#------------------------------------------------------------------------------
#$Date: 2022-08-24 04:31:05 +0300 (Wed, 24 Aug 2022) $
#$Revision: 277367 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/41/2244150.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_2244150
loop_
_publ_author_name
'Mu\~noz S\'anchez, Gaby M.'
'Zdilla, Michael J.'
_publ_section_title
;
Crystal structure of
N-butyl-2,3-bis(dicyclohexylamino)cyclopropeniminium chloride
benzene monosolvate
;
_journal_coeditor_code JQ2013
_journal_issue 9
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi 10.1107/S2056989022008076
_journal_volume 78
_journal_year 2022
_chemical_formula_iupac 'C31 H54 N3 +, Cl -, C6 H6'
_chemical_formula_moiety 'C31 H54 N3 +, Cl -, C6 H6'
_chemical_formula_sum 'C37 H60 Cl N3'
_chemical_formula_weight 582.33
_chemical_melting_point 356
_chemical_name_systematic
;
N-Butyl-2,3-bis(dicyclohexylamino)cyclopropeniminium
chloride benzene monosolvate
;
_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 dual
_atom_sites_solution_secondary difmap
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha 90
_cell_angle_beta 104.164(7)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.253(3)
_cell_length_b 22.699(7)
_cell_length_c 12.884(3)
_cell_measurement_reflns_used 9959
_cell_measurement_temperature 100.0
_cell_measurement_theta_max 29.60
_cell_measurement_theta_min 2.64
_cell_volume 3474.5(16)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
COSMO and XPREP (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100.15
_diffrn_detector_area_resol_mean 10.417
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type 'Bruker D8 Quest Photon 100'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71076
_diffrn_reflns_av_R_equivalents 0.0440
_diffrn_reflns_av_unetI/netI 0.0322
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 48756
_diffrn_reflns_theta_full 25.243
_diffrn_reflns_theta_max 27.878
_diffrn_reflns_theta_min 2.639
_diffrn_source 'sealed tube'
_exptl_absorpt_coefficient_mu 0.138
_exptl_absorpt_correction_T_max 0.7459
_exptl_absorpt_correction_T_min 0.6619
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.113
_exptl_crystal_description chunk
_exptl_crystal_F_000 1280
_exptl_crystal_size_max 0.547
_exptl_crystal_size_mid 0.529
_exptl_crystal_size_min 0.164
_refine_diff_density_max 0.546
_refine_diff_density_min -0.403
_refine_ls_extinction_coef 0.0081(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018/3 (Sheldrick 2015b)
;
_refine_ls_goodness_of_fit_ref 1.019
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 385
_refine_ls_number_reflns 8072
_refine_ls_number_restraints 6
_refine_ls_restrained_S_all 1.019
_refine_ls_R_factor_all 0.0708
_refine_ls_R_factor_gt 0.0548
_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^)+(0.0605P)^2^+2.3777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1260
_refine_ls_wR_factor_ref 0.1362
_reflns_number_gt 6516
_reflns_number_total 8072
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jq2013sup1.cif
_cod_data_source_block I
_cod_original_cell_volume 3474.6(16)
_cod_database_code 2244150
_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 0.928
_shelx_estimated_absorpt_t_max 0.978
_shelx_hkl_file
;
-4 0 0 5.75 0.92
-5 0 0 0.03 0.54
-5 0 0 0.87 0.26
-5 0 0 0.87 0.58
-6 0 0 1293.87 36.27
-6 0 0 1194.00 36.23
-6 0 0 1179.28 35.52
-6 0 0 1222.33 35.54
-7 0 0 0.99 0.80
-7 0 0 0.85 0.36
-7 0 0 1.74 0.78
-7 0 0 -0.09 0.35
-8 0 0 113.12 4.61
-8 0 0 105.85 6.07
-8 0 0 114.06 3.70
-8 0 0 120.10 3.77
-9 0 0 0.12 0.96
-9 0 0 3.04 1.24
-9 0 0 -0.28 0.62
-9 0 0 -0.65 0.51
-10 0 0 4.00 0.84
-10 0 0 5.32 0.78
-10 0 0 5.03 1.40
-11 0 0 -0.53 0.79
-11 0 0 -0.75 0.78
-11 0 0 -0.23 1.29
-12 0 0 5.99 1.83
-12 0 0 4.34 1.05
-12 0 0 4.71 1.08
-13 0 0 -0.55 1.01
-13 0 0 -0.80 0.97
-13 0 0 0.57 1.78
-14 0 0 1.40 1.25
-14 0 0 0.75 1.23
-14 0 0 3.13 2.22
-15 0 0 0.70 1.44
-15 0 0 3.82 2.42
-15 0 0 0.31 1.24
-16 0 0 8.50 1.86
-16 0 0 8.96 1.72
-16 0 0 8.51 3.14
-2 -1 0 185.22 6.07
2 -1 0 210.49 6.33
-2 -1 0 211.51 6.25
-2 -1 0 212.18 6.10
-2 1 0 200.14 6.30
2 1 0 201.32 6.04
2 1 0 223.17 6.03
-3 -1 0 333.55 9.94
-3 -1 0 344.91 9.96
-3 -1 0 342.83 10.23
-3 1 0 334.00 10.49
-4 -1 0 505.47 14.66
-4 -1 0 491.36 15.03
-4 -1 0 482.58 14.64
-4 1 0 522.42 15.12
-5 -1 0 778.21 23.63
-5 -1 0 804.07 23.66
-5 -1 0 788.55 24.13
-5 1 0 870.62 24.66
-6 -1 0 467.00 14.23
-6 -1 0 455.28 13.65
-6 -1 0 467.73 13.69
-6 -1 0 451.42 14.23
-6 1 0 468.75 14.31
-7 -1 0 16.46 1.70
-7 -1 0 19.11 1.06
-7 -1 0 16.85 1.63
-7 -1 0 17.78 1.60
-7 1 0 19.91 1.85
-7 1 0 16.82 1.63
-7 1 0 18.58 0.86
-8 -1 0 0.71 0.56
-8 -1 0 1.88 1.03
-8 -1 0 1.51 0.96
-8 -1 0 0.88 0.50
-8 1 0 1.66 1.12
-8 1 0 1.10 0.48
-8 1 0 0.45 0.93
-8 1 0 0.88 0.45
-9 -1 0 3.09 0.77
-9 -1 0 3.47 1.13
-9 -1 0 1.59 1.28
-9 -1 0 3.29 0.68
-9 1 0 2.75 0.56
-9 1 0 3.76 1.29
-9 1 0 3.17 0.63
-9 1 0 3.34 1.27
-10 -1 0 27.56 1.65
-10 -1 0 25.82 1.82
-10 -1 0 27.60 2.60
-10 1 0 27.00 2.66
-10 1 0 28.26 1.51
-10 1 0 26.91 1.56
-11 -1 0 10.81 1.98
-11 -1 0 8.28 1.64
-11 -1 0 6.95 1.16
-11 1 0 8.06 1.02
-11 1 0 7.85 1.01
-11 1 0 7.28 1.78
-12 -1 0 100.70 3.87
-12 -1 0 96.66 3.94
-12 -1 0 98.71 5.03
-12 1 0 96.75 3.78
-12 1 0 100.92 3.72
-12 1 0 91.44 4.99
-13 -1 0 1.93 1.74
-13 -1 0 -0.43 1.13
-13 -1 0 1.21 1.13
-13 1 0 2.02 1.00
-13 1 0 3.19 1.02
-13 1 0 1.27 1.77
-14 -1 0 12.72 2.52
-14 -1 0 16.79 2.26
-14 -1 0 9.68 1.60
-14 1 0 9.94 2.49
-14 1 0 9.39 1.48
-14 1 0 10.50 1.45
-15 -1 0 26.19 2.82
-15 -1 0 30.29 4.66
-15 -1 0 22.25 2.69
-15 1 0 18.84 2.57
-15 1 0 21.72 3.39
-15 1 0 16.76 2.46
-16 -1 0 3.67 2.83
-16 -1 0 0.63 1.80
-16 -1 0 3.40 1.60
-16 1 0 1.72 1.61
-16 1 0 5.05 2.89
-16 1 0 1.72 1.76
-2 -2 0 1.75 0.36
-2 -2 0 1.73 0.34
-2 -2 0 1.85 0.38
2 -2 0 1.87 0.57
2 2 0 1.93 0.32
-2 2 0 1.84 0.51
2 2 0 1.87 0.31
-2 2 0 1.78 0.19
-3 -2 0 178.61 5.51
-3 -2 0 180.43 5.63
3 -2 0 174.95 5.79
-3 -2 0 175.78 5.47
3 2 0 186.62 5.65
3 2 0 176.11 5.37
3 2 0 187.34 5.39
-3 2 0 185.34 5.80
-4 -2 0 3.23 0.47
-4 -2 0 2.88 0.41
-4 -2 0 3.46 0.62
-4 2 0 3.47 0.69
-5 -2 0 484.18 14.71
-5 -2 0 497.25 15.06
-5 -2 0 485.77 14.67
-5 2 0 520.65 15.60
-6 -2 0 0.61 0.45
-6 -2 0 0.32 0.67
-6 -2 0 0.60 0.50
-6 2 0 0.40 0.68
-7 -2 0 6.40 1.08
-7 -2 0 6.70 1.09
-7 -2 0 6.46 1.02
-7 -2 0 7.19 0.87
-7 2 0 6.87 1.28
-7 2 0 6.74 0.55
-8 -2 0 90.30 3.20
-8 -2 0 89.50 3.31
-8 -2 0 92.19 3.85
-8 -2 0 89.69 3.83
-8 2 0 87.78 2.96
-8 2 0 95.37 4.18
-8 2 0 90.29 2.95
-8 2 0 95.88 4.08
-9 -2 0 8.92 1.48
-9 -2 0 8.90 1.13
-9 -2 0 9.85 1.35
-9 -2 0 9.37 1.48
-9 2 0 8.18 1.54
-9 2 0 10.26 0.95
-9 2 0 9.03 0.84
-10 -2 0 20.70 1.58
-10 -2 0 18.70 1.76
-10 -2 0 20.99 2.50
-10 2 0 19.10 2.58
-10 2 0 23.08 1.38
-11 -2 0 36.52 3.12
-11 -2 0 39.17 2.09
-11 -2 0 34.36 2.27
-11 2 0 30.35 3.08
-11 2 0 36.52 1.90
-11 2 0 36.48 1.89
-12 -2 0 11.42 2.08
-12 -2 0 5.85 1.29
-12 -2 0 7.56 1.30
-12 2 0 7.80 2.00
-12 2 0 6.75 1.07
-12 2 0 11.60 1.60
-13 -2 0 8.28 1.44
-13 -2 0 11.84 2.26
-13 -2 0 8.61 1.44
-13 2 0 7.69 1.26
-13 2 0 8.03 1.18
-13 2 0 5.96 1.97
-14 -2 0 5.20 2.16
-14 -2 0 -0.15 1.35
-14 -2 0 0.07 1.28
-14 2 0 1.99 1.14
-14 2 0 0.85 2.09
-14 2 0 0.24 1.03
-15 -2 0 -1.00 1.32
-15 -2 0 3.12 2.53
-15 -2 0 1.70 1.53
-15 2 0 -1.73 1.20
-15 2 0 -0.62 1.33
-15 2 0 -1.37 2.43
-16 -2 0 17.84 3.77
-16 -2 0 22.13 3.34
-16 -2 0 22.12 3.14
-16 2 0 16.00 2.36
-16 2 0 19.15 2.74
-16 2 0 15.99 3.38
0 -3 0 12.45 0.76
0 3 0 13.62 0.74
0 3 0 15.04 0.79
1 -3 0 165.50 5.18
1 -3 0 160.53 5.14
1 -3 0 168.48 5.04
-1 -3 0 177.43 5.18
-1 -3 0 157.48 5.06
-1 3 0 174.61 5.19
1 3 0 151.98 5.10
-1 3 0 165.80 5.06
1 3 0 187.26 5.09
2 -3 0 1710.28 50.60
2 -3 0 1796.51 50.98
-2 -3 0 1724.05 50.78
-2 -3 0 1809.16 50.86
-2 -3 0 1859.38 50.83
-2 3 0 1613.98 50.66
-2 3 0 1732.12 50.68
2 3 0 1739.20 50.86
-3 -3 0 320.15 9.60
-3 -3 0 325.06 9.67
3 -3 0 311.03 9.85
-3 -3 0 314.05 9.63
3 3 0 311.14 9.53
3 3 0 340.90 9.69
3 3 0 325.22 9.55
-3 3 0 310.62 9.39
-3 3 0 313.92 9.38
-3 3 0 332.29 9.89
4 -3 0 257.91 8.29
-4 -3 0 260.45 8.07
-4 -3 0 253.69 7.95
-4 -3 0 257.18 7.91
-4 3 0 269.61 8.31
4 3 0 240.38 7.79
4 3 0 278.98 7.77
4 3 0 268.09 8.09
-5 -3 0 1.53 0.54
-5 -3 0 1.59 0.61
-5 -3 0 2.16 0.51
-5 3 0 2.55 0.83
-6 -3 0 3.26 0.78
-6 -3 0 5.17 0.87
-6 -3 0 2.92 0.64
-6 3 0 2.90 0.96
-7 -3 0 2.42 0.61
-7 -3 0 2.16 0.71
-7 -3 0 1.39 0.82
-7 3 0 2.40 1.09
-8 -3 0 28.56 1.54
-8 -3 0 28.01 2.08
-8 -3 0 28.09 1.72
-8 -3 0 27.92 1.99
-8 3 0 27.13 1.24
-8 3 0 26.94 2.54
-8 3 0 27.80 1.18
-9 -3 0 2.20 0.72
-9 -3 0 2.05 1.27
-9 -3 0 2.42 1.11
-9 -3 0 0.86 0.84
