#------------------------------------------------------------------------------
#$Date: 2019-02-14 05:36:51 +0200 (Thu, 14 Feb 2019) $
#$Revision: 213640 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/15/2021505.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_2021505
loop_
_publ_author_name
'Losev, Evgeniy A.'
'Boldyreva, Elena'
_publ_section_title
;
Concomitant cocrystal and salt: no interconversion in the solid state
;
_journal_coeditor_code KU3233
_journal_issue 3
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2053229619001372
_journal_volume 75
_journal_year 2019
_chemical_formula_iupac 'C3 H7 N O2 +, C4 H6 O6 -'
_chemical_formula_moiety 'C3 H7 N O2 +, C4 H6 O6 -'
_chemical_formula_sum 'C7 H13 N O8'
_chemical_formula_weight 239.18
_chemical_name_common '\b-Alanine--DL-tartaric acid (1/1)'
_chemical_name_systematic '\b-Alaninium DL-tartarate'
_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
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha 90
_cell_angle_beta 103.155(6)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 4.8531(3)
_cell_length_b 9.4182(4)
_cell_length_c 21.7022(12)
_cell_measurement_reflns_used 3013
_cell_measurement_temperature 175
_cell_measurement_theta_max 29.1780
_cell_measurement_theta_min 1.9700
_cell_volume 965.92(9)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_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
;
olex2.solve (Bourhis et al., 2015)
;
_diffrn_ambient_temperature 175
_diffrn_detector 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'STOE IPDS'
_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 0.0769
_diffrn_reflns_av_unetI/netI 0.0500
_diffrn_reflns_limit_h_max 5
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 10812
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.372
_diffrn_reflns_theta_min 1.927
_diffrn_source 'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 0.152
_exptl_absorpt_correction_T_max 0.995
_exptl_absorpt_correction_T_min 0.933
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.645
_exptl_crystal_description block
_exptl_crystal_F_000 504
_exptl_crystal_size_max 1
_exptl_crystal_size_mid 0.0953
_exptl_crystal_size_min 0.04
_refine_diff_density_max 0.334
_refine_diff_density_min -0.381
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.013
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 151
_refine_ls_number_reflns 1963
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.013
_refine_ls_R_factor_all 0.0636
_refine_ls_R_factor_gt 0.0391
_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^)+(0.0423P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0774
_refine_ls_wR_factor_ref 0.0853
_reflns_number_gt 1507
_reflns_number_total 1963
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ku3233sup1.cif
_cod_data_source_block 175_cocrystal_heating
_cod_original_cell_volume 965.93(9)
_cod_database_code 2021505
_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 0.862
_shelx_estimated_absorpt_t_max 0.994
_shelx_hkl_file
;
0 0 -2 55.5480 1.78507 2
0 0 2 59.7993 1.98052 1
0 0 -2 56.1416 1.93321 1
0 0 3-1.55393 1.21323 1
0 0 -3-1.71051 1.11036 2
