#------------------------------------------------------------------------------
#$Date: 2023-04-05 14:17:41 +0300 (Wed, 05 Apr 2023) $
#$Revision: 282401 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/27/2022718.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_2022718
loop_
_publ_author_name
'Archana, Sreeramapura D.'
'Foro, Sabine'
'Yathirajan, Hemmige S.'
'Kiran Kumar, Haruvegowda'
'Balerao, Rishik'
'Butcher, Ray J.'
_publ_section_title
;
Syntheses, crystal structures and Hirshfeld surface analysis of three
salts of 1-(4-nitrophenyl)piperazine
;
_journal_issue 4
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first 373
_journal_page_last 379
_journal_paper_doi 10.1107/S2056989023002517
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac '2C10 H14 N3 O2 +, 2C7 H4 F O2 -, 3H2 O'
_chemical_formula_moiety '2(C10 H14 N3 O2 +), 2(C7 H4 F O2 -), 3(H2 O)'
_chemical_formula_sum 'C34 H42 F2 N6 O11'
_chemical_formula_weight 748.73
_chemical_name_systematic
;
Bis[4-(4-nitrophenyl)piperazin-1-ium] bis(4-fluorobenzoate) trihydrate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 104.170(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 16.882(2)
_cell_length_b 9.7190(10)
_cell_length_c 23.445(4)
_cell_measurement_reflns_used 3000
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 27.92
_cell_measurement_theta_min 2.66
_cell_volume 3729.7(9)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur with Sapphire CCD
;
_diffrn_measurement_method
;
Rotation method data acquisition using \w scans.
;
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0633
_diffrn_reflns_av_unetI/netI 0.1176
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_number 14552
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.346
_diffrn_reflns_theta_min 2.671
_diffrn_source 'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 0.107
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.88736
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2009)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.333
_exptl_crystal_description prism
_exptl_crystal_F_000 1576
_exptl_crystal_size_max 0.320
_exptl_crystal_size_mid 0.160
_exptl_crystal_size_min 0.140
_refine_diff_density_max 0.192
_refine_diff_density_min -0.177
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.057
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 508
_refine_ls_number_reflns 6755
_refine_ls_number_restraints 10
_refine_ls_restrained_S_all 1.057
_refine_ls_R_factor_all 0.2405
_refine_ls_R_factor_gt 0.0891
_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^)+(0.0366P)^2^+1.3296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1181
_refine_ls_wR_factor_ref 0.1536
_reflns_number_gt 2429
_reflns_number_total 6755
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file vm2276sup1.cif
_cod_data_source_block 2
_cod_original_sg_symbol_H-M 'P 21/n'
_cod_database_code 2022718
_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 0.967
_shelx_estimated_absorpt_t_max 0.985
_shelx_hkl_file
;
0 0 4 19.47 4.05 3
0 0 5 -0.27 4.36 3
0 0 6 5088.83 24.29 3
0 0 7 8.97 5.51 3
0 0 8 6888.29 32.67 3
0 0 9 20.11 6.09 3
0 0 10 233.60 8.61 3
0 0 11 0.68 5.87 3
0 0 12 456.71 12.36 3
0 0 13 -3.38 6.42 3
0 0 14 1372.12 21.07 3
0 0 15 27.24 6.85 3
0 0 16 -3.99 8.04 3
0 0 17 -1.80 7.24 3
0 0 18 10.98 7.75 3
0 0 19 -7.56 8.29 3
0 0 20 114.52 11.50 3
0 0 21 14.21 8.40 3
0 0 22 228.52 13.85 3
0 0 23 -2.53 10.39 3
0 0 26 -10.09 13.59 3
0 0 27 -10.39 12.18 3
0 0 28 -9.39 14.63 3
0 1 3 396.56 6.58 3
0 -1 -4 75.24 2.52 0
0 -1 4 72.76 4.29 4
0 1 4 73.07 5.10 3
0 1 5 2318.42 16.38 3
0 -1 5 2368.75 14.46 4
0 -1 -5 2379.29 9.48 0
0 1 613647.60 24.70 0
0 -1 613694.60 36.64 4
0 1 613652.10 41.08 3
0 1 7 1426.87 9.30 0
0 1 7 1450.94 15.33 3
0 1 8 714.46 7.42 0
0 1 8 712.66 12.34 3
0 1 9 57.75 3.87 0
0 1 9 52.47 6.71 3
0 1 10 52.89 7.00 3
0 1 10 63.96 4.11 0
0 1 11 17.42 6.91 3
0 1 11 21.27 4.08 0
0 1 12 219.36 10.40 3
0 1 12 223.63 6.24 0
0 1 13 562.86 9.14 0
0 -1 13 632.18 14.25 3
0 1 13 583.33 14.41 3
0 1 14 298.69 12.21 3
0 1 14 307.46 7.62 0
0 -1 14 347.70 12.04 3
0 1 15 47.16 8.84 3
0 -1 15 51.30 8.52 3
0 1 16 82.93 10.45 3
0 -1 16 80.32 8.56 3
0 1 17 20.40 9.16 3
0 -1 17 18.68 8.38 3
0 -1 18 -1.71 8.23 3
0 1 18 -9.34 9.42 3
0 -1 19 56.20 9.81 3
0 1 19 45.93 11.45 3
0 -1 20 58.79 10.58 3
0 1 20 48.41 11.16 3
0 -1 21 12.22 9.10 3
0 1 21 11.87 11.07 3
0 -1 22 -5.92 10.10 3
0 1 22 6.89 9.96 3
0 1 23 4.66 11.67 3
0 -1 23 -8.48 8.37 3
0 1 24 -11.26 11.82 3
0 -1 24 -8.19 8.75 3
0 -1 25 -0.90 9.43 3
0 1 25 0.80 10.79 3
0 1 26 1.61 10.46 3
0 1 27 5.57 11.96 3
0 -1 27 11.58 10.86 3
0 1 28 12.44 15.18 3
0 -1 28 -4.03 12.50 3
0 2 018941.30 156.24 2
0 2 019218.10 144.76 1
0 -2 -115297.50 30.60 5
0 2 -115344.30 31.55 1
0 2 115135.80 138.52 1
0 2 -115161.40 140.13 2
0 2 115377.20 35.85 2
0 -2 -2 5526.19 20.43 5
0 2 2 5433.26 22.85 1
0 2 2 5471.02 22.38 3
0 2 -2 5437.36 22.34 2
0 -2 -3 98.26 5.05 5
0 2 3 88.60 5.74 3
0 -2 4 8.50 3.39 4
0 2 4 9.64 5.44 3
0 -2 5 1155.15 10.27 4
0 2 5 1138.62 13.05 3
0 -2 6 1336.61 11.91 4
0 2 6 1336.66 14.63 3
0 -2 -7 387.33 5.12 0
0 -2 7 390.30 8.04 4
0 2 7 381.79 9.92 3
0 -2 8 159.44 6.54 4
0 2 8 170.34 8.25 3
0 -2 -8 164.40 3.96 0
0 2 9 21.78 6.87 3
0 2 10 41.48 7.60 3
0 2 11 49.21 7.71 3
0 2 12 54.54 8.17 3
0 2 13 161.34 10.32 3
0 2 14 201.65 11.29 3
0 2 15 4.11 8.09 3
0 2 16 16.08 9.53 3
0 2 17 68.01 10.37 3
0 -2 18 37.10 9.31 3
0 2 18 37.30 10.13 3
0 -2 19 58.17 10.07 3
0 2 19 58.66 11.76 3
0 -2 20 61.45 10.80 3
0 2 20 51.51 11.40 3
0 2 21 100.24 13.05 3
0 -2 21 75.17 11.07 3
0 -2 22 28.06 9.68 3
0 2 22 25.14 11.57 3
0 2 23 5.27 10.56 3
0 -2 23 -27.89 10.01 3
0 -2 24 -10.13 9.31 3
0 2 24 3.27 11.98 3
0 -2 25 -17.46 9.51 3
0 2 25 27.08 12.04 3
0 -2 26 -13.92 10.54 3
0 2 26 -1.95 12.28 3
