# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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 1044300'
_audit_update_record             
;
2015-01-19 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;
# local name eb3241
_audit_creation_date             2013-10-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2013-4
_publ_section_exptl              
;
Any special experimental details
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C42 H44 Mn2 N8 O4, 2(Cl O4), 2(H0.4 O0.22)'
_chemical_formula_sum            'C42 H44.80 Cl2 Mn2 N8 O12.44'
_chemical_formula_weight         1041.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H20 Mn2 Cl O6 N8'
_chemical_oxdiff_usercomment     '@ 120 K PC175'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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                   21.1082(7)
_cell_length_b                   10.3582(3)
_cell_length_c                   22.8139(7)
_cell_angle_alpha                90
_cell_angle_beta                 115.866(4)
_cell_angle_gamma                90
_cell_volume                     4488.4(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12755
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      74.7120
_cell_measurement_theta_min      4.2880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.296
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2145
_exptl_crystal_size_max          0.1218
_exptl_crystal_size_mid          0.0844
_exptl_crystal_size_min          0.0669
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            34109
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.096
_diffrn_reflns_theta_min         4.307
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9909
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0341107000
_diffrn_orient_matrix_UB_12      -0.0456021000
_diffrn_orient_matrix_UB_13      0.0714324000
_diffrn_orient_matrix_UB_21      -0.0601807000
_diffrn_orient_matrix_UB_22      0.0633979000
_diffrn_orient_matrix_UB_23      0.0106992000
_diffrn_orient_matrix_UB_31      -0.0424144000
_diffrn_orient_matrix_UB_32      -0.1265094000
_diffrn_orient_matrix_UB_33      -0.0203326000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4345
_reflns_number_total             4658
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    
;
Olex2
;
_computing_publication_material  
;
Olex2
;
_computing_structure_refinement  
;
ShelXL
;
_computing_structure_solution    
;
ShelXS
;
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0369
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0451P)²+7.6108P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0928
_refine_special_details          
;
Compound PC175 was provided as small black block crystals suitable for single 
crystal X-ray diffraction, yielding structure EB3241.

The asymmetric unit of eb3241 (Figure 1) is one half of the complete complex
(Figure 2) plus perchlorate anion and one water molecule, the occupancy of 
which was freely refined to approximately 22%.  


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ     Please Check
068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...     Please Check

Insignificant rounding.

#===============================================================================
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O7(H7A,H7B)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C15(H15A,H15B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4A), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C19(H19)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.09597(2) 0.45842(3) 0.80783(2) 0.01831(9) Uani 1 1 d . . . . .
O1 O 0.18003(7) 0.50019(14) 0.80457(7) 0.0234(3) Uani 1 1 d . . . . .
O2 O -0.01324(7) 0.42139(13) 0.68158(7) 0.0214(3) Uani 1 1 d . . . . .
N4 N 0.04399(8) 0.50144(16) 0.71273(8) 0.0203(3) Uani 1 1 d . . . . .
N3 N 0.10971(9) 0.63674(17) 0.87219(9) 0.0237(4) Uani 1 1 d . . . . .
N1 N 0.10890(9) 0.24500(17) 0.79260(8) 0.0226(3) Uani 1 1 d . . . . .
N2 N 0.15385(9) 0.38706(17) 0.90246(8) 0.0238(4) Uani 1 1 d . . . . .
H2N H 0.1205(16) 0.361(3) 0.9129(14) 0.042(8) Uiso 1 1 d . . . . .
C1 C 0.18654(10) 0.6006(2) 0.77092(10) 0.0224(4) Uani 1 1 d . . . . .
C2 C 0.24996(11) 0.6710(2) 0.79727(11) 0.0276(4) Uani 1 1 d . . . . .
H2 H 0.2858 0.6488 0.8390 0.033 Uiso 1 1 calc R U . . .
C3 C 0.26036(11) 0.7718(2) 0.76300(12) 0.0310(5) Uani 1 1 d . . . . .
H3 H 0.3034 0.8183 0.7813 0.037 Uiso 1 1 calc R U . . .
C4 C 0.20851(12) 0.8063(2) 0.70179(12) 0.0305(5) Uani 1 1 d . . . . .
H4A H 0.2158 0.8769 0.6789 0.037 Uiso 1 1 calc R U . . .
C5 C 0.14654(11) 0.7372(2) 0.67473(11) 0.0269(4) Uani 1 1 d . . . . .
H5 H 0.1116 0.7599 0.6327 0.032 Uiso 1 1 calc R U . . .
C6 C 0.13411(10) 0.6337(2) 0.70831(10) 0.0221(4) Uani 1 1 d . . . . .
C7 C 0.06890(10) 0.55876(19) 0.67633(10) 0.0206(4) Uani 1 1 d . . . . .
C8 C 0.03574(11) 0.5399(2) 0.60392(10) 0.0241(4) Uani 1 1 d . . . . .
H8A H 0.0364 0.6222 0.5821 0.029 Uiso 1 1 calc R U . . .
H8B H -0.0139 0.5126 0.5886 0.029 Uiso 1 1 calc R U . . .
C9 C 0.07655(13) 0.4367(2) 0.58653(11) 0.0347(5) Uani 1 1 d . . . . .
H9A H 0.0551 0.4246 0.5392 0.052 Uiso 1 1 calc R U . . .
H9B H 0.0751 0.3551 0.6077 0.052 Uiso 1 1 calc R U . . .
H9C H 0.1256 0.4642 0.6016 0.052 Uiso 1 1 calc R U . . .
C10 C 0.07309(12) 0.7472(2) 0.85834(12) 0.0298(5) Uani 1 1 d . . . . .
H10 H 0.0423 0.7653 0.8141 0.036 Uiso 1 1 calc R U . . .
C11 C 0.07792(13) 0.8361(2) 0.90521(14) 0.0377(5) Uani 1 1 d . . . . .
H11 H 0.0515 0.9139 0.8934 0.045 Uiso 1 1 calc R U . . .
C12 C 0.12183(13) 0.8098(2) 0.96947(13) 0.0380(5) Uani 1 1 d . . . . .
H12 H 0.1257 0.8686 1.0028 0.046 Uiso 1 1 calc R U . . .
C13 C 0.16033(12) 0.6962(2) 0.98464(11) 0.0315(5) Uani 1 1 d . . . . .
H13 H 0.1910 0.6760 1.0286 0.038 Uiso 1 1 calc R U . . .
C14 C 0.15350(10) 0.6124(2) 0.93495(10) 0.0244(4) Uani 1 1 d . . . . .
C15 C 0.19551(11) 0.4892(2) 0.94773(11) 0.0298(5) Uani 1 1 d . . . . .
H15A H 0.2390 0.5050 0.9424 0.036 Uiso 1 1 calc R U . . .
H15B H 0.2094 0.4608 0.9931 0.036 Uiso 1 1 calc R U . . .
C16 C 0.07612(11) 0.1737(2) 0.73811(11) 0.0267(4) Uani 1 1 d . . . . .
H16 H 0.0404 0.2131 0.7007 0.032 Uiso 1 1 calc R U . . .
C17 C 0.09228(12) 0.0463(2) 0.73447(12) 0.0319(5) Uani 1 1 d . . . . .
H17 H 0.0690 -0.0006 0.6950 0.038 Uiso 1 1 calc R U . . .
C18 C 0.14312(13) -0.0127(2) 0.78940(13) 0.0344(5) Uani 1 1 d . . . . .
H18 H 0.1547 -0.1010 0.7885 0.041 Uiso 1 1 calc R U . . .
C19 C 0.17664(14) 0.0597(2) 0.84549(12) 0.0345(5) Uani 1 1 d . . . . .
H19 H 0.2117 0.0215 0.8838 0.041 Uiso 1 1 calc R U . . .
C20 C 0.15869(11) 0.1883(2) 0.84546(10) 0.0252(4) Uani 1 1 d . . . . .
C21 C 0.19669(11) 0.2734(2) 0.90385(11) 0.0289(5) Uani 1 1 d . . . . .
H21A H 0.2076 0.2232 0.9441 0.035 Uiso 1 1 calc R U . . .
H21B H 0.2417 0.3025 0.9047 0.035 Uiso 1 1 calc R U . . .
Cl1 Cl 0.08449(3) 0.18875(5) 0.99273(3) 0.03446(14) Uani 1 1 d . . . . .
O3 O 0.13953(10) 0.0999(2) 1.02971(12) 0.0554(6) Uani 1 1 d . . . . .
O4 O 0.02840(10) 0.1750(2) 1.01106(10) 0.0479(5) Uani 1 1 d . . . . .
O5 O 0.06025(13) 0.1642(2) 0.92433(10) 0.0561(5) Uani 1 1 d . . . . .
O6 O 0.11225(13) 0.31837(18) 1.00701(10) 0.0517(5) Uani 1 1 d . . . . .
O7 O 0.0906(5) -0.0732(10) 1.0974(5) 0.050(4) Uani 0.221(9) 1 d G . . . .
H7A H 0.0919 -0.0170 1.0709 0.074 Uiso 0.21(8) 1 d G U . . .
H7B H 0.0542 -0.1202 1.0785 0.074 Uiso 0.18(7) 1 d G 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
Mn1 O1 1.8590(14) . ?
Mn1 O2 1.9035(14) 2_556 ?
Mn1 N4 2.0081(17) . ?
Mn1 N3 2.2979(18) . ?
Mn1 N1 2.2727(18) . ?
Mn1 N2 2.0971(18) . ?
O1 C1 1.335(3) . ?
O2 Mn1 1.9034(13) 2_556 ?
O2 N4 1.379(2) . ?
N4 C7 1.304(3) . ?
N3 C10 1.339(3) . ?
N3 C14 1.347(3) . ?
N1 C16 1.349(3) . ?
N1 C20 1.341(3) . ?
N2 H2N 0.88(3) . ?
N2 C15 1.472(3) . ?
N2 C21 1.477(3) . ?
C1 C2 1.408(3) . ?
C1 C6 1.415(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.378(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.394(3) . ?
C4 H4A 0.9500 . ?
C4 C5 1.378(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.407(3) . ?
C6 C7 1.467(3) . ?
C7 C8 1.500(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.530(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 0.9500 . ?
C10 C11 1.381(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.377(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.386(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.384(3) . ?
C14 C15 1.509(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16 0.9500 . ?
C16 C17 1.375(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.386(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.382(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.385(3) . ?
C20 C21 1.504(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
Cl1 O3 1.433(2) . ?
Cl1 O4 1.4244(19) . ?
Cl1 O5 1.437(2) . ?
Cl1 O6 1.444(2) . ?
O7 H7A 0.8490 . ?
O7 H7B 0.8507 . ?

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
O1 Mn1 O2 175.18(7) . 2_556 ?
O1 Mn1 N4 89.22(6) . . ?
O1 Mn1 N3 88.96(6) . . ?
O1 Mn1 N1 92.29(6) . . ?
O1 Mn1 N2 89.18(7) . . ?
O2 Mn1 N4 94.74(6) 2_556 . ?
O2 Mn1 N3 87.02(6) 2_556 . ?
O2 Mn1 N1 90.08(6) 2_556 . ?
O2 Mn1 N2 87.31(7) 2_556 . ?
N4 Mn1 N3 111.66(7) . . ?
N4 Mn1 N1 95.51(7) . . ?
N4 Mn1 N2 171.38(7) . . ?
N1 Mn1 N3 152.81(6) . . ?
N2 Mn1 N3 76.77(7) . . ?
N2 Mn1 N1 76.09(7) . . ?
C1 O1 Mn1 122.95(12) . . ?
N4 O2 Mn1 117.33(11) . 2_556 ?
O2 N4 Mn1 111.48(11) . . ?
C7 N4 Mn1 127.38(14) . . ?
C7 N4 O2 116.84(16) . . ?
C10 N3 Mn1 129.57(15) . . ?
C10 N3 C14 117.94(19) . . ?
C14 N3 Mn1 111.46(14) . . ?
C16 N1 Mn1 128.77(14) . . ?
C20 N1 Mn1 112.81(14) . . ?
C20 N1 C16 118.35(19) . . ?
Mn1 N2 H2N 102.3(19) . . ?
C15 N2 Mn1 111.74(14) . . ?
C15 N2 H2N 110(2) . . ?
C15 N2 C21 112.66(17) . . ?
C21 N2 Mn1 112.31(13) . . ?
C21 N2 H2N 108(2) . . ?
O1 C1 C2 118.37(19) . . ?
O1 C1 C6 122.52(18) . . ?
C2 C1 C6 118.99(19) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 C1 120.5(2) . . ?
C3 C2 H2 119.8 . . ?
C2 C3 H3 119.6 . . ?
C2 C3 C4 120.9(2) . . ?
C4 C3 H3 119.6 . . ?
C3 C4 H4A 120.2 . . ?
C5 C4 C3 119.5(2) . . ?
C5 C4 H4A 120.2 . . ?
C4 C5 H5 119.4 . . ?
C4 C5 C6 121.2(2) . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C7 121.64(18) . . ?
C5 C6 C1 118.98(19) . . ?
C5 C6 C7 119.31(19) . . ?
N4 C7 C6 118.41(18) . . ?
N4 C7 C8 121.22(18) . . ?
C6 C7 C8 120.17(17) . . ?
C7 C8 H8A 109.8 . . ?
C7 C8 H8B 109.8 . . ?
C7 C8 C9 109.38(17) . . ?
H8A C8 H8B 108.2 . . ?
C9 C8 H8A 109.8 . . ?
C9 C8 H8B 109.8 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10 118.4 . . ?
N3 C10 C11 123.2(2) . . ?
C11 C10 H10 118.4 . . ?
C10 C11 H11 120.7 . . ?
C12 C11 C10 118.7(2) . . ?
C12 C11 H11 120.7 . . ?
C11 C12 H12 120.6 . . ?
C11 C12 C13 118.9(2) . . ?
C13 C12 H12 120.6 . . ?
C12 C13 H13 120.4 . . ?
C14 C13 C12 119.2(2) . . ?
C14 C13 H13 120.4 . . ?
N3 C14 C13 122.1(2) . . ?
N3 C14 C15 115.89(18) . . ?
C13 C14 C15 122.0(2) . . ?
N2 C15 C14 110.60(17) . . ?
N2 C15 H15A 109.5 . . ?
N2 C15 H15B 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
N1 C16 H16 118.6 . . ?
N1 C16 C17 122.7(2) . . ?
C17 C16 H16 118.6 . . ?
C16 C17 H17 120.6 . . ?
C16 C17 C18 118.9(2) . . ?
C18 C17 H17 120.6 . . ?
C17 C18 H18 120.7 . . ?
C19 C18 C17 118.7(2) . . ?
C19 C18 H18 120.7 . . ?
C18 C19 H19 120.3 . . ?
C18 C19 C20 119.5(2) . . ?
C20 C19 H19 120.3 . . ?
N1 C20 C19 121.9(2) . . ?
N1 C20 C21 116.50(18) . . ?
C19 C20 C21 121.5(2) . . ?
N2 C21 C20 111.29(17) . . ?
N2 C21 H21A 109.4 . . ?
N2 C21 H21B 109.4 . . ?
C20 C21 H21A 109.4 . . ?
C20 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
O3 Cl1 O5 109.81(14) . . ?
O3 Cl1 O6 108.61(14) . . ?
O4 Cl1 O3 109.12(14) . . ?
O4 Cl1 O5 110.70(13) . . ?
O4 Cl1 O6 109.51(12) . . ?
O5 Cl1 O6 109.06(13) . . ?
H7A O7 H7B 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
N2 H2N O5 0.88(3) 2.47(3) 3.216(3) 143(3) .
N2 H2N O6 0.88(3) 2.27(3) 2.966(3) 136(2) .
O7 H7A O3 0.85 2.05 2.839(10) 155.4 .
O7 H7B O4 0.85 2.11 2.851(10) 146.0 5_557

