Surfactant-assisted Synthesis and Electrochemical Properties of Unprecedented Polyoxometalate-constituting Metal-Organic Nanocaged Framework
Yang, Xiya; Zhu, Pei-Pei; Ren, Jing; Chen, Yu-Hao; Li, Xiao; Sha, Jing-Quan; Jiang, Jianzhuang; Chemical Communications  (2018) –; doi:10.1039/C8CC08559E

data_7122679
_publ_section_title
;
 Surfactant-assisted Synthesis and Electrochemical Properties of
 Unprecedented Polyoxometalate-constituting Metal-Organic Nanocaged
 Framework
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08559E
_journal_year                    2018
_chemical_formula_moiety         'C6 H6 N9 O13 V0.25 W3 Zn3, H2 O'
_chemical_formula_sum            'C6 H8 N9 O14 V0.25 W3 Zn3'
_chemical_formula_weight         1190.64
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-25 deposited with the CCDC.
2018-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.7950(19)
_cell_length_b                   18.7950(19)
_cell_length_c                   12.808(3)
_cell_measurement_reflns_used    3498
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.260
_cell_measurement_theta_min      2.898
_cell_volume                     4524.5(12)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11519
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.532
_exptl_absorpt_coefficient_mu    18.501
_exptl_absorpt_correction_T_max  0.079
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.496
_exptl_crystal_description       block
_exptl_crystal_F_000             4294
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         4.970
_refine_diff_density_min         -6.080
_refine_diff_density_rms         0.478
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2094
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0866P)^2^+692.7762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1853
_reflns_number_total             2088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08559e2.cif
_cod_data_source_block           ZnVW12-trz
_cod_original_cell_volume        4524.3(13)
_cod_database_code               7122679
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Riding coordinates:
 O1W(H1W)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3)
;
_shelx_res_checksum              58422
_olex2_submission_special_instructions 'No special instructions were received'