# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2309459'
loop_
_audit_author_name
_audit_author_address
'Carla Bazzicalupi'
;University of Firenze
Italy
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2023-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H109 Cl3 N28 O31'
_chemical_formula_weight         1680.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   36.1345(14)
_cell_length_b                   8.3617(3)
_cell_length_c                   25.1795(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.056(3)
_cell_angle_gamma                90
_cell_volume                     7603.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9797
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      79.66

_exptl_crystal_description       prismatic
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_F_000             3568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          1.000
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    1.966
_shelx_estimated_absorpt_T_min   0.244
_shelx_estimated_absorpt_T_max   0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4447
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44576
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.447
_diffrn_reflns_theta_max         80.154
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8184
_reflns_number_gt                7018
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_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)+(0.1406P)²+15.6119P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8184
_refine_ls_number_parameters     529
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0793
_refine_ls_wR_factor_ref         0.2401
_refine_ls_wR_factor_gt          0.2294
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.23037(2) 0.96986(9) 0.66127(3) 0.0347(2) Uani 1 1 d . . . . .
O21 O 0.47949(11) 0.2632(4) 0.7128(2) 0.0924(13) Uani 1 1 d . . . . .
N2 N 0.32882(7) 0.6829(3) 0.50666(9) 0.0311(5) Uani 1 1 d . . . . .
Cl2 Cl 0.500000 0.36114(14) 0.750000 0.0495(3) Uani 1 2 d S T P . .
O22 O 0.47505(11) 0.4580(6) 0.77667(18) 0.1026(15) Uani 1 1 d . . . . .
N13 N 0.34984(7) 0.7306(3) 0.28157(10) 0.0339(5) Uani 1 1 d . . . . .
H13A H 0.344128 0.664527 0.307227 0.041 Uiso 1 1 calc R U . . .
H13B H 0.334873 0.741128 0.253449 0.041 Uiso 1 1 calc R U . . .
O3 O 0.43328(6) 1.1181(3) 0.21756(8) 0.0348(5) Uani 1 1 d . . . . .
O11 O 0.23138(6) 0.8887(3) 0.71228(9) 0.0475(6) Uani 1 1 d . . . . .
N8 N 0.41409(7) 0.6162(3) 0.81937(10) 0.0316(5) Uani 1 1 d . . . . .
H8A H 0.417946 0.558039 0.790970 0.038 Uiso 1 1 calc R U . . .
H8B H 0.430567 0.616990 0.845966 0.038 Uiso 1 1 calc R U . . .
OW4 O 0.40621(6) 1.0890(3) 1.09849(8) 0.0377(5) Uani 1 1 d . . . . .
O14 O 0.24304(6) 0.8629(3) 0.62105(9) 0.0431(5) Uani 1 1 d . . . . .
O4 O 0.34131(6) 0.8656(3) 0.18809(9) 0.0388(5) Uani 1 1 d . . . . .
O12 O 0.19255(6) 1.0157(3) 0.64911(9) 0.0403(5) Uani 1 1 d . . . . .
O2 O 0.43001(6) 0.7353(3) 0.91285(8) 0.0398(5) Uani 1 1 d . . . . .
O13 O 0.25341(8) 1.1079(4) 0.66505(13) 0.0600(7) Uani 1 1 d . . . . .
OW6 O 0.48243(6) 0.8133(3) 0.98581(9) 0.0380(5) Uani 1 1 d . . . . .
OW5 O 0.47685(6) 0.9781(3) 1.07735(9) 0.0392(5) Uani 1 1 d . . . . .
N9 N 0.35949(6) 0.6971(3) 0.78087(8) 0.0254(5) Uani 1 1 d . . . . .
N1 N 0.40882(6) 0.6571(3) 0.48850(8) 0.0264(5) Uani 1 1 d . . . . .
N5 N 0.30387(6) 0.7713(3) 0.74371(8) 0.0280(5) Uani 1 1 d . . . . .
H5 H 0.284261 0.833740 0.743414 0.034 Uiso 1 1 calc R U . . .
N10 N 0.45671(6) 0.8552(3) 0.37479(8) 0.0278(5) Uani 1 1 d . . . . .
H10 H 0.476450 0.916096 0.379169 0.033 Uiso 1 1 calc R U . . .
N11 N 0.44338(6) 0.9975(3) 0.29796(8) 0.0270(5) Uani 1 1 d . . . . .
N14 N 0.40278(6) 0.7938(3) 0.32874(9) 0.0277(5) Uani 1 1 d . . . . .
N6 N 0.32057(6) 0.8860(3) 0.82451(8) 0.0270(5) Uani 1 1 d . . . . .
N4 N 0.42475(7) 0.5799(3) 0.60662(8) 0.0293(5) Uani 1 1 d . . . . .
N3 N 0.34130(7) 0.6092(3) 0.61607(9) 0.0305(5) Uani 1 1 d . . . . .
O1 O 0.33337(8) 0.9648(4) 0.90931(10) 0.0580(8) Uani 1 1 d . . . . .
N12 N 0.37221(7) 0.9400(3) 0.19599(9) 0.0323(5) Uani 1 1 d . . . . .
N7 N 0.39897(7) 0.8113(3) 0.91218(9) 0.0355(6) Uani 1 1 d . . . . .
C17 C 0.38349(7) 0.7025(3) 0.82209(10) 0.0258(5) Uani 1 1 d . . . . .
C20 C 0.43380(7) 0.8804(3) 0.33311(10) 0.0264(5) Uani 1 1 d . . . . .
C24 C 0.38082(7) 0.8136(3) 0.28526(10) 0.0269(5) Uani 1 1 d . . . . .
C13 C 0.32867(7) 0.7832(3) 0.78354(10) 0.0245(5) Uani 1 1 d . . . . .
C16 C 0.37700(8) 0.7960(4) 0.86902(10) 0.0290(6) Uani 1 1 d . . . . .
C22 C 0.42344(7) 1.0188(4) 0.24959(10) 0.0278(6) Uani 1 1 d . . . . .
OW1 O 0.37448(10) 0.8718(5) 0.02418(11) 0.0743(10) Uani 1 1 d . . . . .
C18 C 0.42420(7) 0.7873(3) 0.45684(10) 0.0268(5) Uani 1 1 d . . . . .
H18A H 0.438139 0.860950 0.480968 0.032 Uiso 1 1 calc R U . . .
H18B H 0.403503 0.848426 0.439878 0.032 Uiso 1 1 calc R U . . .
C23 C 0.39041(7) 0.9204(3) 0.24294(10) 0.0278(5) Uani 1 1 d . . . . .
C11 C 0.33427(8) 0.7228(3) 0.65870(10) 0.0277(5) Uani 1 1 d . . . . .
H11A H 0.323441 0.821420 0.642939 0.033 Uiso 1 1 calc R U . . .
H11B H 0.358147 0.751804 0.676673 0.033 Uiso 1 1 calc R U . . .
C19 C 0.45004(7) 0.7299(4) 0.41336(10) 0.0290(6) Uani 1 1 d . . . . .
H19A H 0.473942 0.695435 0.430074 0.035 Uiso 1 1 calc R U . . .
H19B H 0.438760 0.636390 0.394882 0.035 Uiso 1 1 calc R U . . .
C10 C 0.43924(8) 0.5550(4) 0.51084(10) 0.0304(6) Uani 1 1 d . . . . .
H10A H 0.461233 0.622376 0.519094 0.036 Uiso 1 1 calc R U . . .
H10B H 0.446143 0.475076 0.483928 0.036 Uiso 1 1 calc R U . . .
C12 C 0.30808(8) 0.6579(4) 0.70028(10) 0.0296(6) Uani 1 1 d . . . . .
H12A H 0.283528 0.636112 0.683089 0.036 Uiso 1 1 calc R U . . .
H12B H 0.317993 0.555778 0.714722 0.036 Uiso 1 1 calc R U . . .
C21 C 0.47661(7) 1.0950(4) 0.30865(11) 0.0300(6) Uani 1 1 d . . . . .
H21A H 0.479342 1.172260 0.279781 0.045 Uiso 1 1 calc R U . . .
H21B H 0.474225 1.152360 0.342302 0.045 Uiso 1 1 calc R U . . .
H21C H 0.498453 1.025552 0.311009 0.045 Uiso 1 1 calc R U . . .
C1 C 0.38120(8) 0.5642(4) 0.45750(10) 0.0317(6) Uani 1 1 d . . . . .
H1A H 0.377618 0.459324 0.474836 0.038 Uiso 1 1 calc R U . . .
H1B H 0.390365 0.544419 0.421509 0.038 Uiso 1 1 calc R U . . .
C15 C 0.34285(9) 0.8886(4) 0.87085(11) 0.0343(6) Uani 1 1 d . . . . .
C14 C 0.28608(8) 0.9789(4) 0.82280(12) 0.0349(6) Uani 1 1 d . . . . .
H14A H 0.284968 1.044853 0.854881 0.052 Uiso 1 1 calc R U . . .
H14B H 0.285372 1.048073 0.791356 0.052 Uiso 1 1 calc R U . . .
H14C H 0.264866 0.905847 0.821022 0.052 Uiso 1 1 calc R U . . .
C9 C 0.42803(9) 0.4687(4) 0.56115(11) 0.0322(6) Uani 1 1 d . . . . .
H9A H 0.403986 0.414425 0.554255 0.039 Uiso 1 1 calc R U . . .
H9B H 0.446715 0.385792 0.570462 0.039 Uiso 1 1 calc R U . . .
C5 C 0.30647(9) 0.5594(4) 0.58829(11) 0.0349(6) Uani 1 1 d . . . . .
H5A H 0.287255 0.642153 0.592941 0.042 Uiso 1 1 calc R U . . .
H5B H 0.297588 0.458268 0.603805 0.042 Uiso 1 1 calc R U . . .
C6 C 0.36290(9) 0.4695(4) 0.63445(12) 0.0380(7) Uani 1 1 d . . . . .
H6A H 0.362526 0.388393 0.605791 0.046 Uiso 1 1 calc R U . . .
H6B H 0.350785 0.421974 0.665362 0.046 Uiso 1 1 calc R U . . .
C4 C 0.31276(9) 0.5360(4) 0.52959(12) 0.0374(7) Uani 1 1 d . . . . .
H4A H 0.329807 0.444829 0.524751 0.045 Uiso 1 1 calc R U . . .
H4B H 0.288946 0.510741 0.510791 0.045 Uiso 1 1 calc R U . . .
C8 C 0.46169(9) 0.6249(5) 0.62914(11) 0.0405(7) Uani 1 1 d . . . . .
H8C H 0.458774 0.698204 0.659054 0.061 Uiso 1 1 calc R U . . .
H8D H 0.474830 0.528590 0.641533 0.061 Uiso 1 1 calc R U . . .
H8E H 0.475914 0.677583 0.601727 0.061 Uiso 1 1 calc R U . . .
C2 C 0.34472(8) 0.6507(4) 0.45296(10) 0.0359(7) Uani 1 1 d . . . . .
H2A H 0.326908 0.585751 0.431358 0.043 Uiso 1 1 calc R U . . .
H2B H 0.348191 0.753578 0.434304 0.043 Uiso 1 1 calc R U . . .
C7 C 0.40259(10) 0.5070(4) 0.65011(11) 0.0384(7) Uani 1 1 d . . . . .
H7A H 0.414928 0.407002 0.662145 0.046 Uiso 1 1 calc R U . . .
H7B H 0.402893 0.581545 0.680665 0.046 Uiso 1 1 calc R U . . .
OW2 O 0.31066(13) 0.8577(5) 0.07933(18) 0.1022(16) Uani 1 1 d . . . . .
C3 C 0.30182(10) 0.8161(5) 0.50230(14) 0.0478(8) Uani 1 1 d . . . . .
H3A H 0.313738 0.909924 0.487006 0.072 Uiso 1 1 calc R U . . .
H3B H 0.280670 0.783780 0.479333 0.072 Uiso 1 1 calc R U . . .
H3C H 0.293220 0.842839 0.537693 0.072 Uiso 1 1 calc R U . . .
OW3 O 0.2382(2) 0.7326(11) 0.0414(3) 0.094(3) Uani 0.5 1 d . . P . .
H3 H 0.4534(13) 1.004(5) 1.0868(18) 0.054(12) Uiso 1 1 d . . . . .
H2 H 0.4617(13) 0.800(6) 0.9652(19) 0.057(12) Uiso 1 1 d . . . . .
H4 H 0.4735(12) 0.908(6) 1.0522(19) 0.051(12) Uiso 1 1 d . . . . .
H1 H 0.4957(15) 0.876(7) 0.969(2) 0.069(15) Uiso 1 1 d . . . . .
H8 H 0.3954(18) 1.066(8) 1.127(3) 0.10(2) Uiso 1 1 d . . . . .
H12 H 0.3468(11) 0.714(5) 0.5296(16) 0.041(10) Uiso 1 1 d . . . . .
H11 H 0.4139(16) 0.677(8) 0.597(2) 0.016(13) Uiso 0.5 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 O13 1.424(3) . ?
Cl1 O14 1.438(2) . ?
Cl1 O12 1.442(2) . ?
Cl1 O11 1.452(2) . ?
O21 Cl2 1.431(4) . ?
N2 C3 1.483(4) . ?
N2 C4 1.484(4) . ?
N2 C2 1.512(3) . ?
Cl2 O22 1.401(3) 2_656 ?
Cl2 O22 1.401(3) . ?
N13 C24 1.318(4) . ?
O3 C22 1.219(3) . ?
N8 C17 1.324(4) . ?
O4 N12 1.288(3) . ?
O2 N7 1.289(3) . ?
N9 C17 1.329(3) . ?
N9 C13 1.330(3) . ?
N1 C1 1.467(3) . ?
N1 C18 1.470(3) . ?
N1 C10 1.486(4) . ?
N5 C13 1.325(3) . ?
N5 C12 1.460(3) . ?
N10 C20 1.330(4) . ?
N10 C19 1.455(3) . ?
N11 C20 1.373(3) . ?
N11 C22 1.404(3) . ?
N11 C21 1.468(3) . ?
N14 C20 1.336(4) . ?
N14 C24 1.339(4) . ?
N6 C13 1.382(3) . ?
N6 C15 1.394(4) . ?
N6 C14 1.468(3) . ?
N4 C8 1.480(4) . ?
N4 C9 1.483(3) . ?
N4 C7 1.508(4) . ?
N3 C11 1.462(3) . ?
N3 C6 1.470(4) . ?
N3 C5 1.477(4) . ?
O1 C15 1.219(4) . ?
N12 C23 1.342(4) . ?
N7 C16 1.329(4) . ?
C17 C16 1.443(4) . ?
C24 C23 1.442(4) . ?
C16 C15 1.459(4) . ?
C22 C23 1.454(4) . ?
C18 C19 1.541(3) . ?
C11 C12 1.535(3) . ?
C10 C9 1.525(4) . ?
C1 C2 1.504(4) . ?
C5 C4 1.516(4) . ?
C6 C7 1.506(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O13 Cl1 O14 110.56(16) . . ?
O13 Cl1 O12 110.24(17) . . ?
O14 Cl1 O12 109.82(14) . . ?
O13 Cl1 O11 108.88(18) . . ?
O14 Cl1 O11 109.49(15) . . ?
O12 Cl1 O11 107.80(14) . . ?
C3 N2 C4 112.7(2) . . ?
C3 N2 C2 109.7(2) . . ?
C4 N2 C2 111.5(2) . . ?
O22 Cl2 O22 109.4(5) 2_656 . ?
O22 Cl2 O21 110.1(3) 2_656 . ?
O22 Cl2 O21 108.5(2) . . ?
O22 Cl2 O21 108.5(2) 2_656 2_656 ?
O22 Cl2 O21 110.1(3) . 2_656 ?
O21 Cl2 O21 110.2(4) . 2_656 ?
C17 N9 C13 117.8(2) . . ?
C1 N1 C18 111.5(2) . . ?
C1 N1 C10 112.1(2) . . ?
C18 N1 C10 110.0(2) . . ?
C13 N5 C12 122.0(2) . . ?
C20 N10 C19 121.8(2) . . ?
C20 N11 C22 121.1(2) . . ?
C20 N11 C21 120.1(2) . . ?
C22 N11 C21 118.7(2) . . ?
C20 N14 C24 118.1(2) . . ?
C13 N6 C15 120.2(2) . . ?
C13 N6 C14 120.6(2) . . ?
C15 N6 C14 118.7(2) . . ?
C8 N4 C9 111.0(2) . . ?
C8 N4 C7 108.6(2) . . ?
C9 N4 C7 111.5(2) . . ?
C11 N3 C6 112.9(2) . . ?
C11 N3 C5 111.3(2) . . ?
C6 N3 C5 111.0(2) . . ?
O4 N12 C23 118.1(2) . . ?
O2 N7 C16 117.2(2) . . ?
N8 C17 N9 117.6(2) . . ?
N8 C17 C16 119.9(2) . . ?
N9 C17 C16 122.5(2) . . ?
N10 C20 N14 118.4(2) . . ?
N10 C20 N11 117.2(2) . . ?
N14 C20 N11 124.3(2) . . ?
N13 C24 N14 118.0(2) . . ?
N13 C24 C23 120.0(2) . . ?
N14 C24 C23 122.0(2) . . ?
N5 C13 N9 117.8(2) . . ?
N5 C13 N6 117.1(2) . . ?
N9 C13 N6 125.1(2) . . ?
N7 C16 C17 127.7(3) . . ?
N7 C16 C15 113.8(3) . . ?
C17 C16 C15 118.4(2) . . ?
O3 C22 N11 120.5(3) . . ?
O3 C22 C23 124.5(3) . . ?
N11 C22 C23 114.9(2) . . ?
N1 C18 C19 113.9(2) . . ?
N12 C23 C24 127.1(3) . . ?
N12 C23 C22 114.0(2) . . ?
C24 C23 C22 118.9(2) . . ?
N3 C11 C12 113.5(2) . . ?
N10 C19 C18 111.6(2) . . ?
N1 C10 C9 111.8(2) . . ?
N5 C12 C11 111.4(2) . . ?
N1 C1 C2 111.3(2) . . ?
O1 C15 N6 120.2(3) . . ?
O1 C15 C16 124.4(3) . . ?
N6 C15 C16 115.4(2) . . ?
N4 C9 C10 112.1(2) . . ?
N3 C5 C4 110.1(2) . . ?
N3 C6 C7 114.0(3) . . ?
N2 C4 C5 110.3(2) . . ?
C1 C2 N2 112.2(2) . . ?
C6 C7 N4 114.8(2) . . ?

