#------------------------------------------------------------------------------
#$Date: 2024-12-14 03:55:55 +0100 (Sat, 14 Dec 2024) $
#$Revision: 296873 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023334.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_2023334
loop_
_publ_author_name
'Kucheriv, Olesia I.'
'Apostu, Mircea-Odin'
'Prysiazhna, Olena'
'Potaskalov, Vadim A.'
'Malinkin, Sergey O.'
_publ_section_title
;
Crystal structure and Hirshfeld surface analysis of the layered hybrid
metal halide poly[bis(2-iodoethylammonium)
[di-\m-iodido-diiodidogermanate(II)]]
;
_journal_coeditor_code OO2009
_journal_issue 1
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi 10.1107/S2056989024011800
_journal_volume 81
_journal_year 2025
_chemical_formula_iupac '(C2 H7 I N)2 [Ge I4]'
_chemical_formula_moiety '2(C2 H7 I N +), Ge I4 2-'
_chemical_formula_sum 'C4 H14 Ge I6 N2'
_chemical_formula_weight 924.16
_chemical_name_systematic
;
Poly[bis(2-iodoethylammonium) [di-\m-iodido-diiodidogermanate(II)]]
;
_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 geom
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha 90
_cell_angle_beta 97.264(2)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 8.1431(2)
_cell_length_b 8.8362(2)
_cell_length_c 25.1787(7)
_cell_measurement_reflns_used 10013
_cell_measurement_temperature 100.02(10)
_cell_measurement_theta_max 30.4960
_cell_measurement_theta_min 3.2620
_cell_volume 1797.17(8)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature 100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0304
_diffrn_reflns_av_unetI/netI 0.0238
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 31
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 5413
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 30.216
_diffrn_reflns_theta_min 2.445
_exptl_absorpt_coefficient_mu 11.986
_exptl_absorpt_correction_T_max 0.852
_exptl_absorpt_correction_T_min 0.399
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour 'clear intense orange'
_exptl_crystal_density_diffrn 3.416
_exptl_crystal_description plate
_exptl_crystal_F_000 1608
_exptl_crystal_size_max 0.135
_exptl_crystal_size_mid 0.081
_exptl_crystal_size_min 0.014
_refine_diff_density_max 1.213
_refine_diff_density_min -1.271
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.189
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 121
_refine_ls_number_reflns 5413
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.189
_refine_ls_R_factor_all 0.0421
_refine_ls_R_factor_gt 0.0352
_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^)+(0.0215P)^2^+42.6836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0861
_refine_ls_wR_factor_ref 0.0917
_reflns_number_gt 4967
_reflns_number_total 5413
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file oo2009.cif
_cod_data_source_block I
_cod_original_cell_volume 1797.16(8)
_cod_database_code 2023334
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 4 5084.67 13.0897 -2
0 0 -4 5084.67 13.0897 1
0 0 6 80.3500 5.44474 -2
0 0 -6 80.3500 5.44474 1
0 0 8 35541.2 114.717 -2
0 0 -8 35541.2 114.717 1
0 0 10 1254.35 22.6517 -2
0 0 -10 1254.35 22.6517 1
0 0 12 458.927 14.7418 -2
0 0 -12 458.927 14.7418 1
0 0 14 303.819 10.0282 -2
0 0 -14 303.819 10.0282 1
0 0 16 1246.29 18.2780 -2
0 0 -16 1246.29 18.2780 1
0 0 -18 586.875 13.2541 -2
0 0 18 586.875 13.2541 1
0 0 20 1359.19 18.7094 -2
0 0 -20 1359.19 18.7094 1
0 0 22 64.0250 7.64254 -2
0 0 -22 64.0250 7.64254 1
0 0 -24 1147.98 44.8151 -2
0 0 24 1147.98 44.8151 1
0 0 -26 123.545 17.7418 -2
0 0 26 123.545 17.7418 1
0 0 -28 1729.98 59.0878 -2
0 0 28 1729.98 59.0878 1
0 0 -30 45.1646 13.4715 -2
0 0 30 45.1646 13.4715 1
0 -1 -1 7.85015 1.18523 -2
0 1 1 7.85015 1.18523 1
0 1 -2 5.23319 1.11417 -2
0 -1 2 5.23319 1.11417 1
0 1 -3 15.8823 0.89116 -2
0 -1 3 15.8823 0.89116 1
0 1 4 23.0425 2.19047 -2
0 -1 -4 23.0425 2.19047 1
0 1 -5 346.005 3.38034 -2
0 -1 5 346.005 3.38034 1
0 1 -6 4864.94 23.7999 -2
0 -1 6 4864.94 23.7999 1
0 1 -7 4931.84 16.5972 -2
0 -1 7 4931.84 16.5972 1
0 1 8 20.9838 1.54635 -2
0 -1 -8 20.9838 1.54635 1
0 -1 9 3148.59 23.4428 -2
0 1 -9 3148.59 23.4428 1
0 1 -10 1634.81 11.7687 -2
