#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:51:57 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180279 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/65/7116539.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_7116539
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            'C29 H21'
_chemical_formula_weight         369.46
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   heavy
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 99.76(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.911(3)
_cell_length_b                   9.1555(18)
_cell_length_c                   16.101(3)
_cell_measurement_reflns_used    5057
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.370
_cell_measurement_theta_min      2.567
_cell_volume                     2021.0(7)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21399
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.370
_diffrn_reflns_theta_min         2.567
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       chunk
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.035
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0451
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3796
_reflns_number_total             5057
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4cc05329j2.cif
_cod_data_source_block           H2pxylene
_cod_database_code               7116539
#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   0.970
_shelx_estimated_absorpt_t_max   0.990
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 0.29073(8) 0.61326(13) 0.29431(7) 0.0287(3) Uani 1 1 d . .
C2 C 0.26455(8) 0.77408(13) 0.29651(8) 0.0301(3) Uani 1 1 d . .
C3 C 0.23123(9) 0.86497(15) 0.22944(9) 0.0382(3) Uani 1 1 d . .
H3 H 0.2239 0.8297 0.1732 0.046 Uiso 1 1 calc R U
C4 C 0.20861(10) 1.00833(16) 0.24531(11) 0.0473(4) Uani 1 1 d . .
H4 H 0.1865 1.0724 0.1997 0.057 Uiso 1 1 calc R U
C5 C 0.21805(10) 1.05861(15) 0.32687(12) 0.0503(4) Uani 1 1 d . .
H5 H 0.2012 1.1569 0.3368 0.060 Uiso 1 1 calc R U
C6 C 0.25159(10) 0.96888(16) 0.39467(10) 0.0443(4) Uani 1 1 d . .
H6 H 0.2579 1.0046 0.4507 0.053 Uiso 1 1 calc R U
C7 C 0.27593(8) 0.82475(14) 0.37914(8) 0.0324(3) Uani 1 1 d . .
C8 C 0.31502(8) 0.70608(13) 0.43596(8) 0.0313(3) Uani 1 1 d . .
C9 C 0.34282(9) 0.70214(16) 0.52294(8) 0.0403(3) Uani 1 1 d . .
H9 H 0.3369 0.7865 0.5561 0.048 Uiso 1 1 calc R U
C10 C 0.37915(9) 0.57352(18) 0.56035(9) 0.0454(4) Uani 1 1 d . .
H10 H 0.3982 0.5694 0.6198 0.054 Uiso 1 1 calc R U
C11 C 0.38815(10) 0.45091(17) 0.51258(9) 0.0453(4) Uani 1 1 d . .
H11 H 0.4136 0.3635 0.5396 0.054 Uiso 1 1 calc R U
C12 C 0.36047(9) 0.45339(15) 0.42521(9) 0.0381(3) Uani 1 1 d . .
H12 H 0.3666 0.3687 0.3925 0.046 Uiso 1 1 calc R U
C13 C 0.32408(8) 0.58134(13) 0.38754(7) 0.0296(3) Uani 1 1 d . .
C14 C 0.20456(9) 0.51972(13) 0.25390(7) 0.0300(3) Uani 1 1 d . .
C15 C 0.11351(9) 0.50768(14) 0.27595(8) 0.0372(3) Uani 1 1 d . .
H15 H 0.0973 0.5615 0.3221 0.045 Uiso 1 1 calc R U
C16 C 0.04580(10) 0.41515(16) 0.22926(10) 0.0464(4) Uani 1 1 d . .
H16 H -0.0170 0.4046 0.2444 0.056 Uiso 1 1 calc R U
C17 C 0.06818(11) 0.33837(16) 0.16140(10) 0.0490(4) Uani 1 1 d . .
H17 H 0.0207 0.2762 0.1301 0.059 Uiso 1 1 calc R U
C18 C 0.15899(11) 0.35113(14) 0.13861(9) 0.0433(3) Uani 1 1 d . .
H18 H 0.1742 0.2990 0.0915 0.052 Uiso 1 1 calc R U
C19 C 0.22789(9) 0.44128(13) 0.18562(8) 0.0326(3) Uani 1 1 d . .
C20 C 0.32845(9) 0.47624(13) 0.17683(8) 0.0339(3) Uani 1 1 d . .
C21 C 0.38575(11) 0.42716(16) 0.11962(9) 0.0470(4) Uani 1 1 d . .
H21 H 0.3605 0.3589 0.0770 0.056 Uiso 1 1 calc R U
C22 C 0.47968(12) 0.47898(19) 0.12558(10) 0.0551(4) Uani 1 1 d . .
H22 H 0.5194 0.4459 0.0869 0.066 Uiso 1 1 calc R U
C23 C 0.51660(10) 0.57855(19) 0.18726(10) 0.0525(4) Uani 1 1 d . .
