Ni-Catalyzed Carboxylation of C(sp2)–S Bonds with CO2: Evidence for the Multifaceted Role of Zn
Yanagi, Tomoyuki; Somerville, Rosie J.; Nogi, Keisuke; Martin, Ruben; Yorimitsu, Hideki; ACS Catalysis  (2020) 2117–2123; doi:10.1021/acscatal.9b05141

data_4517327
_publ_section_title
;
 Ni-Catalyzed Carboxylation of C(sp2)--S Bonds with CO2: Evidence for the
 Multifaceted Role of Zn
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              2117
_journal_page_last               2123
_journal_paper_doi               10.1021/acscatal.9b05141
_journal_year                    2020
_chemical_formula_sum            'C28 H24 Br N4 Ni'
_chemical_formula_weight         555.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.3683(6)
_cell_length_b                   11.2848(5)
_cell_length_c                   32.6128(13)
_cell_measurement_reflns_used    17630
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5930
_cell_measurement_theta_min      2.4650
_cell_volume                     4551.9(3)
_computing_cell_refinement
'CrysAlisPro 1.171.40.53 64bit (Rigaku OD, 2019)'
_computing_data_collection
'CrysAlisPro 1.171.40.53 64bit (Rigaku OD, 2019)'
_computing_data_reduction
'CrysAlisPro 1.171.40.53 64bit (Rigaku OD, 2019)'
_computing_molecular_graphics
'shelXle (H&#x00FC;bschle, Sheldrick and Dittirch, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    Sir2019
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'PILATUS 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  '1/4chi goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_radiation_monochromator  'Confocal Max Flux optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1289
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_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       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            101654
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.210
_diffrn_reflns_theta_min         2.498
_diffrn_source                   'Microfocus rotating anode X-ray tube'
_diffrn_source_current           24
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Rigaku MicroMax-007HF'
_exptl_absorpt_coefficient_mu    2.634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       Block
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.796
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         7802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0496P)^2^+22.4456P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4571
_reflns_number_total             7802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b05141_si_003.cif
_cod_data_source_block           RJS9-64
_cod_depositor_comments
'Adding full bibliography for 4517326--4517327.cif.'
_cod_database_code               4517327
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.693
_shelx_estimated_absorpt_t_max   0.880
_shelx_res_checksum              47357
_shelx_hkl_checksum              80784