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#$Date: 2016-03-22 10:37:57 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178878 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/07/4110785.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_4110785
loop_
_publ_author_name
'P. S. Lakshminarayanan'
'D. Krishna Kumar'
'Pradyut Ghosh'
_publ_section_title
;
 Solid State Structural Evidence of Chloroform-Benzene-Chloroform Adduct
 Trapped in Hexaanthryl Octaaminocryptand Channels
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9600
_journal_page_last               9601
_journal_paper_doi               10.1021/ja063228g
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C22.33 H18.33 Cl N1.33'
_chemical_formula_weight         340.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 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            12
_cell_length_a                   15.5002(10)
_cell_length_b                   15.5002(10)
_cell_length_c                   25.940(4)
_cell_measurement_temperature    100(2)
_cell_volume                     5397.3(10)
_computing_cell_refinement       'BRUKER AXS SMART 3'
_computing_data_collection       'BRUKER AXS SMART 3'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_molecular_graphics    'PLATON, 'MERCURY 1.4'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART CCD AREA DETECTOR'
_diffrn_measurement_method       PHI-OMEGA
_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  0.1971
_diffrn_reflns_av_sigmaI/netI    0.1071
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21143
_diffrn_reflns_theta_full        22.48
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'PALE YELLOW'
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2368
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1498
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1011P)²+10.9944P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1880
_refine_ls_wR_factor_ref         0.2333
_reflns_number_gt                1323
_reflns_number_total             2368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063228gsi20060515_053243.cif
_cod_data_source_block           kkln50m
_cod_original_cell_volume        5397.3(9)
_cod_database_code               4110785
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-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
Cl1 Cl 0.00932(18) 0.11156(17) 0.40897(14) 0.1237(14) Uani 1 1 d . . .
N1 N 0.3333 0.6667 0.3438(5) 0.069(4) Uani 1 3 d SD . .
C2A C 0.2498(7) 0.5707(7) 0.3700(3) 0.028(2) Uiso 0.66 1 d PD A 1
C2B C 0.2377(9) 0.6019(11) 0.3119(5) 0.028(4) Uiso 0.34 1 d PD A 2
C3 C 0.1652(7) 0.5361(6) 0.3429(4) 0.118(5) Uani 1 1 d D . .
H3A H 0.1837 0.5326 0.3075 0.142 Uiso 1 1 calc R A 1
H3B H 0.1494 0.5893 0.3436 0.142 Uiso 1 1 calc R A 1
N4 N 0.0718(4) 0.4463(3) 0.35065(19) 0.0310(14) Uani 1 1 d . A .
C5 C 0.0774(5) 0.3556(4) 0.3447(2) 0.0295(16) Uani 1 1 d . . .
H5A H 0.0104 0.2986 0.3456 0.035 Uiso 1 1 calc R A .
H5B H 0.1137 0.3498 0.3737 0.035 Uiso 1 1 calc R . .
C6 C 0.1273(4) 0.3527(4) 0.2955(2) 0.0247(15) Uani 1 1 d . . .
C7 C 0.2166(5) 0.3526(5) 0.2970(2) 0.0321(17) Uani 1 1 d . . .
H7 H 0.2444 0.3525 0.3288 0.038 Uiso 1 1 calc R A .
C8 C 0.2655(5) 0.3526(4) 0.2518(2) 0.0321(16) Uani 1 1 d . . .
H8 H 0.3254 0.3526 0.2537 0.039 Uiso 1 1 calc R . .
C9 C 0.0208(4) 0.4414(4) 0.3991(2) 0.0285(16) Uani 1 1 d . . .
H9A H 0.0570 0.4336 0.4275 0.034 Uiso 1 1 calc R A .
H9B H -0.0454 0.3832 0.3985 0.034 Uiso 1 1 calc R . .
C10 C 0.0122(5) 0.5331(4) 0.4082(2) 0.0285(16) Uani 1 1 d . A .
C11 C -0.0521(5) 0.5500(5) 0.3768(2) 0.0318(17) Uani 1 1 d . . .
C12 C -0.1135(5) 0.4811(5) 0.3380(2) 0.0378(18) Uani 1 1 d . A .
H12 H -0.1084 0.4247 0.3317 0.045 Uiso 1 1 calc R . .
C13 C -0.1787(5) 0.4960(6) 0.3105(3) 0.0467(19) Uani 1 1 d . . .
H13 H -0.2197 0.4484 0.2865 0.056 Uiso 1 1 calc R A .
C14 C -0.1861(5) 0.5833(6) 0.3173(3) 0.0414(19) Uani 1 1 d . A .
H14 H -0.2306 0.5931 0.2977 0.050 Uiso 1 1 calc R . .
C15 C -0.1283(5) 0.6508(5) 0.3524(3) 0.0378(18) Uani 1 1 d . . .
H15 H -0.1328 0.7081 0.3564 0.045 Uiso 1 1 calc R A .
C16 C -0.0599(5) 0.6383(5) 0.3839(2) 0.0326(17) Uani 1 1 d . A .
C17 C -0.0009(5) 0.7075(5) 0.4209(2) 0.0363(17) Uani 1 1 d . . .
H17 H -0.0045 0.7653 0.4247 0.044 Uiso 1 1 calc R A .
C18 C 0.0630(5) 0.6935(5) 0.4523(2) 0.0346(17) Uani 1 1 d . A .
C19 C 0.1247(6) 0.7659(5) 0.4899(3) 0.046(2) Uani 1 1 d . . .
H19 H 0.1230 0.8248 0.4927 0.055 Uiso 1 1 calc R A .
C20 C 0.1853(6) 0.7507(6) 0.5212(3) 0.051(2) Uani 1 1 d . A .
