# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_MnMn_dmbpy
_database_code_depnum_ccdc_archive 'CCDC 2304502'
loop_
_audit_author_name
_audit_author_address
'Haruka Yoshino'
;Tohoku University
Japan
;
_audit_update_record             
;
2023-12-22 deposited with the CCDC.	2024-01-16 downloaded from the CCDC.
;
_audit_creation_date             2023-02-24
_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         '0.5(C32 H24 Mn4 N14)'
_chemical_formula_sum            'C16 H12 Mn2 N7'
_chemical_formula_weight         412.21
_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'
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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   13.990
_cell_length_b                   7.058
_cell_length_c                   16.715
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1650.4
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.71
_cell_measurement_theta_min      2.41
_shelx_estimated_absorpt_T_max   0.877
_shelx_estimated_absorpt_T_min   0.830
_exptl_absorpt_coefficient_mu    1.544
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6219
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1263 before and 0.0649 after correction. The Ratio of minimum to maximum transmission is 0.8338. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'pinkish orange'
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.0973
_exptl_crystal_size_min          0.0875
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17116
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.362
_diffrn_reflns_theta_min         1.898
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1997
_reflns_number_total             2367
_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       'SAINT V8.40A (?, 2016)'
_computing_data_collection       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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         0.623
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2367
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0329
_refine_ls_restrained_S_all      1.048
_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)+(0.0427P)²+0.8429P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0864
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5) H13A(0.5) H13B(0.5) H13C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C13(H13A,H13B,H13C)
;
_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 0.39793(2) 0.250000 0.68110(2) 0.00942(11) Uani 1 2 d S T P . .
Mn2 Mn 0.62139(2) 0.750000 0.81595(2) 0.01130(11) Uani 1 2 d S T P . .
N4 N 0.34484(14) 0.250000 0.55431(13) 0.0148(4) Uani 1 2 d S T P . .
N5 N 0.52457(15) 0.250000 0.59577(12) 0.0147(4) Uani 1 2 d S T P . .
N1 N 0.48078(10) 0.4579(2) 0.74744(9) 0.0179(3) Uani 1 1 d . . . . .
N3 N 0.60311(15) 0.750000 0.90314(14) 0.0199(5) Uani 1 2 d S T P . .
N2 N 0.78302(11) 1.0423(2) 0.80083(10) 0.0180(3) Uani 1 1 d . . . . .
C1 C 0.53232(12) 0.5631(2) 0.77505(11) 0.0154(3) Uani 1 1 d . . . . .
