#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/68/4106808.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_4106808
loop_
_publ_author_name
'Tom Hasell'
'Marc Schmidtmann'
'Andrew I. Cooper'
_publ_section_title
;
 Molecular Doping of Porous Organic Cages
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14920
_journal_page_last               14923
_journal_paper_doi               10.1021/ja205969q
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration syn
_chemical_formula_sum            'C72 H84 I4.5 N12'
_chemical_formula_weight         1688.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           210
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'F 4d 2 3'
_symmetry_space_group_name_H-M   'F 41 3 2'
_atom_sites_solution_hydrogens   difmap
_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            8
_cell_length_a                   24.9673(18)
_cell_length_b                   24.9673(18)
_cell_length_c                   24.9673(18)
_cell_measurement_reflns_used    978
_cell_measurement_temperature    318(2)
_cell_measurement_theta_max      20.80
_cell_measurement_theta_min      2.52
_cell_volume                     15563.8(19)
_computing_cell_refinement       'Bruker AXS SAINT V7.68A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker AXS SAINT V7.68A'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      318(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_source         Synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8285
_diffrn_reflns_theta_full        25.47
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    2.179
_exptl_absorpt_correction_T_max  0.4902
_exptl_absorpt_correction_T_min  0.4176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_F_000             6708
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0900P)²+55.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1932
_refine_ls_wR_factor_ref         0.2179
_reflns_number_gt                636
_reflns_number_total             941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja205969q_si_004.cif
_cod_data_source_block           egc020318k
_cod_original_formula_sum        'C72 H84 I4.50 N12'
_cod_database_code               4106808
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z'
'x+1/2, -y, -z+1/2'
'z, x, y'
'z+1/2, -x, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y'
'y, z, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z, -x+1/2'
'-y, -z+1/2, x+1/2'
'y+3/4, x+1/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'y+1/4, -x+3/4, z+3/4'
'-y+3/4, x+3/4, z+1/4'
'x+3/4, z+1/4, -y+3/4'
'-x+3/4, z+3/4, y+1/4'
'-x+1/4, -z+1/4, -y+1/4'
'x+1/4, -z+3/4, y+3/4'
'z+3/4, y+1/4, -x+3/4'
'z+1/4, -y+3/4, x+3/4'
'-z+3/4, y+3/4, x+1/4'
'-z+1/4, -y+1/4, -x+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1, z+1'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'z, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1'
'-z, -x+1, y+1'
'-z+1/2, x+1, -y+1/2'
'y, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1/2'
'y+1/2, -z+1/2, -x+1'
'-y, -z+1, x+1'
'y+3/4, x+3/4, -z+5/4'
'-y+1/4, -x+3/4, -z+3/4'
'y+1/4, -x+5/4, z+5/4'
'-y+3/4, x+5/4, z+3/4'
'x+3/4, z+3/4, -y+5/4'
'-x+3/4, z+5/4, y+3/4'
'-x+1/4, -z+3/4, -y+3/4'
'x+1/4, -z+5/4, y+5/4'
'z+3/4, y+3/4, -x+5/4'
'z+1/4, -y+5/4, x+5/4'
'-z+3/4, y+5/4, x+3/4'
'-z+1/4, -y+3/4, -x+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y+1/2, z+1'
'-x+1, y+1/2, -z+1/2'
'x+1, -y, -z+1'
'z+1/2, x, y+1/2'
'z+1, -x, -y+1'
'-z+1/2, -x+1/2, y+1'
'-z+1, x+1/2, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1, z+1/2, -x+1/2'
'y+1, -z, -x+1'
'-y+1/2, -z+1/2, x+1'
'y+5/4, x+1/4, -z+5/4'
'-y+3/4, -x+1/4, -z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-y+5/4, x+3/4, z+3/4'
'x+5/4, z+1/4, -y+5/4'
'-x+5/4, z+3/4, y+3/4'
'-x+3/4, -z+1/4, -y+3/4'
'x+3/4, -z+3/4, y+5/4'
'z+5/4, y+1/4, -x+5/4'
'z+3/4, -y+3/4, x+5/4'
'-z+5/4, y+3/4, x+3/4'
'-z+3/4, -y+1/4, -x+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1, y+1, -z'
'x+1, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y'
'z+1, -x+1/2, -y+1/2'
'-z+1/2, -x+1, y+1/2'
'-z+1, x+1, -y'
'y+1/2, z+1/2, x'
'-y+1, z+1, -x'
'y+1, -z+1/2, -x+1/2'
'-y+1/2, -z+1, x+1/2'
'y+5/4, x+3/4, -z+3/4'
'-y+3/4, -x+3/4, -z+1/4'
'y+3/4, -x+5/4, z+3/4'
'-y+5/4, x+5/4, z+1/4'
'x+5/4, z+3/4, -y+3/4'
'-x+5/4, z+5/4, y+1/4'
'-x+3/4, -z+3/4, -y+1/4'
'x+3/4, -z+5/4, y+3/4'
'z+5/4, y+3/4, -x+3/4'
'z+3/4, -y+5/4, x+3/4'
'-z+5/4, y+5/4, x+1/4'
'-z+3/4, -y+3/4, -x+1/4'
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
N1 N 0.0459(3) 0.7772(2) 0.0363(3) 0.0990(19) Uani 1 1 d .
C1 C 0.1127(3) 0.8695(3) 0.0555(3) 0.090(2) Uani 1 1 d .
H1 H 0.1213 0.8489 0.0257 0.108 Uiso 1 1 calc R
C2 C 0.0684(3) 0.8559(3) 0.0865(3) 0.088(2) Uani 1 1 d .
