#------------------------------------------------------------------------------
#$Date: 2015-12-13 04:38:46 +0200 (Sun, 13 Dec 2015) $
#$Revision: 171471 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/13/2241389.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_2241389
loop_
_publ_author_name
'Tiritiris, Ioannis'
'Kantlehner, Willi'
_publ_section_title
;
Crystal structure of
N''-(2-ethoxy-2-oxoethyl)-N,N,N',N'-tetramethyl-N''-[3-(1,3,3-trimethylureido)propyl]guanidinium
tetraphenylborate
;
_journal_coeditor_code RZ5179
_journal_issue 12
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first o1026
_journal_page_last o1027
_journal_paper_doi 10.1107/S2056989015023142
_journal_volume 71
_journal_year 2015
_chemical_formula_iupac 'C16 H34 N5 O3 +, C24 H20 B -'
_chemical_formula_moiety 'C16 H34 N5 O3 +, C24 H20 B -'
_chemical_formula_sum 'C40 H54 B N5 O3'
_chemical_formula_weight 663.69
_chemical_name_systematic
;N''-(2-Ethoxy-2-oxoethyl)-N,N,N',N'-tetramethyl-N''-[3-(1,3,3-trimethylureido)propyl]guanidinium
tetraphenylborate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2ybc'
_space_group_name_H-M_alt 'P 1 21/c 1'
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 1 21/c 1'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2014/7
_cell_angle_alpha 90.00
_cell_angle_beta 93.7590(10)
_cell_angle_gamma 90.00
_cell_formula_units_Z 4
_cell_length_a 9.6650(3)
_cell_length_b 33.8756(9)
_cell_length_c 11.1543(5)
_cell_measurement_reflns_used 8389
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 27.88
_cell_measurement_theta_min 0.41
_cell_volume 3644.1(2)
_computing_cell_refinement
;
DENZO-SMN (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Hooft, 2004)
;
_computing_data_reduction
;
DENZO-SMN (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type 'Bruker--Nonius KappaCCD'
_diffrn_measurement_method '\f scans, and \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0476
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 44
_diffrn_reflns_limit_k_min -44
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 16724
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.018
_diffrn_reflns_theta_min 1.202
_diffrn_standards_decay_% 0
_diffrn_standards_interval_count 0
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.076
_exptl_absorpt_correction_type none
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.210
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1432
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.15
_refine_diff_density_max 0.266
_refine_diff_density_min -0.308
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.060
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 450
_refine_ls_number_reflns 8666
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.060
_refine_ls_R_factor_all 0.0798
_refine_ls_R_factor_gt 0.0481
_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^)+(0.0606P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1105
_refine_ls_wR_factor_ref 0.1219
_reflns_number_gt 6067
_reflns_number_total 8666
_reflns_threshold_expression >2sigma(I)
_cod_data_source_file rz5179sup1.cif
_cod_data_source_block I
_cod_original_cell_volume 3644.2(2)
_cod_database_code 2241389
_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_hkl_file
;
1 0 0 2086.87 20.27 0
2 0 0 2713.67 43.31 0
3 0 0 9372.62 205.27 0
4 0 0 846.63 14.53 0
5 0 0 606.92 16.68 0
6 0 0 -2.69 3.77 0
7 0 0 50.58 5.65 0
8 0 0 22.60 5.92 0
9 0 0 640.55 18.56 0
10 0 0 181.86 11.30 0
11 0 0 51.38 9.95 0
12 0 0 112.18 18.56 0
-1 -1 0 175.00 10.27 0
1 1 0 176.00 10.54 0
2 1 0 159.53 6.99 0
-2 -1 0 193.43 4.30 0
-3 -1 0 503.35 8.88 0
3 1 0 453.58 12.11 0
4 1 0 139.36 5.38 0
-4 -1 0 151.46 3.23 0
-5 -1 0 1196.63 23.67 0
5 1 0 1097.09 26.90 0
-6 -1 0 2.96 3.77 0
6 1 0 -0.27 3.77 0
7 1 0 616.07 17.22 0
-7 -1 0 605.31 16.41 0
-8 -1 0 9.15 5.92 0
8 1 0 18.02 9.15 0
-9 -1 0 154.69 9.68 0
9 1 0 181.32 10.22 0
-10 -1 0 8.07 7.53 0
10 1 0 9.15 11.30 0
11 1 0 50.04 9.95 0
-11 -1 0 37.39 9.68 0
12 1 0 -19.91 7.26 0
-12 -1 0 -12.38 14.80 0
0 2 0 21.00 4.27 0
0 -2 0 20.95 4.27 0
-1 -2 0 1884.00 10.81 0
1 2 0 1891.00 10.81 0
2 2 0 617.95 14.80 0
-2 -2 0 681.18 11.57 0
-3 -2 0 1110.81 18.29 0
3 2 0 1023.38 24.48 0
-4 -2 0 71.83 2.15 0
4 2 0 60.53 2.96 0
5 2 0 11.03 3.50 0
-5 -2 0 14.26 1.35 0
-6 -2 0 444.43 8.34 0
6 2 0 395.74 12.11 0
7 2 0 325.25 11.03 0
-7 -2 0 340.86 11.84 0
8 2 0 361.03 12.38 0
-8 -2 0 354.58 12.64 0
-9 -2 0 2.42 6.46 0
9 2 0 18.83 9.68 0
-10 -2 0 11.30 6.46 0
10 2 0 5.38 7.80 0
11 2 0 28.79 9.68 0
-11 -2 0 25.02 14.53 0
12 2 0 17.76 8.61 0
-12 -2 0 20.45 12.11 0
-1 -3 0 21.88 4.54 0
1 3 0 20.54 5.27 0
-3 -3 0 306.69 5.65 0
3 3 0 261.76 7.26 0
-4 -3 0 9.68 1.35 0
4 3 0 8.34 2.69 0
5 3 0 27.44 5.11 0
-5 -3 0 25.02 1.61 0
-6 -3 0 136.67 3.77 0
6 3 0 123.48 5.92 0
7 3 0 202.31 8.61 0
-7 -3 0 216.30 8.88 0
8 3 0 1323.34 35.24 0
-8 -3 0 1239.67 31.75 0
9 3 0 15.07 6.73 0
-9 -3 0 9.42 9.42 0
10 3 0 199.62 11.30 0
-10 -3 0 200.42 11.84 0
11 3 0 6.99 9.15 0
-11 -3 0 11.03 7.53 0
-12 -3 0 11.57 15.87 0
12 3 0 26.90 10.76 0
0 -4 0 7020.00 21.08 0
