New Half-Sandwich Alkyl, Aryl, Aryloxide, and Propargyloxide Titanium(IV) Complexes Containing a Cyclopentadienyl Ligand with a Pendant Ether Substituent: Behavior and Influence in the Hydroamination of Alkynes of the Ether Group
Esteruelas, Miguel A.; López, Ana M.; Mateo, A. Concepción; Oñate, Enrique; Organometallics 25 (2006) 1448–1460; doi:10.1021/om051031b

data_4074943
_publ_section_title
;
 New Half-Sandwich Alkyl, Aryl, Aryloxide, and Propargyloxide Titanium(IV)
 Complexes Containing a Cyclopentadienyl Ligand with a Pendant Ether
 Substituent: Behavior and Influence in the Hydroamination of
 Alkynes of the Ether Group
;
_journal_coden_ASTM              ORGND7
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1448
_journal_page_last               1460
_journal_paper_doi               10.1021/om051031b
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C23 H34 Cl2 O2 Ti'
_chemical_formula_weight         461.30
_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                 100.225(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.191(4)
_cell_length_b                   10.3853(17)
_cell_length_c                   11.541(2)
_cell_measurement_reflns_used    820
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      2
_cell_volume                     2381.6(7)
_computing_cell_refinement       'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_computing_data_collection       'SMART v. 5.625 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.02 (Bruker AXS, 1999)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0833
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20777
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.79
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         5770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                3636
_reflns_number_total             5770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om051031bsi20060118_072729.cif
_cod_data_source_block           mae36bs
_cod_original_cell_volume        2381.6(8)
_cod_database_code               4074943