#------------------------------------------------------------------------------
#$Date: 2024-12-07 18:01:47 +0100 (Sat, 07 Dec 2024) $
#$Revision: 296751 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023308.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_2023308
loop_
_publ_author_name
'Czapla, Zbigniew'
'Krawczyk, Monika K.'
'Kinzhybalo, Vasyl'
_publ_section_title
;
Atypical phase transition, twinning and ferroelastic domain structure in
bis(ethylenediammonium) tetrabromozincate(II) bromide,
[NH3(CH2)2NH3]2[ZnBr4]Br2.
;
_journal_coeditor_code XK5110
_journal_issue 6
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first 738
_journal_page_last 745
_journal_paper_doi 10.1107/S2052520624009740
_journal_volume 80
_journal_year 2024
_chemical_formula_moiety 'Br4 Zn, 2(C2 H10 N2), 2Br'
_chemical_formula_sum 'C4 H20 Br6 N4 Zn'
_chemical_formula_weight 669.07
_space_group_crystal_system monoclinic
_space_group_IT_number 11
_space_group_name_Hall '-P 2yb'
_space_group_name_H-M_alt 'P 1 21/m 1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2014/7
_cell_angle_alpha 90
_cell_angle_beta 93.16(3)
_cell_angle_gamma 90
_cell_formula_units_Z 2
_cell_length_a 6.438(3)
_cell_length_b 19.945(6)
_cell_length_c 6.726(3)
_cell_measurement_reflns_used 1964
_cell_measurement_temperature 290(2)
_cell_measurement_theta_max 28.0860
_cell_measurement_theta_min 3.0410
_cell_volume 862.3(6)
_computing_cell_refinement 'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection 'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction 'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature 290(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.864
_diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0416
_diffrn_reflns_av_unetI/netI 0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -5
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_l_max 8
_diffrn_reflns_limit_l_min -6
_diffrn_reflns_number 3952
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full 25.500
_diffrn_reflns_theta_max 28.961
_diffrn_reflns_theta_min 3.169
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 15.306
_exptl_absorpt_correction_T_max 0.315
_exptl_absorpt_correction_T_min 0.126
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 2.577
_exptl_crystal_description plate
_exptl_crystal_F_000 624
_exptl_crystal_size_max 0.240
_exptl_crystal_size_mid 0.200
_exptl_crystal_size_min 0.100
_refine_diff_density_max 0.839
_refine_diff_density_min -0.868
_refine_diff_density_rms 0.205
_refine_ls_extinction_coef 0.0041(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref 0.997
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 76
_refine_ls_number_reflns 2031
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 0.997
_refine_ls_R_factor_all 0.0680
_refine_ls_R_factor_gt 0.0421
_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^)+(0.0144P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0567
_refine_ls_wR_factor_ref 0.0638
_reflns_Friedel_coverage 0.000
_reflns_number_gt 1526
_reflns_number_total 2031
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file xk5110sup1.cif
_cod_data_source_block 290K
_cod_depositor_comments
'Adding full bibliography for 2023307--2023308.cif.'
