# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_TEMMnCl2_a
_database_code_depnum_ccdc_archive 'CCDC 2116535'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2022-11-10 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H60 Cl8 Mn2 N4'
_chemical_formula_weight         798.24

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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   11.9192(5)
_cell_length_b                   13.1713(6)
_cell_length_c                   25.8199(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4053.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    14603
_cell_measurement_theta_min      2.8510
_cell_measurement_theta_max      30.3130

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_F_000             1672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    1.170
_shelx_estimated_absorpt_T_min   0.844
_shelx_estimated_absorpt_T_max   0.882
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual offset/far'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48181
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.436
_diffrn_reflns_theta_max         30.172
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10819
_reflns_number_gt                10040
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_max     0.867
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0828P)²+3.2520P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.510(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10819
_refine_ls_number_parameters     356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0875
_refine_ls_wR_factor_gt          0.0737
_refine_ls_goodness_of_fit_ref   0.742
_refine_ls_restrained_S_all      0.742
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Mn01 Mn 0.05013(3) 0.71719(3) 0.62144(2) 0.01340(9) Uani 1 1 d . . . . .
Mn02 Mn 0.44263(4) 0.20493(3) 0.63279(2) 0.01545(9) Uani 1 1 d . . . . .
Cl03 Cl 0.39923(6) 0.23327(6) 0.72233(2) 0.01862(14) Uani 1 1 d . . . . .
Cl04 Cl 0.07105(6) 0.77187(6) 0.70915(3) 0.02141(14) Uani 1 1 d . . . . .
Cl05 Cl -0.06567(6) 0.57231(5) 0.61947(3) 0.01832(13) Uani 1 1 d . . . . .
Cl06 Cl 0.22840(6) 0.68272(6) 0.58644(3) 0.02233(15) Uani 1 1 d . . . . .
Cl07 Cl -0.03379(6) 0.84546(6) 0.56845(3) 0.02120(14) Uani 1 1 d . . . . .
Cl08 Cl 0.58809(6) 0.08458(6) 0.62867(3) 0.02230(14) Uani 1 1 d . . . . .
Cl09 Cl 0.27637(6) 0.15757(6) 0.58966(3) 0.02421(15) Uani 1 1 d . . . . .
Cl0A Cl 0.50171(8) 0.35979(6) 0.59358(3) 0.0309(2) Uani 1 1 d . . . . .
N00B N 0.10929(19) 0.80205(18) 0.46706(9) 0.0141(4) Uani 1 1 d . . . . .
N00C N 0.38931(19) 0.31184(18) 0.48224(9) 0.0137(4) Uani 1 1 d . . . . .
N00D N 0.2497(2) 0.43070(19) 0.73006(9) 0.0162(5) Uani 1 1 d . . . . .
N00E N 0.2628(2) 0.93114(19) 0.74197(9) 0.0142(4) Uani 1 1 d . . . . .
C00F C 0.3850(2) 0.2029(2) 0.46389(11) 0.0176(5) Uani 1 1 d . . . . .
H00A H 0.366122 0.201638 0.426557 0.021 Uiso 1 1 calc R U . . .
H00B H 0.324810 0.166607 0.482773 0.021 Uiso 1 1 calc R U . . .
C00G C 0.2258(2) 0.8455(2) 0.47127(12) 0.0189(5) Uani 1 1 d . . . . .
H00C H 0.262762 0.841742 0.436990 0.023 Uiso 1 1 calc R U . . .
H00D H 0.270073 0.803789 0.495771 0.023 Uiso 1 1 calc R U . . .
C00H C 0.0329(3) 0.8626(2) 0.43213(12) 0.0218(6) Uani 1 1 d . . . . .
H00E H 0.024410 0.931702 0.446685 0.026 Uiso 1 1 calc R U . . .
H00F H -0.042113 0.830383 0.431977 0.026 Uiso 1 1 calc R U . . .
C00I C 0.4953(3) 0.1481(2) 0.47229(12) 0.0215(6) Uani 1 1 d . . . . .
H00G H 0.487942 0.077343 0.461125 0.032 Uiso 1 1 calc R U . . .
H00H H 0.514948 0.150213 0.509128 0.032 Uiso 1 1 calc R U . . .
H00I H 0.554280 0.181470 0.452052 0.032 Uiso 1 1 calc R U . . .
C00J C 0.1147(3) 0.6910(2) 0.45317(11) 0.0177(5) Uani 1 1 d . . . . .
H00J H 0.176965 0.658899 0.472521 0.021 Uiso 1 1 calc R U . . .
H00K H 0.131136 0.684383 0.415745 0.021 Uiso 1 1 calc R U . . .
C00K C 0.3214(2) 0.8812(2) 0.78724(11) 0.0184(5) Uani 1 1 d . . . . .
H00L H 0.369591 0.931993 0.804656 0.022 Uiso 1 1 calc R U . . .
H00M H 0.370666 0.826444 0.774035 0.022 Uiso 1 1 calc R U . . .
C00L C 0.1838(2) 0.4340(3) 0.77976(11) 0.0210(6) Uani 1 1 d . . . . .
H00N H 0.106812 0.408964 0.773274 0.025 Uiso 1 1 calc R U . . .
H00O H 0.178343 0.505242 0.791785 0.025 Uiso 1 1 calc R U . . .
C00M C 0.1059(3) 0.3610(3) 0.66974(12) 0.0241(6) Uani 1 1 d . . . . .
H00P H 0.054824 0.378770 0.641406 0.036 Uiso 1 1 calc R U . . .
H00Q H 0.062116 0.340220 0.700088 0.036 Uiso 1 1 calc R U . . .
H00R H 0.154442 0.304846 0.658864 0.036 Uiso 1 1 calc R U . . .
C00N C 0.3440(2) 0.9579(2) 0.69932(11) 0.0166(5) Uani 1 1 d . . . . .
H00S H 0.402832 1.002965 0.713600 0.020 Uiso 1 1 calc R U . . .
H00T H 0.303405 0.996274 0.672181 0.020 Uiso 1 1 calc R U . . .
C00O C 0.0065(3) 0.6352(2) 0.46526(12) 0.0210(6) Uani 1 1 d . . . . .
H00U H 0.012184 0.564849 0.453124 0.031 Uiso 1 1 calc R U . . .
H00V H -0.056228 0.668857 0.447719 0.031 Uiso 1 1 calc R U . . .
H00W H -0.006467 0.635678 0.502742 0.031 Uiso 1 1 calc R U . . .
C00P C 0.2722(2) 0.3544(2) 0.48398(12) 0.0198(5) Uani 1 1 d . . . . .
H00X H 0.224447 0.309430 0.505405 0.024 Uiso 1 1 calc R U . . .
H00Y H 0.240760 0.355139 0.448483 0.024 Uiso 1 1 calc R U . . .
C00Q C 0.3995(3) 0.8666(2) 0.67475(11) 0.0204(6) Uani 1 1 d . . . . .
H00Z H 0.445049 0.888691 0.645218 0.031 Uiso 1 1 calc R U . . .
H010 H 0.341824 0.819069 0.662813 0.031 Uiso 1 1 calc R U . . .
H011 H 0.447639 0.833014 0.700295 0.031 Uiso 1 1 calc R U . . .
C00R C 0.4712(3) 0.3771(2) 0.45254(13) 0.0223(6) Uani 1 1 d . . . . .
H012 H 0.547269 0.347668 0.455890 0.027 Uiso 1 1 calc R U . . .
H013 H 0.472695 0.445726 0.468140 0.027 Uiso 1 1 calc R U . . .
C00S C 0.2380(3) 0.3699(3) 0.82191(12) 0.0264(7) Uani 1 1 d . . . . .
H014 H 0.193945 0.375363 0.853827 0.040 Uiso 1 1 calc R U . . .
H015 H 0.314483 0.394284 0.828290 0.040 Uiso 1 1 calc R U . . .
H016 H 0.240574 0.298844 0.810762 0.040 Uiso 1 1 calc R U . . .
C00T C 0.1776(3) 0.4527(3) 0.68352(12) 0.0233(6) Uani 1 1 d . . . . .
H017 H 0.226036 0.470434 0.653710 0.028 Uiso 1 1 calc R U . . .
H018 H 0.128475 0.511475 0.690931 0.028 Uiso 1 1 calc R U . . .
C00U C 0.1977(3) 1.0234(3) 0.75946(11) 0.0213(6) Uani 1 1 d . . . . .
H019 H 0.251209 1.077152 0.769866 0.026 Uiso 1 1 calc R U . . .
H01A H 0.152514 1.005257 0.790277 0.026 Uiso 1 1 calc R U . . .
C00V C 0.1205(3) 1.0650(3) 0.71804(13) 0.0261(7) Uani 1 1 d . . . . .
H01B H 0.071268 1.116658 0.733185 0.039 Uiso 1 1 calc R U . . .
H01C H 0.074906 1.009716 0.703813 0.039 Uiso 1 1 calc R U . . .
H01D H 0.165359 1.095514 0.690305 0.039 Uiso 1 1 calc R U . . .
C00W C 0.2407(3) 0.8365(3) 0.82666(12) 0.0227(6) Uani 1 1 d . . . . .
H01E H 0.282352 0.794391 0.851323 0.034 Uiso 1 1 calc R U . . .
H01F H 0.184661 0.794806 0.808805 0.034 Uiso 1 1 calc R U . . .
H01G H 0.202913 0.891627 0.845290 0.034 Uiso 1 1 calc R U . . .
C00X C 0.2256(3) 0.9548(3) 0.48964(14) 0.0265(7) Uani 1 1 d . . . . .
H01H H 0.302982 0.977440 0.495142 0.040 Uiso 1 1 calc R U . . .
H01I H 0.183811 0.959768 0.522233 0.040 Uiso 1 1 calc R U . . .
H01J H 0.189833 0.997757 0.463426 0.040 Uiso 1 1 calc R U . . .
C00Y C 0.3546(3) 0.4958(2) 0.73112(12) 0.0204(6) Uani 1 1 d . . . . .
H01K H 0.403130 0.476348 0.701633 0.024 Uiso 1 1 calc R U . . .
H01L H 0.396421 0.481359 0.763408 0.024 Uiso 1 1 calc R U . . .
C00Z C 0.0739(4) 0.8714(3) 0.37685(13) 0.0358(8) Uani 1 1 d . . . . .
H01M H 0.023767 0.916290 0.357370 0.054 Uiso 1 1 calc R U . . .
H01N H 0.074550 0.804010 0.360750 0.054 Uiso 1 1 calc R U . . .
H01O H 0.150034 0.899545 0.376634 0.054 Uiso 1 1 calc R U . . .
C010 C 0.3315(3) 0.6090(3) 0.72819(15) 0.0295(7) Uani 1 1 d . . . . .
H01P H 0.402444 0.646310 0.730794 0.044 Uiso 1 1 calc R U . . .
H01Q H 0.282087 0.628827 0.756777 0.044 Uiso 1 1 calc R U . . .
H01R H 0.295218 0.624899 0.695126 0.044 Uiso 1 1 calc R U . . .
C011 C 0.2683(3) 0.4608(3) 0.50598(15) 0.0289(7) Uani 1 1 d . . . . .
H01S H 0.190131 0.480344 0.512194 0.043 Uiso 1 1 calc R U . . .
H01T H 0.302394 0.508201 0.481308 0.043 Uiso 1 1 calc R U . . .
H01U H 0.309947 0.462825 0.538698 0.043 Uiso 1 1 calc R U . . .
C012 C 0.4421(4) 0.3865(3) 0.39513(13) 0.0360(9) Uani 1 1 d . . . . .
H01V H 0.489915 0.438231 0.379129 0.054 Uiso 1 1 calc R U . . .
H01W H 0.363177 0.406233 0.391466 0.054 Uiso 1 1 calc R U . . .
H01X H 0.454383 0.321084 0.377969 0.054 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Mn01 Cl06 2.3531(8) . ?
Mn01 Cl05 2.3556(8) . ?
Mn01 Cl04 2.3896(8) . ?
Mn01 Cl07 2.3931(8) . ?
Mn02 Cl08 2.3515(8) . ?
Mn02 Cl09 2.3572(8) . ?
Mn02 Cl0A 2.3835(9) . ?
Mn02 Cl03 2.3985(8) . ?
N00B C00G 1.505(4) . ?
N00B C00J 1.507(4) . ?
N00B C00H 1.509(4) . ?
N00C C00P 1.505(4) . ?
N00C C00R 1.510(4) . ?
N00C C00F 1.512(4) . ?
N00D C00L 1.505(4) . ?
N00D C00T 1.505(4) . ?
N00D C00Y 1.516(4) . ?
N00E C00N 1.508(3) . ?
N00E C00U 1.511(4) . ?
N00E C00K 1.512(3) . ?
C00F C00I 1.515(4) . ?
C00F H00A 0.9900 . ?
C00F H00B 0.9900 . ?
C00G C00X 1.516(4) . ?
C00G H00C 0.9900 . ?
C00G H00D 0.9900 . ?
C00H C00Z 1.513(5) . ?
C00H H00E 0.9900 . ?
C00H H00F 0.9900 . ?
C00I H00G 0.9800 . ?
C00I H00H 0.9800 . ?
C00I H00I 0.9800 . ?
C00J C00O 1.517(4) . ?
C00J H00J 0.9900 . ?
C00J H00K 0.9900 . ?
C00K C00W 1.519(4) . ?
C00K H00L 0.9900 . ?
C00K H00M 0.9900 . ?
C00L C00S 1.521(4) . ?
C00L H00N 0.9900 . ?
C00L H00O 0.9900 . ?
C00M C00T 1.522(4) . ?
C00M H00P 0.9800 . ?
C00M H00Q 0.9800 . ?
C00M H00R 0.9800 . ?
C00N C00Q 1.512(4) . ?
C00N H00S 0.9900 . ?
C00N H00T 0.9900 . ?
C00O H00U 0.9800 . ?
C00O H00V 0.9800 . ?
C00O H00W 0.9800 . ?
C00P C011 1.513(5) . ?
C00P H00X 0.9900 . ?
C00P H00Y 0.9900 . ?
C00Q H00Z 0.9800 . ?
C00Q H010 0.9800 . ?
C00Q H011 0.9800 . ?
C00R C012 1.527(5) . ?
C00R H012 0.9900 . ?
C00R H013 0.9900 . ?
C00S H014 0.9800 . ?
C00S H015 0.9800 . ?
C00S H016 0.9800 . ?
C00T H017 0.9900 . ?
C00T H018 0.9900 . ?
C00U C00V 1.513(4) . ?
C00U H019 0.9900 . ?
C00U H01A 0.9900 . ?
C00V H01B 0.9800 . ?
C00V H01C 0.9800 . ?
C00V H01D 0.9800 . ?
C00W H01E 0.9800 . ?
C00W H01F 0.9800 . ?
C00W H01G 0.9800 . ?
C00X H01H 0.9800 . ?
C00X H01I 0.9800 . ?
C00X H01J 0.9800 . ?
C00Y C010 1.518(5) . ?
C00Y H01K 0.9900 . ?
C00Y H01L 0.9900 . ?
C00Z H01M 0.9800 . ?
C00Z H01N 0.9800 . ?
C00Z H01O 0.9800 . ?
C010 H01P 0.9800 . ?
C010 H01Q 0.9800 . ?
C010 H01R 0.9800 . ?
C011 H01S 0.9800 . ?
C011 H01T 0.9800 . ?
C011 H01U 0.9800 . ?
C012 H01V 0.9800 . ?
C012 H01W 0.9800 . ?
C012 H01X 0.9800 . ?

