Tertiary arsine-stabilised arsenium salts: syntheses and comparisons with phosphine analogues
Kilah, Nathan L.; Weir, Michelle L.; Wild, S. Bruce; Dalton Transactions  (2008) 2480–2486; doi:10.1039/b800965a

data_7003880
_publ_section_title
;
 Tertiary arsine-stabilised arsenium salts: syntheses and comparisons
 with phosphine analogues
;
_journal_issue                   18
_journal_name_full               'Dalton Transactions'
_journal_page_first              2480
_journal_page_last               2486
_journal_paper_doi               10.1039/b800965a
_journal_year                    2008
_chemical_formula_moiety         'C27 H27 As2 O1, C1 F3 O3 S1'
_chemical_formula_sum            'C28 H27 As2 F3 O4 S'
_chemical_formula_weight         666.42
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-03-18
_audit_creation_method           CRYSTALS_ver_12.18
_audit_update_record
;
2007-03-25 - Report on C28 H27 As2 F3 O4 S1
by Nathan L. Kilah
for Michelle L. Weir and S. Bruce Wild

2007-03-25 - Passed CheckCif with minor warnings.

;
_cell_angle_alpha                93.6545(9)
_cell_angle_beta                 111.8762(9)
_cell_angle_gamma                112.4184(9)
_cell_formula_units_Z            2
_cell_length_a                   11.0285(2)
_cell_length_b                   11.4661(2)
_cell_length_c                   13.0560(2)
_cell_measurement_reflns_used    24403
_cell_measurement_temperature    200
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     1374.93(4)
_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 KappaCCD'
_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  0.033
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            42711
_diffrn_reflns_theta_full        27.907
_diffrn_reflns_theta_max         27.907
_diffrn_reflns_theta_min         2.926
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.559
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0626
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4611
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.000390
_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:
1.05 0.215 0.834
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0344
_refine_ls_wR_factor_gt          0.0305
_refine_ls_wR_factor_ref         0.0305
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                4611
_reflns_number_total             6580
_reflns_threshold_expression     I>3.0\s(I)
_cod_data_source_file            b800965a.txt
_cod_data_source_block           michelle07_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 '
_cod_original_formula_sum        'C28 H27 As2 F3 O4 S1'
_cod_database_code               7003880