#------------------------------------------------------------------------------
#$Date: 2018-11-17 05:48:50 +0200 (Sat, 17 Nov 2018) $
#$Revision: 212035 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/27/2242744.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_2242744
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_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 'C9 H14 N +, C2 H O4 -'
_chemical_formula_moiety 'C9 H14 N +, C2 H O4 -'
_chemical_formula_sum 'C11 H15 N O4'
_chemical_formula_weight 225.24
_chemical_name_common '4-t-butylpyridinium hydrogen oxalate'
_chemical_name_systematic
;
4-tert-Butylpyridinium hydrogen oxalate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 90
_cell_angle_beta 95.3010(10)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 9.70430(10)
_cell_length_b 20.6128(2)
_cell_length_c 11.3649(2)
_cell_measurement_reflns_used 12822
_cell_measurement_temperature 100.9(4)
_cell_measurement_theta_max 76.7270
_cell_measurement_theta_min 4.2840
_cell_volume 2263.63(5)
_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
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 100.9(4)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_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 0.0262
_diffrn_reflns_av_unetI/netI 0.0175
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 23245
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 76.881
_diffrn_reflns_theta_min 4.290
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.844
_exptl_absorpt_correction_T_max 0.914
_exptl_absorpt_correction_T_min 0.875
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2017)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.322
_exptl_crystal_description block
_exptl_crystal_F_000 960
_exptl_crystal_size_max 0.226
_exptl_crystal_size_mid 0.207
_exptl_crystal_size_min 0.151
_refine_diff_density_max 0.296
_refine_diff_density_min -0.195
_refine_ls_extinction_coef 0.0014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref 1.030
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 298
_refine_ls_number_reflns 4749
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.030
_refine_ls_R_factor_all 0.0353
_refine_ls_R_factor_gt 0.0316
_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^)+(0.0436P)^2^+0.6305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0826
_refine_ls_wR_factor_ref 0.0858
_reflns_number_gt 4309
_reflns_number_total 4749
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file qm2130sup1.cif
_cod_data_source_block 2
_cod_database_code 2242744
_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 1 4.16959 12.3216 27
0 0 2 165071. 983.081 27
0 0 3-12.1822 62.5857 27
0 0 4 3.43670 56.2882 27
0 0 5-26.9005 77.9130 27
0 0 6 3078.10 279.529 27
0 0 7 3.52030 86.1894 27
0 0 8 298.383 130.071 27
0 0 9-46.2423 58.7460 16
0 0 9-118.748 104.514 14
0 0 9 35.7031 66.0959 20
0 0 9-54.7006 121.368 27
0 0 10 112489. 1500.79 20
0 0 10 115263. 1518.07 16
0 0 10 109946. 1543.21 14
0 0 11-91.2194 96.7064 14
0 0 11-4.41867 68.7301 16
0 0 12 6125.54 338.435 14
0 0 12 6440.28 322.443 16
0 0 13 56.0275 34.5161 29
0 0 -13 2.01550 67.7812 12
0 0 13 41.9756 58.7108 14
0 0 -14 364.657 67.9271 12
0 1 1 233.606 30.9142 27
0 -1 1 185.852 31.0208 27
0 -1 -2 59956.6 387.595 2
0 -1 2 59758.7 613.652 27
0 -1 3 126685. 1103.20 27
0 1 3 127967. 1063.75 27
0 -1 4 621.089 108.084 27
0 1 4 509.312 90.1527 27
0 -1 5 195481. 1851.41 27
0 1 5 190372. 1786.69 27
0 1 6 646.797 140.332 27
0 -1 6 518.376 127.592 27
0 1 7 10031.1 526.189 27
0 -1 7 9550.23 525.524 27
0 -1 8 667.163 175.993 27
0 1 8 608.807 150.702 27
0 1 9 1915.76 193.434 16
0 -1 9 1765.47 189.652 20
0 -1 9 2351.80 325.639 27
0 1 9 1920.44 300.721 27
0 -1 9 2075.65 207.780 16
0 1 9 1930.31 204.968 20
0 1 9 2196.59 223.931 14
0 1 10 2329.79 223.902 20
0 -1 10 2218.47 243.166 14
0 1 10 2559.70 262.371 14
0 -1 10 2310.16 227.594 16
0 -1 10 2409.16 238.837 20
0 1 10 2731.72 247.692 16
0 1 11 980.112 152.923 16
0 1 11 864.984 155.257 14
0 -1 11 791.882 138.002 16
0 -1 11 665.781 154.605 14
0 -1 11 591.711 140.805 20
0 -1 12 15512.3 528.665 14
0 1 12 14299.0 479.782 16
0 1 12 14531.5 509.951 14
0 -1 12 13919.6 462.175 16
0 -1 -13 3697.01 257.202 12
0 1 13 3598.22 177.689 29
0 1 13 3565.00 218.287 14
