##############################################################################
# #
# This CIF contains the data in a paper accepted for publication in #
# Acta Crystallographica Section E. It conforms to the requirements of #
# Notes for Authors for Acta Crystallographica Section E, and has been #
# peer reviewed under the auspices of the IUCr Commission on Journals. #
# #
# Full details of the Crystallographic Information File format #
# are given in the paper "The Crystallographic Information File (CIF): #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H. #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. #
# #
# The current version of the core CIF dictionary is obtainable from #
# ftp://ftp.iucr.org/pub/cif_core.dic. #
# #
# Software is freely available for graphical display of the structure(s) #
# in this CIF. For information consult the CIF software page #
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# #
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data_General
_journal_date_recd_electronic 2017-11-01
_journal_date_accepted 2017-11-03
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2017
_journal_volume 73
_journal_issue 12
_journal_page_first 1840
_journal_page_last 1844
_journal_paper_category GO
_journal_paper_doi 10.1107/S2056989017015997
_journal_coeditor_code LH5860
_publ_contact_author_name ' Prof. Hiroyuki Ishida'
_publ_contact_author_address
;
Department of Chemistry
Faculty of Science
Okayama University
Okayama 700-8530
Japan
;
_publ_contact_author_email ' ishidah@cc.okayama-u.ac.jp '
_publ_contact_author_fax ' 81-86-251-7832'
_publ_contact_author_phone ' 81-86-251-7832'
_publ_section_title
;
Crystal structures of two 1:2 dihydrate compounds of chloranilic acid with
2-carboxypyridine and 2-carboxyquinoline
;
loop_
_publ_author_name
_publ_author_address
'Gotoh, Kazuma'
;
Department of Chemistry
Faculty of Science
Okayama University
Okayama 700-8530
Japan
;
'Ishida, Hiroyuki'
;
Department of Chemistry
Faculty of Science
Okayama University
Okayama 700-8530
Japan
;
_publ_section_synopsis
;
Crystal structures of hydrogen-bonded 1:2 dihydrate compounds of chloranilic
acid with 2-carboxypyridine (I) and 2-carboxyquinoline (II) have been
determined at 180 and 200 K, respectively. The base molecule in (I) is
disordered over cationic and twitterionic states, while that in (II) is in a
twitterionic form. In each crystal, the three components are linked by
O---H...O and N---H...O hydrogen bonds, forming a layer structure.
;
data_I
_chemical_name_systematic
;
Bis(2-carboxypyridinium) chloranilate dihydrate--bis(pyridinium-2-carboxylate)
chloranilic acid dihydrate (1/1)
;
_chemical_formula_moiety '2(C6 H5.5 N O2), C6 H Cl2 O4, 2(H2 O)'
_chemical_formula_sum 'C18 H16 Cl2 N2 O10'
_chemical_formula_iupac '2C6 H5.5 N O2 0.5+, C6 H Cl2 O4 -, 2H2 O'
_chemical_formula_weight 491.24
_chemical_melting_point ?
_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.
;
_space_group_crystal_system monoclinic
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 15.1028(10)
_cell_length_b 3.6851(3)
_cell_length_c 17.5689(13)
_cell_angle_alpha 90.0000
_cell_angle_beta 101.871(3)
_cell_angle_gamma 90.0000
_cell_volume 956.89(12)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 15838
_cell_measurement_theta_min 3.21
_cell_measurement_theta_max 30.02
_cell_measurement_temperature 180(2)
_exptl_crystal_description block
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.350
_exptl_crystal_size_mid 0.180
_exptl_crystal_size_min 0.130
_exptl_crystal_density_diffrn 1.705
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 504.00
_exptl_absorpt_coefficient_mu 0.404
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
(NUMABS; Higashi, 1999)
;
_exptl_absorpt_correction_T_min 0.896
_exptl_absorpt_correction_T_max 0.949
_diffrn_ambient_temperature 180(2)
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71075
_diffrn_measurement_device_type 'Rigaku R-AXIS RAPIDII'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number 17752
_diffrn_reflns_av_R_equivalents 0.0211
_diffrn_reflns_theta_min 3.245
_diffrn_reflns_theta_max 30.015
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_k_max 4
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 24
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_decay_% ?
_reflns_number_total 2789
_reflns_number_gt 2537
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all 0.0332
_refine_ls_R_factor_gt 0.0297
_refine_ls_wR_factor_gt 0.0775
_refine_ls_wR_factor_ref 0.0793
_refine_ls_goodness_of_fit_ref 1.108
_refine_ls_restrained_S_all 1.107
_refine_ls_number_reflns 2789
_refine_ls_number_parameters 176
_refine_ls_number_restraints 8
_refine_ls_hydrogen_treatment mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.3065P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.537
_refine_diff_density_min -0.237
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
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'
'N' 'N' 0.0061 0.0033
'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'
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2010) and PLATON (Spek, 2015)
;
loop_
_atom_site_type_symbol
_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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl Cl1 0.48813(2) 0.21752(7) 0.32764(2) 0.01728(8) Uani d 1 . .
O O1 0.64061(5) 0.6016(2) 0.43110(4) 0.02004(16) Uani d 1 . .
O O2 0.34886(5) 0.1370(2) 0.42588(4) 0.02038(17) Uani d 1 . .
H H2 0.317(2) 0.137(9) 0.4593(16) 0.031 Uiso d 0.5 . .
O O3 0.06134(7) 0.3759(3) 0.54909(5) 0.0313(2) Uani d 1 . .
H H3 0.018(2) 0.445(12) 0.516(2) 0.047 Uiso d 0.5 . .
O O4 -0.03494(6) 0.1653(3) 0.62162(5) 0.0303(2) Uani d 1 . .
O O5A 0.19794(11) 0.1042(7) 0.48308(10) 0.0265(4) Uani d 0.5 A 1
H H9A 0.1547(18) 0.038(11) 0.4493(18) 0.040 Uiso d 0.5 B 1
H H10A 0.2453(15) 0.043(11) 0.4682(18) 0.040 Uiso d 0.5 C 1
O O5B 0.20132(11) -0.1191(6) 0.48529(9) 0.0199(3) Uani d 0.5 D 2
H H9B 0.1501(15) -0.090(9) 0.4587(19) 0.030 Uiso d 0.5 E 2
H H10B 0.209(2) -0.347(5) 0.4873(19) 0.030 Uiso d 0.5 F 2
N N1 0.19857(6) 0.0209(3) 0.63805(5) 0.01977(18) Uani d 1 . .
C C1 0.57374(6) 0.5511(3) 0.45987(5) 0.01438(18) Uani d 1 . .
C C2 0.49294(7) 0.3688(3) 0.42158(5) 0.01476(18) Uani d 1 . .
C C3 0.42138(6) 0.3090(3) 0.45734(6) 0.01574(19) Uani d 1 . .
C C4 0.12231(7) 0.0793(3) 0.66495(6) 0.01658(19) Uani d 1 . .
C C5 0.12193(7) 0.0166(3) 0.74206(6) 0.0198(2) Uani d 1 . .
H H5 0.068573 0.056090 0.761605 0.024 Uiso calc 1 . .
C C6 0.20078(8) -0.1057(3) 0.79117(6) 0.0226(2) Uani d 1 . .
H H6 0.201710 -0.146932 0.844701 0.027 Uiso calc 1 . .
C C7 0.27772(7) -0.1668(3) 0.76174(7) 0.0226(2) Uani d 1 . .
H H7 0.331694 -0.251819 0.794609 0.027 Uiso calc 1 . .
C C8 0.27478(7) -0.1023(3) 0.68384(7) 0.0236(2) Uani d 1 . .
H H8 0.326860 -0.145258 0.662656 0.028 Uiso calc 1 . .
C C9 0.04024(8) 0.2152(3) 0.60747(6) 0.0210(2) Uani d 1 . .
H H1 0.1993(12) 0.049(5) 0.5876(10) 0.039(4) Uiso d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cl1 0.01956(13) 0.02040(13) 0.01184(12) -0.00159(8) 0.00314(8) -0.00202(8)
O1 0.0170(3) 0.0273(4) 0.0174(3) -0.0029(3) 0.0071(3) -0.0028(3)
O2 0.0159(3) 0.0286(4) 0.0168(3) -0.0068(3) 0.0037(3) -0.0038(3)
O3 0.0340(5) 0.0363(5) 0.0200(4) -0.0003(4) -0.0028(3) 0.0107(4)
O4 0.0212(4) 0.0433(5) 0.0243(4) 0.0042(4) -0.0003(3) 0.0001(4)
O5A 0.0152(8) 0.0467(13) 0.0185(8) -0.0033(8) 0.0052(6) -0.0080(8)
O5B 0.0160(7) 0.0243(9) 0.0188(7) -0.0013(7) 0.0028(5) -0.0010(7)
N1 0.0231(4) 0.0215(4) 0.0160(4) 0.0002(4) 0.0071(3) -0.0002(3)
C1 0.0148(4) 0.0154(4) 0.0132(4) 0.0008(3) 0.0035(3) 0.0012(3)
C2 0.0171(4) 0.0174(4) 0.0100(4) -0.0015(3) 0.0033(3) -0.0007(3)
C3 0.0147(4) 0.0186(5) 0.0137(4) 0.0012(4) 0.0025(3) 0.0021(3)
C4 0.0177(4) 0.0163(4) 0.0151(4) -0.0002(4) 0.0022(3) 0.0005(3)
C5 0.0183(4) 0.0251(5) 0.0166(4) 0.0003(4) 0.0052(3) 0.0026(4)
C6 0.0236(5) 0.0271(6) 0.0163(4) -0.0015(4) 0.0018(4) 0.0051(4)
C7 0.0185(5) 0.0209(5) 0.0261(5) 0.0010(4) -0.0009(4) 0.0032(4)
C8 0.0197(5) 0.0245(5) 0.0281(5) 0.0025(4) 0.0083(4) -0.0013(4)
C9 0.0241(5) 0.0207(5) 0.0156(4) 0.0022(4) -0.0017(4) -0.0013(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cl1 C2 . 1.7293(9) ?
