# 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_a20150352_esh13_22
_database_code_depnum_ccdc_archive 'CCDC 1908371'
loop_
_audit_author_name
_audit_author_address
'Santiago Reinoso'
;Universidad Publica de Navarra
Spain
;
_audit_update_record             
;
2019-04-05 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H46 Mn3 N12 O6, C H4 O'
_chemical_formula_sum            'C41 H50 Mn3 N12 O7'
_chemical_formula_weight         987.75

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_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                   14.5962(4)
_cell_length_b                   17.2040(4)
_cell_length_c                   17.6348(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.876(3)
_cell_angle_gamma                90.00
_cell_volume                     4164.53(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6013
_cell_measurement_theta_min      4.1030
_cell_measurement_theta_max      76.3410

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.111
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2044
_exptl_absorpt_coefficient_mu    7.849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83394
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.2012
_diffrn_reflns_number            16569
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.12
_diffrn_reflns_theta_max         70.98
_reflns_number_total             4013
_reflns_number_gt                3567
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'OLEX2 (Dolomanov, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
'WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2003)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0550P)²+1.6003P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4013
_refine_ls_number_parameters     299
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0961
_refine_ls_wR_factor_gt          0.0918
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.18360(2) 0.499080(18) 0.72762(2) 0.01701(11) Uani 1 1 d . . .
Mn2 Mn 0.0000 0.42583(3) 0.7500 0.01475(13) Uani 1 2 d S . .
O1 O 0.20950(12) 0.59565(9) 0.79813(11) 0.0280(4) Uani 1 1 d . . .
C1 C 0.28225(18) 0.60666(13) 0.86468(15) 0.0256(5) Uani 1 1 d . . .
C2 C 0.2738(2) 0.65978(14) 0.92312(17) 0.0354(6) Uani 1 1 d . . .
H2 H 0.2129 0.6844 0.9150 0.042 Uiso 1 1 calc R . .
C3 C 0.3515(3) 0.67676(15) 0.99148(18) 0.0404(7) Uani 1 1 d . . .
H3 H 0.3429 0.7125 1.0296 0.048 Uiso 1 1 calc R . .
C4 C 0.4421(2) 0.64278(16) 1.00583(17) 0.0388(7) Uani 1 1 d . . .
H4 H 0.4958 0.6563 1.0523 0.047 Uiso 1 1 calc R . .
C5 C 0.4526(2) 0.58907(15) 0.95129(16) 0.0313(5) Uani 1 1 d . . .
H5 H 0.5143 0.5654 0.9607 0.038 Uiso 1 1 calc R . .
C6 C 0.37376(17) 0.56844(13) 0.88181(14) 0.0234(5) Uani 1 1 d . . .
C7 C 0.39017(17) 0.50666(13) 0.83355(14) 0.0213(5) Uani 1 1 d . . .
H7 H 0.4556 0.4896 0.8463 0.026 Uiso 1 1 calc R . .
N1 N 0.32541(13) 0.47164(11) 0.77441(11) 0.0192(4) Uani 1 1 d . . .
C8 C 0.35795(16) 0.40315(13) 0.73967(14) 0.0224(5) Uani 1 1 d . . .
H8A H 0.3748 0.3606 0.7798 0.027 Uiso 1 1 calc R . .
H8B H 0.4174 0.4168 0.7275 0.027 Uiso 1 1 calc R . .
C9 C 0.27971(16) 0.37514(13) 0.66296(14) 0.0213(5) Uani 1 1 d . . .
H9A H 0.2815 0.4076 0.6171 0.026 Uiso 1 1 calc R . .
H9B H 0.2941 0.3209 0.6520 0.026 Uiso 1 1 calc R . .
N2 N 0.18090(13) 0.37861(10) 0.66833(11) 0.0172(4) Uani 1 1 d . . .
C10 C 0.10518(17) 0.37457(13) 0.58693(13) 0.0213(5) Uani 1 1 d . . .
H10A H 0.1287 0.3441 0.5496 0.026 Uiso 1 1 calc R . .
H10B H 0.0872 0.4273 0.5643 0.026 Uiso 1 1 calc R . .
C11 C 0.01840(16) 0.33447(14) 0.60006(13) 0.0221(5) Uani 1 1 d . . .
H11A H -0.0401 0.3681 0.5818 0.026 Uiso 1 1 calc R . .
H11B H 0.0034 0.2847 0.5702 0.026 Uiso 1 1 calc R . .
N3 N 0.04934(13) 0.32064(10) 0.68885(10) 0.0168(4) Uani 1 1 d . . .
C12 C 0.15643(15) 0.31203(12) 0.71158(13) 0.0166(4) Uani 1 1 d . . .
H12 H 0.1704 0.2627 0.6876 0.020 Uiso 1 1 calc R . .
C13 C 0.21152(15) 0.31112(12) 0.80041(13) 0.0167(4) Uani 1 1 d . . .
C14 C 0.26807(16) 0.24696(13) 0.83535(14) 0.0207(4) Uani 1 1 d . . .
H14 H 0.2711 0.2038 0.8027 0.025 Uiso 1 1 calc R . .
C15 C 0.31995(17) 0.24530(13) 0.91712(14) 0.0248(5) Uani 1 1 d . . .
H15 H 0.3579 0.2011 0.9407 0.030 Uiso 1 1 calc R . .
C16 C 0.31611(17) 0.30891(14) 0.96443(14) 0.0260(5) Uani 1 1 d . . .
H16 H 0.3521 0.3081 1.0206 0.031 Uiso 1 1 calc R . .
C17 C 0.26037(16) 0.37363(13) 0.93064(13) 0.0211(5) Uani 1 1 d . . .
H17 H 0.2584 0.4168 0.9636 0.025 Uiso 1 1 calc R . .
C18 C 0.20740(15) 0.37527(12) 0.84850(13) 0.0170(4) Uani 1 1 d . . .
O2 O 0.15217(11) 0.43796(8) 0.81524(9) 0.0166(3) Uani 1 1 d . . .
C19 C 0.00145(16) 0.25042(12) 0.70739(14) 0.0213(5) Uani 1 1 d . . .
H19A H 0.0369 0.2036 0.6998 0.026 Uiso 1 1 calc R . .
H19B H -0.0660 0.2473 0.6688 0.026 Uiso 1 1 calc R . .
O1B O 0.04786(11) 0.50797(9) 0.68147(10) 0.0219(3) Uani 1 1 d . . .
C1B C -0.0054(2) 0.55623(18) 0.61869(18) 0.0404(7) Uani 1 1 d . . .
H1BA H -0.0062 0.5341 0.5672 0.061 Uiso 1 1 calc R . .
H1BB H 0.0249 0.6078 0.6258 0.061 Uiso 1 1 calc R . .
H1BC H -0.0723 0.5608 0.6188 0.061 Uiso 1 1 calc R . .
N1T N 0.20738(15) 0.54839(12) 0.63052(13) 0.0286(5) Uani 1 1 d . . .
N2T N 0.28901(16) 0.56442(12) 0.63456(13) 0.0294(5) Uani 1 1 d . . .
N3T N 0.36695(17) 0.58012(15) 0.63719(15) 0.0420(6) Uani 1 1 d . . .
C1S C -0.0044(12) 0.7175(5) 0.7627(16) 0.112(8) Uani 0.50 1 d P A -1
H1SA H 0.0405 0.7557 0.7535 0.168 Uiso 0.50 1 calc PR A -1
H1SB H 0.0227 0.6652 0.7640 0.168 Uiso 0.50 1 calc PR A -1
H1SC H -0.0132 0.7283 0.8143 0.168 Uiso 0.50 1 calc PR A -1
O1S O -0.0855(3) 0.7216(2) 0.7066(3) 0.0506(12) Uani 0.50 1 d PD A -1
H1S H -0.117(5) 0.686(4) 0.718(5) 0.076 Uiso 0.50 1 d PD B -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
Mn1 O1B 1.8748(16) . ?
Mn1 N1 2.0067(18) . ?
Mn1 O1 2.0322(18) . ?
Mn1 N1T 2.043(2) . ?
Mn1 O2 2.0460(15) . ?
Mn1 N2 2.3156(18) . ?
Mn1 Mn2 3.1056(4) . ?
Mn2 O1B 2.1259(16) . ?
Mn2 O1B 2.1259(16) 2_556 ?
Mn2 O2 2.1361(14) . ?
Mn2 O2 2.1361(14) 2_556 ?
Mn2 N3 2.3419(18) . ?
Mn2 N3 2.3419(18) 2_556 ?
Mn2 Mn1 3.1056(4) 2_556 ?
O1 C1 1.301(3) . ?
C1 C2 1.414(4) . ?
C1 C6 1.426(3) . ?
C2 C3 1.377(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.389(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.412(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.432(3) . ?
C7 N1 1.294(3) . ?
C7 H7 0.9500 . ?
N1 C8 1.479(3) . ?
C8 C9 1.522(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N2 1.478(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
N2 C12 1.486(3) . ?
N2 C10 1.486(3) . ?
C10 C11 1.528(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N3 1.494(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N3 C12 1.483(3) . ?
N3 C19 1.487(3) . ?
C12 C13 1.498(3) . ?
C12 H12 1.0000 . ?
C13 C14 1.391(3) . ?
C13 C18 1.405(3) . ?
C14 C15 1.382(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(3) . ?
C17 H17 0.9500 . ?
C18 O2 1.355(3) . ?
C19 C19 1.518(5) 2_556 ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
O1B C1B 1.391(3) . ?
C1B H1BA 0.9800 . ?
C1B H1BB 0.9800 . ?
C1B H1BC 0.9800 . ?
N1T N2T 1.201(3) . ?
N2T N3T 1.155(3) . ?
C1S O1S 1.26(2) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
O1S H1S 0.83(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
O1B Mn1 N1 171.04(7) . . ?
O1B Mn1 O1 98.52(7) . . ?
N1 Mn1 O1 89.40(7) . . ?
O1B Mn1 N1T 93.32(8) . . ?
N1 Mn1 N1T 89.82(8) . . ?
O1 Mn1 N1T 97.13(8) . . ?
O1B Mn1 O2 83.94(6) . . ?
N1 Mn1 O2 91.91(7) . . ?
O1 Mn1 O2 90.05(6) . . ?
N1T Mn1 O2 172.64(7) . . ?
O1B Mn1 N2 91.36(7) . . ?
N1 Mn1 N2 80.32(7) . . ?
O1 Mn1 N2 168.26(7) . . ?
N1T Mn1 N2 88.56(8) . . ?
O2 Mn1 N2 84.68(6) . . ?
O1B Mn1 Mn2 42.10(5) . . ?
