Copper(i) and cobalt(ii) frameworks with a tetraphenylethene–imidazole ligand for the electroreduction of CO2 to CH4
Wang, Fang-Fang; Wang, Yu-Jie; Qiu, Zhao-Feng; Zhang, Kai-Yang; Zhao, Yue; Sun, Wei-Yin; CrystEngComm 26 (2024) 6465–6471; doi:10.1039/D4CE00991F

data_7249488
_publ_section_title
;
 Copper(i) and cobalt(ii) frameworks with a tetraphenylethene--imidazole
 ligand for the electroreduction of CO2 to CH4
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              6465
_journal_page_last               6471
_journal_paper_doi               10.1039/D4CE00991F
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C19 H14 Cu N4, Cl O4'
_chemical_formula_sum            'C19 H14 Cl Cu N4 O4'
_chemical_formula_weight         461.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-29 deposited with the CCDC.	2024-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.940(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5135(5)
_cell_length_b                   15.5149(5)
_cell_length_c                   11.9063(5)
_cell_measurement_reflns_used    5737
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      53.76
_cell_measurement_theta_min      4.18
_cell_volume                     2112.70(14)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX5 V2023.9-2 (Bruker, 2023)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE MetalJet PHOTON II'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12530
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.979
_diffrn_reflns_theta_min         4.178
_diffrn_source                   MetalJet
_diffrn_source_current           2.85
_diffrn_source_power             0.1986735
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.537
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1105 before and 0.0509 after correction.
The Ratio of minimum to maximum transmission is 0.9075.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.482(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         3765
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0733P)^2^+2.7305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    0.946
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                3241
_reflns_number_total             3765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00991f2.cif
_cod_data_source_block           Cu-MOF
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' 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 7249488--7249489.cif.
;
_cod_original_cell_volume        2112.69(14)
_cod_database_code               7249488
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.591
_shelx_estimated_absorpt_t_min   0.508
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.518(9)
 0.482(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 Cl1A-O1A \\sim Cl1A-O2A \\sim Cl1A-O3A \\sim Cl1A-O4A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Cl1B \\sim O1B \\sim O2B \\sim O3B \\sim O4B \\sim Cl1A \\sim O1A \\sim O2A
\\sim O3A \\sim O4A: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
5. Same fragment restrains
{Cl1B, O1B, O2B, O3B, O4B} sigma for 1-2: 0.01, 1-3: 0.02
as in
{Cl1A, O1A, O2A, O3A, O4A}
6. Others
 Sof(Cl1B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=1-FVAR(1)
 Sof(Cl1A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              343
_shelx_hkl_checksum              65064
_shelx_fab_checksum              49924
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU