Reactivity of [Fe2(CO)6(μ-S2)] toward a Base-Containing Diphosphine (Ph2PCH2)2NCH3: Formation of Diiron Carbonyl Compounds Having Polydentate Heterofunctionalized Phosphine (PNS = Ph2PCH2N(CH3)CH2S) and Bidentate Thiophosphinito (Ph2PS = PS) Bridges
Lounissi, Sondès; Capon, Jean-François; Gloaguen, Frédéric; Matoussi, Fatma; Pétillon, François Y.; Schollhammer, Philippe; Talarmin, Jean; Organometallics 29 (2010) 1296–; doi:10.1021/om9011054

data_4067739
_publ_section_title
;
 Reactivity of [Fe2(CO)6(\m-S2)] toward a Base-Containing Diphosphine
 (Ph2PCH2)2NCH3: Formation of Diiron Carbonyl Compounds Having Polydentate
 Heterofunctionalized Phosphine (PNS = Ph2PCH2N(CH3)CH2S) and Bidentate
 Thiophosphinito (Ph2PS = PS) Bridges
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1296
_journal_paper_doi               10.1021/om9011054
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety
;
        C30 H24 Fe2 N2 O4 P S2, C12 H26
;
_chemical_formula_sum            'C42 H50 Fe2 N2 O4 P2 S2'
_chemical_formula_weight         884.6
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2009-11-06T16:33:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 106.165(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.1289(10)
_cell_length_b                   9.3337(4)
_cell_length_c                   25.7957(13)
_cell_measurement_reflns_used    5007
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      24.26
_cell_measurement_theta_min      2.36
_cell_volume                     4423.6(4)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1980-2002)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'XCALIBUR-2 with SAPPHIRE-2 detector'
_diffrn_measurement_method
;
4 stepped omega-scans over 115 deg. with kappa -79 deg. (chi -58.3 deg.),
        phi 0, 90, 180, 270 deg.
        step 1 deg., exposure time 150 s
        detector distance 50 mm
        detector angle 30 deg.
;
_diffrn_orient_matrix_UB_11      -0.0183919362
_diffrn_orient_matrix_UB_12      0.0050855078
_diffrn_orient_matrix_UB_13      0.0202846056
_diffrn_orient_matrix_UB_21      0.0324630612
_diffrn_orient_matrix_UB_22      -0.0191499849
_diffrn_orient_matrix_UB_23      0.0198249612
_diffrn_orient_matrix_UB_31      0.0097817743
_diffrn_orient_matrix_UB_32      0.0732806352
_diffrn_orient_matrix_UB_33      0.0037704934
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1154
_diffrn_reflns_av_unetI/netI     0.1531
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            28904
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.45
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.9581
_exptl_absorpt_correction_T_min  0.9028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
        (compiled May  8 2007,13:10:02)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
        rectangular plate, main faces {1 0 1}, long axis [0 1 0],
        unstable in open air at room temperature
;
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7526
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0398P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                3792
_reflns_number_total             7526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9011054_si_002.cif
_cod_data_source_block           sl74-d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'const' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4067739