#------------------------------------------------------------------------------
#$Date: 2018-11-17 05:48:50 +0200 (Sat, 17 Nov 2018) $
#$Revision: 212035 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/27/2242743.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_2242743
loop_
_publ_author_name
'Mulrooney, David Z. T.'
'Madden, Eimear C.'
'Lonergan, Rhona F.'
'Slyusarchuk, Valentyna D.'
'M\"uller-Bunz, Helge'
'Keene, Tony D.'
_publ_section_title
;
Hydrogen-bonding chain and dimer motifs in pyridinium and morpholinium
hydrogen oxalate salts
;
_journal_coeditor_code QM2130
_journal_issue 12
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 1804
_journal_page_last 1807
_journal_paper_doi 10.1107/S2056989018015827
_journal_volume 74
_journal_year 2018
_chemical_formula_iupac 'C7 H11 N2 +, C2 H O4 -, 0.22H2 O'
_chemical_formula_moiety 'C7 H11 N2 +, C2 H O4 -, 0.22(H2 O)'
_chemical_formula_sum 'C9 H12.44 N2 O4.22'
_chemical_formula_weight 216.21
_chemical_name_common
'4-dimethylaminopyridinium hydrogen oxalate 0.22 hydrate'
_chemical_name_systematic
;
4-(Dimethylamino)pyridinum hydrogen oxalate 0.22-hydrate,
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 89.738(3)
_cell_angle_beta 79.626(3)
_cell_angle_gamma 64.741(4)
_cell_formula_units_Z 4
_cell_length_a 7.5241(3)
_cell_length_b 8.2898(3)
_cell_length_c 18.7359(6)
_cell_measurement_reflns_used 6456
_cell_measurement_temperature 101.3(8)
_cell_measurement_theta_max 76.7320
_cell_measurement_theta_min 4.8010
_cell_volume 1036.17(8)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 101.3(8)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Rigaku SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0239
_diffrn_reflns_av_unetI/netI 0.0234
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 12774
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 76.797
_diffrn_reflns_theta_min 4.815
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.945
_exptl_absorpt_correction_T_max 0.918
_exptl_absorpt_correction_T_min 0.857
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2017)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.386
_exptl_crystal_description block
_exptl_crystal_F_000 457
_exptl_crystal_size_max 0.217
_exptl_crystal_size_mid 0.119
_exptl_crystal_size_min 0.116
_refine_diff_density_max 0.641
_refine_diff_density_min -0.605
_refine_ls_extinction_coef 0.0050(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2017 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.033
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 290
_refine_ls_number_reflns 4321
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.033
_refine_ls_R_factor_all 0.0453
_refine_ls_R_factor_gt 0.0386
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.4606P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0961
_refine_ls_wR_factor_ref 0.1024
_reflns_number_gt 3792
_reflns_number_total 4321
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file qm2130sup1.cif
_cod_data_source_block 1
_cod_original_cell_volume 1036.17(7)
_cod_database_code 2242743
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 2 52.40 1.65
0 0 2 62.05 1.60
0 0 3 190.83 3.42
0 0 3 182.16 3.77
0 0 4 0.19 0.58
0 0 4 0.52 0.68
0 0 5 67.89 3.10
0 0 5 69.72 3.12
0 0 5 71.38 2.77
0 0 6 600.81 9.90
0 0 6 616.49 8.71
0 0 6 609.83 10.04
0 0 7 28.83 2.53
0 0 7 31.13 2.61
0 0 7 33.41 2.86
0 0 7 31.81 2.22
0 0 8 2.04 1.23
0 0 8 2.06 1.37
0 0 8 1.82 1.15
0 0 9 357.75 8.41
0 0 9 365.47 9.87
0 0 9 352.17 9.91
0 0 9 360.86 10.39
0 0 10 211.05 6.80
0 0 10 213.84 8.38
0 0 10 221.23 8.82
0 0 10 218.39 8.21
0 0 11 121.10 6.51
0 0 11 137.47 7.25
0 0 11 134.86 7.24
0 0 12 17.15 2.91
0 0 12 20.61 3.04
0 0 12 18.69 2.95
0 0 13 1.95 1.61
0 0 13 0.55 0.90
0 0 13 -2.00 1.96
0 0 14 4.17 1.96
0 0 14 7.90 2.05
0 0 14 4.90 1.95
0 0 14 7.35 1.96
0 0 14 8.61 3.13
0 0 14 5.81 1.63
0 0 15 78.37 6.73
0 0 15 81.77 5.35
0 0 15 87.87 5.05
0 0 15 85.50 5.89
0 0 15 84.18 5.44
0 0 16 10.83 2.02
0 0 16 14.26 2.74
0 0 16 10.20 2.25
0 0 16 16.04 3.27
0 0 17 14.07 2.97
0 0 17 15.69 2.83
0 0 18 72.73 5.11
0 0 18 77.09 5.75
0 0 19 45.88 4.59
0 0 -19 37.10 3.15
0 0 19 43.09 4.06
0 0 20 7.91 1.88
0 0 -20 10.52 1.78
0 0 20 8.14 2.47
0 0 21 20.41 2.76
0 0 21 21.42 2.33
0 0 22 9.26 1.31
0 0 22 8.67 1.59
0 0 22 8.76 1.47
0 0 23 234.46 5.30
0 -1 23 24.55 1.93
0 1 -22 -1.27 0.63
0 -1 22 0.29 0.89
0 -1 22 -1.73 1.10
0 -1 22 0.37 0.74
0 -1 21 55.01 3.49
0 -1 21 52.26 3.95
0 1 -21 47.44 3.04
0 -1 20 0.33 1.41
0 -1 20 -0.65 0.81
0 1 -20 -0.12 1.17
0 -1 19 7.58 2.32
0 -1 19 6.99 2.46
0 -1 19 6.33 1.83
0 -1 18 255.34 9.21
0 -1 18 265.84 10.38
0 -1 18 276.64 9.82
0 -1 17 227.04 9.86
0 -1 17 232.11 9.42
0 -1 17 232.74 8.95
0 -1 16 491.08 13.71
0 -1 16 463.31 13.74
0 -1 15 512.33 13.82
0 -1 15 515.42 14.15
0 -1 14 55.73 5.47
0 -1 14 60.21 4.64
0 -1 14 61.69 5.01
0 -1 13 258.74 11.09
0 -1 13 269.32 11.92
0 -1 13 268.80 10.48
0 -1 12 96.04 6.09
0 -1 12 111.54 6.92
0 -1 12 91.91 6.69
0 -1 11 89.28 5.48
0 -1 11 94.10 5.60
0 -1 10 67.09 4.58
0 -1 10 71.17 4.66
0 -1 10 69.47 5.17
0 -1 9 2.29 1.67
0 -1 9 1.34 1.20
0 -1 9 1.93 0.93
0 -1 8 23.00 2.63
0 -1 8 23.19 2.64
0 -1 7 378.50 9.38
0 -1 7 364.97 8.99
0 -1 6 609.73 10.46
0 -1 6 617.40 11.33
0 -1 5 768.14 12.08
0 -1 5 794.73 10.89
0 -1 4 13.15 2.05
0 -1 4 10.79 1.38
0 -1 3 2962.76 21.01
0 -1 3 3033.00 16.86
0 -1 2 5230.64 25.53
0 -1 2 5117.64 18.63
0 -1 1 120.29 3.68
0 -1 0 94.11 3.01
0 1 1 41.40 1.22
0 1 1 37.32 1.60
0 -1 -1 36.42 1.77
0 1 2 553.68 5.40
0 1 2 542.72 5.55
0 1 3 269.86 3.88
0 1 3 265.36 4.50
0 1 4 4648.30 17.01
0 1 4 4672.21 21.68
0 1 4 4660.16 25.55
0 1 5 773.15 9.99
0 1 5 764.13 11.48
0 1 5 757.81 12.14
0 1 5 753.79 7.42
0 1 6 1144.03 15.94
0 1 6 1112.59 15.04
0 1 6 1103.08 9.71
0 1 6 1119.72 13.42
0 1 7 116.03 5.27
0 1 7 119.01 5.73
0 1 7 114.96 4.79
0 1 7 115.95 3.39
0 1 8 71.02 4.50
0 1 8 72.87 4.18
0 1 8 70.89 2.77
0 1 8 73.48 4.86
0 1 9 811.26 16.67
0 1 9 828.05 14.89
0 1 9 819.59 15.84
0 1 10 439.33 11.76
0 1 10 439.30 13.10
0 1 10 432.62 12.15
0 1 11 -1.08 1.13
0 1 11 2.94 1.29
0 1 11 1.58 1.39
0 1 12 36.21 4.06
0 1 12 27.52 3.81
0 1 12 32.93 3.95
0 1 13 258.93 11.88
0 1 13 222.95 10.18
0 1 13 233.21 7.74
0 1 13 229.23 7.84
0 1 13 248.21 9.03
0 1 13 239.53 10.82
0 1 13 255.10 8.77
0 1 14 69.92 5.05
0 1 14 64.40 5.70
0 1 14 76.82 5.18
0 1 14 73.66 6.62
0 1 14 72.46 4.84
0 1 14 73.06 4.74
0 1 14 70.04 6.56
0 1 15 114.59 8.85
0 1 15 124.35 7.03
0 1 15 120.12 6.55
0 1 16 289.36 10.71
0 1 16 277.87 9.82
0 1 17 65.91 5.31
0 1 17 64.04 4.90
0 1 18 95.40 6.05
0 1 18 86.69 5.57
0 1 19 52.10 4.57
0 1 19 54.51 4.36
0 1 20 3.18 1.58
0 1 20 -1.30 1.06
0 1 20 1.90 0.82
0 1 20 1.24 1.44
0 1 21 4.22 1.14
0 1 21 4.36 1.10
0 1 21 3.34 1.58
0 1 21 2.79 1.35
0 1 22 171.97 5.13
0 1 22 178.68 4.99
0 -2 22 2.94 1.00
0 -2 22 2.63 1.10
0 2 -22 2.94 0.91
0 -2 21 2.15 1.13
0 -2 21 1.15 1.17
0 2 -21 1.55 0.90
0 -2 21 2.64 1.25
0 2 -20 -0.55 1.09
0 -2 20 0.76 1.40
0 -2 20 0.66 1.11
0 -2 20 2.50 1.51
0 -2 19 28.97 3.35
0 -2 19 32.77 3.42
0 -2 19 34.91 4.08
0 2 -19 29.02 2.66
0 -2 18 49.87 4.78
0 -2 18 47.42 4.78
0 -2 18 47.53 4.19
0 2 -18 48.96 3.68
0 -2 17 70.87 5.54
0 2 -17 72.67 4.50
0 -2 17 65.85 5.36
0 2 -16 26.20 3.11
0 -2 16 33.23 3.95
0 -2 16 29.32 3.84
0 -2 15 82.79 5.89
0 -2 15 84.52 5.95
0 2 -15 92.68 5.29
0 -2 14 649.21 15.27
0 -2 14 674.47 16.11
0 2 -14 674.14 13.45
0 -2 13 462.97 12.91
0 -2 13 439.26 12.05
0 2 -13 482.86 11.00
0 -2 12 56.46 4.81
0 -2 12 53.20 5.42
0 -2 11 95.79 6.81
0 -2 10 1264.83 23.38
0 -2 9 146.97 7.87
0 -2 8 16.60 3.23
0 -2 7 2225.88 27.59
0 -2 6 7615.92 48.94
0 -2 5 1680.71 22.24
0 -2 4 104.36 5.46
0 -2 3 14.04 2.37
0 -2 2 674.88 12.38
0 -2 1 86.70 4.45
0 2 -1 77.44 3.59
0 -2 0 50.96 3.35
0 -2 -1 2133.26 19.53
0 2 1 2123.46 11.15
0 2 2 3.80 0.64
0 -2 -2 5.12 1.23
0 2 3 4.51 1.44
0 -2 -3 3.52 1.05
0 2 3 4.08 0.73
0 2 3 4.89 1.37
0 2 4 508.33 10.28
0 2 4 504.58 10.99
0 2 4 511.59 7.50
0 -2 -4 527.66 8.56
0 2 5 1051.40 15.57
0 2 5 1018.23 11.84
0 -2 -5 1009.46 10.96
0 2 5 1014.23 16.48
0 2 6 1014.04 16.17
0 2 6 983.36 12.87
0 2 6 969.18 17.18
0 2 7 783.18 16.16
0 2 7 797.01 15.25
0 2 7 776.54 12.50
0 2 8 187.39 6.72
0 2 8 198.53 8.73
0 2 8 188.96 7.94
0 2 9 104.50 5.49
0 2 9 113.79 6.93
0 2 9 109.50 6.39
0 2 10 57.22 4.56
0 2 10 56.20 5.33
0 2 10 69.05 5.45
0 2 11 -0.69 1.69
0 2 11 0.95 1.11
0 2 11 1.62 1.74
0 2 12 310.73 9.03
0 2 12 300.54 12.20
0 2 12 313.77 11.71
0 2 12 304.92 13.18
0 2 12 325.42 9.71
