#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:03:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179360 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/57/4325749.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_4325749
loop_
_publ_author_name
'Wen-Jian Chen'
'Da-Hai Yu'
'Xin Xiao'
'Yun-Qian Zhang'
'Qian-Jiang Zhu'
'Sai-Feng Xue'
'Zhu Tao'
'Gang Wei'
_publ_section_title
;
 Difference of Coordination between Alkali- and Alkaline-Earth-Metal Ions
 to a Symmetrical α,α',δ,δ'-Tetramethylcucurbit[6]uril
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6956
_journal_page_last               6964
_journal_paper_doi               10.1021/ic200109s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C40 H56 N24 O18 Ba2 Cl2, Cl2, 8(H2 O)'
_chemical_formula_sum            'C40 H72 Ba2 Cl4 N24 O26'
_chemical_formula_weight         1721.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 117.976(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.055(6)
_cell_length_b                   10.464(2)
_cell_length_c                   16.667(4)
_cell_measurement_reflns_used    68
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      22.3
_cell_measurement_theta_min      1.78
_cell_volume                     3551.0(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker CCD Area Detector'
_diffrn_measurement_method       'φ and ω scan'
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12059
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    1.344
_exptl_absorpt_correction_T_max  0.7939
_exptl_absorpt_correction_T_min  0.7655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3335
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0499P)²+9.0717P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0944
_reflns_number_gt                3032
_reflns_number_total             3335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200109s_si_003_12.cif
_cod_data_source_block           complex12
_cod_original_cell_volume        3551.1(14)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4325749
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1W O 0.58391(17) 0.5000 0.7117(3) 0.0300(8) Uani 1 2 d S A .
O2W O 0.15242(17) 0.0000 0.5747(2) 0.0285(8) Uani 1 2 d S . .
O3W O 0.5000 0.3500(4) 0.5000 0.0349(10) Uani 0.90 2 d SP . .
O3W' O 0.5000 0.264(4) 0.5000 0.0349(10) Uani 0.10 2 d SP . .
Cl1 Cl 0.39412(11) 0.5000 0.7477(2) 0.0421(11) Uani 0.859(10) 2 d SP A 1
Cl1A Cl 0.4715(9) 0.5000 0.8130(11) 0.094(6) Uani 0.141(7) 2 d SP A 2
Cl1B Cl 0.3727(13) 0.5000 0.689(2) 0.094(6) Uani 0.119(9) 2 d SP A 3
Cl1C Cl 0.3952(13) 0.5000 0.8259(13) 0.25(2) Uani 0.192(10) 2 d SP B 4
Cl2 Cl 0.6157(4) 0.5000 0.8997(4) 0.156(3) Uani 0.686(8) 2 d SP C 5
Ba1 Ba 0.447888(13) 0.5000 0.603594(19) 0.02341(12) Uani 1 2 d S . .
C1 C 0.33641(15) 0.1858(3) 0.5400(2) 0.0201(7) Uani 1 1 d . . .
C2 C 0.3092(2) 0.0000 0.5945(3) 0.0163(9) Uani 1 2 d S . .
H2 H 0.2788 0.0000 0.6211 0.020 Uiso 1 2 calc SR A .
C3 C 0.2716(2) 0.0000 0.4891(3) 0.0169(9) Uani 1 2 d S . .
H3 H 0.2235 0.0000 0.4660 0.020 Uiso 1 2 calc SR . .
C4 C 0.26669(15) 0.1685(3) 0.3740(2) 0.0183(7) Uani 1 1 d . . .
H4A H 0.2193 0.1516 0.3424 0.022 Uiso 1 1 calc R A .
H4B H 0.2728 0.2614 0.3777 0.022 Uiso 1 1 calc R . .
C5 C 0.66310(15) 0.1839(3) 0.7012(2) 0.0186(7) Uani 1 1 d . . .
C6 C 0.2717(2) 0.0000 0.2678(3) 0.0159(9) Uani 1 2 d S . .
H6 H 0.2233 0.0000 0.2305 0.019 Uiso 1 2 calc SR A .
C7 C 0.6928(2) 0.0000 0.7920(3) 0.0171(9) Uani 1 2 d S . .
H7 H 0.7244 0.0000 0.8577 0.020 Uiso 1 2 calc SR . .
