#------------------------------------------------------------------------------
#$Date: 2024-01-06 09:59:37 +0200 (Sat, 06 Jan 2024) $
#$Revision: 288795 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247687.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_7247687
loop_
_publ_author_name
'Bothma, Shalene N.'
'Sheppard, Charles J.'
'Turnbull, Mark M.'
'Landee, Christopher P.'
'Rademeyer, Melanie'
_publ_section_title
;
The odd--even effect in n-carboxyalkylammonium-containing
organic--inorganic hybrids of Mn(ii) halides: structural and magnetic
characterisation
;
_journal_issue 47
_journal_name_full CrystEngComm
_journal_page_first 6568
_journal_page_last 6591
_journal_paper_doi 10.1039/D3CE00855J
_journal_volume 25
_journal_year 2023
_chemical_formula_moiety '2(C5 H12 N O2), Cl4 H4 Mn O2'
_chemical_formula_sum 'C10 H28 Cl4 Mn N2 O6'
_chemical_formula_weight 469.08
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary difmap
_audit_creation_method SHELXL-2018/3
_audit_update_record
;
2023-07-14 deposited with the CCDC. 2023-11-08 downloaded from the CCDC.
;
_cell_angle_alpha 91.740(2)
_cell_angle_beta 99.872(2)
_cell_angle_gamma 104.651(2)
_cell_formula_units_Z 1
_cell_length_a 5.9046(4)
_cell_length_b 7.8188(5)
_cell_length_c 11.5638(7)
_cell_measurement_reflns_used 9947
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 26.46
_cell_measurement_theta_min 2.70
_cell_volume 507.33(6)
_computing_cell_refinement 'SAINT (Bruker, 2014)'
_computing_data_collection 'APEX2 (Bruker, 2014)'
_computing_data_reduction 'SAINT (Bruker, 2014)'
_computing_molecular_graphics 'Mercury (Macrae et al., 2008)'
_computing_publication_material 'Mercury (Macrae et al., 2008)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature 150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type 'Bruker kappa, Photon 100 CMOS'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0302
_diffrn_reflns_av_unetI/netI 0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 7
_diffrn_reflns_limit_h_min -7
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 14955
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.499
_diffrn_reflns_theta_min 2.701
_exptl_absorpt_coefficient_mu 1.202
_exptl_absorpt_correction_T_max 0.7454
_exptl_absorpt_correction_T_min 0.6830
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Bruker, 2014)'
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.535
_exptl_crystal_description plate
_exptl_crystal_F_000 243
_exptl_crystal_size_max 0.347
_exptl_crystal_size_mid 0.263
_exptl_crystal_size_min 0.021
_refine_diff_density_max 0.247
_refine_diff_density_min -0.238
_refine_diff_density_rms 0.047
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.077
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 130
_refine_ls_number_reflns 2113
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.077
_refine_ls_R_factor_all 0.0233
_refine_ls_R_factor_gt 0.0192
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+0.2016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0459
_refine_ls_wR_factor_ref 0.0476
_reflns_Friedel_coverage 0.000
_reflns_number_gt 1927
_reflns_number_total 2113
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d3ce00855j2.cif
_cod_data_source_block C5MnClH2O
_cod_depositor_comments
'Adding full bibliography for 7247685--7247688.cif.'
