# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pCZn2ONO
_database_code_depnum_ccdc_archive 'CCDC 1884272'
_audit_update_record             
;
2018-12-11 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT088_pCZn2ONO            
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.14 Note  
RESPONSE: There are a large number of disordered atoms in the model which 
greatly increases the number of parameters refined.  The disorder combined 
with the high symmetry space group, which limits the number of unique 
reflections possible, results in a poor data/parameter ratio.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H54 N9 O2 Zn2, 3(Cl O4)'
_chemical_formula_sum            'C36 H54 Cl3 N9 O14 Zn2'
_chemical_formula_weight         1073.97

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_H-M_alt        'P -3 1 c'
_space_group_name_Hall           '-P 3 2c'

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

_cell_length_a                   9.758(2)
_cell_length_b                   9.758(2)
_cell_length_c                   26.267(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2166.2(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2215
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      22.24
_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_F_000             1112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.370
_shelx_estimated_absorpt_T_min   0.771
_shelx_estimated_absorpt_T_max   0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6132
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_measurement_device       'Bruker APEX ApexII CCD'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21530
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_av_R_equivalents  0.0922
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         0.775
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_full        25.242
_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             1341
_reflns_number_gt                1212
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_reduction        
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2016) 
;
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELX-2018-1 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXLE v932 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
Refined as a 2-component twin.

Structure was phased by direct methods (Sheldrick, 2015).  Systematic 
conditions suggested the ambiguous space group.  The space group choice 
was confirmed by successful convergence of the full-matrix least-squares 
refinement on F².  The highest peaks in the final difference Fourier 
map were in the vicinity of ClO4 anions; the final map had no other 
significant features.  A final analysis of variance between observed and 
calculated structure factors showed some dependence on amplitude and 
little dependence on resolution. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0966P)²+37.2634P] 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         1341
_refine_ls_number_parameters     324
_refine_ls_number_restraints     960
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0961
_refine_ls_wR_factor_ref         0.2518
_refine_ls_wR_factor_gt          0.2457
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_restrained_S_all      0.917
_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
Zn1 Zn 0.333333 0.666667 0.13493(7) 0.0196(6) Uani 1 3 d DS T P . .
O1 O 0.291(11) 0.667(12) 0.206(2) 0.021(13) Uani 0.1667 1 d D U P A -1
O2 O 0.284(8) 0.649(13) 0.286(2) 0.015(12) Uani 0.1667 1 d D U P A -1
N4 N 0.367(3) 0.701(6) 0.247(3) 0.015(12) Uani 0.1667 1 d D U P A -1
N1 N 0.333333 0.666667 0.0509(5) 0.025(3) Uani 1 3 d DS T P A .
C1 C 0.227(5) 0.723(7) 0.0340(15) 0.022(5) Uani 0.39(3) 1 d D U P A -1
H1A H 0.194507 0.690816 -0.001751 0.026 Uiso 0.39(3) 1 calc R U P A -1
H1B H 0.281180 0.839758 0.035996 0.026 Uiso 0.39(3) 1 calc R U P A -1
C2 C 0.079(4) 0.647(5) 0.0697(16) 0.021(4) Uani 0.39(3) 1 d D U P A -1
H2A H 0.005395 0.685304 0.059912 0.025 Uiso 0.39(3) 1 calc R U P A -1
H2B H 0.022183 0.530811 0.066295 0.025 Uiso 0.39(3) 1 calc R U P A -1
N2 N 0.131(4) 0.693(4) 0.1238(15) 0.022(4) Uani 0.39(3) 1 d D U P A -1
H2 H 0.045520 0.612341 0.145800 0.026 Uiso 0.39(3) 1 calc R U P A -1
C3 C 0.146(5) 0.842(5) 0.1364(11) 0.022(4) Uani 0.39(3) 1 d D U P A -1
H3A H 0.048951 0.842758 0.125917 0.027 Uiso 0.39(3) 1 calc R U P A -1
H3B H 0.236493 0.927408 0.117650 0.027 Uiso 0.39(3) 1 calc R U P A -1
C4 C 0.172(4) 0.874(5) 0.1934(12) 0.020(3) Uani 0.39(3) 1 d D U P A -1
C5 C 0.048(4) 0.761(5) 0.2274(12) 0.020(4) Uani 0.39(3) 1 d D U P A -1
H5 H -0.043218 0.670336 0.214740 0.024 Uiso 0.39(3) 1 calc R U P A -1
C6 C 0.072(4) 0.794(5) 0.2809(12) 0.021(4) Uani 0.39(3) 1 d D U P A -1
H6 H -0.013431 0.735582 0.303633 0.025 Uiso 0.39(3) 1 calc R U P A -1
C7 C 0.219(4) 0.909(5) 0.3008(12) 0.018(3) Uani 0.39(3) 1 d D U P A -1
C8 C 0.334(4) 1.003(4) 0.2667(11) 0.020(4) Uani 0.39(3) 1 d D U P A -1
H8 H 0.433377 1.082185 0.279714 0.023 Uiso 0.39(3) 1 calc R U P A -1
C9 C 0.314(4) 0.989(4) 0.2136(12) 0.022(4) Uani 0.39(3) 1 d D U P A -1
H9 H 0.397735 1.058995 0.191734 0.026 Uiso 0.39(3) 1 calc R U P A -1
C10 C 0.231(5) 0.919(5) 0.3569(11) 0.019(3) Uani 0.39(3) 1 d D U P A -1
H10A H 0.131014 0.835602 0.372201 0.022 Uiso 0.39(3) 1 calc R U P A -1
H10B H 0.248148 1.023149 0.368410 0.022 Uiso 0.39(3) 1 calc R U P A -1
N3 N 0.371(4) 0.897(4) 0.3744(12) 0.018(4) Uani 0.39(3) 1 d D U P A -1
H3 H 0.463504 0.968171 0.352409 0.021 Uiso 0.39(3) 1 calc R U P A -1
C11 C 0.419(4) 0.948(4) 0.4270(12) 0.017(4) Uani 0.39(3) 1 d D U P A -1