O1 C1 . 1.2330(11) ?
O2 C3 . 1.2875(12) ?
O2 H2 . 0.830(18) ?
O3 C9 . 1.2801(14) ?
O3 H3 . 0.814(17) ?
O4 C9 . 1.2250(15) ?
O5A H9A . 0.824(18) ?
O5A H10A . 0.841(18) ?
O5B H9B . 0.824(17) ?
O5B H10B . 0.849(17) ?
N1 C8 . 1.3406(14) ?
N1 C4 . 1.3492(13) ?
N1 H1 . 0.895(18) ?
C1 C2 . 1.4335(13) ?
C1 C3 3_666 1.5307(13) ?
C2 C3 . 1.3751(13) ?
C4 C5 . 1.3754(13) ?
C4 C9 . 1.5139(14) ?
C5 C6 . 1.3939(15) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.3840(16) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.3808(16) ?
C7 H7 . 0.9500 ?
C8 H8 . 0.9500 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C3 O2 H2 . . 105(2) ?
C9 O3 H3 . . 115(3) ?
H9A O5A H10A . . 107(3) ?
H9B O5B H10B . . 105(3) ?
C8 N1 C4 . . 122.23(9) ?
C8 N1 H1 . . 116.7(11) ?
C4 N1 H1 . . 120.9(11) ?
O1 C1 C2 . . 124.63(9) ?
O1 C1 C3 . 3_666 117.08(9) ?
C2 C1 C3 . 3_666 118.29(8) ?
C3 C2 C1 . . 122.26(8) ?
C3 C2 Cl1 . . 120.12(8) ?
C1 C2 Cl1 . . 117.62(7) ?
O2 C3 C2 . . 124.19(9) ?
O2 C3 C1 . 3_666 116.38(8) ?
C2 C3 C1 . 3_666 119.43(8) ?
N1 C4 C5 . . 119.67(9) ?
N1 C4 C9 . . 117.38(9) ?
C5 C4 C9 . . 122.95(9) ?
C4 C5 C6 . . 119.20(9) ?
C4 C5 H5 . . 120.4 ?
C6 C5 H5 . . 120.4 ?
C7 C6 C5 . . 119.83(10) ?
C7 C6 H6 . . 120.1 ?
C5 C6 H6 . . 120.1 ?
C8 C7 C6 . . 118.95(10) ?
C8 C7 H7 . . 120.5 ?
C6 C7 H7 . . 120.5 ?
N1 C8 C7 . . 120.11(10) ?
N1 C8 H8 . . 119.9 ?
C7 C8 H8 . . 119.9 ?
O4 C9 O3 . . 128.74(11) ?
O4 C9 C4 . . 118.74(10) ?
O3 C9 C4 . . 112.51(10) ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1 C1 C2 C3 . . . . 177.79(10) ?
C3 C1 C2 C3 3_666 . . . -1.60(16) ?
O1 C1 C2 Cl1 . . . . -1.39(14) ?
C3 C1 C2 Cl1 3_666 . . . 179.22(7) ?
C1 C2 C3 O2 . . . . -177.81(10) ?
Cl1 C2 C3 O2 . . . . 1.35(15) ?
C1 C2 C3 C1 . . . 3_666 1.61(16) ?
Cl1 C2 C3 C1 . . . 3_666 -179.22(7) ?
C8 N1 C4 C5 . . . . 0.93(17) ?
C8 N1 C4 C9 . . . . -179.41(10) ?
N1 C4 C5 C6 . . . . 0.18(17) ?
C9 C4 C5 C6 . . . . -179.46(10) ?
C4 C5 C6 C7 . . . . -0.86(17) ?
C5 C6 C7 C8 . . . . 0.46(18) ?
C4 N1 C8 C7 . . . . -1.34(17) ?
C6 C7 C8 N1 . . . . 0.62(18) ?
N1 C4 C9 O4 . . . . 157.55(11) ?
C5 C4 C9 O4 . . . . -22.81(16) ?
N1 C4 C9 O3 . . . . -23.17(14) ?
C5 C4 C9 O3 . . . . 156.48(11) ?
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 H1 O5A . 0.895(17) 1.843(17) 2.7380(19) 179(2) y
N1 H1 O5B . 0.895(17) 1.907(17) 2.7417(18) 154.4(17) y
O2 H2 O5B . 0.83(3) 2.12(3) 2.8111(19) 141(3) y
O3 H3 O3 3_566 0.82(3) 1.62(4) 2.4352(14) 174(4) y
O5A H9A O4 3_556 0.82(3) 2.11(3) 2.927(2) 170(3) y
O5B H9B O4 3_556 0.82(3) 2.02(3) 2.8159(19) 162(3) y
O5A H10A O2 . 0.84(3) 1.90(3) 2.6762(19) 154(4) y
O5B H10B O1 3_656 0.848(19) 2.60(3) 3.095(2) 119(2) y
C8 H8 Cl1 3_656 0.95 2.78 3.6524(12) 154 y
C8 H8 O1 3_656 0.95 2.47 3.1871(14) 132 y
_shelx_hkl_file
;
-2 0 -1 21.69 5.50
2 0 1 23.06 6.99
2 0 1 34.44 3.76
-2 0 -1 1.46 1.89
-2 0 261237.80 819.65
2 0 -261096.95 816.78
2 0 -262212.39 831.13
-2 0 260990.95 814.27
-1 0 3 2.61 6.23
1 0 -3 5.97 6.81
-1 0 3 -0.29 12.41
1 0 -3 -0.53 7.07
0 0 3 1.70 9.77
0 0 3 1.78 6.72
0 0 -3 0.23 10.51
0 0 -3 3.24 6.62
2 0 2 357.05 12.03
-2 0 -2 359.13 13.91
2 0 2 335.41 14.24
2 0 2 327.78 19.35
-2 0 3 115.18 11.49
2 0 -3 137.93 10.93
2 0 -3 101.58 11.81
-2 0 3 77.27 18.88
3 0 -1 4.92 7.80
-3 0 1 4.01 12.87
-3 0 1 4.43 4.58
3 0 -1 2.26 4.27
1 0 3 2.85 8.83
1 0 3 -1.00 5.49
-1 0 -3 5.58 7.08
-1 0 -3 -1.26 11.95
-3 0 026367.08 344.24
-3 0 026241.47 319.78
3 0 026376.20 324.42
3 0 025726.05 329.03
-3 0 234159.70 446.11
-3 0 234274.69 446.90
3 0 -233619.91 439.10
3 0 -233707.14 436.18
-3 0 -1 5.73 3.88
3 0 1 5.19 7.54
-3 0 -1 3.30 7.92
3 0 1 1.95 3.61
1 0 -4 3781.80 65.52
1 0 -4 3685.24 55.79
-1 0 4 3767.21 54.75
-1 0 4 3719.01 67.59
0 0 4 2543.74 39.07
0 0 -4 2566.75 40.05
0 0 -4 2465.49 40.40
0 0 4 2511.50 52.48
-3 0 3 -0.10 8.97
3 0 -3 29.73 11.16
3 0 -3 1.87 8.68
-3 0 3 17.90 10.39
-2 0 -3 6.94 8.03
2 0 3 1.83 7.00
2 0 3 5.44 7.72
-2 0 -3 3.06 7.10
2 0 -459612.95 809.78
2 0 -456577.20 771.21
-2 0 458124.96 792.39
-2 0 458328.52 793.92
3 0 230373.75 385.68
-3 0 -229988.89 390.87
-3 0 -230268.86 384.22
3 0 229622.38 386.07
-1 0 -4 1166.94 24.32
-1 0 -4 1120.52 24.71
1 0 4 1097.22 24.75
1 0 4 1124.74 23.51
-4 0 1 6.22 5.57
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1 -3 18 233.88 54.80
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14 -2 12 1606.02 85.46
-5 -5 1 927.16 72.28
-14 -2 -12 1563.60 58.57
-5 -5 1 756.05 70.15
5 -5 -1 669.93 43.74
-14 -2 -12 1555.67 60.25
14 -1 14 1103.49 69.77
-14 -1 -14 1132.46 61.71
14 -1 14 1036.85 68.00
14 1 14 1040.36 74.76
14 1 14 1147.12 74.70
-14 -1 -14 1083.51 45.72
-13 -4 0 76.55 79.15
-19 0 15 -11.99 22.70
-13 -4 0 104.05 47.35
13 -4 0 60.40 57.54
19 0 -15 1.84 23.32
-19 0 15 10.85 38.63
19 0 -15 21.96 42.43
13 -4 0 68.53 36.76
5 -5 -2 101.16 30.32
-8 4 14 1096.79 58.25
5 -5 -2 65.60 49.69
8 4 -14 906.44 71.62
-5 -5 2 89.42 48.07
-5 -5 2 92.52 51.92
-8 -4 14 1155.96 57.29
-8 -4 14 1187.69 115.82
8 -4 -14 958.34 87.12
8 4 -14 972.35 49.35
6 -1 -24 766.86 83.70
-7 0 -21 -20.52 50.60
6 1 -24 802.59 71.02
7 0 21 49.53 36.61
-6 1 24 842.96 86.47
-9 -4 -9 -11.01 40.67
-6 1 24 719.46 67.27
7 0 21 15.46 33.94
6 1 -24 803.61 70.73
-9 -4 -9 -1.70 62.88
-6 -1 24 683.53 71.70
-6 -1 24 895.54 67.39
7 0 21 -2.55 27.98
6 -1 -24 815.41 69.78
5 -5 0 383.01 38.50
-5 -5 0 685.98 103.12
-5 -5 0 513.39 63.34
-3 -5 -4 551.84 66.25
3 -5 4 464.74 42.80
7 -2 19 959.81 76.47
7 2 19 1067.50 95.80
5 -5 0 453.86 58.11
3 -5 4 601.44 72.00
-7 -2 -19 926.09 64.89
