# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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. 
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data_dd491b
_database_code_depnum_ccdc_archive 'CCDC 1025942'
_audit_update_record             
;
2016-06-27 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H60 Cl2 Mn N8 O10'
_chemical_formula_weight         1082.92

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_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'
'-x+1/4, y+1/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+3/4, -y+5/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+5/4, -y+3/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+5/4, -y+5/4, z+1/4'

_cell_length_a                   19.971(2)
_cell_length_b                   40.861(6)
_cell_length_c                   13.081(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10675(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    291(1)
_cell_measurement_reflns_used    405
_cell_measurement_theta_min      2
_cell_measurement_theta_max      20

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale pink'
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.086
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_F_000             4536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_absorpt_coefficient_mu    0.412
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      291(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14
_diffrn_reflns_number            14575
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.927
_diffrn_reflns_theta_max         22.666
_diffrn_reflns_theta_full        22.666
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             3482
_reflns_number_gt                3019
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_max     0.957
_reflns_Friedel_fraction_full    0.958

_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2008)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    
;XP in SHELXTL/PC (Sheldrick, 2008)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material  
;SHELXL-97 (Sheldrick, 2008) and
 PLATON (Spek, 1990)
;
_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)+(0.0554P)²+6.8099P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1235 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3482
_refine_ls_number_parameters     333
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.0989
_refine_ls_wR_factor_gt          0.0918
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.7500 0.2500 0.48049(8) 0.0498(3) Uani 1 2 d S T P . .
O1 O 0.70326(18) 0.28063(8) 0.5891(3) 0.0561(9) Uani 1 1 d . . . . .
N1 N 0.6537(2) 0.22183(9) 0.5012(4) 0.0538(11) Uani 1 1 d . . . . .
N2 N 0.7719(2) 0.21276(11) 0.3609(4) 0.0616(12) Uani 1 1 d . . . . .
N3 N 0.7603(2) 0.32654(11) 0.6966(4) 0.0592(13) Uani 1 1 d . . . . .
H3N H 0.7500 0.3201 0.6420 0.071 Uiso 1 1 d R U . . .
N4 N 0.7017(3) 0.37810(15) 0.5257(6) 0.0950(19) Uani 1 1 d . . . . .
C8 C 0.6762(3) 0.26990(11) 0.6715(5) 0.0504(12) Uani 1 1 d . . . . .
C9 C 0.6883(3) 0.28579(11) 0.7668(4) 0.0521(13) Uani 1 1 d . . . . .
C10 C 0.6579(3) 0.27465(12) 0.8566(5) 0.0620(15) Uani 1 1 d . . . . .
H10 H 0.6675 0.2853 0.9177 0.074 Uiso 1 1 calc R U . . .
C5 C 0.6146(3) 0.24865(12) 0.8583(4) 0.0587(14) Uani 1 1 d . . . . .
C3 C 0.5817(3) 0.23603(16) 0.9574(5) 0.0735(17) Uani 1 1 d . . . . .
C6 C 0.6045(3) 0.23276(12) 0.7658(4) 0.0554(14) Uani 1 1 d . . . . .
H6 H 0.5759 0.2148 0.7654 0.067 Uiso 1 1 calc R U . . .
C7 C 0.6338(2) 0.24178(11) 0.6739(4) 0.0495(13) Uani 1 1 d . . . . .
C11 C 0.6215(3) 0.22169(11) 0.5851(5) 0.0532(13) Uani 1 1 d . . . . .
H11 H 0.5861 0.2070 0.5898 0.064 Uiso 1 1 calc R U . . .
C12 C 0.6340(3) 0.19656(14) 0.4250(5) 0.0704(16) Uani 1 1 d . . . . .
H12A H 0.5857 0.1939 0.4268 0.084 Uiso 1 1 calc R U . . .
H12B H 0.6540 0.1758 0.4439 0.084 Uiso 1 1 calc R U . . .
C13 C 0.6551(3) 0.20519(15) 0.3175(5) 0.0709(17) Uani 1 1 d . . . . .
H13A H 0.6291 0.1921 0.2700 0.085 Uiso 1 1 calc R U . . .
H13B H 0.6441 0.2280 0.3050 0.085 Uiso 1 1 calc R U . . .
C14 C 0.7276(3) 0.20017(12) 0.2949(4) 0.0594(14) Uani 1 1 d . . . . .
C15 C 0.7491(4) 0.18302(17) 0.2091(5) 0.076(2) Uani 1 1 d . . . . .
H15 H 0.7184 0.1748 0.1622 0.092 Uiso 1 1 calc R U . . .
C16 C 0.8172(5) 0.17836(17) 0.1948(6) 0.100(3) Uani 1 1 d . . . . .
H16 H 0.8324 0.1669 0.1381 0.120 Uiso 1 1 calc R U . . .
C17 C 0.8611(4) 0.19040(15) 0.2628(6) 0.084(2) Uani 1 1 d . . . . .
H17 H 0.9069 0.1873 0.2543 0.101 Uiso 1 1 calc R U . . .
C18 C 0.8367(3) 0.20738(13) 0.3445(5) 0.0727(17) Uani 1 1 d . . . . .
H18 H 0.8672 0.2157 0.3916 0.087 Uiso 1 1 calc R U . . .
C19 C 0.7324(3) 0.31266(13) 0.7735(5) 0.0602(16) Uani 1 1 d . . . . .
H19 H 0.7418 0.3209 0.8382 0.072 Uiso 1 1 calc R U . . .
C20 C 0.8075(3) 0.35394(12) 0.7038(5) 0.0688(17) Uani 1 1 d . . . . .
H20A H 0.8463 0.3493 0.6617 0.083 Uiso 1 1 calc R U . . .
H20B H 0.8226 0.3560 0.7740 0.083 Uiso 1 1 calc R U . . .
C21 C 0.7768(4) 0.38598(14) 0.6699(6) 0.0772(18) Uani 1 1 d . . . . .
H21A H 0.7355 0.3894 0.7072 0.093 Uiso 1 1 calc R U . . .
H21B H 0.8071 0.4037 0.6873 0.093 Uiso 1 1 calc R U . . .
C22 C 0.7623(4) 0.38732(14) 0.5570(6) 0.0713(18) Uani 1 1 d . . . . .
C23 C 0.8096(5) 0.3969(2) 0.4890(9) 0.116(3) Uani 1 1 d . . . . .
H23 H 0.8520 0.4030 0.5116 0.139 Uiso 1 1 calc R U . . .
C24 C 0.7946(10) 0.3974(3) 0.3865(10) 0.168(6) Uani 1 1 d . . . . .
H24 H 0.8269 0.4038 0.3394 0.201 Uiso 1 1 calc R U . . .
C25 C 0.7321(10) 0.3886(3) 0.3539(10) 0.146(5) Uani 1 1 d . . . . .
H25 H 0.7207 0.3892 0.2850 0.176 Uiso 1 1 calc R U . . .
C26 C 0.6877(6) 0.3789(2) 0.4256(10) 0.124(3) Uani 1 1 d . . . . .