0 -2 27 -7.34 12.13 3
0 2 27 -19.40 13.49 3
0 2 28 21.02 14.21 3
0 -2 28 -20.19 12.56 3
0 3 0 -0.87 4.84 2
0 3 0 -2.14 5.14 1
0 3 1 5845.95 27.30 2
0 3 1 5931.60 26.27 1
0 -3 -1 5887.97 19.43 4
0 3 -1 5861.53 24.56 1
0 -3 -1 5783.09 23.06 5
0 3 -1 5814.04 27.08 2
0 -3 -2 176.32 6.09 5
0 -3 -2 172.40 5.43 4
0 3 2 181.45 7.08 1
0 3 2 174.16 6.86 2
0 3 -2 187.46 6.65 2
0 -3 -3 356.59 7.65 5
0 -3 3 334.35 5.14 4
0 3 3 361.98 8.88 1
0 3 -3 362.42 8.43 2
0 3 4 159.37 7.73 1
0 3 4 146.56 7.64 3
0 -3 4 143.69 4.31 4
0 -3 -4 162.13 6.45 5
0 3 5 243.15 8.65 3
0 -3 5 244.35 5.61 4
0 3 6 20.68 6.37 3
0 -3 6 22.70 4.17 4
0 -3 7 237.71 6.67 4
0 3 7 252.39 9.51 3
0 -3 8 258.35 7.21 4
0 3 8 277.83 10.05 3
0 -3 9 88.96 5.79 4
0 -3 -9 87.94 3.65 0
0 3 9 102.88 8.29 3
0 -3 -10 34.69 3.12 0
0 3 10 53.40 7.63 3
0 3 11 137.10 9.30 3
0 3 12 12.29 8.18 3
0 3 13 52.10 9.01 3
0 3 14 5.39 8.38 3
0 3 15 51.41 9.31 3
0 3 16 12.34 9.37 3
0 3 17 9.82 8.98 3
0 3 18 52.54 10.50 3
0 3 19 26.51 11.13 3
0 3 20 9.89 11.70 3
0 3 21 10.41 10.45 3
0 -3 21 5.98 7.28 3
0 -3 22 7.37 9.29 3
0 3 22 12.56 11.08 3
0 3 23 9.38 10.25 3
0 -3 23 7.85 9.24 3
0 -3 24 -4.54 9.39 3
0 3 24 16.47 11.21 3
0 -3 25 -10.96 9.93 3
0 3 25 5.18 13.41 3
0 -3 26 2.42 11.54 3
0 3 26 5.72 12.05 3
0 3 27 42.81 13.83 3
0 -3 27 31.83 12.33 3
0 4 0 17.17 5.36 1
0 4 0 8.61 5.80 2
0 -4 0 14.49 3.98 4
0 -4 -1 0.26 4.11 5
0 4 -1 5.60 5.21 1
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0 -4 1 6.27 3.48 4
0 -4 -1 12.38 3.64 4
0 4 -1 2.62 4.87 2
0 4 -2 401.65 9.50 2
0 4 2 387.95 10.03 2
0 -4 -2 409.67 8.40 5
0 -4 2 386.15 5.91 4
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0 4 3 839.72 13.56 2
0 -4 -3 900.92 10.80 4
0 4 -3 900.09 13.33 2
0 -4 -3 905.93 12.12 5
0 -4 3 874.22 8.17 4
0 4 3 940.24 14.04 1
0 4 4 7.93 6.27 1
0 4 -4 7.96 5.13 2
0 -4 -4 15.91 5.05 5
0 -4 4 7.33 3.20 4
0 -4 5 413.76 6.62 4
0 4 5 398.34 10.99 3
0 4 5 430.76 11.56 1
0 -4 6 75.05 4.62 4
0 4 6 75.32 7.71 1
0 4 6 75.44 8.30 3
0 4 7 66.95 8.04 3
0 -4 7 80.81 5.10 4
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0 -4 8 45.82 4.72 4
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0 -4 9 22.50 4.60 4
0 -4 10 22.26 4.91 4
0 4 10 51.41 8.63 3
0 4 11 4.23 8.55 3
0 4 12 21.59 9.06 3
0 4 13 7.47 7.37 3
0 4 14 45.54 10.22 3
0 4 15 7.98 9.33 3
0 4 16 31.66 9.83 3
0 4 17 134.14 12.30 3
0 4 18 30.29 10.19 3
0 4 19 32.82 11.11 3
0 4 20 44.17 11.08 3
0 4 21 39.76 11.41 3
0 4 22 8.67 12.14 3
0 -4 23 49.26 10.42 3
0 4 23 0.00 12.28 3
0 -4 24 30.21 10.03 3
0 4 24 22.56 12.75 3
0 4 25 26.05 12.03 3
0 -4 25 -8.89 10.97 3
0 -4 26 20.65 11.61 3
0 4 26 27.17 12.29 3
0 5 0 -6.24 6.23 2
0 5 0 -4.48 6.11 1
0 -5 0 -1.97 4.32 4
0 5 -1 1450.08 18.35 2
0 5 1 1498.35 17.66 1
0 5 1 1498.56 18.81 2
0 -5 -1 1441.81 12.51 4
0 -5 -1 1498.93 15.07 5
0 5 -1 1496.42 16.85 1
0 -5 1 1411.36 10.95 4
0 -5 2 104.87 4.80 4
0 -5 -2 131.65 5.33 4
0 5 -2 130.22 7.62 2
0 5 2 106.68 8.27 1
0 -5 -2 117.25 6.19 5
0 5 2 132.21 8.36 2
0 5 3 46.44 7.09 1
0 -5 3 37.11 3.60 4
0 -5 -3 43.72 5.25 5
0 5 3 46.02 7.31 2
0 -5 -3 40.19 4.94 4
0 5 -3 35.11 6.36 2
0 -5 4 95.07 4.02 4
0 -5 -4 114.25 6.14 4
0 -5 -4 118.11 6.54 5
0 5 4 114.91 8.38 2
0 5 -4 113.96 7.60 2
0 5 4 118.93 8.30 1
0 5 -5 17.67 5.58 2
0 -5 5 9.94 3.27 4
0 -5 -5 24.37 5.26 5
0 5 5 20.83 7.09 1
0 5 5 14.33 6.54 2
0 5 6 67.82 7.87 1
0 -5 6 62.04 4.26 4
0 5 7 9.96 7.87 3
0 -5 7 14.20 4.04 4
0 5 7 16.70 7.50 1
0 5 8 -1.34 7.34 1
0 -5 8 -1.25 3.75 4
0 5 8 -0.37 7.70 3
0 5 9 0.49 8.20 3
0 -5 9 -3.08 4.11 4
0 -5 10 1.08 4.55 4
0 5 10 -0.99 8.70 3
0 5 11 6.69 9.18 3
0 5 12 13.19 8.98 3
0 5 13 7.32 10.02 3
0 5 14 -2.21 10.56 3
0 5 15 2.14 10.51 3
0 5 16 1.02 10.81 3
0 5 17 17.64 11.33 3
0 5 18 7.79 11.55 3
0 5 19 5.13 12.33 3
0 5 20 28.76 13.53 3
0 5 21 0.52 13.12 3
0 5 22 20.30 14.57 3
0 5 23 9.64 13.80 3
0 5 24 -2.26 14.30 3
0 5 25 42.50 16.71 3
0 5 26 8.07 15.95 3
0 -5 26 7.12 13.59 3
0 6 0 12.78 7.22 1
0 6 0 1.08 6.91 2
0 -6 0 15.92 5.03 5
0 -6 -1 195.43 7.03 5
0 6 1 184.88 9.39 1
0 6 -1 191.41 9.26 2
0 6 -1 183.63 9.05 1
0 6 1 197.13 9.95 2
0 6 2 6.47 6.89 1
0 -6 -2 3.85 5.01 5
0 6 -2 4.18 6.03 2
0 6 2 8.76 7.27 2
0 -6 -3 462.16 10.45 5
0 6 3 444.81 13.10 1
0 6 -3 454.50 12.72 2
0 -6 -3 459.08 8.86 4
0 6 3 468.79 13.42 2
0 -6 -4 270.26 8.00 4
0 6 -4 275.18 10.69 2
0 6 4 278.85 11.57 1
0 -6 -4 288.43 8.72 5
0 6 4 285.65 11.52 2
0 -6 -5 5.13 5.23 4
0 6 5 0.32 7.47 2
0 6 -5 2.98 6.03 2
0 -6 -5 15.21 4.81 5
0 6 5 11.95 6.98 1
0 6 6 49.27 8.30 1
0 -6 -6 47.68 6.27 4
0 6 6 54.96 8.25 2
0 6 7 35.90 8.23 1
0 6 8 11.24 8.38 1
0 6 9 7.06 8.49 1
0 6 10 8.74 8.69 1
0 6 10 9.61 9.48 3
0 6 11 37.91 10.14 3
0 6 11 41.11 10.49 1
0 6 12 -4.22 9.81 3
0 6 12 8.60 9.02 1
0 6 13 -2.44 10.16 3
0 6 14 34.82 11.46 3
0 6 15 5.25 11.24 3
0 6 16 5.20 10.65 3
0 6 17 7.15 11.85 3
0 6 18 -3.36 12.24 3
0 6 19 10.62 11.96 3
0 6 20 3.01 13.98 3
0 6 21 3.71 13.32 3
0 6 22 -5.83 13.11 3
0 6 23 1.30 13.66 3
0 6 24 1.96 11.26 3
0 7 0 4.66 6.91 1
0 7 0 -0.77 6.64 2
0 7 -1 5.60 6.62 2
0 7 1 16.21 7.27 1
0 7 1 -1.02 7.24 2
0 7 2 2.37 7.53 2
0 7 2 -0.67 7.24 1
0 7 -2 -1.78 6.46 2
0 7 -3 8.49 6.98 2
0 -7 -3 9.06 5.12 5
0 7 3 2.93 7.50 2
0 7 3 7.12 7.65 1
0 7 4 48.80 9.02 1
0 7 4 61.02 8.92 2
0 7 -4 50.16 6.02 2
0 -7 -4 58.75 6.35 5
0 7 -5 224.13 8.92 2
0 7 5 257.66 12.07 1
0 7 5 233.37 12.25 2
0 7 6 31.97 8.90 2
0 7 -6 31.33 7.74 2
0 7 6 40.31 7.98 1
0 7 7 10.28 8.82 2
0 7 7 5.04 8.05 1
0 7 8 -1.08 7.65 1
0 7 8 13.97 9.02 2
0 7 9 65.11 10.28 1
0 7 9 106.01 10.90 2
0 7 10 2.94 8.71 1
0 7 11 13.64 9.16 1
0 7 12 10.25 10.18 1
0 7 13 4.22 10.65 3
0 7 13 6.10 10.06 1
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0 7 14 0.26 11.58 3
0 7 15 -14.07 11.81 3
0 7 15 -2.34 10.55 1
0 7 16 28.14 14.03 3
0 7 16 35.03 10.80 1
0 7 17 28.87 11.00 1
0 7 17 24.25 13.21 3
0 7 18 4.06 10.79 1