H11A H 0.403176 1.037703 0.435589 0.020 Uiso 0.39(3) 1 calc R U P A -1
H11B H 0.531701 0.980782 0.431941 0.020 Uiso 0.39(3) 1 calc R U P A -1
C12 C 0.311(8) 0.801(5) 0.4613(13) 0.019(5) Uani 0.39(3) 1 d D U P A -1
H12A H 0.337121 0.829355 0.497568 0.023 Uiso 0.39(3) 1 calc R U P A -1
H12B H 0.198619 0.769456 0.456062 0.023 Uiso 0.39(3) 1 calc R U P A -1
C1B C 0.232(16) 0.72(2) 0.029(4) 0.021(6) Uani 0.11(3) 1 d D U P A -2
H1C H 0.213523 0.698353 -0.007625 0.026 Uiso 0.11(3) 1 calc R U P A -2
H1D H 0.276451 0.837314 0.034556 0.026 Uiso 0.11(3) 1 calc R U P A -2
C2B C 0.077(12) 0.623(16) 0.061(3) 0.021(5) Uani 0.11(3) 1 d D U P A -2
H2C H -0.002958 0.653175 0.051025 0.026 Uiso 0.11(3) 1 calc R U P A -2
H2D H 0.031841 0.509071 0.053481 0.026 Uiso 0.11(3) 1 calc R U P A -2
N2B N 0.114(10) 0.654(14) 0.116(3) 0.022(4) Uani 0.11(3) 1 d D U P A -2
H2E H 0.033020 0.552999 0.132867 0.026 Uiso 0.11(3) 1 calc R U P A -2
C3B C 0.075(17) 0.768(14) 0.135(2) 0.022(4) Uani 0.11(3) 1 d D U P A -2
H3C H -0.035671 0.734438 0.126361 0.026 Uiso 0.11(3) 1 calc R U P A -2
H3D H 0.144595 0.871264 0.118957 0.026 Uiso 0.11(3) 1 calc R U P A -2
C4B C 0.096(15) 0.785(10) 0.193(2) 0.021(4) Uani 0.11(3) 1 d D U P A -2
C5B C -0.008(14) 0.648(8) 0.224(3) 0.021(5) Uani 0.11(3) 1 d D U P A -2
H5B H -0.091009 0.553573 0.209464 0.026 Uiso 0.11(3) 1 calc R U P A -2
C6B C 0.021(13) 0.664(8) 0.278(3) 0.021(5) Uani 0.11(3) 1 d D U P A -2
H6B H -0.021366 0.571042 0.298395 0.025 Uiso 0.11(3) 1 calc R U P A -2
C7B C 0.110(13) 0.813(9) 0.301(2) 0.020(4) Uani 0.11(3) 1 d D U P A -2
C8B C 0.180(14) 0.942(7) 0.269(2) 0.020(4) Uani 0.11(3) 1 d D U P A -2
H8B H 0.226578 1.043944 0.284282 0.024 Uiso 0.11(3) 1 calc R U P A -2
C9B C 0.188(14) 0.931(9) 0.216(2) 0.021(4) Uani 0.11(3) 1 d D U P A -2
H9B H 0.254509 1.021715 0.196556 0.025 Uiso 0.11(3) 1 calc R U P A -2
C10B C 0.112(9) 0.816(10) 0.357(2) 0.020(4) Uani 0.11(3) 1 d D U P A -2
H10C H 0.026022 0.713852 0.370625 0.024 Uiso 0.11(3) 1 calc R U P A -2
H10D H 0.094247 0.901373 0.369651 0.024 Uiso 0.11(3) 1 calc R U P A -2
N3B N 0.275(11) 0.844(10) 0.376(3) 0.019(4) Uani 0.11(3) 1 d D U P A -2
H3E H 0.349367 0.927965 0.352655 0.022 Uiso 0.11(3) 1 calc R U P A -2
C11B C 0.321(12) 0.925(9) 0.425(3) 0.018(5) Uani 0.11(3) 1 d D U P A -2
H11C H 0.247115 0.961676 0.435698 0.022 Uiso 0.11(3) 1 calc R U P A -2
H11D H 0.429285 1.018170 0.423427 0.022 Uiso 0.11(3) 1 calc R U P A -2
C12B C 0.32(3) 0.801(16) 0.465(3) 0.018(5) Uani 0.11(3) 1 d D U P A -2
H12C H 0.400101 0.861273 0.490240 0.022 Uiso 0.11(3) 1 calc R U P A -2
H12D H 0.213945 0.757195 0.483040 0.022 Uiso 0.11(3) 1 calc R U P A -2
Cl1 Cl 0.666667 0.333333 0.1293(4) 0.0263(14) Uani 0.769(16) 3 d DS TU P B 1
O3 O 0.666667 0.333333 0.0737(5) 0.042(4) Uani 0.769(16) 3 d DS TU P B 1
O4 O 0.6840(18) 0.4833(15) 0.1467(6) 0.064(3) Uani 0.769(16) 1 d D U P B 1
Cl1B Cl 0.666667 0.333333 0.1264(16) 0.033(4) Uani 0.231(16) 3 d DS TU P B 2
O3B O 0.666667 0.333333 0.1822(16) 0.043(6) Uani 0.231(16) 3 d DS TU P B 2
O4B O 0.708(5) 0.488(3) 0.1052(14) 0.043(6) Uani 0.231(16) 1 d D U P B 2
Cl2 Cl 0.000000 0.000000 0.000000 0.088(3) Uani 1 6 d DS TU P . .
O5 O 0.1101(18) 0.1426(16) -0.0291(6) 0.064(3) Uani 0.6667 1 d D U 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.
;

