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_2017161
_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 (C12 H14 N2)]'
_chemical_formula_moiety         'C20 H34 N4 Ti'
_chemical_formula_sum            'C20 H34 N4 Ti'
_chemical_formula_weight         378.41
_chemical_name_systematic
;{2-[2-(\h^5^-cyclopentadienyl)-2-methylpropyl]-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           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.749(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.729(3)
_cell_length_b                   14.829(3)
_cell_length_c                   10.679(2)
_cell_measurement_reflns_used    4438
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.119
_cell_measurement_theta_min      2.352
_cell_volume                     2171.6(8)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11087
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  0.9457
_exptl_absorpt_correction_T_min  0.8684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4213
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.1364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                3287
_reflns_number_total             4213
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg3099.cif
_cod_data_source_block           I
_cod_original_cell_volume        2171.7(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2017161
_cod_database_fobs_code          2017161