#------------------------------------------------------------------------------
#$Date: 2019-10-05 07:00:24 +0300 (Sat, 05 Oct 2019) $
#$Revision: 219113 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/17/2021790.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_2021790
loop_
_publ_author_name
'Wang, Ai'
'Englert, Ulli'
_publ_section_title
;
Absolute structure of the chiral pyrrolidine derivative (2S)-methyl
(Z)-5-(2-tert-butoxy-1-cyano-2-oxoethylidene)pyrrolidine-2-carboxylate, a
compound with low resonant scattering
;
_journal_coeditor_code YF3192
_journal_issue 11
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi 10.1107/S2053229619012324
_journal_volume 75
_journal_year 2019
_chemical_absolute_configuration unk
_chemical_formula_iupac 'C13 H18 N2 O4'
_chemical_formula_moiety 'C13 H18 N2 O4'
_chemical_formula_sum 'C13 H18 N2 O4'
_chemical_formula_weight 266.29
_chemical_name_common 1mo
_chemical_name_systematic
;(2S)-Methyl
(Z)-5-(2-tert-butoxy-1-cyano-2-oxoethylidene)pyrrolidine-2-carboxylate
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_Hall 'P 2ac 2ab'
_space_group_name_H-M_alt 'P 21 21 21'
_symmetry_space_group_name_Hall 'P 2ac 2ab'
_symmetry_space_group_name_H-M 'P 21 21 21'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_audit_creation_method SHELXL-2014/7
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.347(4)
_cell_length_b 10.197(6)
_cell_length_c 18.477(10)
_cell_measurement_reflns_used 1389
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 20.42
_cell_measurement_theta_min 2.28
_cell_volume 1384.2(13)
_computing_cell_refinement
;
SMART (Bruker, 2001)
;
_computing_data_collection
;
SMART (Bruker, 2001)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2009)
;
_computing_publication_material
;
SHELXL2017 (Sheldrick, 2015) and
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'D8 goniometer with APEX CCD area detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator 'multilayer optics'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0909
_diffrn_reflns_av_unetI/netI 0.0819
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 10626
_diffrn_reflns_theta_full 24.479
_diffrn_reflns_theta_max 24.479
_diffrn_reflns_theta_min 2.205
_diffrn_source 'Incoatec microsource'
_exptl_absorpt_coefficient_mu 0.095
_exptl_absorpt_correction_T_max 0.7451
_exptl_absorpt_correction_T_min 0.4725
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.278
_exptl_crystal_description block
_exptl_crystal_F_000 568
_exptl_crystal_size_max 0.350
_exptl_crystal_size_mid 0.290
_exptl_crystal_size_min 0.280
_refine_diff_density_max 0.207
_refine_diff_density_min -0.182
_refine_ls_abs_structure_details
;
Flack x determined using 710 quotients [(I+)-(I)-]/[(I+)+(I)-]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 1.1(10)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.077
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 180
_refine_ls_number_reflns 2290
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.077
_refine_ls_R_factor_all 0.0584
_refine_ls_R_factor_gt 0.0512
_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^)+(0.0228P)^2^+0.6063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1197
_refine_ls_wR_factor_ref 0.1236
_reflns_number_gt 2051
_reflns_number_total 2290
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file yf3192sup1.cif
_cod_data_source_block 1mo
_cod_original_cell_volume 1384.1(13)
_cod_database_code 2021790
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min 0.967
_shelx_estimated_absorpt_t_max 0.974
_shelx_hkl_file
;
1 0 0 -0.80 2.10
1 0 0 -1.10 2.30
1 0 0 0.90 2.10
2 0 0 1296.97 187.48
2 0 0 1361.66 177.98
3 0 0 20.40 8.50
3 0 0 -1.90 5.70
3 0 0 6.20 6.30
4 0 0 67.39 15.50
4 0 0 75.59 13.60
4 0 0 57.09 13.80
5 0 0 -8.60 10.70
5 0 0 10.60 8.80
5 0 0 10.40 9.10
6 0 0 47.80 17.70
6 0 0 88.09 17.70
7 0 0 13.50 15.60
-7 0 0 18.60 8.30
-7 0 0 4.20 6.80
-8 0 0 19.30 10.70
8 0 0 13.90 20.50
0 -1 0 -1.90 0.50
