#------------------------------------------------------------------------------
#$Date: 2022-08-27 05:38:19 +0300 (Sat, 27 Aug 2022) $
#$Revision: 277424 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/41/2244153.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_2244153
loop_
_publ_author_name
'Shankara Prasad, Holehundi J.'
Devaraju
Vinaya
'Yathirajan, Hemmige S.'
'Parkin, Sean R.'
'Glidewell, Christopher'
_publ_section_title
;
Syntheses and crystal structures of 4-(4-methoxyphenyl)piperazin-1-ium
4-methylbenzoate monohydrate and bis[4-(4-methoxyphenyl)piperazin-1-ium]
benzene-1,2-dicarboxylate
;
_journal_coeditor_code ZL5034
_journal_issue 9
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989022008337
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac '2C11 H17 N2 O +, C8 H4 O4 2-'
_chemical_formula_moiety '2(C11 H17 N2 O +), C8 H4 O4 2-'
_chemical_formula_sum 'C30 H38 N4 O6'
_chemical_formula_weight 550.64
_chemical_name_systematic
;
Bis[4-(4-methoxyphenyl)piperazin-1-ium] benzene-1,2-dicarboxylate
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 33
_space_group_name_Hall 'P 2c -2n'
_space_group_name_H-M_alt 'P n a 21'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_method SHELXL-2014
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 17.8424(4)
_cell_length_b 8.8124(2)
_cell_length_c 34.9337(9)
_cell_measurement_reflns_used 10053
_cell_measurement_temperature 180(2)
_cell_measurement_theta_max 70.082
_cell_measurement_theta_min 4.957
_cell_volume 5492.8(2)
_computing_cell_refinement
;
APEX3 (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
APEX3 (Bruker, 2016)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015b) and PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014/5 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 180(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type 'Bruker D8 Venture dual source'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'multilayer optics'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0305
_diffrn_reflns_av_unetI/netI 0.0315
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_h_min -21
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 42
_diffrn_reflns_limit_l_min -41
_diffrn_reflns_number 36488
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 70.082
_diffrn_reflns_theta_min 4.957
_diffrn_source microsource
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.763
_exptl_absorpt_correction_T_max 0.942
_exptl_absorpt_correction_T_min 0.814
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.332
_exptl_crystal_description plate
_exptl_crystal_F_000 2352
_exptl_crystal_size_max 0.260
_exptl_crystal_size_mid 0.240
_exptl_crystal_size_min 0.040
_refine_diff_density_max 0.267
_refine_diff_density_min -0.167
_refine_ls_abs_structure_details
;
Flack x determined using 4511 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.45(5)
_refine_ls_extinction_coef 0.0018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method SHELXL
_refine_ls_goodness_of_fit_ref 1.070
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 750
_refine_ls_number_reflns 10053
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.070
_refine_ls_R_factor_all 0.0385
_refine_ls_R_factor_gt 0.0372
_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^)+(0.0511P)^2^+1.5447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0965
_refine_ls_wR_factor_ref 0.0976
_reflns_number_gt 9727
_reflns_number_total 10053
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zl5034sup1.cif
_cod_data_source_block II
_cod_database_code 2244153
_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 0.826
_shelx_estimated_absorpt_t_max 0.970
_shelx_hkl_file
;
1 0 0 0.00600 0.31343 7
1 0 0 0.10935 0.28706 1
3 0 0 0.38395 0.81713 7
3 0 0 -0.1402 0.66896 1
4 0 0 258.713 11.7182 7
4 0 0 269.736 11.6169 1
5 0 0 0.76906 1.25672 7
6 0 0 4379.61 191.102 7
-6 0 0 4830.60 191.601 8
-7 0 0 0.50443 1.82997 5
-7 0 0 0.06014 2.65691 8
7 0 0 -0.2003 1.28365 7
-8 0 0 59.7407 10.8713 8
-8 0 0 61.8285 5.67527 5
-9 0 0 -2.5953 7.92305 5
-9 0 0 -4.8924 6.08368 8
10 0 0 91.4076 4.80734 4
0 1 0 1.50258 0.23586 7
0 1 0 2.07977 0.28358 1
1 1 0 68.7187 3.13075 7
1 -1 0 65.4818 2.82993 1
1 1 0 70.0065 3.09563 1
1 -1 0 64.8999 2.80163 1
2 1 0 3.67174 0.99366 7
2 -1 0 2.58909 0.55966 1
2 1 0 3.24538 0.84644 1
2 -1 0 4.36312 0.66120 7
2 -1 0 2.92279 0.46595 1
3 1 0 1630.03 67.9993 7
3 -1 0 1609.61 67.7362 1
3 1 0 1674.21 67.9684 1
3 -1 0 1616.64 67.7770 7
4 -1 0 1006.50 42.3625 1
4 -1 0 997.592 42.4419 7
4 1 0 1017.55 42.7010 7
4 1 0 1033.23 42.6391 1
5 1 0 487.951 20.0570 1
-5 -1 0 444.654 19.9113 8
5 1 0 468.787 20.1288 7
5 -1 0 458.550 19.8292 7
-5 1 0 442.334 19.8430 8
-6 -1 0 724.878 34.6906 8
6 1 0 847.693 34.4958 7
-6 1 0 809.369 34.2722 8
6 -1 0 828.136 34.1292 7
7 1 0 15.7278 2.14331 4
-7 1 0 18.9434 3.01919 5
7 -1 0 18.5150 2.34803 7
7 1 0 17.7058 2.76255 7
-7 -1 0 18.4644 3.37387 5
-7 -1 0 17.3280 5.45080 8
-7 1 0 18.1385 3.18624 8
-8 -1 0 1.03676 5.05881 5
-8 1 0 2.13835 2.24395 5
-8 -1 0 4.54391 6.63818 8
-8 1 0 2.61454 5.62657 8
8 1 0 3.13849 1.59658 4
-9 1 0 5.94543 6.70984 8
-9 1 0 5.90255 5.86885 5
10 -1 0 39.6988 2.66526 4
0 2 0 50.3366 2.28880 7
0 2 0 41.7320 2.14200 1
1 -2 0 62.0457 2.52068 7
1 -2 0 59.8238 2.58434 7
1 2 0 62.7998 3.12269 7
1 2 0 59.3467 3.08659 1
1 -2 0 55.1247 2.59994 1
2 -2 0 58.5048 2.48377 1
2 2 0 58.4941 3.28883 7
2 2 0 59.4319 3.18006 1
2 -2 0 55.9589 2.57565 7
3 2 0 50.8373 3.25972 7
3 -2 0 52.6439 2.61306 7
-3 -2 0 48.5943 2.69073 1
3 2 0 55.0497 3.21338 1
3 -2 0 52.2463 2.48883 1
4 2 0 1.68278 1.43420 7
4 2 0 2.80174 1.42404 1
4 -2 0 4.09040 0.97936 7
-5 -2 0 71.3851 4.98087 8
5 -2 0 97.0730 4.41298 7
5 2 0 81.6833 4.78736 1
-5 2 0 86.9267 4.74799 8
-6 2 0 47.6266 3.48057 8
6 2 0 46.3004 3.83364 7
6 2 0 48.6624 3.58414 1
6 -2 0 40.5625 2.87995 7
-6 -2 0 49.8573 5.05432 8
6 2 0 48.1935 3.22704 4
-7 -2 0 28.6958 3.70682 5
7 2 0 25.7689 3.02956 7
-7 2 0 24.2224 3.36945 5
-7 2 0 23.8236 3.25935 8
7 2 0 23.9785 2.60038 4
7 -2 0 24.3549 2.25925 7
-7 -2 0 22.6337 6.89602 8
-8 2 0 2.25014 2.16504 5
8 2 0 0.36252 1.51257 4
-8 -2 0 2.88267 7.63626 5
8 -2 0 0.82836 1.33567 4
8 2 0 -1.2768 2.09281 2
-8 -2 0 2.17857 6.07264 8
-8 2 0 1.14073 3.19269 8
-9 2 0 1.64088 6.36628 8
9 -2 0 1.02272 1.22335 4
-9 2 0 0.02545 2.69238 5
9 2 0 2.08727 1.69591 2
10 -2 0 2.38668 1.17558 4
0 3 0 6.80333 1.37187 7
0 3 0 1.78559 0.80064 1
3 -3 0 320.524 13.2615 7
3 -3 0 302.314 13.1777 1
3 3 0 326.274 14.2156 1
-4 -3 0 79.8593 4.04089 1
4 -3 0 79.2133 3.87037 7
4 3 0 90.3023 4.80162 1
4 3 0 90.6724 4.95291 7
-4 3 0 76.1617 4.38268 8
5 3 0 80.4706 4.73026 1
-5 3 0 68.0350 3.91125 8
5 -3 0 55.9207 3.25106 7
5 3 0 58.1570 4.18687 7
-5 -3 0 71.4271 5.27190 8
-6 -3 0 20.5159 4.34492 8
6 -3 0 21.7737 1.96587 7
6 3 0 24.4082 2.99046 1
-6 3 0 23.9688 3.09468 8
6 3 0 26.0505 3.38899 7
7 -3 0 96.0926 4.98574 7
7 3 0 104.384 5.59511 4
-7 3 0 106.710 5.99826 5
7 3 0 97.6346 6.31806 7
-7 -3 0 108.057 9.30594 8
-7 -3 0 114.172 11.0348 5
8 3 0 146.943 8.14823 2
8 -3 0 137.872 7.08248 4
-8 3 0 152.662 8.04937 8
-8 3 0 162.902 7.98756 5
-9 3 0 0.30756 5.65621 8
9 -3 0 2.18672 1.32937 4
-9 3 0 3.72013 2.61485 5
10 -3 0 0.90541 1.22816 4
2 -4 0 336.588 14.5422 1
2 4 0 357.439 15.1602 1
2 4 0 351.226 15.1835 7
2 -4 0 345.032 14.4595 7
3 -4 0 790.444 35.1717 1
3 4 0 871.005 36.0060 1
3 -4 0 876.552 35.2040 7
3 4 0 860.853 36.0801 7
-4 -4 0 17.1049 1.79942 1
4 4 0 15.0955 2.57264 1
4 4 0 16.8447 2.73786 7
-4 4 0 18.9209 2.30817 8
4 -4 0 18.7621 1.30910 7
5 4 0 1494.00 64.5714 7
-5 4 0 1535.36 64.0679 8
5 4 0 1418.29 63.8436 4
5 -4 0 1583.37 63.4657 7
-5 -4 0 1564.45 64.1857 8
5 4 0 1578.14 64.5060 1
6 4 0 2550.04 111.525 4
6 4 0 2728.83 112.394 7
-6 -4 0 2671.05 111.819 8
6 4 0 2651.18 112.156 1
6 -4 0 2746.99 111.035 7
-6 4 0 2731.83 111.766 8
7 -4 0 2.13067 0.92561 7
-7 4 0 -1.1365 1.81652 5
7 4 0 2.50257 2.15786 2
-7 4 0 0.41080 1.81917 8
7 4 0 0.56707 2.07864 7
-8 4 0 25.2907 3.50570 5
8 4 0 22.2593 3.46769 2
-8 4 0 18.1170 3.38020 8
9 -4 0 24.6006 2.24364 4
-9 4 0 21.4593 5.02121 8
-9 4 0 24.7086 3.50583 5
0 5 0 0.27497 0.79646 1
0 5 0 0.53874 0.87368 7
1 5 0 24.1709 2.16873 1
1 -5 0 17.4104 1.67882 7
2 5 0 1173.08 49.5191 1
2 5 0 1195.43 49.5884 7
2 -5 0 1168.52 48.8796 7
3 5 0 620.355 26.2060 7
3 5 0 628.828 26.1499 1
3 -5 0 576.295 25.1787 1
3 -5 0 600.942 25.1918 7
4 -5 0 15.5229 1.10728 7
4 -5 0 13.8928 1.00555 1
-4 5 0 17.1132 2.06502 8
4 5 0 19.4220 2.86431 7
4 5 0 13.2656 2.25322 1
5 5 0 69.0069 4.70582 7
5 5 0 68.4796 4.67678 1
5 5 0 67.3915 4.32083 4
-5 5 0 69.2046 4.14941 8
6 5 0 43.8858 4.14617 7
