# Electronic Supplementary Material (ESI) for ChemComm.
# 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_C6N2H16MnCl4
_database_code_depnum_ccdc_archive 'CCDC 2076753'
loop_
_audit_author_name
_audit_author_address
'Xiao-Wu Lei'
;Jining University
China
;
_audit_update_record             
;
2021-04-12 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
#================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C6N2H16MnCl4
_chemical_formula_sum            'C6 H16 Cl4 Mn N2'
_chemical_formula_weight         312.95

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/m 1'

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

_cell_length_a                   6.1119(2)
_cell_length_b                   14.5023(5)
_cell_length_c                   6.9450(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.477(4)
_cell_angle_gamma                90.00
_cell_volume                     615.56(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9922
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      24.29

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             318
_exptl_absorpt_coefficient_mu    16.393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3993
_exptl_absorpt_correction_T_max  0.7291
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1958
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         6.10
_diffrn_reflns_theta_max         75.56
_reflns_number_total             1057
_reflns_number_gt                976
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 Software Suite (Bruker,2005)'
_computing_cell_refinement       'APEX2 Software Suite (Bruker,2005)'
_computing_data_reduction        'APEX2 Software Suite (Bruker,2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0836P)²+0.1206P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0143(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1057
_refine_ls_number_parameters     66
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1232
_refine_ls_wR_factor_gt          0.1188
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.45601(12) 0.7500 0.25621(10) 0.0266(3) Uani 1 2 d S . .
Cl3 Cl 0.37409(15) 0.61009(5) 0.10609(12) 0.0377(3) Uani 1 1 d . . .
Cl2 Cl 0.3297(2) 0.7500 0.58209(16) 0.0386(4) Uani 1 2 d S . .
Cl1 Cl 0.84717(19) 0.7500 0.2969(2) 0.0396(4) Uani 1 2 d S . .
N1 N -0.0475(4) 0.57989(18) 0.6199(4) 0.0281(6) Uani 1 1 d . . .
H1 H 0.0166 0.6247 0.5481 0.034 Uiso 1 1 calc R . .
C1 C 0.2201(6) 0.4664(2) 0.5009(5) 0.0313(7) Uani 1 1 d . . .
H1A H 0.3282 0.4211 0.5407 0.038 Uiso 1 1 calc R . .
H1B H 0.2935 0.5128 0.4245 0.038 Uiso 1 1 calc R . .
C2 C 0.1238(6) 0.5109(2) 0.6758(5) 0.0312(7) Uani 1 1 d . . .
H2A H 0.0594 0.4640 0.7571 0.037 Uiso 1 1 calc R . .
H2B H 0.2387 0.5413 0.7490 0.037 Uiso 1 1 calc R . .
C3 C -0.1456(7) 0.6240(3) 0.7956(6) 0.0418(9) Uani 1 1 d . . .
H3A H -0.2500 0.6699 0.7564 0.063 Uiso 1 1 calc R . .
H3B H -0.0319 0.6524 0.8710 0.063 Uiso 1 1 calc R . .
H3C H -0.2174 0.5778 0.8712 0.063 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 Cl3 2.3336(8) . ?
Mn1 Cl3 2.3336(8) 4_575 ?
Mn1 Cl2 2.3973(13) . ?
Mn1 Cl1 2.4050(13) . ?
N1 C2 1.497(4) . ?
N1 C1 1.501(4) 3_566 ?
N1 C3 1.506(5) . ?
N1 H1 0.9100 . ?
C1 C2 1.500(5) . ?
C1 N1 1.501(4) 3_566 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

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
Cl3 Mn1 Cl3 120.79(5) . 4_575 ?
Cl3 Mn1 Cl2 110.62(3) . . ?
Cl3 Mn1 Cl2 110.62(3) 4_575 . ?
Cl3 Mn1 Cl1 105.18(3) . . ?
Cl3 Mn1 Cl1 105.18(3) 4_575 . ?
Cl2 Mn1 Cl1 102.51(5) . . ?
C2 N1 C1 109.4(3) . 3_566 ?
C2 N1 C3 110.9(3) . . ?
C1 N1 C3 111.1(3) 3_566 . ?
C2 N1 H1 108.4 . . ?
C1 N1 H1 108.4 3_566 . ?
C3 N1 H1 108.4 . . ?
C2 C1 N1 111.5(3) . 3_566 ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1A 109.3 3_566 . ?
C2 C1 H1B 109.3 . . ?
N1 C1 H1B 109.3 3_566 . ?
H1A C1 H1B 108.0 . . ?
N1 C2 C1 110.8(3) . . ?
N1 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        75.56
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.122
####################################################################### 
# 
# 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_C6H16N2MnCl4
_database_code_depnum_ccdc_archive 'CCDC 2076754'
loop_
_audit_author_name
_audit_author_address
'Xiao-Wu Lei'
;Jining University
China
;
_audit_update_record             
;
2021-04-12 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
#================================================

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         C6H16N2MnCl4
_chemical_formula_sum            'C6 H16 Cl4 Mn N2'
_chemical_formula_weight         312.95

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca

loop_
_symmetry_equiv_pos_as_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'
'-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                   11.5561(2)
_cell_length_b                   9.7596(2)
_cell_length_c                   23.9095(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2696.58(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9922
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      24.29

