Asymmetric Hydroformylation of Olefins with Rh Catalysts Modified with Chiral Phosphine−Phosphite Ligands
Rubio, Miguel; Suárez, Andrés; Álvarez, Eleuterio; Bianchini, Claudio; Oberhauser, Werner; Peruzzini, Maurizio; Pizzano, Antonio; Organometallics 26 (2007) 6428–; doi:10.1021/om700744b

data_4073934
_publ_section_title
;
 Asymmetric Hydroformylation of Olefins with Rh Catalysts Modified with
 Chiral Phosphine&#x2212;Phosphite Ligands
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              6428
_journal_paper_doi               10.1021/om700744b
_journal_volume                  26
_journal_year                    2007
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C44 H50 Cl2 O3 P2 Pd, 2.5(C7 H8)'
_chemical_formula_sum            'C61.5 H70 Cl2 O3 P2 Pd'
_chemical_formula_weight         1096.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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                101.028(2)
_cell_angle_beta                 96.166(2)
_cell_angle_gamma                92.380(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4905(6)
_cell_length_b                   14.6466(9)
_cell_length_c                   18.4648(11)
_cell_measurement_reflns_used    9462
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.31
_cell_measurement_theta_min      2.49
_cell_volume                     2763.0(3)
_computing_cell_refinement       'SAINT+ v. 7.06 a (Bruker AXS, 2003)'
_computing_data_collection       'APEX-W2K-NT v. 1.0 (Bruker AXS, 2004)'
_computing_data_reduction        'SAINT+ v. 7.06 a (Bruker AXS, 2001)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.10 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker-Nonius X8kappa APEX II CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            74197
_diffrn_reflns_theta_full        30.58
_diffrn_reflns_theta_max         30.58
_diffrn_reflns_theta_min         2.90
_diffrn_standards_number         'no decay'
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  0.9386
_exptl_absorpt_correction_T_min  0.8915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. Bruker-AXS
 within v. 7.06 a (Bruker AXS, 2003).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1146
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.749
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.020(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1452
_refine_ls_number_reflns         31966
_refine_ls_number_restraints     1251
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0657P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                26744
_reflns_number_total             31966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700744b-file003.cif
_cod_data_source_block           7e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

2026-02-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C123 H140 Cl4 O6 P4 Pd2'
_cod_original_formula_weight         2192.83
_cod_original_formula_moiety         '2(C44 H50 Cl2 O3 P2 Pd), 5(C7 H8)'
_cod_original_formula_units_Z            1
_cod_original_sg_symbol_H-M      P1
_cod_database_code               4073934