#------------------------------------------------------------------------------
#$Date: 2019-06-18 16:09:00 +0300 (Tue, 18 Jun 2019) $
#$Revision: 216075 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/16/2021679.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_2021679
loop_
_publ_author_name
'Eugenia D. Voronova'
'Alexander A. Golovanov'
'Ivan S. Odin'
'Maksim A. Anisimov'
'Pavel V. Dorovatovskii'
'Yan V. Zubavichus'
'Anna V. Vologzhanina'
_publ_section_title
;
Peculiarities of supramolecular organization of cyclic ketones with
vinylacetylene fragments
;
_journal_coeditor_code JX3023
_journal_issue 12
_journal_name_full 'Acta Crystallographica, Section C'
_journal_page_first 1674
_journal_page_last 1683
_journal_paper_doi 10.1107/S2053229618015838
_journal_volume 74
_journal_year 2018
_chemical_absolute_configuration .
_chemical_formula_iupac 'C20 H16 O2'
_chemical_formula_moiety 'C20 H16 O2'
_chemical_formula_sum 'C20 H16 O2'
_chemical_formula_weight 288.33
_chemical_name_systematic
;
2-(Furan-2-ylmethylene)-6-(3-phenylprop-2-yn-1-ylidene)cyclohexanone
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 29
_space_group_name_Hall 'P 2c -2ac'
_space_group_name_H-M_alt 'P c a 21'
_atom_sites_solution_hydrogens geom
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 9.5892(19)
_cell_length_b 10.145(2)
_cell_length_c 30.080(6)
_cell_measurement_reflns_used 7860
_cell_measurement_temperature 100
_cell_measurement_theta_max 37
_cell_measurement_theta_min 4
_cell_volume 2926.3(10)
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature 100
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type 'Mar CCD'
_diffrn_measurement_method 'phi scan'
_diffrn_radiation_type synchrotron
_diffrn_radiation_wavelength 0.9699
_diffrn_reflns_av_R_equivalents 0.0907
_diffrn_reflns_av_unetI/netI 0.1532
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 37
_diffrn_reflns_limit_l_min -37
_diffrn_reflns_number 15016
_diffrn_reflns_theta_full 35.587
_diffrn_reflns_theta_max 38.360
_diffrn_reflns_theta_min 3.306
_exptl_absorpt_coefficient_mu 0.187
_exptl_absorpt_correction_T_max 0.999
_exptl_absorpt_correction_T_min 0.945
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SCALA; Evans, 2006)
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.309
_exptl_crystal_description needle
_exptl_crystal_F_000 1216
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.015
_refine_diff_density_max 1.077
_refine_diff_density_min -0.510
_refine_ls_abs_structure_details
;
Flack x determined using 1267 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.3(8)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.011
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 397
_refine_ls_number_reflns 5675
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.011
_refine_ls_R_factor_all 0.1374
_refine_ls_R_factor_gt 0.0948
_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^)+(0.0100P)^2^+9.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2136
_refine_ls_wR_factor_ref 0.2496
_reflns_number_gt 3732
_reflns_number_total 5675
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file 5a.cif
_cod_data_source_block 5a
_cod_original_cell_volume 2926.2(10)
_cod_database_code 2021679
_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 0.929
_shelx_estimated_absorpt_t_max 0.997
_shelx_hkl_file
;
0 0 4 259.12 39.60
0 0 -4 275.43 39.62
0 0 5 -2.97 2.56
0 0 -5 1.85 3.12
0 0 6 3550.84 527.63
0 0 -6 3551.39 527.64
0 0 7 2.39 3.19
0 0 -7 0.78 3.84
0 0 8 984.14 152.30
0 0 -8 1062.12 152.34
0 0 9 0.25 3.17
0 0 -9 1.75 2.76
0 0 -9 -0.89 4.06
0 0 10 376.02 56.57
0 0 -10 377.28 111.93
0 0 -10 389.48 56.65
0 0 11 -2.02 4.27
0 0 -11 1.10 2.60
0 0 -11 5.34 4.24
0 0 12 1155.71 162.60
0 0 -12 1034.11 320.99
0 0 -12 1116.25 162.60
0 0 13 1.64 4.47
0 0 -13 4.43 3.27
0 0 -13 0.92 4.55
0 0 14 4247.03 625.34
0 0 -14 4177.33 1233.82
0 0 -14 4211.73 625.34
0 0 15 -0.62 3.76
0 0 -15 6.72 3.73
0 0 -15 3.69 4.61
0 0 16 202.58 22.74
0 0 -16 182.74 56.45
0 0 -16 191.66 28.77
0 0 17 5.54 4.07
0 0 -17 6.26 4.27
0 0 -17 2.89 4.74
0 0 18 100.91 14.52
0 0 -18 97.20 29.72
0 0 -18 101.29 15.52
0 0 19 -0.87 3.58
0 0 -19 -1.15 3.50
0 0 -19 4.38 4.89
0 0 20 69.95 11.75
0 0 -20 61.35 20.95
0 0 -20 75.64 11.41
0 0 21 -2.95 3.68
0 0 -21 5.03 3.20
0 0 -21 -1.82 4.76
0 0 22 34.06 8.57
0 0 -22 31.36 12.62
0 0 -22 54.13 7.73
0 0 23 2.14 5.58
0 0 -23 -1.51 2.91
0 0 -23 10.10 4.83
0 0 -24 701.56 61.48
0 0 24 559.83 95.98
0 0 -24 643.14 189.27
0 0 -25 5.72 3.33
0 0 25 -6.88 5.41
0 0 -25 1.76 4.76
0 0 -26 186.84 28.15
0 0 -27 4.08 5.29
0 0 -28 51.00 9.31
0 0 -29 0.15 5.18
0 0 -30 819.65 122.14
0 0 -31 0.99 3.75
0 0 -32 477.88 47.15
0 0 -33 -0.83 5.47
0 0 -34 855.08 127.58
0 0 -35 3.31 6.46
0 0 -36 31.55 7.82
0 0 -37 1.10 6.64
0 1 2 1018.10 101.23
0 -1 -2 1030.08 319.06
0 -1 -2 1109.94 161.39
0 -1 -2 1166.72 161.46
0 1 3 4.84 3.04
0 -1 -3 -0.49 1.19
0 -1 -3 -0.08 3.34
0 -1 -3 2.15 2.27
0 1 3 -1.10 2.54
0 -1 -4 127.95 16.36
0 1 4 138.91 39.86
0 1 4 133.67 20.12
0 -1 -4 123.95 39.87
0 -1 -4 141.02 20.16
0 1 4 146.52 20.12
0 1 5 0.47 2.60
0 -1 -5 7.56 2.75
0 -1 -5 -0.58 2.89
0 1 5 0.94 2.77