N1 Mn1 Mn2 131.78(5) . . ?
O1 Mn1 Mn2 104.06(5) . . ?
N1T Mn1 Mn2 132.43(6) . . ?
O2 Mn1 Mn2 43.17(4) . . ?
N2 Mn1 Mn2 79.12(5) . . ?
O1B Mn2 O1B 96.68(9) . 2_556 ?
O1B Mn2 O2 76.04(6) . . ?
O1B Mn2 O2 96.39(6) 2_556 . ?
O1B Mn2 O2 96.39(6) . 2_556 ?
O1B Mn2 O2 76.04(6) 2_556 2_556 ?
O2 Mn2 O2 168.79(8) . 2_556 ?
O1B Mn2 N3 92.29(6) . . ?
O1B Mn2 N3 170.87(7) 2_556 . ?
O2 Mn2 N3 84.10(6) . . ?
O2 Mn2 N3 104.70(6) 2_556 . ?
O1B Mn2 N3 170.87(7) . 2_556 ?
O1B Mn2 N3 92.29(6) 2_556 2_556 ?
O2 Mn2 N3 104.70(6) . 2_556 ?
O2 Mn2 N3 84.10(6) 2_556 2_556 ?
N3 Mn2 N3 78.80(9) . 2_556 ?
O1B Mn2 Mn1 36.24(4) . . ?
O1B Mn2 Mn1 105.49(5) 2_556 . ?
O2 Mn2 Mn1 40.94(4) . . ?
O2 Mn2 Mn1 132.54(4) 2_556 . ?
N3 Mn2 Mn1 80.87(4) . . ?
N3 Mn2 Mn1 141.80(4) 2_556 . ?
O1B Mn2 Mn1 105.49(5) . 2_556 ?
O1B Mn2 Mn1 36.24(4) 2_556 2_556 ?
O2 Mn2 Mn1 132.54(4) . 2_556 ?
O2 Mn2 Mn1 40.94(4) 2_556 2_556 ?
N3 Mn2 Mn1 141.80(4) . 2_556 ?
N3 Mn2 Mn1 80.87(4) 2_556 2_556 ?
Mn1 Mn2 Mn1 132.119(19) . 2_556 ?
C1 O1 Mn1 126.57(14) . . ?
O1 C1 C2 120.3(2) . . ?
O1 C1 C6 122.8(2) . . ?
C2 C1 C6 116.8(2) . . ?
C3 C2 C1 121.7(3) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C2 C3 C4 121.4(2) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C5 C4 C3 118.7(3) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C4 C5 C6 121.5(3) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C1 119.8(2) . . ?
C5 C6 C7 116.8(2) . . ?
C1 C6 C7 123.4(2) . . ?
N1 C7 C6 126.9(2) . . ?
N1 C7 H7 116.5 . . ?
C6 C7 H7 116.5 . . ?
C7 N1 C8 117.10(18) . . ?
C7 N1 Mn1 126.20(16) . . ?
C8 N1 Mn1 116.66(14) . . ?
N1 C8 C9 111.78(18) . . ?
N1 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
N1 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
N2 C9 C8 112.57(18) . . ?
N2 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
N2 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C9 N2 C12 114.32(17) . . ?
C9 N2 C10 110.95(17) . . ?
C12 N2 C10 103.31(16) . . ?
C9 N2 Mn1 101.42(12) . . ?
C12 N2 Mn1 115.37(13) . . ?
C10 N2 Mn1 111.77(13) . . ?
N2 C10 C11 104.91(17) . . ?
N2 C10 H10A 110.8 . . ?
C11 C10 H10A 110.8 . . ?
N2 C10 H10B 110.8 . . ?
C11 C10 H10B 110.8 . . ?
H10A C10 H10B 108.8 . . ?
N3 C11 C10 105.08(17) . . ?
N3 C11 H11A 110.7 . . ?
C10 C11 H11A 110.7 . . ?
N3 C11 H11B 110.7 . . ?
C10 C11 H11B 110.7 . . ?
H11A C11 H11B 108.8 . . ?
C12 N3 C19 112.98(16) . . ?
C12 N3 C11 102.39(16) . . ?
C19 N3 C11 111.27(16) . . ?
C12 N3 Mn2 114.43(12) . . ?
C19 N3 Mn2 106.59(13) . . ?
C11 N3 Mn2 109.20(13) . . ?
N3 C12 N2 101.51(16) . . ?
N3 C12 C13 115.17(17) . . ?
N2 C12 C13 114.05(17) . . ?
N3 C12 H12 108.6 . . ?
N2 C12 H12 108.6 . . ?
C13 C12 H12 108.6 . . ?
C14 C13 C18 119.8(2) . . ?
C14 C13 C12 119.88(19) . . ?
C18 C13 C12 120.33(19) . . ?
C15 C14 C13 120.7(2) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 119.4(2) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C17 C16 C15 120.8(2) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C16 C17 C18 120.0(2) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
O2 C18 C17 120.34(19) . . ?
O2 C18 C13 120.33(19) . . ?
C17 C18 C13 119.3(2) . . ?
C18 O2 Mn1 118.88(13) . . ?
C18 O2 Mn2 120.81(12) . . ?
Mn1 O2 Mn2 95.88(6) . . ?
N3 C19 C19 113.03(14) . 2_556 ?
N3 C19 H19A 109.0 . . ?
C19 C19 H19A 109.0 2_556 . ?
N3 C19 H19B 109.0 . . ?
C19 C19 H19B 109.0 2_556 . ?
H19A C19 H19B 107.8 . . ?
C1B O1B Mn1 128.04(16) . . ?
C1B O1B Mn2 130.30(16) . . ?
Mn1 O1B Mn2 101.66(7) . . ?
O1B C1B H1BA 109.5 . . ?
O1B C1B H1BB 109.5 . . ?
H1BA C1B H1BB 109.5 . . ?
O1B C1B H1BC 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
N2T N1T Mn1 119.56(17) . . ?
N3T N2T N1T 179.0(3) . . ?
C1S O1S H1S 102(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1S O1 0.83(2) 2.01(4) 2.807(4) 159(8) 2_556

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        70.98
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.066

####################################################################### 
# 
# 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_a20150351_esh14_1
_database_code_depnum_ccdc_archive 'CCDC 1908372'
loop_
_audit_author_name
_audit_author_address
'Santiago Reinoso'
;Universidad Publica de Navarra
Spain
;
_audit_update_record             
;
2019-04-05 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H54 Mn3 N12 O10, C H4 O'
_chemical_formula_sum            'C45 H58 Mn3 N12 O11'
_chemical_formula_weight         1107.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   13.06284(12)
_cell_length_b                   27.2891(3)
_cell_length_c                   13.51506(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.8012(8)
_cell_angle_gamma                90.00
_cell_volume                     4812.00(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19797
_cell_measurement_theta_min      3.6250
_cell_measurement_theta_max      76.4150

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.047
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2300
_exptl_absorpt_coefficient_mu    6.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.47499
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.2012
_diffrn_reflns_number            44120
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.24
_diffrn_reflns_theta_max         71.00
_reflns_number_total             9291
_reflns_number_gt                8291
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'OLEX2 (Dolomanov, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
'WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2003)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0365P)²+2.6486P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9291
_refine_ls_number_parameters     650
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0789
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.034
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.53014(2) 0.131250(11) 0.71844(2) 0.01605(7) Uani 1 1 d . . .
Mn2 Mn 0.40892(2) 0.221502(11) 0.62853(2) 0.01330(7) Uani 1 1 d . . .
Mn3 Mn 0.31984(2) 0.318632(11) 0.71515(2) 0.01452(7) Uani 1 1 d . . .
O1 O 0.48919(12) 0.12864(5) 0.85094(10) 0.0227(3) Uani 1 1 d . . .
C1 C 0.45082(15) 0.09188(8) 0.89942(15) 0.0209(4) Uani 1 1 d . . .
C2 C 0.41536(16) 0.10092(8) 0.99593(15) 0.0238(4) Uani 1 1 d . . .
C3 C 0.36848(17) 0.06450(9) 1.04741(16) 0.0295(5) Uani 1 1 d . . .
H3 H 0.3427 0.0716 1.1103 0.035 Uiso 1 1 calc R . .
C4 C 0.35804(19) 0.01690(9) 1.00852(18) 0.0332(5) Uani 1 1 d . . .
H4 H 0.3246 -0.0078 1.0445 0.040 Uiso 1 1 calc R . .
C5 C 0.39627(18) 0.00634(8) 0.91868(17) 0.0295(5) Uani 1 1 d . . .
H5 H 0.3918 -0.0261 0.8935 0.035 Uiso 1 1 calc R . .
C6 C 0.44251(16) 0.04340(8) 0.86275(15) 0.0230(4) Uani 1 1 d . . .
C7 C 0.47895(16) 0.02986(8) 0.76794(15) 0.0223(4) Uani 1 1 d . . .
H7 H 0.4769 -0.0040 0.7515 0.027 Uiso 1 1 calc R . .
N1 N 0.51432(13) 0.05936(6) 0.70278(12) 0.0205(3) Uani 1 1 d . . .
C8 C 0.54337(17) 0.03920(8) 0.60685(15) 0.0248(4) Uani 1 1 d . . .
H8A H 0.4813 0.0343 0.5629 0.030 Uiso 1 1 calc R . .
H8B H 0.5774 0.0071 0.6172 0.030 Uiso 1 1 calc R . .
C9 C 0.61584(16) 0.07470(8) 0.55895(15) 0.0235(4) Uani 1 1 d . . .
H9A H 0.6850 0.0720 0.5918 0.028 Uiso 1 1 calc R . .
H9B H 0.6210 0.0662 0.4882 0.028 Uiso 1 1 calc R . .
N2 N 0.57777(12) 0.12619(6) 0.56763(12) 0.0183(3) Uani 1 1 d . . .
C10 C 0.66166(15) 0.16188(8) 0.54764(15) 0.0229(4) Uani 1 1 d . . .
H10A H 0.7084 0.1482 0.4992 0.027 Uiso 1 1 calc R . .
H10B H 0.7020 0.1698 0.6095 0.027 Uiso 1 1 calc R . .
C11 C 0.60739(15) 0.20751(8) 0.50573(14) 0.0203(4) Uani 1 1 d . . .
H11A H 0.6159 0.2354 0.5523 0.024 Uiso 1 1 calc R . .
H11B H 0.6349 0.2169 0.4415 0.024 Uiso 1 1 calc R . .
N3 N 0.49660(12) 0.19293(6) 0.49283(11) 0.0151(3) Uani 1 1 d . . .
