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_7124778
_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         'C144 H168 O100 S4 V24'
_chemical_formula_sum            'C183.5 H280.5 N9.5 O101.5 S4 V24'
_chemical_formula_weight         5594.46
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.983(5)
_cell_length_b                   28.983(5)
_cell_length_c                   25.744(5)
_cell_measurement_reflns_used    5219
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      16.508
_cell_measurement_theta_min      2.221
_cell_volume                     21625(7)
_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  0.0881
_diffrn_reflns_av_unetI/netI     0.1292
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60011
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.499
_diffrn_reflns_theta_max         24.499
_diffrn_reflns_theta_min         0.993
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.874
_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    0.859
_exptl_crystal_F_000             5752
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 2632 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.763
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         17997
_refine_ls_number_restraints     976
_refine_ls_restrained_S_all      0.761
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.950
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7332
_reflns_number_total             17997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc04583a2.cif
_cod_data_source_block           VMOP-15_sq
_cod_original_cell_volume        21625(9)
_cod_original_formula_sum        'C183.50 H280.50 N9.50 O101.50 S4 V24'
_cod_database_code               7124778
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.877
_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
 O7-C22A = O7-C22B
 1.35 with sigma of 0.01
 O12-C33A = O12-C33B
 1.35 with sigma of 0.01
3. Rigid bond restraints
 S1, O4
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 O13, C1
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C5, C6
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C8, C13
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C17, C20
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 V1, O19
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C17, C20
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C13
\\sim C10 \\sim C11 \\sim C12 \\sim C21 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C28 \\sim C22A \\sim C23A \\sim C24A \\sim
C25A \\sim C26A \\sim C33A \\sim C22B \\sim C23B \\sim C24B \\sim C25B \\sim
C26B \\sim C33B \\sim C27 \\sim C9 \\sim C29 \\sim C30 \\sim C31A \\sim C32A
\\sim C31B \\sim C32B \\sim C34 \\sim C35 \\sim C36: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.03
Uanis(C3) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C22A) \\sim Ueq, Uanis(C22B) \\sim Ueq, Uanis(C33A) \\sim Ueq,
Uanis(C33B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C32A) = Uanis(C32B)
Uanis(C33A) = Uanis(C33B)
Uanis(C22A) = Uanis(C22B)
5. Others
 Fixed Sof: C22A(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C23A(0.5) H23A(0.5)
 C24A(0.5) H24A(0.5) C25A(0.5) H25A(0.5) C26A(0.5) H26A(0.5) C33A(0.5)
 H33A(0.5) H33B(0.5) H33C(0.5) C22B(0.5) H22D(0.5) H22E(0.5) H22F(0.5)
 C23B(0.5) H23B(0.5) C24B(0.5) H24B(0.5) C25B(0.5) H25B(0.5) C26B(0.5)
 H26B(0.5) C33B(0.5) H33D(0.5) H33E(0.5) H33F(0.5) C31A(0.5) H31A(0.5)
 H31B(0.5) H31C(0.5) C32A(0.5) H32A(0.5) H32B(0.5) H32C(0.5) C31B(0.5)
 H31D(0.5) H31E(0.5) H31F(0.5) C32B(0.5) H32D(0.5) H32E(0.5) H32F(0.5)
6.a Riding coordinates:
 C22A(H22A,H22B,H22C), C33A(H33A,H33B,H33C), C22B(H22D,H22E,H22F), C33B(H33D,
 H33E,H33F), C31A(H31A,H31B,H31C), C32A(H32A,H32B,H32C), C31B(H31D,H31E,H31F),
 C32B(H32D,H32E,H32F)
6.b Me refined with riding coordinates:
 C3(H3A,H3B,H3C), C29(H29A,H29B,H29C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C13(H13), C10(H10), C12(H12), C15(H15), C16(H16),
 C18(H18), C19(H19), C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C23B(H23B),
  C24B(H24B), C25B(H25B), C26B(H26B), C9(H9)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              34019
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'