Carbodiimide Synthesis via Ti-Catalyzed Nitrene Transfer from Diazenes to Isocyanides
Beaumier, Evan P.; McGreal, Meghan E.; Pancoast, Adam R.; Wilson, R. Hunter; Moore, James T.; Graziano, Brendan J.; Goodpaster, Jason D.; Tonks, Ian A.; ACS Catalysis  (2019) 11753–; doi:10.1021/acscatal.9b04107

data_4516585
_publ_section_title
;
 Carbodiimide Synthesis via Ti-Catalyzed Nitrene Transfer from Diazenes to
 Isocyanides
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              11753
_journal_paper_doi               10.1021/acscatal.9b04107
_journal_year                    2019
_chemical_formula_moiety         'C28.5 H39 Br4 N6 Ti2 Cl1'
_chemical_formula_sum            'C28.5 H39 Br4 Cl N6 Ti2'
_chemical_formula_weight         916.54
_chemical_name_common            19019
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.789(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.481(2)
_cell_length_b                   9.2829(7)
_cell_length_c                   32.174(3)
_cell_measurement_reflns_used    9913
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.2965
_cell_measurement_theta_min      2.385
_cell_volume                     7101.0(10)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            64204
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         2.355
_diffrn_source                   fine
_exptl_absorpt_coefficient_mu    5.055
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       plates
_exptl_crystal_F_000             3624
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         8817
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0054P)^2^+98.2898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7314
_reflns_number_total             8817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b04107_si_002.cif
_cod_data_source_block           mo_19019_0m_a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C28.50 H39 Br4 Cl N6 Ti2'
_cod_database_code               4516585
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.719
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              25415
_shelx_hkl_checksum              7774