Using a flexible bis(pyrazol) ligand to construct four new Keggin-based compounds: syntheses, structures and properties
Tian, Aixiang; Ni, Huaiping; Ji, Xuebin; Tian, Yan; Liu, Guocheng; Ying, Jun; RSC Adv. 7 (2017) 5774–; doi:10.1039/C6RA25156K

data_7227484
_publ_section_title
;
 Using a flexible bis(pyrazol) ligand to construct four new Keggin-based
 compounds: syntheses, structures and properties
;
_journal_issue                   10
_journal_name_full               'RSC Adv.'
_journal_page_first              5774
_journal_paper_doi               10.1039/C6RA25156K
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C44 H100 Cu2 N16 O58 Si W12'
_chemical_formula_weight         4142.6
_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_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-20 deposited with the CCDC.
2017-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 117.176(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   35.318(5)
_cell_length_b                   23.532(5)
_cell_length_c                   23.250(5)
_cell_measurement_reflns_used    7241
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.72
_cell_measurement_theta_min      1.65
_cell_volume                     17190(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            56211
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         26.723
_diffrn_reflns_theta_min         1.649
_exptl_absorpt_coefficient_mu    16.570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.957
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             13760
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_exptl_transmission_factor_max   0.083
_exptl_transmission_factor_min   0.071
_refine_diff_density_max         5.769
_refine_diff_density_min         -2.026
_refine_diff_density_rms         0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         18241
_refine_ls_number_restraints     478
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+686.4167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12596
_reflns_number_total             18259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra25156k2.cif
_cod_data_source_block           compound-3
_cod_database_code               7227484
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.154
_shelx_estimated_absorpt_t_max   0.190
_shelx_res_checksum              99184
_platon_squeeze_void_probe_radius 1.20