# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

####################################################################### 
# 
# 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_skc-1g
_database_code_depnum_ccdc_archive 'CCDC 1571830'
_audit_update_record             
;
2017-08-31 deposited with the CCDC.
2018-03-07 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            'C29 H32 Cl Cu2 N5 O9'
_chemical_formula_weight         757.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   10.7931(2)
_cell_length_b                   26.2307(5)
_cell_length_c                   11.9127(2)
_cell_angle_alpha                90
_cell_angle_beta                 106.6950(10)
_cell_angle_gamma                90
_cell_volume                     3230.45(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4507
_cell_measurement_theta_min      1.946
_cell_measurement_theta_max      24.999

_exptl_crystal_description       plates
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_F_000             1552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    1.459
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_process_details   'Face indexing'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24714
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.946
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5673
_reflns_number_gt                4507
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0630P)²+2.9210P] 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         5673
_refine_ls_number_parameters     432
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0430
_refine_ls_wR_factor_ref         0.1339
_refine_ls_wR_factor_gt          0.1202
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_restrained_S_all      1.172
_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
O4 O 0.9039(19) 0.7647(6) 0.7902(12) 0.186(10) Uani 0.53(2) 1 d . . . . .
O5 O 0.7689(8) 0.8057(5) 0.7197(8) 0.212(7) Uani 0.92(2) 1 d . . . . .
O8 O 0.8685(5) 0.7685(3) 0.5989(5) 0.195(4) Uani 1 1 d . . . . .
Cu1 Cu 0.17246(4) 0.91537(2) 0.09338(4) 0.04372(16) Uani 1 1 d . . . . .
Cu2 Cu 0.40452(4) 0.85394(2) 0.23905(4) 0.04706(16) Uani 1 1 d . . . . .
C2 C 0.3971(4) 0.86114(14) -0.0080(3) 0.0437(9) Uani 1 1 d . . . . .
C7 C 0.2280(4) 0.99611(16) -0.0444(4) 0.0602(11) Uani 1 1 d . . . . .
C13 C 0.0098(4) 0.95601(16) -0.1231(4) 0.0545(10) Uani 1 1 d . . . . .
H13 H -0.0689 0.9574 -0.1813 0.065 Uiso 1 1 calc R U . . .
C12 C 0.1120(4) 0.98842(16) -0.1361(4) 0.0572(11) Uani 1 1 d . . . . .
C1 C 0.5238(4) 0.84061(14) 0.0137(4) 0.0464(9) Uani 1 1 d . . . . .
C3 C 0.3317(4) 0.87427(17) -0.1237(4) 0.0572(11) Uani 1 1 d . . . . .
H3 H 0.2482 0.8873 -0.1405 0.069 Uiso 1 1 calc R U . . .
C6 C 0.5773(4) 0.83544(18) -0.0809(4) 0.0606(12) Uani 1 1 d . . . . .
H6 H 0.6604 0.8223 -0.0669 0.073 Uiso 1 1 calc R U . . .
C11 C 0.0952(6) 1.01262(19) -0.2460(4) 0.0719(14) Uani 1 1 d . . . . .
H11 H 0.0174 1.0091 -0.3047 0.086 Uiso 1 1 calc R U . . .
C8 C 0.3247(5) 1.02717(17) -0.0692(5) 0.0732(14) Uani 1 1 d . . . . .
H8 H 0.4010 1.0337 -0.0106 0.088 Uiso 1 1 calc R U . . .
C5 C 0.5111(5) 0.84909(19) -0.1912(5) 0.0709(13) Uani 1 1 d . . . . .
H5 H 0.5486 0.8455 -0.2519 0.085 Uiso 1 1 calc R U . . .
C9 C 0.3066(7) 1.04779(19) -0.1792(6) 0.0844(17) Uani 1 1 d . . . . .
H9 H 0.3731 1.0666 -0.1945 0.101 Uiso 1 1 calc R U . . .
C10 C 0.1933(8) 1.04132(19) -0.2664(6) 0.0857(18) Uani 1 1 d . . . . .
H10 H 0.1826 1.0563 -0.3393 0.103 Uiso 1 1 calc R U . . .
C4 C 0.3876(5) 0.8684(2) -0.2131(4) 0.0693(13) Uani 1 1 d . . . . .
H4 H 0.3417 0.8776 -0.2891 0.083 Uiso 1 1 calc R U . . .
C14 C 0.6013(4) 0.82700(16) 0.1282(4) 0.0552(11) Uani 1 1 d . . . . .
H14 H 0.6825 0.8134 0.1341 0.066 Uiso 1 1 calc R U . . .
C16 C 0.2883(4) 0.77248(17) 0.3525(4) 0.0586(11) Uani 1 1 d . . . . .
H16A H 0.3367 0.7440 0.3346 0.070 Uiso 1 1 calc R U . . .
H16B H 0.2177 0.7588 0.3786 0.070 Uiso 1 1 calc R U . . .
C15 C 0.3767(5) 0.80443(19) 0.4506(4) 0.0617(12) Uani 1 1 d . . . . .
H15A H 0.3255 0.8292 0.4784 0.074 Uiso 1 1 calc R U . . .
H15B H 0.4196 0.7825 0.5157 0.074 Uiso 1 1 calc R U . . .
O2 O 0.2897(3) 0.91418(10) 0.2561(2) 0.0476(6) Uani 1 1 d . . . . .
O1 O 0.3398(2) 0.86693(11) 0.0746(2) 0.0514(7) Uani 1 1 d . . . . .
N3 N 0.4738(4) 0.83096(16) 0.4074(3) 0.0572(9) Uani 1 1 d . . . . .
C18 C 0.2253(4) 0.91103(16) 0.3388(3) 0.0518(10) Uani 1 1 d . . . . .
C17 C 0.1360(4) 0.87254(17) 0.3344(3) 0.0517(10) Uani 1 1 d . . . . .
C21 C 0.0979(7) 0.9047(3) 0.5103(5) 0.0934(19) Uani 1 1 d . . . . .
H21 H 0.0547 0.9033 0.5674 0.112 Uiso 1 1 calc R U . . .
C19 C 0.0719(5) 0.8691(2) 0.4208(4) 0.0698(13) Uani 1 1 d . . . . .
H19 H 0.0123 0.8432 0.4181 0.084 Uiso 1 1 calc R U . . .
C20 C 0.2507(6) 0.94624(19) 0.4305(4) 0.0748(15) Uani 1 1 d . . . . .
H20 H 0.3100 0.9724 0.4344 0.090 Uiso 1 1 calc R U . . .
O3 O 0.2496(3) 0.97689(12) 0.0613(3) 0.0671(9) Uani 1 1 d . . . . .
Cl1 Cl 0.87939(13) 0.80039(7) 0.69157(12) 0.0850(5) Uani 1 1 d . . . . .
N4 N 0.0763(3) 0.85068(11) 0.1212(3) 0.0405(7) Uani 1 1 d . . . . .
N2 N 0.5704(3) 0.83162(14) 0.2234(3) 0.0540(9) Uani 1 1 d . . . . .
N5 N 0.2355(3) 0.80334(11) 0.2460(3) 0.0429(7) Uani 1 1 d . . . . .
C22 C 0.1161(4) 0.83165(15) 0.2434(3) 0.0459(9) Uani 1 1 d . . . . .
H22 H 0.0509 0.8076 0.2540 0.055 Uiso 1 1 calc R U . . .
N1 N 0.0187(3) 0.92536(12) -0.0376(3) 0.0482(8) Uani 1 1 d . . . . .
C23 C -0.0888(4) 0.89149(17) -0.0361(4) 0.0550(10) Uani 1 1 d . . . . .
H23A H -0.0975 0.8648 -0.0942 0.066 Uiso 1 1 calc R U . . .
H23B H -0.1691 0.9106 -0.0543 0.066 Uiso 1 1 calc R U . . .
C24 C -0.0610(4) 0.86858(17) 0.0837(4) 0.0523(10) Uani 1 1 d . . . . .
H24A H -0.0745 0.8938 0.1386 0.063 Uiso 1 1 calc R U . . .
H24B H -0.1188 0.8401 0.0824 0.063 Uiso 1 1 calc R U . . .
C26 C 0.5859(5) 0.7977(2) 0.4114(4) 0.0732(14) Uani 1 1 d . . . . .
H26A H 0.6401 0.7946 0.4916 0.088 Uiso 1 1 calc R U . . .
H26B H 0.5558 0.7640 0.3830 0.088 Uiso 1 1 calc R U . . .
C25 C 0.6618(4) 0.8198(2) 0.3377(4) 0.0747(14) Uani 1 1 d . . . . .
H25A H 0.7057 0.8505 0.3736 0.090 Uiso 1 1 calc R U . . .
H25B H 0.7261 0.7956 0.3286 0.090 Uiso 1 1 calc R U . . .
C27 C 0.0970(4) 0.80589(15) 0.0505(3) 0.0485(9) Uani 1 1 d . . . . .
H27A H 0.1314 0.8168 -0.0124 0.058 Uiso 1 1 calc R U . . .
H27B H 0.0165 0.7878 0.0171 0.058 Uiso 1 1 calc R U . . .
C28 C 0.1942(4) 0.77217(16) 0.1374(4) 0.0521(10) Uani 1 1 d . . . . .
H28A H 0.1540 0.7406 0.1514 0.063 Uiso 1 1 calc R U . . .
H28B H 0.2673 0.7641 0.1087 0.063 Uiso 1 1 calc R U . . .
C29 C 0.1880(7) 0.9420(3) 0.5142(5) 0.095(2) Uani 1 1 d . . . . .
H29 H 0.2068 0.9651 0.5760 0.114 Uiso 1 1 calc R U . . .
O6 O 1.0036(6) 0.8100(4) 0.7576(6) 0.160(5) Uani 0.877(18) 1 d . . . . .
O7 O 0.8565(12) 0.8508(4) 0.6507(10) 0.185(7) Uani 0.73(2) 1 d . . . . .
O10 O 0.4304(6) 0.0178(2) 0.2696(5) 0.157(2) Uani 1 1 d . . . . .
O9 O 0.6143(7) 0.9115(2) 0.5657(7) 0.177(3) Uani 1 1 d . . . . .
H3N H 0.495(4) 0.8541(17) 0.444(4) 0.047(14) 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
O4 Cl1 1.466(14) . ?
O5 Cl1 1.335(7) . ?
O8 Cl1 1.363(4) . ?
Cu1 O3 1.905(3) . ?
Cu1 N1 1.942(3) . ?
Cu1 O2 1.988(3) . ?
Cu1 N4 2.065(3) . ?
Cu1 O1 2.271(3) . ?
Cu2 O1 1.912(3) . ?
Cu2 N2 1.943(3) . ?
Cu2 N3 2.021(4) . ?
Cu2 O2 2.054(3) . ?
Cu2 N5 2.277(3) . ?
C2 O1 1.313(5) . ?
C2 C3 1.399(6) . ?
C2 C1 1.423(5) . ?
C7 O3 1.313(5) . ?
C7 C12 1.420(6) . ?
C7 C8 1.420(7) . ?
C13 N1 1.279(5) . ?
C13 C12 1.436(6) . ?
C13 H13 0.9300 . ?
C12 C11 1.419(6) . ?
C1 C6 1.413(6) . ?
C1 C14 1.425(6) . ?
C3 C4 1.376(6) . ?
C3 H3 0.9300 . ?
C6 C5 1.351(7) . ?
C6 H6 0.9300 . ?
C11 C10 1.377(8) . ?
C11 H11 0.9300 . ?
C8 C9 1.378(8) . ?
C8 H8 0.9300 . ?
C5 C4 1.378(7) . ?
C5 H5 0.9300 . ?
C9 C10 1.369(9) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C4 H4 0.9300 . ?
C14 N2 1.278(6) . ?
C14 H14 0.9300 . ?
C16 N5 1.475(5) . ?
C16 C15 1.529(6) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C15 N3 1.468(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
O2 C18 1.362(5) . ?
N3 C26 1.481(6) . ?
N3 H3N 0.75(4) . ?
C18 C17 1.387(6) . ?
C18 C20 1.396(6) . ?
C17 C19 1.397(6) . ?
C17 C22 1.496(5) . ?
C21 C29 1.370(9) . ?
C21 C19 1.384(8) . ?
C21 H21 0.9300 . ?
C19 H19 0.9300 . ?
C20 C29 1.361(8) . ?
C20 H20 0.9300 . ?
Cl1 O6 1.369(6) . ?
Cl1 O7 1.405(9) . ?
N4 C22 1.481(5) . ?
N4 C24 1.494(5) . ?
N4 C27 1.499(5) . ?
N2 C25 1.466(6) . ?
N5 C22 1.480(5) . ?
N5 C28 1.486(5) . ?
C22 H22 0.9800 . ?
N1 C23 1.465(5) . ?
C23 C24 1.497(6) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C26 C25 1.480(7) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C27 C28 1.526(6) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29 0.9300 . ?

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
O3 Cu1 N1 92.65(13) . . ?
O3 Cu1 O2 90.95(12) . . ?
N1 Cu1 O2 160.68(13) . . ?
O3 Cu1 N4 175.92(12) . . ?
N1 Cu1 N4 83.51(13) . . ?
O2 Cu1 N4 92.24(11) . . ?
O3 Cu1 O1 92.77(13) . . ?
N1 Cu1 O1 121.11(12) . . ?
O2 Cu1 O1 77.62(11) . . ?
N4 Cu1 O1 90.39(11) . . ?
O1 Cu2 N2 91.79(13) . . ?
O1 Cu2 N3 172.85(16) . . ?
N2 Cu2 N3 85.23(16) . . ?
O1 Cu2 O2 84.89(11) . . ?
N2 Cu2 O2 147.15(13) . . ?
N3 Cu2 O2 101.13(15) . . ?
O1 Cu2 N5 94.61(12) . . ?
N2 Cu2 N5 126.73(13) . . ?
N3 Cu2 N5 82.05(14) . . ?
O2 Cu2 N5 86.12(11) . . ?
O1 C2 C3 119.8(3) . . ?
O1 C2 C1 122.9(3) . . ?
C3 C2 C1 117.3(4) . . ?
O3 C7 C12 123.9(4) . . ?
O3 C7 C8 118.8(4) . . ?
C12 C7 C8 117.4(5) . . ?
N1 C13 C12 125.0(4) . . ?
N1 C13 H13 117.5 . . ?
C12 C13 H13 117.5 . . ?
C11 C12 C7 119.8(5) . . ?
C11 C12 C13 117.8(4) . . ?
C7 C12 C13 122.4(4) . . ?
C6 C1 C2 118.9(4) . . ?
C6 C1 C14 118.5(4) . . ?
C2 C1 C14 122.6(4) . . ?
C4 C3 C2 121.7(4) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C5 C6 C1 121.8(4) . . ?
C5 C6 H6 119.1 . . ?
C1 C6 H6 119.1 . . ?
C10 C11 C12 120.4(5) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C9 C8 C7 120.8(5) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C6 C5 C4 119.7(5) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C10 C9 C8 121.6(6) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C9 C10 C11 119.9(5) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C3 C4 C5 120.6(5) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
N2 C14 C1 126.5(4) . . ?
N2 C14 H14 116.8 . . ?
C1 C14 H14 116.8 . . ?
N5 C16 C15 111.0(3) . . ?
N5 C16 H16A 109.4 . . ?
C15 C16 H16A 109.4 . . ?
N5 C16 H16B 109.4 . . ?
C15 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
N3 C15 C16 110.1(4) . . ?
N3 C15 H15A 109.6 . . ?
C16 C15 H15A 109.6 . . ?
N3 C15 H15B 109.6 . . ?
C16 C15 H15B 109.6 . . ?
H15A C15 H15B 108.2 . . ?
C18 O2 Cu1 113.1(2) . . ?
C18 O2 Cu2 118.2(2) . . ?
Cu1 O2 Cu2 98.57(11) . . ?
C2 O1 Cu2 129.4(2) . . ?
C2 O1 Cu1 134.2(2) . . ?
Cu2 O1 Cu1 93.76(11) . . ?
C15 N3 C26 111.6(4) . . ?
C15 N3 Cu2 113.1(3) . . ?
C26 N3 Cu2 105.8(3) . . ?
C15 N3 H3N 108(4) . . ?
C26 N3 H3N 111(4) . . ?
Cu2 N3 H3N 108(3) . . ?
O2 C18 C17 120.7(3) . . ?
O2 C18 C20 120.0(4) . . ?
C17 C18 C20 119.3(4) . . ?
C18 C17 C19 120.3(4) . . ?
C18 C17 C22 120.2(4) . . ?
C19 C17 C22 119.3(4) . . ?
C29 C21 C19 119.5(5) . . ?
C29 C21 H21 120.3 . . ?
C19 C21 H21 120.3 . . ?
C21 C19 C17 119.4(6) . . ?
C21 C19 H19 120.3 . . ?
C17 C19 H19 120.3 . . ?
C29 C20 C18 119.5(5) . . ?
C29 C20 H20 120.3 . . ?
C18 C20 H20 120.3 . . ?
C7 O3 Cu1 123.4(3) . . ?
O5 Cl1 O8 113.0(5) . . ?
O5 Cl1 O6 129.4(4) . . ?
O8 Cl1 O6 114.9(4) . . ?
O5 Cl1 O7 84.8(7) . . ?
O8 Cl1 O7 109.4(6) . . ?
O6 Cl1 O7 94.1(7) . . ?
O5 Cl1 O4 80.4(9) . . ?
O8 Cl1 O4 102.1(7) . . ?
O6 Cl1 O4 74.7(7) . . ?
O7 Cl1 O4 148.4(8) . . ?
C22 N4 C24 112.5(3) . . ?
C22 N4 C27 103.9(3) . . ?
C24 N4 C27 111.9(3) . . ?
C22 N4 Cu1 114.7(2) . . ?
C24 N4 Cu1 101.2(2) . . ?
C27 N4 Cu1 113.0(2) . . ?
C14 N2 C25 121.8(4) . . ?
C14 N2 Cu2 126.6(3) . . ?
C25 N2 Cu2 111.6(3) . . ?
C16 N5 C22 114.4(3) . . ?
C16 N5 C28 113.1(3) . . ?
C22 N5 C28 102.5(3) . . ?
C16 N5 Cu2 103.6(2) . . ?
C22 N5 Cu2 114.1(2) . . ?
C28 N5 Cu2 109.4(2) . . ?
N5 C22 N4 101.2(3) . . ?
N5 C22 C17 113.7(3) . . ?
N4 C22 C17 114.3(3) . . ?
N5 C22 H22 109.1 . . ?
N4 C22 H22 109.1 . . ?
C17 C22 H22 109.1 . . ?
C13 N1 C23 120.8(3) . . ?
C13 N1 Cu1 125.2(3) . . ?
C23 N1 Cu1 113.9(3) . . ?
N1 C23 C24 108.2(3) . . ?
N1 C23 H23A 110.1 . . ?
C24 C23 H23A 110.1 . . ?
N1 C23 H23B 110.1 . . ?
C24 C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
N4 C24 C23 108.8(3) . . ?
N4 C24 H24A 109.9 . . ?
C23 C24 H24A 109.9 . . ?
N4 C24 H24B 109.9 . . ?
C23 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
C25 C26 N3 109.7(4) . . ?
C25 C26 H26A 109.7 . . ?
N3 C26 H26A 109.7 . . ?
C25 C26 H26B 109.7 . . ?
N3 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
N2 C25 C26 107.1(4) . . ?
N2 C25 H25A 110.3 . . ?
C26 C25 H25A 110.3 . . ?
N2 C25 H25B 110.3 . . ?
C26 C25 H25B 110.3 . . ?
H25A C25 H25B 108.5 . . ?
N4 C27 C28 104.9(3) . . ?
N4 C27 H27A 110.8 . . ?
C28 C27 H27A 110.8 . . ?
N4 C27 H27B 110.8 . . ?
C28 C27 H27B 110.8 . . ?
H27A C27 H27B 108.8 . . ?
N5 C28 C27 104.3(3) . . ?
N5 C28 H28A 110.9 . . ?
C27 C28 H28A 110.9 . . ?
N5 C28 H28B 110.9 . . ?
C27 C28 H28B 110.9 . . ?
H28A C28 H28B 108.9 . . ?
C20 C29 C21 122.1(5) . . ?
C20 C29 H29 119.0 . . ?
C21 C29 H29 119.0 . . ?

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
O3 C7 C12 C11 177.2(4) . . . . ?
C8 C7 C12 C11 -1.8(6) . . . . ?
O3 C7 C12 C13 -3.8(7) . . . . ?
C8 C7 C12 C13 177.2(4) . . . . ?
N1 C13 C12 C11 168.0(4) . . . . ?
N1 C13 C12 C7 -11.0(6) . . . . ?
O1 C2 C1 C6 179.5(4) . . . . ?
C3 C2 C1 C6 1.1(6) . . . . ?
O1 C2 C1 C14 -3.2(6) . . . . ?
C3 C2 C1 C14 178.4(4) . . . . ?
O1 C2 C3 C4 -179.4(4) . . . . ?
C1 C2 C3 C4 -1.0(6) . . . . ?
C2 C1 C6 C5 -0.5(6) . . . . ?
C14 C1 C6 C5 -177.9(4) . . . . ?
C7 C12 C11 C10 3.5(7) . . . . ?
C13 C12 C11 C10 -175.5(4) . . . . ?
O3 C7 C8 C9 179.5(4) . . . . ?
C12 C7 C8 C9 -1.5(7) . . . . ?
C1 C6 C5 C4 -0.3(7) . . . . ?
C7 C8 C9 C10 3.3(8) . . . . ?
C8 C9 C10 C11 -1.6(8) . . . . ?
C12 C11 C10 C9 -1.8(7) . . . . ?
C2 C3 C4 C5 0.2(8) . . . . ?
C6 C5 C4 C3 0.5(8) . . . . ?
C6 C1 C14 N2 176.4(4) . . . . ?
C2 C1 C14 N2 -0.9(7) . . . . ?
N5 C16 C15 N3 -51.4(5) . . . . ?
C3 C2 O1 Cu2 -178.5(3) . . . . ?
C1 C2 O1 Cu2 3.1(6) . . . . ?
C3 C2 O1 Cu1 -21.7(6) . . . . ?
C1 C2 O1 Cu1 159.9(3) . . . . ?
C16 C15 N3 C26 -83.4(5) . . . . ?
C16 C15 N3 Cu2 35.8(5) . . . . ?
Cu1 O2 C18 C17 53.8(4) . . . . ?
Cu2 O2 C18 C17 -60.6(4) . . . . ?
Cu1 O2 C18 C20 -127.3(4) . . . . ?
Cu2 O2 C18 C20 118.3(4) . . . . ?
O2 C18 C17 C19 179.0(4) . . . . ?
C20 C18 C17 C19 0.1(6) . . . . ?
O2 C18 C17 C22 4.4(6) . . . . ?
C20 C18 C17 C22 -174.4(4) . . . . ?
C29 C21 C19 C17 -1.3(9) . . . . ?
C18 C17 C19 C21 0.4(7) . . . . ?
C22 C17 C19 C21 174.9(5) . . . . ?
O2 C18 C20 C29 -178.5(5) . . . . ?
C17 C18 C20 C29 0.4(7) . . . . ?
C12 C7 O3 Cu1 27.9(6) . . . . ?
C8 C7 O3 Cu1 -153.1(3) . . . . ?
C1 C14 N2 C25 -175.4(4) . . . . ?
C1 C14 N2 Cu2 4.7(7) . . . . ?
C15 C16 N5 C22 -86.1(4) . . . . ?
C15 C16 N5 C28 157.1(4) . . . . ?
C15 C16 N5 Cu2 38.8(4) . . . . ?
C16 N5 C22 N4 -170.7(3) . . . . ?
C28 N5 C22 N4 -47.9(3) . . . . ?
Cu2 N5 C22 N4 70.2(3) . . . . ?
C16 N5 C22 C17 66.3(4) . . . . ?
C28 N5 C22 C17 -171.0(3) . . . . ?
Cu2 N5 C22 C17 -52.8(4) . . . . ?
C24 N4 C22 N5 164.1(3) . . . . ?
C27 N4 C22 N5 42.9(3) . . . . ?
Cu1 N4 C22 N5 -80.9(3) . . . . ?
C24 N4 C22 C17 -73.3(4) . . . . ?
C27 N4 C22 C17 165.5(3) . . . . ?
Cu1 N4 C22 C17 41.7(4) . . . . ?
C18 C17 C22 N5 57.1(5) . . . . ?
C19 C17 C22 N5 -117.4(4) . . . . ?
C18 C17 C22 N4 -58.4(5) . . . . ?
C19 C17 C22 N4 127.0(4) . . . . ?
C12 C13 N1 C23 -176.1(4) . . . . ?
C12 C13 N1 Cu1 -0.4(6) . . . . ?
C13 N1 C23 C24 -168.6(4) . . . . ?
Cu1 N1 C23 C24 15.3(4) . . . . ?
C22 N4 C24 C23 174.8(3) . . . . ?
C27 N4 C24 C23 -68.7(4) . . . . ?
Cu1 N4 C24 C23 51.9(3) . . . . ?
N1 C23 C24 N4 -45.9(4) . . . . ?
C15 N3 C26 C25 164.0(4) . . . . ?
Cu2 N3 C26 C25 40.6(5) . . . . ?
C14 N2 C25 C26 -145.0(5) . . . . ?
Cu2 N2 C25 C26 34.9(5) . . . . ?
N3 C26 C25 N2 -50.0(6) . . . . ?
C22 N4 C27 C28 -21.5(4) . . . . ?
C24 N4 C27 C28 -143.2(3) . . . . ?
Cu1 N4 C27 C28 103.4(3) . . . . ?
C16 N5 C28 C27 157.8(3) . . . . ?
C22 N5 C28 C27 34.2(4) . . . . ?
Cu2 N5 C28 C27 -87.3(3) . . . . ?
N4 C27 C28 N5 -7.7(4) . . . . ?
C18 C20 C29 C21 -1.4(9) . . . . ?
C19 C21 C29 C20 1.9(10) . . . . ?

