#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/41/7014185.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_7014185
loop_
_publ_author_name
'Schneider, Daniel'
'Schier, Annette'
'Schmidbaur, Hubert'
_publ_section_title
;
 Governing the oxidative addition of iodine to gold(I) complexes by
 ligand tuning.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1995
_journal_page_last               2005
_journal_paper_doi               10.1039/b403005b
_journal_year                    2004
_chemical_formula_moiety         '[(Me2PhP)AuI30.75CH2Cl2]'
_chemical_formula_sum            'C8.75 H12.5 Au Cl1.5 I3 P'
_chemical_formula_weight         779.50
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 116.494(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   35.9785(4)
_cell_length_b                   8.3066(1)
_cell_length_c                   25.1157(4)
_cell_measurement_reflns_used    101645
_cell_measurement_temperature    143(2)
_cell_volume                     6717.78(16)
_computing_cell_refinement       HKL2000
_computing_data_collection       XPRESS
_computing_data_reduction        HKL2000
_computing_molecular_graphics    SHELXTL-PLUS
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Nonius DIP 2020 HU'
_diffrn_measurement_method       phi-rotation
_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  0.057
_diffrn_reflns_av_sigmaI/netI    0.064
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            101645
_diffrn_reflns_theta_full        27.29
_diffrn_reflns_theta_max         27.29
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    14.582
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_type   DEABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5496
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.499
_refine_diff_density_min         -3.515
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         7357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0053P)²+116.6794P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                7281
_reflns_number_total             7357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b403005b.txt
_cod_data_source_block           '[(Me2PhP)AuI30.75CH2Cl2]'
_cod_original_cell_volume        6717.77(15)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C8.75 H12.50 Au Cl1.50 I3 P'
_cod_database_code               7014185
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.215719(7) 0.86197(3) 0.162299(11) 0.02132(7) Uani 1 1 d . . .
Au2 Au 0.367449(8) 0.81600(3) 0.122606(11) 0.02281(7) Uani 1 1 d . . .
I1 I 0.213405(16) 1.14180(6) 0.11251(2) 0.03213(11) Uani 1 1 d . . .
I2 I 0.277530(15) 0.77207(7) 0.13885(2) 0.03326(12) Uani 1 1 d . . .
I3 I 0.211829(15) 0.56597(6) 0.19598(2) 0.03184(11) Uani 1 1 d . . .
I4 I 0.408987(14) 0.56660(6) 0.18791(2) 0.03012(11) Uani 1 1 d . . .
I5 I 0.338172(16) 0.63029(6) 0.02824(2) 0.03049(11) Uani 1 1 d . . .
I6 I 0.39900(2) 0.99130(8) 0.21968(3) 0.05073(17) Uani 1 1 d . . .
P1 P 0.16241(5) 0.9323(2) 0.18736(8) 0.0228(3) Uani 1 1 d . . .
P2 P 0.33491(6) 1.0387(2) 0.06246(8) 0.0253(3) Uani 1 1 d . . .
C11 C 0.1533(3) 1.1453(9) 0.1897(4) 0.0333(16) Uani 1 1 d . . .
H11A H 0.1306 1.1619 0.2006 0.050 Uiso 1 1 calc R . .
H11B H 0.1459 1.1927 0.1506 0.050 Uiso 1 1 calc R . .
H11C H 0.1786 1.1968 0.2194 0.050 Uiso 1 1 calc R . .
C12 C 0.1714(2) 0.8608(10) 0.2594(3) 0.0299(15) Uani 1 1 d . . .
H12A H 0.1482 0.8933 0.2676 0.045 Uiso 1 1 calc R . .
H12B H 0.1973 0.9069 0.2896 0.045 Uiso 1 1 calc R . .
H12C H 0.1735 0.7431 0.2604 0.045 Uiso 1 1 calc R . .
C21 C 0.2840(2) 1.0022(10) 0.0022(4) 0.0342(16) Uani 1 1 d . . .
H21A H 0.2731 1.1022 -0.0201 0.051 Uiso 1 1 calc R . .
H21B H 0.2653 0.9648 0.0185 0.051 Uiso 1 1 calc R . .