-9 3 0 2.74 0.48
-9 3 0 1.17 0.54
-9 3 0 1.47 1.28
-10 -3 0 99.02 4.03
-10 -3 0 104.21 3.90
-10 -3 0 107.70 4.72
-10 3 0 105.47 4.93
-10 3 0 104.94 3.59
-10 3 0 103.79 3.54
-11 -3 0 18.78 2.03
-11 -3 0 21.55 1.81
-11 -3 0 21.87 2.65
-11 3 0 19.77 2.82
-11 3 0 20.81 1.56
-11 3 0 20.78 1.48
-12 -3 0 64.18 3.19
-12 -3 0 70.51 4.13
-12 -3 0 59.70 4.20
-12 3 0 58.51 4.12
-12 3 0 62.72 2.66
-12 3 0 59.45 2.70
-13 -3 0 7.28 1.45
-13 -3 0 8.47 1.61
-13 -3 0 7.77 2.23
-13 3 0 12.51 1.73
-13 3 0 3.69 1.98
-13 3 0 7.22 1.14
-14 -3 0 24.14 2.83
-14 -3 0 25.60 2.70
-14 3 0 23.42 2.18
-14 3 0 24.52 3.86
-14 3 0 26.56 2.15
-15 -3 0 6.92 1.84
-15 -3 0 4.11 2.73
-15 -3 0 4.23 1.68
-15 3 0 5.12 1.42
-15 3 0 10.52 2.91
-15 3 0 4.54 1.40
-16 -3 0 30.15 3.36
-16 -3 0 30.47 3.60
-16 -3 0 40.72 5.69
-16 3 0 22.53 2.62
-16 3 0 25.90 2.65
-16 3 0 32.80 5.40
0 -4 0 9.11 6.87
-1 -4 0 235.56 7.37
-1 -4 0 250.09 7.27
-1 -4 0 247.39 7.32
1 -4 0 235.27 7.23
1 -4 0 235.25 7.37
-1 4 0 238.66 7.37
1 4 0 239.09 7.31
-1 4 0 233.30 7.26
-1 4 0 235.06 7.28
1 4 0 255.42 7.39
-2 -4 0 847.79 24.41
2 -4 0 805.60 24.59
-2 -4 0 841.17 24.46
2 -4 0 829.19 24.28
-2 -4 0 850.27 24.53
2 -4 0 811.59 24.27
2 4 0 844.72 24.40
-2 4 0 788.79 24.33
2 4 0 880.54 24.51
-2 4 0 869.84 24.62
-2 4 0 796.84 24.33
-3 -4 0 231.58 7.33
-3 -4 0 238.34 7.27
-3 -4 0 233.98 7.27
3 -4 0 229.84 7.51
-3 4 0 238.21 7.52
-3 4 0 231.56 7.09
3 4 0 243.54 7.26
-3 4 0 236.26 7.08
3 4 0 246.75 7.28
3 4 0 239.20 7.21
-4 -4 0 385.08 11.82
-4 -4 0 385.87 11.89
4 -4 0 380.35 12.15
-4 -4 0 374.56 11.86
-4 4 0 382.22 11.55
-4 4 0 382.16 11.57
-4 4 0 431.78 12.69
4 4 0 407.30 11.92
4 4 0 417.90 11.92
4 4 0 386.69 11.68
-5 -4 0 27.94 1.52
5 -4 0 23.80 1.84
-5 -4 0 28.14 1.56
-5 -4 0 29.17 1.45
5 4 0 29.24 1.15
-5 4 0 28.70 1.08
5 4 0 29.57 1.19
5 4 0 31.28 1.61
-5 4 0 28.49 1.93
-5 4 0 28.64 1.11
-6 -4 0 327.67 10.11
-6 -4 0 329.56 10.04
-6 -4 0 322.43 10.28
-6 4 0 332.69 10.61
-6 4 0 326.60 9.68
-6 4 0 327.19 9.67
-7 -4 0 31.29 1.83
-7 -4 0 32.33 1.97
-7 -4 0 33.38 1.67
-7 4 0 31.81 1.24
-7 4 0 31.14 1.53
-7 4 0 31.01 2.37
-8 -4 0 61.99 2.82
-8 -4 0 64.87 3.05
-8 -4 0 64.76 2.64
-8 4 0 68.23 3.57
-8 4 0 64.71 2.22
-8 4 0 64.48 2.26
-9 -4 0 44.95 2.79
-9 -4 0 41.68 2.39
-9 -4 0 43.25 2.72
-9 -4 0 44.04 2.16
-9 4 0 44.18 1.71
-9 4 0 43.21 1.80
-10 -4 0 7.85 1.61
-10 -4 0 7.49 1.94
-10 -4 0 8.49 1.25
-10 -4 0 9.70 1.55
-10 4 0 10.71 1.81
-10 4 0 8.73 1.14
-10 4 0 6.50 1.10
-11 -4 0 10.06 1.72
-11 -4 0 8.06 1.40
-11 -4 0 8.48 1.82
-11 4 0 10.22 1.37
-11 4 0 9.97 1.26
-11 4 0 8.47 1.85
-12 -4 0 1.39 1.26
-12 -4 0 2.90 1.65
-12 -4 0 1.96 1.05
-12 4 0 0.65 0.76
-12 4 0 1.69 0.91
-12 4 0 0.08 1.50
-13 -4 0 10.29 2.18
-13 -4 0 7.28 1.59
-13 -4 0 5.66 1.53
-13 4 0 9.44 1.60
-13 4 0 3.71 1.96
-13 4 0 7.53 1.09
-14 -4 0 11.31 2.67
-14 -4 0 10.87 1.90
-14 -4 0 10.32 1.83
-14 4 0 10.64 1.42
-14 4 0 11.19 1.34
-14 4 0 11.48 2.67
-15 -4 0 6.52 2.83
-15 -4 0 9.52 1.97
-15 -4 0 8.43 1.96
-15 4 0 7.36 1.37
-15 4 0 10.92 1.43
-15 4 0 8.66 2.84
-16 -4 0 1.83 1.77
-16 -4 0 -4.35 2.91
-16 -4 0 1.28 2.02
-16 4 0 -0.30 1.64
-16 4 0 6.13 2.95
-1 -5 0 34.72 1.55
1 -5 0 31.81 1.68
-1 -5 0 39.35 1.93
-1 -5 0 35.10 1.72
1 -5 0 32.85 1.63
1 5 0 33.12 1.54
-1 5 0 32.57 1.52
-1 5 0 31.60 1.51
-1 5 0 26.77 2.35
1 5 0 37.85 1.52
1 5 0 33.97 1.65
2 -5 0 396.96 12.23
-2 -5 0 420.49 12.49
-2 -5 0 432.04 12.33
2 -5 0 415.83 12.22
-2 -5 0 440.53 12.44
2 -5 0 403.12 12.53
-2 5 0 408.30 12.29
-2 5 0 433.07 12.56
2 5 0 347.55 12.35
2 5 0 435.48 12.47
2 5 0 422.38 12.31
-2 5 0 400.14 12.30
-3 -5 0 17.82 1.25
-3 -5 0 17.47 1.12
3 -5 0 17.82 0.75
3 -5 0 16.66 1.39
-3 -5 0 17.83 1.05
3 -5 0 15.83 0.72
3 5 0 17.44 1.03
-3 5 0 17.47 0.96
-3 5 0 16.64 1.32
-3 5 0 16.64 0.96
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2 -2 -8 28.82 2.15
2 -2 -8 26.94 2.09
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0 -2 -8 40.44 2.56
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-5 -2 9 8.09 1.34
-5 -2 9 8.53 1.15
5 -2 -9 10.02 1.37
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-5 2 9 6.96 1.30
-5 2 9 5.62 1.21
5 2 -9 7.59 1.10
5 2 -9 8.87 1.45
-3 -2 9 148.33 5.68
-3 -2 9 140.05 5.21
3 -2 -9 143.63 5.51
-3 -2 9 145.60 5.68
3 -2 -9 144.35 5.61
3 2 -9 143.60 5.55
-3 2 9 146.01 5.70
3 2 -9 143.81 5.30
3 2 -9 148.52 5.59
-3 2 9 143.06 5.46
-3 2 9 140.49 5.54
-2 -2 9 0.96 1.15
2 -2 -9 1.18 1.13
-2 -2 9 2.81 0.84
2 -2 -9 3.80 1.16
-2 -2 9 0.75 0.92
2 2 -9 1.13 0.83
2 2 -9 2.25 1.15
2 2 -9 2.23 0.92
-2 2 9 -0.41 1.10
-2 2 9 3.73 1.11
1 -2 -9 1.26 0.97
-1 -2 9 1.93 0.84
-1 -2 9 0.12 0.95
1 -2 -9 0.69 1.08
1 -2 -9 2.74 1.31
-1 -2 9 2.52 1.12
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1 2 -9 2.32 1.05
-1 2 9 3.10 1.32
-1 2 9 2.37 1.34
1 2 -9 1.06 0.99
1 2 -9 2.47 1.02
0 -2 9 44.37 2.85
0 -2 -9 50.43 2.94
0 -2 9 44.88 2.70
0 -2 9 44.46 3.02
0 -2 -9 47.81 2.92
0 -2 -9 47.40 3.07
0 2 -9 44.77 2.88
0 2 -9 45.63 2.91
0 2 -9 41.68 2.83
0 2 9 43.12 2.69
0 2 9 44.84 3.08
1 -2 9 75.16 3.95
-1 -2 -9 80.83 3.95
-1 -2 -9 83.37 3.91
-1 -2 -9 83.63 4.24
1 -2 9 77.89 3.71
1 2 9 79.27 3.71
-1 2 -9 78.19 3.98
-1 2 -9 79.68 3.89
1 2 9 72.21 4.14
-2 -2 -9 54.56 3.67
2 -2 9 51.88 2.98
-2 -2 -9 50.79 3.37
-2 -2 -9 56.48 3.32
-2 2 -9 54.65 3.37
-2 2 -9 54.40 3.39
2 2 9 55.76 3.06
-2 2 -9 50.41 3.45
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3 -2 9 0.16 0.81
-3 -2 -9 -0.40 1.51
-3 -2 -9 1.45 1.54
-3 2 -9 -0.28 1.33
-3 2 -9 1.62 1.30
3 2 9 1.48 0.97
-3 2 -9 0.32 1.48
-4 -2 -9 67.25 4.28
-4 -2 -9 71.73 4.07
4 -2 9 62.08 3.29
-4 -2 -9 58.65 5.94
-4 2 -9 66.40 4.24
4 2 9 70.22 3.43
-4 2 -9 69.54 3.94
-4 2 -9 66.39 3.83
-5 -2 -9 82.30 4.86
5 -2 9 81.50 3.77
-5 -2 -9 81.31 4.53
-5 -2 -9 78.25 4.52
-5 2 -9 85.57 4.47
-5 2 -9 82.99 4.47
-5 2 -9 86.47 4.78
-6 -2 -9 76.73 4.83
-6 -2 -9 81.70 4.61
-6 -2 -9 76.76 4.54
-6 2 -9 76.39 4.92
6 2 9 75.53 3.67
-6 2 -9 81.41 4.44
-6 2 -9 69.61 4.27
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-7 -2 -9 9.48 2.03
-7 -2 -9 9.22 2.24
-7 2 -9 9.39 2.32
-7 2 -9 10.71 2.69
7 2 9 9.20 1.36
-7 2 -9 7.09 1.79
-8 -2 -9 0.26 2.17
-8 -2 -9 0.87 1.78
-8 2 -9 0.25 1.58
-8 2 -9 -0.53 2.10
-8 2 -9 -1.19 1.73
-9 -2 -9 -1.86 1.74
-9 -2 -9 -0.89 2.24
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-9 2 -9 -0.18 1.76
-10 -2 -9 10.21 3.09
-10 -2 -9 5.23 2.35
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-10 2 -9 13.89 3.28
-11 -2 -9 17.12 5.54
-11 -2 -9 15.71 5.01
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-11 2 -9 12.52 3.62
-12 -2 -9 1.71 2.37
-12 -2 -9 0.31 3.24
-12 2 -9 6.24 3.42
-12 2 -9 -3.01 2.20
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-15 -3 9 1.89 2.11
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-14 -3 9 0.39 1.40
-14 -3 9 -1.54 1.31
-14 3 9 0.15 1.41
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13 -3 -9 10.17 1.81
-13 -3 9 12.36 1.98
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-13 3 9 9.19 1.63
12 -3 -9 2.33 1.34
-12 -3 9 0.71 1.35
-12 -3 9 -0.96 1.21
-12 3 9 0.92 1.15
-12 3 9 1.38 1.34
-11 -3 9 34.10 2.35
11 -3 -9 32.67 2.83
-11 -3 9 35.27 2.80
-11 -3 9 31.31 2.76
-11 3 9 36.02 2.77
-11 3 9 33.10 2.70
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-10 -3 9 5.98 1.09
-10 -3 9 6.24 1.45
10 -3 -9 7.01 1.48
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-10 3 9 4.79 1.28
-10 3 9 7.27 1.42
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9 -3 -9 52.47 3.06
-9 -3 9 45.51 2.25
-9 -3 9 46.43 3.01
-9 3 9 44.73 3.31
-9 3 9 48.30 2.99
9 3 -9 46.92 2.11
-9 3 9 50.36 2.99
-8 -3 9 1.42 0.82
-8 -3 9 -0.49 1.07
8 -3 -9 -1.15 1.14
8 3 -9 0.84 0.75
8 3 -9 1.41 0.72
-8 3 9 0.47 1.11
-8 3 9 1.10 1.17
-8 3 9 0.09 1.46
-7 -3 9 154.96 5.42
-7 -3 9 170.93 6.35
7 -3 -9 163.03 6.25
7 -3 -9 162.52 5.47
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-7 3 9 156.08 6.05
7 3 -9 164.98 5.49
7 3 -9 162.40 5.69
-7 3 9 165.46 6.19
-6 -3 9 44.80 2.23
6 -3 -9 48.60 2.41
-6 -3 9 46.84 3.42
6 -3 -9 47.84 2.91
-6 -3 9 43.78 2.97
6 3 -9 51.02 2.31
6 3 -9 47.07 2.50
-6 3 9 49.78 2.96
-6 3 9 46.82 2.92
-6 3 9 48.57 2.92
-5 -3 9 2.70 1.18
-5 -3 9 3.11 1.08
-5 -3 9 2.82 1.20
5 -3 -9 3.31 1.22
5 3 -9 3.85 0.99
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-5 3 9 4.07 1.20
-4 -3 9 23.06 2.25
-4 -3 9 19.05 1.64
4 -3 -9 21.72 2.26
-4 -3 9 23.03 2.38
4 3 -9 22.06 1.70
-4 3 9 16.47 2.10
-4 3 9 22.60 2.18
4 3 -9 21.40 1.94
-4 3 9 19.58 2.90
-3 -3 9 46.72 2.95
3 -3 -9 49.32 3.04
-3 -3 9 46.13 2.50
-3 -3 9 47.09 3.02
3 -3 -9 46.79 2.74
3 3 -9 45.33 2.48
-3 3 9 51.58 3.07
3 3 -9 49.27 2.82
-3 3 9 48.69 2.92
