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_7232073
_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         'C14 H40 Cr2 Cu3 Mo12 N12 O52, 6(H2 O)'
_chemical_formula_sum            'C14 H52 Cr2 Cu3 Mo12 N12 O58'
_chemical_formula_weight         2762.57
_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             2018-12-12
_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                96.9610(10)
_cell_angle_beta                 99.6830(10)
_cell_angle_gamma                98.5300(10)
_cell_formula_units_Z            1
_cell_length_a                   6.4711(3)
_cell_length_b                   15.2046(6)
_cell_length_c                   16.6977(7)
_cell_measurement_reflns_used    7344
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.366
_cell_measurement_theta_min      2.503
_cell_volume                     1583.48(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0141
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8907
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         1.989
_exptl_absorpt_coefficient_mu    3.727
_exptl_absorpt_correction_T_max  0.9871
_exptl_absorpt_correction_T_min  0.5982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1323
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         5390
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+1.3408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0474
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5030
_reflns_number_total             5390
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01971a2.cif
_cod_data_source_block           y_CCDC5
_cod_depositor_comments
'Adding full bibliography for 7232067--7232073.cif.'
_cod_database_code               7232073
_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,H) groups, All O(H,H,H,H,H,H,H,H) groups
2. Restrained distances
 O15-H15 = O21-H21 = O17-H17 = O23-H23 = O18-H18 = O19-H19
 0.85 with sigma of 0.02
 H23-H5WA
 2.2 with sigma of 0.02
3.a Free rotating group:
 O3W(H15,H17,H18,H19,H21,H23,H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
3.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
3.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C7(H7)
;
_shelx_res_checksum              14316
_olex2_submission_special_instructions 'No special instructions were received'