Dy/Ho-encapsulated tartaric acid-functionalized tungstoantimonates: heterogeneous catalysts for isoindolinone synthesis.
Yang, Guoping; Liu, Haoqi; Chen, Jincao; Lin, Xiaoling; Tan, Kexin; Dong, Yayu; Liu, Yufeng; Wei, Yongge; Chemical communications (Cambridge, England) 60 (2024) 10934–10937; doi:10.1039/d4cc03675a

data_7133676
_publ_section_title
;
 Dy/Ho-encapsulated tartaric acid-functionalized tungstoantimonates:
 heterogeneous catalysts for isoindolinone synthesis.
;
_journal_issue                   78
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10934
_journal_page_last               10937
_journal_paper_doi               10.1039/d4cc03675a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C8 H4 Dy4 Na10 O174.5 Sb4 W42'
_chemical_formula_sum            'C8 H4 Dy4 Na10 O174.5 Sb4 W42'
_chemical_formula_weight         11980.71
_chemical_name_systematic        Dy4tar2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-14 deposited with the CCDC.	2024-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                98.669(2)
_cell_angle_beta                 110.256(2)
_cell_angle_gamma                111.317(2)
_cell_formula_units_Z            2
_cell_length_a                   24.7234(11)
_cell_length_b                   25.8468(11)
_cell_length_c                   26.5303(11)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.621
_cell_measurement_theta_min      2.360
_cell_volume                     14055.2(11)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            171482
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.268
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    18.615
_exptl_absorpt_correction_T_max  0.0825
_exptl_absorpt_correction_T_min  0.0250
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1450 before and 0.0906 after correction.
The Ratio of minimum to maximum transmission is 0.3030.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.831
_exptl_crystal_description       block
_exptl_crystal_F_000             10268
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.586
_refine_diff_density_min         -2.984
_refine_diff_density_rms         0.387
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2305
_refine_ls_number_reflns         49332
_refine_ls_number_restraints     4116
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0636P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.000
_reflns_number_gt                40106
_reflns_number_total             49332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03675a2.cif
_cod_data_source_block           DySbW_sq
_cod_depositor_comments
'Adding full bibliography for 7133676--7133677.cif.'
_cod_original_formula_sum        'C8 H4 Dy4 Na10 O174.50 Sb4 W42'
_cod_database_code               7133676
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.196
_shelx_estimated_absorpt_t_min   0.047
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
O1 \\sim O1L \\sim O1W \\sim O2 \\sim O2L \\sim O2W \\sim O3 \\sim O3L \\sim
O3W \\sim O4 \\sim O4L \\sim O4W \\sim O5 \\sim O5L \\sim O5W \\sim O6 \\sim
O6L \\sim O6W \\sim O7 \\sim O7L \\sim O7W \\sim O8 \\sim O8L \\sim O8W \\sim
O9 \\sim O9L \\sim O9W \\sim O10 \\sim O10L \\sim O10W \\sim O11 \\sim O11L
\\sim O11W \\sim O12 \\sim O12L \\sim O12W \\sim O13 \\sim O13W \\sim O14 \\sim
O14W \\sim O15 \\sim O15W \\sim O16 \\sim O16W \\sim O17 \\sim O17W \\sim O18
\\sim O18W \\sim O19 \\sim O19W \\sim O20 \\sim O20W \\sim O21 \\sim O21W \\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 \\sim O92 \\sim O93 \\sim
O94 \\sim O95 \\sim O96 \\sim O97 \\sim O98 \\sim O99 \\sim O100 \\sim O101
\\sim O102 \\sim O103 \\sim O104 \\sim O105 \\sim O106 \\sim O107 \\sim O108
\\sim O109 \\sim O110 \\sim O111 \\sim O112 \\sim O113 \\sim O114 \\sim O115
\\sim O116 \\sim O117 \\sim O118 \\sim O119 \\sim O120 \\sim O121 \\sim O122
\\sim O123 \\sim O124 \\sim O125 \\sim O126 \\sim O127 \\sim O128 \\sim O129
\\sim O130 \\sim O131 \\sim O132 \\sim O133 \\sim O134 \\sim O135 \\sim O136
\\sim O137 \\sim O138 \\sim O139 \\sim O140 \\sim O142 \\sim O143 \\sim O144
\\sim O145 \\sim O22W \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6
\\sim C7 \\sim C8: within 3.5A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 3.5A
Uanis(Na1) \\sim Ueq, Uanis(Na2) \\sim Ueq, Uanis(Na3) \\sim Ueq, Uanis(Na4)
\\sim Ueq, Uanis(Na5) \\sim Ueq, Uanis(Na6) \\sim Ueq, Uanis(Na7) \\sim Ueq,
Uanis(Na8) \\sim Ueq, Uanis(Na9) \\sim Ueq, Uanis(Na10) \\sim Ueq, Uanis(Na11)
\\sim Ueq, Uanis(Na12) \\sim Ueq, Uanis(Na13) \\sim Ueq, Uanis(Na14) \\sim Ueq,
Uanis(Na15) \\sim Ueq, Uanis(Na16) \\sim Ueq, Uanis(Na17) \\sim Ueq,
Uanis(Na18) \\sim Ueq, Uanis(Na19) \\sim Ueq, Uanis(Na20) \\sim Ueq, Uanis(O50)
\\sim Ueq, Uanis(O16W) \\sim Ueq, Uanis(O17W) \\sim Ueq, Uanis(O21W) \\sim Ueq,
Uanis(Na19) \\sim Ueq, Uanis(O22W) \\sim Ueq, Uanis(Na20) \\sim Ueq: with sigma
of 0.003 and sigma for terminal atoms of 0.006
3. Others
 Fixed Sof: Na4(0.35) Na5(0.25) Na6(0.6) Na7(0.3) Na8(0.5) Na9(0.25)
 Na10(0.35) Na11(0.5) Na12(0.4) Na13(0.5) Na14(0.5) Na15(0.5) Na16(0.65)
 Na17(0.35) Na18(0.5) O16W(0.25) O17W(0.3) O18W(0.35) O19W(0.5) O21W(0.7)
 Na19(0.2) O22W(0.4) Na20(0.3)
4.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7)
;
_shelx_res_checksum              45093
_shelx_hkl_checksum              26458
_shelx_fab_checksum              1411
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'