Reactions of Titanium Hydrazides with Silanes and Boranes: N-N Bond Cleavage and N Atom Functionalization.
Stevenson, Laura C.; Mellino, Simona; Clot, Eric; Mountford, Philip; Journal of the American Chemical Society 137 (2015) 10140–10143; doi:10.1021/jacs.5b06627

data_4124240
_publ_section_title
;
 Reactions of Titanium Hydrazides with Silanes and Boranes: N-N Bond
 Cleavage and N Atom Functionalization.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10140
_journal_page_last               10143
_journal_paper_doi               10.1021/jacs.5b06627
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C31 H50 B1 N5 Ti1'
_chemical_formula_sum            'C31 H50 B N5 Ti'
_chemical_formula_weight         551.48
_chemical_name_systematic
;
Ti(N2iPrN){N(H)BC8H14}(NPh2)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 96.9475(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.21150(10)
_cell_length_b                   15.0835(2)
_cell_length_c                   20.0607(3)
_cell_measurement_reflns_used    7116
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3067.16(7)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            45334
_diffrn_reflns_theta_full        26.941
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         5.112
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.38
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0624
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         5689
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.0010937
_refine_ls_shift/su_mean         0.0000356
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 2.28 2.24 2.52 0.924 0.654 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0499
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0457
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                6007
_reflns_number_total             6983
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.97
_oxford_diffrn_Wilson_scale      4.07
_oxford_refine_ls_r_factor_ref   0.0562
_oxford_refine_ls_scale          0.4882(7)
_oxford_reflns_number_all        6983
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja5b06627_si_003.cif
_cod_data_source_block           COMPOUND_5
_cod_depositor_comments
'Adding full bibliography for 4124239--4124243.cif.'
_cod_original_cell_volume        3067.17(7)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C31 H50 B1 N5 Ti1'
_cod_database_code               4124240