2 1 23 572.97 48.79
2 -1 23 714.90 52.86
2 1 23 783.64 61.06
-2 1 -23 775.79 84.16
2 -1 23 648.46 67.27
-2 -1 -23 622.84 68.33
-2 1 -23 751.95 62.32
-2 -1 -23 772.05 99.07
18 1 -16 821.27 84.56
-18 1 16 745.65 41.95
18 -1 -16 800.45 66.04
18 -1 -16 1018.62 110.40
-18 -1 16 818.06 54.38
-18 1 16 807.90 105.75
-18 -1 16 841.29 67.99
1 -5 -6 239.00 76.82
-1 -5 6 419.47 52.15
-1 -5 6 372.03 51.79
-20 1 11 188.70 56.75
-20 -1 11 180.97 31.85
-14 -3 -8 31.34 54.21
20 -1 -11 142.06 61.94
-20 -1 11 117.90 79.80
14 -3 8 45.61 43.21
20 1 -11 179.69 33.61
20 1 -11 150.58 50.91
-14 -3 -8 8.58 54.44
14 -3 8 21.94 72.22
-17 -3 7 148.37 44.58
-17 -3 7 172.48 30.84
-17 -3 7 6.49 74.36
17 3 -7 217.24 32.05
6 -4 -15 598.56 56.76
17 -3 -7 131.39 47.78
-19 -1 14 1782.80 121.04
-6 4 15 646.97 56.35
-6 -4 15 737.15 100.99
6 4 -15 498.93 59.68
-19 -1 14 1757.80 67.06
6 4 -15 581.96 68.50
20 0 3 -13.67 33.87
19 -1 -14 1833.41 94.21
-17 3 7 199.36 75.76
19 1 -14 1902.85 90.95
20 0 3 -15.54 34.69
-19 1 14 1819.74 86.82
19 1 -14 1804.40 71.39
-6 -4 15 659.73 51.89
-16 3 11 457.12 52.27
16 3 -11 403.10 60.30
19 0 6 128.99 43.85
19 0 6 261.73 44.09
-16 -3 11 467.08 42.30
-16 -3 11 492.32 57.43
16 3 -11 456.91 42.33
16 -3 -11 456.41 83.58
-16 -3 11 485.69 58.68
-3 -3 20 497.28 61.75
-3 -3 20 374.00 85.24
3 3 -20 387.41 52.09
3 3 -20 450.98 86.11
-4 -3 20 147.65 50.59
4 3 -20 155.44 47.10
-3 3 20 388.99 95.97
-4 3 20 119.50 54.69
-4 -3 20 352.68 60.40
4 -3 -20 109.06 53.59
2 -5 5 532.57 46.57
3 -3 -20 311.88 96.67
-2 -5 -5 644.16 64.32
2 -5 5 620.09 49.11
4 3 -20 148.40 47.17
-15 -3 -6 4670.34 120.10
15 -3 6 4854.07 177.82
-15 -3 -6 4579.89 119.51
15 -3 6 4836.39 137.26
11 -4 6 60.93 60.25
-11 -4 -6 60.56 48.76
11 -4 6 2.24 36.21
-11 -4 -6 78.68 77.23
-2 -5 6 152.64 47.67
-5 -5 3 -3.91 38.71
2 -5 -6 250.87 45.36
5 -5 -3 29.82 27.53
-17 -3 1 1326.73 94.84
5 -5 -3 33.61 44.08
-2 -5 6 187.06 46.89
17 -3 -1 1353.71 72.86
-17 -3 1 1384.21 64.90
17 -3 -1 1316.65 71.71
-5 -5 3 43.19 61.83
2 1 -24 160.34 50.24
0 -5 -6 12.74 36.46
2 -1 -24 144.99 89.73
-2 1 24 217.68 88.09
2 1 -24 200.13 80.29
-2 1 24 246.66 42.40
0 -5 6 11.71 33.34
-2 -1 24 182.69 55.88
2 -1 -24 164.75 37.16
-2 -1 24 279.22 51.15
0 -5 6 26.66 52.91
-21 0 8 114.83 79.79
-4 -5 -3 1135.49 118.53
2 -3 19 899.55 112.35
2 3 19 928.07 73.02
4 -5 3 885.32 47.10
4 -5 3 918.10 49.11
-2 3 -19 815.94 62.02
-2 -3 -19 874.80 72.24
2 -3 19 864.04 49.78
-4 -5 -3 1170.88 78.47
-2 3 -19 804.29 50.04
19 -1 5 605.43 62.29
-21 0 2 1485.04 76.87
19 1 5 500.78 70.56
19 -1 5 483.16 98.71
21 0 -2 1361.64 74.95
19 1 5 516.73 46.47
18 0 -17 27.79 28.95
-18 0 17 -0.10 36.82
18 0 -17 -8.28 45.54
-18 0 17 -1.98 32.60
-17 2 15 4.89 63.65
-13 -3 16 1346.24 98.96
-17 -2 15 40.16 37.63
-13 -3 16 1290.84 123.77
13 -3 -16 1321.82 80.95
17 2 -15 28.71 63.14
17 -2 -15 28.74 71.78
-13 3 16 1348.55 84.53
-17 -2 15 19.22 38.80
13 3 -16 1163.27 79.41
-13 3 16 1241.43 53.63
13 3 -16 1316.24 66.40
17 2 -15 32.43 40.12
13 -3 -16 1295.53 90.08
-11 -2 21 37.83 45.49
4 -5 -5 77.69 57.09
-11 -2 21 26.09 42.99
-4 -5 5 158.76 49.98
-11 2 21 29.86 50.37
11 -2 -21 42.02 34.63
11 2 -21 24.42 44.46
11 2 -21 12.34 45.02
-4 -5 5 202.95 49.50
11 -2 -21 42.37 64.66
-11 2 21 -1.56 35.36
5 -5 1 21.51 25.94
-5 -5 -1 18.01 38.82
5 -5 1 48.14 25.84
-5 -5 -1 -10.38 36.93
-5 -3 20 3469.35 156.75
-5 3 20 3378.03 111.57
1 -4 15 281.52 47.98
-5 -3 20 3537.47 110.42
-1 -4 -15 191.70 54.96
5 3 -20 3561.16 109.61
1 4 15 163.53 54.51
-1 4 -15 203.61 38.08
-1 -4 -15 198.87 51.85
5 3 -20 3368.22 108.01
5 -3 -20 3420.92 152.30
1 -4 15 184.28 38.96
-12 -3 17 846.26 75.50
-5 -4 -13 1401.31 82.41
12 -4 4 485.81 52.25
-12 3 17 845.11 51.77
-12 3 17 846.28 73.37
-2 -3 20 103.42 51.78
2 3 -20 107.47 46.50
-2 3 20 123.58 51.03
5 -4 13 1328.68 73.35
-12 -3 17 875.21 61.29
12 -3 -17 840.78 50.11
12 3 -17 820.93 91.76
9 0 -24 1284.67 75.99
9 0 -24 1230.99 77.06
-12 -4 -4 314.85 60.37
-2 -3 20 122.52 43.05
-5 -4 -13 1280.34 79.81
-12 -4 -4 389.61 93.79
12 -4 4 427.85 50.62
5 4 13 1443.23 82.26
2 -3 -20 110.01 52.75
2 3 -20 140.07 43.18
-9 0 24 1155.53 75.21
12 -3 -17 919.24 80.27
12 3 -17 778.10 74.12
-13 -4 7 250.82 63.52
16 0 12 0.04 66.67
13 -4 -7 286.59 40.81
16 0 12 145.87 62.46
-13 -4 7 229.60 61.09
-6 -3 -17 3365.81 107.62
6 3 17 3698.37 116.54
18 2 -13 543.28 55.66
18 2 -13 505.55 53.24
-11 0 -18 1214.99 48.65
6 -3 17 3761.12 122.90
-18 -2 13 587.56 53.33
-18 2 13 610.74 60.62
18 -2 -13 610.86 63.70
-18 -2 13 625.22 54.05
6 -3 17 4960.47 185.21
-15 1 20 2188.21 75.33
-15 -1 20 2216.23 94.22
15 -1 -20 2313.36 81.06
-15 1 20 2091.43 87.15
-15 -1 20 2235.54 86.82
15 1 -20 2267.52 125.25
15 -1 -20 2361.20 95.78
15 1 -20 2467.63 100.67
1 2 22 391.64 58.67
-1 2 -22 264.04 56.01
-1 -2 -22 339.20 60.21
1 -2 22 372.53 71.23
-1 2 -22 323.70 46.13
1 -2 22 229.76 61.86
-16 -2 -9 143.05 31.81
16 -2 9 41.23 45.21
16 -2 9 -2.45 43.73
-16 -2 -9 135.93 31.61
3 -5 -6 12.40 50.77
16 1 -19 -0.40 41.47
7 -1 -24 189.37 43.26
16 -1 -19 -6.98 39.04
7 1 -24 173.93 56.04
-7 -1 24 190.01 55.68
-7 -1 24 160.58 53.16
-16 1 19 9.14 26.70
-3 -5 6 19.46 36.89
16 1 -19 8.09 56.11
-3 -5 6 13.91 63.53
-7 1 24 142.67 51.90
-16 -1 19 1.40 32.81
-16 -1 19 7.64 37.75
7 1 -24 164.64 54.06
-7 1 24 166.33 42.75
7 -1 -24 151.02 55.13
16 -1 -19 -15.54 29.36
-17 -2 -7 2652.83 73.36
17 -2 7 2707.16 105.84
-17 -2 -7 2762.57 72.84
17 -2 7 2966.54 108.41
13 -4 1 395.07 46.51
13 -4 1 404.52 49.31
-13 -4 -1 436.81 59.90
