Synthesis and Catalytic Reactivity of Bis(amino)cyclopropenylidene Carbene–Borane Adducts
Huchenski, Blake S. N.; Adams, Matt R.; McDonald, Robert; Ferguson, Michael J.; Speed, Alexander W. H.; Organometallics 35 (2016) 3101–; doi:10.1021/acs.organomet.6b00654

data_4086728
_publ_section_title
;
 Synthesis and Catalytic Reactivity of Bis(amino)cyclopropenylidene
 Carbene--Borane Adducts
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              3101
_journal_paper_doi               10.1021/acs.organomet.6b00654
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C33 H43 B N2'
_chemical_formula_sum            'C33 H43 B N2'
_chemical_formula_weight         478.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                113.9745(6)
_cell_angle_beta                 90.0092(7)
_cell_angle_gamma                93.4348(7)
_cell_formula_units_Z            4
_cell_length_a                   10.79160(10)
_cell_length_b                   15.6476(2)
_cell_length_c                   19.1459(3)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.16
_cell_measurement_theta_min      3.10
_cell_volume                     2947.73(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20770
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.208
_diffrn_reflns_theta_min         2.527
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  0.9333
_exptl_absorpt_correction_T_min  0.8233
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       needle
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         11229
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0507P)^2^+0.6030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9699
_reflns_number_total             11229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00654_si_003.cif
_cod_data_source_block           dal1633
_cod_database_code               4086728
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.858
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              99587
_shelx_hkl_checksum              1734