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_4133533
_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         'C240 H120 O304.5 S12 V60 W12, O9 V5 W3'
_chemical_formula_sum            'C240 H120 O313.5 S12 V65 W15'
_chemical_formula_weight         14632.90
_space_group_crystal_system      tetragonal
_space_group_IT_number           136
_space_group_name_Hall           '-P 4n 2n'
_space_group_name_H-M_alt        'P 42/m n m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-01-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   55.536(9)
_cell_length_b                   55.536(9)
_cell_length_c                   35.633(6)
_cell_measurement_temperature    292(2)
_cell_volume                     109901(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      291.99
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1537
_diffrn_reflns_av_unetI/netI     0.1259
_diffrn_reflns_Laue_measured_fraction_full 0.947
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       58
_diffrn_reflns_limit_k_min       -58
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            267220
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        22.000
_diffrn_reflns_theta_max         22.000
_diffrn_reflns_theta_min         2.152
_exptl_absorpt_coefficient_mu    2.152
_exptl_crystal_density_diffrn    0.867
_exptl_crystal_F_000             26981
_refine_diff_density_max         4.161
_refine_diff_density_min         -4.227
_refine_diff_density_rms         0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         33152
_refine_ls_number_restraints     947
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.2339
_refine_ls_R_factor_gt           0.1694
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.3000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4577
_refine_ls_wR_factor_ref         0.5044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15761
_reflns_number_total             33152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10866_si_002.cif
_cod_data_source_block           GMOP-1
_cod_original_cell_volume        109902(42)
_cod_original_formula_sum        'C240 H120 O313.50 S12 V65 W15'
_cod_database_code               4133533
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C53-O82
 1.25 with sigma of 0.02
 C53-O83
 1.25 with sigma of 0.02
 C53-C50
 1.5 with sigma of 0.02
 C50-C49
 1.38 with sigma of 0.02
 C49-C48
 1.38 with sigma of 0.02
 C48-C47
 1.38 with sigma of 0.02
 C47-C52
 1.38 with sigma of 0.02
 C52-C51
 1.38 with sigma of 0.02
 C51-C50
 1.38 with sigma of 0.02
 C47-C46
 1.5 with sigma of 0.02
 C46-O44
 1.25 with sigma of 0.02
 C46-O43
 1.25 with sigma of 0.02
 C61-O74
 1.25 with sigma of 0.02
 C61-C58
 1.5 with sigma of 0.02
 C57-C56
 1.38 with sigma of 0.02
 C58-C57
 1.38 with sigma of 0.02
 C56-C55
 1.38 with sigma of 0.02
 C55-C60
 1.38 with sigma of 0.02
 C60-C59
