#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:14:17 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185190 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/54/7225424.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_7225424
loop_
_publ_author_name
'Yang, Bo'
'Gao, Zhong-Zheng'
'Lu, Ji-Hong'
'Zhu, Qian-Jiang'
'Xue, Sai-Feng'
'Tao, Zhu'
'Prior, Timothy J.'
'Redshaw, Carl'
'Wei, Gang'
'Xiao, Xin'
_publ_section_title
;
 Interaction of a symmetrical
 α,α′,δ,δ′-tetramethyl-cucurbit[6]uril with Ln3+:
 potential applications for isolation of lanthanides
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              5028
_journal_paper_doi               10.1039/C6CE00134C
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C40 H44 N24 O20 Sm'
_chemical_formula_weight         1331.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-05-31 deposited with the CCDC.
2016-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.685(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.308(10)
_cell_length_b                   12.540(6)
_cell_length_c                   14.747(7)
_cell_measurement_reflns_used    5407
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.13
_cell_measurement_theta_min      2.16
_cell_volume                     3718(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9884
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         1.532
_exptl_absorpt_coefficient_mu    0.861
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0354
_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)+(0.0518P)²+3.2968P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3323
_reflns_number_total             3482
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce00134c2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7225407--7225427.cif.'
_cod_database_code               7225424
_shelx_shelxl_version_number     2014/7
_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   0.801
_shelx_estimated_absorpt_t_max   0.853
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_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
Sm1 Sm 1.0000 1.0000 0.5000 0.03602(14) Uani 1 4 d S T P . .
N1 N 0.77308(14) 0.4025(2) 0.4147(2) 0.0430(6) Uani 1 1 d . . . . .
N2 N 0.82035(13) 0.40229(19) 0.5807(2) 0.0424(6) Uani 1 1 d . . . . .
N3 N 0.92412(14) 0.40308(19) 0.7316(2) 0.0437(7) Uani 1 1 d . . . . .
N4 N 1.03399(13) 0.4028(2) 0.8111(2) 0.0425(6) Uani 1 1 d . . . . .
N5 N 1.14270(14) 0.4031(2) 0.8118(2) 0.0448(7) Uani 1 1 d . . . . .
N6 N 1.20783(14) 0.4032(2) 0.7346(2) 0.0442(7) Uani 1 1 d . . . . .
O1 O 0.83586(13) 0.25832(18) 0.4980(2) 0.0546(6) Uani 1 1 d . . . . .
O2 O 0.98116(14) 0.2571(2) 0.7164(2) 0.0707(8) Uani 1 1 d . . . . .
O3 O 1.14136(16) 0.2580(2) 0.7169(2) 0.0705(8) Uani 1 1 d . . . . .
O4 O 0.9053(3) 0.9308(4) 0.3574(4) 0.0709(17) Uani 0.5 1 d . . P A 1
O6 O 0.9521(3) 0.8528(4) 0.5530(4) 0.0610(14) Uani 0.5 1 d . . P A 1
O5 O 0.9218(3) 0.8524(4) 0.4472(4) 0.0608(14) Uani 0.5 1 d . . P B 2
O7 O 0.9890(3) 0.9312(4) 0.6442(4) 0.0643(15) Uani 0.5 1 d . . P A 2
C1 C 0.81281(15) 0.3468(2) 0.4980(3) 0.0418(8) Uani 1 1 d . . . . .
C2 C 0.7802(2) 0.5000 0.5563(4) 0.0399(10) Uani 1 2 d S T P . .
C3 C 0.7468(2) 0.5000 0.4386(4) 0.0402(10) Uani 1 2 d S T P . .
C4 C 0.85782(17) 0.3600(3) 0.6800(3) 0.0472(8) Uani 1 1 d . . . . .
H4A H 0.8609 0.2833 0.6753 0.057 Uiso 1 1 calc R U . . .
H4B H 0.8338 0.3744 0.7200 0.057 Uiso 1 1 calc R U . . .
C5 C 0.97977(18) 0.3462(2) 0.7491(3) 0.0453(8) Uani 1 1 d . . . . .
C6 C 1.0155(2) 0.5000 0.8452(3) 0.0413(10) Uani 1 2 d S T P . .
H6 H 1.0311 0.5000 0.9184 0.050 Uiso 1 2 calc R U P . .
C7 C 0.9389(2) 0.5000 0.7902(4) 0.0418(10) Uani 1 2 d S T P . .
H7 H 0.9188 0.5000 0.8376 0.050 Uiso 1 2 calc R U P . .
