# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_co-2b
_database_code_depnum_ccdc_archive 'CCDC 1997742'
loop_
_audit_author_name
_audit_author_address
'Klaus Wurst'
;University of Innsbruck
Austria
;
_audit_update_record             
;
2020-04-24 deposited with the CCDC.	2020-06-29 downloaded from the CCDC.
;

_vrf_THETM01_co-2b               
;
PROBLEM: low diffraction              
RESPONSE: small crystal size and disordering
         see: _refine_special_details
;


_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            'C35 H39 Cl2 Co N8 O10'
_chemical_formula_weight         861.57

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   20.6162(3)
_cell_length_b                   10.9186(4)
_cell_length_c                   34.6060(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.872(2)
_cell_angle_gamma                90
_cell_volume                     7772.0(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    233(2)
_cell_measurement_reflns_used    30391
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      24.1

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_F_000             3568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.646
_shelx_estimated_absorpt_T_min   0.882
_shelx_estimated_absorpt_T_max   0.981
_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      233(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_detector_area_resol_mean 9.6
_diffrn_reflns_number            16664
_diffrn_reflns_av_unetI/netI     0.0780
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.980
_diffrn_reflns_theta_max         23.997
_diffrn_reflns_theta_full        23.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6091
_reflns_number_gt                3793
_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       COLLECT
_computing_cell_refinement       ?
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Small crystall with low diffraction, visible reflections on frames 
 could only seen until two theta of 40 degrees. 
 Positional disorder in ratio of 1 : 1 for the oxygen atoms of the
 two perchlorate anions at Cl1 and Cl2 (O3-O10:O3A-O10A). 
 Occupational disorder of solvent acetonitrile: C31-C30-N8 at a
 common position is only half occupated, whereas C33-C32-N9 is
 half occupated by a symmetry centre nearby. Hydrogens atoms of
 solvents were omitted. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0740P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6091
_refine_ls_number_parameters     578
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1418
_refine_ls_wR_factor_gt          0.1233
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.003
_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
Co1 Co 0.63866(3) 0.14277(4) 0.32330(2) 0.0393(2) Uani 1 1 d . . . . .
O1 O 0.58585(15) 0.4989(2) 0.50294(8) 0.0630(8) Uani 1 1 d . . . . .
O2 O 0.54349(17) 0.7241(2) 0.39101(8) 0.0719(9) Uani 1 1 d . . . . .
N1 N 0.64963(16) -0.0512(3) 0.31283(9) 0.0432(8) Uani 1 1 d . . . . .
N2 N 0.54991(15) 0.0732(2) 0.33971(8) 0.0373(8) Uani 1 1 d . . . . .
N3 N 0.71264(16) 0.0992(3) 0.36303(9) 0.0437(8) Uani 1 1 d . . . . .
N4 N 0.66396(16) 0.1421(3) 0.26657(9) 0.0447(8) Uani 1 1 d . . . . .
N5 N 0.57650(16) 0.5886(3) 0.47917(9) 0.0460(8) Uani 1 1 d . . . . .
N6 N 0.55380(17) 0.6949(3) 0.42680(10) 0.0517(9) Uani 1 1 d . . . . .
N7 N 0.63331(16) 0.3291(3) 0.32707(9) 0.0487(9) Uani 1 1 d . . . . .
C1 C 0.5843(2) -0.0952(3) 0.30034(12) 0.0492(11) Uani 1 1 d . . . . .
H1A H 0.5826 -0.1846 0.3027 0.059 Uiso 1 1 calc R U . . .
H1B H 0.5742 -0.0739 0.2731 0.059 Uiso 1 1 calc R U . . .
C2 C 0.5350(2) -0.0382(3) 0.32484(11) 0.0435(10) Uani 1 1 d . . . . .
C3 C 0.4772(2) -0.0970(4) 0.33065(12) 0.0514(11) Uani 1 1 d . . . . .
H3 H 0.4686 -0.1752 0.3202 0.062 Uiso 1 1 calc R U . . .
C4 C 0.4325(2) -0.0388(4) 0.35210(13) 0.0558(12) Uani 1 1 d . . . . .
H4 H 0.3924 -0.0763 0.3560 0.067 Uiso 1 1 calc R U . . .
C5 C 0.4468(2) 0.0744(3) 0.36766(12) 0.0510(11) Uani 1 1 d . . . . .
H5 H 0.4168 0.1148 0.3825 0.061 Uiso 1 1 calc R U . . .
C6 C 0.50585(19) 0.1288(3) 0.36146(11) 0.0399(10) Uani 1 1 d . . . . .
C7 C 0.5231(2) 0.2481(3) 0.38023(10) 0.0392(10) Uani 1 1 d . . . . .
C8 C 0.57513(19) 0.2577(3) 0.40720(11) 0.0420(10) Uani 1 1 d . . . . .
H8 H 0.6018 0.1892 0.4125 0.050 Uiso 1 1 calc R U . . .
C9 C 0.58892(19) 0.3669(3) 0.42671(11) 0.0423(10) Uani 1 1 d . . . . .
H9 H 0.6247 0.3723 0.4449 0.051 Uiso 1 1 calc R U . . .
C10 C 0.5491(2) 0.4683(3) 0.41897(11) 0.0395(10) Uani 1 1 d . . . . .
C11 C 0.4980(2) 0.4602(3) 0.39132(11) 0.0467(11) Uani 1 1 d . . . . .
H11 H 0.4722 0.5295 0.3853 0.056 Uiso 1 1 calc R U . . .
C12 C 0.4844(2) 0.3509(3) 0.37242(11) 0.0446(10) Uani 1 1 d . . . . .
H12 H 0.4486 0.3457 0.3541 0.054 Uiso 1 1 calc R U . . .
C13 C 0.56078(19) 0.5814(3) 0.44136(11) 0.0398(9) Uani 1 1 d . . . . .
C14 C 0.5898(2) 0.7192(3) 0.49176(11) 0.0497(11) Uani 1 1 d . . . . .
C15 C 0.5517(2) 0.7880(3) 0.45842(12) 0.0563(12) Uani 1 1 d . . . . .
C16 C 0.6758(2) -0.1068(3) 0.34958(12) 0.0495(11) Uani 1 1 d . . . . .
H16A H 0.6977 -0.1840 0.3442 0.059 Uiso 1 1 calc R U . . .
H16B H 0.6400 -0.1249 0.3660 0.059 Uiso 1 1 calc R U . . .
C17 C 0.7230(2) -0.0209(3) 0.37046(12) 0.0481(11) Uani 1 1 d . . . . .
C18 C 0.7728(3) -0.0587(4) 0.39628(14) 0.0662(13) Uani 1 1 d . . . . .
H18 H 0.7791 -0.1424 0.4016 0.079 Uiso 1 1 calc R U . . .
C19 C 0.8134(3) 0.0277(5) 0.41435(15) 0.0799(15) Uani 1 1 d . . . . .
H19 H 0.8477 0.0031 0.4319 0.096 Uiso 1 1 calc R U . . .
C20 C 0.8033(2) 0.1487(4) 0.40653(14) 0.0695(14) Uani 1 1 d . . . . .
H20 H 0.8305 0.2087 0.4185 0.083 Uiso 1 1 calc R U . . .
C21 C 0.7528(2) 0.1811(4) 0.38090(13) 0.0568(12) Uani 1 1 d . . . . .
H21 H 0.7460 0.2647 0.3755 0.068 Uiso 1 1 calc R U . . .
C22 C 0.6950(2) -0.0651(3) 0.28224(12) 0.0498(11) Uani 1 1 d . . . . .
H22A H 0.6881 -0.1448 0.2696 0.060 Uiso 1 1 calc R U . . .
H22B H 0.7398 -0.0626 0.2937 0.060 Uiso 1 1 calc R U . . .
C23 C 0.6852(2) 0.0352(4) 0.25272(12) 0.0481(11) Uani 1 1 d . . . . .
C24 C 0.6996(2) 0.0228(4) 0.21475(13) 0.0626(13) Uani 1 1 d . . . . .
H24 H 0.7134 -0.0531 0.2054 0.075 Uiso 1 1 calc R U . . .
C25 C 0.6937(2) 0.1223(5) 0.19048(14) 0.0694(14) Uani 1 1 d . . . . .
H25 H 0.7042 0.1152 0.1646 0.083 Uiso 1 1 calc R U . . .
C26 C 0.6725(2) 0.2318(4) 0.20405(13) 0.0621(13) Uani 1 1 d . . . . .
H26 H 0.6678 0.3006 0.1878 0.075 Uiso 1 1 calc R U . . .
C27 C 0.6583(2) 0.2383(4) 0.24212(12) 0.0507(11) Uani 1 1 d . . . . .
