Anderson-like alkoxo-polyoxovanadate clusters serving as unprecedented second building units to construct metal-organic polyhedra.
Zhang, Yu-Teng; Wang, Xin-Long; Li, Shuang-Bao; Gong, Ya-Ru; Song, Bai-Qiao; Shao, Kui-Zhan; Su, Zhong-Min; Chemical communications (Cambridge, England) 52 (2016) 9632–9635; doi:10.1039/c6cc04583a

data_7124775
_publ_section_title
;
 Anderson-like alkoxo-polyoxovanadate clusters serving as unprecedented
 second building units to construct metal-organic polyhedra.
;
_journal_issue                   62
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9632
_journal_page_last               9635
_journal_paper_doi               10.1039/c6cc04583a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C84 H108 N6 O100 S4 V24'
_chemical_formula_sum            'C123.5 H250.5 N15.5 O101.5 S4 V24'
_chemical_formula_weight         4927.68
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-21 deposited with the CCDC.
2016-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   21.841(5)
_cell_length_b                   21.841(5)
_cell_length_c                   21.841(5)
_cell_measurement_reflns_used    5012
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.477
_cell_measurement_theta_min      2.284
_cell_volume                     10419(4)
_computing_cell_refinement       'Bruker SAINT v8.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v8.34a'
_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    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30504
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.985
_diffrn_reflns_theta_max         24.985
_diffrn_reflns_theta_min         1.318
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_crystal_colour            yellowish-brown
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       block
_exptl_crystal_F_000             5056
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1725
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0541P)^2^+3.5331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1521
_reflns_number_total             1725
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc04583a2.cif
_cod_data_source_block           VMOP-12_sq
_cod_original_cell_volume        10419(7)
_cod_original_formula_sum        'C123.50 H250.50 N15.50 O101.50 S4 V24'
_cod_database_code               7124775
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.785
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(6) 0.47(6)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
O6 \\sim C5: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H4A(0.5) H4B(0.5) H4C(0.5) H6B(0.5) H6A(0.5) H6C(0.5) H5A(0.5)
 H5B(0.5) H5C(0.5) N1(0.25)
5.a Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C6(H6B,H6A,H6C), C5(H5A,H5B,H5C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              93881
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'