Co(dppbsa)-catalyzed reductive N,N-dimethylation of nitroaromatics with CO2 and hydrosilane
Ma, Shuang-Shuang; Sun, Rui; Zhang, Zi-Heng; Guan, Peng-Xin; Lin, Jin-Qing; Li, Chun-Shan; Xu, Bao-Hua; Green Chemistry 25 (2023) 8625–8632; doi:10.1039/D3GC02517A

data_7247437
_publ_section_title
;
 Co(dppbsa)-catalyzed reductive N,N-dimethylation of nitroaromatics with
 CO2 and hydrosilane
;
_journal_issue                   21
_journal_name_full               'Green Chemistry'
_journal_page_first              8625
_journal_page_last               8632
_journal_paper_doi               10.1039/D3GC02517A
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_sum            'C29 H31 Cl2 Co I O3 P S'
_chemical_formula_weight         747.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-02-02 deposited with the CCDC.	2023-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.510(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7008(4)
_cell_length_b                   13.6759(3)
_cell_length_c                   11.2342(5)
_cell_measurement_reflns_used    5651
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.4130
_cell_measurement_theta_min      2.4530
_cell_volume                     1507.58(11)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12198
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.782
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.603
_diffrn_reflns_theta_min         2.475
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.922
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       block
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 2447 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7272
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    0.905
_reflns_Friedel_fraction_max     0.711
_reflns_number_gt                6364
_reflns_number_total             7272
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3gc02517a2.cif
_cod_data_source_block           3
_cod_depositor_comments          'Adding full bibliography for 7247437.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7247437
_shelx_shelxl_version_number     2014/7
_oxdiff_exptl_absorpt_empirical_full_min 0.746
_oxdiff_exptl_absorpt_empirical_full_max 1.626
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              97506
_shelx_hkl_checksum              66975