Synthesis and Reactivity of Titanium Hydrazido Complexes Supported by Diamido-Ether Ligands
Unruangsri, Junjuda; Morgan, Hannah; Schwarz, Andrew D.; Schofield, A. Daniel; Mountford, Philip; Organometallics 32 (2013) 3091–; doi:10.1021/om400311w

data_4080892
_publ_section_title
;
 Synthesis and Reactivity of Titanium Hydrazido Complexes Supported by
 Diamido-Ether Ligands
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              3091
_journal_paper_doi               10.1021/om400311w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C32 H43 F3 N4 O1 Si2 Ti1'
_chemical_formula_sum            'C32 H43 F3 N4 O Si2 Ti'
_chemical_formula_weight         660.79
_chemical_name_systematic
;
Ti(N2O)(CH2CH2NC(Me)C(C6H4CF3)NSiMe3)NPh2
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 96.1280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6564(2)
_cell_length_b                   10.49603(11)
_cell_length_c                   15.80991(17)
_cell_measurement_reflns_used    9581
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     3408.16(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.989
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18509
_diffrn_reflns_theta_full        74.269
_diffrn_reflns_theta_max         76.566
_diffrn_reflns_theta_min         4.305
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.196
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0880
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6318
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.0012216
_refine_ls_shift/su_mean         0.0000556
_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: 
 14.3 4.81 11.8 4.50 -0.142 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0406
_refine_ls_wR_factor_gt          0.0396
_refine_ls_wR_factor_ref         0.0393
_reflns_limit_h_max              25
_reflns_limit_h_min              -25
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                6526
_reflns_number_total             7072
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.76
_oxford_diffrn_Wilson_scale      0.06
_oxford_refine_ls_r_factor_ref   0.0342
_oxford_refine_ls_scale          4.409(6)
_oxford_reflns_number_all        7047
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om400311w_si_002.cif
_cod_data_source_block           COMPOUND_30
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.3.1 from
2005-06-27.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.3.1 from 2005-06-27.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     '    -P 2ybc'
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C32 H43 F3 N4 O1 Si2 Ti1'
_cod_database_code               4080892