# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1860806'
_audit_update_record             
;
2019-01-31 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C62.80 H57.60 Cu4 N32 O8.80'
_chemical_formula_weight         1655.57

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

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'

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

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

_cell_length_a                   13.1705(9)
_cell_length_b                   13.1705(9)
_cell_length_c                   19.6437(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3407.4(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    1625
_cell_measurement_theta_min      3.47
_cell_measurement_theta_max      21.89

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_F_000             1690
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.314
_shelx_estimated_absorpt_T_min   0.678
_shelx_estimated_absorpt_T_max   0.779
_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      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  "Bruker APEX II CCD area detector'"
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20253
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.862
_diffrn_reflns_theta_max         28.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4536
_reflns_number_gt                3931
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 4.0.0'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0504P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.013(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4536
_refine_ls_number_parameters     254
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_ref         0.0939
_refine_ls_wR_factor_gt          0.0895
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.074
_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
Cu1 Cu 0.55708(4) 0.34016(4) 0.43638(3) 0.01121(13) Uani 1 1 d . . . . .
N1 N 0.5465(3) 0.3243(3) 0.33993(18) 0.0145(8) Uani 1 1 d . . . . .
N2 N 0.5232(3) 0.3461(3) 0.2292(2) 0.0208(9) Uani 1 1 d . . . . .
N3 N 0.4639(3) 0.2639(3) 0.2498(2) 0.0202(8) Uani 1 1 d . . . . .
N4 N 0.4649(3) 0.2071(2) 0.4299(2) 0.0139(7) Uani 1 1 d . . . . .
N5 N 0.7145(3) 0.5973(3) 0.3622(2) 0.0141(8) Uani 1 1 d . . . . .
N6 N 0.6228(3) 0.4772(3) 0.41610(17) 0.0114(7) Uani 1 1 d . . . . .
N7 N 0.6564(3) 0.5473(3) 0.46337(17) 0.0102(6) Uani 1 1 d . . . . .
N8 N 0.7465(3) 0.6972(3) 0.5328(2) 0.0166(8) Uani 1 1 d . . . . .
C1 C 0.6467(4) 0.4628(3) 0.2871(2) 0.0173(9) Uani 1 1 d . . . . .
H1A H 0.6264 0.5159 0.2541 0.021 Uiso 1 1 calc R U . . .
H1B H 0.7133 0.4358 0.2724 0.021 Uiso 1 1 calc R U . . .
C2 C 0.5707(4) 0.3791(3) 0.2847(2) 0.0158(9) Uani 1 1 d . . . . .
C3 C 0.4804(3) 0.2545(3) 0.3156(2) 0.0157(9) Uani 1 1 d . . . . .
C4 C 0.4407(3) 0.1819(3) 0.3649(3) 0.0160(9) Uani 1 1 d . . . . .
C5 C 0.4349(3) 0.1448(4) 0.4798(3) 0.0203(10) Uani 1 1 d . . . . .
H5 H 0.4511 0.1616 0.5256 0.024 Uiso 1 1 calc R U . . .
C6 C 0.3805(4) 0.0561(4) 0.4668(3) 0.0251(12) Uani 1 1 d . . . . .
H6 H 0.3606 0.0128 0.5031 0.030 Uiso 1 1 calc R U . . .
C7 C 0.3560(4) 0.0322(4) 0.4006(3) 0.0265(12) Uani 1 1 d . . . . .
H7 H 0.3188 -0.0278 0.3908 0.032 Uiso 1 1 calc R U . . .
C8 C 0.3858(4) 0.0958(4) 0.3489(3) 0.0228(11) Uani 1 1 d . . . . .
H8 H 0.3689 0.0808 0.3029 0.027 Uiso 1 1 calc R U . . .
C9 C 0.6589(4) 0.5111(3) 0.3560(2) 0.0133(9) Uani 1 1 d . . . . .
C10 C 0.7102(3) 0.6159(3) 0.4288(3) 0.0139(9) Uani 1 1 d . . . . .
C11 C 0.7609(3) 0.6988(3) 0.4652(2) 0.0132(8) Uani 1 1 d . . . . .
C12 C 0.7890(3) 0.7700(3) 0.5699(3) 0.0195(9) Uani 1 1 d . . . . .
H12 H 0.7786 0.7696 0.6177 0.023 Uiso 1 1 calc R U . . .
C13 C 0.8484(4) 0.8472(4) 0.5415(3) 0.0236(11) Uani 1 1 d . . . . .
H13 H 0.8773 0.8983 0.5696 0.028 Uiso 1 1 calc R U . . .
C14 C 0.8643(4) 0.8477(4) 0.4724(3) 0.0235(11) Uani 1 1 d . . . . .
H14 H 0.9053 0.8987 0.4521 0.028 Uiso 1 1 calc R U . . .
C15 C 0.8192(3) 0.7720(3) 0.4322(3) 0.0193(9) Uani 1 1 d . . . . .
H15 H 0.8282 0.7707 0.3842 0.023 Uiso 1 1 calc R U . . .
O1W O 0.7582(3) 0.7078(3) 0.2418(2) 0.0392(11) Uani 1 1 d . . . . .
H1WA H 0.7492 0.6773 0.2795 0.047 Uiso 1 1 d R U . . .
H1WB H 0.6961 0.7245 0.2381 0.047 Uiso 1 1 d R U . . .
O2W O 0.5000 0.5000 0.1283(2) 0.0236(11) Uani 1 2 d S T P . .
H2W H 0.5093 0.4507 0.1555 0.028 Uiso 1 1 d R U . . .
O1SA O 0.8934(9) 0.6056(9) 0.1585(8) 0.085(4) Uani 0.5 1 d D . P . .
C1S C 0.8676(10) 0.5040(10) 0.1620(6) 0.069(4) Uani 0.7 1 d D . P . .
O1SB O 0.9588(18) 0.480(3) 0.1191(16) 0.090(10) Uiso 0.2 1 d 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
Cu1 N1 1.911(4) . ?
Cu1 N7 1.974(3) 3_566 ?
Cu1 N6 2.041(4) . ?
Cu1 N4 2.136(3) . ?
Cu1 N8 2.252(4) 3_566 ?
N1 C2 1.343(6) . ?
N1 C3 1.352(6) . ?
N2 C2 1.330(6) . ?
N2 N3 1.394(6) . ?
N3 C3 1.318(6) . ?
N4 C5 1.338(6) . ?
N4 C4 1.357(6) . ?
N5 C10 1.332(6) . ?
N5 C9 1.357(5) . ?
N6 C9 1.349(6) . ?
N6 N7 1.382(5) . ?
N7 C10 1.334(6) . ?
N7 Cu1 1.974(3) 4_656 ?
N8 C12 1.328(6) . ?
N8 C11 1.342(6) . ?
N8 Cu1 2.252(4) 4_656 ?
C1 C2 1.489(6) . ?
C1 C9 1.504(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C3 C4 1.458(7) . ?
C4 C8 1.381(6) . ?
C5 C6 1.394(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.376(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.374(8) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C10 C11 1.466(6) . ?
C11 C15 1.393(6) . ?
C12 C13 1.398(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.373(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.404(7) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8501 . ?
O2W H2W 0.8500 . ?
O1SA C1S 1.382(12) . ?
C1S O1SB 1.499(14) . ?
O1SB O1SB 1.20(5) 2_765 ?

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 Cu1 N7 170.62(15) . 3_566 ?
N1 Cu1 N6 86.24(15) . . ?
N7 Cu1 N6 101.66(15) 3_566 . ?
N1 Cu1 N4 79.02(16) . . ?
N7 Cu1 N4 92.36(16) 3_566 . ?
N6 Cu1 N4 162.78(15) . . ?
N1 Cu1 N8 105.71(16) . 3_566 ?
N7 Cu1 N8 78.30(15) 3_566 3_566 ?
N6 Cu1 N8 98.78(14) . 3_566 ?
N4 Cu1 N8 93.78(13) . 3_566 ?
C2 N1 C3 103.5(4) . . ?
C2 N1 Cu1 136.5(3) . . ?
C3 N1 Cu1 118.1(3) . . ?
C2 N2 N3 106.3(4) . . ?
C3 N3 N2 105.3(4) . . ?
C5 N4 C4 118.1(4) . . ?
C5 N4 Cu1 128.8(4) . . ?
C4 N4 Cu1 113.0(3) . . ?
C10 N5 C9 102.6(4) . . ?
C9 N6 N7 104.7(3) . . ?
C9 N6 Cu1 127.8(3) . . ?
N7 N6 Cu1 126.5(3) . . ?
C10 N7 N6 106.3(3) . . ?
C10 N7 Cu1 116.8(3) . 4_656 ?
N6 N7 Cu1 136.1(3) . 4_656 ?
C12 N8 C11 118.1(4) . . ?
C12 N8 Cu1 131.2(4) . 4_656 ?
C11 N8 Cu1 110.5(3) . 4_656 ?
C2 C1 C9 114.4(4) . . ?
C2 C1 H1A 108.7 . . ?
C9 C1 H1A 108.7 . . ?
C2 C1 H1B 108.7 . . ?
C9 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
N2 C2 N1 112.0(4) . . ?
N2 C2 C1 125.8(4) . . ?
N1 C2 C1 122.2(4) . . ?
N3 C3 N1 112.9(4) . . ?
N3 C3 C4 130.8(4) . . ?
N1 C3 C4 116.2(4) . . ?
N4 C4 C8 122.6(5) . . ?
N4 C4 C3 112.3(4) . . ?
C8 C4 C3 125.1(5) . . ?
N4 C5 C6 122.0(5) . . ?
N4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C7 C6 C5 119.0(5) . . ?
C7 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
C8 C7 C6 119.5(5) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C4 118.8(5) . . ?
C7 C8 H8 120.6 . . ?
C4 C8 H8 120.6 . . ?
N6 C9 N5 112.9(4) . . ?
N6 C9 C1 127.6(4) . . ?
N5 C9 C1 119.5(4) . . ?
N7 C10 N5 113.5(4) . . ?
N7 C10 C11 119.9(4) . . ?
N5 C10 C11 126.6(4) . . ?
N8 C11 C15 123.3(4) . . ?
N8 C11 C10 114.0(4) . . ?
C15 C11 C10 122.7(5) . . ?
N8 C12 C13 122.9(5) . . ?
N8 C12 H12 118.6 . . ?
C13 C12 H12 118.6 . . ?
C14 C13 C12 118.9(5) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 119.2(5) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C11 C15 C14 117.6(5) . . ?
C11 C15 H15 121.2 . . ?
C14 C15 H15 121.2 . . ?
H1WA O1W H1WB 93.7 . . ?
O1SA C1S O1SB 88.7(17) . . ?
O1SB O1SB C1S 129(3) 2_765 . ?

