Thermal Rearrangement via P‒C Bond Cleavage of a Tridentate Diphosphine‒N-Heterocyclic Carbene Ligand System Coordinated to Rhodium
Shaw, Bryan K.; Patrick, Brian O.; Fryzuk, Michael D.; Organometallics 31 (2012) 783–; doi:10.1021/om201233e

data_4068212
_publ_section_title
;
 Thermal Rearrangement via P--C Bond Cleavage of a Tridentate
 Diphosphine--N-Heterocyclic Carbene Ligand System Coordinated to Rhodium
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              783
_journal_paper_doi               10.1021/om201233e
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C65.75 H86 N4 O P4 Rh2'
_chemical_formula_weight         1278.09
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.000(5)
_cell_angle_beta                 115.799(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   29.629(5)
_cell_length_b                   8.564(5)
_cell_length_c                   27.107(5)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      1.70
_cell_volume                     6193(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker X8 Apex 2'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            43466
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.9342
_exptl_absorpt_correction_T_min  0.7036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS,Sheldrick(2008)
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2666
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.586
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         8575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.095
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+6.0316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                5846
_reflns_number_total             8575
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201233e_si_004.cif
_cod_data_source_block           m790_0m
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4068212