Direct synthesis of chiral tertiary diphosphines via Pd(II)-catalyzed asymmetric hydrophosphination of dienones.
Huang, Yinhua; Chew, Renta Jonathan; Li, Yongxin; Pullarkat, Sumod A.; Leung, Pak-Hing; Organic letters 13 (2011) 5862–5865; doi:10.1021/ol202480r

data_1502564
_publ_section_title
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 Direct synthesis of chiral tertiary diphosphines via Pd(II)-catalyzed
 asymmetric hydrophosphination of dienones.
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_journal_issue                   21
_journal_name_full               'Organic letters'
_journal_page_first              5862
_journal_page_last               5865
_journal_paper_doi               10.1021/ol202480r
_journal_volume                  13
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_sum            'C108 H104 Cl2 N2 O2 P2 Pd2'
_chemical_formula_weight         1807.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           97
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            24
_cell_length_a                   39.8657(12)
_cell_length_b                   39.8657(12)
_cell_length_c                   38.2114(13)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      18.75
_cell_measurement_theta_min      2.52
_cell_volume                     60728(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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
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_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            246984
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.8444
_exptl_absorpt_correction_T_min  0.8292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             22512
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.36
_refine_diff_density_max         1.670
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
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_refine_ls_number_parameters     1371
_refine_ls_number_reflns         26847
_refine_ls_number_restraints     463
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1037P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.1752
_reflns_number_gt                19798
_reflns_number_total             26847
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol202480r_si_003.cif
_cod_data_source_block           leung613p
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 
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_cod_original_sg_symbol_H-M      I422
_cod_database_code               1502564