_cod_original_sg_symbol_H-M 'P 21/m'
_cod_database_code 2023308
_cod_database_fobs_code 2023308
_shelx_shelxl_version_number 2014/7
_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 0.120
_shelx_estimated_absorpt_t_max 0.310
_shelx_res_file
;
enzn290bb.res created by SHELXL-2014/7
TITL enznbr.res in P2(1)/m
CELL 0.71073 6.438 19.945 6.726 90.0 93.16 90.0
ZERR 2 0.003 0.006 0.003 0.0 0.03 0.0
LATT 1
SYMM -X,0.5+Y,-Z
SFAC C H N Zn Br
UNIT 8 40 8 2 12
EQIV $1 1-X,1-Y,1-Z
EQIV $2 1-X,1-Y,2-Z
EQIV $3 -1+X,+Y,+Z
EQIV $4 +X,+Y,1+Z
EQIV $5 -1+X,0.5-Y,1+Z
EQIV $6 -1+X,0.5-Y,+Z
L.S. 10
PLAN 20
SIZE 0.24 0.20 0.10
TEMP 17
HTAB N1 Br4
HTAB N1 Br4_$1
HTAB N1 Br4_$2
HTAB N1 Br4_$3
HTAB N2 Br3
HTAB N2 Br1_$4
HTAB N2 Br4
HTAB N2 Br4_$1
HTAB C1 Br2_$5
HTAB C2 Br2_$6
HTAB C2 Br4_$3
CONF
BOND $H
HTAB 2.1
fmap 2 53
acta 51
OMIT -1 4 3
OMIT 0 1 1
OMIT 0 0 1
OMIT -1 0 1
OMIT 1 0 1
WGHT 0.014400
EXTI 0.004055
FVAR 3.52252
BR1 5 0.711903 0.250000 -0.269370 10.50000 0.04736 0.04964 =
0.02447 0.00000 0.00548 0.00000
BR2 5 0.796058 0.144138 0.217953 11.00000 0.04163 0.02732 =
0.04167 0.00657 0.00447 0.00623
BR3 5 0.300465 0.250000 0.142726 10.50000 0.02800 0.03269 =
0.03536 0.00000 0.00310 0.00000
BR4 5 0.730171 0.488471 0.701257 11.00000 0.02594 0.03878 =
0.02736 0.00039 -0.00159 0.00042
ZN1 4 0.675747 0.250000 0.086725 10.50000 0.03156 0.02336 =
0.02582 0.00000 0.00282 0.00000
N1 3 0.233964 0.472455 0.811970 11.00000 0.02790 0.04060 =
0.02796 -0.00403 0.00241 0.00059
AFIX 137
H1A 2 0.333805 0.485597 0.734261 11.00000 -1.20000
H1B 2 0.249141 0.493316 0.928841 11.00000 -1.20000
H1C 2 0.110328 0.482555 0.753969 11.00000 -1.20000
AFIX 0
N2 3 0.371515 0.362582 0.513517 11.00000 0.06211 0.03225 =
0.03161 -0.00462 0.00865 0.00511
AFIX 137
H2A 2 0.345686 0.333565 0.414708 11.00000 -1.20000
H2B 2 0.492361 0.352452 0.577055 11.00000 -1.20000
H2C 2 0.377733 0.403882 0.464093 11.00000 -1.20000
AFIX 0
C1 1 0.248334 0.398911 0.843388 11.00000 0.03701 0.03217 =
0.03128 0.00735 0.00609 0.00348
AFIX 23
H1D 2 0.150326 0.385786 0.940734 11.00000 -1.20000
H1E 2 0.386955 0.387947 0.897493 11.00000 -1.20000
AFIX 0
C2 1 0.203617 0.359013 0.653984 11.00000 0.03959 0.03234 =
0.04058 -0.00313 0.00507 -0.00712
AFIX 23
H2D 2 0.181566 0.312459 0.688831 11.00000 -1.20000
H2E 2 0.075930 0.375530 0.588025 11.00000 -1.20000
AFIX 0
HKLF 4
REM enznbr.res in P2(1)/m
REM R1 = 0.0421 for 1526 Fo > 4sig(Fo) and 0.0680 for all 2031 data
REM 76 parameters refined using 0 restraints
END
WGHT 0.0144 0.0000
REM Instructions for potential hydrogen bonds
HTAB N1 Br4
