# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2014526'
loop_
_audit_author_name
_audit_author_address
'Qing-Lun Wang'
;NANKAI University
China
;
_audit_update_record             
;
2021-09-17 deposited with the CCDC.	2021-11-01 downloaded from the CCDC.
;
_audit_creation_date             2020-02-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(Cl8 Mn2), C3 H12 N2'
_chemical_formula_sum            'C3 H12 Cl4 Mn N2'
_chemical_formula_weight         272.89
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     ' '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_H-M_alt        'I m m a'
_space_group_name_Hall           '-I 2b 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z'
'-x, y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z'
'x, -y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y, z+1/2'

_cell_length_a                   7.1701(9)
_cell_length_b                   18.986(2)
_cell_length_c                   7.3547(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1001.2(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1259
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.7740
_cell_measurement_theta_min      8.6440
_shelx_estimated_absorpt_T_max   0.690
_shelx_estimated_absorpt_T_min   0.585
_exptl_absorpt_coefficient_mu    20.050
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42679
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            1344
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        64.939
_diffrn_reflns_theta_max         64.939
_diffrn_reflns_theta_min         4.658
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -28.00  25.00   0.50    0.85    --    0.00  57.00  60.00  106
  2  ω     56.00  83.00   0.50    0.85    --    0.00  57.00  60.00   54
  3  ω    -28.00  22.00   0.50    0.85    --    0.00  57.00-180.00  100
  4  ω     22.00 104.00   0.50    3.41    --   97.60 -45.00  90.00  164
  5  ω     12.00 111.00   0.50    3.41    --   97.60 -61.00 -30.00  198
  6  ω      9.00  36.00   0.50    3.41    --   97.60 -61.00  90.00   54
  7  ω     91.00 116.00   0.50    3.41    --   97.60 -61.00  90.00   50
  8  ω     96.00 122.00   0.50    3.41    --   97.60 -45.00 -30.00   52
  9  ω      9.00  80.00   0.50    3.41    --   97.60 -45.00 -30.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0720166000
_diffrn_orient_matrix_UB_12      0.0935647000
_diffrn_orient_matrix_UB_13      -0.0241638000
_diffrn_orient_matrix_UB_21      -0.0109607000
_diffrn_orient_matrix_UB_22      -0.0044028000
_diffrn_orient_matrix_UB_23      0.2129001000
_diffrn_orient_matrix_UB_31      0.0357893000
_diffrn_orient_matrix_UB_32      0.1872737000
_diffrn_orient_matrix_UB_33      0.0165268000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                460
_reflns_number_total             481
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.100
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         481
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0654
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1046P)²+1.4692P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1596
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
2. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.25) H1E(0.25) H2A(0.5) H2B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.000000 0.500000 0.000000 0.0220(6) Uani 1 4 d S T P . .
Cl1 Cl 0.250000 0.48583(8) 0.250000 0.0404(6) Uani 1 2 d S T P . .
Cl2 Cl 0.000000 0.62981(8) 0.0465(2) 0.0360(6) Uani 1 2 d S T P . .
N1 N 0.000000 0.6193(3) 0.4790(8) 0.0452(18) Uani 1 2 d S T P . .
H1A H -0.062937 0.588242 0.545773 0.054 Uiso 0.5 1 calc GR . . A -1
H1B H 0.116913 0.604526 0.464903 0.054 Uiso 0.5 1 calc GR . . A -1
H1C H -0.053976 0.623514 0.370607 0.054 Uiso 0.5 1 calc GR . . A -1
C1 C 0.000000 0.750000 0.4709(15) 0.061(4) Uani 1 4 d S T P . .
H1D H 0.108642 0.750000 0.392298 0.073 Uiso 0.5 2 calc RS T P . .
H1E H -0.108642 0.750000 0.392298 0.073 Uiso 0.5 2 calc RS T P . .
C2 C 0.000000 0.6849(4) 0.5671(10) 0.061(3) Uani 1 2 d S T P . .
H2A H 0.108449 0.685506 0.645881 0.074 Uiso 0.5 1 calc R . . . .
H2B H -0.108449 0.685506 0.645881 0.074 Uiso 0.5 1 calc R . . . .


