Investigation on the Protonation of a Trisubstituted [Fe2(CO)3(PPh3)(κ2-phen)(μ-pdt)] Complex: Rotated versus Unrotated Intermediate Pathways
Pierre-Yves Orain; Jean-François Capon; Frédéric Gloaguen; François Y. Pétillon; Philippe Schollhammer; Jean Talarmin; Giuseppe Zampella; Luca De Gioia; Thierry Roisnel; Inorganic Chemistry 49 (2010) 5003–5008; doi:10.1021/ic100108h

data_4315594
_publ_section_title
;
 Investigation on the Protonation of a Trisubstituted
 [Fe2(CO)3(PPh3)(\k2-phen)(\m-pdt)] Complex: Rotated versus Unrotated
 Intermediate Pathways
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5003
_journal_page_last               5008
_journal_paper_doi               10.1021/ic100108h
_journal_volume                  49
_journal_year                    2010
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'C19 H15 Fe2 N2 O4 S2, B F3 H2 O, C H2 Cl2, B F4'
_chemical_formula_sum            'C20 H19 B2 Cl2 F7 Fe2 N2 O5 S2'
_chemical_formula_weight         768.71
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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             2009-10-16T14:15:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                88.214(3)
_cell_angle_beta                 64.190(3)
_cell_angle_gamma                81.344(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3463(7)
_cell_length_b                   11.4918(7)
_cell_length_c                   12.4419(8)
_cell_measurement_reflns_used    9326
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.51
_cell_measurement_wavelength     0.71073
_cell_volume                     1442.75(16)
_computing_cell_refinement       'Bruker SMART, 2006'
_computing_data_collection       'Bruker SMART, 2006'
_computing_data_reduction        'Bruker SAINT, 2006'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24721
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    1.416
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.77
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         6559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0372P)^2^+1.2164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                5158
_reflns_number_total             6559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100108h_si_002.cif
_cod_data_source_block           job
_cod_database_code               4315594