#------------------------------------------------------------------------------
#$Date: 2024-08-07 01:03:54 +0300 (Wed, 07 Aug 2024) $
#$Revision: 293987 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023152.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_2023152
loop_
_publ_author_name
'Kumagai, Hitoshi'
'Kawata, Satoshi'
'Ogihara, Nobuhiro'
_publ_section_title
;
Crystal structures of 1,1'-bis-(carb-oxy-meth-yl)-4,4'-bipyridinium
derivatives.
;
_journal_coeditor_code JP2007
_journal_issue 'Pt 7'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 695
_journal_page_last 698
_journal_paper_doi 10.1107/S2056989024005127
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac 'C14 H13 N2 O4.5 +, B F4 -'
_chemical_formula_moiety 'C14 H13 N2 O4.5 +, B F4 -'
_chemical_formula_sum 'C14 H14 B F4 N2 O4.5'
_chemical_formula_weight 368.08
_chemical_name_systematic
;
2-[1'-(Carboxymethyl)-4,4'-bipyridine-1,1'-diium-1-yl]acetate
tetrafluoroborate
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 90
_cell_angle_beta 95.123(3)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 7.6794(16)
_cell_length_b 20.987(4)
_cell_length_c 10.0514(19)
_cell_measurement_reflns_used 2543
_cell_measurement_temperature 100
_cell_measurement_theta_max 27.41
_cell_measurement_theta_min 5.63
_cell_volume 1613.5(5)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 1995)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 1995)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 1995)
;
_computing_molecular_graphics
;
Yadokari-XG 2009 (Kabuto et al., 2009)
;
_computing_publication_material
;
Yadokari-XG 2009 (Kabuto et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
Il Milione (Burla et al., 2007)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type 'Rigaku R-AXIS RAPID'
_diffrn_measurement_method \w
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71075
_diffrn_reflns_av_R_equivalents 0.0318
_diffrn_reflns_av_unetI/netI 0.0274
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_number 15631
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.427
_diffrn_reflns_theta_min 3.204
_exptl_absorpt_coefficient_mu 0.141
_exptl_absorpt_correction_T_max 0.987
_exptl_absorpt_correction_T_min 0.656
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Rigaku, 1995)
;
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.519
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description platelet
_exptl_crystal_F_000 756
_exptl_crystal_size_max 0.600
_exptl_crystal_size_mid 0.400
_exptl_crystal_size_min 0.400
_refine_diff_density_max 0.721
_refine_diff_density_min -0.560
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.051
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 292
_refine_ls_number_reflns 3652
_refine_ls_number_restraints 1
_refine_ls_restrained_S_all 1.051
_refine_ls_R_factor_all 0.0589
_refine_ls_R_factor_gt 0.0510
_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^)+(0.0594P)^2^+1.2013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1255
_refine_ls_wR_factor_ref 0.1315
_reflns_number_gt 3119
_reflns_number_total 3652
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jp2007.cif
_cod_data_source_block HbcbpyBF4
_cod_depositor_comments
'Adding full bibliography for 2023152--2023153.cif.'
_cod_original_formula_sum 'C14 H14 B F4 N2 O4.50'
_cod_database_code 2023152
_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 0.920
_shelx_estimated_absorpt_t_max 0.946
_shelx_hkl_file
;
0 0 2 2119.51 70.11
0 0 -2 2123.41 69.76
0 0 -2 2033.11 69.34
0 0 3 -0.51 0.41
0 0 -3 -1.42 0.99
0 0 -3 -0.60 0.35
0 0 4 112.28 3.01
0 0 -4 108.01 2.16
0 0 -4 108.95 3.79
0 0 5 0.09 0.59
0 0 -5 -0.33 0.55
0 0 -5 -0.42 0.88
0 0 6 543.54 16.06
0 0 6 535.14 14.19
0 0 -6 535.88 14.39
0 0 -6 549.80 14.18
0 0 7 0.10 0.99
0 0 7 0.02 0.66
0 0 -7 0.75 0.65
0 0 8 403.51 13.22
0 0 8 386.30 11.17
0 0 -8 393.01 10.07
0 0 9 -0.69 0.83
0 0 9 0.82 1.23
0 0 -9 0.40 0.50
0 0 10 73.94 3.09
0 0 10 61.56 2.36
0 0 -10 58.83 2.25
0 0 11 0.69 1.01
0 0 11 0.00 0.67
0 0 -11 2.07 1.05
0 0 12 49.56 2.83
0 0 12 40.04 2.95
0 0 -12 27.17 2.91
0 -1 2 1856.42 62.02
0 1 2 1883.16 58.69
0 -1 2 1818.43 58.43
0 1 2 1793.85 59.23
0 1 -2 1850.26 61.00
0 -1 -2 1797.80 59.32
0 -1 -2 1907.41 59.47
0 -1 3 3822.76 171.29
0 1 3 3930.11 171.07
0 1 3 3772.89 173.45
0 -1 3 3659.99 166.80
0 -1 -3 3987.31 173.17
0 1 -3 3915.44 174.12
0 -1 -3 3744.82 168.80
0 1 4 19.83 1.16
0 -1 4 21.66 1.44
0 1 4 22.06 1.13
0 -1 4 16.10 1.02
0 -1 -4 23.44 1.93
0 -1 -4 21.61 1.02
0 1 -4 21.58 1.29
0 -1 5 86.62 3.30
0 1 5 89.82 3.49
0 1 5 86.41 2.30
0 -1 5 85.88 2.74
0 -1 -5 86.26 3.59
0 1 -5 89.55 2.65
0 -1 -5 89.60 2.30
0 -1 6 159.47 4.36
0 1 6 163.20 3.92
0 -1 6 161.75 4.96
0 1 6 157.68 4.09
0 1 -6 157.64 4.21
0 -1 -6 151.99 3.73
0 -1 -6 152.12 5.23
0 -1 7 13.24 1.23
0 -1 7 11.57 1.60
0 1 7 10.37 1.01
0 1 7 10.94 1.68
0 -1 -7 11.15 1.74
0 1 -7 11.74 1.19
0 -1 -7 9.66 1.01
0 -1 8 44.53 2.29
0 1 8 42.09 1.96
0 -1 8 44.42 2.88
0 1 8 44.86 3.12
0 -1 -8 40.15 1.94
0 1 -8 45.31 2.35
