Modular functionalized polyphosphines for supported materials: previously unobserved 31P-NMR 'through-space' ABCD spin systems and heterogeneous palladium-catalysed C-C and C-H arylation
Matthieu Beauperin; Radomyr Smaliy; Helene Cattey; Philippe Meunier; Jun Ou; Patrick H. Toy; Jean-Cyrille Hierso; Chem.Commun. 50 (2014) 9505–; doi:10.1039/C4cc04307C

data_7115473
_publ_section_title
;
 Modular functionalized polyphosphines for supported materials: previously
 unobserved 31P-NMR 'through-space' ABCD spin systems and heterogeneous
 palladium-catalysed C-C and C-H arylation
;
_journal_name_full               Chem.Commun.
_journal_page_first              9505
_journal_paper_doi               10.1039/C4cc04307C
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C76 H78 Fe1 O4 P4, 2 (C H2 Cl2)'
_chemical_formula_sum            'C78 H82 Cl4 Fe O4 P4'
_chemical_formula_weight         1404.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.6180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1018(2)
_cell_length_b                   15.8815(2)
_cell_length_c                   26.2016(3)
_cell_measurement_reflns_used    25968
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     7116.00(15)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.988
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            20341
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         2.822
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       prism
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         16153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+3.4243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12404
_reflns_number_total             16153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc04307c2.cif
_cod_data_source_block           jc12
_cod_original_formula_sum        'C78 H82 Cl4 Fe1 O4 P4'
_cod_database_code               7115473
_shelx_estimated_absorpt_t_min   0.832
_shelx_estimated_absorpt_t_max   0.906
_shelxl_version_number           2013-4
_shelx_res_checksum              64575