# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_jcmxra
_database_code_depnum_ccdc_archive 'CCDC 2099919'
loop_
_audit_author_name
_audit_author_address
'Jan L. Wikaira'
;University of Canterbury
New Zealand
;
_audit_update_record             
;
2021-07-28 deposited with the CCDC.	2022-02-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H14 Cl4 Cu N5 O10'
_chemical_formula_weight         641.66

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'
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'
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'

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

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

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

_cell_length_a                   21.3908(5)
_cell_length_b                   6.83271(13)
_cell_length_c                   16.4846(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.288(2)
_cell_angle_gamma                90
_cell_volume                     2377.77(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    10061
_cell_measurement_theta_min      4.1800
_cell_measurement_theta_max      76.6050

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_F_000             1288
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.083
_exptl_absorpt_coefficient_mu    6.020
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_T_max  0.724
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23688
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.188
_diffrn_reflns_theta_max         76.846
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4963
_reflns_number_gt                4233
_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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0860P)²+9.6681P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4963
_refine_ls_number_parameters     371
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0593
_refine_ls_wR_factor_ref         0.1720
_refine_ls_wR_factor_gt          0.1634
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.13222(2) -0.00384(6) 0.40769(3) 0.01089(16) Uani 1 1 d . . . . .
Cl13 Cl 0.25923(7) 0.3124(2) 0.63449(9) 0.0572(4) Uani 1 1 d . . . . .
Cl23 Cl 0.27316(7) -0.3042(2) 0.26218(10) 0.0573(4) Uani 1 1 d . . . . .
O24 O 0.19867(12) -0.0249(4) 0.34058(16) 0.0191(5) Uani 1 1 d . . . . .
O14 O 0.19548(12) 0.0021(4) 0.52719(16) 0.0178(5) Uani 1 1 d . . . . .
N3 N 0.12943(12) 0.2928(4) 0.40401(16) 0.0115(5) Uani 1 1 d . . . . .
N1 N 0.05336(14) -0.0023(4) 0.46236(18) 0.0118(5) Uani 1 1 d . . . . .
N2 N 0.12817(12) -0.3020(4) 0.40434(16) 0.0120(5) Uani 1 1 d . . . . .
C25 C 0.2826(2) 0.1976(7) 0.3871(3) 0.0343(10) Uani 1 1 d . . . . .
H25 H 0.257420 0.278615 0.413598 0.041 Uiso 1 1 calc R U . . .
C14 C 0.25312(18) -0.0305(6) 0.5513(2) 0.0211(8) Uani 1 1 d . . . . .
C4 C 0.12816(16) -0.4032(5) 0.3346(2) 0.0143(6) Uani 1 1 d . . . . .
H4 H 0.127847 -0.336026 0.285474 0.017 Uiso 1 1 calc R U . . .
C6 C 0.12914(15) 0.3940(5) 0.4737(2) 0.0132(6) Uani 1 1 d . . . . .
H6 H 0.129493 0.326915 0.522826 0.016 Uiso 1 1 calc R U . . .
C24 C 0.25616(18) 0.0267(6) 0.3466(2) 0.0213(8) Uani 1 1 d . . . . .
C5 C 0.12860(16) 0.3939(5) 0.3345(2) 0.0144(6) Uani 1 1 d . . . . .
H5 H 0.128317 0.327105 0.285262 0.017 Uiso 1 1 calc R U . . .
C15 C 0.2858(2) -0.2005(7) 0.5289(3) 0.0358(10) Uani 1 1 d . . . . .
H15 H 0.263687 -0.293589 0.494406 0.043 Uiso 1 1 calc R U . . .
C3 C 0.12832(15) -0.4035(5) 0.4737(2) 0.0133(6) Uani 1 1 d . . . . .
H3 H 0.127874 -0.336849 0.522747 0.016 Uiso 1 1 calc R U . . .
C23 C 0.2995(2) -0.0899(7) 0.3101(3) 0.0328(10) Uani 1 1 d . . . . .
C13 C 0.2930(2) 0.1015(7) 0.6035(3) 0.0307(9) Uani 1 1 d . . . . .
C2 C -0.00464(17) -0.0036(5) 0.4176(2) 0.0142(7) Uani 1 1 d . . . . .
H2 H -0.009226 -0.006004 0.360582 0.017 Uiso 1 1 calc R U . . .
C1 C 0.05799(17) 0.0015(5) 0.5446(2) 0.0140(7) Uani 1 1 d . . . . .
H1 H 0.097880 0.002747 0.576862 0.017 Uiso 1 1 calc R U . . .
C26 C 0.3444(2) 0.2444(9) 0.3876(5) 0.0611(17) Uani 1 1 d . . . . .
H26 H 0.360738 0.358247 0.413773 0.073 Uiso 1 1 calc R U . . .
N11 N 0.38188(19) -0.0988(9) 0.6070(3) 0.0602(14) Uani 1 1 d . . . . .
H11 H 0.421282 -0.121333 0.624585 0.072 Uiso 1 1 calc R U . . .
C12 C 0.3552(2) 0.0658(9) 0.6299(4) 0.0471(13) Uani 1 1 d . . . . .
H12 H 0.379450 0.155264 0.664048 0.057 Uiso 1 1 calc R U . . .
C16 C 0.3480(2) -0.2281(10) 0.5571(4) 0.0566(15) Uani 1 1 d . . . . .
H16 H 0.367849 -0.339797 0.541388 0.068 Uiso 1 1 calc R U . . .
N21 N 0.3823(2) 0.1290(9) 0.3508(4) 0.0688(17) Uani 1 1 d . . . . .
H21 H 0.421134 0.162557 0.351465 0.083 Uiso 1 1 calc R U . . .
C22 C 0.3610(2) -0.0356(10) 0.3136(4) 0.0533(16) Uani 1 1 d . . . . .
H22 H 0.388455 -0.114666 0.289743 0.064 Uiso 1 1 calc R U . . .
Cl1 Cl 0.06737(4) -0.00585(11) 0.17738(5) 0.0147(2) Uani 1 1 d . . . . .