_refine_diff_density_max         1.123
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.071

####################################################################### 
# 
# 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_SKC-15G_0m
_database_code_depnum_ccdc_archive 'CCDC 1571831'
_audit_update_record             
;
2017-08-31 deposited with the CCDC.
2018-03-07 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            'C32 H40 Cl Cu2 N5 O11'
_chemical_formula_weight         833.22

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   11.1835(3)
_cell_length_b                   15.4275(4)
_cell_length_c                   20.3944(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.173(2)
_cell_angle_gamma                90
_cell_volume                     3452.02(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4175
_cell_measurement_theta_min      1.667
_cell_measurement_theta_max      25.000

_exptl_crystal_description       blocks
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_F_000             1720
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    1.377
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.596
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_process_details   'face indexing'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44015
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.667
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6083
_reflns_number_gt                4175
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+1.2822P] 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         6083
_refine_ls_number_parameters     475
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.1640
_refine_ls_wR_factor_gt          0.1405
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
Cu1 Cu 0.50891(5) 0.09410(4) 0.21118(3) 0.0480(2) Uani 1 1 d . . . . .
Cu2 Cu 0.67572(5) 0.06240(4) 0.10861(3) 0.0556(2) Uani 1 1 d . . . . .
Cl1 Cl 0.00479(13) 0.29492(9) 0.94431(6) 0.0649(4) Uani 1 1 d . . . . .
N2 N 0.4622(4) 0.1198(2) 0.29691(17) 0.0493(9) Uani 1 1 d . . . . .
N3 N 0.6431(3) 0.1873(2) 0.24266(18) 0.0503(9) Uani 1 1 d . . . . .
N1 N 0.7568(4) -0.0389(3) 0.07994(19) 0.0572(10) Uani 1 1 d . . . . .
N5 N 0.7264(4) 0.1220(3) 0.0301(2) 0.0604(11) Uani 1 1 d . . . . .
N4 N 0.7653(3) 0.1822(3) 0.16403(19) 0.0576(10) Uani 1 1 d . . . . .
C7 C 0.3667(4) 0.0922(3) 0.3161(2) 0.0504(11) Uani 1 1 d . . . . .
H7 H 0.3513 0.1144 0.3561 0.060 Uiso 1 1 calc R U . . .
C19 C 0.8267(5) 0.0703(4) 0.0129(3) 0.0693(15) Uani 1 1 d . . . . .
H19A H 0.9014 0.0810 0.0450 0.083 Uiso 1 1 calc R U . . .
H19B H 0.8398 0.0859 -0.0312 0.083 Uiso 1 1 calc R U . . .
C24 C 0.6736(4) -0.0983(3) 0.2749(2) 0.0553(12) Uani 1 1 d . . . . .
H24 H 0.6277 -0.0632 0.2977 0.066 Uiso 1 1 calc R U . . .
C12 C 0.4949(4) 0.2036(3) 0.0980(2) 0.0464(11) Uani 1 1 d . . . . .
C5 C 0.1822(4) 0.0086(3) 0.3122(2) 0.0524(11) Uani 1 1 d . . . . .
H5 H 0.1754 0.0344 0.3525 0.063 Uiso 1 1 calc R U . . .
C6 C 0.2813(4) 0.0304(3) 0.2821(2) 0.0461(10) Uani 1 1 d . . . . .
C10 C 0.6767(4) 0.2403(3) 0.1873(2) 0.0508(11) Uani 1 1 d . . . . .
H10 H 0.7196 0.2925 0.2067 0.061 Uiso 1 1 calc R U . . .
C1 C 0.2924(4) -0.0071(3) 0.2201(2) 0.0451(10) Uani 1 1 d . . . . .
C11 C 0.5700(4) 0.2671(3) 0.1352(2) 0.0484(11) Uani 1 1 d . . . . .
C13 C 0.4034(4) 0.2312(3) 0.0460(2) 0.0528(12) Uani 1 1 d . . . . .
H13 H 0.3560 0.1902 0.0194 0.063 Uiso 1 1 calc R U . . .
C4 C 0.0956(4) -0.0497(3) 0.2833(3) 0.0580(13) Uani 1 1 d . . . . .
C27 C 0.8047(4) -0.2074(3) 0.2070(2) 0.0540(12) Uani 1 1 d . . . . .
H27 H 0.8468 -0.2448 0.1838 0.065 Uiso 1 1 calc R U . . .
C26 C 0.7892(4) -0.2298(3) 0.2701(2) 0.0541(12) Uani 1 1 d . . . . .
C23 C 0.6932(4) -0.0725(3) 0.2116(2) 0.0494(11) Uani 1 1 d . . . . .
C9 C 0.5903(5) 0.2423(3) 0.2898(2) 0.0582(13) Uani 1 1 d . . . . .
H9A H 0.5251 0.2778 0.2652 0.070 Uiso 1 1 calc R U . . .
H9B H 0.6524 0.2803 0.3141 0.070 Uiso 1 1 calc R U . . .
C16 C 0.5471(4) 0.3546(3) 0.1215(2) 0.0519(12) Uani 1 1 d . . . . .
H16 H 0.5970 0.3961 0.1461 0.062 Uiso 1 1 calc R U . . .
C2 C 0.2002(4) -0.0656(3) 0.1916(2) 0.0518(12) Uani 1 1 d . . . . .
H2 H 0.2037 -0.0909 0.1506 0.062 Uiso 1 1 calc R U . . .
C25 C 0.7215(4) -0.1753(3) 0.3036(2) 0.0553(12) Uani 1 1 d . . . . .
H25 H 0.7084 -0.1908 0.3458 0.066 Uiso 1 1 calc R U . . .
C14 C 0.3813(5) 0.3195(4) 0.0329(2) 0.0613(13) Uani 1 1 d . . . . .
H14 H 0.3195 0.3366 -0.0021 0.074 Uiso 1 1 calc R U . . .
C8 C 0.5415(5) 0.1843(3) 0.3377(2) 0.0614(13) Uani 1 1 d . . . . .
H8A H 0.6080 0.1556 0.3675 0.074 Uiso 1 1 calc R U . . .
H8B H 0.4953 0.2178 0.3644 0.074 Uiso 1 1 calc R U . . .
C22 C 0.7586(4) -0.1294(3) 0.1766(2) 0.0498(11) Uani 1 1 d . . . . .
C15 C 0.4512(5) 0.3811(3) 0.0717(2) 0.0568(12) Uani 1 1 d . . . . .
C3 C 0.1057(5) -0.0862(3) 0.2222(2) 0.0568(12) Uani 1 1 d . . . . .
H3 H 0.0469 -0.1254 0.2018 0.068 Uiso 1 1 calc R U . . .
C21 C 0.7854(4) -0.1104(3) 0.1125(2) 0.0579(13) Uani 1 1 d . . . . .
H21 H 0.8264 -0.1524 0.0926 0.069 Uiso 1 1 calc R U . . .
C18 C 0.7602(5) 0.2147(4) 0.0450(3) 0.0698(15) Uani 1 1 d . . . . .
H18A H 0.6870 0.2499 0.0387 0.084 Uiso 1 1 calc R U . . .
H18B H 0.8102 0.2352 0.0142 0.084 Uiso 1 1 calc R U . . .
C20 C 0.7912(5) -0.0240(4) 0.0145(3) 0.0695(15) Uani 1 1 d . . . . .
H20A H 0.7231 -0.0366 -0.0215 0.083 Uiso 1 1 calc R U . . .
H20B H 0.8591 -0.0609 0.0095 0.083 Uiso 1 1 calc R U . . .
C28 C 0.8468(5) 0.1567(4) 0.2267(3) 0.0715(15) Uani 1 1 d . . . . .
H28A H 0.9083 0.2007 0.2410 0.086 Uiso 1 1 calc R U . . .
H28B H 0.8869 0.1020 0.2215 0.086 Uiso 1 1 calc R U . . .
C17 C 0.8292(5) 0.2243(4) 0.1156(3) 0.0740(16) Uani 1 1 d . . . . .
H17A H 0.9095 0.1987 0.1193 0.089 Uiso 1 1 calc R U . . .
H17B H 0.8397 0.2854 0.1264 0.089 Uiso 1 1 calc R U . . .
C29 C 0.7613(4) 0.1480(4) 0.2766(2) 0.0668(15) Uani 1 1 d . . . . .
H29A H 0.7503 0.0876 0.2871 0.080 Uiso 1 1 calc R U . . .
H29B H 0.7940 0.1787 0.3177 0.080 Uiso 1 1 calc R U . . .
O4 O 0.8442(3) -0.3055(2) 0.29563(18) 0.0667(9) Uani 1 1 d . . . . .
O5 O -0.0030(3) -0.0755(3) 0.3097(2) 0.0811(12) Uani 1 1 d . . . . .
C30 C 0.8295(5) -0.3312(4) 0.3607(3) 0.0681(14) Uani 1 1 d . . . . .
H30A H 0.8639 -0.2878 0.3925 0.102 Uiso 1 1 calc R U . . .
H30B H 0.8705 -0.3854 0.3721 0.102 Uiso 1 1 calc R U . . .
H30C H 0.7444 -0.3378 0.3612 0.102 Uiso 1 1 calc R U . . .
C31 C -0.0124(6) -0.0439(5) 0.3732(3) 0.090(2) Uani 1 1 d . . . . .
H31A H 0.0586 -0.0605 0.4052 0.135 Uiso 1 1 calc R U . . .
H31B H -0.0838 -0.0677 0.3861 0.135 Uiso 1 1 calc R U . . .
H31C H -0.0185 0.0182 0.3717 0.135 Uiso 1 1 calc R U . . .
O1 O 0.3819(3) 0.0098(2) 0.18833(15) 0.0544(8) Uani 1 1 d . . . . .
O3 O 0.6476(3) 0.0029(2) 0.18682(16) 0.0562(8) Uani 1 1 d . . . . .
O2 O 0.5121(3) 0.1185(2) 0.11297(14) 0.0477(7) Uani 1 1 d . . . . .
O6 O 0.4328(4) 0.4696(2) 0.06637(19) 0.0768(11) Uani 1 1 d . . . . .
O9 O -0.0869(6) 0.3526(4) 0.9527(3) 0.144(2) Uani 1 1 d . . . . .
O8 O 0.0911(6) 0.3286(4) 0.9113(3) 0.153(3) Uani 1 1 d . . . . .
O10 O -0.0533(7) 0.2299(5) 0.9037(4) 0.186(3) Uani 1 1 d . . . . .
O7 O 0.0537(6) 0.2535(8) 0.9982(3) 0.245(5) Uani 1 1 d . . . . .
C32 C 0.3303(6) 0.4994(4) 0.0193(3) 0.0903(19) Uani 1 1 d . . . . .
H32A H 0.3338 0.4766 -0.0241 0.135 Uiso 1 1 calc R U . . .
H32B H 0.3312 0.5616 0.0178 0.135 Uiso 1 1 calc R U . . .
H32C H 0.2568 0.4801 0.0324 0.135 Uiso 1 1 calc R U . . .
O11 O 0.4411(4) 0.8960(3) 0.0951(2) 0.0756(11) Uani 1 1 d D . . . .
H11A H 0.427(7) 0.929(4) 0.132(3) 0.14(3) Uiso 1 1 d D . . . .
H11B H 0.473(6) 0.932(4) 0.064(3) 0.11(3) Uiso 1 1 d D . . . .
H5N H 0.657(6) 0.121(4) -0.005(3) 0.10(2) 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
Cu1 O1 1.915(3) . ?
Cu1 N2 1.960(4) . ?
Cu1 O2 2.045(3) . ?
Cu1 N3 2.088(4) . ?
Cu1 O3 2.221(3) . ?
Cu2 O3 1.919(3) . ?
Cu2 N1 1.952(4) . ?
Cu2 N5 2.021(4) . ?
Cu2 O2 2.042(3) . ?
Cu2 N4 2.293(4) . ?
Cl1 O7 1.297(6) . ?
Cl1 O8 1.380(5) . ?
Cl1 O10 1.381(7) . ?
Cl1 O9 1.393(5) . ?
N2 C7 1.281(6) . ?
N2 C8 1.478(6) . ?
N3 C9 1.487(6) . ?
N3 C29 1.497(6) . ?
N3 C10 1.499(6) . ?
N1 C21 1.295(6) . ?
N1 C20 1.477(6) . ?
N5 C19 1.472(7) . ?
N5 C18 1.496(7) . ?
N5 H5N 0.95(6) . ?
N4 C28 1.472(6) . ?
N4 C17 1.477(6) . ?
N4 C10 1.482(6) . ?
C7 C6 1.430(6) . ?
C7 H7 0.9300 . ?
C19 C20 1.510(8) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C24 C25 1.385(7) . ?
C24 C23 1.409(7) . ?
C24 H24 0.9300 . ?
C12 O2 1.354(5) . ?
C12 C13 1.389(6) . ?
C12 C11 1.412(6) . ?
C5 C4 1.368(7) . ?
C5 C6 1.409(6) . ?
C5 H5 0.9300 . ?
C6 C1 1.417(6) . ?
C10 C11 1.495(6) . ?
C10 H10 0.9800 . ?
C1 O1 1.320(5) . ?
C1 C2 1.409(6) . ?
C11 C16 1.393(7) . ?
C13 C14 1.401(7) . ?
C13 H13 0.9300 . ?
C4 O5 1.376(6) . ?
C4 C3 1.392(7) . ?
C27 C26 1.377(7) . ?
C27 C22 1.405(7) . ?
C27 H27 0.9300 . ?
C26 O4 1.373(6) . ?
C26 C25 1.396(7) . ?
C23 O3 1.329(5) . ?
C23 C22 1.419(6) . ?
C9 C8 1.503(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C16 C15 1.388(7) . ?
C16 H16 0.9300 . ?
C2 C3 1.365(7) . ?
C2 H2 0.9300 . ?
C25 H25 0.9300 . ?
C14 C15 1.379(7) . ?
C14 H14 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C22 C21 1.429(7) . ?
C15 O6 1.382(6) . ?
C3 H3 0.9300 . ?
C21 H21 0.9300 . ?
C18 C17 1.504(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C28 C29 1.532(7) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
O4 C30 1.424(6) . ?
O5 C31 1.407(7) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
O6 C32 1.422(7) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O11 H11A 0.95(2) . ?
O11 H11B 0.97(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N2 92.37(14) . . ?
O1 Cu1 O2 92.25(12) . . ?
N2 Cu1 O2 153.47(15) . . ?
O1 Cu1 N3 175.84(14) . . ?
N2 Cu1 N3 83.47(15) . . ?
O2 Cu1 N3 91.52(13) . . ?
O1 Cu1 O3 91.85(13) . . ?
N2 Cu1 O3 130.26(14) . . ?
O2 Cu1 O3 75.65(12) . . ?
N3 Cu1 O3 90.78(13) . . ?
O3 Cu2 N1 91.51(16) . . ?
O3 Cu2 N5 173.24(17) . . ?
N1 Cu2 N5 84.75(18) . . ?
O3 Cu2 O2 82.77(13) . . ?
N1 Cu2 O2 145.55(15) . . ?
N5 Cu2 O2 103.48(16) . . ?
O3 Cu2 N4 95.88(14) . . ?
N1 Cu2 N4 127.49(15) . . ?
N5 Cu2 N4 82.04(16) . . ?
O2 Cu2 N4 86.95(13) . . ?
O7 Cl1 O8 112.2(5) . . ?
O7 Cl1 O10 102.9(7) . . ?
O8 Cl1 O10 105.8(5) . . ?
O7 Cl1 O9 114.2(5) . . ?
O8 Cl1 O9 114.9(3) . . ?
O10 Cl1 O9 105.4(5) . . ?
C7 N2 C8 119.8(4) . . ?
C7 N2 Cu1 126.0(3) . . ?
C8 N2 Cu1 113.8(3) . . ?
C9 N3 C29 111.0(4) . . ?
C9 N3 C10 111.3(4) . . ?
C29 N3 C10 104.0(4) . . ?
C9 N3 Cu1 103.8(3) . . ?
C29 N3 Cu1 112.4(3) . . ?
C10 N3 Cu1 114.5(3) . . ?
C21 N1 C20 120.9(4) . . ?
C21 N1 Cu2 127.7(3) . . ?
C20 N1 Cu2 111.3(3) . . ?
C19 N5 C18 113.1(4) . . ?
C19 N5 Cu2 106.6(3) . . ?
C18 N5 Cu2 111.8(3) . . ?
C19 N5 H5N 111(4) . . ?
C18 N5 H5N 108(4) . . ?
Cu2 N5 H5N 106(4) . . ?
C28 N4 C17 113.5(4) . . ?
C28 N4 C10 102.9(4) . . ?
C17 N4 C10 112.9(4) . . ?
C28 N4 Cu2 110.5(3) . . ?
C17 N4 Cu2 104.3(3) . . ?
C10 N4 Cu2 113.0(3) . . ?
N2 C7 C6 126.2(4) . . ?
N2 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
N5 C19 C20 107.5(4) . . ?
N5 C19 H19A 110.2 . . ?
C20 C19 H19A 110.2 . . ?
N5 C19 H19B 110.2 . . ?
C20 C19 H19B 110.2 . . ?
H19A C19 H19B 108.5 . . ?
C25 C24 C23 121.0(5) . . ?
C25 C24 H24 119.5 . . ?
C23 C24 H24 119.5 . . ?
O2 C12 C13 121.4(4) . . ?
O2 C12 C11 120.5(4) . . ?
C13 C12 C11 118.1(4) . . ?
C4 C5 C6 121.3(4) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 120.3(4) . . ?
C5 C6 C7 117.0(4) . . ?
C1 C6 C7 122.7(4) . . ?
N4 C10 C11 115.5(4) . . ?
N4 C10 N3 101.1(4) . . ?
C11 C10 N3 113.9(4) . . ?
N4 C10 H10 108.7 . . ?
C11 C10 H10 108.7 . . ?
N3 C10 H10 108.7 . . ?
O1 C1 C2 119.2(4) . . ?
O1 C1 C6 124.3(4) . . ?
C2 C1 C6 116.5(4) . . ?
C16 C11 C12 119.8(4) . . ?
C16 C11 C10 120.1(4) . . ?
C12 C11 C10 120.1(4) . . ?
C12 C13 C14 121.4(4) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C5 C4 O5 125.1(5) . . ?
C5 C4 C3 118.6(4) . . ?
O5 C4 C3 116.3(4) . . ?
C26 C27 C22 121.7(5) . . ?
C26 C27 H27 119.2 . . ?
C22 C27 H27 119.2 . . ?
O4 C26 C27 116.1(4) . . ?
O4 C26 C25 124.9(5) . . ?
C27 C26 C25 119.0(5) . . ?
O3 C23 C24 118.7(4) . . ?
O3 C23 C22 123.2(4) . . ?
C24 C23 C22 118.2(4) . . ?
N3 C9 C8 108.7(4) . . ?
N3 C9 H9A 109.9 . . ?
C8 C9 H9A 109.9 . . ?
N3 C9 H9B 109.9 . . ?
C8 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
C15 C16 C11 121.2(4) . . ?
C15 C16 H16 119.4 . . ?
C11 C16 H16 119.4 . . ?
C3 C2 C1 122.0(4) . . ?
C3 C2 H2 119.0 . . ?
C1 C2 H2 119.0 . . ?
C24 C25 C26 120.8(5) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C15 C14 C13 120.0(5) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
N2 C8 C9 106.7(4) . . ?
N2 C8 H8A 110.4 . . ?
C9 C8 H8A 110.4 . . ?
N2 C8 H8B 110.4 . . ?
C9 C8 H8B 110.4 . . ?
H8A C8 H8B 108.6 . . ?
C27 C22 C23 119.3(4) . . ?
C27 C22 C21 117.0(4) . . ?
C23 C22 C21 123.6(4) . . ?
C14 C15 O6 125.2(5) . . ?
C14 C15 C16 119.3(5) . . ?
O6 C15 C16 115.5(4) . . ?
C2 C3 C4 121.3(5) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
N1 C21 C22 124.6(5) . . ?
N1 C21 H21 117.7 . . ?
C22 C21 H21 117.7 . . ?
N5 C18 C17 110.6(5) . . ?
N5 C18 H18A 109.5 . . ?
C17 C18 H18A 109.5 . . ?
N5 C18 H18B 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
N1 C20 C19 106.5(4) . . ?
N1 C20 H20A 110.4 . . ?
C19 C20 H20A 110.4 . . ?
N1 C20 H20B 110.4 . . ?
C19 C20 H20B 110.4 . . ?
H20A C20 H20B 108.6 . . ?
N4 C28 C29 103.8(4) . . ?
N4 C28 H28A 111.0 . . ?
C29 C28 H28A 111.0 . . ?
N4 C28 H28B 111.0 . . ?
C29 C28 H28B 111.0 . . ?
H28A C28 H28B 109.0 . . ?
N4 C17 C18 111.8(4) . . ?
N4 C17 H17A 109.2 . . ?
C18 C17 H17A 109.2 . . ?
N4 C17 H17B 109.2 . . ?
C18 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
N3 C29 C28 105.4(4) . . ?
N3 C29 H29A 110.7 . . ?
C28 C29 H29A 110.7 . . ?
N3 C29 H29B 110.7 . . ?
C28 C29 H29B 110.7 . . ?
H29A C29 H29B 108.8 . . ?
C26 O4 C30 117.7(4) . . ?
C4 O5 C31 117.9(4) . . ?
O4 C30 H30A 109.5 . . ?
O4 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O4 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O5 C31 H31A 109.5 . . ?
O5 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O5 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C1 O1 Cu1 127.7(3) . . ?
C23 O3 Cu2 128.5(3) . . ?
C23 O3 Cu1 134.6(3) . . ?
Cu2 O3 Cu1 96.69(14) . . ?
C12 O2 Cu2 119.4(3) . . ?
C12 O2 Cu1 111.8(3) . . ?
Cu2 O2 Cu1 98.65(13) . . ?
C15 O6 C32 117.5(4) . . ?
O6 C32 H32A 109.5 . . ?
O6 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O6 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
H11A O11 H11B 110(6) . . ?

_refine_diff_density_max         0.752
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.071

####################################################################### 
# 
# 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_SKC-11G_0m
_database_code_depnum_ccdc_archive 'CCDC 1571832'
_audit_update_record             
;
2017-08-31 deposited with the CCDC.
2018-03-07 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            'C32 H37 N7 Ni2 O4 S2'
_chemical_formula_weight         765.22

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'
Ni Ni 0.3393 1.1124 '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'

_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                   10.4384(9)
_cell_length_b                   11.4113(10)
_cell_length_c                   15.0620(14)
_cell_angle_alpha                76.527(5)
_cell_angle_beta                 79.072(4)
_cell_angle_gamma                77.323(4)
_cell_volume                     1684.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5056
_cell_measurement_theta_min      1.405
_cell_measurement_theta_max      24.99