 1.38 with sigma of 0.02
 C59-C58
 1.38 with sigma of 0.02
 C55-C54
 1.5 with sigma of 0.02
 C54-O73
 1.25 with sigma of 0.02
 C57-C59
 2.39 with sigma of 0.02
 C60-C56
 2.39 with sigma of 0.02
 C58-C56
 2.39 with sigma of 0.02
 C58-C60
 2.39 with sigma of 0.02
 C55-C57
 2.39 with sigma of 0.02
 C55-C59
 2.39 with sigma of 0.02
 C42-O59
 1.25 with sigma of 0.02
 C42-O58
 1.25 with sigma of 0.02
 C42-C39
 1.5 with sigma of 0.02
 C39-C38
 1.38 with sigma of 0.02
 C38-C37
 1.38 with sigma of 0.02
 C37-C36
 1.38 with sigma of 0.02
 C36-C41
 1.38 with sigma of 0.02
 C41-C40
 1.38 with sigma of 0.02
 C40-C39
 1.38 with sigma of 0.02
 C36-C35
 1.5 with sigma of 0.02
 C35-O38
 1.25 with sigma of 0.02
 C35-O37
 1.25 with sigma of 0.02
 C30-O34
 1.25 with sigma of 0.02
 C30-O35
 1.25 with sigma of 0.02
 C30-C27
 1.5 with sigma of 0.02
 C27-C26
 1.38 with sigma of 0.02
 C26-C25
 1.38 with sigma of 0.02
 C25-C24
 1.38 with sigma of 0.02
 C24-C29
 1.38 with sigma of 0.02
 C29-C28
 1.38 with sigma of 0.02
 C28-C27
 1.38 with sigma of 0.02
 C24-C23
 1.5 with sigma of 0.02
 C23-O90
 1.25 with sigma of 0.02
 C23-O89
 1.25 with sigma of 0.02
 O32-C22
 1.25 with sigma of 0.02
 C22-O31
 1.25 with sigma of 0.02
 C22-C19
 1.5 with sigma of 0.02
 C19-C18
 1.38 with sigma of 0.02
 C18-C17
 1.38 with sigma of 0.02
 C17-C16
 1.38 with sigma of 0.02
 C16-C21
 1.38 with sigma of 0.02
 C21-C20
 1.38 with sigma of 0.02
 C20-C19
 1.38 with sigma of 0.02
 C16-C15
 1.5 with sigma of 0.02
 C15-O26
 1.25 with sigma of 0.02
 C15-O25
 1.25 with sigma of 0.02
 C11-O16
 1.25 with sigma of 0.02
 C11-O15
 1.25 with sigma of 0.02
 C11-C8
 1.5 with sigma of 0.02
 C8-C7
 1.38 with sigma of 0.02
 C7-C6
 1.38 with sigma of 0.02
 C6-C5
 1.38 with sigma of 0.02
 C5-C10
 1.38 with sigma of 0.02
 C10-C9
 1.38 with sigma of 0.02
 C9-C8
 1.38 with sigma of 0.02
 C5-C4
 1.5 with sigma of 0.02
 C4-O14
 1.25 with sigma of 0.02
 C4-O9
 1.25 with sigma of 0.02
 O47-C34
 1.25 with sigma of 0.02
 C34-O46
 1.25 with sigma of 0.02
 C34-C32
 1.5 with sigma of 0.02
 C31-C32
 1.38 with sigma of 0.02
 C32-C33
 1.38 with sigma of 0.02
 C33-C31
 2.39 with sigma of 0.02
 O76-C64
 1.25 with sigma of 0.02
 C64-C63
 1.5 with sigma of 0.02
 C63-C62
 1.38 with sigma of 0.02
 C45-O61
 1.25 with sigma of 0.02
 C45-C44
 1.5 with sigma of 0.02
 C44-C43
 1.38 with sigma of 0.02
 C12-O17
 1.25 with sigma of 0.02
 C12-C13
 1.5 with sigma of 0.02
 C13-C14
 1.38 with sigma of 0.02
 O1-C3
 1.25 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.02
 C2-C1
 1.38 with sigma of 0.02
 S3-O49
 1.47 with sigma of 0.02
 V8-O45
 2.25 with sigma of 0.02
 V7-O49
 2.25 with sigma of 0.02
 C50-C51 = C52-C51 = C52-C47 = C48-C47 = C49-C48 = C50-C49
 1.38 with sigma of 0.02
 C49-C51
 2.39 with sigma of 0.02
 C48-C52
 2.39 with sigma of 0.02
 C50-C52
 2.39 with sigma of 0.02
 C50-C48
 2.39 with sigma of 0.02
 C47-C51