-6 5 0 40.5985 3.45048 8
6 5 0 38.6112 3.53488 1
-6 5 0 43.4613 3.54004 5
6 5 0 42.6391 3.35794 4
6 -5 0 37.1853 2.22600 7
7 5 0 55.9468 4.01553 4
7 -5 0 49.6441 2.63679 7
-7 5 0 54.4285 4.18343 8
7 5 0 57.4143 4.68998 7
7 5 0 46.0183 4.66154 2
-7 5 0 53.5458 4.34422 5
8 5 0 15.2515 2.75458 2
-8 5 0 18.7617 3.29505 5
-8 5 0 16.7647 3.12472 8
-9 5 0 29.7558 2.79466 5
-9 5 0 27.9129 4.91764 8
-10 5 0 9.98670 3.84810 5
0 6 0 42.0819 2.54393 7
0 6 0 36.4671 2.58276 1
1 6 0 19.0318 2.20132 1
1 -6 0 19.6289 1.77548 7
1 6 0 23.3346 2.46191 7
2 -6 0 42.3470 2.41127 1
2 6 0 45.2933 3.15760 1
2 6 0 45.1797 3.30058 7
3 -6 0 1.72206 0.55845 1
3 6 0 3.49573 1.64064 1
3 6 0 4.41776 1.72522 7
-3 6 0 2.99685 1.21806 8
3 -6 0 5.62352 1.12240 7
4 -6 0 48.9908 2.43893 7
-4 6 0 49.0116 3.31305 8
4 6 0 46.7627 3.60081 1
4 6 0 52.8470 4.14505 7
5 6 0 83.6765 5.47731 7
5 6 0 81.4788 4.61434 4
5 6 0 78.3348 5.06427 1
-5 6 0 78.0083 4.65487 8
5 -6 0 79.5161 3.69552 7
6 6 0 108.339 6.98137 2
6 6 0 113.514 6.73787 1
6 -6 0 118.307 5.20785 7
-6 6 0 124.425 6.39925 8
7 6 0 1.77775 2.21645 2
-7 6 0 -1.0353 1.87391 5
-7 6 0 0.79354 1.83332 8
-8 6 0 6.13717 2.15594 5
-9 6 0 1.43215 2.97264 8
-9 6 0 5.13278 2.01861 5
-10 6 0 15.5670 3.40882 5
0 7 0 1.47720 0.93633 1
1 7 0 113.117 5.85461 1
1 7 0 116.558 5.96507 7
2 7 0 87.6565 5.32605 7
2 7 0 84.7046 5.05500 1
3 -7 0 2.08716 0.71011 1
3 7 0 2.45860 1.59170 1
-3 7 0 4.04456 1.34469 8
3 7 0 3.77160 1.70875 7
-4 7 0 120.193 6.53830 8
4 7 0 129.854 7.44404 1
4 7 0 135.090 7.33361 7
4 -7 0 122.297 5.67058 7
5 7 0 484.846 21.9071 1
5 -7 0 480.655 20.4963 7
-5 7 0 493.923 21.4002 8
5 7 0 491.086 22.2201 7
6 7 0 234.889 12.1178 2
-6 7 0 225.731 12.8125 6
-6 7 0 261.600 11.6916 8
-6 7 0 254.544 11.6176 5
6 7 0 247.805 12.5766 7
6 7 0 242.980 12.2517 1
-7 7 0 34.6481 4.20813 5
7 7 0 34.3839 4.20663 7
-7 7 0 38.9226 3.77278 8
-8 7 0 0.31972 1.95466 5
-8 7 0 -0.0950 1.90278 8
-9 7 0 67.0652 4.40658 5
-9 7 0 67.0443 4.79512 8
-10 7 0 92.8948 6.75865 5
0 8 0 2317.50 96.6719 1
1 8 0 13.9748 2.23649 1
1 8 0 13.3258 2.64431 7
2 8 0 884.768 37.7628 1
2 8 0 884.164 37.8701 7
-3 8 0 173.277 8.43480 8
3 8 0 175.730 8.97077 7
3 8 0 179.443 8.91125 1
4 8 0 276.363 13.4058 1
4 8 0 285.175 12.6343 4
-4 8 0 281.844 13.2767 8
5 8 0 360.452 17.0300 7
-5 8 0 347.709 16.1355 8
5 8 0 366.199 16.8594 1
-6 8 0 556.144 26.6643 6
6 8 0 588.583 26.4137 7
-6 8 0 604.710 25.4582 5
6 8 0 577.250 26.1242 1
-7 8 0 34.1618 3.72551 8
-7 8 0 39.4819 4.85102 6
-7 8 0 38.8278 3.92164 5
-8 8 0 92.4266 5.66471 8
-9 8 0 5.50429 1.42359 5
-9 8 0 6.26069 2.08716 8
1 9 0 299.430 13.5689 1
2 9 0 226.219 11.0189 7
2 9 0 233.192 10.9753 1
3 9 0 56.6856 4.44160 7
-3 9 0 59.9306 4.17439 8
3 9 0 64.8128 4.54508 1
4 9 0 107.450 6.74603 7
-4 9 0 99.5016 5.81401 8
4 9 0 103.908 6.37316 1
-5 9 0 251.312 13.8947 6
5 9 0 278.022 13.5888 7
-5 9 0 267.929 12.5009 8
-6 9 0 80.3871 5.16871 5
6 9 0 65.7474 5.30496 1
6 9 0 72.2618 5.79228 7
-6 9 0 78.3501 5.07673 8
-6 9 0 78.8469 6.76324 6
-7 9 0 18.0726 2.60525 5
-7 9 0 18.1445 3.43612 6
-7 9 0 16.1216 3.24148 8
-8 9 0 0.71312 1.33967 8
-8 9 0 0.80509 1.31543 5
1 10 0 29.9079 2.81349 1
2 10 0 18.5584 2.66559 1
-2 10 0 14.4016 2.41853 8
2 10 0 15.3502 2.75369 7
-2 -10 0 14.7192 2.23732 4
3 10 0 2.96040 1.88138 7
-3 10 0 4.17778 1.89646 8
-3 -10 0 6.44525 1.56208 4
3 10 0 6.25420 2.08675 1
4 10 0 6.49356 1.92213 1
-4 10 0 2.20738 1.71973 8
4 10 0 3.54385 2.13985 7
-5 10 0 23.2010 3.26746 5
5 10 0 29.6713 4.17797 1
-5 10 0 27.9349 3.35634 8
-5 10 0 25.4391 4.57913 6
5 10 0 25.1754 5.10949 7
-6 10 0 4.76442 2.15451 8
6 10 0 0.92526 1.90067 1
-7 10 0 -0.8894 2.29893 6
-7 10 0 1.29248 1.96870 5
-8 10 0 -0.5302 1.73653 8
-8 10 0 0.20422 1.18910 5
-9 10 0 0.59940 1.39477 5
0 -11 0 -0.9417 1.21267 4
1 -11 0 91.5527 5.29404 4
-1 -11 0 109.320 5.90815 4
-2 11 0 868.440 36.7916 8
-2 -11 0 851.555 36.5826 4
2 11 0 850.212 36.9983 1
-3 -11 0 1.00823 1.59847 4
3 11 0 6.46543 2.15179 1
-3 11 0 5.71029 1.87944 8
4 11 0 145.934 8.52824 1
4 11 0 157.434 9.32880 7
-4 11 0 158.313 8.17756 8
5 11 0 179.901 9.87559 1
-5 11 0 183.553 10.7463 6
-5 -11 0 183.715 9.08454 2
5 11 0 162.219 10.2714 7
-5 11 0 190.206 9.40320 8
-5 11 0 191.297 9.23185 5
-6 11 0 18.9155 3.26589 5
-6 11 0 17.4338 3.23086 8
-6 11 0 14.1113 3.17743 6
-7 11 0 1.02919 2.05490 8
-7 11 0 4.54165 2.06888 6
-8 11 0 16.2246 2.72354 8
-8 11 0 19.9253 2.72099 5
-9 11 0 -0.5593 1.18998 5
0 -12 0 18.5943 2.64859 4
-1 -12 0 168.990 8.25717 4
1 -12 0 158.149 8.10688 4
2 -12 0 270.609 12.9981 4
-2 12 0 286.421 13.5043 8
-2 -12 0 285.303 13.1287 4
2 12 0 293.994 13.6372 1
-3 -12 0 1085.45 45.5061 2
3 -12 0 985.211 43.9202 4
-3 12 0 904.662 46.1926 6
-3 12 0 1094.82 44.4971 8
-3 -12 0 1074.78 44.0385 4
3 12 0 1053.24 45.6681 3
3 12 0 1061.20 44.8704 1
4 12 0 153.821 9.81101 3
-4 -12 0 196.186 9.08870 2
-4 12 0 158.979 8.37901 5
4 12 0 150.568 9.02940 1
-5 12 0 5.69927 2.35043 8
5 12 0 5.55098 2.77178 3
-6 12 0 150.024 7.94186 8
-6 12 0 142.906 8.98729 6
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2 -4 -39 16.5394 2.74802 3
3 -4 39 2.22239 1.37284 4
-3 -4 -39 1.40520 1.58556 3
3 4 -39 1.95506 2.11168 3
3 -4 -39 -0.0048 1.80154 3
-3 4 -39 0.25125 1.88016 6
0 -5 39 -0.2179 2.38549 4
0 -5 -39 -0.9750 1.97008 3
0 5 -39 1.80416 2.23031 3
-1 5 39 19.0844 3.54727 3
-1 -5 -39 21.7975 3.37449 3
1 -5 39 18.5866 2.63553 4
1 5 -39 20.6466 3.58886 3
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1 -5 -39 14.9931 2.66351 3
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2 -5 39 30.9849 3.12182 4
-2 -5 -39 30.0543 3.34739 3
2 5 -39 25.3625 3.08900 3
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3 -5 39 26.3764 2.87147 4
3 5 -39 24.8401 3.57815 3
3 -5 -39 16.7724 3.89187 3
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0 6 -39 95.2469 5.45271 3
0 -6 -39 78.4180 5.03053 3
1 6 -39 49.4189 4.21477 3
-1 -6 -39 54.5503 4.17229 3
-1 6 39 48.1604 4.31007 3
1 -6 39 52.4739 3.65189 4
-1 6 -39 50.9749 3.19600 3
1 -6 -39 42.6774 3.65665 3
2 -6 39 -0.3129 1.57328 4
-2 -6 -39 1.66289 1.67548 3
2 6 -39 2.21040 1.99073 3
-2 6 39 2.54494 2.12364 3
-2 6 -39 3.28481 1.69424 6
2 -6 -39 4.40994 1.93549 3
3 -6 39 15.9069 2.73585 4
-3 6 -39 13.1252 2.53896 6
0 -7 -39 0.35010 1.79466 3
0 7 39 1.17018 1.80306 3
0 7 -39 1.03975 1.37454 3
1 7 -39 8.43482 2.19847 3
-1 -7 -39 11.4893 2.11077 3
1 7 39 3.63562 3.35378 3
1 -7 -39 6.33206 2.67912 3
-2 -7 -39 18.5696 2.68665 3
2 7 -39 20.5465 2.98469 3
2 -7 -39 16.7655 3.64801 3
0 8 -39 6.24377 1.23240 3
0 -8 -39 3.16322 1.54611 3
0 8 39 3.62846 1.86291 3
-1 8 39 1.98312 1.81753 3
1 -8 -39 0.68737 1.59671 3
0 0 -40 274.179 13.2119 3
1 0 -40 -2.3544 1.39205 3
-1 0 -40 -0.6410 1.77838 3
-2 0 -40 120.514 6.30488 3
2 0 40 99.1583 6.31577 4
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3 0 -40 -0.4203 1.95196 3
-3 0 -40 0.96656 2.16432 6
0 1 -40 0.03149 1.71416 6
0 -1 -40 1.43175 2.22293 3
0 1 -40 2.65894 2.19630 3
-1 -1 -40 1.91967 1.95178 3
1 -1 40 2.72469 2.20004 4
1 1 -40 2.29691 2.24797 3
1 -1 -40 -0.0426 2.13224 3
-1 1 -40 0.31204 1.75592 6
-1 1 -40 3.75205 2.29484 3
-2 -1 -40 23.4700 3.32604 3
2 1 -40 22.7391 3.80560 3
2 -1 40 23.7159 2.91347 4
-2 1 -40 25.1739 3.58596 6
2 -1 -40 18.0033 2.84283 3
-2 1 -40 25.8960 2.87969 3
3 -1 -40 41.8329 4.06196 3
-3 1 -40 52.0390 4.43172 6
0 2 -40 6.80522 2.26527 3
0 -2 -40 8.57130 2.42067 3
-1 -2 -40 126.834 7.03087 3
1 2 -40 122.978 7.32033 3
-1 2 40 124.962 7.71925 3
-1 2 -40 122.445 7.04580 3
-1 2 -40 122.743 9.43415 6
1 -2 -40 121.868 7.27413 3
-2 -2 -40 58.9919 4.36155 3
2 2 -40 55.0965 4.82372 3
2 -2 40 51.6916 3.64168 4
-2 2 -40 57.4599 4.57736 6
2 -2 -40 58.2004 4.76421 3
-2 2 -40 55.6905 3.71486 3
3 -2 40 84.9663 5.74315 4
3 -2 -40 69.2365 4.69884 3
-3 2 -40 88.5292 8.02940 6
0 3 40 2.23003 2.12617 3
0 3 -40 -0.2419 1.90361 3
0 -3 -40 0.31816 2.05542 3
1 -3 40 20.7494 3.40310 4
1 3 -40 28.1954 3.85634 3
-1 3 40 15.9806 2.99354 3
-1 -3 -40 19.6680 3.32936 3
-1 3 -40 26.2160 3.43056 3
1 -3 -40 22.5992 3.66298 3
-1 3 -40 22.3547 3.13845 6
2 -3 40 1.60452 1.46396 4
-2 -3 -40 3.06166 1.66449 3
2 3 -40 2.33548 1.64220 3
2 -3 -40 5.43547 2.18991 3
3 3 -40 96.2024 8.11545 3
3 -3 -40 87.0842 5.64640 3
-3 3 -40 99.2872 5.79462 6
0 4 40 89.4386 5.70175 3
0 4 -40 95.7867 5.60417 3
0 -4 -40 83.1284 5.27252 3
1 4 -40 4.00284 2.11926 3
-1 4 40 6.45774 2.67925 3
-1 -4 -40 3.16389 1.91926 3
-1 4 -40 2.75275 3.20177 6
1 -4 -40 4.12966 2.15283 3
-1 4 -40 1.01101 1.59164 3
-2 -4 -40 72.0326 4.70906 3
2 -4 40 63.5284 4.90752 4
2 4 -40 65.0485 4.92779 3
-2 4 -40 62.7901 4.59117 6
2 -4 -40 58.6394 6.75415 3
3 4 -40 4.54154 2.05359 3
3 -4 -40 3.19222 2.26606 3