0 -1 0 -0.90 1.40
0 -1 0 -3.30 1.00
0 1 0 -2.60 0.90
0 1 0 -2.90 0.60
0 1 0 -1.10 1.80
-1 1 0 3328.57 466.95
1 -1 0 3273.47 478.65
-1 -1 0 3356.26 442.76
-1 -1 0 3423.56 467.15
1 1 0 3319.57 467.05
1 -1 0 3529.25 443.46
1 1 0 3048.40 478.95
2 -1 0 578.04 76.19
2 1 0 492.65 77.89
2 1 0 543.35 75.59
2 -1 0 500.25 72.19
-2 -1 0 542.05 71.09
2 -1 0 515.95 77.39
3 1 0 154.18 26.50
-3 -1 0 164.68 21.80
3 -1 0 180.98 24.90
3 -1 0 189.38 25.60
3 -1 0 112.29 24.70
3 1 0 147.59 24.30
-4 -1 0 53.19 8.40
4 1 0 27.80 12.90
4 1 0 62.99 12.20
4 -1 0 81.89 13.70
4 -1 0 31.60 11.40
4 -1 0 45.00 12.10
5 -1 0 152.98 27.80
5 1 0 200.58 27.30
-5 -1 0 136.89 22.00
5 -1 0 197.48 27.40
5 1 0 121.69 28.20
6 -1 0 44.20 14.30
6 -1 0 38.30 15.50
-6 1 0 45.90 9.70
-6 -1 0 46.40 9.80
6 1 0 41.50 17.00
6 1 0 82.79 16.60
-7 -1 0 58.39 11.70
7 1 0 82.39 18.30
7 1 0 34.60 19.50
7 -1 0 20.90 18.30
7 -1 0 45.60 17.50
-7 1 0 51.49 11.20
-8 1 0 25.20 11.20
8 -1 0 37.60 22.40
-8 -1 0 33.60 11.70
-8 1 0 41.80 12.40
0 -2 0 1607.74 223.78
0 2 0 1524.15 218.58
0 -2 0 1510.95 207.48
1 2 0 6732.23 941.41
-1 -2 0 6652.03 964.50
-1 -2 0 7007.80 892.51
-1 2 0 6731.83 941.21
1 -2 0 6050.09 893.21
1 -2 0 6954.70 964.60
-2 -2 0 113.59 16.30
-2 -2 0 103.69 14.60
-2 2 0 103.59 15.80
2 2 0 89.29 16.30
2 -2 0 124.89 17.80
2 -2 0 106.09 16.90
3 2 0 241.28 31.90
-3 2 0 202.98 30.10
3 -2 0 234.08 32.00
-3 -2 0 204.18 28.20
3 2 0 186.28 34.30
3 -2 0 188.58 32.20
4 -2 0 128.69 27.10
-4 -2 0 172.18 23.30
4 2 0 173.98 26.60
-4 2 0 168.08 24.90
4 -2 0 199.18 28.30
4 2 0 147.49 29.60
-5 -2 0 50.69 9.30
5 2 0 39.50 12.60
5 2 0 48.50 16.50
-5 2 0 63.19 10.30
5 -2 0 57.29 15.60
5 -2 0 62.99 15.00
-6 -2 0 163.68 22.00
6 2 0 131.09 26.60
6 -2 0 140.39 27.20
6 2 0 148.09 31.10
6 -2 0 142.89 27.00
-6 2 0 139.39 23.20
-7 2 0 45.20 9.70
7 -2 0 8.70 18.10
7 -2 0 19.30 13.20
-7 -2 0 25.70 8.70
8 -2 0 -7.80 21.60
8 -2 0 20.50 22.00
-8 2 0 14.20 9.40
-8 -2 0 19.40 9.20
-8 -2 0 15.00 11.40
0 -3 0 -0.20 3.10
0 3 0 1.20 2.20
0 -3 0 0.00 1.20
-1 -3 0 563.74 71.29
1 -3 0 538.75 76.99
1 3 0 507.05 75.49
1 -3 0 510.95 72.29
-1 3 0 498.95 75.29
-1 -3 0 545.15 76.89
-2 -3 0 3.00 1.90
2 -3 0 6.30 4.80
2 -3 0 16.50 6.70
2 3 0 6.30 4.70
-2 3 0 8.10 3.10
-2 -3 0 4.80 2.40
-3 -3 0 573.84 80.69
3 -3 0 515.75 83.79
-3 -3 0 576.04 87.49
3 3 0 746.63 86.49
-3 3 0 621.64 85.59
4 -3 0 92.59 15.80
-4 3 0 71.69 12.80
4 3 0 97.09 15.90
-4 -3 0 81.69 13.20
-4 -3 0 66.89 11.50
4 -3 0 79.49 16.70
-5 3 0 15.90 5.90
5 -3 0 -0.50 9.00
5 -3 0 14.20 11.10
5 3 0 4.50 9.60
-5 -3 0 19.10 5.00
-5 -3 0 20.20 5.60
-6 -3 0 307.07 49.00
6 3 0 361.76 51.19
-6 3 0 305.77 47.70
6 -3 0 341.17 50.89
-6 -3 0 322.57 44.20
7 -3 0 84.49 23.80
-7 3 0 96.49 17.50
7 -3 0 94.19 24.10
-7 -3 0 86.29 16.90
-7 -3 0 98.59 16.30
-8 3 0 19.70 9.70
8 -3 0 2.60 29.50
-8 -3 0 16.30 8.40
8 -3 0 -20.80 16.50
0 -4 0 1047.40 149.09
0 4 0 1108.09 156.78
0 -4 0 1144.69 160.18
1 4 0 20.00 5.80
-1 -4 0 26.90 4.50
-1 -4 0 24.70 5.10
1 -4 0 23.70 5.10
1 -4 0 31.20 8.00
-1 4 0 14.80 4.80
2 4 0 48.20 10.70
-2 -4 0 43.00 8.80
2 -4 0 86.99 11.20
-2 4 0 72.19 9.70
2 -4 0 50.59 11.70
-2 -4 0 46.80 8.20
-3 -4 0 17.30 4.70
-3 -4 0 15.40 4.00
3 4 0 13.00 7.40
-3 4 0 22.80 5.20
3 -4 0 41.10 8.60
3 -4 0 8.90 8.90
-4 4 0 301.37 39.90
-4 -4 0 260.67 36.30
-4 -4 0 276.07 40.50
4 -4 0 191.68 40.80
4 4 0 312.27 41.20
4 -4 0 308.87 42.00
5 -4 0 35.70 12.30
-5 -4 0 22.80 5.60
5 -4 0 29.20 13.10
-5 -4 0 19.50 6.40
-5 4 0 18.70 6.80
5 4 0 11.20 11.20
6 -4 0 401.76 63.99
-6 4 0 453.55 62.39
-6 -4 0 432.86 62.29
-6 -4 0 397.16 57.19
7 -4 0 168.28 34.80
-7 -4 0 212.58 30.70
-7 4 0 188.48 30.30
7 -4 0 128.79 36.50
-8 -4 0 54.39 12.60
8 -4 0 25.00 22.40
-8 4 0 37.90 13.20
0 -5 0 2.80 2.70
0 5 0 10.50 4.50
0 -5 0 16.30 6.50
-1 -5 0 12.00 6.40
-1 -5 0 24.50 5.10
1 -5 0 35.00 6.20
-1 5 0 26.10 6.00
1 -5 0 17.30 9.10
1 5 0 39.20 7.60
2 5 0 667.23 86.59
2 -5 0 546.45 87.89
-2 5 0 629.94 85.89
-2 -5 0 597.94 87.49
-2 -5 0 608.44 81.09
2 -5 0 572.24 84.39