_cod_database_code 7247687
_shelx_shelxl_version_number 2018/3
_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_res_file
;
TITL mo_SB1630_0m_a.res in P-1
shelx.res
created by SHELXL-2018/3 at 16:26:25 on 16-Nov-2022
CELL 0.71073 5.9046 7.8188 11.5638 91.740 99.872 104.651
ZERR 1.00 0.0004 0.0005 0.0007 0.002 0.002 0.002
LATT 1
SFAC C H CL MN N O
UNIT 10 28 4 1 2 6
MERG 2
HTAB O1 O2
HTAB O3 Cl1
EQIV_$1 -x+2, -y+2, -z+1
HTAB N1 Cl2_$1
EQIV_$2 -x+1, -y+1, -z+1
HTAB N1 Cl1_$2
EQIV_$3 x, y, z+1
HTAB N1 Cl2_$3
EQIV_$4 -x+1, -y+2, -z+1
HTAB N1 Cl2_$4
HTAB N1 O1_$4
EQIV_$5 x-1, y, z
HTAB O1 Cl1_$5
HTAB N1 Cl2_$1
HTAB N1 Cl1_$2
HTAB N1 Cl2_$3
HTAB N1 Cl2_$4
HTAB N1 O1_$4
HTAB O1 Cl1_$5
HTAB O1 O2
EQIV $7 -x+2, -y+1, -z+1
HTAB C4 O3_$7
HTAB C2 Cl2_$1
HTAB C1 O2_$4
HTAB O3 Cl1
HTAB N1 Cl2_$1
HTAB N1 Cl1_$2
HTAB N1 Cl2_$3
HTAB N1 Cl2_$4
HTAB N1 O1_$4
HTAB O1 Cl1_$5
HTAB O1 O2
FMAP 2
PLAN 20
ACTA
BOND $H
CONF
LIST 4
L.S. 10
TEMP -123.15
WGHT 0.019400 0.201600
FVAR 1.09557
MN1 4 0.500000 0.500000 0.000000 10.50000 0.01303 0.01290 =
0.01525 -0.00120 0.00376 0.00351
CL1 3 0.750663 0.339507 0.138856 11.00000 0.01536 0.01701 =
0.01984 0.00142 0.00214 0.00526
CL2 3 0.770439 0.796007 0.080794 11.00000 0.01348 0.01463 =
0.02345 -0.00242 0.00147 0.00220
O1 6 0.290579 0.534916 0.133442 11.00000 0.01322 0.02409 =
0.01569 -0.00069 0.00348 0.00281
O3 6 0.913782 0.602740 0.359475 11.00000 0.02634 0.04961 =
0.02178 -0.01205 -0.00032 0.01878
O2 6 0.537031 0.606171 0.361263 11.00000 0.02000 0.03093 =
0.01896 -0.00475 -0.00046 0.00696
N1 5 0.668896 1.057114 0.869602 11.00000 0.01707 0.01821 =
0.01821 0.00033 0.00464 0.00680
C5 1 0.744662 0.641094 0.408848 11.00000 0.02305 0.01649 =
0.01911 0.00198 0.00427 0.00848
C4 1 0.836741 0.727774 0.531037 11.00000 0.01984 0.02552 =
0.01842 -0.00259 0.00004 0.00809
AFIX 23
H4A 2 0.998531 0.806227 0.534301 11.00000 -1.20000
H4B 2 0.850303 0.634953 0.586205 11.00000 -1.20000
AFIX 0
C3 1 0.680768 0.836149 0.571899 11.00000 0.02085 0.01918 =
0.01788 -0.00053 0.00083 0.00774
AFIX 23
H3A 2 0.513401 0.763632 0.557239 11.00000 -1.20000
H3B 2 0.688310 0.941048 0.525417 11.00000 -1.20000
AFIX 0
C2 1 0.758056 0.897368 0.702133 11.00000 0.02113 0.02159 =
0.01777 -0.00192 0.00095 0.00953
AFIX 23
H2A 2 0.739249 0.792619 0.749124 11.00000 -1.20000
H2B 2 0.928616 0.962843 0.717992 11.00000 -1.20000
AFIX 0
C1 1 0.612384 1.015867 0.739517 11.00000 0.02026 0.01996 =
0.01564 0.00109 0.00165 0.00814
AFIX 23
H1B 2 0.646515 1.127554 0.699891 11.00000 -1.20000
H1A 2 0.440716 0.956074 0.714990 11.00000 -1.20000
AFIX 0
H3 2 0.860320 0.543365 0.298199 11.00000 0.04807
H1E 2 0.820921 1.117843 0.892615 11.00000 0.03676
H1D 2 0.644759 0.954822 0.906531 11.00000 0.02736
H1C 2 0.576833 1.121383 0.890736 11.00000 0.02873
H1 2 0.164411 0.484063 0.127825 11.00000 0.04082
