# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_MnMoDMF
_audit_block_doi                 10.5517/ccdc.csd.cc21q98c
_database_code_depnum_ccdc_archive 'CCDC 1898262'
_audit_update_record             
;
2019-05-13 deposited with the CCDC.	2019-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H17 Mn2 Mo N8 O5'
_chemical_formula_weight         547.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   7.961(6)
_cell_length_b                   8.932(6)
_cell_length_c                   14.020(10)
_cell_angle_alpha                93.206(11)
_cell_angle_beta                 92.618(11)
_cell_angle_gamma                107.265(10)
_cell_volume                     948.5(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    153
_cell_measurement_reflns_used    905
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      22.17

_exptl_crystal_description       foliated
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_F_000             542
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    2.002
_shelx_estimated_absorpt_T_min   0.690
_shelx_estimated_absorpt_T_max   0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2538
_exptl_absorpt_correction_T_max  0.3334
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   'SADABS: Bruker, 2000'
_diffrn_ambient_temperature      153
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4486
_diffrn_reflns_av_unetI/netI     0.1121
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.458
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             3442
_reflns_number_gt                2291
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0764P)²+0.7414P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3442
_refine_ls_number_parameters     259
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0633
_refine_ls_wR_factor_ref         0.1723
_refine_ls_wR_factor_gt          0.1504
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.31030(10) 0.65196(9) 0.75977(6) 0.0176(2) Uani 1 1 d . . . . .
Mn2 Mn -0.31343(18) 0.25104(16) 0.85463(11) 0.0231(4) Uani 1 1 d . . . . .
Mn1 Mn 0.84493(19) 0.81924(17) 0.52400(11) 0.0249(4) Uani 1 1 d . . . . .
O1 O 0.9406(9) 1.0705(8) 0.5794(5) 0.0358(18) Uani 1 1 d . . . . .
H1A H 0.984638 1.079849 0.636753 0.043 Uiso 1 1 d R U . . .
H1B H 0.858287 1.112749 0.577253 0.043 Uiso 1 1 d R U . . .
O3 O -0.1650(9) 0.0809(8) 0.8839(6) 0.0359(18) Uani 1 1 d . . . . .
N8 N -0.1859(13) -0.1599(10) 0.9356(6) 0.037(2) Uani 1 1 d . . . . .
N2 N -0.0655(11) 0.4029(10) 0.8192(6) 0.029(2) Uani 1 1 d . . . . .
N1 N 0.6238(11) 0.7657(11) 0.6127(7) 0.037(2) Uani 1 1 d . . . . .
O2 O 0.6764(10) 0.9197(10) 0.4168(7) 0.060(3) Uani 1 1 d . . . . .
H2A H 0.736275 1.013062 0.404246 0.090 Uiso 1 1 d R U . . .
H2B H 0.586420 0.933066 0.443876 0.090 Uiso 1 1 d R U . . .
N7 N 0.0386(11) 0.7702(10) 0.6192(6) 0.035(2) Uani 1 1 d . . . . .
C1 C 0.5240(13) 0.7308(11) 0.6675(7) 0.025(2) Uani 1 1 d . . . . .
C2 C 0.0699(12) 0.4916(11) 0.8005(7) 0.020(2) Uani 1 1 d . . . . .
N4 N 0.4786(13) 1.0322(9) 0.8099(7) 0.040(2) Uani 1 1 d . . . . .
C4 C 0.4125(15) 0.8991(11) 0.7936(7) 0.033(3) Uani 1 1 d . . . . .
C7 C 0.1360(12) 0.7370(10) 0.6709(7) 0.022(2) Uani 1 1 d . . . . .
C8 C -0.2200(13) -0.0227(13) 0.9439(8) 0.036(3) Uani 1 1 d D . . . .
H8 H -0.280350 -0.024728 1.005120 0.054 Uiso 1 1 d DR U . . .
C10 C -0.2366(18) -0.2747(13) 1.0087(9) 0.054(4) Uani 1 1 d . . . . .
H10A H -0.208089 -0.221017 1.071344 0.081 Uiso 1 1 calc R U . . .
H10B H -0.173723 -0.350769 1.001692 0.081 Uiso 1 1 calc R U . . .
H10C H -0.361080 -0.326918 1.000811 0.081 Uiso 1 1 calc R U . . .