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    14.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3993
_exptl_absorpt_correction_T_max  0.7291
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8628
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.70
_diffrn_reflns_theta_max         75.71
_reflns_number_total             2659
_reflns_number_gt                2391
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 Software Suite (Bruker,2005)'
_computing_cell_refinement       'APEX2 Software Suite (Bruker,2005)'
_computing_data_reduction        'APEX2 Software Suite (Bruker,2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0753P)²+1.8828P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0045(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2659
_refine_ls_number_parameters     119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.1194
_refine_ls_wR_factor_gt          0.1054
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.44355(4) 0.66113(5) 0.391941(18) 0.03170(19) Uani 1 1 d . . .
Cl2 Cl 0.56403(6) 0.49994(7) 0.34597(3) 0.0384(2) Uani 1 1 d . . .
Cl3 Cl 0.34695(6) 0.54295(7) 0.46371(3) 0.0385(2) Uani 1 1 d . . .
Cl4 Cl 0.57027(7) 0.82139(7) 0.43705(3) 0.0396(2) Uani 1 1 d . . .
Cl1 Cl 0.33690(7) 0.79191(10) 0.32915(4) 0.0538(3) Uani 1 1 d . . .
N2 N 0.54066(19) 0.0704(2) 0.35000(9) 0.0268(5) Uani 1 1 d . . .
H2C H 0.5321 -0.0095 0.3692 0.032 Uiso 1 1 calc R . .
N1 N 0.5195(2) 0.2702(2) 0.43896(9) 0.0307(5) Uani 1 1 d . . .
H1D H 0.5280 0.3479 0.4191 0.037 Uiso 1 1 calc R . .
H1E H 0.5087 0.2933 0.4750 0.037 Uiso 1 1 calc R . .
C6 C 0.4164(2) 0.1935(3) 0.41820(13) 0.0353(6) Uani 1 1 d . . .
H6A H 0.3480 0.2504 0.4218 0.042 Uiso 1 1 calc R . .
H6B H 0.4051 0.1119 0.4407 0.042 Uiso 1 1 calc R . .
C5 C 0.6443(2) 0.1440(3) 0.37347(13) 0.0361(6) Uani 1 1 d . . .
H5A H 0.6596 0.2252 0.3512 0.043 Uiso 1 1 calc R . .
H5B H 0.7116 0.0848 0.3710 0.043 Uiso 1 1 calc R . .
C4 C 0.4324(2) 0.1534(3) 0.35811(12) 0.0329(6) Uani 1 1 d . . .
H4A H 0.4366 0.2354 0.3352 0.039 Uiso 1 1 calc R . .
H4B H 0.3661 0.1004 0.3458 0.039 Uiso 1 1 calc R . .
C3 C 0.6258(3) 0.1853(3) 0.43372(12) 0.0377(7) Uani 1 1 d . . .
H3A H 0.6185 0.1040 0.4568 0.045 Uiso 1 1 calc R . .
H3B H 0.6922 0.2371 0.4469 0.045 Uiso 1 1 calc R . .
C2 C 0.5543(3) 0.0354(4) 0.28908(12) 0.0446(8) Uani 1 1 d . . .
H2A H 0.5757 0.1175 0.2686 0.054 Uiso 1 1 calc R . .
H2B H 0.4808 0.0035 0.2745 0.054 Uiso 1 1 calc R . .
C1 C 0.6455(4) -0.0740(6) 0.27947(17) 0.0722(13) Uani 1 1 d . . .
H1A H 0.6513 -0.0930 0.2402 0.108 Uiso 1 1 calc R . .
H1B H 0.6240 -0.1560 0.2990 0.108 Uiso 1 1 calc R . .
H1C H 0.7188 -0.0421 0.2931 0.108 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 2.3243(8) . ?
Mn1 Cl3 2.3497(8) . ?
Mn1 Cl2 2.3709(8) . ?
Mn1 Cl4 2.3987(8) . ?
N2 C4 1.503(3) . ?
N2 C2 1.504(3) . ?
N2 C5 1.506(4) . ?
N1 C3 1.487(4) . ?
N1 C6 1.492(4) . ?
C6 C4 1.501(4) . ?
C5 C3 1.511(4) . ?
C2 C1 1.517(6) . ?

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 Cl3 119.30(3) . . ?
Cl1 Mn1 Cl2 112.10(4) . . ?
Cl3 Mn1 Cl2 106.97(3) . . ?
Cl1 Mn1 Cl4 104.84(3) . . ?
Cl3 Mn1 Cl4 106.37(3) . . ?
Cl2 Mn1 Cl4 106.41(3) . . ?
C4 N2 C2 109.5(2) . . ?
C4 N2 C5 110.9(2) . . ?
C2 N2 C5 112.7(2) . . ?
C3 N1 C6 110.6(2) . . ?
N1 C6 C4 110.5(2) . . ?
N2 C5 C3 111.7(2) . . ?
C6 C4 N2 111.5(2) . . ?
N1 C3 C5 110.2(2) . . ?
N2 C2 C1 112.3(3) . . ?

