Self-Assembly of Goldberg Polyhedra from a Concave [WV<sub>5</sub>O<sub>11</sub>(RCO<sub>2</sub>)<sub>5</sub>(SO<sub>4</sub>)]<sup>3-</sup> Building Block with 5-Fold Symmetry.
Zhang, Yuteng; Gan, Hongmei; Qin, Chao; Wang, Xinlong; Su, Zhongmin; Zaworotko, Michael J.; Journal of the American Chemical Society 140 (2018) 17365–17368; doi:10.1021/jacs.8b10866

data_4133534
_publ_section_title
;
 Self-Assembly of Goldberg Polyhedra from a Concave
 [WV<sub>5</sub>O<sub>11</sub>(RCO<sub>2</sub>)<sub>5</sub>(SO<sub>4</sub>)]<sup>3-</sup>
 Building Block with 5-Fold Symmetry.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17365
_journal_page_last               17368
_journal_paper_doi               10.1021/jacs.8b10866
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C350 O264 V60 W12'
_chemical_formula_sum            'C450 H540 N45 O323.5 S12 V65 W15'
_chemical_formula_weight         18208.81
_space_group_crystal_system      tetragonal
_space_group_IT_number           131
_space_group_name_Hall           '-P 4c 2'
_space_group_name_H-M_alt        'P 42/m m c'
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   43.2511(16)
_cell_length_b                   43.2511(16)
_cell_length_c                   39.0469(13)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      57.000
_cell_measurement_theta_min      1.953
_cell_volume                     73043(5)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.02
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       '0.60\ % \ w and 0.6\ % \ f scans'
_diffrn_radiation_collimation    '0.5 mm double- pinhole'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1581
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48520
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        30.949
_diffrn_reflns_theta_max         30.949
_diffrn_reflns_theta_min         2.043
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_exptl_absorpt_coefficient_mu    5.965
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             17880
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6132
_refine_ls_number_restraints     574
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1300
_refine_ls_R_factor_gt           0.0825
_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^)+(0.1269P)^2^+1351.4927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2223
_refine_ls_wR_factor_ref         0.2612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3965
_reflns_number_total             6132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10866_si_002.cif
_cod_data_source_block           MOP-2
_cod_original_cell_volume        73043(6)
_cod_original_formula_sum        'C450 H540 N45 O323.50 S12 V65 W15'
_cod_database_code               4133534
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Restrained distances
 O61-O44
 2.2 with sigma of 0.01
 O59_$1-O26_$1 = O59-O26
 2.2 with sigma of 0.01
 O68-O68_$1
 2.2 with sigma of 0.01
 O55-O24
 2.2 with sigma of 0.01
 O53-O53_$3
 2.2 with sigma of 0.01
 O36-O30
 2.2 with sigma of 0.01
 O70-O64
 2.2 with sigma of 0.01
 O32-O32_$2
 2.2 with sigma of 0.01
 O70_$2-O64_$2
 2.2 with sigma of 0.01
 O36_$2-O30_$2
 2.2 with sigma of 0.01
 O70-C4 = O64-C4
 1.25 with sigma of 0.01
 O24-C2 = O55-C2
 1.25 with sigma of 0.01
 O30-C8 = O36-C8
 1.25 with sigma of 0.01
 O26-C10 = O59-C10
 1.25 with sigma of 0.01
 C10-C36 = C8-C46
 1.45 with sigma of 0.01
 C36-O26
 2.38 with sigma of 0.01
 C36-O59
 2.38 with sigma of 0.01
 C46-O30
 2.38 with sigma of 0.01
 C46-O36
 2.38 with sigma of 0.01
 C8-C46
 1.45 with sigma of 0.01
 O30-C44
 2.8 with sigma of 0.01
 C48-O36
 2.8 with sigma of 0.01
 C34-O59
 2.8 with sigma of 0.01
 C38-O26
 2.8 with sigma of 0.01
 O72_$3-O40
 2.2 with sigma of 0.01
 O72_$3-C52_$3 = O40-C52_$3
 1.25 with sigma of 0.01
 C52_$3-C68 = C6-C58
 1.45 with sigma of 0.01
 O40-C70
 2.8 with sigma of 0.01
 O72_$3-C66
 2.8 with sigma of 0.01
 C56-O44
 2.8 with sigma of 0.01
