Asymmetric Hydrovinylation of Unactivated Linear 1,3-Dienes
Rakesh K. Sharma; T. V. RajanBabu; Journal of the American Chemical Society 132 (2010) 3295–3297; doi:10.1021/ja1004703

data_4102032
_publ_section_title
;
 Asymmetric Hydrovinylation of Unactivated Linear 1,3-Dienes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3295
_journal_page_last               3297
_journal_paper_doi               10.1021/ja1004703
_journal_volume                  132
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C31 H32 Cl2 Co1 O2 P2'
_chemical_formula_sum            'C31 H32 Cl2 Co O2 P2'
_chemical_formula_weight         628.34
_chemical_name_common            'RajanBabu 1745'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-01-11T13:50:35-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 91.6380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2321(2)
_cell_length_b                   9.5331(1)
_cell_length_c                   18.4717(2)
_cell_measurement_reflns_used    7292
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     3033.20(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'omega scans'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.541704E-1
_diffrn_orient_matrix_UB_12      -0.20895E-1
_diffrn_orient_matrix_UB_13      0.176554E-1
_diffrn_orient_matrix_UB_21      0.198103E-1
_diffrn_orient_matrix_UB_22      0.79023E-1
_diffrn_orient_matrix_UB_23      -0.299065E-1
_diffrn_orient_matrix_UB_31      -0.65949E-2
_diffrn_orient_matrix_UB_32      0.657441E-1
_diffrn_orient_matrix_UB_33      0.415582E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.047
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            70698
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.21
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.874
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.012(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     713
_refine_ls_number_reflns         13262
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+1.3339P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0795
_reflns_number_gt                11294
_reflns_number_total             13262
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja1004703_si_003.cif
_cod_data_source_block           RajanBabu1745
_cod_database_code               4102032