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_4080885
_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         'C40 H58 N6 O1 S1 Si2 Ti1, 2 (C6 H6)'
_chemical_formula_sum            'C52 H70 N6 O S Si2 Ti'
_chemical_formula_weight         931.30
_chemical_name_systematic
;
Ti (N2O)(NNPh2){N(NPh2)C(NAr)S}(py)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            16
_cell_length_a                   19.8316(2)
_cell_length_b                   22.3574(2)
_cell_length_c                   47.3876(7)
_cell_measurement_reflns_used    23171
_cell_measurement_temperature    150
_cell_measurement_theta_max      76.5318
_cell_measurement_theta_min      3.1187
_cell_volume                     21010.9(4)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.985
_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  0.069
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            104672
_diffrn_reflns_theta_full        73.662
_diffrn_reflns_theta_max         76.732
_diffrn_reflns_theta_min         3.121
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.503
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7968
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.98
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9054
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1135
_refine_ls_number_reflns         14254
_refine_ls_number_restraints     210
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0799
_refine_ls_shift/su_max          0.0011309
_refine_ls_shift/su_mean         0.0000361
_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: 
 14.7 1.75 10.0 2.93 -2.56 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0736
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0648
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              58
_reflns_limit_l_min              0
_reflns_number_gt                16011
_reflns_number_total             21805
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.08
_oxford_diffrn_Wilson_scale      2.79
_oxford_refine_ls_r_factor_ref   0.0734
_oxford_refine_ls_scale          0.6288(9)
_oxford_reflns_number_all        21805
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om400311w_si_002.cif
_cod_data_source_block           COMPOUND_20
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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_H-M      'P b c a '
_cod_original_formula_sum        'C52 H70 N6 O1 S1 Si2 Ti1'
_cod_database_code               4080885