0 2 13 77.93 5.10
0 2 13 78.41 5.12
0 2 13 80.82 6.49
0 2 13 75.78 6.49
0 2 13 83.01 5.33
0 2 13 78.13 7.05
0 2 14 503.43 18.25
0 2 14 515.54 17.02
0 2 14 528.54 13.48
0 2 14 548.07 17.20
0 2 14 506.29 12.27
0 2 14 520.10 13.19
0 2 15 -1.35 2.80
0 2 15 0.45 1.06
0 2 15 2.66 2.63
0 2 15 4.65 1.96
0 2 16 16.24 2.83
0 2 16 12.10 2.54
0 2 17 6.23 1.78
0 2 17 -0.42 1.60
0 2 18 141.84 6.85
0 2 18 134.54 6.09
0 2 18 137.09 6.66
0 2 19 34.88 2.98
0 2 19 30.65 3.12
0 2 19 32.08 2.98
0 2 19 27.50 2.96
0 2 20 31.40 2.45
0 2 20 35.31 2.95
0 2 20 36.41 2.63
0 2 20 28.89 2.75
0 2 21 3.19 0.86
0 2 21 3.34 1.13
0 2 22 1.07 0.57
0 3 -22 4.32 0.92
0 -3 21 22.51 1.97
0 -3 21 26.99 2.39
0 3 -21 22.12 2.12
0 -3 21 23.91 2.34
0 -3 20 31.22 2.90
0 -3 20 28.95 2.93
0 3 -20 26.01 2.59
0 3 -20 31.08 2.45
0 -3 20 28.21 2.59
0 -3 19 1.17 1.49
0 3 -19 0.95 0.93
0 -3 19 -0.25 1.07
0 -3 19 0.64 1.44
0 -3 18 2.66 1.77
0 3 -18 2.23 1.39
0 -3 18 4.37 2.37
0 -3 17 85.75 6.06
0 -3 17 89.74 5.89
0 3 -17 82.47 5.07
0 -3 16 87.15 6.08
0 -3 16 89.26 6.44
0 3 -16 90.65 5.51
0 3 -15 224.83 8.45
0 -3 15 218.07 8.98
0 -3 15 227.08 9.93
0 -3 14 225.80 8.92
0 3 -14 245.06 8.74
0 -3 14 260.28 10.44
0 3 -13 8.18 1.85
0 -3 13 4.07 2.23
0 -3 13 9.99 2.23
0 -3 12 53.42 4.48
0 3 -12 55.24 4.07
0 -3 12 58.58 6.66
0 -3 11 52.04 6.13
0 -3 10 15.05 3.48
0 -3 9 81.54 6.94
0 -3 8 499.29 16.03
0 -3 7 177.15 9.25
0 -3 6 54.65 5.51
0 -3 5 16.38 3.62
0 -3 4 253.72 10.14
0 -3 3 104.33 6.47
0 -3 2 3808.48 35.99
0 -3 1 200.20 8.16
0 -3 0 1014.49 17.76
0 3 0 989.31 16.17
0 3 1 44.77 3.74
0 -3 -1 42.14 3.76
0 3 1 41.22 1.81
0 3 2 8.26 1.94
0 3 2 6.24 1.89
0 -3 -2 9.20 2.12
0 3 2 8.38 0.88
0 -3 -3 269.96 8.47
0 3 3 273.74 8.78
0 3 3 280.55 5.18
0 3 3 269.84 9.38
0 -3 -4 380.32 9.62
0 3 4 371.26 6.58
0 3 4 385.13 11.57
0 3 4 390.84 10.75
0 3 5 289.74 10.51
0 -3 -5 311.54 8.16
0 3 5 291.81 9.80
0 3 5 302.57 6.55
0 3 6 15.70 1.65
0 3 6 12.80 2.66
0 3 6 12.58 2.49
0 3 7 716.73 16.68
0 3 7 742.03 12.25
0 3 7 706.34 17.84
0 3 8 163.40 8.37
0 3 8 157.89 8.77
0 3 8 174.89 6.56
0 3 9 264.20 11.05
0 3 9 272.59 12.08
0 3 10 106.75 7.38
0 3 10 115.53 8.21
0 3 11 82.24 4.87
0 3 11 82.17 5.06
0 3 11 83.38 4.80
0 3 11 82.40 7.05
0 3 11 85.89 7.39
0 3 12 7.91 1.99
0 3 12 7.30 1.92
0 3 12 4.90 1.63
0 3 12 6.45 2.49
0 3 12 8.89 2.74
0 3 13 142.34 10.06
0 3 13 149.90 6.75
0 3 13 154.85 9.82
0 3 13 146.07 7.00
0 3 13 153.16 7.25
0 3 14 42.61 4.39
0 3 14 45.19 4.32
0 3 14 44.61 3.74
0 3 14 50.72 6.08
0 3 14 53.40 5.94
0 3 15 2.47 1.01
0 3 15 2.70 2.15
0 3 15 5.25 2.76
0 3 16 104.25 5.37
0 3 16 93.47 5.87
0 3 16 102.88 5.90
0 3 17 14.89 2.35
0 3 17 16.88 2.91
0 3 17 19.14 2.91
0 3 18 39.01 3.33
0 3 18 39.45 3.01
0 3 18 36.94 3.41
0 3 19 10.17 1.75
0 3 19 11.62 1.92
0 3 20 1.83 1.02
0 3 20 4.51 1.27
0 3 21 58.71 2.68
0 4 -21 0.81 0.74
0 4 -21 -0.95 0.61
0 -4 21 -0.64 0.78
0 4 -20 252.10 6.76
0 -4 20 253.95 6.18
0 4 -20 237.22 6.10
0 -4 20 259.29 7.70
0 4 -19 20.95 2.24
0 4 -19 25.69 2.60
0 -4 19 20.35 2.70
0 -4 18 13.12 2.46
0 4 -18 9.90 1.84
0 -4 17 41.64 4.41
0 4 -17 46.15 3.95
0 -4 16 53.79 4.91
0 4 -16 45.20 3.99
0 -4 15 167.43 8.68
0 4 -15 172.09 7.58
0 4 -14 0.93 1.66
0 -4 14 1.91 1.60
0 -4 13 61.99 7.98
0 -4 13 53.37 5.05
0 4 -13 64.05 4.71
0 4 -12 10.25 2.44
0 -4 12 15.55 3.13
0 4 -12 14.24 2.56
0 -4 12 11.89 4.02
0 4 -11 86.57 5.12
0 -4 11 88.08 6.16
0 4 -11 81.09 5.34
0 -4 11 86.65 8.63
0 4 -10 157.75 6.56
0 -4 10 148.42 10.69
0 -4 10 158.37 7.79
0 -4 9 49.47 6.54
0 -4 8 440.85 17.05
0 -4 7 2.08 2.88
0 -4 6 36.29 5.22
0 -4 5 615.75 18.56
0 -4 4 994.02 23.12
0 -4 3 258.94 11.66
0 -4 2 272.71 11.68
0 -4 1 156.21 8.90
0 -4 0 18.05 3.60
0 -4 -1 818.95 18.83
0 4 1 780.39 17.89
0 4 2 86.91 6.20
0 -4 -2 90.76 6.39
0 -4 -3 -0.20 1.79
0 4 3 9.01 2.13
0 -4 -4 502.67 13.43
0 4 4 479.03 15.21
0 4 5 -0.76 1.24
0 4 5 0.23 0.92
0 4 6 22.29 3.54
0 4 6 20.26 3.54
0 4 7 29.06 4.16
0 4 7 22.80 3.67
0 4 8 96.66 7.33
0 4 8 98.03 5.20
0 4 8 89.87 5.09
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-8 -6 7 29.30 1.80
8 6 -7 28.58 1.77
-8 -6 6 36.22 2.17
-8 -6 6 41.37 2.39
-8 -6 5 27.59 2.03
8 6 -5 24.39 2.13
-8 -6 5 27.65 2.27
-8 -6 4 9.16 1.62
-8 -6 4 8.22 1.31
8 6 -4 8.02 1.66
-8 -6 3 7.72 1.68
-8 -6 3 8.74 1.40
8 6 -3 9.37 2.04
