# 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_1Re
_database_code_depnum_ccdc_archive 'CCDC 1899234'
loop_
_audit_author_name
_audit_author_address
'Michal Magott'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2019-06-17 deposited with the CCDC.	2019-06-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_1Re                 
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        8.3 Ratio
RESPONSE: These alerts regard elongated ellipsoids of non-bridging cyanide ligand, which can show increased mobility compared to the others. 
;
_vrf_PLAT306_1Re                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O2 Check
RESPONSE: Hydrogen atoms connected to crystallization water molecules cannot be clearly defined in this case.
;
_vrf_PLAT342_1Re                 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0254 Ang.
RESPONSE: Low bond precision is a result of a twin refinement.
;
_vrf_PLAT430_1Re                 
;
PROBLEM: Short Inter D...A Contact  O3       ..O4       .       2.76 Ang.
RESPONSE: Solvent molecules residing in the pores of the network are hard to describe accurately.
;
# Added during the CSD deposition process: Monday 17 June 2019 02:03 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H42 Mn4 N36 O7 Re2'
_chemical_formula_weight         1815.32

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   32.116(15)
_cell_length_b                   10.630(5)
_cell_length_c                   21.932(14)
_cell_angle_alpha                90
_cell_angle_beta                 113.96(2)
_cell_angle_gamma                90
_cell_volume                     6842(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    21164
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      26.79

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_F_000             3528
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    4.314
_shelx_estimated_absorpt_T_min   0.291
_shelx_estimated_absorpt_T_max   0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5400
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0789 before and 0.0491 after correction.
The Ratio of minimum to maximum transmission is 0.7244.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_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            33190
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.400
_diffrn_reflns_theta_max         26.707
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7281
_reflns_number_gt                6623
_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_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Refined as a 2-component twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+239.7896P] 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         7281
_refine_ls_number_parameters     449
_refine_ls_number_restraints     98
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1164
_refine_ls_wR_factor_gt          0.1106
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_restrained_S_all      1.238
_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
Re1 Re 0.64963(2) 0.71587(3) 0.24113(2) 0.01316(9) Uani 1 1 d . . . . .
O2 O 0.5094(5) 0.716(2) 0.0883(8) 0.217(13) Uani 1 1 d . . . . .
C1 C 0.7165(2) 0.7187(7) 0.2448(4) 0.0149(14) Uani 1 1 d . . . . .
N18 N 0.5000 0.3206(9) 0.2500 0.029(2) Uani 1 2 d S T P A .
Mn1 Mn 0.82096(4) 0.71672(11) 0.25534(6) 0.0176(2) Uani 1 1 d . . . . .
O4 O 1.0418(5) 0.6002(15) 0.4897(12) 0.183(10) Uani 1 1 d . . . . .
C2 C 0.6698(3) 0.5268(8) 0.2410(5) 0.026(2) Uani 1 1 d . . . . .
N1 N 0.7521(2) 0.7173(6) 0.2478(4) 0.0207(13) Uani 1 1 d . . . . .
Mn3 Mn 0.5000 0.52596(17) 0.2500 0.0238(4) Uani 1 2 d DS T P . .
O3 O 1.0483(8) 0.4194(18) 0.4035(9) 0.196(10) Uani 1 1 d . . . . .
C19 C 0.8477(5) 0.8221(17) 0.1429(7) 0.074(5) Uani 1 1 d . . . . .
H19 H 0.8481 0.9062 0.1577 0.089 Uiso 1 1 calc R U . . .
N7 N 0.8228(3) 0.5091(6) 0.2581(4) 0.0256(16) Uani 1 1 d . . . . .
Mn2 Mn 0.7500 0.7500 0.5000 0.0403(6) Uani 1 2 d S . P . .
C18 C 0.8536(7) 0.653(2) 0.0861(9) 0.098(6) Uani 1 1 d . U . . .
H18 H 0.8587 0.6014 0.0544 0.118 Uiso 1 1 calc R U . . .
N11 N 0.8258(8) 0.5088(17) 0.4169(10) 0.125(6) Uani 1 1 d . U . . .
H11 H 0.8301 0.4586 0.3880 0.150 Uiso 1 1 calc R U . . .
O1 O 0.5000 0.7354(10) 0.2500 0.050(3) Uani 1 2 d DS T P . .
H1 H 0.498(4) 0.792(4) 0.215(3) 0.060 Uiso 1 1 d D U . . .
C15 C 0.9410(5) 0.7950(17) 0.4359(7) 0.069(4) Uani 1 1 d . . . . .
H15 H 0.9592 0.8462 0.4726 0.083 Uiso 1 1 calc R U . . .
N15 N 0.8576(6) 0.785(2) 0.0927(9) 0.119(6) Uani 1 1 d . U . . .
H15A H 0.8654 0.8353 0.0672 0.143 Uiso 1 1 calc R U . . .
C5 C 0.6217(3) 0.7194(10) 0.1368(5) 0.034(2) Uani 1 1 d . . . . .
N6 N 0.6920(4) 0.7121(12) 0.4020(4) 0.066(4) Uani 1 1 d . . . . .
N17 N 0.5789(3) 0.4541(10) 0.4655(5) 0.050(2) Uani 1 1 d . . . . .
H17 H 0.5842 0.4098 0.5019 0.059 Uiso 1 1 calc R U . . .
N19 N 0.4750(7) 0.1260(19) 0.2432(11) 0.031(5) Uani 0.5 1 d . U P A 1
C24 C 0.5127(11) 0.124(3) 0.2314(15) 0.043(7) Uani 0.5 1 d . U P A 1
C20 C 0.5848(4) 0.5905(11) 0.3948(6) 0.043(3) Uani 1 1 d . . . . .
H20 H 0.5962 0.6553 0.3759 0.051 Uiso 1 1 calc R U . . .
C9 C 0.7246(4) 0.5886(12) 0.6038(5) 0.047(3) Uani 1 1 d . . . . .
H9 H 0.7266 0.6631 0.6287 0.057 Uiso 1 1 calc R U . . .
C6 C 0.6764(4) 0.7121(11) 0.3448(4) 0.039(3) Uani 1 1 d . . . . .
C16 C 0.9149(4) 0.6361(13) 0.3679(6) 0.053(3) Uani 1 1 d . . . . .
H16 H 0.9131 0.5546 0.3492 0.063 Uiso 1 1 calc R U . . .
C21 C 0.6048(4) 0.5508(12) 0.4585(6) 0.052(3) Uani 1 1 d . . . . .
H21 H 0.6319 0.5836 0.4923 0.062 Uiso 1 1 calc R U . . .
C14 C 0.9012(4) 0.8257(13) 0.3864(6) 0.053(3) Uani 1 1 d . . . . .
H14 H 0.8870 0.9055 0.3814 0.064 Uiso 1 1 calc R U . . .
C22 C 0.5434(4) 0.4402(11) 0.4057(6) 0.045(3) Uani 1 1 d . . . . .
H22 H 0.5201 0.3790 0.3965 0.054 Uiso 1 1 calc R U . . .
C4 C 0.5997(4) 0.8293(12) 0.2478(9) 0.070(4) Uani 1 1 d . U . . .
N13 N 0.9498(4) 0.6786(15) 0.4233(6) 0.076(4) Uani 1 1 d . . . . .
H13 H 0.9745 0.6355 0.4472 0.091 Uiso 1 1 calc R U . . .
C17 C 0.8410(5) 0.6167(17) 0.1343(7) 0.070(4) Uani 1 1 d . . . . .
H17A H 0.8357 0.5319 0.1430 0.084 Uiso 1 1 calc R U . . .
C13 C 0.8605(10) 0.559(2) 0.4752(15) 0.124(7) Uani 1 1 d . U . . .
H13A H 0.8925 0.5445 0.4923 0.148 Uiso 1 1 calc R U . . .
C8 C 0.7257(4) 0.4596(11) 0.5298(6) 0.050(3) Uani 1 1 d . . . . .
H8 H 0.7283 0.4260 0.4913 0.060 Uiso 1 1 calc R U . . .
C11 C 0.7827(8) 0.5531(15) 0.4125(9) 0.090(5) Uani 1 1 d . U . . .
H11A H 0.7534 0.5342 0.3791 0.108 Uiso 1 1 calc R U . . .
C12 C 0.8383(9) 0.6263(19) 0.4985(13) 0.106(6) Uani 1 1 d . U . . .
H12 H 0.8535 0.6745 0.5378 0.127 Uiso 1 1 calc R U . . .
N16 N 0.5452(3) 0.5233(8) 0.3608(5) 0.037(2) Uani 1 1 d . . . . .
N4 N 0.5714(5) 0.8910(14) 0.2565(12) 0.130(6) Uani 1 1 d . U . . .
N2 N 0.6805(3) 0.4239(7) 0.2438(6) 0.041(2) Uani 1 1 d . . . . .
N9 N 0.7153(3) 0.4747(11) 0.6208(5) 0.053(3) Uani 1 1 d . . . . .
H9A H 0.7095 0.4571 0.6557 0.064 Uiso 1 1 calc R U . . .
C7 C 0.8317(3) 0.4045(8) 0.2579(4) 0.0196(16) Uani 1 1 d . . . . .
C3 C 0.5940(2) 0.6015(7) 0.2341(4) 0.0177(16) Uani 1 1 d . . . . .
N12 N 0.8838(3) 0.7254(8) 0.3436(4) 0.0327(17) Uani 1 1 d . . . . .
C23 C 0.4673(3) 0.2452(9) 0.2535(6) 0.039(2) Uani 1 1 d . . . . .
N10 N 0.7931(5) 0.6290(11) 0.4672(6) 0.066(3) Uani 1 1 d . U . . .
N5 N 0.6050(4) 0.7200(14) 0.0783(5) 0.068(3) Uani 1 1 d . . . . .
C10 C 0.7165(4) 0.3921(13) 0.5755(8) 0.060(4) Uani 1 1 d . . . . .
H10 H 0.7117 0.3038 0.5752 0.072 Uiso 1 1 calc R U . . .
N8 N 0.7308(3) 0.5843(9) 0.5481(4) 0.039(2) Uani 1 1 d . . . . .
N14 N 0.8368(3) 0.7175(9) 0.1694(4) 0.0381(19) Uani 1 1 d . . . . .
N3 N 0.5625(3) 0.5464(7) 0.2283(4) 0.0283(17) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C4 2.059(11) . ?
Re1 C6 2.079(9) . ?
Re1 C7 2.090(8) 4_655 ?
Re1 C5 2.091(9) . ?
Re1 C2 2.112(8) . ?
Re1 C3 2.114(7) . ?
Re1 C1 2.115(7) . ?
C1 N1 1.119(9) . ?
N18 C23 1.348(11) . ?
N18 C23 1.348(11) 2_655 ?
N18 Mn3 2.183(10) . ?
Mn1 N14 2.144(8) . ?
Mn1 N1 2.151(6) . ?
Mn1 N12 2.158(8) . ?
Mn1 N2 2.203(8) 4_655 ?
Mn1 N7 2.207(7) . ?
C2 N2 1.141(11) . ?
Mn3 O1 2.226(11) . ?
Mn3 N3 2.253(7) 2_655 ?
Mn3 N3 2.253(7) . ?
Mn3 N16 2.269(9) 2_655 ?
Mn3 N16 2.269(9) . ?
C19 N15 1.32(2) . ?
C19 N14 1.364(15) . ?
C19 H19 0.9500 . ?
N7 C7 1.150(11) . ?
Mn2 N10 2.214(12) . ?
Mn2 N10 2.214(12) 7_666 ?
Mn2 N6 2.236(10) . ?
Mn2 N6 2.236(10) 7_666 ?
Mn2 N8 2.264(8) 7_666 ?
Mn2 N8 2.264(8) . ?
C18 C17 1.33(2) . ?
C18 N15 1.41(3) . ?
C18 H18 0.9500 . ?
N11 C13 1.41(3) . ?
N11 C11 1.43(3) . ?
N11 H11 0.8800 . ?
O1 H1 0.95(2) . ?
C15 N13 1.32(2) . ?
C15 C14 1.337(18) . ?
C15 H15 0.9500 . ?
N15 H15A 0.8800 . ?
C5 N5 1.174(13) . ?
N6 C6 1.145(12) . ?
N17 C22 1.351(14) . ?
N17 C21 1.371(16) . ?
N17 H17 0.8800 . ?
N19 C24 0.54(3) 2_655 ?
N19 C23 1.33(2) . ?
N19 C24 1.34(3) . ?
N19 N19 1.51(4) 2_655 ?
C24 N19 0.54(3) 2_655 ?
C24 C24 1.37(6) 2_655 ?
C24 C23 1.42(3) 2_655 ?
C20 C21 1.347(17) . ?
C20 N16 1.381(13) . ?
C20 H20 0.9500 . ?
C9 N8 1.316(13) . ?
C9 N9 1.336(15) . ?
C9 H9 0.9500 . ?
C16 N12 1.322(15) . ?
C16 N13 1.353(16) . ?
C16 H16 0.9500 . ?
C21 H21 0.9500 . ?
C14 N12 1.380(14) . ?
C14 H14 0.9500 . ?
C22 N16 1.341(14) . ?
C22 H22 0.9500 . ?
C4 N4 1.196(16) . ?
N13 H13 0.8800 . ?
C17 N14 1.357(17) . ?
C17 H17A 0.9500 . ?
C13 C12 1.26(3) . ?
C13 H13A 0.9500 . ?
C8 C10 1.360(16) . ?
C8 N8 1.375(15) . ?
C8 H8 0.9500 . ?
C11 N10 1.37(2) . ?
C11 H11A 0.9500 . ?
C12 N10 1.33(3) . ?
C12 H12 0.9500 . ?
N2 Mn1 2.203(8) 4_645 ?
N9 C10 1.339(18) . ?
N9 H9A 0.8800 . ?
C7 Re1 2.090(8) 4_645 ?
C3 N3 1.131(10) . ?
C23 C24 1.42(3) 2_655 ?
C10 H10 0.9500 . ?

