#------------------------------------------------------------------------------
#$Date: 2019-02-14 05:36:51 +0200 (Thu, 14 Feb 2019) $
#$Revision: 213640 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/15/2021500.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_2021500
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 102.948(5)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 4.8745(3)
_cell_length_b 9.4321(4)
_cell_length_c 21.7086(11)
_cell_measurement_reflns_used 3198
_cell_measurement_temperature 250
_cell_measurement_theta_max 29.2980
_cell_measurement_theta_min 1.9240
_cell_volume 972.71(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 250
_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 0.0764
_diffrn_reflns_av_unetI/netI 0.0497
_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 10880
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.371
_diffrn_reflns_theta_min 1.925
_diffrn_source 'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 0.151
_exptl_absorpt_correction_T_max 0.995
_exptl_absorpt_correction_T_min 0.937
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.633
_exptl_crystal_description block
_exptl_crystal_F_000 504
_exptl_crystal_size_max 1
_exptl_crystal_size_mid 0.0952
_exptl_crystal_size_min 0.04
_refine_diff_density_max 0.214
_refine_diff_density_min -0.203
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.021
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 151
_refine_ls_number_reflns 1983
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.021
_refine_ls_R_factor_all 0.0694
_refine_ls_R_factor_gt 0.0421
_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^)+(0.0373P)^2^+0.0773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0764
_refine_ls_wR_factor_ref 0.0834
_reflns_number_gt 1488
_reflns_number_total 1983
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file ku3233sup1.cif
_cod_data_source_block 250_cocrystal
_cod_original_cell_volume 972.72(9)
_cod_database_code 2021500
_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 0.863
_shelx_estimated_absorpt_t_max 0.994
_shelx_hkl_file
;
0 0 -2 65.5741 1.78498 1
0 0 2 64.6390 1.83787 1
0 0 3 1.36668 1.08484 2
0 0 -3 1.26402 0.97384 1
0 0 3-0.83735 1.18715 1
0 0 4 18.3265 1.83544 1
0 0 4 18.6199 1.68449 2
0 0 -4 21.4064 1.70346 1
0 0 -5-1.75689 1.25690 1
0 0 5 2.04369 1.43373 2
0 0 5 0.92912 1.59272 1
0 0 6 96.3209 3.43202 2
0 0 6 105.366 3.98832 1
0 0 -6 103.902 3.79579 1
0 0 7 0.07791 1.54037 2
0 0 -7-1.12604 1.49303 1
0 0 7 0.03132 1.87550 1
0 0 8 225.459 5.83925 2
0 0 8 233.032 6.55433 1
0 0 -8 229.024 6.37542 1
0 0 9-2.38541 2.35284 1
0 0 9 1.43177 2.00735 2
0 0 -9 1.36702 1.94954 1
0 0 10 6.51787 2.31407 2
0 0 -10 4.75782 2.24525 1
0 0 10 3.08229 2.55370 1
0 0 11 2.48327 2.68475 1
0 0 -11-0.68576 2.29315 1
0 0 11 0.27096 2.12178 2
0 0 12 50.6546 4.58700 1
0 0 12 55.6046 4.10618 2
0 0 -12 54.6879 4.46836 1
0 0 13-1.52831 2.73071 2
0 0 -13-1.22636 2.80170 1
0 0 13-0.24451 3.04065 1
0 0 -14 131.205 6.95565 1
0 0 14 119.634 6.17668 2
0 0 14 115.763 6.78572 1
0 0 15-0.61378 3.66272 1
0 0 15-5.11388 3.05098 2
0 0 -15-0.79459 3.26421 1
0 0 16 267.308 10.5469 1
0 0 -16 266.871 10.3639 1
0 0 16 288.778 9.71592 2
0 0 17 1.88250 3.63568 2
0 0 -17-0.12537 3.76272 1
0 0 17 8.71637 4.61094 1
0 0 18 230.469 10.7711 1
0 0 -18 245.625 10.7995 1
0 0 18 239.822 9.78770 2
0 0 -19-3.45029 4.23866 1
0 0 19 3.12537 4.00746 2
0 0 19-5.24036 4.94098 1
0 0 20 46.6542 6.12904 2
0 0 20 57.8446 7.36009 1
0 0 -20 52.4952 6.51765 1
0 0 -21 1.52655 4.50429 1
0 0 21 0.98961 5.60852 1
0 0 21-3.13255 5.01080 2
0 0 22-0.88126 6.35862 1
0 0 22 6.00735 5.10095 2
0 0 -22-4.22942 4.87672 1
0 0 23-6.09870 5.29498 2
0 0 23-3.69548 7.18047 1
0 0 -23 1.84507 5.49881 1
0 0 24 4.26886 7.36760 1
0 0 24-6.48238 6.49699 2
0 0 -24 9.26526 6.82476 1
0 0 25 8.63671 6.50953 2
0 0 -25-1.45242 7.77919 1
0 0 25-0.28388 7.48560 1
0 0 26 5.75561 7.31867 2
0 0 -26 8.78524 9.00856 1
0 0 26 8.36897 7.79837 1
0 0 27 23.5815 9.18484 2
0 0 27-1.51814 7.82027 1
0 0 -27-1.00613 10.3786 1
0 0 28 1.51960 9.46155 1
0 0 28 7.71300 8.57239 2
0 0 29 16.3207 11.2213 1
0 0 29-9.35412 10.1625 2
0 0 -29-2.50150 12.7967 1
0 -1 0-0.52582 0.82631 2
0 1 0-0.41357 1.07849 2
0 -1 -1 18.5787 1.27655 2
0 1 1 18.3703 1.44948 2
0 -1 -1 16.8363 1.00380 1
0 1 1 17.7502 1.02579 1
0 1 -2 67.1632 1.81796 1
0 -1 2 67.8620 1.85446 1
0 -1 -2 68.8163 2.32610 2
0 1 2 66.2009 2.32244 2
0 1 2 62.6900 1.99054 1
0 -1 -2 65.8198 2.02121 1
0 -1 -3 261.146 4.53720 2
0 -1 -3 252.575 4.33160 1
0 1 -3 246.573 3.93393 1
0 1 3 260.248 4.38775 1
0 1 3 259.194 4.53606 2
0 -1 3 245.448 3.96178 1
0 -1 -4 5.47453 1.64863 2
0 -1 -4 5.02456 1.41874 1
0 1 4 4.64960 1.58977 1
0 1 -4 6.74454 1.36328 1
0 1 4 5.51399 1.50036 2
0 -1 4 3.26284 1.42365 1
0 1 5 1.00325 1.43969 1
0 1 5-0.22226 1.60151 2
0 1 -5 2.09935 1.45362 1
0 -1 -5 0.33722 1.51391 2
0 -1 5 1.59022 1.46807 1
0 -1 -5 1.92246 1.34071 1
0 -1 -6 187.991 5.23432 1
0 -1 -6 193.139 5.07238 2
0 1 6 175.725 4.99301 1
0 1 -6 185.291 4.98718 1
0 1 6 181.730 4.87988 2
0 -1 6 184.320 4.89449 1
0 1 7 4.66994 2.03631 2
0 -1 -7 7.18948 2.10276 2
0 1 7 5.85946 2.08447 1
0 -1 -7 3.17036 2.00713 1
0 -1 7 8.11905 2.04684 1
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0 -1 -8 3.16566 2.05619 2
0 -1 8 3.94635 2.08208 1
0 -1 -8 5.52321 2.30201 1
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0 1 -8-0.51079 1.70648 1
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0 -1 -9 19.5001 2.72150 1
0 -1 -9 23.0128 2.92747 2
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0 1 9 19.9900 2.71197 2
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0 -1 -10 2.84204 2.54834 1
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0 1 10 2.20009 2.12604 2
0 -1 11 244.130 7.75697 1
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0 -1 -11 242.163 7.90042 1
0 1 11 239.664 7.40005 2
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0 1 -12 13.0915 3.20245 1
0 -1 12 14.3233 3.37920 1
0 1 12 12.7389 3.03348 2
0 1 12 13.4454 3.34440 1
0 -1 -12 6.63026 3.17629 1
0 -1 13 288.625 8.48694 2