13 0 16 4229.94 115.25
1 -5 6 -8.55 51.13
5 -5 -4 120.60 50.78
-9 3 19 531.13 37.49
-19 -2 10 893.15 55.45
-19 -2 10 899.49 57.82
-19 -2 10 934.60 80.83
19 -2 -10 924.82 73.62
-9 -3 19 0.15 95.25
19 2 -10 883.73 57.37
9 3 -19 555.26 64.98
19 2 -10 955.65 57.71
8 1 20 2448.55 100.24
8 1 20 2558.89 80.55
8 -1 20 2570.18 66.90
-8 -1 -20 2456.53 80.29
-8 1 -20 2622.51 92.44
8 1 20 2342.40 70.51
-19 -2 -1 324.36 52.94
19 2 1 218.14 34.36
20 0 -13 41.92 26.10
;
_shelx_hkl_checksum 21605
_shelx_res_file
;
TITL 09031018
shelxl.res
created by SHELXL-2016/6 at 11:48:49 on 22-Oct-2017
CELL 0.71075 15.10281 3.68511 17.56890 90.000 101.871 90.000
ZERR 2 0.00099 0.00023 0.00130 0.000 0.002 0.000
LATT 1
SYMM -X, .50+Y, .50-Z
SFAC C H O N CL
UNIT 36 32 20 4 4
SHEL 99999.000000 0.000000
L.S. 20
FMAP 2
PLAN -25
WPDB -2
HTAB
BOND $H
CONF
LIST 4
TEMP -93.0
ACTA
SIZE 0.130 0.180 0.350
DFIX 0.8400 0.0200 O3 H3
DFIX 0.8400 0.0200 O5B H10B
DFIX 0.8400 0.0200 O2 H2
DFIX 0.8400 0.0200 O5A H10A
DFIX 0.8400 0.0200 O5A H9A
DFIX 0.8400 0.0200 O5B H9B
DFIX 1.3700 0.0400 H9A H10A
DFIX 1.3700 0.0400 H9B H10B
WGHT 0.044500 0.306500
FVAR 3.25368
CL1 5 0.488132 0.217524 0.327641 11.00000 0.01956 0.02040 =
0.01184 -0.00202 0.00314 -0.00159
O1 3 0.640607 0.601636 0.431097 11.00000 0.01696 0.02728 =
0.01743 -0.00277 0.00711 -0.00293
O2 3 0.348858 0.137043 0.425881 11.00000 0.01590 0.02865 =
0.01677 -0.00376 0.00374 -0.00676
H2 2 0.317159 0.137351 0.459275 10.50000 -1.50000
O3 3 0.061336 0.375889 0.549090 11.00000 0.03397 0.03626 =
0.01999 0.01067 -0.00283 -0.00033
H3 2 0.018351 0.445230 0.516456 10.50000 -1.50000
O4 3 -0.034939 0.165268 0.621616 11.00000 0.02115 0.04332 =
0.02430 0.00009 -0.00026 0.00417
PART 1
O5A 3 0.197943 0.104240 0.483078 10.50000 0.01516 0.04673 =
0.01850 -0.00804 0.00517 -0.00327
H9A 2 0.154664 0.038190 0.449276 10.50000 -1.50000
H10A 2 0.245290 0.042718 0.468225 10.50000 -1.50000
PART 2
O5B 3 0.201318 -0.119114 0.485292 10.50000 0.01605 0.02433 =
0.01884 -0.00100 0.00276 -0.00134
H9B 2 0.150146 -0.089755 0.458667 10.50000 -1.50000
H10B 2 0.209391 -0.347230 0.487275 10.50000 -1.50000
PART 0
N1 4 0.198569 0.020868 0.638046 11.00000 0.02306 0.02152 =
0.01604 -0.00025 0.00707 0.00024
C1 1 0.573737 0.551052 0.459874 11.00000 0.01475 0.01544 =
0.01323 0.00118 0.00351 0.00082
C2 1 0.492941 0.368794 0.421577 11.00000 0.01708 0.01740 =
0.01003 -0.00073 0.00333 -0.00150
C3 1 0.421381 0.308980 0.457341 11.00000 0.01468 0.01863 =
0.01373 0.00212 0.00250 0.00125
C4 1 0.122308 0.079288 0.664949 11.00000 0.01773 0.01633 =
0.01515 0.00051 0.00216 -0.00017
C5 1 0.121932 0.016567 0.742055 11.00000 0.01835 0.02514 =
0.01663 0.00255 0.00523 0.00028
AFIX 43
H5 2 0.068573 0.056090 0.761605 11.00000 -1.20000
AFIX 0
C6 1 0.200782 -0.105682 0.791166 11.00000 0.02359 0.02709 =
0.01626 0.00507 0.00185 -0.00150
AFIX 43
H6 2 0.201710 -0.146932 0.844701 11.00000 -1.20000
AFIX 0
C7 1 0.277719 -0.166814 0.761736 11.00000 0.01850 0.02086 =
0.02612 0.00316 -0.00087 0.00098
AFIX 43
H7 2 0.331694 -0.251819 0.794609 11.00000 -1.20000
AFIX 0
C8 1 0.274785 -0.102297 0.683837 11.00000 0.01973 0.02448 =
0.02811 -0.00133 0.00832 0.00247
AFIX 43
H8 2 0.326860 -0.145258 0.662656 11.00000 -1.20000
AFIX 0
C9 1 0.040236 0.215196 0.607473 11.00000 0.02413 0.02070 =
0.01562 -0.00128 -0.00171 0.00225
H1 2 0.199309 0.049284 0.587587 11.00000 0.03888
HKLF 4
REM 09031018
REM R1 = 0.0297 for 2537 Fo > 4sig(Fo) and 0.0332 for all 2789 data
REM 176 parameters refined using 8 restraints
END
WGHT 0.0442 0.3075
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, -y+1, -z+1
HTAB O2 O1_$1
HTAB O2 O5A
HTAB O2 O5B
EQIV $2 -x, -y+1, -z+1
HTAB O3 O3_$2
EQIV $3 -x, -y, -z+1
HTAB O5A O4_$3
HTAB O5A O2
HTAB O5B O4_$3
EQIV $4 -x+1, -y, -z+1
HTAB O5B O1_$4
EQIV $5 -x, y-1/2, -z+3/2
HTAB C5 O4_$5
EQIV $6 x, -y-1/2, z+1/2
HTAB C7 Cl1_$6
HTAB C8 Cl1_$4
HTAB C8 O1_$4
HTAB N1 O5A
HTAB N1 O5B
REM Highest difference peak 0.537, deepest hole -0.237, 1-sigma level 0.071
Q1 1 0.5306 0.4651 0.4408 11.00000 0.05 0.54
Q2 1 0.4601 0.3246 0.4401 11.00000 0.05 0.49
Q3 1 0.8779 0.9745 0.2993 11.00000 0.05 0.49
Q4 1 0.8350 1.0555 0.2357 11.00000 0.05 0.47
Q5 1 0.5729 0.6248 0.5013 11.00000 0.05 0.46
Q6 1 0.9160 0.8450 0.3625 11.00000 0.05 0.46
Q7 1 0.7646 1.1588 0.2284 11.00000 0.05 0.44
Q8 1 0.7321 1.1280 0.2789 11.00000 0.05 0.41
Q9 1 0.8416 0.9523 0.3474 11.00000 0.05 0.40
Q10 1 0.4934 0.2628 0.3809 11.00000 0.05 0.33
Q11 1 0.7614 1.0445 0.3361 11.00000 0.05 0.33
Q12 1 0.5982 0.5925 0.4385 11.00000 0.05 0.33
Q13 1 1.0015 0.8890 0.3954 11.00000 0.05 0.28
Q14 1 0.9527 0.7521 0.4288 11.00000 0.05 0.27
Q15 1 1.0329 0.8964 0.3602 11.00000 0.05 0.27
Q16 1 1.0031 0.7410 0.3784 11.00000 0.05 0.27
Q17 1 0.3471 0.0899 0.3897 11.00000 0.05 0.27
Q18 1 0.3896 0.2320 0.4376 11.00000 0.05 0.26
Q19 1 0.5382 0.2189 0.3244 11.00000 0.05 0.24
Q20 1 0.6256 0.5966 0.3866 11.00000 0.05 0.23
Q21 1 0.9027 0.6105 0.4589 11.00000 0.05 0.22
Q22 1 0.9623 0.7365 0.4681 11.00000 0.05 0.21
Q23 1 0.3279 0.1413 0.4277 11.00000 0.05 0.21
Q24 1 0.4287 0.1541 0.3154 11.00000 0.05 0.20
Q25 1 0.6908 1.0300 0.3559 11.00000 0.05 0.19
;
_shelx_res_checksum 11940
data_II
_chemical_name_systematic
;
chloranilic acid--2-carboxyquinoline (1/2) dihydrate
;
_chemical_formula_moiety '2(C10 H7 N O2), C6 H2 Cl2 O4, 2(H2 O)'
_chemical_formula_sum 'C26 H20 Cl2 N2 O10'
_chemical_formula_iupac '2C10 H7 N O2, C6 H2 Cl2 O4, 2H2 O'
_chemical_formula_weight 591.36
_chemical_melting_point ?