0 1 9 11.78 1.33
0 -1 9 11.43 1.99
0 1 9 9.44 1.30
0 1 -9 9.89 1.46
0 -1 -9 9.59 1.28
0 -1 10 0.08 1.07
0 -1 10 0.80 1.42
0 1 10 -0.17 1.52
0 1 10 -0.69 0.92
0 1 -10 0.84 1.00
0 -1 -10 1.53 0.87
0 -1 11 1.00 1.20
0 -1 11 2.58 1.64
0 1 11 1.07 1.04
0 1 11 2.75 1.69
0 -1 -11 0.31 1.03
0 1 -11 -0.11 1.17
0 -1 12 71.57 4.83
0 -1 12 53.99 3.67
0 1 12 68.96 4.94
0 1 12 55.31 3.35
0 1 -12 51.26 3.59
0 -1 -12 44.14 2.35
0 2 2 1568.52 50.23
0 -2 2 1604.80 50.15
0 -2 -2 1746.70 50.82
0 -2 -2 1553.55 52.53
0 2 -2 1641.42 51.21
0 -2 3 726.80 20.20
0 2 3 802.26 18.82
0 -2 3 734.11 20.53
0 2 3 742.88 22.46
0 2 -3 716.12 18.32
0 -2 -3 752.07 20.26
0 -2 -3 851.83 19.70
0 2 4 5.12 1.44
0 2 4 5.26 0.63
0 -2 4 5.83 1.09
0 -2 4 6.25 0.71
0 -2 -4 8.11 0.63
0 -2 -4 4.75 1.47
0 -2 5 88.45 3.00
0 -2 5 96.34 2.43
0 2 5 95.75 3.79
0 2 5 91.39 2.20
0 2 -5 90.68 2.22
0 -2 -5 91.19 2.19
0 -2 -5 94.82 2.77
0 2 6 29.70 1.20
0 2 6 32.04 1.48
0 -2 6 31.46 1.72
0 -2 6 31.67 1.93
0 -2 -6 30.14 2.35
0 -2 -6 29.65 1.20
0 2 -6 32.02 1.14
0 2 7 -0.33 1.16
0 -2 7 0.61 1.00
0 2 7 0.16 0.58
0 -2 7 0.79 0.82
0 -2 -7 -0.22 1.15
0 2 -7 0.67 0.52
0 -2 -7 1.35 0.57
0 2 8 0.18 0.61
0 2 8 -0.67 0.72
0 -2 8 -0.08 1.01
0 -2 8 -0.51 0.83
0 -2 -8 0.10 1.18
0 -2 -8 0.35 0.60
0 2 -8 0.33 0.52
0 2 9 4.61 0.66
0 -2 9 5.21 1.02
0 2 9 5.43 1.84
0 -2 9 5.27 1.33
0 -2 -9 7.10 1.01
0 -2 -9 0.37 1.16
0 2 -9 6.39 0.85
0 2 10 27.16 1.30
0 -2 10 31.56 1.92
0 2 10 33.67 3.18
0 -2 10 27.83 2.39
0 -2 -10 22.29 1.83
0 2 -10 23.92 1.56
0 -2 11 1.61 0.99
0 2 11 0.14 1.14
0 2 11 1.15 0.99
0 -2 11 1.48 1.33
0 -2 -11 0.70 0.98
0 2 -11 1.47 0.78
0 2 12 -0.08 0.62
0 2 12 -0.09 1.10
0 -2 12 -0.85 0.96
0 -2 12 -0.23 1.22
0 2 -12 0.19 1.23
0 -2 -12 -0.01 0.93
0 3 1 1575.92 51.33
0 -3 1 1611.31 49.00
0 3 1 1672.93 45.95
0 -3 -1 1527.83 47.39
0 3 -1 1563.89 49.78
0 -3 -1 1686.65 45.93
0 3 2 497.09 12.12
0 -3 2 498.36 13.15
0 -3 -2 491.56 14.04
0 3 -2 492.41 11.55
0 -3 -2 561.24 9.97
0 3 3 693.65 14.48
0 -3 3 611.99 15.47
0 3 3 614.59 18.20
0 -3 -3 707.67 15.25
0 3 -3 614.84 15.45
0 -3 -3 629.60 16.51
0 3 4 -0.61 0.63
0 -3 4 0.10 0.43
0 -3 4 -0.95 0.78
0 3 4 -0.34 0.45
0 3 -4 0.00 0.48
0 -3 -4 0.43 0.32
0 -3 -4 0.14 0.62
0 3 5 702.34 19.48
0 -3 5 679.20 19.78
0 3 5 708.57 17.20
0 -3 5 704.89 19.96
0 -3 -5 709.88 17.26
0 3 -5 700.30 19.94
0 -3 -5 691.60 19.73
0 -3 6 51.50 1.66
0 -3 6 50.23 2.38
0 3 6 51.76 1.46
0 3 6 52.51 2.02
0 -3 -6 53.12 1.45
0 -3 -6 52.21 3.11
0 3 -6 51.72 2.36
0 -3 7 67.01 2.08
0 3 7 67.87 3.53
0 -3 7 72.28 3.05
0 3 7 66.62 1.95
0 -3 -7 69.42 1.96
0 3 -7 65.73 2.85
0 -3 -7 68.84 3.69
0 -3 8 14.33 1.20
0 -3 8 14.19 1.08
0 3 8 15.12 1.39
0 3 8 15.03 1.10
0 -3 -8 13.28 2.27
0 -3 -8 13.01 1.06
0 3 -8 14.00 1.68
0 -3 9 61.02 2.43
0 3 9 57.79 2.30
0 -3 9 58.24 2.28
0 3 9 62.70 4.11
0 3 -9 59.58 3.18
0 -3 -9 57.83 4.19
0 -3 -9 55.33 2.24
0 -3 10 107.52 3.83
0 3 10 100.40 3.74
0 3 10 117.20 4.54
0 -3 10 114.70 5.38
0 -3 -10 104.33 3.82
0 3 -10 104.61 4.89
0 -3 11 77.88 3.24
0 3 11 68.96 2.42
0 -3 11 83.17 4.79
0 3 11 82.30 5.44
0 3 -11 74.87 4.25
0 -3 -11 59.38 2.99
0 -3 12 0.80 0.96
0 3 12 2.42 2.14
0 -3 12 1.50 1.73
0 -3 -12 1.04 1.03
0 3 -12 2.01 0.94
0 4 0 9265.50 591.68
0 -4 0 9440.12 602.01
0 -4 1 272.99 6.69
0 4 1 290.93 4.66
0 4 -1 249.60 6.70
0 -4 -1 285.34 4.79
0 -4 -1 246.68 7.07
0 -4 2 230.76 6.36
0 4 2 228.51 5.46
0 4 -2 226.79 5.09
0 -4 -2 232.65 5.46
0 -4 3 832.01 22.77
0 4 3 837.47 23.52
0 -4 -3 946.88 21.03
0 4 -3 828.24 22.48
0 -4 -3 835.93 25.93
0 -4 4 231.66 6.73
0 4 4 229.17 4.21
0 4 4 231.79 7.46
0 -4 4 228.22 4.90
0 -4 -4 218.91 3.90
0 4 -4 239.71 6.72
0 -4 -4 230.99 5.89
0 -4 5 165.13 4.65
0 4 5 160.56 4.31
0 -4 5 165.81 5.03
0 4 5 164.87 3.04
0 4 -5 168.21 5.09
0 -4 -5 162.16 5.93
0 -4 -5 169.00 3.17
0 4 6 683.38 19.80
0 -4 6 676.80 20.78
0 -4 6 704.03 20.37
0 4 6 695.15 17.22
0 -4 -6 691.80 20.56
0 -4 -6 689.12 17.11
0 4 -6 680.15 20.55
0 -4 7 81.40 2.54
0 -4 7 85.89 3.40
0 4 7 89.68 2.18
0 4 7 87.12 4.18
0 -4 -7 87.53 4.31
0 -4 -7 81.96 2.11
0 4 -7 82.97 3.49
0 -4 8 2.36 0.82
0 4 8 5.57 1.69
0 -4 8 4.37 0.81
0 4 8 3.69 0.68
0 -4 -8 3.47 1.08
0 4 -8 3.21 1.31
0 -4 -8 2.44 0.70
0 -4 9 21.09 1.45
0 -4 9 24.59 2.34
0 4 9 21.04 1.29
0 4 9 25.13 1.93
0 -4 -9 22.40 1.93
0 -4 -9 20.95 1.31
0 4 -9 24.23 2.29
0 4 10 17.14 3.10
0 -4 10 19.84 1.52
0 -4 10 20.00 2.41
0 4 10 17.09 1.41
0 -4 -10 26.31 2.05
0 -4 -10 16.61 1.38
0 4 -10 22.14 2.38
0 -4 11 -0.58 1.30
0 4 11 -0.71 0.48
0 4 11 0.73 1.75
0 -4 11 1.49 0.84
0 4 -11 -2.08 1.25
0 -4 -11 0.32 0.73
0 -4 12 26.66 3.26
0 4 12 33.88 2.71
0 -4 12 24.55 2.08
0 4 -12 25.56 3.07
0 5 0 0.13 0.62
0 -5 0 0.46 0.34
0 5 1 40.05 1.22
0 -5 1 40.44 1.31
0 -5 -1 43.08 2.48
0 5 -1 40.52 1.38
0 -5 -1 37.41 0.87
0 -5 2 260.72 6.12
0 5 2 312.21 9.47
0 5 -2 278.07 7.99
0 -5 -2 299.31 7.05
0 5 3 20.97 2.05
0 -5 3 17.33 1.80
0 -5 -3 16.43 2.08
0 5 -3 15.82 1.10
0 -5 4 318.51 7.66
0 5 4 321.14 9.86
0 -5 -4 329.25 8.52
0 -5 -4 326.93 5.77
0 5 -4 315.78 8.98
0 -5 5 3.83 1.06
0 5 5 1.60 0.78
0 -5 5 1.28 0.50
0 5 5 1.87 0.29
0 -5 -5 2.33 0.30
