#------------------------------------------------------------------------------
#$Date: 2024-08-07 01:04:33 +0300 (Wed, 07 Aug 2024) $
#$Revision: 293990 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023174.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_2023174
loop_
_publ_author_name
'Seidel, Rüdiger W'
'Kolev, Tsonko M.'
_publ_section_title
;
Crystal structure of 1,2,3,4-tetra-hydro-isoquinolin-2-ium
(2S,3S)-3-carb-oxy-2,3-di-hydroxy-propano-ate monohydrate.
;
_journal_coeditor_code TX2087
_journal_issue 'Pt 7'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 763
_journal_page_last 766
_journal_paper_doi 10.1107/S2056989024005711
_journal_volume 80
_journal_year 2024
_chemical_absolute_configuration syn
_chemical_formula_iupac 'C9 H12 N +, C4 H5 O6 -, H2 O'
_chemical_formula_moiety 'C9 H12 N +, C4 H5 O6 -, H2 O'
_chemical_formula_sum 'C13 H19 N O7'
_chemical_formula_weight 301.29
_chemical_name_common
;
1,2,3,4-Tetrahydroisoquinolinium D-hydrogen tartrate monohydrate
;
_chemical_name_systematic
;
1,2,3,4-Tetrahydroisoquinolin-2-ium
(2S,3S)-3-carboxy-2,3-dihydroxypropanoate monohydrate
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2019/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.0695(3)
_cell_length_b 7.4842(3)
_cell_length_c 26.9573(10)
_cell_measurement_reflns_used 5780
_cell_measurement_temperature 115(2)
_cell_measurement_theta_max 27.7030
_cell_measurement_theta_min 3.0140
_cell_volume 1426.30(10)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlis system (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2018)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2019/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 115(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur2'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0381
_diffrn_reflns_av_unetI/netI 0.0342
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 35
_diffrn_reflns_limit_l_min -35
_diffrn_reflns_number 16488
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.463
_diffrn_reflns_theta_min 2.825
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.115
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.96657
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(ABSPACK in CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.403
_exptl_crystal_description prism
_exptl_crystal_F_000 640
_exptl_crystal_size_max 0.490
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_min 0.200
_refine_diff_density_max 0.248
_refine_diff_density_min -0.193
_refine_ls_abs_structure_details
;
The absolute structure was inferred from the known absolute configuration
of the starting material.
;
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 218
_refine_ls_number_reflns 3307
_refine_ls_number_restraints 7
_refine_ls_restrained_S_all 1.037
_refine_ls_R_factor_all 0.0473
_refine_ls_R_factor_gt 0.0367
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+0.2898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0734
_refine_ls_wR_factor_ref 0.0776
_reflns_number_gt 2900
_reflns_number_total 3307
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file tx2087.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2023174.cif.'
_cod_database_code 2023174
_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_estimated_absorpt_t_min 0.946