-3 4 -40 7.01579 1.89670 6
0 5 40 -3.5705 1.76862 3
0 -5 -40 -1.4103 1.79318 3
0 5 -40 0.39096 1.50627 3
-1 5 40 9.17298 2.30795 3
1 5 -40 11.7324 2.22919 3
-1 -5 -40 12.1423 2.24589 3
1 -5 -40 8.63124 2.20733 3
-2 -5 -40 39.2842 3.31791 3
-2 5 40 35.2296 3.89931 3
2 -5 40 29.3252 3.37468 4
2 5 -40 40.2938 3.80212 3
-2 5 -40 40.5002 3.13314 6
2 -5 -40 37.5786 3.44228 3
0 6 -40 19.8711 2.65092 3
0 -6 -40 18.2905 2.97183 3
0 6 40 14.2289 2.81815 3
-1 6 40 4.33783 1.90697 3
1 6 -40 3.17150 1.67929 3
-1 -6 -40 1.98340 1.70177 3
1 -6 -40 3.39836 1.82878 3
2 6 -40 49.8183 4.48944 3
-2 -6 -40 48.0615 4.03887 3
-2 6 40 42.0702 3.35169 3
2 -6 -40 42.4228 4.13521 3
0 7 -40 0.28090 1.08847 3
0 -7 -40 2.81356 1.71528 3
-1 7 40 2.52324 1.68808 3
1 -7 -40 1.01099 1.60148 3
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0 1 -41 0.13911 1.94406 3
1 1 -41 22.3860 3.56538 3
-1 -1 -41 19.5996 3.10765 3
-1 1 -41 18.4790 2.91344 6
1 -1 -41 18.2855 3.42342 3
-1 1 -41 21.8807 2.90483 3
-2 -1 -41 60.5985 3.80484 3
2 1 -41 61.0749 4.66550 3
-2 1 -41 52.2407 4.81873 6
2 -1 -41 47.1709 4.54570 3
0 -2 -41 55.2054 4.39957 3
0 2 -41 50.8464 4.27429 3
1 2 -41 10.4078 2.33754 3
-1 -2 -41 9.51914 2.13505 3
-1 2 -41 12.4584 2.13381 3
1 -2 -41 16.5943 3.29188 3
-1 2 -41 9.00492 1.94493 6
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2 2 -41 40.7901 3.96669 3
-2 2 -41 34.3208 3.72058 6
2 -2 -41 39.9259 3.90732 3
0 3 -41 3.25060 2.11562 3
-1 -3 -41 2.26150 1.75649 3
1 3 -41 2.52402 1.98867 3
-1 3 -41 2.83733 1.48654 3
1 -3 -41 4.16151 2.05685 3
2 3 -41 6.53309 2.48294 3
-2 -3 -41 3.53348 1.47462 3
2 -3 -41 2.18982 1.33003 3
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0 -4 -41 54.6473 4.32235 3
0 4 -41 59.8774 4.27503 3
1 4 -41 15.4521 2.65578 3
-1 4 41 19.0000 3.11995 3
-1 -4 -41 18.1870 2.92931 3
2 4 -41 12.5050 3.67859 3
2 -4 -41 11.9742 2.03781 3
-1 -5 -41 6.47368 1.79750 3
-1 5 41 3.15590 1.80697 3
1 5 -41 4.36547 2.29565 3
1 -5 -41 2.54964 1.41811 3
0 0 -42 267.552 12.4749 3
1 0 -42 3.61657 1.91646 3
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0 1 -42 0.38003 1.68272 3
1 1 -42 19.2691 3.06785 3
-1 -1 -42 23.6303 2.72799 3
1 -1 -42 21.2699 3.19679 3
0 -2 -42 324.130 14.8487 3
0 2 -42 328.503 14.6923 3
1 2 -42 26.1984 3.26731 3
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1 -3 -42 1.52508 1.72614 3
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0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 25531
_shelx_res_file
;
TITL hsy6cgm
CELL 1.54178 17.8424 8.8124 34.9337 90.000 90.000 90.000
ZERR 8 0.0004 0.0002 0.0009 0.000 0.000 0.000
LATT -1
SYMM -X, -Y, 1/2+Z
SYMM 1/2+X, 1/2-Y, Z
SYMM 1/2-X, 1/2+Y, 1/2+Z
SFAC C H N O
UNIT 240 304 32 48
TEMP -93
SIZE 0.26 0.24 0.04
L.S. 20
ACTA
BOND $H
CONF
HTAB
LIST 4
FMAP 2
PLAN 20
MPLA 6 C141 > C147
MPLA 6 C241 > C247
MPLA 6 C341 > C347
MPLA 6 C441 > C447
WGHT 0.051100 1.544700
EXTI 0.001771
FVAR 0.49806
MOLE 1
N11 3 0.871336 0.754971 0.461607 11.00000 0.02250 0.03524 =
0.02394 -0.00438 0.00182 -0.00279
H11 2 0.864171 0.778206 0.489054 11.00000 -1.20000
H12 2 0.908742 0.798533 0.456343 11.00000 -1.20000
C12 1 0.805525 0.809052 0.439025 11.00000 0.02735 0.03632 =
0.03222 -0.00774 -0.00264 0.00804
AFIX 23
H12A 2 0.801914 0.920901 0.440931 11.00000 -1.20000
H12B 2 0.759024 0.765034 0.449785 11.00000 -1.20000
AFIX 0
C13 1 0.812863 0.763624 0.397404 11.00000 0.03389 0.02275 =
0.02893 -0.00078 -0.00262 0.00537
AFIX 23
H13A 2 0.766896 0.793072 0.383378 11.00000 -1.20000
H13B 2 0.855770 0.817826 0.385746 11.00000 -1.20000
AFIX 0
N14 3 0.824337 0.599861 0.394001 11.00000 0.02249 0.02198 =
0.02595 0.00026 -0.00298 0.00253
C15 1 0.893380 0.555822 0.413229 11.00000 0.02451 0.02455 =
0.03101 0.00052 -0.00325 0.00537
AFIX 23
H15A 2 0.936243 0.612593 0.402331 11.00000 -1.20000
H15B 2 0.902638 0.446029 0.409533 11.00000 -1.20000
AFIX 0
C16 1 0.885719 0.590866 0.455480 11.00000 0.03075 0.03151 =
0.02695 0.00544 -0.00476 -0.00280
AFIX 23
H16A 2 0.843880 0.530990 0.466358 11.00000 -1.20000
H16B 2 0.932298 0.561239 0.468944 11.00000 -1.20000
AFIX 0
C141 1 0.812242 0.539964 0.356828 11.00000 0.02373 0.01998 =
0.02542 0.00267 -0.00189 -0.00028
C142 1 0.739821 0.549712 0.341521 11.00000 0.02144 0.03612 =
0.04081 -0.00779 -0.00352 0.00552
AFIX 43
H142 2 0.701438 0.598958 0.355694 11.00000 -1.20000
AFIX 0
C143 1 0.723600 0.488755 0.306169 11.00000 0.02833 0.03919 =
0.04098 -0.00587 -0.01185 0.00708
AFIX 43
H143 2 0.674241 0.497287 0.296201 11.00000 -1.20000
AFIX 0
C144 1 0.778477 0.414804 0.284820 11.00000 0.03721 0.02840 =
0.02568 0.00112 -0.00491 0.00413
C145 1 0.849932 0.404651 0.299465 11.00000 0.03128 0.03030 =
0.02786 0.00033 0.00349 0.00468
AFIX 43
H145 2 0.888026 0.354623 0.285263 11.00000 -1.20000
AFIX 0
C146 1 0.866570 0.467720 0.335155 11.00000 0.02269 0.02940 =
0.02862 0.00105 -0.00156 0.00077
AFIX 43
H146 2 0.916258 0.460904 0.344774 11.00000 -1.20000
AFIX 0
O144 4 0.755686 0.357696 0.250051 11.00000 0.05089 0.04961 =
0.03388 -0.01239 -0.01158 0.01201
C147 1 0.807025 0.260072 0.230977 11.00000 0.04543 0.03782 =
0.03039 -0.00463 0.00098 -0.00481
AFIX 137
H17A 2 0.853287 0.315739 0.225368 11.00000 -1.50000
H17B 2 0.784672 0.224205 0.207003 11.00000 -1.50000
H17C 2 0.818486 0.173009 0.247420 11.00000 -1.50000
AFIX 0
MOLE 2
N21 3 0.628707 0.745464 1.036198 11.00000 0.02391 0.03598 =
0.02549 -0.00679 -0.00136 0.00277
H21 2 0.622231 0.722063 1.008772 11.00000 -1.20000
H22 2 0.676121 0.689484 1.043640 11.00000 -1.20000
C22 1 0.563048 0.692086 1.058993 11.00000 0.02871 0.03279 =
0.03629 -0.00956 0.00286 -0.00428
AFIX 23
H22A 2 0.558921 0.580356 1.056922 11.00000 -1.20000
H22B 2 0.516584 0.737162 1.048476 11.00000 -1.20000
AFIX 0
C23 1 0.571038 0.736163 1.100619 11.00000 0.03084 0.02451 =
0.03030 -0.00272 0.00439 -0.00535
AFIX 23
H23A 2 0.524962 0.707727 1.114684 11.00000 -1.20000
H23B 2 0.613612 0.680296 1.112094 11.00000 -1.20000
AFIX 0
N24 3 0.583787 0.899542 1.104339 11.00000 0.02426 0.02317 =
0.02375 -0.00153 0.00217 -0.00146
C25 1 0.652611 0.941777 1.084824 11.00000 0.03072 0.02698 =
0.02447 -0.00096 0.00731 -0.00365
AFIX 23
H25A 2 0.695186 0.882835 1.095273 11.00000 -1.20000
H25B 2 0.662994 1.050994 1.088815 11.00000 -1.20000
AFIX 0
C26 1 0.643732 0.909312 1.042576 11.00000 0.03237 0.03524 =
0.02539 0.00370 0.00288 0.00300
AFIX 23
H26A 2 0.601757 0.970144 1.032183 11.00000 -1.20000
H26B 2 0.690030 0.938989 1.028867 11.00000 -1.20000
AFIX 0
C241 1 0.571532 0.959713 1.141485 11.00000 0.02461 0.02154 =
0.02276 0.00233 0.00045 0.00150
C242 1 0.499421 0.953198 1.156524 11.00000 0.02520 0.03114 =
0.03490 -0.00456 -0.00014 -0.00315
AFIX 43
H242 2 0.461032 0.904138 1.142314 11.00000 -1.20000
AFIX 0
C243 1 0.482333 1.016385 1.191630 11.00000 0.02637 0.03908 =
0.04150 -0.00526 0.01093 -0.00042
AFIX 43
H243 2 0.432650 1.010041 1.201277 11.00000 -1.20000
AFIX 0
C244 1 0.537643 1.089489 1.213006 11.00000 0.03621 0.02545 =
0.02681 -0.00022 0.00804 0.00451
C245 1 0.609584 1.097679 1.198611 11.00000 0.03234 0.02780 =
0.02652 -0.00152 -0.00112 -0.00305
AFIX 43
H245 2 0.647704 1.147568 1.212826 11.00000 -1.20000
AFIX 0
C246 1 0.626403 1.032609 1.163123 11.00000 0.02486 0.02849 =
0.02861 0.00179 0.00356 -0.00272
AFIX 43
H246 2 0.676186 1.038201 1.153582 11.00000 -1.20000
AFIX 0
O244 4 0.514932 1.148975 1.247455 11.00000 0.04625 0.04357 =
0.03239 -0.00964 0.01214 0.00265
C247 1 0.569019 1.230814 1.269053 11.00000 0.06413 0.03679 =
0.02912 -0.00851 -0.00077 0.00865
AFIX 137
H27A 2 0.609365 1.162054 1.276893 11.00000 -1.50000
H27B 2 0.545134 1.274130 1.291829 11.00000 -1.50000
H27C 2 0.589845 1.312679 1.253325 11.00000 -1.50000
AFIX 0
MOLE 3
N31 3 0.596502 0.717359 0.526261 11.00000 0.02126 0.02930 =
0.02766 0.00053 -0.00299 -0.00548
H31 2 0.578384 0.717505 0.500985 11.00000 -1.20000
H32 2 0.639614 0.773971 0.527223 11.00000 -1.20000
C32 1 0.616585 0.555532 0.533202 11.00000 0.03137 0.02987 =
0.02608 -0.00246 0.00140 0.00217
AFIX 23
H32A 2 0.658877 0.526702 0.516360 11.00000 -1.20000
H32B 2 0.573294 0.490139 0.526713 11.00000 -1.20000
AFIX 0
C33 1 0.638471 0.529691 0.574593 11.00000 0.02765 0.02979 =
0.02834 -0.00363 0.00211 0.00705
AFIX 23
H33A 2 0.649108 0.420695 0.578788 11.00000 -1.20000
H33B 2 0.684503 0.587810 0.580545 11.00000 -1.20000
AFIX 0
N34 3 0.577703 0.578272 0.599900 11.00000 0.02492 0.02499 =
0.02428 -0.00283 -0.00059 0.00353
C35 1 0.562052 0.740282 0.594252 11.00000 0.03083 0.02265 =
0.03175 -0.00287 0.00214 0.00383
AFIX 23
H35A 2 0.607616 0.800095 0.600073 11.00000 -1.20000
H35B 2 0.521971 0.772743 0.612057 11.00000 -1.20000
AFIX 0
C36 1 0.537832 0.770645 0.553507 11.00000 0.02550 0.02981 =