0 1 -13 3230.47 234.139 12
0 -1 13 3181.13 206.883 14
0 -1 -14 312.635 69.1752 12
0 1 -14 313.828 62.8787 12
0 -2 0 16721.9 209.956 3
0 2 0 18514.3 225.479 1
0 2 1 16136.4 245.783 1
0 -2 1 15688.4 275.430 27
0 -2 2 9639.84 266.962 27
0 2 2 7397.39 218.205 27
0 2 3 105313. 984.933 27
0 -2 3 106638. 1049.53 27
0 2 4 8323.83 326.113 27
0 -2 4 8263.79 344.270 27
0 2 5 167.475 77.7715 27
0 -2 5 182.160 90.9334 27
0 -2 6 7472.68 424.013 27
0 2 6 7094.80 398.669 27
0 2 7 4419.05 352.845 27
0 -2 7 4480.26 372.427 27
0 2 8 2006.25 278.463 27
0 -2 8 2320.21 293.949 27
0 2 8 2162.75 199.401 20
0 -2 8 1907.69 190.256 20
0 2 9 9063.19 436.880 14
0 2 9 9637.12 436.173 16
0 2 9 9039.27 422.176 20
0 2 9 9480.45 620.034 27
0 -2 9 9725.88 441.155 20
0 -2 9 8920.79 626.188 27
0 -2 9 9130.05 418.921 16
0 -2 10 13722.0 517.227 16
0 2 10 13261.6 542.002 14
0 2 10 14054.3 542.415 16
0 -2 10 12896.0 518.618 20
0 -2 11 2940.31 256.520 20
0 2 11 3132.78 259.404 16
0 -2 11 3129.00 243.373 16
0 -2 11 3012.37 262.837 14
0 2 11 3040.60 263.565 14
0 2 12 352.455 95.9846 16
0 2 12 258.962 100.549 14
0 -2 12 381.661 120.516 14
0 -2 12 356.676 91.6284 16
0 -2 -13 1174.60 149.425 12
0 -2 13 1321.32 137.366 14
0 2 -13 1168.98 153.220 12
0 -2 -13 1130.58 114.945 9
0 2 13 1245.44 136.052 14
0 -2 -14 105.345 52.8195 12
0 2 -14 1.06586 33.4519 12
0 3 0 6.62203 9.45312 4
0 3 0-10.7539 19.6064 1
0 -3 0-20.7919 23.1216 3
0 -3 -1 3066.49 115.006 3
0 -3 1 2915.07 140.989 27
0 3 1 3055.97 122.368 1
0 3 2 26102.7 438.468 1
0 -3 2 26540.9 479.045 27
0 3 2 26344.9 429.698 27
0 -3 -3 38655.5 377.627 2
0 -3 3 37716.4 657.574 27
0 3 3 36930.6 601.797 27
0 3 4 13981.5 429.171 27
0 -3 4 13577.7 454.311 27
0 3 5 16261.2 527.542 27
0 -3 5 16905.7 577.867 27
0 3 6 9847.97 465.405 27
0 -3 6 9954.84 503.806 27
0 -3 7 8712.23 521.457 27
0 3 7 9677.06 517.172 27
0 3 8 9432.83 566.786 27
0 3 8 10243.9 417.334 20
0 3 8 10422.3 430.324 16
0 -3 8 10513.9 422.070 20
0 3 8 10032.8 426.582 14
0 -3 8 9589.46 606.592 27
0 -3 9 1474.53 171.856 20
0 3 9 1328.59 186.848 14
0 3 9 1463.32 180.236 20
0 3 9 1445.75 244.055 27
0 -3 9 1863.28 308.274 27
0 -3 9 1475.63 167.258 16
0 3 9 1765.67 195.892 16
0 -3 10 8998.97 421.976 16
0 -3 10 8523.05 424.076 20
0 3 10 8401.49 423.892 16
0 3 10 8732.50 438.871 14
0 -3 11 1570.14 189.579 20
0 -3 11 1616.65 217.108 14
0 3 11 1181.55 175.314 16
0 3 11 1437.23 194.329 14
0 -3 11 1346.18 169.502 16
0 -3 12 3205.51 246.922 14
0 3 12 3034.72 232.978 16
0 -3 12 2891.01 207.619 16
0 3 12 2803.88 231.725 14
0 3 -13 311.733 98.2224 12
0 -3 13 366.304 77.9911 14
0 3 13 554.679 99.3740 14
0 -3 -13 385.429 101.490 12
0 -3 -13 418.078 82.2629 9
0 -3 -14 1011.70 95.7031 12
0 3 -14 1074.93 99.1728 12
0 4 1 7951.02 219.974 1
0 -4 1 8310.61 264.944 27
0 -4 -1 8263.92 209.162 3
0 4 2 21581.1 418.961 27
0 -4 2 23211.4 484.907 27
0 -4 -2 21835.7 389.643 3
0 4 2 22599.5 424.997 1
0 4 3 14579.1 392.101 27
0 -4 3 14541.0 434.669 27
0 -4 -4 4988.61 140.564 2
0 4 4 5053.36 267.701 27
0 -4 4 4997.76 293.734 27
0 4 5 17951.5 563.910 27
0 -4 5 18808.2 630.700 27
0 -4 6 1255.63 193.254 27
0 4 6 891.604 148.511 27
0 -4 7-69.7934 96.6285 27
0 4 7-66.8802 71.7199 27
0 -4 8 19082.5 860.082 27
0 4 8 19569.2 811.310 27
0 4 8 19296.8 584.917 16
0 4 8 18605.6 587.235 14
0 -4 8 19186.5 570.617 20
0 -4 9 14897.3 825.658 27
0 4 9 13864.4 542.693 14
0 -4 9 13036.4 498.788 16
0 4 9 14031.4 533.136 16
0 -4 9 13581.2 516.534 20
0 4 9 14115.5 752.216 27
0 -4 10 18837.2 620.508 20
0 4 10 19694.4 636.648 16
0 -4 10 19667.2 610.672 16
0 4 10 18544.3 635.470 14
0 -4 11 30201.0 709.698 16
0 -4 11 30267.4 799.076 14
0 -4 11 30630.2 768.956 20
0 4 11 29935.0 764.650 16
0 4 11 28757.9 764.073 14
0 -4 12 1684.42 156.736 16
0 -4 12 1975.82 200.936 14
0 4 12 2045.56 193.590 14
0 -4 -12 1907.56 211.970 12
0 -4 -13 3346.83 184.559 9
0 4 -13 2826.68 208.519 12
0 4 13 3089.59 189.009 14
0 -4 -13 2939.27 214.586 12
0 -4 13 3087.72 193.519 14
0 -5 0-13.5452 32.1824 3
0 5 0 32.0496 31.6493 1
0 5 0 7.89345 11.4506 4
0 5 1 13795.8 220.426 4
0 5 1 13848.5 318.567 1
0 -5 1 14085.4 376.370 27
0 -5 1 13437.2 332.284 3
0 -5 -1 13499.5 297.985 3
0 5 2 6536.56 250.568 1
0 -5 2 6913.05 290.965 27
0 -5 -2 6632.71 228.127 3
0 5 3 30114.8 591.510 27
0 5 3 29551.5 608.108 1