_shelx_estimated_absorpt_t_max 0.977
_shelx_hkl_file
;
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0 0 -6 13222.6 158.569 2
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0 0 6 13603.0 160.581 8
0 0 6 13491.5 161.921 5
0 0 -7 49.2766 10.8707 3
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0 0 -7 21.2662 22.4934 2
0 0 7-5.28181 18.9190 8
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-8 1 8 66.0598 54.0990 1
8 1 -8 132.281 59.9511 8
8 -1 8 48.7711 60.4180 8
-8 1 7 256.305 74.4083 1
8 1 -7 231.516 70.1707 8
8 -1 7 296.829 75.5439 8
-8 1 6 173.198 63.8310 1
8 1 -6 210.327 69.2455 8
8 -1 6 225.921 67.0211 8
-8 1 5 235.321 77.1894 1
8 1 -5 212.227 67.3956 8
8 -1 5 297.220 72.2618 8
-8 1 4 580.450 99.0643 1
8 1 -4 457.613 92.1094 8
8 -1 4 626.938 90.9023 8
8 1 -3 29.8580 48.0554 8
8 -1 3 46.6041 47.9477 8
-8 1 2 318.953 76.0699 1
8 -1 2 318.138 72.9029 8
8 1 -2 456.139 87.2980 8
-8 1 1 15.7495 54.1151 1
8 -1 1 34.0584 54.4440 8
8 1 -1-32.6535 51.1959 8
-8 1 0 535.838 94.4724 1
8 -1 0 429.653 82.1026 8
8 1 0 454.026 80.9659 8
-8 1 -1 26.7733 55.5475 1
8 1 1 47.2534 51.2397 8
8 -1 -1 82.3394 58.7871 8
-8 1 -2 349.917 81.1747 1
8 1 2 418.829 79.2478 8
-8 1 -3 100.145 61.2218 1
8 1 3 160.259 59.8645 8
-8 -1 4 635.973 95.1482 1
-8 1 -4 320.715 81.5413 1
8 1 4 557.682 88.8758 8
-8 -1 5 166.349 65.2936 1
8 1 5 119.731 54.8967 8
-8 1 -6 406.894 88.6610 1
-8 -1 6 294.510 79.2593 1
8 1 6 161.028 62.9865 8
-8 1 -7 160.970 65.4000 1
-8 -1 7 184.427 61.3257 1
8 1 7 132.411 68.1748 8
-8 -1 8 66.3740 60.5195 1
8 1 8 103.534 61.7595 8
-8 -1 9 174.955 64.8856 1
-8 1 -9 84.7415 63.7791 1
8 1 9 204.830 77.0643 8
-8 -1 10 66.9381 52.3294 1
-8 1 -10 83.1085 65.8972 1
8 1 10 22.2035 54.6547 8
-8 1 -11 518.136 98.3032 1
-8 -1 11 466.295 87.3335 1
8 1 11 565.552 97.6711 8
-8 1 -12 36.2357 58.4228 1
-8 -1 12-24.7682 49.1243 1
8 1 12-17.2513 58.3419 8
-8 1 -13 252.298 72.8563 1
-8 -1 13 477.187 93.3603 1
8 1 13 481.722 92.7379 8
-8 1 -14-114.266 86.2357 1
-8 -1 14 15.8083 64.2624 1
8 1 14 84.5654 67.6008 8
-8 -1 15 110.919 59.4687 1
-8 -1 16 62.1467 59.4019 1
8 -2 16 239.082 69.9544 8
8 -2 15 79.9808 72.0547 8
8 -2 14 45.4102 62.4393 8
-8 -2 -14-60.0211 58.4153 5
8 -2 13 207.358 77.9447 8
-8 -2 -13 14.7316 53.8518 5
-8 2 12 715.025 118.367 1
8 -2 12 709.497 106.899 8
-8 -2 -12 982.987 118.287 5
-8 2 11 275.202 82.5165 1
8 -2 11 249.799 72.8824 8
-8 -2 -11 258.782 70.4469 5
-8 2 10 1526.97 156.023 1
8 -2 10 1600.93 145.588 8
8 2 -10 1319.97 137.863 8
-8 -2 -10 1482.82 144.848 5
-8 2 9 64.7478 65.7694 1
8 2 -9 107.566 57.3975 8
8 -2 9 21.3411 58.0245 8
-8 -2 -9 23.0707 58.8878 5
-8 2 8 39.7578 62.1737 1
8 2 -8 33.2248 56.1580 8
8 -2 8 60.6899 54.1945 8
-8 -2 -8 145.463 65.6610 5
-8 2 7 144.750 67.6682 1
8 2 -7 205.926 73.8042 8
8 -2 7 141.668 69.6126 8
-8 -2 -7 141.040 55.3476 5
-8 2 6 309.201 80.8686 1
8 2 -6 146.252 63.5762 8
-8 -2 -6 152.454 64.6715 5
-8 2 5 49.3151 57.7315 1
8 2 -5 226.557 74.3659 8
-8 -2 -5 144.970 65.8869 5
-8 2 4 97.6058 65.7889 1
8 2 -4 51.0516 57.2920 8
-8 -2 -4 64.7666 50.4211 5
-8 2 3 55.4052 65.9544 1
8 2 -3 151.709 62.6206 8
-8 -2 -3 63.3252 55.4879 5
-8 2 2 74.6260 65.5155 1
8 2 -2 152.877 63.5319 8
-8 -2 -2 66.6794 62.1063 5
-8 2 1 980.153 124.586 1
8 2 -1 786.597 114.638 8
-8 -2 -1 872.729 106.676 5
-8 2 0 76.4087 63.8975 1
8 2 0 18.6672 50.0235 8