0 0 -3-1.12728 1.19645 1
0 0 -4 17.0417 1.76121 2
0 0 4 15.8297 1.91751 1
0 0 -4 16.7665 1.89951 1
0 0 5-0.96296 1.62760 1
0 0 -5 0.50889 1.49000 1
0 0 -5-1.34917 1.37781 2
0 0 -6 108.969 4.45857 1
0 0 6 110.201 4.55023 1
0 0 -6 108.858 4.17419 2
0 0 -7 1.12809 1.75612 1
0 0 -7 0.81533 1.62296 2
0 0 7 0.68216 1.91259 1
0 0 -8 248.570 7.03650 2
0 0 8 241.089 7.51846 1
0 0 -8 249.391 7.50928 1
0 0 9 0.68908 2.22649 1
0 0 -9-2.21848 2.05880 1
0 0 -9 1.55257 2.01735 2
0 0 -10 7.58511 2.51862 1
0 0 10 7.33761 2.80947 1
0 0 -10 8.95424 2.53478 2
0 0 -11 3.98559 2.46182 1
0 0 -11 0.92468 2.14702 2
0 0 11-0.32803 2.65345 1
0 0 -12 56.7596 4.93564 1
0 0 12 53.0382 5.08236 1
0 0 -12 59.0324 4.72719 2
0 0 -13 1.18749 2.67202 1
0 0 13 0.12199 3.11050 1
0 0 -13 2.96003 2.72873 2
0 0 -14 137.918 7.39797 2
0 0 -14 139.178 7.92489 1
0 0 14 139.056 8.15691 1
0 0 -15 3.51211 3.22097 1
0 0 15 1.26116 3.64736 1
0 0 -15 3.68251 3.26558 2
0 0 -16 332.738 11.8876 2
0 0 -16 315.169 12.5300 1
0 0 16 321.270 12.9310 1
0 0 -17 3.53825 3.68967 2
0 0 17 5.98568 4.50899 1
0 0 -17 3.74923 3.84502 1
0 0 -18 240.724 12.1363 1
0 0 -18 233.093 10.9552 2
0 0 18 226.514 12.0368 1
0 0 -19-1.91942 5.11007 1
0 0 -19 5.11228 4.43055 2
0 0 19 2.79213 5.38259 1
0 0 -20 47.0465 6.66014 2
0 0 -20 46.5699 7.19062 1
0 0 20 36.9707 7.22011 1
0 0 21 5.97631 6.44648 1
0 0 -21 3.63151 5.05834 2
0 0 -21 6.60603 6.10555 1
0 0 -22 3.80078 6.36767 1
0 0 -22 15.5483 6.00261 2
0 0 22 9.28848 6.70609 1
0 0 -23-9.06934 7.86852 1
0 0 23-8.84822 7.95257 1
0 0 -23 2.40315 6.01061 2
0 0 24 2.68823 8.03299 1
0 0 -24 1.15821 8.09816 1
0 0 -24-2.21653 6.27323 2
0 0 -25 10.3260 8.83918 1
0 0 -25-4.22818 7.37395 2
0 0 25 10.4915 8.78398 1
0 0 26 22.1290 9.45093 1
0 0 -26 20.6812 10.4059 1
0 0 -26 23.1834 8.76693 2
0 0 -27 14.8549 11.1650 1
0 0 -27-6.09253 8.41239 2
0 0 27 13.3096 10.0601 1
0 0 -28 30.2977 9.75796 2
0 0 -28 4.31712 11.9452 1
0 0 28 3.37740 10.0409 1
0 0 -29-0.94706 10.6279 2
0 0 29 7.74271 11.7993 1
0 -1 0-1.11287 0.99118 2
0 1 0 0.67157 0.95920 2
0 1 1 17.1597 1.08172 1
0 -1 -1 16.2827 1.47235 2
0 1 1 16.4239 1.35790 2
0 -1 -1 18.1691 1.15464 1
0 1 2 65.1706 2.23848 1
0 -1 -2 67.4808 2.28463 1
0 -1 2 65.6113 2.04230 1
0 -1 -2 64.2181 2.56155 2
0 1 -2 66.7552 2.05330 1
0 1 2 67.6030 2.58198 2
0 1 3 271.261 5.04286 1
0 -1 3 274.927 4.72176 1
0 1 -3 245.381 4.51622 1
0 -1 -3 272.780 5.34666 2
0 1 3 262.401 5.24166 2
0 -1 -3 261.844 4.94611 1
0 1 4 6.96971 1.62832 1
0 -1 -4 5.50369 1.56415 1
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0 -1 4 5.20059 1.48270 1
0 1 -4 5.48354 1.46346 1
0 -1 -4 5.73966 1.59874 2
0 -1 -5 1.65531 1.66411 1
0 1 5-2.10650 1.69233 1
0 -1 5 0.04284 1.43378 1
0 -1 -5-0.70384 1.55174 2
0 1 5-0.83056 1.60734 2
0 1 -5-2.80057 1.58344 1
0 1 -6 190.411 5.70203 1
0 -1 -6 190.573 5.73432 2
0 1 6 191.310 5.77040 2
0 -1 -6 187.770 5.85384 1
0 1 6 189.313 5.84471 1
0 -1 6 190.094 5.67499 1
0 -1 -7 2.83920 1.96993 2
0 1 -7 1.03868 1.73097 1
0 1 7 1.56939 1.92258 2
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0 1 7 0.51617 1.69105 1
0 -1 -7 1.81738 1.97936 1
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0 -1 -8 0.58294 2.08529 1
