A series of 0D to 3D Anderson-type polyoxometalate-based compounds obtained under ambient and hydrothermal conditions
Ying, Jun; Chen, Ya-Guang; Wang, Xiu-Yan; CrystEngComm 21 (2019) 1168–; doi:10.1039/C8CE01971A

data_7232068
_publ_section_title
;
 A series of 0D to 3D Anderson-type polyoxometalate-based compounds
 obtained under ambient and hydrothermal conditions
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1168
_journal_paper_doi               10.1039/C8CE01971A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C12 H24 Cr Cu Mo6 N12 O25, 5(H2 O), O'
_chemical_formula_sum            'C12 H34 Cr Cu Mo6 N12 O31'
_chemical_formula_weight         1533.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-18 deposited with the CCDC.
2019-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2068(5)
_cell_length_b                   21.0385(13)
_cell_length_c                   24.5141(15)
_cell_measurement_reflns_used    3101
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.822
_cell_measurement_theta_min      2.558
_cell_volume                     4207.8(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            29130
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.428
_diffrn_reflns_theta_min         1.279
_exptl_absorpt_coefficient_mu    2.582
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2972
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.890
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         9606
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0354P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6185
_reflns_number_total             9606
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01971a2.cif
_cod_data_source_block           y
_cod_depositor_comments
'Adding full bibliography for 7232067--7232073.cif.'
_cod_database_code               7232068
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O22-H22 = O17-H17 = O10-H10 = O23-H23 = O16-H16 = O20-H20
 0.85 with sigma of 0.02
3. Others
 Fixed Sof: O7W(0.5) O7WA(0.5) O6W(0.5) H6WA(0.5) H6WB(0.5) O26(0.5) H26A(0.5)
 H26B(0.5)
4.a Riding coordinates:
 O5W(H5WA,H5WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O6W(H6WA,H6WB), O26(H26A,H26B)
4.b Free rotating group:
 O2W(H2WA,H2WB)
4.c Rotating group:
 O1W(H1WA,H1WB)
4.d Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C9(H9A,H9B), C10(H10A,H10B)
4.e Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12)
;
_shelx_res_checksum              79332
_olex2_submission_special_instructions 'No special instructions were received'