3 3 -9 52.72 3.09
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2 -3 -9 3.43 0.98
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2 -3 -9 3.99 1.25
-2 -3 9 2.30 0.89
2 -3 -9 3.48 1.26
2 3 -9 1.95 0.91
2 3 -9 3.28 0.93
2 3 -9 2.60 1.14
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1 -3 -9 122.47 5.10
-1 -3 9 128.93 5.23
1 -3 -9 127.26 5.26
-1 -3 9 122.32 4.87
1 -3 -9 124.30 4.99
1 3 -9 118.81 5.37
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1 3 -9 124.56 5.07
-1 3 9 126.23 5.25
-1 3 9 126.45 5.18
1 3 -9 125.99 5.13
0 -3 9 0.39 1.04
0 -3 -9 -0.92 1.16
0 -3 -9 1.07 1.08
0 -3 -9 0.65 1.17
0 -3 9 0.13 0.91
0 -3 9 -0.47 1.08
0 3 -9 0.19 0.99
0 3 -9 -1.93 0.95
0 3 9 -0.12 0.73
0 3 -9 -0.53 0.98
0 3 9 -0.45 1.11
1 -3 9 45.33 3.03
-1 -3 -9 45.45 3.24
-1 -3 -9 44.53 2.99
-1 -3 -9 49.11 3.00
1 -3 9 40.83 2.63
-1 3 -9 49.06 3.08
-1 3 -9 41.42 2.99
1 3 9 45.63 3.29
1 3 9 46.68 2.79
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-2 -3 -9 3.04 1.26
2 -3 9 4.39 1.10
-2 -3 -9 4.17 1.62
-2 -3 -9 1.31 1.21
2 3 9 4.99 1.19
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-2 3 -9 3.49 1.39
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3 -3 9 15.14 1.87
-3 -3 -9 19.99 2.64
-3 -3 -9 21.55 2.90
3 3 9 17.92 2.04
-3 3 -9 18.47 2.75
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4 -3 9 0.02 0.92
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-4 -3 -9 1.39 1.54
-4 -3 -9 -1.22 1.23
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-4 3 -9 0.40 1.37
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4 3 9 1.10 0.96
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5 -3 9 13.22 1.66
-5 -3 -9 9.55 2.03
-5 -3 -9 12.50 2.15
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-5 3 -9 12.99 2.31
-5 3 -9 12.72 1.96
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-6 -3 -9 0.38 1.60
-6 -3 -9 0.83 1.68
6 -3 9 0.28 1.60
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6 3 9 1.88 1.55
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-7 -3 -9 17.35 2.90
-7 -3 -9 11.99 2.31
7 -3 9 18.37 2.36
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7 3 9 13.87 2.07
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-8 -3 -9 1.26 2.77
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-8 3 -9 0.62 1.61
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-9 -3 -9 13.38 2.67
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-10 -3 -9 8.90 2.41
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-11 -3 -9 7.20 3.57
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-12 -3 -9 3.70 3.16
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-15 -4 9 15.26 2.74
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-14 -4 9 2.79 1.47
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-13 -4 9 45.98 3.54
-13 -4 9 51.93 2.55
13 -4 -9 51.81 3.65
-13 -4 9 59.27 3.70
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-12 -4 9 8.02 1.64
-12 -4 9 8.61 1.19
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12 -4 -9 9.99 1.78
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-11 -4 9 -1.13 1.01
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11 -4 -9 -0.05 1.33
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-11 4 9 0.25 1.22
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10 -4 -9 4.42 1.45
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-9 -4 9 0.14 1.08
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8 -4 -9 14.49 2.44
-8 -4 9 18.80 2.28
-8 -4 9 14.18 1.30
-8 -4 9 16.13 2.37
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-8 4 9 17.29 2.28
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7 -4 -9 100.68 3.63
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7 -4 -9 99.96 4.56
-7 -4 9 93.48 4.44
7 4 -9 96.41 3.87
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6 -4 -9 8.85 1.53
6 -4 -9 10.87 1.45
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6 4 -9 8.24 1.17
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5 -4 -9 1.80 1.20
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5 4 -9 0.51 0.67
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4 -4 -9 50.64 3.08
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-4 -4 9 51.58 3.00
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4 4 -9 47.93 2.38
-4 4 9 46.62 3.77
-4 4 9 49.52 2.97
4 4 -9 51.26 2.76
3 -4 -9 317.59 10.74
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3 -4 -9 319.33 10.88
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3 4 -9 317.94 10.38
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3 4 -9 320.14 10.79
3 4 -9 330.03 11.38
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2 -4 -9 67.43 3.47
2 -4 -9 71.53 3.77
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2 -4 -9 65.38 3.39
2 4 -9 69.84 3.56
2 4 -9 72.41 3.22
2 4 -9 74.04 3.57
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1 -4 -9 9.19 1.51
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1 -4 -9 5.52 1.44
1 -4 -9 10.55 1.56
-1 -4 9 8.66 1.62
-1 -4 9 7.39 1.37
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1 4 -9 5.87 2.12
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1 4 -9 4.79 1.34
1 4 -9 8.26 1.50
0 -4 -9 8.28 1.54
0 -4 -9 6.57 1.63
0 -4 9 6.52 1.53
0 -4 9 5.31 1.12
0 -4 9 8.11 1.45
0 -4 -9 5.33 1.27
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0 4 9 7.51 1.33
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1 -4 9 20.62 2.66
-1 -4 -9 21.60 2.78
1 -4 9 21.53 2.11
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-1 4 -9 27.60 2.41
-1 4 -9 23.51 2.49
1 4 9 20.46 2.71
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-2 -4 -9 33.67 2.96
2 -4 9 35.24 2.46
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2 4 9 32.93 2.50
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3 -4 9 304.78 10.41
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-4 -4 -9 0.45 1.40
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-12 -4 -9 3.23 3.27
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14 -5 -9 2.99 1.72
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13 -5 -9 3.54 1.72
-13 -5 9 -0.77 1.40
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-11 -5 9 -0.32 1.21
11 -5 -9 1.50 1.42
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10 -5 -9 11.53 1.81
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9 -5 -9 36.88 2.97
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-8 -5 9 6.63 1.57
8 -5 -9 8.19 1.77
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7 -5 -9 16.04 2.22
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7 5 -9 13.48 1.05
7 5 -9 12.04 1.58
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6 -5 -9 -0.23 0.80
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-6 -5 9 -0.12 0.62
6 -5 -9 -0.99 1.13
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6 5 -9 -0.28 0.61
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-5 -5 9 157.31 6.73
5 -5 -9 164.67 6.42
5 -5 -9 181.20 6.66
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-5 5 9 167.22 6.28
5 5 -9 167.39 5.56
4 -5 -9 34.06 2.77
-4 -5 9 34.74 2.77
-4 -5 9 35.21 2.70
4 5 -9 31.85 1.86
-4 5 9 34.28 2.53
-4 5 9 29.58 3.82
4 5 -9 33.55 2.35
-4 5 9 31.30 2.57
3 -5 -9 68.63 3.40
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-3 -5 9 68.38 2.98
3 -5 -9 71.05 3.73
-3 -5 9 62.11 5.45
3 5 -9 69.92 3.02
-3 5 9 68.51 3.67
-3 5 9 70.62 3.57
3 5 -9 65.13 3.41
-3 5 9 65.85 3.60
2 -5 -9 41.77 3.07
2 -5 -9 44.17 3.62
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-2 -5 9 43.22 2.69
2 -5 -9 44.00 2.78
-2 -5 9 44.33 2.45
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2 5 -9 42.73 2.74
2 5 -9 37.86 2.34
2 5 -9 43.43 2.81
-1 -5 9 86.46 3.92
-1 -5 9 88.37 4.07
-1 -5 9 92.08 4.38
1 -5 -9 94.46 4.28
1 -5 -9 89.47 4.47
1 -5 -9 90.12 4.15
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0 9 -16 1.49 2.53
-1 9 -16 2.32 2.79
-1 9 -16 2.54 2.72
-2 -9 -16 7.35 3.51
-2 -9 -16 7.56 3.70
-2 9 -16 12.30 3.17
-2 9 -16 13.69 3.35
9 -10 -16 5.59 3.05
-9 -10 16 -4.64 3.49
-9 10 16 -0.79 2.30
8 -10 -16 2.67 2.66
-8 -10 16 8.06 2.73
-8 10 16 1.20 2.93
7 -10 -16 6.72 2.87
-7 -10 16 13.86 3.04
-7 10 16 11.38 2.70
-6 -10 16 64.59 5.74
6 -10 -16 51.26 5.49
-6 10 16 68.35 5.31
-5 -10 16 2.32 2.62
5 -10 -16 0.92 2.67
-5 10 16 1.16 2.27
-4 -10 16 1.56 2.50
4 -10 -16 0.08 2.88
-4 10 16 3.27 2.53
4 10 -16 -3.09 1.91
-3 -10 16 3.35 2.36
3 -10 -16 3.72 2.78
-3 10 16 2.43 2.42
3 10 -16 2.43 2.04
-2 -10 16 4.81 2.48
-2 10 16 4.45 2.56
2 10 -16 -3.55 2.11
1 -10 -16 29.31 4.34
1 10 -16 28.36 3.47
