#------------------------------------------------------------------------------
#$Date: 2023-05-06 12:47:32 +0200 (Sat, 06 May 2023) $
#$Revision: 283590 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022728.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_2022728
loop_
_publ_author_name
'Vassilyeva, Olga Yu'
'Buvaylo, Elena A.'
'Kokozay, Vladimir N.'
'Skelton, Brian W.'
_publ_section_title
;
Synthesis, crystal structure and Hirshfeld surface analysis of the hybrid
salt bis-(2-methyl-imidazo[1,5-a]pyridin-2-ium)
tetra-chlorido-manganate(II).
;
_journal_coeditor_code JQ2027
_journal_issue 'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first 397
_journal_page_last 401
_journal_paper_doi 10.1107/S2056989023002761
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac '(C8 H9 N2)2 [Mn Cl4]'
_chemical_formula_moiety '2(C8 H9 N2 +), Cl4 Mn 2-'
_chemical_formula_sum 'C16 H18 Cl4 Mn N4'
_chemical_formula_weight 463.08
_chemical_name_systematic
;
Bis(2-methylimidazo[1,5-a]pyridin-2-ium) tetrachloridomanganate(II)
;
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_atom_sites_solution_hydrogens geom
_audit_creation_method 'WinGX routine CIF_UPDATE'
_cell_angle_alpha 99.211(5)
_cell_angle_beta 110.852(6)
_cell_angle_gamma 91.515(5)
_cell_formula_units_Z 2
_cell_length_a 9.4042(6)
_cell_length_b 10.7074(6)
_cell_length_c 10.7401(6)
_cell_measurement_reflns_used 3962
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 31.18
_cell_measurement_theta_min 2.077
_cell_volume 993.52(11)
_computing_cell_refinement
;
CrysAlis Pro (Rigaku OD, 2016)
;
_computing_data_collection
;
CrysAlis Pro (Rigaku OD, 2016)
;
_computing_data_reduction
;
CrysAlis Pro (Rigaku OD, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae et al., 2020)
;
_computing_publication_material
;
WinGX publication routines (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature 100(2)
_diffrn_detector 'CCD plate'
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type 'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.023
_diffrn_reflns_av_unetI/netI 0.0432
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -11
_diffrn_reflns_number 11038
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 32.11
_diffrn_reflns_theta_min 2.063
_diffrn_source 'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu 1.209
_exptl_absorpt_correction_T_max 0.908
_exptl_absorpt_correction_T_min 0.706
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
(CrysAlis Pro; Rigaku OD, 2016)
;
_exptl_crystal_colour 'light brown'
_exptl_crystal_density_diffrn 1.548
_exptl_crystal_description needle
_exptl_crystal_F_000 470
_exptl_crystal_size_max 0.43
_exptl_crystal_size_mid 0.155
_exptl_crystal_size_min 0.1
_refine_diff_density_max 1.32
_refine_diff_density_min -0.648
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 228
_refine_ls_number_reflns 6374
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.026
_refine_ls_R_factor_all 0.0604
_refine_ls_R_factor_gt 0.0469
_refine_ls_shift/su_max 0
_refine_ls_shift/su_mean 0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.8647P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1146
_refine_ls_wR_factor_ref 0.1263
_reflns_number_gt 5151
_reflns_number_total 6374
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file jq2027sup1.cif
_cod_data_source_block I
_cod_depositor_comments 'Adding full bibliography for 2022728.cif.'