C12 C 0.50044(15) 0.13878(7) 0.48579(13) 0.0173(4) Uani 1 1 d . . .
H12 H 0.5306 0.1301 0.4215 0.021 Uiso 1 1 calc R . .
C13 C 0.39805(15) 0.11438(7) 0.48861(14) 0.0170(4) Uani 1 1 d . . .
C14 C 0.35947(16) 0.08901(7) 0.40477(14) 0.0193(4) Uani 1 1 d . . .
H14 H 0.4006 0.0853 0.3492 0.023 Uiso 1 1 calc R . .
C15 C 0.26160(16) 0.06923(7) 0.40226(15) 0.0222(4) Uani 1 1 d . . .
H15 H 0.2352 0.0525 0.3448 0.027 Uiso 1 1 calc R . .
C16 C 0.20249(16) 0.07405(8) 0.48456(15) 0.0223(4) Uani 1 1 d . . .
H16 H 0.1350 0.0609 0.4828 0.027 Uiso 1 1 calc R . .
C17 C 0.24107(15) 0.09784(7) 0.56935(15) 0.0194(4) Uani 1 1 d . . .
C18 C 0.33901(14) 0.11963(7) 0.57246(14) 0.0158(4) Uani 1 1 d . . .
O2 O 0.37515(10) 0.14528(5) 0.65117(9) 0.0165(3) Uani 1 1 d . . .
C19 C 0.44760(15) 0.21539(7) 0.40256(13) 0.0181(4) Uani 1 1 d . . .
H19A H 0.4629 0.1951 0.3444 0.022 Uiso 1 1 calc R . .
H19B H 0.4775 0.2483 0.3929 0.022 Uiso 1 1 calc R . .
C20 C 0.33151(15) 0.22032(7) 0.40795(13) 0.0181(4) Uani 1 1 d . . .
H20A H 0.3038 0.2374 0.3478 0.022 Uiso 1 1 calc R . .
H20B H 0.3006 0.1872 0.4088 0.022 Uiso 1 1 calc R . .
N4 N 0.30135(12) 0.24784(6) 0.49705(11) 0.0154(3) Uani 1 1 d . . .
C21 C 0.19351(14) 0.23681(7) 0.52265(14) 0.0177(4) Uani 1 1 d . . .
H21A H 0.1921 0.2108 0.5735 0.021 Uiso 1 1 calc R . .
H21B H 0.1521 0.2261 0.4632 0.021 Uiso 1 1 calc R . .
C22 C 0.15246(14) 0.28527(7) 0.56276(14) 0.0190(4) Uani 1 1 d . . .
H22A H 0.0967 0.2983 0.5181 0.023 Uiso 1 1 calc R . .
H22B H 0.1260 0.2806 0.6295 0.023 Uiso 1 1 calc R . .
N5 N 0.24285(12) 0.31934(6) 0.56698(11) 0.0158(3) Uani 1 1 d . . .
C23 C 0.30245(14) 0.30168(7) 0.48185(13) 0.0156(4) Uani 1 1 d . . .
H23 H 0.2617 0.3091 0.4191 0.019 Uiso 1 1 calc R . .
C24 C 0.40661(14) 0.32391(7) 0.47461(14) 0.0166(4) Uani 1 1 d . . .
C25 C 0.43224(16) 0.34706(8) 0.38749(14) 0.0218(4) Uani 1 1 d . . .
H25 H 0.3827 0.3496 0.3339 0.026 Uiso 1 1 calc R . .
C26 C 0.52907(18) 0.36632(9) 0.37841(16) 0.0294(5) Uani 1 1 d . . .
H26 H 0.5469 0.3812 0.3181 0.035 Uiso 1 1 calc R . .
C27 C 0.60048(17) 0.36372(9) 0.45849(17) 0.0298(5) Uani 1 1 d . . .
H27 H 0.6670 0.3772 0.4528 0.036 Uiso 1 1 calc R . .
C28 C 0.57504(15) 0.34163(8) 0.54615(15) 0.0215(4) Uani 1 1 d . . .
C29 C 0.47763(14) 0.32047(7) 0.55584(13) 0.0160(4) Uani 1 1 d . . .
O3 O 0.45333(10) 0.29738(5) 0.63839(9) 0.0153(3) Uani 1 1 d . . .
C30 C 0.20982(15) 0.37152(7) 0.55150(14) 0.0191(4) Uani 1 1 d . . .
H30A H 0.1473 0.3779 0.5879 0.023 Uiso 1 1 calc R . .
H30B H 0.1935 0.3774 0.4802 0.023 Uiso 1 1 calc R . .
C31 C 0.29519(16) 0.40602(7) 0.58834(14) 0.0199(4) Uani 1 1 d . . .
H31A H 0.3529 0.4046 0.5436 0.024 Uiso 1 1 calc R . .
H31B H 0.2695 0.4401 0.5897 0.024 Uiso 1 1 calc R . .
N6 N 0.32981(12) 0.39044(6) 0.68891(12) 0.0177(3) Uani 1 1 d . . .
C32 C 0.34850(16) 0.42328(7) 0.75630(15) 0.0213(4) Uani 1 1 d . . .
H32 H 0.3424 0.4566 0.7364 0.026 Uiso 1 1 calc R . .
C33 C 0.37759(16) 0.41407(8) 0.85852(15) 0.0207(4) Uani 1 1 d . . .
C34 C 0.38518(18) 0.45509(8) 0.92276(16) 0.0275(5) Uani 1 1 d . . .
H34 H 0.3730 0.4871 0.8972 0.033 Uiso 1 1 calc R . .
C35 C 0.41001(17) 0.44885(8) 1.02144(16) 0.0271(5) Uani 1 1 d . . .
H35 H 0.4136 0.4764 1.0645 0.033 Uiso 1 1 calc R . .
C36 C 0.43015(16) 0.40180(8) 1.05903(15) 0.0236(4) Uani 1 1 d . . .
H36 H 0.4478 0.3977 1.1276 0.028 Uiso 1 1 calc R . .
C37 C 0.42469(15) 0.36126(8) 0.99780(14) 0.0191(4) Uani 1 1 d . . .
C38 C 0.39679(15) 0.36633(7) 0.89501(14) 0.0187(4) Uani 1 1 d . . .
O4 O 0.39133(11) 0.32647(5) 0.83996(10) 0.0208(3) Uani 1 1 d . . .
O1M O 0.43134(12) 0.14770(6) 1.02860(11) 0.0271(3) Uani 1 1 d . . .
C1M C 0.40419(18) 0.15790(10) 1.12759(16) 0.0322(5) Uani 1 1 d . . .
H1MA H 0.3300 0.1541 1.1324 0.048 Uiso 1 1 calc R . .
H1MB H 0.4239 0.1916 1.1450 0.048 Uiso 1 1 calc R . .
H1MC H 0.4400 0.1350 1.1733 0.048 Uiso 1 1 calc R . .
O2M O 0.17959(11) 0.10051(6) 0.64943(11) 0.0242(3) Uani 1 1 d . . .
C2M C 0.22401(17) 0.07678(9) 0.73638(16) 0.0276(5) Uani 1 1 d . . .
H2MA H 0.2649 0.0486 0.7166 0.041 Uiso 1 1 calc R . .
H2MB H 0.1693 0.0655 0.7780 0.041 Uiso 1 1 calc R . .
H2MC H 0.2681 0.1000 0.7738 0.041 Uiso 1 1 calc R . .
O3M O 0.64868(11) 0.33800(6) 0.62279(11) 0.0282(3) Uani 1 1 d . . .
C3M C 0.62440(19) 0.36454(9) 0.71083(17) 0.0337(5) Uani 1 1 d . . .
H3MA H 0.6134 0.3992 0.6944 0.051 Uiso 1 1 calc R . .
H3MB H 0.6813 0.3616 0.7605 0.051 Uiso 1 1 calc R . .
H3MC H 0.5620 0.3509 0.7375 0.051 Uiso 1 1 calc R . .
O4M O 0.44351(12) 0.31425(5) 1.02784(10) 0.0247(3) Uani 1 1 d . . .
C4M C 0.4662(2) 0.30783(9) 1.13128(15) 0.0308(5) Uani 1 1 d . . .
H4MA H 0.5268 0.3272 1.1515 0.046 Uiso 1 1 calc R . .
H4MB H 0.4795 0.2731 1.1452 0.046 Uiso 1 1 calc R . .
H4MC H 0.4077 0.3188 1.1683 0.046 Uiso 1 1 calc R . .
O1B O 0.53784(10) 0.19965(5) 0.71680(9) 0.0178(3) Uani 1 1 d . . .
C1B C 0.57606(19) 0.22800(8) 0.79776(16) 0.0294(5) Uani 1 1 d . . .
H1BA H 0.5337 0.2226 0.8546 0.044 Uiso 1 1 calc R . .
H1BB H 0.5741 0.2628 0.7796 0.044 Uiso 1 1 calc R . .
H1BC H 0.6469 0.2183 0.8152 0.044 Uiso 1 1 calc R . .
O2B O 0.30458(10) 0.25061(5) 0.72823(9) 0.0169(3) Uani 1 1 d . . .
C2B C 0.2754(2) 0.22706(8) 0.81622(16) 0.0298(5) Uani 1 1 d . . .
H2BA H 0.3026 0.2454 0.8740 0.045 Uiso 1 1 calc R . .
H2BB H 0.3029 0.1936 0.8184 0.045 Uiso 1 1 calc R . .
H2BC H 0.2004 0.2258 0.8170 0.045 Uiso 1 1 calc R . .
N1T N 0.69451(14) 0.12193(7) 0.76692(14) 0.0277(4) Uani 1 1 d . . .
N2T N 0.73117(15) 0.08253(8) 0.78058(14) 0.0297(4) Uani 1 1 d . . .
N3T N 0.7670(2) 0.04365(10) 0.7925(2) 0.0526(6) Uani 1 1 d . . .
N4T N 0.16681(13) 0.33531(6) 0.77441(12) 0.0214(3) Uani 1 1 d . . .
N5T N 0.13463(13) 0.37630(7) 0.77611(12) 0.0216(4) Uani 1 1 d . . .
N6T N 0.10247(16) 0.41621(7) 0.77824(15) 0.0311(4) Uani 1 1 d . . .
O1S O 0.5266(2) 0.50814(13) 0.7228(2) 0.0879(10) Uani 1 1 d D . .
C1S C 0.5119(3) 0.50086(15) 0.6215(3) 0.0742(11) Uani 1 1 d . . .
H1SA H 0.4398 0.5068 0.6015 0.111 Uiso 1 1 calc R . .