_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
Mn1 Cl1 2.5819(3) 9_565 ?
Mn1 Cl1 2.5819(3) 6_554 ?
Mn1 Cl1 2.5819(3) . ?
Mn1 Cl1 2.5819(3) 14_455 ?
Mn1 Cl2 2.4880(15) . ?
Mn1 Cl2 2.4880(15) 9_565 ?
Cl1 Mn1 2.5819(3) 6 ?
N1 C2 1.404(9) . ?
C1 C2 1.424(9) . ?
C1 C2 1.424(9) 2_565 ?

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
Cl1 Mn1 Cl1 92.062(12) 9_565 14_455 ?
Cl1 Mn1 Cl1 180.0 9_565 . ?
Cl1 Mn1 Cl1 180.00(7) 14_455 6_554 ?
Cl1 Mn1 Cl1 92.063(12) 6_554 . ?
Cl1 Mn1 Cl1 87.937(12) 14_455 . ?
Cl1 Mn1 Cl1 87.938(12) 9_565 6_554 ?
Cl2 Mn1 Cl1 90.31(4) . . ?
Cl2 Mn1 Cl1 90.31(4) 9_565 9_565 ?
Cl2 Mn1 Cl1 89.69(4) 9_565 14_455 ?
Cl2 Mn1 Cl1 89.69(4) . 9_565 ?
Cl2 Mn1 Cl1 89.69(4) 9_565 . ?
Cl2 Mn1 Cl1 89.69(4) . 6_554 ?
Cl2 Mn1 Cl1 90.31(4) 9_565 6_554 ?
Cl2 Mn1 Cl1 90.31(4) . 14_455 ?
Cl2 Mn1 Cl2 180.0 9_565 . ?
Mn1 Cl1 Mn1 168.04(7) 6 . ?
C2 C1 C2 120.4(10) 2_565 . ?
N1 C2 C1 122.8(7) . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.436
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 2014528'
loop_
_audit_author_name
_audit_author_address
'Qing-Lun Wang'
;NANKAI University
China
;
_audit_update_record             
;
2021-09-17 deposited with the CCDC.	2021-11-01 downloaded from the CCDC.
;
_audit_creation_date             2020-02-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl6 Mn, 2(C4 H9 N5)'
_chemical_formula_sum            'C8 H18 Cl6 Mn N10'
_chemical_formula_weight         521.96
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     ' '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'I 1 2/m 1'
_space_group_name_Hall           '-I 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   8.9461(3)
_cell_length_b                   9.6604(3)
_cell_length_c                   11.2084(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.229(3)
_cell_angle_gamma                90
_cell_volume                     934.65(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1069
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      72.4100
_cell_measurement_theta_min      5.6430
_shelx_estimated_absorpt_T_max   0.545
_shelx_estimated_absorpt_T_min   0.445
_exptl_absorpt_coefficient_mu    13.802
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1961
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.220
_diffrn_reflns_theta_min         5.656
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     62.00  87.00   0.50    0.50    --    0.00  57.00-180.00   50
  2  ω    -23.00  27.00   0.50    0.50    --    0.00  38.00-120.00  100
  3  ω    -28.00  -2.00   0.50    0.50    --    0.00  57.00-180.00   52
  4  ω     53.00  81.00   0.50    0.50    --    0.00  38.00-120.00   56
  5  ω     63.00 187.00   0.50    0.70    --   97.60  77.00 -60.00  248
  6  ω     80.00 135.00   0.50    0.70    --   97.60  77.00   0.00  110
  7  ω     95.00 187.00   0.50    0.70    --   97.60  61.00-120.00  184
  8  ω     64.00 129.00   0.50    0.70    --   97.60 -82.00  90.00  130
  9  ω    139.00 181.00   0.50    0.70    --   97.60  77.00   0.00   84
 10  ω     10.00  74.00   0.50    0.70    --   97.60 -77.00  90.00  128
 11  ω     77.00 103.00   0.50    0.70    --   97.60  45.00-120.00   52
 12  ω     77.00 103.00   0.50    0.70    --   97.60  61.00 150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0841774000
_diffrn_orient_matrix_UB_12      -0.1356628000
_diffrn_orient_matrix_UB_13      -0.0491084000
_diffrn_orient_matrix_UB_21      -0.0989806000
_diffrn_orient_matrix_UB_22      0.0777110000
_diffrn_orient_matrix_UB_23      -0.1134670000
_diffrn_orient_matrix_UB_31      0.1224475000
_diffrn_orient_matrix_UB_32      -0.0306774000
_diffrn_orient_matrix_UB_33      -0.0709000000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                907
_reflns_number_total             963
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         963
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0375
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0750P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1031
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2. Others
 Fixed Sof: H3A(0.5) H3B(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3)
3.b X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N3(H3A,H3B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.500000 0.500000 0.500000 0.0232(2) Uani 1 4 d S T P . .