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 4.4745(2)
_cell_length_b 10.5448(8)
_cell_length_c 13.6111(6)
_cell_angle_alpha 96.652(4)
_cell_angle_beta 94.109(3)
_cell_angle_gamma 99.009(4)
_cell_volume 627.38(6)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 9714
_cell_measurement_theta_min 3.02
_cell_measurement_theta_max 30.14
_cell_measurement_temperature 200(2)
_exptl_crystal_description platelet
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.410
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_min 0.030
_exptl_crystal_density_diffrn 1.565
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 304.00
_exptl_absorpt_coefficient_mu 0.323
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
(NUMABS; Higashi, 1999)
;
_exptl_absorpt_correction_T_min 0.925
_exptl_absorpt_correction_T_max 0.990
_diffrn_ambient_temperature 200(2)
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71075
_diffrn_measurement_device_type 'Rigaku R-AXIS RAPIDII'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number 12358
_diffrn_reflns_av_R_equivalents 0.1217
_diffrn_reflns_theta_min 3.026
_diffrn_reflns_theta_max 30.034
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_decay_% ?
_reflns_number_total 3666
_reflns_number_gt 2755
_reflns_threshold_expression 'I > 2\s(I)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all 0.0722
_refine_ls_R_factor_gt 0.0524
_refine_ls_wR_factor_gt 0.1388
_refine_ls_wR_factor_ref 0.1493
_refine_ls_goodness_of_fit_ref 1.005
_refine_ls_restrained_S_all 1.005
_refine_ls_number_reflns 3666
_refine_ls_number_parameters 197
_refine_ls_number_restraints 2
_refine_ls_hydrogen_treatment mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0879P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.518
_refine_diff_density_min -0.450
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
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'
'N' 'N' 0.0061 0.0033
'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'
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2010) and PLATON (Spek, 2015)
;
loop_
_atom_site_type_symbol
_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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl Cl1 0.49390(9) 0.23664(4) -0.02842(3) 0.04300(16) Uani d 1 . .
O O1 0.0319(3) 0.08081(12) -0.17653(8) 0.0426(3) Uani d 1 . .
O O2 0.4150(3) 0.11710(11) 0.15510(9) 0.0391(3) Uani d 1 . .
O O3 -0.1769(3) 0.36216(11) 0.47121(9) 0.0372(3) Uani d 1 . .
O O4 -0.0712(3) 0.16160(11) 0.43604(9) 0.0425(3) Uani d 1 . .
O O5 0.3938(3) 0.07471(12) 0.33231(9) 0.0406(3) Uani d 1 . .
N N1 0.3233(3) 0.41970(12) 0.60390(9) 0.0298(3) Uani d 1 . .
C C1 0.0207(3) 0.04635(14) -0.09469(11) 0.0317(3) Uani d 1 . .
C C2 0.2276(3) 0.10762(14) -0.00985(11) 0.0320(3) Uani d 1 . .
C C3 0.2197(3) 0.06514(14) 0.07971(11) 0.0313(3) Uani d 1 . .
C C4 0.2151(3) 0.29703(14) 0.56909(11) 0.0305(3) Uani d 1 . .
C C5 0.3274(3) 0.19702(15) 0.61140(11) 0.0336(3) Uani d 1 . .
H H5 0.250293 0.109195 0.586437 0.040 Uiso calc 1 . .
C C6 0.5493(4) 0.22680(15) 0.68906(12) 0.0342(3) Uani d 1 . .
H H6 0.622423 0.159293 0.719133 0.041 Uiso calc 1 . .
C C7 0.6694(3) 0.35659(14) 0.72449(11) 0.0312(3) Uani d 1 . .
C C8 0.9050(4) 0.39332(16) 0.80217(12) 0.0363(3) Uani d 1 . .
H H8 0.985438 0.328869 0.834065 0.044 Uiso calc 1 . .
C C9 1.0170(4) 0.52094(18) 0.83147(13) 0.0411(4) Uani d 1 . .
H H9 1.175836 0.545100 0.883608 0.049 Uiso calc 1 . .
C C10 0.8980(4) 0.61764(17) 0.78463(13) 0.0418(4) Uani d 1 . .
H H10 0.980263 0.706066 0.805678 0.050 Uiso calc 1 . .
C C11 0.6677(4) 0.58722(15) 0.70983(13) 0.0372(3) Uani d 1 . .
H H11 0.587483 0.653070 0.679646 0.045 Uiso calc 1 . .
C C12 0.5532(3) 0.45558(14) 0.67897(10) 0.0294(3) Uani d 1 . .
C C13 -0.0333(3) 0.27243(14) 0.48397(11) 0.0315(3) Uani d 1 . .
H H1 0.252(5) 0.481(2) 0.5760(17) 0.055(6) Uiso d 1 . .
H H2 0.359(7) 0.083(3) 0.216(2) 0.092(10) Uiso d 1 . .
H H3 0.255(4) 0.086(2) 0.3667(15) 0.054(6) Uiso d 1 . .
H H4 0.560(4) 0.111(2) 0.3651(17) 0.063(7) Uiso d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cl1 0.0402(2) 0.0380(2) 0.0465(2) -0.00570(16) -0.00095(18) 0.00725(17)
O1 0.0451(7) 0.0452(7) 0.0354(6) 0.0008(5) -0.0026(5) 0.0093(5)
O2 0.0388(6) 0.0380(6) 0.0359(6) -0.0005(5) -0.0079(5) 0.0012(4)
O3 0.0376(6) 0.0319(6) 0.0427(6) 0.0068(4) -0.0017(5) 0.0089(4)
O4 0.0403(6) 0.0368(6) 0.0471(6) 0.0091(5) -0.0071(5) -0.0052(5)
O5 0.0400(7) 0.0419(7) 0.0357(6) 0.0047(5) -0.0066(5) -0.0029(5)
N1 0.0302(6) 0.0269(6) 0.0326(6) 0.0053(5) 0.0020(5) 0.0055(5)
C1 0.0292(7) 0.0304(7) 0.0353(7) 0.0061(5) -0.0004(6) 0.0039(6)
C2 0.0287(7) 0.0274(7) 0.0384(7) 0.0022(5) -0.0010(6) 0.0032(5)
C3 0.0298(7) 0.0278(7) 0.0354(7) 0.0064(5) -0.0016(6) 0.0007(5)
C4 0.0297(7) 0.0291(7) 0.0330(7) 0.0046(5) 0.0044(6) 0.0045(5)
C5 0.0347(7) 0.0273(7) 0.0384(7) 0.0043(5) 0.0005(6) 0.0051(5)
C6 0.0357(7) 0.0301(7) 0.0378(7) 0.0059(6) 0.0020(6) 0.0089(6)
C7 0.0299(7) 0.0315(7) 0.0325(7) 0.0047(5) 0.0039(6) 0.0054(5)
C8 0.0347(7) 0.0388(8) 0.0353(7) 0.0063(6) 0.0011(6) 0.0060(6)
C9 0.0358(8) 0.0453(9) 0.0382(8) 0.0033(7) -0.0036(7) -0.0030(7)
C10 0.0402(8) 0.0329(8) 0.0484(9) 0.0026(6) 0.0006(7) -0.0046(7)
C11 0.0376(8) 0.0289(7) 0.0443(8) 0.0061(6) 0.0027(7) 0.0014(6)
C12 0.0281(6) 0.0287(7) 0.0311(6) 0.0044(5) 0.0042(6) 0.0021(5)
C13 0.0293(7) 0.0311(7) 0.0339(7) 0.0037(5) 0.0024(6) 0.0058(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cl1 C2 . 1.7174(15) ?
O1 C1 . 1.2130(18) ?
O2 C3 . 1.3070(17) ?
O2 H2 . 0.98(3) ?
O3 C13 . 1.2453(18) ?
O4 C13 . 1.2512(18) ?
O5 H3 . 0.821(16) ?
O5 H4 . 0.848(16) ?
N1 C4 . 1.3270(19) ?
N1 C12 . 1.3722(19) ?
N1 H1 . 0.88(2) ?
C1 C2 . 1.447(2) ?
C1 C3 2 1.507(2) ?
C2 C3 . 1.348(2) ?
C4 C5 . 1.401(2) ?
C4 C13 . 1.517(2) ?
C5 C6 . 1.370(2) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.405(2) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.413(2) ?
C7 C12 . 1.420(2) ?
C8 C9 . 1.363(2) ?
C8 H8 . 0.9500 ?
