) 0.6694(5) 0.0176(3) 0.038(2) Uani 1 1 d . . . H49A H -0.2063 0.6978 0.0012 0.046 Uiso 1 1 calc R . . C50 C -0.0911(6) 0.6888(4) 0.0572(3) 0.027(2) Uani 1 1 d . . . H50A H -0.0994 0.7309 0.0681 0.032 Uiso 1 1 calc R . . C51 C 0.2232(6) 0.5086(4) 0.2524(3) 0.038(2) Uani 1 1 d . . . H51A H 0.2988 0.5171 0.2523 0.056 Uiso 1 1 calc R . . H51B H 0.2069 0.4646 0.2423 0.056 Uiso 1 1 calc R . . H51C H 0.2068 0.5145 0.2842 0.056 Uiso 1 1 calc R . . C52 C 0.0374(6) 0.5409(4) 0.2183(3) 0.039(2) Uani 1 1 d . . . H52A H -0.0060 0.5701 0.1967 0.058 Uiso 1 1 calc R . . H52B H 0.0207 0.5467 0.2501 0.058 Uiso 1 1 calc R . . H52C H 0.0218 0.4969 0.2082 0.058 Uiso 1 1 calc R . . C53 C -0.0514(7) 0.7743(5) -0.1952(3) 0.049(3) Uani 1 1 d . . . H53A H -0.1254 0.7642 -0.2096 0.059 Uiso 1 1 calc R . . H53B H -0.0054 0.7693 -0.2197 0.059 Uiso 1 1 calc R . . C54 C -0.0458(6) 0.8404(5) -0.1782(3) 0.048(3) Uani 1 1 d . . . H54A H -0.0952 0.8459 -0.1552 0.058 Uiso 1 1 calc R . . H54B H -0.0686 0.8696 -0.2048 0.058 Uiso 1 1 calc R . . C55 C 0.0635(6) 0.9135(5) -0.1315(3) 0.049(3) Uani 1 1 d . . . H55A H 0.0281 0.9074 -0.1037 0.059 Uiso 1 1 calc R . . H55B H 0.0233 0.9464 -0.1516 0.059 Uiso 1 1 calc R . . C56 C 0.1741(7) 0.9363(4) -0.1160(4) 0.059(3) Uani 1 1 d . . . H56A H 0.1712 0.9791 -0.1019 0.071 Uiso 1 1 calc R . . H56B H 0.2099 0.9406 -0.1439 0.071 Uiso 1 1 calc R . . C57 C 0.2170(7) 0.9094(4) -0.0341(3) 0.047(3) Uani 1 1 d . . . H57A H 0.1391 0.9133 -0.0355 0.056 Uiso 1 1 calc R . . H57B H 0.2491 0.9512 -0.0245 0.056 Uiso 1 1 calc R . . C58 C 0.2579(7) 0.8616(4) 0.0020(3) 0.048(3) Uani 1 1 d . . . H58A H 0.3361 0.8580 0.0043 0.057 Uiso 1 1 calc R . . H58B H 0.2418 0.8753 0.0329 0.057 Uiso 1 1 calc R . . C59 C 0.2399(6) 0.7549(4) 0.0254(3) 0.041(2) Uani 1 1 d . . . H59A H 0.2299 0.7720 0.0564 0.049 Uiso 1 1 calc R . . H59B H 0.3159 0.7437 0.0268 0.049 Uiso 1 1 calc R . . C60 C 0.1726(7) 0.6972(4) 0.0141(3) 0.039(2) Uani 1 1 d . . . H60A H 0.1863 0.6664 0.0403 0.046 Uiso 1 1 calc R . . H60B H 0.0964 0.7092 0.0098 0.046 Uiso 1 1 calc R . . C61 C 0.1402(7) 0.6106(4) -0.0379(3) 0.048(3) Uani 1 1 d . . . H61A H 0.0632 0.6182 -0.0385 0.058 Uiso 1 1 calc R . . H61B H 0.1643 0.5792 -0.0128 0.058 Uiso 1 1 calc R . . C62 C 0.1585(7) 0.5849(4) -0.0841(3) 0.044(2) Uani 1 1 d . . . H62A H 0.2359 0.5783 -0.0830 0.053 Uiso 1 1 calc R . . H62B H 0.1237 0.5427 -0.0888 0.053 Uiso 1 1 calc R . . C63 C 0.0043(6) 0.6228(4) -0.1332(3) 0.043(2) Uani 1 1 d . . . H63A H -0.0224 0.6333 -0.1036 0.051 Uiso 1 1 calc R . . H63B H -0.0186 0.5789 -0.1421 0.051 Uiso 1 1 calc R . . C64 C -0.0461(7) 0.6679(5) -0.1712(3) 0.048(3) Uani 1 1 d . . . H64A H -0.0212 0.6575 -0.2012 0.058 Uiso 1 1 calc R . . H64B H -0.1244 0.6630 -0.1759 0.058 Uiso 1 1 calc R . . C65 C 0.1652(6) 0.6033(4) -0.1659(3) 0.042(2) Uani 1 1 d . . . H65A H 0.1221 0.6209 -0.1946 0.050 Uiso 1 1 calc R . . H65B H 0.1602 0.5563 -0.1679 0.050 Uiso 1 1 calc R . . C66 C 0.2794(6) 0.6225(4) -0.1648(3) 0.039(2) Uani 1 1 d . . . H66A H 0.3232 0.6061 -0.1358 0.047 Uiso 1 1 calc R . . H66B H 0.3067 0.6040 -0.1921 0.047 Uiso 1 1 calc R . . C67 C 0.3937(6) 0.7093(4) -0.1691(3) 0.035(2) Uani 1 1 d . . . H67A H 0.4162 0.6908 -0.1975 0.042 Uiso 1 1 calc R . . H67B H 0.4430 0.6939 -0.1413 0.042 Uiso 1 1 calc R . . C68 C 0.3976(6) 0.7796(4) -0.1713(3) 0.034(2) Uani 1 1 d . . . H68A H 0.4705 0.7936 -0.1744 0.040 Uiso 1 1 calc R . . H68B H 0.3484 0.7949 -0.1991 0.040 Uiso 1 1 calc R . . C69 C 0.3868(6) 0.8723(4) -0.1278(3) 0.037(2) Uani 1 1 d . . . H69A H 0.3460 0.8930 -0.1558 0.045 Uiso 1 1 calc R . . H69B H 0.4634 0.8808 -0.1276 0.045 Uiso 1 1 calc R . . C70 C 0.3528(7) 0.8992(4) -0.0836(3) 0.046(2) Uani 1 1 d . . . H70A H 0.3931 0.8770 -0.0561 0.055 Uiso 1 1 calc R . . H70B H 0.3730 0.9448 -0.0811 0.055 Uiso 1 1 calc R . . K1 K 0.59480(12) 0.73336(8) 0.09188(5) 0.0253(5) Uani 1 1 d . . . Ni1 Ni 0.68784(7) 0.83925(4) -0.15050(3) 0.0211(3) Uani 1 1 d . . . O1 O 0.5845(4) 0.8333(3) 0.02188(18) 0.0396(15) Uani 1 1 d . . . O2 O 0.5586(4) 0.7046(3) -0.00494(17) 0.0319(13) Uani 1 1 d . . . O3 O 0.3982(4) 0.6875(3) 0.11191(18) 0.0339(14) Uani 1 1 d . . . O4 O 0.4855(4) 0.7998(3) 0.15457(18) 0.0349(14) Uani 1 1 d . . . O5 O 0.6995(4) 0.6275(3) 0.13660(19) 0.0391(15) Uani 1 1 d . . . O6 O 0.7873(4) 0.7505(3) 0.1503(2) 0.0450(16) Uani 1 1 d . . . N1 N 0.6786(4) 0.7483(3) -0.1511(2) 0.0248(16) Uani 1 1 d . . . N2 N 0.6408(4) 0.8326(3) -0.21569(19) 0.0218(15) Uani 1 1 d . . . N3 N 0.6491(5) 0.9252(3) -0.1465(2) 0.0292(17) Uani 1 1 d . . . N4 N 0.7852(5) 0.8575(3) -0.0940(2) 0.0244(16) Uani 1 1 d . . . N5 N 0.6638(6) 0.8641(3) 0.1216(3) 0.045(2) Uani 1 1 d . . . N6 N 0.5224(5) 0.6024(3) 0.0605(2) 0.0376(18) Uani 1 1 d . . . C1 C 0.6992(5) 0.7035(4) -0.1159(3) 0.0275(19) Uani 1 1 d . . . H1A H 0.7225 0.7183 -0.0848 0.033 Uiso 1 1 calc R . . C2 C 0.6887(6) 0.6406(4) -0.1225(3) 0.033(2) Uani 1 1 d . . . H2A H 0.7040 0.6122 -0.0967 0.039 Uiso 1 1 calc R . . C3 C 0.6543(6) 0.6164(4) -0.1688(3) 0.033(2) Uani 1 1 d . . . H3A H 0.6454 0.5719 -0.1741 0.040 Uiso 1 1 calc R . . C4 C 0.6350(6) 0.6576(4) -0.2042(3) 0.029(2) Uani 1 1 d . . . H4A H 0.6129 0.6419 -0.2351 0.035 Uiso 1 1 calc R . . C5 C 0.6464(5) 0.7238(4) -0.1971(3) 0.0225(19) Uani 1 1 d . . . C6 C 0.6206(5) 0.7712(4) -0.2300(3) 0.0224(19) Uani 1 1 d . . . H6A H 0.5900 0.7615 -0.2614 0.027 Uiso 1 1 calc R . . C7 C 0.5889(6) 0.8810(4) -0.2467(2) 0.027(2) Uani 1 1 d . . . H7A H 0.5110 0.8754 -0.2492 0.033 Uiso 1 1 calc R . . H7B H 0.6076 0.8740 -0.2784 0.033 Uiso 1 1 calc R . . C8 C 0.6160(6) 0.9495(4) -0.2325(3) 0.028(2) Uani 1 1 d . . . C9 C 0.5866(6) 0.9622(4) -0.1834(2) 0.027(2) Uani 1 1 d . . . H9A H 0.5968 1.0081 -0.1759 0.033 Uiso 1 1 calc R . . H9B H 0.5103 0.9523 -0.1841 0.033 Uiso 1 1 calc R . . C10 C 0.7073(6) 0.9567(4) -0.1109(3) 0.033(2) Uani 1 1 d . . . H10A H 0.6985 1.0012 -0.1068 0.040 Uiso 1 1 calc R . . C11 C 0.7801(6) 0.9222(4) -0.0807(3) 0.029(2) Uani 1 1 d . . . C12 C 0.8467(6) 0.9454(5) -0.0406(3) 0.040(2) Uani 1 1 d . . . H12A H 0.8418 0.9887 -0.0318 0.047 Uiso 1 1 calc R . . C13 C 0.9177(7) 0.9065(5) -0.0144(3) 0.049(3) Uani 1 1 d . . . H13A H 0.9621 0.9223 0.0127 0.059 Uiso 1 