HTAB N1 Br4_$1
HTAB N1 Br4_$2
HTAB N1 Br4_$3
HTAB N2 Br3
HTAB N2 Br1_$4
HTAB N2 Br4
HTAB N2 Br4_$1
HTAB C1 Br2_$5
HTAB C2 Br2_$6
REM Highest difference peak 0.839, deepest hole -0.868, 1-sigma level 0.205
Q1 1 0.4954 0.2500 0.1167 10.50000 0.05 0.84
Q2 1 0.5623 0.2500 -0.2582 10.50000 0.05 0.84
Q3 1 0.5379 0.4806 0.6949 11.00000 0.05 0.78
Q4 1 0.0396 0.4425 0.4711 11.00000 0.05 0.76
Q5 1 0.9596 0.1455 0.2058 11.00000 0.05 0.69
Q6 1 0.8362 0.1428 0.0731 11.00000 0.05 0.66
Q7 1 0.0437 0.5403 0.9627 11.00000 0.05 0.65
Q8 1 -0.1150 0.3567 0.4824 11.00000 0.05 0.64
Q9 1 -0.0025 0.4611 0.7710 11.00000 0.05 0.63
Q10 1 0.4534 0.3402 0.2052 11.00000 0.05 0.62
Q11 1 0.0388 0.3406 0.6083 11.00000 0.05 0.61
Q12 1 -0.0648 0.4779 0.7096 11.00000 0.05 0.61
Q13 1 0.0208 0.5559 0.8948 11.00000 0.05 0.61
Q14 1 0.0680 0.2500 0.1132 10.50000 0.05 0.60
Q15 1 0.8900 0.4921 0.7268 11.00000 0.05 0.60
Q16 1 0.5216 0.3175 0.7808 11.00000 0.05 0.59
Q17 1 0.7761 0.1775 -0.2516 11.00000 0.05 0.58
Q18 1 0.3921 0.3242 0.8688 11.00000 0.05 0.58
Q19 1 0.6193 0.1576 0.2111 11.00000 0.05 0.58
Q20 1 0.5525 0.2500 -0.4939 10.50000 0.05 0.57
;
_shelx_res_checksum 57915
_shelx_hkl_file
;
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5 -19 0 8130.37 2027.22 1
-5 -19 0 7573.56 1870.77 2
5 -19 1-354.408 804.878 1
-5 -19 -1 1424.60 1140.81 2
5 -19 2 752.021 677.233 1
5 -19 3 1918.72 1217.82 1
5 -20 -3 1076.25 1243.86 1
-5 -20 3 693.000 1031.50 2
-5 -20 2-759.121 1101.51 2
5 -20 -2-1054.31 1223.20 1
-5 -20 1-618.956 1111.97 2
5 -20 -1-2914.29 1661.67 1
5 -20 0 2247.18 1224.07 1
-5 -20 0 2640.02 1382.48 2
5 -20 1 4743.64 1489.86 1
-5 -20 -1 6289.17 1911.56 2
-5 -20 -2 2732.98 1448.67 2
5 -20 2 579.091 931.450 1
-5 -21 2 14286.7 2359.59 2
5 -21 -2 13099.7 2273.71 1
5 -21 -1-104.273 998.425 1
-5 -21 1-984.073 1151.64 2
5 -21 0 1142.89 999.292 1
-5 -21 0 772.737 896.687 2
-5 -21 -1 7599.40 2105.67 2
5 -21 1 4580.15 1398.68 1
5 -21 2 27.0339 934.560 1
-5 -21 -2 2519.76 1422.17 2
-5 -22 1-1058.43 1108.18 2
5 -22 0 13913.9 2390.75 1
-5 -22 0 12546.1 2385.09 2
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6 0 1 198321. 9667.94 1
6 0 2 18963.2 3081.17 1
6 0 3 74678.7 5909.66 1
6 0 4 2778.17 1323.56 1
6 0 5 3887.98 1546.36 1
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6 -1 -4 2219.43 1721.49 1
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6 -1 -3 7997.46 2377.57 1
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6 -1 -2-6278.13 2997.74 1
6 -1 -1 28733.3 4305.65 1
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6 -1 0 3491.35 1378.15 1