0 5 -5 1.61 1.06
0 -5 -5 2.40 1.33
0 5 6 49.66 1.13
0 -5 6 52.45 2.29
0 -5 6 47.52 2.62
0 5 6 50.26 2.10
0 5 -6 50.21 2.66
0 -5 -6 47.70 1.15
0 -5 -6 43.78 3.26
0 5 7 329.30 9.25
0 -5 7 318.14 8.67
0 5 7 309.43 6.94
0 -5 7 324.05 9.34
0 -5 -7 306.51 11.23
0 -5 -7 330.60 7.25
0 5 -7 313.16 9.85
0 5 8 1.27 1.39
0 -5 8 1.03 0.99
0 -5 8 0.09 0.66
0 5 8 -0.19 0.60
0 -5 -8 0.05 0.46
0 5 -8 1.68 1.11
0 -5 -8 1.09 0.89
0 -5 9 -0.81 1.16
0 5 9 0.41 0.53
0 5 9 1.21 1.54
0 -5 9 0.72 1.10
0 -5 -9 -0.69 0.53
0 -5 -9 0.65 1.57
0 5 -9 -1.21 0.74
0 -5 10 10.87 2.01
0 5 10 8.44 2.70
0 -5 10 13.19 1.25
0 5 -10 9.61 1.31
0 -5 -10 8.73 2.70
0 -5 -10 8.96 1.03
0 5 11 1.07 1.27
0 -5 11 0.65 1.53
0 -5 11 2.42 1.48
0 5 -11 -0.72 1.48
0 -5 -11 1.80 0.75
0 -5 -11 -0.56 1.27
0 -5 12 3.16 1.78
0 -5 12 2.33 1.82
0 5 12 2.96 2.47
0 5 -12 1.53 1.80
0 6 0 272.47 6.26
0 -6 0 265.35 6.01
0 -6 1 144.28 4.08
0 6 1 117.13 2.34
0 -6 -1 116.24 2.26
0 -6 -1 123.39 4.44
0 6 -1 117.87 2.81
0 -6 2 211.14 6.00
0 6 2 203.63 3.01
0 -6 -2 210.19 5.12
0 6 -2 194.47 5.78
0 6 3 447.79 11.52
0 -6 3 441.53 12.54
0 -6 -3 435.76 11.37
0 6 -3 426.62 10.50
0 -6 4 35.41 1.49
0 6 4 34.14 1.69
0 -6 -4 36.15 1.77
0 6 -4 35.91 1.49
0 6 5 78.05 2.58
0 -6 5 74.66 3.23
0 -6 -5 78.31 2.72
0 -6 -5 74.92 1.26
0 6 -5 69.07 3.21
0 -6 6 258.16 8.22
0 6 6 267.78 7.27
0 6 6 237.87 4.46
0 -6 6 272.03 7.32
0 -6 -6 264.89 5.16
0 -6 -6 253.96 9.32
0 6 -6 263.86 8.18
0 -6 7 9.50 1.06
0 -6 7 9.56 1.36
0 6 7 8.88 0.35
0 6 7 9.88 1.27
0 -6 -7 7.51 1.31
0 6 -7 8.78 1.03
0 -6 -7 8.12 0.54
0 6 8 7.23 1.43
0 -6 8 10.33 1.14
0 -6 8 10.78 1.52
0 6 -8 7.69 1.13
0 -6 -8 8.47 2.34
0 -6 -8 9.13 0.65
0 -6 9 168.97 4.82
0 -6 9 156.70 6.89
0 6 9 162.22 8.15
0 6 -9 156.25 5.28
0 -6 -9 166.07 8.30
0 6 10 84.73 3.93
0 -6 10 74.48 4.56
0 -6 10 81.21 4.05
0 6 -10 64.36 3.08
0 -6 -10 69.76 3.81
0 -6 11 26.29 3.26
0 -6 11 27.33 1.89
0 6 11 33.43 4.17
0 6 -11 27.38 2.08
0 -6 -11 32.58 2.69
0 -6 12 0.70 1.80
0 6 12 1.93 1.58
0 -6 12 2.53 1.65
0 6 -12 1.84 1.12
0 -7 0 0.14 0.66
0 7 0 1.85 0.68
0 7 1 18.69 0.84
0 -7 1 20.17 0.95
0 -7 -1 25.17 1.25
0 7 -1 19.81 1.56
0 -7 -1 19.97 0.83
0 -7 2 304.51 8.38
0 7 2 309.84 5.39
0 7 -2 293.36 6.82
0 -7 -2 306.88 9.47
0 -7 3 110.44 3.09
0 7 3 113.00 3.40
0 -7 -3 116.05 3.39
0 7 -3 112.70 4.32
0 -7 4 377.67 11.14
0 7 4 397.06 10.41
0 7 -4 388.50 9.74
0 -7 -4 382.24 12.29
0 -7 5 727.95 21.13
0 7 5 760.15 22.17
0 -7 -5 743.47 22.38
0 7 -5 748.69 23.01
0 -7 6 9.56 0.77
0 -7 6 10.92 1.65
0 7 6 9.78 1.24
0 -7 -6 9.84 1.27
0 7 -6 9.96 1.67
0 -7 7 55.14 2.28
0 7 7 61.49 4.00
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8 9 -2 3.66 2.64
-8 -9 2 4.19 2.32
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-8 9 2 4.43 0.92
8 9 -1 21.18 2.35
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-8 9 -4 14.10 3.31
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8 10 -3 1.27 2.14
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8 10 -1 3.08 2.35
-8 -10 1 4.12 2.28
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8 11 -3 0.51 1.27
-8 -11 3 -1.59 1.98
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8 11 -2 2.34 1.50
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-8 -11 1 10.89 2.90
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8 13 -3 1.75 2.08
-8 -13 3 0.90 1.96
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8 13 -2 9.81 3.79
-8 -13 2 19.40 3.72
-8 13 2 21.27 2.07
-8 13 2 21.02 2.39
8 13 -1 94.32 6.67
-8 -13 1 93.91 4.52
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8 13 0 0.02 3.21
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-8 13 0 15.70 3.84
-8 -13 0 20.14 2.02
8 13 1 15.22 1.92
-8 -13 -1 16.66 2.91
-8 13 -1 14.62 3.40
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8 13 2 -0.01 1.87
-8 13 -2 2.32 2.31
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-8 -13 -2 1.70 1.81
8 13 3 13.98 2.93
-8 -13 -3 18.41 2.91
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8 14 -4 5.24 2.97
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-8 -14 3 56.39 5.90
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8 14 -2 146.90 8.75
-8 -14 2 156.46 8.85
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8 14 -1 82.40 6.06
-8 -14 1 82.98 5.98
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8 14 0 0.00 1.48
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8 16 -1 8.87 2.89
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9 1 -5 5.65 1.93
9 -1 -5 5.57 2.97
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9 1 -4 5.97 1.87
9 -1 -4 6.06 1.86
-9 -1 4 5.63 1.67
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9 1 -3 1.22 1.47
9 -1 -3 0.36 1.46
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9 1 -2 97.13 5.11
9 -1 -2 93.81 5.24
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9 1 -1 13.59 2.31
9 -1 -1 12.96 2.36
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9 1 0 35.36 5.10
9 -1 0 37.21 5.12
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9 1 1 42.69 5.10
-9 -1 -1 43.90 4.88
-9 1 -1 32.99 5.09
