Asymmetric Synthesis of a Tertiary Arsine by Nucleophilic Addition to a Chiral Phosphine-Stabilized Arsenium Salt
Coote, Michelle L.; Krenske, Elizabeth H.; Porter, Keith A.; Weir, Michelle L.; Willis, Anthony C.; Zhou, Xiangting; Wild, S. Bruce; Organometallics 27 (2008) 5099–; doi:10.1021/om8006272

data_4072158
_publ_section_title
;
 Asymmetric Synthesis of a Tertiary Arsine by Nucleophilic Addition to a
 Chiral Phosphine-Stabilized Arsenium Salt
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5099
_journal_paper_doi               10.1021/om8006272
_journal_volume                  27
_journal_year                    2008
_chemical_absolute_configuration rmad
_chemical_compound_source
;
?
;
_chemical_formula_moiety
' C37 H33 As O P +, P F6 -, .37(C4 H10 O), .13(C H2 Cl2), .13(C H2 Cl2) '
_chemical_formula_sum            'C38.73 H37.2 As Cl0.53 F6 O1.37 P2'
_chemical_formula_weight         794.34
_chemical_melting_point          ?
_chemical_name_systematic
;                                                                               
?                                                                               
;
_space_group_IT_number           178
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61 2 (0 0 5)'
_symmetry_space_group_name_H-M   'P 61 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             04-26-03
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2004-03-26 - Report on C38.62 H36.89 As1 Cl0.60 F6 O1.33 P2 
             by Anthony C. Willis
             for  Bruce Wild and Elizabeth Krenske

2002-03-26 - passes checkcif tests with minor warnings  
2006-10-11 - cif edited for paper

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   16.4243(2)
_cell_length_b                   16.4243(2)
_cell_length_c                   47.0990(4)
_cell_measurement_reflns_used    113171
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     11003.1(2)
_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
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.07
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            53391
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.518
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' needle '
_exptl_crystal_F_000             4879.122
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.63
_refine_ls_abs_structure_details 'Flack, 2636 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.009(11)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1271
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         4312
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.002
_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: 
 1.01 -0.433 0.946 -0.171 0.234 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0432
_refine_ls_wR_factor_gt          0.0386
_refine_ls_wR_factor_ref         0.0386
_reflns_limit_h_max              0
_reflns_limit_h_min              -16
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              55
_reflns_limit_l_min              0
_reflns_number_gt                4312
_reflns_number_total             6473
_reflns_threshold_expression     I>2.00u(I)
_cod_data_source_file            om8006272_si_002.cif
_cod_data_source_block           ehk9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_symmetry_cell_setting' value
'Hexagonal' changed to 'hexagonal' 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 

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 61 2 2 '
_cod_original_formula_sum        ' C38.73 H37.20 As1 Cl0.53 F6 O1.37 P2 '
_cod_database_code               4072158