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_4133535
_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
'C180 H60 O300 S12 V60 W12, 14(C2 H8 N), 3(C4 H12 N2), 4(O4 S)'
_chemical_formula_sum            'C268 H412 N44 O316 S16 V60 W12'
_chemical_formula_weight         15081.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.903(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   51.595(5)
_cell_length_b                   29.778(5)
_cell_length_c                   29.872(5)
_cell_measurement_reflns_used    8016
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.938
_cell_measurement_theta_min      2.168
_cell_volume                     42875(11)
_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      293
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1375
_diffrn_reflns_av_unetI/netI     0.1541
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            123939
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.550
_exptl_absorpt_coefficient_mu    2.324
_exptl_absorpt_correction_T_max  0.498
_exptl_absorpt_correction_T_min  0.430
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             14760
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.480
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1505
_refine_ls_number_reflns         38382
_refine_ls_number_restraints     692
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1675
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1252P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.2440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19246
_reflns_number_total             38382
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b10866_si_002.cif
_cod_data_source_block           GMOP-3
_cod_database_code               4133535
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.722
_shelx_estimated_absorpt_t_min   0.667
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2. Restrained distances
 V1-O75 = V2-O71 = V3-O89 = V4-O69 = V5-O82 = V6-O70 = V7-O90 = V8-O84
 2.33 with sigma of 0.03
 V9-O88 = V10-O72 = V11-O76 = V12-O83 = V13-O85 = V14-O77 = V15-O73 = V16-O81
 2.33 with sigma of 0.03
 W4-O79 = W3-O78 = W2-O67 = W1-O87
 2.4 with sigma of 0.02
 N1-C49 = N1-C50
 1.4 with sigma of 0.02
 N2-C51 = N2-C52
 1.4 with sigma of 0.02
 C49-C50 = C51-C52 = C53_$1-C54_$1 = C68-C69 = C57_$1-C58_$1 = C67_$1-C66_$1 =
 C55_$1-C56_$1 = C59_$1-C60_$1 = C61_$2-C62_$2 = C63_$1-C64_$1
 2.6 with sigma of 0.02
 N3-C68 = N3-C69
 1.4 with sigma of 0.02
 N4-C53 = N4-C54
 1.4 with sigma of 0.02
 N5-C57 = N5-C58
 1.4 with sigma of 0.02
 N6-C66 = N6-C67
 1.4 with sigma of 0.02
 N7-C55 = N7-C56
 1.4 with sigma of 0.02
 N8-C59 = N8-C60
 1.4 with sigma of 0.02
 N9-C61 = N9-C62
 1.4 with sigma of 0.02
 N10-C63 = N10-C64
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S4A \\sim S4B \\sim S4C \\sim S4D \\sim S4E \\sim S5A \\sim S5B \\sim S5C \\sim
S6A \\sim S6B \\sim S6C \\sim S6D \\sim S7A \\sim S7B \\sim S7C \\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 S3 \\sim
O3SA \\sim O3SB \\sim O3SC \\sim O3SD \\sim S2 \\sim O2SA \\sim O2SB \\sim O2SC
\\sim O2SD \\sim S1 \\sim O1SA \\sim O1SB \\sim O1SC: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.03
N2 \\sim C51 \\sim C52 \\sim N8 \\sim C59 \\sim C60 \\sim N6 \\sim C66 \\sim