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
Mn1 O1 C1 C2 143.19(15) . . . . ?
Mn1 O1 C1 C6 -40.8(2) . . . . ?
Mn1 O2 N4 Mn1 78.75(13) 2_556 . . . ?
Mn1 O2 N4 C7 -122.77(15) 2_556 . . . ?
Mn1 N4 C7 C6 -19.1(3) . . . . ?
Mn1 N4 C7 C8 155.65(15) . . . . ?
Mn1 N3 C10 C11 166.91(17) . . . . ?
Mn1 N3 C14 C13 -168.21(17) . . . . ?
Mn1 N3 C14 C15 12.7(2) . . . . ?
Mn1 N1 C16 C17 175.74(16) . . . . ?
Mn1 N1 C20 C19 -177.50(17) . . . . ?
Mn1 N1 C20 C21 -0.4(2) . . . . ?
Mn1 N2 C15 C14 40.9(2) . . . . ?
Mn1 N2 C21 C20 -36.9(2) . . . . ?
O1 C1 C2 C3 177.08(19) . . . . ?
O1 C1 C6 C5 -176.92(18) . . . . ?
O1 C1 C6 C7 -0.1(3) . . . . ?
O2 N4 C7 C6 -173.64(16) . . . . ?
O2 N4 C7 C8 1.1(3) . . . . ?
N4 Mn1 O1 C1 40.09(16) . . . . ?
N4 C7 C8 C9 -97.4(2) . . . . ?
N3 Mn1 O1 C1 -71.59(16) . . . . ?
N3 C10 C11 C12 -0.7(4) . . . . ?
N3 C14 C15 N2 -35.2(3) . . . . ?
N1 Mn1 O1 C1 135.58(15) . . . . ?
N1 C16 C17 C18 1.6(3) . . . . ?
N1 C20 C21 N2 23.8(3) . . . . ?
N2 Mn1 O1 C1 -148.38(16) . . . . ?
C1 C2 C3 C4 0.1(3) . . . . ?
C1 C6 C7 N4 30.2(3) . . . . ?
C1 C6 C7 C8 -144.63(19) . . . . ?
C2 C1 C6 C5 -0.9(3) . . . . ?
C2 C1 C6 C7 175.87(18) . . . . ?
C2 C3 C4 C5 -1.1(3) . . . . ?
C3 C4 C5 C6 1.1(3) . . . . ?
C4 C5 C6 C1 -0.1(3) . . . . ?
C4 C5 C6 C7 -176.97(19) . . . . ?
C5 C6 C7 N4 -153.04(19) . . . . ?
C5 C6 C7 C8 32.2(3) . . . . ?
C6 C1 C2 C3 0.9(3) . . . . ?
C6 C7 C8 C9 77.2(2) . . . . ?
C10 N3 C14 C13 1.3(3) . . . . ?
C10 N3 C14 C15 -177.84(19) . . . . ?
C10 C11 C12 C13 1.0(4) . . . . ?
C11 C12 C13 C14 -0.1(4) . . . . ?
C12 C13 C14 N3 -1.1(3) . . . . ?
C12 C13 C14 C15 178.0(2) . . . . ?
C13 C14 C15 N2 145.7(2) . . . . ?
C14 N3 C10 C11 -0.4(3) . . . . ?
C15 N2 C21 C20 -164.15(18) . . . . ?
C16 N1 C20 C19 -0.4(3) . . . . ?
C16 N1 C20 C21 176.62(18) . . . . ?
C16 C17 C18 C19 -1.2(3) . . . . ?
C17 C18 C19 C20 0.1(4) . . . . ?
C18 C19 C20 N1 0.8(3) . . . . ?
C18 C19 C20 C21 -176.1(2) . . . . ?
C19 C20 C21 N2 -159.1(2) . . . . ?
C20 N1 C16 C17 -0.8(3) . . . . ?
C21 N2 C15 C14 168.47(18) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4 6 2 0.0334 4.0067 6.0016 1.9880 0.0050 0.1606 -0.9696
-4 -6 -2 0.0334 -4.0067 -6.0016 -1.9880 -0.0050 -0.1606 0.9696
13 -1 -11 0.0464 12.9913 -1.0060 -10.9981 -0.2966 -0.9633 -0.2001
-13 1 10 0.0582 -12.9910 1.0063 9.9978 0.2251 0.9526 0.2204
-2 -1 14 0.0394 -2.0049 -1.0041 14.0057 0.9779 0.2068 -0.0727
2 1 -14 0.0394 2.0049 1.0041 -14.0057 -0.9779 -0.2068 0.0727
-3 -3 -10 0.0348 -2.9995 -2.9971 -9.9967 -0.6797 -0.1165 0.7096
5 5 -10 0.0410 5.0081 5.0040 -10.0129 -0.7726 -0.0913 -0.6419
4 -5 5 0.0433 3.9862 -5.0085 5.0134 0.7225 -0.5038 0.3626
-9 -3 -4 0.0423 -8.9966 -2.9951 -3.9963 -0.4558 0.3088 0.8417
-5 5 -5 0.0358 -4.9854 5.0091 -5.0136 -0.7566 0.5640 -0.3203
3 2 11 0.0453 2.9974 1.9960 10.9992 0.7969 0.0638 -0.6033
11 1 -13 0.0358 10.9972 0.9976 -13.0035 -0.5992 -0.7377 -0.3283
5 -4 -12 0.0450 4.9929 -4.0027 -11.9933 -0.5039 -0.6826 0.5385
-6 6 -2 0.0323 -5.9838 6.0097 -2.0152 -0.6221 0.7195 -0.4655
8 -5 -7 0.0476 7.9870 -5.0072 -6.9891 0.0015 -0.8729 0.4368

####################################################################### 
# 
# 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 1044301'
_audit_update_record             
;
2015-01-19 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;
# local name 2013ncs0819

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H38 Mn2 N8 O4, 2(Cl O4), 2(C H4 O)'
_chemical_formula_sum            'C42 H46 Cl2 Mn2 N8 O14'
_chemical_formula_weight         1067.65

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'
Cl Cl 0.1484 0.1585 '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                   13.1019(7)
_cell_length_b                   14.5141(7)
_cell_length_c                   14.8351(10)
_cell_angle_alpha                105.116(7)
_cell_angle_beta                 110.267(8)
_cell_angle_gamma                108.665(8)
_cell_volume                     2277.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15726
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.6

_exptl_crystal_description       lath
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_F_000             1100
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.748
_shelx_estimated_absorpt_T_min   0.890
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.317
_exptl_absorpt_process_details   'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support Mitegen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_reflns_number            24513
_diffrn_reflns_av_unetI/netI     0.1689
_diffrn_reflns_av_R_equivalents  0.1040
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.037
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             10234
_reflns_number_gt                6066
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_computing_cell_refinement       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_computing_data_reduction        'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)'
_computing_structure_solution    
'SUPERFLIP (Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  
'WinGX, ver.2013.3 (L.J. Farrugia, J.App.Cryst.(2012),45,849-854)'

_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)+(0.1699P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10234
_refine_ls_number_parameters     642
_refine_ls_number_restraints     166
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.0949
_refine_ls_wR_factor_ref         0.2895
_refine_ls_wR_factor_gt          0.2502
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.009
_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
C1 C 0.7866(6) 0.4219(4) 0.1890(4) 0.0394(13) Uani 1 1 d . . . . .
C2 C 0.7087(7) 0.4252(5) 0.0992(4) 0.0486(15) Uani 1 1 d . . . . .
H2 H 0.6285 0.4132 0.0870 0.058 Uiso 1 1 calc R U . . .
C3 C 0.7470(7) 0.4457(5) 0.0279(4) 0.0542(17) Uani 1 1 d . . . . .
H3 H 0.6930 0.4476 -0.0332 0.065 Uiso 1 1 calc R U . . .
C4 C 0.8637(7) 0.4636(5) 0.0444(5) 0.0531(16) Uani 1 1 d . . . . .
H4 H 0.8909 0.4807 -0.0035 0.064 Uiso 1 1 calc R U . . .
C5 C 0.9389(7) 0.4566(5) 0.1294(4) 0.0497(16) Uani 1 1 d . . . . .
H5 H 1.0177 0.4662 0.1387 0.060 Uiso 1 1 calc R U . . .
C6 C 0.9032(6) 0.4356(4) 0.2043(4) 0.0406(13) Uani 1 1 d . . . . .
C7 C 0.9861(6) 0.4254(4) 0.2927(4) 0.0374(12) Uani 1 1 d . . . . .
C8 C 1.0794(6) 0.3899(5) 0.2842(4) 0.0459(14) Uani 1 1 d . . . . .
H8A H 1.0588 0.3570 0.2096 0.069 Uiso 1 1 calc R U . . .
H8B H 1.0801 0.3376 0.3146 0.069 Uiso 1 1 calc R U . . .
H8C H 1.1602 0.4519 0.3228 0.069 Uiso 1 1 calc R U . . .
C10 C 0.7805(6) 0.2827(4) 0.4518(4) 0.0429(13) Uani 1 1 d . . . . .
H10 H 0.8404 0.2741 0.4334 0.051 Uiso 1 1 calc R U . . .
C11 C 0.7238(6) 0.2121(5) 0.4858(4) 0.0467(15) Uani 1 1 d . . . . .
H11 H 0.7446 0.1560 0.4910 0.056 Uiso 1 1 calc R U . . .
C12 C 0.6372(7) 0.2244(5) 0.5118(5) 0.0526(16) Uani 1 1 d . . . . .
H12 H 0.5968 0.1767 0.5354 0.063 Uiso 1 1 calc R U . . .
C13 C 0.6088(6) 0.3063(5) 0.5036(4) 0.0491(15) Uani 1 1 d . . . . .
H13 H 0.5489 0.3157 0.5218 0.059 Uiso 1 1 calc R U . . .
C14 C 0.6681(5) 0.3746(4) 0.4688(4) 0.0376(12) Uani 1 1 d . . . . .
C15 C 0.6397(6) 0.4645(5) 0.4576(4) 0.0424(13) Uani 1 1 d . . . . .
H15A H 0.5504 0.4359 0.4151 0.051 Uiso 1 1 calc R U . . .
H15B H 0.6652 0.5174 0.5286 0.051 Uiso 1 1 calc R U . . .
C16 C 0.9597(6) 0.6867(5) 0.3482(4) 0.0460(14) Uani 1 1 d . . . . .
H16 H 1.0095 0.6554 0.3352 0.055 Uiso 1 1 calc R U . . .
C17 C 0.9756(7) 0.7812(5) 0.3375(5) 0.0518(16) Uani 1 1 d . . . . .
H17 H 1.0360 0.8153 0.3198 0.062 Uiso 1 1 calc R U . . .
C18 C 0.9004(7) 0.8238(5) 0.3535(5) 0.0536(17) Uani 1 1 d . . . . .
H18 H 0.9074 0.8883 0.3460 0.064 Uiso 1 1 calc R U . . .
C19 C 0.8158(7) 0.7732(5) 0.3801(5) 0.0517(16) Uani 1 1 d . . . . .
H19 H 0.7621 0.8012 0.3896 0.062 Uiso 1 1 calc R U . . .
C20 C 0.8085(6) 0.6809(4) 0.3931(4) 0.0414(13) Uani 1 1 d . . . . .
C21 C 0.7273(7) 0.6285(5) 0.4344(6) 0.0583(18) Uani 1 1 d . . . . .
H21A H 0.7675 0.6674 0.5123 0.070 Uiso 1 1 calc R U . . .
H21B H 0.6497 0.6332 0.4047 0.070 Uiso 1 1 calc R U . . .
Mn1 Mn 0.84934(8) 0.48559(6) 0.40186(5) 0.0339(2) Uani 1 1 d . . . . .
N1 N 0.8794(4) 0.6369(3) 0.3755(3) 0.0361(10) Uani 1 1 d . . . . .
N2 N 0.7013(5) 0.5180(4) 0.4069(4) 0.0500(13) Uani 1 1 d . . . . .
N3 N 0.7545(4) 0.3622(3) 0.4439(3) 0.0349(10) Uani 1 1 d . . . . .
N4 N 0.9765(4) 0.4461(3) 0.3801(3) 0.0356(10) Uani 1 1 d . . . . .
O1 O 0.7457(4) 0.4016(3) 0.2571(3) 0.0399(9) Uani 1 1 d . . . . .
O2 O 0.9555(4) 0.5806(3) 0.5465(3) 0.0372(9) Uani 1 1 d . . . . .
C101 C 0.8262(6) 1.0946(4) 0.2557(4) 0.0414(13) Uani 1 1 d . . . . .
C102 C 0.9146(6) 1.0949(4) 0.3412(4) 0.0461(14) Uani 1 1 d . . . . .
H102 H 0.9014 1.0925 0.3998 0.055 Uiso 1 1 calc R U . . .
C103 C 1.0225(6) 1.0988(5) 0.3421(5) 0.0514(16) Uani 1 1 d . . . . .
H103 H 1.0834 1.1004 0.4014 0.062 Uiso 1 1 calc R U . . .
C104 C 1.0399(7) 1.1001(5) 0.2560(5) 0.0554(16) Uani 1 1 d . . . . .
H104 H 1.1111 1.0980 0.2548 0.066 Uiso 1 1 calc R U . . .
C105 C 0.9580(6) 1.1045(5) 0.1726(5) 0.0509(15) Uani 1 1 d . . . . .
H105 H 0.9748 1.1095 0.1162 0.061 Uiso 1 1 calc R U . . .
C106 C 0.8475(6) 1.1015(5) 0.1696(4) 0.0449(13) Uani 1 1 d . . . . .
C107 C 0.7616(6) 1.1101(4) 0.0823(4) 0.0409(13) Uani 1 1 d . . . . .
C108 C 0.8063(6) 1.1676(5) 0.0223(4) 0.0458(14) Uani 1 1 d . . . . .
H10A H 0.8956 1.2063 0.0602 0.069 Uiso 1 1 calc R U . . .
H10B H 0.7728 1.2185 0.0163 0.069 Uiso 1 1 calc R U . . .
H10C H 0.7795 1.1155 -0.0485 0.069 Uiso 1 1 calc R U . . .
C110 C 0.4946(7) 1.1889(5) 0.1651(5) 0.0490(15) Uani 1 1 d . . . . .
H110 H 0.5415 1.2128 0.1320 0.059 Uiso 1 1 calc R U . . .
C111 C 0.4290(6) 1.2411(5) 0.1887(5) 0.0482(15) Uani 1 1 d . . . . .
H111 H 0.4308 1.3002 0.1718 0.058 Uiso 1 1 calc R U . . .
C112 C 0.3614(7) 1.2063(5) 0.2367(5) 0.0497(15) Uani 1 1 d . . . . .
H112 H 0.3143 1.2402 0.2518 0.060 Uiso 1 1 calc R U . . .
C113 C 0.3620(6) 1.1239(5) 0.2624(4) 0.0453(14) Uani 1 1 d . . . . .
H113 H 0.3171 1.1007 0.2973 0.054 Uiso 1 1 calc R U . . .
C114 C 0.4290(6) 1.0727(4) 0.2376(4) 0.0381(12) Uani 1 1 d . . . . .
C115 C 0.4344(6) 0.9813(5) 0.2647(4) 0.0431(13) Uani 1 1 d . . . . .
H11A H 0.4621 1.0040 0.3415 0.052 Uiso 1 1 calc R U . . .
H11B H 0.3510 0.9212 0.2270 0.052 Uiso 1 1 calc R U . . .
C116 C 0.6697(7) 0.8232(5) 0.0784(5) 0.0545(17) Uani 1 1 d . . . . .
H116 H 0.7104 0.8670 0.0520 0.065 Uiso 1 1 calc R U . . .
C117 C 0.6760(7) 0.7273(5) 0.0689(5) 0.0580(18) Uani 1 1 d . . . . .
H117 H 0.7174 0.7045 0.0335 0.070 Uiso 1 1 calc R U . . .
C118 C 0.6217(7) 0.6665(5) 0.1112(5) 0.0569(18) Uani 1 1 d . . . . .
H118 H 0.6245 0.6006 0.1049 0.068 Uiso 1 1 calc R U . . .
C119 C 0.5633(7) 0.7019(5) 0.1629(5) 0.0522(16) Uani 1 1 d . . . . .
H119 H 0.5281 0.6625 0.1955 0.063 Uiso 1 1 calc R U . . .
C120 C 0.5566(6) 0.7971(4) 0.1666(4) 0.0439(14) Uani 1 1 d . . . . .
C121 C 0.4822(8) 0.8318(5) 0.2113(5) 0.0585(18) Uani 1 1 d . . . . .
H12A H 0.3947 0.7886 0.1589 0.070 Uiso 1 1 calc R U . . .
H12B H 0.4941 0.8182 0.2753 0.070 Uiso 1 1 calc R U . . .
Mn2 Mn 0.57345(9) 1.00202(6) 0.13726(6) 0.0378(3) Uani 1 1 d . . . . .
N101 N 0.6065(5) 0.8553(4) 0.1247(3) 0.0393(11) Uani 1 1 d . . . . .
N102 N 0.5147(5) 0.9433(4) 0.2384(4) 0.0486(13) Uani 1 1 d . . . . .
N103 N 0.4929(5) 1.1046(4) 0.1884(4) 0.0418(11) Uani 1 1 d . . . . .
N104 N 0.6462(5) 1.0704(3) 0.0576(3) 0.0389(10) Uani 1 1 d . . . . .
O101 O 0.7243(4) 1.0893(3) 0.2577(3) 0.0430(9) Uani 1 1 d . . . . .
O102 O 0.4240(4) 0.9043(3) 0.0143(3) 0.0398(9) Uani 1 1 d . . . . .
Cl2 Cl 0.30716(16) 0.05176(12) 0.48637(13) 0.0486(4) Uani 1 1 d D . . . .
O7 O 0.4089(5) 0.0299(4) 0.5119(4) 0.0596(12) Uani 1 1 d D . . . .
O8 O 0.2216(5) -0.0142(4) 0.3775(4) 0.0751(15) Uani 1 1 d D . . . .
O9 O 0.2513(5) 0.0287(4) 0.5512(4) 0.0662(14) Uani 1 1 d D . . . .
O10 O 0.3433(5) 0.1608(3) 0.5015(4) 0.0681(15) Uani 1 1 d D . . . .
Cl1A Cl 0.3540(7) 0.4735(6) 0.2225(5) 0.0564(15) Uani 0.70(3) 1 d D U P A 1
O3A O 0.4632(9) 0.4871(11) 0.2120(10) 0.056(3) Uani 0.70(3) 1 d D U P A 1
O4A O 0.2512(8) 0.3763(11) 0.1378(7) 0.096(4) Uani 0.70(3) 1 d D U P A 1
O5A O 0.3721(15) 0.4664(11) 0.3208(9) 0.051(3) Uani 0.70(3) 1 d D U P A 1
O6A O 0.3227(19) 0.5583(14) 0.2208(11) 0.098(5) Uani 0.70(3) 1 d D U P A 1
Cl1B Cl 0.3609(14) 0.4933(15) 0.2305(13) 0.062(4) Uani 0.30(3) 1 d D U P A 2
O3B O 0.429(3) 0.475(2) 0.174(2) 0.061(7) Uani 0.30(3) 1 d D U P A 2
O4B O 0.2400(19) 0.442(4) 0.144(2) 0.124(12) Uani 0.30(3) 1 d D U P A 2
O5B O 0.376(3) 0.446(2) 0.302(2) 0.049(6) Uani 0.30(3) 1 d D U P A 2
O6B O 0.400(4) 0.6046(18) 0.278(3) 0.094(9) Uani 0.30(3) 1 d D U P A 2
C201 C 0.1981(12) 0.7277(11) 0.2397(9) 0.126(4) Uiso 1 1 d D . . . .
H20A H 0.1189 0.6851 0.2336 0.189 Uiso 1 1 calc R U . . .
H20B H 0.2387 0.7981 0.2992 0.189 Uiso 1 1 calc R U . . .
H20C H 0.2490 0.6909 0.2519 0.189 Uiso 1 1 calc R U . . .
O201 O 0.1794(12) 0.7414(10) 0.1420(9) 0.200(5) Uiso 1 1 d D . . . .
H201 H 0.1184 0.7529 0.1203 0.301 Uiso 1 1 calc R U . . .
C202 C -0.040(2) 0.8453(19) 0.0556(18) 0.272(12) Uiso 1 1 d D . . . .
H20D H -0.1224 0.8220 0.0000 0.408 Uiso 1 1 calc R U . . .
H20E H 0.0205 0.8857 0.0384 0.408 Uiso 1 1 calc R U . . .
H20F H -0.0289 0.8911 0.1234 0.408 Uiso 1 1 calc R U . . .
O202 O -0.0244(16) 0.7480(15) 0.0633(13) 0.270(7) Uiso 1 1 d D . . . .
H202 H -0.0598 0.6985 0.0024 0.405 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
C1 O1 1.350(6) . ?
C1 C2 1.393(8) . ?
C1 C6 1.402(8) . ?
C2 C3 1.377(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.357(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.413(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.463(8) . ?
C7 N4 1.312(6) . ?
C7 C8 1.500(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C10 N3 1.325(7) . ?
C10 C11 1.377(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.366(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.376(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(8) . ?
C13 H13 0.9500 . ?
C14 N3 1.355(7) . ?
C14 C15 1.499(7) . ?
C15 N2 1.466(7) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 N1 1.325(7) . ?
C16 C17 1.379(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.372(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.364(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.381(8) . ?
C19 H19 0.9500 . ?
C20 N1 1.341(7) . ?
C20 C21 1.504(9) . ?
C21 N2 1.439(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
Mn1 O1 1.870(4) . ?
Mn1 O2 1.898(4) . ?
Mn1 N4 2.024(5) . ?
Mn1 N2 2.157(5) . ?
Mn1 N3 2.199(4) . ?
Mn1 N1 2.265(4) . ?
N4 O2 1.377(5) 2_766 ?
O2 N4 1.377(5) 2_766 ?
C101 O101 1.324(7) . ?
C101 C102 1.388(8) . ?
C101 C106 1.420(8) . ?
C102 C103 1.392(9) . ?
C102 H102 0.9500 . ?
C103 C104 1.376(9) . ?
C103 H103 0.9500 . ?
C104 C105 1.360(9) . ?
C104 H104 0.9500 . ?
C105 C106 1.418(9) . ?
C105 H105 0.9500 . ?
C106 C107 1.459(8) . ?
C107 N104 1.303(8) . ?
C107 C108 1.506(8) . ?
C108 H10A 0.9800 . ?
C108 H10B 0.9800 . ?
C108 H10C 0.9800 . ?
C110 N103 1.352(7) . ?
C110 C111 1.386(8) . ?
C110 H110 0.9500 . ?
C111 C112 1.374(9) . ?
C111 H111 0.9500 . ?
C112 C113 1.349(8) . ?
C112 H112 0.9500 . ?
C113 C114 1.398(7) . ?
C113 H113 0.9500 . ?
C114 N103 1.341(7) . ?
C114 C115 1.498(7) . ?
C115 N102 1.453(7) . ?
C115 H11A 0.9900 . ?
C115 H11B 0.9900 . ?
C116 N101 1.359(7) . ?
C116 C117 1.393(8) . ?
C116 H116 0.9500 . ?
C117 C118 1.369(10) . ?
C117 H117 0.9500 . ?
C118 C119 1.376(9) . ?
C118 H118 0.9500 . ?
C119 C120 1.401(8) . ?
C119 H119 0.9500 . ?
C120 N101 1.315(7) . ?
C120 C121 1.494(8) . ?
C121 N102 1.436(8) . ?
C121 H12A 0.9900 . ?
C121 H12B 0.9900 . ?
Mn2 O101 1.864(4) . ?
Mn2 O102 1.890(4) . ?
Mn2 N104 2.020(5) . ?
Mn2 N102 2.148(5) . ?
Mn2 N103 2.209(4) . ?
Mn2 N101 2.279(4) . ?
N104 O102 1.364(6) 2_675 ?
O102 N104 1.364(6) 2_675 ?
Cl2 O7 1.416(5) . ?
Cl2 O8 1.426(6) . ?
Cl2 O10 1.429(4) . ?
Cl2 O9 1.440(4) . ?
Cl1A O6A 1.419(8) . ?
Cl1A O5A 1.431(7) . ?
Cl1A O4A 1.438(9) . ?
Cl1A O3A 1.449(8) . ?
Cl1B O5B 1.407(13) . ?
Cl1B O6B 1.411(14) . ?
Cl1B O4B 1.429(15) . ?
Cl1B O3B 1.467(13) . ?
C201 O201 1.461(11) . ?
C201 H20A 0.9800 . ?
C201 H20B 0.9800 . ?
C201 H20C 0.9800 . ?
O201 H201 0.8400 . ?
C202 O202 1.519(16) . ?
C202 H20D 0.9800 . ?
C202 H20E 0.9800 . ?
C202 H20F 0.9800 . ?
O202 H202 0.8400 . ?