0 -5 4 64589.4 1082.43 27
0 5 4 62042.8 950.765 27
0 -5 -4 63362.7 546.146 2
0 5 5 92308.0 1296.89 27
0 -5 5 92622.4 1445.89 27
0 -5 6 7724.94 470.198 27
0 5 6 6953.19 399.611 27
0 5 7 49744.3 1182.02 27
0 -5 7 51155.9 1314.99 27
0 -5 8 9926.72 637.853 27
0 5 8 10145.5 430.922 16
0 -5 8 10008.8 416.908 20
0 5 8 9914.95 442.668 14
0 5 8 9505.44 573.456 27
0 -5 9 477.287 123.941 20
0 -5 9 232.784 167.493 27
0 -5 9 504.968 113.554 16
0 5 9 543.517 130.167 16
0 5 9 469.506 140.945 14
0 5 9 401.657 169.523 27
0 5 10 30758.1 813.042 14
0 5 10 30661.4 796.915 16
0 -5 10 33295.9 776.860 16
0 -5 10 31575.5 799.732 20
0 -5 11 345.581 87.4128 16
0 5 11 634.198 151.389 14
0 -5 11 440.920 125.396 20
0 5 11 384.244 135.058 16
0 -5 12 3836.85 250.333 20
0 -5 12 3290.96 246.308 14
0 -5 -12 3523.17 226.031 9
0 5 12 3618.09 247.371 14
0 -5 -12 3313.93 258.012 12
0 5 -12 3226.76 255.364 12
0 -5 12 3191.67 195.327 16
0 5 12 3411.74 182.006 11
0 -5 -13 1606.00 154.456 12
0 5 -13 1625.62 156.508 12
0 5 13 1760.02 134.035 14
0 -5 13 1914.05 148.983 14
0 -5 -13 1912.44 138.987 9
0 -6 0 29425.3 491.371 3
0 6 0 29145.2 495.645 1
0 -6 -1 71508.2 747.986 3
0 -6 1 72335.8 829.214 3
0 6 1 72461.5 512.239 4
0 6 1 71193.9 801.473 1
0 6 2 34719.2 611.674 1
0 -6 -2 34403.5 551.197 3
0 -6 2 35224.4 698.654 27
0 -6 3 29788.7 699.123 27
0 6 3 28489.2 606.903 27
0 6 3 28343.1 623.537 1
0 -6 4 1709.19 205.740 27
0 -6 -4 2041.22 111.092 2
0 6 4 1814.95 178.469 27
0 -6 5 19412.0 686.030 27
0 6 5 18862.9 605.271 27
0 6 6 4902.48 347.379 27
0 -6 6 5617.49 414.394 27
0 6 7 51670.6 1215.40 27
0 -6 7 53252.5 1375.66 27
0 6 8 12676.2 667.869 27
0 -6 8 13062.7 745.925 27
0 -6 8 12369.9 465.391 20
0 6 8 12522.1 482.681 16
0 6 8 12493.3 497.740 14
0 -6 9-135.147 80.4168 20
0 6 9 39.1363 118.997 27
0 -6 9 160.314 56.5857 16
0 6 9 144.297 80.5167 16
0 -6 9 122.060 106.243 27
0 6 9-117.125 92.8959 14
0 6 10 12092.4 514.508 14
0 6 10 12633.2 514.209 16
0 -6 10 12111.6 492.198 20
0 -6 10 13277.3 479.663 16
0 -6 11 1115.36 161.651 20
0 -6 11 843.412 125.386 16
0 6 11 905.379 159.623 14
0 6 12 207.258 68.7052 11
0 -6 -12 177.680 90.0028 12
0 -6 12 268.111 90.9762 20
0 6 -12 298.989 103.642 12
0 6 12 226.818 86.2639 14
0 -6 12 222.110 90.0256 14
0 -6 -12 276.738 83.6387 9
0 -6 13 715.181 98.2161 14
0 6 13 668.697 83.4947 14
0 -6 -13 600.618 83.4169 9
0 6 -13 665.769 101.141 12
0 -6 -13 610.955 92.7826 12
0 7 0 150.968 61.0382 1
0 -7 0 0.87612 36.9331 3
0 -7 1 91198.1 1007.77 3
0 7 1 93806.1 991.312 1
0 7 1 93011.6 584.685 4
0 -7 -1 89629.7 912.272 3
0 -7 2 5763.57 310.027 27
0 7 2 6239.33 201.510 4
0 -7 2 6202.91 288.279 3
0 -7 -2 6284.30 252.673 3
0 7 2 6363.14 277.003 1
0 -7 -3 8154.16 314.895 3
0 7 3 9040.45 372.270 1
0 7 3 8338.89 348.859 27
0 -7 3 8782.18 408.277 27
0 7 4 91166.0 1239.71 27
0 -7 4 92789.5 1435.26 27
0 -7 5 72237.7 1374.80 27
0 7 5 72765.0 1213.96 27
0 -7 6 31068.6 991.647 27
0 7 6 31305.8 877.388 27
0 7 7 6781.37 452.566 27
0 -7 7 6960.45 520.769 27
0 7 8 6444.82 353.958 16
0 7 8 6342.53 472.747 27
0 -7 8 6007.08 518.726 27
0 -7 8 6122.33 333.212 20
0 7 8 6125.83 359.260 14
0 7 9 2128.32 213.481 16
0 7 9 2813.78 345.992 27
0 7 9 2356.67 246.880 14
0 -7 9 2402.36 228.796 20
0 7 10 3725.58 291.316 14
0 7 10 4389.03 310.023 16
0 -7 10 3945.97 283.564 20
0 -7 11 1094.38 158.973 20
0 -7 -11 1222.58 164.697 9
0 7 11 1054.80 162.194 14
0 -7 -12 10747.2 410.068 12
0 7 -12 10529.3 407.348 12
0 -7 -12 11613.0 381.423 9
0 7 12 10911.6 328.178 11
0 7 12 10623.8 392.744 14
0 -7 12 10395.9 378.486 20
0 -7 12 11758.2 429.118 14
0 -7 -13 6301.63 235.165 12
0 7 -13 6218.04 236.427 12
0 -7 13 6590.77 250.010 14
0 7 13 7010.22 240.563 29
0 -7 -13 7303.21 243.179 9
0 -8 0 737387. 2894.07 3
0 8 0 734226. 2951.14 1
0 8 1 3927.30 119.264 4
0 8 1 4078.55 231.084 1
0 -8 -1 4087.83 213.368 3
0 8 -1 3875.87 226.141 1
0 -8 1 4070.25 233.370 3
0 8 2 17105.8 328.314 4
0 -8 2 16501.6 497.570 3
0 8 2 16830.8 487.745 1
0 -8 -2 16745.7 434.701 3
0 8 3 3925.46 261.502 1
0 8 3 3696.79 250.200 27
0 -8 3 3610.30 288.012 27
0 8 3 3997.96 197.523 4
0 -8 -3 3905.06 229.401 3
0 8 4 582.834 121.560 27
0 -8 4 396.325 132.664 27
0 8 4 451.639 120.275 1
0 8 5 7609.81 411.854 27
0 -8 5 7422.27 469.935 27
0 -8 6 2788.49 331.019 27
0 8 6 3238.14 296.960 27