_cod_database_code 2022728
_cod_database_fobs_code 2022728
_shelx_hkl_file
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13 -2 -8 326.257 196.128 4
13 -2 -7 7230.52 796.109 4
13 -2 -6 1678.27 408.462 4
13 -2 -5 12884.7 1077.84 3
13 -2 -5 13660.1 1086.68 4
13 -2 -4 4569.80 647.854 4
13 -2 -4 3441.38 581.555 3
13 -2 -3 1724.37 442.121 3
13 -2 -2 2393.46 477.549 3
13 -1 -10 794.162 272.689 4
13 -1 -9 1407.43 354.741 4
13 -1 -8 473.457 227.480 4
13 -1 -7-91.4893 166.319 4
13 -1 -7 93.5254 145.738 3
13 -1 -6 10401.4 956.048 3
13 -1 -6 8936.45 870.888 4
13 -1 -5 1641.71 398.285 3
13 -1 -4 465.909 259.980 3
13 -1 -3 22229.6 1431.51 3
13 -1 -2 709.821 333.679 3
-13 0 10 2819.58 521.197 1
-13 0 9 7283.60 816.637 1
13 0 -8 1356.44 339.327 3
13 0 -7 492.143 222.645 3
13 0 -6 9.42227 110.779 3
13 0 -5 581.125 250.563 3
13 0 -4 2210.65 449.326 3
13 0 -3 247.193 211.111 3
13 0 -2 5422.24 735.583 3
-13 -1 11 179.310 161.549 1
-13 -1 10 1621.73 391.351 1
-13 -1 9 159.206 186.700 1
-13 -1 8 281.658 197.597 1
13 1 -8-67.7047 132.517 3
13 1 -7 3231.74 518.351 3
13 1 -6 2341.14 450.229 3
13 1 -5 3045.95 517.784 3
13 1 -4 1115.32 342.893 3
13 1 -3 8252.83 883.233 3
13 1 -2-174.956 184.231 3
-13 -2 10 258.817 204.847 1
-13 -2 9 3333.98 569.026 1
-13 -2 8 81.1730 159.611 1
-13 -2 7 96.9120 161.170 1
13 2 -7-68.6917 126.409 3
-13 -2 6 753.624 274.524 1
13 2 -6 515.051 232.387 3
13 2 -5 350.873 207.050 3
13 2 -4 3125.48 542.954 3
13 2 -3 3.76350 132.355 3
-13 -3 8 1113.17 339.311 1
-13 -3 7 3049.98 572.419 1
-13 -3 6 4864.04 688.810 1
13 3 -6 4080.45 598.041 3
-13 -3 5-27.8984 151.193 1
13 3 -5 120.361 159.019 3
13 3 -4 9768.45 946.998 3
13 3 -3 109.870 147.689 3
13 4 -5 6204.34 755.884 3
13 4 -4 763.903 293.264 3
13 5 -5 2422.19 474.124 3
0 0 0 0.00 0.00 0
TITL lv748_bs12_analyt in P-1
REM P-1 (#2 in standard setting)
CELL 0.71073 9.404178 10.707445 10.740052 99.2108 110.8522 91.5150
ZERR 2.00 0.000629 0.000607 0.000582 0.0046 0.0056 0.0050
LATT 1
SFAC C H N Cl Mn
UNIT 32.00 36.00 8.00 8.00 2.00
TREF
HKLF 4
END
;
_shelx_hkl_checksum 72344
_shelx_res_file
;
TITL lv748 in P-1
shelx.res
created by SHELXL-2017/1 at 11:13:53 on 15-Oct-2019
CELL 0.71073 9.4042 10.7074 10.7401 99.211 110.852 91.515
ZERR 2.00 0.0006 0.0006 0.0006 0.005 0.006 0.005
LATT 1
SFAC C H N CL MN
UNIT 32 36 8 8 2
MERG 2
OMIT 0 1 0
HTAB C11 Cl4
EQIV $1 x, y+1, z
EQIV $2 -x+2, -y+1, -z
EQIV $3 -x+1, -y+1, -z
HTAB C13 Cl1_$3
HTAB C14 Cl1_$3
EQIV $4 x-1, y+1, z
HTAB C21 Cl3_$4
HTAB C22 Cl2_$3
HTAB C23 Cl1_$1
HTAB C24 Cl3_$1
EQIV $5 -x+1, -y+1, -z+1
