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#$Date: 2016-03-22 11:40:12 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178910 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/39/4113904.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_4113904
loop_
_publ_author_name
'Ke Zhang'
'Janardhana Prabhavathy'
'John H. K. Yip'
'Lip Lin Koh'
'Geok Kheng Tan'
'Jagadese J. Vittal'
_publ_section_title
;
 First Examples of AuI-X-AgI Halonium Cations (X = Cl and Br)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8452
_journal_page_last               8453
_journal_paper_doi               10.1021/ja035064z
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C78 H60 Ag Au4 Cl8 F6 P4 Sb'
_chemical_formula_weight         2536.23
_chemical_name_common            3.2CH2Cl2
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.952(3)
_cell_length_b                   17.952(3)
_cell_length_c                   25.388
_cell_measurement_reflns_used    4269
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      24.05
_cell_measurement_theta_min      2.27
_cell_volume                     8181.9(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23539
_diffrn_reflns_theta_full        24.95
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    8.100
_exptl_absorpt_correction_T_max  0.4432
_exptl_absorpt_correction_T_min  0.2272
_exptl_absorpt_correction_type   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             4768
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.505
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3693
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0805P)²+17.2551P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1318
_reflns_number_gt                2757
_reflns_number_total             3693
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja035064zsi20030309_013304.cif
_cod_data_source_block           2223a
_cod_original_cell_volume        8182.0(18)
_cod_database_code               4113904
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
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
Au1 Au 0.562269(18) 0.904116(19) 0.847625(13) 0.03805(17) Uani 1 1 d .
Ag1 Ag 0.5000 1.0000 0.7500 0.0779(6) Uani 1 4 d S
Cl1 Cl 0.44082(12) 0.90602(13) 0.81719(9) 0.0477(6) Uani 1 1 d .
P1 P 0.68117(12) 0.89281(12) 0.87325(8) 0.0354(5) Uani 1 1 d .
C1 C 0.5765(5) 1.0660(5) 0.9730(4) 0.047(2) Uani 1 1 d .
H1A H 0.5496 1.1028 0.9548 0.056 Uiso 1 1 calc R
C2 C 0.6148(5) 1.0134(5) 0.9450(4) 0.043(2) Uani 1 1 d .
H2A H 0.6140 1.0143 0.9080 0.051 Uiso 1 1 calc R
C3 C 0.6558(4) 0.9575(4) 0.9717(3) 0.0304(17) Uani 1 1 d .
C4 C 0.6985(4) 0.9046(4) 0.9444(3) 0.0317(18) Uani 1 1 d .
C5 C 0.7515(4) 0.8619(5) 0.9719(3) 0.0341(18) Uani 1 1 d .
C6 C 0.8102(5) 0.8213(5) 0.9464(3) 0.046(2) Uani 1 1 d .
H6A H 0.8116 0.8210 0.9094 0.055 Uiso 1 1 calc R
C7 C 0.8636(5) 0.7833(5) 0.9727(4) 0.052(2) Uani 1 1 d .
H7A H 0.9004 0.7571 0.9541 0.062 Uiso 1 1 calc R
C1A C 0.7441(4) 0.9558(4) 0.8402(3) 0.0343(19) Uani 1 1 d .
C2A C 0.8081(5) 0.9825(5) 0.8658(4) 0.044(2) Uani 1 1 d .
H2AA H 0.8179 0.9697 0.9011 0.053 Uiso 1 1 calc R
C3A C 0.8571(6) 1.0287(6) 0.8377(5) 0.059(3) Uani 1 1 d .
H3AA H 0.9003 1.0470 0.8541 0.070 Uiso 1 1 calc R
C4A C 0.8419(6) 1.0476(5) 0.7855(4) 0.056(3) Uani 1 1 d .
H4AA H 0.8751 1.0782 0.7667 0.068 Uiso 1 1 calc R
C5A C 0.7784(6) 1.0214(6) 0.7616(4) 0.059(3) Uani 1 1 d .
H5AA H 0.7680 1.0348 0.7266 0.071 Uiso 1 1 calc R
C6A C 0.7303(5) 0.9763(5) 0.7883(3) 0.046(2) Uani 1 1 d .
H6AA H 0.6873 0.9587 0.7713 0.055 Uiso 1 1 calc R
C1B C 0.7046(5) 0.7985(5) 0.8542(3) 0.040(2) Uani 1 1 d .
C2B C 0.7630(5) 0.7806(6) 0.8215(4) 0.052(2) Uani 1 1 d .
H2BA H 0.7932 0.8188 0.8079 0.062 Uiso 1 1 calc R
C3B C 0.7782(7) 0.7082(6) 0.8082(4) 0.064(3) Uani 1 1 d .
H3BA H 0.8184 0.6977 0.7858 0.077 Uiso 1 1 calc R
C4B C 0.7358(8) 0.6514(7) 0.8271(6) 0.089(4) Uani 1 1 d .