C9 C -0.0947(16) -0.2036(13) 0.8548(9) 0.046(3) Uani 1 1 d . . . . .
H9A H -0.152161 -0.189381 0.795755 0.069 Uiso 1 1 calc R U . . .
H9B H -0.098145 -0.311722 0.856650 0.069 Uiso 1 1 calc R U . . .
H9C H 0.025646 -0.138252 0.859120 0.069 Uiso 1 1 calc R U . . .
C5 C 0.4599(12) 0.4961(11) 0.8015(7) 0.023(2) Uani 1 1 d . . . . .
C3 C 0.3172(13) 0.6898(11) 0.9126(7) 0.024(2) Uani 1 1 d . . . . .
N5 N 0.5327(10) 0.4063(9) 0.8194(6) 0.0255(19) Uani 1 1 d . . . . .
N3 N 0.3219(11) 0.7122(9) 0.9939(7) 0.032(2) Uani 1 1 d . . . . .
C6 C 0.2399(12) 0.4748(12) 0.6378(7) 0.026(2) Uani 1 1 d . . . . .
N6 N 0.2121(11) 0.3815(10) 0.5770(7) 0.033(2) Uani 1 1 d . . . . .
O4 O 0.8898(11) 0.8645(10) 0.2478(5) 0.050(2) Uani 1 1 d G . . . .
H4A H 0.961492 0.902090 0.205856 0.075 Uiso 1 1 d R U . . .
H4C H 0.806561 0.905950 0.246056 0.075 Uiso 1 1 d R U . . .
C11 C -0.2783(17) 0.3601(16) 0.5973(12) 0.067(4) Uani 0.47(2) 1 d . . P A 1
H11A H -0.199261 0.436317 0.561350 0.100 Uiso 0.47(2) 1 d R U P A 1
H11B H -0.384061 0.390107 0.604912 0.100 Uiso 0.47(2) 1 d R U P A 1
H11C H -0.222511 0.359807 0.659742 0.100 Uiso 0.47(2) 1 d R U P A 1
C11B C -0.2783(17) 0.3601(16) 0.5973(12) 0.067(4) Uani 0.53(2) 1 d . . P A 2
H11D H -0.228551 0.340617 0.539092 0.100 Uiso 0.53(2) 1 d R U P A 2
H11E H -0.388091 0.381597 0.583501 0.100 Uiso 0.53(2) 1 d R U P A 2
H11F H -0.198051 0.451207 0.633182 0.100 Uiso 0.53(2) 1 d R U P A 2
O5B O -0.307(2) 0.2119(18) 0.6536(15) 0.067(7) Uani 0.53(2) 1 d . . P A 2
H5BB H -0.275114 0.240404 0.712518 0.080 Uiso 0.53(2) 1 d R U P A 2
O5A O -0.320(2) 0.210(2) 0.5498(13) 0.050(6) Uani 0.47(2) 1 d . . P A 1
H5AB H -0.302533 0.220892 0.481902 0.075 Uiso 0.47(2) 1 d R U P A 1


_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
Mo1 C4 2.131(10) . ?
Mo1 C2 2.146(10) . ?
Mo1 C3 2.146(10) . ?
Mo1 C7 2.151(10) . ?
Mo1 C1 2.158(10) . ?
Mo1 C5 2.171(10) . ?
Mo1 C6 2.197(11) . ?
Mn2 N2 2.135(9) . ?
Mn2 N3 2.138(9) 2_567 ?
Mn2 N5 2.167(7) 1_455 ?
Mn2 N4 2.191(9) 1_445 ?
Mn2 O3 2.228(6) . ?
Mn2 H5BB 2.0307 . ?
Mn1 N6 2.144(9) 2_666 ?
Mn1 N7 2.152(9) 1_655 ?
Mn1 N1 2.155(9) . ?
Mn1 O1 2.227(7) . ?
Mn1 O1 2.319(7) 2_776 ?
Mn1 O2 2.355(8) . ?
O1 H1A 0.8515 . ?
O1 H1B 0.8475 . ?
O3 C8 1.279(12) . ?
N8 C8 1.331(12) . ?
N8 C9 1.468(13) . ?
N8 C10 1.475(13) . ?
N2 C2 1.183(12) . ?
N1 C1 1.119(12) . ?
O2 H2A 0.8616 . ?
O2 H2B 0.8614 . ?
