#------------------------------------------------------------------------------
#$Date: 2021-08-25 05:10:05 +0300 (Wed, 25 Aug 2021) $
#$Revision: 268200 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/39/2243903.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_2243903
loop_
_publ_author_name
'Rue, Kelly'
'Raptis, Raphael G.'
_publ_section_title
;
Low-temperature crystal structure of 4-chloro-1H-pyrazole
;
_journal_coeditor_code ZL5013
_journal_issue 9
_journal_name_full 'Acta Crystallographica Section E'
_journal_page_first 1
_journal_page_last 0
_journal_paper_doi 10.1107/S2056989021008604
_journal_volume 77
_journal_year 2021
_chemical_formula_iupac 'C3 H3 Cl N2'
_chemical_formula_moiety 'C3 H3 Cl N2'
_chemical_formula_sum 'C3 H3 Cl N2'
_chemical_formula_weight 102.52
_chemical_name_systematic 4-Chloro-1H-pyrazole
_space_group_crystal_system orthorhombic
_space_group_IT_number 62
_space_group_name_Hall '-P 2ac 2n'
_space_group_name_H-M_alt 'P n m a'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary difmap
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 12
_cell_length_a 14.9122(10)
_cell_length_b 17.6410(9)
_cell_length_c 4.9878(3)
_cell_measurement_reflns_used 6701
_cell_measurement_temperature 170
_cell_measurement_theta_max 30.1820
_cell_measurement_theta_min 2.3340
_cell_volume 1312.12(14)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_data_collection
;
APEX3 (Bruker, 2020)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature 170.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'abstract diffractometer'
_diffrn_measurement_device_type 'Bruker D8 CMOS'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0429
_diffrn_reflns_av_unetI/netI 0.0158
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 6
_diffrn_reflns_limit_l_min -6
_diffrn_reflns_number 25891
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.995
_diffrn_reflns_theta_min 2.309
_exptl_absorpt_coefficient_mu 0.689
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.76001
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2019)
;
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_density_diffrn 1.557
_exptl_crystal_description 'rect. Prism'
_exptl_crystal_F_000 624
_exptl_crystal_size_max 0.285
_exptl_crystal_size_mid 0.137
_exptl_crystal_size_min 0.076
_refine_diff_density_max 0.270
_refine_diff_density_min -0.264
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.062
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 97
_refine_ls_number_reflns 1798
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.062
_refine_ls_R_factor_all 0.0427
_refine_ls_R_factor_gt 0.0327
_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^)+(0.0418P)^2^+0.5547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0835
_refine_ls_wR_factor_ref 0.0919
_reflns_number_gt 1481
_reflns_number_total 1798
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file zl5013sup1.cif
