#------------------------------------------------------------------------------
#$Date: 2024-10-25 04:56:58 +0300 (Fri, 25 Oct 2024) $
#$Revision: 295623 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/29/1572951.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1572951
loop_
_publ_author_name
'Mrad, Houda'
'Elboulali, Adel'
'Baptiste, Beno\^it'
'Akriche, Samah'
_journal_coeditor_code HB8111
_journal_paper_doi 10.1107/S2056989024010132
_journal_year 2024
_chemical_formula_iupac 'C6 H16 N2 2+, H2 O7 P2 2-'
_chemical_formula_moiety 'C6 H16 N2 2+, H2 O7 P2 2-'
_chemical_formula_structural 'P2 O7 H2, C6 H16 N2'
_chemical_formula_sum 'C6 H18 N2 O7 P2'
_chemical_formula_weight 292.16
_chemical_name_systematic
;
trans-2,5-Dimethylpiperazine-1,4-diium
dihydrogen diphosphate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-C 2yc'
_space_group_name_H-M_alt 'C 1 2/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2013
_cell_angle_alpha 90
_cell_angle_beta 91.422(4)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 10.2557(5)
_cell_length_b 8.3978(5)
_cell_length_c 13.7681(7)
_cell_measurement_reflns_used 2302
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 31.8280
_cell_measurement_theta_min 3.9640
_cell_volume 1185.42(11)
_computing_cell_refinement
;
CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material
;
WinGX publication routines (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.0318
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Xcalibur diffractometer with Sapphire3 CCD detector'
_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 0.0398
_diffrn_reflns_av_unetI/netI 0.0354
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 9376
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 33.136
_diffrn_reflns_theta_min 3.447
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.394
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.97921
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2019)
;
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.637
_exptl_crystal_description Needle
_exptl_crystal_F_000 616
_exptl_crystal_size_max 0.300
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_min 0.100
_refine_diff_density_max 0.585
_refine_diff_density_min -0.385
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 114
_refine_ls_number_reflns 2255
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.045
_refine_ls_R_factor_all 0.0601
_refine_ls_R_factor_gt 0.0405
_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^)+(0.0380P)^2^+1.0885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0904
_refine_ls_wR_factor_ref 0.1034
_reflns_number_gt 1738
_reflns_number_total 2255
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb8111.cif
_cod_data_source_block I
_cod_original_sg_symbol_H-M 'C 2/c'
_cod_database_code 1572951
_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 0.891
_shelx_estimated_absorpt_t_max 0.962
_shelx_hkl_file
;
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0 0 -3 127.629 123.758 4
0 0 -4 824711. 3270.31 1
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0 0 -5 58.2888 57.2806 1
0 0 5 90.9707 169.043 7
0 0 -5-99.1072 152.376 4