N7 C7 1.151(12) . ?
N4 C4 1.153(12) . ?
C8 H8 1.0016 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C5 N5 1.152(11) . ?
C3 N3 1.143(12) . ?
C6 N6 1.125(13) . ?
O4 H4A 0.8502 . ?
O4 H4C 0.8493 . ?
C11 O5A 1.40(2) . ?
C11 H11A 0.9629 . ?
C11 H11B 0.9649 . ?
C11 H11C 0.9641 . ?
C11B O5B 1.54(2) . ?
C11B H11D 0.9527 . ?
C11B H11E 0.9625 . ?
C11B H11F 0.9698 . ?
O5B H5BB 0.8557 . ?
O5A H5AB 0.9746 . ?

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
C4 Mo1 C2 128.7(4) . . ?
C4 Mo1 C3 73.0(4) . . ?
C2 Mo1 C3 75.0(4) . . ?
C4 Mo1 C7 78.8(4) . . ?
C2 Mo1 C7 83.7(3) . . ?
C3 Mo1 C7 119.7(3) . . ?
C4 Mo1 C1 75.0(4) . . ?
C2 Mo1 C1 154.0(4) . . ?
C3 Mo1 C1 127.9(4) . . ?
C7 Mo1 C1 92.3(3) . . ?
C4 Mo1 C5 120.6(4) . . ?
C2 Mo1 C5 91.5(3) . . ?
C3 Mo1 C5 80.2(3) . . ?
C7 Mo1 C5 157.0(4) . . ?
C1 Mo1 C5 82.1(3) . . ?
C4 Mo1 C6 141.9(4) . . ?
C2 Mo1 C6 77.7(3) . . ?
C3 Mo1 C6 145.1(4) . . ?
C7 Mo1 C6 77.8(4) . . ?
C1 Mo1 C6 76.4(4) . . ?
C5 Mo1 C6 79.2(4) . . ?
N2 Mn2 N3 105.9(3) . 2_567 ?
N2 Mn2 N5 96.4(3) . 1_455 ?
N3 Mn2 N5 95.0(3) 2_567 1_455 ?
N2 Mn2 N4 143.9(3) . 1_445 ?
N3 Mn2 N4 106.6(4) 2_567 1_445 ?
N5 Mn2 N4 95.8(3) 1_455 1_445 ?
N2 Mn2 O3 85.2(3) . . ?
N3 Mn2 O3 87.5(3) 2_567 . ?
N5 Mn2 O3 176.5(3) 1_455 . ?
N4 Mn2 O3 81.1(3) 1_445 . ?
N2 Mn2 H5BB 66.5 . . ?
N3 Mn2 H5BB 172.3 2_567 . ?
N5 Mn2 H5BB 85.2 1_455 . ?
N4 Mn2 H5BB 81.0 1_445 . ?
O3 Mn2 H5BB 92.6 . . ?
N6 Mn1 N7 100.2(3) 2_666 1_655 ?
N6 Mn1 N1 103.9(3) 2_666 . ?
N7 Mn1 N1 99.5(4) 1_655 . ?
N6 Mn1 O1 158.5(3) 2_666 . ?
N7 Mn1 O1 89.4(3) 1_655 . ?
N1 Mn1 O1 93.4(3) . . ?
N6 Mn1 O1 83.5(3) 2_666 2_776 ?
N7 Mn1 O1 90.9(3) 1_655 2_776 ?
N1 Mn1 O1 165.9(3) . 2_776 ?
O1 Mn1 O1 77.1(3) . 2_776 ?
N6 Mn1 O2 86.1(3) 2_666 . ?
N7 Mn1 O2 168.8(3) 1_655 . ?
N1 Mn1 O2 87.8(3) . . ?
O1 Mn1 O2 81.6(3) . . ?
O1 Mn1 O2 80.6(3) 2_776 . ?
Mn1 O1 Mn1 102.9(3) . 2_776 ?
Mn1 O1 H1A 111.0 . . ?
Mn1 O1 H1A 110.9 2_776 . ?
Mn1 O1 H1B 111.3 . . ?
Mn1 O1 H1B 111.2 2_776 . ?
H1A O1 H1B 109.3 . . ?
C8 O3 Mn2 119.8(6) . . ?
C8 N8 C9 122.1(9) . . ?
C8 N8 C10 121.0(10) . . ?