_cod_data_source_block I
_cod_original_cell_volume 1312.13(14)
_cod_database_code 2243903
_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 0.828
_shelx_estimated_absorpt_t_max 0.949
_shelx_hkl_file
;
0 2 0 224.00 13.74 4
0 -2 0 228.23 14.11 4
0 2 0 166.96 11.25 3
0 -2 0 291.96 14.58 3
0 -2 0 210.81 12.93 3
0 2 0 296.39 14.70 3
0 2 0 238.58 12.96 2
0 -2 0 177.15 11.32 2
0 -3 0 2.68 3.60 4
0 3 0 -0.04 2.61 3
0 -3 0 -1.56 2.00 2
0 -3 0 -0.83 1.42 3
0 -3 0 7.54 2.80 1
0 -3 0 2.48 1.72 1
0 3 0 4.28 1.73 1
0 4 010854.77 132.46 4
0 -4 010608.47 126.67 3
0 4 010713.91 124.09 2
0 -4 010356.99 87.80 1
0 4 010936.53 130.12 3
0 -4 010467.77 128.85 4
0 -4 010607.36 88.28 1
0 4 010049.78 85.61 1
0 5 0 9.54 6.45 3
0 -5 0 20.66 6.75 3
0 5 0 14.99 6.00 2
0 -5 0 15.45 7.18 2
0 -5 0 14.11 4.74 3
0 -5 0 26.39 8.19 4
0 -5 0 7.86 3.97 1
0 5 0 9.86 6.92 4
0 -5 0 11.19 5.63 4
0 6 0 1087.00 51.54 4
0 -6 0 1140.65 54.27 4
0 6 0 1079.96 51.02 3
0 -6 0 1035.49 48.72 3
0 6 0 1049.93 47.85 2
0 -6 0 1157.10 52.60 3
0 -6 0 1150.66 50.85 2
0 -6 0 1047.55 33.42 1
0 -6 0 1039.24 49.29 4
0 -6 0 1063.58 34.13 1
0 6 0 1000.00 32.21 1
0 7 0 11.78 5.12 2
0 -7 0 4.88 3.33 2
0 -7 0 2.22 6.07 3
0 -7 0 -2.03 4.97 4
0 -7 0 4.94 5.24 1
0 -7 0 11.59 9.09 4
0 7 0 1.59 7.16 4
0 7 0 0.08 5.01 3
0 -7 0 6.88 4.06 3
0 -8 0 1799.76 79.08 4
0 8 0 1868.54 78.05 4
0 8 0 1687.28 74.23 3
0 -8 0 1890.71 77.11 3
0 8 0 1815.75 72.73 2
0 -8 0 1828.61 77.48 3
0 -8 0 1932.77 78.03 2
0 -8 0 1765.79 50.37 1
0 -8 0 1788.69 77.43 4
0 -8 0 1752.22 52.99 1
0 9 0 0.55 4.84 3
0 -9 0 -2.69 6.19 3
0 -9 0 -0.39 4.00 1
0 -9 0 3.68 6.48 2
0 9 0 8.89 8.21 2
0 -9 0 6.12 8.41 3
0 -9 0 6.67 5.08 1
0 -9 0 2.55 4.30 4
0 -9 0 5.84 10.23 4
0 9 0 0.46 5.23 4
0 -10 028968.09 357.21 4
0 -10 028847.50 341.50 3
0 10 027962.37 338.44 3
0 10 028316.60 326.27 2
0 -10 029439.90 346.60 3
0 -10 030335.07 350.06 2
0 -10 027090.66 225.20 1
0 -10 027833.25 239.18 1
0 11 0 65.56 21.81 3
0 -11 0 78.14 26.22 3
0 11 0 71.05 21.47 2
0 -11 0 86.72 25.18 2
0 -11 0 69.23 22.74 3
0 11 0 77.01 24.02 4
0 -11 0 87.54 29.20 4
0 -11 0 94.24 17.21 1
0 -11 0 98.29 17.93 1
0 -11 0 118.24 31.80 4
0 12 0 9156.07 205.56 2
0 -12 0 8728.35 141.17 1
0 -12 0 9183.41 213.08 3
0 12 0 8973.43 213.30 4
0 -12 0 9232.50 152.84 1
0 -12 0 9138.32 215.13 4
0 13 0 53.39 19.80 2
0 -13 0 37.43 11.82 1
0 -13 0 48.06 22.13 3
0 13 0 58.56 22.54 4
0 -13 0 35.12 12.82 1
0 -13 0 47.72 20.78 4
0 14 0 9875.46 234.95 2
0 -14 0 9841.57 162.63 1
0 -14 010516.30 250.43 3
0 14 0 9699.41 240.29 4
0 -14 0 9751.96 171.02 1
0 -14 0 9772.63 243.68 4
0 15 0 56.78 17.81 2
0 -15 0 55.42 15.13 1
0 -15 0 70.56 23.92 3
0 15 0 60.22 22.65 4
0 -15 0 57.29 19.00 1
0 -15 0 46.68 19.00 4
0 16 0 575.53 60.96 2
0 -16 0 516.04 39.22 1
0 -16 0 608.68 63.43 4
0 16 0 541.80 61.88 4
0 -16 0 546.99 43.80 1
0 -16 0 551.95 60.42 3
0 -17 0 9.52 11.50 1
0 17 0 19.29 17.32 4