0 0 -6 321491. 2421.59 1
0 0 6 311817. 4324.90 7
0 0 -6 316468. 4528.11 4
0 0 7-12.0157 172.243 7
0 0 -7 187.927 217.527 4
0 0 -7 126.860 76.2776 1
0 0 8 268072. 4685.52 7
0 0 -8 266960. 4874.49 4
0 0 -8 269081. 2478.32 1
0 0 9 10.1538 252.165 7
0 0 -9-85.4502 295.979 4
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0 0 -10 502.285 301.426 4
0 0 -10 486.228 111.346 1
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0 0 11-522.362 381.003 7
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0 0 -12 1504.03 576.290 4
0 0 -13-27.8747 331.814 2
0 0 -13 253.579 507.341 4
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0 0 -14 18076.3 1831.05 2
0 0 14 16740.0 1676.81 7
0 0 -14 18570.1 1809.45 4
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0 0 -15-198.868 349.181 2
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0 0 -16 627.752 409.638 4
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0 0 -18 1208.72 680.414 4
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0 0 -19-641.584 588.198 2
0 0 -19-61.6443 500.870 4
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0 0 -20 23148.3 2623.06 2
0 0 -20 21770.6 2510.30 4
0 0 -21 363.365 414.197 2
0 0 21 435.988 416.922 7
0 0 -21 1248.56 718.024 4
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0 -2 0 433931. 3713.22 5
0 -2 -1 301027. 3243.30 4
0 -2 1 310097. 3388.67 5
0 -2 -1 312147. 3026.74 5
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0 -2 -2 315676. 2323.70 2
0 -2 2 302091. 3608.20 5
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0 -2 -4 26460.5 1235.54 4
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0 2 5 118002. 2825.67 3
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0 -2 5 114810. 2713.82 7
0 -2 -6 209493. 4018.95 4
0 -2 6 208022. 3930.66 7
0 2 6 203241. 3985.42 3
0 2 6 208123. 3451.29 7
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0 2 -7 161.910 217.270 4
0 2 7 390.447 219.473 7
0 -2 -7-32.2167 254.154 4
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0 -2 -10 19749.8 1516.81 2
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14 -2 -3 1596.88 698.252 5
-14 2 3 1269.77 630.340 1
14 -2 -3 250.782 510.395 2
14 2 -3 1164.00 656.984 2
-14 -2 3 1403.93 685.420 1
14 -2 -2 5316.67 1235.96 5
-14 2 2 5409.20 1196.77 1
14 -2 -2 5562.23 1394.67 2
14 2 -2 8728.11 1632.19 2
-14 -2 2 4535.31 1111.61 1
14 -2 -1 1615.22 701.569 5
14 2 -1 1236.69 678.136 2
-14 2 1 1968.61 869.054 1
-14 -2 1 944.009 547.782 1
-14 -2 0 4112.17 1088.80 1
-14 2 0 5966.56 1293.03 1
-14 -2 -1 243.228 413.541 1
-14 2 -1 136.960 393.721 1
-14 -2 -2 1204.78 652.883 1
-14 2 -2 896.019 531.882 1
-14 -2 -3 1981.09 807.325 1
-14 2 -3 1687.72 832.779 1
-14 -2 -4 11773.2 1848.52 1
-14 2 -4 7700.13 1592.61 1
-14 -2 -5 5367.78 1269.51 1
-14 2 -5 6190.92 1401.96 1
-14 -2 -6 4383.71 1168.76 1
-14 2 -6 6522.53 1437.39 1
-14 -2 -7 1133.61 675.235 1
-14 2 -7 2000.43 931.424 1
-14 -2 -8 4302.40 1171.53 1
-14 2 -8 1895.21 830.191 1
14 -4 -7 727.129 590.568 5
14 -4 -7 1219.38 723.503 2
14 4 -7-778.314 713.090 2
14 -4 -6 196.986 409.123 5
14 -4 -6-44.0639 339.995 2
14 4 -6 48.8641 391.100 2
14 -4 -5 5731.56 1375.73 5
-14 4 5 3538.16 931.812 1
