#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/19/2101965.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2101965
loop_
_publ_author_name
'Feng Xue'
'Thomas C. W. Mak'
_publ_section_title
;
 Channel- and layer-type anionic host structures in inclusion compounds
 of urea, tetraalkylammonium terephthalate/trimesate and water
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              142
_journal_page_last               154
_journal_paper_doi               10.1107/S0108768199011283
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac
'2[N(C4 H9)4]+,C8 H4 O4 2-,6(C H4 N2 O),2(H2 O)'
_chemical_formula_sum            'C46 H104 N14 O12'
_chemical_formula_weight         1045.43
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL97
_cell_angle_alpha                105.06(2)
_cell_angle_beta                 94.910(10)
_cell_angle_gamma                93.82(2)
_cell_formula_units_Z            1
_cell_length_a                   8.390(2)
_cell_length_b                   9.894(2)
_cell_length_c                   18.908(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      5
_cell_volume                     1503.6(6)
_computing_cell_refinement       'MSC/AFC (MSC, 1988)'
_computing_data_collection       'MSC/AFC (MSC, 1988)'
_computing_data_reduction        'MSC/AFC (MSC, 1988)'
_computing_molecular_graphics    'Siemens SHELXTL-PC (Siemens, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full .985
_diffrn_measured_fraction_theta_max .985
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
;
Rigaku RU-200 rotating-anode generator operated at 50kV and 90mA
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0185
_diffrn_reflns_av_sigmaI/netI    .0528
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5604
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        -.36
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .084
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  .951
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'psi scan (Kopfmann & Huber, 1968)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             574
_exptl_crystal_size_max          .40
_exptl_crystal_size_mid          .38
_exptl_crystal_size_min          .22
_refine_diff_density_max         .319
_refine_diff_density_min         -.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5277
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          .1041
_refine_ls_R_factor_gt           .0503
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0779P)²+0.1259P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1642
_reflns_number_gt                2982
_reflns_number_total             5277
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hr0043.cif
_cod_data_source_block           compd1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+0.1259P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+0.1259P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1503.6(2)
_cod_database_code               2101965
_cod_database_fobs_code          2101965
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
C1 .9589(3) .1839(2) -.03177(12) .0526(6) Uani d D 1 C
O1 .8567(2) .14061(17) .00384(9) .0605(4) Uani d D 1 O
