Supramolecular Host–Guest Assemblies of [M6Cl14]2–, M = Mo, W, Clusters with γ-Cyclodextrin for the Development of CLUSPOMs
Ivanov, Anton A.; Abramov, Pavel A.; Haouas, Mohamed; Molard, Yann; Cordier, Stéphane; Falaise, Clément; Cadot, Emmanuel; Shestopalov, Michael A.; Inorganics 11 (2023) 77–; doi:10.3390/inorganics11020077

data_1568593
_publ_section_title
;
 Supramolecular Host--Guest Assemblies of [M6Cl14]2--, M = Mo, W, Clusters
 with \g-Cyclodextrin for the Development of CLUSPOMs
;
_journal_issue                   2
_journal_name_full               Inorganics
_journal_page_first              77
_journal_paper_doi               10.3390/inorganics11020077
_journal_volume                  11
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_sum            'C96 H110 Cl42 Mo18 O97'
_chemical_formula_weight         6031.65
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                116.936(2)
_cell_angle_beta                 116.807(2)
_cell_angle_gamma                90.0120(10)
_cell_formula_units_Z            1
_cell_length_a                   17.8167(3)
_cell_length_b                   17.9076(3)
_cell_length_c                   19.7519(4)
_cell_measurement_reflns_used    44279
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.4550
_cell_measurement_theta_min      3.5170
_cell_volume                     4846.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.868
_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  0.0228
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            85634
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.676
_diffrn_reflns_theta_min         3.246
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.791
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_description       block
_exptl_crystal_F_000             2932
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         4.983
_refine_diff_density_min         -3.690
_refine_diff_density_rms         0.445
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.28(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1314
_refine_ls_number_reflns         44790
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1486
_refine_ls_R_factor_gt           0.1443
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+478.8877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3181
_refine_ls_wR_factor_ref         0.3202
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.868
_reflns_number_gt                42664
_reflns_number_total             44790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            all_CD.cif
_cod_data_source_block           mo
_cod_original_cell_volume        4846.01(19)
_cod_database_code               1568593
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.663
_shelx_estimated_absorpt_t_max   0.716
_shelx_res_checksum              39154
_shelx_hkl_checksum              97452