C3 C 0.0343(3) 0.8097(3) 0.0724(3) 0.096(2) Uani 1 1 d .
H3 H 0.0026 0.8046 0.0913 0.115 Uiso 1 1 calc R
C4 C 0.0103(3) 0.7310(2) 0.0284(3) 0.092(2) Uani 1 1 d .
H4 H -0.0200 0.7334 0.0533 0.110 Uiso 1 1 calc R
C5 C 0.0419(4) 0.6803(3) 0.0398(4) 0.142(3) Uani 1 1 d .
H5A H 0.0533 0.6802 0.0769 0.170 Uiso 1 1 calc R
H5B H 0.0737 0.6796 0.0174 0.170 Uiso 1 1 calc R
C6 C 0.0080(7) 0.6301(3) 0.0287(4) 0.183(7) Uani 1 1 d .
H6A H 0.0285 0.5982 0.0367 0.219 Uiso 1 1 calc R
H6B H -0.0237 0.6303 0.0512 0.219 Uiso 1 1 calc R
I1 I -0.1250 0.8750 0.1250 0.216(2) Uani 0.894(9) 6 d SP
I2 I -0.06518(10) 0.93482(10) 0.06518(10) 0.1663(19) Uani 0.449(5) 3 d SP
I3 I -0.01468(15) 0.98532(15) 0.01468(15) 0.189(5) Uani 0.219(4) 3 d SP
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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'
N N 0.0080 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3150 2.1150 '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
C3 N1 C4 117.9(7) . .
C2 C1 C2 120.8(8) 36_654 .
C2 C1 H1 119.6 36_654 .
C2 C1 H1 119.6 . .
C1 C2 C1 119.2(8) 54_465 .
C1 C2 C3 119.8(7) 54_465 .
C1 C2 C3 121.0(7) . .
N1 C3 C2 123.2(7) . .
N1 C3 H3 118.4 . .
C2 C3 H3 118.4 . .
N1 C4 C4 109.3(5) . 75_445
N1 C4 C5 108.4(7) . .
C4 C4 C5 110.6(5) 75_445 .
N1 C4 H4 109.5 . .
C4 C4 H4 109.5 75_445 .
C5 C4 H4 109.5 . .
C4 C5 C6 111.0(9) . .
C4 C5 H5A 109.4 . .
C6 C5 H5A 109.4 . .
C4 C5 H5B 109.4 . .
C6 C5 H5B 109.4 . .
H5A C5 H5B 108.0 . .
C6 C6 C5 108.7(8) 75_445 .
C6 C6 H6A 109.9 75_445 .
C5 C6 H6A 109.9 . .
C6 C6 H6B 109.9 75_445 .
C5 C6 H6B 109.9 . .
H6A C6 H6B 108.3 . .
I2 I1 I2 180.000(1) . 86
I3 I2 I1 180.0(3) . .
I3 I2 I3 11.17(10) . 26_564
I1 I2 I3 168.83(10) . 26_564
I3 I2 I3 11.17(10) . 52_474
I1 I2 I3 168.83(10) . 52_474
I3 I2 I3 19.32(18) 26_564 52_474
I3 I2 I3 11.17(10) . 75_445
I1 I2 I3 168.83(10) . 75_445
I3 I2 I3 19.32(18) 26_564 75_445
I3 I2 I3 19.32(18) 52_474 75_445
I3 I3 I3 60.003(1) 26_564 52_474
I3 I3 I3 60.0 26_564 75_445
I3 I3 I3 60.0 52_474 75_445
I3 I3 I2 144.734(1) 26_564 .
I3 I3 I2 144.734(2) 52_474 .
I3 I3 I2 144.734(1) 75_445 .
I3 I3 I2 24.09(10) 26_564 26_564
I3 I3 I2 80.34(9) 52_474 26_564
I3 I3 I2 80.34(9) 75_445 26_564
I2 I3 I2 120.64(10) . 26_564
I3 I3 I2 80.34(9) 26_564 52_474
I3 I3 I2 24.09(11) 52_474 52_474
I3 I3 I2 80.34(9) 75_445 52_474
I2 I3 I2 120.64(10) . 52_474
I2 I3 I2 96.34(13) 26_564 52_474
I3 I3 I2 80.34(9) 26_564 75_445
I3 I3 I2 80.34(9) 52_474 75_445
I3 I3 I2 24.09(10) 75_445 75_445
I2 I3 I2 120.64(10) . 75_445
I2 I3 I2 96.34(13) 26_564 75_445
I2 I3 I2 96.34(13) 52_474 75_445
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C3 1.246(9) .
N1 C4 1.469(8) .
C1 C2 1.388(8) 36_654
C1 C2 1.392(9) .
C1 H1 0.9300 .
C2 C1 1.388(8) 54_465
C2 C3 1.477(10) .
C3 H3 0.9300 .
C4 C4 1.509(14) 75_445
C4 C5 1.519(10) .
C4 H4 0.9800 .
C5 C6 1.536(15) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 C6 1.49(2) 75_445
C6 H6A 0.9700 .
C6 H6B 0.9700 .
I1 I2 2.587(4) .
I1 I2 2.587(4) 86
I2 I3 2.184(7) .
I2 I3 3.089(6) 26_564
I2 I3 3.089(6) 52_474
I2 I3 3.089(6) 75_445
I3 I3 1.036(10) 26_564
I3 I3 1.036(10) 52_474
I3 I3 1.036(10) 75_445
I3 I2 3.089(6) 26_564
I3 I2 3.089(6) 52_474
I3 I2 3.089(6) 75_445
