Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Ding, Y.' 'Simonyan, M.' 'Uruichi, M.' 'Yakushi, Kyuya' 'Yonehara, Y.' _publ_contact_author_name 'Prof Kyuya Yakushi' _publ_contact_author_address ; Prof Kyuya Yakushi Institute for Molecular Science Graduate University of Advanced Studies Myodaiji Okazaki 444-8585 JAPAN ; _publ_contact_author_email 'yakushi@ims.ac.jp' data_co1ni1 _database_code_CSD 156502 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Nov 19 13:02:53 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1331.59 _chemical_formula_analytical ? _chemical_formula_sum 'C64 H32 As Co0.90 F6 N16 Ni1.10 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 14.226(2) _cell_length_b 14.226(2) _cell_length_c 6.414(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1298.0699 _cell_formula_units_Z 1 _cell_measurement_temperature 288.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 4/m c c ' _symmetry_Int_Tables_number 124 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, +z' ' -y, +x, +z' ' +y, -x, +z' ' -x, +y,1/2+z' ' +x, -y,1/2+z' ' +y, +x,1/2+z' ' -y, -x,1/2+z' ' -x, -y, -z' ' +x, +y, -z' ' +y, -x, -z' ' -y, +x, -z' ' +x, -y,1/2-z' ' -x, +y,1/2-z' ' -y, -x,1/2-z' ' +y, +x,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 670.10 _exptl_absorpt_coefficient_mu 1.405 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 288.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 1113 _reflns_number_total 664 _reflns_number_observed 436 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 6.35 _diffrn_reflns_av_sigmaI/netI 0.099 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 64 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 32 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 16 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Co 0 0 0.349 0.972 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ni 0 1 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; As 0 1 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 6 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags As1 0.0000 0.0000 0.0000 0.222(3) Uani d . 0.06 S Ni1 0.5000 0.5000 0.0000 0.0423(6) Uani d . 0.07 S Co1 0.5000 0.5000 0.0000 0.0440(7) Uani d . 0.06 S F1 -0.0582 0.0865 -0.1531 0.1454 Uani d . 0.12 . F2 0.1194 0.0501 0.0000 0.16(1) Uani d . 0.12 S F3 -0.0430 0.0430 0.2500 0.2234 Uani d . 0.12 . N1 0.3791(4) 0.4446(4) 0.0000 0.044(2) Uani d . 0.50 S N2 0.2769(4) 0.5821(4) 0.0000 0.047(2) Uani d . 0.50 S C1 0.3571(5) 0.3490(5) 0.0000 0.045(2) Uani d . 0.50 S C2 0.2557(5) 0.3339(5) 0.0000 0.046(2) Uani d . 0.50 S C3 0.2007(6) 0.2539(5) 0.0000 0.057(2) Uani d . 0.50 S C4 0.1045(5) 0.2646(6) 0.0000 0.068(3) Uani d . 0.50 S C5 0.0626(5) 0.3540(6) 0.0000 0.071(3) Uani d . 0.50 S C6 0.1184(5) 0.4341(6) 0.0000 0.062(2) Uani d . 0.50 S C7 0.2154(5) 0.4227(5) 0.0000 0.049(2) Uani d . 0.50 S C8 0.2929(5) 0.4904(5) 0.0000 0.049(2) Uani d . 0.50 S H3 0.2283 0.1903 0.0000 0.0681 Uiso calc . 0.50 . H4 0.0638 0.2090 0.0000 0.0857 Uiso calc . 0.50 . H5 -0.0096 0.3638 0.0000 0.0791 Uiso calc . 0.50 . H6 0.0937 0.5013 0.0000 0.0794 Uiso calc . 0.50 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As(1) 0.072(2) 0.0717 0.52(1) 0.0000 0.0000 0.0000 Ni(1) 0.041(1) 0.0413 0.044(2) 0.0000 0.0000 0.0000 Co(1) 0.045(2) 0.0447 0.043(3) 0.0000 0.0000 0.0000 F(1) 0.1454 0.1454 0.1454 0.0000 0.0000 0.0000 F(2) 0.12(2) 0.03(1) 0.33(4) 0.00(1) 0.0000 0.0000 F(3) 0.1560 0.1560 0.3582 0.1366 -0.1047 -0.1047 N(1) 0.045(4) 0.048(4) 0.040(3) 0.002(3) 0.0000 0.0000 N(2) 0.044(4) 0.054(4) 0.043(3) 0.004(3) 0.0000 0.0000 C(1) 0.053(4) 0.048(4) 0.033(3) -0.001(3) 0.0000 0.0000 C(2) 0.047(4) 0.053(4) 0.038(3) -0.005(3) 0.0000 0.0000 C(3) 0.065(5) 0.052(4) 0.055(4) -0.006(4) 0.0000 0.0000 C(4) 0.053(5) 0.064(6) 0.087(5) -0.012(4) 0.0000 0.0000 C(5) 0.040(5) 0.086(6) 0.088(5) -0.007(4) 0.0000 0.0000 C(6) 0.053(5) 0.071(5) 0.061(4) -0.002(4) 0.0000 0.0000 C(7) 0.049(4) 0.060(5) 0.038(3) -0.003(4) 0.0000 0.0000 C(8) 0.055(4) 0.053(4) 0.038(3) 0.006(4) 0.0000 0.0000 #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.041(3) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 436 _refine_ls_number_parameters 72 _refine_ls_number_restraints 0 _refine_ls_number_constraints 6 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0701 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0727 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.138 _refine_ls_shift/esd_max 0.0343 _refine_ls_shift/esd_mean 0.0064 _refine_diff_density_min -0.68 _refine_diff_density_max 0.67 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) F(1) 1.7789(1) 1_555 1_555 yes As(1) F(1) 1.7789(1) 