14 -4 -5 5386.99 1342.56 2
14 4 -5 4438.18 1292.96 2
14 -4 -4 4921.05 1307.39 5
-14 4 4 7910.94 1466.95 1
14 -4 -4 4986.11 1275.80 2
14 4 -4 7053.90 1483.54 2
14 -4 -3 2549.02 925.278 5
-14 -4 3 1527.61 720.569 1
14 -4 -3 1514.50 817.183 2
-14 4 3 796.915 611.861 1
14 4 -3 2298.55 906.009 2
14 -4 -2-229.653 404.675 5
14 4 -2 33.7122 350.214 2
-14 4 2 249.204 414.295 1
-14 -4 2 225.266 425.724 1
14 -4 -1 1831.92 797.433 5
-14 4 1 4513.63 1128.90 1
-14 -4 1 2850.36 982.213 1
14 -4 0 979.021 609.388 5
-14 -4 0 154.451 382.571 1
14 -4 1 1179.31 614.193 5
-14 -4 -1 43.5779 318.812 1
14 -4 2 184.182 413.319 5
-14 4 -2-660.772 523.157 1
-14 -4 -2-136.774 503.101 1
-14 -4 -2 505.428 492.059 6
-14 4 -3 7883.12 1559.82 1
-14 -4 -3 6202.25 1405.76 1
-14 -4 -3 5386.48 1271.41 6
-14 -4 -4 992.518 565.770 6
-14 4 -4 988.159 634.577 1
-14 -4 -4 227.105 479.684 1
-14 -4 -5 2662.76 943.993 6
-14 4 -5 5715.23 1366.45 1
-14 -4 -5 6445.08 1395.06 1
-14 -4 -6 918.035 696.606 6
-14 4 -6-91.9232 274.903 1
-14 -4 -6 902.562 585.865 1
-15 1 6 581.102 389.015 1
15 -1 -6 1440.19 727.951 2
15 1 -6 368.945 485.449 2
-15 -1 6-860.586 598.444 1
-15 1 6 33.6847 344.943 7
-15 1 5 6637.98 1319.65 1
15 -1 -5 5916.71 1459.08 2
15 1 -5 5600.63 1426.98 2
-15 -1 5 5420.22 1223.97 1
-15 1 4 1542.14 672.658 1
15 -1 -4 1933.99 864.290 2
15 1 -4 1440.99 755.729 2
-15 -1 3 4076.72 1156.80 1
-15 1 3 5280.25 1229.97 1
15 -1 -3 5169.28 1332.66 2
15 1 -3 5497.56 1439.68 2
-15 -1 2 181.955 367.266 1
-15 1 2 143.824 331.477 1
15 -1 -2 701.085 535.667 2
15 1 -2 287.670 570.791 2
-15 -1 1-602.787 507.096 1
-15 1 1-250.457 344.817 1
-15 -1 0-156.231 422.874 1
-15 1 0-621.521 558.323 1
-15 -1 -1 3659.43 1022.39 1
-15 1 -1 5004.51 1233.91 1
-15 -1 -2 1874.56 793.874 1
-15 1 -2 2832.12 950.031 1
-15 -1 -3 4139.15 1227.13 1
-15 1 -3 3938.75 1187.90 1
-15 -1 -4 974.589 559.131 1
-15 1 -4-1364.96 731.347 1
-15 -1 -5-546.559 480.804 1
-15 1 -5-202.510 437.762 1
15 -3 -4 4648.14 1213.90 5
-15 3 4 3485.29 965.931 1
15 -3 -4 5418.28 1432.28 2
15 3 -4 4359.30 1263.98 2
-15 -3 4 5438.77 1271.25 1
15 -3 -3 522.411 501.604 5
15 -3 -3 694.939 673.499 2
-15 3 3 1105.34 644.427 1
15 3 -3 830.325 604.422 2
-15 -3 3 1917.47 735.919 1
15 -3 -2 836.331 657.790 5
-15 3 2 254.684 352.138 1
-15 -3 2 394.990 442.316 1
15 -3 -1 968.509 773.984 5
-15 3 1 237.274 593.859 1
-15 -3 1 109.217 351.947 1
-15 3 0-781.622 490.711 1
-15 -3 0 196.517 462.609 1
-15 3 -1-382.123 466.382 1
-15 -3 -1 234.738 405.662 1
-15 3 -2 975.954 633.483 1
-15 -3 -2 3209.62 1046.73 1
-15 3 -3 14.9785 272.374 1
-15 -3 -3 317.022 343.614 1
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 24238
_shelx_res_file
;
TITL SIR92 run in space group C 2/c
CELL 0.71073 10.2557 8.3978 13.7681 90.000 91.422 90.000
ZERR 4.00 0.0005 0.0005 0.0007 0.000 0.004 0.000
LATT 7
SYMM - X, Y, 1/2 - Z
SFAC C H N O P
UNIT 24 72 8 28 8
MERG 2
EQIV $1 -x+3/2, y-1/2, -z+1/2
HTAB O1 O3_$1
EQIV $2 -x+3/2, -y+1/2, -z+1
HTAB N1 O2_$2
HTAB N1 O2
EQIV $3 x, -y+1, z+1/2
HTAB C1 O3_$3
EQIV $4 -x+3/2, y+1/2, -z+1/2
HTAB C1 O1_$4
EQIV $5 -x+1, y, -z+1/2
HTAB C2 O3_$5
HTAB O1 O3_$1
HTAB N1 O2_$2
HTAB N1 O2
HTAB C1 O3_$3
HTAB C1 O1_$4