_diffrn_measured_fraction_theta_max 1
_diffrn_reflns_theta_full        75.71
_diffrn_measured_fraction_theta_full 1
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.107





####################################################################### 
# 
# 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_C9H23N3MnCl4
_database_code_depnum_ccdc_archive 'CCDC 2076750'
loop_
_audit_author_name
_audit_author_address
'Hong-Mei Pan'
;Jining University
China
;
_audit_update_record             
;
2021-05-27 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
#================================================
_audit_creation_date             2021-05-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'Cl4 Mn, C9 H23 N3'
_chemical_formula_sum            'C9 H23 Cl4 Mn N3'
_chemical_formula_weight         370.04
_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 0.0180 0.0090 '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 0.3640 0.7020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5300 2.8050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0310 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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   9.9960(2)
_cell_length_b                   14.3566(2)
_cell_length_c                   15.3780(3)
_cell_angle_alpha                90
_cell_angle_beta                 128.6570(10)
_cell_angle_gamma                90
_cell_volume                     1723.35(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.29
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   0.811
_shelx_estimated_absorpt_T_min   0.218
_exptl_absorpt_coefficient_mu    11.815
_exptl_absorpt_correction_T_max  0.7291
_exptl_absorpt_correction_T_min  0.3993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10246
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.927
_diffrn_reflns_theta_min         4.801
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3042
_reflns_number_total             3461
_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       'APEX2 Software Suite (Bruker,2005)'
_computing_data_collection       'APEX2 Software Suite (Bruker,2005)'
_computing_data_reduction        'APEX2 Software Suite (Bruker,2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.510
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.0019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3461
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0351
_refine_ls_restrained_S_all      1.042
_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)+(0.0590P)²+0.7376P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1083
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 N2(H2), N3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C7(H7A,H7B,H7C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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 0.66659(5) 0.27678(3) 0.40418(3) 0.04023(15) Uani 1 1 d . . . . .
Cl1 Cl 0.84259(10) 0.39178(5) 0.54099(6) 0.0680(3) Uani 1 1 d . . . . .
Cl2 Cl 0.53311(9) 0.18102(5) 0.45716(7) 0.0564(2) Uani 1 1 d . . . . .
Cl3 Cl 0.46487(9) 0.35140(5) 0.23421(6) 0.0613(2) Uani 1 1 d . . . . .
Cl4 Cl 0.82473(10) 0.16677(5) 0.38859(8) 0.0625(2) Uani 1 1 d . . . . .
N1 N 0.2990(3) 0.40069(16) 0.55770(19) 0.0490(5) Uani 1 1 d . . . . .
N2 N 0.0759(3) 0.37437(14) 0.31665(17) 0.0397(4) Uani 1 1 d . . . . .
H2 H 0.140072 0.425567 0.355220 0.048 Uiso 1 1 d R . . . .
N3 N -0.1573(2) 0.46052(14) 0.10201(16) 0.0396(4) Uani 1 1 d . . . . .
H3 H -0.220703 0.409006 0.063898 0.048 Uiso 1 1 d R . . . .
C1 C 0.4652(4) 0.3918(3) 0.5813(3) 0.0775(10) Uani 1 1 d . . . . .
H1A H 0.533696 0.445808 0.621254 0.116 Uiso 1 1 calc GR . . . .
H1B H 0.447565 0.386646 0.512591 0.116 Uiso 1 1 calc GR . . . .
H1C H 0.523001 0.337169 0.625638 0.116 Uiso 1 1 calc GR . . . .
C2 C 0.3197(5) 0.4190(2) 0.6600(3) 0.0691(9) Uani 1 1 d . . . . .
H2A H 0.382117 0.475985 0.693389 0.104 Uiso 1 1 calc GR . . . .
H2B H 0.381421 0.368569 0.711433 0.104 Uiso 1 1 calc GR . . . .
H2C H 0.208884 0.424454 0.641642 0.104 Uiso 1 1 calc GR . . . .
C3 C 0.1850(4) 0.31643(19) 0.5012(2) 0.0532(7) Uani 1 1 d . . . . .
H3A H 0.240732 0.263004 0.550110 0.064 Uiso 1 1 calc R . . . .
H3B H 0.078590 0.327209 0.488982 0.064 Uiso 1 1 calc R . . . .
C4 C 0.1455(4) 0.29474(19) 0.3926(2) 0.0507(6) Uani 1 1 d . . . . .
H4A H 0.249408 0.273853 0.406201 0.061 Uiso 1 1 calc R . . . .
H4B H 0.063481 0.244040 0.357227 0.061 Uiso 1 1 calc R . . . .
C5 C -0.1004(3) 0.3929(2) 0.2692(2) 0.0526(7) Uani 1 1 d . . . . .
H5A H -0.106820 0.404494 0.328651 0.063 Uiso 1 1 calc R . . . .