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 Re1 C6 85.5(6) . . ?
C4 Re1 C7 70.5(4) . 4_655 ?
C6 Re1 C7 91.0(4) . 4_655 ?
C4 Re1 C5 93.9(6) . . ?
C6 Re1 C5 179.2(4) . . ?
C7 Re1 C5 89.3(4) 4_655 . ?
C4 Re1 C2 143.6(4) . . ?
C6 Re1 C2 89.5(4) . . ?
C7 Re1 C2 145.7(3) 4_655 . ?
C5 Re1 C2 90.7(4) . . ?
C4 Re1 C3 71.5(4) . . ?
C6 Re1 C3 91.8(3) . . ?
C7 Re1 C3 141.5(3) 4_655 . ?
C5 Re1 C3 87.5(3) . . ?
C2 Re1 C3 72.7(3) . . ?
C4 Re1 C1 142.8(4) . . ?
C6 Re1 C1 89.7(3) . . ?
C7 Re1 C1 72.8(3) 4_655 . ?
C5 Re1 C1 91.1(3) . . ?
C2 Re1 C1 72.9(3) . . ?
C3 Re1 C1 145.6(3) . . ?
N1 C1 Re1 178.1(7) . . ?
C23 N18 C23 107.1(11) . 2_655 ?
C23 N18 Mn3 126.5(5) . . ?
C23 N18 Mn3 126.5(5) 2_655 . ?
N14 Mn1 N1 122.5(3) . . ?
N14 Mn1 N12 108.6(3) . . ?
N1 Mn1 N12 128.8(3) . . ?
N14 Mn1 N2 91.0(4) . 4_655 ?
N1 Mn1 N2 88.5(3) . 4_655 ?
N12 Mn1 N2 88.0(3) . 4_655 ?
N14 Mn1 N7 90.9(3) . . ?
N1 Mn1 N7 91.1(3) . . ?
N12 Mn1 N7 90.7(3) . . ?
N2 Mn1 N7 178.0(3) 4_655 . ?
N2 C2 Re1 176.7(9) . . ?
C1 N1 Mn1 178.9(7) . . ?
N18 Mn3 O1 180.0 . . ?
N18 Mn3 N3 95.54(19) . 2_655 ?
O1 Mn3 N3 84.46(19) . 2_655 ?
N18 Mn3 N3 95.54(19) . . ?
O1 Mn3 N3 84.46(19) . . ?
N3 Mn3 N3 168.9(4) 2_655 . ?
N18 Mn3 N16 89.3(2) . 2_655 ?
O1 Mn3 N16 90.7(2) . 2_655 ?
N3 Mn3 N16 89.4(3) 2_655 2_655 ?
N3 Mn3 N16 90.7(3) . 2_655 ?
N18 Mn3 N16 89.3(2) . . ?
O1 Mn3 N16 90.7(2) . . ?
N3 Mn3 N16 90.7(3) 2_655 . ?
N3 Mn3 N16 89.4(3) . . ?
N16 Mn3 N16 178.6(5) 2_655 . ?
N15 C19 N14 107.5(17) . . ?
N15 C19 H19 126.2 . . ?
N14 C19 H19 126.2 . . ?
C7 N7 Mn1 166.2(7) . . ?
N10 Mn2 N10 180.0(5) . 7_666 ?
N10 Mn2 N6 88.2(5) . . ?
N10 Mn2 N6 91.8(5) 7_666 . ?
N10 Mn2 N6 91.8(5) . 7_666 ?
N10 Mn2 N6 88.2(5) 7_666 7_666 ?
N6 Mn2 N6 180.0 . 7_666 ?
N10 Mn2 N8 88.6(4) . 7_666 ?
N10 Mn2 N8 91.4(4) 7_666 7_666 ?
N6 Mn2 N8 88.3(3) . 7_666 ?
N6 Mn2 N8 91.7(3) 7_666 7_666 ?
N10 Mn2 N8 91.4(4) . . ?
N10 Mn2 N8 88.6(4) 7_666 . ?
N6 Mn2 N8 91.7(3) . . ?
N6 Mn2 N8 88.3(3) 7_666 . ?
N8 Mn2 N8 180.0(5) 7_666 . ?
C17 C18 N15 104.5(16) . . ?
C17 C18 H18 127.8 . . ?
N15 C18 H18 127.8 . . ?
C13 N11 C11 109.0(18) . . ?
C13 N11 H11 125.5 . . ?
C11 N11 H11 125.5 . . ?
Mn3 O1 H1 129(4) . . ?
N13 C15 C14 105.9(12) . . ?
N13 C15 H15 127.1 . . ?
C14 C15 H15 127.1 . . ?
C19 N15 C18 109.8(16) . . ?
C19 N15 H15A 125.1 . . ?
C18 N15 H15A 125.1 . . ?
N5 C5 Re1 178.2(9) . . ?
C6 N6 Mn2 151.1(8) . . ?
C22 N17 C21 106.4(11) . . ?
C22 N17 H17 126.8 . . ?
C21 N17 H17 126.8 . . ?
C24 N19 C23 88(5) 2_655 . ?
C24 N19 C24 82(5) 2_655 . ?
C23 N19 C24 107(2) . . ?
C24 N19 N19 61(5) 2_655 2_655 ?
C23 N19 N19 102.9(11) . 2_655 ?
C24 N19 N19 20.6(14) . 2_655 ?
N19 C24 N19 98(5) 2_655 . ?
N19 C24 C24 75(5) 2_655 2_655 ?
N19 C24 C24 22.8(14) . 2_655 ?
N19 C24 C23 70(5) 2_655 2_655 ?
N19 C24 C23 108(3) . 2_655 ?
C24 C24 C23 100.7(16) 2_655 2_655 ?
C21 C20 N16 110.2(11) . . ?
C21 C20 H20 124.9 . . ?
N16 C20 H20 124.9 . . ?
N8 C9 N9 111.3(11) . . ?
N8 C9 H9 124.4 . . ?
N9 C9 H9 124.4 . . ?
N6 C6 Re1 178.3(9) . . ?
N12 C16 N13 109.7(12) . . ?
N12 C16 H16 125.2 . . ?
N13 C16 H16 125.2 . . ?
C20 C21 N17 107.2(10) . . ?
C20 C21 H21 126.4 . . ?
N17 C21 H21 126.4 . . ?
C15 C14 N12 110.7(13) . . ?
C15 C14 H14 124.7 . . ?
N12 C14 H14 124.7 . . ?
N16 C22 N17 111.8(10) . . ?
N16 C22 H22 124.1 . . ?
N17 C22 H22 124.1 . . ?
N4 C4 Re1 174.9(18) . . ?
C15 N13 C16 109.3(12) . . ?
C15 N13 H13 125.4 . . ?
C16 N13 H13 125.4 . . ?
C18 C17 N14 110.7(17) . . ?
C18 C17 H17A 124.7 . . ?
N14 C17 H17A 124.7 . . ?
C12 C13 N11 102(3) . . ?
C12 C13 H13A 128.9 . . ?
N11 C13 H13A 128.9 . . ?
C10 C8 N8 109.2(12) . . ?
C10 C8 H8 125.4 . . ?
N8 C8 H8 125.4 . . ?
N10 C11 N11 104.5(19) . . ?
N10 C11 H11A 127.8 . . ?
N11 C11 H11A 127.8 . . ?
C13 C12 N10 119(3) . . ?
C13 C12 H12 120.6 . . ?
N10 C12 H12 120.6 . . ?
C22 N16 C20 104.4(10) . . ?
C22 N16 Mn3 126.5(7) . . ?
C20 N16 Mn3 128.3(8) . . ?
C2 N2 Mn1 162.2(7) . 4_645 ?
C9 N9 C10 108.1(10) . . ?
C9 N9 H9A 125.9 . . ?
C10 N9 H9A 125.9 . . ?
N7 C7 Re1 178.0(7) . 4_645 ?
N3 C3 Re1 175.6(7) . . ?
C16 N12 C14 104.4(10) . . ?
C16 N12 Mn1 127.5(8) . . ?
C14 N12 Mn1 128.0(8) . . ?
N19 C23 N18 110.7(12) . . ?
N19 C23 C24 22.2(12) . 2_655 ?
N18 C23 C24 105.3(15) . 2_655 ?
C12 N10 C11 105.5(17) . . ?
C12 N10 Mn2 122.7(14) . . ?
C11 N10 Mn2 131.7(13) . . ?
N9 C10 C8 106.3(11) . . ?
N9 C10 H10 126.9 . . ?
C8 C10 H10 126.9 . . ?
C9 N8 C8 105.1(9) . . ?
C9 N8 Mn2 125.3(8) . . ?
C8 N8 Mn2 129.5(7) . . ?
C17 N14 C19 107.6(11) . . ?
C17 N14 Mn1 127.5(9) . . ?
C19 N14 Mn1 124.8(10) . . ?
C3 N3 Mn3 149.3(7) . . ?

