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_7018082
_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_absolute_configuration ad
_chemical_formula_moiety         'C20 H39 N4 Ti1, C24 H20 B1'
_chemical_formula_sum            'C44 H59 B N4 Ti'
_chemical_formula_weight         702.69
_chemical_name_systematic
;
[Cp*Ti{MeC(NiPr)2}{N(H)(NMe2)}][BPh4]
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.0165(4)
_cell_length_b                   15.8661(2)
_cell_length_c                   8.97260(10)
_cell_measurement_reflns_used    8605
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3988.43(9)
_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 0.990
_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  0.039
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            26420
_diffrn_reflns_theta_full        26.911
_diffrn_reflns_theta_max         27.460
_diffrn_reflns_theta_min         5.191
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.96
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.49
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1289
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         6840
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.001904
_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:
1.80 0.960 1.73 0.178 0.351
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0695
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0576
_reflns_limit_h_max              36
_reflns_limit_h_min              0
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              -11
_reflns_number_gt                7420
_reflns_number_total             8965
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.67
_oxford_diffrn_Wilson_scale      4.58
_oxford_refine_ls_r_factor_ref   0.0519
_oxford_refine_ls_scale          0.4725(8)
_oxford_reflns_number_all        8965
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c2dt12359b.txt
_cod_data_source_block           compound_23-BPh4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 n a 21 '
_cod_original_formula_sum        'C44 H59 B1 N4 Ti1'
_cod_database_code               7018082