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0 -2 -1 2.05811 1.57412 2
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-6 -2 -2-3.50548 10.6583 1
-6 -2 -2 0.86306 4.76895 2
6 2 2-10.1267 11.9641 1
6 -2 3-10.2849 9.77646 1
-6 2 -3 7.64631 8.59983 1
-6 -2 -3 11.6733 10.3180 1
-6 -2 -3-2.57988 4.37273 2
6 2 3 11.4356 11.8066 1
-6 2 -4 3.08195 9.10377 1
6 -2 4 14.5004 9.57451 1
-6 -2 -4-5.14773 12.1191 1
6 2 4 6.94719 10.2883 1
-6 -2 -4 14.2746 3.64485 2
-6 2 -5 17.4047 10.2445 1
6 2 5-8.29094 14.6447 1
-6 -2 -5-5.07136 9.88538 1
-6 -2 -5 1.02822 2.19642 2
6 -2 5-9.64770 10.4373 1
-6 -2 -6 12.3681 12.5599 1
6 2 6-8.38080 11.1221 1
-6 2 -6 7.22904 9.57637 1
-6 -2 -7-3.81876 9.51498 1
6 -2 7-16.3148 9.60188 1
6 2 7-12.0241 11.9619 1
-6 2 -7-0.77531 8.04681 1
-6 3 18-2.98899 9.21450 1
-6 3 18-5.44818 8.08953 1
-6 3 18-15.2861 8.93065 2
-6 -3 17 8.78328 9.95450 1
-6 3 17-0.93855 11.3693 1
-6 3 17-5.26638 9.25873 1
-6 3 17-2.27846 9.76997 2
-6 -3 16-0.08723 11.0984 1
-6 3 16 13.0611 10.3529 1
-6 3 16 1.28998 9.38693 2
-6 -3 16-2.66010 13.7150 1
-6 3 16 1.36210 11.3610 1
-6 -3 15 9.42635 12.3683 1
-6 3 15-16.9239 10.0775 1
-6 3 15-0.06463 9.66497 2
-6 -3 15 8.54852 10.7248 1
-6 3 15-2.79302 10.4635 1
-6 -3 14-12.7493 12.4878 1
-6 3 14-2.51267 8.32384 1
-6 3 14 6.07889 8.99163 2
-6 -3 14 5.37039 12.2792 1
-6 3 14-13.5602 10.8349 1
-6 3 13 25.8699 8.75561 1
-6 3 13 9.11205 8.20524 2
-6 -3 13 41.2184 13.4110 1
-6 3 13 20.4949 9.44228 1
-6 -3 13-1.42048 9.80162 1
-6 3 12 3.77094 8.52150 1
-6 3 12 7.45492 7.63219 2
-6 3 12-9.74566 8.74937 1
-6 -3 12 0.61321 10.2604 1
-6 -3 12 9.42759 9.51224 1
-6 3 11-1.52884 8.01857 1
-6 3 11 4.69567 7.26601 2
-6 3 11 24.1096 9.45991 1
-6 -3 11 15.5034 9.16102 1
-6 -3 11 14.1675 11.3970 1
-6 3 10 9.94617 8.32231 1
-6 3 10-0.77036 8.23340 1
-6 -3 10 4.52385 8.97722 1
-6 3 10 3.47767 6.67663 2
-6 -3 10 0.08183 10.8190 1
-6 3 9 7.03897 7.90840 1
-6 3 9-2.50785 8.01281 1
-6 -3 9 0.25323 8.97701 1
-6 3 9-5.07710 6.63755 2
-6 -3 9-17.9896 9.01673 1
-6 3 8-8.77959 7.91562 1
-6 3 8 5.09980 8.06945 1
-6 -3 8-0.08354 8.40514 1
-6 3 8 0.04152 5.76913 2
-6 -3 8-4.92194 8.47833 1
-6 -3 7 7.46206 9.17325 1
-6 3 7-2.81228 5.58431 2
-6 -3 7 3.55164 10.0196 1
-6 3 7-1.99648 8.10611 1
-6 3 7 2.92126 7.60103 1
-6 3 6 1.52699 5.40017 2
-6 3 6-16.8074 8.01277 1
-6 -3 6 11.6491 10.8676 1
-6 3 6-12.5763 7.49445 1
-6 -3 6 12.3698 11.0239 1
-6 3 5 7.09322 5.16711 2
-6 -3 5 17.5267 8.03471 2
-6 3 5 0.35188 8.03034 1
-6 -3 5 19.5212 11.0407 1
-6 -3 5 14.1652 11.0868 1
-6 3 5 13.5350 7.72556 1
-6 3 4 2.80594 4.38916 2
-6 3 4-3.41255 7.79628 1
-6 -3 4 21.3043 7.70967 2
-6 -3 4 0.24553 10.0134 1
-6 -3 4 9.19793 10.6265 1
-6 3 4 25.8717 8.49507 1
-6 3 3 1.62159 3.29115 2
-6 3 3-2.06941 7.79968 1
-6 -3 3-3.67607 6.93651 2
-6 -3 3 1.47038 8.22514 1
-6 -3 3-11.8294 11.3677 1
-6 3 3 0.74631 7.36636 1
-6 3 2 17.9478 8.40986 1
-6 -3 2 3.94868 6.73400 2
-6 3 2 6.24699 1.71119 2
-6 3 2 10.1485 7.89898 1
6 3 -1-13.1714 11.8119 1
-6 3 1 3.78300 7.88582 1
-6 -3 1-14.1401 10.9941 1
