Congested Ferrocenyl Polyphosphanes Bearing Electron-Donating or Electron-Withdrawing Phosphanyl Groups: Assessment of Metallocene Conformation from NMR Spin Couplings and Use in Palladium-Catalyzed Chloroarenes Activation
Sophal Mom; Matthieu Beaupérin; David Roy; Sylviane Royer; Régine Amardeil; Hélène Cattey; Henri Doucet; Jean-Cyrille Hierso; Inorganic Chemistry 50 (2011) 11592–11603; doi:10.1021/ic2015379

data_4326883
_publ_contact_author_address
;
ICMUB UMR 5260
Universit\'e de Bourgogne
Facult\'e des Sciences
9 Avenue Alain Savary
21000 DIJON
France
;
_publ_contact_author_email       hcattey@u-bourgogne.fr
_publ_contact_author_fax         +33-0380393835
_publ_contact_author_name        'Cattey, H\'el\`ene'
_publ_contact_author_phone       +33-0380393665
_publ_section_title
;
 Congested Ferrocenyl Polyphosphanes Bearing Electron-Donating or
 Electron-Withdrawing Phosphanyl Groups: Assessment of Metallocene
 Conformation from NMR Spin Couplings and Use in Palladium-Catalyzed
 Chloroarenes Activation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11592
_journal_page_last               11603
_journal_paper_doi               10.1021/ic2015379
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C63 H63 Fe P3'
_chemical_formula_sum            'C63 H63 Fe P3'
_chemical_formula_weight         968.89
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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      2.2
_audit_creation_method           'wingx routine cif_update'
_audit_update_record
;
2009-01-09 # Formatted by publCIF
;
_cell_angle_alpha                75.3279(8)
_cell_angle_beta                 71.2575(8)
_cell_angle_gamma                88.8294(9)
_cell_formula_units_Z            2
_cell_length_a                   11.4411(2)
_cell_length_b                   14.0636(3)
_cell_length_c                   17.2603(4)
_cell_measurement_reflns_used    78090
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2538.57(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius,1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett, 1996)'
_computing_publication_material  'SHELXL97 and WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f scans (\k = 0) + additional \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19021
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         11548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+3.5957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                10077
_reflns_number_total             11548
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2015379_si_002.cif
_cod_data_source_block           1005jc26
_cod_original_cell_volume        2538.56(9)
_cod_database_code               4326883