Reactions of a Cyclopentadienyl–Amidinate Titanium Benzimidamido Complex
Groom, Laura R.; Russell, Adam F.; Schwarz, Andrew D.; Mountford, Philip; Organometallics 33 (2014) 1002–; doi:10.1021/om4011752

data_4082402
_publ_section_title
;
 Reactions of a Cyclopentadienyl--Amidinate Titanium Benzimidamido Complex
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1002
_journal_paper_doi               10.1021/om4011752
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C20 H20 F5 N3 O1'
_chemical_formula_sum            'C20 H20 F5 N3 O'
_chemical_formula_weight         413.39
_chemical_name_systematic
;
Me2NPhC(NC(C6F5)NOtBu)H
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 92.337(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.1540(4)
_cell_length_b                   7.9437(9)
_cell_length_c                   14.4166(7)
_cell_measurement_reflns_used    7902
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     4022.5(5)
_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 0.992
_diffrn_measured_fraction_theta_max 0.990
_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  0.087
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13942
_diffrn_reflns_theta_full        26.590
_diffrn_reflns_theta_max         27.132
_diffrn_reflns_theta_min         5.133
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.22
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0550
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         1948
_refine_ls_number_restraints     95
_refine_ls_R_factor_all          0.1511
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.0003304
_refine_ls_shift/su_mean         0.0000178
_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: 
 -0.223 -0.736 -0.491 -0.264 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0952
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0425
_reflns_limit_h_max              44
_reflns_limit_h_min              -44
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                1948
_reflns_number_total             4411
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.64
_oxford_diffrn_Wilson_scale      159.83
_oxford_refine_ls_r_factor_ref   0.0614
_oxford_refine_ls_scale          0.0975(3)
_oxford_reflns_number_all        4411
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            om4011752_si_002.cif
_cod_data_source_block           compound_14e
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C20 H20 F5 N3 O1'
_cod_database_code               4082402