#------------------------------------------------------------------------------
#$Date: 2025-01-22 04:40:13 +0200 (Wed, 22 Jan 2025) $
#$Revision: 297408 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/37/1573731.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1573731
loop_
_publ_author_name
'Yang, Yongqi'
'Ke, Bao'
'Yang, Chengzhi'
'Xue, Yang'
'Huang, Kaihuang'
'Lu, Xintong'
'Zou, Bingsuo'
_publ_section_title
;
Multifunctional applications enabled by tunable multi-emission and
ultra-broadband VIS-NIR luminescence via energy transfer in
Sn2+/Mn2+-doped lead-free Zn-based metal halides.
;
_journal_name_full 'Materials horizons'
_journal_paper_doi 10.1039/d4mh01821d
_journal_year 2025
_chemical_formula_moiety '2(C12 H28 N), Br4 Zn'
_chemical_formula_sum 'C24 H56 Br4 N2 Zn'
_chemical_formula_weight 757.71
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_Hall '-I 2ya'
_space_group_name_H-M_alt 'I 1 2/a 1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_audit_creation_date 2024-06-28
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-22 deposited with the CCDC. 2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 96.596(2)
_cell_angle_gamma 90
_cell_formula_units_Z 8
_cell_length_a 15.0869(3)
_cell_length_b 14.2481(2)
_cell_length_c 31.3091(5)
_cell_measurement_reflns_used 14921
_cell_measurement_temperature 296.00
_cell_measurement_theta_max 73.4440
_cell_measurement_theta_min 3.4340
_cell_volume 6685.6(2)
_computing_cell_refinement 'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_collection 'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_data_reduction 'CrysAlisPro 1.171.41.49a (Rigaku OD, 2019)'
_computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature 296.00
_diffrn_detector 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -100.00 -5.00 0.50 0.05 -- -39.95 -77.00 0.00 190
2 \w -63.00 35.00 0.50 0.05 -- -39.95 57.00 150.00 196
3 \w -25.00 44.00 0.50 0.05 -- -39.95 19.00 60.00 138
4 \w -104.00 -56.00 0.50 0.05 -- -39.95-178.00-150.00 96
5 \w -26.00 46.00 0.50 0.05 -- -39.95 19.00 120.00 144
6 \w 64.00 123.00 0.50 0.05 -- 39.95 178.00 -60.00 118
7 \w -18.00 21.00 0.50 0.05 -- 39.95 -19.00 -90.00 78
8 \w -86.00 -36.00 0.50 0.20 -- -94.50 125.00 30.00 100
9 \w -55.00 -26.00 0.50 0.20 -- -94.50 61.00-150.00 58
10 \w -177.00 -58.00 0.50 0.20 -- -94.50 -30.00 120.00 238
11 \w -71.00 -37.00 0.50 0.20 -- -94.50 61.00 30.00 68
12 \w -118.00 -83.00 0.50 0.20 -- -94.50 -94.00-120.00 70
13 \w -168.00-142.00 0.50 0.20 -- -94.50 -94.00-120.00 52
14 \w -51.00 -15.00 0.50 0.20 -- -94.50 45.00 -90.00 72
15 \w -56.00 -19.00 0.50 0.20 -- -94.50 61.00 120.00 74
16 \w 34.00 59.00 0.50 0.20 -- 108.87 -77.00-150.00 50
17 \w 93.00 120.00 0.50 0.20 -- 108.87 0.00-150.00 54
18 \w 31.00 68.00 0.50 0.20 -- 108.87 0.00-150.00 74
19 \w 38.00 71.00 0.50 0.20 -- 108.87 -61.00-150.00 66
20 \w 31.00 57.00 0.50 0.20 -- 108.87 -94.00 0.00 52
21 \w 37.00 95.00 0.50 0.20 -- 108.87 -77.00 90.00 116
22 \w 29.00 61.00 0.50 0.20 -- 108.87-102.00 -34.46 64
23 \w 73.00 111.00 0.50 0.20 -- 108.87-125.00 0.00 76
24 \w 69.00 103.00 0.50 0.20 -- 108.87 -94.00 0.00 68
25 \w 39.00 106.00 0.50 0.20 -- 108.87-125.00 -30.00 134
26 \w 34.00 62.00 0.50 0.20 -- 108.87 -61.00 30.00 56
27 \w 35.00 64.00 0.50 0.20 -- 108.87 -77.00-180.00 58
28 \w 29.00 86.00 0.50 0.20 -- 108.87 0.00 0.00 114
29 \w 124.00 177.00 0.50 0.20 -- 108.87 0.00-150.00 106
30 \w 71.00 110.00 0.50 0.20 -- 108.87-125.00-120.00 78
31 \w 72.00 97.00 0.50 0.20 -- 108.87 -94.00 150.00 50
32 \w 34.00 59.00 0.50 0.20 -- 108.87 -61.00 150.00 50
33 \w 34.00 62.00 0.50 0.20 -- 108.87 -94.00 150.00 56
34 \w 81.00 106.00 0.50 0.20 -- 108.87 -77.00 -30.00 50
35 \w 35.00 62.00 0.50 0.20 -- 108.87 -77.00 -30.00 54
36 \w 120.00 165.00 0.50 0.20 -- 108.87 45.00 30.00 90
37 \w 51.00 77.00 0.50 0.20 -- 108.87 -94.00 -90.00 52
38 \w 83.00 111.00 0.50 0.20 -- 108.87-125.00-180.00 56
39 \w 80.00 111.00 0.50 0.20 -- 108.87 45.00 30.00 62
40 \w 99.00 178.00 0.50 0.20 -- 108.87 0.00 0.00 158
41 \w 77.00 103.00 0.50 0.20 -- 108.87 -94.00 90.00 52
42 \w 81.00 106.00 0.50 0.20 -- 108.87 -77.00-180.00 50
43 \w 31.00 56.00 0.50 0.20 -- 108.87 -94.00 90.00 50
44 \w 82.00 107.00 0.50 0.20 -- 108.87-102.00 -34.46 50
45 \w 86.00 111.00 0.50 0.20 -- 108.87-125.00 -60.00 50
46 \w 42.00 68.00 0.50 0.20 -- 108.87-125.00 0.00 52
47 \w 76.00 96.00 0.50 0.20 -- 108.87-104.00 57.97 40
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11 -0.0537246000
_diffrn_orient_matrix_UB_12 -0.0285343000
_diffrn_orient_matrix_UB_13 0.0368967000
_diffrn_orient_matrix_UB_21 0.0336468000
_diffrn_orient_matrix_UB_22 -0.1016788000
