Tripyrrolylphosphine as a Unique Bridging Ligand in the Rh6(CO)14(μ2-P(NC4H4)3) Cluster: Structure, Bonding, Fluxionality, Thermodynamics, and Kinetics Studies
Claudia Babij; C. Scott Browning; David H. Farrar; Igor O. Koshevoy; Ivan S. Podkorytov; Anthony J. Poë; Sergey P. Tunik; Journal of the American Chemical Society 124 (2002) 8922–8931; doi:10.1021/ja012440b

data_4114971
_publ_contact_author_address
;
Lash Miller Chemical Laboratories
University of Toronto
80 St. George St.
Toronto, Ontario, Canada M5S 3H6
;
_publ_contact_author_email       dfarrar@chem.utoronto.ca
_publ_contact_author_fax         '416 978 1631'
_publ_contact_author_name        'David H. Farrar'
_publ_section_title
;
 Tripyrrolylphosphine as a Unique Bridging Ligand in the
 Rh6(CO)14(\m2-P(NC4H4)3) Cluster: Structure, Bonding, Fluxionality,
 Thermodynamics, and Kinetics Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8922
_journal_page_last               8931
_journal_paper_doi               10.1021/ja012440b
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C26 H12 N3 O14 P Rh6'
_chemical_formula_weight         1238.82
_chemical_name_common            Rh6(CO)14(Ppy3)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 96.38(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9505(8)
_cell_length_b                   9.4316(4)
_cell_length_c                   23.3019(13)
_cell_measurement_reflns_used    24441
_cell_measurement_temperature    100(1)
_cell_volume                     3265.4(3)
_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    'Bruker SHELXTL V5.1'
_computing_publication_material  'Bruker SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans & \w scans with \k offsets'
_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  0.0686
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24441
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         4.11
_exptl_absorpt_coefficient_mu    3.083
_exptl_absorpt_correction_T_max  0.6145
_exptl_absorpt_correction_T_min  0.4116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.520
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.659
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.212
_refine_ls_extinction_coef       0.00055(7)
_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   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         7434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+35.6773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                4965
_reflns_number_total             7434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja012440b.cif
_cod_data_source_block           k9924
_cod_database_code               4114971