_refine_diff_density_max         3.288
_refine_diff_density_min         -1.926
_refine_diff_density_rms         0.189


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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1899236'
loop_
_audit_author_name
_audit_author_address
'Michal Magott'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2019-06-17 deposited with the CCDC.	2019-06-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT975_2                   
;
PROBLEM: Check Calcd Resid. Dens.  1.06A   From O4              2.43 eA-3
RESPONSE: Crystals of 2 are not stable in contact with oxygen, which deteriorates diffraction data and increases difficulties with disorder refinement.
;
_vrf_PLAT220_2                   
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        6.6 Ratio
RESPONSE: Crystals of 2 are not stable in contact with oxygen, which deteriorates diffraction data and increases difficulties with disorder refinement.
;
_vrf_PLAT306_2                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O5 Check
RESPONSE: Hydrogen atoms connected to crystallization water molecules cannot be clearly defined in this case.
;
_vrf_PLAT975_2_2                 
;
PROBLEM: Check Calcd Resid. Dens.  1.04A   From O7              1.69 eA-3
RESPONSE: Crystals of 2 are not stable in contact with oxygen, which deteriorates diffraction data and increases difficulties with disorder refinement.
;
# Added during the CSD deposition process: Monday 17 June 2019 02:34 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14.50 Mn2 Mo N12 O6'
_chemical_formula_weight         644.08

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'
Mo Mo -1.6832 0.6857 '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'

_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                   10.6308(7)
_cell_length_b                   10.8192(7)
_cell_length_c                   11.8287(8)
_cell_angle_alpha                70.190(3)
_cell_angle_beta                 77.920(3)
_cell_angle_gamma                88.094(3)
_cell_volume                     1250.59(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    11404
_cell_measurement_theta_min      2.98
_cell_measurement_theta_max      27.16

_exptl_crystal_description       column
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_F_000             622
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.541
_shelx_estimated_absorpt_T_min   0.728
_shelx_estimated_absorpt_T_max   0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6477
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0573 before and 0.0479 after correction.
The Ratio of minimum to maximum transmission is 0.8688.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_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            20013
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.745
_diffrn_reflns_theta_max         27.267
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5549
_reflns_number_gt                4928
_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_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0285P)²+13.5225P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5549
_refine_ls_number_parameters     388
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0551
_refine_ls_wR_factor_ref         0.1372
_refine_ls_wR_factor_gt          0.1331
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.131
_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 0.19489(4) 0.30502(4) 0.78565(4) 0.00925(12) Uani 1 1 d . . . . .
Mn2 Mn 0.17146(8) 0.80402(7) 0.78441(7) 0.01554(18) Uani 1 1 d . . . . .
Mn1 Mn 0.71490(8) 0.36494(10) 0.69348(8) 0.0235(2) Uani 1 1 d . . . . .
N2 N -0.0274(5) 0.2271(5) 1.0429(5) 0.0263(11) Uani 1 1 d . . . . .
N7 N 0.7505(5) 0.5088(5) 0.5085(4) 0.0243(11) Uani 1 1 d . . . . .
C4 C 0.1895(5) 0.1205(5) 0.7540(5) 0.0160(10) Uani 1 1 d . . . . .
N1 N 0.1973(5) 0.5935(5) 0.8235(5) 0.0264(11) Uani 1 1 d . . . . .
C2 C 0.0479(5) 0.2511(5) 0.9528(5) 0.0159(10) Uani 1 1 d . . . . .
O6 O 0.5138(5) 1.0024(5) 0.8230(5) 0.0410(12) Uani 1 1 d . . . . .
N3 N -0.0823(5) 0.3504(6) 0.6978(5) 0.0372(14) Uani 1 1 d . . . . .
N4 N 0.1810(5) 0.0183(5) 0.7451(5) 0.0267(11) Uani 1 1 d . . . . .
C3 C 0.0137(5) 0.3364(6) 0.7291(5) 0.0207(11) Uani 1 1 d . . . . .
C1 C 0.1967(5) 0.4910(5) 0.8139(5) 0.0184(11) Uani 1 1 d . . . . .
N8 N 0.0276(7) 0.8022(6) 0.6734(6) 0.0393(15) Uani 1 1 d . . . . .
C7 C 0.7685(5) 0.5766(5) 0.4074(5) 0.0170(10) Uani 1 1 d . . . . .
C6 C 0.3999(5) 0.3340(6) 0.7251(5) 0.0213(11) Uani 1 1 d . . . . .
N6 N 0.5100(5) 0.3494(6) 0.6974(5) 0.0354(14) Uani 1 1 d . . . . .
C5 C 0.2863(6) 0.1924(6) 0.9322(5) 0.0232(12) Uani 1 1 d . . . . .
N5 N 0.3378(6) 0.1292(6) 1.0070(5) 0.0384(14) Uani 1 1 d . . . . .
N13 N 0.6862(7) 0.4946(7) 0.8013(7) 0.0501(18) Uani 1 1 d . . . . .
C15 C 0.5774(19) 0.587(3) 0.942(2) 0.100(11) Uani 0.5 1 d . . P A 2
C16 C 0.5612(16) 0.519(3) 0.868(3) 0.107(12) Uani 0.5 1 d . . P A 2
O3 O 0.6876(8) 0.1943(7) 0.8825(6) 0.071(2) Uani 1 1 d . . . . .
O7 O 0.3400(8) 0.7940(7) 0.8803(9) 0.099(3) Uani 1 1 d . . . . .
C17 C 0.7590(9) 0.5160(9) 0.8689(9) 0.054(2) Uani 1 1 d . . . . .
N12 N 0.7197(13) 0.6027(10) 0.9192(11) 0.105(4) Uani 1 1 d . . . . .
C9A C -0.1084(16) 0.845(2) 0.700(2) 0.070(6) Uani 0.5 1 d . . P B 1
C10A C -0.176(2) 0.807(3) 0.632(3) 0.096(9) Uani 0.5 1 d . . P B 1
C9 C -0.067(2) 0.8684(17) 0.5132(18) 0.069(5) Uani 0.5 1 d D U P B 2
C10 C -0.002(3) 0.9079(18) 0.585(2) 0.090(9) Uani 0.5 1 d . . P B 2
C15A C 0.652(2) 0.6288(19) 0.7481(17) 0.065(6) Uani 0.5 1 d . . P A 1
C16A C 0.680(3) 0.704(2) 0.811(2) 0.082(7) Uani 0.5 1 d . . P A 1
O5 O 0.8776(8) 0.0462(9) 0.8424(15) 0.193(8) Uani 1 1 d . . . . .
N9 N -0.0727(11) 0.7349(11) 0.5589(10) 0.090(3) Uani 1 1 d D . . . .
C8 C 0.0138(9) 0.7194(11) 0.6194(11) 0.069(3) Uani 1 1 d . . . . .
C13 C 0.5200(11) 0.9419(11) 0.4944(11) 0.024(2) Uani 0.5 1 d . . P C 1
C11 C 0.4188(13) 0.9541(13) 0.5773(12) 0.031(3) Uani 0.5 1 d . . P C 1
C12 C 0.3994(16) 0.7598(15) 0.5702(15) 0.049(5) Uani 0.5 1 d . . P C 1
N11 N 0.5093(16) 0.8184(16) 0.4884(14) 0.063(5) Uani 0.5 1 d . . P C 1
N10 N 0.3504(18) 0.843(2) 0.6335(19) 0.047(5) Uani 0.5 1 d . U P C 1
O4 O 0.7280(6) 0.1702(7) 0.6468(9) 0.088(3) Uani 1 1 d . U . . .
O2 O 0.490(2) 0.6683(17) 0.5746(16) 0.108(7) Uani 0.5 1 d . . P D 2
O1 O 0.3104(14) 0.8319(14) 0.5986(13) 0.039(3) Uani 0.5 1 d . . P C 2


_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 C6 2.145(5) . ?
Mo1 C3 2.148(5) . ?
Mo1 C1 2.150(5) . ?
Mo1 C5 2.151(6) . ?
Mo1 C4 2.157(5) . ?
Mo1 C2 2.163(5) . ?
Mo1 C7 2.165(6) 2_666 ?
Mn2 N1 2.185(5) . ?
Mn2 N4 2.206(5) 1_565 ?
Mn2 N2 2.211(5) 2_567 ?
Mn2 N8 2.220(6) . ?
Mn2 N10 2.260(17) . ?
Mn2 O7 2.294(6) . ?
Mn2 O1 2.307(14) . ?
Mn1 N3 2.166(5) 1_655 ?
Mn1 N13 2.170(7) . ?
Mn1 N7 2.177(5) . ?
Mn1 N6 2.180(5) . ?
Mn1 O3 2.336(7) . ?
Mn1 O4 2.346(8) . ?
N2 C2 1.146(7) . ?
N2 Mn2 2.211(5) 2_567 ?
N7 C7 1.150(7) . ?
C4 N4 1.153(7) . ?
N1 C1 1.153(7) . ?
N3 C3 1.145(7) . ?
N3 Mn1 2.166(5) 1_455 ?
N4 Mn2 2.206(5) 1_545 ?
N8 C8 1.291(10) . ?
N8 C10 1.343(17) . ?
N8 C9A 1.505(18) . ?
C7 Mo1 2.165(6) 2_666 ?
C6 N6 1.149(7) . ?
C5 N5 1.148(8) . ?
N13 C17 1.299(10) . ?
N13 C15A 1.44(2) . ?
N13 C16 1.460(18) . ?
C15 C16 1.36(2) . ?
C15 N12 1.49(2) . ?
C17 N12 1.287(12) . ?
N12 C16A 1.50(3) . ?
C9A C10A 1.34(3) . ?
C10A N9 1.60(3) . ?
C9 N9 1.358(16) . ?
C9 C10 1.37(2) . ?
C9 C8 1.97(2) . ?
C10 C8 1.95(2) . ?
C15A C16A 1.35(3) . ?
N9 C8 1.253(13) . ?
C13 C11 1.256(17) 2_676 ?
C13 C11 1.331(17) . ?
C13 C13 1.35(2) 2_676 ?
C13 N11 1.371(18) . ?
C11 C13 1.256(17) 2_676 ?
C11 N10 1.32(2) . ?
C12 N11 1.365(19) . ?
C12 N10 1.38(2) . ?

