Phosphine Complexes of an Enantiomerically Pure, Atropisomeric Arsenium Ion
Kilah, Nathan L.; Wild, S. Bruce; Organometallics 31 (2012) 2658–; doi:10.1021/om200853d

data_4077862
_publ_section_title
;
 Phosphine Complexes of an Enantiomerically Pure, Atropisomeric Arsenium
 Ion
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2658
_journal_paper_doi               10.1021/om200853d
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration rmad
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C22 H16 As I '
_chemical_formula_sum            'C22 H16 As I'
_chemical_formula_weight         482.20
_space_group_IT_number           170
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-14-06
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2006-06-19 - Report on C22 H16 As1 I1
             by Nathan L. Kilah
             for S. Bruce Wild

2006-06-19 - Passed CheckCif with minor warnings.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   16.8728(5)
_cell_length_b                   16.8728(5)
_cell_length_c                   11.2567(2)
_cell_measurement_reflns_used    32747
_cell_measurement_temperature    200
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     2775.34(13)
_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  0.04
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            35246
_diffrn_reflns_theta_full        27.475
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         2.788
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.505
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' needle '
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.20
_refine_diff_density_min         -1.48
_refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.008(12)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0007
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2929
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.000569
_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: 
 1.75 0.865 1.52 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0339
_refine_ls_wR_factor_gt          0.0301
_refine_ls_wR_factor_ref         0.0301
_reflns_limit_h_max              0
_reflns_limit_h_min              -18
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -14
_reflns_number_gt                2929
_reflns_number_total             4121
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            om200853d_si_002.cif
_cod_data_source_block           kilah10_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_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_Hall     'P 65 '
_cod_original_sg_symbol_H-M      'P 65 '
_cod_original_formula_sum        ' C22 H16 As I '
_cod_database_code               4077862