-8 -6 2 2.03 1.14
-8 -6 2 0.99 0.98
8 6 -2 4.48 1.57
-8 -6 1 32.90 2.33
8 6 -1 40.64 3.90
-8 -6 1 34.44 2.91
-8 -6 0 1.12 1.35
-8 -6 0 0.64 0.66
8 6 0 2.28 1.85
-8 -6 -1 132.57 6.00
8 6 1 145.28 7.12
-8 -6 -1 150.90 5.81
-8 -6 -2 41.46 3.61
8 6 2 46.44 4.37
-8 -6 -2 47.79 3.32
-8 -6 -3 37.53 3.55
8 6 3 40.25 2.73
8 6 3 37.37 4.05
-8 -6 -3 38.66 3.01
-8 -6 -4 1.08 1.03
-8 -6 -4 1.97 1.72
8 6 4 2.29 1.02
8 6 4 3.79 2.23
-8 -6 -5 23.13 2.79
8 6 5 26.99 2.27
8 6 5 27.10 3.61
-8 -6 -5 25.54 2.43
-8 -6 -6 63.22 4.07
8 6 6 65.77 3.59
8 6 6 65.87 4.83
-8 -6 -6 65.25 3.42
-8 -6 -7 3.39 1.41
8 6 7 2.55 1.17
8 6 7 3.86 1.96
-8 -6 -8 2.59 1.38
8 6 8 1.98 1.07
8 6 8 0.16 1.47
-8 -6 -9 5.95 1.59
8 6 9 3.67 1.09
8 6 9 4.81 1.65
-8 -6 -10 3.95 1.37
8 6 10 2.84 0.96
8 6 10 6.89 1.67
-8 -6 -11 1.82 1.03
8 6 11 2.67 0.99
-8 -6 -12 1.35 0.81
8 6 12 0.26 0.73
8 6 13 1.83 0.75
-8 -6 -13 1.23 0.69
8 6 13 0.57 0.52
-8 -6 -14 79.78 2.78
-8 -7 6 2.63 0.60
-8 -7 5 29.56 1.78
8 7 -5 26.90 2.02
-8 -7 4 3.92 1.01
-8 -7 4 3.51 0.84
8 7 -4 4.87 1.25
-8 -7 3 1.81 0.89
-8 -7 3 1.58 0.71
8 7 -3 2.85 1.09
-8 -7 2 16.98 1.61
-8 -7 2 19.85 1.96
8 7 -2 17.98 2.35
-8 -7 1 34.35 2.09
8 7 -1 44.50 3.71
-8 -7 1 40.74 2.71
8 7 0 26.43 1.96
8 7 0 27.01 3.18
-8 -7 0 25.23 2.24
8 7 1 51.15 2.74
8 7 1 49.69 3.97
-8 -7 -1 55.14 3.09
-8 -7 -2 1.08 0.93
8 7 2 0.13 0.83
8 7 2 -1.30 1.84
-8 -7 -3 38.93 3.16
8 7 3 40.37 2.66
8 7 3 41.95 3.88
-8 -7 -3 43.20 2.65
-8 -7 -4 147.68 5.62
8 7 4 154.09 4.99
8 7 4 163.41 7.04
-8 -7 -4 158.16 4.61
-8 -7 -5 211.29 6.58
8 7 5 215.24 5.91
8 7 5 230.27 7.93
-8 -7 -6 125.11 4.99
8 7 6 126.62 4.57
8 7 6 133.40 5.81
-8 -7 -7 13.75 1.92
8 7 7 14.22 1.72
8 7 7 13.83 2.11
-8 -7 -8 16.05 1.78
8 7 8 16.21 1.76
8 7 8 14.45 1.98
-8 -7 -9 0.18 0.74
8 7 9 0.78 0.90
8 7 9 -0.68 0.82
-8 -7 -10 44.57 2.50
8 7 10 46.84 2.55
-8 -7 -11 0.88 0.62
8 7 11 0.19 0.54
8 7 12 28.85 1.77
8 7 12 29.57 1.74
8 8 -3 -0.14 0.61
8 8 -2 3.12 1.13
8 8 -1 0.59 0.91
8 8 0 16.11 2.07
8 8 1 3.72 0.91
8 8 1 4.10 1.55
8 8 2 213.67 4.91
8 8 2 230.02 5.14
8 8 2 229.00 6.92
-8 -8 -3 126.11 4.22
8 8 3 135.17 4.06
8 8 3 134.46 5.33
8 8 4 98.55 3.53
8 8 4 97.25 4.38
8 8 5 3.13 0.97
8 8 5 3.18 1.01
8 8 5 4.77 1.21
8 8 6 34.83 2.36
8 8 6 31.11 2.02
8 8 7 68.71 3.19
8 8 7 64.56 2.75
8 8 8 55.65 2.79
8 8 8 51.56 2.36
8 8 9 23.43 1.74
8 8 9 23.12 1.50
-9 -2 0 5.42 1.00
-9 -2 -1 123.95 3.82
-9 -2 -2 244.45 5.51
-9 -2 -2 231.16 4.62
-9 -2 -3 7.07 1.01
-9 -2 -3 7.53 1.29
-9 -2 -4 -0.08 0.61
-9 -2 -4 0.01 0.52
-9 -2 -5 1.80 0.72
-9 -2 -5 1.20 0.62
-9 -2 -6 29.64 1.83
9 2 6 34.36 2.30
-9 -2 -6 34.15 2.05
-9 -2 -7 6.92 1.02
-9 -2 -7 6.09 0.94
9 2 7 4.40 0.99
-9 -2 -8 8.64 1.02
9 2 8 9.38 1.21
-9 -2 -8 10.75 1.18
9 2 9 31.98 2.06
-9 -2 -9 32.34 1.74
-9 -3 2 67.61 2.70
-9 -3 1 17.05 1.70
-9 -3 1 18.67 1.38
-9 -3 0 168.81 4.84
-9 -3 0 161.39 4.18
-9 -3 -1 -0.03 0.71
-9 -3 -1 0.05 0.92
-9 -3 -2 1.77 0.90
-9 -3 -2 2.44 1.11
9 3 3 16.74 1.95
-9 -3 -3 12.86 1.53
9 3 4 80.55 3.83
-9 -3 -4 76.22 3.38
-9 -3 -5 58.91 2.48
9 3 5 64.69 3.52
-9 -3 -5 62.49 3.05
-9 -3 -6 114.20 3.48
-9 -3 -6 119.13 4.16
-9 -3 -7 60.25 2.59
9 3 7 64.78 3.60
-9 -3 -7 57.20 2.87
-9 -3 -8 84.14 2.97
-9 -3 -8 89.54 3.33
-9 -3 -9 22.31 1.53
9 3 9 22.85 1.99
-9 -3 -9 22.23 1.59
9 3 10 18.62 1.77
-9 -4 2 44.21 2.25
-9 -4 2 50.67 2.23
-9 -4 1 162.25 4.46
-9 -4 1 171.79 4.40
-9 -4 0 41.95 2.49
9 4 0 38.51 2.25
-9 -4 0 45.71 2.48
-9 -4 -1 26.07 2.10
9 4 1 22.91 2.07
-9 -4 -1 23.67 1.99
-9 -4 -2 2.33 1.08
-9 -4 -2 0.90 0.98
9 4 2 2.57 1.03
-9 -4 -3 1.03 0.86
9 4 3 1.54 1.12
-9 -4 -4 0.24 0.86
9 4 4 2.21 1.24
9 4 5 12.65 2.01
-9 -4 -5 12.28 1.57
-9 -4 -6 55.59 2.80
9 4 6 63.07 3.78
-9 -4 -6 55.28 2.89
-9 -4 -7 1.67 0.79
-9 -4 -7 1.62 0.73
-9 -4 -8 4.99 0.90
-9 -4 -8 6.19 0.93
9 4 8 4.14 1.46
-9 -4 -9 2.97 0.71
-9 -4 -9 3.69 0.79
9 4 9 3.58 1.25
9 4 10 17.18 1.80
-9 -5 2 17.84 1.48
-9 -5 1 5.70 1.03
9 5 0 207.70 5.65
-9 -5 0 227.63 5.39
-9 -5 -1 1.53 0.84
-9 -5 -1 0.49 0.77
9 5 1 1.94 1.00
-9 -5 -2 3.05 0.93
-9 -5 -2 1.11 0.91
9 5 2 1.69 1.11
-9 -5 -3 11.62 1.45
9 5 3 14.10 2.02
-9 -5 -3 14.86 1.69
9 5 4 36.79 2.92
-9 -5 -4 37.87 2.41
-9 -5 -5 5.93 1.14
-9 -5 -5 5.75 1.30
-9 -5 -5 4.09 1.02
9 5 5 7.32 1.66
-9 -5 -6 10.21 1.42
9 5 6 9.27 1.67
