#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:34:33 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180268 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/54/7115467.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_7115467
loop_
_publ_author_name
'Marc A. Little'
'Samantha Y. Chong'
'Marc Schmidtmann'
'Tom Hasell'
'Andrew I. Cooper'
_publ_section_title
;
 Guest control of structure in porous organic cages
;
_journal_name_full               Chem.Commun.
_journal_page_first              9465
_journal_paper_doi               10.1039/C4cc04158E
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C72 H84 N12, C H2 Cl2, 3(C4 H10 O)'
_chemical_formula_sum            'C85 H116 Cl2 N12 O3'
_chemical_formula_weight         1424.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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            3
_cell_length_a                   25.629(3)
_cell_length_b                   25.629(3)
_cell_length_c                   11.1848(15)
_cell_measurement_reflns_used    8881
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.367
_cell_measurement_theta_min      2.457
_cell_volume                     6362.4(14)
_computing_cell_refinement       'Bruker AXS SAINT V7.68A'
_computing_data_collection       'CrystalClear-SM Expert 2.1 (Rigaku, 2011)'
_computing_data_reduction        'Bruker AXS SAINT V7.68A'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0906
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14584
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.4973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2313
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.156
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         3644
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.1095
_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)+(0.1535P)²+49.8181P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3007
_refine_ls_wR_factor_ref         0.3020
_reflns_number_gt                3527
_reflns_number_total             3644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc04158e2.cif
_cod_data_source_block           Cage3_R_3(Et2O)_CH2Cl2_100K
_cod_original_cell_volume        6362.6(14)
_cod_original_sg_symbol_H-M      R3
_cod_database_code               7115467
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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
Cl1 Cl 0.6338(8) 0.3459(8) 0.7214(9) 0.072(4) Uani 0.17 1 d PDU . 1
Cl3 Cl 0.6608(13) 0.3712(7) 0.8643(10) 0.157(7) Uiso 0.17 1 d PDU . 2
Cl2 Cl 0.666(3) 0.3180(18) 0.9525(10) 0.157(7) Uiso 0.17 1 d PDU . 1
Cl4 Cl 0.6667 0.3333 1.1051(9) 0.171(8) Uani 0.50 3 d SPDU . 2
O1 O 0.6175(4) 0.5141(3) 0.7322(8) 0.098(3) Uani 1 1 d DU A 2
N1 N 0.5022(3) 0.2794(3) 0.4418(6) 0.0375(15) Uani 1 1 d . . .
N2 N 0.4366(3) 0.2352(3) 0.6675(7) 0.0385(16) Uani 1 1 d . . .
N3 N 0.5220(3) 0.4029(3) 1.1346(6) 0.0358(15) Uani 1 1 d . . .
N4 N 0.6448(3) 0.4994(3) 1.1534(7) 0.0370(15) Uani 1 1 d . . .
C1 C 0.6316(3) 0.3607(3) 0.4258(8) 0.0338(17) Uani 1 1 d . . .
H1 H 0.6074 0.3792 0.4260 0.041 Uiso 1 1 calc R . .
C2 C 0.6028(3) 0.2970(3) 0.4256(7) 0.0312(17) Uani 1 1 d . . .
C3 C 0.5380(4) 0.2591(4) 0.4299(7) 0.0355(17) Uani 1 1 d . . .
H3 H 0.5213 0.2167 0.4233 0.043 Uiso 1 1 calc R . .
C4 C 0.4383(3) 0.2373(3) 0.4464(8) 0.0372(18) Uani 1 1 d . . .
H4 H 0.4315 0.1953 0.4432 0.045 Uiso 1 1 calc R . .
C5 C 0.4099(3) 0.2445(4) 0.5594(8) 0.043(2) Uani 1 1 d . . .
H5 H 0.4178 0.2869 0.5612 0.051 Uiso 1 1 calc R . .
C6 C 0.3420(4) 0.2029(5) 0.5602(9) 0.054(2) Uani 1 1 d . . .
H6A H 0.3250 0.2099 0.6339 0.064 Uiso 1 1 calc R . .
H6B H 0.3329 0.1605 0.5610 0.064 Uiso 1 1 calc R . .
C7 C 0.3124(4) 0.2130(6) 0.4518(9) 0.068(3) Uani 1 1 d . . .
H7A H 0.2686 0.1838 0.4530 0.082 Uiso 1 1 calc R . .
H7B H 0.3180 0.2541 0.4550 0.082 Uiso 1 1 calc R . .
C8 C 0.3397(4) 0.2055(5) 0.3370(8) 0.049(2) Uani 1 1 d . . .
H8A H 0.3218 0.2149 0.2675 0.059 Uiso 1 1 calc R . .
H8B H 0.3303 0.1632 0.3295 0.059 Uiso 1 1 calc R . .
C9 C 0.4084(4) 0.2477(4) 0.3371(9) 0.047(2) Uani 1 1 d . . .
H9A H 0.4175 0.2900 0.3368 0.056 Uiso 1 1 calc R . .
H9B H 0.4256 0.2409 0.2633 0.056 Uiso 1 1 calc R . .
C10 C 0.4528(4) 0.2736(4) 0.7448(9) 0.0402(18) Uani 1 1 d . . .
H10 H 0.4499 0.3084 0.7284 0.048 Uiso 1 1 calc R . .
C11 C 0.4773(3) 0.2695(3) 0.8653(8) 0.0340(17) Uani 1 1 d . . .
C12 C 0.4808(3) 0.2183(4) 0.8949(8) 0.0357(18) Uani 1 1 d . . .
H12 H 0.4717 0.1878 0.8371 0.043 Uiso 1 1 calc R . .
C13 C 0.4977(3) 0.2130(3) 1.0090(8) 0.0355(18) Uani 1 1 d . . .
C14 C 0.5148(3) 0.2593(3) 1.0911(8) 0.0293(16) Uani 1 1 d . . .
H14 H 0.5280 0.2558 1.1685 0.035 Uiso 1 1 calc R . .
C15 C 0.5129(3) 0.3105(3) 1.0610(8) 0.0356(18) Uani 1 1 d . . .
C16 C 0.4941(3) 0.3153(3) 0.9467(8) 0.0380(19) Uani 1 1 d . . .
H16 H 0.4930 0.3505 0.9248 0.046 Uiso 1 1 calc R . .
C17 C 0.5306(3) 0.3594(4) 1.1500(7) 0.0382(19) Uani 1 1 d . . .
H17 H 0.5493 0.3576 1.2219 0.046 Uiso 1 1 calc R . .
C18 C 0.5418(3) 0.4463(3) 1.2287(8) 0.0338(17) Uani 1 1 d . . .
H18 H 0.5559 0.4319 1.2979 0.041 Uiso 1 1 calc R . .
C19 C 0.5936(3) 0.5071(4) 1.1838(8) 0.0391(19) Uani 1 1 d . . .
H19 H 0.5802 0.5198 1.1110 0.047 Uiso 1 1 calc R . .
C20 C 0.6127(4) 0.5546(4) 1.2772(8) 0.045(2) Uani 1 1 d . . .
H20A H 0.6460 0.5928 1.2452 0.054 Uiso 1 1 calc R . .
H20B H 0.6284 0.5430 1.3469 0.054 Uiso 1 1 calc R . .
C21 C 0.5620(5) 0.5651(4) 1.3188(9) 0.052(2) Uani 1 1 d . . .
H21A H 0.5489 0.5813 1.2521 0.062 Uiso 1 1 calc R . .
H21B H 0.5763 0.5947 1.3850 0.062 Uiso 1 1 calc R . .
C22 C 0.5095(4) 0.5050(4) 1.3611(9) 0.050(2) Uani 1 1 d . . .
H22A H 0.5221 0.4921 1.4339 0.060 Uiso 1 1 calc R . .
H22B H 0.4755 0.5110 1.3833 0.060 Uiso 1 1 calc R . .