-1 10 16 31.30 4.86
1 10 -16 27.34 4.57
0 -10 -16 7.25 3.48
0 10 -16 10.48 2.87
0 10 -16 15.48 3.21
0 10 16 16.07 3.01
-1 -10 -16 2.93 3.28
-1 10 -16 8.16 2.91
-1 10 -16 -0.64 2.76
-8 -11 16 -2.29 2.55
8 -11 -16 2.49 2.86
-8 11 16 3.89 2.40
7 -11 -16 2.66 2.99
-7 -11 16 10.52 3.06
-7 11 16 6.97 2.69
6 -11 -16 -0.81 2.57
-6 -11 16 9.71 3.05
-6 11 16 0.97 2.26
5 -11 -16 13.39 3.53
-5 -11 16 9.87 3.17
-5 11 16 10.28 2.62
-4 -11 16 4.01 2.57
4 -11 -16 2.50 3.38
4 11 -16 -1.53 1.84
-4 11 16 3.58 2.39
-3 -11 16 1.58 2.54
3 11 -16 6.88 2.18
-3 11 16 6.24 2.47
2 -11 -16 32.96 4.78
2 11 -16 25.25 4.01
-2 11 16 34.75 4.96
1 -11 -16 22.51 4.02
1 11 -16 18.45 3.13
-1 11 16 18.27 3.19
1 11 -16 22.20 3.47
0 -11 -16 -4.43 2.94
0 11 -16 -1.34 2.36
0 11 -16 -0.24 2.64
-1 -11 -16 -1.41 3.11
-1 11 -16 -2.55 2.46
-1 11 -16 7.59 2.73
-7 -12 16 -0.69 2.41
-7 12 16 5.53 3.93
-6 -12 16 17.59 3.43
-6 12 16 8.57 2.67
5 -12 -16 3.18 5.41
-5 -12 16 8.05 2.99
-5 12 16 10.10 2.76
4 -12 -16 5.63 3.15
-4 -12 16 4.30 2.74
-4 12 16 -0.52 2.39
3 -12 -16 6.66 3.29
-3 -12 16 -4.94 2.39
3 12 -16 2.12 2.03
-3 12 16 1.11 2.61
2 -12 -16 6.09 3.28
-2 -12 16 2.76 2.62
2 12 -16 1.84 2.33
-2 12 16 3.77 2.78
1 -12 -16 -3.26 3.09
-1 12 16 -2.34 2.60
1 12 -16 -2.70 2.32
0 -12 -16 3.12 3.45
0 12 -16 2.26 2.88
0 12 16 1.73 3.46
0 12 -16 -0.65 2.48
-6 -13 16 1.17 2.59
6 -13 -16 3.75 3.02
-6 13 16 -2.53 2.21
5 -13 -16 4.65 3.21
-5 -13 16 8.06 2.90
-5 13 16 8.83 2.80
4 -13 -16 8.03 3.01
-4 -13 16 0.20 2.70
-4 13 16 1.36 2.66
-3 -13 16 10.16 3.01
3 -13 -16 6.94 3.61
3 13 -16 10.78 2.34
-3 13 16 8.55 3.07
2 -13 -16 67.18 6.77
2 13 -16 60.94 4.81
-2 13 16 55.26 5.96
1 -13 -16 42.05 6.20
1 13 -16 47.71 4.98
-1 13 16 48.42 5.52
5 -14 -16 -0.08 3.07
-5 -14 16 1.83 2.96
-5 14 16 5.96 2.81
-4 -14 16 4.30 2.75
4 -14 -16 2.61 3.40
-4 14 16 -3.84 2.57
3 -14 -16 -3.54 3.40
-3 -14 16 4.55 2.62
-3 14 16 -3.14 2.87
2 -14 -16 3.59 3.52
9 0 -17 25.34 4.38
-9 0 17 20.96 3.57
-8 0 17 -3.49 2.42
8 0 -17 -3.41 2.15
-7 0 17 12.16 3.15
7 0 -17 5.54 2.49
-6 0 17 2.51 2.45
6 0 -17 -2.16 2.26
-5 0 17 32.27 5.10
5 0 -17 33.93 4.64
-4 0 17 3.44 2.46
4 0 -17 -0.65 2.27
3 0 -17 12.71 2.88
-2 0 17 8.34 2.45
2 0 -17 -4.88 2.42
-1 0 17 112.37 6.67
1 0 -17 108.43 6.87
0 0 -17 1.00 2.84
-1 0 -17 19.63 3.86
-1 0 -17 21.10 3.46
9 -1 -17 30.52 4.16
-9 -1 17 25.13 3.52
-9 1 17 26.77 4.03
8 -1 -17 0.38 2.32
-8 -1 17 -1.14 2.54
8 1 -17 -2.05 2.12
-8 1 17 1.39 2.82
7 -1 -17 -3.14 2.30
-7 -1 17 5.73 2.63
-7 1 17 -0.29 2.41
7 1 -17 -1.12 2.25
6 -1 -17 0.77 2.48
-6 -1 17 1.84 2.45
-6 1 17 2.88 2.45
6 1 -17 -1.46 2.37
5 -1 -17 27.91 4.52
-5 -1 17 35.71 5.08
-5 1 17 37.04 5.43
5 1 -17 27.22 3.51
4 -1 -17 11.28 2.97
-4 -1 17 14.23 2.96
4 1 -17 13.59 2.91
-4 1 17 15.38 2.99
3 -1 -17 6.67 2.69
-3 -1 17 9.17 2.96
3 1 -17 6.31 2.69
2 -1 -17 0.08 2.65
-2 1 17 9.19 2.48
2 1 -17 2.41 2.49
1 -1 -17 7.67 3.07
-1 1 17 15.07 2.76
0 1 -17 -4.35 2.66
0 1 -17 -0.44 3.30
-1 -1 -17 23.53 3.92
-1 -1 -17 27.92 4.01
-1 1 -17 30.28 4.21
-1 1 -17 29.93 5.05
-9 -2 17 25.15 3.54
-9 2 17 17.95 3.61
-8 -2 17 6.04 2.86
8 -2 -17 3.05 2.52
8 2 -17 1.67 2.36
-8 2 17 7.60 5.04
7 -2 -17 -1.43 2.42
-7 -2 17 9.39 2.79
7 2 -17 0.67 2.10
-7 2 17 8.53 2.83
-6 -2 17 0.41 2.52
6 -2 -17 3.07 2.48
-6 2 17 4.85 2.79
6 2 -17 -1.52 2.35
5 -2 -17 -0.41 2.42
-5 -2 17 -3.19 2.23
5 2 -17 3.02 2.30
-5 2 17 3.33 2.39
-4 -2 17 -2.00 2.30
4 -2 -17 2.49 2.56
4 2 -17 -2.86 2.30
-4 2 17 5.28 2.50
-3 -2 17 2.58 2.68
3 -2 -17 -1.10 2.37
-3 2 17 7.03 2.44
3 2 -17 -3.19 2.13
-2 -2 17 17.39 3.23
2 -2 -17 13.01 2.99
2 2 -17 10.17 3.03
-2 2 17 16.18 2.89
1 -2 -17 0.56 2.77
-1 -2 17 2.66 2.51
1 2 -17 0.48 2.68
-1 2 17 -0.64 2.31
0 2 -17 42.59 5.91
0 2 -17 28.37 4.79
-1 -2 -17 11.10 3.58
-1 -2 -17 8.44 3.57
-1 2 -17 12.59 3.50
-1 2 -17 10.36 3.48
-8 -3 17 10.02 3.07
8 -3 -17 8.57 2.76
7 -3 -17 16.07 3.17
-7 -3 17 22.35 3.49
7 3 -17 17.85 2.60
-7 3 17 21.64 3.49
-6 -3 17 -0.87 2.26
6 -3 -17 0.65 2.42
-6 3 17 7.19 2.67
6 3 -17 -0.89 2.21
5 -3 -17 -3.82 2.56
-5 -3 17 -0.84 2.37
5 3 -17 -0.18 2.27
-5 3 17 3.45 2.51
4 -3 -17 7.11 2.85
-4 -3 17 4.11 2.49
-4 3 17 5.98 2.43
4 3 -17 6.87 2.56
-3 -3 17 11.44 3.14
3 -3 -17 11.97 2.91
-3 3 17 11.63 2.78
3 3 -17 9.47 2.90
2 -3 -17 2.98 2.54
-2 -3 17 6.57 2.57
-2 3 17 -1.48 2.35
2 3 -17 -4.58 2.57
1 -3 -17 -5.67 2.69
-1 -3 17 5.56 2.34
-1 3 17 -4.34 2.28
1 3 -17 2.38 2.67
0 -3 -17 -3.14 3.22
0 3 -17 -5.57 4.02
0 3 -17 -2.32 2.35
-1 -3 -17 -2.42 3.05
-1 3 -17 2.08 4.54
-8 -4 17 5.75 3.07
8 -4 -17 0.32 2.55
7 -4 -17 -0.32 2.50
-7 -4 17 5.74 2.59
7 4 -17 3.84 2.42
-7 4 17 6.10 2.68
-6 -4 17 3.27 2.42
6 -4 -17 2.18 2.34
6 4 -17 -1.96 2.13
-6 4 17 6.68 2.41
5 -4 -17 29.08 4.89
-5 -4 17 21.59 3.35
-5 4 17 29.86 4.64
5 4 -17 23.57 4.03
4 -4 -17 3.86 2.66
-4 -4 17 1.03 2.67
-4 4 17 0.08 2.31
4 4 -17 0.34 2.16
-3 -4 17 -2.04 2.19
3 -4 -17 2.30 2.50
-3 4 17 1.37 2.48
2 -4 -17 4.58 2.65
-2 -4 17 1.51 2.20
-2 4 17 4.28 2.59
2 4 -17 3.56 2.57
-1 -4 17 18.22 3.34
1 -4 -17 6.77 4.09
1 4 -17 4.34 2.73
-1 4 17 10.12 2.67
0 -4 -17 3.27 3.19
0 4 -17 6.50 2.78
0 4 -17 7.75 4.32
8 -5 -17 108.56 6.78
-8 -5 17 122.02 8.54
-8 5 17 121.62 8.01
-7 -5 17 4.92 2.56
7 -5 -17 2.12 2.61
-7 5 17 3.95 2.53
-6 -5 17 7.71 2.88
6 -5 -17 13.04 2.85
-6 5 17 10.48 2.82
6 5 -17 3.86 2.28
-5 -5 17 2.29 2.50
5 -5 -17 1.64 2.75
5 5 -17 -0.59 2.15
-5 5 17 0.14 2.25
-4 -5 17 1.68 2.34
4 -5 -17 3.77 2.84
-4 5 17 6.60 2.84
4 5 -17 5.99 2.34
3 -5 -17 28.17 4.81
-3 -5 17 20.77 3.67
3 5 -17 26.92 3.46
-3 5 17 23.32 3.57
-2 -5 17 4.26 2.87
2 -5 -17 6.09 2.92
-2 5 17 -2.29 2.35
2 5 -17 3.96 2.69
1 -5 -17 4.36 4.80
-1 5 17 8.48 2.75
1 5 -17 3.96 2.60
0 -5 -17 -3.61 2.87
0 5 -17 0.76 2.67
8 -6 -17 1.52 2.73
-8 -6 17 4.14 3.46
-8 6 17 1.69 2.47
-7 -6 17 6.48 3.02
7 -6 -17 1.88 2.69
-7 6 17 6.31 2.47
-6 -6 17 13.87 2.95
6 -6 -17 13.25 3.21
6 6 -17 8.71 2.73
-6 6 17 11.26 2.65
-5 -6 17 3.40 2.31
5 -6 -17 1.24 2.83
5 6 -17 5.19 2.23
-5 6 17 2.81 2.53
-4 -6 17 3.49 2.69
4 -6 -17 6.20 2.92
-4 6 17 4.64 2.50
4 6 -17 5.35 2.24
-3 -6 17 79.93 6.33
3 -6 -17 78.87 6.27
3 6 -17 74.93 5.55
-3 6 17 83.61 6.35
-2 -6 17 -0.20 2.32
2 6 -17 -3.43 2.37
-2 6 17 1.41 2.54
1 -6 -17 0.97 3.03
1 6 -17 11.67 2.87
-1 6 17 5.71 2.66
0 6 -17 -3.52 2.47
-7 -7 17 -3.94 2.49
7 -7 -17 0.93 2.72
-7 7 17 4.85 3.18
-6 -7 17 7.74 3.12
6 -7 -17 11.12 3.00
-6 7 17 7.83 2.74
5 -7 -17 20.76 3.55
-5 -7 17 21.17 3.75
5 7 -17 18.02 2.66
-5 7 17 18.75 3.35
-4 -7 17 4.05 2.42
4 -7 -17 4.99 3.08
4 7 -17 6.94 2.38
-4 7 17 5.80 2.71
-3 -7 17 1.34 2.61
3 -7 -17 4.63 4.05
3 7 -17 0.14 2.50
-3 7 17 8.12 2.68
-2 -7 17 -1.58 2.35
2 -7 -17 5.11 3.39
2 7 -17 2.80 2.59
1 -7 -17 7.02 3.12
-1 7 17 12.34 2.88
1 7 -17 5.12 2.66
-7 -8 17 3.68 2.78
7 -8 -17 2.89 2.86
6 -8 -17 3.32 2.74
-6 -8 17 -1.70 2.68
-6 8 17 3.43 2.58
-5 -8 17 8.17 3.14
5 -8 -17 2.02 2.81
-5 8 17 6.63 2.60
4 -8 -17 3.93 4.71
-4 -8 17 6.34 2.94
-4 8 17 5.25 2.75
-3 -8 17 2.20 2.64
3 -8 -17 -2.41 3.64
-3 8 17 -0.62 2.61
-2 -8 17 0.93 2.69
2 -8 -17 0.59 3.16
2 8 -17 -3.10 2.34
-2 8 17 5.91 2.79
1 -8 -17 -4.45 2.87
1 8 -17 6.50 2.75
-1 8 17 2.62 2.66
-6 -9 17 2.09 2.88
6 -9 -17 1.79 4.86
-6 9 17 1.52 2.38
-5 -9 17 2.41 2.84
-5 9 17 5.34 2.57
4 -9 -17 -3.52 3.09
-4 -9 17 2.66 2.97
-4 9 17 -1.64 2.45
3 -9 -17 2.71 3.21
-3 -9 17 0.73 2.61
3 9 -17 -0.94 2.35
-3 9 17 1.62 2.74
2 -9 -17 2.08 3.30
-2 9 17 -1.30 2.50
2 9 -17 1.77 2.46
-4 -10 17 7.60 3.15
4 -10 -17 -2.31 3.08
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
;
_shelx_hkl_checksum 70152
_shelx_res_file
;
TITL z162_4_0m_a.res in P2(1)/n
z162_4_0m_a.res
created by SHELXL-2018/3 at 20:25:32 on 12-Jul-2022
REM Old TITL Integration of 1-butyl-2,3-bis(dicyclohe
REM SHELXT solution in P2(1)/n
REM R1 0.184, Rweak 0.012, Alpha 0.047, Orientation as input
REM Formula found by SHELXT: C1S N3 Cl
CELL 0.71076 12.2534 22.6986 12.8843 90 104.164 90
ZERR 4 0.003 0.0067 0.0032 0 0.007 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Cl N
UNIT 148 240 4 12
RIGU C7A C7
SIMU 0.003 0.006 2 C7A C7
L.S. 32
PLAN 12
SIZE 0.164 0.529 0.547
TEMP -173
CONF
MPLA N1 N2 N3 C1 C2 C3
BOND $H
LIST 6
MORE -1
fmap 2
acta
SHEL 99999 0.76
REM
REM
REM
WGHT 0.060500 2.377700
EXTI 0.008137
FVAR 0.33141 0.70898
CL1 3 0.442955 0.745521 0.693732 11.00000 0.03692 0.02768 =
0.02322 -0.00049 -0.00559 -0.01656
N1 4 0.368086 0.619969 0.640211 11.00000 0.03711 0.01934 =
0.01934 0.00021 -0.01277 -0.00477
N2 4 0.280589 0.476714 0.522281 11.00000 0.02699 0.01642 =
0.01739 -0.00203 -0.00133 0.00602
N3 4 0.167098 0.618038 0.382944 11.00000 0.01686 0.01378 =
0.01228 -0.00097 -0.00209 0.00137
