#------------------------------------------------------------------------------
#$Date: 2021-05-29 08:15:26 +0300 (Sat, 29 May 2021) $
#$Revision: 265611 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243842.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_2243842
loop_
_publ_author_name
'Miyamoto, Hisakazu'
'Takahashi, Hiroki'
_publ_section_title
;
Crystal structure and photoreactive behaviour of
N,N-diisopropyl(p-phenylphenyl)glyoxylamide
;
_journal_coeditor_code DJ2024
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 653
_journal_page_last 657
_journal_paper_doi 10.1107/S2056989021005387
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac 'C20 H23 N O2'
_chemical_formula_moiety 'C20 H23 N O2'
_chemical_formula_sum 'C20 H23 N O2'
_chemical_formula_weight 309.39
_chemical_name_common
;
N,N-Diisopropyl(p-phenylphenyl)glyoxylamide
;
_chemical_name_systematic
;
2-([1,1'-Biphenyl]-4-yl)-2-oxo-N,N-bis(propan-2-yl)acetamide
;
_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'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 6.1313(2)
_cell_length_b 7.3710(2)
_cell_length_c 38.1143(11)
_cell_measurement_reflns_used 2939
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 3.4
_cell_volume 1722.53(9)
_computing_cell_refinement
;
CrystalClear-SM Expert (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert (Rigaku, 2009)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type 'Rigaku Saturn 724+ CCD'
_diffrn_measurement_method 'profile data from \w-scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0207
_diffrn_reflns_av_unetI/netI 0.0180
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 48
_diffrn_reflns_limit_l_min -48
_diffrn_reflns_number 16094
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.965
_diffrn_reflns_theta_min 3.365
_diffrn_source 'sealed tube'
_exptl_absorpt_coefficient_mu 0.076
_exptl_absorpt_correction_T_max 0.985
_exptl_absorpt_correction_T_min 0.985
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
(CrystalClear-SM Expert; Rigaku, 2009)
;
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 1.193
_exptl_crystal_description Prism
_exptl_crystal_F_000 664
_exptl_crystal_size_max 0.310
_exptl_crystal_size_mid 0.290
_exptl_crystal_size_min 0.290
_refine_diff_density_max 0.164
_refine_diff_density_min -0.146
_refine_ls_abs_structure_details
;
Flack x determined using 1346 quotients
[(I^+^)-(I^-^)]/[(I^+^)+(I^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack 0.1(4)
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 212
_refine_ls_number_reflns 3877
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.045
_refine_ls_R_factor_all 0.0399
_refine_ls_R_factor_gt 0.0361
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+0.3778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0787
_refine_ls_wR_factor_ref 0.0803
_reflns_number_gt 3614
_reflns_number_total 3877
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file dj2024sup1.cif
_cod_data_source_block I
_cod_database_code 2243842
_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 0.977
_shelx_estimated_absorpt_t_max 0.978
_shelx_hkl_file
;
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0 0 -9 14.64 2.23
0 0 -9 15.63 2.27
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0 0 -10 253.40 4.74
0 0 -10 268.73 4.90
0 0 -11 0.14 1.28
0 0 -11 2.09 1.45
0 0 -11 1.09 1.49
0 0 -12 205.27 4.76
0 0 -12 213.04 4.70
0 0 -12 222.14 4.83
0 0 -13 1.22 1.41
0 0 -13 2.04 1.49
0 0 -13 -0.22 1.41
0 0 -14 19.27 2.02
0 0 -14 21.12 2.11
0 0 -14 22.29 2.13
0 0 -15 2.01 1.62
0 0 -15 2.21 1.64
0 0 -15 3.33 1.64
0 0 -16 779.19 10.48
0 0 -16 817.53 10.33
0 0 -16 802.71 10.42
0 0 -17 5.26 1.98
0 0 -17 1.28 1.72
0 0 -17 5.69 2.00
0 0 -18 32.96 2.72
0 0 -18 30.01 2.71
0 0 -18 35.26 2.96
0 0 -19 4.91 2.31
0 0 -19 2.59 2.22
0 0 -20 1303.02 14.64
0 0 -20 1281.77 14.75
0 0 -21 11.67 2.69
0 0 -21 13.26 2.77
0 0 -22 663.83 11.12
0 0 -22 685.03 11.40
0 0 -23 5.12 2.69
0 0 -23 5.17 2.49
0 0 -24 802.56 12.81
0 0 -24 794.12 12.96
0 0 -25 9.58 2.80
0 0 -25 4.86 2.56
0 0 -26 33.97 3.58
0 0 -26 26.48 3.26
0 0 -27 77.04 5.62
0 0 -27 67.36 5.17
0 0 -28 7046.95 41.40
0 0 -28 7104.60 41.16
0 0 -29 139.49 7.33
0 0 -29 123.57 7.05
0 0 -30 4256.84 33.48
0 0 -30 4411.59 33.81
0 0 -31 73.60 5.96
0 0 -31 84.41 6.34
0 0 -32 1981.37 23.79
0 0 -32 1822.72 22.66
0 0 -33 44.44 5.16
