#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:51:57 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180279 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/65/7116540.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_7116540
loop_
_publ_author_name
'Luigi R. Nassimbeni'
'Nikoletta B. Bathori'
'Leena Desiree Patel'
'Hong Su'
'Edwin Weber'
_publ_section_title
;
 Separation of xylenes by enclathration
;
_journal_name_full               Chem.Commun.
_journal_page_first              3627
_journal_paper_doi               10.1039/C4cc05329J
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C37 H30 O2'
_chemical_formula_weight         506.61
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.92(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.733(4)
_cell_length_b                   8.5251(17)
_cell_length_c                   17.406(4)
_cell_measurement_reflns_used    3448
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.331
_cell_measurement_theta_min      2.186
_cell_volume                     2764.9(10)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16302
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.331
_diffrn_reflns_theta_min         2.186
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3448
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0561P)²+1.3316P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2654
_reflns_number_total             3448
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4cc05329j2.cif
_cod_data_source_block           H3oxylene
_cod_original_cell_volume        2765.0(10)
_cod_database_code               7116540
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.985
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.02931(4) 0.30985(10) 0.12013(5) 0.0306(2) Uani 1 1 d . . . . .
C1 C 0.3086(3) 0.7024(17) -0.0297(8) 0.0496(13) Uani 0.5 1 d D . P A -1
H1 H 0.3590 0.7080 -0.0323 0.059 Uiso 0.5 1 calc R U P A -1
C2 C 0.26926(18) 0.6014(4) -0.07943(19) 0.0615(9) Uani 0.5 1 d D . P A -1
H2 H 0.2924 0.5381 -0.1143 0.074 Uiso 0.5 1 calc R U P A -1
C3 C 0.19583(19) 0.5934(6) -0.0778(3) 0.0586(13) Uani 0.5 1 d D . P A -1
H3 H 0.1673 0.5258 -0.1118 0.070 Uiso 0.5 1 calc R U P A -1
C4 C 0.16509(19) 0.6867(3) -0.02529(17) 0.0504(8) Uani 0.5 1 d D . P A -1
H4 H 0.1146 0.6822 -0.0233 0.061 Uiso 0.5 1 calc R U P A -1
C5 C 0.2056(2) 0.7862(17) 0.0244(8) 0.0573(18) Uani 0.5 1 d D . P A -1
C6 C 0.27904(15) 0.7959(3) 0.02348(17) 0.0385(6) Uani 0.5 1 d D . P A -1
C7 C 0.1699(2) 0.8853(5) 0.0792(2) 0.0595(9) Uani 0.5 1 d . . P A -1
H7A H 0.1185 0.8615 0.0746 0.089 Uiso 0.5 1 calc R U P A -1
H7B H 0.1769 0.9962 0.0672 0.089 Uiso 0.5 1 calc R U P A -1
H7C H 0.1908 0.8637 0.1321 0.089 Uiso 0.5 1 calc R U P A -1
C8 C 0.3259(3) 0.8990(9) 0.0726(4) 0.0603(13) Uiso 0.5 1 d . . P A -1
H8A H 0.3197 0.8782 0.1269 0.090 Uiso 0.5 1 calc R U P A -1
H8B H 0.3135 1.0085 0.0603 0.090 Uiso 0.5 1 calc R U P A -1
H8C H 0.3759 0.8798 0.0635 0.090 Uiso 0.5 1 calc R U P A -1
C10 C -0.00847(6) -0.20710(14) 0.20805(7) 0.0295(3) Uani 1 1 d . . . . .
C11 C -0.01836(7) -0.33096(16) 0.15634(9) 0.0407(3) Uani 1 1 d . . . . .
H11 H -0.0127 -0.4362 0.1739 0.049 Uiso 1 1 calc R U . . .
C12 C -0.03650(8) -0.29896(18) 0.07914(9) 0.0451(4) Uani 1 1 d . . . . .
H12 H -0.0418 -0.3826 0.0430 0.054 Uiso 1 1 calc R U . . .
C13 C -0.04697(7) -0.14609(18) 0.05396(8) 0.0416(3) Uani 1 1 d . . . . .
H13 H -0.0613 -0.1264 0.0009 0.050 Uiso 1 1 calc R U . . .
C14 C -0.03686(6) -0.02066(16) 0.10509(7) 0.0319(3) Uani 1 1 d . . . . .
H14 H -0.0446 0.0841 0.0875 0.038 Uiso 1 1 calc R U . . .
C15 C -0.01524(6) -0.05149(13) 0.18212(6) 0.0246(2) Uani 1 1 d . . . . .
