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_7229562
_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
'Co Cr H14 Mo6 O28, Cr H6 Mo6 O24, C24 H30 Co2 N6 O12, 7(H2 O), 2(C2 H6 O)'
_chemical_formula_sum            'C28 H76 Co3 Cr2 Mo12 N6 O73'
_chemical_formula_weight         3097.01
_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             2017-10-14
_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                106.0600(10)
_cell_angle_beta                 97.8180(10)
_cell_angle_gamma                111.8130(10)
_cell_formula_units_Z            1
_cell_length_a                   12.3636(5)
_cell_length_b                   13.0466(5)
_cell_length_c                   14.4949(5)
_cell_measurement_reflns_used    8814
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.283
_cell_measurement_theta_min      2.14
_cell_volume                     2009.83(13)
_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 0.996
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14801
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.283
_diffrn_reflns_theta_min         1.799
_exptl_absorpt_coefficient_mu    2.789
_exptl_absorpt_correction_T_max  0.677
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1503
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.893
_refine_diff_density_min         -1.327
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         9866
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0365P)^2^+2.6676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8622
_reflns_number_total             9866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01092c2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7229561--7229565.cif.'
_cod_database_code               7229562
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H23 of O23, H24 of O24, H27 of O27, H9A of O9, H10A of O10,
   H12A of O12, {H5WA,H5WB} of O5W, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H1WA,H1WB} of O1W, {H2WA,H2WB} of O2W, H30 of O30,
  H29 of O29, {H4WA,H4WB} of O4W, {H3WA,H3WB} of O3W, {H8WA,H8WB} of O8W, {H7WA,
  H7WB} of O7W, {H6WA,H6WB} of O6W
2. Restrained distances
 C16-C15 = C13-C14
 1.52 with sigma of 0.02
 C16-O29 = O30-C13
 1.42 with sigma of 0.02
 H10B-O10W
 0.85 with sigma of 0.001
 O10W-H10C
 0.85 with sigma of 0.001
 O30-C13 = C16-O29
 1.402 with sigma of 0.02
 H10C-H10B
 1.389 with sigma of 0.02
 C13-C14
 1.52 with sigma of 0.02
 C15-O29 = C14-O30
 2.52 with sigma of 0.04
3. Rigid bond restraints
 O29, C15, C16, O30, C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O29 \\sim C15 \\sim C16 \\sim O30 \\sim C13 \\sim C14: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: O6W(0.5) H6WA(0.5) H6WB(0.5) O29(0.5) H29(0.5) C15(0.5) H15A(0.5)
 H15B(0.5) H15C(0.5) C16(0.5) H16A(0.5) H16B(0.5) O30(0.5) H30(0.5) C13(0.5)
 H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
6.a Riding coordinates:
 O5W(H5WA,H5WB)
6.b Free rotating group:
 O6W(H6WA,H6WB), O7W(H7WA,H7WB), O8W(H8WA,H8WB)
6.c Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
6.d Ternary CH refined with riding coordinates:
 O23(H23), O24(H24), O27(H27), O9(H9A), O10(H10A), O12(H12A)
6.e Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C13(H13A,H13B)
6.f Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12)
6.g Tetrahedral OH refined with riding coordinates:
 O29(H29), O30(H30)
6.h Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C)
;
_olex2_submission_special_instructions 'No special instructions were received'