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_4080887
_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         'C47 H46 F5 N7 O1 Si2 Ti1'
_chemical_formula_sum            'C47 H46 F5 N7 O Si2 Ti'
_chemical_formula_weight         923.99
_chemical_name_systematic
;
 Ti(N2ArO)(NC(ArF)NNPh2)(py)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                73.5239(5)
_cell_angle_beta                 86.8122(5)
_cell_angle_gamma                65.5205(5)
_cell_formula_units_Z            2
_cell_length_a                   12.1879(2)
_cell_length_b                   12.46310(10)
_cell_length_c                   18.7917(3)
_cell_measurement_reflns_used    10188
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2484.90(6)
_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 0.989
_diffrn_measured_fraction_theta_max 0.984
_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  0.027
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62187
_diffrn_reflns_theta_full        25.029
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         5.095
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.280
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.87
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0426
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         7556
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.0059391
_refine_ls_shift/su_mean         6.1787796
_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: 
 1.81 1.41 1.25 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0990
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0737
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                8309
_reflns_number_total             11232
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.93
_oxford_diffrn_Wilson_scale      3.39
_oxford_refine_ls_r_factor_ref   0.0670
_oxford_refine_ls_scale          0.5653(12)
_oxford_reflns_number_all        11232
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om400311w_si_002.cif
_cod_data_source_block           COMPOUND_22
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        2484.91(6)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C47 H46 F5 N7 O1 Si2 Ti1'
_cod_database_code               4080887