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
C6 Mo1 C3 145.1(2) . . ?
C6 Mo1 C1 86.6(2) . . ?
C3 Mo1 C1 93.2(2) . . ?
C6 Mo1 C5 70.5(2) . . ?
C3 Mo1 C5 143.5(2) . . ?
C1 Mo1 C5 98.3(2) . . ?
C6 Mo1 C4 94.3(2) . . ?
C3 Mo1 C4 85.3(2) . . ?
C1 Mo1 C4 178.5(2) . . ?
C5 Mo1 C4 83.2(2) . . ?
C6 Mo1 C2 140.4(2) . . ?
C3 Mo1 C2 73.9(2) . . ?
C1 Mo1 C2 83.4(2) . . ?
C5 Mo1 C2 73.2(2) . . ?
C4 Mo1 C2 96.73(19) . . ?
C6 Mo1 C7 73.4(2) . 2_666 ?
C3 Mo1 C7 71.86(19) . 2_666 ?
C1 Mo1 C7 84.4(2) . 2_666 ?
C5 Mo1 C7 143.5(2) . 2_666 ?
C4 Mo1 C7 94.6(2) . 2_666 ?
C2 Mo1 C7 142.76(19) . 2_666 ?
N1 Mn2 N4 170.1(2) . 1_565 ?
N1 Mn2 N2 93.05(19) . 2_567 ?
N4 Mn2 N2 91.81(19) 1_565 2_567 ?
N1 Mn2 N8 90.9(2) . . ?
N4 Mn2 N8 97.3(2) 1_565 . ?
N2 Mn2 N8 94.8(2) 2_567 . ?
N1 Mn2 N10 88.5(5) . . ?
N4 Mn2 N10 84.8(5) 1_565 . ?
N2 Mn2 N10 166.8(5) 2_567 . ?
N8 Mn2 N10 98.3(6) . . ?
N1 Mn2 O7 84.6(2) . . ?
N4 Mn2 O7 86.6(2) 1_565 . ?
N2 Mn2 O7 92.3(3) 2_567 . ?
N8 Mn2 O7 171.7(3) . . ?
N10 Mn2 O7 74.7(6) . . ?
N1 Mn2 O1 86.0(4) . . ?
N4 Mn2 O1 89.8(4) 1_565 . ?
N2 Mn2 O1 175.9(4) 2_567 . ?
N8 Mn2 O1 81.2(4) . . ?
O7 Mn2 O1 91.5(5) . . ?
N3 Mn1 N13 92.2(3) 1_655 . ?
N3 Mn1 N7 93.30(19) 1_655 . ?
N13 Mn1 N7 100.3(3) . . ?
N3 Mn1 N6 171.9(2) 1_655 . ?
N13 Mn1 N6 93.0(3) . . ?
N7 Mn1 N6 91.84(19) . . ?
N3 Mn1 O3 84.3(2) 1_655 . ?
N13 Mn1 O3 85.5(3) . . ?
N7 Mn1 O3 173.8(2) . . ?
N6 Mn1 O3 89.9(2) . . ?
N3 Mn1 O4 87.8(3) 1_655 . ?
N13 Mn1 O4 159.8(3) . . ?
N7 Mn1 O4 99.9(3) . . ?
N6 Mn1 O4 85.2(2) . . ?
O3 Mn1 O4 74.4(3) . . ?
C2 N2 Mn2 175.8(5) . 2_567 ?
C7 N7 Mn1 174.5(5) . . ?
N4 C4 Mo1 175.1(5) . . ?
C1 N1 Mn2 160.1(5) . . ?
N2 C2 Mo1 176.7(5) . . ?
C3 N3 Mn1 163.8(5) . 1_455 ?
C4 N4 Mn2 163.2(5) . 1_545 ?
N3 C3 Mo1 178.1(6) . . ?
N1 C1 Mo1 176.8(5) . . ?
C8 N8 C10 95.4(11) . . ?
C8 N8 C9A 101.0(11) . . ?
C8 N8 Mn2 128.3(6) . . ?
C10 N8 Mn2 124.6(9) . . ?
C9A N8 Mn2 123.8(10) . . ?
N7 C7 Mo1 177.0(5) . 2_666 ?
N6 C6 Mo1 177.2(6) . . ?
C6 N6 Mn1 165.9(5) . . ?
N5 C5 Mo1 176.8(5) . . ?
C17 N13 C15A 97.1(10) . . ?
C17 N13 C16 99.3(10) . . ?
C17 N13 Mn1 129.1(6) . . ?
C15A N13 Mn1 120.5(8) . . ?
C16 N13 Mn1 124.5(9) . . ?
C16 C15 N12 102.7(14) . . ?
C15 C16 N13 110.0(15) . . ?
N12 C17 N13 115.5(9) . . ?
C17 N12 C15 102.7(12) . . ?
C17 N12 C16A 98.6(11) . . ?
C10A C9A N8 108(2) . . ?
C9A C10A N9 103.8(16) . . ?
N9 C9 C10 105.8(14) . . ?
N9 C9 C8 39.0(6) . . ?
C10 C9 C8 68.6(11) . . ?
N8 C10 C9 109.7(15) . . ?
N8 C10 C8 41.3(7) . . ?
C9 C10 C8 70.5(12) . . ?
C16A C15A N13 111.2(17) . . ?
C15A C16A N12 101.6(17) . . ?
C8 N9 C9 98.0(11) . . ?
C8 N9 C10A 99.8(11) . . ?
N9 C8 N8 119.4(10) . . ?
N9 C8 C10 82.7(10) . . ?
N8 C8 C10 43.3(7) . . ?
N9 C8 C9 43.0(7) . . ?
N8 C8 C9 82.9(8) . . ?
C10 C8 C9 41.0(7) . . ?
C11 C13 C11 117.0(11) 2_676 . ?
C11 C13 C13 61.2(10) 2_676 2_676 ?
C11 C13 C13 55.8(10) . 2_676 ?
C11 C13 N11 133.4(13) 2_676 . ?
C11 C13 N11 106.9(11) . . ?
C13 C13 N11 157.4(16) 2_676 . ?
C13 C11 N10 169.3(16) 2_676 . ?
C13 C11 C13 63.0(11) 2_676 . ?
N10 C11 C13 111.6(13) . . ?
N11 C12 N10 108.1(13) . . ?
C12 N11 C13 106.7(12) . . ?
C11 N10 C12 105.9(14) . . ?
C11 N10 Mn2 127.3(13) . . ?
C12 N10 Mn2 126.3(12) . . ?

_refine_diff_density_max         2.501
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.160


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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1899235'
loop_
_audit_author_name
_audit_author_address
'Michal Magott'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2019-06-17 deposited with the CCDC.	2019-06-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_1                   
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        7.2 Ratio
RESPONSE: These alerts regard elongated ellipsoids of non-bridging cyanide ligand, which can show increased mobility compared to the others. 
;
_vrf_PLAT260_1                   
;
PROBLEM: Large Average Ueq of Residue Including        O4      0.360 Check
RESPONSE: Solvent molecules residing in the pores of the network are hard to describe accurately.
;
_vrf_PLAT306_1                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O2 Check
RESPONSE: Hydrogen atoms connected to crystallization water molecules  cannot be clearly defined in this case.
;
_vrf_PLAT430_1                   
;
PROBLEM: Short Inter D...A Contact  O2       ..O3       .       2.63 Ang.
RESPONSE: Solvent molecules residing in the pores of the network are hard to describe accurately.
;
# Added during the CSD deposition process: Monday 17 June 2019 02:08 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47 H42 Mn4 Mo2 N36 O7'
_chemical_formula_weight         1634.80

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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   32.2732(9)
_cell_length_b                   10.7266(3)
_cell_length_c                   21.8215(6)
_cell_angle_alpha                90
_cell_angle_beta                 113.4260(10)
_cell_angle_gamma                90
_cell_volume                     6931.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    8595
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      25.42

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_F_000             3264
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.130
_shelx_estimated_absorpt_T_min   0.806
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6457
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0671 before and 0.0571 after correction.
The Ratio of minimum to maximum transmission is 0.8665.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_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            32259
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.381
_diffrn_reflns_theta_max         25.463
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6404
_reflns_number_gt                4872
_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_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0468P)²+94.0211P] 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         6404
_refine_ls_number_parameters     448
_refine_ls_number_restraints     98
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1387
_refine_ls_wR_factor_gt          0.1277
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.083
_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 0.35139(2) 0.27883(4) 0.26097(2) 0.01384(13) Uani 1 1 d . . . . .
O1 O 0.5000 0.2630(6) 0.2500 0.059(2) Uani 1 2 d DS T P . .
N1 N 0.3074(3) 0.2846(8) 0.0972(3) 0.066(2) Uani 1 1 d . . . . .
C1 C 0.3234(2) 0.2843(7) 0.1545(3) 0.0388(17) Uani 1 1 d . . . . .
Mn1 Mn 0.2500 0.2500 0.0000 0.0378(4) Uani 1 2 d S . P . .
Mn2 Mn 0.32106(3) -0.22216(8) 0.25457(4) 0.0197(2) Uani 1 1 d . . . . .
H1 H 0.5261(12) 0.212(3) 0.259(3) 0.024 Uiso 1 1 d D U . . .
O2 O 0.4583(5) 0.1015(13) 0.5153(9) 0.240(8) Uani 1 1 d . . . . .
N2 N 0.3941(3) 0.2776(10) 0.4259(4) 0.089(3) Uani 1 1 d . . . . .
C2 C 0.3777(2) 0.2766(8) 0.3675(3) 0.0437(18) Uani 1 1 d . . . . .
C5 C 0.3304(2) 0.4697(6) 0.2585(3) 0.0265(14) Uani 1 1 d . . . . .
N5 N 0.31976(18) 0.5734(5) 0.2555(3) 0.0410(15) Uani 1 1 d . . . . .
C4 C 0.28340(18) 0.2763(5) 0.2570(3) 0.0183(11) Uani 1 1 d . . . . .
O4 O 0.5105(4) 0.286(2) 0.0866(6) 0.359(16) Uani 1 1 d . . . . .
N4 N 0.24738(16) 0.2777(4) 0.2543(2) 0.0223(10) Uani 1 1 d . . . . .
Mn3 Mn 0.5000 0.47193(12) 0.2500 0.0244(3) Uani 1 2 d DS T P . .
O3 O 0.4520(6) 0.0738(13) 0.0957(7) 0.234(8) Uani 1 1 d . . . . .
N3 N 0.32266(18) -0.0180(5) 0.2578(3) 0.0291(12) Uani 1 1 d . . . . .
C3 C 0.3316(2) 0.0875(5) 0.2587(3) 0.0221(12) Uani 1 1 d . . . . .
N6 N 0.43894(17) 0.4515(5) 0.2726(3) 0.0304(13) Uani 1 1 d . . . . .
C6 C 0.40782(19) 0.3958(5) 0.2687(3) 0.0202(12) Uani 1 1 d . . . . .
C7 C 0.4025(3) 0.1652(8) 0.2540(7) 0.080(3) Uani 1 1 d . U . . .
N7 N 0.4300(4) 0.1053(9) 0.2470(9) 0.169(6) Uani 1 1 d . U . . .
N8 N 0.2079(3) 0.3715(7) 0.0340(4) 0.061(2) Uani 1 1 d . . . . .
C8 C 0.2190(5) 0.4432(10) 0.0891(5) 0.090(4) Uani 1 1 d . . . . .
H8 H 0.2480 0.4571 0.1234 0.108 Uiso 1 1 calc R U . . .
C19 C 0.3537(6) -0.1552(17) 0.0861(7) 0.132(5) Uani 1 1 d . U . . .
H19 H 0.3592 -0.1022 0.0552 0.158 Uiso 1 1 calc R U . . .
N15 N 0.3568(5) -0.2859(14) 0.0903(6) 0.144(5) Uani 1 1 d . U . . .
H15 H 0.3638 -0.3352 0.0635 0.172 Uiso 1 1 calc R U . . .
C15 C 0.4004(3) -0.3276(8) 0.3858(4) 0.055(2) Uani 1 1 d . . . . .
H15A H 0.3864 -0.4070 0.3806 0.066 Uiso 1 1 calc R U . . .
N16 N 0.54495(19) 0.4712(6) 0.3594(3) 0.0397(14) Uani 1 1 d . . . . .
C16 C 0.4395(3) -0.2995(10) 0.4349(5) 0.067(3) Uani 1 1 d . . . . .
H16 H 0.4576 -0.3508 0.4712 0.080 Uiso 1 1 calc R U . . .
C9 C 0.1637(5) 0.3785(12) 0.0023(7) 0.101(4) Uani 1 1 d . . . . .
H9 H 0.1485 0.3356 -0.0386 0.121 Uiso 1 1 calc R U . . .
N9 N 0.1769(5) 0.4927(13) 0.0839(7) 0.141(5) Uani 1 1 d . U . . .
H9A H 0.1735 0.5464 0.1121 0.169 Uiso 1 1 calc R U . . .
C20 C 0.5439(3) 0.5532(9) 0.4045(4) 0.058(2) Uani 1 1 d . . . . .
H20 H 0.5209 0.6141 0.3961 0.070 Uiso 1 1 calc R U . . .
C21 C 0.5840(2) 0.4074(8) 0.3916(4) 0.0471(19) Uani 1 1 d . . . . .
H21 H 0.5952 0.3444 0.3718 0.056 Uiso 1 1 calc R U . . .
C22 C 0.6045(3) 0.4452(9) 0.4553(5) 0.062(2) Uani 1 1 d . . . . .
H22 H 0.6314 0.4122 0.4883 0.075 Uiso 1 1 calc R U . . .
C23 C 0.5319(3) 0.7503(6) 0.2446(5) 0.048(2) Uani 1 1 d . . . . .
C24 C 0.5149(10) 0.877(3) 0.2324(11) 0.038(6) Uani 0.5 1 d . U P A 1
N19 N 0.5246(8) 0.867(2) 0.2585(10) 0.039(5) Uani 0.5 1 d . U P A 1
C10 C 0.1418(6) 0.4448(16) 0.0282(9) 0.128(5) Uani 1 1 d . U . . .
H10 H 0.1102 0.4577 0.0133 0.153 Uiso 1 1 calc R U . . .
N10 N 0.2307(2) 0.0856(6) 0.0480(3) 0.0380(14) Uani 1 1 d . . . . .
C12 C 0.2259(3) -0.0370(8) 0.0298(5) 0.058(2) Uani 1 1 d . . . . .
H12 H 0.2286 -0.0695 -0.0089 0.070 Uiso 1 1 calc R U . . .
N12 N 0.38262(18) -0.2303(5) 0.3435(3) 0.0332(12) Uani 1 1 d . . . . .
C11 C 0.2258(3) 0.0883(8) 0.1050(3) 0.051(2) Uani 1 1 d . . . . .
H11 H 0.2284 0.1615 0.1308 0.061 Uiso 1 1 calc R U . . .
N11 N 0.2167(2) -0.0233(7) 0.1219(3) 0.0569(19) Uani 1 1 d . . . . .
H11A H 0.2114 -0.0412 0.1575 0.068 Uiso 1 1 calc R U . . .
C13 C 0.2169(3) -0.1056(9) 0.0750(6) 0.072(3) Uani 1 1 d . . . . .
H13 H 0.2117 -0.1929 0.0740 0.086 Uiso 1 1 calc R U . . .
N13 N 0.4475(3) -0.1820(10) 0.4217(4) 0.083(3) Uani 1 1 d . . . . .
H13A H 0.4718 -0.1384 0.4452 0.099 Uiso 1 1 calc R U . . .
C14 C 0.4128(3) -0.1409(9) 0.3670(4) 0.058(2) Uani 1 1 d . . . . .
H14 H 0.4104 -0.0599 0.3482 0.070 Uiso 1 1 calc R U . . .
N14 N 0.3376(2) -0.2208(6) 0.1687(3) 0.0414(14) Uani 1 1 d . U . . .
C18 C 0.3412(4) -0.1225(11) 0.1348(5) 0.094(4) Uani 1 1 d . U . . .
H18 H 0.3357 -0.0392 0.1442 0.113 Uiso 1 1 calc R U . . .
N18 N 0.5000 0.6756(6) 0.2500 0.0276(17) Uani 1 2 d S T P A .
C17 C 0.3479(4) -0.3206(11) 0.1396(5) 0.080(3) Uani 1 1 d . U . . .
H17 H 0.3484 -0.4045 0.1538 0.095 Uiso 1 1 calc R U . . .
N17 N 0.5792(3) 0.5397(8) 0.4633(3) 0.067(2) Uani 1 1 d . . . . .
H17A H 0.5848 0.5836 0.4999 0.080 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C7 2.105(8) . ?
Mo1 C1 2.132(7) . ?
Mo1 C2 2.135(7) . ?
Mo1 C3 2.145(6) . ?
Mo1 C5 2.151(6) . ?
Mo1 C4 2.161(5) . ?
Mo1 C6 2.163(6) . ?
O1 Mn3 2.242(7) . ?
O1 H1 0.954(19) . ?
N1 C1 1.148(9) . ?
N1 Mn1 2.224(6) . ?
Mn1 N8 2.212(8) . ?
Mn1 N8 2.212(8) 7 ?
Mn1 N1 2.224(6) 7 ?
Mn1 N10 2.261(5) 7 ?
Mn1 N10 2.261(5) . ?
Mn2 N4 2.139(5) 4_545 ?
Mn2 N14 2.142(6) . ?
Mn2 N12 2.158(5) . ?
Mn2 N3 2.191(5) . ?
Mn2 N5 2.193(5) 1_545 ?
N2 C2 1.169(9) . ?
C5 N5 1.158(8) . ?
N5 Mn2 2.193(5) 1_565 ?
C4 N4 1.140(7) . ?
N4 Mn2 2.139(5) 4 ?
Mn3 N18 2.185(7) . ?
Mn3 N6 2.224(5) . ?
Mn3 N6 2.224(5) 2_655 ?
Mn3 N16 2.248(6) . ?
Mn3 N16 2.248(6) 2_655 ?
N3 C3 1.166(8) . ?
N6 C6 1.142(7) . ?
C7 N7 1.156(12) . ?
N8 C9 1.318(15) . ?
N8 C8 1.351(13) . ?
C8 N9 1.420(16) . ?
C8 H8 0.9500 . ?
C19 C18 1.324(15) . ?
C19 N15 1.407(19) . ?
C19 H19 0.9500 . ?
N15 C17 1.274(15) . ?
N15 H15 0.8800 . ?
C15 C16 1.324(12) . ?
C15 N12 1.359(10) . ?
C15 H15A 0.9500 . ?
N16 C20 1.331(10) . ?
N16 C21 1.358(9) . ?
C16 N13 1.342(13) . ?
C16 H16 0.9500 . ?
C9 C10 1.281(18) . ?
C9 H9 0.9500 . ?
N9 C10 1.390(19) . ?
N9 H9A 0.8800 . ?
C20 N17 1.344(10) . ?
C20 H20 0.9500 . ?
C21 C22 1.342(12) . ?
C21 H21 0.9500 . ?
C22 N17 1.356(11) . ?
C22 H22 0.9500 . ?
C23 N19 1.33(3) . ?
C23 N18 1.347(8) . ?
C23 C24 1.45(3) . ?
C24 N19 0.54(3) . ?
C24 N19 1.368(17) 2_655 ?
C24 C24 1.45(6) 2_655 ?
N19 C24 1.368(17) 2_655 ?
N19 N19 1.48(5) 2_655 ?
C10 H10 0.9500 . ?
N10 C11 1.316(9) . ?
N10 C12 1.365(10) . ?
C12 C13 1.351(11) . ?
C12 H12 0.9500 . ?
N12 C14 1.316(10) . ?
C11 N11 1.319(10) . ?
C11 H11 0.9500 . ?
N11 C13 1.353(12) . ?
N11 H11A 0.8800 . ?
C13 H13 0.9500 . ?
N13 C14 1.347(11) . ?
N13 H13A 0.8800 . ?
C14 H14 0.9500 . ?
N14 C18 1.320(11) . ?
N14 C17 1.353(10) . ?
C18 H18 0.9500 . ?
N18 C23 1.347(8) 2_655 ?
C17 H17 0.9500 . ?
N17 H17A 0.8800 . ?