H26 H 0.6453 0.3724 0.4044 0.148 Uiso 1 1 calc R U . . .
C4 C 0.5091(4) 0.2263(2) 0.9378(7) 0.114(3) Uani 1 1 d . . . . .
H4A H 0.5078 0.2080 0.8916 0.170 Uiso 1 1 calc R U . . .
H4B H 0.4855 0.2444 0.9082 0.170 Uiso 1 1 calc R U . . .
H4C H 0.4883 0.2203 1.0012 0.170 Uiso 1 1 calc R U . . .
C2 C 0.6186(4) 0.2052(2) 0.9900(7) 0.137(4) Uani 1 1 d . . . . .
H2A H 0.6149 0.1890 0.9373 0.206 Uiso 1 1 calc R U . . .
H2B H 0.5993 0.1970 1.0521 0.206 Uiso 1 1 calc R U . . .
H2C H 0.6650 0.2103 1.0013 0.206 Uiso 1 1 calc R U . . .
C1 C 0.5832(7) 0.2618(2) 1.0409(7) 0.164(5) Uani 1 1 d . . . . .
H1A H 0.5625 0.2533 1.1015 0.246 Uiso 1 1 calc R U . . .
H1B H 0.5593 0.2809 1.0185 0.246 Uiso 1 1 calc R U . . .
H1C H 0.6288 0.2676 1.0555 0.246 Uiso 1 1 calc R U . . .
Cl1 Cl 0.74272(9) 0.38284(3) 0.98161(15) 0.0764(5) Uani 1 1 d . . . . .
O2 O 0.6947(3) 0.35825(12) 0.9604(5) 0.1186(19) Uani 1 1 d . . . . .
O3 O 0.7320(4) 0.39446(17) 1.0790(5) 0.159(3) Uani 1 1 d . . . . .
O4 O 0.7381(3) 0.40903(15) 0.9142(5) 0.131(2) Uani 1 1 d . . . . .
O5 O 0.8060(3) 0.36894(15) 0.9728(6) 0.136(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 2.111(4) . ?
Mn1 O1 2.111(4) 14_655 ?
Mn1 N2 2.226(5) . ?
Mn1 N2 2.226(5) 14_655 ?
Mn1 N1 2.257(4) 14_655 ?
Mn1 N1 2.257(4) . ?
O1 C8 1.283(6) . ?
N1 C11 1.273(7) . ?
N1 C12 1.488(7) . ?
N2 C18 1.330(7) . ?
N2 C14 1.339(7) . ?
N3 C19 1.283(7) . ?
N3 C20 1.466(7) . ?
N3 H3N 0.7887 . ?
N4 C22 1.331(8) . ?
N4 C26 1.339(12) . ?
C8 C7 1.427(7) . ?
C8 C9 1.427(7) . ?
C9 C10 1.398(8) . ?
C9 C19 1.410(8) . ?
C10 C5 1.371(7) . ?
C10 H10 0.9300 . ?
C5 C6 1.387(7) . ?
C5 C3 1.542(8) . ?
C3 C1 1.518(10) . ?
C3 C2 1.520(10) . ?
C3 C4 1.525(10) . ?
C6 C7 1.388(7) . ?
C6 H6 0.9300 . ?
C7 C11 1.444(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.510(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.492(8) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.391(9) . ?
C15 C16 1.384(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.343(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.365(9) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 C21 1.512(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.506(10) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.355(11) . ?
C23 C24 1.373(18) . ?
C23 H23 0.9300 . ?
C24 C25 1.369(18) . ?
C24 H24 0.9300 . ?
C25 C26 1.350(16) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
Cl1 O3 1.376(6) . ?
Cl1 O4 1.390(6) . ?
Cl1 O5 1.390(5) . ?
Cl1 O2 1.417(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 O1 95.4(2) . 14_655 ?
O1 Mn1 N2 164.84(15) . . ?
O1 Mn1 N2 88.90(15) 14_655 . ?
O1 Mn1 N2 88.90(15) . 14_655 ?
O1 Mn1 N2 164.84(15) 14_655 14_655 ?
N2 Mn1 N2 90.7(2) . 14_655 ?
O1 Mn1 N1 89.64(15) . 14_655 ?
O1 Mn1 N1 81.08(15) 14_655 14_655 ?
N2 Mn1 N1 105.40(17) . 14_655 ?
N2 Mn1 N1 84.42(17) 14_655 14_655 ?
O1 Mn1 N1 81.08(15) . . ?
O1 Mn1 N1 89.64(15) 14_655 . ?
N2 Mn1 N1 84.43(17) . . ?
N2 Mn1 N1 105.41(17) 14_655 . ?
N1 Mn1 N1 166.2(2) 14_655 . ?
C8 O1 Mn1 123.3(3) . . ?
C11 N1 C12 116.1(4) . . ?
C11 N1 Mn1 122.4(3) . . ?
C12 N1 Mn1 120.0(4) . . ?
C18 N2 C14 118.4(5) . . ?
C18 N2 Mn1 114.6(4) . . ?
C14 N2 Mn1 125.9(4) . . ?
C19 N3 C20 124.5(5) . . ?
C19 N3 H3N 116.7 . . ?
C20 N3 H3N 118.8 . . ?
C22 N4 C26 118.9(8) . . ?
O1 C8 C7 123.0(5) . . ?
O1 C8 C9 120.5(4) . . ?
C7 C8 C9 116.6(5) . . ?
C10 C9 C19 118.2(5) . . ?
C10 C9 C8 120.9(5) . . ?
C19 C9 C8 121.0(5) . . ?
C5 C10 C9 122.6(5) . . ?
C5 C10 H10 118.7 . . ?
C9 C10 H10 118.7 . . ?
C10 C5 C6 116.2(5) . . ?
C10 C5 C3 122.8(6) . . ?
C6 C5 C3 120.9(5) . . ?
C1 C3 C2 111.2(8) . . ?
C1 C3 C4 108.8(7) . . ?
C2 C3 C4 107.0(6) . . ?
C1 C3 C5 111.4(5) . . ?
C2 C3 C5 107.8(5) . . ?
C4 C3 C5 110.6(6) . . ?
C5 C6 C7 124.7(5) . . ?
C5 C6 H6 117.6 . . ?
C7 C6 H6 117.6 . . ?
C6 C7 C8 118.9(5) . . ?
C6 C7 C11 118.3(4) . . ?
C8 C7 C11 122.7(5) . . ?
N1 C11 C7 127.3(5) . . ?
N1 C11 H11 116.4 . . ?
C7 C11 H11 116.4 . . ?
N1 C12 C13 112.8(5) . . ?
N1 C12 H12A 109.0 . . ?
C13 C12 H12A 109.0 . . ?
N1 C12 H12B 109.0 . . ?
C13 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C14 C13 C12 115.0(5) . . ?
C14 C13 H13A 108.5 . . ?
C12 C13 H13A 108.5 . . ?
C14 C13 H13B 108.5 . . ?
C12 C13 H13B 108.5 . . ?
H13A C13 H13B 107.5 . . ?
N2 C14 C15 120.6(6) . . ?
N2 C14 C13 117.5(5) . . ?
C15 C14 C13 122.0(6) . . ?
C16 C15 C14 118.8(7) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
C17 C16 C15 120.1(7) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 118.1(6) . . ?
C16 C17 H17 121.0 . . ?
C18 C17 H17 121.0 . . ?
N2 C18 C17 123.9(6) . . ?
N2 C18 H18 118.1 . . ?
C17 C18 H18 118.1 . . ?
N3 C19 C9 124.6(5) . . ?
N3 C19 H19 117.7 . . ?
C9 C19 H19 117.7 . . ?
N3 C20 C21 112.4(5) . . ?
N3 C20 H20A 109.1 . . ?
C21 C20 H20A 109.1 . . ?
N3 C20 H20B 109.1 . . ?
C21 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
C22 C21 C20 113.4(5) . . ?
C22 C21 H21A 108.9 . . ?
C20 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
C20 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
N4 C22 C23 120.9(8) . . ?
N4 C22 C21 117.8(7) . . ?
C23 C22 C21 121.3(8) . . ?
C22 C23 C24 119.6(11) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 H23 120.2 . . ?
C25 C24 C23 119.9(13) . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C26 C25 C24 117.4(12) . . ?
C26 C25 H25 121.3 . . ?
C24 C25 H25 121.3 . . ?
N4 C26 C25 123.3(12) . . ?
N4 C26 H26 118.3 . . ?
C25 C26 H26 118.3 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C1 H1A 109.5 . . ?
C3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O3 Cl1 O4 108.1(5) . . ?
O3 Cl1 O5 111.0(5) . . ?
O4 Cl1 O5 108.8(4) . . ?
O3 Cl1 O2 108.7(4) . . ?
O4 Cl1 O2 112.1(4) . . ?
O5 Cl1 O2 108.0(3) . . ?

