Synthesis and Characterization of a Series of [M2(β-SiW8O31)2](n-) Clusters and Mechanistic Insight into the Reorganization of {β-SiW8O31} into {α-SiW9O34}.
Winter, Ross S.; Long, De-Liang; Cronin, Leroy; Inorganic chemistry 54 (2015) 4151–4155; doi:10.1021/acs.inorgchem.5b00405

data_4342752
_publ_section_title
;
 Synthesis and Characterization of a Series of [M2(\b-SiW8O31)2](n-)
 Clusters and Mechanistic Insight into the Reorganization of {\b-SiW8O31}
 into {\a-SiW9O34}.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4151
_journal_page_last               4155
_journal_paper_doi               10.1021/acs.inorgchem.5b00405
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'Cu2 H99 Na15 O111 Si2 W16'
_chemical_formula_weight         5345.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                71.425(2)
_cell_angle_beta                 80.487(2)
_cell_angle_gamma                69.964(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7071(6)
_cell_length_b                   13.4442(7)
_cell_length_c                   17.5941(9)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.45
_cell_volume                     2461.2(2)
_computing_cell_refinement       Apex2
_computing_data_collection       Apex2
_computing_data_reduction        Apex2
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex II Quasar'
_diffrn_measurement_method       '\w & \p scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36128
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.082
_diffrn_source                   '1uS Microfocus x-ray'
_exptl_absorpt_coefficient_mu    19.259
_exptl_absorpt_correction_T_max  0.093
_exptl_absorpt_correction_T_min  0.048
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    3.607
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             2422
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.63
_refine_diff_density_min         -1.34
_refine_diff_density_rms         0.19
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         9638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.001
_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^+14.8328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8873
_reflns_number_total             9638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Cu2W16.cif
_cod_data_source_block           rw851b1
_cod_depositor_comments
;Adding full bibliography for 4342749--4342755.cif.

The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4342752
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.249
_shelx_estimated_absorpt_t_max   0.446
_shelx_res_checksum              35500
_shelx_hkl_checksum              4163