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
C7 Mo1 C1 86.7(4) . . ?
C7 Mo1 C2 95.0(4) . . ?
C1 Mo1 C2 178.2(3) . . ?
C7 Mo1 C3 71.3(3) . . ?
C1 Mo1 C3 90.5(2) . . ?
C2 Mo1 C3 90.0(3) . . ?
C7 Mo1 C5 142.9(3) . . ?
C1 Mo1 C5 87.3(3) . . ?
C2 Mo1 C5 91.3(3) . . ?
C3 Mo1 C5 145.3(2) . . ?
C7 Mo1 C4 143.3(3) . . ?
C1 Mo1 C4 88.4(2) . . ?
C2 Mo1 C4 90.1(2) . . ?
C3 Mo1 C4 72.5(2) . . ?
C5 Mo1 C4 72.9(2) . . ?
C7 Mo1 C6 71.4(3) . . ?
C1 Mo1 C6 92.7(2) . . ?
C2 Mo1 C6 87.9(2) . . ?
C3 Mo1 C6 142.3(2) . . ?
C5 Mo1 C6 72.4(2) . . ?
C4 Mo1 C6 145.1(2) . . ?
Mn3 O1 H1 125(3) . . ?
C1 N1 Mn1 151.9(6) . . ?
N1 C1 Mo1 178.0(6) . . ?
N8 Mn1 N8 180.0 . 7 ?
N8 Mn1 N1 88.4(3) . . ?
N8 Mn1 N1 91.6(3) 7 . ?
N8 Mn1 N1 91.6(3) . 7 ?
N8 Mn1 N1 88.4(3) 7 7 ?
N1 Mn1 N1 180.0 . 7 ?
N8 Mn1 N10 90.8(2) . 7 ?
N8 Mn1 N10 89.2(2) 7 7 ?
N1 Mn1 N10 91.9(2) . 7 ?
N1 Mn1 N10 88.1(2) 7 7 ?
N8 Mn1 N10 89.2(2) . . ?
N8 Mn1 N10 90.8(2) 7 . ?
N1 Mn1 N10 88.1(2) . . ?
N1 Mn1 N10 91.9(2) 7 . ?
N10 Mn1 N10 180.0(3) 7 . ?
N4 Mn2 N14 121.9(2) 4_545 . ?
N4 Mn2 N12 129.0(2) 4_545 . ?
N14 Mn2 N12 109.1(2) . . ?
N4 Mn2 N3 90.80(19) 4_545 . ?
N14 Mn2 N3 90.6(2) . . ?
N12 Mn2 N3 90.6(2) . . ?
N4 Mn2 N5 88.68(19) 4_545 1_545 ?
N14 Mn2 N5 91.6(2) . 1_545 ?
N12 Mn2 N5 88.0(2) . 1_545 ?
N3 Mn2 N5 177.7(2) . 1_545 ?
N2 C2 Mo1 176.6(7) . . ?
N5 C5 Mo1 177.5(6) . . ?
C5 N5 Mn2 162.6(5) . 1_565 ?
N4 C4 Mo1 178.4(5) . . ?
C4 N4 Mn2 177.8(5) . 4 ?
N18 Mn3 N6 95.64(13) . . ?
N18 Mn3 N6 95.64(13) . 2_655 ?
N6 Mn3 N6 168.7(3) . 2_655 ?
N18 Mn3 O1 180.0 . . ?
N6 Mn3 O1 84.36(13) . . ?
N6 Mn3 O1 84.36(13) 2_655 . ?
N18 Mn3 N16 90.21(16) . . ?
N6 Mn3 N16 91.1(2) . . ?
N6 Mn3 N16 88.9(2) 2_655 . ?
O1 Mn3 N16 89.79(16) . . ?
N18 Mn3 N16 90.21(16) . 2_655 ?
N6 Mn3 N16 88.9(2) . 2_655 ?
N6 Mn3 N16 91.1(2) 2_655 2_655 ?
O1 Mn3 N16 89.79(16) . 2_655 ?
N16 Mn3 N16 179.6(3) . 2_655 ?
C3 N3 Mn2 166.7(5) . . ?
N3 C3 Mo1 177.1(5) . . ?
C6 N6 Mn3 149.9(5) . . ?
N6 C6 Mo1 176.1(5) . . ?
N7 C7 Mo1 176.5(14) . . ?
C9 N8 C8 106.4(10) . . ?
C9 N8 Mn1 122.6(9) . . ?
C8 N8 Mn1 130.8(8) . . ?
N8 C8 N9 103.7(12) . . ?
N8 C8 H8 128.2 . . ?
N9 C8 H8 128.2 . . ?
C18 C19 N15 104.4(11) . . ?
C18 C19 H19 127.8 . . ?
N15 C19 H19 127.8 . . ?
C17 N15 C19 108.1(10) . . ?
C17 N15 H15 125.9 . . ?
C19 N15 H15 125.9 . . ?
C16 C15 N12 112.6(8) . . ?
C16 C15 H15A 123.7 . . ?
N12 C15 H15A 123.7 . . ?
C20 N16 C21 104.0(7) . . ?
C20 N16 Mn3 126.0(5) . . ?
C21 N16 Mn3 128.7(5) . . ?
C15 C16 N13 104.0(8) . . ?
C15 C16 H16 128.0 . . ?
N13 C16 H16 128.0 . . ?
C10 C9 N8 118.2(16) . . ?
C10 C9 H9 120.9 . . ?
N8 C9 H9 120.9 . . ?
C10 N9 C8 110.6(13) . . ?
C10 N9 H9A 124.7 . . ?
C8 N9 H9A 124.7 . . ?
N16 C20 N17 111.9(8) . . ?
N16 C20 H20 124.1 . . ?
N17 C20 H20 124.1 . . ?
C22 C21 N16 111.0(8) . . ?
C22 C21 H21 124.5 . . ?
N16 C21 H21 124.5 . . ?
C21 C22 N17 106.6(8) . . ?
C21 C22 H22 126.7 . . ?
N17 C22 H22 126.7 . . ?
N19 C23 N18 109.1(12) . . ?
N19 C23 C24 21.8(12) . . ?
N18 C23 C24 108.9(14) . . ?
N19 C24 N19 91(6) . 2_655 ?
N19 C24 C24 71(5) . 2_655 ?
N19 C24 C24 21.8(13) 2_655 2_655 ?
N19 C24 C23 67(5) . . ?
N19 C24 C23 102(3) 2_655 . ?
C24 C24 C23 100.8(12) 2_655 . ?
C24 N19 C23 92(6) . . ?
C24 N19 C24 87(6) . 2_655 ?
C23 N19 C24 112(3) . 2_655 ?
C24 N19 N19 68(5) . 2_655 ?
C23 N19 N19 102.4(11) . 2_655 ?
C24 N19 N19 21.4(12) 2_655 2_655 ?
C9 C10 N9 101.0(15) . . ?
C9 C10 H10 129.5 . . ?
N9 C10 H10 129.5 . . ?
C11 N10 C12 104.7(6) . . ?
C11 N10 Mn1 125.5(5) . . ?
C12 N10 Mn1 129.6(5) . . ?
C13 C12 N10 110.1(8) . . ?
C13 C12 H12 124.9 . . ?
N10 C12 H12 124.9 . . ?
C14 N12 C15 104.4(7) . . ?
C14 N12 Mn2 126.4(5) . . ?
C15 N12 Mn2 129.1(5) . . ?
N10 C11 N11 111.6(8) . . ?
N10 C11 H11 124.2 . . ?
N11 C11 H11 124.2 . . ?
C11 N11 C13 108.2(7) . . ?
C11 N11 H11A 125.9 . . ?
C13 N11 H11A 125.9 . . ?
C12 C13 N11 105.3(8) . . ?
C12 C13 H13 127.3 . . ?
N11 C13 H13 127.3 . . ?
C16 N13 C14 109.5(8) . . ?
C16 N13 H13A 125.2 . . ?
C14 N13 H13A 125.2 . . ?
N12 C14 N13 109.4(9) . . ?
N12 C14 H14 125.3 . . ?
N13 C14 H14 125.3 . . ?
C18 N14 C17 106.0(8) . . ?
C18 N14 Mn2 127.2(6) . . ?
C17 N14 Mn2 126.8(7) . . ?
N14 C18 C19 111.2(12) . . ?
N14 C18 H18 124.4 . . ?
C19 C18 H18 124.4 . . ?
C23 N18 C23 107.0(8) . 2_655 ?
C23 N18 Mn3 126.5(4) . . ?
C23 N18 Mn3 126.5(4) 2_655 . ?
N15 C17 N14 110.3(11) . . ?
N15 C17 H17 124.9 . . ?
N14 C17 H17 124.9 . . ?
C20 N17 C22 106.4(8) . . ?
C20 N17 H17A 126.8 . . ?
C22 N17 H17A 126.8 . . ?