_exptl_special_details           
; 
One distinct cell was identified using APEX3 (Bruker, 2016).  Five 
frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2016) then corrected for absorption by integration 
using SAINT/SADABS v2014/2 (Bruker, 2016) to sort, merge, and scale 
the combined data.  No decay correction was applied.    
;

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
Zn1 O1 1.92(6) . ?
Zn1 N2 2.13(3) . ?
Zn1 N2B 2.14(6) . ?
Zn1 N1 2.206(14) . ?
O1 N4 1.249(11) . ?
O2 N4 1.248(11) . ?
N1 C1B 1.464(15) . ?
N1 C1 1.465(14) . ?
C1 C2 1.57(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N2 1.50(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
N2 C3 1.43(4) . ?
N2 H2 1.0000 . ?
C3 C4 1.52(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C9 1.39(5) . ?
C4 C5 1.46(5) . ?
C5 C6 1.43(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.41(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.37(4) . ?
C7 C10 1.48(4) . ?
C8 C9 1.40(4) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 N3 1.56(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
N3 C11 1.46(4) . ?
N3 H3 1.0000 . ?
C11 C12 1.57(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C1B C2B 1.57(4) . ?
C1B H1C 0.9900 . ?
C1B H1D 0.9900 . ?
C2B N2B 1.50(4) . ?
C2B H2C 0.9900 . ?
C2B H2D 0.9900 . ?
N2B C3B 1.43(4) . ?
N2B H2E 1.0000 . ?
C3B C4B 1.52(4) . ?
C3B H3C 0.9900 . ?
C3B H3D 0.9900 . ?
C4B C9B 1.39(5) . ?
C4B C5B 1.46(5) . ?
C5B C6B 1.44(4) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.41(4) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.37(4) . ?
C7B C10B 1.48(4) . ?
C8B C9B 1.41(4) . ?
C8B H8B 0.9500 . ?
C9B H9B 0.9500 . ?
C10B N3B 1.55(4) . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
N3B C11B 1.46(4) . ?
N3B H3E 1.0000 . ?
C11B C12B 1.57(5) . ?
C11B H11C 0.9900 . ?
C11B H11D 0.9900 . ?
C12B H12C 0.9900 . ?
C12B H12D 0.9900 . ?
Cl1 O4 1.460(11) 3_665 ?
Cl1 O4 1.460(11) 2_655 ?
Cl1 O4 1.460(11) . ?
Cl1 O3 1.461(12) . ?
Cl1B O4B 1.464(13) 3_665 ?
Cl1B O4B 1.464(13) . ?
Cl1B O4B 1.464(13) 2_655 ?
Cl1B O3B 1.465(13) . ?
Cl2 O5 1.477(12) 8 ?
Cl2 O5 1.477(12) 2 ?
Cl2 O5 1.477(12) 7 ?
Cl2 O5 1.477(12) 9 ?
Cl2 O5 1.477(12) 3 ?
Cl2 O5 1.477(12) . ?