_exptl_crystal_description       plates
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_F_000             796
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_absorpt_coefficient_mu    1.290
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_process_details   'Face indexing'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16281
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.405
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             5904
_reflns_number_gt                5256
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0644P)²+1.2822P] 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         5904
_refine_ls_number_parameters     437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.1144
_refine_ls_wR_factor_gt          0.1087
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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
Ni1 Ni 0.35405(3) 0.83703(3) 0.30790(2) 0.03204(12) Uani 1 1 d . . . . .
Ni2 Ni 0.58974(3) 0.65543(3) 0.23577(2) 0.03688(12) Uani 1 1 d . . . . .
O2 O 0.53636(18) 0.75963(18) 0.33928(13) 0.0365(4) Uani 1 1 d . . . . .
O3 O 0.43707(19) 0.78767(17) 0.18546(12) 0.0369(4) Uani 1 1 d . . . . .
C1 C 0.3553(3) 0.7515(3) 0.14252(19) 0.0391(6) Uani 1 1 d . . . . .
C6 C 0.2882(3) 0.6555(3) 0.1873(2) 0.0409(6) Uani 1 1 d . . . . .
C5 C 0.1994(3) 0.6219(3) 0.1436(2) 0.0532(8) Uani 1 1 d . . . . .
H5 H 0.1543 0.5588 0.1742 0.064 Uiso 1 1 calc R U . . .
C7 C 0.3096(3) 0.5910(3) 0.2833(2) 0.0389(6) Uani 1 1 d . . . . .
H7 H 0.2577 0.5251 0.3029 0.047 Uiso 1 1 calc R U . . .
C2 C 0.3334(4) 0.8096(3) 0.0531(2) 0.0537(8) Uani 1 1 d . . . . .
H2 H 0.3783 0.8725 0.0215 0.064 Uiso 1 1 calc R U . . .
C4 C 0.1782(4) 0.6816(4) 0.0556(3) 0.0642(10) Uani 1 1 d . . . . .
H4 H 0.1188 0.6591 0.0267 0.077 Uiso 1 1 calc R U . . .
C3 C 0.2450(4) 0.7742(4) 0.0108(2) 0.0655(10) Uani 1 1 d . . . . .
H3 H 0.2310 0.8140 -0.0488 0.079 Uiso 1 1 calc R U . . .
N4 N 0.4499(2) 0.5383(2) 0.29557(16) 0.0377(5) Uani 1 1 d . . . . .
C13 C 0.5123(3) 0.8268(2) 0.48318(18) 0.0348(6) Uani 1 1 d . . . . .
C32 C 0.5883(3) 0.7699(2) 0.41068(18) 0.0344(6) Uani 1 1 d . . . . .
C14 C 0.3735(3) 0.8851(3) 0.48764(19) 0.0383(6) Uani 1 1 d . . . . .
H14 H 0.3364 0.9220 0.5379 0.046 Uiso 1 1 calc R U . . .
C11 C 0.7038(3) 0.7792(3) 0.5631(2) 0.0486(7) Uani 1 1 d . . . . .
H11 H 0.7413 0.7796 0.6142 0.058 Uiso 1 1 calc R U . . .
C9 C 0.7237(3) 0.7238(3) 0.4160(2) 0.0423(7) Uani 1 1 d . . . . .
H9 H 0.7767 0.6904 0.3677 0.051 Uiso 1 1 calc R U . . .
C12 C 0.5742(3) 0.8296(3) 0.5577(2) 0.0425(7) Uani 1 1 d . . . . .
H12 H 0.5246 0.8673 0.6050 0.051 Uiso 1 1 calc R U . . .
C10 C 0.7796(3) 0.7269(3) 0.4907(2) 0.0488(7) Uani 1 1 d . . . . .
H10 H 0.8689 0.6938 0.4930 0.059 Uiso 1 1 calc R U . . .
N1 N 0.2977(2) 0.8905(2) 0.42915(16) 0.0374(5) Uani 1 1 d . . . . .
C16 C 0.1172(3) 1.0116(3) 0.3498(2) 0.0517(8) Uani 1 1 d . . . . .
H16A H 0.0215 1.0369 0.3570 0.062 Uiso 1 1 calc R U . . .
H16B H 0.1565 1.0838 0.3229 0.062 Uiso 1 1 calc R U . . .
C15 C 0.1600(3) 0.9551(3) 0.4433(2) 0.0474(7) Uani 1 1 d . . . . .
H15A H 0.1533 1.0186 0.4779 0.057 Uiso 1 1 calc R U . . .
H15B H 0.1031 0.8983 0.4779 0.057 Uiso 1 1 calc R U . . .
C17 C 0.4434(3) 0.5059(3) 0.39765(19) 0.0437(7) Uani 1 1 d . . . . .
H17A H 0.5230 0.5182 0.4158 0.052 Uiso 1 1 calc R U . . .
H17B H 0.4342 0.4209 0.4206 0.052 Uiso 1 1 calc R U . . .
C18 C 0.3218(3) 0.5913(3) 0.43517(19) 0.0434(7) Uani 1 1 d . . . . .
H18A H 0.2555 0.5452 0.4718 0.052 Uiso 1 1 calc R U . . .
H18B H 0.3459 0.6388 0.4731 0.052 Uiso 1 1 calc R U . . .
N3 N 0.2714(2) 0.6724(2) 0.35168(15) 0.0359(5) Uani 1 1 d . . . . .
C19 C 0.1251(3) 0.7143(3) 0.3706(2) 0.0488(7) Uani 1 1 d . . . . .
H19A H 0.1018 0.7308 0.4325 0.059 Uiso 1 1 calc R U . . .
H19B H 0.0809 0.6491 0.3680 0.059 Uiso 1 1 calc R U . . .
C20 C 0.0753(3) 0.8289(3) 0.3025(2) 0.0511(8) Uani 1 1 d . . . . .
H20A H 0.0745 0.8070 0.2441 0.061 Uiso 1 1 calc R U . . .
H20B H -0.0151 0.8629 0.3257 0.061 Uiso 1 1 calc R U . . .
N2 N 0.1588(2) 0.9227(2) 0.28709(19) 0.0429(6) Uani 1 1 d . . . . .
N5 N 0.6223(3) 0.5651(2) 0.12991(18) 0.0478(6) Uani 1 1 d . . . . .
C21 C 0.5035(3) 0.4288(3) 0.2528(2) 0.0501(8) Uani 1 1 d . . . . .
H21A H 0.4357 0.3789 0.2638 0.060 Uiso 1 1 calc R U . . .
H21B H 0.5785 0.3800 0.2819 0.060 Uiso 1 1 calc R U . . .
C22 C 0.5472(4) 0.4642(3) 0.1495(2) 0.0543(8) Uani 1 1 d . . . . .
H22A H 0.6026 0.3939 0.1270 0.065 Uiso 1 1 calc R U . . .
H22B H 0.4700 0.4898 0.1177 0.065 Uiso 1 1 calc R U . . .
O1 O 0.7205(2) 0.7678(3) 0.15633(18) 0.0574(6) Uani 1 1 d . . . . .
C24 C 0.7778(4) 0.6812(4) 0.0200(3) 0.0611(9) Uani 1 1 d . . . . .
C23 C 0.7829(3) 0.7725(3) 0.0669(2) 0.0567(8) Uani 1 1 d . . . . .
N6 N 0.7412(3) 0.5306(3) 0.2915(2) 0.0567(7) Uani 1 1 d . . . . .
C8 C 0.8381(3) 0.4681(3) 0.3121(2) 0.0503(8) Uani 1 1 d . . . . .
S1 S 0.97592(11) 0.38264(12) 0.34329(9) 0.0848(4) Uani 1 1 d . . . . .
C26 C 0.8524(4) 0.6829(4) -0.0684(3) 0.0758(11) Uani 1 1 d . . . . .
H26 H 0.8522 0.6210 -0.0991 0.091 Uiso 1 1 calc R U . . .
O4 O 0.4289(3) 1.0072(2) 0.25485(19) 0.0537(6) Uani 1 1 d . . . . .
C27 C 0.8545(4) 0.8635(4) 0.0235(3) 0.0670(10) Uani 1 1 d . . . . .
H27 H 0.8563 0.9252 0.0539 0.080 Uiso 1 1 calc R U . . .
C28 C 0.9242(4) 0.8644(5) -0.0652(3) 0.0783(13) Uani 1 1 d . . . . .
H28 H 0.9703 0.9276 -0.0937 0.094 Uiso 1 1 calc R U . . .
C29 C 0.9253(4) 0.7721(5) -0.1110(3) 0.0841(14) Uani 1 1 d . . . . .
H29 H 0.9742 0.7707 -0.1693 0.101 Uiso 1 1 calc R U . . .
C30 C 0.6995(4) 0.5834(4) 0.0545(3) 0.0630(9) Uani 1 1 d . . . . .
H30 H 0.7077 0.5281 0.0163 0.076 Uiso 1 1 calc R U . . .
C25 C 0.4161(5) 1.0808(5) 0.1675(4) 0.1012(17) Uani 1 1 d . . . . .
H25A H 0.4428 1.0307 0.1217 0.152 Uiso 1 1 calc R U . . .
H25B H 0.4714 1.1414 0.1551 0.152 Uiso 1 1 calc R U . . .
H25C H 0.3252 1.1207 0.1658 0.152 Uiso 1 1 calc R U . . .
C31 C 0.7485(3) 0.0443(3) 0.2401(2) 0.0485(7) Uani 1 1 d . . . . .
N8 N 0.7174(4) -0.0348(4) 0.2197(3) 0.0892(12) Uani 1 1 d . . . . .
S2 S 0.78487(12) 0.15935(11) 0.26848(8) 0.0751(3) Uani 1 1 d . . . . .
H1O H 0.724(4) 0.817(3) 0.181(3) 0.052(12) Uiso 1 1 d . . . . .
H4O H 0.489(4) 0.992(4) 0.256(3) 0.052(15) Uiso 1 1 d . . . . .
H2N H 0.154(4) 0.965(3) 0.235(3) 0.054(11) 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
Ni1 N1 2.002(2) . ?
Ni1 O2 2.0084(18) . ?
Ni1 O3 2.0330(19) . ?
Ni1 N2 2.105(2) . ?
Ni1 N3 2.151(2) . ?
Ni1 O4 2.174(3) . ?
Ni2 N5 2.032(3) . ?
Ni2 N6 2.047(3) . ?
Ni2 O3 2.0642(19) . ?
Ni2 O1 2.091(2) . ?
Ni2 O2 2.0973(19) . ?
Ni2 N4 2.127(2) . ?
O2 C32 1.331(3) . ?
O3 C1 1.344(3) . ?
C1 C2 1.393(4) . ?
C1 C6 1.399(4) . ?
C6 C5 1.394(4) . ?
C6 C7 1.496(4) . ?
C5 C4 1.377(5) . ?
C5 H5 0.9300 . ?
C7 N4 1.485(4) . ?
C7 N3 1.487(4) . ?
C7 H7 0.9800 . ?
C2 C3 1.388(5) . ?
C2 H2 0.9300 . ?
C4 C3 1.368(6) . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?
N4 C17 1.487(4) . ?
N4 C21 1.490(4) . ?
C13 C12 1.407(4) . ?
C13 C32 1.421(4) . ?
C13 C14 1.452(4) . ?
C32 C9 1.406(4) . ?
C14 N1 1.274(4) . ?
C14 H14 0.9300 . ?
C11 C12 1.359(4) . ?
C11 C10 1.392(5) . ?
C11 H11 0.9300 . ?
C9 C10 1.373(4) . ?
C9 H9 0.9300 . ?
C12 H12 0.9300 . ?
C10 H10 0.9300 . ?
N1 C15 1.465(4) . ?
C16 N2 1.486(4) . ?
C16 C15 1.512(5) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C17 C18 1.523(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 N3 1.487(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
N3 C19 1.489(4) . ?
C19 C20 1.521(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 N2 1.475(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
N2 H2N 0.82(4) . ?
N5 C30 1.264(4) . ?
N5 C22 1.475(4) . ?
C21 C22 1.520(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
O1 C23 1.375(4) . ?
O1 H1O 0.75(4) . ?
C24 C23 1.403(5) . ?
C24 C26 1.409(5) . ?
C24 C30 1.467(5) . ?
C23 C27 1.379(5) . ?
N6 C8 1.152(4) . ?
C8 S1 1.634(3) . ?
C26 C29 1.370(6) . ?
C26 H26 0.9300 . ?
O4 C25 1.398(5) . ?
O4 H4O 0.62(4) . ?
C27 C28 1.393(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.386(7) . ?
C28 H28 0.9300 . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C31 N8 1.145(5) . ?
C31 S2 1.610(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
N1 Ni1 O2 91.84(9) . . ?
N1 Ni1 O3 171.84(9) . . ?
O2 Ni1 O3 81.53(8) . . ?
N1 Ni1 N2 82.84(10) . . ?
O2 Ni1 N2 174.69(9) . . ?
O3 Ni1 N2 103.77(9) . . ?
N1 Ni1 N3 95.13(9) . . ?
O2 Ni1 N3 96.26(8) . . ?
O3 Ni1 N3 90.34(8) . . ?
N2 Ni1 N3 84.24(10) . . ?
N1 Ni1 O4 87.48(10) . . ?
O2 Ni1 O4 87.20(10) . . ?
O3 Ni1 O4 87.46(9) . . ?
N2 Ni1 O4 92.57(11) . . ?
N3 Ni1 O4 175.59(10) . . ?
N5 Ni2 N6 88.52(11) . . ?
N5 Ni2 O3 94.95(9) . . ?
N6 Ni2 O3 176.47(10) . . ?
N5 Ni2 O1 87.89(11) . . ?
N6 Ni2 O1 92.00(12) . . ?
O3 Ni2 O1 87.49(9) . . ?
N5 Ni2 O2 173.52(9) . . ?
N6 Ni2 O2 97.84(10) . . ?
O3 Ni2 O2 78.70(7) . . ?
O1 Ni2 O2 93.10(9) . . ?
N5 Ni2 N4 83.93(10) . . ?
N6 Ni2 N4 92.33(11) . . ?
O3 Ni2 N4 88.68(8) . . ?
O1 Ni2 N4 170.64(10) . . ?
O2 Ni2 N4 94.52(8) . . ?
C32 O2 Ni1 126.98(17) . . ?
C32 O2 Ni2 136.60(17) . . ?
Ni1 O2 Ni2 96.09(8) . . ?
C1 O3 Ni1 115.29(16) . . ?
C1 O3 Ni2 116.85(17) . . ?
Ni1 O3 Ni2 96.37(8) . . ?
O3 C1 C2 121.0(3) . . ?
O3 C1 C6 120.7(2) . . ?
C2 C1 C6 118.3(3) . . ?
C5 C6 C1 120.3(3) . . ?
C5 C6 C7 120.0(3) . . ?
C1 C6 C7 119.7(3) . . ?
C4 C5 C6 120.3(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
N4 C7 N3 101.3(2) . . ?
N4 C7 C6 115.2(2) . . ?
N3 C7 C6 113.8(2) . . ?
N4 C7 H7 108.7 . . ?
N3 C7 H7 108.7 . . ?
C6 C7 H7 108.7 . . ?
C3 C2 C1 120.4(3) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C3 C4 C5 119.7(3) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C4 C3 C2 121.0(3) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C7 N4 C17 102.8(2) . . ?
C7 N4 C21 112.7(2) . . ?
C17 N4 C21 111.6(2) . . ?
C7 N4 Ni2 116.10(17) . . ?
C17 N4 Ni2 110.79(18) . . ?
C21 N4 Ni2 103.16(18) . . ?
C12 C13 C32 118.8(3) . . ?
C12 C13 C14 115.5(3) . . ?
C32 C13 C14 125.7(3) . . ?
O2 C32 C9 119.8(2) . . ?
O2 C32 C13 122.6(2) . . ?
C9 C32 C13 117.6(3) . . ?
N1 C14 C13 126.1(3) . . ?
N1 C14 H14 117.0 . . ?
C13 C14 H14 117.0 . . ?
C12 C11 C10 119.0(3) . . ?
C12 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
C10 C9 C32 121.6(3) . . ?
C10 C9 H9 119.2 . . ?
C32 C9 H9 119.2 . . ?
C11 C12 C13 122.3(3) . . ?
C11 C12 H12 118.9 . . ?
C13 C12 H12 118.9 . . ?
C9 C10 C11 120.6(3) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 H10 119.7 . . ?
C14 N1 C15 119.1(2) . . ?
C14 N1 Ni1 125.87(19) . . ?
C15 N1 Ni1 114.57(19) . . ?
N2 C16 C15 110.8(3) . . ?
N2 C16 H16A 109.5 . . ?
C15 C16 H16A 109.5 . . ?
N2 C16 H16B 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
N1 C15 C16 108.3(2) . . ?
N1 C15 H15A 110.0 . . ?
C16 C15 H15A 110.0 . . ?
N1 C15 H15B 110.0 . . ?
C16 C15 H15B 110.0 . . ?
H15A C15 H15B 108.4 . . ?
N4 C17 C18 105.5(2) . . ?
N4 C17 H17A 110.6 . . ?
C18 C17 H17A 110.6 . . ?
N4 C17 H17B 110.6 . . ?
C18 C17 H17B 110.6 . . ?
H17A C17 H17B 108.8 . . ?
N3 C18 C17 104.6(2) . . ?
N3 C18 H18A 110.8 . . ?
C17 C18 H18A 110.8 . . ?
N3 C18 H18B 110.8 . . ?
C17 C18 H18B 110.8 . . ?
H18A C18 H18B 108.9 . . ?
C18 N3 C7 102.3(2) . . ?
C18 N3 C19 110.6(2) . . ?
C7 N3 C19 112.6(2) . . ?
C18 N3 Ni1 112.80(18) . . ?
C7 N3 Ni1 113.21(16) . . ?
C19 N3 Ni1 105.53(18) . . ?
N3 C19 C20 112.7(2) . . ?
N3 C19 H19A 109.0 . . ?
C20 C19 H19A 109.0 . . ?
N3 C19 H19B 109.0 . . ?
C20 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
N2 C20 C19 111.9(3) . . ?
N2 C20 H20A 109.2 . . ?
C19 C20 H20A 109.2 . . ?
N2 C20 H20B 109.2 . . ?
C19 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C20 N2 C16 115.3(3) . . ?
C20 N2 Ni1 109.63(19) . . ?
C16 N2 Ni1 105.49(19) . . ?
C20 N2 H2N 109(3) . . ?
C16 N2 H2N 104(3) . . ?
Ni1 N2 H2N 114(3) . . ?
C30 N5 C22 119.4(3) . . ?
C30 N5 Ni2 127.9(3) . . ?
C22 N5 Ni2 112.68(19) . . ?
N4 C21 C22 112.0(3) . . ?
N4 C21 H21A 109.2 . . ?
C22 C21 H21A 109.2 . . ?
N4 C21 H21B 109.2 . . ?
C22 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
N5 C22 C21 109.9(3) . . ?
N5 C22 H22A 109.7 . . ?
C21 C22 H22A 109.7 . . ?
N5 C22 H22B 109.7 . . ?
C21 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
C23 O1 Ni2 130.2(2) . . ?
C23 O1 H1O 119(3) . . ?
Ni2 O1 H1O 110(3) . . ?
C23 C24 C26 118.1(4) . . ?
C23 C24 C30 125.7(3) . . ?
C26 C24 C30 116.2(4) . . ?
O1 C23 C27 120.9(4) . . ?
O1 C23 C24 119.7(3) . . ?
C27 C23 C24 119.4(3) . . ?
C8 N6 Ni2 170.1(3) . . ?
N6 C8 S1 178.1(3) . . ?
C29 C26 C24 122.5(4) . . ?
C29 C26 H26 118.7 . . ?
C24 C26 H26 118.7 . . ?
C25 O4 Ni1 124.9(3) . . ?
C25 O4 H4O 106(4) . . ?
Ni1 O4 H4O 104(4) . . ?
C23 C27 C28 121.1(4) . . ?
C23 C27 H27 119.5 . . ?
C28 C27 H27 119.5 . . ?
C29 C28 C27 120.5(4) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C26 C29 C28 118.4(4) . . ?
C26 C29 H29 120.8 . . ?
C28 C29 H29 120.8 . . ?
N5 C30 C24 128.0(3) . . ?
N5 C30 H30 116.0 . . ?
C24 C30 H30 116.0 . . ?
O4 C25 H25A 109.5 . . ?
O4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N8 C31 S2 177.2(4) . . ?

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
Ni1 O3 C1 C2 123.0(3) . . . . ?
Ni2 O3 C1 C2 -124.9(3) . . . . ?
Ni1 O3 C1 C6 -56.0(3) . . . . ?
Ni2 O3 C1 C6 56.2(3) . . . . ?
O3 C1 C6 C5 177.4(3) . . . . ?
C2 C1 C6 C5 -1.6(4) . . . . ?
O3 C1 C6 C7 -1.2(4) . . . . ?
C2 C1 C6 C7 179.9(3) . . . . ?
C1 C6 C5 C4 0.9(5) . . . . ?
C7 C6 C5 C4 179.4(3) . . . . ?
C5 C6 C7 N4 125.8(3) . . . . ?
C1 C6 C7 N4 -55.7(4) . . . . ?
C5 C6 C7 N3 -117.9(3) . . . . ?
C1 C6 C7 N3 60.7(4) . . . . ?
O3 C1 C2 C3 -177.6(3) . . . . ?
C6 C1 C2 C3 1.3(5) . . . . ?
C6 C5 C4 C3 0.2(6) . . . . ?
C5 C4 C3 C2 -0.4(6) . . . . ?
C1 C2 C3 C4 -0.3(6) . . . . ?
N3 C7 N4 C17 44.9(2) . . . . ?
C6 C7 N4 C17 168.2(2) . . . . ?
N3 C7 N4 C21 165.2(2) . . . . ?
C6 C7 N4 C21 -71.6(3) . . . . ?
N3 C7 N4 Ni2 -76.2(2) . . . . ?
C6 C7 N4 Ni2 47.1(3) . . . . ?
Ni1 O2 C32 C9 -171.24(19) . . . . ?
Ni2 O2 C32 C9 17.1(4) . . . . ?
Ni1 O2 C32 C13 8.5(4) . . . . ?
Ni2 O2 C32 C13 -163.17(19) . . . . ?
C12 C13 C32 O2 177.7(2) . . . . ?
C14 C13 C32 O2 -3.1(4) . . . . ?
C12 C13 C32 C9 -2.5(4) . . . . ?
C14 C13 C32 C9 176.7(3) . . . . ?
C12 C13 C14 N1 -178.1(3) . . . . ?
C32 C13 C14 N1 2.6(4) . . . . ?
O2 C32 C9 C10 -176.6(3) . . . . ?
C13 C32 C9 C10 3.6(4) . . . . ?
C10 C11 C12 C13 2.5(5) . . . . ?
C32 C13 C12 C11 -0.5(4) . . . . ?
C14 C13 C12 C11 -179.8(3) . . . . ?
C32 C9 C10 C11 -1.7(5) . . . . ?
C12 C11 C10 C9 -1.4(5) . . . . ?
C13 C14 N1 C15 -178.9(3) . . . . ?
C13 C14 N1 Ni1 -7.5(4) . . . . ?
C14 N1 C15 C16 147.9(3) . . . . ?
Ni1 N1 C15 C16 -24.5(3) . . . . ?
N2 C16 C15 N1 45.0(4) . . . . ?
C7 N4 C17 C18 -25.5(3) . . . . ?
C21 N4 C17 C18 -146.5(3) . . . . ?
Ni2 N4 C17 C18 99.2(2) . . . . ?
N4 C17 C18 N3 -3.4(3) . . . . ?
C17 C18 N3 C7 30.9(3) . . . . ?
C17 C18 N3 C19 151.0(3) . . . . ?
C17 C18 N3 Ni1 -91.0(2) . . . . ?
N4 C7 N3 C18 -47.2(2) . . . . ?
C6 C7 N3 C18 -171.4(2) . . . . ?
N4 C7 N3 C19 -165.9(2) . . . . ?
C6 C7 N3 C19 69.8(3) . . . . ?
N4 C7 N3 Ni1 74.5(2) . . . . ?
C6 C7 N3 Ni1 -49.8(3) . . . . ?
C18 N3 C19 C20 159.9(3) . . . . ?
C7 N3 C19 C20 -86.4(3) . . . . ?
Ni1 N3 C19 C20 37.6(3) . . . . ?
N3 C19 C20 N2 -45.8(4) . . . . ?
C19 C20 N2 C16 -90.6(3) . . . . ?
C19 C20 N2 Ni1 28.3(3) . . . . ?
C15 C16 N2 C20 78.2(3) . . . . ?
C15 C16 N2 Ni1 -42.8(3) . . . . ?
C7 N4 C21 C22 81.1(3) . . . . ?
C17 N4 C21 C22 -163.8(3) . . . . ?
Ni2 N4 C21 C22 -44.9(3) . . . . ?
C30 N5 C22 C21 159.1(3) . . . . ?
Ni2 N5 C22 C21 -18.7(3) . . . . ?
N4 C21 C22 N5 44.0(4) . . . . ?
Ni2 O1 C23 C27 172.7(3) . . . . ?
Ni2 O1 C23 C24 -9.6(5) . . . . ?
C26 C24 C23 O1 -174.5(4) . . . . ?
C30 C24 C23 O1 6.3(6) . . . . ?
C26 C24 C23 C27 3.3(6) . . . . ?
C30 C24 C23 C27 -176.0(4) . . . . ?
C23 C24 C26 C29 -2.3(6) . . . . ?
C30 C24 C26 C29 177.0(4) . . . . ?
O1 C23 C27 C28 176.2(4) . . . . ?
C24 C23 C27 C28 -1.5(6) . . . . ?
C23 C27 C28 C29 -1.4(6) . . . . ?
C24 C26 C29 C28 -0.5(7) . . . . ?
C27 C28 C29 C26 2.4(7) . . . . ?
C22 N5 C30 C24 176.9(4) . . . . ?
Ni2 N5 C30 C24 -5.6(6) . . . . ?
C23 C24 C30 N5 1.5(7) . . . . ?
C26 C24 C30 N5 -177.7(4) . . . . ?

_refine_diff_density_max         0.662
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.065

####################################################################### 
# 
# 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_SKC-23G-A
_database_code_depnum_ccdc_archive 'CCDC 1571833'
_audit_update_record             
;
2017-08-31 deposited with the CCDC.
2018-03-07 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            'C30 H35 N9 Ni2 O12 S'
_chemical_formula_weight         863.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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                   11.5055(2)
_cell_length_b                   13.2976(2)
_cell_length_c                   13.8302(4)
_cell_angle_alpha                88.1120(10)
_cell_angle_beta                 71.8510(10)
_cell_angle_gamma                64.9750(10)
_cell_volume                     1809.89(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4317
_cell_measurement_theta_min      1.560
_cell_measurement_theta_max      24.998

_exptl_crystal_description       blocks
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_F_000             892
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    1.172
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_process_details   'face indexing'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17756
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.560
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.962
_reflns_number_total             6129
_reflns_number_gt                4317
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0439P)²+0.1067P] 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         6129
_refine_ls_number_parameters     512
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0904
_refine_ls_wR_factor_gt          0.0798
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_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
Ni1 Ni 0.10666(4) 0.21818(3) 0.20442(3) 0.03496(13) Uani 1 1 d . . . . .
Ni2 Ni 0.36132(4) 0.24644(3) 0.21544(3) 0.03517(13) Uani 1 1 d . . . . .
S1 S 0.76431(9) 0.20971(8) -0.04793(7) 0.0509(3) Uani 1 1 d . . . . .
C7 C 0.4086(3) 0.3380(3) 0.3856(2) 0.0396(8) Uani 1 1 d . . . . .
H7 H 0.4291 0.3289 0.4462 0.048 Uiso 1 1 calc R U . . .
C14 C -0.1283(3) 0.1789(3) 0.2205(3) 0.0539(10) Uani 1 1 d . . . . .
H14A H -0.1876 0.2512 0.2067 0.065 Uiso 1 1 calc R U . . .
H14B H -0.1834 0.1405 0.2521 0.065 Uiso 1 1 calc R U . . .
C24 C 0.2016(3) 0.1474(2) 0.4128(2) 0.0328(7) Uani 1 1 d . . . . .
C25 C 0.1814(3) 0.1172(3) 0.5110(2) 0.0378(8) Uani 1 1 d . . . . .
H25 H 0.2262 0.0432 0.5216 0.045 Uiso 1 1 calc R U . . .
C2 C 0.3579(3) 0.5328(3) 0.4159(3) 0.0424(8) Uani 1 1 d . . . . .
H2 H 0.3741 0.5166 0.4777 0.051 Uiso 1 1 calc R U . . .
C28 C 0.0441(3) 0.3391(3) 0.4829(2) 0.0410(8) Uani 1 1 d . . . . .
H28 H -0.0033 0.4132 0.4737 0.049 Uiso 1 1 calc R U . . .
C17 C 0.2123(3) 0.2259(2) -0.0437(2) 0.0352(8) Uani 1 1 d . . . . .
C27 C 0.0245(3) 0.3082(3) 0.5798(3) 0.0438(8) Uani 1 1 d . . . . .
H27 H -0.0350 0.3610 0.6361 0.053 Uiso 1 1 calc R U . . .
C18 C 0.2806(3) 0.2548(2) 0.0127(2) 0.0353(8) Uani 1 1 d . . . . .
C23 C 0.6398(3) 0.2015(3) 0.0450(3) 0.0380(8) Uani 1 1 d . . . . .
C1 C 0.3619(3) 0.4500(3) 0.3541(2) 0.0372(8) Uani 1 1 d . . . . .
C6 C 0.3305(3) 0.4760(3) 0.2604(2) 0.0362(8) Uani 1 1 d . . . . .
C22 C 0.2291(3) 0.2513(3) -0.1450(3) 0.0471(9) Uani 1 1 d . . . . .
H22 H 0.1874 0.2302 -0.1829 0.057 Uiso 1 1 calc R U . . .
C26 C 0.0943(3) 0.1974(3) 0.5934(2) 0.0403(8) Uani 1 1 d . . . . .
C19 C 0.3585(3) 0.3118(3) -0.0361(2) 0.0396(8) Uani 1 1 d . . . . .
H19 H 0.4032 0.3322 -0.0005 0.047 Uiso 1 1 calc R U . . .
C16 C 0.1207(3) 0.1731(3) -0.0050(3) 0.0415(8) Uani 1 1 d . . . . .
H16 H 0.0904 0.1507 -0.0515 0.050 Uiso 1 1 calc R U . . .
C20 C 0.3704(3) 0.3380(3) -0.1345(3) 0.0456(9) Uani 1 1 d . . . . .
H20 H 0.4212 0.3766 -0.1644 0.055 Uiso 1 1 calc R U . . .
C9 C 0.5189(3) 0.0506(3) 0.2942(3) 0.0426(9) Uani 1 1 d . . . . .
H9A H 0.6011 0.0405 0.2393 0.051 Uiso 1 1 calc R U . . .
H9B H 0.5361 -0.0191 0.3243 0.051 Uiso 1 1 calc R U . . .
C3 C 0.3301(3) 0.6386(3) 0.3865(3) 0.0424(8) Uani 1 1 d . . . . .
C12 C 0.1171(3) 0.0106(3) 0.2976(3) 0.0460(9) Uani 1 1 d . . . . .
H12A H 0.1486 -0.0419 0.3444 0.055 Uiso 1 1 calc R U . . .
H12B H 0.1098 -0.0293 0.2440 0.055 Uiso 1 1 calc R U . . .
C8 C 0.4851(3) 0.1423(2) 0.3753(3) 0.0422(8) Uani 1 1 d . . . . .
H8A H 0.4217 0.1382 0.4389 0.051 Uiso 1 1 calc R U . . .
H8B H 0.5668 0.1340 0.3880 0.051 Uiso 1 1 calc R U . . .
C21 C 0.3059(3) 0.3065(3) -0.1892(3) 0.0474(9) Uani 1 1 d . . . . .
C5 C 0.3090(3) 0.5849(3) 0.2324(3) 0.0430(9) Uani 1 1 d . . . . .
H5 H 0.2946 0.6027 0.1703 0.052 Uiso 1 1 calc R U . . .
C4 C 0.3087(3) 0.6637(3) 0.2925(3) 0.0466(9) Uani 1 1 d . . . . .
H4 H 0.2944 0.7339 0.2714 0.056 Uiso 1 1 calc R U . . .
C13 C -0.0224(3) 0.1033(3) 0.3552(3) 0.0483(9) Uani 1 1 d . . . . .
H13A H -0.0889 0.0732 0.3735 0.058 Uiso 1 1 calc R U . . .
H13B H -0.0203 0.1319 0.4180 0.058 Uiso 1 1 calc R U . . .
C10 C 0.4533(3) -0.0023(3) 0.1590(3) 0.0452(9) Uani 1 1 d . . . . .
H10A H 0.5288 -0.0718 0.1608 0.054 Uiso 1 1 calc R U . . .
H10B H 0.4821 0.0295 0.0971 0.054 Uiso 1 1 calc R U . . .
C11 C 0.3326(3) -0.0225(3) 0.1621(3) 0.0442(9) Uani 1 1 d . . . . .
H11A H 0.3119 -0.0063 0.0989 0.053 Uiso 1 1 calc R U . . .
H11B H 0.3499 -0.0993 0.1724 0.053 Uiso 1 1 calc R U . . .
C15 C -0.0229(3) 0.1115(3) 0.1204(3) 0.0505(9) Uani 1 1 d . . . . .
H15A H 0.0196 0.0332 0.1300 0.061 Uiso 1 1 calc R U . . .
H15B H -0.0655 0.1182 0.0685 0.061 Uiso 1 1 calc R U . . .
N1 N 0.4237(2) 0.2511(2) 0.3364(2) 0.0367(6) Uani 1 1 d . . . . .
N5 N 0.0794(2) 0.1556(2) 0.0882(2) 0.0387(7) Uani 1 1 d . . . . .
N4 N -0.0626(3) 0.1948(3) 0.2920(2) 0.0447(8) Uani 1 1 d . . . . .
N7 N 0.0788(3) 0.1657(3) 0.6960(2) 0.0464(7) Uani 1 1 d . . . . .
N6 N 0.5511(3) 0.1954(2) 0.1094(2) 0.0496(8) Uani 1 1 d . . . . .
N8 N 0.3292(3) 0.7216(2) 0.4511(3) 0.0526(8) Uani 1 1 d . . . . .
N9 N 0.3193(3) 0.3315(3) -0.2942(3) 0.0719(11) Uani 1 1 d . . . . .
O1 O 0.27169(19) 0.23151(16) 0.10678(15) 0.0372(5) Uani 1 1 d . . . . .
O2 O 0.3196(2) 0.40847(17) 0.20281(17) 0.0425(6) Uani 1 1 d . . . . .
O7 O -0.0021(2) 0.2366(2) 0.76945(18) 0.0596(7) Uani 1 1 d . . . . .
O6 O 0.3381(2) 0.7012(2) 0.5369(2) 0.0599(7) Uani 1 1 d . . . . .
O8 O 0.1486(3) 0.0691(2) 0.70772(19) 0.0674(8) Uani 1 1 d . . . . .
O5 O 0.3191(3) 0.8116(2) 0.4193(2) 0.0810(9) Uani 1 1 d . . . . .
O9 O 0.3745(3) 0.3917(3) -0.3292(2) 0.0830(10) Uani 1 1 d . . . . .
O10 O 0.2751(4) 0.2910(4) -0.3439(2) 0.1325(16) Uani 1 1 d . . . . .
N3 N 0.2186(2) 0.05590(19) 0.25081(19) 0.0347(6) Uani 1 1 d . . . . .
O3 O 0.15573(19) 0.29181(15) 0.30410(15) 0.0353(5) Uani 1 1 d . . . . .
N2 N 0.4072(2) 0.07722(19) 0.25140(19) 0.0339(6) Uani 1 1 d . . . . .
C30 C 0.2909(3) 0.0605(2) 0.3215(2) 0.0348(8) Uani 1 1 d . . . . .
H30 H 0.3263 -0.0127 0.3461 0.042 Uiso 1 1 calc R U . . .
O4 O -0.0293(2) 0.3795(2) 0.1895(2) 0.0496(7) Uani 1 1 d . . . . .
H4B H -0.0623 0.3757 0.1458 0.074 Uiso 1 1 calc R U . . .
C29 C 0.1342(3) 0.2610(2) 0.3973(2) 0.0337(7) Uani 1 1 d . . . . .
O11 O 0.0924(4) 0.5231(3) 0.1477(3) 0.0665(9) Uani 1 1 d . . . . .
O12 O 0.8356(4) 0.3984(3) 0.0504(3) 0.0809(10) Uani 1 1 d . . . . .
H4A H -0.003(3) 0.427(3) 0.189(3) 0.058(13) Uiso 1 1 d . . . . .
H12D H 0.858(4) 0.432(3) 0.001(3) 0.070(15) Uiso 1 1 d . . . . .
H12C H 0.811(6) 0.352(5) 0.037(5) 0.14(3) Uiso 1 1 d . . . . .
H11C H 0.158(4) 0.491(3) 0.162(3) 0.074(16) Uiso 1 1 d . . . . .
H11D H 0.054(6) 0.583(5) 0.179(5) 0.16(3) Uiso 1 1 d . . . . .
H4N H -0.115(3) 0.251(2) 0.332(2) 0.036(10) 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
Ni1 N5 2.000(3) . ?
Ni1 O1 2.033(2) . ?
Ni1 O3 2.054(2) . ?
Ni1 N4 2.092(3) . ?
Ni1 O4 2.104(2) . ?
Ni1 N3 2.191(2) . ?
Ni2 O2 2.014(2) . ?
Ni2 N1 2.028(3) . ?
Ni2 N6 2.048(3) . ?
Ni2 O3 2.1206(19) . ?
Ni2 O1 2.126(2) . ?
Ni2 N2 2.162(2) . ?
S1 C23 1.641(3) . ?
C7 N1 1.278(4) . ?
C7 C1 1.458(4) . ?
C7 H7 0.9300 . ?
C14 N4 1.487(4) . ?
C14 C15 1.518(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C24 C25 1.381(4) . ?
C24 C29 1.422(4) . ?
C24 C30 1.506(4) . ?
C25 C26 1.380(4) . ?
C25 H25 0.9300 . ?
C2 C3 1.383(4) . ?
C2 C1 1.392(4) . ?
C2 H2 0.9300 . ?
C28 C27 1.367(4) . ?
C28 C29 1.400(4) . ?
C28 H28 0.9300 . ?
C17 C22 1.404(4) . ?
C17 C18 1.425(4) . ?
C17 C16 1.463(4) . ?
C27 C26 1.388(4) . ?
C27 H27 0.9300 . ?
C18 O1 1.311(3) . ?
C18 C19 1.413(4) . ?
C23 N6 1.158(4) . ?
C1 C6 1.444(4) . ?
C6 O2 1.289(4) . ?
C6 C5 1.424(4) . ?
C22 C21 1.369(5) . ?
C22 H22 0.9300 . ?
C26 N7 1.445(4) . ?
C19 C20 1.373(4) . ?
C19 H19 0.9300 . ?
C16 N5 1.278(4) . ?
C16 H16 0.9300 . ?
C20 C21 1.389(5) . ?
C20 H20 0.9300 . ?
C9 N2 1.484(4) . ?
C9 C8 1.521(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C3 C4 1.401(5) . ?
C3 N8 1.437(4) . ?
C12 N3 1.497(4) . ?
C12 C13 1.525(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C8 N1 1.484(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C21 N9 1.454(4) . ?
C5 C4 1.357(4) . ?
C5 H5 0.9300 . ?
C4 H4 0.9300 . ?
C13 N4 1.471(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C10 N2 1.492(4) . ?
C10 C11 1.510(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N3 1.495(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C15 N5 1.473(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
N4 H4N 0.81(3) . ?
N7 O8 1.232(3) . ?
N7 O7 1.232(3) . ?
N8 O5 1.232(4) . ?
N8 O6 1.234(4) . ?
N9 O9 1.222(4) . ?
N9 O10 1.223(4) . ?
N3 C30 1.485(4) . ?
O3 C29 1.320(3) . ?
N2 C30 1.486(4) . ?
C30 H30 0.9800 . ?
O4 H4B 0.8200 . ?
O4 H4A 0.81(3) . ?
O11 H11C 0.78(4) . ?
O11 H11D 0.79(6) . ?
O12 H12D 0.83(4) . ?
O12 H12C 0.82(6) . ?