-9 -1 -2 60.48 5.77
-9 1 -2 55.56 6.08
-9 -1 -3 72.77 4.36
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9 -2 -6 2.32 2.91
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9 -2 -5 2.71 1.54
9 2 -5 -1.38 2.59
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9 2 -4 76.87 6.93
9 -2 -4 74.48 6.84
-9 -2 4 69.54 6.09
-9 2 4 70.83 5.36
-9 2 4 68.39 6.11
9 2 -3 57.47 5.89
9 -2 -3 54.05 6.03
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-9 -2 3 49.12 5.66
9 2 -2 1.92 2.06
9 -2 -2 -1.54 2.13
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-9 2 2 -0.34 1.21
9 2 -1 35.20 5.12
9 -2 -1 36.86 5.14
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9 2 0 4.38 1.89
9 -2 0 5.78 1.94
-9 -2 0 6.28 1.72
-9 2 0 4.51 1.87
9 2 1 55.42 3.76
-9 2 -1 52.89 3.87
-9 -2 -1 50.94 3.56
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-9 -2 -3 12.42 3.45
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9 -3 -6 7.40 2.14
9 3 -6 9.38 3.63
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9 3 -5 9.40 2.22
9 -3 -5 1.21 3.33
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9 -3 -4 0.29 2.15
9 3 -4 0.40 1.43
-9 -3 4 -0.89 2.02
-9 3 4 0.77 1.62
-9 3 4 -0.06 1.96
9 3 -3 3.37 1.79
9 -3 -3 3.53 1.81
-9 -3 3 4.40 1.66
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-9 3 3 3.20 1.62
9 3 -2 21.17 2.54
9 -3 -2 19.92 2.56
-9 -3 2 15.26 2.35
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9 3 -1 -0.42 1.32
9 -3 -1 1.31 2.18
-9 -3 1 -1.39 1.94
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9 3 0 158.62 9.69
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-9 3 0 148.74 9.74
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-9 -3 -1 -1.76 2.17
-9 3 -1 0.22 2.45
9 3 2 99.15 5.01
-9 -3 -2 88.66 4.63
-9 3 -2 98.11 7.53
-9 -3 -3 8.05 1.89
-9 3 -3 9.42 3.43
-9 -3 -4 55.57 5.27
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9 4 -6 57.50 4.19
9 -4 -6 56.51 5.92
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9 -4 -5 -0.11 1.44
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9 4 -4 47.47 5.87
9 -4 -4 47.13 3.65
-9 -4 4 49.49 3.46
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9 -4 -3 54.04 3.83
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9 -4 -2 8.94 2.09
9 4 -2 10.96 3.42
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9 4 -1 4.22 3.06
9 -4 -1 6.32 2.04
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9 4 0 26.68 2.85
-9 -4 0 30.29 4.15
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-9 4 0 30.09 2.90
9 4 1 37.50 4.69
-9 -4 -1 37.15 4.45
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9 4 2 10.76 2.09
-9 -4 -2 9.95 3.14
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-9 -4 -3 13.42 2.08
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-9 -4 -4 14.34 2.80
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9 5 -5 45.92 3.74
9 -5 -5 44.59 3.53
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9 5 -4 123.78 6.14
9 -5 -4 124.19 8.47
-9 5 4 117.85 6.61
-9 5 4 120.63 7.77
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9 5 -3 -0.35 1.43
9 -5 -3 1.76 2.24
-9 -5 3 2.06 2.06
-9 5 3 -0.29 1.47
-9 5 3 0.27 1.28
9 5 -2 30.97 3.10
9 -5 -2 35.43 4.87
-9 5 2 27.74 4.41
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-9 -5 2 29.59 2.81
9 5 -1 0.65 1.32
-9 -5 1 -1.85 1.21
-9 5 1 0.50 2.09
-9 5 1 0.48 1.14
9 5 0 1.02 2.20
-9 5 0 0.37 1.05
-9 5 0 -0.31 2.31
-9 -5 0 0.65 1.24
9 5 1 -0.18 1.27
-9 -5 -1 -0.67 1.22
-9 5 -1 0.56 0.84
-9 5 -1 3.33 2.30
9 5 2 95.24 6.81
-9 -5 -2 83.85 6.38
-9 5 -2 85.66 7.49
-9 -5 -3 19.37 3.32
-9 5 -3 10.61 4.13
9 6 -5 21.13 4.59
9 -6 -5 23.28 4.09
-9 -6 5 21.72 2.50
-9 6 5 12.02 3.35
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9 6 -4 1.39 2.51
9 -6 -4 -1.11 2.33
-9 -6 4 -0.04 1.34
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-9 6 4 0.73 1.66
9 6 -3 -2.78 3.72
9 -6 -3 12.62 2.22
-9 -6 3 12.11 2.04
-9 6 3 11.69 3.26
-9 6 3 11.04 2.31
9 -6 -2 16.08 2.38
9 6 -2 4.60 3.72
-9 -6 2 12.42 3.33
-9 6 2 13.62 2.14
-9 6 2 11.56 3.54
9 6 -1 7.88 3.64
-9 -6 1 9.53 3.24
-9 6 1 12.98 1.19
-9 6 1 10.86 2.20
9 6 0 6.59 1.82
-9 -6 0 4.35 2.70
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-9 6 0 6.24 1.93
9 6 1 6.82 3.19
-9 -6 -1 7.06 1.79
-9 6 -1 10.89 2.24
9 6 2 0.42 1.20
-9 -6 -2 -1.67 1.15
-9 6 -2 1.22 1.40
-9 -6 -3 39.20 4.53
-9 6 -3 46.83 5.93
9 7 -5 24.02 4.97
9 -7 -5 32.03 4.37
-9 -7 5 18.44 4.26
-9 7 5 25.34 3.58
-9 7 5 24.60 4.00
9 7 -4 5.76 1.93
9 -7 -4 5.71 1.81
-9 -7 4 0.45 2.74
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-9 7 4 5.03 2.63
9 7 -3 10.82 2.23
9 -7 -3 8.06 2.12
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9 7 -2 6.20 1.92
-9 -7 2 2.72 2.65
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-9 7 2 5.16 1.74
9 7 -1 17.34 4.06
-9 -7 1 20.49 3.70
-9 7 1 22.33 4.11
9 7 0 30.55 4.65
-9 -7 0 35.75 4.41
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-9 7 0 35.87 5.07
9 7 1 9.15 2.01
-9 -7 -1 8.92 2.93
9 7 2 46.76 4.78
-9 -7 -2 39.55 2.93
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-9 -7 -3 0.22 1.19
