M−Cl/Si−Cl Preferential Reactivity in Chlorosilyl-Substituted Cyclopentadienyl Early Transition Metal Complexes in Reactions with Amines: Key to Understanding the Nature of the Final Product
Paniagua, Cristina; Mosquera, Marta E. G.; Jacobsen, Heiko; Jiménez, Gerardo; Cuenca, Tomás; Organometallics 28 (2009) 6975–; doi:10.1021/om9008026

data_4070437
_publ_section_title
;
 M&#x2212;Cl/Si&#x2212;Cl Preferential Reactivity in
 Chlorosilyl-Substituted Cyclopentadienyl Early Transition Metal Complexes
 in Reactions with Amines: Key to Understanding the Nature of the Final
 Product
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6975
_journal_paper_doi               10.1021/om9008026
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C15 H28 Cl2 N2 Si1 Ti1'
_chemical_formula_sum            'C15 H28 Cl2 N2 Si Ti'
_chemical_formula_weight         383.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.644(2)
_cell_length_b                   13.3646(3)
_cell_length_c                   14.971(2)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20.360
_cell_measurement_theta_min      3.562
_cell_volume                     1929.6(5)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0701
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16052
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(5)
_refine_ls_extinction_coef       0.0151(17)
_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   1.149
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0237P)^2^+3.5772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                3566
_reflns_number_total             4419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9008026_si_001.cif
_cod_data_source_block           3
_cod_database_code               4070437