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_4126343
_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_absolute_configuration ad
_chemical_formula_sum            'C96 H206 Cl1.2 Cs Na6.2 O165 P2 W18'
_chemical_formula_weight         7689.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   17.2589(16)
_cell_length_b                   31.374(3)
_cell_length_c                   41.297(3)
_cell_measurement_reflns_used    9493
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.33
_cell_volume                     22362(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_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    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.1167
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            249509
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.061
_diffrn_reflns_theta_max         25.061
_diffrn_reflns_theta_min         2.183
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    9.529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.284
_exptl_crystal_description       platelet
_exptl_crystal_F_000             14430
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.4689
_refine_diff_density_max         6.344
_refine_diff_density_min         -6.723
_refine_diff_density_rms         0.575
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.213(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2330
_refine_ls_number_reflns         38493
_refine_ls_number_restraints     2915
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1451
_refine_ls_R_factor_gt           0.1302
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+4675.1694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3100
_refine_ls_wR_factor_ref         0.3181
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                32586
_reflns_number_total             38493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nl86.cif
_cod_data_source_block           nl86
_cod_original_formula_sum        'C96 H206 Cl1.20 Cs Na6.20 O165 P2 W18'
_cod_database_code               4126343
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.162
_shelx_estimated_absorpt_t_max   0.832
_exptl_absorpt_special_details   'Blessing, Acta Cryst. (1995) A51, 33-38'
_shelx_res_checksum              51714
_shelx_hkl_checksum              4082