Diversion of Catalytic C-N Bond Formation to Catalytic Oxidation of NH<sub>3</sub> through Modification of the Hydrogen Atom Abstractor.
Dunn, Peter L.; Johnson, Samantha I.; Kaminsky, Werner; Bullock, R. Morris; Journal of the American Chemical Society 142 (2020) 3361–3365; doi:10.1021/jacs.9b13706

data_4134151
_publ_section_title
;
 Diversion of Catalytic C-N Bond Formation to Catalytic Oxidation of
 NH<sub>3</sub> through Modification of the Hydrogen Atom Abstractor.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3361
_journal_page_last               3365
_journal_paper_doi               10.1021/jacs.9b13706
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         '2(C33 H35 O), C2 H3 N'
_chemical_formula_sum            'C68 H73 N O2'
_chemical_formula_weight         936.27
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90.781(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8007(8)
_cell_length_b                   15.2538(10)
_cell_length_c                   18.0720(12)
_cell_measurement_reflns_used    10718
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.211
_cell_measurement_theta_min      2.349
_cell_volume                     2701.5(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker AXS Area Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24074
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.270
_diffrn_reflns_theta_min         2.078
_exptl_absorpt_coefficient_mu    0.068
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         12579
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0528P)^2^+0.3102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                10997
_reflns_number_total             12579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13706_si_003.cif
_cod_data_source_block           4tritylArO_0m_b
_cod_depositor_comments
'Adding full bibliography for 4134149--4134151.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4134151
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              72901
_shelx_hkl_checksum              4127