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 Zn1 N2 86(2) . . ?
O1 Zn1 N1 168(2) . . ?
N2 Zn1 N1 82.1(11) . . ?
N2B Zn1 N1 77(2) . . ?
N4 O1 Zn1 137(7) . . ?
O2 N4 O1 114(3) . . ?
C1B N1 Zn1 113(4) . . ?
C1 N1 Zn1 107.7(17) . . ?
N1 C1 C2 108(2) . . ?
N1 C1 H1A 110.2 . . ?
C2 C1 H1A 110.2 . . ?
N1 C1 H1B 110.2 . . ?
C2 C1 H1B 110.2 . . ?
H1A C1 H1B 108.5 . . ?
N2 C2 C1 109(2) . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
C3 N2 C2 112(2) . . ?
C3 N2 Zn1 118(2) . . ?
C2 N2 Zn1 107(2) . . ?
C3 N2 H2 106.6 . . ?
C2 N2 H2 106.6 . . ?
Zn1 N2 H2 106.6 . . ?
N2 C3 C4 111(3) . . ?
N2 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
N2 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C9 C4 C5 119(3) . . ?
C9 C4 C3 122(3) . . ?
C5 C4 C3 117(3) . . ?
C6 C5 C4 117(3) . . ?
C6 C5 H5 121.6 . . ?
C4 C5 H5 121.6 . . ?
C7 C6 C5 122(3) . . ?
C7 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C8 C7 C6 117(3) . . ?
C8 C7 C10 127(3) . . ?
C6 C7 C10 116(3) . . ?
C7 C8 C9 124(3) . . ?
C7 C8 H8 118.1 . . ?
C9 C8 H8 118.1 . . ?
C4 C9 C8 120(3) . . ?
C4 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C7 C10 N3 109(2) . . ?
C7 C10 H10A 109.8 . . ?
N3 C10 H10A 109.8 . . ?
C7 C10 H10B 109.8 . . ?
N3 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
C11 N3 C10 113(2) . . ?
C11 N3 Zn1 109(2) . 4_665 ?
C10 N3 Zn1 115(3) . 4_665 ?
C11 N3 H3 106.7 . . ?
C10 N3 H3 106.7 . . ?
Zn1 N3 H3 106.7 4_665 . ?
N3 C11 C12 106(3) . . ?
N3 C11 H11A 110.5 . . ?
C12 C11 H11A 110.5 . . ?
N3 C11 H11B 110.5 . . ?
C12 C11 H11B 110.5 . . ?
H11A C11 H11B 108.7 . . ?
N1 C12 C11 111(3) 4_665 . ?
N1 C12 H12A 109.4 4_665 . ?
C11 C12 H12A 109.4 . . ?
N1 C12 H12B 109.4 4_665 . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
N1 C1B C2B 101(6) . . ?
N1 C1B H1C 111.6 . . ?
C2B C1B H1C 111.6 . . ?
N1 C1B H1D 111.6 . . ?
C2B C1B H1D 111.6 . . ?
H1C C1B H1D 109.4 . . ?
N2B C2B C1B 109(3) . . ?
N2B C2B H2C 109.8 . . ?
C1B C2B H2C 109.8 . . ?
N2B C2B H2D 109.8 . . ?
C1B C2B H2D 109.8 . . ?
H2C C2B H2D 108.3 . . ?
C3B N2B C2B 111(3) . . ?
C3B N2B Zn1 121(8) . . ?
C2B N2B Zn1 112(5) . . ?
C3B N2B H2E 103.4 . . ?
C2B N2B H2E 103.4 . . ?
Zn1 N2B H2E 103.4 . . ?
N2B C3B C4B 111(3) . . ?
N2B C3B H3C 109.4 . . ?
C4B C3B H3C 109.4 . . ?
N2B C3B H3D 109.4 . . ?
C4B C3B H3D 109.4 . . ?
H3C C3B H3D 108.0 . . ?
C9B C4B C5B 119(3) . . ?
C9B C4B C3B 122(3) . . ?
C5B C4B C3B 118(4) . . ?
C6B C5B C4B 117(4) . . ?
C6B C5B H5B 121.7 . . ?
C4B C5B H5B 121.8 . . ?
C7B C6B C5B 121(3) . . ?
C7B C6B H6B 119.3 . . ?
C5B C6B H6B 119.3 . . ?
C8B C7B C6B 117(3) . . ?
C8B C7B C10B 126(3) . . ?
C6B C7B C10B 117(3) . . ?
C7B C8B C9B 124(3) . . ?
C7B C8B H8B 118.2 . . ?
C9B C8B H8B 118.2 . . ?
C4B C9B C8B 119(3) . . ?
C4B C9B H9B 120.5 . . ?
C8B C9B H9B 120.5 . . ?
C7B C10B N3B 109(3) . . ?
C7B C10B H10C 109.8 . . ?
N3B C10B H10C 109.8 . . ?
C7B C10B H10D 109.8 . . ?
N3B C10B H10D 109.8 . . ?
H10C C10B H10D 108.3 . . ?
C11B N3B C10B 113(3) . . ?
C11B N3B H3E 101.6 . . ?
C10B N3B H3E 101.6 . . ?
Zn1 N3B H3E 101.6 4_665 . ?
N3B C11B C12B 106(3) . . ?
N3B C11B H11C 110.5 . . ?
C12B C11B H11C 110.5 . . ?
N3B C11B H11D 110.5 . . ?
C12B C11B H11D 110.5 . . ?
H11C C11B H11D 108.7 . . ?
N1 C12B C11B 122(4) 4_665 . ?
N1 C12B H12C 106.8 4_665 . ?
C11B C12B H12C 106.8 . . ?
N1 C12B H12D 106.8 4_665 . ?
C11B C12B H12D 106.8 . . ?
H12C C12B H12D 106.7 . . ?
O4 Cl1 O4 110.7(7) 3_665 2_655 ?
O4 Cl1 O4 110.7(7) 3_665 . ?
O4 Cl1 O4 110.7(7) 2_655 . ?
O4 Cl1 O3 108.2(8) 3_665 . ?
O4 Cl1 O3 108.2(8) 2_655 . ?
O4 Cl1 O3 108.2(8) . . ?
O4B Cl1B O4B 106(2) 3_665 . ?
O4B Cl1B O4B 106(2) 3_665 2_655 ?
O4B Cl1B O4B 106(2) . 2_655 ?
O4B Cl1B O3B 112(2) 3_665 . ?
O4B Cl1B O3B 112(2) . . ?
O4B Cl1B O3B 112(2) 2_655 . ?
O5 Cl2 O5 180.0(15) 8 2 ?
O5 Cl2 O5 95.6(9) 8 7 ?
O5 Cl2 O5 84.4(9) 2 7 ?
O5 Cl2 O5 95.6(9) 8 9 ?
O5 Cl2 O5 84.4(9) 2 9 ?
O5 Cl2 O5 95.6(9) 7 9 ?
O5 Cl2 O5 84.4(9) 8 3 ?
O5 Cl2 O5 95.6(9) 2 3 ?
O5 Cl2 O5 84.4(9) 7 3 ?
O5 Cl2 O5 180.0(12) 9 3 ?
O5 Cl2 O5 84.4(9) 8 . ?
O5 Cl2 O5 95.6(9) 2 . ?
O5 Cl2 O5 180.0 7 . ?
O5 Cl2 O5 84.4(9) 9 . ?
O5 Cl2 O5 95.6(9) 3 . ?