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
O1 C1 C2 118.8(6) . . ?
O1 C1 C6 121.7(5) . . ?
C2 C1 C6 119.4(5) . . ?
C3 C2 C1 120.6(7) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 120.5(6) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 119.5(6) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 121.7(7) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C5 118.2(5) . . ?
C1 C6 C7 122.3(5) . . ?
C5 C6 C7 119.6(6) . . ?
N4 C7 C6 118.8(5) . . ?
N4 C7 C8 119.9(5) . . ?
C6 C7 C8 121.3(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C10 C11 122.6(6) . . ?
N3 C10 H10 118.7 . . ?
C11 C10 H10 118.7 . . ?
C12 C11 C10 118.5(5) . . ?
C12 C11 H11 120.7 . . ?
C10 C11 H11 120.7 . . ?
C11 C12 C13 119.7(6) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C12 C13 C14 119.4(6) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
N3 C14 C13 120.6(5) . . ?
N3 C14 C15 118.0(5) . . ?
C13 C14 C15 121.4(5) . . ?
N2 C15 C14 112.2(4) . . ?
N2 C15 H15A 109.2 . . ?
C14 C15 H15A 109.2 . . ?
N2 C15 H15B 109.2 . . ?
C14 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
N1 C16 C17 124.2(6) . . ?
N1 C16 H16 117.9 . . ?
C17 C16 H16 117.9 . . ?
C18 C17 C16 117.3(6) . . ?
C18 C17 H17 121.4 . . ?
C16 C17 H17 121.4 . . ?
C19 C18 C17 119.6(5) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C18 C19 C20 119.6(6) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
N1 C20 C19 121.4(6) . . ?
N1 C20 C21 116.4(5) . . ?
C19 C20 C21 122.0(5) . . ?
N2 C21 C20 111.7(5) . . ?
N2 C21 H21A 109.3 . . ?
C20 C21 H21A 109.3 . . ?
N2 C21 H21B 109.3 . . ?
C20 C21 H21B 109.3 . . ?
H21A C21 H21B 107.9 . . ?
O1 Mn1 O2 175.41(14) . . ?
O1 Mn1 N4 87.06(16) . . ?
O2 Mn1 N4 94.35(16) . . ?
O1 Mn1 N2 86.76(19) . . ?
O2 Mn1 N2 91.79(18) . . ?
N4 Mn1 N2 173.81(19) . . ?
O1 Mn1 N3 92.35(16) . . ?
O2 Mn1 N3 91.55(15) . . ?
N4 Mn1 N3 103.97(16) . . ?
N2 Mn1 N3 76.60(17) . . ?
O1 Mn1 N1 90.67(15) . . ?
O2 Mn1 N1 84.75(15) . . ?
N4 Mn1 N1 104.91(17) . . ?
N2 Mn1 N1 74.87(18) . . ?
N3 Mn1 N1 151.08(17) . . ?
C16 N1 C20 117.8(4) . . ?
C16 N1 Mn1 127.7(3) . . ?
C20 N1 Mn1 114.5(4) . . ?
C21 N2 C15 115.9(4) . . ?
C21 N2 Mn1 113.8(4) . . ?
C15 N2 Mn1 115.2(3) . . ?
C10 N3 C14 119.3(5) . . ?
C10 N3 Mn1 125.1(4) . . ?
C14 N3 Mn1 115.6(3) . . ?
C7 N4 O2 115.4(4) . 2_766 ?
C7 N4 Mn1 125.1(4) . . ?
O2 N4 Mn1 118.4(3) 2_766 . ?
C1 O1 Mn1 118.1(4) . . ?
N4 O2 Mn1 123.9(2) 2_766 . ?
O101 C101 C102 118.6(5) . . ?
O101 C101 C106 121.8(5) . . ?
C102 C101 C106 119.6(6) . . ?
C101 C102 C103 120.7(6) . . ?
C101 C102 H102 119.7 . . ?
C103 C102 H102 119.7 . . ?
C104 C103 C102 119.3(6) . . ?
C104 C103 H103 120.4 . . ?
C102 C103 H103 120.4 . . ?
C105 C104 C103 121.9(7) . . ?
C105 C104 H104 119.0 . . ?
C103 C104 H104 119.0 . . ?
C104 C105 C106 120.1(6) . . ?
C104 C105 H105 119.9 . . ?
C106 C105 H105 119.9 . . ?
C105 C106 C101 118.2(5) . . ?
C105 C106 C107 120.3(5) . . ?
C101 C106 C107 121.4(6) . . ?
N104 C107 C106 120.1(5) . . ?
N104 C107 C108 119.8(5) . . ?
C106 C107 C108 120.1(6) . . ?
C107 C108 H10A 109.5 . . ?
C107 C108 H10B 109.5 . . ?
H10A C108 H10B 109.5 . . ?
C107 C108 H10C 109.5 . . ?
H10A C108 H10C 109.5 . . ?
H10B C108 H10C 109.5 . . ?
N103 C110 C111 121.2(6) . . ?
N103 C110 H110 119.4 . . ?
C111 C110 H110 119.4 . . ?
C112 C111 C110 119.2(5) . . ?
C112 C111 H111 120.4 . . ?
C110 C111 H111 120.4 . . ?
C113 C112 C111 119.7(5) . . ?
C113 C112 H112 120.2 . . ?
C111 C112 H112 120.2 . . ?
C112 C113 C114 119.9(5) . . ?
C112 C113 H113 120.1 . . ?
C114 C113 H113 120.1 . . ?
N103 C114 C113 120.8(5) . . ?
N103 C114 C115 116.7(5) . . ?
C113 C114 C115 122.5(5) . . ?
N102 C115 C114 114.3(5) . . ?
N102 C115 H11A 108.7 . . ?
C114 C115 H11A 108.7 . . ?
N102 C115 H11B 108.7 . . ?
C114 C115 H11B 108.7 . . ?
H11A C115 H11B 107.6 . . ?
N101 C116 C117 121.5(6) . . ?
N101 C116 H116 119.3 . . ?
C117 C116 H116 119.3 . . ?
C118 C117 C116 119.2(6) . . ?
C118 C117 H117 120.4 . . ?
C116 C117 H117 120.4 . . ?
C117 C118 C119 119.2(5) . . ?
C117 C118 H118 120.4 . . ?
C119 C118 H118 120.4 . . ?
C118 C119 C120 118.8(6) . . ?
C118 C119 H119 120.6 . . ?
C120 C119 H119 120.6 . . ?
N101 C120 C119 122.5(5) . . ?
N101 C120 C121 117.0(5) . . ?
C119 C120 C121 120.3(6) . . ?
N102 C121 C120 112.1(5) . . ?
N102 C121 H12A 109.2 . . ?
C120 C121 H12A 109.2 . . ?
N102 C121 H12B 109.2 . . ?
C120 C121 H12B 109.2 . . ?
H12A C121 H12B 107.9 . . ?
O101 Mn2 O102 175.35(15) . . ?
O101 Mn2 N104 87.54(18) . . ?
O102 Mn2 N104 93.42(17) . . ?
O101 Mn2 N102 85.9(2) . . ?
O102 Mn2 N102 93.2(2) . . ?
N104 Mn2 N102 173.4(2) . . ?
O101 Mn2 N103 92.33(18) . . ?
O102 Mn2 N103 91.90(18) . . ?
N104 Mn2 N103 102.51(17) . . ?
N102 Mn2 N103 76.62(16) . . ?
O101 Mn2 N101 91.21(17) . . ?
O102 Mn2 N101 84.15(16) . . ?
N104 Mn2 N101 106.89(17) . . ?
N102 Mn2 N101 74.44(16) . . ?
N103 Mn2 N101 150.50(18) . . ?
C120 N101 C116 118.6(5) . . ?
C120 N101 Mn2 114.4(4) . . ?
C116 N101 Mn2 126.9(4) . . ?
C121 N102 C115 116.7(5) . . ?
C121 N102 Mn2 113.9(3) . . ?
C115 N102 Mn2 114.5(3) . . ?
C114 N103 C110 119.3(5) . . ?
C114 N103 Mn2 115.7(3) . . ?
C110 N103 Mn2 124.7(4) . . ?
C107 N104 O102 115.9(4) . 2_675 ?
C107 N104 Mn2 124.9(4) . . ?
O102 N104 Mn2 118.0(4) 2_675 . ?
C101 O101 Mn2 120.7(3) . . ?
N104 O102 Mn2 126.0(3) 2_675 . ?
O7 Cl2 O8 108.9(3) . . ?
O7 Cl2 O10 110.8(3) . . ?
O8 Cl2 O10 107.7(3) . . ?
O7 Cl2 O9 109.2(3) . . ?
O8 Cl2 O9 109.8(3) . . ?
O10 Cl2 O9 110.4(3) . . ?
O6A Cl1A O5A 108.0(7) . . ?
O6A Cl1A O4A 107.2(8) . . ?
O5A Cl1A O4A 108.7(8) . . ?
O6A Cl1A O3A 114.0(8) . . ?
O5A Cl1A O3A 108.7(7) . . ?
O4A Cl1A O3A 110.2(7) . . ?
O5B Cl1B O6B 113.9(16) . . ?
O5B Cl1B O4B 113.9(17) . . ?
O6B Cl1B O4B 110.1(17) . . ?
O5B Cl1B O3B 108.9(14) . . ?
O6B Cl1B O3B 108.5(15) . . ?
O4B Cl1B O3B 100.7(15) . . ?
O201 C201 H20A 109.5 . . ?
O201 C201 H20B 109.5 . . ?
H20A C201 H20B 109.5 . . ?
O201 C201 H20C 109.5 . . ?
H20A C201 H20C 109.5 . . ?
H20B C201 H20C 109.5 . . ?
C201 O201 H201 109.5 . . ?
O202 C202 H20D 109.5 . . ?
O202 C202 H20E 109.5 . . ?
H20D C202 H20E 109.5 . . ?
O202 C202 H20F 109.5 . . ?
H20D C202 H20F 109.5 . . ?
H20E C202 H20F 109.5 . . ?
C202 O202 H202 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
O201 H201 O202 0.84 1.73 2.56(2) 168.2 .
C202 H20D O4A 0.98 2.60 3.20(3) 119.6 2_565
O202 H202 O4B 0.84 2.35 3.10(4) 149.8 2_565
C11 H11 O9 0.95 2.61 3.531(7) 163.1 2_656
C13 H13 O6B 0.95 2.63 3.21(3) 120.1 2_666
C15 H15A O5A 0.99 2.52 3.402(15) 148.9 .
C15 H15A O5B 0.99 2.39 3.30(3) 151.7 .
C15 H15B O5A 0.99 2.42 3.250(12) 141.4 2_666
C17 H17 O8 0.95 2.52 3.346(9) 144.8 1_665
C19 H19 O9 0.95 2.48 3.285(7) 142.5 2_666
C19 H19 O10 0.95 2.53 3.359(8) 146.3 2_666
C102 H102 O9 0.95 2.65 3.448(8) 141.4 2_666
C110 H110 O102 0.95 2.65 3.326(7) 128.1 2_675
C111 H111 O3A 0.95 2.48 3.360(14) 154.6 1_565
C111 H111 O3B 0.95 2.53 3.45(3) 163.7 1_565
C113 H113 O8 0.95 2.55 3.452(8) 159.1 1_565
C115 H11A O7 0.99 2.52 3.317(7) 137.0 2_666
C115 H11B O201 0.99 2.45 3.411(14) 162.7 .
C119 H119 O3A 0.95 2.52 3.347(14) 145.5 .
C119 H119 O3B 0.95 2.49 3.28(3) 140.3 .
C119 H119 O6B 0.95 2.47 3.37(3) 158.6 .
C121 H12A O201 0.99 2.58 3.414(15) 141.5 .
C201 H20C O6A 0.98 2.43 3.366(15) 160.5 .
C201 H20C O6B 0.98 2.64 3.61(3) 173.9 .
O201 H201 O202 0.84 1.73 2.56(2) 168.2 .
C202 H20D O4A 0.98 2.60 3.20(3) 119.6 2_565
O202 H202 O4B 0.84 2.35 3.10(4) 149.8 2_565