H1SB H 0.5301 0.4671 0.6052 0.111 Uiso 1 1 calc R . .
H1SC H 0.5554 0.5236 0.5862 0.111 Uiso 1 1 calc R . .
H1S H 0.593(2) 0.5200(18) 0.740(3) 0.111 Uiso 1 1 d 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
Mn1 O1B 1.8695(14) . ?
Mn1 O1 1.8952(14) . ?
Mn1 N1 1.9829(17) . ?
Mn1 N2 2.1642(16) . ?
Mn1 O2 2.2118(13) . ?
Mn1 N1T 2.2286(18) . ?
Mn1 Mn2 3.1403(4) . ?
Mn2 O1B 2.1021(13) . ?
Mn2 O2B 2.1174(13) . ?
Mn2 O2 2.1512(14) . ?
Mn2 O3 2.1527(13) . ?
Mn2 N4 2.3247(15) . ?
Mn2 N3 2.3429(15) . ?
Mn2 Mn3 3.1438(4) . ?
Mn3 O2B 1.8762(14) . ?
Mn3 O4 1.8998(14) . ?
Mn3 N6 1.9968(17) . ?
Mn3 O3 2.1519(13) . ?
Mn3 N5 2.1966(15) . ?
Mn3 N4T 2.2363(17) . ?
O1 C1 1.311(3) . ?
C1 C6 1.415(3) . ?
C1 C2 1.427(3) . ?
C2 O1M 1.363(3) . ?
C2 C3 1.374(3) . ?
C3 C4 1.405(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.366(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.415(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.437(3) . ?
C7 N1 1.295(3) . ?
C7 H7 0.9500 . ?
N1 C8 1.475(3) . ?
C8 C9 1.521(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N2 1.497(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
N2 C10 1.501(3) . ?
N2 C12 1.501(2) . ?
C10 C11 1.528(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N3 1.503(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N3 C12 1.482(2) . ?
N3 C19 1.482(2) . ?
C12 C13 1.496(3) . ?
C12 H12 1.0000 . ?
C13 C14 1.401(3) . ?
C13 C18 1.409(3) . ?
C14 C15 1.387(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.391(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.390(3) . ?
C16 H16 0.9500 . ?
C17 O2M 1.381(3) . ?
C17 C18 1.410(3) . ?
C18 O2 1.340(2) . ?
C19 C20 1.528(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 N4 1.489(2) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
N4 C23 1.484(2) . ?
N4 C21 1.498(2) . ?
C21 C22 1.536(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N5 1.502(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
N5 C30 1.500(2) . ?
N5 C23 1.500(2) . ?
C23 C24 1.497(3) . ?
C23 H23 1.0000 . ?
C24 C25 1.391(3) . ?
C24 C29 1.405(3) . ?
C25 C26 1.381(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.396(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.384(3) . ?
C27 H27 0.9500 . ?
C28 O3M 1.382(2) . ?
C28 C29 1.409(3) . ?
C29 O3 1.333(2) . ?
C30 C31 1.524(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 N6 1.474(2) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
N6 C32 1.292(3) . ?
C32 C33 1.437(3) . ?
C32 H32 0.9500 . ?
C33 C38 1.411(3) . ?
C33 C34 1.417(3) . ?
C34 C35 1.368(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.401(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.381(3) . ?
C36 H36 0.9500 . ?
C37 O4M 1.364(3) . ?
C37 C38 1.426(3) . ?
C38 O4 1.318(2) . ?
O1M C1M 1.428(3) . ?
C1M H1MA 0.9800 . ?
C1M H1MB 0.9800 . ?
C1M H1MC 0.9800 . ?
O2M C2M 1.439(3) . ?
C2M H2MA 0.9800 . ?
C2M H2MB 0.9800 . ?
C2M H2MC 0.9800 . ?
O3M C3M 1.441(3) . ?
C3M H3MA 0.9800 . ?
C3M H3MB 0.9800 . ?
C3M H3MC 0.9800 . ?
O4M C4M 1.426(2) . ?
C4M H4MA 0.9800 . ?
C4M H4MB 0.9800 . ?
C4M H4MC 0.9800 . ?
O1B C1B 1.411(2) . ?
C1B H1BA 0.9800 . ?
C1B H1BB 0.9800 . ?
C1B H1BC 0.9800 . ?
O2B C2B 1.420(2) . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
N1T N2T 1.188(3) . ?
N2T N3T 1.168(3) . ?
N4T N5T 1.195(3) . ?
N5T N6T 1.168(3) . ?
O1S C1S 1.388(5) . ?
O1S H1S 0.946(19) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?

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
O1B Mn1 O1 93.81(6) . . ?
O1B Mn1 N1 172.73(6) . . ?
O1 Mn1 N1 91.77(7) . . ?
O1B Mn1 N2 91.97(6) . . ?
O1 Mn1 N2 174.18(6) . . ?
N1 Mn1 N2 82.51(7) . . ?
O1B Mn1 O2 82.59(5) . . ?
O1 Mn1 O2 95.73(6) . . ?
N1 Mn1 O2 92.23(6) . . ?
N2 Mn1 O2 85.61(5) . . ?
O1B Mn1 N1T 93.77(7) . . ?
O1 Mn1 N1T 91.74(7) . . ?
N1 Mn1 N1T 90.71(7) . . ?
N2 Mn1 N1T 87.27(7) . . ?
O2 Mn1 N1T 171.88(6) . . ?
O1B Mn1 Mn2 40.43(4) . . ?
O1 Mn1 Mn2 103.58(5) . . ?
N1 Mn1 Mn2 133.37(5) . . ?
N2 Mn1 Mn2 81.28(4) . . ?
O2 Mn1 Mn2 43.20(4) . . ?
N1T Mn1 Mn2 131.57(5) . . ?
O1B Mn2 O2B 105.55(5) . . ?
O1B Mn2 O2 79.00(5) . . ?
O2B Mn2 O2 97.44(5) . . ?
O1B Mn2 O3 91.81(5) . . ?
O2B Mn2 O3 77.27(5) . . ?
O2 Mn2 O3 167.88(5) . . ?
O1B Mn2 N4 163.54(6) . . ?
O2B Mn2 N4 89.23(5) . . ?
O2 Mn2 N4 106.69(5) . . ?
O3 Mn2 N4 84.31(5) . . ?
O1B Mn2 N3 86.62(5) . . ?
O2B Mn2 N3 167.83(5) . . ?
O2 Mn2 N3 84.32(5) . . ?
O3 Mn2 N3 103.18(5) . . ?
N4 Mn2 N3 78.75(5) . . ?
O1B Mn2 Mn1 35.22(4) . . ?
O2B Mn2 Mn1 112.09(4) . . ?
O2 Mn2 Mn1 44.74(4) . . ?
O3 Mn2 Mn1 126.95(4) . . ?
N4 Mn2 Mn1 144.37(4) . . ?
N3 Mn2 Mn1 77.60(4) . . ?
O1B Mn2 Mn3 109.19(4) . . ?
O2B Mn2 Mn3 35.44(4) . . ?
O2 Mn2 Mn3 132.85(4) . . ?
O3 Mn2 Mn3 43.08(3) . . ?
N4 Mn2 Mn3 78.64(4) . . ?
N3 Mn2 Mn3 140.91(4) . . ?
Mn1 Mn2 Mn3 134.909(12) . . ?
O2B Mn3 O4 94.45(6) . . ?
O2B Mn3 N6 174.76(6) . . ?
O4 Mn3 N6 90.78(6) . . ?
O2B Mn3 O3 82.59(5) . . ?
O4 Mn3 O3 94.80(6) . . ?
N6 Mn3 O3 96.75(6) . . ?
O2B Mn3 N5 92.79(6) . . ?
O4 Mn3 N5 172.62(6) . . ?
N6 Mn3 N5 81.97(6) . . ?
O3 Mn3 N5 84.76(5) . . ?
O2B Mn3 N4T 93.83(6) . . ?
O4 Mn3 N4T 93.92(6) . . ?
N6 Mn3 N4T 86.05(6) . . ?
O3 Mn3 N4T 170.81(6) . . ?
N5 Mn3 N4T 86.98(6) . . ?
O2B Mn3 Mn2 40.87(4) . . ?
O4 Mn3 Mn2 104.52(4) . . ?
N6 Mn3 Mn2 137.12(5) . . ?
O3 Mn3 Mn2 43.10(4) . . ?
N5 Mn3 Mn2 80.17(4) . . ?
N4T Mn3 Mn2 131.19(5) . . ?
C1 O1 Mn1 129.30(13) . . ?
O1 C1 C6 124.40(19) . . ?
O1 C1 C2 118.27(19) . . ?
C6 C1 C2 117.33(19) . . ?
O1M C2 C3 125.3(2) . . ?
O1M C2 C1 113.99(19) . . ?
C3 C2 C1 120.7(2) . . ?
C2 C3 C4 121.1(2) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 119.6(2) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.5(2) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 120.6(2) . . ?
C1 C6 C7 121.98(19) . . ?
C5 C6 C7 117.5(2) . . ?
N1 C7 C6 126.26(19) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
C7 N1 C8 118.79(18) . . ?
C7 N1 Mn1 125.54(14) . . ?
C8 N1 Mn1 115.65(13) . . ?
N1 C8 C9 109.19(17) . . ?
N1 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
N1 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
N2 C9 C8 110.39(16) . . ?
N2 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
N2 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
C9 N2 C10 110.29(16) . . ?
C9 N2 C12 111.80(15) . . ?
C10 N2 C12 100.95(15) . . ?
C9 N2 Mn1 104.22(12) . . ?
C10 N2 Mn1 111.98(12) . . ?
C12 N2 Mn1 117.73(12) . . ?
N2 C10 C11 105.43(15) . . ?
N2 C10 H10A 110.7 . . ?
C11 C10 H10A 110.7 . . ?
N2 C10 H10B 110.7 . . ?
C11 C10 H10B 110.7 . . ?
H10A C10 H10B 108.8 . . ?
N3 C11 C10 104.70(16) . . ?
N3 C11 H11A 110.8 . . ?
C10 C11 H11A 110.8 . . ?
N3 C11 H11B 110.8 . . ?
C10 C11 H11B 110.8 . . ?
H11A C11 H11B 108.9 . . ?
C12 N3 C19 111.97(14) . . ?
C12 N3 C11 103.67(14) . . ?
C19 N3 C11 111.14(15) . . ?
C12 N3 Mn2 113.67(11) . . ?
C19 N3 Mn2 107.37(11) . . ?
C11 N3 Mn2 109.02(11) . . ?
N3 C12 C13 114.15(15) . . ?
N3 C12 N2 101.81(14) . . ?