H4BA H 0.7463 0.6017 0.8181 0.107 Uiso 1 1 calc R
C5B C 0.6772(8) 0.6689(6) 0.8597(6) 0.086(4) Uani 1 1 d .
H5BA H 0.6471 0.6303 0.8728 0.103 Uiso 1 1 calc R
C6B C 0.6611(6) 0.7411(6) 0.8739(5) 0.066(3) Uani 1 1 d .
H6BA H 0.6211 0.7514 0.8966 0.079 Uiso 1 1 calc R
Sb1 Sb 0.5000 0.5000 0.86215(13) 0.0562(7) Uani 0.50 4 d SPD
F1 F 0.5014(8) 0.5954(10) 0.8566(10) 0.145(8) Uani 0.50 1 d PDU
F2 F 0.5000 0.5000 0.7957(10) 0.31(3) Uani 0.50 4 d SPDU
F3 F 0.5000 0.5000 0.9282(10) 0.22(2) Uani 0.50 4 d SPDU
Sb2 Sb 0.0000 0.0000 0.0000 0.0465(4) Uani 1 8 d S
F4 F 0.1002(5) 0.0150(6) 0.0000 0.115(4) Uani 1 2 d S
F5 F 0.0000 0.0000 0.0719(6) 0.174(9) Uani 1 4 d S
Cl2B Cl 0.7612(8) 0.4577(7) 1.0000 0.277(7) Uani 1 2 d SD
Cl2A Cl 0.7161(10) 0.5961(17) 1.0000 0.443(15) Uani 1 2 d SD
C100 C 0.739(2) 0.5274(12) 0.9500(16) 0.134(13) Uiso 0.50 1 d PD
H10A H 0.7814 0.5414 0.9281 0.161 Uiso 0.50 1 calc PR
H10B H 0.6960 0.5136 0.9280 0.161 Uiso 0.50 1 calc PR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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_1
_geom_angle_site_symmetry_3
P1 Au1 Cl1 174.95(8) . .
P1 Au1 Ag1 127.08(6) . .
Cl1 Au1 Ag1 53.66(6) . .
Cl1 Ag1 Cl1 115.00(5) 2_675 15_466
Cl1 Ag1 Cl1 98.90(9) 2_675 .
Cl1 Ag1 Cl1 115.00(5) 15_466 .
Cl1 Ag1 Cl1 115.00(5) 2_675 16_656
Cl1 Ag1 Cl1 98.90(9) 15_466 16_656
Cl1 Ag1 Cl1 115.00(5) . 16_656
Cl1 Ag1 Au1 160.16(5) 2_675 15_466
Cl1 Ag1 Au1 45.25(5) 15_466 15_466
Cl1 Ag1 Au1 93.48(5) . 15_466
Cl1 Ag1 Au1 72.70(5) 16_656 15_466
Cl1 Ag1 Au1 93.48(5) 2_675 16_656
Cl1 Ag1 Au1 72.70(5) 15_466 16_656
Cl1 Ag1 Au1 160.16(5) . 16_656
Cl1 Ag1 Au1 45.25(5) 16_656 16_656
Au1 Ag1 Au1 79.256(15) 15_466 16_656
Cl1 Ag1 Au1 45.25(5) 2_675 2_675
Cl1 Ag1 Au1 93.48(5) 15_466 2_675
Cl1 Ag1 Au1 72.70(5) . 2_675
Cl1 Ag1 Au1 160.16(5) 16_656 2_675
Au1 Ag1 Au1 126.385(9) 15_466 2_675
Au1 Ag1 Au1 126.385(9) 16_656 2_675
Cl1 Ag1 Au1 72.70(5) 2_675 .
Cl1 Ag1 Au1 160.16(5) 15_466 .
Cl1 Ag1 Au1 45.25(5) . .
Cl1 Ag1 Au1 93.48(5) 16_656 .
Au1 Ag1 Au1 126.385(9) 15_466 .
Au1 Ag1 Au1 126.385(9) 16_656 .
Au1 Ag1 Au1 79.256(15) 2_675 .
Au1 Cl1 Ag1 81.08(7) . .
C1A P1 C1B 108.5(4) . .
C1A P1 C4 106.1(4) . .
C1B P1 C4 109.2(4) . .
C1A P1 Au1 113.8(3) . .
C1B P1 Au1 103.2(3) . .
C4 P1 Au1 115.8(3) . .
C2 C1 C1 121.2(6) . 10_557
C1 C2 C3 120.2(8) . .
C4 C3 C2 121.8(7) . .
C4 C3 C3 119.6(4) . 10_557
C2 C3 C3 118.5(5) . 10_557
C3 C4 C5 119.4(7) . .
C3 C4 P1 118.0(6) . .
C5 C4 P1 122.5(6) . .