H2 2 0.362036 0.543422 0.203654 11.00000 0.03498
HKLF 4
REM mo_SB1630_0m_a.res in P-1
REM wR2 = 0.0476, GooF = S = 1.077, Restrained GooF = 1.077 for all data
REM R1 = 0.0192 for 1927 Fo > 4sig(Fo) and 0.0233 for all 2113 data
REM 130 parameters refined using 0 restraints
END
WGHT 0.0194 0.2016
REM Highest difference peak 0.247, deepest hole -0.238, 1-sigma level 0.047
Q1 1 0.7157 0.8644 0.6370 11.00000 0.05 0.25
Q2 1 0.7949 0.7026 0.4697 11.00000 0.05 0.24
Q3 1 0.7656 0.7816 0.5549 11.00000 0.05 0.23
Q4 1 0.6771 0.9493 0.7175 11.00000 0.05 0.22
Q5 1 0.6283 0.6727 0.3599 11.00000 0.05 0.17
Q6 1 0.6450 1.0328 0.7985 11.00000 0.05 0.17
Q7 1 0.5066 0.6184 0.2921 11.00000 0.05 0.16
Q8 1 0.3111 0.6764 0.1351 11.00000 0.05 0.16
Q9 1 0.8821 0.6075 0.1139 11.00000 0.05 0.16
Q10 1 0.4458 0.6197 0.3875 11.00000 0.05 0.16
Q11 1 0.0759 0.4923 0.0143 11.00000 0.05 0.16
Q12 1 -0.0447 0.5320 0.0796 11.00000 0.05 0.16
Q13 1 0.8541 0.8797 0.7394 11.00000 0.05 0.16
Q14 1 0.7315 0.4887 0.0963 11.00000 0.05 0.14
Q15 1 0.3386 0.5523 0.0692 11.00000 0.05 0.14
Q16 1 1.0631 0.7642 0.3062 11.00000 0.05 0.14
Q17 1 0.6817 0.1557 0.1601 11.00000 0.05 0.13
Q18 1 0.7255 0.9054 0.9942 11.00000 0.05 0.13
Q19 1 0.5347 0.2284 0.1155 11.00000 0.05 0.13
Q20 1 0.9979 1.3043 0.9188 11.00000 0.05 0.13
;
_shelx_res_checksum 55956
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Mn1 Mn 0.500000 0.500000 0.000000 0.01362(8) Uani 1 2 d S . P . .
Cl1 Cl 0.75066(6) 0.33951(4) 0.13886(3) 0.01735(8) Uani 1 1 d . . . . .
Cl2 Cl 0.77044(5) 0.79601(4) 0.08079(3) 0.01778(9) Uani 1 1 d . . . . .
O1 O 0.2906(2) 0.53492(14) 0.13344(9) 0.0180(2) Uani 1 1 d . . . . .
O3 O 0.9138(2) 0.60274(17) 0.35947(10) 0.0319(3) Uani 1 1 d . . . . .
O2 O 0.53703(18) 0.60617(14) 0.36126(9) 0.0239(2) Uani 1 1 d . . . . .
N1 N 0.6689(2) 1.05711(17) 0.86960(10) 0.0173(2) Uani 1 1 d . . . . .
C5 C 0.7447(3) 0.64109(18) 0.40885(12) 0.0189(3) Uani 1 1 d . . . . .
C4 C 0.8367(3) 0.7278(2) 0.53104(12) 0.0214(3) Uani 1 1 d . . . . .
H4A H 0.998531 0.806227 0.534301 0.026 Uiso 1 1 calc R U . . .
H4B H 0.850303 0.634953 0.586205 0.026 Uiso 1 1 calc R U . . .
C3 C 0.6808(3) 0.83615(19) 0.57190(12) 0.0192(3) Uani 1 1 d . . . . .
H3A H 0.513401 0.763632 0.557239 0.023 Uiso 1 1 calc R U . . .
H3B H 0.688310 0.941048 0.525417 0.023 Uiso 1 1 calc R U . . .
C2 C 0.7581(3) 0.89737(19) 0.70213(12) 0.0198(3) Uani 1 1 d . . . . .
H2A H 0.739249 0.792619 0.749124 0.024 Uiso 1 1 calc R U . . .
H2B H 0.928616 0.962843 0.717992 0.024 Uiso 1 1 calc R U . . .
C1 C 0.6124(2) 1.01587(19) 0.73952(12) 0.0183(3) Uani 1 1 d . . . . .
H1B H 0.646515 1.127554 0.699891 0.022 Uiso 1 1 calc R U . . .
H1A H 0.440716 0.956074 0.714990 0.022 Uiso 1 1 calc R U . . .
H3 H 0.860(4) 0.543(3) 0.298(2) 0.048(6) Uiso 1 1 d . . . . .