-9 -5 -6 11.47 1.32
-9 -5 -7 0.46 0.54
-9 -5 -7 0.72 0.71
9 5 7 0.26 1.15
-9 -5 -8 44.18 2.49
9 5 8 43.01 2.84
-9 -5 -9 13.51 1.43
9 5 9 13.90 1.67
-9 -5 -10 2.36 0.67
-9 -6 2 70.96 2.49
-9 -6 1 1.74 0.68
-9 -6 0 8.00 1.13
9 6 0 6.08 1.20
-9 -6 -1 2.89 0.83
9 6 1 2.48 1.04
-9 -6 -2 9.48 1.19
9 6 2 9.09 1.70
-9 -6 -3 1.08 0.62
9 6 3 1.61 1.15
-9 -6 -4 14.59 1.37
9 6 4 15.55 1.86
-9 -6 -5 1.15 0.65
-9 -6 -5 0.08 0.87
9 6 5 1.57 1.11
-9 -6 -6 10.64 1.44
9 6 6 11.19 1.70
-9 -6 -7 -0.02 0.63
9 6 7 1.32 0.99
-9 -6 -8 10.67 1.33
9 6 8 12.30 1.42
-9 -6 -9 1.83 0.68
9 7 1 5.78 1.06
9 7 2 5.98 1.13
9 7 3 22.75 1.96
9 7 4 1.67 0.84
9 7 5 0.00 0.71
0 0 0 0.00 0.00
TITL kee10 in P-1
REM P-1 (#2 in standard setting)
CELL 1.54184 7.524057 8.289831 18.735926 89.7378 79.6264 64.7408
ZERR 4.00 0.000283 0.000261 0.000558 0.0025 0.0029 0.0034
LATT 1
SFAC C H N O
UNIT 36.00 49.76 8.00 16.88
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 98137
_shelx_res_file
;
TITL kee10_a.res in P-1
kee10.res
created by SHELXL-2017/1 at 17:48:19 on 22-Oct-2018
REM Old TITL kee10 in P-1 #2
REM SHELXT solution in P-1
REM R1 0.151, Rweak 0.007, Alpha 0.039, Orientation as input
REM Formula found by SHELXT: C18 N5 O8
CELL 1.54184 7.5241 8.2898 18.7359 89.738 79.626 64.741
ZERR 4 0.0003 0.0003 0.0006 0.003 0.003 0.004
LATT 1
SFAC C H N O
UNIT 36 49.77 8 16.89
L.S. 10
PLAN 10
TEMP -173
BOND $H
list 4
fmap 2
ACTA
REM
REM
REM
WGHT 0.045900 0.460600
EXTI 0.004951
FVAR 0.99235 0.44285
C21 1 0.639473 0.247572 0.816494 11.00000 0.01998 0.01890 =
0.02334 0.00086 -0.00739 -0.00687
O23 4 0.815559 0.129195 0.792881 11.00000 0.02204 0.02778 =
0.02688 0.00295 -0.00407 -0.00119
O24 4 0.534514 0.260881 0.876728 11.00000 0.02438 0.02737 =
0.02717 0.00803 -0.00212 -0.00454
SAME 0.02 0.04 C22 > O27
C22 1 0.548693 0.384245 0.762922 11.00000 0.01928 0.03088 =
0.02109 0.00438 -0.00534 -0.00615
O28 4 0.440654 0.367761 0.726797 11.00000 0.09999 0.11244 =
0.08453 0.06978 -0.07814 -0.08172
O27 4 0.602700 0.513645 0.761215 11.00000 0.06406 0.02660 =
0.04741 0.01803 -0.03605 -0.02050
AFIX 83
H27 2 0.543889 0.587961 0.732904 11.00000 -1.50000
AFIX 0
C41 1 0.310164 0.881865 0.695967 11.00000 0.02135 0.02137 =
0.02220 0.00444 -0.00513 -0.00765
C42 1 0.203331 1.003183 0.638891 11.00000 0.02310 0.02095 =
0.02326 0.00380 -0.00596 -0.00771
O43 4 0.280180 0.978913 0.574866 11.00000 0.03038 0.03019 =
0.02323 0.00798 -0.00481 -0.00643
O44 4 0.026090 1.134927 0.664420 11.00000 0.02511 0.02737 =
0.02456 0.00466 -0.00589 -0.00250
AFIX 147
H44 2 -0.013467 1.120732 0.707824 11.00000 -1.50000
AFIX 0
O45 4 0.460615 0.739009 0.669429 11.00000 0.04079 0.02380 =
0.02407 0.00509 -0.00412 0.00368
O46 4 0.242682 0.933780 0.760302 11.00000 0.02763 0.03640 =
0.02166 0.00140 -0.00548 -0.00014
N31 3 0.648256 0.590629 0.534714 11.00000 0.02488 0.02526 =
0.02633 -0.00176 -0.00398 -0.00838
AFIX 43
H31 2 0.559425 0.667206 0.570245 11.00000 -1.20000
AFIX 0
C32 1 0.786448 0.432789 0.550256 11.00000 0.02935 0.02737 =
0.02199 0.00369 -0.00810 -0.01309
AFIX 43
H32 2 0.785917 0.406403 0.599668 11.00000 -1.20000
AFIX 0
C33 1 0.926451 0.310500 0.497046 11.00000 0.02584 0.02173 =
0.02240 0.00459 -0.00898 -0.00951
AFIX 43
H33 2 1.022104 0.200326 0.509378 11.00000 -1.20000
AFIX 0
C34 1 0.928878 0.348478 0.422806 11.00000 0.02540 0.02198 =
0.02125 0.00266 -0.00779 -0.01209
C35 1 0.779664 0.516103 0.408838 11.00000 0.02812 0.02614 =
0.02309 0.00701 -0.01148 -0.01237
AFIX 43
H35 2 0.773915 0.547156 0.360160 11.00000 -1.20000
AFIX 0
C36 1 0.645530 0.631622 0.465115 11.00000 0.02477 0.02372 =
0.03187 0.00536 -0.01120 -0.00899
AFIX 43
H36 2 0.547814 0.743611 0.455160 11.00000 -1.20000
AFIX 0
N37 3 1.065732 0.232418 0.368999 11.00000 0.03207 0.02452 =
0.02083 0.00139 -0.00459 -0.01059
C38 1 1.224142 0.065618 0.385138 11.00000 0.03006 0.02402 =
0.03337 -0.00199 -0.00469 -0.00771
AFIX 137
H38A 2 1.306530 -0.004623 0.339489 11.00000 -1.50000
H38B 2 1.163647 -0.003441 0.414125 11.00000 -1.50000
H38C 2 1.308285 0.093268 0.412603 11.00000 -1.50000
AFIX 0
C39 1 1.074094 0.280387 0.293566 11.00000 0.04543 0.03862 =
0.01976 0.00177 -0.00408 -0.01915
AFIX 137
H39A 2 1.177294 0.178370 0.261209 11.00000 -1.50000
H39B 2 1.106919 0.382807 0.288657 11.00000 -1.50000
