Palladacycle-Catalyzed Asymmetric Intermolecular Construction of Chiral Tertiary P-Heterocycles by Stepwise Addition of H‒P‒H Bonds to Bis(enones)
Huang, Yinhua; Pullarkat, Sumod A.; Teong, Siewping; Chew, Renta Jonathan; Li, Yongxin; Leung, Pak-Hing; Organometallics 31 (2012) 4871–; doi:10.1021/om300405h

data_4078767
_publ_section_title
;
 Palladacycle-Catalyzed Asymmetric Intermolecular Construction of Chiral
 Tertiary P-Heterocycles by Stepwise Addition of H--P--H Bonds to
 Bis(enones)
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              4871
_journal_paper_doi               10.1021/om300405h
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C37 H37 Cl N O P Pd, 0.5(C4 H8 O)'
_chemical_formula_sum            'C39 H41 Cl N O1.5 P Pd'
_chemical_formula_weight         720.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.523(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0288(5)
_cell_length_b                   16.9223(7)
_cell_length_c                   18.7700(7)
_cell_measurement_reflns_used    6177
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      22.79
_cell_measurement_theta_min      2.26
_cell_volume                     3375.3(2)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0688
_diffrn_reflns_av_sigmaI/netI    0.1371
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39398
_diffrn_reflns_theta_full        31.20
_diffrn_reflns_theta_max         31.20
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  0.9586
_exptl_absorpt_correction_T_min  0.7943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.075
_refine_diff_density_min         -2.113
_refine_diff_density_rms         0.238
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         18756
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0623
_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^)+(0.0868P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1763
_reflns_number_gt                12205
_reflns_number_total             18756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300405h_si_003.cif
_cod_data_source_block           leung639s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_original_formula_sum        'C39 H41 Cl N O1.50 P Pd'
_cod_database_code               4078767