 2.39 with sigma of 0.02
 C47-C49
 2.39 with sigma of 0.02
 S3-O55
 1.46 with sigma of 0.02
 S3-O56
 1.46 with sigma of 0.02
 S3-O49 = S3-O55 = S3-O56 = S3-O57
 1.46 with sigma of 0.02
 C16-C17 = C18-C17 = C19-C18 = C19-C20 = C20-C21 = C16-C21
 1.38 with sigma of 0.02
 C16-C15 = C19-C22
 1.5 with sigma of 0.02
 C21-C17
 2.39 with sigma of 0.02
 C20-C18
 2.39 with sigma of 0.02
 C16-C20
 2.39 with sigma of 0.02
 C16-C18
 2.39 with sigma of 0.02
 C19-C21
 2.39 with sigma of 0.02
 C17-C19
 2.39 with sigma of 0.02
 O56-O57
 2.4 with sigma of 0.02
 O56-O55
 2.4 with sigma of 0.02
 O56-O49
 2.4 with sigma of 0.02
 O55-O57
 2.4 with sigma of 0.02
 O55-O49
 2.4 with sigma of 0.02
 O49-O57
 2.4 with sigma of 0.02
 O57-V11
 2.3 with sigma of 0.02
 V14-O70
 2.3 with sigma of 0.02
 V13_$3-O72_$3
 2.3 with sigma of 0.02
 V13-O72
 2.3 with sigma of 0.02
 V2-O13
 2.3 with sigma of 0.02
 W4-O69
 2.3 with sigma of 0.02
 W1-O29
 2.3 with sigma of 0.02
 S4-O69 = S4-O72_$3 = S4-O72 = S4-O70
 1.4 with sigma of 0.02
 S4-O70 = S4-O72_$3 = S4-O69 = S4-O72
 1.4 with sigma of 0.02
 S4-O71
 1.4 with sigma of 0.02
 O71-O69
 2.4 with sigma of 0.02
 O71-O72_$3
 2.4 with sigma of 0.02
 O71-O70
 2.4 with sigma of 0.02
 O72-O71
 2.4 with sigma of 0.02
 S4-O72 = S4-O70 = S4-O72_$3 = S4-O69 = S4-O71
 1.46 with sigma of 0.02
 V15_$1-O88
 2.3 with sigma of 0.02
 O88-V15_$1
 2.3 with sigma of 0.02
 W5-O86
 2.3 with sigma of 0.02
 S5-O88 = S5-O86 = S5-O88_$1 = S5-O87 = S5-O87
 1.46 with sigma of 0.02
 S2-O29 = S2-O28 = S2-O27 = S2-O30
 1.46 with sigma of 0.02
 S1-O6
 1.46 with sigma of 0.02
 S1-O11
 1.46 with sigma of 0.02
 S1-O13
 1.46 with sigma of 0.02
 S1-O12
 1.46 with sigma of 0.02
 O6-V3
 3.3 with sigma of 0.02
 V19_$4-O97_$4
 1.72 with sigma of 0.02
 V20_$4-O97_$4
 1.72 with sigma of 0.02
 C43-C43_$3
 2.38 with sigma of 0.02
 C1_$1-C1_$2
 2.38 with sigma of 0.02
 C43-C2_$2
 2.38 with sigma of 0.02
 C43-C1_$2
 2.8 with sigma of 0.02
 C44-C2_$2
 2.8 with sigma of 0.02
 O29-V4
 3.4 with sigma of 0.02
 O29-V6
 3.4 with sigma of 0.02
 O29-V5
 3.4 with sigma of 0.02
 O55-V9
 3.4 with sigma of 0.02
 O55-V10
 3.4 with sigma of 0.02
 O55-V11
 3.4 with sigma of 0.02
 O55-V7
 3.4 with sigma of 0.02
 O55-V8
 3.4 with sigma of 0.02
 O69-V14
 3.4 with sigma of 0.02
 O69-V13
 3.4 with sigma of 0.02
 O69-V12
 3.4 with sigma of 0.02
 V16-O86
 3.4 with sigma of 0.02
 O86-V15
 3.4 with sigma of 0.02
 O86-V17
 3.4 with sigma of 0.02
 O6-V1
 3.4 with sigma of 0.02
 O6-V2
 3.4 with sigma of 0.02
 W3-O6
 2.3 with sigma of 0.02
 O28-V6
 2.3 with sigma of 0.02
3. Restrained planarity
 C57, O74, O73, C55, C56, C54, C61, C58, C59, C60
 with sigma of 0.1
 O58, O37, O38, C36, C37, C38, C39, C40, C41, O59, C42, C35
 with sigma of 0.1
 O35, O34, C27, C28, C30, C29, C25, C24, C26, O89, C23, O90
 with sigma of 0.1
 O26, O31, O25, O32, C20, C16, C19, C15, C18, C21, C22, C17
 with sigma of 0.1