HTAB C27 Cl4_$5
FMAP 2
PLAN 25
ACTA
BOND $H
CONF
L.S. 10
TEMP -173.00
WGHT 0.056400 0.864700
FVAR 5.33891
C11 1 0.764454 0.546812 0.266921 11.00000 0.01868 0.02009 =
0.02468 0.00282 0.00794 0.00263
AFIX 43
H11 2 0.838597 0.507280 0.330658 11.00000 -1.20000
AFIX 0
N12 3 0.789930 0.615155 0.181826 11.00000 0.01476 0.01848 =
0.02064 0.00167 0.00617 0.00233
C12 1 0.938154 0.639116 0.169990 11.00000 0.01718 0.02712 =
0.03394 0.00421 0.01167 0.00237
AFIX 137
H12A 2 0.989164 0.719825 0.228348 11.00000 -1.50000
H12B 2 0.922869 0.643492 0.075695 11.00000 -1.50000
H12C 2 1.001665 0.570072 0.198003 11.00000 -1.50000
AFIX 0
C13 1 0.657226 0.657182 0.104137 11.00000 0.01603 0.02126 =
0.02178 0.00255 0.00492 0.00430
AFIX 43
H13 2 0.645655 0.707320 0.036315 11.00000 -1.20000
AFIX 0
N13A 3 0.544573 0.613475 0.142463 11.00000 0.02250 0.02317 =
0.03120 -0.00126 0.00895 0.00298
C14 1 0.385632 0.624813 0.099965 11.00000 0.01782 0.02633 =
0.02944 -0.00113 0.00810 0.00504
AFIX 43
H14 2 0.336093 0.668856 0.028430 11.00000 -1.20000
AFIX 0
C15 1 0.306153 0.571415 0.163708 11.00000 0.01760 0.03062 =
0.04385 -0.00658 0.01408 -0.00081
AFIX 43
H15 2 0.199452 0.578985 0.136942 11.00000 -1.20000
AFIX 0
C16 1 0.378562 0.503943 0.270226 11.00000 0.03768 0.02819 =
0.04789 0.00177 0.02796 -0.00277
AFIX 43
H16 2 0.319686 0.468677 0.314078 11.00000 -1.20000
AFIX 0
C17 1 0.529337 0.489322 0.309819 11.00000 0.03705 0.02314 =
0.03554 0.00665 0.01870 0.00202
AFIX 43
H17 2 0.576756 0.442786 0.379620 11.00000 -1.20000
AFIX 0
C17A 1 0.614212 0.544400 0.245534 11.00000 0.01392 0.01191 =
0.01854 0.00048 0.00507 0.00086
C21 1 0.293249 0.897640 0.319457 11.00000 0.02211 0.02291 =
0.02910 -0.00152 0.01076 0.00233
AFIX 43
H21 2 0.196989 0.897717 0.329702 11.00000 -1.20000
AFIX 0
N22 3 0.327054 0.935892 0.216967 11.00000 0.03051 0.02184 =
0.02357 0.00048 0.00631 0.00547
C22 1 0.220051 0.987897 0.104742 11.00000 0.04197 0.03202 =
0.02732 0.00356 0.00113 0.01249
AFIX 137
H22A 2 0.275187 1.018410 0.051736 11.00000 -1.50000
H22B 2 0.173674 1.058598 0.141160 11.00000 -1.50000
H22C 2 0.139884 0.921389 0.046435 11.00000 -1.50000
AFIX 0
C23 1 0.472926 0.922509 0.234492 11.00000 0.03431 0.02189 =
0.02363 0.00179 0.01382 0.00241
AFIX 43
H23 2 0.523166 0.942318 0.176507 11.00000 -1.20000
AFIX 0
N23A 3 0.536384 0.875858 0.349165 11.00000 0.02433 0.01865 =
0.02742 0.00010 0.01235 -0.00051
C24 1 0.685789 0.845272 0.411899 11.00000 0.02010 0.02616 =
0.03854 -0.00694 0.01429 -0.00143
AFIX 43
H24 2 0.761335 0.856740 0.374017 11.00000 -1.20000
AFIX 0