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 H3N O1 0.79 1.99 2.607(5) 135.2 .
C16 H16 O2 0.93 2.60 3.421(10) 147.7 14_654
C19 H19 O2 0.93 2.40 3.164(8) 139.0 .

_refine_diff_density_max         0.169
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.035


# start Validation Reply Form
_vrf_THETM01_dd491b              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: At higher \t angles all reflections were unobservable what affects the 
maximum, possible to measure, resolution.
;
_vrf_PLAT090_dd491b              
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.60 Note  
RESPONSE: At higher \t angles all reflections were unobservable what affects the 
maximum, possible to measure, resolution, and consequently affects the number
of measured reflection, and finally the data to parameter ratio.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_pamn1
_database_code_depnum_ccdc_archive 'CCDC 1025943'
_audit_update_record             
;
2016-06-27 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H30 Mn N6 O S2'
_chemical_formula_weight         585.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

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

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

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

_cell_length_a                   10.4398(10)
_cell_length_b                   10.9965(10)
_cell_length_c                   13.7776(18)
_cell_angle_alpha                80.040(17)
_cell_angle_beta                 79.204(12)
_cell_angle_gamma                72.490(9)
_cell_volume                     1470.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    131
_cell_measurement_theta_min      2
_cell_measurement_theta_max      20