0 1 6 9178.08 1363.94
0 1 7 0.01 3.51
0 -1 -7 -2.95 4.11
0 -1 -7 2.95 3.32
0 1 7 2.10 2.19
0 1 8 17.04 4.49
0 1 8 15.46 3.88
0 -1 -8 10.63 4.73
0 -1 -8 13.19 4.50
0 -1 -8 14.78 3.88
0 -1 -9 0.60 2.87
0 1 9 5.40 3.36
0 -1 -9 -0.79 3.28
0 1 9 2.75 3.80
0 1 10 415.35 60.93
0 -1 -10 429.42 60.99
0 -1 -10 390.15 60.92
0 1 10 408.66 60.96
0 -1 -11 0.61 2.80
0 1 11 1.98 2.68
0 1 11 2.31 3.96
0 -1 -11 -2.19 2.13
0 -1 -11 1.94 3.85
0 1 12 118.22 17.04
0 -1 -12 132.33 16.77
0 -1 -12 130.42 38.97
0 -1 -12 141.68 19.90
0 1 12 133.92 19.92
0 1 13 -1.77 2.60
0 -1 -13 5.98 3.59
0 -1 -13 -2.45 2.81
0 -1 -13 -3.36 3.26
0 1 13 4.84 2.76
0 1 13 -2.76 4.23
0 1 14 1530.10 232.50
0 -1 -14 1639.77 458.96
0 -1 -14 1528.91 232.51
0 1 14 1571.64 458.93
0 1 14 1540.94 232.52
0 1 15 1.21 2.76
0 1 15 -3.20 4.28
0 -1 -15 -3.01 2.42
0 -1 -15 -0.26 4.91
0 -1 -15 1.86 3.51
0 1 15 2.96 2.78
0 1 16 233.22 24.48
0 1 16 232.22 33.53
0 -1 -16 215.39 65.93
0 -1 -16 238.56 33.60
0 -1 -16 208.38 33.43
0 1 16 215.73 65.90
0 1 17 1.47 2.65
0 -1 -17 0.68 3.05
0 -1 -17 0.53 2.35
0 -1 -17 1.22 2.34
0 1 17 0.62 2.83
0 1 17 -6.04 4.45
0 1 18 713.00 84.76
0 1 18 925.82 136.69
0 -1 -18 976.21 269.70
0 -1 -18 1047.50 136.73
0 -1 -18 947.59 136.69
0 1 18 936.00 269.68
0 -1 -19 0.61 2.76
0 1 19 2.65 4.58
0 -1 -19 -1.78 2.05
0 -1 -19 -5.78 5.22
0 1 19 -1.32 3.31
0 1 19 -1.89 4.63
0 1 20 1042.98 116.41
0 1 20 1291.21 191.19
0 -1 -20 1244.19 377.18
0 -1 -20 1441.97 191.23
0 -1 -20 1357.23 191.23
0 1 20 1388.12 377.19
0 -1 -21 1.73 3.54
0 1 21 1.00 4.87
0 -1 -21 -1.55 2.29
0 -1 -21 1.78 5.35
0 1 21 1.65 3.71
0 1 21 0.41 4.70
0 1 22 121.78 16.43
0 -1 -22 121.66 17.98
0 -1 -22 105.35 18.09
0 1 22 100.52 34.17
0 1 22 121.76 17.64
0 1 23 0.78 3.61
0 -1 -23 1.57 3.68
0 -1 -23 2.77 4.18
0 1 23 -1.37 2.83
0 -1 -23 -1.04 4.85
0 1 23 6.50 3.74
0 1 24 621.48 94.95
0 -1 -24 578.27 186.88
0 -1 -24 784.09 94.88
0 -1 -24 532.11 94.74
0 1 24 578.81 186.86
0 1 24 663.66 94.69
0 -1 -25 0.56 3.46
0 -1 -25 -2.51 5.58
0 -1 -25 1.83 7.03
0 1 25 -1.62 4.16
0 -1 -26 5.12 5.62
0 1 26 3.88 4.35
0 -1 -27 2.38 5.72
0 1 27 -0.95 5.22
0 -1 -28 767.53 71.72
0 1 28 750.18 113.02
0 -1 -29 -0.96 6.04
0 1 29 1.94 3.25
0 1 30 1689.69 166.74
0 -1 -30 2040.06 276.97
0 -1 -31 -2.75 3.39
0 1 31 -0.85 2.64
0 1 32 6.74 4.37
0 -1 -32 11.32 5.73
0 1 33 -3.13 2.84
0 -1 -33 1.29 5.56
0 -1 -34 8.37 4.81
0 1 34 10.28 8.90
0 -1 -35 -2.87 7.05
0 1 35 1.58 8.85
0 -1 -36 129.25 17.60
0 1 36 140.23 22.26
0 -1 -37 -3.19 6.54
0 1 37 3.58 8.89
0 2 1 0.57 1.63
0 2 2 73.53 21.84
0 -2 -3 1.00 3.66
0 2 3 1.59 1.46
0 -2 -4 3437.28 318.85
0 -2 -4 3759.92 316.48
0 -2 -4 3550.20 1058.47
0 -2 -5 -3.05 2.64
0 2 5 -1.21 4.92
0 -2 -5 -3.14 3.17
0 2 6 374.14 111.18
0 2 6 389.52 56.25
0 -2 -6 340.07 111.23
0 -2 -6 395.19 56.29
0 -2 -6 373.99 56.19
0 2 6 406.00 56.22
0 2 7 -0.28 2.52
0 2 7 -0.11 2.19
0 -2 -7 -0.43 1.79
0 -2 -7 -2.62 4.50
0 -2 -7 -0.76 2.70
0 2 7 0.23 3.77
0 -2 -8 1188.78 111.27
0 2 8 1241.32 182.28
0 -2 -8 1164.91 359.98
0 -2 -8 1295.73 182.31
0 2 8 1264.19 182.31
0 2 9 0.28 5.12
0 -2 -9 3.41 2.28
0 -2 -9 4.26 5.28
0 -2 -9 1.41 2.97
0 2 9 -1.54 3.79
0 2 10 1098.38 158.16
0 -2 -10 1046.26 312.25
0 -2 -10 1061.66 158.18
0 -2 -10 1043.49 158.15
0 2 10 1079.28 158.14
0 2 11 2.13 3.25
0 -2 -11 -0.08 2.40
0 2 11 2.27 2.61
0 -2 -11 -3.50 4.62
0 2 12 173.08 20.29
0 -2 -12 153.56 19.06
0 -2 -12 153.75 47.43
0 -2 -12 148.11 24.26
0 2 12 174.46 24.17
0 -2 -13 -0.19 2.96
0 2 13 -1.17 4.85
0 -2 -13 1.70 2.42
0 -2 -13 2.23 4.64
0 2 13 8.64 3.93
0 2 14 725.33 104.15
0 -2 -14 680.86 205.56
0 -2 -14 729.83 104.16
0 -2 -14 670.60 104.11
0 2 14 705.87 104.10
0 -2 -15 1.14 3.04
0 -2 -15 1.06 2.69
0 2 15 -3.20 4.57
0 -2 -15 0.57 3.03
0 2 15 -0.66 3.74
0 2 16 686.70 65.83
0 2 16 649.07 63.91
0 -2 -16 679.41 198.56
0 -2 -16 713.12 100.68
0 -2 -16 680.33 100.60
0 2 16 659.65 198.55
0 2 17 0.94 3.03
0 -2 -17 1.25 2.77
0 -2 -17 -3.25 6.30
0 -2 -17 -3.94 4.46
0 2 17 1.10 2.98
0 2 17 2.33 3.85
0 2 18 669.11 66.95
0 -2 -18 667.30 201.74
0 -2 -18 729.09 102.35
0 -2 -18 598.50 102.16
0 2 18 722.95 201.71
0 2 18 715.69 102.21
0 2 19 0.36 3.25
0 -2 -19 0.11 3.64
0 -2 -19 -2.95 3.07
0 -2 -19 1.57 3.67
0 2 19 0.53 3.17
0 2 19 2.02 3.98
0 -2 -20 962.65 97.23
0 2 20 1051.44 156.53
0 -2 -20 1116.93 308.73
0 -2 -20 939.84 156.42
0 2 20 1061.94 308.68
0 2 20 1157.73 156.48
0 2 21 -1.41 2.87
0 2 21 1.97 5.26
0 -2 -21 0.25 4.15
0 -2 -21 3.13 5.64
0 -2 -21 6.07 4.26
0 2 21 -1.24 3.72
0 2 22 0.13 3.51
0 -2 -22 1.57 4.40
0 -2 -22 -3.08 5.69
0 -2 -22 1.64 4.59
0 2 22 1.03 3.42
0 2 22 2.42 4.20
0 -2 -23 1.69 3.36
0 -2 -23 -0.22 3.11
0 2 23 -2.75 7.28
0 -2 -23 -3.72 5.64
0 2 23 -3.00 3.74
0 2 23 -3.84 4.36
0 2 24 76.93 10.64
0 2 24 58.98 11.70
0 -2 -24 59.62 21.03
0 -2 -24 85.47 11.84
0 -2 -24 48.56 11.31
0 -2 -25 -2.06 4.58
0 -2 -25 6.35 5.99
0 2 25 0.76 4.78
0 -2 -26 -0.49 3.81
0 2 26 0.86 5.25
0 -2 -27 7.13 6.00
0 2 27 -0.09 4.62
0 -2 -28 17.60 6.63
0 2 28 27.17 5.85
0 2 29 1.81 3.47
0 -2 -29 4.88 5.94
0 2 30 54.73 9.70
0 -2 -30 61.66 10.60
0 -2 -31 5.96 6.10
0 2 31 1.26 4.70
0 -2 -32 171.14 23.77
0 2 32 136.00 23.31
0 -2 -33 -1.42 6.33
0 2 33 -0.91 6.18
0 -2 -34 59.87 11.83
0 2 34 72.13 11.93