C2 C 0.72229(12) 0.9366(3) 0.80502(11) 0.0158(3) Uani 1 1 d . . . . .
C3 C 0.25241(17) 0.250000 0.53704(16) 0.0173(5) Uani 1 2 d S T P . .
H3 H 0.208230 0.250000 0.580201 0.021 Uiso 1 2 calc RS T P . .
C4 C 0.21682(19) 0.250000 0.46101(17) 0.0204(5) Uani 1 2 d S T P . .
C5 C 0.1121(2) 0.250000 0.4467(2) 0.0296(7) Uani 1 2 d S T P . .
H5A H 0.079880 0.182866 0.490364 0.044 Uiso 0.5 1 calc GR . . A -1
H5B H 0.098332 0.186230 0.395884 0.044 Uiso 0.5 1 calc GR . . A -1
H5C H 0.088869 0.380903 0.444338 0.044 Uiso 0.5 1 calc GR . . A -1
C6 C 0.2821(2) 0.250000 0.39997(17) 0.0234(6) Uani 1 2 d S T P . .
H6 H 0.260994 0.250000 0.345956 0.028 Uiso 1 2 calc RS T P . .
C7 C 0.3772(2) 0.250000 0.41673(16) 0.0221(6) Uani 1 2 d S T P . .
H7 H 0.422657 0.250000 0.374518 0.027 Uiso 1 2 calc RS T P . .
C8 C 0.40692(17) 0.250000 0.49418(15) 0.0141(5) Uani 1 2 d S T P . .
C9 C 0.50765(17) 0.250000 0.51780(15) 0.0139(5) Uani 1 2 d S T P . .
C10 C 0.58088(19) 0.250000 0.46350(16) 0.0205(5) Uani 1 2 d S T P . .
H10 H 0.567963 0.250000 0.407700 0.025 Uiso 1 2 calc RS T P . .
C11 C 0.67245(19) 0.250000 0.49082(16) 0.0208(5) Uani 1 2 d S T P . .
H11 H 0.723860 0.250000 0.453688 0.025 Uiso 1 2 calc RS T P . .
C12 C 0.69141(17) 0.250000 0.57099(15) 0.0171(5) Uani 1 2 d S T P . .
C13 C 0.78982(18) 0.250000 0.60370(17) 0.0230(6) Uani 1 2 d S T P . .
H13A H 0.835287 0.220953 0.560826 0.034 Uiso 0.5 1 calc GR . . B -1
H13B H 0.794946 0.153971 0.645837 0.034 Uiso 0.5 1 calc GR . . B -1
H13C H 0.804315 0.375076 0.626095 0.034 Uiso 0.5 1 calc GR . . B -1
C14 C 0.61348(17) 0.250000 0.62084(16) 0.0169(5) Uani 1 2 d S T P . .
H14 H 0.624553 0.250000 0.676911 0.020 Uiso 1 2 calc RS T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.00233(17) 0.01137(19) 0.01456(19) 0.000 -0.00056(12) 0.000
Mn2 0.00331(17) 0.0136(2) 0.0169(2) 0.000 -0.00145(13) 0.000
N4 0.0081(9) 0.0196(11) 0.0168(10) 0.000 -0.0006(8) 0.000
N5 0.0079(9) 0.0197(10) 0.0164(10) 0.000 0.0008(8) 0.000
N1 0.0077(6) 0.0192(7) 0.0268(8) -0.0055(6) -0.0003(6) 0.0001(5)
N3 0.0079(9) 0.0294(12) 0.0223(12) 0.000 -0.0001(8) 0.000
N2 0.0093(7) 0.0195(8) 0.0252(8) -0.0048(6) 0.0015(6) -0.0028(6)
C1 0.0078(7) 0.0173(8) 0.0210(8) 0.0005(6) 0.0001(6) 0.0026(6)
C2 0.0092(7) 0.0173(8) 0.0210(9) -0.0008(7) -0.0013(6) 0.0024(6)
C3 0.0089(11) 0.0237(13) 0.0192(13) 0.000 -0.0016(9) 0.000
C4 0.0147(12) 0.0229(13) 0.0238(14) 0.000 -0.0064(10) 0.000
C5 0.0141(13) 0.0441(19) 0.0306(15) 0.000 -0.0097(11) 0.000
C6 0.0204(13) 0.0331(15) 0.0168(13) 0.000 -0.0056(10) 0.000
C7 0.0215(13) 0.0283(15) 0.0165(12) 0.000 0.0001(10) 0.000
C8 0.0117(11) 0.0146(11) 0.0158(12) 0.000 -0.0004(9) 0.000
C9 0.0099(11) 0.0137(11) 0.0180(12) 0.000 0.0023(9) 0.000
C10 0.0146(12) 0.0292(14) 0.0178(13) 0.000 0.0041(10) 0.000
C11 0.0121(11) 0.0280(14) 0.0224(13) 0.000 0.0081(10) 0.000
C12 0.0081(11) 0.0203(13) 0.0228(13) 0.000 0.0034(9) 0.000
C13 0.0071(11) 0.0353(15) 0.0266(14) 0.000 0.0041(10) 0.000
C14 0.0073(10) 0.0252(13) 0.0180(12) 0.000 0.0017(9) 0.000