1 calc R . . C14 C 0.9249(6) 0.8426(5) -0.0279(3) 0.041(2) Uani 1 1 d . . . H14A H 0.9746 0.8148 -0.0101 0.049 Uiso 1 1 calc R . . C15 C 0.8590(6) 0.8210(4) -0.0671(3) 0.033(2) Uani 1 1 d . . . H15A H 0.8656 0.7778 -0.0759 0.039 Uiso 1 1 calc R . . C16 C 0.7331(6) 0.9644(4) -0.2324(3) 0.039(2) Uani 1 1 d . . . H16A H 0.7515 0.9554 -0.2635 0.059 Uiso 1 1 calc R . . H16B H 0.7769 0.9380 -0.2088 0.059 Uiso 1 1 calc R . . H16C H 0.7464 1.0095 -0.2248 0.059 Uiso 1 1 calc R . . C17 C 0.5486(6) 0.9935(4) -0.2676(3) 0.040(2) Uani 1 1 d . . . H17A H 0.4730 0.9841 -0.2679 0.060 Uiso 1 1 calc R . . H17B H 0.5666 0.9866 -0.2990 0.060 Uiso 1 1 calc R . . H17C H 0.5629 1.0379 -0.2582 0.060 Uiso 1 1 calc R . . C18 C 0.5993(6) 0.8117(4) -0.0234(3) 0.041(2) Uani 1 1 d . . . H18A H 0.6745 0.7991 -0.0230 0.050 Uiso 1 1 calc R . . H18B H 0.5818 0.8461 -0.0468 0.050 Uiso 1 1 calc R . . C19 C 0.5280(7) 0.7558(4) -0.0364(3) 0.040(2) Uani 1 1 d . . . H19A H 0.4534 0.7679 -0.0350 0.047 Uiso 1 1 calc R . . H19B H 0.5326 0.7423 -0.0689 0.047 Uiso 1 1 calc R . . C20 C 0.5070(7) 0.6482(4) -0.0210(3) 0.046(2) Uani 1 1 d . . . H20A H 0.5219 0.6382 -0.0528 0.055 Uiso 1 1 calc R . . H20B H 0.4291 0.6534 -0.0228 0.055 Uiso 1 1 calc R . . C21 C 0.5460(8) 0.5944(4) 0.0124(3) 0.054(3) Uani 1 1 d . . . H21A H 0.5133 0.5542 -0.0007 0.065 Uiso 1 1 calc R . . H21B H 0.6240 0.5904 0.0140 0.065 Uiso 1 1 calc R . . C22 C 0.4091(7) 0.5971(4) 0.0622(3) 0.045(2) Uani 1 1 d . . . H22A H 0.3880 0.5518 0.0581 0.054 Uiso 1 1 calc R . . H22B H 0.3694 0.6212 0.0355 0.054 Uiso 1 1 calc R . . C23 C 0.3773(6) 0.6210(4) 0.1069(3) 0.039(2) Uani 1 1 d . . . H23A H 0.3005 0.6131 0.1065 0.047 Uiso 1 1 calc R . . H23B H 0.4175 0.5979 0.1339 0.047 Uiso 1 1 calc R . . C24 C 0.3706(6) 0.7100(4) 0.1554(3) 0.040(2) Uani 1 1 d . . . H24A H 0.4196 0.6915 0.1821 0.048 Uiso 1 1 calc R . . H24B H 0.2973 0.6965 0.1580 0.048 Uiso 1 1 calc R . . C25 C 0.3780(6) 0.7805(4) 0.1571(3) 0.042(2) Uani 1 1 d . . . H25A H 0.3288 0.7991 0.1305 0.051 Uiso 1 1 calc R . . H25B H 0.3570 0.7963 0.1867 0.051 Uiso 1 1 calc R . . C26 C 0.4984(7) 0.8671(4) 0.1568(3) 0.049(3) Uani 1 1 d . . . H26A H 0.4671 0.8844 0.1835 0.058 Uiso 1 1 calc R . . H26B H 0.4612 0.8868 0.1275 0.058 Uiso 1 1 calc R . . C27 C 0.6140(7) 0.8825(4) 0.1629(3) 0.047(3) Uani 1 1 d . . . H27A H 0.6236 0.9288 0.1683 0.056 Uiso 1 1 calc R . . H27B H 0.6510 0.8601 0.1910 0.056 Uiso 1 1 calc R . . C28 C 0.6316(9) 0.9094(5) 0.0821(4) 0.070(3) Uani 1 1 d . . . H28A H 0.6700 0.9500 0.0894 0.084 Uiso 1 1 calc R . . H28B H 0.5545 0.9182 0.0797 0.084 Uiso 1 1 calc R . . C29 C 0.6534(9) 0.8855(5) 0.0358(4) 0.069(3) Uani 1 1 d . . . H29A H 0.6408 0.9198 0.0120 0.083 Uiso 1 1 calc R . . H29B H 0.7285 0.8717 0.0385 0.083 Uiso 1 1 calc R . . C30 C 0.5813(7) 0.5552(4) 0.0914(3) 0.053(3) Uani 1 1 d . . . H30A H 0.5784 0.5139 0.0747 0.064 Uiso 1 1 calc R . . H30B H 0.5456 0.5495 0.1192 0.064 Uiso 1 1 calc R . . C31 C 0.6951(7) 0.5720(4) 0.1078(3) 0.053(3) Uani 1 1 d . . . H31A H 0.7318 0.5362 0.1260 0.064 Uiso 1 1 calc R . . H31B H 0.7313 0.5803 0.0804 0.064 Uiso 1 1 calc R . . C32 C 0.8067(6) 0.6378(5) 0.1583(3) 0.047(3) Uani 1 1 d . . . H32A H 0.8539 0.6371 0.1341 0.056 Uiso 1 1 calc R . . H32B H 0.8292 0.6032 0.1810 0.056 Uiso 1 1 calc R . . C33 C 0.8172(6) 0.7000(6) 0.1830(3) 0.057(3) Uani 1 1 d . . . H33A H 0.7709 0.7006 0.2076 0.068 Uiso 1 1 calc R . . H33B H 0.8917 0.7061 0.1985 0.068 Uiso 1 1 calc R . . C34 C 0.8211(7) 0.8096(6) 0.1698(4) 0.060(3) Uani 1 1 d . . . H34A H 0.8998 0.8108 0.1768 0.072 Uiso 1 1 calc R . . H34B H 0.7928 0.8163 0.1994 0.072 Uiso 1 1 calc R . . C35 C 0.7810(8) 0.8613(5) 0.1349(4) 0.065(3) Uani 1 1 d . . . H35A H 0.8063 0.9029 0.1485 0.078 Uiso 1 1 calc R . . H35B H 0.8130 0.8548 0.1061 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K2 0.0203(10) 0.0407(12) 0.0186(10) 0.0047(8) 0.0073(8) 0.0010(8) Ni2 0.0182(6) 0.0400(7) 0.0094(6) 0.0004(4) 0.0034(4) 0.0006(4) O7 0.028(3) 0.072(5) 0.019(3) 0.003(3) 0.000(3) 0.005(3) O8 0.041(4) 0.055(4) 0.045(4) 0.018(3) 0.024(3) 0.017(3) O9 0.034(3) 0.049(4) 0.017(3) -0.001(3) -0.002(3) 0.007(3) O10 0.032(3) 0.043(4) 0.021(3) 0.000(3) 0.014(3) -0.005(3) O11 0.021(3) 0.053(4) 0.029(4) -0.002(3) 0.014(3) -0.001(3) O12 0.027(3) 0.038(4) 0.027(3) 0.006(3) 0.015(3) 0.002(3) N7 0.016(4) 0.050(5) 0.028(5) 0.007(4) 0.016(3) 0.003(3) N8 0.023(4) 0.041(5) 0.009(4) -0.001(3) 0.002(3) 0.001(3) N9 0.017(4) 0.042(4) 0.016(4) 0.002(3) 0.001(3) 0.007(3) N10 0.015(4) 0.045(5) 0.015(4) 0.000(3) 0.008(3) -0.001(3) N11 0.027(4) 0.041(4) 0.029(4) -0.005(3) 0.008(3) -0.003(3) N12 0.025(4) 0.038(4) 0.048(5) 0.005(4) 0.012(4) 0.001(3) C36 0.032(5) 0.048(6) 0.013(5) 0.001(4) 0.010(4) -0.004(4) C37 0.042(6) 0.038(6) 0.036(6) 0.007(5) 0.002(4) -0.006(4) C38 0.051(6) 0.031(6) 0.050(7) -0.009(5) 0.004(5) 0.000(4) C39 0.031(5) 0.044(6) 0.028(6) -0.008(5) 0.006(4) -0.004(4) C40 0.013(4) 0.050(6) 0.013(5) -0.009(4) 0.002(3) -0.003(4) C41 0.012(4) 0.049(6) 0.019(5) -0.009(5) 0.005(4) -0.001(4) C42 0.031(5) 0.048(6) 0.017(5) 0.000(4) 0.009(4) -0.002(4) C43 0.016(5) 0.045(6) 0.020(5) 0.008(4) 0.010(4) 0.005(4) C44 0.016(4) 0.043(5) 0.023(5) 0.000(4) 0.007(4) 0.007(4) C45 0.028(5) 0.029(5) 0.012(5) 0.003(4) 0.003(4) 0.000(4) C46 0.018(4) 0.034(5) 0.010(5) 0.002(4) 0.005(4) -0.013(4) C47 0.031(5) 0.047(6) 0.029(6) -0.007(5) 0.007(4) -0.001(4) C48 0.033(6) 0.074(8) 0.017(5) -0.005(5) 0.003(4) -0.015(5) C49 0.021(5) 0.071(7) 0.020(5) 0.009(5) -0.003(4) -0.005(4) C50 0.018(5) 0.048(5) 0.014(5) 0.009(4) 0.004(4) 0.005(4) C51 0.039(5) 0.046(6) 0.027(5) 0.014(4) 0.005(4) 0.011(4) C52 0.034(5) 0.055(6) 0.031(5) 0.005(4) 0.016(4) 0.005(4) C53 0.025(5) 0.094(9) 0.028(6) 0.009(6) 0.006(4) 0.009(5) C54 0.008(5) 0.090(8) 0.048(6) 0.033(6) 0.007(4) 0.008(5) C55 0.022(6) 0.062(7) 0.064(7) 0.036(6) 0.013(5) 0.012(5) C56 0.052(7) 0.051(6) 0.079(8) 0.026(6) 0.019(6) 0.016(5) C57 0.051(6) 0.034(6) 0.060(7) -0.011(5) 0.022(5) 0.002(5) C58 0.053(6) 0.055(7) 0.038(6) -0.022(5) 0.017(5) -0.016(5) C59 0.030(5) 0.077(7) 0.016(5) -0.012(5) 0.005(4) -0.001(5) C60 0.051(6) 0.056(6) 0.012(5) 0.005(4) 0.016(4) 0.011(5) C61 0.055(6) 0.060(7) 0.034(6) 0.013(5) 