0.03211 0.00146 -0.00107 0.00024
AFIX 23
H36A 2 0.490120 0.717197 0.548265 11.00000 -1.20000
H36B 2 0.529339 0.880758 0.549939 11.00000 -1.20000
AFIX 0
C341 1 0.583802 0.532925 0.638676 11.00000 0.02631 0.02189 =
0.02517 -0.00362 -0.00118 -0.00085
C342 1 0.645663 0.455691 0.653287 11.00000 0.03036 0.03533 =
0.02797 -0.00208 0.00452 0.00962
AFIX 43
H342 2 0.687430 0.437188 0.637080 11.00000 -1.20000
AFIX 0
C343 1 0.647863 0.405001 0.690962 11.00000 0.04057 0.03908 =
0.03335 -0.00209 -0.00320 0.01465
AFIX 43
H343 2 0.690141 0.350360 0.700087 11.00000 -1.20000
AFIX 0
C344 1 0.588386 0.434467 0.714982 11.00000 0.04765 0.03024 =
0.02460 -0.00235 0.00256 0.00271
C345 1 0.527566 0.513759 0.700971 11.00000 0.04216 0.04130 =
0.03516 -0.00111 0.00970 0.00897
AFIX 43
H345 2 0.486848 0.536004 0.717570 11.00000 -1.20000
AFIX 0
C346 1 0.524648 0.561206 0.663533 11.00000 0.03043 0.04110 =
0.03372 0.00183 0.00297 0.01010
AFIX 43
H346 2 0.481682 0.613962 0.654542 11.00000 -1.20000
AFIX 0
O344 4 0.587486 0.397513 0.753367 11.00000 0.07824 0.04498 =
0.02647 0.00687 0.00654 0.01754
C347 1 0.614364 0.251133 0.763433 11.00000 0.06274 0.03526 =
0.03222 0.00799 -0.00688 -0.00035
AFIX 137
H37A 2 0.584431 0.173646 0.750350 11.00000 -1.50000
H37B 2 0.610252 0.237210 0.791186 11.00000 -1.50000
H37C 2 0.666953 0.241551 0.755708 11.00000 -1.50000
AFIX 0
MOLE 4
N41 3 0.353474 0.783421 0.967440 11.00000 0.02289 0.02983 =
0.03234 -0.00003 0.00349 0.00362
H41 2 0.333292 0.780415 0.994035 11.00000 -1.20000
H42 2 0.394388 0.722964 0.966033 11.00000 -1.20000
C42 1 0.376141 0.943571 0.960967 11.00000 0.02791 0.03104 =
0.03421 -0.00422 -0.00222 -0.00076
AFIX 23
H42A 2 0.419268 0.968311 0.977670 11.00000 -1.20000
H42B 2 0.334163 1.011546 0.967995 11.00000 -1.20000
AFIX 0
C43 1 0.397503 0.970900 0.919720 11.00000 0.02736 0.03154 =
0.03370 -0.00147 -0.00318 -0.00626
AFIX 23
H43A 2 0.409960 1.079378 0.916004 11.00000 -1.20000
H43B 2 0.442389 0.910053 0.913246 11.00000 -1.20000
AFIX 0
N44 3 0.336056 0.929074 0.894653 11.00000 0.02486 0.02394 =
0.03133 -0.00272 -0.00177 -0.00330
C45 1 0.318639 0.767518 0.899050 11.00000 0.02857 0.02531 =
0.03792 -0.00590 -0.00125 -0.00048
AFIX 23
H45A 2 0.363392 0.706238 0.892594 11.00000 -1.20000
H45B 2 0.277896 0.739147 0.881192 11.00000 -1.20000
AFIX 0
C46 1 0.294729 0.734002 0.939666 11.00000 0.02327 0.02670 =
0.04448 -0.00164 0.00234 -0.00358
AFIX 23
H46A 2 0.247225 0.787663 0.945253 11.00000 -1.20000
H46B 2 0.285744 0.623739 0.942560 11.00000 -1.20000
AFIX 0
C441 1 0.338563 0.984722 0.856472 11.00000 0.02720 0.02422 =
0.02825 -0.00654 0.00092 0.00054
C442 1 0.399030 1.061867 0.841168 11.00000 0.02469 0.02860 =
0.03502 -0.00435 -0.00267 -0.00201
AFIX 43
H442 2 0.444174 1.068242 0.855497 11.00000 -1.20000
AFIX 0
C443 1 0.395455 1.131025 0.805008 11.00000 0.03192 0.03008 =
0.03420 -0.00293 0.00240 -0.00292
AFIX 43
H443 2 0.437543 1.184791 0.795339 11.00000 -1.20000
AFIX 0
C444 1 0.330678 1.120810 0.783504 11.00000 0.03895 0.02907 =
0.02866 -0.00572 -0.00127 0.00129
C445 1 0.270561 1.036948 0.797822 11.00000 0.03304 0.03757 =
0.03465 -0.00754 -0.00793 0.00058
AFIX 43
H445 2 0.226540 1.025234 0.782812 11.00000 -1.20000
AFIX 0
C446 1 0.274436 0.971038 0.833483 11.00000 0.02565 0.03533 =
0.03367 -0.00414 -0.00044 -0.00508
AFIX 43
H446 2 0.232729 0.914985 0.842748 11.00000 -1.20000
AFIX 0
O447 4 0.319005 1.187033 0.748354 11.00000 0.04594 0.04349 =
0.03276 0.00284 -0.00399 0.00140
C447 1 0.379433 1.273010 0.732646 11.00000 0.05847 0.03861 =
0.03437 0.00536 0.00353 0.00087
AFIX 137
H47A 2 0.423613 1.207810 0.729948 11.00000 -1.50000
H47B 2 0.391235 1.357906 0.749734 11.00000 -1.50000
H47C 2 0.364937 1.312340 0.707472 11.00000 -1.50000
AFIX 0
MOLE 5
C51 1 0.778132 0.927391 0.584295 11.00000 0.02060 0.02170 =
0.02302 -0.00135 -0.00079 -0.00327
C52 1 0.721446 1.034778 0.590168 11.00000 0.02060 0.02126 =
0.02709 -0.00206 0.00281 -0.00469
C53 1 0.706256 1.083652 0.627390 11.00000 0.02558 0.02992 =
0.03138 -0.00419 0.00653 -0.00297
AFIX 43
H53 2 0.667451 1.155524 0.631632 11.00000 -1.20000
AFIX 0
C54 1 0.747013 1.028795 0.658305 11.00000 0.04237 0.03405 =
0.02660 -0.00629 0.00626 -0.00408
AFIX 43
H54 2 0.735627 1.061964 0.683519 11.00000 -1.20000
AFIX 0
C55 1 0.804259 0.925662 0.652245 11.00000 0.04444 0.03206 =
0.02386 0.00145 -0.00603 -0.00389
AFIX 43
H55 2 0.833064 0.889275 0.673193 11.00000 -1.20000
AFIX 0
C56 1 0.819344 0.875664 0.615331 11.00000 0.02729 0.02321 =
0.03026 -0.00087 -0.00010 0.00136
AFIX 43
H56 2 0.858627 0.804703 0.611264 11.00000 -1.20000
AFIX 0
C57 1 0.792591 0.858675 0.545005 11.00000 0.02063 0.02079 =
0.02330 -0.00209 0.00146 -0.00021
O51 4 0.858831 0.825309 0.536986 11.00000 0.02585 0.07502 =
0.03170 -0.01787 -0.00329 0.01494
O52 4 0.737738 0.836673 0.523622 11.00000 0.02158 0.05083 =
0.02919 -0.01240 -0.00003 -0.00742
C58 1 0.679391 1.111781 0.557568 11.00000 0.02058 0.02354 =
0.03335 -0.00356 -0.00144 0.00026
O53 4 0.720159 1.188056 0.534945 11.00000 0.02647 0.03368 =
0.03436 0.00842 -0.00648 -0.00338
O54 4 0.610566 1.103766 0.556631 11.00000 0.01783 0.05556 =
0.05583 0.01038 -0.00163 0.00192
MOLE 6
C61 1 0.537543 0.576308 0.912670 11.00000 0.01780 0.01883 =
0.02438 -0.00113 -0.00090 0.00371
C62 1 0.480632 0.470451 0.905660 11.00000 0.01683 0.02217 =
0.02398 -0.00111 0.00001 0.00312
C63 1 0.467082 0.422476 0.868445 11.00000 0.02503 0.02473 =
0.02862 -0.00318 -0.00489 0.00074
AFIX 43
H63 2 0.427987 0.351762 0.863689 11.00000 -1.20000
AFIX 0
C64 1 0.509441 0.475759 0.838231 11.00000 0.03479 0.03209 =
0.01983 -0.00265 -0.00327 0.00653
AFIX 43
H64 2 0.499151 0.442334 0.812917 11.00000 -1.20000
AFIX 0
C65 1 0.567081 0.578216 0.844872 11.00000 0.03172 0.03020 =
0.02519 0.00542 0.00432 0.00248
AFIX 43
H65 2 0.596757 0.614230 0.824201 11.00000 -1.20000
AFIX 0
C66 1 0.581133 0.627899 0.882048 11.00000 0.02560 0.02107 =
0.02682 0.00057 0.00314 0.00080
AFIX 43
H66 2 0.620752 0.697574 0.886645 11.00000 -1.20000
AFIX 0
C67 1 0.550325 0.643887 0.951870 11.00000 0.02230 0.02241 =
0.02535 -0.00154 -0.00054 0.00139
O61 4 0.616081 0.679850 0.960785 11.00000 0.02178 0.06988 =
0.03068 -0.01688 0.00180 -0.01231
O62 4 0.494578 0.662861 0.973232 11.00000 0.02071 0.04859 =
0.02814 -0.01119 0.00007 0.00550
C68 1 0.437767 0.392655 0.937377 11.00000 0.02084 0.02382 =
0.02658 -0.00279 0.00082 -0.00068
O63 4 0.477751 0.310991 0.959793 11.00000 0.02476 0.03445 =
0.02956 0.00629 0.00496 0.00593
O64 4 0.369204 0.403765 0.939071 11.00000 0.01812 0.05556 =
0.04359 0.00916 0.00272 -0.00059
HKLF 4 1 0 1 0 1 0 0 0 0 -1
REM hsy6cgm
REM R1 = 0.0372 for 9727 Fo > 4sig(Fo) and 0.0385 for all 10053 data
REM 750 parameters refined using 1 restraints
END
WGHT 0.0511 1.5449
REM Instructions for potential hydrogen bonds
HTAB N11 O51
HTAB N11 O52
EQIV $1 -x+3/2, y+1/2, z-1/2
HTAB N11 O63_$1
EQIV $2 x+1/2, -y+3/2, z-1
HTAB C145 O244_$2
HTAB N21 O61
HTAB N21 O62
EQIV $3 -x+3/2, y-1/2, z+1/2
HTAB N21 O53_$3
EQIV $4 -x+1, -y+1, z-1/2
HTAB N31 O63_$4
HTAB N31 O64_$4
HTAB N31 O52
HTAB C32 O62_$4
EQIV $5 x-1/2, -y+3/2, z
HTAB C36 O51_$5
HTAB C36 O54
EQIV $6 -x+1, -y+2, z+1/2
HTAB N41 O53_$6
HTAB N41 O54_$6
HTAB N41 O62
HTAB C46 O61_$5
HTAB C46 O64
REM Highest difference peak 0.267, deepest hole -0.167, 1-sigma level 0.040
Q1 1 0.6448 0.3740 0.5555 11.00000 0.05 0.27
Q2 1 0.7549 1.3167 0.5372 11.00000 0.05 0.25
Q3 1 0.3312 1.0998 0.9371 11.00000 0.05 0.23
Q4 1 0.4383 0.1816 0.9568 11.00000 0.05 0.23
Q5 1 0.3043 0.5610 0.8962 11.00000 0.05 0.23
Q6 1 0.4339 1.0954 0.8650 11.00000 0.05 0.22
Q7 1 0.5074 0.6419 0.7487 11.00000 0.05 0.22
Q8 1 0.4634 0.8262 0.9730 11.00000 0.05 0.22
Q9 1 0.8325 0.6482 0.5428 11.00000 0.05 0.21
Q10 1 0.7102 0.3841 0.5583 11.00000 0.05 0.21
Q11 1 0.4607 0.4518 0.6432 11.00000 0.05 0.20
Q12 1 0.3961 1.1036 0.9371 11.00000 0.05 0.20
Q13 1 0.5796 0.8288 0.9620 11.00000 0.05 0.20
Q14 1 0.5104 0.8646 0.9541 11.00000 0.05 0.19
Q15 1 0.6508 1.1096 1.1178 11.00000 0.05 0.19
Q16 1 0.8943 0.6554 0.5383 11.00000 0.05 0.19
Q17 1 0.6490 0.6218 0.3026 11.00000 0.05 0.19
Q18 1 0.7731 0.6695 0.5241 11.00000 0.05 0.19
Q19 1 0.4450 1.0369 0.9073 11.00000 0.05 0.19
Q20 1 0.4919 0.5995 0.7192 11.00000 0.05 0.19
;
_shelx_res_checksum 15697
_shelxl_version_number 2.014
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'
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
N N11 0.87134(14) 0.7550(3) 0.46161(8) 0.0272(5) Uani d 1 . .
H H11 0.8642(18) 0.778(4) 0.4891(11) 0.033 Uiso d 1 . .
H H12 0.909(2) 0.799(4) 0.4563(10) 0.033 Uiso d 1 . .
C C12 0.80552(16) 0.8091(3) 0.43903(9) 0.0320(6) Uani d 1 . .
H H12A 0.8019 0.9209 0.4409 0.038 Uiso calc 1 . .
H H12B 0.7590 0.7650 0.4498 0.038 Uiso calc 1 . .