H27 H 0.6439 0.3134 0.2517 0.061 Uiso 1 1 calc R U . . .
C28 C 0.6293(2) 0.4314(4) 0.32868(12) 0.0568(12) Uani 1 1 d . . . . .
C29 C 0.6221(3) 0.5650(3) 0.32980(16) 0.100(2) Uani 1 1 d . . . . .
H29A H 0.6374 0.6002 0.3063 0.149 Uiso 1 1 calc R U . . .
H29B H 0.6476 0.5974 0.3521 0.149 Uiso 1 1 calc R U . . .
H29C H 0.5767 0.5858 0.3317 0.149 Uiso 1 1 calc R U . . .
C141 C 0.6634(2) 0.7368(4) 0.49275(14) 0.0729(14) Uani 1 1 d . . . . .
H14A H 0.6743 0.8199 0.5007 0.109 Uiso 1 1 calc R U . . .
H14B H 0.6845 0.6795 0.5110 0.109 Uiso 1 1 calc R U . . .
H14C H 0.6783 0.7222 0.4672 0.109 Uiso 1 1 calc R U . . .
C142 C 0.5653(2) 0.7407(4) 0.53173(12) 0.0639(13) Uani 1 1 d . . . . .
H14D H 0.5740 0.8247 0.5396 0.096 Uiso 1 1 calc R U . . .
H14E H 0.5189 0.7256 0.5309 0.096 Uiso 1 1 calc R U . . .
H14F H 0.5874 0.6855 0.5502 0.096 Uiso 1 1 calc R U . . .
C151 C 0.5819(3) 0.9080(4) 0.44599(14) 0.0893(18) Uani 1 1 d . . . . .
H15A H 0.5803 0.9676 0.4667 0.134 Uiso 1 1 calc R U . . .
H15B H 0.6268 0.8939 0.4404 0.134 Uiso 1 1 calc R U . . .
H15C H 0.5579 0.9387 0.4229 0.134 Uiso 1 1 calc R U . . .
C152 C 0.4794(2) 0.8055(4) 0.46485(15) 0.0781(15) Uani 1 1 d . . . . .
H15D H 0.4748 0.8654 0.4852 0.117 Uiso 1 1 calc R U . . .
H15E H 0.4568 0.8342 0.4411 0.117 Uiso 1 1 calc R U . . .
H15F H 0.4609 0.7281 0.4724 0.117 Uiso 1 1 calc R U . . .
N8 N 0.5000 0.1598(7) 0.2500 0.102(2) Uani 1 2 d S T P . .
C30 C 0.5000 0.2638(10) 0.2500 0.085(2) Uani 1 2 d S T P . .
C31 C 0.5000 0.4003(7) 0.2500 0.113(3) Uani 1 2 d S T P . .
Cl1 Cl 0.77085(9) 0.53500(12) 0.41618(4) 0.0895(5) Uani 1 1 d . . . . .
Cl2 Cl 0.86899(7) 0.12093(10) 0.28888(4) 0.0659(4) Uani 1 1 d . . . . .
O3 O 0.8375(4) 0.4812(9) 0.4375(3) 0.145(4) Uani 0.5 1 d . . P A 1
O4 O 0.7474(9) 0.4716(17) 0.3838(6) 0.134(7) Uani 0.5 1 d . . P A 1
O5 O 0.7869(10) 0.6491(9) 0.4116(5) 0.102(7) Uani 0.5 1 d . . P A 1
O6 O 0.7273(10) 0.508(2) 0.4438(8) 0.128(7) Uani 0.5 1 d . . P A 1
O7 O 0.9051(6) 0.1940(9) 0.2654(3) 0.104(4) Uani 0.5 1 d . . P B 1
O8 O 0.8472(7) 0.0221(10) 0.2668(5) 0.132(8) Uani 0.5 1 d . . P B 1
O9 O 0.8087(6) 0.1993(17) 0.2954(5) 0.107(5) Uani 0.5 1 d . . P B 1
O10 O 0.9018(8) 0.0994(15) 0.3220(4) 0.176(6) Uani 0.5 1 d . . P B 1
O3A O 0.7063(8) 0.6294(11) 0.4032(3) 0.165(4) Uani 0.5 1 d . . P A 2
O4A O 0.7812(8) 0.4598(14) 0.3843(6) 0.119(9) Uani 0.5 1 d . . P A 2
O5A O 0.8098(10) 0.6304(17) 0.4127(7) 0.144(9) Uani 0.5 1 d . . P A 2
O6A O 0.7475(12) 0.487(2) 0.4451(6) 0.157(10) Uani 0.5 1 d . . P A 2
O7A O 0.8628(7) 0.0298(8) 0.3180(4) 0.136(4) Uani 0.5 1 d . . P B 2
O8A O 0.8446(10) 0.0618(18) 0.2563(4) 0.190(10) Uani 0.5 1 d . . P B 2
O9A O 0.8431(7) 0.2182(16) 0.2990(7) 0.146(7) Uani 0.5 1 d . . P B 2
O10A O 0.9374(5) 0.1351(13) 0.2882(6) 0.168(7) Uani 0.5 1 d . . P B 2
N9 N 0.3222(8) -0.1466(12) 0.5231(4) 0.168(5) Uiso 0.5 1 d . . P . .
C32 C 0.2755(9) -0.1940(13) 0.5121(4) 0.103(4) Uiso 0.5 1 d . . P . .
C33 C 0.2203(7) -0.2429(14) 0.5012(4) 0.106(5) Uiso 0.5 1 d . . P . .


_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
Co1 N3 2.039(3) . ?
Co1 N7 2.042(3) . ?
Co1 N4 2.065(3) . ?
Co1 N2 2.095(3) . ?
Co1 N1 2.163(3) . ?
O1 N5 1.285(4) . ?
O2 N6 1.283(4) . ?
N1 C22 1.467(5) . ?
N1 C1 1.468(5) . ?
N1 C16 1.478(5) . ?
N2 C2 1.348(4) . ?
N2 C6 1.361(4) . ?
N3 C21 1.341(5) . ?
N3 C17 1.351(4) . ?
N4 C23 1.346(4) . ?
N4 C27 1.349(5) . ?
N5 C13 1.329(5) . ?
N5 C14 1.511(5) . ?
N6 C13 1.341(5) . ?
N6 C15 1.497(5) . ?
N7 C28 1.122(5) . ?
C1 C2 1.501(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 C3 1.379(5) . ?
C3 C4 1.378(6) . ?
C3 H3 0.9400 . ?
C4 C5 1.373(5) . ?
C4 H4 0.9400 . ?
C5 C6 1.383(5) . ?
C5 H5 0.9400 . ?
C6 C7 1.488(5) . ?
C7 C8 1.377(5) . ?
C7 C12 1.393(5) . ?
C8 C9 1.390(5) . ?
C8 H8 0.9400 . ?
C9 C10 1.393(5) . ?
C9 H9 0.9400 . ?
C10 C11 1.377(5) . ?
C10 C13 1.470(5) . ?
C11 C12 1.381(5) . ?
C11 H11 0.9400 . ?
C12 H12 0.9400 . ?
C14 C142 1.522(5) . ?
C14 C141 1.529(6) . ?
C14 C15 1.546(6) . ?
C15 C151 1.525(6) . ?
C15 C152 1.534(6) . ?
C16 C17 1.502(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C17 C18 1.377(6) . ?
C18 C19 1.382(6) . ?
C18 H18 0.9400 . ?
C19 C20 1.362(6) . ?
C19 H19 0.9400 . ?
C20 C21 1.367(6) . ?
C20 H20 0.9400 . ?
C21 H21 0.9400 . ?
C22 C23 1.502(5) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C23 C24 1.373(6) . ?
C24 C25 1.374(6) . ?
C24 H24 0.9400 . ?
C25 C26 1.367(6) . ?
C25 H25 0.9400 . ?
C26 C27 1.371(6) . ?
C26 H26 0.9400 . ?
C27 H27 0.9400 . ?
C28 C29 1.467(6) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 H29C 0.9700 . ?
C141 H14A 0.9700 . ?
C141 H14B 0.9700 . ?
C141 H14C 0.9700 . ?
C142 H14D 0.9700 . ?
C142 H14E 0.9700 . ?
C142 H14F 0.9700 . ?
C151 H15A 0.9700 . ?
C151 H15B 0.9700 . ?
C151 H15C 0.9700 . ?
C152 H15D 0.9700 . ?
C152 H15E 0.9700 . ?
C152 H15F 0.9700 . ?
N8 C30 1.136(9) . ?
C30 C31 1.490(12) . ?
Cl1 O6A 1.256(16) . ?
Cl1 O5 1.301(10) . ?