C13 C12 N2 116.72(16) . . ?
N3 C12 H12 107.9 . . ?
C13 C12 H12 107.9 . . ?
N2 C12 H12 107.9 . . ?
C14 C13 C18 120.76(18) . . ?
C14 C13 C12 119.09(17) . . ?
C18 C13 C12 120.03(17) . . ?
C15 C14 C13 120.47(19) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 119.39(18) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C17 C16 C15 120.69(19) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
O2M C17 C16 118.00(18) . . ?
O2M C17 C18 121.08(17) . . ?
C16 C17 C18 120.90(19) . . ?
O2 C18 C13 120.41(17) . . ?
O2 C18 C17 121.88(17) . . ?
C13 C18 C17 117.71(17) . . ?
C18 O2 Mn2 117.32(11) . . ?
C18 O2 Mn1 121.05(11) . . ?
Mn2 O2 Mn1 92.06(5) . . ?
N3 C19 C20 112.76(15) . . ?
N3 C19 H19A 109.0 . . ?
C20 C19 H19A 109.0 . . ?
N3 C19 H19B 109.0 . . ?
C20 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
N4 C20 C19 112.67(15) . . ?
N4 C20 H20A 109.1 . . ?
C19 C20 H20A 109.1 . . ?
N4 C20 H20B 109.1 . . ?
C19 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
C23 N4 C20 112.51(15) . . ?
C23 N4 C21 104.28(14) . . ?
C20 N4 C21 111.99(14) . . ?
C23 N4 Mn2 113.73(11) . . ?
C20 N4 Mn2 106.76(11) . . ?
C21 N4 Mn2 107.55(11) . . ?
N4 C21 C22 104.89(15) . . ?
N4 C21 H21A 110.8 . . ?
C22 C21 H21A 110.8 . . ?
N4 C21 H21B 110.8 . . ?
C22 C21 H21B 110.8 . . ?
H21A C21 H21B 108.8 . . ?
N5 C22 C21 105.02(15) . . ?
N5 C22 H22A 110.7 . . ?
C21 C22 H22A 110.7 . . ?
N5 C22 H22B 110.7 . . ?
C21 C22 H22B 110.7 . . ?
H22A C22 H22B 108.8 . . ?
C30 N5 C23 110.78(14) . . ?
C30 N5 C22 111.24(15) . . ?
C23 N5 C22 102.04(14) . . ?
C30 N5 Mn3 104.56(11) . . ?
C23 N5 Mn3 117.69(11) . . ?
C22 N5 Mn3 110.69(11) . . ?
N4 C23 C24 115.16(15) . . ?
N4 C23 N5 101.72(14) . . ?
C24 C23 N5 115.30(15) . . ?
N4 C23 H23 108.1 . . ?
C24 C23 H23 108.1 . . ?
N5 C23 H23 108.1 . . ?
C25 C24 C29 120.96(18) . . ?
C25 C24 C23 119.75(17) . . ?
C29 C24 C23 119.29(17) . . ?
C26 C25 C24 120.49(19) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 119.5(2) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
C28 C27 C26 120.4(2) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
O3M C28 C27 119.03(19) . . ?
O3M C28 C29 119.97(18) . . ?
C27 C28 C29 120.90(18) . . ?
O3 C29 C24 120.68(17) . . ?
O3 C29 C28 121.63(17) . . ?
C24 C29 C28 117.69(17) . . ?
C29 O3 Mn3 120.51(11) . . ?
C29 O3 Mn2 118.51(11) . . ?
Mn3 O3 Mn2 93.83(5) . . ?
N5 C30 C31 109.87(15) . . ?
N5 C30 H30A 109.7 . . ?
C31 C30 H30A 109.7 . . ?
N5 C30 H30B 109.7 . . ?
C31 C30 H30B 109.7 . . ?
H30A C30 H30B 108.2 . . ?
N6 C31 C30 108.04(15) . . ?
N6 C31 H31A 110.1 . . ?
C30 C31 H31A 110.1 . . ?
N6 C31 H31B 110.1 . . ?
C30 C31 H31B 110.1 . . ?
H31A C31 H31B 108.4 . . ?
C32 N6 C31 119.25(17) . . ?
C32 N6 Mn3 124.54(14) . . ?
C31 N6 Mn3 115.28(12) . . ?
N6 C32 C33 126.03(19) . . ?
N6 C32 H32 117.0 . . ?
C33 C32 H32 117.0 . . ?
C38 C33 C34 120.61(19) . . ?
C38 C33 C32 122.12(18) . . ?
C34 C33 C32 117.27(19) . . ?
C35 C34 C33 120.3(2) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C35 C36 119.95(19) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.0 . . ?
C37 C36 C35 120.89(19) . . ?
C37 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
O4M C37 C36 124.86(18) . . ?
O4M C37 C38 114.52(17) . . ?
C36 C37 C38 120.62(19) . . ?
O4 C38 C33 124.12(18) . . ?
O4 C38 C37 118.32(18) . . ?
C33 C38 C37 117.56(18) . . ?
C38 O4 Mn3 127.23(13) . . ?
C2 O1M C1M 116.41(18) . . ?
O1M C1M H1MA 109.5 . . ?
O1M C1M H1MB 109.5 . . ?
H1MA C1M H1MB 109.5 . . ?
O1M C1M H1MC 109.5 . . ?
H1MA C1M H1MC 109.5 . . ?
H1MB C1M H1MC 109.5 . . ?
C17 O2M C2M 112.93(15) . . ?
O2M C2M H2MA 109.5 . . ?
O2M C2M H2MB 109.5 . . ?
H2MA C2M H2MB 109.5 . . ?
O2M C2M H2MC 109.5 . . ?
H2MA C2M H2MC 109.5 . . ?
H2MB C2M H2MC 109.5 . . ?
C28 O3M C3M 114.16(17) . . ?
O3M C3M H3MA 109.5 . . ?
O3M C3M H3MB 109.5 . . ?
H3MA C3M H3MB 109.5 . . ?
O3M C3M H3MC 109.5 . . ?
H3MA C3M H3MC 109.5 . . ?
H3MB C3M H3MC 109.5 . . ?
C37 O4M C4M 115.66(16) . . ?
O4M C4M H4MA 109.5 . . ?
O4M C4M H4MB 109.5 . . ?
H4MA C4M H4MB 109.5 . . ?
O4M C4M H4MC 109.5 . . ?
H4MA C4M H4MC 109.5 . . ?
H4MB C4M H4MC 109.5 . . ?
C1B O1B Mn1 123.73(12) . . ?
C1B O1B Mn2 121.86(12) . . ?
Mn1 O1B Mn2 104.35(6) . . ?
O1B C1B H1BA 109.5 . . ?
O1B C1B H1BB 109.5 . . ?
H1BA C1B H1BB 109.5 . . ?
O1B C1B H1BC 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
C2B O2B Mn3 124.10(12) . . ?
C2B O2B Mn2 124.80(12) . . ?
Mn3 O2B Mn2 103.69(6) . . ?
O2B C2B H2BA 109.5 . . ?
O2B C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
O2B C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
N2T N1T Mn1 121.62(16) . . ?
N3T N2T N1T 179.0(3) . . ?
N5T N4T Mn3 121.24(14) . . ?
N6T N5T N4T 179.4(2) . . ?
C1S O1S H1S 112(3) . . ?
O1S C1S H1SA 109.5 . . ?
O1S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
O1S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1S N3T 0.946(19) 2.00(3) 2.882(4) 154(4) 2_656

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        71.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.053

####################################################################### 
# 
# 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_a20160412esh141_ta
_database_code_depnum_ccdc_archive 'CCDC 1908373'
loop_
_audit_author_name
_audit_author_address
'Santiago Reinoso'
;Universidad Publica de Navarra
Spain
;
_audit_update_record             
;
2019-04-05 deposited with the CCDC.	2019-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H54 Mn3 N12 O10, C H4 O'
_chemical_formula_sum            'C45 H58 Mn3 N12 O11'
_chemical_formula_weight         1107.85

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   13.1976(3)
_cell_length_b                   27.4846(6)
_cell_length_c                   13.6058(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.0647(18)
_cell_angle_gamma                90.00
_cell_volume                     4928.19(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13380
_cell_measurement_theta_min      3.0400
_cell_measurement_theta_max      26.8100

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.515
_exptl_crystal_size_mid          0.213
_exptl_crystal_size_min          0.113
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2300
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77407
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'micro-focus sealed X-ray tube'
_diffrn_radiation_source_type    'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2439
_diffrn_reflns_number            38440
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.66
_diffrn_reflns_theta_max         25.25
_reflns_number_total             8915
_reflns_number_gt                7321
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_structure_solution    'OLEX2 (Dolomanov, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
'WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2003)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0310P)²+4.2997P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8915
_refine_ls_number_parameters     648
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.0996
_refine_ls_wR_factor_gt          0.0933
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.52816(3) 0.131049(15) 0.71711(3) 0.03646(12) Uani 1 1 d . . .
Mn2 Mn 0.40658(3) 0.221083(15) 0.62928(3) 0.02974(11) Uani 1 1 d . . .
Mn3 Mn 0.31637(3) 0.317477(15) 0.71466(3) 0.03321(12) Uani 1 1 d . . .
O1 O 0.48809(18) 0.12829(7) 0.84844(16) 0.0503(6) Uani 1 1 d . . .
C1 C 0.4494(2) 0.09199(12) 0.8961(2) 0.0447(8) Uani 1 1 d . . .
C2 C 0.4131(3) 0.10109(13) 0.9907(3) 0.0524(9) Uani 1 1 d . . .
C3 C 0.3681(3) 0.06454(16) 1.0426(3) 0.0680(11) Uani 1 1 d . . .
H3 H 0.3434 0.0712 1.1038 0.082 Uiso 1 1 calc R . .
C4 C 0.3594(3) 0.01763(16) 1.0037(4) 0.0785(12) Uani 1 1 d . . .
H4 H 0.3273 -0.0066 1.0384 0.094 Uiso 1 1 calc R . .
C5 C 0.3975(3) 0.00729(14) 0.9159(3) 0.0681(11) Uani 1 1 d . . .
H5 H 0.3942 -0.0244 0.8921 0.082 Uiso 1 1 calc R . .
C6 C 0.4422(3) 0.04385(12) 0.8599(3) 0.0489(8) Uani 1 1 d . . .
C7 C 0.4779(3) 0.03065(11) 0.7660(3) 0.0499(8) Uani 1 1 d . . .
H7 H 0.4763 -0.0023 0.7500 0.060 Uiso 1 1 calc R . .