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
Cl06 Mn01 Cl05 111.38(3) . . ?
Cl06 Mn01 Cl04 109.14(3) . . ?
Cl05 Mn01 Cl04 109.01(3) . . ?
Cl06 Mn01 Cl07 107.10(3) . . ?
Cl05 Mn01 Cl07 108.34(3) . . ?
Cl04 Mn01 Cl07 111.88(3) . . ?
Cl08 Mn02 Cl09 114.84(3) . . ?
Cl08 Mn02 Cl0A 109.87(4) . . ?
Cl09 Mn02 Cl0A 105.92(3) . . ?
Cl08 Mn02 Cl03 107.91(3) . . ?
Cl09 Mn02 Cl03 108.37(3) . . ?
Cl0A Mn02 Cl03 109.87(3) . . ?
C00G N00B C00J 110.3(2) . . ?
C00G N00B C00H 113.5(2) . . ?
C00J N00B C00H 113.3(2) . . ?
C00P N00C C00R 113.8(2) . . ?
C00P N00C C00F 109.3(2) . . ?
C00R N00C C00F 113.8(2) . . ?
C00L N00D C00T 112.2(2) . . ?
C00L N00D C00Y 113.5(2) . . ?
C00T N00D C00Y 112.1(2) . . ?
C00N N00E C00U 111.1(2) . . ?
C00N N00E C00K 111.7(2) . . ?
C00U N00E C00K 110.9(2) . . ?
N00C C00F C00I 112.2(2) . . ?
N00C C00F H00A 109.2 . . ?
C00I C00F H00A 109.2 . . ?
N00C C00F H00B 109.2 . . ?
C00I C00F H00B 109.2 . . ?
H00A C00F H00B 107.9 . . ?
N00B C00G C00X 112.4(2) . . ?
N00B C00G H00C 109.1 . . ?
C00X C00G H00C 109.1 . . ?
N00B C00G H00D 109.1 . . ?
C00X C00G H00D 109.1 . . ?
H00C C00G H00D 107.8 . . ?
N00B C00H C00Z 114.2(3) . . ?
N00B C00H H00E 108.7 . . ?
C00Z C00H H00E 108.7 . . ?
N00B C00H H00F 108.7 . . ?
C00Z C00H H00F 108.7 . . ?
H00E C00H H00F 107.6 . . ?
C00F C00I H00G 109.5 . . ?
C00F C00I H00H 109.5 . . ?
H00G C00I H00H 109.5 . . ?
C00F C00I H00I 109.5 . . ?
H00G C00I H00I 109.5 . . ?
H00H C00I H00I 109.5 . . ?
N00B C00J C00O 112.7(2) . . ?
N00B C00J H00J 109.1 . . ?
C00O C00J H00J 109.1 . . ?
N00B C00J H00K 109.1 . . ?
C00O C00J H00K 109.1 . . ?
H00J C00J H00K 107.8 . . ?
N00E C00K C00W 113.2(2) . . ?
N00E C00K H00L 108.9 . . ?
C00W C00K H00L 108.9 . . ?
N00E C00K H00M 108.9 . . ?
C00W C00K H00M 108.9 . . ?
H00L C00K H00M 107.8 . . ?
N00D C00L C00S 111.9(2) . . ?
N00D C00L H00N 109.2 . . ?
C00S C00L H00N 109.2 . . ?
N00D C00L H00O 109.2 . . ?
C00S C00L H00O 109.2 . . ?
H00N C00L H00O 107.9 . . ?
C00T C00M H00P 109.5 . . ?
C00T C00M H00Q 109.5 . . ?
H00P C00M H00Q 109.5 . . ?
C00T C00M H00R 109.5 . . ?
H00P C00M H00R 109.5 . . ?
H00Q C00M H00R 109.5 . . ?
N00E C00N C00Q 113.7(2) . . ?
N00E C00N H00S 108.8 . . ?
C00Q C00N H00S 108.8 . . ?
N00E C00N H00T 108.8 . . ?
C00Q C00N H00T 108.8 . . ?
H00S C00N H00T 107.7 . . ?
C00J C00O H00U 109.5 . . ?
C00J C00O H00V 109.5 . . ?
H00U C00O H00V 109.5 . . ?
C00J C00O H00W 109.5 . . ?
H00U C00O H00W 109.5 . . ?
H00V C00O H00W 109.5 . . ?
N00C C00P C011 112.6(3) . . ?
N00C C00P H00X 109.1 . . ?
C011 C00P H00X 109.1 . . ?
N00C C00P H00Y 109.1 . . ?
C011 C00P H00Y 109.1 . . ?
H00X C00P H00Y 107.8 . . ?
C00N C00Q H00Z 109.5 . . ?
C00N C00Q H010 109.5 . . ?
H00Z C00Q H010 109.5 . . ?
C00N C00Q H011 109.5 . . ?
H00Z C00Q H011 109.5 . . ?
H010 C00Q H011 109.5 . . ?
N00C C00R C012 113.1(3) . . ?
N00C C00R H012 109.0 . . ?
C012 C00R H012 109.0 . . ?
N00C C00R H013 109.0 . . ?
C012 C00R H013 109.0 . . ?
H012 C00R H013 107.8 . . ?
C00L C00S H014 109.5 . . ?
C00L C00S H015 109.5 . . ?
H014 C00S H015 109.5 . . ?
C00L C00S H016 109.5 . . ?
H014 C00S H016 109.5 . . ?
H015 C00S H016 109.5 . . ?
N00D C00T C00M 110.8(2) . . ?
N00D C00T H017 109.5 . . ?
C00M C00T H017 109.5 . . ?
N00D C00T H018 109.5 . . ?
C00M C00T H018 109.5 . . ?
H017 C00T H018 108.1 . . ?
N00E C00U C00V 113.1(3) . . ?
N00E C00U H019 109.0 . . ?
C00V C00U H019 109.0 . . ?
N00E C00U H01A 109.0 . . ?
C00V C00U H01A 109.0 . . ?
H019 C00U H01A 107.8 . . ?
C00U C00V H01B 109.5 . . ?
C00U C00V H01C 109.5 . . ?
H01B C00V H01C 109.5 . . ?
C00U C00V H01D 109.5 . . ?
H01B C00V H01D 109.5 . . ?
H01C C00V H01D 109.5 . . ?
C00K C00W H01E 109.5 . . ?
C00K C00W H01F 109.5 . . ?
H01E C00W H01F 109.5 . . ?
C00K C00W H01G 109.5 . . ?
H01E C00W H01G 109.5 . . ?
H01F C00W H01G 109.5 . . ?
C00G C00X H01H 109.5 . . ?
C00G C00X H01I 109.5 . . ?
H01H C00X H01I 109.5 . . ?
C00G C00X H01J 109.5 . . ?
H01H C00X H01J 109.5 . . ?
H01I C00X H01J 109.5 . . ?
N00D C00Y C010 113.9(3) . . ?
N00D C00Y H01K 108.8 . . ?
C010 C00Y H01K 108.8 . . ?
N00D C00Y H01L 108.8 . . ?
C010 C00Y H01L 108.8 . . ?
H01K C00Y H01L 107.7 . . ?
C00H C00Z H01M 109.5 . . ?
C00H C00Z H01N 109.5 . . ?
H01M C00Z H01N 109.5 . . ?
C00H C00Z H01O 109.5 . . ?
H01M C00Z H01O 109.5 . . ?
H01N C00Z H01O 109.5 . . ?
C00Y C010 H01P 109.5 . . ?
C00Y C010 H01Q 109.5 . . ?
H01P C010 H01Q 109.5 . . ?
C00Y C010 H01R 109.5 . . ?
H01P C010 H01R 109.5 . . ?
H01Q C010 H01R 109.5 . . ?
C00P C011 H01S 109.5 . . ?
C00P C011 H01T 109.5 . . ?
H01S C011 H01T 109.5 . . ?
C00P C011 H01U 109.5 . . ?
H01S C011 H01U 109.5 . . ?
H01T C011 H01U 109.5 . . ?
C00R C012 H01V 109.5 . . ?
C00R C012 H01W 109.5 . . ?
H01V C012 H01W 109.5 . . ?
C00R C012 H01X 109.5 . . ?
H01V C012 H01X 109.5 . . ?
H01W C012 H01X 109.5 . . ?