Cl1 Cl 0.79537(9) 0.500000 0.54034(7) 0.0288(3) Uani 1 2 d S T P . .
Cl2 Cl 0.46240(6) 0.31016(6) 0.33430(5) 0.0270(2) Uani 1 1 d . . . . .
N1 N 0.7558(2) 0.1199(2) 0.51632(18) 0.0257(5) Uani 1 1 d . . . . .
H1 H 0.736439 0.196575 0.548333 0.031 Uiso 1 1 calc R . . . .
N2 N 0.8577(2) 0.2455(2) 0.38078(19) 0.0271(5) Uani 1 1 d . . . . .
H2A H 0.840492 0.319408 0.417897 0.032 Uiso 1 1 calc R . . . .
H2B H 0.898654 0.251297 0.319595 0.032 Uiso 1 1 calc R . . . .
N3 N 0.6536(4) 0.000000 0.6541(3) 0.0313(7) Uani 1 2 d S T P . .
H3A H 0.630746 -0.077094 0.683384 0.038 Uiso 0.5 1 calc R . . . .
H3B H 0.631843 0.077094 0.684036 0.038 Uiso 0.5 1 calc R . . . .
C1 C 0.8213(2) 0.1235(3) 0.4176(2) 0.0233(5) Uani 1 1 d . . . . .
C2 C 0.7215(4) 0.000000 0.5636(3) 0.0240(7) Uani 1 2 d S T P . .
C3 C 0.8498(4) 0.000000 0.3650(3) 0.0258(7) Uani 1 2 d S T P . .
H3 H 0.887592 0.000000 0.295258 0.031 Uiso 1 2 calc RS 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
Mn1 Cl1 2.5611(8) . ?
Mn1 Cl1 2.5611(8) 5_666 ?
Mn1 Cl2 2.5686(6) 2_656 ?
Mn1 Cl2 2.5686(6) 5_666 ?
Mn1 Cl2 2.5686(6) 6_565 ?
Mn1 Cl2 2.5686(6) . ?
N1 H1 0.8600 . ?
N1 C1 1.381(3) . ?
N1 C2 1.342(3) . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
N2 C1 1.318(3) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N3 C2 1.312(4) . ?
C1 C3 1.384(3) . ?
C2 N1 1.342(3) 6 ?
C3 C1 1.384(3) 6 ?
C3 H3 0.9300 . ?

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
Cl1 Mn1 Cl1 180.0 . 5_666 ?
Cl1 Mn1 Cl2 93.482(18) . 6_565 ?
Cl1 Mn1 Cl2 93.481(18) 5_666 2_656 ?
Cl1 Mn1 Cl2 93.481(18) 5_666 5_666 ?
Cl1 Mn1 Cl2 86.518(18) 5_666 . ?
Cl1 Mn1 Cl2 86.518(18) . 2_656 ?
Cl1 Mn1 Cl2 86.519(17) 5_666 6_565 ?
Cl1 Mn1 Cl2 93.482(18) . . ?
Cl1 Mn1 Cl2 86.518(18) . 5_666 ?
Cl2 Mn1 Cl2 88.88(3) 5_666 6_565 ?
Cl2 Mn1 Cl2 88.88(3) . 2_656 ?
Cl2 Mn1 Cl2 91.12(3) . 6_565 ?