O1 O 0.05773(13) -0.0076(4) 0.26259(16) 0.0217(6) Uani 1 1 d . . . . .
O2 O 0.10419(14) -0.1747(4) 0.16216(16) 0.0253(6) Uani 1 1 d . . . . .
O3 O 0.10133(15) 0.1683(4) 0.16241(16) 0.0266(6) Uani 1 1 d . . . . .
O4 O 0.00778(15) -0.0099(5) 0.1237(2) 0.0395(8) Uani 1 1 d . . . . .
Cl2 Cl 0.49941(13) -0.0673(9) 0.8095(3) 0.0968(17) Uani 0.517(4) 1 d . . P A 1
O5 O 0.5000(3) -0.134(2) 0.7295(4) 0.083(4) Uani 0.517(4) 1 d . . P A 1
O6 O 0.5012(4) -0.201(3) 0.8649(6) 0.086(5) Uani 0.517(4) 1 d . . P A 1
O7 O 0.5537(4) -0.019(2) 0.8337(12) 0.140(7) Uani 0.517(4) 1 d . . P A 1
O8 O 0.4436(4) -0.022(2) 0.8157(12) 0.146(8) Uani 0.517(4) 1 d . . P A 1
Cl2A Cl 0.49975(14) -0.2078(11) 0.9474(3) 0.123(3) Uani 0.483(4) 1 d . . P A 2
O5A O 0.4980(3) -0.3119(16) 1.0338(6) 0.066(3) Uani 0.483(4) 1 d . . P A 2
O6A O 0.5009(8) -0.342(3) 0.8653(13) 0.122(6) Uani 0.483(4) 1 d . U P A 2
O7A O 0.5536(5) -0.124(2) 0.9597(10) 0.100(4) Uani 0.483(4) 1 d . . P A 2
O8A O 0.4439(5) -0.127(2) 0.9366(9) 0.095(4) Uani 0.483(4) 1 d . . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O24 1.942(2) . ?
Cu1 N3 2.028(3) . ?
Cu1 N1 2.037(3) . ?
Cu1 N2 2.040(3) . ?
Cu1 O14 2.203(3) . ?
Cl13 C13 1.727(5) . ?
Cl23 C23 1.716(5) . ?
O24 C24 1.268(5) . ?
O14 C14 1.253(5) . ?
N3 C5 1.336(4) . ?
N3 C6 1.341(4) . ?
N1 C2 1.337(5) . ?
N1 C1 1.343(4) . ?
N2 C3 1.336(4) . ?
N2 C4 1.341(4) . ?
C25 C26 1.359(6) . ?
C25 C24 1.417(6) . ?
C25 H25 0.9300 . ?
C14 C13 1.430(6) . ?
C14 C15 1.434(6) . ?
C4 C5 1.387(5) 1_545 ?
C4 H4 0.9300 . ?
C6 C3 1.384(5) 1_565 ?
C6 H6 0.9300 . ?
C24 C23 1.427(6) . ?
C5 H5 0.9300 . ?
C15 C16 1.351(7) . ?
C15 H15 0.9300 . ?
C3 H3 0.9300 . ?
C23 C22 1.359(7) . ?
C13 C12 1.353(7) . ?
C2 C1 1.385(5) 3_556 ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?
C26 N21 1.343(9) . ?
C26 H26 0.9300 . ?
N11 C16 1.338(8) . ?
N11 C12 1.343(9) . ?
N11 H11 0.8600 . ?
C12 H12 0.9300 . ?
C16 H16 0.9300 . ?
N21 C22 1.326(9) . ?
N21 H21 0.8600 . ?
C22 H22 0.9300 . ?
Cl1 O4 1.430(3) . ?
Cl1 O3 1.436(3) . ?
Cl1 O2 1.441(3) . ?
Cl1 O1 1.452(3) . ?
Cl2 O7 1.212(10) . ?
Cl2 O8 1.253(9) . ?
Cl2 O6 1.286(17) . ?
Cl2 O5 1.396(9) . ?
O6 O7 1.80(2) . ?
Cl2A O7A 1.273(13) . ?
Cl2A O8A 1.300(11) . ?
Cl2A O5A 1.598(10) . ?
Cl2A O6A 1.64(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
O24 Cu1 N3 94.46(11) . . ?
O24 Cu1 N1 170.70(11) . . ?
N3 Cu1 N1 89.17(10) . . ?
O24 Cu1 N2 86.69(11) . . ?
N3 Cu1 N2 175.16(11) . . ?
N1 Cu1 N2 89.00(10) . . ?
O24 Cu1 O14 96.34(11) . . ?
N3 Cu1 O14 91.11(10) . . ?
N1 Cu1 O14 92.14(11) . . ?
N2 Cu1 O14 93.43(10) . . ?
C24 O24 Cu1 136.4(3) . . ?
C14 O14 Cu1 135.3(2) . . ?
C5 N3 C6 117.8(3) . . ?
C5 N3 Cu1 122.6(2) . . ?
C6 N3 Cu1 119.6(2) . . ?
C2 N1 C1 117.8(3) . . ?
C2 N1 Cu1 121.1(2) . . ?
C1 N1 Cu1 121.0(2) . . ?
C3 N2 C4 117.7(3) . . ?
C3 N2 Cu1 120.1(2) . . ?
C4 N2 Cu1 122.1(2) . . ?
C26 C25 C24 120.8(5) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
O14 C14 C13 122.7(4) . . ?
O14 C14 C15 123.9(4) . . ?
C13 C14 C15 113.4(4) . . ?
N2 C4 C5 121.2(3) . 1_545 ?
N2 C4 H4 119.4 . . ?
C5 C4 H4 119.4 1_545 . ?
N3 C6 C3 121.1(3) . 1_565 ?
N3 C6 H6 119.4 . . ?
C3 C6 H6 119.4 1_565 . ?
O24 C24 C25 125.1(4) . . ?
O24 C24 C23 120.0(4) . . ?
C25 C24 C23 114.9(4) . . ?
N3 C5 C4 121.0(3) . 1_565 ?
N3 C5 H5 119.5 . . ?
