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_4126342
_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            'C48 H116 Cl3.5 K Na8.5 O120 P2 W18'
_chemical_formula_weight         6343.23
_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                   17.671(4)
_cell_length_b                   24.533(5)
_cell_length_c                   40.756(8)
_cell_measurement_temperature    100(2)
_cell_volume                     17669(6)
_computing_cell_refinement       'XDS package'
_computing_data_collection       'XDS package'
_computing_data_reduction        'XDS package'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'PROXIMA 2A - Synchrotron SOLEIL'
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72925
_diffrn_reflns_av_R_equivalents  0.1099
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            184384
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.482
_diffrn_reflns_theta_max         25.482
_diffrn_reflns_theta_min         0.994
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    12.237
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.385
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             11592
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         3.153
_refine_diff_density_min         -5.437
_refine_diff_density_rms         0.497
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.26(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         29038
_refine_ls_number_restraints     452
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.0973
_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^)+(0.0818P)^2^+1659.0830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2362
_refine_ls_wR_factor_ref         0.2925
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                21536
_reflns_number_total             29038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nl373.cif
_cod_data_source_block           nl373
_cod_original_formula_sum        'C48 H116 Cl3.50 K Na8.50 O120 P2 W18'
_cod_database_code               4126342
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.441
_shelx_estimated_absorpt_t_max   0.640
_shelx_res_checksum              95866
_shelx_hkl_checksum              91763
_shelx_fab_checksum              37035