0 7 18 2.01 12.26 3
0 7 19 4.86 13.72 3
0 7 20 0.72 15.04 3
0 7 21 12.67 14.47 3
0 7 22 -15.29 15.51 3
0 7 23 2.12 14.65 3
0 8 0 124.29 10.39 2
0 8 0 114.64 9.80 1
0 8 -1 -6.34 8.22 2
0 8 1 -3.51 8.16 2
0 8 1 6.35 8.13 1
0 8 2 107.39 10.60 2
0 8 -2 104.18 10.09 2
0 8 2 107.13 10.80 1
0 8 3 156.80 11.68 1
0 8 -3 150.10 11.12 2
0 8 3 165.46 11.75 2
0 8 4 81.34 10.76 1
0 8 -4 62.49 9.43 2
0 8 4 58.80 9.97 2
0 8 -5 153.57 11.02 2
0 8 5 163.74 12.01 1
0 8 5 181.16 12.78 2
0 8 6 9.87 8.85 2
0 8 -6 10.09 7.83 2
0 8 6 6.47 9.75 1
0 8 7 6.43 9.91 1
0 8 7 7.06 9.58 2
0 8 8 28.88 10.06 2
0 8 8 34.84 9.37 1
0 8 9 14.76 9.26 1
0 8 9 9.80 9.80 2
0 8 10 2.69 9.60 2
0 8 10 -36.79 8.57 1
0 8 11 62.92 11.64 1
0 8 11 64.22 11.81 2
0 8 12 19.82 9.86 1
0 8 13 2.22 9.57 1
0 8 14 16.76 10.10 1
0 8 15 25.10 11.58 1
0 8 16 4.49 10.78 1
0 8 17 9.60 10.42 1
0 8 17 14.55 14.29 3
0 8 18 29.55 15.28 3
0 8 18 26.04 10.68 1
0 8 19 -18.02 14.41 3
0 8 19 14.68 11.12 1
0 8 20 -34.65 13.87 3
0 8 20 42.12 11.15 1
0 8 21 -17.39 14.37 3
0 8 21 2.25 12.20 1
0 9 0 -2.94 6.85 2
0 9 1 1.10 7.09 2
0 9 -1 0.73 6.40 2
0 9 1 -4.58 8.99 1
0 9 -2 5.72 7.25 2
0 9 2 9.73 9.03 1
0 9 2 1.37 7.73 2
0 9 -3 10.39 7.40 2
0 9 3 21.81 9.25 1
0 9 4 31.90 10.05 1
0 9 4 6.65 10.54 2
0 9 -4 16.91 7.53 2
0 9 -5 31.43 5.66 2
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19 -1 -20 23.53 18.42 4
19 -1 -19 23.98 16.83 4
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19 -1 -15 -1.71 14.65 4
19 -1 -14 -3.80 14.27 4
19 -1 -13 25.15 13.41 4
19 -1 -12 8.43 13.33 4
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19 -1 -3 -27.83 13.42 4
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19 -2 -19 29.71 16.81 4
19 -2 -18 18.40 17.17 4
19 -2 -17 7.30 15.77 4
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19 -2 -5 4.19 14.37 4
19 -2 -4 -20.29 14.15 4
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19 -2 0 8.66 9.76 4
19 -2 1 -22.33 10.34 4
19 -2 2 -17.42 10.37 4
19 -2 3 11.72 12.30 4
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19 -2 4 11.61 11.26 4
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19 -3 -17 1.51 15.05 4
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19 -3 -11 26.07 15.15 4
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19 -3 -7 -1.49 14.44 4
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19 -3 -5 -13.69 12.29 4
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20 0 -5 -31.84 14.34 4
20 0 -3 17.02 11.22 4
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20 -1 -18 2.88 17.16 4
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20 -1 -16 0.38 17.28 4
20 -1 -15 9.02 14.59 4
20 -1 -14 17.70 15.86 4
20 -1 -13 26.30 16.43 4
20 -1 -12 39.47 14.74 4
20 -1 -10 27.95 15.03 4
20 -1 -9 -0.81 14.36 4
20 -1 -8 15.86 14.63 4
20 -1 -7 -3.14 14.24 4
20 1 -7 -11.21 12.55 4
20 -1 -6 -13.14 13.44 4
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20 1 -5 -24.82 11.60 4
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20 1 -4 5.64 11.03 4
20 -1 -3 -16.82 13.27 4
20 1 -3 -22.50 10.73 4
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20 -1 0 10.04 12.04 4
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20 1 1 1.47 11.09 4
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21 -1 -8 -20.93 15.25 4
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21 -1 -2 12.22 11.64 4
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21 1 2 -0.43 12.25 4
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21 -2 -10 18.01 14.71 4
21 -2 -9 27.20 15.66 4
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;
_shelx_hkl_checksum 84842
_shelx_res_file
;
TITL NP2 IN P2(1)/N
shelx.res
created by SHELXL-2018/3 at 13:10:11 on 03-Dec-2022
CELL 0.71073 16.882 9.719 23.445 90 104.17 90
ZERR 4 0.002 0.001 0.004 0 0.01 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H F N O
UNIT 136 168 8 24 44
SIZE 0.32 0.16 0.14
L.S. 14
ACTA
BOND $H
HTAB
CONF
EQIV $1 1+X,+Y,+Z
EQIV $2 -X,-Y,-Z
EQIV $3 1.5+X,0.5-Y,-0.5+Z
EQIV $4 -1+X,+Y,+Z
EQIV $5 1-X,-Y,-Z
EQIV $6 -1.5+X,0.5-Y,0.5+Z
EQIV $7 0.5-X,0.5+Y,0.5-Z
EQIV $8 1-X,1-Y,-Z
DFIX 0.86 n2c H2ca n2c H2cb n2b H2ba n2b H2bb
DFIX 0.82 o5 H5a o5 H5d o6 H6a o6 H6d o7 H7a o7 H7b
HTAB n2c o3d
HTAB n2c o4a_$1
HTAB c3c o1c_$2
HTAB c9c o5
HTAB c9c o2b
HTAB c15d f1a_$3
HTAB n2b o4d_$4
HTAB n2b o3a
HTAB c3b f1d_$5
HTAB c8b o1c
HTAB c8b o6_$2
HTAB c15a f1d_$6
HTAB o5 o3a_$7
HTAB o5 o4d
HTAB o6 o4a_$2
HTAB o6 o7
HTAB o7 o3d
HTAB o7 o5_$8
LIST 4
SHEL 24 0.83
OMIT -8 2 23
OMIT -12 4 16
OMIT 3 5 22
OMIT -8 2 27
OMIT -4 3 17
OMIT -12 5 20
OMIT 0 4 17
OMIT -13 4 19
OMIT -15 3 22
OMIT -12 6 21
OMIT -8 2 26
OMIT -14 3 23
OMIT -13 5 20
REM
REM
REM
WGHT 0.036600 1.329600
FVAR 0.43404
O1C 5 -0.031197 0.099348 0.057668 11.00000 0.07687 0.20253 =
0.11875 -0.04788 0.03224 -0.05890
O2C 5 -0.027616 0.316612 0.074693 11.00000 0.06394 0.18749 =
0.11051 -0.01879 0.02515 0.00839
N1C 4 0.333016 0.225696 0.056821 11.00000 0.04523 0.06312 =
0.11979 -0.01545 0.01434 0.00300
N2C 4 0.502879 0.203188 0.105031 11.00000 0.04306 0.12339 =
0.05996 0.01321 0.01217 0.00087
H2CA 2 0.524977 0.228032 0.075456 11.00000 -1.20000
H2CB 2 0.544336 0.180713 0.133553 11.00000 -1.20000
N3C 4 0.004156 0.207916 0.064189 11.00000 0.06239 0.16536 =
0.06018 -0.02883 0.00978 -0.00960
C1C 1 0.252111 0.222244 0.057180 11.00000 0.04097 0.06543 =
0.05204 0.00219 -0.00029 -0.00185
C2C 1 0.207874 0.100138 0.048139 11.00000 0.05530 0.07500 =
0.08041 -0.01197 0.01178 -0.00766
AFIX 43
H2C 2 0.233224 0.019457 0.040707 11.00000 -1.20000
AFIX 0
C3C 1 0.126709 0.097130 0.050055 11.00000 0.05894 0.09143 =
0.07827 -0.01331 0.01119 -0.02599
AFIX 43
H3C 2 0.097724 0.014854 0.044109 11.00000 -1.20000
AFIX 0
C4C 1 0.089236 0.215873 0.060749 11.00000 0.04028 0.11083 =
0.05100 -0.00896 0.00662 -0.00298