C25 1 0.719362 0.799123 0.527493 11.00000 0.02435 0.02695 =
0.03782 -0.00429 0.00123 0.00410
AFIX 43
H25 2 0.819593 0.775808 0.570203 11.00000 -1.20000
AFIX 0
C26 1 0.609316 0.784435 0.587032 11.00000 0.04380 0.02227 =
0.02666 0.00539 0.00356 0.00005
AFIX 43
H26 2 0.637870 0.754350 0.670355 11.00000 -1.20000
AFIX 0
C27 1 0.465001 0.812373 0.527575 11.00000 0.03556 0.02253 =
0.02748 0.00095 0.01508 -0.00501
AFIX 43
H27 2 0.391259 0.800913 0.567407 11.00000 -1.20000
AFIX 0
C27A 1 0.424557 0.859190 0.404541 11.00000 0.01964 0.01798 =
0.02425 -0.00032 0.01143 -0.00081
MN1 5 0.845777 0.191040 0.250824 11.00000 0.01803 0.02251 =
0.01970 0.00445 0.00538 0.00204
CL1 4 0.578644 0.187564 0.133232 11.00000 0.01874 0.03281 =
0.02679 0.01002 0.00467 0.00303
CL2 4 0.987564 0.300198 0.150373 11.00000 0.02663 0.02637 =
0.03066 0.00723 0.01355 0.00141
CL3 4 0.901553 -0.022869 0.241685 11.00000 0.03501 0.02682 =
0.03954 0.01333 0.01614 0.01030
CL4 4 0.895379 0.307804 0.470870 11.00000 0.02688 0.03801 =
0.02218 0.00035 0.00624 -0.00093
HKLF 4
REM lv748 in P-1
REM R1 = 0.0469 for 5151 Fo > 4sig(Fo) and 0.0604 for all 6374 data
REM 228 parameters refined using 0 restraints
END
WGHT 0.0564 0.8648
REM Highest difference peak 1.320, deepest hole -0.648, 1-sigma level 0.097
Q1 1 0.9262 0.2309 0.4904 11.00000 0.05 1.32
Q2 1 1.0013 0.6552 0.2664 11.00000 0.05 0.52
Q3 1 0.8644 0.2627 0.2580 11.00000 0.05 0.52
Q4 1 0.9619 0.0424 0.2417 11.00000 0.05 0.50
Q5 1 0.9532 0.5720 0.1226 11.00000 0.05 0.46
Q6 1 0.8447 0.2406 0.3127 11.00000 0.05 0.46
Q7 1 0.4660 0.8677 0.3797 11.00000 0.05 0.46
Q8 1 0.1806 0.5018 0.4366 11.00000 0.05 0.45
Q9 1 0.6011 0.2610 0.1368 11.00000 0.05 0.42
Q10 1 0.1408 0.9772 0.1035 11.00000 0.05 0.42
Q11 1 0.7247 0.6284 0.1281 11.00000 0.05 0.40
Q12 1 0.9268 0.7010 0.1168 11.00000 0.05 0.39
Q13 1 0.3807 0.8988 0.3789 11.00000 0.05 0.39
Q14 1 0.5843 0.2223 0.0668 11.00000 0.05 0.39
Q15 1 0.6578 0.8002 0.5554 11.00000 0.05 0.39
Q16 1 0.6850 0.1968 0.1838 11.00000 0.05 0.38
Q17 1 0.9146 0.2140 0.2248 11.00000 0.05 0.38
Q18 1 0.7941 0.5842 0.2323 11.00000 0.05 0.38
Q19 1 0.7193 0.8630 0.4865 11.00000 0.05 0.37
Q20 1 0.9691 0.2900 0.2144 11.00000 0.05 0.37
Q21 1 0.8377 0.1205 0.2511 11.00000 0.05 0.36
Q22 1 0.7780 0.1955 0.2331 11.00000 0.05 0.35
Q23 1 0.8824 0.3831 0.5179 11.00000 0.05 0.35
Q24 1 0.9893 0.3673 0.1277 11.00000 0.05 0.34
Q25 1 0.3570 0.5596 0.2358 11.00000 0.05 0.34
;
_shelx_res_checksum 59810
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C11 0.7645(3) 0.5468(2) 0.2669(2) 0.0213(4) Uani d 1 . .
