Characteristic features of polytypism in compounds with the La~18~W~10~O~57~-type structure
Novikova, Nataliya E.; Sorokin, Timofei A.; Antipin, Alexander M.; Bolotina, Nadezhda B.; Alekseeva, Olga A.; Sorokina, Nataliya I.; Voronkova, Valentina I.; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619006107

data_2021639
_publ_section_title
;
 Characteristic features of polytypism in compounds with the
 La~18~W~10~O~57~-type structure
;
_journal_coeditor_code           SK3724
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619006107
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'La30 W17 O96'
_chemical_formula_moiety         'La30 O96 W17'
_chemical_formula_sum            'La15 O48 W8.5'
_chemical_formula_weight         4414.3
_space_group_IT_number           150
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 2"'
_symmetry_space_group_name_H-M   'P 3 2 1'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   9.0363(3)
_cell_length_b                   9.0363(3)
_cell_length_c                   27.3412(3)
_cell_measurement_reflns_used    37067
_cell_measurement_temperature    293.00(10)
_cell_measurement_theta_max      53.22
_cell_measurement_theta_min      4.01
_cell_volume                     1933.43(9)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2018)
;
_computing_publication_material
;
<i>JANA2006</i> (Petricek <i>et al.</i>, 2014)
;
_computing_structure_refinement
;
<i>JANA2006</i> (Petricek <i>et al.</i>, 2014)
;
_computing_structure_solution
;
<i>JANA2006</i> (Petricek <i>et al.</i>, 2014)
;
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
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_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, EosS2 with high theta cut'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1896
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            195204
_diffrn_reflns_theta_full        53.47
_diffrn_reflns_theta_max         53.47
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    41.356
_exptl_absorpt_correction_T_max  0.074
_exptl_absorpt_correction_T_min  0.003
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Rigaku OD, 2018), based on crystal shape and size
(Clark & Reid, 1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    7.5824
_exptl_crystal_description       plate
_exptl_crystal_F_000             3736
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.331
_exptl_crystal_size_min          0.156
_refine_diff_density_max         11.12
_refine_diff_density_min         -9.39
_refine_ls_abs_structure_details
;
4435 of Friedel pairs used in the refinement (Flack, 1983)
;
_refine_ls_abs_structure_Flack   0.119(9)
_refine_ls_extinction_coef       48E2(2)
_refine_ls_extinction_method
;
B-C type 2 (Becker & Coppens, 1974)
;
_refine_ls_goodness_of_fit_gt    1.98
_refine_ls_goodness_of_fit_ref   1.95
_refine_ls_number_constraints    0
_refine_ls_number_parameters     159
_refine_ls_number_reflns         11140
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.0335
_refine_ls_shift/su_mean         0.0039
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F)+0.0001F^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                10049
_reflns_number_total             11140
_reflns_threshold_expression     I>3\s(I)
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_cod_data_source_block           II
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_cod_database_fobs_code 2021639