H21C H 0.2860 0.9199 -0.0243 0.051 Uiso 1 1 calc R . .
C22 C 0.3257(2) 1.2073(9) 0.0996(4) 0.0325(16) Uani 1 1 d . . .
H22A H 0.3121 1.2934 0.0707 0.049 Uiso 1 1 calc R . .
H22B H 0.3522 1.2465 0.1306 0.049 Uiso 1 1 calc R . .
H22C H 0.3078 1.1740 0.1177 0.049 Uiso 1 1 calc R . .
C111 C 0.1149(2) 0.8491(9) 0.1316(3) 0.0263(14) Uani 1 1 d . . .
C112 C 0.0897(2) 0.7479(11) 0.1456(4) 0.0373(18) Uani 1 1 d . . .
H11D H 0.0976 0.7195 0.1859 0.045 Uiso 1 1 calc R . .
C113 C 0.0529(3) 0.6884(12) 0.1006(4) 0.046(2) Uani 1 1 d . . .
H11E H 0.0356 0.6200 0.1103 0.055 Uiso 1 1 calc R . .
C114 C 0.0414(2) 0.7283(11) 0.0420(4) 0.0416(19) Uani 1 1 d . . .
H11F H 0.0163 0.6870 0.0114 0.050 Uiso 1 1 calc R . .
C115 C 0.0661(3) 0.8275(12) 0.0278(4) 0.046(2) Uani 1 1 d . . .
H11G H 0.0582 0.8551 -0.0126 0.055 Uiso 1 1 calc R . .
C116 C 0.1028(2) 0.8878(11) 0.0726(4) 0.0359(17) Uani 1 1 d . . .
H11H H 0.1198 0.9565 0.0626 0.043 Uiso 1 1 calc R . .
C211 C 0.3688(2) 1.1045(9) 0.0308(3) 0.0290(15) Uani 1 1 d . . .
C212 C 0.3639(3) 1.0408(10) -0.0231(3) 0.0354(17) Uani 1 1 d . . .
H21D H 0.3426 0.9646 -0.0436 0.042 Uiso 1 1 calc R . .
C213 C 0.3902(3) 1.0889(11) -0.0467(4) 0.0409(19) Uani 1 1 d . . .
H21E H 0.3867 1.0468 -0.0839 0.049 Uiso 1 1 calc R . .
C214 C 0.4215(3) 1.1982(12) -0.0166(4) 0.045(2) Uani 1 1 d . . .
H21F H 0.4396 1.2298 -0.0330 0.054 Uiso 1 1 calc R . .
C215 C 0.4270(2) 1.2624(12) 0.0375(4) 0.042(2) Uani 1 1 d . . .
H21G H 0.4486 1.3372 0.0581 0.051 Uiso 1 1 calc R . .
C216 C 0.4000(2) 1.2154(10) 0.0613(4) 0.0354(17) Uani 1 1 d . . .
H21I H 0.4031 1.2591 0.0980 0.043 Uiso 1 1 calc R . .
C1 C 0.0000 0.689(2) 0.2500 0.088(7) Uani 1 2 d S . .
H1A H 0.0233 0.6235 0.2723 0.106 Uiso 1 1 d . . .
C2 C -0.0037(3) 0.7688(12) -0.1595(4) 0.043(2) Uani 1 1 d . . .
H2A H -0.0251 0.7296 -0.1984 0.052 Uiso 1 1 calc R . .
H2B H 0.0138 0.8481 -0.1674 0.052 Uiso 1 1 calc R . .
Cl11 Cl 0.01075(8) 0.8026(3) 0.20004(10) 0.0486(5) Uani 1 1 d . . .
Cl21 Cl -0.02856(8) 0.8658(3) -0.12114(11) 0.0543(6) Uani 1 1 d . . .
Cl22 Cl 0.02710(7) 0.6076(3) -0.11997(11) 0.0473(5) 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 0.0033 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
P1 Au1 I1 92.95(5) . . ?
P1 Au1 I3 88.81(5) . . ?
I1 Au1 I3 171.507(19) . . ?