HTAB C2 O3_$5
FMAP 2
PLAN 25
SIZE 0.100 0.200 0.300
ACTA
BOND
L.S. 10
TEMP 20.00
WGHT 0.038000 1.088500
FVAR 6.04965
MOLE 1
P1 5 0.641967 0.211840 0.267666 11.00000 0.02956 0.02871 =
0.01809 0.00137 -0.00450 0.00277
O1 4 0.727412 0.097370 0.209501 11.00000 0.07919 0.06857 =
0.02907 -0.00045 0.01483 0.03339
O2 4 0.672848 0.203282 0.373976 11.00000 0.03231 0.03441 =
0.01894 -0.00123 -0.00548 0.00732
O3 4 0.646285 0.373001 0.222181 11.00000 0.05555 0.03867 =
0.04001 0.01689 -0.00996 -0.00634
O4 4 0.500000 0.140228 0.250000 10.50000 0.04145 0.02436 =
0.08230 0.00000 -0.03469 0.00000
H1 2 0.757071 0.011943 0.240274 11.00000 0.08378
MOLE 2
N1 3 0.613784 0.408352 0.522679 11.00000 0.02246 0.02793 =
0.02097 0.00102 -0.00250 0.00531
C1 1 0.624513 0.577432 0.492452 11.00000 0.02330 0.02765 =
0.02334 0.00082 -0.00087 -0.00220
C2 1 0.511065 0.626714 0.426707 11.00000 0.02522 0.02596 =
0.02060 0.00308 -0.00057 0.00186
C3 1 0.517442 0.801791 0.402124 11.00000 0.04789 0.03026 =
0.05476 0.01436 0.00288 0.00157
H1A 2 0.682600 0.385419 0.562485 11.00000 0.04190
H1B 2 0.621945 0.344916 0.470674 11.00000 0.03902
H1C 2 0.625859 0.642239 0.551826 11.00000 0.02824
H1D 2 0.704193 0.587979 0.456542 11.00000 0.03151
H2 2 0.509510 0.558992 0.366821 11.00000 0.03918
H3A 2 0.516342 0.862126 0.460378 11.00000 0.08424
H3B 2 0.441677 0.833260 0.359371 11.00000 0.06394
H3C 2 0.602696 0.816873 0.369382 11.00000 0.06082
HKLF 4
REM SIR92 run in space group C 2/c
REM R1 = 0.0405 for 1738 Fo > 4sig(Fo) and 0.0601 for all 2255 data
REM 114 parameters refined using 0 restraints
END
WGHT 0.0360 1.0665
REM Highest difference peak 0.585, deepest hole -0.385, 1-sigma level 0.065
Q1 1 0.4832 0.1794 0.2865 11.00000 0.05 0.58
Q2 1 0.5000 0.0954 0.2500 10.50000 0.05 0.30
Q3 1 0.6639 0.2228 0.3199 11.00000 0.05 0.27
Q4 1 0.5644 0.5960 0.4618 11.00000 0.05 0.27
Q5 1 0.5170 0.7129 0.4227 11.00000 0.05 0.27
Q6 1 0.6618 0.1097 0.2163 11.00000 0.05 0.27
Q7 1 0.6191 0.4948 0.5061 11.00000 0.05 0.27
Q8 1 0.6408 0.3694 0.2694 11.00000 0.05 0.25
Q9 1 0.6771 0.0402 0.2274 11.00000 0.05 0.24
Q10 1 0.7623 0.1522 0.2381 11.00000 0.05 0.23
Q11 1 0.6771 0.6074 0.4863 11.00000 0.05 0.22
Q12 1 0.6808 0.3151 0.2187 11.00000 0.05 0.22
Q13 1 0.7393 0.1626 0.2236 11.00000 0.05 0.21
Q14 1 0.6017 0.2054 0.3747 11.00000 0.05 0.20
Q15 1 0.6931 0.1583 0.3211 11.00000 0.05 0.20
Q16 1 0.6806 0.4343 0.2524 11.00000 0.05 0.20
Q17 1 0.4901 0.8413 0.3221 11.00000 0.05 0.20
Q18 1 0.6605 0.3202 0.2614 11.00000 0.05 0.20
Q19 1 0.6798 0.1293 0.2389 11.00000 0.05 0.19
Q20 1 0.7810 0.0946 0.2373 11.00000 0.05 0.19
Q21 1 0.5667 0.4051 0.5531 11.00000 0.05 0.18
Q22 1 0.5670 0.8879 0.5698 11.00000 0.05 0.18
Q23 1 0.4206 0.8618 0.3961 11.00000 0.05 0.18
Q24 1 0.5152 0.4569 0.3127 11.00000 0.05 0.18
Q25 1 0.8045 0.2798 0.2832 11.00000 0.05 0.18
;
_shelx_res_checksum 28259
_shelxl_version_number .2013
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
P P1 0.64197(4) 0.21184(5) 0.26767(3) 0.02554(12) Uani d 1 . .
O O1 0.72741(18) 0.0974(2) 0.20950(10) 0.0587(5) Uani d 1 . .
O O2 0.67285(11) 0.20328(14) 0.37398(7) 0.0287(2) Uani d 1 . .
O O3 0.64629(15) 0.37300(17) 0.22218(10) 0.0449(3) Uani d 1 . .
