Rhodium Complexes of Cyclopropenylidene Carbene Ligands: Synthesis, Structure, and Hydroformylation Catalysis
Green, Michael; McMullin, Claire L.; Morton, George J. P.; Orpen, A. Guy; Wass, Duncan F.; Wingad, Richard L.; Organometallics 28 (2009) 1476–; doi:10.1021/om801031a

data_4068682
_publ_section_title
;
 Rhodium Complexes of Cyclopropenylidene Carbene Ligands: Synthesis,
 Structure, and Hydroformylation Catalysis
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1476
_journal_paper_doi               10.1021/om801031a
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C51 H40 Cl3 P2 Rh, 2(C H Cl3)'
_chemical_formula_sum            'C53 H42 Cl9 P2 Rh'
_chemical_formula_weight         1162.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.8530(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8965(3)
_cell_length_b                   23.6104(6)
_cell_length_c                   17.0719(3)
_cell_measurement_reflns_used    35506
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     5087.4(2)
_computing_cell_refinement
; 
DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
Although determined using DirAx, the cell is refined in the HKL 
package during data reduction 
;
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998) '
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
; 
Bruker-Nonius Roper CCD camera on \k-goniostat 
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1256
_diffrn_reflns_av_sigmaI/netI    0.1130
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            59125
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_meas      x
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.333
_refine_diff_density_min         -1.548
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         11673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.0778
_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^)+(0.1046P)^2^+4.8819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.2025
_reflns_number_gt                7589
_reflns_number_total             11673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801031a_si_001.cif
_cod_data_source_block           gm039
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4068682