_refine_diff_density_max         1.821
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.103


# start Validation Reply Form
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact Ow3 ..Ow3 . 2.30 Ang.
RESPONSE: This is not a real intermolecular contact. The Ow3 water molecule is disordered and spread over two symmetry related position. It has been introduced in the calculation with 0.5 o.f. 

PROBLEM: Short Inter D...A Contact Ow1 ..Ow2 . 2.74 Ang.
RESPONSE: This distance correspond to a hydrogen bond contact. All attempts carried out to localize and refine the hydrogen atoms for these water molecules were unsuccesful
;
_vrf_PLAT097_shelx               
;
PROBLEM: Large Reported Max. (Positive) Residual Density 1.82 eA-3
RESPONSE: The signalled residual density is located near a water oxygen atom and can possibly be a hydrogen atom. Nevertheless, all attempts carried out to localize and refine the hydrogen atoms for this water molecule were unsuccesful
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow1 Check
RESPONSE: all attempts carried out to localize and refine the hydrogen atoms for this water molecule were unsuccesful
;

# end Validation Reply Form

#===END
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2309460'
loop_
_audit_author_name
_audit_author_address
'Carla Bazzicalupi'
;University of Firenze
Italy
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2023-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H96 Cl4 N12 O16 Pd2 S4'
_chemical_formula_weight         1676.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.8464(3)
_cell_length_b                   18.5362(7)
_cell_length_c                   21.2826(8)
_cell_angle_alpha                97.607(2)
_cell_angle_beta                 99.894(2)
_cell_angle_gamma                100.807(2)
_cell_volume                     3704.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9980
_cell_measurement_theta_min      3.53
_cell_measurement_theta_max      64.28