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0 1 -8 5.31540 2.14096 1
0 -1 -9 16.2677 3.05203 1
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0 1 9 15.2045 2.98661 1
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0 -1 -9 14.5693 2.67044 2
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0 -1 -10 2.63278 2.31258 1
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0 -1 -10-4.88005 2.40217 2
0 1 -11 284.924 9.53789 1
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0 -1 -12 15.0110 3.19851 2
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0 -2 -4 187.547 5.76687 2
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-6 -2 -3 9.90936 9.92838 2
-6 2 -3-11.7860 14.5665 1
-6 -2 -3 20.2027 11.8691 1
-6 2 -4 11.7535 12.4527 1
-6 -2 -4 11.9190 11.4053 1
-6 -2 -4 17.9140 10.4431 2
-6 2 -4 17.7705 12.7806 1
-6 2 -5 9.33874 14.4970 1
-6 2 -5 17.9343 11.8034 1
-6 -2 -5 9.96038 12.1417 1
-6 -2 -5 6.72316 11.5313 1
-6 -2 -5 10.7446 11.8943 2
-6 2 -6-6.61484 12.6981 1
-6 2 -6 1.98017 12.2586 1
-6 -2 -6-10.0153 11.3553 1
-6 -2 -6 9.14737 12.5827 1
-6 -2 -6 13.2424 12.2342 2
6 3 -18 2.99825 6.90427 1
-6 3 18 22.8551 8.07771 1
-6 3 18 18.2688 3.47333 2
-6 -3 18 9.12794 6.16294 1
6 -3 -18 12.5534 8.37706 1
-6 3 17 26.9631 12.3654 1
-6 3 17 37.2596 6.52332 2
6 3 -17 53.4783 12.6207 1
-6 -3 17 23.0703 10.6740 1
-6 -3 16 3.02533 9.70588 1
-6 3 16 11.3523 13.8976 1
6 -3 -16-1.53546 12.6453 1
-6 3 16 11.2406 5.95259 2
6 3 -16-7.92414 10.4250 1
-6 -3 15-2.02741 9.43431 1
-6 3 15 11.9021 12.7515 1
-6 3 15-0.72627 6.65579 2
6 -3 -15-0.28271 14.5503 1
-6 -3 14-8.02669 9.74151 1
-6 3 14-7.30951 11.3423 1
-6 3 14 1.71745 6.52744 2
6 -3 -14 8.52419 13.5747 1
-6 -3 13 27.8368 9.80023 1
6 -3 -13 12.6561 11.0913 1
-6 3 13 55.0661 14.1385 1
-6 3 13 39.5339 7.62915 2
-6 -3 13 17.9020 9.35474 1
-6 -3 12 33.8408 9.84354 1
-6 3 12 41.3284 12.8661 1
-6 3 12 19.8980 7.44269 2
-6 -3 12 46.3082 9.84413 1
6 -3 -11 6.48741 12.5145 1
-6 -3 11 6.43850 8.60010 1
-6 3 11 1.81050 9.72049 1
-6 3 11 9.39845 7.25597 2
-6 -3 11-8.45614 8.34759 1
-6 -3 10 8.55058 8.94128 1
-6 3 10 8.08120 7.09018 2
-6 3 10-2.54544 11.3500 1
-6 -3 10 22.0346 9.00762 1
-6 -3 9-2.73711 3.08539 2
-6 -3 9-2.41677 8.26779 1
-6 3 9 10.9375 7.52109 2
-6 3 9 24.8293 12.0412 1
-6 3 9-23.4622 10.9557 1
-6 -3 9-10.7171 8.45433 1
-6 -3 8 0.62119 4.36939 2
-6 -3 8 1.04377 8.35745 1
-6 3 8 8.66314 7.70109 2
-6 3 8-6.44826 9.83459 1
-6 3 8 2.16149 10.4647 1
-6 -3 8 4.56423 7.90928 1
-6 -3 7 10.3649 5.53537 2
-6 -3 7 13.5349 9.24747 1
-6 3 7 29.6103 8.90907 2
-6 3 7 32.1013 12.0402 1
-6 3 7 15.3979 10.8755 1
-6 -3 7 9.38031 7.91849 1
-6 -3 6-0.61705 5.80720 2
-6 -3 6-1.66959 8.48083 1
-6 3 6-14.8104 11.0456 1
-6 3 6-11.1314 11.0140 1
-6 -3 6 0.40270 7.95637 1
-6 -3 5 13.7375 8.62604 1
-6 3 5 11.2300 11.9526 1
-6 -3 5 1.92419 6.26437 2
-6 3 5 28.2962 12.2064 1
-6 -3 5 2.36010 8.47898 1
-6 -3 4-11.7703 8.71131 1
-6 3 4-2.53499 12.2562 1
-6 -3 4 4.64793 7.11001 2
-6 3 4 6.31589 10.5917 1
-6 -3 4-4.55705 8.81347 1
-6 -3 3 10.8734 8.47459 1
-6 -3 3 9.73463 8.91455 1
-6 3 3-6.47902 12.4353 1
-6 -3 3-2.71250 6.93068 2
-6 3 3-3.60871 9.90430 1