C5C 1 0.130476 0.336585 0.068333 11.00000 0.05325 0.09112 =
0.07272 -0.00298 0.00995 0.01043
AFIX 43
H5C 2 0.104210 0.417170 0.074714 11.00000 -1.20000
AFIX 0
C6C 1 0.210089 0.339801 0.066611 11.00000 0.04937 0.06543 =
0.08810 -0.00021 0.01321 0.00303
AFIX 43
H6C 2 0.237594 0.423523 0.071920 11.00000 -1.20000
AFIX 0
C7C 1 0.378115 0.111943 0.040220 11.00000 0.05229 0.08784 =
0.09035 -0.01869 0.01062 0.00266
AFIX 23
H7CA 2 0.395409 0.135654 0.004936 11.00000 -1.20000
H7CB 2 0.343097 0.031626 0.031706 11.00000 -1.20000
AFIX 0
C8C 1 0.451277 0.079543 0.088855 11.00000 0.05833 0.08870 =
0.08883 0.00734 0.02249 0.00921
AFIX 23
H8CA 2 0.433740 0.046830 0.122885 11.00000 -1.20000
H8CB 2 0.482818 0.007113 0.076378 11.00000 -1.20000
AFIX 0
C9C 1 0.455954 0.319691 0.120123 11.00000 0.06252 0.10313 =
0.11031 -0.02512 0.03518 -0.02285
AFIX 23
H9CA 2 0.490449 0.400734 0.127955 11.00000 -1.20000
H9CB 2 0.438091 0.298123 0.155397 11.00000 -1.20000
AFIX 0
C10C 1 0.383433 0.348275 0.070614 11.00000 0.05411 0.06858 =
0.16250 0.00388 0.01702 -0.00120
AFIX 23
H10A 2 0.351600 0.422484 0.081479 11.00000 -1.20000
H10B 2 0.401437 0.376935 0.036203 11.00000 -1.20000
AFIX 0
F1D 3 0.809576 0.296129 -0.151393 11.00000 0.10678 0.17881 =
0.08441 -0.01165 0.05785 -0.00978
O3D 5 0.563893 0.276513 0.011631 11.00000 0.04827 0.15653 =
0.06308 0.01928 0.01517 0.00431
O4D 5 0.681382 0.281236 0.078935 11.00000 0.06496 0.09991 =
0.05427 0.00908 0.01361 0.00965
C11D 1 0.685847 0.279948 -0.021706 11.00000 0.04510 0.05311 =
0.05008 0.00524 0.01362 -0.00019
C12D 1 0.644675 0.274259 -0.080084 11.00000 0.05607 0.09029 =
0.05926 -0.00818 0.00883 -0.00481
AFIX 43
H12D 2 0.588034 0.266742 -0.090222 11.00000 -1.20000
AFIX 0
C13D 1 0.686569 0.279592 -0.123761 11.00000 0.08413 0.12408 =
0.04844 -0.01733 0.02413 -0.01007
AFIX 43
H13D 2 0.658864 0.276926 -0.163259 11.00000 -1.20000
AFIX 0
C14D 1 0.769171 0.288818 -0.107527 11.00000 0.07263 0.08960 =
0.07429 -0.00785 0.04769 -0.00567
C15D 1 0.811861 0.293176 -0.050783 11.00000 0.05762 0.08549 =
0.06944 0.00187 0.01635 0.00329
AFIX 43
H15D 2 0.868565 0.299146 -0.041181 11.00000 -1.20000
AFIX 0
C16D 1 0.769800 0.288609 -0.007445 11.00000 0.05833 0.07954 =
0.05362 0.01147 0.01919 0.00356
AFIX 43
H16D 2 0.798341 0.291399 0.031866 11.00000 -1.20000
AFIX 0
C17D 1 0.640049 0.278571 0.026327 11.00000 0.05612 0.07214 =
0.04974 0.00804 0.01184 0.00351
O2B 5 0.323073 0.276916 0.206815 11.00000 0.07278 0.14700 =
0.10139 -0.03528 0.03580 -0.04258
O1B 5 0.329027 0.056317 0.200741 11.00000 0.05529 0.14459 =
0.13435 0.01571 0.02818 0.02166
N1B 4 -0.034938 0.123502 0.216866 11.00000 0.04117 0.06492 =
0.13068 -0.01360 0.02037 -0.00371
N2B 4 -0.204403 0.145631 0.165276 11.00000 0.04743 0.07365 =
0.05611 0.00881 0.01405 0.00831
H2BA 2 -0.244272 0.171562 0.135803 11.00000 -1.20000
H2BB 2 -0.226896 0.119578 0.194246 11.00000 -1.20000
N3B 4 0.291666 0.163829 0.204812 11.00000 0.05147 0.12264 =
0.05401 0.00058 0.01230 -0.00641
C1B 1 0.044068 0.134794 0.212701 11.00000 0.03905 0.06464 =
0.05934 0.00170 -0.00119 0.00680
C2B 1 0.089843 0.018108 0.206748 11.00000 0.04378 0.06894 =
0.10322 0.00917 0.01023 0.00179
AFIX 43
H2B 2 0.065666 -0.068307 0.204790 11.00000 -1.20000
AFIX 0
C3B 1 0.169762 0.028747 0.203744 11.00000 0.05175 0.07990 =
0.08543 0.00616 0.01037 0.01069
AFIX 43
H3B 2 0.199054 -0.050062 0.199530 11.00000 -1.20000
AFIX 0
C4B 1 0.206339 0.154444 0.206919 11.00000 0.03794 0.09097 =
0.04991 0.00175 0.00535 -0.00772
C5B 1 0.163388 0.271114 0.212491 11.00000 0.06009 0.07845 =
0.05441 -0.00493 0.00926 -0.01042
AFIX 43
H5B 2 0.188542 0.356672 0.214251 11.00000 -1.20000
AFIX 0
C6B 1 0.083579 0.262333 0.215483 11.00000 0.05262 0.06927 =
0.06763 -0.01000 0.01023 -0.00185
AFIX 43
H6B 2 0.055117 0.342280 0.219424 11.00000 -1.20000
AFIX 0
C7B 1 -0.084821 -0.000051 0.200125 11.00000 0.04860 0.06559 =
0.13738 0.00265 0.02476 0.00216
AFIX 23
H7BA 2 -0.104035 -0.032659 0.233468 11.00000 -1.20000
H7BB 2 -0.051975 -0.072114 0.188784 11.00000 -1.20000
AFIX 0
C8B 1 -0.156711 0.031327 0.149634 11.00000 0.05743 0.07396 =
0.09986 -0.01749 0.03328 -0.00368
AFIX 23
H8BA 2 -0.137606 0.055819 0.115176 11.00000 -1.20000
H8BB 2 -0.191039 -0.049624 0.140231 11.00000 -1.20000
AFIX 0
C9B 1 -0.153910 0.270059 0.184018 11.00000 0.06008 0.06007 =
0.08083 0.00119 0.02075 0.00356
AFIX 23
H9BA 2 -0.186574 0.340691 0.196546 11.00000 -1.20000
H9BB 2 -0.134516 0.305835 0.151264 11.00000 -1.20000
AFIX 0
C10B 1 -0.082213 0.233456 0.234090 11.00000 0.05170 0.08208 =
0.08605 -0.01361 0.01823 0.00436
AFIX 23
H10C 2 -0.047802 0.313746 0.245332 11.00000 -1.20000
H10D 2 -0.101734 0.204666 0.267845 11.00000 -1.20000
AFIX 0
F1A 3 -0.496829 0.169929 0.432164 11.00000 0.09954 0.24631 =
0.08999 -0.04327 0.05516 -0.01797
O4A 5 -0.383696 0.098379 0.198210 11.00000 0.06678 0.14526 =
0.05095 -0.00348 0.00763 0.01968
O3A 5 -0.263816 0.093724 0.261860 11.00000 0.04379 0.11598 =
0.06134 0.01206 0.01745 0.00974
C11A 1 -0.380978 0.125534 0.298818 11.00000 0.04170 0.05234 =
0.04837 -0.00045 0.00966 0.00132
C16A 1 -0.465405 0.121001 0.287992 11.00000 0.05487 0.06976 =
0.05363 -0.00478 0.00968 -0.00062
AFIX 43
H16A 2 -0.496139 0.108480 0.249617 11.00000 -1.20000
AFIX 0
C15A 1 -0.505086 0.134563 0.332605 11.00000 0.05546 0.10161 =
0.06960 -0.01824 0.02126 -0.01318
AFIX 43
H15A 2 -0.561728 0.129803 0.325026 11.00000 -1.20000
AFIX 0
C14A 1 -0.458913 0.154925 0.387483 11.00000 0.06850 0.13057 =
0.06932 -0.02288 0.04304 -0.01051
C13A 1 -0.375641 0.162917 0.401237 11.00000 0.07495 0.14108 =
0.05036 -0.02352 0.01680 -0.01192
AFIX 43
H13A 2 -0.345964 0.178267 0.439690 11.00000 -1.20000
AFIX 0
C12A 1 -0.336828 0.147349 0.355865 11.00000 0.05515 0.08963 =
0.05345 -0.00901 0.01044 -0.00508
AFIX 43
H12A 2 -0.280128 0.151696 0.364060 11.00000 -1.20000