_exptl_crystal_description       prismatic
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_F_000             1736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    6.872
_shelx_estimated_absorpt_T_min   0.547
_shelx_estimated_absorpt_T_max   0.609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5695
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46600
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_av_R_equivalents  0.0946
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.462
_diffrn_reflns_theta_max         58.930
_diffrn_reflns_theta_full        58.930
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measured_fraction_theta_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.968
_reflns_number_total             10301
_reflns_number_gt                6687
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_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)+(0.1375P)²+28.9133P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10301
_refine_ls_number_parameters     867
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1327
_refine_ls_R_factor_gt           0.0874
_refine_ls_wR_factor_ref         0.2643
_refine_ls_wR_factor_gt          0.2264
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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
Pd1 Pd 0.18385(9) 0.55476(5) 0.31931(4) 0.0424(3) Uani 1 1 d . . . . .
OW2 O -0.2946(9) 0.5329(6) 0.4044(5) 0.073(3) Uani 1 1 d . . . . .
S3 S 0.8754(3) 0.06730(16) 0.15642(16) 0.0475(8) Uani 1 1 d . . . . .
Pd2 Pd 0.75361(9) 0.06267(5) 0.32559(4) 0.0448(3) Uani 1 1 d . . . . .
OW6 O -0.3442(10) 0.8452(6) 0.5080(5) 0.089(3) Uani 1 1 d . . . . .
S1 S 0.1024(3) 0.82818(16) 0.19635(16) 0.0500(8) Uani 1 1 d . . . . .
OW4 O -0.3454(11) 0.7156(6) 0.5828(5) 0.089(3) Uani 1 1 d . . . . .
Cl2 Cl -0.2167(3) 0.78096(16) 0.72790(17) 0.0556(8) Uani 1 1 d . . . . .
OW8 O -0.6241(14) 0.8317(7) 0.4279(7) 0.116(4) Uani 1 1 d . . . . .
OW5 O -0.1856(13) 0.7672(7) 0.4301(6) 0.109(4) Uani 1 1 d . . . . .
S4 S 0.5967(3) 0.28393(16) 0.19723(17) 0.0513(8) Uani 1 1 d . . . . .
S2 S 0.3423(4) 0.5246(2) 0.14198(19) 0.0630(10) Uani 1 1 d . . . . .
Cl4 Cl -0.5470(4) 0.72304(19) 0.2592(2) 0.0747(10) Uani 1 1 d . . . . .
Cl3 Cl -0.2671(5) 1.0209(3) 0.5316(2) 0.1008(14) Uani 1 1 d . . . . .
Cl1 Cl -0.0500(6) 0.4298(3) 0.4451(3) 0.1081(15) Uani 1 1 d . . . . .
O6 O 0.7688(8) 0.0012(4) 0.1449(4) 0.049(2) Uani 1 1 d . . . . .
OW1 O -0.3433(7) 0.3678(4) 0.3968(3) 0.0380(18) Uani 1 1 d . . . . .
O5 O 0.8389(8) 0.1363(4) 0.1442(4) 0.053(2) Uani 1 1 d . . . . .
O7 O 0.7436(8) 0.2809(5) 0.2092(4) 0.058(2) Uani 1 1 d . . . . .
O1 O 0.2037(9) 0.8971(4) 0.2070(4) 0.060(2) Uani 1 1 d . . . . .
O8 O 0.5529(9) 0.3515(4) 0.2175(4) 0.059(2) Uani 1 1 d . . . . .
N11 N 0.9490(11) 0.0820(5) 0.2327(5) 0.045(3) Uani 1 1 d . . . . .
O4 O 0.2782(9) 0.4459(5) 0.1261(5) 0.069(3) Uani 1 1 d . . . . .
O2 O -0.0403(9) 0.8302(5) 0.2017(4) 0.063(2) Uani 1 1 d . . . . .
N2 N 0.0149(10) 0.4865(5) 0.2562(5) 0.046(2) Uani 1 1 d . . . . .
OW3 O -0.1811(9) 0.6510(5) 0.5082(4) 0.063(2) Uani 1 1 d . . . . .
N7 N 0.9334(10) 0.0278(5) 0.3594(5) 0.050(3) Uani 1 1 d . . . . .
N12 N 0.5194(11) 0.2193(5) 0.2334(5) 0.048(3) Uani 1 1 d . . . . .
N8 N 0.8466(11) 0.1655(6) 0.3781(5) 0.051(3) Uani 1 1 d . . . . .
N3 N 0.2740(10) 0.4634(5) 0.3249(5) 0.045(2) Uani 1 1 d . . . . .
N10 N 0.6488(10) -0.0474(5) 0.3075(5) 0.051(3) Uani 1 1 d . . . . .
N1 N 0.0532(10) 0.6259(5) 0.3362(5) 0.050(3) Uani 1 1 d . . . . .
O3 O 0.2677(10) 0.5757(6) 0.1139(6) 0.085(3) Uani 1 1 d . . . . .
N6 N 0.3770(11) 0.5498(5) 0.2192(6) 0.061(3) Uani 1 1 d . . . . .
N9 N 0.5635(10) 0.0916(6) 0.3239(5) 0.054(3) Uani 1 1 d . . . . .
N4 N 0.3122(10) 0.6046(5) 0.4060(5) 0.053(3) Uani 1 1 d . . . . .
N5 N 0.1679(11) 0.7810(5) 0.2473(5) 0.052(3) Uani 1 1 d . . . . .
C44 C 1.2259(12) 0.0239(6) 0.0537(6) 0.044(3) Uani 1 1 d . . . . .
C13 C 0.0953(11) 0.7800(5) 0.1177(5) 0.037(3) Uani 1 1 d . . . . .
C50 C 0.5343(12) 0.2579(6) 0.1132(6) 0.043(3) Uani 1 1 d . . . . .
C20 C 0.3615(12) 0.4400(6) 0.2774(6) 0.044(3) Uani 1 1 d . . . . .
H20A H 0.419424 0.406806 0.296067 0.052 Uiso 1 1 calc R U . . .
H20B H 0.297377 0.410951 0.237354 0.052 Uiso 1 1 calc R U . . .
C27 C 0.6599(13) 0.4848(7) 0.0561(6) 0.050(3) Uani 1 1 d . . . . .
H27 H 0.677723 0.443840 0.029396 0.060 Uiso 1 1 calc R U . . .
C3 C -0.0226(12) 0.4965(6) 0.1878(6) 0.046(3) Uani 1 1 d . . . . .
H3A H 0.053000 0.487178 0.165377 0.068 Uiso 1 1 calc R U . . .
H3B H -0.110924 0.461411 0.166501 0.068 Uiso 1 1 calc R U . . .
H3C H -0.034522 0.547654 0.186380 0.068 Uiso 1 1 calc R U . . .
C39 C 1.0614(11) 0.0377(6) 0.3282(6) 0.044(3) Uani 1 1 d . . . . .
H39A H 1.117570 0.089222 0.342839 0.053 Uiso 1 1 calc R U . . .
H39B H 1.121324 0.003223 0.342590 0.053 Uiso 1 1 calc R U . . .
C14 C -0.0113(13) 0.7843(6) 0.0679(6) 0.046(3) Uani 1 1 d . . . . .
H14 H -0.083107 0.809992 0.076016 0.055 Uiso 1 1 calc R U . . .
C25 C 0.7571(12) 0.5509(7) 0.0709(6) 0.048(3) Uani 1 1 d . . . . .
C5 C 0.1428(12) 0.4060(6) 0.3186(6) 0.048(3) Uani 1 1 d . . . . .
H5A H 0.100472 0.415339 0.357094 0.057 Uiso 1 1 calc R U . . .
H5B H 0.165502 0.356044 0.316383 0.057 Uiso 1 1 calc R U . . .
C46 C 1.2190(11) 0.0958(6) 0.0763(6) 0.045(3) Uani 1 1 d . . . . .
H46 H 1.288419 0.136304 0.070885 0.055 Uiso 1 1 calc R U . . .
C21 C 0.4572(12) 0.5040(6) 0.2600(6) 0.049(3) Uani 1 1 d . . . . .
H21A H 0.523794 0.484484 0.235831 0.059 Uiso 1 1 calc R U . . .
H21B H 0.513349 0.536684 0.300233 0.059 Uiso 1 1 calc R U . . .
C43 C 1.1201(13) -0.0342(6) 0.0582(6) 0.048(3) Uani 1 1 d . . . . .
H43 H 1.121843 -0.083548 0.039777 0.057 Uiso 1 1 calc R U . . .
C10 C 0.0722(13) 0.6302(7) 0.4083(6) 0.051(3) Uani 1 1 d . . . . .
H10A H 0.031315 0.581115 0.418387 0.061 Uiso 1 1 calc R U . . .
H10B H 0.022011 0.667184 0.426059 0.061 Uiso 1 1 calc R U . . .
C53 C 0.4410(12) 0.2209(6) -0.0204(6) 0.048(3) Uani 1 1 d . . . . .
C55 C 0.5440(13) 0.1912(6) 0.0107(6) 0.050(3) Uani 1 1 d . . . . .
H55 H 0.583633 0.156691 -0.013502 0.059 Uiso 1 1 calc R U . . .
C48 C 0.4709(12) 0.0939(7) 0.2608(7) 0.055(3) Uani 1 1 d . . . . .
H48A H 0.439771 0.042506 0.236178 0.066 Uiso 1 1 calc R U . . .
H48B H 0.385517 0.110532 0.270243 0.066 Uiso 1 1 calc R U . . .
C47 C 1.1119(13) 0.1091(6) 0.1069(6) 0.046(3) Uani 1 1 d . . . . .
H47 H 1.110474 0.158607 0.124825 0.055 Uiso 1 1 calc R U . . .
C11 C 0.0868(15) 0.7033(7) 0.3215(7) 0.059(4) Uani 1 1 d . . . . .
H11A H 0.179774 0.729638 0.348252 0.071 Uiso 1 1 calc R U . . .
H11B H 0.015234 0.730327 0.334033 0.071 Uiso 1 1 calc R U . . .
C51 C 0.4244(13) 0.2885(6) 0.0824(7) 0.052(3) Uani 1 1 d . . . . .
H51 H 0.380900 0.320339 0.107241 0.062 Uiso 1 1 calc R U . . .
C19 C 0.1997(14) 0.7439(7) 0.1070(6) 0.053(3) Uani 1 1 d . . . . .
H19 H 0.272622 0.741431 0.141703 0.064 Uiso 1 1 calc R U . . .
C9 C 0.2294(13) 0.6529(7) 0.4396(6) 0.056(3) Uani 1 1 d . . . . .
H9A H 0.265677 0.705763 0.437064 0.067 Uiso 1 1 calc R U . . .
H9B H 0.242159 0.647940 0.485919 0.067 Uiso 1 1 calc R U . . .
C31 C 0.8846(14) 0.2311(6) 0.3452(6) 0.054(3) Uani 1 1 d . . . . .
H31A H 0.799841 0.238024 0.317070 0.081 Uiso 1 1 calc R U . . .
H31B H 0.924038 0.276042 0.377941 0.081 Uiso 1 1 calc R U . . .
H31C H 0.954725 0.222202 0.319233 0.081 Uiso 1 1 calc R U . . .
C29 C 0.9695(13) 0.0744(6) 0.4271(6) 0.051(3) Uani 1 1 d . . . . .
H29A H 0.896740 0.057434 0.451834 0.061 Uiso 1 1 calc R U . . .
H29B H 1.061751 0.068553 0.450423 0.061 Uiso 1 1 calc R U . . .
C40 C 1.0209(12) 0.0227(6) 0.2554(6) 0.043(3) Uani 1 1 d . . . . .
H40A H 0.956643 -0.026817 0.240521 0.052 Uiso 1 1 calc R U . . .
H40B H 1.106428 0.022589 0.236782 0.052 Uiso 1 1 calc R U . . .
C41 C 1.0058(11) 0.0503(6) 0.1118(6) 0.041(3) Uani 1 1 d . . . . .
C12 C 0.0903(14) 0.7055(7) 0.2506(6) 0.053(3) Uani 1 1 d . . . . .
H12A H 0.138797 0.667336 0.233506 0.063 Uiso 1 1 calc R U . . .
H12B H -0.006889 0.695664 0.224649 0.063 Uiso 1 1 calc R U . . .
C23 C 0.6053(13) 0.6025(7) 0.1336(6) 0.048(3) Uani 1 1 d . . . . .
H23 H 0.587432 0.642702 0.161308 0.058 Uiso 1 1 calc R U . . .
C18 C 0.1973(13) 0.7108(7) 0.0443(7) 0.057(4) Uani 1 1 d . . . . .
H18 H 0.268689 0.684642 0.036611 0.068 Uiso 1 1 calc R U . . .
C35 C 0.5005(13) -0.0462(7) 0.3189(7) 0.057(3) Uani 1 1 d . . . . .
H35A H 0.471541 -0.085271 0.344377 0.068 Uiso 1 1 calc R U . . .
H35B H 0.433245 -0.057194 0.276779 0.068 Uiso 1 1 calc R U . . .
C15 C -0.0114(14) 0.7507(7) 0.0059(7) 0.057(4) Uani 1 1 d . . . . .
H15 H -0.086362 0.752264 -0.028195 0.068 Uiso 1 1 calc R U . . .
C56 C 0.5924(12) 0.2101(6) 0.0769(6) 0.045(3) Uani 1 1 d . . . . .
H56 H 0.666512 0.189731 0.097383 0.054 Uiso 1 1 calc R U . . .
C49 C 0.5346(12) 0.1427(6) 0.2186(6) 0.050(3) Uani 1 1 d . . . . .
H49A H 0.636203 0.142154 0.223764 0.060 Uiso 1 1 calc R U . . .
H49B H 0.489178 0.122351 0.172906 0.060 Uiso 1 1 calc R U . . .
C7 C 0.3155(12) 0.5360(7) 0.4362(6) 0.048(3) Uani 1 1 d . . . . .
H7A H 0.220496 0.515331 0.443716 0.057 Uiso 1 1 calc R U . . .
H7B H 0.382127 0.549068 0.478548 0.057 Uiso 1 1 calc R U . . .
C4 C 0.0383(12) 0.4083(6) 0.2581(7) 0.050(3) Uani 1 1 d . . . . .
H4A H 0.074340 0.390970 0.219407 0.060 Uiso 1 1 calc R U . . .
H4B H -0.052746 0.374180 0.257014 0.060 Uiso 1 1 calc R U . . .
C52 C 0.3811(12) 0.2717(6) 0.0159(7) 0.048(3) Uani 1 1 d . . . . .
H52 H 0.311270 0.294181 -0.005400 0.057 Uiso 1 1 calc R U . . .
C2 C -0.0988(13) 0.5005(6) 0.2913(7) 0.053(3) Uani 1 1 d . . . . .
H2A H -0.085010 0.482139 0.333055 0.064 Uiso 1 1 calc R U . . .
H2B H -0.191979 0.473579 0.265185 0.064 Uiso 1 1 calc R U . . .
C6 C 0.3611(13) 0.4786(7) 0.3922(6) 0.050(3) Uani 1 1 d . . . . .
H6A H 0.461521 0.496386 0.390657 0.060 Uiso 1 1 calc R U . . .
H6B H 0.352555 0.431656 0.410092 0.060 Uiso 1 1 calc R U . . .
C22 C 0.5072(13) 0.5367(6) 0.1170(6) 0.047(3) Uani 1 1 d . . . . .
C16 C 0.0928(13) 0.7150(7) -0.0081(7) 0.054(3) Uani 1 1 d . . . . .
C24 C 0.7280(13) 0.6118(7) 0.1112(6) 0.055(3) Uani 1 1 d . . . . .
H24 H 0.793553 0.658329 0.122239 0.066 Uiso 1 1 calc R U . . .
C42 C 1.0117(13) -0.0224(6) 0.0888(6) 0.049(3) Uani 1 1 d . . . . .
H42 H 0.942505 -0.063178 0.094044 0.058 Uiso 1 1 calc R U . . .
C1 C -0.0941(12) 0.5851(6) 0.3036(7) 0.052(3) Uani 1 1 d . . . . .
H1A H -0.121756 0.602138 0.262012 0.062 Uiso 1 1 calc R U . . .
H1B H -0.161268 0.595722 0.331437 0.062 Uiso 1 1 calc R U . . .
C30 C 0.9758(14) 0.1549(7) 0.4211(6) 0.057(3) Uani 1 1 d . . . . .
H30A H 0.986479 0.184453 0.464674 0.068 Uiso 1 1 calc R U . . .
H30B H 1.059787 0.173879 0.403513 0.068 Uiso 1 1 calc R U . . .
C8 C 0.4549(13) 0.6486(7) 0.4113(6) 0.055(3) Uani 1 1 d . . . . .
H8A H 0.449596 0.692903 0.391232 0.083 Uiso 1 1 calc R U . . .
H8B H 0.500800 0.663936 0.457024 0.083 Uiso 1 1 calc R U . . .
H8C H 0.509810 0.618387 0.389072 0.083 Uiso 1 1 calc R U . . .
C17 C 0.0868(14) 0.6783(8) -0.0769(6) 0.059(4) Uani 1 1 d . . . . .
H17A H -0.002227 0.641488 -0.092445 0.089 Uiso 1 1 calc R U . . .
H17B H 0.166149 0.653481 -0.077791 0.089 Uiso 1 1 calc R U . . .
H17C H 0.092660 0.716306 -0.104824 0.089 Uiso 1 1 calc R U . . .
C28 C 0.5357(13) 0.4765(7) 0.0794(7) 0.054(3) Uani 1 1 d . . . . .
H28 H 0.470463 0.429840 0.069616 0.065 Uiso 1 1 calc R U . . .
C38 C 0.8868(13) -0.0534(7) 0.3629(7) 0.054(3) Uani 1 1 d . . . . .
H38A H 0.940682 -0.064558 0.402892 0.065 Uiso 1 1 calc R U . . .
H38B H 0.907402 -0.084156 0.325457 0.065 Uiso 1 1 calc R U . . .
C37 C 0.7286(13) -0.0737(7) 0.3628(7) 0.057(3) Uani 1 1 d . . . . .
H37A H 0.697499 -0.128370 0.358711 0.069 Uiso 1 1 calc R U . . .
H37B H 0.709902 -0.050053 0.403990 0.069 Uiso 1 1 calc R U . . .
C36 C 0.6391(13) -0.0931(7) 0.2435(6) 0.056(3) Uani 1 1 d . . . . .
H36A H 0.585361 -0.072584 0.209630 0.084 Uiso 1 1 calc R U . . .
H36B H 0.734236 -0.092367 0.235296 0.084 Uiso 1 1 calc R U . . .
H36C H 0.591224 -0.144534 0.243243 0.084 Uiso 1 1 calc R U . . .
C34 C 0.4955(15) 0.0297(7) 0.3551(7) 0.061(4) Uani 1 1 d . . . . .
H34A H 0.396021 0.032580 0.354996 0.073 Uiso 1 1 calc R U . . .
H34B H 0.545313 0.035850 0.400631 0.073 Uiso 1 1 calc R U . . .
C54 C 0.3912(14) 0.2012(7) -0.0927(6) 0.059(4) Uani 1 1 d . . . . .
H54A H 0.472972 0.206702 -0.113556 0.088 Uiso 1 1 calc R U . . .
H54B H 0.330629 0.234437 -0.107419 0.088 Uiso 1 1 calc R U . . .
H54C H 0.337686 0.149447 -0.104048 0.088 Uiso 1 1 calc R U . . .
C45 C 1.3441(13) 0.0084(7) 0.0204(7) 0.055(3) Uani 1 1 d . . . . .
H45A H 1.357257 0.042050 -0.010911 0.082 Uiso 1 1 calc R U . . .
H45B H 1.319893 -0.043385 -0.002164 0.082 Uiso 1 1 calc R U . . .
H45C H 1.431641 0.016329 0.052763 0.082 Uiso 1 1 calc R U . . .
C33 C 0.5935(14) 0.1648(7) 0.3704(7) 0.058(3) Uani 1 1 d . . . . .
H33A H 0.517340 0.164771 0.395337 0.070 Uiso 1 1 calc R U . . .
H33B H 0.594354 0.206399 0.345551 0.070 Uiso 1 1 calc R U . . .
C26 C 0.8933(14) 0.5609(9) 0.0447(7) 0.070(4) Uani 1 1 d . . . . .
H26A H 0.926891 0.514241 0.042260 0.105 Uiso 1 1 calc R U . . .
H26B H 0.965297 0.600718 0.073647 0.105 Uiso 1 1 calc R U . . .
H26C H 0.875071 0.574079 0.001423 0.105 Uiso 1 1 calc R U . . .
C32 C 0.7345(13) 0.1769(8) 0.4169(7) 0.063(4) Uani 1 1 d . . . . .
H32A H 0.759117 0.228104 0.442074 0.076 Uiso 1 1 calc R U . . .
H32B H 0.728696 0.141232 0.447524 0.076 Uiso 1 1 calc R U . . .
OW7 O -0.2229(17) 0.7409(8) 0.2888(7) 0.063(6) Uani 0.68(3) 1 d . . P . .
OW7' O -0.326(2) 0.7103(9) 0.2967(10) 0.023(8) Uani 0.32(3) 1 d . . P . .
H2 H 0.997(13) 0.117(7) 0.236(7) 0.050 Uiso 1 1 d . U . . .
H1 H 0.444(13) 0.226(7) 0.230(6) 0.050 Uiso 1 1 d . U . . .