C4 C5 H5 119.5 1_565 . ?
C16 C15 C14 121.3(5) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
N2 C3 C6 121.1(3) . 1_545 ?
N2 C3 H3 119.4 . . ?
C6 C3 H3 119.4 1_545 . ?
C22 C23 C24 121.4(5) . . ?
C22 C23 Cl23 119.8(4) . . ?
C24 C23 Cl23 118.9(3) . . ?
C12 C13 C14 122.7(5) . . ?
C12 C13 Cl13 119.5(4) . . ?
C14 C13 Cl13 117.8(3) . . ?
N1 C2 C1 120.7(3) . 3_556 ?
N1 C2 H2 119.7 . . ?
C1 C2 H2 119.7 3_556 . ?
N1 C1 C2 121.5(3) . 3_556 ?
N1 C1 H1 119.3 . . ?
C2 C1 H1 119.3 3_556 . ?
N21 C26 C25 121.1(6) . . ?
N21 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C16 N11 C12 120.9(4) . . ?
C16 N11 H11 119.5 . . ?
C12 N11 H11 119.5 . . ?
N11 C12 C13 120.0(5) . . ?
N11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
N11 C16 C15 121.7(6) . . ?
N11 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C22 N21 C26 121.3(5) . . ?
C22 N21 H21 119.3 . . ?
C26 N21 H21 119.3 . . ?
N21 C22 C23 120.6(5) . . ?
N21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
O4 Cl1 O3 109.6(2) . . ?
O4 Cl1 O2 109.55(19) . . ?
O3 Cl1 O2 109.12(18) . . ?
O4 Cl1 O1 110.27(19) . . ?
O3 Cl1 O1 109.13(15) . . ?
O2 Cl1 O1 109.19(15) . . ?
O7 Cl2 O8 141.5(10) . . ?
O7 Cl2 O6 92.4(11) . . ?
O8 Cl2 O6 91.9(11) . . ?
O7 Cl2 O5 104.2(9) . . ?
O8 Cl2 O5 108.1(8) . . ?
O6 Cl2 O5 115.9(9) . . ?
Cl2 O6 O7 42.2(7) . . ?
Cl2 O7 O6 45.4(7) . . ?
O7A Cl2A O8A 128.2(11) . . ?
O7A Cl2A O5A 102.1(8) . . ?
O8A Cl2A O5A 99.0(7) . . ?
O7A Cl2A O6A 104.5(9) . . ?
O8A Cl2A O6A 105.0(9) . . ?
O5A Cl2A O6A 119.5(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O14 C14 C13 130.8(3) . . . . ?
Cu1 O14 C14 C15 -48.5(6) . . . . ?
C3 N2 C4 C5 -0.3(5) . . . 1_545 ?
Cu1 N2 C4 C5 176.7(2) . . . 1_545 ?
C5 N3 C6 C3 -0.3(5) . . . 1_565 ?
Cu1 N3 C6 C3 178.9(2) . . . 1_565 ?
Cu1 O24 C24 C25 -33.1(6) . . . . ?
Cu1 O24 C24 C23 147.7(3) . . . . ?
C26 C25 C24 O24 -177.5(5) . . . . ?
C26 C25 C24 C23 1.8(7) . . . . ?
C6 N3 C5 C4 0.7(5) . . . 1_565 ?
Cu1 N3 C5 C4 -178.5(2) . . . 1_565 ?
O14 C14 C15 C16 -179.7(5) . . . . ?
C13 C14 C15 C16 0.9(7) . . . . ?
C4 N2 C3 C6 0.7(5) . . . 1_545 ?
Cu1 N2 C3 C6 -176.4(2) . . . 1_545 ?
O24 C24 C23 C22 178.2(4) . . . . ?
C25 C24 C23 C22 -1.1(6) . . . . ?
O24 C24 C23 Cl23 -2.6(5) . . . . ?
C25 C24 C23 Cl23 178.0(3) . . . . ?
O14 C14 C13 C12 179.5(4) . . . . ?
C15 C14 C13 C12 -1.1(6) . . . . ?
O14 C14 C13 Cl13 0.5(5) . . . . ?
C15 C14 C13 Cl13 179.9(3) . . . . ?
C1 N1 C2 C1 -0.1(5) . . . 3_556 ?
Cu1 N1 C2 C1 -179.7(2) . . . 3_556 ?
C2 N1 C1 C2 0.1(5) . . . 3_556 ?
Cu1 N1 C1 C2 179.7(2) . . . 3_556 ?
C24 C25 C26 N21 -1.0(9) . . . . ?
C16 N11 C12 C13 0.9(9) . . . . ?
C14 C13 C12 N11 0.3(8) . . . . ?
Cl13 C13 C12 N11 179.3(4) . . . . ?
C12 N11 C16 C15 -1.1(10) . . . . ?
C14 C15 C16 N11 0.1(9) . . . . ?
C25 C26 N21 C22 -0.8(11) . . . . ?
C26 N21 C22 C23 1.5(10) . . . . ?
C24 C23 C22 N21 -0.5(8) . . . . ?
Cl23 C23 C22 N21 -179.6(5) . . . . ?
O8 Cl2 O6 O7 -141.7(10) . . . . ?
O5 Cl2 O6 O7 107.1(7) . . . . ?
O8 Cl2 O7 O6 96(2) . . . . ?
O5 Cl2 O7 O6 -117.5(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N11 H11 O5 0.86 2.21 2.979(8) 148.4 . yes
N11 H11 O5A 0.86 2.44 2.994(9) 123.1 4 yes
N11 H11 O6A 0.86 2.52 3.034(18) 119.2 2_656 yes
N21 H21 O5 0.86 2.32 3.028(8) 139.5 3_656 yes
N21 H21 O8 0.86 2.59 3.086(13) 117.7 4_565 yes
N21 H21 O5A 0.86 2.35 2.961(9) 127.8 2_656 yes

_refine_diff_density_max         1.917
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.129


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

data_jcmaa
_database_code_depnum_ccdc_archive 'CCDC 2099944'
loop_
_audit_author_name
_audit_author_address
'Louise N. Dawe'
;Wilfrid Laurier University
Canada
;
_audit_update_record             
;
2021-07-28 deposited with the CCDC.	2022-02-24 downloaded from the CCDC.