0 -2 -35 2.87 8.06
0 2 35 0.83 6.24
0 -2 -36 8.89 8.07
0 2 36 0.95 6.27
0 -2 -37 2.78 7.35
0 2 37 1.63 5.76
0 3 1 -0.10 2.00
0 3 2 519.22 152.48
0 3 3 -2.21 1.79
0 -3 -4 3275.69 486.76
0 -3 -5 8.93 5.41
0 -3 -5 0.92 3.24
0 -3 -6 4612.39 406.82
0 -3 -6 4682.29 1359.15
0 -3 -6 4612.16 688.83
0 3 7 -0.57 1.74
0 -3 -7 2.19 1.85
0 -3 -7 5.90 5.30
0 -3 -7 2.02 2.95
0 3 8 194.36 29.25
0 -3 -8 199.30 28.80
0 -3 -8 184.43 28.56
0 -3 -9 -2.03 2.35
0 3 9 4.09 7.18
0 -3 -9 -4.06 1.87
0 -3 -9 3.21 4.97
0 -3 -10 793.81 84.38
0 -3 -10 770.75 82.99
0 3 10 1047.94 133.70
0 -3 -10 945.55 263.74
0 3 10 978.83 133.57
0 3 11 4.00 5.37
0 -3 -11 1.10 2.28
0 -3 -11 -0.16 4.88
0 -3 -11 -0.66 2.79
0 3 11 2.97 3.47
0 3 12 727.68 74.91
0 -3 -12 760.09 225.96
0 -3 -12 766.48 114.52
0 -3 -12 756.56 114.45
0 3 12 812.36 114.45
0 3 13 2.61 3.21
0 -3 -13 1.19 3.58
0 3 13 -3.34 2.55
0 -3 -13 -5.79 2.63
0 -3 -13 1.63 4.15
0 3 14 589.28 56.30
0 -3 -14 556.65 163.16
0 -3 -14 554.61 82.71
0 -3 -14 505.80 82.60
0 3 14 583.83 82.65
0 3 15 3.18 3.93
0 -3 -15 -1.44 3.48
0 -3 -15 -3.98 5.04
0 -3 -15 3.49 4.08
0 3 15 -0.17 4.35
0 3 16 255.68 28.56
0 3 16 304.65 40.76
0 -3 -16 251.91 79.72
0 -3 -16 298.50 40.60
0 -3 -16 261.85 40.44
0 3 17 -2.35 4.05
0 -3 -17 5.39 3.36
0 -3 -17 2.58 4.11
0 -3 -17 3.52 4.55
0 3 17 -2.37 3.21
0 3 17 -2.12 4.49
0 3 18 56.63 9.54
0 -3 -18 43.52 14.75
0 -3 -18 58.02 9.03
0 -3 -18 45.41 8.61
0 3 18 44.98 14.83
0 3 18 45.94 8.47
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0 -3 -19 -2.08 3.08
0 -3 -19 3.10 5.39
0 -3 -19 0.25 4.56
0 3 19 4.29 3.35
0 3 19 -0.62 4.66
0 3 20 581.86 90.34
0 -3 -20 568.31 177.85
0 -3 -20 735.70 90.39
0 -3 -20 551.81 90.17
0 3 20 572.27 177.82
0 3 20 615.68 90.16
0 -3 -21 2.07 3.03
0 3 21 0.26 3.28
0 3 21 10.99 9.33
0 -3 -21 0.43 4.30
0 -3 -21 -0.29 7.04
0 3 21 2.70 3.96
0 -3 -22 114.89 18.55
0 3 22 154.55 17.79
0 3 22 140.49 24.00
0 -3 -22 137.15 43.64
0 -3 -22 191.21 23.06
0 3 22 138.01 43.54
0 -3 -23 -0.88 4.26
0 -3 -23 2.15 4.15
0 3 23 6.48 10.19
0 -3 -23 0.90 3.95
0 3 23 3.71 3.51
0 -3 -24 49.97 8.78
0 -3 -24 30.19 13.15
0 3 24 39.60 7.87
0 -3 -25 -2.09 4.11
0 -3 -25 3.28 6.83
0 3 25 0.07 5.03
0 -3 -26 71.55 12.45
0 3 26 61.37 10.49
0 -3 -27 2.31 7.63
0 3 27 -3.43 5.13
0 -3 -28 74.68 12.01
0 3 28 69.93 12.01
0 -3 -29 1.64 6.27
0 3 29 5.00 5.83
0 -3 -30 1506.62 212.22
0 3 30 1362.80 212.13
0 -3 -31 1.57 3.75
0 3 31 -3.10 6.38
0 3 32 280.30 30.51
0 -3 -32 291.59 43.14
0 -3 -33 -0.13 6.07
0 3 33 1.83 7.43
0 -3 -34 112.88 19.08
0 3 34 124.57 19.57
0 -3 -35 -4.13 6.55
0 3 35 0.58 7.53
0 -3 -36 162.48 19.26
0 3 36 136.45 18.69
0 4 0 678.36 199.13
0 4 2 119.28 35.29
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11 -1 16 1.70 9.96
-11 -2 0 56.00 25.93
11 -2 0 86.02 23.37
-11 -2 -1 30.10 14.06
11 -2 -1 28.88 13.67
11 -2 1 27.70 10.96
-11 -2 1 16.21 10.84
-11 -2 -2 13.80 11.64
11 -2 -2 10.21 10.73
11 -2 2 -6.61 7.94
-11 -2 2 13.27 7.65
-11 -2 -3 21.43 14.28
11 -2 -3 -3.15 10.00
11 -2 3 7.75 7.91
-11 -2 3 1.31 7.57
-11 -2 -4 16.18 11.78
11 -2 -4 9.79 10.02
11 -2 4 2.04 7.88
-11 -2 4 0.22 7.97
-11 -2 -5 1.40 12.61
11 -2 -5 33.25 12.72
11 -2 5 9.49 8.65
-11 -2 5 7.07 8.83
11 -2 -6 28.93 11.43
11 -2 6 22.83 11.03
-11 -2 6 5.13 11.24
-11 -2 -7 19.64 15.12
11 -2 -7 10.79 10.10
11 -2 7 -7.68 9.43
-11 -2 7 -4.89 7.78
-11 -2 -8 2.26 15.11
11 -2 -8 -12.20 10.78
11 -2 8 -5.19 9.20
-11 -2 8 -3.43 7.59
-11 -2 -9 12.52 12.84
11 -2 -9 8.92 11.75
11 -2 9 25.54 10.50
-11 -2 9 7.09 8.67
-11 -2 -10 10.80 12.29
11 -2 -10 15.10 12.19
11 -2 10 5.06 10.67
-11 -2 10 25.91 9.21
11 -2 -11 5.47 11.56
11 -2 11 0.33 8.32
-11 -2 11 1.18 8.14
11 -2 -12 4.15 12.57
11 -2 12 17.63 9.01
-11 -2 12 11.84 11.48
11 -2 -13 14.46 12.38
11 -2 13 3.41 8.44
-11 -2 13 0.30 10.18
11 -2 -14 12.55 12.09
11 -2 14 -1.96 8.99
-11 -2 14 3.58 10.18
11 -2 15 -0.38 9.55
11 -2 16 -7.99 10.07
-11 -3 0 34.31 18.37
11 -3 0 44.53 14.30
-11 -3 -1 13.45 14.43
11 -3 -1 13.58 11.33
11 -3 1 11.91 9.98
-11 -3 1 19.03 8.86
-11 -3 -2 13.66 13.61
11 -3 -2 44.37 14.09
11 -3 2 13.03 9.88
-11 -3 2 8.47 9.82
-11 -3 -3 -2.38 13.73
11 -3 -3 12.84 11.84
11 -3 3 27.40 9.20
-11 -3 3 20.18 9.32
-11 -3 -4 -9.03 12.94
11 -3 -4 5.31 11.33
11 -3 4 9.67 7.62
-11 -3 4 -0.62 9.68
-11 -3 -5 14.57 16.08
11 -3 -5 5.32 14.12
11 -3 5 9.22 8.26
-11 -3 5 8.01 8.43
-11 -3 -6 -10.96 15.84
11 -3 -6 4.05 11.46
11 -3 6 -2.46 7.54
-11 -3 6 -0.04 7.70
11 -3 -7 0.79 11.66
11 -3 7 7.22 9.62
-11 -3 7 12.64 7.95
11 -3 -8 27.06 13.10
11 -3 8 7.82 11.98
-11 -3 8 15.43 9.23
11 -3 -9 16.75 14.90
11 -3 9 13.23 11.46
-11 -3 9 1.41 10.16
11 -3 -10 25.44 16.02
11 -3 10 23.68 12.73
-11 -3 10 15.16 14.86
11 -3 -11 0.01 12.40
11 -3 11 0.95 8.41
-11 -3 11 7.76 10.93
11 -3 -12 3.70 12.27
11 -3 12 1.82 8.60
-11 -3 12 5.86 11.02
11 -3 13 -3.74 8.49
-11 -3 13 -2.19 11.25
11 -3 14 -4.54 8.62
11 -4 0 9.23 8.28
11 -4 1 23.28 10.12
-11 -4 1 17.30 10.34
11 -4 2 19.71 10.11
-11 -4 2 20.23 10.26
11 -4 3 17.17 10.44
-11 -4 3 7.41 8.90
11 -4 4 1.60 10.20
-11 -4 4 19.78 8.75
11 -4 5 12.96 9.75
-11 -4 5 -3.50 7.98
11 -4 6 10.15 9.84
-11 -4 6 -1.83 7.87
11 -4 7 16.42 11.27
-11 -4 7 12.12 8.87
11 -4 8 48.93 16.78
-11 -4 8 32.61 15.68
