High-nuclear polyoxovanadates assembled from pentagonal building blocks
Zhang, Ting; Hou, Yuhan; Hou, Baoshan; Zhao, Liang; Wang, Xinlong; Qin, Chao; Su, Zhongmin; Chemical Communications  (2022) –; doi:10.1039/D2CC04436F

data_7130715
_publ_section_title
;
 High-nuclear polyoxovanadates assembled from pentagonal building blocks
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04436F
_journal_year                    2022
_chemical_formula_moiety
'C120 H96 Na10 O100 P20 S2 V20 W2, [+ solvents]'
_chemical_formula_sum            'C154 H204 N10 Na10 O110 P20 S2 V20 W2'
_chemical_formula_weight         6255.18
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-29
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
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2022-08-30 deposited with the CCDC.	2022-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.4190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.1926(13)
_cell_length_b                   19.4384(7)
_cell_length_c                   33.8946(18)
_cell_measurement_reflns_used    9818
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      57.000
_cell_measurement_theta_min      1.953
_cell_volume                     22727.5(17)
_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 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.02
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker D8 VENTURE'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '0.60\ % \ w and 0.6\ % \ f scans'
_diffrn_radiation_collimation    '0.5 mm double- pinhole'
_diffrn_radiation_detector       'Bruker D8 VENTURE'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            117735
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.583
_diffrn_reflns_theta_min         2.562
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.924
_exptl_absorpt_correction_T_max  0.138
_exptl_absorpt_correction_T_min  0.113
_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    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12512
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.669
_refine_diff_density_min         -1.998
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1180
_refine_ls_number_reflns         22368
_refine_ls_number_restraints     2652
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1052P)^2^+472.6447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1885
_refine_ls_wR_factor_ref         0.1948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19746
_reflns_number_total             22368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04436f2.cif
_cod_data_source_block           V20W2P20
_cod_original_cell_volume        22727.4(17)
_cod_database_code               7130715
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 S1-O5 \\sim S1-O23 \\sim S1-O6
 with sigma of 0.02
 S1-O5 \\sim S1-O23 \\sim S1-O49 \\sim S1-O6 \\sim S1-O50
 with sigma of 0.02
3. Rigid bond restraints
 P7, C43, P5, C49, P4, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
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 C1 \\sim C2 \\sim C3 \\sim C4
\\sim C5 \\sim C6 \\sim C7 \\sim C12 \\sim C11 \\sim C10 \\sim C9 \\sim C8
\\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 C36 \\sim C35 \\sim C34 \\sim C33 \\sim C32
\\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 S1 \\sim S2: within 3.8A with sigma of 0.01 and sigma for terminal atoms
of 0.03 within 3.8A
Uanis(S1) \\sim Ueq, Uanis(Na7) \\sim Ueq, Uanis(Na5) \\sim Ueq, Uanis(Na1)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C43) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.008 and
sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: S1(0.5) S2(0.5) Na2(0.5) Na3(0.6) Na5(0.4) Na6(0.5) O6(0.5)
 O13(0.5) O23(0.5) O26(0.5) O49(0.5) O50(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C12(H12), C11(H11), C10(H10), C9(H9),
 C8(H8), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C36(H36), C35(H35), C34(H34), C33(H33), C32(H32), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
  C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
6.b Fitted hexagon refined as free rotating group:
 C7(C12,C11,C10,C9,C8), C13(C14,C15,C16,C17,C18), C19(C20,C21,C22,C23,C24),
 C25(C26,C27,C28,C29,C30), C31(C36,C35,C34,C33,C32), C37(C38,C39,C40,C41,C42),
 C43(C44,C45,C46,C47,C48), C49(C50,C51,C52,C53,C54), C55(C56,C57,C58,C59,C60)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              70060
_shelx_hkl_checksum              74656
_shelx_fab_checksum              98624
_olex2_submission_special_instructions 'No special instructions were received'