Incorporating polyoxometalates and organic ligands to pursue 3d‒4f heterometallic clusters: a series of {Cr4Ln4} clusters stabilized by phthalic acid and [SiW12O40]4−
Gu, Ya-Nan; Zhao, Dan; Yu, Hao; Ge, Rui; Li, Zhong; Tian, Chong-Bian; Li, Xin-Xiong; Sun, Yan-Qiong; Zheng, Shou-Tian; RSC Advances 9 (2019) 13543–; doi:10.1039/C9RA01731C

data_7232707
_publ_section_title
;
 Incorporating polyoxometalates and organic ligands to pursue 3d--4f
 heterometallic clusters: a series of {Cr4Ln4} clusters stabilized by
 phthalic acid and [SiW12O40]4&#x2212;
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              13543
_journal_paper_doi               10.1039/C9RA01731C
_journal_volume                  9
_journal_year                    2019
_chemical_formula_sum            'C32 H16 Ce4 Cl Cr4 Cs2 O83.5 Si W12'
_chemical_formula_weight         5040.49
_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_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-03-13 deposited with the CCDC.    2019-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                81.6102(15)
_cell_angle_beta                 82.6279(16)
_cell_angle_gamma                89.5941(17)
_cell_formula_units_Z            2
_cell_length_a                   13.5174(11)
_cell_length_b                   13.5216(11)
_cell_length_c                   29.869(2)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      50.216
_cell_measurement_theta_min      5.071
_cell_volume                     5355.9(7)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruke duo apx2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            41293
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.135
_diffrn_reflns_theta_max         25.135
_diffrn_reflns_theta_min         1.390
_exptl_absorpt_coefficient_mu    15.682
_exptl_absorpt_correction_T_max  2.3
_exptl_absorpt_correction_T_min  0.9
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    3.125
_exptl_crystal_description       block
_exptl_crystal_F_000             4466
_platon_squeeze_details          ' ?'
_refine_diff_density_max         5.215
_refine_diff_density_min         -4.921
_refine_diff_density_rms         0.453
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1267
_refine_ls_number_reflns         18701
_refine_ls_number_restraints     558
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0897P)^2^+336.8908P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1818
_refine_ls_wR_factor_ref         0.1897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16241
_reflns_number_total             18701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra01731c2.cif
_cod_data_source_block           1
_cod_original_cell_volume        5356.0(8)
_cod_original_formula_sum        'C32 H16 Ce4 Cl Cr4 Cs2 O83.50 Si W12'
_cod_database_code               7232707
_shelx_shelxl_version_number     2018/3