0.017(5) -0.011(5) C62 0.053(6) 0.037(6) 0.043(6) 0.006(5) 0.008(5) -0.003(4) C63 0.032(6) 0.060(6) 0.038(6) -0.012(5) 0.008(4) -0.004(5) C64 0.028(5) 0.076(8) 0.041(6) -0.029(6) 0.006(5) -0.013(5) C65 0.033(6) 0.059(6) 0.035(6) -0.023(5) 0.014(4) -0.002(4) C66 0.034(6) 0.057(7) 0.029(5) -0.013(4) 0.015(4) 0.002(4) C67 0.018(5) 0.067(7) 0.022(5) -0.009(4) 0.013(4) -0.001(4) C68 0.016(5) 0.073(7) 0.015(5) 0.006(4) 0.013(4) -0.002(4) C69 0.020(5) 0.054(6) 0.042(6) 0.016(5) 0.015(4) -0.001(4) C70 0.039(6) 0.030(5) 0.068(7) -0.002(5) 0.013(5) -0.006(4) K1 0.0232(10) 0.0385(11) 0.0150(10) 0.0002(8) 0.0053(8) -0.0009(8) Ni1 0.0175(6) 0.0376(7) 0.0089(6) -0.0017(4) 0.0038(4) 0.0008(4) O1 0.053(4) 0.045(4) 0.026(4) 0.002(3) 0.025(3) -0.008(3) O2 0.035(3) 0.045(4) 0.014(3) -0.005(3) -0.002(2) 0.004(3) O3 0.029(3) 0.045(4) 0.031(4) 0.004(3) 0.016(3) -0.001(3) O4 0.020(3) 0.057(4) 0.028(3) -0.005(3) 0.005(2) 0.005(3) O5 0.021(4) 0.067(4) 0.031(4) 0.019(3) 0.010(3) 0.020(3) O6 0.029(4) 0.074(5) 0.032(4) -0.012(4) 0.004(3) 0.001(3) N1 0.019(4) 0.047(4) 0.007(4) -0.002(3) -0.003(3) 0.000(3) N2 0.019(4) 0.039(4) 0.007(4) 0.005(3) 0.002(3) 0.002(3) N3 0.028(4) 0.047(5) 0.015(4) -0.003(3) 0.010(3) 0.001(3) N4 0.017(4) 0.051(5) 0.006(4) 0.000(3) 0.003(3) 0.000(3) N5 0.044(5) 0.045(5) 0.046(5) -0.019(4) 0.010(4) -0.014(4) N6 0.040(5) 0.031(4) 0.047(5) 0.000(4) 0.025(4) 0.005(3) C1 0.021(5) 0.046(6) 0.015(5) 0.002(4) 0.000(4) 0.003(4) C2 0.035(5) 0.035(6) 0.026(6) 0.012(4) 0.000(4) 0.001(4) C3 0.031(5) 0.032(5) 0.035(6) -0.004(5) 0.001(4) 0.002(4) C4 0.021(5) 0.044(6) 0.024(5) -0.009(5) 0.005(4) 0.003(4) C5 0.018(4) 0.038(6) 0.015(5) -0.007(4) 0.012(3) -0.002(4) C6 0.020(5) 0.040(6) 0.008(5) -0.002(4) 0.002(4) -0.006(4) C7 0.029(5) 0.039(5) 0.011(5) 0.000(4) -0.002(4) -0.001(4) C8 0.021(5) 0.039(5) 0.024(5) 0.007(4) 0.001(4) 0.008(4) C9 0.027(5) 0.036(5) 0.021(5) 0.004(4) 0.010(4) 0.011(4) C10 0.033(5) 0.045(6) 0.027(5) -0.013(5) 0.019(4) 0.005(4) C11 0.024(5) 0.042(6) 0.024(5) -0.009(4) 0.013(4) 0.002(4) C12 0.033(5) 0.068(7) 0.018(5) -0.019(5) 0.006(4) -0.010(5) C13 0.037(6) 0.092(9) 0.018(5) -0.023(6) 0.004(5) -0.026(6) C14 0.025(5) 0.065(7) 0.031(6) 0.003(5) 0.001(4) -0.010(5) C15 0.021(5) 0.054(6) 0.025(5) -0.004(4) 0.011(4) 0.000(4) C16 0.034(6) 0.050(6) 0.038(6) 0.006(4) 0.020(4) -0.003(4) C17 0.039(5) 0.056(6) 0.026(5) 0.012(4) 0.007(4) 0.007(4) C18 0.027(5) 0.062(6) 0.036(6) 0.019(5) 0.008(4) 0.005(5) C19 0.042(6) 0.071(7) 0.008(5) 0.002(5) 0.011(4) 0.016(5) C20 0.046(6) 0.061(7) 0.032(6) -0.016(5) 0.011(5) -0.003(5) C21 0.069(7) 0.043(6) 0.057(7) -0.023(5) 0.030(6) -0.004(5) C22 0.041(6) 0.036(6) 0.060(7) -0.004(5) 0.015(5) -0.008(4) C23 0.030(5) 0.049(6) 0.038(6) 0.017(5) 0.006(4) 0.002(4) C24 0.025(5) 0.079(8) 0.018(5) 0.000(5) 0.011(4) -0.001(5) C25 0.016(5) 0.087(8) 0.025(5) -0.012(5) 0.007(4) 0.008(5) C26 0.046(7) 0.054(7) 0.046(6) -0.011(5) 0.009(5) 0.014(5) C27 0.053(7) 0.052(6) 0.035(6) -0.030(5) 0.005(5) -0.007(5) C28 0.093(9) 0.043(7) 0.073(9) 0.002(6) 0.015(7) -0.028(6) C29 0.085(8) 0.069(8) 0.060(8) 0.011(6) 0.027(6) -0.028(6) C30 0.051(7) 0.036(6) 0.079(8) 0.012(5) 0.026(6) 0.014(5) C31 0.049(7) 0.055(7) 0.058(7) 0.014(6) 0.019(5) 0.026(5) C32 0.017(5) 0.090(8) 0.037(6) 0.031(6) 0.013(4) 0.017(5) C33 0.009(5) 0.141(11) 0.021(6) 0.011(7) 0.004(4) 0.002(6) C34 0.028(6) 0.103(9) 0.051(7) -0.029(7) 0.010(5) -0.006(6) C35 0.065(8) 0.060(7) 0.074(8) -0.043(6) 0.024(6) -0.036(6) _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 K2 O7 2.772(5) . ? K2 O8 2.803(6) . ? K2 O12 2.817(5) . ? K2 O9 2.829(5) . ? K2 O11 2.845(5) . ? K2 O10 2.905(5) . ? K2 N11 2.964(6) . ? K2 N12 2.968(7) . ? Ni2 N9 1.861(6) . ? Ni2 N8 1.875(6) . ? Ni2 N7 1.897(7) . ? Ni2 N10 1.923(6) . ? O7 C64 1.424(9) . ? O7 C53 1.400(10) . ? O8 C55 1.384(10) . ? O8 C54 1.435(10) . ? O9 C58 1.419(9) . ? O9 C59 1.424(9) . ? O10 C61 1.426(9) . ? O10 C60 1.434(8) . ? O11 C66 1.411(9) . ? O11 C67 1.439(8) . ? O12 C69 1.407(9) . ? O12 C68 1.432(8) . ? N7 C36 1.362(9) . ? N7 C40 1.446(9) . ? N8 C41 1.344(9) . ? N8 C42 1.453(9) . ? N9 C45 1.363(9) . ? N9 C44 1.446(9) . ? N10 C50 1.367(9) . ? N10 C46 1.385(9) . ? N11 C63 1.448(9) . ? N11 C62 1.460(10) . ? N11 C65 1.480(9) . ? N12 C57 1.471(10) . ? N12 C70 1.459(10) . ? N12 C56 1.490(10) . ? C36 C37 1.358(11) . ? C37 C38 1.389(11) . ? C38 C39 1.374(11) . ? C39 C40 1.412(10) . ? C40 C41 1.370(10) . ? C42 C43 1.523(10) . ? C43 C52 1.528(10) . ? C43 C51 1.547(10) . ? C43 C44 1.550(10) . ? C45 C46 1.371(10) . ? C46 C47 1.418(10) . ? C47 C48 1.344(11) . ? C48 C49 1.397(11) . ? C49 C50 1.357(10) . ? C53 C54 1.472(12) . ? C55 C56 1.487(12) . ? C57 C58 1.479(12) . ? C59 C60 1.489(11) . ? C61 C62 1.490(11) . ? C63 C64 1.513(12) . ? C65 C66 1.503(11) . ? C67 C68 1.480(11) . ? C69 C70 1.517(11) . ? K1 O6 2.769(6) . ? K1 O5 2.800(5) . ? K1 O4 2.819(5) . ? K1 O2 2.822(5) . ? K1 O3 2.825(5) . ? K1 O1 2.901(5) . ? K1 N5 2.967(7) . ? K1 N6 2.995(7) . ? Ni1 N2 1.885(6) . ? Ni1 N3 1.880(6) . ? Ni1 N1 1.913(6) . ? Ni1 N4 1.921(6) . ? O1 C29 1.420(10) . ? O1 C18 1.424(10) . ? O2 C20 1.398(9) . ? O2 C19 1.420(9) . ? O3 C23 1.424(9) . ? O3 C24 1.434(9) . ? O4 C26 1.423(10) . ? O4 C25 1.441(9) . ? O5 C31 1.426(10) . ? O5 C32 1.426(9) . ? O6 C34 1.400(11) . ? O6 C33 1.430(11) . ? N1 C1 1.378(9) . ? N1 C5 1.421(9) . ? N2 C6 1.366(9) . ? N2 C7 1.443(9) . ? N3 C10 1.340(9) . ? N3 C9 1.450(9) . ? N4 C15 1.358(9) . ? N4 C11 1.416(9) . ? N5 C35 1.482(12) . ? N5 C28 1.489(11) . ? N5 C27 1.486(10) . ? N6 C22 1.454(10) . ? N6 C30 1.460(10) . ? N6 C21 1.473(10) . ? C1 C2 1.340(10) . ? C2 C3 1.429(11) . ? C3 C4 1.331(10) . ? C4 C5 1.410(10) . ? C5 C6 1.379(10) . ? C7 C8 1.520(10) . ? C8 C16 1.523(10) . ? C8 C17 1.529(10) . ? C8 C9 1.544(10) . ? C10 C11 1.374(10) . ? C11 C12 1.408(11) . ? C12 C13 1.355(12) . ? C13 C14 1.402(12) . ? C14 C15 1.373(11) . ? C18 C19 1.494(11) . ? C20 C21 1.515(12) . ? C22 C23 1.497(11) . ? C24 C25 1.484(11) . ? C26 C27 1.489(11) . ? C28 C29 1.495(13) . ? C30 C31 1.493(12) . ? C32 C33 1.484(13) . ? C34 C35 1.512(14) . ? 