_refine_diff_density_max         1.171
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.120


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

data_4
_database_code_depnum_ccdc_archive 'CCDC 1899238'
loop_
_audit_author_name
_audit_author_address
'Michal Magott'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2019-06-17 deposited with the CCDC.	2019-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H20 Mn2 Mo N9 O9'
_chemical_formula_weight         592.15

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'
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'
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'

_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                   7.239(5)
_cell_length_b                   12.039(5)
_cell_length_c                   12.344(5)
_cell_angle_alpha                80.062(5)
_cell_angle_beta                 89.517(5)
_cell_angle_gamma                89.216(5)
_cell_volume                     1059.5(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3312
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      26.58

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_F_000             590
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.815
_shelx_estimated_absorpt_T_min   0.798
_shelx_estimated_absorpt_T_max   0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7983
_exptl_absorpt_correction_T_max  0.9147
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0671 before and 0.0571 after correction.
The Ratio of minimum to maximum transmission is 0.8665.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_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            11350
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.675
_diffrn_reflns_theta_max         26.664
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4390
_reflns_number_gt                3675
_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_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0294P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4390
_refine_ls_number_parameters     328
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0757
_refine_ls_wR_factor_gt          0.0713
_refine_ls_goodness_of_fit_ref   1.036
_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
Mo01 Mo 0.49418(3) 0.20228(2) 0.71909(2) 0.00772(8) Uani 1 1 d . . . . .
Mn4 Mn 1.0000 0.5000 0.5000 0.01021(15) Uani 1 2 d S . P . .
Mn1 Mn 0.0000 0.0000 0.5000 0.00953(15) Uani 1 2 d S . P . .
Mn2 Mn 0.0000 0.0000 1.0000 0.01262(16) Uani 1 2 d S . P . .
Mn3 Mn 0.5000 0.5000 1.0000 0.01426(16) Uani 1 2 d S . P . .
O1 O -0.0182(3) -0.18590(19) 0.57651(19) 0.0159(5) Uani 1 1 d D . . . .
H1A H -0.033(4) -0.232(2) 0.526(2) 0.019 Uiso 1 1 d D U . . .
H1B H 0.074(4) -0.211(3) 0.626(2) 0.019 Uiso 1 1 d D U . . .
O3 O 0.6650(3) 0.3540(2) 1.07663(19) 0.0221(6) Uani 1 1 d D . . . .
H3A H 0.704(5) 0.348(3) 1.1480(17) 0.027 Uiso 1 1 d D U . . .
H3B H 0.623(5) 0.2838(19) 1.069(3) 0.027 Uiso 1 1 d D U . . .
O2 O 0.0526(3) -0.0778(2) 0.85031(19) 0.0206(5) Uani 1 1 d D . . . .
H2B H -0.024(4) -0.137(2) 0.846(3) 0.025 Uiso 1 1 d D U . . .
H2A H 0.055(5) -0.025(2) 0.789(2) 0.025 Uiso 1 1 d D U . . .
O01 O 0.2671(3) 0.70179(19) 0.69784(18) 0.0183(5) Uani 1 1 d . . . . .
O5 O 1.0131(3) 0.5402(2) 0.66906(19) 0.0205(5) Uani 1 1 d D . . . .
H5A H 1.005(4) 0.486(2) 0.730(2) 0.025 Uiso 1 1 d D U . . .
H5B H 1.113(4) 0.583(3) 0.683(3) 0.025 Uiso 1 1 d D U . . .
O1S O 1.0110(4) 0.6098(2) 1.1228(2) 0.0274(6) Uani 1 1 d D . . . .
H1SA H 1.031(5) 0.6851(17) 1.122(3) 0.033 Uiso 1 1 d D U . . .
H1SB H 1.108(4) 0.579(3) 1.088(3) 0.033 Uiso 1 1 d D U . . .
O3S O 0.7921(4) 0.7787(2) 0.7977(2) 0.0283(6) Uani 1 1 d D . . . .
H3SA H 0.821(5) 0.788(3) 0.7213(17) 0.034 Uiso 1 1 d D U . . .
H3SB H 0.677(3) 0.816(3) 0.806(3) 0.034 Uiso 1 1 d D U . . .
O4 O 0.7717(3) 0.5735(2) 0.9421(2) 0.0249(6) Uani 1 1 d D . . . .
H4B H 0.840(4) 0.593(3) 1.000(2) 0.030 Uiso 1 1 d D U . . .
H4A H 0.780(5) 0.634(2) 0.884(2) 0.030 Uiso 1 1 d D U . . .
N1 N 0.2153(4) 0.0307(2) 0.6210(2) 0.0145(6) Uani 1 1 d . . . . .
N04 N 0.4916(4) 0.8073(2) 0.6009(2) 0.0207(7) Uani 1 1 d D . . . .
H04A H 0.591(4) 0.812(3) 0.546(2) 0.025 Uiso 1 1 d D U . . .
H04B H 0.410(4) 0.872(2) 0.600(3) 0.025 Uiso 1 1 d D U . . .
N4 N 0.1992(4) 0.3579(2) 0.5509(2) 0.0176(6) Uani 1 1 d . . . . .
O4S O 0.4748(4) 0.8627(2) 0.8862(2) 0.0316(6) Uani 1 1 d D . . . .
H4SA H 0.531(5) 0.883(3) 0.947(2) 0.038 Uiso 1 1 d D U . . .
H4SB H 0.369(4) 0.908(3) 0.871(3) 0.038 Uiso 1 1 d D U . . .
N3 N 0.4725(4) 0.4169(2) 0.8561(2) 0.0199(6) Uani 1 1 d . . . . .
N5 N 0.7798(4) 0.3804(2) 0.5633(2) 0.0173(6) Uani 1 1 d . . . . .
N6 N 0.8234(4) 0.1308(3) 0.9051(2) 0.0216(7) Uani 1 1 d . . . . .
C2 C 0.3256(4) 0.1377(3) 0.8588(3) 0.0139(7) Uani 1 1 d . . . . .
N7 N 0.7795(4) 0.0385(2) 0.6087(2) 0.0174(6) Uani 1 1 d . . . . .
N03 N 0.5291(4) 0.6155(3) 0.6527(3) 0.0273(7) Uani 1 1 d D . . . .
H03A H 0.496(5) 0.5420(19) 0.688(3) 0.033 Uiso 1 1 d D U . . .
H03B H 0.645(3) 0.612(3) 0.614(3) 0.033 Uiso 1 1 d D U . . .
C1 C 0.3188(4) 0.0882(3) 0.6571(2) 0.0102(6) Uani 1 1 d . . . . .
C4 C 0.2993(4) 0.3031(3) 0.6121(3) 0.0126(7) Uani 1 1 d . . . . .
C6 C 0.7110(4) 0.1568(3) 0.8392(3) 0.0134(7) Uani 1 1 d . . . . .
C5 C 0.6815(4) 0.3170(3) 0.6155(2) 0.0126(7) Uani 1 1 d . . . . .
C3 C 0.4755(4) 0.3459(3) 0.8057(3) 0.0137(7) Uani 1 1 d . . . . .
N2 N 0.2425(4) 0.1036(2) 0.9390(2) 0.0208(7) Uani 1 1 d . . . . .
C7 C 0.6723(4) 0.0935(3) 0.6459(3) 0.0125(7) Uani 1 1 d . . . . .
C02 C 0.4235(5) 0.7075(3) 0.6507(3) 0.0167(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo01 C1 2.124(3) . ?
Mo01 C7 2.130(3) . ?
Mo01 C2 2.144(3) . ?
Mo01 C4 2.153(3) . ?
Mo01 C6 2.167(3) . ?
Mo01 C3 2.187(3) . ?
Mo01 C5 2.190(3) . ?
Mn4 N5 2.209(3) 2_766 ?
Mn4 N5 2.209(3) . ?
Mn4 O5 2.225(2) 2_766 ?
Mn4 O5 2.225(2) . ?
Mn4 N4 2.231(3) 1_655 ?
Mn4 N4 2.231(3) 2_666 ?
Mn1 N7 2.173(3) 2_656 ?
Mn1 N7 2.173(3) 1_455 ?
Mn1 N1 2.245(3) 2_556 ?
Mn1 N1 2.245(3) . ?
Mn1 O1 2.279(2) . ?
Mn1 O1 2.279(2) 2_556 ?
Mn2 N6 2.195(3) 2_657 ?
Mn2 N6 2.195(3) 1_455 ?
Mn2 N2 2.218(3) . ?
Mn2 N2 2.218(3) 2_557 ?
Mn2 O2 2.239(2) 2_557 ?
Mn2 O2 2.239(2) . ?
Mn3 O3 2.191(2) . ?
Mn3 O3 2.191(2) 2_667 ?
Mn3 N3 2.195(3) 2_667 ?
Mn3 N3 2.195(3) . ?
Mn3 O4 2.229(3) . ?
Mn3 O4 2.229(3) 2_667 ?
O01 C02 1.266(4) . ?
N1 C1 1.169(4) . ?
N04 C02 1.350(4) . ?
N4 C4 1.164(4) . ?
N4 Mn4 2.231(3) 1_455 ?
N3 C3 1.141(4) . ?
N5 C5 1.158(4) . ?
N6 C6 1.157(4) . ?
N6 Mn2 2.195(3) 1_655 ?
C2 N2 1.168(4) . ?
N7 C7 1.156(4) . ?
N7 Mn1 2.173(3) 1_655 ?
N03 C02 1.333(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Mo01 C7 74.10(12) . . ?
C1 Mo01 C2 77.07(12) . . ?
C7 Mo01 C2 120.91(12) . . ?
C1 Mo01 C4 73.29(12) . . ?
C7 Mo01 C4 116.73(12) . . ?
C2 Mo01 C4 102.17(12) . . ?
C1 Mo01 C6 125.92(12) . . ?
C7 Mo01 C6 75.97(12) . . ?
C2 Mo01 C6 81.29(12) . . ?
C4 Mo01 C6 160.49(12) . . ?
C1 Mo01 C3 139.69(12) . . ?
C7 Mo01 C3 146.20(12) . . ?
C2 Mo01 C3 77.76(12) . . ?
C4 Mo01 C3 81.93(12) . . ?
C6 Mo01 C3 80.06(12) . . ?
C1 Mo01 C5 123.45(12) . . ?
C7 Mo01 C5 75.76(12) . . ?
C2 Mo01 C5 158.17(12) . . ?
C4 Mo01 C5 79.43(12) . . ?
C6 Mo01 C5 90.35(12) . . ?
C3 Mo01 C5 80.96(12) . . ?
N5 Mn4 N5 180.0 2_766 . ?
N5 Mn4 O5 86.62(9) 2_766 2_766 ?
N5 Mn4 O5 93.38(9) . 2_766 ?
N5 Mn4 O5 93.38(9) 2_766 . ?
N5 Mn4 O5 86.63(9) . . ?
O5 Mn4 O5 180.0 2_766 . ?
N5 Mn4 N4 93.27(11) 2_766 1_655 ?
N5 Mn4 N4 86.73(11) . 1_655 ?
O5 Mn4 N4 91.04(10) 2_766 1_655 ?
O5 Mn4 N4 88.96(10) . 1_655 ?
N5 Mn4 N4 86.73(11) 2_766 2_666 ?
N5 Mn4 N4 93.27(11) . 2_666 ?
O5 Mn4 N4 88.96(10) 2_766 2_666 ?
O5 Mn4 N4 91.04(10) . 2_666 ?
N4 Mn4 N4 180.00(14) 1_655 2_666 ?
N7 Mn1 N7 180.0 2_656 1_455 ?
N7 Mn1 N1 91.27(11) 2_656 2_556 ?
N7 Mn1 N1 88.73(11) 1_455 2_556 ?
N7 Mn1 N1 88.73(11) 2_656 . ?
N7 Mn1 N1 91.27(11) 1_455 . ?
N1 Mn1 N1 180.00(10) 2_556 . ?
N7 Mn1 O1 90.35(9) 2_656 . ?
N7 Mn1 O1 89.65(9) 1_455 . ?
N1 Mn1 O1 88.04(9) 2_556 . ?
N1 Mn1 O1 91.97(9) . . ?
N7 Mn1 O1 89.65(10) 2_656 2_556 ?
N7 Mn1 O1 90.35(9) 1_455 2_556 ?
N1 Mn1 O1 91.97(9) 2_556 2_556 ?
N1 Mn1 O1 88.03(9) . 2_556 ?
O1 Mn1 O1 180.0 . 2_556 ?
N6 Mn2 N6 180.0 2_657 1_455 ?
N6 Mn2 N2 91.79(12) 2_657 . ?
N6 Mn2 N2 88.21(11) 1_455 . ?
N6 Mn2 N2 88.21(12) 2_657 2_557 ?
N6 Mn2 N2 91.79(12) 1_455 2_557 ?
N2 Mn2 N2 180.0 . 2_557 ?
N6 Mn2 O2 90.81(10) 2_657 2_557 ?
N6 Mn2 O2 89.19(10) 1_455 2_557 ?
N2 Mn2 O2 96.60(10) . 2_557 ?
N2 Mn2 O2 83.40(10) 2_557 2_557 ?
N6 Mn2 O2 89.19(10) 2_657 . ?
N6 Mn2 O2 90.81(10) 1_455 . ?
N2 Mn2 O2 83.40(10) . . ?
N2 Mn2 O2 96.60(10) 2_557 . ?
O2 Mn2 O2 180.0 2_557 . ?
O3 Mn3 O3 180.0 . 2_667 ?
O3 Mn3 N3 92.20(10) . 2_667 ?
O3 Mn3 N3 87.80(10) 2_667 2_667 ?
O3 Mn3 N3 87.80(10) . . ?
O3 Mn3 N3 92.20(10) 2_667 . ?
N3 Mn3 N3 180.0 2_667 . ?
O3 Mn3 O4 84.64(10) . . ?
O3 Mn3 O4 95.36(10) 2_667 . ?
N3 Mn3 O4 87.51(10) 2_667 . ?
N3 Mn3 O4 92.49(10) . . ?
O3 Mn3 O4 95.36(10) . 2_667 ?
O3 Mn3 O4 84.64(10) 2_667 2_667 ?
N3 Mn3 O4 92.49(10) 2_667 2_667 ?
N3 Mn3 O4 87.51(10) . 2_667 ?
O4 Mn3 O4 180.0 . 2_667 ?
C1 N1 Mn1 152.6(2) . . ?
C4 N4 Mn4 154.1(3) . 1_455 ?
C3 N3 Mn3 158.4(3) . . ?
C5 N5 Mn4 166.9(3) . . ?
C6 N6 Mn2 149.8(3) . 1_655 ?
N2 C2 Mo01 175.9(3) . . ?
C7 N7 Mn1 157.3(3) . 1_655 ?
N1 C1 Mo01 176.0(3) . . ?
N4 C4 Mo01 177.3(3) . . ?
N6 C6 Mo01 178.1(3) . . ?
N5 C5 Mo01 177.5(3) . . ?
N3 C3 Mo01 175.6(3) . . ?
C2 N2 Mn2 142.2(3) . . ?
N7 C7 Mo01 175.1(3) . . ?
O01 C02 N03 120.9(3) . . ?
O01 C02 N04 121.0(3) . . ?
N03 C02 N04 118.0(3) . . ?

