Polyoxometalate, Cationic Cluster and γ-Cyclodextrin. From Primary Interactions to Supramolecular Hybrid Materials.
Moussawi, Mhamad Aly; Leclerc-Laronze, Nathalie; Floquet, Sébastien; Abramov, Pavel A.; Sokolov, Maxim Nailyevich; Cordier, Stephane; Ponchel, Anne; Monflier, Eric; Bricout, Herve; Landy, David; Haouas, Mohamed; Marrot, Jerome; Cadot, Emmanuel; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b07317

data_4126341
_publ_section_title
;
 Polyoxometalate, Cationic Cluster and &#xF067;\g-Cyclodextrin. From
 Primary Interactions to Supramolecular Hybrid Materials.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b07317
_journal_year                    2017
_chemical_formula_sum            'C96 H200 Br14 O100 Ta6'
_chemical_formula_weight         5158.99
_space_group_crystal_system      tetragonal
_space_group_IT_number           97
_space_group_name_Hall           'I 4 2'
_space_group_name_H-M_alt        'I 4 2 2'
_symmetry_space_group_name_Hall  'I 4 2'
_symmetry_space_group_name_H-M   'I 4 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8984(11)
_cell_length_b                   23.8984(11)
_cell_length_c                   34.8186(19)
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      2.34
_cell_volume                     19886.1(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1648
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            129482
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.105
_diffrn_reflns_theta_max         25.105
_diffrn_reflns_theta_min         2.067
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    6.189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             10016
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.4679
_refine_diff_density_max         2.674
_refine_diff_density_min         -2.828
_refine_diff_density_rms         0.320
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.096(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         8872
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0858P)^2^+828.7637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2121
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7074
_reflns_number_total             8872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cdr02b.cif
_cod_data_source_block           cdr02b
_cod_original_cell_volume        19886(2)
_cod_database_code               4126341
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.371
_shelx_estimated_absorpt_t_max   0.708
_exptl_absorpt_special_details   'Blessing, Acta Cryst. (1995) A51, 33-38'
_shelx_res_checksum              33801
_shelx_hkl_checksum              1997