-6 -3 2-13.7882 8.96918 1
-6 -3 2 2.18174 9.11544 1
-6 3 2-12.4464 12.4975 1
-6 -3 2 2.22870 7.68669 2
-6 3 2 1.20920 10.7147 1
-6 -3 1 29.4884 9.41759 1
-6 -3 1 18.5926 9.86223 1
-6 -3 1 7.63326 8.05211 2
-6 3 1 31.7800 13.3981 1
-6 3 1 19.5075 11.5721 1
-6 -3 0-4.62308 9.29788 1
-6 -3 0-3.05010 8.86662 2
-6 -3 0-2.34723 9.63337 1
-6 3 0 26.8938 12.8434 1
-6 3 0 8.76269 11.8962 1
-6 3 -1 25.9136 10.8903 1
-6 -3 -1 27.7847 9.68881 1
-6 -3 -1 4.54778 9.00199 2
-6 3 -1 3.85206 11.3282 1
-6 -3 -1 8.18641 10.2306 1
-6 3 -2 9.51818 10.8461 1
-6 -3 -2 8.11011 9.22820 1
-6 -3 -2-1.76868 10.1132 2
-6 3 -2-15.2244 14.3974 1
-6 -3 -2 10.3963 11.0994 1
-6 3 -3 16.0391 13.3136 1
-6 -3 -3 0.06542 9.54932 1
-6 -3 -3-17.5572 11.4193 2
-6 3 -3 4.26858 14.1739 1
-6 -3 -3-6.33461 10.7928 1
-6 3 -4-26.7281 12.8630 1
-6 -3 -4-6.13570 10.3663 1
-6 -3 -4-2.94291 10.7351 2
-6 3 -4-9.19141 12.4381 1
-6 -3 -4 9.60605 12.1612 1
-6 -3 -5 2.56599 12.4010 1
-6 3 -5 23.9905 12.4821 1
-6 -3 -5 14.9140 11.1661 1
-6 -3 -5 2.71871 11.4922 2
-6 3 -5 21.1850 14.5613 1
-6 -3 -6 3.92371 5.63646 2
-6 4 16-5.96292 12.0863 1
6 -4 -16-3.42973 13.8919 1
-6 4 16 10.0652 6.73765 2
-6 -4 16-5.81599 7.50186 1
-6 4 15 8.30925 14.0100 1
-6 4 15 8.26009 7.85231 2
6 -4 -15-6.44256 12.4567 1
-6 -4 15-12.0932 9.12281 1
-6 -4 15 27.9423 9.76223 1
6 -4 -14-6.43497 15.0487 1
-6 -4 14 1.97440 8.81851 1
-6 4 14 5.38803 11.9552 1
-6 4 14 8.18702 8.07043 2
-6 -4 14 10.9503 9.66743 1
-6 -4 13 6.10441 8.65664 1
-6 4 13 20.4617 11.9377 1
6 -4 -13 24.2506 14.6337 1
-6 4 13 5.54094 7.73560 2
-6 -4 13-2.54483 8.41515 1
-6 -4 12 16.2749 7.98804 1
6 -4 -12-13.5204 13.2223 1
-6 4 12 26.9549 13.5041 1
-6 4 12 18.9970 7.72941 2
-6 -4 12 15.2859 8.86460 1
-6 -4 11 22.6724 8.22076 1
6 -4 -11 52.0231 14.6486 1
-6 4 11 1.21218 12.9792 1
-6 4 11 36.4569 8.66110 2
-6 -4 11 21.8630 8.29586 1
-6 -4 10 24.6337 8.49579 1
-6 4 10 17.7965 11.0422 1
-6 4 10 10.9681 8.14789 2
-6 -4 10 9.27786 8.52639 1
-6 -4 9-1.04462 8.62611 1
-6 -4 9 3.88681 2.43577 2
-6 4 9-13.2061 8.61480 2
-6 4 9 13.4265 10.4421 1
-6 4 9-5.58075 12.1957 1
-6 -4 9 0.41803 8.08841 1
-6 -4 8 8.45440 8.14514 1
-6 -4 8-4.96574 4.14238 2
-6 4 8 9.99100 8.69951 2
-6 4 8-14.2359 12.6174 1
-6 4 8-6.65358 12.2964 1
-6 -4 8-5.85090 8.75364 1
-6 -4 7 0.60970 5.07804 2
-6 -4 7-7.02238 8.37979 1
-6 4 7 6.22615 9.17571 2
-6 4 7 12.5458 11.0212 1
-6 4 7 11.1233 12.2950 1
-6 -4 7 15.3340 7.85590 1
-6 -4 6-0.26607 8.32308 1
-6 -4 6 3.60456 5.74106 2
-6 -4 6 24.4370 8.70246 1
-6 4 6 10.6982 8.88113 2
-6 4 6-3.68347 11.4265 1
-6 4 6 29.9483 13.7940 1
-6 4 5-10.1872 13.1437 1
-6 -4 5 7.51667 8.46215 1
-6 -4 5-4.15785 6.30906 2
-6 4 5 4.00425 9.10713 2
-6 -4 5-4.76918 8.32518 1
-6 -4 4-2.03788 8.32420 1
-6 4 4 11.7821 13.3437 1
-6 -4 4-3.13132 6.78185 2
-6 4 4-26.1900 13.2513 1
-6 -4 3 9.38761 8.28462 1
-6 4 3 17.6051 13.5195 1
-6 -4 3 3.38860 7.42588 2
-6 4 3 9.25606 12.5051 1
-6 -4 3-3.82697 9.07566 1
-6 -4 2 24.5532 9.08181 1
-6 -4 2 8.00189 8.10098 1
-6 4 2 14.8656 12.9699 1
-6 -4 2 5.76418 7.78212 2
-6 4 2 6.50761 12.0990 1
-6 -4 1 18.5337 8.84881 1
-6 -4 1 3.73062 9.43491 1
-6 4 1 3.45064 12.8268 1
