Radical and Thermal Reactions of N-Heterocyclic Carbene Boranes with Diazo Compounds
Allen, Thomas H.; Geib, Steven J.; Curran, Dennis P.; Organometallics 35 (2016) 2975–; doi:10.1021/acs.organomet.6b00497

data_4088860
_publ_section_title
;
 Radical and Thermal Reactions of N-Heterocyclic Carbene Boranes with
 Diazo Compounds
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2975
_journal_paper_doi               10.1021/acs.organomet.6b00497
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C11 H17 B N4 O4'
_chemical_formula_weight         280.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90.0104(18)
_cell_angle_beta                 96.5593(17)
_cell_angle_gamma                91.4265(19)
_cell_formula_units_Z            2
_cell_length_a                   7.8797(3)
_cell_length_b                   8.5109(4)
_cell_length_c                   10.1918(4)
_cell_measurement_reflns_used    5600
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      68.259
_cell_measurement_theta_min      4.367
_cell_volume                     678.81(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker X8 Prospector Ultra Cu ImuS'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10760
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.365
_diffrn_reflns_theta_min         4.367
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Sadabs'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       needle
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.0044(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.472
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.472
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0680P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2234
_reflns_number_total             2430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00497_si_002.cif
_cod_data_source_block           tomallen3_a
_cod_database_code               4088860
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              23226
_shelx_hkl_checksum              71787