-6 -3 1 9.31870 6.69152 2
-6 3 1 18.2080 7.94696 1
6 3 0 6.04994 11.1615 1
-6 3 0 26.1001 8.40162 1
-6 -3 0 24.1070 10.1059 1
-6 -3 0 30.8586 6.94732 2
-6 3 0 23.0532 8.23279 1
-6 3 -1 24.8525 8.36796 1
6 3 1 0.44418 9.66975 1
-6 -3 -1 27.5538 11.0493 1
-6 -3 -1 16.1720 6.25336 2
-6 3 -1 23.9150 8.89130 1
-6 3 -2 7.50611 8.42564 1
-6 -3 -2-8.54345 12.6433 1
-6 -3 -2-1.13846 6.14985 2
6 3 2-19.4843 13.2220 1
-6 3 -3-0.47777 8.34363 1
-6 -3 -3 1.94386 9.97324 1
-6 -3 -3 5.26650 5.84717 2
6 3 3 22.1967 13.0412 1
-6 3 -4-3.55566 8.65184 1
-6 -3 -4-12.6090 11.5664 1
6 3 4 11.4124 11.0937 1
-6 -3 -4 11.0689 5.75011 2
6 -3 4 9.41640 9.77122 1
-6 -3 -5 19.9001 5.69144 2
-6 -3 -5 32.4384 13.1038 1
6 -3 5 32.6453 10.7053 1
-6 3 -5 39.8468 10.0520 1
-6 3 -6-2.48761 7.34611 1
6 -3 6-8.08305 8.17491 1
-6 -4 16-10.2796 11.2441 1
-6 4 16 14.6746 10.0941 1
-6 4 16-3.70891 10.3350 2
-6 -4 16 3.15447 11.9006 1
-6 4 16 1.79853 10.4727 1
-6 -4 15-7.41803 10.4785 1
-6 4 15 11.9156 9.62061 1
-6 4 15 12.4398 10.2100 2
-6 -4 15 1.44763 14.0463 1
-6 4 15-8.62381 9.35056 1
-6 -4 14 8.19829 12.4097 1
-6 4 14-8.68295 8.56403 1
-6 4 14-2.29960 9.40965 2
-6 4 14 19.9130 10.3529 1
-6 4 13 0.59001 8.53496 1
-6 4 13-1.00112 9.29022 2
-6 4 13-5.12312 9.18322 1
-6 -4 13-4.08028 12.0012 1
-6 -4 13-9.89058 12.6320 1
-6 4 12-5.68637 8.23788 1
-6 4 12 12.4358 8.28816 2
-6 4 12 20.4703 8.91442 1
-6 -4 12 4.38118 13.5353 1
-6 -4 12-6.42565 12.5980 1
-6 4 11 10.2593 7.88828 1
-6 4 11-9.92006 9.06940 1
-6 -4 11 11.2680 12.3688 1
-6 4 11 14.5738 7.76322 2
-6 -4 11 0.60382 10.1144 1
-6 4 10 12.3883 7.98593 1
-6 4 10 9.86689 8.04766 1
-6 -4 10-0.35698 10.8996 1
-6 4 10-7.72367 7.45113 2
-6 4 9-3.71152 8.37862 1
-6 4 9-3.08775 7.78054 1
-6 -4 9-1.67614 9.88250 1
-6 4 9 4.37295 6.90926 2
-6 -4 9 9.86002 11.0598 1
-6 4 8-0.37567 7.52401 1
-6 -4 8-1.39807 9.30516 1
-6 4 8 0.49777 6.46469 2
-6 -4 8-11.1793 12.2685 1
-6 4 8-11.9516 8.10928 1
-6 -4 7 16.7510 9.95379 1
-6 4 7 13.1510 7.73080 1
-6 4 7-2.62192 6.20479 2
-6 4 7-13.4922 7.78869 1
-6 -4 7 6.20039 11.7090 1
-6 4 6 10.8911 7.45376 1
-6 4 6 13.8106 5.87076 2
-6 4 6-2.16138 7.68219 1
-6 -4 6 1.44108 8.35790 2
-6 -4 6 17.0847 11.6056 1
-6 -4 6 2.24755 9.98877 1
-6 4 5 8.62065 5.15554 2
-6 4 5-6.84394 7.36272 1
-6 -4 5 28.6425 9.00405 2
-6 -4 5 20.1790 11.2914 1
-6 -4 5 2.41297 11.6432 1
-6 4 5-5.03954 7.38946 1
-6 4 4 8.66207 7.70550 1
-6 4 4-1.53155 4.14246 2
-6 -4 4-3.50956 8.04040 2
-6 -4 4-10.8259 12.5686 1
-6 -4 4 6.44674 11.1271 1
-6 4 4-6.97294 7.22486 1
-6 4 3 7.70706 7.40310 1
-6 -4 3-3.53877 8.05811 2
-6 -4 3-13.4200 12.0610 1
-6 4 3 1.31169 7.35069 1
-6 4 2 3.57284 7.52139 1
-6 -4 2 25.8986 10.4181 1
-6 -4 2 10.5902 7.74439 2
-6 4 2 26.6994 7.89432 1
-6 4 1 11.1233 7.41006 1
6 4 -1-1.64076 12.2999 1
-6 -4 1 14.6812 9.40897 1
-6 -4 1 3.62667 7.68589 2
-6 4 1 22.5761 7.99091 1
6 4 0-5.16435 10.6725 1
-6 4 0 0.10395 7.82169 1
-6 -4 0 0.95059 11.9765 1
-6 -4 0-6.09430 7.78225 2
-6 4 0-7.14314 8.12642 1
-6 4 -1-4.56577 8.16078 1
6 4 1 15.9732 12.6305 1
-6 -4 -1 19.1756 12.7860 1