0 -1 10 1634.81 11.7687 1
0 1 11 523.311 9.61790 -2
0 -1 -11 523.311 9.61790 1
0 -1 12 362.634 8.32234 -2
0 1 -12 362.634 8.32234 1
0 1 13 356.244 9.40910 -2
0 -1 -13 356.244 9.40910 1
0 1 14 5730.02 25.1734 -2
0 -1 -14 5730.02 25.1734 1
0 1 15 3758.19 21.1181 -2
0 -1 -15 3758.19 21.1181 1
0 1 -16 104.460 5.30767 -2
0 -1 16 104.460 5.30767 1
0 -1 17 3795.89 29.3357 -2
0 1 -17 3795.89 29.3357 1
0 -1 18 775.203 10.6791 -2
0 1 -18 775.203 10.6791 1
0 1 -19 790.003 12.6807 -2
0 -1 19 790.003 12.6807 1
0 1 -20 66.7781 7.50301 -2
0 -1 20 66.7781 7.50301 1
0 -1 21 7.45572 4.49351 -2
0 1 -21 7.45572 4.49351 1
0 1 -22 1938.08 28.6818 -2
0 -1 22 1938.08 28.6818 1
0 1 -23 492.429 18.7321 -2
0 -1 23 492.429 18.7321 1
0 -1 24 223.745 13.5529 -2
0 1 -24 223.745 13.5529 1
0 1 -25 1632.04 54.6872 -2
0 -1 25 1632.04 54.6872 1
0 1 -26 33.3292 12.7484 -2
0 -1 26 33.3292 12.7484 1
0 1 -27 359.319 28.0132 -2
0 -1 27 359.319 28.0132 1
0 1 -28 1.98193 8.21619 -2
0 -1 28 1.98193 8.21619 1
0 1 -29 231.290 23.6892 -2
0 -1 29 231.290 23.6892 1
0 1 -30 141.977 20.3363 -2
0 -1 30 141.977 20.3363 1
0 1 -31 27.0974 12.8445 -2
0 -1 31 27.0974 12.8445 1
0 -2 0 5000.56 27.0544 -2
0 2 0 5000.56 27.0544 1
0 -2 1 8.54030 1.60324 -2
0 2 -1 8.54030 1.60324 1
0 -2 -2 189.999 2.05014 -2
0 2 2 189.999 2.05014 1
0 -2 -3 8158.54 11.7001 -2
0 2 3 8158.54 11.7001 1
0 -2 -4 1383.21 6.20709 -2
0 2 4 1383.21 6.20709 1
0 2 -5 9125.09 21.9749 -2
0 -2 5 9125.09 21.9749 1
0 -2 -6 1038.78 6.11366 -2
0 2 6 1038.78 6.11366 1
0 -2 -7 81.5751 2.01464 -2
0 2 7 81.5751 2.01464 1
0 2 -8 2424.07 10.0542 -2
0 -2 8 2424.07 10.0542 1
0 2 -9 323.058 4.96193 -2
0 -2 9 323.058 4.96193 1
0 -2 -10 268.061 3.81039 -2
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0 2 11 246.574 4.00955 -2
0 -2 -11 246.574 4.00955 1
0 2 12 634.329 8.37047 -2
0 -2 -12 634.329 8.37047 1
0 2 -13 1039.37 18.8894 -2
0 -2 13 1039.37 18.8894 1
0 -2 14 291.341 6.73804 -2
0 2 -14 291.341 6.73804 1
0 2 15 884.401 14.3494 -2
0 -2 -15 884.401 14.3494 1
0 2 -16 25.4506 3.29182 -2
0 -2 16 25.4506 3.29182 1
0 2 -17 1297.70 17.9570 -2
0 -2 17 1297.70 17.9570 1
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0 -2 -18 1194.13 17.5953 1
0 -2 -19 659.694 12.0273 -2
0 2 19 659.694 12.0273 1
0 -2 -20 176.334 12.3196 -2
0 2 20 176.334 12.3196 1
0 2 -21 153.975 11.9433 -2
0 -2 21 153.975 11.9433 1
0 -2 -22 6.90459 2.99469 -2
0 2 22 6.90459 2.99469 1
0 -2 -23 1167.56 31.5051 -2
0 2 23 1167.56 31.5051 1
0 2 -24 333.216 17.9081 -2
0 -2 24 333.216 17.9081 1
0 2 -25 1196.37 33.0672 -2
0 -2 25 1196.37 33.0672 1
0 -2 -26 745.402 27.0015 -2
0 2 26 745.402 27.0015 1
0 -2 -27 606.749 25.0179 -2
0 2 27 606.749 25.0179 1
0 2 -28 4.19912 7.28377 -2
0 -2 28 4.19912 7.28377 1
0 2 -29 453.909 22.8267 -2
0 -2 29 453.909 22.8267 1
0 -2 -30 13.3664 6.11482 -2
0 2 30 13.3664 6.11482 1
0 2 -31 423.853 22.7778 -2
0 -2 31 423.853 22.7778 1
0 -3 1 4435.98 26.3555 -2
0 3 -1 4435.98 26.3555 1
0 -3 -2 1743.08 32.0555 -2
0 3 2 1743.08 32.0555 1
0 -3 -3 1478.08 6.39326 -2
0 3 3 1478.08 6.39326 1
0 -3 -4 32.0826 1.03311 -2
0 3 4 32.0826 1.03311 1
0 -3 -5 119.377 2.06555 -2
0 3 5 119.377 2.06555 1
0 -3 6 1142.43 6.63419 -2
0 3 -6 1142.43 6.63419 1
0 3 -7 1160.61 7.54004 -2
0 -3 7 1160.61 7.54004 1
0 -3 -8 1310.08 8.46421 -2
0 3 8 1310.08 8.46421 1
0 3 9 3404.47 15.1666 -2
0 -3 -9 3404.47 15.1666 1
0 3 -10 6365.70 25.4432 -2
0 -3 10 6365.70 25.4432 1
0 3 -11 3184.49 13.1759 -2
0 -3 11 3184.49 13.1759 1
0 3 12 15.4930 2.27455 -2
0 -3 -12 15.4930 2.27455 1
0 -3 13 364.362 6.35854 -2
0 3 -13 364.362 6.35854 1
0 3 -14 4778.88 28.9494 -2
0 -3 14 4778.88 28.9494 1
0 3 -15 4.70237 1.35387 -2
0 -3 15 4.70237 1.35387 1
0 3 16 1783.30 17.5240 -2
0 -3 -16 1783.30 17.5240 1
0 3 -17 710.495 13.6387 -2
0 -3 17 710.495 13.6387 1
0 3 18 2728.49 26.7107 -2
0 -3 -18 2728.49 26.7107 1
0 3 19 1265.38 24.3633 -2
0 -3 -19 1265.38 24.3633 1
0 3 -20 5.05408 4.70338 -2
0 -3 20 5.05408 4.70338 1
0 -3 -21-0.76921 4.80167 -2
0 3 21-0.76921 4.80167 1
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0 -3 22 2565.38 45.4615 1
0 3 -23 12.6541 6.05197 -2
0 -3 23 12.6541 6.05197 1
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0 -3 24 855.788 27.8147 1