3 -5 0 61.39 15.90
3 -5 0 32.30 15.80
-3 -5 0 111.19 14.70
-3 -5 0 122.09 13.50
-3 5 0 66.59 14.20
4 5 0 42.70 11.60
-4 -5 0 32.20 6.10
4 -5 0 28.70 11.30
-4 -5 0 29.00 5.60
4 -5 0 26.90 10.30
-4 5 0 7.20 5.80
-5 -5 0 17.20 5.50
-5 5 0 16.60 6.90
5 -5 0 33.70 13.20
-5 -5 0 8.50 5.10
5 5 0 7.80 15.80
5 -5 0 7.30 12.80
-6 5 0 451.95 65.39
-6 -5 0 432.06 65.39
6 -5 0 451.05 67.89
-7 5 0 57.59 14.50
-7 -5 0 70.19 14.00
7 -5 0 81.69 24.70
0 -6 0 56.79 10.00
0 -6 0 19.80 5.00
0 6 0 36.10 7.30
1 -6 0 335.87 51.99
-1 -6 0 399.66 50.39
-1 -6 0 366.06 51.69
1 6 0 353.86 52.59
1 -6 0 337.87 51.59
-1 6 0 343.47 51.39
2 -6 0 11.60 6.10
-2 -6 0 19.70 6.00
-2 -6 0 15.70 4.00
2 -6 0 15.20 9.50
-2 6 0 15.20 5.60
2 6 0 12.80 8.50
-3 -6 0 129.89 16.60
-3 -6 0 80.19 16.90
3 -6 0 164.78 20.30
-4 -6 0 16.30 5.40
-4 -6 0 18.50 5.80
4 6 0 25.40 12.50
-4 6 0 28.90 7.30
4 -6 0 25.80 11.00
4 -6 0 4.30 14.30
-5 -6 0 153.88 21.30
-5 -6 0 144.89 23.30
5 -6 0 121.89 28.10
5 -6 0 134.09 27.10
-5 6 0 130.79 23.30
-6 6 0 -7.80 7.40
6 -6 0 6.50 16.80
-6 -6 0 2.20 5.60
-7 6 0 0.00 9.30
-7 -6 0 8.90 7.00
7 -6 0 3.80 20.10
0 -7 0 4.80 3.20
0 7 0 4.90 5.80
0 -7 0 28.00 9.10
-1 7 0 84.59 15.40
1 -7 0 108.09 15.30
1 -7 0 40.60 15.90
-1 -7 0 91.79 14.00
1 7 0 79.49 16.10
-1 -7 0 88.39 16.20
2 7 0 408.86 61.99
2 -7 0 361.06 61.19
-2 -7 0 430.56 60.49
2 -7 0 382.86 60.79
-2 7 0 437.96 60.19
-2 -7 0 441.96 57.29
3 -7 0 207.28 33.20
-3 -7 0 207.88 31.30
3 -7 0 195.08 34.70
3 7 0 229.48 34.10
-3 7 0 160.78 31.20
-3 -7 0 244.98 30.40
-4 -7 0 26.30 8.70
4 -7 0 4.50 14.40
4 -7 0 13.10 12.90
-4 7 0 13.70 6.60
-4 -7 0 9.30 4.50
-5 7 0 26.60 9.70
5 -7 0 8.00 17.70
-5 -7 0 36.90 8.20
-6 7 0 14.10 9.40
6 -7 0 11.80 20.10
-6 -7 0 -3.80 4.90
0 8 0 493.35 61.99
0 -8 0 403.76 61.69
0 -8 0 371.86 60.89
-1 8 0 107.29 17.40
-1 -8 0 92.39 15.60
1 8 0 119.39 19.10
1 -8 0 87.29 16.70
-1 -8 0 85.19 18.80
1 -8 0 98.29 21.00
2 -8 0 70.09 15.30
-2 -8 0 77.69 13.30
2 -8 0 78.79 19.20
-2 8 0 85.69 15.20
2 8 0 115.09 18.30
-2 -8 0 74.99 15.90
-3 -8 0 5.30 3.50
3 -8 0 -1.20 9.50
3 8 0 9.50 13.60
-3 8 0 -7.60 4.40
-3 -8 0 1.30 9.70
3 -8 0 -10.50 15.20
4 -8 0 414.26 73.29
-4 8 0 589.24 72.09
-4 -8 0 486.15 71.99
4 -8 0 403.86 75.29
-5 8 0 14.00 9.70
-5 -8 0 12.00 6.00
5 -8 0 10.50 21.20
-6 -8 0 65.89 12.60
6 -8 0 26.40 23.60
-6 8 0 56.89 15.70
0 -9 0 0.70 14.10
0 -9 0 2.50 4.40
0 9 0 10.30 7.10
1 -9 0 348.47 63.29
1 9 0 526.95 66.09
-1 -9 0 420.86 62.99
-1 9 0 439.16 64.39
-1 -9 0 396.56 62.49
1 -9 0 440.76 63.69
2 9 0 35.80 11.70
-2 9 0 29.90 8.70
-2 -9 0 21.70 5.90
-2 -9 0 26.30 13.40
2 -9 0 14.70 15.50
2 -9 0 22.60 9.30
-3 9 0 15.60 7.80
3 -9 0 16.10 14.20
3 -9 0 36.50 19.10
-3 -9 0 3.20 4.30
4 -9 0 4.00 20.90
-4 -9 0 3.50 4.80
-4 9 0 0.10 6.80
-5 9 0 -3.10 7.70
5 -9 0 -5.20 22.40
-5 -9 0 -0.20 5.20
0 -10 0 2066.99 301.47
0 10 0 2418.06 296.57
0 -10 0 1786.32 281.37
-1 -10 0 240.78 39.00
-1 -10 0 201.18 41.50
1 -10 0 302.77 44.80
1 10 0 304.67 43.00
-1 10 0 294.57 41.60
1 -10 0 245.38 40.30
-2 -10 0 55.89 22.70
2 -10 0 33.40 14.80
-2 -10 0 51.19 9.80
2 10 0 60.59 18.80
-2 10 0 47.30 12.70
2 -10 0 19.10 20.40
-3 -10 0 95.29 17.10
-3 10 0 129.89 20.90
3 -10 0 71.19 26.90
-4 10 0 23.80 10.70
4 -10 0 11.70 20.60
-4 -10 0 38.00 8.50
0 11 0 15.50 11.80
0 -11 0 5.70 21.20
0 -11 0 18.00 8.40
-1 -11 0 21.60 7.30
1 11 0 45.70 17.00
1 -11 0 10.40 11.60
-1 11 0 19.70 11.30
1 -11 0 19.70 20.80
-1 -11 0 21.90 25.00
-2 11 0 28.40 12.00
-2 -11 0 13.80 6.40
2 -11 0 13.40 22.50
3 -11 0 15.30 25.50
-3 11 0 -7.00 9.90
-3 -11 0 2.80 5.20
0 0 1 -2.40 0.30
0 0 1 -2.30 0.70
0 0 -1 -2.40 1.10
0 0 -1 -2.50 0.40
0 0 -1 -2.50 0.60
0 0 1 -1.90 0.70
-1 0 1 2426.76 358.66
1 0 -1 2489.55 367.96
1 0 1 2489.55 359.06
1 0 1 2663.63 340.47
-1 0 1 2583.24 358.96
1 0 -1 2711.43 340.67
2 0 1 128.29 17.30
2 0 -1 90.89 17.40
2 0 1 84.29 17.80
2 0 -1 192.18 18.60
2 0 1 114.09 18.70
2 0 -1 114.09 18.60
3 0 1 278.47 37.80
3 0 1 196.48 37.90
3 0 -1 240.58 38.30
3 0 -1 259.67 35.80
