Synthesis and characterisation of derivatives of monocyclopentadienylbis(arene-1,2-dithiolato)titanium(IV); crystal structures of M[Ti(η5-C5Me5)(1,2-S2C6H4)2] [M = Tl or N(PPh3)2]
Spence, Malcolm A.; Rosair, Georgina M.; Lindsell, W. Edward; Journal of the Chemical Society, Dalton Transactions  (1998) 1581–; doi:10.1039/a800890f

data_7028077
_publ_section_title
;
 Synthesis and characterisation of derivatives of
 monocyclopentadienylbis(arene-1,2-dithiolato)titanium(IV); crystal
 structures of M[Ti(\h5-C5Me5)(1,2-S2C6H4)2] [M&#x2005;=&#x2005;Tl or
 N(PPh3)2]
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1581
_journal_paper_doi               10.1039/a800890f
_journal_year                    1998
_chemical_formula_sum            'C61 H59 Cl6 N P2 S4 Ti'
_chemical_formula_weight         1256.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                89.08(2)
_cell_angle_beta                 88.04(2)
_cell_angle_gamma                89.859(14)
_cell_formula_units_Z            2
_cell_length_a                   11.473(3)
_cell_length_b                   15.545(4)
_cell_length_c                   16.778(6)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      13.16
_cell_measurement_theta_min      3.58
_cell_volume                     2990.2(15)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0681
_diffrn_reflns_av_sigmaI/netI    0.1073
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12059
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        8.5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_type   'semi-empirical via \y scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.058
_refine_ls_goodness_of_fit_obs   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         10377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_restrained_S_obs      1.123
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_obs          0.0646
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+6.0023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1893
_refine_ls_wR_factor_obs         0.1451
_reflns_number_observed          6296
_reflns_number_total             10398
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            f800890sup1.cif
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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^)+(0.0618P)^2^+6.0023P] 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^)+(0.0618P)^2^+6.0023P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7028077