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
O1W H1WA N5 0.85 1.99 2.836(6) 173.2 .
O1W H1WB N3 0.85 2.13 2.953(6) 164.4 2_665
O2W H2W N2 0.85 2.01 2.851(5) 172.4 .

_refine_diff_density_max         0.625
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.085

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

data_3
_database_code_depnum_ccdc_archive 'CCDC 1860807'
_audit_update_record             
;
2019-01-14 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H14 Cl2 Cu N8 O8'
_chemical_formula_weight         580.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1590 '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                   13.0990(11)
_cell_length_b                   11.6970(7)
_cell_length_c                   14.5274(12)
_cell_angle_alpha                90
_cell_angle_beta                 112.745(10)
_cell_angle_gamma                90
_cell_volume                     2052.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5455
_cell_measurement_theta_min      3.0239
_cell_measurement_theta_max      33.2377

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_F_000             1172
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    1.392
_shelx_estimated_absorpt_T_min   0.641
_shelx_estimated_absorpt_T_max   0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93945
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 8.3611
_diffrn_reflns_number            6730
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.041
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_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             1819
_reflns_number_gt                1595
_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       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXLS-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_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)+(0.0416P)²+1.2874P] 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         1819
_refine_ls_number_parameters     159
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0695
_refine_ls_wR_factor_gt          0.0683
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.59145(17) 0.02357(18) 0.37296(16) 0.0189(5) Uani 1 1 d . . . . .
H1 H 0.5750 -0.0162 0.3119 0.023 Uiso 1 1 calc R U . . .
C2 C 0.63070(18) -0.03768(19) 0.46117(17) 0.0214(5) Uani 1 1 d . . . . .
H2 H 0.6387 -0.1183 0.4601 0.026 Uiso 1 1 calc R U . . .
C3 C 0.65808(18) 0.0191(2) 0.55062(17) 0.0219(5) Uani 1 1 d . . . . .
H3 H 0.6827 -0.0219 0.6118 0.026 Uiso 1 1 calc R U . . .
C4 C 0.60827(17) 0.19236(18) 0.45888(16) 0.0159(4) Uani 1 1 d . . . . .
C5 C 0.59668(16) 0.31660(18) 0.44908(15) 0.0152(4) Uani 1 1 d . . . . .
C6 C 0.64903(18) 0.1371(2) 0.54968(16) 0.0206(5) Uani 1 1 d . . . . .
H6 H 0.6704 0.1790 0.6103 0.025 Uiso 1 1 calc R U . . .
C7 C 0.54463(16) 0.47424(17) 0.37069(15) 0.0158(4) Uani 1 1 d . . . . .
C8 C 0.48869(18) 0.56576(17) 0.29848(15) 0.0167(5) Uani 1 1 d . . . . .
H8A H 0.5121 0.6405 0.3320 0.020 Uiso 1 1 calc R U . . .
H8B H 0.4079 0.5588 0.2801 0.020 Uiso 1 1 calc R U . . .
O1 O 0.27317(15) 0.40371(14) 0.29344(12) 0.0325(4) Uani 1 1 d . . . . .
O2 O 0.35756(14) 0.29208(14) 0.43680(12) 0.0277(4) Uani 1 1 d . . . . .
O3 O 0.32405(13) 0.21335(14) 0.27855(12) 0.0251(4) Uani 1 1 d . . . . .
O4 O 0.17613(17) 0.25105(17) 0.32634(17) 0.0476(6) Uani 1 1 d . . . . .
N1 N 0.57564(14) 0.13770(14) 0.37029(13) 0.0148(4) Uani 1 1 d . . . . .
N2 N 0.54624(14) 0.36103(14) 0.35603(13) 0.0143(4) Uani 1 1 d . . . . .
N3 N 0.59605(14) 0.49202(15) 0.46877(13) 0.0179(4) Uani 1 1 d . . . . .
H3A H 0.6072 0.5602 0.4965 0.021 Uiso 1 1 calc R U . . .
N4 N 0.62926(15) 0.39286(16) 0.52095(13) 0.0189(4) Uani 1 1 d . . . . .
Cu1 Cu 0.5000 0.24447(3) 0.2500 0.01446(13) Uani 1 2 d S T P . .
Cl Cl 0.28156(4) 0.29033(4) 0.33299(4) 0.01863(15) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.349(3) . ?
C1 C2 1.382(3) . ?
C2 C3 1.378(3) . ?
C3 C6 1.384(3) . ?
C4 N1 1.350(3) . ?
C4 C6 1.378(3) . ?
C4 C5 1.462(3) . ?
C5 N4 1.313(3) . ?
C5 N2 1.358(3) . ?
C7 N3 1.336(3) . ?
C7 N2 1.343(3) . ?
C7 C8 1.480(3) . ?
C8 C8 1.547(4) 2_655 ?
O1 Cl 1.4326(17) . ?
O2 Cl 1.4509(17) . ?
O3 Cl 1.4444(16) . ?
O4 Cl 1.4228(19) . ?
N1 Cu1 2.0630(17) . ?
N2 Cu1 1.9690(17) . ?
N3 N4 1.362(3) . ?
Cu1 N2 1.9690(17) 2_655 ?
Cu1 N1 2.0631(17) 2_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 C1 C2 122.5(2) . . ?
C3 C2 C1 119.5(2) . . ?
C2 C3 C6 118.8(2) . . ?
N1 C4 C6 123.57(19) . . ?
N1 C4 C5 113.28(17) . . ?
C6 C4 C5 123.15(19) . . ?
N4 C5 N2 114.53(18) . . ?
N4 C5 C4 127.46(19) . . ?
N2 C5 C4 118.00(17) . . ?
C4 C6 C3 118.5(2) . . ?
N3 C7 N2 106.87(18) . . ?
N3 C7 C8 123.43(18) . . ?
N2 C7 C8 129.42(19) . . ?
C7 C8 C8 115.39(16) . 2_655 ?
C1 N1 C4 116.91(18) . . ?
C1 N1 Cu1 129.90(15) . . ?
C4 N1 Cu1 113.09(13) . . ?
C7 N2 C5 104.54(17) . . ?
C7 N2 Cu1 142.00(15) . . ?
C5 N2 Cu1 113.45(13) . . ?
C7 N3 N4 112.46(17) . . ?
C5 N4 N3 101.55(17) . . ?
N2 Cu1 N2 92.35(10) 2_655 . ?
N2 Cu1 N1 169.59(7) 2_655 . ?
N2 Cu1 N1 81.65(7) . . ?
N2 Cu1 N1 81.65(7) 2_655 2_655 ?
N2 Cu1 N1 169.59(7) . 2_655 ?
N1 Cu1 N1 105.49(10) . 2_655 ?
O4 Cl O1 110.47(12) . . ?
O4 Cl O3 109.32(10) . . ?
O1 Cl O3 110.09(10) . . ?
O4 Cl O2 109.45(12) . . ?
O1 Cl O2 108.62(10) . . ?
O3 Cl O2 108.85(10) . . ?

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
C2 H2 O2 0.95 2.51 3.301(3) 140.4 5_656
C8 H8A O4 0.99 2.54 3.181(3) 122.6 3
C8 H8B O1 0.99 2.59 3.378(3) 136.6 .
N3 H3A O2 0.88 1.95 2.826(2) 176.0 5_666
N3 H3A Cl 0.88 2.92 3.7116(18) 150.6 5_666

_refine_diff_density_max         0.386
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.065


_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_a_a_sq
_database_code_depnum_ccdc_archive 'CCDC 1860809'
_audit_update_record             
;
2019-01-29 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cu2 Cl2  N16  C30  H24, 2Cl, 6.5 (CH3OH)'
_chemical_formula_sum            'C36.50 H50 Cl4 Cu2 N16 O6.50'
_chemical_formula_weight         1085.80

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           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                   19.725(3)
_cell_length_b                   18.998(3)
_cell_length_c                   12.833(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.971(5)
_cell_angle_gamma                90
_cell_volume                     4783.0(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    424
_cell_measurement_theta_min      3
_cell_measurement_theta_max      25