0 -17 0 12.42 16.36 4
0 -17 0 -2.30 10.89 1
0 -18 0 28.64 12.21 3
0 -18 0 20.09 9.28 1
0 18 0 34.84 20.57 2
0 -18 0 31.40 23.24 2
0 -18 0 25.10 16.61 4
0 18 0 11.74 11.09 4
0 -19 0 4.49 11.45 1
0 19 0 2.59 11.15 2
0 -19 0 3.80 14.10 2
0 -19 0 9.71 22.97 4
0 -19 0 -31.59 26.36 3
0 19 0 -16.25 20.37 4
0 -20 0 1735.47 126.39 3
0 -20 0 1269.92 66.78 1
0 -20 0 1637.79 119.56 2
0 20 0 1514.90 117.38 2
0 -20 0 1721.51 131.17 4
0 20 0 1560.50 122.90 4
0 21 0 7.49 18.05 2
0 -21 0 10.25 18.50 3
0 -21 0 34.99 28.83 4
0 -21 0 30.65 17.28 2
0 -22 0 258.62 56.03 4
0 23 0 10.74 25.27 2
0 -23 0 9.04 22.24 2
0 -23 0 7.28 19.70 3
-1 -1 0 0.59 1.20 3
1 1 0 1.80 1.21 3
1 -1 0 -0.05 0.67 3
-1 1 0 -1.48 1.72 3
-1 -1 0 0.78 1.56 4
1 1 0 0.46 1.11 4
-1 1 0 0.55 1.35 1
1 -1 0 -0.34 1.34 1
1 -1 0 -0.01 0.74 4
-1 1 0 0.38 0.90 4
-1 -1 0 -0.12 0.96 2
1 1 0 -0.02 0.71 2
-1 2 0 1.97 1.23 2
1 2 0 0.38 1.23 2
-1 -2 0 2.69 2.21 2
1 -2 0 3.07 1.77 2
1 -2 0 7.37 2.82 3
-1 2 0 2.22 2.12 3
1 2 0 4.21 1.69 3
-1 -2 0 3.73 2.55 3
1 -2 0 0.96 1.75 1
-1 2 0 0.98 2.18 1
1 -2 0 4.55 3.05 4
-1 2 0 4.46 2.89 4
-1 -2 0 3.33 1.43 4
1 2 0 5.14 2.54 4
1 -3 0 4.33 3.86 4
-1 -3 0 2.11 1.93 4
-1 3 0 3.93 2.93 4
1 -3 0 3.40 2.76 2
1 3 0 4.70 2.72 2
-1 -3 0 5.31 3.90 2
-1 3 0 5.80 3.95 3
1 -3 0 3.14 2.54 3
1 3 0 0.97 2.73 3
1 3 0 2.96 2.09 4
-1 3 0 3.60 1.78 1
1 -3 0 3.45 2.73 1
1 3 0 8.08 2.45 1
-1 -3 0 2.83 1.50 1
1 3 0 4.15 3.49 4
-1 -3 0 -1.46 1.61 4
-1 4 0 2.39 3.90 4
-1 -4 0 -0.17 2.11 4
1 4 0 2.97 3.55 4
1 4 0 1.47 4.02 2
-1 -4 0 0.51 2.70 2
-1 4 0 10.58 4.08 2
1 -4 0 1.77 3.66 2
-1 4 0 2.39 4.09 3
-1 -4 0 4.22 3.37 3
1 -4 0 -1.39 1.99 3
-1 4 0 8.98 3.69 1
-1 -4 0 1.94 2.37 1
1 -4 0 4.17 2.39 1
1 4 0 1.16 1.73 1
1 4 0 1.77 2.49 4
-1 -4 0 6.17 4.05 4
1 -5 0 7.31 5.30 4
-1 -5 0 3.42 3.57 4
-1 5 0 6.17 4.43 4
1 5 0 10.86 8.21 4
-1 -5 0 3.51 2.55 3
1 -5 0 -2.75 3.72 3
1 5 0 -1.66 3.66 3
-1 5 0 4.54 5.41 2
1 5 0 4.77 4.04 2
-1 -5 0 3.53 3.40 2
1 -5 0 1.56 2.78 2
-1 5 0 4.21 5.18 3
1 -5 0 8.15 5.26 3
-1 5 0 3.98 4.65 1
1 -5 0 11.23 5.53 1
-1 -5 0 1.82 4.07 4
1 5 0 6.19 5.40 4
1 -5 0 8.57 3.54 1
1 5 0 3.13 1.83 1
-1 -5 0 3.40 2.62 1
1 -6 0 6.01 4.15 4
-1 6 0 2.02 4.63 4
1 6 0 0.46 4.83 4
-1 -6 0 -1.73 4.44 4
1 6 0 -0.92 3.42 3
-1 -6 0 4.50 4.87 3
1 -6 0 -0.63 4.94 3
1 -6 0 1.94 6.26 2
-1 -6 0 1.83 3.21 2
1 6 0 -0.35 3.36 2
-1 6 0 -1.77 3.67 2
1 -6 0 6.19 5.08 3
-1 6 0 6.30 4.97 3
1 -6 0 2.96 4.21 1
-1 -6 0 0.41 4.14 3
-1 -6 0 -0.89 2.88 1
1 6 0 0.04 3.78 4
-1 -6 0 4.35 6.00 4
-1 -7 0 4.39 5.17 4
-1 7 0 -0.64 4.04 4
1 7 0 3.99 6.90 4
1 -7 0 -8.36 7.94 4
1 7 0 6.85 7.71 2
-1 -7 0 -2.55 5.25 2
-1 7 0 3.79 4.33 2
1 -7 0 -2.39 3.27 2
-1 -7 0 4.05 6.79 3
1 -7 0 8.83 5.50 3
-1 7 0 2.71 4.21 3
-1 -7 0 0.60 4.31 3
1 -7 0 8.70 5.83 3
1 7 0 2.35 5.55 3
1 -7 0 4.78 2.73 1
-1 -7 0 2.48 3.27 1
-1 7 0 2.60 4.57 1
1 7 0 4.02 3.89 1
-1 -7 0 0.68 2.67 1
1 -7 0 1.24 3.79 1
-1 -7 0 2.63 5.41 4
