#------------------------------------------------------------------------------
#$Date: 2016-11-09 04:05:53 +0200 (Wed, 09 Nov 2016) $
#$Revision: 188334 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/19/2241939.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_2241939
loop_
_publ_author_name
'Tabuchi, Yohei'
'Gotoh, Kazuma'
'Ishida, Hiroyuki'
_publ_section_title
;
Crystal structures of hydrogen-bonded co-crystals as liquid crystal
precursors: 4-(n-pentyloxy)benzoic
acid--(E)-1,2-bis(pyridin-4-yl)ethene (2/1) and
4-(n-hexyloxy)benzoic acid--(E)-1,2-bis(pyridin-4-yl)ethene
(2/1)
;
_journal_issue 12
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 1771
_journal_page_last 1775
_journal_paper_doi 10.1107/S2056989016017655
_journal_volume 72
_journal_year 2016
_chemical_formula_iupac '2C12 H16 O3, C12 H10 N2'
_chemical_formula_moiety '2(C12 H16 O3), C12 H10 N2'
_chemical_formula_sum 'C36 H42 N2 O6'
_chemical_formula_weight 598.74
_chemical_name_systematic
'4-(n-Pentyloxy)benzoic acid--(E)-1,2-bis(pyridin-4-yl)ethene (2/1)'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_cell_angle_alpha 80.420(17)
_cell_angle_beta 81.03(2)
_cell_angle_gamma 87.66(3)
_cell_formula_units_Z 1
_cell_length_a 7.406(4)
_cell_length_b 9.042(4)
_cell_length_c 11.719(5)
_cell_measurement_reflns_used 10871
_cell_measurement_temperature 93.0(10)
_cell_measurement_theta_max 29.99
_cell_measurement_theta_min 3.07
_cell_volume 764.3(6)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2006)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2010) and PLATON (Spek, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
Il Milione (Burla et al., 2007)
;
_diffrn_ambient_temperature 93(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Rigaku R-AXIS RAPIDII'
_diffrn_measurement_method \w
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71075
_diffrn_reflns_av_R_equivalents 0.0215
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 9720
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.485
_diffrn_reflns_theta_min 3.072
_diffrn_standards_number 0
_exptl_absorpt_coefficient_mu 0.088
_exptl_absorpt_correction_T_max 0.991
_exptl_absorpt_correction_T_min 0.789
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.301
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 320.00
_exptl_crystal_size_max 0.45
_exptl_crystal_size_mid 0.28
_exptl_crystal_size_min 0.10
_refine_diff_density_max 0.215
_refine_diff_density_min -0.487
_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 204
_refine_ls_number_reflns 3500
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.077
_refine_ls_R_factor_all 0.0443
_refine_ls_R_factor_gt 0.0416
_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^)+(0.0823P)^2^+0.0761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1154
_refine_ls_wR_factor_ref 0.1178
_reflns_number_gt 3146
_reflns_number_total 3500
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file hb7630sup1.cif
_cod_data_source_block I
_cod_original_cell_volume 764.2(6)
_cod_database_code 2241939
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 2 1092.11 21.11
0 0 2 1080.49 20.48
0 0 -2 1084.70 20.98
0 0 -2 1099.46 21.26