_refine_diff_density_max         1.443
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.126

_shelxl_version_number           2013-3

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1044302'
_audit_update_record             
;
2015-01-19 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;
# local name eb4070
_audit_creation_date             2014-04-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4813)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C42 H44 Mn2 N8 O4, 2(Cl O4)'
_chemical_formula_sum            'C46 H60 Cl2 Mn2 N8 O16'
_chemical_formula_weight         1161.80
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H30 N5 O10 Mn1 Cl1'
_chemical_oxdiff_usercomment     '@ 120 K PC865'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
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                   25.9020(12)
_cell_length_b                   10.4638(4)
_cell_length_c                   21.9889(11)
_cell_angle_alpha                90
_cell_angle_beta                 103.471(5)
_cell_angle_gamma                90
_cell_volume                     5795.8(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9405
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.1300
_cell_measurement_theta_min      3.3850
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.3641
_exptl_crystal_size_mid          0.1467
_exptl_crystal_size_min          0.1093
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28756
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.965
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0261085000
_diffrn_orient_matrix_UB_12      0.0177232000
_diffrn_orient_matrix_UB_13      0.0014959000
_diffrn_orient_matrix_UB_21      -0.0072995000
_diffrn_orient_matrix_UB_22      0.0046637000
_diffrn_orient_matrix_UB_23      -0.0330817000
_diffrn_orient_matrix_UB_31      -0.0076161000
_diffrn_orient_matrix_UB_32      -0.0652490000
_diffrn_orient_matrix_UB_33      -0.0019565000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4983
_reflns_number_total             5895
_reflns_odcompleteness_completeness 99.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_refine_diff_density_max         0.806
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5895
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0492
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0632P)²+12.0531P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1359
_refine_special_details          
;
SQUEEZE was used to remove four molecules of methanol per asymmetric unit, 
which could not be modelled with discrete atoms. This solvent was included 
in the total chemical formula and thus triggers a lot of checkCIF alerts, 
which should be ignored.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 

#===============================================================================
041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ     Please Check
068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...     Please Check

Consequence of SQUEEZE.

761_ALERT_1_C CIF Contains no X-H Bonds ......................     Please Check
762_ALERT_1_C CIF Contains no X-Y-H or H-Y-H Angles ..........     Please Check
906_ALERT_3_C Large K value in the Analysis of Variance ......      3.292 Check
910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          8 Why ?
911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          4 Why ?
975_ALERT_2_C Check Calcd Residual Density  0.92A From      O1       0.43 eA-3
976_ALERT_2_C Check Calcd Residual Density  1.02A From      N3      -0.41 eA-3
#===============================================================================




;


# start Validation Reply Form
_vrf_CHEMW03_eb4070              
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: SQUEEZE was used.  Please see the _refine_special_details part of 
the CIF.
;
# end Validation Reply Form


_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16),
 C17(H17), C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.43724(2) 0.85974(3) 0.18538(2) 0.01703(13) Uani 1 1 d . . . . .
O1 O 0.41919(8) 0.89253(17) 0.09991(8) 0.0242(4) Uani 1 1 d . . . . .
O2 O 0.54937(7) 0.82907(16) 0.22681(8) 0.0191(4) Uani 1 1 d . . . . .
N1 N 0.51295(8) 0.90287(19) 0.18605(10) 0.0172(4) Uani 1 1 d . . . . .
N2 N 0.39610(9) 1.0427(2) 0.20141(11) 0.0242(5) Uani 1 1 d . . . . .
N3 N 0.35854(9) 0.7996(2) 0.17980(12) 0.0252(5) Uani 1 1 d . . . . .
H3 H 0.3581(14) 0.772(3) 0.2160(17) 0.034(9) Uiso 1 1 d . . . . .
N4 N 0.43924(9) 0.6505(2) 0.16495(11) 0.0220(5) Uani 1 1 d . . . . .
C1 C 0.43817(11) 0.9959(2) 0.07625(12) 0.0231(6) Uani 1 1 d . . . . .
C2 C 0.40379(13) 1.0669(3) 0.03021(13) 0.0298(6) Uani 1 1 d . . . . .
H2 H 0.3680 1.0451 0.0187 0.036 Uiso 1 1 calc R . . . .
C3 C 0.42223(14) 1.1691(3) 0.00158(13) 0.0333(7) Uani 1 1 d . . . . .
H3A H 0.3985 1.2152 -0.0288 0.040 Uiso 1 1 calc R . . . .
C4 C 0.47518(14) 1.2045(3) 0.01692(13) 0.0321(7) Uani 1 1 d . . . . .
C5 C 0.50955(12) 1.1361(2) 0.06344(13) 0.0267(6) Uani 1 1 d . . . . .
H5 H 0.5452 1.1591 0.0745 0.032 Uiso 1 1 calc R . . . .
C6 C 0.49196(11) 1.0327(2) 0.09439(12) 0.0220(6) Uani 1 1 d . . . . .
C7 C 0.53030(11) 0.9633(2) 0.14305(12) 0.0197(5) Uani 1 1 d . . . . .
C8 C 0.58800(11) 0.9599(3) 0.14314(13) 0.0266(6) Uani 1 1 d . . . . .
H8A H 0.6073 1.0143 0.1757 0.040 Uiso 1 1 calc GR . . . .
H8B H 0.5928 0.9892 0.1035 0.040 Uiso 1 1 calc GR . . . .
H8C H 0.6009 0.8739 0.1503 0.040 Uiso 1 1 calc GR . . . .
C9 C 0.49568(17) 1.3141(3) -0.01609(17) 0.0476(9) Uani 1 1 d . . . . .
H9A H 0.5178 1.3685 0.0143 0.071 Uiso 1 1 calc GR . . . .
H9B H 0.4662 1.3625 -0.0396 0.071 Uiso 1 1 calc GR . . . .
H9C H 0.5159 1.2807 -0.0439 0.071 Uiso 1 1 calc GR . . . .
C10 C 0.41859(12) 1.1538(3) 0.22491(15) 0.0312(7) Uani 1 1 d . . . . .
H10 H 0.4547 1.1652 0.2279 0.037 Uiso 1 1 calc R . . . .
C11 C 0.39079(14) 1.2509(3) 0.24474(17) 0.0419(8) Uani 1 1 d . . . . .
H11 H 0.4077 1.3260 0.2611 0.050 Uiso 1 1 calc R . . . .
C12 C 0.33723(14) 1.2339(3) 0.23971(17) 0.0417(8) Uani 1 1 d . . . . .
H12 H 0.3173 1.2978 0.2528 0.050 Uiso 1 1 calc R . . . .
C13 C 0.31319(13) 1.1214(3) 0.21509(16) 0.0389(8) Uani 1 1 d . . . . .
H13 H 0.2770 1.1087 0.2113 0.047 Uiso 1 1 calc R . . . .
C14 C 0.34388(11) 1.0277(3) 0.19609(14) 0.0280(6) Uani 1 1 d . . . . .
C15 C 0.32010(12) 0.9058(3) 0.16518(17) 0.0358(7) Uani 1 1 d . . . . .
H15A H 0.2885 0.8846 0.1796 0.043 Uiso 1 1 calc R . . . .
H15B H 0.3098 0.9181 0.1203 0.043 Uiso 1 1 calc R . . . .
C16 C 0.48179(12) 0.5771(3) 0.16694(13) 0.0256(6) Uani 1 1 d . . . . .
H16 H 0.5153 0.6109 0.1837 0.031 Uiso 1 1 calc R . . . .
C17 C 0.47793(13) 0.4527(3) 0.14505(14) 0.0318(7) Uani 1 1 d . . . . .
H17 H 0.5083 0.4041 0.1464 0.038 Uiso 1 1 calc R . . . .
C18 C 0.42800(15) 0.4021(3) 0.12108(16) 0.0404(8) Uani 1 1 d . . . . .
H18 H 0.4242 0.3185 0.1064 0.049 Uiso 1 1 calc R . . . .
C19 C 0.38415(13) 0.4771(3) 0.11926(16) 0.0375(8) Uani 1 1 d . . . . .
H19 H 0.3503 0.4446 0.1033 0.045 Uiso 1 1 calc R . . . .
C20 C 0.39066(12) 0.6018(3) 0.14139(14) 0.0279(6) Uani 1 1 d . . . . .
C21 C 0.34446(12) 0.6915(3) 0.13638(17) 0.0362(7) Uani 1 1 d . . . . .
H21A H 0.3336 0.7235 0.0939 0.043 Uiso 1 1 calc R . . . .
H21B H 0.3147 0.6455 0.1458 0.043 Uiso 1 1 calc R . . . .
Cl1 Cl 0.34611(3) 0.58918(7) 0.31746(4) 0.0348(2) Uani 1 1 d . . . . .
O3 O 0.31834(10) 0.7010(2) 0.28843(13) 0.0514(7) Uani 1 1 d . . . . .
O4 O 0.30885(9) 0.4884(2) 0.31878(12) 0.0453(6) Uani 1 1 d . . . . .
O5 O 0.38263(11) 0.5506(2) 0.28098(17) 0.0670(9) Uani 1 1 d . . . . .
O6 O 0.37345(17) 0.6217(3) 0.37829(15) 0.0923(12) 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
Mn1 O1 1.8596(18) . ?
Mn1 O2 1.9080(18) 2_655 ?
Mn1 N1 2.009(2) . ?
Mn1 N2 2.258(2) . ?
Mn1 N3 2.110(2) . ?
Mn1 N4 2.238(2) . ?
O1 C1 1.342(3) . ?
O2 Mn1 1.9079(18) 2_655 ?
O2 N1 1.377(3) . ?
N1 C7 1.301(3) . ?
N2 C10 1.348(4) . ?
N2 C14 1.339(4) . ?
N3 C15 1.477(4) . ?
N3 C21 1.470(4) . ?
N4 C16 1.336(4) . ?
N4 C20 1.345(4) . ?
C1 C2 1.396(4) . ?
C1 C6 1.410(4) . ?
C2 C3 1.381(4) . ?
C3 C4 1.384(5) . ?
C4 C5 1.388(4) . ?
C4 C9 1.518(4) . ?
C5 C6 1.409(4) . ?
C6 C7 1.471(4) . ?
C7 C8 1.494(4) . ?
C10 C11 1.374(4) . ?
C11 C12 1.377(5) . ?
C12 C13 1.382(5) . ?
C13 C14 1.387(4) . ?
C14 C15 1.508(4) . ?
C16 C17 1.383(4) . ?
C17 C18 1.383(5) . ?
C18 C19 1.373(5) . ?
C19 C20 1.389(4) . ?
C20 C21 1.505(4) . ?
Cl1 O3 1.442(3) . ?
Cl1 O4 1.434(2) . ?
Cl1 O5 1.433(3) . ?
Cl1 O6 1.402(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 O2 175.88(8) . 2_655 ?
O1 Mn1 N1 88.93(8) . . ?
O1 Mn1 N2 89.12(8) . . ?
O1 Mn1 N3 89.10(10) . . ?
O1 Mn1 N4 89.41(8) . . ?
O2 Mn1 N1 94.78(8) 2_655 . ?
O2 Mn1 N2 88.04(8) 2_655 . ?
O2 Mn1 N3 87.36(9) 2_655 . ?
O2 Mn1 N4 91.80(8) 2_655 . ?
N1 Mn1 N2 107.67(8) . . ?
N1 Mn1 N3 174.76(9) . . ?
N1 Mn1 N4 98.81(8) . . ?
N3 Mn1 N2 77.14(9) . . ?
N3 Mn1 N4 76.32(9) . . ?
N4 Mn1 N2 153.44(9) . . ?
C1 O1 Mn1 120.78(16) . . ?
N1 O2 Mn1 119.99(14) . 2_655 ?
O2 N1 Mn1 113.48(14) . . ?
C7 N1 Mn1 127.26(18) . . ?
C7 N1 O2 116.4(2) . . ?
C10 N2 Mn1 127.84(19) . . ?
C14 N2 Mn1 112.99(18) . . ?
C14 N2 C10 118.2(2) . . ?
C15 N3 Mn1 112.41(18) . . ?
C21 N3 Mn1 110.95(18) . . ?
C21 N3 C15 112.6(2) . . ?
C16 N4 Mn1 127.86(19) . . ?
C16 N4 C20 119.0(2) . . ?
C20 N4 Mn1 112.66(18) . . ?
O1 C1 C2 118.7(3) . . ?
O1 C1 C6 122.5(2) . . ?
C2 C1 C6 118.7(3) . . ?
C3 C2 C1 120.8(3) . . ?
C2 C3 C4 121.6(3) . . ?
C3 C4 C5 118.1(3) . . ?
C3 C4 C9 121.5(3) . . ?
C5 C4 C9 120.4(3) . . ?
C4 C5 C6 121.8(3) . . ?
C1 C6 C7 121.7(2) . . ?
C5 C6 C1 118.8(2) . . ?
C5 C6 C7 119.4(2) . . ?
N1 C7 C6 118.6(2) . . ?
N1 C7 C8 120.1(2) . . ?
C6 C7 C8 121.2(2) . . ?
N2 C10 C11 123.2(3) . . ?
C10 C11 C12 118.1(3) . . ?
C11 C12 C13 119.7(3) . . ?
C12 C13 C14 118.9(3) . . ?
N2 C14 C13 121.9(3) . . ?
N2 C14 C15 115.9(2) . . ?
C13 C14 C15 122.1(3) . . ?
N3 C15 C14 110.8(2) . . ?
N4 C16 C17 122.5(3) . . ?
C16 C17 C18 118.6(3) . . ?
C19 C18 C17 119.1(3) . . ?
C18 C19 C20 119.6(3) . . ?
N4 C20 C19 121.2(3) . . ?
N4 C20 C21 116.6(2) . . ?
C19 C20 C21 122.1(3) . . ?
N3 C21 C20 111.1(2) . . ?
O4 Cl1 O3 109.66(15) . . ?
O5 Cl1 O3 107.88(17) . . ?
O5 Cl1 O4 109.83(15) . . ?
O6 Cl1 O3 108.32(19) . . ?
O6 Cl1 O4 110.6(2) . . ?
O6 Cl1 O5 110.5(2) . . ?