_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 N4 2.246(2) . ?
Mn1 N5 2.275(2) . ?
Mn1 N1 2.1740(15) . ?
Mn1 N1 2.1740(15) 7_565 ?
Mn1 N2 2.1963(15) 4_466 ?
Mn1 N2 2.1963(15) 6_547 ?
Mn2 N3 1.480(2) . ?
Mn2 C1 1.9392(18) . ?
Mn2 C1 1.9393(18) 7_575 ?
Mn2 C2 1.9391(18) 7_575 ?
Mn2 C2 1.9391(18) . ?
N4 C3 1.325(3) . ?
N4 C8 1.328(3) . ?
N5 C9 1.325(3) . ?
N5 C14 1.313(3) . ?
N1 C1 1.133(2) . ?
N2 C2 1.133(2) . ?
C3 C4 1.365(4) . ?
C4 C5 1.485(4) . ?
C4 C6 1.370(4) . ?
C6 C7 1.359(4) . ?
C7 C8 1.360(4) . ?
C8 C9 1.464(3) . ?
C9 C10 1.369(3) . ?
C10 C11 1.360(4) . ?
C11 C12 1.366(4) . ?
C12 C13 1.481(4) . ?
C12 C14 1.372(3) . ?

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
N4 Mn1 N5 70.48(7) . . ?
N1 Mn1 N4 131.12(5) . . ?
N1 Mn1 N4 131.12(5) 7_565 . ?
N1 Mn1 N5 84.52(6) 7_565 . ?
N1 Mn1 N5 84.52(6) . . ?
N1 Mn1 N1 84.90(8) 7_565 . ?
N1 Mn1 N2 140.40(6) . 6_547 ?
N1 Mn1 N2 82.52(6) 7_565 6_547 ?
N1 Mn1 N2 140.40(6) 7_565 4_466 ?
N1 Mn1 N2 82.51(5) . 4_466 ?
N2 Mn1 N4 83.55(6) 4_466 . ?
N2 Mn1 N4 83.55(6) 6_547 . ?
N2 Mn1 N5 131.03(5) 6_547 . ?
N2 Mn1 N5 131.03(5) 4_466 . ?
N2 Mn1 N2 83.71(8) 6_547 4_466 ?
N3 Mn2 C1 103.66(8) . . ?
N3 Mn2 C1 103.66(8) . 7_575 ?
N3 Mn2 C2 102.62(8) . . ?
N3 Mn2 C2 102.62(8) . 7_575 ?
C1 Mn2 C1 85.74(10) . 7_575 ?
C2 Mn2 C1 88.43(7) . 7_575 ?
C2 Mn2 C1 153.72(8) . . ?
C2 Mn2 C1 88.43(7) 7_575 . ?
C2 Mn2 C1 153.72(8) 7_575 7_575 ?
C2 Mn2 C2 85.55(10) . 7_575 ?
C3 N4 Mn1 121.90(17) . . ?
C3 N4 C8 118.3(2) . . ?
C8 N4 Mn1 119.85(16) . . ?
C9 N5 Mn1 118.54(16) . . ?
C14 N5 Mn1 122.55(17) . . ?
C14 N5 C9 118.9(2) . . ?
C1 N1 Mn1 171.57(15) . . ?
C2 N2 Mn1 168.50(14) . 6_667 ?
N1 C1 Mn2 176.52(17) . . ?
N2 C2 Mn2 177.48(16) . . ?
N4 C3 C4 124.0(2) . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 C6 116.8(2) . . ?
C6 C4 C5 122.6(3) . . ?
C7 C6 C4 119.9(3) . . ?
C6 C7 C8 119.7(3) . . ?
N4 C8 C7 121.3(2) . . ?
N4 C8 C9 115.2(2) . . ?
C7 C8 C9 123.5(2) . . ?
N5 C9 C8 115.9(2) . . ?
N5 C9 C10 121.2(2) . . ?
C10 C9 C8 122.8(2) . . ?
C11 C10 C9 118.8(2) . . ?
C10 C11 C12 120.8(2) . . ?
C11 C12 C13 122.9(2) . . ?
C11 C12 C14 116.2(2) . . ?
C14 C12 C13 121.0(2) . . ?
N5 C14 C12 124.0(2) . . ?