;
_audit_creation_date             2021-02-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H14 Br2 Cu N5 O2, 2(Cl O4)'
_chemical_formula_sum            'C16 H14 Br2 Cl2 Cu N5 O10'
_chemical_formula_weight         730.58
_chemical_melting_point          ?

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'
Br Br -0.2901 2.4595 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_symmetry_space_group_name_H-M_alt 'P 1 21/c 1'
_cell_length_a                   21.4129(7)
_cell_length_b                   6.8466(2)
_cell_length_c                   16.6158(6)
_cell_angle_alpha                90
_cell_angle_beta                 99.172(3)
_cell_angle_gamma                90
_cell_volume                     2404.83(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6490
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      28.7500
_cell_measurement_theta_min      3.5190
_cell_oxdiff_angle_alpha         89.986(3)
_cell_oxdiff_angle_beta          99.114(3)
_cell_oxdiff_angle_gamma         90.029(3)
_cell_oxdiff_length_a            21.4211(8)
_cell_oxdiff_length_b            6.8510(3)
_cell_oxdiff_length_c            16.6064(8)
_cell_oxdiff_measurement_reflns_used 4876
_cell_oxdiff_volume              2406.33(17)
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.516
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.018
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0213
-3 -4 2 0.0723
3 1 1 0.0514
3 0 -1 0.0460
-3 -4 -1 0.0968
3 0 2 0.0674
2 -2 5 0.0813
0 1 -5 0.0552
-3 2 2 0.0648
3 -2 1 0.0742
1 0 0 0.0382
-1 0 5 0.0865

_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.06
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.5003 -0.0001 -0.0002 0.0156 0.0025 -0.0058
-2.5012 -4.0020 2.0018 0.2200 -0.0583 0.3634
2.5009 1.0011 1.0014 -0.1131 -0.0597 -0.0667
2.5019 0.0001 -0.9999 -0.0780 0.0307 0.0272
-2.5001 -4.0027 -1.0006 0.2195 0.0714 0.3584
2.5008 0.0008 2.0025 -0.0774 -0.0990 0.0322
2.0000 -1.9996 5.0052 0.0096 -0.2184 0.2258
-0.4988 0.9992 -5.0044 -0.0208 0.2148 -0.1113
-2.5027 2.0012 2.0002 0.0072 -0.0818 -0.2200
2.5017 -2.0005 1.0022 -0.0066 -0.0479 0.2250
0.5003 0.0001 0.0002 -0.0156 -0.0025 0.0058
-1.0023 0.0011 5.0037 0.0320 -0.2112 -0.0033

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14769
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.308
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00 100.00   1.00   32.79    --   11.05 178.00-120.00   65
  2  ω    -84.00  13.00   1.00   32.79    --  -11.98 -57.00 -90.00   97
  3  ω     -5.00  29.00   1.00   32.79    --  -11.98 -99.00 120.00   34
  4  ω    -85.00 -56.00   1.00   32.79    --  -11.98 -37.00-120.00   29
  5  ω     -7.00  41.00   1.00   32.79    --  -11.98  37.00-120.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0310892000
_diffrn_orient_matrix_UB_12      -0.0354658000
_diffrn_orient_matrix_UB_13      0.0001786000
_diffrn_orient_matrix_UB_21      -0.0049890000
_diffrn_orient_matrix_UB_22      -0.0039223000
_diffrn_orient_matrix_UB_23      -0.0432101000
_diffrn_orient_matrix_UB_31      0.0115460000
_diffrn_orient_matrix_UB_32      -0.0971675000
_diffrn_orient_matrix_UB_33      0.0016839000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3896
_reflns_number_total             4578
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.652
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4578
_refine_ls_number_restraints     202
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0634
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0351P)²+33.6168P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1479
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Shared sites
{C24, C24A}
{C14, C14A}
3. Restrained distances
 Br1A-C13A \\sim Br1-C13
 with sigma of 0.02
 C13A-C12A \\sim C14A-C13A \\sim C15A-C14A \\sim C16A-C15A \\sim C13-C12 \\sim
C14-C13 \\sim C15-C14 ~
 C16-C15
 with sigma of 0.02
 N11-C16 \\sim N11A-C16A \\sim N11-C12 \\sim N11A-C12A
 with sigma of 0.02
 Br2A-C23A \\sim Br2-C23
 with sigma of 0.02
 C24A-C23A \\sim C25A-C24A \\sim C26-C25 \\sim C23-C22 \\sim C23A-C22A \\sim
C24-C23 \\sim C25-C24 ~
 C26A-C25A
 with sigma of 0.02
 N21A-C22A \\sim N21-C22 \\sim N21A-C26A \\sim N21-C26
 with sigma of 0.02
 O24-C24A \\sim O24-C24
 with sigma of 0.02
 O14-C14 \\sim O14-C14A
 with sigma of 0.02
 O5-O6 \\sim O5-O7 \\sim O6-O8 \\sim O7-O8 \\sim O5A-O6A \\sim O5A-O7A \\sim
O6A-O8A \\sim O7A-O8A