0 0 -33 31.82 4.79
0 0 -34 987.45 17.57
0 0 -34 1033.97 17.78
0 0 -35 14.00 4.08
0 -1 -4 2606.45 13.33
0 1 -4 2597.77 13.17
0 -1 -4 2558.49 12.96
0 -1 -5 2063.10 12.45
0 -1 -5 2127.04 12.20
0 -1 -6 599.55 7.21
0 1 -6 616.85 7.12
0 -1 -6 594.96 6.83
0 -1 -7 3125.76 16.89
0 1 -7 3124.25 14.59
0 1 -7 3108.88 16.48
0 -1 -7 3097.56 16.02
0 1 8 1797.10 11.16
0 -1 -8 1822.20 13.43
0 -1 -8 1812.87 12.79
0 1 -8 1835.52 11.65
0 1 -8 1846.59 13.30
0 1 9 30.70 1.94
0 -1 -9 36.43 2.33
0 1 -9 37.20 2.46
0 -1 -9 40.33 2.60
0 -1 -9 35.23 1.87
0 1 -9 36.94 2.14
0 -1 -10 4962.24 18.08
0 1 10 5001.88 20.44
0 1 -10 4937.07 18.37
0 1 -10 4996.58 20.65
0 1 -10 5056.98 23.74
0 -1 -10 4919.17 22.60
0 -1 -10 4981.52 23.70
0 -1 -11 1848.62 11.23
0 1 11 1863.81 13.12
0 1 -11 1855.59 11.85
0 1 -11 1851.29 13.17
0 1 -11 1862.55 15.02
0 -1 -11 1861.17 14.42
0 -1 -11 1834.50 14.95
0 -1 -12 1742.04 11.08
0 1 12 1697.52 13.07
0 1 -12 1712.63 11.91
0 1 -12 1751.59 13.23
0 1 -12 1747.89 15.00
0 -1 -12 1704.49 14.25
0 -1 -12 1732.56 15.01
0 -1 -13 464.26 5.88
0 1 13 440.02 6.99
0 1 -13 451.76 6.51
0 1 -13 460.03 7.16
0 1 -13 458.14 8.04
0 -1 -13 472.00 7.82
0 -1 -13 465.06 8.15
0 -1 -14 196.65 4.00
0 1 14 200.94 5.07
0 1 -14 189.92 4.53
0 1 -14 186.61 4.81
0 1 -14 197.19 5.59
0 -1 -14 193.97 5.33
0 -1 -14 211.09 5.89
0 -1 -15 3085.73 15.25
0 1 -15 3072.47 19.37
0 1 -15 3051.01 18.07
0 -1 -15 3077.39 20.89
0 1 -15 3094.67 21.75
0 -1 -15 3022.46 21.58
0 1 15 3057.47 19.47
0 1 -16 1.20 1.68
0 1 16 2.05 1.84
0 -1 -16 1.32 1.48
0 1 -16 0.55 2.06
0 -1 -16 3.36 2.20
0 -1 -16 8.83 2.70
0 1 -16 2.64 1.68
0 1 17 657.75 9.80
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0 -1 -17 672.36 10.47
0 1 -17 674.64 9.76
0 -1 -17 689.87 7.49
0 1 -17 684.49 9.28
0 -1 -17 681.20 10.92
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0 1 -18 89.85 4.60
0 -1 -18 93.55 4.77
0 1 -18 85.99 3.99
0 -1 -18 86.54 3.04
0 1 -18 83.17 3.76
0 -1 -18 98.95 4.97
0 1 19 4683.47 27.26
0 1 -19 4609.56 29.44
0 -1 -19 4663.42 28.40
0 1 -19 4595.29 26.65
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0 1 20 4.75 2.86
0 1 -20 1.16 2.35
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0 -1 -20 0.05 1.78
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0 1 -21 136.62 4.91
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0 1 -22 185.42 6.12
0 1 22 193.71 6.36
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0 -1 -22 199.52 6.93
0 1 -23 154.24 6.32
0 -1 -23 156.88 6.23
0 1 -23 154.83 5.83
0 1 23 157.88 5.99
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0 1 -30 70.95 5.56
0 -1 -30 70.53 5.46
0 1 -30 76.37 5.46
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0 -1 -32 698.87 14.68
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0 -1 -33 368.15 11.15
0 -1 -34 216.87 9.21
0 -1 -34 200.10 8.59
0 -1 -35 34.67 5.31
0 -1 -35 38.97 5.08
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0 -1 -36 388.76 11.93
0 -1 -37 402.38 12.88
0 -1 -38 969.09 19.70
0 -1 -39 72.70 6.92
0 -1 -40 224.65 10.37
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0 -2 2 1656.35 13.20
0 -2 -2 1654.36 13.39
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0 2 -2 1629.45 12.75
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0 2 4 1087.38 9.82
0 2 -4 1103.67 9.01
0 -2 4 1100.07 10.74
0 -2 -4 1092.55 11.05
0 2 -4 1094.81 10.53
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0 -2 -5 8280.30 30.78
0 2 -5 8332.94 24.33
0 -2 5 8211.86 29.04
0 -2 -5 8246.35 30.30
0 2 -5 8296.04 28.88
0 2 -6 1265.09 12.56
0 2 -6 1304.51 9.63
0 -2 -6 1278.62 12.60
0 2 6 1286.88 10.72
0 2 -6 1309.60 11.79
0 -2 6 1286.82 11.60
0 -2 -6 1274.28 12.11
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0 2 -7 161.57 3.56
0 -2 -7 147.41 4.60
0 -2 -7 146.78 4.69
0 2 7 144.95 3.84
0 2 -7 143.46 4.18
0 -2 7 146.80 4.17
0 -2 -7 162.79 4.61
0 2 -8 506.92 8.43
0 2 -8 513.90 6.28
0 -2 -8 496.94 8.22
0 -2 -8 503.48 8.43
0 2 8 509.92 7.02
0 2 -8 487.12 7.46
0 -2 -8 507.33 7.77
0 -2 8 492.76 7.22
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0 -2 9 1511.11 12.43
0 -2 -9 1482.00 13.22
0 -2 -9 1493.21 14.74
0 2 -9 1469.53 13.07
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0 -2 10 1690.51 13.18
0 -2 -10 1671.42 14.12
0 2 -10 1679.10 14.21
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0 -2 -11 45.87 2.76
0 2 -11 49.35 3.18