0 3 -25-4.42333 4.89781 -2
0 -3 25-4.42333 4.89781 1
0 3 -26 97.9149 11.1480 -2
0 -3 26 97.9149 11.1480 1
0 3 -27 129.197 13.3088 -2
0 -3 27 129.197 13.3088 1
0 3 -28-5.56002 5.49138 -2
0 -3 28-5.56002 5.49138 1
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0 -3 29 228.953 16.8957 1
0 3 -30 275.282 18.2392 -2
0 -3 30 275.282 18.2392 1
0 -4 0 10666.7 55.3323 -2
0 4 0 10666.7 55.3323 1
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0 4 1 223.641 5.96391 1
0 -4 -2 934.299 16.8153 -2
0 4 2 934.299 16.8153 1
0 4 3 130.766 2.06586 -2
0 -4 -3 130.766 2.06586 1
0 -4 -4 3464.46 11.8239 -2
0 4 4 3464.46 11.8239 1
0 -4 -5 25.4298 1.52660 -2
0 4 5 25.4298 1.52660 1
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0 4 6 782.474 6.91305 1
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0 4 7 196.107 3.72827 1
0 -4 -8 5065.54 24.6127 -2
0 4 8 5065.54 24.6127 1
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0 -4 -9 913.657 5.80296 1
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0 -4 -10 37.7762 2.03618 1
0 -4 -11 241.460 4.49408 -2
0 4 11 241.460 4.49408 1
0 4 -12 106.154 5.10425 -2
0 -4 12 106.154 5.10425 1
0 4 13 16.6055 2.16055 -2
0 -4 -13 16.6055 2.16055 1
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0 -4 14 267.631 7.29795 1
0 -4 -15 866.195 12.9269 -2
0 4 15 866.195 12.9269 1
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0 -4 16 271.210 5.14789 1
0 -4 -17 291.455 8.96607 -2
0 4 17 291.455 8.96607 1
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0 4 18 106.136 5.94658 1
0 4 -19 488.648 19.3233 -2
0 -4 19 488.648 19.3233 1
0 4 -20 572.560 21.2614 -2
0 -4 20 572.560 21.2614 1
0 4 -21 12.6632 3.08649 -2
0 -4 21 12.6632 3.08649 1
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0 4 22 11.1467 3.89248 1
0 -4 -23 820.513 26.7779 -2
0 4 23 820.513 26.7779 1
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0 -4 24 77.5170 10.3671 1
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0 -4 28 1040.17 32.8324 1
0 -4 -29 187.963 15.6845 -2
0 4 29 187.963 15.6845 1
0 -4 -30 5.01811 4.58411 -2
0 4 30 5.01811 4.58411 1
0 -5 -1 242.721 6.87537 -2
0 5 1 242.721 6.87537 1
0 -5 -2 4109.84 38.6170 -2
0 5 2 4109.84 38.6170 1
0 -5 -3 131.145 7.67670 -2
0 5 3 131.145 7.67670 1
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0 -5 4 112.096 1.84279 1
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0 -5 5 799.754 4.74563 1
0 -5 -6 3055.95 9.44071 -2
0 5 6 3055.95 9.44071 1
0 -5 -7 190.352 4.20101 -2
0 5 7 190.352 4.20101 1
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0 -5 8 2178.34 14.0348 1
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0 -5 9 830.230 7.08749 1
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0 -5 10 1238.15 9.39895 1
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0 -5 11 139.392 3.88065 1
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0 5 14 519.021 12.9207 1
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0 -5 15 846.172 14.5164 1
0 -5 -16 2428.83 24.8095 -2
0 5 16 2428.83 24.8095 1
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0 5 17 410.967 12.0063 1
0 5 -18 414.536 12.4210 -2
0 -5 18 414.536 12.4210 1
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0 -5 19 541.218 14.3831 1
0 5 -20 13.8032 3.28853 -2
0 -5 20 13.8032 3.28853 1
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0 -5 22-6.28217 4.83195 1
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0 5 23 758.666 26.1642 1
0 5 -24 352.755 18.6666 -2
0 -5 24 352.755 18.6666 1
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0 -5 25 28.2934 7.47658 1
0 5 -26 141.293 13.3856 -2
0 -5 26 141.293 13.3856 1
0 5 -27 342.504 19.4035 -2
0 -5 27 342.504 19.4035 1
0 5 -28-1.15105 5.71734 -2
0 -5 28-1.15105 5.71734 1
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0 -5 30 67.0302 10.8493 1
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0 -6 0 1951.27 20.6613 1
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0 -6 -1 960.602 14.7130 1
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0 -6 -2 155.346 7.69893 1
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0 -6 -3 24.3566 4.29787 1
