Rhodium(I)-Catalyzed Directed Trideuteromethylation of (Hetero)arene C–H Bonds with CD3CO2D
Zhao, Haoqiang; Zeng, Qi; yang, ji; Xu, Bing; Lei, Haimin; Xu, Lijin; Walsh, Patrick; Organic & Biomolecular Chemistry  (2022) –; doi:10.1039/D2OB01581A

data_7158885
_publ_section_title
;
 Rhodium(I)-Catalyzed Directed Trideuteromethylation of (Hetero)arene C--H
 Bonds with CD3CO2D
;
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_paper_doi               10.1039/D2OB01581A
_journal_year                    2022
_chemical_formula_sum            'C15 H17 N4'
_chemical_formula_weight         253.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2021-08-07 deposited with the CCDC.	2022-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.168(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5969(7)
_cell_length_b                   7.4254(3)
_cell_length_c                   15.4359(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1327.39(13)
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.944
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7148
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.048
_diffrn_reflns_theta_min         3.817
_exptl_absorpt_coefficient_mu    0.618
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_F_000             540
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0025(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0716P)^2^+0.1858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1257
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2113
_reflns_number_total             2547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ob01581a2.cif
_cod_data_source_block           exp_5929
_cod_original_cell_volume        1327.40(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7158885
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              83904
_shelx_hkl_checksum              85353