_shelx_res_file                  
;
TITL 220127_mn55dmebpymn_7_sc_analysis2_0m_a.res in Pnma
    220127_mn55dmebpymn_7_sc_analysis2_0m.res
    created by SHELXL-2018/3 at 10:08:09 on 24-Feb-2023
REM Old TITL 220127_mn55dmebpymn_7_sc_analysis2_0m_a.res in Pnma
REM SHELXT solution in Pnma: R1 0.081, Rweak 0.002, Alpha 0.031
REM <I/s> 0.577 for 143 systematic absences, Orientation as input
REM Formula found by SHELXT: C16 Mn1 N7
CELL 0.71073 13.9905 7.0575 16.7147 90 90 90
ZERR 4 0 0 0 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Mn N
UNIT 64 48 8 28

L.S. 30
PLAN  3
SIZE 0.125 0.0973 0.0875
TEMP -173(2)
list 4
fmap 2 53
acta
OMIT 1 2 2
OMIT 3 0 5
OMIT 2 0 0
OMIT 2 2 0
OMIT 2 1 3
OMIT 5 0 3
OMIT 4 0 2
OMIT 6 1 1
OMIT 3 0 1
OMIT 8 3 0
OMIT 0 4 2
REM <olex2.extras>
REM <HklSrc "%.\\220127_mn55dmebpymn_7_sc_analysis2_0m.hkl">
REM </olex2.extras>

WGHT    0.042700    0.842900
FVAR       0.30272
MN1   3    0.397932    0.250000    0.681102    10.50000    0.00233    0.01137 =
         0.01456    0.00000   -0.00056    0.00000
MN2   3    0.621386    0.750000    0.815946    10.50000    0.00331    0.01363 =
         0.01695    0.00000   -0.00145    0.00000
N4    4    0.344839    0.250000    0.554308    10.50000    0.00812    0.01965 =
         0.01676    0.00000   -0.00059    0.00000
N5    4    0.524570    0.250000    0.595768    10.50000    0.00793    0.01974 =
         0.01639    0.00000    0.00083    0.00000
N1    4    0.480781    0.457918    0.747442    11.00000    0.00768    0.01917 =
         0.02682   -0.00550   -0.00030    0.00008
N3    4    0.603109    0.750000    0.903138    10.50000    0.00791    0.02939 =
         0.02227    0.00000   -0.00015    0.00000
N2    4    0.783021    1.042346    0.800825    11.00000    0.00933    0.01945 =
         0.02522   -0.00479    0.00152   -0.00284
C1    1    0.532316    0.563060    0.775053    11.00000    0.00782    0.01726 =
         0.02100    0.00051    0.00012    0.00262
C2    1    0.722288    0.936587    0.805022    11.00000    0.00918    0.01728 =
         0.02105   -0.00075   -0.00129    0.00236
C3    1    0.252412    0.250000    0.537042    10.50000    0.00889    0.02366 =
         0.01924    0.00000   -0.00162    0.00000
AFIX  43
H3    2    0.208230    0.250000    0.580201    10.50000   -1.20000
AFIX   0
C4    1    0.216820    0.250000    0.461015    10.50000    0.01469    0.02285 =
         0.02377    0.00000   -0.00642    0.00000
C5    1    0.112070    0.250000    0.446682    10.50000    0.01409    0.04413 =
         0.03055    0.00000   -0.00973    0.00000
PART -1
AFIX 137
H5A   2    0.079880    0.182866    0.490364    10.50000   -1.50000
H5B   2    0.098332    0.186230    0.395884    10.50000   -1.50000
H5C   2    0.088869    0.380903    0.444338    10.50000   -1.50000
AFIX   0
PART 0
C6    1    0.282126    0.250000    0.399970    10.50000    0.02037    0.03312 =
         0.01680    0.00000   -0.00556    0.00000
AFIX  43
H6    2    0.260994    0.250000    0.345956    10.50000   -1.20000
AFIX   0
C7    1    0.377187    0.250000    0.416729    10.50000    0.02147    0.02826 =
         0.01653    0.00000    0.00014    0.00000
AFIX  43
H7    2    0.422657    0.250000    0.374518    10.50000   -1.20000
AFIX   0
C8    1    0.406924    0.250000    0.494179    10.50000    0.01174    0.01461 =
         0.01583    0.00000   -0.00045    0.00000
C9    1    0.507653    0.250000    0.517799    10.50000    0.00992    0.01373 =
         0.01802    0.00000    0.00229    0.00000
C10   1    0.580875    0.250000    0.463499    10.50000    0.01455    0.02920 =
         0.01776    0.00000    0.00410    0.00000
AFIX  43
H10   2    0.567963    0.250000    0.407700    10.50000   -1.20000
AFIX   0
C11   1    0.672450    0.250000    0.490818    10.50000    0.01206    0.02796 =
         0.02242    0.00000    0.00811    0.00000
AFIX  43
H11   2    0.723860    0.250000    0.453688    10.50000   -1.20000
AFIX   0
C12   1    0.691409    0.250000    0.570989    10.50000    0.00808    0.02031 =
         0.02278    0.00000    0.00338    0.00000
C13   1    0.789816    0.250000    0.603705    10.50000    0.00714    0.03526 =
         0.02656    0.00000    0.00405    0.00000
PART -1
AFIX 137
H13A  2    0.835287    0.220953    0.560826    10.50000   -1.50000
H13B  2    0.794946    0.153971    0.645837    10.50000   -1.50000
H13C  2    0.804315    0.375076    0.626095    10.50000   -1.50000
AFIX   0
PART 0
C14   1    0.613480    0.250000    0.620835    10.50000    0.00735    0.02523 =
         0.01803    0.00000    0.00172    0.00000
AFIX  43
H14   2    0.624553    0.250000    0.676911    10.50000   -1.20000
AFIX   0
HKLF 4