0 -2 -11 47.18 3.11
0 2 11 48.08 2.68
0 -2 -11 45.33 3.28
0 2 -11 44.39 2.26
0 2 -11 48.59 2.90
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0 2 -12 290.43 6.30
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0 2 -13 1362.60 15.44
0 -2 -13 1358.59 14.73
0 2 -13 1329.99 11.22
0 -2 -14 207.17 6.49
0 2 -14 219.68 6.69
0 2 14 207.23 5.38
0 2 -14 219.78 5.76
0 -2 14 215.37 4.99
0 -2 -14 224.55 5.51
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0 2 -14 209.65 4.75
0 -2 -15 179.53 6.21
0 2 -15 193.35 6.37
0 -2 15 200.22 4.77
0 -2 -15 192.38 5.17
0 2 15 185.97 5.20
0 2 -15 182.79 5.47
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0 2 -16 2.98 2.03
0 2 16 2.90 1.88
0 -2 -16 1.55 2.15
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0 2 17 153.38 5.08
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0 2 -17 144.51 4.41
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0 2 -17 151.58 6.02
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0 -2 -17 160.09 5.83
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0 2 -18 1030.38 11.39
0 -2 -18 1028.13 11.75
0 2 -18 1000.71 14.80
0 -2 -18 1046.88 15.32
0 -2 -18 1039.52 14.45
0 -2 19 2726.49 16.80
0 -2 -19 2824.46 19.38
0 2 -19 2885.26 19.44
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0 2 -19 2834.58 25.20
0 2 19 2805.99 21.40
0 2 -19 2786.24 21.83
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0 2 -20 83.69 4.96
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0 2 -20 83.15 4.36
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0 -2 -21 2167.24 17.31
0 2 -21 2152.39 17.83
0 -2 -21 2188.17 22.06
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0 2 -21 2130.46 20.04
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0 -2 -22 56.16 3.46
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0 2 -24 31.11 3.42
0 2 -24 26.63 4.05
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0 -2 -26 5.01 3.67
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0 -2 -26 8.11 3.58
0 -2 -27 974.81 17.56
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0 2 -28 1476.48 19.22
0 2 -28 1410.23 21.12
0 2 28 1451.64 19.09
0 -2 -28 1458.03 20.56
0 -2 -29 1012.37 18.44
0 2 -29 1004.01 16.42
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0 -2 -29 1044.26 17.94
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0 -2 -30 1036.51 19.06
0 2 -30 1032.44 16.90
0 -2 -31 2174.61 27.63
0 2 -31 2104.35 27.07
0 -2 -31 2156.66 26.22
0 -2 -32 664.54 15.97
0 -2 -32 626.43 14.92
0 -2 -33 191.58 9.07
0 2 -33 173.85 8.77
0 -2 -33 182.88 8.65
0 -2 -34 216.68 9.83
0 2 -34 223.27 9.85
0 -2 -34 233.24 9.63
0 -2 -35 8.11 4.28
0 2 -35 7.50 4.36
0 -2 -35 2.30 3.91
0 -2 -36 -2.25 4.37
0 2 -36 4.97 4.39
0 -2 -36 -0.27 3.89
0 -2 -37 39.46 5.70
0 2 -37 23.66 4.98
0 -2 -37 34.15 5.41
0 -2 -38 29.62 5.63
0 2 -38 26.24 5.28
0 -2 -38 32.86 5.36
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0 2 -39 49.63 6.39
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0 -2 -41 2.31 4.58
0 -2 -42 60.06 7.18
0 -2 -43 8.49 5.55
0 -2 -44 13.67 5.55
0 -3 0 0.84 1.61
0 3 0 1.98 1.90
0 -3 0 -1.57 2.10
0 3 0 3.71 1.88
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0 -3 1 2181.24 18.67
0 3 1 2242.55 18.72
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-6 -6 -8 5.73 7.29
6 6 -8 12.90 7.17
-6 -6 -7 47.92 8.63
6 6 -7 54.95 8.54
6 -6 7 65.23 8.94
6 -6 6 151.48 11.52
-6 -6 -6 147.27 11.89
6 6 -6 141.46 11.26
6 6 -5 36.32 7.72
-6 -6 -5 41.08 8.68
6 -6 5 28.06 7.59
6 6 -4 14.60 6.86
-6 -6 -4 1.10 6.96
6 -6 4 6.94 6.51
6 6 -3 31.39 7.47
-6 -6 -3 17.06 7.41
6 -6 3 16.34 7.28
6 6 -2 33.78 7.41
-6 -6 -2 18.27 7.51
6 -6 2 17.28 7.35
6 6 -1 2.46 6.39
6 -6 1 8.94 7.03
6 6 0 12.36 6.60
6 -6 0 25.41 7.75
6 6 1 17.88 7.23
6 -6 -1 7.67 7.02
-6 6 -2 2.82 6.19
6 6 2 16.09 7.15
6 -6 -2 11.37 6.84
-6 6 -3 13.71 7.28
6 6 3 -2.98 6.77
6 -6 -3 23.00 7.26
-6 6 -4 15.80 6.61
-6 6 -5 34.35 7.85
-6 6 -6 167.74 11.87
-6 6 -7 47.54 8.67
-6 6 -8 4.95 7.29
-6 6 -9 167.43 12.41
-7 0 -6 13.54 5.50
-7 0 -7 3.98 5.25
-7 0 -8 10.27 5.34
-7 0 -9 15.55 5.90
-7 0 -9 18.51 6.02
-7 0 -10 8.21 6.09
-7 0 -10 -2.80 5.16
-7 0 -11 109.94 9.27
-7 0 -12 20.08 6.67
-7 0 -13 -0.70 5.39
-7 0 -14 11.36 5.80
-7 0 -15 14.18 6.70
-7 0 -16 -2.10 5.40
-7 0 -17 10.55 5.93
7 0 18 3.82 5.65
-7 0 -18 -0.59 5.73
-7 0 -19 47.87 8.16
7 0 19 42.72 7.69