0 8 7 1560.04 227.879 27
0 -8 7 1822.16 286.700 27
0 -8 7 1689.50 175.454 20
0 8 7 1887.06 195.823 14
0 8 7 2122.29 197.133 16
0 -8 8 46155.0 904.251 20
0 8 8 44361.6 956.235 14
0 8 8 45327.0 1266.99 27
0 -8 8 45955.4 1456.74 27
0 8 8 45396.7 932.746 16
0 8 9 2823.82 262.003 14
0 -8 9 2699.47 235.656 20
0 8 9 2772.50 256.237 16
0 8 10 1893.22 215.646 14
0 -8 -10 2023.21 199.516 9
0 -8 10 1890.97 205.127 20
0 8 -11 3761.60 272.082 12
0 -8 -11 3961.16 256.408 9
0 8 11 3753.56 270.005 14
0 -8 -11 3845.38 276.994 12
0 -8 11 3857.29 265.609 20
0 -8 12 685.952 120.219 14
0 8 12 368.327 80.6458 14
0 -8 12 692.795 103.139 20
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-11 -5 -1 737.894 97.7592 18
-11 -5 -1 701.786 109.438 17
-11 5 -1 853.618 117.167 25
-11 -5 -1 666.797 89.8534 24
-11 5 -1 731.178 118.701 24
-11 -5 -2 80.0152 59.9854 17
-11 5 -2 3.18955 50.3464 25
-11 5 -2 11.8311 61.4574 24
-11 -5 -3 54.8897 46.1181 17
-11 5 -3-9.53699 48.7172 24
-11 -5 -4 5367.75 192.188 17
-11 5 -4 5706.88 214.192 24
-11 -6 6-40.2941 32.6612 19
-11 6 5 427.912 61.0254 6
-11 -6 5 427.630 76.0118 19
-11 6 5 368.223 66.2795 7
-11 -6 4 750.438 102.445 19
-11 -6 4 735.884 93.5523 17
-11 6 4 862.739 90.7011 6
-11 -6 3 827.850 106.361 19
-11 6 3 680.776 112.875 17
-11 -6 3 575.072 93.0381 17
-11 6 3 814.118 96.4590 6
-11 -6 2 1724.35 141.003 19
-11 -6 2 1626.96 155.464 18
-11 6 2 1717.31 151.919 17
-11 -6 2 1621.50 152.430 17
-11 6 2 1498.53 147.003 25
-11 6 2 1850.39 163.851 24
-11 6 2 1780.58 139.060 6
-11 -6 1 7686.17 313.315 18
-11 6 1 6962.54 289.785 17
-11 -6 1 7447.42 314.741 17
-11 6 1 7641.01 306.643 25
-11 6 1 7996.30 327.442 24
-11 -6 0 1681.08 149.354 18
-11 -6 0 1380.45 147.570 17
-11 6 0 1471.83 145.247 25
-11 6 0 1291.99 142.435 24
-11 -6 -1 44.4842 49.9103 18
-11 -6 -1 110.966 62.7159 17
-11 6 -1 171.347 82.6345 25
-11 6 -1 136.932 71.2058 24
-11 -6 -2 158.462 62.5241 17
-11 6 -2 117.310 61.7003 25
-11 6 -2 87.8837 65.4816 24
-11 -6 -3 1582.03 122.570 17
-11 6 -3 1475.10 124.360 24
-11 -6 -4 364.007 51.9439 17
-11 6 -4 390.311 57.7578 24
-11 -7 6 730.037 71.1588 19
-11 7 5 64.2992 37.1057 6
-11 -7 5 144.079 45.0073 19
-11 7 4 217.100 56.7621 6
-11 -7 4 253.373 64.9335 19
-11 7 3 567.507 84.5438 6
-11 -7 3 470.072 84.4931 19
-11 -7 3 546.307 85.0610 18
-11 -7 3 627.415 92.6193 17
-11 7 2 40.2132 52.3213 6
-11 -7 2 11.7784 35.3089 19
-11 -7 2 74.5291 55.7679 18
-11 -7 2-38.7273 45.6298 17
-11 7 2 33.5110 57.3955 25
-11 7 2-7.65801 45.1735 24
-11 -7 1 3725.08 176.008 19
-11 -7 1 7028.58 289.729 18
-11 7 1 4579.60 212.271 17
-11 -7 1 6524.46 277.788 17
-11 7 1 7214.57 286.458 25
-11 7 1 6398.12 277.392 24
-11 -7 0 936.996 116.458 18
-11 -7 0 1054.64 124.914 17
-11 7 0 888.698 114.232 25
-11 7 0 827.737 112.266 24
-11 -7 -1 2230.06 147.297 18
-11 -7 -1 2417.66 167.852 17
-11 7 -1 2488.87 169.558 25
-11 7 -1 2490.39 172.703 24
-11 -7 -2 1531.30 129.049 17
-11 7 -2 1606.98 123.811 25
-11 7 -2 1515.02 130.945 24
-11 -7 -3 2611.62 146.881 17
-11 7 -3 2670.25 153.828 24
-11 8 5 427.426 55.4618 6
-11 -8 5 489.027 67.0215 19
-11 8 4 38.7206 38.2290 6
-11 -8 4-18.6345 37.6065 19
-11 -8 3 3152.98 173.037 19
-11 -8 3 3168.00 181.307 18
-11 8 3 3370.51 165.777 6
-11 8 2 354.532 71.1911 6
-11 -8 2 257.780 65.1139 19
-11 -8 2 324.322 75.9216 18
-11 -8 2 307.450 65.6073 17
-11 8 2 334.873 75.1131 25
-11 -8 1 3693.98 202.824 18
-11 -8 1 3456.36 190.593 17
-11 8 1 3786.61 200.857 25
-11 8 1 3481.41 190.640 24
-11 -8 0 502.504 89.3101 18
-11 -8 0 467.148 81.0287 17
-11 8 0 493.376 91.8706 25
-11 8 0 584.566 89.2287 24
-11 -8 -1 1162.61 105.175 18
-11 -8 -1 1232.67 114.784 17
-11 8 -1 1281.19 116.090 25
-11 8 -1 1137.27 112.263 24
-11 -8 -2 2599.79 153.656 17
-11 8 -2 2422.90 140.674 25
-11 8 -2 2337.52 144.306 24
-11 -8 -3 2190.76 126.190 17
-11 8 -3 2288.39 126.465 24
-11 -9 5 26.5175 33.3543 19
-11 -9 4 1530.56 110.866 19
-11 9 4 1543.48 99.5629 6
-11 9 3 37.8758 39.6891 6
-11 -9 3-18.8435 36.7948 19
-11 -9 2 1771.94 120.337 19
-11 -9 2 1785.38 135.966 18
-11 -9 2 1524.33 112.199 17
-11 9 2 1600.64 120.920 25
-11 9 2 1697.34 119.443 6
-11 -9 1 4970.07 220.865 18
-11 -9 1 4416.21 195.307 17
-11 9 1 4422.72 200.598 25
-11 -9 0 963.414 97.7817 18
-11 -9 0 836.722 91.1574 17
-11 9 0 953.495 106.454 25