C8 C 1.10047(17) 0.3593(3) 0.8534(3) 0.0473(8) Uani 1 1 d . . . . .
H8A H 1.1210 0.3718 0.9254 0.057 Uiso 1 1 calc R U . . .
H8B H 1.0976 0.2827 0.8429 0.057 Uiso 1 1 calc R U . . .
C9 C 1.16158(18) 0.3463(3) 0.7504(3) 0.0473(8) Uani 1 1 d . . . . .
C10 C 1.2259(2) 0.5000 0.7933(3) 0.0409(11) Uani 1 2 d S T P . .
H10 H 1.2731 0.5000 0.8412 0.049 Uiso 1 2 calc R U P . .
C11 C 1.1810(2) 0.5000 0.8471(3) 0.0395(10) Uani 1 2 d S T P . .
H11 H 1.2068 0.5000 0.9204 0.047 Uiso 1 2 calc R U P . .
C12 C 0.75465(18) 0.3605(3) 0.3151(3) 0.0486(9) Uani 1 1 d . . . . .
H12A H 0.7603 0.2836 0.3198 0.058 Uiso 1 1 calc R U . . .
H12B H 0.7079 0.3750 0.2742 0.058 Uiso 1 1 calc R U . . .
C13 C 0.7331(3) 0.5000 0.6061(5) 0.0622(15) Uani 1 2 d S T P . .
H13A H 0.7123 0.4314 0.5976 0.093 Uiso 0.5 1 calc R U P . .
H13B H 0.6996 0.5537 0.5756 0.093 Uiso 0.5 1 calc R U P . .
H13C H 0.7577 0.5150 0.6766 0.093 Uiso 0.5 1 calc R U P . .
C14 C 0.6712(2) 0.5000 0.3897(4) 0.0604(14) Uani 1 2 d S T P . .
H14A H 0.6554 0.4353 0.4066 0.091 Uiso 0.5 1 calc R U P . .
H14B H 0.6555 0.5600 0.4135 0.091 Uiso 0.5 1 calc R U P . .
H14C H 0.6551 0.5047 0.3179 0.091 Uiso 1 2 calc R U P . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 '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
O7 Sm1 O7 42.0(2) . 6_575
O7 Sm1 O7 138.0(2) . 2_756
O7 Sm1 O7 180.0 6_575 2_756
O7 Sm1 O7 180.0 . 5_776
O7 Sm1 O7 138.0(2) 6_575 5_776
O7 Sm1 O7 42.0(2) 2_756 5_776
O4 Sm1 O4 180.0 . 5_776
O4 Sm1 O4 137.7(2) . 2_756
O4 Sm1 O4 42.3(2) 5_776 2_756
O4 Sm1 O4 42.3(2) . 6_575
O4 Sm1 O4 137.7(2) 5_776 6_575
O4 Sm1 O4 180.0 2_756 6_575
O4 Sm1 O6 70.4(2) . .
O4 Sm1 O6 109.6(2) 5_776 .
O4 Sm1 O6 77.7(2) 2_756 .
O4 Sm1 O6 102.3(2) 6_575 .
O4 Sm1 O6 109.6(2) . 5_776
O4 Sm1 O6 70.4(2) 5_776 5_776
O4 Sm1 O6 102.3(2) 2_756 5_776
O4 Sm1 O6 77.7(2) 6_575 5_776
O6 Sm1 O6 180.0 . 5_776
O4 Sm1 O6 77.7(2) . 2_756
O4 Sm1 O6 102.3(2) 5_776 2_756
O4 Sm1 O6 70.4(2) 2_756 2_756
O4 Sm1 O6 109.6(2) 6_575 2_756
O6 Sm1 O6 80.9(3) . 2_756
O6 Sm1 O6 99.1(3) 5_776 2_756
O4 Sm1 O6 102.3(2) . 6_575
O4 Sm1 O6 77.7(2) 5_776 6_575
O4 Sm1 O6 109.6(2) 2_756 6_575
O4 Sm1 O6 70.4(2) 6_575 6_575
O6 Sm1 O6 99.1(3) . 6_575
O6 Sm1 O6 80.9(3) 5_776 6_575
O6 Sm1 O6 180.0(3) 2_756 6_575
C1 N1 C12 121.3(3) . .
C1 N1 C3 112.7(3) . .
C12 N1 C3 125.7(3) . .
C1 N2 C4 121.4(3) . .
C1 N2 C2 112.6(3) . .
C4 N2 C2 125.6(3) . .