P1 Au1 I2 176.98(5) . . ?
I1 Au1 I2 89.718(17) . . ?
I3 Au1 I2 88.757(17) . . ?
P2 Au2 I5 89.88(5) . . ?
P2 Au2 I6 92.61(5) . . ?
I5 Au2 I6 177.43(2) . . ?
P2 Au2 I4 175.44(5) . . ?
I5 Au2 I4 89.297(17) . . ?
I6 Au2 I4 88.167(19) . . ?
C12 P1 C111 109.8(3) . . ?
C12 P1 C11 104.2(4) . . ?
C111 P1 C11 106.3(4) . . ?
C12 P1 Au1 112.9(3) . . ?
C111 P1 Au1 107.6(2) . . ?
C11 P1 Au1 115.8(3) . . ?
C22 P2 C21 102.3(4) . . ?
C22 P2 C211 108.0(4) . . ?
C21 P2 C211 108.3(4) . . ?
C22 P2 Au2 115.9(3) . . ?
C21 P2 Au2 115.8(3) . . ?
C211 P2 Au2 106.3(2) . . ?
P1 C11 H11A 109.5 . . ?
P1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
P1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
P1 C12 H12A 109.5 . . ?
P1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
P1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
P2 C21 H21A 109.5 . . ?
P2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
P2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
P2 C22 H22A 109.5 . . ?
P2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
P2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C116 C111 C112 118.9(7) . . ?
C116 C111 P1 118.7(6) . . ?
C112 C111 P1 122.4(6) . . ?
C111 C112 C113 120.0(8) . . ?
C111 C112 H11D 120.0 . . ?
C113 C112 H11D 120.0 . . ?
C114 C113 C112 120.2(8) . . ?
C114 C113 H11E 119.9 . . ?
C112 C113 H11E 119.9 . . ?
C115 C114 C113 120.1(8) . . ?
C115 C114 H11F 119.9 . . ?
C113 C114 H11F 119.9 . . ?
C114 C115 C116 119.8(8) . . ?
C114 C115 H11G 120.1 . . ?
C116 C115 H11G 120.1 . . ?
C111 C116 C115 121.0(8) . . ?
C111 C116 H11H 119.5 . . ?
C115 C116 H11H 119.5 . . ?
C216 C211 C212 120.6(7) . . ?
C216 C211 P2 119.8(6) . . ?
C212 C211 P2 119.7(6) . . ?
C213 C212 C211 119.7(8) . . ?
C213 C212 H21D 120.2 . . ?
C211 C212 H21D 120.2 . . ?
C214 C213 C212 120.2(8) . . ?
C214 C213 H21E 119.9 . . ?
C212 C213 H21E 119.9 . . ?
C213 C214 C215 120.8(8) . . ?
C213 C214 H21F 119.6 . . ?
C215 C214 H21F 119.6 . . ?
C214 C215 C216 119.2(8) . . ?
C214 C215 H21G 120.4 . . ?
C216 C215 H21G 120.4 . . ?
C211 C216 C215 119.6(8) . . ?
C211 C216 H21I 120.2 . . ?
C215 C216 H21I 120.2 . . ?
Cl11 C1 Cl11 114.5(10) . 2 ?
Cl11 C1 H1A 108.3 . . ?
Cl11 C1 H1A 108.0 2 . ?
Cl22 C2 Cl21 112.7(5) . . ?
Cl22 C2 H2A 109.0 . . ?
Cl21 C2 H2A 109.0 . . ?
Cl22 C2 H2B 109.0 . . ?
Cl21 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 P1 2.3439(17) . ?
Au1 I1 2.6231(5) . ?
Au1 I3 2.6242(5) . ?
Au1 I2 2.6493(5) . ?
Au2 P2 2.3445(18) . ?
Au2 I5 2.6228(5) . ?
Au2 I6 2.6236(6) . ?
Au2 I4 2.6511(5) . ?
P1 C12 1.791(7) . ?
P1 C111 1.796(7) . ?
P1 C11 1.805(8) . ?
P2 C22 1.793(8) . ?
P2 C21 1.806(8) . ?