REM  220127_mn55dmebpymn_7_sc_analysis2_0m_a.res in Pnma
REM wR2 = 0.0864, GooF = S = 1.048, Restrained GooF = 1.048 for all data
REM R1 = 0.0329 for 1997 Fo > 4sig(Fo) and 0.0420 for all 2367 data
REM 141 parameters refined using 0 restraints

END

WGHT      0.0427      0.8429

REM Highest difference peak  0.623,  deepest hole -0.794,  1-sigma level  0.085
Q1    1   0.6242  0.6220  0.8154  11.00000  0.05    0.62
Q2    1   0.6121  0.8494  0.8625  11.00000  0.05    0.45
Q3    1   0.3961  0.3618  0.6781  11.00000  0.05    0.44
;
_shelx_res_checksum              30975
_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_MnCr_dmbpy
_database_code_depnum_ccdc_archive 'CCDC 2304698'
loop_
_audit_author_name
_audit_author_address
'Haruka Yoshino'
;Tohoku University
Japan
;
_audit_update_record             
;
2023-10-31 deposited with the CCDC.	2024-01-16 downloaded from the CCDC.
;

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            MnCr_dmbpy
# Get _chemical_formula_moiety using checkCIF
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C16 H11 Cr N7 Mn'
_chemical_formula_weight         408.240
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mn Mn 0.1939 1.7118 'International Tables for Crystallography, Vol. C'
N N 0.0136 0.0094 'International Tables for Crystallography, Vol. C'
C C 0.0072 0.0048 'International Tables for Crystallography, Vol. C'
H H -0.0006 0.0000 'International Tables for Crystallography, Vol. C'
Cr Cr 0.2683 1.4563 'International Tables for Crystallography, Vol. C'

#===============================================================================
# 6. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
_space_group_IT_number           62

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,-y,z+1/2
3 -x,y+1/2,-z
4 x+1/2,-y+1/2,-z+1/2
5 -x,-y,-z
6 x+1/2,y,-z+1/2
7 x,-y+1/2,z
8 -x+1/2,y+1/2,z+1/2

_cell_length_a                   14.3053(7)
_cell_length_b                   7.2469(2)
_cell_length_c                   17.0304(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1765.5(1)
# If checkCIF gives a different Z value, change both
# _chemical_formula_sum and _chemical_formula_weight.
_cell_formula_units_Z            4
_cell_measurement_temperature    100

_cell_special_details            ?

_exptl_crystal_density_diffrn    1.5359
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             820.00
_exptl_crystal_description       powder

# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; ?
;
_pd_spec_mount_mode              reflection

_pd_spec_shape                   flat_sheet

_pd_char_particle_morphology     ?
_pd_char_colour                  ?