C9 N8 C10 116.8(9) . . ?
C2 N2 Mn2 177.6(7) . . ?
C1 N1 Mn1 170.1(9) . . ?
Mn1 O2 H2A 109.5 . . ?
Mn1 O2 H2B 110.2 . . ?
H2A O2 H2B 103.9 . . ?
C7 N7 Mn1 176.6(8) . 1_455 ?
N1 C1 Mo1 173.6(9) . . ?
N2 C2 Mo1 177.3(8) . . ?
C4 N4 Mn2 158.4(9) . 1_665 ?
N4 C4 Mo1 175.3(10) . . ?
N7 C7 Mo1 174.2(9) . . ?
O3 C8 N8 120.8(10) . . ?
O3 C8 H8 134.4 . . ?
N8 C8 H8 104.6 . . ?
N8 C10 H10A 109.5 . . ?
N8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N8 C9 H9A 109.5 . . ?
N8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N5 C5 Mo1 175.7(8) . . ?
N3 C3 Mo1 179.0(9) . . ?
C5 N5 Mn2 176.0(8) . 1_655 ?
C3 N3 Mn2 176.5(9) . 2_567 ?
N6 C6 Mo1 176.0(9) . . ?
C6 N6 Mn1 172.0(9) . 2_666 ?
H4A O4 H4C 109.5 . . ?
O5A C11 H11A 110.4 . . ?
O5A C11 H11B 110.0 . . ?
H11A C11 H11B 108.8 . . ?
O5A C11 H11C 110.0 . . ?
H11A C11 H11C 108.9 . . ?
H11B C11 H11C 108.7 . . ?
O5B C11B H11D 107.3 . . ?
O5B C11B H11E 110.8 . . ?
H11D C11B H11E 109.9 . . ?
O5B C11B H11F 111.1 . . ?
H11D C11B H11F 109.3 . . ?
H11E C11B H11F 108.5 . . ?
C11B O5B H5BB 108.7 . . ?
C11 O5A H5AB 109.2 . . ?

_refine_diff_density_max         1.178
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.181

####################################################################### 
# 
# 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_MnMoDEF
_audit_block_doi                 10.5517/ccdc.csd.cc21q99d
_database_code_depnum_ccdc_archive 'CCDC 1898263'
_audit_update_record             
;
2019-05-13 deposited with the CCDC.	2019-05-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H13 Mn2 Mo N8 O2'
_chemical_formula_weight         507.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.0369(19)
_cell_length_b                   16.263(4)
_cell_length_c                   13.159(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.805(3)
_cell_angle_gamma                90
_cell_volume                     1885.8(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    153
_cell_measurement_reflns_used    8902
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      31.39

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_F_000             996
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.996
_shelx_estimated_absorpt_T_min   0.635
_shelx_estimated_absorpt_T_max   0.754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2039
_exptl_absorpt_correction_T_max  0.3383
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      153
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20815
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.022
_diffrn_reflns_theta_max         31.572
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             5841
_reflns_number_gt                5200
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0303P)²+1.1056P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5841
_refine_ls_number_parameters     229
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0711
_refine_ls_wR_factor_gt          0.0690
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.65759(2) 0.13988(2) 0.27838(2) 0.01533(5) Uani 1 1 d . . . . .
Mn2 Mn 0.22978(3) 0.13577(2) 0.49731(2) 0.01963(7) Uani 1 1 d . . . . .
Mn1 Mn 0.85338(3) -0.07398(2) 0.01229(2) 0.01857(7) Uani 1 1 d . . . . .
N2 N 0.3954(3) 0.13993(14) 0.41304(18) 0.0422(5) Uani 1 1 d . . . . .
N8 N 0.7509(2) 0.09498(15) -0.22445(16) 0.0424(5) Uani 1 1 d . . . . .
O1 O 0.90434(16) 0.03384(10) -0.08573(11) 0.0309(3) Uani 1 1 d . . . . .
C2 C 0.4898(3) 0.13907(14) 0.36676(18) 0.0302(4) Uani 1 1 d . . . . .
C1 C 0.7404(2) 0.05601(13) 0.17414(15) 0.0227(4) Uani 1 1 d . . . . .
N1 N 0.7812(2) 0.01368(12) 0.11614(14) 0.0301(4) Uani 1 1 d . . . . .