3 0 1 329.17 36.50
3 0 -1 208.38 36.40
4 0 1 24.60 12.60
4 0 1 63.89 12.10
4 0 -1 35.80 11.90
4 0 1 42.90 11.30
4 0 -1 54.09 11.80
4 0 -1 55.89 11.80
5 0 1 219.48 33.80
5 0 1 210.18 32.10
5 0 -1 189.08 34.30
5 0 1 181.98 35.00
6 0 1 10.00 11.10
6 0 1 -5.60 12.00
-6 0 1 13.10 6.50
6 0 -1 10.00 14.80
-6 0 1 2.40 4.90
6 0 1 5.60 14.20
-7 0 -1 177.08 23.00
7 0 1 56.49 27.90
7 0 -1 87.49 28.10
-7 0 1 153.98 22.90
-7 0 1 152.78 22.80
7 0 1 169.18 29.00
8 0 -1 12.60 19.70
-8 0 -1 9.60 10.30
8 0 1 38.60 23.40
-8 0 -1 9.10 10.50
-8 0 1 13.20 10.30
0 -1 1 2021.70 284.67
0 1 1 1926.71 277.97
1 -1 1 1705.73 246.18
1 1 -1 1938.71 266.07
-1 -1 -1 1840.82 245.58
1 1 -1 1890.61 258.97
-1 -1 -1 1817.22 265.47
1 -1 1 1789.92 259.67
-1 1 1 1869.31 259.07
1 -1 -1 1808.42 246.18
1 -1 -1 1927.71 265.77
-1 -1 1 1892.11 245.68
-1 1 -1 1753.92 265.47
1 1 1 1868.81 245.58
-1 -1 1 1878.81 258.97
1 1 1 1775.92 259.37
2 -1 1 2244.88 295.87
-2 -1 -1 2127.39 279.47
2 1 -1 2053.69 294.97
-2 1 1 2206.28 294.87
2 -1 1 1995.80 280.47
2 -1 -1 1781.92 280.37
-2 -1 1 2158.38 279.57
2 -1 -1 2091.89 302.67
2 1 1 2134.09 295.47
3 -1 1 1257.67 160.88
3 1 -1 1123.89 173.58
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-1 -6 -17 -8.40 10.80
-1 6 17 4.40 19.30
1 -6 17 28.20 32.50
1 6 17 15.50 23.10
1 -6 -17 7.60 12.90
-1 -6 17 4.20 8.20
2 -6 17 8.20 23.40
2 -6 17 -19.70 12.50
-2 -6 -17 22.70 12.40
-2 6 17 -1.30 20.60
2 -6 -17 13.80 15.80
2 6 17 5.20 20.70
-2 -6 17 2.90 7.80
0 7 17 41.60 23.20
0 -7 17 75.09 15.70
0 -7 -17 20.50 14.70
1 -7 17 65.69 18.70
-1 7 17 17.20 23.30
-1 -7 -17 30.10 14.90
1 7 17 41.40 22.60
-1 -7 17 43.00 13.00
1 -7 -17 30.30 15.80
0 0 18 43.60 10.60
0 0 18 146.69 27.90
0 0 -18 106.89 21.60
-1 0 18 841.02 67.39
1 0 18 391.36 49.60
-1 0 -18 277.87 56.29
1 0 18 301.97 59.39
1 0 -18 219.08 54.99
-1 0 18 363.86 49.30
-2 0 18 22.60 26.20
2 0 18 12.50 21.90
-2 0 18 17.50 7.20
2 0 -18 20.30 16.60
3 0 18 51.49 25.10
-3 0 18 26.40 8.00
3 0 -18 6.00 19.10
4 0 -18 36.40 22.10
4 0 18 29.40 26.00
-4 0 18 33.40 9.30
0 -1 -18 216.88 46.00
0 1 18 297.77 40.00
0 -1 18 302.27 40.60
0 1 -18 226.28 47.50
0 1 18 363.36 52.49
-1 1 18 30.70 8.20
1 -1 18 62.09 24.30
-1 -1 -18 38.20 16.50
1 1 -18 18.90 17.20
1 -1 18 36.70 9.60
-1 1 18 47.30 22.70
-1 -1 18 24.70 8.20
1 -1 -18 44.30 18.70
1 1 18 84.29 24.80
-1 -1 18 55.09 26.50
2 1 -18 6.30 18.70
-2 1 18 24.00 22.00
-2 -1 -18 10.60 17.00
2 -1 18 2.70 11.50
-2 1 18 4.20 5.90
2 -1 18 10.40 22.00
2 -1 -18 7.30 15.30
-2 -1 18 13.70 7.10
2 1 18 21.30 23.10
3 1 -18 26.30 22.90
3 -1 18 27.20 24.40
-3 1 18 26.00 8.10
3 -1 -18 4.00 15.00
3 1 18 18.50 21.80
-3 -1 18 25.10 7.90
4 1 -18 -2.80 22.90
4 -1 18 14.80 24.10
-4 1 18 19.50 7.50
-4 -1 18 6.80 7.40
4 1 18 27.90 24.60
4 -1 -18 8.50 20.60
0 -2 -18 20.20 14.70
0 -2 18 -6.90 21.40
0 2 18 18.00 8.10
0 2 18 24.70 21.40
0 -2 18 3.40 6.80
1 -2 18 154.18 23.80
-1 2 18 160.58 22.40
-1 2 18 135.69 34.40
-1 -2 -18 95.69 27.10
1 -2 18 136.89 34.50
1 2 -18 118.89 32.30
1 2 18 113.69 34.60
1 -2 -18 119.89 28.90
-1 -2 18 168.88 23.20
-1 -2 18 182.38 37.20
-2 2 18 57.39 27.10
2 2 -18 32.00 22.30
2 -2 18 6.60 22.70
-2 2 18 38.70 9.80
2 -2 18 50.09 13.60
-2 -2 -18 42.50 16.50
2 -2 -18 34.50 17.70
-2 -2 18 49.40 10.70
2 2 18 80.79 27.40
3 -2 18 7.60 20.00
3 -2 18 5.70 22.30
3 2 -18 -13.60 21.30
-3 2 18 -13.90 25.00
-3 2 18 5.30 6.10
3 2 18 -9.10 23.90
-3 -2 18 -9.20 6.00
3 -2 -18 -6.30 16.20
-4 2 18 14.80 7.80
4 -2 18 11.60 23.00
4 2 -18 19.70 25.80
4 -2 -18 33.60 19.10
4 2 18 23.00 24.00
-4 -2 18 3.00 7.00
0 -3 18 123.39 30.90
0 3 18 116.79 27.70
0 -3 18 80.79 16.50
0 -3 -18 101.89 22.10
-1 -3 -18 32.90 15.60
-1 3 18 43.30 10.80
-1 3 18 58.89 26.60
1 -3 18 128.39 29.20
1 -3 18 61.49 13.10
1 -3 -18 20.10 17.30
-1 -3 18 46.40 11.00
1 3 18 59.39 23.30
2 -3 18 31.40 24.50
-2 3 18 27.60 7.70
2 3 -18 26.40 25.90
-2 -3 -18 14.30 13.80
2 -3 18 -12.40 9.70
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2 -3 -18 7.10 15.90
