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_1560194
_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         'O16 Te6, 2(Ca)'
_chemical_formula_sum            'Ca O8 Te3'
_chemical_formula_weight         550.88
_chemical_name_common            carlfriesite
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   .
_cell_angle_alpha                90
_cell_angle_beta                 111.913(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9866(7)
_cell_length_b                   5.67205(19)
_cell_length_c                   12.2351(14)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.024
_cell_measurement_theta_min      3.590
_cell_volume                     642.98(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0384
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4142
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.024
_diffrn_reflns_theta_min         3.590
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    14.327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 2001)'
_exptl_crystal_colour            'translucent white'
_exptl_crystal_density_diffrn    5.691
_exptl_crystal_description       blade
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   0.870
_exptl_transmission_factor_min   0.239
_refine_diff_density_max         2.500
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.470
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.298
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.298
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+1.2698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0538
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                874
_reflns_number_total             928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CIF_carlfriesite_Missen_et_al.cif
_cod_data_source_block           cf
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               1560194
_shelx_estimated_absorpt_t_min   0.239
_shelx_estimated_absorpt_t_max   0.870
_shelx_res_checksum              23049
_shelx_hkl_checksum              51802