Asymmetric Synthesis of Bis(tertiary arsines): Highly Stereoselective Alkylations of Diastereomers of a Chiral Phosphine-Stabilized Bis(arsenium triflate)
Michelle L. Weir; Ian A. Cade; Nathan L. Kilah; Xiangting Zhou; S. Bruce Wild; Inorganic Chemistry 48 (2009) 7482–7490; doi:10.1021/ic900797y

data_4302852
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       ' sbw@rsc.anu.edu.au '
_publ_contact_author_fax         ' 61 2 6125 0750 '
_publ_contact_author_name        ' S. Bruce Wild '
_publ_contact_author_phone       ' 61 2 6125 4236 '
_publ_section_title
;
Asymmetric Synthesis of Bis(tertiary arsines): Highly Stereoselective
Alkylations of Diastereomers of a Chiral Phosphine-Stabilized Bis(arsenium
triflate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7482
_journal_page_last               7490
_journal_paper_doi               10.1021/ic900797y
_journal_volume                  48
_journal_year                    2009
_chemical_absolute_configuration rmad
_chemical_compound_source        local
_chemical_formula_moiety         '(C36 H40 As2 P2 Pt1), (C1 F3 O3 S1)2 '
_chemical_formula_sum            'C38 H40 As2 F6 O6 P2 Pt S2'
_chemical_formula_weight         1177.73
_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
_audit_creation_date             09-04-14
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9541(2)
_cell_length_b                   16.5910(1)
_cell_length_c                   18.8238(2)
_cell_measurement_reflns_used    48061
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      0
_cell_volume                     4357.94(8)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            61481
_diffrn_reflns_theta_full        27.490
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         1.817
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.965
_exptl_absorpt_correction_T_max  0.386
_exptl_absorpt_correction_T_min  0.180
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.10
_refine_diff_density_min         -1.44
_refine_ls_abs_structure_details 'Flack (1983), 4486 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.024(4)
_refine_ls_extinction_coef       50(10)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.8661
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         9978
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.011394
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.01P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0534
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0534
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                8962
_reflns_number_total             10011
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.33
_oxford_diffrn_Wilson_scale      29.01
_oxford_refine_ls_r_factor_ref   0.0286
_oxford_refine_ls_scale          0.33715(18)
_oxford_reflns_number_all        9978
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '9301834 MLW3.17'
_cod_data_source_file            ic900797y_si_001_2.cif
_cod_data_source_block           cade015_cif
_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      'P 21 21 21 '
_cod_original_formula_sum        'C38 H40 As2 F6 O6 P2 Pt1 S2'
_cod_database_code               4302852