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_7229564
_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, C31 H38 Cu3 N8 O12, C H2 O, 4(H2 O)'
_chemical_formula_sum            'C32 H53 Cr Cu3 Mo6 N8 O41'
_chemical_formula_weight         2024.08
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-10-12
_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                61.168(4)
_cell_angle_beta                 70.680(5)
_cell_angle_gamma                88.297(5)
_cell_formula_units_Z            1
_cell_length_a                   9.624(2)
_cell_length_b                   13.716(4)
_cell_length_c                   14.061(3)
_cell_measurement_reflns_used    3639
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.04
_cell_measurement_theta_min      2.27
_cell_volume                     1515.4(6)
_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      296.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0307
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8589
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         1.716
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.508
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0690 before and 0.0432 after correction. The Ratio of minimum to maximum transmission is 0.6975. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.218
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.354
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         5309
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0547
_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^)+(0.1241P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4327
_reflns_number_total             5309
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01092c2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7229561--7229565.cif.'
_cod_database_code               7229564
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.770
_shelx_estimated_absorpt_t_min   0.705
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 H17B-C17
 0.93 with sigma of 0.02
 H17A-C17
 0.93 with sigma of 0.02
 H5WA-H8
 2.13 with sigma of 0.02
 C14-N4 \\sim N4-C15 \\sim C15A-N14 \\sim N14-C14A
 with sigma of 0.02
 C13-O1F \\sim O1F-C13A
 with sigma of 0.02
 H16B-O1A \\sim H17A-O2A
 with sigma of 0.02
 H17B-O2A \\sim H16A-O1A
 with sigma of 0.02
 H17A-H17B \\sim H16A-H16B
 with sigma of 0.02
3. Rigid bond restraints
 O1A, O2W, C16, C17, O2A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C14A \\sim C14: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C16 \\sim O1A \\sim C17 \\sim O2A \\sim O2W: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O2W \\sim O1A \\sim C16 \\sim O2A \\sim C17: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 N4, C13, H13, N14, C15, H15A, H15B, C14, H14A, H14B, H14C, C14A, H14D, H14E,
 H14F, C13A, H13A, C15A, H15D, H15E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(N14)=Sof(C13A)=Sof(H13A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(N4)=Sof(C13)=Sof(H13)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(2)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(2)
 Fixed Sof: H5(0.83333) H7(0.83333) H8(0.83333) O1A(0.5) O2W(0.5) H2WA(0.5)
 H2WB(0.5) C16(0.5) H16A(0.5) H16B(0.5) O2A(0.5) C17(0.5) H17A(0.5) H17B(0.5)
7.a Free rotating group:
 O4W(H4WA,H4WB), O5W(H5WA,H5WB)
7.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
7.c Ternary CH refined with riding coordinates:
 O5(H5), O7(H7), O8(H8)
7.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C2(H2A), C1(H1), C12(H12), C11(H11), C10(H10), C9(H9),
 C13(H13), C13A(H13A)
7.e X=CH2 refined with riding coordinates:
 C16(H16A,H16B)
7.f Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C15A(H15D,
 H15E,H15F)
;
_olex2_submission_special_instructions 'No special instructions were received'