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
N3 H3 O3 0.85(4) 2.22(4) 3.002(4) 154(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
Mn1 O1 C1 C2 -137.2(2) . . . . ?
Mn1 O1 C1 C6 45.3(3) . . . . ?
Mn1 O2 N1 Mn1 -74.91(17) 2_655 . . . ?
Mn1 O2 N1 C7 122.70(19) 2_655 . . . ?
Mn1 N1 C7 C6 14.1(3) . . . . ?
Mn1 N1 C7 C8 -164.98(18) . . . . ?
Mn1 N2 C10 C11 -166.3(2) . . . . ?
Mn1 N2 C14 C13 168.1(2) . . . . ?
Mn1 N2 C14 C15 -15.0(3) . . . . ?
Mn1 N3 C15 C14 -35.7(3) . . . . ?
Mn1 N3 C21 C20 37.9(3) . . . . ?
Mn1 N4 C16 C17 -170.8(2) . . . . ?
Mn1 N4 C20 C19 172.7(2) . . . . ?
Mn1 N4 C20 C21 -3.3(3) . . . . ?
O1 C1 C2 C3 -175.8(2) . . . . ?
O1 C1 C6 C5 174.7(2) . . . . ?
O1 C1 C6 C7 -3.2(4) . . . . ?
O2 N1 C7 C6 173.7(2) . . . . ?
O2 N1 C7 C8 -5.4(3) . . . . ?
N1 Mn1 O1 C1 -44.4(2) . . . . ?
N2 Mn1 O1 C1 63.3(2) . . . . ?
N2 C10 C11 C12 -0.6(5) . . . . ?
N2 C14 C15 N3 33.5(4) . . . . ?
N3 Mn1 O1 C1 140.4(2) . . . . ?
N4 Mn1 O1 C1 -143.2(2) . . . . ?
N4 C16 C17 C18 -1.0(4) . . . . ?
N4 C20 C21 N3 -22.3(4) . . . . ?
C1 C2 C3 C4 0.4(4) . . . . ?
C1 C6 C7 N1 -27.0(4) . . . . ?
C1 C6 C7 C8 152.1(3) . . . . ?
C2 C1 C6 C5 -2.8(4) . . . . ?
C2 C1 C6 C7 179.3(2) . . . . ?
C2 C3 C4 C5 -1.6(4) . . . . ?
C2 C3 C4 C9 178.0(3) . . . . ?
C3 C4 C5 C6 0.5(4) . . . . ?
C4 C5 C6 C1 1.7(4) . . . . ?
C4 C5 C6 C7 179.6(2) . . . . ?
C5 C6 C7 N1 155.1(2) . . . . ?
C5 C6 C7 C8 -25.7(4) . . . . ?
C6 C1 C2 C3 1.8(4) . . . . ?
C9 C4 C5 C6 -179.1(3) . . . . ?
C10 N2 C14 C13 -1.3(4) . . . . ?
C10 N2 C14 C15 175.7(3) . . . . ?
C10 C11 C12 C13 -0.2(5) . . . . ?
C11 C12 C13 C14 0.2(5) . . . . ?
C12 C13 C14 N2 0.6(5) . . . . ?
C12 C13 C14 C15 -176.2(3) . . . . ?
C13 C14 C15 N3 -149.6(3) . . . . ?
C14 N2 C10 C11 1.3(4) . . . . ?
C15 N3 C21 C20 164.9(3) . . . . ?
C16 N4 C20 C19 0.0(4) . . . . ?
C16 N4 C20 C21 -176.1(3) . . . . ?
C16 C17 C18 C19 0.6(5) . . . . ?
C17 C18 C19 C20 0.0(5) . . . . ?
C18 C19 C20 N4 -0.3(5) . . . . ?
C18 C19 C20 C21 175.5(3) . . . . ?
C19 C20 C21 N3 161.7(3) . . . . ?
C20 N4 C16 C17 0.7(4) . . . . ?
C21 N3 C15 C14 -162.0(3) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-10 0 -27 0.0710 -9.9997 -0.0000 -26.9998 0.2207 0.9662 0.1290
10 0 27 0.0710 9.9997 0.0000 26.9998 -0.2207 -0.9662 -0.1290
-9 -14 3 0.1716 -8.9999 -14.0001 3.0001 -0.0087 -0.0988 0.9762
9 14 -3 0.1716 8.9999 14.0001 -3.0001 0.0087 0.0988 -0.9762
35 0 0 0.0410 34.9989 0.0001 -0.0003 -0.9138 -0.2555 -0.2666
-35 -1 0 0.0653 -34.9989 -1.0001 0.0003 0.8960 0.2508 0.3318
1 -8 25 0.1276 0.9999 -8.0001 24.9999 -0.1305 -0.8716 0.4655
15 -13 0 0.1536 14.9994 -13.0001 -0.0001 -0.6220 -0.1701 0.7340
34 0 -17 0.0405 33.9989 0.0001 -17.0002 -0.9131 0.3142 -0.2257
-34 0 17 0.0708 -33.9989 -0.0001 17.0002 0.9131 -0.3142 0.2257
21 -11 -14 0.1416 20.9992 -11.0001 -14.0001 -0.7642 0.2586 0.5852
-33 3 -4 0.0738 -32.9990 3.0000 -3.9997 0.9087 0.3872 0.0634
19 5 20 0.0897 18.9995 5.0001 19.9997 -0.3775 -0.7770 -0.5101
-17 0 30 0.0675 -16.9994 -0.0000 30.0000 0.4887 -0.8684 0.0708
17 0 -30 0.0675 16.9994 0.0000 -30.0000 -0.4887 0.8684 -0.0708
15 3 -30 0.0696 14.9995 3.0001 -30.0000 -0.3833 0.8970 -0.2513
-35 3 12 0.0723 -34.9989 3.0000 12.0002 0.9849 -0.1275 0.0473
-11 4 -25 0.0758 -10.9996 4.0000 -24.9998 0.3207 0.9260 -0.1283

####################################################################### 
# 
# 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 1044303'
_audit_update_record             
;
2015-01-19 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;
# local name eb3260
_audit_creation_date             2013-12-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C38 H36 Mn2 N8 O4, 2(Cl1 O4)'
_chemical_formula_sum            'C40 H44 Cl2 Mn2 N8 O14'
_chemical_formula_weight         1041.61
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H40 N4 O20 Mn3 Cl4'
_chemical_oxdiff_usercomment     '@ 120 K PC152b'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.2526(7)
_cell_length_b                   22.2504(12)
_cell_length_c                   15.7127(11)
_cell_angle_alpha                90
_cell_angle_beta                 116.936(8)
_cell_angle_gamma                90
_cell_volume                     4442.3(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4853
_cell_measurement_temperature    120
_cell_measurement_theta_max      51.9940
_cell_measurement_theta_min      3.4640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.388
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.0705
_exptl_crystal_size_min          0.0264
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.600
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19662
_diffrn_reflns_point_group_measured_fraction_full 0.600
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         52.004
_diffrn_reflns_theta_min         3.478
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.3147
_diffrn_measured_fraction_theta_full 0.600
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0315335000
_diffrn_orient_matrix_UB_12      0.0667725000
_diffrn_orient_matrix_UB_13      -0.0175412000
_diffrn_orient_matrix_UB_21      -0.1081829000
_diffrn_orient_matrix_UB_22      -0.0152547000
_diffrn_orient_matrix_UB_23      -0.0058748000
_diffrn_orient_matrix_UB_31      0.0447155000
_diffrn_orient_matrix_UB_32      0.0100507000
_diffrn_orient_matrix_UB_33      0.1084215000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3243
_reflns_number_total             4819
_reflns_odcompleteness_completeness 98.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         4819
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0692
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1144P)²+3.1849P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1739
_refine_ls_wR_factor_ref         0.2073
_refine_special_details          
;
The crystals were of generally poor quality and the diffraction pattern 
obtained quite weak. The resolution of the data set was cut at 1 A during 
integration. One of the perchlorate ions was modelled over two sites as 
evidenced by residual peaks in an difference Fourier map. and by 
significantly elongated ellipsoids. When the bulk of the structure had been 
identified there remained density corresponding to two molecules of methanol 
per asymmetric unit. This was badly disordered as a result ot the crystal 
drying out, and so was removed using the SQUEEZE routine of PLATON.


#===============================================================================
The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<<
#===============================================================================
     Format: alert-number_ALERT_alert-type_alert-level text
 
023_ALERT_3_A Resolution (too) Low [sin(theta)/Lambda < 0.6]..      52.00 Deg.

Data cut at 1 A as described above.

#===============================================================================
019_ALERT_1_B Check _diffrn_measured_fraction_theta_full/_max       0.618
088_ALERT_3_B Poor Data / Parameter Ratio ....................       7.97
341_ALERT_3_B Low Bond Precision on  C-C Bonds ...............     0.0153 Ang.

Weak data, cut at 1 A as described above.

#===============================================================================
041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ     Please Check
051_ALERT_1_C Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .       1.12 %
068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...     Please Check

This is because SQUEEZE was used.

234_ALERT_4_C Large Hirshfeld Difference C6     --  C7      ..       0.16 Ang.
241_ALERT_2_C High      Ueq as Compared to Neighbors for .....         C3 Check
241_ALERT_2_C High      Ueq as Compared to Neighbors for .....         C4 Check
241_ALERT_2_C High      Ueq as Compared to Neighbors for .....        C32 Check
241_ALERT_2_C High      Ueq as Compared to Neighbors for .....        C38 Check

Noted, but not changed.

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

;

# start Validation Reply Form
_vrf_THETM01_eb3260              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Please see the _refine_special_details section of the CIF.
;
# end Validation Reply Form


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.500 0.500 0.000 272 69 ' '
2 0.500 0.000 0.500 272 69 ' '
_platon_squeeze_details          '2 MeOH per asymmetric unit removed'


_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H) groups
2. Rigid bond restraints
 Cl2', O9', O10', O11', O12'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Cl2' \\sim O9' \\sim O10' \\sim O11' \\sim O12': within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 Cl2', O10'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{Cl2, O9, O10, O11, O12}
as
{Cl2', O9', O10', O11', O12'}
6. Others
 Sof(Cl2')=Sof(O9')=Sof(O10')=Sof(O11')=Sof(O12')=1-FVAR(1)
 Sof(Cl2)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 N5(H5), N8(H8)
7.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C26(H26A,H26B), C32(H32A,H32B), C38(H38A,H38B)
7.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5A), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
  C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22),
 C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34),
  C35(H35), C36(H36)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.37831(8) 0.27251(5) 0.44846(9) 0.0529(4) Uani 1 1 d . . . . .
Mn2 Mn 0.15349(8) 0.22228(5) 0.21052(9) 0.0530(4) Uani 1 1 d . . . . .
O1 O 0.4259(4) 0.2543(3) 0.5761(4) 0.0696(15) Uani 1 1 d . . . . .
O2 O 0.1806(4) 0.2042(2) 0.3368(4) 0.0592(14) Uani 1 1 d . . . . .
O3 O 0.1095(3) 0.2436(2) 0.0839(3) 0.0574(13) Uani 1 1 d . . . . .
O4 O 0.3454(3) 0.2926(2) 0.3215(3) 0.0564(13) Uani 1 1 d . . . . .
N1 N 0.2767(4) 0.2026(3) 0.4157(4) 0.0537(16) Uani 1 1 d . . . . .
N2 N 0.2451(4) 0.2955(3) 0.2456(4) 0.0496(15) Uani 1 1 d . . . . .
N3 N 0.2758(4) 0.3438(3) 0.4495(4) 0.0564(16) Uani 1 1 d . . . . .
N4 N 0.5281(4) 0.2377(3) 0.4577(4) 0.0604(17) Uani 1 1 d . . . . .
N5 N 0.4796(5) 0.3498(3) 0.4897(5) 0.077(2) Uani 1 1 d . . . . .
H5 H 0.5127 0.3488 0.5610 0.116 Uiso 1 1 calc R . . . .
N6 N 0.2713(5) 0.1583(3) 0.2095(4) 0.0596(17) Uani 1 1 d . . . . .
N7 N -0.0057(4) 0.2456(3) 0.1976(4) 0.0604(17) Uani 1 1 d . . . . .
N8 N 0.0676(5) 0.1412(3) 0.1650(5) 0.0647(18) Uani 1 1 d . . . . .
H8 H 0.0329 0.1437 0.0937 0.097 Uiso 1 1 calc R . . . .
C1 C 0.4447(6) 0.1986(5) 0.6116(6) 0.075(3) Uani 1 1 d . . . . .
C2 C 0.5303(7) 0.1889(7) 0.7012(7) 0.109(4) Uani 1 1 d . . . . .
H2 H 0.5761 0.2212 0.7340 0.131 Uiso 1 1 calc R . . . .
C3 C 0.5482(12) 0.1329(10) 0.7416(12) 0.153(7) Uani 1 1 d . . . . .
H3 H 0.6090 0.1262 0.8005 0.183 Uiso 1 1 calc R . . . .
C4 C 0.4802(15) 0.0861(8) 0.6988(12) 0.158(7) Uani 1 1 d . . . . .
H4 H 0.4921 0.0480 0.7293 0.190 Uiso 1 1 calc R . . . .
C5 C 0.3936(9) 0.0949(5) 0.6103(8) 0.114(4) Uani 1 1 d . . . . .
H5A H 0.3461 0.0628 0.5801 0.137 Uiso 1 1 calc R . . . .
C6 C 0.3767(7) 0.1515(5) 0.5658(7) 0.078(3) Uani 1 1 d . . . . .
C7 C 0.2878(6) 0.1578(4) 0.4734(7) 0.071(2) Uani 1 1 d . . . . .
H7 H 0.2344 0.1279 0.4533 0.085 Uiso 1 1 calc R . . . .
C8 C 0.0801(5) 0.2994(4) 0.0519(5) 0.055(2) Uani 1 1 d . . . . .
C9 C -0.0056(6) 0.3071(4) -0.0386(6) 0.063(2) Uani 1 1 d . . . . .
H9 H -0.0419 0.2731 -0.0753 0.076 Uiso 1 1 calc R . . . .
C10 C -0.0371(7) 0.3644(4) -0.0742(6) 0.077(3) Uani 1 1 d . . . . .
H10 H -0.0962 0.3695 -0.1348 0.092 Uiso 1 1 calc R . . . .
C11 C 0.0157(8) 0.4142(4) -0.0234(7) 0.086(3) Uani 1 1 d . . . . .
H11 H -0.0061 0.4532 -0.0493 0.103 Uiso 1 1 calc R . . . .
C12 C 0.1017(7) 0.4073(4) 0.0664(7) 0.078(3) Uani 1 1 d . . . . .
H12 H 0.1386 0.4418 0.1011 0.094 Uiso 1 1 calc R . . . .
C13 C 0.1335(6) 0.3507(4) 0.1054(6) 0.063(2) Uani 1 1 d . . . . .
C14 C 0.2257(6) 0.3443(4) 0.1959(6) 0.060(2) Uani 1 1 d . . . . .
H14 H 0.2736 0.3769 0.2198 0.072 Uiso 1 1 calc R . . . .
C15 C 0.1767(6) 0.3368(4) 0.4388(6) 0.070(2) Uani 1 1 d . . . . .
H15 H 0.1506 0.2973 0.4371 0.083 Uiso 1 1 calc R . . . .
C16 C 0.1127(6) 0.3851(4) 0.4302(6) 0.081(3) Uani 1 1 d . . . . .
H16 H 0.0436 0.3791 0.4231 0.097 Uiso 1 1 calc R . . . .
C17 C 0.1502(7) 0.4419(5) 0.4321(7) 0.088(3) Uani 1 1 d . . . . .
H17 H 0.1066 0.4756 0.4257 0.106 Uiso 1 1 calc R . . . .
C18 C 0.2515(6) 0.4505(4) 0.4432(5) 0.071(2) Uani 1 1 d . . . . .
H18 H 0.2782 0.4897 0.4440 0.085 Uiso 1 1 calc R . . . .
C19 C 0.3127(6) 0.3998(4) 0.4532(5) 0.058(2) Uani 1 1 d . . . . .
C20 C 0.4232(6) 0.4055(4) 0.4662(6) 0.071(2) Uani 1 1 d . . . . .
H20A H 0.4213 0.4214 0.4066 0.085 Uiso 1 1 calc R . . . .
H20B H 0.4615 0.4350 0.5176 0.085 Uiso 1 1 calc R . . . .
C21 C 0.5515(7) 0.1800(5) 0.4500(6) 0.084(3) Uani 1 1 d . . . . .
H21 H 0.5039 0.1497 0.4488 0.101 Uiso 1 1 calc R . . . .
C22 C 0.6411(8) 0.1626(5) 0.4437(7) 0.092(3) Uani 1 1 d . . . . .
H22 H 0.6536 0.1216 0.4352 0.110 Uiso 1 1 calc R . . . .
C23 C 0.7114(7) 0.2064(6) 0.4502(6) 0.089(3) Uani 1 1 d . . . . .
H23 H 0.7745 0.1957 0.4475 0.107 Uiso 1 1 calc R . . . .
C24 C 0.6916(6) 0.2656(5) 0.4606(6) 0.084(3) Uani 1 1 d . . . . .
H24 H 0.7402 0.2962 0.4656 0.101 Uiso 1 1 calc R . . . .
C25 C 0.5977(6) 0.2793(4) 0.4637(6) 0.067(2) Uani 1 1 d . . . . .
C26 C 0.5681(6) 0.3426(4) 0.4690(7) 0.086(3) Uani 1 1 d . . . . .
H26A H 0.6297 0.3636 0.5189 0.103 Uiso 1 1 calc R . . . .
H26B H 0.5511 0.3625 0.4073 0.103 Uiso 1 1 calc R . . . .
C27 C 0.3664(6) 0.1722(4) 0.2182(6) 0.071(2) Uani 1 1 d . . . . .
H27 H 0.3879 0.2131 0.2280 0.085 Uiso 1 1 calc R . . . .
C28 C 0.4348(7) 0.1300(5) 0.2137(6) 0.081(3) Uani 1 1 d . . . . .
H28 H 0.5028 0.1413 0.2223 0.097 Uiso 1 1 calc R . . . .
C29 C 0.4029(8) 0.0723(5) 0.1970(6) 0.084(3) Uani 1 1 d . . . . .
H29 H 0.4485 0.0424 0.1931 0.101 Uiso 1 1 calc R . . . .
C30 C 0.3057(8) 0.0569(4) 0.1856(7) 0.088(3) Uani 1 1 d . . . . .
H30 H 0.2826 0.0163 0.1733 0.105 Uiso 1 1 calc R . . . .
C31 C 0.2395(6) 0.1019(4) 0.1924(6) 0.067(2) Uani 1 1 d . . . . .
C32 C 0.1335(6) 0.0884(4) 0.1865(7) 0.094(3) Uani 1 1 d . . . . .
H32A H 0.0978 0.0578 0.1364 0.113 Uiso 1 1 calc R . . . .
H32B H 0.1431 0.0713 0.2481 0.113 Uiso 1 1 calc R . . . .
C33 C -0.0410(6) 0.2996(4) 0.2056(6) 0.075(2) Uani 1 1 d . . . . .
H33 H -0.0006 0.3340 0.2074 0.091 Uiso 1 1 calc R . . . .
C34 C -0.1363(7) 0.3080(5) 0.2113(6) 0.087(3) Uani 1 1 d . . . . .
H34 H -0.1591 0.3467 0.2197 0.105 Uiso 1 1 calc R . . . .
C35 C -0.1946(7) 0.2569(6) 0.2043(7) 0.095(3) Uani 1 1 d . . . . .
H35 H -0.2600 0.2606 0.2062 0.114 Uiso 1 1 calc R . . . .
C36 C -0.1605(6) 0.2016(5) 0.1946(6) 0.084(3) Uani 1 1 d . . . . .
H36 H -0.2009 0.1667 0.1904 0.101 Uiso 1 1 calc R . . . .
C37 C -0.0652(6) 0.1970(4) 0.1908(5) 0.064(2) Uani 1 1 d . . . . .
C38 C -0.0189(7) 0.1375(4) 0.1889(7) 0.089(3) Uani 1 1 d . . . . .
H38A H 0.0062 0.1183 0.2523 0.106 Uiso 1 1 calc R . . . .
H38B H -0.0744 0.1115 0.1416 0.106 Uiso 1 1 calc R . . . .
Cl2 Cl 0.3107(7) 0.5571(4) 0.2664(7) 0.083(3) Uani 0.741(18) 1 d . . P A 1
O9 O 0.3905(7) 0.5212(6) 0.3356(8) 0.108(6) Uani 0.741(18) 1 d . . P A 1
O10 O 0.2988(11) 0.5451(6) 0.1723(9) 0.113(4) Uani 0.741(18) 1 d . . P A 1
O11 O 0.3388(7) 0.6205(5) 0.2864(10) 0.098(4) Uani 0.741(18) 1 d . . P A 1
O12 O 0.2105(11) 0.5467(9) 0.2659(15) 0.133(8) Uani 0.741(18) 1 d . . P A 1
Cl2' Cl 0.2857(17) 0.5477(8) 0.2503(16) 0.059(6) Uani 0.259(18) 1 d . U P A 2
O9' O 0.333(2) 0.4896(8) 0.257(3) 0.087(11) Uani 0.259(18) 1 d . U P A 2
O10' O 0.283(2) 0.583(2) 0.174(3) 0.145(17) Uani 0.259(18) 1 d . U P A 2
O11' O 0.356(2) 0.578(2) 0.340(2) 0.114(14) Uani 0.259(18) 1 d . U P A 2
O12' O 0.184(2) 0.542(2) 0.247(4) 0.087(11) Uani 0.259(18) 1 d . U P A 2
Cl1 Cl -0.15661(15) 0.09382(10) -0.07640(19) 0.0758(7) Uani 1 1 d . . . . .
O5 O -0.0719(4) 0.0532(3) -0.0253(5) 0.103(2) Uani 1 1 d . . . . .
O6 O -0.2400(4) 0.0835(2) -0.0507(4) 0.0819(18) Uani 1 1 d . . . . .
O7 O -0.1177(4) 0.1550(2) -0.0536(4) 0.0853(19) Uani 1 1 d . . . . .
O8 O -0.1967(5) 0.0844(3) -0.1759(5) 0.109(2) 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
Mn1 O1 1.847(5) . ?
Mn1 O4 1.884(5) . ?
Mn1 N1 2.026(6) . ?
Mn1 N3 2.162(6) . ?
Mn1 N4 2.213(6) . ?
Mn1 N5 2.148(6) . ?
Mn2 O2 1.886(5) . ?
Mn2 O3 1.856(5) . ?
Mn2 N2 2.002(6) . ?
Mn2 N6 2.207(6) . ?
Mn2 N7 2.245(6) . ?
Mn2 N8 2.116(6) . ?
O1 C1 1.336(11) . ?
O2 N1 1.369(7) . ?
O3 C8 1.333(8) . ?
O4 N2 1.388(7) . ?
N1 C7 1.308(9) . ?
N2 C14 1.291(8) . ?
N3 C15 1.353(9) . ?
N3 C19 1.343(9) . ?
N4 C21 1.346(10) . ?
N4 C25 1.329(9) . ?
N5 H5 1.0000 . ?
N5 C20 1.432(9) . ?
N5 C26 1.447(10) . ?
N6 C27 1.334(9) . ?
N6 C31 1.322(9) . ?
N7 C33 1.332(10) . ?
N7 C37 1.349(10) . ?
N8 H8 1.0000 . ?
N8 C32 1.445(9) . ?
N8 C38 1.444(10) . ?
C1 C2 1.401(12) . ?
C1 C6 1.387(12) . ?
C2 H2 0.9500 . ?
C2 C3 1.368(18) . ?
C3 H3 0.9500 . ?
C3 C4 1.37(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.393(17) . ?
C5 H5A 0.9500 . ?
C5 C6 1.408(12) . ?
C6 C7 1.437(12) . ?
C7 H7 0.9500 . ?
C8 C9 1.404(10) . ?
C8 C13 1.417(10) . ?
C9 H9 0.9500 . ?
C9 C10 1.384(11) . ?
C10 H10 0.9500 . ?
C10 C11 1.373(11) . ?
C11 H11 0.9500 . ?
C11 C12 1.396(11) . ?
C12 H12 0.9500 . ?
C12 C13 1.385(10) . ?
C13 C14 1.441(10) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C15 C16 1.376(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.367(12) . ?
C17 H17 0.9500 . ?
C17 C18 1.386(11) . ?
C18 H18 0.9500 . ?
C18 C19 1.392(10) . ?
C19 C20 1.499(10) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21 0.9500 . ?
C21 C22 1.381(11) . ?
C22 H22 0.9500 . ?
C22 C23 1.367(13) . ?
C23 H23 0.9500 . ?
C23 C24 1.374(13) . ?
C24 H24 0.9500 . ?
C24 C25 1.394(11) . ?
C25 C26 1.482(11) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27 0.9500 . ?
C27 C28 1.379(10) . ?
C28 H28 0.9500 . ?
C28 C29 1.347(12) . ?
C29 H29 0.9500 . ?
C29 C30 1.358(11) . ?
C30 H30 0.9500 . ?
C30 C31 1.413(11) . ?
C31 C32 1.501(11) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33 0.9500 . ?
C33 C34 1.414(11) . ?
C34 H34 0.9500 . ?
C34 C35 1.382(13) . ?
C35 H35 0.9500 . ?
C35 C36 1.358(13) . ?
C36 H36 0.9500 . ?
C36 C37 1.389(11) . ?
C37 C38 1.485(12) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
Cl2 O9 1.412(9) . ?
Cl2 O10 1.434(11) . ?
Cl2 O11 1.463(10) . ?
Cl2 O12 1.443(8) . ?
Cl2' O9' 1.443(17) . ?
Cl2' O10' 1.410(17) . ?
Cl2' O11' 1.480(18) . ?
Cl2' O12' 1.437(16) . ?
Cl1 O5 1.429(5) . ?
Cl1 O6 1.436(5) . ?
Cl1 O7 1.453(5) . ?
Cl1 O8 1.416(7) . ?