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_F_000             2236
_exptl_transmission_factor_min   0.698
_exptl_transmission_factor_max   0.872
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.175
_shelx_estimated_absorpt_T_min   0.698
_shelx_estimated_absorpt_T_max   0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  "Bruker APEX II CCD area detector'"
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26949
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.104
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5761
_reflns_number_gt                4107
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0823P)²+8.5519P] 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         5761
_refine_ls_number_parameters     311
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1544
_refine_ls_wR_factor_gt          0.1323
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.010
_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_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 -0.09877(2) 0.11754(2) -0.08311(3) 0.02108(14) Uani 1 1 d . . . . .
Cl1 Cl -0.05349(5) 0.20470(5) 0.02350(8) 0.0314(2) Uani 1 1 d . . . . .
N1 N -0.00933(14) 0.08457(15) -0.1191(2) 0.0197(6) Uani 1 1 d . . . . .
N2 N 0.05901(14) -0.00908(15) -0.1302(2) 0.0199(6) Uani 1 1 d . . . . .
N3 N 0.09464(15) 0.05238(15) -0.1285(2) 0.0207(6) Uani 1 1 d . . . . .
H3N H 0.141834 0.054898 -0.139737 0.025 Uiso 1 1 d R U . . .
N4 N -0.12105(15) 0.01131(15) -0.1126(2) 0.0195(6) Uani 1 1 d . . . . .
N5 N 0.14369(15) 0.16928(15) -0.2738(2) 0.0229(6) Uani 1 1 d . . . . .
N6 N 0.23325(17) 0.23883(17) -0.2208(2) 0.0308(7) Uani 1 1 d . . . . .
N7 N 0.18755(17) 0.23718(17) -0.1492(2) 0.0297(7) Uani 1 1 d . . . . .
H7N H 0.190285 0.265429 -0.097600 0.036 Uiso 1 1 d R U . . .
N8 N 0.19151(16) 0.13820(15) -0.4567(2) 0.0247(6) Uani 1 1 d . . . . .
C1 C 0.07594(18) 0.18308(18) -0.1201(3) 0.0234(7) Uani 1 1 d . . . . .
H1A H 0.037084 0.212567 -0.149045 0.028 Uiso 1 1 calc R U . . .
H1B H 0.088493 0.197700 -0.046568 0.028 Uiso 1 1 calc R U . . .
C2 C 0.05419(18) 0.10770(18) -0.1219(3) 0.0204(7) Uani 1 1 d . . . . .
C3 C -0.00336(17) 0.01318(17) -0.1246(2) 0.0184(6) Uani 1 1 d . . . . .
C4 C -0.06587(17) -0.02827(18) -0.1281(2) 0.0185(7) Uani 1 1 d . . . . .
C5 C -0.06997(18) -0.09923(18) -0.1490(3) 0.0221(7) Uani 1 1 d . . . . .
H5A H -0.030233 -0.125692 -0.158604 0.026 Uiso 1 1 calc R U . . .
C6 C -0.13332(19) -0.13123(19) -0.1557(3) 0.0251(8) Uani 1 1 d . . . . .
H6A H -0.137800 -0.180084 -0.170632 0.030 Uiso 1 1 calc R U . . .
C7 C -0.18983(19) -0.0914(2) -0.1404(3) 0.0268(8) Uani 1 1 d . . . . .
H7A H -0.233740 -0.112369 -0.144663 0.032 Uiso 1 1 calc R U . . .
C8 C -0.18173(18) -0.02064(19) -0.1189(3) 0.0236(7) Uani 1 1 d . . . . .
H8A H -0.220837 0.006526 -0.108233 0.028 Uiso 1 1 calc R U . . .
C9 C 0.13458(18) 0.19567(18) -0.1811(3) 0.0231(7) Uani 1 1 d . . . . .
C10 C 0.20496(19) 0.19622(19) -0.2940(3) 0.0249(7) Uani 1 1 d . . . . .
C11 C 0.2341(2) 0.17613(19) -0.3905(3) 0.0262(8) Uani 1 1 d . . . . .
C12 C 0.2985(2) 0.1933(2) -0.4125(3) 0.0345(9) Uani 1 1 d . . . . .
H12A H 0.327770 0.220231 -0.364494 0.041 Uiso 1 1 calc R U . . .
C13 C 0.3201(2) 0.1706(2) -0.5061(4) 0.0416(11) Uani 1 1 d . . . . .
H13A H 0.364781 0.181142 -0.522761 0.050 Uiso 1 1 calc R U . . .
C14 C 0.2757(2) 0.1324(2) -0.5748(3) 0.0364(10) Uani 1 1 d . . . . .
H14A H 0.289451 0.116554 -0.639661 0.044 Uiso 1 1 calc R U . . .
C15 C 0.2117(2) 0.11759(19) -0.5484(3) 0.0292(8) Uani 1 1 d . . . . .
H15A H 0.180926 0.092123 -0.596282 0.035 Uiso 1 1 calc R U . . .
Cl2 Cl 0.25084(5) 0.44589(5) 0.13068(8) 0.0340(2) Uani 1 1 d . . . . .
O1S O 0.3426(4) 0.0196(5) 0.2342(7) 0.101(3) Uani 0.697(8) 1 d D . P A 1
H1SO H 0.316293 -0.001145 0.272806 0.121 Uiso 0.697(8) 1 d R U P A 1
C1S C 0.3813(9) -0.0289(10) 0.1832(13) 0.111(5) Uani 0.697(8) 1 d D . P A 1
H1SE H 0.357339 -0.033682 0.114467 0.134 Uiso 0.697(8) 1 d R U P A 1
H1SF H 0.379489 -0.073852 0.216987 0.134 Uiso 0.697(8) 1 d R U P A 1
H1SD H 0.428139 -0.019093 0.174897 0.134 Uiso 0.697(8) 1 d R U P A 1
C1S' C 0.357(3) -0.004(3) 0.176(2) 0.111(5) Uani 0.303(8) 1 d D . P A 2
H1SB H 0.370805 0.044008 0.163326 0.134 Uiso 0.303(8) 1 d R U P A 2
H1SC H 0.319115 -0.001892 0.191576 0.134 Uiso 0.303(8) 1 d R U P A 2
H1SA H 0.356505 -0.028702 0.111436 0.134 Uiso 0.303(8) 1 d R U P A 2
O1S' O 0.3957(8) -0.0237(11) 0.2713(16) 0.101(3) Uani 0.303(8) 1 d D . P A 2
H1O' H 0.358331 -0.030158 0.297558 0.121 Uiso 0.303(8) 1 d R U P A 2
O2S O 0.17401(15) 0.32492(18) 0.0126(2) 0.0461(8) Uani 1 1 d D . . . .
H2SO H 0.197399 0.361635 0.048322 0.10(3) Uiso 1 1 d R . . B .
C2S C 0.1119(3) 0.3609(4) -0.0131(9) 0.064(3) Uani 0.677(13) 1 d D . P B 1
H2SA H 0.111858 0.384155 -0.079489 0.096 Uiso 0.677(13) 1 d R U P B 1
H2SB H 0.075308 0.327415 -0.016459 0.096 Uiso 0.677(13) 1 d R U P B 1
H2SC H 0.106008 0.395045 0.040341 0.096 Uiso 0.677(13) 1 d R U P B 1
C2S' C 0.1096(5) 0.3402(11) 0.0510(16) 0.064(3) Uani 0.323(13) 1 d D . P B 2
H2SD H 0.108665 0.317271 0.117525 0.096 Uiso 0.323(13) 1 d R U P B 2
H2SE H 0.103765 0.392041 0.059745 0.096 Uiso 0.323(13) 1 d R U P B 2
H2SF H 0.073285 0.322321 0.002585 0.096 Uiso 0.323(13) 1 d R U P B 2
O4S O 0.500000 0.1934(2) 0.250000 0.0428(10) Uani 1 2 d DS T P C 1
H4SO H 0.525360 0.163119 0.224400 0.051 Uiso 0.5 1 d R U P C 1
C4S C 0.4510(5) 0.1534(5) 0.2969(9) 0.058(3) Uani 0.5 1 d D . P C 1
H4SA H 0.419831 0.184177 0.327324 0.087 Uiso 0.5 1 d R U P C 1
H4SB H 0.426272 0.124287 0.244894 0.087 Uiso 0.5 1 d R U P C 1
H4SC H 0.473982 0.124287 0.350514 0.087 Uiso 0.5 1 d R U P C 1