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0 -6 -4 4690.80 32.3404 1
0 6 -5 103.011 2.08234 -2
0 -6 5 103.011 2.08234 1
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0 -6 -6 185.019 2.69558 1
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0 -6 7 128.791 2.67212 1
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0 -6 8 998.787 6.68553 1
0 6 -9 1983.04 9.69894 -2
0 -6 9 1983.04 9.69894 1
0 -6 -10 142.751 2.80269 -2
0 6 10 142.751 2.80269 1
0 -6 -11 27.6296 1.95168 -2
0 6 11 27.6296 1.95168 1
0 6 -12 2516.07 17.2004 -2
0 -6 12 2516.07 17.2004 1
0 6 -13 17.8798 4.65219 -2
0 -6 13 17.8798 4.65219 1
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0 -6 14-1.21350 3.32580 1
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0 -6 16 49.6103 3.07764 1
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0 -6 18 1047.81 13.0596 1
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0 -6 20 485.758 14.1671 1
0 6 -21-0.05980 4.20164 -2
0 -6 21-0.05980 4.20164 1
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0 -6 22 132.025 9.20359 1
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0 -6 24 245.002 16.0754 1
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0 -6 26 809.011 28.1450 1
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0 -6 27-4.72530 5.85351 1
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2 -5 16 72.8837 9.81613 2
2 6 -20 63.3942 9.56337 2
2 6 -17 26.0532 6.49609 2
2 6 -15 7.82648 4.41884 2
2 6 -13 56.0459 6.10846 2
2 6 -12 0.39235 3.15710 2
2 6 -11 133.689 7.81617 2
2 6 -10 78.4002 4.17651 2
2 6 -9 30.7787 2.80893 2
-2 6 8 153.199 4.51131 2
2 6 -7 18.2086 2.31542 2
2 6 -6 283.882 5.98816 2
2 6 -5 179.175 3.94531 2
-2 6 4 26.2767 2.46477 2
-2 6 3 38.1344 5.79849 2
2 6 -2 187.788 7.04143 2
-2 -6 1 4.72263 4.28995 2
2 6 0 134.782 7.90400 2
-2 -6 -1 74.2420 4.16723 2
2 6 2 414.408 6.74455 2
-2 -6 -3 52.6397 2.63602 2
-2 -6 -4 23.8091 2.37968 2
-2 -6 -5 430.058 7.13283 2
-2 -6 -6 41.2596 3.04378 2
-2 -6 -7 3.20676 1.82447 2
-2 -6 -8 34.4293 3.20585 2
-2 -6 -9 27.3833 3.30232 2
2 7 -17 27.3101 7.56883 2
2 -7 -16-0.99417 3.50400 2
2 -7 -15 66.8856 7.59213 2
2 7 -14 122.025 6.12941 2
2 7 -13-2.87235 1.93362 2
2 7 -12 10.8635 2.51584 2
2 7 -11 60.6143 3.78244 2
2 7 -10 14.0130 2.18969 2
2 7 -9 52.8166 2.87121 2
2 7 -8 0.67550 1.34531 2
2 7 -7 178.103 4.02854 2
2 7 -6 6.98162 1.63294 2
2 7 -5 22.9687 1.55269 2
2 7 -4 16.2331 2.00807 2
2 -7 -2 0.81358 0.98111 2
2 7 0-1.67566 5.61766 2
-2 -7 -2 35.7254 1.76295 2
-2 -7 -3 20.6591 1.68838 2
2 7 4 8.92702 1.32364 2
2 7 5 267.787 4.76533 2
-2 -7 -6 3.93590 1.39851 2
-2 -7 -7 13.1181 1.88455 2
2 7 8 32.6684 2.52718 2
2 7 9 2.08881 1.86329 2
-2 -7 -10 74.4105 4.61732 2
-2 7 -11 3.90000 2.65919 2
2 7 12 5.43566 2.68578 2
2 -8 -13 296.614 11.2586 2
2 -8 -11-1.68631 1.71524 2
2 -8 -10 63.1787 3.05927 2
2 -8 -9 2.38915 1.44724 2
2 -8 -8 1.85558 1.15547 2
-2 -8 -5 96.6523 3.10667 2
-2 -8 -6 22.8489 2.55281 2
-2 -8 -7 60.4072 2.93869 2
-2 -8 -8 17.3438 2.18505 2
-2 -8 -9 58.5325 3.13301 2
-2 -8 -10 32.6342 4.46183 2
-2 -8 -13 122.612 8.84342 2
-2 -8 -14 2.95665 3.54665 2
-2 -8 -15 9.75528 4.25892 2
-2 -8 -16 0.58955 4.20149 2
3 0 -11 4.76012 2.95160 2
3 0 -7 23.7653 1.86729 2
3 0 -5 40.5513 4.42131 2
-3 0 3 44.9248 2.37697 2
3 0 -1 2.08857 2.27081 2
3 0 1 12.2367 1.99472 2
3 0 3 190.818 8.38814 2
3 0 5 11.9711 3.15074 2
3 0 7 70.0532 5.99669 2
3 -1 -10 1278.41 20.3473 2
-3 1 9 206.648 9.77404 2
3 -1 -8 1.70189 1.88289 2
3 1 -7 14.3506 1.93502 2
3 1 -6-0.13528 1.11541 2
3 1 -5 28.4393 2.01740 2
3 1 -4 0.55959 0.74825 2
-3 -1 3 223.999 2.79165 2
3 1 -2 463.989 5.28129 2
3 1 -1 257.393 4.00579 2
-3 1 0 519.204 4.62789 2
-3 1 -1 0.52742 1.18699 2
-3 1 -2 116.309 4.86295 2
-3 1 -3 99.1808 4.48707 2
3 1 4 77.0087 4.17954 2
3 1 5 40.3146 4.56706 2
3 1 7 190.149 9.19581 2
3 -2 -13 2.31121 1.74028 2
3 -2 -12 249.197 6.54459 2
3 -2 -11 78.9201 3.45873 2
-3 2 8 356.044 12.2135 2
3 2 -7 39.4960 2.31851 2
3 2 -6 287.703 3.97906 2
3 2 -5 19.7107 1.36563 2
3 2 -4 563.945 4.98283 2
3 2 -3 456.730 4.40838 2
3 2 -2 392.458 4.10035 2
3 2 -1 0.35577 0.78857 2
-3 -2 0 154.121 2.70718 2
-3 -2 -1 10.5041 1.16348 2
-3 -2 -2 271.159 3.80675 2