Cl2 Mn1 Cl2 180.0 6_565 2_656 ?
Cl2 Mn1 Cl2 91.12(3) 5_666 2_656 ?
Cl2 Mn1 Cl2 180.0 . 5_666 ?
C1 N1 H1 119.1 . . ?
C2 N1 H1 119.1 . . ?
C2 N1 C1 121.8(2) . . ?
H2A N2 H2B 120.0 . . ?
C1 N2 H2A 120.0 . . ?
C1 N2 H2B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C2 N3 H3A 120.0 . . ?
C2 N3 H3B 120.0 . . ?
N1 C1 C3 118.9(2) . . ?
N2 C1 N1 117.7(2) . . ?
N2 C1 C3 123.3(2) . . ?
N1 C2 N1 119.3(3) 6 . ?
N3 C2 N1 120.34(15) . 6 ?
N3 C2 N1 120.34(15) . . ?
C1 C3 C1 119.1(3) 6 . ?
C1 C3 H3 120.4 . . ?
C1 C3 H3 120.4 6 . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.695
_oxdiff_exptl_absorpt_empirical_full_min 0.675
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 2014529'
loop_
_audit_author_name
_audit_author_address
'Qing-Lun Wang'
;NANKAI University
China
;
_audit_update_record             
;
2021-09-17 deposited with the CCDC.	2021-11-01 downloaded from the CCDC.
;
_audit_creation_date             2020-02-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl5 Mn, 2(C3 H8 N6), Cl'
_chemical_formula_sum            'C6 H16 Cl6 Mn N12'
_chemical_formula_weight         523.95
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C N H Cu S'
_chemical_oxdiff_usercomment     ' '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   5.40460(10)
_cell_length_b                   15.3969(4)
_cell_length_c                   10.8565(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.166(2)
_cell_angle_gamma                90
_cell_volume                     902.03(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3206
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.5100
_cell_measurement_theta_min      2.8570
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    14.338
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            4101
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.854
_diffrn_reflns_theta_min         4.078
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     32.00  58.00   0.50    0.50    --    0.00  57.00 -60.00   52
  2  ω    -29.00  17.00   0.50    0.50    --    0.00  38.00-150.00   92
  3  ω     42.00  85.00   0.50    0.50    --    0.00  57.00-120.00   86
  4  ω    -24.00  36.00   0.50    0.50    --    0.00  57.00-120.00  120
  5  ω     94.00 186.00   0.50    0.50    --   98.80  45.00 -60.00  184
  6  ω     41.00 133.00   0.50    0.50    --   98.80 -77.00 -60.00  184
  7  ω     69.00 175.00   0.50    0.50    --   98.80  61.00 -90.00  212
  8  ω     11.00 131.00   0.50    0.50    --   98.80 -82.00  90.00  240
  9  ω     88.00 128.00   0.50    0.50    --   98.80 -82.00 150.00   80
 10  ω     78.00 103.00   0.50    0.50    --   98.80 -45.00 -30.00   50
 11  ω    100.00 126.00   0.50    0.50    --   98.80  45.00-150.00   52
 12  ω      9.00  46.00   0.50    0.50    --   98.80 -45.00 -30.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0562024000
_diffrn_orient_matrix_UB_12      0.0980793000
_diffrn_orient_matrix_UB_13      -0.0047106000
_diffrn_orient_matrix_UB_21      -0.2600164000
_diffrn_orient_matrix_UB_22      -0.0174343000
_diffrn_orient_matrix_UB_23      0.0457485000
_diffrn_orient_matrix_UB_31      0.1033511000
_diffrn_orient_matrix_UB_32      0.0094230000
_diffrn_orient_matrix_UB_33      0.1345184000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1736
_reflns_number_total             1849
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.846
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1849
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0576
_refine_ls_restrained_S_all      1.137
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1083P)²+1.3796P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1694
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3)
2.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N4(H4A,H4B), N5(H5A,H5B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.48922(17) 0.250000 0.39050(8) 0.0176(3) Uani 1 2 d S T P . .
Cl1 Cl 0.50670(17) 0.41226(6) 0.39860(9) 0.0212(3) Uani 1 1 d . . . . .