-8 -2 0 23.7921 52.1282 5
-8 2 -1 958.367 123.175 1
8 2 1 918.062 113.097 8
-8 -2 1 1017.44 118.862 5
-8 2 -2 65.9679 66.5593 1
8 2 2 141.333 63.8476 8
-8 -2 2 51.3647 57.8497 5
-8 2 -3 135.507 71.8610 1
8 2 3 41.6812 60.1176 8
-8 -2 3 105.235 64.8384 5
8 2 4 14.9748 54.5590 8
-8 -2 4 62.5521 51.4947 5
-8 2 -5 131.982 64.6071 1
8 2 5 142.853 64.7139 8
-8 -2 5 108.380 61.3585 5
-8 2 -6 54.5342 61.7906 1
8 2 6 190.945 68.4388 8
-8 -2 6 200.839 68.1223 5
-8 2 -7 53.4117 61.3867 1
8 2 7 81.1037 64.4519 8
-8 -2 7 46.8549 56.1594 5
-8 2 -8 141.001 78.4395 1
8 2 8 143.634 58.9939 8
-8 -2 8 128.907 63.2419 5
-8 2 -9 134.044 73.3557 1
8 2 9 60.6359 48.5302 8
-8 -2 9 100.669 65.3929 5
-8 2 -10 1212.20 139.966 1
8 2 10 1494.53 153.003 8
-8 -2 10 1594.91 155.122 5
-8 2 -11 284.253 80.4904 1
8 2 11 353.493 88.1636 8
-8 -2 11 483.432 101.717 5
-8 2 -12 739.395 116.740 1
8 2 12 1018.01 129.452 8
-8 -2 12 807.135 117.658 5
-8 2 -13 124.376 77.7488 1
-8 -2 13 89.2252 63.2373 5
-8 2 -14 157.486 84.6456 1
-8 -2 14-33.0866 71.0691 5
-8 2 -15-44.7345 80.1379 1
-8 -2 15 175.694 92.0825 5
-8 -2 17 405.543 91.0502 1
8 -3 14 409.283 78.5830 4
8 -3 13-12.1079 64.1743 4
-8 -3 -13-29.4277 71.0472 5
8 -3 12 133.858 64.0633 4
-8 -3 -12 314.255 90.9659 5
8 -3 11 46.5213 48.7690 4
-8 -3 -11-72.9076 65.5601 5
8 -3 10 114.675 59.7463 4
-8 -3 -10 367.382 88.2948 5
8 -3 9 31.1511 52.4905 4
8 3 -9 148.223 72.2071 8
8 -3 8 139.337 54.3195 4
-8 3 8 211.482 71.3914 1
8 3 -8 310.971 83.4403 8
-8 -3 -8 398.709 91.5481 5
8 -3 7 45.7482 48.4467 4
-8 3 7-52.7510 80.0221 1
8 3 -7 106.701 61.8001 8
-8 -3 -7 63.8603 65.8787 5
8 -3 6 400.254 85.4857 4
-8 3 6 343.942 91.5070 1
8 3 -6 472.876 98.0959 8
-8 -3 -6 527.354 94.9435 5
8 -3 5 952.559 115.953 4
-8 3 5 1216.21 145.155 1
8 3 -5 939.107 121.038 8
-8 -3 -5 1085.48 128.554 5
8 -3 4 84.2350 57.9193 4
-8 3 4 35.0509 67.3482 1
8 3 -4 73.0306 61.3683 8
-8 -3 -4 111.754 59.8507 5
8 -3 3 230.790 73.6916 4
-8 3 3 336.849 91.3045 1
8 3 -3 300.158 83.0234 8
-8 -3 -3 243.728 74.9881 5
8 -3 2 46.0049 57.2976 4
-8 3 2 115.944 66.0154 1
8 3 -2-23.8158 56.3195 8
-8 -3 -2-80.1094 67.9278 5
8 -3 1 1012.55 117.716 4
-8 3 1 1038.60 131.602 1
8 3 -1 794.076 114.853 8
-8 -3 -1 1042.02 124.363 5
8 -3 0 38.7461 51.6070 4
-8 3 0 38.7355 62.8166 1
8 3 0-40.2926 54.8865 8
-8 -3 0-8.44833 58.9325 5
8 -3 -1 831.797 109.108 4
-8 3 -1 837.429 117.457 1
8 3 1 843.805 116.202 8
-8 -3 1 993.879 121.670 5
8 -3 -2 22.6364 55.6575 4
-8 3 -2-141.728 77.2212 1
8 3 2-17.8527 61.2723 8
-8 -3 2-82.6221 71.2981 5
8 -3 -3 153.159 57.2234 4
-8 3 -3 372.075 92.8584 1
8 3 3 295.768 86.4808 8
-8 -3 3 196.562 67.8099 5
8 -3 -4 83.8740 54.2526 4
-8 3 -4 116.076 77.0319 1
8 3 4 44.0121 56.1000 8
-8 -3 4 13.4975 64.5167 5
8 -3 -5 1180.80 128.835 4
-8 3 -5 988.364 135.452 1
8 3 5 1117.83 131.152 8
-8 -3 5 1140.60 133.724 5
8 -3 -6 266.411 65.8214 4
-8 3 -6 501.954 99.0508 1
8 3 6 564.027 107.328 8
-8 -3 6 459.419 92.4700 5
8 -3 -7-6.65861 47.3255 4
-8 3 -7 105.644 65.8678 1
8 3 7 119.758 76.8623 8
-8 -3 7-86.4271 80.4096 5
8 -3 -8 314.080 77.9550 4
-8 3 -8 142.469 76.5311 1
8 3 8 312.319 84.9497 8
-8 -3 8 415.004 93.6373 5
8 -3 -9-27.9904 51.6725 4
-8 3 -9-6.22038 77.9607 1
8 3 9 167.594 70.5261 8
-8 -3 9 74.9238 80.9996 5
8 -3 -10 554.433 99.1404 4
-8 3 -10 367.124 99.9966 1
8 3 10 487.419 98.5393 8