1_555 2_555 yes As(1) F(1) 1.7789(1) 1_555 3_555 yes As(1) F(1) 1.7789(1) 1_555 4_555 yes As(1) F(1) 1.7789(1) 1_555 9_555 yes As(1) F(1) 1.7789(1) 1_555 10_555 yes As(1) F(1) 1.7789(1) 1_555 11_555 yes As(1) F(1) 1.7789(1) 1_555 12_555 yes As(1) F(2) 1.8422(2) 1_555 1_555 yes As(1) F(2) 1.8422(2) 1_555 2_555 yes As(1) F(2) 1.842 1_555 3_555 yes As(1) F(2) 1.842 1_555 4_555 yes As(1) F(3) 1.822 1_555 1_555 yes As(1) F(3) 1.822 1_555 2_555 yes As(1) F(3) 1.822 1_555 3_555 yes As(1) F(3) 1.822 1_555 4_555 yes As(1) F(3) 1.822 1_555 5_554 yes As(1) F(3) 1.822 1_555 6_554 yes As(1) F(3) 1.822 1_555 7_554 yes As(1) F(3) 1.822 1_555 8_554 yes Ni(1) N(1) 1.892(5) 1_555 1_555 yes Ni(1) N(1) 1.892(5) 1_555 4_565 yes Ni(1) N(1) 1.892(5) 1_555 3_655 yes Ni(1) N(1) 1.892(5) 1_555 2_665 yes Co(1) N(1) 1.892(5) 1_555 1_555 yes Co(1) N(1) 1.892(5) 1_555 4_565 yes Co(1) N(1) 1.892(5) 1_555 3_655 yes Co(1) N(1) 1.892(5) 1_555 2_665 yes F(1) F(1) 1.366 1_555 15_554 yes F(1) F(2) 1.095 1_555 3_555 yes F(1) F(3) 1.6860(2) 1_555 5_554 yes F(1) F(3) 0.903 1_555 8_554 yes F(3) F(3) 1.223 1_555 3_555 yes F(3) F(3) 1.2233(2) 1_555 4_555 yes N(1) C(1) 1.394(8) 1_555 1_555 yes N(1) C(8) 1.389(8) 1_555 1_555 yes N(2) C(1) 1.341(9) 1_555 4_565 yes N(2) C(8) 1.324(9) 1_555 1_555 yes C(1) C(2) 1.458(10) 1_555 1_555 yes C(2) C(3) 1.382(10) 1_555 1_555 yes C(2) C(7) 1.387(10) 1_555 1_555 yes C(3) C(4) 1.38(1) 1_555 1_555 yes C(4) C(5) 1.40(1) 1_555 1_555 yes C(5) C(6) 1.39(1) 1_555 1_555 yes C(6) C(7) 1.390(10) 1_555 1_555 yes C(7) C(8) 1.464(10) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F(1) As(1) F(1) 112.966(2) 1_555 1_555 2_555 yes F(1) As(1) F(1) 72.248(4) 1_555 1_555 3_555 yes F(1) As(1) F(1) 72.248(7) 1_555 1_555 4_555 yes F(1) As(1) F(1) 180.0 1_555 1_555 9_555 yes F(1) As(1) F(1) 67.034(2) 1_555 1_555 10_555 yes F(1) As(1) F(1) 107.752(4) 1_555 1_555 11_555 yes F(1) As(1) F(1) 107.752(7) 1_555 1_555 12_555 yes F(1) As(1) F(2) 99.340(6) 1_555 1_555 1_555 yes F(1) As(1) F(2) 80.660(6) 1_555 1_555 2_555 yes F(1) As(1) F(2) 35.1374(8) 1_555 1_555 3_555 yes F(1) As(1) F(2) 144.8626(8) 1_555 1_555 4_555 yes F(1) As(1) F(3) 95.596(3) 1_555 1_555 1_555 yes F(1) As(1) F(3) 150.9822(4) 1_555 1_555 2_555 yes F(1) As(1) F(3) 124.178(5) 1_555 1_555 3_555 yes F(1) As(1) F(3) 114.218(2) 1_555 1_555 4_555 yes F(1) As(1) F(3) 55.822(5) 1_555 1_555 5_554 yes F(1) As(1) F(3) 65.782(2) 1_555 1_555 6_554 yes F(1) As(1) F(3) 84.404(3) 1_555 1_555 7_554 yes F(1) As(1) F(3) 29.0178(4) 1_555 1_555 8_554 yes F(1) As(1) F(1) 72.248(7) 2_555 1_555 3_555 yes F(1) As(1) F(1) 72.248(4) 2_555 1_555 4_555 yes F(1) As(1) F(1) 67.034(2) 2_555 1_555 9_555 yes F(1) As(1) F(1) 180.0 2_555 1_555 10_555 yes F(1) As(1) F(1) 107.752(7) 2_555 1_555 11_555 yes F(1) As(1) F(1) 107.752(4) 2_555 1_555 12_555 yes F(1) As(1) F(2) 80.660(6) 2_555 1_555 1_555 yes F(1) As(1) F(2) 99.340(6) 2_555 1_555 2_555 yes F(1) As(1) F(2) 144.8626(8) 2_555 1_555 3_555 yes F(1) As(1) F(2) 35.1374(8) 2_555 1_555 4_555 yes F(1) As(1) F(3) 150.9822(4) 2_555 1_555 1_555 yes F(1) As(1) F(3) 95.596(3) 2_555 1_555 2_555 yes F(1) As(1) F(3) 114.218(2) 2_555 1_555 3_555 yes F(1) As(1) F(3) 124.178(5) 2_555 1_555 4_555 yes F(1) As(1) F(3) 65.782(2) 2_555 1_555 5_554 yes F(1) As(1) F(3) 55.822(5) 2_555 1_555 6_554 yes F(1) As(1) F(3) 29.0178(4) 2_555 1_555 7_554 yes F(1) As(1) F(3) 84.404(3) 2_555 1_555 8_554 yes F(1) As(1) F(1) 112.966(5) 3_555 1_555 4_555 yes F(1) As(1) F(1) 107.752(4) 3_555 1_555 9_555 yes F(1) As(1) F(1) 107.752(7) 3_555 1_555 10_555 yes F(1) As(1) F(1) 180.0 3_555 1_555 11_555 yes F(1) As(1) F(1) 67.034(5) 3_555 1_555 12_555 yes F(1) As(1) F(2) 144.863(3) 3_555 1_555 1_555 yes F(1) As(1) F(2) 35.137(3) 3_555 1_555 2_555 yes F(1) As(1) F(2) 99.340(5) 3_555 1_555 3_555 yes F(1) As(1) F(2) 80.660(5) 3_555 1_555 4_555 yes F(1) As(1) F(3) 114.218(6) 3_555 1_555 1_555 yes F(1) As(1) F(3) 124.178(1) 3_555 1_555 2_555 yes F(1) As(1) F(3) 95.596(4) 3_555 1_555 3_555 yes F(1) As(1) F(3) 150.9822(9) 3_555 1_555 4_555 yes F(1) As(1) F(3) 84.404(4) 3_555 1_555 5_554 yes F(1) As(1) F(3) 29.0178(9) 3_555 1_555 6_554 yes F(1) As(1) F(3) 65.782(6) 3_555 1_555 7_554 yes F(1) As(1) F(3) 55.822(1) 3_555 1_555 8_554 yes F(1) As(1) F(1) 107.752(7) 4_555 1_555 9_555 yes F(1) As(1) F(1) 107.752(4) 4_555 1_555 10_555 yes F(1) As(1) F(1) 67.034(5) 4_555 1_555 11_555 yes F(1) As(1) F(1) 180.0 4_555 1_555 12_555 yes F(1) As(1) F(2) 35.137(3) 4_555 1_555 1_555 yes F(1) As(1) F(2) 144.863(3) 4_555 1_555 2_555 yes F(1) As(1) F(2) 80.660(5) 4_555 1_555 3_555 yes F(1) As(1) F(2) 99.340(5) 4_555 1_555 4_555 yes F(1) As(1) F(3) 124.178(1) 4_555 1_555 1_555 