AFIX 0
C17A 1 -0.339498 0.106112 0.249710 11.00000 0.05523 0.07156 =
0.05045 0.00699 0.01620 0.00725
O5 5 0.637388 0.475224 0.152589 11.00000 0.06103 0.11218 =
0.09972 -0.03584 0.00778 -0.00220
H5A 2 0.677937 0.512505 0.175638 11.00000 -1.20000
H5D 2 0.653328 0.419163 0.130945 11.00000 -1.20000
O6 5 0.342683 0.062792 -0.110931 11.00000 0.11532 0.16984 =
0.14915 -0.06828 0.05554 -0.04108
H6A 2 0.348798 0.041630 -0.144425 11.00000 -1.20000
H6D 2 0.370582 0.134807 -0.106061 11.00000 -1.20000
O7 5 0.431764 0.300983 -0.086417 11.00000 0.12242 0.12781 =
0.15645 0.01943 -0.05048 -0.02352
H7A 2 0.472624 0.311163 -0.058581 11.00000 -1.20000
H7B 2 0.413748 0.373153 -0.103807 11.00000 -1.20000
HKLF 4
REM NP2 IN P2(1)/N
REM wR2 = 0.1536, GooF = S = 1.057, Restrained GooF = 1.057 for all data
REM R1 = 0.0891 for 2429 Fo > 4sig(Fo) and 0.2405 for all 6755 data
REM 508 parameters refined using 10 restraints
END
WGHT 0.0361 1.3795
REM Instructions for potential hydrogen bonds
HTAB N2C O3D
HTAB N2C O4A_$1
HTAB C3C O1C_$2
HTAB C9C O5
HTAB C9C O2B
HTAB C15D F1A_$3
HTAB N2B O4D_$4
HTAB N2B O3A
HTAB C3B F1D_$5
HTAB C8B O1C
HTAB C8B O6_$2
HTAB C15A F1D_$6
HTAB O5 O3A_$7
HTAB O5 O4D
HTAB O6 O4A_$2
HTAB O6 O7
HTAB O7 O3D
HTAB O7 O5_$8
REM Highest difference peak 0.192, deepest hole -0.177, 1-sigma level 0.034
Q1 1 -0.3578 0.2139 0.2081 11.00000 0.05 0.19
Q2 1 0.3095 0.1461 -0.1605 11.00000 0.05 0.17
Q3 1 0.0015 -0.0079 0.0750 11.00000 0.05 0.14
Q4 1 0.0453 0.3544 0.1984 11.00000 0.05 0.14
Q5 1 0.2687 0.3929 0.1952 11.00000 0.05 0.13
Q6 1 0.9153 0.2679 -0.0726 11.00000 0.05 0.13
Q7 1 0.7612 0.4384 -0.0342 11.00000 0.05 0.12
Q8 1 0.3002 0.2158 0.0205 11.00000 0.05 0.12
Q9 1 0.6540 0.1319 0.0598 11.00000 0.05 0.11
Q10 1 -0.2370 0.1239 0.3085 11.00000 0.05 0.11
Q11 1 -0.0687 0.0002 0.1550 11.00000 0.05 0.11
Q12 1 0.7363 0.2947 0.0863 11.00000 0.05 0.11
Q13 1 0.1986 0.4143 0.2047 11.00000 0.05 0.11
Q14 1 0.7998 0.3182 -0.0328 11.00000 0.05 0.11
Q15 1 0.0834 0.0833 0.1636 11.00000 0.05 0.11
Q16 1 0.6143 0.3004 -0.2241 11.00000 0.05 0.11
Q17 1 0.3398 0.4967 0.1909 11.00000 0.05 0.11
Q18 1 -0.2952 0.0808 0.3651 11.00000 0.05 0.11
Q19 1 0.3273 0.3883 0.1656 11.00000 0.05 0.11
Q20 1 0.6916 0.1564 0.0552 11.00000 0.05 0.11
;
_shelx_res_checksum 21244
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
O O1C -0.0312(2) 0.0993(6) 0.05767(19) 0.1313(19) Uani d 1 . .
O O2C -0.0276(2) 0.3166(5) 0.07469(19) 0.1200(17) Uani d 1 . .
N N1C 0.3330(2) 0.2257(4) 0.05682(18) 0.0771(13) Uani d 1 . .
N N2C 0.5029(2) 0.2032(6) 0.10503(19) 0.0755(13) Uani d 1 . .
H H2CA 0.525(3) 0.228(5) 0.0755(15) 0.091 Uiso d 1 . .
H H2CB 0.5443(19) 0.181(4) 0.1336(15) 0.091 Uiso d 1 . .
N N3C 0.0042(3) 0.2079(7) 0.0642(2) 0.0969(18) Uani d 1 . .
C C1C 0.2521(3) 0.2222(5) 0.05718(18) 0.0548(12) Uani d 1 . .
C C2C 0.2079(3) 0.1001(5) 0.0481(2) 0.0711(15) Uani d 1 . .
H H2C 0.233224 0.019457 0.040707 0.085 Uiso calc 1 . .
C C3C 0.1267(3) 0.0971(6) 0.0501(2) 0.0772(16) Uani d 1 . .
H H3C 0.097724 0.014854 0.044109 0.093 Uiso calc 1 . .
C C4C 0.0892(3) 0.2159(7) 0.0607(2) 0.0682(15) Uani d 1 . .
C C5C 0.1305(3) 0.3366(6) 0.0683(2) 0.0733(15) Uani d 1 . .
H H5C 0.104210 0.417170 0.074714 0.088 Uiso calc 1 . .
C C6C 0.2101(3) 0.3398(5) 0.0666(2) 0.0683(14) Uani d 1 . .
H H6C 0.237594 0.423523 0.071920 0.082 Uiso calc 1 . .
C C7C 0.3781(3) 0.1119(5) 0.0402(2) 0.0780(16) Uani d 1 . .
H H7CA 0.395409 0.135654 0.004936 0.094 Uiso calc 1 . .
H H7CB 0.343097 0.031626 0.031706 0.094 Uiso calc 1 . .
C C8C 0.4513(3) 0.0795(5) 0.0889(2) 0.0778(15) Uani d 1 . .
H H8CA 0.433740 0.046830 0.122885 0.093 Uiso calc 1 . .
H H8CB 0.482818 0.007113 0.076378 0.093 Uiso calc 1 . .
C C9C 0.4560(3) 0.3197(6) 0.1201(2) 0.0896(18) Uani d 1 . .
H H9CA 0.490449 0.400734 0.127955 0.107 Uiso calc 1 . .
H H9CB 0.438091 0.298123 0.155397 0.107 Uiso calc 1 . .
C C10C 0.3834(3) 0.3483(5) 0.0706(3) 0.0967(19) Uani d 1 . .
H H10A 0.351600 0.422484 0.081479 0.116 Uiso calc 1 . .
H H10B 0.401437 0.376935 0.036203 0.116 Uiso calc 1 . .
F F1D 0.80958(18) 0.2961(4) -0.15139(13) 0.1174(11) Uani d 1 . .
O O3D 0.56389(18) 0.2765(4) 0.01163(13) 0.0890(12) Uani d 1 . .
O O4D 0.68138(17) 0.2812(3) 0.07894(14) 0.0732(9) Uani d 1 . .
C C11D 0.6858(2) 0.2799(4) -0.02171(19) 0.0491(11) Uani d 1 . .
C C12D 0.6447(3) 0.2743(5) -0.0801(2) 0.0695(14) Uani d 1 . .
H H12D 0.588034 0.266742 -0.090222 0.083 Uiso calc 1 . .
C C13D 0.6866(3) 0.2796(5) -0.1238(2) 0.0842(17) Uani d 1 . .
H H13D 0.658864 0.276926 -0.163259 0.101 Uiso calc 1 . .
C C14D 0.7692(3) 0.2888(5) -0.1075(2) 0.0737(15) Uani d 1 . .
C C15D 0.8119(3) 0.2932(5) -0.0508(2) 0.0707(14) Uani d 1 . .
H H15D 0.868565 0.299146 -0.041181 0.085 Uiso calc 1 . .
C C16D 0.7698(3) 0.2886(5) -0.0074(2) 0.0629(13) Uani d 1 . .
H H16D 0.798341 0.291399 0.031866 0.075 Uiso calc 1 . .
C C17D 0.6400(3) 0.2786(5) 0.0263(2) 0.0595(13) Uani d 1 . .
O O2B 0.3231(2) 0.2769(5) 0.20682(17) 0.1045(14) Uani d 1 . .
O O1B 0.3290(2) 0.0563(5) 0.20074(18) 0.1105(15) Uani d 1 . .
N N1B -0.0349(2) 0.1235(4) 0.21687(19) 0.0790(13) Uani d 1 . .
N N2B -0.2044(2) 0.1456(5) 0.16528(17) 0.0588(11) Uani d 1 . .
H H2BA -0.2443(18) 0.172(4) 0.1358(13) 0.071 Uiso d 1 . .
H H2BB -0.227(2) 0.120(4) 0.1942(13) 0.071 Uiso d 1 . .
N N3B 0.2917(3) 0.1638(6) 0.20481(18) 0.0761(14) Uani d 1 . .
C C1B 0.0441(3) 0.1348(5) 0.21270(19) 0.0566(13) Uani d 1 . .
C C2B 0.0898(3) 0.0181(5) 0.2067(2) 0.0733(15) Uani d 1 . .
H H2B 0.065666 -0.068307 0.204790 0.088 Uiso calc 1 . .
C C3B 0.1698(3) 0.0287(6) 0.2037(2) 0.0735(15) Uani d 1 . .
H H3B 0.199054 -0.050062 0.199530 0.088 Uiso calc 1 . .
C C4B 0.2063(3) 0.1544(7) 0.20692(19) 0.0605(14) Uani d 1 . .
C C5B 0.1634(3) 0.2711(5) 0.21249(18) 0.0651(14) Uani d 1 . .
H H5B 0.188542 0.356672 0.214251 0.078 Uiso calc 1 . .