Cl1 O5A 1.326(18) . ?
Cl1 O4 1.378(19) . ?
Cl1 O6 1.385(19) . ?
Cl1 O4A 1.403(15) . ?
Cl1 O3 1.624(8) . ?
Cl1 O3A 1.719(13) . ?
Cl2 O9A 1.250(16) . ?
Cl2 O10 1.313(10) . ?
Cl2 O8A 1.366(13) . ?
Cl2 O8 1.380(10) . ?
Cl2 O7 1.391(8) . ?
Cl2 O10A 1.421(11) . ?
Cl2 O7A 1.428(10) . ?
Cl2 O9 1.538(14) . ?
N9 C32 1.135(18) . ?
N9 C33 1.68(2) 7_546 ?
C32 C33 0.838(16) 7_546 ?
C32 C33 1.290(16) . ?
C32 C32 1.78(3) 7_546 ?
C33 C32 0.838(16) 7_546 ?
C33 C33 1.24(3) 7_546 ?
C33 N9 1.68(2) 7_546 ?

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
N3 Co1 N7 103.31(13) . . ?
N3 Co1 N4 114.50(13) . . ?
N7 Co1 N4 94.74(12) . . ?
N3 Co1 N2 111.09(12) . . ?
N7 Co1 N2 106.98(12) . . ?
N4 Co1 N2 122.53(12) . . ?
N3 Co1 N1 78.62(12) . . ?
N7 Co1 N1 173.16(12) . . ?
N4 Co1 N1 78.55(11) . . ?
N2 Co1 N1 78.08(11) . . ?
C22 N1 C1 111.8(3) . . ?
C22 N1 C16 111.4(3) . . ?
C1 N1 C16 113.1(3) . . ?
C22 N1 Co1 107.5(2) . . ?
C1 N1 Co1 105.4(2) . . ?
C16 N1 Co1 107.1(2) . . ?
C2 N2 C6 118.0(3) . . ?
C2 N2 Co1 113.9(2) . . ?
C6 N2 Co1 128.0(2) . . ?
C21 N3 C17 118.3(4) . . ?
C21 N3 Co1 124.5(3) . . ?
C17 N3 Co1 117.2(3) . . ?
C23 N4 C27 117.9(3) . . ?
C23 N4 Co1 116.8(2) . . ?
C27 N4 Co1 125.2(3) . . ?
O1 N5 C13 126.9(3) . . ?
O1 N5 C14 121.2(3) . . ?
C13 N5 C14 111.6(3) . . ?
O2 N6 C13 126.8(3) . . ?
O2 N6 C15 121.7(3) . . ?
C13 N6 C15 111.1(3) . . ?
C28 N7 Co1 178.6(4) . . ?
N1 C1 C2 109.9(3) . . ?
N1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N2 C2 C3 122.8(4) . . ?
N2 C2 C1 116.4(3) . . ?
C3 C2 C1 120.8(3) . . ?
C4 C3 C2 118.7(4) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C5 C4 C3 119.5(4) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 119.6(4) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
N2 C6 C5 121.4(3) . . ?
N2 C6 C7 118.9(3) . . ?
C5 C6 C7 119.7(3) . . ?
C8 C7 C12 118.7(3) . . ?
C8 C7 C6 121.0(3) . . ?
C12 C7 C6 120.2(4) . . ?
C7 C8 C9 121.3(3) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C8 C9 C10 119.3(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 119.7(3) . . ?
C11 C10 C13 120.7(3) . . ?
C9 C10 C13 119.5(4) . . ?
C10 C11 C12 120.4(3) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 120.6(4) . . ?
C11 C12 H12 119.7 . . ?
C7 C12 H12 119.7 . . ?
N5 C13 N6 109.1(3) . . ?
N5 C13 C10 126.1(3) . . ?
N6 C13 C10 124.7(3) . . ?
N5 C14 C142 110.0(3) . . ?
N5 C14 C141 106.6(3) . . ?
C142 C14 C141 110.5(4) . . ?
N5 C14 C15 99.8(3) . . ?
C142 C14 C15 114.9(3) . . ?
C141 C14 C15 114.2(3) . . ?
N6 C15 C151 110.2(3) . . ?
N6 C15 C152 105.5(4) . . ?
C151 C15 C152 110.7(4) . . ?
N6 C15 C14 100.2(3) . . ?
C151 C15 C14 115.6(4) . . ?
C152 C15 C14 113.7(4) . . ?
N1 C16 C17 110.1(3) . . ?
N1 C16 H16A 109.6 . . ?
C17 C16 H16A 109.6 . . ?
N1 C16 H16B 109.6 . . ?
C17 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
N3 C17 C18 121.1(4) . . ?
N3 C17 C16 115.2(4) . . ?
C18 C17 C16 123.7(4) . . ?
C17 C18 C19 119.4(4) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C20 C19 C18 119.5(5) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C19 C20 C21 118.7(4) . . ?
C19 C20 H20 120.7 . . ?
C21 C20 H20 120.7 . . ?
N3 C21 C20 123.1(4) . . ?
N3 C21 H21 118.5 . . ?
C20 C21 H21 118.5 . . ?
N1 C22 C23 110.6(3) . . ?
N1 C22 H22A 109.5 . . ?
C23 C22 H22A 109.5 . . ?
N1 C22 H22B 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
N4 C23 C24 121.5(4) . . ?
N4 C23 C22 115.0(3) . . ?
C24 C23 C22 123.4(4) . . ?
C23 C24 C25 119.4(4) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C26 C25 C24 119.9(4) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C27 118.0(4) . . ?
C25 C26 H26 121.0 . . ?
C27 C26 H26 121.0 . . ?
N4 C27 C26 123.2(4) . . ?
N4 C27 H27 118.4 . . ?
C26 C27 H27 118.4 . . ?
N7 C28 C29 178.1(6) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C14 C141 H14A 109.5 . . ?
C14 C141 H14B 109.5 . . ?
H14A C141 H14B 109.5 . . ?
C14 C141 H14C 109.5 . . ?
H14A C141 H14C 109.5 . . ?
H14B C141 H14C 109.5 . . ?
C14 C142 H14D 109.5 . . ?
C14 C142 H14E 109.5 . . ?
H14D C142 H14E 109.5 . . ?
C14 C142 H14F 109.5 . . ?
H14D C142 H14F 109.5 . . ?
H14E C142 H14F 109.5 . . ?
C15 C151 H15A 109.5 . . ?
C15 C151 H15B 109.5 . . ?
H15A C151 H15B 109.5 . . ?
C15 C151 H15C 109.5 . . ?
H15A C151 H15C 109.5 . . ?
H15B C151 H15C 109.5 . . ?
C15 C152 H15D 109.5 . . ?
C15 C152 H15E 109.5 . . ?
H15D C152 H15E 109.5 . . ?
C15 C152 H15F 109.5 . . ?
H15D C152 H15F 109.5 . . ?
H15E C152 H15F 109.5 . . ?
N8 C30 C31 180.0 . . ?
O6A Cl1 O5A 132.0(17) . . ?
O5 Cl1 O4 117.4(11) . . ?
O5 Cl1 O6 117.8(12) . . ?
O4 Cl1 O6 104.4(13) . . ?
O6A Cl1 O4A 117.9(15) . . ?
O5A Cl1 O4A 105.2(11) . . ?
O5 Cl1 O3 100.8(10) . . ?
O4 Cl1 O3 115.3(9) . . ?
O6 Cl1 O3 100.3(10) . . ?
O6A Cl1 O3A 97.3(11) . . ?
O5A Cl1 O3A 88.2(10) . . ?
O4A Cl1 O3A 107.5(9) . . ?
O9A Cl2 O8A 119.6(13) . . ?
O10 Cl2 O8 118.3(10) . . ?
O10 Cl2 O7 110.4(8) . . ?
O8 Cl2 O7 107.0(8) . . ?
O9A Cl2 O10A 110.8(8) . . ?
O8A Cl2 O10A 110.4(11) . . ?
O9A Cl2 O7A 109.5(11) . . ?
O8A Cl2 O7A 102.0(9) . . ?
O10A Cl2 O7A 102.8(9) . . ?
O10 Cl2 O9 110.1(10) . . ?
O8 Cl2 O9 106.3(8) . . ?
O7 Cl2 O9 103.7(8) . . ?
C32 N9 C33 26.6(10) . 7_546 ?
C33 C32 N9 116(3) 7_546 . ?
C33 C32 C33 68(2) 7_546 . ?
N9 C32 C33 176(2) . . ?
C33 C32 C32 42.0(15) 7_546 7_546 ?
N9 C32 C32 158(2) . 7_546 ?
C33 C32 C32 25.8(8) . 7_546 ?
