Self-assembly of a unique triangle-like tungstovanadate containing pentagonal {(WO<sub>7</sub>)W<sub>3</sub>(SnR)<sub>2</sub>} cluster.
Zhu, Hao-Tian; Sun, Yang; Su, Fang; Zhang, Ya-Jun; Sang, Xiao-Jing; Ren, Jing; Zhang, Lan-Cui; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10226–10234; doi:10.1039/d4dt01281j

data_7716131
_publ_section_title
;
 Self-assembly of a unique triangle-like tungstovanadate containing
 pentagonal {(WO<sub>7</sub>)W<sub>3</sub>(SnR)<sub>2</sub>} cluster.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10226
_journal_page_last               10234
_journal_paper_doi               10.1039/d4dt01281j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C24 H46.5 K10 O148 Sn8 V3 W34.75,33H2O'
_chemical_formula_sum            'C24 H112.5 K10 O181 Sn8 V3 W34.75'
_chemical_formula_weight         11179.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-04-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-30 deposited with the CCDC.	2024-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.4530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.6015(6)
_cell_length_b                   40.4127(17)
_cell_length_c                   19.2506(8)
_cell_measurement_reflns_used    6683
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.159
_cell_measurement_theta_min      2.183
_cell_volume                     11217.4(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SMART (Bruker, 2005)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-alpha (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.1085
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20040
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.735
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    19.007
_exptl_absorpt_correction_T_max  0.438
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.310
_exptl_crystal_description       block
_exptl_crystal_F_000             9870
_exptl_crystal_size_max          0.089
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.052
_platon_squeeze_details
;
;
_refine_diff_density_max         2.590
_refine_diff_density_min         -2.325
_refine_diff_density_rms         0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1128
_refine_ls_number_reflns         20040
_refine_ls_number_restraints     340
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11978
_reflns_number_total             20040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01281j2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7716131.cif.
;
_cod_original_formula_sum        'C24 H112.50 K10 O181 Sn8 V3 W34.75'
_cod_database_code               7716131
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.438
_shelx_estimated_absorpt_t_min   0.283
_olex2_refinement_description
;
1. Shared sites
{W17, V17}
2. Restrained distances
 C1-C2 = C2-C3
 1.52 with sigma of 0.01
 C10-C11 = C11-C12
 1.52 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Sn1 \\sim C1 \\sim C2 \\sim C3 \\sim O73 \\sim O74: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 3.8A
Sn2 \\sim C4 \\sim C5 \\sim C6 \\sim O75 \\sim O76: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 3.8A
Sn4 \\sim C10 \\sim C11 \\sim C12 \\sim O79 \\sim O80: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
K3 \\sim K3A: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
Uanis(K3) \\sim Ueq, Uanis(K5) \\sim Ueq, Uanis(K6) \\sim Ueq, Uanis(K7) \\sim
Ueq, Uanis(K8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O8) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O43)
\\sim Ueq, Uanis(O63) \\sim Ueq, Uanis(O64) \\sim Ueq, Uanis(O3W) \\sim Ueq,
Uanis(O4W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(W17) = Uanis(V17)
4. Others
 Fixed Sof: W17(0.875) V17(0.125) W19(0.375) W19A(0.125) V2(0.375) K3(0.375)
 K3A(0.125) K4(0.5) K5(0.5) K6(0.5) K7(0.25) K8(0.5) K9(0.25) K9A(0.25)
 K10(0.25) O3W(0.5) O4W(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B),
 C10(H10A,H10B), C11(H11A,H11B)
;
_shelx_res_checksum              5694
_olex2_submission_special_instructions 'No special instructions were received'