Synthesis of a titanium ethylene complex via C-H-activation and alternative access to Cp<sub>2</sub>Ti(η<sup>2</sup>-Me<sub>3</sub>SiC<sub>2</sub>SiMe<sub>3</sub>).
Fischer, Malte; Vincent-Heldt, Lisa; Hillje, Malena; Schmidtmann, Marc; Beckhaus, Ruediger; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2068–2072; doi:10.1039/d0dt00237b

data_7703408
_publ_section_title
;
 Synthesis of a titanium ethylene complex via C-H-activation and
 alternative access to
 Cp<sub>2</sub>Ti(\h<sup>2</sup>-Me<sub>3</sub>SiC<sub>2</sub>SiMe<sub>3</sub>).
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2068
_journal_page_last               2072
_journal_paper_doi               10.1039/d0dt00237b
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_structural     Ti(C10H15)(C15H19)(C2(Si(CH3)3)2)
_chemical_formula_sum            'C33 H52 Si2 Ti'
_chemical_formula_weight         552.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-11-27 deposited with the CCDC.	2020-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3854(3)
_cell_length_b                   12.8121(3)
_cell_length_c                   21.3362(5)
_cell_measurement_reflns_used    9542
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.29
_cell_measurement_theta_min      2.39
_cell_volume                     3112.33(13)
_computing_cell_refinement       'Bruker SAINT V8.37A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.37A'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(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  0.0271
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            188971
_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         36.316
_diffrn_reflns_theta_min         1.854
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.9261
_exptl_absorpt_correction_T_min  0.8596
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 6575 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0069(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         15106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0193
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0550
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                14681
_reflns_number_total             15106
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00237b2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7703407--7703408.cif.'
_cod_database_code               7703408
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.836
_shelx_estimated_absorpt_t_max   0.897
_exptl_absorpt_special_details
;
 numerical absorption correction followed by correction based on
 symmetry-related measurements (multi-scan)
;
_shelx_res_checksum              73222