-1 -8 0 12.28 8.67 4
1 8 0 -1.57 6.65 4
1 -8 0 -3.29 7.92 4
-1 8 0 -2.16 8.10 4
1 8 0 -4.10 8.23 3
1 -8 0 -2.96 5.33 3
-1 -8 0 4.89 6.10 3
1 8 0 -2.52 5.20 2
-1 -8 0 -0.75 5.00 2
1 -8 0 8.38 8.26 2
-1 8 0 0.66 5.32 2
-1 8 0 -3.04 4.25 3
-1 -8 0 3.52 6.11 3
1 -8 0 3.41 6.98 3
1 -8 0 0.32 3.78 1
-1 -8 0 0.10 3.74 1
-1 -8 0 5.51 4.49 4
1 -8 0 5.45 5.42 1
1 8 0 -0.65 3.68 1
1 -9 0 -3.14 5.68 4
1 9 0 4.12 4.73 4
-1 9 0 -6.03 4.83 4
1 -9 0 -8.20 8.77 3
1 9 0 2.98 5.18 3
-1 -9 0 4.32 4.70 3
1 -9 0 -3.49 6.25 2
1 9 0 -8.10 7.20 2
-1 9 0 -0.10 7.87 2
-1 -9 0 5.59 6.15 2
1 -9 0 1.73 7.48 3
-1 -9 0 -2.62 6.27 3
-1 -9 0 1.18 3.12 1
1 -9 0 -2.16 4.95 1
-1 9 0 -9.60 9.20 3
1 -9 0 2.87 4.63 1
-1 -9 0 -3.20 4.17 1
1 9 0 -2.39 3.72 1
-1 -9 0 -5.35 8.53 4
1 -9 0 4.30 4.55 4
1 -10 0 -4.25 7.91 4
-1 -10 0 -5.73 10.81 4
-1 -10 0 16.04 10.02 2
-1 10 0 3.97 7.81 2
1 -10 0 4.31 5.89 3
-1 -10 0 -11.40 13.13 3
-1 -10 0 -4.34 9.37 3
1 10 0 0.06 10.52 3
-1 -10 0 5.80 7.40 1
1 -10 0 4.71 6.05 1
-1 -10 0 4.29 5.35 1
1 -10 0 3.07 4.40 1
-1 11 0 -2.22 7.49 4
1 -11 0 8.51 9.48 4
1 11 0 -0.57 5.56 4
1 -11 0 9.03 8.26 2
-1 -11 0 0.29 8.59 2
1 11 0 -6.14 10.04 2
1 -11 0 -6.78 13.94 3
-1 -11 0 7.95 6.71 3
-1 -11 0 -0.58 5.22 1
1 -11 0 7.77 6.46 1
-1 -11 0 7.97 5.62 4
1 -11 0 -0.50 11.51 4
-1 -11 0 -0.97 10.51 3
1 -11 0 -3.18 9.03 3
1 11 0 0.68 7.85 3
1 -11 0 1.22 5.97 1
-1 -11 0 1.49 4.80 1
1 -12 0 -3.22 9.21 3
-1 -12 0 -8.33 10.86 3
1 -12 0 5.22 5.46 1
-1 -12 0 3.19 5.83 1
1 12 0 1.68 9.14 2
-1 12 0 2.98 6.54 2
-1 -12 0 0.91 7.22 1
1 -12 0 -4.47 7.57 1
-1 12 0 3.91 8.79 4
1 12 0 -3.24 6.62 4
1 -12 0 -10.56 11.02 4
-1 -12 0 -3.72 8.83 4
1 -13 0 0.17 6.76 3
-1 -13 0 -4.61 8.19 3
1 -13 0 -1.25 7.02 1
-1 -13 0 -3.62 7.78 1
1 13 0 -8.27 10.24 2
-1 13 0 -3.67 11.35 2
-1 -13 0 5.33 6.55 1
1 -13 0 -0.41 8.49 1
1 13 0 7.90 14.05 4
-1 13 0 -2.58 8.53 4
1 -13 0 4.97 10.31 4
-1 -13 0 -10.29 14.83 4
1 -14 0 6.86 11.28 3
-1 -14 0 -12.79 13.41 3
1 -14 0 3.84 6.28 1
-1 -14 0 -10.40 6.40 1
1 14 0 6.31 12.90 2
-1 14 0 2.11 9.40 2
-1 -14 0 2.89 6.82 1
1 -14 0 0.49 8.65 1
1 14 0 0.19 7.63 4
-1 14 0 -18.12 16.77 4
-1 -14 0 -3.20 11.85 4
1 -14 0 -15.68 17.63 4
1 -15 0 -3.18 15.22 3
-1 -15 0 5.46 8.78 3
-1 -15 0 0.12 7.82 1
1 -15 0 9.94 8.99 1
-1 15 0 10.71 8.38 2
1 15 0 -4.78 10.17 2
-1 -15 0 5.69 9.46 1
1 -15 0 17.30 8.81 1
1 15 0 -2.45 8.63 4
-1 15 0 -2.41 10.64 4
-1 -15 0 7.48 10.98 4
1 -15 0 4.83 13.31 4
-1 -16 0 -0.11 10.88 3
1 -16 0 -16.01 14.50 3
1 16 0 7.60 8.81 4
1 16 0 -8.70 17.14 2
-1 16 0 -16.94 15.99 2
1 -16 0 7.27 10.11 1
-1 -16 0 8.17 6.86 1
-1 -16 0 10.26 9.20 1
-1 16 0 -16.60 13.95 4
1 -16 0 10.87 17.21 4
-1 -16 0 4.11 13.84 4
1 17 0 21.58 18.35 4
1 17 0 -2.47 9.87 2
-1 -17 0 4.17 10.39 1
1 -17 0 2.37 9.72 1
1 -17 0 13.09 13.79 1
-1 -17 0 4.53 9.59 1
-1 -17 0 4.23 13.84 2
-1 17 0 3.47 13.22 4
1 -17 0 -4.69 18.08 4
-1 -17 0 9.76 16.26 4
-1 -18 0 26.06 19.93 3
1 -18 0 -14.07 12.21 3