-6 -4 1-2.18601 8.55896 2
-6 4 1 4.93767 10.3651 1
-6 -4 0 10.8159 8.62684 1
-6 -4 0 17.0093 10.1512 1
-6 -4 0 7.50259 8.83687 2
-6 4 0-0.27660 12.2945 1
-6 4 0-1.37166 10.9357 1
-6 -4 -1 10.4479 9.45727 1
-6 -4 -1 7.52678 9.24117 2
-6 -4 -1 29.0234 11.1590 1
-6 4 -1 32.2714 14.9766 1
-6 4 -1 22.1276 13.7657 1
-6 4 -2-13.8258 13.4614 1
-6 -4 -2 8.80882 9.92138 1
-6 -4 -2 4.58239 10.1483 2
-6 4 -2-1.99502 14.3058 1
-6 -4 -2-5.20124 10.2772 1
-6 4 -3 39.4131 14.9856 1
-6 -4 -3 11.2348 10.3113 1
-6 -4 -3 12.1326 11.2384 2
-6 4 -3 1.16082 12.9169 1
-6 -4 -3 18.9352 11.0705 1
-6 -4 -4 34.3533 8.78657 1
-6 -4 -4 33.6833 9.08374 1
-6 5 14 13.9565 5.96485 2
-6 -5 14 15.0172 5.17776 1
-6 -5 14 8.42986 4.47776 1
-6 5 13 49.5052 15.3923 1
-6 5 13 11.0338 8.47406 2
6 -5 -13 26.9169 13.8792 1
-6 -5 13 16.9143 8.25090 1
-6 -5 13 30.0015 8.44916 1
-6 -5 12 12.9381 8.24349 1
-6 5 12 55.4051 11.1546 2
-6 5 12 32.5921 14.7017 1
6 -5 -12 26.5977 16.6751 1
-6 -5 12 32.2478 9.11385 1
-6 -5 11 7.35421 8.09579 1
-6 5 11-2.09032 12.2137 1
-6 -5 11 7.94516 8.22417 1
-6 -5 10 22.9740 8.78891 1
-6 5 10 34.6211 13.1649 1
-6 5 10 21.1969 9.59619 2
-6 -5 10 26.3898 8.89694 1
-6 -5 9-2.34576 7.96562 1
-6 -5 9 20.7654 8.41093 1
-6 5 9-0.18327 9.49306 2
-6 5 9-3.53902 11.6864 1
-6 -5 8 0.41224 7.88238 1
-6 -5 8 1.19476 8.10112 1
-6 -5 8-1.18738 4.14358 2
-6 5 8-12.0714 10.1544 2
-6 5 8 14.2342 12.9246 1
-6 5 8 2.12816 13.7325 1
-6 -5 7 4.62909 7.52771 1
-6 -5 7 12.0654 7.71453 1
-6 -5 7-0.38252 5.68584 2
-6 5 7 26.9971 10.7041 2
-6 5 7 4.01666 12.7530 1
-6 5 7 16.7507 14.2128 1
-6 -5 6 7.48398 8.10211 1
-6 -5 6-10.9076 8.02458 1
-6 -5 6-7.21289 6.72679 2
-6 5 6-1.14522 10.2971 2
-6 5 6-24.4013 14.7783 1
-6 5 6-1.37296 13.8848 1
-6 -5 5-13.3320 8.59097 1
-6 -5 5-0.03756 7.02094 2
-6 -5 5 4.73504 8.40342 1
-6 5 5-10.5648 10.1886 2
-6 5 5 9.56216 14.0619 1
-6 5 4 13.4284 13.6256 1
-6 -5 4 13.6688 7.73658 1
-6 -5 4 2.17735 7.56794 2
-6 5 4 21.7141 10.4989 2
-6 -5 4-11.9444 8.08896 1
-6 5 4-9.79452 13.5496 1
-6 5 3 2.71262 11.8295 1
-6 -5 3 12.6782 8.04599 1
-6 -5 3 8.73328 7.77549 2
-6 -5 3 9.40125 8.78802 1
-6 5 3-0.44196 13.1640 1
-6 5 2-0.28341 12.1135 1
-6 -5 2-7.52734 8.15200 1
-6 -5 2-9.19549 8.26056 2
-6 5 2 11.2664 12.9286 1
-6 -5 2 1.44837 8.74931 1
-6 -5 1 9.56522 9.28843 1
-6 -5 1 18.6149 8.67447 1
-6 5 1 12.4688 14.9515 1
-6 -5 1 1.88897 8.84474 2
-6 5 1 15.3568 12.2680 1
-6 -5 0-4.26367 9.34675 1
-6 -5 0 5.50830 8.63043 1
-6 5 0 9.13679 14.8864 1
-6 -5 0 17.9789 10.1262 2
-6 5 0 16.0786 11.7242 1
-6 -5 -1 17.5560 8.80947 1
-6 -5 -1 14.7752 8.82085 1
-6 -5 -2 14.5851 6.06378 2
-6 6 9 8.08457 6.46506 2
-6 6 8 13.5234 7.73830 2
-6 -6 8 35.5816 5.70832 1
-6 -6 8 26.7857 5.45159 1
-6 -6 7 8.15141 5.48778 1
-6 -6 7 12.8029 5.58879 1
-6 -6 7-4.46159 4.96274 2
-6 6 7 0.57406 8.62737 2
-6 -6 6-11.1741 5.82361 2
-6 6 6 0.95867 8.87281 2
-6 -6 5-6.54849 5.46597 1
-6 -6 5 14.3165 5.78185 1
-6 6 5 8.55452 9.05784 2
-6 -6 4 42.1134 7.10549 2
-6 6 4 30.6018 9.61327 2
-6 -6 4 34.7514 6.05594 1
-6 -6 4 37.8977 6.17431 1
-6 -6 3 14.4126 5.28674 2
-6 6 3 9.17290 6.67582 2
0 0 0 0.00 0.00 0
