Electronic and Magnetic Couplings in Free and π-Coordinated 1,4-Diethynylnaphthalene-Bridged [Cp*(dppe)Fe]n+(n= 0, 1) Units
Tanaka, Yuya; Shaw-Taberlet, Jennifer A.; Justaud, Frédéric; Cador, Olivier; Roisnel, Thierry; Akita, Munetaka; Hamon, Jean-René; Lapinte, Claude; Organometallics 28 (2009) 4656–; doi:10.1021/om900352q

data_4069683
_publ_section_title
;
 Electronic and Magnetic Couplings in Free and \p-Coordinated
 1,4-Diethynylnaphthalene-Bridged [Cp*(dppe)Fe]n+(n= 0, 1) Units
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4656
_journal_paper_doi               10.1021/om900352q
_journal_volume                  28
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C96 H99 Fe2 P4 Ru, P F6'
_chemical_formula_sum            'C96 H99 F6 Fe2 P5 Ru'
_chemical_formula_weight         1734.37
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2c 2n'
_symmetry_space_group_name_H-M   'P n a m'
_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             2008-09-17T16:51:11-00:00
_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                   17.49240(10)
_cell_length_b                   20.2251(2)
_cell_length_c                   26.9637(3)
_cell_measurement_reflns_used    11648
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     9539.37(15)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.144767E-1
_diffrn_orient_matrix_UB_12      -0.345552E-1
_diffrn_orient_matrix_UB_13      -0.248077E-1
_diffrn_orient_matrix_UB_21      0.31877E-2
_diffrn_orient_matrix_UB_22      -0.336092E-1
_diffrn_orient_matrix_UB_23      0.271224E-1
_diffrn_orient_matrix_UB_31      -0.552124E-1
_diffrn_orient_matrix_UB_32      -0.110008E-1
_diffrn_orient_matrix_UB_33      -0.49387E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            21005
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.306
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         11104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.085
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1004P)^2^+8.0237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1894
_reflns_number_gt                7935
_reflns_number_total             11104
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900352q_si_003.cif
_cod_data_source_block           renum
_cod_database_code               4069683