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_7229561
_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_moiety
'Cr H5 Mo6 O24, 2.5(C8.8 H8.4 N2.4 O0.8), 0.5(H4 O2)'
_chemical_formula_sum            'C22 H28 Cr Mo6 N6 O27'
_chemical_formula_weight         1436.14
_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   mixed
_audit_creation_date             2017-09-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-11-10 deposited with the CCDC.
2017-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                77.8710(10)
_cell_angle_beta                 77.2590(10)
_cell_angle_gamma                79.4860(10)
_cell_formula_units_Z            1
_cell_length_a                   6.0210(5)
_cell_length_b                   12.3200(9)
_cell_length_c                   13.2940(10)
_cell_measurement_reflns_used    3571
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.253
_cell_measurement_theta_min      1.51
_cell_volume                     930.75(12)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0142
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6844
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.253
_diffrn_reflns_theta_min         1.596
_exptl_absorpt_coefficient_mu    2.347
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         4541
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0230
_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^)+(0.0290P)^2^+0.1837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4048
_reflns_number_total             4541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01092c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7229561--7229565.cif.'
_cod_database_code               7229561
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1-C6 \\sim O1A-C6A
 with sigma of 0.02
 N1-C1 \\sim N1A-C1A
 with sigma of 0.02
 N1-C2 \\sim N1A-C2A
 with sigma of 0.02
 C1-C5 \\sim C1A-C5A
 with sigma of 0.02
 N2-C5 \\sim N2A-C5A
 with sigma of 0.02
 N2-C6 \\sim N2A-C6A
 with sigma of 0.02
 C2-C3 \\sim C2A-C3A
 with sigma of 0.02
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 N3-C11 \\sim N3A-C8A
 with sigma of 0.02
 N3-C10 \\sim N3A-C9A
 with sigma of 0.02
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 C6-C7 \\sim C6A-C7A
 with sigma of 0.02
 C7-C11 \\sim C7A-C8A
 with sigma of 0.02
 C7-C8 \\sim C7A-C11A
 with sigma of 0.02
 C9-C10 \\sim C10A-C9A
 with sigma of 0.02
 C9-C8 \\sim C10A-C11A
 with sigma of 0.02
 O1-N2 \\sim O1A-N2A
 with sigma of 0.04
 O1-C7 \\sim O1A-C7A
 with sigma of 0.04
 N1-C3 \\sim N1A-C3A
 with sigma of 0.04
 N1-C5 \\sim N1A-C5A
 with sigma of 0.04
 C1-N2 \\sim C1A-N2A
 with sigma of 0.04
 C1-C2 \\sim C1A-C2A
 with sigma of 0.04
 C1-C4 \\sim C1A-C4A
 with sigma of 0.04
 N2-C4 \\sim N2A-C4A
 with sigma of 0.04
 N2-C7 \\sim N2A-C7A
 with sigma of 0.04
 C2-C4 \\sim C2A-C4A
 with sigma of 0.04
 C3-C5 \\sim C3A-C5A
 with sigma of 0.04
 N3-C7 \\sim N3A-C7A
 with sigma of 0.04
 N3-C9 \\sim N3A-C10A
 with sigma of 0.04
 C5-C6 \\sim C5A-C6A
 with sigma of 0.04
 C6-C11 \\sim C6A-C8A
 with sigma of 0.04
 C6-C8 \\sim C6A-C11A
 with sigma of 0.04
 C7-C9 \\sim C7A-C10A
 with sigma of 0.04
 C11-C10 \\sim C8A-C9A
 with sigma of 0.04
 C11-C8 \\sim C8A-C11A
 with sigma of 0.04
 C10-C8 \\sim C9A-C11A
 with sigma of 0.04
3. Rigid bond restraints
 C6, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Rigid body (RIGU) restrains
 O1A, N1A, N2A, N3A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1, N1, N2, N3, C1, C11, C2, C3, C4, C5, C6, C7, C8, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H8B(0.5) O1(0.8) N1(0.8) H1(0.8) N2(0.8) H2(0.8) N3(0.8) H3(0.4)
 C1(0.8) H1A(0.8) C11(0.8) H11(0.8) C2(0.8) H2A(0.8) C3(0.8) H3A(0.8) C4(0.8)
 H4(0.8) C5(0.8) C6(0.8) C7(0.8) C8(0.8) H8(0.8) C9(0.8) H9(0.8) C10(0.8)
 H10(0.8) O1A(0.2) N1A(0.2) H1AC(0.15) N2A(0.2) H2AA(0.2) N3A(0.2) H3AA(0.15)
 C1A(0.2) H1AB(0.2) C2A(0.2) H2AB(0.2) C3A(0.2) H3AB(0.2) C4A(0.2) H4A(0.2)
 C5A(0.2) C6A(0.2) C7A(0.2) C8A(0.2) H8A(0.2) C9A(0.2) H9A(0.2) C10A(0.2)
 H10A(0.2) C11A(0.2) H11A(0.2) H1WA(0.5) H1WB(0.5)
6.a Free rotating group:
 O1W(H1WA,H1WB)
6.b Ternary CH refined with riding coordinates:
 O4(H4B), O8(H8B), O9(H9B)
6.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), C1(H1A), C11(H11), C2(H2A), C3(H3A), C4(H4), C8(H8),
 C9(H9), C10(H10), N1A(H1AC), N2A(H2AA), N3A(H3AA), C1A(H1AB), C2A(H2AB),
 C3A(H3AB), C4A(H4A), C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A)
;
_olex2_submission_special_instructions 'No special instructions were received'