C1 1 0.306248 0.588436 0.561403 11.00000 0.01794 0.01848 =
0.01660 0.00132 -0.00169 0.00116
C2 1 0.272262 0.535052 0.513601 11.00000 0.01533 0.01854 =
0.01286 -0.00094 0.00027 0.00279
C3 1 0.230001 0.587030 0.462566 11.00000 0.01420 0.01676 =
0.01377 -0.00226 0.00170 -0.00052
C4 1 0.426577 0.596548 0.743856 11.00000 0.02860 0.02596 =
0.01586 0.00025 -0.00807 -0.00200
AFIX 23
H4A 2 0.482194 0.625847 0.781488 11.00000 -1.20000
H4B 2 0.468020 0.560497 0.733256 11.00000 -1.20000
AFIX 0
C5 1 0.345333 0.581873 0.812980 11.00000 0.02507 0.03431 =
0.02617 -0.01155 -0.00067 0.00348
AFIX 23
H5A 2 0.299691 0.617193 0.818508 11.00000 -1.20000
H5B 2 0.293374 0.550454 0.777551 11.00000 -1.20000
AFIX 0
C6 1 0.404701 0.561763 0.924213 11.00000 0.04142 0.06156 =
0.02172 -0.00499 0.00677 -0.00928
PART 1
AFIX 23
H6AA 2 0.453690 0.528001 0.917569 21.00000 -1.20000
H6AB 2 0.454139 0.594103 0.959793 21.00000 -1.20000
AFIX 23
PART 2
H6BC 2 0.463745 0.589993 0.959547 -21.00000 -1.20000
H6BD 2 0.438414 0.522186 0.923334 -21.00000 -1.20000
AFIX 0
PART 1
C7 1 0.330264 0.543687 0.995612 21.00000 0.04395 0.09059 =
0.02568 -0.01233 0.01188 -0.01915
AFIX 33
H7A 2 0.376946 0.531504 1.065397 21.00000 -1.50000
H7B 2 0.282871 0.577033 1.005181 21.00000 -1.50000
H7C 2 0.282420 0.510733 0.962831 21.00000 -1.50000
AFIX 0
PART 2
C7A 1 0.302039 0.560729 0.980430 -21.00000 0.04718 0.08527 =
0.02852 -0.01700 0.01646 -0.02356
AFIX 33
H7AA 2 0.329164 0.548113 1.055049 -21.00000 -1.50000
H7AB 2 0.269538 0.600292 0.978288 -21.00000 -1.50000
H7AC 2 0.244456 0.533150 0.942430 -21.00000 -1.50000
AFIX 0
PART 0
C8 1 0.362211 0.452556 0.617742 11.00000 0.02451 0.01997 =
0.01673 -0.00100 -0.00229 0.00706
AFIX 13
H8 2 0.381382 0.485489 0.670631 11.00000 -1.20000
AFIX 0
C9 1 0.470840 0.432896 0.594471 11.00000 0.02379 0.05071 =
0.03370 0.01908 0.01122 0.00753
AFIX 23
H9A 2 0.502862 0.465328 0.559880 11.00000 -1.20000
H9B 2 0.456679 0.398984 0.544653 11.00000 -1.20000
AFIX 0
C10 1 0.554726 0.415048 0.699012 11.00000 0.02177 0.05860 =
0.03951 0.02299 0.00627 0.01129
AFIX 23
H10A 2 0.624144 0.399694 0.682382 11.00000 -1.20000
H10B 2 0.575268 0.450269 0.744965 11.00000 -1.20000
AFIX 0
C11 1 0.507110 0.369031 0.758840 11.00000 0.03533 0.02488 =
0.02542 0.00457 -0.00329 0.00386
AFIX 23
H11A 2 0.560159 0.362242 0.829220 11.00000 -1.20000
H11B 2 0.499093 0.331562 0.718347 11.00000 -1.20000
AFIX 0
C12 1 0.394649 0.386601 0.775772 11.00000 0.02958 0.07278 =
0.02985 0.02708 0.00597 0.00273
AFIX 23
H12A 2 0.404691 0.420050 0.826542 11.00000 -1.20000
H12B 2 0.362632 0.353219 0.807993 11.00000 -1.20000
AFIX 0
C13 1 0.312729 0.404333 0.671296 11.00000 0.01888 0.10181 =
0.02839 0.03387 0.00271 -0.00302
AFIX 23
H13A 2 0.295939 0.369777 0.623135 11.00000 -1.20000
H13B 2 0.241307 0.418020 0.686061 11.00000 -1.20000
AFIX 0
C14 1 0.228998 0.437334 0.434227 11.00000 0.03343 0.01578 =
0.01657 -0.00207 0.00111 -0.00012
AFIX 13
H14 2 0.251060 0.396403 0.459615 11.00000 -1.20000
AFIX 0
C15 1 0.101373 0.439615 0.409043 11.00000 0.03228 0.03295 =
0.01983 0.00494 0.00028 -0.00717
AFIX 23
H15A 2 0.075663 0.480402 0.389687 11.00000 -1.20000
H15B 2 0.075736 0.428155 0.473345 11.00000 -1.20000
AFIX 0
C16 1 0.049276 0.397999 0.316276 11.00000 0.05223 0.03480 =
0.02918 0.00688 -0.00962 -0.01846
AFIX 23
H16A 2 0.065028 0.356690 0.339859 11.00000 -1.20000
H16B 2 -0.033395 0.403439 0.296143 11.00000 -1.20000
AFIX 0
C17 1 0.096332 0.409605 0.218912 11.00000 0.06354 0.02198 =
0.02053 -0.00352 -0.00962 -0.00532
AFIX 23
H17A 2 0.064423 0.380550 0.162311 11.00000 -1.20000
H17B 2 0.073038 0.449374 0.190386 11.00000 -1.20000
AFIX 0
C18 1 0.222954 0.405512 0.246334 11.00000 0.06673 0.03038 =
0.02012 -0.00753 0.00296 0.01266
AFIX 23
H18A 2 0.250416 0.415061 0.182158 11.00000 -1.20000
H18B 2 0.246121 0.364657 0.268072 11.00000 -1.20000
AFIX 0
C19 1 0.276023 0.447449 0.336397 11.00000 0.03495 0.02866 =
0.02050 -0.00218 0.00625 0.01067
AFIX 23
H19A 2 0.261060 0.488590 0.311459 11.00000 -1.20000
H19B 2 0.358567 0.441498 0.356404 11.00000 -1.20000
AFIX 0
C20 1 0.100544 0.589999 0.284370 11.00000 0.01572 0.01511 =
0.01272 -0.00211 -0.00133 0.00230
AFIX 13
H20 2 0.121932 0.547404 0.287367 11.00000 -1.20000
AFIX 0
C21 1 -0.025574 0.593165 0.277774 11.00000 0.01616 0.02675 =
0.01778 -0.00622 0.00067 -0.00226
AFIX 23
H21A 2 -0.048940 0.634910 0.277906 11.00000 -1.20000
H21B 2 -0.041475 0.573704 0.341256 11.00000 -1.20000
AFIX 0
C22 1 -0.093118 0.562989 0.175978 11.00000 0.01748 0.03486 =
0.02509 -0.00989 -0.00147 -0.00237
AFIX 23
H22A 2 -0.076043 0.520300 0.179794 11.00000 -1.20000
H22B 2 -0.174555 0.567825 0.170890 11.00000 -1.20000
AFIX 0
C23 1 -0.065156 0.588934 0.076594 11.00000 0.02435 0.03319 =
0.01815 -0.00583 -0.00691 0.00621
AFIX 23
H23A 2 -0.106868 0.567204 0.012491 11.00000 -1.20000
H23B 2 -0.089479 0.630630 0.068675 11.00000 -1.20000
AFIX 0
C24 1 0.060455 0.585323 0.083838 11.00000 0.02702 0.02771 =
0.01289 -0.00214 0.00099 0.00578
AFIX 23
H24A 2 0.076785 0.604027 0.019878 11.00000 -1.20000
H24B 2 0.083535 0.543480 0.085098 11.00000 -1.20000
AFIX 0
C25 1 0.127750 0.616162 0.184479 11.00000 0.01723 0.02312 =
0.01505 0.00026 0.00186 0.00433
AFIX 23
H25A 2 0.109634 0.658734 0.180255 11.00000 -1.20000
H25B 2 0.209217 0.611798 0.189237 11.00000 -1.20000
AFIX 0
C26 1 0.155507 0.682254 0.396460 11.00000 0.01705 0.01251 =
0.01525 -0.00062 0.00053 0.00131
AFIX 13
H26 2 0.099398 0.696644 0.331400 11.00000 -1.20000
AFIX 0
C27 1 0.108607 0.697334 0.492748 11.00000 0.02130 0.01947 =
0.01854 -0.00355 0.00457 -0.00104
AFIX 23
H27A 2 0.037198 0.675821 0.487607 11.00000 -1.20000
H27B 2 0.162771 0.684987 0.559541 11.00000 -1.20000
AFIX 0
C28 1 0.087838 0.763467 0.495787 11.00000 0.02324 0.02160 =
0.02483 -0.00673 0.00418 0.00121
AFIX 23
H28A 2 0.028444 0.774989 0.432041 11.00000 -1.20000
H28B 2 0.060970 0.773161 0.560235 11.00000 -1.20000
AFIX 0
C29 1 0.194807 0.798148 0.497786 11.00000 0.02709 0.01702 =
0.02948 -0.00535 -0.00015 -0.00168
AFIX 23
H29A 2 0.251074 0.790334 0.565857 11.00000 -1.20000
H29B 2 0.177627 0.840825 0.494357 11.00000 -1.20000
AFIX 0
C30 1 0.243955 0.781221 0.404054 11.00000 0.02433 0.01640 =
0.02810 0.00311 0.00236 -0.00355
AFIX 23
H30A 2 0.315816 0.802469 0.410204 11.00000 -1.20000
H30B 2 0.191359 0.793486 0.336272 11.00000 -1.20000
AFIX 0
C31 1 0.264842 0.715059 0.400779 11.00000 0.01877 0.01826 =
0.01908 0.00139 0.00317 -0.00138
AFIX 23
H31A 2 0.292722 0.705234 0.336957 11.00000 -1.20000
H31B 2 0.322722 0.703020 0.465293 11.00000 -1.20000
AFIX 0
C1S 1 0.689080 0.746473 0.544107 11.00000 0.05484 0.02812 =
0.03714 0.00167 0.01345 -0.00116
AFIX 43
H1S 2 0.696225 0.738475 0.617844 11.00000 -1.20000
AFIX 0
C2S 1 0.783380 0.744719 0.502403 11.00000 0.03476 0.04047 =
0.05539 0.00350 0.00555 0.00199
AFIX 43
H2S 2 0.855070 0.735644 0.547561 11.00000 -1.20000
AFIX 0
C3S 1 0.772657 0.756181 0.395329 11.00000 0.03942 0.03782 =
0.05740 -0.00417 0.02291 -0.00942
AFIX 43
H3S 2 0.836697 0.754721 0.366155 11.00000 -1.20000
AFIX 0
C4S 1 0.668122 0.769803 0.330779 11.00000 0.05843 0.02769 =
0.03888 -0.00113 0.01368 -0.01270
AFIX 43
H4S 2 0.660378 0.777832 0.256966 11.00000 -1.20000
AFIX 0
C5S 1 0.574862 0.771833 0.372746 11.00000 0.03805 0.02407 =
0.04995 -0.00257 0.00102 -0.00068
AFIX 43
H5S 2 0.503360 0.781612 0.327955 11.00000 -1.20000
AFIX 0
C6S 1 0.585125 0.759809 0.478589 11.00000 0.03407 0.02614 =
0.05320 -0.00773 0.01714 -0.00185
AFIX 43
H6S 2 0.520582 0.760638 0.507068 11.00000 -1.20000
AFIX 0
H1 2 0.371036 0.656707 0.633725 11.00000 0.03545
HKLF 4
REM z162_4_0m_a.res in P2(1)/n
REM wR2 = 0.136156, GooF = S = 1.01948, Restrained GooF = 1.01928 for all data
REM R1 = 0.054835 for 6516 Fo > 4sig(Fo) and 0.070781 for all 8072 data
REM 385 parameters refined using 6 restraints
END
WGHT 0.0605 2.3778
REM Highest difference peak 0.546, deepest hole -0.403, 1-sigma level 0.061
Q1 1 0.5248 0.3942 0.6358 11.00000 0.05 0.55
Q2 1 0.1656 0.4522 0.4003 11.00000 0.05 0.45
Q3 1 0.3054 0.4373 0.6804 11.00000 0.05 0.38
Q4 1 0.2326 0.4258 0.3008 11.00000 0.05 0.38
Q5 1 0.5127 0.4023 0.7424 11.00000 0.05 0.37
Q6 1 0.4204 0.6003 0.8378 11.00000 0.05 0.33
Q7 1 0.1178 0.6043 0.2379 11.00000 0.05 0.33
Q8 1 0.5869 0.7519 0.4181 11.00000 0.05 0.31
Q9 1 0.3555 0.3940 0.7199 11.00000 0.05 0.31
Q10 1 0.3291 0.5570 0.8607 11.00000 0.05 0.28
Q11 1 0.1001 0.7301 0.4965 11.00000 0.05 0.28
Q12 1 0.2502 0.4639 0.4755 11.00000 0.05 0.28
;
_shelx_res_checksum 66262
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
Cl Cl1 0.44296(4) 0.74552(2) 0.69373(3) 0.03152(13) Uani d 1 . .