-6 -4 -1-4.04770 7.25464 2
-6 4 -1 1.47221 8.18250 1
-6 4 -2 11.6106 8.19674 1
-6 -4 -2-6.06141 11.9111 1
-6 -4 -2-1.43774 7.11557 2
-6 4 -2 7.68152 8.37322 1
6 4 2-14.5063 13.6356 1
-6 -4 -3 3.01626 9.96743 1
-6 -4 -3 8.22805 7.50277 2
6 4 3 10.4087 11.4699 1
-6 4 -3 3.03285 8.34897 1
-6 4 -3-2.83711 7.98739 1
-6 -4 -4 21.1504 12.6203 1
-6 -4 -4 18.0548 6.91220 2
-6 4 -4 10.1472 8.49994 1
-6 5 14 28.7647 8.10449 2
-6 5 14-13.6482 7.89743 1
-6 5 13 11.2335 8.79270 1
-6 5 13 30.0656 9.57467 1
-6 5 13 5.41393 9.25351 2
-6 -5 13 10.9235 14.4004 1
-6 -5 13-5.03821 13.0053 1
-6 5 12-2.30975 8.65195 1
-6 5 12 15.6000 8.44625 1
-6 -5 12 9.44275 12.1194 1
-6 5 12 16.0952 9.47848 2
-6 -5 12-1.81921 11.3117 1
-6 5 11 6.06139 8.52954 1
-6 5 11 13.7678 8.14953 1
-6 -5 11 1.60360 11.4382 1
-6 5 11 12.5805 8.49455 2
-6 -5 11-8.32017 9.43944 1
-6 5 10-1.83976 7.18470 1
-6 -5 10-6.14687 13.0549 1
-6 5 10 0.59344 7.89202 2
-6 -5 10 28.8862 11.8293 1
-6 5 10 17.7776 8.58625 1
-6 -5 9-2.49177 13.0111 1
-6 5 9-10.2733 7.00342 1
-6 5 9-10.4421 7.83402 2
-6 5 9 9.63897 7.96255 1
-6 -5 9-6.33651 11.6547 1
-6 -5 8 20.4086 13.0599 1
-6 5 8 5.68739 7.28875 1
-6 5 8 2.01409 7.34037 2
-6 -5 8 14.8810 10.4616 2
-6 5 8 4.87815 7.72425 1
-6 -5 8-15.7483 11.8379 1
-6 5 7-0.04653 7.48527 1
-6 5 7-5.00613 6.73655 2
-6 5 7 20.3658 7.88317 1
-6 -5 7-21.4257 10.5153 2
-6 -5 7-3.38584 12.2148 1
-6 -5 7 4.45619 13.3384 1
-6 5 6-0.73740 6.76607 1
-6 5 6 1.43887 5.87899 2
-6 5 6-8.41644 7.81644 1
-6 -5 6 5.18896 9.94412 2
-6 -5 6-1.16186 12.7525 1
-6 -5 6-1.45153 12.5693 1
-6 5 5 6.53954 7.15890 1
-6 5 5 5.40054 7.20585 1
-6 5 5-1.81174 5.04766 2
-6 -5 5-6.99834 10.0251 2
-6 -5 5 1.62555 13.0872 1
-6 -5 5 23.4044 13.2348 1
-6 5 4-5.59339 7.22542 1
-6 5 4-1.55680 6.87567 1
-6 5 4 2.63904 4.07885 2
-6 -5 4-2.10172 9.65974 2
-6 -5 4 8.55034 13.1417 1
-6 -5 4 2.95102 11.9332 1
-6 5 3 4.42988 7.07406 1
-6 -5 3 12.5974 9.42949 2
-6 -5 3-3.75988 13.4689 1
-6 -5 3-3.39903 10.9491 1
-6 5 3-2.54120 6.86888 1
-6 5 2-4.90795 6.98650 1
-6 -5 2 17.2926 12.7082 1
-6 -5 2 17.5494 9.43579 2
-6 5 2 20.4496 7.95656 1
-6 5 1 5.35044 7.26925 1
6 5 -1 5.75573 13.4725 1
-6 -5 1 10.4437 11.2776 1
-6 -5 1 10.6150 9.26202 2
-6 5 1 1.61817 7.35013 1
-6 5 0 22.3226 7.84360 1
-6 -5 0 23.2102 10.8949 1
-6 -5 0 26.9521 9.27751 2
-6 5 0 26.4540 8.02907 1
-6 -5 -1 15.6334 11.6926 1
-6 -5 -1 13.6302 8.50184 2
-6 5 -1 6.24171 7.82636 1
-6 5 -1 13.7447 7.52237 1
-6 -5 -2 34.7994 6.83648 2
-6 5 -2 24.3771 6.31206 1
-6 6 10 11.4183 4.20681 1
-6 6 10 6.72124 4.95175 2
-6 -6 10 14.7289 6.63992 2
-6 6 10 3.63789 4.00598 1
-6 6 9 30.6730 6.81269 2
-6 -6 9 30.1706 9.28522 2
-6 6 8 25.8826 6.64458 1
-6 6 8 11.9774 7.05527 2
-6 6 8 18.2627 6.74541 1
-6 6 7 12.0873 6.47882 1
-6 6 7 5.28197 6.54354 1
-6 6 7 11.1796 6.66217 2
-6 6 6 14.9560 6.37264 1
-6 6 6 5.52081 6.53214 1
-6 6 6 13.2719 6.29404 2
-6 -6 6 9.48236 10.4223 2
-6 6 5 14.6536 6.19233 1
-6 6 5 30.1323 6.76389 1
-6 6 5 21.5355 5.80010 2
-6 6 4 18.3222 5.90428 1
-6 6 4 2.21198 5.63202 1
-6 6 4 25.2933 4.48067 2