C67 \\sim N9 \\sim C61 \\sim C62 \\sim N1 \\sim C49 \\sim C50 \\sim N10 \\sim
C63 \\sim C64 \\sim N5 \\sim C57 \\sim C58 \\sim N7 \\sim C55 \\sim C56 \\sim
N3 \\sim C68 \\sim C69 \\sim N4 \\sim C53 \\sim C54: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.03
S5A \\sim S5B \\sim S5C \\sim O2 \\sim O5 \\sim O18 \\sim O19 \\sim O21 \\sim
O35 \\sim O36 \\sim O43 \\sim O74 \\sim O75 \\sim O76 \\sim O77: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.03
S7A \\sim S7B \\sim O8 \\sim O10 \\sim O13 \\sim O50 \\sim O51 \\sim O63 \\sim
O64 \\sim O65 \\sim O86 \\sim O87 \\sim O88 \\sim O89 \\sim O90: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.03
Uiso(N1) = Uiso(C49) = Uiso(C50) = Uiso(N2) = Uiso(C51) = Uiso(C52) = Uiso(N3)
= Uiso(C68) = Uiso(C69) = Uiso(N4) = Uiso(C53) = Uiso(C54) = Uiso(N5) =
Uiso(C57) = Uiso(C58) = Uiso(N6) = Uiso(C67) = Uiso(C66) = Uiso(N7) = Uiso(C55)
= Uiso(C56) = Uiso(N8) = Uiso(C59) = Uiso(C60) = Uiso(N9) = Uiso(C61) =
Uiso(C62) = Uiso(N10) = Uiso(C63) = Uiso(C64)
4. Others
 Fixed Sof: S4A(0.2) S4B(0.2) S4C(0.2) S4D(0.2) S4E(0.2) S5A(0.125) S5B(0.125)
 S5C(0.25) S6A(0.25) S6B(0.25) S6C(0.25) S6D(0.25) S7A(0.16667) S7B(0.16667)
 S7C(0.16667) O69(0.4) O70(0.4) O71(0.4) O72(0.4) O73(0.4) O75(0.2) O76(0.4)
 O77(0.4) O81(0.4) O82(0.4) O83(0.4) O84(0.4) O85(0.4) O88(0.2) O89(0.4)
 O90(0.4) N2(0.5) H2A(0.5) H2B(0.5) C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5)
 C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) N8(0.5) H8A(0.5) H8B(0.5) C59(0.5)
 H59A(0.5) H59B(0.5) H59C(0.5) C60(0.5) H60A(0.5) H60B(0.5) H60C(0.5) N6(0.5)
 H6A(0.5) H6B(0.5) C66(0.5) H66A(0.5) H66B(0.5) H66C(0.5) C67(0.5) H67A(0.5)
 H67B(0.5) H67C(0.5) N9(0.5) H9A(0.5) H9B(0.5) C61(0.5) H61A(0.5) H61B(0.5)
 H61C(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5) N1(0.5) H1A(0.5) H1B(0.5)
 C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5)
 N10(0.5) H10A(0.5) H10B(0.5) C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5) C64(0.5)
 H64A(0.5) H64B(0.5) H64C(0.5) N5(0.5) H5A(0.5) H5B(0.5) C57(0.5) H57A(0.5)
 H57B(0.5) H57C(0.5) C58(0.5) H58A(0.5) H5C(0.5) H58B(0.5) H7A(0.5) H7B(0.5)
 H55B(0.5) H56B(0.5) H3A(0.5) H3B(0.5) H68B(0.5) H69B(0.5) H4A(0.5) H4B(0.5)
 H53B(0.5) H54B(0.5) S3(0.25) O3SA(0.25) O3SB(0.25) O3SC(0.25) O3SD(0.25)
 S2(0.25) O2SA(0.25) O2SB(0.25) O2SC(0.25) O2SD(0.25)
5.a Riding coordinates:
 N2(H2A,H2B), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C59(H59A,H59B,H59C),
 N6(H6A,H6B), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), N9(H9A,H9B), C61(H61A,
 H61B,H61C), C62(H62A,H62B,H62C), N1(H1A,H1B), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), N10(H10A,H10B), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C58(H58A,
 H5C,H58B), N7(H7A,H7B), C55(H55A,H55B), C56(H56A,H56B), N3(H3A,H3B), C68(H68A,
 H68B), C69(H69A,H69B), N4(H4A,H4B), C53(H53A,H53B), C54(H54A,H54B)
5.b Secondary CH2 refined with riding coordinates:
 N8(H8A,H8B), N5(H5A,H5B)
5.c Me refined with riding coordinates:
 C60(H60A,H60B,H60C), C57(H57A,H57B,H57C)
5.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C12(H12), C15(H15), C18(H18), C21(H21),
 C24(H24), C25(H25), C32(H32), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45)
;