TITL 175_II in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 4.853103 9.418216 21.702247 90.0000 103.1546 90.0000
ZERR 4.00 0.000307 0.000397 0.001203 0.0000 0.0060 0.0000
LATT 1
SYMM -x, y+1/2,-z+1/2
SFAC C H N O
UNIT 28.00 52.00 4.00 32.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 88540
_shelx_res_file
;
TITL 175_II in P2(1)/c
175_ii.res
created by SHELXL-2018/3 at 16:14:20 on 31-Aug-2018
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 4.853103 9.418216 21.702247 90 103.1546 90
ZERR 4 0.000307 0.000397 0.001203 0 0.006 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O
UNIT 28 52 4 32
EQIV $1 1-X,1-Y,-Z
EQIV $2 1+X,+Y,+Z
EQIV $3 2-X,0.5+Y,0.5-Z
EQIV $4 -1+X,1.5-Y,-0.5+Z
EQIV $5 1-X,0.5+Y,0.5-Z
L.S. 10
PLAN 20
SIZE 0.04 0.0953 1
TEMP -98.15
HTAB O4 O3_$1
HTAB O3 O4_$2
HTAB O6 O8_$3
HTAB O1 O7_$4
HTAB N1 O7
HTAB N1 O8_$5
HTAB N1 O2_$1
CONF
BOND $H
BOND
fmap 2
acta
SHEL 40 0.8
TWIN -1 0 0 0 -1 0 2 0 1 2
REM
REM
REM
WGHT 0.042300
BASF 0.78399
FVAR 0.46086
O4 4 0.281041 0.645584 0.000395 11.00000 0.01816 0.02377 =
0.02374 0.00679 0.00013 -0.00311
AFIX 147
H4 2 0.364526 0.583503 0.025664 11.00000 -1.20000
AFIX 0
O3 4 0.726278 0.614815 -0.068235 11.00000 0.01358 0.01771 =
0.02205 -0.00170 -0.00069 0.00428
AFIX 147
H3 2 0.896560 0.624678 -0.049327 11.00000 -1.20000
AFIX 0
O6 4 0.873818 0.872494 0.051749 11.00000 0.02638 0.01980 =
0.01761 -0.00094 -0.00581 -0.00522
AFIX 147
H6 2 1.003818 0.874941 0.084741 11.00000 -1.20000
AFIX 0
O1 4 0.177102 0.864296 -0.118373 11.00000 0.02686 0.02333 =
0.01906 -0.00418 -0.00622 0.01258
AFIX 147
H1 2 0.039344 0.866732 -0.149821 11.00000 -1.20000
AFIX 0
C4 1 0.717339 0.759718 0.052822 11.00000 0.01989 0.01756 =
0.01610 -0.00355 0.00678 0.00213
C3 1 0.471390 0.756813 -0.003878 11.00000 0.01656 0.01604 =
0.01562 0.00022 0.00178 -0.00098
AFIX 13
H3A 2 0.367047 0.848716 -0.005153 11.00000 -1.20000
AFIX 0
O5 4 0.757626 0.667766 0.092803 11.00000 0.02525 0.02601 =
0.01913 0.00704 0.00120 -0.00161
O7 4 0.729535 0.583713 0.300934 11.00000 0.01831 0.01738 =
0.02080 0.00095 -0.00069 -0.00566
O8 4 0.707053 0.380025 0.352109 11.00000 0.02480 0.01889 =
0.02256 0.00497 -0.00723 0.00014
O2 4 0.287205 0.664874 -0.164520 11.00000 0.02217 0.01774 =
0.01732 -0.00318 -0.00160 0.00002
C2 1 0.578462 0.744522 -0.065458 11.00000 0.01622 0.01284 =
0.01670 -0.00110 0.00385 0.00016
AFIX 13
H2 2 0.708579 0.825750 -0.067657 11.00000 -1.20000
AFIX 0
C5 1 0.611154 0.468560 0.309440 11.00000 0.01636 0.01382 =
0.01560 -0.00314 0.00391 0.00191
C1 1 0.330822 0.751224 -0.121840 11.00000 0.01559 0.01396 =
0.01520 0.00299 0.00357 -0.00181
C6 1 0.332866 0.433280 0.264761 11.00000 0.01872 0.01411 =
0.01556 0.00093 0.00344 -0.00196
AFIX 23
H6A 2 0.194448 0.406805 0.289973 11.00000 -1.20000
H6B 2 0.360152 0.349545 0.239222 11.00000 -1.20000
AFIX 0
N1 3 0.397734 0.589355 0.176649 11.00000 0.02718 0.01533 =
0.01788 0.00160 0.00745 0.00397
AFIX 137
H1A 2 0.391051 0.518143 0.148006 11.00000 -1.50000
H1B 2 0.578671 0.600162 0.199417 11.00000 -1.50000
H1C 2 0.337766 0.671688 0.155960 11.00000 -1.50000
AFIX 0
C7 1 0.209893 0.553315 0.220306 11.00000 0.01599 0.02051 =
0.01463 0.00099 0.00100 0.00008
AFIX 23