H1E H 0.821(4) 1.118(3) 0.8926(16) 0.037(5) Uiso 1 1 d . . . . .
H1D H 0.645(3) 0.955(2) 0.9065(15) 0.027(4) Uiso 1 1 d . . . . .
H1C H 0.577(3) 1.121(2) 0.8907(15) 0.029(5) Uiso 1 1 d . . . . .
H1 H 0.164(4) 0.484(3) 0.1278(18) 0.041(6) Uiso 1 1 d . . . . .
H2 H 0.362(3) 0.543(2) 0.2037(18) 0.035(5) Uiso 1 1 d . . . . .
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
Mn1 0.01303(14) 0.01290(15) 0.01525(15) -0.00120(11) 0.00376(11) 0.00351(11)
Cl1 0.01536(16) 0.01701(17) 0.01984(17) 0.00142(12) 0.00214(12) 0.00526(12)
Cl2 0.01348(16) 0.01463(16) 0.02345(17) -0.00242(12) 0.00147(12) 0.00220(12)
O1 0.0132(5) 0.0241(6) 0.0157(5) -0.0007(4) 0.0035(4) 0.0028(4)
O3 0.0263(6) 0.0496(8) 0.0218(6) -0.0120(5) -0.0003(5) 0.0188(5)
O2 0.0200(5) 0.0309(6) 0.0190(5) -0.0048(4) -0.0005(4) 0.0070(4)
N1 0.0171(6) 0.0182(6) 0.0182(6) 0.0003(5) 0.0046(5) 0.0068(5)
C5 0.0231(7) 0.0165(7) 0.0191(7) 0.0020(5) 0.0043(6) 0.0085(6)
C4 0.0198(7) 0.0255(8) 0.0184(7) -0.0026(6) 0.0000(6) 0.0081(6)
C3 0.0208(7) 0.0192(7) 0.0179(7) -0.0005(5) 0.0008(6) 0.0077(6)
C2 0.0211(7) 0.0216(7) 0.0178(7) -0.0019(6) 0.0010(6) 0.0095(6)
C1 0.0203(7) 0.0200(7) 0.0156(7) 0.0011(5) 0.0016(5) 0.0081(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
O O 0.0106 0.0060 '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
O1 Mn1 O1 180.0 2_665 . ?
O1 Mn1 Cl2 86.11(3) 2_665 2_665 ?
O1 Mn1 Cl2 93.90(3) . 2_665 ?
O1 Mn1 Cl2 93.89(3) 2_665 . ?
O1 Mn1 Cl2 86.10(3) . . ?
Cl2 Mn1 Cl2 180.000(14) 2_665 . ?
O1 Mn1 Cl1 91.99(3) 2_665 2_665 ?
O1 Mn1 Cl1 88.01(3) . 2_665 ?
Cl2 Mn1 Cl1 91.374(11) 2_665 2_665 ?
Cl2 Mn1 Cl1 88.625(11) . 2_665 ?
O1 Mn1 Cl1 88.01(3) 2_665 . ?
O1 Mn1 Cl1 91.99(3) . . ?
Cl2 Mn1 Cl1 88.626(11) 2_665 . ?
Cl2 Mn1 Cl1 91.375(11) . . ?
Cl1 Mn1 Cl1 180.000(11) 2_665 . ?
Mn1 O1 H1 121.3(16) . . ?
Mn1 O1 H2 115.5(13) . . ?
H1 O1 H2 111(2) . . ?
C5 O3 H3 112.0(16) . . ?
C1 N1 H1E 110.6(12) . . ?
C1 N1 H1D 109.9(11) . . ?
H1E N1 H1D 108.3(16) . . ?
C1 N1 H1C 110.0(11) . . ?
H1E N1 H1C 108.7(16) . . ?
H1D N1 H1C 109.4(16) . . ?
O2 C5 O3 123.60(13) . . ?
O2 C5 C4 123.79(13) . . ?
O3 C5 C4 112.59(12) . . ?
C5 C4 C3 113.72(11) . . ?
C5 C4 H4A 108.8 . . ?
C3 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C4 C3 C2 111.99(11) . . ?
C4 C3 H3A 109.2 . . ?
C2 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C1 C2 C3 111.36(11) . . ?
C1 C2 H2A 109.4 . . ?
