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_4072159
_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 ad
_chemical_formula_moiety         'C25 H33 As Cl N Pd '
_chemical_formula_sum            'C25 H33 As Cl N Pd'
_chemical_formula_weight         564.32
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             2000-03-06
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
2000-03-08 - Report on C25 H33 As Cl N Pd   by Anthony C. Willis
             for
             Keith A. Porter and S. Bruce Wild
2000-03-08 - passes checkcif with some alerts
2006-10-11 - cif edited for paper
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9468(1)
_cell_length_b                   13.5370(2)
_cell_length_c                   18.6809(2)
_cell_measurement_reflns_used    65545
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     2515.38(5)
_computing_cell_refinement
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full .99
_diffrn_measured_fraction_theta_max .99
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \w scans'
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.07581
_diffrn_reflns_av_sigmaI/netI    0.100
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            59091
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        30.
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         2.99
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.161
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144.00
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.85
_refine_ls_abs_structure_details
;
Absolute configuration by refinement of Flack parameter.
In agreement with known chirality of synthetic precursor.
;
_refine_ls_abs_structure_Flack   0.00010(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.746
_refine_ls_goodness_of_fit_ref   0.734
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    3
_refine_ls_number_parameters     269
_refine_ls_number_reflns         6019
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.0213
_refine_ls_shift/su_mean         0.2190
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)] '
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0362
_refine_ls_wR_factor_ref         0.0321
_reflns_number_gt                6019
_reflns_number_total             7346
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            om8006272_si_002.cif
_cod_data_source_block           kap5_with_numabs
_cod_depositor_comments
;
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_cell_volume        2515.38(4)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C25 H33 As Cl N Pd '
_cod_database_code               4072159