_refine_diff_density_max         1.839
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.160

####################################################################### 
# 
# 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_pCCu2ONO
_database_code_depnum_ccdc_archive 'CCDC 1884273'
_audit_update_record             
;
2018-12-11 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT260_pCCu2ONO            
;
PROBLEM: Large Average Ueq of Residue Including       CL2      0.168 Check 
RESPONSE: The residue including Cl2 is a perchlorate ion sitting at the unit cell
origin.  The Cl2 atom is on the origin and thus the site occupancy is fixed at 1/6.  
Due to the symmetry of the site, only one oxygen atom (O5) is defined for the ClO4 
ion.  By symmetry, at total of six oxygen atoms are generated and so the O5 site 
occupancy is fixed at 2/3.  Attempts to model the oxygen site as disordered over 
two positions were unsuccessful and resulted in non-convergence of the model and 
unrealistic geometric parameters.  The unmodeled disorder is likely the cause of 
the large average Ueq of the residue.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H54 Cu2 N9 O2, 3(Cl O4)'
_chemical_formula_sum            'C36 H54 Cl3 Cu2 N9 O14'
_chemical_formula_weight         1070.31


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

_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_H-M_alt        'P -3 1 c'
_space_group_name_Hall           '-P 3 2c'

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

_cell_length_a                   9.9795(5)
_cell_length_b                   9.9795(5)
_cell_length_c                   25.6934(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2216.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5558
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      22.34
_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_F_000             1108
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.216
_shelx_estimated_absorpt_T_min   0.793
_shelx_estimated_absorpt_T_max   0.909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6374
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_absorpt_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  'multilayer mirrors'
_diffrn_measurement_device       'Bruker APEX ApexII CCD'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26086
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.357
_diffrn_reflns_theta_max         25.365
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1365
_reflns_number_gt                1111
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_reduction        
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2016) 
;
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELX-2018-1 (Sheldrick, 2015)'
_computing_molecular_graphics    'SHELXLE v932 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'