0 0 3 316.22 5.53
0 0 3 315.05 5.01
0 0 -3 320.93 5.67
0 0 -3 345.28 5.96
0 0 4 110.03 2.11
0 0 4 109.97 2.12
0 0 -4 113.51 2.20
0 0 -4 111.21 1.76
0 0 5 176.15 2.73
0 0 5 181.17 3.18
0 0 -5 180.18 2.81
0 0 -5 178.61 2.78
0 0 6 573.20 10.04
0 0 -6 599.85 11.13
0 0 -6 596.75 10.53
0 0 7 1.68 0.65
0 0 -7 1.24 0.73
0 0 8 509.06 9.67
0 0 -8 515.58 9.91
0 0 -8 518.39 9.94
0 0 9 8.03 1.03
0 0 -9 8.46 1.12
0 0 -9 8.25 1.12
0 0 10 1233.60 27.07
0 0 -10 1260.33 28.07
0 0 -10 1263.76 28.01
0 0 11 31.77 1.50
0 0 -11 31.92 1.62
0 0 -11 35.05 1.66
0 0 12 120.49 2.30
0 0 -12 123.31 3.17
0 0 -12 119.80 3.09
0 0 13 63.79 1.42
0 0 -13 64.04 1.38
0 0 -13 63.37 2.20
0 0 -13 65.20 2.16
0 0 14 15.05 0.74
0 0 -14 15.07 1.37
0 0 -14 14.33 0.67
0 0 -14 13.83 1.32
0 1 -14 118.31 3.14
0 1 -14 114.68 2.82
0 1 -14 114.30 3.38
0 -1 14 113.58 2.61
0 1 -13 70.17 2.09
0 1 -13 67.28 2.61
0 -1 13 69.31 1.41
0 1 -12 159.15 3.67
0 1 -12 154.33 4.27
0 -1 12 148.58 2.71
0 1 -11 3154.12 86.54
0 1 -11 3139.57 85.69
0 -1 11 3014.99 78.45
0 1 -10 1041.28 23.15
0 1 -10 1068.24 22.83
0 -1 10 1018.56 20.49
0 1 -9 239.27 5.39
0 1 -9 238.44 4.07
0 -1 9 232.51 3.87
0 1 -8 45.66 1.84
0 1 -8 48.17 1.40
0 -1 8 44.89 0.89
0 1 -7 62.49 1.47
0 1 -7 62.12 1.91
0 -1 7 58.57 1.32
0 1 -6 366.11 6.34
0 1 -6 355.50 6.70
0 -1 6 343.87 5.85
0 1 -5 27.12 0.79
0 1 -5 27.35 0.85
0 -1 5 25.68 0.77
0 -1 5 26.40 1.19
0 1 -4 195.08 3.17
0 1 -4 204.81 3.28
0 -1 4 192.89 3.13
0 -1 4 196.99 3.12
0 1 -3 348.50 5.70
0 1 -3 366.12 6.09
0 -1 3 343.06 5.53
0 -1 3 379.52 6.89
0 1 -2 75.78 1.45
0 1 -2 79.90 1.47
0 -1 2 73.10 1.22
0 -1 2 76.21 1.42
0 1 -1 322.48 5.02
0 -1 1 328.99 5.09
0 1 2 2306.32 53.01
0 1 2 2441.25 55.08
0 -1 -2 2348.88 54.80
0 1 3 152.09 2.51
0 1 3 146.44 2.42
0 -1 -3 155.36 2.55
0 -1 -3 150.73 2.32
0 1 4 138.17 2.26
0 1 4 143.39 2.23
0 -1 -4 145.55 2.31
0 -1 -4 140.97 2.32
0 1 5 636.34 11.84
0 1 5 606.42 10.34
0 -1 -5 604.89 10.74
0 -1 -5 640.24 11.39
0 1 6 398.55 7.34
0 -1 -6 399.16 6.86
0 -1 -6 408.14 6.98
0 1 7 2.90 0.47
0 -1 -7 3.25 0.49
0 -1 -7 2.91 0.61
0 1 8 602.81 11.90
0 -1 -8 637.31 11.87
0 -1 -8 604.84 11.29
0 1 9 59.83 1.97
0 -1 -9 60.34 1.41
0 -1 -9 60.43 1.64
0 1 10 47.95 1.22
0 -1 -10 47.43 1.92
0 -1 -10 50.34 1.55
0 1 11 89.56 1.86
0 -1 -11 93.11 2.21
0 -1 -11 92.50 2.68
0 1 12 81.97 2.52
0 -1 -12 82.21 2.10
0 -1 -12 83.12 2.65
0 -1 -12 80.90 1.47
0 1 13 10.41 1.29
0 -1 -13 8.84 0.98
0 -1 -13 8.41 0.48
0 -1 -13 9.69 1.41
0 1 14 6.08 1.26
0 1 14 5.78 1.24
0 -1 -14 7.08 0.76
0 -1 -14 5.43 0.94
0 -1 -14 6.64 1.39
0 2 -14 7.04 0.81
0 2 -14 1.04 1.67
0 2 -13 99.01 3.42
0 2 -13 99.11 3.42
0 2 -13 97.30 2.30
0 -2 13 92.68 2.02
0 2 -12 28.81 2.14
0 2 -12 28.65 1.25
0 -2 12 25.84 1.03
0 2 -11 72.83 2.88
0 2 -11 75.10 1.41
0 -2 11 71.24 1.62
0 2 -10 15.67 1.68
0 -2 10 15.38 0.78
0 2 -9 103.31 2.28
0 -2 9 100.18 1.59
0 2 -8 5.00 0.74
0 2 -8 6.06 0.67
0 -2 8 5.04 0.54
0 2 -7 98.84 2.03
0 2 -7 106.55 1.96
0 -2 7 99.96 1.73
0 2 -6 94.71 2.55
0 -2 6 92.18 1.50
0 2 -5 88.57 2.39
0 -2 5 89.73 1.71
0 -2 5 88.74 1.56
0 2 -4 599.20 11.40
0 -2 4 612.06 11.54
0 -2 4 531.21 9.06
0 2 -3 3651.01 95.47
0 -2 3 3694.61 96.47
0 -2 3 3752.49 95.95
0 2 -2 460.07 7.95
