Titanium tert-Butoxyimido Compounds
Andrew D. Schwarz; Ainara Nova; Eric Clot; Philip Mountford; Inorganic Chemistry 50 (2011) 12155–12171; doi:10.1021/ic201896q

data_4327038
_publ_contact_author
;
 Prof P. Mountford           
 Chemistry Research Laboratory
 Mansfield Road
 Oxford
 OX1 3TA
 UK
;
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 285141'
_publ_contact_author_phone       '+44 1865 285140'
_publ_section_title
;
 Titanium tert-Butoxyimido Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12155
_journal_page_last               12171
_journal_paper_doi               10.1021/ic201896q
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C19 H24 Cl2 N4 O1 Ti1'
_chemical_formula_sum            'C19 H24 Cl2 N4 O Ti'
_chemical_formula_weight         443.23
_chemical_name_systematic
;
Ti(NOtBu)Cl2(py)3
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 97.1358(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.79620(10)
_cell_length_b                   21.8932(3)
_cell_length_c                   11.4868(2)
_cell_measurement_reflns_used    4544
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2194.96(5)
_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 0.990
_diffrn_measured_fraction_theta_max 0.989
_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  0.028
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8673
_diffrn_reflns_theta_full        26.104
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         5.140
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.26
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.1111
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3235
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.0003448
_refine_ls_shift/su_mean         3.4503958
_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: 
 0.292 -0.198E-02 0.312E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0673
_refine_ls_wR_factor_gt          0.0335
_refine_ls_wR_factor_ref         0.0307
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                3570
_reflns_number_total             4991
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.01
_oxford_diffrn_Wilson_scale      9.87
_oxford_refine_ls_r_factor_ref   0.0323
_oxford_refine_ls_scale          0.3122(3)
_oxford_reflns_number_all        4991
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title '9011420 ADS141'
_cod_data_source_file            ic201896q_si_002_06.cif
_cod_data_source_block           COMPOUND_5
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C19 H24 Cl2 N4 O1 Ti1'
_cod_database_code               4327038