C C13 0.81286(17) 0.7636(3) 0.39740(8) 0.0285(6) Uani d 1 . .
H H13A 0.7669 0.7931 0.3834 0.034 Uiso calc 1 . .
H H13B 0.8558 0.8178 0.3857 0.034 Uiso calc 1 . .
N N14 0.82434(12) 0.5999(2) 0.39400(6) 0.0235(5) Uani d 1 . .
C C15 0.89338(15) 0.5558(3) 0.41323(8) 0.0267(6) Uani d 1 . .
H H15A 0.9362 0.6126 0.4023 0.032 Uiso calc 1 . .
H H15B 0.9026 0.4460 0.4095 0.032 Uiso calc 1 . .
C C16 0.88572(16) 0.5909(3) 0.45548(8) 0.0297(6) Uani d 1 . .
H H16A 0.8439 0.5310 0.4664 0.036 Uiso calc 1 . .
H H16B 0.9323 0.5612 0.4689 0.036 Uiso calc 1 . .
C C141 0.81224(15) 0.5400(3) 0.35683(7) 0.0230(5) Uani d 1 . .
C C142 0.73982(16) 0.5497(4) 0.34152(9) 0.0328(6) Uani d 1 . .
H H142 0.7014 0.5990 0.3557 0.039 Uiso calc 1 . .
C C143 0.72360(18) 0.4888(4) 0.30617(10) 0.0362(7) Uani d 1 . .
H H143 0.6742 0.4973 0.2962 0.043 Uiso calc 1 . .
C C144 0.77848(17) 0.4148(3) 0.28482(8) 0.0304(6) Uani d 1 . .
C C145 0.84993(16) 0.4047(3) 0.29947(8) 0.0298(6) Uani d 1 . .
H H145 0.8880 0.3546 0.2853 0.036 Uiso calc 1 . .
C C146 0.86657(15) 0.4677(3) 0.33516(8) 0.0269(6) Uani d 1 . .
H H146 0.9163 0.4609 0.3448 0.032 Uiso calc 1 . .
O O144 0.75569(14) 0.3577(3) 0.25005(7) 0.0448(6) Uani d 1 . .
C C147 0.80702(19) 0.2601(4) 0.23098(9) 0.0379(7) Uani d 1 . .
H H17A 0.8533 0.3157 0.2254 0.057 Uiso calc 1 . .
H H17B 0.7847 0.2242 0.2070 0.057 Uiso calc 1 . .
H H17C 0.8185 0.1730 0.2474 0.057 Uiso calc 1 . .
N N21 0.62871(13) 0.7455(3) 1.03620(8) 0.0285(5) Uani d 1 . .
H H21 0.6222(19) 0.722(4) 1.0088(11) 0.034 Uiso d 1 . .
H H22 0.676(2) 0.689(4) 1.0436(10) 0.034 Uiso d 1 . .
C C22 0.56305(16) 0.6921(3) 1.05899(9) 0.0326(6) Uani d 1 . .
H H22A 0.5589 0.5804 1.0569 0.039 Uiso calc 1 . .
H H22B 0.5166 0.7372 1.0485 0.039 Uiso calc 1 . .
C C23 0.57104(16) 0.7362(3) 1.10062(8) 0.0286(6) Uani d 1 . .
H H23A 0.5250 0.7077 1.1147 0.034 Uiso calc 1 . .
H H23B 0.6136 0.6803 1.1121 0.034 Uiso calc 1 . .
N N24 0.58379(12) 0.8995(2) 1.10434(6) 0.0237(5) Uani d 1 . .
C C25 0.65261(16) 0.9418(3) 1.08482(8) 0.0274(6) Uani d 1 . .
H H25A 0.6952 0.8828 1.0953 0.033 Uiso calc 1 . .
H H25B 0.6630 1.0510 1.0888 0.033 Uiso calc 1 . .
C C26 0.64373(17) 0.9093(3) 1.04258(8) 0.0310(6) Uani d 1 . .
H H26A 0.6018 0.9701 1.0322 0.037 Uiso calc 1 . .
H H26B 0.6900 0.9390 1.0289 0.037 Uiso calc 1 . .
C C241 0.57153(15) 0.9597(3) 1.14149(8) 0.0230(5) Uani d 1 . .
C C242 0.49942(16) 0.9532(3) 1.15652(9) 0.0304(6) Uani d 1 . .
H H242 0.4610 0.9041 1.1423 0.036 Uiso calc 1 . .
C C243 0.48233(17) 1.0164(4) 1.19163(10) 0.0356(7) Uani d 1 . .
H H243 0.4327 1.0100 1.2013 0.043 Uiso calc 1 . .
C C244 0.53764(17) 1.0895(3) 1.21301(8) 0.0295(6) Uani d 1 . .
C C245 0.60958(16) 1.0977(3) 1.19861(8) 0.0289(6) Uani d 1 . .
H H245 0.6477 1.1476 1.2128 0.035 Uiso calc 1 . .
C C246 0.62640(15) 1.0326(3) 1.16312(8) 0.0273(6) Uani d 1 . .
H H246 0.6762 1.0382 1.1536 0.033 Uiso calc 1 . .
O O244 0.51493(13) 1.1490(3) 1.24745(6) 0.0407(5) Uani d 1 . .
C C247 0.5690(2) 1.2308(4) 1.26905(10) 0.0433(8) Uani d 1 . .
H H27A 0.6094 1.1621 1.2769 0.065 Uiso calc 1 . .
H H27B 0.5451 1.2741 1.2918 0.065 Uiso calc 1 . .
H H27C 0.5898 1.3127 1.2533 0.065 Uiso calc 1 . .
N N31 0.59650(13) 0.7174(3) 0.52626(7) 0.0261(5) Uani d 1 . .
H H31 0.5784(19) 0.718(4) 0.5010(10) 0.031 Uiso d 1 . .
H H32 0.640(2) 0.774(4) 0.5272(10) 0.031 Uiso d 1 . .
C C32 0.61659(16) 0.5555(3) 0.53320(8) 0.0291(6) Uani d 1 . .
H H32A 0.6589 0.5267 0.5164 0.035 Uiso calc 1 . .
H H32B 0.5733 0.4901 0.5267 0.035 Uiso calc 1 . .
C C33 0.63847(16) 0.5297(3) 0.57459(8) 0.0286(6) Uani d 1 . .
H H33A 0.6491 0.4207 0.5788 0.034 Uiso calc 1 . .
H H33B 0.6845 0.5878 0.5805 0.034 Uiso calc 1 . .
N N34 0.57770(13) 0.5783(3) 0.59990(6) 0.0247(5) Uani d 1 . .
C C35 0.56205(17) 0.7403(3) 0.59425(9) 0.0284(6) Uani d 1 . .
H H35A 0.6076 0.8001 0.6001 0.034 Uiso calc 1 . .
H H35B 0.5220 0.7727 0.6121 0.034 Uiso calc 1 . .
C C36 0.53783(16) 0.7706(3) 0.55351(8) 0.0291(6) Uani d 1 . .
H H36A 0.4901 0.7172 0.5483 0.035 Uiso calc 1 . .
H H36B 0.5293 0.8808 0.5499 0.035 Uiso calc 1 . .
C C341 0.58380(15) 0.5329(3) 0.63868(8) 0.0245(5) Uani d 1 . .
C C342 0.64566(17) 0.4557(3) 0.65329(8) 0.0312(6) Uani d 1 . .
H H342 0.6874 0.4372 0.6371 0.037 Uiso calc 1 . .
C C343 0.64786(19) 0.4050(4) 0.69096(9) 0.0377(7) Uani d 1 . .
H H343 0.6901 0.3504 0.7001 0.045 Uiso calc 1 . .
C C344 0.58839(19) 0.4345(3) 0.71498(8) 0.0342(7) Uani d 1 . .
C C345 0.52757(19) 0.5138(4) 0.70097(10) 0.0395(7) Uani d 1 . .
H H345 0.4868 0.5360 0.7176 0.047 Uiso calc 1 . .
C C346 0.52465(17) 0.5612(4) 0.66353(9) 0.0351(7) Uani d 1 . .
H H346 0.4817 0.6140 0.6545 0.042 Uiso calc 1 . .
O O344 0.58749(16) 0.3975(3) 0.75337(6) 0.0499(6) Uani d 1 . .
C C347 0.6144(2) 0.2511(4) 0.76343(10) 0.0434(8) Uani d 1 . .
H H37A 0.5844 0.1736 0.7504 0.065 Uiso calc 1 . .
H H37B 0.6103 0.2372 0.7912 0.065 Uiso calc 1 . .
H H37C 0.6670 0.2416 0.7557 0.065 Uiso calc 1 . .
N N41 0.35347(13) 0.7834(3) 0.96744(7) 0.0284(5) Uani d 1 . .
H H41 0.3333(19) 0.780(4) 0.9940(11) 0.034 Uiso d 1 . .
H H42 0.394(2) 0.723(4) 0.9660(10) 0.034 Uiso d 1 . .
C C42 0.37614(16) 0.9436(3) 0.96097(9) 0.0311(6) Uani d 1 . .
H H42A 0.4193 0.9683 0.9777 0.037 Uiso calc 1 . .
H H42B 0.3342 1.0115 0.9680 0.037 Uiso calc 1 . .
C C43 0.39750(16) 0.9709(3) 0.91972(9) 0.0309(6) Uani d 1 . .
H H43A 0.4100 1.0794 0.9160 0.037 Uiso calc 1 . .
H H43B 0.4424 0.9101 0.9132 0.037 Uiso calc 1 . .
N N44 0.33606(13) 0.9291(2) 0.89465(7) 0.0267(5) Uani d 1 . .
C C45 0.31864(16) 0.7675(3) 0.89905(9) 0.0306(6) Uani d 1 . .
H H45A 0.3634 0.7062 0.8926 0.037 Uiso calc 1 . .
H H45B 0.2779 0.7391 0.8812 0.037 Uiso calc 1 . .
C C46 0.29473(16) 0.7340(3) 0.93967(10) 0.0315(6) Uani d 1 . .
H H46A 0.2472 0.7877 0.9453 0.038 Uiso calc 1 . .
H H46B 0.2857 0.6237 0.9426 0.038 Uiso calc 1 . .
C C441 0.33856(16) 0.9847(3) 0.85647(8) 0.0266(6) Uani d 1 . .
C C442 0.39903(16) 1.0619(3) 0.84117(8) 0.0294(6) Uani d 1 . .
H H442 0.4442 1.0682 0.8555 0.035 Uiso calc 1 . .
C C443 0.39546(17) 1.1310(3) 0.80501(9) 0.0321(6) Uani d 1 . .
H H443 0.4375 1.1848 0.7953 0.038 Uiso calc 1 . .
C C444 0.33068(17) 1.1208(3) 0.78350(8) 0.0322(6) Uani d 1 . .
C C445 0.27056(18) 1.0369(4) 0.79782(9) 0.0351(7) Uani d 1 . .
H H445 0.2265 1.0252 0.7828 0.042 Uiso calc 1 . .
C C446 0.27444(16) 0.9710(3) 0.83348(9) 0.0315(6) Uani d 1 . .
H H446 0.2327 0.9150 0.8427 0.038 Uiso calc 1 . .
O O447 0.31901(13) 1.1870(2) 0.74835(6) 0.0407(5) Uani d 1 . .
C C447 0.3794(2) 1.2730(4) 0.73265(10) 0.0438(8) Uani d 1 . .
H H47A 0.4236 1.2078 0.7299 0.066 Uiso calc 1 . .
H H47B 0.3912 1.3579 0.7497 0.066 Uiso calc 1 . .
H H47C 0.3649 1.3123 0.7075 0.066 Uiso calc 1 . .
C C51 0.77813(14) 0.9274(3) 0.58429(7) 0.0218(5) Uani d 1 . .
C C52 0.72145(14) 1.0348(3) 0.59017(8) 0.0230(5) Uani d 1 . .
C C53 0.70626(16) 1.0837(3) 0.62739(8) 0.0290(6) Uani d 1 . .
H H53 0.6675 1.1555 0.6316 0.035 Uiso calc 1 . .
C C54 0.74701(18) 1.0288(3) 0.65831(9) 0.0343(6) Uani d 1 . .
H H54 0.7356 1.0620 0.6835 0.041 Uiso calc 1 . .
C C55 0.80426(18) 0.9257(3) 0.65224(8) 0.0335(6) Uani d 1 . .
H H55 0.8331 0.8893 0.6732 0.040 Uiso calc 1 . .
C C56 0.81934(15) 0.8757(3) 0.61533(8) 0.0269(6) Uani d 1 . .
H H56 0.8586 0.8047 0.6113 0.032 Uiso calc 1 . .
C C57 0.79259(14) 0.8587(3) 0.54501(7) 0.0216(5) Uani d 1 . .
O O51 0.85883(12) 0.8253(3) 0.53699(6) 0.0442(6) Uani d 1 . .
O O52 0.73774(11) 0.8367(3) 0.52362(6) 0.0339(5) Uani d 1 . .
C C58 0.67939(15) 1.1118(3) 0.55757(8) 0.0258(6) Uani d 1 . .
O O53 0.72016(11) 1.1881(2) 0.53494(6) 0.0315(4) Uani d 1 . .
O O54 0.61057(11) 1.1038(3) 0.55663(7) 0.0431(6) Uani d 1 . .
C C61 0.53754(14) 0.5763(3) 0.91267(7) 0.0203(5) Uani d 1 . .
C C62 0.48063(14) 0.4705(3) 0.90566(7) 0.0210(5) Uani d 1 . .