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_F_000             610
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.084
_exptl_absorpt_coefficient_mu    0.622
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_process_details   '(SADABS; Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19656
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.322
_diffrn_reflns_theta_max         28.408
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7266
_reflns_number_gt                4799
_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       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2016)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    
;XP in SHELXTL/PC (Sheldrick, 2008)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material  
;SHELXL-2014/7 (Sheldrick, 2015) and
 PLATON (Spek, 1990)
;
_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)+(0.0780P)²+1.6433P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7266
_refine_ls_number_parameters     380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0672
_refine_ls_wR_factor_ref         0.1946
_refine_ls_wR_factor_gt          0.1655
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.55680(5) 0.35559(5) 0.35179(4) 0.03900(17) Uani 1 1 d . . . . .
C1 C 0.0141(15) 1.0232(13) 0.3035(11) 0.126(6) Uani 0.66(2) 1 d . . P A 1
H1A H -0.0689 1.0897 0.2960 0.189 Uiso 0.66(2) 1 calc R U P A 1
H1B H 0.0791 1.0589 0.3206 0.189 Uiso 0.66(2) 1 calc R U P A 1
H1C H -0.0033 0.9573 0.3554 0.189 Uiso 0.66(2) 1 calc R U P A 1
C2 C -0.0325(14) 0.9173(11) 0.1772(14) 0.126(8) Uani 0.66(2) 1 d . . P A 1
H2A H -0.1169 0.9837 0.1787 0.189 Uiso 0.66(2) 1 calc R U P A 1
H2B H -0.0443 0.8442 0.2234 0.189 Uiso 0.66(2) 1 calc R U P A 1
H2C H -0.0038 0.8928 0.1113 0.189 Uiso 0.66(2) 1 calc R U P A 1
C4 C 0.1092(11) 1.0659(13) 0.1293(13) 0.158(11) Uani 0.66(2) 1 d . . P A 1
H4A H 0.1518 1.0299 0.0687 0.238 Uiso 0.66(2) 1 calc R U P A 1
H4B H 0.1713 1.0988 0.1531 0.238 Uiso 0.66(2) 1 calc R U P A 1
H4C H 0.0294 1.1344 0.1168 0.238 Uiso 0.66(2) 1 calc R U P A 1
C1' C -0.059(3) 0.946(4) 0.260(3) 0.22(3) Uani 0.34(2) 1 d . . P A 2
H1'1 H -0.0528 0.8562 0.2723 0.331 Uiso 0.34(2) 1 calc R U P A 2
H1'2 H -0.1310 0.9898 0.2212 0.331 Uiso 0.34(2) 1 calc R U P A 2
H1'3 H -0.0784 0.9806 0.3223 0.331 Uiso 0.34(2) 1 calc R U P A 2
C2' C 0.0484(19) 0.9690(19) 0.0964(14) 0.085(8) Uani 0.34(2) 1 d . . P A 2
H2'1 H 0.0200 0.8954 0.0910 0.127 Uiso 0.34(2) 1 calc R U P A 2
H2'2 H 0.1317 0.9679 0.0525 0.127 Uiso 0.34(2) 1 calc R U P A 2
H2'3 H -0.0204 1.0460 0.0785 0.127 Uiso 0.34(2) 1 calc R U P A 2
C4' C 0.094(5) 1.089(3) 0.219(4) 0.25(3) Uani 0.34(2) 1 d . . P A 2
H4'1 H 0.0448 1.1149 0.2817 0.382 Uiso 0.34(2) 1 calc R U P A 2
H4'2 H 0.0625 1.1540 0.1661 0.382 Uiso 0.34(2) 1 calc R U P A 2
H4'3 H 0.1890 1.0765 0.2184 0.382 Uiso 0.34(2) 1 calc R U P A 2
C3 C 0.0707(4) 0.9652(4) 0.2050(4) 0.0704(13) Uani 1 1 d . . . . .
C5 C 0.1963(4) 0.8517(3) 0.2255(3) 0.0511(9) Uani 1 1 d . . . . .
C6 C 0.1856(4) 0.7490(4) 0.2962(3) 0.0500(9) Uani 1 1 d . . . . .
H6 H 0.1010 0.7516 0.3335 0.060 Uiso 1 1 calc R U . . .
C7 C 0.2933(3) 0.6415(3) 0.3153(2) 0.0409(7) Uani 1 1 d . . . . .
C8 C 0.4237(3) 0.6348(3) 0.2593(2) 0.0372(7) Uani 1 1 d . . . . .
C9 C 0.4355(3) 0.7429(3) 0.1894(2) 0.0423(7) Uani 1 1 d . . . . .
C10 C 0.3231(4) 0.8473(3) 0.1741(3) 0.0511(9) Uani 1 1 d . . . . .
H10 H 0.3344 0.9165 0.1273 0.061 Uiso 1 1 calc R U . . .
O1 O 0.5274(2) 0.5365(2) 0.27039(19) 0.0497(6) Uani 1 1 d . . . . .
C11 C 0.2652(3) 0.5410(3) 0.3915(3) 0.0483(8) Uani 1 1 d . . . . .
H11 H 0.1764 0.5558 0.4239 0.058 Uiso 1 1 calc R U . . .
N1 N 0.3475(3) 0.4349(3) 0.4194(2) 0.0485(7) Uani 1 1 d . . . . .
C12 C 0.2885(4) 0.3480(4) 0.4968(4) 0.0691(12) Uani 1 1 d . . . . .
H12A H 0.1964 0.3939 0.5219 0.083 Uiso 1 1 calc R U . . .
H12B H 0.2841 0.2760 0.4669 0.083 Uiso 1 1 calc R U . . .
C13 C 0.3658(5) 0.2993(5) 0.5797(3) 0.0712(12) Uani 1 1 d . . . . .
H13A H 0.3061 0.2739 0.6374 0.085 Uiso 1 1 calc R U . . .
H13B H 0.3944 0.3689 0.5955 0.085 Uiso 1 1 calc R U . . .
C14 C 0.4894(4) 0.1871(4) 0.5627(3) 0.0570(10) Uani 1 1 d . . . . .
C15 C 0.5154(5) 0.0808(5) 0.6333(3) 0.0752(13) Uani 1 1 d . . . . .
H15 H 0.4518 0.0746 0.6897 0.090 Uiso 1 1 calc R U . . .
C16 C 0.6312(5) -0.0139(4) 0.6216(3) 0.0724(13) Uani 1 1 d . . . . .
H16 H 0.6479 -0.0861 0.6688 0.087 Uiso 1 1 calc R U . . .
C17 C 0.7242(5) -0.0020(5) 0.5386(4) 0.0872(17) Uani 1 1 d . . . . .
H17 H 0.8068 -0.0643 0.5287 0.105 Uiso 1 1 calc R U . . .
C18 C 0.6915(5) 0.1045(5) 0.4711(4) 0.0843(16) Uani 1 1 d . . . . .
H18 H 0.7538 0.1120 0.4141 0.101 Uiso 1 1 calc R U . . .
N2 N 0.5765(3) 0.1986(3) 0.4811(2) 0.0505(7) Uani 1 1 d . . . . .
C19 C 0.5644(4) 0.7482(3) 0.1353(3) 0.0481(8) Uani 1 1 d . . . . .
H19 H 0.5687 0.8216 0.0912 0.058 Uiso 1 1 calc R U . . .
N3 N 0.6747(3) 0.6585(3) 0.1434(2) 0.0508(8) Uani 1 1 d . . . . .
H3N H 0.670(4) 0.593(4) 0.179(3) 0.061 Uiso 1 1 d . U . . .
C20 C 0.8099(4) 0.6620(4) 0.0897(3) 0.0590(10) Uani 1 1 d . . . . .
H20A H 0.8240 0.6296 0.0263 0.071 Uiso 1 1 calc R U . . .
H20B H 0.8152 0.7501 0.0767 0.071 Uiso 1 1 calc R U . . .
C21 C 0.9157(4) 0.5837(5) 0.1487(3) 0.0701(12) Uani 1 1 d . . . . .
H21A H 0.9082 0.4964 0.1622 0.084 Uiso 1 1 calc R U . . .
H21B H 0.8999 0.6166 0.2122 0.084 Uiso 1 1 calc R U . . .
C22 C 1.0581(4) 0.5810(4) 0.0995(3) 0.0576(10) Uani 1 1 d . . . . .
C23 C 1.1680(4) 0.5004(5) 0.1403(3) 0.0721(12) Uani 1 1 d . . . . .
H23 H 1.1559 0.4442 0.1977 0.087 Uiso 1 1 calc R U . . .
C24 C 1.2960(5) 0.5035(6) 0.0954(4) 0.0825(15) Uani 1 1 d . . . . .
H24 H 1.3721 0.4516 0.1230 0.099 Uiso 1 1 calc R U . . .
C25 C 1.3092(5) 0.5837(5) 0.0102(4) 0.0829(15) Uani 1 1 d . . . . .
H25 H 1.3947 0.5880 -0.0216 0.099 Uiso 1 1 calc R U . . .
