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#$Date: 2016-03-26 17:11:47 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180380 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/49/7204952.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_7204952
loop_
_publ_author_name
'Caira, Mino R.'
'Nassimbeni, Luigi R.'
'Vujovic, Dejana'
'Weber, Edwin'
_publ_section_title
;
 Guest exchange and competition in inclusion compounds
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              861
_journal_paper_doi               10.1039/b009446n
_journal_year                    2001
_chemical_formula_sum            'C38 H38 O4'
_chemical_formula_weight         558.72
_chemical_name_systematic
;4  
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.095(8)
_cell_angle_beta                 96.159(8)
_cell_angle_gamma                106.679(7)
_cell_formula_units_Z            2
_cell_length_a                   8.3480(10)
_cell_length_b                   9.2270(10)
_cell_length_c                   10.369(2)
_cell_measurement_temperature    293(2)
_cell_volume                     752.77(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3460
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.078
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             298
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2517
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0512
_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)+(0.0549P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                1565
_reflns_number_total             2517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009446n.txt
_cod_data_source_block           c:\dejana\struct~1\4
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7204952
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
O9 O 0.11307(18) 0.49662(15) 0.67030(14) 0.0310(4) Uani 1 1 d D . .
C10 C 0.0768(2) 0.5552(2) 0.8932(2) 0.0246(5) Uani 1 1 d . . .
C5A C 0.2908(3) 0.8866(2) 0.7869(2) 0.0308(6) Uani 1 1 d . . .
C1A C 0.3592(3) 0.6648(2) 0.82341(19) 0.0275(6) Uani 1 1 d . . .
C4A C 0.4264(3) 0.8241(2) 0.8327(2) 0.0311(6) Uani 1 1 d . . .
C8A C 0.1405(3) 0.7663(2) 0.7504(2) 0.0276(6) Uani 1 1 d . . .
C8 C -0.0044(3) 0.7915(3) 0.6938(2) 0.0342(6) Uani 1 1 d . . .
H8 H -0.1038 0.7111 0.6690 0.041 Uiso 1 1 calc R . .
C9 C 0.1684(3) 0.6159(2) 0.7804(2) 0.0266(6) Uani 1 1 d . . .
C1 C 0.4617(3) 0.5760(3) 0.8511(2) 0.0364(6) Uani 1 1 d . . .
H1 H 0.4164 0.4704 0.8440 0.044 Uiso 1 1 calc R . .
C6 C 0.1474(3) 1.0592(3) 0.7128(2) 0.0440(7) Uani 1 1 d . . .
H6 H 0.1483 1.1576 0.7000 0.053 Uiso 1 1 calc R . .
C4 C 0.5982(3) 0.8927(3) 0.8740(2) 0.0411(7) Uani 1 1 d . . .
H4 H 0.6441 0.9984 0.8826 0.049 Uiso 1 1 calc R . .
C5 C 0.2933(3) 1.0342(3) 0.7704(2) 0.0392(7) Uani 1 1 d . . .
H5 H 0.3914 1.1155 0.7974 0.047 Uiso 1 1 calc R . .
C3 C 0.6999(3) 0.8026(3) 0.9019(2) 0.0470(7) Uani 1 1 d . . .
H3 H 0.8149 0.8482 0.9295 0.056 Uiso 1 1 calc R . .
C7 C 0.0012(3) 0.9390(3) 0.6745(2) 0.0428(7) Uani 1 1 d . . .
H7 H -0.0952 0.9573 0.6351 0.051 Uiso 1 1 calc R . .
C2 C 0.6334(3) 0.6455(3) 0.8897(2) 0.0447(7) Uani 1 1 d . . .
H2 H 0.7041 0.5862 0.9074 0.054 Uiso 1 1 calc R . .
O1G O 0.2297(2) 0.57125(17) 0.44344(15) 0.0360(5) Uani 1 1 d D . .
C1G C 0.3544(3) 0.6944(2) 0.4020(2) 0.0344(6) Uani 1 1 d . . .
H1GA H 0.3617 0.6658 0.3095 0.041 Uiso 1 1 calc R . .
C3G C 0.5215(3) 0.7108(3) 0.4815(3) 0.0454(7) Uani 1 1 d . . .
H3G1 H 0.5137 0.7308 0.5730 0.068 Uiso 1 1 calc R . .
H3G2 H 0.6069 0.7941 0.4579 0.068 Uiso 1 1 calc R . .
H3G3 H 0.5508 0.6180 0.4645 0.068 Uiso 1 1 calc R . .
C2G C 0.3034(3) 0.8382(3) 0.4151(3) 0.0457(7) Uani 1 1 d . . .
H2G1 H 0.1929 0.8189 0.3668 0.069 Uiso 1 1 calc R . .
H2G2 H 0.3831 0.9169 0.3811 0.069 Uiso 1 1 calc R . .
H2G3 H 0.3017 0.8707 0.5059 0.069 Uiso 1 1 calc R . .
C11 C 0.0020(3) 0.3998(2) 0.8924(2) 0.0301(6) Uani 1 1 d . . .
H11 H 0.0031 0.3309 0.8204 0.036 Uiso 1 1 calc R . .
C12 C -0.0741(3) 0.3463(2) 0.9973(2) 0.0300(6) Uani 1 1 d . . .
H12 H -0.1245 0.2418 0.9942 0.035(6) Uiso 1 1 calc R . .
H9 H 0.173(3) 0.526(2) 0.596(2) 0.061(8) Uiso 1 1 d D . .
H1G H 0.124(3) 0.563(3) 0.398(3) 0.078(10) Uiso 1 1 d D . .
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
_geom_angle_publ_flag
C12 C10 C11 117.75(19) 2_567 . ?