C8 C 0.62476(15) 0.1715(3) 0.8169(2) 0.0195(7) Uani 1 1 d . . .
H8A H 0.6551 0.1600 0.8817 0.023 Uiso 1 1 calc R . .
H8B H 0.6191 0.2636 0.8050 0.023 Uiso 1 1 calc R . .
C9 C 0.50490(16) 0.1814(3) 0.7468(2) 0.0189(7) Uani 1 1 d . . .
C10 C 0.5530(2) 0.0000 0.8396(3) 0.0176(9) Uani 1 2 d S . .
C11 C 0.4762(2) 0.0000 0.8054(3) 0.0177(9) Uani 1 2 d S . .
C12 C 0.38819(15) 0.1648(3) 0.7073(2) 0.0201(7) Uani 1 1 d . . .
H12A H 0.3897 0.2583 0.7054 0.024 Uiso 1 1 calc R A .
H12B H 0.3674 0.1415 0.7449 0.024 Uiso 1 1 calc R . .
C13 C 0.5959(3) 0.0000 0.9419(3) 0.0300(12) Uani 1 2 d S A .
H13A H 0.5888 0.0785 0.9670 0.045 Uiso 0.50 1 calc PR . .
H13B H 0.6417 -0.0060 0.9560 0.045 Uiso 0.50 1 calc PR . .
H13C H 0.5844 -0.0725 0.9679 0.045 Uiso 0.50 1 calc PR . .
C14 C 0.4559(2) 0.0000 0.8798(3) 0.0300(12) Uani 1 2 d S . .
H14A H 0.4707 0.0784 0.9147 0.045 Uiso 0.50 1 calc PR A .
H14B H 0.4756 -0.0727 0.9195 0.045 Uiso 0.50 1 calc PR . .
H14C H 0.4085 -0.0057 0.8527 0.045 Uiso 0.50 1 calc PR . .
N1 N 0.34778(13) 0.1174(3) 0.61573(18) 0.0202(6) Uani 1 1 d . A .
N2 N 0.29387(13) 0.1173(3) 0.46544(17) 0.0181(6) Uani 1 1 d . . .
N3 N 0.29555(13) 0.1164(2) 0.32086(18) 0.0182(6) Uani 1 1 d . . .
N4 N 0.65408(13) 0.1168(3) 0.76444(18) 0.0187(6) Uani 1 1 d . . .
N5 N 0.56184(13) 0.1163(3) 0.79736(18) 0.0185(6) Uani 1 1 d . A .
N6 N 0.45448(13) 0.1164(3) 0.74980(18) 0.0195(6) Uani 1 1 d . . .
O1 O 0.35804(12) 0.2921(2) 0.53910(16) 0.0273(6) Uani 1 1 d . A .
O2 O 0.50027(11) 0.2821(2) 0.70700(17) 0.0279(6) Uani 1 1 d . A .
O3 O 0.63894(12) 0.2885(2) 0.66970(17) 0.0272(6) Uani 1 1 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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 '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
O3W' O3W Ba1 121.87(7) . 5_666
O3W' O3W Ba1 121.87(7) . .
Ba1 O3W Ba1 116.25(14) 5_666 .
Cl1B Ba1 O2 82.7(4) . 6_565
Cl1B Ba1 O2 82.7(4) . .
O2 Ba1 O2 110.78(11) 6_565 .
Cl1B Ba1 O2W 98.3(7) . 7_556
O2 Ba1 O2W 124.48(5) 6_565 7_556
O2 Ba1 O2W 124.48(5) . 7_556
Cl1B Ba1 O1W 117.6(7) . .
O2 Ba1 O1W 64.42(6) 6_565 .
O2 Ba1 O1W 64.42(6) . .
O2W Ba1 O1W 144.08(10) 7_556 .
Cl1B Ba1 O1 70.5(4) . .
O2 Ba1 O1 153.16(7) 6_565 .
O2 Ba1 O1 68.48(7) . .
O2W Ba1 O1 60.19(6) 7_556 .
O1W Ba1 O1 130.01(5) . .