C C63 0.46708(15) 0.4225(3) 0.86845(8) 0.0261(6) Uani d 1 . .
H H63 0.4280 0.3518 0.8637 0.031 Uiso calc 1 . .
C C64 0.50944(16) 0.4758(3) 0.83823(8) 0.0289(6) Uani d 1 . .
H H64 0.4992 0.4423 0.8129 0.035 Uiso calc 1 . .
C C65 0.56708(16) 0.5782(3) 0.84487(8) 0.0290(6) Uani d 1 . .
H H65 0.5968 0.6142 0.8242 0.035 Uiso calc 1 . .
C C66 0.58113(15) 0.6279(3) 0.88205(8) 0.0245(5) Uani d 1 . .
H H66 0.6208 0.6976 0.8866 0.029 Uiso calc 1 . .
C C67 0.55033(15) 0.6439(3) 0.95187(7) 0.0234(5) Uani d 1 . .
O O61 0.61608(11) 0.6799(3) 0.96078(6) 0.0408(6) Uani d 1 . .
O O62 0.49458(10) 0.6629(2) 0.97323(6) 0.0325(5) Uani d 1 . .
C C68 0.43777(14) 0.3927(3) 0.93738(8) 0.0237(5) Uani d 1 . .
O O63 0.47775(10) 0.3110(2) 0.95979(6) 0.0296(4) Uani d 1 . .
O O64 0.36920(11) 0.4038(3) 0.93907(7) 0.0391(5) Uani 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
N11 0.0225(12) 0.0352(14) 0.0239(13) -0.0028(9) 0.0018(9) -0.0044(10)
C12 0.0274(13) 0.0363(16) 0.0322(15) 0.0080(12) -0.0026(12) -0.0077(12)
C13 0.0339(15) 0.0227(13) 0.0289(16) 0.0054(11) -0.0026(11) -0.0008(11)
N14 0.0225(11) 0.0220(11) 0.0260(11) 0.0025(8) -0.0030(9) 0.0003(9)
C15 0.0245(13) 0.0246(13) 0.0310(15) 0.0054(11) -0.0033(11) 0.0005(11)
C16 0.0307(14) 0.0315(15) 0.0270(15) -0.0028(12) -0.0048(11) 0.0054(11)
C141 0.0237(13) 0.0200(12) 0.0254(13) -0.0003(10) -0.0019(10) 0.0027(10)
C142 0.0214(13) 0.0361(15) 0.0408(17) 0.0055(11) -0.0035(12) -0.0078(13)
C143 0.0283(15) 0.0392(17) 0.0410(18) 0.0071(13) -0.0119(13) -0.0059(14)
C144 0.0372(15) 0.0284(14) 0.0257(14) 0.0041(12) -0.0049(11) 0.0011(11)
C145 0.0313(15) 0.0303(14) 0.0279(14) 0.0047(12) 0.0035(11) 0.0003(11)
C146 0.0227(13) 0.0294(14) 0.0286(14) 0.0008(10) -0.0016(10) 0.0011(11)
O144 0.0509(14) 0.0496(13) 0.0339(12) 0.0120(11) -0.0116(10) -0.0124(10)
C147 0.0454(18) 0.0378(17) 0.0304(17) -0.0048(14) 0.0010(13) -0.0046(13)
N21 0.0239(12) 0.0360(14) 0.0255(13) 0.0028(10) -0.0014(9) -0.0068(10)
C22 0.0287(14) 0.0328(16) 0.0363(16) -0.0043(12) 0.0029(12) -0.0096(12)
C23 0.0308(14) 0.0245(14) 0.0303(16) -0.0054(11) 0.0044(11) -0.0027(11)
N24 0.0243(11) 0.0232(11) 0.0237(11) -0.0015(9) 0.0022(8) -0.0015(8)
C25 0.0307(14) 0.0270(13) 0.0245(14) -0.0036(11) 0.0073(11) -0.0010(10)
C26 0.0324(15) 0.0352(16) 0.0254(14) 0.0030(12) 0.0029(11) 0.0037(12)
C241 0.0246(12) 0.0215(12) 0.0228(13) 0.0015(10) 0.0005(10) 0.0023(10)
C242 0.0252(13) 0.0311(14) 0.0349(16) -0.0031(11) -0.0001(11) -0.0046(12)
C243 0.0264(15) 0.0391(16) 0.0415(18) -0.0004(13) 0.0109(12) -0.0053(13)
C244 0.0362(15) 0.0254(14) 0.0268(14) 0.0045(12) 0.0080(11) -0.0002(11)
C245 0.0323(15) 0.0278(14) 0.0265(14) -0.0031(11) -0.0011(11) -0.0015(11)
C246 0.0249(13) 0.0285(14) 0.0286(14) -0.0027(11) 0.0036(10) 0.0018(11)
O244 0.0462(13) 0.0436(12) 0.0324(11) 0.0027(10) 0.0121(10) -0.0096(10)
C247 0.064(2) 0.0368(17) 0.0291(17) 0.0086(16) -0.0008(15) -0.0085(13)
N31 0.0213(11) 0.0293(12) 0.0277(12) -0.0055(10) -0.0030(9) 0.0005(9)
C32 0.0314(14) 0.0299(14) 0.0261(14) 0.0022(11) 0.0014(11) -0.0025(11)
C33 0.0277(14) 0.0298(14) 0.0283(14) 0.0071(11) 0.0021(11) -0.0036(11)
N34 0.0249(11) 0.0250(11) 0.0243(11) 0.0035(9) -0.0006(9) -0.0028(9)
C35 0.0308(14) 0.0226(13) 0.0317(15) 0.0038(11) 0.0021(11) -0.0029(11)
C36 0.0255(14) 0.0298(14) 0.0321(16) 0.0002(11) -0.0011(11) 0.0015(11)
C341 0.0263(13) 0.0219(12) 0.0252(13) -0.0009(10) -0.0012(10) -0.0036(10)
C342 0.0304(14) 0.0353(15) 0.0280(15) 0.0096(12) 0.0045(11) -0.0021(12)
C343 0.0406(17) 0.0391(17) 0.0334(16) 0.0147(13) -0.0032(13) -0.0021(13)
C344 0.0477(18) 0.0302(14) 0.0246(14) 0.0027(13) 0.0026(12) -0.0023(11)
C345 0.0422(17) 0.0413(17) 0.0352(17) 0.0090(14) 0.0097(13) -0.0011(13)
C346 0.0304(15) 0.0411(16) 0.0337(16) 0.0101(13) 0.0030(12) 0.0018(13)
O344 0.0782(18) 0.0450(12) 0.0265(11) 0.0175(12) 0.0065(11) 0.0069(10)
C347 0.063(2) 0.0353(17) 0.0322(18) -0.0003(15) -0.0069(15) 0.0080(13)
N41 0.0229(11) 0.0298(12) 0.0323(13) 0.0036(10) 0.0035(9) 0.0000(10)
C42 0.0279(14) 0.0310(15) 0.0342(15) -0.0008(11) -0.0022(11) -0.0042(12)
C43 0.0274(14) 0.0315(15) 0.0337(15) -0.0063(12) -0.0032(11) -0.0015(12)
N44 0.0249(11) 0.0239(11) 0.0313(12) -0.0033(9) -0.0018(9) -0.0027(9)
C45 0.0286(14) 0.0253(14) 0.0379(17) -0.0005(11) -0.0013(12) -0.0059(12)
C46 0.0233(13) 0.0267(14) 0.0445(18) -0.0036(11) 0.0023(12) -0.0016(12)
C441 0.0272(14) 0.0242(13) 0.0282(14) 0.0005(11) 0.0009(10) -0.0065(11)
C442 0.0247(13) 0.0286(14) 0.0350(16) -0.0020(11) -0.0027(11) -0.0044(11)
C443 0.0319(15) 0.0301(15) 0.0342(15) -0.0029(12) 0.0024(12) -0.0029(12)
C444 0.0390(16) 0.0291(14) 0.0287(14) 0.0013(12) -0.0013(12) -0.0057(11)
C445 0.0330(16) 0.0376(17) 0.0346(16) 0.0006(13) -0.0079(12) -0.0075(12)
C446 0.0257(14) 0.0353(15) 0.0337(15) -0.0051(11) -0.0004(11) -0.0041(12)
O447 0.0459(12) 0.0435(12) 0.0328(11) 0.0014(10) -0.0040(9) 0.0028(9)
C447 0.058(2) 0.0386(17) 0.0344(18) 0.0009(16) 0.0035(15) 0.0054(14)
C51 0.0206(12) 0.0217(12) 0.0230(13) -0.0033(10) -0.0008(10) -0.0014(10)
C52 0.0206(12) 0.0213(12) 0.0271(13) -0.0047(9) 0.0028(10) -0.0021(10)
C53 0.0256(14) 0.0299(14) 0.0314(15) -0.0030(11) 0.0065(11) -0.0042(11)
C54 0.0424(17) 0.0340(16) 0.0266(14) -0.0041(13) 0.0063(12) -0.0063(12)
C55 0.0444(17) 0.0321(14) 0.0239(14) -0.0039(12) -0.0060(12) 0.0014(11)
C56 0.0273(13) 0.0232(13) 0.0303(15) 0.0014(11) -0.0001(11) -0.0009(10)
C57 0.0206(12) 0.0208(12) 0.0233(13) -0.0002(9) 0.0015(10) -0.0021(10)
O51 0.0259(10) 0.0750(17) 0.0317(11) 0.0149(10) -0.0033(9) -0.0179(11)
O52 0.0216(10) 0.0508(13) 0.0292(10) -0.0074(9) 0.0000(8) -0.0124(9)
C58 0.0206(13) 0.0235(13) 0.0334(14) 0.0003(10) -0.0014(10) -0.0036(11)
O53 0.0265(10) 0.0337(11) 0.0344(11) -0.0034(8) -0.0065(8) 0.0084(9)
O54 0.0178(10) 0.0556(14) 0.0558(14) 0.0019(9) -0.0016(9) 0.0104(12)
C61 0.0178(11) 0.0188(12) 0.0244(13) 0.0037(9) -0.0009(9) -0.0011(10)
C62 0.0168(11) 0.0222(12) 0.0240(13) 0.0031(9) 0.0000(9) -0.0011(10)
C63 0.0250(13) 0.0247(13) 0.0286(14) 0.0007(10) -0.0049(10) -0.0032(11)
C64 0.0348(15) 0.0321(14) 0.0198(13) 0.0065(12) -0.0033(11) -0.0026(11)
C65 0.0317(14) 0.0302(14) 0.0252(14) 0.0025(11) 0.0043(11) 0.0054(11)
C66 0.0256(13) 0.0211(12) 0.0268(13) 0.0008(10) 0.0031(10) 0.0006(10)
C67 0.0223(13) 0.0224(12) 0.0254(13) 0.0014(10) -0.0005(10) -0.0015(10)
O61 0.0218(10) 0.0699(16) 0.0307(11) -0.0123(10) 0.0018(8) -0.0169(11)
O62 0.0207(9) 0.0486(12) 0.0281(10) 0.0055(8) 0.0001(8) -0.0112(9)
C68 0.0208(12) 0.0238(13) 0.0266(13) -0.0007(10) 0.0008(10) -0.0028(10)
O63 0.0248(9) 0.0344(11) 0.0296(10) 0.0059(8) 0.0050(8) 0.0063(8)
O64 0.0181(9) 0.0556(14) 0.0436(12) -0.0006(9) 0.0027(9) 0.0092(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
C16 N11 C12 . . 111.8(2) ?
C16 N11 H11 . . 111(2) ?
C12 N11 H11 . . 110.2(19) ?
C16 N11 H12 . . 107(3) ?
C12 N11 H12 . . 113(3) ?
H11 N11 H12 . . 104(3) ?
N11 C12 C13 . . 110.8(2) ?
N11 C12 H12A . . 109.5 ?
C13 C12 H12A . . 109.5 ?
N11 C12 H12B . . 109.5 ?
C13 C12 H12B . . 109.5 ?
H12A C12 H12B . . 108.1 ?
N14 C13 C12 . . 110.6(2) ?
N14 C13 H13A . . 109.5 ?
C12 C13 H13A . . 109.5 ?
N14 C13 H13B . . 109.5 ?
C12 C13 H13B . . 109.5 ?
H13A C13 H13B . . 108.1 ?
C141 N14 C15 . . 116.9(2) ?
C141 N14 C13 . . 114.9(2) ?
C15 N14 C13 . . 110.1(2) ?
N14 C15 C16 . . 108.6(2) ?
N14 C15 H15A . . 110.0 ?
C16 C15 H15A . . 110.0 ?
N14 C15 H15B . . 110.0 ?
C16 C15 H15B . . 110.0 ?
H15A C15 H15B . . 108.4 ?
N11 C16 C15 . . 110.8(2) ?
N11 C16 H16A . . 109.5 ?
C15 C16 H16A . . 109.5 ?
N11 C16 H16B . . 109.5 ?
C15 C16 H16B . . 109.5 ?
H16A C16 H16B . . 108.1 ?
C146 C141 C142 . . 117.7(2) ?
C146 C141 N14 . . 124.4(2) ?
C142 C141 N14 . . 117.8(2) ?
C143 C142 C141 . . 120.8(3) ?
C143 C142 H142 . . 119.6 ?
C141 C142 H142 . . 119.6 ?
C142 C143 C144 . . 121.0(3) ?
C142 C143 H143 . . 119.5 ?
C144 C143 H143 . . 119.5 ?
O144 C144 C145 . . 125.3(3) ?
O144 C144 C143 . . 115.8(3) ?
C145 C144 C143 . . 118.8(3) ?
C144 C145 C146 . . 120.2(3) ?