H39C 2 0.943665 0.312091 0.280341 11.00000 -1.50000
AFIX 0
N11 3 0.935509 -0.089179 0.902576 11.00000 0.03470 0.02278 =
0.02605 0.00629 -0.01407 -0.01147
AFIX 43
H11 2 0.905583 -0.023294 0.865684 11.00000 -1.20000
AFIX 0
C12 1 1.109567 -0.238484 0.894169 11.00000 0.03216 0.02700 =
0.02554 0.00161 -0.00834 -0.01266
AFIX 43
H12 2 1.198139 -0.271263 0.848133 11.00000 -1.20000
AFIX 0
C13 1 1.161745 -0.343634 0.950031 11.00000 0.02530 0.02113 =
0.02849 0.00083 -0.00917 -0.00764
AFIX 43
H13 2 1.284904 -0.448706 0.942505 11.00000 -1.20000
AFIX 0
C14 1 1.032545 -0.296523 1.019393 11.00000 0.02785 0.02071 =
0.02677 0.00427 -0.01275 -0.01315
C15 1 0.849514 -0.138567 1.025761 11.00000 0.02926 0.02298 =
0.02639 0.00110 -0.00855 -0.01001
AFIX 43
H15 2 0.756700 -0.101448 1.070848 11.00000 -1.20000
AFIX 0
C16 1 0.807208 -0.040464 0.967248 11.00000 0.02923 0.01997 =
0.03154 0.00209 -0.01254 -0.00806
AFIX 43
H16 2 0.684523 0.064542 0.972233 11.00000 -1.20000
AFIX 0
N17 3 1.079774 -0.395051 1.075858 11.00000 0.02861 0.02510 =
0.02781 0.00751 -0.01160 -0.01220
C18 1 1.272288 -0.551486 1.069373 11.00000 0.03173 0.02702 =
0.03757 0.01013 -0.01794 -0.01086
AFIX 137
H18A 2 1.380322 -0.513174 1.062420 11.00000 -1.50000
H18B 2 1.291850 -0.631894 1.027518 11.00000 -1.50000
H18C 2 1.273973 -0.614446 1.113826 11.00000 -1.50000
AFIX 0
C19 1 0.943814 -0.344563 1.146850 11.00000 0.03840 0.03526 =
0.02562 0.00655 -0.01005 -0.01675
AFIX 137
H19A 2 0.815307 -0.342245 1.141889 11.00000 -1.50000
H19B 2 0.922145 -0.225643 1.165034 11.00000 -1.50000
H19C 2 1.002919 -0.431983 1.181181 11.00000 -1.50000
AFIX 6
O51 4 0.535176 0.904323 0.847045 21.00000 0.02545 0.02231 =
0.03064 0.00314 -0.00927 -0.00754
H51A 2 0.525878 1.012002 0.852157 21.00000 -1.50000
H51B 2 0.451198 0.913256 0.819034 21.00000 -1.50000
AFIX 0
HKLF 4
REM kee10_a.res in P-1
REM R1 = 0.0386 for 3792 Fo > 4sig(Fo) and 0.0453 for all 4321 data
REM 290 parameters refined using 0 restraints
END
WGHT 0.0459 0.4606
REM Highest difference peak 0.641, deepest hole -0.605, 1-sigma level 0.042
Q1 1 0.3830 0.4645 0.7524 11.00000 0.05 0.64
Q2 1 0.5121 0.3567 0.7004 11.00000 0.05 0.46
Q3 1 0.4380 0.3186 0.7264 11.00000 0.05 0.35
Q4 1 0.2516 0.9426 0.6667 11.00000 0.05 0.28
Q5 1 0.5990 0.3147 0.7900 11.00000 0.05 0.28
Q6 1 0.9396 -0.2243 1.0235 11.00000 0.05 0.23
Q7 1 1.1007 -0.3037 0.9868 11.00000 0.05 0.21
Q8 1 0.9399 0.3351 0.4608 11.00000 0.05 0.20
Q9 1 0.8422 0.3658 0.5189 11.00000 0.05 0.20
Q10 1 1.0262 0.3026 0.3973 11.00000 0.05 0.20
;
_shelx_res_checksum 69565
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
C C21 0.63947(19) 0.24757(17) 0.81649(7) 0.0209(3) Uani d 1
O O23 0.81556(15) 0.12920(14) 0.79288(5) 0.0291(2) Uani d 1
O O24 0.53451(15) 0.26088(13) 0.87673(5) 0.0291(2) Uani d 1
C C22 0.5487(2) 0.38424(19) 0.76292(7) 0.0252(3) Uani d 1
O O28 0.4407(3) 0.3678(3) 0.72680(10) 0.0782(6) Uani d 1
O O27 0.6027(2) 0.51364(15) 0.76121(7) 0.0423(3) Uani d 1
H H27 0.543889 0.587961 0.732904 0.063 Uiso calc 1
C C41 0.31016(19) 0.88186(18) 0.69597(7) 0.0221(3) Uani d 1
C C42 0.2033(2) 1.00318(18) 0.63889(7) 0.0229(3) Uani d 1
O O43 0.28018(16) 0.97891(14) 0.57487(5) 0.0304(2) Uani d 1
O O44 0.02609(15) 1.13493(14) 0.66442(5) 0.0287(2) Uani d 1
H H44 -0.013467 1.120732 0.707824 0.043 Uiso calc 1
O O45 0.46062(17) 0.73901(14) 0.66943(6) 0.0362(3) Uani d 1
O O46 0.24268(16) 0.93378(15) 0.76030(5) 0.0334(3) Uani d 1
N N31 0.64826(18) 0.59063(16) 0.53471(7) 0.0265(3) Uani d 1
H H31 0.559425 0.667206 0.570245 0.032 Uiso calc 1
C C32 0.7864(2) 0.43279(19) 0.55026(7) 0.0255(3) Uani d 1
H H32 0.785917 0.406403 0.599668 0.031 Uiso calc 1
C C33 0.9265(2) 0.31050(18) 0.49705(7) 0.0230(3) Uani d 1
H H33 1.022104 0.200326 0.509378 0.028 Uiso calc 1
C C34 0.9289(2) 0.34848(17) 0.42281(7) 0.0218(3) Uani d 1
C C35 0.7797(2) 0.51610(18) 0.40884(7) 0.0247(3) Uani d 1
H H35 0.773915 0.547156 0.360160 0.030 Uiso calc 1
C C36 0.6455(2) 0.63162(19) 0.46511(8) 0.0266(3) Uani d 1
H H36 0.547814 0.743611 0.455160 0.032 Uiso calc 1
N N37 1.06573(19) 0.23242(16) 0.36900(6) 0.0265(3) Uani d 1
C C38 1.2241(2) 0.0656(2) 0.38514(8) 0.0308(3) Uani d 1
H H38A 1.306530 -0.004623 0.339489 0.046 Uiso calc 1
H H38B 1.163647 -0.003441 0.414125 0.046 Uiso calc 1