C C6B 0.0836(3) 0.2623(5) 0.21548(18) 0.0640(14) Uani d 1 . .
H H6B 0.055117 0.342280 0.219424 0.077 Uiso calc 1 . .
C C7B -0.0848(3) -0.0001(5) 0.2001(2) 0.0835(16) Uani d 1 . .
H H7BA -0.104035 -0.032659 0.233468 0.100 Uiso calc 1 . .
H H7BB -0.051975 -0.072114 0.188784 0.100 Uiso calc 1 . .
C C8B -0.1567(3) 0.0313(5) 0.1496(2) 0.0746(15) Uani d 1 . .
H H8BA -0.137606 0.055819 0.115176 0.090 Uiso calc 1 . .
H H8BB -0.191039 -0.049624 0.140231 0.090 Uiso calc 1 . .
C C9B -0.1539(3) 0.2701(5) 0.1840(2) 0.0664(14) Uani d 1 . .
H H9BA -0.186574 0.340691 0.196546 0.080 Uiso calc 1 . .
H H9BB -0.134516 0.305835 0.151264 0.080 Uiso calc 1 . .
C C10B -0.0822(3) 0.2335(5) 0.2341(2) 0.0730(15) Uani d 1 . .
H H10C -0.047802 0.313746 0.245332 0.088 Uiso calc 1 . .
H H10D -0.101734 0.204666 0.267845 0.088 Uiso calc 1 . .
F F1A -0.49683(18) 0.1699(4) 0.43216(14) 0.1397(14) Uani d 1 . .
O O4A -0.38370(18) 0.0984(4) 0.19821(14) 0.0888(11) Uani d 1 . .
O O3A -0.26382(17) 0.0937(3) 0.26186(12) 0.0729(10) Uani d 1 . .
C C11A -0.3810(2) 0.1255(4) 0.29882(19) 0.0477(11) Uani d 1 . .
C C16A -0.4654(3) 0.1210(4) 0.2880(2) 0.0600(13) Uani d 1 . .
H H16A -0.496139 0.108480 0.249617 0.072 Uiso calc 1 . .
C C15A -0.5051(3) 0.1346(5) 0.3326(2) 0.0745(15) Uani d 1 . .
H H15A -0.561728 0.129803 0.325026 0.089 Uiso calc 1 . .
C C14A -0.4589(3) 0.1549(6) 0.3875(2) 0.0849(17) Uani d 1 . .
C C13A -0.3756(3) 0.1629(6) 0.4012(2) 0.0885(18) Uani d 1 . .
H H13A -0.345964 0.178267 0.439690 0.106 Uiso calc 1 . .
C C12A -0.3368(3) 0.1473(5) 0.3559(2) 0.0666(14) Uani d 1 . .
H H12A -0.280128 0.151696 0.364060 0.080 Uiso calc 1 . .
C C17A -0.3395(3) 0.1061(5) 0.2497(2) 0.0585(13) Uani d 1 . .
O O5 0.6374(2) 0.4752(4) 0.15259(17) 0.0930(12) Uani d 1 . .
H H5A 0.678(2) 0.513(5) 0.1756(19) 0.112 Uiso d 1 . .
H H5D 0.653(3) 0.419(4) 0.131(2) 0.112 Uiso d 1 . .
O O6 0.3427(3) 0.0628(6) -0.1109(2) 0.1407(17) Uani d 1 . .
H H6A 0.349(4) 0.042(7) -0.1444(15) 0.169 Uiso d 1 . .
H H6D 0.371(4) 0.135(4) -0.106(3) 0.169 Uiso d 1 . .
O O7 0.4318(3) 0.3010(5) -0.0864(3) 0.1502(18) Uani d 1 . .
H H7A 0.473(3) 0.311(7) -0.059(2) 0.180 Uiso d 1 . .
H H7B 0.414(4) 0.373(4) -0.104(3) 0.180 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
O1C 0.077(3) 0.203(5) 0.119(4) -0.059(3) 0.032(2) -0.048(4)
O2C 0.064(3) 0.187(5) 0.111(4) 0.008(3) 0.025(2) -0.019(4)
N1C 0.045(3) 0.063(3) 0.120(4) 0.003(2) 0.014(2) -0.015(3)
N2C 0.043(3) 0.123(4) 0.060(3) 0.001(3) 0.012(2) 0.013(3)
N3C 0.062(4) 0.165(6) 0.060(3) -0.010(4) 0.010(3) -0.029(4)
C1C 0.041(3) 0.065(3) 0.052(3) -0.002(3) 0.000(2) 0.002(3)
C2C 0.055(3) 0.075(4) 0.080(4) -0.008(3) 0.012(3) -0.012(3)
C3C 0.059(4) 0.091(5) 0.078(4) -0.026(3) 0.011(3) -0.013(3)
C4C 0.040(3) 0.111(5) 0.051(3) -0.003(4) 0.007(2) -0.009(4)
C5C 0.053(3) 0.091(5) 0.073(4) 0.010(3) 0.010(3) -0.003(3)
C6C 0.049(3) 0.065(4) 0.088(4) 0.003(3) 0.013(3) 0.000(3)
C7C 0.052(3) 0.088(4) 0.090(4) 0.003(3) 0.011(3) -0.019(3)
C8C 0.058(3) 0.089(4) 0.089(4) 0.009(3) 0.022(3) 0.007(3)
C9C 0.063(4) 0.103(5) 0.110(5) -0.023(3) 0.035(3) -0.025(4)
C10C 0.054(3) 0.069(4) 0.162(6) -0.001(3) 0.017(3) 0.004(4)
F1D 0.107(2) 0.179(3) 0.084(2) -0.010(2) 0.0579(19) -0.012(2)
O3D 0.048(2) 0.157(3) 0.063(2) 0.004(2) 0.0152(17) 0.019(2)
O4D 0.065(2) 0.100(3) 0.054(2) 0.0097(18) 0.0136(17) 0.009(2)
C11D 0.045(3) 0.053(3) 0.050(3) 0.000(2) 0.014(2) 0.005(3)
C12D 0.056(3) 0.090(4) 0.059(4) -0.005(3) 0.009(3) -0.008(3)
C13D 0.084(4) 0.124(5) 0.048(3) -0.010(4) 0.024(3) -0.017(3)
C14D 0.073(4) 0.090(4) 0.074(4) -0.006(3) 0.048(3) -0.008(4)
C15D 0.058(3) 0.085(4) 0.069(4) 0.003(3) 0.016(3) 0.002(4)
C16D 0.058(3) 0.080(4) 0.054(3) 0.004(3) 0.019(3) 0.011(3)
C17D 0.056(3) 0.072(4) 0.050(3) 0.004(3) 0.012(3) 0.008(3)
O2B 0.073(3) 0.147(4) 0.101(3) -0.043(3) 0.036(2) -0.035(3)
O1B 0.055(2) 0.145(4) 0.134(4) 0.022(2) 0.028(2) 0.016(3)
N1B 0.041(2) 0.065(3) 0.131(4) -0.004(2) 0.020(2) -0.014(3)
N2B 0.047(3) 0.074(3) 0.056(3) 0.008(3) 0.0141(19) 0.009(3)
N3B 0.051(3) 0.123(5) 0.054(3) -0.006(3) 0.012(2) 0.001(3)
C1B 0.039(3) 0.065(4) 0.059(3) 0.007(3) -0.001(2) 0.002(3)
C2B 0.044(3) 0.069(4) 0.103(4) 0.002(3) 0.010(3) 0.009(3)
C3B 0.052(3) 0.080(4) 0.085(4) 0.011(3) 0.010(3) 0.006(3)
C4B 0.038(3) 0.091(4) 0.050(3) -0.008(3) 0.005(2) 0.002(3)
C5B 0.060(3) 0.078(4) 0.054(3) -0.010(3) 0.009(2) -0.005(3)
C6B 0.053(3) 0.069(4) 0.068(4) -0.002(3) 0.010(2) -0.010(3)
C7B 0.049(3) 0.066(4) 0.137(5) 0.002(3) 0.025(3) 0.003(4)
C8B 0.057(3) 0.074(4) 0.100(4) -0.004(3) 0.033(3) -0.017(3)
C9B 0.060(3) 0.060(3) 0.081(4) 0.004(3) 0.021(3) 0.001(3)
C10B 0.052(3) 0.082(4) 0.086(4) 0.004(3) 0.018(3) -0.014(3)
F1A 0.100(2) 0.246(4) 0.090(2) -0.018(2) 0.055(2) -0.043(3)
O4A 0.067(2) 0.145(3) 0.051(2) 0.020(2) 0.0076(18) -0.003(2)
O3A 0.0438(19) 0.116(3) 0.061(2) 0.0097(18) 0.0175(16) 0.012(2)
C11A 0.042(3) 0.052(3) 0.048(3) 0.001(2) 0.010(2) 0.000(3)
C16A 0.055(3) 0.070(3) 0.054(3) -0.001(3) 0.010(2) -0.005(3)
C15A 0.055(3) 0.102(4) 0.070(4) -0.013(3) 0.021(3) -0.018(4)
C14A 0.068(4) 0.131(5) 0.069(4) -0.011(4) 0.043(3) -0.023(4)
C13A 0.075(4) 0.141(5) 0.050(3) -0.012(4) 0.017(3) -0.024(4)
C12A 0.055(3) 0.090(4) 0.053(3) -0.005(3) 0.010(3) -0.009(3)
C17A 0.055(3) 0.072(4) 0.050(3) 0.007(3) 0.016(3) 0.007(3)
O5 0.061(2) 0.112(3) 0.100(3) -0.002(2) 0.008(2) -0.036(3)
O6 0.115(3) 0.170(5) 0.149(4) -0.041(3) 0.056(3) -0.068(4)
O7 0.122(4) 0.128(4) 0.156(5) -0.024(3) -0.050(3) 0.019(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
F F 0.0171 0.0103 '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
C1C N1C C7C . . 125.0(4) ?