O5S O 0.4193(5) 0.0955(5) 0.3333(8) 0.102(4) Uani 0.5 1 d D . P D 2
H5SO H 0.444649 0.125724 0.307653 0.122 Uiso 0.5 1 d R U P D 2
C5S C 0.4424(8) 0.0571(8) 0.4251(10) 0.086(4) Uiso 0.5 1 d D . P D 2
H5SA H 0.407053 0.025637 0.442204 0.129 Uiso 0.5 1 d R U P D 2
H5SB H 0.482193 0.030397 0.413274 0.129 Uiso 0.5 1 d R U P D 2
H5SC H 0.453303 0.089287 0.481944 0.129 Uiso 0.5 1 d R U P D 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 N1 1.972(3) . ?
Cu1 N8 1.989(3) 2_554 ?
Cu1 N4 2.092(3) . ?
Cu1 N5 2.187(3) 2_554 ?
Cu1 Cl1 2.2709(10) . ?
N1 C2 1.332(4) . ?
N1 C3 1.364(4) . ?
N2 C3 1.310(4) . ?
N2 N3 1.362(4) . ?
N3 C2 1.328(4) . ?
N3 H3N 0.9578 . ?
N4 C8 1.337(5) . ?
N4 C4 1.355(4) . ?
N5 C9 1.320(5) . ?
N5 C10 1.362(5) . ?
N6 C10 1.319(5) . ?
N6 N7 1.352(5) . ?
N7 C9 1.339(4) . ?
N7 H7N 0.8501 . ?
N8 C11 1.340(5) . ?
N8 C15 1.341(5) . ?
C1 C9 1.482(5) . ?
C1 C2 1.494(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C3 C4 1.460(5) . ?
C4 C5 1.375(5) . ?
C5 C6 1.384(5) . ?
C5 H5A 0.9500 . ?
C6 C7 1.378(5) . ?
C6 H6A 0.9500 . ?
C7 C8 1.378(5) . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
C10 C11 1.469(5) . ?
C11 C12 1.369(6) . ?
C12 C13 1.384(6) . ?
C12 H12A 0.9500 . ?
C13 C14 1.383(6) . ?
C13 H13A 0.9500 . ?
C14 C15 1.370(6) . ?
C14 H14A 0.9500 . ?
C15 H15A 0.9500 . ?
O1S C1S 1.401(4) . ?
O1S H1SO 0.8501 . ?
C1S H1SE 0.9601 . ?
C1S H1SF 0.9600 . ?
C1S H1SD 0.9600 . ?
C1S' O1S' 1.417(4) . ?
C1S' H1SB 0.9603 . ?
C1S' H1SC 0.8001 . ?
C1S' H1SA 0.9600 . ?
O1S' H1O' 0.8502 . ?
O2S C2S 1.411(4) . ?
O2S C2S' 1.439(4) . ?
O2S H2SO 0.9301 . ?
C2S H2SA 0.9600 . ?
C2S H2SB 0.9599 . ?
C2S H2SC 0.9599 . ?
C2S' H2SD 0.9602 . ?
C2S' H2SE 1.0000 . ?
C2S' H2SF 0.9599 . ?
O4S C4S 1.411(4) 2_655 ?
O4S C4S 1.411(4) . ?
O4S H4SO 0.8499 . ?
O4S H4SO 0.8500 2_655 ?
C4S H4SA 0.9601 . ?
C4S H4SB 0.9599 . ?
C4S H4SC 0.9600 . ?
O5S C5S 1.420(4) . ?
O5S H5SO 0.8499 . ?
C5S H5SA 0.9600 . ?
C5S H5SB 0.9599 . ?
C5S H5SC 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
N1 Cu1 N8 172.81(12) . 2_554 ?
N1 Cu1 N4 80.06(11) . . ?
N8 Cu1 N4 93.17(12) 2_554 . ?
N1 Cu1 N5 103.92(11) . 2_554 ?
N8 Cu1 N5 79.84(12) 2_554 2_554 ?
N4 Cu1 N5 102.87(11) . 2_554 ?
N1 Cu1 Cl1 93.85(9) . . ?
N8 Cu1 Cl1 90.92(9) 2_554 . ?
N4 Cu1 Cl1 150.99(8) . . ?
N5 Cu1 Cl1 106.12(8) 2_554 . ?
C2 N1 C3 103.9(3) . . ?
C2 N1 Cu1 140.2(2) . . ?
C3 N1 Cu1 114.4(2) . . ?
C3 N2 N3 102.0(3) . . ?
C2 N3 N2 111.5(3) . . ?
C2 N3 H3N 124.8 . . ?
N2 N3 H3N 123.3 . . ?
C8 N4 C4 117.8(3) . . ?
C8 N4 Cu1 128.3(2) . . ?
C4 N4 Cu1 113.9(2) . . ?
C9 N5 C10 103.6(3) . . ?
C9 N5 Cu1 147.8(3) . 2_554 ?
C10 N5 Cu1 107.4(2) . 2_554 ?
C10 N6 N7 101.9(3) . . ?
C9 N7 N6 111.1(3) . . ?
C9 N7 H7N 126.5 . . ?
N6 N7 H7N 121.4 . . ?
C11 N8 C15 119.3(3) . . ?
C11 N8 Cu1 118.4(3) . 2_554 ?
C15 N8 Cu1 122.2(3) . 2_554 ?
C9 C1 C2 112.6(3) . . ?
C9 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
C9 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
N3 C2 N1 108.3(3) . . ?
N3 C2 C1 125.9(3) . . ?
N1 C2 C1 125.8(3) . . ?
N2 C3 N1 114.2(3) . . ?
N2 C3 C4 128.3(3) . . ?
N1 C3 C4 117.4(3) . . ?
N4 C4 C5 122.7(3) . . ?
N4 C4 C3 112.7(3) . . ?
C5 C4 C3 124.6(3) . . ?
C4 C5 C6 118.5(3) . . ?
C4 C5 H5A 120.8 . . ?
C6 C5 H5A 120.8 . . ?
C7 C6 C5 119.2(3) . . ?
C7 C6 H6A 120.4 . . ?
C5 C6 H6A 120.4 . . ?
C8 C7 C6 119.1(3) . . ?
C8 C7 H7A 120.5 . . ?
C6 C7 H7A 120.5 . . ?
N4 C8 C7 122.7(3) . . ?
N4 C8 H8A 118.7 . . ?
C7 C8 H8A 118.7 . . ?
N5 C9 N7 108.9(3) . . ?
N5 C9 C1 127.0(3) . . ?
N7 C9 C1 124.1(3) . . ?
N6 C10 N5 114.4(3) . . ?
N6 C10 C11 125.9(3) . . ?
N5 C10 C11 119.7(3) . . ?
N8 C11 C12 122.0(4) . . ?
N8 C11 C10 113.6(3) . . ?
C12 C11 C10 124.4(3) . . ?
C11 C12 C13 118.8(4) . . ?
C11 C12 H12A 120.6 . . ?
C13 C12 H12A 120.6 . . ?
C14 C13 C12 119.0(4) . . ?
C14 C13 H13A 120.5 . . ?
C12 C13 H13A 120.5 . . ?
C15 C14 C13 119.2(4) . . ?
C15 C14 H14A 120.4 . . ?
C13 C14 H14A 120.4 . . ?
N8 C15 C14 121.6(4) . . ?
N8 C15 H15A 119.2 . . ?
C14 C15 H15A 119.2 . . ?
C1S O1S H1SO 111.2 . . ?
O1S C1S H1SE 104.6 . . ?
O1S C1S H1SF 109.1 . . ?
H1SE C1S H1SF 107.1 . . ?
O1S C1S H1SD 120.1 . . ?
H1SE C1S H1SD 107.7 . . ?
H1SF C1S H1SD 107.7 . . ?
O1S' C1S' H1SB 105.9 . . ?
O1S' C1S' H1SC 103.5 . . ?
H1SB C1S' H1SC 106.9 . . ?
O1S' C1S' H1SA 124.9 . . ?
H1SB C1S' H1SA 107.3 . . ?
H1SC C1S' H1SA 107.3 . . ?
C1S' O1S' H1O' 88.5 . . ?
C2S O2S H2SO 97.2 . . ?
C2S' O2S H2SO 95.2 . . ?
O2S C2S H2SA 110.6 . . ?
O2S C2S H2SB 108.7 . . ?
H2SA C2S H2SB 109.5 . . ?
O2S C2S H2SC 109.1 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
O2S C2S' H2SD 108.2 . . ?
O2S C2S' H2SE 110.7 . . ?
H2SD C2S' H2SE 109.5 . . ?
O2S C2S' H2SF 109.5 . . ?
H2SD C2S' H2SF 109.5 . . ?
H2SE C2S' H2SF 109.5 . . ?
C4S O4S C4S 115.0(9) 2_655 . ?
C4S O4S H4SO 10.1 2_655 . ?
C4S O4S H4SO 105.0 . . ?
C4S O4S H4SO 105.0(4) 2_655 2_655 ?
C4S O4S H4SO 10.1(4) . 2_655 ?
H4SO O4S H4SO 94.9 . 2_655 ?
O4S C4S H4SA 110.0 . . ?
O4S C4S H4SB 109.6 . . ?
H4SA C4S H4SB 109.5 . . ?
O4S C4S H4SC 108.8 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
O4S C4S H4SO 14.5(6) . 2_655 ?
H4SA C4S H4SO 124.5 . 2_655 ?
H4SB C4S H4SO 103.1 . 2_655 ?
H4SC C4S H4SO 100.0 . 2_655 ?
C5S O5S H5SO 121.2 . . ?
O5S C5S H5SA 109.4 . . ?
O5S C5S H5SB 109.7 . . ?
H5SA C5S H5SB 109.5 . . ?
O5S C5S H5SC 109.3 . . ?
H5SA C5S H5SC 109.5 . . ?
H5SB C5S H5SC 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3N Cl2 0.96 2.11 3.051(3) 167.8 7
N7 H7N O2S 0.85 1.86 2.698(4) 166.5 .
C5 H5A Cl1 0.95 2.72 3.424(4) 131.6 5
C8 H8A N8 0.95 2.68 3.182(5) 113.6 2_554
O1S H1SO Cl2 0.85 2.15 3.004(7) 179.4 4_545
O1S' H1O' Cl2 0.85 2.47 3.320(16) 177.3 4_545
O2S H2SO Cl2 0.93 2.14 3.065(3) 179.8 .