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
C00P N00C C00F C00I -167.4(2) . . . . ?
C00R N00C C00F C00I 64.2(3) . . . . ?
C00J N00B C00G C00X -175.1(2) . . . . ?
C00H N00B C00G C00X 56.5(3) . . . . ?
C00G N00B C00H C00Z 59.7(3) . . . . ?
C00J N00B C00H C00Z -67.1(3) . . . . ?
C00G N00B C00J C00O 161.3(2) . . . . ?
C00H N00B C00J C00O -70.3(3) . . . . ?
C00N N00E C00K C00W -169.9(3) . . . . ?
C00U N00E C00K C00W 65.6(3) . . . . ?
C00T N00D C00L C00S 155.1(3) . . . . ?
C00Y N00D C00L C00S -76.6(3) . . . . ?
C00U N00E C00N C00Q -171.6(3) . . . . ?
C00K N00E C00N C00Q 64.0(3) . . . . ?
C00R N00C C00P C011 -56.1(3) . . . . ?
C00F N00C C00P C011 175.5(3) . . . . ?
C00P N00C C00R C012 -63.9(3) . . . . ?
C00F N00C C00R C012 62.2(3) . . . . ?
C00L N00D C00T C00M -76.3(3) . . . . ?
C00Y N00D C00T C00M 154.6(3) . . . . ?
C00N N00E C00U C00V 65.8(3) . . . . ?
C00K N00E C00U C00V -169.4(3) . . . . ?
C00L N00D C00Y C010 -73.2(3) . . . . ?
C00T N00D C00Y C010 55.1(4) . . . . ?

_refine_diff_density_max         0.742
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.164



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_100_temmnbr2_2_a_pl
_database_code_depnum_ccdc_archive 'CCDC 2178483'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Sejong University
South Korea
;
_audit_update_record             
;
2022-06-11 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H30 Br4 Mn N2'
_chemical_formula_weight         576.96

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'
Br Br -0.2901 2.4595 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.203(2)
_cell_length_b                   12.945(3)
_cell_length_c                   13.940(3)
_cell_angle_alpha                82.61(3)
_cell_angle_beta                 89.09(3)
_cell_angle_gamma                87.74(3)
_cell_volume                     2182.0(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    29283
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       plate
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_F_000             1124
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    7.922
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.536
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21043
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.473
_diffrn_reflns_theta_max         33.896
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.726
_diffrn_measured_fraction_theta_full 0.913
_diffrn_reflns_Laue_measured_fraction_max 0.726
_diffrn_reflns_Laue_measured_fraction_full 0.913
_diffrn_reflns_point_group_measured_fraction_max 0.726
_diffrn_reflns_point_group_measured_fraction_full 0.913
_reflns_number_total             12828
_reflns_number_gt                9288
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.026(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         12828
_refine_ls_number_parameters     356
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1529
_refine_ls_R_factor_gt           0.1335
_refine_ls_wR_factor_ref         0.4028
_refine_ls_wR_factor_gt          0.3863
_refine_ls_goodness_of_fit_ref   1.574
_refine_ls_restrained_S_all      1.574
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.001

