#------------------------------------------------------------------------------
#$Date: 2024-08-07 01:02:43 +0300 (Wed, 07 Aug 2024) $
#$Revision: 293981 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312523.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_2312523
loop_
_publ_author_name
'Erickson, Alexander N.'
'Haltiwanger, Curtis'
'Rahim, Masoumeh'
'Garner, Charles M.'
_publ_section_title
;
Preferential crystallization of (±)-pinenyllithium·TMEDA.
;
_journal_coeditor_code OJ3017
_journal_issue 'Pt 7'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first 297
_journal_page_last 301
_journal_paper_doi 10.1107/S2053229624004662
_journal_volume 80
_journal_year 2024
_chemical_formula_iupac '[Li (C10 H15) (C6 H16 N2)]'
_chemical_formula_moiety 'C16 H31 Li N2'
_chemical_formula_sum 'C16 H31 Li N2'
_chemical_formula_weight 258.37
_chemical_name_common
;
(+-)-Pinenyllithium tetramethylethylenediamine
;
_chemical_name_systematic
;
(Tetramethylethylenediamine-\k^2^N,N')(\h^3^-2,6,6-\
trimethylbicyclo[3.1.1]heptyl)lithium
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens difmap
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 97.3360(10)
_cell_angle_beta 99.662(2)
_cell_angle_gamma 93.520(2)
_cell_formula_units_Z 2
_cell_length_a 6.3160(2)
_cell_length_b 9.6925(2)
_cell_length_c 13.7463(2)
_cell_measurement_reflns_used 17767
_cell_measurement_temperature 120(2)
_cell_measurement_theta_max 77.8490
_cell_measurement_theta_min 3.2670
_cell_volume 819.83(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
ShelXle (H\"ubschle et al., 2011)
;
_computing_publication_material
;
CIFTAB2014 (Sheldrick, 2008) and
FinalCif (D. Kratzert, https://dkratzert.de/finalcif.html)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 120(2)
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-S single source'
_diffrn_measurement_method 'combination of \w and \f-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0560
_diffrn_reflns_av_unetI/netI 0.0247
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_number 20391
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 77.923
_diffrn_reflns_theta_min 3.294
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.442
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.675
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2021)
;
_exptl_crystal_colour 'Translucent Pale Yellow'
_exptl_crystal_density_diffrn 1.047
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_description Plate
_exptl_crystal_F_000 288
_exptl_crystal_size_max 0.349
_exptl_crystal_size_mid 0.108
_exptl_crystal_size_min 0.044
_refine_diff_density_max 0.282
_refine_diff_density_min -0.218
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.089
_refine_ls_hydrogen_treatment refall
_refine_ls_matrix_type full
_refine_ls_number_parameters 296
_refine_ls_number_reflns 3373
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.089
_refine_ls_R_factor_all 0.0402
_refine_ls_R_factor_gt 0.0387
_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^)+(0.0589P)^2^+0.1668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1062
_refine_ls_wR_factor_ref 0.1075
_reflns_number_gt 3167
_reflns_number_total 3373
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file oj3017sup1.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2312523.cif.'
_cod_database_code 2312523
_cod_database_fobs_code 2312523
_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 0.861
_shelx_estimated_absorpt_t_max 0.983
_shelx_hkl_file
;
0 0 -1 17.86 0.93
0 0 -1 17.46 1.03
0 0 1 20.21 1.11
0 0 1 20.20 1.20
0 0 1 20.72 1.18
0 0 -1 17.44 1.01
0 0 1 21.64 1.24
0 0 -2 4445.21 166.65
0 0 -2 4751.22 166.98
0 0 2 4775.93 167.11
0 0 2 4913.71 167.32
0 0 2 4752.44 167.40
0 0 -2 4271.86 166.87
0 0 2 4336.61 167.30
0 0 -3 1834.94 71.09
0 0 -3 2021.68 71.58
0 0 3 1973.46 71.81
0 0 -3 1878.91 71.07
0 0 3 2128.91 72.40
0 0 3 2027.11 72.16
0 0 -3 1887.06 71.46
0 0 -4 217.47 9.41
0 0 -4 236.57 9.93
0 0 4 246.03 10.35
0 0 -4 204.74 9.30
0 0 4 254.39 11.01
0 0 4 244.56 10.69
0 0 -4 219.30 9.75
0 0 -4 252.47 10.02
0 0 -5 2103.36 69.61
0 0 -5 1678.98 68.66
0 0 5 1829.30 69.91
0 0 -5 1781.33 68.72
0 0 5 1951.56 70.94
0 0 5 1981.62 70.72
0 0 -5 1852.93 69.39
0 0 -5 1860.09 69.18
0 0 -6 9.50 1.54
0 0 -6 6.85 1.14
0 0 -6 6.33 1.10
0 0 6 7.99 1.68
0 0 6 7.08 1.83
0 0 6 7.49 1.94
0 0 -6 7.71 1.35
0 0 -6 8.08 1.44
0 0 -7 217.08 10.45
0 0 -7 212.29 10.30
0 0 7 231.67 11.90
0 0 7 238.87 12.61
0 0 7 241.67 13.03
0 0 -7 224.50 11.01
0 0 -7 269.58 11.58
0 0 -7 222.09 10.75
0 0 -8 0.46 0.74
0 0 8 1.24 1.47
0 0 8 -0.35 1.64
0 0 -8 1.02 0.77
0 0 8 1.28 1.14
0 0 -8 0.19 0.81
0 0 -8 1.17 0.93
0 0 8 0.61 1.54
0 0 -9 73.11 5.10
0 0 9 72.18 6.37
0 0 -9 62.27 3.76
0 0 -9 91.93 5.90
0 0 -9 75.33 5.59
0 0 9 83.63 7.90
0 0 9 81.51 7.14
0 0 9 75.20 7.32
0 0 9 73.63 6.84
0 0 -9 75.08 3.50
0 0 10 39.73 2.84
0 0 10 28.46 4.95
0 0 10 38.74 5.18
0 0 10 37.24 4.59
0 0 -10 29.78 3.28
