"Through-Space" Nuclear Spin-Spin JPP Coupling in Tetraphosphine Ferrocenyl Derivatives: A 31P NMR and X-ray Structure Correlation Study for Coordination Complexes
Jean-Cyrille Hierso; Aziz Fihri; Vladimir V. Ivanov; Bernard Hanquet; Nadine Pirio; Bruno Donnadieu; Bertrand Rebière; Régine Amardeil; Philippe Meunier; Journal of the American Chemical Society 126 (2004) 11077–11087; doi:10.1021/ja048907a

data_4112928
_publ_contact_author             'Dr Jean Cyrille Hierso'
_publ_contact_author_address
;
Laboratoire de Synthese et 
d'Electrosynthese Organometalliques
UMR-CNRS 5188
Universite de Bourgogne
Facultes des
Mirande 
9, Avenue Alain Savary
BP 47870 F-21078 
Dijon cedex, France
;
_publ_contact_author_email       ' jean-cyrille.hierso@u-bourgogne.fr '
_publ_section_title
;
 "Through-Space" Nuclear Spin-Spin JPP Coupling in Tetraphosphine
 Ferrocenyl Derivatives: A 31P NMR and X-ray Structure Correlation Study
 for Coordination Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11077
_journal_page_last               11087
_journal_paper_doi               10.1021/ja048907a
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C67 H64 Cl6 Fe Ni2 P4'
_chemical_formula_weight         1379.03
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.850(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3226(19)
_cell_length_b                   22.814(3)
_cell_length_c                   21.159(3)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.45
_cell_measurement_theta_min      1.75
_cell_volume                     6682.9(16)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \f
_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  0.2055
_diffrn_reflns_av_sigmaI/netI    0.2225
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26464
_diffrn_reflns_theta_full        21.73
_diffrn_reflns_theta_max         21.73
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  5
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  0.5978
_exptl_absorpt_correction_T_min  0.1277
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       prism
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.0035(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.823
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         7847
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.823
_refine_ls_R_factor_all          0.2044
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0877P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.2386
_reflns_number_gt                2328
_reflns_number_total             7847
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048907asi20040309_020107_1.cif
_cod_data_source_block           2
_cod_original_cell_volume        6682.8(15)
_cod_original_sg_symbol_H-M      ' P 1 21/n 1'
_cod_database_code               4112928