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_7246180
_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         'C52 H46 Co2 N16 O12, O40 P W12, 2(H2 O)'
_chemical_formula_sum            'C52 H51 Co2 N16 O54 P W12'
_chemical_formula_weight         4119.12
_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                66.873(2)
_cell_angle_beta                 73.720(2)
_cell_angle_gamma                84.454(2)
_cell_formula_units_Z            1
_cell_length_a                   12.3693(7)
_cell_length_b                   13.7755(8)
_cell_length_c                   13.7884(8)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    279(2)
_cell_measurement_theta_max      27.488
_cell_measurement_theta_min      2.689
_cell_volume                     2073.8(2)
_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      279.0
_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  0.0576
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35312
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.69
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.086
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3184
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear pinkish pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    3.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.962
_refine_diff_density_min         -6.236
_refine_diff_density_rms         0.412
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         7369
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0709P)^2^+119.4647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1596
_reflns_number_gt                6595
_reflns_number_total             7369
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2ce01634f2.cif
_cod_data_source_block           314
_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 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7246180--7246184.cif.
;
_cod_database_code               7246180
_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. Restrained distances
 O3-O4
 2.1 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(O18A) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O14)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.008 and
sigma for terminal atoms of 0.016
Uanis(O9) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O26)
\\sim Ueq, Uanis(O16A) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.004
Uanis(O16B) = Uanis(O16A)
Uanis(O18B) = Uanis(O18A)
4. Others
 Sof(O18B)=Sof(O16B)=1-FVAR(1)
 Sof(O16A)=Sof(O18A)=FVAR(1)
 Fixed Sof: O8(0.5) O9(0.5) O17(0.5) O26(0.5)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
5.b 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), N5(H5A)
;
_olex2_submission_special_instructions 'No special instructions were received'