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_7243920
_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            'C21.8 H130.8 Cl3 Mo132 N65.4 O581.4 Se30'
_chemical_formula_weight         25751.54
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2021-08-09 deposited with the CCDC.	2021-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   50.337(7)
_cell_length_b                   50.337(7)
_cell_length_c                   61.099(12)
_cell_measurement_reflns_used    969
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.23
_cell_volume                     134072(4)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'ShelXle (H\"ubschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 12.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rayonix SX-165 CCD'
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_monochromator  'Double Crystal Monochromator'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.79272
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       59
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_k_max       65
_diffrn_reflns_limit_k_min       -65
_diffrn_reflns_limit_l_max       79
_diffrn_reflns_limit_l_min       -78
_diffrn_reflns_number            287412
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        28.401
_diffrn_reflns_theta_max         31.004
_diffrn_reflns_theta_min         1.428
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    4.160
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_description       block
_exptl_crystal_F_000             71914
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.805
_refine_diff_density_min         -4.054
_refine_diff_density_rms         0.303
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1294
_refine_ls_number_reflns         34107
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.0921
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2929
_refine_ls_wR_factor_ref         0.3187
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23366
_reflns_number_total             34107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01121a4.cif
_cod_data_source_block           wk627
_cod_depositor_comments
'Adding full bibliography for 7243919--7243920.cif.'
_cod_original_cell_volume        134072(46)
_cod_original_formula_sum
'C21.80 H130.80 Cl3 Mo132 N65.40 O581.40 Se30'
_cod_database_code               7243920
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.368
_shelx_estimated_absorpt_t_max   0.490
_shelx_res_checksum              12137