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6 -1 1 1647.58 1502.86 1
6 1 1 1742.83 1416.63 1
6 -1 2 16963.6 3023.74 1
6 1 2 18069.4 2876.35 1
6 -1 3 23350.0 3301.84 1
6 1 3 23842.8 3243.68 1
6 -1 4 2528.00 1342.43 1
6 1 4 2125.20 1096.90 1
6 -1 5 3252.16 1510.97 1
6 1 5 3980.66 1508.51 1
6 2 -5 12292.5 3342.76 1
6 -2 -5 12599.7 3200.62 1
6 2 -4 8424.53 2594.95 1
6 -2 -4 8563.17 2747.40 1
6 2 -3 540.701 1272.10 1
6 -2 -3 814.043 1480.98 1
6 -2 -2 27676.7 3916.85 1
6 2 -2 26322.7 3597.19 1
6 -2 -1 2328.74 1988.56 1
6 2 -1 2497.05 1641.04 1
6 -2 0 44009.8 4790.87 1
6 2 0 46947.2 4582.68 1
6 -2 1 5413.06 2082.34 1
6 2 1 3917.72 1555.28 1
6 -2 2 778.261 1159.31 1
6 2 2-391.438 1126.53 1
6 -2 3 2038.52 1070.97 1
6 2 3 2008.60 944.875 1
6 -2 4 13250.2 2639.89 1
6 2 4 11483.5 2254.02 1
6 -2 5 14744.1 2966.83 1
6 2 5 13879.5 2625.84 1
6 3 -5 5262.32 2521.54 1
6 -3 -5 4021.41 2524.52 1
6 3 -4 8537.21 2666.58 1
6 -3 -4 8219.23 2647.01 1
6 3 -3 624.456 1245.25 1
6 -3 -3 646.808 1179.07 1
6 3 -2 11285.9 2374.93 1
6 -3 -2 15493.6 3651.85 1
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6 3 -1 2178.22 1659.33 1
6 -3 0-823.999 1340.65 1
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6 -3 1 2911.48 1801.39 1
6 3 1 788.726 1137.13 1
6 -3 2 431.622 903.345 1
6 3 2 139.820 688.368 1
6 3 3 10504.0 2005.98 1
6 -3 3 8949.37 2272.30 1
6 -3 4 11392.4 2620.06 1
6 3 4 12104.2 2175.66 1
6 -3 5 707.324 1190.17 1
6 3 5 1360.94 1070.94 1
6 -4 -5 8584.43 2808.57 1
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6 -4 -3 4926.58 1767.61 1
6 4 -2 27907.4 3562.65 1
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6 -4 -1 2755.52 1989.67 1
6 4 -1 1001.71 1238.42 1
6 -4 0 2756.48 1236.03 1
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6 -4 1 37212.0 4634.08 1
6 4 1 37119.5 3721.85 1
6 -4 2 6556.77 2141.77 1
6 4 2 6998.11 1601.66 1
6 4 3 15315.4 2381.67 1
6 -4 3 14377.3 2835.85 1
6 4 4 367.133 677.158 1
6 -4 4 313.312 1069.48 1
6 -4 5-335.892 945.840 1
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6 -5 -5 3770.61 2332.02 1
6 5 -4 10089.4 2759.96 1
6 -5 -4 10396.0 2748.82 1
6 5 -3 997.363 1248.46 1
6 -5 -3-2091.61 2154.43 1
6 5 -2 46008.0 4681.50 1
6 -5 -2 63217.7 6382.68 1
6 -5 -1 12058.7 3077.47 1
6 5 -1 8955.24 2020.02 1
6 5 0 22105.3 2792.65 1
6 -5 0 19508.7 3099.22 1
6 -5 1 10300.6 2793.64 1
6 5 1 7180.67 1635.93 1
6 -5 2 13067.2 2811.82 1
6 5 2 13705.3 2089.82 1
6 5 3 5972.86 1483.92 1
6 -5 3 2824.08 1373.02 1
6 -5 4 35258.4 4700.10 1
6 5 4 35559.6 3468.78 1
6 -5 5-557.111 1265.82 1