_refine_diff_density_max         1.053
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.116



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

data_1_sq
_database_code_depnum_ccdc_archive 'CCDC 1860808'
_audit_update_record             
;
2019-01-31 deposited with the CCDC.
2019-02-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H70 Cl Cu3 N30 Na2 O16'
_chemical_formula_weight         1883.63

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'
Cu Cu 0.3201 1.2651 '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'
Na Na 0.0362 0.0249 '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                   15.506(3)
_cell_length_b                   16.160(3)
_cell_length_c                   20.311(4)
_cell_angle_alpha                86.840(3)
_cell_angle_beta                 89.884(3)
_cell_angle_gamma                61.689(3)
_cell_volume                     4472.5(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1664
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      19.23

_exptl_crystal_description       prismatic
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_F_000             1932
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.824
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25974
_diffrn_reflns_av_unetI/netI     0.4572
_diffrn_reflns_av_R_equivalents  0.1480
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.396
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measured_fraction_theta_full 0.891
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_Laue_measured_fraction_full 0.891
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_point_group_measured_fraction_full 0.891
_reflns_number_total             14633
_reflns_number_gt                4410
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 4.0.0'
_computing_publication_material  'Bruker SHELXTL'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0200P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14633
_refine_ls_number_parameters     1124
_refine_ls_number_restraints     101
_refine_ls_R_factor_all          0.2127
_refine_ls_R_factor_gt           0.0658
_refine_ls_wR_factor_ref         0.1459
_refine_ls_wR_factor_gt          0.1142
_refine_ls_goodness_of_fit_ref   0.713
_refine_ls_restrained_S_all      0.719
_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
Cu1 Cu 0.08570(8) 0.35337(7) -0.71763(5) 0.0291(3) Uani 1 1 d . . . . .
Cu2 Cu 0.13442(8) 0.11825(7) -0.72382(5) 0.0309(3) Uani 1 1 d . . . . .
Cu3 Cu 0.32845(8) 0.16772(7) -0.70573(5) 0.0283(3) Uani 1 1 d . . . . .
Na1 Na 0.1488(2) 0.2049(2) -0.51756(14) 0.0278(8) Uani 1 1 d . . . . .
Na2 Na 0.2098(2) 0.2347(2) -0.91676(14) 0.0298(8) Uani 1 1 d . . . . .
N1 N 0.0132(5) 0.2943(5) -0.5939(3) 0.0280(17) Uani 1 1 d . . . . .
N2 N 0.0032(5) 0.3331(4) -0.6561(3) 0.0231(16) Uani 1 1 d . . . . .
N3 N -0.1411(5) 0.3382(5) -0.6314(3) 0.0265(17) Uani 1 1 d . . . . .
N4 N -0.0458(5) 0.4114(4) -0.7755(3) 0.0246(17) Uani 1 1 d . . . . .
N5 N -0.0093(6) 0.2138(5) -0.4766(3) 0.0353(19) Uani 1 1 d . . . . .
N6 N 0.1583(5) 0.3853(4) -0.7808(3) 0.0228(16) Uani 1 1 d . . . . .
N7 N 0.1981(5) 0.3540(5) -0.8401(3) 0.0317(19) Uani 1 1 d . . . . .
N8 N 0.2437(5) 0.4610(5) -0.8096(3) 0.0285(18) Uani 1 1 d . . . . .
N9 N 0.1072(5) 0.4523(5) -0.6658(3) 0.0274(17) Uani 1 1 d . . . . .
N10 N 0.2929(4) 0.3266(4) -0.9575(3) 0.0310(18) Uani 1 1 d D . . . .
N11 N 0.0592(5) 0.1794(5) -0.8047(3) 0.0291(18) Uani 1 1 d . . . . .
N12 N 0.0773(5) 0.2127(5) -0.8631(3) 0.0293(18) Uani 1 1 d . . . . .
N13 N -0.0812(5) 0.2420(5) -0.8643(3) 0.0315(18) Uani 1 1 d . . . . .
N14 N -0.0028(5) 0.1261(5) -0.6990(4) 0.0329(19) Uani 1 1 d . . . . .
N15 N 0.0575(6) 0.2979(5) -0.9871(3) 0.036(2) Uani 1 1 d . . . . .
N16 N 0.2033(5) 0.0481(5) -0.6440(3) 0.0278(18) Uani 1 1 d . . . . .
N17 N 0.2054(6) 0.0667(5) -0.5811(3) 0.0330(19) Uani 1 1 d . . . . .
N18 N 0.3091(5) -0.0878(5) -0.5909(3) 0.0286(18) Uani 1 1 d . . . . .
N19 N 0.2240(5) -0.0187(5) -0.7619(4) 0.035(2) Uani 1 1 d . . . . .
N20 N 0.2480(5) 0.0567(5) -0.4483(3) 0.0359(19) Uani 1 1 d . . . . .
N21 N 0.3117(5) 0.2402(5) -0.6296(3) 0.0226(17) Uani 1 1 d . . . . .
N22 N 0.2646(5) 0.2497(5) -0.5712(3) 0.0270(17) Uani 1 1 d . . . . .
N23 N 0.3307(5) 0.3493(4) -0.5761(3) 0.0258(17) Uani 1 1 d . . . . .
N24 N 0.4076(5) 0.2409(5) -0.7345(3) 0.0288(18) Uani 1 1 d . . . . .
N25 N 0.1830(5) 0.3094(5) -0.4503(3) 0.0316(18) Uani 1 1 d . . . . .
N26 N 0.3634(5) 0.0927(4) -0.7813(3) 0.0210(16) Uani 1 1 d . . . . .
N27 N 0.3366(5) 0.1102(5) -0.8468(3) 0.0269(17) Uani 1 1 d . . . . .
N28 N 0.4562(5) -0.0432(4) -0.8289(3) 0.0248(17) Uani 1 1 d . . . . .
N29 N 0.4302(5) 0.0341(5) -0.6608(3) 0.0254(17) Uani 1 1 d . . . . .
N30 N 0.3188(4) 0.0897(4) -0.9795(3) 0.0340(19) Uani 1 1 d D . . . .
O1MB O 0.1836(8) 0.2157(8) -0.7331(5) 0.021(3) Uiso 0.55 1 d . . P A 2
C1 C -0.0896(7) 0.3586(6) -0.6765(4) 0.029(2) Uani 1 1 d . . . . .
C2 C -0.0734(6) 0.2972(5) -0.5812(4) 0.024(2) Uani 1 1 d . . . . .
C3 C -0.1194(7) 0.4050(6) -0.7435(4) 0.029(2) Uani 1 1 d . U . . .
C4 C -0.2116(7) 0.4414(6) -0.7727(4) 0.034(2) Uani 1 1 d . U . . .
H4 H -0.2634 0.4388 -0.7492 0.040 Uiso 1 1 calc R U . . .
C5 C -0.2288(7) 0.4829(6) -0.8381(4) 0.043(2) Uani 1 1 d . U . . .
H5 H -0.2906 0.5055 -0.8601 0.051 Uiso 1 1 calc R U . . .
C6 C -0.1533(7) 0.4889(6) -0.8680(4) 0.039(2) Uani 1 1 d . . . . .
H6 H -0.1629 0.5186 -0.9111 0.047 Uiso 1 1 calc R U . . .
C7 C -0.0622(7) 0.4521(6) -0.8361(4) 0.034(2) Uani 1 1 d . . . . .
H7 H -0.0102 0.4562 -0.8583 0.041 Uiso 1 1 calc R U . . .
C8 C -0.0875(7) 0.2544(6) -0.5194(4) 0.031(2) Uani 1 1 d . . . . .
C9 C -0.1752(7) 0.2565(6) -0.5055(4) 0.038(2) Uani 1 1 d . . . . .
H9 H -0.2292 0.2881 -0.5358 0.045 Uiso 1 1 calc R U . . .
C10 C -0.1856(8) 0.2122(7) -0.4470(5) 0.047(3) Uani 1 1 d . . . . .
H10 H -0.2450 0.2113 -0.4370 0.056 Uiso 1 1 calc R U . . .
C11 C -0.1059(8) 0.1706(7) -0.4054(5) 0.050(3) Uani 1 1 d . . . . .
H11 H -0.1085 0.1384 -0.3655 0.060 Uiso 1 1 calc R U . . .
C12 C -0.0203(8) 0.1749(7) -0.4208(4) 0.054(3) Uani 1 1 d . . . . .
H12 H 0.0327 0.1483 -0.3895 0.064 Uiso 1 1 calc R U . . .
C13 C 0.1862(6) 0.4493(6) -0.7642(3) 0.029(2) Uani 1 1 d D . . . .
C14 C 0.2473(6) 0.4010(5) -0.8554(3) 0.023(2) Uani 1 1 d D . . . .
C15 C 0.1570(6) 0.4904(6) -0.7005(4) 0.026(2) Uani 1 1 d . . . . .
C16 C 0.1744(6) 0.5582(6) -0.6760(4) 0.030(2) Uani 1 1 d . . . . .
H16 H 0.2081 0.5842 -0.7016 0.036 Uiso 1 1 calc R U . . .
C17 C 0.1434(7) 0.5886(6) -0.6147(4) 0.037(2) Uani 1 1 d . . . . .
H17 H 0.1553 0.6357 -0.5974 0.045 Uiso 1 1 calc R U . . .
C18 C 0.0956(7) 0.5509(6) -0.5790(4) 0.040(3) Uani 1 1 d . . . . .
H18 H 0.0746 0.5713 -0.5361 0.048 Uiso 1 1 calc R U . . .
C19 C 0.0766(6) 0.4817(6) -0.6047(4) 0.033(2) Uani 1 1 d . . . . .
H19 H 0.0425 0.4559 -0.5794 0.040 Uiso 1 1 calc R U . . .
C20 C 0.3028(5) 0.3859(5) -0.9149(3) 0.032(2) Uani 1 1 d D . . . .
C21 C 0.3644(6) 0.4241(5) -0.9299(3) 0.066(4) Uani 1 1 d D U . . .
H21 H 0.3713 0.4645 -0.9005 0.079 Uiso 1 1 calc R U . . .
C22 C 0.4158(6) 0.4035(6) -0.9875(4) 0.086(5) Uani 1 1 d D U . . .
H22 H 0.4583 0.4293 -0.9976 0.103 Uiso 1 1 calc R U . . .
C23 C 0.4054(6) 0.3447(6) -1.0311(3) 0.046(3) Uani 1 1 d D U . . .
H23 H 0.4393 0.3312 -1.0714 0.055 Uiso 1 1 calc R U . . .
C24 C 0.3447(6) 0.3067(5) -1.0143(3) 0.036(2) Uani 1 1 d D . . . .
H24 H 0.3387 0.2652 -1.0431 0.043 Uiso 1 1 calc R U . . .
C25 C -0.0359(7) 0.1986(6) -0.8079(4) 0.029(2) Uani 1 1 d . . . . .