-11 9 0 666.032 80.7635 24
-11 -9 -1 47.7224 38.9293 18
-11 -9 -1 279.721 59.3148 17
-11 9 -1 196.673 59.5139 25
-11 9 -1 94.5956 42.0213 24
-11 -9 -2 167.350 45.4022 17
-11 9 -2 74.4864 42.8824 25
-11 10 4-44.7345 24.5793 6
-11 -10 4-48.4605 29.2366 19
-11 -10 3 1352.40 100.907 19
-11 10 3 1500.66 101.041 6
-11 -10 2 2918.03 138.700 19
-11 10 2 2658.24 134.027 25
-11 -10 1 49.2082 49.5700 18
-11 10 1 111.454 48.3899 25
-11 -10 0 757.205 84.2806 18
-11 -10 0 579.667 67.8757 17
-11 10 0 734.995 84.4523 25
-11 -10 -1 220.384 48.1671 18
-11 -10 -1 66.2996 33.6492 17
-11 10 -1 154.728 46.5316 25
-11 -11 2 425.484 56.5576 18
-11 -11 1 2347.16 127.225 18
-11 11 1 2289.43 118.260 25
-11 -11 0-60.4830 32.7198 18
-11 11 0 4.49499 32.8567 25
-12 0 3 8.74218 39.8878 17
-12 0 2 108.992 44.2441 17
-12 0 1-0.15615 32.6400 17
-12 0 0 703.932 86.2115 17
-12 0 0 781.198 83.2167 24
-12 0 -1 47.6114 28.4273 24
-12 1 3 134.309 52.3326 17
-12 -1 3 190.426 51.1124 17
-12 1 2 4885.48 209.167 17
-12 -1 2 4572.54 204.964 17
-12 1 1 239.543 60.2441 17
-12 -1 1 359.940 73.2470 17
-12 1 0 203.685 52.2234 17
-12 -1 0 120.806 53.8267 17
-12 1 0 146.586 49.1289 24
-12 1 -1 840.288 81.1506 24
-12 2 3 6102.03 222.991 17
-12 -2 3 6192.61 221.354 17
-12 2 2 2515.04 148.931 17
-12 -2 2 2822.93 161.273 17
-12 2 1 1185.14 102.829 17
-12 -2 1 1334.44 113.305 17
-12 -2 0 56.0741 39.0349 17
-12 2 0 237.599 52.1810 24
-12 -2 -1 976.545 85.7914 17
-12 2 -1 1010.97 88.5574 24
-12 -3 3 3442.25 156.743 17
-12 3 2 69.4917 41.6755 17
-12 -3 2 172.345 52.0394 17
-12 3 1 931.897 86.4393 17
-12 -3 1 845.343 90.8654 17
-12 -3 0 496.685 70.1755 17
-12 3 0 509.527 75.8884 24
-12 3 -1 970.382 84.2483 24
-12 -4 2 370.511 62.0412 17
-12 -4 1 1156.56 97.2497 17
-12 -4 0 48.1573 39.3231 17
-12 4 0 110.945 37.8643 24
0 0 0 0.00 0.00 0
TITL kee11 in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 1.54184 9.704339 20.612803 11.364873 90.0000 95.3008 90.0000
ZERR 8.00 0.000097 0.000204 0.000125 0.0000 0.0010 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O
UNIT 88.00 120.00 8.00 32.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 42939
_shelx_res_file
;
TITL kee11 in P21/c #14
kee11.res
created by SHELXL-2018/3 at 14:33:25 on 24-Oct-2018
REM reset to P21/c #14
CELL 1.54184 9.7043 20.6128 11.3649 90 95.301 90
ZERR 8 0.0001 0.0002 0.0002 0 0.001 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 88 120 8 32
L.S. 10
PLAN 20
TEMP -173
BOND
fmap 2
acta
OMIT 6 21 4
REM
REM
REM
WGHT 0.043600 0.630500
EXTI 0.001431
FVAR 4.77088
O1 4 0.255502 0.436219 0.704942 11.00000 0.03069 0.01841 =
0.01891 -0.00100 0.00734 0.00060
O2 4 0.323036 0.443618 0.522131 11.00000 0.03648 0.01779 =
0.02139 0.00215 0.01112 0.00189
O3 4 0.334587 0.310948 0.516502 11.00000 0.03127 0.01910 =
0.02183 -0.00167 0.00884 0.00182
O5 4 0.262338 0.305293 0.695052 11.00000 0.03723 0.01594 =
0.01960 0.00008 0.00937 0.00087
AFIX 147
H5 2 0.236580 0.331294 0.745548 11.00000 -1.50000
AFIX 0
C11 1 0.297448 0.338071 0.602291 11.00000 0.01853 0.01753 =
0.01740 0.00048 0.00244 0.00037
C15 1 0.290572 0.413317 0.611036 11.00000 0.01772 0.01729 =
0.01807 0.00020 0.00260 0.00079
O4 4 0.188572 0.464513 0.921457 11.00000 0.03937 0.01772 =
0.02258 -0.00311 0.01262 -0.00591
AFIX 147
H4 2 0.195934 0.439668 0.863786 11.00000 -1.50000
AFIX 0
O6 4 0.087010 0.324545 1.071515 11.00000 0.02624 0.01870 =
0.01923 0.00039 0.00631 -0.00150
O7 4 0.151760 0.337436 0.888664 11.00000 0.03835 0.02038 =
0.01894 -0.00243 0.00900 -0.00398
N8 3 0.011871 0.138392 0.778059 11.00000 0.02172 0.02205 =
0.01690 0.00224 0.00410 0.00204
AFIX 43
H8 2 0.048459 0.141529 0.710267 11.00000 -1.20000
AFIX 0
O9 4 0.134642 0.455087 1.106039 11.00000 0.06527 0.02522 =
0.02809 -0.00969 0.02301 -0.01458
N10 3 -0.581394 0.103537 0.824352 11.00000 0.02243 0.02072 =
0.01622 -0.00031 0.00404 -0.00058
AFIX 43
H10 2 -0.618785 0.096784 0.890936 11.00000 -1.20000
AFIX 0
C12 1 -0.029979 0.184122 0.962077 11.00000 0.02231 0.01616 =
0.02026 -0.00059 0.00068 -0.00018
AFIX 43
H12 2 -0.017786 0.219014 1.016658 11.00000 -1.20000
AFIX 0
C13 1 0.127570 0.356744 0.988298 11.00000 0.01813 0.01798 =
0.01788 -0.00111 0.00231 -0.00077
C14 1 -0.117524 0.078778 0.906617 11.00000 0.02197 0.01609 =
0.01895 0.00084 0.00241 -0.00044