0 4 0 7021.00 20.81 0
-1 -4 0 335.48 6.73 0
1 4 0 329.79 6.46 0
2 4 0 9.15 1.61 0
-2 -4 0 5.65 0.54 0
-3 -4 0 94.70 2.42 0
3 4 0 101.15 3.77 0
4 4 0 36.59 3.50 0
-4 -4 0 40.08 1.61 0
5 4 0 10.22 3.50 0
-5 -4 0 6.73 1.61 0
-6 -4 0 28.25 1.88 0
6 4 0 31.75 3.77 0
7 4 0 59.45 5.92 0
-7 -4 0 57.57 5.92 0
-8 -4 0 -2.69 6.19 0
8 4 0 -4.04 5.65 0
-9 -4 0 17.76 7.26 0
9 4 0 12.64 10.22 0
10 4 0 37.66 8.07 0
-10 -4 0 39.55 8.34 0
11 4 0 0.54 9.42 0
-11 -4 0 6.46 9.68 0
-12 -4 0 31.21 16.68 0
12 4 0 57.30 11.57 0
1 5 0 392.24 6.99 0
-1 -5 0 387.94 6.99 0
-2 -5 0 3801.08 85.82 0
2 5 0 3499.77 77.48 0
3 5 0 3284.55 107.34 0
-3 -5 0 3190.66 60.26 0
4 5 0 1142.02 26.90 0
-4 -5 0 1210.89 19.91 0
5 5 0 1208.47 31.75 0
-5 -5 0 1177.80 19.91 0
-6 -5 0 289.74 9.95 0
6 5 0 282.21 9.15 0
-7 -5 0 100.08 6.99 0
7 5 0 91.20 6.46 0
-8 -5 0 274.14 11.03 0
8 5 0 276.56 11.03 0
-9 -5 0 567.92 18.56 0
9 5 0 550.16 17.49 0
10 5 0 115.68 14.26 0
-10 -5 0 123.48 10.22 0
11 5 0 23.41 9.15 0
-11 -5 0 2.69 9.42 0
-12 -5 0 92.81 16.95 0
12 5 0 43.58 11.30 0
0 6 0 578.95 20.45 0
0 -6 0 545.59 21.52 0
-1 -6 0 72.64 2.42 0
1 6 0 81.78 2.96 0
2 6 0 2056.98 46.54 0
-2 -6 0 2052.67 47.35 0
3 6 0 2762.37 61.61 0
-3 -6 0 2904.95 52.46 0
4 6 0 1193.40 30.67 0
-4 -6 0 1192.33 19.91 0
-5 -6 0 442.28 8.34 0
5 6 0 447.12 12.38 0
-6 -6 0 37.93 2.69 0
6 6 0 40.62 4.57 0
7 6 0 695.16 19.64 0
-7 -6 0 750.85 30.40 0
8 6 0 3.23 4.84 0
-8 -6 0 -1.08 4.04 0
9 6 0 60.80 6.99 0
-9 -6 0 61.61 8.61 0
-10 -6 0 7.26 7.53 0
10 6 0 -3.77 7.53 0
-11 -6 0 22.06 9.42 0
11 6 0 4.30 8.88 0
12 6 0 8.61 10.49 0
-12 -6 0 31.21 15.60 0
1 7 0 7.45 1.35 0
-1 -7 0 6.91 1.35 0
2 7 0 256.65 5.38 0
-2 -7 0 248.04 6.73 0
-3 -7 0 129.67 4.57 0
3 7 0 108.69 5.92 0
-4 -7 0 624.41 12.91 0
4 7 0 674.45 26.10 0
-5 -7 0 289.74 5.92 0
5 7 0 319.33 10.49 0
6 7 0 9.95 4.04 0
-6 -7 0 10.49 2.69 0
7 7 0 67.53 8.34 0
-7 -7 0 82.86 6.19 0
8 7 0 389.55 13.72 0
-8 -7 0 356.19 13.18 0
-9 -7 0 95.50 8.61 0
9 7 0 108.15 8.61 0
10 7 0 9.95 7.53 0
-10 -7 0 19.10 6.73 0
-11 -7 0 37.13 13.99 0
11 7 0 46.27 9.42 0
12 7 0 156.04 20.18 0
-12 -7 0 135.59 12.38 0
-1 -8 0 2529.93 56.23 0
1 8 0 2659.33 61.34 0
2 8 0 3486.32 64.30 0
-2 -8 0 3121.52 98.19 0
3 8 0 2057.79 46.81 0
-3 -8 0 2028.19 45.20 0
-4 -8 0 226.79 5.38 0
4 8 0 211.19 6.99 0
-5 -8 0 774.53 13.99 0
5 8 0 677.41 24.75 0
-6 -8 0 270.91 7.53 0
6 8 0 246.16 8.88 0
7 8 0 22.87 5.11 0
-7 -8 0 21.79 5.38 0
-8 -8 0 1114.04 30.40 0
8 8 0 1128.57 29.05 0
9 8 0 122.41 9.15 0
-9 -8 0 123.75 8.88 0
-10 -8 0 9.15 8.34 0
10 8 0 6.19 7.53 0
-11 -8 0 16.14 10.22 0
11 8 0 24.48 8.34 0
12 8 0 43.58 11.84 0
-12 -8 0 30.67 9.68 0
1 9 0 2598.26 58.38 0
-1 -9 0 2790.88 64.03 0
-2 -9 0 -2.15 1.35 0
2 9 0 -1.61 1.35 0
-3 -9 0 225.98 6.73 0
3 9 0 228.94 6.99 0
-4 -9 0 221.95 7.53 0
4 9 0 198.27 6.73 0
-5 -9 0 396.55 7.26 0
5 9 0 400.58 11.84 0
6 9 0 6.19 4.04 0
-6 -9 0 1.88 1.08 0
7 9 0 12.91 5.11 0
-7 -9 0 15.60 7.80 0
-8 -9 0 116.49 8.34 0
8 9 0 97.66 7.53 0
9 9 0 286.24 12.64 0
-9 -9 0 300.50 18.83 0
10 9 0 41.70 8.61 0
-10 -9 0 44.12 12.91 0
-11 -9 0 -1.88 9.42 0
11 9 0 7.53 9.42 0
-12 -9 0 94.70 12.64 0
12 9 0 107.07 11.03 0
1 10 0 2900.38 64.84 0
-1 -10 0 3051.57 70.22 0
-2 -10 0 579.48 15.07 0
2 10 0 518.41 18.02 0
-3 -10 0 1713.97 38.47 0
3 10 0 1747.87 41.43 0
4 10 0 1384.41 33.63 0
-4 -10 0 1369.08 32.82 0
-5 -10 0 451.96 13.18 0
5 10 0 460.30 12.38 0
-6 -10 0 193.43 4.57 0
6 10 0 177.83 7.80 0
7 10 0 114.34 6.19 0
-7 -10 0 134.24 6.99 0
8 10 0 808.16 23.14 0
-8 -10 0 760.81 21.25 0
9 10 0 156.30 9.68 0
-9 -10 0 160.07 9.95 0
-10 -10 0 205.00 12.11 0
10 10 0 184.28 11.03 0
-11 -10 0 -7.26 9.68 0
11 10 0 9.95 13.45 0
12 10 0 26.36 15.60 0
-12 -10 0 25.29 11.84 0
1 11 0 85.55 3.50 0
-1 -11 0 80.44 2.96 0
2 11 0 881.87 20.98 0
-2 -11 0 879.99 21.25 0
-3 -11 0 559.58 15.07 0
3 11 0 563.88 11.03 0
4 11 0 1093.06 26.10 0
-4 -11 0 1090.63 26.90 0
5 11 0 904.20 22.33 0
-5 -11 0 897.20 22.60 0
-6 -11 0 1.61 2.42 0
6 11 0 -0.81 4.04 0
7 11 0 552.04 16.41 0
-7 -11 0 514.38 15.33 0
8 11 0 9.68 5.92 0
-8 -11 0 -5.65 5.92 0
9 11 0 2.69 5.38 0
-9 -11 0 10.49 7.26 0
10 11 0 100.88 9.95 0
-10 -11 0 96.85 9.68 0
11 11 0 11.57 9.68 0
-11 -11 0 -11.84 9.68 0
-12 -11 0 77.75 13.18 0
12 11 0 100.88 12.38 0
1 12 0 1424.77 32.82 0
-1 -12 0 1478.30 34.44 0
2 12 0 13.18 2.15 0
-2 -12 0 12.11 2.15 0
3 12 0 729.60 14.26 0
-3 -12 0 713.73 18.02 0
-4 -12 0 4.57 2.42 0
4 12 0 0.54 2.42 0
-5 -12 0 0.27 3.50 0
5 12 0 -0.81 3.23 0
-6 -12 0 16.14 3.23 0
6 12 0 24.48 6.46 0
7 12 0 47.89 8.34 0
-7 -12 0 37.13 6.19 0
8 12 0 234.86 9.95 0
-8 -12 0 250.19 11.57 0
9 12 0 249.12 11.57 0
-9 -12 0 218.45 11.30 0
-10 -12 0 137.47 11.03 0
10 12 0 125.64 9.15 0
11 12 0 10.49 9.42 0
-11 -12 0 0.81 13.99 0
-12 -12 0 78.82 13.18 0
12 12 0 50.04 12.11 0
1 13 0 590.78 16.95 0
-1 -13 0 534.29 18.83 0
-2 -13 0 984.64 23.14 0
2 13 0 1004.81 26.36 0
3 13 0 2097.33 50.58 0
-3 -13 0 1971.97 44.66 0
-4 -13 0 1.88 3.23 0
4 13 0 -0.81 2.69 0
-5 -13 0 37.39 4.57 0
5 13 0 33.09 4.04 0
-6 -13 0 377.98 9.42 0
6 13 0 389.28 12.64 0
7 13 0 565.49 16.68 0
-7 -13 0 561.46 17.22 0