11 -4 9 25.74 15.27
-11 -4 9 40.23 15.24
11 -4 10 25.87 12.78
-11 -4 10 13.11 12.69
11 -4 11 2.50 10.14
-11 -4 11 -7.57 11.13
11 -4 12 -12.20 8.95
-11 -4 12 0.37 11.17
11 -5 0 -0.96 7.96
11 -5 1 11.59 8.57
-11 -5 1 7.28 8.84
11 -5 2 -2.47 8.07
-11 -5 2 4.28 8.32
11 -5 3 12.07 9.87
-11 -5 3 11.50 9.20
11 -5 4 7.36 10.16
-11 -5 4 4.93 8.48
11 -5 5 15.76 10.99
-11 -5 5 12.69 9.36
11 -5 6 8.88 11.28
-11 -5 6 21.77 9.49
11 -5 7 2.70 10.85
-11 -5 7 1.47 7.79
11 -5 8 -4.74 11.44
-11 -5 8 -5.79 9.68
-12 0 0 73.10 26.97
-12 0 -1 7.34 11.93
12 0 -1 -8.84 12.72
-12 0 -2 125.86 50.51
12 0 -2 200.32 50.64
-12 0 -3 17.52 14.51
12 0 -3 32.13 14.88
12 0 -4 -2.54 12.55
12 0 -5 112.93 36.01
12 0 -6 8.06 9.48
12 -1 0 9.79 10.36
12 -1 1 -7.76 9.98
-12 -1 1 -4.45 10.28
12 -1 2 17.42 11.51
-12 -1 2 9.67 11.23
12 -1 3 15.58 12.40
-12 -1 3 19.32 12.84
12 -1 4 9.95 11.82
-12 -1 4 14.15 11.77
12 -1 5 -11.12 11.64
12 -1 6 0.81 11.29
12 -2 0 91.48 29.41
12 -2 1 10.06 10.10
-12 -2 1 -1.57 10.42
12 -2 2 11.53 11.07
-12 -2 2 17.24 10.58
12 -2 3 -2.77 10.74
-12 -2 3 4.58 8.28
12 -2 4 0.71 11.38
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 3496
_shelx_res_file
;
TITL 2316 in Pca2(1)
CELL 0.9699 9.5892 10.1448 30.0797 90 90 90
ZERR 8 0.0019 0.002 0.006 0 0 0
LATT -1
SYMM -X,-Y,0.5+Z
SYMM 0.5+X,-Y,+Z
SYMM 0.5-X,+Y,0.5+Z
SFAC C H O
DISP C 0.008 0.003 25.571
DISP H -0 0 0.636
DISP O 0.023 0.012 81.964
UNIT 160 128 16
L.S. 10
PLAN 20
SIZE 0.015 0.03 0.4
TEMP -173.15
BOND $H
CONF
fmap 2
acta
OMIT 8 7 -12
OMIT 6 9 -18
OMIT 8 0 25
OMIT 5 9 -21
OMIT 0 10 -16
OMIT 0 10 14
OMIT 8 7 12
OMIT 8 5 -21
OMIT 8 9 5
OMIT 4 10 14
OMIT 6 8 -21
OMIT 8 9 6
OMIT 8 9 1
OMIT 8 2 -27
OMIT 6 10 5
OMIT 1 3 -2
OMIT 1 2 1
OMIT 8 3 -25
OMIT 8 0 27
OMIT 8 6 -18
OMIT 8 5 -15
OMIT 8 5 21
OMIT 1 1 -2
OMIT 3 1 6
OMIT 5 9 21
OMIT 0 10 20
OMIT 3 2 8
OMIT 3 2 -8
OMIT 2 0 25
OMIT 6 10 11
OMIT 3 2 -7
OMIT 1 2 -10
OMIT 1 1 1
OMIT 3 2 -6
OMIT 3 2 7
OMIT 1 1 2
OMIT 0 10 18
OMIT 7 9 5
OMIT 1 1 -3
OMIT 1 2 7
OMIT 8 6 18
OMIT 3 2 5
OMIT 1 2 -7
OMIT 1 1 12
OMIT 1 1 -1
OMIT 1 1 -12
OMIT 4 10 11
OMIT 3 11 6
OMIT 3 1 -6
OMIT 8 6 -19
OMIT 5 10 11
OMIT 1 1 3
OMIT 4 10 16
OMIT 0 11 -14
OMIT 4 10 -8
OMIT 1 2 10
OMIT 8 1 -25
OMIT 1 2 -11
OMIT 3 2 -9
OMIT 1 3 -4
OMIT 3 2 3
OMIT 6 10 8
OMIT 4 7 -21
OMIT 1 3 2
OMIT 7 5 -27
OMIT 1 11 15
OMIT 3 2 -2
OMIT 2 11 11
OMIT 8 2 27
OMIT 1 2 4
OMIT 2 0 -16
OMIT 1 3 1
OMIT 6 10 9
OMIT 2 7 -20
OMIT 1 1 0
OMIT 1 5 -3
OMIT 3 2 -3
OMIT 3 2 0
OMIT 3 2 2
OMIT 1 2 11
OMIT 3 2 9
OMIT 5 10 4
OMIT 2 0 16
OMIT 3 2 -5
OMIT 1 1 -11
OMIT 6 7 -9
OMIT 3 1 7
OMIT 1 1 11
OMIT 8 1 -11
OMIT 3 1 2
OMIT 7 9 -1
OMIT 0 10 -24
OMIT 1 3 -11
OMIT 1 2 -4
OMIT 3 2 6
OMIT 3 1 -2
OMIT 1 2 -12
OMIT 1 1 13
OMIT 1 3 -3
OMIT 1 1 8
OMIT 1 1 -8
OMIT 8 0 14
OMIT 3 3 2
REM
REM
REM
WGHT 0.010000 9.000000
FVAR 0.51246
O1 3 0.377314 1.196196 0.604354 11.00000 0.03027 0.01624 =
0.02403 0.00001 0.00415 -0.00368
O2 3 0.623137 1.107443 0.467279 11.00000 0.06008 0.01522 =
0.02114 -0.00036 0.01350 -0.00174
C1 1 0.477349 1.069077 0.529055 11.00000 0.02694 0.02256 =
0.02728 0.00323 0.00345 0.00238
AFIX 43
H1 2 0.494258 1.159551 0.535166 11.00000 -1.20000
AFIX 0
C2 1 0.403742 1.001705 0.558234 11.00000 0.02229 0.01567 =
0.00985 0.00196 0.00441 0.00137
C3 1 0.348648 1.077165 0.599063 11.00000 0.03480 0.02059 =
0.02864 0.00546 -0.00171 0.00142
C4 1 0.256086 1.007520 0.630640 11.00000 0.01524 0.01104 =
0.02459 0.00017 -0.00079 -0.00372
C5 1 0.185172 1.085748 0.660945 11.00000 0.03014 0.03044 =
0.02534 0.00557 -0.00103 -0.00335
AFIX 43
H5 2 0.204211 1.177575 0.659728 11.00000 -1.20000
AFIX 0
C6 1 0.086953 1.044426 0.693741 11.00000 0.03598 0.03080 =
0.03032 -0.00398 -0.00587 -0.00251
C7 1 -0.000881 1.019970 0.721067 11.00000 0.02331 0.03026 =
0.01991 0.00719 0.00585 0.00348
C8 1 0.373246 0.855473 0.557071 11.00000 0.03655 0.01900 =
0.03419 0.00100 0.00475 -0.00233
AFIX 23
H8A 2 0.449216 0.809608 0.541027 11.00000 -1.20000
H8B 2 0.285399 0.840163 0.540570 11.00000 -1.20000
AFIX 0
C9 1 0.359868 0.797564 0.603985 11.00000 0.02335 0.01498 =
0.01458 -0.00204 0.00154 0.00193
AFIX 23
H9A 2 0.445891 0.815402 0.621160 11.00000 -1.20000
H9B 2 0.346861 0.700898 0.602213 11.00000 -1.20000
AFIX 0
C10 1 0.231223 0.862385 0.627760 11.00000 0.03362 0.02823 =
0.02593 0.00239 0.00348 0.00164
AFIX 23
H10A 2 0.145056 0.844623 0.610649 11.00000 -1.20000
H10B 2 0.219934 0.824916 0.657937 11.00000 -1.20000
AFIX 0
C11 1 0.533948 1.015595 0.488630 11.00000 0.00973 0.03049 =
0.00575 -0.00045 0.00122 -0.00074
C12 1 0.524443 0.911020 0.461975 11.00000 0.08125 0.01668 =
0.01881 -0.00648 0.01526 -0.02054
AFIX 43
H12 2 0.471167 0.833869 0.467628 11.00000 -1.20000
AFIX 0
C13 1 0.608367 0.934758 0.423278 11.00000 0.08724 0.03026 =
0.02151 0.00037 0.01768 0.01727
AFIX 43
H13 2 0.619583 0.876932 0.398695 11.00000 -1.20000
AFIX 0
C14 1 0.665878 1.049098 0.427971 11.00000 0.03216 0.03586 =
0.01681 0.00171 0.00277 0.00693
AFIX 43
H14 2 0.728727 1.087736 0.407326 11.00000 -1.20000
AFIX 0
C15 1 -0.102831 1.008276 0.757075 11.00000 0.00927 0.02780 =
0.01564 -0.00195 0.00158 -0.00219
C16 1 -0.155672 0.887379 0.771206 11.00000 0.03198 0.02033 =
0.01710 -0.01067 -0.00935 0.00710
