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_7013321
_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 H38 N2'
_chemical_formula_sum            'C25 H38 N2'
_chemical_formula_weight         366.57
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2003-07-28T09:43:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.31(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.111(2)
_cell_length_b                   11.650(3)
_cell_length_c                   15.729(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      23.7
_cell_measurement_theta_min      13.2
_cell_measurement_wavelength     0.71073
_cell_volume                     2267.3(9)
_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      203(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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      -0.39845E-1
_diffrn_orient_matrix_UB_12      -0.1165E-2
_diffrn_orient_matrix_UB_13      -0.66241E-1
_diffrn_orient_matrix_UB_21      0.42127E-1
_diffrn_orient_matrix_UB_22      0.68523E-1
_diffrn_orient_matrix_UB_23      -0.7895E-2
_diffrn_orient_matrix_UB_31      0.56313E-1
_diffrn_orient_matrix_UB_32      -0.05177
_diffrn_orient_matrix_UB_33      -0.9048E-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  0.2799
_diffrn_reflns_av_unetI/netI     0.1959
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12063
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.22
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        6
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.062
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       0.004(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   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1935
_refine_ls_R_factor_gt           0.1074
_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^)+(0.1448P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2531
_refine_ls_wR_factor_ref         0.3275
_reflns_number_gt                1849
_reflns_number_total             3954
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306401h.txt
_cod_data_source_block           3b
_cod_original_cell_volume        2267.4(8)
_cod_database_code               7013321
_diffrn_standards_decay_corr_max 1.156
_diffrn_standards_decay_corr_min 0.996