#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/34/7103420.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_7103420
loop_
_publ_author_name
'Bardelang, David'
'Udachin, Konstantin A'
'Anedda, Roberto'
'Moudrakovski, Igor'
'Leek, Donald M'
'Ripmeester, John A'
'Ratcliffe, Christopher I'
_publ_section_title
;
 Single-crystal to single-crystal phase transition of cucurbit[5]uril
 hydrochloride hydrates: large water-filled channels transforming to
 layers of unusual stability.
;
_journal_issue                   40
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4927
_journal_page_last               4929
_journal_paper_doi               10.1039/b807033d
_journal_year                    2008
_chemical_formula_sum            'C30 H45 Cl2 N20 O17.5'
_chemical_formula_weight         1036.76
_chemical_name_common            cucurbit(5)uril
_chemical_name_systematic
;
?
;
_space_group_IT_number           31
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.280(4)
_cell_length_b                   11.560(3)
_cell_length_c                   13.183(3)
_cell_measurement_temperature    100.0(10)
_cell_volume                     2176.2(9)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'ATOMS V.5.0'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       ' φ & ω scans'
_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  0.1190
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15278
_diffrn_reflns_theta_full        23.42
_diffrn_reflns_theta_max         23.42
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_correction_T_min  0.8864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1078
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.386
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     172
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1535
_refine_ls_R_factor_gt           0.1102
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1580P)²+20.7790P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2653
_refine_ls_wR_factor_ref         0.3116
_reflns_number_gt                2378
_reflns_number_total             3289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b807033d.txt
_cod_data_source_block           dav6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_cell_measurement_temperature' value '100.0(1)K' was changed to
'100.0(10)' - the value should be numeric and without a unit
designator.

'_diffrn_ambient_temperature' value '100.0(1)K' was
changed to '100.0(10)' - the value should be numeric and without a
unit designator.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      Pmn2(1)
_cod_original_formula_sum        'C30 H45 Cl2 N20 O17.50'
_cod_database_code               7103420
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-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
O1 O 0.8907(2) -0.0772(3) 0.4072(2) 0.0359(10) Uani 1 1 d . . .
O2 O 0.8871(2) 0.1538(3) -0.0078(2) 0.0306(9) Uani 1 1 d U . .
O3 O 0.8201(2) 0.1741(3) 0.5076(3) 0.0320(8) Uani 1 1 d U . .
O4 O 0.8185(2) 0.3868(3) 0.0845(3) 0.0380(10) Uani 1 1 d . . .
O5 O 1.0000 0.3196(4) 0.5609(4) 0.0351(12) Uani 1 2 d SU . .
O6 O 1.0000 0.5311(4) 0.1430(4) 0.0439(17) Uani 1 2 d S . .
N1 N 0.9152(2) -0.1153(3) 0.2365(3) 0.0213(9) Uani 1 1 d U . .
N2 N 0.9141(3) -0.0200(3) 0.0717(3) 0.0255(11) Uani 1 1 d . . .
N3 N 0.7963(3) -0.0024(3) 0.2801(3) 0.0265(9) Uani 1 1 d U . .
N4 N 0.7845(3) 0.0768(3) 0.1109(3) 0.0268(9) Uani 1 1 d U . .
N5 N 0.7360(3) 0.1734(4) 0.3580(3) 0.0322(10) Uani 1 1 d U . .
N6 N 0.7392(3) 0.2589(4) 0.1872(3) 0.0333(10) Uani 1 1 d U . .
N7 N 0.7859(3) 0.3414(4) 0.4227(3) 0.0336(10) Uani 1 1 d U . .
N8 N 0.7870(3) 0.4259(3) 0.2510(3) 0.0372(13) Uani 1 1 d . . .
N9 N 0.9234(3) 0.4574(4) 0.4663(3) 0.0320(11) Uani 1 1 d U . .
N10 N 0.9208(3) 0.5422(4) 0.2977(3) 0.0369(12) Uani 1 1 d U . .