H7A 2 0.021214 0.525099 0.195116 11.00000 -1.20000
H7B 2 0.185410 0.638273 0.245388 11.00000 -1.20000
AFIX 0
HKLF 4
REM 175_II in P2(1)/c
REM wR2 = 0.0853, GooF = S = 1.013, Restrained GooF = 1.013 for all data
REM R1 = 0.0391 for 1507 Fo > 4sig(Fo) and 0.0636 for all 1963 data
REM 151 parameters refined using 0 restraints
END
WGHT 0.0423 0.0000
REM Highest difference peak 0.334, deepest hole -0.381, 1-sigma level 0.088
Q1 1 0.6327 0.5387 -0.0670 11.00000 0.05 0.33
Q2 1 0.8069 0.6184 0.2845 11.00000 0.05 0.33
Q3 1 0.3349 0.5374 -0.0141 11.00000 0.05 0.33
Q4 1 0.2221 0.6250 -0.0537 11.00000 0.05 0.32
Q5 1 0.1563 0.8541 -0.0728 11.00000 0.05 0.32
Q6 1 0.8096 0.3739 0.3470 11.00000 0.05 0.31
Q7 1 0.0908 0.6356 0.2271 11.00000 0.05 0.30
Q8 1 0.5443 0.4376 0.3872 11.00000 0.05 0.30
Q9 1 0.8165 0.3089 0.3547 11.00000 0.05 0.30
Q10 1 0.6430 0.7183 0.0696 11.00000 0.05 0.30
Q11 1 0.0592 0.8304 -0.1231 11.00000 0.05 0.30
Q12 1 0.7729 0.5770 0.0899 11.00000 0.05 0.29
Q13 1 0.6841 0.8945 -0.0908 11.00000 0.05 0.29
Q14 1 0.2456 0.6669 0.2486 11.00000 0.05 0.29
Q15 1 0.4113 0.6499 -0.0070 11.00000 0.05 0.29
Q16 1 0.8630 0.6215 0.1300 11.00000 0.05 0.28
Q17 1 0.6014 0.6095 0.3060 11.00000 0.05 0.28
Q18 1 0.3798 0.5802 -0.1686 11.00000 0.05 0.28
Q19 1 0.7367 0.4568 0.2216 11.00000 0.05 0.28
Q20 1 0.3677 0.3549 0.1892 11.00000 0.05 0.28
;
_shelx_res_checksum 99288
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 O4 0.2810(3) 0.64558(15) 0.00040(8) 0.0226(4) Uani d 1
H H4 0.364526 0.583503 0.025664 0.027 Uiso calc 1
O O3 0.7263(3) 0.61482(14) -0.06824(7) 0.0185(4) Uani d 1
H H3 0.896560 0.624678 -0.049327 0.022 Uiso calc 1
O O6 0.8738(4) 0.87249(15) 0.05175(7) 0.0230(4) Uani d 1
H H6 1.003818 0.874941 0.084741 0.028 Uiso calc 1
O O1 0.1771(4) 0.86430(15) -0.11837(7) 0.0249(4) Uani d 1
H H1 0.039344 0.866732 -0.149821 0.030 Uiso calc 1
C C4 0.7173(5) 0.7597(2) 0.05282(10) 0.0174(5) Uani d 1
C C3 0.4714(5) 0.7568(2) -0.00388(10) 0.0164(5) Uani d 1
H H3A 0.367047 0.848716 -0.005153 0.020 Uiso calc 1
O O5 0.7576(4) 0.66777(16) 0.09280(8) 0.0241(4) Uani d 1
O O7 0.7295(4) 0.58371(15) 0.30093(7) 0.0197(4) Uani d 1
O O8 0.7071(4) 0.38003(15) 0.35211(7) 0.0241(4) Uani d 1
O O2 0.2872(4) 0.66487(14) -0.16452(7) 0.0201(4) Uani d 1
C C2 0.5785(5) 0.7445(2) -0.06546(10) 0.0152(5) Uani d 1
H H2 0.708579 0.825750 -0.067657 0.018 Uiso calc 1
C C5 0.6112(5) 0.4686(2) 0.30944(10) 0.0152(5) Uani d 1
C C1 0.3308(5) 0.7512(2) -0.12184(10) 0.0149(5) Uani d 1
C C6 0.3329(5) 0.4333(2) 0.26476(10) 0.0162(5) Uani d 1
H H6A 0.194448 0.406805 0.289973 0.019 Uiso calc 1
H H6B 0.360152 0.349545 0.239222 0.019 Uiso calc 1
N N1 0.3977(4) 0.58936(18) 0.17665(9) 0.0198(5) Uani d 1
H H1A 0.391051 0.518143 0.148006 0.030 Uiso calc 1
H H1B 0.578671 0.600162 0.199417 0.030 Uiso calc 1
H H1C 0.337766 0.671688 0.155960 0.030 Uiso calc 1
C C7 0.2099(5) 0.5533(2) 0.22031(10) 0.0174(5) Uani d 1
H H7A 0.021214 0.525099 0.195116 0.021 Uiso calc 1
H H7B 0.185410 0.638273 0.245388 0.021 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
O4 0.0182(9) 0.0238(8) 0.0237(9) -0.0031(7) 0.0001(8) 0.0068(7)
O3 0.0136(9) 0.0177(7) 0.0220(9) 0.0043(7) -0.0007(8) -0.0017(6)