-8 -3 10 247.388 87.9006 5
-8 3 -11 176.557 85.8677 1
8 -3 -11 127.707 77.1205 4
-8 -3 11 62.9250 64.6611 5
8 -3 -12 164.280 67.5384 4
8 -3 -13 42.0311 51.8045 4
8 -3 -14 257.167 73.6265 4
8 -4 8-21.7444 57.4223 4
8 -4 7 249.229 67.5925 4
8 -4 6 529.786 99.4376 4
-8 -4 -6 338.135 92.3118 5
8 -4 5 590.186 100.941 4
-8 -4 -5 693.586 121.628 5
8 -4 4 24.6953 54.7532 4
-8 -4 -4 73.5914 68.6223 5
8 -4 3 761.705 114.377 4
8 4 -3 745.974 119.007 8
-8 -4 -3 485.497 106.679 5
8 -4 2 515.179 99.3326 4
8 4 -2 379.365 89.3032 8
-8 -4 -2 563.595 102.791 5
8 -4 1 51.2444 49.7517 4
8 4 -1 122.455 64.2614 8
-8 -4 -1 3.57424 59.1091 5
8 -4 0 455.249 92.8539 4
8 4 0 394.933 94.7756 8
-8 -4 0 428.454 97.5182 5
8 -4 -1 33.7494 60.5628 4
8 4 1 21.8052 60.9740 8
-8 -4 1 30.8740 64.6656 5
8 -4 -2 543.102 105.444 4
8 4 2 406.563 93.1993 8
-8 -4 2 614.279 109.589 5
8 -4 -3 712.079 116.708 4
8 4 3 636.373 109.010 8
-8 -4 3 613.236 110.951 5
8 -4 -4 64.3960 57.6057 4
-8 -4 4 171.175 78.1225 5
8 -4 -5 637.999 105.252 4
-8 -4 5 549.873 103.799 5
8 -4 -6 495.918 99.8232 4
8 -4 -7 222.559 79.7957 4
8 -4 -8 141.282 60.6299 4
9 0 0-52.1858 70.2995 8
9 0 1 249.371 59.3793 8
9 0 -1 241.514 74.6793 8
-9 0 2 64.5318 62.2132 1
9 0 -2 88.8790 51.5321 8
9 0 2 218.161 73.7720 8
-9 0 3 103.579 71.3566 1
9 0 -3 236.291 75.7742 8
9 0 3 158.006 69.7843 8
-9 0 4 118.736 72.7402 1
9 0 4-30.9298 73.3577 8
-9 0 5 252.725 84.4580 1
9 0 5 78.2713 69.4325 8
-9 0 6 970.728 117.870 1
9 0 6 1361.41 145.804 8
-9 0 7 67.6148 52.5638 1
9 0 7-33.5005 74.7084 8
-9 0 8-16.3880 64.9335 1
9 1 -10 275.948 81.1160 8
9 1 -9-109.381 62.3035 8
9 -1 9-16.8934 66.4608 8
9 1 -8 534.615 110.020 8
9 -1 8 264.608 74.4571 8
9 1 -7 186.812 77.1432 8
9 -1 7 173.908 71.0879 8
9 1 -6 777.980 110.904 8
9 -1 6 597.569 98.7847 8
9 1 -5 298.099 83.3495 8
9 -1 5 181.634 72.7569 8
-9 1 4 849.334 123.290 1
9 1 -4 795.906 114.503 8
9 -1 4 760.892 113.198 8
-9 1 3 221.984 80.2333 1
9 1 -3 345.719 84.8451 8
-9 1 2 51.3040 67.2729 1
9 1 -2 323.735 93.0760 8
-9 1 1-36.0914 64.3790 1
9 1 -1 114.810 63.3266 8
-9 1 0 112.091 61.6038 1
9 1 0 125.239 67.1374 8
-9 1 -1-14.8111 62.3321 1
9 1 1 135.862 71.6481 8
-9 1 -2 114.284 75.9101 1
9 1 2 114.093 72.4519 8
-9 1 -3 230.943 82.0500 1
9 1 3 314.581 88.5394 8
-9 1 -4 486.375 102.212 1
9 1 4 616.914 109.497 8
-9 1 -5 260.736 98.1799 1
-9 1 -6 455.578 101.260 1
-9 1 -7 88.8127 71.0293 1
0 0 0 0.00 0.00 0
TITL exp_471 in P2(1)2(1)2(1)
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 0.71073 7.069546 7.484249 26.957350 90.0000 90.0000 90.0000
ZERR 4.00 0.000287 0.000336 0.000996 0.0000 0.0000 0.0000
LATT -1
SYMM -x+1/2,-y, z+1/2
SYMM -x, y+1/2,-z+1/2
SYMM x+1/2,-y+1/2,-z
SFAC C H N O
UNIT 52.00 76.00 4.00 28.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 26216
_shelx_res_file
;
TITL exp_471 in P2(1)2(1)2(1)
exp_471.res
created by SHELXL-2019/3 at 15:07:28 on 30-May-2024
CELL 0.71073 7.0695 7.4842 26.9573 90.000 90.000 90.000
ZERR 4.00 0.0003 0.0003 0.0010 0.000 0.000 0.000
LATT -1
SYMM 1/2 - X, - Y, 1/2 + Z
SYMM - X, 1/2 + Y, 1/2 - Z
SYMM 1/2 + X, 1/2 - Y, - Z
SFAC C H N O
UNIT 52 76 4 28
MERG 2
OMIT 0 0 4
OMIT 1 0 1
OMIT 0 1 3
DFIX 0.88 0.02 N2 H2A N2 H2B
DFIX 0.84 0.02 O3 H3 O4 H4 O5 H5A O7 H7A O7 H7B
FMAP 2
PLAN 20
SIZE 0.200 0.210 0.490
ACTA
CONF
BOND $H
EQIV $1 x, y-1, z
HTAB C1 O2_$1