yes F(1) As(1) F(3) 114.218(6) 4_555 1_555 2_555 yes F(1) As(1) F(3) 150.9822(9) 4_555 1_555 3_555 yes F(1) As(1) F(3) 95.596(4) 4_555 1_555 4_555 yes F(1) As(1) F(3) 29.0178(9) 4_555 1_555 5_554 yes F(1) As(1) F(3) 84.404(4) 4_555 1_555 6_554 yes F(1) As(1) F(3) 55.822(1) 4_555 1_555 7_554 yes F(1) As(1) F(3) 65.782(6) 4_555 1_555 8_554 yes F(1) As(1) F(1) 112.966(2) 9_555 1_555 10_555 yes F(1) As(1) F(1) 72.248(4) 9_555 1_555 11_555 yes F(1) As(1) F(1) 72.248(7) 9_555 1_555 12_555 yes F(1) As(1) F(2) 80.660(6) 9_555 1_555 1_555 yes F(1) As(1) F(2) 99.340(6) 9_555 1_555 2_555 yes F(1) As(1) F(2) 144.8626(8) 9_555 1_555 3_555 yes F(1) As(1) F(2) 35.1374(8) 9_555 1_555 4_555 yes F(1) As(1) F(3) 84.404(3) 9_555 1_555 1_555 yes F(1) As(1) F(3) 29.0178(4) 9_555 1_555 2_555 yes F(1) As(1) F(3) 55.822(5) 9_555 1_555 3_555 yes F(1) As(1) F(3) 65.782(2) 9_555 1_555 4_555 yes F(1) As(1) F(3) 124.178(5) 9_555 1_555 5_554 yes F(1) As(1) F(3) 114.218(2) 9_555 1_555 6_554 yes F(1) As(1) F(3) 95.596(3) 9_555 1_555 7_554 yes F(1) As(1) F(3) 150.9822(4) 9_555 1_555 8_554 yes F(1) As(1) F(1) 72.248(7) 10_555 1_555 11_555 yes F(1) As(1) F(1) 72.248(4) 10_555 1_555 12_555 yes F(1) As(1) F(2) 99.340(6) 10_555 1_555 1_555 yes F(1) As(1) F(2) 80.660(6) 10_555 1_555 2_555 yes F(1) As(1) F(2) 35.1374(8) 10_555 1_555 3_555 yes F(1) As(1) F(2) 144.8626(8) 10_555 1_555 4_555 yes F(1) As(1) F(3) 29.0178(4) 10_555 1_555 1_555 yes F(1) As(1) F(3) 84.404(3) 10_555 1_555 2_555 yes F(1) As(1) F(3) 65.782(2) 10_555 1_555 3_555 yes F(1) As(1) F(3) 55.822(5) 10_555 1_555 4_555 yes F(1) As(1) F(3) 114.218(2) 10_555 1_555 5_554 yes F(1) As(1) F(3) 124.178(5) 10_555 1_555 6_554 yes F(1) As(1) F(3) 150.9822(4) 10_555 1_555 7_554 yes F(1) As(1) F(3) 95.596(3) 10_555 1_555 8_554 yes F(1) As(1) F(1) 112.966(5) 11_555 1_555 12_555 yes F(1) As(1) F(2) 35.137(3) 11_555 1_555 1_555 yes F(1) As(1) F(2) 144.863(3) 11_555 1_555 2_555 yes F(1) As(1) F(2) 80.660(5) 11_555 1_555 3_555 yes F(1) As(1) F(2) 99.340(5) 11_555 1_555 4_555 yes F(1) As(1) F(3) 65.782(6) 11_555 1_555 1_555 yes F(1) As(1) F(3) 55.822(1) 11_555 1_555 2_555 yes F(1) As(1) F(3) 84.404(4) 11_555 1_555 3_555 yes F(1) As(1) F(3) 29.0178(9) 11_555 1_555 4_555 yes F(1) As(1) F(3) 95.596(4) 11_555 1_555 5_554 yes F(1) As(1) F(3) 150.9822(9) 11_555 1_555 6_554 yes F(1) As(1) F(3) 114.218(6) 11_555 1_555 7_554 yes F(1) As(1) F(3) 124.178(1) 11_555 1_555 8_554 yes F(1) As(1) F(2) 144.863(3) 12_555 1_555 1_555 yes F(1) As(1) F(2) 35.137(3) 12_555 1_555 2_555 yes F(1) As(1) F(2) 99.340(5) 12_555 1_555 3_555 yes F(1) As(1) F(2) 80.660(5) 12_555 1_555 4_555 yes F(1) As(1) F(3) 55.822(1) 12_555 1_555 1_555 yes F(1) As(1) F(3) 65.782(6) 12_555 1_555 2_555 yes F(1) As(1) F(3) 29.0178(9) 12_555 1_555 3_555 yes F(1) As(1) F(3) 84.404(4) 12_555 1_555 4_555 yes F(1) As(1) F(3) 150.9822(9) 12_555 1_555 5_554 yes F(1) As(1) F(3) 95.596(4) 12_555 1_555 6_554 yes F(1) As(1) F(3) 124.178(1) 12_555 1_555 7_554 yes F(1) As(1) F(3) 114.218(6) 12_555 1_555 8_554 yes F(2) As(1) F(2) 180.0 1_555 1_555 2_555 yes F(2) As(1) F(2) 90.000(6) 1_555 1_555 3_555 yes F(2) As(1) F(2) 90.000(6) 1_555 1_555 4_555 yes F(2) As(1) F(3) 100.361(4) 1_555 1_555 1_555 yes F(2) As(1) F(3) 79.639(4) 1_555 1_555 2_555 yes F(2) As(1) F(3) 116.062(2) 1_555 1_555 3_555 yes F(2) As(1) F(3) 63.938(2) 1_555 1_555 4_555 yes F(2) As(1) F(3) 63.938(2) 1_555 1_555 5_554 yes F(2) As(1) F(3) 116.062(2) 1_555 1_555 6_554 yes F(2) As(1) F(3) 79.639(4) 1_555 1_555 7_554 yes F(2) As(1) F(3) 100.361(4) 1_555 1_555 8_554 yes F(2) As(1) F(2) 90.000(6) 2_555 1_555 3_555 yes F(2) As(1) F(2) 90.000(6) 2_555 1_555 4_555 yes F(2) As(1) F(3) 79.639(4) 2_555 1_555 1_555 yes F(2) As(1) F(3) 100.361(4) 2_555 1_555 2_555 yes F(2) As(1) F(3) 63.938(2) 2_555 1_555 3_555 yes F(2) As(1) F(3) 116.062(2) 2_555 1_555 4_555 yes F(2) As(1) F(3) 116.062(2) 2_555 1_555 5_554 yes F(2) As(1) F(3) 63.938(2) 2_555 1_555 6_554 yes F(2) As(1) F(3) 100.361(4) 2_555 1_555 7_554 yes F(2) As(1) F(3) 79.639(4) 2_555 1_555 8_554 yes F(2) As(1) F(2) 180.0 3_555 1_555 4_555 yes F(2) As(1) F(3) 63.938(1) 3_555 1_555 1_555 yes F(2) As(1) F(3) 116.062(1) 3_555 1_555 2_555 yes F(2) As(1) F(3) 100.361(3) 3_555 1_555 3_555 yes F(2) As(1) F(3) 79.639(3) 3_555 1_555 4_555 yes F(2) As(1) F(3) 79.639(3) 3_555 1_555 5_554 yes F(2) As(1) F(3) 100.361(3) 3_555 1_555 6_554 yes F(2) As(1) F(3) 116.062(1) 3_555 1_555 7_554 yes F(2) As(1) F(3) 63.938(1) 3_555 1_555 8_554 yes F(2) As(1) F(3) 116.062(1) 4_555 1_555 1_555 yes F(2) As(1) F(3) 63.938(1) 4_555 1_555 2_555 yes F(2) As(1) F(3) 79.639(3) 4_555 1_555 3_555 yes F(2) As(1) F(3) 100.361(3) 4_555 1_555 4_555 