data_publication_text _publ_contact_author_name 'Frank C Hawthorne' _publ_contact_author_address ;Department of Geological Sciences, University of Manitoba Winnipeg, MB, R3T 2N2, Canada ; _publ_contact_author_email clhawth@cc.umanitoba.ca loop_ _publ_author_name _publ_author_address 'Hawthorne, Frank C ' ;Department of Geological Sciences, University of Manitoba Winnipeg, MB, R3T 2N2, Canada ; 'Cooper, Mark A.' ;Department of Geological Sciences, University of Manitoba Winnipeg, MB, R3T 2N2, Canada ; 'Ball, Neil A.' ;Department of Geological Sciences, University of Manitoba Winnipeg, MB, R3T 2N2, Canada ; '?ERN\'Y, PETR' ;Department of Geological Sciences, University of Manitoba Winnipeg, MB, R3T 2N2, Canada ; 'C\'AMARA, Fernando' ;Dipartimento di Scienze Mineralogiche e Petrologiche Via Valperga Caluso 35 - 10125 Torino, Italy ; 'LAURS , BRENDAN M.' ;Gemological Institute of America, 5345 Armada Drive, Carlsbad, California 92008, USA ; data_billwiseite _audit_creation_method SHELXL-97 _chemical_name_systematic Billwiseite _chemical_name_common ? _chemical_formula_moiety 'Nb6.24 O72 Sb20.08 Ta9.76' _chemical_formula_sum 'Nb6.24 O72 Sb20.08 Ta9.76' _chemical_compound_source 'from Stak Nala, Karakoram Mountains, northern Pakistan' _chemical_melting_point ? _exptl_crystal_description 'lath' _exptl_crystal_colour 'pale yellow' _diffrn_ambient_temperature 298(2) _chemical_formula_weight 5943.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_int_tables_number 15 _symmetry_space_group_name_Hall '-C 2yc' _chemical_absolute_configuration ? 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 54.116(5) _cell_length_b 4.9143(5) _cell_length_c 5.5482(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.425(2) _cell_angle_gamma 90.00 _cell_volume 1475.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5795 _cell_measurement_theta_min 2 _cell_measurement_theta_max 60 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.035 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2610 _exptl_absorpt_coefficient_mu 28.391 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.097 _exptl_absorpt_correction_T_max 0.356 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 8754 reflections reduced R(int) from 0.1600 to 0.0564 Ratio of minimum to maximum apparent transmission: 0.492447 The given Tmax was generated using the SHELX SIZE command Tmis was calculated as Tmin = relative-correction-factor * Tmax. ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source_type SIEMENS _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER-AXS SMART APEX CCD' _diffrn_measurement_method \\w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11046 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -76 _diffrn_reflns_limit_h_max 76 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 0.75 _diffrn_reflns_theta_max 30.00 _reflns_number_total 2138 _reflns_number_gt 2122 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART,version 5.625' _computing_cell_refinement 'SAINT version 6.45' _computing_data_reduction 'SAINT version 6.45' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0217P)^2^+194.5181P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2138 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.186 _refine_ls_shift/su_max 0.003 _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 Ta1 Ta 0.054795(11) 0.25442(14) 1.13172(11) 0.0084(2) Uani 0.60(2) 1 d P . . Nb1 Nb 0.054795(11) 0.25442(14) 1.13172(11) 0.0084(2) Uani 0.40(2) 1 d P . . Ta2 Ta 0.164630(11) 0.23919(13) 0.37332(12) 0.0075(2) Uani 0.62(2) 1 d P . . Nb2 Nb 0.164630(11) 0.23919(13) 0.37332(12) 0.0075(2) Uani 0.38(2) 1 d P . . Sb1 Sb 0.0000 0.1983(3) 0.7500 0.0138(4) Uani 1.011(16) 2 d SP . . Sb2 Sb 0.221519(16) -0.20656(18) 0.32554(16) 0.0132(3) Uani 1.019(15) 1 d P . . Sb3 Sb 0.109969(16) 0.29999(19) 0.72606(17) 0.0129(3) Uani 0.986(15) 1 d P . . O1 O 0.12890(15) 0.413(2) 0.4089(18) 0.0119(19) Uani 1 1 d . . . O2 O 0.02086(16) 0.087(2) 1.0867(18) 0.0113(19) Uani 1 1 d . . . O3 O 0.06472(16) 0.013(2) 1.3665(18) 0.0127(19) Uani 1 1 d . . . O4 O 0.23860(15) 0.068(2) 0.1263(17) 0.0117(19) Uani 1 1 d . . . O5 O 0.08747(15) 0.4130(19) 1.0794(17) 0.0096(18) Uani 1 1 d . . . O6 O 0.15095(16) 0.0356(19) 0.6676(18) 0.0113(19) Uani 1 1 d . . . O7 O 0.19594(17) 0.085(2) 0.4244(18) 0.0132(19) Uani 1 1 d . . . O8 O 0.17287(17) 0.521(2) 0.6311(19) 0.016(2) Uani 1 1 d . . . O9 O 0.04268(16) 0.477(2) 0.8372(18) 0.013(2) 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 Ta1 0.0060(3) 0.0074(3) 0.0116(3) -0.0003(2) 0.0003(2) -0.0006(2) Nb1 0.0060(3) 0.0074(3) 0.0116(3) -0.0003(2) 0.0003(2) -0.0006(2) Ta2 0.0062(3) 0.0069(3) 0.0093(3) 0.0003(2) -0.00038(19) 0.0007(2) Nb2 0.0062(3) 0.0069(3) 0.0093(3) 0.0003(2) -0.00038(19) 0.0007(2) Sb1 0.0115(6) 0.0087(6) 0.0214(7) 0.000 0.0062(4) 0.000 Sb2 0.0161(4) 0.0103(4) 0.0133(5) -0.0012(3) 0.0035(3) -0.0056(3) Sb3 0.0126(4) 0.0096(5) 0.0163(5) 0.0014(3) -0.0049(3) -0.0035(3) O1 0.002(3) 0.013(4) 0.020(5) 0.001(4) -0.002(3) 0.001(3) O2 0.005(4) 0.014(4) 0.015(5) -0.002(3) -0.002(3) -0.002(3) O3 0.008(4) 0.013(4) 0.017(5) 0.010(4) 0.002(3) 0.000(3) O4 0.005(4) 0.017(5) 0.013(4) 0.001(4) -0.004(3) -0.006(3) O5 0.006(4) 0.008(4) 0.015(4) 0.002(3) 0.002(3) -0.005(3) O6 0.011(4) 0.006(4) 0.017(5) 0.002(3) -0.003(3) 0.000(3) O7 0.012(4) 0.012(4) 0.015(5) -0.002(3) 0.001(3) 0.001(3) O8 0.012(4) 0.016(5) 0.020(5) -0.006(4) -0.002(4) 0.000(4) O9 0.008(4) 0.017(5) 0.015(5) 0.007(4) -0.002(3) 0.002(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ta1 O3 1.840(9) . ? Ta1 O9 1.868(10) 6_566 ? Ta1 O5 1.956(8) . ? Ta1 O2 