EQIV $2 x-1, y-1, z
HTAB C3 O1_$2
HTAB N2 O7
EQIV $3 x-1/2, -y+1/2, -z+1
HTAB N2 O6_$3
HTAB N2 O5
HTAB O3 O1
EQIV $4 x+1/2, -y+3/2, -z+1
HTAB O3 O4_$4
HTAB O4 O2_$4
HTAB O5 O1_$1
HTAB O7 O2
EQIV $5 x-1, y, z
HTAB O7 O3_$5
L.S. 10
TEMP -158.00
WGHT 0.032600 0.289800
FVAR 2.24704
C1 1 0.418904 0.169393 0.341419 11.00000 0.01932 0.03311 =
0.01923 0.00045 -0.00186 0.00448
AFIX 23
H1A 2 0.464782 0.045500 0.345983 11.00000 -1.20000
H1B 2 0.528981 0.250520 0.344259 11.00000 -1.20000
AFIX 0
C3 1 0.094601 0.124265 0.372835 11.00000 0.02437 0.04043 =
0.02079 0.00469 0.00042 -0.01005
AFIX 23
H3A 2 0.011223 0.144808 0.401784 11.00000 -1.20000
H3B 2 0.112372 -0.006161 0.368861 11.00000 -1.20000
AFIX 0
C4 1 0.004497 0.201595 0.326465 11.00000 0.01969 0.03950 =
0.02184 0.00092 -0.00005 -0.00362
AFIX 23
H4A 2 -0.108849 0.130433 0.317815 11.00000 -1.20000
H4B 2 -0.037111 0.325477 0.333300 11.00000 -1.20000
AFIX 0
C4A 1 0.139224 0.202268 0.282886 11.00000 0.02363 0.02137 =
0.01905 0.00039 -0.00035 -0.00126
C5 1 0.071546 0.218078 0.234384 11.00000 0.02274 0.04402 =
0.02445 0.00248 -0.00505 0.00059
AFIX 43
H5 2 -0.060695 0.228797 0.228874 11.00000 -1.20000
AFIX 0
C6 1 0.193326 0.218421 0.194266 11.00000 0.03673 0.04325 =
0.01455 0.00137 -0.00448 0.00002
AFIX 43
H6 2 0.144780 0.230122 0.161566 11.00000 -1.20000
AFIX 0
C7 1 0.385561 0.201730 0.201823 11.00000 0.03173 0.04133 =
0.01974 -0.00093 0.00620 -0.00187
AFIX 43
H7 2 0.469721 0.200425 0.174352 11.00000 -1.20000
AFIX 0
C8 1 0.455020 0.186919 0.249574 11.00000 0.02214 0.03891 =
0.02351 -0.00175 0.00107 0.00075
AFIX 43
H8 2 0.587475 0.176093 0.254702 11.00000 -1.20000
AFIX 0
C8A 1 0.333659 0.187631 0.290306 11.00000 0.02252 0.01882 =
0.01683 -0.00116 -0.00210 0.00029
C9 1 0.622047 0.817779 0.430052 11.00000 0.01785 0.01525 =
0.01586 -0.00040 0.00127 0.00038
C10 1 0.694401 0.625613 0.433600 11.00000 0.01244 0.01437 =
0.01817 -0.00162 -0.00008 0.00002
AFIX 13
H10 2 0.659059 0.561013 0.402479 11.00000 -1.20000
AFIX 0
C11 1 0.600520 0.531052 0.477672 11.00000 0.01369 0.01689 =
0.01412 -0.00237 -0.00185 -0.00110
AFIX 13
H11 2 0.460966 0.528552 0.471655 11.00000 -1.20000
AFIX 0
C12 1 0.670618 0.338933 0.479872 11.00000 0.01295 0.01746 =
0.01477 0.00133 0.00112 -0.00223
N2 3 0.280864 0.212289 0.381079 11.00000 0.02319 0.02979 =
0.01492 0.00267 -0.00122 -0.00288
H2A 2 0.262995 0.333216 0.382291 11.00000 0.02887
H2B 2 0.325738 0.179401 0.410272 11.00000 0.02431
O1 4 0.741961 0.937380 0.437125 11.00000 0.02020 0.01259 =
0.04432 -0.00191 -0.00354 0.00000
O2 4 0.449314 0.840382 0.420428 11.00000 0.01495 0.01946 =
0.02041 0.00007 -0.00003 0.00194
O3 4 0.893711 0.619279 0.439015 11.00000 0.01411 0.01397 =
0.03307 -0.00209 0.00142 0.00074
H3 2 0.933077 0.721218 0.450083 11.00000 0.03914
O4 4 0.633227 0.623923 0.522240 11.00000 0.01695 0.02546 =
0.01945 -0.00903 -0.00226 0.00310
H4 2 0.742732 0.609054 0.531558 11.00000 0.04127
O6 4 0.747211 0.275500 0.515972 11.00000 0.02793 0.02599 =
0.01871 0.00310 -0.00496 0.00512
O5 4 0.639616 0.254334 0.438027 11.00000 0.02404 0.01156 =
0.01875 -0.00081 -0.00293 0.00185
H5A 2 0.675207 0.141137 0.440380 11.00000 0.05512
O7 4 0.215584 0.576190 0.381496 11.00000 0.02216 0.03360 =
0.03121 -0.01077 0.00340 -0.00260
H7A 2 0.295573 0.651484 0.394673 11.00000 0.05027
H7B 2 0.107924 0.581003 0.396706 11.00000 0.06302
