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_7043159
_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_sum            'C40 H62.5 Cl0.25 Ti2'
_chemical_formula_weight         648.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-25 deposited with the CCDC.
2017-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.247(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.9059(17)
_cell_length_b                   8.4278(3)
_cell_length_c                   22.7517(10)
_cell_measurement_reflns_used    9099
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.4316
_cell_measurement_theta_min      2.6307
_cell_volume                     7460.0(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            71286
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.473
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2806
_exptl_crystal_size_max          0.862
_exptl_crystal_size_mid          0.309
_exptl_crystal_size_min          0.232
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         8538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0494P)^2^+9.6539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7045
_reflns_number_total             8538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01545c8.cif
_cod_data_source_block           tiebh2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' 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_formula_sum        'C40 H62.50 Cl0.25 Ti2'
_cod_database_code               7043159
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.687
_shelx_estimated_absorpt_t_max   0.899
_shelx_res_checksum              74927