AFIX 43
H16 2 -0.121357 0.808120 0.758429 11.00000 -1.20000
AFIX 0
C17 1 -0.260558 0.881600 0.804598 11.00000 0.02837 0.02564 =
0.01540 0.00134 -0.00293 -0.00748
AFIX 43
H17 2 -0.296020 0.798795 0.814070 11.00000 -1.20000
AFIX 0
C18 1 -0.310763 0.996829 0.823234 11.00000 0.02065 0.03424 =
0.01374 0.00273 -0.00231 0.00170
AFIX 43
H18 2 -0.380847 0.992794 0.845515 11.00000 -1.20000
AFIX 0
C19 1 -0.259288 1.119099 0.809572 11.00000 0.02585 0.03076 =
0.00968 -0.00189 0.00162 0.00658
AFIX 43
H19 2 -0.293865 1.198176 0.822405 11.00000 -1.20000
AFIX 0
C20 1 -0.156481 1.123465 0.776846 11.00000 0.02771 0.02234 =
0.01580 0.00325 -0.00657 -0.00566
AFIX 43
H20 2 -0.121526 1.206681 0.767594 11.00000 -1.20000
AFIX 0
O1A 3 0.379598 0.695505 0.398054 11.00000 0.04939 0.02164 =
0.02360 0.00658 0.00547 0.00790
O2A 3 0.124233 0.609437 0.534721 11.00000 0.03323 0.02757 =
0.03356 0.00447 0.00318 0.00575
C1A 1 0.275878 0.568406 0.472443 11.00000 0.03389 0.03021 =
0.02639 0.00345 -0.00534 0.00737
AFIX 43
H1A 2 0.262920 0.659674 0.466706 11.00000 -1.20000
AFIX 0
C2A 1 0.348532 0.499703 0.440072 11.00000 0.01248 0.01700 =
0.01748 0.00104 -0.00946 -0.00074
C3A 1 0.405822 0.574759 0.403272 11.00000 0.03486 0.02712 =
0.02257 -0.00078 -0.00333 -0.00361
C4A 1 0.503963 0.503347 0.371333 11.00000 0.01557 0.02726 =
0.00917 -0.00169 -0.00557 -0.00084
C5A 1 0.564271 0.580410 0.340166 11.00000 0.03115 0.02489 =
0.02616 0.00105 0.00129 0.00568
AFIX 43
H5A 2 0.540132 0.671185 0.339189 11.00000 -1.20000
AFIX 0
C6A 1 0.663412 0.531037 0.308402 11.00000 0.02630 0.04868 =
0.01225 -0.00240 0.00162 -0.00574
C7A 1 0.748426 0.507455 0.278645 11.00000 0.01984 0.02837 =
0.01254 0.00223 -0.00789 -0.00193
C8A 1 0.375591 0.352963 0.445135 11.00000 0.04081 0.01984 =
0.02368 0.00033 0.00195 -0.00021
AFIX 23
H8AA 2 0.459149 0.338513 0.463841 11.00000 -1.20000
H8AB 2 0.294961 0.310235 0.459793 11.00000 -1.20000
AFIX 0
C9A 1 0.398109 0.293501 0.399556 11.00000 0.02764 0.01562 =
0.01786 -0.00636 0.00039 -0.00309
AFIX 23
H9AA 2 0.312776 0.305537 0.381481 11.00000 -1.20000
H9AB 2 0.415089 0.197674 0.402624 11.00000 -1.20000
AFIX 0
C10A 1 0.521791 0.357096 0.375635 11.00000 0.04094 0.02359 =
0.03494 -0.00634 0.00299 0.00182
AFIX 23
H10C 2 0.608436 0.338300 0.392371 11.00000 -1.20000
H10D 2 0.531323 0.317822 0.345659 11.00000 -1.20000
AFIX 0
C11A 1 0.215219 0.519689 0.514922 11.00000 0.02925 0.02903 =
0.02934 -0.00229 0.00182 0.00738
C12A 1 0.233356 0.412146 0.539831 11.00000 0.02530 0.03116 =
0.03883 -0.00612 0.00258 -0.00120
AFIX 43
H12A 2 0.291522 0.338511 0.533758 11.00000 -1.20000
AFIX 0
C13A 1 0.143522 0.432954 0.578654 11.00000 0.03700 0.01676 =
0.02101 0.00703 0.00555 -0.00094
AFIX 43
H13A 2 0.124708 0.372312 0.601960 11.00000 -1.20000
AFIX 0
C14A 1 0.093417 0.556084 0.574270 11.00000 0.08665 0.01870 =
0.01935 0.00584 0.02037 0.02147
AFIX 43
H14A 2 0.041868 0.600349 0.596732 11.00000 -1.20000
AFIX 0
C15A 1 0.855002 0.497979 0.246207 11.00000 0.02547 0.02072 =
0.01480 0.00001 -0.00363 -0.00130
C16A 1 0.897379 0.372981 0.229020 11.00000 0.02378 0.01642 =
0.02289 0.00416 0.00879 0.00525
AFIX 43
H16A 2 0.857282 0.293784 0.240004 11.00000 -1.20000
AFIX 0
C17A 1 0.996464 0.369554 0.196553 11.00000 0.02451 0.01804 =
0.02640 -0.00010 0.00613 0.00373
AFIX 43
H17A 2 1.024176 0.286983 0.184557 11.00000 -1.20000
AFIX 0
C18A 1 1.058283 0.485257 0.180509 11.00000 0.02764 0.03612 =
0.01530 0.00219 0.00388 -0.00061
AFIX 43
H18A 2 1.128788 0.480996 0.158368 11.00000 -1.20000
AFIX 0
C19A 1 1.015757 0.605705 0.197188 11.00000 0.03677 0.02450 =
0.02713 0.00792 0.00461 -0.00937
AFIX 43
H19A 2 1.057755 0.684410 0.186529 11.00000 -1.20000
AFIX 0
C20A 1 0.912139 0.612722 0.229403 11.00000 0.02474 0.02001 =
0.02439 0.00057 0.00592 -0.00745
AFIX 43
H20A 2 0.880724 0.695982 0.239826 11.00000 -1.20000
AFIX 0
HKLF 4
REM 2316 in Pca2(1)
REM R1 = 0.0948 for 3732 Fo > 4sig(Fo) and 0.1374 for all 5675 data
REM 397 parameters refined using 1 restraints
END
WGHT 0.1365 1.5765
REM Highest difference peak 1.077, deepest hole -0.510, 1-sigma level 0.097
Q1 1 0.6271 0.8908 0.4686 11.00000 0.05 1.08
Q2 1 0.1201 0.3958 0.5345 11.00000 0.05 1.02
Q3 1 0.4761 0.9317 0.5300 11.00000 0.05 1.02
Q4 1 0.4082 0.4273 0.4039 11.00000 0.05 0.91
Q5 1 0.5661 0.4209 0.3418 11.00000 0.05 0.89
Q6 1 0.3435 0.9299 0.5995 11.00000 0.05 0.88
Q7 1 0.2313 1.1365 0.6277 11.00000 0.05 0.87
Q8 1 0.3729 0.6454 0.4471 11.00000 0.05 0.87
Q9 1 0.2365 0.5829 0.5419 11.00000 0.05 0.85
Q10 1 0.2767 0.4309 0.4717 11.00000 0.05 0.85
Q11 1 0.3796 1.1490 0.5557 11.00000 0.05 0.78
Q12 1 0.1848 0.9215 0.6595 11.00000 0.05 0.74
Q13 1 0.5211 0.6402 0.3765 11.00000 0.05 0.72
Q14 1 0.5162 1.0836 0.4611 11.00000 0.05 0.65
Q15 1 0.6576 0.4480 0.3094 11.00000 0.05 0.65
Q16 1 0.0898 0.9484 0.6937 11.00000 0.05 0.64
Q17 1 0.6908 0.9415 0.4284 11.00000 0.05 0.39
Q18 1 0.0739 0.4433 0.5737 11.00000 0.05 0.38
Q19 1 0.1520 0.5751 0.5792 11.00000 0.05 0.36
Q20 1 0.5958 1.0675 0.4222 11.00000 0.05 0.33
;
_shelx_res_checksum 33649
_shelxl_version_number 2.014
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.3773(6) 1.1962(6) 0.60435(19) 0.0235(13) Uani d 1 . .