H H38C 1.308285 0.093268 0.412603 0.046 Uiso calc 1
C C39 1.0741(3) 0.2804(2) 0.29357(8) 0.0346(3) Uani d 1
H H39A 1.177294 0.178370 0.261209 0.052 Uiso calc 1
H H39B 1.106919 0.382807 0.288657 0.052 Uiso calc 1
H H39C 0.943665 0.312091 0.280341 0.052 Uiso calc 1
N N11 0.93551(19) -0.08918(16) 0.90258(6) 0.0271(3) Uani d 1
H H11 0.905583 -0.023294 0.865684 0.033 Uiso calc 1
C C12 1.1096(2) -0.23848(19) 0.89417(8) 0.0279(3) Uani d 1
H H12 1.198139 -0.271263 0.848133 0.034 Uiso calc 1
C C13 1.1617(2) -0.34363(18) 0.95003(8) 0.0253(3) Uani d 1
H H13 1.284904 -0.448706 0.942505 0.030 Uiso calc 1
C C14 1.0325(2) -0.29652(18) 1.01939(7) 0.0232(3) Uani d 1
C C15 0.8495(2) -0.13857(18) 1.02576(8) 0.0262(3) Uani d 1
H H15 0.756700 -0.101448 1.070848 0.031 Uiso calc 1
C C16 0.8072(2) -0.04046(18) 0.96725(8) 0.0269(3) Uani d 1
H H16 0.684523 0.064542 0.972233 0.032 Uiso calc 1
N N17 1.07977(18) -0.39505(16) 1.07586(7) 0.0262(3) Uani d 1
C C18 1.2723(2) -0.5515(2) 1.06937(9) 0.0313(3) Uani d 1
H H18A 1.380322 -0.513174 1.062420 0.047 Uiso calc 1
H H18B 1.291850 -0.631894 1.027518 0.047 Uiso calc 1
H H18C 1.273973 -0.614446 1.113826 0.047 Uiso calc 1
C C19 0.9438(2) -0.3446(2) 1.14685(8) 0.0323(3) Uani d 1
H H19A 0.815307 -0.342245 1.141889 0.048 Uiso calc 1
H H19B 0.922145 -0.225643 1.165034 0.048 Uiso calc 1
H H19C 1.002919 -0.431983 1.181181 0.048 Uiso calc 1
O O51 0.5352(3) 0.9043(3) 0.84705(12) 0.0266(7) Uani d 0.443(4)
H H51A 0.525878 1.012002 0.852157 0.040 Uiso d 0.443(4)
H H51B 0.451198 0.913256 0.819034 0.040 Uiso d 0.443(4)
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
C21 0.0200(6) 0.0189(6) 0.0233(6) -0.0069(5) -0.0074(5) 0.0009(5)
O23 0.0220(5) 0.0278(5) 0.0269(5) -0.0012(4) -0.0041(4) 0.0030(4)
O24 0.0244(5) 0.0274(5) 0.0272(5) -0.0045(4) -0.0021(4) 0.0080(4)
C22 0.0193(6) 0.0309(7) 0.0211(6) -0.0061(5) -0.0053(5) 0.0044(5)
O28 0.1000(13) 0.1124(14) 0.0845(12) -0.0817(12) -0.0781(11) 0.0698(11)
O27 0.0641(8) 0.0266(6) 0.0474(7) -0.0205(6) -0.0360(6) 0.0180(5)
C41 0.0213(6) 0.0214(6) 0.0222(6) -0.0077(5) -0.0051(5) 0.0044(5)
C42 0.0231(6) 0.0210(6) 0.0233(6) -0.0077(5) -0.0060(5) 0.0038(5)
O43 0.0304(5) 0.0302(5) 0.0232(5) -0.0064(4) -0.0048(4) 0.0080(4)
O44 0.0251(5) 0.0274(5) 0.0246(5) -0.0025(4) -0.0059(4) 0.0047(4)
O45 0.0408(6) 0.0238(5) 0.0241(5) 0.0037(5) -0.0041(4) 0.0051(4)
O46 0.0276(5) 0.0364(6) 0.0217(5) -0.0001(4) -0.0055(4) 0.0014(4)
N31 0.0249(6) 0.0253(6) 0.0263(6) -0.0084(5) -0.0040(5) -0.0018(5)
C32 0.0293(7) 0.0274(7) 0.0220(6) -0.0131(6) -0.0081(5) 0.0037(5)
C33 0.0258(6) 0.0217(6) 0.0224(6) -0.0095(5) -0.0090(5) 0.0046(5)
C34 0.0254(6) 0.0220(6) 0.0213(6) -0.0121(5) -0.0078(5) 0.0027(5)
C35 0.0281(7) 0.0261(7) 0.0231(6) -0.0124(6) -0.0115(5) 0.0070(5)
C36 0.0248(7) 0.0237(7) 0.0319(7) -0.0090(5) -0.0112(5) 0.0054(5)
N37 0.0321(6) 0.0245(6) 0.0208(6) -0.0106(5) -0.0046(5) 0.0014(4)
C38 0.0301(7) 0.0240(7) 0.0334(8) -0.0077(6) -0.0047(6) -0.0020(6)
C39 0.0454(9) 0.0386(8) 0.0198(7) -0.0191(7) -0.0041(6) 0.0018(6)
N11 0.0347(6) 0.0228(6) 0.0261(6) -0.0115(5) -0.0141(5) 0.0063(4)
C12 0.0322(7) 0.0270(7) 0.0255(7) -0.0127(6) -0.0083(6) 0.0016(5)
C13 0.0253(6) 0.0211(6) 0.0285(7) -0.0076(5) -0.0092(5) 0.0008(5)
C14 0.0278(7) 0.0207(6) 0.0268(7) -0.0132(5) -0.0127(5) 0.0043(5)
C15 0.0293(7) 0.0230(7) 0.0264(7) -0.0100(6) -0.0085(5) 0.0011(5)
C16 0.0292(7) 0.0200(6) 0.0315(7) -0.0081(5) -0.0125(6) 0.0021(5)
N17 0.0286(6) 0.0251(6) 0.0278(6) -0.0122(5) -0.0116(5) 0.0075(5)
C18 0.0317(7) 0.0270(7) 0.0376(8) -0.0109(6) -0.0179(6) 0.0101(6)
C19 0.0384(8) 0.0353(8) 0.0256(7) -0.0167(7) -0.0100(6) 0.0065(6)
O51 0.0255(12) 0.0223(12) 0.0306(13) -0.0075(9) -0.0093(9) 0.0031(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0673
-2 3 6 0.0988
-1 -5 0 0.0720
0 1 1 0.0840
-3 -5 -4 0.0541
-4 -5 -3 0.0518
3 0 -5 0.0891
-3 -5 -1 0.0506
-3 0 5 0.0992
-4 -4 -1 0.0623
0 1 -12 0.0464
-2 4 2 0.0913
5 2 -2 0.0741
2 -4 6 0.1065
0 5 -1 0.0905
-2 -3 8 0.0759
-2 -2 9 0.0765
0 -4 -3 0.0770
-2 -5 -3 0.0584
0 1 -12 0.0517
-1 -3 -10 0.0587
-2 -2 -11 0.0518
-4 1 -6 0.1092
1 1 -12 0.0436
0 2 -11 0.0524
3 3 -7 0.0539
2 5 -3 0.0783
4 4 1 0.0575
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O23 C21 C22 115.43(11) ?