C26 C -0.0080(7) 0.2490(6) -0.8964(4) 0.025(2) Uani 1 1 d . . . . .
C27 C -0.0720(7) 0.1700(6) -0.7498(4) 0.035(2) Uani 1 1 d . . . . .
C28 C -0.1678(9) 0.1849(7) -0.7421(5) 0.053(3) Uani 1 1 d . . . . .
H28 H -0.2166 0.2174 -0.7758 0.063 Uiso 1 1 calc R U . . .
C29 C -0.1895(9) 0.1509(8) -0.6839(5) 0.060(3) Uani 1 1 d . . . . .
H29 H -0.2541 0.1600 -0.6778 0.073 Uiso 1 1 calc R U . . .
C30 C -0.1199(8) 0.1046(7) -0.6351(5) 0.047(3) Uani 1 1 d . . . . .
H30 H -0.1341 0.0785 -0.5962 0.056 Uiso 1 1 calc R U . . .
C31 C -0.0303(8) 0.0971(6) -0.6439(4) 0.041(3) Uani 1 1 d . . . . .
H31 H 0.0165 0.0693 -0.6085 0.049 Uiso 1 1 calc R U . . .
C32 C -0.0228(7) 0.2947(6) -0.9632(4) 0.029(2) Uani 1 1 d . . . . .
C33 C -0.1073(7) 0.3288(7) -0.9981(4) 0.047(3) Uani 1 1 d . . . . .
H33 H -0.1626 0.3262 -0.9800 0.057 Uiso 1 1 calc R U . . .
C34 C -0.1115(8) 0.3676(7) -1.0607(5) 0.060(3) Uani 1 1 d . U . . .
H34 H -0.1711 0.3924 -1.0859 0.072 Uiso 1 1 calc R U . . .
C35 C -0.0344(8) 0.3715(7) -1.0875(5) 0.054(2) Uani 1 1 d . U . . .
H35 H -0.0380 0.3984 -1.1308 0.064 Uiso 1 1 calc R U . . .
C36 C 0.0489(7) 0.3355(7) -1.0498(4) 0.046(2) Uani 1 1 d . U . . .
H36 H 0.1047 0.3366 -1.0684 0.055 Uiso 1 1 calc R U . . .
C37 C 0.2626(6) -0.0447(6) -0.6478(4) 0.027(2) Uani 1 1 d D . . . .
C38 C 0.2680(6) -0.0142(6) -0.5493(4) 0.029(2) Uani 1 1 d D . . . .
C39 C 0.2760(6) -0.0848(6) -0.7135(4) 0.027(2) Uani 1 1 d . . . . .
C40 C 0.3324(7) -0.1774(6) -0.7266(5) 0.046(3) Uani 1 1 d . . . . .
H40 H 0.3693 -0.2228 -0.6922 0.055 Uiso 1 1 calc R U . . .
C41 C 0.3349(8) -0.2038(7) -0.7897(5) 0.060(3) Uani 1 1 d . . . . .
H41 H 0.3702 -0.2681 -0.7994 0.072 Uiso 1 1 calc R U . . .
C42 C 0.2857(8) -0.1355(7) -0.8384(5) 0.056(3) Uani 1 1 d . . . . .
H42 H 0.2905 -0.1517 -0.8830 0.067 Uiso 1 1 calc R U . . .
C43 C 0.2282(7) -0.0419(7) -0.8230(4) 0.047(3) Uani 1 1 d . . . . .
H43 H 0.1922 0.0049 -0.8570 0.056 Uiso 1 1 calc R U . . .
C44 C 0.2943(7) -0.0237(6) -0.4788(4) 0.031(2) Uani 1 1 d . . . . .
C45 C 0.3623(7) -0.1042(6) -0.4454(4) 0.040(2) Uani 1 1 d . . . . .
H45 H 0.3970 -0.1596 -0.4686 0.048 Uiso 1 1 calc R U . . .
C46 C 0.3813(7) -0.1070(7) -0.3798(4) 0.039(2) Uani 1 1 d . . . . .
H46 H 0.4266 -0.1641 -0.3568 0.047 Uiso 1 1 calc R U . . .
C47 C 0.3338(7) -0.0254(7) -0.3474(4) 0.041(3) Uani 1 1 d . . . . .
H47 H 0.3459 -0.0250 -0.3016 0.049 Uiso 1 1 calc R U . . .
C48 C 0.2671(7) 0.0570(7) -0.3831(4) 0.039(3) Uani 1 1 d . . . . .
H48 H 0.2347 0.1141 -0.3614 0.047 Uiso 1 1 calc R U . . .
C49 C 0.3486(6) 0.2988(6) -0.6307(4) 0.027(2) Uani 1 1 d . . . . .
C50 C 0.2792(6) 0.3143(6) -0.5405(4) 0.023(2) Uani 1 1 d . . . . .
C51 C 0.4067(6) 0.2993(6) -0.6883(4) 0.028(2) Uani 1 1 d . . . . .
C52 C 0.4573(6) 0.3510(6) -0.6945(4) 0.036(2) Uani 1 1 d . . . . .
H52 H 0.4529 0.3931 -0.6622 0.043 Uiso 1 1 calc R U . . .
C53 C 0.5142(7) 0.3389(7) -0.7493(4) 0.044(3) Uani 1 1 d . . . . .
H53 H 0.5534 0.3695 -0.7543 0.053 Uiso 1 1 calc R U . . .
C54 C 0.5129(7) 0.2809(7) -0.7972(4) 0.049(3) Uani 1 1 d . . . . .
H54 H 0.5479 0.2753 -0.8365 0.059 Uiso 1 1 calc R U . . .
C55 C 0.4611(6) 0.2311(6) -0.7879(4) 0.034(2) Uani 1 1 d . . . . .
H55 H 0.4637 0.1895 -0.8201 0.041 Uiso 1 1 calc R U . . .
C56 C 0.2428(6) 0.3427(5) -0.4751(4) 0.026(2) Uani 1 1 d . . . . .
C57 C 0.2697(6) 0.3997(6) -0.4410(4) 0.031(2) Uani 1 1 d . . . . .
H57 H 0.3072 0.4264 -0.4607 0.038 Uiso 1 1 calc R U . . .
C58 C 0.2384(7) 0.4153(6) -0.3764(4) 0.039(2) Uani 1 1 d . . . . .
H58 H 0.2580 0.4509 -0.3504 0.046 Uiso 1 1 calc R U . . .
C59 C 0.1809(7) 0.3810(6) -0.3499(4) 0.038(2) Uani 1 1 d . . . . .
H59 H 0.1592 0.3926 -0.3059 0.046 Uiso 1 1 calc R U . . .
C60 C 0.1542(6) 0.3281(6) -0.3889(4) 0.026(2) Uani 1 1 d . . . . .
H60 H 0.1134 0.3042 -0.3706 0.031 Uiso 1 1 calc R U . . .
C61 C 0.4323(6) 0.0041(6) -0.7733(4) 0.027(2) Uani 1 1 d . . . . .
C62 C 0.3928(6) 0.0257(6) -0.8721(4) 0.024(2) Uani 1 1 d . . . . .
C63 C 0.4719(6) -0.0324(6) -0.7061(4) 0.028(2) Uani 1 1 d . . . . .
C64 C 0.5396(6) -0.1243(6) -0.6890(4) 0.030(2) Uani 1 1 d . . . . .
H64 H 0.5668 -0.1694 -0.7214 0.036 Uiso 1 1 calc R U . . .
C65 C 0.5674(6) -0.1494(6) -0.6221(4) 0.035(2) Uani 1 1 d . . . . .
H65 H 0.6144 -0.2118 -0.6080 0.042 Uiso 1 1 calc R U . . .
C66 C 0.5244(7) -0.0809(6) -0.5777(4) 0.036(2) Uani 1 1 d . . . . .
H66 H 0.5415 -0.0959 -0.5321 0.043 Uiso 1 1 calc R U . . .
C67 C 0.4565(6) 0.0097(6) -0.5991(4) 0.031(2) Uani 1 1 d . . . . .
H67 H 0.4280 0.0559 -0.5676 0.038 Uiso 1 1 calc R U . . .
C68 C 0.3867(5) 0.0122(5) -0.9423(3) 0.030(2) Uani 1 1 d D . . . .
C69 C 0.4429(5) -0.0722(4) -0.9709(3) 0.040(3) Uani 1 1 d D . . . .
H69 H 0.4894 -0.1256 -0.9449 0.048 Uiso 1 1 calc R U . . .
C70 C 0.4307(5) -0.0781(5) -1.0385(3) 0.051(3) Uani 1 1 d D . . . .
H70 H 0.4688 -0.1357 -1.0587 0.062 Uiso 1 1 calc R U . . .
C71 C 0.3632(6) -0.0001(5) -1.0758(3) 0.048(3) Uani 1 1 d D . . . .
H71 H 0.3544 -0.0040 -1.1215 0.057 Uiso 1 1 calc R U . . .
C72 C 0.3081(5) 0.0841(5) -1.0461(3) 0.040(3) Uani 1 1 d D . . . .
H72 H 0.2627 0.1382 -1.0720 0.048 Uiso 1 1 calc R U . . .
Cl1 Cl 0.1608(3) 0.2072(3) -0.21190(14) 0.0842(11) Uani 1 1 d . U . . .
O1S O 0.1334(6) 0.1625(6) -0.1595(3) 0.089(3) Uani 1 1 d . U . . .
O2S O 0.1813(7) 0.2765(7) -0.1861(4) 0.122(3) Uani 1 1 d . U . . .
O3S O 0.2484(8) 0.1412(9) -0.2368(5) 0.149(4) Uani 1 1 d . U . . .
O4S O 0.0921(8) 0.2379(9) -0.2626(4) 0.168(5) Uani 1 1 d . U . . .
O1W O 0.3818(4) 0.4939(4) -0.5606(3) 0.0464(17) Uani 1 1 d . . . . .
H1WA H 0.3731 0.4446 -0.5610 0.070 Uiso 1 1 d R U . . .
H1WB H 0.3882 0.5052 -0.5200 0.070 Uiso 1 1 d R U . . .
O2W O 0.5409(4) -0.3983(4) -0.6626(3) 0.0520(18) Uani 1 1 d . . . . .
H2WA H 0.4905 -0.4045 -0.6745 0.078 Uiso 1 1 d R U . . .
H2WB H 0.5192 -0.3582 -0.6319 0.078 Uiso 1 1 d R U . . .
O3W O 0.6152(5) -0.2276(4) -0.8380(3) 0.0542(19) Uani 1 1 d . . . . .
H3WA H 0.6016 -0.2716 -0.8235 0.081 Uiso 1 1 d R U . . .
H3WB H 0.5618 -0.1754 -0.8327 0.081 Uiso 1 1 d R U . . .
O4W O 0.4654(4) -0.2780(4) -0.5647(3) 0.0539(18) Uani 1 1 d . . . . .
H4WA H 0.4220 -0.2219 -0.5548 0.081 Uiso 1 1 d R U . . .
H4WB H 0.5036 -0.3011 -0.5297 0.081 Uiso 1 1 d R U . . .
O5W O -0.3483(4) 0.4087(4) -0.6442(3) 0.0521(18) Uani 1 1 d . . . . .
H5WA H -0.2871 0.3956 -0.6423 0.078 Uiso 1 1 d R U . . .
H5WB H -0.3652 0.4110 -0.6032 0.078 Uiso 1 1 d R U . . .
O6W O 0.3628(5) 0.6033(5) -0.6709(3) 0.063(2) Uani 1 1 d . . . . .
H6WA H 0.3131 0.6596 -0.6706 0.095 Uiso 1 1 d R U . . .
H6WB H 0.3539 0.5810 -0.7067 0.095 Uiso 1 1 d R U . . .
O7W O 0.5670(5) -0.3613(5) -0.7917(3) 0.070(2) Uani 1 1 d . . . . .
H7WA H 0.5641 -0.3922 -0.8246 0.105 Uiso 1 1 d R U . . .
H7WB H 0.5548 -0.3882 -0.7573 0.105 Uiso 1 1 d R U . . .
O8W O 0.3199(7) 0.5851(6) -0.8002(3) 0.127(4) Uani 1 1 d . . . . .
H8WA H 0.3474 0.5705 -0.8382 0.190 Uiso 1 1 d R U . . .
H8WB H 0.2812 0.5599 -0.7982 0.190 Uiso 1 1 d R U . . .
O9W O 0.5811(4) 0.3899(4) -0.5237(3) 0.0566(19) Uani 1 1 d . . . . .
H9WA H 0.5890 0.3331 -0.5168 0.085 Uiso 1 1 d R U . . .
H9WB H 0.5179 0.4255 -0.5273 0.085 Uiso 1 1 d R U . . .
O1 O 0.7043(8) 0.3141(9) -0.8874(4) 0.083(4) Uani 0.67 1 d . . P B 1
O2 O 0.5441(8) 0.5013(8) -0.8559(5) 0.073(3) Uani 0.67 1 d . . P C 1
O3 O 0.4679(16) 0.5716(15) -0.8804(9) 0.052(6) Uiso 0.33 1 d . . P D 2
O4 O 0.6133(19) 0.4105(18) -0.9255(12) 0.091(8) Uiso 0.33 1 d . . P E 2
O1MA O 0.1837(10) 0.2083(9) -0.7081(7) 0.023(4) Uiso 0.45 1 d . . P A 1