H5B H -0.170088 0.338739 0.227992 0.063 Uiso 1 1 calc R . . . .
C6 C -0.1700(4) 0.4765(2) 0.1922(2) 0.0544(7) Uani 1 1 d . . . . .
H6A H -0.288711 0.486664 0.159976 0.065 Uiso 1 1 calc R . . . .
H6B H -0.105226 0.531653 0.234193 0.065 Uiso 1 1 calc R . . . .
C7 C -0.2284(4) 0.5386(2) 0.0206(3) 0.0617(8) Uani 1 1 d . . . . .
H7A H -0.337562 0.556737 -0.000490 0.093 Uiso 1 1 calc GR . . . .
H7B H -0.242317 0.518726 -0.044252 0.093 Uiso 1 1 calc GR . . . .
H7C H -0.151229 0.590583 0.054004 0.093 Uiso 1 1 calc GR . . . .
C8 C 0.0231(4) 0.4391(2) 0.1517(3) 0.0567(7) Uani 1 1 d . . . . .
H8A H 0.094859 0.492669 0.193032 0.068 Uiso 1 1 calc R . . . .
H8B H 0.030449 0.425836 0.092904 0.068 Uiso 1 1 calc R . . . .
C9 C 0.0859(4) 0.3567(2) 0.2279(2) 0.0523(6) Uani 1 1 d . . . . .
H9A H 0.017151 0.302556 0.185718 0.063 Uiso 1 1 calc R . . . .
H9B H 0.203657 0.343456 0.259835 0.063 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 2.3712(8) . ?
Mn1 Cl2 2.3859(8) . ?
Mn1 Cl3 2.3369(7) . ?
Mn1 Cl4 2.3503(8) . ?
N1 C1 1.467(4) . ?
N1 C2 1.477(4) . ?
N1 C3 1.510(4) . ?
N2 H2 0.9100 . ?
N2 C4 1.463(3) . ?
N2 C5 1.450(3) . ?
N2 C9 1.451(3) . ?
N3 H3 0.9100 . ?
N3 C6 1.487(3) . ?
N3 C7 1.489(3) . ?
N3 C8 1.486(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.489(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.515(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.500(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 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 Cl2 111.19(4) . . ?
Cl3 Mn1 Cl1 108.47(3) . . ?
Cl3 Mn1 Cl2 111.73(3) . . ?
Cl3 Mn1 Cl4 111.06(3) . . ?
Cl4 Mn1 Cl1 112.63(3) . . ?
Cl4 Mn1 Cl2 101.70(3) . . ?
C1 N1 C2 111.6(3) . . ?
C1 N1 C3 113.8(3) . . ?
C2 N1 C3 108.0(2) . . ?
C4 N2 H2 108.7 . . ?
C5 N2 H2 108.6 . . ?
C5 N2 C4 111.6(2) . . ?
C5 N2 C9 109.6(2) . . ?
C9 N2 H2 108.6 . . ?
C9 N2 C4 109.7(2) . . ?
C6 N3 H3 107.2 . . ?
C6 N3 C7 113.2(2) . . ?
C7 N3 H3 107.2 . . ?
C8 N3 H3 107.2 . . ?
C8 N3 C6 109.6(2) . . ?
C8 N3 C7 112.1(2) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3A 109.0 . . ?
N1 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 N1 112.9(2) . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
N2 C4 C3 113.1(2) . . ?
N2 C4 H4A 109.0 . . ?
N2 C4 H4B 109.0 . . ?
C3 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
N2 C5 H5A 109.4 . . ?
N2 C5 H5B 109.4 . . ?
N2 C5 C6 111.0(2) . . ?
H5A C5 H5B 108.0 . . ?
C6 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
N3 C6 C5 110.0(2) . . ?
N3 C6 H6A 109.7 . . ?
N3 C6 H6B 109.7 . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N3 C7 H7A 109.5 . . ?
N3 C7 H7B 109.5 . . ?
N3 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 H8A 109.6 . . ?
N3 C8 H8B 109.6 . . ?
N3 C8 C9 110.2(2) . . ?
H8A C8 H8B 108.1 . . ?
C9 C8 H8A 109.6 . . ?
C9 C8 H8B 109.6 . . ?
N2 C9 C8 110.9(2) . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_C16H30N4MnCl4
_database_code_depnum_ccdc_archive 'CCDC 2076751'
loop_
_audit_author_name
_audit_author_address
'Hong-Mei Pan'
;Jining University
China
;
_audit_update_record             
;
2021-05-26 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
#================================================
_audit_creation_date             2021-05-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Mn, 2(C8 H15 N2)'
_chemical_formula_sum            'C16 H30 Cl4 Mn N4'
_chemical_formula_weight         475.18
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
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'
'-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                   16.387(4)
_cell_length_b                   15.292(4)
_cell_length_c                   18.810(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4714(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.29
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   0.811
_shelx_estimated_absorpt_T_min   0.218
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_T_max  0.7291
_exptl_absorpt_correction_T_min  0.3993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            29234
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         2.119
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3964
_reflns_number_total             4148
_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       'APEX2 Software Suite (Bruker,2005)'
_computing_data_collection       'APEX2 Software Suite (Bruker,2005)'
_computing_data_reduction        'APEX2 Software Suite (Bruker,2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.184
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4148
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0563