C9 C10 . 1.415(3) ?
C9 H9 . 0.9500 ?
C10 C11 . 1.368(2) ?
C10 H10 . 0.9500 ?
C11 C12 . 1.406(2) ?
C11 H11 . 0.9500 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C3 O2 H2 . . 111.3(18) ?
H3 O5 H4 . . 108(2) ?
C4 N1 C12 . . 122.93(13) ?
C4 N1 H1 . . 119.1(16) ?
C12 N1 H1 . . 117.9(16) ?
O1 C1 C2 . . 123.09(14) ?
O1 C1 C3 . 2 118.94(13) ?
C2 C1 C3 . 2 117.97(13) ?
C3 C2 C1 . . 122.39(13) ?
C3 C2 Cl1 . . 120.62(11) ?
C1 C2 Cl1 . . 116.98(11) ?
O2 C3 C2 . . 122.30(14) ?
O2 C3 C1 . 2 118.13(13) ?
C2 C3 C1 . 2 119.57(12) ?
N1 C4 C5 . . 120.22(13) ?
N1 C4 C13 . . 116.94(13) ?
C5 C4 C13 . . 122.84(13) ?
C6 C5 C4 . . 119.50(14) ?
C6 C5 H5 . . 120.2 ?
C4 C5 H5 . . 120.2 ?
C5 C6 C7 . . 120.39(14) ?
C5 C6 H6 . . 119.8 ?
C7 C6 H6 . . 119.8 ?
C6 C7 C8 . . 123.01(14) ?
C6 C7 C12 . . 118.61(13) ?
C8 C7 C12 . . 118.37(14) ?
C9 C8 C7 . . 120.18(15) ?
C9 C8 H8 . . 119.9 ?
C7 C8 H8 . . 119.9 ?
C8 C9 C10 . . 120.32(15) ?
C8 C9 H9 . . 119.8 ?
C10 C9 H9 . . 119.8 ?
C11 C10 C9 . . 121.78(15) ?
C11 C10 H10 . . 119.1 ?
C9 C10 H10 . . 119.1 ?
C10 C11 C12 . . 118.00(15) ?
C10 C11 H11 . . 121.0 ?
C12 C11 H11 . . 121.0 ?
N1 C12 C11 . . 120.39(13) ?
N1 C12 C7 . . 118.27(13) ?
C11 C12 C7 . . 121.34(14) ?
O3 C13 O4 . . 128.04(14) ?
O3 C13 C4 . . 117.19(13) ?
O4 C13 C4 . . 114.76(13) ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1 C1 C2 C3 . . . . -177.43(15) ?
C3 C1 C2 C3 2 . . . 2.8(2) ?
O1 C1 C2 Cl1 . . . . 1.2(2) ?
C3 C1 C2 Cl1 2 . . . -178.60(10) ?
C1 C2 C3 O2 . . . . 177.00(13) ?
Cl1 C2 C3 O2 . . . . -1.6(2) ?
C1 C2 C3 C1 . . . 2 -2.8(2) ?
Cl1 C2 C3 C1 . . . 2 178.61(10) ?
C12 N1 C4 C5 . . . . 2.4(2) ?
C12 N1 C4 C13 . . . . -178.34(12) ?
N1 C4 C5 C6 . . . . 0.1(2) ?
C13 C4 C5 C6 . . . . -179.12(14) ?
C4 C5 C6 C7 . . . . -1.6(2) ?
C5 C6 C7 C8 . . . . -177.95(14) ?
C5 C6 C7 C12 . . . . 0.8(2) ?
C6 C7 C8 C9 . . . . 178.31(16) ?
C12 C7 C8 C9 . . . . -0.4(2) ?
C7 C8 C9 C10 . . . . 0.2(3) ?
C8 C9 C10 C11 . . . . 0.5(3) ?
C9 C10 C11 C12 . . . . -1.0(3) ?
C4 N1 C12 C11 . . . . 177.18(14) ?
C4 N1 C12 C7 . . . . -3.2(2) ?
C10 C11 C12 N1 . . . . -179.65(14) ?
C10 C11 C12 C7 . . . . 0.7(2) ?
C6 C7 C12 N1 . . . . 1.5(2) ?
C8 C7 C12 N1 . . . . -179.66(13) ?
C6 C7 C12 C11 . . . . -178.84(14) ?
C8 C7 C12 C11 . . . . 0.0(2) ?
N1 C4 C13 O3 . . . . -19.8(2) ?
C5 C4 C13 O3 . . . . 159.47(14) ?
N1 C4 C13 O4 . . . . 161.50(14) ?
C5 C4 C13 O4 . . . . -19.3(2) ?
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 H1 O3 2_566 0.88(2) 1.91(2) 2.7724(17) 167(2) y
O2 H2 O5 . 0.98(3) 1.59(3) 2.5092(17) 155(3) y
O5 H3 O4 . 0.819(19) 2.011(19) 2.8072(19) 164(2) y
O5 H4 O4 1_655 0.85(2) 1.82(2) 2.6632(19) 171(2) y
C6 H6 O1 1_656 0.95 2.54 3.392(2) 150 y
C6 H6 O5 2_656 0.95 2.47 3.211(2) 134 y
_shelx_hkl_file
;
0 0 2 4755.67 193.27
0 0 -2 5483.62 262.86
0 0 -2 5340.64 254.51
0 1 -233502.57 2166.09
0 -1 234818.66 2292.70
0 1 -236186.92 2366.67
0 -1 231944.92 2006.17
0 1 220229.56 1172.73
0 1 221383.57 1188.53
0 -1 -222118.93 1356.99
0 -1 -221397.90 1213.10
0 -2 0 1661.56 98.18
0 2 0 1486.51 83.40
0 2 0 1676.21 120.30
0 -2 0 2009.57 104.68
0 -2 136557.80 2546.59
0 -2 136890.55 2504.70
0 2 -129316.96 1869.18
0 2 -131902.20 2091.17
0 -2 -1 151.49 49.82
0 2 1 125.08 36.78
0 2 1 149.11 29.90
0 -2 -1 146.07 47.31
0 0 -3 1189.04 69.92
0 0 3 1153.75 67.55
0 0 -3 1159.43 69.43
1 0 0 2110.06 108.65
-1 0 0 2383.76 209.51
-1 0 0 2131.58 157.61
1 0 0 2367.41 141.95
0 2 -2 203747. 22315.
0 -2 2 157128. 16163.
0 -2 2 171211. 18011.
0 2 -2 183603. 20139.
0 -1 3 59.07 17.39
0 1 -3 99.88 35.16
0 1 -3 110.43 34.26
0 -1 3 107.10 32.90
1 -1 013718.62 748.12
1 -1 013057.20 720.78
-1 1 011145.56 632.98
-1 1 011775.13 626.93
-1 0 1 6289.68 437.45
-1 0 1 6611.54 437.31
1 0 -1 6779.84 375.17
1 0 -1 6219.23 402.35
1 -1 -1 684.38 72.88
-1 1 1 669.35 46.84
1 -1 -1 838.57 88.09
-1 1 1 658.73 66.56
1 0 156685.57 4400.53
1 0 149079.41 3615.80
-1 0 -154407.23 4054.90
-1 0 -145417.81 3244.44
-1 1 -1 9673.72 535.07
-1 1 -1 9138.41 428.32
1 -1 1 11.87 26.03
-1 1 -1 9991.00 537.79
-1 1 -1 9851.47 466.81
0 1 311196.69 630.56
0 -1 -3 9925.82 535.96
0 1 311467.95 594.56
0 -1 -310654.49 542.93
0 -2 -235781.69 2376.30
0 2 235721.61 2514.93
0 2 234635.98 2394.56
0 -2 -228130.40 1813.70
1 0 -246017.90 3693.04
-1 0 242497.26 3124.80
1 0 -253564.48 4061.08
-1 0 245466.77 3298.94
-1 -1 026253.67 1696.06
-1 -1 023982.04 1802.39
1 1 019573.90 1184.89
1 1 018670.89 1112.84
-1 -1 1 827.19 76.50
-1 -1 1 1096.50 152.15
1 1 -1 1185.71 179.25
1 1 -1 1454.52 139.45
-1 1 234534.64 2346.47
1 -1 -240626.25 2860.89
1 -1 -231973.55 2085.33
-1 1 231931.55 2057.33
1 -2 0 134597. 12772.
-1 2 0 158624. 16613.
-1 2 0 149570. 15230.
1 -2 0 115337. 10996.
0 -2 3 561.74 76.19
0 2 -3 557.07 81.05
0 2 -3 458.37 111.36
0 -2 3 586.36 83.01
-1 1 -2 1885.38 91.71
-1 1 -2 1842.11 152.60
-1 1 -2 1782.70 140.37
1 1 111360.48 688.54
-1 -1 -1 8984.20 515.35
-1 -1 -1 8976.82 452.68
1 1 113391.69 756.49
1 -2 140524.05 2877.31
1 -2 138200.36 2826.56
-1 2 -146002.84 3346.41
-1 2 -145115.48 3321.16
-1 0 -217145.83 1107.67
1 0 2 -2.77 1.50
-1 0 -217815.12 975.27
1 1 -2 8946.50 488.16
1 1 -210302.31 705.03
-1 -1 2 7975.64 534.54
-1 -1 2 9890.42 543.13
-1 2 1 457922. 67822.
-1 2 1 471571. 68154.
-1 2 1 431283. 63042.
-1 2 1 530292. 76628.