C6 C 0.4550(2) 0.11423(14) 0.16408(15) 0.0263(4) Uani 1 1 d . . . . .
C8 C 0.8515(3) 0.04027(17) -0.18218(18) 0.0373(5) Uani 1 1 d D . . . .
H8 H 0.876513 0.006136 -0.239159 0.046(8) Uiso 1 1 d DR . . . .
C5 C 0.7053(2) 0.22317(13) 0.16185(15) 0.0252(4) Uani 1 1 d . . . . .
C3 C 0.6900(2) 0.02789(14) 0.36495(16) 0.0280(4) Uani 1 1 d . . . . .
C7 C 0.6507(2) 0.25839(14) 0.34775(16) 0.0279(4) Uani 1 1 d . . . . .
C9 C 0.7067(4) 0.1014(2) -0.3389(2) 0.0656(10) Uani 1 1 d . . . . .
H9A H 0.599970 0.115547 -0.359542 0.079 Uiso 1 1 calc R U . . .
H9B H 0.720844 0.048518 -0.369506 0.079 Uiso 1 1 calc R U . . .
C4 C 0.8939(2) 0.14603(13) 0.35600(17) 0.0281(4) Uani 1 1 d . . . . .
N3 N 0.7195(3) -0.03114(13) 0.41400(17) 0.0401(5) Uani 1 1 d . . . . .
C11 C 0.6901(4) 0.1549(2) -0.1589(3) 0.0590(8) Uani 1 1 d . . . . .
H11A H 0.679307 0.208204 -0.192776 0.071 Uiso 1 1 calc R U . . .
H11B H 0.761169 0.160606 -0.092234 0.071 Uiso 1 1 calc R U . . .
C12 C 0.5365(5) 0.1274(3) -0.1410(4) 0.0887(14) Uani 1 1 d . . . . .
H12A H 0.465263 0.123083 -0.206737 0.133 Uiso 1 1 calc R U . . .
H12B H 0.500527 0.166937 -0.097937 0.133 Uiso 1 1 calc R U . . .
H12C H 0.547098 0.074817 -0.106922 0.133 Uiso 1 1 calc R U . . .
N5 N 0.7334(2) 0.26725(13) 0.10016(15) 0.0362(4) Uani 1 1 d . . . . .
N4 N 1.0197(2) 0.14257(13) 0.39756(18) 0.0410(5) Uani 1 1 d . . . . .
N6 N 0.3489(2) 0.09840(14) 0.10042(15) 0.0357(4) Uani 1 1 d . . . . .
N7 N 0.6449(2) 0.32184(13) 0.38696(17) 0.0388(5) Uani 1 1 d . . . . .
C10 C 0.7987(6) 0.1652(3) -0.3796(3) 0.1024(17) Uani 1 1 d . . . . .
H10A H 0.792489 0.216476 -0.344547 0.154 Uiso 1 1 calc R U . . .
H10B H 0.759704 0.172258 -0.453098 0.154 Uiso 1 1 calc R U . . .
H10C H 0.902627 0.147809 -0.367162 0.154 Uiso 1 1 calc R U . . .
O2 O 0.9733(3) -0.15168(14) -0.0877(2) 0.0583(6) Uani 1 1 d . . . . .
H2A H 0.994731 -0.113421 -0.126052 0.070 Uiso 1 1 d R U . . .
H2B H 1.063121 -0.167881 -0.061702 0.070 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C2 2.105(2) . ?
Mo1 C3 2.134(2) . ?
Mo1 C6 2.137(2) . ?
Mo1 C7 2.139(2) . ?
Mo1 C4 2.155(2) . ?
Mo1 C5 2.160(2) . ?
Mo1 C1 2.181(2) . ?
Mn2 N2 2.052(2) . ?
Mn2 N3 2.057(2) 3_656 ?
Mn2 N4 2.0578(19) 1_455 ?
Mn2 N5 2.0738(19) 4_566 ?
Mn1 N6 2.1208(18) 3_655 ?
Mn1 N7 2.149(2) 2_645 ?
Mn1 N1 2.1726(18) . ?
Mn1 O2 2.2659(19) . ?
Mn1 O1 2.2834(16) . ?
Mn1 O1 2.2838(15) 3_755 ?
N2 C2 1.153(3) . ?
N8 C8 1.305(3) . ?
N8 C9 1.474(3) . ?