C16 C 0.0000 0.05570(18) 0.2500 0.0224(3) Uani 1 2 d S T P . .
C17 C 0.03959(6) 0.21305(13) 0.24832(6) 0.0237(2) Uani 1 1 d . . . . .
H17 H 0.0687 0.2423 0.2976 0.028 Uiso 1 1 calc R U . . .
C18 C 0.06888(6) 0.26882(13) 0.17645(6) 0.0244(2) Uani 1 1 d . . . . .
C19 C 0.14810(6) 0.27592(14) 0.17668(7) 0.0267(3) Uani 1 1 d . . . . .
C20 C 0.19418(7) 0.19840(16) 0.23146(8) 0.0369(3) Uani 1 1 d . . . . .
H20 H 0.1753 0.1396 0.2711 0.044 Uiso 1 1 calc R U . . .
C21 C 0.26760(8) 0.2067(2) 0.22841(9) 0.0470(4) Uani 1 1 d . . . . .
H21 H 0.2992 0.1524 0.2655 0.056 Uiso 1 1 calc R U . . .
C22 C 0.29493(7) 0.29378(19) 0.17142(9) 0.0466(4) Uani 1 1 d . . . . .
H22 H 0.3454 0.2999 0.1697 0.056 Uiso 1 1 calc R U . . .
C23 C 0.24964(8) 0.37170(19) 0.11716(9) 0.0470(4) Uani 1 1 d . . . . .
H23 H 0.2688 0.4318 0.0782 0.056 Uiso 1 1 calc R U . . .
C24 C 0.17638(7) 0.36283(17) 0.11915(8) 0.0367(3) Uani 1 1 d . . . . .
H24 H 0.1452 0.4160 0.0813 0.044 Uiso 1 1 calc R U . . .
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'
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
C2 C1 C6 123.8(4) . .
C1 C2 C3 119.2(4) . .
C2 C3 C4 118.0(4) . .
C5 C4 C3 121.9(4) . .
C6 C5 C4 120.9(4) . .
C6 C5 C7 119.3(3) . .
C4 C5 C7 119.9(3) . .
C5 C6 C1 116.3(4) . .
C5 C6 C8 124.8(4) . .
C1 C6 C8 118.9(3) . .
C11 C10 C15 120.62(12) . .
C11 C10 C10 130.44(9) . 2
C15 C10 C10 108.93(7) . 2
C12 C11 C10 118.99(13) . .
C11 C12 C13 120.54(13) . .
C12 C13 C14 121.07(13) . .
C15 C14 C13 118.69(13) . .
C14 C15 C10 119.91(11) . .
C14 C15 C16 131.36(11) . .
C10 C15 C16 108.64(10) . .
C15 C16 C15 104.80(13) 2 .
C15 C16 C17 124.86(7) 2 2
C15 C16 C17 119.69(7) . 2
C15 C16 C17 119.68(7) 2 .
C15 C16 C17 124.86(7) . .
C17 C16 C17 58.11(10) 2 .
C17 C17 C18 119.05(12) 2 .
C17 C17 C16 60.95(5) 2 .
C18 C17 C16 120.93(8) . .
O1 C18 C19 121.04(10) . .
O1 C18 C17 121.32(10) . .
C19 C18 C17 117.63(10) . .
C20 C19 C24 119.47(12) . .
C20 C19 C18 122.26(11) . .
C24 C19 C18 118.27(11) . .
C21 C20 C19 120.01(12) . .
C22 C21 C20 119.95(14) . .
C23 C22 C21 120.39(13) . .
C22 C23 C24 120.14(13) . .
C23 C24 C19 120.03(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C18 1.2177(14) .
C1 C2 1.3790(11) .
C1 C6 1.3803(11) .
C2 C3 1.3805(11) .
C3 C4 1.3813(11) .
C4 C5 1.3813(11) .
C5 C6 1.3805(11) .
C5 C7 1.484(5) .
C6 C8 1.455(6) .
C10 C11 1.3875(18) .
C10 C15 1.4027(16) .
C10 C10 1.462(3) 2
C11 C12 1.379(2) .
C12 C13 1.383(2) .
C13 C14 1.3916(18) .
C14 C15 1.3853(17) .
C15 C16 1.4976(14) .
C16 C15 1.4976(14) 2
C16 C17 1.5345(17) 2
C16 C17 1.5345(17) .
C17 C17 1.490(2) 2
C17 C18 1.4944(15) .
C18 C19 1.4849(15) .
C19 C20 1.3861(18) .
C19 C24 1.3935(17) .
C20 C21 1.3839(19) .
C21 C22 1.379(2) .
C22 C23 1.374(2) .
C23 C24 1.3785(19) .
