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_7013318
_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         'C31 H49 B1 N2'
_chemical_formula_sum            'C31 H49 B N2'
_chemical_formula_weight         460.53
_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             2003-07-27T22:29:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                102.29(5)
_cell_angle_beta                 94.25(5)
_cell_angle_gamma                112.19(7)
_cell_formula_units_Z            2
_cell_length_a                   8.539(8)
_cell_length_b                   9.459(7)
_cell_length_c                   19.457(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      11.9
_cell_measurement_theta_min      6.7
_cell_measurement_wavelength     0.71073
_cell_volume                     1401(2)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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      223(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.52965E-1
_diffrn_orient_matrix_UB_12      0.106571
_diffrn_orient_matrix_UB_13      0.34988E-1
_diffrn_orient_matrix_UB_21      -0.6925E-2
_diffrn_orient_matrix_UB_22      -0.51586E-1
_diffrn_orient_matrix_UB_23      0.40219E-1
_diffrn_orient_matrix_UB_31      0.117004
_diffrn_orient_matrix_UB_32      0.1102E-2
_diffrn_orient_matrix_UB_33      -0.3387E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5200
_diffrn_reflns_theta_full        24.93
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         2.37
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_correction_T_min  0.9724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1298
_refine_ls_R_factor_gt           0.0793
_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^)+(0.1577P)^2^+0.2040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.214
_refine_ls_wR_factor_ref         0.2562
_reflns_number_gt                2988
_reflns_number_total             4876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306401h.txt
_cod_data_source_block           2a
_cod_original_cell_volume        1401.0(17)
_cod_database_code               7013318
_exptl_absorpt_factor_mur        0.019
_exptl_absorpt_correction_t_ave  0.9602
_diffrn_standards_decay_corr_max 1.049
_diffrn_standards_decay_corr_min 0.991