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_4124243
_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_absolute_configuration ad
_chemical_formula_moiety         'C26 H46 B1 N3 Ti1'
_chemical_formula_sum            'C26 H46 B N3 Ti'
_chemical_formula_weight         459.38
_chemical_name_systematic
;
Cp*Ti{MeC(NiPr)2){(NBC8H14)}
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 100.199(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6670(2)
_cell_length_b                   15.0475(3)
_cell_length_c                   10.9960(3)
_cell_measurement_reflns_used    7764
_cell_measurement_temperature    200
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     1411.40(6)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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      200
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13049
_diffrn_reflns_theta_full        74.716
_diffrn_reflns_theta_max         76.241
_diffrn_reflns_theta_min         4.085
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.668
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.46
_refine_ls_abs_structure_details 'Flack (1983), 2528 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.505(13)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9361
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5150
_refine_ls_number_restraints     112
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.0015383
_refine_ls_shift/su_mean         0.0002335
_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: 
 15.2 17.3 12.2 4.43 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0900
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0823
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              18
_reflns_limit_k_min              -18
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                5300
_reflns_number_total             5566
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.81
_oxford_diffrn_Wilson_scale      0.02
_oxford_refine_ls_r_factor_ref   0.0737
_oxford_refine_ls_scale          8.72(3)
_oxford_reflns_number_all        5549
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja5b06627_si_003.cif
_cod_data_source_block           COMPOUND_10
_cod_depositor_comments
'Adding full bibliography for 4124239--4124243.cif.'
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C26 H46 B1 N3 Ti1'
_cod_database_code               4124243