0 -2 2 461.20 7.92
0 2 -1 72.04 1.15
0 2 -1 70.54 2.06
0 -2 1 73.65 1.24
0 -2 1 69.41 1.38
0 2 0 654.20 11.49
0 2 0 665.41 11.82
0 -2 0 681.94 12.08
0 -2 0 665.99 11.72
0 2 1 14.42 0.95
0 2 1 13.91 0.66
0 -2 -1 13.45 0.96
0 2 2 21.54 0.56
0 2 2 20.89 0.56
0 2 2 20.51 0.74
0 -2 -2 20.80 1.27
0 2 3 240.86 4.60
0 -2 -3 245.64 4.01
0 2 4 3809.15 101.16
0 -2 -4 3776.86 99.23
0 2 5 200.91 3.95
0 -2 -5 198.84 3.06
0 -2 -5 209.92 3.49
0 2 6 719.70 13.30
0 -2 -6 680.25 12.40
0 -2 -6 736.69 13.70
0 2 7 4121.07 114.02
0 -2 -7 4144.11 111.30
0 -2 -7 4126.96 112.98
0 2 8 98.27 1.96
0 -2 -8 106.20 1.92
0 -2 -8 98.79 2.71
0 2 9 45.64 1.91
0 -2 -9 46.40 1.19
0 -2 -9 45.90 2.01
0 2 10 71.75 1.69
0 -2 -10 74.80 1.63
0 -2 -10 72.10 2.53
0 2 11 59.41 1.53
0 -2 -11 61.01 1.45
0 -2 -11 60.89 2.39
0 -2 -11 58.27 1.27
0 2 12 151.04 3.91
0 -2 -12 147.42 2.78
0 -2 -12 140.58 2.53
0 -2 -12 147.53 3.95
0 2 13 9.43 1.50
0 -2 -13 8.08 0.61
0 -2 -13 9.48 1.60
0 -2 -13 8.35 0.76
0 2 14 64.96 2.52
0 -2 -14 64.47 2.72
0 2 15 61.80 1.74
0 -2 -15 61.39 2.79
0 3 -13 1.10 0.87
0 3 -12 8.87 0.99
0 -3 12 6.61 0.51
0 3 -11 13.02 1.85
0 -3 11 11.31 0.54
0 3 -10 10.63 1.82
0 -3 10 12.41 0.53
0 3 -9 1.18 1.37
0 -3 9 1.11 0.34
0 3 -8 25.58 1.17
0 -3 8 23.11 0.60
0 3 -7 1637.18 36.39
0 -3 7 1527.85 32.60
0 3 -6 49.75 2.12
0 -3 6 48.35 0.88
0 3 -5 254.17 5.26
0 -3 5 228.41 3.25
0 3 -4 1001.08 19.72
0 -3 4 978.37 19.24
0 3 -3 10.21 0.67
0 -3 3 11.69 0.66
0 3 -2 350.28 6.52
0 -3 2 301.34 4.56
0 -3 2 349.90 5.80
0 3 -1 168.30 2.78
0 3 -1 169.73 2.57
0 -3 1 164.87 2.72
0 -3 1 163.85 2.45
0 3 0 612.16 10.85
0 3 0 604.19 10.61
0 -3 0 611.92 10.81
0 3 1 468.65 8.16
0 3 1 455.49 7.64
0 -3 -1 481.62 8.51
0 3 2 1314.53 26.35
0 3 2 1315.63 27.48
0 -3 -2 1315.30 27.42
0 3 3 390.34 6.16
0 3 3 425.13 7.15
0 3 3 387.88 6.11
0 -3 -3 426.16 7.77
0 3 4 246.92 4.72
0 -3 -4 243.84 4.69
0 3 5 33.99 1.54
0 -3 -5 34.99 1.53
0 3 6 590.59 11.56
0 -3 -6 588.40 11.50
0 3 7 429.93 7.62
0 -3 -7 395.16 6.16
0 -3 -7 428.35 7.58
0 3 8 1.31 1.12
0 -3 -8 1.70 0.64
0 -3 -8 1.55 0.25
0 -3 -8 1.20 0.33
0 3 9 26.16 1.05
0 -3 -9 25.66 0.51
0 -3 -9 26.19 1.07
0 -3 -9 24.91 0.77
0 3 10 73.82 2.67
0 -3 -10 75.61 1.33
0 -3 -10 75.60 2.75
0 -3 -10 74.95 1.27
0 3 11 255.77 4.90
0 -3 -11 257.83 4.06
0 -3 -11 261.16 4.20
0 -3 -11 264.05 6.18
0 3 12 71.02 2.82
0 -3 -12 66.81 2.82
0 -3 -12 69.98 1.28
0 -3 -12 66.47 1.16
0 3 13 0.65 1.38
0 -3 -13 0.80 1.44
0 3 14 11.84 1.04
0 -3 -14 12.51 1.97
0 4 -13 9.32 1.24
0 4 -12 6.07 1.11
0 4 -11 262.23 6.91
0 4 -10 5.53 1.87
0 -4 10 5.86 0.25
0 4 -9 19.14 2.10
0 -4 9 19.20 0.45
0 4 -8 0.79 0.76
0 -4 8 0.68 0.18
0 4 -7 1.02 0.76
0 4 -6 186.68 4.62
0 4 -5 295.64 5.38
0 4 -4 208.69 3.71
0 4 -3 741.02 13.71
0 -4 3 467.89 7.43
0 4 -2 13.54 1.25
0 -4 2 13.85 0.45
0 4 -1 183.28 2.86
0 4 -1 182.45 3.06
0 -4 1 187.53 2.88
0 4 0 350.06 5.92
0 4 0 356.86 6.50
0 -4 0 338.26 5.35
0 4 1 5965.72 177.73
0 4 1 6121.10 183.78
0 -4 -1 6106.85 183.12
0 4 2 644.14 11.44
0 4 2 611.25 10.91
0 -4 -2 618.88 11.00
0 4 3 0.38 0.41
0 4 3 0.16 0.26
0 4 3 0.25 0.72
0 -4 -3 0.09 0.39
0 4 4 0.94 0.23
0 4 4 1.72 0.47
0 4 4 0.81 0.22
0 -4 -4 0.89 0.85
0 4 5 702.13 13.86
0 -4 -5 699.23 13.83
