Triarylphosphine Ligands with Pendant Electron-Rich "[Fe(κ2-dppe)(η5-C5Me5)(C\τbC)]-" Substituents
Ayham Tohmé; Guillaume Grelaud; Gilles Argouarch; Thierry Roisnel; Arnaud Bondon; Frédéric Paul; Inorganic Chemistry 52 (2013) 8993–9004; doi:10.1021/ic4011828

data_4335625
_publ_contact_author             'ROISNEL, Thierry'
_publ_contact_author_email       thierry.roisnel@univ-rennes1.fr
_publ_section_title
;
 Triarylphosphine Ligands with Pendant Electron-Rich
 "[Fe(\k2-dppe)(\h5-C5Me5)(C\\tbC)]-" Substituents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8993
_journal_page_last               9004
_journal_paper_doi               10.1021/ic4011828
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C56 H53 Fe P3, F6 P'
_chemical_formula_sum            'C56 H53 F6 Fe P4'
_chemical_formula_weight         1019.71
_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
_cell_angle_alpha                90
_cell_angle_beta                 93.027(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3940(6)
_cell_length_b                   11.9823(6)
_cell_length_c                   16.4380(9)
_cell_measurement_reflns_used    6824
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.31
_cell_measurement_theta_min      2.37
_cell_measurement_wavelength     0.71073
_cell_volume                     2437.8(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0386
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19502
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.4
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.790
_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    1.389
_exptl_crystal_description       prism
_exptl_crystal_F_000             1058
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.47
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.010(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         10348
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+1.0295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                9370
_reflns_number_total             10348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4011828_si_002_4.cif
_cod_data_source_block           2[PF6]
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4335625