C32 C33 C33 73.7(18) 7_546 7_546 ?
C32 C33 C32 112(2) 7_546 . ?
C33 C33 C32 38.6(10) 7_546 . ?
C32 C33 N9 37.3(18) 7_546 7_546 ?
C33 C33 N9 111.0(19) 7_546 7_546 ?
C32 C33 N9 149.5(17) . 7_546 ?

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
C22 N1 C1 C2 -158.5(3) . . . . ?
C16 N1 C1 C2 74.7(4) . . . . ?
Co1 N1 C1 C2 -42.0(3) . . . . ?
C6 N2 C2 C3 0.3(5) . . . . ?
Co1 N2 C2 C3 -176.8(3) . . . . ?
C6 N2 C2 C1 178.8(3) . . . . ?
Co1 N2 C2 C1 1.7(4) . . . . ?
N1 C1 C2 N2 28.5(5) . . . . ?
N1 C1 C2 C3 -153.0(3) . . . . ?
N2 C2 C3 C4 1.0(6) . . . . ?
C1 C2 C3 C4 -177.5(4) . . . . ?
C2 C3 C4 C5 -1.3(6) . . . . ?
C3 C4 C5 C6 0.3(6) . . . . ?
C2 N2 C6 C5 -1.2(5) . . . . ?
Co1 N2 C6 C5 175.3(3) . . . . ?
C2 N2 C6 C7 176.2(3) . . . . ?
Co1 N2 C6 C7 -7.3(5) . . . . ?
C4 C5 C6 N2 1.0(6) . . . . ?
C4 C5 C6 C7 -176.4(4) . . . . ?
N2 C6 C7 C8 -61.5(5) . . . . ?
C5 C6 C7 C8 115.9(4) . . . . ?
N2 C6 C7 C12 122.3(4) . . . . ?
C5 C6 C7 C12 -60.3(5) . . . . ?
C12 C7 C8 C9 0.6(5) . . . . ?
C6 C7 C8 C9 -175.7(3) . . . . ?
C7 C8 C9 C10 0.4(6) . . . . ?
C8 C9 C10 C11 -2.0(6) . . . . ?
C8 C9 C10 C13 175.9(3) . . . . ?
C9 C10 C11 C12 2.7(6) . . . . ?
C13 C10 C11 C12 -175.2(3) . . . . ?
C10 C11 C12 C7 -1.8(6) . . . . ?
C8 C7 C12 C11 0.1(5) . . . . ?
C6 C7 C12 C11 176.4(3) . . . . ?
O1 N5 C13 N6 178.5(3) . . . . ?
C14 N5 C13 N6 -7.5(4) . . . . ?
O1 N5 C13 C10 1.7(6) . . . . ?
C14 N5 C13 C10 175.7(4) . . . . ?
O2 N6 C13 N5 174.5(4) . . . . ?
C15 N6 C13 N5 -12.2(5) . . . . ?
O2 N6 C13 C10 -8.6(6) . . . . ?
C15 N6 C13 C10 164.6(4) . . . . ?
C11 C10 C13 N5 137.4(4) . . . . ?
C9 C10 C13 N5 -40.6(6) . . . . ?
C11 C10 C13 N6 -39.0(6) . . . . ?
C9 C10 C13 N6 143.1(4) . . . . ?
O1 N5 C14 C142 -42.0(5) . . . . ?
C13 N5 C14 C142 143.7(4) . . . . ?
O1 N5 C14 C141 77.9(4) . . . . ?
C13 N5 C14 C141 -96.5(4) . . . . ?
O1 N5 C14 C15 -163.1(3) . . . . ?
C13 N5 C14 C15 22.6(4) . . . . ?
O2 N6 C15 C151 -38.7(6) . . . . ?
C13 N6 C15 C151 147.6(4) . . . . ?
O2 N6 C15 C152 80.8(5) . . . . ?
C13 N6 C15 C152 -92.9(4) . . . . ?
O2 N6 C15 C14 -160.9(4) . . . . ?
C13 N6 C15 C14 25.4(4) . . . . ?
N5 C14 C15 N6 -26.4(4) . . . . ?
C142 C14 C15 N6 -144.0(3) . . . . ?
C141 C14 C15 N6 86.9(4) . . . . ?
N5 C14 C15 C151 -144.7(3) . . . . ?
C142 C14 C15 C151 97.7(4) . . . . ?
C141 C14 C15 C151 -31.4(5) . . . . ?
N5 C14 C15 C152 85.7(4) . . . . ?
C142 C14 C15 C152 -31.9(5) . . . . ?
C141 C14 C15 C152 -161.0(3) . . . . ?
C22 N1 C16 C17 80.9(4) . . . . ?
C1 N1 C16 C17 -152.2(3) . . . . ?
Co1 N1 C16 C17 -36.4(4) . . . . ?
C21 N3 C17 C18 1.2(6) . . . . ?
Co1 N3 C17 C18 178.6(3) . . . . ?
C21 N3 C17 C16 179.6(4) . . . . ?
Co1 N3 C17 C16 -3.0(4) . . . . ?
N1 C16 C17 N3 27.6(5) . . . . ?
N1 C16 C17 C18 -154.1(4) . . . . ?
N3 C17 C18 C19 -1.1(7) . . . . ?
C16 C17 C18 C19 -179.3(4) . . . . ?
C17 C18 C19 C20 0.4(8) . . . . ?
C18 C19 C20 C21 0.1(8) . . . . ?
C17 N3 C21 C20 -0.7(6) . . . . ?
Co1 N3 C21 C20 -177.9(3) . . . . ?
C19 C20 C21 N3 0.0(7) . . . . ?
C1 N1 C22 C23 78.7(4) . . . . ?
C16 N1 C22 C23 -153.7(3) . . . . ?
Co1 N1 C22 C23 -36.6(4) . . . . ?
C27 N4 C23 C24 -1.2(6) . . . . ?
Co1 N4 C23 C24 176.1(3) . . . . ?
C27 N4 C23 C22 175.7(4) . . . . ?
Co1 N4 C23 C22 -7.0(4) . . . . ?
N1 C22 C23 N4 30.1(5) . . . . ?
N1 C22 C23 C24 -153.1(4) . . . . ?
N4 C23 C24 C25 1.5(7) . . . . ?
C22 C23 C24 C25 -175.1(4) . . . . ?
C23 C24 C25 C26 -1.2(7) . . . . ?
C24 C25 C26 C27 0.6(7) . . . . ?
C23 N4 C27 C26 0.6(6) . . . . ?
Co1 N4 C27 C26 -176.4(3) . . . . ?
C25 C26 C27 N4 -0.4(7) . . . . ?
C33 N9 C32 C32 1(3) 7_546 . . 7_546 ?
C33 C32 C33 C32 -0.002(4) 7_546 . . 7_546 ?
C32 C32 C33 C33 0.002(5) 7_546 . . 7_546 ?
C33 C32 C33 N9 -1(2) 7_546 . . 7_546 ?
C32 C32 C33 N9 -1(2) 7_546 . . 7_546 ?

_refine_diff_density_max         0.397
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.060

####################################################################### 
# 
# 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_cu-3a
_database_code_depnum_ccdc_archive 'CCDC 1997743'
loop_
_audit_author_name
_audit_author_address
'Klaus Wurst'
;University of Innsbruck
Austria
;
_audit_update_record             
;
2020-04-24 deposited with the CCDC.	2020-06-29 downloaded from the CCDC.
;

_vrf_THETM01_cu-3a               
;
PROBLEM: low diffraction              
RESPONSE: small crystal size and disordering
         see: _refine_special_details
;


_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            'C35 H40 Cl3 Cu N8 O13'
_chemical_formula_weight         950.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      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                   11.3545(5)
_cell_length_b                   13.8512(6)
_cell_length_c                   14.6307(7)
_cell_angle_alpha                80.651(2)
_cell_angle_beta                 72.087(3)
_cell_angle_gamma                86.640(3)
_cell_volume                     2160.30(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    233(2)
_cell_measurement_reflns_used    66680
_cell_measurement_theta_min      1.0
_cell_measurement_theta_max      24.8

_exptl_crystal_description       plate
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_F_000             980
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.761
_shelx_estimated_absorpt_T_min   0.833
_shelx_estimated_absorpt_T_max   0.978
_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      233(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_detector_area_resol_mean 9.6
_diffrn_reflns_number            11860
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_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         1.885
_diffrn_reflns_theta_max         23.995
_diffrn_reflns_theta_full        23.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6729
_reflns_number_gt                4978
_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       COLLECT
_computing_cell_refinement       ?
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Small crystall with low diffraction, visible reflections on frames 
 could only seen until two theta of 41 degrees. 