C1 C 1.0000 -0.1842(6) 0.2508(7) 0.042(2) Uani 1 2 d S . .
H1B H 1.0000 -0.2172 0.3201 0.050 Uiso 1 2 calc SR . .
H1A H 1.0000 -0.2492 0.2019 0.050 Uiso 1 2 calc SR . .
C2 C 0.8686(3) -0.0937(4) 0.1442(3) 0.0264(12) Uani 1 1 d U . .
H2 H 0.8487 -0.1679 0.1117 0.032 Uiso 1 1 calc R . .
C3 C 1.0000 -0.0517(6) 0.0151(5) 0.0288(19) Uani 1 2 d S . .
H3B H 1.0000 -0.0119 -0.0513 0.035 Uiso 1 2 calc SR . .
H3A H 1.0000 -0.1361 0.0024 0.035 Uiso 1 2 calc SR . .
C4 C 0.8715(3) -0.0673(4) 0.3186(3) 0.0266(12) Uani 1 1 d U . .
C5 C 0.7802(3) -0.0198(4) 0.1763(4) 0.0235(10) Uani 1 1 d U . .
H5 H 0.7211 -0.0644 0.1652 0.028 Uiso 1 1 calc R . .
C6 C 0.8680(3) 0.0785(4) 0.0532(3) 0.0242(10) Uani 1 1 d U . .
C7 C 0.7278(3) 0.0523(4) 0.3494(4) 0.0268(11) Uani 1 1 d U . .
H7B H 0.6639 0.0337 0.3254 0.032 Uiso 1 1 calc R . .
H7A H 0.7352 0.0178 0.4177 0.032 Uiso 1 1 calc R . .
C8 C 0.7206(4) 0.1746(4) 0.1116(4) 0.0354(11) Uani 1 1 d U . .
H8B H 0.7230 0.2126 0.0443 0.042 Uiso 1 1 calc R . .
H8A H 0.6561 0.1452 0.1214 0.042 Uiso 1 1 calc R . .
C9 C 0.7013(4) 0.2588(4) 0.2897(4) 0.0369(9) Uani 1 1 d U . .
H9 H 0.6314 0.2546 0.2868 0.044 Uiso 1 1 calc R . .
C10 C 0.7861(3) 0.2249(5) 0.4343(4) 0.0299(10) Uani 1 1 d U . .
C11 C 0.7306(4) 0.3728(5) 0.3336(4) 0.0392(10) Uani 1 1 d U . .
H11 H 0.6754 0.4217 0.3520 0.047 Uiso 1 1 calc R . .
C12 C 0.7855(4) 0.3584(4) 0.1664(4) 0.0332(11) Uani 1 1 d U . .
C13 C 0.8273(4) 0.4212(4) 0.4941(4) 0.0339(11) Uani 1 1 d U . .
H13B H 0.8288 0.3845 0.5619 0.041 Uiso 1 1 calc R . .
H13A H 0.7871 0.4908 0.4988 0.041 Uiso 1 1 calc R . .
C14 C 0.8273(4) 0.5399(5) 0.2529(4) 0.0439(17) Uani 1 1 d . . .
H14B H 0.7858 0.5919 0.2921 0.053 Uiso 1 1 calc R . .
H14A H 0.8309 0.5699 0.1827 0.053 Uiso 1 1 calc R . .
C15 C 1.0000 0.4006(6) 0.5048(6) 0.0278(15) Uani 1 2 d SU . .
C16 C 0.9426(3) 0.5558(4) 0.4037(4) 0.0331(15) Uani 1 1 d U . .
H16 H 0.9161 0.6288 0.4325 0.040 Uiso 1 1 calc R . .
C17 C 1.0000 0.5372(5) 0.2358(6) 0.035(2) Uani 1 2 d S . .