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-3 -3 -18 18.40 13.90
-3 3 18 33.50 23.60
3 -3 18 24.80 16.70
3 -3 18 27.50 24.00
-3 3 18 16.60 7.60
3 3 -18 19.90 23.70
3 -3 -18 9.60 16.70
3 3 18 26.80 22.80
-3 -3 18 5.90 8.30
-4 3 18 33.50 9.90
4 3 -18 23.90 26.80
4 -3 18 16.80 25.00
4 3 18 9.30 24.20
-4 -3 18 47.00 11.00
4 -3 -18 12.70 18.80
0 -4 -18 -0.80 12.90
0 -4 18 -1.30 7.50
0 4 18 -12.10 20.20
-1 4 18 57.49 25.00
1 -4 18 91.59 28.00
-1 -4 -18 49.50 16.80
1 -4 18 65.39 13.70
1 4 18 40.20 22.30
-1 -4 18 34.80 11.40
1 -4 -18 58.69 18.50
-2 4 18 60.49 11.00
2 -4 18 34.30 15.00
-2 -4 -18 34.80 15.00
2 -4 18 43.50 25.20
-2 4 18 76.39 25.60
-2 -4 18 23.80 9.80
2 -4 -18 25.60 17.00
2 4 18 67.99 26.50
3 -4 18 22.00 18.00
3 -4 18 46.60 25.50
-3 4 18 19.50 8.80
-3 4 18 35.00 24.60
3 4 -18 15.20 29.70
-3 -4 -18 24.30 13.50
3 -4 -18 8.80 17.70
3 4 18 20.20 24.60
-3 -4 18 35.60 9.90
0 -5 -18 0.80 12.60
0 -5 18 13.10 9.00
0 5 18 -1.40 19.20
1 -5 18 328.67 51.89
1 -5 18 462.85 64.29
-1 5 18 384.76 61.29
-1 -5 -18 260.47 55.29
1 5 18 446.46 64.59
-1 -5 18 433.46 52.29
1 -5 -18 290.47 56.29
2 -5 18 42.30 25.00
-2 5 18 32.60 24.10
2 -5 18 36.60 15.70
-2 -5 -18 14.50 14.30
-2 -5 18 37.60 10.30
2 -5 -18 57.89 19.60
2 5 18 48.70 24.50
0 6 18 149.39 34.10
0 -6 18 126.69 23.00
0 -6 -18 106.79 25.60
1 -6 18 10.10 11.90
-1 -6 -18 -1.50 12.60
-1 6 18 -7.00 20.40
-1 -6 18 5.50 9.20
1 6 18 -14.00 22.10
1 -6 -18 -4.30 14.20
0 0 -19 58.29 21.80
0 0 19 106.09 28.80
0 0 19 25.50 8.50
1 0 19 12.00 10.90
1 0 19 16.00 24.20
-1 0 19 18.00 7.50
1 0 -19 -0.90 17.50
-1 0 19 23.60 25.60
2 0 19 207.38 38.60
-2 0 19 171.38 24.10
2 0 -19 84.79 30.00
3 0 -19 9.90 20.30
-3 0 19 35.70 9.70
3 0 19 16.40 25.50
4 0 19 46.70 29.80
0 1 19 11.60 7.30
0 -1 -19 7.40 16.80
0 -1 19 10.90 23.70
0 1 19 19.60 23.90
0 -1 19 0.20 5.70
-1 -1 -19 59.89 24.30
1 -1 19 101.19 17.00
-1 1 19 103.19 15.70
-1 1 19 143.79 30.30
1 1 -19 67.09 25.60
1 -1 19 58.79 28.20
-1 -1 19 73.99 15.60
1 1 19 67.59 30.00
-1 -1 19 189.08 36.80
1 -1 -19 72.39 23.60
-2 1 19 34.10 9.00
-2 1 19 21.40 28.60
2 -1 19 28.80 24.60
2 1 -19 4.50 21.40
-2 -1 19 35.20 9.40
2 -1 -19 21.10 18.60
2 1 19 40.00 27.50
3 1 -19 4.40 22.40
3 -1 19 13.00 24.60
-3 1 19 1.10 7.30
3 1 19 7.70 24.50
-3 -1 19 -4.00 6.70
3 -1 -19 21.10 18.90
0 -2 -19 -10.60 15.30
0 -2 19 2.10 26.80
0 2 19 6.60 22.80
0 -2 19 -0.90 6.90
-1 2 19 83.39 27.70
1 -2 19 45.30 27.00
1 -2 19 58.99 13.10
-1 -2 -19 31.90 17.90
-1 2 19 72.59 12.20
-1 -2 19 57.89 12.20
1 -2 -19 29.90 19.40
1 2 19 38.50 26.40
2 2 -19 48.50 27.30
-2 2 19 46.70 9.90
-2 -2 -19 23.90 18.80
2 -2 19 38.00 25.70
-2 2 19 58.69 26.50
2 -2 19 24.80 14.20
2 -2 -19 52.39 19.70
-2 -2 19 20.30 9.80
2 2 19 77.89 27.80
-3 2 19 13.50 8.10
3 -2 19 45.30 26.60
3 2 -19 49.80 27.30
-3 2 19 52.49 37.70
3 2 19 41.20 28.90
3 -2 -19 14.30 18.00
-3 -2 19 47.30 10.40
0 3 19 160.88 36.00
0 -3 19 154.28 24.50
0 -3 19 183.08 41.30
0 -3 -19 122.09 28.80
1 -3 19 22.70 26.60
-1 3 19 20.00 24.80
-1 -3 -19 9.00 14.70
1 -3 19 26.70 11.10
-1 -3 19 4.60 6.80
1 -3 -19 3.80 16.50
1 3 19 4.40 23.10
-2 3 19 92.09 30.60
2 -3 19 97.99 20.70
-2 -3 -19 78.39 22.60
-2 3 19 94.09 16.60
2 -3 19 131.09 32.20
2 3 19 58.69 30.20
2 -3 -19 69.89 24.10
-2 -3 19 110.49 17.80
3 -3 19 26.30 24.70
-3 -3 -19 47.40 20.00
-3 3 19 82.29 12.60
3 3 -19 17.70 28.70
-3 3 19 46.60 28.90
3 -3 19 36.00 25.40
3 -3 -19 12.90 19.90
3 3 19 14.20 27.50
-3 -3 19 44.70 12.60
0 4 19 3.50 20.60
0 -4 -19 17.20 16.00
0 -4 19 -4.90 8.10
-1 -4 -19 69.79 25.70
1 -4 19 152.38 24.80
1 -4 19 172.38 38.40
-1 4 19 189.58 36.40
1 4 19 161.88 38.10
1 -4 -19 92.19 27.20
-1 -4 19 185.08 24.20
2 -4 19 57.59 29.40
2 -4 19 63.99 18.90
-2 4 19 62.79 27.40
-2 4 19 64.09 15.70
-2 -4 -19 63.59 19.80
2 4 19 124.09 34.00
2 -4 -19 67.49 22.40
-2 -4 19 80.59 15.50
0 -5 -19 32.10 17.90
0 -5 19 70.89 15.30
0 5 19 71.29 30.60
1 -5 19 15.60 12.50
-1 5 19 33.20 24.10
-1 -5 -19 24.50 15.10
1 -5 -19 11.10 16.70
-1 -5 19 26.50 11.00
1 5 19 -4.50 21.30
0 0 20 95.49 31.60