 Positional disorder in range of 0.85 : 0.15 by rotation of the
 imino nizroxide radical ring about 67 degrees around the C11-C13
 bond with overlying methyl carbon atoms C143=C153 and C144=C151.
 Hydrogens of the minor disordered part were omitted. The hydrogen 
 atom at N6 was found and refined isotropically with bond 
 restraint (d = 89 pm).
 Positional disorder of two oxygen atoms at one perchlorate (Cl3)
 in ratio 1 : 1 for O12 and O13 : O12A and O13A. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0978P)²+3.1734P] 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         6729
_refine_ls_number_parameters     593
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0767
_refine_ls_wR_factor_ref         0.2083
_refine_ls_wR_factor_gt          0.1890
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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 0.17604(6) 0.15811(4) 0.06802(4) 0.0533(3) Uani 1 1 d . . . . .
N1 N 0.1721(4) 0.1910(3) 0.1986(3) 0.0483(10) Uani 1 1 d . . . . .
N2 N 0.3964(4) 0.1945(3) 0.0327(3) 0.0567(11) Uani 1 1 d . . . . .
N3 N 0.1690(4) 0.0214(3) 0.1381(3) 0.0539(11) Uani 1 1 d . . . . .
N4 N 0.1631(4) 0.3028(3) 0.0335(3) 0.0582(11) Uani 1 1 d . . . . .
N7 N 0.1694(4) 0.1238(3) -0.0560(4) 0.0597(11) Uani 1 1 d . . . . .
C1 C 0.3004(5) 0.1966(4) 0.2037(4) 0.0637(15) Uani 1 1 d . . . . .
H1A H 0.3291 0.1306 0.2231 0.076 Uiso 1 1 calc R U . . .
H1B H 0.2998 0.2360 0.2537 0.076 Uiso 1 1 calc R U . . .
C2 C 0.3895(5) 0.2406(4) 0.1085(4) 0.0594(14) Uani 1 1 d . . . . .
C3 C 0.4624(6) 0.3199(5) 0.1004(5) 0.0722(17) Uani 1 1 d . . . . .
H3 H 0.4581 0.3493 0.1550 0.087 Uiso 1 1 calc R U . . .
C4 C 0.5413(6) 0.3545(5) 0.0104(6) 0.0799(19) Uani 1 1 d . . . . .
H4 H 0.5892 0.4101 0.0021 0.096 Uiso 1 1 calc R U . . .
C5 C 0.5503(6) 0.3080(4) -0.0676(5) 0.0696(16) Uani 1 1 d . . . . .
H5 H 0.6060 0.3306 -0.1288 0.083 Uiso 1 1 calc R U . . .
C6 C 0.4767(5) 0.2276(4) -0.0555(4) 0.0579(14) Uani 1 1 d . . . . .
C7 C 0.4846(5) 0.1727(4) -0.1351(4) 0.0542(13) Uani 1 1 d . . . . .
C8 C 0.4609(5) 0.0717(4) -0.1157(4) 0.0614(15) Uani 1 1 d . . . . .
H8 H 0.4390 0.0397 -0.0511 0.074 Uiso 1 1 calc R U . . .
C9 C 0.4691(5) 0.0192(4) -0.1893(4) 0.0622(14) Uani 1 1 d . . . . .
H9 H 0.4535 -0.0484 -0.1746 0.075 Uiso 1 1 calc R U . . .
C10 C 0.5000(5) 0.0643(4) -0.2843(4) 0.0631(15) Uani 1 1 d . . . . .
H10 H 0.5045 0.0281 -0.3344 0.076 Uiso 1 1 calc R U . . .
C11 C 0.5244(5) 0.1642(4) -0.3059(4) 0.0560(13) Uani 1 1 d . . . . .
C12 C 0.5162(5) 0.2176(4) -0.2321(4) 0.0584(14) Uani 1 1 d . . . . .
H12 H 0.5320 0.2851 -0.2473 0.070 Uiso 1 1 calc R U . . .
C13 C 0.5578(5) 0.2109(4) -0.4076(4) 0.0599(14) Uani 1 1 d . . . . .
C16 C 0.1044(5) 0.1107(4) 0.2725(4) 0.0574(13) Uani 1 1 d . . . . .
H16A H 0.0150 0.1211 0.2856 0.069 Uiso 1 1 calc R U . . .
H16B H 0.1242 0.1094 0.3333 0.069 Uiso 1 1 calc R U . . .
C17 C 0.1416(5) 0.0156(4) 0.2348(4) 0.0540(13) Uani 1 1 d . . . . .
C18 C 0.1400(6) -0.0730(4) 0.2944(4) 0.0644(15) Uani 1 1 d . . . . .
H18 H 0.1221 -0.0763 0.3620 0.077 Uiso 1 1 calc R U . . .
C19 C 0.1656(6) -0.1568(4) 0.2511(6) 0.0758(18) Uani 1 1 d . . . . .
H19 H 0.1660 -0.2180 0.2896 0.091 Uiso 1 1 calc R U . . .
C20 C 0.1900(6) -0.1514(4) 0.1539(5) 0.0724(17) Uani 1 1 d . . . . .
H20 H 0.2043 -0.2085 0.1249 0.087 Uiso 1 1 calc R U . . .
C21 C 0.1935(5) -0.0616(4) 0.0987(4) 0.0623(14) Uani 1 1 d . . . . .
H21 H 0.2138 -0.0576 0.0309 0.075 Uiso 1 1 calc R U . . .
C22 C 0.1063(5) 0.2870(4) 0.2074(4) 0.0592(14) Uani 1 1 d . . . . .
H22A H 0.1322 0.3202 0.2523 0.071 Uiso 1 1 calc R U . . .
H22B H 0.0168 0.2765 0.2338 0.071 Uiso 1 1 calc R U . . .
C23 C 0.1354(5) 0.3498(4) 0.1097(5) 0.0584(14) Uani 1 1 d . . . . .
C24 C 0.1297(6) 0.4514(4) 0.0996(6) 0.0773(19) Uani 1 1 d . . . . .
H24 H 0.1100 0.4836 0.1543 0.093 Uiso 1 1 calc R U . . .
C25 C 0.1533(7) 0.5032(5) 0.0083(7) 0.094(2) Uani 1 1 d . . . . .
H25 H 0.1497 0.5720 -0.0004 0.113 Uiso 1 1 calc R U . . .
C26 C 0.1821(7) 0.4556(5) -0.0699(7) 0.092(2) Uani 1 1 d . . . . .
H26 H 0.1992 0.4914 -0.1328 0.110 Uiso 1 1 calc R U . . .
C27 C 0.1864(6) 0.3536(4) -0.0568(5) 0.0731(17) Uani 1 1 d . . . . .
H27 H 0.2054 0.3204 -0.1108 0.088 Uiso 1 1 calc R U . . .
C28 C 0.1613(5) 0.1053(4) -0.1257(4) 0.0554(13) Uani 1 1 d . . . . .
C29 C 0.1541(6) 0.0796(4) -0.2158(4) 0.0685(16) Uani 1 1 d . . . . .
H29A H 0.2269 0.1033 -0.2684 0.103 Uiso 1 1 calc R U . . .
H29B H 0.0806 0.1092 -0.2295 0.103 Uiso 1 1 calc R U . . .
H29C H 0.1500 0.0090 -0.2100 0.103 Uiso 1 1 calc R U . . .
Cl1 Cl -0.15134(13) 0.21091(9) 0.09883(10) 0.0584(4) Uani 1 1 d . . . . .
O2 O -0.0603(4) 0.1502(3) 0.1330(3) 0.0790(12) Uani 1 1 d . . . . .
O4 O -0.2567(4) 0.1539(3) 0.1131(3) 0.0813(12) Uani 1 1 d . . . . .
O3 O -0.0989(4) 0.2471(3) -0.0019(3) 0.0790(12) Uani 1 1 d . . . . .
O5 O -0.1820(5) 0.2918(3) 0.1521(3) 0.0868(13) Uani 1 1 d . . . . .
Cl2 Cl 0.22487(19) 0.06930(14) -0.48755(13) 0.0881(5) Uani 1 1 d . . . . .
O6 O 0.3195(7) 0.0559(6) -0.4401(5) 0.154(3) Uani 1 1 d . . . . .
O7 O 0.2718(7) 0.0335(7) -0.5719(5) 0.170(3) Uani 1 1 d . . . . .
O8 O 0.1218(7) 0.0202(8) -0.4296(7) 0.191(4) Uani 1 1 d . . . . .
O9 O 0.1978(14) 0.1646(6) -0.5126(11) 0.270(6) Uani 1 1 d . . . . .
