#======================================================================= 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 'Fe0.236 Nb1 S2' _chemical_formula_weight 170.2 _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 3.3326(5) _cell_length_b 3.3326(5) _cell_length_c 12.105(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 116.43(3) _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 4.8535 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 158 _exptl_absorpt_coefficient_mu 7.932 _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 0.3156 _exptl_absorpt_correction_T_max 0.9313 #======================================================================= # 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 1343 _diffrn_reflns_theta_min 6.74 _diffrn_reflns_theta_max 29.05 _diffrn_reflns_theta_full 29.05 _diffrn_measured_fraction_theta_max 0.93 _diffrn_measured_fraction_theta_full 0.94 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0031 _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 14 _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 78 _reflns_number_gt 73 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0215 _refine_ls_wR_factor_gt 0.0243 _refine_ls_R_factor_all 0.0241 _refine_ls_wR_factor_ref 0.0253 _refine_ls_goodness_of_fit_ref 2.51 _refine_ls_goodness_of_fit_gt 2.52 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 78 _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 0.0022 _refine_ls_shift/su_mean 0.0009 _refine_diff_density_max 1.86 _refine_diff_density_min -1.52 _refine_ls_extinction_method 'B-C type 2 (Becker & Coppens, 1974)' _refine_ls_extinction_coef 10200(900) _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 0.0060(3) 2 1 d . . . Fe1 Fe 0 0 0 Uani 0.0056(18) 2 0.236(11) d . . . S1 S 0.333333 0.666667 0.62049(9) Uani 0.0070(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 0.0053(4) 0.0053(4) 0.0076(4) 0.00263(20) 0 0 Fe1 Fe 0.006(2) 0.006(2) 0.006(3) 0.0028(12) 0 0 S1 S 0.0062(5) 0.0062(5) 0.0085(6) 0.0031(2) 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 2.4819(10) yes Nb1 S1 . 4_564 2.4819(8) yes Nb1 S1 . 4_664 2.4819(10) yes Nb1 S1 . 7_446 2.4819(10) yes Nb1 S1 . 7_456 2.4819(8) yes Nb1 S1 . 7_556 2.4819(10) yes Fe1 S1 . 4_554 2.4144(10) yes Fe1 S1 . 4_564 2.4144(7) yes Fe1 S1 . 4_664 2.4144(10) yes Fe1 S1 . 10_555 2.4144(10) yes Fe1 S1 . 10_655 2.4144(7) yes Fe1 S1 . 10_665 2.4144(10) 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 ? ? ? ? ? ? ? ? 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 -1 2 0 1268.46 1056.08 5.54 o 0 2 0 1174.88 1171.47 2.11 o -1 3 0 793.80 815.92 1.87 o 0 3 0 2557.78 2735.36 4.54 o -2 4 0 2523.77 2639.58 5.93 o -1 4 0 464.59 448.00 2.28 o 0 1 1 720.79 733.40 1.10 o 0 2 1 352.03 326.57 0.94 o -1 3 1 250.15 246.24 0.81 o 0 3 1 0.00 1.55 0.87 < -1 4 1 145.85 140.85 1.04 o -1 2 2 1319.47 1324.43 1.58 o 0 2 2 1313.78 1312.61 1.50 o -1 3 2 950.40 953.47 1.52 o 0 3 2 672.10 666.73 1.96 o -2 4 2 547.18 542.51 2.18 o -1 4 2 578.95 571.47 1.94 o 0 1 3 729.79 735.67 0.92 o 0 2 3 404.13 396.05 1.05 o -1 3 3 294.76 284.67 0.87 o 0 3 3 0.00 0.90 0.78 < -1 4 3 172.55 168.68 1.43 o 0 0 4 567.40 553.08 1.42 o -1 2 4 402.72 414.72 0.90 o 0 2 4 2721.95 3069.63 2.95 o -1 3 4 2282.26 2369.81 1.95 o 0 3 4 176.59 172.08 1.22 o -2 4 4 137.68 132.01 1.44 o -1 4 4 1463.62 1475.87 3.87 o 0 1 5 354.41 345.52 0.66 o 0 2 5 224.14 211.15 0.86 o -1 3 5 166.22 162.89 0.74 o 0 3 5 0.00 0.93 0.80 < -1 4 5 97.74 96.04 1.49 o 0 0 6 1877.70 2010.09 4.90 o 0 1 6 1194.93 1205.97 1.16 o -1 2 6 1379.01 1418.96 1.76 o 0 2 6 849.21 841.89 1.36 o -1 3 6 650.61 649.43 1.34 o 0 3 6 811.08 821.33 2.20 o -2 4 6 664.61 649.59 3.90 o -1 4 6 413.21 414.04 4.18 o 0 1 7 501.79 487.47 0.85 o 0 2 7 357.95 336.22 1.10 o -1 3 7 274.59 272.62 1.05 o 0 3 7 0.00 1.25 0.92 < 0 1 8 1000.20 1055.81 1.23 o -1 2 8 3069.23 3598.86 3.09 o 0 2 8 711.19 727.01 1.72 o -1 3 8 548.86 546.75 1.54 o 0 3 8 2041.99 2211.76 4.49 o 0 1 9 150.79 145.01 0.72 o 0 2 9 112.03 111.32 1.03 o -1 3 9 85.76 84.95 0.86 o 0 3 9 0.00 0.65 1.96 < 0 0 10 595.43 591.47 2.48 o 0 1 10 1030.52 1048.50 1.68 o -1 2 10 435.11 433.38 1.84 o 0 2 10 822.94 859.65 2.35 o -1 3 10 660.65 682.03 1.81 o 0 3 10 276.56 284.92 6.33 o 0 1 11 349.44 336.80 1.18 o 0 2 11 271.00 279.83 1.64 o -1 3 11 209.72 215.82 1.73 o 0 0 12 238.13 234.69 2.58 o 0 1 12 1777.88 1961.55 2.99 o -1 2 12 174.57 166.50 1.39 o 0 2 12 1440.23 1556.24 3.74 o -1 3 12 1136.88 1204.04 5.60 o 0 1 13 57.13 57.29 0.95 o 0 2 13 43.81 45.64 1.42 o 0 0 14 990.56 964.98 8.90 o 0 1 14 372.79 368.24 2.19 o -1 2 14 768.44 733.70 6.49 o 0 2 14 293.13 296.52 5.29 o 0 1 15 220.31 206.17 2.70 o 0 0 16 1745.41 1661.02 12.32 o 0 1 16 369.64 354.29 6.81 o