[Disulfanediylbis(ferrocenylthiophosphinato)-κ^2^<i>O</i>,<i>O</i>]titanocene tetrahydrofuran trisolvate
Karakus, Mehmet; Woollins, J. Derek; Lönnecke, Peter; Hey-Hawkins, Evamarie; Acta Crystallographica Section E 68 (2012) m428–; doi:10.1107/S1600536812010811

data_2234271
_publ_section_title
;
 [Disulfanediylbis(ferrocenylthiophosphinato)-\k^2^<i>O</i>,<i>O</i>]titanocene
 tetrahydrofuran trisolvate
;
_journal_coeditor_code           IM2362
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m428
_journal_paper_doi               10.1107/S1600536812010811
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Fe2 Ti1 (C5 H5)4 (C10 H8 O2 P2 S4)], 3C4 H8 O'
_chemical_formula_moiety         'C30 H28 Fe2 O2 P2 S4 Ti, 3(C4 H8 O)'
_chemical_formula_sum            'C42 H52 Fe2 O5 P2 S4 Ti'
_chemical_formula_weight         986.62
_chemical_name_systematic
;
[Disulfanediylbis(ferrocenylthiophosphinato)-
\k^2^<i>O</i>,<i>O</i>]titanocene tetrahydrofuran trisolvate
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9784(3)
_cell_length_b                   30.6984(8)
_cell_length_c                   8.7072(2)
_cell_measurement_reflns_used    16673
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.9472
_cell_measurement_theta_min      2.8662
_cell_volume                     4270.98(17)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Sapphire3 Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            48502
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    1.168
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.94414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flattened needle'
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.653
_refine_ls_abs_structure_details 'Flack (1983), 3819 Friedel pairs'
_refine_ls_abs_structure_Flack   0.122(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8729
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                7146
_reflns_number_total             8729
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            im2362.cif
_cod_data_source_block           I
_cod_database_code               2234271
_cod_database_fobs_code          2234271