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_7249489
_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_formula_moiety         'C42 H28 Co F6 N8 O4, 2(C3 H7 N O)'
_chemical_formula_sum            'C48 H42 Co F6 N10 O6'
_chemical_formula_weight         1027.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-05
_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                 93.932(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0501(15)
_cell_length_b                   13.4447(13)
_cell_length_c                   24.018(3)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      53.844
_cell_measurement_theta_min      3.209
_cell_volume                     4848.5(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            58700
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.188
_diffrn_reflns_theta_min         2.927
_diffrn_source_current           2.86
_diffrn_source_power             0.19931339999999997
_diffrn_source_voltage           69.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.396
_exptl_absorpt_correction_T_max  0.3012
_exptl_absorpt_correction_T_min  0.2024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1675 before and 0.0816 after correction.
The Ratio of minimum to maximum transmission is 0.6720.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         8906
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1169P)^2^+5.8011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1935
_refine_ls_wR_factor_ref         0.2031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7199
_reflns_number_total             8906
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00991f2.cif
_cod_data_source_block           Co-MOF
_cod_depositor_comments
'Adding full bibliography for 7249488--7249489.cif.'
_cod_original_cell_volume        4848.4(9)
_cod_database_code               7249489
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.762
_shelx_estimated_absorpt_t_min   0.715
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2A-C39A
 1.38 with sigma of 0.02
 C40A-F3A
 1.35 with sigma of 0.02
 C39A-C40A
 1.53 with sigma of 0.02
 C40A-F1A
 1.36 with sigma of 0.02
 C40A-F2A
 1.37 with sigma of 0.02
 F3A-F2A = F2A-F1A
 2 with sigma of 0.02
 C39A-F1A = C39A-F3A
 2.4 with sigma of 0.04
 C39A-F2A
 2.38 with sigma of 0.04
 O2A-C40A
 2.415 with sigma of 0.04
 F1A-C40A \\sim F2A-C40A \\sim F3A-C40A
 with sigma of 0.02
 F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.04
 F1A-C39A \\sim F2A-C39A \\sim F3A-C39A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O1A \\sim F1A \\sim O2A \\sim F2A \\sim F3A \\sim C39A \\sim C40A: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A
4. Others
 Sof(O1A)=Sof(F1A)=Sof(O2A)=Sof(F2A)=Sof(F3A)=Sof(C39A)=Sof(C40A)=1-FVAR(1)
 Sof(O1)=Sof(F1)=Sof(F2)=Sof(O2)=Sof(F3)=Sof(C39)=Sof(C40)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C12(H12), C13(H13),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C34(H34),
 C35(H35), C36(H36), C37(H37), C38(H38), C46(H46), C43(H43)
5.b Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C44(H44A,H44B,H44C), C45(H45A,H45B,
 H45C)
;
_shelx_res_checksum              27294
_shelx_hkl_checksum              64648
_olex2_submission_special_instructions 'No special instructions were received'