C23 C 0.4880(4) 0.4554(4) 1.2692(9) 0.048(2) Uani 1 1 d . . .
H23A H 0.4715 0.4659 1.1991 0.058 Uiso 1 1 calc R . .
H23B H 0.4555 0.4174 1.3037 0.058 Uiso 1 1 calc R . .
C24 C 0.6597(3) 0.5049(3) 1.0445(8) 0.0339(17) Uani 1 1 d . . .
H24 H 0.6363 0.5107 0.9857 0.041 Uiso 1 1 calc R . .
C25 C 0.6014(9) 0.4172(5) 0.7126(15) 0.113(6) Uani 1 1 d DU A 2
H25A H 0.6238 0.3983 0.6823 0.170 Uiso 1 1 calc R A 2
H25B H 0.5581 0.3900 0.6998 0.170 Uiso 1 1 calc R A 2
H25C H 0.6092 0.4252 0.7983 0.170 Uiso 1 1 calc R A 2
C26 C 0.6208(3) 0.4744(3) 0.6486(7) 0.0528(19) Uani 1 1 d DU A 2
H26A H 0.6625 0.4911 0.6187 0.063 Uiso 1 1 calc R A 2
H26B H 0.5939 0.4678 0.5797 0.063 Uiso 1 1 calc R A 2
C27 C 0.6499(6) 0.5679(4) 0.6639(9) 0.087(3) Uani 1 1 d DU A 2
H27A H 0.6300 0.5672 0.5877 0.104 Uiso 1 1 calc R A 2
H27B H 0.6926 0.5796 0.6501 0.104 Uiso 1 1 calc R A 2
C28 C 0.6421(4) 0.6031(4) 0.7573(9) 0.060(2) Uani 1 1 d DU A 2
H28A H 0.6353 0.6339 0.7206 0.091 Uiso 1 1 calc R A 2
H28B H 0.6783 0.6226 0.8072 0.091 Uiso 1 1 calc R A 2
H28C H 0.6073 0.5764 0.8070 0.091 Uiso 1 1 calc R A 2
C29 C 0.6608(13) 0.3712(7) 0.8643(10) 0.157(7) Uiso 0.17 1 d PDU B 1
H29A H 0.6339 0.3832 0.9042 0.189 Uiso 0.17 1 calc PR B 1
H29B H 0.7012 0.4075 0.8582 0.189 Uiso 0.17 1 calc PR B 1
C30 C 0.666(3) 0.3180(18) 0.9525(10) 0.157(7) Uiso 0.17 1 d PDU C 2
H30A H 0.7029 0.3173 0.9317 0.189 Uiso 0.17 1 calc PR C 2
H30B H 0.6310 0.2777 0.9353 0.189 Uiso 0.17 1 calc PR C 2
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
Cl1 Cl1 Cl1 60.000(1) 3_665 2_655
Cl1 Cl1 C29 82.9(6) 3_665 2_655
Cl1 Cl1 C29 51.8(7) 2_655 2_655
C30 Cl3 C30 27.9(12) 3_665 2_655
C30 Cl3 Cl3 50(3) 3_665 2_655
C30 Cl3 Cl3 63.6(10) 2_655 2_655
C30 Cl3 Cl3 64.9(15) 3_665 3_665
C30 Cl3 Cl3 45.5(16) 2_655 3_665
Cl3 Cl3 Cl3 60.000(2) 2_655 3_665
Cl2 Cl2 Cl2 60.000(10) 2_655 3_665
Cl2 Cl2 C29 120(3) 2_655 2_655
Cl2 Cl2 C29 84(7) 3_665 2_655
Cl2 Cl2 C29 68(7) 2_655 3_665
Cl2 Cl2 C29 110(6) 3_665 3_665
C29 Cl2 C29 84.7(16) 2_655 3_665
C30 Cl4 C30 21.8(10) 2_655 3_665
C26 O1 C27 97.3(7) . .
C3 N1 C4 118.7(7) . .