Cl2 Cl 0.5030(2) 0.250000 0.16562(12) 0.0214(3) Uani 1 2 d S T P . .
Cl3 Cl 0.5275(3) 0.250000 0.62840(13) 0.0216(3) Uani 1 2 d S T P . .
Cl4 Cl 0.0069(2) 0.250000 0.40700(13) 0.0236(4) Uani 1 2 d S T P . .
N1 N -0.0786(7) 0.5833(2) 0.4030(3) 0.0266(8) Uani 1 1 d . . . . .
H1A H -0.025605 0.631488 0.434517 0.032 Uiso 1 1 calc R . . . .
H1B H -0.202013 0.557124 0.433341 0.032 Uiso 1 1 calc R . . . .
N2 N -0.0535(6) 0.4749(2) 0.2573(3) 0.0191(7) Uani 1 1 d . . . . .
H2 H -0.176269 0.448128 0.287254 0.023 Uiso 1 1 calc R . . . .
N3 N 0.2203(6) 0.58891(19) 0.2598(3) 0.0175(7) Uani 1 1 d . . . . .
H3 H 0.279722 0.635927 0.292372 0.021 Uiso 1 1 calc R . . . .
N4 N -0.0326(7) 0.3678(2) 0.1128(3) 0.0240(8) Uani 1 1 d . . . . .
H4A H 0.028619 0.344784 0.049005 0.029 Uiso 1 1 calc R . . . .
H4B H -0.152988 0.342753 0.147299 0.029 Uiso 1 1 calc R . . . .
N5 N 0.5078(6) 0.5976(3) 0.1121(3) 0.0247(8) Uani 1 1 d . . . . .
H5A H 0.576569 0.577882 0.048204 0.030 Uiso 1 1 calc R . . . .
H5B H 0.559677 0.645208 0.145911 0.030 Uiso 1 1 calc R . . . .
N6 N 0.2436(6) 0.4813(2) 0.1057(3) 0.0166(7) Uani 1 1 d . . . . .
C1 C 0.0282(7) 0.5498(2) 0.3090(4) 0.0182(8) Uani 1 1 d . . . . .
C2 C 0.0571(7) 0.4408(2) 0.1571(3) 0.0153(7) Uani 1 1 d . . . . .
C3 C 0.3229(7) 0.5548(2) 0.1582(4) 0.0167(8) Uani 1 1 d . . . . .
Cl5 Cl -0.0861(3) 0.750000 0.12236(13) 0.0229(4) Uani 1 2 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
Mn1 Cl1 2.5015(9) . ?
Mn1 Cl1 2.5015(9) 4_565 ?
Mn1 Cl2 2.4467(16) . ?
Mn1 Cl3 2.5797(16) . ?
Mn1 Cl4 2.6226(16) . ?
Mn1 Cl4 2.7939(16) 1_655 ?
Cl4 Mn1 2.7939(16) 1_455 ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C1 1.307(5) . ?
N2 H2 0.8600 . ?
N2 C1 1.346(5) . ?
N2 C2 1.374(5) . ?
N3 H3 0.8600 . ?
N3 C1 1.337(5) . ?
N3 C3 1.367(5) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N4 C2 1.306(5) . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
N5 C3 1.319(5) . ?
N6 C2 1.333(5) . ?
N6 C3 1.328(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
Cl1 Mn1 Cl1 174.25(6) . 4_565 ?
Cl1 Mn1 Cl3 87.94(3) . . ?
Cl1 Mn1 Cl3 87.94(3) 4_565 . ?
Cl1 Mn1 Cl4 87.82(3) 4_565 1_655 ?
Cl1 Mn1 Cl4 91.91(3) . . ?
Cl1 Mn1 Cl4 91.91(3) 4_565 . ?
Cl1 Mn1 Cl4 87.82(3) . 1_655 ?
Cl2 Mn1 Cl1 91.83(3) . 4_565 ?
Cl2 Mn1 Cl1 91.83(3) . . ?
Cl2 Mn1 Cl3 173.68(6) . . ?
Cl2 Mn1 Cl4 88.77(5) . 1_655 ?