6 5 5 739.704 1030.70 1
6 -6 -5 5354.68 2225.31 1
6 6 -4 5365.59 2377.20 1
6 -6 -4 1723.60 1809.86 1
6 6 -3 147.442 887.592 1
6 -6 -3-2745.90 2342.82 1
6 -6 -2 16937.9 3513.02 1
6 6 -2 10988.5 2275.27 1
6 -6 -1 13643.8 3068.14 1
6 6 -1 10947.0 2115.34 1
6 6 0 23635.6 2770.33 1
6 -6 0 20256.7 3326.03 1
6 -6 1 6975.65 2526.59 1
6 6 1 3098.33 1136.08 1
6 -6 2 1140.94 1395.26 1
6 6 2 558.768 481.331 1
6 6 3 16719.7 2265.68 1
6 -6 3 13306.6 2700.70 1
6 -6 4 3068.36 1831.17 1
6 6 4 5334.64 1355.43 1
6 6 5 16448.5 2586.73 1
6 7 -5 9078.90 2913.09 1
6 -7 -5 1945.77 1825.56 1
6 7 -4 12526.8 2856.16 1
6 -7 -4 5976.97 2187.65 1
6 7 -3 3208.23 1505.01 1
6 -7 -3-397.221 1782.90 1
6 -7 -2 13774.8 3563.12 1
6 7 -2 7506.86 1967.80 1
6 -7 -1 3653.39 2139.84 1
6 7 -1-15.6972 651.641 1
6 -7 0 190.153 1334.32 1
6 7 0 2030.20 937.868 1
6 -7 1 3901.12 2135.53 1
6 7 1 1196.41 743.346 1
6 -7 2 11892.8 2822.07 1
6 7 2 10340.3 1694.18 1
6 7 3 14696.2 2026.80 1
6 -7 3 10753.5 2466.69 1
6 7 4 2613.84 1010.71 1
6 -7 4 2267.84 1524.84 1
6 8 -5 13387.3 2980.50 1
6 -8 -5 2322.33 1816.66 1
6 8 -4 10552.5 2613.85 1
6 -8 -4 5047.20 2038.78 1
6 8 -3 1769.20 1007.13 1
6 -8 -3-382.719 1629.61 1
6 8 -2 7529.66 1814.67 1
6 -8 -2 13797.1 3383.91 1
6 -8 -1 27765.8 4111.61 1
6 8 -1 23633.3 2798.58 1
6 8 0 1207.43 882.909 1
6 -8 0-2250.82 1960.59 1
6 -8 1 101450. 7645.69 1
6 8 1 99082.2 5057.10 1
6 -8 2 9555.50 2505.70 1
6 8 2 10146.7 1618.87 1
6 -8 3 31072.7 4219.35 1
6 8 3 31949.5 2921.96 1
6 -8 4 1122.89 1270.20 1
6 8 4 3705.41 1177.73 1
6 9 -5 21035.9 3324.62 1
6 -9 -5 19319.4 3488.02 1
6 9 -4 6854.96 2087.77 1
6 -9 -4-2202.12 1945.02 1
6 9 -3 20435.0 2834.49 1
6 -9 -3 22131.9 3467.69 1
6 9 -2 524.323 859.391 1
6 -9 -2 8545.83 3012.54 1
6 -9 -1 48904.4 5315.35 1
6 9 -1 45196.1 3644.41 1
6 9 0 1201.44 892.788 1
6 -9 0-1108.21 1763.26 1
6 -9 1 6503.88 2486.58 1
6 9 1 2302.84 775.596 1
6 9 2 2367.69 782.400 1
6 -9 2 3846.21 1703.16 1
6 9 3 18263.9 2087.35 1
6 -9 3 16814.2 3127.81 1
6 -9 4 7091.51 2221.75 1
6 10 -4 12574.5 2374.46 1
6 -10 -4 7062.61 2067.82 1
6 10 -3 4108.58 1268.74 1
6 -10 -3 1419.53 1860.05 1
6 10 -2 23346.7 2733.16 1
6 -10 -2 28795.1 4275.92 1
6 -10 -1 7027.93 2256.72 1
6 10 -1 6510.74 1348.05 1
6 -10 0 27655.7 3736.67 1
6 10 0 29979.5 2546.11 1
6 -10 1 27424.8 4076.46 1
6 -10 2 2151.94 1566.29 1
6 -10 3-879.403 1673.14 1
6 -10 4 12302.7 2932.90 1
6 -11 -4-221.941 1260.53 1
6 -11 -3-2716.38 1337.63 1
6 -11 -2 7158.79 2660.43 1
6 -11 -1 144.556 1180.96 1
6 -11 0 10596.8 2147.14 1
6 -11 1 3760.81 2033.72 1
6 -11 2 26643.8 4012.79 1