N8 C11 1.486(4) . ?
O1 C8 1.257(3) . ?
C1 N1 1.148(3) . ?
C6 N6 1.153(3) . ?
C5 N5 1.153(3) . ?
C3 N3 1.155(3) . ?
C7 N7 1.160(3) . ?
C9 C10 1.501(5) . ?
C4 N4 1.149(3) . ?
C11 C12 1.525(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Mo1 C3 74.35(8) . . ?
C2 Mo1 C6 77.17(9) . . ?
C3 Mo1 C6 101.77(8) . . ?
C2 Mo1 C7 71.18(8) . . ?
C3 Mo1 C7 123.69(9) . . ?
C6 Mo1 C7 112.01(8) . . ?
C2 Mo1 C4 119.84(9) . . ?
C3 Mo1 C4 77.42(8) . . ?
C6 Mo1 C4 161.22(8) . . ?
C7 Mo1 C4 82.84(8) . . ?
C2 Mo1 C5 132.66(8) . . ?
C3 Mo1 C5 152.74(8) . . ?
C6 Mo1 C5 84.12(8) . . ?
C7 Mo1 C5 76.53(8) . . ?
C4 Mo1 C5 88.54(8) . . ?
C2 Mo1 C1 137.14(8) . . ?
C3 Mo1 C1 77.08(8) . . ?
C6 Mo1 C1 78.19(8) . . ?
C7 Mo1 C1 151.41(8) . . ?
C4 Mo1 C1 83.39(8) . . ?
C5 Mo1 C1 78.19(8) . . ?
N2 Mn2 N3 103.67(9) . 3_656 ?
N2 Mn2 N4 109.50(10) . 1_455 ?
N3 Mn2 N4 117.68(9) 3_656 1_455 ?
N2 Mn2 N5 114.81(9) . 4_566 ?
N3 Mn2 N5 106.83(9) 3_656 4_566 ?
N4 Mn2 N5 104.73(9) 1_455 4_566 ?
N6 Mn1 N7 99.85(9) 3_655 2_645 ?
N6 Mn1 N1 103.32(8) 3_655 . ?
N7 Mn1 N1 95.25(8) 2_645 . ?
N6 Mn1 O2 86.48(9) 3_655 . ?
N7 Mn1 O2 88.83(9) 2_645 . ?
N1 Mn1 O2 168.53(8) . . ?
N6 Mn1 O1 89.96(7) 3_655 . ?
N7 Mn1 O1 168.24(7) 2_645 . ?
N1 Mn1 O1 88.71(7) . . ?
O2 Mn1 O1 85.30(8) . . ?
N6 Mn1 O1 161.16(7) 3_655 3_755 ?
N7 Mn1 O1 95.11(7) 2_645 3_755 ?
N1 Mn1 O1 86.53(7) . 3_755 ?
O2 Mn1 O1 82.42(7) . 3_755 ?
O1 Mn1 O1 74.04(6) . 3_755 ?
C2 N2 Mn2 177.3(2) . . ?
C8 N8 C9 119.3(3) . . ?
C8 N8 C11 120.8(2) . . ?
C9 N8 C11 119.7(3) . . ?
C8 O1 Mn1 123.71(16) . . ?
C8 O1 Mn1 121.14(14) . 3_755 ?
Mn1 O1 Mn1 105.96(6) . 3_755 ?
N2 C2 Mo1 178.1(2) . . ?
N1 C1 Mo1 177.38(18) . . ?
C1 N1 Mn1 175.84(18) . . ?
N6 C6 Mo1 177.3(2) . . ?
O1 C8 N8 124.0(2) . . ?
N5 C5 Mo1 178.82(19) . . ?
N3 C3 Mo1 174.6(2) . . ?
N7 C7 Mo1 178.31(19) . . ?
N8 C9 C10 111.6(3) . . ?
N4 C4 Mo1 174.5(2) . . ?
C3 N3 Mn2 179.2(2) . 3_656 ?
N8 C11 C12 111.4(3) . . ?
C5 N5 Mn2 163.43(19) . 4_665 ?
C4 N4 Mn2 169.2(2) . 1_655 ?
C6 N6 Mn1 176.7(2) . 3_655 ?
C7 N7 Mn1 168.7(2) . 2_655 ?

_refine_diff_density_max         0.697
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.093

