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

data_4327042
_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         'C21 H28 Cl1 N5 O1 Ti1, 0.5 (C7 H8)'
_chemical_formula_sum            'C24.5 H32 Cl N5 O Ti'
_chemical_formula_weight         495.91
_chemical_name_systematic
; 
Ti(NC4H3CH2NMe2)(NOtBu)Cl(bipy)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 101.8811(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6310(3)
_cell_length_b                   11.7210(2)
_cell_length_c                   24.2188(5)
_cell_measurement_reflns_used    13076
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      9
_cell_volume                     5175.45(17)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_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      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13076
_diffrn_reflns_theta_full        74.043
_diffrn_reflns_theta_max         76.333
_diffrn_reflns_theta_min         3.730
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.947
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.91
_refine_diff_density_min         -0.94
_refine_ls_extinction_coef       20.136
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.1130
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4591
_refine_ls_number_restraints     43
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.0079340
_refine_ls_shift/su_mean         0.0000978
_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: 
 3.62 -9.25 -1.11 -3.19 -2.77 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0369
_refine_ls_wR_factor_gt          0.0346
_refine_ls_wR_factor_ref         0.0337
_reflns_limit_h_max              22
_reflns_limit_h_min              -23
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                4813
_reflns_number_total             5360
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.11
_oxford_diffrn_Wilson_scale      0.24
_oxford_refine_ls_r_factor_ref   0.0396
_oxford_refine_ls_scale          1.908(2)
_oxford_reflns_number_all        5339
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ic201896q_si_002_10.cif
_cod_data_source_block           COMPOUND_11
_cod_original_cell_volume        5175.42(17)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C24.50 H32 Cl1 N5 O1 Ti1'
_cod_database_code               4327042