_refine_diff_density_max         0.505
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.109


_chemical_properties_physical    Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_m308_final_xprep-auto
_database_code_depnum_ccdc_archive 'CCDC 1899237'
loop_
_audit_author_name
_audit_author_address
'Michal Magott'
;Jagiellonian University
Poland
;
_audit_update_record             
;
2019-06-17 deposited with the CCDC.	2019-06-27 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_m308_final_xprep-auto 
;
PROBLEM: Non-Solvent  Resd 1  C   Ueq(max)/Ueq(min) Range        6.7 Ratio
RESPONSE: Crystals of 3 are not stable in contact with oxygen, which deteriorates diffraction data and increases difficulties with disorder refinement.
;
_vrf_PLAT306_m308_final_xprep-auto 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O8 Check
RESPONSE: Hydrogen atoms connected to crystallization water molecules cannot be clearly defined in this case.
;
_vrf_PLAT975_m308_final_xprep-auto 
;
PROBLEM: Check Calcd Resid. Dens.  0.90A   From O11             1.92 eA-3
RESPONSE: Crystals of 3 are not stable in contact with oxygen, which deteriorates diffraction data and increases difficulties with disorder refinement.
;
# Added during the CSD deposition process: Monday 17 June 2019 02:36 PM
# end Validation Reply Form

_audit_creation_date             2018-08-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2015/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10.4 H11 Mn2 Mo N12.1 O4.3, 5.6(O)'
_chemical_formula_sum            'C10.40 H11 Mn2 Mo N12.10 O9.90'
_chemical_formula_weight         669.73
_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'
Mo Mo -1.6832 0.6857 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x+, y+, z+'
'-x+, -y+, -z+'