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
N1 N 0.6359(6) 0.0612(6) 0.3234(6) 0.0415(14) Uani 1 1 d . . . . .
C1 C 0.7095(8) 0.1530(8) 0.3024(8) 0.050(2) Uani 1 1 d . . . . .
H1A H 0.780089 0.134400 0.332073 0.059 Uiso 1 1 calc R U . . .
H1B H 0.721383 0.166940 0.233084 0.059 Uiso 1 1 calc R U . . .
C2 C 0.6643(11) 0.2506(9) 0.3384(9) 0.061(3) Uani 1 1 d . . . . .
H2A H 0.719905 0.301518 0.333153 0.091 Uiso 1 1 calc R U . . .
H2B H 0.641836 0.235086 0.404779 0.091 Uiso 1 1 calc R U . . .
H2C H 0.602394 0.277543 0.300116 0.091 Uiso 1 1 calc R U . . .
C3 C 0.6236(9) 0.0231(9) 0.4299(7) 0.052(2) Uani 1 1 d . . . . .
H3A H 0.586950 0.077510 0.461647 0.063 Uiso 1 1 calc R U . . .
H3B H 0.577485 -0.036832 0.437735 0.063 Uiso 1 1 calc R U . . .
C4 C 0.7319(10) -0.0068(10) 0.4784(9) 0.059(3) Uani 1 1 d . . . . .
H4A H 0.719391 -0.048571 0.539315 0.089 Uiso 1 1 calc R U . . .
H4B H 0.768406 0.055028 0.488903 0.089 Uiso 1 1 calc R U . . .
H4C H 0.776903 -0.046012 0.437719 0.089 Uiso 1 1 calc R U . . .
C5 C 0.5254(8) 0.0805(9) 0.2766(8) 0.053(2) Uani 1 1 d . . . . .
H5A H 0.482052 0.019435 0.293388 0.063 Uiso 1 1 calc R U . . .
H5B H 0.487737 0.138499 0.302416 0.063 Uiso 1 1 calc R U . . .
C6 C 0.5318(11) 0.1044(12) 0.1681(9) 0.068(3) Uani 1 1 d . . . . .
H6A H 0.568130 0.046940 0.141832 0.102 Uiso 1 1 calc R U . . .
H6B H 0.572386 0.166189 0.150816 0.102 Uiso 1 1 calc R U . . .
H6C H 0.459124 0.115119 0.142512 0.102 Uiso 1 1 calc R U . . .
N2 N 0.2545(7) 0.4475(7) 0.5110(7) 0.0512(18) Uani 1 1 d . . . . .
C7 C 0.2979(10) 0.5422(10) 0.4522(9) 0.062(3) Uani 1 1 d . . . . .
H7A H 0.374493 0.528678 0.436590 0.074 Uiso 1 1 calc R U . . .
H7B H 0.294082 0.599616 0.490603 0.074 Uiso 1 1 calc R U . . .
C8 C 0.2359(15) 0.5736(16) 0.3596(12) 0.094(6) Uani 1 1 d . . . . .
H8A H 0.277775 0.621869 0.317193 0.141 Uiso 1 1 calc R U . . .
H8B H 0.166547 0.606080 0.374015 0.141 Uiso 1 1 calc R U . . .
H8C H 0.223951 0.512922 0.328778 0.141 Uiso 1 1 calc R U . . .
C9 C 0.1390(9) 0.4676(10) 0.5433(10) 0.062(3) Uani 1 1 d . . . . .
H9A H 0.090053 0.464071 0.489698 0.075 Uiso 1 1 calc R U . . .
H9B H 0.131777 0.537466 0.561370 0.075 Uiso 1 1 calc R U . . .
C10 C 0.1048(12) 0.3902(13) 0.6280(11) 0.076(4) Uani 1 1 d . . . . .
H10A H 0.035408 0.412800 0.653137 0.114 Uiso 1 1 calc R U . . .
H10B H 0.158997 0.385867 0.677706 0.114 Uiso 1 1 calc R U . . .
H10C H 0.098241 0.322966 0.607126 0.114 Uiso 1 1 calc R U . . .
C11 C 0.2668(10) 0.3496(10) 0.4653(11) 0.065(3) Uani 1 1 d . . . . .
H11A H 0.225492 0.357988 0.405724 0.078 Uiso 1 1 calc R U . . .
H11B H 0.235914 0.293009 0.508328 0.078 Uiso 1 1 calc R U . . .
C12 C 0.3866(10) 0.3207(10) 0.4428(10) 0.062(3) Uani 1 1 d . . . . .
H12A H 0.393667 0.247754 0.436614 0.094 Uiso 1 1 calc R U . . .
H12B H 0.432226 0.335743 0.494385 0.094 Uiso 1 1 calc R U . . .
H12C H 0.409016 0.360581 0.383362 0.094 Uiso 1 1 calc R U . . .
N3 N 0.7535(7) 0.5502(7) -0.0174(7) 0.0513(18) Uani 1 1 d . . . . .
C13 C 0.7796(12) 0.4346(9) 0.0111(10) 0.067(3) Uani 1 1 d . . . . .
H13A H 0.854889 0.425652 0.032846 0.081 Uiso 1 1 calc R U . . .
H13B H 0.773786 0.399050 -0.045613 0.081 Uiso 1 1 calc R U . . .
C14 C 0.7044(16) 0.3830(11) 0.0911(12) 0.081(4) Uani 1 1 d . . . . .
H14A H 0.629221 0.399020 0.073974 0.122 Uiso 1 1 calc R U . . .
H14B H 0.719237 0.408852 0.150942 0.122 Uiso 1 1 calc R U . . .
H14C H 0.717816 0.308845 0.098449 0.122 Uiso 1 1 calc R U . . .
C15 C 0.7828(13) 0.6090(13) 0.0700(11) 0.077(4) Uani 1 1 d . . . . .
H15A H 0.721444 0.606517 0.115229 0.092 Uiso 1 1 calc R U . . .
H15B H 0.845440 0.573494 0.103393 0.092 Uiso 1 1 calc R U . . .
C16 C 0.8079(15) 0.7163(15) 0.0398(12) 0.091(5) Uani 1 1 d . . . . .
H16A H 0.861630 0.719695 -0.011432 0.137 Uiso 1 1 calc R U . . .
H16B H 0.836421 0.745843 0.093593 0.137 Uiso 1 1 calc R U . . .
H16C H 0.742432 0.754721 0.017269 0.137 Uiso 1 1 calc R U . . .
C17 C 0.6408(11) 0.5787(12) -0.0492(11) 0.075(4) Uani 1 1 d . . . . .
H17A H 0.630330 0.653876 -0.055421 0.089 Uiso 1 1 calc R U . . .
H17B H 0.590047 0.548996 0.000095 0.089 Uiso 1 1 calc R U . . .
C18 C 0.6141(16) 0.5428(17) -0.1422(13) 0.102(6) Uani 1 1 d . . . . .
H18A H 0.548655 0.579043 -0.167650 0.153 Uiso 1 1 calc R U . . .
H18B H 0.602744 0.469224 -0.132075 0.153 Uiso 1 1 calc R U . . .
H18C H 0.673697 0.556813 -0.187181 0.153 Uiso 1 1 calc R U . . .
N4 N 0.1164(7) 0.9487(6) 0.1872(6) 0.0470(17) Uani 1 1 d . . . . .
C19 C 0.0445(9) 0.8755(9) 0.1418(9) 0.057(2) Uani 1 1 d . . . . .
H19A H 0.040085 0.897586 0.072753 0.068 Uiso 1 1 calc R U . . .
H19B H -0.029018 0.879376 0.168894 0.068 Uiso 1 1 calc R U . . .
C20 C 0.0891(16) 0.7633(9) 0.1591(12) 0.084(5) Uani 1 1 d . . . . .
H20A H 0.051847 0.726682 0.213571 0.126 Uiso 1 1 calc R U . . .
H20B H 0.166251 0.762481 0.171873 0.126 Uiso 1 1 calc R U . . .
H20C H 0.077441 0.729805 0.102696 0.126 Uiso 1 1 calc R U . . .
C21 C 0.2297(9) 0.9529(9) 0.1466(8) 0.054(2) Uani 1 1 d . . . . .
H21A H 0.265046 0.884194 0.159346 0.065 Uiso 1 1 calc R U . . .
H21B H 0.270830 1.000108 0.179615 0.065 Uiso 1 1 calc R U . . .
C22 C 0.2341(11) 0.9887(11) 0.0383(9) 0.063(3) Uani 1 1 d . . . . .
H22A H 0.307317 1.007750 0.019661 0.095 Uiso 1 1 calc R U . . .
H22B H 0.184560 1.047779 0.023059 0.095 Uiso 1 1 calc R U . . .
H22C H 0.213057 0.932993 0.003976 0.095 Uiso 1 1 calc R U . . .
C23 C 0.1198(9) 0.9275(10) 0.2957(8) 0.058(3) Uani 1 1 d . . . . .
H23A H 0.167772 0.976335 0.319420 0.070 Uiso 1 1 calc R U . . .
H23B H 0.151119 0.857828 0.314113 0.070 Uiso 1 1 calc R U . . .
C24 C 0.0088(9) 0.9362(9) 0.3436(9) 0.057(2) Uani 1 1 d . . . . .
H24A H 0.016365 0.921634 0.412489 0.085 Uiso 1 1 calc R U . . .
H24B H -0.038828 0.887057 0.321558 0.085 Uiso 1 1 calc R U . . .
H24C H -0.021984 1.005547 0.327209 0.085 Uiso 1 1 calc R U . . .
Br1 Br 0.45853(11) 0.76351(10) 0.08466(8) 0.0634(4) Uani 1 1 d . . . . .
Br2 Br 0.71585(9) 0.83653(10) 0.25453(11) 0.0650(4) Uani 1 1 d . . . . .
Br3 Br 0.40510(8) 0.81306(8) 0.36686(7) 0.0501(3) Uani 1 1 d . . . . .
Br4 Br 0.58153(8) 0.55269(7) 0.30308(8) 0.0497(3) Uani 1 1 d . . . . .
Mn1 Mn 0.53721(12) 0.74450(11) 0.24871(11) 0.0468(3) Uani 1 1 d . . . . .
Br5 Br 0.04357(9) 0.45464(8) 0.17891(8) 0.0527(3) Uani 1 1 d . . . . .
Br6 Br 0.24189(9) 0.20185(11) 0.25011(9) 0.0648(4) Uani 1 1 d . . . . .
Br7 Br -0.03613(9) 0.24815(9) 0.41552(7) 0.0544(3) Uani 1 1 d . . . . .
Br8 Br -0.05017(7) 0.16411(7) 0.13370(7) 0.0455(3) Uani 1 1 d . . . . .
Mn2 Mn 0.04556(12) 0.26540(11) 0.24993(11) 0.0458(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
N1 C5 1.506(12) . ?
N1 C3 1.509(12) . ?
N1 C1 1.513(12) . ?
C1 C2 1.500(16) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.509(15) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.505(16) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
N2 C11 1.492(14) . ?
N2 C7 1.494(15) . ?
N2 C9 1.496(15) . ?
C7 C8 1.508(18) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.51(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.532(17) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N3 C17 1.470(15) . ?
N3 C13 1.521(14) . ?
N3 C15 1.570(16) . ?
C13 C14 1.53(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.44(2) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.48(2) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
N4 C21 1.486(15) . ?
N4 C23 1.503(14) . ?
N4 C19 1.518(13) . ?
C19 C20 1.522(17) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.521(16) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.508(17) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
Br1 Mn1 2.4736(19) . ?
Br2 Mn1 2.5324(19) . ?
Br3 Mn1 2.506(2) . ?
Br4 Mn1 2.5407(19) . ?
Br5 Mn2 2.5207(19) . ?
Br6 Mn2 2.5022(19) . ?
Br7 Mn2 2.487(2) . ?
Br8 Mn2 2.5371(17) . ?

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
C5 N1 C3 110.7(8) . . ?
C5 N1 C1 112.9(7) . . ?
C3 N1 C1 113.6(7) . . ?
C2 C1 N1 113.9(9) . . ?
C2 C1 H1A 108.8 . . ?
N1 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
N1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 N1 112.8(9) . . ?
C4 C3 H3A 109.0 . . ?
N1 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
N1 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 N1 113.4(9) . . ?
C6 C5 H5A 108.9 . . ?
N1 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
N1 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C11 N2 C7 115.0(11) . . ?
C11 N2 C9 112.0(8) . . ?
C7 N2 C9 110.8(9) . . ?
N2 C7 C8 113.0(10) . . ?
N2 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
N2 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 112.4(10) . . ?
N2 C9 H9A 109.1 . . ?
C10 C9 H9A 109.1 . . ?
N2 C9 H9B 109.1 . . ?
C10 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 C12 112.8(9) . . ?
N2 C11 H11A 109.0 . . ?
C12 C11 H11A 109.0 . . ?
N2 C11 H11B 109.0 . . ?
C12 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C17 N3 C13 116.2(10) . . ?
C17 N3 C15 110.4(11) . . ?
C13 N3 C15 108.0(10) . . ?
N3 C13 C14 114.0(11) . . ?
N3 C13 H13A 108.8 . . ?
C14 C13 H13A 108.8 . . ?
N3 C13 H13B 108.8 . . ?
C14 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N3 112.4(13) . . ?
C16 C15 H15A 109.1 . . ?
N3 C15 H15A 109.1 . . ?
C16 C15 H15B 109.1 . . ?
N3 C15 H15B 109.1 . . ?
H15A C15 H15B 107.9 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C18 113.6(15) . . ?
N3 C17 H17A 108.9 . . ?
C18 C17 H17A 108.9 . . ?
N3 C17 H17B 108.9 . . ?
C18 C17 H17B 108.9 . . ?
H17A C17 H17B 107.7 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 N4 C23 110.0(8) . . ?
C21 N4 C19 113.5(8) . . ?
C23 N4 C19 113.5(9) . . ?
N4 C19 C20 111.8(10) . . ?
N4 C19 H19A 109.3 . . ?
C20 C19 H19A 109.3 . . ?
N4 C19 H19B 109.3 . . ?
C20 C19 H19B 109.3 . . ?
H19A C19 H19B 107.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N4 C21 C22 113.5(9) . . ?
N4 C21 H21A 108.9 . . ?
C22 C21 H21A 108.9 . . ?
N4 C21 H21B 108.9 . . ?
C22 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N4 C23 C24 113.5(8) . . ?
N4 C23 H23A 108.9 . . ?
C24 C23 H23A 108.9 . . ?
N4 C23 H23B 108.9 . . ?
C24 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Br1 Mn1 Br3 111.04(7) . . ?
Br1 Mn1 Br2 112.90(8) . . ?
Br3 Mn1 Br2 108.44(7) . . ?
Br1 Mn1 Br4 108.95(7) . . ?
Br3 Mn1 Br4 109.21(7) . . ?
Br2 Mn1 Br4 106.14(7) . . ?
Br7 Mn2 Br6 112.13(7) . . ?
Br7 Mn2 Br5 109.90(7) . . ?
Br6 Mn2 Br5 106.35(8) . . ?
Br7 Mn2 Br8 114.15(7) . . ?
Br6 Mn2 Br8 105.54(7) . . ?
Br5 Mn2 Br8 108.37(6) . . ?

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
C5 N1 C1 C2 61.1(11) . . . . ?
C3 N1 C1 C2 -66.1(11) . . . . ?
C5 N1 C3 C4 174.7(9) . . . . ?
C1 N1 C3 C4 -56.9(12) . . . . ?
C3 N1 C5 C6 -172.0(10) . . . . ?
C1 N1 C5 C6 59.3(12) . . . . ?
C11 N2 C7 C8 65.2(16) . . . . ?
C9 N2 C7 C8 -63.1(16) . . . . ?
C11 N2 C9 C10 69.2(14) . . . . ?
C7 N2 C9 C10 -160.9(10) . . . . ?
C7 N2 C11 C12 59.2(14) . . . . ?
C9 N2 C11 C12 -173.1(11) . . . . ?
C17 N3 C13 C14 -56.5(16) . . . . ?
C15 N3 C13 C14 68.1(15) . . . . ?
C17 N3 C15 C16 -77.6(16) . . . . ?
C13 N3 C15 C16 154.4(13) . . . . ?
C13 N3 C17 C18 -67.7(16) . . . . ?
C15 N3 C17 C18 168.9(13) . . . . ?
C21 N4 C19 C20 62.1(14) . . . . ?
C23 N4 C19 C20 -64.5(14) . . . . ?
C23 N4 C21 C22 -172.1(10) . . . . ?
C19 N4 C21 C22 59.5(12) . . . . ?
C21 N4 C23 C24 172.2(9) . . . . ?
C19 N4 C23 C24 -59.3(13) . . . . ?