HKLF 4
REM exp_471 in P2(1)2(1)2(1)
REM wR2 = 0.0776, GooF = S = 1.036, Restrained GooF = 1.037 for all data
REM R1 = 0.0367 for 2900 Fo > 4sig(Fo) and 0.0473 for all 3307 data
REM 218 parameters refined using 7 restraints
END
WGHT 0.0326 0.2899
REM Highest difference peak 0.248, deepest hole -0.193, 1-sigma level 0.043
Q1 1 0.6648 0.7171 0.4286 11.00000 0.05 0.25
Q2 1 0.2376 0.1469 0.2846 11.00000 0.05 0.24
Q3 1 0.0668 0.1869 0.3021 11.00000 0.05 0.23
Q4 1 0.6227 0.5638 0.4505 11.00000 0.05 0.20
Q5 1 0.2405 0.2694 0.2898 11.00000 0.05 0.19
Q6 1 0.3377 0.2152 0.3578 11.00000 0.05 0.18
Q7 1 0.1670 0.1517 0.1656 11.00000 0.05 0.18
Q8 1 0.3588 0.1834 0.3136 11.00000 0.05 0.18
Q9 1 0.1417 0.2656 0.2158 11.00000 0.05 0.17
Q10 1 0.2881 0.2418 0.1990 11.00000 0.05 0.17
Q11 1 0.2796 0.4635 0.3708 11.00000 0.05 0.17
Q12 1 0.1140 0.1796 0.2586 11.00000 0.05 0.17
Q13 1 0.1383 0.2623 0.2533 11.00000 0.05 0.17
Q14 1 0.3880 0.1361 0.2674 11.00000 0.05 0.17
Q15 1 0.8195 0.2865 0.4315 11.00000 0.05 0.17
Q16 1 0.6278 0.4382 0.4767 11.00000 0.05 0.16
Q17 1 0.8439 0.6529 0.4771 11.00000 0.05 0.16
Q18 1 0.1335 0.1494 0.2500 11.00000 0.05 0.16
Q19 1 0.2021 0.1496 0.3777 11.00000 0.05 0.16
Q20 1 0.8608 0.6255 0.4023 11.00000 0.05 0.16
;
_shelx_res_checksum 17245
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.4189(3) 0.1694(3) 0.34142(7) 0.0239(5) Uani d 1 . .
H H1A 0.464782 0.045500 0.345983 0.029 Uiso calc 1 . .
H H1B 0.528981 0.250520 0.344259 0.029 Uiso calc 1 . .
C C3 0.0946(3) 0.1243(4) 0.37283(8) 0.0285(5) Uani d 1 . .
H H3A 0.011223 0.144808 0.401784 0.034 Uiso calc 1 . .
H H3B 0.112372 -0.006161 0.368861 0.034 Uiso calc 1 . .
C C4 0.0045(3) 0.2016(4) 0.32647(8) 0.0270(6) Uani d 1 . .
H H4A -0.108849 0.130433 0.317815 0.032 Uiso calc 1 . .
H H4B -0.037111 0.325477 0.333300 0.032 Uiso calc 1 . .
C C4A 0.1392(3) 0.2023(3) 0.28289(7) 0.0214(5) Uani d 1 . .
C C5 0.0715(3) 0.2181(4) 0.23438(8) 0.0304(6) Uani d 1 . .
H H5 -0.060695 0.228797 0.228874 0.036 Uiso calc 1 . .
C C6 0.1933(4) 0.2184(4) 0.19427(8) 0.0315(6) Uani d 1 . .
H H6 0.144780 0.230122 0.161566 0.038 Uiso calc 1 . .
C C7 0.3856(4) 0.2017(4) 0.20182(8) 0.0309(6) Uani d 1 . .
H H7 0.469721 0.200425 0.174352 0.037 Uiso calc 1 . .
C C8 0.4550(3) 0.1869(3) 0.24957(8) 0.0282(5) Uani d 1 . .
H H8 0.587475 0.176093 0.254702 0.034 Uiso calc 1 . .
C C8A 0.3337(3) 0.1876(3) 0.29031(7) 0.0194(5) Uani d 1 . .
C C9 0.6220(3) 0.8178(3) 0.43005(7) 0.0163(4) Uani d 1 . .
C C10 0.6944(3) 0.6256(3) 0.43360(7) 0.0150(4) Uani d 1 . .
H H10 0.659059 0.561013 0.402479 0.018 Uiso calc 1 . .
C C11 0.6005(3) 0.5311(3) 0.47767(7) 0.0149(4) Uani d 1 . .
H H11 0.460966 0.528552 0.471655 0.018 Uiso calc 1 . .
C C12 0.6706(3) 0.3389(3) 0.47987(7) 0.0151(4) Uani d 1 . .
N N2 0.2809(3) 0.2123(3) 0.38108(7) 0.0226(4) Uani d 1 . .
H H2A 0.263(4) 0.333(3) 0.3823(9) 0.029(7) Uiso d 1 . .
H H2B 0.326(3) 0.179(3) 0.4103(7) 0.024(6) Uiso d 1 . .
O O1 0.7420(2) 0.93738(19) 0.43712(6) 0.0257(4) Uani d 1 . .
O O2 0.4493(2) 0.8404(2) 0.42043(5) 0.0183(3) Uani d 1 . .
O O3 0.8937(2) 0.6193(2) 0.43902(6) 0.0204(3) Uani d 1 . .
H H3 0.933(4) 0.721(3) 0.4501(9) 0.039(8) Uiso d 1 . .
O O4 0.6332(2) 0.6239(2) 0.52224(5) 0.0206(3) Uani d 1 . .
H H4 0.743(3) 0.609(4) 0.5316(10) 0.041(8) Uiso d 1 . .
O O6 0.7472(2) 0.2755(2) 0.51597(5) 0.0242(4) Uani d 1 . .