_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
Pd1 N4 2.041(10) . ?
Pd1 N2 2.040(9) . ?
Pd1 N1 2.047(10) . ?
Pd1 N3 2.062(9) . ?
S3 O6 1.418(8) . ?
S3 O5 1.435(8) . ?
S3 N11 1.625(11) . ?
S3 C41 1.773(11) . ?
Pd2 N9 2.037(9) . ?
Pd2 N8 2.037(10) . ?
Pd2 N7 2.045(10) . ?
Pd2 N10 2.060(9) . ?
S1 O1 1.430(9) . ?
S1 O2 1.437(9) . ?
S1 N5 1.606(11) . ?
S1 C13 1.774(11) . ?
S4 O7 1.437(8) . ?
S4 O8 1.437(9) . ?
S4 N12 1.646(11) . ?
S4 C50 1.758(12) . ?
S2 O3 1.432(10) . ?
S2 O4 1.446(10) . ?
S2 N6 1.606(12) . ?
S2 C22 1.779(12) . ?
N11 C40 1.502(15) . ?
N2 C3 1.485(15) . ?
N2 C2 1.491(15) . ?
N2 C4 1.515(14) . ?
N7 C38 1.505(15) . ?
N7 C39 1.515(15) . ?
N7 C29 1.525(15) . ?
N12 C49 1.454(15) . ?
N8 C30 1.495(16) . ?
N8 C31 1.502(15) . ?
N8 C32 1.515(15) . ?
N3 C5 1.486(14) . ?
N3 C6 1.499(15) . ?
N3 C20 1.510(14) . ?
N10 C37 1.489(16) . ?
N10 C36 1.484(16) . ?
N10 C35 1.524(15) . ?
N1 C1 1.503(15) . ?
N1 C11 1.497(15) . ?
N1 C10 1.503(16) . ?
N6 C21 1.520(16) . ?
N9 C48 1.497(16) . ?
N9 C34 1.507(15) . ?
N9 C33 1.519(16) . ?
N4 C8 1.464(15) . ?
N4 C7 1.501(15) . ?
N4 C9 1.510(15) . ?
N5 C12 1.479(15) . ?
C44 C46 1.373(16) . ?
C44 C43 1.378(16) . ?
C44 C45 1.514(16) . ?
C13 C19 1.362(16) . ?
C13 C14 1.380(16) . ?
C50 C56 1.367(16) . ?
C50 C51 1.417(17) . ?
C20 C21 1.499(15) . ?
C27 C25 1.367(17) . ?
C27 C28 1.386(17) . ?
C39 C40 1.508(16) . ?
C14 C15 1.382(17) . ?
C25 C24 1.429(18) . ?
C25 C26 1.528(16) . ?
C5 C4 1.516(17) . ?
C46 C47 1.374(16) . ?
C43 C42 1.379(16) . ?
C10 C9 1.531(17) . ?
C53 C55 1.359(17) . ?
C53 C52 1.415(17) . ?
C53 C54 1.505(17) . ?
C55 C56 1.382(17) . ?
C48 C49 1.488(17) . ?
C47 C41 1.389(16) . ?
C11 C12 1.522(18) . ?
C51 C52 1.380(17) . ?
C19 C18 1.387(18) . ?
C29 C30 1.505(17) . ?
C41 C42 1.387(16) . ?
C23 C24 1.363(17) . ?
C23 C22 1.369(17) . ?
C18 C16 1.403(18) . ?
C35 C34 1.526(18) . ?
C15 C16 1.374(18) . ?
C7 C6 1.507(16) . ?
C2 C1 1.545(16) . ?
C22 C28 1.385(17) . ?
C16 C17 1.515(18) . ?
C38 C37 1.532(17) . ?
C33 C32 1.520(18) . ?
OW7 OW7' 1.12(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Pd1 N2 158.2(4) . . ?
N4 Pd1 N1 88.2(4) . . ?
N2 Pd1 N1 87.3(4) . . ?
N4 Pd1 N3 88.4(4) . . ?
N2 Pd1 N3 88.0(4) . . ?
N1 Pd1 N3 158.5(4) . . ?
O6 S3 O5 120.0(5) . . ?
O6 S3 N11 107.1(5) . . ?
O5 S3 N11 105.5(5) . . ?
O6 S3 C41 108.0(5) . . ?
O5 S3 C41 108.3(5) . . ?
N11 S3 C41 107.4(5) . . ?
N9 Pd2 N8 88.1(4) . . ?
N9 Pd2 N7 159.5(4) . . ?
N8 Pd2 N7 88.2(4) . . ?
N9 Pd2 N10 88.3(4) . . ?
N8 Pd2 N10 157.9(4) . . ?
N7 Pd2 N10 87.7(4) . . ?
O1 S1 O2 118.6(5) . . ?
O1 S1 N5 104.8(5) . . ?
O2 S1 N5 110.1(6) . . ?
O1 S1 C13 108.6(5) . . ?
O2 S1 C13 106.9(5) . . ?
N5 S1 C13 107.4(5) . . ?
O7 S4 O8 120.7(5) . . ?
O7 S4 N12 105.5(5) . . ?
O8 S4 N12 107.3(5) . . ?
O7 S4 C50 106.5(5) . . ?
O8 S4 C50 107.7(6) . . ?
N12 S4 C50 108.6(5) . . ?
O3 S2 O4 118.4(6) . . ?
O3 S2 N6 108.1(6) . . ?
O4 S2 N6 109.2(6) . . ?
O3 S2 C22 106.8(6) . . ?
O4 S2 C22 107.1(6) . . ?
N6 S2 C22 106.6(6) . . ?
C40 N11 S3 116.0(7) . . ?
C3 N2 C2 110.4(9) . . ?
C3 N2 C4 109.2(9) . . ?
C2 N2 C4 110.8(9) . . ?
C3 N2 Pd1 121.7(7) . . ?
C2 N2 Pd1 99.0(7) . . ?
C4 N2 Pd1 105.3(7) . . ?
C38 N7 C39 108.8(9) . . ?
C38 N7 C29 110.3(10) . . ?
C39 N7 C29 110.1(9) . . ?
C38 N7 Pd2 105.9(7) . . ?
C39 N7 Pd2 123.3(7) . . ?
C29 N7 Pd2 97.8(7) . . ?
C49 N12 S4 120.3(8) . . ?
C30 N8 C31 109.5(10) . . ?
C30 N8 C32 110.5(10) . . ?
C31 N8 C32 110.4(9) . . ?
C30 N8 Pd2 105.3(7) . . ?
C31 N8 Pd2 120.9(8) . . ?
C32 N8 Pd2 99.6(8) . . ?
C5 N3 C6 111.5(9) . . ?
C5 N3 C20 111.0(9) . . ?
C6 N3 C20 109.4(9) . . ?
C5 N3 Pd1 98.2(6) . . ?
C6 N3 Pd1 104.3(7) . . ?
C20 N3 Pd1 121.8(7) . . ?
C37 N10 C36 114.1(10) . . ?
C37 N10 C35 108.9(10) . . ?
C36 N10 C35 109.3(9) . . ?
C37 N10 Pd2 99.2(7) . . ?
C36 N10 Pd2 119.2(8) . . ?
C35 N10 Pd2 105.3(7) . . ?
C1 N1 C11 112.1(10) . . ?
C1 N1 C10 110.3(9) . . ?
C11 N1 C10 108.7(9) . . ?
C1 N1 Pd1 106.8(7) . . ?
C11 N1 Pd1 119.6(8) . . ?
C10 N1 Pd1 98.3(7) . . ?
C21 N6 S2 117.9(8) . . ?
C48 N9 C34 110.1(10) . . ?
C48 N9 C33 111.9(10) . . ?
C34 N9 C33 109.1(10) . . ?
C48 N9 Pd2 120.4(8) . . ?
C34 N9 Pd2 98.2(7) . . ?
C33 N9 Pd2 105.8(7) . . ?
C8 N4 C7 111.2(10) . . ?
C8 N4 C9 108.3(9) . . ?
C7 N4 C9 110.0(10) . . ?
C8 N4 Pd1 122.7(8) . . ?
C7 N4 Pd1 98.1(7) . . ?
C9 N4 Pd1 105.9(7) . . ?
C12 N5 S1 120.2(8) . . ?
C46 C44 C43 119.5(11) . . ?
C46 C44 C45 120.7(10) . . ?
C43 C44 C45 119.7(10) . . ?
C19 C13 C14 121.6(11) . . ?
C19 C13 S1 119.5(9) . . ?
C14 C13 S1 118.8(9) . . ?
C56 C50 C51 119.5(12) . . ?
C56 C50 S4 121.1(10) . . ?
C51 C50 S4 119.4(9) . . ?
C21 C20 N3 113.8(9) . . ?
C25 C27 C28 121.3(11) . . ?
C40 C39 N7 112.1(9) . . ?
C13 C14 C15 118.7(12) . . ?
C27 C25 C24 118.4(11) . . ?
C27 C25 C26 121.7(12) . . ?
C24 C25 C26 120.0(11) . . ?
N3 C5 C4 110.0(10) . . ?
C44 C46 C47 120.1(11) . . ?
C20 C21 N6 112.6(10) . . ?
C42 C43 C44 121.4(11) . . ?
N1 C10 C9 110.0(10) . . ?
C55 C53 C52 119.2(12) . . ?
C55 C53 C54 120.9(12) . . ?
C52 C53 C54 119.8(11) . . ?
C53 C55 C56 121.4(12) . . ?
C49 C48 N9 116.4(10) . . ?
C46 C47 C41 120.2(11) . . ?
N1 C11 C12 113.4(10) . . ?
C52 C51 C50 119.5(12) . . ?
C13 C19 C18 118.6(12) . . ?
N4 C9 C10 110.7(10) . . ?
C30 C29 N7 108.9(10) . . ?
C39 C40 N11 109.5(9) . . ?
C42 C41 C47 120.1(11) . . ?
C42 C41 S3 119.7(9) . . ?
C47 C41 S3 119.8(9) . . ?
N5 C12 C11 106.9(10) . . ?
C24 C23 C22 121.5(12) . . ?
C19 C18 C16 122.0(13) . . ?
N10 C35 C34 110.7(10) . . ?
C16 C15 C14 122.5(12) . . ?
C50 C56 C55 120.5(12) . . ?
N12 C49 C48 112.9(11) . . ?
N4 C7 C6 109.8(10) . . ?
N2 C4 C5 110.9(10) . . ?
C51 C52 C53 119.8(12) . . ?
N2 C2 C1 109.2(9) . . ?
N3 C6 C7 112.0(10) . . ?
C23 C22 C28 119.7(11) . . ?
C23 C22 S2 122.4(9) . . ?
C28 C22 S2 117.9(9) . . ?
C15 C16 C18 116.7(13) . . ?
C15 C16 C17 120.3(13) . . ?
C18 C16 C17 122.9(12) . . ?
C23 C24 C25 119.5(11) . . ?
C43 C42 C41 118.5(11) . . ?
N1 C1 C2 109.1(9) . . ?
N8 C30 C29 112.2(10) . . ?
C22 C28 C27 119.6(11) . . ?
N7 C38 C37 111.1(10) . . ?
N10 C37 C38 109.4(10) . . ?
N9 C34 C35 110.7(10) . . ?
N9 C33 C32 111.2(11) . . ?
N8 C32 C33 108.7(11) . . ?

_refine_diff_density_max         3.825
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.155


# start Validation Reply Form
_vrf_THETM01_shelx               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: Due to too low intensity, data collection has been carried out only up to theta=58.930 deg
;
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens. 2.22Ang From Cl3 3.64 eA-3
RESPONSE: This peak is too close to the chloride ion. It most likely is due to series' truncation errors
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow2 Check
RESPONSE: The water hydrogens have not been localized in the Fourier density map
;
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact Ow2 ..Ow3 . 2.81 Ang.
RESPONSE: This distance correspond to a hydrogen bond contact. All attempts carried out to localize and refine the hydrogen atoms for these water molecules were unsuccesful
;
_vrf_PLAT973_shelx               
;
PROBLEM: Check Calcd Positive Resid. Density on Pd2 1.62 eA-3
RESPONSE: This peak is due to series' truncation errors
;
# end Validation Reply Form

#===END
####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2309462'
loop_
_audit_author_name
_audit_author_address
'Carla Bazzicalupi'
;University of Firenze
Italy
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2023-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H48 Cl2 Cu N14 O7'
_chemical_formula_weight         779.20

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

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

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

_cell_length_a                   10.7356(14)
_cell_length_b                   13.2246(16)
_cell_length_c                   13.6742(16)
_cell_angle_alpha                62.602(4)
_cell_angle_beta                 75.161(5)
_cell_angle_gamma                80.721(5)
_cell_volume                     1664.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9920
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      30.49

