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_1512959
_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 O3.41 S0.59 Zr'
_chemical_formula_weight         396.05
_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                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   11.948(5)
_cell_length_b                   8.280(5)
_cell_length_c                   7.847(5)
_cell_measurement_temperature    293(2)
_cell_volume                     776.3(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.773
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            2190
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.28
_diffrn_reflns_theta_min         3.41
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66945
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red-orange
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             396
_exptl_crystal_recrystallization_method
'Chloroform and Petroleum ether (60-80)'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.53(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1148
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+0.2064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                880
_reflns_number_total             1148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-395-230-236-4.cif
_cod_data_source_block           cp2zrpdtc
_cod_database_code               1512959