N1 N 0.51197(19) 0.05979(9) 0.70154(19) 0.0429(6) Uani 1 1 d . . .
C8 C 0.5406(3) 0.03977(12) 0.6061(2) 0.0544(9) Uani 1 1 d . . .
H8A H 0.4802 0.0347 0.5635 0.065 Uiso 1 1 calc R . .
H8B H 0.5741 0.0086 0.6163 0.065 Uiso 1 1 calc R . .
C9 C 0.6105(3) 0.07458(12) 0.5584(3) 0.0521(9) Uani 1 1 d . . .
H9A H 0.6147 0.0661 0.4895 0.063 Uiso 1 1 calc R . .
H9B H 0.6780 0.0719 0.5898 0.063 Uiso 1 1 calc R . .
N2 N 0.57346(17) 0.12599(9) 0.56649(18) 0.0368(6) Uani 1 1 d . . .
C10 C 0.6561(2) 0.16121(12) 0.5462(3) 0.0501(8) Uani 1 1 d . . .
H10A H 0.7011 0.1477 0.4992 0.060 Uiso 1 1 calc R . .
H10B H 0.6954 0.1691 0.6063 0.060 Uiso 1 1 calc R . .
C11 C 0.6022(2) 0.20636(12) 0.5040(2) 0.0430(7) Uani 1 1 d . . .
H11A H 0.6114 0.2337 0.5486 0.052 Uiso 1 1 calc R . .
H11B H 0.6281 0.2151 0.4410 0.052 Uiso 1 1 calc R . .
N3 N 0.49277(17) 0.19226(8) 0.49249(16) 0.0323(5) Uani 1 1 d . . .
C12 C 0.4959(2) 0.13842(10) 0.4858(2) 0.0346(6) Uani 1 1 d . . .
H12 H 0.5242 0.1298 0.4230 0.041 Uiso 1 1 calc R . .
C13 C 0.3946(2) 0.11433(10) 0.4895(2) 0.0345(6) Uani 1 1 d . . .
C14 C 0.3552(2) 0.08862(10) 0.4075(2) 0.0427(7) Uani 1 1 d . . .
H14 H 0.3943 0.0847 0.3532 0.051 Uiso 1 1 calc R . .
C15 C 0.2594(3) 0.06914(11) 0.4063(3) 0.0522(9) Uani 1 1 d . . .
H15 H 0.2333 0.0523 0.3513 0.063 Uiso 1 1 calc R . .
C16 C 0.2021(3) 0.07479(12) 0.4878(3) 0.0520(9) Uani 1 1 d . . .
H16 H 0.1367 0.0622 0.4866 0.062 Uiso 1 1 calc R . .
C17 C 0.2405(2) 0.09882(11) 0.5709(2) 0.0421(7) Uani 1 1 d . . .
C18 C 0.3379(2) 0.12006(10) 0.5726(2) 0.0334(6) Uani 1 1 d . . .
O2 O 0.37399(14) 0.14557(7) 0.65061(13) 0.0338(4) Uani 1 1 d . . .
C19 C 0.4426(2) 0.21452(11) 0.4031(2) 0.0376(7) Uani 1 1 d . . .
H19A H 0.4564 0.1947 0.3463 0.045 Uiso 1 1 calc R . .
H19B H 0.4715 0.2465 0.3932 0.045 Uiso 1 1 calc R . .
C20 C 0.3285(2) 0.21944(11) 0.4096(2) 0.0397(7) Uani 1 1 d . . .
H20A H 0.3008 0.2358 0.3510 0.048 Uiso 1 1 calc R . .
H20B H 0.2987 0.1872 0.4109 0.048 Uiso 1 1 calc R . .
N4 N 0.29915(16) 0.24681(8) 0.49752(16) 0.0312(5) Uani 1 1 d . . .
C21 C 0.1927(2) 0.23629(11) 0.5220(2) 0.0391(7) Uani 1 1 d . . .
H21A H 0.1909 0.2110 0.5716 0.047 Uiso 1 1 calc R . .
H21B H 0.1528 0.2258 0.4639 0.047 Uiso 1 1 calc R . .
C22 C 0.1518(2) 0.28422(11) 0.5611(2) 0.0408(7) Uani 1 1 d . . .
H22A H 0.0979 0.2969 0.5170 0.049 Uiso 1 1 calc R . .
H22B H 0.1258 0.2797 0.6258 0.049 Uiso 1 1 calc R . .
N5 N 0.24098(16) 0.31795(8) 0.56598(17) 0.0324(5) Uani 1 1 d . . .
C23 C 0.3007(2) 0.30020(10) 0.4821(2) 0.0328(6) Uani 1 1 d . . .
H23 H 0.2617 0.3074 0.4206 0.039 Uiso 1 1 calc R . .
C24 C 0.4034(2) 0.32239(10) 0.4763(2) 0.0334(6) Uani 1 1 d . . .
C25 C 0.4286(3) 0.34523(12) 0.3901(2) 0.0478(8) Uani 1 1 d . . .
H25 H 0.3809 0.3476 0.3374 0.057 Uiso 1 1 calc R . .
C26 C 0.5240(3) 0.36439(15) 0.3825(3) 0.0685(11) Uani 1 1 d . . .
H26 H 0.5413 0.3791 0.3242 0.082 Uiso 1 1 calc R . .
C27 C 0.5942(3) 0.36187(15) 0.4613(3) 0.0679(11) Uani 1 1 d . . .
H27 H 0.6587 0.3749 0.4558 0.081 Uiso 1 1 calc R . .
C28 C 0.5693(2) 0.34025(12) 0.5478(2) 0.0466(8) Uani 1 1 d . . .
C29 C 0.4736(2) 0.31921(10) 0.5571(2) 0.0326(6) Uani 1 1 d . . .
O3 O 0.44867(14) 0.29669(7) 0.63915(13) 0.0323(4) Uani 1 1 d . . .
C30 C 0.2085(2) 0.36977(10) 0.5504(2) 0.0414(7) Uani 1 1 d . . .
H30A H 0.1472 0.3758 0.5847 0.050 Uiso 1 1 calc R . .
H30B H 0.1936 0.3755 0.4808 0.050 Uiso 1 1 calc R . .
C31 C 0.2911(2) 0.40408(11) 0.5881(2) 0.0445(8) Uani 1 1 d . . .
H31A H 0.3475 0.4032 0.5453 0.053 Uiso 1 1 calc R . .
H31B H 0.2654 0.4371 0.5894 0.053 Uiso 1 1 calc R . .
N6 N 0.32532(18) 0.38861(8) 0.68850(18) 0.0376(6) Uani 1 1 d . . .
C32 C 0.3434(2) 0.42102(11) 0.7551(2) 0.0469(8) Uani 1 1 d . . .
H32 H 0.3368 0.4533 0.7355 0.056 Uiso 1 1 calc R . .
C33 C 0.3728(2) 0.41260(11) 0.8563(2) 0.0455(8) Uani 1 1 d . . .
C34 C 0.3804(3) 0.45313(13) 0.9200(3) 0.0636(10) Uani 1 1 d . . .
H34 H 0.3682 0.4842 0.8948 0.076 Uiso 1 1 calc R . .
C35 C 0.4051(3) 0.44745(13) 1.0174(3) 0.0666(11) Uani 1 1 d . . .
H35 H 0.4087 0.4744 1.0587 0.080 Uiso 1 1 calc R . .
C36 C 0.4250(3) 0.40112(13) 1.0554(3) 0.0553(9) Uani 1 1 d . . .
H36 H 0.4423 0.3974 1.1221 0.066 Uiso 1 1 calc R . .
C37 C 0.4193(2) 0.36092(12) 0.9954(2) 0.0444(8) Uani 1 1 d . . .
C38 C 0.3919(2) 0.36548(11) 0.8936(2) 0.0399(7) Uani 1 1 d . . .
O4 O 0.38647(17) 0.32594(7) 0.83913(15) 0.0474(5) Uani 1 1 d . . .
O1M O 0.4277(2) 0.14777(10) 1.02293(19) 0.0671(7) Uani 1 1 d . . .
C1M C 0.3962(3) 0.15941(19) 1.1177(3) 0.0920(16) Uani 1 1 d . . .
H1M1 H 0.3242 0.1546 1.1195 0.138 Uiso 1 1 calc R . .
H1M2 H 0.4123 0.1928 1.1323 0.138 Uiso 1 1 calc R . .
H1M3 H 0.4305 0.1387 1.1655 0.138 Uiso 1 1 calc R . .
O2M O 0.17975(16) 0.10310(9) 0.64972(18) 0.0561(6) Uani 1 1 d . . .
C2M C 0.2202(3) 0.07998(15) 0.7364(3) 0.0689(11) Uani 1 1 d . . .
H2M1 H 0.2581 0.0517 0.7188 0.103 Uiso 1 1 calc R . .
H2M2 H 0.1658 0.0704 0.7763 0.103 Uiso 1 1 calc R . .
H2M3 H 0.2641 0.1022 0.7727 0.103 Uiso 1 1 calc R . .
O3M O 0.64212(17) 0.33665(10) 0.62464(18) 0.0629(7) Uani 1 1 d . . .
C3M C 0.6202(3) 0.36281(16) 0.7112(3) 0.0797(13) Uani 1 1 d . . .
H3M1 H 0.6109 0.3966 0.6954 0.120 Uiso 1 1 calc R . .
H3M2 H 0.6756 0.3593 0.7593 0.120 Uiso 1 1 calc R . .
H3M3 H 0.5593 0.3502 0.7372 0.120 Uiso 1 1 calc R . .
O4M O 0.4377(2) 0.31440(8) 1.02667(17) 0.0602(7) Uani 1 1 d . . .
C4M C 0.4587(4) 0.30815(15) 1.1286(3) 0.0765(12) Uani 1 1 d . . .
H4M1 H 0.5194 0.3256 1.1485 0.115 Uiso 1 1 calc R . .
H4M2 H 0.4680 0.2742 1.1429 0.115 Uiso 1 1 calc R . .
H4M3 H 0.4031 0.3204 1.1639 0.115 Uiso 1 1 calc R . .
O1B O 0.53473(14) 0.19890(7) 0.71578(14) 0.0364(5) Uani 1 1 d . . .
C1B C 0.5785(3) 0.22727(13) 0.7928(3) 0.0731(13) Uani 1 1 d . . .
H1B1 H 0.5433 0.2215 0.8517 0.110 Uiso 1 1 calc R . .
H1B2 H 0.5733 0.2611 0.7755 0.110 Uiso 1 1 calc R . .
H1B3 H 0.6486 0.2186 0.8039 0.110 Uiso 1 1 calc R . .
