(<i>R</i>)-2-[(Dimethylamino)methyl]-1,1'-bis(diphenylphosphinothioyl)ferrocene dichloromethane monsolvate
Philippe, Elisabeth; Manoury, Eric; Daran, Jean-Claude; Acta Crystallographica Section E 68 (2012) m799–m800; doi:10.1107/S1600536812022301

data_2235091
_publ_section_title
;
 (<i>R</i>)-2-[(Dimethylamino)methyl]-1,1'-bis(diphenylphosphinothioyl)ferrocene
 dichloromethane monsolvate
;
_journal_coeditor_code           IM2377
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m799
_journal_page_last               m800
_journal_paper_doi               10.1107/S1600536812022301
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Fe (C20 H21 N P S) (C17 H14 P S)] , C H2 Cl2'
_chemical_formula_moiety         'C37 H35 Fe N P2 S2 , C H2 Cl2'
_chemical_formula_sum            'C38 H37 Cl2 Fe N P2 S2'
_chemical_formula_weight         760.50
_chemical_name_systematic
;
(<i>R</i>)-2-[(Dimethylamino)methyl]-1,1'-bis(diphenylphosphinothioyl)ferrocene
dichloromethane monosolvate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9493(3)
_cell_length_b                   16.8206(7)
_cell_length_c                   23.7697(9)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      26.61
_cell_measurement_theta_min      2.43
_cell_volume                     3578.1(2)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\w and \f 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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            61147
_diffrn_reflns_theta_full        27.06
_diffrn_reflns_theta_max         27.06
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Some residual electron density were difficult to modelize and therefore, the
SQUEEZE function of PLATON (Spek, 2003) was used to eliminate the contribution
of the electron density in the solvent region from the intensity data, and the
solvent-free model was employed for the final refinement. There are two
cavities of 246 \%A^3^ per unitl cell. PLATON estimated that each cavity
contains 82 electrons which may correspond to two solvent molecules of
dichloromethane as suggested by chemical analyses.
;
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.357
_refine_ls_abs_structure_details 'Flack (1983), 3441 Friedel pairs'
_refine_ls_abs_structure_Flack   0.043(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         7854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0472P)^2^+2.2997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                7097
_reflns_number_total             7854
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            im2377.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking atoms 'CT1', 'CT2' and 'CT3' as dummy atoms.

 Antanas Vaitkus,
 2017-02-20
;
_cod_database_code               2235091
_cod_database_fobs_code          2235091