-3 -2 -3 87.2169 2.71623 2
-3 2 -4 500.017 5.18700 2
3 2 5 379.192 12.0583 2
3 2 6 258.351 10.4847 2
3 3 -13 78.1853 7.71111 2
3 3 -12 99.3900 8.36213 2
3 -3 -8 18.5136 3.52437 2
3 -3 -7 4.58166 2.46846 2
-3 3 6 181.442 4.90093 2
-3 3 5 118.135 4.10883 2
3 3 -4 32.1435 2.01891 2
3 -3 -3 22.2775 1.57589 2
3 3 -2 1.77605 0.82674 2
3 -3 -1 195.029 3.01817 2
3 3 0 15.4827 1.16478 2
-3 -3 -1 0.75798 1.12240 2
-3 -3 -2 123.484 3.64927 2
3 -3 3 10.7333 1.92355 2
3 -3 4 33.6036 4.40904 2
3 4 -17 77.3220 8.98542 2
-3 4 7 21.9154 3.37004 2
-3 4 6 7.50209 2.18006 2
-3 4 5 17.4229 3.30305 2
3 -4 -3 59.3183 4.22391 2
3 -4 -2 138.264 5.83572 2
3 -4 -1 3.26092 1.50178 2
-3 4 0 1639.93 19.7666 2
3 -4 1 126.870 3.94695 2
3 -4 2 81.2359 3.64176 2
-3 4 -3 113.006 7.68933 2
-3 4 -10 190.891 5.24261 2
-3 4 -11 51.9142 2.90216 2
-3 5 8 68.4071 5.81167 2
-3 5 7 262.237 10.7324 2
-3 5 6 249.897 10.4337 2
-3 5 5 14.1502 3.54592 2
3 6 -26 31.3684 10.1055 2
4 0 -30-3.52888 5.46927 2
4 0 -28 72.1363 7.71362 2
4 0 -26-1.24356 4.78891 2
4 0 -24 373.684 8.42929 2
4 0 -22 216.501 6.53937 2
4 0 -20 0.57498 2.49255 2
4 0 -18 0.65989 2.43769 2
4 0 -16 56.7082 4.72558 2
-4 0 14 1044.21 9.81680 2
-4 0 12 203.075 5.27837 2
-4 0 10 68.4244 4.09169 2
-4 0 8 671.009 10.0872 2
4 0 -6 1086.05 13.0603 2
-4 0 4 1333.77 8.95145 2
4 0 -2 785.563 9.03539 2
4 0 0 3174.62 19.3505 2
4 0 2 129.078 5.66441 2
4 0 4 1150.65 20.9383 2
4 0 6 846.556 17.9945 2
4 0 8 1596.81 25.5984 2
4 0 10 67.7498 4.52999 2
-4 0 -12 210.619 7.20485 2
-4 0 -14 539.371 16.2717 2
-4 0 -16 183.776 10.1747 2
-4 0 -18 123.719 9.07393 2
-4 0 -20 19.0586 2.87152 2
-4 0 -22 81.0373 8.00839 2
-4 0 -24 39.6157 6.58383 2
-4 0 -26 31.4479 6.36077 2
6 0 -28 175.983 11.6707 2
6 0 -26 34.5470 4.79134 2
6 0 -24 8.50159 3.93253 2
6 0 -22 87.0323 8.70728 2
6 0 -20 339.368 14.6141 2
6 0 -18 391.875 15.2344 2
-6 0 16-2.74702 2.68786 2
-6 0 14 221.716 13.2498 2
-6 0 12 234.708 12.9473 2
-6 0 10 1322.59 27.4524 2
-6 0 8 174.975 11.1639 2
-6 0 6 49.0128 3.22809 2
6 0 -4 2.12254 1.79735 2
6 0 -2 837.456 14.6149 2
6 0 0 579.461 11.9229 2
-6 0 -2 53.9834 3.38360 2
-6 0 -4 186.521 5.88943 2
-6 0 -6 44.1652 3.47607 2
-6 0 -8 251.253 5.79013 2
-6 0 -10 244.741 5.08176 2
-6 0 -12 61.1987 4.08372 2
-6 0 -14 15.9338 3.25466 2
-6 0 -16-1.29554 6.43937 2
-6 0 -18 109.498 10.7162 2
-6 0 -20-6.48118 5.76176 2
-6 0 -22 24.4557 8.15598 2
6 -1 -10 206.921 6.46249 2
-6 1 6 216.056 6.04293 2
-6 1 5 179.734 6.44779 2
-6 2 -1 87.3633 3.06404 2
-7 0 5 38.8600 4.29626 2
-7 0 3 113.599 7.27965 2
-7 0 -5 76.1108 4.77125 2
7 1 -14 75.2275 5.71129 2
7 1 -13 8.52521 2.93835 2
7 1 -12 47.4923 3.69949 2
7 1 -11 92.6356 4.49886 2
7 1 -10 107.351 3.88773 2
-7 1 6 0.19152 1.76270 2
-7 1 5 31.6342 2.76557 2
-7 -1 4 197.310 9.64769 2
-7 -1 3 148.683 8.73191 2
-7 -1 2 100.989 7.90769 2
-7 -1 1 10.2177 4.06210 2
-7 -1 0 32.3831 5.34024 2
-7 -1 -3 45.9083 3.48070 2
-7 -1 -4 253.797 8.20070 2
-7 -1 -5 34.1203 4.25123 2
-7 -1 -6 33.6074 4.51137 2
-7 -1 -7 10.6454 3.71692 2
-7 1 -20 67.4219 14.8560 2
7 2 -15-0.85588 3.16888 2
7 2 -14 4.70696 3.10879 2
7 2 -13 7.80928 3.24867 2
7 2 -12 117.896 6.99884 2
7 2 -11 13.0534 3.50013 2
7 2 -10 42.4774 4.15985 2
7 2 -9 185.913 7.13268 2
-7 2 6 14.8354 2.18501 2
-7 -2 4 52.8762 6.23151 2
-7 -2 3 9.01034 3.90079 2
-7 -2 2 149.492 9.92946 2
-7 -2 1 62.1990 6.89780 2
-7 -2 0 77.9990 7.88669 2
-7 -2 -1 0.61240 3.76571 2
-7 -2 -2 3.89907 2.43956 2
-7 -2 -3 44.9880 3.52425 2
-7 -2 -4 5.07588 1.87345 2
-7 2 -5 36.0814 3.01971 2
-7 -2 -6 118.522 7.95137 2
-7 -2 -7 4.71963 3.68162 2
-7 -2 -8-1.88457 3.54758 2
-7 -2 -9-0.50459 3.73156 2
-7 -2 -10 40.0593 6.58801 2
7 3 -25 27.2503 7.35177 2
7 3 -24 13.3805 6.70620 2
7 3 -23 12.0887 5.41578 2
7 3 -22 2.91948 5.82918 2
7 3 -21 35.1229 10.0751 2
7 3 -20 39.9081 9.49631 2
7 3 -19 57.4281 9.80443 2
7 3 -18 20.6871 4.66632 2
-7 -3 3 18.3029 4.90762 2
-7 -3 2 81.1926 8.06160 2
-7 -3 1 15.0240 4.67214 2
-7 -3 -2 11.6661 3.83144 2
-7 -3 -3 3.01233 1.84092 2
-7 -3 -4 17.2430 2.52006 2
-7 3 -5 5.07892 2.31290 2
-7 3 -6 20.4710 3.12764 2
-7 3 -7 93.0892 5.20394 2
-7 -3 -8 55.7242 6.96526 2
-7 -3 -9 45.3708 6.97006 2
-7 -3 -10 6.65288 4.66914 2
7 4 -24 37.3614 12.5502 2