C144 C145 H145 . . 119.9 ?
C146 C145 H145 . . 119.9 ?
C141 C146 C145 . . 121.5(3) ?
C141 C146 H146 . . 119.3 ?
C145 C146 H146 . . 119.3 ?
C144 O144 C147 . . 116.4(2) ?
O144 C147 H17A . . 109.5 ?
O144 C147 H17B . . 109.5 ?
H17A C147 H17B . . 109.5 ?
O144 C147 H17C . . 109.5 ?
H17A C147 H17C . . 109.5 ?
H17B C147 H17C . . 109.5 ?
C26 N21 C22 . . 111.6(2) ?
C26 N21 H21 . . 112(2) ?
C22 N21 H21 . . 111(2) ?
C26 N21 H22 . . 107(2) ?
C22 N21 H22 . . 111(2) ?
H21 N21 H22 . . 104(3) ?
N21 C22 C23 . . 111.0(2) ?
N21 C22 H22A . . 109.4 ?
C23 C22 H22A . . 109.4 ?
N21 C22 H22B . . 109.4 ?
C23 C22 H22B . . 109.4 ?
H22A C22 H22B . . 108.0 ?
N24 C23 C22 . . 110.7(2) ?
N24 C23 H23A . . 109.5 ?
C22 C23 H23A . . 109.5 ?
N24 C23 H23B . . 109.5 ?
C22 C23 H23B . . 109.5 ?
H23A C23 H23B . . 108.1 ?
C241 N24 C25 . . 117.6(2) ?
C241 N24 C23 . . 115.1(2) ?
C25 N24 C23 . . 110.0(2) ?
N24 C25 C26 . . 108.7(2) ?
N24 C25 H25A . . 109.9 ?
C26 C25 H25A . . 109.9 ?
N24 C25 H25B . . 109.9 ?
C26 C25 H25B . . 109.9 ?
H25A C25 H25B . . 108.3 ?
N21 C26 C25 . . 110.4(2) ?
N21 C26 H26A . . 109.6 ?
C25 C26 H26A . . 109.6 ?
N21 C26 H26B . . 109.6 ?
C25 C26 H26B . . 109.6 ?
H26A C26 H26B . . 108.1 ?
C242 C241 C246 . . 117.6(2) ?
C242 C241 N24 . . 118.2(2) ?
C246 C241 N24 . . 124.1(2) ?
C243 C242 C241 . . 121.5(3) ?
C243 C242 H242 . . 119.2 ?
C241 C242 H242 . . 119.2 ?
C242 C243 C244 . . 120.4(3) ?
C242 C243 H243 . . 119.8 ?
C244 C243 H243 . . 119.8 ?
O244 C244 C245 . . 125.0(3) ?
O244 C244 C243 . . 115.9(3) ?
C245 C244 C243 . . 119.1(3) ?
C244 C245 C246 . . 120.1(3) ?
C244 C245 H245 . . 120.0 ?
C246 C245 H245 . . 120.0 ?
C241 C246 C245 . . 121.3(3) ?
C241 C246 H246 . . 119.4 ?
C245 C246 H246 . . 119.4 ?
C244 O244 C247 . . 117.3(3) ?
O244 C247 H27A . . 109.5 ?
O244 C247 H27B . . 109.5 ?
H27A C247 H27B . . 109.5 ?
O244 C247 H27C . . 109.5 ?
H27A C247 H27C . . 109.5 ?
H27B C247 H27C . . 109.5 ?
C32 N31 C36 . . 111.5(2) ?
C32 N31 H31 . . 104(2) ?
C36 N31 H31 . . 111(2) ?
C32 N31 H32 . . 108(2) ?
C36 N31 H32 . . 113(2) ?
H31 N31 H32 . . 109(3) ?
N31 C32 C33 . . 111.2(2) ?
N31 C32 H32A . . 109.4 ?
C33 C32 H32A . . 109.4 ?
N31 C32 H32B . . 109.4 ?
C33 C32 H32B . . 109.4 ?
H32A C32 H32B . . 108.0 ?
N34 C33 C32 . . 110.0(2) ?
N34 C33 H33A . . 109.7 ?
C32 C33 H33A . . 109.7 ?
N34 C33 H33B . . 109.7 ?
C32 C33 H33B . . 109.7 ?
H33A C33 H33B . . 108.2 ?
C341 N34 C33 . . 116.0(2) ?
C341 N34 C35 . . 114.7(2) ?
C33 N34 C35 . . 110.1(2) ?
N34 C35 C36 . . 110.7(2) ?
N34 C35 H35A . . 109.5 ?
C36 C35 H35A . . 109.5 ?
N34 C35 H35B . . 109.5 ?
C36 C35 H35B . . 109.5 ?
H35A C35 H35B . . 108.1 ?
N31 C36 C35 . . 110.2(2) ?
N31 C36 H36A . . 109.6 ?
C35 C36 H36A . . 109.6 ?
N31 C36 H36B . . 109.6 ?
C35 C36 H36B . . 109.6 ?
H36A C36 H36B . . 108.1 ?
C346 C341 C342 . . 117.4(3) ?
C346 C341 N34 . . 119.3(2) ?
C342 C341 N34 . . 123.3(2) ?
C343 C342 C341 . . 121.7(3) ?
C343 C342 H342 . . 119.1 ?
C341 C342 H342 . . 119.1 ?
C344 C343 C342 . . 119.6(3) ?
C344 C343 H343 . . 120.2 ?
C342 C343 H343 . . 120.2 ?
C343 C344 O344 . . 123.8(3) ?
C343 C344 C345 . . 119.0(3) ?
O344 C344 C345 . . 117.1(3) ?
C346 C345 C344 . . 121.4(3) ?
C346 C345 H345 . . 119.3 ?
C344 C345 H345 . . 119.3 ?
C345 C346 C341 . . 120.8(3) ?
C345 C346 H346 . . 119.6 ?
C341 C346 H346 . . 119.6 ?
C344 O344 C347 . . 116.8(2) ?
O344 C347 H37A . . 109.5 ?
O344 C347 H37B . . 109.5 ?
H37A C347 H37B . . 109.5 ?
O344 C347 H37C . . 109.5 ?
H37A C347 H37C . . 109.5 ?
H37B C347 H37C . . 109.5 ?
C42 N41 C46 . . 111.7(2) ?
C42 N41 H41 . . 105(2) ?
C46 N41 H41 . . 110(2) ?
C42 N41 H42 . . 109(2) ?
C46 N41 H42 . . 111(2) ?
H41 N41 H42 . . 109(3) ?
N41 C42 C43 . . 111.4(2) ?
N41 C42 H42A . . 109.3 ?
C43 C42 H42A . . 109.3 ?
N41 C42 H42B . . 109.3 ?
C43 C42 H42B . . 109.3 ?
H42A C42 H42B . . 108.0 ?
N44 C43 C42 . . 110.2(2) ?
N44 C43 H43A . . 109.6 ?
C42 C43 H43A . . 109.6 ?
N44 C43 H43B . . 109.6 ?
C42 C43 H43B . . 109.6 ?
H43A C43 H43B . . 108.1 ?
C441 N44 C43 . . 117.1(2) ?
C441 N44 C45 . . 116.1(2) ?
C43 N44 C45 . . 110.1(2) ?
N44 C45 C46 . . 110.4(2) ?
N44 C45 H45A . . 109.6 ?
C46 C45 H45A . . 109.6 ?
N44 C45 H45B . . 109.6 ?
C46 C45 H45B . . 109.6 ?
H45A C45 H45B . . 108.1 ?
N41 C46 C45 . . 110.8(2) ?
N41 C46 H46A . . 109.5 ?
C45 C46 H46A . . 109.5 ?
N41 C46 H46B . . 109.5 ?
C45 C46 H46B . . 109.5 ?
H46A C46 H46B . . 108.1 ?
C442 C441 C446 . . 117.2(3) ?
C442 C441 N44 . . 123.8(3) ?
C446 C441 N44 . . 118.8(3) ?
C441 C442 C443 . . 121.7(3) ?
C441 C442 H442 . . 119.1 ?
C443 C442 H442 . . 119.1 ?
C444 C443 C442 . . 119.9(3) ?
C444 C443 H443 . . 120.0 ?
C442 C443 H443 . . 120.0 ?
O447 C444 C443 . . 125.8(3) ?
O447 C444 C445 . . 115.4(3) ?
C443 C444 C445 . . 118.9(3) ?
C446 C445 C444 . . 120.6(3) ?
C446 C445 H445 . . 119.7 ?
C444 C445 H445 . . 119.7 ?
C445 C446 C441 . . 121.5(3) ?
C445 C446 H446 . . 119.2 ?
C441 C446 H446 . . 119.2 ?
C444 O447 C447 . . 117.0(2) ?
O447 C447 H47A . . 109.5 ?
O447 C447 H47B . . 109.5 ?
H47A C447 H47B . . 109.5 ?
O447 C447 H47C . . 109.5 ?
H47A C447 H47C . . 109.5 ?
H47B C447 H47C . . 109.5 ?
C56 C51 C52 . . 119.4(2) ?
C56 C51 C57 . . 119.0(2) ?
C52 C51 C57 . . 121.6(2) ?
C53 C52 C51 . . 119.0(3) ?
C53 C52 C58 . . 117.6(2) ?
C51 C52 C58 . . 123.2(2) ?
C54 C53 C52 . . 121.0(3) ?
C54 C53 H53 . . 119.5 ?
C52 C53 H53 . . 119.5 ?
C55 C54 C53 . . 119.7(3) ?
C55 C54 H54 . . 120.1 ?
C53 C54 H54 . . 120.1 ?
C54 C55 C56 . . 119.6(3) ?
C54 C55 H55 . . 120.2 ?
C56 C55 H55 . . 120.2 ?
C51 C56 C55 . . 121.2(3) ?
C51 C56 H56 . . 119.4 ?
C55 C56 H56 . . 119.4 ?
O52 C57 O51 . . 124.9(2) ?
O52 C57 C51 . . 118.0(2) ?
O51 C57 C51 . . 117.1(2) ?
O54 C58 O53 . . 125.9(3) ?
O54 C58 C52 . . 119.1(3) ?
O53 C58 C52 . . 114.8(2) ?
C66 C61 C62 . . 119.1(2) ?
C66 C61 C67 . . 118.8(2) ?
C62 C61 C67 . . 122.0(2) ?
C63 C62 C61 . . 119.5(2) ?
C63 C62 C68 . . 117.4(2) ?
C61 C62 C68 . . 122.8(2) ?
C64 C63 C62 . . 121.1(3) ?
C64 C63 H63 . . 119.4 ?
C62 C63 H63 . . 119.4 ?
C63 C64 C65 . . 119.9(3) ?
C63 C64 H64 . . 120.0 ?
C65 C64 H64 . . 120.0 ?
C64 C65 C66 . . 119.6(3) ?
C64 C65 H65 . . 120.2 ?
C66 C65 H65 . . 120.2 ?
C65 C66 C61 . . 120.7(3) ?
C65 C66 H66 . . 119.6 ?
C61 C66 H66 . . 119.6 ?
O61 C67 O62 . . 124.1(2) ?
O61 C67 C61 . . 117.8(2) ?
O62 C67 C61 . . 118.2(2) ?
O64 C68 O63 . . 124.7(3) ?
O64 C68 C62 . . 120.2(2) ?
O63 C68 C62 . . 114.9(2) ?
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
N11 C16 . 1.484(4) ?
N11 C12 . 1.493(4) ?
N11 H11 . 0.99(4) ?
N11 H12 . 0.79(4) ?
C12 C13 . 1.514(4) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C13 N14 . 1.462(3) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
N14 C141 . 1.418(3) ?
N14 C15 . 1.456(3) ?
C15 C16 . 1.514(4) ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C141 C146 . 1.385(4) ?
C141 C142 . 1.401(4) ?
C142 C143 . 1.378(5) ?
C142 H142 . 0.9500 ?
C143 C144 . 1.393(4) ?
C143 H143 . 0.9500 ?
C144 O144 . 1.376(4) ?
C144 C145 . 1.377(4) ?
C145 C146 . 1.397(4) ?
C145 H145 . 0.9500 ?
C146 H146 . 0.9500 ?
O144 C147 . 1.422(4) ?
C147 H17A . 0.9800 ?
C147 H17B . 0.9800 ?
C147 H17C . 0.9800 ?
N21 C26 . 1.485(4) ?
N21 C22 . 1.493(4) ?
N21 H21 . 0.99(4) ?
N21 H22 . 1.01(4) ?
C22 C23 . 1.512(4) ?
C22 H22A . 0.9900 ?
C22 H22B . 0.9900 ?
C23 N24 . 1.463(4) ?
C23 H23A . 0.9900 ?
C23 H23B . 0.9900 ?
N24 C241 . 1.419(3) ?
N24 C25 . 1.453(3) ?
C25 C26 . 1.512(4) ?
C25 H25A . 0.9900 ?
C25 H25B . 0.9900 ?
C26 H26A . 0.9900 ?
C26 H26B . 0.9900 ?
C241 C242 . 1.391(4) ?
C241 C246 . 1.394(4) ?
C242 C243 . 1.381(4) ?
C242 H242 . 0.9500 ?
C243 C244 . 1.395(4) ?
C243 H243 . 0.9500 ?
C244 O244 . 1.374(3) ?
C244 C245 . 1.380(4) ?
C245 C246 . 1.398(4) ?
C245 H245 . 0.9500 ?
C246 H246 . 0.9500 ?
O244 C247 . 1.422(4) ?
C247 H27A . 0.9800 ?
C247 H27B . 0.9800 ?
