Blurring the line between addenda and heteroatoms in a giant polyoxotungstotellurite
Liu, Jin-Xiu; Izarova, Natalya V.; Kögerler, Paul; Chemical Communications  (2019) –; doi:10.1039/C9CC04623B

data_7123986
_publ_section_title
;
 Blurring the line between addenda and heteroatoms in a giant
 polyoxotungstotellurite
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04623B
_journal_year                    2019
_chemical_formula_sum            'Cl1.5 H454 Li30.5 Na51 O597 Te48 W78'
_chemical_formula_weight         31912.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-04-05 deposited with the CCDC.    2019-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.7502(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   58.0985(5)
_cell_length_b                   17.79804(15)
_cell_length_c                   61.6119(6)
_cell_measurement_reflns_used    101340
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.1760
_cell_measurement_theta_min      3.2210
_cell_volume                     57382.6(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4623
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova (Mo) X-ray Source'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1254
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       69
_diffrn_reflns_limit_h_min       -69
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_limit_l_min       -73
_diffrn_reflns_number            518548
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         3.142
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    18.132
_exptl_absorpt_correction_T_max  0.1920
_exptl_absorpt_correction_T_min  0.0460
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
 multifaceted crystal model
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             56704
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.159
_refine_diff_density_max         3.889
_refine_diff_density_min         -3.227
_refine_diff_density_rms         0.376
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1743
_refine_ls_number_reflns         50577
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+3857.5986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                36849
_reflns_number_total             50577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04623b2.cif
_cod_data_source_block           tew3_sq_s
_cod_original_formula_sum        'Cl1.50 H454 Li30.50 Na51 O597 Te48 W78'
_cod_database_code               7123986
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.076
_shelx_estimated_absorpt_t_max   0.161
_shelx_res_checksum              72553
_shelx_fab_checksum              996