7 4 -23 28.7701 6.96966 2
7 4 -22 70.6592 9.03836 2
7 4 -21 3.04593 5.03961 2
7 4 -20 20.7383 4.39569 2
7 4 -19 7.81217 3.86783 2
7 4 -18 0.55659 3.28033 2
7 4 -17 32.4021 6.56772 2
-7 -4 16 17.0539 4.32157 2
-7 -4 15 16.9965 4.33942 2
7 4 -14 413.893 12.9398 2
7 4 -13 60.3885 5.56905 2
7 4 -12 10.7123 3.29469 2
7 4 -11 13.9561 3.30524 2
7 4 -10 12.0514 3.24333 2
7 4 -9 41.0767 4.65770 2
7 4 -8 86.0474 6.41166 2
-7 4 7 1.48572 1.29618 2
-7 -4 6 392.700 19.6719 2
-7 4 -2 31.1308 4.29614 2
-7 4 -3 106.636 6.78679 2
-7 4 -4 16.2017 3.73801 2
-7 4 -5 14.1836 4.01399 2
-7 4 -8 259.606 13.1322 2
-7 -4 -9 16.8759 5.08650 2
-7 -4 -10 25.6835 8.11697 2
-7 -4 -11 62.6885 11.0236 2
-7 -4 -12 11.1329 8.39495 2
-7 -4 -13-2.08450 7.05820 2
-7 -4 -14 42.8500 10.1465 2
-7 -4 -15-2.19021 7.16880 2
-7 -4 -16 31.7698 14.0091 2
-7 -4 -17 75.3323 14.6730 2
-7 -4 -18 80.4791 14.2946 2
-7 4 -19-1.27991 9.47109 2
7 5 -23 87.0183 14.9726 2
7 5 -22 42.9645 13.5414 2
7 5 -21 79.8080 10.6830 2
7 5 -20 50.0515 6.48487 2
7 5 -19-3.87846 3.22529 2
7 5 -18 70.1894 6.49391 2
7 5 -17 20.5017 4.62198 2
7 5 -16 6.19139 3.56482 2
-7 -5 15-1.07332 3.36956 2
-7 -5 14 147.221 8.78901 2
7 5 -13 104.116 7.90655 2
7 5 -12 45.5298 5.72901 2
7 5 -11 56.6522 5.20036 2
7 5 -10 150.560 7.49724 2
7 5 -9 68.5771 6.84666 2
-7 -5 8 130.473 7.89143 2
-7 5 7 72.6538 5.52614 2
-7 5 6 56.4197 10.6961 2
-7 -5 5 149.447 15.1369 2
-7 -5 4 110.047 11.8992 2
7 -5 -3 92.7158 8.55817 2
7 -5 -2 45.9530 4.47387 2
7 -5 -1 16.5318 3.78947 2
-7 -5 -8 199.993 17.0434 2
-7 -5 -9 2.70726 8.35621 2
-7 -5 -10-1.84473 4.41662 2
-7 -5 -11 17.2338 7.21666 2
-7 -5 -12 72.4204 12.1697 2
-7 -5 -13 7.15866 9.18734 2
-7 -5 -14-2.11292 5.27220 2
-7 -5 -15 169.887 16.4466 2
-7 -5 -16 62.7642 13.1380 2
-7 -5 -17 116.932 17.0802 2
-7 -5 -18 17.8394 12.9421 2
7 6 -23 19.3205 12.3440 2
7 6 -22 20.5694 9.78517 2
7 6 -21 22.7060 10.3282 2
7 6 -20 25.6236 8.72892 2
7 6 -19 136.935 15.4258 2
7 6 -18 59.8272 7.70885 2
7 6 -17 259.285 10.7126 2
7 6 -16 72.1721 6.81665 2
7 6 -15 49.1638 5.54234 2
-7 6 7 3.97035 2.98589 2
-7 6 6 33.1786 4.72311 2
-7 7 5 52.1927 6.69813 2
-8 0 -6 165.717 6.25509 2
-8 1 6 18.0435 3.11287 2
-8 1 5 43.4816 4.39460 2
-8 1 4 148.482 7.74785 2
-8 -1 -5 40.6305 3.78118 2
-8 2 5 217.758 7.54531 2
-8 2 -6 25.4148 3.15090 2
-8 2 -7 222.256 8.35756 2
-8 3 6 37.7936 2.73103 2
-8 3 -5 2.73673 2.08313 2
-8 3 -6 2.63232 2.60460 2
-8 3 -7 54.8865 5.19505 2
9 0 -25 2.81066 5.17402 2
9 0 -23-4.38616 4.09705 2
9 0 -21-3.31054 4.46770 2
9 0 -19 3.31034 4.70412 2
9 0 -17 3.31575 3.22981 2
-9 0 15 53.0926 8.09111 2
-9 0 13 10.7114 6.50671 2
-9 0 11 1.03041 6.53647 2
-9 0 9-4.29182 5.33932 2
-9 0 7 62.2060 10.6919 2
-9 0 5 80.0736 9.72574 2
-9 0 3-4.34416 4.99695 2
-9 0 1-11.9499 4.49108 2
-9 0 -1 75.6409 9.84193 2
-9 0 -3 42.4727 9.19538 2
-9 0 -5 47.7875 8.77368 2
-9 0 -7-1.40357 5.71803 2
-9 0 -9 1.19995 6.14348 2
-9 0 -11 0.74254 5.41009 2
0 0 0 0.00000 0.00000 0
TITL shS_497_IlGu_twin1_hklf4 in P2(1)/n
REM P2(1)/n (#14 in standard setting)
CELL 0.71073 8.143060 8.836231 25.178678 90.0000 97.2640 90.0000
ZERR 8.00 0.000197 0.000208 0.000717 0.0000 0.0023 0.0000
LATT 1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC C H N Ge I
UNIT 32.00 112.00 16.00 8.00 48.00
REM CrysAlisPro recorded range (K): Min=100.0; max=100.1; aver:100.0
TEMP -173
TREF
HKLF 5
BASF 0.24487
END
;
_shelx_hkl_checksum 28687
_shelx_res_file
;
TITL shS_497_IlGu_twin1_hklf4 in P21/n #14
shs_497_ilgu_twin1_hklf4.res
created by SHELXL-2018/3 at 14:05:38 on 04-Oct-2024
CELL 0.71073 8.14306 8.836231 25.178678 90 97.264 90
ZERR 4 0.000197 0.000208 0.000717 0 0.0023 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Ge I N
UNIT 16 56 4 24 8
EQIV $1 1.5-X,0.5+Y,1.5-Z
EQIV $2 1.5-X,-0.5+Y,1.5-Z
EQIV $3 2.5-X,-0.5+Y,1.5-Z
EQIV $4 +X,-1+Y,+Z
L.S. 4 0 0
PLAN 16
TEMP -173
CONF
HTAB N1 I2_$1
HTAB N1 I3
HTAB N1 I4_$2
HTAB N2 I3_$2
HTAB N2 I1
HTAB N2 I4_$3
HTAB C4 I1_$4
BIND I4 Ge1
BOND
MORE -1
BOND $H
fmap 2 53
acta
OMIT -8 2 -7
OMIT -7 -7 1
OMIT -7 -7 3
OMIT 1 -5 -2
REM
REM
REM
WGHT 0.021500 42.683598
BASF 0.15043
FVAR 0.20580
I2 4 1.224176 0.351275 0.769792 11.00000 0.01379 0.01415 =