Cl1 Cl 1.0000 -0.06069(15) -0.26490(13) 0.0289(4) Uani 1 2 d SU A 1
Cl2 Cl 1.0000 0.53032(17) -0.21170(15) 0.0398(5) Uani 1 2 d SU B 2
O1W O 1.0000 0.3605(5) -0.0211(5) 0.0558(19) Uani 1 2 d S C 3
H1Y H 1.0000 0.2760 -0.0036 0.084 Uiso 1 2 d S D 3
H1W H 1.0000 0.4056 0.0394 0.084 Uiso 1 2 d S E 3
O2W O 1.0000 0.0758(5) 0.5278(4) 0.0526(19) Uani 1 2 d S F 4
H2Y H 1.0000 0.0274 0.4698 0.079 Uiso 1 2 d S G 4
H2W H 1.0000 0.0325 0.5918 0.079 Uiso 1 2 d S H 4
O3W O 1.0000 -0.3042(5) 0.5952(4) 0.0460(17) Uani 1 2 d S I 5
H3Y H 1.0000 -0.3593 0.6436 0.069 Uiso 1 2 d S J 5
H3W H 1.0000 -0.2237 0.6187 0.069 Uiso 1 2 d S K 5
O4W O 0.5000 0.7707(6) 0.2601(5) 0.074(2) Uani 1 2 d S L 6
H4Y H 0.5000 0.7391 0.3273 0.112 Uiso 1 2 d S M 6
H4W H 0.5000 0.7142 0.2011 0.112 Uiso 1 2 d S N 6
O5W O 0.6965(4) 0.7510(5) 0.3142(4) 0.0844(18) Uani 1 1 d . O 7
H5Y H 0.6543 0.7863 0.2705 0.127 Uiso 1 1 d . P 7
H5W H 0.6829 0.7760 0.3889 0.127 Uiso 1 1 d . Q 7
O6W O 0.9519(7) -0.3213(7) -0.0149(6) 0.064(3) Uani 0.50 1 d P . 8
H6W H 0.9566 -0.3661 0.0527 0.095 Uiso 0.50 1 d P R 8
H6Y H 1.0000 -0.3535 -0.0584 0.095 Uiso 1 2 d S S 8
O7W O 1.0137(7) 0.2150(8) 0.2868(9) 0.123(3) Uani 0.25 1 d PDU T -11
H7W H 1.0113 0.1508 0.3359 0.184 Uiso 0.25 1 d PD U -11
H7Y H 1.0749 0.2540 0.2932 0.184 Uiso 0.25 1 d PD V -11
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'
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
C4 N1 C2 113.3(4) . . ?
C4 N1 C1 119.8(5) . . ?
C2 N1 C1 126.8(5) . . ?
C6 N2 C2 113.8(4) . . ?
C6 N2 C3 121.8(4) . . ?
C2 N2 C3 124.2(4) . . ?
C5 N3 C4 113.7(4) . . ?
C5 N3 C7 123.8(4) . . ?
C4 N3 C7 120.7(4) . . ?
C5 N4 C6 112.1(4) . . ?
C5 N4 C8 125.7(4) . . ?
C6 N4 C8 121.5(4) . . ?
C10 N5 C7 122.3(4) . . ?
C10 N5 C9 110.1(4) . . ?
C7 N5 C9 127.5(4) . . ?
C12 N6 C8 122.1(4) . . ?
C12 N6 C9 111.7(4) . . ?
C8 N6 C9 125.6(4) . . ?
C10 N7 C13 124.1(4) . . ?
C10 N7 C11 109.8(4) . . ?
C13 N7 C11 125.9(4) . . ?
C12 N8 C14 123.0(4) . . ?
C12 N8 C11 110.8(4) . . ?
C14 N8 C11 125.6(4) . . ?
C15 N9 C16 116.0(4) . . ?
C15 N9 C13 120.9(4) . . ?
C16 N9 C13 123.0(4) . . ?
C17 N10 C16 113.3(5) . . ?
C17 N10 C14 120.2(4) . . ?
