Synthesis, structures, and magnetic properties of metal-organic polyhedra based on unprecedented {V7} isopolyoxometalate clusters.
Zhang, Yu-Teng; Li, Shuang-Bao; Wang, Xin-Long; Gong, Ya-Ru; Shao, Kui-Zhan; Su, Zhong-Min; Dalton transactions (Cambridge, England : 2003) 45 (2016) 14898–14901; doi:10.1039/c6dt02764d

data_7040492
_publ_section_title
;
 Synthesis, structures, and magnetic properties of metal-organic polyhedra
 based on unprecedented {V7} isopolyoxometalate clusters.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14898
_journal_page_last               14901
_journal_paper_doi               10.1039/c6dt02764d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C84 H140 O100 V28'
_chemical_formula_sum            'C102.5 H193.5 N4.5 O100.5 V28'
_chemical_formula_weight         4523.43
_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_Hall           'I -4 2 3'
_space_group_name_H-M_alt        'I -4 3 m'
_symmetry_space_group_name_Hall  'I -4 2 3'
_symmetry_space_group_name_H-M   'I -4 3 m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-08-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-14 deposited with the CCDC.
2016-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.911(5)
_cell_length_b                   21.911(5)
_cell_length_c                   21.911(5)
_cell_measurement_reflns_used    3295
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.407
_cell_measurement_theta_min      2.276
_cell_volume                     10519(4)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0963
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29227
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.979
_diffrn_reflns_theta_max         24.979
_diffrn_reflns_theta_min         1.859
_exptl_absorpt_coefficient_mu    1.260
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellowish-brown
_exptl_crystal_colour_primary    yellowish-brown
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1735
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0559P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.848
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1445
_reflns_number_total             1735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02764d2.cif
_cod_data_source_block           1490971_sq
_cod_depositor_comments
;Adding full bibliography for 7040492--7040493.cif.

 Adding full bibliography for 7040492--7040493.cif.
;
_cod_original_cell_volume        10519(7)
_cod_original_formula_sum        'C102.50 H193.50 N4.50 O100.50 V28'
_cod_database_code               7040492
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.769
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.95(6) 0.05(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Rigid bond restraints
 V2, O1W
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 C6, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.005
5. Rigid body (RIGU) restrains
 C6, O5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: H1WA(0.16667) H1WB(0.16667) H4A(0.5) H4B(0.5) H4C(0.5) H5A(0.5)
 H5B(0.5) H5C(0.5) H6A(0.5) H6B(0.5) H6C(0.5)
7.a Riding coordinates:
 O1W(H1WA,H1WB)
7.b Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              70345
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'