N N1 0.36809(13) 0.61997(7) 0.64021(11) 0.0287(3) Uani d 1 . .
N N2 0.28059(11) 0.47671(6) 0.52228(11) 0.0214(3) Uani d 1 . .
N N3 0.16710(10) 0.61804(5) 0.38294(10) 0.0153(3) Uani d 1 . .
C C1 0.30625(12) 0.58844(7) 0.56140(12) 0.0187(3) Uani d 1 . .
C C2 0.27226(12) 0.53505(7) 0.51360(11) 0.0161(3) Uani d 1 . .
C C3 0.23000(12) 0.58703(6) 0.46257(11) 0.0152(3) Uani d 1 . .
C C4 0.42658(14) 0.59655(8) 0.74386(13) 0.0258(4) Uani d 1 . .
H H4A 0.482194 0.625847 0.781488 0.031 Uiso calc 1 . .
H H4B 0.468020 0.560497 0.733256 0.031 Uiso calc 1 . .
C C5 0.34533(15) 0.58187(9) 0.81298(14) 0.0297(4) Uani d 1 . .
H H5A 0.299691 0.617193 0.818508 0.036 Uiso calc 1 . .
H H5B 0.293374 0.550454 0.777551 0.036 Uiso calc 1 . .
C C6 0.40470(18) 0.56176(11) 0.92421(15) 0.0417(5) Uani d 1 . .
H H6AA 0.453690 0.528001 0.917569 0.050 Uiso calc 0.71(3) A 1
H H6AB 0.454139 0.594103 0.959793 0.050 Uiso calc 0.71(3) A 1
H H6BC 0.463745 0.589993 0.959547 0.050 Uiso calc 0.29(3) A 2
H H6BD 0.438414 0.522186 0.923334 0.050 Uiso calc 0.29(3) A 2
C C7 0.3303(10) 0.5437(7) 0.9956(7) 0.053(2) Uani d 0.71(3) A 1
H H7A 0.376946 0.531504 1.065397 0.079 Uiso calc 0.71(3) A 1
H H7B 0.282871 0.577033 1.005181 0.079 Uiso calc 0.71(3) A 1
H H7C 0.282420 0.510733 0.962831 0.079 Uiso calc 0.71(3) A 1
C C7A 0.302(2) 0.5607(13) 0.980(2) 0.052(3) Uani d 0.29(3) A 2
H H7AA 0.329164 0.548113 1.055049 0.079 Uiso calc 0.29(3) A 2
H H7AB 0.269538 0.600292 0.978288 0.079 Uiso calc 0.29(3) A 2
H H7AC 0.244456 0.533150 0.942430 0.079 Uiso calc 0.29(3) A 2
C C8 0.36221(13) 0.45256(7) 0.61774(12) 0.0217(3) Uani d 1 . .
H H8 0.381382 0.485489 0.670631 0.026 Uiso calc 1 . .
C C9 0.47084(15) 0.43290(10) 0.59447(16) 0.0353(4) Uani d 1 . .
H H9A 0.502862 0.465328 0.559880 0.042 Uiso calc 1 . .
H H9B 0.456679 0.398984 0.544653 0.042 Uiso calc 1 . .
C C10 0.55473(15) 0.41505(11) 0.69901(17) 0.0402(5) Uani d 1 . .
H H10A 0.624144 0.399694 0.682382 0.048 Uiso calc 1 . .
H H10B 0.575268 0.450269 0.744965 0.048 Uiso calc 1 . .
C C11 0.50711(16) 0.36903(8) 0.75884(15) 0.0304(4) Uani d 1 . .
H H11A 0.560159 0.362242 0.829220 0.036 Uiso calc 1 . .
H H11B 0.499093 0.331562 0.718347 0.036 Uiso calc 1 . .
C C12 0.39465(16) 0.38660(12) 0.77577(17) 0.0443(6) Uani d 1 . .
H H12A 0.404691 0.420050 0.826542 0.053 Uiso calc 1 . .
H H12B 0.362632 0.353219 0.807993 0.053 Uiso calc 1 . .
C C13 0.31273(15) 0.40433(13) 0.67130(17) 0.0502(7) Uani d 1 . .
H H13A 0.295939 0.369777 0.623135 0.060 Uiso calc 1 . .
H H13B 0.241307 0.418020 0.686061 0.060 Uiso calc 1 . .
C C14 0.22900(14) 0.43733(7) 0.43423(12) 0.0228(3) Uani d 1 . .
H H14 0.251060 0.396403 0.459615 0.027 Uiso calc 1 . .
C C15 0.10137(15) 0.43961(8) 0.40904(14) 0.0294(4) Uani d 1 . .
H H15A 0.075663 0.480402 0.389687 0.035 Uiso calc 1 . .
H H15B 0.075736 0.428155 0.473345 0.035 Uiso calc 1 . .
C C16 0.04928(19) 0.39800(10) 0.31628(16) 0.0421(5) Uani d 1 . .
H H16A 0.065028 0.356690 0.339859 0.051 Uiso calc 1 . .
H H16B -0.033395 0.403439 0.296143 0.051 Uiso calc 1 . .
C C17 0.09633(19) 0.40960(8) 0.21891(15) 0.0388(5) Uani d 1 . .
H H17A 0.064423 0.380550 0.162311 0.047 Uiso calc 1 . .
H H17B 0.073038 0.449374 0.190386 0.047 Uiso calc 1 . .
C C18 0.2230(2) 0.40551(9) 0.24633(15) 0.0404(5) Uani d 1 . .
H H18A 0.250416 0.415061 0.182158 0.048 Uiso calc 1 . .
H H18B 0.246121 0.364657 0.268072 0.048 Uiso calc 1 . .
C C19 0.27602(15) 0.44745(8) 0.33640(13) 0.0281(4) Uani d 1 . .
H H19A 0.261060 0.488590 0.311459 0.034 Uiso calc 1 . .
H H19B 0.358567 0.441498 0.356404 0.034 Uiso calc 1 . .
C C20 0.10054(12) 0.59000(6) 0.28437(11) 0.0154(3) Uani d 1 . .
H H20 0.121932 0.547404 0.287367 0.018 Uiso calc 1 . .
C C21 -0.02557(12) 0.59316(7) 0.27777(12) 0.0208(3) Uani d 1 . .
H H21A -0.048940 0.634910 0.277906 0.025 Uiso calc 1 . .
H H21B -0.041475 0.573704 0.341256 0.025 Uiso calc 1 . .
C C22 -0.09312(14) 0.56299(8) 0.17598(14) 0.0270(4) Uani d 1 . .
H H22A -0.076043 0.520300 0.179794 0.032 Uiso calc 1 . .
H H22B -0.174555 0.567825 0.170890 0.032 Uiso calc 1 . .
C C23 -0.06516(14) 0.58893(8) 0.07659(13) 0.0273(4) Uani d 1 . .
H H23A -0.106868 0.567204 0.012491 0.033 Uiso calc 1 . .
H H23B -0.089479 0.630630 0.068675 0.033 Uiso calc 1 . .
C C24 0.06045(14) 0.58532(8) 0.08384(12) 0.0232(3) Uani d 1 . .
H H24A 0.076785 0.604027 0.019878 0.028 Uiso calc 1 . .
H H24B 0.083535 0.543480 0.085098 0.028 Uiso calc 1 . .
C C25 0.12775(12) 0.61616(7) 0.18448(12) 0.0188(3) Uani d 1 . .
H H25A 0.109634 0.658734 0.180255 0.023 Uiso calc 1 . .
H H25B 0.209217 0.611798 0.189237 0.023 Uiso calc 1 . .
C C26 0.15551(12) 0.68225(6) 0.39646(12) 0.0155(3) Uani d 1 . .
H H26 0.099398 0.696644 0.331400 0.019 Uiso calc 1 . .
C C27 0.10861(13) 0.69733(7) 0.49275(12) 0.0198(3) Uani d 1 . .
H H27A 0.037198 0.675821 0.487607 0.024 Uiso calc 1 . .
H H27B 0.162771 0.684987 0.559541 0.024 Uiso calc 1 . .
C C28 0.08784(14) 0.76347(7) 0.49579(14) 0.0235(3) Uani d 1 . .
H H28A 0.028444 0.774989 0.432041 0.028 Uiso calc 1 . .
H H28B 0.060970 0.773161 0.560235 0.028 Uiso calc 1 . .
C C29 0.19481(14) 0.79815(7) 0.49779(14) 0.0258(3) Uani d 1 . .
H H29A 0.251074 0.790334 0.565857 0.031 Uiso calc 1 . .
H H29B 0.177627 0.840825 0.494357 0.031 Uiso calc 1 . .
C C30 0.24396(14) 0.78122(7) 0.40405(14) 0.0236(3) Uani d 1 . .
H H30A 0.315816 0.802469 0.410204 0.028 Uiso calc 1 . .
H H30B 0.191359 0.793486 0.336272 0.028 Uiso calc 1 . .
C C31 0.26484(12) 0.71506(7) 0.40078(12) 0.0190(3) Uani d 1 . .
H H31A 0.292722 0.705234 0.336957 0.023 Uiso calc 1 . .
H H31B 0.322722 0.703020 0.465293 0.023 Uiso calc 1 . .
C C1S 0.68908(19) 0.74647(9) 0.54411(18) 0.0396(5) Uani d 1 . .
