Reactivity of functionalised decamethyltitanocenes: Synthesis and structure of chiral monocyclopentadienyl titanium halogenides
Vladimir V. Burlakov; Konstantin A. Lyssenko; Anke Spannenberg; Wolfgang Baumann; Perdita Arndt; Vladimir B. Shur; Uwe Rosenthal; Inorganica Chimica Acta 401 (2013) 76–80; doi:

data_1517015
_publ_section_title
;
 Reactivity of functionalised decamethyltitanocenes: Synthesis and
 structure of chiral monocyclopentadienyl titanium halogenides
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              76
_journal_page_last               80
_journal_volume                  401
_journal_year                    2013
_chemical_formula_moiety         'C22 H35 Cl3 Ti'
_chemical_formula_sum            'C22 H35 Cl3 Ti'
_chemical_formula_weight         453.75
_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
_cell_angle_alpha                103.627(5)
_cell_angle_beta                 97.146(5)
_cell_angle_gamma                112.576(5)
_cell_formula_units_Z            2
_cell_length_a                   9.3969(10)
_cell_length_b                   11.5366(11)
_cell_length_c                   11.951(2)
_cell_measurement_reflns_used    2021
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     1128.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector''
_diffrn_measurement_method       'omega 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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9666
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0470P)^2^+0.5026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                4081
_reflns_number_total             5378
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ICA-2013-401-76-86-2.cif
_cod_data_source_block           w
_cod_database_code               1517015