Cl2 Mn1 Cl4 98.81(6) . . ?
Cl3 Mn1 Cl4 84.90(5) . 1_655 ?
Cl3 Mn1 Cl4 87.51(5) . . ?
Cl4 Mn1 Cl4 172.42(7) . 1_655 ?
Mn1 Cl4 Mn1 172.42(7) . 1_455 ?
H1A N1 H1B 120.0 . . ?
C1 N1 H1A 120.0 . . ?
C1 N1 H1B 120.0 . . ?
C1 N2 H2 119.7 . . ?
C1 N2 C2 120.7(3) . . ?
C2 N2 H2 119.7 . . ?
C1 N3 H3 119.8 . . ?
C1 N3 C3 120.5(3) . . ?
C3 N3 H3 119.8 . . ?
H4A N4 H4B 120.0 . . ?
C2 N4 H4A 120.0 . . ?
C2 N4 H4B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C3 N5 H5A 120.0 . . ?
C3 N5 H5B 120.0 . . ?
C3 N6 C2 116.9(3) . . ?
N1 C1 N2 121.0(4) . . ?
N1 C1 N3 121.3(4) . . ?
N3 C1 N2 117.7(3) . . ?
N4 C2 N2 116.8(3) . . ?
N4 C2 N6 121.4(4) . . ?
N6 C2 N2 121.7(4) . . ?
N5 C3 N3 117.6(4) . . ?
N5 C3 N6 119.8(4) . . ?
N6 C3 N3 122.6(3) . . ?

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
C1 N2 C2 N4 179.7(4) . . . . ?
C1 N2 C2 N6 -1.8(6) . . . . ?
C1 N3 C3 N5 178.3(4) . . . . ?
C1 N3 C3 N6 -1.7(6) . . . . ?
C2 N2 C1 N1 178.9(4) . . . . ?
C2 N2 C1 N3 -0.4(6) . . . . ?
C2 N6 C3 N3 -0.4(6) . . . . ?
C2 N6 C3 N5 179.6(4) . . . . ?
C3 N3 C1 N1 -177.2(4) . . . . ?
C3 N3 C1 N2 2.0(6) . . . . ?
C3 N6 C2 N2 2.1(6) . . . . ?
C3 N6 C2 N4 -179.5(4) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.095
_oxdiff_exptl_absorpt_empirical_full_min 0.526
####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 2014527'
loop_
_audit_author_name
_audit_author_address
'Qing-Lun Wang'
;NANKAI University
China
;
_audit_update_record             
;
2021-09-17 deposited with the CCDC.	2021-11-01 downloaded from the CCDC.
;
_audit_creation_date             2020-02-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl6 Mn, 2(C8 H14 N2)'
_chemical_formula_sum            'C16 H28 Cl6 Mn N4'
_chemical_formula_weight         544.06
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0193 0.0097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3694 0.7045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5661 2.8539 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0328 0.0186 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.5206(3)
_cell_length_b                   8.4873(3)
_cell_length_c                   10.5291(3)
_cell_angle_alpha                101.991(3)
_cell_angle_beta                 99.889(3)
_cell_angle_gamma                112.943(3)
_cell_volume                     581.09(3)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3780
_cell_measurement_temperature    296.6(6)
_cell_measurement_theta_max      72.7890
_cell_measurement_theta_min      5.9230
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    11.160
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             279
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4761
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        68.230
_diffrn_reflns_theta_max         73.781
_diffrn_reflns_theta_min         4.490
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.6(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -57.00   0.00   0.50    0.50    --    0.00 -38.00  90.00  114
  2  ω    -56.00  12.00   0.50    0.50    --    0.00 -37.00-176.00  136
  3  ω    -13.00  29.00   0.50    0.50    --    0.00 -38.00 -60.00   84
  4  ω    -87.00 -37.00   0.50    0.50    --    0.00 -38.00 -60.00  100
  5  ω      8.00 135.00   0.50    0.50    --   97.60 -82.00   0.00  254