0 4 6 111.16 2.85
0 -4 -6 111.58 2.12
0 4 7 0.23 0.58
0 -4 -7 0.38 0.57
0 4 8 0.10 0.62
0 -4 -8 0.52 1.14
0 4 9 30.65 2.05
0 -4 -9 31.97 2.08
0 4 10 0.57 0.72
0 -4 -10 1.06 1.37
0 4 11 342.33 7.90
0 -4 -11 353.42 6.90
0 4 12 76.64 2.12
0 -4 -12 78.89 2.16
0 4 13 -0.20 1.45
0 -4 -13 -0.12 0.79
0 4 14 75.28 3.32
0 -4 -14 78.18 3.46
0 5 -12 71.28 2.46
0 5 -11 136.82 5.00
0 5 -10 355.78 9.08
0 5 -9 213.11 4.57
0 5 -8 8.09 1.06
0 5 -7 7.13 1.79
0 5 -6 10.42 1.06
0 5 -5 190.26 4.82
0 5 -4 93.53 2.08
0 5 -3 154.24 3.66
0 -5 3 141.82 1.93
0 5 -2 14.75 0.78
0 -5 2 14.87 0.41
0 5 -1 409.67 7.87
0 5 -1 413.76 6.94
0 -5 1 405.79 6.75
0 5 0 177.73 3.55
0 5 0 177.22 3.09
0 -5 0 176.47 2.99
0 5 1 1640.87 35.59
0 5 1 1719.17 37.90
0 -5 -1 1736.91 38.20
0 5 2 41.71 1.11
0 5 2 41.68 1.36
0 -5 -2 40.91 0.91
0 5 3 494.40 8.53
0 5 3 493.99 9.32
0 5 3 491.60 8.41
0 -5 -3 506.96 9.50
0 5 4 28.24 0.88
0 5 4 29.12 0.58
0 5 4 29.93 0.63
0 -5 -4 28.83 0.90
0 5 5 226.92 4.71
0 -5 -5 232.35 4.83
0 5 6 178.72 4.10
0 -5 -6 182.12 3.35
0 5 7 52.21 2.29
0 -5 -7 53.13 1.52
0 5 8 66.77 1.78
0 -5 -8 70.08 2.80
0 5 9 187.32 3.78
0 -5 -9 196.69 5.04
0 5 10 52.53 2.70
0 -5 -10 54.77 1.74
0 5 11 4.95 0.98
0 -5 -11 4.86 1.01
0 5 12 113.07 4.02
0 -5 -12 112.42 4.06
0 5 13 45.01 1.80
0 -5 -13 45.42 2.98
0 5 14 33.79 2.84
0 -5 -14 32.50 2.88
0 6 -11 4.14 2.41
0 6 -10 40.89 1.91
0 6 -9 1.49 1.09
0 6 -8 9.68 2.23
0 6 -7 25.22 1.47
0 6 -6 3.57 1.80
0 6 -5 139.43 3.10
0 6 -4 45.49 2.51
0 6 -3 9.27 0.88
0 -6 3 7.04 0.22
0 6 -2 68.96 1.68
0 -6 2 70.60 1.16
0 6 -1 292.87 4.93
0 6 -1 302.66 6.14
0 -6 1 294.74 4.86
0 6 0 57.62 1.37
0 6 0 58.62 1.87
0 -6 0 57.10 1.30
0 6 1 399.20 7.30
0 6 1 405.22 6.99
0 -6 -1 410.54 7.40
0 6 2 202.99 3.72
0 6 2 197.56 3.84
0 -6 -2 199.53 3.84
0 6 3 80.79 1.58
0 6 3 85.40 1.70
0 6 3 82.36 1.57
0 -6 -3 82.29 1.61
0 6 4 279.99 4.76
0 6 4 279.96 4.58
0 6 4 275.85 5.62
0 -6 -4 278.77 5.64
0 6 5 702.25 12.54
0 6 5 714.87 13.70
0 6 5 692.12 12.40
0 -6 -5 734.24 14.01
0 6 6 255.95 5.80
0 -6 -6 254.44 5.83
0 6 7 25.24 2.30
0 -6 -7 24.64 1.42
0 6 8 2305.74 58.42
0 -6 -8 2302.40 58.76
0 6 9 491.22 9.72
0 -6 -9 505.22 11.30
0 6 10 1.17 0.90
0 -6 -10 1.01 0.89
0 6 11 46.75 2.90
0 -6 -11 45.43 2.93
0 6 12 5.72 1.15
0 -6 -12 7.00 2.13
0 6 13 0.58 1.79
0 -6 -13 0.23 0.99
0 7 -10 0.12 2.03
0 7 -9 93.42 4.46
0 7 -8 13.99 1.49
0 7 -7 38.73 3.26
0 7 -6 1634.42 38.17
0 7 -5 1028.39 24.21
0 7 -4 651.07 13.16
0 7 -3 761.86 14.99
0 -7 3 637.65 11.26
0 7 -2 500.06 10.68
0 -7 2 483.21 8.24
0 7 -1 37.42 1.98
0 7 -1 36.27 0.71
0 -7 1 33.57 0.91
0 7 0 337.24 6.86
0 7 0 331.54 5.98
0 -7 0 330.75 5.85
0 7 1 9.01 0.90
0 7 1 8.15 0.61
0 -7 -1 7.33 0.48
0 7 2 9.77 1.03
0 7 2 10.26 0.98
0 -7 -2 10.69 1.00
0 7 3 22.73 0.88
0 7 3 21.28 1.00
0 7 3 19.60 1.39
0 -7 -3 19.92 0.83
0 7 4 1515.44 32.70
0 7 4 1555.72 33.59
0 7 4 1550.07 35.37
0 -7 -4 1495.53 32.78
0 7 5 1455.57 30.73
0 7 5 1510.83 33.47
0 7 5 1453.31 30.58
0 -7 -5 1591.83 36.48
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9 3 1 9.18 1.75
-9 -3 -1 9.57 2.70
9 3 2 -0.55 1.30
-9 -3 -2 0.09 2.07
9 3 3 18.77 1.95
-9 -3 -3 19.96 1.73
9 3 4 178.65 4.92
-9 -3 -4 186.58 4.81
9 3 5 4.24 1.59
-9 -3 -5 3.56 1.41