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 O7 K2 O8 60.41(18) . . ? O7 K2 O12 131.60(16) . . ? O8 K2 O12 91.21(16) . . ? O7 K2 O9 126.08(16) . . ? O8 K2 O9 106.05(18) . . ? O12 K2 O9 97.82(15) . . ? O7 K2 O11 91.53(16) . . ? O8 K2 O11 108.60(17) . . ? O12 K2 O11 59.28(15) . . ? O9 K2 O11 138.26(15) . . ? O7 K2 O10 104.34(16) . . ? O8 K2 O10 149.26(15) . . ? O12 K2 O10 116.35(15) . . ? O9 K2 O10 59.27(15) . . ? O11 K2 O10 97.72(15) . . ? O7 K2 N11 61.08(18) . . ? O8 K2 N11 119.9(2) . . ? O12 K2 N11 118.36(17) . . ? O9 K2 N11 118.42(18) . . ? O11 K2 N11 60.63(16) . . ? O10 K2 N11 60.29(16) . . ? O7 K2 N12 120.94(18) . . ? O8 K2 N12 62.32(19) . . ? O12 K2 N12 61.28(16) . . ? O9 K2 N12 59.82(17) . . ? O11 K2 N12 119.52(17) . . ? O10 K2 N12 117.69(17) . . ? N11 K2 N12 177.77(19) . . ? N9 Ni2 N8 95.5(3) . . ? N9 Ni2 N7 159.3(2) . . ? N8 Ni2 N7 85.1(3) . . ? N9 Ni2 N10 84.2(3) . . ? N8 Ni2 N10 157.9(2) . . ? N7 Ni2 N10 102.8(3) . . ? C64 O7 C53 111.6(7) . . ? C64 O7 K2 120.7(5) . . ? C53 O7 K2 115.1(5) . . ? C55 O8 C54 112.7(6) . . ? C55 O8 K2 112.1(5) . . ? C54 O8 K2 116.0(5) . . ? C58 O9 C59 112.4(6) . . ? C58 O9 K2 120.1(5) . . ? C59 O9 K2 117.6(4) . . ? C61 O10 C60 110.7(6) . . ? C61 O10 K2 115.7(4) . . ? C60 O10 K2 111.4(4) . . ? C66 O11 C67 111.0(6) . . ? C66 O11 K2 117.6(4) . . ? C67 O11 K2 116.9(4) . . ? C69 O12 C68 110.4(6) . . ? C69 O12 K2 118.7(4) . . ? C68 O12 K2 115.8(4) . . ? C36 N7 C40 114.8(7) . . ? C36 N7 Ni2 133.3(6) . . ? C40 N7 Ni2 111.8(5) . . ? C41 N8 C42 115.9(6) . . ? C41 N8 Ni2 112.6(5) . . ? C42 N8 Ni2 127.3(5) . . ? C45 N9 C44 117.3(6) . . ? C45 N9 Ni2 113.6(5) . . ? C44 N9 Ni2 126.7(5) . . ? C50 N10 C46 117.6(6) . . ? C50 N10 Ni2 130.6(5) . . ? C46 N10 Ni2 111.7(5) . . ? C63 N11 C62 109.0(6) . . ? C63 N11 C65 111.6(6) . . ? C62 N11 C65 109.8(6) . . ? C63 N11 K2 105.9(5) . . ? C62 N11 K2 110.8(5) . . ? C65 N11 K2 109.6(5) . . ? C57 N12 C70 111.4(7) . . ? C57 N12 C56 108.7(7) . . ? C70 N12 C56 112.0(7) . . ? C57 N12 K2 109.4(5) . . ? C70 N12 K2 107.2(4) . . ? C56 N12 K2 108.1(5) . . ? N7 C36 C37 125.2(8) . . ? C36 C37 C38 120.3(8) . . ? C39 C38 C37 118.7(8) . . ? C38 C39 C40 120.6(8) . . ? C41 C40 C39 128.2(7) . . ? C41 C40 N7 111.3(7) . . ? C39 C40 N7 120.5(7) . . ? N8 C41 C40 118.8(7) . . ? N8 C42 C43 115.0(6) . . ? C52 C43 C42 111.8(6) . . ? C52 C43 C51 109.2(6) . . ? C42 C43 C51 108.4(6) . . ? C52 C43 C44 110.3(6) . . ? C42 C43 C44 109.5(6) . . ? C51 C43 C44 107.5(6) . . ? N9 C44 C43 113.3(6) . . ? N9 C45 C46 116.0(7) . . ? C45 C46 N10 114.2(7) . . ? C45 C46 C47 126.6(7) . . ? N10 C46 C47 119.2(7) . . ? C48 C47 C46 121.7(8) . . ? C47 C48 C49 118.5(8) . . ? C50 C49 C48 119.5(8) . . ? N10 C50 C49 123.5(8) . . ? O7 C53 C54 110.6(7) . . ? C53 C54 O8 111.6(7) . . ? O8 C55 C56 112.5(7) . . ? C55 C56 N12 114.3(7) . . ? N12 C57 C58 113.8(7) . . ? O9 C58 C57 110.0(7) . . ? O9 C59 C60 108.9(6) . . ? O10 C60 C59 109.2(6) . . ? O10 C61 C62 110.0(7) . . ? N11 C62 C61 115.1(7) . . ? N11 C63 C64 113.9(7) . . ? O7 C64 C63 110.0(7) . . ? N11 C65 C66 113.7(7) . . ? O11 C66 C65 109.6(6) . . ? O11 C67 C68 109.3(6) . . ? O12 C68 C67 109.8(6) . . ? O12 C69 C70 109.1(6) . . ? N12 C70 C69 115.1(7) . . ? O6 K1 O5 60.83(18) . . ? O6 K1 O4 91.37(16) . . ? O5 K1 O4 110.18(16) . . ? O6 K1 O2 128.34(16) . . ? O5 K1 O2 106.09(17) . . ? O4 K1 O2 136.09(15) . . ? O6 K1 O3 130.30(17) . . ? O5 K1 O3 90.40(16) . . ? O4 K1 O3 59.65(16) . . ? O2 K1 O3 96.81(16) . . ? O6 K1 O1 105.50(18) . . ? O5 K1 O1 149.43(16) . . ? O4 K1 O1 96.64(16) . . ? O2 K1 O1 58.93(16) . . ? O3 K1 O1 116.46(16) . . ? O6 K1 N5 60.7(2) . . ? O5 K1 N5 120.3(2) . . ? O4 K1 N5 60.68(18) . . ? O2 K1 N5 118.54(19) . . ? O3 K1 N5 119.18(18) . . ? O1 K1 N5 60.65(18) . . ? O6 K1 N6 120.3(2) . . ? O5 K1 N6 60.73(18) . . ? O4 K1 N6 119.28(17) . . ? O2 K1 N6 60.68(17) . . ? O3 K1 N6 60.57(16) . . ? O1 K1 N6 118.44(18) . . ? N5 K1 N6 179.0(2) . . ? N2 Ni1 N3 95.0(3) . . ? N2 Ni1 N1 84.8(3) . . ? N3 Ni1 N1 160.5(3) . . ? N2 Ni1 N4 156.9(2) . . ? N3 Ni1 N4 84.0(3) . . ? N1 Ni1 N4 103.7(3) . . ? C29 O1 C18 109.9(6) . . ? C29 O1 K1 113.9(5) . . ? C18 O1 K1 114.2(4) . . ? C20 O2 C19 111.3(6) . . ? C20 O2 K1 120.2(5) . . ? C19 O2 K1 117.1(4) . . ? C23 O3 C24 110.2(6) . . ? C23 O3 K1 118.1(4) . . ? C24 O3 K1 114.4(4) . . ? C26 O4 C25 112.4(6) . . ? C26 O4 K1 117.1(4) . . ? C25 O4 K1 117.6(4) . . ? C31 O5 C32 109.0(6) . . ? C31 O5 K1 114.1(5) . . ? C32 O5 K1 115.7(5) . . ? C34 O6 C33 111.1(8) . . ? C34 O6 K1 123.0(5) . . ? C33 O6 K1 114.9(5) . . ? C1 N1 C5 115.7(6) . . ? C1 N1 Ni1 132.1(5) . . ? C5 N1 Ni1 112.2(5) . . ? C6 N2 C7 115.6(6) . . ? C6 N2 Ni1 112.7(5) . . ? C7 N2 Ni1 127.5(5) . . ? C10 N3 C9 118.0(7) . . ? C10 N3 Ni1 113.8(5) . . ? C9 N3 Ni1 126.0(5) . . ? C15 N4 C11 116.3(6) . . ? C15 N4 Ni1 131.8(6) . . ? C11 N4 Ni1 111.7(5) . . ? C35 N5 C28 111.6(8) . . ? C35 N5 C27 110.0(7) . . ? C28 N5 C27 110.2(7) . . ? C35 N5 K1 106.1(5) . . ? C28 N5 K1 109.7(5) . . ? C27 N5 K1 109.2(5) . . ? C22 N6 C30 110.0(6) . . ? C22 N6 C21 112.0(7) . . ? C30 N6 C21 109.7(7) . . ? C22 N6 K1 108.6(4) . . ? C30 N6 K1 109.5(5) . . ? C21 N6 K1 106.8(5) . . ? C2 C1 N1 124.4(7) . . ? C1 C2 C3 119.6(7) . . ? C4 C3 C2 118.4(8) . . ? C3 C4 C5 121.8(8) . . ? C6 C5 C4 127.1(7) . . ? C6 C5 N1 112.5(7) . . ? C4 C5 N1 120.1(7) . . ? N2 C6 C5 117.4(7) . . ? N2 C7 C8 115.9(6) . . ? C7 C8 C16 112.0(6) . . ? C7 C8 C17 108.3(6) . . ? C16 C8 C17 108.9(6) . . ? C7 C8 C9 109.5(6) . . ? C16 C8 C9 110.0(6) . . ? C17 C8 C9 108.0(6) . . ? N3 C9 C8 113.3(6) . . ? N3 C10 C11 117.4(7) . . ? C10 C11 N4 112.9(7) . . ? C10 C11 C12 126.6(8) . . ? N4 C11 C12 120.4(7) . . ? C13 C12 C11 120.7(8) . . ? C12 C13 C14 119.2(8) . . ? C15 C14 C13 119.1(8) . . ? N4 C15 C14 124.1(8) . . ? O1 C18 C19 108.5(6) . . ? O2 C19 C18 109.9(7) . . ? O2 C20 C21 109.4(7) . . ? N6 C21 C20 114.7(7) . . ? N6 C22 C23 114.1(7) . . ? O3 C23 C22 110.2(6) . . ? O3 C24 C25 109.6(7) . . ? O4 C25 C24 109.5(6) . . ? O4 C26 C27 109.0(7) . . ? N5 C27 C26 112.8(7) . . ? N5 C28 C29 113.6(9) . . ? O1 C29 C28 108.5(8) . . ? N6 C30 C31 114.3(7) . . ? O5 C31 C30 108.8(7) . . ? O5 C32 C33 110.6(7) . . ? O6 C33 C32 110.0(7) . . ? O6 C34 C35 108.7(8) . . ? N5 C35 C34 114.9(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 21.26 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.159 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.113 _database_code_depnum_ccdc_archive 'CCDC 921478' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_vw17 #TrackingRef 'vw17.