Cl1B Ba1 O1 70.5(4) . 6_565
O2 Ba1 O1 68.48(7) 6_565 6_565
O2 Ba1 O1 153.16(7) . 6_565
O2W Ba1 O1 60.19(6) 7_556 6_565
O1W Ba1 O1 130.01(5) . 6_565
O1 Ba1 O1 99.79(10) . 6_565
Cl1B Ba1 O3W 146.87(19) . .
O2 Ba1 O3W 128.24(7) 6_565 .
O2 Ba1 O3W 75.51(8) . .
O2W Ba1 O3W 74.90(6) 7_556 .
O1W Ba1 O3W 74.75(7) . .
O1 Ba1 O3W 78.33(8) . .
O1 Ba1 O3W 127.27(7) 6_565 .
Cl1B Ba1 O3W 146.87(18) . 5_666
O2 Ba1 O3W 75.51(8) 6_565 5_666
O2 Ba1 O3W 128.24(7) . 5_666
O2W Ba1 O3W 74.90(6) 7_556 5_666
O1W Ba1 O3W 74.75(7) . 5_666
O1 Ba1 O3W 127.27(7) . 5_666
O1 Ba1 O3W 78.33(8) 6_565 5_666
O3W Ba1 O3W 63.75(14) . 5_666
Cl1B Ba1 Cl1 14.2(6) . .
O2 Ba1 Cl1 74.97(6) 6_565 .
O2 Ba1 Cl1 74.97(6) . .
O2W Ba1 Cl1 112.57(9) 7_556 .
O1W Ba1 Cl1 103.35(9) . .
O1 Ba1 Cl1 79.19(6) . .
O1 Ba1 Cl1 79.19(6) 6_565 .
O3W Ba1 Cl1 147.82(7) . .
O3W Ba1 Cl1 147.82(7) 5_666 .
Cl1B Ba1 Cl1A 42.9(7) . .
O2 Ba1 Cl1A 61.98(13) 6_565 .
O2 Ba1 Cl1A 61.98(13) . .
O2W Ba1 Cl1A 141.2(3) 7_556 .
O1W Ba1 Cl1A 74.7(3) . .
O1 Ba1 Cl1A 97.5(2) . .
O1 Ba1 Cl1A 97.5(2) 6_565 .
O3W Ba1 Cl1A 135.2(2) . .
O3W Ba1 Cl1A 135.2(2) 5_666 .
Cl1 Ba1 Cl1A 28.6(3) . .
O1 C1 N1 125.9(3) . .
O1 C1 N2 126.0(3) . .
N1 C1 N2 108.0(3) . .
N1 C2 N1 114.7(3) . 6
N1 C2 C3 103.1(2) . .
N1 C2 C3 103.1(2) 6 .
N1 C2 H2 111.8 . .
N1 C2 H2 111.8 6 .
C3 C2 H2 111.8 . .
N2 C3 N2 115.2(4) . 6
N2 C3 C2 103.1(2) . .
N2 C3 C2 103.1(2) 6 .
N2 C3 H3 111.6 . .
N2 C3 H3 111.6 6 .
C2 C3 H3 111.6 . .
N3 C4 N2 114.2(3) . .
N3 C4 H4A 108.7 . .
N2 C4 H4A 108.7 . .
N3 C4 H4B 108.7 . .
N2 C4 H4B 108.7 . .
H4A C4 H4B 107.6 . .
O3 C5 N4 126.0(3) . .
O3 C5 N3 125.3(3) . 2_656
N4 C5 N3 108.7(3) . 2_656
N3 C6 N3 113.9(4) . 6
N3 C6 C7 103.1(2) . 5_656
N3 C6 C7 103.1(2) 6 5_656
N3 C6 H6 112.0 . .
N3 C6 H6 112.0 6 .
C7 C6 H6 112.0 5_656 .
N4 C7 N4 114.3(4) 6 .
N4 C7 C6 103.1(2) 6 5_656
N4 C7 C6 103.1(2) . 5_656
N4 C7 H7 111.9 6 .
N4 C7 H7 111.9 . .
C6 C7 H7 111.9 5_656 .
N5 C8 N4 114.0(3) . .
N5 C8 H8A 108.7 . .
N4 C8 H8A 108.7 . .
N5 C8 H8B 108.7 . .
N4 C8 H8B 108.7 . .
H8A C8 H8B 107.6 . .