H H1S 0.696225 0.738475 0.617844 0.048 Uiso calc 1 . .
C C2S 0.78338(18) 0.74472(10) 0.5024(2) 0.0445(5) Uani d 1 . .
H H2S 0.855070 0.735644 0.547561 0.053 Uiso calc 1 . .
C C3S 0.77266(19) 0.75618(10) 0.3953(2) 0.0430(5) Uani d 1 . .
H H3S 0.836697 0.754721 0.366155 0.052 Uiso calc 1 . .
C C4S 0.6681(2) 0.76980(9) 0.33078(18) 0.0414(5) Uani d 1 . .
H H4S 0.660378 0.777832 0.256966 0.050 Uiso calc 1 . .
C C5S 0.57486(18) 0.77183(9) 0.37275(18) 0.0390(5) Uani d 1 . .
H H5S 0.503360 0.781612 0.327955 0.047 Uiso calc 1 . .
C C6S 0.58513(17) 0.75981(8) 0.47859(18) 0.0367(4) Uani d 1 . .
H H6S 0.520582 0.760638 0.507068 0.044 Uiso calc 1 . .
H H1 0.3710(18) 0.6567(11) 0.6337(18) 0.035(6) Uiso d 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
Cl1 0.0369(2) 0.0277(2) 0.0232(2) -0.01656(17) -0.00559(16) -0.00049(16)
N1 0.0371(8) 0.0193(7) 0.0193(7) -0.0048(6) -0.0128(6) 0.0002(6)
N2 0.0270(7) 0.0164(6) 0.0174(6) 0.0060(5) -0.0013(5) -0.0020(5)
N3 0.0169(6) 0.0138(6) 0.0123(6) 0.0014(5) -0.0021(5) -0.0010(5)
C1 0.0179(7) 0.0185(7) 0.0166(7) 0.0012(6) -0.0017(6) 0.0013(6)
C2 0.0153(6) 0.0185(7) 0.0129(6) 0.0028(5) 0.0003(5) -0.0009(5)
C3 0.0142(6) 0.0168(7) 0.0138(7) -0.0005(5) 0.0017(5) -0.0023(5)
C4 0.0286(8) 0.0260(8) 0.0159(7) -0.0020(7) -0.0081(6) 0.0003(6)
C5 0.0251(8) 0.0343(10) 0.0262(9) 0.0035(7) -0.0007(7) -0.0116(7)
C6 0.0414(11) 0.0616(14) 0.0217(9) -0.0093(10) 0.0068(8) -0.0050(9)
C7 0.044(4) 0.091(6) 0.026(3) -0.019(3) 0.012(2) -0.012(3)
C7A 0.047(7) 0.085(8) 0.029(5) -0.024(5) 0.016(5) -0.017(5)
C8 0.0245(8) 0.0200(7) 0.0167(7) 0.0071(6) -0.0023(6) -0.0010(6)
C9 0.0238(8) 0.0507(12) 0.0337(10) 0.0075(8) 0.0112(7) 0.0191(9)
C10 0.0218(8) 0.0586(13) 0.0395(11) 0.0113(8) 0.0063(8) 0.0230(10)
C11 0.0353(9) 0.0249(9) 0.0254(9) 0.0039(7) -0.0033(7) 0.0046(7)
C12 0.0296(9) 0.0728(16) 0.0298(10) 0.0027(10) 0.0060(8) 0.0271(10)
C13 0.0189(8) 0.102(2) 0.0284(10) -0.0030(10) 0.0027(7) 0.0339(12)
C14 0.0334(8) 0.0158(7) 0.0166(7) -0.0001(6) 0.0011(6) -0.0021(6)
C15 0.0323(9) 0.0330(9) 0.0198(8) -0.0072(7) 0.0003(7) 0.0049(7)
C16 0.0522(12) 0.0348(10) 0.0292(10) -0.0185(9) -0.0096(9) 0.0069(8)
C17 0.0635(13) 0.0220(9) 0.0205(8) -0.0053(9) -0.0096(8) -0.0035(7)
C18 0.0667(14) 0.0304(10) 0.0201(8) 0.0127(9) 0.0030(9) -0.0075(7)
C19 0.0349(9) 0.0287(9) 0.0205(8) 0.0107(7) 0.0063(7) -0.0022(7)
C20 0.0157(6) 0.0151(7) 0.0127(6) 0.0023(5) -0.0013(5) -0.0021(5)
C21 0.0162(7) 0.0268(8) 0.0178(7) -0.0023(6) 0.0007(6) -0.0062(6)
C22 0.0175(7) 0.0349(9) 0.0251(8) -0.0024(7) -0.0015(6) -0.0099(7)
C23 0.0243(8) 0.0332(9) 0.0182(8) 0.0062(7) -0.0069(6) -0.0058(7)
C24 0.0270(8) 0.0277(8) 0.0129(7) 0.0058(7) 0.0010(6) -0.0021(6)
C25 0.0172(7) 0.0231(8) 0.0151(7) 0.0043(6) 0.0019(6) 0.0003(6)
C26 0.0170(6) 0.0125(7) 0.0152(7) 0.0013(5) 0.0005(5) -0.0006(5)
C27 0.0213(7) 0.0195(7) 0.0185(7) -0.0010(6) 0.0046(6) -0.0036(6)
C28 0.0232(8) 0.0216(8) 0.0248(8) 0.0012(6) 0.0042(6) -0.0067(6)
C29 0.0271(8) 0.0170(7) 0.0295(9) -0.0017(6) -0.0001(7) -0.0053(6)
C30 0.0243(8) 0.0164(7) 0.0281(8) -0.0035(6) 0.0024(6) 0.0031(6)
C31 0.0188(7) 0.0183(7) 0.0191(7) -0.0014(6) 0.0032(6) 0.0014(6)
C1S 0.0548(12) 0.0281(10) 0.0371(11) -0.0012(9) 0.0135(9) 0.0017(8)
C2S 0.0348(10) 0.0405(12) 0.0554(14) 0.0020(9) 0.0056(10) 0.0035(10)
C3S 0.0394(11) 0.0378(11) 0.0574(14) -0.0094(9) 0.0229(10) -0.0042(10)
C4S 0.0584(13) 0.0277(10) 0.0389(11) -0.0127(9) 0.0137(10) -0.0011(8)
C5S 0.0381(10) 0.0241(9) 0.0500(12) -0.0007(8) 0.0010(9) -0.0026(9)
C6S 0.0341(10) 0.0261(9) 0.0532(13) -0.0018(7) 0.0171(9) -0.0077(8)
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 N1 C4 . . 124.75(15) ?
C1 N1 H1 . . 119.5(16) ?
C4 N1 H1 . . 115.5(16) ?
C2 N2 C8 . . 117.30(13) ?
C2 N2 C14 . . 122.26(13) ?
C14 N2 C8 . . 119.49(13) ?
C3 N3 C20 . . 122.13(12) ?
C3 N3 C26 . . 119.14(12) ?
C20 N3 C26 . . 118.54(11) ?
N1 C1 C2 . . 151.11(15) ?
N1 C1 C3 . . 148.47(15) ?
C2 C1 C3 . . 60.37(11) ?
N2 C2 C1 . . 146.06(14) ?
N2 C2 C3 . . 153.88(14) ?
C1 C2 C3 . . 60.04(11) ?
N3 C3 C1 . . 146.57(14) ?
N3 C3 C2 . . 153.84(14) ?
C1 C3 C2 . . 59.59(11) ?
N1 C4 H4A . . 109.3 ?
N1 C4 H4B . . 109.3 ?
N1 C4 C5 . . 111.76(15) ?
H4A C4 H4B . . 107.9 ?
C5 C4 H4A . . 109.3 ?
C5 C4 H4B . . 109.3 ?
C4 C5 H5A . . 109.0 ?
C4 C5 H5B . . 109.0 ?
H5A C5 H5B . . 107.8 ?
C6 C5 C4 . . 112.84(15) ?
C6 C5 H5A . . 109.0 ?
C6 C5 H5B . . 109.0 ?
C5 C6 H6AA . . 108.3 ?
C5 C6 H6AB . . 108.3 ?
C5 C6 H6BC . . 111.6 ?
C5 C6 H6BD . . 111.6 ?
C5 C6 C7A . . 100.6(11) ?
H6AA C6 H6AB . . 107.4 ?
H6BC C6 H6BD . . 109.4 ?
C7 C6 C5 . . 116.1(5) ?
C7 C6 H6AA . . 108.3 ?
C7 C6 H6AB . . 108.3 ?
C7A C6 H6BC . . 111.6 ?
C7A C6 H6BD . . 111.6 ?
C6 C7 H7A . . 109.5 ?
C6 C7 H7B . . 109.5 ?
C6 C7 H7C . . 109.5 ?
H7A C7 H7B . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C6 C7A H7AA . . 109.5 ?
C6 C7A H7AB . . 109.5 ?
C6 C7A H7AC . . 109.5 ?
H7AA C7A H7AB . . 109.5 ?
H7AA C7A H7AC . . 109.5 ?
H7AB C7A H7AC . . 109.5 ?
N2 C8 H8 . . 106.6 ?
N2 C8 C9 . . 113.20(14) ?
N2 C8 C13 . . 112.58(14) ?
C9 C8 H8 . . 106.6 ?
C13 C8 H8 . . 106.6 ?
C13 C8 C9 . . 110.67(16) ?
C8 C9 H9A . . 109.7 ?
C8 C9 H9B . . 109.7 ?
C8 C9 C10 . . 109.82(15) ?
H9A C9 H9B . . 108.2 ?
C10 C9 H9A . . 109.7 ?
C10 C9 H9B . . 109.7 ?
C9 C10 H10A . . 109.2 ?
C9 C10 H10B . . 109.2 ?
H10A C10 H10B . . 107.9 ?
C11 C10 C9 . . 111.95(16) ?
C11 C10 H10A . . 109.2 ?
C11 C10 H10B . . 109.2 ?
C10 C11 H11A . . 109.2 ?
C10 C11 H11B . . 109.2 ?
C10 C11 C12 . . 112.11(16) ?
H11A C11 H11B . . 107.9 ?
C12 C11 H11A . . 109.2 ?
C12 C11 H11B . . 109.2 ?
C11 C12 H12A . . 109.3 ?
C11 C12 H12B . . 109.3 ?
C11 C12 C13 . . 111.82(17) ?
H12A C12 H12B . . 107.9 ?
C13 C12 H12A . . 109.3 ?
C13 C12 H12B . . 109.3 ?
C8 C13 C12 . . 110.27(17) ?
C8 C13 H13A . . 109.6 ?
C8 C13 H13B . . 109.6 ?
C12 C13 H13A . . 109.6 ?
C12 C13 H13B . . 109.6 ?
H13A C13 H13B . . 108.1 ?
N2 C14 H14 . . 106.5 ?
N2 C14 C15 . . 111.86(14) ?
N2 C14 C19 . . 111.73(14) ?
C15 C14 H14 . . 106.5 ?
C15 C14 C19 . . 113.31(14) ?
C19 C14 H14 . . 106.5 ?
C14 C15 H15A . . 109.5 ?
C14 C15 H15B . . 109.5 ?
C14 C15 C16 . . 110.85(17) ?
H15A C15 H15B . . 108.1 ?
C16 C15 H15A . . 109.5 ?
C16 C15 H15B . . 109.5 ?
C15 C16 H16A . . 109.3 ?
C15 C16 H16B . . 109.3 ?
H16A C16 H16B . . 108.0 ?
C17 C16 C15 . . 111.41(16) ?
C17 C16 H16A . . 109.3 ?
C17 C16 H16B . . 109.3 ?
C16 C17 H17A . . 109.3 ?
C16 C17 H17B . . 109.3 ?
H17A C17 H17B . . 107.9 ?
C18 C17 C16 . . 111.77(16) ?
C18 C17 H17A . . 109.3 ?
C18 C17 H17B . . 109.3 ?
C17 C18 H18A . . 109.4 ?
C17 C18 H18B . . 109.4 ?
C17 C18 C19 . . 111.36(16) ?
H18A C18 H18B . . 108.0 ?
C19 C18 H18A . . 109.4 ?
C19 C18 H18B . . 109.4 ?
C14 C19 H19A . . 109.4 ?
C14 C19 H19B . . 109.4 ?
C18 C19 C14 . . 111.05(16) ?
C18 C19 H19A . . 109.4 ?
C18 C19 H19B . . 109.4 ?
H19A C19 H19B . . 108.0 ?
N3 C20 H20 . . 107.4 ?
N3 C20 C21 . . 111.47(12) ?
N3 C20 C25 . . 111.67(12) ?
C21 C20 H20 . . 107.4 ?
C25 C20 H20 . . 107.4 ?
C25 C20 C21 . . 111.18(12) ?
C20 C21 H21A . . 109.5 ?
C20 C21 H21B . . 109.5 ?
C20 C21 C22 . . 110.73(13) ?