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min.  The pressure at which the sample was
# prepared is in kPa.  The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

_exptl_absorpt_coefficient_mu    ?
# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_correction_type   ? # include if applicable
_exptl_absorpt_process_details   ? # include if applicable
_exptl_absorpt_correction_T_min  ? # include if applicable
_exptl_absorpt_correction_T_max  ? # include if applicable

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      100
_diffrn_source                   'Synchrotron radiation'
_diffrn_source_target            ?
_diffrn_source_type              'SAGA-LS BL15'
_diffrn_radiation_type           Synchrotron
_diffrn_measurement_device_type  Debye-Scherrer
_diffrn_detector                 'Imaging plate'
_diffrn_detector_type            ?

_pd_meas_scan_method             step # options are 'step', 'cont',
#' 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
; ?
;

_diffrn_radiation_wavelength     1.138000
_diffrn_radiation_monochromator  ?

# The following four items give details of the measured (not processed)
# powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        3001
_pd_meas_2theta_range_min        5.0000
_pd_meas_2theta_range_max        50.0000
_pd_meas_2theta_range_inc        0.0150

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/detc         ?
_pd_meas_2theta_fixed            ?

#===============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_pd_calc_method                  'Rietveld Refinement'

_pd_proc_ls_profile_function     'split Pearson VII function'
_pd_proc_ls_background_function  'composite background function'
_pd_proc_ls_pref_orient_corr     
; ?
;
# Replace '; ?' with the following four lines for the March-Dollase function:
#; $P_k = \sum_{j=1}^{m_k} \frac{1}{m_k}
#\left( r^2 \cos^2 \alpha_j +r^{-1}\ sin^2 \alpha_j \right)^{-3/2}$
#with a preferred-orientation vector, (hkl),
#and <i>r</i> = 1.0(0)

_pd_proc_ls_prof_R_factor        0.00646
_pd_proc_ls_prof_wR_factor       0.00868
_pd_proc_ls_prof_wR_expected     0.06045
_refine_ls_R_I_factor            0.01064
_refine_ls_R_Fsqd_factor         0.00747
_refine_ls_R_factor_all          0.00589

_refine_special_details          
; ?
;

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/yi
# The following line must be commented out in the absence of H atoms.
#_refine_ls_hydrogen_treatment       riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     50
_refine_ls_number_restraints     0
_refine_ls_number_constraints    18

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   0.1436

_refine_ls_restrained_S_all      ?
# The following item can be obtained by setting NPRINT at 2 in *.ins.
_refine_ls_shift/su_max          0.0
_refine_ls_shift/su_mean         ?

_refine_diff_density_max         0.0
_refine_diff_density_min         0.0

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.

_pd_proc_2theta_range_min        5.0000
_pd_proc_2theta_range_max        50.0000
_pd_proc_2theta_range_inc        0.0150
_pd_proc_wavelength              ?


# Each refinement must be accompanied by a listing of the powder data
# in CIF format. Each listing should be sent as a separate file consisting
# of one data block containing a single powder profile. The value of
# _pd_block_diffractogram_id is used to associate each refinement with
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. A template
# for supplying powder data in CIF format is available by ftp at
# ftp://ftp.iucr.org/pub/rietdataform.cif and an example is given
# at ftp://ftp.iucr.org/pub/rietdataxmpl.cif.

_pd_block_diffractogram_id       ?

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       ?
_computing_cell_refinement       'RIETAN-FP (Izumi and Momma, 2007)'
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics    'VESTA (Momma and Izumi, 2008)'
_computing_publication_material  ?

