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_4325361
_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_sum            'C33 H35 P Rh n'
_chemical_formula_weight         579.50
_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                72.4250(2)
_cell_angle_beta                 82.6184(3)
_cell_angle_gamma                68.1805(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3000(3)
_cell_length_b                   11.3914(3)
_cell_length_c                   14.3271(4)
_cell_measurement_reflns_used    9189
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.36
_cell_volume                     1343.08(7)
_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    'SIR-97 (Altomare et al, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0079
_diffrn_reflns_av_sigmaI/netI    0.0124
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11885
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  0.8489
_exptl_absorpt_correction_T_min  0.6645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       fragment
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         6116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0186
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+0.7218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0507
_reflns_number_gt                5995
_reflns_number_total             6116
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic101883u_si_001_1.cif
_cod_data_source_block           compound1a
_cod_original_formula_sum        'C33 H35 n P Rh'
_cod_database_code               4325361