_diffrn_orient_matrix_UB_23 -0.0028080000
_diffrn_orient_matrix_UB_31 0.0809301000
_diffrn_orient_matrix_UB_32 0.0232570000
_diffrn_orient_matrix_UB_33 0.0329191000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.1281
_diffrn_reflns_av_unetI/netI 0.0824
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 38
_diffrn_reflns_limit_l_min -38
_diffrn_reflns_number 33243
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 74.000
_diffrn_reflns_theta_min 2.842
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu 6.705
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.24162
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.49a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn 1.506
_exptl_crystal_description block
_exptl_crystal_F_000 3072
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.12
_refine_diff_density_max 0.869
_refine_diff_density_min -1.846
_refine_diff_density_rms 0.201
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 345
_refine_ls_number_reflns 6675
_refine_ls_number_restraints 194
_refine_ls_restrained_S_all 1.033
_refine_ls_R_factor_all 0.0839
_refine_ls_R_factor_gt 0.0768
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1568P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2031
_refine_ls_wR_factor_ref 0.2144
_reflns_Friedel_coverage 0.000
_reflns_number_gt 5506
_reflns_number_total 6675
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d4mh01821d2.cif
_cod_data_source_block 26-1
_cod_database_code 1573731
_shelx_shelxl_version_number 2019/2
_chemical_oxdiff_formula 'C N H O'
_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_max 0.500
_shelx_estimated_absorpt_t_min 0.433
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
C5-C4 = C5A-C4A
1.52 with sigma of 0.01
C2-C1 = C2A-C1A
1.52 with sigma of 0.01
N1-C4 \\sim N1-C4A
with sigma of 0.02
C6-C5 \\sim C6A-C5A
with sigma of 0.02
C4-C5 \\sim C4A-C5A
with sigma of 0.02
N1-C5 \\sim N1-C5A
with sigma of 0.04
C6-C4 \\sim C6A-C4A
with sigma of 0.04
N1-C3 \\sim N1-C3A
with sigma of 0.02
C1-C2 \\sim C1A-C2A
with sigma of 0.02
C3-C2 \\sim C3A-C2A
with sigma of 0.02
N1-C2 \\sim N1-C2A
with sigma of 0.04
C1-C3 \\sim C1A-C3A
with sigma of 0.04
C2A-C1A \\sim C2-C1 \\sim C3-C2 \\sim C3A-C2A \\sim C5A-C4A \\sim C5-C4 \\sim
C6-C5 \\sim C6A-C5A
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N1 \\sim C6 \\sim C1 \\sim C3 \\sim C4 \\sim C5 \\sim C2 \\sim C4A \\sim C5A
\\sim C6A \\sim C3A \\sim C2A \\sim C1A: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4. Others
Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=
Sof(H6AB)=Sof(H6AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=
Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C3)=
Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C2)=
Sof(H2A)=Sof(H2B)=FVAR(1)
5.a Riding coordinates:
C7(H7A,H7B,H7C)
5.b Secondary CH2 refined with riding coordinates:
C15(H15A,H15B), C21(H21A,H21B), C9(H9A,H9B), C20(H20A,H20B), C22(H22A,H22B),
C10(H10A,H10B), C16(H16A,H16B), C14(H14A,H14B), C17(H17A,H17B), C23(H23A,H23B),
C8(H8A,H8B), C11(H11A,H11B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C2(H2A,
H2B), C4A(H4AA,H4AB), C5A(H5AA,H5AB), C3A(H3AA,H3AB), C2A(H2AA,H2AB)
5.c Idealised Me refined as rotating group:
C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C12(H12A,H12B,H12C), C19(H19A,H19B,
H19C), C24(H24A,H24B,H24C), C6(H6A,H6B,H6C), C1(H1A,H1B,H1C), C6A(H6AA,H6AB,
H6AC), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_file
;
TITL 26-1_a.res in I2/a
26-1.res
created by SHELXL-2019/2 at 18:16:44 on 28-Jun-2024
REM Old TITL 26-1 in I2/a
REM SHELXT solution in I2/a: R1 0.241, Rweak 0.030, Alpha 0.039
REM 0.700 for 276 systematic absences, Orientation as input
REM Formula found by SHELXT: C23 N2 Br4 Zn
CELL 1.54184 15.0869 14.2481 31.3091 90 96.596 90
ZERR 8 0.0003 0.0002 0.0005 0 0.002 0
LATT 2
SYMM 0.5-X,+Y,-Z
SFAC C H Br N Zn
UNIT 192 448 32 16 8
EQIV $1 0.5-X,+Y,2-Z
SADI N1 C4 N1 C4A
SADI C6 C5 C6A C5A
SADI C4 C5 C4A C5A
SADI 0.04 N1 C5 N1 C5A
SADI 0.04 C6 C4 C6A C4A
SADI N1 C3 N1 C3A
SADI C1 C2 C1A C2A
SADI C3 C2 C3A C2A
SADI 0.04 N1 C2 N1 C2A
SADI 0.04 C1 C3 C1A C3A
SIMU 0.01 0.02 2 N1 C6 C1 C3 C4 C5 C2 C4A C5A C6A C3A C2A C1A
SADI C2A C1A C2 C1 C3 C2 C3A C2A C5A C4A C5 C4 C6 C5 C6A C5A
DFIX 1.52 0.01 C5 C4 C5A C4A
DFIX 1.52 0.01 C2 C1 C2A C1A
L.S. 10
PLAN 22
SIZE 0.12 0.13 0.15
TEMP 22.85
FREE C4A C3A_$1
list 4
MORE -1
BOND $H
fmap 2
acta
OMIT -2 0 24
OMIT -2 0 26
OMIT 2 2 2
OMIT 2 3 11
REM
REM
REM
WGHT 0.156800
FVAR 0.15671 0.48883
BR3 3 0.578119 0.338792 0.920948 11.00000 0.07450 0.07099 =
0.05963 -0.00455 -0.01219 -0.01451