yes F(2) As(1) F(3) 100.361(3) 4_555 1_555 5_554 yes F(2) As(1) F(3) 79.639(3) 4_555 1_555 6_554 yes F(2) As(1) F(3) 63.938(1) 4_555 1_555 7_554 yes F(2) As(1) F(3) 116.062(1) 4_555 1_555 8_554 yes F(3) As(1) F(3) 56.685(3) 1_555 1_555 2_555 yes F(3) As(1) F(3) 39.2290(6) 1_555 1_555 3_555 yes F(3) As(1) F(3) 39.229(5) 1_555 1_555 4_555 yes F(3) As(1) F(3) 140.7710(6) 1_555 1_555 5_554 yes F(3) As(1) F(3) 140.771(5) 1_555 1_555 6_554 yes F(3) As(1) F(3) 180.0 1_555 1_555 7_554 yes F(3) As(1) F(3) 123.315(3) 1_555 1_555 8_554 yes F(3) As(1) F(3) 39.229(5) 2_555 1_555 3_555 yes F(3) As(1) F(3) 39.2290(6) 2_555 1_555 4_555 yes F(3) As(1) F(3) 140.771(5) 2_555 1_555 5_554 yes F(3) As(1) F(3) 140.7710(6) 2_555 1_555 6_554 yes F(3) As(1) F(3) 123.315(3) 2_555 1_555 7_554 yes F(3) As(1) F(3) 180.0 2_555 1_555 8_554 yes F(3) As(1) F(3) 56.685(3) 3_555 1_555 4_555 yes F(3) As(1) F(3) 180.0 3_555 1_555 5_554 yes F(3) As(1) F(3) 123.315(3) 3_555 1_555 6_554 yes F(3) As(1) F(3) 140.7710(6) 3_555 1_555 7_554 yes F(3) As(1) F(3) 140.771(5) 3_555 1_555 8_554 yes F(3) As(1) F(3) 123.315(3) 4_555 1_555 5_554 yes F(3) As(1) F(3) 180.0 4_555 1_555 6_554 yes F(3) As(1) F(3) 140.771(5) 4_555 1_555 7_554 yes F(3) As(1) F(3) 140.7710(6) 4_555 1_555 8_554 yes F(3) As(1) F(3) 56.685(3) 5_554 1_555 6_554 yes F(3) As(1) F(3) 39.2290(6) 5_554 1_555 7_554 yes F(3) As(1) F(3) 39.229(5) 5_554 1_555 8_554 yes F(3) As(1) F(3) 39.229(5) 6_554 1_555 7_554 yes F(3) As(1) F(3) 39.2290(6) 6_554 1_555 8_554 yes F(3) As(1) F(3) 56.685(3) 7_554 1_555 8_554 yes N(1) Ni(1) N(1) 90.000(6) 1_555 1_555 4_565 yes N(1) Ni(1) N(1) 90.000(6) 1_555 1_555 3_655 yes N(1) Ni(1) N(1) 180.0 1_555 1_555 2_665 yes N(1) Ni(1) N(1) 180.0 4_565 1_555 3_655 yes N(1) Ni(1) N(1) 90.000(6) 4_565 1_555 2_665 yes N(1) Ni(1) N(1) 90.000(6) 3_655 1_555 2_665 yes N(1) Co(1) N(1) 90.000(6) 1_555 1_555 4_565 yes N(1) Co(1) N(1) 90.000(6) 1_555 1_555 3_655 yes N(1) Co(1) N(1) 180.0 1_555 1_555 2_665 yes N(1) Co(1) N(1) 180.0 4_565 1_555 3_655 yes N(1) Co(1) N(1) 90.000(6) 4_565 1_555 2_665 yes N(1) Co(1) N(1) 90.000(6) 3_655 1_555 2_665 yes As(1) F(1) F(1) 115.841(1) 1_555 1_555 15_554 yes As(1) F(1) F(2) 75.5897(4) 1_555 1_555 3_555 yes As(1) F(1) F(3) 63.382(3) 1_555 1_555 5_554 yes As(1) F(1) F(3) 78.137(1) 1_555 1_555 8_554 yes F(1) F(1) F(2) 166.735(1) 15_554 1_555 3_555 yes F(1) F(1) F(3) 78.935(5) 15_554 1_555 5_554 yes F(1) F(1) F(3) 40.852(3) 15_554 1_555 8_554 yes F(2) F(1) F(3) 113.382(4) 3_555 1_555 5_554 yes F(2) F(1) F(3) 152.264(2) 3_555 1_555 8_554 yes F(3) F(1) F(3) 44.771(2) 5_554 1_555 8_554 yes As(1) F(2) F(1) 69.273(4) 1_555 1_555 4_555 yes As(1) F(2) F(1) 69.273(4) 1_555 1_555 11_555 yes F(1) F(2) F(1) 127.616(6) 4_555 1_555 11_555 yes As(1) F(3) As(1) 123.315(3) 1_555 1_555 5_555 yes As(1) F(3) F(1) 99.249(6) 1_555 1_555 5_555 yes As(1) F(3) F(1) 156.352(2) 1_555 1_555 8_555 yes As(1) F(3) F(1) 72.845(2) 1_555 1_555 10_555 yes As(1) F(3) F(1) 60.795(3) 1_555 1_555 12_555 yes As(1) F(3) F(3) 70.3855(3) 1_555 1_555 3_555 yes As(1) F(3) F(3) 70.385(3) 1_555 1_555 4_555 yes As(1) F(3) F(1) 60.795(2) 5_555 1_555 5_555 yes As(1) F(3) F(1) 72.845(5) 5_555 1_555 8_555 yes As(1) F(3) F(1) 156.3518(1) 5_555 1_555 10_555 yes As(1) F(3) F(1) 99.249(2) 5_555 1_555 12_555 yes As(1) F(3) F(3) 70.3855(3) 5_555 1_555 3_555 yes As(1) F(3) F(3) 70.385(3) 5_555 1_555 4_555 yes F(1) F(3) F(1) 104.085(7) 5_555 1_555 8_555 yes F(1) F(3) F(1) 101.975(2) 5_555 1_555 10_555 yes F(1) F(3) F(1) 139.6830(4) 5_555 1_555 12_555 yes F(1) F(3) F(3) 111.520(2) 5_555 1_555 3_555 yes F(1) F(3) F(3) 31.329(4) 5_555 1_555 4_555 yes F(1) F(3) F(1) 98.295(3) 8_555 1_555 10_555 yes F(1) F(3) F(1) 101.975(5) 8_555 1_555 12_555 yes F(1) F(3) F(3) 103.8992(9) 8_555 1_555 3_555 yes F(1) F(3) F(3) 133.223(4) 8_555 1_555 4_555 yes F(1) F(3) F(1) 104.085(2) 10_555 1_555 12_555 yes F(1) F(3) F(3) 133.2230(4) 10_555 1_555 3_555 yes F(1) F(3) F(3) 103.899(2) 10_555 1_555 4_555 yes F(1) F(3) F(3) 31.329(2) 12_555 1_555 3_555 yes F(1) F(3) F(3) 111.520(3) 12_555 1_555 4_555 yes F(3) F(3) F(3) 90.0 3_555 1_555 4_555 yes Ni(1) N(1) C(1) 127.6(5) 1_555 1_555 1_555 yes Ni(1) N(1) C(8) 127.3(5) 1_555 1_555 1_555 yes C(1) N(1) C(8) 105.1(6) 1_555 1_555 1_555 yes C(1) N(2) C(8) 120.3(6) 4_565 1_555 1_555 yes N(1) C(1) N(2) 126.9(6) 1_555 1_555 3_655 yes N(1) C(1) C(2) 111.4(6) 1_555 1_555 1_555 yes N(2) C(1) C(2) 121.6(6) 3_655 1_555 1_555 yes C(1) C(2) C(3) 133.0(7) 1_555 1_555 1_555 yes C(1) C(2) C(7) 105.9(6) 1_555 1_555 1_555 yes C(3) C(2) C(7) 121.1(7) 1_555 1_555 1_555 yes C(2) C(3) C(4) 118.1(7) 1_555 1_555 1_555 yes C(2) C(3) H(3) 122.1(8) 1_555 1_555 