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_7040493
_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 H116 N6 O100 V28'
_chemical_formula_sum            'C103 H201.5 N10.5 O101 V28'
_chemical_formula_weight         4629.55
_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   difmap
_audit_creation_date             2016-08-14
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.07.08 svn.r3312 for OlexSys, GUI svn.r5203)
;
_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                   21.9542(12)
_cell_length_b                   21.9542(12)
_cell_length_c                   21.9542(12)
_cell_measurement_reflns_used    2741
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.212
_cell_measurement_theta_min      2.272
_cell_volume                     10581.6(10)
_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      298.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1185
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30780
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.045
_diffrn_reflns_theta_max         25.045
_diffrn_reflns_theta_min         1.855
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellowish-brown
_exptl_crystal_colour_primary    yellowish-brown
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       block
_exptl_crystal_F_000             4690
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1757
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0927P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1179
_reflns_number_total             1757
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02764d2.cif
_cod_data_source_block           1490972_sq
_cod_depositor_comments
;Adding full bibliography for 7040492--7040493.cif.

 Adding full bibliography for 7040492--7040493.cif.
;
_cod_original_cell_volume        10581.6(17)
_cod_original_formula_sum        'C103 H201.50 N10.50 O101 V28'
_cod_database_code               7040493
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(9) 0.45(9)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Rigid bond restraints
 C5, O3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C6, O2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O5, C4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C2, C3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
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 0.002
5. Others
 Fixed Sof: H1WA(0.16667) H1WB(0.16667) H6A(0.5) H6B(0.5) H6C(0.5) H4A(0.5)
 H4B(0.5) H4C(0.5) N1(0.25) H5A(0.5) H5C(0.5)
6.a Riding coordinates:
 O1W(H1WA,H1WB), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              57801
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'