O O2 0.6231(7) 1.1074(5) 0.46728(17) 0.0321(14) Uani d 1 . .
C C1 0.4773(8) 1.0691(8) 0.5291(3) 0.0256(17) Uani d 1 . .
H H1 0.4943 1.1596 0.5352 0.031 Uiso calc 1 . .
C C2 0.4037(10) 1.0017(6) 0.5582(3) 0.016(2) Uani d 1 . .
C C3 0.3486(9) 1.0772(8) 0.5991(3) 0.0280(18) Uani d 1 . .
C C4 0.2561(10) 1.0075(7) 0.6306(3) 0.0170(19) Uani d 1 . .
C C5 0.1852(9) 1.0857(9) 0.6609(3) 0.0286(18) Uani d 1 . .
H H5 0.2042 1.1776 0.6597 0.034 Uiso calc 1 . .
C C6 0.0870(10) 1.0444(10) 0.6937(3) 0.0324(19) Uani d 1 . .
C C7 -0.0009(10) 1.0200(9) 0.7211(3) 0.024(2) Uani d 1 . .
C C8 0.3732(9) 0.8555(8) 0.5571(3) 0.0299(19) Uani d 1 . .
H H8A 0.4492 0.8096 0.5410 0.036 Uiso calc 1 . .
H H8B 0.2854 0.8402 0.5406 0.036 Uiso calc 1 . .
C C9 0.3599(8) 0.7976(9) 0.6040(3) 0.0176(17) Uani d 1 . .
H H9A 0.4459 0.8154 0.6212 0.021 Uiso calc 1 . .
H H9B 0.3469 0.7009 0.6022 0.021 Uiso calc 1 . .
C C10 0.2312(9) 0.8624(9) 0.6278(3) 0.0293(18) Uani d 1 . .
H H10A 0.1451 0.8446 0.6106 0.035 Uiso calc 1 . .
H H10B 0.2199 0.8249 0.6579 0.035 Uiso calc 1 . .
C C11 0.5339(9) 1.0156(8) 0.4886(2) 0.0153(17) Uani d 1 . .
C C12 0.5244(12) 0.9110(8) 0.4620(3) 0.039(2) Uani d 1 . .
H H12 0.4712 0.8339 0.4676 0.047 Uiso calc 1 . .
C C13 0.6084(13) 0.9348(11) 0.4233(3) 0.046(3) Uani d 1 . .
H H13 0.6196 0.8769 0.3987 0.056 Uiso calc 1 . .
C C14 0.6659(9) 1.0491(10) 0.4280(3) 0.028(2) Uani d 1 . .
H H14 0.7287 1.0877 0.4073 0.034 Uiso calc 1 . .
C C15 -0.1028(9) 1.0083(7) 0.7571(3) 0.018(2) Uani d 1 . .
C C16 -0.1557(9) 0.8874(9) 0.7712(3) 0.023(2) Uani d 1 . .
H H16 -0.1214 0.8081 0.7584 0.028 Uiso calc 1 . .
C C17 -0.2606(9) 0.8816(9) 0.8046(3) 0.0231(19) Uani d 1 . .
H H17 -0.2960 0.7988 0.8141 0.028 Uiso calc 1 . .
C C18 -0.3108(10) 0.9968(8) 0.8232(3) 0.023(2) Uani d 1 . .
H H18 -0.3808 0.9928 0.8455 0.027 Uiso calc 1 . .
C C19 -0.2593(9) 1.1191(9) 0.8096(2) 0.0221(19) Uani d 1 . .
H H19 -0.2939 1.1982 0.8224 0.027 Uiso calc 1 . .
C C20 -0.1565(9) 1.1235(10) 0.7768(3) 0.0219(19) Uani d 1 . .
H H20 -0.1215 1.2067 0.7676 0.026 Uiso calc 1 . .
O O1A 0.3796(7) 0.6955(7) 0.39805(19) 0.0315(15) Uani d 1 . .
O O2A 0.1242(6) 0.6094(6) 0.5347(2) 0.0315(14) Uani d 1 . .
C C1A 0.2759(9) 0.5684(9) 0.4724(3) 0.0302(19) Uani d 1 . .
H H1A 0.2629 0.6597 0.4667 0.036 Uiso calc 1 . .
C C2A 0.3485(9) 0.4997(6) 0.4401(3) 0.016(2) Uani d 1 . .
C C3A 0.4058(9) 0.5748(9) 0.4033(3) 0.0282(18) Uani d 1 . .
C C4A 0.5040(10) 0.5033(7) 0.3713(3) 0.017(2) Uani d 1 . .
C C5A 0.5643(8) 0.5804(9) 0.3402(3) 0.0274(18) Uani d 1 . .
H H5A 0.5401 0.6712 0.3392 0.033 Uiso calc 1 . .
C C6A 0.6634(9) 0.5310(11) 0.3084(3) 0.0291(19) Uani d 1 . .
C C7A 0.7484(11) 0.5075(7) 0.2786(3) 0.0202(19) Uani d 1 . .
C C8A 0.3756(9) 0.3530(8) 0.4451(3) 0.0281(18) Uani d 1 . .
H H8AA 0.4591 0.3385 0.4638 0.034 Uiso calc 1 . .
H H8AB 0.2950 0.3102 0.4598 0.034 Uiso calc 1 . .
C C9A 0.3981(8) 0.2935(9) 0.3996(3) 0.0204(17) Uani d 1 . .
H H9AA 0.3128 0.3055 0.3815 0.024 Uiso calc 1 . .
H H9AB 0.4151 0.1977 0.4026 0.024 Uiso calc 1 . .
C C10A 0.5218(10) 0.3571(9) 0.3756(3) 0.033(2) Uani d 1 . .
H H10C 0.6084 0.3383 0.3924 0.040 Uiso calc 1 . .
H H10D 0.5313 0.3178 0.3457 0.040 Uiso calc 1 . .
C C11A 0.2152(11) 0.5197(9) 0.5149(3) 0.029(2) Uani d 1 . .
C C12A 0.2334(9) 0.4121(9) 0.5398(3) 0.0318(19) Uani d 1 . .
H H12A 0.2915 0.3385 0.5338 0.038 Uiso calc 1 . .
C C13A 0.1435(9) 0.4330(9) 0.5787(3) 0.0249(18) Uani d 1 . .
H H13A 0.1247 0.3723 0.6020 0.030 Uiso calc 1 . .
C C14A 0.0934(12) 0.5561(10) 0.5743(3) 0.042(3) Uani d 1 . .
H H14A 0.0419 0.6003 0.5967 0.050 Uiso calc 1 . .
C C15A 0.8550(10) 0.4980(7) 0.2462(3) 0.020(2) Uani d 1 . .
C C16A 0.8974(9) 0.3730(9) 0.2290(3) 0.0210(19) Uani d 1 . .
H H16A 0.8573 0.2938 0.2400 0.025 Uiso calc 1 . .
C C17A 0.9965(9) 0.3696(9) 0.1966(3) 0.0230(19) Uani d 1 . .
H H17A 1.0242 0.2870 0.1846 0.028 Uiso calc 1 . .
C C18A 1.0583(11) 0.4853(9) 0.1805(3) 0.026(2) Uani d 1 . .
H H18A 1.1288 0.4810 0.1584 0.032 Uiso calc 1 . .
C C19A 1.0158(10) 0.6057(10) 0.1972(3) 0.029(2) Uani d 1 . .
H H19A 1.0578 0.6844 0.1865 0.035 Uiso calc 1 . .
C C20A 0.9121(9) 0.6127(9) 0.2294(3) 0.0230(19) Uani d 1 . .