_exptl_crystal_description       prismatic
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_F_000             818
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.883
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5720
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54357
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_av_R_equivalents  0.0913
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.324
_diffrn_reflns_theta_max         30.593
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10201
_reflns_number_gt                7812
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_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)+(0.0819P)²+7.7826P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10201
_refine_ls_number_parameters     460
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0757
_refine_ls_wR_factor_ref         0.2069
_refine_ls_wR_factor_gt          0.1867
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.002
_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
Cu Cu 0.19618(4) 0.26073(3) 0.53669(3) 0.01397(11) Uani 1 1 d . . . . .
Cl1 Cl -0.00039(8) 0.29787(8) 0.65074(7) 0.02007(18) Uani 1 1 d . . . . .
Cl2 Cl 0.76663(10) 0.24718(10) 0.39756(9) 0.0302(2) Uani 1 1 d . . . . .
O1 O 0.0814(3) 0.2329(3) -0.0438(3) 0.0263(6) Uani 1 1 d . . . . .
OW3 O 0.5370(3) 0.2181(3) 1.3056(3) 0.0299(6) Uani 1 1 d D . . . .
OW2 O 0.7338(3) 0.2432(3) 0.6338(3) 0.0317(7) Uani 1 1 d D . . . .
O3 O 0.3633(3) 0.1436(3) 1.2067(3) 0.0315(7) Uani 1 1 d . . . . .
O2 O 0.3798(3) 0.4314(3) -0.2309(3) 0.0294(6) Uani 1 1 d . . . . .
N10 N 0.2986(3) 0.0239(3) 0.9588(3) 0.0191(6) Uani 1 1 d . . . . .
N14 N 0.4609(3) 0.1443(3) 0.8986(3) 0.0191(6) Uani 1 1 d . . . . .
O4 O 0.6490(3) 0.3373(3) 0.9814(3) 0.0347(7) Uani 1 1 d . . . . .
N9 N 0.1618(3) 0.4571(3) 0.0559(3) 0.0206(6) Uani 1 1 d . . . . .
N11 N 0.3258(3) 0.0904(3) 1.0814(3) 0.0189(6) Uani 1 1 d . . . . .
N6 N 0.0324(3) 0.3159(3) 0.0759(3) 0.0211(6) Uani 1 1 d . . . . .
N1 N 0.3080(3) 0.1443(3) 0.6479(3) 0.0274(7) Uani 1 1 d . . . . .
N7 N 0.2828(3) 0.3696(3) -0.1744(3) 0.0233(6) Uani 1 1 d . . . . .
N5 N -0.0131(3) 0.3999(3) 0.1984(3) 0.0216(6) Uani 1 1 d . . . . .
OW1 O -0.0822(4) 0.1172(4) -0.0875(3) 0.0425(9) Uani 1 1 d D . . . .
N8 N 0.3389(3) 0.5174(3) -0.0852(3) 0.0248(7) Uani 1 1 d . . . . .
H8A H 0.350920 0.563020 -0.058050 0.030 Uiso 1 1 calc R U . . .
H8B H 0.392651 0.516148 -0.145234 0.030 Uiso 1 1 calc R U . . .
N12 N 0.5568(4) 0.2758(3) 1.0540(3) 0.0271(7) Uani 1 1 d . . . . .
N3 N 0.1739(4) 0.3616(3) 0.3725(3) 0.0302(8) Uani 1 1 d . U . . .
N13 N 0.6242(3) 0.2640(3) 0.8379(3) 0.0264(7) Uani 1 1 d . . . . .
H13A H 0.643151 0.258331 0.773970 0.032 Uiso 1 1 calc R U . . .
H13B H 0.669648 0.306704 0.848162 0.032 Uiso 1 1 calc R U . . .
N2 N 0.1615(3) 0.1248(3) 0.5165(3) 0.0292(8) Uani 1 1 d . . . . .
N4 N 0.3183(4) 0.3783(3) 0.5081(4) 0.0332(9) Uani 1 1 d . . . . .
C13 C 0.0617(4) 0.3921(3) 0.1087(3) 0.0195(7) Uani 1 1 d . . . . .
C20 C 0.3635(4) 0.0884(3) 0.9782(3) 0.0169(6) Uani 1 1 d . . . . .
C17 C 0.2397(4) 0.4503(3) -0.0355(3) 0.0200(7) Uani 1 1 d . . . . .
C11 C 0.0398(4) 0.4094(3) 0.3627(3) 0.0197(7) Uani 1 1 d . . . . .
H11A H 0.017631 0.461480 0.399034 0.024 Uiso 1 1 calc R U . . .
H11B H -0.019013 0.345735 0.406336 0.024 Uiso 1 1 calc R U . . .
C18 C 0.2572(4) 0.1231(3) 0.7663(3) 0.0186(6) Uani 1 1 d . . . . .
H18A H 0.164491 0.107686 0.786643 0.022 Uiso 1 1 calc R U . . .
H18B H 0.264331 0.192743 0.773921 0.022 Uiso 1 1 calc R U . . .
C24 C 0.5274(4) 0.2084(3) 0.9184(3) 0.0193(7) Uani 1 1 d . . . . .
C8 C 0.2603(4) 0.4690(3) 0.5410(3) 0.0228(7) Uani 1 1 d . . . . .
H8C H 0.223273 0.435445 0.621984 0.034 Uiso 1 1 calc R U . . .
H8D H 0.326650 0.521110 0.523734 0.034 Uiso 1 1 calc R U . . .
H8E H 0.192192 0.511168 0.499308 0.034 Uiso 1 1 calc R U . . .
C16 C 0.2166(4) 0.3757(3) -0.0782(3) 0.0198(7) Uani 1 1 d . . . . .
C12 C 0.0119(4) 0.4744(3) 0.2437(3) 0.0210(7) Uani 1 1 d . . . . .
H12A H -0.063975 0.527707 0.245102 0.025 Uiso 1 1 calc R U . . .
H12B H 0.086563 0.520422 0.192556 0.025 Uiso 1 1 calc R U . . .
C15 C 0.1094(4) 0.3035(3) -0.0183(3) 0.0212(7) Uani 1 1 d . . . . .
C3 C 0.0449(4) 0.0627(3) 0.5893(3) 0.0224(7) Uani 1 1 d . . . . .
H3A H -0.031410 0.115103 0.576837 0.034 Uiso 1 1 calc R U . . .
H3B H 0.037365 0.000630 0.571176 0.034 Uiso 1 1 calc R U . . .
H3C H 0.051186 0.030927 0.668414 0.034 Uiso 1 1 calc R U . . .
C22 C 0.3930(4) 0.1502(3) 1.1114(3) 0.0216(7) Uani 1 1 d . . . . .
C23 C 0.4970(4) 0.2160(3) 1.0233(3) 0.0206(7) Uani 1 1 d . . . . .
C19 C 0.3281(4) 0.0224(3) 0.8492(3) 0.0228(7) Uani 1 1 d . . . . .
H19A H 0.301788 -0.050141 0.857894 0.027 Uiso 1 1 calc R U . . .
H19B H 0.422287 0.026951 0.818808 0.027 Uiso 1 1 calc R U . . .
C21 C 0.2171(4) 0.0239(4) 1.1658(3) 0.0281(8) Uani 1 1 d . . . . .
H21A H 0.203814 0.035259 1.233722 0.042 Uiso 1 1 calc R U . . .
H21B H 0.138685 0.049400 1.134851 0.042 Uiso 1 1 calc R U . . .
H21C H 0.236496 -0.057230 1.184801 0.042 Uiso 1 1 calc R U . . .
C14 C -0.0826(4) 0.2492(4) 0.1364(4) 0.0286(8) Uani 1 1 d . . . . .
H14A H -0.088410 0.199954 0.101994 0.043 Uiso 1 1 calc R U . . .
H14B H -0.076894 0.202173 0.215375 0.043 Uiso 1 1 calc R U . . .
H14C H -0.159608 0.300985 0.132387 0.043 Uiso 1 1 calc R U . . .
C6 C 0.2707(5) 0.4589(4) 0.3267(4) 0.0336(9) Uani 1 1 d . U . . .
H6A H 0.308436 0.480576 0.246021 0.040 Uiso 1 1 calc R U . . .
H6B H 0.223230 0.527014 0.333093 0.040 Uiso 1 1 calc R U . . .
C4 C 0.1468(5) 0.1815(5) 0.3884(4) 0.0374(11) Uani 1 1 d . . . . .
H4A H 0.177280 0.126089 0.356349 0.045 Uiso 1 1 calc R U . . .
H4B H 0.054927 0.202948 0.384301 0.045 Uiso 1 1 calc R U . . .
C1 C 0.3062(5) 0.0308(4) 0.6380(4) 0.0364(10) Uani 1 1 d . . . . .
H1A H 0.390465 -0.011869 0.646515 0.044 Uiso 1 1 calc R U . . .
H1B H 0.238646 -0.017474 0.699184 0.044 Uiso 1 1 calc R U . . .
C2 C 0.2802(5) 0.0560(4) 0.5278(4) 0.0322(9) Uani 1 1 d . . . . .
H2A H 0.351628 0.097734 0.466194 0.039 Uiso 1 1 calc R U . . .
H2B H 0.271838 -0.015675 0.524282 0.039 Uiso 1 1 calc R U . . .
C10 C 0.4341(5) 0.1895(4) 0.6004(4) 0.0329(9) Uani 1 1 d . . . . .
H10A H 0.470283 0.183719 0.528775 0.040 Uiso 1 1 calc R U . . .
H10B H 0.492691 0.145407 0.652974 0.040 Uiso 1 1 calc R U . . .
C7 C 0.3747(5) 0.4220(4) 0.3895(4) 0.0320(9) Uani 1 1 d . U . . .
H7A H 0.431262 0.362007 0.373798 0.038 Uiso 1 1 calc R U . . .
H7B H 0.427716 0.487260 0.366051 0.038 Uiso 1 1 calc R U . . .
C9 C 0.4231(4) 0.3104(5) 0.5797(4) 0.0364(10) Uani 1 1 d . . . . .
H9A H 0.507433 0.345071 0.539195 0.044 Uiso 1 1 calc R U . . .
H9B H 0.399262 0.314910 0.652571 0.044 Uiso 1 1 calc R U . . .
C5 C 0.2235(5) 0.2835(4) 0.3234(4) 0.0325(9) Uani 1 1 d . . . . .
H5A H 0.315599 0.262463 0.326746 0.039 Uiso 1 1 calc R U . . .
H5B H 0.215901 0.319201 0.243538 0.039 Uiso 1 1 calc R U . . .
H1 H 0.232(6) -0.011(5) 0.999(5) 0.036(15) Uiso 1 1 d . . . . .
H5 H 0.745(6) 0.231(6) 0.581(4) 0.046(7) Uiso 1 1 d D . . . .
H2 H -0.074(5) 0.359(4) 0.233(4) 0.014(10) Uiso 1 1 d . . . . .
H4 H -0.041(5) 0.128(5) -0.052(5) 0.046(7) Uiso 1 1 d D . . . .
H6 H 0.805(3) 0.255(6) 0.633(5) 0.046(7) Uiso 1 1 d D . . . .
H8 H 0.604(4) 0.232(5) 1.311(5) 0.046(7) Uiso 1 1 d D . . . .
H7 H 0.543(6) 0.233(6) 1.241(2) 0.046(7) Uiso 1 1 d D . . . .
H3 H -0.077(6) 0.157(5) -0.154(2) 0.046(7) Uiso 1 1 d 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
Cu N4 2.031(4) . ?
Cu N2 2.042(3) . ?
Cu N3 2.072(4) . ?
Cu N1 2.075(3) . ?
Cu Cl1 2.4107(10) . ?
O1 C15 1.235(5) . ?
O3 C22 1.224(5) . ?
O2 N7 1.276(4) . ?
N10 C20 1.333(5) . ?
N10 C19 1.459(5) . ?
N14 C20 1.322(5) . ?
N14 C24 1.344(5) . ?
O4 N12 1.281(5) . ?
N9 C13 1.320(5) . ?
N9 C17 1.346(5) . ?
N11 C20 1.376(4) . ?
N11 C22 1.396(5) . ?
N11 C21 1.474(5) . ?
N6 C13 1.381(5) . ?
N6 C15 1.405(5) . ?
N6 C14 1.464(5) . ?
N1 C10 1.438(6) . ?
N1 C18 1.475(5) . ?
N1 C1 1.571(6) . ?
N7 C16 1.357(5) . ?
N5 C13 1.322(5) . ?
N5 C12 1.470(5) . ?
N8 C17 1.327(5) . ?
N12 C23 1.350(5) . ?
N3 C5 1.442(6) . ?
N3 C11 1.489(5) . ?
N3 C6 1.577(6) . ?
N13 C24 1.322(5) . ?
N2 C2 1.440(6) . ?
N2 C3 1.475(5) . ?
N2 C4 1.598(7) . ?
N4 C7 1.442(6) . ?
N4 C8 1.462(5) . ?
N4 C9 1.569(7) . ?
C17 C16 1.436(5) . ?
C11 C12 1.534(5) . ?
C18 C19 1.537(5) . ?
C24 C23 1.434(5) . ?
C16 C15 1.435(5) . ?
C22 C23 1.454(5) . ?
C6 C7 1.468(7) . ?
C4 C5 1.472(7) . ?
C1 C2 1.478(7) . ?
C10 C9 1.480(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
N4 Cu N2 149.65(14) . . ?
N4 Cu N3 86.15(18) . . ?
N2 Cu N3 87.03(17) . . ?
N4 Cu N1 85.70(17) . . ?
N2 Cu N1 85.22(17) . . ?
N3 Cu N1 149.25(14) . . ?
N4 Cu Cl1 105.08(11) . . ?
N2 Cu Cl1 105.27(10) . . ?
N3 Cu Cl1 104.47(10) . . ?
N1 Cu Cl1 106.27(10) . . ?
C20 N10 C19 120.6(3) . . ?
C20 N14 C24 118.5(3) . . ?
C13 N9 C17 119.0(3) . . ?
C20 N11 C22 121.2(3) . . ?
C20 N11 C21 120.5(3) . . ?
C22 N11 C21 118.2(3) . . ?
C13 N6 C15 120.9(3) . . ?
C13 N6 C14 120.4(3) . . ?
C15 N6 C14 118.6(3) . . ?
C10 N1 C18 114.8(3) . . ?
C10 N1 C1 110.7(3) . . ?
C18 N1 C1 108.7(3) . . ?
C10 N1 Cu 103.6(3) . . ?
C18 N1 Cu 114.4(2) . . ?
C1 N1 Cu 104.1(3) . . ?
O2 N7 C16 118.0(3) . . ?
C13 N5 C12 123.3(3) . . ?
O4 N12 C23 117.9(4) . . ?
C5 N3 C11 115.9(4) . . ?
C5 N3 C6 110.2(3) . . ?
C11 N3 C6 111.4(3) . . ?
C5 N3 Cu 100.6(3) . . ?
C11 N3 Cu 114.0(2) . . ?
C6 N3 Cu 103.7(3) . . ?
C2 N2 C3 114.4(4) . . ?
C2 N2 C4 109.4(3) . . ?
C3 N2 C4 109.0(3) . . ?
C2 N2 Cu 103.5(3) . . ?
C3 N2 Cu 116.8(2) . . ?
C4 N2 Cu 102.9(3) . . ?
C7 N4 C8 112.3(4) . . ?
C7 N4 C9 110.5(3) . . ?
C8 N4 C9 107.8(4) . . ?
C7 N4 Cu 104.5(3) . . ?
C8 N4 Cu 115.8(3) . . ?
C9 N4 Cu 105.8(3) . . ?
N9 C13 N5 117.9(3) . . ?
N9 C13 N6 123.5(3) . . ?
N5 C13 N6 118.6(3) . . ?
N14 C20 N10 118.3(3) . . ?
N14 C20 N11 124.3(3) . . ?
N10 C20 N11 117.3(3) . . ?
N8 C17 N9 116.5(3) . . ?
N8 C17 C16 121.4(4) . . ?
N9 C17 C16 122.1(3) . . ?
N3 C11 C12 117.3(3) . . ?
N1 C18 C19 113.3(3) . . ?
N13 C24 N14 117.8(3) . . ?
N13 C24 C23 120.3(3) . . ?
N14 C24 C23 121.9(3) . . ?
N7 C16 C15 115.2(3) . . ?
N7 C16 C17 126.5(4) . . ?
C15 C16 C17 118.2(3) . . ?
N5 C12 C11 113.6(3) . . ?
O1 C15 N6 119.0(4) . . ?
O1 C15 C16 124.8(4) . . ?
N6 C15 C16 116.2(3) . . ?
O3 C22 N11 119.8(4) . . ?
O3 C22 C23 125.0(4) . . ?
N11 C22 C23 115.2(3) . . ?
N12 C23 C24 127.8(4) . . ?
N12 C23 C22 113.5(3) . . ?
C24 C23 C22 118.7(3) . . ?
N10 C19 C18 110.7(3) . . ?
C7 C6 N3 111.4(4) . . ?
C5 C4 N2 109.3(3) . . ?
C2 C1 N1 110.5(4) . . ?
N2 C2 C1 107.2(4) . . ?
N1 C10 C9 108.7(4) . . ?
N4 C7 C6 108.8(4) . . ?
C10 C9 N4 110.5(4) . . ?
N3 C5 C4 107.5(4) . . ?

_refine_diff_density_max         2.833
_refine_diff_density_min         -1.202
_refine_diff_density_rms         0.146


# start Validation Reply Form
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens. 1.13Ang From C9 2.75 eA-3
RESPONSE: Residual electron density near these carbon atoms and a bit high values for their ADP show possible conformational disorder, which was not possible to resolve
;
# end Validation Reply Form

#===END
####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2309461'
loop_
_audit_author_name
_audit_author_address
'Carla Bazzicalupi'
;University of Firenze
Italy
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2023-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H49 Cl3 N14 O18'
_chemical_formula_weight         928.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   12.5685(3)
_cell_length_b                   12.8470(3)
_cell_length_c                   12.9863(3)
_cell_angle_alpha                74.359(1)
_cell_angle_beta                 86.816(1)
_cell_angle_gamma                76.531(1)
_cell_volume                     1963.62(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9994
_cell_measurement_theta_min      3.53
_cell_measurement_theta_max      68.35