0 0 20 19.50 8.90
0 0 -20 25.60 24.20
-1 0 20 57.09 12.10
1 0 20 16.80 27.30
1 0 -20 33.20 22.20
-1 0 20 147.59 36.60
-2 0 20 37.70 9.80
2 0 -20 -3.30 19.90
2 0 20 25.50 28.40
3 0 -20 -0.90 22.40
3 0 20 13.20 28.80
-3 0 20 28.80 9.70
0 -1 20 -7.30 24.50
0 -1 -20 -2.30 20.20
0 1 20 13.30 27.90
0 -1 20 11.00 8.00
1 -1 20 29.10 28.70
1 1 -20 15.20 27.10
1 -1 20 62.39 15.10
-1 1 20 57.79 12.00
-1 1 20 52.29 27.50
-1 -1 20 54.49 12.30
1 1 20 96.69 32.60
1 -1 -20 56.89 22.10
-2 1 20 10.00 7.80
-2 1 20 45.60 34.60
2 -1 20 44.40 29.60
2 1 -20 0.70 22.70
2 -1 -20 -14.80 17.80
-2 -1 20 30.80 9.40
2 1 20 19.50 26.30
-3 1 20 33.60 10.00
3 -1 20 52.69 30.20
3 1 -20 52.19 26.50
-3 -1 20 33.00 10.40
3 1 20 39.80 29.70
3 -1 -20 2.50 19.70
0 -2 20 21.60 9.60
0 2 20 18.20 24.90
0 -2 -20 6.60 18.40
0 -2 20 15.20 32.40
-1 -2 -20 52.49 23.30
1 -2 20 74.69 31.20
-1 2 20 42.40 27.70
1 -2 20 71.79 16.90
-1 2 20 110.89 17.20
-1 -2 20 98.99 16.40
1 -2 -20 58.79 23.90
1 2 20 69.39 32.10
2 -2 20 61.89 21.70
2 -2 20 17.40 28.50
2 2 -20 41.10 32.00
-2 2 20 40.10 30.30
-2 2 20 32.40 10.80
2 -2 -20 40.70 20.60
2 2 20 50.89 30.90
-2 -2 20 55.09 11.40
0 3 20 25.40 26.10
0 -3 -20 48.10 19.30
0 -3 20 11.40 9.50
1 -3 20 6.80 11.30
-1 -3 -20 34.10 17.90
-1 3 20 60.89 28.70
1 -3 20 15.30 29.10
-1 -3 20 16.50 9.20
1 3 20 -1.70 25.00
1 -3 -20 46.70 20.00
2 -3 20 56.99 18.70
2 -3 20 46.40 28.30
-2 3 20 51.09 13.90
-2 -3 -20 22.30 20.30
-2 3 20 68.19 33.00
2 -3 -20 56.29 22.90
2 3 20 70.89 30.10
-2 -3 20 62.79 13.40
0 4 20 652.13 94.39
0 -4 -20 485.05 89.09
0 -4 20 635.74 82.29
-1 -4 -20 9.40 16.20
1 -4 20 35.10 32.30
-1 4 20 20.60 28.00
1 -4 20 24.50 12.50
1 4 20 40.80 25.20
1 -4 -20 -16.30 17.10
-1 -4 20 8.70 8.90
0 0 21 10.20 11.90
0 0 21 56.99 31.70
1 0 21 -3.50 26.50
-1 0 21 -19.30 37.00
-1 0 21 2.40 8.20
1 0 -21 21.60 24.70
0 -1 21 28.80 10.70
0 -1 21 20.00 31.50
0 -1 -21 28.30 26.10
0 1 21 47.70 29.80
1 -1 21 0.90 28.10
-1 1 21 0.80 10.90
-1 1 21 34.30 29.40
1 -1 -21 -5.80 19.70
1 1 21 -0.60 29.70
-1 -1 21 10.80 8.40
0 2 21 26.90 29.20
0 -2 21 33.50 11.50
0 -2 -21 51.99 22.90
1 -2 21 35.60 31.00
1 -2 21 35.40 14.30
-1 2 21 44.40 30.10
-1 -2 21 14.50 9.10
1 2 21 28.70 30.70
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 45367
_shelx_res_file
;
TITL mo for general quality
new_mo.res
created by SHELXL-2017/1 at 10:43:31 on 15-Jun-2019
CELL 0.71073 7.3466 10.1967 18.4766 90.000 90.000 90.000
ZERR 4.000 0.0040 0.0056 0.0101 0.000 0.000 0.000
LATT -1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, -Z
SFAC C H N O
UNIT 52 72 8 16
OMIT 0 1 1
L.S. 10
ACTA
BOND $H
FMAP 2
PLAN -20
SIZE 0.29 0.28 0.35
TEMP -173
WGHT 0.022800 0.606300
FVAR 0.90649
O1 4 0.470115 0.350843 0.578748 11.00000 0.04345 0.03759 =
0.03622 0.00206 -0.00708 -0.02133
O2 4 0.655051 0.442700 0.660518 11.00000 0.03120 0.02247 =
0.02242 0.00214 -0.00231 -0.00399
O3 4 0.780568 0.881772 0.626639 11.00000 0.01965 0.02165 =
0.03508 -0.00573 0.00105 0.00043
O4 4 1.066344 0.954114 0.649168 11.00000 0.02289 0.01400 =
0.02595 -0.00070 -0.00177 -0.00075
N1 3 0.749830 0.638511 0.569254 11.00000 0.01990 0.01797 =
0.02475 -0.00022 -0.00109 0.00086
H1N 2 0.677598 0.705861 0.587027 11.00000 0.02154
N2 3 1.378647 0.726030 0.596934 11.00000 0.02606 0.03041 =
0.02995 -0.00046 -0.00015 0.00119
C1 1 0.674901 0.518329 0.538748 11.00000 0.02698 0.01560 =
0.02395 -0.00053 -0.00831 -0.00117
AFIX 13
H1 2 0.582280 0.541944 0.501289 11.00000 -1.20000
AFIX 0
C2 1 0.841506 0.457050 0.500751 11.00000 0.03549 0.01937 =
0.02347 -0.00323 -0.00341 -0.00111
AFIX 23
H2A 2 0.843025 0.360684 0.507255 11.00000 -1.20000
H2B 2 0.840489 0.477085 0.448324 11.00000 -1.20000
AFIX 0
C3 1 1.005598 0.520235 0.537645 11.00000 0.02689 0.01639 =
0.02424 -0.00037 0.00089 0.00317
AFIX 23
H3A 2 1.055995 0.462237 0.575657 11.00000 -1.20000
H3B 2 1.102471 0.540554 0.502126 11.00000 -1.20000
AFIX 0
C4 1 0.927826 0.644119 0.570059 11.00000 0.02492 0.01699 =
0.01458 0.00397 -0.00018 0.00149
