#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:28:04 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179897 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/93/7019357.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7019357
loop_
_publ_author_name
'Alhanash, Fatma B.'
'Barnes, Nicholas A.'
'Godfrey, Stephen M.'
'Hurst, Paul A.'
'Hutchinson, Adrian'
'Khan, Rana Z.'
'Pritchard, Robin G.'
_publ_section_title
;
 Structural isomerism in tris-tolyl halo-phosphonium and halo-arsonium
 tri-halides, [(CH(3)C(6)H(4))(3)EX][X(3)], (E = P, As; X = Br, I).
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7708
_journal_page_last               7728
_journal_paper_doi               10.1039/c2dt30235g
_journal_volume                  41
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H15 As1 I4'
_chemical_formula_sum            'C18 H15 As I4'
_chemical_formula_weight         813.7
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-07-07T13:29:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.2801(2)
_cell_length_b                   38.8869(9)
_cell_length_c                   9.13000(10)
_cell_measurement_reflns_used    5394
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      52
_cell_measurement_theta_min      2
_cell_measurement_wavelength     0.71073
_cell_volume                     4359.89(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99 (Beurskens et al, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.537006E-1
_diffrn_orient_matrix_UB_12      0.154205E-1
_diffrn_orient_matrix_UB_13      0.218774E-1
_diffrn_orient_matrix_UB_21      0.899396E-1
_diffrn_orient_matrix_UB_22      -0.184662E-1
_diffrn_orient_matrix_UB_23      0.134678E-1
_diffrn_orient_matrix_UB_31      0.319916E-1
_diffrn_orient_matrix_UB_32      0.777997E-1
_diffrn_orient_matrix_UB_33      -0.11396E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.093
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13398
_diffrn_reflns_reduction_process
;
Scaled and merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         3.14
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    7.222
_exptl_absorpt_correction_T_max  0.7141
_exptl_absorpt_correction_T_min  0.2654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.517
_refine_diff_density_min         -1.876
_refine_diff_density_rms         0.367
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.18
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.18
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.079
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0432P)²+193.9326P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1965
_reflns_number_gt                2709
_reflns_number_total             4078
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2dt30235g.txt
_cod_data_source_block           new6
_cod_original_cell_volume        4359.87(13)
_cod_database_code               7019357
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.4673(12) 0.0976(5) 0.4300(19) 0.042(4) Uani 1 1 d .
C2 C 0.4525(14) 0.0941(5) 0.5767(19) 0.048(4) Uani 1 1 d .
H2 H 0.4133 0.111 0.6303 0.057 Uiso 1 1 calc R
C3 C 0.4967(15) 0.0645(4) 0.6499(17) 0.046(4) Uani 1 1 d .
H3 H 0.4884 0.0616 0.7526 0.055 Uiso 1 1 calc R
C4 C 0.5525(15) 0.0400(6) 0.566(2) 0.057(5) Uani 1 1 d .
H4 H 0.5789 0.0195 0.6097 0.069 Uiso 1 1 calc R
C5 C 0.5685(16) 0.0459(4) 0.420(2) 0.055(5) Uani 1 1 d .
H5 H 0.6114 0.03 0.3662 0.066 Uiso 1 1 calc R
C6 C 0.5251(12) 0.0740(4) 0.3476(16) 0.036(4) Uani 1 1 d .
H6 H 0.5346 0.077 0.2452 0.044 Uiso 1 1 calc R
C7 C 0.3491(14) 0.1235(4) 0.1450(18) 0.043(4) Uani 1 1 d .
C8 C 0.3340(13) 0.0892(4) 0.1053(18) 0.041(4) Uani 1 1 d .
H8 H 0.351 0.0713 0.1723 0.049 Uiso 1 1 calc R
C9 C 0.2944(12) 0.0816(5) -0.0316(19) 0.045(4) Uani 1 1 d .
H9 H 0.2866 0.0583 -0.0613 0.055 Uiso 1 1 calc R
C10 C 0.2655(13) 0.1082(5) -0.1271(19) 0.046(4) Uani 1 1 d .
H10 H 0.236 0.1026 -0.2203 0.055 Uiso 1 1 calc R
C11 C 0.2789(14) 0.1434(5) -0.089(2) 0.052(5) Uani 1 1 d .
H11 H 0.2586 0.1612 -0.1545 0.062 Uiso 1 1 calc R
C12 C 0.3226(14) 0.1508(5) 0.048(2) 0.049(4) Uani 1 1 d .
H12 H 0.3348 0.174 0.0762 0.059 Uiso 1 1 calc R
C13 C 0.2812(13) 0.1511(4) 0.4470(16) 0.034(3) Uani 1 1 d .
C14 C 0.2682(13) 0.1829(5) 0.5071(18) 0.043(4) Uani 1 1 d .
H14 H 0.3252 0.1992 0.4953 0.052 Uiso 1 1 calc R
C15 C 0.1783(14) 0.1926(4) 0.5829(18) 0.042(4) Uani 1 1 d .
H15 H 0.172 0.2154 0.6193 0.051 Uiso 1 1 calc R
C16 C 0.0963(14) 0.1692(5) 0.607(2) 0.050(4) Uani 1 1 d .