Cl3 Cl 0.7453(3) 0.48775(16) -0.30837(16) 0.1120(8) Uani 1 1 d . . . . .
O10 O 0.7298(9) 0.4691(5) -0.3938(5) 0.161(3) Uani 1 1 d . . . . .
O11 O 0.7932(5) 0.4084(4) -0.2586(4) 0.1089(17) Uani 1 1 d . . . . .
O12 O 0.769(2) 0.5825(9) -0.3174(13) 0.120(5) Uani 0.5 1 d . . P A 1
O13 O 0.5976(12) 0.4821(12) -0.2561(13) 0.154(7) Uani 0.5 1 d . . P A 1
O12A O 0.871(2) 0.5505(11) -0.3518(11) 0.143(6) Uani 0.5 1 d . . P A 2
O13A O 0.6776(17) 0.5396(16) -0.2451(13) 0.151(6) Uani 0.5 1 d . . P A 2
N8 N -0.230(2) 0.6712(10) 0.2942(9) 0.259(9) Uani 1 1 d . . . . .
C30 C -0.1705(19) 0.6548(8) 0.3435(9) 0.180(7) Uani 1 1 d . . . . .
C31 C -0.0950(11) 0.6377(9) 0.4107(8) 0.149(4) Uani 1 1 d . . . . .
H31A H -0.0573 0.6987 0.4112 0.224 Uiso 1 1 calc R U . . .
H31B H -0.0308 0.5898 0.3895 0.224 Uiso 1 1 calc R U . . .
H31C H -0.1473 0.6136 0.4757 0.224 Uiso 1 1 calc R U . . .
O1 O 0.7353(5) 0.2889(4) -0.4123(4) 0.0809(14) Uani 0.85 1 d . . P B 1
N5 N 0.6397(6) 0.2805(4) -0.4522(4) 0.0632(14) Uani 0.85 1 d . . P B 1
N6 N 0.5096(6) 0.1872(4) -0.4739(4) 0.0645(15) Uani 0.85 1 d D . P B 1
H6N H 0.452(4) 0.139(3) -0.461(4) 0.039(15) Uiso 0.85 1 d D . P C 1
C14 C 0.6763(9) 0.2909(7) -0.5605(5) 0.072(2) Uani 0.85 1 d . . P B 1
C15 C 0.5535(7) 0.2521(6) -0.5687(5) 0.0722(19) Uani 0.85 1 d . . P B 1
C141 C 0.7092(12) 0.3934(7) -0.6059(7) 0.118(4) Uani 0.85 1 d . . P B 1
H14A H 0.7326 0.3980 -0.6760 0.177 Uiso 0.85 1 calc R U P B 1
H14B H 0.6385 0.4359 -0.5840 0.177 Uiso 0.85 1 calc R U P B 1
H14C H 0.7781 0.4134 -0.5873 0.177 Uiso 0.85 1 calc R U P B 1
C142 C 0.7835(7) 0.2225(7) -0.5932(6) 0.108(3) Uani 0.85 1 d . . P B 1
H14D H 0.7596 0.1561 -0.5625 0.162 Uiso 0.85 1 calc R U P B 1
H14E H 0.8069 0.2261 -0.6633 0.162 Uiso 0.85 1 calc R U P B 1
H14F H 0.8532 0.2412 -0.5749 0.162 Uiso 0.85 1 calc R U P B 1
C151 C 0.4524(8) 0.3303(7) -0.5676(7) 0.116(3) Uani 0.85 1 d . . P B 1
H15A H 0.4757 0.3755 -0.6281 0.175 Uiso 0.85 1 calc R U P B 1
H15B H 0.3750 0.2993 -0.5604 0.175 Uiso 0.85 1 calc R U P B 1
H15C H 0.4424 0.3657 -0.5137 0.175 Uiso 0.85 1 calc R U P B 1
C152 C 0.5686(9) 0.1957(8) -0.6520(6) 0.089(3) Uani 0.85 1 d . . P B 1
H15D H 0.5973 0.2394 -0.7131 0.134 Uiso 0.85 1 calc R U P B 1
H15E H 0.6285 0.1432 -0.6496 0.134 Uiso 0.85 1 calc R U P B 1
H15F H 0.4896 0.1683 -0.6466 0.134 Uiso 0.85 1 calc R U P B 1
O1A O 0.467(3) 0.370(3) -0.372(3) 0.098(10) Uiso 0.15 1 d . . P B 2
N5A N 0.539(3) 0.305(2) -0.428(2) 0.058(7) Uiso 0.15 1 d . . P B 2
N6A N 0.608(4) 0.172(3) -0.461(3) 0.082(10) Uiso 0.15 1 d . . P B 2
C14A C 0.560(4) 0.327(3) -0.537(3) 0.058(9) Uiso 0.15 1 d . . P B 2
C15A C 0.648(4) 0.250(3) -0.558(3) 0.041(10) Uiso 0.15 1 d . . P B 2
C143 C 0.588(5) 0.429(4) -0.557(4) 0.094(14) Uiso 0.15 1 d . . P B 2
C144 C 0.4524(8) 0.3303(7) -0.5676(7) 0.116(3) Uani 0.15 1 d . . P B 2
C153 C 0.7835(7) 0.2225(7) -0.5932(6) 0.108(3) Uani 0.15 1 d . . P B 2
C154 C 0.637(8) 0.176(6) -0.634(6) 0.13(3) Uiso 0.15 1 d . . P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N7 1.973(5) . ?
Cu1 N4 1.993(4) . ?
Cu1 N3 1.995(4) . ?
Cu1 N1 2.021(4) . ?
Cu1 N2 2.460(4) . ?
Cu1 O2 2.559(4) . ?
N1 C16 1.481(7) . ?
N1 C1 1.489(7) . ?
N1 C22 1.491(6) . ?
N2 C2 1.347(7) . ?
N2 C6 1.357(7) . ?
N3 C17 1.342(7) . ?
N3 C21 1.345(7) . ?
N4 C23 1.327(7) . ?
N4 C27 1.348(7) . ?
N7 C28 1.123(7) . ?
C1 C2 1.506(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 C3 1.381(8) . ?
C3 C4 1.374(9) . ?
C3 H3 0.9400 . ?
C4 C5 1.373(9) . ?
C4 H4 0.9400 . ?
C5 C6 1.387(8) . ?
C5 H5 0.9400 . ?
C6 C7 1.470(8) . ?
C7 C12 1.398(8) . ?
C7 C8 1.406(7) . ?
C8 C9 1.372(8) . ?
C8 H8 0.9400 . ?
C9 C10 1.375(8) . ?
C9 H9 0.9400 . ?
C10 C11 1.392(8) . ?
C10 H10 0.9400 . ?
C11 C12 1.383(8) . ?
C11 C13 1.465(8) . ?
C12 H12 0.9400 . ?
C13 N6A 1.03(4) . ?
C13 N5A 1.31(3) . ?
C13 N5 1.322(8) . ?
C13 N6 1.341(8) . ?
C16 C17 1.499(7) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C17 C18 1.383(7) . ?
C18 C19 1.385(9) . ?
C18 H18 0.9400 . ?
C19 C20 1.353(9) . ?
C19 H19 0.9400 . ?
C20 C21 1.363(8) . ?
C20 H20 0.9400 . ?
C21 H21 0.9400 . ?
C22 C23 1.498(8) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C23 C24 1.392(8) . ?
C24 C25 1.365(10) . ?
C24 H24 0.9400 . ?
C25 C26 1.357(11) . ?
C25 H25 0.9400 . ?
C26 C27 1.395(9) . ?
C26 H26 0.9400 . ?
C27 H27 0.9400 . ?
C28 C29 1.447(8) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 H29C 0.9700 . ?
Cl1 O4 1.415(4) . ?
Cl1 O3 1.426(4) . ?
Cl1 O5 1.433(4) . ?
Cl1 O2 1.451(4) . ?
Cl2 O7 1.348(6) . ?
Cl2 O9 1.354(9) . ?
Cl2 O8 1.359(7) . ?
Cl2 O6 1.438(6) . ?
Cl3 O13A 1.295(13) . ?
Cl3 O12 1.334(11) . ?
Cl3 O10 1.381(7) . ?
Cl3 O11 1.396(5) . ?
Cl3 O12A 1.614(18) . ?
Cl3 O13 1.616(13) . ?
N8 C30 1.12(2) . ?
C30 C31 1.476(19) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 H31C 0.9700 . ?
O1 N5 1.400(7) . ?
N5 C14 1.494(9) . ?
N6 C15 1.484(9) . ?
N6 H6N 0.92(2) . ?
C14 C141 1.483(12) . ?
C14 C142 1.504(12) . ?
C14 C15 1.569(12) . ?
C15 C152 1.513(11) . ?