-6 -6 4 7.10978 9.35742 2
-6 6 3-0.39799 4.90770 1
-6 -6 3 27.7802 7.65444 2
-6 6 2 1.67294 3.18621 1
-6 6 2 1.88210 3.30096 1
-6 -6 2 7.22633 5.01417 2
0 0 0 0.00 0.00 0
TITL 250_III in P2(1)/c
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 4.874545 9.432103 21.708558 90.0000 102.9478 90.0000
ZERR 4.00 0.000282 0.000398 0.001066 0.0000 0.0053 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 84610
_shelx_res_file
;
TITL 250_II in P2(1)/c
250_iii.res
created by SHELXL-2018/3 at 15:35:25 on 11-Aug-2018
REM P2(1)/c (#14 in standard setting)
CELL 0.71073 4.874545 9.432103 21.708558 90 102.9478 90
ZERR 4 0.000282 0.000398 0.001066 0 0.0053 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 0.0952 1
TEMP -23.15
HTAB O4 O3_$1
HTAB O3 O4_$2
HTAB O6 O8_$3
HTAB O1 O7_$4
HTAB N1 O7
HTAB N1 O8_$5
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 0.037300 0.077300
BASF 0.22650
FVAR 0.46182
O4 4 0.282911 0.646401 0.000849 11.00000 0.02272 0.03167 =
0.03253 0.00958 0.00174 -0.00408
AFIX 147
H4 2 0.365377 0.584342 0.025225 11.00000 -1.20000
AFIX 0
O3 4 0.726408 0.616436 -0.067183 11.00000 0.01544 0.02437 =
0.02942 -0.00224 -0.00054 0.00471
AFIX 147
H3 2 0.892784 0.626309 -0.047959 11.00000 -1.20000
AFIX 0
O6 4 0.873436 0.872796 0.052337 11.00000 0.03192 0.02951 =
0.02620 -0.00057 -0.00781 -0.00727
AFIX 147
H6 2 0.997341 0.876901 0.085467 11.00000 -1.20000
AFIX 0
O1 4 0.175598 0.862482 -0.117957 11.00000 0.03455 0.03437 =
0.02446 -0.00660 -0.00915 0.01600
AFIX 147
H1 2 0.040071 0.864208 -0.148893 11.00000 -1.20000
AFIX 0
C4 1 0.717754 0.760443 0.053555 11.00000 0.02247 0.02420 =
0.02039 -0.00280 0.00552 0.00233
C3 1 0.472397 0.757628 -0.003218 11.00000 0.01887 0.02049 =
0.02248 0.00100 0.00234 0.00052
AFIX 13
H3A 2 0.369526 0.848453 -0.004435 11.00000 -1.20000
AFIX 0
O5 4 0.759201 0.668403 0.093080 11.00000 0.03543 0.03695 =
0.02351 0.00993 -0.00168 -0.00293
O7 4 0.730126 0.583941 0.300785 11.00000 0.01996 0.02531 =
0.02774 0.00203 -0.00355 -0.00711
O8 4 0.708144 0.380713 0.351606 11.00000 0.03390 0.02613 =
0.03105 0.00753 -0.01280 -0.00039
O2 4 0.287947 0.664845 -0.163537 11.00000 0.02765 0.02603 =
0.02385 -0.00670 -0.00173 0.00210
C2 1 0.578112 0.745041 -0.064644 11.00000 0.01815 0.01872 =
0.02060 -0.00037 0.00290 0.00188
AFIX 13
H2 2 0.705425 0.825603 -0.067088 11.00000 -1.20000
AFIX 0
C5 1 0.612463 0.469281 0.308922 11.00000 0.01836 0.02075 =
0.01933 -0.00305 0.00323 0.00349
C1 1 0.329835 0.750857 -0.121428 11.00000 0.01711 0.01928 =
0.02050 0.00316 0.00478 -0.00085
C6 1 0.334841 0.434168 0.264484 11.00000 0.01983 0.01978 =
0.02125 0.00152 0.00225 -0.00337
AFIX 23
H6A 2 0.199123 0.407897 0.289680 11.00000 -1.20000
H6B 2 0.361674 0.351299 0.239244 11.00000 -1.20000
AFIX 0
N1 3 0.393790 0.587847 0.175845 11.00000 0.03470 0.02396 =
0.02398 0.00351 0.00975 0.00726
AFIX 137
H1A 2 0.388979 0.516121 0.148282 11.00000 -1.50000
H1B 2 0.571704 0.600681 0.197906 11.00000 -1.50000
H1C 2 0.331693 0.667772 0.154604 11.00000 -1.50000
AFIX 0
C7 1 0.210430 0.553106 0.220022 11.00000 0.01914 0.02522 =