0 0 -10 31.66 1.78
0 0 -10 30.35 1.99
0 0 10 36.97 5.52
0 0 10 31.47 4.76
0 0 -10 32.38 3.62
0 0 -10 35.53 3.79
0 0 11 91.84 9.08
0 0 11 79.53 8.17
0 0 11 104.77 5.45
0 0 -11 86.69 6.51
0 0 11 89.30 8.62
0 0 11 83.42 8.97
0 0 -11 103.98 7.11
0 0 -11 88.68 3.98
0 0 -11 88.80 4.34
0 0 -11 84.08 4.18
0 0 12 190.02 14.30
0 0 12 184.07 7.94
0 0 12 213.09 9.49
0 0 12 173.73 13.10
0 0 12 173.38 13.23
0 0 12 172.57 14.10
0 0 -12 187.68 7.71
0 0 -12 192.14 7.99
0 0 -12 193.25 8.14
0 0 13 57.30 3.12
0 0 13 74.52 4.54
0 0 13 69.03 8.12
0 0 13 43.78 6.12
0 0 -13 64.46 3.04
0 0 -13 61.18 3.20
0 0 -13 66.99 3.48
0 0 13 43.45 6.71
0 0 14 94.68 5.55
0 0 -14 91.36 4.20
0 0 -14 93.94 4.43
0 0 -14 85.93 3.97
0 0 15 2.78 1.16
0 0 15 0.94 0.55
0 0 -15 0.99 0.57
0 0 -15 0.85 0.45
0 0 -15 1.22 0.42
0 0 -16 -0.08 0.31
0 0 -16 -0.04 0.38
0 0 -16 0.07 0.26
0 1 -17 16.79 0.84
0 -1 16 2.34 0.54
0 1 -16 2.59 0.58
0 1 -16 3.16 0.50
0 1 -16 3.09 0.43
0 -1 15 84.55 4.90
0 1 -15 74.53 3.68
0 1 -15 73.78 3.46
0 1 -15 77.14 3.33
0 -1 14 151.61 7.68
0 1 -14 138.73 5.81
0 1 -14 132.69 5.99
0 1 -14 140.01 6.23
0 -1 13 121.28 6.70
0 -1 13 115.02 10.12
0 -1 13 82.08 8.63
0 -1 13 84.10 9.63
0 1 -13 113.61 4.94
0 1 -13 115.63 5.17
0 1 -13 115.19 5.35
0 -1 12 35.56 5.54
0 -1 12 34.39 3.03
0 -1 12 32.49 4.75
0 -1 12 29.08 5.47
0 -1 12 28.17 4.80
0 1 -12 31.35 1.90
0 1 -12 34.18 2.12
0 1 -12 32.47 2.18
0 -1 11 212.76 14.03
0 -1 11 220.20 9.46
0 1 -11 193.68 10.76
0 -1 11 171.00 12.19
0 -1 11 197.68 13.43
0 -1 11 198.69 14.50
0 1 -11 186.12 7.81
0 1 -11 195.27 8.08
0 1 -11 195.19 8.24
0 -1 10 -0.42 1.59
0 -1 10 1.07 0.81
0 -1 10 1.76 1.39
0 1 -10 0.68 0.52
0 1 -10 0.62 0.91
0 -1 10 0.82 1.28
0 -1 10 0.98 1.74
0 1 -10 0.63 0.79
0 1 -10 0.62 0.38
0 1 -10 1.06 0.50
0 1 -10 0.70 0.49
0 -1 9 27.32 4.54
0 1 -9 29.69 3.21
0 -1 9 33.66 4.55
0 -1 9 36.07 2.55
0 1 -9 32.76 1.93
0 1 -9 29.98 1.81
0 1 -9 33.83 3.21
0 -1 9 29.44 4.05
0 1 -8 33.98 3.02
0 -1 8 36.02 4.07
0 -1 8 37.91 4.67
0 1 -8 42.76 3.86
0 1 -8 33.73 3.26
0 -1 8 38.01 4.44
0 1 -7 18.49 2.35
0 -1 7 19.09 2.67
0 1 -7 14.52 1.78
0 1 -7 14.67 1.97
0 -1 7 16.28 2.94
0 -1 7 18.11 2.83
0 -1 6 468.44 19.66
0 1 -6 430.41 18.08
0 -1 6 453.41 19.96
0 1 -6 457.84 18.93
0 1 -5 54.43 2.86
0 -1 5 56.38 3.75
0 1 -5 62.86 3.61
0 -1 5 58.73 3.99
0 -1 4 636.40 22.58
0 1 -4 576.74 22.32
0 1 -4 600.54 23.21
0 1 -4 576.09 21.40
0 1 -4 552.95 21.39
0 1 -4 603.53 21.49
0 1 -4 595.89 21.43
0 -1 4 648.55 23.66
0 -1 3 887.95 32.24
0 1 -3 906.14 31.45
0 -1 3 946.76 33.05
0 1 -3 856.41 32.05
0 1 -2 322.06 12.12
0 -1 2 318.55 12.02
0 -1 2 332.07 12.65
0 -1 2 327.01 12.27
0 1 -2 282.76 12.32
0 -1 1 139.22 5.61
0 -1 1 155.95 5.75
0 1 -1 137.36 5.78
0 -1 1 146.86 5.86
0 1 0 598.71 22.30
0 -1 0 570.78 21.47
0 -1 0 564.63 21.62
0 -1 0 579.74 21.38
0 1 0 598.27 21.94
0 -1 -1 32.79 1.84
0 1 1 31.50 2.24
0 1 1 38.85 2.34
0 -1 -1 34.96 1.97
0 -1 -1 40.61 1.74
0 1 1 35.70 2.35
0 -1 -2 2841.63 111.59
0 1 2 3309.44 112.91
0 -1 -2 3180.97 111.58
0 1 2 2651.80 112.37
0 1 2 3247.67 112.66
0 1 2 3250.11 112.45
0 1 3 2570.14 84.28
0 1 3 2591.12 83.95
0 -1 -3 2440.62 82.47
0 1 3 2506.59 83.20
0 -1 -3 2168.74 82.40
0 1 3 2373.12 81.50
0 1 3 2258.59 81.54
0 1 3 1957.77 81.46
0 1 3 2591.83 84.02
0 1 3 2631.24 83.74
0 -1 -4 614.13 20.89
0 1 4 654.79 22.68
0 -1 -4 612.58 21.45
0 1 4 626.40 23.03
0 1 4 650.13 21.85
0 -1 -4 569.26 20.72
0 1 4 530.06 19.35
0 -1 -4 494.05 19.36
0 1 4 543.21 19.43
0 1 4 523.69 19.38
0 1 4 512.03 19.34
0 1 4 632.92 22.85
0 1 4 674.86 22.54
0 -1 -5 897.46 36.86
0 1 5 987.36 38.09
0 1 5 1029.10 39.27
0 1 5 1070.61 38.99
0 -1 -5 1006.32 37.17
0 -1 -5 966.96 37.61
0 1 5 979.05 38.84
0 1 5 879.37 38.94
0 -1 -6 331.05 14.51
0 1 6 357.38 15.85
0 1 6 338.88 16.41
0 1 6 366.71 17.13
0 -1 -6 326.08 15.20
0 1 6 337.28 16.41
0 -1 -6 357.47 14.75
0 -1 -7 348.50 15.03
0 -1 -7 313.11 13.21
0 1 7 368.93 16.57
0 1 7 384.47 17.60
0 1 7 384.93 18.18
0 -1 -7 342.20 15.73
0 1 7 391.78 17.88
0 -1 -7 404.38 15.56
0 -1 -8 489.46 20.38
0 -1 -8 478.55 21.13
0 1 8 482.63 23.18
0 1 8 530.54 23.37
0 1 8 501.89 23.84
0 -1 -8 446.70 18.12
0 1 9 60.57 6.71
0 1 9 62.29 6.35
0 -1 -9 81.97 5.47
0 -1 -9 68.81 5.39
0 1 9 74.98 7.04
0 -1 -9 62.41 4.83
0 -1 -9 58.70 2.80
0 -1 -9 62.41 3.13
0 1 10 725.60 33.49
0 -1 -10 704.96 29.60
0 -1 -10 737.87 29.43
0 1 10 693.74 32.69
0 -1 -10 626.05 28.49
0 1 10 621.94 31.98
0 -1 -10 702.49 29.00
0 -1 -10 665.26 25.40
0 -1 -10 698.37 25.85
0 -1 -11 92.90 6.92
0 1 11 85.33 8.72
0 1 11 95.74 9.60
0 1 11 103.02 9.63
0 1 11 83.40 8.43
0 -1 -11 88.43 3.97
0 -1 -11 89.82 4.38
0 1 12 2.54 2.33
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0 -1 -12 1.75 1.07
0 1 12 0.56 1.99
0 1 12 3.41 2.24
0 -1 -12 1.39 0.47
0 -1 -12 1.39 0.66
0 -1 -12 1.25 0.58
0 1 13 1.11 1.62
0 1 13 0.54 1.82
0 1 13 2.18 0.69
0 -1 -13 2.18 0.51
0 -1 -13 3.05 0.73
0 -1 -13 2.12 0.63
0 -1 -13 2.71 1.27
0 -1 -14 265.88 10.23
0 -1 -14 283.45 10.53