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H34 N8 Ni, 2(C18 H36 K N2 O6)' _chemical_formula_sum 'C70 H106 K2 N12 Ni O12' _chemical_formula_weight 1444.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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 34.460(7) _cell_length_b 10.852(5) _cell_length_c 23.144(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.903(4) _cell_angle_gamma 90.00 _cell_volume 8499(4) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 467 _cell_measurement_theta_min 4.33 _cell_measurement_theta_max 20.35 _exptl_crystal_description rombus _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.384 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9271 _exptl_absorpt_correction_T_max 0.9886 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 X8 APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24183 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 23.26 _reflns_number_total 6091 _reflns_number_gt 4267 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disordered THF was SQEEZEd ; # SQUEEZE RESULTS # 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 -0.126 0.232 671 143 ' ' 2 0.500 0.029 0.457 671 143 ' ' _platon_squeeze_details ; ; _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^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6091 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.48881(4) 0.2500 0.03943(16) Uani 1 2 d S . . N1 N 0.04420(6) 0.60055(18) 0.26787(9) 0.0379(5) Uani 1 1 d . . . N2 N 0.03973(6) 0.38234(18) 0.23052(9) 0.0402(5) Uani 1 1 d . . . N3 N 0.14259(6) 0.37885(18) 0.22281(9) 0.0378(5) Uani 1 1 d . . . N4 N 0.23339(6) 0.2778(2) 0.18117(10) 0.0478(6) Uani 1 1 d . . . C1 C 0.04479(9) 0.7193(3) 0.28663(12) 0.0470(7) Uani 1 1 d . . . C2 C 0.07639(9) 0.7954(3) 0.29159(13) 0.0535(8) Uani 1 1 d . . . C3 C 0.11148(9) 0.7519(3) 0.27675(13) 0.0522(8) Uani 1 1 d . . . C4 C 0.11266(8) 0.6321(3) 0.25814(11) 0.0416(7) Uani 1 1 d . . . C5 C 0.07930(7) 0.5570(2) 0.25358(10) 0.0350(6) Uani 1 1 d . . . C6 C 0.07644(7) 0.4306(2) 0.23578(10) 0.0351(6) Uani 1 1 d . . . C7 C 0.04384(8) 0.2484(3) 0.22277(16) 0.0496(8) Uani 1 1 d . . . C8 C 0.08314(7) 0.2280(2) 0.20069(13) 0.0448(7) Uani 1 1 d . . . C9 C 0.10537(7) 0.3470(2) 0.22194(11) 0.0364(6) Uani 1 1 d . . . C10 C 0.16949(7) 0.3092(3) 0.20356(12) 0.0407(7) Uani 1 1 d . . . C11 C 0.20865(7) 0.3519(2) 0.20551(11) 0.0373(6) Uani 1 1 d . . . C12 C 0.26993(9) 0.3190(3) 0.18108(14) 0.0532(8) Uani 1 1 d . . . C13 C 0.28489(9) 0.4298(3) 0.20312(13) 0.0521(8) Uani 1 1 d . . . C14 C 0.26028(8) 0.5048(3) 0.22933(12) 0.0448(7) Uani 1 1 d . . . C15 C 0.22275(8) 0.4661(2) 0.23097(11) 0.0382(7) Uani 1 1 d . . . C16 C 0.07518(13) 0.2242(4) 0.13370(17) 0.0682(10) Uani 1 1 d . . . C17 C 0.10241(12) 0.1085(3) 0.2269(2) 0.0713(11) Uani 1 1 d . . . K1 K 0.150376(17) 0.21315(5) 0.48177(2) 0.04405(19) Uani 1 1 d . . . O1 O 0.20922(6) 0.10694(19) 0.43019(9) 0.0631(6) Uani 1 1 d . . . O2 O 0.19006(6) 0.36075(18) 0.40972(8) 0.0592(5) Uani 1 1 d . . . O3 O 0.13938(5) 0.38757(18) 0.56629(8) 0.0585(5) Uani 1 1 d . . . O4 O 0.18194(5) 0.17218(19) 0.60145(8) 0.0597(5) Uani 1 1 d . . . O5 O 0.09946(6) 0.00738(19) 0.46722(12) 0.0845(8) Uani 1 1 d . . . O6 O 0.07440(6) 0.2333(2) 0.41217(10) 0.0770(7) Uani 1 1 d . . . N5 N 0.18206(8) -0.0372(2) 0.52048(13) 0.0667(7) Uani 1 1 d . . . N6 N 0.11809(7) 0.4611(2) 0.44313(11) 0.0566(6) Uani 1 1 d . . . C18 C 0.20625(11) -0.0832(3) 0.47874(18) 0.0872(12) Uani 1 1 d . . . H18A H 0.1886 -0.1156 0.4439 0.105 Uiso 1 1 calc R . . H18B H 0.2225 -0.1519 0.4972 0.105 Uiso 1 1 calc R . . C19 C 0.23259(10) 0.0106(3) 0.45954(17) 0.0776(10) Uani 1 1 d . . . H19A H 0.2508 0.0433 0.4938 0.093 Uiso 1 1 calc R . . H19B H 0.2483 -0.0272 0.4331 0.093 Uiso 1 1 calc R . . C20 C 0.23202(10) 0.1911(3) 0.40265(15) 0.0730(10) Uani 1 1 d . . . H20A H 0.2456 0.1461 0.3756 0.088 Uiso 1 1 calc R . . H20B H 0.2521 0.2305 0.4326 0.088 Uiso 1 1 calc R . . C21 C 0.20606(10) 0.2861(3) 0.36985(14) 0.0737(10) Uani 1 1 d . . . H21A H 0.2212 0.3373 0.3472 0.088 Uiso 1 1 calc R . . H21B H 0.1846 0.2465 0.3422 0.088 Uiso 1 1 calc R . . C22 C 0.16945(10) 0.4646(3) 0.38093(15) 0.0775(10) Uani 1 1 d . . . H22A H 0.1500 0.4369 0.3469 0.093 Uiso 1 1 calc R . . H22B H 0.1882 0.5197 0.3668 0.093 Uiso 1 1 calc R . . C23 C 0.14922(10) 0.5315(3) 0.42247(16) 0.0757(10) Uani 1 1 d . . . H23A H 0.1690 0.5563 0.4567 0.091 Uiso 1 1 calc R . . H23B H 0.1375 0.6069 0.4033 0.091 Uiso 1 1 calc R . . C24 C 0.10628(10) 0.5226(3) 0.49304(15) 0.0734(10) Uani 1 1 d . . . H24A H 0.0812 0.4872 0.4990 0.088 Uiso 1 1 calc R . . H24B H 0.1016 0.6099 0.4833 0.088 Uiso 1 1 calc R . . C25 C 0.13521(11) 0.5137(3) 0.54896(15) 0.0762(10) Uani 1 1 d . . . H25A H 0.1608 0.5467 0.5437 0.091 Uiso 1 1 calc R . . H25B H 0.1260 0.5621 0.5795 0.091 Uiso 1 1 calc R . . C26 C 0.16322(9) 0.3773(4) 0.62263(13) 0.0725(10) Uani 1 1 d . . . H26A H 0.1521 0.4275 0.6507 0.087 Uiso 1 1 calc R . . H26B H 0.1899 0.4077 0.6217 0.087 Uiso 1 1 calc R . . C27 C 0.16521(10) 0.2464(4) 0.64154(14) 0.0816(11) Uani 1 1 d . . . H27A H 0.1814 0.2395 0.6811 0.098 Uiso 1 1 calc R . . H27B H 0.1386 0.2167 0.6432 0.098 Uiso 1 1 calc R . . C28 C 0.18890(11) 0.0502(4) 0.62178(16) 0.0900(12) Uani 1 1 d . . . H28A H 0.1639 0.0123 0.6267 0.108 Uiso 1 1 calc R . . H28B H 0.2067 0.0507 0.6602 0.108 Uiso 1 1 calc R . . C29 C 0.20698(10) -0.0244(3) 0.57906(17) 0.0802(11) Uani 1 1 d . . . H29A H 0.2320 0.0142 0.5748 0.096 Uiso 1 1 calc R . . H29B H 0.2131 -0.1068 0.5956 0.096 Uiso 1 1 calc R . . C30 C 0.14884(11) -0.1194(3) 0.5225(2) 0.1098(16) Uani 1 1 d . . . H30A H 0.1382 -0.1010 0.5579 0.132 Uiso 1 1 calc R . . H30B H 0.1585 -0.2045 0.5257 0.132 Uiso 1 1 calc R . . C31 C 0.11644(12) -0.1100(3) 0.4706(3) 0.135(2) Uani 1 1 d . . . H31A H 0.1268 -0.1265 0.4348 0.162 Uiso 1 1 calc R . . H31B H 0.0962 -0.1720 0.4735 0.162 Uiso 1 1 calc R . . C32 C 0.06857(13) 0.0197(4) 0.4180(2) 0.131(2) Uani 1 1 d . . . H32A H 0.0495 -0.0473 