7 0 20 14.16 6.18
-7 0 -20 10.68 6.33
-7 0 -20 25.99 7.35
7 0 21 36.24 7.29
-7 0 -21 25.37 7.04
-7 0 -21 15.77 6.75
7 0 22 16.89 6.66
-7 0 -22 21.71 7.16
-7 0 -22 23.42 7.21
7 0 23 25.45 6.97
-7 0 -23 22.18 6.95
7 0 24 -3.18 6.50
-7 0 -24 -5.56 6.34
7 -1 24 2.02 6.08
-7 -1 -24 -1.89 6.66
7 -1 23 3.48 6.08
-7 -1 -23 6.33 6.25
-7 -1 -22 3.30 6.42
-7 -1 -21 14.08 6.79
-7 -1 -20 32.13 7.59
-7 -1 -19 144.60 11.12
-7 -1 -18 55.18 8.40
-7 -1 -17 36.03 7.44
-7 -1 -16 -4.19 5.97
-7 -1 -15 20.21 6.54
-7 -1 -14 38.72 7.20
-7 -1 -13 64.12 7.88
-7 -1 -12 18.68 6.09
-7 -1 -11 11.74 5.80
-7 -1 -10 96.81 8.84
-7 -1 -9 77.44 8.45
-7 -1 -8 24.46 6.95
-7 -1 -7 45.69 7.37
-7 -1 -6 43.14 7.22
-7 -1 -5 26.02 6.68
-7 -1 -4 117.71 9.60
-7 -1 -3 73.81 8.56
-7 -1 -2 121.50 9.80
-7 -1 -1 57.42 7.92
-7 -1 0 145.06 10.48
-7 1 -1 29.05 6.15
-7 -1 1 38.55 7.45
-7 1 -2 103.49 8.79
-7 -1 2 117.85 10.12
-7 1 -3 65.32 7.69
-7 -1 3 56.05 8.22
-7 1 -4 112.34 9.14
-7 -1 4 81.54 8.92
-7 1 -5 18.47 5.99
-7 -1 5 27.59 7.28
-7 1 -6 33.62 6.68
-7 -1 6 50.93 7.64
-7 1 -7 47.30 7.31
-7 -1 7 39.62 7.78
-7 1 -8 11.41 5.70
-7 -1 8 20.78 6.61
-7 1 -9 74.62 8.26
-7 -1 9 78.72 9.03
-7 1 -10 98.92 9.10
-7 -1 10 92.55 9.56
-7 1 -11 6.38 5.72
-7 -1 11 12.05 6.51
-7 1 -12 14.88 6.51
-7 -1 12 17.35 6.67
-7 1 -13 48.12 7.36
7 1 13 63.60 7.73
-7 -1 13 64.98 8.81
7 1 14 49.01 7.26
-7 1 -14 29.73 7.30
-7 -1 14 40.88 8.11
-7 1 -15 39.56 7.30
7 1 15 17.04 6.18
-7 -1 15 26.17 7.21
-7 1 -16 18.21 7.09
7 1 16 8.22 5.87
-7 -1 16 14.04 6.91
-7 1 -17 27.31 7.29
-7 -1 17 38.37 7.64
7 1 17 27.41 6.73
-7 1 -18 64.17 8.50
-7 -1 18 79.15 9.44
7 1 18 72.01 8.63
-7 1 -18 52.14 8.24
-7 1 -19 141.42 11.01
7 1 19 141.38 10.54
-7 -1 19 152.95 11.65
-7 1 -19 177.96 12.23
-7 1 -20 7.98 6.55
-7 -1 20 21.54 7.49
-7 1 -20 30.19 7.39
7 1 20 25.51 7.08
-7 -1 21 15.84 7.28
-7 1 -21 14.76 6.62
7 1 21 14.11 6.47
-7 1 -22 7.59 6.41
7 1 22 -7.84 6.49
-7 1 -23 11.07 7.03
7 1 23 5.42 6.19
-7 -2 -21 173.06 12.45
-7 -2 -20 24.39 7.60
-7 -2 -19 126.16 10.49
-7 -2 -18 37.17 7.78
-7 -2 -17 79.17 8.92
-7 -2 -16 0.93 6.15
-7 -2 -11 39.20 7.65
-7 -2 -10 67.85 8.27
-7 -2 -9 73.07 8.39
-7 -2 -8 26.55 6.75
-7 -2 -7 8.86 6.40
-7 -2 -6 52.65 7.84
-7 -2 -5 12.38 6.07
-7 2 4 7.46 5.45
-7 -2 -4 1.30 6.10
-7 2 3 30.11 6.29
-7 -2 -3 40.21 7.21
-7 2 2 81.77 8.28
-7 -2 -2 44.03 7.73
-7 2 1 27.39 6.33
-7 -2 -1 17.71 6.79
-7 2 0 40.12 6.77
-7 -2 0 37.22 7.27
-7 2 -1 27.43 6.45
7 -2 -1 32.00 6.85
-7 -2 1 36.26 7.46
-7 2 -2 70.89 8.31
7 -2 -2 61.86 8.28
-7 -2 2 69.08 8.30
-7 2 -3 23.77 6.44
7 -2 -3 32.03 7.38
-7 -2 3 25.03 6.81
-7 2 -4 4.68 5.49
7 -2 -4 5.40 5.77
-7 -2 4 18.21 7.07
-7 2 -5 20.00 6.29
7 -2 -5 11.76 6.23
-7 -2 5 23.97 7.02
-7 2 -6 38.24 6.90
7 -2 -6 47.85 7.69
-7 -2 6 38.79 7.46
-7 2 -7 9.91 6.05
7 -2 -7 7.15 5.91
-7 -2 7 10.19 6.42
-7 2 -8 24.62 6.60
7 -2 -8 18.69 6.93
-7 -2 8 14.65 6.78
7 2 9 62.34 7.89
-7 2 -9 56.76 7.95
7 -2 -9 64.29 8.62
-7 -2 9 50.27 8.22
7 2 10 73.39 7.99
-7 2 -10 67.56 8.44
7 -2 -10 82.18 9.01
-7 -2 10 100.51 9.63
-7 2 -11 50.79 8.05
7 -2 -11 55.48 8.49
-7 -2 11 45.26 7.92
7 2 12 15.18 5.99
-7 2 -12 25.50 7.17
7 -2 -12 21.21 6.91
-7 -2 12 32.76 7.46
7 2 13 47.96 7.23
-7 2 -13 43.18 7.77
7 -2 -13 47.87 8.51
7 2 14 25.96 6.93
-7 -2 14 24.51 7.42
-7 2 -14 17.13 6.58
7 -2 -14 13.72 6.78
7 2 15 5.00 5.52
-7 -2 15 4.18 6.43
-7 2 -15 4.69 6.12
7 2 16 9.46 6.29
-7 2 -16 1.82 6.04
-7 2 -17 107.38 9.59
-7 -2 17 100.24 10.47
-7 2 -17 91.97 9.62
7 2 17 75.10 8.81
7 2 18 39.70 7.68
-7 2 -18 34.40 7.91
-7 -2 18 37.49 7.91
-7 2 -18 33.39 7.45
7 2 19 99.84 9.64
-7 2 -19 111.03 10.03
7 2 20 26.08 7.37
-7 2 -20 31.14 7.73
-7 2 -21 167.86 12.01
-7 -3 -11 11.42 6.57
-7 -3 -10 55.61 8.29
-7 -3 -9 15.72 6.99
-7 3 9 10.27 6.12
-7 -3 -8 44.35 8.03
-7 3 8 30.79 6.85
7 -3 7 11.87 6.39
-7 -3 -7 15.21 6.78
-7 3 7 5.32 5.90
-7 -3 -6 46.96 8.23
7 -3 6 44.60 7.77
-7 -3 -5 55.44 8.18
7 -3 5 47.97 7.85
-7 3 5 52.66 7.89
7 -3 4 20.83 6.82
-7 -3 -4 18.51 6.56
-7 3 4 7.01 6.09
7 -3 3 12.50 6.48
-7 -3 -3 8.09 6.75
-7 3 3 2.47 5.62
7 -3 2 26.89 7.04
-7 -3 -2 29.31 7.33
-7 3 2 30.06 7.08
7 -3 1 17.59 6.53
-7 -3 -1 29.94 7.63
-7 3 1 27.73 7.20
-7 -3 0 96.40 9.47
7 -3 0 85.88 9.21
-7 3 0 83.84 8.96
7 -3 -1 23.42 6.77
-7 3 -1 25.20 6.62
-7 -3 1 10.97 6.55
7 -3 -2 21.30 6.86
-7 3 -2 12.56 6.14
-7 -3 2 19.71 7.33
7 -3 -3 12.13 6.66
-7 3 -3 10.70 6.16
-7 -3 3 19.59 7.12