H H11 0.838597 0.50728 0.330658 0.026 Uiso calc 1 . .
N N12 0.7899(2) 0.61515(18) 0.18183(18) 0.0182(3) Uani d 1 . .
C C12 0.9382(3) 0.6391(2) 0.1700(3) 0.0256(5) Uani d 1 . .
H H12A 0.989164 0.719825 0.228348 0.038 Uiso calc 1 . .
H H12B 0.922869 0.643492 0.075695 0.038 Uiso calc 1 . .
H H12C 1.001665 0.570072 0.198003 0.038 Uiso calc 1 . .
C C13 0.6572(2) 0.6572(2) 0.1041(2) 0.0204(4) Uani d 1 . .
H H13 0.645655 0.70732 0.036315 0.024 Uiso calc 1 . .
N N13A 0.5446(2) 0.6135(2) 0.1425(2) 0.0266(4) Uani d 1 . .
C C14 0.3856(3) 0.6248(2) 0.1000(3) 0.0253(5) Uani d 1 . .
H H14 0.336093 0.668856 0.02843 0.03 Uiso calc 1 . .
C C15 0.3062(3) 0.5714(3) 0.1637(3) 0.0315(6) Uani d 1 . .
H H15 0.199452 0.578985 0.136942 0.038 Uiso calc 1 . .
C C16 0.3786(3) 0.5039(3) 0.2702(3) 0.0352(6) Uani d 1 . .
H H16 0.319686 0.468677 0.314078 0.042 Uiso calc 1 . .
C C17 0.5293(3) 0.4893(2) 0.3098(3) 0.0303(5) Uani d 1 . .
H H17 0.576756 0.442786 0.37962 0.036 Uiso calc 1 . .
C C17A 0.6142(2) 0.54440(19) 0.2455(2) 0.0153(4) Uani d 1 . .
C C21 0.2932(3) 0.8976(2) 0.3195(2) 0.0250(5) Uani d 1 . .
H H21 0.196989 0.897717 0.329702 0.03 Uiso calc 1 . .
N N22 0.3271(3) 0.9359(2) 0.2170(2) 0.0267(4) Uani d 1 . .
C C22 0.2201(4) 0.9879(3) 0.1047(3) 0.0370(6) Uani d 1 . .
H H22A 0.275187 1.01841 0.051736 0.056 Uiso calc 1 . .
H H22B 0.173674 1.058598 0.14116 0.056 Uiso calc 1 . .
H H22C 0.139884 0.921389 0.046435 0.056 Uiso calc 1 . .
C C23 0.4729(3) 0.9225(2) 0.2345(2) 0.0260(5) Uani d 1 . .
H H23 0.523166 0.942318 0.176507 0.031 Uiso calc 1 . .
N N23A 0.5364(2) 0.87586(19) 0.3492(2) 0.0232(4) Uani d 1 . .
C C24 0.6858(3) 0.8453(2) 0.4119(3) 0.0289(5) Uani d 1 . .
H H24 0.761335 0.85674 0.374017 0.035 Uiso calc 1 . .
C C25 0.7194(3) 0.7991(3) 0.5275(3) 0.0337(6) Uani d 1 . .
H H25 0.819593 0.775808 0.570203 0.04 Uiso calc 1 . .
C C26 0.6093(3) 0.7844(2) 0.5870(3) 0.0334(6) Uani d 1 . .
H H26 0.63787 0.75435 0.670355 0.04 Uiso calc 1 . .
C C27 0.4650(3) 0.8124(2) 0.5276(3) 0.0281(5) Uani d 1 . .
H H27 0.391259 0.800913 0.567407 0.034 Uiso calc 1 . .
C C27A 0.4246(3) 0.8592(2) 0.4045(2) 0.0202(4) Uani d 1 . .
Mn Mn1 0.84578(4) 0.19104(3) 0.25082(3) 0.02042(9) Uani d 1 . .
Cl Cl1 0.57864(6) 0.18756(6) 0.13323(6) 0.02657(13) Uani d 1 . .