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
N5 Ni1 O1 90.77(9) . . ?
N5 Ni1 O3 169.90(9) . . ?
O1 Ni1 O3 79.58(8) . . ?
N5 Ni1 N4 83.30(12) . . ?
O1 Ni1 N4 173.98(11) . . ?
O3 Ni1 N4 106.39(11) . . ?
N5 Ni1 O4 90.03(10) . . ?
O1 Ni1 O4 93.56(9) . . ?
O3 Ni1 O4 87.61(9) . . ?
N4 Ni1 O4 87.52(11) . . ?
N5 Ni1 N3 95.46(10) . . ?
O1 Ni1 N3 96.49(8) . . ?
O3 Ni1 N3 88.66(9) . . ?
N4 Ni1 N3 83.08(10) . . ?
O4 Ni1 N3 168.47(10) . . ?
O2 Ni2 N1 90.43(10) . . ?
O2 Ni2 N6 91.73(10) . . ?
N1 Ni2 N6 94.23(11) . . ?
O2 Ni2 O3 90.39(8) . . ?
N1 Ni2 O3 95.49(9) . . ?
N6 Ni2 O3 170.04(10) . . ?
O2 Ni2 O1 95.29(8) . . ?
N1 Ni2 O1 169.76(9) . . ?
N6 Ni2 O1 94.07(10) . . ?
O3 Ni2 O1 76.04(8) . . ?
O2 Ni2 N2 171.42(10) . . ?
N1 Ni2 N2 81.28(10) . . ?
N6 Ni2 N2 91.09(10) . . ?
O3 Ni2 N2 88.21(8) . . ?
O1 Ni2 N2 92.59(9) . . ?
N1 C7 C1 125.2(3) . . ?
N1 C7 H7 117.4 . . ?
C1 C7 H7 117.4 . . ?
N4 C14 C15 111.1(3) . . ?
N4 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
N4 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C25 C24 C29 119.8(3) . . ?
C25 C24 C30 120.7(3) . . ?
C29 C24 C30 119.5(3) . . ?
C26 C25 C24 119.8(3) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C3 C2 C1 120.8(3) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C27 C28 C29 121.1(3) . . ?
C27 C28 H28 119.4 . . ?
C29 C28 H28 119.4 . . ?
C22 C17 C18 119.0(3) . . ?
C22 C17 C16 115.0(3) . . ?
C18 C17 C16 125.9(3) . . ?
C28 C27 C26 119.4(3) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
O1 C18 C19 120.2(3) . . ?
O1 C18 C17 122.3(3) . . ?
C19 C18 C17 117.5(3) . . ?
N6 C23 S1 178.9(3) . . ?
C2 C1 C6 119.9(3) . . ?
C2 C1 C7 116.4(3) . . ?
C6 C1 C7 123.6(3) . . ?
O2 C6 C5 119.1(3) . . ?
O2 C6 C1 124.6(3) . . ?
C5 C6 C1 116.3(3) . . ?
C21 C22 C17 121.3(3) . . ?
C21 C22 H22 119.4 . . ?
C17 C22 H22 119.4 . . ?
C25 C26 C27 121.3(3) . . ?
C25 C26 N7 119.2(3) . . ?
C27 C26 N7 119.4(3) . . ?
C20 C19 C18 122.1(3) . . ?
C20 C19 H19 119.0 . . ?
C18 C19 H19 119.0 . . ?
N5 C16 C17 124.6(3) . . ?
N5 C16 H16 117.7 . . ?
C17 C16 H16 117.7 . . ?
C19 C20 C21 119.5(3) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
N2 C9 C8 111.9(2) . . ?
N2 C9 H9A 109.2 . . ?
C8 C9 H9A 109.2 . . ?
N2 C9 H9B 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C2 C3 C4 120.4(3) . . ?
C2 C3 N8 119.4(3) . . ?
C4 C3 N8 120.1(3) . . ?
N3 C12 C13 111.7(3) . . ?
N3 C12 H12A 109.3 . . ?
C13 C12 H12A 109.3 . . ?
N3 C12 H12B 109.3 . . ?
C13 C12 H12B 109.3 . . ?
H12A C12 H12B 107.9 . . ?
N1 C8 C9 107.7(3) . . ?
N1 C8 H8A 110.2 . . ?
C9 C8 H8A 110.2 . . ?
N1 C8 H8B 110.2 . . ?
C9 C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
C22 C21 C20 120.5(3) . . ?
C22 C21 N9 119.1(3) . . ?
C20 C21 N9 120.4(3) . . ?
C4 C5 C6 122.9(3) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
C5 C4 C3 119.5(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
N4 C13 C12 110.8(3) . . ?
N4 C13 H13A 109.5 . . ?
C12 C13 H13A 109.5 . . ?
N4 C13 H13B 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
N2 C10 C11 106.0(2) . . ?
N2 C10 H10A 110.5 . . ?
C11 C10 H10A 110.5 . . ?
N2 C10 H10B 110.5 . . ?
C11 C10 H10B 110.5 . . ?
H10A C10 H10B 108.7 . . ?
N3 C11 C10 104.8(3) . . ?
N3 C11 H11A 110.8 . . ?
C10 C11 H11A 110.8 . . ?
N3 C11 H11B 110.8 . . ?
C10 C11 H11B 110.8 . . ?
H11A C11 H11B 108.9 . . ?
N5 C15 C14 107.8(3) . . ?
N5 C15 H15A 110.1 . . ?
C14 C15 H15A 110.1 . . ?
N5 C15 H15B 110.1 . . ?
C14 C15 H15B 110.1 . . ?
H15A C15 H15B 108.5 . . ?
C7 N1 C8 117.2(3) . . ?
C7 N1 Ni2 126.9(2) . . ?
C8 N1 Ni2 115.7(2) . . ?
C16 N5 C15 119.9(3) . . ?
C16 N5 Ni1 124.4(2) . . ?
C15 N5 Ni1 114.0(2) . . ?
C13 N4 C14 115.0(3) . . ?
C13 N4 Ni1 110.2(2) . . ?
C14 N4 Ni1 107.4(2) . . ?
C13 N4 H4N 106(2) . . ?
C14 N4 H4N 109(2) . . ?
Ni1 N4 H4N 108(2) . . ?
O8 N7 O7 121.7(3) . . ?
O8 N7 C26 119.1(3) . . ?
O7 N7 C26 119.2(3) . . ?
C23 N6 Ni2 158.5(3) . . ?
O5 N8 O6 121.7(3) . . ?
O5 N8 C3 119.0(3) . . ?
O6 N8 C3 119.4(3) . . ?
O9 N9 O10 122.7(3) . . ?
O9 N9 C21 118.8(4) . . ?
O10 N9 C21 118.6(4) . . ?
C18 O1 Ni1 122.44(19) . . ?
C18 O1 Ni2 136.1(2) . . ?
Ni1 O1 Ni2 98.73(9) . . ?
C6 O2 Ni2 127.85(19) . . ?
C30 N3 C11 101.9(2) . . ?
C30 N3 C12 111.8(2) . . ?
C11 N3 C12 111.1(2) . . ?
C30 N3 Ni1 114.12(17) . . ?
C11 N3 Ni1 111.88(18) . . ?
C12 N3 Ni1 106.20(17) . . ?
C29 O3 Ni1 115.77(18) . . ?
C29 O3 Ni2 116.08(17) . . ?
Ni1 O3 Ni2 98.22(8) . . ?
C9 N2 C30 113.0(2) . . ?
C9 N2 C10 110.5(2) . . ?
C30 N2 C10 102.9(2) . . ?
C9 N2 Ni2 102.88(17) . . ?
C30 N2 Ni2 115.33(16) . . ?
C10 N2 Ni2 112.48(19) . . ?
N3 C30 N2 101.9(2) . . ?
N3 C30 C24 113.3(2) . . ?
N2 C30 C24 115.9(2) . . ?
N3 C30 H30 108.5 . . ?
N2 C30 H30 108.5 . . ?
C24 C30 H30 108.5 . . ?
Ni1 O4 H4B 109.5 . . ?
Ni1 O4 H4A 115(3) . . ?
H4B O4 H4A 119.3 . . ?
O3 C29 C28 120.9(3) . . ?
O3 C29 C24 120.6(3) . . ?
C28 C29 C24 118.5(3) . . ?
H11C O11 H11D 107(5) . . ?
H12D O12 H12C 114(5) . . ?

_refine_diff_density_max         0.235
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.055

####################################################################### 
# 
# 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_SKC-25G_0m
_database_code_depnum_ccdc_archive 'CCDC 1571837'
_audit_update_record             
;
2017-08-31 deposited with the CCDC.
2018-03-07 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            'C64 H76 Cl2 Cu N16 Ni4 O20'
_chemical_formula_weight         1758.68

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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                   15.3234(4)
_cell_length_b                   15.4364(4)
_cell_length_c                   15.7415(3)
_cell_angle_alpha                83.393(2)
_cell_angle_beta                 78.868(2)
_cell_angle_gamma                85.688(2)
_cell_volume                     3623.78(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6041
_cell_measurement_theta_min      1.325
_cell_measurement_theta_max      24.99