7 -3 -4 23.06 7.17
-7 3 -4 16.38 6.49
-7 -3 4 29.94 7.38
-7 3 -5 63.45 8.32
7 -3 -5 60.82 8.75
7 3 5 60.23 7.72
-7 -3 5 60.75 8.60
-7 3 -6 59.05 8.51
7 -3 -6 48.11 7.89
7 3 6 55.47 7.93
-7 -3 6 78.18 9.30
-7 3 -7 10.20 6.54
7 -3 -7 0.87 6.14
7 3 7 2.75 6.03
-7 -3 7 2.36 6.66
-7 3 -8 36.21 7.37
7 -3 -8 28.72 7.28
7 3 8 31.70 7.05
-7 -3 8 47.55 8.16
-7 3 -9 16.24 6.86
7 -3 -9 20.56 7.53
7 3 9 11.93 6.13
-7 -3 9 16.76 7.21
-7 3 -10 67.62 8.95
7 -3 -10 65.61 9.39
7 3 10 60.88 7.96
-7 -3 10 53.04 8.46
-7 3 -11 4.60 6.43
7 -3 -11 7.15 7.10
7 3 11 8.68 6.27
-7 -3 11 9.62 6.95
-7 3 -12 35.87 7.63
7 -3 -12 32.09 7.56
7 3 12 43.31 7.69
-7 -3 12 46.54 8.50
-7 3 -13 45.97 8.35
7 -3 -13 45.30 8.32
-7 -3 13 47.94 8.68
7 3 13 53.28 8.13
-7 3 -14 4.37 6.63
7 3 14 5.39 6.24
-7 3 -15 32.56 7.64
7 3 15 32.96 7.58
-7 3 -16 36.19 7.72
7 3 16 39.04 7.90
-7 3 -17 33.18 7.67
7 3 17 26.26 7.40
-7 3 -18 22.45 7.27
-7 4 13 2.39 6.59
-7 4 12 15.87 7.18
-7 -4 -11 98.15 10.18
-7 4 11 96.29 10.06
-7 -4 -10 11.46 7.34
-7 4 10 27.77 7.46
-7 4 9 67.10 9.01
-7 -4 -9 72.51 9.33
-7 4 8 42.50 8.01
-7 -4 -8 43.15 8.46
-7 -4 -7 48.47 8.77
7 -4 7 35.64 7.74
-7 4 7 40.86 8.00
7 -4 6 17.61 7.22
-7 4 6 22.32 7.01
-7 -4 -6 30.18 8.07
7 -4 5 11.30 7.29
-7 4 5 7.32 6.36
-7 -4 -5 14.93 7.30
7 -4 4 12.61 6.97
-7 4 4 -2.54 6.31
-7 -4 -4 6.82 6.96
-7 4 3 12.65 6.82
-7 -4 -3 25.94 7.35
7 -4 2 21.14 7.21
-7 4 2 19.94 7.04
-7 -4 -2 9.68 6.98
-7 -4 -1 28.64 7.65
7 -4 1 21.15 7.00
-7 4 1 40.53 8.20
-7 4 0 19.36 6.99
7 -4 0 5.52 6.77
-7 -4 0 16.29 7.49
7 -4 -1 50.82 8.69
-7 -4 1 29.10 7.73
-7 4 -1 25.65 7.23
7 4 1 29.13 7.19
-7 -4 2 33.93 8.60
7 4 2 10.30 6.44
-7 4 -2 19.93 7.08
7 -4 -2 16.51 7.10
-7 -4 3 44.01 8.64
7 -4 -3 44.73 8.29
-7 4 -3 17.14 6.52
7 4 3 41.23 7.64
7 4 4 5.39 6.10
-7 4 -4 -13.99 6.95
7 -4 -4 -8.27 7.18
7 4 5 8.67 6.58
-7 4 -5 14.63 6.92
7 -4 -5 4.35 6.82
7 4 6 25.77 7.02
7 4 7 51.68 8.17
7 4 8 41.59 7.97
7 4 9 33.28 7.79
7 4 10 15.27 7.18
7 4 11 91.10 9.97
-7 4 -13 14.27 6.89
-7 4 -14 18.70 7.47
-8 0 -5 10.59 7.28
-8 0 -6 17.62 7.75
-8 0 -7 6.27 6.76
0 0 0 0.00 0.00
TITL pPh-2 in P2(1)2(1)2
REM P2(1)2(1)2 (#18 in standard setting)
CELL 0.71073 6.131272 7.371038 38.114260 90.0000 90.0000 90.0000
ZERR 4.00 0.000181 0.000219 0.001120 0.0000 0.0000 0.0000
LATT -1
SYMM -x,-y, z
SYMM -x+1/2, y+1/2,-z
SYMM x+1/2,-y+1/2,-z
SFAC C H N O
UNIT 80.00 96.00 4.00 8.00
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 63284
_shelx_res_file
;
TITL pph-2_a.res in P2(1)2(1)2(1)
pPh-2.res
created by SHELXL-2018/3 at 18:43:43 on 24-Mar-2021
REM Yadorkari-X generated
CELL 0.71073 6.1313 7.3710 38.1143 90.0000 90.0000 90.0000
ZERR 4.0 0.0002 0.0002 0.0011 0.0000 0.0000 0.0000
LATT -1
SYMM 1/2-X, -Y, 1/2+Z
SYMM 1/2+X, 1/2-Y, -Z
SYMM -X, 1/2+Y, 1/2-Z
REM SPGR P212121 orthorhombic
SFAC C H N O
UNIT 80 92 4 8
SIZE 0.31 0.29 0.29
TEMP -100.0
L.S. 10
FMAP 2
PLAN -2
ACTA
CONF
HTAB
LIST 4
BOND $H
list 4
fmap 2 53
HTAB C9 O1
HTAB C14 O2
WGHT 0.031400 0.377800
FVAR 1.33237
C1 1 0.509290 0.572772 0.664694 11.00000 0.02849 0.02339 =
0.02008 0.00115 -0.00348 0.00242
C2 1 0.616063 0.649088 0.693556 11.00000 0.02488 0.02750 =
0.02674 0.00017 -0.00310 -0.00269
AFIX 43
H1 2 0.757076 0.700514 0.690769 11.00000 -1.20000
AFIX 0
C3 1 0.517117 0.649902 0.726088 11.00000 0.02748 0.02775 =
0.02162 -0.00222 -0.00615 -0.00330
AFIX 43
H2 2 0.591743 0.702783 0.745390 11.00000 -1.20000
AFIX 0
C4 1 0.309739 0.574953 0.731455 11.00000 0.02671 0.02018 =
0.02228 0.00087 -0.00315 0.00283
O1 4 0.812817 0.613273 0.626559 11.00000 0.03588 0.05939 =
0.02856 -0.00201 0.00361 -0.00635
O2 4 0.486930 0.326285 0.596650 11.00000 0.05984 0.02591 =
0.02850 0.00041 -0.00790 0.00302
N1 3 0.418843 0.610841 0.575092 11.00000 0.03761 0.02549 =
0.01975 -0.00014 -0.00165 0.00023
C5 1 0.203960 0.500748 0.702096 11.00000 0.02520 0.03125 =
0.02828 -0.00169 -0.00368 -0.00482
AFIX 43
H3 2 0.062937 0.449217 0.704797 11.00000 -1.20000
AFIX 0
C6 1 0.301194 0.501145 0.669218 11.00000 0.03025 0.03336 =
0.02235 -0.00335 -0.00812 -0.00056
AFIX 43
H4 2 0.225190 0.452194 0.649669 11.00000 -1.20000
AFIX 0
C7 1 0.622739 0.569664 0.630282 11.00000 0.03383 0.02707 =
0.02443 0.00209 -0.00234 -0.00001
C8 1 0.498538 0.492713 0.598625 11.00000 0.03649 0.02844 =
0.01940 -0.00002 0.00067 0.00096
C9 1 0.436361 0.809947 0.580339 11.00000 0.04421 0.02636 =
0.02476 0.00110 -0.00176 -0.00253