AFIX 43
H14 2 -0.167076 0.040537 0.922749 11.00000 -1.20000
AFIX 0
C16 1 -0.437309 0.076921 0.416977 11.00000 0.02733 0.02623 =
0.01708 -0.00352 0.00357 -0.00301
AFIX 137
H16A 2 -0.537903 0.075552 0.398349 11.00000 -1.50000
H16B 2 -0.406152 0.036516 0.456362 11.00000 -1.50000
H16C 2 -0.392251 0.081887 0.343806 11.00000 -1.50000
AFIX 0
C17 1 -0.331342 0.114002 1.073112 11.00000 0.02135 0.03011 =
0.02140 0.00228 0.00378 0.00259
AFIX 137
H17A 2 -0.348024 0.073140 1.030059 11.00000 -1.50000
H17B 2 -0.367429 0.150194 1.023517 11.00000 -1.50000
H17C 2 -0.378245 0.112917 1.145842 11.00000 -1.50000
AFIX 0
C18 1 -0.560684 0.168187 0.654996 11.00000 0.02176 0.01820 =
0.01874 0.00110 0.00222 0.00194
AFIX 43
H18 2 -0.587545 0.205627 0.609813 11.00000 -1.20000
AFIX 0
C19 1 -0.431040 0.069911 0.684623 11.00000 0.02210 0.01652 =
0.01840 -0.00133 0.00210 0.00128
AFIX 43
H19 2 -0.365858 0.039443 0.660399 11.00000 -1.20000
AFIX 0
C20 1 0.026891 0.187480 0.855193 11.00000 0.02086 0.01791 =
0.02296 0.00358 0.00197 -0.00086
AFIX 43
H20 2 0.077167 0.225023 0.836279 11.00000 -1.20000
AFIX 0
C21 1 -0.448181 0.197446 0.436872 11.00000 0.02990 0.02469 =
0.02187 0.00673 0.00719 0.00486
AFIX 137
H21A 2 -0.406218 0.201309 0.361993 11.00000 -1.50000
H21B 2 -0.420537 0.234575 0.487513 11.00000 -1.50000
H21C 2 -0.549192 0.196699 0.421293 11.00000 -1.50000
AFIX 0
C22 1 -0.490706 0.060057 0.788146 11.00000 0.02513 0.01676 =
0.01828 0.00041 0.00166 -0.00026
AFIX 43
H22 2 -0.467953 0.022485 0.834317 11.00000 -1.20000
AFIX 0
C23 1 0.149993 0.430453 1.012137 11.00000 0.02792 0.01959 =
0.02126 -0.00279 0.00864 -0.00481
C24 1 -0.174896 0.123034 1.104376 11.00000 0.02167 0.01831 =
0.01649 0.00064 0.00290 0.00092
C25 1 -0.116697 0.062942 1.171997 11.00000 0.02658 0.02442 =
0.01986 0.00598 0.00263 0.00305
AFIX 137
H25A 2 -0.158292 0.059412 1.247100 11.00000 -1.50000
H25B 2 -0.016064 0.067113 1.187537 11.00000 -1.50000
H25C 2 -0.138637 0.023997 1.124460 11.00000 -1.50000
AFIX 0
C26 1 -0.615750 0.156844 0.760974 11.00000 0.02171 0.02049 =
0.02000 -0.00062 0.00334 0.00262
AFIX 43
H26 2 -0.678645 0.187189 0.789160 11.00000 -1.20000
AFIX 0
C27 1 -0.465460 0.124596 0.614225 11.00000 0.01773 0.01674 =
0.01621 -0.00164 0.00083 -0.00180
C28 1 -0.399120 0.134573 0.499076 11.00000 0.02075 0.01844 =
0.01576 0.00046 0.00310 0.00077
C29 1 -0.105586 0.129261 0.989886 11.00000 0.01748 0.01693 =
0.01658 0.00150 0.00029 0.00239
C30 1 -0.241027 0.136591 0.526765 11.00000 0.02112 0.02430 =
0.02271 0.00128 0.00360 -0.00225
AFIX 137
H30A 2 -0.208251 0.094310 0.557250 11.00000 -1.50000
H30B 2 -0.216597 0.170110 0.586209 11.00000 -1.50000
H30C 2 -0.197493 0.146638 0.454478 11.00000 -1.50000
AFIX 0
C31 1 -0.149534 0.182958 1.182721 11.00000 0.03613 0.02501 =
0.01932 -0.00432 0.00572 0.00032
AFIX 137
H31A 2 -0.186910 0.221388 1.140180 11.00000 -1.50000
H31B 2 -0.049865 0.188524 1.202940 11.00000 -1.50000
H31C 2 -0.195574 0.177365 1.255250 11.00000 -1.50000
AFIX 0
C32 1 -0.058059 0.084306 0.802023 11.00000 0.02400 0.01831 =
0.01895 -0.00108 0.00157 0.00163
AFIX 43
H32 2 -0.066310 0.049822 0.746359 11.00000 -1.20000
AFIX 0
HKLF 4
REM kee11 in P21/c #14
REM wR2 = 0.0858, GooF = S = 1.030, Restrained GooF = 1.030 for all data
REM R1 = 0.0316 for 4309 Fo > 4sig(Fo) and 0.0353 for all 4749 data
REM 298 parameters refined using 0 restraints
END
WGHT 0.0436 0.6305
REM Highest difference peak 0.296, deepest hole -0.195, 1-sigma level 0.038
Q1 1 0.1387 0.3923 1.0040 11.00000 0.05 0.30
Q2 1 0.2934 0.3743 0.6086 11.00000 0.05 0.27
Q3 1 -0.1453 0.1287 1.0400 11.00000 0.05 0.25
Q4 1 -0.1474 0.0959 1.1350 11.00000 0.05 0.25
Q5 1 -0.1598 0.1520 1.1415 11.00000 0.05 0.24
Q6 1 -0.4161 0.1085 0.4554 11.00000 0.05 0.24
Q7 1 -0.4290 0.1322 0.5559 11.00000 0.05 0.23
Q8 1 -0.4368 0.1029 0.6618 11.00000 0.05 0.23
Q9 1 -0.3258 0.1335 0.5077 11.00000 0.05 0.22
Q10 1 -0.4989 0.1488 0.6383 11.00000 0.05 0.22
Q11 1 -0.4236 0.1631 0.4659 11.00000 0.05 0.22
Q12 1 -0.0803 0.1603 0.9689 11.00000 0.05 0.20
Q13 1 -0.0935 0.1000 0.9520 11.00000 0.05 0.20
Q14 1 -0.2493 0.1193 1.0883 11.00000 0.05 0.19
Q15 1 -0.1238 0.1074 0.9398 11.00000 0.05 0.19
Q16 1 -0.5670 0.1654 0.7195 11.00000 0.05 0.17
Q17 1 -0.5467 0.0787 0.7996 11.00000 0.05 0.17
Q18 1 -0.0206 0.1879 0.8956 11.00000 0.05 0.17
