New Titanium Complexes with Symmetric or Asymmetric cis-9,10-Dihydrophenanthrenediamide Ligands Formed through Sequential Intramolecular C-C Bond-Forming Reactions
Dapeng Zhao; Bo Gao; Wei Gao; Xuyang Luo; Duihai Tang; Ying Mu; Ling Ye; Inorganic Chemistry 50 (2011) 30–36; doi:10.1021/ic1008768

data_4324077
_publ_section_title
;
 New Titanium Complexes with Symmetric or Asymmetric
 cis-9,10-Dihydrophenanthrenediamide Ligands Formed through Sequential
 Intramolecular C-C Bond-Forming Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              30
_journal_page_last               36
_journal_paper_doi               10.1021/ic1008768
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C40 H50 N2 O2 Ti'
_chemical_formula_weight         638.72
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 98.0210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.1690(8)
_cell_length_b                   21.0622(10)
_cell_length_c                   20.0823(10)
_cell_measurement_temperature    185(2)
_cell_volume                     7191.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39987
_diffrn_reflns_theta_full        26.07
_diffrn_reflns_theta_max         26.07
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  0.9680
_exptl_absorpt_correction_T_min  0.9602
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         14163
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0762P)^2^+0.3863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1470
_reflns_number_gt                9392
_reflns_number_total             14163
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1008768_si_001_3.cif
_cod_data_source_block           2e
_cod_database_code               4324077