Controllable synthesis of P-chiral 1,2- and 1,3-diphosphines via asymmetric Diels‒Alder reactions involving functionalized allylic phosphines as dienophiles
Yuan, Mingjun; Pullarkat, Sumod A.; Yeong, Crystal Huixian; Li, Yongxin; Krishnan, Deepa; Leung, Pak-Hing; Dalton Transactions  (2009) 3668–3670; doi:10.1039/b904090k

data_7001238
_publ_section_title
;
 Controllable synthesis of P-chiral 1,2- and 1,3-diphosphines via
 asymmetric Diels--Alder reactions involving functionalized allylic
 phosphines as dienophiles
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              3668
_journal_page_last               3670
_journal_paper_doi               10.1039/b904090k
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H30 Cl2 O2 P2 Pd'
_chemical_formula_sum            'C29 H30 Cl2 O2 P2 Pd'
_chemical_formula_weight         649.77
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8932(2)
_cell_length_b                   15.1804(3)
_cell_length_c                   20.1229(4)
_cell_measurement_reflns_used    9130
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.93
_cell_measurement_theta_min      2.43
_cell_volume                     2716.64(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43231
_diffrn_reflns_theta_full        31.96
_diffrn_reflns_theta_max         31.96
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  0.9602
_exptl_absorpt_correction_T_min  0.7487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         9379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0220
_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^)+(0.0310P)^2^+0.2765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0633
_reflns_number_gt                8789
_reflns_number_total             9379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b904090k.txt
_cod_data_source_block           leung355
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               7001238