O2B O 0.30264(14) 0.25009(7) 0.72797(14) 0.0359(4) Uani 1 1 d . . .
C2B C 0.2721(3) 0.22626(12) 0.8136(3) 0.0707(12) Uani 1 1 d . . .
H2B1 H 0.2962 0.2442 0.8708 0.106 Uiso 1 1 calc R . .
H2B2 H 0.2999 0.1940 0.8163 0.106 Uiso 1 1 calc R . .
H2B3 H 0.1994 0.2244 0.8120 0.106 Uiso 1 1 calc R . .
N1T N 0.6904(2) 0.12206(12) 0.7642(2) 0.0625(9) Uani 1 1 d . . .
N2T N 0.7267(2) 0.08418(14) 0.7833(2) 0.0677(9) Uani 1 1 d . . .
N3T N 0.7628(4) 0.04691(18) 0.8004(4) 0.139(2) Uani 1 1 d . . .
N4T N 0.1642(2) 0.33415(10) 0.7718(2) 0.0505(7) Uani 1 1 d . . .
N5T N 0.1308(2) 0.37404(11) 0.77412(19) 0.0490(7) Uani 1 1 d . . .
N6T N 0.0975(3) 0.41313(12) 0.7769(3) 0.0764(10) Uani 1 1 d . . .
O1S O 0.5335(7) 0.5024(4) 0.6947(10) 0.323(6) Uani 1 1 d . . .
H1S H 0.5933 0.5045 0.7141 0.484 Uiso 1 1 calc R . .
C1S C 0.527(2) 0.4959(8) 0.5970(12) 0.53(2) Uani 1 1 d . . .
H1S1 H 0.5603 0.5225 0.5658 0.799 Uiso 1 1 calc R . .
H1S2 H 0.4575 0.4946 0.5740 0.799 Uiso 1 1 calc R . .
H1S3 H 0.5604 0.4659 0.5812 0.799 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1B 1.8671(19) . ?
Mn1 O1 1.892(2) . ?
Mn1 N1 1.980(2) . ?
Mn1 N2 2.170(2) . ?
Mn1 N1T 2.216(3) . ?
Mn1 O2 2.2184(18) . ?
Mn1 Mn2 3.1498(6) . ?
Mn2 O1B 2.0987(18) . ?
Mn2 O2B 2.1254(19) . ?
Mn2 O2 2.1424(19) . ?
Mn2 O3 2.1533(19) . ?
Mn2 N4 2.335(2) . ?
Mn2 N3 2.369(2) . ?
Mn2 Mn3 3.1518(6) . ?
Mn3 O2B 1.8706(19) . ?
Mn3 O4 1.900(2) . ?
Mn3 N6 1.992(2) . ?
Mn3 O3 2.1500(19) . ?
Mn3 N5 2.206(2) . ?
Mn3 N4T 2.239(3) . ?
O1 C1 1.308(4) . ?
C1 C6 1.413(4) . ?
C1 C2 1.420(5) . ?
C2 O1M 1.366(4) . ?
C2 C3 1.380(5) . ?
C3 C4 1.396(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.351(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.410(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.432(5) . ?
C7 N1 1.286(4) . ?
C7 H7 0.9300 . ?
N1 C8 1.478(4) . ?
C8 C9 1.501(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.501(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N2 C10 1.495(4) . ?
N2 C12 1.500(3) . ?
C10 C11 1.527(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N3 1.495(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
N3 C12 1.483(3) . ?
N3 C19 1.486(3) . ?
C12 C13 1.495(4) . ?
C12 H12 0.9800 . ?
C13 C14 1.397(4) . ?
C13 C18 1.397(4) . ?
C14 C15 1.372(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.383(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.382(4) . ?
C16 H16 0.9300 . ?
C17 O2M 1.379(4) . ?
C17 C18 1.410(4) . ?
C18 O2 1.339(3) . ?
C19 C20 1.519(4) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N4 1.482(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
N4 C23 1.483(3) . ?
N4 C21 1.490(4) . ?
C21 C22 1.529(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 N5 1.497(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
N5 C30 1.499(3) . ?
N5 C23 1.502(3) . ?
C23 C24 1.492(4) . ?
C23 H23 0.9800 . ?
C24 C25 1.387(4) . ?
C24 C29 1.401(4) . ?
C25 C26 1.374(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.381(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.374(5) . ?
C27 H27 0.9300 . ?
C28 O3M 1.385(4) . ?
C28 C29 1.402(4) . ?
C29 O3 1.333(3) . ?
C30 C31 1.511(4) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 N6 1.477(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
N6 C32 1.284(4) . ?
C32 C33 1.429(4) . ?
C32 H32 0.9300 . ?
C33 C38 1.409(4) . ?
C33 C34 1.412(4) . ?
C34 C35 1.357(5) . ?
C34 H34 0.9300 . ?
C35 C36 1.394(5) . ?
C35 H35 0.9300 . ?
C36 C37 1.374(4) . ?
C36 H36 0.9300 . ?
C37 O4M 1.365(4) . ?
C37 C38 1.417(4) . ?
C38 O4 1.316(3) . ?
O1M C1M 1.412(5) . ?
C1M H1M1 0.9600 . ?
C1M H1M2 0.9600 . ?
C1M H1M3 0.9600 . ?
O2M C2M 1.418(4) . ?
C2M H2M1 0.9600 . ?
C2M H2M2 0.9600 . ?
C2M H2M3 0.9600 . ?
O3M C3M 1.422(5) . ?
C3M H3M1 0.9600 . ?
C3M H3M2 0.9600 . ?
C3M H3M3 0.9600 . ?
O4M C4M 1.411(4) . ?
C4M H4M1 0.9600 . ?
C4M H4M2 0.9600 . ?
C4M H4M3 0.9600 . ?
O1B C1B 1.405(4) . ?
C1B H1B1 0.9600 . ?
C1B H1B2 0.9600 . ?
C1B H1B3 0.9600 . ?
O2B C2B 1.414(4) . ?
C2B H2B1 0.9600 . ?
C2B H2B2 0.9600 . ?
C2B H2B3 0.9600 . ?
N1T N2T 1.170(4) . ?
N2T N3T 1.148(5) . ?
N4T N5T 1.183(4) . ?
N5T N6T 1.162(4) . ?
O1S C1S 1.340(18) . ?
O1S H1S 0.8200 . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1B Mn1 O1 93.71(9) . . ?
O1B Mn1 N1 172.59(9) . . ?
O1 Mn1 N1 91.57(10) . . ?
O1B Mn1 N2 92.27(9) . . ?
O1 Mn1 N2 174.02(9) . . ?
N1 Mn1 N2 82.48(10) . . ?
O1B Mn1 N1T 93.99(10) . . ?
O1 Mn1 N1T 92.11(11) . . ?
N1 Mn1 N1T 91.01(11) . . ?
N2 Mn1 N1T 87.44(11) . . ?
O1B Mn1 O2 81.86(7) . . ?
O1 Mn1 O2 95.50(9) . . ?
N1 Mn1 O2 92.46(8) . . ?
N2 Mn1 O2 85.37(8) . . ?
N1T Mn1 O2 171.54(10) . . ?
O1B Mn1 Mn2 40.06(5) . . ?
O1 Mn1 Mn2 103.14(7) . . ?
N1 Mn1 Mn2 133.36(7) . . ?
N2 Mn1 Mn2 81.52(6) . . ?
N1T Mn1 Mn2 131.46(9) . . ?
O2 Mn1 Mn2 42.81(5) . . ?
O1B Mn2 O2B 106.42(8) . . ?
O1B Mn2 O2 78.71(7) . . ?
O2B Mn2 O2 97.86(7) . . ?
O1B Mn2 O3 92.74(7) . . ?
O2B Mn2 O3 76.80(7) . . ?
O2 Mn2 O3 168.34(7) . . ?
O1B Mn2 N4 163.05(8) . . ?
O2B Mn2 N4 89.17(8) . . ?
O2 Mn2 N4 106.22(7) . . ?
O3 Mn2 N4 84.24(7) . . ?
O1B Mn2 N3 86.39(8) . . ?
O2B Mn2 N3 167.17(8) . . ?
O2 Mn2 N3 83.73(8) . . ?
O3 Mn2 N3 103.81(8) . . ?
N4 Mn2 N3 78.20(8) . . ?
O1B Mn2 Mn1 34.93(5) . . ?
O2B Mn2 Mn1 112.82(5) . . ?
O2 Mn2 Mn1 44.72(5) . . ?
O3 Mn2 Mn1 127.59(5) . . ?
N4 Mn2 Mn1 143.64(6) . . ?
N3 Mn2 Mn1 77.24(6) . . ?
O1B Mn2 Mn3 110.27(5) . . ?
O2B Mn2 Mn3 35.17(5) . . ?
O2 Mn2 Mn3 132.99(5) . . ?
O3 Mn2 Mn3 42.87(5) . . ?
N4 Mn2 Mn3 78.61(6) . . ?
N3 Mn2 Mn3 141.02(6) . . ?
Mn1 Mn2 Mn3 135.671(17) . . ?
O2B Mn3 O4 94.59(8) . . ?
O2B Mn3 N6 174.92(9) . . ?
O4 Mn3 N6 90.48(9) . . ?
O2B Mn3 O3 82.44(8) . . ?
O4 Mn3 O3 95.12(9) . . ?
N6 Mn3 O3 96.78(9) . . ?
O2B Mn3 N5 93.05(8) . . ?
O4 Mn3 N5 172.20(9) . . ?
N6 Mn3 N5 81.87(9) . . ?
O3 Mn3 N5 84.34(8) . . ?
O2B Mn3 N4T 94.34(9) . . ?
O4 Mn3 N4T 93.91(10) . . ?
N6 Mn3 N4T 85.64(10) . . ?
O3 Mn3 N4T 170.62(9) . . ?
N5 Mn3 N4T 87.05(10) . . ?
O2B Mn3 Mn2 40.88(6) . . ?
O4 Mn3 Mn2 104.83(6) . . ?
N6 Mn3 Mn2 137.06(7) . . ?
O3 Mn3 Mn2 42.95(5) . . ?
N5 Mn3 Mn2 80.08(6) . . ?
N4T Mn3 Mn2 131.57(7) . . ?
C1 O1 Mn1 129.4(2) . . ?
O1 C1 C6 124.2(3) . . ?
O1 C1 C2 118.3(3) . . ?
C6 C1 C2 117.5(3) . . ?
O1M C2 C3 125.2(3) . . ?
O1M C2 C1 114.1(3) . . ?
C3 C2 C1 120.7(3) . . ?
C2 C3 C4 120.5(4) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.0(4) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 120.1(3) . . ?