N1 .9502(3) .3089(2) -.04676(11) .0653(6) Uani d D 1 N
H1A .8742 .3598 -.0319 .078 Uiso calc R 1 H
H1B 1.0207 .3380 -.0712 .078 Uiso calc R 1 H
N2 1.0768(2) .1074(2) -.05694(11) .0667(6) Uani d D 1 N
H2A 1.0841 .0263 -.0489 .080 Uiso calc R 1 H
H2B 1.1456 .1391 -.0813 .080 Uiso calc R 1 H
C2 .7819(3) .4801(2) .12811(12) .0482(5) Uani d D 1 C
O2 .7496(2) .48508(17) .06272(8) .0593(4) Uani d D 1 O
N3 .8076(2) .3595(2) .14417(10) .0610(5) Uani d D 1 N
H3A .8023 .2829 .1095 .073 Uiso calc R 1 H
H3B .8296 .3583 .1893 .073 Uiso calc R 1 H
N4 .7935(2) .5958(2) .18342(10) .0587(5) Uani d D 1 N
H4A .7788 .6755 .1748 .070 Uiso calc R 1 H
H4B .8157 .5912 .2279 .070 Uiso calc R 1 H
C3 .5428(3) -.1820(2) .09938(12) .0518(6) Uani d D 1 C
O3 .66105(19) -.15794(16) .14637(8) .0598(4) Uani d D 1 O
N5 .5029(3) -.3112(2) .05539(11) .0668(6) Uani d D 1 N
H5A .5594 -.3787 .0595 .080 Uiso calc R 1 H
H5B .4207 -.3269 .0230 .080 Uiso calc R 1 H
N6 .4510(3) -.0807(2) .09192(13) .0802(7) Uani d D 1 N
H6A .4734 .0033 .1200 .096 Uiso calc R 1 H
H6B .3694 -.0992 .0590 .096 Uiso calc R 1 H
C4 .8915(3) .4774(2) .34632(12) .0483(5) Uani d D 1 C
O4 .8560(2) .35831(18) .30353(9) .0752(6) Uani d D 1 O
O5 .8868(2) .59110(18) .32875(8) .0661(5) Uani d D 1 O
C5 .9462(2) .4881(2) .42630(11) .0416(5) Uani d D 1 C
C6 .9891(3) .6183(2) .47560(11) .0508(6) Uani d D 1 C
H6C .9820 .6991 .4595 .061 Uiso calc R 1 H
C7 .9575(3) .3699(2) .45156(12) .0510(6) Uani d D 1 C
H7 .9290 .2814 .4193 .061 Uiso calc R 1 H
N7 .3708(2) .67174(19) .29879(9) .0488(4) Uani d D 1 N
C8 .5364(3) .7504(2) .31717(12) .0518(6) Uani d D 1 C
H8A .6153 .6823 .3139 .062 Uiso calc R 1 H
H8B .5536 .8001 .2801 .062 Uiso calc R 1 H
C9 .5672(3) .8544(3) .39183(13) .0627(7) Uani d D 1 C
H9A .5534 .8065 .4299 .075 Uiso calc R 1 H
H9B .4907 .9247 .3960 .075 Uiso calc R 1 H
C10 .7370(3) .9250(3) .40214(15) .0677(7) Uani d D 1 C
H10A .8121 .8536 .3933 .081 Uiso calc R 1 H
H10B .7473 .9787 .3663 .081 Uiso calc R 1 H
C11 .7790(4) 1.0211(3) .47833(17) .0883(9) Uani d D 1 C
H11A .8869 1.0637 .4828 .132 Uiso calc R 1 H
H11B .7709 .9679 .5139 .132 Uiso calc R 1 H
H11C .7061 1.0930 .4869 .132 Uiso calc R 1 H
C12 .3359(3) .5858(2) .35255(12) .0527(6) Uani d D 1 C
H12A .3353 .6502 .4009 .063 Uiso calc R 1 H
H12B .2285 .5384 .3380 .063 Uiso calc R 1 H
C13 .4496(3) .4770(3) .35927(14) .0640(7) Uani d D 1 C
H13A .5540 .5231 .3821 .077 Uiso calc R 1 H
H13B .4628 .4183 .3107 .077 Uiso calc R 1 H
C14 .3828(3) .3866(3) .40587(15) .0697(7) Uani d D 1 C
H14A .3679 .4467 .4539 .084 Uiso calc R 1 H
H14B .2783 .3414 .3826 .084 Uiso calc R 1 H
C15 .4895(4) .2761(3) .41598(18) .0903(9) Uani d D 1 C
H15A .4417 .2225 .4457 .136 Uiso calc R 1 H
H15B .5925 .3201 .4400 .136 Uiso calc R 1 H
H15C .5028 .2148 .3688 .136 Uiso calc R 1 H
C16 .3691(3) .5771(3) .22132(12) .0555(6) Uani d D 1 C
H16A .3910 .6359 .1888 .067 Uiso calc R 1 H
H16B .4565 .5176 .2210 .067 Uiso calc R 1 H
C17 .2167(3) .4846(3) .18990(14) .0742(8) Uani d D 1 C
H17A .1298 .5423 .1845 .089 Uiso calc R 1 H
H17B .1885 .4294 .2233 .089 Uiso calc R 1 H
C18 .2381(4) .3874(3) .11571(15) .0789(8) Uani d D 1 C
H18A .1334 .3422 .0928 .095 Uiso calc R 1 H