_exptl_crystal_description       blocks
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_F_000             1814
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.466
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26494
_diffrn_reflns_av_unetI/netI     0.1033
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.325
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             12389
_reflns_number_gt                6041
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] 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         12389
_refine_ls_number_parameters     972
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.0680
_refine_ls_wR_factor_ref         0.2103
_refine_ls_wR_factor_gt          0.1664
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.004
_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
Ni2 Ni 0.71694(6) 0.43761(7) 0.46552(6) 0.0447(3) Uani 1 1 d . . . . .
Ni1 Ni 0.59601(7) 0.37997(7) 0.63615(6) 0.0463(3) Uani 1 1 d . . . . .
Cu2 Cu 0.0000 1.0000 0.0000 0.0569(4) Uani 1 2 d S . P . .
Cu1 Cu 0.5000 0.5000 0.5000 0.0508(4) Uani 1 2 d S . P . .
Ni4 Ni -0.10559(7) 0.82734(7) 0.00863(7) 0.0552(3) Uani 1 1 d . . . . .
Ni3 Ni 0.08842(7) 0.79951(7) 0.01798(8) 0.0596(3) Uani 1 1 d . . . . .
C17 C 0.7002(5) 0.5636(6) 0.6330(5) 0.049(2) Uani 1 1 d . . . . .
C21 C 0.4794(6) 0.3421(6) 0.7998(6) 0.063(2) Uani 1 1 d . . . . .
H21A H 0.4242 0.3409 0.7785 0.075 Uiso 1 1 calc R U . . .
H21B H 0.4644 0.3490 0.8615 0.075 Uiso 1 1 calc R U . . .
C3 C 0.6441(5) 0.4525(6) 0.1494(6) 0.056(2) Uani 1 1 d . . . . .
H3 H 0.6155 0.4294 0.1107 0.067 Uiso 1 1 calc R U . . .
C12 C 0.6215(5) 0.5698(5) 0.5980(5) 0.0448(19) Uani 1 1 d . . . . .
C1 C 0.6660(5) 0.4574(5) 0.2981(5) 0.048(2) Uani 1 1 d . . . . .
C4 C 0.7040(6) 0.5159(6) 0.1187(5) 0.058(2) Uani 1 1 d . . . . .
C7 C 0.7790(5) 0.5593(6) 0.3184(6) 0.054(2) Uani 1 1 d . . . . .
H7 H 0.8159 0.6037 0.2916 0.065 Uiso 1 1 calc R U . . .
C8 C 0.8318(6) 0.5794(6) 0.4472(5) 0.059(2) Uani 1 1 d . . . . .
H8A H 0.7954 0.6213 0.4822 0.070 Uiso 1 1 calc R U . . .
H8B H 0.8786 0.6099 0.4070 0.070 Uiso 1 1 calc R U . . .
C2 C 0.6257(5) 0.4225(5) 0.2366(5) 0.050(2) Uani 1 1 d . . . . .
H2 H 0.5861 0.3785 0.2554 0.060 Uiso 1 1 calc R U . . .
C5 C 0.7454(6) 0.5506(6) 0.1756(6) 0.056(2) Uani 1 1 d . . . . .
H5 H 0.7856 0.5938 0.1549 0.067 Uiso 1 1 calc R U . . .
C13 C 0.5667(5) 0.6457(6) 0.6040(5) 0.052(2) Uani 1 1 d . . . . .
H13 H 0.5133 0.6484 0.5837 0.063 Uiso 1 1 calc R U . . .
C16 C 0.7202(6) 0.6365(6) 0.6699(6) 0.062(2) Uani 1 1 d . . . . .
H16 H 0.7711 0.6335 0.6942 0.075 Uiso 1 1 calc R U . . .
C9 C 0.8711(6) 0.5087(6) 0.5041(6) 0.065(3) Uani 1 1 d . . . . .
H9A H 0.9163 0.4743 0.4684 0.078 Uiso 1 1 calc R U . . .
H9B H 0.8994 0.5347 0.5443 0.078 Uiso 1 1 calc R U . . .
C22 C 0.5328(6) 0.2566(6) 0.7869(5) 0.065(3) Uani 1 1 d . . . . .
H22A H 0.5782 0.2491 0.8228 0.078 Uiso 1 1 calc R U . . .
H22B H 0.4942 0.2081 0.8028 0.078 Uiso 1 1 calc R U . . .
C23 C 0.5747(6) 0.1930(7) 0.6547(6) 0.076(3) Uani 1 1 d . . . . .
H23 H 0.5502 0.1434 0.6869 0.091 Uiso 1 1 calc R U . . .
C29 C 0.6568(6) 0.2536(6) 0.5039(6) 0.058(2) Uani 1 1 d . . . . .
C15 C 0.6672(6) 0.7116(7) 0.6713(6) 0.066(3) Uani 1 1 d . . . . .
C14 C 0.5888(6) 0.7165(6) 0.6389(6) 0.063(2) Uani 1 1 d . . . . .
H14 H 0.5518 0.7671 0.6409 0.076 Uiso 1 1 calc R U . . .
C6 C 0.7277(5) 0.5215(5) 0.2652(5) 0.049(2) Uani 1 1 d . . . . .
C28 C 0.6875(7) 0.2363(7) 0.4193(7) 0.079(3) Uani 1 1 d . . . . .
H28 H 0.7180 0.2788 0.3805 0.095 Uiso 1 1 calc R U . . .
C24 C 0.6114(7) 0.1877(7) 0.5605(7) 0.076(3) Uani 1 1 d . . . . .
C27 C 0.6749(8) 0.1578(9) 0.3896(8) 0.108(4) Uani 1 1 d . . . . .
H27 H 0.6989 0.1479 0.3324 0.130 Uiso 1 1 calc R U . . .
C25 C 0.5972(9) 0.1094(8) 0.5298(8) 0.109(4) Uani 1 1 d . . . . .
H25 H 0.5670 0.0666 0.5683 0.130 Uiso 1 1 calc R U . . .
C31 C 0.6850(8) 0.5180(8) -0.0289(6) 0.095(4) Uani 1 1 d . . . . .
H31A H 0.7006 0.4568 -0.0311 0.143 Uiso 1 1 calc R U . . .
H31B H 0.7044 0.5487 -0.0852 0.143 Uiso 1 1 calc R U . . .
H31C H 0.6216 0.5267 -0.0123 0.143 Uiso 1 1 calc R U . . .
C26 C 0.6268(10) 0.0939(9) 0.4445(9) 0.126(5) Uani 1 1 d . . . . .
O5 O 0.7265(5) 0.5498(5) 0.0322(4) 0.087(2) Uani 1 1 d . . . . .
C39 C -0.2184(6) 0.7845(6) 0.1766(8) 0.073(3) Uani 1 1 d . . . . .
H39 H -0.2748 0.7809 0.2112 0.088 Uiso 1 1 calc R U . . .
C33 C -0.0517(6) 0.7800(5) 0.1796(6) 0.056(2) Uani 1 1 d . . . . .
C37 C -0.1681(7) 0.7982(6) 0.3112(7) 0.076(3) Uani 1 1 d . . . . .
H37 H -0.2277 0.8040 0.3375 0.091 Uiso 1 1 calc R U . . .
C38 C -0.1430(6) 0.7870(6) 0.2203(6) 0.067(3) Uani 1 1 d . . . . .
C35 C -0.0118(9) 0.7893(7) 0.3210(8) 0.084(3) Uani 1 1 d . . . . .
H35 H 0.0319 0.7891 0.3546 0.101 Uiso 1 1 calc R U . . .
C42 C -0.1838(7) 0.8057(8) -0.1420(7) 0.083(3) Uani 1 1 d . . . . .
H42A H -0.1419 0.8309 -0.1913 0.100 Uiso 1 1 calc R U . . .
H42B H -0.2397 0.8011 -0.1609 0.100 Uiso 1 1 calc R U . . .
C41 C -0.2879(6) 0.8610(7) -0.0123(7) 0.078(3) Uani 1 1 d . . . . .
H41A H -0.3006 0.9158 0.0135 0.094 Uiso 1 1 calc R U . . .
H41B H -0.3330 0.8558 -0.0467 0.094 Uiso 1 1 calc R U . . .
C49 C 0.2644(8) 0.8877(8) 0.0573(8) 0.092(3) Uani 1 1 d . . . . .
C40 C -0.2941(6) 0.7895(7) 0.0570(7) 0.077(3) Uani 1 1 d . . . . .
H40A H -0.2989 0.7347 0.0340 0.093 Uiso 1 1 calc R U . . .
H40B H -0.3462 0.7991 0.1015 0.093 Uiso 1 1 calc R U . . .
C45 C 0.0391(7) 0.6215(6) -0.0104(7) 0.081(3) Uani 1 1 d . . . . .
H45A H 0.0520 0.6162 0.0480 0.097 Uiso 1 1 calc R U . . .
H45B H 0.0631 0.5695 -0.0378 0.097 Uiso 1 1 calc R U . . .
C47 C 0.2219(6) 0.7657(8) -0.1277(8) 0.084(3) Uani 1 1 d . . . . .
H47A H 0.2850 0.7521 -0.1468 0.101 Uiso 1 1 calc R U . . .
H47B H 0.2000 0.8030 -0.1738 0.101 Uiso 1 1 calc R U . . .
C36 C -0.1014(9) 0.8002(7) 0.3586(7) 0.081(3) Uani 1 1 d . . . . .
C44 C -0.0613(7) 0.6348(6) -0.0083(7) 0.080(3) Uani 1 1 d . . . . .
H44A H -0.0832 0.5864 -0.0307 0.096 Uiso 1 1 calc R U . . .
H44B H -0.0932 0.6397 0.0507 0.096 Uiso 1 1 calc R U . . .
C54 C 0.1740(9) 0.9076(8) 0.1105(8) 0.089(4) Uani 1 1 d . . . . .
C43 C -0.1486(7) 0.7165(7) -0.1126(8) 0.085(3) Uani 1 1 d . . . . .
H43A H -0.1289 0.6843 -0.1629 0.103 Uiso 1 1 calc R U . . .
H43B H -0.1964 0.6856 -0.0744 0.103 Uiso 1 1 calc R U . . .
C46 C 0.1712(7) 0.6812(7) -0.1066(8) 0.090(3) Uani 1 1 d . . . . .
H46A H 0.1712 0.6551 -0.1598 0.108 Uiso 1 1 calc R U . . .
H46B H 0.2003 0.6397 -0.0685 0.108 Uiso 1 1 calc R U . . .
C48 C 0.2727(8) 0.8444(8) -0.0220(7) 0.090(3) Uani 1 1 d . . . . .
H48 H 0.3290 0.8410 -0.0568 0.108 Uiso 1 1 calc R U . . .
C34 C 0.0116(7) 0.7787(6) 0.2337(7) 0.074(3) Uani 1 1 d . . . . .
H34 H 0.0716 0.7705 0.2096 0.089 Uiso 1 1 calc R U . . .
C61 C 0.0247(5) 0.8868(6) -0.1515(6) 0.055(2) Uani 1 1 d . . . . .
C56 C 0.0307(6) 0.8067(6) -0.1837(6) 0.061(2) Uani 1 1 d . . . . .
C58 C 0.0645(8) 0.8731(9) -0.3317(8) 0.091(3) Uani 1 1 d . . . . .
C60 C 0.0386(6) 0.9605(6) -0.2099(6) 0.065(2) Uani 1 1 d . . . . .
H60 H 0.0345 1.0150 -0.1894 0.078 Uiso 1 1 calc R U . . .
C57 C 0.0495(7) 0.8015(7) -0.2739(7) 0.077(3) Uani 1 1 d . . . . .
H57 H 0.0517 0.7471 -0.2945 0.093 Uiso 1 1 calc R U . . .
C59 C 0.0591(7) 0.9539(8) -0.3013(7) 0.085(3) Uani 1 1 d . . . . .
H59 H 0.0687 1.0039 -0.3402 0.102 Uiso 1 1 calc R U . . .
C55 C 0.0151(6) 0.7228(6) -0.1244(6) 0.066(3) Uani 1 1 d . . . . .
H55 H 0.0209 0.6748 -0.1611 0.079 Uiso 1 1 calc R U . . .
C63 C 0.1141(16) 0.9152(17) -0.4772(12) 0.234(12) Uani 1 1 d . . . . .
H63A H 0.0677 0.9582 -0.4877 0.351 Uiso 1 1 calc R U . . .
H63B H 0.1372 0.8879 -0.5293 0.351 Uiso 1 1 calc R U . . .
H63C H 0.1612 0.9430 -0.4602 0.351 Uiso 1 1 calc R U . . .
O10 O 0.0833(8) 0.8587(9) -0.4177(6) 0.160(5) Uani 1 1 d . . . . .
N1 N 0.7776(4) 0.5362(5) 0.3999(4) 0.0534(18) Uani 1 1 d . . . . .
O3 O 0.6432(3) 0.4299(4) 0.3819(3) 0.0562(15) Uani 1 1 d . . . . .
O2 O 0.6018(3) 0.4994(3) 0.5612(3) 0.0453(13) Uani 1 1 d . . . . .
O1 O 0.6731(3) 0.3279(4) 0.5324(3) 0.0539(14) Uani 1 1 d . . . . .
Cl1 Cl 0.03133(19) 0.4995(2) 0.2421(2) 0.0854(8) Uani 1 1 d . . . . .
O20 O 0.0147(6) 0.5591(6) 0.3041(6) 0.130(3) Uani 1 1 d . . . . .
O18 O 0.1135(6) 0.5095(11) 0.1876(6) 0.211(7) Uani 1 1 d . . . . .
O17 O -0.0348(5) 0.5013(7) 0.1916(6) 0.133(3) Uani 1 1 d . . . . .
N9 N 0.2076(5) 0.8093(6) -0.0496(7) 0.089(3) Uani 1 1 d . . . . .
O7 O 0.1004(5) 0.8940(5) 0.0868(5) 0.091(2) Uani 1 1 d . . . . .
N11 N -0.0727(5) 0.7189(5) -0.0656(5) 0.064(2) Uani 1 1 d . . . . .
N12 N -0.1979(5) 0.8637(5) -0.0717(5) 0.069(2) Uani 1 1 d . . . . .
H12 H -0.1886 0.9239 -0.0977 0.083 Uiso 1 1 calc R U . . .
N14 N -0.1136(5) 0.9470(5) 0.0609(5) 0.0606(19) Uani 1 1 d . . . . .
N15 N -0.1776(6) 0.9755(5) 0.1092(6) 0.069(2) Uani 1 1 d . . . . .
N16 N -0.2411(6) 1.0005(7) 0.1557(7) 0.106(3) Uani 1 1 d . . . . .
N6 N 0.4814(4) 0.3900(4) 0.5776(4) 0.0514(17) Uani 1 1 d . . . . .
N7 N 0.4235(5) 0.3378(5) 0.5947(4) 0.0538(18) Uani 1 1 d . . . . .
N8 N 0.3691(6) 0.2877(6) 0.6128(6) 0.082(3) Uani 1 1 d . . . . .
N2 N 0.8017(4) 0.4506(5) 0.5541(4) 0.0534(18) Uani 1 1 d . . . . .
O8 O -0.0280(4) 0.7741(4) 0.0944(4) 0.0611(15) Uani 1 1 d . . . . .
O9 O 0.0053(3) 0.8922(3) -0.0630(4) 0.0541(14) Uani 1 1 d . . . . .
N13 N -0.2127(5) 0.7869(5) 0.0936(5) 0.066(2) Uani 1 1 d . . . . .
N10 N 0.0775(5) 0.7023(5) -0.0631(5) 0.068(2) Uani 1 1 d . . . . .
N4 N 0.5292(5) 0.4173(5) 0.7537(5) 0.054(2) Uani 1 1 d . . . . .
C19 C 0.6824(6) 0.4089(7) 0.7808(5) 0.065(3) Uani 1 1 d . . . . .
H19A H 0.6830 0.3506 0.8112 0.078 Uiso 1 1 calc R U . . .
H19B H 0.7240 0.4422 0.8014 0.078 Uiso 1 1 calc R U . . .
C20 C 0.5909(6) 0.4514(6) 0.8011(5) 0.061(2) Uani 1 1 d . . . . .
H20A H 0.5684 0.4414 0.8632 0.073 Uiso 1 1 calc R U . . .
H20B H 0.5939 0.5140 0.7857 0.073 Uiso 1 1 calc R U . . .
N3 N 0.7120(4) 0.4034(5) 0.6847(4) 0.0518(17) Uani 1 1 d . . . . .
C11 C 0.7836(6) 0.3329(6) 0.6698(6) 0.064(2) Uani 1 1 d . . . . .
H11A H 0.7584 0.2779 0.6665 0.077 Uiso 1 1 calc R U . . .
H11B H 0.8173 0.3255 0.7166 0.077 Uiso 1 1 calc R U . . .
C18 C 0.7574(5) 0.4818(6) 0.6392(5) 0.054(2) Uani 1 1 d . . . . .
H18 H 0.8044 0.4924 0.6705 0.064 Uiso 1 1 calc R U . . .
C10 C 0.8426(6) 0.3625(6) 0.5843(5) 0.061(2) Uani 1 1 d . . . . .
H10A H 0.8436 0.3212 0.5421 0.073 Uiso 1 1 calc R U . . .
H10B H 0.9031 0.3680 0.5924 0.073 Uiso 1 1 calc R U . . .
N5 N 0.5744(5) 0.2600(5) 0.6942(4) 0.0556(18) Uani 1 1 d . . . . .
Cl2 Cl 0.4971(4) 0.7234(3) 0.9392(3) 0.1356(15) Uani 1 1 d . . . . .
O16 O 0.5109(8) 0.7864(8) 0.9898(8) 0.182(5) Uani 1 1 d . . . . .
O13 O 0.4606(7) 0.7534(10) 0.8688(7) 0.189(6) Uani 1 1 d . . . . .
O4 O 0.6099(10) 0.0136(8) 0.4238(8) 0.214(7) Uani 1 1 d . . . . .
O6 O 0.6967(5) 0.7796(5) 0.7058(5) 0.097(2) Uani 1 1 d . . . . .
O12 O -0.1177(7) 0.8121(7) 0.4449(6) 0.129(3) Uani 1 1 d . . . . .
C32 C 0.6355(11) 0.8540(9) 0.7156(11) 0.147(6) Uani 1 1 d . . . . .
H32A H 0.6321 0.8840 0.6593 0.221 Uiso 1 1 calc R U . . .
H32B H 0.6557 0.8927 0.7504 0.221 Uiso 1 1 calc R U . . .
H32C H 0.5777 0.8353 0.7435 0.221 Uiso 1 1 calc R U . . .
C50 C 0.3432(7) 0.9075(7) 0.0825(8) 0.082(3) Uani 1 1 d . . . . .
H50 H 0.3976 0.8976 0.0459 0.098 Uiso 1 1 calc R U . . .
C53 C 0.1820(8) 0.9371(7) 0.1854(10) 0.101(4) Uani 1 1 d . . . . .
H53 H 0.1287 0.9488 0.2230 0.121 Uiso 1 1 calc R U . . .
C51 C 0.3419(8) 0.9404(8) 0.1583(8) 0.086(3) Uani 1 1 d . . . . .
C52 C 0.2612(9) 0.9532(8) 0.2157(8) 0.098(4) Uani 1 1 d . . . . .
H52 H 0.2590 0.9711 0.2705 0.118 Uiso 1 1 calc R U . . .
O15 O 0.4335(17) 0.6813(14) 0.9952(9) 0.363(17) Uani 1 1 d . . . . .
O19 O 0.0361(12) 0.4195(8) 0.2892(9) 0.228(8) Uani 1 1 d . . . . .
C30 C 0.6337(15) -0.0063(16) 0.3422(15) 0.224(9) Uiso 1 1 d . . . . .
H30A H 0.6084 0.0374 0.3041 0.336 Uiso 1 1 calc R U . . .
H30B H 0.6125 -0.0622 0.3377 0.336 Uiso 1 1 calc R U . . .
H30C H 0.6975 -0.0083 0.3259 0.336 Uiso 1 1 calc R U . . .
O11 O 0.4155(6) 0.9633(6) 0.1874(6) 0.111(3) Uani 1 1 d . . . . .
C64 C 0.4954(8) 0.9840(10) 0.1237(9) 0.129(5) Uani 1 1 d . . . . .
H64A H 0.5134 0.9359 0.0895 0.193 Uiso 1 1 calc R U . . .
H64B H 0.5422 0.9944 0.1533 0.193 Uiso 1 1 calc R U . . .
H64C H 0.4831 1.0354 0.0864 0.193 Uiso 1 1 calc R U . . .
C62 C -0.2013(15) 0.8330(13) 0.4846(10) 0.198(9) Uani 1 1 d . . . . .
H62A H -0.2228 0.8862 0.4557 0.297 Uiso 1 1 calc R U . . .
H62B H -0.2015 0.8408 0.5442 0.297 Uiso 1 1 calc R U . . .
H62C H -0.2391 0.7869 0.4821 0.297 Uiso 1 1 calc R U . . .
O14 O 0.5825(17) 0.6851(15) 0.9099(19) 0.434(19) Uani 1 1 d . . . . .
H4N H 0.495(4) 0.450(4) 0.756(4) 0.010(19) 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
Ni2 O3 1.912(5) . ?
Ni2 N1 1.930(7) . ?
Ni2 O1 1.979(6) . ?
Ni2 N2 2.115(6) . ?
Ni2 O2 2.312(5) . ?
Ni1 N5 1.990(7) . ?
Ni1 O1 2.031(5) . ?
Ni1 N4 2.057(8) . ?
Ni1 O2 2.070(5) . ?
Ni1 N6 2.124(6) . ?
Ni1 N3 2.135(6) . ?
Cu2 N14 2.002(7) 2_575 ?
Cu2 N14 2.002(7) . ?
Cu2 O9 2.021(5) . ?
Cu2 O9 2.021(5) 2_575 ?
Cu1 N6 1.979(7) . ?
Cu1 N6 1.979(7) 2_666 ?
Cu1 O2 1.984(5) . ?
Cu1 O2 1.984(5) 2_666 ?
Ni4 N13 1.997(7) . ?
Ni4 O8 2.033(6) . ?
Ni4 N12 2.080(7) . ?
Ni4 N14 2.093(7) . ?
Ni4 O9 2.102(5) . ?
Ni4 N11 2.126(7) . ?
Ni3 N9 1.935(9) . ?
Ni3 O7 1.954(7) . ?
Ni3 O8 1.988(6) . ?
Ni3 N10 2.113(7) . ?
Ni3 O9 2.286(6) . ?
C17 C16 1.402(11) . ?
C17 C12 1.413(10) . ?
C17 C18 1.487(11) . ?
C21 N4 1.478(11) . ?
C21 C22 1.513(12) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C3 C4 1.375(12) . ?
C3 C2 1.378(11) . ?
C3 H3 0.9300 . ?
C12 O2 1.367(9) . ?
C12 C13 1.390(11) . ?
C1 O3 1.327(9) . ?
C1 C6 1.404(11) . ?
C1 C2 1.418(10) . ?
C4 C5 1.368(11) . ?
C4 O5 1.389(10) . ?
C7 N1 1.289(10) . ?
C7 C6 1.448(11) . ?
C7 H7 0.9300 . ?
C8 N1 1.459(10) . ?
C8 C9 1.497(12) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C2 H2 0.9300 . ?
C5 C6 1.411(11) . ?
C5 H5 0.9300 . ?
C13 C14 1.371(11) . ?
C13 H13 0.9300 . ?
C16 C15 1.363(12) . ?
C16 H16 0.9300 . ?
C9 N2 1.487(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C22 N5 1.471(10) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 N5 1.266(12) . ?
C23 C24 1.490(13) . ?
C23 H23 0.9300 . ?
C29 O1 1.335(10) . ?
C29 C28 1.373(12) . ?
C29 C24 1.404(13) . ?
C15 O6 1.379(10) . ?
C15 C14 1.387(11) . ?
C14 H14 0.9300 . ?
C28 C27 1.387(14) . ?
C28 H28 0.9300 . ?
C24 C25 1.398(14) . ?
C27 C26 1.390(16) . ?
C27 H27 0.9300 . ?
C25 C26 1.375(16) . ?
C25 H25 0.9300 . ?
C31 O5 1.401(11) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C26 O4 1.372(14) . ?
C39 N13 1.289(11) . ?
C39 C38 1.459(13) . ?
C39 H39 0.9300 . ?
C33 O8 1.333(10) . ?
C33 C34 1.406(12) . ?
C33 C38 1.424(12) . ?
C37 C36 1.381(14) . ?
C37 C38 1.434(13) . ?
C37 H37 0.9300 . ?
C35 C34 1.376(14) . ?
C35 C36 1.391(15) . ?
C35 H35 0.9300 . ?
C42 N12 1.475(12) . ?
C42 C43 1.497(14) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C41 C40 1.455(13) . ?
C41 N12 1.509(11) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C49 C50 1.406(13) . ?
C49 C48 1.463(15) . ?
C49 C54 1.504(16) . ?
C40 N13 1.468(11) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C45 N10 1.508(11) . ?
C45 C44 1.530(13) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C47 N9 1.440(13) . ?
C47 C46 1.539(14) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C36 O12 1.364(13) . ?
C44 N11 1.512(11) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C54 O7 1.293(13) . ?
C54 C53 1.342(15) . ?
C43 N11 1.499(11) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C46 N10 1.496(11) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C48 N9 1.334(13) . ?
C48 H48 0.9300 . ?
C34 H34 0.9300 . ?
C61 O9 1.378(10) . ?
C61 C56 1.379(12) . ?
C61 C60 1.380(12) . ?
C56 C57 1.403(12) . ?
C56 C55 1.512(12) . ?
C58 C57 1.353(15) . ?
C58 O10 1.368(14) . ?
C58 C59 1.377(15) . ?
C60 C59 1.426(13) . ?
C60 H60 0.9300 . ?
C57 H57 0.9300 . ?
C59 H59 0.9300 . ?
C55 N11 1.479(11) . ?
C55 N10 1.480(11) . ?
C55 H55 0.9800 . ?
C63 O10 1.25(2) . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
Cl1 O19 1.370(12) . ?
Cl1 O18 1.388(10) . ?
Cl1 O20 1.394(8) . ?
Cl1 O17 1.399(8) . ?
N12 H12 0.9800 . ?
N14 N15 1.208(10) . ?
N15 N16 1.168(11) . ?
N6 N7 1.214(9) . ?
N7 N8 1.153(10) . ?
N2 C18 1.494(10) . ?
N2 C10 1.519(11) . ?
N4 C20 1.471(11) . ?
N4 H4N 0.70(6) . ?
C19 C20 1.495(12) . ?
C19 N3 1.503(10) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
N3 C18 1.483(10) . ?
N3 C11 1.492(10) . ?
C11 C10 1.513(12) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C18 H18 0.9800 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
Cl2 O15 1.334(16) . ?
Cl2 O13 1.356(10) . ?
Cl2 O16 1.379(10) . ?
Cl2 O14 1.41(2) . ?
O4 C30 1.33(2) . ?
O6 C32 1.430(14) . ?
O12 C62 1.34(2) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C50 C51 1.345(14) . ?
C50 H50 0.9300 . ?
C53 C52 1.434(15) . ?
C53 H53 0.9300 . ?
C51 O11 1.380(12) . ?
C51 C52 1.400(15) . ?
C52 H52 0.9300 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
O11 C64 1.455(13) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ni2 N1 93.7(3) . . ?
O3 Ni2 O1 91.3(2) . . ?
N1 Ni2 O1 171.3(3) . . ?
O3 Ni2 N2 177.4(3) . . ?
N1 Ni2 N2 83.7(3) . . ?
O1 Ni2 N2 91.2(2) . . ?
O3 Ni2 O2 92.8(2) . . ?
N1 Ni2 O2 104.4(2) . . ?
O1 Ni2 O2 82.5(2) . . ?
N2 Ni2 O2 88.1(2) . . ?
N5 Ni1 O1 89.5(3) . . ?
N5 Ni1 N4 83.6(3) . . ?
O1 Ni1 N4 170.3(3) . . ?
N5 Ni1 O2 169.1(2) . . ?
O1 Ni1 O2 87.6(2) . . ?
N4 Ni1 O2 100.4(3) . . ?
N5 Ni1 N6 94.7(3) . . ?
O1 Ni1 N6 92.3(2) . . ?
N4 Ni1 N6 95.0(3) . . ?
O2 Ni1 N6 74.9(2) . . ?
N5 Ni1 N3 99.2(3) . . ?
O1 Ni1 N3 90.6(2) . . ?
N4 Ni1 N3 83.9(3) . . ?
O2 Ni1 N3 91.4(2) . . ?
N6 Ni1 N3 165.9(3) . . ?
N14 Cu2 N14 180.0 2_575 . ?
N14 Cu2 O9 100.5(2) 2_575 . ?
N14 Cu2 O9 79.5(2) . . ?
N14 Cu2 O9 79.4(2) 2_575 2_575 ?
N14 Cu2 O9 100.5(2) . 2_575 ?
O9 Cu2 O9 180.0 . 2_575 ?
N6 Cu1 N6 180.0 . 2_666 ?
N6 Cu1 O2 80.1(2) . . ?
N6 Cu1 O2 99.9(2) 2_666 . ?
N6 Cu1 O2 99.9(2) . 2_666 ?
N6 Cu1 O2 80.1(2) 2_666 2_666 ?
O2 Cu1 O2 180.0 . 2_666 ?
N13 Ni4 O8 89.0(3) . . ?
N13 Ni4 N12 83.2(3) . . ?
O8 Ni4 N12 170.3(3) . . ?
N13 Ni4 N14 91.9(3) . . ?
O8 Ni4 N14 90.2(3) . . ?
N12 Ni4 N14 95.9(3) . . ?
N13 Ni4 O9 167.3(3) . . ?
O8 Ni4 O9 88.6(2) . . ?
N12 Ni4 O9 100.2(3) . . ?
N14 Ni4 O9 75.6(2) . . ?
N13 Ni4 N11 101.3(3) . . ?
O8 Ni4 N11 90.9(3) . . ?
N12 Ni4 N11 84.9(3) . . ?
N14 Ni4 N11 166.7(3) . . ?
O9 Ni4 N11 91.2(3) . . ?
N9 Ni3 O7 93.2(3) . . ?
N9 Ni3 O8 172.3(3) . . ?
O7 Ni3 O8 89.7(3) . . ?
N9 Ni3 N10 84.9(4) . . ?
O7 Ni3 N10 176.7(3) . . ?
O8 Ni3 N10 92.6(3) . . ?
N9 Ni3 O9 102.5(3) . . ?
O7 Ni3 O9 89.9(3) . . ?
O8 Ni3 O9 84.7(2) . . ?
N10 Ni3 O9 87.8(2) . . ?
C16 C17 C12 117.5(8) . . ?
C16 C17 C18 119.2(7) . . ?
C12 C17 C18 123.1(7) . . ?
N4 C21 C22 111.6(7) . . ?
N4 C21 H21A 109.3 . . ?
C22 C21 H21A 109.3 . . ?
N4 C21 H21B 109.3 . . ?
C22 C21 H21B 109.3 . . ?
H21A C21 H21B 108.0 . . ?
C4 C3 C2 121.0(8) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
O2 C12 C13 122.9(7) . . ?
O2 C12 C17 118.0(7) . . ?
C13 C12 C17 119.1(7) . . ?
O3 C1 C6 124.0(7) . . ?
O3 C1 C2 119.5(7) . . ?
C6 C1 C2 116.6(7) . . ?
C5 C4 C3 119.6(8) . . ?
C5 C4 O5 115.5(8) . . ?
C3 C4 O5 124.9(8) . . ?
N1 C7 C6 125.0(8) . . ?
N1 C7 H7 117.5 . . ?
C6 C7 H7 117.5 . . ?
N1 C8 C9 106.0(7) . . ?
N1 C8 H8A 110.5 . . ?
C9 C8 H8A 110.5 . . ?
N1 C8 H8B 110.5 . . ?
C9 C8 H8B 110.5 . . ?
H8A C8 H8B 108.7 . . ?
C3 C2 C1 121.4(8) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C4 C5 C6 120.6(8) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C14 C13 C12 122.0(8) . . ?
C14 C13 H13 119.0 . . ?
C12 C13 H13 119.0 . . ?
C15 C16 C17 122.2(8) . . ?
C15 C16 H16 118.9 . . ?
C17 C16 H16 118.9 . . ?
N2 C9 C8 111.3(7) . . ?
N2 C9 H9A 109.4 . . ?
C8 C9 H9A 109.4 . . ?
N2 C9 H9B 109.4 . . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N5 C22 C21 107.1(7) . . ?
N5 C22 H22A 110.3 . . ?
C21 C22 H22A 110.3 . . ?
N5 C22 H22B 110.3 . . ?
C21 C22 H22B 110.3 . . ?
H22A C22 H22B 108.6 . . ?
N5 C23 C24 124.9(10) . . ?
N5 C23 H23 117.6 . . ?
C24 C23 H23 117.6 . . ?
O1 C29 C28 121.7(9) . . ?
O1 C29 C24 121.2(8) . . ?
C28 C29 C24 117.0(9) . . ?
C16 C15 O6 116.2(8) . . ?
C16 C15 C14 120.1(8) . . ?
O6 C15 C14 123.7(9) . . ?
C13 C14 C15 119.0(9) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C1 C6 C5 120.7(7) . . ?
C1 C6 C7 123.5(7) . . ?
C5 C6 C7 115.8(8) . . ?
C29 C28 C27 122.5(11) . . ?
C29 C28 H28 118.8 . . ?
C27 C28 H28 118.8 . . ?
C25 C24 C29 120.3(10) . . ?
C25 C24 C23 114.4(10) . . ?
C29 C24 C23 125.3(9) . . ?
C28 C27 C26 120.7(11) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C26 C25 C24 121.9(12) . . ?
C26 C25 H25 119.0 . . ?
C24 C25 H25 119.0 . . ?
O5 C31 H31A 109.5 . . ?
O5 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O5 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O4 C26 C25 115.7(13) . . ?
O4 C26 C27 126.7(12) . . ?
C25 C26 C27 117.5(11) . . ?
C4 O5 C31 118.2(7) . . ?
N13 C39 C38 124.9(9) . . ?
N13 C39 H39 117.6 . . ?
C38 C39 H39 117.6 . . ?
O8 C33 C34 122.0(8) . . ?
O8 C33 C38 121.1(8) . . ?
C34 C33 C38 116.9(9) . . ?
C36 C37 C38 118.3(10) . . ?
C36 C37 H37 120.8 . . ?
C38 C37 H37 120.8 . . ?
C33 C38 C37 120.8(9) . . ?
C33 C38 C39 125.2(9) . . ?
C37 C38 C39 113.9(9) . . ?
C34 C35 C36 119.6(10) . . ?
C34 C35 H35 120.2 . . ?
C36 C35 H35 120.2 . . ?
N12 C42 C43 111.6(9) . . ?
N12 C42 H42A 109.3 . . ?
C43 C42 H42A 109.3 . . ?
N12 C42 H42B 109.3 . . ?
C43 C42 H42B 109.3 . . ?
H42A C42 H42B 108.0 . . ?
C40 C41 N12 113.6(8) . . ?
C40 C41 H41A 108.8 . . ?
N12 C41 H41A 108.8 . . ?
C40 C41 H41B 108.8 . . ?
N12 C41 H41B 108.8 . . ?
H41A C41 H41B 107.7 . . ?
C50 C49 C48 117.8(11) . . ?
C50 C49 C54 121.9(11) . . ?
C48 C49 C54 120.2(10) . . ?
C41 C40 N13 107.0(7) . . ?
C41 C40 H40A 110.3 . . ?
N13 C40 H40A 110.3 . . ?
C41 C40 H40B 110.3 . . ?
N13 C40 H40B 110.3 . . ?
H40A C40 H40B 108.6 . . ?
N10 C45 C44 104.5(8) . . ?
N10 C45 H45A 110.9 . . ?
C44 C45 H45A 110.9 . . ?
N10 C45 H45B 110.9 . . ?
C44 C45 H45B 110.9 . . ?
H45A C45 H45B 108.9 . . ?
N9 C47 C46 107.7(9) . . ?
N9 C47 H47A 110.2 . . ?
C46 C47 H47A 110.2 . . ?
N9 C47 H47B 110.2 . . ?
C46 C47 H47B 110.2 . . ?
H47A C47 H47B 108.5 . . ?
O12 C36 C37 123.1(12) . . ?
O12 C36 C35 115.2(11) . . ?
C37 C36 C35 121.7(11) . . ?
N11 C44 C45 105.2(8) . . ?
N11 C44 H44A 110.7 . . ?
C45 C44 H44A 110.7 . . ?
N11 C44 H44B 110.7 . . ?
C45 C44 H44B 110.7 . . ?
H44A C44 H44B 108.8 . . ?
O7 C54 C53 126.3(11) . . ?
O7 C54 C49 123.2(10) . . ?
C53 C54 C49 110.4(12) . . ?
C42 C43 N11 112.6(8) . . ?
C42 C43 H43A 109.1 . . ?
N11 C43 H43A 109.1 . . ?
C42 C43 H43B 109.1 . . ?
N11 C43 H43B 109.1 . . ?
H43A C43 H43B 107.8 . . ?
N10 C46 C47 109.1(8) . . ?
N10 C46 H46A 109.9 . . ?
C47 C46 H46A 109.9 . . ?
N10 C46 H46B 109.9 . . ?
C47 C46 H46B 109.9 . . ?
H46A C46 H46B 108.3 . . ?
N9 C48 C49 126.6(11) . . ?
N9 C48 H48 116.7 . . ?
C49 C48 H48 116.7 . . ?
C35 C34 C33 122.5(10) . . ?
C35 C34 H34 118.7 . . ?
C33 C34 H34 118.7 . . ?
O9 C61 C56 120.2(8) . . ?
O9 C61 C60 121.4(8) . . ?
C56 C61 C60 118.4(9) . . ?
C61 C56 C57 120.1(9) . . ?
C61 C56 C55 121.9(9) . . ?
C57 C56 C55 118.0(8) . . ?
C57 C58 O10 116.0(12) . . ?
C57 C58 C59 119.1(11) . . ?
O10 C58 C59 124.9(13) . . ?
C61 C60 C59 120.8(10) . . ?
C61 C60 H60 119.6 . . ?
C59 C60 H60 119.6 . . ?
C58 C57 C56 122.0(10) . . ?
C58 C57 H57 119.0 . . ?
C56 C57 H57 119.0 . . ?
C58 C59 C60 119.6(11) . . ?
C58 C59 H59 120.2 . . ?
C60 C59 H59 120.2 . . ?
N11 C55 N10 102.3(7) . . ?
N11 C55 C56 115.6(7) . . ?
N10 C55 C56 114.9(7) . . ?
N11 C55 H55 107.8 . . ?
N10 C55 H55 107.8 . . ?
C56 C55 H55 107.8 . . ?
O10 C63 H63A 109.5 . . ?
O10 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
O10 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C63 O10 C58 123.1(16) . . ?
C7 N1 C8 120.2(7) . . ?
C7 N1 Ni2 124.7(6) . . ?
C8 N1 Ni2 114.8(5) . . ?
C1 O3 Ni2 123.6(5) . . ?
C12 O2 Cu1 123.5(5) . . ?
C12 O2 Ni1 117.7(4) . . ?
Cu1 O2 Ni1 103.1(2) . . ?
C12 O2 Ni2 116.2(4) . . ?
Cu1 O2 Ni2 102.2(2) . . ?
Ni1 O2 Ni2 87.52(19) . . ?
C29 O1 Ni2 129.6(5) . . ?
C29 O1 Ni1 123.8(5) . . ?
Ni2 O1 Ni1 98.4(2) . . ?
O19 Cl1 O18 106.7(10) . . ?
O19 Cl1 O20 104.8(7) . . ?
O18 Cl1 O20 112.1(7) . . ?
O19 Cl1 O17 109.6(8) . . ?
O18 Cl1 O17 109.2(6) . . ?
O20 Cl1 O17 114.1(6) . . ?
C48 N9 C47 123.1(9) . . ?
C48 N9 Ni3 123.3(9) . . ?
C47 N9 Ni3 113.2(6) . . ?
C54 O7 Ni3 123.2(7) . . ?
C55 N11 C43 113.3(7) . . ?
C55 N11 C44 101.9(7) . . ?
C43 N11 C44 111.6(7) . . ?
C55 N11 Ni4 113.7(5) . . ?
C43 N11 Ni4 105.0(6) . . ?
C44 N11 Ni4 111.6(6) . . ?
C42 N12 C41 115.6(7) . . ?
C42 N12 Ni4 109.1(6) . . ?
C41 N12 Ni4 105.5(6) . . ?
C42 N12 H12 108.8 . . ?
C41 N12 H12 108.8 . . ?
Ni4 N12 H12 108.8 . . ?
N15 N14 Cu2 132.0(6) . . ?
N15 N14 Ni4 125.0(6) . . ?
Cu2 N14 Ni4 102.7(3) . . ?
N16 N15 N14 177.5(10) . . ?
N7 N6 Cu1 134.7(6) . . ?
N7 N6 Ni1 123.9(6) . . ?
Cu1 N6 Ni1 101.4(3) . . ?
N8 N7 N6 178.4(9) . . ?
C9 N2 C18 113.3(7) . . ?
C9 N2 C10 111.2(6) . . ?
C18 N2 C10 101.1(6) . . ?
C9 N2 Ni2 104.4(5) . . ?
C18 N2 Ni2 115.9(5) . . ?
C10 N2 Ni2 111.2(5) . . ?
C33 O8 Ni3 128.0(5) . . ?
C33 O8 Ni4 122.0(5) . . ?
Ni3 O8 Ni4 96.6(3) . . ?
C61 O9 Cu2 127.7(5) . . ?
C61 O9 Ni4 117.4(5) . . ?
Cu2 O9 Ni4 101.6(2) . . ?
C61 O9 Ni3 115.8(5) . . ?
Cu2 O9 Ni3 99.3(2) . . ?
Ni4 O9 Ni3 86.2(2) . . ?
C39 N13 C40 119.7(8) . . ?
C39 N13 Ni4 122.6(7) . . ?
C40 N13 Ni4 114.5(6) . . ?
C55 N10 C46 113.7(8) . . ?
C55 N10 C45 101.1(7) . . ?
C46 N10 C45 109.5(7) . . ?
C55 N10 Ni3 116.8(5) . . ?
C46 N10 Ni3 104.7(6) . . ?
C45 N10 Ni3 111.2(6) . . ?
C20 N4 C21 115.6(7) . . ?
C20 N4 Ni1 110.7(5) . . ?
C21 N4 Ni1 107.1(6) . . ?
C20 N4 H4N 103(5) . . ?
C21 N4 H4N 100(5) . . ?
Ni1 N4 H4N 121(5) . . ?
C20 C19 N3 111.5(6) . . ?
C20 C19 H19A 109.3 . . ?
N3 C19 H19A 109.3 . . ?
C20 C19 H19B 109.3 . . ?
N3 C19 H19B 109.3 . . ?
H19A C19 H19B 108.0 . . ?
N4 C20 C19 111.8(7) . . ?
N4 C20 H20A 109.3 . . ?
C19 C20 H20A 109.3 . . ?
N4 C20 H20B 109.3 . . ?
C19 C20 H20B 109.3 . . ?
H20A C20 H20B 107.9 . . ?
C18 N3 C11 102.2(6) . . ?
C18 N3 C19 112.8(7) . . ?
C11 N3 C19 109.6(6) . . ?
C18 N3 Ni1 113.1(4) . . ?
C11 N3 Ni1 112.9(5) . . ?
C19 N3 Ni1 106.4(5) . . ?
N3 C11 C10 105.5(7) . . ?
N3 C11 H11A 110.6 . . ?
C10 C11 H11A 110.6 . . ?
N3 C11 H11B 110.6 . . ?
C10 C11 H11B 110.6 . . ?
H11A C11 H11B 108.8 . . ?
N3 C18 C17 115.9(7) . . ?
N3 C18 N2 102.1(6) . . ?
C17 C18 N2 115.4(7) . . ?
N3 C18 H18 107.7 . . ?
C17 C18 H18 107.7 . . ?
N2 C18 H18 107.7 . . ?
C11 C10 N2 105.4(7) . . ?
C11 C10 H10A 110.7 . . ?
N2 C10 H10A 110.7 . . ?
C11 C10 H10B 110.7 . . ?
N2 C10 H10B 110.7 . . ?
H10A C10 H10B 108.8 . . ?
C23 N5 C22 118.8(8) . . ?
C23 N5 Ni1 124.7(7) . . ?
C22 N5 Ni1 114.4(6) . . ?
O15 Cl2 O13 106.0(9) . . ?
O15 Cl2 O16 99.2(10) . . ?
O13 Cl2 O16 115.2(10) . . ?
O15 Cl2 O14 123.4(16) . . ?
O13 Cl2 O14 108.4(13) . . ?
O16 Cl2 O14 104.9(14) . . ?
C30 O4 C26 119.9(16) . . ?
C15 O6 C32 115.1(8) . . ?
C62 O12 C36 119.5(13) . . ?
O6 C32 H32A 109.5 . . ?
O6 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O6 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C51 C50 C49 121.6(11) . . ?
C51 C50 H50 119.2 . . ?
C49 C50 H50 119.2 . . ?
C54 C53 C52 129.1(13) . . ?
C54 C53 H53 115.5 . . ?
C52 C53 H53 115.5 . . ?
C50 C51 O11 125.6(11) . . ?
C50 C51 C52 120.2(11) . . ?
O11 C51 C52 114.2(11) . . ?
C51 C52 C53 116.4(12) . . ?
C51 C52 H52 121.8 . . ?
C53 C52 H52 121.8 . . ?
O4 C30 H30A 109.5 . . ?
O4 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O4 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C51 O11 C64 118.6(10) . . ?
O11 C64 H64A 109.5 . . ?
O11 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
O11 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
O12 C62 H62A 109.5 . . ?
O12 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
O12 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?