C3 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
C3 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N1 C1 C2 110.89(11) . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
H1B C1 H1A 108.0 . . ?
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
Mn1 O1 2.1872(10) 2_665 ?
Mn1 O1 2.1873(10) . ?
Mn1 Cl2 2.5034(3) 2_665 ?
Mn1 Cl2 2.5034(3) . ?
Mn1 Cl1 2.5672(3) 2_665 ?
Mn1 Cl1 2.5672(3) . ?
O1 H1 0.74(2) . ?
O1 H2 0.84(2) . ?
O3 C5 1.3227(18) . ?
O3 H3 0.80(2) . ?
O2 C5 1.2127(17) . ?
N1 C1 1.4907(17) . ?
N1 H1E 0.89(2) . ?
N1 H1D 0.909(19) . ?
N1 H1C 0.885(19) . ?
C5 C4 1.4978(19) . ?
C4 C3 1.5196(19) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C3 C2 1.5217(19) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C2 C1 1.5138(18) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 H1B 0.9900 . ?
C1 H1A 0.9900 . ?
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
_geom_hbond_publ_flag
O1 H2 O2 0.84(2) 1.92(2) 2.7486(15) 170.1(18) . yes
O3 H3 Cl1 0.80(2) 2.29(2) 3.0835(12) 169(2) . yes
N1 H1E Cl2 0.89(2) 2.30(2) 3.1612(13) 162.6(16) 2_776 yes
N1 H1D Cl1 0.909(19) 2.795(18) 3.4316(14) 128.1(13) 2_666 yes
N1 H1D Cl2 0.909(19) 2.502(18) 3.3033(13) 147.3(14) 1_556 yes
N1 H1C Cl2 0.885(19) 2.370(19) 3.2178(13) 160.3(15) 2_676 yes
N1 H1C O1 0.885(19) 2.640(18) 3.1396(17) 116.7(14) 2_676 yes
O1 H1 Cl1 0.74(2) 2.45(2) 3.1799(11) 171(2) 1_455 yes
N1 H1E Cl2 0.89(2) 2.30(2) 3.1612(13) 162.6(16) 2_776 yes
N1 H1D Cl1 0.909(19) 2.795(18) 3.4316(14) 128.1(13) 2_666 yes
N1 H1D Cl2 0.909(19) 2.502(18) 3.3033(13) 147.3(14) 1_556 yes
N1 H1C Cl2 0.885(19) 2.370(19) 3.2178(13) 160.3(15) 2_676 yes
N1 H1C O1 0.885(19) 2.640(18) 3.1396(17) 116.7(14) 2_676 yes
O1 H1 Cl1 0.74(2) 2.45(2) 3.1799(11) 171(2) 1_455 yes
O1 H2 O2 0.84(2) 1.92(2) 2.7486(15) 170.1(18) . yes
C4 H4B O3 0.99 2.62 3.4549(18) 141.9 2_766 yes
C2 H2B Cl2 0.99 2.96 3.6961(14) 132.2 2_776 yes
C1 H1B O2 0.99 2.64 3.4706(17) 141.4 2_676 yes
O3 H3 Cl1 0.80(2) 2.29(2) 3.0835(12) 169(2) . yes
N1 H1E Cl2 0.89(2) 2.30(2) 3.1612(13) 162.6(16) 2_776 yes
N1 H1D Cl1 0.909(19) 2.795(18) 3.4316(14) 128.1(13) 2_666 yes
N1 H1D Cl2 0.909(19) 2.502(18) 3.3033(13) 147.3(14) 1_556 yes
N1 H1C Cl2 0.885(19) 2.370(19) 3.2178(13) 160.3(15) 2_676 yes
N1 H1C O1 0.885(19) 2.640(18) 3.1396(17) 116.7(14) 2_676 yes
O1 H1 Cl1 0.74(2) 2.45(2) 3.1799(11) 171(2) 1_455 yes
O1 H2 O2 0.84(2) 1.92(2) 2.7486(15) 170.1(18) . 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C5 C4 C3 -24.1(2) . . . . ?
O3 C5 C4 C3 157.43(13) . . . . ?
C5 C4 C3 C2 170.93(12) . . . . ?
C4 C3 C2 C1 175.96(12) . . . . ?
C3 C2 C1 N1 173.10(12) . . . . ?