 with sigma of 0.04
 Cl2-O5 \\sim Cl2-O6 \\sim Cl2-O7 \\sim Cl2-O8 \\sim Cl2A-O5A \\sim Cl2A-O6A
\\sim Cl2A-O7A \\sim Cl2A-O8A
 with sigma of 0.02
 O9-O10 \\sim O9-O12 \\sim O10-O11 \\sim O10-O12 \\sim O11-O12 \\sim O9A-O10A
\\sim O9A-O12A \\sim O10A-
 O11A \\sim O10A-O12A \\sim O11A-O12A
 with sigma of 0.04
 Cl3-O9 \\sim Cl3-O10 \\sim Cl3-O11 \\sim Cl3-O12 \\sim Cl3A-O9A \\sim
Cl3A-O10A \\sim Cl3A-O11A ~
 Cl3A-O12A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Br1A) = Uanis(Br1)
Uanis(C12A) = Uanis(C13A) = Uanis(C14A) = Uanis(C15) = Uanis(C16) = Uanis(N11)
= Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15A) = Uanis(C16A) = Uanis(N11A)
Uanis(Br2A) = Uanis(Br2)
Uanis(C23A) = Uanis(C24A) = Uanis(C25A) = Uanis(C26) = Uanis(N21) = Uanis(C22)
= Uanis(C23) = Uanis(C22A) = Uanis(C24) = Uanis(C25) = Uanis(C26A) = Uanis(N21A)
Uanis(O9A) = Uanis(O9) = Uanis(O10A) = Uanis(O10) = Uanis(O11A) = Uanis(O11) =
Uanis(O12A) = Uanis(O12) = Uanis(O6A) = Uanis(O6) = Uanis(O8A) = Uanis(O7) =
Uanis(O7A) = Uanis(O5) = Uanis(O5A) = Uanis(O8)
Uanis(Cl3) = Uanis(Cl3A) = Uanis(Cl2) = Uanis(Cl2A)
5. Others
 1*[Sof(Cl2)+Sof(O5)+Sof(O6)+Sof(O7)+Sof(O8)]+1*[Sof(Cl2A)+Sof(O5A)+Sof(O6A)+
 Sof(O7A)+Sof(O8A)]+1*[Sof(Cl3)+Sof(O9)+Sof(O10)+Sof(O11)+Sof(O12)]+1*
 [Sof(Cl3A)+Sof(O9A)+Sof(O10A)+Sof(O11A)+Sof(O12A)]=1 with esd of 0.001
 Sof(Br1A)=Sof(N11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(C14A)=
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=1-FVAR(1)
 Sof(Br1)=Sof(N11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(C14)=Sof(C15)=
 Sof(H15)=Sof(C16)=Sof(H16)=FVAR(1)
 Sof(Br2A)=Sof(N21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(C24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=1-FVAR(2)
 Sof(Br2)=Sof(N21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=FVAR(2)
 Sof(Cl2)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=FVAR(3)
 Sof(Cl2A)=Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(O8A)=FVAR(4)
 Sof(Cl3)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=FVAR(5)
 Sof(Cl3A)=Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=FVAR(6)
6.a Aromatic/amide H refined with riding coordinates:
 N11(H11), N21(H21), N11A(H11A), N21A(H21A), C1(H1), C2(H2), C4(H4), C5(H5),
 C7(H7), C8(H8), C12(H12), C15(H15), C16(H16), C22(H22), C25(H25), C26(H26),
 C12A(H12A), C15A(H15A), C16A(H16A), C22A(H22A), C25A(H25A), C26A(H26A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
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
Br1 Br 0.2150(3) 0.2036(12) 0.2308(6) 0.0359(8) Uani 0.438(9) 1 d D . P A 1
Br2 Br 0.2327(4) 0.8130(14) -0.1316(6) 0.0389(8) Uani 0.328(15) 1 d D . P B 1
Br1A Br 0.2300(3) 0.1676(9) 0.2388(4) 0.0359(8) Uani 0.562(9) 1 d D . P A 2
Br2A Br 0.2486(3) 0.8327(6) -0.1398(3) 0.0389(8) Uani 0.672(15) 1 d D . P B 2
Cu1 Cu 0.36783(3) 0.49546(10) 0.09163(4) 0.00820(18) Uani 1 1 d . . . . .
O14 O 0.30044(19) 0.4739(6) 0.1564(2) 0.0143(9) Uani 1 1 d D . . . .
O24 O 0.30507(19) 0.5004(6) -0.0269(2) 0.0145(9) Uani 1 1 d D . . . .
N1 N 0.4467(2) 0.4975(7) 0.0373(3) 0.0102(10) Uani 1 1 d . . . . .
N3 N 0.3719(2) 0.7921(7) 0.0961(3) 0.0081(10) Uani 1 1 d . . . . .
N6 N 0.3722(2) 1.1971(7) 0.0959(3) 0.0090(10) Uani 1 1 d . . . . .
N11 N 0.1166(6) 0.665(2) 0.1229(9) 0.0244(9) Uani 0.438(9) 1 d D . P A 1
H11 H 0.078326 0.707786 0.117078 0.029 Uiso 0.438(9) 1 calc R U P A 1
N21 N 0.1187(9) 0.364(3) -0.0857(13) 0.0238(8) Uani 0.328(15) 1 d D . P B 1
H21 H 0.079411 0.332814 -0.097769 0.029 Uiso 0.328(15) 1 calc R U P B 1
N11A N 0.1185(5) 0.6241(17) 0.1540(7) 0.0244(9) Uani 0.562(9) 1 d D . P A 2
H11A H 0.079928 0.656100 0.156220 0.029 Uiso 0.562(9) 1 calc R U P A 2
N21A N 0.1189(4) 0.4183(16) -0.1083(6) 0.0238(8) Uani 0.672(15) 1 d D . P B 2
H21A H 0.079113 0.402000 -0.125271 0.029 Uiso 0.672(15) 1 calc R U P B 2
C1 C 0.5042(3) 0.4999(9) 0.0815(4) 0.0120(12) Uani 1 1 d . . . . .
H1 H 0.508630 0.500622 0.138074 0.014 Uiso 1 1 calc R U . . .
C2 C 0.4425(3) 0.4989(9) -0.0441(4) 0.0126(12) Uani 1 1 d . . . . .
H2 H 0.402711 0.498920 -0.076219 0.015 Uiso 1 1 calc R U . . .
C4 C 0.3724(3) 0.8936(9) 0.0274(4) 0.0116(12) Uani 1 1 d . . . . .
H4 H 0.372315 0.826878 -0.021385 0.014 Uiso 1 1 calc R U . . .
C5 C 0.3730(3) 1.0948(9) 0.0273(3) 0.0110(12) Uani 1 1 d . . . . .
H5 H 0.374026 1.160960 -0.021323 0.013 Uiso 1 1 calc R U . . .
C7 C 0.3723(3) 1.0961(9) 0.1644(4) 0.0128(12) Uani 1 1 d . . . . .