C16 N10 C14 126.3(4) . . ?
N1 C1 N1 111.9(5) 4_755 . ?
N1 C2 N2 117.7(4) . . ?
N1 C2 C5 104.0(4) . . ?
N2 C2 C5 102.6(4) . . ?
N2 C3 N2 111.8(5) . 4_755 ?
O1 C4 N1 128.7(4) . . ?
O1 C4 N3 125.1(4) . . ?
N1 C4 N3 106.2(4) . . ?
N3 C5 N4 118.4(4) . . ?
N3 C5 C2 102.0(4) . . ?
N4 C5 C2 103.2(4) . . ?
O2 C6 N2 128.3(4) . . ?
O2 C6 N4 123.7(4) . . ?
N2 C6 N4 107.7(4) . . ?
N5 C7 N3 114.8(4) . . ?
N6 C8 N4 114.9(4) . . ?
N5 C9 N6 117.3(4) . . ?
N5 C9 C11 105.6(4) . . ?
N6 C9 C11 104.8(4) . . ?
O3 C10 N7 124.3(5) . . ?
O3 C10 N5 125.1(5) . . ?
N7 C10 N5 110.4(4) . . ?
N7 C11 N8 113.5(4) . . ?
N7 C11 C9 104.1(4) . . ?
N8 C11 C9 103.4(4) . . ?
O4 C12 N6 126.4(5) . . ?
O4 C12 N8 124.4(5) . . ?
N6 C12 N8 109.1(4) . . ?
N7 C13 N9 113.5(4) . . ?
N8 C14 N10 112.9(4) . . ?
O5 C15 N9 127.1(3) . 4_755 ?
O5 C15 N9 127.1(3) . . ?
N9 C15 N9 105.7(6) 4_755 . ?
N9 C16 N10 115.5(4) . . ?
N9 C16 C16 101.1(2) . 4_755 ?
N10 C16 C16 102.5(3) . 4_755 ?
O6 C17 N10 125.9(3) . . ?
O6 C17 N10 125.9(3) . 4_755 ?
N10 C17 N10 108.2(6) . 4_755 ?
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
O1 C4 1.204(5) . ?
O2 C6 1.216(5) . ?
O3 C10 1.232(6) . ?
O4 C12 1.223(6) . ?
O5 C15 1.194(8) . ?
O6 C17 1.225(9) . ?
N1 C4 1.368(6) . ?
N1 C2 1.410(6) . ?
N1 C1 1.461(5) . ?
N2 C6 1.337(6) . ?
N2 C2 1.436(6) . ?
N2 C3 1.482(5) . ?
N3 C5 1.402(6) . ?
N3 C4 1.405(6) . ?
N3 C7 1.481(6) . ?
N4 C5 1.412(6) . ?
N4 C6 1.415(6) . ?
N4 C8 1.454(7) . ?
N5 C10 1.370(6) . ?
N5 C7 1.409(6) . ?
N5 C9 1.425(7) . ?
N6 C12 1.356(7) . ?
N6 C8 1.419(7) . ?
N6 C9 1.455(7) . ?
N7 C10 1.355(7) . ?
N7 C13 1.444(7) . ?
N7 C11 1.461(7) . ?
N8 C12 1.361(7) . ?
N8 C14 1.439(7) . ?
N8 C11 1.487(7) . ?
N9 C15 1.373(6) . ?
N9 C16 1.433(7) . ?
N9 C13 1.480(6) . ?
N10 C17 1.396(6) . ?
N10 C16 1.440(7) . ?
N10 C14 1.459(7) . ?
C1 N1 1.461(5) 4_755 ?
C2 C5 1.581(7) . ?
C3 N2 1.482(5) 4_755 ?
C9 C11 1.498(8) . ?
C15 N9 1.373(6) 4_755 ?
C16 C16 1.638(10) 4_755 ?
C17 N10 1.396(6) 4_755 ?
O6W O6W 1.374(19) 4_755 ?
