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_1568594
_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 rm
_chemical_formula_moiety         'Cl13.3 Mo6, 3(C48 H56 O40), 18(O), 0.7(Cl)'
_chemical_formula_sum            'C144 H168 Cl14 Mo6 O140'
_chemical_formula_weight         5210.71
_space_group_crystal_system      tetragonal
_space_group_IT_number           90
_space_group_name_Hall           'P 4ab 2ab'
_space_group_name_H-M_alt        'P 4 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   23.8060(10)
_cell_length_b                   23.8060(10)
_cell_length_c                   22.8310(10)
_cell_measurement_reflns_used    9012
_cell_measurement_temperature    200.15
_cell_measurement_theta_max      28.299
_cell_measurement_theta_min      2.472
_cell_volume                     12938.9(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1215
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            257159
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.068
_diffrn_reflns_theta_max         25.068
_diffrn_reflns_theta_min         2.420
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1213 before and 0.1053 after correction.
The Ratio of minimum to maximum transmission is 0.8080.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       plate
_exptl_crystal_F_000             5284
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.349
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         11500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0749
_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^)+(0.1333P)^2^+49.8256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2134
_refine_ls_wR_factor_ref         0.2199
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                10490
_reflns_number_total             11500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            all_CD.cif
_cod_data_source_block           iaa065_0m_pl
_cod_original_cell_volume        12938.9(12)
_cod_database_code               1568594
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.950
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.93(7)
 0.07(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(Cl10) = Uanis(Cl11) = Uanis(Cl8) = Uanis(Cl7) = Uanis(Cl6) = Uanis(Cl9)
4. Others
 Fixed Sof: Mo1(0.85) Mo3(0.175) Mo2(0.175) Mo5(0.15) Mo4(0.15) O3W(0.5)
 O2W(0.5) O1W(0.5) Cl1(0.85) Cl4(0.7) Cl5(0.7) Cl3(0.175) Cl10(0.15) Cl7(0.15)
 Cl2(0.175) Cl8(0.15) Cl9(0.15) Cl6(0.15) Cl11(0.15)
5.a Riding coordinates:
 C1A(H1AA,H1AB), C3A(H3A), C2A(H2A), C1B(H1B), C2C(H2C), C4C(H4C), C11C(H11C),
 C12C(H12D)
5.b Ternary CH refined with riding coordinates:
 C4A(H4A), C5A(H5A), C6A(H6A), C9A(H9A), C10A(H10A), C11A(H11A), C8A(H8A),
 C12A(H12A), C2B(H2B), C3B(H3B), C5B(H5B), C4B(H4B), C7B(H7B), C8B(H8B),
 C9B(H9B), C10B(H10B), C11B(H11B), C3C(H3C), C5C(H5C), C10C(H10C), C9C(H9C),
 C8C(H8C), C6C(H6C)
5.c Secondary CH2 refined with riding coordinates:
 C7A(H7AA,H7AB), C6B(H6BA,H6BB), C12B(H12B,H12C), C1C(H1CA,H1CB), C7C(H7CA,H7CB)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              79224
_shelx_hkl_checksum              4998
_shelx_fab_checksum              30461
_olex2_submission_special_instructions 'No special instructions were received'