H7 H 0.372544 1.162967 0.213202 0.015 Uiso 1 1 calc R U . . .
C8 C 0.3719(3) 0.8925(9) 0.1648(4) 0.0134(12) Uani 1 1 d . . . . .
H8 H 0.371629 0.826043 0.213544 0.016 Uiso 1 1 calc R U . . .
C12 C 0.1309(7) 0.501(3) 0.1659(11) 0.0244(9) Uani 0.438(9) 1 d D . P A 1
H12 H 0.099878 0.433498 0.187733 0.029 Uiso 0.438(9) 1 calc R U P A 1
C13 C 0.1927(6) 0.433(3) 0.1772(14) 0.0244(9) Uani 0.438(9) 1 d D . P A 1
C14 C 0.2428(3) 0.5305(10) 0.1491(4) 0.0244(9) Uani 0.438(9) 1 d D . P A 1
C15 C 0.2214(9) 0.698(3) 0.1020(13) 0.0244(9) Uani 0.438(9) 1 d D . P A 1
H15 H 0.251155 0.766904 0.078262 0.029 Uiso 0.438(9) 1 calc R U P A 1
C16 C 0.1594(7) 0.767(3) 0.0885(11) 0.0244(9) Uani 0.438(9) 1 d D . P A 1
H16 H 0.148059 0.877490 0.057190 0.029 Uiso 0.438(9) 1 calc R U P A 1
C22 C 0.1376(9) 0.529(4) -0.1171(15) 0.0238(8) Uani 0.328(15) 1 d D . P B 1
H22 H 0.109407 0.605578 -0.151987 0.029 Uiso 0.328(15) 1 calc R U P B 1
C23 C 0.2002(7) 0.583(3) -0.0964(17) 0.0238(8) Uani 0.328(15) 1 d D . P B 1
C24 C 0.2463(3) 0.4684(10) -0.0494(4) 0.0238(8) Uani 0.328(15) 1 d D . P B 1
C25 C 0.2199(12) 0.301(4) -0.019(2) 0.0238(8) Uani 0.328(15) 1 d D . P B 1
H25 H 0.246844 0.221050 0.016637 0.029 Uiso 0.328(15) 1 calc R U P B 1
C26 C 0.1568(9) 0.245(4) -0.0368(16) 0.0238(8) Uani 0.328(15) 1 d D . P B 1
H26 H 0.141917 0.131042 -0.016053 0.029 Uiso 0.328(15) 1 calc R U P B 1
C12A C 0.1413(5) 0.456(2) 0.1881(9) 0.0244(9) Uani 0.562(9) 1 d D . P A 2
H12A H 0.115093 0.373110 0.212113 0.029 Uiso 0.562(9) 1 calc R U P A 2
C13A C 0.2036(5) 0.404(2) 0.1877(11) 0.0244(9) Uani 0.562(9) 1 d D . P A 2
C14A C 0.2428(3) 0.5305(10) 0.1491(4) 0.0244(9) Uani 0.562(9) 1 d D . P A 2
C15A C 0.2171(7) 0.705(2) 0.1138(10) 0.0244(9) Uani 0.562(9) 1 d D . P A 2
H15A H 0.241822 0.791204 0.089157 0.029 Uiso 0.562(9) 1 calc R U P A 2
C16A C 0.1547(6) 0.745(2) 0.1164(9) 0.0244(9) Uani 0.562(9) 1 d D . P A 2
H16A H 0.136765 0.857628 0.091605 0.029 Uiso 0.562(9) 1 calc R U P A 2
C22A C 0.1471(5) 0.5786(18) -0.1305(7) 0.0238(8) Uani 0.672(15) 1 d D . P B 2
H22A H 0.124079 0.671051 -0.163842 0.029 Uiso 0.672(15) 1 calc R U P B 2
C23A C 0.2110(4) 0.6063(18) -0.1034(8) 0.0238(8) Uani 0.672(15) 1 d D . P B 2
C24A C 0.2463(3) 0.4684(10) -0.0494(4) 0.0238(8) Uani 0.672(15) 1 d D . P B 2
C25A C 0.2137(6) 0.301(2) -0.0299(10) 0.0238(8) Uani 0.672(15) 1 d D . P B 2
H25A H 0.234629 0.204185 0.003235 0.029 Uiso 0.672(15) 1 calc R U P B 2
C26A C 0.1504(5) 0.2826(18) -0.0607(7) 0.0238(8) Uani 0.672(15) 1 d D . P B 2
H26A H 0.128941 0.171689 -0.047894 0.029 Uiso 0.672(15) 1 calc R U P B 2
Cl1 Cl 0.43275(7) 0.4921(2) 0.32171(8) 0.0131(3) Uani 1 1 d . . . . .
O1 O 0.4421(2) 0.4896(7) 0.2370(3) 0.0219(10) Uani 1 1 d . . . . .
O2 O 0.4029(3) 0.6721(7) 0.3378(3) 0.0290(12) Uani 1 1 d . . . . .
O3 O 0.3927(2) 0.3322(7) 0.3369(3) 0.0266(11) Uani 1 1 d . . . . .
O4 O 0.4923(2) 0.4760(10) 0.3743(3) 0.0416(15) Uani 1 1 d . . . . .