BR1 3 0.534398 0.197186 0.808913 11.00000 0.08384 0.08629 =
0.06842 -0.01750 0.01071 -0.03235
BR4 3 0.411444 0.122417 0.908505 11.00000 0.08174 0.07283 =
0.08249 0.03215 -0.00397 -0.01957
ZN1 5 0.470302 0.253395 0.871750 11.00000 0.05799 0.05229 =
0.04945 0.00952 -0.00778 -0.00900
BR2 3 0.349447 0.356201 0.845894 11.00000 0.08601 0.07663 =
0.07444 0.02100 -0.01551 0.01506
N3 4 0.250000 0.591956 0.500000 10.50000 0.05401 0.04352 =
0.04710 0.00000 -0.00031 0.00000
N2 4 0.158931 0.513444 0.753590 11.00000 0.04660 0.04071 =
0.05606 0.00641 -0.00408 0.00115
N1 4 0.250000 0.417283 1.000000 10.50000 0.05720 0.06252 =
0.05400 0.00000 -0.00851 0.00000
C15 1 0.246313 0.468561 0.744257 11.00000 0.04866 0.05247 =
0.05687 0.01013 -0.00018 0.00354
AFIX 23
H15A 2 0.279730 0.514740 0.729910 11.00000 -1.20000
H15B 2 0.280877 0.453910 0.771501 11.00000 -1.20000
AFIX 0
C21 1 0.172992 0.654650 0.508135 11.00000 0.06104 0.04909 =
0.04968 0.00163 0.00355 0.00983
AFIX 23
H21A 2 0.161915 0.697889 0.484186 11.00000 -1.20000
H21B 2 0.190975 0.691678 0.533662 11.00000 -1.20000
AFIX 0
C9 1 0.107846 0.444531 0.777893 11.00000 0.05625 0.05227 =
0.06771 0.00518 0.00636 -0.00127
AFIX 23
H9A 2 0.146403 0.423488 0.802994 11.00000 -1.20000
H9B 2 0.093528 0.390192 0.759740 11.00000 -1.20000
AFIX 0
C20 1 0.086115 0.605709 0.514096 11.00000 0.06235 0.07679 =
0.07695 0.00475 0.01228 0.00640
AFIX 23
H20A 2 0.065011 0.571384 0.488153 11.00000 -1.20000
H20B 2 0.096060 0.561061 0.537545 11.00000 -1.20000
AFIX 0
C22 1 0.224294 0.528426 0.461182 11.00000 0.05539 0.05111 =
0.06539 -0.01361 -0.00416 -0.00170
AFIX 23
H22A 2 0.275296 0.489430 0.457013 11.00000 -1.20000
H22B 2 0.176767 0.487049 0.467917 11.00000 -1.20000
AFIX 0
C13 1 0.332624 0.344548 0.712487 11.00000 0.08049 0.07380 =
0.05996 -0.00279 0.01463 0.01428
AFIX 137
H13A 2 0.328829 0.288048 0.695671 11.00000 -1.50000
H13B 2 0.363369 0.331774 0.740452 11.00000 -1.50000
H13C 2 0.364690 0.391392 0.698447 11.00000 -1.50000
AFIX 0
C10 1 0.101514 0.539425 0.712216 11.00000 0.05853 0.05693 =
0.06666 0.01377 -0.01412 0.00001
AFIX 23
H10A 2 0.083481 0.481984 0.697004 11.00000 -1.20000
H10B 2 0.047807 0.569721 0.719676 11.00000 -1.20000
AFIX 0
C16 1 0.182966 0.601794 0.779717 11.00000 0.06144 0.04416 =
0.07547 -0.00261 -0.00170 0.00085
AFIX 23
H16A 2 0.130443 0.641466 0.778149 11.00000 -1.20000
H16B 2 0.228048 0.635631 0.766180 11.00000 -1.20000
AFIX 0
C14 1 0.239064 0.380108 0.717069 11.00000 0.06537 0.06575 =
0.06178 -0.00724 0.00270 0.00465
AFIX 23
H14A 2 0.207723 0.393600 0.688932 11.00000 -1.20000
H14B 2 0.205814 0.332576 0.730676 11.00000 -1.20000
AFIX 0
C18 1 0.257170 0.676769 0.846098 11.00000 0.06990 0.07035 =
0.08932 -0.02145 -0.00918 0.00314
AFIX 137
H18A 2 0.303572 0.697720 0.829801 11.00000 -1.50000
H18B 2 0.281697 0.665594 0.875320 11.00000 -1.50000
H18C 2 0.211691 0.724041 0.845433 11.00000 -1.50000
AFIX 0
C12 1 0.073434 0.631259 0.645383 11.00000 0.11195 0.07505 =
0.07398 0.01814 -0.02765 -0.00131
AFIX 137
H12A 2 0.101914 0.661535 0.623201 11.00000 -1.50000
H12B 2 0.031815 0.673794 0.656063 11.00000 -1.50000
H12C 2 0.042312 0.576463 0.633842 11.00000 -1.50000
AFIX 0
C17 1 0.217400 0.587619 0.826938 11.00000 0.07404 0.05941 =
0.06914 -0.00815 -0.00271 0.00448
AFIX 23
H17A 2 0.168677 0.567961 0.842568 11.00000 -1.20000
H17B 2 0.262218 0.538503 0.829550 11.00000 -1.20000
AFIX 0
C19 1 0.016424 0.676083 0.523794 11.00000 0.06770 0.10393 =
0.07639 0.00820 0.01843 0.01766
AFIX 137
H19A 2 0.005461 0.719223 0.500227 11.00000 -1.50000
H19B 2 0.037332 0.709959 0.549494 11.00000 -1.50000
H19C 2 -0.037864 0.643844 0.527833 11.00000 -1.50000
AFIX 0
C23 1 0.194148 0.577381 0.419382 11.00000 0.08680 0.07743 =
0.05512 -0.01713 -0.00929 0.00740
AFIX 23
H23A 2 0.243369 0.612473 0.409872 11.00000 -1.20000
H23B 2 0.146466 0.621062 0.423358 11.00000 -1.20000
AFIX 0
C8 1 0.021901 0.481967 0.792554 11.00000 0.06323 0.08345 =
0.10949 0.00614 0.02224 0.00097
AFIX 23
H8A 2 0.034599 0.537950 0.809805 11.00000 -1.20000
H8B 2 -0.019406 0.498798 0.767680 11.00000 -1.20000
AFIX 0
C11 1 0.143952 0.602558 0.682097 11.00000 0.08235 0.10330 =
0.08024 0.04156 -0.01813 -0.01369
AFIX 23
H11A 2 0.192556 0.570015 0.670673 11.00000 -1.20000
H11B 2 0.167975 0.657891 0.697338 11.00000 -1.20000
AFIX 0
C24 1 0.161305 0.504384 0.385765 11.00000 0.09050 0.11581 =
0.07434 -0.03401 -0.01811 0.01134
AFIX 137
H24A 2 0.148491 0.534258 0.358266 11.00000 -1.50000
H24B 2 0.108128 0.475273 0.393625 11.00000 -1.50000
H24C 2 0.206576 0.457565 0.384195 11.00000 -1.50000
AFIX 0
PART 1
C6 1 0.416909 0.555716 0.936818 21.00000 0.07793 0.09560 =
0.06870 -0.00874 0.02156 -0.01349