_cell_length_a                   10.5826(2)
_cell_length_b                   10.9297(2)
_cell_length_c                   12.3540(3)
_cell_angle_alpha                67.6550(10)
_cell_angle_beta                 78.1670(10)
_cell_angle_gamma                86.3500(10)
_cell_volume                     1293.38(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15346
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.93
_shelx_estimated_absorpt_T_max   0.753
_shelx_estimated_absorpt_T_min   0.661
_exptl_absorpt_coefficient_mu    1.504
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0431 before and 0.0352 after correction.
The Ratio of minimum to maximum transmission is 0.8880.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             659
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0193
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19094
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.493
_diffrn_reflns_theta_min         2.794
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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                5506
_reflns_number_total             5911
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    ?
_refine_diff_density_max         1.932
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.0080(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2015/1 (Sheldrick 2015'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5911
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0332
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0329P)²+3.7856P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0837
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H,H) groups
2. Restrained distances
 H6B-O6
 0.95 with sigma of 0.02
 H6A-O6
 0.95 with sigma of 0.02
 H7A-O7
 0.95 with sigma of 0.02
 H7B-O7
 0.95 with sigma of 0.02
 H5B-O5
 0.95 with sigma of 0.02
 H5A-O5
 0.95 with sigma of 0.02
 H4B-O4
 0.95 with sigma of 0.02
 H4A-O4
 0.95 with sigma of 0.02
 C11-C10
 2.13 with sigma of 0.01
 H7A-H7B
 1.5 with sigma of 0.2
 H6A-H6B
 1.5 with sigma of 0.2
 H5A-H5B
 1.5 with sigma of 0.2
 H4A-H4B
 1.5 with sigma of 0.2
3. Uiso/Uaniso restraints and constraints
N11 \\sim C10 \\sim C11 \\sim N13: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C3) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(N11) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: N11(0.7) C10(0.7) N12(0.7) C11(0.7) N13(0.7) O2(0.3) O3(0.3) O1(0.3)
5.a Aromatic/amide H refined with riding coordinates:
 C8(H8), N10(H10), C9(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Mo1 Mo 0.80190(2) 0.18269(2) 0.71380(2) 0.00963(8) Uani 1 1 d . . . . .
Mn1 Mn 1.19581(4) 0.30308(4) 0.31837(4) 0.01712(11) Uani 1 1 d . . . . .
Mn2 Mn 0.28060(4) 0.12357(4) 0.81789(4) 0.01633(11) Uani 1 1 d . . . . .
O12 O 0.0067(3) 0.8074(2) 0.9216(2) 0.0330(5) Uani 1 1 d . . . . .
O7 O 0.3048(2) 0.3074(2) 0.6510(2) 0.0253(5) Uani 1 1 d D . . . .
H7A H 0.241(4) 0.342(4) 0.639(4) 0.030 Uiso 1 1 d DR . . . .
H7B H 0.360(4) 0.350(4) 0.651(4) 0.030 Uiso 1 1 d DR . . . .
O4 O 1.3396(2) 0.2718(3) 0.4322(2) 0.0328(6) Uani 1 1 d D . . . .
H4A H 1.330(4) 0.274(4) 0.496(4) 0.039 Uiso 1 1 d DR . . . .
H4B H 1.411(4) 0.215(4) 0.427(4) 0.039 Uiso 1 1 d DR . . . .
O8 O 0.1633(4) 0.5967(3) 1.0047(3) 0.0610(9) Uani 1 1 d . . . . .
O9 O 0.2264(5) -0.4764(5) 0.8150(5) 0.116(2) Uani 1 1 d . . . . .
O10 O 0.1039(3) 0.4691(3) 0.6567(4) 0.0737(12) Uani 1 1 d . . . . .
C5 C 0.9822(2) 0.1404(3) 0.7719(2) 0.0140(5) Uani 1 1 d . . . . .
N5 N 1.0800(2) 0.1164(3) 0.8027(2) 0.0211(5) Uani 1 1 d . . . . .
C4 C 0.7121(3) 0.2793(3) 0.5623(3) 0.0241(6) Uani 1 1 d . . . . .
N8 N 0.3293(3) 0.0013(3) 0.7062(2) 0.0253(5) Uani 1 1 d . . . . .
O6 O 0.2281(3) 0.2519(4) 0.9224(3) 0.0515(9) Uani 1 1 d D . . . .
H6A H 0.236(6) 0.320(6) 0.891(5) 0.062 Uiso 1 1 d DR . . . .
H6B H 0.160(6) 0.232(6) 0.960(5) 0.062 Uiso 1 1 d DR . . . .
N7 N 0.8021(3) -0.1026(2) 0.6785(2) 0.0250(5) Uani 1 1 d . . . . .
N6 N 1.0375(3) 0.2658(3) 0.4738(2) 0.0248(5) Uani 1 1 d . . . . .
O5 O 1.0600(3) 0.3552(3) 0.1914(2) 0.0349(6) Uani 1 1 d D . . . .
H5A H 1.063(5) 0.415(5) 0.149(4) 0.042 Uiso 1 1 d DR . . . .
H5B H 1.039(4) 0.298(5) 0.165(4) 0.042 Uiso 1 1 d DR . . . .
C1 C 0.7996(3) 0.3759(3) 0.7216(2) 0.0173(5) Uani 1 1 d . . . . .
N1 N 0.7981(3) 0.4822(3) 0.7205(3) 0.0294(6) Uani 1 1 d . . . . .
C3 C 0.7628(3) 0.0916(3) 0.9058(3) 0.0193(6) Uani 1 1 d . U . . .
N3 N 0.7423(3) 0.0410(3) 1.0087(2) 0.0316(6) Uani 1 1 d . U . . .
N4 N 0.6637(3) 0.3331(3) 0.4818(3) 0.0411(8) Uani 1 1 d . . . . .
C2 C 0.5966(3) 0.1593(3) 0.7746(3) 0.0187(5) Uani 1 1 d . . . . .
N2 N 0.4867(2) 0.1471(3) 0.8062(3) 0.0306(6) Uani 1 1 d . . . . .
C8 C 0.2589(4) -0.0323(4) 0.6458(4) 0.0383(8) Uani 1 1 d . . . . .
H8 H 0.1732 -0.0043 0.6385 0.046 Uiso 1 1 calc R . . . .
N10 N 0.3249(3) -0.1110(4) 0.5963(4) 0.0470(9) Uani 1 1 d . . . . .
H10 H 0.2952 -0.1461 0.5528 0.056 Uiso 1 1 calc R . . . .
N9 N 0.4453(3) -0.1300(4) 0.6222(3) 0.0443(8) Uani 1 1 d . . . . .
C9 C 0.4433(4) -0.0597(4) 0.6878(3) 0.0353(8) Uani 1 1 d . . . . .
H9 H 0.5153 -0.0520 0.7198 0.042 Uiso 1 1 calc R . . . .
C7 C 0.8028(3) -0.0044(3) 0.6929(3) 0.0165(5) Uani 1 1 d . . . . .
C6 C 0.9560(3) 0.2387(3) 0.5575(3) 0.0175(5) Uani 1 1 d . . . . .
N11 N 1.3712(6) 0.3297(6) 0.1617(6) 0.0328(15) Uani 0.7 1 d . U P A 1
C10 C 1.3784(6) 0.2651(8) 0.0796(7) 0.0568(17) Uani 0.7 1 d D U P A 1
N12 N 1.5603(10) 0.3691(12) 0.0332(11) 0.153(6) Uani 0.7 1 d . . P A 1
C11 C 1.4807(9) 0.3896(10) 0.1275(9) 0.094(3) Uani 0.7 1 d D U P A 1
N13 N 1.4886(6) 0.2720(10) 0.0103(6) 0.074(2) Uani 0.7 1 d . U P A 1
O2 O 1.4623(10) 0.1986(9) 0.0406(9) 0.032(2) Uani 0.3 1 d . U P B 2
O3 O 1.3515(11) 0.3564(10) 0.1685(10) 0.027(3) Uani 0.3 1 d . U P A 2
O1 O 1.5028(13) 0.5409(14) 0.1590(12) 0.071(3) Uani 0.3 1 d . . P C 2
O11 O 0.4824(3) 0.4777(3) 0.6718(3) 0.0570(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C5 2.137(3) . ?
Mo1 C4 2.149(3) . ?
Mo1 C1 2.148(3) . ?
Mo1 C3 2.155(3) . ?
Mo1 C2 2.146(3) . ?
Mo1 C7 2.155(3) . ?
Mo1 C6 2.168(3) . ?
N11a C10 1.428(9) . ?
N11a C11 1.279(10) . ?
N12a C11 1.374(11) . ?
C10a N13 1.285(8) . ?
N12a N13 1.484(11) . ?
Mn1 O4 2.204(3) . ?
Mn1 N7 2.175(2) 2_756 ?
Mn1 N6 2.198(3) . ?
Mn1 O5 2.234(3) . ?
Mn1 N1 2.212(3) 2_766 ?
Mn1 N11 2.333(6) . ?
Mn1 O3 2.129(10) . ?
Mn2 O7 2.248(2) . ?
Mn2 N5 2.179(2) 1_455 ?
Mn2 N8 2.231(3) . ?
Mn2 O6 2.220(3) . ?
Mn2 N3 2.190(3) 2_657 ?
Mn2 N2 2.181(3) . ?
O7 H7A 0.77(4) . ?
O7 H7B 0.77(4) . ?
O4 H4A 0.78(5) . ?
O4 H4B 0.95(5) . ?
C5 N5 1.155(4) . ?
N5 Mn2 2.179(2) 1_655 ?
C4 N4 1.151(4) . ?
N8 C8 1.311(5) . ?
N8 C9 1.361(4) . ?
O6 H6A 0.70(6) . ?
O6 H6B 0.77(6) . ?
N7 Mn1 2.175(2) 2_756 ?
N7 C7 1.154(4) . ?
N6 C6 1.156(4) . ?
O5 H5A 0.66(5) . ?
O5 H5B 0.87(5) . ?
C1 N1 1.156(4) . ?
N1 Mn1 2.212(3) 2_766 ?
C3 N3 1.156(4) . ?
N3 Mn2 2.190(3) 2_657 ?
C2 N2 1.148(4) . ?
C8 H8 0.9500 . ?
C8 N10 1.323(5) . ?
N10 H10 0.8800 . ?
N10 N9 1.361(5) . ?
N9 C9 1.308(5) . ?
C9 H9 0.9500 . ?

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
C10a N11a Mn1 122.9(4) . . ?
C11a N11a Mn1 134.9(6) . . ?
C5 Mo1 C4 144.59(11) . . ?
C5 Mo1 C1 91.27(10) . . ?
C5 Mo1 C3 71.74(10) . . ?
C5 Mo1 C2 143.44(11) . . ?
C5 Mo1 C7 91.02(10) . . ?
C5 Mo1 C6 71.61(10) . . ?
C4 Mo1 C3 143.17(11) . . ?
C4 Mo1 C7 92.02(11) . . ?
N13a C10a N11 115.8(6) . . ?
C11a N11a C10 102.1(6) . . ?
N11a C11a N12 114.8(7) . . ?
C10a N13a N12 102.2(6) . . ?
C11a N12a N13 104.4(6) . . ?
O3b Mn1 O4 87.9(3) . . ?
O3b Mn1 N7 89.8(3) . 2_756 ?
O3b Mn1 N6 174.7(3) . . ?
O3b Mn1 O5 88.3(3) . . ?
C4 Mo1 C6 73.53(11) . . ?
C1 Mo1 C4 84.17(11) . . ?
C1 Mo1 C3 90.86(11) . . ?
C1 Mo1 C7 175.93(11) . . ?
C1 Mo1 C6 92.46(10) . . ?
C3 Mo1 C6 143.26(10) . . ?
C2 Mo1 C4 71.93(12) . . ?
C2 Mo1 C1 91.98(11) . . ?
C2 Mo1 C3 71.80(10) . . ?
C2 Mo1 C7 88.18(10) . . ?
C2 Mo1 C6 144.50(11) . . ?
C7 Mo1 C3 93.04(11) . . ?
C7 Mo1 C6 85.08(10) . . ?
O4 Mn1 O5 174.03(11) . . ?
O4 Mn1 N1 89.61(11) . 2_766 ?
O4 Mn1 N11 86.33(18) . . ?
N7 Mn1 O4 96.40(10) 2_756 . ?
N7 Mn1 N6 95.37(10) 2_756 . ?
N7 Mn1 O5 88.14(10) 2_756 . ?
N7 Mn1 N1 169.56(11) 2_756 2_766 ?
N7 Mn1 N11 82.16(17) 2_756 . ?
N6 Mn1 O4 90.77(10) . . ?
N6 Mn1 O5 92.66(11) . . ?
N6 Mn1 N1 93.06(10) . 2_766 ?
N6 Mn1 N11 175.95(17) . . ?
O5 Mn1 N11 90.48(18) . . ?
N1 Mn1 O5 85.33(11) 2_766 . ?
N1 Mn1 N11 89.75(17) 2_766 . ?
O3b Mn1 N1 81.9(3) . 2_766 ?
N5 Mn2 O7 87.43(10) 1_455 . ?
N5 Mn2 N8 88.05(10) 1_455 . ?
N5 Mn2 O6 90.46(12) 1_455 . ?
N5 Mn2 N3 94.35(10) 1_455 2_657 ?
N5 Mn2 N2 171.93(11) 1_455 . ?
N8 Mn2 O7 89.54(9) . . ?
O6 Mn2 O7 88.23(12) . . ?
O6 Mn2 N8 177.37(13) . . ?
N3 Mn2 O7 173.62(11) 2_657 . ?
N3 Mn2 N8 96.64(11) 2_657 . ?
N3 Mn2 O6 85.63(13) 2_657 . ?
N2 Mn2 O7 85.16(10) . . ?
N2 Mn2 N8 88.70(11) . . ?
N2 Mn2 O6 92.50(13) . . ?
N2 Mn2 N3 93.36(10) . 2_657 ?
Mn2 O7 H7A 113(3) . . ?
Mn2 O7 H7B 109(3) . . ?
H7A O7 H7B 117(4) . . ?
Mn1 O4 H4A 128(3) . . ?
Mn1 O4 H4B 120(3) . . ?
H4A O4 H4B 106(4) . . ?
N5 C5 Mo1 179.2(2) . . ?
C5 N5 Mn2 163.7(2) . 1_655 ?
N4 C4 Mo1 178.7(3) . . ?
C8 N8 Mn2 130.3(2) . . ?
C8 N8 C9 103.2(3) . . ?
C9 N8 Mn2 126.4(2) . . ?
Mn2 O6 H6A 117(5) . . ?
Mn2 O6 H6B 108(4) . . ?
H6A O6 H6B 113(7) . . ?
C7 N7 Mn1 170.6(3) . 2_756 ?
C6 N6 Mn1 176.1(2) . . ?
Mn1 O5 H5A 119(4) . . ?
Mn1 O5 H5B 121(3) . . ?
H5A O5 H5B 110(5) . . ?
N1 C1 Mo1 176.9(3) . . ?
C1 N1 Mn1 169.3(3) . 2_766 ?
N3 C3 Mo1 179.0(3) . . ?
C3 N3 Mn2 156.7(3) . 2_657 ?
N2 C2 Mo1 179.4(3) . . ?
C2 N2 Mn2 164.4(3) . . ?
N8 C8 H8 125.0 . . ?
N8 C8 N10 110.0(3) . . ?
N10 C8 H8 125.0 . . ?
C8 N10 H10 124.9 . . ?
C8 N10 N9 110.2(3) . . ?
N9 N10 H10 124.9 . . ?
C9 N9 N10 102.2(3) . . ?
N8 C9 H9 122.8 . . ?
N9 C9 N8 114.3(3) . . ?
N9 C9 H9 122.8 . . ?
N7 C7 Mo1 177.9(3) . . ?
N6 C6 Mo1 178.3(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11a N12a N13a C10a 7.8(14) . . . . ?
N13a N12a C11a N11a -4.0(16) . . . . ?
C10a N11a C11a N12a -1.3(14) . . . . ?
C11a N11a C10a N13a 7.3(11) . . . . ?
N11a C10a N13a N12a -9.4(12) . . . . ?
Mn1 N11a C11a N12a 174.7(9) . . . . ?
Mn1 N11a C10a N13a -169.3(6) . . . . ?
Mn2 N8 C8 N10 -177.2(3) . . . . ?
Mn2 N8 C9 N9 177.4(3) . . . . ?
N8 C8 N10 N9 -1.1(5) . . . . ?
C8 N8 C9 N9 -1.3(5) . . . . ?
C8 N10 N9 C9 0.2(5) . . . . ?
N10 N9 C9 N8 0.7(5) . . . . ?
C9 N8 C8 N10 1.4(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