Cl Cl2 0.98756(7) 0.30020(6) 0.15037(6) 0.02681(13) Uani d 1 . .
Cl Cl3 0.90155(8) -0.02287(6) 0.24168(7) 0.03208(14) Uani d 1 . .
Cl Cl4 0.89538(7) 0.30780(6) 0.47087(6) 0.03045(14) Uani d 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C11 0.0187(10) 0.0201(10) 0.0247(10) 0.0026(8) 0.0079(8) 0.0028(8)
N12 0.0148(8) 0.0185(8) 0.0206(8) 0.0023(6) 0.0062(7) 0.0017(7)
C12 0.0172(10) 0.0271(12) 0.0339(12) 0.0024(8) 0.0117(9) 0.0042(10)
C13 0.0160(9) 0.0213(10) 0.0218(10) 0.0043(8) 0.0049(8) 0.0026(8)
N13A 0.0225(10) 0.0232(10) 0.0312(10) 0.0030(8) 0.0089(8) -0.0013(8)
C14 0.0178(10) 0.0263(11) 0.0294(12) 0.0050(8) 0.0081(9) -0.0011(9)
C15 0.0176(11) 0.0306(13) 0.0439(15) -0.0008(9) 0.0141(10) -0.0066(11)
C16 0.0377(15) 0.0282(13) 0.0479(16) -0.0028(11) 0.0280(13) 0.0018(12)
C17 0.0370(14) 0.0231(12) 0.0355(13) 0.0020(10) 0.0187(11) 0.0067(10)
C17A 0.0139(9) 0.0119(8) 0.0185(9) 0.0009(7) 0.0051(7) 0.0005(7)
C21 0.0221(11) 0.0229(11) 0.0291(12) 0.0023(9) 0.0108(9) -0.0015(9)
N22 0.0305(11) 0.0218(10) 0.0236(10) 0.0055(8) 0.0063(8) 0.0005(8)
C22 0.0420(16) 0.0320(14) 0.0273(13) 0.0125(12) 0.0011(11) 0.0036(11)
C23 0.0343(13) 0.0219(11) 0.0236(11) 0.0024(9) 0.0138(10) 0.0018(9)
N23A 0.0243(10) 0.0186(9) 0.0274(10) -0.0005(7) 0.0124(8) 0.0001(7)
C24 0.0201(11) 0.0262(12) 0.0385(13) -0.0014(9) 0.0143(10) -0.0069(10)
C25 0.0244(12) 0.0270(13) 0.0378(14) 0.0041(10) 0.0012(10) -0.0043(11)
C26 0.0438(16) 0.0223(12) 0.0267(12) 0.0001(11) 0.0036(11) 0.0054(10)
C27 0.0356(13) 0.0225(11) 0.0275(12) -0.0050(10) 0.0151(10) 0.0010(9)
C27A 0.0196(10) 0.0180(10) 0.0242(10) -0.0008(8) 0.0114(8) -0.0003(8)
Mn1 0.01803(16) 0.02251(18) 0.01970(17) 0.00204(12) 0.00538(13) 0.00445(13)
Cl1 0.0187(2) 0.0328(3) 0.0268(3) 0.0030(2) 0.0047(2) 0.0100(2)
Cl2 0.0266(3) 0.0264(3) 0.0307(3) 0.0014(2) 0.0136(2) 0.0072(2)
Cl3 0.0350(3) 0.0268(3) 0.0395(3) 0.0103(2) 0.0161(3) 0.0133(3)
Cl4 0.0269(3) 0.0380(3) 0.0222(3) -0.0009(2) 0.0062(2) 0.0003(2)
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 0 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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
-1 0 0 0.0672
2 1 -1 0.0172
0 -1 1 0.0832
0 1 -1 0.0637
0 2 1 0.1701
0 -2 -1 0.1887
-2 -1 1 0.0812
-1 -3 3 0.0782
1 -1 1 0.064
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
N12 C11 C17A . . 107.34(19) ?
N12 C11 H11 . . 126.3 ?
C17A C11 H11 . . 126.3 ?