Cl2 Cl -0.0008(3) 0.7656(12) -0.0495(4) 0.0452(13) Uani 0.363(5) 1 d D . P C 3
O5 O -0.0570(6) 0.869(3) -0.0553(10) 0.0503(19) Uani 0.363(5) 1 d D . P C 3
O6 O 0.0009(8) 0.821(3) -0.1352(9) 0.0503(19) Uani 0.363(5) 1 d D . P C 3
O7 O -0.0015(6) 0.692(3) 0.0296(8) 0.0503(19) Uani 0.363(5) 1 d D . P C 3
O8 O 0.0521(6) 0.880(3) -0.0318(10) 0.0503(19) Uani 0.363(5) 1 d D . P C 3
Cl2A Cl 0.0015(5) 0.874(2) -0.0710(9) 0.0452(13) Uani 0.173(5) 1 d D . P D 4
O5A O -0.0646(8) 0.865(6) -0.0907(19) 0.0503(19) Uani 0.173(5) 1 d D . P D 4
O6A O 0.0035(13) 0.690(4) -0.115(2) 0.0503(19) Uani 0.173(5) 1 d D . P D 4
O7A O -0.0059(12) 0.890(6) 0.0124(12) 0.0503(19) Uani 0.173(5) 1 d D . P D 4
O8A O 0.0666(8) 0.871(6) -0.052(2) 0.0503(19) Uani 0.173(5) 1 d D . P D 4
Cl3 Cl 0.0007(4) 0.9087(15) -0.1982(6) 0.0452(13) Uani 0.280(6) 1 d D . P E 5
O9 O -0.0548(8) 1.019(3) -0.2030(12) 0.0503(19) Uani 0.280(6) 1 d D . P E 5
O10 O -0.0010(10) 0.837(4) -0.2761(10) 0.0503(19) Uani 0.280(6) 1 d D . P E 5
O11 O 0.0565(7) 1.017(3) -0.1838(13) 0.0503(19) Uani 0.280(6) 1 d D . P E 5
O12 O 0.0038(11) 0.756(3) -0.1431(13) 0.0503(19) Uani 0.280(6) 1 d D . P E 5
Cl3A Cl -0.0012(6) 0.986(2) -0.1846(8) 0.0452(13) Uani 0.184(5) 1 d D . P F 6
O9A O -0.0001(13) 1.188(3) -0.1976(19) 0.0503(19) Uani 0.184(5) 1 d D . P F 6
O10A O -0.0025(15) 0.897(5) -0.2618(14) 0.0503(19) Uani 0.184(5) 1 d D . P F 6
O11A O 0.0562(9) 0.945(6) -0.1358(16) 0.0503(19) Uani 0.184(5) 1 d D . P F 6
O12A O -0.0514(10) 0.934(5) -0.1467(17) 0.0503(19) Uani 0.184(5) 1 d D . P F 6


_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
Br1 C13 1.833(13) . ?
Br2 C23 1.852(15) . ?
Br1A C13A 1.875(11) . ?
Br2A C23A 1.890(9) . ?
Cu1 O14 1.939(4) . ?
Cu1 O24 2.201(4) . ?
Cu1 N1 2.039(5) . ?
Cu1 N3 2.033(5) . ?
Cu1 N6 2.045(5) 1_545 ?
O14 C14 1.282(8) . ?
O14 C14A 1.282(8) . ?
O24 C24 1.274(8) . ?
O24 C24A 1.274(8) . ?
N1 C1 1.329(7) . ?
N1 C2 1.340(7) . ?
N3 C4 1.338(8) . ?
N3 C8 1.333(8) . ?
N6 C5 1.341(8) . ?
N6 C7 1.332(8) . ?
N11 H11 0.8600 . ?
N11 C12 1.341(14) . ?
N11 C16 1.348(14) . ?
N21 H21 0.8600 . ?
N21 C22 1.333(15) . ?
N21 C26 1.335(15) . ?
N11A H11A 0.8600 . ?
N11A C12A 1.343(13) . ?
N11A C16A 1.352(13) . ?
N21A H21A 0.8600 . ?
N21A C22A 1.333(11) . ?
N21A C26A 1.332(11) . ?
C1 H1 0.9300 . ?
C1 C2 1.384(8) 3_665 ?
C2 H2 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.378(8) . ?
C5 H5 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.394(9) . ?
C8 H8 0.9300 . ?
C12 H12 0.9300 . ?
C12 C13 1.386(13) . ?
C13 C14 1.403(12) . ?
C14 C15 1.422(13) . ?
C15 H15 0.9300 . ?
C15 C16 1.392(13) . ?
C16 H16 0.9300 . ?
C22 H22 0.9300 . ?
C22 C23 1.380(14) . ?
C23 C24 1.398(13) . ?
C24 C25 1.412(14) . ?
C25 H25 0.9300 . ?
C25 C26 1.390(14) . ?
C26 H26 0.9300 . ?
C12A H12A 0.9300 . ?
C12A C13A 1.380(12) . ?
C13A C14A 1.425(11) . ?
C14A C15A 1.403(12) . ?
C15A H15A 0.9300 . ?
C15A C16A 1.372(12) . ?
C16A H16A 0.9300 . ?
C22A H22A 0.9300 . ?
C22A C23A 1.384(10) . ?
C23A C24A 1.432(10) . ?
C24A C25A 1.406(11) . ?
C25A H25A 0.9300 . ?
C25A C26A 1.376(11) . ?
C26A H26A 0.9300 . ?
Cl1 O1 1.452(4) . ?
Cl1 O2 1.433(5) . ?
Cl1 O3 1.437(5) . ?
Cl1 O4 1.431(5) . ?
Cl2 O5 1.388(12) . ?
Cl2 O6 1.481(14) . ?
Cl2 O7 1.408(12) . ?
Cl2 O8 1.371(13) . ?
Cl2A O5A 1.402(15) . ?
Cl2A O6A 1.459(16) . ?
Cl2A O7A 1.425(16) . ?
Cl2A O7A 1.88(4) 3_575 ?
Cl2A O8A 1.379(15) . ?
O7A O7A 1.59(9) 3_575 ?
Cl3 O9 1.399(14) . ?
Cl3 O10 1.378(14) . ?
Cl3 O11 1.393(14) . ?
Cl3 O12 1.384(15) . ?
Cl3A O9A 1.400(16) . ?
Cl3A O10A 1.418(15) . ?
Cl3A O11A 1.390(16) . ?
Cl3A O12A 1.377(15) . ?
O9A O10A 1.58(3) 2_554 ?

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
O14 Cu1 O24 95.50(16) . . ?
O14 Cu1 N1 171.59(19) . . ?
O14 Cu1 N3 95.00(18) . . ?
O14 Cu1 N6 86.48(19) . 1_545 ?
N1 Cu1 O24 91.96(17) . . ?
N1 Cu1 N6 89.18(19) . 1_545 ?
