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

data_4077867
_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         ' C41 H35 As1 O1 P1, F6 P1, C2 H4 O0.5 '
_chemical_formula_sum            'C43 H39 As F6 O1.5 P2'
_chemical_formula_weight         830.64
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-08-11
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2007-11-08 - Report on C47 H47 As1 F6 O1.5 P2
             by Nathan L. Kilah
             for S. Bruce Wild

2007-11-08 - Passed CheckCif with minor warnings.
 

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.7230(4)
_cell_length_b                   18.7230(4)
_cell_length_c                   23.0827(4)
_cell_measurement_reflns_used    127298
_cell_measurement_temperature    200
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     8091.7(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.068
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            94598
_diffrn_reflns_theta_full        27.875
_diffrn_reflns_theta_max         27.875
_diffrn_reflns_theta_min         2.588
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.54
_refine_ls_abs_structure_details 'Flack, 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.012(10)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8645
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         3553
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0389
_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: 
 1.74 0.728 1.51 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0584
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0412
_reflns_limit_h_max              17
_reflns_limit_h_min              -16
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                3553
_reflns_number_total             9636
_reflns_threshold_expression     I>2.00u(I)
_cod_data_source_file            om200853d_si_002.cif
_cod_data_source_block           kilah22_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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 4nw 2abw '
_cod_original_sg_symbol_H-M      'P 43 21 2 '
_cod_original_formula_sum        ' C43 H39 As1 F6 O1.5 P2 '
_cod_database_code               4077867