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_7130716
_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
'C92 H70 Na7 O96 P14 V18 W4, 18[C2N1H8], 2[C3N1O1H10]'
_chemical_formula_sum            'C132 H206 N13 Na7 O110 P14 V18 W4'
_chemical_formula_weight         5981.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_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
;
2022-08-30 deposited with the CCDC.	2022-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   37.4678(17)
_cell_length_b                   28.5413(10)
_cell_length_c                   20.4155(8)
_cell_measurement_reflns_used    9591
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      57.000
_cell_measurement_theta_min      1.953
_cell_volume                     21831.9(15)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0964
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            100373
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        63.900
_diffrn_reflns_theta_max         63.900
_diffrn_reflns_theta_min         2.358
_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
_exptl_absorpt_coefficient_mu    11.876
_exptl_absorpt_correction_T_max  0.110
_exptl_absorpt_correction_T_min  0.093
_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    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11864
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.581
_refine_diff_density_min         -3.143
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         18209
_refine_ls_number_restraints     2508
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1405
_refine_ls_R_factor_gt           0.0988
_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^)+(0.1315P)^2^+378.1234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2526
_refine_ls_wR_factor_ref         0.2844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11717
_reflns_number_total             18209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04436f2.cif
_cod_data_source_block           V18W4P14
_cod_database_code               7130716
_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
 V1-O15 \\sim V9-O14 \\sim V9-O42 \\sim V9-O25 \\sim V9-O39 \\sim V7-O43 \\sim
V2-O47 \\sim V3-O23 \\sim V10-O37
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C36 \\sim C37 \\sim
C38 \\sim C39 \\sim C40 \\sim C41 \\sim C51 \\sim C1 \\sim C6 \\sim C5 \\sim C4
\\sim C3 \\sim C2 \\sim C48 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34
\\sim C35 \\sim C10 \\sim C9 \\sim C8 \\sim C7 \\sim C12 \\sim C11 \\sim C42
\\sim C47 \\sim C46 \\sim C45 \\sim C44 \\sim C43 \\sim C19 \\sim C20 \\sim C21
\\sim C22 \\sim C23 \\sim C52 \\sim C50 \\sim C49 \\sim C13 \\sim C18 \\sim C17
\\sim C16 \\sim C15 \\sim C14 \\sim 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: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03 within 3.8A
4. Others
 Fixed Sof: C1(0.5) C6(0.5) H6(0.5) C5(0.5) H5(0.5) C4(0.5) H4(0.5) C3(0.5)
 H3(0.5) C2(0.5) H2(0.5) C13(0.5) C18(0.5) H18(0.5) C17(0.5) H17(0.5) C16(0.5)
 H16(0.5) C15(0.5) H15(0.5) C14(0.5) H14(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C37(H37), C38(H38),
 C39(H39), C6(H6), C5(H5), C4(H4), C3(H3), C2(H2), C31(H31), C32(H32), C33(H33),
  C34(H34), C35(H35), C10(H10), C9(H9), C8(H8), C12(H12), C11(H11), C47(H47),
 C46(H46), C45(H45), C44(H44), C43(H43), C20(H20), C21(H21), C22(H22), C23(H23),
  C52(H52), C18(H18), C17(H17), C16(H16), C15(H15), C14(H14)
5.b Fitted hexagon refined as free rotating group:
 C24(C25,C26,C27,C28,C29), C36(C37,C38,C39,C40,C41), C1(C6,C5,C4,C3,C2),
 C30(C31,C32,C33,C34,C35), C10(C9,C8,C7,C12,C11), C42(C47,C46,C45,C44,C43),
 C19(C20,C21,C22,C23,C52), C13(C18,C17,C16,C15,C14)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              15544
_shelx_hkl_checksum              39793
_shelx_fab_checksum              17533
_olex2_submission_special_instructions 'No special instructions were received'