0.4182 0.157 Uiso 1 1 calc R . . H32B H 0.0794 0.0123 0.3819 0.157 Uiso 1 1 calc R . . C33 C 0.04851(11) 0.1360(4) 0.4178(2) 0.1196(17) Uani 1 1 d . . . H33A H 0.0259 0.1383 0.3850 0.144 Uiso 1 1 calc R . . H33B H 0.0385 0.1454 0.4545 0.144 Uiso 1 1 calc R . . C34 C 0.05548(10) 0.3491(3) 0.40571(17) 0.0856(11) Uani 1 1 d . . . H34A H 0.0455 0.3693 0.4415 0.103 Uiso 1 1 calc R . . H34B H 0.0330 0.3466 0.3727 0.103 Uiso 1 1 calc R . . C35 C 0.08406(10) 0.4452(3) 0.39473(15) 0.0753(10) Uani 1 1 d . . . H35A H 0.0701 0.5241 0.3876 0.090 Uiso 1 1 calc R . . H35B H 0.0938 0.4236 0.3589 0.090 Uiso 1 1 calc R . . H10 H 0.1645(7) 0.231(2) 0.1868(11) 0.046(8) Uiso 1 1 d . . . H15 H 0.2058(6) 0.5147(19) 0.2496(9) 0.026(6) Uiso 1 1 d . . . H4 H 0.1358(6) 0.5959(19) 0.2475(9) 0.029(6) Uiso 1 1 d . . . H7B H 0.0455(7) 0.204(2) 0.2617(12) 0.044(7) Uiso 1 1 d . . . H1 H 0.0189(7) 0.750(2) 0.2956(10) 0.041(7) Uiso 1 1 d . . . H12 H 0.2848(7) 0.265(2) 0.1622(12) 0.050(8) Uiso 1 1 d . . . H3 H 0.1320(8) 0.802(2) 0.2809(12) 0.054(9) Uiso 1 1 d . . . H7A H 0.0196(8) 0.214(2) 0.1928(13) 0.069(9) Uiso 1 1 d . . . H13 H 0.3121(8) 0.458(2) 0.2005(11) 0.052(8) Uiso 1 1 d . . . H16C H 0.0989(10) 0.225(3) 0.1215(13) 0.071(11) Uiso 1 1 d . . . H14 H 0.2690(7) 0.583(3) 0.2466(12) 0.061(9) Uiso 1 1 d . . . H17C H 0.1260(11) 0.086(3) 0.2129(15) 0.096(12) Uiso 1 1 d . . . H17B H 0.1109(8) 0.122(3) 0.2722(15) 0.071(11) Uiso 1 1 d . . . H2 H 0.0723(7) 0.876(3) 0.3023(11) 0.054(8) Uiso 1 1 d . . . H16B H 0.0615(9) 0.146(3) 0.1192(14) 0.087(11) Uiso 1 1 d . . . H16A H 0.0610(11) 0.296(4) 0.1167(17) 0.107(15) Uiso 1 1 d . . . H17A H 0.0815(10) 0.043(3) 0.2182(15) 0.095(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0332(3) 0.0392(3) 0.0484(3) 0.000 0.0138(2) 0.000 N1 0.0407(13) 0.0331(13) 0.0418(13) -0.0012(10) 0.0126(10) 0.0008(10) N2 0.0363(13) 0.0363(13) 0.0502(14) -0.0025(10) 0.0135(10) -0.0034(10) N3 0.0327(13) 0.0430(13) 0.0386(13) 0.0042(10) 0.0091(10) -0.0005(10) N4 0.0419(14) 0.0462(14) 0.0586(16) -0.0036(11) 0.0182(11) 0.0015(11) C1 0.0463(18) 0.0462(19) 0.0522(19) -0.0038(14) 0.0185(14) 0.0028(15) C2 0.062(2) 0.0399(19) 0.061(2) -0.0096(15) 0.0176(16) -0.0042(16) C3 0.050(2) 0.046(2) 0.062(2) -0.0048(16) 0.0139(15) -0.0153(17) C4 0.0361(17) 0.050(2) 0.0392(17) 0.0025(14) 0.0095(13) -0.0020(14) C5 0.0328(15) 0.0393(16) 0.0333(15) 0.0041(12) 0.0071(11) -0.0020(12) C6 0.0345(15) 0.0367(16) 0.0353(15) 0.0034(12) 0.0099(11) -0.0021(12) C7 0.0412(17) 0.0352(18) 0.076(2) -0.0034(17) 0.0210(16) -0.0008(13) C8 0.0374(15) 0.0391(16) 0.060(2) -0.0026(14) 0.0161(13) 0.0008(13) C9 0.0366(15) 0.0374(16) 0.0365(16) 0.0016(12) 0.0099(11) -0.0006(12) C10 0.0360(16) 0.0416(18) 0.0460(17) -0.0029(14) 0.0118(12) 0.0001(14) C11 0.0384(16) 0.0379(16) 0.0361(16) 0.0041(13) 0.0086(12) 0.0059(13) C12 0.0413(19) 0.059(2) 0.063(2) 0.0010(17) 0.0183(15) 0.0078(17) C13 0.0325(17) 0.060(2) 0.064(2) 0.0102(17) 0.0100(15) -0.0006(15) C14 0.0405(17) 0.0470(19) 0.0429(17) 0.0077(15) -0.0025(13) -0.0015(15) C15 0.0392(17) 0.0417(18) 0.0338(16) 0.0036(13) 0.0074(12) 0.0065(14) C16 0.059(2) 0.079(3) 0.070(3) -0.024(2) 0.019(2) -0.015(2) C17 0.054(2) 0.045(2) 0.121(4) 0.011(2) 0.032(2) 0.0045(18) K1 0.0539(4) 0.0393(4) 0.0383(4) 0.0011(3) 0.0071(3) -0.0007(3) O1 0.0600(13) 0.0613(14) 0.0713(15) -0.0053(11) 0.0211(11) 0.0061(11) O2 0.0760(14) 0.0635(14) 0.0406(12) 0.0103(10) 0.0178(10) 0.0012(11) O3 0.0665(13) 0.0682(15) 0.0383(12) -0.0109(10) 0.0035(10) 0.0031(11) O4 0.0656(13) 0.0764(15) 0.0385(12) 0.0179(11) 0.0129(10) 0.0082(11) O5 0.0719(15) 0.0444(14) 0.127(2) 0.0047(13) -0.0068(14) -0.0078(11) O6 0.0682(14) 0.0644(15) 0.0888(18) 0.0059(12) -0.0095(12) -0.0023(13) N5 0.0664(17) 0.0411(15) 0.090(2) 0.0159(14) 0.0068(16) 0.0033(13) N6 0.0695(17) 0.0475(15) 0.0504(16) 0.0092(12) 0.0053(13) 0.0065(13) C18 0.092(3) 0.049(2) 0.113(3) -0.002(2) 0.001(2) 0.018(2) C19 0.065(2) 0.076(3) 0.093(3) -0.016(2) 0.0186(19) 0.017(2) C20 0.067(2) 0.089(3) 0.072(2) -0.022(2) 0.0341(18) -0.009(2) C21 0.084(2) 0.095(3) 0.048(2) 0.000(2) 0.0276(18) -0.007(2) C22 0.091(3) 0.075(2) 0.066(2) 0.034(2) 0.013(2) -0.002(2) C23 0.096(3) 0.053(2) 0.078(3) 0.0205(19) 0.014(2) 0.0041(19) C24 0.090(3) 0.048(2) 0.080(3) -0.0013(18) 0.012(2) 0.0192(18) C25 0.100(3) 0.052(2) 0.077(3) -0.0192(18) 0.020(2) 0.0047(19) C26 0.069(2) 0.107(3) 0.040(2) -0.021(2) 0.0066(16) 0.015(2) C27 0.072(2) 0.146(4) 0.0282(18) 0.005(2) 0.0135(15) 0.026(2) C28 0.097(3) 0.109(3) 0.063(3) 0.044(2) 0.015(2) 0.016(2) C29 0.081(2) 0.063(2) 0.093(3) 0.040(2) 0.008(2) 0.0217(19) C30 0.081(3) 0.049(2) 0.191(5) 0.050(3) 0.003(3) -0.007(2) C31 0.090(3) 0.042(2) 0.253(6) -0.003(3) -0.020(4) -0.016(2) C32 0.105(3) 0.080(3) 0.179(5) -0.018(3) -0.044(3) -0.025(3) C33 0.072(3) 0.086(3) 0.177(5) 0.028(3) -0.037(3) -0.019(3) C34 0.075(2) 0.083(3) 0.087(3) 0.013(2) -0.017(2) 0.010(2) C35 0.084(2) 0.070(2) 0.064(2) 0.0193(18) -0.0052(19) 0.015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 1.909(2) 2 ? Ni1 N2 1.909(2) . ? Ni1 N1 1.930(2) . ? Ni1 N1 1.930(2) 2 ? N1 C1 1.359(3) . ? N1 C5 1.395(3) . ? N2 C6 1.353(3) . ? N2 C7 1.475(3) . ? N3 C9 1.325(3) . ? N3 C10 1.336(3) . ? N4 C12 1.337(3) . ? N4 C11 1.368(3) . ? C1 C2 1.354(4) . ? C2 C3 1.400(4) . ? C3 C4 1.373(4) . ? C4 C5 1.397(3) . ? C5 C6 1.430(3) . ? C6 C9 1.429(3) . ? C7 C8 1.551(4) . ? C8 C9 1.534(3) . ? C8 C16 1.523(5) . ? C8 C17 1.529(4) . ? C10 C11 1.419(3) . ? C11 C15 1.419(3) . ? C12 C13 1.368(4) . ? C13 C14 1.394(4) . ? C14 C15 1.367(4) . ? K1 O1 2.790(2) . ? K1 O3 2.799(2) . ? K1 O4 2.8132(19) . ? K1 O5 2.820(2) . ? K1 O6 2.811(2) . ? K1 O2 2.842(2) . ? K1 N6 2.983(2) . ? K1 N5 3.001(3) . ? O1 C19 1.413(4) . ? O1 C20 1.431(4) . ? O2 C21 1.415(4) . ? O2 C22 1.428(3) . ? O3 C26 1.408(3) . ? O3 C25 1.426(4) . ? O4 C27 1.430(4) . ? O4 C28 1.411(4) . ? O5 C31 1.398(4) . ? O5 C32 1.411(4) . ? O6 C34 1.411(4) . ? O6 C33 1.404(4) . ? N5 C30 1.458(4) . ? N5 C18 1.477(4) . ? N5 C29 1.468(4) . ? N6 C24 1.457(4) . ? N6 C23 1.469(4) . ? N6 C35 1.471(4) . ? C18 C19 1.487(5) . ? C20 C21 1.478(4) . ? C22 C23 1.480(5) . ? C24 C25 1.480(4) . ? C26 C27 1.484(5) . ? C28 C29 1.501(5) . ? C30 C31 1.480(5) . ? C32 C33 1.439(5) . ? C34 C35 1.489(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 N2 Ni1 N2 105.53(12) 2 . ? N2 Ni1 N1 154.40(8) 2 . ? N2 Ni1 N1 81.88(9) . . ? N2 Ni1 N1 81.88(9) 2 2 ? N2 Ni1 N1 154.40(8) . 