C26 C 1.1971(5) 0.6573(5) -0.0280(5) 0.096(2) Uani 1 1 d . . . . .
H26 H 1.2081 0.7108 -0.0872 0.116 Uiso 1 1 calc R U . . .
N6 N 0.5585(4) 0.2423(3) 0.2440(3) 0.0619(9) Uani 1 1 d . . . . .
C28 C 0.5567(4) 0.1825(4) 0.1862(3) 0.0532(9) Uani 1 1 d . . . . .
S1 S 0.5549(2) 0.09611(15) 0.10378(10) 0.1038(6) Uani 1 1 d . . . . .
N5 N 0.7565(3) 0.3606(3) 0.3551(3) 0.0634(9) Uani 1 1 d . . . . .
C29 C 0.8621(4) 0.3525(4) 0.3721(3) 0.0522(9) Uani 1 1 d . . . . .
S2 S 1.01063(11) 0.34329(15) 0.39682(11) 0.0810(4) Uani 1 1 d . . . . .
N4 N 1.0706(4) 0.6576(4) 0.0146(3) 0.0847(13) 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 2.073(2) . ?
Mn1 N6 2.091(3) . ?
Mn1 N5 2.111(3) . ?
Mn1 N1 2.185(3) . ?
Mn1 N2 2.249(3) . ?
C1 C3 1.540(13) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.466(12) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C4 C3 1.479(11) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C1' C3 1.48(3) . ?
C1' H1'1 0.9600 . ?
C1' H1'2 0.9600 . ?
C1' H1'3 0.9600 . ?
C2' C3 1.548(17) . ?
C2' H2'1 0.9600 . ?
C2' H2'2 0.9600 . ?
C2' H2'3 0.9600 . ?
C4' C3 1.50(4) . ?
C4' H4'1 0.9600 . ?
C4' H4'2 0.9600 . ?
C4' H4'3 0.9600 . ?
C3 C5 1.545(5) . ?
C5 C10 1.371(5) . ?
C5 C6 1.375(5) . ?
C6 C7 1.391(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.422(5) . ?
C7 C11 1.444(5) . ?
C8 O1 1.290(4) . ?
C8 C9 1.415(5) . ?
C9 C10 1.392(4) . ?
C9 C19 1.424(5) . ?
C10 H10 0.9300 . ?
C11 N1 1.271(4) . ?
C11 H11 0.9300 . ?
N1 C12 1.478(5) . ?
C12 C13 1.455(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.507(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 N2 1.320(5) . ?
C14 C15 1.379(6) . ?
C15 C16 1.341(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.370(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.361(6) . ?
C17 H17 0.9300 . ?
C18 N2 1.331(5) . ?
C18 H18 0.9300 . ?
C19 N3 1.280(4) . ?
C19 H19 0.9300 . ?
N3 C20 1.474(5) . ?
N3 H3N 0.81(4) . ?
C20 C21 1.465(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.508(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 N4 1.328(5) . ?
C22 C23 1.368(6) . ?
C23 C24 1.371(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.352(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.347(7) . ?
C25 H25 0.9300 . ?
C26 N4 1.340(5) . ?
C26 H26 0.9300 . ?
N6 C28 1.124(5) . ?
C28 S1 1.607(4) . ?
N5 C29 1.144(5) . ?
C29 S2 1.619(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 N6 101.71(12) . . ?
O1 Mn1 N5 87.07(11) . . ?
N6 Mn1 N5 109.65(15) . . ?
O1 Mn1 N1 83.29(10) . . ?
N6 Mn1 N1 109.14(14) . . ?
N5 Mn1 N1 141.16(14) . . ?
O1 Mn1 N2 161.08(11) . . ?
N6 Mn1 N2 96.96(13) . . ?
N5 Mn1 N2 89.55(12) . . ?
N1 Mn1 N2 87.76(11) . . ?
C3 C1 H1A 109.5 . . ?
C3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C1' H1'1 109.5 . . ?
C3 C1' H1'2 109.5 . . ?
H1'1 C1' H1'2 109.5 . . ?
C3 C1' H1'3 109.5 . . ?
H1'1 C1' H1'3 109.5 . . ?
H1'2 C1' H1'3 109.5 . . ?
C3 C2' H2'1 109.5 . . ?
C3 C2' H2'2 109.5 . . ?
H2'1 C2' H2'2 109.5 . . ?
C3 C2' H2'3 109.5 . . ?
H2'1 C2' H2'3 109.5 . . ?
H2'2 C2' H2'3 109.5 . . ?
C3 C4' H4'1 109.5 . . ?
C3 C4' H4'2 109.5 . . ?
H4'1 C4' H4'2 109.5 . . ?
C3 C4' H4'3 109.5 . . ?
H4'1 C4' H4'3 109.5 . . ?
H4'2 C4' H4'3 109.5 . . ?
C2 C3 C4 112.7(9) . . ?
C1' C3 C4' 113(3) . . ?
C2 C3 C1 108.8(9) . . ?
C4 C3 C1 108.0(10) . . ?
C2 C3 C5 109.6(5) . . ?
C4 C3 C5 111.0(5) . . ?
C1' C3 C5 114.2(11) . . ?
C4' C3 C5 110.1(13) . . ?
C1 C3 C5 106.4(6) . . ?
C1' C3 C2' 101(2) . . ?
C4' C3 C2' 110.4(17) . . ?
C5 C3 C2' 107.8(6) . . ?
C10 C5 C6 116.6(3) . . ?
C10 C5 C3 122.1(4) . . ?
C6 C5 C3 121.3(4) . . ?
C5 C6 C7 124.1(3) . . ?
C5 C6 H6 117.9 . . ?
C7 C6 H6 117.9 . . ?
C6 C7 C8 119.2(3) . . ?
C6 C7 C11 117.4(3) . . ?
C8 C7 C11 123.4(3) . . ?
O1 C8 C9 120.7(3) . . ?
O1 C8 C7 122.8(3) . . ?
C9 C8 C7 116.5(3) . . ?
C10 C9 C8 121.2(3) . . ?
C10 C9 C19 118.6(3) . . ?
C8 C9 C19 120.2(3) . . ?
C5 C10 C9 122.3(3) . . ?
C5 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
C8 O1 Mn1 134.7(2) . . ?
N1 C11 C7 127.7(3) . . ?
N1 C11 H11 116.1 . . ?
C7 C11 H11 116.1 . . ?
C11 N1 C12 115.7(3) . . ?
C11 N1 Mn1 127.2(2) . . ?
C12 N1 Mn1 116.4(2) . . ?
C13 C12 N1 113.0(4) . . ?
C13 C12 H12A 109.0 . . ?
N1 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
N1 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C12 C13 C14 115.5(4) . . ?
C12 C13 H13A 108.4 . . ?
C14 C13 H13A 108.4 . . ?
C12 C13 H13B 108.4 . . ?
C14 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?
N2 C14 C15 121.3(4) . . ?
N2 C14 C13 117.4(3) . . ?
C15 C14 C13 121.1(4) . . ?
C16 C15 C14 120.8(4) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 118.6(4) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
C18 C17 C16 117.6(4) . . ?
C18 C17 H17 121.2 . . ?
C16 C17 H17 121.2 . . ?
N2 C18 C17 124.5(4) . . ?
N2 C18 H18 117.7 . . ?
C17 C18 H18 117.7 . . ?
C14 N2 C18 117.1(3) . . ?
C14 N2 Mn1 128.9(3) . . ?
C18 N2 Mn1 114.0(3) . . ?
N3 C19 C9 124.3(3) . . ?
N3 C19 H19 117.9 . . ?
C9 C19 H19 117.9 . . ?
C19 N3 C20 125.6(3) . . ?
C19 N3 H3N 118(3) . . ?
C20 N3 H3N 116(3) . . ?
C21 C20 N3 110.3(3) . . ?
C21 C20 H20A 109.6 . . ?
N3 C20 H20A 109.6 . . ?
C21 C20 H20B 109.6 . . ?
N3 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
C20 C21 C22 114.2(4) . . ?
C20 C21 H21A 108.7 . . ?
C22 C21 H21A 108.7 . . ?
C20 C21 H21B 108.7 . . ?
C22 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
N4 C22 C23 122.4(4) . . ?
N4 C22 C21 116.8(4) . . ?
C23 C22 C21 120.8(4) . . ?
C22 C23 C24 119.3(5) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C25 C24 C23 118.4(5) . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
C26 C25 C24 119.4(4) . . ?
C26 C25 H25 120.3 . . ?
C24 C25 H25 120.3 . . ?
N4 C26 C25 123.6(5) . . ?
N4 C26 H26 118.2 . . ?
C25 C26 H26 118.2 . . ?
C28 N6 Mn1 178.7(4) . . ?
N6 C28 S1 179.6(5) . . ?
C29 N5 Mn1 168.8(4) . . ?
N5 C29 S2 179.1(4) . . ?
C22 N4 C26 116.8(4) . . ?