AFIX 137
H6A 2 0.377945 0.572239 0.911515 21.00000 -1.50000
H6B 2 0.475099 0.541360 0.929011 21.00000 -1.50000
H6C 2 0.421111 0.607412 0.956612 21.00000 -1.50000
AFIX 0
C1 1 0.142788 0.279223 0.898823 21.00000 0.09554 0.12236 =
0.07566 -0.01717 -0.00219 -0.01072
AFIX 137
H1A 2 0.107711 0.299708 0.872979 21.00000 -1.50000
H1B 2 0.107279 0.239461 0.914852 21.00000 -1.50000
H1C 2 0.193704 0.244893 0.891538 21.00000 -1.50000
AFIX 0
PART 0
C7 1 -0.019157 0.410092 0.818155 11.00000 0.10551 0.13291 =
0.19343 0.05529 0.08914 0.01587
AFIX 3
H7A 2 0.021313 0.394782 0.843135 11.00000 -1.50000
H7B 2 -0.073687 0.434082 0.826955 11.00000 -1.50000
H7C 2 -0.031617 0.354742 0.801055 11.00000 -1.50000
AFIX 0
PART 1
C3 1 0.231065 0.339717 0.966345 21.00000 0.07386 0.08132 =
0.06432 -0.02363 -0.00612 -0.00607
AFIX 23
H3A 2 0.287919 0.317395 0.958722 21.00000 -1.20000
H3B 2 0.203374 0.287823 0.979861 21.00000 -1.20000
AFIX 0
C4 1 0.297389 0.497695 0.978203 21.00000 0.06199 0.08190 =
0.06730 0.00005 -0.00353 -0.01037
AFIX 23
H4A 2 0.254717 0.525384 0.956249 21.00000 -1.20000
H4B 2 0.313658 0.545760 0.999616 21.00000 -1.20000
AFIX 0
C5 1 0.380356 0.471680 0.957593 21.00000 0.07185 0.09531 =
0.07244 0.00588 0.00159 -0.01143
AFIX 23
H5A 2 0.425241 0.446823 0.979319 21.00000 -1.20000
H5B 2 0.365719 0.423253 0.936165 21.00000 -1.20000
AFIX 0
C2 1 0.173583 0.363140 0.925590 21.00000 0.08174 0.10285 =
0.06735 -0.02384 -0.01086 -0.00508
AFIX 23
H2A 2 0.206634 0.404405 0.908528 21.00000 -1.20000
H2B 2 0.121616 0.397272 0.932704 21.00000 -1.20000
AFIX 0
PART 2
C4A 1 0.337091 0.455469 0.987381 -21.00000 0.05657 0.07882 =
0.06399 0.00981 -0.00541 -0.00461
AFIX 23
H4AA 2 0.372192 0.403198 0.978755 -21.00000 -1.20000
H4AB 2 0.370009 0.483617 1.012601 -21.00000 -1.20000
AFIX 0
C5A 1 0.328825 0.527567 0.951451 -21.00000 0.06917 0.09160 =
0.06589 0.01603 0.00036 -0.01275
AFIX 23
H5AA 2 0.306916 0.498031 0.924370 -21.00000 -1.20000
H5AB 2 0.287304 0.576558 0.957386 -21.00000 -1.20000
AFIX 0
C6A 1 0.419875 0.568500 0.948969 -21.00000 0.08724 0.10797 =
0.06607 0.01156 0.01360 -0.02572
AFIX 137
H6AA 2 0.414846 0.622738 0.930659 -21.00000 -1.50000
H6AB 2 0.457139 0.522576 0.937423 -21.00000 -1.50000
H6AC 2 0.445813 0.586340 0.977239 -21.00000 -1.50000
AFIX 0
C3A 1 0.187358 0.380082 0.963161 -21.00000 0.07787 0.09288 =
0.06681 -0.00589 -0.00907 -0.00995
AFIX 23
H3AA 2 0.132010 0.361665 0.973797 -21.00000 -1.20000
H3AB 2 0.173707 0.430022 0.942390 -21.00000 -1.20000
AFIX 0
C2A 1 0.223521 0.297987 0.940941 -21.00000 0.09653 0.10310 =
0.07693 -0.01763 -0.00270 -0.00565
AFIX 23
H2AA 2 0.234010 0.246923 0.961387 -21.00000 -1.20000
H2AB 2 0.280615 0.315398 0.931847 -21.00000 -1.20000
AFIX 0
C1A 1 0.163920 0.263481 0.902591 -21.00000 0.09269 0.12163 =
0.07900 -0.04110 0.00067 -0.01927
AFIX 137
H1AA 2 0.199070 0.231740 0.883361 -21.00000 -1.50000
H1AB 2 0.133817 0.315781 0.888039 -21.00000 -1.50000
H1AC 2 0.120675 0.220806 0.911796 -21.00000 -1.50000
AFIX 0
HKLF 4
REM 26-1_a.res in I2/a
REM wR2 = 0.2144, GooF = S = 1.036, Restrained GooF = 1.033 for all data
REM R1 = 0.0768 for 5506 Fo > 4sig(Fo) and 0.0839 for all 6675 data
REM 345 parameters refined using 194 restraints
END
WGHT 0.1568 0.0000
REM Highest difference peak 0.869, deepest hole -1.846, 1-sigma level 0.201
Q1 1 0.3625 0.3912 0.8695 11.00000 0.05 0.87
Q2 1 0.5586 0.1481 0.8276 11.00000 0.05 0.86
Q3 1 0.4141 0.1641 0.9314 11.00000 0.05 0.78
Q4 1 0.5534 0.2386 0.8354 11.00000 0.05 0.68
Q5 1 0.4292 0.0730 0.9311 11.00000 0.05 0.68
Q6 1 0.4865 0.1963 0.8907 11.00000 0.05 0.67
Q7 1 0.3968 0.1761 0.8894 11.00000 0.05 0.62
Q8 1 0.5972 0.2773 0.9424 11.00000 0.05 0.62
Q9 1 0.5616 0.3875 0.8982 11.00000 0.05 0.62
Q10 1 0.3969 0.0823 0.8701 11.00000 0.05 0.59
Q11 1 0.4529 0.3043 0.8455 11.00000 0.05 0.58
Q12 1 0.1755 0.2166 0.9245 11.00000 0.05 0.58
Q13 1 0.5917 0.3821 0.9484 11.00000 0.05 0.55
Q14 1 0.1592 0.2812 0.9662 11.00000 0.05 0.53
Q15 1 0.0313 0.6343 0.8092 11.00000 0.05 0.49
Q16 1 0.6577 0.1890 0.7905 11.00000 0.05 0.49
Q17 1 0.4785 0.3001 0.8927 11.00000 0.05 0.48
Q18 1 0.0322 0.5927 0.3947 11.00000 0.05 0.48
Q19 1 0.2040 0.6532 0.9061 11.00000 0.05 0.47
Q20 1 0.1585 0.1442 0.9582 11.00000 0.05 0.46
Q21 1 0.0739 0.5620 0.6190 11.00000 0.05 0.46
Q22 1 0.0878 0.6398 0.8273 11.00000 0.05 0.46
;
_shelx_res_checksum 19149
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 7.607
_oxdiff_exptl_absorpt_empirical_full_min 0.239
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
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
Br3 Br 0.57812(4) 0.33879(4) 0.92095(2) 0.0699(2) Uani 1 1 d . . . . .