_refine_ls_restrained_S_all      1.068
_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)+(0.0845P)²+6.3225P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1667
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Cl1A)=1-FVAR(1)
 Sof(Cl1)=FVAR(1)
 Sof(Cl3A)=1-FVAR(2)
 Sof(Cl3)=FVAR(2)
 Sof(Cl4A)=1-FVAR(3)
 Sof(Cl4)=FVAR(3)
 Sof(Cl2A)=1-FVAR(4)
 Sof(Cl2)=FVAR(4)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C14(H14A,H14B), C15(H15A,H15B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C9(H9), C10(H10)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C16(H16A,H16B,H16C)
;
_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 0.47060(3) 0.76537(4) 0.65609(3) 0.0443(2) Uani 1 1 d . . . . .
Cl1 Cl 0.4748(11) 0.7860(17) 0.7822(9) 0.065(3) Uani 0.56(11) 1 d . . P A 1
Cl1A Cl 0.4739(15) 0.805(3) 0.7756(17) 0.077(5) Uani 0.44(11) 1 d . . P A 2
Cl2 Cl 0.383(2) 0.870(3) 0.6062(15) 0.061(8) Uani 0.24(16) 1 d . . P A 1
Cl2A Cl 0.3902(13) 0.8764(12) 0.6068(6) 0.080(3) Uani 0.76(16) 1 d . . P A 2
Cl3 Cl 0.4196(7) 0.6217(6) 0.6389(5) 0.0561(16) Uani 0.80(7) 1 d . . P A 1
Cl3A Cl 0.407(2) 0.634(3) 0.630(2) 0.075(8) Uani 0.20(7) 1 d . . P A 2
Cl4 Cl 0.595(3) 0.782(3) 0.596(2) 0.055(6) Uani 0.13(8) 1 d . . P A 1
Cl4A Cl 0.6041(7) 0.7688(10) 0.6071(9) 0.0689(19) Uani 0.87(8) 1 d . . P A 2
N1 N 0.3500(2) 0.6039(2) 0.45594(19) 0.0574(9) Uani 1 1 d . . . . .
N2 N 0.3367(2) 0.4692(2) 0.48513(18) 0.0526(8) Uani 1 1 d . . . . .
C1 C 0.4117(3) 0.5586(4) 0.4235(3) 0.0689(13) Uani 1 1 d . . . . .
H1 H 0.451765 0.582130 0.394189 0.083 Uiso 1 1 calc R . . . .
C2 C 0.4042(3) 0.4749(4) 0.4416(3) 0.0663(13) Uani 1 1 d . . . . .
H2 H 0.437847 0.429093 0.427563 0.080 Uiso 1 1 calc R . . . .
C3 C 0.2335(3) 0.5724(3) 0.5372(3) 0.0679(13) Uani 1 1 d . . . . .
H3A H 0.204615 0.520392 0.550831 0.102 Uiso 1 1 calc GR . . . .
H3B H 0.198152 0.609427 0.509904 0.102 Uiso 1 1 calc GR . . . .
H3C H 0.251127 0.602951 0.579102 0.102 Uiso 1 1 calc GR . . . .
C4 C 0.3379(4) 0.6994(3) 0.4529(3) 0.0833(16) Uani 1 1 d . . . . .
H4A H 0.282210 0.711797 0.440575 0.125 Uiso 1 1 calc GR . . . .
H4B H 0.373466 0.723962 0.417602 0.125 Uiso 1 1 calc GR . . . .
H4C H 0.350063 0.724499 0.498411 0.125 Uiso 1 1 calc GR . . . .
C5 C 0.3099(3) 0.3884(3) 0.5202(3) 0.0643(12) Uani 1 1 d . . . . .
H5A H 0.321365 0.338999 0.489478 0.077 Uiso 1 1 calc R . . . .
H5B H 0.251404 0.390838 0.527753 0.077 Uiso 1 1 calc R . . . .
C6 C 0.3522(4) 0.3751(4) 0.5908(4) 0.101(2) Uani 1 1 d . . . . .
H6A H 0.410787 0.377547 0.583725 0.121 Uiso 1 1 calc R . . . .
H6B H 0.337257 0.422273 0.622732 0.121 Uiso 1 1 calc R . . . .
C7 C 0.3306(4) 0.2895(4) 0.6248(4) 0.110(2) Uani 1 1 d . . . . .
H7A H 0.347036 0.242395 0.594213 0.164 Uiso 1 1 calc GR . . . .
H7B H 0.272697 0.286791 0.632278 0.164 Uiso 1 1 calc GR . . . .
H7C H 0.358197 0.284398 0.669614 0.164 Uiso 1 1 calc GR . . . .
C8 C 0.3052(2) 0.5484(3) 0.4941(2) 0.0496(9) Uani 1 1 d . . . . .
N3 N 0.3009(2) 0.4742(3) 0.2652(2) 0.0608(10) Uani 1 1 d . . . . .
N4 N 0.1770(2) 0.4820(2) 0.30129(19) 0.0550(9) Uani 1 1 d . . . . .
C9 C 0.2062(3) 0.5659(3) 0.2961(3) 0.0773(15) Uani 1 1 d . . . . .
H9 H 0.177471 0.616866 0.306027 0.093 Uiso 1 1 calc R . . . .
C10 C 0.2832(3) 0.5608(4) 0.2741(3) 0.0828(16) Uani 1 1 d . . . . .
H10 H 0.318414 0.607490 0.266199 0.099 Uiso 1 1 calc R . . . .
C11 C 0.2359(2) 0.4269(3) 0.2817(2) 0.0513(10) Uani 1 1 d . . . . .
C12 C 0.3802(3) 0.4404(4) 0.2421(3) 0.0851(16) Uani 1 1 d . . . . .
H12A H 0.408539 0.415886 0.282040 0.128 Uiso 1 1 calc GR . . . .
H12B H 0.411972 0.487236 0.222271 0.128 Uiso 1 1 calc GR . . . .
H12C H 0.372146 0.396022 0.206674 0.128 Uiso 1 1 calc GR . . . .
C13 C 0.2305(3) 0.3313(3) 0.2786(3) 0.0751(14) Uani 1 1 d . . . . .
H13A H 0.176659 0.313146 0.292109 0.113 Uiso 1 1 calc GR . . . .
H13B H 0.269731 0.306232 0.310545 0.113 Uiso 1 1 calc GR . . . .
H13C H 0.241700 0.312018 0.231000 0.113 Uiso 1 1 calc GR . . . .
C14 C 0.0943(2) 0.4583(3) 0.3251(2) 0.0579(11) Uani 1 1 d . . . . .
H14A H 0.076085 0.407021 0.299186 0.069 Uiso 1 1 calc R . . . .
H14B H 0.057130 0.505826 0.314254 0.069 Uiso 1 1 calc R . . . .
C15 C 0.0911(3) 0.4394(4) 0.4038(2) 0.0646(12) Uani 1 1 d . . . . .
H15A H 0.104105 0.492357 0.429847 0.078 Uiso 1 1 calc R . . . .
H15B H 0.132005 0.395861 0.415418 0.078 Uiso 1 1 calc R . . . .
C16 C 0.0083(3) 0.4067(4) 0.4268(3) 0.0760(14) Uani 1 1 d . . . . .
H16A H -0.005756 0.355612 0.399812 0.114 Uiso 1 1 calc GR . . . .
H16B H -0.031764 0.451463 0.418799 0.114 Uiso 1 1 calc GR . . . .
H16C H 0.009715 0.392281 0.476465 0.114 Uiso 1 1 calc GR . . . .