0 -1 -14 256.44 9.96
0 -1 -15 78.67 3.51
0 -1 -15 77.55 3.73
0 -1 -15 79.06 3.37
0 -1 -16 16.84 0.99
0 -1 -16 12.61 0.63
0 -2 16 6.56 0.84
0 2 -16 7.92 0.74
0 2 -16 7.66 0.83
0 -2 15 107.32 5.26
0 2 -15 112.83 4.94
0 2 -15 119.02 5.18
0 -2 14 29.50 2.30
0 -2 14 35.66 3.23
0 2 -14 34.53 2.24
0 2 -14 31.82 2.03
0 -2 13 1.66 1.56
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0 -2 13 -1.12 1.75
0 -2 13 0.46 1.14
0 2 -13 0.28 1.00
0 -2 13 0.57 1.65
0 2 -13 0.14 0.62
0 2 -13 -0.12 0.51
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0 -2 12 -0.51 1.36
0 -2 12 0.44 1.10
0 2 -12 -0.18 0.53
0 2 -12 0.14 0.58
0 -2 12 0.47 1.66
0 -2 12 0.58 1.81
0 2 -12 0.28 0.93
0 2 -11 0.26 0.97
0 -2 11 -1.08 1.43
0 -2 11 -0.48 1.62
0 -2 11 -0.13 0.97
0 -2 11 -0.40 1.59
0 2 -11 0.72 0.64
0 2 -11 0.63 0.42
0 2 -11 0.46 0.36
0 2 -11 0.77 0.48
0 2 -11 0.77 0.61
0 -2 10 2.20 1.79
0 2 -10 0.96 0.68
0 2 -10 1.39 1.07
0 2 -10 2.58 1.00
0 -2 10 1.44 1.71
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0 -2 10 0.43 1.53
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0 2 -10 1.91 0.56
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0 2 -9 318.53 14.79
0 2 -9 319.86 15.98
0 -2 9 338.37 18.49
0 -2 9 355.39 13.75
0 -2 9 311.77 17.74
0 2 -9 306.23 12.52
0 2 -9 328.86 12.70
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0 2 -8 0.19 0.86
0 -2 8 -0.34 1.38
0 2 -8 1.39 0.86
0 2 -8 1.19 0.85
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0 -2 7 0.22 1.12
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0 2 -6 0.28 0.85
0 -2 6 0.45 0.64
0 -2 6 0.20 1.06
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0 2 -6 0.15 0.19
0 2 -6 0.09 0.20
0 2 -6 -0.10 0.66
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0 -2 5 641.98 23.71
0 -2 5 685.70 25.49
0 -2 5 668.02 25.07
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0 2 -5 584.20 22.25
0 2 -5 643.71 22.24
0 2 -5 559.71 22.36
0 -2 4 1007.26 37.60
0 2 -4 909.31 37.72
0 2 -4 982.09 38.45
0 -2 4 1052.29 38.58
0 2 -4 1015.05 36.49
0 2 -4 964.55 36.78
0 2 -3 4359.92 156.66
0 -2 3 4057.44 155.37
0 -2 3 4427.29 155.41
0 2 -3 3938.64 155.83
0 -2 3 4549.50 155.90
0 2 -2 20.74 2.10
0 -2 2 24.60 1.55
0 -2 2 26.76 1.68
0 2 -2 22.30 1.79
0 -2 2 27.57 1.92
0 2 -1 6301.26 209.66
0 2 -1 6186.22 208.00
0 -2 1 5391.59 207.03
0 -2 1 5374.69 207.05
0 -2 1 5734.46 207.58
0 -2 1 5511.39 207.01
0 -2 1 6365.13 207.53
0 2 0 1505.35 51.59
0 -2 0 1364.93 49.49
0 -2 0 1456.68 50.06
0 2 1 4639.17 164.39
0 2 1 4348.04 162.43
0 -2 -1 4687.00 163.70
0 -2 -1 4854.22 163.54
0 2 2 3804.06 151.71
0 2 2 3995.08 152.25
0 -2 -2 4225.15 150.90
0 2 2 4379.46 152.15
0 2 3 801.26 31.62
0 -2 -3 748.07 30.07
0 -2 -3 855.15 29.49
0 2 3 783.72 31.49
0 2 3 838.17 31.43
0 2 3 718.18 28.90
0 2 3 791.96 28.71
0 -2 -3 743.42 29.64
0 2 4 1542.56 58.18
0 2 4 1536.97 58.09
0 -2 -4 1686.01 55.69
0 -2 -4 1491.69 55.78
0 2 4 1605.61 58.05
0 2 4 1479.91 54.55
0 2 4 1404.71 54.40
0 2 4 1490.10 54.43
0 2 5 43.04 4.38
0 2 5 38.81 4.12
0 -2 -5 35.38 3.13
0 -2 -5 37.75 2.71
0 2 5 35.57 3.83
0 -2 -5 33.38 2.69
0 2 5 38.11 4.00
0 2 5 36.24 1.67
0 2 5 35.62 1.66
0 2 5 37.53 1.76
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-4 -2 -3 74.76 3.05
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-4 -2 -4 409.04 15.26
-4 -2 -4 351.65 16.57
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4 3 -11 66.63 6.84
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4 4 -8 647.80 22.59
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-6 -2 1 52.45 2.70
-6 -2 1 53.37 2.77
-6 -2 1 58.21 2.84
-6 -2 1 58.51 2.93
-6 -2 1 45.63 4.17
-6 -2 1 52.96 2.83
-6 -2 1 61.89 2.90
-6 -2 0 27.77 1.76
-6 -2 0 26.41 1.78
-6 -2 0 30.85 1.72
-6 -2 0 29.32 1.77
-6 -2 0 31.68 1.89
-6 -2 0 28.14 1.78
-6 -2 0 31.77 1.83
-6 -2 -1 1.81 0.58
-6 -2 -1 2.48 0.56
-6 -2 -1 1.59 0.56
-6 -2 -1 2.41 0.60
-6 -2 -1 1.90 0.55
-6 -2 -1 1.69 0.53
-6 -2 -2 135.97 5.86
-6 -2 -2 127.57 5.79
-6 -2 -2 131.48 5.63
-6 -2 -2 141.97 5.69
-6 -2 -2 133.46 5.61
-6 -2 -2 151.91 5.72
-6 -2 -3 6.57 0.83
-6 -2 -3 6.97 0.82
-6 -2 -3 6.03 0.61
-6 -2 -3 6.37 0.65
-6 -2 -3 6.11 0.61
-6 -2 -3 5.58 0.61
-6 -2 -4 66.32 3.12
-6 -2 -5 90.16 3.91
-6 -2 -5 87.53 3.85
-6 -2 -6 13.10 0.93
-6 -2 -6 12.16 0.87
-6 -2 -7 137.77 5.26
-6 -2 -7 130.84 5.21
-6 -3 13 74.93 3.10
-6 -3 12 100.79 4.34
-6 -3 12 102.60 4.21
-6 -3 11 25.89 1.69
-6 -3 11 26.27 1.52
-6 -3 10 12.08 1.22
-6 -3 10 14.23 1.10
-6 -3 10 14.93 1.34
-6 -3 9 43.92 2.18
-6 -3 9 38.27 2.12
-6 -3 9 43.18 2.49
-6 -3 9 39.64 1.74
-6 -3 8 4.76 0.95
-6 -3 8 6.91 0.85
-6 -3 8 6.09 0.62
-6 -3 8 6.14 0.65
-6 -3 8 5.95 0.64
-6 -3 8 6.56 0.65
-6 -3 7 60.70 2.92
-6 -3 7 55.84 3.01
-6 -3 7 58.77 2.76
-6 -3 7 55.04 2.79
-6 -3 7 56.56 2.78
-6 -3 7 66.19 2.85
-6 -3 6 90.73 4.23
-6 -3 6 89.36 3.96
-6 -3 6 91.83 4.09
-6 -3 6 87.74 4.00
-6 -3 6 87.18 3.98
-6 -3 5 36.10 2.19
-6 -3 5 35.26 2.01
-6 -3 5 37.36 2.13
-6 -3 5 34.14 2.07
-6 -3 5 37.14 2.06