AFIX 13
H5 2 0.497384 0.829750 0.604367 11.00000 -1.20000
AFIX 0
C10 1 0.594948 0.894656 0.554486 11.00000 0.04456 0.03823 =
0.05814 0.01043 0.00893 -0.00287
AFIX 137
H6 2 0.736401 0.833410 0.556225 11.00000 -1.50000
H7 2 0.612914 1.023717 0.559944 11.00000 -1.50000
H8 2 0.537864 0.881506 0.530604 11.00000 -1.50000
AFIX 0
C11 1 0.214463 0.901298 0.579288 11.00000 0.05062 0.03155 =
0.04514 -0.00447 0.01347 0.00383
AFIX 137
H9 2 0.156583 0.896594 0.555338 11.00000 -1.50000
H10 2 0.229103 1.028114 0.586642 11.00000 -1.50000
H11 2 0.114502 0.838140 0.595205 11.00000 -1.50000
AFIX 0
C12 1 0.311127 0.544467 0.542502 11.00000 0.04212 0.03108 =
0.01953 -0.00203 -0.00497 0.00740
AFIX 13
H12 2 0.270143 0.654227 0.528562 11.00000 -1.20000
AFIX 0
C13 1 0.467955 0.434545 0.519928 11.00000 0.05932 0.05703 =
0.02341 -0.00811 -0.00233 0.01837
AFIX 137
H13 2 0.601203 0.504937 0.515886 11.00000 -1.50000
H14 2 0.398812 0.406781 0.497376 11.00000 -1.50000
H15 2 0.504725 0.321214 0.532000 11.00000 -1.50000
AFIX 0
C14 1 0.100730 0.444152 0.550627 11.00000 0.04757 0.04331 =
0.03947 -0.00805 -0.00929 -0.00282
AFIX 137
H16 2 0.134408 0.331101 0.563027 11.00000 -1.50000
H17 2 0.024513 0.416204 0.528682 11.00000 -1.50000
H18 2 0.007510 0.520425 0.565414 11.00000 -1.50000
AFIX 0
C15 1 0.206828 0.572909 0.766995 11.00000 0.02934 0.01932 =
0.02403 -0.00016 -0.00040 0.00186
C16 1 0.314950 0.645021 0.796305 11.00000 0.03965 0.03233 =
0.02598 -0.00159 0.00046 -0.00756
AFIX 43
H19 2 0.454724 0.698538 0.793378 11.00000 -1.20000
AFIX 0
C17 1 0.221902 0.639734 0.829444 11.00000 0.05680 0.03506 =
0.02376 -0.00334 0.00094 -0.00800
AFIX 43
H20 2 0.299212 0.687471 0.848972 11.00000 -1.20000
AFIX 0
C18 1 0.017205 0.565321 0.834177 11.00000 0.05546 0.03224 =
0.02854 0.00310 0.01258 0.00053
AFIX 43
H21 2 -0.047408 0.563386 0.856828 11.00000 -1.20000
AFIX 0
C19 1 -0.092955 0.493691 0.805721 11.00000 0.03596 0.03480 =
0.03733 0.00376 0.00896 -0.00092
AFIX 43
H22 2 -0.233437 0.441822 0.808872 11.00000 -1.20000
AFIX 0
C20 1 0.000499 0.497174 0.772632 11.00000 0.03046 0.02808 =
0.02998 0.00003 -0.00234 0.00115
AFIX 43
H23 2 -0.077146 0.447082 0.753360 11.00000 -1.20000
AFIX 0
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM pph-2_a.res in P2(1)2(1)2(1)
REM wR2 = 0.0803, GooF = S = 1.045, Restrained GooF = 1.045 for all data
REM R1 = 0.0361 for 3614 Fo > 4sig(Fo) and 0.0399 for all 3877 data
REM 212 parameters refined using 0 restraints
END
WGHT 0.0308 0.3780
REM Instructions for potential hydrogen bonds
HTAB C9 O1
HTAB C13 O2
HTAB C14 O2
REM Highest difference peak 0.164, deepest hole -0.146, 1-sigma level 0.029
Q1 1 0.2423 0.6380 0.7803 11.00000 0.05 0.16
Q2 1 0.2769 0.4954 0.7200 11.00000 0.05 0.16
;
_shelx_res_checksum 28522
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.5093(3) 0.5728(2) 0.66469(4) 0.0240(3) Uani d 1 . .
C C2 0.6161(3) 0.6491(2) 0.69356(4) 0.0264(4) Uani d 1 . .
H H1 0.757076 0.700514 0.690769 0.032 Uiso calc 1 . .
C C3 0.5171(3) 0.6499(2) 0.72609(4) 0.0256(3) Uani d 1 . .
H H2 0.591743 0.702783 0.745390 0.031 Uiso calc 1 . .
C C4 0.3097(3) 0.5750(2) 0.73146(4) 0.0231(3) Uani d 1 . .
O O1 0.8128(2) 0.6133(2) 0.62656(3) 0.0413(3) Uani d 1 . .
O O2 0.4869(2) 0.32629(16) 0.59665(3) 0.0381(3) Uani d 1 . .
N N1 0.4188(2) 0.61084(19) 0.57509(4) 0.0276(3) Uani d 1 . .
C C5 0.2040(3) 0.5007(2) 0.70210(5) 0.0282(4) Uani d 1 . .
H H3 0.062937 0.449217 0.704797 0.034 Uiso calc 1 . .
C C6 0.3012(3) 0.5011(2) 0.66922(4) 0.0287(4) Uani d 1 . .
H H4 0.225190 0.452194 0.649669 0.034 Uiso calc 1 . .
C C7 0.6227(3) 0.5697(2) 0.63028(4) 0.0284(4) Uani d 1 . .
C C8 0.4985(3) 0.4927(2) 0.59863(4) 0.0281(4) Uani d 1 . .
C C9 0.4364(3) 0.8099(2) 0.58034(5) 0.0318(4) Uani d 1 . .
H H5 0.497384 0.829750 0.604367 0.038 Uiso calc 1 . .
C C10 0.5949(4) 0.8947(3) 0.55449(6) 0.0470(5) Uani d 1 . .
H H6 0.736401 0.833410 0.556225 0.070 Uiso calc 1 . .
H H7 0.612914 1.023717 0.559944 0.070 Uiso calc 1 . .
H H8 0.537864 0.881506 0.530604 0.070 Uiso calc 1 . .
C C11 0.2145(4) 0.9013(3) 0.57929(6) 0.0424(5) Uani d 1 . .
H H9 0.156583 0.896594 0.555338 0.064 Uiso calc 1 . .
H H10 0.229103 1.028114 0.586642 0.064 Uiso calc 1 . .
H H11 0.114502 0.838140 0.595205 0.064 Uiso calc 1 . .
C C12 0.3111(3) 0.5445(2) 0.54250(4) 0.0309(4) Uani d 1 . .
H H12 0.270143 0.654227 0.528562 0.037 Uiso calc 1 . .