C5 N3 C4 123.3(3) . .
C5 N3 C7 112.1(3) . .
C4 N3 C7 123.1(3) . .
C5 N4 C8 122.8(3) . .
C5 N4 C6 111.7(3) . .
C8 N4 C6 124.3(3) . .
C9 N5 C8 122.4(3) . .
C9 N5 C11 112.1(3) . .
C8 N5 C11 124.1(3) . .
C9 N6 C12 123.2(3) . 2_756
C9 N6 C10 112.0(3) . .
C12 N6 C10 123.2(3) 2_756 .
O4 O4 Sm1 68.85(12) 6_575 .
O7 O7 Sm1 68.98(12) 6_575 .
O1 C1 N2 125.4(3) . .
O1 C1 N1 125.3(3) . .
N2 C1 N1 109.2(3) . .
N2 C2 N2 113.2(4) 6_565 .
N2 C2 C13 110.9(3) 6_565 .
N2 C2 C13 110.9(3) . .
N2 C2 C3 102.7(3) 6_565 .
N2 C2 C3 102.7(3) . .
C13 C2 C3 116.0(4) . .
N1 C3 N1 113.3(4) 6_565 .
N1 C3 C14 111.3(2) 6_565 .
N1 C3 C14 111.3(2) . .
N1 C3 C2 102.6(2) 6_565 .
N1 C3 C2 102.6(2) . .
C14 C3 C2 115.2(4) . .
N2 C4 N3 114.2(3) . .
O2 C5 N3 125.7(3) . .
O2 C5 N4 125.2(3) . .
N3 C5 N4 109.2(3) . .
N4 C6 N4 115.0(4) . 6_565
N4 C6 C7 103.6(3) . .
N4 C6 C7 103.6(3) 6_565 .
N3 C7 N3 114.6(4) . 6_565
N3 C7 C6 103.2(3) . .
N3 C7 C6 103.2(3) 6_565 .
N5 C8 N4 114.3(3) . .
O3 C9 N5 125.6(4) . .
O3 C9 N6 125.8(4) . .
N5 C9 N6 108.6(3) . .
N6 C10 N6 114.5(4) 6_565 .
N6 C10 C11 103.7(3) 6_565 .
N6 C10 C11 103.7(3) . .
N5 C11 N5 114.3(4) 6_565 .
N5 C11 C10 103.4(3) 6_565 .
N5 C11 C10 103.4(3) . .
N6 C12 N1 114.3(3) 2_756 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sm1 O7 2.404(5) .
Sm1 O7 2.404(5) 6_575
Sm1 O7 2.404(5) 2_756
Sm1 O7 2.404(5) 5_776
Sm1 O4 2.405(5) .
Sm1 O4 2.405(5) 5_776
Sm1 O4 2.405(5) 2_756
Sm1 O4 2.405(5) 6_575
Sm1 O6 2.425(5) .
Sm1 O6 2.425(5) 5_776
Sm1 O6 2.425(5) 2_756
Sm1 O6 2.425(5) 6_575
N1 C1 1.356(4) .
N1 C12 1.443(4) .
N1 C3 1.463(4) .
N2 C1 1.350(4) .
N2 C4 1.436(4) .
N2 C2 1.467(3) .
N3 C5 1.356(4) .
N3 C4 1.443(4) .
N3 C7 1.444(4) .
N4 C5 1.358(4) .
N4 C8 1.444(4) .
N4 C6 1.445(4) .
N5 C9 1.355(5) .
N5 C8 1.438(4) .
N5 C11 1.447(4) .
N6 C9 1.355(5) .
N6 C12 1.434(4) 2_756
N6 C10 1.444(4) .
O1 C1 1.223(4) .
O2 C5 1.222(4) .
O3 C9 1.217(4) .
O4 O4 1.736(10) 6_575
O7 O7 1.724(10) 6_575
C2 N2 1.467(3) 6_565
C2 C13 1.521(7) .
C2 C3 1.564(7) .
C3 N1 1.463(4) 6_565
C3 C14 1.518(7) .
C6 N4 1.445(4) 6_565
C6 C7 1.541(7) .
C7 N3 1.444(4) 6_565
C10 N6 1.444(4) 6_565
C10 C11 1.524(7) .
C11 N5 1.447(4) 6_565
C12 N6 1.434(4) 2_756
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_4
C4 N2 C1 O1 0.1(5) . .
C2 N2 C1 O1 -173.0(3) . .
C4 N2 C1 N1 177.3(3) . .
C2 N2 C1 N1 4.2(4) . .