Br1 Br 0.53440(4) 0.19719(5) 0.80891(2) 0.0794(2) Uani 1 1 d . . . . .
Br4 Br 0.41144(4) 0.12242(5) 0.90851(2) 0.0801(2) Uani 1 1 d . . . . .
Zn1 Zn 0.47030(4) 0.25339(4) 0.87175(2) 0.0543(2) Uani 1 1 d . . . . .
Br2 Br 0.34945(5) 0.35620(5) 0.84589(2) 0.0809(2) Uani 1 1 d . . . . .
N3 N 0.250000 0.5920(3) 0.500000 0.0487(10) Uani 1 2 d S T P . .
N2 N 0.1589(2) 0.5134(2) 0.75359(12) 0.0486(7) Uani 1 1 d . . . . .
N1 N 0.250000 0.4173(4) 1.000000 0.0591(12) Uani 1 2 d DS TU P . .
C15 C 0.2463(3) 0.4686(3) 0.74426(14) 0.0532(9) Uani 1 1 d . . . . .
H15A H 0.279730 0.514740 0.729910 0.064 Uiso 1 1 calc R U . . .
H15B H 0.280877 0.453910 0.771501 0.064 Uiso 1 1 calc R U . . .
C21 C 0.1730(3) 0.6547(3) 0.50813(14) 0.0535(9) Uani 1 1 d . . . . .
H21A H 0.161915 0.697889 0.484186 0.064 Uiso 1 1 calc R U . . .
H21B H 0.190975 0.691678 0.533662 0.064 Uiso 1 1 calc R U . . .
C9 C 0.1078(3) 0.4445(3) 0.77789(16) 0.0588(10) Uani 1 1 d . . . . .
H9A H 0.146403 0.423488 0.802994 0.071 Uiso 1 1 calc R U . . .
H9B H 0.093528 0.390192 0.759740 0.071 Uiso 1 1 calc R U . . .
C20 C 0.0861(4) 0.6057(4) 0.5141(2) 0.0717(13) Uani 1 1 d . . . . .
H20A H 0.065011 0.571384 0.488153 0.086 Uiso 1 1 calc R U . . .
H20B H 0.096060 0.561061 0.537545 0.086 Uiso 1 1 calc R U . . .
C22 C 0.2243(3) 0.5284(3) 0.46118(16) 0.0582(10) Uani 1 1 d . . . . .
H22A H 0.275296 0.489430 0.457013 0.070 Uiso 1 1 calc R U . . .
H22B H 0.176767 0.487049 0.467917 0.070 Uiso 1 1 calc R U . . .
C13 C 0.3326(4) 0.3445(4) 0.71249(18) 0.0709(13) Uani 1 1 d . . . . .
H13A H 0.328829 0.288048 0.695671 0.106 Uiso 1 1 calc R U . . .
H13B H 0.363369 0.331774 0.740452 0.106 Uiso 1 1 calc R U . . .
H13C H 0.364690 0.391392 0.698447 0.106 Uiso 1 1 calc R U . . .
C10 C 0.1015(3) 0.5394(4) 0.71222(17) 0.0624(11) Uani 1 1 d . . . . .
H10A H 0.083481 0.481984 0.697004 0.075 Uiso 1 1 calc R U . . .
H10B H 0.047807 0.569721 0.719676 0.075 Uiso 1 1 calc R U . . .
C16 C 0.1830(3) 0.6018(3) 0.77972(17) 0.0611(11) Uani 1 1 d . . . . .
H16A H 0.130443 0.641466 0.778149 0.073 Uiso 1 1 calc R U . . .
H16B H 0.228048 0.635631 0.766180 0.073 Uiso 1 1 calc R U . . .
C14 C 0.2391(4) 0.3801(4) 0.71707(17) 0.0647(11) Uani 1 1 d . . . . .
H14A H 0.207723 0.393600 0.688932 0.078 Uiso 1 1 calc R U . . .
H14B H 0.205814 0.332576 0.730676 0.078 Uiso 1 1 calc R U . . .
C18 C 0.2572(4) 0.6768(4) 0.8461(2) 0.0779(15) Uani 1 1 d . . . . .
H18A H 0.303572 0.697720 0.829801 0.117 Uiso 1 1 calc R U . . .
H18B H 0.281697 0.665594 0.875320 0.117 Uiso 1 1 calc R U . . .
H18C H 0.211691 0.724041 0.845433 0.117 Uiso 1 1 calc R U . . .
C12 C 0.0734(6) 0.6313(5) 0.6454(2) 0.090(2) Uani 1 1 d . . . . .
H12A H 0.101914 0.661535 0.623201 0.135 Uiso 1 1 calc R U . . .
H12B H 0.031815 0.673794 0.656063 0.135 Uiso 1 1 calc R U . . .
H12C H 0.042312 0.576463 0.633842 0.135 Uiso 1 1 calc R U . . .
C17 C 0.2174(4) 0.5876(4) 0.82694(18) 0.0684(12) Uani 1 1 d . . . . .
H17A H 0.168677 0.567961 0.842568 0.082 Uiso 1 1 calc R U . . .
H17B H 0.262218 0.538503 0.829550 0.082 Uiso 1 1 calc R U . . .
C19 C 0.0164(4) 0.6761(5) 0.5238(2) 0.0819(16) Uani 1 1 d . . . . .
H19A H 0.005461 0.719223 0.500227 0.123 Uiso 1 1 calc R U . . .
H19B H 0.037332 0.709959 0.549494 0.123 Uiso 1 1 calc R U . . .
H19C H -0.037864 0.643844 0.527833 0.123 Uiso 1 1 calc R U . . .
C23 C 0.1941(5) 0.5774(4) 0.41938(17) 0.0745(14) Uani 1 1 d . . . . .
H23A H 0.243369 0.612473 0.409872 0.089 Uiso 1 1 calc R U . . .