8 13 0 98.73 10.76 0
-8 -13 0 108.96 11.57 0
-9 -13 0 -2.96 6.99 0
9 13 0 11.84 6.99 0
10 13 0 9.42 7.80 0
-10 -13 0 12.64 8.88 0
-11 -13 0 16.95 10.76 0
11 13 0 29.05 14.80 0
12 13 0 -4.57 11.84 0
-12 -13 0 9.95 11.57 0
-1 -14 0 51.92 3.23 0
1 14 0 49.23 2.69 0
2 14 0 149.58 5.11 0
-2 -14 0 173.52 6.19 0
3 14 0 175.67 4.57 0
-3 -14 0 154.42 7.80 0
-4 -14 0 27.98 3.50 0
4 14 0 30.13 3.23 0
5 14 0 108.42 5.92 0
-5 -14 0 104.92 5.92 0
-6 -14 0 304.54 10.76 0
6 14 0 285.44 9.68 0
7 14 0 103.84 6.99 0
-7 -14 0 108.42 7.53 0
8 14 0 15.60 8.61 0
-8 -14 0 19.91 6.73 0
-9 -14 0 1.35 9.95 0
9 14 0 9.42 6.99 0
-10 -14 0 69.14 10.22 0
10 14 0 87.16 7.80 0
-11 -14 0 -8.34 10.49 0
11 14 0 -1.35 9.68 0
12 14 0 18.29 11.30 0
-12 -14 0 20.98 12.11 0
1 15 0 300.50 8.88 0
-1 -15 0 310.99 9.68 0
2 15 0 148.23 5.38 0
-2 -15 0 151.19 7.80 0
3 15 0 226.79 6.99 0
-3 -15 0 234.05 7.26 0
4 15 0 0.81 2.96 0
-4 -15 0 1.88 3.23 0
5 15 0 258.00 8.61 0
-5 -15 0 221.68 8.07 0
6 15 0 418.34 12.64 0
-6 -15 0 450.89 13.99 0
-7 -15 0 305.61 11.84 0
7 15 0 352.69 12.38 0
-8 -15 0 460.57 15.87 0
8 15 0 438.51 14.53 0
9 15 0 134.24 13.18 0
-9 -15 0 124.56 9.68 0
10 15 0 17.49 8.34 0
-10 -15 0 18.83 9.15 0
11 15 0 5.65 9.95 0
-11 -15 0 4.57 9.95 0
12 15 0 8.88 11.57 0
-12 -15 0 14.80 11.84 0
-1 -16 0 821.61 21.52 0
1 16 0 727.99 17.49 0
-2 -16 0 219.26 7.26 0
2 16 0 214.41 6.73 0
3 16 0 1664.20 32.82 0
-3 -16 0 1475.88 35.78 0
4 16 0 34.70 3.77 0
-4 -16 0 42.24 3.77 0
-5 -16 0 18.02 4.57 0
5 16 0 8.61 3.77 0
6 16 0 390.63 12.38 0
-6 -16 0 423.18 13.72 0
-7 -16 0 14.26 5.92 0
7 16 0 13.72 5.38 0
-8 -16 0 16.68 5.38 0
8 16 0 19.64 5.11 0
9 16 0 22.87 7.53 0
-9 -16 0 44.39 12.38 0
-10 -16 0 8.34 8.88 0
10 16 0 21.79 8.61 0
-11 -16 0 6.73 11.03 0
11 16 0 6.99 9.68 0
-1 -17 0 0.27 2.15 0
1 17 0 0.54 2.15 0
-2 -17 0 204.46 6.73 0
2 17 0 190.74 6.46 0
3 17 0 40.35 2.15 0
-3 -17 0 39.01 3.77 0
4 17 0 445.24 12.64 0
-4 -17 0 458.96 13.45 0
5 17 0 189.39 7.53 0
-5 -17 0 186.70 7.53 0
6 17 0 -1.35 3.23 0
-6 -17 0 -5.92 4.84 0
-7 -17 0 0.54 9.15 0
7 17 0 2.15 5.11 0
8 17 0 0.81 5.92 0
-8 -17 0 4.84 6.46 0
9 17 0 4.57 6.99 0
-9 -17 0 -2.69 8.07 0
10 17 0 17.76 6.99 0
-10 -17 0 15.87 9.42 0
-11 -17 0 26.10 15.87 0
11 17 0 -2.69 8.07 0
1 18 0 620.38 15.87 0
-1 -18 0 633.02 16.68 0
2 18 0 1394.10 34.44 0
-2 -18 0 1541.79 54.07 0
-3 -18 0 312.61 10.22 0
3 18 0 342.20 8.07 0
4 18 0 121.06 5.65 0
-4 -18 0 107.34 5.65 0
-5 -18 0 438.24 13.18 0
5 18 0 476.45 14.53 0
-6 -18 0 19.91 5.38 0
6 18 0 27.44 4.84 0
-7 -18 0 -2.69 5.92 0
7 18 0 5.38 4.30 0
8 18 0 55.42 9.95 0
-8 -18 0 52.73 7.53 0
-9 -18 0 1.35 7.80 0
9 18 0 8.07 5.92 0
-10 -18 0 2.15 7.80 0
10 18 0 4.84 6.73 0
11 18 0 109.22 9.42 0
-11 -18 0 94.43 10.76 0
-1 -19 0 260.96 8.07 0
1 19 0 237.28 7.26 0
2 19 0 5.92 2.15 0
-2 -19 0 2.15 2.69 0
3 19 0 1.08 1.61 0
-3 -19 0 -1.35 3.23 0
-4 -19 0 189.93 7.53 0
4 19 0 192.89 6.99 0
-5 -19 0 358.88 12.11 0
5 19 0 345.70 10.76 0
-6 -19 0 593.47 17.76 0
6 19 0 585.13 16.68 0
-7 -19 0 1.88 6.19 0
7 19 0 0.54 5.11 0
8 19 0 121.06 8.61 0
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-1 -8 -14 39.55 18.02 0
1 8 14 77.48 11.84 0
-2 -8 -14 4.57 16.41 0
2 8 14 0.81 13.99 0
-3 -9 14 21.25 16.95 0
3 9 -14 15.07 13.72 0
-2 -9 14 4.30 9.15 0
2 9 -14 16.14 13.72 0
-1 -9 14 40.62 11.30 0
1 9 -14 22.60 13.45 0
0 -9 -14 10.22 9.68 0
0 9 14 21.52 10.49 0
-1 -9 -14 -0.54 12.11 0
1 9 14 15.33 10.76 0
-2 -9 -14 -22.60 15.60 0
-3 -10 14 -4.04 16.41 0
3 10 -14 -8.34 12.64 0
-2 -10 14 60.80 18.02 0
2 10 -14 17.49 13.45 0
-1 -10 14 71.02 11.84 0
1 10 -14 63.76 12.38 0
0 -10 -14 79.63 10.76 0
0 10 14 50.31 11.30 0
-1 -10 -14 -3.77 9.15 0
1 10 14 9.68 14.26 0
3 11 -14 34.70 13.99 0
-2 -11 14 1.61 16.95 0
2 11 -14 25.56 14.80 0
-1 -11 14 68.33 10.76 0
1 11 -14 66.45 11.84 0
0 -11 -14 18.02 8.88 0
0 11 14 7.53 14.53 0
-1 -11 -14 49.77 18.02 0
-2 -12 14 16.68 18.56 0
2 12 -14 0.00 13.99 0
-1 -12 14 13.72 16.41 0
1 12 -14 16.41 14.53 0
0 -12 -14 1.08 8.88 0
0 12 14 -6.19 14.53 0
-1 -12 -14 57.03 16.95 0
-1 -13 14 118.37 19.37 0
0 -13 -14 -13.72 10.76 0
;
_shelx_hkl_checksum 40225
_shelx_res_file
;
C:\Crystal\x-step32\jtfeb12c.res created by SHELXL-2014/7
TITL GUA4EEBPH4 (MONOKLINIC, P21/C)
CELL 0.71073 9.66500 33.87560 11.15430 90.00000 93.75900 90.00000
ZERR 4 0.00030 0.00090 0.00050 0.00000 0.00100 0.00000
LATT 1
SYMM -X, Y+ 0.50000, -Z+ 0.50000
SFAC C B N O H
UNIT 160 4 20 12 216
TEMP -173
PLAN 20
FMAP 2
L.S. 5
BOND $H
ACTA
CONF
WGHT 0.060600
FVAR 0.52513
C1 1 0.840932 0.123841 0.925149 11.00000 0.01524 0.01596 =
0.01116 0.00070 0.00110 -0.00232
N1 3 0.733516 0.141316 0.973240 11.00000 0.01156 0.02493 =
0.01305 -0.00070 0.00098 -0.00062
N2 3 0.832129 0.113148 0.809542 11.00000 0.01921 0.02099 =
0.01098 -0.00008 0.00004 -0.00049
N3 3 0.958538 0.116949 0.995671 11.00000 0.01239 0.01924 =
0.01111 0.00107 0.00205 -0.00076
C2 1 0.749393 0.171001 1.067824 11.00000 0.02037 0.02434 =
0.01710 -0.00384 0.00577 0.00174
AFIX 137
H2A 5 0.847768 0.177594 1.082549 11.00000 -1.50000
H2B 5 0.713602 0.160572 1.141674 11.00000 -1.50000
H2C 5 0.697479 0.194785 1.042810 11.00000 -1.50000