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_type_symbol
C1 0.530(3) 0.564(5) 0.7753(17) 1 8 d Uiso 0.01615 C
C2 0.722(3) 0.937(6) 0.812(3) 1 8 d Uiso 0.01615 C
C3 0.255(4) 0.25 0.531(3) 1 4 c Uiso 0.01615 C
C4 0.224(4) 0.25 0.452(4) 1 4 c Uiso 0.01615 C
C5 0.122(4) 0.25 0.430(3) 1 4 c Uiso 0.01615 C
C6 0.288(5) 0.25 0.392(4) 1 4 c Uiso 0.01615 C
C7 0.381(5) 0.25 0.412(3) 1 4 c Uiso 0.01615 C
C8 0.408(4) 0.25 0.493(4) 1 4 c Uiso 0.01615 C
C9 0.507(4) 0.25 0.519(4) 1 4 c Uiso 0.01615 C
C10 0.579(5) 0.25 0.465(3) 1 4 c Uiso 0.01615 C
C11 0.670(4) 0.25 0.491(3) 1 4 c Uiso 0.01615 C
C12 0.692(4) 0.25 0.569(4) 1 4 c Uiso 0.01615 C
C13 0.791(4) 0.25 0.600(4) 1 4 c Uiso 0.01615 C
C14 0.617(5) 0.25 0.6235(22) 1 4 c Uiso 0.01615 C
Mn1 0.3975(9) 0.25 0.6777(9) 1 4 c Uiso 0.03032 Mn
Cr1 0.6202(8) 0.75 0.8191(9) 1 4 c Uiso 0.04173 Cr
N4 0.346(4) 0.25 0.5525(24) 1 4 c Uiso 0.01615 N
N1 0.478(3) 0.463(5) 0.7441(18) 1 8 d Uiso 0.01615 N
N5 0.525(3) 0.25 0.597(3) 1 4 c Uiso 0.01615 N
N2 0.780(3) 1.051(5) 0.806(3) 1 8 d Uiso 0.01615 N
N3 0.603(3) 0.75 0.906(16) 1 4 c Uiso 0.01615 N
H3 0.2099 0.25 0.57084 1 4 c Uiso 0.01938 H
H5C 0.11536 0.25 0.3744 0.5 4 c Uiso 0.01938 H
H5B 0.09231 0.35816 0.45174 0.5 8 d Uiso 0.01938 H
H5A 0.0922 0.14179 0.45447 0.5 8 d Uiso 0.01938 H
H6 0.26929 0.25 0.33979 1 4 c Uiso 0.01938 H
H7 0.4262 0.25 0.37283 1 4 c Uiso 0.01938 H
H10 0.5658 0.25 0.41079 1 4 c Uiso 0.01938 H
H13B 0.82314 0.35816 0.58164 0.5 8 d Uiso 0.01938 H
H13C 0.79005 0.25 0.65635 0.5 4 c Uiso 0.01938 H
H14 0.62887 0.25 0.67698 1 4 c Uiso 0.01938 H
H13A 0.82318 0.14179 0.58168 0.5 8 d Uiso 0.01938 H
H11 0.71796 0.25 0.45374 1 4 c Uiso 0.01938 H

#===============================================================================

#10. GEOMETRICAL PARAMETERS

_geom_special_details            ?

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C3 C4 1.43(6) . 1_555 ?
C4 C6 1.38(8) . 1_555 ?
C4 C5 1.50(6) . 1_555 ?
C5 H5C 0.96(5) . 1_555 ?
C6 C7 1.37(8) . 1_555 ?
C7 C8 1.43(5) . 1_555 ?
C8 C9 1.49(7) . 1_555 ?
C9 N5 1.35(5) . 1_555 ?
C9 C10 1.39(6) . 1_555 ?
C10 C11 1.38(6) . 1_555 ?
C11 H11 0.93(5) . 1_555 ?
C11 C12 1.38(7) . 1_555 ?
C12 C14 1.43(5) . 1_555 ?
C12 C13 1.50(7) . 1_555 ?
Mn1 N1 2.23(4) . 1_555 ?
Mn1 N1 2.23(4) . 7_555 ?
Mn1 N2 2.23(4) . 4_466 ?
Mn1 N2 2.23(4) . 6_446 ?
Mn1 N4 2.26(4) . 1_555 ?
Mn1 N5 2.29(4) . 1_555 ?
Cr1 N3 1.50(3) . 1_555 ?
Cr1 C2 1.99(5) . 1_555 ?
Cr1 C2 1.99(5) . 7_565 ?
Cr1 C1 2.01(4) . 1_555 ?
Cr1 C1 2.01(4) . 7_565 ?
N4 C8 1.35(6) . 1_555 ?
N4 C3 1.35(6) . 1_555 ?
N1 C1 1.17(3) . 1_555 ?
N5 C9 1.35(5) . 1_555 ?
N5 C14 1.38(6) . 1_555 ?
N2 C2 1.175(24) . 1_555 ?
N3 Cr1 1.50(3) . 1_555 ?