_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 N2 1.911(6) . ?
Cu1 N6 1.911(6) . ?
Cu1 O1MB 2.056(11) . ?
Cu1 O1MA 2.102(14) . ?
Cu1 N9 2.115(6) . ?
Cu1 N4 2.120(7) . ?
Cu2 N16 1.927(6) . ?
Cu2 N11 1.942(7) . ?
Cu2 O1MA 1.977(13) . ?
Cu2 O1MB 2.049(10) . ?
Cu2 N14 2.132(7) . ?
Cu2 N19 2.167(7) . ?
Cu3 N26 1.923(6) . ?
Cu3 N21 1.934(6) . ?
Cu3 O1MA 2.018(14) . ?
Cu3 O1MB 2.065(11) . ?
Cu3 N24 2.131(6) . ?
Cu3 N29 2.131(7) . ?
Na1 N1 2.408(7) . ?
Na1 N17 2.424(7) . ?
Na1 N22 2.465(7) . ?
Na1 N25 2.471(7) . ?
Na1 N20 2.495(8) . ?
Na1 N5 2.528(7) . ?
Na2 N27 2.425(7) . ?
Na2 N7 2.484(7) . ?
Na2 N12 2.486(7) . ?
Na2 N10 2.494(6) . ?
Na2 N15 2.495(8) . ?
Na2 N30 2.556(6) . ?
N1 C2 1.346(9) . ?
N1 N2 1.354(8) . ?
N2 C1 1.355(10) . ?
N3 C1 1.342(9) . ?
N3 C2 1.360(10) . ?
N4 C7 1.329(9) . ?
N4 C3 1.355(9) . ?
N5 C12 1.316(10) . ?
N5 C8 1.357(10) . ?
N6 C13 1.357(9) . ?
N6 N7 1.362(8) . ?
N7 C14 1.333(8) . ?
N8 C13 1.347(9) . ?
N8 C14 1.363(9) . ?
N9 C19 1.355(9) . ?
N9 C15 1.368(9) . ?
N10 C24 1.367(6) . ?
N10 C20 1.387(6) . ?
N11 C25 1.357(10) . ?
N11 N12 1.359(8) . ?
N12 C26 1.331(10) . ?
N13 C25 1.321(10) . ?
N13 C26 1.355(9) . ?
N14 C31 1.335(10) . ?
N14 C27 1.386(11) . ?
N15 C32 1.358(10) . ?
N15 C36 1.360(10) . ?
N16 N17 1.332(8) . ?
N16 C37 1.343(10) . ?
N17 C38 1.332(11) . ?
N18 C37 1.334(10) . ?
N18 C38 1.387(9) . ?
N19 C43 1.310(9) . ?
N19 C39 1.351(10) . ?
N20 C44 1.337(10) . ?
N20 C48 1.359(9) . ?
N21 C49 1.317(9) . ?
N21 N22 1.369(8) . ?
N22 C50 1.352(9) . ?
N23 C49 1.362(9) . ?
N23 C50 1.364(9) . ?
N24 C55 1.336(9) . ?
N24 C51 1.363(9) . ?
N25 C60 1.326(9) . ?
N25 C56 1.359(9) . ?
N26 C61 1.320(10) . ?
N26 N27 1.367(8) . ?
N27 C62 1.355(10) . ?
N28 C61 1.351(9) . ?
N28 C62 1.355(10) . ?
N29 C67 1.298(9) . ?
N29 C63 1.367(9) . ?
N30 C72 1.376(6) . ?
N30 C68 1.377(7) . ?
C1 C3 1.479(11) . ?
C2 C8 1.465(10) . ?
C3 C4 1.383(11) . ?
C4 C5 1.420(11) . ?
C5 C6 1.359(11) . ?
C6 C7 1.391(11) . ?
C8 C9 1.374(10) . ?
C9 C10 1.401(11) . ?
C10 C11 1.359(12) . ?
C11 C12 1.395(12) . ?
C13 C15 1.459(10) . ?
C14 C20 1.447(9) . ?
C15 C16 1.364(10) . ?
C16 C17 1.365(11) . ?
C17 C18 1.350(10) . ?
C18 C19 1.410(10) . ?
C20 C21 1.387(7) . ?
C21 C22 1.379(7) . ?
C22 C23 1.397(7) . ?
C23 C24 1.380(6) . ?
C25 C27 1.450(11) . ?
C26 C32 1.474(11) . ?
C27 C28 1.398(12) . ?
C28 C29 1.383(12) . ?
C29 C30 1.365(13) . ?
C30 C31 1.348(11) . ?
C32 C33 1.341(11) . ?
C33 C34 1.375(11) . ?
C34 C35 1.340(12) . ?
C35 C36 1.354(12) . ?
C37 C39 1.486(10) . ?
C38 C44 1.469(10) . ?
C39 C40 1.370(12) . ?
C40 C41 1.368(12) . ?
C41 C42 1.364(13) . ?
C42 C43 1.397(12) . ?
C44 C45 1.367(12) . ?
C45 C46 1.360(11) . ?
C46 C47 1.372(12) . ?
C47 C48 1.400(12) . ?
C49 C51 1.476(10) . ?
C50 C56 1.452(10) . ?
C51 C52 1.392(10) . ?
C52 C53 1.384(11) . ?
C53 C54 1.394(11) . ?
C54 C55 1.386(10) . ?
C56 C57 1.391(10) . ?
C57 C58 1.392(11) . ?
C58 C59 1.353(10) . ?
C59 C60 1.393(10) . ?
C61 C63 1.468(11) . ?
C62 C68 1.463(9) . ?
C63 C64 1.377(11) . ?
C64 C65 1.404(10) . ?
C65 C66 1.375(11) . ?
C66 C67 1.383(11) . ?
C68 C69 1.385(7) . ?
C69 C70 1.402(7) . ?
C70 C71 1.380(7) . ?
C71 C72 1.389(7) . ?
Cl1 O4S 1.374(9) . ?
Cl1 O3S 1.386(11) . ?
Cl1 O2S 1.426(9) . ?
Cl1 O1S 1.428(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
N2 Cu1 N6 174.6(3) . . ?
N2 Cu1 O1MB 99.3(4) . . ?
N6 Cu1 O1MB 85.8(4) . . ?
N2 Cu1 O1MA 88.7(4) . . ?
N6 Cu1 O1MA 96.6(4) . . ?
N2 Cu1 N9 98.1(3) . . ?
N6 Cu1 N9 80.0(2) . . ?
O1MB Cu1 N9 129.0(4) . . ?
O1MA Cu1 N9 122.3(4) . . ?
N2 Cu1 N4 80.6(3) . . ?
N6 Cu1 N4 95.6(3) . . ?
O1MB Cu1 N4 115.3(3) . . ?
O1MA Cu1 N4 123.0(4) . . ?
N9 Cu1 N4 114.7(2) . . ?
N16 Cu2 N11 173.7(3) . . ?
N16 Cu2 O1MA 88.1(4) . . ?
N11 Cu2 O1MA 98.2(4) . . ?
N16 Cu2 O1MB 100.7(4) . . ?
N11 Cu2 O1MB 85.6(4) . . ?
N16 Cu2 N14 95.8(3) . . ?
N11 Cu2 N14 79.8(3) . . ?
O1MA Cu2 N14 129.1(4) . . ?
O1MB Cu2 N14 133.7(4) . . ?
N16 Cu2 N19 80.0(3) . . ?
N11 Cu2 N19 96.9(3) . . ?
O1MA Cu2 N19 123.3(4) . . ?
O1MB Cu2 N19 118.1(4) . . ?
N14 Cu2 N19 107.2(2) . . ?
N26 Cu3 N21 172.1(3) . . ?
N26 Cu3 O1MA 97.8(4) . . ?
N21 Cu3 O1MA 90.1(4) . . ?
N26 Cu3 O1MB 87.6(3) . . ?
N21 Cu3 O1MB 99.9(4) . . ?
N26 Cu3 N24 94.8(2) . . ?
N21 Cu3 N24 79.3(2) . . ?
O1MA Cu3 N24 131.5(4) . . ?
O1MB Cu3 N24 122.8(3) . . ?
N26 Cu3 N29 79.8(3) . . ?
N21 Cu3 N29 97.0(3) . . ?
O1MA Cu3 N29 120.4(4) . . ?
O1MB Cu3 N29 128.6(3) . . ?
N24 Cu3 N29 107.9(2) . . ?
N1 Na1 N17 91.5(2) . . ?
N1 Na1 N22 96.6(2) . . ?
N17 Na1 N22 91.5(2) . . ?
N1 Na1 N25 111.3(2) . . ?
N17 Na1 N25 150.5(3) . . ?
N22 Na1 N25 68.2(2) . . ?
N1 Na1 N20 148.6(2) . . ?
N17 Na1 N20 68.1(2) . . ?
N22 Na1 N20 107.1(3) . . ?
N25 Na1 N20 96.7(2) . . ?
N1 Na1 N5 67.7(2) . . ?
N17 Na1 N5 99.4(2) . . ?
N22 Na1 N5 160.9(3) . . ?
N25 Na1 N5 106.4(3) . . ?
N20 Na1 N5 91.5(2) . . ?
N27 Na2 N7 90.7(2) . . ?
N27 Na2 N12 92.8(2) . . ?
N7 Na2 N12 93.6(2) . . ?
N27 Na2 N10 102.1(2) . . ?
N7 Na2 N10 66.9(2) . . ?
N12 Na2 N10 155.2(2) . . ?
N27 Na2 N15 151.1(2) . . ?
N7 Na2 N15 110.2(3) . . ?
N12 Na2 N15 67.0(2) . . ?
N10 Na2 N15 104.4(2) . . ?
N27 Na2 N30 67.4(2) . . ?
N7 Na2 N30 148.1(3) . . ?
N12 Na2 N30 109.6(2) . . ?
N10 Na2 N30 94.4(2) . . ?
N15 Na2 N30 99.1(2) . . ?
C2 N1 N2 105.4(7) . . ?
C2 N1 Na1 118.4(5) . . ?
N2 N1 Na1 135.1(5) . . ?
C1 N2 N1 106.0(6) . . ?
C1 N2 Cu1 117.5(5) . . ?
N1 N2 Cu1 136.4(6) . . ?
C1 N3 C2 101.0(7) . . ?
C7 N4 C3 119.6(7) . . ?
C7 N4 Cu1 127.9(6) . . ?
C3 N4 Cu1 112.4(5) . . ?
C12 N5 C8 117.1(8) . . ?
