#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:49:05 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179457 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/54/4335433.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_4335433
loop_
_publ_author_name
'Sang Ho Lim'
'Seth M. Cohen'
_publ_section_title
;
 Self-Assembled Supramolecular Clusters Based on Phosphines and Coinage
 Metals: Tetrahedra, Helicates, and Mesocates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7862
_journal_page_last               7872
_journal_paper_doi               10.1021/ic302840x
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C99 H69 Au2 I2 N3 P6, 3(C H2 Cl)'
_chemical_formula_sum            'C102 H75 Au2 Cl3 I2 N3 P6'
_chemical_formula_weight         2282.55
_chemical_name_common            '[Au2(2,6-dppeb)3]I2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           190
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   13.3154(9)
_cell_length_b                   13.3154(9)
_cell_length_c                   38.938(3)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.63
_cell_measurement_theta_min      29.21
_cell_volume                     5978.8(7)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            3498
_diffrn_reflns_theta_full        66.67
_diffrn_reflns_theta_max         66.67
_diffrn_reflns_theta_min         3.83
_exptl_absorpt_coefficient_mu    10.267
_exptl_absorpt_correction_T_max  0.323
_exptl_absorpt_correction_T_min  0.174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       plate
_exptl_crystal_F_000             2226
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_platon_squeeze_details
;
;
_refine_diff_density_max         5.396
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.249
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         3498
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0852
_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)+(0.1688P)²+24.5321P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2364
_refine_ls_wR_factor_ref         0.2390
_reflns_number_gt                3354
_reflns_number_total             3498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302840x_si_002_08.cif
_cod_data_source_block           '[Au2[2,6-dppeb]3]I2'
_cod_original_cell_volume        5978.9(7)
_cod_original_sg_symbol_H-M      'P -6 2 c '
_cod_database_code               4335433
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+y, -x, -z+1/2'
'-y, x-y, z'
'x, y, -z+1/2'
'-x+y, -x, z'
'-y, x-y, -z+1/2'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, 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 0.6667 0.3333 0.595912(14) 0.0425(3) Uani 1 3 d S . .
I2 I 0.6667 0.3333 0.52421(3) 0.0700(4) Uani 1 3 d S . .
P2 P 0.8223(3) 0.3111(2) 0.61660(6) 0.0418(6) Uani 1 1 d . B .
C2 C 0.8850(12) 0.4608(14) 0.7188(2) 0.061(4) Uani 1 1 d . . .
N3 N 0.8588(14) 0.3991(16) 0.7500 0.069(5) Uani 1 2 d S . .
C6 C 0.8701(11) 0.4113(12) 0.6865(3) 0.063(4) Uani 1 1 d . . .
C5 C 0.9650(7) 0.3918(10) 0.5956(3) 0.0815(12) Uani 1 1 d G . .
C3 C 1.0662(9) 0.4442(10) 0.6150(2) 0.0815(12) Uani 1 1 d G . .
H3 H 1.0621 0.4415 0.6393 0.098 Uiso 1 1 calc R . .
C18 C 1.1735(7) 0.5005(10) 0.5987(3) 0.0815(12) Uani 1 1 d G . .
H18 H 1.2426 0.5363 0.6119 0.098 Uiso 1 1 calc R . .
C8 C 1.1795(6) 0.5044(10) 0.5630(3) 0.0815(12) Uani 1 1 d G . .
H8 H 1.2528 0.5429 0.5519 0.098 Uiso 1 1 calc R . .
C20 C 1.0783(8) 0.4520(10) 0.5437(2) 0.0815(12) Uani 1 1 d G . .
H20 H 1.0824 0.4547 0.5193 0.098 Uiso 1 1 calc R . .
C16 C 0.9710(7) 0.3957(10) 0.5599(3) 0.0815(12) Uani 1 1 d G . .
H16 H 0.9019 0.3599 0.5467 0.098 Uiso 1 1 calc R . .
C9 C 0.8553(12) 0.3627(12) 0.6594(3) 0.054(3) Uani 1 1 d . . .
C4 C 0.8038(9) 0.1700(7) 0.6208(3) 0.0815(12) Uani 1 1 d G . .
C12 C 0.8624(8) 0.1435(8) 0.6454(2) 0.0815(12) Uani 1 1 d G B .
H12 H 0.9199 0.2033 0.6593 0.098 Uiso 1 1 calc R . .
C13 C 0.8369(9) 0.0295(9) 0.6498(2) 0.0815(12) Uani 1 1 d G B .