-6 -3 4 7.17 0.86
-6 -3 4 8.31 0.97
-6 -3 4 7.96 0.89
-6 -3 3 0.43 0.50
-6 -3 3 0.13 0.43
-6 -3 3 0.24 0.48
-6 -3 3 0.69 0.54
-6 -3 2 41.16 2.14
-6 -3 2 43.89 2.44
-6 -3 2 48.45 2.52
-6 -3 2 43.41 2.41
-6 -3 1 1.66 0.55
-6 -3 1 1.81 0.52
-6 -3 1 1.58 0.56
-6 -3 1 2.28 0.65
-6 -3 1 1.90 0.57
-6 -3 1 1.77 0.60
-6 -3 0 19.01 1.33
-6 -3 0 18.81 1.30
-6 -3 0 16.08 1.30
-6 -3 0 16.99 1.27
-6 -3 0 18.57 1.37
-6 -3 0 18.88 1.36
-6 -3 0 20.52 1.36
-6 -3 -1 63.08 3.01
-6 -3 -1 55.61 2.95
-6 -3 -1 59.09 2.85
-6 -3 -1 64.06 2.95
-6 -3 -1 59.02 2.88
-6 -3 -1 64.20 2.91
-6 -3 -2 1.55 0.53
-6 -3 -2 1.36 0.41
-6 -3 -2 1.38 0.57
-6 -3 -2 1.31 0.44
-6 -3 -2 0.86 0.38
-6 -3 -2 1.11 0.41
-6 -3 -3 11.23 0.99
-6 -3 -3 9.95 0.73
-6 -3 -3 10.13 0.92
-6 -3 -3 9.26 0.69
-6 -3 -4 9.25 0.84
-6 -3 -5 0.06 0.33
-6 -3 -6 43.84 2.05
-6 -3 -6 47.57 2.09
-6 -3 -7 14.77 0.78
-6 -3 -7 16.67 0.82
-6 -4 11 237.80 9.21
-6 -4 11 247.72 9.48
-6 -4 10 3.89 0.74
-6 -4 10 4.09 0.67
-6 -4 9 22.27 1.42
-6 -4 9 19.33 1.05
-6 -4 8 353.79 13.11
-6 -4 8 330.61 12.71
-6 -4 8 316.45 12.37
-6 -4 8 336.66 12.36
-6 -4 8 353.40 12.40
-6 -4 7 7.46 1.00
-6 -4 7 6.36 0.68
-6 -4 7 5.00 0.68
-6 -4 7 5.29 0.67
-6 -4 7 6.83 0.71
-6 -4 6 571.90 20.81
-6 -4 6 589.14 20.55
-6 -4 6 558.94 20.57
-6 -4 6 575.81 20.53
-6 -4 5 71.10 3.29
-6 -4 5 64.64 3.00
-6 -4 5 61.86 3.08
-6 -4 5 55.64 2.99
-6 -4 5 62.72 3.02
-6 -4 4 114.00 5.06
-6 -4 4 110.19 4.84
-6 -4 4 112.93 4.90
-6 -4 3 80.32 3.83
-6 -4 3 80.71 3.68
-6 -4 3 77.19 3.72
-6 -4 3 77.82 3.66
-6 -4 3 81.93 3.78
-6 -4 2 15.80 1.29
-6 -4 2 13.05 1.19
-6 -4 1 0.60 0.50
-6 -4 1 0.36 0.35
-6 -4 1 0.27 0.37
-6 -4 1 -0.18 0.49
-6 -4 1 0.33 0.46
-6 -4 1 0.26 0.44
-6 -4 0 57.31 2.77
-6 -4 0 63.77 2.91
-6 -4 0 64.40 2.91
-6 -4 0 52.05 2.76
-6 -4 0 58.51 2.80
-6 -4 0 57.54 2.77
-6 -4 -1 106.51 4.50
-6 -4 -1 106.21 4.43
-6 -4 -1 106.86 4.39
-6 -4 -1 97.81 4.34
-6 -4 -1 103.54 4.38
-6 -4 -2 0.96 0.47
-6 -4 -2 0.49 0.31
-6 -4 -2 0.63 0.32
-6 -4 -2 1.21 0.37
-6 -4 -3 7.79 0.78
-6 -4 -4 137.87 5.57
-6 -4 -6 0.81 0.23
-6 -5 10 16.88 1.21
-6 -5 9 35.87 1.84
-6 -5 8 97.97 3.91
-6 -5 8 99.97 3.59
-6 -5 8 86.01 3.57
-6 -5 8 91.98 3.56
-6 -5 7 48.69 2.28
-6 -5 7 45.50 2.00
-6 -5 7 45.64 2.04
-6 -5 6 341.73 11.64
-6 -5 6 315.49 11.66
-6 -5 6 311.91 11.61
-6 -5 5 137.24 5.31
-6 -5 5 133.67 5.08
-6 -5 5 101.20 4.99
-6 -5 5 114.93 5.04
-6 -5 4 17.83 1.33
-6 -5 4 17.73 1.20
-6 -5 4 17.31 1.27
-6 -5 4 14.24 1.15
-6 -5 3 27.51 1.65
-6 -5 3 21.73 1.44
-6 -5 3 22.81 1.51
-6 -5 3 23.47 1.45
-6 -5 3 22.05 1.49
-6 -5 2 109.90 5.22
-6 -5 2 121.12 5.24
-6 -5 1 113.44 5.03
-6 -5 1 125.70 5.05
-6 -5 1 110.10 4.97
-6 -5 1 131.31 5.03
-6 -5 0 2.59 0.57
-6 -5 0 3.34 0.51
-6 -5 0 2.56 0.51
-6 -5 0 3.75 0.52
-6 -5 -1 68.87 2.95
-6 -5 -1 69.15 2.90
-6 -5 -1 69.55 2.88
-6 -5 -1 65.23 2.84
-6 -5 -1 61.39 2.84
-6 -5 -2 3.62 0.49
-6 -5 -2 1.92 0.32
-6 -5 -3 18.39 1.06
-6 -5 -4 10.57 0.70
-6 -6 10 19.80 1.10
-6 -6 9 0.06 0.23
-6 -6 8 15.50 0.92
-6 -6 8 12.92 0.67
-6 -6 7 16.23 1.03
-6 -6 7 16.57 0.87
-6 -6 7 10.07 0.78
-6 -6 7 14.39 0.86
-6 -6 7 12.32 0.79
-6 -6 6 31.99 1.63
-6 -6 6 34.80 1.49
-6 -6 6 29.90 1.47
-6 -6 5 45.24 1.92
-6 -6 5 31.73 1.79
-6 -6 4 154.27 5.44
-6 -6 4 156.55 5.27
-6 -6 4 110.18 5.15
-6 -6 4 127.42 5.21
-6 -6 4 106.37 5.08
-6 -6 3 -0.07 0.37
-6 -6 3 0.57 0.41
-6 -6 3 0.09 0.36
-6 -6 2 66.84 2.67
-6 -6 2 58.14 2.47
-6 -6 2 51.10 2.48
-6 -6 2 55.40 2.47
-6 -6 2 41.82 2.35
-6 -6 1 36.47 1.70
-6 -6 1 36.97 1.61
-6 -6 1 28.39 1.56
-6 -6 1 31.85 1.56
-6 -6 1 23.54 1.47
-6 -6 0 3.60 0.47
-6 -6 0 3.54 0.41
-6 -6 0 2.14 0.37
-6 -6 0 2.90 0.38
-6 -6 0 2.90 0.39
-6 -6 -1 0.36 0.20
-6 -7 7 2.45 0.33
-6 -7 6 177.42 4.47
-6 -7 6 172.61 4.26
6 7 -6 147.43 4.30
-6 -7 6 123.97 4.17
6 7 -5 14.84 0.84
-6 -7 5 20.57 0.87
-6 -7 4 59.41 3.00
-6 -7 4 58.44 3.03
-6 -7 3 8.33 0.62
-6 -7 3 6.36 0.52
-6 -7 2 21.19 0.98
-6 -7 2 20.47 0.89
6 7 -2 15.73 0.88
-6 -7 2 12.10 0.79
-6 -7 2 15.35 0.82
-6 -7 2 10.49 0.75
-6 -7 1 1.78 0.28
-6 -7 1 1.52 0.23
-6 -7 1 0.45 0.20
-6 -7 1 1.55 0.23
6 7 -1 1.18 0.23
-6 -7 1 0.66 0.22
-7 4 6 4.76 0.72
-7 4 5 0.39 0.54
-7 4 4 13.99 1.21
-7 4 3 97.83 4.49
-7 4 0 18.12 1.03
-7 4 -1 13.21 0.81
-7 4 -1 14.18 0.86
-7 4 -2 18.50 0.98
-7 4 -2 16.68 0.98
-7 4 -3 2.94 0.35
-7 4 -4 8.26 0.53
-7 4 -4 8.52 0.55
-7 3 8 0.63 0.43
-7 3 7 78.77 3.64
-7 3 6 9.96 1.02
-7 3 5 21.61 1.56
-7 3 4 1.85 0.63
-7 3 4 1.04 0.39
-7 3 3 0.94 0.54
-7 3 2 48.13 2.11
-7 3 2 39.49 1.90
-7 3 1 14.33 0.97
-7 3 1 13.35 0.87
-7 3 0 44.88 2.07
-7 3 0 44.73 2.08
-7 3 -1 0.58 0.31
-7 3 -1 0.42 0.30
-7 3 -2 22.61 1.23
-7 3 -2 23.39 1.25
-7 3 -4 20.94 1.08
-7 3 -5 8.77 0.55
-7 3 -5 9.26 0.55
-7 2 9 20.72 1.30
-7 2 8 49.84 2.52
-7 2 7 0.13 0.45
-7 2 6 62.96 2.72
-7 2 6 64.92 3.16
-7 2 5 26.77 1.42
-7 2 5 27.17 1.77
-7 2 4 1.66 0.49
-7 2 4 1.76 0.44
-7 2 4 1.55 0.57
-7 2 2 10.53 0.87
-7 2 2 9.99 0.90
-7 2 1 28.37 1.50
-7 2 1 26.28 1.39
-7 2 1 26.50 1.55
-7 2 0 4.34 0.56
-7 2 0 5.42 0.56
-7 2 0 3.42 0.57
