Rhodium(0) Metalloradicals in Binuclear C-H Activation
Florian F. Puschmann; Hansjörg Grützmacher; Bas de Bruin; Journal of the American Chemical Society 132 (2010) 73–75; doi:10.1021/ja909022p

data_4101771
_publ_contact_author_address
;Department of Chemistry and Applied Biosciences
ETH Zurich
Wolfgang Pauli Str. 10
CH-8093 Zurich
Switzerland
;
_publ_contact_author_email       gruetzmacher@inorg.chem.ethz.ch
_publ_contact_author_fax         '+41 44 633 14 18'
_publ_contact_author_name        'Hansjoerg Gruetzmacher'
_publ_contact_author_phone       '+41 44 632 28 55'
_publ_section_title
;
 Rhodium(0) Metalloradicals in Binuclear C-H Activation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              73
_journal_page_last               75
_journal_paper_doi               10.1021/ja909022p
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         '2(C54 H41 P2 Rh), C4 H10 O'
_chemical_formula_sum            'C112 H92 O P4 Rh2'
_chemical_formula_weight         1783.56
_chemical_melting_point          250
_chemical_name_common            '[Rh((C6H4)PPh2)(trop2PPh)]'
_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                63.58(3)
_cell_angle_beta                 78.33(3)
_cell_angle_gamma                66.59(3)
_cell_formula_units_Z            1
_cell_length_a                   12.245(3)
_cell_length_b                   14.106(3)
_cell_length_c                   15.104(3)
_cell_measurement_reflns_used    10598
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      1.7
_cell_volume                     2143.1(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep32 for Windows'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Apex'
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22493
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.51
_diffrn_standards_interval_time  15
_diffrn_standards_number         22493
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  0.9748
_exptl_absorpt_correction_T_min  0.9410
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS 2008/1, Bruker'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       undef
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         10598
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0364P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0857
_reflns_number_gt                8995
_reflns_number_total             10598
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja909022p_si_002.cif
_cod_data_source_block           '[rh(c6h4pph2)(trop2pph)]'
_cod_original_cell_volume        2143.1(8)
_cod_database_code               4101771