C1C N1C C10C . . 123.3(4) ?
C7C N1C C10C . . 111.6(4) ?
C9C N2C C8C . . 111.6(4) ?
C9C N2C H2CA . . 109(3) ?
C8C N2C H2CA . . 111(3) ?
C9C N2C H2CB . . 113(3) ?
C8C N2C H2CB . . 108(3) ?
H2CA N2C H2CB . . 105(4) ?
O1C N3C O2C . . 123.3(6) ?
O1C N3C C4C . . 120.2(6) ?
O2C N3C C4C . . 116.5(6) ?
N1C C1C C2C . . 121.3(5) ?
N1C C1C C6C . . 122.0(5) ?
C2C C1C C6C . . 116.7(4) ?
C3C C2C C1C . . 120.9(5) ?
C3C C2C H2C . . 119.6 ?
C1C C2C H2C . . 119.6 ?
C4C C3C C2C . . 119.6(5) ?
C4C C3C H3C . . 120.2 ?
C2C C3C H3C . . 120.2 ?
C5C C4C C3C . . 120.6(5) ?
C5C C4C N3C . . 121.3(6) ?
C3C C4C N3C . . 118.1(6) ?
C4C C5C C6C . . 119.9(5) ?
C4C C5C H5C . . 120.1 ?
C6C C5C H5C . . 120.1 ?
C5C C6C C1C . . 122.3(5) ?
C5C C6C H6C . . 118.9 ?
C1C C6C H6C . . 118.9 ?
N1C C7C C8C . . 110.3(4) ?
N1C C7C H7CA . . 109.6 ?
C8C C7C H7CA . . 109.6 ?
N1C C7C H7CB . . 109.6 ?
C8C C7C H7CB . . 109.6 ?
H7CA C7C H7CB . . 108.1 ?
N2C C8C C7C . . 110.4(4) ?
N2C C8C H8CA . . 109.6 ?
C7C C8C H8CA . . 109.6 ?
N2C C8C H8CB . . 109.6 ?
C7C C8C H8CB . . 109.6 ?
H8CA C8C H8CB . . 108.1 ?
N2C C9C C10C . . 110.1(4) ?
N2C C9C H9CA . . 109.6 ?
C10C C9C H9CA . . 109.6 ?
N2C C9C H9CB . . 109.6 ?
C10C C9C H9CB . . 109.6 ?
H9CA C9C H9CB . . 108.2 ?
N1C C10C C9C . . 110.2(4) ?
N1C C10C H10A . . 109.6 ?
C9C C10C H10A . . 109.6 ?
N1C C10C H10B . . 109.6 ?
C9C C10C H10B . . 109.6 ?
H10A C10C H10B . . 108.1 ?
C12D C11D C16D . . 118.9(4) ?
C12D C11D C17D . . 120.9(4) ?
C16D C11D C17D . . 120.2(4) ?
C11D C12D C13D . . 120.7(4) ?
C11D C12D H12D . . 119.7 ?
C13D C12D H12D . . 119.7 ?
C14D C13D C12D . . 118.2(5) ?
C14D C13D H13D . . 120.9 ?
C12D C13D H13D . . 120.9 ?
C15D C14D C13D . . 122.9(5) ?
C15D C14D F1D . . 119.7(5) ?
C13D C14D F1D . . 117.4(5) ?
C14D C15D C16D . . 118.7(5) ?
C14D C15D H15D . . 120.7 ?
C16D C15D H15D . . 120.7 ?
C15D C16D C11D . . 120.6(4) ?
C15D C16D H16D . . 119.7 ?
C11D C16D H16D . . 119.7 ?
O3D C17D O4D . . 123.9(4) ?
O3D C17D C11D . . 118.3(4) ?
O4D C17D C11D . . 117.8(4) ?
C1B N1B C10B . . 125.1(4) ?
C1B N1B C7B . . 123.7(4) ?
C10B N1B C7B . . 111.1(4) ?
C8B N2B C9B . . 112.3(3) ?
C8B N2B H2BA . . 113(3) ?
C9B N2B H2BA . . 106(3) ?
C8B N2B H2BB . . 110(3) ?
C9B N2B H2BB . . 109(3) ?
H2BA N2B H2BB . . 107(4) ?
O2B N3B O1B . . 122.8(5) ?
O2B N3B C4B . . 118.7(5) ?
O1B N3B C4B . . 118.5(5) ?
N1B C1B C2B . . 121.0(5) ?
N1B C1B C6B . . 122.0(5) ?
C2B C1B C6B . . 117.0(4) ?
C3B C2B C1B . . 121.2(5) ?
C3B C2B H2B . . 119.4 ?
C1B C2B H2B . . 119.4 ?
C4B C3B C2B . . 120.2(5) ?
C4B C3B H3B . . 119.9 ?
C2B C3B H3B . . 119.9 ?
C3B C4B C5B . . 120.3(4) ?
C3B C4B N3B . . 119.5(6) ?
C5B C4B N3B . . 120.2(5) ?
C6B C5B C4B . . 120.3(5) ?
C6B C5B H5B . . 119.9 ?
C4B C5B H5B . . 119.9 ?
C5B C6B C1B . . 121.1(5) ?
C5B C6B H6B . . 119.5 ?
C1B C6B H6B . . 119.5 ?
N1B C7B C8B . . 110.2(4) ?
N1B C7B H7BA . . 109.6 ?
C8B C7B H7BA . . 109.6 ?
N1B C7B H7BB . . 109.6 ?
C8B C7B H7BB . . 109.6 ?
H7BA C7B H7BB . . 108.1 ?
N2B C8B C7B . . 110.0(4) ?
N2B C8B H8BA . . 109.7 ?
C7B C8B H8BA . . 109.7 ?
N2B C8B H8BB . . 109.7 ?
C7B C8B H8BB . . 109.7 ?
H8BA C8B H8BB . . 108.2 ?
N2B C9B C10B . . 109.4(4) ?
N2B C9B H9BA . . 109.8 ?
C10B C9B H9BA . . 109.8 ?
N2B C9B H9BB . . 109.8 ?
C10B C9B H9BB . . 109.8 ?
H9BA C9B H9BB . . 108.2 ?
N1B C10B C9B . . 110.4(4) ?
N1B C10B H10C . . 109.6 ?
C9B C10B H10C . . 109.6 ?
N1B C10B H10D . . 109.6 ?
C9B C10B H10D . . 109.6 ?
H10C C10B H10D . . 108.1 ?
C12A C11A C16A . . 118.0(4) ?
C12A C11A C17A . . 121.4(4) ?
C16A C11A C17A . . 120.5(4) ?
C15A C16A C11A . . 121.8(4) ?
C15A C16A H16A . . 119.1 ?
C11A C16A H16A . . 119.1 ?
C14A C15A C16A . . 117.6(5) ?
C14A C15A H15A . . 121.2 ?
C16A C15A H15A . . 121.2 ?
C15A C14A F1A . . 118.7(5) ?
C15A C14A C13A . . 123.8(5) ?
F1A C14A C13A . . 117.6(5) ?
C14A C13A C12A . . 117.7(5) ?
C14A C13A H13A . . 121.1 ?
C12A C13A H13A . . 121.1 ?
C11A C12A C13A . . 121.1(4) ?
C11A C12A H12A . . 119.5 ?
C13A C12A H12A . . 119.5 ?
O3A C17A O4A . . 123.3(4) ?
O3A C17A C11A . . 118.9(4) ?
O4A C17A C11A . . 117.8(4) ?
H5A O5 H5D . . 110(5) ?
H6A O6 H6D . . 98(7) ?
H7A O7 H7B . . 115(7) ?
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
O1C N3C . 1.203(6) ?
O2C N3C . 1.237(6) ?
N1C C1C . 1.368(5) ?
N1C C7C . 1.449(5) ?
N1C C10C . 1.454(5) ?
N2C C9C . 1.474(6) ?
N2C C8C . 1.478(6) ?
N2C H2CA . 0.897(19) ?
N2C H2CB . 0.869(19) ?
N3C C4C . 1.460(6) ?
C1C C2C . 1.391(5) ?
C1C C6C . 1.391(5) ?
C2C C3C . 1.382(6) ?
C2C H2C . 0.9300 ?
C3C C4C . 1.368(6) ?
C3C H3C . 0.9300 ?
C4C C5C . 1.354(6) ?
C5C C6C . 1.355(5) ?
C5C H5C . 0.9300 ?
C6C H6C . 0.9300 ?
C7C C8C . 1.495(5) ?
C7C H7CA . 0.9700 ?
C7C H7CB . 0.9700 ?
C8C H8CA . 0.9700 ?
C8C H8CB . 0.9700 ?
C9C C10C . 1.493(6) ?
C9C H9CA . 0.9700 ?
C9C H9CB . 0.9700 ?
C10C H10A . 0.9700 ?
C10C H10B . 0.9700 ?
F1D C14D . 1.368(5) ?
