Borane and alane reductions of bulky N,N?-diaryl-1,3-diimines: structural characterization of products and intermediates in the diastereoselective synthesis of 1,3-diaminesElectronic supplementary information (ESI) available: preparative and characterization details; substructure of 5. See http://www.rsc.org/suppdata/dt/b3/b306401h/
Carey, David T.; Mair, Francis S.; Pritchard, Robin G.; Warren, John E.; Woods, Rebecca J.; Dalton Transactions  (2003) 3792–; doi:10.1039/b306401h

data_7013319
_publ_section_title
;
 Borane and alane reductions of bulky N,N?-diaryl-1,3-diimines:
 structural characterization of products and intermediates in the
 diastereoselective synthesis of 1,3-diaminesElectronic supplementary
 information (ESI) available: preparative and characterization details;
 substructure of 5. See http://www.rsc.org/suppdata/dt/b3/b306401h/
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              3792
_journal_paper_doi               10.1039/b306401h
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C25 H37 B1 N2'
_chemical_formula_sum            'C25 H37 B N2'
_chemical_formula_weight         376.38
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-07-28T01:40:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                77.6970(10)
_cell_angle_beta                 84.2240(10)
_cell_angle_gamma                89.6990(10)
_cell_formula_units_Z            4
_cell_length_a                   11.0205(2)
_cell_length_b                   12.6758(2)
_cell_length_c                   17.0392(3)
_cell_measurement_reflns_used    97996
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.373
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     2313.48(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.779832E-1
_diffrn_orient_matrix_UB_12      0.398881E-1
_diffrn_orient_matrix_UB_13      -0.73416E-2
_diffrn_orient_matrix_UB_21      -0.43833E-1
_diffrn_orient_matrix_UB_22      -0.572122E-1
_diffrn_orient_matrix_UB_23      0.428828E-1
_diffrn_orient_matrix_UB_31      0.178209E-1
_diffrn_orient_matrix_UB_32      0.407092E-1
_diffrn_orient_matrix_UB_33      0.418703E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1054
_diffrn_reflns_av_unetI/netI     0.1678
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14788
_diffrn_reflns_reduction_process
;
Scaled and merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.22
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         9001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1945
_refine_ls_R_factor_gt           0.0886
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+1.9984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1865
_refine_ls_wR_factor_ref         0.2372
_reflns_number_gt                4369
_reflns_number_total             9001
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306401h.txt
_cod_data_source_block           2b
_cod_database_code               7013319