Site selectivity and reversibility in the reactions of titanium hydrazides with Si-H, Si-X, C-X and H(+) reagents: Ti[double bond, length as m-dash]N(α) 1,2-silane addition, N(β) alkylation, N(α) protonation and σ-bond metathesis.
Tiong, Pei Jen; Nova, Ainara; Schwarz, Andrew D.; Selby, Jonathan D.; Clot, Eric; Mountford, Philip; Dalton transactions (Cambridge, England : 2003) 41 (2012) 2277–2288; doi:10.1039/c2dt12359b

data_7018074
_publ_section_title
;
 Site selectivity and reversibility in the reactions of titanium
 hydrazides with Si-H, Si-X, C-X and H(+) reagents: Ti[double bond, length
 as m-dash]N(\a) 1,2-silane addition, N(\b) alkylation, N(\a) protonation
 and \s-bond metathesis.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2277
_journal_page_last               2288
_journal_paper_doi               10.1039/c2dt12359b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C26 H45 Cl1 N4 Si1 Ti1'
_chemical_formula_sum            'C26 H45 Cl N4 Si Ti'
_chemical_formula_weight         525.11
_chemical_name_systematic
;
Cp*Ti{MeC(NiPr)2}(Cl){N(NMe2)SiH2Ph}
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                94.6300(11)
_cell_angle_beta                 99.7244(13)
_cell_angle_gamma                114.5284(13)
_cell_formula_units_Z            2
_cell_length_a                   9.8784(2)
_cell_length_b                   10.3809(3)
_cell_length_c                   15.6151(4)
_cell_measurement_reflns_used    5873
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1415.38(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_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 0.990
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11308
_diffrn_reflns_theta_full        25.554
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         5.125
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         3817
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.000408
_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:
0.993 0.560 0.687
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0858
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0548
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                4276
_reflns_number_total             6390
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.05
_oxford_diffrn_Wilson_scale      7.36
_oxford_refine_ls_r_factor_ref   0.0481
_oxford_refine_ls_scale          0.3741(8)
_oxford_reflns_number_all        6390
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c2dt12359b.txt
_cod_data_source_block           COMPOUND_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C26 H45 Cl1 N4 Si1 Ti1'
_cod_database_code               7018074