C5 C6 C7 118.0(3) . . ?
C1 C6 C7 121.9(3) . . ?
N1 C7 C6 126.4(3) . . ?
N1 C7 H7 116.8 . . ?
C6 C7 H7 116.8 . . ?
C7 N1 C8 118.8(3) . . ?
C7 N1 Mn1 125.6(2) . . ?
C8 N1 Mn1 115.5(2) . . ?
N1 C8 C9 109.5(3) . . ?
N1 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
N1 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
C8 C9 N2 111.0(3) . . ?
C8 C9 H9A 109.4 . . ?
N2 C9 H9A 109.4 . . ?
C8 C9 H9B 109.4 . . ?
N2 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C10 N2 C12 101.2(2) . . ?
C10 N2 C9 110.6(2) . . ?
C12 N2 C9 111.9(2) . . ?
C10 N2 Mn1 111.93(18) . . ?
C12 N2 Mn1 117.70(17) . . ?
C9 N2 Mn1 103.72(19) . . ?
N2 C10 C11 105.4(2) . . ?
N2 C10 H10A 110.7 . . ?
C11 C10 H10A 110.7 . . ?
N2 C10 H10B 110.7 . . ?
C11 C10 H10B 110.7 . . ?
H10A C10 H10B 108.8 . . ?
N3 C11 C10 104.9(2) . . ?
N3 C11 H11A 110.8 . . ?
C10 C11 H11A 110.8 . . ?
N3 C11 H11B 110.8 . . ?
C10 C11 H11B 110.8 . . ?
H11A C11 H11B 108.9 . . ?
C12 N3 C19 111.9(2) . . ?
C12 N3 C11 103.6(2) . . ?
C19 N3 C11 111.4(2) . . ?
C12 N3 Mn2 113.44(17) . . ?
C19 N3 Mn2 107.07(16) . . ?
C11 N3 Mn2 109.42(17) . . ?
N3 C12 C13 114.3(2) . . ?
N3 C12 N2 101.7(2) . . ?
C13 C12 N2 116.8(2) . . ?
N3 C12 H12 107.8 . . ?
C13 C12 H12 107.8 . . ?
N2 C12 H12 107.8 . . ?
C14 C13 C18 120.7(3) . . ?
C14 C13 C12 119.5(3) . . ?
C18 C13 C12 119.7(2) . . ?
C15 C14 C13 120.7(3) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C14 C15 C16 119.3(3) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C17 C16 C15 121.1(3) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
O2M C17 C16 118.3(3) . . ?
O2M C17 C18 121.3(3) . . ?
C16 C17 C18 120.3(3) . . ?
O2 C18 C13 121.2(3) . . ?
O2 C18 C17 121.0(3) . . ?
C13 C18 C17 117.8(3) . . ?
C18 O2 Mn2 117.74(17) . . ?
C18 O2 Mn1 120.59(16) . . ?
Mn2 O2 Mn1 92.47(7) . . ?
N3 C19 C20 112.9(2) . . ?
N3 C19 H19A 109.0 . . ?
C20 C19 H19A 109.0 . . ?
N3 C19 H19B 109.0 . . ?
C20 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
N4 C20 C19 113.3(2) . . ?
N4 C20 H20A 108.9 . . ?
C19 C20 H20A 108.9 . . ?
N4 C20 H20B 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.7 . . ?
C20 N4 C23 112.5(2) . . ?
C20 N4 C21 111.9(2) . . ?
C23 N4 C21 104.1(2) . . ?
C20 N4 Mn2 106.96(15) . . ?
C23 N4 Mn2 113.31(15) . . ?
C21 N4 Mn2 108.10(17) . . ?
N4 C21 C22 105.3(2) . . ?
N4 C21 H21A 110.7 . . ?
C22 C21 H21A 110.7 . . ?
N4 C21 H21B 110.7 . . ?
C22 C21 H21B 110.7 . . ?
H21A C21 H21B 108.8 . . ?
N5 C22 C21 105.0(2) . . ?
N5 C22 H22A 110.8 . . ?
C21 C22 H22A 110.8 . . ?
N5 C22 H22B 110.8 . . ?
C21 C22 H22B 110.8 . . ?
H22A C22 H22B 108.8 . . ?
C22 N5 C30 111.4(2) . . ?
C22 N5 C23 102.0(2) . . ?
C30 N5 C23 111.0(2) . . ?
C22 N5 Mn3 110.63(17) . . ?
C30 N5 Mn3 104.28(16) . . ?
C23 N5 Mn3 117.72(16) . . ?
N4 C23 C24 115.6(2) . . ?
N4 C23 N5 101.7(2) . . ?
C24 C23 N5 115.0(2) . . ?
N4 C23 H23 108.1 . . ?
C24 C23 H23 108.1 . . ?
N5 C23 H23 108.1 . . ?
C25 C24 C29 120.9(3) . . ?
C25 C24 C23 119.3(3) . . ?
C29 C24 C23 119.8(2) . . ?
C26 C25 C24 119.9(3) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C27 120.2(3) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C28 C27 C26 120.4(3) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 O3M 119.3(3) . . ?
C27 C28 C29 120.9(3) . . ?
O3M C28 C29 119.7(3) . . ?
O3 C29 C24 120.3(2) . . ?
O3 C29 C28 122.1(3) . . ?
C24 C29 C28 117.7(3) . . ?
C29 O3 Mn3 121.30(16) . . ?
C29 O3 Mn2 118.05(16) . . ?
Mn3 O3 Mn2 94.18(7) . . ?
N5 C30 C31 110.5(2) . . ?
N5 C30 H30A 109.6 . . ?
C31 C30 H30A 109.6 . . ?
N5 C30 H30B 109.6 . . ?
C31 C30 H30B 109.6 . . ?
H30A C30 H30B 108.1 . . ?
N6 C31 C30 108.3(2) . . ?
N6 C31 H31A 110.0 . . ?
C30 C31 H31A 110.0 . . ?
N6 C31 H31B 110.0 . . ?
C30 C31 H31B 110.0 . . ?
H31A C31 H31B 108.4 . . ?
C32 N6 C31 119.3(3) . . ?
C32 N6 Mn3 124.4(2) . . ?
C31 N6 Mn3 115.43(18) . . ?
N6 C32 C33 126.8(3) . . ?
N6 C32 H32 116.6 . . ?
C33 C32 H32 116.6 . . ?
C38 C33 C34 119.9(3) . . ?
C38 C33 C32 122.0(3) . . ?
C34 C33 C32 118.0(3) . . ?
C35 C34 C33 120.9(3) . . ?
C35 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C34 C35 C36 119.9(3) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C37 C36 C35 120.7(3) . . ?
C37 C36 H36 119.6 . . ?
C35 C36 H36 119.6 . . ?
O4M C37 C36 124.4(3) . . ?
O4M C37 C38 114.8(3) . . ?
C36 C37 C38 120.8(3) . . ?
O4 C38 C33 123.6(3) . . ?
O4 C38 C37 118.7(3) . . ?
C33 C38 C37 117.7(3) . . ?
C38 O4 Mn3 127.80(19) . . ?
C2 O1M C1M 117.5(3) . . ?
O1M C1M H1M1 109.5 . . ?
O1M C1M H1M2 109.5 . . ?
H1M1 C1M H1M2 109.5 . . ?
O1M C1M H1M3 109.5 . . ?
H1M1 C1M H1M3 109.5 . . ?
H1M2 C1M H1M3 109.5 . . ?
C17 O2M C2M 113.6(3) . . ?
O2M C2M H2M1 109.5 . . ?
O2M C2M H2M2 109.5 . . ?
H2M1 C2M H2M2 109.5 . . ?
O2M C2M H2M3 109.5 . . ?
H2M1 C2M H2M3 109.5 . . ?
H2M2 C2M H2M3 109.5 . . ?
C28 O3M C3M 115.2(3) . . ?
O3M C3M H3M1 109.5 . . ?
O3M C3M H3M2 109.5 . . ?
H3M1 C3M H3M2 109.5 . . ?
O3M C3M H3M3 109.5 . . ?
H3M1 C3M H3M3 109.5 . . ?
H3M2 C3M H3M3 109.5 . . ?
C37 O4M C4M 116.3(3) . . ?
O4M C4M H4M1 109.5 . . ?
O4M C4M H4M2 109.5 . . ?
H4M1 C4M H4M2 109.5 . . ?
O4M C4M H4M3 109.5 . . ?
H4M1 C4M H4M3 109.5 . . ?
H4M2 C4M H4M3 109.5 . . ?
C1B O1B Mn1 124.36(19) . . ?
C1B O1B Mn2 122.93(19) . . ?
Mn1 O1B Mn2 105.02(8) . . ?
O1B C1B H1B1 109.5 . . ?
O1B C1B H1B2 109.5 . . ?
H1B1 C1B H1B2 109.5 . . ?
O1B C1B H1B3 109.5 . . ?
H1B1 C1B H1B3 109.5 . . ?
H1B2 C1B H1B3 109.5 . . ?
C2B O2B Mn3 124.86(19) . . ?
C2B O2B Mn2 124.68(19) . . ?
Mn3 O2B Mn2 103.95(9) . . ?
O2B C2B H2B1 109.5 . . ?
O2B C2B H2B2 109.5 . . ?
H2B1 C2B H2B2 109.5 . . ?
O2B C2B H2B3 109.5 . . ?
H2B1 C2B H2B3 109.5 . . ?
H2B2 C2B H2B3 109.5 . . ?
N2T N1T Mn1 122.8(3) . . ?
N3T N2T N1T 178.8(5) . . ?
N5T N4T Mn3 122.8(2) . . ?
N6T N5T N4T 179.5(4) . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1S N3T 0.82 2.25 2.951(9) 144.2 2_656

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.053

# start Validation Reply Form
_vrf_PLAT260_a20160412esh141_ta  
;
PROBLEM: Large Average Ueq of Residue Including O1S 0.429 Check
RESPONSE: O1S belongs to a losely bound methanol molecule of
crystallization, which is poorly determined at room temperature.
 The crystal might have undergone partial loss of such 
crystallization solvent molecule throughout the room temperature
intensity data acquisition
;
_vrf_PLAT413_a20160412esh141_ta  
;
PROBLEM: Short Inter XH3 .. XHn H1S1 ..H1S2 . 1.96 Ang.
RESPONSE: The title H atoms belong to neighboring, losely bound 
methanol molecules of crystallization, which are poorly determined 
at room temperature.The crystal might have undergone partial loss 
of such crystallization solvent molecules throughout 
the room temperature intensity data acquisition
;
# end Validation Reply Form