C247 H27C . 0.9800 ?
N31 C32 . 1.490(4) ?
N31 C36 . 1.491(4) ?
N31 H31 . 0.94(4) ?
N31 H32 . 0.92(4) ?
C32 C33 . 1.515(4) ?
C32 H32A . 0.9900 ?
C32 H32B . 0.9900 ?
C33 N34 . 1.463(3) ?
C33 H33A . 0.9900 ?
C33 H33B . 0.9900 ?
N34 C341 . 1.416(3) ?
N34 C35 . 1.468(3) ?
C35 C36 . 1.511(4) ?
C35 H35A . 0.9900 ?
C35 H35B . 0.9900 ?
C36 H36A . 0.9900 ?
C36 H36B . 0.9900 ?
C341 C346 . 1.389(4) ?
C341 C342 . 1.394(4) ?
C342 C343 . 1.390(4) ?
C342 H342 . 0.9500 ?
C343 C344 . 1.378(4) ?
C343 H343 . 0.9500 ?
C344 O344 . 1.380(4) ?
C344 C345 . 1.380(5) ?
C345 C346 . 1.374(5) ?
C345 H345 . 0.9500 ?
C346 H346 . 0.9500 ?
O344 C347 . 1.420(4) ?
C347 H37A . 0.9800 ?
C347 H37B . 0.9800 ?
C347 H37C . 0.9800 ?
N41 C42 . 1.485(4) ?
N41 C46 . 1.493(4) ?
N41 H41 . 1.00(4) ?
N41 H42 . 0.91(4) ?
C42 C43 . 1.510(4) ?
C42 H42A . 0.9900 ?
C42 H42B . 0.9900 ?
C43 N44 . 1.451(4) ?
C43 H43A . 0.9900 ?
C43 H43B . 0.9900 ?
N44 C441 . 1.422(4) ?
N44 C45 . 1.465(4) ?
C45 C46 . 1.511(5) ?
C45 H45A . 0.9900 ?
C45 H45B . 0.9900 ?
C46 H46A . 0.9900 ?
C46 H46B . 0.9900 ?
C441 C442 . 1.383(4) ?
C441 C446 . 1.403(4) ?
C442 C443 . 1.404(4) ?
C442 H442 . 0.9500 ?
C443 C444 . 1.381(4) ?
C443 H443 . 0.9500 ?
C444 O447 . 1.375(4) ?
C444 C445 . 1.395(5) ?
C445 C446 . 1.376(4) ?
C445 H445 . 0.9500 ?
C446 H446 . 0.9500 ?
O447 C447 . 1.427(4) ?
C447 H47A . 0.9800 ?
C447 H47B . 0.9800 ?
C447 H47C . 0.9800 ?
C51 C56 . 1.387(4) ?
C51 C52 . 1.400(4) ?
C51 C57 . 1.522(3) ?
C52 C53 . 1.396(4) ?
C52 C58 . 1.523(4) ?
C53 C54 . 1.389(4) ?
C53 H53 . 0.9500 ?
C54 C55 . 1.384(5) ?
C54 H54 . 0.9500 ?
C55 C56 . 1.389(4) ?
C55 H55 . 0.9500 ?
C56 H56 . 0.9500 ?
C57 O52 . 1.246(3) ?
C57 O51 . 1.250(3) ?
C58 O54 . 1.230(3) ?
C58 O53 . 1.267(4) ?
C61 C66 . 1.399(4) ?
C61 C62 . 1.400(4) ?
C61 C67 . 1.511(4) ?
C62 C63 . 1.388(4) ?
C62 C68 . 1.511(4) ?
C63 C64 . 1.380(4) ?
C63 H63 . 0.9500 ?
C64 C65 . 1.388(4) ?
C64 H64 . 0.9500 ?
C65 C66 . 1.393(4) ?
C65 H65 . 0.9500 ?
C66 H66 . 0.9500 ?
C67 O61 . 1.255(3) ?
C67 O62 . 1.255(3) ?
C68 O64 . 1.229(3) ?
C68 O63 . 1.281(3) ?
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
N11 H11 O51 . 0.99(4) 1.73(4) 2.714(4) 175(2) y
N11 H12 O63 4_654 0.80(4) 2.03(4) 2.738(3) 148(3) y
N21 H21 O61 . 0.99(4) 1.72(4) 2.707(4) 177(3) y
N21 H22 O53 4_645 1.01(4) 1.88(4) 2.744(3) 142(3) y
N31 H31 O63 2_664 0.94(3) 1.77(3) 2.685(3) 163(3) y
N31 H32 O52 . 0.92(4) 1.83(4) 2.732(3) 164(3) y
N41 H41 O53 2_675 1.00(4) 1.74(4) 2.711(3) 163(3) y
N41 H42 O62 . 0.90(4) 1.89(4) 2.740(3) 157(3) y
C36 H36A O51 3_465 0.99 2.40 3.354(4) 160 y
C46 H46A O61 3_465 0.99 2.42 3.359(4) 158 y
C13 H13B Cg3 4_654 0.99 2.84 3.795(3) 161 y
C23 H23B Cg4 4_654 0.99 2.85 3.800(3) 162 y
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
C16 N11 C12 C13 . . . . -51.3(3) ?
N11 C12 C13 N14 . . . . 54.6(3) ?
C12 C13 N14 C141 . . . . 164.1(2) ?
C12 C13 N14 C15 . . . . -61.4(3) ?
C141 N14 C15 C16 . . . . -163.5(2) ?
C13 N14 C15 C16 . . . . 63.1(3) ?
C12 N11 C16 C15 . . . . 54.0(3) ?
N14 C15 C16 N11 . . . . -59.3(3) ?
C15 N14 C141 C146 . . . . -12.7(4) ?
C13 N14 C141 C146 . . . . 118.6(3) ?
C15 N14 C141 C142 . . . . 165.0(2) ?
C13 N14 C141 C142 . . . . -63.7(3) ?
C146 C141 C142 C143 . . . . 0.2(4) ?
N14 C141 C142 C143 . . . . -177.6(3) ?
C141 C142 C143 C144 . . . . 0.5(5) ?
C142 C143 C144 O144 . . . . 179.6(3) ?
C142 C143 C144 C145 . . . . -0.6(5) ?
O144 C144 C145 C146 . . . . 179.7(3) ?
C143 C144 C145 C146 . . . . 0.0(4) ?
C142 C141 C146 C145 . . . . -0.9(4) ?
N14 C141 C146 C145 . . . . 176.8(2) ?
C144 C145 C146 C141 . . . . 0.7(4) ?
C145 C144 O144 C147 . . . . 10.7(4) ?
C143 C144 O144 C147 . . . . -169.6(3) ?
C26 N21 C22 C23 . . . . -51.3(3) ?
N21 C22 C23 N24 . . . . 54.2(3) ?
C22 C23 N24 C241 . . . . 163.3(2) ?
C22 C23 N24 C25 . . . . -61.0(3) ?
C241 N24 C25 C26 . . . . -162.1(2) ?
C23 N24 C25 C26 . . . . 63.4(3) ?
C22 N21 C26 C25 . . . . 54.4(3) ?
N24 C25 C26 N21 . . . . -60.0(3) ?
C25 N24 C241 C242 . . . . 164.0(3) ?
C23 N24 C241 C242 . . . . -63.8(3) ?
C25 N24 C241 C246 . . . . -12.4(4) ?
C23 N24 C241 C246 . . . . 119.8(3) ?
C246 C241 C242 C243 . . . . 0.0(4) ?
N24 C241 C242 C243 . . . . -176.6(3) ?
C241 C242 C243 C244 . . . . 0.2(5) ?
C242 C243 C244 O244 . . . . 179.8(3) ?
C242 C243 C244 C245 . . . . 0.0(5) ?
O244 C244 C245 C246 . . . . 179.9(3) ?
C243 C244 C245 C246 . . . . -0.3(4) ?
C242 C241 C246 C245 . . . . -0.3(4) ?
N24 C241 C246 C245 . . . . 176.0(3) ?
C244 C245 C246 C241 . . . . 0.5(4) ?
C245 C244 O244 C247 . . . . 2.9(4) ?
C243 C244 O244 C247 . . . . -176.9(3) ?
C36 N31 C32 C33 . . . . -53.7(3) ?
N31 C32 C33 N34 . . . . 56.5(3) ?
C32 C33 N34 C341 . . . . 167.6(2) ?
C32 C33 N34 C35 . . . . -60.0(3) ?
C341 N34 C35 C36 . . . . -166.1(2) ?
C33 N34 C35 C36 . . . . 60.9(3) ?
C32 N31 C36 C35 . . . . 53.6(3) ?
N34 C35 C36 N31 . . . . -57.2(3) ?
C33 N34 C341 C346 . . . . -173.4(3) ?
C35 N34 C341 C346 . . . . 56.4(3) ?
C33 N34 C341 C342 . . . . 4.3(4) ?
C35 N34 C341 C342 . . . . -125.9(3) ?
C346 C341 C342 C343 . . . . 1.6(4) ?
N34 C341 C342 C343 . . . . -176.1(3) ?
C341 C342 C343 C344 . . . . -1.6(5) ?
C342 C343 C344 O344 . . . . -175.6(3) ?
C342 C343 C344 C345 . . . . 0.2(5) ?
C343 C344 C345 C346 . . . . 1.2(5) ?
O344 C344 C345 C346 . . . . 177.3(3) ?
C344 C345 C346 C341 . . . . -1.1(5) ?
C342 C341 C346 C345 . . . . -0.3(5) ?
N34 C341 C346 C345 . . . . 177.6(3) ?
C343 C344 O344 C347 . . . . -44.2(5) ?
C345 C344 O344 C347 . . . . 139.9(3) ?
C46 N41 C42 C43 . . . . -52.1(3) ?
N41 C42 C43 N44 . . . . 56.6(3) ?
C42 C43 N44 C441 . . . . 163.5(2) ?
C42 C43 N44 C45 . . . . -61.0(3) ?
C441 N44 C45 C46 . . . . -162.8(2) ?
C43 N44 C45 C46 . . . . 61.2(3) ?
C42 N41 C46 C45 . . . . 51.8(3) ?
N44 C45 C46 N41 . . . . -56.2(3) ?
C43 N44 C441 C442 . . . . 6.8(4) ?
C45 N44 C441 C442 . . . . -126.0(3) ?
C43 N44 C441 C446 . . . . -168.4(3) ?
C45 N44 C441 C446 . . . . 58.7(3) ?
C446 C441 C442 C443 . . . . 3.4(4) ?
N44 C441 C442 C443 . . . . -171.9(3) ?
C441 C442 C443 C444 . . . . -1.1(4) ?
C442 C443 C444 O447 . . . . 177.8(3) ?
C442 C443 C444 C445 . . . . -2.1(4) ?
O447 C444 C445 C446 . . . . -177.1(3) ?
C443 C444 C445 C446 . . . . 2.8(5) ?
C444 C445 C446 C441 . . . . -0.4(5) ?
C442 C441 C446 C445 . . . . -2.7(4) ?
N44 C441 C446 C445 . . . . 172.9(3) ?
C443 C444 O447 C447 . . . . 0.5(4) ?
C445 C444 O447 C447 . . . . -179.6(3) ?
C56 C51 C52 C53 . . . . -2.0(4) ?
C57 C51 C52 C53 . . . . 174.2(2) ?
C56 C51 C52 C58 . . . . 172.7(2) ?
C57 C51 C52 C58 . . . . -11.1(4) ?
C51 C52 C53 C54 . . . . 0.8(4) ?
C58 C52 C53 C54 . . . . -174.2(3) ?
C52 C53 C54 C55 . . . . 0.9(4) ?
C53 C54 C55 C56 . . . . -1.3(5) ?
C52 C51 C56 C55 . . . . 1.6(4) ?
C57 C51 C56 C55 . . . . -174.8(3) ?
C54 C55 C56 C51 . . . . 0.1(4) ?
C56 C51 C57 O52 . . . . 141.7(3) ?
C52 C51 C57 O52 . . . . -34.5(4) ?
C56 C51 C57 O51 . . . . -36.7(4) ?
C52 C51 C57 O51 . . . . 147.0(3) ?
C53 C52 C58 O54 . . . . -60.9(4) ?
C51 C52 C58 O54 . . . . 124.3(3) ?
C53 C52 C58 O53 . . . . 114.5(3) ?
C51 C52 C58 O53 . . . . -60.2(3) ?
C66 C61 C62 C63 . . . . -2.0(4) ?
C67 C61 C62 C63 . . . . 174.2(2) ?
C66 C61 C62 C68 . . . . 171.6(2) ?
C67 C61 C62 C68 . . . . -12.3(4) ?
C61 C62 C63 C64 . . . . 0.9(4) ?
C68 C62 C63 C64 . . . . -173.0(2) ?
C62 C63 C64 C65 . . . . 0.5(4) ?
C63 C64 C65 C66 . . . . -0.8(4) ?
C64 C65 C66 C61 . . . . -0.4(4) ?
C62 C61 C66 C65 . . . . 1.7(4) ?
C67 C61 C66 C65 . . . . -174.6(2) ?
C66 C61 C67 O61 . . . . -34.9(4) ?
C62 C61 C67 O61 . . . . 149.0(3) ?
C66 C61 C67 O62 . . . . 144.0(3) ?
C62 C61 C67 O62 . . . . -32.2(4) ?
C63 C62 C68 O64 . . . . -64.0(3) ?
C61 C62 C68 O64 . . . . 122.3(3) ?
C63 C62 C68 O63 . . . . 112.2(3) ?
C61 C62 C68 O63 . . . . -61.4(3) ?
_cod_database_fobs_code 2244153