O6 0.0264(10) 0.0198(8) 0.0176(9) -0.0052(7) -0.0058(8) -0.0009(6)
O1 0.0269(10) 0.0233(8) 0.0191(9) 0.0126(8) -0.0062(8) -0.0042(6)
C4 0.0199(13) 0.0176(11) 0.0161(12) 0.0021(10) 0.0068(10) -0.0035(9)
C3 0.0166(13) 0.0160(10) 0.0156(12) -0.0010(10) 0.0018(10) 0.0002(9)
O5 0.0252(10) 0.0260(8) 0.0191(9) -0.0016(8) 0.0012(8) 0.0070(7)
O7 0.0183(9) 0.0174(7) 0.0208(9) -0.0057(7) -0.0007(7) 0.0010(6)
O8 0.0248(10) 0.0189(7) 0.0226(9) 0.0001(7) -0.0072(8) 0.0050(7)
O2 0.0222(9) 0.0177(8) 0.0173(9) 0.0000(7) -0.0016(7) -0.0032(7)
C2 0.0162(13) 0.0128(10) 0.0167(12) 0.0002(9) 0.0039(10) -0.0011(8)
C5 0.0164(12) 0.0138(10) 0.0156(12) 0.0019(10) 0.0039(10) -0.0031(9)
C1 0.0156(13) 0.0140(10) 0.0152(11) -0.0018(9) 0.0036(10) 0.0030(9)
C6 0.0187(13) 0.0141(10) 0.0156(11) -0.0020(10) 0.0034(10) 0.0009(9)
N1 0.0272(12) 0.0153(8) 0.0179(10) 0.0040(9) 0.0075(9) 0.0016(7)
C7 0.0160(12) 0.0205(11) 0.0146(12) 0.0001(9) 0.0010(10) 0.0010(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 -1 4 0.0320
-4 3 4 0.0300
4 -3 -4 0.0100
2 2 -1 0.2270
1 1 -4 0.0240
-2 -2 1 0.2800
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C3 O4 H4 109.5
C2 O3 H3 109.5
C4 O6 H6 109.5
C1 O1 H1 109.5
O6 C4 C3 110.80(18)
O5 C4 O6 126.4(2)
O5 C4 C3 122.8(2)
O4 C3 C4 111.58(17)
O4 C3 H3A 108.0
O4 C3 C2 110.78(17)
C4 C3 H3A 108.0
C4 C3 C2 110.36(18)
C2 C3 H3A 108.0
O3 C2 C3 111.88(17)
O3 C2 H2 108.9
O3 C2 C1 108.50(17)
C3 C2 H2 108.9
C1 C2 C3 109.62(18)
C1 C2 H2 108.9
O7 C5 C6 117.80(18)
O8 C5 O7 125.1(2)
O8 C5 C6 117.09(18)
O1 C1 C2 110.23(18)
O2 C1 O1 125.8(2)
O2 C1 C2 123.98(19)
C5 C6 H6A 108.7
C5 C6 H6B 108.7
C5 C6 C7 114.16(18)
H6A C6 H6B 107.6
C7 C6 H6A 108.7
C7 C6 H6B 108.7
H1A N1 H1B 109.5
H1A N1 H1C 109.5
H1B N1 H1C 109.5
C7 N1 H1A 109.5
C7 N1 H1B 109.5
C7 N1 H1C 109.5
C6 C7 H7A 109.4
C6 C7 H7B 109.4
N1 C7 C6 111.32(18)
N1 C7 H7A 109.4
N1 C7 H7B 109.4
H7A C7 H7B 108.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O4 H4 0.8400
O4 C3 1.414(3)
O3 H3 0.8400
O3 C2 1.425(2)
O6 H6 0.8400
O6 C4 1.309(3)
O1 H1 0.8400
O1 C1 1.312(3)
C4 C3 1.507(3)
C4 O5 1.210(2)
C3 H3A 1.0000
C3 C2 1.545(3)
O7 C5 1.260(2)
O8 C5 1.254(2)
O2 C1 1.214(2)
C2 H2 1.0000
C2 C1 1.509(3)
C5 C6 1.509(3)
C6 H6A 0.9900
C6 H6B 0.9900
C6 C7 1.518(3)
N1 H1A 0.9100
N1 H1B 0.9100
N1 H1C 0.9100
N1 C7 1.496(3)
C7 H7A 0.9900
C7 H7B 0.9900
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
O4 H4 O3 3_665 0.84 2.17 2.865(2) 139.6 yes
O3 H3 O4 1_655 0.84 1.94 2.780(2) 175.6 yes
O6 H6 O8 2_755 0.84 1.72 2.562(2) 174.6 yes
O1 H1 O7 4_475 0.84 1.70 2.509(2) 160.9 yes
N1 H1A O2 3_665 0.91 2.30 2.885(2) 121.9 yes
N1 H1B O7 . 0.91 2.16 2.810(2) 127.3 yes
N1 H1C O8 2_655 0.91 1.98 2.828(2) 154.9 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
O4 C3 C2 O3 -60.9(2)
O4 C3 C2 C1 59.5(2)
O3 C2 C1 O1 175.26(18)
O3 C2 C1 O2 -6.2(3)
O6 C4 C3 O4 -172.72(18)
O6 C4 C3 C2 63.7(2)
C4 C3 C2 O3 63.2(2)
C4 C3 C2 C1 -176.39(16)
C3 C2 C1 O1 52.8(2)
C3 C2 C1 O2 -128.7(2)
O5 C4 C3 O4 7.5(3)
O5 C4 C3 C2 -116.1(2)
O7 C5 C6 C7 -8.3(3)
O8 C5 C6 C7 171.99(19)
C5 C6 C7 N1 63.7(2)
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.2160(12)
2 0.7840(12)
_cod_database_fobs_code 2021505