#======================================================================= data_global #======================================================================= _audit_creation_method 'Jana2006 Version : 19/07/2010' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_paper_category ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'Canadian Mineralogist' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name ? _publ_contact_author_address ; ? ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal 'Canadian Mineralogist' _publ_requested_category ? _publ_contact_letter ; ? ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ? # name ; ? # footnote ; ; ? # address ; #======================================================================= # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_introduction ; ? ; _publ_section_experimental ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_exptl_solution ; ? ; _publ_section_discussion ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; ; _publ_section_figure_captions ; ? ; _publ_section_table_legends ; ? ; #======================================================================= data_(I) #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'Fe0.477 Nb1 S2' _chemical_formula_weight 183.7 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration . #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63/m m c' _symmetry_space_group_name_Hall '-P 6c;-2c' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -y,x-y,z 3 -x+y,-x,z 4 -x,-y,z+1/2 5 y,-x+y,z+1/2 6 x-y,x,z+1/2 7 y,x,-z 8 x-y,-y,-z 9 -x,-x+y,-z 10 -y,-x,-z+1/2 11 -x+y,y,-z+1/2 12 x,x-y,-z+1/2 13 -x,-y,-z 14 y,-x+y,-z 15 x-y,x,-z 16 x,y,-z+1/2 17 -y,x-y,-z+1/2 18 -x+y,-x,-z+1/2 19 -y,-x,z 20 -x+y,y,z 21 x,x-y,z 22 y,x,z+1/2 23 x-y,-y,z+1/2 24 -x,-x+y,z+1/2 _cell_length_a 3.3322(2) _cell_length_b 3.3322(2) _cell_length_c 12.3533(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 118.789(12) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature ? _cell_special_details ; ? ; _exptl_crystal_density_diffrn 5.1332 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 171 _exptl_absorpt_coefficient_mu 9.161 _exptl_crystal_description ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_size_rad ? _exptl_crystal_colour ? _exptl_absorpt_correction_type Cylindrical _exptl_absorpt_process_details 'Jana2006 (Petricek, Dusek & Palatinus, 2000)' _exptl_absorpt_correction_T_min 0.2077 _exptl_absorpt_correction_T_max 0.8108 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_reflns_number 1413 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 29.14 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0041 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 86 _reflns_number_gt 81 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_gt 0.0301 _refine_ls_R_factor_all 0.0274 _refine_ls_wR_factor_ref 0.0305 _refine_ls_goodness_of_fit_ref 2.99 _refine_ls_goodness_of_fit_gt 3.05 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 86 _refine_ls_number_parameters 10 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0028 _refine_ls_shift/su_mean 0.0006 _refine_diff_density_max 1.35 _refine_diff_density_min -1.69 _refine_ls_extinction_method 'B-C type 2 (Becker & Coppens, 1974)' _refine_ls_extinction_coef 1300(500) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Fe 0.346 0.844 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Nb -2.073 0.622 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.125 0.123 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0 0 0.25 Uani 0.0049(3) 2 1 d . . . Fe1 Fe 0 0 0 Uani 0.0098(12) 2 0.477(12) d . . . S1 S 0.333333 0.666667 0.62235(10) Uani 0.0064(4) 4 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _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 Nb1 Nb 0.0056(4) 0.0056(4) 0.0034(5) 0.0028(2) 0 0 Fe1 Fe 0.0122(16) 0.0122(16) 0.0050(18) 0.0061(8) 0 0 S1 S 0.0072(6) 0.0072(6) 0.0048(7) 0.0036(3) 0 0 #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Nb1 S1 . 4_554 2.4876(9) yes Nb1 S1 . 4_564 2.4876(8) yes Nb1 S1 . 4_664 2.4876(9) yes Nb1 S1 . 