9 3 6 43.45 4.16
-9 -3 -6 47.97 3.90
9 4 1 3.86 1.62
-9 -4 -1 4.33 2.48
9 4 2 2.24 1.52
-9 -4 -2 1.61 2.38
9 4 3 63.24 2.85
-9 -4 -3 65.61 4.16
9 4 4 13.64 1.92
-9 -4 -4 14.28 3.01
9 4 5 193.11 5.44
-9 -4 -5 196.40 5.24
;
_shelx_hkl_checksum 65001
_shelx_res_file
;
shelxl.res created by SHELXL-2014/7
TITL 05111517
CELL 0.71075 7.40560 9.04160 11.71860 80.420 81.035 87.663
ZERR 1 0.00390 0.00350 0.00440 0.017 0.021 0.022
LATT 1
SFAC C H O N
UNIT 36 42 6 2
SHEL 99999.000000 0.000000
OMIT -4 -5 3
OMIT -4 -4 3
L.S. 30
FMAP 2
PLAN -20
WPDB -2
HTAB
BOND $H
CONF
LIST 4
TEMP -180.0
ACTA
SIZE 0.450 0.280 0.100
WGHT 0.082300 0.076100
FVAR 1.46440
O1 3 0.631711 0.222910 0.130604 11.00000 0.03475 0.01718 =
0.02099 -0.00813 -0.00818 0.00878
O2 3 0.743014 0.193774 0.300268 11.00000 0.03196 0.01774 =
0.02728 -0.00525 -0.01243 0.00743
O3 3 0.358903 0.845947 0.259406 11.00000 0.02528 0.01275 =
0.01934 -0.00595 -0.00748 0.00606
N1 4 0.777761 -0.033708 0.093552 11.00000 0.02010 0.01340 =
0.02076 -0.00436 -0.00099 0.00133
C1 1 0.582869 0.420400 0.238816 11.00000 0.01565 0.01306 =
0.01623 -0.00252 0.00014 -0.00006
C2 1 0.485718 0.497879 0.154030 11.00000 0.02203 0.01604 =
0.01333 -0.00396 -0.00123 0.00070
AFIX 43
H2 2 0.467678 0.451885 0.089542 11.00000 -1.20000
AFIX 0
C3 1 0.415218 0.640283 0.162075 11.00000 0.02134 0.01562 =
0.01481 -0.00170 -0.00386 0.00259
AFIX 43
H3 2 0.351478 0.692288 0.102755 11.00000 -1.20000
AFIX 0
C4 1 0.438150 0.707456 0.257941 11.00000 0.01579 0.01205 =
0.01735 -0.00264 -0.00071 0.00049
C5 1 0.534736 0.631449 0.343687 11.00000 0.01747 0.01615 =
0.01747 -0.00567 -0.00407 0.00030
AFIX 43
H5 2 0.551467 0.676859 0.408723 11.00000 -1.20000
AFIX 0
C6 1 0.606482 0.488607 0.333375 11.00000 0.01565 0.01558 =
0.01773 -0.00209 -0.00390 0.00083
AFIX 43
H6 2 0.672433 0.437073 0.391713 11.00000 -1.20000
AFIX 0
C7 1 0.661503 0.267964 0.227651 11.00000 0.01732 0.01463 =
0.01754 -0.00309 -0.00059 -0.00003
C8 1 0.372846 0.919035 0.357749 11.00000 0.01935 0.01387 =
0.01769 -0.00502 -0.00507 0.00237
AFIX 23
H8A 2 0.499944 0.951490 0.354220 11.00000 -1.20000
H8B 2 0.338866 0.849035 0.431862 11.00000 -1.20000
AFIX 0
C9 1 0.244062 1.053853 0.352573 11.00000 0.01965 0.01281 =
0.01854 -0.00428 -0.00572 0.00371
AFIX 23
H9A 2 0.118861 1.021454 0.350020 11.00000 -1.20000
H9B 2 0.283325 1.126131 0.280507 11.00000 -1.20000
AFIX 0
C10 1 0.243762 1.129760 0.459970 11.00000 0.02384 0.01501 =
0.01738 -0.00433 -0.00564 0.00467
AFIX 23
H10A 2 0.233902 1.051627 0.530593 11.00000 -1.20000
H10B 2 0.362057 1.180317 0.452698 11.00000 -1.20000
AFIX 0
C11 1 0.088890 1.244970 0.477051 11.00000 0.02297 0.01750 =
0.01912 -0.00430 0.00010 0.00386
AFIX 23
H11A 2 -0.029202 1.195313 0.481247 11.00000 -1.20000
H11B 2 0.089666 1.279346 0.552887 11.00000 -1.20000
AFIX 0
C12 1 0.101026 1.380690 0.381014 11.00000 0.02101 0.01660 =
0.02744 -0.00228 -0.00104 0.00454
AFIX 137
H12A 2 0.219062 1.429070 0.374451 11.00000 -1.50000
H12B 2 0.001938 1.451852 0.400034 11.00000 -1.50000
H12C 2 0.089922 1.348881 0.306475 11.00000 -1.50000
AFIX 0
C13 1 0.868236 -0.116352 0.172383 11.00000 0.02249 0.01777 =
0.01900 -0.00774 -0.00178 0.00123
AFIX 43