AFIX 0
C3 1 0.590412 0.133367 0.929913 11.00000 0.01310 0.03865 =
0.02598 0.00398 0.00031 -0.00032
AFIX 137
H3A 5 0.587396 0.109691 0.879322 11.00000 -1.50000
H3B 5 0.553943 0.155929 0.882788 11.00000 -1.50000
H3C 5 0.533837 0.129145 0.998545 11.00000 -1.50000
AFIX 0
C4 1 0.899267 0.077499 0.767167 11.00000 0.02808 0.02431 =
0.01505 -0.00468 0.00086 0.00148
AFIX 137
H4A 5 0.974703 0.084957 0.717119 11.00000 -1.50000
H4B 5 0.831144 0.061531 0.719731 11.00000 -1.50000
H4C 5 0.936900 0.062145 0.836282 11.00000 -1.50000
AFIX 0
C5 1 0.751318 0.135345 0.717056 11.00000 0.02850 0.02597 =
0.01272 0.00176 -0.00317 0.00000
AFIX 137
H5A 5 0.667350 0.120513 0.691812 11.00000 -1.50000
H5B 5 0.807033 0.139428 0.647800 11.00000 -1.50000
H5C 5 0.725358 0.160986 0.749512 11.00000 -1.50000
AFIX 0
C6 1 1.096495 0.117744 0.946742 11.00000 0.01248 0.02105 =
0.01978 0.00145 0.00397 0.00198
AFIX 23
H6A 5 1.086961 0.127095 0.862516 11.00000 -1.20000
H6B 5 1.134312 0.090586 0.946516 11.00000 -1.20000
AFIX 0
C7 1 1.197808 0.144342 1.018543 11.00000 0.01345 0.02655 =
0.02085 0.00573 -0.00062 -0.00053
AFIX 23
H7A 5 1.289727 0.142199 0.984792 11.00000 -1.20000
H7B 5 1.207626 0.134633 1.102383 11.00000 -1.20000
AFIX 0
C8 1 1.156003 0.187798 1.019988 11.00000 0.01900 0.02603 =
0.01336 0.00069 -0.00404 -0.00387
AFIX 23
H8A 5 1.061203 0.189940 1.048019 11.00000 -1.20000
H8B 5 1.219602 0.202090 1.078096 11.00000 -1.20000
AFIX 0
N4 3 1.159084 0.206716 0.902286 11.00000 0.01622 0.02299 =
0.01725 0.00388 0.00099 -0.00403
C9 1 1.287887 0.226395 0.877188 11.00000 0.01780 0.02523 =
0.02769 0.00164 0.00324 -0.00426
AFIX 137
H9A 5 1.270521 0.244902 0.810364 11.00000 -1.50000
H9B 5 1.356154 0.206680 0.855571 11.00000 -1.50000
H9C 5 1.323714 0.240855 0.948730 11.00000 -1.50000
AFIX 0
C10 1 1.036761 0.211110 0.832958 11.00000 0.02188 0.01468 =
0.01307 -0.00080 0.00116 -0.00110
O1 4 0.923021 0.206264 0.874734 11.00000 0.01626 0.03042 =
0.01630 0.00249 0.00165 -0.00417
N5 3 1.048503 0.221958 0.714484 11.00000 0.02192 0.02283 =
0.01286 0.00059 0.00305 0.00110
C11 1 0.918777 0.231467 0.645567 11.00000 0.03105 0.02311 =
0.01554 0.00190 -0.00310 -0.00185
AFIX 137
H11A 5 0.872245 0.206990 0.618952 11.00000 -1.50000
H11B 5 0.938821 0.247352 0.575352 11.00000 -1.50000
H11C 5 0.858368 0.246429 0.696231 11.00000 -1.50000
AFIX 0
C12 1 1.146265 0.201451 0.641731 11.00000 0.04107 0.03044 =
0.02233 -0.00115 0.01218 0.00555
AFIX 137
H12A 5 1.221636 0.190316 0.694269 11.00000 -1.50000
H12B 5 1.184602 0.220132 0.585585 11.00000 -1.50000
H12C 5 1.098134 0.180151 0.596539 11.00000 -1.50000
AFIX 0
C13 1 0.948995 0.101559 1.116805 11.00000 0.01794 0.02106 =
0.01230 0.00194 -0.00193 -0.00189
AFIX 23
H13A 5 0.895323 0.120285 1.163654 11.00000 -1.20000
H13B 5 1.043361 0.099561 1.156568 11.00000 -1.20000
AFIX 0
C14 1 0.880684 0.061633 1.117574 11.00000 0.01508 0.02244 =
0.01480 0.00018 0.00110 0.00044
O2 4 0.831815 0.044339 1.030913 11.00000 0.05490 0.03394 =
0.01586 -0.00343 0.00003 -0.02081
O3 4 0.879434 0.048867 1.230217 11.00000 0.02717 0.02313 =
0.01507 0.00488 -0.00199 -0.00907
C15 1 0.811307 0.011311 1.250498 11.00000 0.03147 0.02399 =
0.02327 0.00545 -0.00346 -0.01180
AFIX 23
H15A 5 0.852204 -0.009826 1.202757 11.00000 -1.20000
H15B 5 0.711054 0.013146 1.226561 11.00000 -1.20000
AFIX 0
C16 1 0.832843 0.002515 1.381699 11.00000 0.04871 0.03636 =
0.02885 0.01441 -0.01336 -0.01989
AFIX 137
H16A 5 0.932209 -0.000443 1.403381 11.00000 -1.50000
H16B 5 0.784695 -0.022019 1.399804 11.00000 -1.50000
H16C 5 0.795744 0.024239 1.427938 11.00000 -1.50000
AFIX 0
B1 2 0.340420 0.115346 0.399386 11.00000 0.01436 0.01696 =
0.01134 -0.00065 -0.00015 0.00165
C17 1 0.438425 0.155045 0.393513 11.00000 0.01198 0.01780 =
0.01727 -0.00018 0.00080 0.00445
C18 1 0.497816 0.173487 0.497701 11.00000 0.01468 0.02202 =
0.01894 -0.00060 -0.00081 0.00324
AFIX 43
H18A 5 0.484361 0.161765 0.573428 11.00000 -1.20000
AFIX 0
C19 1 0.575266 0.208061 0.495016 11.00000 0.01550 0.02301 =
0.02805 -0.00800 -0.00162 0.00266
AFIX 43
H19A 5 0.613162 0.219274 0.568024 11.00000 -1.20000
AFIX 0
C20 1 0.597566 0.226259 0.386824 11.00000 0.01605 0.01786 =
0.03979 -0.00367 0.00708 -0.00046
AFIX 43
H20A 5 0.652279 0.249510 0.384480 11.00000 -1.20000
AFIX 0
C21 1 0.538207 0.209758 0.282087 11.00000 0.02227 0.02210 =
0.02530 0.00167 0.01144 0.00283
AFIX 43
H21A 5 0.549958 0.222177 0.207071 11.00000 -1.20000
AFIX 0
C22 1 0.461458 0.175089 0.286163 11.00000 0.01691 0.02213 =
0.01682 -0.00115 0.00235 0.00221
AFIX 43
H22A 5 0.422634 0.164409 0.212720 11.00000 -1.20000
AFIX 0
C23 1 0.355483 0.085792 0.282638 11.00000 0.01779 0.01658 =
0.01065 0.00262 -0.00119 0.00439
C24 1 0.472677 0.083869 0.215270 11.00000 0.01933 0.02158 =
0.01794 0.00145 0.00281 0.00084
AFIX 43
H24A 5 0.549353 0.100520 0.236986 11.00000 -1.20000
AFIX 0
C25 1 0.481220 0.058504 0.117697 11.00000 0.02713 0.02337 =
0.01731 0.00152 0.00719 0.00789
AFIX 43
H25A 5 0.562631 0.058330 0.074377 11.00000 -1.20000
AFIX 0
C26 1 0.372520 0.033592 0.083250 11.00000 0.03299 0.02192 =
0.01180 -0.00247 -0.00181 0.01080