-7 2 -1 28.64 1.54
-7 2 -1 33.89 1.62
-7 2 -2 38.12 1.84
-7 2 -3 5.67 0.54
-7 2 -4 2.67 0.35
-7 2 -5 36.04 1.59
-7 1 10 3.41 0.47
-7 1 9 -0.10 0.36
-7 1 8 -0.04 0.42
-7 1 7 32.23 1.78
-7 1 7 26.13 1.33
-7 1 6 208.46 8.74
-7 1 6 213.47 8.37
-7 1 6 231.24 8.49
-7 1 5 22.79 1.53
-7 1 5 24.05 1.38
-7 1 5 22.63 1.30
-7 1 5 20.97 1.36
-7 1 4 59.69 2.83
-7 1 3 14.19 1.04
-7 1 3 12.47 0.95
-7 1 3 11.13 0.96
-7 1 2 56.45 2.65
-7 1 2 54.35 2.57
-7 1 1 1.42 0.47
-7 1 1 0.88 0.46
-7 1 1 1.65 0.45
-7 1 1 1.24 0.37
-7 1 0 1.39 0.46
-7 1 0 0.77 0.40
-7 1 0 0.73 0.39
-7 1 0 1.43 0.38
-7 1 -1 27.68 1.40
-7 1 -1 28.74 1.45
-7 1 -2 24.26 1.28
-7 1 -2 20.18 1.12
-7 1 -2 22.44 1.23
-7 1 -3 45.92 2.14
-7 1 -3 51.05 2.22
-7 1 -5 264.14 9.89
-7 0 10 40.99 1.93
-7 0 9 0.10 0.34
-7 0 8 37.49 1.98
-7 0 7 95.09 4.41
-7 0 7 104.58 4.15
-7 0 7 101.78 4.21
-7 0 7 110.28 4.22
-7 0 6 0.60 0.36
-7 0 6 0.32 0.33
-7 0 6 0.33 0.35
-7 0 5 21.29 1.28
-7 0 5 22.07 1.39
-7 0 5 24.44 1.40
-7 0 4 377.65 14.39
-7 0 3 142.08 5.99
-7 0 3 151.54 6.10
-7 0 3 153.65 6.09
-7 0 2 6.63 0.71
-7 0 2 7.10 0.75
-7 0 1 81.99 3.50
-7 0 1 77.72 3.55
-7 0 1 77.98 3.36
-7 0 1 85.51 3.57
-7 0 0 4.43 0.56
-7 0 0 4.58 0.60
-7 0 0 4.48 0.52
-7 0 0 3.38 0.56
-7 0 -1 0.68 0.35
-7 0 -1 0.45 0.35
-7 0 -1 0.52 0.36
-7 0 -1 0.39 0.33
-7 0 -2 38.57 1.85
-7 0 -2 39.49 1.81
-7 0 -3 32.17 1.59
-7 0 -5 26.28 1.22
-7 -1 10 115.98 4.61
-7 -1 7 30.29 1.52
-7 -1 7 33.30 1.59
-7 -1 7 32.99 1.58
-7 -1 6 62.02 2.82
-7 -1 6 67.80 2.90
-7 -1 6 66.30 2.88
-7 -1 5 49.90 2.44
-7 -1 5 56.64 2.55
-7 -1 5 54.60 2.52
-7 -1 4 6.29 0.69
-7 -1 3 21.15 1.32
-7 -1 3 23.41 1.39
-7 -1 3 22.27 1.38
-7 -1 2 27.94 1.57
-7 -1 2 29.61 1.64
-7 -1 1 9.10 0.81
-7 -1 1 8.81 0.77
-7 -1 1 8.63 0.78
-7 -1 0 75.77 3.35
-7 -1 0 81.73 3.47
-7 -1 0 80.29 3.42
-7 -1 0 86.86 3.52
-7 -1 -1 0.10 0.32
-7 -1 -1 -0.03 0.30
-7 -1 -1 -0.10 0.31
-7 -1 -1 0.20 0.29
-7 -1 -2 48.62 2.07
-7 -1 -2 47.73 2.11
-7 -1 -3 32.08 1.55
-7 -1 -4 253.84 9.56
-7 -2 8 1.58 0.27
-7 -2 7 131.40 5.74
-7 -2 7 148.62 5.81
-7 -2 6 134.32 5.23
-7 -2 6 152.13 5.27
-7 -2 5 1.74 0.46
-7 -2 5 1.93 0.45
-7 -2 5 2.04 0.44
-7 -2 5 1.76 0.41
-7 -2 4 40.97 1.97
-7 -2 4 35.85 1.91
-7 -2 3 5.29 0.64
-7 -2 3 4.07 0.58
-7 -2 3 4.29 0.59
-7 -2 3 4.58 0.60
-7 -2 2 20.26 1.26
-7 -2 2 19.97 1.22
-7 -2 1 57.60 2.47
-7 -2 1 46.38 2.35
-7 -2 1 46.27 2.32
-7 -2 1 59.58 2.48
-7 -2 0 10.04 0.73
-7 -2 0 9.72 0.76
-7 -2 0 9.57 0.76
-7 -2 -1 2.90 0.41
-7 -2 -1 2.62 0.40
-7 -2 -1 2.48 0.36
-7 -2 -1 3.03 0.41
-7 -2 -2 3.69 0.44
-7 -2 -3 61.09 2.54
-7 -2 -4 4.65 0.37
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-7 -3 7 6.96 0.58
-7 -3 6 2.41 0.39
-7 -3 6 3.44 0.46
-7 -3 6 3.10 0.43
-7 -3 6 2.81 0.41
-7 -3 5 9.24 0.77
-7 -3 5 10.61 0.79
-7 -3 5 9.54 0.75
-7 -3 5 11.34 0.80
-7 -3 5 9.46 0.75
-7 -3 4 40.37 1.89
-7 -3 4 34.98 1.82
-7 -3 3 33.38 1.73
-7 -3 3 31.63 1.67
-7 -3 3 35.33 1.74
-7 -3 2 32.21 1.58
-7 -3 2 27.00 1.49
-7 -3 2 28.67 1.52
-7 -3 1 46.46 2.02
-7 -3 1 38.80 1.95
-7 -3 1 43.66 1.96
-7 -3 1 40.63 1.97
-7 -3 0 14.84 0.86
-7 -3 0 13.19 0.80
-7 -3 0 13.44 0.85
-7 -3 -1 3.66 0.36
-7 -3 -1 3.39 0.32
-7 -3 -2 33.66 1.46
-7 -4 7 196.66 7.19
-7 -4 7 224.97 7.23
-7 -4 6 7.74 0.63
-7 -4 6 8.08 0.57
-7 -4 6 6.21 0.55
-7 -4 6 7.38 0.56
-7 -4 5 47.77 2.10
-7 -4 5 47.20 2.04
-7 -4 5 52.03 2.07
-7 -4 4 122.97 5.43
-7 -4 4 125.11 5.40
-7 -4 4 157.43 5.51
-7 -4 4 155.37 5.51
-7 -4 3 87.32 3.52
-7 -4 3 82.07 3.46
-7 -4 2 0.25 0.28
-7 -4 2 0.06 0.26
-7 -4 2 0.23 0.26
-7 -4 2 0.16 0.25
-7 -4 1 8.71 0.62
-7 -4 1 7.66 0.57
-7 -4 1 9.05 0.62
-7 -4 0 97.02 3.49
-7 -4 0 81.55 3.47
-7 -5 5 5.59 0.48
-7 -5 5 7.81 0.50
-7 -5 4 0.88 0.24
-7 -5 4 1.09 0.23
-7 -5 4 1.42 0.26
-7 -5 3 0.78 0.23
-7 -5 3 1.05 0.22
-7 -5 2 5.70 0.37
-7 -5 2 4.73 0.36
0 0 0 0.00 0.00
TITL 04112023 in P-1
REM P-1 (#2 in standard setting)
CELL 1.54184 6.316001 9.692527 13.746303 97.3357 99.6623 93.5202
ZERR 2.00 0.000166 0.000151 0.000169 0.0012 0.0018 0.0017
LATT 1
SFAC C H Li N
UNIT 32.00 64.00 2.00 4.00
REM CrysAlisPro recorded range (K): Min=119.9; max=120.0; aver:120.0
TEMP -153
SIZE 0.04 0.11 0.35
TREF
HKLF 4
END
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 52460
_shelx_res_file
;
TITL 04112023.res in P-1
04112023.res
created by SHELXL-2018/3 at 16:46:50 on 11-Apr-2023
REM Old TITL 04112023 in P-1
REM SHELXT solution in P-1: R1 0.161, Rweak 0.005, Alpha 0.031
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C16 Li N2
CELL 1.54184 6.3160 9.6925 13.7463 97.336 99.662 93.520
ZERR 2.000 0.0002 0.0002 0.0002 0.001 0.002 0.002
LATT 1
SFAC C H LI N
UNIT 32 62 2 4
TEMP -153
SIZE 0.04 0.11 0.35
L.S. 10
BOND $H
CONF
HTAB
ACTA
LIST 4
FMAP 2
PLAN 1
WGHT 0.058900 0.166800
FVAR 1.30724
LI 3 0.733309 0.332861 0.299853 11.00000 0.02568 0.02300 =
0.02139 0.00531 0.00095 -0.00400
C1 1 0.961265 0.549768 0.177067 11.00000 0.01839 0.02064 =
0.01878 0.00323 0.00358 0.00258
H1 2 1.092963 0.505940 0.156096 11.00000 0.02505
