The crystal structures of the mixed-valence tellurium oxysalts tlapallite, (Ca,Pb)3CaCu6[Te4+3Te6+O12]2(Te4+O3)2(SO4)2 . 3H2O, and carlfriesite, CaTe4+2Te6+O8
Owen P. Missen; Anthony R. Kampf; Stuart J. Mills; Robert M. Housley; John Spratt; Mark D. Welch; Mark F. Coolbaugh; Joe Marty; Marek Chorazewicz; Cristiano Ferraris; Mineralogical Magazine 83 (2019) 439–549; doi:10.1180/mgm.2019.9

data_1560195
_publ_section_title
;
 The crystal structures of the mixed-valence tellurium oxysalts
 tlapallite, (Ca,Pb)3CaCu6[Te4+3Te6+O12]2(Te4+O3)2(SO4)2 . 3H2O, and
 carlfriesite, CaTe4+2Te6+O8
;
_journal_name_full               'Mineralogical Magazine'
_journal_page_first              439
_journal_page_last               549
_journal_paper_doi               10.1180/mgm.2019.9
_journal_volume                  83
_journal_year                    2019
_chemical_formula_moiety
'Cu6 O30 Pb0.39 Sb0.27 Te9.73, 2(O4 S), 3(H2 O), 3.613(Ca)'
_chemical_formula_sum            'Ca1.81 Cu3 H3 O20.5 Pb0.19 S Sb0.13 Te4.87'
_chemical_formula_weight         1303.50
_chemical_name_common            tlapallite
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_atom_sites_solution_hydrogens   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   9.1219(17)
_cell_length_b                   9.1219(17)
_cell_length_c                   11.9320(9)
_cell_measurement_reflns_used    660
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.241
_cell_measurement_theta_min      3.093
_cell_volume                     859.8(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'three-circle diffractometer, Rigaku R-Axis Rapid II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4092
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        23.241
_diffrn_reflns_theta_max         23.241
_diffrn_reflns_theta_min         3.093
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    14.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    5.035
_exptl_crystal_description       'partial hexagonal plate'
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.004
_exptl_transmission_factor_max   0.944
_exptl_transmission_factor_min   0.592
_refine_diff_density_max         0.848
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.195
_refine_ls_abs_structure_details
;
 Flack x determined using 283 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(4)
_refine_ls_extinction_coef       0.0003(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         832
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+5.2653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0625
_reflns_Friedel_coverage         0.651
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                786
_reflns_number_total             832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CIF_tlapallite_Missen_et_al.cif
_cod_data_source_block           14584-84
_cod_original_cell_volume        859.8(3)
_cod_original_formula_sum        'Ca1.81 H3 Cu3 O20.50 Pb0.19 S Sb0.13 Te4.87'
_cod_database_code               1560195
_shelx_estimated_absorpt_t_min   0.592
_shelx_estimated_absorpt_t_max   0.944
_shelx_res_checksum              91279
_shelx_hkl_checksum              68164