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 Cr1 175(3) 1_555 . 1_555 ?
N2 C2 Cr1 178(4) 1_555 . 1_555 ?
N4 C3 C4 124(5) 1_555 . 1_555 ?
C6 C4 C5 118(6) 1_555 . 1_555 ?
C3 C4 C5 122(6) 1_555 . 1_555 ?
C7 C6 C4 118(6) 1_555 . 1_555 ?
C6 C7 C8 120(6) 1_555 . 1_555 ?
N4 C8 C7 123(6) 1_555 . 1_555 ?
N4 C8 C9 113(6) 1_555 . 1_555 ?
C7 C8 C9 124(8) 1_555 . 1_555 ?
N5 C9 C10 121(5) 1_555 . 1_555 ?
N5 C9 C8 119(8) 1_555 . 1_555 ?
C10 C9 C8 120(7) 1_555 . 1_555 ?
C11 C10 C9 119(6) 1_555 . 1_555 ?
C10 C11 C12 122(6) 1_555 . 1_555 ?
C11 C12 C14 117(5) 1_555 . 1_555 ?
C11 C12 C13 124(7) 1_555 . 1_555 ?
C14 C12 C13 119(7) 1_555 . 1_555 ?
C13 C12 H11 100(5) 1_555 . 1_555 ?
N5 C14 C12 121(4) 1_555 . 1_555 ?
N1 Mn1 N1 87.4(17) 1_555 . 7_555 ?
N1 Mn1 N2 83.2(13) 1_555 . 4_466 ?
N1 Mn1 N2 140.6(16) 1_555 . 6_446 ?
N1 Mn1 N4 130.3(10) 1_555 . 1_555 ?
N1 Mn1 N5 83.7(14) 1_555 . 1_555 ?
N1 Mn1 N2 140.6(16) 7_555 . 4_466 ?
N1 Mn1 N2 83.2(13) 7_555 . 6_446 ?
N1 Mn1 N4 130.3(10) 7_555 . 1_555 ?
N1 Mn1 N5 83.7(14) 7_555 . 1_555 ?
N2 Mn1 N2 80.3(20) 4_466 . 6_446 ?
N2 Mn1 N4 82.5(15) 4_466 . 1_555 ?
N2 Mn1 N5 132.6(13) 4_466 . 1_555 ?
N2 Mn1 N4 82.5(15) 6_446 . 1_555 ?
N2 Mn1 N5 132.6(13) 6_446 . 1_555 ?
N4 Mn1 N5 72.2(21) 1_555 . 1_555 ?
N3 Cr1 C2 100.5(21) 1_555 . 1_555 ?
N3 Cr1 C2 100.5(21) 1_555 . 7_565 ?
N3 Cr1 C1 105.2(16) 1_555 . 1_555 ?
N3 Cr1 C1 105.2(16) 1_555 . 7_565 ?
C2 Cr1 C2 85.7(24) 1_555 . 7_565 ?
C2 Cr1 C1 154.3(20) 1_555 . 1_555 ?
C2 Cr1 C1 89.5(14) 1_555 . 7_565 ?
C2 Cr1 C1 89.5(14) 7_565 . 1_555 ?
C2 Cr1 C1 154.3(20) 7_565 . 7_565 ?
C1 Cr1 C1 84.1(22) 1_555 . 7_565 ?
C8 N4 Mn1 120(4) 1_555 . 1_555 ?
C3 N4 Mn1 125(4) 1_555 . 1_555 ?
C1 N1 Mn1 172(4) 1_555 . 1_555 ?
C9 N5 Mn1 116(5) 1_555 . 1_555 ?
C14 N5 Mn1 124(4) 1_555 . 1_555 ?
C2 N2 Mn1 168(6) 1_555 . 4_566 ?