2.026(9) . ? Ta1 O3 2.047(9) 6 ? Ta1 O9 2.068(9) . ? Ta2 O8 1.844(10) 6_565 ? Ta2 O7 1.875(9) . ? Ta2 O6 1.914(9) 6 ? Ta2 O8 2.039(10) . ? Ta2 O6 2.057(10) . ? Ta2 O1 2.125(9) . ? Sb1 O2 2.019(10) 5_557 ? Sb1 O2 2.019(10) 6 ? Sb1 O2 2.243(9) 2_556 ? Sb1 O2 2.243(9) . ? Sb2 O4 1.979(9) . ? Sb2 O4 2.019(9) 6_556 ? Sb2 O7 2.069(10) . ? Sb2 O4 2.438(8) 4_545 ? Sb3 O1 2.012(9) 6_566 ? Sb3 O5 2.030(9) 6_565 ? Sb3 O1 2.117(10) . ? Sb3 O5 2.381(9) . ? O1 Sb3 2.012(9) 6_565 ? O2 Sb1 2.019(10) 5_557 ? O3 Nb1 2.047(9) 6_556 ? O3 Ta1 2.047(9) 6_556 ? O4 Sb2 2.019(9) 6 ? O4 Sb2 2.438(8) 4 ? O5 Sb3 2.030(9) 6_566 ? O6 Nb2 1.914(9) 6_556 ? O6 Ta2 1.914(9) 6_556 ? O8 Nb2 1.844(10) 6_566 ? O8 Ta2 1.844(10) 6_566 ? O9 Nb1 1.868(10) 6_565 ? O9 Ta1 1.868(10) 6_565 ? 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 O3 Ta1 O9 97.3(4) . 6_566 ? O3 Ta1 O5 95.9(4) . . ? O9 Ta1 O5 97.5(4) 6_566 . ? O3 Ta1 O2 94.9(4) . . ? O9 Ta1 O2 92.3(4) 6_566 . ? O5 Ta1 O2 164.4(4) . . ? O3 Ta1 O3 91.04(15) . 6 ? O9 Ta1 O3 171.1(4) 6_566 6 ? O5 Ta1 O3 84.6(4) . 6 ? O2 Ta1 O3 83.9(4) . 6 ? O3 Ta1 O9 171.7(4) . . ? O9 Ta1 O9 89.89(18) 6_566 . ? O5 Ta1 O9 87.4(4) . . ? O2 Ta1 O9 80.5(4) . . ? O3 Ta1 O9 81.6(4) 6 . ? O8 Ta2 O7 98.3(4) 6_565 . ? O8 Ta2 O6 96.3(4) 6_565 6 ? O7 Ta2 O6 98.6(4) . 6 ? O8 Ta2 O8 91.40(14) 6_565 . ? O7 Ta2 O8 88.6(4) . . ? O6 Ta2 O8 168.5(4) 6 . ? O8 Ta2 O6 168.3(4) 6_565 . ? O7 Ta2 O6 90.8(4) . . ? O6 Ta2 O6 89.4(2) 6 . ? O8 Ta2 O6 81.5(4) . . ? O8 Ta2 O1 92.1(4) 6_565 . ? O7 Ta2 O1 166.0(4) . . ? O6 Ta2 O1 89.5(4) 6 . ? O8 Ta2 O1 81.7(4) . . ? O6 Ta2 O1 77.8(4) . . ? O2 Sb1 O2 92.0(5) 5_557 6 ? O2 Sb1 O2 85.7(3) 5_557 2_556 ? O2 Sb1 O2 74.7(4) 6 2_556 ? O2 Sb1 O2 74.7(4) 5_557 . ? O2 Sb1 O2 85.7(3) 6 . ? O2 Sb1 O2 151.8(5) 2_556 . ? O4 Sb2 O4 91.1(3) . 6_556 ? O4 Sb2 O7 89.5(4) . . ? O4 Sb2 O7 81.4(4) 6_556 . ? O4 Sb2 O4 87.4(2) . 4_545 ? O4 Sb2 O4 70.3(4) 6_556 4_545 ? O7 Sb2 O4 151.5(4) . 4_545 ? O1 Sb3 O5 91.0(4) 6_566 6_565 ? O1 Sb3 O1 89.3(3) 6_566 . ? O5 Sb3 O1 77.1(4) 6_565 . ? O1 Sb3 O5 71.5(3) 6_566 . ? O5 Sb3 O5 81.9(3) 6_565 . ? O1 Sb3 O5 151.2(4) . . ? Sb3 O1 Sb3 110.8(4) 6_565 . ? Sb3 O1 Ta2 134.1(5) 6_565 . ? Sb3 O1 Ta2 114.7(4) . . ? Sb1 O2 Ta1 137.4(5) 5_557 . ? Sb1 O2 Sb1 105.3(4) 5_557 . ? Ta1 O2 Sb1 117.0(5) . . ? Ta1 O3 Nb1 147.8(5) . 6_556 ? Ta1 O3 Ta1 147.8(5) . 6_556 ? Sb2 O4 Sb2 118.6(4) . 6 ? Sb2 O4 Sb2 131.7(4) . 4 ? Sb2 O4 Sb2 109.7(4) 6 4 ? Ta1 O5 Sb3 139.2(5) . 6_566 ? Ta1 O5 Sb3 119.8(4) . . ? Sb3 O5 Sb3 100.6(3) 6_566 . ? Nb2 O6 Ta2 132.6(5) 6_556 . ? Ta2 O6 Ta2 132.6(5) 6_556 . ? Ta2 O7 Sb2 147.7(6) . . ? Nb2 O8 Ta2 153.2(5) 6_566 . ? Ta2 O8 Ta2 153.2(5) 6_566 . ? Nb1 O9 Ta1 138.2(5) 6_565 . ? Ta1 O9 Ta1 138.2(5) 6_565 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 4.312 _refine_diff_density_min -4.349 _refine_diff_density_rms 0.540