C12 C10 C9 120.72(18) 2_567 . ?
C11 C10 C9 121.4(2) . . ?
C5 C5A C8A 119.8(2) . . ?
C5 C5A C4A 131.3(2) . . ?
C8A C5A C4A 108.82(19) . . ?
C1 C1A C4A 120.8(2) . . ?
C1 C1A C9 128.99(19) . . ?
C4A C1A C9 110.2(2) . . ?
C4 C4A C1A 119.4(2) . . ?
C4 C4A C5A 131.9(2) . . ?
C1A C4A C5A 108.67(18) . . ?
C8 C8A C5A 120.9(2) . . ?
C8 C8A C9 128.87(18) . . ?
C5A C8A C9 110.17(19) . . ?
C8A C8 C7 118.6(2) . . ?
O9 C9 C1A 113.00(17) . . ?
O9 C9 C8A 113.29(17) . . ?
C1A C9 C8A 101.70(16) . . ?
O9 C9 C10 107.15(16) . . ?
C1A C9 C10 109.64(16) . . ?
C8A C9 C10 112.07(18) . . ?
C1A C1 C2 119.2(2) . . ?
C7 C6 C5 120.5(2) . . ?
C3 C4 C4A 119.3(2) . . ?
C5A C5 C6 119.1(2) . . ?
C4 C3 C2 121.0(2) . . ?
C6 C7 C8 121.1(2) . . ?
C3 C2 C1 120.2(2) . . ?
O1G C1G C3G 107.43(17) . . ?
O1G C1G C2G 110.44(18) . . ?
C3G C1G C2G 113.3(2) . . ?
C12 C11 C10 120.8(2) . . ?
C10 C12 C11 121.45(19) 2_567 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O9 C9 1.434(3) . ?
C10 C12 1.383(3) 2_567 ?
C10 C11 1.389(3) . ?
C10 C9 1.533(3) . ?
C5A C5 1.385(3) . ?
C5A C8A 1.399(3) . ?
C5A C4A 1.470(3) . ?
C1A C1 1.373(3) . ?
C1A C4A 1.403(3) . ?
C1A C9 1.527(3) . ?
C4A C4 1.389(3) . ?
C8A C8 1.379(3) . ?
C8A C9 1.529(3) . ?
C8 C7 1.385(3) . ?
C1 C2 1.386(3) . ?
C6 C7 1.380(3) . ?
C6 C5 1.388(3) . ?
C4 C3 1.378(3) . ?
C3 C2 1.382(3) . ?
O1G C1G 1.442(2) . ?
C1G C3G 1.501(3) . ?
C1G C2G 1.504(3) . ?
C11 C12 1.384(3) . ?
C12 C10 1.383(3) 2_567 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C1A C4A C4 -1.8(3) . . . . ?
C9 C1A C4A C4 178.31(19) . . . . ?
C1 C1A C4A C5A 175.22(19) . . . . ?
C9 C1A C4A C5A -4.7(2) . . . . ?
C5 C5A C4A C4 0.3(4) . . . . ?
C8A C5A C4A C4 176.9(2) . . . . ?
C5 C5A C4A C1A -176.2(2) . . . . ?
C8A C5A C4A C1A 0.4(2) . . . . ?
C5 C5A C8A C8 2.3(3) . . . . ?
C4A C5A C8A C8 -174.76(18) . . . . ?
C5 C5A C8A C9 -178.92(19) . . . . ?
C4A C5A C8A C9 4.0(2) . . . . ?
C5A C8A C8 C7 -0.5(3) . . . . ?
C9 C8A C8 C7 -179.1(2) . . . . ?
C1 C1A C9 O9 -51.4(3) . . . . ?
C4A C1A C9 O9 128.45(18) . . . . ?
C1 C1A C9 C8A -173.2(2) . . . . ?
C4A C1A C9 C8A 6.7(2) . . . . ?
C1 C1A C9 C10 68.0(3) . . . . ?
C4A C1A C9 C10 -112.11(19) . . . . ?
C8 C8A C9 O9 50.7(3) . . . . ?
C5A C8A C9 O9 -128.00(18) . . . . ?
C8 C8A C9 C1A 172.3(2) . . . . ?
C5A C8A C9 C1A -6.4(2) . . . . ?
C8 C8A C9 C10 -70.7(3) . . . . ?
C5A C8A C9 C10 110.60(19) . . . . ?
C12 C10 C9 O9 -165.44(19) 2_567 . . . ?
C11 C10 C9 O9 18.1(3) . . . . ?
C12 C10 C9 C1A 71.6(3) 2_567 . . . ?
C11 C10 C9 C1A -104.9(2) . . . . ?
C12 C10 C9 C8A -40.6(3) 2_567 . . . ?
C11 C10 C9 C8A 143.0(2) . . . . ?
C4A C1A C1 C2 0.5(3) . . . . ?
C9 C1A C1 C2 -179.6(2) . . . . ?
C1A C4A C4 C3 1.5(3) . . . . ?
C5A C4A C4 C3 -174.7(2) . . . . ?
C8A C5A C5 C6 -2.5(3) . . . . ?
C4A C5A C5 C6 173.8(2) . . . . ?
C7 C6 C5 C5A 1.0(3) . . . . ?
C4A C4 C3 C2 -0.1(3) . . . . ?
C5 C6 C7 C8 0.8(4) . . . . ?
C8A C8 C7 C6 -1.0(3) . . . . ?
C4 C3 C2 C1 -1.2(3) . . . . ?
C1A C1 C2 C3 0.9(3) . . . . ?
C12 C10 C11 C12 0.7(3) 2_567 . . . ?
C9 C10 C11 C12 177.27(19) . . . . ?
C10 C11 C12 C10 -0.7(4) . . . 2_567 ?
