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_7123979
_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 O168 S4 V40 W4, 2(O4 S), 14(C2 H8 N)'
_chemical_formula_sum            'C156 H228 Cl4 N24 O176 S6 V40 W4'
_chemical_formula_weight         8362.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-31
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-31 deposited with the CCDC.    2019-08-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.267(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   41.892(5)
_cell_length_b                   21.947(2)
_cell_length_c                   46.700(5)
_cell_measurement_reflns_used    105495
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.953
_cell_volume                     41790(8)
_computing_cell_refinement       'APEX2(Bruker, 2005)'
_computing_data_collection       'APEX2(Bruker, 2005)'
_computing_data_reduction        'SAINT(Bruker, 2006)'
_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      296.02
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            105495
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.136
_diffrn_reflns_theta_max         25.136
_diffrn_reflns_theta_min         2.176
_exptl_absorpt_coefficient_mu    2.072
_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            green
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             16480
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.571
_refine_diff_density_min         -3.366
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1761
_refine_ls_number_reflns         36825
_refine_ls_number_restraints     1638
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+473.9878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1640
_refine_ls_wR_factor_ref         0.1853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26809
_reflns_number_total             36825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05984a2.cif
_cod_data_source_block           VMOP_28
_cod_original_cell_volume        41791(8)
_cod_database_code               7123979
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.682
_shelx_estimated_absorpt_t_min   0.636
_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,H) groups
2. Restrained distances
 N7-C68 = N7-C67 = N6-C66 = N6-C65
 1.5 with sigma of 0.02
3. Rigid bond restraints
 O75, O87
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 S2, S2, O76, O76
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S2, O80
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 W2, O76
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 V5, O80
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 W2, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 W2, O7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 V5, O1
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
4. Uiso/Uaniso restraints and constraints
S2 \\sim O76 \\sim O77 \\sim O80 \\sim O82 \\sim O86: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
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 O91: within 3.8A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C67 \\sim N7 \\sim C68: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C67 \\sim N7 \\sim C68 \\sim C66 \\sim N6 \\sim C65 \\sim C64 \\sim N5 \\sim
C63: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O75) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.1
Uanis(S1) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(S3) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.001
Uanis(O87) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C64) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq,
Uanis(N7) \\sim Ueq, Uanis(C68) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
5. Others
 Fixed Sof: S1(0.6) S3(0.4) O79(0.5) O81(0.5) O82(0.5) O85(0.5) O86(0.5)
 O87(0.5)
6.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B),
 N7(H7A,H7B)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C11(H11), C13(H13), C15(H15), C16(H16), C17(H17),
 C28(H28), C29(H29), C35(H35), C37(H37), C41(H41), C42(H42), C45(H45), C46(H46),
  C50(H50), C51(H51)
6.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              23707
_shelx_fab_checksum              50833
_olex2_submission_special_instructions 'No special instructions were received'