Structural features of selenate based {Mo132} keplerate capsules
Korenev, Vladimir S.; Dorovatovskii, Pavel V.; Lazarenko, Vladimir A.; Abramov, Pavel A.; Sokolov, Maxim N.; CrystEngComm 24 (2022) 321–329; doi:10.1039/D1CE01121A

data_7243919
_publ_section_title
;
 Structural features of selenate based {Mo132} keplerate capsules
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              321
_journal_page_last               329
_journal_paper_doi               10.1039/D1CE01121A
_journal_volume                  24
_journal_year                    2022
_chemical_formula_sum            'Mo132 N25.8 O628.56 Se30'
_chemical_formula_weight         25451.30
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   32.7739(5)
_cell_length_b                   32.7739(5)
_cell_length_c                   73.5789(11)
_cell_measurement_reflns_used    29572
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.2580
_cell_measurement_theta_min      3.4940
_cell_volume                     68444.8(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       88
_diffrn_reflns_limit_l_min       -73
_diffrn_reflns_number            51926
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.350
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.319
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.025
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_description       block
_exptl_crystal_F_000             35319
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.093
_refine_diff_density_min         -3.353
_refine_diff_density_rms         0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1288
_refine_ls_number_reflns         27808
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1345P)^2^+512.9554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2187
_refine_ls_wR_factor_ref         0.2442
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18484
_reflns_number_total             27808
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            d1ce01121a3.cif
_cod_data_source_block           sm119_a
_cod_depositor_comments
'Adding full bibliography for 7243919--7243920.cif.'
_cod_original_cell_volume        68445(2)
_cod_original_formula_sum        'Mo132 N25.80 O628.56 Se30'
_cod_database_code               7243919
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.464
_shelx_estimated_absorpt_t_max   0.583
_shelx_res_checksum              28247
_shelx_hkl_checksum              64172