O2 C9 N5 125.4(3) . .
O2 C9 N6 126.1(3) . .
N5 C9 N6 108.6(3) . .
N5 C10 N5 112.1(3) 6 .
N5 C10 C13 112.1(2) 6 .
N5 C10 C13 112.1(2) . .
N5 C10 C11 102.1(2) 6 .
N5 C10 C11 102.1(2) . .
C13 C10 C11 115.6(4) . .
N6 C11 N6 112.0(4) 6 .
N6 C11 C14 111.7(2) 6 .
N6 C11 C14 111.7(2) . .
N6 C11 C10 102.7(2) 6 .
N6 C11 C10 102.7(2) . .
C14 C11 C10 115.3(4) . .
N6 C12 N1 113.9(3) . .
N6 C12 H12A 108.8 . .
N1 C12 H12A 108.8 . .
N6 C12 H12B 108.8 . .
N1 C12 H12B 108.8 . .
H12A C12 H12B 107.7 . .
C10 C13 H13A 109.5 . .
C10 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C10 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C11 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C1 N1 C12 122.9(3) . .
C1 N1 C2 112.8(3) . .
C12 N1 C2 124.0(3) . .
C1 N2 C4 122.1(3) . .
C1 N2 C3 112.9(3) . .
C4 N2 C3 124.3(3) . .
C5 N3 C4 123.5(3) 2_656 .
C5 N3 C6 112.4(3) 2_656 .
C4 N3 C6 122.6(3) . .
C5 N4 C8 123.1(3) . .
C5 N4 C7 112.6(3) . .
C8 N4 C7 122.1(3) . .
C9 N5 C8 120.8(3) . .
C9 N5 C10 113.6(3) . .
C8 N5 C10 124.9(3) . .
C9 N6 C12 122.1(3) . .
C9 N6 C11 113.0(3) . .
C12 N6 C11 124.8(3) . .
C1 O1 Ba1 157.0(2) . .
C9 O2 Ba1 161.5(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1W Ba1 2.789(4) .
O2W Ba1 2.780(4) 7_556
O3W O3W' 0.90(4) .
O3W Ba1 2.972(2) 5_666
O3W Ba1 2.972(2) .
Cl1 Ba1 3.177(2) .
Cl1A Ba1 3.270(17) .
Cl1B Ba1 2.71(3) .
Ba1 O2 2.771(2) 6_565
Ba1 O2 2.771(2) .
Ba1 O2W 2.780(4) 7_556
Ba1 O1 2.844(2) .
Ba1 O1 2.844(2) 6_565
Ba1 O3W 2.972(2) 5_666
C1 O1 1.222(4) .
C1 N1 1.365(4) .
C1 N2 1.371(4) .
C2 N1 1.459(3) .
C2 N1 1.459(3) 6
C2 C3 1.553(6) .
C2 H2 0.9900 .
C3 N2 1.454(3) .
C3 N2 1.454(3) 6
C3 H3 0.9900 .
C4 N3 1.441(4) .
C4 N2 1.452(4) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C5 O3 1.229(4) .
C5 N4 1.361(4) .
C5 N3 1.368(4) 2_656
C6 N3 1.454(3) .
C6 N3 1.454(3) 6
C6 C7 1.559(6) 5_656
C6 H6 0.9900 .
C7 N4 1.455(4) 6
C7 N4 1.455(4) .
C7 C6 1.559(6) 5_656
C7 H7 0.9900 .
C8 N5 1.449(4) .
C8 N4 1.451(4) .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C9 O2 1.223(4) .
C9 N5 1.363(4) .
C9 N6 1.368(4) .
C10 N5 1.467(4) 6
C10 N5 1.467(4) .
C10 C13 1.517(7) .
C10 C11 1.585(6) .
C11 N6 1.469(4) 6
C11 N6 1.469(4) .
C11 C14 1.518(6) .
C12 N6 1.442(4) .
C12 N1 1.452(4) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C13 H13C 0.9700 .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C14 H14C 0.9700 .
N3 C5 1.368(4) 2_656
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 -0.005 -0.014 0.000 879 324 ' '
2 0.500 0.000 0.500 94 15 ' '
3 1.000 0.500 0.500 94 15 ' '