AFIX 43
H26A 5 0.377092 0.016987 0.014989 11.00000 -1.20000
AFIX 0
C27 1 0.257078 0.033314 0.150053 11.00000 0.02462 0.02090 =
0.01908 -0.00282 -0.00555 0.00212
AFIX 43
H27A 5 0.182471 0.015825 0.129342 11.00000 -1.20000
AFIX 0
C28 1 0.250089 0.058669 0.247734 11.00000 0.01817 0.02084 =
0.01430 0.00005 0.00003 0.00390
AFIX 43
H28A 5 0.170290 0.057610 0.293031 11.00000 -1.20000
AFIX 0
C29 1 0.176919 0.129552 0.399474 11.00000 0.01673 0.01823 =
0.00649 -0.00427 -0.00010 0.00122
C30 1 0.128272 0.165487 0.349576 11.00000 0.01772 0.02031 =
0.00851 -0.00011 -0.00052 -0.00021
AFIX 43
H30A 5 0.192996 0.182775 0.316302 11.00000 -1.20000
AFIX 0
C31 1 -0.009794 0.176869 0.346670 11.00000 0.02198 0.02214 =
0.01170 -0.00113 -0.00300 0.00577
AFIX 43
H31A 5 -0.036962 0.201669 0.313048 11.00000 -1.20000
AFIX 0
C32 1 -0.108369 0.152398 0.392350 11.00000 0.01654 0.02815 =
0.01253 -0.00561 -0.00110 0.00556
AFIX 43
H32A 5 -0.202942 0.160151 0.390601 11.00000 -1.20000
AFIX 0
C33 1 -0.065882 0.116276 0.440768 11.00000 0.01805 0.02599 =
0.01029 -0.00215 0.00267 -0.00194
AFIX 43
H33A 5 -0.131947 0.098781 0.471192 11.00000 -1.20000
AFIX 0
C34 1 0.073629 0.105698 0.444716 11.00000 0.01886 0.01907 =
0.01026 -0.00021 0.00026 0.00189
AFIX 43
H34A 5 0.100234 0.081070 0.479841 11.00000 -1.20000
AFIX 0
C35 1 0.387595 0.090290 0.521894 11.00000 0.01544 0.01708 =
0.01329 -0.00078 -0.00231 -0.00227
C36 1 0.336047 0.098531 0.634225 11.00000 0.01701 0.01963 =
0.01582 -0.00081 -0.00193 0.00051
AFIX 43
H36A 5 0.268384 0.118703 0.639214 11.00000 -1.20000
AFIX 0
C37 1 0.380382 0.078243 0.738623 11.00000 0.02067 0.02719 =
0.01160 -0.00022 -0.00009 -0.00449
AFIX 43
H37A 5 0.342167 0.084597 0.812541 11.00000 -1.20000
AFIX 0
C38 1 0.479459 0.048989 0.735117 11.00000 0.02218 0.02260 =
0.01570 0.00484 -0.00517 -0.00311
AFIX 43
H38A 5 0.510465 0.035330 0.806264 11.00000 -1.20000
AFIX 0
C39 1 0.532993 0.039845 0.626338 11.00000 0.02069 0.01821 =
0.02253 0.00050 -0.00501 0.00208
AFIX 43
H39A 5 0.600966 0.019711 0.622398 11.00000 -1.20000
AFIX 0
C40 1 0.487093 0.060197 0.522668 11.00000 0.01961 0.02069 =
0.01495 -0.00141 -0.00036 0.00180
AFIX 43
H40A 5 0.525059 0.053342 0.449043 11.00000 -1.20000
AFIX 0
HKLF 4
REM GUA4EEBPH4 (MONOKLINIC, P21/C)
REM R1 = 0.0481 for 6067 Fo > 4sig(Fo) and 0.0798 for all 8666 data
REM 450 parameters refined using 0 restraints
END
WGHT 0.0606 0.0000
REM Highest difference peak 0.266, deepest hole -0.308, 1-sigma level 0.051
Q1 1 0.3450 0.1026 0.3277 11.00000 0.05 0.27
Q2 1 1.2349 0.2082 0.6591 11.00000 0.05 0.24
Q3 1 0.2558 0.1225 0.3947 11.00000 0.05 0.23
Q4 1 0.9080 0.0322 1.0611 11.00000 0.05 0.23
Q5 1 0.1579 0.1517 0.3921 11.00000 0.05 0.22
Q6 1 0.3683 0.1387 0.4187 11.00000 0.05 0.22
Q7 1 1.1764 0.1646 1.0171 11.00000 0.05 0.21
Q8 1 0.3874 0.1099 0.4788 11.00000 0.05 0.21
Q9 1 0.9506 0.1447 1.0180 11.00000 0.05 0.20
Q10 1 0.3993 0.1029 0.5812 11.00000 0.05 0.20
Q11 1 0.7959 0.1040 0.8590 11.00000 0.05 0.20
Q12 1 -0.0854 0.1279 0.3924 11.00000 0.05 0.20
Q13 1 0.4078 0.1327 0.3922 11.00000 0.05 0.20
Q14 1 0.3280 0.0769 0.6927 11.00000 0.05 0.20
Q15 1 0.0052 0.2099 0.3376 11.00000 0.05 0.20
Q16 1 0.0111 0.1169 0.4685 11.00000 0.05 0.19
Q17 1 0.7615 -0.0002 1.1948 11.00000 0.05 0.19
Q18 1 0.0064 0.1094 0.4073 11.00000 0.05 0.19
Q19 1 0.4731 0.0469 0.5789 11.00000 0.05 0.19
Q20 1 0.4224 0.1747 0.3445 11.00000 0.05 0.18
;
_shelx_res_checksum 63267
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, 1/2+y, 1/2-z'
'-x, -y, -z'
'x, 1/2-y, 1/2+z'
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
C C1 0.84093(14) 0.12384(4) 0.92515(11) 0.0141(3) Uani d 1
N N1 0.73352(12) 0.14132(4) 0.97324(9) 0.0165(3) Uani d 1
N N2 0.83213(12) 0.11315(4) 0.80954(10) 0.0171(3) Uani d 1
N N3 0.95854(12) 0.11695(3) 0.99567(9) 0.0142(2) Uani d 1
C C2 0.74939(16) 0.17100(4) 1.06782(12) 0.0204(3) Uani d 1
H H2A 0.8478 0.1776 1.0825 0.031 Uiso calc 1
H H2B 0.7136 0.1606 1.1417 0.031 Uiso calc 1
H H2C 0.6975 0.1948 1.0428 0.031 Uiso calc 1
C C3 0.59041(15) 0.13337(5) 0.92991(13) 0.0260(4) Uani d 1
H H3A 0.5874 0.1097 0.8793 0.039 Uiso calc 1
H H3B 0.5539 0.1559 0.8828 0.039 Uiso calc 1
H H3C 0.5338 0.1291 0.9985 0.039 Uiso calc 1
C C4 0.89927(16) 0.07750(5) 0.76717(12) 0.0225(3) Uani d 1
H H4A 0.9747 0.0850 0.7171 0.034 Uiso calc 1
H H4B 0.8311 0.0615 0.7197 0.034 Uiso calc 1
H H4C 0.9369 0.0621 0.8363 0.034 Uiso calc 1
C C5 0.75132(16) 0.13535(5) 0.71706(12) 0.0226(3) Uani d 1
H H5A 0.6674 0.1205 0.6918 0.034 Uiso calc 1
H H5B 0.8070 0.1394 0.6478 0.034 Uiso calc 1
H H5C 0.7254 0.1610 0.7495 0.034 Uiso calc 1
C C6 1.09650(14) 0.11774(4) 0.94674(12) 0.0176(3) Uani d 1
H H6A 1.0870 0.1271 0.8625 0.021 Uiso calc 1
H H6B 1.1343 0.0906 0.9465 0.021 Uiso calc 1
C C7 1.19781(15) 0.14434(4) 1.01854(13) 0.0204(3) Uani d 1
H H7A 1.2897 0.1422 0.9848 0.024 Uiso calc 1
H H7B 1.2076 0.1346 1.1024 0.024 Uiso calc 1
C C8 1.15600(16) 0.18780(4) 1.01999(12) 0.0197(3) Uani d 1
H H8A 1.0612 0.1899 1.0480 0.024 Uiso calc 1
H H8B 1.2196 0.2021 1.0781 0.024 Uiso calc 1
N N4 1.15908(12) 0.20672(4) 0.90229(10) 0.0188(3) Uani d 1