H13 2 0.881571 -0.077533 0.241072 11.00000 -1.20000
AFIX 0
C14 1 0.943458 -0.256087 0.158448 11.00000 0.02090 0.01727 =
0.01778 -0.00374 -0.00471 0.00321
AFIX 43
H14 2 1.006659 -0.311253 0.216792 11.00000 -1.20000
AFIX 0
C15 1 0.925939 -0.315537 0.058149 11.00000 0.01684 0.01327 =
0.01756 -0.00365 -0.00078 0.00067
C16 1 0.832930 -0.227735 -0.024407 11.00000 0.02739 0.01528 =
0.01919 -0.00576 -0.00646 0.00384
AFIX 43
H16 2 0.818881 -0.262892 -0.094486 11.00000 -1.20000
AFIX 0
C17 1 0.761354 -0.089412 -0.003755 11.00000 0.02599 0.01483 =
0.02152 -0.00345 -0.00567 0.00422
AFIX 43
H17 2 0.697935 -0.031282 -0.060671 11.00000 -1.20000
AFIX 0
C18 1 1.003750 -0.464687 0.044977 11.00000 0.02245 0.01346 =
0.01925 -0.00306 -0.00525 0.00441
AFIX 43
H18 2 1.064881 -0.515247 0.106119 11.00000 -1.20000
AFIX 0
H1 2 0.689408 0.120911 0.120614 11.00000 0.09162
HKLF 4
REM 05111517
REM R1 = 0.0416 for 3146 Fo > 4sig(Fo) and 0.0443 for all 3500 data
REM 204 parameters refined using 0 restraints
END
WGHT 0.0823 0.0761
REM Instructions for potential hydrogen bonds
HTAB O1 N1
REM Highest difference peak 0.215, deepest hole -0.487, 1-sigma level 0.113
Q1 1 0.3219 1.1649 0.2253 11.00000 0.05 0.21
Q2 1 1.0322 -0.0047 0.0237 11.00000 0.05 0.21
Q3 1 0.6504 0.6333 0.1419 11.00000 0.05 0.21
Q4 1 0.4649 1.2711 0.4042 11.00000 0.05 0.20
Q5 1 0.2721 1.3934 0.3175 11.00000 0.05 0.20
Q6 1 0.7237 0.4060 0.0560 11.00000 0.05 0.20
Q7 1 0.2770 1.4917 0.3970 11.00000 0.05 0.19
Q8 1 0.3672 1.2461 0.3202 11.00000 0.05 0.19
Q9 1 0.2116 1.3620 0.2835 11.00000 0.05 0.19
Q10 1 0.2509 1.4642 0.4194 11.00000 0.05 0.19
Q11 1 0.5076 0.9037 0.1857 11.00000 0.05 0.19
Q12 1 0.0856 0.9544 0.5855 11.00000 0.05 0.19
Q13 1 0.2517 1.5983 0.4303 11.00000 0.05 0.18
Q14 1 0.8846 0.3099 0.1033 11.00000 0.05 0.18
Q15 1 0.6634 0.5490 0.0776 11.00000 0.05 0.18
Q16 1 0.2197 0.7720 0.0244 11.00000 0.05 0.18
Q17 1 0.3440 0.5008 0.4358 11.00000 0.05 0.18
Q18 1 0.5263 0.8539 0.1073 11.00000 0.05 0.18
Q19 1 -0.0226 0.9358 0.4228 11.00000 0.05 0.18
Q20 1 0.9644 0.2130 0.0999 11.00000 0.05 0.18
;
_shelx_res_checksum 40949
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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 0.63171(10) 0.22291(7) 0.13060(6) 0.02355(18) Uani d 1
H H1 0.689(3) 0.121(2) 0.1206(19) 0.092(7) Uiso d 1
O O2 0.74301(10) 0.19377(7) 0.30027(6) 0.02484(18) Uani d 1
O O3 0.35890(9) 0.84595(7) 0.25941(5) 0.01847(16) Uani d 1
N N1 0.77776(10) -0.03371(8) 0.09355(7) 0.01817(18) Uani d 1
C C1 0.58287(11) 0.42040(9) 0.23882(7) 0.01524(19) Uani d 1
C C2 0.48572(12) 0.49788(9) 0.15403(7) 0.01714(19) Uani d 1
H H2 0.4677 0.4519 0.0895 0.021 Uiso calc 1
C C3 0.41522(12) 0.64028(9) 0.16208(7) 0.01730(19) Uani d 1
H H3 0.3515 0.6923 0.1028 0.021 Uiso calc 1
C C4 0.43815(11) 0.70746(9) 0.25794(7) 0.01525(19) Uani d 1
C C5 0.53474(11) 0.63145(9) 0.34369(7) 0.01655(19) Uani d 1
H H5 0.5515 0.6769 0.4087 0.020 Uiso calc 1
C C6 0.60648(11) 0.48861(9) 0.33337(7) 0.01627(19) Uani d 1
H H6 0.6724 0.4371 0.3917 0.020 Uiso calc 1
C C7 0.66150(11) 0.26796(9) 0.22765(7) 0.01667(19) Uani d 1
C C8 0.37285(12) 0.91903(9) 0.35775(7) 0.01651(19) Uani d 1
H H8A 0.4999 0.9515 0.3542 0.020 Uiso calc 1