H21A C21 H21B . . 108.1 ?
C22 C21 H21A . . 109.5 ?
C22 C21 H21B . . 109.5 ?
C21 C22 H22A . . 109.4 ?
C21 C22 H22B . . 109.4 ?
H22A C22 H22B . . 108.0 ?
C23 C22 C21 . . 111.21(14) ?
C23 C22 H22A . . 109.4 ?
C23 C22 H22B . . 109.4 ?
C22 C23 H23A . . 109.4 ?
C22 C23 H23B . . 109.4 ?
H23A C23 H23B . . 108.0 ?
C24 C23 C22 . . 111.10(13) ?
C24 C23 H23A . . 109.4 ?
C24 C23 H23B . . 109.4 ?
C23 C24 H24A . . 109.5 ?
C23 C24 H24B . . 109.5 ?
C23 C24 C25 . . 110.84(13) ?
H24A C24 H24B . . 108.1 ?
C25 C24 H24A . . 109.5 ?
C25 C24 H24B . . 109.5 ?
C20 C25 H25A . . 109.5 ?
C20 C25 H25B . . 109.5 ?
C24 C25 C20 . . 110.73(13) ?
C24 C25 H25A . . 109.5 ?
C24 C25 H25B . . 109.5 ?
H25A C25 H25B . . 108.1 ?
N3 C26 H26 . . 106.8 ?
N3 C26 C27 . . 112.48(12) ?
N3 C26 C31 . . 112.18(12) ?
C27 C26 H26 . . 106.8 ?
C31 C26 H26 . . 106.8 ?
C31 C26 C27 . . 111.30(12) ?
C26 C27 H27A . . 109.7 ?
C26 C27 H27B . . 109.7 ?
H27A C27 H27B . . 108.2 ?
C28 C27 C26 . . 109.86(13) ?
C28 C27 H27A . . 109.7 ?
C28 C27 H27B . . 109.7 ?
C27 C28 H28A . . 109.4 ?
C27 C28 H28B . . 109.4 ?
H28A C28 H28B . . 108.0 ?
C29 C28 C27 . . 111.15(13) ?
C29 C28 H28A . . 109.4 ?
C29 C28 H28B . . 109.4 ?
C28 C29 H29A . . 109.4 ?
C28 C29 H29B . . 109.4 ?
C28 C29 C30 . . 111.18(13) ?
H29A C29 H29B . . 108.0 ?
C30 C29 H29A . . 109.4 ?
C30 C29 H29B . . 109.4 ?
C29 C30 H30A . . 109.3 ?
C29 C30 H30B . . 109.3 ?
C29 C30 C31 . . 111.80(13) ?
H30A C30 H30B . . 107.9 ?
C31 C30 H30A . . 109.3 ?
C31 C30 H30B . . 109.3 ?
C26 C31 C30 . . 109.30(12) ?
C26 C31 H31A . . 109.8 ?
C26 C31 H31B . . 109.8 ?
C30 C31 H31A . . 109.8 ?
C30 C31 H31B . . 109.8 ?
H31A C31 H31B . . 108.3 ?
C2S C1S H1S . . 120.0 ?
C6S C1S H1S . . 120.0 ?
C6S C1S C2S . . 120.1(2) ?
C1S C2S H2S . . 120.1 ?
C3S C2S C1S . . 119.8(2) ?
C3S C2S H2S . . 120.1 ?
C2S C3S H3S . . 120.3 ?
C2S C3S C4S . . 119.5(2) ?
C4S C3S H3S . . 120.3 ?
C3S C4S H4S . . 119.8 ?
C5S C4S C3S . . 120.4(2) ?
C5S C4S H4S . . 119.8 ?
C4S C5S H5S . . 119.9 ?
C6S C5S C4S . . 120.1(2) ?
C6S C5S H5S . . 119.9 ?
C1S C6S H6S . . 120.0 ?
C5S C6S C1S . . 120.05(19) ?
C5S C6S H6S . . 120.0 ?
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
N1 C1 . 1.319(2) ?
N1 C4 . 1.453(2) ?
N1 H1 . 0.84(2) ?
N2 C2 . 1.331(2) ?
N2 C8 . 1.4872(19) ?
N2 C14 . 1.461(2) ?
N3 C3 . 1.3247(19) ?
N3 C20 . 1.4752(18) ?
N3 C26 . 1.4789(19) ?
C1 C2 . 1.377(2) ?
C1 C3 . 1.383(2) ?
C2 C3 . 1.388(2) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C4 C5 . 1.526(3) ?
C5 H5A . 0.9900 ?
C5 H5B . 0.9900 ?
C5 C6 . 1.510(3) ?
C6 H6AA . 0.9900 ?
C6 H6AB . 0.9900 ?
C6 H6BC . 0.9900 ?
C6 H6BD . 0.9900 ?
C6 C7 . 1.502(9) ?
C6 C7A . 1.60(2) ?
C7 H7A . 0.9800 ?
C7 H7B . 0.9800 ?
C7 H7C . 0.9800 ?
C7A H7AA . 0.9800 ?
C7A H7AB . 0.9800 ?
C7A H7AC . 0.9800 ?
C8 H8 . 1.0000 ?
C8 C9 . 1.502(2) ?
C8 C13 . 1.499(3) ?
C9 H9A . 0.9900 ?
C9 H9B . 0.9900 ?
C9 C10 . 1.535(3) ?
C10 H10A . 0.9900 ?
C10 H10B . 0.9900 ?
C10 C11 . 1.499(3) ?
C11 H11A . 0.9900 ?
C11 H11B . 0.9900 ?
C11 C12 . 1.501(3) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C12 C13 . 1.523(3) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 H14 . 1.0000 ?
C14 C15 . 1.518(2) ?
C14 C19 . 1.526(2) ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C15 C16 . 1.535(3) ?
C16 H16A . 0.9900 ?
C16 H16B . 0.9900 ?
C16 C17 . 1.526(3) ?
C17 H17A . 0.9900 ?
C17 H17B . 0.9900 ?
C17 C18 . 1.507(3) ?
C18 H18A . 0.9900 ?
C18 H18B . 0.9900 ?
C18 C19 . 1.519(3) ?
C19 H19A . 0.9900 ?
C19 H19B . 0.9900 ?
C20 H20 . 1.0000 ?
C20 C21 . 1.528(2) ?
C20 C25 . 1.527(2) ?
C21 H21A . 0.9900 ?
C21 H21B . 0.9900 ?
C21 C22 . 1.531(2) ?
C22 H22A . 0.9900 ?
C22 H22B . 0.9900 ?
C22 C23 . 1.523(3) ?
C23 H23A . 0.9900 ?
C23 H23B . 0.9900 ?
C23 C24 . 1.521(2) ?
C24 H24A . 0.9900 ?
C24 H24B . 0.9900 ?
C24 C25 . 1.526(2) ?
C25 H25A . 0.9900 ?
C25 H25B . 0.9900 ?
C26 H26 . 1.0000 ?
C26 C27 . 1.528(2) ?
C26 C31 . 1.522(2) ?
C27 H27A . 0.9900 ?
C27 H27B . 0.9900 ?
C27 C28 . 1.525(2) ?
C28 H28A . 0.9900 ?
C28 H28B . 0.9900 ?
C28 C29 . 1.524(2) ?
C29 H29A . 0.9900 ?
C29 H29B . 0.9900 ?
C29 C30 . 1.525(2) ?
C30 H30A . 0.9900 ?
C30 H30B . 0.9900 ?
C30 C31 . 1.526(2) ?
C31 H31A . 0.9900 ?
C31 H31B . 0.9900 ?
C1S H1S . 0.9500 ?
C1S C2S . 1.389(3) ?
C1S C6S . 1.379(3) ?
C2S H2S . 0.9500 ?
C2S C3S . 1.378(4) ?
C3S H3S . 0.9500 ?
C3S C4S . 1.381(3) ?
C4S H4S . 0.9500 ?
C4S C5S . 1.379(3) ?
C5S H5S . 0.9500 ?
C5S C6S . 1.366(3) ?
C6S H6S . 0.9500 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C1 C2 N2 . . . . 4.0(5) ?
N1 C1 C2 C3 . . . . -177.3(3) ?
N1 C1 C3 N3 . . . . -2.2(5) ?
N1 C1 C3 C2 . . . . 177.5(3) ?
N1 C4 C5 C6 . . . . -175.67(16) ?
N2 C2 C3 N3 . . . . -2.0(6) ?
N2 C2 C3 C1 . . . . 178.3(4) ?
N2 C8 C9 C10 . . . . 173.80(16) ?
N2 C8 C13 C12 . . . . -172.96(18) ?
N2 C14 C15 C16 . . . . 179.90(14) ?
N2 C14 C19 C18 . . . . 179.06(14) ?
N3 C20 C21 C22 . . . . -179.07(13) ?
N3 C20 C25 C24 . . . . 178.39(12) ?
N3 C26 C27 C28 . . . . -174.43(12) ?
N3 C26 C31 C30 . . . . 174.66(12) ?
C1 N1 C4 C5 . . . . -73.7(2) ?
C1 C2 C3 N3 . . . . 179.7(3) ?
C2 N2 C8 C9 . . . . -100.70(18) ?
C2 N2 C8 C13 . . . . 132.84(18) ?
C2 N2 C14 C15 . . . . -67.2(2) ?
C2 N2 C14 C19 . . . . 61.1(2) ?
C2 C1 C3 N3 . . . . -179.8(3) ?
C3 N3 C20 C21 . . . . 109.43(15) ?
C3 N3 C20 C25 . . . . -125.54(14) ?
C3 N3 C26 C27 . . . . -57.58(17) ?
C3 N3 C26 C31 . . . . 68.81(17) ?
C3 C1 C2 N2 . . . . -178.7(3) ?
C4 N1 C1 C2 . . . . -15.3(4) ?
C4 N1 C1 C3 . . . . 169.1(2) ?
C4 C5 C6 C7 . . . . -177.2(6) ?
C4 C5 C6 C7A . . . . 170.9(10) ?
C8 N2 C2 C1 . . . . -4.6(3) ?
C8 N2 C2 C3 . . . . 178.0(3) ?
C8 N2 C14 C15 . . . . 124.29(15) ?
C8 N2 C14 C19 . . . . -107.48(16) ?
C8 C9 C10 C11 . . . . 55.2(2) ?
C9 C8 C13 C12 . . . . 59.2(3) ?
C9 C10 C11 C12 . . . . -52.4(3) ?
C10 C11 C12 C13 . . . . 52.5(3) ?
C11 C12 C13 C8 . . . . -55.7(3) ?
C13 C8 C9 C10 . . . . -58.7(2) ?
C14 N2 C2 C1 . . . . -173.4(2) ?
C14 N2 C2 C3 . . . . 9.2(4) ?
C14 N2 C8 C9 . . . . 68.4(2) ?
C14 N2 C8 C13 . . . . -58.1(2) ?
C14 C15 C16 C17 . . . . -52.9(2) ?
C15 C14 C19 C18 . . . . -53.5(2) ?
C15 C16 C17 C18 . . . . 55.6(2) ?
C16 C17 C18 C19 . . . . -56.5(2) ?
C17 C18 C19 C14 . . . . 54.6(2) ?
C19 C14 C15 C16 . . . . 52.51(19) ?
C20 N3 C3 C1 . . . . 175.9(2) ?
C20 N3 C3 C2 . . . . -3.7(4) ?
C20 N3 C26 C27 . . . . 117.46(14) ?
C20 N3 C26 C31 . . . . -116.15(14) ?
C20 C21 C22 C23 . . . . -55.36(18) ?
C21 C20 C25 C24 . . . . -56.42(16) ?
C21 C22 C23 C24 . . . . 56.07(19) ?
C22 C23 C24 C25 . . . . -56.65(19) ?
C23 C24 C25 C20 . . . . 56.72(17) ?
C25 C20 C21 C22 . . . . 55.63(18) ?
C26 N3 C3 C1 . . . . -9.3(3) ?
C26 N3 C3 C2 . . . . 171.2(3) ?
C26 N3 C20 C21 . . . . -65.46(17) ?
C26 N3 C20 C25 . . . . 59.57(16) ?
C26 C27 C28 C29 . . . . -56.36(17) ?
C27 C26 C31 C30 . . . . -58.31(16) ?
C27 C28 C29 C30 . . . . 54.94(18) ?
C28 C29 C30 C31 . . . . -55.23(18) ?
C29 C30 C31 C26 . . . . 56.37(17) ?
C31 C26 C27 C28 . . . . 58.71(16) ?
C1S C2S C3S C4S . . . . 0.5(3) ?
C2S C1S C6S C5S . . . . -0.6(3) ?
C2S C3S C4S C5S . . . . -0.2(3) ?
C3S C4S C5S C6S . . . . -0.6(3) ?
C4S C5S C6S C1S . . . . 1.0(3) ?
C6S C1S C2S C3S . . . . -0.2(3) ?
_cod_database_fobs_code 2244150