0.01971 -0.00163 0.00002 0.00441
I3 4 0.721098 0.411536 0.763961 11.00000 0.01307 0.01533 =
0.02133 0.00069 0.00231 -0.00384
I1 4 0.958900 0.553345 0.639109 11.00000 0.02331 0.01322 =
0.01400 0.00011 0.00062 0.00101
I4 4 1.066539 0.655498 0.876885 11.00000 0.01924 0.01725 =
0.01547 -0.00085 0.00118 -0.00015
I6 4 0.776653 -0.099242 0.515645 11.00000 0.02440 0.02005 =
0.01703 -0.00217 0.00193 -0.00364
I5 4 0.250371 0.564755 0.514477 11.00000 0.02229 0.02966 =
0.01974 -0.00354 -0.00154 -0.00092
GE1 3 0.997254 0.588427 0.754557 11.00000 0.01119 0.01008 =
0.01720 0.00022 0.00160 -0.00001
N1 5 0.444867 0.552058 0.644397 11.00000 0.05568 0.02869 =
0.01901 0.00039 -0.00300 0.01140
AFIX 137
H1A 2 0.423703 0.465891 0.624939 11.00000 -1.20000
H1B 2 0.352259 0.580595 0.658589 11.00000 -1.20000
H1C 2 0.528452 0.534821 0.671279 11.00000 -1.20000
AFIX 0
C3 1 0.915666 0.124324 0.600022 11.00000 0.01563 0.01704 =
0.01650 -0.00806 0.00415 -0.00146
AFIX 23
H3A 2 0.957632 0.183196 0.571113 11.00000 -1.20000
H3B 2 0.798169 0.151794 0.600885 11.00000 -1.20000
AFIX 0
N2 5 1.013472 0.162133 0.652280 11.00000 0.02511 0.01487 =
0.01987 0.00178 0.00141 0.00157
AFIX 137
H2A 2 1.123115 0.148652 0.649940 11.00000 -1.20000
H2B 2 0.982275 0.100583 0.678197 11.00000 -1.20000
H2C 2 0.994867 0.260296 0.660675 11.00000 -1.20000
AFIX 0
C2 1 0.352126 0.731234 0.571881 11.00000 0.02378 0.01734 =
0.02181 -0.00045 -0.00355 -0.00195
AFIX 23
H2D 2 0.388261 0.820189 0.552453 11.00000 -1.20000
H2E 2 0.264226 0.765182 0.592961 11.00000 -1.20000
AFIX 0
C4 1 0.928923 -0.042055 0.588829 11.00000 0.02982 0.01496 =
0.02535 0.00238 0.00069 -0.00098
AFIX 23
H4A 2 0.893086 -0.100939 0.618776 11.00000 -1.20000
H4B 2 1.045603 -0.068378 0.585890 11.00000 -1.20000
AFIX 0
C1 1 0.494225 0.674470 0.609054 11.00000 0.02125 0.01386 =
0.03504 -0.00834 -0.00639 -0.00124
AFIX 23
H1D 2 0.543005 0.759248 0.631442 11.00000 -1.20000
H1E 2 0.580109 0.635510 0.588073 11.00000 -1.20000
AFIX 0
HKLF 5
REM shS_497_IlGu_twin1_hklf4 in P21/n #14
REM wR2 = 0.0917, GooF = S = 1.189, Restrained GooF = 1.189 for all data
REM R1 = 0.0352 for 4967 Fo > 4sig(Fo) and 0.0421 for all 5413 data
REM 121 parameters refined using 0 restraints
END
WGHT 0.0215 42.6753
REM Highest difference peak 1.213, deepest hole -1.271, 1-sigma level 0.312
Q1 1 0.4166 0.5451 0.6580 11.00000 0.05 1.21
Q2 1 0.8730 0.5571 0.6186 11.00000 0.05 1.21
Q3 1 1.1283 0.4081 0.7577 11.00000 0.05 1.15
Q4 1 0.7813 0.4534 0.7402 11.00000 0.05 1.13
Q5 1 0.7592 0.3179 0.7612 11.00000 0.05 1.11
Q6 1 1.0078 0.4556 0.6365 11.00000 0.05 1.11
Q7 1 0.9825 0.3955 0.7562 11.00000 0.05 1.09
Q8 1 0.8047 0.4804 0.7755 11.00000 0.05 1.09
Q9 1 0.9585 -0.2469 0.6407 11.00000 0.05 1.08
Q10 1 0.5003 0.7227 0.5218 11.00000 0.05 1.07
Q11 1 1.0578 -0.0982 0.5172 11.00000 0.05 1.06
Q12 1 0.7629 -0.1203 0.6188 11.00000 0.05 1.05
Q13 1 0.9153 -0.1122 0.5171 11.00000 0.05 1.03
Q14 1 0.9798 0.4956 0.6194 11.00000 0.05 1.02
Q15 1 0.8968 0.0305 0.5992 11.00000 0.05 1.00
Q16 1 0.4233 0.7435 0.6013 11.00000 0.05 1.00
;
_shelx_res_checksum 63160
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
I I2 1.22418(8) 0.35127(7) 0.76979(3) 0.01606(14) Uani d 1 . .
I I3 0.72110(8) 0.41154(7) 0.76396(3) 0.01657(14) Uani d 1 . .
I I1 0.95890(8) 0.55334(7) 0.63911(3) 0.01699(14) Uani d 1 . .
I I4 1.06654(8) 0.65550(7) 0.87689(3) 0.01740(14) Uani d 1 . .
I I6 0.77665(9) -0.09924(8) 0.51564(3) 0.02055(15) Uani d 1 . .
I I5 0.25037(9) 0.56475(9) 0.51448(3) 0.02426(16) Uani d 1 . .
Ge Ge1 0.99725(12) 0.58843(11) 0.75456(4) 0.0128(2) Uani d 1 . .
N N1 0.4449(15) 0.5521(12) 0.6444(4) 0.035(3) Uani d 1 . .
H H1A 0.423703 0.465891 0.624939 0.042 Uiso calc 1 . .
H H1B 0.352259 0.580595 0.658589 0.042 Uiso calc 1 . .
H H1C 0.528452 0.534821 0.671279 0.042 Uiso calc 1 . .
C C3 0.9157(12) 0.1243(11) 0.6000(4) 0.016(2) Uani d 1 . .
H H3A 0.957632 0.183196 0.571113 0.019 Uiso calc 1 . .
H H3B 0.798169 0.151794 0.600885 0.019 Uiso calc 1 . .
N N2 1.0135(11) 0.1621(10) 0.6523(4) 0.0201(19) Uani d 1 . .
H H2A 1.123115 0.148652 0.649940 0.024 Uiso calc 1 . .
H H2B 0.982275 0.100583 0.678197 0.024 Uiso calc 1 . .
H H2C 0.994867 0.260296 0.660675 0.024 Uiso calc 1 . .
