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

data_4327037
_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_absolute_configuration ad
_chemical_formula_moiety         'C10 H24 Cl2 N4 O1 Ti1'
_chemical_formula_sum            'C10 H24 Cl2 N4 O Ti'
_chemical_formula_weight         335.13
_chemical_name_systematic
;
Ti(NOtBu)(Me3[6]aneN3)Cl2
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   7.0669(2)
_cell_length_b                   12.7144(3)
_cell_length_c                   18.4571(5)
_cell_measurement_reflns_used    3817
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      5
_cell_volume                     1658.40(8)
_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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.045
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8337
_diffrn_reflns_theta_full        25.468
_diffrn_reflns_theta_max         25.468
_diffrn_reflns_theta_min         5.277
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.834
_exptl_absorpt_correction_T_max  0.96
_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            pink
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       plate
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.19
_refine_diff_density_min         -0.29
_refine_ls_abs_structure_details 'Flack (1983), 1252 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0571
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2451
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.0005844
_refine_ls_shift/su_mean         0.0000262
_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: 
 0.723 0.143 0.512 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0450
_refine_ls_wR_factor_gt          0.0388
_refine_ls_wR_factor_ref         0.0378
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                2594
_reflns_number_total             2999
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.19
_oxford_diffrn_Wilson_scale      5.24
_oxford_refine_ls_r_factor_ref   0.0333
_oxford_refine_ls_scale          0.4200(8)
_oxford_reflns_number_all        2999
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic201896q_si_002_05.cif
_cod_data_source_block           COMPOUND_4
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C10 H24 Cl2 N4 O1 Ti1'
_cod_database_code               4327037