1 18 0 -9.95 10.29 2
-1 18 0 -6.14 18.26 2
-1 -18 0 0.40 8.87 1
-1 -18 0 1.33 10.86 1
1 -18 0 3.64 12.98 1
-1 -18 0 0.96 12.33 2
-1 18 0 -13.62 20.21 4
1 -18 0 -4.56 14.10 4
-1 -18 0 9.56 15.96 4
-1 -19 0 -25.56 23.64 3
1 -19 0 -0.41 21.45 3
-1 19 0 6.14 12.00 2
1 19 0 4.98 11.95 2
1 -19 0 25.00 15.53 1
-1 -19 0 -10.39 12.77 1
1 -19 0 9.92 20.96 1
-1 -19 0 -0.60 15.70 1
-1 -19 0 12.35 13.62 2
1 -19 0 -3.95 11.91 2
-1 -19 0 6.03 16.62 4
1 -19 0 -13.71 13.50 4
-1 19 0 -0.42 16.69 4
-1 -20 0 -4.77 20.28 3
1 -20 0 10.63 21.01 3
-1 20 0 2.34 16.53 2
1 20 0 2.12 20.38 2
-1 -20 0 5.80 12.78 1
1 -20 0 13.96 17.45 2
-1 -20 0 5.32 14.37 2
-1 20 0 -21.64 22.65 4
1 -20 0 -8.82 11.91 1
1 -20 0 -6.71 17.89 4
-1 -20 0 -0.93 15.69 4
-1 21 0 -3.25 15.60 2
1 21 0 0.61 16.61 2
-1 -21 0 3.79 19.23 2
1 -21 0 16.59 13.54 2
1 -21 0 -18.22 20.92 4
-1 -21 0 2.16 17.03 4
1 -21 0 11.15 18.21 1
-1 -21 0 -2.44 12.79 1
-1 -21 0 10.62 21.61 3
1 -21 0 -24.06 22.52 3
-1 21 0 20.83 18.69 4
-1 -22 0 -14.13 22.95 4
1 -22 0 13.21 22.47 4
-1 -22 0 -2.78 25.31 2
1 22 0 25.20 24.03 2
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-7 -5 -6 405.54 61.31 4
7 -5 -6 274.06 51.84 2
7 5 -6 460.82 69.46 2
7 5 -6 584.56 67.53 1
-7 -5 6 534.91 62.24 1
7 -5 6 586.22 78.30 1
-7 -6 6 -42.50 24.79 3
-7 6 -6 -2.50 20.98 4
-7 -6 -6 4.10 21.43 4
7 -6 -6 -0.76 16.25 2
7 -6 6 -9.78 26.66 1
-7 -6 6 -44.19 25.20 1
7 6 -6 6.26 22.27 2
7 6 -6 -1.18 18.89 1
-7 7 -6 -38.88 30.23 4
-7 -7 -6 -7.75 18.46 4
-7 -7 6 -0.43 20.25 3
7 7 -6 3.87 20.84 1
7 -7 6 40.81 30.15 1
-7 -8 -6 -23.05 21.92 4
7 8 -6 43.54 29.20 2
7 -8 6 43.83 32.02 1
-7 -9 6 1.26 24.12 3
7 9 -6 59.10 31.44 2
-7 9 -6 99.35 49.93 4
7 -9 6 118.29 40.02 1
-7 10 -6 -21.28 28.29 4
7 -10 6 54.26 31.93 1
-7 -10 6 24.25 32.69 3
7 -11 6 52.45 33.25 1
7 -12 6 295.76 58.49 1
-8 0 -6 24.35 23.85 4
8 0 -6 40.91 27.42 2
-8 0 6 15.68 21.49 3
-8 1 6 27.44 19.71 3
-8 -1 6 52.99 29.33 3
-8 -1 -6 23.07 24.47 4
-8 1 -6 36.32 29.85 4
8 -1 -6 45.15 20.13 1
8 1 -6 80.53 30.91 1
8 1 -6 86.32 35.65 2
8 -1 -6 25.27 19.37 2
-8 1 6 93.23 32.09 1
-8 -1 6 42.45 21.84 1
-8 -2 6 108.81 37.98 3
-8 2 6 78.54 29.56 3
-8 2 -6 128.59 34.57 4
-8 -2 -6 92.48 30.13 4
8 -2 -6 208.56 46.85 1
8 2 -6 142.43 35.19 1
8 2 -6 90.97 33.39 2
8 -2 -6 70.98 28.15 2
-8 -2 6 209.43 48.59 1
-8 2 6 168.44 40.38 1
-8 -3 6 150.08 42.10 3
-8 3 6 93.60 34.30 3
8 -3 -6 218.03 49.77 1
8 3 -6 203.06 46.29 1
8 -3 6 233.47 53.90 1
-8 -3 6 227.61 51.68 1
-8 3 6 242.15 51.63 1
8 3 -6 134.67 39.34 2
8 -3 -6 59.87 26.94 2
-8 3 -6 183.38 45.00 4
-8 -3 -6 133.98 42.74 4
-8 4 -6 84.14 32.83 4
-8 -4 -6 34.38 24.38 4
-8 -4 6 50.38 21.87 3
8 4 -6 124.48 37.87 1
8 4 -6 30.05 19.62 2
8 -4 6 130.73 42.84 1
-8 5 -6 0.81 27.55 4
-8 -5 -6 34.15 27.61 4
8 5 -6 20.17 29.88 1
-8 -5 6 33.67 29.27 3
8 5 -6 33.08 28.01 2
8 -5 6 26.40 24.02 1
8 6 -6 20.05 20.01 1
-8 -6 6 80.11 39.27 3
-8 -6 -6 -29.66 25.92 4
8 6 -6 117.79 41.03 2