O O5 0.6396(2) 0.25433(19) 0.43803(5) 0.0181(3) Uani d 1 . .
H H5A 0.675(4) 0.141(3) 0.4404(11) 0.055(9) Uiso d 1 . .
O O7 0.2156(3) 0.5762(2) 0.38150(6) 0.0290(4) Uani d 1 . .
H H7A 0.296(4) 0.651(4) 0.3947(11) 0.050(9) Uiso d 1 . .
H H7B 0.108(4) 0.581(5) 0.3967(11) 0.063(11) 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
C1 0.0193(11) 0.0331(13) 0.0192(10) 0.0045(11) -0.0019(9) 0.0004(9)
C3 0.0244(13) 0.0404(15) 0.0208(10) -0.0100(12) 0.0004(10) 0.0047(10)
C4 0.0197(12) 0.0395(15) 0.0218(11) -0.0036(11) 0.0000(9) 0.0009(10)
C4A 0.0236(12) 0.0214(11) 0.0190(10) -0.0013(10) -0.0003(9) 0.0004(8)
C5 0.0227(12) 0.0440(15) 0.0244(11) 0.0006(12) -0.0051(9) 0.0025(10)
C6 0.0367(14) 0.0433(16) 0.0145(10) 0.0000(13) -0.0045(10) 0.0014(10)
C7 0.0317(13) 0.0413(15) 0.0197(11) -0.0019(13) 0.0062(10) -0.0009(10)
C8 0.0221(12) 0.0389(15) 0.0235(11) 0.0007(11) 0.0011(9) -0.0017(10)
C8A 0.0225(11) 0.0188(11) 0.0168(9) 0.0003(9) -0.0021(8) -0.0012(8)
C9 0.0179(10) 0.0152(10) 0.0159(9) 0.0004(9) 0.0013(8) -0.0004(8)
C10 0.0124(10) 0.0144(10) 0.0182(9) 0.0000(8) -0.0001(8) -0.0016(8)
C11 0.0137(10) 0.0169(10) 0.0141(9) -0.0011(8) -0.0019(8) -0.0024(8)
C12 0.0130(10) 0.0175(10) 0.0148(9) -0.0022(8) 0.0011(8) 0.0013(8)
N2 0.0232(10) 0.0298(12) 0.0149(8) -0.0029(9) -0.0012(8) 0.0027(8)
O1 0.0202(8) 0.0126(7) 0.0443(9) 0.0000(7) -0.0035(8) -0.0019(7)
O2 0.0149(7) 0.0195(8) 0.0204(7) 0.0019(6) 0.0000(6) 0.0001(6)
O3 0.0141(7) 0.0140(8) 0.0331(8) 0.0007(6) 0.0014(7) -0.0021(6)
O4 0.0169(8) 0.0255(8) 0.0194(7) 0.0031(7) -0.0023(7) -0.0090(6)
O6 0.0279(8) 0.0260(9) 0.0187(7) 0.0051(8) -0.0050(6) 0.0031(6)
O5 0.0240(8) 0.0116(8) 0.0188(7) 0.0018(6) -0.0029(6) -0.0008(6)
O7 0.0222(9) 0.0336(10) 0.0312(9) -0.0026(8) 0.0034(8) -0.0108(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N2 C1 C8A . . 112.07(18) ?
N2 C1 H1A . . 109.2 ?
C8A C1 H1A . . 109.2 ?
N2 C1 H1B . . 109.2 ?
C8A C1 H1B . . 109.2 ?
H1A C1 H1B . . 107.9 ?
N2 C3 C4 . . 108.99(18) ?
N2 C3 H3A . . 109.9 ?
C4 C3 H3A . . 109.9 ?
N2 C3 H3B . . 109.9 ?
C4 C3 H3B . . 109.9 ?
H3A C3 H3B . . 108.3 ?
C4A C4 C3 . . 112.13(19) ?
C4A C4 H4A . . 109.2 ?
C3 C4 H4A . . 109.2 ?
C4A C4 H4B . . 109.2 ?
C3 C4 H4B . . 109.2 ?
H4A C4 H4B . . 107.9 ?
C8A C4A C5 . . 118.6(2) ?
C8A C4A C4 . . 120.63(19) ?
C5 C4A C4 . . 120.8(2) ?
C6 C5 C4A . . 121.3(2) ?
C6 C5 H5 . . 119.4 ?
C4A C5 H5 . . 119.4 ?
C7 C6 C5 . . 119.9(2) ?
C7 C6 H6 . . 120.1 ?
C5 C6 H6 . . 120.1 ?
C6 C7 C8 . . 119.6(2) ?
C6 C7 H7 . . 120.2 ?
C8 C7 H7 . . 120.2 ?
C7 C8 C8A . . 121.0(2) ?
C7 C8 H8 . . 119.5 ?
C8A C8 H8 . . 119.5 ?
C4A C8A C8 . . 119.6(2) ?
C4A C8A C1 . . 122.13(19) ?
C8 C8A C1 . . 118.22(19) ?
O1 C9 O2 . . 126.43(19) ?
O1 C9 C10 . . 115.97(17) ?
O2 C9 C10 . . 117.60(17) ?
O3 C10 C9 . . 111.74(16) ?
O3 C10 C11 . . 109.57(16) ?
C9 C10 C11 . . 109.73(16) ?
O3 C10 H10 . . 108.6 ?