_refine_diff_density_max         4.549
_refine_diff_density_min         -3.240
_refine_diff_density_rms         0.357



# start Validation Reply Form
_vrf_PLAT029_100_temmnbr2_2_a_pl 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.913 Why?
RESPONSE: We made many times attempts to obtain better 
quality data for this structure however, most importantly 
due to empty space in crystal structure, disorder, and other
problems such as poor crystal quality etc
However, Goodness-of-fit is close to 1.756. 
We are confidant the structural characterization is valid 
because all molecules are assigned completely.
;
# end Validation Reply Form


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_298_IMMnCl2_a
_database_code_depnum_ccdc_archive 'CCDC 2218868'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Department of Nanotechnology and Advanced Materials Engineering, Sejong University
South Korea
;
_audit_update_record             
;
2022-11-10 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H10 Cl8 Mn2 N4'
_chemical_formula_weight         531.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 '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 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1507 0.1611 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3393 0.7367 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.3290(15)
_cell_length_b                   16.389(3)
_cell_length_c                   16.584(3)
_cell_angle_alpha                95.34(3)
_cell_angle_beta                 90.01(3)
_cell_angle_gamma                90.01(3)
_cell_volume                     1983.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    27798
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_F_000             1040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    2.320
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.865
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20692
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.671
_diffrn_reflns_theta_max         34.147
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.721
_diffrn_measured_fraction_theta_full 0.899
_diffrn_reflns_Laue_measured_fraction_max 0.721
_diffrn_reflns_Laue_measured_fraction_full 0.899
_diffrn_reflns_point_group_measured_fraction_max 0.721
_diffrn_reflns_point_group_measured_fraction_full 0.899
_reflns_number_total             11819
_reflns_number_gt                10750
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.31(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         11819
_refine_ls_number_parameters     362
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1909
_refine_ls_R_factor_gt           0.1856
_refine_ls_wR_factor_ref         0.5224
_refine_ls_wR_factor_gt          0.5137
_refine_ls_goodness_of_fit_ref   2.620
_refine_ls_restrained_S_all      2.620
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
N3 N 0.2493(17) 0.5315(6) 1.0956(4) 0.078(3) Uani 1 1 d . . . . .
H3A H 0.243430 0.562824 1.140128 0.094 Uiso 1 1 calc R U . . .
Cl3 Cl 0.9306(2) 0.64073(7) 0.72808(8) 0.0372(4) Uani 1 1 d . . . . .
Mn3 Mn 0.12086(13) 0.24676(4) 0.75136(4) 0.0350(3) Uani 1 1 d . . . . .
C4 C 0.279(3) 0.5585(8) 1.0215(6) 0.085(4) Uani 1 1 d . . . . .
H4 H 0.308634 0.611567 1.010695 0.102 Uiso 1 1 calc R U . . .
N4 N 0.2591(18) 0.4981(7) 0.9714(4) 0.085(3) Uani 1 1 d . . . . .
H4A H 0.274643 0.499516 0.920182 0.102 Uiso 1 1 calc R U . . .
Cl1 Cl 0.6405(7) 0.7225(3) 0.8711(2) 0.0976(11) Uani 1 1 d . . . . .
N1 N 0.7385(13) 1.0942(4) 1.0365(4) 0.0563(15) Uani 1 1 d . . . . .
H1A H 0.734718 1.140074 1.066219 0.068 Uiso 1 1 calc R U . . .
C1 C 0.7760(18) 1.0224(6) 1.0624(5) 0.065(2) Uani 1 1 d . . . . .
H1B H 0.803595 1.013080 1.115506 0.079 Uiso 1 1 calc R U . . .
Mn1 Mn 0.68203(12) 0.75186(4) 0.74573(4) 0.0332(3) Uani 1 1 d . . . . .
C2 C 0.7069(18) 1.0845(5) 0.9557(4) 0.064(2) Uani 1 1 d . . . . .
H2 H 0.679607 1.125787 0.922789 0.076 Uiso 1 1 calc R U . . .
N2 N 0.7676(12) 0.9662(3) 1.0003(5) 0.0607(17) Uani 1 1 d . . . . .
H2A H 0.786993 0.914589 1.001809 0.073 Uiso 1 1 calc R U . . .
Cl2 Cl 0.4325(2) 0.64800(7) 0.70421(8) 0.0370(4) Uani 1 1 d . . . . .
Mn2 Mn 1.18209(12) 0.74821(4) 0.75429(4) 0.0333(3) Uani 1 1 d . . . . .
C3 C 0.7220(18) 1.0049(5) 0.9320(5) 0.065(2) Uani 1 1 d . . . . .
H3B H 0.705251 0.980022 0.879837 0.078 Uiso 1 1 calc R U . . .
Cl4 Cl 0.7169(2) 0.78458(9) 0.60034(8) 0.0425(4) Uani 1 1 d . . . . .
Mn4 Mn 0.62095(13) 0.25331(4) 0.74876(4) 0.0351(3) Uani 1 1 d . . . . .
C5 C 0.232(3) 0.4561(6) 1.0906(6) 0.087(5) Uani 1 1 d . . . . .
H5 H 0.231651 0.422553 1.132771 0.104 Uiso 1 1 calc R U . . .
N5 N 1.2683(12) 0.5334(3) 0.5015(5) 0.0609(17) Uani 1 1 d . . . . .
H5A H 1.288876 0.584937 0.500626 0.073 Uiso 1 1 calc R U . . .
Cl5 Cl 0.93219(19) 0.85194(7) 0.79563(8) 0.0372(4) Uani 1 1 d . . . . .
C6 C 0.211(3) 0.4315(5) 1.0052(7) 0.085(4) Uani 1 1 d . . . . .
H6 H 0.173971 0.381086 0.980254 0.102 Uiso 1 1 calc R U . . .
N6 N 1.2074(15) 0.4163(5) 0.5436(4) 0.0667(19) Uani 1 1 d . . . . .
H6A H 1.182096 0.377710 0.573480 0.080 Uiso 1 1 calc R U . . .
C7 C 1.218(2) 0.4950(6) 0.5690(5) 0.077(3) Uani 1 1 d . . . . .
H7 H 1.196578 0.519407 0.621001 0.093 Uiso 1 1 calc R U . . .
N7 N 0.731(3) 0.0415(7) 0.4078(6) 0.116(6) Uani 1 1 d . . . . .
H7A H 0.732688 0.072068 0.368405 0.139 Uiso 1 1 calc R U . . .
C8 C 1.2798(17) 0.4760(6) 0.4366(5) 0.069(2) Uani 1 1 d . . . . .
H8 H 1.308776 0.485309 0.383596 0.082 Uiso 1 1 calc R U . . .
N8 N 0.7602(16) 0.0031(6) 0.5290(4) 0.076(3) Uani 1 1 d . . . . .
H8A H 0.786702 0.002670 0.579507 0.092 Uiso 1 1 calc R U . . .
Cl6 Cl 0.4303(2) 0.85926(7) 0.77184(8) 0.0370(4) Uani 1 1 d . . . . .
Cl7 Cl 1.1408(7) 0.7775(3) 0.6285(2) 0.0973(10) Uani 1 1 d . . . . .
Cl8 Cl 1.2171(2) 0.71561(9) 0.89972(7) 0.0423(4) Uani 1 1 d . . . . .
C9 C 1.2423(15) 0.4059(4) 0.4634(4) 0.0540(17) Uani 1 1 d . . . . .
H9 H 1.239777 0.355940 0.431903 0.065 Uiso 1 1 calc R U . . .
Cl9 Cl 0.0831(8) 0.3732(2) 0.7239(2) 0.0980(11) Uani 1 1 d . . . . .
C10 C 0.700(3) 0.0674(5) 0.4966(7) 0.101(6) Uani 1 1 d . . . . .
H10 H 0.652326 0.115976 0.521338 0.121 Uiso 1 1 calc R U . . .
Cl10 Cl -0.1300(2) 0.26908(8) 0.85687(7) 0.0378(4) Uani 1 1 d . . . . .
C11 C 0.775(2) -0.0588(7) 0.4773(6) 0.076(3) Uani 1 1 d . . . . .
H11 H 0.797788 -0.112137 0.489307 0.091 Uiso 1 1 calc R U . . .
Cl11 Cl -0.1291(2) 0.20855(9) 0.64728(7) 0.0411(4) Uani 1 1 d . . . . .
C12 C 0.7519(18) -0.0358(6) 0.4045(4) 0.067(2) Uani 1 1 d . . . . .
H12 H 0.751515 -0.070959 0.357143 0.080 Uiso 1 1 calc R U . . .
Cl12 Cl 0.1551(3) 0.09855(8) 0.78065(9) 0.0454(4) Uani 1 1 d . . . . .
Cl13 Cl 0.3712(2) 0.29144(9) 0.85272(7) 0.0409(4) Uani 1 1 d . . . . .
Cl14 Cl 0.3694(2) 0.23101(8) 0.64312(7) 0.0381(4) Uani 1 1 d . . . . .
Cl15 Cl 0.5830(7) 0.1273(2) 0.7756(2) 0.0961(11) Uani 1 1 d . . . . .
Cl16 Cl 0.6549(3) 0.40153(8) 0.71936(9) 0.0447(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
N3 C5 1.237(13) . ?
N3 C4 1.361(13) . ?
Cl3 Mn2 2.5582(17) . ?
Cl3 Mn1 2.5738(17) . ?
Mn3 Cl9 2.180(4) . ?
Mn3 Cl12 2.5335(16) . ?
Mn3 Cl10 2.5415(17) . ?
Mn3 Cl13 2.5492(18) . ?
Mn3 Cl14 2.5535(18) . ?
Mn3 Cl11 2.5542(17) . ?
C4 N4 1.240(15) . ?
N4 C6 1.321(15) . ?
Cl1 Mn1 2.198(4) . ?
N1 C1 1.319(10) . ?
N1 C2 1.354(9) . ?
C1 N2 1.318(12) . ?
Mn1 Cl4 2.5313(16) . ?
Mn1 Cl5 2.5461(17) . ?
Mn1 Cl2 2.5489(16) . ?
Mn1 Cl6 2.5592(16) . ?
C2 C3 1.331(11) . ?
N2 C3 1.390(12) . ?
Cl2 Mn2 2.5499(17) 1_455 ?
Mn2 Cl7 2.205(4) . ?
Mn2 Cl8 2.5313(15) . ?
Mn2 Cl5 2.5495(16) . ?
Mn2 Cl6 2.5703(17) 1_655 ?
Mn4 Cl15 2.171(4) . ?
Mn4 Cl16 2.5339(17) . ?
Mn4 Cl14 2.5461(17) . ?
Mn4 Cl11 2.5493(19) 1_655 ?
Mn4 Cl13 2.5524(18) . ?
Mn4 Cl10 2.5544(17) 1_655 ?
C5 C6 1.443(15) . ?
N5 C8 1.364(13) . ?
N5 C7 1.383(13) . ?
N6 C7 1.322(12) . ?
N6 C9 1.349(10) . ?
N7 C12 1.273(14) . ?
N7 C10 1.510(17) . ?
C8 C9 1.299(11) . ?
N8 C11 1.272(15) . ?
N8 C10 1.302(15) . ?
C11 C12 1.308(12) . ?