C5 1 0.586304 0.428517 0.594587 11.00000 0.02729 0.02029 =
0.02749 0.00000 -0.00279 -0.00050
C6 1 0.575445 0.359253 0.716708 11.00000 0.03897 0.03249 =
0.02974 0.00777 0.00502 -0.00437
AFIX 137
H6A 2 0.447561 0.383309 0.723879 11.00000 -1.50000
H6B 2 0.642325 0.371383 0.762109 11.00000 -1.50000
H6C 2 0.583167 0.267216 0.701744 11.00000 -1.50000
AFIX 0
C7 1 1.031108 0.748351 0.596619 11.00000 0.02160 0.01636 =
0.01931 0.00032 -0.00157 0.00168
C8 1 1.222319 0.737307 0.596007 11.00000 0.02952 0.01471 =
0.01967 0.00110 0.00305 0.00021
C9 1 0.942820 0.865489 0.624854 11.00000 0.02345 0.01775 =
0.01725 0.00227 0.00051 -0.00152
C10 1 1.004000 1.083036 0.677512 11.00000 0.03422 0.01332 =
0.02574 -0.00481 0.00041 0.00137
C11 1 1.179396 1.149995 0.698839 11.00000 0.04266 0.02224 =
0.03796 -0.00645 -0.00394 -0.00628
AFIX 137
H11A 2 1.260278 1.154912 0.656748 11.00000 -1.50000
H11B 2 1.238827 1.099748 0.737386 11.00000 -1.50000
H11C 2 1.152872 1.238765 0.716218 11.00000 -1.50000
AFIX 0
C12 1 0.910935 1.159245 0.617737 11.00000 0.04663 0.02006 =
0.02975 -0.00005 0.00001 0.00857
AFIX 137
H12A 2 0.985600 1.155885 0.573823 11.00000 -1.50000
H12B 2 0.895526 1.250717 0.632817 11.00000 -1.50000
H12C 2 0.791425 1.120475 0.607869 11.00000 -1.50000
AFIX 0
C13 1 0.885135 1.062289 0.743025 11.00000 0.04916 0.02716 =
0.02543 -0.00498 0.00874 -0.00380
AFIX 137
H13A 2 0.861422 1.146855 0.766397 11.00000 -1.50000
H13B 2 0.947119 1.003897 0.777191 11.00000 -1.50000
H13C 2 0.769592 1.022628 0.728074 11.00000 -1.50000
AFIX 0
HKLF 4
REM mo for general quality
REM R1 = 0.0512 for 2051 Fo > 4sig(Fo) and 0.0584 for all 2290 data
REM 180 parameters refined using 0 restraints
END
WGHT 0.0197 0.6186
REM Highest difference peak 0.207, deepest hole -0.182, 1-sigma level 0.051
Q1 1 0.5118 0.7311 0.5879 11.00000 0.05 0.21
Q2 1 0.7221 0.9605 0.6316 11.00000 0.05 0.20
Q3 1 0.5019 0.7547 0.5977 11.00000 0.05 0.20
Q4 1 1.4692 0.8011 0.5970 11.00000 0.05 0.19
Q5 1 1.1211 0.7677 0.5859 11.00000 0.05 0.19
Q6 1 0.7631 0.6427 0.6232 11.00000 0.05 0.18
Q7 1 1.0029 0.3919 0.5986 11.00000 0.05 0.18
Q8 1 0.4935 0.4561 0.7194 11.00000 0.05 0.18
Q9 1 1.4403 0.8511 0.6032 11.00000 0.05 0.17
Q10 1 0.5330 0.9503 0.6515 11.00000 0.05 0.17
Q11 1 1.2113 0.8776 0.6008 11.00000 0.05 0.17
Q12 1 0.4371 0.4470 0.5979 11.00000 0.05 0.17
Q13 1 0.5906 0.8600 0.5980 11.00000 0.05 0.17
Q14 1 1.2495 1.1748 0.6002 11.00000 0.05 0.16
Q15 1 1.2855 0.6450 0.5780 11.00000 0.05 0.16
Q16 1 0.6642 1.0622 0.5999 11.00000 0.05 0.16
Q17 1 0.9606 0.6677 0.6122 11.00000 0.05 0.16
Q18 1 1.2492 0.6582 0.5927 11.00000 0.05 0.16
Q19 1 0.3310 0.3670 0.5922 11.00000 0.05 0.16
Q20 1 1.2491 0.4660 0.5948 11.00000 0.05 0.16
;
_shelx_res_checksum 50600
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'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
O O1 0.4701(4) 0.3508(3) 0.57875(17) 0.0391(9) Uani d 1
O O2 0.6551(4) 0.4427(3) 0.66052(15) 0.0254(7) Uani d 1
O O3 0.7806(4) 0.8818(3) 0.62664(16) 0.0255(7) Uani d 1
O O4 1.0663(4) 0.9541(2) 0.64917(14) 0.0209(7) Uani d 1
N N1 0.7498(4) 0.6385(3) 0.56925(18) 0.0209(8) Uani d 1
H H1N 0.678(6) 0.706(4) 0.587(2) 0.022(11) Uiso d 1
N N2 1.3786(5) 0.7260(3) 0.5969(2) 0.0288(9) Uani d 1
C C1 0.6749(6) 0.5183(3) 0.5387(2) 0.0222(9) Uani d 1
H H1 0.582280 0.541944 0.501289 0.027 Uiso calc 1
C C2 0.8415(6) 0.4571(4) 0.5008(2) 0.0261(10) Uani d 1
H H2A 0.843025 0.360684 0.507255 0.031 Uiso calc 1
H H2B 0.840489 0.477085 0.448324 0.031 Uiso calc 1
C C3 1.0056(6) 0.5202(4) 0.5376(2) 0.0225(9) Uani d 1
H H3A 1.055995 0.462237 0.575657 0.027 Uiso calc 1
H H3B 1.102471 0.540554 0.502126 0.027 Uiso calc 1
C C4 0.9278(5) 0.6441(4) 0.5701(2) 0.0188(9) Uani d 1
C C5 0.5863(6) 0.4285(4) 0.5946(2) 0.0250(10) Uani d 1
C C6 0.5754(7) 0.3593(5) 0.7167(2) 0.0337(11) Uani d 1
H H6A 0.447561 0.383309 0.723879 0.051 Uiso calc 1
H H6B 0.642325 0.371383 0.762109 0.051 Uiso calc 1
H H6C 0.583167 0.267216 0.701744 0.051 Uiso calc 1