Q19 1 -0.0717 0.0805 0.8640 11.00000 0.05 0.15
Q20 1 -0.4557 0.0694 0.7404 11.00000 0.05 0.15
;
_shelx_res_checksum 94961
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'
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
O O1 0.25550(8) 0.43622(3) 0.70494(6) 0.02235(17) Uani d 1
O O2 0.32304(8) 0.44362(4) 0.52213(7) 0.02470(17) Uani d 1
O O3 0.33459(8) 0.31095(4) 0.51650(7) 0.02367(17) Uani d 1
O O5 0.26234(8) 0.30529(3) 0.69505(6) 0.02384(17) Uani d 1
H H5 0.236580 0.331294 0.745548 0.036 Uiso calc 1
C C11 0.29745(10) 0.33807(5) 0.60229(9) 0.0178(2) Uani d 1
C C15 0.29057(10) 0.41332(5) 0.61104(9) 0.0176(2) Uani d 1
O O4 0.18857(9) 0.46451(4) 0.92146(7) 0.02595(18) Uani d 1
H H4 0.195934 0.439668 0.863786 0.039 Uiso calc 1
O O6 0.08701(8) 0.32454(3) 1.07151(6) 0.02113(16) Uani d 1
O O7 0.15176(9) 0.33744(4) 0.88866(7) 0.02549(18) Uani d 1
N N8 0.01187(9) 0.13839(4) 0.77806(8) 0.02008(18) Uani d 1
H H8 0.048459 0.141529 0.710267 0.024 Uiso calc 1
O O9 0.13464(11) 0.45509(4) 1.10604(8) 0.0384(2) Uani d 1
N N10 -0.58139(9) 0.10354(4) 0.82435(8) 0.01965(18) Uani d 1
H H10 -0.618785 0.096784 0.890936 0.024 Uiso calc 1
C C12 -0.02998(10) 0.18412(5) 0.96208(9) 0.0197(2) Uani d 1
H H12 -0.017786 0.219014 1.016658 0.024 Uiso calc 1
C C13 0.12757(10) 0.35674(5) 0.98830(9) 0.0180(2) Uani d 1
C C14 -0.11752(10) 0.07878(5) 0.90662(9) 0.0190(2) Uani d 1
H H14 -0.167076 0.040537 0.922749 0.023 Uiso calc 1
C C16 -0.43731(11) 0.07692(5) 0.41698(9) 0.0235(2) Uani d 1
H H16A -0.537903 0.075552 0.398349 0.035 Uiso calc 1
H H16B -0.406152 0.036516 0.456362 0.035 Uiso calc 1
H H16C -0.392251 0.081887 0.343806 0.035 Uiso calc 1
C C17 -0.33134(11) 0.11400(6) 1.07311(10) 0.0242(2) Uani d 1
H H17A -0.348024 0.073140 1.030059 0.036 Uiso calc 1
H H17B -0.367429 0.150194 1.023517 0.036 Uiso calc 1
H H17C -0.378245 0.112917 1.145842 0.036 Uiso calc 1
C C18 -0.56068(10) 0.16819(5) 0.65500(9) 0.0195(2) Uani d 1
H H18 -0.587545 0.205627 0.609813 0.023 Uiso calc 1
C C19 -0.43104(10) 0.06991(5) 0.68462(9) 0.0190(2) Uani d 1
H H19 -0.365858 0.039443 0.660399 0.023 Uiso calc 1
C C20 0.02689(11) 0.18748(5) 0.85519(9) 0.0206(2) Uani d 1
H H20 0.077167 0.225023 0.836279 0.025 Uiso calc 1
C C21 -0.44818(12) 0.19745(5) 0.43687(10) 0.0252(2) Uani d 1
H H21A -0.406218 0.201309 0.361993 0.038 Uiso calc 1
H H21B -0.420537 0.234575 0.487513 0.038 Uiso calc 1
H H21C -0.549192 0.196699 0.421293 0.038 Uiso calc 1
C C22 -0.49071(11) 0.06006(5) 0.78815(9) 0.0201(2) Uani d 1
H H22 -0.467953 0.022485 0.834317 0.024 Uiso calc 1
C C23 0.14999(11) 0.43045(5) 1.01214(9) 0.0225(2) Uani d 1
C C24 -0.17490(11) 0.12303(5) 1.10438(9) 0.0188(2) Uani d 1
C C25 -0.11670(11) 0.06294(5) 1.17200(9) 0.0236(2) Uani d 1
H H25A -0.158292 0.059412 1.247100 0.035 Uiso calc 1
H H25B -0.016064 0.067113 1.187537 0.035 Uiso calc 1
H H25C -0.138637 0.023997 1.124460 0.035 Uiso calc 1
C C26 -0.61575(10) 0.15684(5) 0.76097(9) 0.0206(2) Uani d 1
H H26 -0.678645 0.187189 0.789160 0.025 Uiso calc 1
C C27 -0.46546(10) 0.12460(5) 0.61422(9) 0.0169(2) Uani d 1
C C28 -0.39912(10) 0.13457(5) 0.49908(9) 0.0182(2) Uani d 1
C C29 -0.10559(10) 0.12926(5) 0.98989(9) 0.0171(2) Uani d 1
C C30 -0.24103(11) 0.13659(5) 0.52676(10) 0.0226(2) Uani d 1
H H30A -0.208251 0.094310 0.557250 0.034 Uiso calc 1
H H30B -0.216597 0.170110 0.586209 0.034 Uiso calc 1
H H30C -0.197493 0.146638 0.454478 0.034 Uiso calc 1
C C31 -0.14953(13) 0.18296(5) 1.18272(10) 0.0266(2) Uani d 1
H H31A -0.186910 0.221388 1.140180 0.040 Uiso calc 1
H H31B -0.049865 0.188524 1.202940 0.040 Uiso calc 1
H H31C -0.195574 0.177365 1.255250 0.040 Uiso calc 1
C C32 -0.05806(11) 0.08431(5) 0.80202(9) 0.0204(2) Uani d 1
H H32 -0.066310 0.049822 0.746359 0.025 Uiso calc 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
O1 0.0307(4) 0.0184(3) 0.0189(4) 0.0006(3) 0.0073(3) -0.0010(3)
O2 0.0365(4) 0.0178(4) 0.0214(4) 0.0019(3) 0.0111(3) 0.0021(3)
O3 0.0313(4) 0.0191(4) 0.0218(4) 0.0018(3) 0.0088(3) -0.0017(3)
O5 0.0372(4) 0.0159(3) 0.0196(4) 0.0009(3) 0.0094(3) 0.0001(3)
C11 0.0185(4) 0.0175(5) 0.0174(5) 0.0004(3) 0.0024(4) 0.0005(4)
C15 0.0177(4) 0.0173(5) 0.0181(5) 0.0008(3) 0.0026(4) 0.0002(4)
O4 0.0394(4) 0.0177(4) 0.0226(4) -0.0059(3) 0.0126(3) -0.0031(3)