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
O1 Mn1 O4 173.7(2) . . ?
O1 Mn1 N1 88.7(3) . . ?
O1 Mn1 N3 94.0(2) . . ?
O1 Mn1 N4 89.0(2) . . ?
O1 Mn1 N5 89.0(3) . . ?
O4 Mn1 N1 96.1(2) . . ?
O4 Mn1 N3 89.4(2) . . ?
O4 Mn1 N4 85.6(2) . . ?
O4 Mn1 N5 86.6(3) . . ?
N1 Mn1 N3 99.1(2) . . ?
N1 Mn1 N4 107.8(2) . . ?
N1 Mn1 N5 175.2(3) . . ?
N3 Mn1 N4 153.0(2) . . ?
N5 Mn1 N3 76.9(2) . . ?
N5 Mn1 N4 76.3(2) . . ?
O2 Mn2 N2 95.0(2) . . ?
O2 Mn2 N6 94.4(2) . . ?
O2 Mn2 N7 82.0(2) . . ?
O2 Mn2 N8 89.1(2) . . ?
O3 Mn2 O2 172.4(2) . . ?
O3 Mn2 N2 87.0(2) . . ?
O3 Mn2 N6 92.6(2) . . ?
O3 Mn2 N7 90.4(2) . . ?
O3 Mn2 N8 89.6(2) . . ?
N2 Mn2 N6 97.1(2) . . ?
N2 Mn2 N7 110.1(2) . . ?
N2 Mn2 N8 173.0(2) . . ?
N6 Mn2 N7 152.8(2) . . ?
N8 Mn2 N6 76.9(2) . . ?
N8 Mn2 N7 76.1(2) . . ?
C1 O1 Mn1 124.2(6) . . ?
N1 O2 Mn2 127.0(4) . . ?
C8 O3 Mn2 122.6(5) . . ?
N2 O4 Mn1 125.9(4) . . ?
O2 N1 Mn1 121.1(4) . . ?
C7 N1 Mn1 124.1(5) . . ?
C7 N1 O2 113.9(6) . . ?
O4 N2 Mn2 119.2(4) . . ?
C14 N2 Mn2 125.6(5) . . ?
C14 N2 O4 114.4(6) . . ?
C15 N3 Mn1 125.8(5) . . ?
C19 N3 Mn1 115.4(5) . . ?
C19 N3 C15 118.6(6) . . ?
C21 N4 Mn1 126.8(6) . . ?
C25 N4 Mn1 115.3(6) . . ?
C25 N4 C21 117.7(7) . . ?
Mn1 N5 H5 103.4 . . ?
C20 N5 Mn1 113.2(4) . . ?
C20 N5 H5 103.4 . . ?
C20 N5 C26 118.9(7) . . ?
C26 N5 Mn1 112.3(5) . . ?
C26 N5 H5 103.4 . . ?
C27 N6 Mn2 126.2(5) . . ?
C31 N6 Mn2 114.9(5) . . ?
C31 N6 C27 118.7(7) . . ?
C33 N7 Mn2 127.6(6) . . ?
C33 N7 C37 118.7(7) . . ?
C37 N7 Mn2 113.3(5) . . ?
Mn2 N8 H8 104.3 . . ?
C32 N8 Mn2 113.5(5) . . ?
C32 N8 H8 104.3 . . ?
C38 N8 Mn2 113.1(5) . . ?
C38 N8 H8 104.3 . . ?
C38 N8 C32 115.7(7) . . ?
O1 C1 C2 118.8(11) . . ?
O1 C1 C6 121.6(7) . . ?
C6 C1 C2 119.3(11) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 C1 120.1(14) . . ?
C3 C2 H2 119.9 . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.4(16) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.5(16) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 H5A 120.1 . . ?
C4 C5 C6 119.8(13) . . ?
C6 C5 H5A 120.1 . . ?
C1 C6 C5 119.8(10) . . ?
C1 C6 C7 122.7(8) . . ?
C5 C6 C7 117.6(10) . . ?
N1 C7 C6 123.3(8) . . ?
N1 C7 H7 118.4 . . ?
C6 C7 H7 118.4 . . ?
O3 C8 C9 118.5(7) . . ?
O3 C8 C13 122.2(7) . . ?
C9 C8 C13 119.3(7) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.8(8) . . ?
C10 C9 H9 120.1 . . ?
C9 C10 H10 119.5 . . ?
C11 C10 C9 121.1(8) . . ?
C11 C10 H10 119.5 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 119.9(9) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 119.7 . . ?
C13 C12 C11 120.5(9) . . ?
C13 C12 H12 119.7 . . ?
C8 C13 C14 120.7(7) . . ?
C12 C13 C8 119.4(8) . . ?
C12 C13 C14 119.7(8) . . ?
N2 C14 C13 122.0(7) . . ?
N2 C14 H14 119.0 . . ?
C13 C14 H14 119.0 . . ?
N3 C15 H15 119.0 . . ?
N3 C15 C16 122.1(8) . . ?
C16 C15 H15 119.0 . . ?
C15 C16 H16 120.5 . . ?
C17 C16 C15 119.0(8) . . ?
C17 C16 H16 120.5 . . ?
C16 C17 H17 119.8 . . ?
C16 C17 C18 120.3(8) . . ?
C18 C17 H17 119.8 . . ?
C17 C18 H18 121.1 . . ?
C17 C18 C19 117.8(8) . . ?
C19 C18 H18 121.1 . . ?
N3 C19 C18 122.3(7) . . ?
N3 C19 C20 116.9(7) . . ?
C18 C19 C20 120.9(7) . . ?
N5 C20 C19 113.2(6) . . ?
N5 C20 H20A 108.9 . . ?
N5 C20 H20B 108.9 . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
H20A C20 H20B 107.8 . . ?
N4 C21 H21 118.4 . . ?
N4 C21 C22 123.3(9) . . ?
C22 C21 H21 118.4 . . ?
C21 C22 H22 121.1 . . ?
C23 C22 C21 117.7(10) . . ?
C23 C22 H22 121.1 . . ?
C22 C23 H23 119.7 . . ?
C22 C23 C24 120.6(9) . . ?
C24 C23 H23 119.7 . . ?
C23 C24 H24 121.1 . . ?
C23 C24 C25 117.8(9) . . ?
C25 C24 H24 121.1 . . ?
N4 C25 C24 122.8(9) . . ?
N4 C25 C26 116.3(7) . . ?
C24 C25 C26 120.8(9) . . ?
N5 C26 C25 114.6(7) . . ?
N5 C26 H26A 108.6 . . ?
N5 C26 H26B 108.6 . . ?
C25 C26 H26A 108.6 . . ?
C25 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
N6 C27 H27 118.4 . . ?
N6 C27 C28 123.1(8) . . ?
C28 C27 H27 118.4 . . ?
C27 C28 H28 120.8 . . ?
C29 C28 C27 118.3(9) . . ?
C29 C28 H28 120.8 . . ?
C28 C29 H29 120.0 . . ?
C28 C29 C30 120.0(9) . . ?
C30 C29 H29 120.0 . . ?
C29 C30 H30 120.4 . . ?
C29 C30 C31 119.2(8) . . ?
C31 C30 H30 120.4 . . ?
N6 C31 C30 120.6(8) . . ?
N6 C31 C32 116.5(7) . . ?
C30 C31 C32 122.8(8) . . ?
N8 C32 C31 112.4(7) . . ?
N8 C32 H32A 109.1 . . ?
N8 C32 H32B 109.1 . . ?
C31 C32 H32A 109.1 . . ?
C31 C32 H32B 109.1 . . ?
H32A C32 H32B 107.8 . . ?
N7 C33 H33 118.7 . . ?
N7 C33 C34 122.7(9) . . ?
C34 C33 H33 118.7 . . ?
C33 C34 H34 121.7 . . ?
C35 C34 C33 116.6(9) . . ?
C35 C34 H34 121.7 . . ?
C34 C35 H35 119.3 . . ?
C36 C35 C34 121.4(9) . . ?
C36 C35 H35 119.3 . . ?
C35 C36 H36 120.7 . . ?
C35 C36 C37 118.6(10) . . ?
C37 C36 H36 120.7 . . ?
N7 C37 C36 122.0(9) . . ?
N7 C37 C38 116.5(7) . . ?
C36 C37 C38 121.2(9) . . ?
N8 C38 C37 113.2(7) . . ?
N8 C38 H38A 108.9 . . ?
N8 C38 H38B 108.9 . . ?
C37 C38 H38A 108.9 . . ?
C37 C38 H38B 108.9 . . ?
H38A C38 H38B 107.7 . . ?
O9 Cl2 O10 111.5(9) . . ?
O9 Cl2 O11 109.5(9) . . ?
O9 Cl2 O12 111.4(9) . . ?
O10 Cl2 O11 107.1(8) . . ?
O10 Cl2 O12 108.1(10) . . ?
O12 Cl2 O11 109.2(9) . . ?
O9' Cl2' O11' 104.5(18) . . ?
O10' Cl2' O9' 113(2) . . ?
O10' Cl2' O11' 108(2) . . ?
O10' Cl2' O12' 113(2) . . ?
O12' Cl2' O9' 111(2) . . ?
O12' Cl2' O11' 108(2) . . ?
O5 Cl1 O6 109.7(4) . . ?
O5 Cl1 O7 108.9(3) . . ?
O6 Cl1 O7 110.6(3) . . ?
O8 Cl1 O5 110.0(4) . . ?
O8 Cl1 O6 108.4(4) . . ?
O8 Cl1 O7 109.2(4) . . ?

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
N5 H5 O11 1.00 2.47 3.357(14) 147.6 3_666
N5 H5 O11' 1.00 2.43 3.08(2) 122.4 3_666
N8 H8 O7 1.00 2.35 3.263(9) 151.2 .