C C7 1.0311(5) 0.7484(4) 0.5966(2) 0.0191(9) Uani d 1
C C8 1.2223(6) 0.7373(4) 0.5960(2) 0.0213(9) Uani d 1
C C9 0.9428(6) 0.8655(4) 0.6249(2) 0.0195(9) Uani d 1
C C10 1.0040(6) 1.0830(3) 0.6775(2) 0.0244(10) Uani d 1
C C11 1.1794(7) 1.1500(4) 0.6988(3) 0.0343(11) Uani d 1
H H11A 1.260278 1.154912 0.656748 0.051 Uiso calc 1
H H11B 1.238827 1.099748 0.737386 0.051 Uiso calc 1
H H11C 1.152872 1.238765 0.716218 0.051 Uiso calc 1
C C12 0.9109(7) 1.1592(4) 0.6177(2) 0.0321(11) Uani d 1
H H12A 0.985600 1.155885 0.573823 0.048 Uiso calc 1
H H12B 0.895526 1.250717 0.632817 0.048 Uiso calc 1
H H12C 0.791425 1.120475 0.607869 0.048 Uiso calc 1
C C13 0.8851(7) 1.0623(4) 0.7430(2) 0.0339(11) Uani d 1
H H13A 0.861422 1.146855 0.766397 0.051 Uiso calc 1
H H13B 0.947119 1.003897 0.777191 0.051 Uiso calc 1
H H13C 0.769592 1.022628 0.728074 0.051 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
O1 0.043(2) 0.0376(18) 0.0362(19) -0.0213(16) -0.0071(16) 0.0021(15)
O2 0.0312(16) 0.0225(13) 0.0224(15) -0.0040(13) -0.0023(13) 0.0021(12)
O3 0.0196(15) 0.0217(14) 0.0351(17) 0.0004(12) 0.0010(13) -0.0057(13)
O4 0.0229(14) 0.0140(13) 0.0259(16) -0.0008(11) -0.0018(12) -0.0007(12)
N1 0.0199(19) 0.0180(17) 0.0247(19) 0.0009(15) -0.0011(14) -0.0002(15)
N2 0.026(2) 0.030(2) 0.030(2) 0.0012(15) -0.0002(16) -0.0005(16)
C1 0.027(2) 0.0156(18) 0.024(2) -0.0012(16) -0.0083(18) -0.0005(16)
C2 0.035(2) 0.019(2) 0.023(2) -0.001(2) -0.0034(19) -0.0032(17)
C3 0.027(2) 0.0164(19) 0.024(2) 0.0032(17) 0.0009(18) -0.0004(17)
C4 0.025(2) 0.017(2) 0.015(2) 0.0015(17) -0.0002(17) 0.0040(16)
C5 0.027(2) 0.020(2) 0.027(3) -0.0005(18) -0.0028(19) 0.0000(18)
C6 0.039(3) 0.032(2) 0.030(3) -0.004(2) 0.005(2) 0.008(2)
C7 0.022(2) 0.0164(18) 0.019(2) 0.0017(17) -0.0016(17) 0.0003(16)
C8 0.030(2) 0.0147(19) 0.020(2) 0.0002(17) 0.0030(18) 0.0011(16)
C9 0.023(2) 0.0178(19) 0.017(2) -0.0015(17) 0.0005(17) 0.0023(17)
C10 0.034(2) 0.0133(18) 0.026(2) 0.0014(17) 0.000(2) -0.0048(16)
C11 0.043(3) 0.022(2) 0.038(3) -0.006(2) -0.004(2) -0.006(2)
C12 0.047(3) 0.020(2) 0.030(3) 0.009(2) 0.000(2) 0.0000(19)
C13 0.049(3) 0.027(2) 0.025(2) -0.004(2) 0.009(2) -0.005(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C5 O2 C6 115.8(3)
C9 O4 C10 119.9(3)
C4 N1 C1 114.7(4)
C4 N1 H1N 122(3)
C1 N1 H1N 123(3)
N1 C1 C5 113.9(3)
N1 C1 C2 102.5(3)
C5 C1 C2 113.8(3)
N1 C1 H1 108.8
C5 C1 H1 108.8
C2 C1 H1 108.8
C3 C2 C1 104.6(3)
C3 C2 H2A 110.8
C1 C2 H2A 110.8
C3 C2 H2B 110.8
C1 C2 H2B 110.8
H2A C2 H2B 108.9
C4 C3 C2 103.4(3)
C4 C3 H3A 111.1
C2 C3 H3A 111.1
C4 C3 H3B 111.1
C2 C3 H3B 111.1
H3A C3 H3B 109.1
N1 C4 C7 125.5(4)
N1 C4 C3 109.7(4)
C7 C4 C3 124.8(3)
O1 C5 O2 124.5(4)
O1 C5 C1 122.3(4)
O2 C5 C1 113.2(3)
O2 C6 H6A 109.5
O2 C6 H6B 109.5
H6A C6 H6B 109.5
O2 C6 H6C 109.5
H6A C6 H6C 109.5
H6B C6 H6C 109.5
C4 C7 C8 118.6(4)
C4 C7 C9 120.6(3)
C8 C7 C9 120.8(4)
N2 C8 C7 178.3(5)
O3 C9 O4 124.1(4)
O3 C9 C7 124.3(4)
O4 C9 C7 111.5(3)
O4 C10 C13 109.7(3)
O4 C10 C11 103.2(3)
C13 C10 C11 110.4(4)
O4 C10 C12 109.6(3)
C13 C10 C12 113.3(4)
C11 C10 C12 110.1(4)
C10 C11 H11A 109.5
C10 C11 H11B 109.5
H11A C11 H11B 109.5
C10 C11 H11C 109.5
H11A C11 H11C 109.5
H11B C11 H11C 109.5
C10 C12 H12A 109.5
C10 C12 H12B 109.5
H12A C12 H12B 109.5
C10 C12 H12C 109.5
H12A C12 H12C 109.5
H12B C12 H12C 109.5
C10 C13 H13A 109.5
C10 C13 H13B 109.5
H13A C13 H13B 109.5
C10 C13 H13C 109.5
H13A C13 H13C 109.5
H13B C13 H13C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C5 1.201(5)
O2 C5 1.327(5)
O2 C6 1.464(5)
O3 C9 1.204(5)
O4 C9 1.357(5)
O4 C10 1.487(5)
N1 C4 1.309(5)
N1 C1 1.457(5)
N1 H1N 0.93(4)
N2 C8 1.154(5)
C1 C5 1.525(6)
C1 C2 1.543(6)
C1 H1 1.0000
C2 C3 1.527(6)
C2 H2A 0.9900
C2 H2B 0.9900
C3 C4 1.510(5)
C3 H3A 0.9900
C3 H3B 0.9900
C4 C7 1.395(5)
C6 H6A 0.9800
C6 H6B 0.9800
C6 H6C 0.9800
C7 C8 1.409(6)
C7 C9 1.456(5)
C10 C13 1.507(6)
C10 C11 1.511(6)
C10 C12 1.514(6)
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 H13A 0.9800
C13 H13B 0.9800
C13 H13C 0.9800
_cod_database_fobs_code 2021790