_refine_diff_density_max         0.929
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.075



# start Validation Reply Form
_vrf_PLAT213_pamn1               
;
PROBLEM: Atom C4'             has ADP max/min Ratio .....        5.7 prolat
RESPONSE: The tert-butyl group is disordered over two positions 
with 0.66 : 0.34 participation of domains. The C4' atom
belongs to minor domain atoms and exhibits some effects
of further disorder. 
The introduction of third domain leads to unstable refinement,
what can suggest the presence of some dynamic disorder.
;
_vrf_PLAT234_pamn1               
;
PROBLEM: Large Hirshfeld Difference C3     --  C4'     ..       0.32 Ang.  
RESPONSE: Not a real interactions, both atoms belong to different domains.
;
_vrf_PLAT220_pamn1               
;
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range        7.0 Ratio 
RESPONSE:  The tert-butyl group is disordered over two positions 
with 0.66 : 0.34 participation of domains. The disordered atoms
exhibit some effects of further disorder. 
The introduction of third domain leads to unstable refinement,
what can suggest the presence of some dynamic disorder,
causing _vrf_PLAT220_pamn1 alert.
;
_vrf_PLAT242_pamn1               
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C3 Check 
RESPONSE: False alarm occurs for terminal t-butyl moiety.  
;
# end Validation Reply Form
####################################################################### 
# 
# 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_dd546
_database_code_depnum_ccdc_archive 'CCDC 1025944'
_audit_update_record             
;
2016-06-27 deposited with the CCDC.
2016-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H34 Cl Mn N7 O7'
_chemical_formula_weight         671.01

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

_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                   9.8005(5)
_cell_length_b                   12.8410(6)
_cell_length_c                   14.5139(7)
_cell_angle_alpha                65.0060(10)
_cell_angle_beta                 80.9370(10)
_cell_angle_gamma                70.8760(10)
_cell_volume                     1563.74(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(1)
_cell_measurement_reflns_used    583
_cell_measurement_theta_min      2
_cell_measurement_theta_max      20