O24 C21 O23 126.89(13) y
O24 C21 C22 117.66(11) ?
O28 C22 C21 121.46(14) ?
O28 C22 O27 125.39(14) y
O27 C22 C21 113.14(12) ?
C22 O27 H27 109.5 ?
O45 C41 C42 114.75(11) ?
O46 C41 C42 117.86(12) ?
O46 C41 O45 127.39(13) y
O43 C42 C41 121.78(12) ?
O43 C42 O44 122.19(12) y
O44 C42 C41 116.02(11) ?
C42 O44 H44 109.5 ?
C32 N31 H31 119.8 ?
C36 N31 H31 119.8 ?
C36 N31 C32 120.39(12) ?
N31 C32 H32 119.1 ?
N31 C32 C33 121.76(13) ?
C33 C32 H32 119.1 ?
C32 C33 H33 120.2 ?
C32 C33 C34 119.66(13) ?
C34 C33 H33 120.2 ?
C33 C34 C35 116.72(12) ?
N37 C34 C33 121.39(12) ?
N37 C34 C35 121.88(12) ?
C34 C35 H35 120.0 ?
C36 C35 C34 120.06(13) ?
C36 C35 H35 120.0 ?
N31 C36 C35 121.40(13) ?
N31 C36 H36 119.3 ?
C35 C36 H36 119.3 ?
C34 N37 C38 120.70(12) ?
C34 N37 C39 120.23(12) ?
C38 N37 C39 118.64(12) ?
N37 C38 H38A 109.5 ?
N37 C38 H38B 109.5 ?
N37 C38 H38C 109.5 ?
H38A C38 H38B 109.5 ?
H38A C38 H38C 109.5 ?
H38B C38 H38C 109.5 ?
N37 C39 H39A 109.5 ?
N37 C39 H39B 109.5 ?
N37 C39 H39C 109.5 ?
H39A C39 H39B 109.5 ?
H39A C39 H39C 109.5 ?
H39B C39 H39C 109.5 ?
C12 N11 H11 119.9 ?
C16 N11 H11 119.9 ?
C16 N11 C12 120.22(12) ?
N11 C12 H12 119.2 ?
N11 C12 C13 121.67(14) ?
C13 C12 H12 119.2 ?
C12 C13 H13 119.9 ?
C12 C13 C14 120.14(13) ?
C14 C13 H13 119.9 ?
C13 C14 C15 116.37(12) ?
N17 C14 C13 121.90(13) ?
N17 C14 C15 121.73(13) ?
C14 C15 H15 119.9 ?
C16 C15 C14 120.14(13) ?
C16 C15 H15 119.9 ?
N11 C16 C15 121.46(13) ?
N11 C16 H16 119.3 ?
C15 C16 H16 119.3 ?
C14 N17 C18 121.00(12) ?
C14 N17 C19 121.01(12) ?
C18 N17 C19 117.93(12) ?
N17 C18 H18A 109.5 ?
N17 C18 H18B 109.5 ?
N17 C18 H18C 109.5 ?
H18A C18 H18B 109.5 ?
H18A C18 H18C 109.5 ?
H18B C18 H18C 109.5 ?
N17 C19 H19A 109.5 ?
N17 C19 H19B 109.5 ?
N17 C19 H19C 109.5 ?
H19A C19 H19B 109.5 ?
H19A C19 H19C 109.5 ?
H19B C19 H19C 109.5 ?
H51A O51 H51B 104.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C21 O23 1.2639(16) y
C21 O24 1.2310(17) y
C21 C22 1.5276(18) y
C22 O28 1.196(2) y
C22 O27 1.2976(19) y
O27 H27 0.8400 ?
C41 C42 1.5527(18) y
C41 O45 1.2608(17) ?
C41 O46 1.2222(17) ?
C42 O43 1.2112(17) ?
C42 O44 1.3161(16) ?
O44 H44 0.8400 ?
N31 H31 0.8800 ?
N31 C32 1.3500(19) ?
N31 C36 1.3476(19) ?
C32 H32 0.9500 ?
C32 C33 1.360(2) ?
C33 H33 0.9500 ?
C33 C34 1.4234(18) ?
C34 C35 1.4251(19) ?
C34 N37 1.3386(18) ?
C35 H35 0.9500 ?
C35 C36 1.360(2) ?
C36 H36 0.9500 ?
N37 C38 1.4641(19) ?
N37 C39 1.4641(18) ?
C38 H38A 0.9800 ?
C38 H38B 0.9800 ?
C38 H38C 0.9800 ?
C39 H39A 0.9800 ?
C39 H39B 0.9800 ?
C39 H39C 0.9800 ?
N11 H11 0.8800 ?
N11 C12 1.3476(19) ?
N11 C16 1.3467(19) ?
C12 H12 0.9500 ?
C12 C13 1.363(2) ?
C13 H13 0.9500 ?
C13 C14 1.418(2) ?
C14 C15 1.4243(19) ?
C14 N17 1.3388(18) ?
C15 H15 0.9500 ?
C15 C16 1.364(2) ?
C16 H16 0.9500 ?
N17 C18 1.4593(18) ?
N17 C19 1.4630(19) ?
C18 H18A 0.9800 ?
C18 H18B 0.9800 ?
C18 H18C 0.9800 ?
C19 H19A 0.9800 ?
C19 H19B 0.9800 ?
C19 H19C 0.9800 ?
O51 H51A 0.8694 ?
O51 H51B 0.8714 ?
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
O27 H27 O45 . 0.840 1.720 2.553(2) 170.79 yes
O44 H44 O23 1_465 0.840 1.840 2.645(2) 159.95 yes
N31 H31 O45 . 0.880 1.870 2.672(2) 150.73 yes
C33 H33 O43 1_645 0.950 2.538 3.447(2) 160.29 .
C35 H35 O28 2_666 0.950 2.392 3.204(2) 143.20 .
C39 H39A O51 2_766 0.980 2.536 3.367(2) 142.49 .
N11 H11 O23 . 0.880 1.872 2.749(2) 174.17 yes
C12 H12 O46 1_645 0.950 2.444 3.101(2) 126.20 .
C13 H13 O24 1_645 0.950 2.485 3.363(2) 153.57 .
C15 H15 O51 2_667 0.950 2.367 3.254(2) 155.21 .
C16 H16 O24 . 0.950 2.502 3.189(2) 129.24 .
C18 H18C O51 2_757 0.980 2.407 3.204(2) 138.13 .
C19 H19A O24 2_657 0.980 2.514 3.474(2) 166.47 .
C19 H19B O23 2_757 0.980 2.659 3.355(2) 128.23 .
C19 H19B O46 2_667 0.980 2.489 3.419(2) 158.34 .
_cod_database_fobs_code 2242743