1 -2 -1 764.23 105.25
0 3 -1 7334.46 459.25
0 -3 1 6392.33 381.07
0 3 0 1472.58 131.22
0 -3 0 1824.78 153.53
0 3 0 2316.05 179.31
0 -3 1 5581.93 328.73
0 3 -1 7469.48 487.45
0 -3 0 1971.00 237.78
0 0 -4 1913.61 176.98
0 0 4 2249.05 149.06
0 0 -4 1820.83 170.10
0 1 -4 120597. 11310.
0 1 -4 104531. 9820.
0 -1 499086.62 9092.99
0 -1 4 104304. 9584.
-1 0 3 858578. 152973.
1 0 -3 711579. 122384.
-1 0 3 849500. 152145.
1 0 -3 841231. 145878.
0 -3 2 2711.35 198.79
1 -2 2 2959.40 138.54
1 -2 2 3086.00 201.82
0 3 -2 2486.04 285.29
0 3 -2 2380.63 182.81
0 -3 2 2424.29 194.90
-1 2 -2 2972.66 180.51
-1 2 -2 3536.22 233.15
0 3 125307.21 1643.53
0 -3 -125695.57 1827.71
0 3 122840.24 1488.18
0 -3 -131817.66 2136.16
-1 2 217518.93 945.25
-1 2 216744.34 1276.18
-1 2 222334.74 1211.03
-1 2 221236.92 1370.65
0 2 339822.74 2843.46
0 -2 -331898.17 2152.60
0 -2 -341822.38 3075.10
0 2 333389.82 2318.15
-1 1 360535.39 5165.73
1 -1 -367930.58 5315.81
-1 1 368458.23 5288.70
1 -1 -366136.54 5606.49
-1 -1 -224601.53 1477.90
-1 -1 -226233.87 1742.05
1 1 230103.14 2056.89
1 1 230791.55 1995.03
1 2 -115639.09 982.90
1 2 -118069.63 1260.91
-1 -2 121242.76 1546.00
-1 -2 116625.60 1096.70
1 1 -378006.79 6893.77
-1 -1 383757.17 7448.18
1 1 -386907.94 7646.55
-1 -1 392440.20 8188.37
1 2 0 247.15 74.91
-1 -2 0 217.01 56.44
1 2 0 188.51 55.37
-1 -2 0 239.41 79.49
0 1 4 529.46 78.12
0 -1 -4 568.12 119.68
0 -1 -4 490.61 88.45
0 1 4 527.37 74.98
-1 1 -318499.95 1166.42
-1 1 -316594.41 1234.06
-1 0 -366896.96 5011.19
1 0 376712.65 6845.88
-1 0 -359103.94 4861.80
0 -2 446124.15 3408.75
0 2 -465813.93 5417.01
0 -2 456009.37 4419.74
-1 -2 222358.44 1594.19
1 2 -218012.46 1180.33
-1 -2 225167.74 1963.78
1 2 -219308.81 1225.63
-1 3 091016.95 8279.43
1 -3 0 123177. 11821.
-1 3 098038.96 8631.29
1 -3 0 107525. 10379.
-1 -2 -1 102108. 9408.
-1 -2 -1 106581. 10112.
1 2 193793.43 8634.81
1 2 193427.44 8589.00
1 -3 115196.33 934.54
-1 3 -114260.42 835.01
-1 3 -113736.14 926.98
1 -3 115840.76 1070.21
0 3 -3 894.65 190.65
0 -3 3 784.00 154.39
0 -3 3 885.99 111.42
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-2 -7 -13 52.35 131.30
-2 -7 -13 37.37 64.84
2 7 13 19.07 14.21
-6 5 -3 34.38 80.02
-6 5 -3 27.94 139.29
-5 1 -10 195.21 115.43
-5 1 -10 115.81 116.54
-6 3 -4 85.13 119.04
-3 10 11 205.10 175.09
-4 5 14 179.02 210.38
-3 10 11 338.55 166.85
-4 5 14 268.58 198.86
-4 12 4 97.67 131.86
0 10 12 59.17 41.19
1 14 -3 25.36 65.66
-1 -14 3 38.11 75.73
-1 -14 3 28.77 227.41
1 14 -3 13.36 135.48
0 10 12 72.78 92.85
-3 3 -16 21.32 41.55
-3 3 -16 1.14 20.12
-3 7 -15 37.82 108.57
-2 -6 -14 478.52 74.85
1 14 -2 1046.79 197.54
-3 7 -15 31.57 91.04
-1 -14 2 773.38 185.49
-1 -14 2 1016.15 324.08
-5 5 -10 36.00 32.09
-2 -6 -14 779.14 186.59
-5 5 -10 68.86 51.73
-5 8 -8 10.09 69.93
1 14 -2 400.14 158.67
3 11 -8 66.37 163.14
-3 -11 8 50.15 71.27
3 11 -8 88.49 130.32
-4 8 -12 30.25 74.94
-3 -11 8 80.25 79.91
-6 2 -4 -26.27 151.97
1 -14 8 3.26 21.44
-2 -13 1 268.20 78.07
-2 -13 1 155.97 168.13
2 13 -1 354.85 240.23
-1 14 -8 -31.92 58.90
1 -14 8 -10.45 27.30
2 13 -1 456.69 275.57
-3 -3 17 355.99 146.15
-3 -3 17 90.79 55.58
3 3 -17 373.93 153.66
-2 2 18 -1.20 49.04
-3 2 17 17.10 40.06
-2 -4 18 373.51 140.83
2 4 -18 756.18 283.04
-2 2 18 -6.79 47.10
-3 2 17 -7.13 46.30
2 4 -18 577.99 108.37
-2 -4 18 939.74 171.51
-1 13 7 113.69 112.10
0 2 -19 -6.26 92.57
-2 -11 -7 87.45 111.79
2 11 7 299.73 65.59
2 11 7 -6.19 125.29
1 -13 -7 237.38 151.81
-2 -11 -7 125.46 126.03
0 2 -19 52.51 44.55
-6 6 3 454.54 165.97
-3 2 -16 405.26 123.95
-3 2 -16 256.70 86.84
-2 -10 -9 120.04 75.92
2 10 9 484.23 193.13
-2 -10 -9 240.32 130.83
2 10 9 358.56 140.57
-4 10 -10 190.91 122.13
-6 -2 2 1223.04 252.98
6 2 -2 937.70 185.92
-2 -1 -17 50.54 48.16
-6 -2 2 2118.49 316.89
6 2 -2 1261.76 207.92
-2 -1 -17 26.92 20.95
-4 3 15 100.28 99.62
-4 3 15 162.49 153.26
-5 10 4 104.10 57.39
-5 7 -9 114.29 91.77
-2 8 -16 7.66 75.31
-1 11 11 89.30 146.48
-2 8 -16 391.95 81.57
-1 11 11 83.90 55.33
1 14 -4 3978.01 510.01
-6 0 -3 -1.52 76.11
-1 -14 4 1901.96 216.57
-1 -14 4 3680.29 551.31
1 14 -4 3595.11 655.18
1 6 -18 40.52 42.93
1 6 -18 26.68 80.46
-1 -6 18 2.31 35.49
-1 -6 18 -0.71 27.20
-4 11 7 577.38 130.86
0 -14 -3 180.88 190.66
0 14 3 119.74 236.05
-6 4 6 28.46 75.62
0 -14 -3 44.18 179.62
0 14 3 108.47 143.68
-6 4 -4 230.29 248.29
0 1 -19 68.28 58.01
0 1 -19 42.87 55.61
4 6 -13 51.73 102.13
4 6 -13 31.97 62.37
-1 -1 19 -9.10 31.91
1 2 -19 321.19 129.90
-1 -1 19 8.51 72.34
-5 -2 12 662.86 280.68
1 1 -19 63.28 54.00
-2 6 -17 24.43 63.26
-1 14 4 152.35 194.59
5 2 -12 341.48 172.87
-2 6 -17 56.28 109.27
1 2 -19 816.09 146.00
-4 -6 13 -9.29 46.03
5 2 -12 180.71 42.16
1 1 -19 45.07 78.41
-4 -6 13 -9.87 82.52
-1 -2 19 1498.53 434.97
-6 -2 3 544.17 179.56
6 2 -3 415.94 135.73
-2 -13 5 251.48 187.32
6 2 -1 919.66 160.47
2 13 -5 530.77 226.97
-2 -13 5 783.58 214.58
-6 -2 1 1321.14 413.76
2 13 -5 844.50 227.87
-6 -2 1 1337.10 194.19
-1 -14 1 134.64 98.41
-1 -14 1 149.58 276.94
1 14 -1 219.40 191.39
1 10 11 811.78 66.46
1 10 11 818.12 210.94
1 14 -1 112.26 149.27
-1 -10 -11 1658.60 247.69
-1 -10 -11 964.14 169.62
-3 4 -16 484.45 164.97
-6 6 -2 480.25 235.27
-5 -5 -5 6319.74 1282.92
-4 -9 8 0.09 80.13
-4 -9 8 7.81 44.60
4 9 -8 -22.14 62.63
4 9 -8 5.52 54.97
-2 -8 -12 536.20 66.66
-2 -8 -12 745.40 173.06
2 8 12 684.82 126.77
2 8 12 734.71 136.86
-2 14 -7 38.95 108.33
0 3 -19 0.63 33.58
0 3 -19 1.57 25.62
4 3 -15 21.60 230.15
-4 -3 15 11.69 16.05
5 7 -3 67.59 63.99
4 3 -15 125.69 132.75
-5 -7 3 75.87 117.05
-4 -3 15 90.56 112.22
-5 -7 3 1.27 48.34