7_446 2.4876(9) yes Nb1 S1 . 7_456 2.4876(8) yes Nb1 S1 . 7_556 2.4876(9) yes Fe1 S1 . 4_554 2.4465(8) yes Fe1 S1 . 4_564 2.4465(8) yes Fe1 S1 . 4_664 2.4465(8) yes Fe1 S1 . 10_555 2.4465(8) yes Fe1 S1 . 10_655 2.4465(8) yes Fe1 S1 . 10_665 2.4465(8) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag S1 Nb1 S1 4_554 . 4_564 84.10(2) yes S1 Nb1 S1 4_554 . 4_664 84.10(2) yes S1 Nb1 S1 4_554 . 7_446 78.68(3) yes S1 Nb1 S1 4_554 . 7_456 134.502(12) yes S1 Nb1 S1 4_554 . 7_556 134.502(11) yes S1 Nb1 S1 4_564 . 4_664 84.10(2) yes S1 Nb1 S1 4_564 . 7_446 134.502(12) yes S1 Nb1 S1 4_564 . 7_456 78.68(3) yes S1 Nb1 S1 4_564 . 7_556 134.502(12) yes S1 Nb1 S1 4_664 . 7_446 134.502(11) yes S1 Nb1 S1 4_664 . 7_456 134.502(12) yes S1 Nb1 S1 4_664 . 7_556 78.68(3) yes S1 Nb1 S1 7_446 . 7_456 84.10(2) yes S1 Nb1 S1 7_446 . 7_556 84.10(2) yes S1 Nb1 S1 7_456 . 7_556 84.10(2) yes S1 Fe1 S1 4_554 . 4_564 85.84(2) yes S1 Fe1 S1 4_554 . 4_664 85.84(3) yes S1 Fe1 S1 4_554 . 10_555 94.16(3) yes S1 Fe1 S1 4_554 . 10_655 94.16(2) yes S1 Fe1 S1 4_554 . 10_665 180 yes S1 Fe1 S1 4_564 . 4_664 85.84(2) yes S1 Fe1 S1 4_564 . 10_555 94.16(2) yes S1 Fe1 S1 4_564 . 10_655 180 yes S1 Fe1 S1 4_564 . 10_665 94.16(2) yes S1 Fe1 S1 4_664 . 10_555 180 yes S1 Fe1 S1 4_664 . 10_655 94.16(2) yes S1 Fe1 S1 4_664 . 10_665 94.16(3) yes S1 Fe1 S1 10_555 . 10_655 85.84(2) yes S1 Fe1 S1 10_555 . 10_665 85.84(3) yes S1 Fe1 S1 10_655 . 10_665 85.84(2) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? ? ? #======================================================================= # 11. STRUCTURE-FACTOR LIST loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_observed_status 0 1 0 3209.04 2896.26 11.02 o -1 2 0 8425.43 7447.12 25.28 o 0 2 0 1727.94 1648.01 3.37 o -1 3 0 1103.83 1061.37 2.61 o 0 3 0 4080.81 3923.43 8.49 o -2 4 0 2979.24 2973.04 11.71 o -1 4 0 589.19 608.46 3.72 o 0 1 1 771.70 756.68 1.17 o 0 2 1 363.01 332.27 1.12 o -1 3 1 252.14 244.63 0.95 o 0 3 1 0.00 4.27 0.89 o -1 4 1 141.63 146.85 1.50 o 0 0 2 1996.47 2247.08 37.76 o 0 1 2 1689.19 1584.07 2.84 o -1 2 2 1034.70 980.58 1.78 o 0 2 2 995.51 968.09 1.82 o -1 3 2 732.53 713.40 1.53 o 0 3 2 567.43 573.25 2.64 o -2 4 2 457.47 467.98 2.69 o -1 4 2 467.80 493.61 2.94 o 0 1 3 738.38 755.89 1.29 o 0 2 3 389.51 374.89 1.16 o -1 3 3 275.47 270.28 1.03 o 0 3 3 0.00 0.61 0.78 < -1 4 3 155.52 166.67 1.75 o 0 0 4 1212.10 1438.93 6.93 o 0 1 4 6957.86 6851.42 14.96 o -1 2 4 730.51 744.43 1.61 o 0 2 4 4380.89 4121.29 5.34 o -1 3 4 3086.25 3031.15 3.54 o 0 3 4 292.49 297.78 2.04 o -2 4 4 217.39 217.57 1.87 o -1 4 4 1767.39 1863.78 6.07 o 0 1 5 438.58 457.32 1.14 o 0 2 5 267.13 249.97 1.18 o -1 3 5 193.64 196.30 1.06 o 0 3 5 0.00 0.53 0.72 < -1 4 5 110.03 118.09 2.15 o 0 0 6 1643.74 1851.86 6.17 o 0 1 6 1032.74 1072.50 1.77 o -1 2 6 1063.50 1075.40 1.91 o 0 2 6 721.75 693.05 1.96 o -1 3 6 561.20 552.21 1.75 o 0 3 6 639.32 635.04 3.24 o -2 4 6 515.82 529.54 4.54 o -1 4 6 369.17 394.15 3.83 o 0 1 7 503.32 523.95 1.26 o 0 2 7 344.49 336.79 1.30 o -1 3 7 255.01 254.96 1.27 o 0 3 7 0.00 1.15 0.86 < -1 4 7 146.44 147.72 3.78 o 0 0 8 7338.09 8060.48 41.76 o 0 1 8 1689.58 1824.61 2.54 o -1 2 8 5224.64 5125.94 5.42 o 0 2 8 1110.85 1092.71 2.44 o -1 3 8 795.03 784.52 2.15 o 0 3 8 2997.82 2970.50 6.73 o -2 4 8 2292.78 2625.35 17.97 o 0 1 9 232.03 247.40 1.25 o 0 2 9 168.55 169.61 1.38 o -1 3 9 126.50 122.38 1.02 o 0 3 9 0.00 1.27 1.10 < 0 0 10 583.76 607.86 4.53 o 0 1 10 889.26 962.13 2.59 o -1 2 10 453.67 454.72 1.81 o 0 2 10 699.86 679.98 2.90 o -1 3 10 564.79 544.80 2.12 o 0 3 10 304.82 283.88 3.40 o 0 1 11 359.65 389.21 1.84 o 0 2 11 269.24 267.20 2.12 o -1 3 11 203.81 194.62 1.74 o 0 3 11 0.00 -1.42 2.90 < 0 0 12 453.98 465.82 5.00 o 0 1 12 3020.17 3272.73 6.13 o -1 2 12 316.50 318.92 2.33 o 0 2 12 2276.55 2258.00 5.91 o -1 3 12 1767.88 1546.54 12.92 o 0 1 13 123.36 132.78 1.48 o 0 2 13 93.14 87.18 2.28 o 0 0 14 836.77 851.89 8.28 o 0 1 14 409.01 410.74 2.80 o -1 2 14 668.17 635.64 7.07 o 0 2 14 336.10 330.37 5.87 o 0 1 15 244.26 244.42 3.01 o 0 0 16 3025.23 2818.16 23.00 o 0 1 16 644.57 630.38 7.91 o