_exptl_crystal_description       prismatic
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_F_000             972
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    2.934
_shelx_estimated_absorpt_T_min   0.758
_shelx_estimated_absorpt_T_max   0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5842
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            57693
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.534
_diffrn_reflns_theta_max         68.523
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7214
_reflns_number_gt                5836
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_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)+(0.1307P)²+8.8237P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7214
_refine_ls_number_parameters     660
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0904
_refine_ls_wR_factor_ref         0.2577
_refine_ls_wR_factor_gt          0.2432
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.086
_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
Cl1 Cl 0.81690(10) 0.21369(9) 0.31203(9) 0.0319(3) Uani 1 1 d . . . . .
O21 O 0.3693(4) 0.0758(4) 0.2646(4) 0.0647(13) Uani 1 1 d . . . . .
N2 N 0.2691(4) 0.1103(4) 0.8115(4) 0.0407(11) Uani 1 1 d . . . . .
Cl2 Cl 0.32551(11) 0.00765(12) 0.21749(13) 0.0501(4) Uani 1 1 d . . . . .
O4 O 0.7592(3) 0.4476(3) 0.6678(3) 0.0452(9) Uani 1 1 d . . . . .
N3 N 0.0309(4) 0.1592(4) 0.7960(4) 0.0415(11) Uani 1 1 d . . . . .
Cl3 Cl 0.57344(12) 0.29920(13) -0.03116(10) 0.0455(4) Uani 1 1 d . . . . .
O2 O 0.1542(3) 0.4258(3) 1.2724(3) 0.0414(9) Uani 1 1 d . . . . .
N4 N 0.0489(4) 0.2040(4) 0.5655(4) 0.0415(11) Uani 1 1 d . . . . .
N1 N 0.2864(4) 0.1379(3) 0.5833(3) 0.0336(9) Uani 1 1 d . . . . .
O24 O 0.2537(5) -0.0420(5) 0.3041(5) 0.0883(17) Uani 1 1 d . U . . .
OW1 O -0.1512(3) 0.6622(3) 1.3391(3) 0.0345(8) Uani 1 1 d . . . . .
N13 N 0.6419(4) 0.2953(4) 0.6991(3) 0.0365(10) Uani 1 1 d . . . . .
H13A H 0.613704 0.239583 0.734783 0.044 Uiso 1 1 calc R U . . .
H13B H 0.681535 0.324205 0.732758 0.044 Uiso 1 1 calc R U . . .
O23 O 0.2543(5) 0.0622(5) 0.1318(5) 0.0910(18) Uani 1 1 d . U . . .
O32 O 0.6423(3) 0.3624(3) -0.1035(3) 0.0427(9) Uani 1 1 d . . . . .
N7 N 0.0550(4) 0.4778(4) 1.2365(3) 0.0373(10) Uani 1 1 d . . . . .
N12 N 0.7321(4) 0.4840(4) 0.5666(4) 0.0443(11) Uani 1 1 d . . . . .
O22 O 0.4077(3) -0.0807(3) 0.1953(4) 0.0568(11) Uani 1 1 d . . . . .
O34 O 0.5291(6) 0.3696(7) 0.0391(6) 0.108(2) Uani 1 1 d . U . . .
N8 N 0.1634(4) 0.2823(4) 1.1600(4) 0.0410(11) Uani 1 1 d . . . . .
H8A H 0.193337 0.224781 1.135321 0.049 Uiso 1 1 calc R U . . .
H8B H 0.200560 0.302441 1.203771 0.049 Uiso 1 1 calc R U . . .
N6 N -0.1459(3) 0.4528(3) 1.0643(3) 0.0257(8) Uani 1 1 d . . . . .
O33 O 0.4799(3) 0.2984(4) -0.0858(4) 0.0588(12) Uani 1 1 d . . . . .
N11 N 0.5775(3) 0.4199(3) 0.3796(3) 0.0266(8) Uani 1 1 d . . . . .
N9 N 0.0108(3) 0.3039(3) 1.0650(3) 0.0274(8) Uani 1 1 d . . . . .
N5 N -0.1431(3) 0.3210(3) 0.9729(3) 0.0259(8) Uani 1 1 d . . . . .
H5 H -0.209791 0.357731 0.951166 0.031 Uiso 1 1 calc R U . . .
N14 N 0.5644(3) 0.2883(3) 0.5490(3) 0.0269(8) Uani 1 1 d . . . . .
N10 N 0.4832(3) 0.2811(3) 0.4000(3) 0.0267(8) Uani 1 1 d . . . . .
H10 H 0.467928 0.307140 0.331256 0.032 Uiso 1 1 calc R U . . .
C20 C 0.5434(4) 0.3295(4) 0.4447(4) 0.0248(9) Uani 1 1 d . . . . .
C13 C -0.0908(4) 0.3586(4) 1.0362(3) 0.0241(9) Uani 1 1 d . . . . .
C22 C 0.6425(4) 0.4748(4) 0.4193(4) 0.0281(10) Uani 1 1 d . . . . .
C23 C 0.6697(4) 0.4292(4) 0.5350(4) 0.0288(10) Uani 1 1 d . . . . .
C18 C 0.3395(4) 0.2252(4) 0.5241(4) 0.0262(9) Uani 1 1 d . . . . .
H18A H 0.360843 0.261956 0.575037 0.031 Uiso 1 1 calc R U . . .
H18B H 0.285755 0.281451 0.473250 0.031 Uiso 1 1 calc R U . . .
C11 C -0.0193(4) 0.2498(4) 0.8423(4) 0.0266(9) Uani 1 1 d . . . . .
H11A H -0.061948 0.310750 0.785566 0.032 Uiso 1 1 calc R U . . .
H11B H 0.039630 0.278016 0.865473 0.032 Uiso 1 1 calc R U . . .
C15 C -0.0982(4) 0.4947(4) 1.1347(4) 0.0277(10) Uani 1 1 d . . . . .
C24 C 0.6249(4) 0.3355(4) 0.5954(4) 0.0286(10) Uani 1 1 d . . . . .
OW2 O 0.3966(3) 0.2957(4) 0.2029(3) 0.0417(9) Uani 1 1 d . . . . .
C16 C 0.0139(4) 0.4336(4) 1.1715(4) 0.0289(10) Uani 1 1 d . . . . .
O11 O 0.8183(3) 0.3276(3) 0.2969(3) 0.0409(9) Uani 1 1 d . . . . .
C17 C 0.0638(4) 0.3377(4) 1.1315(4) 0.0295(10) Uani 1 1 d . . . . .
C19 C 0.4413(4) 0.1858(4) 0.4616(4) 0.0262(9) Uani 1 1 d . . . . .
H19A H 0.498408 0.134120 0.511880 0.031 Uiso 1 1 calc R U . . .
H19B H 0.422204 0.145675 0.412536 0.031 Uiso 1 1 calc R U . . .
O31 O 0.6350(7) 0.1915(7) 0.0076(7) 0.130(3) Uani 1 1 d . U . . .
C12 C -0.0955(4) 0.2221(4) 0.9381(4) 0.0278(10) Uani 1 1 d . . . . .
H12A H -0.154340 0.192236 0.917199 0.033 Uiso 1 1 calc R U . . .
H12B H -0.053319 0.164717 0.997770 0.033 Uiso 1 1 calc R U . . .
C21 C 0.5504(4) 0.4565(4) 0.2650(4) 0.0346(11) Uani 1 1 d . . . . .
H21A H 0.580686 0.521129 0.231031 0.052 Uiso 1 1 calc R U . . .
H21B H 0.581756 0.396110 0.231809 0.052 Uiso 1 1 calc R U . . .
H21C H 0.470752 0.476497 0.255575 0.052 Uiso 1 1 calc R U . . .
C14 C -0.2597(4) 0.5045(4) 1.0301(4) 0.0338(11) Uani 1 1 d . . . . .
H14A H -0.285546 0.570149 1.057208 0.051 Uiso 1 1 calc R U . . .
H14B H -0.263955 0.526569 0.951826 0.051 Uiso 1 1 calc R U . . .
H14C H -0.305641 0.451298 1.058477 0.051 Uiso 1 1 calc R U . . .
C8 C -0.0158(5) 0.3128(5) 0.5032(5) 0.0470(14) Uani 1 1 d . . . . .
H8C H -0.033067 0.364029 0.548854 0.070 Uiso 1 1 calc R U . . .
H8D H 0.026819 0.343377 0.441752 0.070 Uiso 1 1 calc R U . . .
H8E H -0.083869 0.302829 0.478020 0.070 Uiso 1 1 calc R U . . .
O1 O -0.1478(3) 0.5777(3) 1.1598(3) 0.0350(8) Uani 1 1 d . . . . .
O3 O 0.6708(3) 0.5549(3) 0.3622(3) 0.0372(8) Uani 1 1 d . . . . .
C3 C 0.3357(5) 0.1681(5) 0.8561(5) 0.0472(14) Uani 1 1 d . . . . .
H3A H 0.355848 0.227308 0.798833 0.071 Uiso 1 1 calc R U . . .
H3B H 0.293579 0.200175 0.910374 0.071 Uiso 1 1 calc R U . . .
H3C H 0.402210 0.115158 0.888979 0.071 Uiso 1 1 calc R U . . .
O12 O 0.8857(10) 0.1400(6) 0.3931(10) 0.089(5) Uani 0.587(10) 1 d . . P . .
O13 O 0.7045(5) 0.1961(5) 0.3289(7) 0.052(2) Uani 0.587(10) 1 d . . P . .
O14 O 0.8431(10) 0.1828(8) 0.2128(7) 0.080(4) Uani 0.587(10) 1 d . . P . .
O12' O 0.7804(9) 0.1787(8) 0.4196(8) 0.053(3) Uani 0.413(10) 1 d . . P . .
O14' O 0.9297(11) 0.1542(11) 0.3112(11) 0.075(5) Uani 0.413(10) 1 d . . P . .
O13' O 0.7581(12) 0.1991(12) 0.2378(12) 0.073(4) Uani 0.413(10) 1 d . U P . .
C1A C 0.3720(7) 0.0548(7) 0.6664(8) 0.0285(17) Uani 0.677(10) 1 d . . P A 1
H1A H 0.406436 -0.009495 0.638355 0.034 Uiso 0.677(10) 1 calc R U P A 1
H1B H 0.430132 0.091631 0.676419 0.034 Uiso 0.677(10) 1 calc R U P A 1
C9A C 0.1305(8) 0.1651(7) 0.4761(6) 0.0313(19) Uani 0.677(10) 1 d . . P A 1
H9A H 0.093838 0.127320 0.436339 0.038 Uiso 0.677(10) 1 calc R U P A 1
H9B H 0.148027 0.231085 0.424561 0.038 Uiso 0.677(10) 1 calc R U P A 1
C6A C -0.0556(8) 0.1447(12) 0.7205(13) 0.044(3) Uani 0.677(10) 1 d . . P A 1
H6A H -0.089611 0.083138 0.759184 0.053 Uiso 0.677(10) 1 calc R U P A 1
H6B H -0.114134 0.213427 0.701881 0.053 Uiso 0.677(10) 1 calc R U P A 1
C2A C 0.3203(7) 0.0143(7) 0.7727(6) 0.0343(19) Uani 0.677(10) 1 d . . P A 1
H2A H 0.264832 -0.026444 0.764503 0.041 Uiso 0.677(10) 1 calc R U P A 1
H2B H 0.376717 -0.036663 0.824354 0.041 Uiso 0.677(10) 1 calc R U P A 1
C5A C 0.0832(8) 0.0578(7) 0.8598(8) 0.040(2) Uani 0.677(10) 1 d . . P A 1
H5A H 0.101864 0.002565 0.817375 0.048 Uiso 0.677(10) 1 calc R U P A 1
H5B H 0.034802 0.031192 0.918954 0.048 Uiso 0.677(10) 1 calc R U P A 1
C4A C 0.1853(11) 0.0716(9) 0.9038(7) 0.044(2) Uani 0.677(10) 1 d . . P A 1
H4A H 0.221893 0.000322 0.953034 0.053 Uiso 0.677(10) 1 calc R U P A 1
H4B H 0.165399 0.127420 0.945516 0.053 Uiso 0.677(10) 1 calc R U P A 1
C7A C -0.0032(7) 0.1203(7) 0.6177(7) 0.038(2) Uani 0.677(10) 1 d . . P A 1
H7A H 0.050512 0.048037 0.635339 0.046 Uiso 0.677(10) 1 calc R U P A 1
H7B H -0.060149 0.115822 0.570452 0.046 Uiso 0.677(10) 1 calc R U P A 1
C10A C 0.2354(8) 0.0871(8) 0.5260(8) 0.0236(17) Uani 0.677(10) 1 d . . P A 1
H10A H 0.218729 0.018680 0.574040 0.028 Uiso 0.677(10) 1 calc R U P A 1
H10B H 0.284733 0.065901 0.469269 0.028 Uiso 0.677(10) 1 calc R U P A 1
C9B C 0.0909(12) 0.1078(14) 0.5346(12) 0.030(4) Uani 0.323(10) 1 d . . P A 2
H9C H 0.042990 0.098927 0.481103 0.036 Uiso 0.323(10) 1 calc R U P A 2
H9D H 0.101259 0.041615 0.596666 0.036 Uiso 0.323(10) 1 calc R U P A 2
C6B C -0.0137(19) 0.0947(17) 0.7667(16) 0.034(4) Uani 0.323(10) 1 d . . P A 2
H6C H -0.074942 0.076289 0.813962 0.040 Uiso 0.323(10) 1 calc R U P A 2
H6D H 0.039358 0.025400 0.763263 0.040 Uiso 0.323(10) 1 calc R U P A 2
C7B C -0.0546(14) 0.1670(16) 0.6541(18) 0.031(4) Uani 0.323(10) 1 d . . P A 2
H7C H -0.106081 0.235654 0.661711 0.037 Uiso 0.323(10) 1 calc R U P A 2
H7D H -0.095834 0.126138 0.622418 0.037 Uiso 0.323(10) 1 calc R U P A 2
C2B C 0.3759(13) 0.0547(13) 0.7365(17) 0.031(4) Uani 0.323(10) 1 d . . P A 2
H2C H 0.425521 0.106224 0.713750 0.037 Uiso 0.323(10) 1 calc R U P A 2
H2D H 0.418614 -0.016632 0.780836 0.037 Uiso 0.323(10) 1 calc R U P A 2
C4B C 0.2288(14) 0.0269(14) 0.8667(14) 0.034(4) Uani 0.323(10) 1 d . . P A 2
H4C H 0.276744 -0.017679 0.928487 0.040 Uiso 0.323(10) 1 calc R U P A 2
H4D H 0.220878 -0.021787 0.821436 0.040 Uiso 0.323(10) 1 calc R U P A 2
C5B C 0.1188(18) 0.0798(14) 0.9037(13) 0.026(4) Uani 0.323(10) 1 d . . P A 2
H5C H 0.128972 0.128049 0.948519 0.031 Uiso 0.323(10) 1 calc R U P A 2
H5D H 0.084473 0.021042 0.948385 0.031 Uiso 0.323(10) 1 calc R U P A 2
C1B C 0.3304(16) 0.0361(13) 0.6388(15) 0.028(4) Uani 0.323(10) 1 d . . P A 2
H1C H 0.389216 -0.001069 0.598229 0.034 Uiso 0.323(10) 1 calc R U P A 2
H1D H 0.274722 -0.008988 0.659055 0.034 Uiso 0.323(10) 1 calc R U P A 2
C10B C 0.199(2) 0.127(2) 0.4867(15) 0.030(4) Uani 0.323(10) 1 d . . P A 2
H10C H 0.186113 0.195942 0.427697 0.036 Uiso 0.323(10) 1 calc R U P A 2
H10D H 0.234802 0.064603 0.456472 0.036 Uiso 0.323(10) 1 calc R U P A 2
H3 H 0.433(6) 0.322(6) 0.149(6) 0.050(19) Uiso 1 1 d . . . . .
H1 H -0.189(6) 0.634(6) 1.360(5) 0.04(2) Uiso 1 1 d . . . . .
H2 H -0.130(5) 0.634(5) 1.295(5) 0.038(17) Uiso 1 1 d . . . . .
H4 H 0.400(5) 0.222(6) 0.217(5) 0.050 Uiso 1 1 d . U . . .
H6 H 0.084(5) 0.228(5) 0.606(5) 0.034(14) Uiso 1 1 d . . . . .
H7 H 0.234(6) 0.166(6) 0.766(5) 0.049(18) Uiso 1 1 d . . . . .
H8 H 0.800(4) 0.515(4) 0.691(4) 0.029(13) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 O13' 1.324(13) . ?
Cl1 O12 1.392(7) . ?
Cl1 O11 1.428(4) . ?
Cl1 O12' 1.432(10) . ?
Cl1 O14' 1.446(12) . ?
Cl1 O14 1.447(7) . ?
Cl1 O13 1.478(6) . ?
O21 Cl2 1.413(4) . ?
N2 C4B 1.310(17) . ?
N2 C2A 1.456(8) . ?
N2 C3 1.471(7) . ?
N2 C4A 1.605(12) . ?
N2 C2B 1.745(18) . ?
Cl2 O23 1.389(6) . ?
Cl2 O22 1.426(4) . ?
Cl2 O24 1.501(6) . ?
O4 N12 1.307(6) . ?
N3 C6B 1.247(19) . ?
N3 C5A 1.377(10) . ?
N3 C11 1.452(6) . ?
N3 C6A 1.577(13) . ?
N3 C5B 1.759(18) . ?
Cl3 O31 1.391(9) . ?
Cl3 O33 1.410(4) . ?
Cl3 O34 1.454(7) . ?
Cl3 O32 1.455(4) . ?
O2 N7 1.315(6) . ?
N4 C9B 1.381(15) . ?
N4 C7A 1.389(9) . ?
N4 C8 1.485(7) . ?
N4 C9A 1.610(10) . ?
N4 C7B 1.75(2) . ?
N1 C1B 1.318(17) . ?
N1 C10A 1.380(9) . ?
N1 C18 1.456(6) . ?
N1 C1A 1.560(10) . ?
N1 C10B 1.77(2) . ?
N13 C24 1.316(6) . ?
N7 C16 1.320(6) . ?
N12 C23 1.314(6) . ?
N8 C17 1.306(6) . ?
N6 C13 1.378(6) . ?
N6 C15 1.401(5) . ?
N6 C14 1.467(6) . ?
N11 C20 1.382(6) . ?
N11 C22 1.393(6) . ?
N11 C21 1.468(6) . ?
N9 C13 1.325(6) . ?
N9 C17 1.333(6) . ?
N5 C13 1.328(5) . ?
N5 C12 1.449(6) . ?
N14 C20 1.331(6) . ?
N14 C24 1.331(6) . ?
N10 C20 1.327(6) . ?
N10 C19 1.463(6) . ?
C22 O3 1.211(6) . ?
C22 C23 1.486(7) . ?
C23 C24 1.463(7) . ?
C18 C19 1.535(6) . ?
C11 C12 1.542(6) . ?
C15 O1 1.220(6) . ?
C15 C16 1.479(7) . ?
C16 C17 1.460(7) . ?
O12 O14' 1.160(16) . ?
O12 O12' 1.361(16) . ?
O13 O13' 1.324(17) . ?
O13 O12' 1.495(14) . ?
O14 O13' 1.089(16) . ?
O14 O14' 1.634(18) . ?
C1A C2A 1.506(12) . ?
C9A C10A 1.514(12) . ?
C6A C7A 1.532(13) . ?
C5A C4A 1.500(15) . ?
C9B C10B 1.51(2) . ?
C6B C7B 1.55(3) . ?
C2B C1B 1.52(2) . ?
C4B C5B 1.51(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O13' Cl1 O12 132.7(7) . . ?
O13' Cl1 O11 112.2(6) . . ?
O12 Cl1 O11 114.6(4) . . ?
O13' Cl1 O12' 115.4(8) . . ?
O12 Cl1 O12' 57.6(7) . . ?
O11 Cl1 O12' 104.7(4) . . ?
O13' Cl1 O14' 111.5(9) . . ?
O12 Cl1 O14' 48.2(7) . . ?
O11 Cl1 O14' 106.6(6) . . ?
O12' Cl1 O14' 105.8(7) . . ?
O13' Cl1 O14 46.0(7) . . ?
O12 Cl1 O14 109.6(8) . . ?
O11 Cl1 O14 109.9(4) . . ?
O12' Cl1 O14 145.1(6) . . ?
O14' Cl1 O14 68.8(7) . . ?
O13' Cl1 O13 56.1(7) . . ?
O12 Cl1 O13 110.0(6) . . ?
O11 Cl1 O13 111.4(3) . . ?
O12' Cl1 O13 61.8(6) . . ?
O14' Cl1 O13 141.9(7) . . ?
O14 Cl1 O13 100.3(6) . . ?
C4B N2 C3 125.1(9) . . ?
C2A N2 C3 120.7(5) . . ?
C2A N2 C4A 107.4(6) . . ?
C3 N2 C4A 106.0(6) . . ?
C4B N2 C2B 106.2(11) . . ?
C3 N2 C2B 94.2(7) . . ?
O23 Cl2 O21 116.1(4) . . ?
O23 Cl2 O22 112.5(3) . . ?
O21 Cl2 O22 112.3(3) . . ?
O23 Cl2 O24 103.9(4) . . ?
O21 Cl2 O24 102.8(3) . . ?
O22 Cl2 O24 108.0(3) . . ?
C6B N3 C11 128.6(11) . . ?
C5A N3 C11 120.7(6) . . ?
C5A N3 C6A 110.7(8) . . ?
C11 N3 C6A 108.5(5) . . ?
C6B N3 C5B 107.5(13) . . ?
C11 N3 C5B 97.5(7) . . ?
O31 Cl3 O33 110.1(4) . . ?
O31 Cl3 O34 122.1(6) . . ?
O33 Cl3 O34 103.0(4) . . ?
O31 Cl3 O32 107.7(4) . . ?
O33 Cl3 O32 110.2(3) . . ?
O34 Cl3 O32 103.2(3) . . ?
C9B N4 C8 129.8(8) . . ?
C7A N4 C8 120.3(5) . . ?
C7A N4 C9A 110.3(5) . . ?
C8 N4 C9A 101.8(5) . . ?
C9B N4 C7B 102.3(9) . . ?
C8 N4 C7B 97.2(7) . . ?
C1B N1 C18 129.4(9) . . ?
C10A N1 C18 118.1(5) . . ?
C10A N1 C1A 113.5(6) . . ?
C18 N1 C1A 106.7(5) . . ?
C1B N1 C10B 106.9(13) . . ?
C18 N1 C10B 103.1(7) . . ?
O2 N7 C16 114.9(4) . . ?
O4 N12 C23 114.4(5) . . ?
C13 N6 C15 120.5(4) . . ?
C13 N6 C14 120.7(4) . . ?
C15 N6 C14 118.5(4) . . ?
C20 N11 C22 121.2(4) . . ?
C20 N11 C21 120.2(4) . . ?
C22 N11 C21 118.5(4) . . ?
C13 N9 C17 118.5(4) . . ?
C13 N5 C12 122.9(4) . . ?
C20 N14 C24 118.3(4) . . ?
C20 N10 C19 122.0(4) . . ?
N10 C20 N14 117.3(4) . . ?
N10 C20 N11 117.3(4) . . ?
N14 C20 N11 125.4(4) . . ?
N9 C13 N5 117.4(4) . . ?
N9 C13 N6 125.5(4) . . ?
N5 C13 N6 117.1(4) . . ?
O3 C22 N11 120.9(4) . . ?
O3 C22 C23 124.2(4) . . ?
N11 C22 C23 114.9(4) . . ?
N12 C23 C24 130.3(5) . . ?
N12 C23 C22 111.5(4) . . ?
C24 C23 C22 118.2(4) . . ?
N1 C18 C19 114.9(4) . . ?
N3 C11 C12 116.2(4) . . ?
O1 C15 N6 120.1(4) . . ?
O1 C15 C16 124.3(4) . . ?
N6 C15 C16 115.5(4) . . ?
N13 C24 N14 117.2(4) . . ?
N13 C24 C23 120.7(4) . . ?
N14 C24 C23 122.0(4) . . ?
N7 C16 C17 129.5(5) . . ?
N7 C16 C15 112.6(4) . . ?
C17 C16 C15 117.8(4) . . ?
N8 C17 N9 117.8(4) . . ?
N8 C17 C16 120.2(4) . . ?
N9 C17 C16 122.0(4) . . ?
N10 C19 C18 110.0(4) . . ?
N5 C12 C11 110.1(4) . . ?
O14' O12 O12' 130.9(10) . . ?
O14' O12 Cl1 68.3(8) . . ?
O12' O12 Cl1 62.7(6) . . ?
O13' O13 Cl1 56.1(6) . . ?
O13' O13 O12' 111.4(8) . . ?
Cl1 O13 O12' 57.6(4) . . ?
O13' O14 Cl1 61.0(8) . . ?
O13' O14 O14' 113.0(10) . . ?
Cl1 O14 O14' 55.6(5) . . ?
O12 O12' Cl1 59.7(6) . . ?
O12 O12' O13 110.7(9) . . ?
Cl1 O12' O13 60.6(5) . . ?
O12 O14' Cl1 63.4(7) . . ?
O12 O14' O14 111.2(12) . . ?
Cl1 O14' O14 55.7(6) . . ?
O14 O13' O13 137.0(14) . . ?
O14 O13' Cl1 73.0(9) . . ?
O13 O13' Cl1 67.9(8) . . ?
C2A C1A N1 111.8(6) . . ?
C10A C9A N4 111.3(6) . . ?
C7A C6A N3 111.7(6) . . ?
N2 C2A C1A 108.2(7) . . ?
N3 C5A C4A 108.1(8) . . ?
C5A C4A N2 112.3(6) . . ?
N4 C7A C6A 109.6(7) . . ?
N1 C10A C9A 110.0(7) . . ?
N4 C9B C10B 102.1(13) . . ?
N3 C6B C7B 100.2(15) . . ?
C6B C7B N4 114.6(12) . . ?
C1B C2B N2 109.9(11) . . ?
N2 C4B C5B 104.8(14) . . ?
C4B C5B N3 112.2(12) . . ?
N1 C1B C2B 102.6(14) . . ?
C9B C10B N1 111.4(11) . . ?

