Deactivation of a [PPN][Rh(CO)4]-based catalytic system [PPN+ = (PPh3)2N+]. The first decomposition reaction of PPN+ and the formation of [Rh10P(CO)22]3−
Ragaini, Fabio; Sironi, Angelo; Fumagalli, Alessandro; Chemical Communications  (2000) 2117–; doi:10.1039/b006135m

data_7111085
_publ_section_title
;
 Deactivation of a [PPN][Rh(CO)4]-based catalytic system [PPN+ =
 (PPh3)2N+]. The first decomposition reaction of PPN+ and the formation of
 [Rh10P(CO)22]3&#x2212;
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2117
_journal_paper_doi               10.1039/b006135m
_journal_year                    2000
_chemical_formula_sum            'C130 H90 N3 O22 P7 Rh10'
_chemical_formula_weight         3291.94
_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                91.241(1)
_cell_angle_beta                 94.880(1)
_cell_angle_gamma                90.067(1)
_cell_formula_units_Z            2
_cell_length_a                   16.2084(7)
_cell_length_b                   16.3039(7)
_cell_length_c                   23.9367(11)
_cell_measurement_temperature    293(2)
_cell_volume                     6301.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.878
_diffrn_measured_fraction_theta_max 0.878
_diffrn_measurement_device_type  SMART
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            66631
_diffrn_reflns_theta_full        27.33
_diffrn_reflns_theta_max         27.33
_diffrn_reflns_theta_min         0.85
_diffrn_standards_decay_%        No
_exptl_absorpt_coefficient_mu    1.431
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3244
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.407
_refine_diff_density_min         -1.102
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     882
_refine_ls_number_reflns         24974
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+27.8601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1696
_reflns_number_gt                17154
_reflns_number_total             24974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006135msup1.cif
_cod_data_source_block           fefa
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111085
_exptl_absorpt_correction_nazim  SADABS
_diffrn_measurement_domega       0.3
_diffrn_measurement_rtime        30