 O16, O9, C5, C9, C6, C8, C11, C10, C4, C7, O14, O15
 with sigma of 0.1
 O1_$2, O1_$1, O61_$3, O61, C44, C2_$2, C3_$2, C1_$1, C1_$2, C45, C43, C43_$3
 with sigma of 0.1
 O1, O1_$3, O61_$1, O61_$2, C44_$2, C2, C3, C1, C1_$3, C45_$2, C43_$1, C43_$2
 with sigma of 0.1
 O1_$3, O1, O61_$2, O61_$1, C44_$2, C2, C3, C1_$3, C1, C45_$2, C43_$2, C43_$1
 with sigma of 0.1
 C63_$2, C63, O76_$1, O76, O76_$3, O76_$2, C64, C64_$2, C62, C62_$1, C62_$3,
 C62_$2
 with sigma of 0.1
 O17_$3, O17_$1, O17_$2, O17, C12_$2, C12, C13_$2, C13, C14_$2, C14_$3, C14,
 C14_$1
 with sigma of 0.1
 O1, O1_$3, O61_$2, O61_$1, C44_$2, C2, C3, C1_$3, C1, C45_$2, C43_$1, C43_$2
 with sigma of 0.1
 O43, O44, C52, C47, C48, C46, C51, C50, C49, O82, O83, C53
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
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 O34 \\sim O35 \\sim O36 \\sim O37 \\sim O38 \\sim O39 \\sim O40 \\sim O41
\\sim O42 \\sim O43 \\sim O44 \\sim O45 \\sim O46 \\sim O47 \\sim O48 \\sim O49
\\sim O50 \\sim O51 \\sim O52 \\sim O53 \\sim O54 \\sim O55 \\sim O56 \\sim O57
\\sim O58 \\sim O59 \\sim O60 \\sim O61 \\sim O62 \\sim O63 \\sim O64 \\sim O65
\\sim O66 \\sim O67 \\sim O68 \\sim O69 \\sim O70 \\sim O71 \\sim O72 \\sim O73
\\sim O74 \\sim O75 \\sim O76 \\sim O77 \\sim O78 \\sim O79 \\sim O80 \\sim O81
\\sim O82 \\sim O83 \\sim O84 \\sim O85 \\sim O86 \\sim O87 \\sim O88 \\sim O89
\\sim O90 \\sim O101 \\sim O102 \\sim O91 \\sim O92 \\sim O93 \\sim O94 \\sim
O95 \\sim O96 \\sim O97 \\sim O98 \\sim O99 \\sim O100 \\sim 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 C16 \\sim C17 \\sim C18 \\sim C19
\\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27
\\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35
\\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43
\\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51
\\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59
\\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim S1 \\sim S2 \\sim S4
\\sim S3 \\sim S5: within 3.8A with sigma of 0.01 and sigma for terminal atoms
of 0.03
Uanis(V15) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.014
Uanis(W5) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: O6(0.125) O10(0.25) O28(0.5) O29(0.25) O41(0.5) O57(0.5) O72(0.25)
 O88(0.25) W6(0.125) W7(0.125) W8(0.25) W9(0.125) W10(0.125) V18(0.125)
 V19(0.25) V20(0.25) V21(0.125) V22(0.25) V23(0.125) V24(0.125) O91(0.25)
 O92(0.25) O93(0.0625) O94(0.25) O95(0.125) O97(0.25) O98(0.25) O99(0.0625)
 O100(0.25)
6.a :
 C36(C37,C38,C39,C40,C41)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C7(H7), C9(H9), C10(H10), C14(H14), C17(H17), C18(H18),
 C20(H20), C21(H21), C25(H25), C26(H26), C28(H28), C29(H29), C31(H31), C33(H33),
  C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C48(H48), C49(H49),
 C51(H51), C52(H52), C56(H56), C57(H57), C59(H59), C60(H60), C62(H62)
;