H H8B 0.3389 0.8490 0.4319 0.020 Uiso calc 1
C C9 0.24406(12) 1.05385(9) 0.35257(7) 0.01660(19) Uani d 1
H H9A 0.1189 1.0215 0.3500 0.020 Uiso calc 1
H H9B 0.2833 1.1261 0.2805 0.020 Uiso calc 1
C C10 0.24376(12) 1.12976(9) 0.45997(7) 0.01841(19) Uani d 1
H H10A 0.2339 1.0516 0.5306 0.022 Uiso calc 1
H H10B 0.3621 1.1803 0.4527 0.022 Uiso calc 1
C C11 0.08889(12) 1.24497(10) 0.47705(7) 0.0202(2) Uani d 1
H H11A -0.0292 1.1953 0.4812 0.024 Uiso calc 1
H H11B 0.0897 1.2793 0.5529 0.024 Uiso calc 1
C C12 0.10103(12) 1.38069(10) 0.38101(8) 0.0223(2) Uani d 1
H H12A 0.2191 1.4291 0.3745 0.033 Uiso calc 1
H H12B 0.0019 1.4519 0.4000 0.033 Uiso calc 1
H H12C 0.0899 1.3489 0.3065 0.033 Uiso calc 1
C C13 0.86824(12) -0.11635(10) 0.17238(8) 0.01939(19) Uani d 1
H H13 0.8816 -0.0775 0.2411 0.023 Uiso calc 1
C C14 0.94346(12) -0.25609(10) 0.15845(7) 0.01845(19) Uani d 1
H H14 1.0067 -0.3113 0.2168 0.022 Uiso calc 1
C C15 0.92594(11) -0.31554(9) 0.05815(7) 0.01598(19) Uani d 1
C C16 0.83293(13) -0.22774(10) -0.02441(8) 0.0201(2) Uani d 1
H H16 0.8189 -0.2629 -0.0945 0.024 Uiso calc 1
C C17 0.76135(13) -0.08941(10) -0.00375(8) 0.0206(2) Uani d 1
H H17 0.6979 -0.0313 -0.0607 0.025 Uiso calc 1
C C18 1.00375(12) -0.46469(9) 0.04498(7) 0.0182(2) Uani d 1
H H18 1.0649 -0.5152 0.1061 0.022 Uiso calc 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.0347(4) 0.0172(3) 0.0210(3) 0.0088(3) -0.0082(3) -0.0081(3)
O2 0.0320(4) 0.0177(3) 0.0273(4) 0.0074(3) -0.0124(3) -0.0053(3)
O3 0.0253(3) 0.0128(3) 0.0193(3) 0.0061(2) -0.0075(2) -0.0059(2)
N1 0.0201(4) 0.0134(3) 0.0208(4) 0.0013(3) -0.0010(3) -0.0044(3)
C1 0.0156(4) 0.0131(4) 0.0162(4) -0.0001(3) 0.0001(3) -0.0025(3)
C2 0.0220(4) 0.0160(4) 0.0133(4) 0.0007(3) -0.0012(3) -0.0040(3)
C3 0.0213(4) 0.0156(4) 0.0148(4) 0.0026(3) -0.0039(3) -0.0017(3)
C4 0.0158(4) 0.0121(4) 0.0173(4) 0.0005(3) -0.0007(3) -0.0026(3)
C5 0.0175(4) 0.0162(4) 0.0175(4) 0.0003(3) -0.0041(3) -0.0057(3)
C6 0.0157(4) 0.0156(4) 0.0177(4) 0.0008(3) -0.0039(3) -0.0021(3)
C7 0.0173(4) 0.0146(4) 0.0175(4) 0.0000(3) -0.0006(3) -0.0031(3)
C8 0.0193(4) 0.0139(4) 0.0177(4) 0.0024(3) -0.0051(3) -0.0050(3)
C9 0.0196(4) 0.0128(4) 0.0185(4) 0.0037(3) -0.0057(3) -0.0043(3)
C10 0.0238(4) 0.0150(4) 0.0174(4) 0.0047(3) -0.0056(3) -0.0043(3)
C11 0.0230(4) 0.0175(4) 0.0191(4) 0.0039(3) 0.0001(3) -0.0043(3)
C12 0.0210(4) 0.0166(4) 0.0274(5) 0.0045(3) -0.0010(3) -0.0023(3)
C13 0.0225(4) 0.0178(4) 0.0190(4) 0.0012(3) -0.0018(3) -0.0077(3)
C14 0.0209(4) 0.0173(4) 0.0178(4) 0.0032(3) -0.0047(3) -0.0037(3)
C15 0.0168(4) 0.0133(4) 0.0176(4) 0.0007(3) -0.0008(3) -0.0036(3)
C16 0.0274(5) 0.0153(4) 0.0192(4) 0.0038(3) -0.0065(3) -0.0058(3)
C17 0.0260(5) 0.0148(4) 0.0215(4) 0.0042(3) -0.0057(3) -0.0035(3)
C18 0.0224(4) 0.0135(4) 0.0193(4) 0.0044(3) -0.0052(3) -0.0031(3)
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'
O O 0.0106 0.0060 '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'
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
C7 O1 H1 . 113.0(12)
C4 O3 C8 . 117.75(7)
C13 N1 C17 . 117.92(8)
C6 C1 C2 . 118.70(8)
C6 C1 C7 . 120.67(8)
C2 C1 C7 . 120.62(8)
C3 C2 C1 . 121.24(8)
C3 C2 H2 . 119.4
C1 C2 H2 . 119.4
C2 C3 C4 . 119.68(8)