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9 8 -4 4.35 1.72
9 -8 -4 1.35 2.57
-9 -8 4 1.62 1.50
-9 8 4 0.75 1.83
-9 8 4 1.17 2.33
9 8 -3 5.47 3.13
-9 8 3 4.52 1.17
-9 8 3 4.65 1.69
-9 -8 3 4.92 1.64
9 8 -2 3.36 1.80
-9 -8 2 4.37 1.57
-9 8 2 2.59 0.96
-9 8 2 2.40 2.68
9 8 -1 44.85 3.36
-9 8 1 42.78 1.92
-9 8 1 41.01 5.29
-9 -8 1 35.91 3.02
9 8 0 16.52 3.81
-9 -8 0 18.52 2.24
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9 8 1 2.25 2.58
-9 -8 -1 3.43 2.38
-9 8 -1 3.06 1.82
9 8 2 -0.22 2.07
-9 -8 -2 1.46 1.97
-9 8 -2 0.03 2.64
9 9 -4 14.82 4.15
-9 -9 4 10.39 2.23
-9 9 4 17.15 2.15
-9 9 4 13.79 2.59
9 9 -3 0.52 2.45
-9 -9 3 2.45 2.21
-9 9 3 0.77 2.17
-9 9 3 0.51 1.43
9 9 -2 1.16 2.59
-9 -9 2 1.71 2.33
-9 9 2 1.74 1.52
-9 9 2 2.51 1.36
9 9 -1 3.29 2.64
-9 -9 1 1.47 1.49
-9 9 1 2.01 1.69
-9 9 1 3.29 1.21
9 9 0 37.26 3.01
-9 -9 0 28.91 2.69
-9 9 0 30.07 3.18
9 9 1 0.00 2.62
-9 -9 -1 5.75 1.56
-9 9 -1 3.24 1.94
9 9 2 5.74 1.57
-9 -9 -2 3.94 2.44
-9 9 -2 0.68 1.80
-9 9 -2 3.59 2.02
9 10 -3 2.63 1.75
-9 -10 3 3.91 2.51
-9 10 3 1.58 2.52
-9 10 3 2.79 1.60
9 10 -2 11.83 2.22
-9 -10 2 9.29 3.12
-9 10 2 10.88 2.16
-9 10 2 9.15 1.83
9 10 -1 3.94 2.71
-9 -10 1 3.03 2.44
-9 10 1 1.69 2.85
9 10 0 0.02 3.16
-9 -10 0 14.32 2.91
9 10 1 -0.03 1.51
-9 -10 -1 4.14 1.41
-9 10 -1 1.99 2.87
9 11 -2 2.13 1.72
-9 -11 2 3.17 1.56
-9 11 2 2.03 1.38
-9 11 2 3.15 2.60
9 11 -1 13.63 2.39
-9 -11 1 14.42 3.42
-9 11 1 15.77 3.93
9 11 0 0.01 2.79
-9 -11 0 4.80 2.54
-9 11 0 8.82 3.11
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 74825
_shelx_res_file
;
TITL ydkr_a.res in P2(1)/n
ydkr_a.res
created by SHELXL-2018/3 at 15:42:59 on 06-Sep-2023
REM Yadorkari-X generated
CELL 0.71075 7.6794 20.9875 10.0514 90.0000 95.1230 90.0000
ZERR 4.0 0.0016 0.0040 0.0019 0.0000 0.0030 0.0000
LATT 1
SYMM 1/2-X, 1/2+Y, 1/2-Z
REM SPGR P21/n monoclinic
SFAC C H O N B F
UNIT 56 56 18 8 4 16
SIZE 0.60 0.40 0.40
TEMP -173.0
L.S. 10
FMAP 2
PLAN -50
ACTA
CONF
HTAB
LIST 4
BOND $H
MERG 2
EQIV $1 3/2-X, -1/2+Y, 3/2-Z
EQIV $2 -X, 1-Y, 1-Z
EQIV $3 -1+X, +Y, +Z
EQIV $4 1/2-X, 1/2+Y, 3/2-Z
EQIV $5 -1/2+X, 3/2-Y, -1/2+Z
EQIV $6 -3/2+X, 3/2-Y, -1/2+Z
SUMP 0.5 0.0001 1.0 3 1.0 4
HTAB C13 O1_$1
HTAB C10 O3_$2
HTAB C10 O1_$1
HTAB C12 O2_$3
HTAB C7 O3_$4
HTAB C2 O3_$4
HTAB C4 O2_$5
HTAB O4 O1_$6
HTAB O4 O2_$6
WGHT 0.059400 1.201300
FVAR 0.59673 0.66190 0.14802 0.35198
O4 3 -0.124336 0.595080 0.515596 11.00000 0.01984 0.01946 =
0.03403 0.00356 -0.00052 -0.00156
O3 3 -0.183916 0.496061 0.584665 11.00000 0.02186 0.02184 =
0.03964 0.00373 0.00195 -0.00563
C14 1 -0.097670 0.545807 0.590829 11.00000 0.01581 0.01997 =
0.02852 -0.00006 0.00566 -0.00055
C13 1 0.054564 0.548665 0.699603 11.00000 0.02035 0.01922 =
0.03034 0.00367 0.00343 -0.00103
AFIX 23
H13 2 0.006964 0.550938 0.787824 11.00000 -1.20000
H13A 2 0.123093 0.508798 0.697034 11.00000 -1.20000
AFIX 0
N2 4 0.172931 0.603487 0.686278 11.00000 0.01721 0.01925 =
0.02509 -0.00018 0.00081 -0.00032
C10 1 0.333449 0.594355 0.644917 11.00000 0.01658 0.02064 =
0.02973 -0.00420 0.00047 0.00276
AFIX 43
H10 2 0.368960 0.552814 0.621280 11.00000 -1.20000
AFIX 0
C9 1 0.446592 0.645268 0.636787 11.00000 0.01679 0.02383 =
0.02940 -0.00566 0.00236 0.00011
AFIX 43
H9 2 0.559646 0.638678 0.607859 11.00000 -1.20000
AFIX 0
C8 1 0.394078 0.706394 0.671248 11.00000 0.01917 0.02038 =
0.02358 -0.00262 0.00019 -0.00140
C5 1 0.516673 0.761264 0.674275 11.00000 0.01831 0.02007 =
0.02734 -0.00163 -0.00163 -0.00015
N1 4 0.750085 0.861599 0.689173 11.00000 0.01999 0.01807 =
0.02938 -0.00044 -0.00192 -0.00148
C12 1 0.224549 0.714463 0.709214 11.00000 0.02132 0.01941 =
0.03389 -0.00468 0.00224 0.00181
AFIX 43
H12 2 0.183872 0.755753 0.729713 11.00000 -1.20000
AFIX 0
C7 1 0.620657 0.860540 0.771439 11.00000 0.02162 0.02045 =
0.03304 -0.00591 0.00053 0.00165
AFIX 43
H7 2 0.611023 0.894042 0.833916 11.00000 -1.20000
AFIX 0
C1 1 1.035539 0.889008 0.804142 11.00000 0.01847 0.01863 =
0.02596 -0.00159 0.00529 -0.00031
O1 3 1.142974 0.934508 0.841022 11.00000 0.02623 0.01950 =
0.04376 0.00157 -0.00869 -0.00497
O2 3 1.046981 0.833481 0.840640 11.00000 0.02315 0.01787 =
0.03106 0.00123 0.00209 -0.00083
C11 1 0.116942 0.662414 0.716769 11.00000 0.01902 0.02292 =
0.03216 -0.00446 0.00461 0.00255
AFIX 43
H11 2 0.002372 0.667885 0.743615 11.00000 -1.20000
AFIX 0
C6 1 0.502510 0.811104 0.765196 11.00000 0.01980 0.02294 =
0.03249 -0.00479 0.00408 0.00070
AFIX 43
H6 2 0.410968 0.810802 0.822826 11.00000 -1.20000
AFIX 0
C2 1 0.884426 0.912143 0.706925 11.00000 0.02164 0.01759 =
0.03381 0.00104 -0.00105 -0.00309
AFIX 23
H2 2 0.832748 0.951166 0.742328 11.00000 -1.20000
H2A 2 0.927993 0.922573 0.619744 11.00000 -1.20000
PART 1
AFIX 0
F1A 6 0.261227 0.836771 0.342150 21.00000 0.03035 0.09920 =
0.05888 -0.03962 0.01248 -0.00845
PART 0
C4 1 0.651211 0.764086 0.589746 11.00000 0.02674 0.02603 =
0.02912 -0.00810 0.00435 -0.00517
AFIX 43
H4 2 0.663465 0.731336 0.526009 11.00000 -1.20000
PART 1
AFIX 0
F2A 6 0.174451 0.843289 0.547617 21.00000 0.03532 0.08289 =
