Hydrogenation of titanocene and zirconocene bis(trimethylsilyl)acetylene complexes.
Pinkas, Jiří; Gyepes, Róbert; Císařová, Ivana; Kubišta, Jiří; Horáček, Michal; Žilková, NaděŽda; Mach, Karel; Dalton transactions (Cambridge, England : 2003) 47 (2018) 8921–8932; doi:10.1039/c8dt01909f

data_7046576
_publ_section_title
;
 Hydrogenation of titanocene and zirconocene bis(trimethylsilyl)acetylene
 complexes.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8921
_journal_page_last               8932
_journal_paper_doi               10.1039/c8dt01909f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C22 H33 Ti'
_chemical_formula_sum            'C22 H33 Ti'
_chemical_formula_weight         345.38
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-03-11 deposited with the CCDC.
2018-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   15.558(3)
_cell_length_b                   15.558(3)
_cell_length_c                   31.543(7)
_cell_measurement_reflns_used    1596
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.6072
_cell_measurement_theta_min      2.6184
_cell_volume                     7635(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type
'Nonius KappaCCD equipped with Bruker APEXII 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  0.0855
_diffrn_reflns_av_sigmaI/netI    0.1228
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            16673
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.447
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'fragment in grease'
_exptl_crystal_F_000             2992
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.55(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         8956
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.0713
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+7.0904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                5567
_reflns_number_total             8956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8dt01909f2.cif
_cod_data_source_block           tbutimehbuta
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 

 Adding full bibliography for 7046575--7046576.cif.
;
_cod_original_sg_symbol_Hall     'P 4cw'
_cod_database_code               7046576