C C9 1.28789(15) 0.22640(5) 0.87719(14) 0.0235(3) Uani d 1
H H9A 1.2705 0.2449 0.8104 0.035 Uiso calc 1
H H9B 1.3562 0.2067 0.8556 0.035 Uiso calc 1
H H9C 1.3237 0.2409 0.9487 0.035 Uiso calc 1
C C10 1.03676(15) 0.21111(4) 0.83296(12) 0.0165(3) Uani d 1
O O1 0.92302(10) 0.20626(3) 0.87473(8) 0.0210(2) Uani d 1
N N5 1.04850(13) 0.22196(4) 0.71448(10) 0.0191(3) Uani d 1
C C11 0.91878(16) 0.23147(5) 0.64557(12) 0.0234(3) Uani d 1
H H11A 0.8722 0.2070 0.6190 0.035 Uiso calc 1
H H11B 0.9388 0.2474 0.5754 0.035 Uiso calc 1
H H11C 0.8584 0.2464 0.6962 0.035 Uiso calc 1
C C12 1.14626(19) 0.20145(5) 0.64173(14) 0.0308(4) Uani d 1
H H12A 1.2216 0.1903 0.6943 0.046 Uiso calc 1
H H12B 1.1846 0.2201 0.5856 0.046 Uiso calc 1
H H12C 1.0981 0.1802 0.5965 0.046 Uiso calc 1
C C13 0.94899(15) 0.10156(4) 1.11681(11) 0.0172(3) Uani d 1
H H13A 0.8953 0.1203 1.1637 0.021 Uiso calc 1
H H13B 1.0434 0.0996 1.1566 0.021 Uiso calc 1
C C14 0.88068(15) 0.06163(4) 1.11757(12) 0.0174(3) Uani d 1
O O2 0.83182(13) 0.04434(4) 1.03091(9) 0.0350(3) Uani d 1
O O3 0.87943(11) 0.04887(3) 1.23022(8) 0.0219(2) Uani d 1
C C15 0.81131(17) 0.01131(5) 1.25050(13) 0.0265(4) Uani d 1
H H15A 0.8522 -0.0098 1.2028 0.032 Uiso calc 1
H H15B 0.7111 0.0131 1.2266 0.032 Uiso calc 1
C C16 0.8328(2) 0.00251(5) 1.38170(14) 0.0387(5) Uani d 1
H H16A 0.9322 -0.0004 1.4034 0.058 Uiso calc 1
H H16B 0.7847 -0.0220 1.3998 0.058 Uiso calc 1
H H16C 0.7957 0.0242 1.4279 0.058 Uiso calc 1
B B1 0.34042(17) 0.11535(5) 0.39939(13) 0.0143(3) Uani d 1
C C17 0.43843(14) 0.15505(4) 0.39351(11) 0.0157(3) Uani d 1
C C18 0.49782(15) 0.17349(4) 0.49770(12) 0.0186(3) Uani d 1
H H18A 0.4844 0.1618 0.5734 0.022 Uiso calc 1
C C19 0.57527(15) 0.20806(5) 0.49502(14) 0.0223(3) Uani d 1
H H19A 0.6132 0.2193 0.5680 0.027 Uiso calc 1
C C20 0.59757(16) 0.22626(5) 0.38682(14) 0.0243(3) Uani d 1
H H20A 0.6523 0.2495 0.3845 0.029 Uiso calc 1
C C21 0.53821(16) 0.20976(5) 0.28209(13) 0.0228(3) Uani d 1
H H21A 0.5500 0.2222 0.2071 0.027 Uiso calc 1
C C22 0.46146(15) 0.17509(4) 0.28616(12) 0.0186(3) Uani d 1
H H22A 0.4226 0.1644 0.2127 0.022 Uiso calc 1
C C23 0.35548(15) 0.08579(4) 0.28264(11) 0.0151(3) Uani d 1
C C24 0.47268(15) 0.08387(4) 0.21527(12) 0.0195(3) Uani d 1
H H24A 0.5494 0.1005 0.2370 0.023 Uiso calc 1
C C25 0.48122(17) 0.05850(5) 0.11770(12) 0.0224(3) Uani d 1
H H25A 0.5626 0.0583 0.0744 0.027 Uiso calc 1
C C26 0.37252(17) 0.03359(5) 0.08325(12) 0.0224(3) Uani d 1
H H26A 0.3771 0.0170 0.0150 0.027 Uiso calc 1
C C27 0.25708(16) 0.03331(5) 0.15005(12) 0.0218(3) Uani d 1
H H27A 0.1825 0.0158 0.1293 0.026 Uiso calc 1
C C28 0.25009(15) 0.05867(4) 0.24773(12) 0.0178(3) Uani d 1
H H28A 0.1703 0.0576 0.2930 0.021 Uiso calc 1
C C29 0.17692(14) 0.12955(4) 0.39947(11) 0.0139(3) Uani d 1
C C30 0.12827(14) 0.16549(4) 0.34958(11) 0.0156(3) Uani d 1
H H30A 0.1930 0.1828 0.3163 0.019 Uiso calc 1
C C31 -0.00979(15) 0.17687(4) 0.34667(11) 0.0188(3) Uani d 1
H H31A -0.0370 0.2017 0.3130 0.023 Uiso calc 1
C C32 -0.10837(15) 0.15240(5) 0.39235(11) 0.0192(3) Uani d 1
H H32A -0.2029 0.1602 0.3906 0.023 Uiso calc 1
C C33 -0.06588(15) 0.11628(4) 0.44077(11) 0.0180(3) Uani d 1
H H33A -0.1319 0.0988 0.4712 0.022 Uiso calc 1
C C34 0.07363(15) 0.10570(4) 0.44472(11) 0.0161(3) Uani d 1
H H34A 0.1002 0.0811 0.4798 0.019 Uiso calc 1
C C35 0.38760(14) 0.09029(4) 0.52189(11) 0.0154(3) Uani d 1
C C36 0.33605(15) 0.09853(4) 0.63423(12) 0.0176(3) Uani d 1
H H36A 0.2684 0.1187 0.6392 0.021 Uiso calc 1
C C37 0.38038(15) 0.07824(5) 0.73862(12) 0.0199(3) Uani d 1
H H37A 0.3422 0.0846 0.8125 0.024 Uiso calc 1
C C38 0.47946(16) 0.04899(4) 0.73512(12) 0.0204(3) Uani d 1
H H38A 0.5105 0.0353 0.8063 0.025 Uiso calc 1
C C39 0.53299(15) 0.03985(4) 0.62634(12) 0.0208(3) Uani d 1
H H39A 0.6010 0.0197 0.6224 0.025 Uiso calc 1
C C40 0.48709(15) 0.06020(4) 0.52267(12) 0.0185(3) Uani d 1
H H40A 0.5251 0.0533 0.4490 0.022 Uiso calc 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0152(7) 0.0160(7) 0.0112(6) -0.0023(5) 0.0011(5) 0.0007(5)
N1 0.0116(6) 0.0249(7) 0.0130(6) -0.0006(5) 0.0010(5) -0.0007(5)
N2 0.0192(7) 0.0210(7) 0.0110(6) -0.0005(5) 0.0000(5) -0.0001(5)
N3 0.0124(6) 0.0192(6) 0.0111(6) -0.0008(5) 0.0020(4) 0.0011(4)
C2 0.0204(8) 0.0243(8) 0.0171(7) 0.0017(6) 0.0058(6) -0.0038(6)
C3 0.0131(8) 0.0386(10) 0.0260(8) -0.0003(7) 0.0003(6) 0.0040(7)
C4 0.0281(9) 0.0243(8) 0.0150(7) 0.0015(7) 0.0009(6) -0.0047(6)
C5 0.0285(9) 0.0260(8) 0.0127(7) 0.0000(7) -0.0032(6) 0.0018(6)
C6 0.0125(7) 0.0210(8) 0.0198(7) 0.0020(6) 0.0040(6) 0.0015(6)
C7 0.0134(8) 0.0265(8) 0.0209(7) -0.0005(6) -0.0006(6) 0.0057(6)
C8 0.0190(8) 0.0260(8) 0.0134(7) -0.0039(6) -0.0040(6) 0.0007(6)
N4 0.0162(7) 0.0230(7) 0.0173(6) -0.0040(5) 0.0010(5) 0.0039(5)
C9 0.0178(8) 0.0252(8) 0.0277(8) -0.0043(6) 0.0032(6) 0.0016(6)
C10 0.0219(8) 0.0147(7) 0.0131(7) -0.0011(6) 0.0012(6) -0.0008(5)
O1 0.0163(6) 0.0304(6) 0.0163(5) -0.0042(4) 0.0017(4) 0.0025(4)
N5 0.0219(7) 0.0228(7) 0.0129(6) 0.0011(5) 0.0030(5) 0.0006(5)
C11 0.0311(9) 0.0231(8) 0.0155(7) -0.0018(7) -0.0031(6) 0.0019(6)
C12 0.0411(11) 0.0304(9) 0.0223(8) 0.0055(8) 0.0122(7) -0.0011(7)