P2 C211 1.812(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C111 C116 1.383(11) . ?
C111 C112 1.392(10) . ?
C112 C113 1.393(12) . ?
C112 H11D 0.9500 . ?
C113 C114 1.381(13) . ?
C113 H11E 0.9500 . ?
C114 C115 1.371(13) . ?
C114 H11F 0.9500 . ?
C115 C116 1.392(11) . ?
C115 H11G 0.9500 . ?
C116 H11H 0.9500 . ?
C211 C216 1.389(11) . ?
C211 C212 1.390(11) . ?
C212 C213 1.380(12) . ?
C212 H21D 0.9500 . ?
C213 C214 1.382(14) . ?
C213 H21E 0.9500 . ?
C214 C215 1.390(13) . ?
C214 H21F 0.9500 . ?
C215 C216 1.402(11) . ?
C215 H21G 0.9500 . ?
C216 H21I 0.9500 . ?
C1 Cl11 1.746(10) . ?
C1 Cl11 1.746(10) 2 ?
C1 H1A 0.9454 . ?
C2 Cl22 1.740(9) . ?
C2 Cl21 1.774(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
I1 Au1 P1 C12 -140.3(3) . . . . ?
I3 Au1 P1 C12 48.0(3) . . . . ?
I2 Au1 P1 C12 11.6(10) . . . . ?
I1 Au1 P1 C111 98.3(3) . . . . ?
I3 Au1 P1 C111 -73.4(3) . . . . ?
I2 Au1 P1 C111 -109.8(9) . . . . ?
I1 Au1 P1 C11 -20.4(3) . . . . ?
I3 Au1 P1 C11 167.9(3) . . . . ?
I2 Au1 P1 C11 131.6(9) . . . . ?
I5 Au2 P2 C22 158.5(3) . . . . ?
I6 Au2 P2 C22 -22.1(3) . . . . ?
I4 Au2 P2 C22 -121.9(6) . . . . ?
I5 Au2 P2 C21 38.7(3) . . . . ?
I6 Au2 P2 C21 -142.0(3) . . . . ?
I4 Au2 P2 C21 118.3(6) . . . . ?
I5 Au2 P2 C211 -81.6(3) . . . . ?
I6 Au2 P2 C211 97.8(3) . . . . ?
I4 Au2 P2 C211 -1.9(7) . . . . ?
C12 P1 C111 C116 -178.9(6) . . . . ?
C11 P1 C111 C116 69.0(7) . . . . ?
Au1 P1 C111 C116 -55.6(7) . . . . ?
C12 P1 C111 C112 1.5(8) . . . . ?
C11 P1 C111 C112 -110.6(7) . . . . ?
Au1 P1 C111 C112 124.8(6) . . . . ?
C116 C111 C112 C113 -0.4(13) . . . . ?
P1 C111 C112 C113 179.2(7) . . . . ?
C111 C112 C113 C114 0.5(14) . . . . ?
C112 C113 C114 C115 -0.3(14) . . . . ?
C113 C114 C115 C116 0.1(15) . . . . ?
C112 C111 C116 C115 0.2(13) . . . . ?
P1 C111 C116 C115 -179.5(7) . . . . ?
C114 C115 C116 C111 0.0(15) . . . . ?
C22 P2 C211 C216 36.2(7) . . . . ?
C21 P2 C211 C216 146.3(6) . . . . ?
Au2 P2 C211 C216 -88.7(6) . . . . ?
C22 P2 C211 C212 -145.1(6) . . . . ?
C21 P2 C211 C212 -35.1(7) . . . . ?
Au2 P2 C211 C212 89.9(6) . . . . ?
C216 C211 C212 C213 -0.3(12) . . . . ?
P2 C211 C212 C213 -179.0(6) . . . . ?
C211 C212 C213 C214 0.9(12) . . . . ?
C212 C213 C214 C215 -0.6(13) . . . . ?
C213 C214 C215 C216 -0.2(13) . . . . ?
C212 C211 C216 C215 -0.5(12) . . . . ?
P2 C211 C216 C215 178.2(6) . . . . ?
C214 C215 C216 C211 0.7(13) . . . . ?