0.04053 0.00963 0.01267 -0.01039
PART 0
C3 1 0.766347 0.814756 0.599329 11.00000 0.02649 0.02943 =
0.02943 -0.00551 0.00541 -0.00506
AFIX 43
H3 2 0.858056 0.816631 0.541966 11.00000 -1.20000
PART 1
AFIX 0
B1A 5 0.244479 0.876875 0.448400 21.00000 0.03408 0.03518 =
0.03243 0.00402 0.00722 -0.00006
F3A 6 0.409606 0.899987 0.497011 21.00000 0.05315 0.06191 =
0.04493 0.01199 -0.00731 -0.02614
F4A 6 0.133298 0.926640 0.409326 21.00000 0.12174 0.04577 =
0.10252 0.00374 -0.05381 0.02580
PART 2
B1B 5 0.163287 0.877162 0.439925 -21.00000 0.02840 0.05823 =
0.02617 -0.00389 0.01093 -0.00945
PART 0
AFIX 1
H1B 2 -0.259900 0.581900 0.413100 11.00000 0.05000
PART 2
AFIX 0
F1B 6 0.252992 0.902436 0.552841 -21.00000 0.04874 0.10023 =
0.03437 -0.01962 -0.00335 -0.00024
F2B 6 0.259555 0.879408 0.332301 -21.00000 0.03282 0.10261 =
0.02689 -0.00630 0.00998 -0.02736
F3B 6 0.131959 0.812945 0.469650 -21.00000 0.07454 0.05919 =
0.08489 0.02083 0.02565 -0.00172
F4B 6 0.000678 0.903754 0.413681 -21.00000 0.03760 0.09078 =
0.02366 -0.01362 0.00023 0.00935
O5B 3 0.583772 0.958251 0.516101 41.00000 0.05038 0.04086 =
0.04104 0.00513 -0.00515 -0.00367
PART 1
O5A 3 -0.155095 0.960873 0.422338 31.00000 0.04021 0.03732 =
0.02981 0.00225 0.00036 -0.00150
PART 0
HKLF 4 1 1 0 0 0 1 0 0 0 1
REM ydkr_a.res in P2(1)/n
REM wR2 = 0.1315, GooF = S = 1.051, Restrained GooF = 1.051 for all data
REM R1 = 0.0510 for 3119 Fo > 4sig(Fo) and 0.0589 for all 3652 data
REM 292 parameters refined using 1 restraints
END
WGHT 0.0594 1.2013
REM Instructions for potential hydrogen bonds
EQIV $7 x-1/2, -y+3/2, z+1/2
HTAB C13 F3A_$7
HTAB C13 F2B_$7
HTAB C13 O5B_$7
HTAB C13 O1_$1
HTAB C10 O3_$2
HTAB C10 O1_$1
HTAB C12 O2_$3
HTAB C12 F2A
HTAB C7 O3_$4
HTAB C11 F1A_$7
HTAB C11 F2B_$7
HTAB C2 O3_$4
EQIV $8 x+1, y, z
HTAB C2 F4B_$8
HTAB C2 O5A_$8
HTAB C4 O2_$5
HTAB C3 F2A_$8
HTAB C3 F3B_$8
HTAB C3 F4B_$8
HTAB O4 O1_$6
HTAB O4 O2_$6
REM Highest difference peak 0.721, deepest hole -0.560, 1-sigma level 0.064
Q1 1 -0.3076 0.5752 0.8448 11.00000 0.05 0.72
Q2 1 -0.2669 0.5498 0.9643 11.00000 0.05 0.44
Q3 1 0.9551 0.8998 0.7607 11.00000 0.05 0.34
Q4 1 0.2612 0.6004 0.6993 11.00000 0.05 0.31
Q5 1 0.8152 0.8864 0.6980 11.00000 0.05 0.30
Q6 1 0.7597 0.8386 0.6503 11.00000 0.05 0.30
Q7 1 -0.0485 0.5473 1.0141 11.00000 0.05 0.30
Q8 1 0.4013 0.6207 0.6752 11.00000 0.05 0.30
Q9 1 0.1584 0.6908 0.6816 11.00000 0.05 0.29
Q10 1 -0.4647 0.6448 0.9370 11.00000 0.05 0.28
Q11 1 0.4013 0.6768 0.6231 11.00000 0.05 0.27
Q12 1 0.1222 0.5781 0.6960 11.00000 0.05 0.27
Q13 1 -0.0178 0.5505 0.6416 11.00000 0.05 0.27
Q14 1 0.0000 0.5000 1.0000 10.50000 0.05 0.26
Q15 1 0.4281 0.6720 0.6736 11.00000 0.05 0.26
Q16 1 0.3802 0.6261 0.6187 11.00000 0.05 0.26
Q17 1 0.5118 0.7854 0.7200 11.00000 0.05 0.25
Q18 1 1.1421 0.8606 0.8440 11.00000 0.05 0.25
Q19 1 0.3219 0.7019 0.7245 11.00000 0.05 0.25
Q20 1 0.4489 0.7345 0.6530 11.00000 0.05 0.25
Q21 1 1.0784 0.9126 0.8243 11.00000 0.05 0.24
Q22 1 0.1615 0.6293 0.7271 11.00000 0.05 0.24
Q23 1 0.1263 0.6335 0.6625 11.00000 0.05 0.23
Q24 1 0.5804 0.7625 0.6383 11.00000 0.05 0.23
Q25 1 1.0515 0.9638 0.8251 11.00000 0.05 0.23
Q26 1 0.7094 0.7931 0.5999 11.00000 0.05 0.22
Q27 1 -0.2260 0.6058 0.4945 11.00000 0.05 0.22
Q28 1 0.5407 0.8374 0.7321 11.00000 0.05 0.22
Q29 1 -0.3609 0.6223 1.0209 11.00000 0.05 0.22
Q30 1 0.6083 0.7537 0.6582 11.00000 0.05 0.21
Q31 1 0.6851 0.8602 0.7107 11.00000 0.05 0.21
Q32 1 1.1334 0.8166 0.8689 11.00000 0.05 0.21
Q33 1 0.1892 0.6860 0.7501 11.00000 0.05 0.19
Q34 1 1.0047 0.8647 0.8617 11.00000 0.05 0.19
Q35 1 0.3047 0.7105 0.6684 11.00000 0.05 0.18
Q36 1 -0.2641 0.6889 0.9190 11.00000 0.05 0.18
Q37 1 -0.1469 0.5744 0.5522 11.00000 0.05 0.17
Q38 1 -0.1797 0.6010 0.8639 11.00000 0.05 0.17
Q39 1 -0.2627 0.5130 0.5433 11.00000 0.05 0.17
Q40 1 -0.2590 0.4904 0.5488 11.00000 0.05 0.17
Q41 1 0.4178 0.8204 0.7595 11.00000 0.05 0.17
Q42 1 -0.2317 0.4799 0.6425 11.00000 0.05 0.16
Q43 1 0.1243 0.5267 0.6832 11.00000 0.05 0.16
Q44 1 0.8005 0.8146 0.5770 11.00000 0.05 0.16
Q45 1 1.0759 0.8613 0.7880 11.00000 0.05 0.16
Q46 1 -0.0117 0.6468 0.7616 11.00000 0.05 0.16
Q47 1 -0.0593 0.6252 0.5402 11.00000 0.05 0.15
Q48 1 -0.1192 0.4774 0.5517 11.00000 0.05 0.15
Q49 1 -0.3206 0.6706 1.0256 11.00000 0.05 0.15
Q50 1 -0.1738 0.6558 0.4970 11.00000 0.05 0.15
;
_shelx_res_checksum 19083
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 -1/2+X,-1/2-Y,-1/2+Z
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O O4 -0.12434(15) 0.59508(5) 0.51560(12) 0.0246(3) Uani d 1 . .
O O3 -0.18392(15) 0.49606(6) 0.58466(13) 0.0278(3) Uani d 1 . .
C C14 -0.0977(2) 0.54581(7) 0.59083(16) 0.0212(3) Uani d 1 . .
C C13 0.0546(2) 0.54866(8) 0.69960(17) 0.0232(3) Uani d 1 . .
H H13 0.006964 0.550938 0.787824 0.028 Uiso calc 1 . .
H H13A 0.123093 0.508798 0.697034 0.028 Uiso calc 1 . .
N N2 0.17293(17) 0.60349(6) 0.68628(13) 0.0206(3) Uani d 1 . .
C C10 0.3334(2) 0.59435(8) 0.64492(17) 0.0224(3) Uani d 1 . .
H H10 0.368960 0.552814 0.621280 0.027 Uiso calc 1 . .