0.02111 0.00073 0.00092 0.00071
AFIX 23
H7A 2 0.023959 0.524863 0.195735 11.00000 -1.20000
H7B 2 0.187477 0.637546 0.244688 11.00000 -1.20000
AFIX 0
HKLF 4
REM 250_II in P2(1)/c
REM wR2 = 0.0834, GooF = S = 1.021, Restrained GooF = 1.021 for all data
REM R1 = 0.0421 for 1488 Fo > 4sig(Fo) and 0.0694 for all 1983 data
REM 151 parameters refined using 0 restraints
END
WGHT 0.0373 0.0773
REM Highest difference peak 0.214, deepest hole -0.203, 1-sigma level 0.048
Q1 1 0.2769 0.4981 0.2498 11.00000 0.05 0.21
Q2 1 0.8916 0.3664 0.3695 11.00000 0.05 0.19
Q3 1 0.1096 0.3994 0.1784 11.00000 0.05 0.18
Q4 1 0.8153 0.5637 0.0544 11.00000 0.05 0.18
Q5 1 0.8602 0.6237 0.3002 11.00000 0.05 0.16
Q6 1 0.1407 0.7271 -0.2033 11.00000 0.05 0.16
Q7 1 0.6321 0.4834 0.0416 11.00000 0.05 0.16
Q8 1 0.6936 0.6158 0.3405 11.00000 0.05 0.16
Q9 1 0.4275 0.4579 0.2949 11.00000 0.05 0.15
Q10 1 0.7065 0.5996 0.2570 11.00000 0.05 0.15
Q11 1 0.7247 0.3015 0.3526 11.00000 0.05 0.15
Q12 1 0.8134 0.6775 0.0618 11.00000 0.05 0.15
Q13 1 0.0868 0.6980 0.0284 11.00000 0.05 0.15
Q14 1 0.3436 0.6356 -0.1197 11.00000 0.05 0.15
Q15 1 0.6900 0.6321 -0.0321 11.00000 0.05 0.15
Q16 1 0.3096 0.6788 -0.2082 11.00000 0.05 0.14
Q17 1 0.0335 0.6053 -0.1399 11.00000 0.05 0.14
Q18 1 0.2413 0.3592 0.2697 11.00000 0.05 0.14
Q19 1 0.5966 0.4401 0.3410 11.00000 0.05 0.14
Q20 1 0.2421 0.4979 -0.0127 11.00000 0.05 0.14
;
_shelx_res_checksum 42198
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 0.2829(4) 0.64640(16) 0.00085(8) 0.0297(4) Uani d 1
H H4 0.365377 0.584342 0.025225 0.036 Uiso calc 1
O O3 0.7264(3) 0.61644(15) -0.06718(8) 0.0240(4) Uani d 1
H H3 0.892784 0.626309 -0.047959 0.029 Uiso calc 1
O O6 0.8734(4) 0.87280(16) 0.05234(8) 0.0315(4) Uani d 1
H H6 0.997341 0.876901 0.085467 0.038 Uiso calc 1
O O1 0.1756(4) 0.86248(16) -0.11796(8) 0.0336(5) Uani d 1
H H1 0.040071 0.864208 -0.148893 0.040 Uiso calc 1
C C4 0.7178(5) 0.7604(2) 0.05356(11) 0.0222(5) Uani d 1
C C3 0.4724(5) 0.7576(2) -0.00322(11) 0.0210(5) Uani d 1
H H3A 0.369526 0.848453 -0.004435 0.025 Uiso calc 1
O O5 0.7592(4) 0.66840(17) 0.09308(8) 0.0333(5) Uani d 1
O O7 0.7301(3) 0.58394(16) 0.30079(8) 0.0257(4) Uani d 1
O O8 0.7081(4) 0.38071(16) 0.35161(8) 0.0335(5) Uani d 1
O O2 0.2879(4) 0.66485(15) -0.16354(8) 0.0270(4) Uani d 1
C C2 0.5781(5) 0.7450(2) -0.06464(10) 0.0194(5) Uani d 1
H H2 0.705425 0.825603 -0.067088 0.023 Uiso calc 1
C C5 0.6125(5) 0.4693(2) 0.30892(10) 0.0196(5) Uani d 1
C C1 0.3298(5) 0.7509(2) -0.12143(10) 0.0189(5) Uani d 1
C C6 0.3348(5) 0.4342(2) 0.26448(11) 0.0207(5) Uani d 1
H H6A 0.199123 0.407897 0.289680 0.025 Uiso calc 1
H H6B 0.361674 0.351299 0.239244 0.025 Uiso calc 1
N N1 0.3938(5) 0.58785(19) 0.17585(9) 0.0270(5) Uani d 1
H H1A 0.388979 0.516121 0.148282 0.041 Uiso calc 1
H H1B 0.571704 0.600681 0.197906 0.041 Uiso calc 1
H H1C 0.331693 0.667772 0.154604 0.041 Uiso calc 1
C C7 0.2104(5) 0.5531(2) 0.22002(10) 0.0224(5) Uani d 1
H H7A 0.023959 0.524863 0.195735 0.027 Uiso calc 1