H23 H 0.5815 0.6131 0.1904 0.063 Uiso 1 1 calc R U
C24 C 0.46027(9) 0.62903(16) 0.24477(9) 0.0411(3) Uani 1 1 d . .
H24 H 0.4858 0.6978 0.2870 0.049 Uiso 1 1 calc R U
C25 C 0.36601(8) 0.57666(13) 0.23904(8) 0.0314(3) Uani 1 1 d . .
C26 C 0.07974(11) 1.06803(18) -0.02154(9) 0.0451(4) Uani 1 1 d . .
H26 H 0.1343(12) 1.118(2) -0.0368(12) 0.065(5) Uiso 1 1 d . .
H27 H 0.1456(13) 0.871(2) 0.0194(12) 0.072(5) Uiso 1 1 d . .
C27 C 0.08715(10) 0.92907(18) 0.01086(9) 0.0457(4) Uani 1 1 d . .
C28 C 0.00759(11) 0.85754(16) 0.03328(8) 0.0444(3) Uani 1 1 d . .
C29 C 0.01555(18) 0.70542(19) 0.06945(12) 0.0805(6) Uani 1 1 d . .
H29A H 0.0193 0.7105 0.1307 0.121 Uiso 1 1 calc R U
H29B H 0.0745 0.6583 0.0564 0.121 Uiso 1 1 calc R U
H29C H -0.0419 0.6485 0.0448 0.121 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'
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 C25 114.75(10) . .
C2 C1 C13 101.38(10) . .
C25 C1 C13 114.16(9) . .
C2 C1 C14 112.33(9) . .
C25 C1 C14 101.28(10) . .
C13 C1 C14 113.50(10) . .
C3 C2 C7 121.04(12) . .
C3 C2 C1 128.06(12) . .
C7 C2 C1 110.88(10) . .
C2 C3 C4 118.96(13) . .
C5 C4 C3 120.37(14) . .
C4 C5 C6 121.29(13) . .
C5 C6 C7 118.69(14) . .
C2 C7 C6 119.64(12) . .
C2 C7 C8 108.65(11) . .
C6 C7 C8 131.71(12) . .
C9 C8 C13 120.28(12) . .
C9 C8 C7 131.28(12) . .
C13 C8 C7 108.43(10) . .
C10 C9 C8 118.78(13) . .
C9 C10 C11 120.86(13) . .
C10 C11 C12 120.93(13) . .
C13 C12 C11 118.47(13) . .
C12 C13 C8 120.67(12) . .
C12 C13 C1 128.76(11) . .
C8 C13 C1 110.56(10) . .
C15 C14 C19 120.57(12) . .
C15 C14 C1 128.72(11) . .
C19 C14 C1 110.71(11) . .
C14 C15 C16 118.57(13) . .
C17 C16 C15 121.09(14) . .
C18 C17 C16 120.53(13) . .
C17 C18 C19 118.96(14) . .
C18 C19 C14 120.25(13) . .
C18 C19 C20 131.27(13) . .
C14 C19 C20 108.47(11) . .
C21 C20 C25 120.11(13) . .
C21 C20 C19 131.08(13) . .
C25 C20 C19 108.80(10) . .
C22 C21 C20 119.06(15) . .
C23 C22 C21 120.65(14) . .
C22 C23 C24 121.05(14) . .
C25 C24 C23 118.36(14) . .
C24 C25 C20 120.77(12) . .
C24 C25 C1 128.50(12) . .
C20 C25 C1 110.73(10) . .
C27 C26 C28 121.22(14) . 3_575
C26 C27 C28 121.70(13) . .
C26 C28 C27 117.08(14) 3_575 .
C26 C28 C29 121.04(16) 3_575 .
C27 C28 C29 121.88(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.5186(17) .
C1 C25 1.5221(16) .
C1 C13 1.5225(17) .
C1 C14 1.5261(17) .
C2 C3 1.3798(17) .
C2 C7 1.3925(17) .
C3 C4 1.384(2) .
C4 C5 1.377(2) .
C5 C6 1.383(2) .
C6 C7 1.3954(18) .
C7 C8 1.4645(18) .
C8 C9 1.3887(18) .
C8 C13 1.4005(17) .
C9 C10 1.379(2) .
C10 C11 1.378(2) .
C11 C12 1.394(2) .
C12 C13 1.3756(17) .
C14 C15 1.3766(17) .
C14 C19 1.3967(18) .
C15 C16 1.3892(19) .
C16 C17 1.378(2) .
C17 C18 1.379(2) .
C18 C19 1.3881(18) .
C19 C20 1.4650(18) .
C20 C21 1.3910(19) .
C20 C25 1.3943(18) .
C21 C22 1.378(2) .
C22 C23 1.381(2) .
C23 C24 1.390(2) .
C24 C25 1.3845(17) .
C26 C27 1.372(2) .
C26 C28 1.378(2) 3_575
C27 C28 1.385(2) .
C28 C26 1.378(2) 3_575
C28 C29 1.506(2) .
