Identification of Single-Atom Ni Site Active toward Electrochemical CO<sub>2</sub> Conversion to CO.
Kim, Haesol; Shin, Dongyup; Yang, Woojin; Won, Da Hye; Oh, Hyung-Suk; Chung, Min Wook; Jeong, Donghyuk; Kim, Sun Hee; Chae, Keun Hwa; Ryu, Ji Yeon; Lee, Junseong; Cho, Sung June; Seo, Jiwon; Kim, Hyungjun; Choi, Chang Hyuck; Journal of the American Chemical Society 143 (2021) 925–933; doi:10.1021/jacs.0c11008

data_4135562
_publ_section_title
;
 Identification of Single-Atom Ni Site Active toward Electrochemical
 CO<sub>2</sub> Conversion to CO.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              925
_journal_page_last               933
_journal_paper_doi               10.1021/jacs.0c11008
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety         'C44 H28 Cl N3 Ni O, 0.83(C H2 Cl2)'
_chemical_formula_sum            'C44.83 H29.67 Cl2.67 N3 Ni O'
_chemical_formula_weight         779.64
_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     iterative
_audit_creation_date             2019-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.949(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0656(5)
_cell_length_b                   21.6889(9)
_cell_length_c                   14.4031(6)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.512
_cell_measurement_theta_min      2.204
_cell_volume                     3673.3(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0563
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41881
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.524
_diffrn_reflns_theta_min         2.205
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1173 before and 0.0567 after correction. The Ratio of minimum to maximum transmission is 0.6361. The \l/2 correction factor is 0.00150.'
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       block
_exptl_crystal_F_000             1604
_refine_diff_density_max         1.245
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         6743
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0700
_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^)+(0.0559P)^2^+13.0740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5419
_reflns_number_total             6743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11008_si_002.cif
_cod_data_source_block           sjw01-1
_cod_database_code               4135562
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl2-Cl3
 3 with sigma of 0.02
 C46-Cl4 = C46-Cl5
 1.8 with sigma of 0.02
 Cl4-Cl5
 3 with sigma of 0.02
 C47-Cl6 = C47-Cl7
 1.8 with sigma of 0.02
 Cl6-Cl7
 3 with sigma of 0.02
 C45-Cl2 = C45-Cl3
 1.8 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C45) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C25) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(Cl3) \\sim Ueq, Uanis(Cl4) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Cl5) \\sim Ueq, Uanis(Cl6) \\sim Ueq, Uanis(Cl7) \\sim Ueq, Uanis(C24)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C45(0.33333) H45A(0.33333) H45B(0.33333) Cl2(0.33333) Cl3(0.33333)
 C46(0.25) H46A(0.25) H46B(0.25) Cl4(0.25) Cl5(0.25) C47(0.25) H47B(0.25)
 H47A(0.25) Cl6(0.25) Cl7(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C46(H46A,H46B), C47(H47B,H47A)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C18(H18),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
  C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
 C40(H40), C41(H41), C42(H42), C43(H43), C44(H44)
;
_shelx_res_checksum              74163
_shelx_hkl_checksum              24337
_olex2_submission_special_instructions 'No special instructions were received'