1_555 no C(4) C(3) H(3) 119.8(8) 1_555 1_555 1_555 no C(3) C(4) C(5) 121.5(8) 1_555 1_555 1_555 yes C(3) C(4) H(4) 119.9(8) 1_555 1_555 1_555 no C(5) C(4) H(4) 118.7(8) 1_555 1_555 1_555 no C(4) C(5) C(6) 120.1(7) 1_555 1_555 1_555 yes C(4) C(5) H(5) 122.8(8) 1_555 1_555 1_555 no C(6) C(5) H(5) 117.1(8) 1_555 1_555 1_555 no C(5) C(6) C(7) 118.1(7) 1_555 1_555 1_555 yes C(5) C(6) H(6) 125.0(8) 1_555 1_555 1_555 no C(7) C(6) H(6) 116.9(7) 1_555 1_555 1_555 no C(2) C(7) C(6) 121.1(7) 1_555 1_555 1_555 yes C(2) C(7) C(8) 106.7(6) 1_555 1_555 1_555 yes C(6) C(7) C(8) 132.1(7) 1_555 1_555 1_555 yes N(1) C(8) N(2) 127.9(6) 1_555 1_555 1_555 yes N(1) C(8) C(7) 110.8(6) 1_555 1_555 1_555 yes N(2) C(8) C(7) 121.3(6) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag As(1) F(1) 2.6739(1) 1_555 7_555 ? As(1) F(1) 2.6739(1) 1_555 8_555 ? As(1) F(1) 2.6739(1) 1_555 16_554 ? F(1) C(4) 3.106(8) 1_555 3_555 ? F(1) F(1) 3.1655(2) 1_555 16_554 ? F(2) C(4) 3.016(8) 1_555 4_555 ? F(2) C(4) 3.059(9) 1_555 1_555 ? F(2) C(3) 3.122(8) 1_555 1_555 ? #------------------------------------------------------------------------------ data_co1ni2 _database_code_CSD 156503 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Nov 18 15:52:05 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SAPI90 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 1331.49 _chemical_formula_analytical ? _chemical_formula_sum 'C64 H32 As Co0.50 F6 N16 Ni1.50 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 14.033(4) _cell_length_b 28.54(1) _cell_length_c 6.435(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2576.8101 _cell_formula_units_Z 2 _cell_measurement_temperature 288.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n c 2 ' _symmetry_Int_Tables_number 30 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, +z' ' -x,1/2+y,1/2+z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1341.00 _exptl_absorpt_coefficient_mu 1.433 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 288.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'Imaging Plate' _diffrn_measurement_device 'Rigaku RAXISII' _diffrn_measurement_method ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 2276 _reflns_number_total 2276 _reflns_number_observed 1739 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.091 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 0.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 128 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 64 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 32 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; As 0 2 0.050 2.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F 0 12 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Co 0 1 0.349 0.972 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ni 0 3 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags As1 0.0000 0.0000 0.0842(8) 0.1020(5) Uani d . 0.50 S Ni1 0.48787(9) 0.25434(4) 0.0708(6) 0.0257(2) Uani d . 0.75 . Co1 0.48784(7) 0.25435(3) 0.0704(5) 0.0400(9) Uani d . 0.25 . F1 -0.0452 0.0412 -0.0741 0.120(2) Uiso d . 1.00 S F2 0.1160 0.0291 0.0531 0.172(3) Uiso d . 1.00 S F3 -0.0192 0.0366 0.3053 0.239(6) Uiso d . 1.00 S N1 0.3639(3) 0.2265(1) 0.070(1) 0.0350(10) Uani d . 1.00 . N2 0.2629(3) 0.2952(1) 0.071(2) 0.035(1) Uani d . 1.00 . N3 0.4310(3) 0.3153(1) 0.079(2) 0.0308(10) Uani d . 1.00 . N4 0.5693(4) 0.3651(1) 0.070(2) 0.039(1) Uani d . 1.00 . N5 0.6106(3) 0.2825(1) 0.070(2) 0.0297(9) Uani d . 1.00 . N6 0.7122(3) 0.2137(1) 0.077(2) 0.037(1) Uani d . 1.00 . N7 0.5442(4) 0.1941(1) 0.077(2) 0.035(1) Uani d . 1.00 . N8 0.4053(3) 0.1435(1) 0.076(2) 0.032(1) Uani d . 1.00 . C1 0.3437(4) 0.1790(2) 0.062(2) 0.029(1) Uani d . 1.00 . C2 0.2416(4) 0.1713(2) 0.066(2) 0.030(1) Uani d . 1.00 . C3 0.1854(5) 0.1310(2) 0.070(2) 0.044(1) Uani d . 1.00 . C4 0.0891(5) 0.1373(2) 0.081(3) 0.054(2) Uani d . 1.00 . C5 0.0472(5) 0.1820(2) 0.067(3) 0.058(2) Uani d . 1.00 . C6 0.1040(4) 0.2220(2) 0.085(2) 0.045(2) Uani d . 1.00 . C7 0.1996(4) 0.2158(2) 0.074(2) 0.032(1) Uani d . 1.00 . C8 0.2790(4) 0.2491(2) 0.076(2) 0.031(1) Uani d . 1.00 . C9 0.3350(4) 0.3252(2) 0.065(2) 0.032(1) Uani d . 1.00 . C10 0.3205(4) 0.3756(2) 0.066(2) 0.036(1) Uani d . 1.00 . C11 0.2361(5) 0.4020(2) 0.075(2) 0.053(2) Uani d . 1.00 . C12 0.2487(6) 0.4508(2) 0.082(2) 0.057(2) Uani d . 1.00 . C13 0.3404(6) 0.4708(2) 0.050(2) 0.051(2) Uani d . 1.00 . C14 0.4219(5) 0.4445(2) 0.068(2) 0.052(2) Uani d . 1.00 . C15 0.4086(5) 0.3960(2) 0.087(2) 0.034(1) Uani d . 1.00 . C16 0.4774(4) 0.3575(2) 0.081(2) 0.031(1) Uani d . 1.00 . C17 0.6317(4) 0.3293(2) 0.079(2) 0.038(1) Uani d . 1.00 . C18 0.7327(4) 0.3373(2) 0.083(2) 0.037(1) Uani d . 