Bis[η5-tetramethyl(trimethylsilyl)cyclopentadienyl]titanium(II) and Its π-Complexes with Bis(trimethylsilyl)acetylene and Ethylene
Horáček, Michal; Kupfer, Volkmar; Thewalt, Ulf; Štěpnička, Petr; Polášek, Miroslav; Mach, Karel; Organometallics 18 (1999) 3572–; doi:10.1021/om990286k

data_4077798
_publ_section_title
;
 Bis[\h5-tetramethyl(trimethylsilyl)cyclopentadienyl]titanium(II) and Its
 \p-Complexes with Bis(trimethylsilyl)acetylene and Ethylene
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              3572
_journal_paper_doi               10.1021/om990286k
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C32 H60 Si4 Ti'
_chemical_formula_weight         605.06
_chemical_name_systematic
; 
 [\h^2^-bis(trimethylsilyl)ethyne]-bis[\h^5^(1-trimethylsilyl-2,3,4,5-
 tetramethyl-cyclopentadienyl)]-titanium(II)  
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.180(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.807(2)
_cell_length_b                   18.927(2)
_cell_length_c                   21.214(2)
_cell_measurement_reflns_used    13477
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.15
_cell_volume                     7492.1(14)
_computing_cell_refinement       'CELL, STOE (1996)'
_computing_data_collection       'EXPOSE, STOE (1996)'
_computing_data_reduction        'X-RED, STOE 1996'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '0.15 mm'
_diffrn_measured_fraction_theta_full 0.482
_diffrn_measured_fraction_theta_max 0.482
_diffrn_measurement_device_type  'STOE IPDS, imaging plate system'
_diffrn_measurement_method       oscillation
_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  0.0705
_diffrn_reflns_av_sigmaI/netI    0.1398
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13477
_diffrn_reflns_theta_full        26.04
_diffrn_reflns_theta_max         26.04
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.730
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.730
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                3059
_reflns_number_total             7125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990286k.cif
_cod_data_source_block           comp1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not performed' was changed to
'?' - the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7492.1(15)
_cod_original_sg_symbol_H-M      I2/a
_cod_database_code               4077798