Two 18ē Ti^IV^ η^5^-Cp-tris(<i>sec</i>-amido)-type complexes derived from 1<i>H</i>-imidazol-2-yl side-chain functionalized cyclopentadienes
Wang, Xiaowu; Nie, Wanli; Ge, Fang; Borzov, Maxim V.; Acta Crystallographica Section C 65 (2009) m255–m259; doi:10.1107/S010827010902112X

data_2017162
_publ_section_title
;
 Two 18\=e Ti^IV^ \h^5^-Cp-tris(<i>sec</i>-amido)-type complexes
 derived from 1<i>H</i>-imidazol-2-yl side-chain functionalized
 cyclopentadienes
;
_journal_coeditor_code           BG3099
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m255
_journal_page_last               m259
_journal_paper_doi               10.1107/S010827010902112X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ti (C4 H10 N)2 (C15 H12 N2)]'
_chemical_formula_moiety         'C23 H32 N4 Ti'
_chemical_formula_sum            'C23 H32 N4 Ti'
_chemical_formula_weight         412.43
_chemical_name_systematic
;(<i>SR</i>)-{2-[(\h^5^-cyclopentadienyl)(phenyl)methyl]-1<i>H</i>-
imidazolyl-\k<i>N</i>}bis(<i>N</i>,<i>N</i>-diethylamido-
\k<i>N</i>)titanium(IV)
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.362(2)
_cell_angle_beta                 76.965(2)
_cell_angle_gamma                72.161(2)
_cell_formula_units_Z            4
_cell_length_a                   9.7472(15)
_cell_length_b                   14.469(2)
_cell_length_c                   18.006(3)
_cell_measurement_reflns_used    3373
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.028
_cell_measurement_theta_min      2.327
_cell_volume                     2350.4(6)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
;
SHELXL97 (Sheldrick, 2008), OLEX2 (Dolomanov <i>et al.</i>,
2009)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), OLEX2 (Dolomanov <i>et al.</i>,
2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0514
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11818
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.9385
_exptl_absorpt_correction_T_min  0.8634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick,1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.272
_refine_ls_extinction_coef       0.0036(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8157
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1157
_reflns_number_gt                5573
_reflns_number_total             8157
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg3099.cif
_cod_data_source_block           II
_cod_database_code               2017162
_cod_database_fobs_code          2017162