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
C5 N3 C4 111.2(8) . . ?
Mn2 Cl3 Mn1 91.25(4) . . ?
Cl9 Mn3 Cl12 178.09(15) . . ?
Cl9 Mn3 Cl10 88.44(14) . . ?
Cl12 Mn3 Cl10 91.08(6) . . ?
Cl9 Mn3 Cl13 90.50(14) . . ?
Cl12 Mn3 Cl13 91.37(6) . . ?
Cl10 Mn3 Cl13 93.01(5) . . ?
Cl9 Mn3 Cl14 88.85(14) . . ?
Cl12 Mn3 Cl14 91.61(6) . . ?
Cl10 Mn3 Cl14 177.27(5) . . ?
Cl13 Mn3 Cl14 87.38(6) . . ?
Cl9 Mn3 Cl11 86.90(14) . . ?
Cl12 Mn3 Cl11 91.23(6) . . ?
Cl10 Mn3 Cl11 87.53(5) . . ?
Cl13 Mn3 Cl11 177.33(5) . . ?
Cl14 Mn3 Cl11 91.95(5) . . ?
N4 C4 N3 106.3(11) . . ?
C4 N4 C6 112.7(8) . . ?
C1 N1 C2 109.4(7) . . ?
N2 C1 N1 108.4(7) . . ?
Cl1 Mn1 Cl4 177.80(14) . . ?
Cl1 Mn1 Cl5 89.04(13) . . ?
Cl4 Mn1 Cl5 92.84(6) . . ?
Cl1 Mn1 Cl2 87.52(13) . . ?
Cl4 Mn1 Cl2 90.61(6) . . ?
Cl5 Mn1 Cl2 176.46(5) . . ?
Cl1 Mn1 Cl6 87.00(12) . . ?
Cl4 Mn1 Cl6 91.76(6) . . ?
Cl5 Mn1 Cl6 92.98(5) . . ?
Cl2 Mn1 Cl6 87.70(5) . . ?
Cl1 Mn1 Cl3 89.48(13) . . ?
Cl4 Mn1 Cl3 91.74(6) . . ?
Cl5 Mn1 Cl3 87.42(5) . . ?
Cl2 Mn1 Cl3 91.69(5) . . ?
Cl6 Mn1 Cl3 176.45(5) . . ?
C3 C2 N1 107.4(7) . . ?
C1 N2 C3 108.0(6) . . ?
Mn1 Cl2 Mn2 91.99(4) . 1_455 ?
Cl7 Mn2 Cl8 177.88(14) . . ?
Cl7 Mn2 Cl5 87.57(13) . . ?
Cl8 Mn2 Cl5 90.63(6) . . ?
Cl7 Mn2 Cl2 88.90(13) . 1_655 ?
Cl8 Mn2 Cl2 92.92(6) . 1_655 ?
Cl5 Mn2 Cl2 176.38(5) . 1_655 ?
Cl7 Mn2 Cl3 86.98(13) . . ?
Cl8 Mn2 Cl3 91.82(6) . . ?
Cl5 Mn2 Cl3 87.68(5) . . ?
Cl2 Mn2 Cl3 92.91(5) 1_655 . ?
Cl7 Mn2 Cl6 89.43(13) . 1_655 ?
Cl8 Mn2 Cl6 91.75(6) . 1_655 ?
Cl5 Mn2 Cl6 91.75(5) . 1_655 ?
Cl2 Mn2 Cl6 87.44(5) 1_655 1_655 ?
Cl3 Mn2 Cl6 176.39(5) . 1_655 ?
C2 C3 N2 106.8(7) . . ?
Cl15 Mn4 Cl16 178.10(15) . . ?
Cl15 Mn4 Cl14 88.30(13) . . ?
Cl16 Mn4 Cl14 90.99(6) . . ?
Cl15 Mn4 Cl11 90.38(14) . 1_655 ?
Cl16 Mn4 Cl11 91.41(7) . 1_655 ?
Cl14 Mn4 Cl11 92.99(5) . 1_655 ?
Cl15 Mn4 Cl13 86.98(14) . . ?
Cl16 Mn4 Cl13 91.23(6) . . ?
Cl14 Mn4 Cl13 87.47(5) . . ?
Cl11 Mn4 Cl13 177.31(5) 1_655 . ?
Cl15 Mn4 Cl10 89.04(13) . 1_655 ?
Cl16 Mn4 Cl10 91.65(6) . 1_655 ?
Cl14 Mn4 Cl10 177.32(5) . 1_655 ?
Cl11 Mn4 Cl10 87.36(5) 1_655 1_655 ?
Cl13 Mn4 Cl10 92.05(5) . 1_655 ?
N3 C5 C6 105.3(8) . . ?
C8 N5 C7 108.9(6) . . ?
Mn1 Cl5 Mn2 92.09(4) . . ?
N4 C6 C5 102.8(8) . . ?
C7 N6 C9 109.4(7) . . ?
N6 C7 N5 105.1(7) . . ?
C12 N7 C10 104.4(8) . . ?
C9 C8 N5 106.4(8) . . ?
C11 N8 C10 112.0(8) . . ?
Mn1 Cl6 Mn2 91.28(4) . 1_455 ?
C8 C9 N6 110.1(7) . . ?
N8 C10 N7 100.9(10) . . ?
Mn3 Cl10 Mn4 92.00(5) . 1_455 ?
N8 C11 C12 109.4(10) . . ?
Mn4 Cl11 Mn3 91.83(5) 1_455 . ?
N7 C12 C11 110.3(8) . . ?
Mn3 Cl13 Mn4 91.91(5) . . ?
Mn4 Cl14 Mn3 91.96(5) . . ?

_refine_diff_density_max         6.674
_refine_diff_density_min         -2.627
_refine_diff_density_rms         0.440



# start Validation Reply Form
_vrf_PLAT029_298_IMMnCl2_a       
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .    0.899 Why?  
RESPONSE: We made many times attempts to obtain better 
quality data for this structure however, most importantly 
due to empty space in crystal structure, disorder, and other
problems such as poor crystal quality etc
We are confidant the structural characterization is valid 
because all molecules are assigned completely.
;
# end Validation Reply Form

# start Validation Reply Form
_vrf_PLAT084_298_IMMnCl2_a       
;
PROBLEM: _A High wR2 Value (i.e. > 0.25) ...................       0.52 Report
RESPONSE: These alerts are generated 
because there is a large amount of disorder of TEM 
cation in the structure.
;
# end Validation Reply Form

# start Validation Reply Form
_vrf_PLAT097_298_IMMnCl2_a       
;
PROBLEM: _A Large Reported Max.  (Positive) Residual Density       6.67 eA-3  
RESPONSE: These alerts are generated 
because there is a large amount of disorder of TEM 
cation in the structure.
;
# end Validation Reply Form






####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_298_immnbr2_a_pl
_database_code_depnum_ccdc_archive 'CCDC 2178482'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Sejong University
South Korea
;
_audit_update_record             
;
2022-06-11 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H15 Br5 Mn N6'
_chemical_formula_weight         661.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 '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 -0.2713 2.4705 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3393 0.7367 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   12.568(3)
_cell_length_b                   12.568(3)
_cell_length_c                   25.478(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4024(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    23596
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.184
_exptl_crystal_F_000             2488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    10.600
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.326
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18802
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_av_R_equivalents  0.1503
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.807
_diffrn_reflns_theta_max         34.159
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3720
_reflns_number_gt                3354
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0874P)²+8.3545P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0093(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3720
_refine_ls_number_parameters     97
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.1785
_refine_ls_wR_factor_gt          0.1748
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
N1 N 0.2896(4) 0.0515(4) 0.28441(18) 0.0651(11) Uani 1 1 d . . . . .
H13 H 0.347159 0.070029 0.300274 0.078 Uiso 1 1 d R U . . .
C2 C 0.4988(10) 0.2050(12) 0.0593(3) 0.144(9) Uani 1 1 d . . . . .
H21 H 0.496407 0.167807 0.030967 0.173 Uiso 1 1 d R U . . .
N2 N 0.1396(5) -0.0186(6) 0.2659(4) 0.108(3) Uani 1 1 d . . . . .
H2 H 0.081653 -0.054924 0.267410 0.129 Uiso 1 1 d R U . . .
C00I C 0.1728(4) 0.0422(4) 0.22624(18) 0.0546(10) Uani 1 1 d . . . . .
H00I H 0.136821 0.052161 0.194718 0.066 Uiso 1 1 calc R U . . .
C00O C 0.2608(5) 0.0842(4) 0.2382(2) 0.0633(12) Uani 1 1 d . . . . .
H00O H 0.298928 0.131285 0.217272 0.076 Uiso 1 1 calc R U . . .
C00Y C 0.2156(6) -0.0128(5) 0.3035(2) 0.0784(16) Uani 1 1 d . . . . .
H00Y H 0.215725 -0.046757 0.335928 0.094 Uiso 1 1 calc R U . . .
Br01 Br 0.21473(3) 0.23978(3) 0.12175(2) 0.03993(15) Uani 1 1 d . . . . .
Br05 Br 0.000000 0.250000 0.01639(2) 0.04506(17) Uani 1 2 d S T P . .
Mn1 Mn 0.000000 0.250000 0.125000 0.0373(2) Uani 1 4 d S T P . .
C1 C 0.500000 0.250000 0.1386(2) 0.0616(19) Uani 1 2 d S T P . .
H1 H 0.500000 0.250000 0.172354 0.074 Uiso 1 2 d R U P . .
N4 N 0.5022(5) 0.1662(7) 0.1071(5) 0.137(3) Uani 1 1 d . . . . .
H4 H 0.505278 0.100312 0.116085 0.165 Uiso 1 1 calc R U . . .
Br07 Br 0.40735(6) 0.62050(5) 0.06631(2) 0.0750(2) Uani 1 1 d . . . . .
Mn0C Mn 0.500000 0.750000 0.125000 0.0449(3) Uani 1 4 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
N1 C00O 1.298(7) . ?
N1 C00Y 1.325(8) . ?
N1 H13 0.8602 . ?
C2 C2 1.13(3) 7_554 ?
C2 N4 1.313(13) . ?
C2 H21 0.8600 . ?
N2 C00I 1.334(10) . ?
N2 C00Y 1.355(10) . ?
N2 H2 0.8603 . ?
C00I C00O 1.263(8) . ?
C00I H00I 0.9300 . ?
C00O H00O 0.9300 . ?
C00Y H00Y 0.9300 . ?
Br01 Mn1 2.7030(7) . ?
Br05 Mn1 2.7673(14) . ?
C1 N4 1.324(11) 7_554 ?
C1 N4 1.324(11) . ?
C1 H1 0.8599 . ?
N4 H4 0.8600 . ?
Br07 Mn0C 2.4981(8) . ?