H20 H 0.2255 0.7993 0.5449 0.061 Uiso 1 1 calc R . .
C21 C 0.1875(5) 0.6613(5) 0.5179(2) 0.0407(19) Uani 1 1 d . . .
H21 H 0.2280 0.6506 0.5403 0.049 Uiso 1 1 calc R A .
C22 C 0.1319(5) 0.5907(5) 0.4827(2) 0.0358(18) Uani 1 1 d . A .
H22 H 0.1348 0.5323 0.4816 0.043 Uiso 1 1 calc R . .
C23 C 0.0687(4) 0.6039(5) 0.4473(2) 0.0308(16) Uani 1 1 d . . .
C24 C 0.0000 0.0000 0.3854(9) 0.097(6) Uani 1 3 d S . .
H24 H 0.0000 0.0000 0.3476 0.117 Uiso 1 3 calc SR . .
C25 C 0.1008(9) 0.0504(5) 0.2500 0.135(8) Uani 1 2 d S . .
H25 H 0.1700 0.0850 0.2500 0.162 Uiso 1 2 calc SR . .
C26 C 0.0491(5) 0.0983(9) 0.2500 0.150(9) Uani 1 2 d S . .
H26 H 0.0838 0.1675 0.2500 0.181 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 0.0033 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'
N N 0.0061 0.0033 '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
C2B N1 C2B 94.1(8) . 2_665
C2B N1 C2B 94.1(9) . 3_565
C2B N1 C2B 94.1(9) 2_665 3_565
C2B N1 C2A 149.1(8) . 2_665
C2B N1 C2A 63.0(6) 2_665 2_665
C2B N1 C2A 107.2(7) 3_565 2_665
C2B N1 C2A 107.2(7) . 3_565
C2B N1 C2A 149.1(8) 2_665 3_565
C2B N1 C2A 63.0(6) 3_565 3_565
C2A N1 C2A 102.3(6) 2_665 3_565
C2B N1 C2A 63.0(6) . .
C2B N1 C2A 107.2(7) 2_665 .
C2B N1 C2A 149.1(8) 3_565 .
C2A N1 C2A 102.3(6) 2_665 .
C2A N1 C2A 102.3(6) 3_565 .
C3 C2A N1 109.4(7) . .
C3 C2B N1 109.8(8) . .
C2B C3 C2A 74.4(8) . .
C2B C3 N4 151.2(10) . .
C2A C3 N4 128.6(10) . .
C3 N4 C5 113.8(6) . .
C3 N4 C9 115.3(5) . .
C5 N4 C9 109.3(5) . .
N4 C5 C6 113.4(5) . .
C8 C6 C7 118.6(5) 5 .
C8 C6 C5 121.1(6) 5 .
C7 C6 C5 120.3(5) . .
C6 C7 C8 121.2(6) . .
C6 C8 C7 120.2(6) 5 .
N4 C9 C10 112.5(5) . .
C11 C10 C23 119.1(6) . .
C11 C10 C9 119.3(6) . .
C23 C10 C9 121.6(6) . .
C10 C11 C12 122.4(6) . .
C10 C11 C16 120.3(6) . .
C12 C11 C16 117.3(6) . .
C13 C12 C11 121.4(6) . .
C12 C13 C14 121.3(7) . .
C15 C14 C13 119.3(7) . .
C14 C15 C16 122.4(7) . .
C17 C16 C15 122.5(6) . .
C17 C16 C11 119.1(6) . .
C15 C16 C11 118.4(6) . .
C18 C17 C16 122.2(6) . .
C17 C18 C19 121.9(6) . .
C17 C18 C23 119.6(6) . .
C19 C18 C23 118.5(7) . .
C20 C19 C18 121.6(7) . .
C19 C20 C21 119.8(7) . .
C22 C21 C20 121.3(7) . .
C21 C22 C23 121.4(7) . .
C22 C23 C10 123.2(6) . .
C22 C23 C18 117.2(6) . .
C10 C23 C18 119.6(6) . .
Cl1 C24 Cl1 108.7(7) 3 .
Cl1 C24 Cl1 108.7(7) 3 2
Cl1 C24 Cl1 108.7(7) . 2
C26 C25 C26 117.5(14) . 3
C25 C26 C25 122.5(14) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 C24 1.771(8) .
N1 C2B 1.550(10) .
N1 C2B 1.550(10) 2_665
N1 C2B 1.550(10) 3_565
N1 C2A 1.558(8) 2_665
N1 C2A 1.558(8) 3_565
N1 C2A 1.558(8) .
C2A C3 1.342(10) .
C2B C3 1.343(12) .
C3 N4 1.435(9) .
N4 C5 1.459(7) .
N4 C9 1.467(7) .
C5 C6 1.507(8) .
C6 C8 1.375(8) 5
C6 C7 1.385(8) .
C7 C8 1.396(8) .
C8 C6 1.375(8) 5
C9 C10 1.512(8) .
C10 C11 1.409(9) .
C10 C23 1.429(9) .
C11 C12 1.430(9) .
C11 C16 1.443(9) .
C12 C13 1.350(9) .
C13 C14 1.424(10) .
C14 C15 1.337(9) .
C15 C16 1.427(9) .
C16 C17 1.388(9) .
C17 C18 1.381(9) .
C18 C19 1.432(9) .
C18 C23 1.440(9) .
C19 C20 1.348(10) .
C20 C21 1.405(10) .
C21 C22 1.352(9) .
C22 C23 1.431(9) .
C24 Cl1 1.771(8) 3
C24 Cl1 1.771(8) 2
C25 C26 1.336(8) .
C25 C26 1.336(8) 3
C26 C25 1.336(8) 2
