Decamethyltitanocene hydride intermediates in hydrogenation of corresponding titanocene-(η2-ethene) or (η2-alkyne) complexes and effects of bulkier auxiliary ligands
Pinkas, Jiri; Gyepes, Robert; Cisarova, Ivana; Kubišta, Jiří; Horacek, Michal; Mach, Karel; Dalton Trans.  (2017) –; doi:10.1039/C7DT01545C

data_7043158
_publ_section_title
;
 Decamethyltitanocene hydride intermediates in hydrogenation of
 corresponding titanocene-(\h2-ethene) or (\h2-alkyne) complexes and
 effects of bulkier auxiliary ligands
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01545C
_journal_year                    2017
_chemical_formula_moiety         'C28 H49 Si2 Ti'
_chemical_formula_sum            'C28 H49 Si2 Ti'
_chemical_formula_weight         489.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-04-25 deposited with the CCDC.
2017-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.825(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9701(6)
_cell_length_b                   14.6030(7)
_cell_length_c                   15.4311(7)
_cell_measurement_reflns_used    127
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.1504
_cell_measurement_theta_min      1.8676
_cell_volume                     2849.8(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Nonius with APEX II detector'
_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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20593
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.8045
_exptl_absorpt_correction_T_min  0.7449
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.787
_exptl_crystal_size_mid          0.656
_exptl_crystal_size_min          0.572
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0555P)^2^+0.5259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                4710
_reflns_number_total             6446
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01545c8.cif
_cod_data_source_block           tmstime140hbutab
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7043158