Comparison of Structure and Reactivity of Phosphine-Amido and Hemilabile Phosphine-Amine Chelates of Rhodium
Lindsay J. Hounjet; Robert McDonald; Michael J. Ferguson; Martin Cowie; Inorganic Chemistry 50 (2011) 5361–5378; doi:10.1021/ic101883u

data_4325364
_publ_section_title
;
 Comparison of Structure and Reactivity of Phosphine-Amido and Hemilabile
 Phosphine-Amine Chelates of Rhodium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5361
_journal_page_last               5378
_journal_paper_doi               10.1021/ic101883u
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C45 H41 n O2 P3 Rh, 2.5(C6 H6)'
_chemical_formula_sum            'C60 H56 O2 P3 Rh n'
_chemical_formula_weight         1018.88
_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                 97.0481(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6143(11)
_cell_length_b                   25.953(3)
_cell_length_c                   18.329(2)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.25
_cell_volume                     5011.0(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43868
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    0.481
_exptl_absorpt_correction_T_max  0.9235
_exptl_absorpt_correction_T_min  0.8375
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       prism
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         11523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0413P)^2^+9.3155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1159
_reflns_number_gt                10092
_reflns_number_total             11523
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic101883u_si_001_4.cif
_cod_data_source_block           compound4
_cod_original_cell_volume        5011.0(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C60 H56 n O2 P3 Rh'
_cod_database_code               4325364