C2 1 0.923713 0.516865 0.278492 11.00000 0.01821 0.01723 =
0.02039 0.00326 0.00285 -0.00181
C3 1 0.735848 0.564320 0.305781 11.00000 0.02237 0.02204 =
0.02391 0.00746 0.00850 0.00245
H3 2 0.709957 0.558626 0.372520 11.00000 0.03165
C4 1 0.609186 0.661182 0.244543 11.00000 0.01841 0.02543 =
0.03395 0.01013 0.00898 0.00434
H4A 2 0.451350 0.626346 0.223426 11.00000 0.03395
H4B 2 0.614244 0.757780 0.284557 11.00000 0.02856
C5 1 0.701542 0.676251 0.149850 11.00000 0.01709 0.02446 =
0.02643 0.00923 0.00168 0.00313
H5 2 0.616756 0.737107 0.105394 11.00000 0.03034
C6 1 0.951592 0.710707 0.173995 11.00000 0.01693 0.02116 =
0.01869 0.00563 0.00363 0.00215
C7 1 0.743593 0.528709 0.102588 11.00000 0.02333 0.02601 =
0.02232 0.00407 -0.00167 -0.00199
H7A 2 0.762056 0.524505 0.030792 11.00000 0.03242
H7B 2 0.636437 0.450879 0.109813 11.00000 0.03184
C8 1 1.042177 0.755837 0.085520 11.00000 0.02349 0.03025 =
0.02111 0.00946 0.00580 0.00247
H8A 2 0.990070 0.694357 0.022618 11.00000 0.03565
H8B 2 1.204130 0.759026 0.097548 11.00000 0.03520
H8C 2 1.000500 0.853852 0.075638 11.00000 0.03408
C9 1 1.049193 0.810889 0.267385 11.00000 0.02227 0.02089 =
0.02285 0.00318 0.00426 0.00021
H9A 2 1.030371 0.911408 0.255934 11.00000 0.03726
H9B 2 0.979847 0.795188 0.323584 11.00000 0.03113
H9C 2 1.209430 0.799985 0.286553 11.00000 0.03147
C10 1 1.064263 0.431936 0.328580 11.00000 0.01948 0.02462 =
0.02286 0.00614 0.00169 0.00117
H10A 2 1.200341 0.413301 0.304659 11.00000 0.02930
H10B 2 1.058359 0.428358 0.399570 11.00000 0.02894
N1 4 0.577572 0.169967 0.190273 11.00000 0.02003 0.02191 =
0.01633 0.00347 0.00326 0.00000
N2 4 0.646984 0.218315 0.409755 11.00000 0.02329 0.02173 =
0.01625 0.00390 0.00153 -0.00010
C11 1 0.487488 0.110363 0.349118 11.00000 0.02572 0.02384 =
0.02085 0.00499 0.00462 -0.00458
H11B 2 0.465244 0.029253 0.387368 11.00000 0.03332
H11A 2 0.345051 0.154393 0.334816 11.00000 0.03283
C12 1 0.555340 0.056913 0.251427 11.00000 0.03012 0.01837 =
0.02211 0.00349 0.00415 -0.00118
H12A 2 0.702652 0.016510 0.264469 11.00000 0.03183
H12B 2 0.446723 -0.019314 0.214529 11.00000 0.03126
C13 1 0.549552 0.291739 0.489252 11.00000 0.03844 0.03175 =
0.02067 0.00294 0.00721 0.00577
H13A 2 0.659251 0.363154 0.532275 11.00000 0.04099
H13B 2 0.501012 0.225283 0.534374 11.00000 0.04482
H13C 2 0.423203 0.337935 0.459379 11.00000 0.03553
C14 1 0.838874 0.155742 0.454852 11.00000 0.02758 0.03616 =
0.02611 0.01264 0.00042 0.00451
H14A 2 0.937203 0.228105 0.495817 11.00000 0.03198
H14B 2 0.912835 0.108696 0.401814 11.00000 0.04063
H14C 2 0.800447 0.081978 0.496432 11.00000 0.04109
C15 1 0.365706 0.197789 0.138163 11.00000 0.02244 0.03021 =
0.02369 0.00342 -0.00088 0.00115
H15A 2 0.378903 0.271730 0.096281 11.00000 0.03966
H15B 2 0.287096 0.111036 0.092654 11.00000 0.03803
H15C 2 0.273180 0.229934 0.186516 11.00000 0.03659
C16 1 0.713514 0.128238 0.116716 11.00000 0.02960 0.03910 =
0.02467 0.00177 0.01124 0.00314
H16A 2 0.863055 0.116331 0.150149 11.00000 0.04445
H16B 2 0.654817 0.038022 0.073658 11.00000 0.04521
H16C 2 0.721327 0.203232 0.074574 11.00000 0.04427
HKLF 4
REM 04112023.res in P-1
REM wR2 = 0.1075, GooF = S = 1.089, Restrained GooF = 1.089 for all data
REM R1 = 0.0387 for 3172 Fo > 4sig(Fo) and 0.0402 for all 3373 data
REM 296 parameters refined using 0 restraints
END
WGHT 0.0589 0.1668
REM No hydrogen bonds found for HTAB generation
REM Highest difference peak 0.282, deepest hole -0.218, 1-sigma level 0.038
Q1 1 1.0027 0.7335 0.1340 11.00000 0.05 0.28
;
_shelx_res_checksum 73055
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Li Li 0.7333(3) 0.33286(17) 0.29985(12) 0.0238(3) Uani d 1 . .
C C1 0.96126(15) 0.54977(10) 0.17707(7) 0.0192(2) Uani d 1 . .
H H1 1.093(2) 0.5059(13) 0.1561(9) 0.025(3) Uiso d 1 . .
C C2 0.92371(15) 0.51687(9) 0.27849(7) 0.0188(2) Uani d 1 . .
C C3 0.73585(15) 0.56432(10) 0.30578(7) 0.0219(2) Uani d 1 . .
H H3 0.710(2) 0.5586(14) 0.3725(10) 0.032(3) Uiso d 1 . .
C C4 0.60919(16) 0.66118(11) 0.24454(8) 0.0248(2) Uani d 1 . .
H H4A 0.451(2) 0.6263(14) 0.2234(10) 0.034(3) Uiso d 1 . .
H H4B 0.614(2) 0.7578(14) 0.2846(9) 0.029(3) Uiso d 1 . .
C C5 0.70154(15) 0.67625(10) 0.14985(7) 0.0224(2) Uani d 1 . .
H H5 0.617(2) 0.7371(14) 0.1054(10) 0.030(3) Uiso d 1 . .
C C6 0.95159(14) 0.71071(10) 0.17399(7) 0.0186(2) Uani d 1 . .
C C7 0.74359(16) 0.52871(11) 0.10259(7) 0.0247(2) Uani d 1 . .
H H7A 0.762(2) 0.5245(14) 0.0308(10) 0.032(3) Uiso d 1 . .
H H7B 0.636(2) 0.4509(14) 0.1098(10) 0.032(3) Uiso d 1 . .
C C8 1.04218(16) 0.75584(11) 0.08552(7) 0.0242(2) Uani d 1 . .
H H8A 0.990(2) 0.6944(15) 0.0226(11) 0.036(3) Uiso d 1 . .
H H8B 1.204(2) 0.7590(14) 0.0975(10) 0.035(3) Uiso d 1 . .
H H8C 1.000(2) 0.8539(15) 0.0756(10) 0.034(3) Uiso d 1 . .
C C9 1.04919(16) 0.81089(10) 0.26738(7) 0.0220(2) Uani d 1 . .
H H9A 1.030(2) 0.9114(15) 0.2559(10) 0.037(4) Uiso d 1 . .
H H9B 0.980(2) 0.7952(14) 0.3236(10) 0.031(3) Uiso d 1 . .