C11 N12 C13 . . 110.61(19) ?
C11 N12 C12 . . 125.11(19) ?
C13 N12 C12 . . 124.3(2) ?
N12 C12 H12A . . 109.5 ?
N12 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
N12 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
N13A C13 N12 . . 106.9(2) ?
N13A C13 H13 . . 126.5 ?
N12 C13 H13 . . 126.5 ?
C13 N13A C17A . . 106.65(18) ?
C13 N13A C14 . . 133.6(2) ?
C17A N13A C14 . . 119.8(2) ?
C15 C14 N13A . . 118.2(2) ?
C15 C14 H14 . . 120.9 ?
N13A C14 H14 . . 120.9 ?
C14 C15 C16 . . 121.5(2) ?
C14 C15 H15 . . 119.2 ?
C16 C15 H15 . . 119.2 ?
C17 C16 C15 . . 121.1(2) ?
C17 C16 H16 . . 119.5 ?
C15 C16 H16 . . 119.5 ?
C16 C17 C17A . . 118.4(2) ?
C16 C17 H17 . . 120.8 ?
C17A C17 H17 . . 120.8 ?
C11 C17A C17 . . 130.5(2) ?
C11 C17A N13A . . 108.49(19) ?
C17 C17A N13A . . 121.0(2) ?
N22 C21 C27A . . 106.9(2) ?
N22 C21 H21 . . 126.5 ?
C27A C21 H21 . . 126.5 ?
C23 N22 C21 . . 110.4(2) ?
C23 N22 C22 . . 124.2(2) ?
C21 N22 C22 . . 125.3(2) ?
N22 C22 H22A . . 109.5 ?
N22 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
N22 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?
N22 C23 N23A . . 107.7(2) ?
N22 C23 H23 . . 126.2 ?
N23A C23 H23 . . 126.2 ?
C23 N23A C24 . . 130.2(2) ?
C23 N23A C27A . . 108.6(2) ?
C24 N23A C27A . . 121.2(2) ?
C25 C24 N23A . . 118.0(2) ?
C25 C24 H24 . . 121 ?
N23A C24 H24 . . 121 ?
C24 C25 C26 . . 121.7(2) ?
C24 C25 H25 . . 119.1 ?
C26 C25 H25 . . 119.1 ?
C27 C26 C25 . . 121.0(2) ?
C27 C26 H26 . . 119.5 ?
C25 C26 H26 . . 119.5 ?
C26 C27 C27A . . 118.9(2) ?
C26 C27 H27 . . 120.5 ?
C27A C27 H27 . . 120.5 ?
C21 C27A N23A . . 106.4(2) ?
C21 C27A C27 . . 134.5(2) ?
N23A C27A C27 . . 119.0(2) ?
Cl3 Mn1 Cl4 . . 115.23(3) y
Cl3 Mn1 Cl1 . . 106.36(3) y
Cl4 Mn1 Cl1 . . 105.81(3) y
Cl3 Mn1 Cl2 . . 110.21(3) y
Cl4 Mn1 Cl2 . . 107.51(3) y
Cl1 Mn1 Cl2 . . 111.72(2) y
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
C11 N12 . 1.337(3) ?
C11 C17A . 1.347(3) ?
C11 H11 . 0.95 ?
N12 C13 . 1.366(3) ?
N12 C12 . 1.464(3) ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C13 N13A . 1.363(3) ?
C13 H13 . 0.95 ?
N13A C17A . 1.405(3) ?
N13A C14 . 1.414(3) ?
C14 C15 . 1.350(4) ?
C14 H14 . 0.95 ?
C15 C16 . 1.425(4) ?
C15 H15 . 0.95 ?
C16 C17 . 1.349(4) ?
C16 H16 . 0.95 ?
C17 C17A . 1.400(3) ?
C17 H17 . 0.95 ?
C21 N22 . 1.366(3) ?
C21 C27A . 1.369(3) ?
C21 H21 . 0.95 ?
N22 C23 . 1.332(3) ?
N22 C22 . 1.468(3) ?