H23B H 0.146466 0.621062 0.423358 0.089 Uiso 1 1 calc R U . . .
C8 C 0.0219(4) 0.4820(5) 0.7926(3) 0.0844(16) Uani 1 1 d . . . . .
H8A H 0.034599 0.537950 0.809805 0.101 Uiso 1 1 calc R U . . .
H8B H -0.019406 0.498798 0.767680 0.101 Uiso 1 1 calc R U . . .
C11 C 0.1440(5) 0.6026(6) 0.6821(2) 0.091(2) Uani 1 1 d . . . . .
H11A H 0.192556 0.570015 0.670673 0.109 Uiso 1 1 calc R U . . .
H11B H 0.167975 0.657891 0.697338 0.109 Uiso 1 1 calc R U . . .
C24 C 0.1613(5) 0.5044(6) 0.3858(2) 0.096(2) Uani 1 1 d . . . . .
H24A H 0.148491 0.534258 0.358266 0.144 Uiso 1 1 calc R U . . .
H24B H 0.108128 0.475273 0.393625 0.144 Uiso 1 1 calc R U . . .
H24C H 0.206576 0.457565 0.384195 0.144 Uiso 1 1 calc R U . . .
C6 C 0.4169(15) 0.5557(14) 0.9368(6) 0.080(4) Uani 0.489(7) 1 d D U P A 1
H6A H 0.377945 0.572239 0.911515 0.120 Uiso 0.489(7) 1 calc R U P A 1
H6B H 0.475099 0.541360 0.929011 0.120 Uiso 0.489(7) 1 calc R U P A 1
H6C H 0.421111 0.607412 0.956612 0.120 Uiso 0.489(7) 1 calc R U P A 1
C1 C 0.143(2) 0.2792(16) 0.8988(9) 0.099(5) Uani 0.489(7) 1 d D U P A 1
H1A H 0.107711 0.299708 0.872979 0.148 Uiso 0.489(7) 1 calc R U P A 1
H1B H 0.107279 0.239461 0.914852 0.148 Uiso 0.489(7) 1 calc R U P A 1
H1C H 0.193704 0.244893 0.891538 0.148 Uiso 0.489(7) 1 calc R U P A 1
C7 C -0.0192(7) 0.4101(8) 0.8182(4) 0.138(4) Uani 1 1 d . . . . .
H7A H 0.021313 0.394782 0.843135 0.208 Uiso 1 1 d R U . . .
H7B H -0.073687 0.434082 0.826955 0.208 Uiso 1 1 d R U . . .
H7C H -0.031617 0.354742 0.801055 0.208 Uiso 1 1 d R U . . .
C3 C 0.2311(9) 0.3397(9) 0.9663(4) 0.074(2) Uani 0.489(7) 1 d D U P A 1
H3A H 0.287919 0.317395 0.958722 0.089 Uiso 0.489(7) 1 calc R U P A 1
H3B H 0.203374 0.287823 0.979861 0.089 Uiso 0.489(7) 1 calc R U P A 1
C4 C 0.2974(7) 0.4977(9) 0.9782(4) 0.071(2) Uani 0.489(7) 1 d D U P A 1
H4A H 0.254717 0.525384 0.956249 0.085 Uiso 0.489(7) 1 calc R U P A 1
H4B H 0.313658 0.545760 0.999616 0.085 Uiso 0.489(7) 1 calc R U P A 1
C5 C 0.3804(7) 0.4717(9) 0.9576(4) 0.080(2) Uani 0.489(7) 1 d D U P A 1
H5A H 0.425241 0.446823 0.979319 0.096 Uiso 0.489(7) 1 calc R U P A 1
H5B H 0.365719 0.423253 0.936165 0.096 Uiso 0.489(7) 1 calc R U P A 1
C2 C 0.1736(10) 0.3631(10) 0.9256(4) 0.085(3) Uani 0.489(7) 1 d D U P A 1
H2A H 0.206634 0.404405 0.908528 0.103 Uiso 0.489(7) 1 calc R U P A 1
H2B H 0.121616 0.397272 0.932704 0.103 Uiso 0.489(7) 1 calc R U P A 1
C4A C 0.3371(7) 0.4555(8) 0.9874(3) 0.067(2) Uani 0.511(7) 1 d D U P A 2
H4AA H 0.372192 0.403198 0.978755 0.081 Uiso 0.511(7) 1 calc R U P A 2
H4AB H 0.370009 0.483617 1.012601 0.081 Uiso 0.511(7) 1 calc R U P A 2
C5A C 0.3288(8) 0.5276(9) 0.9515(3) 0.076(2) Uani 0.511(7) 1 d D U P A 2
H5AA H 0.306916 0.498031 0.924370 0.091 Uiso 0.511(7) 1 calc R U P A 2
H5AB H 0.287304 0.576558 0.957386 0.091 Uiso 0.511(7) 1 calc R U P A 2
C6A C 0.4199(14) 0.5685(17) 0.9490(6) 0.087(5) Uani 0.511(7) 1 d D U P A 2
H6AA H 0.414846 0.622738 0.930659 0.130 Uiso 0.511(7) 1 calc R U P A 2
H6AB H 0.457139 0.522576 0.937423 0.130 Uiso 0.511(7) 1 calc R U P A 2
H6AC H 0.445813 0.586340 0.977239 0.130 Uiso 0.511(7) 1 calc R U P A 2
C3A C 0.1874(9) 0.3801(9) 0.9632(4) 0.081(2) Uani 0.511(7) 1 d D U P A 2
H3AA H 0.132010 0.361665 0.973797 0.097 Uiso 0.511(7) 1 calc R U P A 2
H3AB H 0.173707 0.430022 0.942390 0.097 Uiso 0.511(7) 1 calc R U P A 2
C2A C 0.2235(10) 0.2980(10) 0.9409(4) 0.093(3) Uani 0.511(7) 1 d D U P A 2
H2AA H 0.234010 0.246923 0.961387 0.112 Uiso 0.511(7) 1 calc R U P A 2
H2AB H 0.280615 0.315398 0.931847 0.112 Uiso 0.511(7) 1 calc R U P A 2
C1A C 0.1639(18) 0.263(2) 0.9026(8) 0.098(5) Uani 0.511(7) 1 d D U P A 2
H1AA H 0.199070 0.231740 0.883361 0.148 Uiso 0.511(7) 1 calc R U P A 2
H1AB H 0.133817 0.315781 0.888039 0.148 Uiso 0.511(7) 1 calc R U P A 2