C C9 0.4466(2) 0.64527(8) 0.63679(17) 0.0233(3) Uani d 1 . .
H H9 0.559646 0.638678 0.607859 0.028 Uiso calc 1 . .
C C8 0.3941(2) 0.70639(8) 0.67125(16) 0.0211(3) Uani d 1 . .
C C5 0.5167(2) 0.76126(8) 0.67427(16) 0.0221(3) Uani d 1 . .
N N1 0.75008(18) 0.86160(6) 0.68917(14) 0.0227(3) Uani d 1 . .
C C12 0.2245(2) 0.71446(8) 0.70921(17) 0.0249(4) Uani d 1 . .
H H12 0.183872 0.755753 0.729713 0.030 Uiso calc 1 . .
C C7 0.6207(2) 0.86054(8) 0.77144(18) 0.0252(3) Uani d 1 . .
H H7 0.611023 0.894042 0.833916 0.030 Uiso calc 1 . .
C C1 1.0355(2) 0.88901(7) 0.80414(16) 0.0208(3) Uani d 1 . .
O O1 1.14297(16) 0.93451(6) 0.84102(13) 0.0305(3) Uani d 1 . .
O O2 1.04698(15) 0.83348(5) 0.84064(12) 0.0240(3) Uani d 1 . .
C C11 0.1169(2) 0.66241(8) 0.71677(17) 0.0246(3) Uani d 1 . .
H H11 0.002372 0.667885 0.743615 0.029 Uiso calc 1 . .
C C6 0.5025(2) 0.81110(8) 0.76520(17) 0.0250(3) Uani d 1 . .
H H6 0.410968 0.810802 0.822826 0.030 Uiso calc 1 . .
C C2 0.8844(2) 0.91214(8) 0.70692(18) 0.0246(3) Uani d 1 . .
H H2 0.832748 0.951166 0.742328 0.029 Uiso calc 1 . .
H H2A 0.927993 0.922573 0.619744 0.029 Uiso calc 1 . .
F F1A 0.2612(3) 0.83677(18) 0.3422(3) 0.0623(9) Uani d 0.662(3) A 1
C C4 0.6512(2) 0.76409(8) 0.58975(17) 0.0272(4) Uani d 1 . .
H H4 0.663465 0.731336 0.526009 0.033 Uiso calc 1 . .
F F2A 0.1745(3) 0.84329(14) 0.5476(2) 0.0524(7) Uani d 0.662(3) A 1
C C3 0.7663(2) 0.81476(9) 0.59933(18) 0.0283(4) Uani d 1 . .
H H3 0.858056 0.816631 0.541966 0.034 Uiso calc 1 . .
B B1A 0.2445(7) 0.8769(2) 0.4484(4) 0.0336(9) Uani d 0.662(3) A 1
F F3A 0.4096(3) 0.89999(11) 0.4970(2) 0.0540(7) Uani d 0.662(3) A 1
F F4A 0.1333(5) 0.92664(13) 0.4093(3) 0.0938(13) Uani d 0.662(3) A 1
B B1B 0.1633(13) 0.8772(5) 0.4399(9) 0.037(2) Uani d 0.338(3) A 2
H H1B -0.259900 0.581900 0.413100 0.050 Uiso d 1 . .
F F1B 0.2530(6) 0.9024(3) 0.5528(4) 0.0615(15) Uani d 0.338(3) A 2
F F2B 0.2596(6) 0.8794(4) 0.3323(4) 0.0537(15) Uani d 0.338(3) A 2
F F3B 0.1320(8) 0.8129(3) 0.4697(7) 0.0718(17) Uani d 0.338(3) A 2
F F4B 0.0007(6) 0.9038(2) 0.4137(3) 0.0508(13) Uani d 0.338(3) A 2
O O5B 0.5838(6) 0.9583(2) 0.5161(4) 0.0446(11) Uani d 0.352(2) B 2
O O5A -0.1551(12) 0.9609(5) 0.4223(9) 0.036(2) Uani d 0.148(2) C 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
O4 0.0198(6) 0.0195(6) 0.0340(6) -0.0016(4) -0.0005(5) 0.0036(5)
O3 0.0219(6) 0.0218(6) 0.0396(7) -0.0056(5) 0.0020(5) 0.0037(5)
C14 0.0158(7) 0.0200(7) 0.0285(8) -0.0005(6) 0.0057(6) -0.0001(6)
C13 0.0203(8) 0.0192(7) 0.0303(8) -0.0010(6) 0.0034(6) 0.0037(6)
N2 0.0172(6) 0.0193(6) 0.0251(7) -0.0003(5) 0.0008(5) -0.0002(5)
C10 0.0166(7) 0.0206(7) 0.0297(8) 0.0028(6) 0.0005(6) -0.0042(6)
C9 0.0168(7) 0.0238(8) 0.0294(8) 0.0001(6) 0.0024(6) -0.0057(6)
C8 0.0192(7) 0.0204(8) 0.0236(7) -0.0014(6) 0.0002(6) -0.0026(6)
C5 0.0183(7) 0.0201(7) 0.0273(8) -0.0001(6) -0.0016(6) -0.0016(6)
N1 0.0200(7) 0.0181(6) 0.0294(7) -0.0015(5) -0.0019(5) -0.0004(5)
C12 0.0213(8) 0.0194(8) 0.0339(9) 0.0018(6) 0.0022(6) -0.0047(7)
C7 0.0216(8) 0.0204(8) 0.0330(9) 0.0016(6) 0.0005(6) -0.0059(7)
C1 0.0185(7) 0.0186(7) 0.0260(8) -0.0003(6) 0.0053(6) -0.0016(6)
O1 0.0262(6) 0.0195(6) 0.0438(7) -0.0050(5) -0.0087(5) 0.0016(5)
O2 0.0231(6) 0.0179(6) 0.0311(6) -0.0008(4) 0.0021(5) 0.0012(5)
C11 0.0190(8) 0.0229(8) 0.0322(8) 0.0025(6) 0.0046(6) -0.0045(7)
C6 0.0198(8) 0.0229(8) 0.0325(9) 0.0007(6) 0.0041(6) -0.0048(7)
C2 0.0216(8) 0.0176(7) 0.0338(9) -0.0031(6) -0.0011(6) 0.0010(6)
F1A 0.0304(11) 0.099(2) 0.0589(15) -0.0085(14) 0.0125(10) -0.0396(17)
C4 0.0267(9) 0.0260(8) 0.0291(8) -0.0052(7) 0.0044(7) -0.0081(7)
F2A 0.0353(11) 0.0829(18) 0.0405(11) -0.0104(11) 0.0127(9) 0.0096(12)
C3 0.0265(9) 0.0294(9) 0.0294(9) -0.0051(7) 0.0054(7) -0.0055(7)
B1A 0.034(2) 0.0352(19) 0.032(2) 0.000(2) 0.007(2) 0.0040(14)
F3A 0.0532(13) 0.0619(14) 0.0449(11) -0.0261(10) -0.0073(9) 0.0120(10)
F4A 0.122(3) 0.0458(15) 0.103(2) 0.0258(17) -0.054(2) 0.0037(14)
B1B 0.028(4) 0.058(5) 0.026(4) -0.009(5) 0.011(4) -0.004(3)
F1B 0.049(3) 0.100(4) 0.034(2) 0.000(2) -0.0034(17) -0.020(2)
F2B 0.033(2) 0.103(4) 0.0269(19) -0.027(3) 0.0100(15) -0.006(3)
F3B 0.075(4) 0.059(3) 0.085(4) -0.002(3) 0.026(3) 0.021(3)
F4B 0.038(2) 0.091(3) 0.0237(17) 0.009(2) 0.0002(14) -0.0136(18)
O5B 0.050(3) 0.041(2) 0.041(2) -0.004(2) -0.0052(19) 0.0051(19)
O5A 0.040(5) 0.037(5) 0.030(4) -0.001(4) 0.000(4) 0.002(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
C14 O4 H1B . . 109.7 ?