 C60-O61
 2.8 with sigma of 0.01
 O61-C6 = O44-C6
 1.25 with sigma of 0.01
 C68-O72_$3
 2.38 with sigma of 0.01
 C68-O40
 2.38 with sigma of 0.01
 C58-O61
 2.38 with sigma of 0.01
 C58-O44
 2.38 with sigma of 0.01
 O68_$4-C73_$4 = O68_$5-C73_$4 = O68_$6-C73_$6 = O68_$2-C73_$6
 1.25 with sigma of 0.01
 C76-C74
 1.38 with sigma of 0.01
 C74-C73
 1.45 with sigma of 0.01
 O68_$1-C73 = O68-C73
 1.25 with sigma of 0.01
 C74-O68_$1
 2.38 with sigma of 0.01
 C74-O68
 2.38 with sigma of 0.01
 C76_$1-C76
 2.38 with sigma of 0.01
 C76_$1-C74 = C76-C74
 1.38 with sigma of 0.01
 C76_$1-O68
 2.8 with sigma of 0.01
 C76-O68_$1
 2.8 with sigma of 0.01
 O53_$3-C80
 1.25 with sigma of 0.01
 C80-O53
 1.25 with sigma of 0.01
 C82-O32
 1.25 with sigma of 0.01
 C82-C86
 1.45 with sigma of 0.01
 C89_$2-C86 = C89-C86
 1.38 with sigma of 0.01
 C86-O32
 2.38 with sigma of 0.01
 C89_$2-O32
 2.8 with sigma of 0.01
 C80-C84
 1.45 with sigma of 0.01
 C93-C84
 1.38 with sigma of 0.01
 C93-O53_$3
 2.8 with sigma of 0.01
 C12-C14 \\sim C14-C16 \\sim C16-C18 \\sim C18-C20 \\sim C12-C30 \\sim C20-C22
\\sim C22-C24 \\sim C24-C26
 \\sim C28-C30 \\sim C26-C28 \\sim C20-C30
 with sigma of 0.02
 C22-C26 \\sim C20-C24 \\sim C24-C28 \\sim C18-C22 \\sim C26-C30 \\sim C16-C20
\\sim C14-C18 \\sim C12-C28
 \\sim C12-C16 \\sim C14-C30
 with sigma of 0.04
 C12-C20 \\sim C18-C30 \\sim C22-C30 \\sim C20-C28
 with sigma of 0.04
 C32-C34 \\sim C34-C36 \\sim C36-C38 \\sim C38-C40 \\sim C32-C50 \\sim C40-C42
\\sim C42-C44 \\sim C44-C46
 \\sim C48-C50 \\sim C46-C48 \\sim C40-C50
 with sigma of 0.02
 C42-C46 \\sim C40-C44 \\sim C44-C48 \\sim C38-C42 \\sim C46-C50 \\sim C36-C40
\\sim C34-C38 \\sim C32-C48
 \\sim C32-C36 \\sim C34-C50
 with sigma of 0.04
 C32-C40 \\sim C38-C50 \\sim C42-C50 \\sim C40-C48
 with sigma of 0.04
 C54-C56 \\sim C56-C58 \\sim C58-C60 \\sim C60-C62 \\sim C54-C72 \\sim C62-C64
\\sim C64-C66 \\sim C66-C68
 \\sim C70-C72 \\sim C68-C70 \\sim C62-C72
 with sigma of 0.02
 C64-C68 \\sim C62-C66 \\sim C66-C70 \\sim C60-C64 \\sim C68-C72 \\sim C58-C62
\\sim C56-C60 \\sim C54-C70
 \\sim C54-C58 \\sim C56-C72
 with sigma of 0.04
 C54-C62 \\sim C60-C72 \\sim C64-C72 \\sim C62-C70
 with sigma of 0.04
2. Restrained planarity
 C12, C14, C16, C18, C20, C22, C24, C26, C28, C30
 with sigma of 0.1
 C32, C34, C36, C38, C40, C42, C44, C46, C48, C50
 with sigma of 0.1
 C54, C56, C58, C60, C62, C64, C66, C68, C70, C72
 with sigma of 0.1
 O32, O32_$2, O32_$1, O32_$6, C82, C82_$6
 with sigma of 0.1
 C76_$1, O68_$7, C76_$7, C78_$7, O68_$3, C73_$3, C74_$3, C76_$3, O68, C73, C74,
  C76, C78, O68_$1
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C12 \\sim C14 \\sim C16 \\sim C18 \\sim C20 \\sim C22 \\sim C24 \\sim C26 \\sim
C28 \\sim C30: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C32 \\sim C34 \\sim C36 \\sim C38 \\sim C40 \\sim C42 \\sim C44 \\sim C46 \\sim
C48 \\sim C50: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C54 \\sim C56 \\sim C58 \\sim C60 \\sim C62 \\sim C64 \\sim C66 \\sim C68 \\sim
C70 \\sim C72: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C2 \\sim C4 \\sim C6 \\sim C8 \\sim C10 \\sim C12 \\sim C14 \\sim C16 \\sim C18
\\sim C20 \\sim C22 \\sim C24 \\sim C26 \\sim C28 \\sim C30 \\sim C32 \\sim C34
\\sim C36 \\sim C38 \\sim C40 \\sim C42 \\sim C44 \\sim C46 \\sim C48 \\sim C50
\\sim C52 \\sim C54 \\sim C56 \\sim C58 \\sim C60 \\sim C62 \\sim C64 \\sim C66
\\sim C68 \\sim C70 \\sim C72 \\sim C73 \\sim C74 \\sim C76 \\sim C78 \\sim C80
\\sim C82 \\sim C84 \\sim C86 \\sim C87 \\sim C89 \\sim C91 \\sim C93 \\sim
C95: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03
4. Rigid body (RIGU) restrains
 C12, C14, C16, C18, C20, C22, C24, C26, C28, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C34, C36, C38, C40, C42, C44, C46, C48, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C54, C56, C58, C60, C62, C64, C66, C68, C70, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;