_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 2.395(17) . ?
Mn1 Cl1A 2.33(2) . ?
Mn1 Cl2 2.35(3) . ?
Mn1 Cl2A 2.340(10) . ?
Mn1 Cl3 2.373(6) . ?
Mn1 Cl3A 2.32(3) . ?
Mn1 Cl4 2.35(3) . ?
Mn1 Cl4A 2.374(6) . ?
N1 C1 1.370(6) . ?
N1 C4 1.474(6) . ?
N1 C8 1.333(5) . ?
N2 C2 1.378(5) . ?
N2 C5 1.467(6) . ?
N2 C8 1.327(5) . ?
C1 H1 0.9300 . ?
C1 C2 1.330(7) . ?
C2 H2 0.9300 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 C8 1.474(6) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.512(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.499(8) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
N3 C10 1.366(7) . ?
N3 C11 1.325(5) . ?
N3 C12 1.465(6) . ?
N4 C9 1.373(6) . ?
N4 C11 1.333(5) . ?
N4 C14 1.473(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.330(7) . ?
C10 H10 0.9300 . ?
C11 C13 1.465(7) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.508(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C16 1.510(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?

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
Cl1A Mn1 Cl2A 102.0(11) . . ?
Cl1A Mn1 Cl4A 110.4(7) . . ?
Cl2 Mn1 Cl1 108.9(10) . . ?
Cl2 Mn1 Cl3 111.1(12) . . ?
Cl2A Mn1 Cl4A 110.4(8) . . ?
Cl3 Mn1 Cl1 105.5(6) . . ?
Cl3A Mn1 Cl1A 116.2(15) . . ?
Cl3A Mn1 Cl2A 107.0(16) . . ?
Cl3A Mn1 Cl4A 110.4(8) . . ?
Cl4 Mn1 Cl1 116.0(12) . . ?
Cl4 Mn1 Cl2 105.5(17) . . ?
Cl4 Mn1 Cl3 110.0(10) . . ?
C1 N1 C4 125.7(4) . . ?
C8 N1 C1 108.9(4) . . ?
C8 N1 C4 125.3(4) . . ?
C2 N2 C5 124.1(4) . . ?
C8 N2 C2 109.3(4) . . ?
C8 N2 C5 126.4(4) . . ?
N1 C1 H1 126.1 . . ?
C2 C1 N1 107.7(4) . . ?
C2 C1 H1 126.1 . . ?
N2 C2 H2 126.6 . . ?
C1 C2 N2 106.7(4) . . ?
C1 C2 H2 126.6 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C8 C3 H3A 109.5 . . ?
C8 C3 H3B 109.5 . . ?
C8 C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.3 . . ?
N2 C5 H5B 109.3 . . ?
N2 C5 C6 111.8(4) . . ?
H5A C5 H5B 107.9 . . ?
C6 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C5 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
C7 C6 C5 112.6(5) . . ?
C7 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C3 125.2(4) . . ?
N2 C8 N1 107.4(4) . . ?
N2 C8 C3 127.4(4) . . ?
C10 N3 C12 124.5(4) . . ?
C11 N3 C10 109.2(4) . . ?
C11 N3 C12 126.2(4) . . ?
C9 N4 C14 125.0(4) . . ?
C11 N4 C9 108.5(4) . . ?
C11 N4 C14 126.5(4) . . ?
N4 C9 H9 126.3 . . ?
C10 C9 N4 107.4(5) . . ?
C10 C9 H9 126.3 . . ?
N3 C10 H10 126.4 . . ?
C9 C10 N3 107.2(5) . . ?
C9 C10 H10 126.4 . . ?
N3 C11 N4 107.6(4) . . ?
N3 C11 C13 125.7(4) . . ?
N4 C11 C13 126.7(4) . . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N4 C14 H14A 109.2 . . ?
N4 C14 H14B 109.2 . . ?
N4 C14 C15 112.2(4) . . ?
H14A C14 H14B 107.9 . . ?
C15 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C14 C15 H15A 109.2 . . ?
C14 C15 H15B 109.2 . . ?
C14 C15 C16 112.1(4) . . ?
H15A C15 H15B 107.9 . . ?
C16 C15 H15A 109.2 . . ?
C16 C15 H15B 109.2 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_C10H28N4MnCl4
_database_code_depnum_ccdc_archive 'CCDC 2076752'
loop_
_audit_author_name
_audit_author_address
'Hong-Mei Pan'
;Jining University
China
;
_audit_update_record             
;
2021-05-27 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
#================================================
_audit_creation_date             2021-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Mn, 2(Cl), 2(C5 H14 N2)'
_chemical_formula_sum            'C10 H28 Cl6 Mn N4'
_chemical_formula_weight         472.00
_chemical_absolute_configuration ?
_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 0.0181 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           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
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                   8.04650(10)
_cell_length_b                   15.39100(10)
_cell_length_c                   16.93960(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2097.86(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.29
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   0.811
_shelx_estimated_absorpt_T_min   0.218
_exptl_absorpt_coefficient_mu    12.136
_exptl_absorpt_correction_T_max  0.7291
_exptl_absorpt_correction_T_min  0.3993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48524
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.157
_diffrn_reflns_theta_min         3.880
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.742
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                4189
_reflns_number_total             4312
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'APEX2 Software Suite (Bruker,2005)'
_computing_data_collection       'APEX2 Software Suite (Bruker,2005)'
