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_4069681
_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_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C86 H84 Fe2 P4, 2(P F6)'
_chemical_formula_sum            'C86 H84 F12 Fe2 P6'
_chemical_formula_weight         1643.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 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             2008-09-17T14:33:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.5690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3994(4)
_cell_length_b                   21.8906(8)
_cell_length_c                   16.1491(6)
_cell_measurement_reflns_used    9027
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.25
_cell_measurement_wavelength     0.71073
_cell_volume                     4369.4(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            85734
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.259(11)
_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     956
_refine_ls_number_reflns         19384
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.05
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0872P)^2^+2.1608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                17793
_reflns_number_total             19384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900352q_si_001.cif
_cod_data_source_block           new_sq
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4069681