5 7 -3 42.19 38.95
5 7 -2 101.20 48.14
5 7 -2 127.79 121.38
-5 -7 2 158.16 157.00
0 3 18 20.31 43.78
-2 12 9 102.43 147.68
0 3 18 24.12 34.67
1 9 -16 -2.62 102.22
2 -13 10 27.88 133.40
1 9 -16 231.07 102.43
-1 -9 16 225.09 63.66
-2 13 -10 -6.84 59.42
-1 -9 16 184.39 123.61
3 -12 10 41.04 85.01
-4 10 9 104.78 114.31
-3 -6 -12 246.92 134.11
-3 -6 -12 263.81 166.62
-6 -1 -2 -1.67 74.46
-6 2 7 147.00 128.33
-4 -5 -10 227.42 202.16
-3 13 5 475.83 159.89
5 6 3 77.16 73.55
-5 -6 -3 -6.64 244.40
1 -13 11 -31.77 131.97
-5 -6 -3 138.44 73.81
-1 13 -11 0.09 26.85
-2 -11 12 758.69 268.75
2 11 -12 569.96 161.51
-4 -4 -11 110.42 154.33
-1 -10 15 507.00 91.73
1 10 -15 485.73 129.01
-1 -10 15 263.19 71.26
1 12 -12 -2.96 73.25
-3 -11 -3 535.32 165.73
-1 -12 12 33.93 41.41
3 11 3 875.03 455.01
-6 1 -4 512.75 386.02
4 7 -12 211.14 235.41
-4 -7 12 148.32 170.42
4 7 -12 126.23 98.94
2 13 0 3173.88 837.62
-2 -13 0 1592.53 220.19
5 7 -4 85.18 77.01
-5 -7 4 95.21 110.05
-3 -2 -15 1114.17 292.98
-4 -1 -13 230.32 200.59
2 -12 12 98.71 88.59
3 9 8 1112.41 193.32
-3 -9 -8 1655.59 402.59
-3 -5 -13 733.98 225.89
0 -14 8 356.82 74.61
-3 1 -16 375.13 88.19
-5 -7 1 72.13 168.14
6 2 -4 118.51 93.04
-6 -2 4 160.50 86.16
5 7 -1 112.23 106.45
3 10 -11 0.92 46.78
-3 -10 11 1.69 89.48
;
_shelx_hkl_checksum 15314
_shelx_res_file
;
TITL 13041115
shelxl.res
created by SHELXL-2016/6 at 17:46:29 on 20-Oct-2017
CELL 0.71075 4.47454 10.54484 13.61114 96.652 94.109 99.009
ZERR 1 0.00021 0.00076 0.00061 0.004 0.003 0.004
LATT 1
SFAC C H O N CL
UNIT 26 20 10 2 2
SHEL 99999.000000 0.000000
L.S. 15
FMAP 2
PLAN -20
WPDB -2
HTAB
BOND $H
CONF
LIST 4
TEMP -73.0
ACTA
SIZE 0.030 0.210 0.410
LIST 4
DFIX 0.8400 0.0200 O5 H3
DFIX 0.8400 0.0200 O5 H4
WGHT 0.087900
FVAR 5.82481
CL1 5 0.493904 0.236637 -0.028417 11.00000 0.04021 0.03800 =
0.04653 0.00725 -0.00095 -0.00570
O1 3 0.031943 0.080807 -0.176534 11.00000 0.04508 0.04516 =
0.03541 0.00926 -0.00261 0.00078
O2 3 0.415036 0.117098 0.155105 11.00000 0.03877 0.03802 =
0.03591 0.00121 -0.00791 -0.00047
O3 3 -0.176890 0.362162 0.471214 11.00000 0.03756 0.03190 =
0.04275 0.00888 -0.00174 0.00682
O4 3 -0.071212 0.161599 0.436044 11.00000 0.04034 0.03678 =
0.04715 -0.00516 -0.00714 0.00908
O5 3 0.393782 0.074711 0.332305 11.00000 0.03996 0.04191 =
0.03574 -0.00294 -0.00664 0.00470
N1 4 0.323299 0.419703 0.603901 11.00000 0.03023 0.02694 =
0.03256 0.00554 0.00204 0.00529
C1 1 0.020739 0.046349 -0.094694 11.00000 0.02918 0.03041 =
0.03530 0.00388 -0.00043 0.00615
C2 1 0.227644 0.107615 -0.009852 11.00000 0.02865 0.02739 =
0.03837 0.00320 -0.00101 0.00224
C3 1 0.219720 0.065135 0.079712 11.00000 0.02978 0.02778 =
0.03541 0.00069 -0.00160 0.00636
C4 1 0.215138 0.297033 0.569091 11.00000 0.02973 0.02908 =
0.03298 0.00450 0.00436 0.00456
C5 1 0.327424 0.197024 0.611402 11.00000 0.03470 0.02728 =
0.03839 0.00512 0.00046 0.00431
AFIX 43
H5 2 0.250293 0.109195 0.586437 11.00000 -1.20000
AFIX 0
C6 1 0.549322 0.226800 0.689060 11.00000 0.03567 0.03013 =
0.03785 0.00889 0.00199 0.00593
AFIX 43
H6 2 0.622423 0.159293 0.719133 11.00000 -1.20000
AFIX 0
C7 1 0.669420 0.356586 0.724490 11.00000 0.02994 0.03153 =
0.03252 0.00538 0.00388 0.00475
C8 1 0.904965 0.393316 0.802172 11.00000 0.03473 0.03881 =
0.03530 0.00601 0.00115 0.00633
AFIX 43
H8 2 0.985438 0.328869 0.834065 11.00000 -1.20000
AFIX 0
C9 1 1.017033 0.520944 0.831474 11.00000 0.03577 0.04527 =
0.03819 -0.00304 -0.00358 0.00331
AFIX 43
H9 2 1.175836 0.545100 0.883608 11.00000 -1.20000
AFIX 0
C10 1 0.898022 0.617639 0.784630 11.00000 0.04024 0.03289 =
0.04838 -0.00459 0.00056 0.00260
AFIX 43
H10 2 0.980263 0.706066 0.805678 11.00000 -1.20000
AFIX 0
C11 1 0.667656 0.587224 0.709826 11.00000 0.03765 0.02892 =
0.04432 0.00138 0.00270 0.00606
AFIX 43
H11 2 0.587483 0.653070 0.679646 11.00000 -1.20000
AFIX 0
C12 1 0.553169 0.455578 0.678971 11.00000 0.02808 0.02866 =
0.03111 0.00210 0.00416 0.00441
C13 1 -0.033298 0.272426 0.483965 11.00000 0.02929 0.03111 =
0.03395 0.00578 0.00238 0.00373
H1 2 0.251532 0.481499 0.576021 11.00000 0.05543
H2 2 0.358719 0.082735 0.216411 11.00000 0.09234
H3 2 0.254595 0.086057 0.366749 11.00000 0.05359
H4 2 0.559873 0.110521 0.365109 11.00000 0.06335
HKLF 4
REM 13041115
REM R1 = 0.0524 for 2755 Fo > 4sig(Fo) and 0.0722 for all 3666 data
REM 197 parameters refined using 2 restraints
END
WGHT 0.0873 0.0000
REM Instructions for potential hydrogen bonds
EQIV $2 -x, -y+1, -z+1
HTAB C11 O3_$2
HTAB N1 O3_$2
HTAB O2 O5
HTAB O5 O4
EQIV $3 x+1, y, z
HTAB O5 O4_$3
REM Highest difference peak 0.518, deepest hole -0.450, 1-sigma level 0.154
Q1 1 0.4811 0.1970 -0.3662 11.00000 0.05 0.52
Q2 1 -0.0922 0.4391 0.4818 11.00000 0.05 0.49
Q3 1 0.6310 0.2932 -0.2943 11.00000 0.05 0.45
Q4 1 0.0461 0.5055 0.5594 11.00000 0.05 0.43
Q5 1 0.9578 0.3709 -0.2076 11.00000 0.05 0.43
Q6 1 1.1009 0.2975 -0.1390 11.00000 0.05 0.43
Q7 1 -0.3296 0.3621 0.4172 11.00000 0.05 0.42
Q8 1 0.5916 0.1469 -0.2438 11.00000 0.05 0.42
Q9 1 0.0000 0.0000 0.5000 10.50000 0.05 0.42
Q10 1 0.5942 0.5273 0.6949 11.00000 0.05 0.39
Q11 1 0.8354 0.3562 -0.2398 11.00000 0.05 0.39
Q12 1 0.7725 0.2199 -0.0426 11.00000 0.05 0.39
Q13 1 0.6236 0.7452 0.6398 11.00000 0.05 0.38
Q14 1 0.4228 0.0586 -0.1980 11.00000 0.05 0.38
Q15 1 0.2225 0.1410 0.4250 11.00000 0.05 0.37
Q16 1 0.7607 0.2217 -0.1806 11.00000 0.05 0.37
Q17 1 0.5640 0.6772 0.6475 11.00000 0.05 0.36
Q18 1 0.6173 0.6568 0.6585 11.00000 0.05 0.36
Q19 1 -0.0479 0.0510 0.3559 11.00000 0.05 0.35
Q20 1 0.8292 0.3085 -0.2323 11.00000 0.05 0.34
;
_shelx_res_checksum 63829