  6  ω      9.00  61.00   0.50    0.50    --   97.60 -61.00-150.00  104
  7  ω    133.00 159.00   0.50    0.50    --   97.60  77.00  60.00   52
  8  ω      8.00 127.00   0.50    0.50    --   97.60 -82.00-150.00  238
  9  ω     92.00 118.00   0.50    0.50    --   97.60 -82.00 120.00   52
 10  ω     64.00 186.00   0.50    0.50    --   97.60  30.00  90.00  244
 11  ω    101.00 130.00   0.50    0.50    --   97.60 -30.00 120.00   58
 12  ω     86.00 123.00   0.50    0.50    --   97.60  45.00 120.00   74
 13  ω     21.00  47.00   0.50    0.50    --   97.60 -30.00 120.00   52
 14  ω     69.00 128.00   0.50    0.50    --   97.60 -61.00-150.00  118
 15  ω     33.00  58.00   0.50    0.50    --   97.60 -82.00 120.00   50
 16  ω    128.00 161.00   0.50    0.50    --   97.60  45.00 120.00   66
 17  ω     71.00 105.00   0.50    0.50    --   97.60  77.00  60.00   68
 18  ω     89.00 114.00   0.50    0.50    --   97.60 -82.00 -90.00   50
 19  ω     65.00 135.00   0.50    0.50    --   97.60 -82.00  60.00  140
 20  ω     98.00 130.00   0.50    0.50    --   97.60  45.00-180.00   64
 21  ω     89.00 115.00   0.50    0.50    --   97.60 -82.00  90.00   52
 22  ω     81.00 183.00   0.50    0.50    --   97.60  61.00 150.00  204
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0169878000
_diffrn_orient_matrix_UB_12      -0.1730990000
_diffrn_orient_matrix_UB_13      0.0074552000
_diffrn_orient_matrix_UB_21      0.2272625000
_diffrn_orient_matrix_UB_22      0.1104245000
_diffrn_orient_matrix_UB_23      0.0694795000
_diffrn_orient_matrix_UB_31      -0.0415583000
_diffrn_orient_matrix_UB_32      0.0242963000
_diffrn_orient_matrix_UB_33      0.1391190000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5478
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2139
_reflns_number_total             2227
_reflns_odcompleteness_completeness 98.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0376
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0690P)²+0.0868P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.0981
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C8(H8A,H8B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.000000 0.500000 0.000000 0.02126(15) Uani 1 2 d S T P . .
Cl1 Cl 0.14198(7) 0.26762(6) -0.00536(5) 0.02363(15) Uani 1 1 d . . . . .
Cl2 Cl 0.01214(7) 0.52340(7) 0.24358(5) 0.02661(16) Uani 1 1 d . . . . .
Cl3 Cl -0.37260(7) 0.23826(7) -0.06937(6) 0.02908(16) Uani 1 1 d . . . . .
N1 N 0.5811(3) 0.5298(2) 0.18660(18) 0.0257(4) Uani 1 1 d . . . . .
H1A H 0.518004 0.428913 0.117647 0.031 Uiso 1 1 calc GR . . . .
H1B H 0.713410 0.570909 0.200135 0.031 Uiso 1 1 calc GR . . . .
H1C H 0.543435 0.611554 0.167770 0.031 Uiso 1 1 calc GR . . . .
N2 N 1.1698(3) 0.9104(2) 0.83594(19) 0.0275(4) Uani 1 1 d . . . . .
H2A H 1.099317 0.799823 0.838726 0.033 Uiso 1 1 calc GR . . . .
H2B H 1.124336 0.983506 0.876826 0.033 Uiso 1 1 calc GR . . . .
H2C H 1.298999 0.948631 0.878021 0.033 Uiso 1 1 calc GR . . . .
C1 C 0.5284(4) 0.4931(3) 0.3106(2) 0.0344(5) Uani 1 1 d . . . . .
H1D H 0.563041 0.399367 0.328132 0.041 Uiso 1 1 calc R . . . .
H1E H 0.384471 0.450284 0.296102 0.041 Uiso 1 1 calc R . . . .
C2 C 0.6372(3) 0.6585(3) 0.4320(2) 0.0257(4) Uani 1 1 d . . . . .
C3 C 0.5421(4) 0.7619(3) 0.4731(2) 0.0319(5) Uani 1 1 d . . . . .