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale pink'
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.069
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_F_000             698
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_absorpt_coefficient_mu    0.564
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      291(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 14
_diffrn_reflns_number            19093
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.829
_diffrn_reflns_theta_max         26.447
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             6222
_reflns_number_gt                4972
_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       'APEX2 (Bruker, 2005)'
_computing_cell_refinement       'SAINT-Plus (Bruker, 2008)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_molecular_graphics    
;XP in SHELXTL/PC (Sheldrick, 2008)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material  
;SHELXL-97 (Sheldrick, 2008) and
 PLATON (Spek, 1990)
;
_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)+(0.0599P)²+0.3584P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6222
_refine_ls_number_parameters     448
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.1151
_refine_ls_wR_factor_gt          0.1053
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.28841(3) 0.15495(3) 0.17287(2) 0.04170(12) Uani 1 1 d . . . . .
Cl1 Cl -0.01850(6) 0.23382(5) 0.44205(5) 0.05797(17) Uani 1 1 d . . . . .
O1 O 0.49685(16) 0.07326(14) 0.22823(13) 0.0550(4) Uani 1 1 d . . . . .
N3 N 0.34257(18) 0.00525(15) 0.12093(13) 0.0407(4) Uani 1 1 d . . . . .
O3 O 0.2626(2) 0.28494(17) 0.23843(17) 0.0655(5) Uani 1 1 d . . . . .
N1 N 0.6377(2) 0.10146(17) 0.34545(15) 0.0480(4) Uani 1 1 d . . . . .
O2 O 0.2099(2) 0.03774(19) 0.32019(14) 0.0665(5) Uani 1 1 d . . . . .
O7 O 0.1206(2) 0.2512(2) 0.43326(17) 0.0861(6) Uani 1 1 d . . . . .
C8 C 0.5980(2) -0.02320(18) 0.23281(15) 0.0397(4) Uani 1 1 d . . . . .
C9 C 0.5892(2) -0.09760(18) 0.18518(15) 0.0396(4) Uani 1 1 d . . . . .
N4 N 0.0631(2) 0.21423(16) 0.11840(15) 0.0510(4) Uani 1 1 d . . . . .
N2 N 0.6190(2) 0.20100(17) 0.60180(14) 0.0526(5) Uani 1 1 d . . . . .
C7 C 0.7248(2) -0.05911(18) 0.28791(15) 0.0409(4) Uani 1 1 d . . . . .
N5 N 0.3589(2) 0.28235(18) 0.02824(16) 0.0613(5) Uani 1 1 d . . . . .
C19 C 0.4615(2) -0.07816(18) 0.13311(16) 0.0423(5) Uani 1 1 d . . . . .
H19 H 0.4677 -0.1332 0.1056 0.051 Uiso 1 1 calc R U . . .
C6 C 0.8382(2) -0.16130(19) 0.29150(16) 0.0442(5) Uani 1 1 d . . . . .
H6 H 0.9199 -0.1825 0.3280 0.053 Uiso 1 1 calc R U . . .
C10 C 0.7061(2) -0.19794(18) 0.19153(15) 0.0421(5) Uani 1 1 d . . . . .
H10 H 0.6989 -0.2452 0.1596 0.051 Uiso 1 1 calc R U . . .
C11 C 0.7361(2) 0.00720(19) 0.34371(16) 0.0458(5) Uani 1 1 d . . . . .
H11 H 0.8191 -0.0196 0.3805 0.055 Uiso 1 1 calc R U . . .
C5 C 0.8324(2) -0.23192(18) 0.24243(15) 0.0410(4) Uani 1 1 d . . . . .
C3 C 0.9609(2) -0.3412(2) 0.24497(18) 0.0511(5) Uani 1 1 d . . . . .
C21 C 0.0824(2) 0.0154(2) 0.12903(19) 0.0534(6) Uani 1 1 d . . . . .
H21A H 0.0243 -0.0200 0.1095 0.064 Uiso 1 1 calc R U . . .
H21B H 0.1019 -0.0310 0.2008 0.064 Uiso 1 1 calc R U . . .
C14 C 0.5094(2) 0.2362(2) 0.54097(16) 0.0478(5) Uani 1 1 d . . . . .
C27 C 0.4284(2) 0.3290(2) -0.03612(18) 0.0496(5) Uani 1 1 d . . . . .
C22 C -0.0054(2) 0.1405(2) 0.11519(16) 0.0479(5) Uani 1 1 d . . . . .
N6 N 0.5086(3) 0.3698(2) -0.1136(2) 0.0965(9) Uani 1 1 d . . . . .
C20 C 0.2260(2) 0.0024(2) 0.06999(18) 0.0523(5) Uani 1 1 d . . . . .
H20A H 0.2539 -0.0730 0.0617 0.063 Uiso 1 1 calc R U . . .
H20B H 0.2137 0.0669 0.0028 0.063 Uiso 1 1 calc R U . . .
C23 C -0.1531(3) 0.1794(2) 0.10021(19) 0.0606(6) Uani 1 1 d . . . . .
H23 H -0.1989 0.1276 0.0979 0.073 Uiso 1 1 calc R U . . .
C15 C 0.3972(3) 0.3399(2) 0.5267(2) 0.0634(6) Uani 1 1 d . . . . .
H15 H 0.3215 0.3621 0.4845 0.076 Uiso 1 1 calc R U . . .
C28 C 0.5377(3) 0.4699(2) -0.1433(2) 0.0626(6) Uani 1 1 d . . . . .
C4 C 1.0095(4) -0.4211(2) 0.3541(2) 0.0796(8) Uani 1 1 d . . . . .
H4A H 1.0354 -0.3751 0.3827 0.119 Uiso 1 1 calc R U . . .
H4B H 1.0916 -0.4874 0.3544 0.119 Uiso 1 1 calc R U . . .
H4C H 0.9320 -0.4508 0.3939 0.119 Uiso 1 1 calc R U . . .
C2 C 0.9243(3) -0.4163(3) 0.2002(3) 0.0812(9) Uani 1 1 d . . . . .
H2A H 0.9016 -0.3690 0.1298 0.122 Uiso 1 1 calc R U . . .
H2B H 0.8427 -0.4422 0.2365 0.122 Uiso 1 1 calc R U . . .
H2C H 1.0057 -0.4853 0.2061 0.122 Uiso 1 1 calc R U . . .
C25 C -0.1612(3) 0.3693(3) 0.0902(3) 0.0833(9) Uani 1 1 d . . . . .
H25 H -0.2117 0.4479 0.0816 0.100 Uiso 1 1 calc R U . . .
C24 C -0.2318(3) 0.2943(3) 0.0888(2) 0.0773(8) Uani 1 1 d . . . . .
H24 H -0.3312 0.3205 0.0803 0.093 Uiso 1 1 calc R U . . .
C26 C -0.0156(3) 0.3276(2) 0.1045(2) 0.0679(7) Uani 1 1 d . . . . .
H26 H 0.0315 0.3797 0.1047 0.082 Uiso 1 1 calc R U . . .
C18 C 0.6186(3) 0.2718(3) 0.64798(19) 0.0672(7) Uani 1 1 d . . . . .
H18 H 0.6953 0.2486 0.6897 0.081 Uiso 1 1 calc R U . . .
C16 C 0.4000(4) 0.4100(2) 0.5766(2) 0.0780(9) Uani 1 1 d . . . . .
H16 H 0.3255 0.4802 0.5685 0.094 Uiso 1 1 calc R U . . .
C17 C 0.5124(4) 0.3759(3) 0.6377(2) 0.0771(9) Uani 1 1 d . . . . .
H17 H 0.5167 0.4223 0.6714 0.093 Uiso 1 1 calc R U . . .
C1 C 1.0861(3) -0.2948(3) 0.1824(3) 0.0855(9) Uani 1 1 d . . . . .
H1A H 1.0564 -0.2438 0.1138 0.128 Uiso 1 1 calc R U . . .
H1B H 1.1674 -0.3616 0.1826 0.128 Uiso 1 1 calc R U . . .
H1C H 1.1128 -0.2500 0.2117 0.128 Uiso 1 1 calc R U . . .
N7 N 0.5720(3) 0.5548(2) -0.1778(2) 0.0940(9) Uani 1 1 d . . . . .
O5 O -0.0685(11) 0.2924(10) 0.3438(5) 0.135(4) Uani 0.430(10) 1 d . . P A 1
O4 O 0.0014(6) 0.1154(4) 0.4754(8) 0.090(3) Uani 0.430(10) 1 d . . P A 1
O6 O -0.0938(10) 0.2872(12) 0.5058(10) 0.130(5) Uani 0.430(10) 1 d . . P A 1
O5' O -0.0340(4) 0.1889(8) 0.3690(5) 0.103(3) Uani 0.570(10) 1 d . . P A 2
O4' O -0.0378(5) 0.1409(5) 0.5405(4) 0.092(2) Uani 0.570(10) 1 d . . P A 2
O6' O -0.1376(6) 0.3332(4) 0.4317(7) 0.112(3) Uani 0.570(10) 1 d . . P A 2
C12 C 0.6384(3) 0.1687(2) 0.40499(18) 0.0518(5) Uani 1 1 d . . . . .
H12A H 0.6247 0.2526 0.3605 0.062 Uiso 1 1 calc R U . . .
H12B H 0.7311 0.1379 0.4372 0.062 Uiso 1 1 calc R U . . .
C13 C 0.5183(3) 0.1573(2) 0.48597(18) 0.0540(6) Uani 1 1 d . . . . .
H13A H 0.4269 0.1808 0.4543 0.065 Uiso 1 1 calc R U . . .
H13B H 0.5371 0.0744 0.5342 0.065 Uiso 1 1 calc R U . . .
H3O H 0.308(3) 0.335(3) 0.220(2) 0.084(10) Uiso 1 1 d . . . . .
H2O H 0.250(3) -0.034(3) 0.348(2) 0.069(9) Uiso 1 1 d . . . . .
H3P H 0.215(3) 0.283(3) 0.290(2) 0.076(10) Uiso 1 1 d . . . . .
H2P H 0.132(4) 0.066(3) 0.353(3) 0.096(11) Uiso 1 1 d . . . . .
H1N H 0.567(3) 0.121(2) 0.315(2) 0.068(9) Uiso 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 2.0784(15) . ?
Mn1 O3 2.1784(17) . ?
Mn1 N5 2.223(2) . ?
Mn1 O2 2.2247(18) . ?
Mn1 N3 2.2306(16) . ?
Mn1 N4 2.2408(19) . ?
Cl1 O4 1.340(5) . ?
Cl1 O6 1.364(6) . ?
Cl1 O5 1.382(6) . ?
Cl1 O6' 1.390(5) . ?
Cl1 O7 1.4298(19) . ?
Cl1 O5' 1.451(4) . ?
Cl1 O4' 1.457(4) . ?
O1 C8 1.291(2) . ?
N3 C19 1.274(3) . ?
N3 C20 1.473(3) . ?
O3 H3O 0.83(3) . ?
O3 H3P 0.82(3) . ?
N1 C11 1.284(3) . ?
N1 C12 1.459(3) . ?
N1 H1N 0.79(3) . ?
O2 H2O 0.81(3) . ?
O2 H2P 0.89(4) . ?
C8 C7 1.423(3) . ?
C8 C9 1.424(3) . ?
C9 C10 1.395(3) . ?
C9 C19 1.460(3) . ?
N4 C22 1.346(3) . ?
N4 C26 1.349(3) . ?
N2 C14 1.335(3) . ?
N2 C18 1.337(3) . ?
C7 C6 1.401(3) . ?
C7 C11 1.437(3) . ?
N5 C27 1.135(3) . ?
C19 H19 0.9300 . ?
C6 C5 1.387(3) . ?
C6 H6 0.9300 . ?
C10 C5 1.390(3) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C5 C3 1.539(3) . ?
C3 C2 1.520(3) . ?
C3 C4 1.528(4) . ?
C3 C1 1.535(4) . ?
C21 C22 1.496(3) . ?
C21 C20 1.527(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C14 C15 1.380(3) . ?
C14 C13 1.507(3) . ?
C27 N6 1.285(3) . ?
C22 C23 1.388(3) . ?
N6 C28 1.286(3) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C23 C24 1.373(4) . ?
C23 H23 0.9300 . ?
C15 C16 1.381(4) . ?
C15 H15 0.9300 . ?
C28 N7 1.130(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C25 C26 1.365(4) . ?
C25 C24 1.366(4) . ?
C25 H25 0.9300 . ?
C24 H24 0.9300 . ?
C26 H26 0.9300 . ?
C18 C17 1.364(4) . ?
C18 H18 0.9300 . ?
C16 C17 1.362(4) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C12 C13 1.523(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?