2 ? N1 Ni1 N1 102.13(12) . 2 ? C1 N1 C5 115.8(2) . . ? C1 N1 Ni1 128.90(18) . . ? C5 N1 Ni1 114.90(16) . . ? C6 N2 C7 106.4(2) . . ? C6 N2 Ni1 116.36(16) . . ? C7 N2 Ni1 135.63(17) . . ? C9 N3 C10 125.3(2) . . ? C12 N4 C11 117.7(2) . . ? C2 C1 N1 124.7(3) . . ? C1 C2 C3 119.4(3) . . ? C4 C3 C2 118.3(3) . . ? C5 C4 C3 120.2(3) . . ? C4 C5 N1 121.5(2) . . ? C4 C5 C6 126.3(2) . . ? N1 C5 C6 112.2(2) . . ? N2 C6 C5 114.2(2) . . ? N2 C6 C9 114.4(2) . . ? C5 C6 C9 131.4(2) . . ? N2 C7 C8 106.9(2) . . ? C9 C8 C16 109.4(2) . . ? C9 C8 C17 115.7(2) . . ? C16 C8 C17 111.2(3) . . ? C9 C8 C7 100.9(2) . . ? C16 C8 C7 109.8(3) . . ? C17 C8 C7 109.3(3) . . ? N3 C9 C6 123.1(2) . . ? N3 C9 C8 130.4(2) . . ? C6 C9 C8 106.21(19) . . ? N3 C10 C11 121.4(3) . . ? N4 C11 C10 117.3(2) . . ? N4 C11 C15 119.6(2) . . ? C10 C11 C15 123.2(2) . . ? N4 C12 C13 125.6(3) . . ? C12 C13 C14 117.3(3) . . ? C15 C14 C13 119.3(3) . . ? C14 C15 C11 120.5(3) . . ? O1 K1 O3 141.63(6) . . ? O1 K1 O4 100.32(6) . . ? O3 K1 O4 59.80(6) . . ? O1 K1 O5 96.20(7) . . ? O3 K1 O5 117.10(7) . . ? O4 K1 O5 96.22(7) . . ? O1 K1 O6 117.43(7) . . ? O3 K1 O6 96.51(6) . . ? O4 K1 O6 136.16(7) . . ? O5 K1 O6 60.15(7) . . ? O1 K1 O2 60.82(7) . . ? O3 K1 O2 99.94(7) . . ? O4 K1 O2 121.83(6) . . ? O5 K1 O2 137.19(7) . . ? O6 K1 O2 96.86(6) . . ? O1 K1 N6 120.29(7) . . ? O3 K1 N6 60.49(7) . . ? O4 K1 N6 119.37(7) . . ? O5 K1 N6 119.34(7) . . ? O6 K1 N6 60.26(7) . . ? O2 K1 N6 60.62(7) . . ? O1 K1 N5 60.06(7) . . ? O3 K1 N5 119.56(8) . . ? O4 K1 N5 60.78(7) . . ? O5 K1 N5 60.12(7) . . ? O6 K1 N5 119.23(7) . . ? O2 K1 N5 119.81(7) . . ? N6 K1 N5 179.45(7) . . ? C19 O1 C20 112.1(2) . . ? C19 O1 K1 119.62(19) . . ? C20 O1 K1 115.59(17) . . ? C21 O2 C22 111.6(2) . . ? C21 O2 K1 110.48(18) . . ? C22 O2 K1 117.80(18) . . ? C26 O3 C25 110.3(2) . . ? C26 O3 K1 117.47(17) . . ? C25 O3 K1 118.19(17) . . ? C27 O4 C28 112.1(3) . . ? C27 O4 K1 114.94(17) . . ? C28 O4 K1 119.11(19) . . ? C31 O5 C32 112.1(3) . . ? C31 O5 K1 118.1(2) . . ? C32 O5 K1 112.3(2) . . ? C34 O6 C33 113.0(3) . . ? C34 O6 K1 119.44(18) . . ? C33 O6 K1 115.33(19) . . ? C30 N5 C18 110.9(3) . . ? C30 N5 C29 110.8(3) . . ? C18 N5 C29 109.4(3) . . ? C30 N5 K1 108.62(18) . . ? C18 N5 K1 109.22(19) . . ? C29 N5 K1 107.82(18) . . ? C24 N6 C23 110.5(2) . . ? C24 N6 C35 110.8(3) . . ? C23 N6 C35 109.8(3) . . ? C24 N6 K1 108.66(17) . . ? C23 N6 K1 108.25(17) . . ? C35 N6 K1 108.73(17) . . ? N5 C18 C19 114.6(3) . . ? O1 C19 C18 109.0(3) . . ? O1 C20 C21 110.1(3) . . ? O2 C21 C20 109.7(3) . . ? O2 C22 C23 109.8(3) . . ? N6 C23 C22 114.7(3) . . ? N6 C24 C25 114.9(3) . . ? O3 C25 C24 108.9(2) . . ? O3 C26 C27 109.6(3) . . ? O4 C27 C26 110.5(3) . . ? O4 C28 C29 110.6(3) . . ? N5 C29 C28 114.6(3) . . ? N5 C30 C31 114.1(3) . . ? O5 C31 C30 110.6(3) . . ? O5 C32 C33 112.0(3) . . ? O6 C33 C32 110.3(4) . . ? O6 C34 C35 109.6(3) . . ? C34 C35 N6 114.2(3) . . ? _iucr_refine_instructions_details ; TITL vw17 in C2/c CELL 0.71073 34.4600 10.8519 23.1441 90.000 100.903 90.000 ZERR 4.00 0.0067 0.0047 0.0043 0.000 0.004 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O K NI UNIT 280 424 48 48 8 4 TEMP -30 SIZE 0.03 0.10 0.20 L.S. 8 ACTA WPDB SHEL 100 .9 WGHT 0.054900 FVAR 0.49849 NI1 6 0.000000 0.488808 0.250000 10.50000 0.03317 0.03916 = 0.04838 0.00000 0.01384 0.00000 N1 3 0.044201 0.600552 0.267867 11.00000 0.04069 0.03308 = 0.04181 -0.00124 0.01255 0.00078 N2 3 0.039727 0.382336 0.230521 11.00000 0.03633 0.03626 = 0.05016 -0.00253 0.01346 -0.00340 N3 3 0.142593 0.378850 0.222810 11.00000 0.03267 0.04304 = 0.03856 0.00420 0.00911 -0.00051 N4 3 0.233385 0.277760 0.181169 11.00000 0.04195 0.04616 = 0.05865 -0.00356 0.01819 0.00146 C1 1 0.044791 0.719345 0.286629 11.00000 0.04634 0.04621 = 0.05217 -0.00379 0.01845 0.00278 C2 1 0.076388 0.795435 0.291589 11.00000 0.06225 0.03985 = 0.06065 -0.00965 0.01759 -0.00419 C3 1 0.111485 0.751913 0.276745 11.00000 0.05040 0.04611 = 0.06152 -0.00478 0.01385 -0.01534 C4 1 0.112659 0.632091 0.258139 11.00000 0.03613 0.05042 = 0.03917 0.00247 0.00953 -0.00200 C5 1 0.079296 0.557026 0.253583 11.00000 0.03284 0.03934 = 0.03331 0.00414 0.00714 -0.00198 C6 1 0.076436 0.430648 0.235779 11.00000 0.03452 0.03669 = 0.03530 0.00340 0.00986 -0.00207 C7 1 0.043836 0.248374 0.222767 11.00000 0.04120 0.03516 = 0.07635 -0.00344 0.02100 -0.00085 C8 1 0.083138 0.227995 0.200687 11.00000 0.03743 0.03911 = 0.06044 -0.00261 0.01615 0.00078 C9 1 0.105375 0.346990 0.221940 11.00000 0.03655 0.03742 = 0.03651 0.00159 0.00987 -0.00062 C10 1 0.169485 0.309248 0.203563 11.00000 0.03599 0.04157 = 0.04598 -0.00287 0.01176 0.00008 C11 1 0.208652 0.351869 0.205511 11.00000 0.03843 0.03787 = 0.03612 0.00412 0.00858 0.00591 C12 1 0.269934 0.319016 0.181079 11.00000 0.04134 0.05859 = 0.06310 0.00103 0.01829 0.00776 C13 1 0.284887 0.429796 0.203119 11.00000 0.03248 0.05955 = 0.06447 0.01016 0.01004 -0.00063 C14 1 0.260279 0.504809 0.229330 11.00000 0.04046 0.04699 = 0.04290 0.00769 -0.00249 -0.00151 C15 1 0.222748 0.466123 0.230975 11.00000 0.03917 0.04175 = 0.03385 0.00355 0.00742 0.00646 C16 1 0.075175 0.224157 0.133697 11.00000 0.05901 0.07851 = 0.06960 -0.02437 0.01884 -0.01545 C17 1 0.102415 0.108549 0.226916 11.00000 0.05361 0.04503 = 0.12112 0.01051 0.03173 0.00445 K1 5 0.150376 0.213147 0.481765 11.00000 0.05394 0.03931 = 0.03826 0.00107 0.00713 -0.00067 O1 4 0.209223 0.106941 0.430186 11.00000 0.06001 0.06132 = 0.07126 -0.00529 0.02110 0.00610 O2 4 0.190064 0.360754 0.409715 11.00000 0.07602 0.06355 = 0.04063 0.01029 0.01776 0.00119 O3 4 0.139382 0.387569 0.566288 11.00000 0.06653 0.06820 = 0.03828 -0.01095 0.00352 0.00312 O4 4 0.181941 0.172180 0.601450 11.00000 0.06558 0.07638 = 0.03847 0.01791 0.01290 0.00822 O5 4 0.099463 0.007381 0.467221 11.00000 0.07193 0.04444 = 0.12708 0.00466 -0.00676 -0.00784 O6 4 0.074396 0.233286 0.412168 11.00000 0.06816 0.06435 = 0.08883 0.00590 -0.00948 -0.00225 N5 3 0.182061 -0.037234 0.520481 11.00000 