6 -11 3 8794.55 2310.97 1
6 -12 -4 3328.30 1291.45 1
6 -12 -3 12575.3 3410.84 1
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6 -12 0-4050.08 2273.37 1
6 -12 1 35340.8 4533.64 1
6 -12 2 3061.08 1766.76 1
6 -12 3 9644.91 2336.76 1
6 -13 -4-1759.66 1999.80 1
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6 -13 -2 27376.1 3910.64 1
6 -13 -1 18382.3 3055.84 1
6 -13 0 10633.1 1863.11 1
6 -13 1 10821.3 2648.36 1
6 -13 2 9999.80 2543.84 1
6 -13 3 1645.35 883.990 1
6 -14 -3 6072.27 2330.99 1
6 -14 -2 2482.60 1719.97 1
6 -14 -1 5622.61 1689.85 1
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6 -15 -3 18541.0 3425.82 1
6 -15 -2 11228.8 2590.27 1
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6 -16 -1-2405.28 1798.69 1
6 -16 0 4564.21 2008.66 1
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6 -16 2 1119.79 960.069 1
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6 -18 -1 2102.04 918.894 1
6 -18 0 4985.46 1903.61 1
7 0 -4 11999.7 2910.77 1
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7 -4 3 374.383 1021.18 1
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7 5 -5 5063.42 2334.94 1
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7 -5 2 55.8813 1121.17 1
7 5 2 1209.56 857.774 1
7 5 3-273.577 671.279 1
7 -5 3-420.096 1354.86 1
7 5 4 5832.92 1567.00 1
7 6 -5 2287.43 1866.92 1
7 6 -4-2389.47 1773.13 1
7 -6 -4-1904.21 1931.26 1
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7 -6 -3 46369.0 6043.24 1
7 -6 -2 7268.51 2933.99 1
7 6 -2 5259.07 1761.03 1
7 -6 -1 24274.2 3974.62 1
7 6 -1 23562.1 3217.58 1
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7 -6 2 4.90700 1044.14 1
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7 -6 3-1013.96 1804.99 1
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7 7 -4-418.920 1428.40 1
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7 -7 -3 13045.4 3723.36 1
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7 7 1 733.655 655.475 1
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7 -7 3-535.041 1687.16 1
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7 -9 -1 5043.08 1866.87 1
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7 -10 -1-1112.51 1909.55 1
7 -10 0 542.011 2049.36 1
7 -10 1 1051.48 1463.05 1
7 -10 2 11396.8 2939.60 1
7 -11 -2 2850.21 1762.60 1
7 -11 -1-1497.91 1964.13 1
7 -11 0-1357.92 2700.44 1
7 -11 1 3380.27 2038.34 1
7 -12 -1-1687.40 2125.48 1
7 -12 0 12422.2 2823.81 1
8 0 -3 3485.40 2365.15 1
8 0 -2 1652.88 1784.46 1
8 0 -1 12469.7 2661.40 1
8 0 0 4334.09 1616.95 1
8 0 1 65806.7 6224.72 1