C15 C151 1.530(11) . ?
C141 H14A 0.9700 . ?
C141 H14B 0.9700 . ?
C141 H14C 0.9700 . ?
C142 H14D 0.9700 . ?
C142 H14E 0.9700 . ?
C142 H14F 0.9700 . ?
C151 H15A 0.9700 . ?
C151 H15B 0.9700 . ?
C151 H15C 0.9700 . ?
C152 H15D 0.9700 . ?
C152 H15E 0.9700 . ?
C152 H15F 0.9700 . ?
O1A N5A 1.36(4) . ?
N5A C14A 1.52(5) . ?
N6A C15A 1.60(6) . ?
C14A C15A 1.42(6) . ?
C14A C143 1.42(6) . ?
C14A C144 1.43(4) . ?
C15A C153 1.51(4) . ?
C15A C154 1.67(9) . ?

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
N7 Cu1 N4 97.13(19) . . ?
N7 Cu1 N3 96.47(18) . . ?
N4 Cu1 N3 164.82(19) . . ?
N7 Cu1 N1 176.56(18) . . ?
N4 Cu1 N1 83.57(17) . . ?
N3 Cu1 N1 82.46(17) . . ?
N7 Cu1 N2 102.58(17) . . ?
N4 Cu1 N2 82.78(16) . . ?
N3 Cu1 N2 100.80(16) . . ?
N1 Cu1 N2 80.85(16) . . ?
N7 Cu1 O2 89.55(17) . . ?
N4 Cu1 O2 89.17(16) . . ?
N3 Cu1 O2 84.21(15) . . ?
N1 Cu1 O2 87.09(16) . . ?
N2 Cu1 O2 166.15(15) . . ?
C16 N1 C1 110.1(4) . . ?
C16 N1 C22 112.5(4) . . ?
C1 N1 C22 111.3(4) . . ?
C16 N1 Cu1 106.4(3) . . ?
C1 N1 Cu1 110.1(3) . . ?
C22 N1 Cu1 106.3(3) . . ?
C2 N2 C6 119.0(5) . . ?
C2 N2 Cu1 99.5(3) . . ?
C6 N2 Cu1 126.6(3) . . ?
C17 N3 C21 118.8(5) . . ?
C17 N3 Cu1 113.8(3) . . ?
C21 N3 Cu1 127.3(4) . . ?
C23 N4 C27 120.0(5) . . ?
C23 N4 Cu1 113.5(4) . . ?
C27 N4 Cu1 126.4(4) . . ?
C28 N7 Cu1 177.5(5) . . ?
N1 C1 C2 112.6(4) . . ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
N2 C2 C3 122.6(6) . . ?
N2 C2 C1 114.9(5) . . ?
C3 C2 C1 122.4(6) . . ?
C4 C3 C2 118.0(6) . . ?
C4 C3 H3 121.0 . . ?
C2 C3 H3 121.0 . . ?
C5 C4 C3 120.2(6) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 119.6(6) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
N2 C6 C5 120.5(6) . . ?
N2 C6 C7 117.0(5) . . ?
C5 C6 C7 122.4(5) . . ?
C12 C7 C8 117.6(5) . . ?
C12 C7 C6 122.0(5) . . ?
C8 C7 C6 120.4(5) . . ?
C9 C8 C7 121.1(5) . . ?
C9 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
C8 C9 C10 120.7(5) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C9 C10 C11 119.5(6) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C12 C11 C10 120.2(5) . . ?
C12 C11 C13 121.1(5) . . ?
C10 C11 C13 118.7(5) . . ?
C11 C12 C7 120.9(5) . . ?
C11 C12 H12 119.5 . . ?
C7 C12 H12 119.5 . . ?
N6A C13 N5A 121(3) . . ?
N5 C13 N6 107.3(5) . . ?
N6A C13 C11 119(2) . . ?
N5A C13 C11 119.2(14) . . ?
N5 C13 C11 128.3(5) . . ?
N6 C13 C11 124.4(5) . . ?
N1 C16 C17 108.8(4) . . ?
N1 C16 H16A 109.9 . . ?
C17 C16 H16A 109.9 . . ?
N1 C16 H16B 109.9 . . ?
C17 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
N3 C17 C18 121.8(5) . . ?
N3 C17 C16 114.8(4) . . ?
C18 C17 C16 123.3(5) . . ?
C17 C18 C19 117.7(6) . . ?
C17 C18 H18 121.2 . . ?
C19 C18 H18 121.2 . . ?
C20 C19 C18 120.7(5) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C20 C21 118.8(6) . . ?
C19 C20 H20 120.6 . . ?
C21 C20 H20 120.6 . . ?
N3 C21 C20 122.3(6) . . ?
N3 C21 H21 118.9 . . ?
C20 C21 H21 118.9 . . ?
N1 C22 C23 110.0(4) . . ?
N1 C22 H22A 109.7 . . ?
C23 C22 H22A 109.7 . . ?
N1 C22 H22B 109.7 . . ?
C23 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
N4 C23 C24 121.8(6) . . ?
N4 C23 C22 116.2(4) . . ?
C24 C23 C22 121.9(6) . . ?
C25 C24 C23 118.4(7) . . ?
C25 C24 H24 120.8 . . ?
C23 C24 H24 120.8 . . ?
C26 C25 C24 120.1(6) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C27 119.9(7) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
N4 C27 C26 119.8(7) . . ?
N4 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
N7 C28 C29 178.3(6) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O4 Cl1 O3 110.1(3) . . ?
O4 Cl1 O5 111.3(3) . . ?
O3 Cl1 O5 109.1(3) . . ?
O4 Cl1 O2 109.0(3) . . ?
O3 Cl1 O2 109.1(3) . . ?
O5 Cl1 O2 108.2(3) . . ?
Cl1 O2 Cu1 128.9(2) . . ?
O7 Cl2 O9 105.7(7) . . ?
O7 Cl2 O8 111.4(6) . . ?
O9 Cl2 O8 110.8(8) . . ?
O7 Cl2 O6 106.3(5) . . ?
O9 Cl2 O6 113.3(7) . . ?
O8 Cl2 O6 109.3(5) . . ?
O13A Cl3 O10 129.7(9) . . ?
O12 Cl3 O10 109.0(7) . . ?
O13A Cl3 O11 108.0(9) . . ?
O12 Cl3 O11 128.1(7) . . ?
O10 Cl3 O11 113.7(4) . . ?
O13A Cl3 O12A 101.8(11) . . ?
O10 Cl3 O12A 99.7(7) . . ?
O11 Cl3 O12A 97.0(8) . . ?
O12 Cl3 O13 103.2(11) . . ?
O10 Cl3 O13 90.7(8) . . ?
O11 Cl3 O13 104.3(5) . . ?
N8 C30 C31 177.1(18) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C13 N5 O1 116.9(5) . . ?
C13 N5 C14 113.6(6) . . ?
O1 N5 C14 115.9(6) . . ?
C13 N6 C15 112.3(6) . . ?
C13 N6 H6N 124(3) . . ?
C15 N6 H6N 123(3) . . ?
C141 C14 N5 111.2(7) . . ?
C141 C14 C142 111.1(9) . . ?
N5 C14 C142 108.0(6) . . ?
C141 C14 C15 116.3(8) . . ?
N5 C14 C15 97.5(6) . . ?
C142 C14 C15 111.6(8) . . ?
N6 C15 C152 110.8(7) . . ?
N6 C15 C151 105.4(6) . . ?
C152 C15 C151 109.8(7) . . ?
N6 C15 C14 100.5(6) . . ?
C152 C15 C14 115.6(7) . . ?
C151 C15 C14 114.0(7) . . ?
C14 C141 H14A 109.5 . . ?
C14 C141 H14B 109.5 . . ?
H14A C141 H14B 109.5 . . ?
C14 C141 H14C 109.5 . . ?
H14A C141 H14C 109.5 . . ?
H14B C141 H14C 109.5 . . ?
C14 C142 H14D 109.5 . . ?
C14 C142 H14E 109.5 . . ?
H14D C142 H14E 109.5 . . ?
C14 C142 H14F 109.5 . . ?
H14D C142 H14F 109.5 . . ?
H14E C142 H14F 109.5 . . ?
C15 C151 H15A 109.5 . . ?
C15 C151 H15B 109.5 . . ?
H15A C151 H15B 109.5 . . ?
C15 C151 H15C 109.5 . . ?
H15A C151 H15C 109.5 . . ?
H15B C151 H15C 109.5 . . ?
C15 C152 H15D 109.5 . . ?
C15 C152 H15E 109.5 . . ?
H15D C152 H15E 109.5 . . ?
C15 C152 H15F 109.5 . . ?