_refine_diff_density_max         2.694
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.114


# start Validation Reply Form
_vrf_PLAT097_shelx               
;
PROBLEM: Large Reported Max. (Positive) Residual Density 2.69 eA-3
RESPONSE: the signalled residual density is located near an oxygen atom belonging to a perchlorate anion most likely affected by dynamic or positional disorder. Actually, two of its oxygens shown higher ADPs than the other two, but the overall geometry of the anion appears to be acceptable
;
_vrf_PLAT971_shelx               
;
PROBLEM: Check Calcd Resid. Dens. 1.08Ang From O34 2.72 eA-3
RESPONSE: the signalled residual density is located near an oxygen atom belonging to a perchlorate anion most likely affected by dynamic or positional disorder. Actually, two of its oxygens shown higher ADPs than the other two, but the overall geometry of the anion appears to be acceptable
;
# end Validation Reply Form
#===END
####################################################################### 
# 
# 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_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 2309463'
loop_
_audit_author_name
_audit_author_address
'Carla Bazzicalupi'
;University of Firenze
Italy
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2023-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H64.92 Cl2 Cu N14 O23.46'
_chemical_formula_weight         1059.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.5546(3)
_cell_length_b                   12.9018(4)
_cell_length_c                   19.4955(6)
_cell_angle_alpha                74.443(2)
_cell_angle_beta                 79.300(2)
_cell_angle_gamma                76.145(2)
_cell_volume                     2228.81(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9858
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      66.49

