Conformational Control of Metallocene Backbone by Cyclopentadienyl Ring Substitution: A New Concept in Polyphosphane Ligands Evidenced by “Through-Space” Nuclear Spin−Spin Coupling. Application in Heteroaromatics Arylation by Direct C−H Activation
Smaliy, Radomyr V.; Beaupérin, Matthieu; Cattey, Hélène; Meunier, Philippe; Hierso, Jean-Cyrille; Roger, Julien; Doucet, Henri; Coppel, Yannick; Organometallics 28 (2009) 3152–; doi:10.1021/om8012162

data_4069048
_publ_section_title
;
 Conformational Control of Metallocene Backbone by Cyclopentadienyl Ring
 Substitution: A New Concept in Polyphosphane Ligands Evidenced by
 &#x201C;Through-Space&#x201D; Nuclear Spin&#x2212;Spin Coupling.
 Application in Heteroaromatics Arylation by Direct C&#x2212;H Activation
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3152
_journal_paper_doi               10.1021/om8012162
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C54 H53 Fe P3'
_chemical_formula_sum            'C54 H53 Fe P3'
_chemical_formula_weight         850.72
_chemical_name_systematic
;
 ?
;
_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_creation_method           SHELXL-97
_cell_angle_alpha                81.2257(8)
_cell_angle_beta                 68.2423(10)
_cell_angle_gamma                64.6175(13)
_cell_formula_units_Z            2
_cell_length_a                   12.9826(2)
_cell_length_b                   13.6178(3)
_cell_length_c                   15.4017(5)
_cell_measurement_reflns_used    26306
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2284.76(10)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17940
_diffrn_reflns_theta_full        27.37
_diffrn_reflns_theta_max         27.37
_diffrn_reflns_theta_min         1.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.247
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         10270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+1.7278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1226
_reflns_number_gt                7135
_reflns_number_total             10270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8012162_si_002.cif
_cod_data_source_block           jc13
_cod_database_code               4069048