0.06638 0.04110 = 0.08962 0.01592 0.00675 0.00330 N6 3 0.118093 0.461060 0.443131 11.00000 0.06953 0.04751 = 0.05039 0.00918 0.00530 0.00646 C18 1 0.206254 -0.083237 0.478738 11.00000 0.09188 0.04911 = 0.11342 -0.00209 0.00093 0.01838 AFIX 23 H18A 2 0.188552 -0.115575 0.443866 11.00000 -1.20000 H18B 2 0.222518 -0.151874 0.497168 11.00000 -1.20000 AFIX 0 C19 1 0.232594 0.010560 0.459545 11.00000 0.06525 0.07629 = 0.09276 -0.01573 0.01858 0.01719 AFIX 23 H19A 2 0.250798 0.043303 0.493807 11.00000 -1.20000 H19B 2 0.248255 -0.027227 0.433056 11.00000 -1.20000 AFIX 0 C20 1 0.232023 0.191081 0.402655 11.00000 0.06722 0.08851 = 0.07160 -0.02204 0.03411 -0.00930 AFIX 23 H20A 2 0.245635 0.146114 0.375629 11.00000 -1.20000 H20B 2 0.252056 0.230529 0.432647 11.00000 -1.20000 AFIX 0 C21 1 0.206057 0.286123 0.369849 11.00000 0.08425 0.09458 = 0.04825 -0.00044 0.02755 -0.00655 AFIX 23 H21A 2 0.221239 0.337284 0.347201 11.00000 -1.20000 H21B 2 0.184617 0.246526 0.342232 11.00000 -1.20000 AFIX 0 C22 1 0.169454 0.464577 0.380934 11.00000 0.09107 0.07497 = 0.06578 0.03362 0.01313 -0.00185 AFIX 23 H22A 2 0.149986 0.436882 0.346918 11.00000 -1.20000 H22B 2 0.188153 0.519724 0.366784 11.00000 -1.20000 AFIX 0 C23 1 0.149225 0.531549 0.422469 11.00000 0.09611 0.05254 = 0.07753 0.02053 0.01402 0.00412 AFIX 23 H23A 2 0.169006 0.556322 0.456704 11.00000 -1.20000 H23B 2 0.137523 0.606860 0.403258 11.00000 -1.20000 AFIX 0 C24 1 0.106279 0.522597 0.493042 11.00000 0.09047 0.04817 = 0.08000 -0.00125 0.01191 0.01922 AFIX 23 H24A 2 0.081172 0.487177 0.498997 11.00000 -1.20000 H24B 2 0.101629 0.609889 0.483279 11.00000 -1.20000 AFIX 0 C25 1 0.135207 0.513737 0.548955 11.00000 0.10023 0.05249 = 0.07695 -0.01922 0.01960 0.00475 AFIX 23 H25A 2 0.160782 0.546737 0.543693 11.00000 -1.20000 H25B 2 0.126038 0.562127 0.579516 11.00000 -1.20000 AFIX 0 C26 1 0.163223 0.377289 0.622630 11.00000 0.06890 0.10706 = 0.04016 -0.02122 0.00656 0.01465 AFIX 23 H26A 2 0.152112 0.427460 0.650737 11.00000 -1.20000 H26B 2 0.189871 0.407735 0.621698 11.00000 -1.20000 AFIX 0 C27 1 0.165212 0.246435 0.641541 11.00000 0.07217 0.14611 = 0.02819 0.00472 0.01353 0.02617 AFIX 23 H27A 2 0.181391 0.239549 0.681069 11.00000 -1.20000 H27B 2 0.138583 0.216728 0.643158 11.00000 -1.20000 AFIX 0 C28 1 0.188896 0.050160 0.621784 11.00000 0.09727 0.10917 = 0.06342 0.04377 0.01470 0.01565 AFIX 23 H28A 2 0.163901 0.012340 0.626705 11.00000 -1.20000 H28B 2 0.206701 0.050741 0.660194 11.00000 -1.20000 AFIX 0 C29 1 0.206980 -0.024393 0.579056 11.00000 0.08113 0.06303 = 0.09308 0.03983 0.00806 0.02166 AFIX 23 H29A 2 0.231994 0.014177 0.574769 11.00000 -1.20000 H29B 2 0.213073 -0.106810 0.595613 11.00000 -1.20000 AFIX 0 C30 1 0.148839 -0.119378 0.522453 11.00000 0.08056 0.04863 = 0.19142 0.04995 0.00325 -0.00739 AFIX 23 H30A 2 0.138232 -0.100970 0.557910 11.00000 -1.20000 H30B 2 0.158511 -0.204492 0.525716 11.00000 -1.20000 AFIX 0 C31 1 0.116437 -0.109985 0.470631 11.00000 0.08969 0.04220 = 0.25289 -0.00280 -0.01995 -0.01571 AFIX 23 H31A 2 0.126791 -0.126479 0.434766 11.00000 -1.20000 H31B 2 0.096220 -0.171985 0.473549 11.00000 -1.20000 AFIX 0 C32 1 0.068571 0.019688 0.417985 11.00000 0.10512 0.08049 = 0.17940 -0.01806 -0.04389 -0.02511 AFIX 23 H32A 2 0.049530 -0.047304 0.418211 11.00000 -1.20000 H32B 2 0.079414 0.012313 0.381927 11.00000 -1.20000 AFIX 0 C33 1 0.048511 0.136011 0.417777 11.00000 0.07202 0.08593 = 0.17737 0.02754 -0.03655 -0.01904 AFIX 23 H33A 2 0.025907 0.138261 0.384960 11.00000 -1.20000 H33B 2 0.038528 0.145389 0.454469 11.00000 -1.20000 AFIX 0 C34 1 0.055480 0.349150 0.405713 11.00000 0.07451 0.08297 = 0.08670 0.01348 -0.01676 0.01004 AFIX 23 H34A 2 0.045484 0.369258 0.441504 11.00000 -1.20000 H34B 2 0.033001 0.346554 0.372712 11.00000 -1.20000 AFIX 0 C35 1 0.084064 0.445197 0.394734 11.00000 0.08368 0.07013 = 0.06442 0.01931 -0.00525 0.01514 AFIX 23 H35A 2 0.070116 0.524052 0.387631 11.00000 -1.20000 H35B 2 0.093815 0.423593 0.358918 11.00000 -1.20000 AFIX 0 H10 2 0.164484 0.231370 0.186809 11.00000 0.04565 H15 2 0.205785 0.514728 0.249614 11.00000 0.02554 H4 2 0.135820 0.595866 0.247470 11.00000 0.02939 H7B 2 0.045468 0.204070 0.261735 11.00000 0.04378 H1 2 0.018907 0.749945 0.295632 11.00000 0.04145 H12 2 0.284787 0.264938 0.162233 11.00000 0.05017 H3 2 0.131984 0.802131 0.280921 11.00000 0.05412 H7A 2 0.019586 0.213995 0.192805 11.00000 0.06898 H13 2 0.312088 0.457977 0.200466 11.00000 0.05172 H16C 2 0.098904 0.224899 0.121462 11.00000 0.07102 H14 2 0.268998 0.583213 0.246597 11.00000 0.06070 H17C 2 0.126027 0.085580 0.212858 11.00000 0.09649 H17B 2 0.110935 0.121529 0.272195 11.00000 0.07138 H2 2 0.072252 0.876375 0.302264 11.00000 0.05365 H16B 2 0.061510 0.145698 0.119239 11.00000 0.08672 H16A 2 0.061025 0.295738 0.116696 11.00000 0.10686 H17A 2 0.081454 0.043246 0.218229 11.00000 0.09512 HKLF 4 REM vw17 in C2/c REM R1 = 0.0413 for 4267 Fo > 4sig(Fo) and 0.0676 for all 6091 data REM 506 parameters refined using 0 restraints END WGHT 0.0527 0.0000 REM Highest difference peak 0.202, deepest hole -0.214, 1-sigma level 0.040 Q1 1 0.0964 0.1830 0.3835 11.00000 0.05 0.20 Q2 1 -0.0192 -0.1603 0.4215 11.00000 0.05 0.20 Q3 1 -0.0143 0.3075 0.5228 11.00000 0.05 0.18 Q4 1 0.0179 0.4128 0.2363 11.00000 0.05 0.17 Q5 1 0.0086 0.2622 0.5171 11.00000 0.05 0.17 Q6 1 0.0674 0.0527 0.4720 11.00000 0.05 0.17 Q7 1 0.0070 0.3718 0.5459 11.00000 0.05 0.17 Q8 1 0.0336 0.4379 0.2979 11.00000 0.05 0.17 Q9 1 0.0710 0.1153 0.3823 11.00000 0.05 0.16 Q10 1 0.0005 0.5861 0.4488 11.00000 0.05 0.16 Q11 1 -0.0086 0.5428 0.4393 11.00000 0.05 0.16 Q12 1 0.0106 0.3759 0.2693 11.00000 0.05 0.15 Q13 1 0.1455 0.1630 0.6293 11.00000 0.05 0.15 Q14 1 0.0175 0.5742 0.4672 11.00000 0.05 0.15 Q15 1 0.0362 0.3279 0.2293 11.00000 0.05 0.14 Q16 1 0.0252 0.5695 0.2317 11.00000 0.05 0.14 Q17 1 0.0080 0.6640 0.4029 11.00000 0.05 0.14 Q18 1 0.0867 0.3632 0.3740 11.00000 0.05 0.14 Q19 1 0.0315 0.5589 0.2898 11.00000 0.05 0.14 Q20 1 0.1633 0.1613 0.4273 11.00000 0.05 0.14 ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.202 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.040 _database_code_depnum_ccdc_archive 'CCDC 921479'