Encapsulation of a {Cu16} cluster containing four [Cu4O4] cubanes within an isopolyoxometalate {W44} cluster
Cronin, Lee; Zhan, Caihong; Busche, Christoph; Long, Deliang; Molina, Pedro I.; Winter, Ross S.; Chem. Commun.  (2017) –; doi:10.1039/C7CC03544F

data_7120242
_publ_section_title
;
 Encapsulation of a {Cu16} cluster containing four [Cu4O4] cubanes within
 an isopolyoxometalate {W44} cluster
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC03544F
_journal_year                    2017
_chemical_formula_sum            'C8 H208 Cu16 Na16 O260 W44'
_chemical_formula_weight         13939.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-30 deposited with the CCDC.
2017-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8487(8)
_cell_length_b                   40.9986(16)
_cell_length_c                   27.4044(10)
_cell_measurement_reflns_used    9718
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.30
_cell_volume                     24547.9(16)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_molecular_graphics    Diamond
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II Quazar CCD'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            194846
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         0.894
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    22.027
_exptl_absorpt_correction_T_max  0.0926
_exptl_absorpt_correction_T_min  0.0529
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.772
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             24928
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         6.16
_refine_diff_density_min         -4.72
_refine_diff_density_rms         0.49
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1288
_refine_ls_number_reflns         24124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+3877.9519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17716
_reflns_number_total             24124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc03544f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct method' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7120242
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.217
_shelx_estimated_absorpt_t_max   0.406
_shelx_res_checksum              48455