H18B .2771 .4441 .0849 .095 Uiso calc R 1 H
C19 .3482(4) .2767(3) .11619(18) .0984(11) Uani d D 1 C
H19A .3531 .2214 .0667 .148 Uiso calc R 1 H
H19B .3094 .2173 .1451 .148 Uiso calc R 1 H
H19C .4536 .3196 .1371 .148 Uiso calc R 1 H
C20 .2394(3) .7721(2) .30362(13) .0562(6) Uani d D 1 C
H20A .1364 .7165 .2908 .067 Uiso calc R 1 H
H20B .2428 .8267 .3545 .067 Uiso calc R 1 H
C21 .2467(3) .8726(3) .25614(16) .0761(8) Uani d D 1 C
H21A .2298 .8209 .2046 .091 Uiso calc R 1 H
H21B .3517 .9251 .2653 .091 Uiso calc R 1 H
C22 .1143(4) .9754(4) .2745(2) .1171(13) Uani d D 1 C
H22A .0098 .9228 .2593 .176 Uiso calc R 1 H
H22B .1227 1.0153 .3274 .176 Uiso calc R 1 H
C23 .1241(6) 1.0900(4) .2389(3) .1418(16) Uani d D 1 C
H23A .0395 1.1492 .2524 .213 Uiso calc R 1 H
H23B .1131 1.0518 .1864 .213 Uiso calc R 1 H
H23C .2262 1.1443 .2544 .213 Uiso calc R 1 H
O1W .6301(3) .1113(3) .24613(15) .1206(9) Uani d . 1 O
H1WA .6772 .0456 .2198 .181 Uiso d R 1 H
H1WB .6899 .1880 .2571 .181 Uiso d R 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .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_site_symmetry_3
_geom_angle
O1 C1 N2 . 121.5(2)
O1 C1 N1 . 120.4(2)
N2 C1 N1 . 118.0(2)
O2 C2 N4 . 120.8(2)
O2 C2 N3 . 121.4(2)
N4 C2 N3 . 117.80(19)
O3 C3 N6 . 121.2(2)
O3 C3 N5 . 120.6(2)
N6 C3 N5 . 118.2(2)
O4 C4 O5 . 125.3(2)
O4 C4 C5 . 118.2(2)
O5 C4 C5 . 116.54(19)
C7 C5 C6 . 118.34(19)
C7 C5 C4 . 121.48(19)
C6 C5 C4 . 120.17(19)
C5 C6 C7 2_766 121.1(2)
C5 C7 C6 2_766 120.6(2)
C8 N7 C16 . 105.53(16)
C8 N7 C12 . 112.06(17)
C16 N7 C12 . 110.82(17)
C8 N7 C20 . 111.54(17)
C16 N7 C20 . 111.63(17)
C12 N7 C20 . 105.40(16)
C9 C8 N7 . 115.68(18)
C8 C9 C10 . 109.6(2)
C11 C10 C9 . 111.8(2)
C13 C12 N7 . 116.72(18)
C12 C13 C14 . 109.5(2)
C15 C14 C13 . 113.1(2)
C17 C16 N7 . 116.31(19)
C16 C17 C18 . 110.2(2)
C19 C18 C17 . 116.3(2)
C21 C20 N7 . 116.7(2)
C20 C21 C22 . 109.0(2)
C23 C22 C21 . 113.8(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 O1 . 1.253(3)
C1 N2 . 1.331(3)
C1 N1 . 1.344(3)
C2 O2 . 1.257(2)
C2 N4 . 1.326(3)
C2 N3 . 1.332(3)
C3 O3 . 1.240(3)
C3 N6 . 1.333(3)
C3 N5 . 1.334(3)
C4 O4 . 1.245(3)
C4 O5 . 1.255(3)
C4 C5 . 1.517(3)
C5 C7 . 1.380(3)
C5 C6 . 1.383(3)
C6 C7 2_766 1.384(3)
C7 C6 2_766 1.384(3)
N7 C8 . 1.513(3)
N7 C16 . 1.518(3)
N7 C12 . 1.520(3)
N7 C20 . 1.525(3)
C8 C9 . 1.505(3)
C9 C10 . 1.518(3)
C10 C11 . 1.503(4)
C12 C13 . 1.507(3)
C13 C14 . 1.523(3)
C14 C15 . 1.498(4)
C16 C17 . 1.503(3)
C17 C18 . 1.513(3)
C18 C19 . 1.481(4)
C20 C21 . 1.505(3)
C21 C22 . 1.556(4)
C22 C23 . 1.462(5)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1A O2 . .86 2.27 3.045(3) 149.2 yes
N1 H1B O2 2_765 .86 2.48 3.218(3) 144.2 yes
N2 H2A O1 2_755 .86 2.11 2.951(3) 164.4 yes
N2 H2B O3 2_755 .86 2.15 2.980(3) 163.4 yes
N3 H3A O1 . .86 2.23 3.037(3) 156.8 yes
N3 H3B O4 . .86 2.15 3.009(2) 173.4 yes
N4 H4A O3 1_565 .86 2.14 2.962(3) 160.7 yes
N4 H4B O5 . .86 1.95 2.805(2) 174.2 yes
N5 H5A O2 1_545 .86 2.16 3.003(3) 165.4 yes
N5 H5B O2 2_655 .86 2.26 3.024(2) 148.2 yes
N6 H6A O1W . .86 2.55 3.219(3) 135.1 yes
N6 H6B O1 2_655 .86 2.11 2.955(3) 168.8 yes
O1W H1WA O3 . .85 2.12 2.879(3) 148.6 yes
O1W H1WB O4 . .85 2.06 2.898(3) 167.0 yes