C12 N5 Na1 126.2(7) . . ?
C8 N5 Na1 116.4(5) . . ?
C13 N6 N7 107.0(6) . . ?
C13 N6 Cu1 117.1(5) . . ?
N7 N6 Cu1 135.6(5) . . ?
C14 N7 N6 104.6(6) . . ?
C14 N7 Na2 117.1(5) . . ?
N6 N7 Na2 138.2(5) . . ?
C13 N8 C14 101.2(5) . . ?
C19 N9 C15 118.6(7) . . ?
C19 N9 Cu1 127.8(6) . . ?
C15 N9 Cu1 113.6(5) . . ?
C24 N10 C20 118.8(5) . . ?
C24 N10 Na2 121.8(4) . . ?
C20 N10 Na2 118.1(4) . . ?
C25 N11 N12 106.5(7) . . ?
C25 N11 Cu2 118.2(6) . . ?
N12 N11 Cu2 135.3(6) . . ?
C26 N12 N11 103.8(7) . . ?
C26 N12 Na2 116.4(5) . . ?
N11 N12 Na2 139.6(6) . . ?
C25 N13 C26 100.8(7) . . ?
C31 N14 C27 117.9(8) . . ?
C31 N14 Cu2 130.5(7) . . ?
C27 N14 Cu2 111.6(6) . . ?
C32 N15 C36 116.2(8) . . ?
C32 N15 Na2 119.8(5) . . ?
C36 N15 Na2 124.0(6) . . ?
N17 N16 C37 106.8(6) . . ?
N17 N16 Cu2 136.1(6) . . ?
C37 N16 Cu2 117.0(5) . . ?
C38 N17 N16 106.5(6) . . ?
C38 N17 Na1 115.3(5) . . ?
N16 N17 Na1 137.4(5) . . ?
C37 N18 C38 100.9(7) . . ?
C43 N19 C39 120.3(8) . . ?
C43 N19 Cu2 127.5(7) . . ?
C39 N19 Cu2 112.1(5) . . ?
C44 N20 C48 119.3(8) . . ?
C44 N20 Na1 117.9(6) . . ?
C48 N20 Na1 122.1(6) . . ?
C49 N21 N22 106.8(6) . . ?
C49 N21 Cu3 118.3(5) . . ?
N22 N21 Cu3 134.8(5) . . ?
C50 N22 N21 104.5(6) . . ?
C50 N22 Na1 115.1(5) . . ?
N21 N22 Na1 139.6(5) . . ?
C49 N23 C50 100.1(6) . . ?
C55 N24 C51 118.6(7) . . ?
C55 N24 Cu3 128.4(6) . . ?
C51 N24 Cu3 112.8(5) . . ?
C60 N25 C56 117.4(7) . . ?
C60 N25 Na1 124.1(6) . . ?
C56 N25 Na1 118.2(5) . . ?
C61 N26 N27 107.3(6) . . ?
C61 N26 Cu3 117.9(5) . . ?
N27 N26 Cu3 134.7(5) . . ?
C62 N27 N26 102.9(7) . . ?
C62 N27 Na2 118.6(5) . . ?
N26 N27 Na2 137.7(5) . . ?
C61 N28 C62 99.3(7) . . ?
C67 N29 C63 118.6(8) . . ?
C67 N29 Cu3 129.5(6) . . ?
C63 N29 Cu3 111.9(5) . . ?
C72 N30 C68 119.9(5) . . ?
C72 N30 Na2 123.5(4) . . ?
C68 N30 Na2 116.4(4) . . ?
Cu2 O1MB Cu1 117.8(5) . . ?
Cu2 O1MB Cu3 115.8(5) . . ?
Cu1 O1MB Cu3 117.7(5) . . ?
N3 C1 N2 113.7(7) . . ?
N3 C1 C3 129.9(8) . . ?
N2 C1 C3 116.4(8) . . ?
N1 C2 N3 113.9(7) . . ?
N1 C2 C8 120.8(8) . . ?
N3 C2 C8 125.2(8) . . ?
N4 C3 C4 120.8(8) . . ?
N4 C3 C1 113.0(8) . . ?
C4 C3 C1 126.2(8) . . ?
C3 C4 C5 119.8(9) . . ?
C6 C5 C4 117.4(9) . . ?
C5 C6 C7 120.5(9) . . ?
N4 C7 C6 121.8(8) . . ?
N5 C8 C9 122.2(8) . . ?
N5 C8 C2 116.1(8) . . ?
C9 C8 C2 121.7(9) . . ?
C8 C9 C10 120.5(9) . . ?
C11 C10 C9 116.3(9) . . ?
C10 C11 C12 120.5(9) . . ?
N5 C12 C11 123.3(10) . . ?
N8 C13 N6 112.5(6) . . ?
N8 C13 C15 129.4(7) . . ?
N6 C13 C15 118.0(7) . . ?
N7 C14 N8 114.7(6) . . ?
N7 C14 C20 121.9(7) . . ?
N8 C14 C20 123.3(7) . . ?
C16 C15 N9 121.9(7) . . ?
C16 C15 C13 126.9(8) . . ?
N9 C15 C13 111.2(6) . . ?
C15 C16 C17 119.9(8) . . ?
C18 C17 C16 119.3(8) . . ?
C17 C18 C19 120.7(8) . . ?
N9 C19 C18 119.6(8) . . ?
C21 C20 N10 120.3(5) . . ?
C21 C20 C14 124.7(6) . . ?
N10 C20 C14 115.0(6) . . ?
C22 C21 C20 120.0(5) . . ?
C21 C22 C23 120.2(5) . . ?
C24 C23 C22 118.4(5) . . ?
N10 C24 C23 122.3(5) . . ?
N13 C25 N11 113.5(7) . . ?
N13 C25 C27 130.5(8) . . ?
N11 C25 C27 116.1(8) . . ?
N12 C26 N13 115.4(7) . . ?
N12 C26 C32 122.7(8) . . ?
N13 C26 C32 121.9(8) . . ?
N14 C27 C28 120.3(9) . . ?
N14 C27 C25 114.3(8) . . ?
C28 C27 C25 125.4(9) . . ?
C29 C28 C27 118.0(11) . . ?
C30 C29 C28 121.2(10) . . ?
C31 C30 C29 117.9(10) . . ?
N14 C31 C30 124.5(10) . . ?
C33 C32 N15 122.7(8) . . ?
C33 C32 C26 123.2(9) . . ?
N15 C32 C26 114.0(8) . . ?
C32 C33 C34 118.0(9) . . ?
C35 C34 C33 122.1(10) . . ?
C34 C35 C36 117.0(10) . . ?
C35 C36 N15 124.0(9) . . ?
N18 C37 N16 113.3(6) . . ?
N18 C37 C39 128.1(8) . . ?
N16 C37 C39 118.4(7) . . ?
N17 C38 N18 112.4(7) . . ?
N17 C38 C44 123.9(7) . . ?
N18 C38 C44 123.6(8) . . ?
N19 C39 C40 121.3(8) . . ?
N19 C39 C37 112.3(7) . . ?
C40 C39 C37 126.4(8) . . ?
C41 C40 C39 119.4(9) . . ?
C42 C41 C40 118.5(9) . . ?
C41 C42 C43 120.4(9) . . ?
N19 C43 C42 120.0(9) . . ?
N20 C44 C45 120.6(8) . . ?
N20 C44 C38 113.8(8) . . ?
C45 C44 C38 125.6(8) . . ?
C46 C45 C44 121.6(9) . . ?
C45 C46 C47 118.6(9) . . ?
C46 C47 C48 118.8(9) . . ?
N20 C48 C47 121.0(9) . . ?
N21 C49 N23 114.4(7) . . ?
N21 C49 C51 117.4(7) . . ?
N23 C49 C51 128.1(8) . . ?
N22 C50 N23 114.1(6) . . ?
N22 C50 C56 122.0(7) . . ?
N23 C50 C56 123.9(7) . . ?
N24 C51 C52 123.4(7) . . ?
N24 C51 C49 112.1(7) . . ?
C52 C51 C49 124.5(8) . . ?
C53 C52 C51 117.7(8) . . ?
C52 C53 C54 118.6(8) . . ?
C55 C54 C53 120.8(8) . . ?
N24 C55 C54 120.9(8) . . ?
N25 C56 C57 123.3(7) . . ?
N25 C56 C50 115.8(7) . . ?
C57 C56 C50 120.9(8) . . ?
C56 C57 C58 116.2(8) . . ?
C59 C58 C57 121.5(8) . . ?
C58 C59 C60 118.0(7) . . ?
N25 C60 C59 123.3(8) . . ?
N26 C61 N28 114.8(7) . . ?
N26 C61 C63 117.6(7) . . ?
N28 C61 C63 127.6(8) . . ?
N27 C62 N28 115.7(7) . . ?
N27 C62 C68 121.4(7) . . ?
N28 C62 C68 122.9(7) . . ?
N29 C63 C64 122.7(7) . . ?
N29 C63 C61 112.6(8) . . ?
C64 C63 C61 124.6(8) . . ?
C63 C64 C65 118.0(8) . . ?
C66 C65 C64 118.0(9) . . ?
C65 C66 C67 120.2(8) . . ?
N29 C67 C66 122.5(8) . . ?
N30 C68 C69 120.6(5) . . ?
N30 C68 C62 115.6(6) . . ?
C69 C68 C62 123.8(6) . . ?
C68 C69 C70 119.3(5) . . ?
C71 C70 C69 119.9(5) . . ?
C70 C71 C72 119.8(5) . . ?
N30 C72 C71 120.5(5) . . ?
O4S Cl1 O3S 106.9(7) . . ?
O4S Cl1 O2S 116.2(8) . . ?
O3S Cl1 O2S 105.5(6) . . ?
O4S Cl1 O1S 109.9(5) . . ?
O3S Cl1 O1S 108.7(7) . . ?
O2S Cl1 O1S 109.4(5) . . ?
Cu2 O1MA Cu3 121.5(7) . . ?
Cu2 O1MA Cu1 119.0(7) . . ?
Cu3 O1MA Cu1 117.8(6) . . ?

_refine_diff_density_max         0.569
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.073