1.00 . C19 0.7891(5) 0.3778(2) 0.052(2) 0.037(2) Uani d . 1.00 . C20 0.8849(5) 0.3725(2) 0.074(3) 0.056(2) Uani d . 1.00 . C21 0.9287(5) 0.3290(2) 0.047(2) 0.049(2) Uani d . 1.00 . C22 0.8715(5) 0.2872(2) 0.067(3) 0.055(2) Uani d . 1.00 . C23 0.7759(4) 0.2931(2) 0.081(2) 0.037(1) Uani d . 1.00 . C24 0.6977(4) 0.2593(2) 0.082(2) 0.031(1) Uani d . 1.00 . C25 0.6399(4) 0.1838(2) 0.073(2) 0.033(1) Uani d . 1.00 . C26 0.6557(5) 0.1330(2) 0.078(2) 0.037(1) Uani d . 1.00 . C27 0.7380(5) 0.1064(2) 0.070(2) 0.046(2) Uani d . 1.00 . C28 0.7265(5) 0.0580(2) 0.084(2) 0.053(2) Uani d . 1.00 . C29 0.6379(5) 0.0383(2) 0.079(3) 0.066(2) Uani d . 1.00 . C30 0.5523(5) 0.0638(2) 0.060(2) 0.049(2) Uani d . 1.00 . C31 0.5663(4) 0.1127(2) 0.089(1) 0.030(1) Uani d . 1.00 . C32 0.4964(4) 0.1508(2) 0.063(2) 0.028(1) Uani d . 1.00 . H3 0.2112 0.1006 0.1067 0.0488 Uiso calc . 1.00 . H4 0.0519 0.1100 0.0383 0.0779 Uiso calc . 1.00 . H5 -0.0251 0.1843 0.0161 0.0737 Uiso calc . 1.00 . H6 0.0797 0.2538 0.0966 0.0462 Uiso calc . 1.00 . H11 0.1745 0.3891 0.0335 0.0480 Uiso calc . 1.00 . H12 0.2000 0.4706 0.1363 0.0444 Uiso calc . 1.00 . H13 0.3433 0.5043 0.0111 0.0663 Uiso calc . 1.00 . H14 0.4842 0.4585 0.0623 0.0541 Uiso calc . 1.00 . H19 0.7621 0.4086 0.0883 0.0493 Uiso calc . 1.00 . H20 0.9200 0.3993 0.0203 0.0864 Uiso calc . 1.00 . H21 0.9999 0.3268 0.1067 0.0554 Uiso calc . 1.00 . H22 0.8995 0.2555 0.0805 0.0570 Uiso calc . 1.00 . H27 0.8012 0.1199 0.0376 0.0493 Uiso calc . 1.00 . H28 0.7800 0.0380 0.1136 0.0564 Uiso calc . 1.00 . H29 0.6323 0.0036 0.0125 0.0793 Uiso calc . 1.00 . H30 0.4896 0.0504 0.0377 0.0596 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 As(1) 0.0505(8) 0.0378(5) 0.218(2) 0.0071(5) 0.0000 0.0000 Ni(1) 0.0268(5) 0.0269(4) 0.0234(5) 0.0001(4) 0.004(1) 0.004(1) Co(1) 0.027(2) 0.028(1) 0.065(2) 0.000(1) 0.017(5) 0.010(5) N(1) 0.025(1) 0.034(2) 0.045(2) 0.003(1) -0.019(4) -0.041(4) N(2) 0.030(3) 0.031(2) 0.043(2) -0.001(2) 0.011(6) -0.008(6) N(3) 0.029(2) 0.027(1) 0.037(3) 0.000(1) 0.019(5) 0.012(5) N(4) 0.032(2) 0.032(2) 0.052(3) -0.005(2) 0.003(7) 0.030(5) N(5) 0.027(1) 0.035(2) 0.027(2) -0.003(1) -0.001(6) 0.012(5) N(6) 0.034(3) 0.038(2) 0.040(3) 0.000(2) -0.005(6) 0.022(6) N(7) 0.037(2) 0.031(1) 0.037(2) 0.005(1) -0.021(6) -0.006(5) N(8) 0.031(2) 0.029(2) 0.038(2) 0.001(2) 0.009(6) 0.003(6) C(1) 0.032(2) 0.032(2) 0.024(3) 0.003(2) 0.007(5) 0.005(5) C(2) 0.034(2) 0.030(2) 0.027(3) -0.001(2) 0.010(7) -0.002(6) C(3) 0.043(3) 0.028(2) 0.061(4) -0.004(2) -0.005(8) 0.023(6) C(4) 0.043(3) 0.037(3) 0.082(5) -0.013(2) 0.020(9) -0.016(8) C(5) 0.037(4) 0.042(2) 0.094(5) -0.010(2) -0.01(1) 0.023(9) C(6) 0.027(2) 0.041(3) 0.066(4) -0.001(2) 0.004(7) -0.015(7) C(7) 0.029(2) 0.030(2) 0.036(3) -0.001(2) 0.015(8) 0.003(8) C(8) 0.026(2) 0.032(2) 0.036(3) 0.002(2) 0.013(7) -0.017(6) C(9) 0.032(2) 0.026(2) 0.038(3) 0.002(2) -0.004(7) 0.020(6) C(10) 0.042(3) 0.025(2) 0.042(3) 0.004(2) -0.022(6) 0.000(6) C(11) 0.037(3) 0.043(2) 0.077(4) 0.003(2) 0.017(9) -0.039(6) C(12) 0.058(4) 0.039(2) 0.075(5) 0.019(3) 0.028(9) 0.001(8) C(13) 0.059(3) 0.032(3) 0.061(5) 0.004(2) -0.002(6) -0.005(5) C(14) 0.061(4) 0.026(2) 0.069(4) 0.001(2) -0.036(7) -0.012(6) C(15) 0.039(3) 0.029(2) 0.034(3) 0.001(2) 0.006(6) 0.003(6) C(16) 0.033(2) 0.029(2) 0.031(3) -0.003(2) 0.003(7) -0.002(6) C(17) 0.031(2) 0.037(2) 0.045(3) 0.001(2) -0.027(6) -0.021(6) C(18) 0.033(3) 0.037(2) 0.041(3) -0.007(2) -0.020(7) 0.003(6) C(19) 0.044(3) 0.040(3) 0.026(3) -0.016(2) -0.003(5) -0.005(4) C(20) 0.045(3) 0.050(3) 0.074(4) -0.011(3) 0.01(1) 0.008(10) C(21) 0.032(4) 0.057(3) 0.057(5) -0.007(2) -0.003(6) -0.001(6) C(22) 0.031(3) 0.054(3) 0.080(5) 0.001(2) 0.008(9) 0.022(8) C(23) 0.033(3) 0.040(2) 0.038(3) -0.002(2) 0.004(7) -0.019(6) C(24) 0.028(2) 0.040(2) 0.025(3) 0.003(2) 0.008(7) 0.007(6) C(25) 0.035(2) 0.035(2) 0.028(3) 0.002(2) 0.014(7) -0.001(6) C(26) 0.044(3) 0.036(2) 0.031(3) 0.006(2) 0.021(7) -0.002(6) C(27) 0.038(3) 0.051(3) 0.048(3) 0.009(2) -0.008(8) 0.021(7) C(28) 0.046(3) 0.049(2) 0.064(4) 0.019(2) -0.005(10) 0.011(8) C(29) 0.052(3) 0.033(3) 0.112(6) 0.014(2) -0.01(1) -0.01(1) C(30) 0.046(4) 0.028(2) 0.074(5) 0.000(2) -0.005(7) 0.025(5) C(31) 0.043(3) 0.031(2) 0.017(3) 0.009(2) 0.009(5) -0.001(4) C(32) 0.032(2) 0.033(2) 0.019(3) -0.001(2) -0.002(5) 0.015(4) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00016|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.0116(4) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1739 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_number_constraints 3 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0677 