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_7124777
_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         'C72 H120 O100 S4 V24'
_chemical_formula_sum            'C106.5 H221.5 N8.5 O100.5 S4 V24'
_chemical_formula_weight         4580.21
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_hydrogens   mixed
_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                   21.848(5)
_cell_length_b                   21.848(5)
_cell_length_c                   19.081(5)
_cell_measurement_reflns_used    4594
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.419
_cell_measurement_theta_min      2.341
_cell_volume                     9108(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      298.15
_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  0.0594
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26422
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.318
_exptl_absorpt_coefficient_mu    1.311
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             4680
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 2077 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         8051
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0523P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5561
_reflns_number_total             8051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc04583a2.cif
_cod_data_source_block           VMOP-14_sq
_cod_original_cell_volume        9108(5)
_cod_original_formula_sum        'C106.50 H221.50 N8.50 O100.50 S4 V24'
_cod_database_code               7124777
_shelx_estimated_absorpt_t_max   0.808
_shelx_estimated_absorpt_t_min   0.761
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18-O13
 1.35 with sigma of 0.01
3. Rigid bond restraints
 O13, C18
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11A \\sim C14A \\sim C11B \\sim C14B \\sim C12 \\sim C13 \\sim
C15 \\sim C16 \\sim C17 \\sim C18: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C14A) = Uanis(C14B)
5. Others
 Fixed Sof: C11A(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C14A(0.5) H14A(0.5)
 H14B(0.5) H14C(0.5) C11B(0.5) H11D(0.5) H11E(0.5) H11F(0.5) C14B(0.5)
 H14D(0.5) H14E(0.5) H14F(0.5)
6.a Riding coordinates:
 C11A(H11A,H11B,H11C), C14A(H14A,H14B,H14C), C11B(H11D,H11E,H11F), C14B(H14D,
 H14E,H14F)
6.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              19878
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'