C12 N1 C1 O1 -0.7(5) . .
C3 N1 C1 O1 173.0(3) . .
C12 N1 C1 N2 -177.9(3) . .
C3 N1 C1 N2 -4.2(4) . .
C1 N2 C2 N2 -112.5(4) . 6_565
C4 N2 C2 N2 74.8(5) . 6_565
C1 N2 C2 C13 122.1(4) . .
C4 N2 C2 C13 -50.6(5) . .
C1 N2 C2 C3 -2.5(4) . .
C4 N2 C2 C3 -175.2(3) . .
C1 N1 C3 N1 112.4(4) . 6_565
C12 N1 C3 N1 -74.2(5) . 6_565
C1 N1 C3 C14 -121.2(4) . .
C12 N1 C3 C14 52.1(5) . .
C1 N1 C3 C2 2.5(4) . .
C12 N1 C3 C2 175.9(3) . .
N2 C2 C3 N1 0.0(3) 6_565 6_565
N2 C2 C3 N1 -117.7(3) . 6_565
C13 C2 C3 N1 121.1(2) . 6_565
N2 C2 C3 N1 117.7(3) 6_565 .
N2 C2 C3 N1 0.0(3) . .
C13 C2 C3 N1 -121.1(2) . .
N2 C2 C3 C14 -121.1(2) 6_565 .
N2 C2 C3 C14 121.1(2) . .
C13 C2 C3 C14 0.000(1) . .
C1 N2 C4 N3 101.3(4) . .
C2 N2 C4 N3 -86.6(4) . .
C5 N3 C4 N2 -108.6(4) . .
C7 N3 C4 N2 86.7(4) . .
C4 N3 C5 O2 7.1(6) . .
C7 N3 C5 O2 173.3(4) . .
C4 N3 C5 N4 -171.3(3) . .
C7 N3 C5 N4 -5.1(4) . .
C8 N4 C5 O2 -5.7(6) . .
C6 N4 C5 O2 -173.6(4) . .
C8 N4 C5 N3 172.7(3) . .
C6 N4 C5 N3 4.8(4) . .
C5 N4 C6 N4 -115.0(4) . 6_565
C8 N4 C6 N4 77.4(5) . 6_565
C5 N4 C6 C7 -2.6(4) . .
C8 N4 C6 C7 -170.3(3) . .
C5 N3 C7 N3 114.8(4) . 6_565
C4 N3 C7 N3 -79.0(5) . 6_565
C5 N3 C7 C6 3.3(4) . .
C4 N3 C7 C6 169.5(3) . .
N4 C6 C7 N3 -0.4(4) . .
N4 C6 C7 N3 120.1(3) 6_565 .
N4 C6 C7 N3 -120.1(3) . 6_565
N4 C6 C7 N3 0.4(4) 6_565 6_565
C9 N5 C8 N4 -108.8(4) . .
C11 N5 C8 N4 85.6(4) . .
C5 N4 C8 N5 108.7(4) . .
C6 N4 C8 N5 -84.9(4) . .
C8 N5 C9 O3 6.6(5) . .
C11 N5 C9 O3 173.8(4) . .
C8 N5 C9 N6 -171.9(3) . .
C11 N5 C9 N6 -4.8(4) . .
C12 N6 C9 O3 -7.7(6) 2_756 .
C10 N6 C9 O3 -173.9(4) . .
C12 N6 C9 N5 170.8(3) 2_756 .
C10 N6 C9 N5 4.6(4) . .
C9 N6 C10 N6 -114.8(4) . 6_565
C12 N6 C10 N6 79.0(5) 2_756 6_565
C9 N6 C10 C11 -2.7(4) . .
C12 N6 C10 C11 -168.9(3) 2_756 .
C9 N5 C11 N5 114.7(4) . 6_565
C8 N5 C11 N5 -78.5(5) . 6_565
C9 N5 C11 C10 3.0(4) . .
C8 N5 C11 C10 169.9(3) . .
N6 C10 C11 N5 0.2(3) 6_565 6_565
N6 C10 C11 N5 -119.7(3) . 6_565
N6 C10 C11 N5 119.7(3) 6_565 .
N6 C10 C11 N5 -0.2(3) . .
C1 N1 C12 N6 -100.7(4) . 2_756
C3 N1 C12 N6 86.5(4) . 2_756
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.001 -0.020 0.000 1231 447 ' '
2 0.500 0.000 0.500 120 12 ' '
3 1.000 0.500 0.500 120 12 ' '
