Studies of titanocene and zirconocene pyridine-2,6-bis-thiocarboxylates exhibiting partial desulfurization
Suryabhan Singh; Subrato Bhattacharya; Inorganica Chimica Acta 395 (2013) 230–236; doi:10.1016/j.ica.2012.11.014

data_1512957
_publ_section_title
;
 Studies of titanocene and zirconocene pyridine-2,6-bis-thiocarboxylates
 exhibiting partial desulfurization
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              230
_journal_page_last               236
_journal_paper_doi               10.1016/j.ica.2012.11.014
_journal_volume                  395
_journal_year                    2013
_chemical_formula_sum            'C17 H13 N O3.5 S0.5 Ti'
_chemical_formula_weight         351.21
_space_group_IT_number           31
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      31
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.964(11)
_cell_length_b                   8.167(4)
_cell_length_c                   7.678(5)
_cell_measurement_temperature    293(2)
_cell_volume                     750.2(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.843
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2021
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03289
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             360
_exptl_crystal_recrystallization_method Chloroform
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.18(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1432
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1392
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0974P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.2326
_reflns_number_gt                674
_reflns_number_total             1432
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-395-230-236-2.cif
_cod_data_source_block           ti-pdtc1
_cod_original_formula_sum        'C17 H13 N O3.50 S0.50 Ti'
_cod_database_code               1512957