Five new multifunctional inorganic–organic hybrids based on Keggin-type polyoxometalates and a 3,5-di(1H-imidazol-1-yl)benzoic acid ligand
Yu, Xiao-Yang; Lv, Yanxin; Weng, Xiaoyu; Geng, Jiaqi; Yang, Yanyan; Jin, Hua; Cui, Hao; Fu, Bo; Qu, Xiaoshu; Shi, Hongfei; Cao, Xueling; CrystEngComm 25 (2023) 2185–2195; doi:10.1039/D2CE01634F

data_7246182
_publ_section_title
;
 Five new multifunctional inorganic--organic hybrids based on Keggin-type
 polyoxometalates and a 3,5-di(1H-imidazol-1-yl)benzoic acid ligand
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2185
_journal_page_last               2195
_journal_paper_doi               10.1039/D2CE01634F
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C26 H22 Ag N8 O44 P W12, 2(H2 O)'
_chemical_formula_sum            'C26 H26 Ag N8 O46 P W12'
_chemical_formula_weight         3531.59
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-12-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.08.17 svn.r3210 for OlexSys, GUI svn.r5083)
;
_audit_update_record
;
2022-12-07 deposited with the CCDC.	2023-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                87.0880(10)
_cell_angle_beta                 74.5420(10)
_cell_angle_gamma                88.0950(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2571(5)
_cell_length_b                   13.5874(4)
_cell_length_c                   16.3513(6)
_cell_measurement_reflns_used    112479
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55.014
_cell_measurement_theta_min      5.174
_cell_volume                     2834.55(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            112479
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.59
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    24.719
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5052
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    4.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.791
_refine_diff_density_min         -2.488
_refine_diff_density_rms         0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     850
_refine_ls_number_reflns         13001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0119P)^2^+62.4615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                10284
_reflns_number_total             13001
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2ce01634f2.cif
_cod_data_source_block           yxy309
_cod_depositor_comments
'Adding full bibliography for 7246180--7246184.cif.'
_cod_database_code               7246182
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H,H,H) groups
2.a Free rotating group:
 O45(H45a,H45b,H46a,H46b,O46)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C18(H18), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), N4(H4), N8(H8)
2.c Idealised tetrahedral OH refined as rotating group:
 O41(H41), O44(H44)
;
_olex2_submission_special_instructions 'No special instructions were received'