H H7B 0.187477 0.637546 0.244688 0.027 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 0.0227(10) 0.0317(9) 0.0325(10) -0.0041(8) 0.0017(9) 0.0096(7)
O3 0.0154(8) 0.0244(8) 0.0294(10) 0.0047(7) -0.0005(8) -0.0022(7)
O6 0.0319(11) 0.0295(9) 0.0262(10) -0.0073(8) -0.0078(9) -0.0006(7)
O1 0.0345(11) 0.0344(9) 0.0245(10) 0.0160(9) -0.0091(8) -0.0066(7)
C4 0.0225(14) 0.0242(12) 0.0204(13) 0.0023(11) 0.0055(11) -0.0028(10)
C3 0.0189(13) 0.0205(11) 0.0225(13) 0.0005(10) 0.0023(11) 0.0010(10)
O5 0.0354(11) 0.0369(9) 0.0235(9) -0.0029(9) -0.0017(9) 0.0099(8)
O7 0.0200(9) 0.0253(8) 0.0277(9) -0.0071(7) -0.0036(8) 0.0020(7)
O8 0.0339(11) 0.0261(8) 0.0311(10) -0.0004(8) -0.0128(9) 0.0075(8)
O2 0.0276(10) 0.0260(8) 0.0238(9) 0.0021(8) -0.0017(8) -0.0067(7)
C2 0.0182(13) 0.0187(11) 0.0206(12) 0.0019(9) 0.0029(11) -0.0004(9)
C5 0.0184(12) 0.0208(11) 0.0193(12) 0.0035(10) 0.0032(11) -0.0031(9)
C1 0.0171(13) 0.0193(11) 0.0205(12) -0.0008(10) 0.0048(11) 0.0032(10)
C6 0.0198(12) 0.0198(11) 0.0212(12) -0.0034(10) 0.0023(10) 0.0015(9)
N1 0.0347(13) 0.0240(9) 0.0240(11) 0.0073(9) 0.0098(10) 0.0035(8)
C7 0.0191(12) 0.0252(12) 0.0211(13) 0.0007(10) 0.0009(11) 0.0007(10)
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 -2 0.0320
1 -1 2 0.0240
2 -2 -3 0.2270
-2 2 3 0.2800
4 3 -4 0.0100
-4 -3 4 0.0300
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 110.75(19)
O5 C4 O6 126.4(2)
O5 C4 C3 122.9(2)
O4 C3 C4 111.74(18)
O4 C3 H3A 108.0
O4 C3 C2 110.33(18)
C4 C3 H3A 108.0
C4 C3 C2 110.51(19)
C2 C3 H3A 108.0
O3 C2 C3 111.84(17)
O3 C2 H2 108.8
O3 C2 C1 108.58(17)
C3 C2 H2 108.8
C1 C2 C3 109.83(18)
C1 C2 H2 108.8
O7 C5 O8 124.8(2)
O7 C5 C6 118.09(19)
O8 C5 C6 117.12(19)
O1 C1 C2 110.23(18)
O2 C1 O1 125.8(2)
O2 C1 C2 124.0(2)
C5 C6 H6A 108.6
C5 C6 H6B 108.6
C5 C6 C7 114.68(18)
H6A C6 H6B 107.6
C7 C6 H6A 108.6
C7 C6 H6B 108.6
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 111.19(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 0.8300
O4 C3 1.414(3)
O3 H3 0.8300
O3 C2 1.419(2)
O6 H6 0.8300
O6 C4 1.307(3)
O1 H1 0.8300
O1 C1 1.306(3)
C4 C3 1.513(3)
C4 O5 1.205(3)
C3 H3A 0.9900
C3 C2 1.538(3)
O7 C5 1.255(3)
O8 C5 1.257(2)
O2 C1 1.205(3)
C2 H2 0.9900
C2 C1 1.523(3)
C5 C6 1.512(3)
C6 H6A 0.9800
C6 H6B 0.9800
C6 C7 1.515(3)
N1 H1A 0.9000
N1 H1B 0.9000
N1 H1C 0.9000
N1 C7 1.487(3)
C7 H7A 0.9800
C7 H7B 0.9800
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 0.83 2.19 2.872(2) 139.5 yes
O3 H3 O4 1_655 0.83 1.97 2.797(2) 177.6 yes
O6 H6 O8 2_755 0.83 1.75 2.571(2) 171.8 yes
O1 H1 O7 4_475 0.83 1.72 2.523(2) 160.6 yes
N1 H1B O7 . 0.90 2.20 2.838(2) 127.4 yes
N1 H1C O8 2_655 0.90 2.02 2.846(2) 152.1 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 -61.5(2)
O4 C3 C2 C1 59.1(2)
O3 C2 C1 O1 174.97(19)
O3 C2 C1 O2 -6.1(3)
O6 C4 C3 O4 -173.02(19)
O6 C4 C3 C2 63.7(2)
C4 C3 C2 O3 62.6(2)
C4 C3 C2 C1 -176.78(17)
C3 C2 C1 O1 52.4(2)
C3 C2 C1 O2 -128.7(2)
O5 C4 C3 O4 8.0(3)
O5 C4 C3 C2 -115.3(2)
O7 C5 C6 C7 -8.0(3)
O8 C5 C6 C7 171.9(2)
C5 C6 C7 N1 64.2(2)
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.7735(12)
2 0.2265(12)
_cod_database_fobs_code 2021500