_refine_diff_density_max         1.313
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.103

####################################################################### 
# 
# 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_skc-26g
_database_code_depnum_ccdc_archive 'CCDC 1571835'
_audit_update_record             
;
2017-08-31 deposited with the CCDC.
2018-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H38 Mn2 N11 O12'
_chemical_formula_weight         866.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6851(16)
_cell_length_b                   19.094(3)
_cell_length_c                   19.263(3)
_cell_angle_alpha                103.316(7)
_cell_angle_beta                 101.779(7)
_cell_angle_gamma                94.381(7)
_cell_volume                     3712.3(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1881
_cell_measurement_theta_min      0.00
_cell_measurement_theta_max      0.00

_exptl_crystal_description       blocks
_exptl_crystal_colour            redish
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1788
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26845
_diffrn_reflns_av_R_equivalents  0.1472
_diffrn_reflns_av_sigmaI/netI    0.3867
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.11
_diffrn_reflns_theta_max         28.47
_reflns_number_total             15090
_reflns_number_gt                3283
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         15090
_refine_ls_number_parameters     1039
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.3134
_refine_ls_R_factor_gt           0.0891
_refine_ls_wR_factor_ref         0.3224
_refine_ls_wR_factor_gt          0.1930
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.5000(3) 0.78627(14) 0.27668(17) 0.0438(8) Uani 1 1 d . . .
Mn2 Mn 0.1919(3) 0.79294(15) 0.27240(19) 0.0525(9) Uani 1 1 d . . .
Mn3 Mn 1.0006(3) 0.28559(15) 0.27599(17) 0.0450(8) Uani 1 1 d . . .
Mn4 Mn 0.6923(3) 0.29290(16) 0.27270(19) 0.0513(9) Uani 1 1 d . . .
N3 N 0.4353(13) 0.6693(6) 0.2933(8) 0.038(3) Uani 1 1 d . . .
N12 N 0.9334(13) 0.1690(7) 0.2918(9) 0.043(4) Uani 1 1 d . . .
N5 N 0.6475(14) 0.8504(8) 0.3763(9) 0.046(4) Uani 1 1 d . . .
N14 N 1.1461(15) 0.3511(9) 0.3750(10) 0.050(4) Uani 1 1 d . . .
N15 N 0.7227(14) 0.1769(8) 0.2970(9) 0.043(4) Uani 1 1 d . . .
N16 N 0.5294(15) 0.2164(9) 0.1959(9) 0.054(5) Uani 1 1 d . . .
N9 N 0.484(2) 1.1497(8) 0.4650(10) 0.057(5) Uani 1 1 d . . .
N20 N 0.9815(18) 0.6486(10) 0.4650(9) 0.057(4) Uani 1 1 d . . .
N4 N 0.6762(17) 0.7282(9) 0.2759(10) 0.055(5) Uani 1 1 d . . .
N13 N 1.1788(13) 0.2265(8) 0.2723(10) 0.052(5) Uani 1 1 d . . .
N10 N -0.1159(19) 0.8304(17) -0.0736(16) 0.093(9) Uani 1 1 d . . .
N22 N 0.6657(19) -0.0086(11) -0.0035(14) 0.075(6) Uani 1 1 d . . .
N11 N 0.1702(19) 0.4880(13) -0.0034(15) 0.089(7) Uani 1 1 d . . .
N21 N 0.384(2) 0.3364(18) -0.0735(14) 0.107(8) Uani 1 1 d . . .
O1 O 0.3779(12) 0.8537(6) 0.3284(7) 0.051(3) Uani 1 1 d . . .
O2 O 0.3266(12) 0.7596(6) 0.1980(7) 0.049(4) Uani 1 1 d . . .
O10 O 0.5947(16) 1.1769(8) 0.4937(10) 0.091(6) Uani 1 1 d . . .
O9 O 0.3888(17) 1.1837(8) 0.4656(10) 0.082(5) Uani 1 1 d . . .
O7 O -0.175(2) 0.7733(15) -0.1112(12) 0.127(8) Uani 1 1 d . . .
O6 O 0.157(2) 0.4372(11) 0.0192(11) 0.121(8) Uani 1 1 d . . .
O8 O -0.1051(19) 0.8848(13) -0.1005(11) 0.125(7) Uani 1 1 d . . .
O5 O 0.141(3) 0.4888(11) -0.0678(14) 0.144(9) Uani 1 1 d . . .
O11 O 0.8811(11) 0.3546(6) 0.3297(7) 0.048(4) Uani 1 1 d . . .
O12 O 0.8212(13) 0.2575(7) 0.1940(8) 0.060(4) Uani 1 1 d . . .
O20 O 1.0917(16) 0.6749(8) 0.4898(10) 0.087(5) Uani 1 1 d . . .
O19 O 0.8895(17) 0.6845(8) 0.4657(9) 0.085(5) Uani 1 1 d . . .
O17 O 0.3295(19) 0.2744(13) -0.1116(11) 0.109(7) Uani 1 1 d . . .
O16 O 0.6600(17) -0.0647(9) 0.0182(11) 0.109(7) Uani 1 1 d . . .
O15 O 0.6424(19) -0.0114(11) -0.0687(13) 0.120(8) Uani 1 1 d . . .
O18 O 0.390(2) 0.3859(14) -0.1006(12) 0.141(10) Uani 1 1 d . . .
O13 O 0.6184(17) 0.3660(7) 0.2154(11) 0.100(7) Uani 1 1 d . . .
C4 C 0.457(2) 1.0732(10) 0.4304(11) 0.050(5) Uani 1 1 d . . .
C14 C 0.2369(14) 0.5645(10) 0.1242(11) 0.049(5) Uani 1 1 d . . .
H14 H 0.2275 0.5226 0.1405 0.059 Uiso 1 1 calc R . .
C15 C 0.2129(19) 0.5600(12) 0.0496(14) 0.060(6) Uani 1 1 d . . .
C2 C 0.5346(17) 0.9578(10) 0.3988(10) 0.040(5) Uani 1 1 d . . .
C13 C 0.2762(16) 0.6335(10) 0.1761(11) 0.046(5) Uani 1 1 d . . .
C12 C 0.3007(14) 0.6336(9) 0.2538(11) 0.039(5) Uani 1 1 d . . .
H12 H 0.2889 0.5837 0.2588 0.046 Uiso 1 1 calc R . .
C7 C 0.6452(19) 0.9180(10) 0.4071(10) 0.049(5) Uani 1 1 d . . .
H7 H 0.7218 0.9436 0.4376 0.059 Uiso 1 1 calc R . .
C1 C 0.4032(18) 0.9229(10) 0.3608(10) 0.046(5) Uani 1 1 d . . .
C3 C 0.558(2) 1.0320(9) 0.4329(11) 0.052(5) Uani 1 1 d . . .
H3 H 0.6408 1.0537 0.4572 0.063 Uiso 1 1 calc R . .
C10 C 0.6633(18) 0.6617(10) 0.3015(14) 0.069(7) Uani 1 1 d . . .
H10A H 0.6837 0.6742 0.3547 0.083 Uiso 1 1 calc R . .
H10B H 0.7239 0.6302 0.2850 0.083 Uiso 1 1 calc R . .
C5 C 0.330(2) 1.0422(10) 0.3962(12) 0.054(6) Uani 1 1 d . . .
H5 H 0.2633 1.0705 0.3966 0.065 Uiso 1 1 calc R . .
C16 C 0.2207(19) 0.6216(13) 0.0224(14) 0.077(7) Uani 1 1 d . . .
H16 H 0.1988 0.6181 -0.0276 0.092 Uiso 1 1 calc R . .
C6 C 0.3053(18) 0.9675(10) 0.3611(12) 0.054(6) Uani 1 1 d . . .
H6 H 0.2210 0.9473 0.3374 0.065 Uiso 1 1 calc R . .
C17 C 0.261(2) 0.6870(12) 0.0718(13) 0.065(7) Uani 1 1 d . . .
H17 H 0.2722 0.7280 0.0542 0.078 Uiso 1 1 calc R . .
C11 C 0.5269(18) 0.6218(9) 0.2726(12) 0.053(5) Uani 1 1 d . . .
H11A H 0.5092 0.6051 0.2196 0.064 Uiso 1 1 calc R . .
H11B H 0.5190 0.5798 0.2924 0.064 Uiso 1 1 calc R . .
C9 C 0.7953(18) 0.7792(11) 0.3163(13) 0.062(7) Uani 1 1 d . . .
H9A H 0.8137 0.8137 0.2887 0.074 Uiso 1 1 calc R . .
H9B H 0.8685 0.7527 0.3245 0.074 Uiso 1 1 calc R . .
C8 C 0.7687(15) 0.8187(11) 0.3896(12) 0.061(6) Uani 1 1 d . . .
H8A H 0.7624 0.7848 0.4197 0.073 Uiso 1 1 calc R . .
H8B H 0.8392 0.8567 0.4156 0.073 Uiso 1 1 calc R . .
C18 C 0.2873(16) 0.6954(8) 0.1466(10) 0.034(4) Uani 1 1 d . . .
N1 N 0.0280(14) 0.7183(9) 0.1942(11) 0.054(5) Uani 1 1 d . . .
C23 C -0.0227(17) 0.7206(10) 0.1316(13) 0.053(6) Uani 1 1 d . . .
H23 H -0.0740 0.6796 0.0998 0.063 Uiso 1 1 calc R . .
C24 C -0.0038(18) 0.7884(12) 0.1050(12) 0.059(6) Uani 1 1 d . . .
C25 C -0.063(2) 0.7833(13) 0.0344(13) 0.072(7) Uani 1 1 d . . .
H25 H -0.1085 0.7386 0.0071 0.087 Uiso 1 1 calc R . .
C26 C -0.061(2) 0.8370(19) 0.0008(17) 0.084(9) Uani 1 1 d . . .
C29 C 0.066(2) 0.8584(11) 0.1530(15) 0.085(8) Uani 1 1 d . . .
C28 C 0.062(3) 0.9160(12) 0.1169(17) 0.103(10) Uani 1 1 d . . .
H28 H 0.1009 0.9625 0.1433 0.123 Uiso 1 1 calc R . .
C27 C 0.001(3) 0.9040(19) 0.0413(19) 0.101(11) Uani 1 1 d . . .
H27 H 0.0026 0.9423 0.0191 0.121 Uiso 1 1 calc R . .
O4 O 0.1171(18) 0.8668(8) 0.2176(11) 0.116(7) Uani 1 1 d . . .
N2 N 0.2248(15) 0.6789(8) 0.2974(10) 0.048(4) Uani 1 1 d . . .
C20 C 0.2893(16) 0.6831(11) 0.3747(11) 0.052(5) Uani 1 1 d . . .
H20A H 0.2576 0.6415 0.3900 0.063 Uiso 1 1 calc R . .
H20B H 0.2750 0.7270 0.4074 0.063 Uiso 1 1 calc R . .
C21 C 0.0908(17) 0.6439(11) 0.2839(13) 0.064(7) Uani 1 1 d . . .
H21A H 0.0519 0.6681 0.3226 0.077 Uiso 1 1 calc R . .
H21B H 0.0926 0.5938 0.2863 0.077 Uiso 1 1 calc R . .
C19 C 0.4322(17) 0.6835(11) 0.3742(13) 0.054(6) Uani 1 1 d . . .
H19A H 0.4809 0.7300 0.4017 0.064 Uiso 1 1 calc R . .
H19B H 0.4678 0.6457 0.3951 0.064 Uiso 1 1 calc R . .
O3 O 0.5653(16) 0.8647(8) 0.2205(8) 0.084(5) Uani 1 1 d . . .
N7 N 0.1130(16) 0.8638(10) 0.4221(13) 0.064(6) Uani 1 1 d . . .
N8 N 0.1154(15) 0.9113(11) 0.4760(13) 0.084(7) Uani 1 1 d . . .
N6 N 0.1133(16) 0.8180(10) 0.3710(12) 0.075(6) Uani 1 1 d . . .
C54 C 1.0342(19) 0.4552(10) 0.3989(11) 0.047(5) Uani 1 1 d . . .
C50 C 1.1664(17) 0.1601(10) 0.2990(10) 0.042(5) Uani 1 1 d . . .
H50A H 1.2278 0.1287 0.2832 0.050 Uiso 1 1 calc R . .
H50B H 1.1856 0.1731 0.3521 0.050 Uiso 1 1 calc R . .
C55 C 1.0547(18) 0.5308(10) 0.4325(10) 0.041(5) Uani 1 1 d . . .
H55 H 1.1376 0.5536 0.4559 0.049 Uiso 1 1 calc R . .
C59 C 0.9080(18) 0.4236(9) 0.3631(11) 0.042(5) Uani 1 1 d . . .
C53 C 1.1421(17) 0.4150(11) 0.4053(11) 0.049(5) Uani 1 1 d . . .
H53 H 1.2186 0.4402 0.4363 0.059 Uiso 1 1 calc R . .
C56 C 0.953(2) 0.5701(9) 0.4305(11) 0.049(5) Uani 1 1 d . . .
C57 C 0.827(2) 0.5406(11) 0.3959(11) 0.058(6) Uani 1 1 d . . .
H57 H 0.7597 0.5687 0.3947 0.070 Uiso 1 1 calc R . .
C58 C 0.808(2) 0.4674(10) 0.3637(12) 0.056(6) Uani 1 1 d . . .
H58 H 0.7240 0.4456 0.3410 0.068 Uiso 1 1 calc R . .
C51 C 1.2930(19) 0.2782(10) 0.3191(13) 0.061(6) Uani 1 1 d . . .
H51A H 1.3169 0.3123 0.2922 0.073 Uiso 1 1 calc R . .
H51B H 1.3651 0.2513 0.3293 0.073 Uiso 1 1 calc R . .
C52 C 1.268(2) 0.3198(11) 0.3904(14) 0.070(7) Uani 1 1 d . . .
H52A H 1.2625 0.2876 0.4223 0.084 Uiso 1 1 calc R . .
H52B H 1.3390 0.3582 0.4149 0.084 Uiso 1 1 calc R . .
C49 C 1.0327(17) 0.1209(10) 0.2697(11) 0.045(5) Uani 1 1 d . . .
H49A H 1.0254 0.0780 0.2882 0.054 Uiso 1 1 calc R . .
H49B H 1.0158 0.1054 0.2166 0.054 Uiso 1 1 calc R . .
C39 C 0.5861(18) 0.1447(10) 0.2836(11) 0.053(5) Uani 1 1 d . . .
H39A H 0.5483 0.1712 0.3218 0.063 Uiso 1 1 calc R . .
H39B H 0.5845 0.0950 0.2877 0.063 Uiso 1 1 calc R . .
C37 C 0.4788(18) 0.2252(11) 0.1300(12) 0.059(6) Uani 1 1 d . . .
H37 H 0.4272 0.1846 0.0978 0.070 Uiso 1 1 calc R . .
C36 C 0.4909(19) 0.2868(11) 0.1006(13) 0.061(6) Uani 1 1 d . . .
C38 C 0.504(2) 0.1450(11) 0.2107(12) 0.061(6) Uani 1 1 d . . .
H38A H 0.5232 0.1073 0.1726 0.073 Uiso 1 1 calc R . .
H38B H 0.4135 0.1352 0.2109 0.073 Uiso 1 1 calc R . .
C35 C 0.4349(18) 0.2823(14) 0.0298(14) 0.071(7) Uani 1 1 d . . .
H35 H 0.3897 0.2386 0.0000 0.085 Uiso 1 1 calc R . .
C32 C 0.568(3) 0.4135(14) 0.1138(16) 0.100(9) Uani 1 1 d . . .
H32 H 0.6146 0.4574 0.1421 0.120 Uiso 1 1 calc R . .
C33 C 0.511(2) 0.4089(12) 0.0455(16) 0.102(9) Uani 1 1 d . . .
H33 H 0.5146 0.4495 0.0267 0.123 Uiso 1 1 calc R . .
C31 C 0.560(2) 0.3535(13) 0.1467(14) 0.090(9) Uani 1 1 d . . .
C34 C 0.444(2) 0.3425(14) 0.0012(14) 0.068(7) Uani 1 1 d . . .
C41 C 0.933(2) 0.1810(10) 0.3689(11) 0.054(6) Uani 1 1 d . . .
H41A H 0.9849 0.2263 0.3970 0.065 Uiso 1 1 calc R . .
H41B H 0.9660 0.1418 0.3881 0.065 Uiso 1 1 calc R . .
C40 C 0.795(2) 0.1838(10) 0.3727(11) 0.064(6) Uani 1 1 d . . .
H40A H 0.7644 0.1443 0.3913 0.077 Uiso 1 1 calc R . .
H40B H 0.7853 0.2294 0.4046 0.077 Uiso 1 1 calc R . .
N18 N 0.6155(14) 0.3645(12) 0.4235(13) 0.065(6) Uani 1 1 d . . .
N17 N 0.6171(19) 0.3189(11) 0.3700(13) 0.079(6) Uani 1 1 d . . .
N19 N 0.610(2) 0.4078(10) 0.4719(13) 0.099(8) Uani 1 1 d . . .
O14 O 1.0616(14) 0.3660(8) 0.2194(9) 0.078(5) Uani 1 1 d . . .
C60 C 0.990(3) 0.3938(19) 0.1639(19) 0.149(13) Uani 1 1 d . . .
H60A H 0.9835 0.3612 0.1169 0.224 Uiso 1 1 calc R . .
H60B H 1.0317 0.4405 0.1652 0.224 Uiso 1 1 calc R . .
H60C H 0.9046 0.3986 0.1720 0.224 Uiso 1 1 calc R . .
C30 C 0.483(3) 0.8959(14) 0.1699(17) 0.151(15) Uani 1 1 d . . .
H30A H 0.4184 0.8587 0.1369 0.226 Uiso 1 1 calc R . .
H30B H 0.5336 0.9172 0.1424 0.226 Uiso 1 1 calc R . .
H30C H 0.4418 0.9326 0.1965 0.226 Uiso 1 1 calc R . .
C22 C 0.0062(16) 0.6455(9) 0.2098(11) 0.052(6) Uani 1 1 d . . .
H22A H 0.0260 0.6085 0.1713 0.062 Uiso 1 1 calc R . .
H22B H -0.0838 0.6347 0.2102 0.062 Uiso 1 1 calc R . .
C44 C 0.7905(19) 0.1925(12) 0.1514(13) 0.056(6) Uani 1 1 d . . .
C48 C 0.7337(19) 0.0636(10) 0.1205(14) 0.055(6) Uani 1 1 d . . .
H48 H 0.7223 0.0208 0.1351 0.066 Uiso 1 1 calc R . .
C43 C 0.7732(17) 0.1267(10) 0.1720(13) 0.046(5) Uani 1 1 d . . .
C45 C 0.7653(17) 0.1897(11) 0.0738(11) 0.061(6) Uani 1 1 d . . .
H45 H 0.7757 0.2317 0.0577 0.074 Uiso 1 1 calc R . .
C47 C 0.710(2) 0.0608(13) 0.0477(15) 0.063(7) Uani 1 1 d . . .
C46 C 0.725(2) 0.1223(12) 0.0243(11) 0.066(6) Uani 1 1 d . . .
H46 H 0.7084 0.1191 -0.0257 0.079 Uiso 1 1 calc R . .
C42 C 0.8036(19) 0.1350(10) 0.2543(12) 0.051(5) Uani 1 1 d . . .
H42 H 0.7955 0.0859 0.2618 0.062 Uiso 1 1 calc R . .
O22 O 0.536(2) 0.4926(10) 0.5988(12) 0.104(7) Uani 1 1 d . . .
O21 O 0.045(2) 0.9931(10) 0.5997(13) 0.104(7) Uani 1 1 d . . .
O24 O 0.789(2) 0.9505(9) 0.2653(12) 0.120(7) Uani 1 1 d . . .
H24 H 0.7245 0.9207 0.2549 0.180 Uiso 1 1 calc R . .
O23 O 0.299(2) 0.4452(11) 0.2641(12) 0.121(8) Uani 1 1 d . . .
H23A H 0.3452 0.4493 0.3047 0.182 Uiso 1 1 calc R . .
C61 C 0.352(7) 0.419(2) 0.219(4) 0.49(7) Uani 1 1 d . . .
H61A H 0.3199 0.3684 0.1996 0.739 Uiso 1 1 calc R . .
H61B H 0.4433 0.4241 0.2396 0.739 Uiso 1 1 calc R . .
H61C H 0.3378 0.4430 0.1796 0.739 Uiso 1 1 calc R . .
C62 C 0.8667(19) 0.9259(14) 0.233(2) 0.142(14) Uani 1 1 d . . .
H62A H 0.9341 0.9638 0.2366 0.213 Uiso 1 1 calc R . .
H62B H 0.8254 0.9053 0.1823 0.213 Uiso 1 1 calc R . .
H62C H 0.9030 0.8889 0.2538 0.213 Uiso 1 1 calc R . .
H21C H 0.01(2) 0.986(13) 0.555(15) 0.12(10) Uiso 1 1 d . . .
H21D H -0.07(4) 0.97(2) 0.58(2) 0.3(2) Uiso 1 1 d . . .
H22D H 0.578(8) 0.464(5) 0.568(6) 0.01(2) Uiso 1 1 d . . .
H22C H 0.472(12) 0.516(7) 0.556(8) 0.07(4) Uiso 1 1 d . . .
H13N H 1.201(13) 0.225(7) 0.213(9) 0.06(5) Uiso 1 1 d . . .
H4N H 0.694(9) 0.725(5) 0.240(7) 0.00(3) 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 O2 2.084(13) . ?
Mn1 O1 2.134(13) . ?
Mn1 O3 2.189(13) . ?
Mn1 N5 2.247(15) . ?
Mn1 N4 2.258(17) . ?
Mn1 N3 2.399(13) . ?
Mn2 O4 2.062(16) . ?
Mn2 O1 2.158(12) . ?
Mn2 N6 2.20(2) . ?
Mn2 N1 2.218(16) . ?
Mn2 O2 2.257(14) . ?
Mn2 N2 2.372(15) . ?
Mn3 O11 2.145(13) . ?
Mn3 O12 2.162(13) . ?
Mn3 O14 2.209(14) . ?
Mn3 N14 2.239(18) . ?
Mn3 N13 2.291(15) . ?
Mn3 N12 2.393(13) . ?
Mn4 O13 2.076(17) . ?
Mn4 N17 2.16(2) . ?
Mn4 O11 2.191(11) . ?
Mn4 N16 2.218(16) . ?
Mn4 O12 2.275(16) . ?
Mn4 N15 2.399(14) . ?
N3 C11 1.44(2) . ?
N3 C12 1.51(2) . ?
N3 C19 1.53(2) . ?
N12 C42 1.45(2) . ?
N12 C41 1.45(2) . ?
N12 C49 1.52(2) . ?
N5 C7 1.30(2) . ?
N5 C8 1.47(2) . ?
N14 C53 1.23(2) . ?
N14 C52 1.48(2) . ?
N15 C42 1.47(2) . ?
N15 C40 1.48(2) . ?
N15 C39 1.49(2) . ?
N16 C37 1.33(2) . ?
N16 C38 1.47(2) . ?
N9 O10 1.21(2) . ?
N9 O9 1.25(2) . ?
N9 C4 1.44(2) . ?
N20 O20 1.199(19) . ?
N20 O19 1.24(2) . ?
N20 C56 1.47(2) . ?
N4 C10 1.47(2) . ?
N4 C9 1.49(2) . ?
N13 C50 1.48(2) . ?
N13 C51 1.49(2) . ?
N10 O7 1.21(3) . ?
N10 O8 1.27(3) . ?
N10 C26 1.41(3) . ?
N22 O15 1.22(3) . ?
N22 O16 1.24(2) . ?
N22 C47 1.44(3) . ?
N11 O6 1.16(3) . ?
N11 O5 1.22(3) . ?
N11 C15 1.49(3) . ?
N21 O18 1.18(3) . ?
N21 O17 1.26(3) . ?
N21 C34 1.43(3) . ?
O1 C1 1.305(19) . ?
O2 C18 1.359(19) . ?
O11 C59 1.306(19) . ?
O12 C44 1.30(2) . ?
O13 C31 1.30(3) . ?
C4 C3 1.38(2) . ?
C4 C5 1.40(3) . ?
C14 C15 1.39(3) . ?
C14 C13 1.43(2) . ?
C15 C16 1.40(3) . ?
C2 C3 1.40(2) . ?
C2 C7 1.45(2) . ?
C2 C1 1.47(2) . ?
C13 C18 1.43(2) . ?
C13 C12 1.47(3) . ?
C12 N2 1.47(2) . ?
C1 C6 1.40(2) . ?
C10 C11 1.52(3) . ?
C5 C6 1.41(2) . ?
C16 C17 1.36(3) . ?
C17 C18 1.38(3) . ?
C9 C8 1.53(3) . ?
N1 C23 1.23(2) . ?
N1 C22 1.50(2) . ?
C23 C24 1.51(3) . ?
C24 C25 1.36(3) . ?
C24 C29 1.48(3) . ?
C25 C26 1.33(3) . ?
C26 C27 1.37(4) . ?
C29 O4 1.22(3) . ?
C29 C28 1.43(3) . ?
C28 C27 1.43(4) . ?
N2 C21 1.48(2) . ?
N2 C20 1.49(2) . ?
C20 C19 1.53(2) . ?
C21 C22 1.53(3) . ?
O3 C30 1.44(2) . ?
N7 N6 1.16(2) . ?
N7 N8 1.21(2) . ?
C54 C59 1.40(2) . ?
C54 C55 1.42(2) . ?
C54 C53 1.43(3) . ?
C50 C49 1.49(2) . ?
C55 C56 1.36(2) . ?
C59 C58 1.41(3) . ?
C56 C57 1.39(3) . ?
C57 C58 1.37(2) . ?
C51 C52 1.51(3) . ?
C39 C38 1.50(3) . ?
C37 C36 1.43(3) . ?
C36 C35 1.35(3) . ?
C36 C31 1.42(3) . ?
C35 C34 1.39(3) . ?
C32 C33 1.31(3) . ?
C32 C31 1.44(3) . ?
C33 C34 1.40(3) . ?
C41 C40 1.49(3) . ?
N18 N19 1.11(2) . ?
N18 N17 1.19(3) . ?
O14 C60 1.42(3) . ?
C44 C43 1.41(3) . ?
C44 C45 1.45(3) . ?
C48 C43 1.35(3) . ?
C48 C47 1.36(3) . ?
C43 C42 1.52(3) . ?
C45 C46 1.39(3) . ?
C47 C46 1.36(3) . ?
O24 C62 1.20(3) . ?
O23 C61 1.18(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
O2 Mn1 O1 78.0(5) . . ?
O2 Mn1 O3 89.7(5) . . ?
O1 Mn1 O3 95.3(6) . . ?
O2 Mn1 N5 158.3(5) . . ?
O1 Mn1 N5 81.1(5) . . ?
O3 Mn1 N5 86.2(6) . . ?
O2 Mn1 N4 126.4(6) . . ?
O1 Mn1 N4 153.9(6) . . ?
O3 Mn1 N4 94.0(6) . . ?
N5 Mn1 N4 75.2(6) . . ?
O2 Mn1 N3 81.3(5) . . ?
O1 Mn1 N3 103.2(5) . . ?
O3 Mn1 N3 157.2(6) . . ?
N5 Mn1 N3 109.6(5) . . ?
N4 Mn1 N3 75.2(6) . . ?
O4 Mn2 O1 99.0(6) . . ?
O4 Mn2 N6 101.6(8) . . ?
O1 Mn2 N6 93.3(6) . . ?
O4 Mn2 N1 82.5(6) . . ?
O1 Mn2 N1 165.5(6) . . ?
N6 Mn2 N1 100.5(7) . . ?
O4 Mn2 O2 94.2(7) . . ?
O1 Mn2 O2 73.9(5) . . ?
N6 Mn2 O2 161.1(6) . . ?
N1 Mn2 O2 91.7(6) . . ?
O4 Mn2 N2 158.8(6) . . ?
O1 Mn2 N2 99.8(5) . . ?
N6 Mn2 N2 87.1(7) . . ?
N1 Mn2 N2 76.9(6) . . ?
O2 Mn2 N2 81.7(5) . . ?
O11 Mn3 O12 79.5(5) . . ?
O11 Mn3 O14 93.7(6) . . ?
O12 Mn3 O14 88.7(5) . . ?
O11 Mn3 N14 79.3(5) . . ?
O12 Mn3 N14 157.7(6) . . ?
O14 Mn3 N14 86.0(6) . . ?
O11 Mn3 N13 154.1(6) . . ?
O12 Mn3 N13 125.2(6) . . ?
O14 Mn3 N13 94.6(6) . . ?
N14 Mn3 N13 76.9(6) . . ?
O11 Mn3 N12 103.3(5) . . ?
O12 Mn3 N12 80.6(5) . . ?
O14 Mn3 N12 157.7(6) . . ?
N14 Mn3 N12 110.9(6) . . ?
N13 Mn3 N12 76.3(5) . . ?
O13 Mn4 N17 102.7(8) . . ?
O13 Mn4 O11 99.2(5) . . ?
N17 Mn4 O11 92.6(6) . . ?
O13 Mn4 N16 83.3(6) . . ?
N17 Mn4 N16 100.8(7) . . ?
O11 Mn4 N16 165.5(6) . . ?
O13 Mn4 O12 91.9(7) . . ?
N17 Mn4 O12 162.8(7) . . ?
O11 Mn4 O12 76.1(5) . . ?
N16 Mn4 O12 89.6(6) . . ?
O13 Mn4 N15 157.3(6) . . ?
N17 Mn4 N15 87.5(7) . . ?
O11 Mn4 N15 100.5(5) . . ?
N16 Mn4 N15 74.9(6) . . ?
O12 Mn4 N15 82.1(5) . . ?
C11 N3 C12 109.4(13) . . ?
C11 N3 C19 113.8(14) . . ?
C12 N3 C19 103.8(13) . . ?
C11 N3 Mn1 108.2(10) . . ?
C12 N3 Mn1 116.9(10) . . ?
C19 N3 Mn1 104.7(9) . . ?
C42 N12 C41 103.9(15) . . ?
C42 N12 C49 111.1(15) . . ?
C41 N12 C49 113.0(14) . . ?
C42 N12 Mn3 117.5(11) . . ?
C41 N12 Mn3 105.4(10) . . ?
C49 N12 Mn3 106.0(10) . . ?
C7 N5 C8 119.5(16) . . ?
C7 N5 Mn1 123.5(12) . . ?
C8 N5 Mn1 114.0(11) . . ?
C53 N14 C52 119.2(17) . . ?
C53 N14 Mn3 124.4(14) . . ?
C52 N14 Mn3 114.4(13) . . ?
C42 N15 C40 101.4(16) . . ?
C42 N15 C39 116.4(14) . . ?
C40 N15 C39 112.7(14) . . ?
C42 N15 Mn4 114.7(10) . . ?
C40 N15 Mn4 112.1(10) . . ?
C39 N15 Mn4 100.1(10) . . ?
C37 N16 C38 118.9(16) . . ?
C37 N16 Mn4 121.8(13) . . ?
C38 N16 Mn4 117.0(13) . . ?
O10 N9 O9 124.1(16) . . ?
O10 N9 C4 119.8(19) . . ?
O9 N9 C4 116.1(18) . . ?
O20 N20 O19 123.2(18) . . ?
O20 N20 C56 118.7(18) . . ?
O19 N20 C56 118.1(17) . . ?
C10 N4 C9 113.7(17) . . ?
C10 N4 Mn1 112.0(12) . . ?
C9 N4 Mn1 110.4(12) . . ?
C50 N13 C51 110.6(15) . . ?
C50 N13 Mn3 111.2(10) . . ?
C51 N13 Mn3 107.4(12) . . ?
O7 N10 O8 121(3) . . ?
O7 N10 C26 120(3) . . ?
O8 N10 C26 120(3) . . ?
O15 N22 O16 121(2) . . ?
O15 N22 C47 118(2) . . ?
O16 N22 C47 121(3) . . ?
O6 N11 O5 125(2) . . ?
O6 N11 C15 119(3) . . ?
O5 N11 C15 116(3) . . ?
O18 N21 O17 121(3) . . ?
O18 N21 C34 122(3) . . ?
O17 N21 C34 117(3) . . ?
C1 O1 Mn1 127.5(12) . . ?
C1 O1 Mn2 127.4(12) . . ?
Mn1 O1 Mn2 100.1(5) . . ?
C18 O2 Mn1 126.0(10) . . ?
C18 O2 Mn2 115.6(11) . . ?
Mn1 O2 Mn2 98.5(5) . . ?
C59 O11 Mn3 128.1(11) . . ?
C59 O11 Mn4 128.2(11) . . ?
Mn3 O11 Mn4 98.9(5) . . ?
C44 O12 Mn3 120.3(12) . . ?
C44 O12 Mn4 116.5(13) . . ?
Mn3 O12 Mn4 95.9(6) . . ?
C31 O13 Mn4 128.5(14) . . ?
C3 C4 C5 121.6(18) . . ?
C3 C4 N9 118.5(18) . . ?
C5 C4 N9 119.8(19) . . ?
C15 C14 C13 120(2) . . ?
C14 C15 C16 122(2) . . ?
C14 C15 N11 119(2) . . ?
C16 C15 N11 119(2) . . ?
C3 C2 C7 116.2(16) . . ?
C3 C2 C1 120.4(17) . . ?
C7 C2 C1 123.3(16) . . ?
C14 C13 C18 116.5(19) . . ?
C14 C13 C12 116.8(17) . . ?
C18 C13 C12 126.7(17) . . ?
C13 C12 N2 115.6(16) . . ?
C13 C12 N3 110.9(14) . . ?
N2 C12 N3 100.3(14) . . ?
N5 C7 C2 126.4(17) . . ?
O1 C1 C6 121.1(16) . . ?
O1 C1 C2 122.2(17) . . ?
C6 C1 C2 116.7(16) . . ?
C4 C3 C2 120.0(18) . . ?
N4 C10 C11 110.9(16) . . ?
C6 C5 C4 119.2(18) . . ?
C17 C16 C15 118(2) . . ?
C1 C6 C5 122.0(17) . . ?
C16 C17 C18 123(2) . . ?
N3 C11 C10 110.1(14) . . ?
N4 C9 C8 106.4(16) . . ?
N5 C8 C9 109.6(15) . . ?
O2 C18 C17 125.4(16) . . ?
O2 C18 C13 114.4(17) . . ?
C17 C18 C13 120.3(16) . . ?
C23 N1 C22 114.6(16) . . ?
C23 N1 Mn2 127.8(14) . . ?
C22 N1 Mn2 114.5(12) . . ?
N1 C23 C24 121.7(19) . . ?
C25 C24 C29 121(2) . . ?
C25 C24 C23 116(2) . . ?
C29 C24 C23 123(2) . . ?
C26 C25 C24 125(3) . . ?
C25 C26 C27 118(3) . . ?
C25 C26 N10 125(3) . . ?
C27 C26 N10 117(3) . . ?
O4 C29 C28 123(2) . . ?
O4 C29 C24 123(2) . . ?
C28 C29 C24 113(2) . . ?
C27 C28 C29 122(3) . . ?
C26 C27 C28 121(3) . . ?
C29 O4 Mn2 129.9(14) . . ?
C21 N2 C12 111.6(14) . . ?
C21 N2 C20 107.9(15) . . ?
C12 N2 C20 104.1(15) . . ?
C21 N2 Mn2 101.7(11) . . ?
C12 N2 Mn2 117.0(12) . . ?
C20 N2 Mn2 114.5(11) . . ?
N2 C20 C19 104.3(15) . . ?
N2 C21 C22 113.9(16) . . ?
N3 C19 C20 104.5(15) . . ?
C30 O3 Mn1 125.5(15) . . ?
N6 N7 N8 179(2) . . ?
N7 N6 Mn2 142.8(17) . . ?
C59 C54 C55 117.8(18) . . ?
C59 C54 C53 123.5(17) . . ?
C55 C54 C53 118.6(17) . . ?
C49 C50 N13 110.1(15) . . ?
C56 C55 C54 120.3(16) . . ?
O11 C59 C54 121.7(16) . . ?
O11 C59 C58 119.4(17) . . ?
C54 C59 C58 118.9(17) . . ?
N14 C53 C54 128.1(19) . . ?
C55 C56 C57 123.6(16) . . ?
C55 C56 N20 117.6(18) . . ?
C57 C56 N20 118.8(19) . . ?
C56 C57 C58 115.9(19) . . ?
C57 C58 C59 123.5(19) . . ?
N13 C51 C52 112.9(16) . . ?
N14 C52 C51 108.7(19) . . ?
C50 C49 N12 111.3(15) . . ?
N15 C39 C38 114.9(15) . . ?
N16 C37 C36 130.5(18) . . ?
C35 C36 C31 120(2) . . ?
C35 C36 C37 120.3(18) . . ?
C31 C36 C37 120(2) . . ?
N16 C38 C39 109.3(16) . . ?
C36 C35 C34 121(2) . . ?
C33 C32 C31 123(2) . . ?
C32 C33 C34 120(2) . . ?
O13 C31 C36 127(2) . . ?
O13 C31 C32 116(2) . . ?
C36 C31 C32 117(2) . . ?
C35 C34 C33 120(2) . . ?
C35 C34 N21 119(3) . . ?
C33 C34 N21 120(2) . . ?
N12 C41 C40 105.6(15) . . ?
N15 C40 C41 106.0(16) . . ?
N19 N18 N17 177(3) . . ?
N18 N17 Mn4 145.4(16) . . ?
C60 O14 Mn3 130.3(14) . . ?
N1 C22 C21 111.1(14) . . ?
O12 C44 C43 128(2) . . ?
O12 C44 C45 114.1(18) . . ?
C43 C44 C45 118(2) . . ?
C43 C48 C47 122(2) . . ?
C48 C43 C44 120(2) . . ?
C48 C43 C42 125.4(19) . . ?
C44 C43 C42 114.3(17) . . ?
C46 C45 C44 118(2) . . ?
C46 C47 C48 120.8(19) . . ?
C46 C47 N22 121(3) . . ?
C48 C47 N22 118(2) . . ?
C47 C46 C45 121(2) . . ?
N12 C42 N15 103.2(16) . . ?
N12 C42 C43 114.3(16) . . ?
N15 C42 C43 117.8(17) . . ?