H15D C152 H15F 109.5 . . ?
H15E C152 H15F 109.5 . . ?
C13 N5A O1A 131(3) . . ?
C13 N5A C14A 106(2) . . ?
O1A N5A C14A 118(3) . . ?
C13 N6A C15A 105(3) . . ?
C15A C14A C143 125(4) . . ?
C15A C14A C144 119(3) . . ?
C143 C14A C144 99(3) . . ?
C15A C14A N5A 95(3) . . ?
C143 C14A N5A 102(3) . . ?
C144 C14A N5A 116(3) . . ?
C14A C15A C153 146(4) . . ?
C14A C15A N6A 103(3) . . ?
C153 C15A N6A 99(3) . . ?
C14A C15A C154 120(4) . . ?
C153 C15A C154 83(3) . . ?
N6A C15A C154 97(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
C16 N1 C1 C2 153.9(4) . . . . ?
C22 N1 C1 C2 -80.6(6) . . . . ?
Cu1 N1 C1 C2 37.0(5) . . . . ?
C6 N2 C2 C3 -0.9(8) . . . . ?
Cu1 N2 C2 C3 -142.6(5) . . . . ?
C6 N2 C2 C1 -178.4(4) . . . . ?
Cu1 N2 C2 C1 40.0(5) . . . . ?
N1 C1 C2 N2 -57.0(6) . . . . ?
N1 C1 C2 C3 125.6(6) . . . . ?
N2 C2 C3 C4 2.4(9) . . . . ?
C1 C2 C3 C4 179.7(5) . . . . ?
C2 C3 C4 C5 -2.8(10) . . . . ?
C3 C4 C5 C6 1.8(10) . . . . ?
C2 N2 C6 C5 -0.2(7) . . . . ?
Cu1 N2 C6 C5 130.1(5) . . . . ?
C2 N2 C6 C7 177.7(4) . . . . ?
Cu1 N2 C6 C7 -52.0(6) . . . . ?
C4 C5 C6 N2 -0.2(9) . . . . ?
C4 C5 C6 C7 -178.0(5) . . . . ?
N2 C6 C7 C12 151.0(5) . . . . ?
C5 C6 C7 C12 -31.1(8) . . . . ?
N2 C6 C7 C8 -29.4(7) . . . . ?
C5 C6 C7 C8 148.5(5) . . . . ?
C12 C7 C8 C9 0.3(7) . . . . ?
C6 C7 C8 C9 -179.3(5) . . . . ?
C7 C8 C9 C10 -0.5(8) . . . . ?
C8 C9 C10 C11 0.7(8) . . . . ?
C9 C10 C11 C12 -0.8(8) . . . . ?
C9 C10 C11 C13 179.7(5) . . . . ?
C10 C11 C12 C7 0.7(8) . . . . ?
C13 C11 C12 C7 -179.8(5) . . . . ?
C8 C7 C12 C11 -0.4(7) . . . . ?
C6 C7 C12 C11 179.2(5) . . . . ?
C12 C11 C13 N6A 147(3) . . . . ?
C10 C11 C13 N6A -33(3) . . . . ?
C12 C11 C13 N5A -23.5(18) . . . . ?
C10 C11 C13 N5A 156.0(17) . . . . ?
C12 C11 C13 N5 38.5(9) . . . . ?
C10 C11 C13 N5 -142.0(6) . . . . ?
C12 C11 C13 N6 -143.1(6) . . . . ?
C10 C11 C13 N6 36.4(8) . . . . ?
C1 N1 C16 C17 -79.9(5) . . . . ?
C22 N1 C16 C17 155.4(4) . . . . ?
Cu1 N1 C16 C17 39.4(5) . . . . ?
C21 N3 C17 C18 1.0(8) . . . . ?
Cu1 N3 C17 C18 -176.1(4) . . . . ?
C21 N3 C17 C16 -174.6(5) . . . . ?
Cu1 N3 C17 C16 8.2(6) . . . . ?
N1 C16 C17 N3 -32.5(6) . . . . ?
N1 C16 C17 C18 152.0(5) . . . . ?
N3 C17 C18 C19 -1.1(9) . . . . ?
C16 C17 C18 C19 174.2(5) . . . . ?
C17 C18 C19 C20 -0.7(9) . . . . ?
C18 C19 C20 C21 2.4(10) . . . . ?
C17 N3 C21 C20 0.9(8) . . . . ?
Cu1 N3 C21 C20 177.6(4) . . . . ?
C19 C20 C21 N3 -2.6(9) . . . . ?
C16 N1 C22 C23 -150.4(4) . . . . ?
C1 N1 C22 C23 85.5(5) . . . . ?
Cu1 N1 C22 C23 -34.4(5) . . . . ?
C27 N4 C23 C24 -0.2(8) . . . . ?
Cu1 N4 C23 C24 176.1(4) . . . . ?
C27 N4 C23 C22 177.8(5) . . . . ?
Cu1 N4 C23 C22 -6.0(6) . . . . ?
N1 C22 C23 N4 27.9(7) . . . . ?
N1 C22 C23 C24 -154.2(5) . . . . ?
N4 C23 C24 C25 0.1(9) . . . . ?
C22 C23 C24 C25 -177.8(6) . . . . ?
C23 C24 C25 C26 -0.3(11) . . . . ?
C24 C25 C26 C27 0.6(11) . . . . ?
C23 N4 C27 C26 0.4(9) . . . . ?
Cu1 N4 C27 C26 -175.2(5) . . . . ?
C25 C26 C27 N4 -0.7(10) . . . . ?
O4 Cl1 O2 Cu1 147.2(3) . . . . ?
O3 Cl1 O2 Cu1 27.0(4) . . . . ?
O5 Cl1 O2 Cu1 -91.6(4) . . . . ?
N6 C13 N5 O1 -154.4(5) . . . . ?
C11 C13 N5 O1 24.3(9) . . . . ?
N6 C13 N5 C14 -15.2(8) . . . . ?
C11 C13 N5 C14 163.4(6) . . . . ?
N5 C13 N6 C15 -5.8(8) . . . . ?
C11 C13 N6 C15 175.5(6) . . . . ?
C13 N5 C14 C141 149.6(8) . . . . ?
O1 N5 C14 C141 -70.8(9) . . . . ?
C13 N5 C14 C142 -88.2(8) . . . . ?
O1 N5 C14 C142 51.4(9) . . . . ?
C13 N5 C14 C15 27.5(8) . . . . ?
O1 N5 C14 C15 167.1(6) . . . . ?
C13 N6 C15 C152 144.9(7) . . . . ?
C13 N6 C15 C151 -96.5(7) . . . . ?
C13 N6 C15 C14 22.2(8) . . . . ?
C141 C14 C15 N6 -145.0(8) . . . . ?
N5 C14 C15 N6 -26.8(7) . . . . ?
C142 C14 C15 N6 86.0(7) . . . . ?
C141 C14 C15 C152 95.7(10) . . . . ?
N5 C14 C15 C152 -146.1(7) . . . . ?
C142 C14 C15 C152 -33.3(9) . . . . ?
C141 C14 C15 C151 -32.9(10) . . . . ?
N5 C14 C15 C151 85.3(7) . . . . ?
C142 C14 C15 C151 -161.9(7) . . . . ?
N6A C13 N5A O1A 173(4) . . . . ?
C11 C13 N5A O1A -16(4) . . . . ?
N6A C13 N5A C14A 19(4) . . . . ?
C11 C13 N5A C14A -170.1(18) . . . . ?
N5A C13 N6A C15A 1(4) . . . . ?
C11 C13 N6A C15A -169.7(19) . . . . ?
C13 N5A C14A C15A -29(3) . . . . ?
O1A N5A C14A C15A 173(3) . . . . ?
C13 N5A C14A C143 -157(3) . . . . ?
O1A N5A C14A C143 45(4) . . . . ?
C13 N5A C14A C144 96(3) . . . . ?
O1A N5A C14A C144 -61(4) . . . . ?
C143 C14A C15A C153 8(9) . . . . ?
C144 C14A C15A C153 136(5) . . . . ?
N5A C14A C15A C153 -101(6) . . . . ?
C143 C14A C15A N6A 136(4) . . . . ?
C144 C14A C15A N6A -95(4) . . . . ?
N5A C14A C15A N6A 28(4) . . . . ?
C143 C14A C15A C154 -118(6) . . . . ?
C144 C14A C15A C154 10(6) . . . . ?
N5A C14A C15A C154 133(4) . . . . ?
C13 N6A C15A C14A -22(4) . . . . ?
C13 N6A C15A C153 132(3) . . . . ?
C13 N6A C15A C154 -145(4) . . . . ?

_refine_diff_density_max         0.516
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.082