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
C00O N1 C00Y 109.2(5) . . ?
C00O N1 H13 125.1 . . ?
C00Y N1 H13 125.6 . . ?
C2 C2 N4 111.7(7) 7_554 . ?
C2 C2 H21 122.9 7_554 . ?
N4 C2 H21 125.3 . . ?
C00I N2 C00Y 106.5(5) . . ?
C00I N2 H2 127.1 . . ?
C00Y N2 H2 126.4 . . ?
C00O C00I N2 109.3(5) . . ?
C00O C00I H00I 125.4 . . ?
N2 C00I H00I 125.4 . . ?
C00I C00O N1 109.4(5) . . ?
C00I C00O H00O 125.3 . . ?
N1 C00O H00O 125.3 . . ?
N1 C00Y N2 105.6(5) . . ?
N1 C00Y H00Y 127.2 . . ?
N2 C00Y H00Y 127.2 . . ?
Br01 Mn1 Br01 176.489(14) 12_666 14 ?
Br01 Mn1 Br01 90.1 12_666 7_454 ?
Br01 Mn1 Br01 90.1 14 7_454 ?
Br01 Mn1 Br01 90.054(1) 12_666 . ?
Br01 Mn1 Br01 90.1 14 . ?
Br01 Mn1 Br01 176.489(14) 7_454 . ?
Br01 Mn1 Br05 88.245(7) 12_666 14 ?
Br01 Mn1 Br05 88.245(7) 14 14 ?
Br01 Mn1 Br05 91.755(7) 7_454 14 ?
Br01 Mn1 Br05 91.755(7) . 14 ?
Br01 Mn1 Br05 91.755(7) 12_666 . ?
Br01 Mn1 Br05 91.755(7) 14 . ?
Br01 Mn1 Br05 88.245(7) 7_454 . ?
Br01 Mn1 Br05 88.245(7) . . ?
Br05 Mn1 Br05 180.0 14 . ?
N4 C1 N4 105.4(11) 7_554 . ?
N4 C1 H1 127.3 7_554 . ?
N4 C1 H1 127.3 . . ?
C2 N4 C1 105.5(9) . . ?
C2 N4 H4 127.3 . . ?
C1 N4 H4 127.3 . . ?
Br07 Mn0C Br07 111.00(2) . 12_766 ?
Br07 Mn0C Br07 110.99(2) . 14_565 ?
Br07 Mn0C Br07 106.46(4) 12_766 14_565 ?
Br07 Mn0C Br07 106.46(4) . 7_564 ?
Br07 Mn0C Br07 111.00(2) 12_766 7_564 ?
Br07 Mn0C Br07 111.00(2) 14_565 7_564 ?

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
C00Y N2 C00I C00O -1.2(7) . . . . ?
N2 C00I C00O N1 1.6(7) . . . . ?
C00Y N1 C00O C00I -1.4(7) . . . . ?
C00O N1 C00Y N2 0.7(7) . . . . ?
C00I N2 C00Y N1 0.3(8) . . . . ?
C2 C2 N4 C1 4.2(18) 7_554 . . . ?
N4 C1 N4 C2 -1.4(6) 7_554 . . . ?

_refine_diff_density_max         1.099
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.299



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_298_TEMMnBr2_a
_database_code_depnum_ccdc_archive 'CCDC 2178485'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Sejong University
South Korea
;
_audit_update_record             
;
2022-06-11 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H26 Br4 Mn N2'
_chemical_formula_weight         572.93

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'
Mn Mn 0.3368 0.7283 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.149(3)
_cell_length_b                   12.377(3)
_cell_length_c                   13.958(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.28(3)
_cell_angle_gamma                90
_cell_volume                     2257.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    35429
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_F_000             1108
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    7.655
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21609
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.205
_diffrn_reflns_theta_max         33.885
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.797
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.797
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7287
_reflns_number_gt                3144
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.033(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7287
_refine_ls_number_parameters     179
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1692
_refine_ls_R_factor_gt           0.1168
_refine_ls_wR_factor_ref         0.4726
_refine_ls_wR_factor_gt          0.4228
_refine_ls_goodness_of_fit_ref   1.467
_refine_ls_restrained_S_all      1.467
_refine_ls_shift/su_max          1.090
_refine_ls_shift/su_mean         0.063

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
C2 C 0.8947(19) 0.1033(14) 0.3697(15) 0.202(9) Uani 1 1 d . . . . .
H2A H 0.824795 0.097133 0.382857 0.303 Uiso 1 1 calc R U . . .
H2B H 0.920304 0.033134 0.355347 0.303 Uiso 1 1 calc R U . . .
H2C H 0.898657 0.150306 0.315589 0.303 Uiso 1 1 calc R U . . .
Br3 Br 0.65993(14) 0.55563(13) 0.36105(9) 0.1505(7) Uani 1 1 d . . . . .
N2 N 0.4434(5) 0.3764(7) 0.3108(5) 0.107(2) Uani 1 1 d . . . . .
Mn1 Mn 0.75936(10) 0.45683(11) 0.24580(10) 0.0991(6) Uani 1 1 d . . . . .
N1 N 0.9452(7) 0.2534(7) 0.4801(7) 0.127(3) Uani 1 1 d D . . . .
C1 C 0.950(2) 0.1428(11) 0.4449(19) 0.30(2) Uani 1 1 d D . . . .
H1A H 1.020240 0.130470 0.434222 0.360 Uiso 1 1 calc R U . . .
H1B H 0.936474 0.096946 0.498513 0.360 Uiso 1 1 calc R U . . .
Br1 Br 0.94471(8) 0.43565(12) 0.30556(10) 0.1372(6) Uani 1 1 d . . . . .
Br2 Br 0.74609(12) 0.54782(12) 0.08668(8) 0.1409(7) Uani 1 1 d . . . . .
C3 C 1.0572(13) 0.2826(15) 0.5233(13) 0.176(7) Uani 1 1 d . . . . .
H3A H 1.101571 0.274489 0.472589 0.212 Uiso 1 1 calc R U . . .
H3B H 1.058399 0.358232 0.541483 0.212 Uiso 1 1 calc R U . . .
Br4 Br 0.68036(15) 0.27339(14) 0.23725(15) 0.1791(8) Uani 1 1 d . . . . .
C4 C 1.0983(15) 0.223(2) 0.602(2) 0.250(14) Uani 1 1 d . . . . .
H4A H 1.056985 0.160591 0.608795 0.374 Uiso 1 1 calc R U . . .
H4B H 1.100079 0.266992 0.658894 0.374 Uiso 1 1 calc R U . . .
H4C H 1.166603 0.201528 0.592511 0.374 Uiso 1 1 calc R U . . .
C5 C 0.872(3) 0.276(3) 0.544(2) 0.300(19) Uani 1 1 d . . . . .
H5A H 0.822220 0.217207 0.535314 0.360 Uiso 1 1 calc R U . . .
H5B H 0.906942 0.266409 0.608416 0.360 Uiso 1 1 calc R U . . .
C6 C 0.815(2) 0.368(2) 0.5480(14) 0.225(11) Uani 1 1 d . . . . .
H6A H 0.797322 0.394346 0.483859 0.338 Uiso 1 1 calc R U . . .
H6B H 0.854957 0.420955 0.585432 0.338 Uiso 1 1 calc R U . . .
H6C H 0.754321 0.352087 0.577347 0.338 Uiso 1 1 calc R U . . .
C7 C 0.3675(16) 0.450(3) 0.348(4) 0.50(6) Uani 1 1 d D . . . .
H7A H 0.390026 0.466128 0.414891 0.600 Uiso 1 1 calc R U . . .
H7B H 0.367004 0.517353 0.312363 0.600 Uiso 1 1 calc R U . . .
C8 C 0.2627(16) 0.409(3) 0.3416(19) 0.260(14) Uani 1 1 d D . . . .
H8A H 0.217744 0.457193 0.303690 0.391 Uiso 1 1 calc R U . . .
H8B H 0.241731 0.403083 0.405197 0.391 Uiso 1 1 calc R U . . .
H8C H 0.259824 0.338662 0.311857 0.391 Uiso 1 1 calc R U . . .
C9 C 0.4616(16) 0.2636(15) 0.3576(13) 0.212(10) Uani 1 1 d D . . . .
H9A H 0.397775 0.223553 0.350753 0.254 Uiso 1 1 calc R U . . .
H9B H 0.510409 0.224224 0.323691 0.254 Uiso 1 1 calc R U . . .
C10 C 0.5001(15) 0.2703(16) 0.4600(12) 0.176(6) Uani 1 1 d D . . . .
H10A H 0.548621 0.328236 0.469704 0.264 Uiso 1 1 calc R U . . .
H10B H 0.532709 0.203439 0.480163 0.264 Uiso 1 1 calc R U . . .
H10C H 0.444088 0.283538 0.497165 0.264 Uiso 1 1 calc R U . . .
C11 C 0.4186(18) 0.366(3) 0.205(2) 0.32(2) Uani 1 1 d . . . . .
H11A H 0.353096 0.330072 0.191471 0.379 Uiso 1 1 calc R U . . .
H11B H 0.469968 0.321109 0.179701 0.379 Uiso 1 1 calc R U . . .
C12 C 0.4141(18) 0.4760(15) 0.1522(14) 0.173(6) Uani 1 1 d . . . . .
H12A H 0.462830 0.476536 0.105826 0.260 Uiso 1 1 calc R U . . .
H12B H 0.429929 0.532855 0.198200 0.260 Uiso 1 1 calc R U . . .
H12C H 0.346570 0.486877 0.119895 0.260 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C2 C1 1.30(3) . ?
Br3 Mn1 2.5005(19) . ?
N2 C11 1.48(3) . ?
N2 C7 1.49(3) . ?
N2 C9 1.55(2) . ?
Mn1 Br2 2.4793(19) . ?
Mn1 Br4 2.494(2) . ?
Mn1 Br1 2.5019(18) . ?
N1 C5 1.42(2) . ?
N1 C1 1.458(9) . ?
N1 C3 1.570(19) . ?
C3 C4 1.38(3) . ?
C5 C6 1.36(3) . ?
C7 C8 1.464(10) . ?
C9 C10 1.465(10) . ?
C11 C12 1.54(5) . ?