8 -6 6 6.74 26.97 1
-8 7 -6 110.37 42.40 4
-8 -7 -6 116.83 43.02 4
-8 8 -6 -45.90 36.89 4
-8 -8 6 6.98 20.49 3
8 8 -6 34.88 25.24 2
-8 -8 -6 -52.72 39.53 4
-8 9 -6 32.97 34.16 4
8 9 -6 1.70 23.88 2
-8 -9 6 7.42 21.82 3
9 0 -6 21.77 28.16 1
-9 0 -6 28.53 27.94 4
9 0 -6 39.10 25.74 2
-9 0 6 52.99 28.59 3
9 -1 -6 -34.37 26.63 1
-9 -1 -6 -78.33 44.03 4
-9 1 -6 -1.15 25.14 4
9 1 -6 24.74 22.72 2
-9 1 6 -2.80 19.30 3
-9 -1 6 -92.07 33.37 3
-9 2 6 236.37 47.94 3
-9 -2 6 305.98 55.32 3
-9 2 -6 284.06 60.89 4
-9 -2 -6 288.03 59.04 4
9 -2 -6 406.03 64.14 1
9 2 -6 336.45 57.44 1
9 2 -6 223.92 49.11 2
-9 3 6 1.71 21.37 3
-9 3 -6 -18.70 31.00 4
-9 -3 -6 4.98 20.66 4
9 3 -6 -25.70 24.16 1
-9 -3 6 9.27 22.23 3
9 3 -6 24.44 24.48 2
-9 4 6 92.54 34.37 3
9 4 -6 57.61 30.31 1
-9 -4 -6 57.29 36.09 4
-9 -4 6 0.29 21.84 3
9 4 -6 26.68 24.19 2
9 5 -6 58.29 28.56 1
-9 5 -6 49.02 31.87 4
-9 -5 -6 57.21 30.94 4
9 5 -6 28.34 21.52 2
-9 -6 6 37.33 29.20 3
-9 -6 -6 17.30 25.91 4
9 6 -6 -15.20 26.83 1
9 6 -6 2.81 22.08 2
-9 6 -6 23.20 22.79 4
-9 -7 6 58.13 39.82 3
-9 -7 -6 30.60 23.49 4
-9 -8 -6 32.25 25.41 4
9 8 -6 88.16 36.81 2
9 9 -6 44.64 30.61 2
10 0 -6 -38.10 27.72 1
-10 0 6 -15.54 23.18 3
10 1 -6 29.98 25.48 1
10 -1 -6 44.59 27.20 1
-10 1 6 6.53 21.60 3
-10 -1 6 -8.20 27.35 3
-10 2 -6 376.03 73.71 4
-10 2 6 345.56 64.26 3
-10 -2 6 259.67 57.96 3
-10 3 -6 51.34 27.68 4
-10 3 6 7.85 27.69 3
-10 4 6 12.93 25.51 3
10 4 -6 -13.73 27.87 1
-10 4 -6 58.23 37.24 4
-10 -4 6 3.92 23.79 3
10 4 -6 -8.67 20.22 2
10 5 -6 3.00 22.83 1
-10 5 -6 13.72 30.33 4
-10 -5 6 21.04 26.41 3
10 5 -6 18.88 20.98 2
-10 -6 6 42.73 27.73 3
10 6 -6 7.68 24.14 2
-10 -7 -6 -9.13 31.43 4
10 8 -6 158.15 49.99 2
-10 -8 -6 25.70 28.78 4
-10 -9 -6 40.67 34.00 4
-11 0 -6 37.00 25.61 4
11 1 -6 8.44 23.24 1
-11 -1 6 5.85 24.02 3
-11 1 -6 -51.24 33.78 4
-11 -1 -6 7.48 27.93 4
11 2 -6 16.92 26.94 1
-11 -2 6 -46.50 32.19 3
-11 2 -6 57.55 33.29 4
-11 -2 -6 49.69 31.73 4
11 3 -6 0.13 25.47 1
-11 -3 -6 14.63 34.52 4
-11 -3 6 5.29 28.07 3
-11 -4 -6 9.91 29.88 4
-11 -4 6 18.20 24.03 3
-11 4 6 -42.82 25.47 3
-11 -5 -6 61.96 39.81 4
-11 -6 -6 53.17 42.39 4
-12 0 6 -25.52 30.88 3
-12 1 6 -18.82 27.60 3
12 2 -6 3.66 30.41 1
-12 2 6 33.50 40.77 3
12 3 -6 58.09 36.89 1
-12 3 6 16.61 36.74 3
-12 4 6 0.32 30.19 3
0 -5 7 309.06 62.60 1
0 -6 7 -3.95 28.43 1
0 -7 7 12.46 29.30 1
-1 -5 7 37.93 26.15 1
-1 -6 7 -7.41 35.02 1
1 -7 7 46.18 32.71 1
-1 -7 7 8.76 30.86 1
1 -8 7 93.60 38.26 1
-2 -4 7 152.30 39.94 1
-2 -5 7 -30.06 33.12 1
-2 -6 7 81.32 38.03 1
-3 -4 7 64.25 38.59 1
-3 -5 7 55.38 31.20 1
3 5 -7 -73.51 36.98 1
-3 -6 7 47.93 29.10 1
3 6 -7 -42.52 34.53 1
4 -1 -7 12.37 23.31 2
4 -2 -7 -78.52 39.78 2
4 -3 -7 55.07 38.41 2
-4 -4 7 307.42 56.42 1
4 4 -7 329.32 62.37 1
4 -5 -7 -77.53 43.43 2
-4 -5 7 -23.28 30.56 1
4 5 -7 30.55 29.27 1
4 -6 -7 39.90 38.00 2
5 0 -7 112.75 38.25 2
5 -1 -7 -24.48 28.33 2
