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_4302851
_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_compound_source
;
?
;
_chemical_formula_moiety         ' (C40 H40 As2 P2), (C1 F3 O3 S1)2 '
_chemical_formula_sum            'C42 H40 As2 F6 O6 P2 S2'
_chemical_formula_weight         1030.69
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             05-14-10
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2005-10-14 - Report on C42 H40 As2 F6 O6 P2 S2
             by Nathan L. Kilah
            for Michelle L. Weir and S. Bruce Wild

2005-10-14 - Passes Checkcif with minor warnings.

;
_cell_angle_alpha                90
_cell_angle_beta                 95.6724(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5468(2)
_cell_length_b                   11.2427(2)
_cell_length_c                   17.0825(3)
_cell_measurement_reflns_used    25333
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     2206.74(7)
_computing_cell_refinement
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
 COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_molecular_graphics
; 
 ORTEP3 (Farrugia 1997) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2003) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin 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_type
; 
Nonius Kappa CCD 
;
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45490
_diffrn_reflns_theta_full        27.485
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.728
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.752
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             1044.000
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.2801
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         2863
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.000206
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.739 0.137 0.382 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0571
_refine_ls_wR_factor_gt          0.0427
_refine_ls_wR_factor_ref         0.0427
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                2863
_reflns_number_total             5057
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic900797y_si_001_1.cif
_cod_data_source_block           michelle03_cif
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value ' not measured ' was changed to
'?' - the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C42 H40 As2 F6 O6 P2 S2 '
_cod_database_code               4302851