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
C11 N2 C7 109(2) . . ?
C11 N2 C9 110.4(17) . . ?
C7 N2 C9 119(2) . . ?
Br2 Mn1 Br4 112.49(8) . . ?
Br2 Mn1 Br3 111.33(7) . . ?
Br4 Mn1 Br3 103.39(8) . . ?
Br2 Mn1 Br1 108.46(7) . . ?
Br4 Mn1 Br1 107.82(8) . . ?
Br3 Mn1 Br1 113.31(8) . . ?
C5 N1 C1 116.7(19) . . ?
C5 N1 C3 113(2) . . ?
C1 N1 C3 106.0(14) . . ?
C2 C1 N1 126.0(19) . . ?
C4 C3 N1 116.9(14) . . ?
C6 C5 N1 127(2) . . ?
C8 C7 N2 115(2) . . ?
C10 C9 N2 112.4(14) . . ?
N2 C11 C12 113.0(19) . . ?

_refine_diff_density_max         2.085
_refine_diff_density_min         -2.111
_refine_diff_density_rms         0.158



# start Validation Reply Form
_vrf_SHFSU01_298_TEMMnBr2_a      
;
PROBLEM: _The absolute value of parameter shift to su ratio > 0.20
Absolute value of the parameter shift to su ratio given 1.090
Additional refinement cycles may be required.
RESPONSE: We made many times attempts to obtain better 
quality data for this structure however, most importantly 
due to empty space in crystal structure,these alerts are 
generated because there is a large amount of disorder of TEM 
cation in the structure.
;
# end Validation Reply Form

# start Validation Reply Form
_vrf_PLAT080_298_TEMMnBr2_a      
;
PROBLEM: _A Maximum Shift Error .......1.09 Why ?
RESPONSE: These alerts are generated 
because there is a large amount of disorder of TEM 
cation in the structure.
;
# end Validation Reply Form

# start Validation Reply Form
_vrf_PLAT084_298_TEMMnBr2_a      
;
PROBLEM: _High wR2 Value (i.e. > 0.25) . 0.47 Report
RESPONSE: We made many times attempts to obtain better 
quality data for this structure however, most importantly 
due to empty space in crystal structure, disorder, and other
problems such as poor crystal quality etc. the R2 value is 
inevitably high. However, Goodness-of-fit is close to 1.685. 
We are confidant the structural characterization is valid 
because all molecules are assigned completely.
;
# end Validation Reply Form

# start Validation Reply Form
_vrf_PLAT234_298_TEMMnBr2_a      
;
PROBLEM: _A Large Hirshfeld Difference C1 --C2 . 0.35 Ang.
RESPONSE: These alerts are generated 
because there is a large amount of disorder of TEM 
cation in the structure.
;
# end Validation Reply Form

# start Validation Reply Form
_vrf_PLAT241_298_TEMMnBr2_a      
;
PROBLEM: _A High MainMol Ueq as Compared to Neighbors of C7 Check
RESPONSE: These alerts are generated 
because there is a large amount of disorder of TEM 
cation in the structure.
;
# end Validation Reply Form

# start Validation Reply Form
_vrf_PLAT242_298_TEMMnBr2_a      
;
PROBLEM: _A Low MainMol Ueq as Compared to Neighbors of N2 Check
RESPONSE: These alerts are generated 
because there is a large amount of disorder of TEM 
cation in the structure.
;
# end Validation Reply Form









####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_100_immnbr2_a_pl
_database_code_depnum_ccdc_archive 'CCDC 2178484'
loop_
_audit_author_name
_audit_author_address
'Mi-Hee Jung'
;Sejong University
South Korea
;
_audit_update_record             
;
2022-06-11 deposited with the CCDC.	2023-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H15 Br5 Mn N6'
_chemical_formula_weight         661.76

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'
Br Br -0.2901 2.4595 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   12.413(3)
_cell_length_b                   12.413(3)
_cell_length_c                   25.463(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3923(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    23942
_cell_measurement_theta_min      0.401
_cell_measurement_theta_max      33.749

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.241
_exptl_crystal_F_000             2488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    10.858
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.411
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16373
_diffrn_reflns_av_unetI/netI     0.1122
_diffrn_reflns_av_R_equivalents  0.1984
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.825
_diffrn_reflns_theta_max         33.966
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3627
_reflns_number_gt                3516
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1285P)²+29.0206P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0091(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3627
_refine_ls_number_parameters     97
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0784
_refine_ls_wR_factor_ref         0.2204
_refine_ls_wR_factor_gt          0.2182
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
N1 N 0.2885(4) 0.4192(3) -0.02412(17) 0.0249(8) Uani 1 1 d . . . . .
H1A H 0.296909 0.384293 -0.053013 0.030 Uiso 1 1 d R U . . .
C2 C 0.4512(13) 0.2501(7) 0.1906(3) 0.097(7) Uani 1 1 d . . . . .
H21 H 0.412926 0.249387 0.218779 0.116 Uiso 1 1 d R U . . .
N2 N 0.3022(4) 0.5414(4) 0.03460(17) 0.0239(8) Uani 1 1 d . . . . .
H22 H 0.321512 0.599482 0.050366 0.029 Uiso 1 1 d R U . . .
C1 C 0.3334(4) 0.5122(4) -0.0125(2) 0.0233(8) Uani 1 1 d . . . . .
H1 H 0.379698 0.550928 -0.034142 0.028 Uiso 1 1 calc R U . . .
C00R C 0.2354(5) 0.4651(5) 0.0544(2) 0.0291(10) Uani 1 1 d . . . . .
H00R H 0.201905 0.466371 0.087084 0.035 Uiso 1 1 calc R U . . .
C00X C 0.2266(5) 0.3867(5) 0.0177(3) 0.0307(11) Uani 1 1 d . . . . .
H00X H 0.186643 0.323593 0.020225 0.037 Uiso 1 1 calc R U . . .
Br01 Br 0.28363(3) 0.73920(3) 0.12226(2) 0.01179(18) Uani 1 1 d . . . . .
Br04 Br 0.500000 0.750000 0.01676(2) 0.01457(19) Uani 1 2 d S T P . .
Mn1 Mn 0.500000 0.750000 0.125000 0.0108(3) Uani 1 4 d S T P . .
N6 N 0.4129(7) 0.2523(5) 0.1412(5) 0.071(3) Uani 1 1 d . . . . .
H6 H 0.347245 0.254924 0.130402 0.085 Uiso 1 1 d R U . . .
C00N C 0.500000 0.250000 0.1109(3) 0.0240(14) Uani 1 2 d S T P . .
H00N H 0.500000 0.250000 0.074327 0.029 Uiso 1 2 d R U P . .
Br07 Br 0.09191(5) 0.11728(4) 0.06605(2) 0.0309(2) Uani 1 1 d . . . . .
Mn0C Mn 0.000000 0.250000 0.125000 0.0165(3) Uani 1 4 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
N1 C1 1.316(7) . ?
N1 C00X 1.373(8) . ?
N1 H1A 0.8600 . ?
C2 C2 1.21(3) 7_554 ?
C2 N6 1.345(15) . ?
C2 H21 0.8602 . ?
N2 C1 1.311(7) . ?
N2 C00R 1.356(7) . ?
N2 H22 0.8599 . ?
C1 H1 0.9300 . ?
C00R C00X 1.354(9) . ?
C00R H00R 0.9300 . ?
C00X H00X 0.9300 . ?
Br01 Mn1 2.6901(8) . ?
Br04 Mn1 2.7560(14) . ?
N6 C00N 1.330(9) . ?
N6 H6 0.8601 . ?
C00N H00N 0.9302 . ?
Br07 Mn0C 2.5038(8) . ?

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
C1 N1 C00X 108.7(4) . . ?
C1 N1 H1A 125.7 . . ?
C00X N1 H1A 125.7 . . ?
C2 C2 N6 110.7(7) 7_554 . ?
C2 C2 H21 123.5 7_554 . ?
N6 C2 H21 125.8 . . ?
C1 N2 C00R 109.2(4) . . ?
C1 N2 H22 125.2 . . ?
C00R N2 H22 125.6 . . ?
N2 C1 N1 108.8(5) . . ?
N2 C1 H1 125.6 . . ?
N1 C1 H1 125.6 . . ?
C00X C00R N2 107.1(5) . . ?
C00X C00R H00R 126.5 . . ?
N2 C00R H00R 126.5 . . ?
C00R C00X N1 106.3(4) . . ?
C00R C00X H00X 126.9 . . ?
N1 C00X H00X 126.9 . . ?
Br01 Mn1 Br01 90.0 7_564 14_565 ?
Br01 Mn1 Br01 90.0 7_564 12_766 ?
Br01 Mn1 Br01 177.021(16) 14_565 12_766 ?
Br01 Mn1 Br01 177.023(15) 7_564 . ?
Br01 Mn1 Br01 90.0 14_565 . ?
Br01 Mn1 Br01 90.0 12_766 . ?
Br01 Mn1 Br04 88.510(8) 7_564 . ?
Br01 Mn1 Br04 91.490(8) 14_565 . ?
Br01 Mn1 Br04 91.490(8) 12_766 . ?
Br01 Mn1 Br04 88.512(8) . . ?
Br01 Mn1 Br04 91.490(8) 7_564 14_565 ?
Br01 Mn1 Br04 88.510(8) 14_565 14_565 ?
Br01 Mn1 Br04 88.510(8) 12_766 14_565 ?
Br01 Mn1 Br04 91.488(8) . 14_565 ?
Br04 Mn1 Br04 180.0 . 14_565 ?
C00N N6 C2 104.8(9) . . ?
C00N N6 H6 125.8 . . ?
C2 N6 H6 129.4 . . ?
N6 C00N N6 109.0(11) 7_554 . ?
N6 C00N H00N 125.5 7_554 . ?
N6 C00N H00N 125.5 . . ?
Br07 Mn0C Br07 111.07(2) . 12_666 ?
Br07 Mn0C Br07 111.06(2) . 14 ?
Br07 Mn0C Br07 106.33(4) 12_666 14 ?
Br07 Mn0C Br07 106.33(4) . 7_454 ?
Br07 Mn0C Br07 111.07(2) 12_666 7_454 ?
Br07 Mn0C Br07 111.07(2) 14 7_454 ?

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
C00R N2 C1 N1 0.3(6) . . . . ?
C00X N1 C1 N2 -0.7(6) . . . . ?
C1 N2 C00R C00X 0.2(6) . . . . ?
N2 C00R C00X N1 -0.6(6) . . . . ?
C1 N1 C00X C00R 0.8(6) . . . . ?
C2 C2 N6 C00N 2.0(12) 7_554 . . . ?
C2 N6 C00N N6 -0.7(4) . . . 7_554 ?

_refine_diff_density_max         4.902
_refine_diff_density_min         -4.011
_refine_diff_density_rms         0.475