H H9C 1.209(2) 0.8000(14) 0.2866(10) 0.031(3) Uiso d 1 . .
C C10 1.06426(16) 0.43194(10) 0.32858(7) 0.0223(2) Uani d 1 . .
H H10A 1.200(2) 0.4133(13) 0.3047(10) 0.029(3) Uiso d 1 . .
H H10B 1.058(2) 0.4284(14) 0.3996(10) 0.029(3) Uiso d 1 . .
N N1 0.57757(12) 0.16997(8) 0.19027(6) 0.01942(19) Uani d 1 . .
N N2 0.64698(13) 0.21831(8) 0.40976(6) 0.02063(19) Uani d 1 . .
C C11 0.48749(16) 0.11036(10) 0.34912(7) 0.0235(2) Uani d 1 . .
H H11B 0.465(2) 0.0293(14) 0.3874(10) 0.033(3) Uiso d 1 . .
H H11A 0.345(2) 0.1544(14) 0.3348(10) 0.033(3) Uiso d 1 . .
C C12 0.55534(17) 0.05691(10) 0.25143(7) 0.0237(2) Uani d 1 . .
H H12A 0.703(2) 0.0165(14) 0.2645(10) 0.032(3) Uiso d 1 . .
H H12B 0.447(2) -0.0193(14) 0.2145(10) 0.031(3) Uiso d 1 . .
C C13 0.54955(19) 0.29174(12) 0.48925(8) 0.0300(2) Uani d 1 . .
H H13A 0.659(2) 0.3632(16) 0.5323(11) 0.041(4) Uiso d 1 . .
H H13B 0.501(2) 0.2253(16) 0.5344(11) 0.045(4) Uiso d 1 . .
H H13C 0.423(2) 0.3379(15) 0.4594(10) 0.036(3) Uiso d 1 . .
C C14 0.83887(18) 0.15574(12) 0.45485(8) 0.0297(2) Uani d 1 . .
H H14A 0.937(2) 0.2281(14) 0.4958(10) 0.032(3) Uiso d 1 . .
H H14B 0.913(2) 0.1087(16) 0.4018(11) 0.041(4) Uiso d 1 . .
H H14C 0.800(2) 0.0820(15) 0.4964(11) 0.041(4) Uiso d 1 . .
C C15 0.36571(16) 0.19779(11) 0.13816(8) 0.0261(2) Uani d 1 . .
H H15A 0.379(2) 0.2717(16) 0.0963(11) 0.040(4) Uiso d 1 . .
H H15B 0.287(2) 0.1110(15) 0.0927(11) 0.038(4) Uiso d 1 . .
H H15C 0.273(2) 0.2299(15) 0.1865(11) 0.037(3) Uiso d 1 . .
C C16 0.71351(18) 0.12824(13) 0.11672(8) 0.0306(2) Uani d 1 . .
H H16A 0.863(3) 0.1163(16) 0.1501(11) 0.044(4) Uiso d 1 . .
H H16B 0.655(2) 0.0380(17) 0.0737(12) 0.045(4) Uiso d 1 . .
H H16C 0.721(2) 0.2032(16) 0.0746(12) 0.044(4) 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
Li 0.0257(8) 0.0230(8) 0.0214(8) -0.0040(6) 0.0009(6) 0.0053(6)
C1 0.0184(4) 0.0206(4) 0.0188(4) 0.0026(3) 0.0036(3) 0.0032(3)
C2 0.0182(4) 0.0172(4) 0.0204(4) -0.0018(3) 0.0028(3) 0.0033(3)
C3 0.0224(5) 0.0220(5) 0.0239(5) 0.0024(4) 0.0085(4) 0.0075(4)
C4 0.0184(5) 0.0254(5) 0.0340(5) 0.0043(4) 0.0090(4) 0.0101(4)
C5 0.0171(4) 0.0245(5) 0.0264(5) 0.0031(4) 0.0017(4) 0.0092(4)
C6 0.0169(4) 0.0212(4) 0.0187(4) 0.0022(3) 0.0036(3) 0.0056(3)
C7 0.0233(5) 0.0260(5) 0.0223(5) -0.0020(4) -0.0017(4) 0.0041(4)
C8 0.0235(5) 0.0302(5) 0.0211(5) 0.0025(4) 0.0058(4) 0.0095(4)
C9 0.0223(5) 0.0209(5) 0.0228(5) 0.0002(3) 0.0043(4) 0.0032(4)
C10 0.0195(5) 0.0246(5) 0.0229(5) 0.0012(4) 0.0017(4) 0.0061(4)
N1 0.0200(4) 0.0219(4) 0.0163(4) 0.0000(3) 0.0033(3) 0.0035(3)
N2 0.0233(4) 0.0217(4) 0.0163(4) -0.0001(3) 0.0015(3) 0.0039(3)
C11 0.0257(5) 0.0238(5) 0.0208(5) -0.0046(4) 0.0046(4) 0.0050(4)
C12 0.0301(5) 0.0184(4) 0.0221(5) -0.0012(4) 0.0041(4) 0.0035(4)
C13 0.0384(6) 0.0317(5) 0.0207(5) 0.0058(5) 0.0072(4) 0.0029(4)
C14 0.0276(5) 0.0362(6) 0.0261(5) 0.0045(5) 0.0004(4) 0.0126(4)
C15 0.0224(5) 0.0302(5) 0.0237(5) 0.0012(4) -0.0009(4) 0.0034(4)
C16 0.0296(6) 0.0391(6) 0.0247(5) 0.0031(5) 0.0112(4) 0.0018(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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
N1 Li N2 . . 88.76(7) y
N1 Li C2 . . 127.71(9) ?
N2 Li C2 . . 143.10(9) ?
N1 Li C10 . . 131.22(9) ?
N2 Li C10 . . 116.38(8) ?
C2 Li C10 . . 37.49(4) ?
N1 Li C3 . . 130.88(8) ?
N2 Li C3 . . 125.26(9) ?
C2 Li C3 . . 36.78(4) ?
C10 Li C3 . . 68.75(6) ?
N1 Li H3 . . 144.2(3) ?
N2 Li H3 . . 101.0(4) ?
C2 Li H3 . . 54.2(3) ?
C10 Li H3 . . 74.7(3) ?
C3 Li H3 . . 24.5(3) ?
N1 Li H10B . . 146.3(3) ?
N2 Li H10B . . 93.3(3) ?
C2 Li H10B . . 54.1(3) ?
C10 Li H10B . . 24.9(3) ?
C3 Li H10B . . 73.2(3) ?
H3 Li H10B . . 68.1(5) ?
C2 C1 C7 . . 109.50(8) ?
C2 C1 C6 . . 109.22(7) ?
C7 C1 C6 . . 87.13(7) ?
C2 C1 H1 . . 112.5(7) ?
C7 C1 H1 . . 119.1(7) ?
C6 C1 H1 . . 116.8(7) ?
C3 C2 C10 . . 127.17(9) y
C3 C2 C1 . . 114.19(8) y
C10 C2 C1 . . 118.27(8) y
C3 C2 Li . . 74.15(7) ?
C10 C2 Li . . 72.36(7) ?
C1 C2 Li . . 123.80(7) ?
C2 C3 C4 . . 119.68(8) ?
C2 C3 Li . . 69.07(7) ?
C4 C3 Li . . 134.63(8) ?
C2 C3 H3 . . 119.2(8) y
C4 C3 H3 . . 118.7(8) ?
Li C3 H3 . . 82.2(8) ?
C3 C4 C5 . . 110.65(8) ?
C3 C4 H4A . . 112.3(8) ?
C5 C4 H4A . . 107.7(8) ?
C3 C4 H4B . . 110.8(7) ?
C5 C4 H4B . . 108.5(7) ?
H4A C4 H4B . . 106.7(10) ?
C4 C5 C7 . . 108.05(8) ?
C4 C5 C6 . . 111.37(8) ?
C7 C5 C6 . . 87.51(7) ?
C4 C5 H5 . . 112.9(7) ?
C7 C5 H5 . . 118.0(7) ?
C6 C5 H5 . . 116.4(7) ?
C9 C6 C8 . . 108.90(8) ?
C9 C6 C5 . . 118.81(8) ?
C8 C6 C5 . . 112.52(8) ?
C9 C6 C1 . . 118.35(7) ?
C8 C6 C1 . . 111.55(8) ?
C5 C6 C1 . . 85.08(7) ?
C5 C7 C1 . . 86.05(7) ?
C5 C7 H7A . . 113.1(8) ?
C1 C7 H7A . . 113.2(8) ?