_refine_special_details          
; 
The structure was phased by intrinsic methods (Sheldrick, 2015).  Systematic 
conditions suggested the ambiguous space group.  The space group choice 
was confirmed by successful convergence of the full-matrix least-squares 
refinement on F².  The highest peaks in the final difference Fourier map 
were in the vicinity of disordered perchlorate anions; the final map had 
no other significant features.  A final analysis of variance between 
observed and calculated structure factors showed little dependence on 
amplitude and resolution. 
;
_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+2.0591P] 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         1365
_refine_ls_number_parameters     142
_refine_ls_number_restraints     154
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1748
_refine_ls_wR_factor_gt          0.1638
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_restrained_S_all      1.219
_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 0.333333 0.666667 0.13236(3) 0.0439(4) Uani 1 3 d S T P . .
N1 N 0.333333 0.666667 0.0532(2) 0.0492(14) Uani 1 3 d S T P A .
N2 N 0.1151(5) 0.6546(5) 0.12455(15) 0.0646(11) Uani 1 1 d D . . . .
H2 H 0.058(7) 0.569(5) 0.144(2) 0.097 Uiso 1 1 d D U . . .
O1 O 0.307(10) 0.662(10) 0.2030(15) 0.050(10) Uani 0.1667 1 d D U P A -1
O2 O 0.294(6) 0.650(8) 0.2902(13) 0.040(8) Uani 0.1667 1 d D U P A -1
N3 N 0.344(6) 0.717(2) 0.248(2) 0.073(10) Uani 0.1667 1 d D U P A -1
C1 C 0.2097(6) 0.6966(7) 0.03509(18) 0.0680(14) Uani 1 1 d . . . . .
H1A H 0.183888 0.663941 -0.000843 0.082 Uiso 1 1 calc R U . A .
H1B H 0.245461 0.806426 0.037013 0.082 Uiso 1 1 calc R U . . .
C2 C 0.0681(7) 0.6078(9) 0.0691(2) 0.0843(18) Uani 1 1 d . . . . .
H2A H -0.011563 0.631472 0.059125 0.101 Uiso 1 1 calc R U . . .
H2B H 0.026988 0.497412 0.065115 0.101 Uiso 1 1 calc R U . . .
C3 C 0.1021(9) 0.7916(9) 0.1395(2) 0.0873(19) Uani 1 1 d . . . . .
H3A H 0.000418 0.774008 0.130163 0.105 Uiso 1 1 calc R U . . .
H3B H 0.178535 0.881740 0.120600 0.105 Uiso 1 1 calc R U . . .
C4 C 0.1268(8) 0.8216(8) 0.1967(2) 0.0749(17) Uani 1 1 d . . . . .
C5 C 0.0227(7) 0.7170(10) 0.2326(2) 0.088(2) Uani 1 1 d . . . . .
H5 H -0.065074 0.628276 0.220969 0.105 Uiso 1 1 calc R U . . .
C6 C 0.0491(7) 0.7441(10) 0.2855(2) 0.089(2) Uani 1 1 d . . . . .
H6 H -0.021840 0.673916 0.309142 0.107 Uiso 1 1 calc R U . . .
Cl1 Cl 0.666667 0.333333 0.1323(6) 0.0617(18) Uani 0.583(11) 3 d DS TU P B 1
O3 O 0.666667 0.333333 0.1867(7) 0.132(5) Uani 0.583(11) 3 d DS TU P B 1
O4 O 0.7045(12) 0.4777(10) 0.1111(5) 0.122(3) Uani 0.583(11) 1 d D U P B 1
Cl1B Cl 0.666667 0.333333 0.1326(10) 0.071(3) Uani 0.417(11) 3 d S TU P B 2
O3B O 0.666667 0.333333 0.0793(9) 0.107(5) Uani 0.417(11) 3 d S TU P B 2
O4B O 0.6764(18) 0.4685(16) 0.1509(7) 0.123(4) Uani 0.417(11) 1 d . U P B 2
Cl2 Cl 0.000000 0.000000 0.000000 0.1247(17) Uani 1 6 d DS TU P . .
O5 O 0.1011(17) 0.1287(16) -0.0297(6) 0.210(6) Uani 0.6667 1 d D U 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.
;

_exptl_special_details           
; 
One distinct cell was identified using APEX3 (Bruker, 2016).  Six 
frame series were integrated and filtered for statistical outliers 
using SAINT (Bruker, 2016) then corrected for absorption by integration 
using SAINT/SADABS v2014/2 (Bruker, 2016) to sort, merge, and scale 
the combined data.No decay correction was applied.    
;

