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_7246184
_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         '0.5(C104 H92 N32 Ni4 O24), O40 P W12'
_chemical_formula_sum            'C52 H47 N16 Ni2 O52 P W12'
_chemical_formula_weight         4082.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 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                90.00
_cell_angle_beta                 97.709(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.2241(11)
_cell_length_b                   13.6928(7)
_cell_length_c                   17.4462(11)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.745
_cell_measurement_theta_min      2.780
_cell_volume                     4077.4(4)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      295.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0523
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            108631
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.79
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.432
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.2586
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3692
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.948
_refine_diff_density_min         -4.698
_refine_diff_density_rms         0.677
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         7179
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0956
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+825.0945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2655
_refine_ls_wR_factor_ref         0.2672
_reflns_number_gt                6850
_reflns_number_total             7179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2ce01634f2.cif
_cod_data_source_block           yxy308
_cod_depositor_comments
'Adding full bibliography for 7246180--7246184.cif.'
_cod_database_code               7246184
_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,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(O22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O7)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O13) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O8)
\\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O17) \\sim Ueq,
Uanis(O21) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(N1) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(O6) \\sim Ueq,
Uanis(O15) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C15)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O1(0.5) O2(0.5) O3(0.5) O4(0.5)
4.a Riding coordinates:
 N4(H4)
4.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C20(H20), C22(H22), C24(H24), C25(H25),
  C26(H26)
;
_olex2_submission_special_instructions 'No special instructions were received'