C10 N2 C5 116.9(7) . .
C17 N3 C18 116.1(7) . .
C24 N4 C19 116.8(7) . .
C2 C1 C2 122.2(7) 3_665 .
C1 C2 C1 117.8(7) 2_655 .
C1 C2 C3 119.8(7) 2_655 .
C1 C2 C3 122.4(6) . .
N1 C3 C2 123.5(7) . .
N1 C4 C5 111.9(6) . .
N1 C4 C9 108.7(6) . .
C5 C4 C9 109.3(7) . .
N2 C5 C6 110.1(7) . .
N2 C5 C4 112.0(6) . .
C6 C5 C4 111.7(7) . .
C5 C6 C7 111.7(7) . .
C8 C7 C6 110.6(8) . .
C7 C8 C9 110.4(7) . .
C8 C9 C4 112.0(7) . .
N2 C10 C11 124.3(8) . .
C16 C11 C12 120.3(7) . .
C16 C11 C10 119.7(7) . .
C12 C11 C10 120.0(7) . .
C13 C12 C11 118.9(7) . .
C12 C13 C14 120.6(7) . .
C12 C13 C24 118.7(7) . 2_655
C14 C13 C24 120.6(7) . 2_655
C13 C14 C15 120.4(7) . .
C14 C15 C16 119.0(7) . .
C14 C15 C17 119.9(7) . .
C16 C15 C17 121.1(7) . .
C11 C16 C15 120.6(7) . .
N3 C17 C15 123.0(7) . .
N3 C18 C19 109.8(6) . .
N3 C18 C23 109.3(6) . .
C19 C18 C23 108.6(6) . .
N4 C19 C20 108.9(7) . .
N4 C19 C18 108.4(6) . .
C20 C19 C18 111.3(7) . .
C19 C20 C21 113.4(7) . .
C20 C21 C22 108.3(7) . .
C23 C22 C21 113.9(7) . .
C22 C23 C18 110.1(7) . .
N4 C24 C13 119.1(7) . 3_665
O1 C26 C25 106.4(8) . .
O1 C27 C28 91.1(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 Cl1 1.80(3) 3_665
Cl1 Cl1 1.80(3) 2_655
Cl1 C29 2.11(3) 2_655
Cl3 C30 1.31(4) 3_665
Cl3 C30 1.40(4) 2_655
Cl3 Cl3 1.83(3) 2_655
Cl3 Cl3 1.83(3) 3_665
Cl2 Cl2 0.66(3) 2_655
Cl2 Cl2 0.66(3) 3_665
Cl2 C29 1.31(4) 2_655
Cl2 C29 1.40(4) 3_665
O1 C26 1.416(5) .
O1 C27 1.424(5) .
N1 C3 1.268(10) .
N1 C4 1.442(10) .
N2 C10 1.216(10) .
N2 C5 1.467(10) .
N3 C17 1.254(10) .
N3 C18 1.426(10) .
N4 C24 1.262(10) .
N4 C19 1.463(10) .
C1 C2 1.397(10) 3_665
C1 C2 1.415(10) .
C2 C1 1.397(10) 2_655
C2 C3 1.447(11) .
C4 C5 1.516(11) .
C4 C9 1.535(12) .
C5 C6 1.519(11) .
C6 C7 1.520(13) .
C7 C8 1.520(13) .
C8 C9 1.539(12) .
C10 C11 1.512(11) .
C11 C16 1.374(11) .
C11 C12 1.397(11) .
C12 C13 1.377(12) .
C13 C14 1.387(11) .
C13 C24 1.513(11) 2_655
C14 C15 1.381(11) .
C15 C16 1.392(11) .
C15 C17 1.481(11) .
C18 C19 1.542(11) .
C18 C23 1.575(10) .
C19 C20 1.488(12) .
C20 C21 1.525(12) .
C21 C22 1.528(14) .
C22 C23 1.509(13) .
C24 C13 1.513(11) 3_665
C25 C26 1.477(5) .
C27 C28 1.459(5) .