H H20A 0.8807 0.6960 0.2398 0.028 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 0.030(3) 0.016(3) 0.024(3) -0.004(3) 0.004(2) 0.000(3)
O2 0.060(4) 0.015(3) 0.021(3) -0.002(3) 0.013(3) 0.000(2)
C1 0.027(4) 0.023(4) 0.027(4) 0.002(3) 0.003(3) 0.003(4)
C2 0.022(5) 0.016(5) 0.010(3) 0.001(3) 0.004(3) 0.002(2)
C3 0.035(5) 0.021(4) 0.029(4) 0.001(4) -0.002(3) 0.005(3)
C4 0.015(4) 0.011(4) 0.025(5) -0.004(3) -0.001(3) 0.000(3)
C5 0.030(4) 0.030(5) 0.025(4) -0.003(4) -0.001(3) 0.006(4)
C6 0.036(5) 0.031(5) 0.030(4) -0.003(4) -0.006(4) -0.004(4)
C7 0.023(5) 0.030(5) 0.020(4) 0.003(3) 0.006(4) 0.007(4)
C8 0.037(5) 0.019(4) 0.034(4) -0.002(4) 0.005(4) 0.001(4)
C9 0.023(4) 0.015(4) 0.015(3) 0.002(3) 0.002(3) -0.002(3)
C10 0.034(4) 0.028(5) 0.026(4) 0.002(4) 0.003(3) 0.002(3)
C11 0.010(4) 0.030(4) 0.006(3) -0.001(3) 0.001(3) 0.000(3)
C12 0.081(7) 0.017(4) 0.019(4) -0.021(5) 0.015(4) -0.006(3)
C13 0.087(8) 0.030(6) 0.022(4) 0.017(5) 0.018(5) 0.000(4)
C14 0.032(5) 0.036(6) 0.017(4) 0.007(4) 0.003(3) 0.002(4)
C15 0.009(4) 0.028(5) 0.016(4) -0.002(3) 0.002(3) -0.002(3)
C16 0.032(5) 0.020(5) 0.017(4) 0.007(4) -0.009(3) -0.011(4)
C17 0.028(4) 0.026(5) 0.015(4) -0.007(4) -0.003(3) 0.001(3)
C18 0.021(5) 0.034(6) 0.014(4) 0.002(3) -0.002(4) 0.003(3)
C19 0.026(4) 0.031(5) 0.010(3) 0.007(4) 0.002(3) -0.002(3)
C20 0.028(5) 0.022(5) 0.016(4) -0.006(4) -0.007(3) 0.003(3)
O1A 0.049(4) 0.022(4) 0.024(3) 0.008(3) 0.005(3) 0.007(3)
O2A 0.033(3) 0.028(3) 0.034(3) 0.006(3) 0.003(3) 0.004(3)
C1A 0.034(5) 0.030(5) 0.026(4) 0.007(4) -0.005(3) 0.003(4)
C2A 0.012(4) 0.017(5) 0.017(4) -0.001(3) -0.009(3) 0.001(3)
C3A 0.035(5) 0.027(4) 0.023(4) -0.004(4) -0.003(3) -0.001(3)
C4A 0.016(4) 0.027(5) 0.009(3) -0.001(3) -0.006(3) -0.002(3)
C5A 0.031(5) 0.025(4) 0.026(4) 0.006(4) 0.001(3) 0.001(3)
C6A 0.026(4) 0.049(5) 0.012(4) -0.006(4) 0.002(3) -0.002(4)
C7A 0.020(4) 0.028(5) 0.013(3) -0.002(3) -0.008(3) 0.002(3)
C8A 0.041(5) 0.020(4) 0.024(4) 0.000(4) 0.002(3) 0.000(3)
C9A 0.028(4) 0.016(4) 0.018(4) -0.003(3) 0.000(3) -0.006(3)
C10A 0.041(5) 0.024(5) 0.035(4) 0.002(4) 0.003(4) -0.006(4)
C11A 0.029(5) 0.029(5) 0.029(5) 0.007(4) 0.002(4) -0.002(4)
C12A 0.025(4) 0.031(5) 0.039(4) -0.001(4) 0.003(4) -0.006(4)
C13A 0.037(5) 0.017(4) 0.021(4) -0.001(3) 0.006(3) 0.007(3)
C14A 0.087(8) 0.019(5) 0.019(4) 0.021(5) 0.020(4) 0.006(4)
C15A 0.025(5) 0.021(5) 0.015(4) -0.001(3) -0.004(4) 0.000(3)
C16A 0.024(4) 0.016(4) 0.023(4) 0.005(3) 0.009(3) 0.004(3)
C17A 0.025(4) 0.018(4) 0.026(4) 0.004(3) 0.006(3) 0.000(4)
C18A 0.028(5) 0.036(6) 0.015(4) -0.001(4) 0.004(4) 0.002(3)
C19A 0.037(5) 0.024(5) 0.027(4) -0.009(4) 0.005(4) 0.008(4)
C20A 0.025(4) 0.020(5) 0.024(4) -0.007(4) 0.006(3) 0.001(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0080 0.0030 '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'
O O 0.0230 0.0120 '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
C14 O2 C11 . . 106.5(6)
C2 C1 H1 . . 117.6
C2 C1 C11 . . 124.7(8)
C11 C1 H1 . . 117.6
C1 C2 C3 . . 117.2(7)
C1 C2 C8 . . 126.7(8)
C8 C2 C3 . . 116.1(7)
O1 C3 C2 . . 120.4(7)
O1 C3 C4 . . 120.8(7)
C4 C3 C2 . . 118.7(7)
C3 C4 C10 . . 121.9(8)
C5 C4 C3 . . 116.3(7)
C5 C4 C10 . . 121.6(8)
C4 C5 H5 . . 116.2
C4 C5 C6 . . 127.6(9)
C6 C5 H5 . . 116.2
C7 C6 C5 . . 174.5(11)
C6 C7 C15 . . 171.9(10)
C2 C8 H8A . . 109.3
C2 C8 H8B . . 109.3
C2 C8 C9 . . 111.7(7)
H8A C8 H8B . . 107.9
C9 C8 H8A . . 109.3
C9 C8 H8B . . 109.3
C8 C9 H9A . . 109.9
C8 C9 H9B . . 109.9
C8 C9 C10 . . 108.9(7)
H9A C9 H9B . . 108.3
C10 C9 H9A . . 109.9
C10 C9 H9B . . 109.9
C4 C10 C9 . . 108.3(7)
C4 C10 H10A . . 110.0
C4 C10 H10B . . 110.0
C9 C10 H10A . . 110.0
C9 C10 H10B . . 110.0
H10A C10 H10B . . 108.4
O2 C11 C1 . . 111.3(7)
C12 C11 O2 . . 107.0(7)
C12 C11 C1 . . 141.6(8)
C11 C12 H12 . . 125.8
C11 C12 C13 . . 108.4(8)
C13 C12 H12 . . 125.8
C12 C13 H13 . . 126.2
C14 C13 C12 . . 107.5(8)
C14 C13 H13 . . 126.2
O2 C14 H14 . . 124.7
C13 C14 O2 . . 110.5(8)
C13 C14 H14 . . 124.7
C16 C15 C7 . . 122.7(8)
C16 C15 C20 . . 117.9(9)
C20 C15 C7 . . 119.3(7)
C15 C16 H16 . . 119.7
C15 C16 C17 . . 120.6(8)
C17 C16 H16 . . 119.7
C16 C17 H17 . . 120.1
C18 C17 C16 . . 119.8(9)
C18 C17 H17 . . 120.1
C17 C18 H18 . . 119.7
C17 C18 C19 . . 120.6(9)
C19 C18 H18 . . 119.7
C18 C19 H19 . . 120.5
C20 C19 C18 . . 119.1(9)
C20 C19 H19 . . 120.5
C15 C20 H20 . . 119.0
C19 C20 C15 . . 122.0(9)
C19 C20 H20 . . 119.0
C14A O2A C11A . . 104.7(7)
C2A C1A H1A . . 115.4
C2A C1A C11A . . 129.3(8)
C11A C1A H1A . . 115.4
C1A C2A C3A . . 117.5(7)
C1A C2A C8A . . 120.6(8)
C3A C2A C8A . . 121.7(8)
O1A C3A C2A . . 122.0(8)
O1A C3A C4A . . 120.4(7)
C2A C3A C4A . . 117.6(7)
C5A C4A C3A . . 115.2(7)
C5A C4A C10A . . 125.7(8)
C10A C4A C3A . . 119.0(8)
C4A C5A H5A . . 118.6
C4A C5A C6A . . 122.9(8)
C6A C5A H5A . . 118.6
C7A C6A C5A . . 170.5(10)
C6A C7A C15A . . 171.7(9)
C2A C8A H8AA . . 109.9
C2A C8A H8AB . . 109.9
H8AA C8A H8AB . . 108.3
C9A C8A C2A . . 108.9(7)
C9A C8A H8AA . . 109.9
C9A C8A H8AB . . 109.9
C8A C9A H9AA . . 109.3
C8A C9A H9AB . . 109.3