O6 0.0262(4) 0.0187(3) 0.0192(4) -0.0015(3) 0.0063(3) 0.0004(3)
O7 0.0383(4) 0.0204(4) 0.0189(4) -0.0040(3) 0.0090(3) -0.0024(3)
N8 0.0217(4) 0.0220(4) 0.0169(4) 0.0020(3) 0.0041(3) 0.0022(3)
O9 0.0653(6) 0.0252(4) 0.0281(4) -0.0146(4) 0.0230(4) -0.0097(3)
N10 0.0224(4) 0.0207(4) 0.0162(4) -0.0006(3) 0.0040(3) -0.0003(3)
C12 0.0223(5) 0.0162(4) 0.0203(5) -0.0002(4) 0.0007(4) -0.0006(4)
C13 0.0181(4) 0.0180(5) 0.0179(5) -0.0008(3) 0.0023(4) -0.0011(4)
C14 0.0220(5) 0.0161(4) 0.0189(5) -0.0004(4) 0.0024(4) 0.0008(4)
C16 0.0273(5) 0.0262(5) 0.0171(5) -0.0030(4) 0.0036(4) -0.0035(4)
C17 0.0213(5) 0.0301(5) 0.0214(5) 0.0026(4) 0.0038(4) 0.0023(4)
C18 0.0218(5) 0.0182(5) 0.0187(5) 0.0019(4) 0.0022(4) 0.0011(4)
C19 0.0221(5) 0.0165(4) 0.0184(5) 0.0013(4) 0.0021(4) -0.0013(4)
C20 0.0209(5) 0.0179(5) 0.0230(5) -0.0009(4) 0.0020(4) 0.0036(4)
C21 0.0299(6) 0.0247(5) 0.0219(5) 0.0049(4) 0.0072(4) 0.0067(4)
C22 0.0251(5) 0.0168(5) 0.0183(5) -0.0003(4) 0.0017(4) 0.0004(4)
C23 0.0279(5) 0.0196(5) 0.0213(5) -0.0048(4) 0.0086(4) -0.0028(4)
C24 0.0217(5) 0.0183(5) 0.0165(5) 0.0009(4) 0.0029(4) 0.0006(4)
C25 0.0266(5) 0.0244(5) 0.0199(5) 0.0030(4) 0.0026(4) 0.0060(4)
C26 0.0217(5) 0.0205(5) 0.0200(5) 0.0026(4) 0.0033(4) -0.0006(4)
C27 0.0177(4) 0.0167(4) 0.0162(4) -0.0018(3) 0.0008(4) -0.0016(3)
C28 0.0207(5) 0.0184(5) 0.0158(4) 0.0008(4) 0.0031(4) 0.0005(4)
C29 0.0175(4) 0.0169(4) 0.0166(5) 0.0024(3) 0.0003(4) 0.0015(4)
C30 0.0211(5) 0.0243(5) 0.0227(5) -0.0023(4) 0.0036(4) 0.0013(4)
C31 0.0361(6) 0.0250(5) 0.0193(5) 0.0003(4) 0.0057(4) -0.0043(4)
C32 0.0240(5) 0.0183(5) 0.0189(5) 0.0016(4) 0.0016(4) -0.0011(4)
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
-1 3 -7 0.0874
-3 11 -2 0.0929
-6 2 3 0.0836
0 -5 7 0.0987
5 -9 1 0.0508
2 8 -6 0.0970
3 9 -4 0.1120
-2 4 7 0.0973
-6 1 2 0.0800
-2 2 7 0.0946
-6 -4 1 0.0767
-2 13 1 0.0927
2 -12 2 0.0574
4 9 0 0.1287
2 -13 -1 0.0783
3 5 5 0.1002
2 7 6 0.0974
-3 -5 -5 0.1099
3 2 6 0.0830
6 -6 -1 0.0718
-6 5 -1 0.0934
-2 -1 -7 0.0911
-3 0 -6 0.0939
-2 13 0 0.0878
-6 -3 3 0.0905
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O3 C11 O5 121.67(9)
O3 C11 C15 122.06(9)
O5 C11 C15 116.26(8)
O1 C15 O2 127.77(9)
O1 C15 C11 116.76(9)
O2 C15 C11 115.47(8)
C20 N8 C32 121.35(9)
C26 N10 C22 121.26(9)
C20 C12 C29 119.95(9)
O6 C13 C23 115.87(9)
O7 C13 O6 128.26(9)
O7 C13 C23 115.88(9)
C32 C14 C29 120.45(9)
C26 C18 C27 120.05(9)
C22 C19 C27 120.64(9)
N8 C20 C12 120.67(9)
N10 C22 C19 120.16(9)
O4 C23 C13 115.21(9)
O9 C23 O4 122.11(10)
O9 C23 C13 122.68(10)
C25 C24 C17 109.09(8)
C29 C24 C17 108.48(8)
C29 C24 C25 108.90(8)
C29 C24 C31 111.65(8)
C31 C24 C17 109.55(9)
C31 C24 C25 109.13(9)
N10 C26 C18 120.70(9)
C18 C27 C19 117.17(9)
C18 C27 C28 122.83(9)
C19 C27 C28 120.00(9)
C16 C28 C30 109.00(8)
C21 C28 C16 109.11(8)
C21 C28 C30 109.47(8)
C27 C28 C16 108.66(8)
C27 C28 C21 111.87(8)
C27 C28 C30 108.68(8)
C12 C29 C14 117.31(9)
C12 C29 C24 122.86(9)
C14 C29 C24 119.83(9)
N8 C32 C14 120.26(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C15 1.2429(12)
O2 C15 1.2526(12)
O3 C11 1.2075(12)
O5 C11 1.3230(12)
C11 C15 1.5560(13)
O4 C23 1.3291(13)
O6 C13 1.2485(12)
O7 C13 1.2429(12)
N8 C20 1.3379(14)
N8 C32 1.3460(14)
O9 C23 1.2035(13)
N10 C22 1.3469(13)
N10 C26 1.3390(14)
C12 C20 1.3816(15)
C12 C29 1.3999(14)
C13 C23 1.5551(14)
C14 C29 1.4041(14)
C14 C32 1.3732(14)
C16 C28 1.5350(14)
C17 C24 1.5382(14)
C18 C26 1.3820(14)
C18 C27 1.3982(14)
C19 C22 1.3735(14)
C19 C27 1.4046(14)
C21 C28 1.5310(14)
C24 C25 1.5374(14)
C24 C29 1.5243(13)
C24 C31 1.5293(14)
C27 C28 1.5248(13)
C28 C30 1.5379(14)
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
O5 H5 O1 . 0.840 2.223 2.702(2) 116.33 yes
O5 H5 O7 . 0.840 1.894 2.621(2) 144.08 yes
O4 H4 O1 . 0.840 1.947 2.667(2) 143.10 yes
O4 H4 O7 . 0.840 2.174 2.665(2) 117.22 yes
N8 H8 O6 4_565 0.880 1.796 2.635(2) 158.60 yes
N10 H10 O2 4_466 0.880 1.842 2.691(2) 161.70 yes
C12 H12 O6 . 0.950 2.457 3.310(2) 149.27 .
C14 H14 O2 2_546 0.950 2.617 3.563(2) 173.62 .
C18 H18 O3 1_455 0.950 2.502 3.446(2) 172.30 .
C19 H19 O4 2_546 0.950 2.551 3.498(2) 174.59 .
C20 H20 O7 . 0.950 2.484 3.329(2) 148.23 .
C22 H22 O2 2_546 0.950 2.619 3.523(2) 159.10 .
C26 H26 O3 4_466 0.950 2.575 3.060(2) 111.97 .
C32 H32 O9 4_565 0.950 2.633 3.144(2) 114.24 .
_cod_database_fobs_code 2242744