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_7232067
_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
'2(Al H6 Mo6 O24), 2(C4 H22 Al Cu Mo6 N4 O24), 4(C4 H16 Cu N4), 47(H2 O)'
_chemical_formula_sum            'C24 H214 Al4 Cu6 Mo24 N24 O143'
_chemical_formula_weight         5919.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-12-17
_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                 98.3780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.5506(15)
_cell_length_b                   13.4067(7)
_cell_length_c                   22.7853(12)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.316
_cell_measurement_theta_min      2.171
_cell_volume                     8326.2(8)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0313
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            30337
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.345
_diffrn_reflns_theta_min         1.693
_exptl_absorpt_coefficient_mu    2.631
_exptl_absorpt_correction_T_max  0.729
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5808
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.000257(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         10389
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+16.1436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8602
_reflns_number_total             10389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01971a2.cif
_cod_data_source_block           j
_cod_depositor_comments
'Adding full bibliography for 7232067--7232073.cif.'
_cod_database_code               7232067
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O18-H18 = O23-H23 = O22-H22
 0.85 with sigma of 0.02
 H12-O12 = H10-O10 = H11-O11
 0.85 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N4, N5, C3, C3A, C4, C4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H4BC)=Sof(H4BD)=Sof(H5BC)=Sof(H5BD)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=
 Sof(H4AC)=Sof(H4AD)=1-FVAR(1)
 Sof(H4AA)=Sof(H4AB)=Sof(H5AA)=Sof(H5AB)=Sof(C3)=Sof(H3C)=Sof(H3D)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=FVAR(1)
 Fixed Sof: O12W(0.25) H12A(0.25) H12B(0.25)
5.a Riding coordinates:
 O3W(H3WA,H3WB), O6W(H6WA,H6WB), O7W(H7WA,H7WB), O8W(H8WA,H8WB), O10W(H10W),
 O12W(H12A,H12B), O13W(H13A,H13B)
5.b Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB), O9W(H9WA,
 H9WB), O11W(H11A,H11B)
5.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), C1(H1C,H1D), C2(H2C,H2D), N3(H3A,H3B), N4(H4AA,
 H4AB), N4(H4BC,H4BD), N5(H5AA,H5AB), N5(H5BC,H5BD), N6(H6A,H6B), C3(H3C,H3D),
 C3A(H3AA,H3AB), C4(H4A,H4B), C4A(H4AC,H4AD), C5(H5A,H5B), C6(H6C,H6D)
;
_shelx_res_checksum              79532
_olex2_submission_special_instructions 'No special instructions were received'