C C2 0.3521(13) 0.7312(12) 0.5719(5) 0.022(2) Uani d 1 . .
H H2D 0.388261 0.820189 0.552453 0.026 Uiso calc 1 . .
H H2E 0.264226 0.765182 0.592961 0.026 Uiso calc 1 . .
C C4 0.9289(15) -0.0421(12) 0.5888(5) 0.024(2) Uani d 1 . .
H H4A 0.893086 -0.100939 0.618776 0.028 Uiso calc 1 . .
H H4B 1.045603 -0.068378 0.585890 0.028 Uiso calc 1 . .
C C1 0.4942(13) 0.6745(12) 0.6091(5) 0.024(2) Uani d 1 . .
H H1D 0.543005 0.759248 0.631442 0.029 Uiso calc 1 . .
H H1E 0.580109 0.635510 0.588073 0.029 Uiso calc 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
I2 0.0138(3) 0.0141(3) 0.0197(3) 0.0044(2) 0.0000(2) -0.0016(2)
I3 0.0131(3) 0.0153(3) 0.0213(3) -0.0038(2) 0.0023(2) 0.0007(2)
I1 0.0233(3) 0.0132(3) 0.0140(3) 0.0010(2) 0.0006(3) 0.0001(2)
I4 0.0192(3) 0.0172(3) 0.0155(3) -0.0001(3) 0.0012(3) -0.0008(2)
I6 0.0244(3) 0.0201(3) 0.0170(3) -0.0036(3) 0.0019(3) -0.0022(3)
I5 0.0223(3) 0.0297(4) 0.0197(4) -0.0009(3) -0.0015(3) -0.0035(3)
Ge1 0.0112(4) 0.0101(4) 0.0172(5) 0.0000(4) 0.0016(4) 0.0002(4)
N1 0.056(7) 0.029(5) 0.019(5) 0.011(5) -0.003(5) 0.000(4)
C3 0.016(4) 0.017(5) 0.016(5) -0.001(4) 0.004(4) -0.008(4)
N2 0.025(5) 0.015(4) 0.020(5) 0.002(3) 0.001(4) 0.002(3)
C2 0.024(5) 0.017(5) 0.022(6) -0.002(4) -0.004(4) 0.000(4)
C4 0.030(6) 0.015(5) 0.025(6) -0.001(4) 0.001(5) 0.002(4)
C1 0.021(5) 0.014(5) 0.035(7) -0.001(4) -0.006(5) -0.008(5)
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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0054
0 0 1 0.0083
1 2 -2 0.0404
2 1 0 0.0476
0 1 -1 0.0429
-3 11 -14 0.0406
-8 -8 4 0.0339
3 -11 14 0.0367
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
I2 Ge1 I1 . . 92.47(4) ?
I2 Ge1 I4 . . 88.45(3) ?
I3 Ge1 I2 . . 95.46(4) ?
I3 Ge1 I1 . . 92.27(3) ?
I3 Ge1 I4 . . 94.03(4) ?
I1 Ge1 I4 . . 173.52(4) ?
H1A N1 H1B . . 109.5 ?
H1A N1 H1C . . 109.5 ?
H1B N1 H1C . . 109.5 ?
C1 N1 H1A . . 109.5 ?
C1 N1 H1B . . 109.5 ?
C1 N1 H1C . . 109.5 ?
H3A C3 H3B . . 108.2 ?
N2 C3 H3A . . 109.7 ?
N2 C3 H3B . . 109.7 ?
N2 C3 C4 . . 110.0(9) ?
C4 C3 H3A . . 109.7 ?
C4 C3 H3B . . 109.7 ?
C3 N2 H2A . . 109.5 ?
C3 N2 H2B . . 109.5 ?
C3 N2 H2C . . 109.5 ?
H2A N2 H2B . . 109.5 ?
H2A N2 H2C . . 109.5 ?
H2B N2 H2C . . 109.5 ?
I5 C2 H2D . . 108.9 ?
I5 C2 H2E . . 108.9 ?
H2D C2 H2E . . 107.7 ?
C1 C2 I5 . . 113.4(7) ?
C1 C2 H2D . . 108.9 ?
C1 C2 H2E . . 108.9 ?
I6 C4 H4A . . 109.6 ?
I6 C4 H4B . . 109.6 ?
C3 C4 I6 . . 110.1(7) ?
C3 C4 H4A . . 109.6 ?
C3 C4 H4B . . 109.6 ?
H4A C4 H4B . . 108.2 ?
N1 C1 H1D . . 109.2 ?
N1 C1 H1E . . 109.2 ?
C2 C1 N1 . . 112.1(9) ?
C2 C1 H1D . . 109.2 ?
C2 C1 H1E . . 109.2 ?
H1D C1 H1E . . 107.9 ?
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
I2 Ge1 . 2.7881(11) ?
I3 Ge1 . 2.7732(12) ?
I1 Ge1 . 2.9006(12) ?
I4 Ge1 . 3.1172(12) ?
I6 C4 . 2.147(11) ?
I5 C2 . 2.153(10) ?
N1 H1A . 0.9100 ?
N1 H1B . 0.9100 ?
N1 H1C . 0.9100 ?
N1 C1 . 1.488(16) ?
C3 H3A . 0.9900 ?
C3 H3B . 0.9900 ?
C3 N2 . 1.487(13) ?
C3 C4 . 1.503(14) ?
N2 H2A . 0.9100 ?
N2 H2B . 0.9100 ?
N2 H2C . 0.9100 ?
C2 H2D . 0.9900 ?
C2 H2E . 0.9900 ?
C2 C1 . 1.481(14) ?
C4 H4A . 0.9900 ?
C4 H4B . 0.9900 ?
C1 H1D . 0.9900 ?
C1 H1E . 0.9900 ?
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 I4 2_646 0.91 2.74 3.544(11) 147.3 yes
N1 H1B I2 2_656 0.91 3.11 3.782(11) 132.7 yes
N1 H1C I3 . 0.91 2.86 3.735(10) 162.3 yes
N2 H2A I4 2_746 0.91 2.70 3.588(9) 166.2 yes
N2 H2B I3 2_646 0.91 2.87 3.744(9) 160.3 yes
N2 H2C I1 . 0.91 2.65 3.496(9) 154.1 yes
C4 H4A I1 1_545 0.99 3.13 3.790(10) 125.2 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
I5 C2 C1 N1 . . . . -65.4(11) ?
N2 C3 C4 I6 . . . . 176.7(7) ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.8496(7)
2 0.1504(7)