C22 H22A . 0.98 ?
C22 H22B . 0.98 ?
C22 H22C . 0.98 ?
C23 N23A . 1.346(3) ?
C23 H23 . 0.95 ?
N23A C24 . 1.399(3) ?
N23A C27A . 1.400(3) ?
C24 C25 . 1.346(4) ?
C24 H24 . 0.95 ?
C25 C26 . 1.414(4) ?
C25 H25 . 0.95 ?
C26 C27 . 1.343(4) ?
C26 H26 . 0.95 ?
C27 C27A . 1.416(3) ?
C27 H27 . 0.95 ?
Mn1 Cl3 . 2.3577(7) y
Mn1 Cl4 . 2.3674(7) y
Mn1 Cl1 . 2.3725(7) y
Mn1 Cl2 . 2.3777(7) y
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
C11 H11 Cl4 . 0.95 2.76 3.592(2) 146.4 yes
C13 H13 Cl1 2_665 0.95 2.66 3.422(2) 137.5 yes
C14 H14 Cl1 2_665 0.95 2.79 3.549(3) 137.2 yes
C21 H21 Cl3 1_465 0.95 2.80 3.632(2) 146.6 yes
C22 H22C Cl2 2_665 0.98 2.82 3.742(3) 156.3 yes
C23 H23 Cl1 1_565 0.95 2.81 3.440(3) 125.0 yes
C24 H24 Cl3 1_565 0.95 2.69 3.573(3) 154.4 yes
C27 H27 Cl4 2_666 0.95 2.77 3.600(3) 146.2 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
C17A C11 N12 C13 . . . . -0.3(3) ?
C17A C11 N12 C12 . . . . -178.7(2) ?
C11 N12 C13 N13A . . . . 0.1(2) ?
C12 N12 C13 N13A . . . . 178.5(2) ?
N12 C13 N13A C17A . . . . 0.1(2) ?
N12 C13 N13A C14 . . . . -179.8(2) ?
C13 N13A C14 C15 . . . . -178.1(2) ?
C17A N13A C14 C15 . . . . 2.0(3) ?
N13A C14 C15 C16 . . . . -0.7(4) ?
C14 C15 C16 C17 . . . . -1.1(4) ?
C15 C16 C17 C17A . . . . 1.3(4) ?
N12 C11 C17A C17 . . . . -178.0(2) ?
N12 C11 C17A N13A . . . . 0.4(2) ?
C16 C17 C17A C11 . . . . 178.4(2) ?
C16 C17 C17A N13A . . . . 0.1(4) ?
C13 N13A C17A C11 . . . . -0.3(2) ?
C14 N13A C17A C11 . . . . 179.6(2) ?
C13 N13A C17A C17 . . . . 178.3(2) ?
C14 N13A C17A C17 . . . . -1.8(3) ?
C27A C21 N22 C23 . . . . 0.2(3) ?
C27A C21 N22 C22 . . . . -178.2(2) ?
C21 N22 C23 N23A . . . . -0.3(3) ?
C22 N22 C23 N23A . . . . 178.2(2) ?
N22 C23 N23A C24 . . . . -179.9(2) ?
N22 C23 N23A C27A . . . . 0.3(3) ?
C23 N23A C24 C25 . . . . -179.8(2) ?
C27A N23A C24 C25 . . . . 0.0(3) ?
N23A C24 C25 C26 . . . . -1.6(4) ?
C24 C25 C26 C27 . . . . 2.2(4) ?
C25 C26 C27 C27A . . . . -1.1(4) ?
N22 C21 C27A N23A . . . . 0.0(2) ?
N22 C21 C27A C27 . . . . 178.7(3) ?
C23 N23A C27A C21 . . . . -0.1(3) ?
C24 N23A C27A C21 . . . . 180.0(2) ?
C23 N23A C27A C27 . . . . -179.1(2) ?
C24 N23A C27A C27 . . . . 1.0(3) ?
C26 C27 C27A C21 . . . . -179.1(3) ?
C26 C27 C27A N23A . . . . -0.5(3) ?