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 O3 88.49(7) . . ?
O1 Mn1 N5 92.92(8) . . ?
O3 Mn1 N5 88.05(8) . . ?
O1 Mn1 O2 88.58(8) . . ?
O3 Mn1 O2 88.54(8) . . ?
N5 Mn1 O2 176.23(8) . . ?
O1 Mn1 N3 83.41(6) . . ?
O3 Mn1 N3 171.51(7) . . ?
N5 Mn1 N3 94.86(7) . . ?
O2 Mn1 N3 88.74(7) . . ?
O1 Mn1 N4 171.13(6) . . ?
O3 Mn1 N4 98.77(7) . . ?
N5 Mn1 N4 92.42(8) . . ?
O2 Mn1 N4 86.53(8) . . ?
N3 Mn1 N4 89.08(6) . . ?
O4 Cl1 O6 116.3(6) . . ?
O4 Cl1 O5 110.5(5) . . ?
O6 Cl1 O5 113.7(6) . . ?
O4 Cl1 O7 107.3(3) . . ?
O6 Cl1 O7 103.5(4) . . ?
O5 Cl1 O7 104.3(3) . . ?
O6' Cl1 O7 116.8(3) . . ?
O6' Cl1 O5' 106.7(4) . . ?
O7 Cl1 O5' 111.59(19) . . ?
O6' Cl1 O4' 105.8(3) . . ?
O7 Cl1 O4' 110.91(18) . . ?
O5' Cl1 O4' 104.2(3) . . ?
C8 O1 Mn1 135.19(13) . . ?
C19 N3 C20 117.66(17) . . ?
C19 N3 Mn1 126.68(14) . . ?
C20 N3 Mn1 115.64(13) . . ?
Mn1 O3 H3O 126(2) . . ?
Mn1 O3 H3P 123(2) . . ?
H3O O3 H3P 111(3) . . ?
C11 N1 C12 126.3(2) . . ?
C11 N1 H1N 116(2) . . ?
C12 N1 H1N 117(2) . . ?
Mn1 O2 H2O 123(2) . . ?
Mn1 O2 H2P 122(2) . . ?
H2O O2 H2P 114(3) . . ?
O1 C8 C7 119.63(17) . . ?
O1 C8 C9 123.05(18) . . ?
C7 C8 C9 117.31(18) . . ?
C10 C9 C8 118.86(18) . . ?
C10 C9 C19 117.36(18) . . ?
C8 C9 C19 123.72(18) . . ?
C22 N4 C26 118.0(2) . . ?
C22 N4 Mn1 124.71(15) . . ?
C26 N4 Mn1 116.30(16) . . ?
C14 N2 C18 117.4(2) . . ?
C6 C7 C8 120.84(18) . . ?
C6 C7 C11 119.05(19) . . ?
C8 C7 C11 120.07(19) . . ?
C27 N5 Mn1 162.6(2) . . ?
N3 C19 C9 127.69(18) . . ?
N3 C19 H19 116.2 . . ?
C9 C19 H19 116.2 . . ?
C5 C6 C7 122.15(19) . . ?
C5 C6 H6 118.9 . . ?
C7 C6 H6 118.9 . . ?
C5 C10 C9 124.37(19) . . ?
C5 C10 H10 117.8 . . ?
C9 C10 H10 117.8 . . ?
N1 C11 C7 123.6(2) . . ?
N1 C11 H11 118.2 . . ?
C7 C11 H11 118.2 . . ?
C6 C5 C10 116.39(19) . . ?
C6 C5 C3 120.81(19) . . ?
C10 C5 C3 122.80(18) . . ?
C2 C3 C4 108.6(2) . . ?
C2 C3 C1 108.7(2) . . ?
C4 C3 C1 108.8(2) . . ?
C2 C3 C5 112.20(19) . . ?
C4 C3 C5 110.3(2) . . ?
C1 C3 C5 108.07(19) . . ?
C22 C21 C20 116.44(19) . . ?
C22 C21 H21A 108.2 . . ?
C20 C21 H21A 108.2 . . ?
C22 C21 H21B 108.2 . . ?
C20 C21 H21B 108.2 . . ?
H21A C21 H21B 107.3 . . ?
N2 C14 C15 122.3(2) . . ?
N2 C14 C13 115.7(2) . . ?
C15 C14 C13 122.0(2) . . ?
N5 C27 N6 171.6(2) . . ?
N4 C22 C23 120.9(2) . . ?
N4 C22 C21 117.94(19) . . ?
C23 C22 C21 121.2(2) . . ?
C27 N6 C28 125.1(2) . . ?
N3 C20 C21 112.65(18) . . ?
N3 C20 H20A 109.1 . . ?
C21 C20 H20A 109.1 . . ?
N3 C20 H20B 109.1 . . ?
C21 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
C24 C23 C22 120.2(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C14 C15 C16 118.5(3) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
N7 C28 N6 172.3(3) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C26 C25 C24 119.3(3) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
C25 C24 C23 118.6(3) . . ?
C25 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
N4 C26 C25 123.0(3) . . ?
N4 C26 H26 118.5 . . ?
C25 C26 H26 118.5 . . ?
N2 C18 C17 124.0(3) . . ?
N2 C18 H18 118.0 . . ?
C17 C18 H18 118.0 . . ?
C17 C16 C15 119.7(3) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 118.1(2) . . ?
C16 C17 H17 121.0 . . ?
C18 C17 H17 121.0 . . ?
C3 C1 H1A 109.5 . . ?
C3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C12 C13 110.11(17) . . ?
N1 C12 H12A 109.6 . . ?
C13 C12 H12A 109.6 . . ?
N1 C12 H12B 109.6 . . ?
C13 C12 H12B 109.6 . . ?
H12A C12 H12B 108.2 . . ?
C14 C13 C12 110.31(17) . . ?
C14 C13 H13A 109.6 . . ?
C12 C13 H13A 109.6 . . ?
C14 C13 H13B 109.6 . . ?
C12 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?

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
O2 H2O N2 0.81(3) 1.99(3) 2.791(3) 168(3) 2_656
O2 H2P O5' 0.89(4) 1.92(4) 2.752(5) 154(3) .
O2 H2P O4 0.89(4) 2.21(4) 3.059(10) 158(3) .
O2 H2P Cl1 0.89(4) 2.86(4) 3.647(2) 149(3) .
O3 H3P O7 0.82(3) 2.06(3) 2.871(3) 171(3) .
O3 H3P Cl1 0.82(3) 2.95(3) 3.706(2) 156(3) .
O3 H3O N7 0.83(3) 1.98(3) 2.801(3) 176(3) 2_665
N1 H1N O1 0.79(3) 1.91(3) 2.553(2) 138(3) .
C11 H11 O4' 0.93 2.33 3.220(5) 161.0 2_656
C12 H12B O5' 0.97 2.54 3.247(5) 130.2 1_655
C16 H16 O6' 0.93 2.50 3.421(5) 172.1 2_566

_refine_diff_density_max         0.244
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.045


# start Validation Reply Form
_vrf_PLAT934_dd546               
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          2 Check 
RESPONSE: Two reflections within dataset (i.e. 0 12 0 and 0 1 6) 
had large values of [I(obs)-I(calc)]/sigma
what probably originates from random effect, as these
(and subsequent reflection with considerably different
[I(obs)-I(calc)]/sigma) were placed in different positions
of reciprocal space, and there is no obvious relation between
these reflections.
;
# end Validation Reply Form
