Crystal structure of (η 5-pentamethylcyclopentadienyl)titanium(III)dichloride (THF), C14H23Cl2OTi
Oswald, Tim; Schmidtmann, Marc; Beckhaus, Ruediger; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 637–639; doi:10.1515/ncrs-2015-0221

data_8106962
_publ_section_title
;
 Crystal structure of (\h
 5-pentamethylcyclopentadienyl)titanium(III)dichloride (THF), C14H23Cl2OTi
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              637
_journal_page_last               639
_journal_paper_doi               10.1515/ncrs-2015-0221
_journal_volume                  231
_journal_year                    2016
_chemical_formula_structural     TiCl2(C10H15)(C4H8O)
_chemical_formula_sum            'C14 H23 Cl2 O Ti'
_chemical_formula_weight         326.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.2452(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3163(7)
_cell_length_b                   9.0436(5)
_cell_length_c                   15.0774(8)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.75
_cell_measurement_theta_min      2.65
_cell_volume                     1634.70(16)
_computing_cell_refinement       'Bruker SAINT V8.34A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0111
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            75844
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.034
_diffrn_reflns_theta_min         1.699
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1142
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4111
_reflns_number_total             4787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2015-0221_suppl.cif
_cod_data_source_block           to142
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               8106962
_shelx_estimated_absorpt_t_min   0.850
_shelx_estimated_absorpt_t_max   0.878