_exptl_crystal_description       prismatic
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_F_000             1115
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_min          0.20
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_max          1.00
_exptl_absorpt_coefficient_mu    2.665
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4865
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            53414
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.372
_diffrn_reflns_theta_max         66.603
_diffrn_reflns_theta_full        66.603
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             7832
_reflns_number_gt                6959
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_publication_material  'PARST(Nardelli, 1995)'
_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)+(0.1104P)²+3.6526P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7832
_refine_ls_number_parameters     612
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0602
_refine_ls_wR_factor_ref         0.1798
_refine_ls_wR_factor_gt          0.1727
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu 0.68347(5) 0.50356(4) 0.74093(2) 0.02119(17) Uani 1 1 d . . . . .
N12 N 1.1328(3) 0.8955(2) 0.33739(15) 0.0276(6) Uani 1 1 d . . . . .
OW1 O 0.8860(3) 0.4585(2) 0.78278(14) 0.0350(6) Uani 1 1 d . . . . .
Cl1 Cl 1.25172(8) 0.56756(7) 0.58567(4) 0.0276(2) Uani 1 1 d . . . . .
N7 N 0.3529(4) 0.1140(3) 1.16452(18) 0.0368(8) Uani 1 1 d . . . . .
Cl2 Cl 0.82944(9) 1.26089(7) 0.03451(5) 0.0318(2) Uani 1 1 d . . . . .
N6 N 0.6531(3) 0.0443(2) 1.03323(14) 0.0214(6) Uani 1 1 d . . . . .
O3 O 1.3043(2) 0.8953(2) 0.43323(13) 0.0314(6) Uani 1 1 d . . . . .
N5 N 0.6779(3) 0.0970(2) 0.90968(15) 0.0233(6) Uani 1 1 d . . . . .
O4 O 1.0533(3) 0.8883(2) 0.29330(13) 0.0310(5) Uani 1 1 d . . . . .
N8 N 0.2677(3) 0.2626(3) 1.03021(19) 0.0360(7) Uani 1 1 d . . . . .
H8A H 0.241088 0.302236 0.988650 0.043 Uiso 1 1 calc R U . . .
H8B H 0.211634 0.271126 1.070372 0.043 Uiso 1 1 calc R U . . .
O1 O 0.6267(3) -0.0073(2) 1.15514(13) 0.0349(6) Uani 1 1 d . . . . .
N13 N 0.8520(3) 0.8349(2) 0.39996(16) 0.0283(6) Uani 1 1 d . . . . .
H13A H 0.765692 0.821199 0.419636 0.034 Uiso 1 1 calc R U . . .
H13B H 0.879052 0.839629 0.353731 0.034 Uiso 1 1 calc R U . . .
OW11 O 1.0293(3) 0.9678(2) 0.14645(14) 0.0359(6) Uani 1 1 d . . . . .
N4 N 0.5376(3) 0.5521(2) 0.82191(15) 0.0275(6) Uani 1 1 d . . . . .
OW3 O -0.0459(3) 0.1852(2) 1.24934(14) 0.0355(6) Uani 1 1 d . . . . .
OW5 O 1.0662(3) 0.2560(2) 0.81943(15) 0.0413(7) Uani 1 1 d . . . . .
N2 N 0.7419(3) 0.4745(2) 0.64060(14) 0.0222(6) Uani 1 1 d . . . . .
O11 O 1.2619(3) 0.5876(3) 0.65335(15) 0.0459(7) Uani 1 1 d . . . . .
O12 O 1.1097(3) 0.6135(2) 0.56565(17) 0.0420(7) Uani 1 1 d . . . . .
N10 N 0.9376(3) 0.8493(2) 0.61971(15) 0.0227(6) Uani 1 1 d . . . . .
N1 N 0.6657(3) 0.6665(2) 0.69207(14) 0.0220(6) Uani 1 1 d . . . . .
N9 N 0.4730(3) 0.1807(2) 0.97004(15) 0.0223(6) Uani 1 1 d . . . . .
N11 N 1.1251(3) 0.8683(2) 0.52656(15) 0.0227(6) Uani 1 1 d . . . . .
OW8 O -0.2548(3) 0.0647(2) 1.25744(16) 0.0438(7) Uani 1 1 d . . . . .
O14 O 1.2857(3) 0.4525(2) 0.58941(18) 0.0475(7) Uani 1 1 d . . . . .
N14 N 0.8951(3) 0.8407(2) 0.51009(15) 0.0217(6) Uani 1 1 d . . . . .
N3 N 0.6043(3) 0.3617(2) 0.76978(14) 0.0228(6) Uani 1 1 d . . . . .
O13 O 1.3558(3) 0.6207(3) 0.53340(15) 0.0425(7) Uani 1 1 d . . . . .
O2 O 0.2259(3) 0.1769(3) 1.16866(17) 0.0468(7) Uani 1 1 d . . . . .
OW4 O 1.1230(4) 0.3865(3) 0.9072(2) 0.0572(9) Uani 1 1 d . . . . .
O21 O 0.8220(4) 1.1788(3) 0.10025(17) 0.0577(9) Uani 1 1 d . . . . .
O22 O 0.6883(3) 1.2979(3) 0.01208(19) 0.0539(8) Uani 1 1 d . . . . .
O23 O 0.9232(4) 1.2129(3) -0.02060(19) 0.0625(10) Uani 1 1 d . . . . .
OW6 O 1.2914(4) 0.2205(3) 0.71756(19) 0.0617(10) Uani 1 1 d . . . . .
OW7 O 1.4190(3) 0.2452(3) 0.5645(2) 0.0614(10) Uani 1 1 d . . . . .
C20 C 0.9852(3) 0.8519(2) 0.55112(17) 0.0207(6) Uani 1 1 d . . . . .
C23 C 1.0812(3) 0.8732(3) 0.40768(17) 0.0223(7) Uani 1 1 d . . . . .
C13 C 0.5987(3) 0.1094(2) 0.97168(17) 0.0197(6) Uani 1 1 d . . . . .
C22 C 1.1804(3) 0.8795(3) 0.45436(18) 0.0235(7) Uani 1 1 d . . . . .
C11 C 0.6833(4) 0.2740(3) 0.82350(18) 0.0249(7) Uani 1 1 d . . . . .
H11A H 0.670411 0.299281 0.868377 0.030 Uiso 1 1 calc R U . . .
H11B H 0.788377 0.262018 0.805337 0.030 Uiso 1 1 calc R U . . .
C18 C 0.8044(3) 0.7046(3) 0.68427(18) 0.0230(7) Uani 1 1 d . . . . .
H18A H 0.879344 0.663657 0.653529 0.028 Uiso 1 1 calc R U . . .
H18B H 0.837117 0.686299 0.732170 0.028 Uiso 1 1 calc R U . . .
C2 C 0.7285(4) 0.5834(3) 0.58749(18) 0.0259(7) Uani 1 1 d . . . . .
H2A H 0.692666 0.578520 0.544187 0.031 Uiso 1 1 calc R U . . .
H2B H 0.824947 0.603955 0.572751 0.031 Uiso 1 1 calc R U . . .
C17 C 0.3915(4) 0.1908(3) 1.03229(19) 0.0253(7) Uani 1 1 d . . . . .
C16 C 0.4347(4) 0.1231(3) 1.10042(18) 0.0254(7) Uani 1 1 d . . . . .
C5 C 0.6138(4) 0.3242(3) 0.70247(18) 0.0250(7) Uani 1 1 d . . . . .
H5A H 0.526396 0.294789 0.703755 0.030 Uiso 1 1 calc R U . . .
H5B H 0.700185 0.264607 0.699097 0.030 Uiso 1 1 calc R U . . .
C1 C 0.6232(4) 0.6703(3) 0.62130(18) 0.0254(7) Uani 1 1 d . . . . .
H1A H 0.624789 0.743849 0.589054 0.030 Uiso 1 1 calc R U . . .
H1B H 0.523260 0.656784 0.628224 0.030 Uiso 1 1 calc R U . . .
C15 C 0.5758(4) 0.0494(3) 1.10070(17) 0.0243(7) Uani 1 1 d . . . . .
C24 C 0.9409(4) 0.8485(3) 0.43984(18) 0.0232(7) Uani 1 1 d . . . . .
C4 C 0.6248(4) 0.4190(3) 0.63739(18) 0.0253(7) Uani 1 1 d . . . . .
H4A H 0.645905 0.391364 0.593094 0.030 Uiso 1 1 calc R U . . .
H4B H 0.530940 0.472234 0.635937 0.030 Uiso 1 1 calc R U . . .
C19 C 0.7944(3) 0.8278(3) 0.65191(18) 0.0235(7) Uani 1 1 d . . . . .
H19A H 0.727392 0.853252 0.614966 0.028 Uiso 1 1 calc R U . . .
H19B H 0.755203 0.868781 0.689907 0.028 Uiso 1 1 calc R U . . .
O24 O 0.8799(5) 1.3526(3) 0.0406(3) 0.0897(14) Uani 1 1 d . . . . .
OW10 O -0.5514(5) -0.0574(3) 1.29138(19) 0.0740(11) Uani 1 1 d . U . . .
C21 C 1.2207(4) 0.8700(3) 0.57740(19) 0.0285(7) Uani 1 1 d . . . . .
H21A H 1.315444 0.882445 0.551111 0.043 Uiso 1 1 calc R U . . .
H21B H 1.176515 0.929161 0.602084 0.043 Uiso 1 1 calc R U . . .
H21C H 1.233849 0.799434 0.612768 0.043 Uiso 1 1 calc R U . . .
C10 C 0.5474(4) 0.7289(3) 0.7353(2) 0.0295(8) Uani 1 1 d . . . . .
H10A H 0.490166 0.790473 0.702873 0.035 Uiso 1 1 calc R U . . .
H10B H 0.589909 0.760026 0.765937 0.035 Uiso 1 1 calc R U . . .
C7 C 0.4472(4) 0.4666(3) 0.8534(2) 0.0323(8) Uani 1 1 d . . . . .
H7A H 0.345758 0.502250 0.867318 0.039 Uiso 1 1 calc R U . . .
H7B H 0.485473 0.416888 0.897095 0.039 Uiso 1 1 calc R U . . .
C9 C 0.4487(4) 0.6541(3) 0.7820(2) 0.0313(8) Uani 1 1 d . . . . .
H9A H 0.380598 0.692439 0.816379 0.038 Uiso 1 1 calc R U . . .
H9B H 0.390947 0.635078 0.751603 0.038 Uiso 1 1 calc R U . . .
C12 C 0.6331(4) 0.1643(3) 0.84088(18) 0.0265(7) Uani 1 1 d . . . . .
H12A H 0.525957 0.177891 0.843524 0.032 Uiso 1 1 calc R U . . .
H12B H 0.676514 0.124964 0.802396 0.032 Uiso 1 1 calc R U . . .
C6 C 0.4506(4) 0.4015(3) 0.79912(19) 0.0291(7) Uani 1 1 d . . . . .
H6A H 0.403362 0.338058 0.822203 0.035 Uiso 1 1 calc R U . . .
H6B H 0.396124 0.448243 0.759514 0.035 Uiso 1 1 calc R U . . .
C14 C 0.7955(4) -0.0304(3) 1.02904(19) 0.0279(7) Uani 1 1 d . . . . .
H14A H 0.816695 -0.070033 1.077602 0.042 Uiso 1 1 calc R U . . .
H14B H 0.793982 -0.083142 1.001297 0.042 Uiso 1 1 calc R U . . .
H14C H 0.870807 0.012059 1.005443 0.042 Uiso 1 1 calc R U . . .
C3 C 0.8879(4) 0.4064(3) 0.62644(19) 0.0282(7) Uani 1 1 d . . . . .
H3A H 0.962491 0.445347 0.628962 0.042 Uiso 1 1 calc R U . . .
H3B H 0.897460 0.336477 0.662501 0.042 Uiso 1 1 calc R U . . .
H3C H 0.900396 0.392279 0.578502 0.042 Uiso 1 1 calc R U . . .
C8 C 0.6021(5) 0.5742(3) 0.8795(2) 0.0350(8) Uani 1 1 d . . . . .
H8C H 0.659669 0.505645 0.904729 0.053 Uiso 1 1 calc R U . . .
H8D H 0.664817 0.627606 0.857934 0.053 Uiso 1 1 calc R U . . .
H8E H 0.524013 0.603751 0.913657 0.053 Uiso 1 1 calc R U . . .
OW2 O 1.0869(6) 0.5755(4) 0.7860(3) 0.040(2) Uani 0.557(12) 1 d . . P . .
OW9 O -0.4441(5) 0.0204(4) 1.3758(3) 0.1017(16) Uani 1 1 d . . . . .
OW2' O 0.9949(10) 0.6061(6) 0.8316(5) 0.055(3) Uani 0.443(12) 1 d . . P . .
H1 H 0.764(5) 0.053(4) 0.910(2) 0.036(8) Uiso 1 1 d . . . . .
H2 H 1.000(5) 0.851(3) 0.651(2) 0.036(8) Uiso 1 1 d . . . . .
OW12 O 0.5721(12) 0.9326(9) 0.5083(7) 0.045(3) Uani 0.25 1 d . . P . .
OW13 O 0.9449(15) 0.5158(13) 0.9611(9) 0.047(4) Uani 0.2 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu N4 2.030(3) . ?
Cu N2 2.041(3) . ?
Cu N1 2.042(3) . ?
Cu N3 2.048(3) . ?
Cu OW1 2.131(3) . ?
N12 O4 1.282(4) . ?
N12 C23 1.345(4) . ?
Cl1 O12 1.425(3) . ?
Cl1 O14 1.426(3) . ?
Cl1 O11 1.436(3) . ?
Cl1 O13 1.440(3) . ?
N7 O2 1.290(5) . ?
N7 C16 1.337(5) . ?
Cl2 O24 1.420(4) . ?
Cl2 O22 1.427(3) . ?
Cl2 O21 1.429(3) . ?
Cl2 O23 1.440(3) . ?
N6 C13 1.377(4) . ?
N6 C15 1.393(4) . ?
N6 C14 1.470(4) . ?
O3 C22 1.226(4) . ?
N5 C13 1.329(4) . ?
N5 C12 1.465(4) . ?
N8 C17 1.316(5) . ?
O1 C15 1.226(4) . ?
N13 C24 1.322(4) . ?
N4 C9 1.490(5) . ?
N4 C7 1.494(4) . ?
N4 C8 1.495(5) . ?
N2 C3 1.482(4) . ?
N2 C4 1.484(4) . ?
N2 C2 1.498(4) . ?
N10 C20 1.324(4) . ?
N10 C19 1.453(4) . ?
N1 C10 1.487(4) . ?
N1 C18 1.489(4) . ?
N1 C1 1.494(4) . ?
N9 C13 1.326(4) . ?
N9 C17 1.335(4) . ?
N11 C20 1.379(4) . ?
N11 C22 1.390(4) . ?
N11 C21 1.475(4) . ?
N14 C20 1.335(4) . ?
N14 C24 1.342(4) . ?
N3 C11 1.482(4) . ?
N3 C6 1.494(4) . ?
N3 C5 1.497(4) . ?
C23 C24 1.440(5) . ?
C23 C22 1.459(5) . ?
C11 C12 1.536(4) . ?
C18 C19 1.532(4) . ?
C2 C1 1.520(5) . ?
C17 C16 1.451(5) . ?
C16 C15 1.452(5) . ?
C5 C4 1.516(5) . ?
C10 C9 1.514(5) . ?
C7 C6 1.510(5) . ?
OW2 OW2' 1.204(10) . ?

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
N4 Cu N2 153.52(12) . . ?
N4 Cu N1 86.57(11) . . ?
N2 Cu N1 86.79(11) . . ?
N4 Cu N3 86.59(11) . . ?
N2 Cu N3 86.94(11) . . ?
N1 Cu N3 151.11(11) . . ?
N4 Cu OW1 103.94(12) . . ?
N2 Cu OW1 102.55(11) . . ?
N1 Cu OW1 104.48(11) . . ?
N3 Cu OW1 104.41(10) . . ?
O4 N12 C23 117.5(3) . . ?
O12 Cl1 O14 110.02(18) . . ?
O12 Cl1 O11 110.61(18) . . ?
O14 Cl1 O11 110.31(19) . . ?
O12 Cl1 O13 109.23(18) . . ?
O14 Cl1 O13 109.86(19) . . ?
O11 Cl1 O13 106.75(18) . . ?
O2 N7 C16 118.1(3) . . ?
O24 Cl2 O22 108.9(2) . . ?
O24 Cl2 O21 112.9(3) . . ?
O22 Cl2 O21 108.9(2) . . ?
O24 Cl2 O23 109.5(3) . . ?
O22 Cl2 O23 107.0(2) . . ?
O21 Cl2 O23 109.3(2) . . ?
C13 N6 C15 120.9(3) . . ?
C13 N6 C14 120.5(3) . . ?
C15 N6 C14 118.6(3) . . ?
C13 N5 C12 121.4(3) . . ?
C9 N4 C7 110.2(3) . . ?
C9 N4 C8 111.5(3) . . ?
C7 N4 C8 110.2(3) . . ?
C9 N4 Cu 101.3(2) . . ?
C7 N4 Cu 108.2(2) . . ?
C8 N4 Cu 115.1(2) . . ?
C3 N2 C4 111.6(3) . . ?
C3 N2 C2 109.8(3) . . ?
C4 N2 C2 110.0(3) . . ?
C3 N2 Cu 116.7(2) . . ?
C4 N2 Cu 100.50(19) . . ?
C2 N2 Cu 107.76(19) . . ?
C20 N10 C19 121.8(3) . . ?
C10 N1 C18 110.9(3) . . ?
C10 N1 C1 111.6(3) . . ?
C18 N1 C1 112.4(3) . . ?
C10 N1 Cu 107.7(2) . . ?
C18 N1 Cu 112.42(19) . . ?
C1 N1 Cu 101.41(18) . . ?
C13 N9 C17 118.3(3) . . ?
C20 N11 C22 121.0(3) . . ?
C20 N11 C21 120.2(3) . . ?
C22 N11 C21 118.8(3) . . ?
C20 N14 C24 118.4(3) . . ?
C11 N3 C6 112.2(3) . . ?
C11 N3 C5 110.5(2) . . ?
C6 N3 C5 112.0(3) . . ?
C11 N3 Cu 113.5(2) . . ?
C6 N3 Cu 101.43(19) . . ?
C5 N3 Cu 106.91(19) . . ?
N10 C20 N14 118.4(3) . . ?
N10 C20 N11 117.3(3) . . ?
N14 C20 N11 124.3(3) . . ?
N12 C23 C24 127.5(3) . . ?
N12 C23 C22 114.0(3) . . ?
C24 C23 C22 118.5(3) . . ?
N9 C13 N5 118.3(3) . . ?
N9 C13 N6 124.9(3) . . ?
N5 C13 N6 116.7(3) . . ?
O3 C22 N11 120.2(3) . . ?
O3 C22 C23 124.1(3) . . ?
N11 C22 C23 115.7(3) . . ?
N3 C11 C12 113.9(3) . . ?
N1 C18 C19 114.4(3) . . ?
N2 C2 C1 109.6(3) . . ?
N8 C17 N9 117.9(3) . . ?
N8 C17 C16 120.4(3) . . ?
N9 C17 C16 121.6(3) . . ?
N7 C16 C17 126.7(3) . . ?
N7 C16 C15 114.4(3) . . ?
C17 C16 C15 118.7(3) . . ?
N3 C5 C4 110.2(3) . . ?
N1 C1 C2 109.7(3) . . ?
O1 C15 N6 120.2(3) . . ?
O1 C15 C16 124.4(3) . . ?
N6 C15 C16 115.4(3) . . ?
N13 C24 N14 117.9(3) . . ?
N13 C24 C23 120.3(3) . . ?
N14 C24 C23 121.8(3) . . ?
N2 C4 C5 110.2(3) . . ?
N10 C19 C18 109.8(3) . . ?
N1 C10 C9 110.1(3) . . ?
N4 C7 C6 109.7(3) . . ?
N4 C9 C10 109.8(3) . . ?
N5 C12 C11 109.5(3) . . ?
N3 C6 C7 109.9(3) . . ?

_refine_diff_density_max         1.381
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.114


# start Validation Reply Form
_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact Ow4 ..Ow13 . 2.39 Ang.
RESPONSE: This distance correspond to a hydrogen bond contact. All attempts carried out to localize and refine the hydrogen atoms for these water molecules were unsuccesful
;
_vrf_PLAT043_shelx               
;
PROBLEM: Calculated and Reported Mol. Weight Differ by .. 23.25 Check
RESPONSE: The water hydrogens have not been localized in the Fourier density map
;
_vrf_PLAT306_shelx               
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow11 Check
RESPONSE: The water hydrogens have not been localized in the Fourier density map
;
# end Validation Reply Form
#===END