5 -2 -7 13.85 24.44 2
5 -3 -7 -11.31 25.75 2
5 -4 -7 -1.68 26.05 2
5 5 -7 65.59 36.33 1
-5 -5 7 -33.13 36.36 1
6 0 -7 88.79 41.90 2
6 -1 -7 77.42 40.63 2
6 1 -7 87.48 40.73 2
6 -2 -7 157.63 49.12 2
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 51703
_shelx_res_file
;
TITL KR125 in Pnma #62
kr125.res
created by SHELXL-2018/3 at 15:48:02 on 14-Aug-2021
REM reset to Pnma #62
CELL 0.71073 14.912183 17.641016 4.987817 90 90 90
ZERR 12 0.000983 0.000904 0.000341 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,0.5-Z
SYMM -X,0.5+Y,-Z
SFAC C H Cl N
UNIT 36 36 12 24
EQIV $1 1-X,1-Y,-Z
EQIV $2 +X,1.5-Y,+Z
L.S. 5
PLAN 1
SIZE 0.285 0.137 0.076
TEMP -103.15
CONF
HTAB N3 N2_$1
HTAB N1 N1_$2
HTAB N2 N3_$1
FREE H3a H2_$1
BOND
MORE -1
BOND $H
fmap 2
acta
OMIT -3 58
REM
REM
REM
WGHT 0.041800 0.554700
FVAR 1.46885
CL1 3 0.659124 0.458300 0.736724 11.00000 0.05250 0.03027 =
0.05253 0.00342 -0.00952 0.00392
C1 1 0.666381 0.615040 0.689317 11.00000 0.03790 0.03354 =
0.04115 -0.00200 -0.00269 -0.00168
C2 1 0.635955 0.545545 0.600787 11.00000 0.03396 0.02806 =
0.03705 -0.00057 0.00078 0.00197
N1 4 0.634272 0.668221 0.524804 11.00000 0.04076 0.03300 =
0.04312 -0.00116 0.00172 -0.00067
AFIX 43
H1A 2 0.644141 0.717242 0.538844 10.50000 -1.20000
AFIX 0
C3 1 0.584679 0.560010 0.377602 11.00000 0.04290 0.03454 =
0.03912 -0.00322 -0.00529 0.00282
N2 4 0.584355 0.634622 0.334023 11.00000 0.04496 0.03831 =
0.03836 0.00281 -0.00220 0.00528
AFIX 43
H2 2 0.556236 0.657939 0.202649 10.50000 -1.20000
AFIX 0
CL2 3 0.702558 0.250000 0.599280 10.50000 0.04165 0.03951 =
0.03561 0.00000 -0.00534 0.00000
C5 1 0.623427 0.250000 0.349491 10.50000 0.03593 0.03113 =
0.03087 0.00000 -0.00113 0.00000
N3 4 0.527300 0.288131 0.043185 11.00000 0.04321 0.03701 =
0.03840 -0.00006 -0.00364 0.00676
AFIX 43
H3A 2 0.494432 0.317237 -0.061095 10.50000 -1.20000
AFIX 0
C4 1 0.585427 0.312258 0.227600 11.00000 0.04826 0.03059 =
0.04007 -0.00401 -0.00352 0.00525
H3 2 0.557128 0.526607 0.252702 11.00000 0.04275
H1 2 0.703061 0.627866 0.838719 11.00000 0.04025
H4 2 0.596185 0.366101 0.261226 11.00000 0.05088
HKLF 4
REM KR125 in Pnma #62
REM wR2 = 0.0919, GooF = S = 1.062, Restrained GooF = 1.062 for all data
REM R1 = 0.0327 for 1481 Fo > 4sig(Fo) and 0.0427 for all 1798 data
REM 97 parameters refined using 0 restraints
END
WGHT 0.0419 0.5555
REM Highest difference peak 0.270, deepest hole -0.264, 1-sigma level 0.049
Q1 1 0.6429 0.5788 0.6726 11.00000 0.05 0.27
;
_shelx_res_checksum 22431
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl Cl1 0.65912(3) 0.45830(2) 0.73672(9) 0.04510(15) Uani d 1 . .
C C1 0.66638(11) 0.61504(9) 0.6893(4) 0.0375(3) Uani d 1 . .
C C2 0.63595(10) 0.54554(8) 0.6008(3) 0.0330(3) Uani d 1 . .
N N1 0.63427(9) 0.66822(7) 0.5248(3) 0.0390(3) Uani d 1 . .
H H1A 0.644141 0.717242 0.538844 0.047 Uiso calc 0.5 . .
C C3 0.58468(11) 0.56001(10) 0.3776(3) 0.0389(4) Uani d 1 . .