H16 H 0.0344 0.1758 0.6622 0.06 Uiso 1 1 calc R
C17 C 0.1023(16) 0.1357(5) 0.5499(17) 0.048(4) Uani 1 1 d .
H17 H 0.0453 0.1196 0.5663 0.057 Uiso 1 1 calc R
C18 C 0.1951(13) 0.1266(5) 0.4683(17) 0.041(4) Uani 1 1 d .
H18 H 0.2009 0.1042 0.4273 0.049 Uiso 1 1 calc R
As1 As 0.40159(13) 0.13620(4) 0.33381(18) 0.0385(4) Uani 1 1 d .
I1 I 0.53501(9) 0.18502(3) 0.31500(12) 0.0433(3) Uani 1 1 d .
I2 I 0.72317(13) 0.25 0.30400(19) 0.0478(4) Uani 1 2 d S
I3 I 0.86033(14) 0.25 0.58504(19) 0.0481(4) Uani 1 2 d S
I4 I 0.99036(14) 0.25 0.83870(18) 0.0506(4) Uani 1 2 d S
I5 I 0 0 0.5 0.0464(4) Uani 1 2 d S
I6 I 0.21751(11) 0.02927(3) 0.52673(18) 0.0631(4) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.05 2.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.474 1.812 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
C2 C1 C6 122.6(16) .
C2 C1 As1 118.3(13) .
C6 C1 As1 119.1(12) .
C1 C2 C3 119.2(16) .
C1 C2 H2 120.4 .
C3 C2 H2 120.4 .
C4 C3 C2 118.2(15) .
C4 C3 H3 120.9 .
C2 C3 H3 120.9 .
C5 C4 C3 119.5(19) .
C5 C4 H4 120.3 .
C3 C4 H4 120.3 .
C4 C5 C6 122.9(19) .
C4 C5 H5 118.6 .
C6 C5 H5 118.6 .
C1 C6 C5 117.5(16) .
C1 C6 H6 121.3 .
C5 C6 H6 121.3 .
C8 C7 C12 121.5(16) .
C8 C7 As1 121.8(12) .
C12 C7 As1 116.7(13) .
C9 C8 C7 119.4(16) .
C9 C8 H8 120.3 .
C7 C8 H8 120.3 .
C8 C9 C10 119.8(17) .
C8 C9 H9 120.1 .
C10 C9 H9 120.1 .
C9 C10 C11 122.0(16) .
C9 C10 H10 119 .
C11 C10 H10 119 .
C12 C11 C10 117.8(16) .
C12 C11 H11 121.1 .
C10 C11 H11 121.1 .
C11 C12 C7 119.6(17) .
C11 C12 H12 120.2 .
C7 C12 H12 120.2 .
C14 C13 C18 117.5(15) .
C14 C13 As1 126.0(13) .
C18 C13 As1 116.4(11) .
C15 C14 C13 123.5(17) .
C15 C14 H14 118.2 .
C13 C14 H14 118.2 .
C14 C15 C16 119.5(16) .
C14 C15 H15 120.2 .
C16 C15 H15 120.2 .
C15 C16 C17 121.2(17) .
C15 C16 H16 119.4 .
C17 C16 H16 119.4 .
C16 C17 C18 118.2(17) .
C16 C17 H17 120.9 .
C18 C17 H17 120.9 .
C17 C18 C13 120.0(16) .
C17 C18 H18 120 .
C13 C18 H18 120 .
C13 As1 C7 108.0(7) .
C13 As1 C1 108.5(7) .
C7 As1 C1 110.8(7) .
C13 As1 I1 108.4(5) .
C7 As1 I1 110.7(5) .
C1 As1 I1 110.4(5) .
I4 I3 I2 178.69(8) .
I6 I5 I6 180.00(5) 5_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.36(2) .
C1 C6 1.38(2) .
C1 As1 1.917(17) .
C2 C3 1.44(2) .
C2 H2 0.95 .
C3 C4 1.40(3) .
C3 H3 0.95 .
C4 C5 1.36(3) .
C4 H4 0.95 .
C5 C6 1.39(2) .
C5 H5 0.95 .
C6 H6 0.95 .
C7 C8 1.39(2) .
C7 C12 1.42(2) .
C7 As1 1.905(17) .
C8 C9 1.37(2) .
C8 H8 0.95 .
C9 C10 1.40(2) .
C9 H9 0.95 .
C10 C11 1.42(3) .
C10 H10 0.95 .
C11 C12 1.39(3) .
C11 H11 0.95 .
C12 H12 0.95 .
C13 C14 1.36(2) .
C13 C18 1.44(2) .
C13 As1 1.895(15) .
C14 C15 1.36(2) .
C14 H14 0.95 .
C15 C16 1.37(2) .
C15 H15 0.95 .
C16 C17 1.40(2) .
C16 H16 0.95 .
C17 C18 1.41(2) .
C17 H17 0.95 .
C18 H18 0.95 .
As1 I1 2.514(2) .
I2 I3 3.069(2) .
I3 I4 2.813(2) .
I5 I6 2.9136(13) .
I5 I6 2.9136(13) 5_556