O O4 0.5000 0.1402(2) 0.2500 0.0500(6) Uani d 1 . .
H H1 0.757(3) 0.012(4) 0.240(2) 0.084(10) Uiso d 1 . .
N N1 0.61378(12) 0.40835(16) 0.52268(9) 0.0238(3) Uani d 1 . .
C C1 0.62451(15) 0.57743(19) 0.49245(11) 0.0248(3) Uani d 1 . .
C C2 0.51107(15) 0.62671(18) 0.42671(10) 0.0239(3) Uani d 1 . .
C C3 0.5174(2) 0.8018(2) 0.40212(19) 0.0443(5) Uani d 1 . .
H H1A 0.683(2) 0.385(3) 0.5625(16) 0.042(6) Uiso d 1 . .
H H1B 0.622(2) 0.345(3) 0.4707(16) 0.039(6) Uiso d 1 . .
H H1C 0.6259(18) 0.642(2) 0.5518(14) 0.028(5) Uiso d 1 . .
H H1D 0.7042(19) 0.588(2) 0.4565(14) 0.032(5) Uiso d 1 . .
H H2 0.510(2) 0.559(3) 0.3668(15) 0.039(5) Uiso d 1 . .
H H3A 0.516(3) 0.862(4) 0.460(2) 0.084(10) Uiso d 1 . .
H H3B 0.442(3) 0.833(3) 0.359(2) 0.064(8) Uiso d 1 . .
H H3C 0.603(3) 0.817(3) 0.3694(19) 0.061(7) 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
P1 0.0296(2) 0.0287(2) 0.01809(17) 0.00277(15) -0.00450(13) 0.00137(14)
O1 0.0792(12) 0.0686(11) 0.0291(7) 0.0334(9) 0.0148(7) -0.0004(7)
O2 0.0323(6) 0.0344(6) 0.0189(5) 0.0073(5) -0.0055(4) -0.0012(4)
O3 0.0556(9) 0.0387(7) 0.0400(7) -0.0063(6) -0.0100(6) 0.0169(6)
O4 0.0415(11) 0.0244(9) 0.0823(15) 0.000 -0.0347(10) 0.000
N1 0.0225(6) 0.0279(6) 0.0210(5) 0.0053(5) -0.0025(4) 0.0010(5)
C1 0.0233(6) 0.0276(7) 0.0233(6) -0.0022(5) -0.0009(5) 0.0008(5)
C2 0.0252(7) 0.0260(7) 0.0206(6) 0.0019(5) -0.0006(5) 0.0031(5)
C3 0.0479(11) 0.0303(9) 0.0548(12) 0.0016(8) 0.0029(10) 0.0144(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'
P P 0.1023 0.0942 '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
O2 P1 O3 . . 116.60(8) ?
O2 P1 O1 . . 111.76(8) ?
O3 P1 O1 . . 108.96(9) ?
O2 P1 O4 . . 107.67(5) ?
O3 P1 O4 . . 108.40(8) ?
O1 P1 O4 . . 102.44(9) ?
P1 O4 P1 . 2_655 135.50(12) ?
C1 N1 C2 . 5_666 112.80(12) ?
N1 C1 C2 . . 111.58(12) ?
N1 C2 C3 5_666 . 109.69(14) ?
N1 C2 C1 5_666 . 108.68(11) ?
C3 C2 C1 . . 111.29(15) ?
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
P1 O2 . 1.4916(11) ?
P1 O3 . 1.4924(14) ?
P1 O1 . 1.5389(15) ?
P1 O4 . 1.5884(8) ?
O4 P1 2_655 1.5884(8) ?
N1 C1 . 1.484(2) ?
N1 C2 5_666 1.5020(19) ?
C1 C2 . 1.514(2) ?
C2 N1 5_666 1.5020(19) ?
C2 C3 . 1.510(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
O1 H1 O3 4_645 0.88(3) 1.61(3) 2.460(2) 161(3)
N1 H1A O2 7_656 0.90(2) 1.86(2) 2.7454(17) 167(2)
N1 H1B O2 . 0.90(2) 1.87(2) 2.7543(17) 168(2)
C1 H1C O3 6_566 0.982(19) 2.353(19) 3.193(2) 143.0(15)
C1 H1D O1 4_655 0.970(19) 2.41(2) 3.205(2) 139.1(15)
C2 H2 O3 2_655 1.00(2) 2.53(2) 3.344(2) 138.3(15)