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 1.83(4) . ?
Cu1 N1 2.035(6) . ?
Cu1 N2 2.129(4) 2_665 ?
Cu1 N2 2.129(4) . ?
Cu1 N2 2.129(4) 3_565 ?
N1 C1 1.481(5) . ?
N1 C1 1.481(5) 3_565 ?
N1 C1 1.481(5) 2_665 ?
N2 C3 1.488(7) . ?
N2 C2 1.499(6) . ?
N2 H2 0.90(2) . ?
O1 N3 1.248(10) . ?
O2 N3 1.248(10) . ?
C1 C2 1.515(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.494(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C6 1.368(9) 4_665 ?
C4 C5 1.391(9) . ?
C5 C6 1.386(8) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
Cl1 O3 1.398(11) . ?
Cl1 O4 1.404(9) 2_655 ?
Cl1 O4 1.404(9) . ?
Cl1 O4 1.404(9) 3_665 ?
Cl1B O3B 1.37(3) . ?
Cl1B O4B 1.384(15) . ?
Cl1B O4B 1.385(16) 2_655 ?
Cl1B O4B 1.385(15) 3_665 ?
Cl2 O5 1.397(10) . ?
Cl2 O5 1.397(10) 8 ?
Cl2 O5 1.397(10) 2 ?
Cl2 O5 1.397(10) 9 ?
Cl2 O5 1.397(10) 3 ?
Cl2 O5 1.397(10) 7 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N1 172(3) . . ?
O1 Cu1 N2 98(2) . 2_665 ?
N1 Cu1 N2 84.59(11) . 2_665 ?
O1 Cu1 N2 88(3) . . ?
N1 Cu1 N2 84.60(11) . . ?
N2 Cu1 N2 119.12(3) 2_665 . ?
O1 Cu1 N2 100(3) . 3_565 ?
N1 Cu1 N2 84.59(11) . 3_565 ?
N2 Cu1 N2 119.12(4) 2_665 3_565 ?
N2 Cu1 N2 119.12(3) . 3_565 ?
C1 N1 C1 110.6(3) . 3_565 ?
C1 N1 C1 110.6(3) . 2_665 ?
C1 N1 C1 110.6(3) 3_565 2_665 ?
C1 N1 Cu1 108.3(3) . . ?
C1 N1 Cu1 108.3(3) 3_565 . ?
C1 N1 Cu1 108.3(3) 2_665 . ?
C3 N2 C2 112.0(4) . . ?
C3 N2 Cu1 118.7(4) . . ?
C2 N2 Cu1 105.0(3) . . ?
C3 N2 H2 115(5) . . ?
C2 N2 H2 106(5) . . ?
Cu1 N2 H2 99(4) . . ?
N3 O1 Cu1 153(7) . . ?
O1 N3 O2 128(2) . . ?
N1 C1 C2 109.2(4) . . ?
N1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
N1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.3 . . ?
N2 C2 C1 108.1(4) . . ?
N2 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
N2 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
N2 C3 C4 110.9(4) . . ?
N2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.0 . . ?
C6 C4 C5 119.0(5) 4_665 . ?
C6 C4 C3 120.0(6) 4_665 . ?
C5 C4 C3 121.0(7) . . ?
C6 C5 C4 120.4(7) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C4 C6 C5 120.6(7) 4_665 . ?
C4 C6 H6 119.7 4_665 . ?
C5 C6 H6 119.7 . . ?
O3 Cl1 O4 112.8(8) . 2_655 ?
O3 Cl1 O4 112.8(8) . . ?
O4 Cl1 O4 105.9(9) 2_655 . ?
O3 Cl1 O4 112.8(8) . 3_665 ?
O4 Cl1 O4 105.9(9) 2_655 3_665 ?
O4 Cl1 O4 105.9(9) . 3_665 ?
O3B Cl1B O4B 109.8(13) . . ?
O3B Cl1B O4B 109.8(13) . 2_655 ?
O4B Cl1B O4B 109.2(14) . 2_655 ?
O5 Cl2 O5 87.0(10) . 8 ?
O5 Cl2 O5 93.0(10) . 2 ?
O5 Cl2 O5 180.0(13) 8 2 ?
O5 Cl2 O5 87.0(10) . 9 ?
O5 Cl2 O5 93.0(10) 8 9 ?
O5 Cl2 O5 87.0(10) 2 9 ?
O5 Cl2 O5 93.0(10) . 3 ?
O5 Cl2 O5 87.0(10) 8 3 ?
O5 Cl2 O5 93.0(10) 2 3 ?
O5 Cl2 O5 180.0(11) 9 3 ?
O5 Cl2 O5 180.0 . 7 ?
O5 Cl2 O5 93.0(10) 8 7 ?
O5 Cl2 O5 87.0(10) 2 7 ?
O5 Cl2 O5 93.0(10) 9 7 ?
O5 Cl2 O5 87.0(10) 3 7 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2 O4B^b 0.90(2) 2.56(5) 3.333(17) 144(6) 3_565 yes

_refine_diff_density_max         0.794
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.090