H1AC H 0.120675 0.220806 0.911796 0.148 Uiso 0.511(7) 1 calc R U P A 2
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
Br3 0.0745(4) 0.0710(4) 0.0596(3) -0.0046(2) -0.0122(2) -0.0145(2)
Br1 0.0838(4) 0.0863(4) 0.0684(4) -0.0175(3) 0.0107(3) -0.0323(3)
Br4 0.0817(4) 0.0728(4) 0.0825(4) 0.0322(3) -0.0040(3) -0.0196(3)
Zn1 0.0580(4) 0.0523(4) 0.0494(3) 0.0095(2) -0.0078(2) -0.0090(2)
Br2 0.0860(4) 0.0766(4) 0.0744(4) 0.0210(3) -0.0155(3) 0.0151(3)
N3 0.054(3) 0.044(2) 0.047(2) 0.000 -0.0003(19) 0.000
N2 0.0466(17) 0.0407(16) 0.0561(17) 0.0064(14) -0.0041(13) 0.0011(13)
N1 0.057(3) 0.063(3) 0.054(2) 0.000 -0.009(2) 0.000
C15 0.049(2) 0.052(2) 0.057(2) 0.0101(18) -0.0002(16) 0.0035(17)
C21 0.061(2) 0.049(2) 0.050(2) 0.0016(16) 0.0035(18) 0.0098(17)
C9 0.056(2) 0.052(2) 0.068(3) 0.005(2) 0.0064(19) -0.0013(19)
C20 0.062(3) 0.077(3) 0.077(3) 0.005(3) 0.012(2) 0.006(2)
C22 0.055(2) 0.051(2) 0.065(3) -0.0136(19) -0.0042(19) -0.0017(18)
C13 0.080(3) 0.074(3) 0.060(3) -0.003(2) 0.015(2) 0.014(3)
C10 0.059(2) 0.057(3) 0.067(3) 0.014(2) -0.014(2) 0.000(2)
C16 0.061(3) 0.044(2) 0.075(3) -0.003(2) -0.002(2) 0.0009(18)
C14 0.065(3) 0.066(3) 0.062(3) -0.007(2) 0.003(2) 0.005(2)
C18 0.070(3) 0.070(3) 0.089(4) -0.021(3) -0.009(3) 0.003(3)
C12 0.112(5) 0.075(4) 0.074(4) 0.018(3) -0.028(3) -0.001(3)
C17 0.074(3) 0.059(3) 0.069(3) -0.008(2) -0.003(2) 0.004(2)
C19 0.068(3) 0.104(4) 0.076(3) 0.008(3) 0.018(3) 0.018(3)
C23 0.087(4) 0.077(3) 0.055(3) -0.017(2) -0.009(2) 0.007(3)
C8 0.063(3) 0.083(4) 0.109(5) 0.006(3) 0.022(3) 0.001(3)
C11 0.082(4) 0.103(5) 0.080(4) 0.042(3) -0.018(3) -0.014(3)
C24 0.091(4) 0.116(5) 0.074(4) -0.034(4) -0.018(3) 0.011(4)
C6 0.078(7) 0.096(8) 0.069(9) -0.009(7) 0.022(6) -0.013(6)
C1 0.096(11) 0.122(10) 0.076(8) -0.017(8) -0.002(7) -0.011(9)
C7 0.106(6) 0.133(7) 0.193(10) 0.055(7) 0.089(7) 0.016(5)
C3 0.074(5) 0.081(5) 0.064(4) -0.024(4) -0.006(4) -0.006(4)
C4 0.062(4) 0.082(5) 0.067(4) 0.000(4) -0.004(4) -0.010(4)
C5 0.072(5) 0.095(5) 0.072(4) 0.006(4) 0.002(4) -0.011(4)
C2 0.082(5) 0.103(6) 0.067(4) -0.024(4) -0.011(4) -0.005(5)
C4A 0.057(4) 0.079(5) 0.064(4) 0.010(4) -0.005(3) -0.005(4)
C5A 0.069(4) 0.092(5) 0.066(4) 0.016(4) 0.000(4) -0.013(4)
C6A 0.087(7) 0.108(9) 0.066(8) 0.012(8) 0.014(7) -0.026(7)
C3A 0.078(5) 0.093(5) 0.067(4) -0.006(4) -0.009(4) -0.010(4)
C2A 0.097(6) 0.103(6) 0.077(5) -0.018(5) -0.003(5) -0.006(5)
C1A 0.093(11) 0.122(9) 0.079(8) -0.041(8) 0.001(7) -0.019(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Br Br -0.6763 1.2805 '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'
Zn Zn -1.5491 0.6778 '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
Br1 Zn1 Br3 112.25(3) . . ?
Br4 Zn1 Br3 109.90(3) . . ?
Br4 Zn1 Br1 109.52(3) . . ?
Br2 Zn1 Br3 109.53(3) . . ?
Br2 Zn1 Br1 106.59(3) . . ?
Br2 Zn1 Br4 108.97(3) . . ?
C21 N3 C21 107.5(5) 2_556 . ?
C21 N3 C22 110.2(3) . 2_556 ?
C21 N3 C22 110.8(3) . . ?
C21 N3 C22 110.2(3) 2_556 . ?
C21 N3 C22 110.8(3) 2_556 2_556 ?
C22 N3 C22 107.4(5) 2_556 . ?
C9 N2 C15 109.1(3) . . ?
C9 N2 C10 108.3(4) . . ?
C9 N2 C16 111.8(4) . . ?
C10 N2 C15 111.1(4) . . ?
C10 N2 C16 109.5(3) . . ?
C16 N2 C15 107.0(3) . . ?
C3 N1 C3 87.6(10) . 2_557 ?
C3 N1 C4 106.8(7) . . ?
C3 N1 C4 141.0(7) . 2_557 ?
C3 N1 C4 106.8(7) 2_557 2_557 ?
C3 N1 C4 141.0(7) 2_557 . ?
C4 N1 C4 84.7(9) 2_557 . ?
C4A N1 C4A 137.9(10) 2_557 . ?
C3A N1 C4A 80.7(6) 2_557 . ?
C3A N1 C4A 114.5(7) . . ?
C3A N1 C4A 114.5(7) 2_557 2_557 ?
C3A N1 C4A 80.7(6) . 2_557 ?
N2 C15 H15A 108.1 . . ?
N2 C15 H15B 108.1 . . ?
H15A C15 H15B 107.3 . . ?
C14 C15 N2 116.6(4) . . ?
C14 C15 H15A 108.1 . . ?
C14 C15 H15B 108.1 . . ?
N3 C21 H21A 108.2 . . ?
N3 C21 H21B 108.2 . . ?
N3 C21 C20 116.2(4) . . ?