C2 C3 H3 . 120.2
C4 C3 H3 . 120.2
O3 C4 C5 . 125.07(8)
O3 C4 C3 . 115.09(7)
C5 C4 C3 . 119.84(8)
C6 C5 C4 . 119.63(8)
C6 C5 H5 . 120.2
C4 C5 H5 . 120.2
C1 C6 C5 . 120.90(8)
C1 C6 H6 . 119.5
C5 C6 H6 . 119.5
O2 C7 O1 . 124.03(8)
O2 C7 C1 . 123.45(8)
O1 C7 C1 . 112.52(8)
O3 C8 C9 . 107.92(7)
O3 C8 H8A . 110.1
C9 C8 H8A . 110.1
O3 C8 H8B . 110.1
C9 C8 H8B . 110.1
H8A C8 H8B . 108.4
C8 C9 C10 . 110.10(7)
C8 C9 H9A . 109.6
C10 C9 H9A . 109.6
C8 C9 H9B . 109.6
C10 C9 H9B . 109.6
H9A C9 H9B . 108.2
C11 C10 C9 . 114.03(7)
C11 C10 H10A . 108.7
C9 C10 H10A . 108.7
C11 C10 H10B . 108.7
C9 C10 H10B . 108.7
H10A C10 H10B . 107.6
C12 C11 C10 . 114.07(8)
C12 C11 H11A . 108.7
C10 C11 H11A . 108.7
C12 C11 H11B . 108.7
C10 C11 H11B . 108.7
H11A C11 H11B . 107.6
C11 C12 H12A . 109.5
C11 C12 H12B . 109.5
H12A C12 H12B . 109.5
C11 C12 H12C . 109.5
H12A C12 H12C . 109.5
H12B C12 H12C . 109.5
N1 C13 C14 . 122.91(8)
N1 C13 H13 . 118.5
C14 C13 H13 . 118.5
C13 C14 C15 . 119.64(8)
C13 C14 H14 . 120.2
C15 C14 H14 . 120.2
C16 C15 C14 . 117.09(8)
C16 C15 C18 . 123.67(8)
C14 C15 C18 . 119.25(8)
C17 C16 C15 . 119.71(8)
C17 C16 H16 . 120.1
C15 C16 H16 . 120.1
N1 C17 C16 . 122.73(8)
N1 C17 H17 . 118.6
C16 C17 H17 . 118.6
C18 C18 C15 2_745 125.75(10)
C18 C18 H18 2_745 117.1
C15 C18 H18 . 117.1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
O1 C7 . 1.3220(11)
O1 H1 . 1.02(2)
O2 C7 . 1.2147(12)
O3 C4 . 1.3626(11)
O3 C8 . 1.4393(10)
N1 C13 . 1.3353(12)
N1 C17 . 1.3446(12)
C1 C6 . 1.3912(12)
C1 C2 . 1.3948(13)
C1 C7 . 1.4922(12)
C2 C3 . 1.3819(12)
C2 H2 . 0.9500
C3 C4 . 1.3981(12)
C3 H3 . 0.9500
C4 C5 . 1.3956(13)
C5 C6 . 1.3932(12)
C5 H5 . 0.9500
C6 H6 . 0.9500
C8 C9 . 1.5158(12)
C8 H8A . 0.9900
C8 H8B . 0.9900
C9 C10 . 1.5302(12)
C9 H9A . 0.9900
C9 H9B . 0.9900
C10 C11 . 1.5300(13)
C10 H10A . 0.9900
C10 H10B . 0.9900
C11 C12 . 1.5160(13)
C11 H11A . 0.9900
C11 H11B . 0.9900
C12 H12A . 0.9800
C12 H12B . 0.9800
C12 H12C . 0.9800
C13 C14 . 1.3843(13)
C13 H13 . 0.9500
C14 C15 . 1.3967(12)
C14 H14 . 0.9500
C15 C16 . 1.3957(13)
C15 C18 . 1.4672(13)
C16 C17 . 1.3822(13)
C16 H16 . 0.9500
C17 H17 . 0.9500
C18 C18 2_745 1.3294(17)
C18 H18 . 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
O1 H1 N1 . 1.016(19) 1.580(19) 2.5936(17) 175(2) yes
C12 H12A Cg1 1_565 0.98 2.64 3.592(2) 151 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_4
_geom_torsion
C6 C1 C2 C3 . 0.67(13)
C7 C1 C2 C3 . -178.73(7)
C1 C2 C3 C4 . -1.26(13)
C8 O3 C4 C5 . -1.08(12)
C8 O3 C4 C3 . 178.12(7)
C2 C3 C4 O3 . -178.11(7)
C2 C3 C4 C5 . 1.13(13)
O3 C4 C5 C6 . 178.72(7)
C3 C4 C5 C6 . -0.45(13)
C2 C1 C6 C5 . 0.03(13)
C7 C1 C6 C5 . 179.43(7)
C4 C5 C6 C1 . -0.14(13)
C6 C1 C7 O2 . 2.64(13)
C2 C1 C7 O2 . -177.97(8)
C6 C1 C7 O1 . -177.67(7)
C2 C1 C7 O1 . 1.72(12)
C4 O3 C8 C9 . -168.61(7)
O3 C8 C9 C10 . 176.17(6)
C8 C9 C10 C11 . -167.30(7)
C9 C10 C11 C12 . -65.22(10)
C17 N1 C13 C14 . -0.60(14)
N1 C13 C14 C15 . 0.09(14)
C13 C14 C15 C16 . 0.60(13)
C13 C14 C15 C18 . -179.09(8)
C14 C15 C16 C17 . -0.78(14)
C18 C15 C16 C17 . 178.90(8)
C13 N1 C17 C16 . 0.40(14)
C15 C16 C17 N1 . 0.30(15)
C16 C15 C18 C18 2_745 -0.19(18)
C14 C15 C18 C18 2_745 179.49(11)
_cod_database_fobs_code 2241939