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0881 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.709 _refine_ls_shift/esd_max 2.1676 _refine_ls_shift/esd_mean 0.2763 _refine_diff_density_min -0.52 _refine_diff_density_max 0.95 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag As(1) F(1) 1.680(6) 1_555 1_555 yes As(1) F(1) 1.680(6) 1_555 2_555 yes As(1) F(2) 1.839(1) 1_555 1_555 yes As(1) F(2) 1.839(1) 1_555 2_555 yes As(1) F(3) 1.786(7) 1_555 1_555 yes As(1) F(3) 1.786(7) 1_555 2_555 yes Ni(1) N(1) 1.912(8) 1_555 1_555 yes Ni(1) N(3) 1.914(6) 1_555 1_555 yes Ni(1) N(5) 1.900(7) 1_555 1_555 yes Ni(1) N(7) 1.893(7) 1_555 1_555 yes Co(1) N(1) 1.912(8) 1_555 1_555 yes Co(1) N(3) 1.914(7) 1_555 1_555 yes Co(1) N(5) 1.900(8) 1_555 1_555 yes Co(1) N(7) 1.893(7) 1_555 1_555 yes N(1) C(1) 1.38(1) 1_555 1_555 yes N(1) C(8) 1.36(1) 1_555 1_555 yes N(2) C(8) 1.33(1) 1_555 1_555 yes N(2) C(9) 1.33(1) 1_555 1_555 yes N(3) C(9) 1.38(1) 1_555 1_555 yes N(3) C(16) 1.37(1) 1_555 1_555 yes N(4) C(16) 1.31(1) 1_555 1_555 yes N(4) C(17) 1.35(1) 1_555 1_555 yes N(5) C(17) 1.37(1) 1_555 1_555 yes N(5) C(24) 1.39(1) 1_555 1_555 yes N(6) C(24) 1.32(1) 1_555 1_555 yes N(6) C(25) 1.33(1) 1_555 1_555 yes N(7) C(25) 1.37(1) 1_555 1_555 yes N(7) C(32) 1.41(1) 1_555 1_555 yes N(8) C(1) 1.34(1) 1_555 1_555 yes N(8) C(32) 1.30(1) 1_555 1_555 yes C(1) C(2) 1.45(1) 1_555 1_555 yes C(2) C(3) 1.39(1) 1_555 1_555 yes C(2) C(7) 1.40(1) 1_555 1_555 yes C(3) C(4) 1.37(1) 1_555 1_555 yes C(4) C(5) 1.41(1) 1_555 1_555 yes C(5) C(6) 1.40(1) 1_555 1_555 yes C(6) C(7) 1.35(1) 1_555 1_555 yes C(7) C(8) 1.47(1) 1_555 1_555 yes C(9) C(10) 1.45(1) 1_555 1_555 yes C(10) C(11) 1.41(1) 1_555 1_555 yes C(10) C(15) 1.37(1) 1_555 1_555 yes C(11) C(12) 1.40(1) 1_555 1_555 yes C(12) C(13) 1.42(2) 1_555 1_555 yes C(13) C(14) 1.37(2) 1_555 1_555 yes C(14) C(15) 1.40(1) 1_555 1_555 yes C(15) C(16) 1.46(1) 1_555 1_555 yes C(17) C(18) 1.44(1) 1_555 1_555 yes C(18) C(19) 1.41(1) 1_555 1_555 yes C(18) C(23) 1.40(1) 1_555 1_555 yes C(19) C(20) 1.36(2) 1_555 1_555 yes C(20) C(21) 1.40(2) 1_555 1_555 yes C(21) C(22) 1.45(1) 1_555 1_555 yes C(22) C(23) 1.36(1) 1_555 1_555 yes C(23) C(24) 1.46(1) 1_555 1_555 yes C(25) C(26) 1.47(1) 1_555 1_555 yes C(26) C(27) 1.38(1) 1_555 1_555 yes C(26) C(31) 1.38(1) 1_555 1_555 yes C(27) C(28) 1.39(1) 1_555 1_555 yes C(28) C(29) 1.37(2) 1_555 1_555 yes C(29) C(30) 1.41(2) 1_555 1_555 yes C(30) C(31) 1.42(1) 1_555 1_555 yes C(31) C(32) 1.47(1) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F(1) As(1) F(1) 105.3(5) 1_555 1_555 2_555 yes F(1) As(1) F(2) 87.2(2) 1_555 1_555 1_555 yes F(1) As(1) F(2) 85.2(2) 1_555 1_555 2_555 yes F(1) As(1) F(3) 90.94(7) 1_555 1_555 1_555 yes F(1) As(1) F(3) 161.7(4) 1_555 1_555 2_555 yes F(1) As(1) F(2) 85.2(2) 2_555 1_555 1_555 yes F(1) As(1) F(2) 87.2(2) 2_555 1_555 2_555 yes F(1) As(1) F(3) 161.7(4) 2_555 1_555 1_555 yes F(1) As(1) F(3) 90.94(7) 2_555 1_555 2_555 yes F(2) As(1) F(2) 167.5(6) 1_555 1_555 2_555 yes F(2) As(1) F(3) 87.4(2) 1_555 1_555 1_555 yes F(2) As(1) F(3) 102.6(2) 1_555 1_555 2_555 yes F(2) As(1) F(3) 102.6(2) 2_555 1_555 1_555 yes F(2) As(1) F(3) 87.4(2) 2_555 1_555 2_555 yes F(3) As(1) F(3) 74.4(4) 1_555 1_555 2_555 yes N(1) Ni(1) N(3) 89.9(3) 1_555 1_555 1_555 yes N(1) Ni(1) N(5) 179.5(4) 1_555 1_555 1_555 yes N(1) Ni(1) N(7) 90.2(3) 1_555 1_555 1_555 yes N(3) Ni(1) N(5) 89.6(3) 1_555 1_555 1_555 yes N(3) Ni(1) N(7) 177.0(8) 1_555 1_555 1_555 yes N(5) Ni(1) N(7) 90.3(3) 1_555 1_555 1_555 yes N(1) Co(1) N(3) 89.9(3) 1_555 1_555 1_555 yes N(1) Co(1) N(5) 179.5(4) 1_555 1_555 1_555 yes N(1) Co(1) N(7) 90.2(3) 1_555 1_555 1_555 yes N(3) Co(1) N(5) 89.6(3) 1_555 1_555 1_555 yes N(3) Co(1) N(7) 177.0(8) 1_555 1_555 1_555 yes N(5) Co(1) N(7) 90.3(3) 1_555 1_555 1_555 yes Ni(1) N(1) C(1) 126.4(6) 1_555 1_555 1_555 yes Ni(1) N(1) C(8) 127.0(5) 1_555 1_555 1_555 yes C(1) N(1) C(8) 106.7(7) 1_555 1_555 1_555 yes C(8) N(2) C(9) 120.5(8) 1_555 1_555 1_555 yes Ni(1) N(3) C(9) 126.2(6) 1_555 1_555 1_555 yes Ni(1) N(3) C(16) 126.9(7) 1_555 1_555 1_555 yes C(9) N(3) C(16) 106.6(7) 1_555 1_555 1_555 yes C(16) N(4) C(17) 120.7(8) 1_555 1_555 1_555 yes Ni(1) N(5) C(17) 127.5(6) 1_555 1_555 1_555 yes Ni(1) N(5) C(24) 126.6(6) 1_555 1_555 1_555 yes C(17) N(5) C(24) 105.7(7) 1_555 1_555 1_555 yes C(24) N(6) C(25) 121.2(8) 1_555 1_555 1_555 yes Ni(1) N(7) C(25) 127.0(6) 1_555 1_555 1_555 yes Ni(1) N(7) C(32) 126.6(7) 1_555 1_555 1_555 yes C(25) N(7) C(32) 106.0(7) 1_555 1_555 1_555 yes C(1) N(8) C(32) 120.7(8) 1_555 1_555 1_555 yes N(1) C(1) N(8) 127.5(9) 1_555 1_555 1_555 yes N(1) C(1) C(2) 110.6(7) 1_555 1_555 1_555 yes N(8) C(1) C(2) 121.4(8) 1_555 