data_x _audit_creation_method SHELXL-97 _chemical_name_systematic ; Thomas K. Reynolds, Joshua G. Bales, Francis J. DiSalvo Chemistry of Materials 2002, 14, 4746-4751 ; _chemical_name_common 'Nickel Antimonide Telluride' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ni5.66 Sb Te2' _chemical_formula_weight 709.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I4/mmm' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' '-y, -x, -z' 'y, x, -z' 'y, -x, z' '-y, x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' '-x, y, z' 'x, -y, z' 'y, x, z' '-y, -x, z' '-y, x, -z' 'y, -x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' _cell_length_a 3.7824(5) _cell_length_b 3.7824(5) _cell_length_c 19.244(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 275.32(8) _cell_formula_units_Z 2 _cell_measurement_temperature 164(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 8.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 627 _exptl_absorpt_coefficient_mu 34.002 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 164(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1703 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 4.24 _diffrn_reflns_theta_max 30.42 _reflns_number_total 159 _reflns_number_gt 158 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'SHELXTL' _computing_structure_solution 'Sir92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'WingX (Farrugia, 1999)' _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^)+(0.0340P)^2^+5.3532P] 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 SHELXL _refine_ls_extinction_coef 0.0248(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 159 _refine_ls_number_parameters 17 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0541 _refine_ls_wR_factor_gt 0.0537 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _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 Te1 Te 0.0000 0.0000 0.18143(3) 0.0043(3) Uani 1 8 d S . . Sb1 Sb 0.0000 0.0000 0.5000 0.0029(3) Uani 1 16 d S . . Ni1 Ni 0.0000 0.0000 0.0000 0.0034(4) Uani 1 16 d S . . Ni2 Ni 0.0000 0.5000 0.09372(5) 0.0041(3) Uani 1 4 d S . . Ni3 Ni 0.0000 0.0000 0.3098(2) 0.0057(14) Uani 0.330(8) 8 d SP . . 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 Te1 0.0040(3) 0.0040(3) 0.0048(4) 0.000 0.000 0.000 Sb1 0.0037(3) 0.0037(3) 0.0013(4) 0.000 0.000 0.000 Ni1 0.0041(6) 0.0041(6) 0.0021(8) 0.000 0.000 0.000 Ni2 0.0051(5) 0.0040(5) 0.0033(5) 0.000 0.000 0.000 Ni3 0.0082(16) 0.0082(16) 0.001(2) 0.000 0.000 0.000 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 30.42 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.069 _refine_diff_density_min -3.461 _refine_diff_density_rms 0.531 #===END data_x _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Nickel Antimonide Selenide' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ni5.72 Sb Se2' _chemical_formula_weight 615.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 4/mmm' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' '-y, -x, -z' 'y, x, -z' 'y, -x, z' '-y, x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' '-x, y, z' 'x, -y, z' 'y, x, z' '-y, -x, z' '-y, x, -z' 'y, -x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' _cell_length_a 3.7021(5) _cell_length_b 3.7021(5) _cell_length_c 18.593(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 254.83(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 8.021 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 558 _exptl_absorpt_coefficient_mu 40.012 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1433 _diffrn_reflns_av_R_equivalents 0.1701 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.38 _diffrn_reflns_theta_max 29.12 _reflns_number_total 132 _reflns_number_gt 132 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'SHELXTL' _computing_structure_solution 'Sir92 (Altomare et al., 1993) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL' _computing_publication_material 'WingX (Farrugia, 1999)' _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^)+(0.0132P)^2^+15.7927P] 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 SHELXL _refine_ls_extinction_coef 0.010(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 132 _refine_ls_number_parameters 17 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 1.279 _refine_ls_restrained_S_all 1.279 _refine_ls_shift/su_max 0.000 _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 Se1 Se 0.0000 0.0000 0.18100(15) 0.0159(8) Uani 1 8 d S . . Sb1 Sb 0.0000 0.0000 0.5000 0.0150(8) Uani 1 16 d S . . Ni1 Ni 0.0000 0.0000 0.0000 0.0158(10) Uani 1 16 d S . . Ni2 Ni 0.0000 0.5000 0.10009(14) 0.0163(8) Uani 1 4 d S . . Ni3 Ni 0.0000 0.0000 0.3020(6) 0.022(3) Uani 0.359(17) 8 d SP . . 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 Se1 0.0108(9) 0.0108(9) 0.0261(15) 0.000 0.000 0.000 Sb1 0.0085(8) 0.0085(8) 0.0280(15) 0.000 0.000 0.000 Ni1 0.0109(13) 0.0109(13) 0.026(2) 0.000 0.000 0.000 Ni2 0.0125(12) 0.0097(11) 0.0266(15) 0.000 0.000 0.000 Ni3 0.021(4) 0.021(4) 0.024(6) 0.000 0.000 0.000 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.12 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.995 _refine_diff_density_min -2.568 _refine_diff_density_rms 0.491 #===END