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_7227485
_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            'C33 H56 Cu2 N12 O44 Si W12'
_chemical_formula_weight         3686
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_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
_cell_angle_beta                 97.928(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2377(13)
_cell_length_b                   18.6736(16)
_cell_length_c                   25.291(2)
_cell_measurement_reflns_used    5890
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.577
_cell_measurement_theta_min      1.669
_cell_volume                     7127.6(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0782
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40789
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.577
_diffrn_reflns_theta_min         1.669
_exptl_absorpt_coefficient_mu    19.975
_exptl_absorpt_correction_T_max  0.050
_exptl_absorpt_correction_T_min  0.038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       clavate
_exptl_crystal_F_000             6560
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.121
_refine_diff_density_min         -1.314
_refine_diff_density_rms         0.308
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     927
_refine_ls_number_reflns         13391
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0293P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9112
_reflns_number_total             13391
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra25156k2.cif
_cod_data_source_block           compound-2
_cod_original_cell_volume        7127.7(11)
_cod_database_code               7227485
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.123
_shelx_estimated_absorpt_t_max   0.154
_shelx_res_checksum              45974