C13 0.0179(8) 0.0211(8) 0.0123(7) -0.0019(6) -0.0019(5) 0.0019(6)
C14 0.0151(7) 0.0224(8) 0.0148(7) 0.0004(6) 0.0011(5) 0.0002(6)
O2 0.0549(8) 0.0339(7) 0.0159(6) -0.0208(6) 0.0000(5) -0.0034(5)
O3 0.0272(6) 0.0231(6) 0.0151(5) -0.0091(5) -0.0020(4) 0.0049(4)
C15 0.0315(10) 0.0240(8) 0.0233(8) -0.0118(7) -0.0035(7) 0.0055(7)
C16 0.0487(12) 0.0364(11) 0.0288(9) -0.0199(9) -0.0134(8) 0.0144(8)
B1 0.0144(8) 0.0170(8) 0.0113(7) 0.0017(6) -0.0002(6) -0.0007(6)
C17 0.0120(7) 0.0178(7) 0.0173(7) 0.0045(6) 0.0008(5) -0.0002(6)
C18 0.0147(8) 0.0220(8) 0.0189(7) 0.0032(6) -0.0008(6) -0.0006(6)
C19 0.0155(8) 0.0230(8) 0.0281(8) 0.0027(6) -0.0016(6) -0.0080(6)
C20 0.0160(8) 0.0179(8) 0.0398(9) -0.0005(6) 0.0071(7) -0.0037(7)
C21 0.0223(9) 0.0221(8) 0.0253(8) 0.0028(6) 0.0114(6) 0.0017(6)
C22 0.0169(8) 0.0221(8) 0.0168(7) 0.0022(6) 0.0024(6) -0.0011(6)
C23 0.0178(8) 0.0166(7) 0.0106(6) 0.0044(6) -0.0012(5) 0.0026(5)
C24 0.0193(8) 0.0216(8) 0.0179(7) 0.0008(6) 0.0028(6) 0.0015(6)
C25 0.0271(9) 0.0234(8) 0.0173(7) 0.0079(7) 0.0072(6) 0.0015(6)
C26 0.0330(9) 0.0219(8) 0.0118(7) 0.0108(7) -0.0018(6) -0.0025(6)
C27 0.0246(9) 0.0209(8) 0.0191(7) 0.0021(6) -0.0055(6) -0.0028(6)
C28 0.0182(8) 0.0208(8) 0.0143(7) 0.0039(6) 0.0000(6) 0.0001(6)
C29 0.0167(7) 0.0182(7) 0.0065(6) 0.0012(6) -0.0001(5) -0.0043(5)
C30 0.0177(8) 0.0203(7) 0.0085(6) -0.0002(6) -0.0005(5) -0.0001(5)
C31 0.0220(8) 0.0221(8) 0.0117(7) 0.0058(6) -0.0030(6) -0.0011(6)
C32 0.0165(8) 0.0281(8) 0.0125(7) 0.0056(6) -0.0011(6) -0.0056(6)
C33 0.0180(8) 0.0260(8) 0.0103(6) -0.0019(6) 0.0027(5) -0.0021(6)
C34 0.0189(8) 0.0191(7) 0.0103(6) 0.0019(6) 0.0003(5) -0.0002(5)
C35 0.0154(7) 0.0171(7) 0.0133(7) -0.0023(6) -0.0023(5) -0.0008(5)
C36 0.0170(8) 0.0196(8) 0.0158(7) 0.0005(6) -0.0019(6) -0.0008(6)
C37 0.0207(8) 0.0272(8) 0.0116(7) -0.0045(6) -0.0001(6) -0.0002(6)
C38 0.0222(8) 0.0226(8) 0.0157(7) -0.0031(6) -0.0052(6) 0.0048(6)
C39 0.0207(8) 0.0182(8) 0.0225(8) 0.0021(6) -0.0050(6) 0.0005(6)
C40 0.0196(8) 0.0207(8) 0.0150(7) 0.0018(6) -0.0004(6) -0.0014(6)
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'
B B 0.0013 0.0007 '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'
H H 0.0000 0.0000 '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
N2 C1 N1 120.32(12)
N2 C1 N3 120.64(12)
N1 C1 N3 119.04(11)
C1 N1 C2 123.21(12)
C1 N1 C3 121.94(12)
C2 N1 C3 114.78(12)
C1 N2 C5 122.62(12)
C1 N2 C4 122.24(12)
C5 N2 C4 115.11(11)
C1 N3 C13 119.79(11)
C1 N3 C6 121.67(11)
C13 N3 C6 117.64(11)
N1 C2 H2A 109.5
N1 C2 H2B 109.5
H2A C2 H2B 109.5
N1 C2 H2C 109.5
H2A C2 H2C 109.5
H2B C2 H2C 109.5
N1 C3 H3A 109.5
N1 C3 H3B 109.5
H3A C3 H3B 109.5
N1 C3 H3C 109.5
H3A C3 H3C 109.5
H3B C3 H3C 109.5
N2 C4 H4A 109.5
N2 C4 H4B 109.5
H4A C4 H4B 109.5
N2 C4 H4C 109.5
H4A C4 H4C 109.5
H4B C4 H4C 109.5
N2 C5 H5A 109.5
N2 C5 H5B 109.5
H5A C5 H5B 109.5
N2 C5 H5C 109.5
H5A C5 H5C 109.5
H5B C5 H5C 109.5
N3 C6 C7 112.52(11)
N3 C6 H6A 109.1
C7 C6 H6A 109.1
N3 C6 H6B 109.1
C7 C6 H6B 109.1
H6A C6 H6B 107.8
C6 C7 C8 114.54(12)
C6 C7 H7A 108.6
C8 C7 H7A 108.6
C6 C7 H7B 108.6
C8 C7 H7B 108.6
H7A C7 H7B 107.6
N4 C8 C7 113.07(12)
N4 C8 H8A 109.0
C7 C8 H8A 109.0
N4 C8 H8B 109.0
C7 C8 H8B 109.0
H8A C8 H8B 107.8
C10 N4 C9 123.77(12)
C10 N4 C8 118.94(12)
C9 N4 C8 116.18(11)
N4 C9 H9A 109.5
N4 C9 H9B 109.5
H9A C9 H9B 109.5
N4 C9 H9C 109.5
H9A C9 H9C 109.5
H9B C9 H9C 109.5
O1 C10 N4 121.81(12)
O1 C10 N5 121.83(13)
N4 C10 N5 116.34(13)
C10 N5 C12 120.06(12)
C10 N5 C11 116.06(12)
C12 N5 C11 112.09(12)
N5 C11 H11A 109.5
N5 C11 H11B 109.5
H11A C11 H11B 109.5
N5 C11 H11C 109.5
H11A C11 H11C 109.5
H11B C11 H11C 109.5
N5 C12 H12A 109.5
N5 C12 H12B 109.5
H12A C12 H12B 109.5
N5 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
N3 C13 C14 112.41(11)
N3 C13 H13A 109.1
C14 C13 H13A 109.1
N3 C13 H13B 109.1
C14 C13 H13B 109.1
H13A C13 H13B 107.9
O2 C14 O3 125.09(14)
O2 C14 C13 125.70(13)
O3 C14 C13 109.19(11)
C14 O3 C15 117.58(11)
O3 C15 C16 106.90(12)
O3 C15 H15A 110.3
C16 C15 H15A 110.3
O3 C15 H15B 110.3
C16 C15 H15B 110.3
H15A C15 H15B 108.6
C15 C16 H16A 109.5
C15 C16 H16B 109.5
H16A C16 H16B 109.5
C15 C16 H16C 109.5
H16A C16 H16C 109.5
H16B C16 H16C 109.5
C35 B1 C17 108.95(11)
C35 B1 C29 111.24(11)
C17 B1 C29 108.33(11)
C35 B1 C23 107.87(11)
C17 B1 C23 112.42(11)
C29 B1 C23 108.05(11)
C22 C17 C18 114.18(13)
C22 C17 B1 123.43(12)
C18 C17 B1 122.23(12)
C19 C18 C17 123.13(13)
C19 C18 H18A 118.4
C17 C18 H18A 118.4
C20 C19 C18 120.55(13)
C20 C19 H19A 119.7
C18 C19 H19A 119.7
C19 C20 C21 118.42(14)
C19 C20 H20A 120.8
C21 C20 H20A 120.8
C20 C21 C22 120.35(14)
C20 C21 H21A 119.8
C22 C21 H21A 119.8
C21 C22 C17 123.34(13)
C21 C22 H22A 118.3
C17 C22 H22A 118.3
C24 C23 C28 114.65(12)
C24 C23 B1 124.43(12)
C28 C23 B1 120.84(12)
C25 C24 C23 122.61(14)
C25 C24 H24A 118.7
C23 C24 H24A 118.7
C26 C25 C24 120.71(14)
C26 C25 H25A 119.6
C24 C25 H25A 119.6
C27 C26 C25 118.69(13)
C27 C26 H26A 120.7
C25 C26 H26A 120.7
C26 C27 C28 120.00(14)
C26 C27 H27A 120.0
C28 C27 H27A 120.0
C27 C28 C23 123.21(14)
C27 C28 H28A 118.4
C23 C28 H28A 118.4
C34 C29 C30 114.41(13)