C C13 0.4680(4) 0.4345(3) 0.51993(5) 0.0466(5) Uani d 1 . .
H H13 0.601203 0.504937 0.515886 0.070 Uiso calc 1 . .
H H14 0.398812 0.406781 0.497376 0.070 Uiso calc 1 . .
H H15 0.504725 0.321214 0.532000 0.070 Uiso calc 1 . .
C C14 0.1007(4) 0.4442(3) 0.55063(6) 0.0434(5) Uani d 1 . .
H H16 0.134408 0.331101 0.563027 0.065 Uiso calc 1 . .
H H17 0.024513 0.416204 0.528682 0.065 Uiso calc 1 . .
H H18 0.007510 0.520425 0.565414 0.065 Uiso calc 1 . .
C C15 0.2068(3) 0.5729(2) 0.76699(4) 0.0242(3) Uani d 1 . .
C C16 0.3150(3) 0.6450(2) 0.79631(5) 0.0327(4) Uani d 1 . .
H H19 0.454724 0.698538 0.793378 0.039 Uiso calc 1 . .
C C17 0.2219(4) 0.6397(3) 0.82944(5) 0.0385(5) Uani d 1 . .
H H20 0.299212 0.687471 0.848972 0.046 Uiso calc 1 . .
C C18 0.0172(4) 0.5653(3) 0.83418(5) 0.0387(5) Uani d 1 . .
H H21 -0.047408 0.563386 0.856828 0.046 Uiso calc 1 . .
C C19 -0.0930(3) 0.4937(3) 0.80572(5) 0.0360(4) Uani d 1 . .
H H22 -0.233437 0.441822 0.808872 0.043 Uiso calc 1 . .
C C20 0.0005(3) 0.4972(2) 0.77263(5) 0.0295(4) Uani d 1 . .
H H23 -0.077146 0.447082 0.753360 0.035 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 0.0285(8) 0.0234(7) 0.0201(8) 0.0024(7) -0.0035(6) 0.0011(6)
C2 0.0249(8) 0.0275(8) 0.0267(9) -0.0027(7) -0.0031(7) 0.0002(7)
C3 0.0275(8) 0.0278(8) 0.0216(8) -0.0033(7) -0.0061(7) -0.0022(6)
C4 0.0267(8) 0.0202(7) 0.0223(8) 0.0028(7) -0.0031(6) 0.0009(6)
O1 0.0359(7) 0.0594(9) 0.0286(7) -0.0063(7) 0.0036(6) -0.0020(6)
O2 0.0598(9) 0.0259(6) 0.0285(6) 0.0030(6) -0.0079(6) 0.0004(5)
N1 0.0376(8) 0.0255(7) 0.0198(7) 0.0002(6) -0.0016(6) -0.0001(6)
C5 0.0252(8) 0.0313(8) 0.0283(9) -0.0048(8) -0.0037(7) -0.0017(7)
C6 0.0303(9) 0.0334(9) 0.0224(8) -0.0006(8) -0.0081(7) -0.0034(7)
C7 0.0338(10) 0.0271(8) 0.0244(8) 0.0000(7) -0.0023(7) 0.0021(7)
C8 0.0365(10) 0.0284(8) 0.0194(8) 0.0010(8) 0.0007(7) 0.0000(7)
C9 0.0442(11) 0.0264(8) 0.0248(9) -0.0025(8) -0.0018(8) 0.0011(7)
C10 0.0446(11) 0.0382(11) 0.0581(13) -0.0029(10) 0.0089(10) 0.0104(10)
C11 0.0506(12) 0.0316(9) 0.0451(11) 0.0038(9) 0.0135(10) -0.0045(9)
C12 0.0421(10) 0.0311(9) 0.0195(8) 0.0074(8) -0.0050(7) -0.0020(7)
C13 0.0593(14) 0.0570(13) 0.0234(9) 0.0184(12) -0.0023(9) -0.0081(9)
C14 0.0476(12) 0.0433(11) 0.0395(11) -0.0028(10) -0.0093(10) -0.0081(9)
C15 0.0293(8) 0.0193(7) 0.0240(8) 0.0019(7) -0.0004(7) -0.0002(6)
C16 0.0396(10) 0.0323(9) 0.0260(9) -0.0076(8) 0.0005(8) -0.0016(7)
C17 0.0568(12) 0.0351(10) 0.0238(9) -0.0080(9) 0.0009(9) -0.0033(8)
C18 0.0555(13) 0.0322(9) 0.0285(9) 0.0005(9) 0.0126(9) 0.0031(8)
C19 0.0360(10) 0.0348(9) 0.0373(10) -0.0009(8) 0.0090(9) 0.0038(8)
C20 0.0305(9) 0.0281(8) 0.0300(9) 0.0011(8) -0.0023(7) 0.0000(7)
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C6 C1 C2 . . 118.98(15) ?
C6 C1 C7 . . 122.22(15) ?
C2 C1 C7 . . 118.80(15) ?
C3 C2 C1 . . 120.18(15) ?
C3 C2 H1 . . 119.9 ?
C1 C2 H1 . . 119.9 ?
C2 C3 C4 . . 121.88(15) ?
C2 C3 H2 . . 119.1 ?
C4 C3 H2 . . 119.1 ?
C3 C4 C5 . . 117.15(15) ?
C3 C4 C15 . . 121.29(14) ?
C5 C4 C15 . . 121.56(15) ?
C8 N1 C9 . . 121.65(14) ?
C8 N1 C12 . . 120.38(14) ?
C9 N1 C12 . . 117.97(14) ?
C6 C5 C4 . . 121.36(16) ?
C6 C5 H3 . . 119.3 ?
C4 C5 H3 . . 119.3 ?
C5 C6 C1 . . 120.44(15) ?
C5 C6 H4 . . 119.8 ?
C1 C6 H4 . . 119.8 ?
O1 C7 C1 . . 123.19(16) ?
O1 C7 C8 . . 118.74(16) ?
C1 C7 C8 . . 117.87(15) ?
O2 C8 N1 . . 125.77(17) ?
O2 C8 C7 . . 116.41(16) ?
N1 C8 C7 . . 117.78(15) ?
N1 C9 C10 . . 111.42(16) ?
N1 C9 C11 . . 111.71(16) ?
C10 C9 C11 . . 111.97(16) ?
N1 C9 H5 . . 107.1 ?
C10 C9 H5 . . 107.1 ?
C11 C9 H5 . . 107.1 ?
C9 C10 H6 . . 109.5 ?
C9 C10 H7 . . 109.5 ?
H6 C10 H7 . . 109.5 ?
C9 C10 H8 . . 109.5 ?
H6 C10 H8 . . 109.5 ?
H7 C10 H8 . . 109.5 ?
C9 C11 H9 . . 109.5 ?
C9 C11 H10 . . 109.5 ?
H9 C11 H10 . . 109.5 ?
C9 C11 H11 . . 109.5 ?