_computing_data_reduction        'APEX2 Software Suite (Bruker,2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.005(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4312
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0246
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0285P)²+1.0629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0621
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 1.005(6)
 -0.005(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 N1(H1), N3(H3)
3.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N4(H4A,H4B), C1(H1A,H1B), C2(H2C,H2D), C3(H3A,H3B), C4(H4C,H4D),
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B)
3.c Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C)
;
_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 0.67844(6) 0.55172(3) 0.77719(3) 0.03475(12) Uani 1 1 d . . . . .
Cl1 Cl 0.66052(10) 0.67715(5) 0.69432(4) 0.04190(17) Uani 1 1 d . . . . .
Cl2 Cl 0.95128(10) 0.49809(6) 0.76466(5) 0.04599(18) Uani 1 1 d . . . . .
Cl3 Cl 0.60584(14) 0.60560(7) 0.90244(5) 0.0589(2) Uani 1 1 d . . . . .
Cl4 Cl 0.47577(11) 0.45058(6) 0.73563(5) 0.0526(2) Uani 1 1 d . . . . .
Cl5 Cl 0.76759(10) 0.29314(5) 0.91158(5) 0.04375(18) Uani 1 1 d . . . . .
Cl6 Cl 0.40847(14) 0.37767(5) 0.47113(5) 0.0531(2) Uani 1 1 d . . . . .
N1 N 0.4524(4) 0.22295(17) 0.36540(17) 0.0457(7) Uani 1 1 d . . . . .
H1 H 0.448654 0.274203 0.399680 0.055 Uiso 1 1 calc R . . . .
N2 N 0.1290(4) 0.2402(2) 0.2979(2) 0.0603(9) Uani 1 1 d . . . . .
H2A H 0.032268 0.267751 0.293386 0.072 Uiso 1 1 calc R . . . .
H2B H 0.127528 0.194742 0.265462 0.072 Uiso 1 1 calc R . . . .
N3 N 0.1437(3) 0.61177(16) 0.52553(14) 0.0350(5) Uani 1 1 d . . . . .
H3 H 0.162800 0.673633 0.535814 0.042 Uiso 1 1 calc R . . . .
N4 N 0.4484(3) 0.57522(15) 0.44273(14) 0.0331(5) Uani 1 1 d . . . . .
H4A H 0.545268 0.593492 0.423514 0.040 Uiso 1 1 calc R . . . .
H4B H 0.438631 0.518913 0.431692 0.040 Uiso 1 1 calc R . . . .
C1 C 0.3113(4) 0.6237(2) 0.40413(17) 0.0375(6) Uani 1 1 d . . . . .
H1A H 0.312124 0.611693 0.347916 0.045 Uiso 1 1 calc R . . . .
H1B H 0.328495 0.685547 0.411342 0.045 Uiso 1 1 calc R . . . .
C2 C 0.2645(5) 0.2991(2) 0.2750(2) 0.0457(7) Uani 1 1 d . . . . .
H2C H 0.263119 0.350221 0.308529 0.055 Uiso 1 1 calc R . . . .
H2D H 0.249131 0.317730 0.220826 0.055 Uiso 1 1 calc R . . . .
C3 C 0.2809(4) 0.5620(2) 0.56358(17) 0.0390(7) Uani 1 1 d . . . . .
H3A H 0.263013 0.500326 0.555544 0.047 Uiso 1 1 calc R . . . .
H3B H 0.280378 0.573093 0.619956 0.047 Uiso 1 1 calc R . . . .
C4 C 0.1464(4) 0.5985(2) 0.43792(16) 0.0371(7) Uani 1 1 d . . . . .
H4C H 0.124184 0.537957 0.426075 0.044 Uiso 1 1 calc R . . . .
H4D H 0.059748 0.633274 0.413710 0.044 Uiso 1 1 calc R . . . .
C5 C 0.4276(4) 0.2534(2) 0.2832(2) 0.0469(8) Uani 1 1 d . . . . .
H5A H 0.430783 0.204089 0.247510 0.056 Uiso 1 1 calc R . . . .
H5B H 0.516892 0.292626 0.268696 0.056 Uiso 1 1 calc R . . . .
C6 C 0.3131(5) 0.1650(2) 0.38927(19) 0.0509(9) Uani 1 1 d . . . . .
H6A H 0.326771 0.148251 0.444088 0.061 Uiso 1 1 calc R . . . .
H6B H 0.315144 0.112646 0.357399 0.061 Uiso 1 1 calc R . . . .
C7 C 0.4467(4) 0.5875(2) 0.52977(19) 0.0407(7) Uani 1 1 d . . . . .
H7A H 0.469321 0.647855 0.542134 0.049 Uiso 1 1 calc R . . . .
H7B H 0.533277 0.552286 0.553532 0.049 Uiso 1 1 calc R . . . .
C8 C -0.0218(5) 0.5886(3) 0.5586(2) 0.0566(10) Uani 1 1 d . . . . .
H8A H -0.106381 0.622002 0.532540 0.085 Uiso 1 1 calc R . . . .
H8B H -0.042359 0.527834 0.550412 0.085 Uiso 1 1 calc R . . . .
H8C H -0.023487 0.601070 0.614103 0.085 Uiso 1 1 calc R . . . .
C9 C 0.1494(6) 0.2099(3) 0.3790(3) 0.0659(12) Uani 1 1 d . . . . .
H9A H 0.060130 0.170122 0.392077 0.079 Uiso 1 1 calc R . . . .
H9B H 0.143088 0.259010 0.414773 0.079 Uiso 1 1 calc R . . . .
C10 C 0.6167(6) 0.1816(3) 0.3766(4) 0.096(2) Uani 1 1 d . . . . .
H10A H 0.627672 0.162869 0.430442 0.145 Uiso 1 1 calc R . . . .
H10B H 0.626241 0.132306 0.342164 0.145 Uiso 1 1 calc R . . . .
H10C H 0.702747 0.222678 0.364564 0.145 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 2.3913(9) . ?
Mn1 Cl2 2.3550(9) . ?
Mn1 Cl3 2.3516(9) . ?
Mn1 Cl4 2.3619(9) . ?
N1 H1 0.9800 . ?
N1 C5 1.483(5) . ?
N1 C6 1.489(5) . ?
N1 C10 1.479(5) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.470(5) . ?
N2 C9 1.459(6) . ?
N3 H3 0.9800 . ?
N3 C3 1.490(4) . ?
N3 C4 1.498(3) . ?
N3 C8 1.488(4) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 C1 1.483(4) . ?
N4 C7 1.487(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C4 1.496(4) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C2 C5 1.496(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C7 1.504(5) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C9 1.497(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?