C4 C5 C5 119.8(4) . 10_557
C4 C5 C6 123.3(7) . .
C5 C5 C6 116.8(5) 10_557 .
C7 C6 C5 123.6(8) . .
C6 C7 C7 119.6(5) . 10_557
C6A C1A C2A 119.7(8) . .
C6A C1A P1 119.7(7) . .
C2A C1A P1 120.6(7) . .
C3A C2A C1A 118.5(9) . .
C4A C3A C2A 120.3(10) . .
C5A C4A C3A 119.8(9) . .
C6A C5A C4A 120.6(9) . .
C5A C6A C1A 121.0(9) . .
C2B C1B C6B 118.2(9) . .
C2B C1B P1 123.8(7) . .
C6B C1B P1 117.9(8) . .
C3B C2B C1B 121.4(10) . .
C4B C3B C2B 121.0(11) . .
C3B C4B C5B 117.9(11) . .
C6B C5B C4B 122.2(12) . .
C5B C6B C1B 119.2(11) . .
F3 Sb1 F2 180.000(13) . .
F3 Sb1 F1 94.7(8) . 2_665
F2 Sb1 F1 85.3(8) . 2_665
F3 Sb1 F1 94.7(8) . 3_655
F2 Sb1 F1 85.3(8) . 3_655
F1 Sb1 F1 89.62(14) 2_665 3_655
F3 Sb1 F1 94.7(8) . 4_565
F2 Sb1 F1 85.3(8) . 4_565
F1 Sb1 F1 89.62(14) 2_665 4_565
F1 Sb1 F1 170.6(17) 3_655 4_565
F3 Sb1 F1 94.7(8) . .
F2 Sb1 F1 85.3(8) . .
F1 Sb1 F1 170.6(17) 2_665 .
F1 Sb1 F1 89.62(14) 3_655 .
F1 Sb1 F1 89.62(14) 4_565 .
F4 Sb2 F4 180.0(7) 9 .
F4 Sb2 F4 90.0 9 3
F4 Sb2 F4 90.0 . 3
F4 Sb2 F4 90.0 9 11
F4 Sb2 F4 90.0 . 11
F4 Sb2 F4 180.0 3 11
F4 Sb2 F5 90.0 9 9
F4 Sb2 F5 90.0 . 9
F4 Sb2 F5 90.0 3 9
F4 Sb2 F5 90.0 11 9
F4 Sb2 F5 90.0 9 .
F4 Sb2 F5 90.0 . .
F4 Sb2 F5 90.0 3 .
F4 Sb2 F5 90.0 11 .
F5 Sb2 F5 180.0 9 .
C100 Cl2B C100 88(2) 10_557 .
C100 Cl2A C100 89(2) . 10_557
Cl2A C100 Cl2B 92(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Au1 P1 2.241(2) .
Au1 Cl1 2.313(2) .
Au1 Ag1 3.2180(4) .
Ag1 Cl1 2.624(2) 2_675
Ag1 Cl1 2.624(2) 15_466
Ag1 Cl1 2.624(2) .
Ag1 Cl1 2.624(2) 16_656
Ag1 Au1 3.2180(4) 15_466
Ag1 Au1 3.2180(4) 16_656
Ag1 Au1 3.2180(4) 2_675
P1 C1A 1.805(9) .
P1 C1B 1.810(9) .
P1 C4 1.844(8) .
C1 C2 1.366(13) .
C1 C1 1.37(2) 10_557
C2 C3 1.416(11) .
C3 C4 1.404(10) .
C3 C3 1.437(15) 10_557
C4 C5 1.407(11) .
C5 C5 1.427(15) 10_557
C5 C6 1.437(11) .
C6 C7 1.352(12) .
C7 C7 1.384(19) 10_557
C1A C6A 1.390(11) .
C1A C2A 1.405(12) .
C2A C3A 1.404(13) .
C3A C4A 1.394(14) .
C4A C5A 1.375(14) .
C5A C6A 1.363(12) .
C1B C2B 1.377(13) .
C1B C6B 1.385(14) .
C2B C3B 1.369(13) .
C3B C4B 1.360(16) .
C4B C5B 1.376(19) .
C5B C6B 1.376(15) .
Sb1 F3 1.68(3) .
Sb1 F2 1.69(3) .
Sb1 F1 1.719(18) 2_665
Sb1 F1 1.719(18) 3_655
Sb1 F1 1.719(19) 4_565
Sb1 F1 1.719(18) .
Sb2 F4 1.819(10) 9
Sb2 F4 1.819(10) .
Sb2 F4 1.819(10) 3
Sb2 F4 1.819(10) 11
Sb2 F5 1.826(16) 9
Sb2 F5 1.826(16) .
Cl2B C100 1.83(3) 10_557
Cl2B C100 1.83(3) .
Cl2A C100 1.82(3) .
Cl2A C100 1.82(3) 10_557