_diffrn_measured_fraction_theta_max 0.804
_diffrn_reflns_theta_full        28.47
_diffrn_measured_fraction_theta_full 0.954
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.071
####################################################################### 
# 
# 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_skc-3g_0m
_database_code_depnum_ccdc_archive 'CCDC 1571834'
_audit_update_record             
;
2017-08-31 deposited with the CCDC.
2018-03-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H68 Cl N13 Ni4 O22'
_chemical_formula_weight         1569.54

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthohombic
_symmetry_space_group_name_H-M   Pbcn

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

_cell_length_a                   11.9710(3)
_cell_length_b                   17.2506(4)
_cell_length_c                   32.9419(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6802.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5724
_cell_measurement_theta_min      0.00
_cell_measurement_theta_max      0.00

_exptl_crystal_description       blocks
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3248
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            73688
_diffrn_reflns_av_R_equivalents  0.1034
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         1.24
_diffrn_reflns_theta_max         28.32
_reflns_number_total             8403
_reflns_number_gt                4479
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0983P)²+1.5518P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00002(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         8403
_refine_ls_number_parameters     454
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1331
_refine_ls_R_factor_gt           0.0618
_refine_ls_wR_factor_ref         0.1936
_refine_ls_wR_factor_gt          0.1550
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.101
_refine_ls_shift/su_mean         0.005

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.28336(5) 0.05954(4) 0.156257(17) 0.0491(2) Uani 1 1 d . . .
Ni2 Ni 0.36982(4) -0.01248(3) 0.076862(16) 0.04312(18) Uani 1 1 d . . .
C6 C 0.5000(4) -0.1573(3) 0.06806(18) 0.0631(14) Uani 1 1 d . . .
C15 C 0.1772(5) 0.1165(5) 0.22885(17) 0.092(2) Uani 1 1 d . . .
H15A H 0.2161 0.0835 0.2481 0.110 Uiso 1 1 calc R . .
H15B H 0.1118 0.1375 0.2423 0.110 Uiso 1 1 calc R . .
C13 C 0.6184(4) 0.0692(4) 0.11427(16) 0.0683(15) Uani 1 1 d . . .
H13 H 0.6163 0.0300 0.0949 0.082 Uiso 1 1 calc R . .
C5 C 0.4444(4) -0.1772(3) 0.03145(17) 0.0589(13) Uani 1 1 d . . .
C7 C 0.3507(4) -0.1349(3) 0.01518(16) 0.0586(13) Uani 1 1 d . . .
H7 H 0.3213 -0.1526 -0.0093 0.070 Uiso 1 1 calc R . .
C9 C 0.5264(4) 0.1531(3) 0.16247(15) 0.0582(12) Uani 1 1 d . . .
C1 C 0.5952(5) -0.2017(3) 0.07845(19) 0.0783(17) Uani 1 1 d . . .
H1 H 0.6340 -0.1899 0.1021 0.094 Uiso 1 1 calc R . .
C14 C 0.2525(5) 0.1817(4) 0.21655(19) 0.092(2) Uani 1 1 d . . .
H14A H 0.2091 0.2227 0.2040 0.111 Uiso 1 1 calc R . .
H14B H 0.2897 0.2029 0.2402 0.111 Uiso 1 1 calc R . .
C16 C 0.0478(4) 0.1004(4) 0.16986(16) 0.0753(16) Uani 1 1 d . . .
H16A H -0.0038 0.1268 0.1879 0.090 Uiso 1 1 calc R . .
H16B H 0.0080 0.0580 0.1569 0.090 Uiso 1 1 calc R . .
C11 C 0.7272(5) 0.1626(4) 0.15163(19) 0.0865(19) Uani 1 1 d . . .
H11 H 0.7955 0.1860 0.1572 0.104 Uiso 1 1 calc R . .
C10 C 0.6311(5) 0.1869(4) 0.17047(17) 0.0749(16) Uani 1 1 d . . .
H10 H 0.6353 0.2272 0.1892 0.090 Uiso 1 1 calc R . .
C4 C 0.4839(5) -0.2403(3) 0.00804(19) 0.0741(16) Uani 1 1 d . . .
H4 H 0.4461 -0.2543 -0.0155 0.089 Uiso 1 1 calc R . .
C17 C 0.0886(5) 0.1567(3) 0.13761(16) 0.0712(15) Uani 1 1 d . . .
H17A H 0.0276 0.1683 0.1192 0.085 Uiso 1 1 calc R . .
H17B H 0.1109 0.2047 0.1506 0.085 Uiso 1 1 calc R . .
C8 C 0.4336(5) 0.1793(3) 0.18750(16) 0.0688(14) Uani 1 1 d . . .
H8 H 0.4476 0.2202 0.2052 0.083 Uiso 1 1 calc R . .
C12 C 0.7196(4) 0.1025(4) 0.12420(19) 0.0834(19) Uani 1 1 d . . .
H12 H 0.7844 0.0839 0.1121 0.100 Uiso 1 1 calc R . .
C3 C 0.5773(6) -0.2814(3) 0.0195(3) 0.093(2) Uani 1 1 d . . .
H3 H 0.6031 -0.3222 0.0037 0.112 Uiso 1 1 calc R . .
C2 C 0.6317(6) -0.2615(4) 0.0546(2) 0.095(2) Uani 1 1 d . . .
H2 H 0.6948 -0.2892 0.0624 0.113 Uiso 1 1 calc R . .
N2 N 0.3043(3) -0.0756(2) 0.03097(12) 0.0494(9) Uani 1 1 d . . .
N1 N 0.3360(3) 0.1517(3) 0.18753(12) 0.0634(11) Uani 1 1 d . . .
O1 O 0.4692(3) -0.1014(2) 0.09257(11) 0.0653(9) Uani 1 1 d . . .
N3 N 0.1412(4) 0.0693(3) 0.19351(13) 0.0670(12) Uani 1 1 d . . .
N4 N 0.1847(3) 0.1259(2) 0.11373(11) 0.0485(9) Uani 1 1 d . . .
C18 C 0.2174(4) -0.0357(3) 0.00779(15) 0.0593(13) Uani 1 1 d . . .
H18A H 0.1444 -0.0501 0.0181 0.071 Uiso 1 1 calc R . .
H18B H 0.2216 -0.0509 -0.0205 0.071 Uiso 1 1 calc R . .
C19 C 0.2331(4) 0.0518(3) 0.01146(13) 0.0535(12) Uani 1 1 d . . .
H19A H 0.2963 0.0678 -0.0050 0.064 Uiso 1 1 calc R . .
H19B H 0.1671 0.0780 0.0013 0.064 Uiso 1 1 calc R . .
O3 O 0.4234(2) 0.06030(18) 0.12248(9) 0.0498(7) Uani 1 1 d . . .
O2 O 0.2548(2) -0.03801(18) 0.12255(9) 0.0474(7) Uani 1 1 d . . .
C20 C 0.5187(4) 0.0932(3) 0.13268(13) 0.0515(11) Uani 1 1 d . . .
C22 C 0.2979(4) 0.1546(3) 0.05587(15) 0.0550(12) Uani 1 1 d . . .
H22A H 0.2739 0.1841 0.0324 0.066 Uiso 1 1 calc R . .
H22B H 0.3789 0.1537 0.0566 0.066 Uiso 1 1 calc R . .
C21 C 0.2510(4) 0.1900(3) 0.09490(16) 0.0617(13) Uani 1 1 d . . .
H21A H 0.3109 0.2065 0.1128 0.074 Uiso 1 1 calc R . .
H21B H 0.2038 0.2343 0.0889 0.074 Uiso 1 1 calc R . .
C25 C -0.0179(4) -0.0083(3) 0.07643(15) 0.0619(13) Uani 1 1 d . . .
H25 H -0.0562 0.0292 0.0617 0.074 Uiso 1 1 calc R . .
C24 C 0.0917(4) 0.0056(3) 0.08810(14) 0.0496(11) Uani 1 1 d . . .
C23 C 0.1495(4) -0.0511(3) 0.11047(13) 0.0468(11) Uani 1 1 d . . .
C26 C 0.0949(5) -0.1194(3) 0.11975(17) 0.0680(14) Uani 1 1 d . . .
H26 H 0.1317 -0.1576 0.1345 0.082 Uiso 1 1 calc R . .
C27 C -0.0141(5) -0.1316(4) 0.10726(19) 0.0808(18) Uani 1 1 d . . .
H27 H -0.0489 -0.1784 0.1134 0.097 Uiso 1 1 calc R . .
N5 N 0.2526(3) 0.0746(2) 0.05433(10) 0.0426(8) Uani 1 1 d . . .
C28 C 0.1471(3) 0.0812(3) 0.07806(13) 0.0447(10) Uani 1 1 d . . .
H28 H 0.0943 0.1131 0.0626 0.054 Uiso 1 1 calc R . .
C29 C -0.0712(5) -0.0768(4) 0.08617(18) 0.0781(17) Uani 1 1 d . . .
H29 H -0.1449 -0.0853 0.0784 0.094 Uiso 1 1 calc R . .
O4 O 0.3602(4) -0.0153(3) 0.20079(12) 0.0877(13) Uani 1 1 d . . .
H4A H 0.3851 -0.0540 0.1895 0.132 Uiso 1 1 calc R . .
N8 N 0.5000 0.0000 0.0000 0.0479(12) Uani 1 2 d S . .
N9 N 0.4901(3) 0.0266(2) 0.03279(13) 0.0586(10) Uani 1 1 d . . .
Cl1 Cl 0.5000 0.3957(3) 0.2500 0.271(5) Uani 1 2 d S . .
O6 O 0.0561(10) 0.2821(5) 0.2817(3) 0.260(5) Uani 1 1 d . . .
O5 O 0.463(5) 0.3389(10) 0.2562(13) 0.67(4) Uani 1 1 d . . .
O9 O 0.353(4) 0.973(3) 0.2879(10) 1.15(7) Uani 1 1 d . . .
H4B H 0.437(4) 0.001(3) 0.2248(17) 0.074(15) Uiso 1 1 d . . .
O10 O 0.531(3) 0.4570(7) 0.2303(5) 0.393(17) Uani 1 1 d . . .
O7 O 0.3909(14) 0.8443(5) 0.1670(3) 0.257(5) Uani 1 1 d . . .
O8 O 0.5420(14) 0.8998(10) 0.1688(3) 0.321(8) Uani 1 1 d . . .
O11 O 0.630(5) 0.3858(11) 0.2735(10) 0.73(4) Uani 1 1 d . . .
H3N H 0.105(4) 0.022(3) 0.2045(17) 0.070(17) 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
Ni1 N1 1.996(4) . ?
Ni1 O3 2.012(3) . ?
Ni1 O2 2.045(3) . ?
Ni1 N3 2.105(4) . ?
Ni1 O4 2.160(4) . ?
Ni1 N4 2.161(4) . ?
Ni2 O1 2.008(3) . ?
Ni2 N2 2.022(4) . ?
Ni2 O3 2.060(3) . ?
Ni2 O2 2.087(3) . ?
Ni2 N9 2.153(4) . ?
Ni2 N5 2.185(4) . ?
C6 O1 1.311(6) . ?
C6 C1 1.415(7) . ?
C6 C5 1.420(8) . ?
C15 N3 1.485(7) . ?
C15 C14 1.497(9) . ?
C13 C12 1.380(7) . ?
C13 C20 1.401(6) . ?
C5 C4 1.416(7) . ?
C5 C7 1.441(7) . ?
C7 N2 1.275(6) . ?
C9 C10 1.408(7) . ?
C9 C20 1.428(7) . ?
C9 C8 1.455(7) . ?
C1 C2 1.368(9) . ?
C14 N1 1.477(6) . ?
C16 N3 1.464(7) . ?
C16 C17 1.520(8) . ?
C11 C10 1.373(8) . ?
C11 C12 1.378(9) . ?
C4 C3 1.377(8) . ?
C17 N4 1.490(6) . ?
C8 N1 1.262(7) . ?
C3 C2 1.371(10) . ?
N2 C18 1.462(6) . ?
N4 C28 1.476(5) . ?
N4 C21 1.496(6) . ?
C18 C19 1.526(7) . ?
C19 N5 1.484(5) . ?
O3 C20 1.318(5) . ?
O2 C23 1.341(5) . ?
C22 N5 1.483(6) . ?
C22 C21 1.531(7) . ?
C25 C29 1.381(7) . ?
C25 C24 1.387(6) . ?
C24 C23 1.406(6) . ?
C24 C28 1.501(6) . ?
C23 C26 1.382(6) . ?
C26 C27 1.384(7) . ?
C27 C29 1.358(8) . ?
N5 C28 1.490(5) . ?
N8 N9 1.179(4) . ?
N8 N9 1.179(4) 5_655 ?
Cl1 O5 1.09(2) . ?
Cl1 O5 1.09(2) 3_655 ?
Cl1 O10 1.294(16) 3_655 ?
Cl1 O10 1.294(16) . ?
Cl1 O11 1.74(4) 3_655 ?
Cl1 O11 1.74(4) . ?
O5 O5 0.98(11) 3_655 ?
O5 O11 1.68(6) 3_655 ?
O10 O10 1.49(4) 3_655 ?
O11 O5 1.68(6) 3_655 ?