C34 C29 B1 122.37(12)
C30 C29 B1 123.15(12)
C31 C30 C29 123.08(13)
C31 C30 H30A 118.5
C29 C30 H30A 118.5
C32 C31 C30 120.59(14)
C32 C31 H31A 119.7
C30 C31 H31A 119.7
C31 C32 C33 118.52(14)
C31 C32 H32A 120.7
C33 C32 H32A 120.7
C32 C33 C34 119.99(14)
C32 C33 H33A 120.0
C34 C33 H33A 120.0
C33 C34 C29 123.39(13)
C33 C34 H34A 118.3
C29 C34 H34A 118.3
C40 C35 C36 114.96(12)
C40 C35 B1 122.18(12)
C36 C35 B1 122.81(12)
C37 C36 C35 122.58(13)
C37 C36 H36A 118.7
C35 C36 H36A 118.7
C38 C37 C36 120.38(13)
C38 C37 H37A 119.8
C36 C37 H37A 119.8
C37 C38 C39 119.02(13)
C37 C38 H38A 120.5
C39 C38 H38A 120.5
C38 C39 C40 119.96(14)
C38 C39 H39A 120.0
C40 C39 H39A 120.0
C39 C40 C35 123.10(13)
C39 C40 H40A 118.5
C35 C40 H40A 118.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N2 1.3368(16)
C1 N1 1.3375(18)
C1 N3 1.3594(17)
N1 C2 1.4583(17)
N1 C3 1.4599(18)
N2 C5 1.4608(18)
N2 C4 1.4639(18)
N3 C13 1.4568(16)
N3 C6 1.4737(17)
C2 H2A 0.9800
C2 H2B 0.9800
C2 H2C 0.9800
C3 H3A 0.9800
C3 H3B 0.9800
C3 H3C 0.9800
C4 H4A 0.9800
C4 H4B 0.9800
C4 H4C 0.9800
C5 H5A 0.9800
C5 H5B 0.9800
C5 H5C 0.9800
C6 C7 1.520(2)
C6 H6A 0.9900
C6 H6B 0.9900
C7 C8 1.527(2)
C7 H7A 0.9900
C7 H7B 0.9900
C8 N4 1.4630(17)
C8 H8A 0.9900
C8 H8B 0.9900
N4 C10 1.3777(18)
N4 C9 1.4554(18)
C9 H9A 0.9800
C9 H9B 0.9800
C9 H9C 0.9800
C10 O1 1.2328(17)
C10 N5 1.3835(17)
N5 C12 1.4610(19)
N5 C11 1.4630(18)
C11 H11A 0.9800
C11 H11B 0.9800
C11 H11C 0.9800
C12 H12A 0.9800
C12 H12B 0.9800
C12 H12C 0.9800
C13 C14 1.505(2)
C13 H13A 0.9900
C13 H13B 0.9900
C14 O2 1.2004(16)
C14 O3 1.3296(16)
O3 C15 1.4570(17)
C15 C16 1.495(2)
C15 H15A 0.9900
C15 H15B 0.9900
C16 H16A 0.9800
C16 H16B 0.9800
C16 H16C 0.9800
B1 C35 1.647(2)
B1 C17 1.649(2)
B1 C29 1.652(2)
B1 C23 1.657(2)
C17 C22 1.4069(19)
C17 C18 1.4081(19)
C18 C19 1.391(2)
C18 H18A 0.9500
C19 C20 1.385(2)
C19 H19A 0.9500
C20 C21 1.385(2)
C20 H20A 0.9500
C21 C22 1.391(2)
C21 H21A 0.9500
C22 H22A 0.9500
C23 C24 1.401(2)
C23 C28 1.408(2)
C24 C25 1.393(2)
C24 H24A 0.9500
C25 C26 1.382(2)
C25 H25A 0.9500
C26 C27 1.382(2)
C26 H26A 0.9500
C27 C28 1.3925(19)
C27 H27A 0.9500
C28 H28A 0.9500
C29 C34 1.404(2)
C29 C30 1.4066(19)
C30 C31 1.387(2)
C30 H30A 0.9500
C31 C32 1.385(2)
C31 H31A 0.9500
C32 C33 1.389(2)
C32 H32A 0.9500
C33 C34 1.393(2)
C33 H33A 0.9500
C34 H34A 0.9500
C35 C40 1.401(2)
C35 C36 1.4064(19)
C36 C37 1.3952(19)
C36 H36A 0.9500
C37 C38 1.380(2)
C37 H37A 0.9500
C38 C39 1.385(2)
C38 H38A 0.9500
C39 C40 1.3936(19)
C39 H39A 0.9500
C40 H40A 0.9500
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
C11 H11B O1 4_554 0.98 2.73 3.687(2) 165 y
C25 H25A O2 1_554 0.95 2.72 3.617(2) 158 y
C27 H27A O2 3_656 0.95 2.71 3.392(2) 129 y
C12 H12C Cg1 1 0.98 2.64 3.541(2) 152 y
C13 H13A Cg1 1 0.99 2.91 3.432(2) 114 y
C5 H5A Cg2 1 0.98 2.89 3.868(2) 174 y
C16 H16B Cg2 1 0.98 2.66 3.542(2) 151 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
N2 C1 N1 C2 -146.94(13)
N3 C1 N1 C2 33.4(2)
N2 C1 N1 C3 29.8(2)
N3 C1 N1 C3 -149.78(13)
N1 C1 N2 C5 33.0(2)
N3 C1 N2 C5 -147.38(14)
N1 C1 N2 C4 -144.91(14)
N3 C1 N2 C4 34.7(2)
N2 C1 N3 C13 -136.39(13)
N1 C1 N3 C13 43.24(19)
N2 C1 N3 C6 32.45(19)
N1 C1 N3 C6 -147.92(13)
C1 N3 C6 C7 128.32(14)
C13 N3 C6 C7 -62.61(16)
N3 C6 C7 C8 -62.20(16)
C6 C7 C8 N4 -67.10(16)
C7 C8 N4 C10 99.05(15)
C7 C8 N4 C9 -92.53(15)
C9 N4 C10 O1 -154.18(14)
C8 N4 C10 O1 13.3(2)
C9 N4 C10 N5 24.7(2)
C8 N4 C10 N5 -167.82(13)
O1 C10 N5 C12 -133.66(16)
N4 C10 N5 C12 47.47(19)
O1 C10 N5 C11 6.4(2)
N4 C10 N5 C11 -172.48(12)
C1 N3 C13 C14 61.55(17)
C6 N3 C13 C14 -107.74(14)
N3 C13 C14 O2 -3.7(2)
N3 C13 C14 O3 178.03(12)
O2 C14 O3 C15 -1.2(2)
C13 C14 O3 C15 177.14(12)
C14 O3 C15 C16 176.18(14)
C35 B1 C17 C22 156.72(13)
C29 B1 C17 C22 -82.12(15)
C23 B1 C17 C22 37.21(18)
C35 B1 C17 C18 -28.25(17)
C29 B1 C17 C18 92.91(15)
C23 B1 C17 C18 -147.76(13)
C22 C17 C18 C19 -1.4(2)
B1 C17 C18 C19 -176.82(13)
C17 C18 C19 C20 0.1(2)
C18 C19 C20 C21 1.5(2)
C19 C20 C21 C22 -1.8(2)
C20 C21 C22 C17 0.4(2)
C18 C17 C22 C21 1.1(2)
B1 C17 C22 C21 176.50(13)
C35 B1 C23 C24 -94.23(15)
C17 B1 C23 C24 25.92(18)
C29 B1 C23 C24 145.41(13)
C35 B1 C23 C28 82.39(15)
C17 B1 C23 C28 -157.47(12)
C29 B1 C23 C28 -37.98(16)
C28 C23 C24 C25 3.1(2)
B1 C23 C24 C25 179.88(13)
C23 C24 C25 C26 -0.4(2)
C24 C25 C26 C27 -2.3(2)
C25 C26 C27 C28 1.9(2)
C26 C27 C28 C23 1.0(2)
C24 C23 C28 C27 -3.4(2)
B1 C23 C28 C27 179.65(12)
C35 B1 C29 C34 -37.55(17)
C17 B1 C29 C34 -157.27(12)
C23 B1 C29 C34 80.68(15)
C35 B1 C29 C30 145.51(12)
C17 B1 C29 C30 25.78(16)
C23 B1 C29 C30 -96.26(14)
C34 C29 C30 C31 0.94(18)
B1 C29 C30 C31 178.11(12)
C29 C30 C31 C32 -1.0(2)
C30 C31 C32 C33 -0.12(19)
C31 C32 C33 C34 1.23(19)
C32 C33 C34 C29 -1.3(2)
C30 C29 C34 C33 0.22(18)
B1 C29 C34 C33 -176.97(12)
C17 B1 C35 C40 -91.78(15)
C29 B1 C35 C40 148.86(13)
C23 B1 C35 C40 30.52(18)
C17 B1 C35 C36 85.35(16)
C29 B1 C35 C36 -34.01(18)
C23 B1 C35 C36 -152.35(13)
C40 C35 C36 C37 -0.1(2)
B1 C35 C36 C37 -177.43(13)
C35 C36 C37 C38 0.6(2)
C36 C37 C38 C39 -0.7(2)
C37 C38 C39 C40 0.3(2)
C38 C39 C40 C35 0.2(2)
C36 C35 C40 C39 -0.3(2)
B1 C35 C40 C39 177.04(13)
_cod_database_fobs_code 2241389