C9 C10 H10 . . 108.6 ?
C11 C10 H10 . . 108.6 ?
O4 C11 C12 . . 112.33(16) ?
O4 C11 C10 . . 111.24(16) ?
C12 C11 C10 . . 108.98(16) ?
O4 C11 H11 . . 108.1 ?
C12 C11 H11 . . 108.1 ?
C10 C11 H11 . . 108.1 ?
O6 C12 O5 . . 125.21(19) ?
O6 C12 C11 . . 123.19(18) ?
O5 C12 C11 . . 111.59(16) ?
C1 N2 C3 . . 112.25(17) ?
C1 N2 H2A . . 109.3(17) ?
C3 N2 H2A . . 108.7(18) ?
C1 N2 H2B . . 110.2(16) ?
C3 N2 H2B . . 109.1(16) ?
H2A N2 H2B . . 107(2) ?
C10 O3 H3 . . 109.0(19) ?
C11 O4 H4 . . 110(2) ?
C12 O5 H5A . . 111(2) ?
H7A O7 H7B . . 110(3) ?
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
C1 N2 . 1.483(3) ?
C1 C8A . 1.510(3) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C3 N2 . 1.489(3) ?
C3 C4 . 1.518(3) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C4 C4A . 1.512(3) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C4A C8A . 1.393(3) ?
C4A C5 . 1.397(3) ?
C5 C6 . 1.382(3) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.380(3) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.382(3) ?
C7 H7 . 0.9500 ?
C8 C8A . 1.393(3) ?
C8 H8 . 0.9500 ?
C9 O1 . 1.247(2) ?
C9 O2 . 1.260(3) ?
C9 C10 . 1.529(3) ?
C10 O3 . 1.417(2) ?
C10 C11 . 1.534(3) ?
C10 H10 . 1.0000 ?
C11 O4 . 1.407(2) ?
C11 C12 . 1.522(3) ?
C11 H11 . 1.0000 ?
C12 O6 . 1.211(2) ?
C12 O5 . 1.312(2) ?
N2 H2A . 0.91(2) ?
N2 H2B . 0.883(19) ?
O3 H3 . 0.87(2) ?
O4 H4 . 0.82(2) ?
O5 H5A . 0.89(2) ?
O7 H7A . 0.87(2) ?
O7 H7B . 0.87(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
C1 H1A O2 1_545 0.99 2.53 3.263(3) 130.8 no
C3 H3A O1 1_445 0.99 2.63 3.343(3) 128.6 no
N2 H2A O7 . 0.91(2) 1.85(2) 2.762(3) 176(2) yes
N2 H2B O6 4_456 0.883(19) 2.09(2) 2.787(2) 135(2) yes
N2 H2B O5 . 0.883(19) 2.41(2) 2.981(2) 122.9(19) yes
O3 H3 O1 . 0.87(2) 2.14(3) 2.612(2) 114(2) no
O3 H3 O4 4_566 0.87(2) 1.98(2) 2.766(2) 151(3) yes
O4 H4 O2 4_566 0.82(2) 1.99(2) 2.730(2) 150(3) yes
O5 H5A O1 1_545 0.89(2) 1.60(2) 2.480(2) 173(3) yes
O7 H7A O2 . 0.87(2) 1.91(2) 2.782(2) 173(3) yes
O7 H7B O3 1_455 0.87(2) 1.92(2) 2.772(2) 169(3) yes
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
N2 C3 C4 C4A . . . . 49.8(3) ?
C3 C4 C4A C8A . . . . -18.9(3) ?
C3 C4 C4A C5 . . . . 161.3(2) ?
C8A C4A C5 C6 . . . . 0.3(4) ?
C4 C4A C5 C6 . . . . -179.8(2) ?
C4A C5 C6 C7 . . . . 0.4(4) ?
C5 C6 C7 C8 . . . . -0.8(4) ?
C6 C7 C8 C8A . . . . 0.3(4) ?
C5 C4A C8A C8 . . . . -0.8(4) ?
C4 C4A C8A C8 . . . . 179.4(2) ?
C5 C4A C8A C1 . . . . -179.8(2) ?
C4 C4A C8A C1 . . . . 0.4(4) ?
C7 C8 C8A C4A . . . . 0.4(4) ?
C7 C8 C8A C1 . . . . 179.5(2) ?
N2 C1 C8A C4A . . . . -13.7(3) ?
N2 C1 C8A C8 . . . . 167.3(2) ?
O1 C9 C10 O3 . . . . -6.6(2) ?
O2 C9 C10 O3 . . . . 173.40(17) ?
O1 C9 C10 C11 . . . . 115.09(19) ?
O2 C9 C10 C11 . . . . -64.9(2) ?
O3 C10 C11 O4 . . . . 66.1(2) ?
C9 C10 C11 O4 . . . . -57.0(2) ?
O3 C10 C11 C12 . . . . -58.3(2) ?
C9 C10 C11 C12 . . . . 178.67(15) ?
O4 C11 C12 O6 . . . . -0.7(3) ?
C10 C11 C12 O6 . . . . 123.1(2) ?
O4 C11 C12 O5 . . . . -179.82(16) ?
C10 C11 C12 O5 . . . . -56.1(2) ?
C8A C1 N2 C3 . . . . 46.4(3) ?
C4 C3 N2 C1 . . . . -65.8(3) ?