H9 C11 H11 . . 109.5 ?
H10 C11 H11 . . 109.5 ?
N1 C12 C14 . . 111.50(15) ?
N1 C12 C13 . . 111.46(16) ?
C14 C12 C13 . . 113.10(17) ?
N1 C12 H12 . . 106.8 ?
C14 C12 H12 . . 106.8 ?
C13 C12 H12 . . 106.8 ?
C12 C13 H13 . . 109.5 ?
C12 C13 H14 . . 109.5 ?
H13 C13 H14 . . 109.5 ?
C12 C13 H15 . . 109.5 ?
H13 C13 H15 . . 109.5 ?
H14 C13 H15 . . 109.5 ?
C12 C14 H16 . . 109.5 ?
C12 C14 H17 . . 109.5 ?
H16 C14 H17 . . 109.5 ?
C12 C14 H18 . . 109.5 ?
H16 C14 H18 . . 109.5 ?
H17 C14 H18 . . 109.5 ?
C20 C15 C16 . . 117.12(16) ?
C20 C15 C4 . . 121.66(15) ?
C16 C15 C4 . . 121.21(16) ?
C17 C16 C15 . . 121.34(18) ?
C17 C16 H19 . . 119.3 ?
C15 C16 H19 . . 119.3 ?
C18 C17 C16 . . 120.26(18) ?
C18 C17 H20 . . 119.9 ?
C16 C17 H20 . . 119.9 ?
C17 C18 C19 . . 119.54(17) ?
C17 C18 H21 . . 120.2 ?
C19 C18 H21 . . 120.2 ?
C18 C19 C20 . . 120.33(19) ?
C18 C19 H22 . . 119.8 ?
C20 C19 H22 . . 119.8 ?
C19 C20 C15 . . 121.40(17) ?
C19 C20 H23 . . 119.3 ?
C15 C20 H23 . . 119.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C6 . 1.392(3) ?
C1 C2 . 1.398(2) ?
C1 C7 . 1.485(2) ?
C2 C3 . 1.380(2) ?
C2 H1 . 0.9500 ?
C3 C4 . 1.401(2) ?
C3 H2 . 0.9500 ?
C4 C5 . 1.404(2) ?
C4 C15 . 1.494(2) ?
O1 C7 . 1.217(2) ?
O2 C8 . 1.231(2) ?
N1 C8 . 1.342(2) ?
N1 C9 . 1.485(2) ?
N1 C12 . 1.489(2) ?
C5 C6 . 1.388(2) ?
C5 H3 . 0.9500 ?
C6 H4 . 0.9500 ?
C7 C8 . 1.535(2) ?
C9 C10 . 1.519(3) ?
C9 C11 . 1.519(3) ?
C9 H5 . 1.0000 ?
C10 H6 . 0.9800 ?
C10 H7 . 0.9800 ?
C10 H8 . 0.9800 ?
C11 H9 . 0.9800 ?
C11 H10 . 0.9800 ?
C11 H11 . 0.9800 ?
C12 C14 . 1.519(3) ?
C12 C13 . 1.524(3) ?
C12 H12 . 1.0000 ?
C13 H13 . 0.9800 ?
C13 H14 . 0.9800 ?
C13 H15 . 0.9800 ?
C14 H16 . 0.9800 ?
C14 H17 . 0.9800 ?
C14 H18 . 0.9800 ?
C15 C20 . 1.399(3) ?
C15 C16 . 1.404(2) ?
C16 C17 . 1.386(3) ?
C16 H19 . 0.9500 ?
C17 C18 . 1.382(3) ?
C17 H20 . 0.9500 ?
C18 C19 . 1.382(3) ?
C18 H21 . 0.9500 ?
C19 C20 . 1.385(3) ?
C19 H22 . 0.9500 ?
C20 H23 . 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
C9 H5 O1 . 1.00 2.65 3.245(2) 119 yes
C13 H15 O2 . 0.98 2.47 3.033(3) 117 yes
C14 H16 O2 . 0.98 2.51 3.072(3) 116 yes
C14 H18 O1 1_455 0.98 2.71 3.612(3) 154 yes
C17 H20 O2 4_656 0.95 2.66 3.608(2) 179 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 C1 C2 C3 . . . . 1.2(2) ?
C7 C1 C2 C3 . . . . -178.37(15) ?
C1 C2 C3 C4 . . . . 0.3(2) ?
C2 C3 C4 C5 . . . . -1.0(2) ?
C2 C3 C4 C15 . . . . 178.55(15) ?
C3 C4 C5 C6 . . . . 0.2(3) ?
C15 C4 C5 C6 . . . . -179.27(16) ?
C4 C5 C6 C1 . . . . 1.2(3) ?
C2 C1 C6 C5 . . . . -1.9(2) ?
C7 C1 C6 C5 . . . . 177.64(16) ?
C6 C1 C7 O1 . . . . -171.73(18) ?
C2 C1 C7 O1 . . . . 7.8(3) ?
C6 C1 C7 C8 . . . . 3.1(2) ?
C2 C1 C7 C8 . . . . -177.40(15) ?
C9 N1 C8 O2 . . . . 178.42(19) ?
C12 N1 C8 O2 . . . . -2.2(3) ?
C9 N1 C8 C7 . . . . -3.9(2) ?
C12 N1 C8 C7 . . . . 175.50(16) ?
O1 C7 C8 O2 . . . . 97.1(2) ?
C1 C7 C8 O2 . . . . -77.9(2) ?
O1 C7 C8 N1 . . . . -80.7(2) ?
C1 C7 C8 N1 . . . . 104.20(19) ?
C8 N1 C9 C10 . . . . 110.4(2) ?
C12 N1 C9 C10 . . . . -69.1(2) ?
C8 N1 C9 C11 . . . . -123.57(18) ?
C12 N1 C9 C11 . . . . 57.0(2) ?
C8 N1 C12 C14 . . . . 65.9(2) ?
C9 N1 C12 C14 . . . . -114.69(18) ?
C8 N1 C12 C13 . . . . -61.6(2) ?
C9 N1 C12 C13 . . . . 117.88(18) ?
C3 C4 C15 C20 . . . . -179.53(16) ?
C5 C4 C15 C20 . . . . -0.1(2) ?
C3 C4 C15 C16 . . . . -0.4(2) ?
C5 C4 C15 C16 . . . . 179.07(17) ?
C20 C15 C16 C17 . . . . 0.6(3) ?
C4 C15 C16 C17 . . . . -178.57(17) ?
C15 C16 C17 C18 . . . . -1.1(3) ?
C16 C17 C18 C19 . . . . 1.0(3) ?
C17 C18 C19 C20 . . . . -0.3(3) ?
C18 C19 C20 C15 . . . . -0.2(3) ?
C16 C15 C20 C19 . . . . 0.0(2) ?
C4 C15 C20 C19 . . . . 179.20(16) ?
_cod_database_fobs_code 2243842