8 0 2-1165.38 1455.15 1
8 1 -3 7540.53 2875.84 1
8 -1 -2 7977.90 2850.29 1
8 1 -2 8492.01 2626.01 1
8 -1 -1 11181.0 2679.60 1
8 1 -1 12748.5 2796.87 1
8 -1 0 1592.96 1337.65 1
8 1 0 3721.22 1974.18 1
8 -1 1 2950.22 1932.40 1
8 1 1 1734.19 1474.57 1
8 -1 2 3621.23 1542.31 1
8 1 2 4234.71 1677.96 1
8 2 -3 9675.47 3091.87 1
8 -2 -2 20971.3 4075.25 1
8 2 -2 18136.8 3471.82 1
8 -2 -1 2252.42 1254.49 1
8 2 -1 1529.69 1092.80 1
8 -2 0 21558.1 3968.87 1
8 2 0 22252.8 3628.25 1
8 -2 1 1729.21 1652.92 1
8 2 1-179.119 876.392 1
8 2 2 476.511 836.863 1
8 3 -3 8158.98 2842.83 1
8 -3 -2 8144.66 3076.97 1
8 3 -2 6747.09 2108.51 1
8 -3 -1-350.999 1526.66 1
8 3 -1-1813.42 1659.85 1
8 -3 0-3199.59 2014.48 1
8 3 0 846.099 1150.13 1
8 -3 1 2541.33 1907.99 1
8 3 1 1182.58 1077.17 1
8 3 2 428.739 834.390 1
8 3 3 2978.50 1374.93 1
8 4 -3 3042.43 1746.42 1
8 4 -2 9849.18 2399.81 1
8 -4 -1-543.461 2045.97 1
8 4 -1-491.706 1319.13 1
8 4 0-879.165 1088.63 1
8 -4 0-5187.04 2509.78 1
8 4 1 21566.1 3226.46 1
8 4 2 3200.35 1417.63 1
8 5 -3 4904.70 2110.33 1
8 5 -2 15415.2 3003.75 1
8 5 -1 1268.78 804.732 1
8 5 0 2244.01 1146.67 1
8 5 1 933.343 1029.18 1
8 5 2 3949.69 1501.69 1
8 6 -3 3681.42 1737.21 1
8 6 -2 4124.89 1454.41 1
8 6 -1 4056.21 1377.94 1
8 6 0 7513.11 1815.35 1
0 0 0 0.00 0.00 0
TITL enZn290bb in P2(1)/m
REM P2(1)/m (#11 in standard setting)
CELL 0.71073 6.437594 19.945140 6.726031 90.0000 93.1569 90.0000
ZERR 4.00 0.000327 0.001011 0.000366 0.0000 0.0043 0.0000
LATT 1
SYMM -x, y+1/2,-z
SFAC C H N O
UNIT 44.00 40.00 4.00 4.00
REM CrysAlisPro recorded range (K): Min=290.0; max=290.0; aver:290.0
TEMP 17
SIZE 0.10 0.20 0.24
TREF
HKLF 4
END
;
_shelx_hkl_checksum 97518
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.71190(12) 0.2500 -0.26937(11) 0.0404(2) Uani 1 2 d S T P . .
Br2 Br 0.79606(8) 0.14414(3) 0.21795(9) 0.03679(18) Uani 1 1 d . . . . .
Br3 Br 0.30046(10) 0.2500 0.14273(11) 0.0320(2) Uani 1 2 d S T P . .
Br4 Br 0.73017(7) 0.48847(3) 0.70126(8) 0.03080(17) Uani 1 1 d . . . . .
Zn1 Zn 0.67575(12) 0.2500 0.08672(12) 0.0269(2) Uani 1 2 d S T P . .
N1 N 0.2340(6) 0.4725(2) 0.8120(6) 0.0321(11) Uani 1 1 d . . . . .
H1A H 0.3338 0.4856 0.7343 0.039 Uiso 1 1 calc R U . . .
H1B H 0.2491 0.4933 0.9288 0.039 Uiso 1 1 calc R U . . .
H1C H 0.1103 0.4826 0.7540 0.039 Uiso 1 1 calc R U . . .
N2 N 0.3715(7) 0.3626(2) 0.5135(7) 0.0418(12) Uani 1 1 d . . . . .
H2A H 0.3457 0.3336 0.4147 0.050 Uiso 1 1 calc R U . . .
H2B H 0.4924 0.3525 0.5771 0.050 Uiso 1 1 calc R U . . .
H2C H 0.3777 0.4039 0.4641 0.050 Uiso 1 1 calc R U . . .
