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_7232071
_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
'3(Cr H6 Mo6 O24), C14 H48 Cd3 N12 O14, 16(H2 O)'
_chemical_formula_sum            'C14 H98 Cd3 Cr3 Mo18 N12 O102'
_chemical_formula_weight         4287.16
_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             2018-12-12
_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                90
_cell_angle_beta                 95.280(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.1041(11)
_cell_length_b                   11.6957(8)
_cell_length_c                   27.930(2)
_cell_measurement_reflns_used    4534
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.24
_cell_volume                     5238.3(6)
_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 0.997
_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  0.0611
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            38320
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.321
_diffrn_reflns_theta_min         1.406
_exptl_absorpt_coefficient_mu    3.095
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SABABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4108
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.127
_refine_diff_density_min         -4.800
_refine_diff_density_rms         0.385
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         13016
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1302P)^2^+56.6939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2085
_refine_ls_wR_factor_ref         0.2391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8245
_reflns_number_total             13016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01971a2.cif
_cod_data_source_block           y_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7232067--7232073.cif.'
_cod_database_code               7232071
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H36 of O36, H32 of O32, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups, H16 of O16, H20 of O20, H21 of O21, H22 of O22, H23 of
  O23, H24 of O24, H35 of O35
2. Restrained distances
 C7-C6
 2.4 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N1, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Riding coordinates:
 O20(H20), O21(H21), O22(H22), O23(H23), O24(H24), O32(H32), O35(H35),
 O36(H36), O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB),
 O5W(H5WA,H5WB), O6W(H6WA,H6WB), O7W(H7WA,H7WB), O8W(H8WA,H8WB), O9W(H9WA,H9WB),
  O10W(H10A,H10B), O11W(H11A,H11B), O12W(H12A,H12B), O13W(H13A,H13B), O14W(H14A,
 H14B), O15W(H15A,H15B)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'