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
Mn1 O1 C1 C2 142.9(6) . . . . ?
Mn1 O1 C1 C6 -42.6(10) . . . . ?
Mn1 O4 N2 Mn2 -58.5(6) . . . . ?
Mn1 O4 N2 C14 130.5(5) . . . . ?
Mn1 N1 C7 C6 -3.1(11) . . . . ?
Mn1 N3 C15 C16 -173.0(6) . . . . ?
Mn1 N3 C19 C18 172.4(6) . . . . ?
Mn1 N3 C19 C20 -6.1(9) . . . . ?
Mn1 N4 C21 C22 171.0(7) . . . . ?
Mn1 N4 C25 C24 -173.6(6) . . . . ?
Mn1 N4 C25 C26 3.3(9) . . . . ?
Mn1 N5 C20 C19 21.7(9) . . . . ?
Mn1 N5 C26 C25 -24.5(9) . . . . ?
Mn2 O2 N1 Mn1 51.5(6) . . . . ?
Mn2 O2 N1 C7 -139.1(6) . . . . ?
Mn2 O3 C8 C9 -141.1(5) . . . . ?
Mn2 O3 C8 C13 40.0(9) . . . . ?
Mn2 N2 C14 C13 -1.6(10) . . . . ?
Mn2 N6 C27 C28 -177.8(6) . . . . ?
Mn2 N6 C31 C30 177.2(6) . . . . ?
Mn2 N6 C31 C32 -6.1(9) . . . . ?
Mn2 N7 C33 C34 -169.6(6) . . . . ?
Mn2 N7 C37 C36 171.6(6) . . . . ?
Mn2 N7 C37 C38 -2.4(9) . . . . ?
Mn2 N8 C32 C31 -27.0(10) . . . . ?
Mn2 N8 C38 C37 30.7(9) . . . . ?
O1 C1 C2 C3 176.6(10) . . . . ?
O1 C1 C6 C5 -173.6(7) . . . . ?
O1 C1 C6 C7 6.2(13) . . . . ?
O2 N1 C7 C6 -172.1(7) . . . . ?
O3 C8 C9 C10 -179.2(6) . . . . ?
O3 C8 C13 C12 177.4(7) . . . . ?
O3 C8 C13 C14 2.7(11) . . . . ?
O4 N2 C14 C13 168.8(6) . . . . ?
N1 Mn1 O1 C1 42.6(5) . . . . ?
N1 Mn1 O4 N2 43.4(5) . . . . ?
N2 Mn2 O2 N1 -47.2(5) . . . . ?
N2 Mn2 O3 C8 -47.3(5) . . . . ?
N3 Mn1 O1 C1 141.7(5) . . . . ?
N3 Mn1 O4 N2 -55.6(5) . . . . ?
N3 C15 C16 C17 0.4(13) . . . . ?
N3 C19 C20 N5 -10.4(10) . . . . ?
N4 Mn1 O1 C1 -65.1(6) . . . . ?
N4 Mn1 O4 N2 150.9(5) . . . . ?
N4 C21 C22 C23 3.2(14) . . . . ?
N4 C25 C26 N5 14.1(11) . . . . ?
N5 Mn1 O1 C1 -141.5(6) . . . . ?
N5 Mn1 O4 N2 -132.6(5) . . . . ?
N6 Mn2 O2 N1 50.3(5) . . . . ?
N6 Mn2 O3 C8 -144.2(5) . . . . ?
N6 C27 C28 C29 2.0(13) . . . . ?
N6 C31 C32 N8 21.8(11) . . . . ?
N7 Mn2 O2 N1 -156.8(5) . . . . ?
N7 Mn2 O3 C8 62.8(5) . . . . ?
N7 C33 C34 C35 -2.7(13) . . . . ?
N7 C37 C38 N8 -18.2(11) . . . . ?
N8 Mn2 O2 N1 127.1(5) . . . . ?
N8 Mn2 O3 C8 138.9(5) . . . . ?
C1 C2 C3 C4 -4(2) . . . . ?
C1 C6 C7 N1 16.3(13) . . . . ?
C2 C1 C6 C5 0.9(13) . . . . ?
C2 C1 C6 C7 -179.3(8) . . . . ?
C2 C3 C4 C5 3(3) . . . . ?
C3 C4 C5 C6 0(2) . . . . ?
C4 C5 C6 C1 -1.8(15) . . . . ?
C4 C5 C6 C7 178.4(10) . . . . ?
C5 C6 C7 N1 -163.9(8) . . . . ?
C6 C1 C2 C3 2.0(14) . . . . ?
C8 C9 C10 C11 1.6(12) . . . . ?
C8 C13 C14 N2 -21.6(11) . . . . ?
C9 C8 C13 C12 -1.5(11) . . . . ?
C9 C8 C13 C14 -176.2(7) . . . . ?
C9 C10 C11 C12 -1.1(13) . . . . ?
C10 C11 C12 C13 -0.7(14) . . . . ?
C11 C12 C13 C8 2.0(12) . . . . ?
C11 C12 C13 C14 176.8(8) . . . . ?
C12 C13 C14 N2 163.7(7) . . . . ?
C13 C8 C9 C10 -0.3(11) . . . . ?
C15 N3 C19 C18 -2.2(11) . . . . ?
C15 N3 C19 C20 179.4(7) . . . . ?
C15 C16 C17 C18 -0.5(14) . . . . ?
C16 C17 C18 C19 -0.6(13) . . . . ?
C17 C18 C19 N3 2.0(12) . . . . ?
C17 C18 C19 C20 -179.6(8) . . . . ?
C18 C19 C20 N5 171.1(7) . . . . ?
C19 N3 C15 C16 1.0(11) . . . . ?
C20 N5 C26 C25 -159.9(7) . . . . ?
C21 N4 C25 C24 1.2(12) . . . . ?
C21 N4 C25 C26 178.1(8) . . . . ?
C21 C22 C23 C24 -1.3(14) . . . . ?
C22 C23 C24 C25 -0.4(14) . . . . ?
C23 C24 C25 N4 0.4(13) . . . . ?
C23 C24 C25 C26 -176.3(8) . . . . ?
C24 C25 C26 N5 -169.0(7) . . . . ?
C25 N4 C21 C22 -3.1(13) . . . . ?
C26 N5 C20 C19 156.6(7) . . . . ?
C27 N6 C31 C30 1.3(12) . . . . ?
C27 N6 C31 C32 178.0(7) . . . . ?
C27 C28 C29 C30 -0.5(14) . . . . ?
C28 C29 C30 C31 -0.5(14) . . . . ?
C29 C30 C31 N6 0.1(13) . . . . ?
C29 C30 C31 C32 -176.4(9) . . . . ?
C30 C31 C32 N8 -161.6(8) . . . . ?
C31 N6 C27 C28 -2.4(12) . . . . ?
C32 N8 C38 C37 164.0(7) . . . . ?
C33 N7 C37 C36 -1.8(11) . . . . ?
C33 N7 C37 C38 -175.9(7) . . . . ?
C33 C34 C35 C36 1.5(14) . . . . ?
C34 C35 C36 C37 -0.7(14) . . . . ?
C35 C36 C37 N7 0.8(13) . . . . ?
C35 C36 C37 C38 174.6(9) . . . . ?
C36 C37 C38 N8 167.7(7) . . . . ?
C37 N7 C33 C34 2.8(12) . . . . ?
C38 N8 C32 C31 -160.1(7) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-8 -3 -1 0.0381 -7.9994 -3.0055 -0.5003 0.0603 0.9142 -0.4422
-1 2 9 0.1229 -1.0026 2.0066 9.4991 -0.0010 0.0220 1.0052
-8 6 6 0.0924 -8.0043 6.0047 6.4998 0.5393 0.7361 0.4072
4 3 6 0.0791 3.9981 3.0072 5.9997 -0.0305 -0.5136 0.8595
-1 14 1 0.0132 -1.0059 14.0093 0.5013 0.9584 -0.1078 0.1502
-9 -3 5 0.0927 -9.0005 -3.0026 4.9991 -0.0044 0.9901 0.1094
8 2 0 0.0244 8.0000 2.0042 -0.4997 -0.1097 -0.8931 0.3237
1 -14 -1 0.0132 1.0059 -14.0093 -0.5013 -0.9584 0.1078 -0.1502
-8 5 0 0.0311 -8.0028 5.0002 0.0004 0.5862 0.7895 -0.3075
4 -1 -10 0.1227 4.0025 -1.0050 -9.9990 -0.0179 -0.3589 -0.9152
8 3 1 0.0315 7.9994 3.0055 0.5003 -0.0603 -0.9142 0.4422

####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1044304'
_audit_update_record             
;
2015-01-19 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;
# local name eb3299
_audit_creation_date             2013-11-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C50 H44 Mn2 N8 O4, 2(Cl O4), 1.61(C4 H8 O1)'
_chemical_formula_sum            'C56.44 H56.87 Cl2 Mn2 N8 O13.61'
_chemical_formula_weight         1245.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C30 H40 N8 O20 Mn2 Cl'
_chemical_oxdiff_usercomment     '@ 120 K PC490'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   8.4822(4)
_cell_length_b                   13.2500(4)
_cell_length_c                   13.6070(5)
_cell_angle_alpha                110.595(3)
_cell_angle_beta                 103.803(4)
_cell_angle_gamma                92.048(3)
_cell_volume                     1378.12(10)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9349
_cell_measurement_temperature    120
_cell_measurement_theta_max      75.8080
_cell_measurement_theta_min      4.0180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.247
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.3496
_exptl_crystal_size_mid          0.0523
_exptl_crystal_size_min          0.0464
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21371
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.336
_diffrn_reflns_theta_min         3.595
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Agilent Technologies SuperNova'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0298347000
_diffrn_orient_matrix_UB_12      0.0211278000
_diffrn_orient_matrix_UB_13      0.1221857000
_diffrn_orient_matrix_UB_21      0.0305556000
_diffrn_orient_matrix_UB_22      -0.1189352000
_diffrn_orient_matrix_UB_23      -0.0222326000
_diffrn_orient_matrix_UB_31      0.1837671000
_diffrn_orient_matrix_UB_32      0.0332770000
_diffrn_orient_matrix_UB_33      0.0184659000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5040
_reflns_number_total             5662
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5662
_refine_ls_number_restraints     151
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0572
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0817P)²+1.4581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1590
_refine_special_details          
;
The occupancy of the THF molecule was freely refined to ~80%. C-C and C-O 
bonds in THF were restrained to target values. An attempt at disorder 
modelling yielded a significantly worse refinement.


PLAT041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ   
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...    
PLAT077_ALERT_4_C Unitcell contains non-integer number of atoms ..    
PLAT220_ALERT_2_C Large Non-Solvent    C     Ueq(max)/Ueq(min) ...     
PLAT241_ALERT_2_C High      Ueq as Compared to Neighbors for .....    

All caused by the THF discussed above.
  
PLAT341_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    


;



_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups
2. Restrained distances
 C28-C27
 1.47 with sigma of 0.02
 C29-C28 = C27-C26
 1.48 with sigma of 0.02
 O7-C29 = O7-C26
 1.44 with sigma of 0.02
 N4-H4
 0.84 with sigma of 0.01
3. Rigid bond restraints
 O7, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O7, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C14, C15, C16, C17, C18, C19, N4, C25, C24, C23, C22, C21, C20, N3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C29 \\sim O7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O7 \\sim C26: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N2 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim N4 \\sim
C25 \\sim C24 \\sim C23 \\sim C22 \\sim C21 \\sim C20 \\sim N3: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Others
 Sof(O7)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=
 Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,
 H28B), C29(H29A,H29B)
6.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22),
 C23(H23), C3(H3), C2(H2), C9(H9), C13(H13), C4(H4A), C5(H5), C10(H10),
 C12(H12), C11(H11)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.06958(6) 0.08751(4) 0.92938(4) 0.03285(15) Uani 1 1 d . . . . .
Cl2 Cl 0.23821(12) 0.28837(7) 0.68519(8) 0.0582(3) Uani 1 1 d . . . . .
O2 O 0.1432(2) -0.02871(16) 1.07888(17) 0.0358(4) Uani 1 1 d . . . . .
O1 O 0.2744(3) 0.15305(18) 0.93952(18) 0.0424(5) Uani 1 1 d . . . . .
N1 N 0.1786(3) 0.06979(19) 1.0721(2) 0.0323(5) Uani 1 1 d . . . . .
C8 C 0.3953(3) 0.1016(2) 1.2357(2) 0.0348(6) Uani 1 1 d . . . . .
N2 N 0.1019(4) -0.0670(2) 0.8086(2) 0.0490(7) Uani 1 1 d . U . . .
C14 C 0.1739(5) -0.1480(3) 0.8334(4) 0.0620(10) Uani 1 1 d . U . . .
H14 H 0.2187 -0.1375 0.9078 0.074 Uiso 1 1 calc R . . . .
C15 C 0.1839(7) -0.2447(4) 0.7543(5) 0.0918(17) Uani 1 1 d . U . . .
H15 H 0.2313 -0.3014 0.7734 0.110 Uiso 1 1 calc R . . . .
C16 C 0.1240(10) -0.2575(5) 0.6474(6) 0.115(2) Uani 1 1 d . U . . .
H16 H 0.1317 -0.3230 0.5913 0.138 Uiso 1 1 calc R . . . .
C17 C 0.0535(8) -0.1765(5) 0.6210(4) 0.0969(19) Uani 1 1 d . U . . .
H17 H 0.0125 -0.1849 0.5468 0.116 Uiso 1 1 calc R . . . .
C18 C 0.0421(5) -0.0801(4) 0.7049(3) 0.0623(11) Uani 1 1 d . U . . .
C7 C 0.3052(3) 0.1340(2) 1.1460(2) 0.0317(6) Uani 1 1 d . . . . .
N3 N -0.0296(3) 0.2495(2) 0.9729(3) 0.0459(6) Uani 1 1 d . U . . .
C20 C -0.0069(5) 0.3276(3) 1.0725(4) 0.0552(9) Uani 1 1 d . U . . .
H20 H 0.0634 0.3179 1.1334 0.066 Uiso 1 1 calc R . . . .
C21 C -0.0815(6) 0.4211(4) 1.0899(5) 0.0729(13) Uani 1 1 d . U . . .
H21 H -0.0644 0.4744 1.1611 0.087 Uiso 1 1 calc R . . . .
C22 C -0.1804(6) 0.4343(5) 1.0014(6) 0.0875(17) Uani 1 1 d . U . . .
H22 H -0.2332 0.4978 1.0107 0.105 Uiso 1 1 calc R . . . .
C23 C -0.2040(6) 0.3573(5) 0.8999(6) 0.0813(15) Uani 1 1 d . U . . .
H23 H -0.2721 0.3669 0.8382 0.098 Uiso 1 1 calc R . . . .
C24 C -0.1273(4) 0.2644(4) 0.8874(4) 0.0580(10) Uani 1 1 d . U . . .
C3 C 0.4946(4) 0.4194(3) 1.1144(3) 0.0440(7) Uani 1 1 d . . . . .
H3 H 0.5383 0.4828 1.1075 0.053 Uiso 1 1 calc R . . . .
C1 C 0.3485(4) 0.2373(2) 1.0304(3) 0.0351(6) Uani 1 1 d . . . . .
N4 N -0.0145(5) 0.1098(3) 0.7779(3) 0.0621(9) Uani 1 1 d D U . . .
C2 C 0.4182(4) 0.3303(3) 1.0218(3) 0.0410(7) Uani 1 1 d . . . . .
H2 H 0.4130 0.3321 0.9519 0.049 Uiso 1 1 calc R . . . .
O3 O 0.1735(4) 0.1761(2) 0.6237(3) 0.0728(9) Uani 1 1 d . . . . .
C6 C 0.3646(3) 0.2336(2) 1.1347(2) 0.0336(6) Uani 1 1 d . . . . .
C9 C 0.4906(4) 0.0172(3) 1.2099(3) 0.0410(7) Uani 1 1 d . . . . .
H9 H 0.4957 -0.0171 1.1367 0.049 Uiso 1 1 calc R . . . .
C13 C 0.3882(4) 0.1531(3) 1.3433(3) 0.0468(8) Uani 1 1 d . . . . .
H13 H 0.3239 0.2106 1.3620 0.056 Uiso 1 1 calc R . . . .
C4 C 0.5081(5) 0.4173(3) 1.2169(3) 0.0489(8) Uani 1 1 d . . . . .
H4A H 0.5592 0.4793 1.2801 0.059 Uiso 1 1 calc R . . . .
C5 C 0.4468(4) 0.3245(3) 1.2269(3) 0.0445(7) Uani 1 1 d . . . . .
H5 H 0.4605 0.3221 1.2974 0.053 Uiso 1 1 calc R . . . .
O4 O 0.1767(6) 0.3242(4) 0.7810(3) 0.1008(13) Uani 1 1 d . . . . .
C10 C 0.5776(4) -0.0169(3) 1.2895(4) 0.0555(10) Uani 1 1 d . . . . .
H10 H 0.6410 -0.0750 1.2711 0.067 Uiso 1 1 calc R . . . .
C19 C -0.0388(6) 0.0096(4) 0.6815(3) 0.0716(13) Uani 1 1 d . U . . .
H19A H 0.0042 0.0258 0.6264 0.086 Uiso 1 1 calc R . . . .
H19B H -0.1578 -0.0150 0.6498 0.086 Uiso 1 1 calc R . . . .
C12 C 0.4789(6) 0.1175(4) 1.4234(3) 0.0654(12) Uani 1 1 d . . . . .
H12 H 0.4757 0.1516 1.4969 0.078 Uiso 1 1 calc R . . . .
C25 C -0.1488(5) 0.1735(5) 0.7775(4) 0.0729(12) Uani 1 1 d . U . . .
H25A H -0.2524 0.1256 0.7589 0.087 Uiso 1 1 calc R . . . .
H25B H -0.1564 0.2052 0.7209 0.087 Uiso 1 1 calc R . . . .
O6 O 0.1872(7) 0.3511(3) 0.6222(3) 0.1173(18) Uani 1 1 d . . . . .
C11 C 0.5718(5) 0.0341(4) 1.3964(4) 0.0668(12) Uani 1 1 d . . . . .
H11 H 0.6325 0.0113 1.4514 0.080 Uiso 1 1 calc R . . . .
O5 O 0.4136(5) 0.2985(3) 0.7214(4) 0.0985(13) Uani 1 1 d . . . . .
O7 O 0.3573(19) 0.5671(12) 0.5031(11) 0.280(7) Uani 0.805(8) 1 d D U P . .
C26 C 0.339(2) 0.6177(11) 0.4284(10) 0.179(7) Uani 0.805(8) 1 d D U P . .
H26A H 0.3279 0.6955 0.4636 0.215 Uiso 0.805(8) 1 calc R . P . .
H26B H 0.4350 0.6127 0.3984 0.215 Uiso 0.805(8) 1 calc R . P . .
C27 C 0.2114(15) 0.5692(9) 0.3539(12) 0.136(4) Uani 0.805(8) 1 d D . P . .
H27A H 0.2362 0.5363 0.2827 0.163 Uiso 0.805(8) 1 calc R . P . .
H27B H 0.1287 0.6192 0.3482 0.163 Uiso 0.805(8) 1 calc R . P . .
C28 C 0.1554(16) 0.4863(8) 0.3892(9) 0.139(5) Uani 0.805(8) 1 d D . P . .
H28A H 0.0452 0.4981 0.3999 0.167 Uiso 0.805(8) 1 calc R . P . .
H28B H 0.1450 0.4142 0.3306 0.167 Uiso 0.805(8) 1 calc R . P . .
C29 C 0.2531(16) 0.4849(9) 0.4803(11) 0.141(4) Uani 0.805(8) 1 d D U P . .
H29A H 0.1951 0.4951 0.5375 0.169 Uiso 0.805(8) 1 calc R . P . .
H29B H 0.3041 0.4170 0.4679 0.169 Uiso 0.805(8) 1 calc R . P . .
H4 H 0.061(8) 0.159(5) 0.788(7) 0.169 Uiso 1 1 d DR . . . .