C1 C 0.2483(8) 0.3989(3) 0.8434(8) 0.0333(13) Uani 1 1 d . . . . .
H1D H 0.1503 0.3858 0.9407 0.040 Uiso 1 1 calc R U . . .
H1E H 0.3870 0.3879 0.8975 0.040 Uiso 1 1 calc R U . . .
C2 C 0.2036(8) 0.3590(3) 0.6540(8) 0.0374(14) Uani 1 1 d . . . . .
H2D H 0.1816 0.3125 0.6888 0.045 Uiso 1 1 calc R U . . .
H2E H 0.0759 0.3755 0.5880 0.045 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0474(5) 0.0496(6) 0.0245(4) 0.000 0.0055(3) 0.000
Br2 0.0416(3) 0.0273(3) 0.0417(4) 0.0066(3) 0.0045(2) 0.0062(2)
Br3 0.0280(4) 0.0327(5) 0.0354(5) 0.000 0.0031(3) 0.000
Br4 0.0259(3) 0.0388(4) 0.0274(3) 0.0004(3) -0.0016(2) 0.0004(2)
Zn1 0.0316(5) 0.0234(5) 0.0258(5) 0.000 0.0028(3) 0.000
N1 0.028(2) 0.041(3) 0.028(3) -0.004(2) 0.0024(18) 0.001(2)
N2 0.062(3) 0.032(3) 0.032(3) -0.005(2) 0.009(2) 0.005(2)
C1 0.037(3) 0.032(3) 0.031(3) 0.007(3) 0.006(2) 0.003(3)
C2 0.040(3) 0.032(3) 0.041(4) -0.003(3) 0.005(3) -0.007(3)
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Zn1 Br2 123.19(5) . 4_565 ?
Br2 Zn1 Br1 108.50(3) . . ?
Br2 Zn1 Br1 108.50(3) 4_565 . ?
Br2 Zn1 Br3 104.06(3) . . ?
Br2 Zn1 Br3 104.06(3) 4_565 . ?
Br1 Zn1 Br3 107.45(5) . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N2 H2A 109.5 . . ?
C2 N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
C2 N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
N1 C1 C2 113.1(4) . . ?
N1 C1 H1D 109.0 . . ?
C2 C1 H1D 109.0 . . ?
N1 C1 H1E 109.0 . . ?
C2 C1 H1E 109.0 . . ?
H1D C1 H1E 107.8 . . ?
N2 C2 C1 113.6(4) . . ?
N2 C2 H2D 108.8 . . ?
C1 C2 H2D 108.8 . . ?
N2 C2 H2E 108.8 . . ?
C1 C2 H2E 108.8 . . ?
H2D C2 H2E 107.7 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Zn1 2.4191(16) . ?
Br2 Zn1 2.4004(9) . ?
Br3 Zn1 2.4657(15) . ?
Zn1 Br2 2.4004(9) 4_565 ?
N1 C1 1.484(6) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N2 C2 1.476(7) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
C1 C2 1.516(7) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C2 H2D 0.9700 . ?
C2 H2E 0.9700 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A Br4 0.89 2.57 3.335(4) 144.0 .
N1 H1A Br4 0.89 2.98 3.559(4) 124.3 3_666
N1 H1B Br4 0.89 2.51 3.361(4) 160.1 3_667
N1 H1C Br4 0.89 2.46 3.303(4) 159.1 1_455
N2 H2A Br3 0.89 2.48 3.368(5) 175.8 .
N2 H2B Br1 0.89 2.66 3.409(5) 142.4 1_556
N2 H2C Br4 0.89 3.18 3.593(5) 110.4 .
N2 H2C Br4 0.89 2.50 3.352(5) 160.8 3_666
C1 H1D Br2 0.97 3.08 4.046(6) 172.3 4_466
C2 H2E Br2 0.97 3.02 3.826(6) 141.8 4_465
C2 H2E Br4 0.97 3.29 4.021(6) 134.0 1_455
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 N2 72.5(6) . . . . ?