Synthesis and Reactions of a Cyclopentadienyl-Amidinate Titaniumtert-Butoxyimido Compound
Groom, Laura R.; Schwarz, Andrew D.; Nova, Ainara; Clot, Eric; Mountford, Philip; Organometallics 32 (2013) 7520–; doi:10.1021/om401008a

data_4082196
_publ_section_title
;
 Synthesis and Reactions of a Cyclopentadienyl-Amidinate
 Titaniumtert-Butoxyimido Compound
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7520
_journal_paper_doi               10.1021/om401008a
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H19 N1 O1'
_chemical_formula_sum            'C17 H19 N O'
_chemical_formula_weight         253.34
_chemical_name_systematic
;
PhC(NOtBu)Ph
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_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            4
_cell_length_a                   8.46178(11)
_cell_length_b                   10.87960(15)
_cell_length_c                   15.6091(2)
_cell_measurement_reflns_used    8409
_cell_measurement_temperature    150
_cell_measurement_theta_max      77
_cell_measurement_theta_min      4
_cell_volume                     1436.99(3)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13595
_diffrn_reflns_theta_full        76.760
_diffrn_reflns_theta_max         76.760
_diffrn_reflns_theta_min         4.955
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.16
_refine_diff_density_min         -0.25
_refine_ls_abs_structure_details 'Flack (1983), 1264 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.16(16)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9227
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2865
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.0006012
_refine_ls_shift/su_mean         0.0000599
_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: 
 43.4 -29.0 55.1 -10.6 14.3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0329
_refine_ls_wR_factor_gt          0.0323
_refine_ls_wR_factor_ref         0.0322
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                2898
_reflns_number_total             3008
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.28
_oxford_diffrn_Wilson_scale      0.01
_oxford_refine_ls_r_factor_ref   0.0298
_oxford_refine_ls_scale          10.779(17)
_oxford_reflns_number_all        2996
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            om401008a_si_002.cif
_cod_data_source_block           compound_25c
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C17 H19 N1 O1'
_cod_database_code               4082196