Kinetic isotope effect offers selectivity in CO<sub>2</sub> reduction.
Patra, Suman; Atta, Sayan; Ghosh, Soumili; Majumdar, Amit; Dey, Abhishek; Chemical communications (Cambridge, England) 60 (2024) 4826–4829; doi:10.1039/d3cc06336d

data_7132928
_publ_section_title
;
 Kinetic isotope effect offers selectivity in CO<sub>2</sub> reduction.
;
_journal_issue                   36
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4826
_journal_page_last               4829
_journal_paper_doi               10.1039/d3cc06336d
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C42 H40 N6 Ni2 O4, 2(C24 H20 B)'
_chemical_formula_sum            'C90 H80 B2 N6 Ni2 O4'
_chemical_formula_weight         1448.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-22 deposited with the CCDC.	2024-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 123.2990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.431(2)
_cell_length_b                   24.9205(17)
_cell_length_c                   24.931(3)
_cell_measurement_reflns_used    25990
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.40
_cell_volume                     16841(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      144.99
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8VENTURE with PHOTON II Detector'
_diffrn_measurement_method       'phi, omega and kappa scan'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            79376
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.058
_diffrn_reflns_theta_max         25.058
_diffrn_reflns_theta_min         2.220
_diffrn_source_type              Micro-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6131
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0863 before and 0.0731 after correction.
The Ratio of minimum to maximum transmission is 0.8227.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6080
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     943
_refine_ls_number_reflns         14855
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0301P)^2^+12.9768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11992
_reflns_number_total             14855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06336d2.cif
_cod_data_source_block           mo_am260821_0ma
_cod_depositor_comments
'Adding full bibliography for 7132928--7132929.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7132928
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.890
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C5-C4 \\sim C25B-C24 \\sim C25A-C24
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C25B) = Uanis(C25A)
4. Others
 Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C15(H15A,H15B), C21(H21A,H21B), C30(H30A,H30B), C36(H36A,H36B),
 C42(H42A,H42B)
5.b Me refined with riding coordinates:
 C5(H5A,H5B,H5C)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17),
 C18(H18), C19(H19), C20(H20), C23(H23), C26(H26), C29(H29), C32(H32), C33(H33),
  C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), C44(H44),
 C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53),
  C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60), C62(H62),
 C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71),
  C72(H72), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C80(H80),
 C81(H81), C82(H82), C83(H83), C84(H84), C86(H86), C87(H87), C88(H88), C89(H89),
  C90(H90)
5.d Idealised Me refined as rotating group:
 C25A(H25A,H25B,H25C), C25B(H25D,H25E,H25F)
;
_shelx_res_checksum              84199
_shelx_hkl_checksum              90166
_shelx_fab_checksum              24798
_olex2_submission_special_instructions 'No special instructions were received'