H21A C21 H21B 107.4 . . ?
C20 C21 H21A 108.2 . . ?
C20 C21 H21B 108.2 . . ?
N2 C9 H9A 108.5 . . ?
N2 C9 H9B 108.5 . . ?
N2 C9 C8 115.3(4) . . ?
H9A C9 H9B 107.5 . . ?
C8 C9 H9A 108.5 . . ?
C8 C9 H9B 108.5 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
H20A C20 H20B 108.1 . . ?
C19 C20 C21 110.6(5) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
N3 C22 H22A 108.3 . . ?
N3 C22 H22B 108.3 . . ?
H22A C22 H22B 107.4 . . ?
C23 C22 N3 116.1(4) . . ?
C23 C22 H22A 108.3 . . ?
C23 C22 H22B 108.3 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
N2 C10 H10A 108.3 . . ?
N2 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C11 C10 N2 116.1(4) . . ?
C11 C10 H10A 108.3 . . ?
C11 C10 H10B 108.3 . . ?
N2 C16 H16A 108.2 . . ?
N2 C16 H16B 108.2 . . ?
N2 C16 C17 116.5(4) . . ?
H16A C16 H16B 107.3 . . ?
C17 C16 H16A 108.2 . . ?
C17 C16 H16B 108.2 . . ?
C15 C14 C13 108.8(4) . . ?
C15 C14 H14A 109.9 . . ?
C15 C14 H14B 109.9 . . ?
C13 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
H14A C14 H14B 108.3 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C18 C17 C16 110.6(5) . . ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 108.1 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C23 H23A 109.9 . . ?
C22 C23 H23B 109.9 . . ?
C22 C23 C24 109.0(5) . . ?
H23A C23 H23B 108.3 . . ?
C24 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
C9 C8 H8A 109.6 . . ?
C9 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C7 C8 C9 110.2(6) . . ?
C7 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
C10 C11 C12 108.8(6) . . ?
C10 C11 H11A 109.9 . . ?
C10 C11 H11B 109.9 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C8 C7 H7A 109.4 . . ?
C8 C7 H7B 109.6 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7B 109.4 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C3 H3A 107.8 . . ?
N1 C3 H3B 107.8 . . ?
H3A C3 H3B 107.1 . . ?
C2 C3 N1 118.0(9) . . ?
C2 C3 H3A 107.8 . . ?
C2 C3 H3B 107.8 . . ?
N1 C4 H4A 108.1 . . ?
N1 C4 H4B 108.1 . . ?
H4A C4 H4B 107.3 . . ?
C5 C4 N1 116.8(9) . . ?
C5 C4 H4A 108.1 . . ?
C5 C4 H4B 108.1 . . ?
C6 C5 C4 110.6(12) . . ?
C6 C5 H5A 109.5 . . ?
C6 C5 H5B 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
C1 C2 H2A 108.7 . . ?
C1 C2 H2B 108.7 . . ?
C3 C2 C1 114.2(14) . . ?
C3 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N1 C4A H4AA 108.3 . . ?
N1 C4A H4AB 108.3 . . ?
N1 C4A C5A 115.9(8) . . ?
H4AA C4A H4AB 107.4 . . ?
C5A C4A H4AA 108.3 . . ?
C5A C4A H4AB 108.3 . . ?
C4A C5A H5AA 110.2 . . ?
C4A C5A H5AB 110.2 . . ?
H5AA C5A H5AB 108.5 . . ?
C6A C5A C4A 107.7(11) . . ?
C6A C5A H5AA 110.2 . . ?
C6A C5A H5AB 110.2 . . ?
C5A C6A H6AA 109.5 . . ?
C5A C6A H6AB 109.5 . . ?
C5A C6A H6AC 109.5 . . ?
H6AA C6A H6AB 109.5 . . ?
H6AA C6A H6AC 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?
N1 C3A C4A 50.0(4) . 2_557 ?
N1 C3A H3AA 108.8 . . ?
N1 C3A H3AB 108.8 . . ?
C4A C3A H3AA 68.2 2_557 . ?
C4A C3A H3AB 94.8 2_557 . ?
H3AA C3A H3AB 107.7 . . ?
C2A C3A N1 113.7(9) . . ?
C2A C3A C4A 155.6(11) . 2_557 ?
C2A C3A H3AA 108.8 . . ?
C2A C3A H3AB 108.8 . . ?
C3A C2A H2AA 108.7 . . ?
C3A C2A H2AB 108.7 . . ?
C3A C2A C1A 114.3(13) . . ?
H2AA C2A H2AB 107.6 . . ?
C1A C2A H2AA 108.7 . . ?
C1A C2A H2AB 108.7 . . ?
C2A C1A H1AA 109.5 . . ?
C2A C1A H1AB 109.5 . . ?
C2A C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
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
Br3 Zn1 2.4338(8) . ?
Br1 Zn1 2.4257(9) . ?
Br4 Zn1 2.4146(7) . ?
Zn1 Br2 2.4055(8) . ?
N3 C21 1.510(5) . ?
N3 C21 1.510(5) 2_556 ?
N3 C22 1.529(5) . ?
N3 C22 1.529(5) 2_556 ?
N2 C15 1.523(5) . ?
N2 C9 1.507(6) . ?
N2 C10 1.519(5) . ?
N2 C16 1.522(6) . ?
N1 C3 1.531(10) . ?
N1 C3 1.531(10) 2_557 ?
N1 C4 1.550(11) . ?
N1 C4 1.550(11) 2_557 ?
N1 C4A 1.516(9) . ?
N1 C4A 1.516(9) 2_557 ?
N1 C3A 1.501(10) . ?
N1 C3A 1.501(10) 2_557 ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C14 1.518(7) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C20 1.515(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C8 1.521(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 C19 1.509(8) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.506(8) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C13 C14 1.522(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.499(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.523(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18 C17 1.500(8) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C12 C11 1.530(8) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 C24 1.522(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C7 1.480(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C6 C5 1.498(14) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.503(8) . ?
C7 H7A 0.9604 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9596 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.496(12) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.519(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4A H4AA 0.9700 . ?
C4A H4AB 0.9700 . ?
C4A C5A 1.518(8) . ?
C5A H5AA 0.9700 . ?
C5A H5AB 0.9700 . ?
C5A C6A 1.503(14) . ?
C6A H6AA 0.9600 . ?
C6A H6AB 0.9600 . ?
C6A H6AC 0.9600 . ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?
C3A C2A 1.496(13) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A C1A 1.498(8) . ?
C1A H1AA 0.9600 . ?
C1A H1AB 0.9600 . ?
C1A H1AC 0.9600 . ?