_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 O2 1.902(2) 2_557 ?
Mn1 O1 1.867(2) . ?
Mn1 N1 2.039(2) . ?
Mn1 N2 2.203(3) . ?
Mn1 N3 2.267(3) . ?
Mn1 N4 2.141(3) . ?
Cl2 O3 1.436(3) . ?
Cl2 O4 1.450(4) . ?
Cl2 O6 1.401(3) . ?
Cl2 O5 1.436(4) . ?
O2 Mn1 1.902(2) 2_557 ?
O2 N1 1.368(3) . ?
O1 C1 1.333(4) . ?
N1 C7 1.306(4) . ?
C8 C7 1.486(4) . ?
C8 C9 1.397(5) . ?
C8 C13 1.397(5) . ?
N2 C14 1.358(6) . ?
N2 C18 1.327(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.375(6) . ?
C15 H15 0.9500 . ?
C15 C16 1.368(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.361(11) . ?
C17 H17 0.9500 . ?
C17 C18 1.407(7) . ?
C18 C19 1.484(8) . ?
C7 C6 1.466(4) . ?
N3 C20 1.349(5) . ?
N3 C24 1.339(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.384(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.365(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.360(9) . ?
C23 H23 0.9500 . ?
C23 C24 1.389(6) . ?
C24 C25 1.518(7) . ?
C3 H3 0.9500 . ?
C3 C2 1.382(5) . ?
C3 C4 1.383(5) . ?
C1 C2 1.402(4) . ?
C1 C6 1.411(4) . ?
N4 C19 1.466(6) . ?
N4 C25 1.443(7) . ?
N4 H4 0.844(10) . ?
C2 H2 0.9500 . ?
C6 C5 1.404(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.383(5) . ?
C13 H13 0.9500 . ?
C13 C12 1.410(6) . ?
C4 H4A 0.9500 . ?
C4 C5 1.380(5) . ?
C5 H5 0.9500 . ?
C10 H10 0.9500 . ?
C10 C11 1.385(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C12 H12 0.9500 . ?
C12 C11 1.376(7) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C11 H11 0.9500 . ?
O7 C26 1.384(13) . ?
O7 C29 1.276(12) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.256(13) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.451(11) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.323(12) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?

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
O2 Mn1 N1 94.58(9) 2_557 . ?
O2 Mn1 N2 90.98(10) 2_557 . ?
O2 Mn1 N3 85.01(9) 2_557 . ?
O2 Mn1 N4 92.42(12) 2_557 . ?
O1 Mn1 O2 176.72(9) . 2_557 ?
O1 Mn1 N1 86.40(10) . . ?
O1 Mn1 N2 91.89(10) . . ?
O1 Mn1 N3 91.71(10) . . ?
O1 Mn1 N4 86.70(12) . . ?
N1 Mn1 N2 101.42(11) . . ?
N1 Mn1 N3 107.21(10) . . ?
N1 Mn1 N4 172.82(12) . . ?
N2 Mn1 N3 151.31(12) . . ?
N4 Mn1 N2 76.82(15) . . ?
N4 Mn1 N3 74.98(14) . . ?
O3 Cl2 O4 108.0(2) . . ?
O3 Cl2 O5 109.5(2) . . ?
O6 Cl2 O3 110.1(2) . . ?
O6 Cl2 O4 109.6(3) . . ?
O6 Cl2 O5 111.7(3) . . ?
O5 Cl2 O4 107.8(3) . . ?
N1 O2 Mn1 124.13(16) . 2_557 ?
C1 O1 Mn1 118.22(19) . . ?
O2 N1 Mn1 117.02(17) . . ?
C7 N1 Mn1 124.52(19) . . ?
C7 N1 O2 116.5(2) . . ?
C9 C8 C7 117.7(3) . . ?
C13 C8 C7 122.3(3) . . ?
C13 C8 C9 120.0(3) . . ?
C14 N2 Mn1 124.7(3) . . ?
C18 N2 Mn1 115.9(3) . . ?
C18 N2 C14 119.3(4) . . ?
N2 C14 H14 119.0 . . ?
N2 C14 C15 122.0(5) . . ?
C15 C14 H14 119.0 . . ?
C14 C15 H15 120.8 . . ?
C16 C15 C14 118.5(6) . . ?
C16 C15 H15 120.8 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.2(5) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 120.4 . . ?
C16 C17 C18 119.2(5) . . ?
C18 C17 H17 120.4 . . ?
N2 C18 C17 120.7(5) . . ?
N2 C18 C19 117.5(4) . . ?
C17 C18 C19 121.9(5) . . ?
N1 C7 C8 119.9(2) . . ?
N1 C7 C6 119.4(3) . . ?
C6 C7 C8 120.5(2) . . ?
C20 N3 Mn1 128.0(2) . . ?
C24 N3 Mn1 113.8(3) . . ?
C24 N3 C20 118.2(3) . . ?
N3 C20 H20 118.6 . . ?
N3 C20 C21 122.8(4) . . ?
C21 C20 H20 118.6 . . ?
C20 C21 H21 121.1 . . ?
C22 C21 C20 117.8(5) . . ?
C22 C21 H21 121.1 . . ?
C21 C22 H22 119.7 . . ?
C23 C22 C21 120.5(4) . . ?
C23 C22 H22 119.7 . . ?
C22 C23 H23 120.4 . . ?
C22 C23 C24 119.2(5) . . ?
C24 C23 H23 120.4 . . ?
N3 C24 C23 121.5(5) . . ?
N3 C24 C25 115.7(4) . . ?
C23 C24 C25 122.8(4) . . ?
C2 C3 H3 119.6 . . ?
C2 C3 C4 120.8(3) . . ?
C4 C3 H3 119.6 . . ?
O1 C1 C2 118.9(3) . . ?
O1 C1 C6 121.9(3) . . ?
C2 C1 C6 119.2(3) . . ?
Mn1 N4 H4 98(6) . . ?
C19 N4 Mn1 114.0(3) . . ?
C19 N4 H4 117(6) . . ?
C25 N4 Mn1 112.0(3) . . ?
C25 N4 C19 115.1(4) . . ?
C25 N4 H4 98(6) . . ?
C3 C2 C1 120.4(3) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C1 C6 C7 120.4(3) . . ?
C5 C6 C7 120.7(3) . . ?
C5 C6 C1 118.8(3) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 C8 120.7(4) . . ?
C10 C9 H9 119.7 . . ?
C8 C13 H13 120.8 . . ?
C8 C13 C12 118.3(4) . . ?
C12 C13 H13 120.8 . . ?
C3 C4 H4A 120.2 . . ?
C5 C4 C3 119.6(3) . . ?
C5 C4 H4A 120.2 . . ?
C6 C5 H5 119.4 . . ?
C4 C5 C6 121.1(3) . . ?
C4 C5 H5 119.4 . . ?
C9 C10 H10 120.2 . . ?
C9 C10 C11 119.6(4) . . ?
C11 C10 H10 120.2 . . ?
C18 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
N4 C19 C18 113.7(3) . . ?
N4 C19 H19A 108.8 . . ?
N4 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C13 C12 H12 119.6 . . ?
C11 C12 C13 120.9(4) . . ?
C11 C12 H12 119.6 . . ?
C24 C25 H25A 109.3 . . ?
C24 C25 H25B 109.3 . . ?
N4 C25 C24 111.7(3) . . ?
N4 C25 H25A 109.3 . . ?
N4 C25 H25B 109.3 . . ?
H25A C25 H25B 107.9 . . ?
C10 C11 H11 119.8 . . ?
C12 C11 C10 120.5(4) . . ?
C12 C11 H11 119.8 . . ?
C29 O7 C26 117.0(12) . . ?
O7 C26 H26A 110.4 . . ?
O7 C26 H26B 110.4 . . ?
H26A C26 H26B 108.6 . . ?
C27 C26 O7 106.8(12) . . ?
C27 C26 H26A 110.4 . . ?
C27 C26 H26B 110.4 . . ?
C26 C27 H27A 111.2 . . ?
C26 C27 H27B 111.2 . . ?
C26 C27 C28 102.8(12) . . ?
H27A C27 H27B 109.1 . . ?
C28 C27 H27A 111.2 . . ?
C28 C27 H27B 111.2 . . ?
C27 C28 H28A 108.7 . . ?
C27 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
C29 C28 C27 114.1(12) . . ?
C29 C28 H28A 108.7 . . ?
C29 C28 H28B 108.7 . . ?
O7 C29 C28 99.2(10) . . ?
O7 C29 H29A 111.9 . . ?
O7 C29 H29B 111.9 . . ?
C28 C29 H29A 111.9 . . ?
C28 C29 H29B 111.9 . . ?
H29A C29 H29B 109.6 . . ?

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
N4 H4 O4 0.844(10) 2.41(4) 3.204(6) 156(8) .

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
Mn1 O2 N1 Mn1 -63.0(2) 2_557 . . . ?
Mn1 O2 N1 C7 132.2(2) 2_557 . . . ?
Mn1 O1 C1 C2 -133.7(2) . . . . ?
Mn1 O1 C1 C6 49.1(4) . . . . ?
Mn1 N1 C7 C8 -167.7(2) . . . . ?
Mn1 N1 C7 C6 7.6(4) . . . . ?
Mn1 N2 C14 C15 177.0(3) . . . . ?
Mn1 N2 C18 C17 -178.9(3) . . . . ?
Mn1 N2 C18 C19 0.1(4) . . . . ?
Mn1 N3 C20 C21 -176.3(3) . . . . ?
Mn1 N3 C24 C23 177.4(3) . . . . ?
Mn1 N3 C24 C25 -2.2(4) . . . . ?
Mn1 N4 C19 C18 -16.4(4) . . . . ?
Mn1 N4 C25 C24 37.7(4) . . . . ?
O2 N1 C7 C8 -4.2(4) . . . . ?
O2 N1 C7 C6 171.2(2) . . . . ?
O1 C1 C2 C3 179.4(3) . . . . ?
O1 C1 C6 C7 2.5(4) . . . . ?
O1 C1 C6 C5 178.8(3) . . . . ?
N1 Mn1 O1 C1 -54.6(2) . . . . ?
N1 C7 C6 C1 -31.3(4) . . . . ?
N1 C7 C6 C5 152.5(3) . . . . ?
C8 C7 C6 C1 144.0(3) . . . . ?
C8 C7 C6 C5 -32.2(4) . . . . ?
C8 C9 C10 C11 -0.8(5) . . . . ?
C8 C13 C12 C11 -0.1(5) . . . . ?
N2 Mn1 O1 C1 -156.0(2) . . . . ?
N2 C14 C15 C16 2.2(7) . . . . ?
N2 C18 C19 N4 10.7(5) . . . . ?
C14 N2 C18 C17 -0.4(5) . . . . ?
C14 N2 C18 C19 178.6(3) . . . . ?
C14 C15 C16 C17 -1.3(9) . . . . ?
C15 C16 C17 C18 -0.4(9) . . . . ?
C16 C17 C18 N2 1.3(7) . . . . ?
C16 C17 C18 C19 -177.7(5) . . . . ?
C17 C18 C19 N4 -170.3(4) . . . . ?
C18 N2 C14 C15 -1.4(6) . . . . ?
C7 C8 C9 C10 180.0(3) . . . . ?
C7 C8 C13 C12 -179.5(3) . . . . ?
C7 C6 C5 C4 177.8(3) . . . . ?
N3 Mn1 O1 C1 52.5(2) . . . . ?
N3 C20 C21 C22 -0.8(6) . . . . ?
N3 C24 C25 N4 -22.9(5) . . . . ?
C20 N3 C24 C23 -0.1(5) . . . . ?
C20 N3 C24 C25 -179.7(3) . . . . ?
C20 C21 C22 C23 0.1(7) . . . . ?
C21 C22 C23 C24 0.6(7) . . . . ?
C22 C23 C24 N3 -0.6(6) . . . . ?
C22 C23 C24 C25 179.0(4) . . . . ?
C23 C24 C25 N4 157.5(4) . . . . ?
C24 N3 C20 C21 0.8(5) . . . . ?
C3 C4 C5 C6 -2.8(6) . . . . ?
C1 C6 C5 C4 1.5(5) . . . . ?
N4 Mn1 O1 C1 127.4(2) . . . . ?
C2 C3 C4 C5 1.0(6) . . . . ?
C2 C1 C6 C7 -174.8(3) . . . . ?
C2 C1 C6 C5 1.5(4) . . . . ?
C6 C1 C2 C3 -3.2(5) . . . . ?
C9 C8 C7 N1 71.5(4) . . . . ?
C9 C8 C7 C6 -103.8(3) . . . . ?
C9 C8 C13 C12 0.0(5) . . . . ?
C9 C10 C11 C12 0.7(6) . . . . ?
C13 C8 C7 N1 -109.1(3) . . . . ?
C13 C8 C7 C6 75.7(4) . . . . ?
C13 C8 C9 C10 0.5(4) . . . . ?
C13 C12 C11 C10 -0.2(6) . . . . ?
C4 C3 C2 C1 2.0(5) . . . . ?
C19 N4 C25 C24 170.0(3) . . . . ?
C25 N4 C19 C18 -147.7(3) . . . . ?
O7 C26 C27 C28 -0.1(17) . . . . ?
C26 O7 C29 C28 -4(2) . . . . ?
C26 C27 C28 C29 -2.5(17) . . . . ?
C27 C28 C29 O7 3.8(17) . . . . ?
C29 O7 C26 C27 3(2) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -9 3 0.0275 0.0000 -9.0000 3.0000 0.1764 1.0037 -0.2441
0 9 -3 0.0248 -0.0000 9.0000 -3.0000 -0.1764 -1.0037 0.2441
5 -2 0 0.1504 5.0000 -2.0000 0.0000 0.1069 0.3906 0.8523
0 0 -8 0.0232 -0.0000 0.0000 -8.0000 -0.9775 0.1779 -0.1477
0 0 8 0.0232 0.0000 -0.0000 8.0000 0.9775 -0.1779 0.1477
-5 -2 3 0.1681 -5.0000 -2.0000 3.0000 0.1751 0.0184 -0.9300
0 8 1 0.0219 -0.0000 8.0000 1.0000 0.2912 -0.9737 0.2847
0 -7 7 0.0264 0.0000 -7.0000 7.0000 0.7074 0.6769 -0.1037