1_555 1_555 yes C(1) C(2) C(3) 133.3(8) 1_555 1_555 1_555 yes C(1) C(2) C(7) 106.1(7) 1_555 1_555 1_555 yes C(3) C(2) C(7) 120.6(10) 1_555 1_555 1_555 yes C(2) C(3) C(4) 117.0(8) 1_555 1_555 1_555 yes C(2) C(3) H(3) 122(1) 1_555 1_555 1_555 no C(4) C(3) H(3) 118(1) 1_555 1_555 1_555 no C(3) C(4) C(5) 121.9(9) 1_555 1_555 1_555 yes C(3) C(4) H(4) 114(1) 1_555 1_555 1_555 no C(5) C(4) H(4) 118(1) 1_555 1_555 1_555 no C(4) C(5) C(6) 119(1) 1_555 1_555 1_555 yes C(4) C(5) H(5) 118(1) 1_555 1_555 1_555 no C(6) C(5) H(5) 121(1) 1_555 1_555 1_555 no C(5) C(6) C(7) 117.1(9) 1_555 1_555 1_555 yes C(5) C(6) H(6) 124(1) 1_555 1_555 1_555 no C(7) C(6) H(6) 118.2(9) 1_555 1_555 1_555 no C(2) C(7) C(6) 122.4(8) 1_555 1_555 1_555 yes C(2) C(7) C(8) 105.6(8) 1_555 1_555 1_555 yes C(6) C(7) C(8) 131.9(8) 1_555 1_555 1_555 yes N(1) C(8) N(2) 128.1(8) 1_555 1_555 1_555 yes N(1) C(8) C(7) 111.0(7) 1_555 1_555 1_555 yes N(2) C(8) C(7) 120.7(8) 1_555 1_555 1_555 yes N(2) C(9) N(3) 127.7(7) 1_555 1_555 1_555 yes N(2) C(9) C(10) 122.1(9) 1_555 1_555 1_555 yes N(3) C(9) C(10) 109.8(7) 1_555 1_555 1_555 yes C(9) C(10) C(11) 130.6(9) 1_555 1_555 1_555 yes C(9) C(10) C(15) 107.2(8) 1_555 1_555 1_555 yes C(11) C(10) C(15) 121.7(8) 1_555 1_555 1_555 yes C(10) C(11) C(12) 115.4(9) 1_555 1_555 1_555 yes C(10) C(11) H(11) 122.1(10) 1_555 1_555 1_555 no C(12) C(11) H(11) 119(1) 1_555 1_555 1_555 no C(11) C(12) C(13) 120.5(10) 1_555 1_555 1_555 yes C(11) C(12) H(12) 120(1) 1_555 1_555 1_555 no C(13) C(12) H(12) 117(1) 1_555 1_555 1_555 no C(12) C(13) C(14) 121(1) 1_555 1_555 1_555 yes C(12) C(13) H(13) 117(1) 1_555 1_555 1_555 no C(14) C(13) H(13) 121(1) 1_555 1_555 1_555 no C(13) C(14) C(15) 115(1) 1_555 1_555 1_555 yes C(13) C(14) H(14) 121.9(10) 1_555 1_555 1_555 no C(15) C(14) H(14) 122.2(10) 1_555 1_555 1_555 no C(10) C(15) C(14) 122.1(9) 1_555 1_555 1_555 yes C(10) C(15) C(16) 105.7(7) 1_555 1_555 1_555 yes C(14) C(15) C(16) 130.7(10) 1_555 1_555 1_555 yes N(3) C(16) N(4) 127.9(8) 1_555 1_555 1_555 yes N(3) C(16) C(15) 110.3(8) 1_555 1_555 1_555 yes N(4) C(16) C(15) 121.7(7) 1_555 1_555 1_555 yes N(4) C(17) N(5) 126.8(9) 1_555 1_555 1_555 yes N(4) C(17) C(18) 121.3(8) 1_555 1_555 1_555 yes N(5) C(17) C(18) 111.8(8) 1_555 1_555 1_555 yes C(17) C(18) C(19) 133.0(9) 1_555 1_555 1_555 yes C(17) C(18) C(23) 106.4(8) 1_555 1_555 1_555 yes C(19) C(18) C(23) 119(1) 1_555 1_555 1_555 yes C(18) C(19) C(20) 116.6(10) 1_555 1_555 1_555 yes C(18) C(19) H(19) 118(1) 1_555 1_555 1_555 no C(20) C(19) H(19) 116(1) 1_555 1_555 1_555 no C(19) C(20) C(21) 121(1) 1_555 1_555 1_555 yes C(19) C(20) H(20) 112(1) 1_555 1_555 1_555 no C(21) C(20) H(20) 115(1) 1_555 1_555 1_555 no C(20) C(21) C(22) 118(1) 1_555 1_555 1_555 yes C(20) C(21) H(21) 114(1) 1_555 1_555 1_555 no C(22) C(21) H(21) 115(1) 1_555 1_555 1_555 no C(21) C(22) C(23) 116.9(9) 1_555 1_555 1_555 yes C(21) C(22) H(22) 122(1) 1_555 1_555 1_555 no C(23) C(22) H(22) 120(1) 1_555 1_555 1_555 no C(18) C(23) C(22) 122.8(9) 1_555 1_555 1_555 yes C(18) C(23) C(24) 105.6(9) 1_555 1_555 1_555 yes C(22) C(23) C(24) 131.5(9) 1_555 1_555 1_555 yes N(5) C(24) N(6) 127.0(8) 1_555 1_555 1_555 yes N(5) C(24) C(23) 110.4(7) 1_555 1_555 1_555 yes N(6) C(24) C(23) 122.4(8) 1_555 1_555 1_555 yes N(6) C(25) N(7) 127.6(8) 1_555 1_555 1_555 yes N(6) C(25) C(26) 121.3(9) 1_555 1_555 1_555 yes N(7) C(25) C(26) 111.0(8) 1_555 1_555 1_555 yes C(25) C(26) C(27) 131.9(9) 1_555 1_555 1_555 yes C(25) C(26) C(31) 106.1(8) 1_555 1_555 1_555 yes C(27) C(26) C(31) 122.0(8) 1_555 1_555 1_555 yes C(26) C(27) C(28) 116.5(10) 1_555 1_555 1_555 yes C(26) C(27) H(27) 122.8(9) 1_555 1_555 1_555 no C(28) C(27) H(27) 120(1) 1_555 1_555 1_555 no C(27) C(28) C(29) 120.8(10) 1_555 1_555 1_555 yes C(27) C(28) H(28) 120(1) 1_555 1_555 1_555 no C(29) C(28) H(28) 118(1) 1_555 1_555 1_555 no C(28) C(29) C(30) 124.3(10) 1_555 1_555 1_555 yes C(28) C(29) H(29) 116(1) 1_555 1_555 1_555 no C(30) C(29) H(29) 112(1) 1_555 1_555 1_555 no C(29) C(30) C(31) 112(1) 1_555 1_555 1_555 yes C(29) C(30) H(30) 125.5(9) 1_555 1_555 1_555 no C(31) C(30) H(30) 122.2(10) 1_555 1_555 1_555 no C(26) C(31) C(30) 122.0(9) 1_555 1_555 1_555 yes C(26) C(31) C(32) 106.8(7) 1_555 1_555 1_555 yes C(30) C(31) C(32) 128.1(10) 1_555 1_555 1_555 yes N(7) C(32) N(8) 127.3(8) 1_555 1_555 1_555 yes N(7) C(32) C(31) 108.8(8) 1_555 1_555 1_555 yes N(8) C(32) C(31) 122.0(8) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F(2) C(3) 3.068(9) 1_555 1_555 ? F(2) C(4) 3.114(9) 1_555 1_555 ? N(4) C(31) 3.16(2) 1_555 4_554 ? C(16) C(32) 3.12(3) 1_555 4_555 ? #------------------------------------------------------------------------------