Two polyoxovanadate-based metal-organic polyhedra with undiscovered “Near-miss Johnson Solid” geometry†
Gong, Yaru; Tao, Yanli; Xu, Na; Sun, Chun-Yi; Wang, Xinlong; Su, Zhong-Min; Chemical Communications  (2019) –; doi:10.1039/C9CC05984A

data_7123978
_publ_section_title
;
 Two polyoxovanadate-based metal-organic polyhedra with undiscovered
 &#x201C;Near-miss Johnson Solid&#x201D; geometry&#x2020;
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05984A
_journal_year                    2019
_chemical_formula_moiety         'C108 H36 Cl4 Nb4 O176 S4 V40, 3(O4 S)'
_chemical_formula_sum            'C168 H276 Cl4 N30 Nb4 O180 S7 V40'
_chemical_formula_weight         8371.63
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_symmetry_space_group_name_Hall  'I -4 2'
_symmetry_space_group_name_H-M   'I -4 2 m'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-08-01
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-01 deposited with the CCDC.    2019-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.854(3)
_cell_length_b                   21.854(3)
_cell_length_c                   44.273(6)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.34
_cell_measurement_theta_min      2.50
_cell_volume                     21145(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            54581
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.109
_diffrn_reflns_theta_max         25.109
_diffrn_reflns_theta_min         2.948
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       block
_exptl_crystal_F_000             8396
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.761
_refine_diff_density_min         -1.994
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9693
_refine_ls_number_restraints     1094
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0647
_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^)+(0.1410P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1754
_refine_ls_wR_factor_ref         0.1979
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                7098
_reflns_number_total             9693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05984a2.cif
_cod_data_source_block           VMOP_27
_cod_original_cell_volume        21145(6)
_cod_database_code               7123978
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.92(6)
 0.08(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 O24-V1
 2.4 with sigma of 0.02
 V2-O25
 2.4 with sigma of 0.02
 Nb1-O26
 2.35 with sigma of 0.02
 S2-O26 = S1-O26
 1.45 with sigma of 0.02
 S1-O25
 1.45 with sigma of 0.02
 S1-O24 = S2-O24
 1.45 with sigma of 0.02
 S2-O27
 1.45 with sigma of 0.02
 V3-O27
 2.45 with sigma of 0.02
 S3-O29 = S3-O28 = S3-O30 = S3-O31
 1.45 with sigma of 0.02
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 C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim O1 \\sim O2
\\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9 \\sim O10 \\sim
O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17 \\sim O18 \\sim
O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25 \\sim O26 \\sim
O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31 \\sim O32 \\sim O33 \\sim S1 \\sim
S2 \\sim S3 \\sim S4: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.03
5. Others
 Fixed Sof: S1(0.25) S2(0.25) O25(0.5) S3(0.25) O28(0.25) O29(0.25) O30(0.25)
 O31(0.25) S4(0.125) O32(0.25) O33(0.25)
6.a Riding coordinates:
 C7(H7)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C11(H11), C12(H12), C14(H14)
;
_shelx_res_checksum              47287
_shelx_fab_checksum              16945
_olex2_submission_special_instructions 'No special instructions were received'