O3D C17D . 1.247(4) ?
O4D C17D . 1.260(5) ?
C11D C12D . 1.376(5) ?
C11D C16D . 1.377(5) ?
C11D C17D . 1.514(6) ?
C12D C13D . 1.381(6) ?
C12D H12D . 0.9300 ?
C13D C14D . 1.356(6) ?
C13D H13D . 0.9300 ?
C14D C15D . 1.350(6) ?
C15D C16D . 1.375(6) ?
C15D H15D . 0.9300 ?
C16D H16D . 0.9300 ?
O2B N3B . 1.216(5) ?
O1B N3B . 1.236(5) ?
N1B C1B . 1.365(5) ?
N1B C10B . 1.449(5) ?
N1B C7B . 1.464(5) ?
N2B C8B . 1.470(5) ?
N2B C9B . 1.483(5) ?
N2B H2BA . 0.875(18) ?
N2B H2BB . 0.892(18) ?
N3B C4B . 1.456(6) ?
C1B C2B . 1.398(6) ?
C1B C6B . 1.402(5) ?
C2B C3B . 1.372(5) ?
C2B H2B . 0.9300 ?
C3B C4B . 1.363(6) ?
C3B H3B . 0.9300 ?
C4B C5B . 1.369(6) ?
C5B C6B . 1.369(5) ?
C5B H5B . 0.9300 ?
C6B H6B . 0.9300 ?
C7B C8B . 1.505(5) ?
C7B H7BA . 0.9700 ?
C7B H7BB . 0.9700 ?
C8B H8BA . 0.9700 ?
C8B H8BB . 0.9700 ?
C9B C10B . 1.508(5) ?
C9B H9BA . 0.9700 ?
C9B H9BB . 0.9700 ?
C10B H10C . 0.9700 ?
C10B H10D . 0.9700 ?
F1A C14A . 1.363(5) ?
O4A C17A . 1.257(5) ?
O3A C17A . 1.245(4) ?
C11A C12A . 1.379(5) ?
C11A C16A . 1.386(5) ?
C11A C17A . 1.499(6) ?
C16A C15A . 1.380(6) ?
C16A H16A . 0.9300 ?
C15A C14A . 1.346(6) ?
C15A H15A . 0.9300 ?
C14A C13A . 1.365(6) ?
C13A C12A . 1.387(6) ?
C13A H13A . 0.9300 ?
C12A H12A . 0.9300 ?
O5 H5A . 0.843(19) ?
O5 H5D . 0.833(19) ?
O6 H6A . 0.84(2) ?
O6 H6D . 0.84(2) ?
O7 H7A . 0.83(2) ?
O7 H7B . 0.83(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
N2C H2CA O3D . 0.897(19) 1.84(2) 2.733(5) 176(4) yes
N2C H2CB O4A 1_655 0.869(19) 1.87(2) 2.726(5) 166(4) yes
C3C H3C O1C 3 0.93 2.62 3.261(7) 126 yes
C9C H9CA O5 . 0.97 2.51 3.332(6) 142 yes
C9C H9CB O2B . 0.97 2.53 3.401(6) 149 yes
C15D H15D F1A 4_765 0.93 2.52 3.369(5) 152 yes
N2B H2BA O4D 1_455 0.875(18) 1.92(2) 2.764(5) 163(4) yes
N2B H2BB O3A . 0.892(18) 1.86(2) 2.739(5) 169(4) yes
C3B H3B F1D 3_655 0.93 2.63 3.436(6) 145 yes
C8B H8BA O1C . 0.97 2.53 3.437(6) 155 yes
C8B H8BB O6 3 0.97 2.49 3.182(6) 129 yes
C15A H15A F1D 4_466 0.93 2.48 3.310(5) 149 yes
O5 H5A O3A 2 0.843(19) 1.96(2) 2.794(4) 172(5) yes
O5 H5D O4D . 0.833(19) 1.95(2) 2.778(5) 175(5) yes
O6 H6A O4A 3 0.84(2) 2.04(4) 2.795(6) 149(7) yes
O6 H6D O7 . 0.84(2) 1.91(2) 2.744(7) 174(8) yes
O7 H7A O3D . 0.83(2) 1.99(3) 2.794(5) 163(7) yes
O7 H7B O5 3_665 0.83(2) 1.93(2) 2.759(6) 172(7) 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
C7C N1C C1C C2C . . . . 8.1(7) ?
C10C N1C C1C C2C . . . . -175.0(5) ?
C7C N1C C1C C6C . . . . -172.0(4) ?
C10C N1C C1C C6C . . . . 4.9(7) ?
N1C C1C C2C C3C . . . . 178.4(4) ?
C6C C1C C2C C3C . . . . -1.6(7) ?
C1C C2C C3C C4C . . . . 0.3(7) ?
C2C C3C C4C C5C . . . . 1.3(8) ?
C2C C3C C4C N3C . . . . -178.2(4) ?
O1C N3C C4C C5C . . . . -179.5(5) ?
O2C N3C C4C C5C . . . . -0.4(7) ?
O1C N3C C4C C3C . . . . -0.1(7) ?
O2C N3C C4C C3C . . . . 179.0(5) ?
C3C C4C C5C C6C . . . . -1.4(7) ?
N3C C4C C5C C6C . . . . 178.0(4) ?
C4C C5C C6C C1C . . . . 0.0(7) ?
N1C C1C C6C C5C . . . . -178.5(4) ?
C2C C1C C6C C5C . . . . 1.4(7) ?
C1C N1C C7C C8C . . . . -124.1(5) ?
C10C N1C C7C C8C . . . . 58.7(5) ?
C9C N2C C8C C7C . . . . 55.0(5) ?
N1C C7C C8C N2C . . . . -55.7(5) ?
C8C N2C C9C C10C . . . . -55.5(5) ?
C1C N1C C10C C9C . . . . 123.4(5) ?
C7C N1C C10C C9C . . . . -59.4(6) ?
N2C C9C C10C N1C . . . . 56.9(6) ?
C16D C11D C12D C13D . . . . -1.1(8) ?
C17D C11D C12D C13D . . . . 178.1(5) ?
C11D C12D C13D C14D . . . . 0.8(8) ?
C12D C13D C14D C15D . . . . -0.1(9) ?
C12D C13D C14D F1D . . . . -179.0(5) ?
C13D C14D C15D C16D . . . . -0.3(9) ?
F1D C14D C15D C16D . . . . 178.6(4) ?
C14D C15D C16D C11D . . . . -0.1(8) ?
C12D C11D C16D C15D . . . . 0.8(7) ?
C17D C11D C16D C15D . . . . -178.5(5) ?
C12D C11D C17D O3D . . . . -2.2(7) ?
C16D C11D C17D O3D . . . . 177.0(4) ?
C12D C11D C17D O4D . . . . 178.6(4) ?
C16D C11D C17D O4D . . . . -2.2(7) ?
C10B N1B C1B C2B . . . . 167.7(4) ?
C7B N1B C1B C2B . . . . -17.0(7) ?
C10B N1B C1B C6B . . . . -10.8(7) ?
C7B N1B C1B C6B . . . . 164.5(5) ?
N1B C1B C2B C3B . . . . -178.7(4) ?
C6B C1B C2B C3B . . . . -0.1(7) ?
C1B C2B C3B C4B . . . . 0.4(7) ?
C2B C3B C4B C5B . . . . -0.7(7) ?
C2B C3B C4B N3B . . . . 178.8(4) ?
O2B N3B C4B C3B . . . . 178.9(5) ?
O1B N3B C4B C3B . . . . -0.7(7) ?
O2B N3B C4B C5B . . . . -1.6(7) ?
O1B N3B C4B C5B . . . . 178.8(5) ?
C3B C4B C5B C6B . . . . 0.6(7) ?
N3B C4B C5B C6B . . . . -178.9(4) ?
C4B C5B C6B C1B . . . . -0.3(7) ?
N1B C1B C6B C5B . . . . 178.6(4) ?
C2B C1B C6B C5B . . . . 0.0(6) ?
C1B N1B C7B C8B . . . . -116.6(5) ?
C10B N1B C7B C8B . . . . 59.3(5) ?
C9B N2B C8B C7B . . . . 55.5(5) ?
N1B C7B C8B N2B . . . . -56.2(5) ?
C8B N2B C9B C10B . . . . -55.5(5) ?
C1B N1B C10B C9B . . . . 116.0(5) ?
C7B N1B C10B C9B . . . . -59.8(5) ?
N2B C9B C10B N1B . . . . 56.8(5) ?
C12A C11A C16A C15A . . . . -1.5(7) ?
C17A C11A C16A C15A . . . . 178.1(5) ?
C11A C16A C15A C14A . . . . 1.1(8) ?
C16A C15A C14A F1A . . . . 179.4(5) ?
C16A C15A C14A C13A . . . . 0.1(9) ?
C15A C14A C13A C12A . . . . -0.8(9) ?
F1A C14A C13A C12A . . . . 179.8(5) ?
C16A C11A C12A C13A . . . . 0.6(7) ?
C17A C11A C12A C13A . . . . -178.9(5) ?
C14A C13A C12A C11A . . . . 0.4(8) ?
C12A C11A C17A O3A . . . . 8.3(7) ?
C16A C11A C17A O3A . . . . -171.2(4) ?
C12A C11A C17A O4A . . . . -174.1(4) ?
C16A C11A C17A O4A . . . . 6.4(7) ?
_cod_database_fobs_code 2022718