"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_4112929
_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_moiety         'C66 H62 Br2 Fe1 Ni1 P4, 3(CHCl3)'
_chemical_formula_sum            'C69 H65 Br2 Cl9 Fe Ni P4'
_chemical_formula_weight         1611.52
_chemical_name_systematic
;
 ?
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.320(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1064(2)
_cell_length_b                   40.2368(7)
_cell_length_c                   14.5029(3)
_cell_measurement_reflns_used    8601
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      0.998
_cell_volume                     7052.8(2)
_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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_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  0.0931
_diffrn_reflns_av_sigmaI/netI    0.1763
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26492
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         2.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.078
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       prism
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.390
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         12660
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1668
_refine_ls_R_factor_gt           0.0691
_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^)+(0.0613P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                6571
_reflns_number_total             12660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048907asi20040309_020107_2.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4112929