C5 C7 H7B . . 115.2(8) ?
C1 C7 H7B . . 117.4(7) ?
H7A C7 H7B . . 110.2(11) ?
C6 C8 H8A . . 113.8(8) ?
C6 C8 H8B . . 111.3(8) ?
H8A C8 H8B . . 106.9(11) ?
C6 C8 H8C . . 109.4(8) ?
H8A C8 H8C . . 107.7(11) ?
H8B C8 H8C . . 107.6(11) ?
C6 C9 H9A . . 110.5(8) ?
C6 C9 H9B . . 111.8(8) ?
H9A C9 H9B . . 106.9(11) ?
C6 C9 H9C . . 110.5(7) ?
H9A C9 H9C . . 108.5(11) ?
H9B C9 H9C . . 108.4(11) ?
C2 C10 Li . . 70.15(7) ?
C2 C10 H10A . . 118.8(7) y
Li C10 H10A . . 136.4(8) ?
C2 C10 H10B . . 117.1(8) y
Li C10 H10B . . 85.3(7) ?
H10A C10 H10B . . 118.6(11) ?
C15 N1 C16 . . 109.20(8) ?
C15 N1 C12 . . 110.40(8) ?
C16 N1 C12 . . 109.29(8) ?
C15 N1 Li . . 115.05(8) ?
C16 N1 Li . . 111.74(8) ?
C12 N1 Li . . 100.82(7) ?
C14 N2 C13 . . 109.09(8) ?
C14 N2 C11 . . 110.86(8) ?
C13 N2 C11 . . 109.16(8) ?
C14 N2 Li . . 108.18(8) ?
C13 N2 Li . . 117.95(8) ?
C11 N2 Li . . 101.34(7) ?
N2 C11 C12 . . 111.64(8) ?
N2 C11 H11B . . 110.5(8) ?
C12 C11 H11B . . 109.4(8) ?
N2 C11 H11A . . 107.5(7) ?
C12 C11 H11A . . 109.3(8) ?
H11B C11 H11A . . 108.3(11) ?
N1 C12 C11 . . 111.51(8) ?
N1 C12 H12A . . 107.2(7) ?
C11 C12 H12A . . 110.4(7) ?
N1 C12 H12B . . 110.6(8) ?
C11 C12 H12B . . 108.8(7) ?
H12A C12 H12B . . 108.3(10) ?
N2 C13 H13A . . 109.5(8) ?
N2 C13 H13B . . 111.6(9) ?
H13A C13 H13B . . 107.0(12) ?
N2 C13 H13C . . 109.7(8) ?
H13A C13 H13C . . 110.0(12) ?
H13B C13 H13C . . 109.0(12) ?
N2 C14 H14A . . 108.9(8) ?
N2 C14 H14B . . 110.7(8) ?
H14A C14 H14B . . 108.9(12) ?
N2 C14 H14C . . 111.6(8) ?
H14A C14 H14C . . 109.8(11) ?
H14B C14 H14C . . 107.0(12) ?
N1 C15 H15A . . 111.1(9) ?
N1 C15 H15B . . 112.2(8) ?
H15A C15 H15B . . 107.4(12) ?
N1 C15 H15C . . 110.6(8) ?
H15A C15 H15C . . 107.2(12) ?
H15B C15 H15C . . 108.2(11) ?
N1 C16 H16A . . 111.0(9) ?
N1 C16 H16B . . 111.9(9) ?
H16A C16 H16B . . 107.9(12) ?
N1 C16 H16C . . 108.2(9) ?
H16A C16 H16C . . 108.2(12) ?
H16B C16 H16C . . 109.6(12) ?
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
Li N1 . 2.1057(18) y
Li N2 . 2.1078(18) y
Li C2 . 2.1684(18) y
Li C3 . 2.2334(19) y
Li C10 . 2.1971(19) y
Li H3 . 2.311(13) ?
Li H10B . 2.334(13) ?
C1 C2 . 1.5222(12) ?
C1 C7 . 1.5555(13) ?
C1 C6 . 1.5705(13) ?
C1 H1 . 1.024(13) ?
C2 C3 . 1.3902(14) y
C2 C10 . 1.4032(13) y
C3 C4 . 1.5159(13) ?
C3 H3 . 0.966(14) ?
C4 C5 . 1.5326(14) ?
C4 H4A . 1.014(14) ?
C4 H4B . 1.019(13) ?
C5 C7 . 1.5508(14) ?
C5 C6 . 1.5643(13) ?
C5 H5 . 1.014(13) ?
C6 C9 . 1.5210(13) ?
C6 C8 . 1.5286(12) ?
C7 H7A . 1.009(14) ?
C7 H7B . 1.008(14) ?
C8 H8A . 0.980(15) ?
C8 H8B . 1.006(14) ?
C8 H8C . 1.021(14) ?
C9 H9A . 1.017(15) ?
C9 H9B . 0.973(14) ?
C9 H9C . 1.018(13) ?
C10 H10A . 0.989(13) ?
C10 H10B . 0.988(13) ?
N1 C15 . 1.4657(12) ?
N1 C16 . 1.4673(13) ?
N1 C12 . 1.4775(12) ?
N2 C14 . 1.4680(13) ?
N2 C13 . 1.4698(13) ?
N2 C11 . 1.4732(12) ?
C11 C12 . 1.5160(14) ?
C11 H11B . 1.015(14) ?
C11 H11A . 1.019(14) ?
C12 H12A . 1.029(14) ?
C12 H12B . 1.000(14) ?
C13 H13A . 1.004(15) ?
C13 H13B . 1.017(16) ?
C13 H13C . 0.993(14) ?
C14 H14A . 0.961(14) ?
C14 H14B . 1.007(15) ?
C14 H14C . 1.013(15) ?
C15 H15A . 0.983(15) ?
C15 H15B . 1.027(14) ?
C15 H15C . 0.990(15) ?
C16 H16A . 0.999(16) ?
C16 H16B . 1.003(16) ?
C16 H16C . 0.989(16) ?
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
C7 C1 C2 C3 . . . . -39.93(11) ?
C6 C1 C2 C3 . . . . 53.92(10) ?
C7 C1 C2 C10 . . . . 133.56(9) ?
C6 C1 C2 C10 . . . . -132.58(8) ?
C7 C1 C2 Li . . . . 46.66(11) ?
C6 C1 C2 Li . . . . 140.52(8) ?
C10 C2 C3 C4 . . . . 177.25(9) ?
C1 C2 C3 C4 . . . . -9.94(13) ?
Li C2 C3 C4 . . . . -130.37(10) ?
C10 C2 C3 Li . . . . -52.38(10) ?
C1 C2 C3 Li . . . . 120.43(9) ?
C2 C3 C4 C5 . . . . 7.46(13) ?
Li C3 C4 C5 . . . . -81.66(12) ?
C3 C4 C5 C7 . . . . 45.11(10) ?
C3 C4 C5 C6 . . . . -49.40(11) ?
C4 C5 C6 C9 . . . . -39.25(11) ?
C7 C5 C6 C9 . . . . -147.68(8) ?
C4 C5 C6 C8 . . . . -168.16(8) ?
C7 C5 C6 C8 . . . . 83.41(9) ?
C4 C5 C6 C1 . . . . 80.53(8) ?
C7 C5 C6 C1 . . . . -27.90(7) ?
C2 C1 C6 C9 . . . . 38.36(11) ?
C7 C1 C6 C9 . . . . 148.03(8) ?
C2 C1 C6 C8 . . . . 165.86(7) ?
C7 C1 C6 C8 . . . . -84.47(8) ?
C2 C1 C6 C5 . . . . -81.85(8) ?
C7 C1 C6 C5 . . . . 27.82(7) ?
C4 C5 C7 C1 . . . . -83.53(8) ?
C6 C5 C7 C1 . . . . 28.15(7) ?
C2 C1 C7 C5 . . . . 81.35(8) ?
C6 C1 C7 C5 . . . . -28.04(7) ?
C3 C2 C10 Li . . . . 53.08(10) ?
C1 C2 C10 Li . . . . -119.46(9) ?
C14 N2 C11 C12 . . . . -74.60(10) ?
C13 N2 C11 C12 . . . . 165.20(8) ?
Li N2 C11 C12 . . . . 40.05(10) ?
C15 N1 C12 C11 . . . . -80.01(10) ?
C16 N1 C12 C11 . . . . 159.87(8) ?
Li N1 C12 C11 . . . . 42.06(10) ?
N2 C11 C12 N1 . . . . -60.64(11) ?