Coding the Assembly of Polyoxotungstates with a Programmable Reaction System.
Ruiz de la Oliva, Andreu; Sans, Victor; Miras, Haralampos N.; Long, De-Liang; Cronin, Leroy; Inorganic chemistry 56 (2017) 5089–5095; doi:10.1021/acs.inorgchem.7b00206

data_4345822
_publ_section_title
;
 Coding the Assembly of Polyoxotungstates with a Programmable Reaction
 System.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5089
_journal_page_last               5095
_journal_paper_doi               10.1021/acs.inorgchem.7b00206
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'H66 K8 Na4 O105 W22'
_chemical_formula_weight         6195.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 112.8560(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.2229(16)
_cell_length_b                   12.7409(5)
_cell_length_c                   19.5968(8)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.20
_cell_volume                     9254.4(6)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       '\w & \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8492
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.910
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    27.728
_exptl_absorpt_correction_T_max  0.4034
_exptl_absorpt_correction_T_min  0.1231
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.447
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             10920
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_refine_diff_density_max         3.68
_refine_diff_density_min         -4.14
_refine_diff_density_rms         0.79
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         8492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0575
_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^)+(0.1026P)^2^+1663.0555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1583
_refine_ls_wR_factor_ref         0.1739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7555
_reflns_number_total             8492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00206_si_002.cif
_cod_data_source_block           ar168e
_cod_database_code               4345822
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.123
_shelx_estimated_absorpt_t_max   0.403
_shelx_res_checksum              50216
_shelx_hkl_checksum              19890