Coordination Chemistry of N-Alkylbenzamide-2,3-dithiolates as an Approach to Poly(dithiolate) Ligands: 1,4-Bis[(2,3-dimercaptobenzamido)methyl]benzene and Its Chelate Complex with the (C5H5)Ti Fragment
Wolfram W. Seidel; F. Ekkehardt Hahn; Thomas Lügger; Inorganic Chemistry 37 (1998) 6587–6596; doi:10.1021/ic9706616

data_4323220
_publ_contact_author
;
        F. Ekkehardt Hahn
        Institut f\"ur Analytische und Anorganische Chemie
        Freie Universit\"at Berlin
        Fabeckstr. 34 - 36
        14195 Berlin
        Bundesrepublik Deutschland
;
_publ_contact_author_phone       '049 30 838 4002'
_publ_section_title
;
 Coordination Chemistry of N-Alkylbenzamide-2,3-dithiolates as an Approach
 to Poly(dithiolate) Ligands:
 1,4-Bis[(2,3-dimercaptobenzamido)methyl]benzene and Its Chelate Complex
 with the (C5H5)Ti Fragment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6587
_journal_page_last               6596
_journal_paper_doi               10.1021/ic9706616
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C18 H18 O2 S2 Ti'
_chemical_formula_weight         378.35
_chemical_name_systematic
; 
[1,4-Di(hydroxymethyl)benzene-2,3-dithiolato]bis(cyclopentadienyl) 
titanium(IV)
;
_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                96.42(1)
_cell_angle_beta                 101.74(1)
_cell_angle_gamma                108.82(1)
_cell_formula_units_Z            6
_cell_length_a                   10.1778(11)
_cell_length_b                   11.5806(14)
_cell_length_c                   22.967(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      5
_cell_volume                     2462.3(6)
_computing_cell_refinement       'CAD4, Enraf Nonius'
_computing_data_collection       'CAD4, Enraf Nonius'
_computing_data_reduction        'MolEN, Enraf Nonius'
_computing_molecular_graphics    'Zortep, Zsolnai, Pritzkow 1994'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD 4'
_diffrn_measurement_method       'omega 2-theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6424
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       needles
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.312
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.082
_refine_ls_goodness_of_fit_obs   1.122
_refine_ls_hydrogen_treatment    gliding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         6411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_restrained_S_obs      1.122
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_obs          0.0479
_refine_ls_shift/esd_max         14.998
_refine_ls_shift/esd_mean        0.118
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+3.8959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1451
_refine_ls_wR_factor_obs         0.1327
_reflns_number_observed          5426
_reflns_number_total             6419
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9706616_1.cif
_cod_data_source_block           compound_16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+3.8959P] 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^)+(0.0807P)^2^+3.8959P] 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        2462.3(5)
_cod_database_code               4323220