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_4086726
_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         'C15 H31 B N2'
_chemical_formula_sum            'C15 H31 B N2'
_chemical_formula_weight         250.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.1093(9)
_cell_length_b                   21.6601(10)
_cell_length_c                   8.1721(4)
_cell_measurement_reflns_used    6923
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.51
_cell_measurement_theta_min      6.17
_cell_volume                     3382.5(3)
_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 0.977
_diffrn_measured_fraction_theta_max 0.973
_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  0.0803
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5811
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.119
_diffrn_reflns_theta_min         6.177
_exptl_absorpt_coefficient_mu    0.415
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7478
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.983
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.3(10)
_refine_ls_extinction_coef       0.0011(3)
_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   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1661
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0823P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                1416
_reflns_number_total             1661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00654_si_004.cif
_cod_data_source_block           dal1639
_cod_database_code               4086726
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              48283
_shelx_hkl_checksum              21732