Triphenylamine Derivatives with Para-Disposed Pendant Electron-Rich Organoiron Alkynyl Substituents: Defining the Magnetic Interactions in a Trinuclear Iron(III) Trication
Grelaud, Guillaume; Cador, Olivier; Roisnel, Thierry; Argouarch, Gilles; Cifuentes, Marie P.; Humphrey, Mark G.; Paul, Frédéric; Organometallics 31 (2012) 1635–; doi:10.1021/om2006358

data_4076307
_publ_section_title
;
 Triphenylamine Derivatives with Para-Disposed Pendant Electron-Rich
 Organoiron Alkynyl Substituents: Defining the Magnetic Interactions in a
 Trinuclear Iron(III) Trication
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1635
_journal_paper_doi               10.1021/om2006358
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C56 H53 Fe N P2'
_chemical_formula_sum            'C56 H53 Fe N P2'
_chemical_formula_weight         857.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 104.140(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7646(4)
_cell_length_b                   32.2519(8)
_cell_length_c                   13.6095(5)
_cell_measurement_reflns_used    95551
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     4581.8(3)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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 Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.943282E-1
_diffrn_orient_matrix_UB_12      -0.52701E-2
_diffrn_orient_matrix_UB_13      0.21727E-1
_diffrn_orient_matrix_UB_21      0.99405E-2
_diffrn_orient_matrix_UB_22      0.104525E-1
_diffrn_orient_matrix_UB_23      -0.668691E-1
_diffrn_orient_matrix_UB_31      0.136896E-1
_diffrn_orient_matrix_UB_32      0.28724E-1
_diffrn_orient_matrix_UB_33      0.283196E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39491
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.52
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         10384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.133
_reflns_number_gt                6667
_reflns_number_total             10384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2006358_si_001.cif
_cod_data_source_block           GG51
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4076307