C8A C9A C10A . . 111.6(7)
H9AA C9A H9AB . . 108.0
C10A C9A H9AA . . 109.3
C10A C9A H9AB . . 109.3
C4A C10A C9A . . 111.7(7)
C4A C10A H10C . . 109.3
C4A C10A H10D . . 109.3
C9A C10A H10C . . 109.3
C9A C10A H10D . . 109.3
H10C C10A H10D . . 107.9
O2A C11A C1A . . 113.2(8)
C12A C11A O2A . . 112.0(9)
C12A C11A C1A . . 134.6(9)
C11A C12A H12A . . 127.7
C11A C12A C13A . . 104.6(8)
C13A C12A H12A . . 127.7
C12A C13A H13A . . 127.3
C14A C13A C12A . . 105.4(7)
C14A C13A H13A . . 127.3
O2A C14A C13A . . 112.5(7)
O2A C14A H14A . . 123.7
C13A C14A H14A . . 123.7
C7A C15A C16A . . 121.0(7)
C20A C15A C7A . . 118.7(7)
C20A C15A C16A . . 120.2(9)
C15A C16A H16A . . 120.6
C17A C16A C15A . . 118.7(9)
C17A C16A H16A . . 120.6
C16A C17A H17A . . 119.3
C16A C17A C18A . . 121.4(9)
C18A C17A H17A . . 119.3
C17A C18A H18A . . 120.3
C19A C18A C17A . . 119.4(9)
C19A C18A H18A . . 120.3
C18A C19A H19A . . 119.7
C18A C19A C20A . . 120.6(9)
C20A C19A H19A . . 119.7
C15A C20A C19A . . 119.7(9)
C15A C20A H20A . . 120.2
C19A C20A H20A . . 120.2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
O1 C3 . 1.249(10)
O2 C11 . 1.418(10)
O2 C14 . 1.384(9)
C1 H1 . 0.9500
C1 C2 . 1.317(11)
C1 C11 . 1.438(11)
C2 C3 . 1.541(12)
C2 C8 . 1.512(10)
C3 C4 . 1.480(12)
C4 C5 . 1.387(12)
C4 C10 . 1.494(11)
C5 H5 . 0.9500
C5 C6 . 1.427(12)
C6 C7 . 1.203(13)
C7 C15 . 1.464(13)
C8 H8A . 0.9900
C8 H8B . 0.9900
C8 C9 . 1.534(12)
C9 H9A . 0.9900
C9 H9B . 0.9900
C9 C10 . 1.570(11)
C10 H10A . 0.9900
C10 H10B . 0.9900
C11 C12 . 1.333(11)
C12 H12 . 0.9500
C12 C13 . 1.435(12)
C13 H13 . 0.9500
C13 C14 . 1.292(16)
C14 H14 . 0.9500
C15 C16 . 1.393(12)
C15 C20 . 1.409(13)
C16 H16 . 0.9500
C16 C17 . 1.423(12)
C17 H17 . 0.9500
C17 C18 . 1.383(12)
C18 H18 . 0.9500
C18 C19 . 1.397(12)
C19 H19 . 0.9500
C19 C20 . 1.394(12)
C20 H20 . 0.9500
O1A C3A . 1.260(11)
O2A C11A . 1.395(11)
O2A C14A . 1.340(10)
C1A H1A . 0.9500
C1A C2A . 1.385(12)
C1A C11A . 1.488(13)
C2A C3A . 1.452(12)
C2A C8A . 1.519(10)
C3A C4A . 1.528(12)
C4A C5A . 1.351(12)
C4A C10A . 1.499(11)
C5A H5A . 0.9500
C5A C6A . 1.438(12)
C6A C7A . 1.234(13)
C7A C15A . 1.416(14)
C8A H8AA . 0.9900
C8A H8AB . 0.9900
C8A C9A . 1.513(11)
C9A H9AA . 0.9900
C9A H9AB . 0.9900
C9A C10A . 1.530(12)
C10A H10C . 0.9900
C10A H10D . 0.9900
C11A C12A . 1.335(13)
C12A H12A . 0.9500
C12A C13A . 1.466(11)
C13A H13A . 0.9500
C13A C14A . 1.345(14)
C14A H14A . 0.9500
C15A C16A . 1.428(12)
C15A C20A . 1.382(12)
C16A H16A . 0.9500
C16A C17A . 1.363(11)
C17A H17A . 0.9500
C17A C18A . 1.401(13)
C18A H18A . 0.9500
C18A C19A . 1.382(14)
C19A H19A . 0.9500
C19A C20A . 1.390(12)
C20A H20A . 0.9500
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
O1 C3 C4 C5 . . . . 11.0(13)
O1 C3 C4 C10 . . . . -173.8(8)
O2 C11 C12 C13 . . . . 0.3(11)
C1 C2 C3 O1 . . . . -2.1(13)
C1 C2 C3 C4 . . . . 175.1(8)
C1 C2 C8 C9 . . . . 148.5(9)
C1 C11 C12 C13 . . . . 173.9(11)
C2 C1 C11 O2 . . . . -172.2(8)
C2 C1 C11 C12 . . . . 14.3(19)
C2 C3 C4 C5 . . . . -166.2(8)
C2 C3 C4 C10 . . . . 9.0(13)
C2 C8 C9 C10 . . . . 63.7(9)
C3 C2 C8 C9 . . . . -28.3(10)
C3 C4 C5 C6 . . . . 177.8(8)
C3 C4 C10 C9 . . . . 25.1(12)
C5 C4 C10 C9 . . . . -160.0(8)
C7 C15 C16 C17 . . . . -176.4(9)
C7 C15 C20 C19 . . . . 176.5(9)
C8 C2 C3 O1 . . . . 175.0(8)
C8 C2 C3 C4 . . . . -7.8(12)
C8 C9 C10 C4 . . . . -60.7(9)
C10 C4 C5 C6 . . . . 2.6(14)
C11 O2 C14 C13 . . . . 1.9(10)
C11 C1 C2 C3 . . . . -178.5(7)
C11 C1 C2 C8 . . . . 4.8(15)
C11 C12 C13 C14 . . . . 0.9(13)
C12 C13 C14 O2 . . . . -1.7(12)
C14 O2 C11 C1 . . . . -177.0(7)
C14 O2 C11 C12 . . . . -1.3(9)
C15 C16 C17 C18 . . . . 0.0(13)
C16 C15 C20 C19 . . . . 0.0(13)
C16 C17 C18 C19 . . . . 0.0(14)
C17 C18 C19 C20 . . . . 0.0(13)
C18 C19 C20 C15 . . . . 0.0(12)
C20 C15 C16 C17 . . . . 0.0(13)
O1A C3A C4A C5A . . . . 4.0(12)
O1A C3A C4A C10A . . . . -173.9(8)
O2A C11A C12A C13A . . . . 1.4(11)
C1A C2A C3A O1A . . . . -7.1(13)
C1A C2A C3A C4A . . . . 171.1(7)
C1A C2A C8A C9A . . . . 156.0(8)
C1A C11A C12A C13A . . . . 177.2(11)
C2A C1A C11A O2A . . . . -167.1(8)
C2A C1A C11A C12A . . . . 17.1(19)
C2A C3A C4A C5A . . . . -174.2(7)
C2A C3A C4A C10A . . . . 8.0(12)
C2A C8A C9A C10A . . . . 59.4(9)
C3A C2A C8A C9A . . . . -28.6(11)
C3A C4A C5A C6A . . . . 177.6(7)
C3A C4A C10A C9A . . . . 22.1(12)
C5A C4A C10A C9A . . . . -155.5(9)
C7A C15A C16A C17A . . . . 177.4(9)
C7A C15A C20A C19A . . . . -179.3(9)
C8A C2A C3A O1A . . . . 177.4(8)
C8A C2A C3A C4A . . . . -4.5(12)
C8A C9A C10A C4A . . . . -57.1(10)
C10A C4A C5A C6A . . . . -4.6(14)
C11A O2A C14A C13A . . . . -7.8(12)
C11A C1A C2A C3A . . . . -175.2(8)
C11A C1A C2A C8A . . . . 0.3(14)
C11A C12A C13A C14A . . . . -5.9(11)
C12A C13A C14A O2A . . . . 8.7(12)
C14A O2A C11A C1A . . . . -173.1(9)
C14A O2A C11A C12A . . . . 3.6(11)
C15A C16A C17A C18A . . . . 1.1(13)
C16A C15A C20A C19A . . . . -3.0(14)
C16A C17A C18A C19A . . . . -1.5(15)
C17A C18A C19A C20A . . . . -0.4(15)
C18A C19A C20A C15A . . . . 2.6(14)
C20A C15A C16A C17A . . . . 1.2(14)
_cod_database_fobs_code 2021679