H3 H 0.411391 0.730776 0.424801 0.038 Uiso 1 1 calc R . . . .
C4 C 0.6415(4) 0.9126(3) 0.5869(3) 0.0359(5) Uani 1 1 d . . . . .
H4 H 0.576380 0.980927 0.615123 0.043 Uiso 1 1 calc R . . . .
C5 C 0.8361(4) 0.9606(3) 0.6577(2) 0.0320(5) Uani 1 1 d . . . . .
H5 H 0.902655 1.062862 0.732390 0.038 Uiso 1 1 calc R . . . .
C6 C 0.9337(3) 0.8577(3) 0.6183(2) 0.0257(4) Uani 1 1 d . . . . .
C7 C 0.8325(3) 0.7055(3) 0.5055(2) 0.0262(4) Uani 1 1 d . . . . .
H7 H 0.895938 0.634737 0.479164 0.031 Uiso 1 1 calc R . . . .
C8 C 1.1479(3) 0.9093(4) 0.6933(2) 0.0351(5) Uani 1 1 d . . . . .
H8A H 1.191679 0.825223 0.648035 0.042 Uiso 1 1 calc R . . . .
H8B H 1.234288 1.027753 0.690750 0.042 Uiso 1 1 calc R . . . .


_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
Mn1 Cl1 2.5787(4) . ?
Mn1 Cl1 2.5786(4) 2_565 ?
Mn1 Cl2 2.5138(5) . ?
Mn1 Cl2 2.5138(5) 2_565 ?
Mn1 Cl3 2.6627(5) 2_565 ?
Mn1 Cl3 2.6628(5) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C1 1.486(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C8 1.480(3) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 C2 1.508(3) . ?
C2 C3 1.381(3) . ?
C2 C7 1.393(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.393(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.377(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.388(3) . ?
C6 C7 1.394(3) . ?
C6 C8 1.510(3) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?

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
Cl1 Mn1 Cl1 180.0 2_565 . ?
Cl1 Mn1 Cl3 89.852(15) . 2_565 ?
Cl1 Mn1 Cl3 89.851(15) 2_565 . ?
Cl1 Mn1 Cl3 90.149(15) 2_565 2_565 ?
Cl1 Mn1 Cl3 90.149(15) . . ?
Cl2 Mn1 Cl1 88.831(16) . . ?
Cl2 Mn1 Cl1 91.169(16) 2_565 . ?
Cl2 Mn1 Cl1 91.168(16) . 2_565 ?
Cl2 Mn1 Cl1 88.832(16) 2_565 2_565 ?
Cl2 Mn1 Cl2 180.0 2_565 . ?
Cl2 Mn1 Cl3 91.587(17) . 2_565 ?
Cl2 Mn1 Cl3 88.413(17) 2_565 2_565 ?
Cl2 Mn1 Cl3 91.586(17) 2_565 . ?
Cl2 Mn1 Cl3 88.414(17) . . ?
Cl3 Mn1 Cl3 180.0 2_565 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C8 N2 H2A 109.5 . . ?
C8 N2 H2B 109.5 . . ?
C8 N2 H2C 109.5 . . ?
N1 C1 H1D 109.3 . . ?
N1 C1 H1E 109.3 . . ?
N1 C1 C2 111.72(17) . . ?
H1D C1 H1E 107.9 . . ?
C2 C1 H1D 109.3 . . ?
C2 C1 H1E 109.3 . . ?
C3 C2 C1 120.2(2) . . ?
C3 C2 C7 119.5(2) . . ?
C7 C2 C1 120.2(2) . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.1(2) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.2(2) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.5(2) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C7 119.1(2) . . ?
C5 C6 C8 121.4(2) . . ?
C7 C6 C8 119.5(2) . . ?
C2 C7 C6 120.5(2) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
N2 C8 C6 112.21(18) . . ?
N2 C8 H8A 109.2 . . ?
N2 C8 H8B 109.2 . . ?
C6 C8 H8A 109.2 . . ?
C6 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.013
_oxdiff_exptl_absorpt_empirical_full_min 0.643
