Sulfate-modified Ti IV -Zr IV -heterometallic germanotungstate used for catalyzing Knoevenagel condensation reaction
Gong, Peijun; Li, Hailou; Zhao, Junwei; Yang, Guo-Yu; CrystEngComm  (2026) –; doi:10.1039/D5CE01157D

data_7251836
_publ_section_title
;
 Sulfate-modified TiIV--ZrIV-heterometallic germanotungstate used for
 catalyzing the Knoevenagel condensation reaction
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              2979
_journal_page_last               2986
_journal_paper_doi               10.1039/D5CE01157D
_journal_volume                  28
_journal_year                    2026
_chemical_formula_sum
'C39 H250 Ge4 K4.5 N18.5 Na O223 S4 Ti12 W36 Zr4'
_chemical_formula_weight         12723.40
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2025-12-05 deposited with the CCDC.	2026-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                88.621(2)
_cell_angle_beta                 79.799(2)
_cell_angle_gamma                70.358(2)
_cell_formula_units_Z            2
_cell_length_a                   20.8839(14)
_cell_length_b                   24.4799(15)
_cell_length_c                   25.2479(18)
_cell_measurement_reflns_used    9745
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.28
_cell_volume                     11955.6(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            387581
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    18.510
_exptl_absorpt_correction_T_max  0.3573
_exptl_absorpt_correction_T_min  0.1557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    3.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             11548
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.410
_refine_diff_density_min         -2.185
_refine_diff_density_rms         0.236
_refine_ls_extinction_coef       0.000060(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2436
_refine_ls_number_reflns         42035
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+132.6724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                37128
_reflns_number_total             42035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d5ce01157d2.cif
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' 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 7251836.cif.
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_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum
'C39 H250 Ge4 K4.50 N18.50 Na O223 S4 Ti12 W36 Zr4'
_cod_database_code               7251836