Solvent-controlled synthesis of various Anderson-type polyoxometalate-based metal‒organic complexes with excellent capacity for the chromatographic separation of dyes
Wang, Xiu-Li; Song, Ge; Lin, Hong-Yan; Wang, Xiang; Liu, Guo-Cheng; Rong, Xing; CrystEngComm 20 (2018) 51–; doi:10.1039/C7CE01092C

data_7229565
_publ_section_title
;
 Solvent-controlled synthesis of various Anderson-type
 polyoxometalate-based metal--organic complexes with excellent capacity
 for the chromatographic separation of dyes
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              51
_journal_paper_doi               10.1039/C7CE01092C
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C24 H52 Cl Cr Cu3 Mo6 N6 O45'
_chemical_formula_weight         1998.42
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-11-10 deposited with the CCDC.
2017-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.9220(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.323(2)
_cell_length_b                   9.8415(9)
_cell_length_c                   25.627(3)
_cell_measurement_reflns_used    3446
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.55
_cell_measurement_theta_min      2.26
_cell_volume                     5866.0(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Olex2 (Dolomanov et al., 2009)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16311
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.844
_diffrn_reflns_theta_min         1.751
_exptl_absorpt_coefficient_mu    2.638
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0491 before and 0.0362 after correction. The Ratio of minimum to maximum transmission is 0.8610. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.263
_exptl_crystal_description       block
_exptl_crystal_F_000             3912
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         5652
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0477P)^2^+11.3172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4118
_reflns_number_total             5652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01092c2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7229561--7229565.cif.'
_cod_original_cell_volume        5865.9(11)
_cod_database_code               7229565
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.648
_shelx_estimated_absorpt_t_max   0.817
_shelx_res_checksum              9036