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
N1 Ni1 O3 91.00(15) . . ?
N1 Ni1 O2 171.24(14) . . ?
O3 Ni1 O2 81.05(12) . . ?
N1 Ni1 N3 83.74(19) . . ?
O3 Ni1 N3 174.60(18) . . ?
O2 Ni1 N3 104.28(17) . . ?
N1 Ni1 O4 89.50(18) . . ?
O3 Ni1 O4 91.43(15) . . ?
O2 Ni1 O4 87.04(15) . . ?
N3 Ni1 O4 89.76(17) . . ?
N1 Ni1 N4 94.87(16) . . ?
O3 Ni1 N4 95.37(13) . . ?
O2 Ni1 N4 89.57(13) . . ?
N3 Ni1 N4 83.89(15) . . ?
O4 Ni1 N4 171.85(17) . . ?
O1 Ni2 N2 90.63(15) . . ?
O1 Ni2 O3 95.35(13) . . ?
N2 Ni2 O3 173.92(14) . . ?
O1 Ni2 O2 92.51(13) . . ?
N2 Ni2 O2 99.75(14) . . ?
O3 Ni2 O2 78.93(12) . . ?
O1 Ni2 N9 90.94(16) . . ?
N2 Ni2 N9 85.63(15) . . ?
O3 Ni2 N9 95.34(14) . . ?
O2 Ni2 N9 173.57(14) . . ?
O1 Ni2 N5 172.96(14) . . ?
N2 Ni2 N5 82.35(14) . . ?
O3 Ni2 N5 91.65(13) . . ?
O2 Ni2 N5 88.07(12) . . ?
N9 Ni2 N5 89.17(15) . . ?
O1 C6 C1 118.5(5) . . ?
O1 C6 C5 124.7(5) . . ?
C1 C6 C5 116.9(5) . . ?
N3 C15 C14 112.0(5) . . ?
C12 C13 C20 121.5(5) . . ?
C4 C5 C6 119.5(5) . . ?
C4 C5 C7 116.5(5) . . ?
C6 C5 C7 123.9(4) . . ?
N2 C7 C5 126.4(5) . . ?
C10 C9 C20 119.0(5) . . ?
C10 C9 C8 116.4(5) . . ?
C20 C9 C8 124.4(4) . . ?
C2 C1 C6 121.8(6) . . ?
N1 C14 C15 108.6(5) . . ?
N3 C16 C17 111.1(4) . . ?
C10 C11 C12 118.1(5) . . ?
C11 C10 C9 122.4(6) . . ?
C3 C4 C5 121.1(6) . . ?
N4 C17 C16 112.9(4) . . ?
N1 C8 C9 126.2(5) . . ?
C11 C12 C13 121.8(5) . . ?
C2 C3 C4 119.3(6) . . ?
C1 C2 C3 121.4(6) . . ?
C7 N2 C18 118.4(4) . . ?
C7 N2 Ni2 124.6(3) . . ?
C18 N2 Ni2 114.4(3) . . ?
C8 N1 C14 119.7(5) . . ?
C8 N1 Ni1 126.3(4) . . ?
C14 N1 Ni1 113.6(4) . . ?
C6 O1 Ni2 124.7(3) . . ?
C16 N3 C15 116.0(5) . . ?
C16 N3 Ni1 109.6(3) . . ?
C15 N3 Ni1 105.4(3) . . ?
C28 N4 C17 111.8(4) . . ?
C28 N4 C21 102.6(3) . . ?
C17 N4 C21 111.4(4) . . ?
C28 N4 Ni1 114.0(3) . . ?
C17 N4 Ni1 105.6(3) . . ?
C21 N4 Ni1 111.7(3) . . ?
N2 C18 C19 109.7(4) . . ?
N5 C19 C18 110.9(4) . . ?
C20 O3 Ni1 125.7(3) . . ?
C20 O3 Ni2 135.9(3) . . ?
Ni1 O3 Ni2 98.06(12) . . ?
C23 O2 Ni1 117.2(3) . . ?
C23 O2 Ni2 116.2(3) . . ?
Ni1 O2 Ni2 96.17(13) . . ?
O3 C20 C13 120.0(4) . . ?
O3 C20 C9 122.8(4) . . ?
C13 C20 C9 117.2(4) . . ?
N5 C22 C21 105.5(4) . . ?
N4 C21 C22 104.3(4) . . ?
C29 C25 C24 121.4(5) . . ?
C25 C24 C23 119.3(4) . . ?
C25 C24 C28 120.5(4) . . ?
C23 C24 C28 120.1(4) . . ?
O2 C23 C26 121.5(4) . . ?
O2 C23 C24 120.1(4) . . ?
C26 C23 C24 118.4(4) . . ?
C23 C26 C27 120.7(5) . . ?
C29 C27 C26 121.4(5) . . ?
C19 N5 C22 109.6(3) . . ?
C19 N5 C28 112.7(3) . . ?
C22 N5 C28 102.7(3) . . ?
C19 N5 Ni2 104.0(3) . . ?
C22 N5 Ni2 113.1(3) . . ?
C28 N5 Ni2 114.8(2) . . ?
N4 C28 N5 101.5(3) . . ?
N4 C28 C24 114.4(4) . . ?
N5 C28 C24 115.0(4) . . ?
C27 C29 C25 118.8(5) . . ?
N9 N8 N9 180.0(6) . 5_655 ?
N8 N9 Ni2 124.3(3) . . ?
O5 Cl1 O5 53(5) . 3_655 ?
O5 Cl1 O10 121(3) . 3_655 ?
O5 Cl1 O10 160(3) 3_655 3_655 ?
O5 Cl1 O10 160(3) . . ?
O5 Cl1 O10 121(3) 3_655 . ?
O10 Cl1 O10 70.4(17) 3_655 . ?
O5 Cl1 O11 68(3) . 3_655 ?
O5 Cl1 O11 101(3) 3_655 3_655 ?
O10 Cl1 O11 92.9(18) 3_655 3_655 ?
O10 Cl1 O11 96.3(17) . 3_655 ?
O5 Cl1 O11 101(3) . . ?
O5 Cl1 O11 68(3) 3_655 . ?
O10 Cl1 O11 96.3(17) 3_655 . ?
O10 Cl1 O11 92.9(18) . . ?
O11 Cl1 O11 168.7(13) 3_655 . ?
O5 O5 Cl1 63(3) 3_655 . ?
O5 O5 O11 111(5) 3_655 3_655 ?
Cl1 O5 O11 74(2) . 3_655 ?
Cl1 O10 O10 54.8(8) . 3_655 ?
O5 O11 Cl1 37.2(15) 3_655 . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.32
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.086
####################################################################### 
# 
# 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_SKC-27G_0m
_database_code_depnum_ccdc_archive 'CCDC 1571836'
_audit_update_record             
;
2017-08-31 deposited with the CCDC.
2018-03-07 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            'C33 H38 Mn2 N9 O13'
_chemical_formula_weight         878.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   10.5528(4)
_cell_length_b                   10.6347(4)
_cell_length_c                   18.9784(6)
_cell_angle_alpha                86.4580(10)
_cell_angle_beta                 76.2350(10)
_cell_angle_gamma                63.5880(10)
_cell_volume                     1850.39(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4726
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      24.99

_exptl_crystal_description       plates
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_F_000             906
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    0.761
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17269
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.141
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             6365
_reflns_number_gt                4726
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0867P)²] 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         6365
_refine_ls_number_parameters     521
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1527
_refine_ls_wR_factor_gt          0.1413
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_restrained_S_all      1.264
_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
Mn1 Mn 0.29830(5) 0.21287(5) 0.27359(2) 0.04850(18) Uani 1 1 d . . . . .
Mn2 Mn 0.31269(5) -0.10540(5) 0.27500(3) 0.05470(19) Uani 1 1 d . . . . .
O1 O 0.3845(2) 0.0212(2) 0.32783(12) 0.0544(6) Uani 1 1 d . . . . .
O2 O 0.3236(2) 0.0619(2) 0.19608(11) 0.0543(6) Uani 1 1 d . . . . .
N2 N 0.0580(3) 0.0463(3) 0.29431(13) 0.0486(6) Uani 1 1 d . . . . .
N5 N 0.3286(3) 0.2933(3) 0.37162(15) 0.0553(7) Uani 1 1 d . . . . .
N1 N 0.2359(3) -0.1883(3) 0.19717(14) 0.0564(7) Uani 1 1 d . . . . .
N7 N 0.8416(3) -0.1748(4) 0.46672(14) 0.0638(8) Uani 1 1 d . . . . .
N4 N 0.1843(3) 0.4524(3) 0.26793(16) 0.0553(7) Uani 1 1 d . . . . .
O4 O 0.5152(3) -0.2642(3) 0.22260(15) 0.0935(10) Uani 1 1 d . . . . .
O7 O 0.9118(3) -0.3032(4) 0.46878(16) 0.0893(9) Uani 1 1 d . . . . .
O6 O 0.8671(4) -0.0890(4) 0.49298(18) 0.0957(10) Uani 1 1 d . . . . .
N8 N -0.0079(5) 0.1801(4) -0.0083(2) 0.0863(11) Uani 1 1 d . . . . .
O8 O -0.1402(4) 0.2283(4) 0.01240(19) 0.1123(12) Uani 1 1 d . . . . .
N9 N 0.7404(6) -0.4481(4) -0.0668(2) 0.0923(12) Uani 1 1 d . . . . .
O9 O 0.0552(4) 0.1567(5) -0.07242(18) 0.1289(15) Uani 1 1 d . . . . .
O11 O 0.6603(5) -0.4454(4) -0.10434(18) 0.1160(13) Uani 1 1 d . . . . .
O10 O 0.8719(5) -0.4920(4) -0.0922(2) 0.1259(14) Uani 1 1 d . . . . .
N3 N 0.0470(3) 0.2673(3) 0.28708(12) 0.0461(6) Uani 1 1 d . . . . .
C18 C 0.6330(3) 0.0202(4) 0.43279(15) 0.0486(8) Uani 1 1 d . . . . .
H18 H 0.6520 0.0817 0.4564 0.058 Uiso 1 1 calc R U . . .
C17 C 0.5172(3) 0.0735(3) 0.39875(15) 0.0455(7) Uani 1 1 d . . . . .
C19 C 0.7193(3) -0.1219(4) 0.43190(15) 0.0510(8) Uani 1 1 d . . . . .
C22 C 0.4892(3) -0.0219(3) 0.36241(16) 0.0479(8) Uani 1 1 d . . . . .
C29 C 0.0092(4) 0.1767(4) 0.11841(17) 0.0561(8) Uani 1 1 d . . . . .
H29 H -0.0917 0.2132 0.1328 0.067 Uiso 1 1 calc R U . . .
C24 C 0.0907(3) 0.1469(3) 0.16975(16) 0.0492(8) Uani 1 1 d . . . . .
C23 C 0.0150(3) 0.1711(3) 0.24939(16) 0.0493(8) Uani 1 1 d . . . . .
H23 H -0.0903 0.2122 0.2539 0.059 Uiso 1 1 calc R U . . .
C16 C 0.4288(4) 0.2238(4) 0.40452(17) 0.0531(8) Uani 1 1 d . . . . .
H16 H 0.4470 0.2750 0.4355 0.064 Uiso 1 1 calc R U . . .
C7 C 0.3131(4) -0.2447(4) 0.13401(19) 0.0615(9) Uani 1 1 d . . . . .
H7 H 0.2635 -0.2517 0.1011 0.074 Uiso 1 1 calc R U . . .
C13 C 0.0256(4) 0.5070(4) 0.29150(19) 0.0570(8) Uani 1 1 d . . . . .
H13A H -0.0207 0.6005 0.2741 0.068 Uiso 1 1 calc R U . . .
H13B H -0.0034 0.5139 0.3441 0.068 Uiso 1 1 calc R U . . .
C6 C 0.4692(4) -0.2984(4) 0.10881(18) 0.0611(9) Uani 1 1 d . . . . .
C20 C 0.6901(4) -0.2161(4) 0.39894(18) 0.0631(10) Uani 1 1 d . . . . .
H20 H 0.7463 -0.3123 0.4005 0.076 Uiso 1 1 calc R U . . .
C26 C 0.3078(4) 0.0752(4) 0.07313(17) 0.0635(10) Uani 1 1 d . . . . .
H26 H 0.4081 0.0425 0.0576 0.076 Uiso 1 1 calc R U . . .
C25 C 0.2444(4) 0.0939(4) 0.14779(16) 0.0516(8) Uani 1 1 d . . . . .
C28 C 0.0788(4) 0.1520(4) 0.04520(18) 0.0629(10) Uani 1 1 d . . . . .
C12 C -0.0241(4) 0.4127(4) 0.26291(19) 0.0564(8) Uani 1 1 d . . . . .
H12A H -0.1289 0.4496 0.2799 0.068 Uiso 1 1 calc R U . . .
H12B H -0.0010 0.4111 0.2103 0.068 Uiso 1 1 calc R U . . .
C10 C -0.0090(4) 0.1111(4) 0.36926(17) 0.0580(9) Uani 1 1 d . . . . .
H10A H 0.0466 0.0530 0.4029 0.070 Uiso 1 1 calc R U . . .
H10B H -0.1081 0.1223 0.3850 0.070 Uiso 1 1 calc R U . . .
C8 C 0.0779(4) -0.1380(4) 0.21066(19) 0.0606(9) Uani 1 1 d . . . . .
H8A H 0.0560 -0.2176 0.2114 0.073 Uiso 1 1 calc R U . . .
H8B H 0.0423 -0.0797 0.1717 0.073 Uiso 1 1 calc R U . . .
C21 C 0.5790(4) -0.1672(4) 0.3643(2) 0.0643(10) Uani 1 1 d . . . . .
H21 H 0.5620 -0.2310 0.3414 0.077 Uiso 1 1 calc R U . . .
C11 C -0.0070(4) 0.2524(4) 0.36577(17) 0.0574(9) Uani 1 1 d . . . . .
H11A H -0.1039 0.3271 0.3844 0.069 Uiso 1 1 calc R U . . .
H11B H 0.0576 0.2552 0.3938 0.069 Uiso 1 1 calc R U . . .
C5 C 0.5319(5) -0.3474(4) 0.03634(19) 0.0692(10) Uani 1 1 d . . . . .
H5 H 0.4725 -0.3437 0.0063 0.083 Uiso 1 1 calc R U . . .
C1 C 0.5641(4) -0.3044(4) 0.1545(2) 0.0717(11) Uani 1 1 d . . . . .
C9 C 0.0022(4) -0.0541(4) 0.28217(19) 0.0602(9) Uani 1 1 d . . . . .
H9A H -0.1010 -0.0023 0.2841 0.072 Uiso 1 1 calc R U . . .
H9B H 0.0134 -0.1185 0.3213 0.072 Uiso 1 1 calc R U . . .
C27 C 0.2280(5) 0.1032(4) 0.02242(18) 0.0689(10) Uani 1 1 d . . . . .
H27 H 0.2731 0.0897 -0.0268 0.083 Uiso 1 1 calc R U . . .
C14 C 0.2417(5) 0.5162(4) 0.3120(2) 0.0699(10) Uani 1 1 d . . . . .
H14A H 0.1786 0.6163 0.3201 0.084 Uiso 1 1 calc R U . . .
H14B H 0.3380 0.5034 0.2860 0.084 Uiso 1 1 calc R U . . .
C15 C 0.2495(5) 0.4465(4) 0.3852(2) 0.0738(11) Uani 1 1 d . . . . .
H15A H 0.2994 0.4784 0.4112 0.089 Uiso 1 1 calc R U . . .
H15B H 0.1520 0.4721 0.4146 0.089 Uiso 1 1 calc R U . . .
C4 C 0.6806(5) -0.4014(4) 0.0084(2) 0.0732(11) Uani 1 1 d . . . . .
C2 C 0.7129(5) -0.3605(5) 0.1230(2) 0.0887(14) Uani 1 1 d . . . . .
H2 H 0.7752 -0.3662 0.1518 0.106 Uiso 1 1 calc R U . . .
C3 C 0.7713(5) -0.4073(5) 0.0519(2) 0.0869(13) Uani 1 1 d . . . . .
H3 H 0.8711 -0.4429 0.0329 0.104 Uiso 1 1 calc R U . . .
N6 N 0.2723(4) -0.2060(3) 0.37234(18) 0.0714(9) Uani 1 1 d . . . . .
C30 C 0.2882(5) -0.2415(4) 0.4290(2) 0.0679(10) Uani 1 1 d . . . . .
O5 O 0.3101(5) -0.2825(4) 0.4877(2) 0.1270(14) Uani 1 1 d . . . . .
O3 O 0.5114(3) 0.1984(4) 0.21747(18) 0.1076(11) Uani 1 1 d . . . . .
C31 C 0.6267(7) 0.0823(12) 0.1720(4) 0.223(5) Uani 1 1 d . . . . .
H31A H 0.7129 0.0492 0.1903 0.335 Uiso 1 1 calc R U . . .
H31B H 0.6459 0.1118 0.1234 0.335 Uiso 1 1 calc R U . . .
H31C H 0.5988 0.0078 0.1718 0.335 Uiso 1 1 calc R U . . .
O12 O 0.3959(7) 0.5331(8) 0.5912(5) 0.236(4) Uani 1 1 d . . . . .
C32 C 0.6149(8) 0.3835(13) 0.2652(5) 0.181(4) Uani 1 1 d . . . . .
H32A H 0.5238 0.3804 0.2880 0.217 Uiso 1 1 calc R U . . .
H32B H 0.6903 0.3002 0.2798 0.217 Uiso 1 1 calc R U . . .
O13 O 0.6115(14) 0.4943(11) 0.3012(11) 0.349(8) Uani 1 1 d . . . . .
H13 H 0.5918 0.5624 0.2757 0.523 Uiso 1 1 calc R U . . .
C33 C 0.6364(10) 0.3561(13) 0.1832(7) 0.226(5) Uani 1 1 d . . . . .
H33A H 0.6778 0.4135 0.1559 0.339 Uiso 1 1 calc R U . . .
H33B H 0.5441 0.3791 0.1729 0.339 Uiso 1 1 calc R U . . .
H33C H 0.7008 0.2588 0.1699 0.339 Uiso 1 1 calc R U . . .
H4N H 0.203(3) 0.480(3) 0.2226(18) 0.047(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 O2 2.130(2) . ?
Mn1 O1 2.140(2) . ?
Mn1 O3 2.188(3) . ?
Mn1 N5 2.240(3) . ?
Mn1 N4 2.291(3) . ?
Mn1 N3 2.401(2) . ?
Mn2 O4 2.096(3) . ?
Mn2 N6 2.128(3) . ?
Mn2 O1 2.198(2) . ?
Mn2 N1 2.232(2) . ?
Mn2 O2 2.279(2) . ?
Mn2 N2 2.389(3) . ?
O1 C22 1.311(3) . ?
O2 C25 1.314(4) . ?
N2 C9 1.481(4) . ?
N2 C23 1.484(4) . ?
N2 C10 1.486(4) . ?
N5 C16 1.271(4) . ?
N5 C15 1.469(5) . ?
N1 C7 1.284(4) . ?
N1 C8 1.467(4) . ?
N7 O6 1.221(4) . ?
N7 O7 1.234(4) . ?
N7 C19 1.461(4) . ?
N4 C13 1.468(4) . ?
N4 C14 1.484(4) . ?
N4 H4N 0.90(3) . ?
O4 C1 1.294(4) . ?
N8 O9 1.221(5) . ?
N8 O8 1.222(5) . ?
N8 C28 1.456(4) . ?
N9 O11 1.219(6) . ?
N9 O10 1.228(6) . ?
N9 C4 1.436(5) . ?
N3 C23 1.478(4) . ?
N3 C12 1.486(4) . ?
N3 C11 1.492(4) . ?
C18 C19 1.373(5) . ?
C18 C17 1.395(4) . ?
C18 H18 0.9300 . ?
C17 C22 1.429(4) . ?
C17 C16 1.443(5) . ?
C19 C20 1.389(5) . ?
C22 C21 1.412(5) . ?
C29 C24 1.381(4) . ?
C29 C28 1.388(5) . ?
C29 H29 0.9300 . ?
C24 C25 1.420(5) . ?
C24 C23 1.510(4) . ?
C23 H23 0.9800 . ?
C16 H16 0.9300 . ?
C7 C6 1.446(5) . ?
C7 H7 0.9300 . ?
C13 C12 1.498(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C6 C5 1.396(5) . ?
C6 C1 1.451(5) . ?
C20 C21 1.363(5) . ?
C20 H20 0.9300 . ?
C26 C27 1.361(5) . ?
C26 C25 1.400(4) . ?
C26 H26 0.9300 . ?
C28 C27 1.383(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C10 C11 1.510(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C8 C9 1.509(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C21 H21 0.9300 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C5 C4 1.383(6) . ?
C5 H5 0.9300 . ?
C1 C2 1.394(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C27 H27 0.9300 . ?
C14 C15 1.536(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C4 C3 1.385(6) . ?
C2 C3 1.366(6) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
N6 C30 1.142(5) . ?
C30 O5 1.208(5) . ?
O3 C31 1.430(8) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 O13 1.380(13) . ?
C32 C33 1.546(13) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
O13 H13 0.8402 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mn1 O1 78.10(8) . . ?
O2 Mn1 O3 89.33(12) . . ?
O1 Mn1 O3 94.81(12) . . ?
O2 Mn1 N5 157.47(10) . . ?
O1 Mn1 N5 80.14(9) . . ?
O3 Mn1 N5 86.72(12) . . ?
O2 Mn1 N4 126.45(10) . . ?
O1 Mn1 N4 154.31(9) . . ?
O3 Mn1 N4 93.09(13) . . ?
N5 Mn1 N4 75.96(10) . . ?
O2 Mn1 N3 80.83(8) . . ?
O1 Mn1 N3 104.44(9) . . ?
O3 Mn1 N3 155.94(11) . . ?
N5 Mn1 N3 110.43(9) . . ?
N4 Mn1 N3 75.76(9) . . ?
O4 Mn2 N6 99.36(14) . . ?
O4 Mn2 O1 99.95(10) . . ?
N6 Mn2 O1 92.58(10) . . ?
O4 Mn2 N1 82.07(10) . . ?
N6 Mn2 N1 103.34(11) . . ?
O1 Mn2 N1 163.46(10) . . ?
O4 Mn2 O2 94.86(11) . . ?
N6 Mn2 O2 161.88(11) . . ?
O1 Mn2 O2 73.85(8) . . ?
N1 Mn2 O2 89.64(9) . . ?
O4 Mn2 N2 156.58(9) . . ?
N6 Mn2 N2 89.86(11) . . ?
O1 Mn2 N2 101.09(8) . . ?
N1 Mn2 N2 74.85(9) . . ?
O2 Mn2 N2 81.28(8) . . ?
C22 O1 Mn1 128.0(2) . . ?
C22 O1 Mn2 128.5(2) . . ?
Mn1 O1 Mn2 99.83(8) . . ?
C25 O2 Mn1 122.6(2) . . ?
C25 O2 Mn2 117.4(2) . . ?
Mn1 O2 Mn2 97.60(8) . . ?
C9 N2 C23 114.3(2) . . ?
C9 N2 C10 110.1(2) . . ?
C23 N2 C10 102.1(2) . . ?
C9 N2 Mn2 101.1(2) . . ?
C23 N2 Mn2 116.56(18) . . ?
C10 N2 Mn2 113.02(19) . . ?
C16 N5 C15 118.6(3) . . ?
C16 N5 Mn1 124.9(2) . . ?
C15 N5 Mn1 114.6(2) . . ?
C7 N1 C8 117.5(3) . . ?
C7 N1 Mn2 123.9(2) . . ?
C8 N1 Mn2 116.02(19) . . ?
O6 N7 O7 123.8(3) . . ?
O6 N7 C19 118.0(3) . . ?
O7 N7 C19 118.2(3) . . ?
C13 N4 C14 112.0(3) . . ?
C13 N4 Mn1 111.2(2) . . ?
C14 N4 Mn1 109.0(2) . . ?
C13 N4 H4N 107(2) . . ?
C14 N4 H4N 106(2) . . ?
Mn1 N4 H4N 112(2) . . ?
C1 O4 Mn2 128.7(2) . . ?
O9 N8 O8 122.8(3) . . ?
O9 N8 C28 118.2(4) . . ?
O8 N8 C28 119.1(4) . . ?
O11 N9 O10 120.8(4) . . ?
O11 N9 C4 119.6(5) . . ?
O10 N9 C4 119.6(5) . . ?
C23 N3 C12 110.4(2) . . ?
C23 N3 C11 104.2(2) . . ?
C12 N3 C11 113.9(3) . . ?
C23 N3 Mn1 117.31(18) . . ?
C12 N3 Mn1 106.31(18) . . ?
C11 N3 Mn1 104.83(18) . . ?
C19 C18 C17 120.9(3) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.5 . . ?
C18 C17 C22 119.1(3) . . ?
C18 C17 C16 117.3(3) . . ?
C22 C17 C16 123.5(3) . . ?
C18 C19 C20 120.6(3) . . ?
C18 C19 N7 119.7(3) . . ?
C20 C19 N7 119.7(3) . . ?
O1 C22 C21 119.8(3) . . ?
O1 C22 C17 122.3(3) . . ?
C21 C22 C17 117.9(3) . . ?
C24 C29 C28 119.5(3) . . ?
C24 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C29 C24 C25 120.3(3) . . ?
C29 C24 C23 119.5(3) . . ?
C25 C24 C23 120.3(3) . . ?
N3 C23 N2 101.8(2) . . ?
N3 C23 C24 112.2(2) . . ?
N2 C23 C24 116.5(3) . . ?
N3 C23 H23 108.7 . . ?
N2 C23 H23 108.7 . . ?
C24 C23 H23 108.7 . . ?
N5 C16 C17 126.7(3) . . ?
N5 C16 H16 116.7 . . ?
C17 C16 H16 116.7 . . ?
N1 C7 C6 126.7(3) . . ?
N1 C7 H7 116.7 . . ?
C6 C7 H7 116.7 . . ?
N4 C13 C12 110.8(3) . . ?
N4 C13 H13A 109.5 . . ?
C12 C13 H13A 109.5 . . ?
N4 C13 H13B 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C5 C6 C7 117.9(3) . . ?
C5 C6 C1 118.3(3) . . ?
C7 C6 C1 123.8(3) . . ?
C21 C20 C19 119.9(3) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C27 C26 C25 122.4(3) . . ?
C27 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
O2 C25 C26 121.6(3) . . ?
O2 C25 C24 120.9(3) . . ?
C26 C25 C24 117.5(3) . . ?
C27 C28 C29 121.3(3) . . ?
C27 C28 N8 119.7(3) . . ?
C29 C28 N8 119.0(4) . . ?
N3 C12 C13 111.2(3) . . ?
N3 C12 H12A 109.4 . . ?
C13 C12 H12A 109.4 . . ?
N3 C12 H12B 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
N2 C10 C11 105.7(2) . . ?
N2 C10 H10A 110.6 . . ?
C11 C10 H10A 110.6 . . ?
N2 C10 H10B 110.6 . . ?
C11 C10 H10B 110.6 . . ?
H10A C10 H10B 108.7 . . ?
N1 C8 C9 110.5(3) . . ?
N1 C8 H8A 109.5 . . ?
C9 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C20 C21 C22 121.6(3) . . ?
C20 C21 H21 119.2 . . ?
C22 C21 H21 119.2 . . ?
N3 C11 C10 104.8(2) . . ?
N3 C11 H11A 110.8 . . ?
C10 C11 H11A 110.8 . . ?
N3 C11 H11B 110.8 . . ?
C10 C11 H11B 110.8 . . ?
H11A C11 H11B 108.9 . . ?
C4 C5 C6 121.3(4) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.3 . . ?
O4 C1 C2 120.2(3) . . ?
O4 C1 C6 122.2(3) . . ?
C2 C1 C6 117.6(3) . . ?
N2 C9 C8 113.7(3) . . ?
N2 C9 H9A 108.8 . . ?
C8 C9 H9A 108.8 . . ?
N2 C9 H9B 108.8 . . ?
C8 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C26 C27 C28 119.0(3) . . ?
C26 C27 H27 120.5 . . ?
C28 C27 H27 120.5 . . ?
N4 C14 C15 109.8(3) . . ?
N4 C14 H14A 109.7 . . ?
C15 C14 H14A 109.7 . . ?
N4 C14 H14B 109.7 . . ?
C15 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
N5 C15 C14 108.8(3) . . ?
N5 C15 H15A 109.9 . . ?
C14 C15 H15A 109.9 . . ?
N5 C15 H15B 109.9 . . ?
C14 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
C5 C4 C3 120.5(4) . . ?
C5 C4 N9 119.5(4) . . ?
C3 C4 N9 120.0(4) . . ?
C3 C2 C1 122.9(4) . . ?
C3 C2 H2 118.5 . . ?
C1 C2 H2 118.5 . . ?
C2 C3 C4 119.4(4) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C30 N6 Mn2 152.7(3) . . ?
N6 C30 O5 177.6(5) . . ?
C31 O3 Mn1 126.1(4) . . ?
O3 C31 H31A 109.5 . . ?
O3 C31 H31B 109.4 . . ?
H31A C31 H31B 109.5 . . ?
O3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O13 C32 C33 129.8(12) . . ?
O13 C32 H32A 104.1 . . ?
C33 C32 H32A 105.1 . . ?
O13 C32 H32B 105.1 . . ?
C33 C32 H32B 105.1 . . ?
H32A C32 H32B 105.9 . . ?
C32 O13 H13 111.7 . . ?
C32 C33 H33A 109.6 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.4 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

_refine_diff_density_max         0.472
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.057