H13 H 0.8769 0.0114 0.6667 0.098 Uiso 1 1 calc R . .
C11 C 0.7528(9) -0.0580(7) 0.6295(3) 0.0815(12) Uani 1 1 d G B .
H11 H 0.7353 -0.1359 0.6325 0.098 Uiso 1 1 calc R . .
C14 C 0.6942(8) -0.0315(8) 0.6048(3) 0.0815(12) Uani 1 1 d G B .
H14 H 0.6367 -0.0913 0.5910 0.098 Uiso 1 1 calc R A 1
C10 C 0.7197(9) 0.0825(9) 0.6004(3) 0.0815(12) Uani 1 1 d G B 1
H10 H 0.6796 0.1005 0.5836 0.098 Uiso 1 1 calc R B 1
C1 C 0.9553(19) 0.6416(18) 0.7500 0.063(5) Uani 1 2 d S . .
H1 H 0.9871 0.7233 0.7500 0.075 Uiso 1 2 calc SR . .
C7 C 0.9340(17) 0.5869(18) 0.7214(4) 0.077(5) Uani 1 1 d . . .
H7 H 0.9509 0.6304 0.7007 0.093 Uiso 1 1 calc R . .
Cl1 Cl 0.669(4) 0.7597(15) 0.7145(3) 0.32(2) Uani 0.50 1 d PD . .
C50 C 0.603(5) 0.769(4) 0.7500 0.32(2) Uani 1 2 d SD . .
H50A H 0.6040 0.8435 0.7500 0.378 Uiso 1 2 calc SR . .
H50B H 0.5215 0.7055 0.7500 0.378 Uiso 1 2 calc SR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -4.4197 7.2980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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
P2 Au1 P2 109.13(6) . 5_665
P2 Au1 P2 109.13(6) . 3_655
P2 Au1 P2 109.13(6) 5_665 3_655
P2 Au1 I2 109.81(6) . .
P2 Au1 I2 109.81(6) 5_665 .
P2 Au1 I2 109.81(6) 3_655 .
C9 P2 C4 101.6(6) . .
C9 P2 C5 102.0(6) . .
C4 P2 C5 102.4(6) . .
C9 P2 Au1 109.4(5) . .
C4 P2 Au1 119.6(3) . .
C5 P2 Au1 119.1(4) . .
C6 C2 N3 124.7(15) . .
C6 C2 C7 118.8(12) . .
N3 C2 C7 116.4(12) . .
C2 N3 C2 119.1(18) 4_556 .
C9 C6 C2 176.5(14) . .
C3 C5 C16 120.0 . .
C3 C5 P2 120.7(6) . .
C16 C5 P2 119.3(6) . .
C5 C3 C18 120.0 . .
C8 C18 C3 120.0 . .
C18 C8 C20 120.0 . .
C16 C20 C8 120.0 . .
C20 C16 C5 120.0 . .
C6 C9 P2 167.7(12) . .
C12 C4 C10 120.0 . .
C12 C4 P2 122.2(6) . .
C10 C4 P2 117.5(6) . .
C13 C12 C4 120.0 . .
C12 C13 C11 120.0 . .
C14 C11 C13 120.0 . .
C11 C14 C10 120.0 . .
C14 C10 C4 120.0 . .
C7 C1 C7 121(2) 4_556 .
C1 C7 C2 123.7(16) . .
Cl1 C50 Cl1 112(2) 4_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Au1 P2 2.376(3) .
Au1 P2 2.376(3) 5_665
Au1 P2 2.376(3) 3_655
Au1 I2 2.7919(12) .
P2 C9 1.771(10) .
P2 C4 1.776(8) .
P2 C5 1.842(8) .
C2 C6 1.386(17) .
C2 N3 1.409(15) .
C2 C7 1.47(3) .
N3 C2 1.409(15) 4_556
C6 C9 1.204(17) .
C5 C3 1.3900 .
C5 C16 1.3900 .
C3 C18 1.3900 .
C18 C8 1.3900 .
C8 C20 1.3900 .
C20 C16 1.3900 .
C4 C12 1.3900 .
C4 C10 1.3900 .
C12 C13 1.3900 .
C13 C11 1.3900 .
C11 C14 1.3900 .
C14 C10 1.3900 .
C1 C7 1.28(2) 4_556
C1 C7 1.28(2) .
Cl1 C50 1.672(19) .
C50 Cl1 1.672(19) 4_556
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 536 156 ' '