N N2 0.58435(9) 0.63462(8) 0.3340(3) 0.0405(3) Uani d 1 . .
H H2 0.556236 0.657939 0.202649 0.049 Uiso calc 0.5 . .
Cl Cl2 0.70256(4) 0.250000 0.59928(11) 0.03892(16) Uani d 1 . .
C C5 0.62343(15) 0.250000 0.3495(4) 0.0326(4) Uani d 1 . .
N N3 0.52730(9) 0.28813(7) 0.0432(3) 0.0395(3) Uani d 1 . .
H H3A 0.494432 0.317237 -0.061095 0.047 Uiso calc 0.5 . .
C C4 0.58543(12) 0.31226(10) 0.2276(3) 0.0396(4) Uani d 1 . .
H H3 0.5571(14) 0.5266(11) 0.253(4) 0.043(5) Uiso d 1 . .
H H1 0.7031(12) 0.6279(11) 0.839(4) 0.040(5) Uiso d 1 . .
H H4 0.5962(12) 0.3661(12) 0.261(4) 0.051(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 0.0525(3) 0.0303(2) 0.0525(3) 0.00392(16) -0.00952(19) 0.00342(16)
C1 0.0379(8) 0.0335(8) 0.0412(8) -0.0017(6) -0.0027(7) -0.0020(7)
C2 0.0340(7) 0.0281(7) 0.0371(8) 0.0020(6) 0.0008(6) -0.0006(6)
N1 0.0408(7) 0.0330(6) 0.0431(7) -0.0007(6) 0.0017(6) -0.0012(6)
C3 0.0429(9) 0.0345(8) 0.0391(8) 0.0028(6) -0.0053(7) -0.0032(7)
N2 0.0450(8) 0.0383(7) 0.0384(7) 0.0053(6) -0.0022(6) 0.0028(6)
Cl2 0.0416(3) 0.0395(3) 0.0356(3) 0.000 -0.0053(2) 0.000
C5 0.0359(11) 0.0311(10) 0.0309(10) 0.000 -0.0011(9) 0.000
N3 0.0432(7) 0.0370(7) 0.0384(7) 0.0068(6) -0.0036(6) -0.0001(6)
C4 0.0483(10) 0.0306(8) 0.0401(8) 0.0052(7) -0.0035(7) -0.0040(7)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C2 C1 H1 . . 130.6(11) ?
N1 C1 C2 . . 108.04(14) ?
N1 C1 H1 . . 121.4(11) ?
C1 C2 Cl1 . . 127.15(13) ?
C3 C2 Cl1 . . 126.74(12) ?
C3 C2 C1 . . 106.09(14) ?
C1 N1 H1A . . 125.6 ?
C1 N1 N2 . . 108.87(13) ?
N2 N1 H1A . . 125.6 ?
C2 C3 H3 . . 131.0(12) ?
N2 C3 C2 . . 108.49(15) ?
N2 C3 H3 . . 120.2(12) ?
N1 N2 H2 . . 125.7 ?
C3 N2 N1 . . 108.50(14) ?
C3 N2 H2 . . 125.7 ?
C4 C5 Cl2 8_565 . 127.11(10) ?
C4 C5 Cl2 . . 127.11(10) ?
C4 C5 C4 . 8_565 105.8(2) ?
N3 N3 H3A 8_565 . 125.7 ?
C4 N3 N3 . 8_565 108.61(9) ?
C4 N3 H3A . . 125.7 ?
C5 C4 H4 . . 129.2(11) ?
N3 C4 C5 . . 108.50(15) ?
N3 C4 H4 . . 122.3(11) ?
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
Cl1 C2 . 1.7169(15) ?
C1 C2 . 1.380(2) ?
C1 N1 . 1.335(2) ?
C1 H1 . 0.952(19) ?
C2 C3 . 1.374(2) ?
N1 H1A . 0.8800 ?
N1 N2 . 1.3457(19) ?
C3 N2 . 1.334(2) ?
C3 H3 . 0.951(19) ?
N2 H2 . 0.8800 ?
Cl2 C5 . 1.716(2) ?
C5 C4 . 1.377(2) ?
C5 C4 8_565 1.377(2) ?
N3 N3 8_565 1.345(3) ?
N3 H3A . 0.8800 ?
N3 C4 . 1.334(2) ?
C4 H4 . 0.98(2) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1A N1 8_575 0.88 2.03 2.885(3) 164.7 yes
N2 H2 N3 5_665 0.88 1.99 2.8582(19) 168.7 yes
N3 H3A N2 5_665 0.88 1.99 2.8582(19) 169.4 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cl1 C2 C3 N2 . . . . -178.73(13) ?
C1 C2 C3 N2 . . . . 0.03(19) ?
C1 N1 N2 C3 . . . . 0.07(18) ?
C2 C1 N1 N2 . . . . -0.05(18) ?
C2 C3 N2 N1 . . . . -0.06(19) ?
N1 C1 C2 Cl1 . . . . 178.76(12) ?
N1 C1 C2 C3 . . . . 0.01(18) ?
Cl2 C5 C4 N3 . . . . 179.74(15) ?
N3 N3 C4 C5 8_565 . . . -0.20(16) ?
C4 C5 C4 N3 8_565 . . . 0.3(3) ?
_cod_database_fobs_code 2243903