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
Cl2 Mn1 Cl1 106.64(3) . . ?
Cl2 Mn1 Cl4 112.69(4) . . ?
Cl3 Mn1 Cl1 103.30(4) . . ?
Cl3 Mn1 Cl2 115.88(4) . . ?
Cl3 Mn1 Cl4 109.26(4) . . ?
Cl4 Mn1 Cl1 108.38(4) . . ?
C5 N1 H1 107.3 . . ?
C5 N1 C6 110.1(3) . . ?
C6 N1 H1 107.3 . . ?
C10 N1 H1 107.3 . . ?
C10 N1 C5 112.1(4) . . ?
C10 N1 C6 112.3(3) . . ?
H2A N2 H2B 108.0 . . ?
C2 N2 H2A 109.4 . . ?
C2 N2 H2B 109.4 . . ?
C9 N2 H2A 109.4 . . ?
C9 N2 H2B 109.4 . . ?
C9 N2 C2 111.2(3) . . ?
C3 N3 H3 107.8 . . ?
C3 N3 C4 110.3(2) . . ?
C4 N3 H3 107.8 . . ?
C8 N3 H3 107.8 . . ?
C8 N3 C3 112.2(3) . . ?
C8 N3 C4 110.7(3) . . ?
H4A N4 H4B 108.0 . . ?
C1 N4 H4A 109.3 . . ?
C1 N4 H4B 109.3 . . ?
C1 N4 C7 111.5(2) . . ?
C7 N4 H4A 109.3 . . ?
C7 N4 H4B 109.3 . . ?
N4 C1 H1A 109.4 . . ?
N4 C1 H1B 109.4 . . ?
N4 C1 C4 111.2(2) . . ?
H1A C1 H1B 108.0 . . ?
C4 C1 H1A 109.4 . . ?
C4 C1 H1B 109.4 . . ?
N2 C2 H2C 109.7 . . ?
N2 C2 H2D 109.7 . . ?
N2 C2 C5 109.7(3) . . ?
H2C C2 H2D 108.2 . . ?
C5 C2 H2C 109.7 . . ?
C5 C2 H2D 109.7 . . ?
N3 C3 H3A 109.4 . . ?
N3 C3 H3B 109.4 . . ?
N3 C3 C7 111.0(2) . . ?
H3A C3 H3B 108.0 . . ?
C7 C3 H3A 109.4 . . ?
C7 C3 H3B 109.4 . . ?
N3 C4 H4C 109.5 . . ?
N3 C4 H4D 109.5 . . ?
C1 C4 N3 110.9(3) . . ?
C1 C4 H4C 109.5 . . ?
C1 C4 H4D 109.5 . . ?
H4C C4 H4D 108.0 . . ?
N1 C5 C2 110.7(3) . . ?
N1 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
N1 C6 C9 110.7(3) . . ?
H6A C6 H6B 108.1 . . ?
C9 C6 H6A 109.5 . . ?
C9 C6 H6B 109.5 . . ?
N4 C7 C3 110.7(3) . . ?
N4 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C6 110.8(3) . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.005(6)
2 -0.005(6)

