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_4133532
_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         'O35 S6 V5 W, O4 S, 6(C2 H8 N), C2 H6.5 N'
_chemical_formula_sum            'C18 H66.5 N8 O35 S6 V5 W'
_chemical_formula_weight         1586.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-11-24
_audit_creation_method
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.490(5)
_cell_length_b                   16.481(5)
_cell_length_c                   21.309(5)
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    296
_cell_measurement_theta_max      28.224
_cell_measurement_theta_min      2.276
_cell_volume                     5440(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31003
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.562
_exptl_absorpt_coefficient_mu    3.260
_exptl_absorpt_correction_T_max  0.521
_exptl_absorpt_correction_T_min  0.447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4 Bruker AXS Madison WI USA'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_description       block
_exptl_crystal_F_000             3182
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.040
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Flack x determined using 3821 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.009(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         9573
_refine_ls_number_restraints     1249
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+5.2723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.809
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                9079
_reflns_number_total             9573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10866_si_002.cif
_cod_data_source_block           WV5
_cod_original_formula_sum        'C18 H66.50 N8 O35 S6 V5 W'
_cod_database_code               4133532
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C1-N1
 1.47 with sigma of 0.02
 N2-C3
 1.47 with sigma of 0.02
 S10-O16
 1.47 with sigma of 0.02
 N4-C8
 1.47 with sigma of 0.02
 N4-C7
 1.47 with sigma of 0.02
 C7-C8
 2.47 with sigma of 0.02
 C5-N3
 1.47 with sigma of 0.02
 C6-N3
 1.47 with sigma of 0.02
 C6-C5
 2.47 with sigma of 0.02
 N2-C4
 1.47 with sigma of 0.02
 N2-C3
 1.47 with sigma of 0.02
 C3-C4
 2.47 with sigma of 0.02
 N1-C2
 1.47 with sigma of 0.02
 N1-C1
 1.47 with sigma of 0.02
 C1-C2
 2.47 with sigma of 0.02
 N8-C11
 1.47 with sigma of 0.02
 N7-C11
 1.47 with sigma of 0.02
 N8-C12
 1.47 with sigma of 0.02
 N7-C12
 1.47 with sigma of 0.02
 C12-C11
 2.47 with sigma of 0.02
 N9-C13
 1.47 with sigma of 0.02
 N9-C14
 1.47 with sigma of 0.02
 C14-C13
 2.47 with sigma of 0.02
 N5-C9
 1.47 with sigma of 0.02
 N5-C10
 1.47 with sigma of 0.02
 N6-C10
 1.47 with sigma of 0.02
 N6-C9
 1.47 with sigma of 0.02
 C9-C10
 2.47 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O6 \\sim O33 \\sim O35 \\sim O12 \\sim O22 \\sim O21 \\sim O26 \\sim O11 \\sim
O34 \\sim O3AA \\sim O7 \\sim O2AA \\sim O3 \\sim O28 \\sim O23 \\sim O5 \\sim
O1 \\sim O30 \\sim O13 \\sim O8 \\sim O1AA \\sim O31 \\sim O4 \\sim O27 \\sim
O29 \\sim O2 \\sim O32 \\sim O0AA \\sim O10 \\sim O20 \\sim O9 \\sim O19 \\sim
O14 \\sim O16 \\sim O18 \\sim O17 \\sim O15 \\sim O24 \\sim O25 \\sim O25A
\\sim O24A \\sim C3 \\sim C1 \\sim C7 \\sim C8 \\sim C6 \\sim C5 \\sim C11
\\sim C12 \\sim C4 \\sim C2 \\sim C14 \\sim C13 \\sim C9 \\sim C10 \\sim N4
\\sim N1 \\sim N2 \\sim N3 \\sim N9 \\sim N5 \\sim N7 \\sim N6 \\sim N8: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03
4. Others
 Fixed Sof: H11A(0.5) H11B(0.5) H11C(0.5) H11D(0.5) H11E(0.5) H11F(0.5)
 H12A(0.5) H12B(0.5) H12C(0.5) H12D(0.5) H12E(0.5) H12F(0.5) H9AA(0.5)
 H9AB(0.5) H9AC(0.5) H9BD(0.5) H9BE(0.5) H9BF(0.5) H10A(0.5) H10B(0.5)
 H10C(0.5) O24(0.5) O25(0.5) N5(0.5) H5A(0.5) H5B(0.5) N7(0.5) H7A(0.5)
 H7B(0.5) O25A(0.5) O24A(0.5) N6(0.5) H6A(0.5) H6B(0.5) N8(0.5) H8A(0.5)
 H8B(0.5)
5.a Riding coordinates:
 C11(H11A,H11B,H11C,H11D,H11E,H11F), C12(H12A,H12B,H12C,H12D,H12E,H12F),
 C9(H9AA,H9AB,H9AC,H9BD,H9BE,H9BF)
5.b Secondary CH2 refined with riding coordinates:
 N4(H4A,H4B), N1(H1A,H1B), N2(H2D,H2E), N3(H3D,H3E), N9(H9A,H9B), N5(H5A,H5B),
 N7(H7A,H7B), N6(H6A,H6B), N8(H8A,H8B)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C1(H1C,H1D,H1E), C7(H7C,H7D,H7E), C8(H8C,H8D,H8E), C6(H6C,
 H6D,H6E), C5(H5C,H5D,H5E), C4(H4C,H4D,H4E), C2(H2A,H2B,H2C), C14(H14A,H14B,
 H14C), C13(H13A,H13B,H13C), C10(H10A,H10B,H10C)
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