O3 C14 O4 . . 126.40(15) ?
O3 C14 C13 . . 116.20(14) ?
O4 C14 C13 . . 117.40(14) ?
N2 C13 C14 . . 113.73(13) ?
N2 C13 H13 . . 108.8 ?
C14 C13 H13 . . 108.8 ?
N2 C13 H13A . . 108.8 ?
C14 C13 H13A . . 108.8 ?
H13 C13 H13A . . 107.7 ?
C10 N2 C11 . . 121.13(14) ?
C10 N2 C13 . . 120.19(13) ?
C11 N2 C13 . . 118.68(13) ?
N2 C10 C9 . . 120.27(15) ?
N2 C10 H10 . . 119.9 ?
C9 C10 H10 . . 119.9 ?
C10 C9 C8 . . 119.83(14) ?
C10 C9 H9 . . 120.1 ?
C8 C9 H9 . . 120.1 ?
C9 C8 C12 . . 118.34(15) ?
C9 C8 C5 . . 121.34(14) ?
C12 C8 C5 . . 120.25(14) ?
C4 C5 C6 . . 118.07(15) ?
C4 C5 C8 . . 121.48(15) ?
C6 C5 C8 . . 120.43(15) ?
C3 N1 C7 . . 121.07(14) ?
C3 N1 C2 . . 119.89(14) ?
C7 N1 C2 . . 118.82(14) ?
C11 C12 C8 . . 119.80(15) ?
C11 C12 H12 . . 120.1 ?
C8 C12 H12 . . 120.1 ?
N1 C7 C6 . . 120.23(15) ?
N1 C7 H7 . . 119.9 ?
C6 C7 H7 . . 119.9 ?
O2 C1 O1 . . 126.19(15) ?
O2 C1 C2 . . 121.66(14) ?
O1 C1 C2 . . 112.15(13) ?
N2 C11 C12 . . 120.56(15) ?
N2 C11 H11 . . 119.7 ?
C12 C11 H11 . . 119.7 ?
C7 C6 C5 . . 120.26(15) ?
C7 C6 H6 . . 119.9 ?
C5 C6 H6 . . 119.9 ?
N1 C2 C1 . . 109.32(13) ?
N1 C2 H2 . . 109.8 ?
C1 C2 H2 . . 109.8 ?
N1 C2 H2A . . 109.8 ?
C1 C2 H2A . . 109.8 ?
H2 C2 H2A . . 108.3 ?
C3 C4 C5 . . 119.62(16) ?
C3 C4 H4 . . 120.2 ?
C5 C4 H4 . . 120.2 ?
N1 C3 C4 . . 120.75(16) ?
N1 C3 H3 . . 119.6 ?
C4 C3 H3 . . 119.6 ?
F2A B1A F1A . . 108.7(4) ?
F2A B1A F4A . . 108.8(4) ?
F1A B1A F4A . . 109.9(4) ?
F2A B1A F3A . . 109.0(3) ?
F1A B1A F3A . . 109.7(4) ?
F4A B1A F3A . . 110.7(4) ?
F2B B1B F4B . . 112.4(7) ?
F2B B1B F1B . . 111.9(7) ?
F4B B1B F1B . . 112.4(7) ?
F2B B1B F3B . . 108.5(8) ?
F4B B1B F3B . . 105.1(7) ?
F1B B1B F3B . . 106.0(8) ?
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
O4 C14 . 1.287(2) ?
O4 H1B . 1.4248 ?
O3 C14 . 1.2350(19) ?
C14 C13 . 1.529(2) ?
C13 N2 . 1.480(2) ?
C13 H13 . 0.9900 ?
C13 H13A . 0.9900 ?
N2 C10 . 1.349(2) ?
N2 C11 . 1.353(2) ?
C10 C9 . 1.384(2) ?
C10 H10 . 0.9500 ?
C9 C8 . 1.398(2) ?
C9 H9 . 0.9500 ?
C8 C12 . 1.399(2) ?
C8 C5 . 1.486(2) ?
C5 C4 . 1.396(2) ?
C5 C6 . 1.400(2) ?
N1 C3 . 1.348(2) ?
N1 C7 . 1.349(2) ?
N1 C2 . 1.479(2) ?
C12 C11 . 1.376(2) ?
C12 H12 . 0.9500 ?
C7 C6 . 1.376(2) ?
C7 H7 . 0.9500 ?
C1 O2 . 1.2226(19) ?
C1 O1 . 1.2944(19) ?
C1 C2 . 1.528(2) ?
C11 H11 . 0.9500 ?
C6 H6 . 0.9500 ?
C2 H2 . 0.9900 ?
C2 H2A . 0.9900 ?
F1A B1A . 1.375(5) ?
C4 C3 . 1.381(2) ?
C4 H4 . 0.9500 ?
F2A B1A . 1.370(5) ?
C3 H3 . 0.9500 ?
B1A F4A . 1.384(5) ?
B1A F3A . 1.404(6) ?
B1B F2B . 1.364(9) ?
B1B F4B . 1.372(12) ?
B1B F1B . 1.380(10) ?
B1B F3B . 1.406(11) ?
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
C13 H13A O1 2_646 0.99 2.43 3.387(2) 161.2 no
C10 H10 O3 3_566 0.95 2.61 3.126(2) 114.2 no
C10 H10 O1 2_646 0.95 2.51 3.362(2) 148.6 no
C12 H12 O2 1_455 0.95 2.28 3.188(2) 158.7 no
C7 H7 O3 2_556 0.95 2.34 3.208(2) 151.3 no
C2 H2 O3 2_556 0.99 2.36 3.231(2) 146.2 no
C4 H4 O2 4_575 0.95 2.41 3.278(2) 151.2 no
O4 H1B O2 4_475 1.42 2.39 3.3044(17) 118.1 no
O1 H1B O4 4_120 1.05 1.42 2.4694(18) 172.0 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
O3 C14 C13 N2 . . . . 168.93(14) ?
O4 C14 C13 N2 . . . . -11.5(2) ?
C14 C13 N2 C10 . . . . -107.12(17) ?
C14 C13 N2 C11 . . . . 73.10(19) ?
C11 N2 C10 C9 . . . . 2.0(2) ?
C13 N2 C10 C9 . . . . -177.78(15) ?
N2 C10 C9 C8 . . . . -0.2(2) ?
C10 C9 C8 C12 . . . . -2.0(2) ?
C10 C9 C8 C5 . . . . 175.02(15) ?
C9 C8 C5 C4 . . . . 30.3(2) ?
C12 C8 C5 C4 . . . . -152.72(17) ?
C9 C8 C5 C6 . . . . -148.12(17) ?
C12 C8 C5 C6 . . . . 28.9(2) ?
C9 C8 C12 C11 . . . . 2.5(2) ?
C5 C8 C12 C11 . . . . -174.60(15) ?
C3 N1 C7 C6 . . . . 0.2(3) ?
C2 N1 C7 C6 . . . . -174.36(15) ?
C10 N2 C11 C12 . . . . -1.5(2) ?
C13 N2 C11 C12 . . . . 178.25(15) ?
C8 C12 C11 N2 . . . . -0.8(3) ?
N1 C7 C6 C5 . . . . 0.6(3) ?
C4 C5 C6 C7 . . . . -1.1(2) ?
C8 C5 C6 C7 . . . . 177.33(15) ?
C3 N1 C2 C1 . . . . -84.48(19) ?
C7 N1 C2 C1 . . . . 90.16(17) ?
O2 C1 C2 N1 . . . . 10.3(2) ?
O1 C1 C2 N1 . . . . -169.22(14) ?
C6 C5 C4 C3 . . . . 0.9(3) ?
C8 C5 C4 C3 . . . . -177.53(16) ?
C7 N1 C3 C4 . . . . -0.4(3) ?
C2 N1 C3 C4 . . . . 174.09(16) ?
C5 C4 C3 N1 . . . . -0.1(3) ?