N3 Cu1 O24 91.91(18) . . ?
N3 Cu1 N1 88.60(19) . . ?
N3 Cu1 N6 174.03(18) . 1_545 ?
N6 Cu1 O24 93.71(18) 1_545 . ?
C14 O14 Cu1 135.7(4) . . ?
C14A O14 Cu1 135.7(4) . . ?
C24 O24 Cu1 134.0(4) . . ?
C24A O24 Cu1 134.0(4) . . ?
C1 N1 Cu1 121.0(4) . . ?
C1 N1 C2 117.7(5) . . ?
C2 N1 Cu1 121.3(4) . . ?
C4 N3 Cu1 119.6(4) . . ?
C8 N3 Cu1 122.7(4) . . ?
C8 N3 C4 117.6(5) . . ?
C5 N6 Cu1 119.9(4) . 1_565 ?
C7 N6 Cu1 122.8(4) . 1_565 ?
C7 N6 C5 117.2(5) . . ?
C12 N11 H11 118.5 . . ?
C12 N11 C16 123.0(14) . . ?
C16 N11 H11 118.5 . . ?
C22 N21 H21 117.9 . . ?
C22 N21 C26 124.1(18) . . ?
C26 N21 H21 117.9 . . ?
C12A N11A H11A 119.3 . . ?
C12A N11A C16A 121.5(11) . . ?
C16A N11A H11A 119.3 . . ?
C22A N21A H21A 119.1 . . ?
C26A N21A H21A 119.1 . . ?
C26A N21A C22A 121.9(9) . . ?
N1 C1 H1 119.7 . . ?
N1 C1 C2 120.6(5) . 3_665 ?
C2 C1 H1 119.7 3_665 . ?
N1 C2 C1 121.6(5) . 3_665 ?
N1 C2 H2 119.2 . . ?
C1 C2 H2 119.2 3_665 . ?
N3 C4 H4 119.3 . . ?
N3 C4 C5 121.4(6) . . ?
C5 C4 H4 119.3 . . ?
N6 C5 C4 121.4(5) . . ?
N6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
N6 C7 H7 119.2 . . ?
N6 C7 C8 121.6(6) . . ?
C8 C7 H7 119.2 . . ?
N3 C8 C7 120.8(6) . . ?
N3 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
N11 C12 H12 120.5 . . ?
N11 C12 C13 119.1(13) . . ?
C13 C12 H12 120.5 . . ?
C12 C13 Br1 121.5(10) . . ?
C12 C13 C14 124.0(12) . . ?
C14 C13 Br1 114.5(9) . . ?
O14 C14 C13 126.9(8) . . ?
O14 C14 C15 121.1(9) . . ?
C13 C14 C15 111.7(11) . . ?
C14 C15 H15 117.4 . . ?
C16 C15 C14 125.2(16) . . ?
C16 C15 H15 117.4 . . ?
N11 C16 C15 116.9(16) . . ?
N11 C16 H16 121.5 . . ?
C15 C16 H16 121.5 . . ?
N21 C22 H22 120.8 . . ?
N21 C22 C23 118.3(17) . . ?
C23 C22 H22 120.8 . . ?
C22 C23 Br2 123.3(12) . . ?
C22 C23 C24 123.9(14) . . ?
C24 C23 Br2 112.8(10) . . ?
O24 C24 C23 130.0(9) . . ?
O24 C24 C25 117.9(11) . . ?
C23 C24 C25 111.9(13) . . ?
C24 C25 H25 117.5 . . ?
C26 C25 C24 125(2) . . ?
C26 C25 H25 117.5 . . ?
N21 C26 C25 116(2) . . ?
N21 C26 H26 121.8 . . ?
C25 C26 H26 121.8 . . ?
N11A C12A H12A 119.9 . . ?
N11A C12A C13A 120.3(11) . . ?
C13A C12A H12A 119.9 . . ?
C12A C13A Br1A 116.1(8) . . ?
C12A C13A C14A 119.1(10) . . ?
C14A C13A Br1A 124.8(7) . . ?
O14 C14A C13A 113.7(7) . . ?
O14 C14A C15A 127.2(8) . . ?
C15A C14A C13A 119.0(9) . . ?
C14A C15A H15A 120.9 . . ?
C16A C15A C14A 118.3(13) . . ?
C16A C15A H15A 120.9 . . ?
N11A C16A C15A 121.8(13) . . ?
N11A C16A H16A 119.1 . . ?
C15A C16A H16A 119.1 . . ?
N21A C22A H22A 120.3 . . ?
N21A C22A C23A 119.5(9) . . ?
C23A C22A H22A 120.3 . . ?
C22A C23A Br2A 117.3(7) . . ?
C22A C23A C24A 120.6(8) . . ?
C24A C23A Br2A 122.2(6) . . ?
O24 C24A C23A 117.9(6) . . ?
O24 C24A C25A 125.2(7) . . ?
C25A C24A C23A 116.8(7) . . ?
C24A C25A H25A 120.5 . . ?
C26A C25A C24A 119.0(11) . . ?
C26A C25A H25A 120.5 . . ?
N21A C26A C25A 122.2(10) . . ?
N21A C26A H26A 118.9 . . ?
C25A C26A H26A 118.9 . . ?
O2 Cl1 O1 109.0(3) . . ?
O2 Cl1 O3 109.0(3) . . ?
O3 Cl1 O1 109.9(3) . . ?
O4 Cl1 O1 110.1(3) . . ?
O4 Cl1 O2 109.5(4) . . ?
O4 Cl1 O3 109.4(3) . . ?
O5 Cl2 O6 87.4(9) . . ?
O5 Cl2 O7 96.2(9) . . ?
O7 Cl2 O6 174.1(13) . . ?
O8 Cl2 O5 113.5(13) . . ?
O8 Cl2 O6 84.9(10) . . ?
O8 Cl2 O7 97.8(10) . . ?
O5A Cl2A O6A 87.5(15) . . ?
O5A Cl2A O7A 88.1(14) . . ?
O7A Cl2A O6A 125(3) . . ?
O8A Cl2A O5A 177(3) . . ?
O8A Cl2A O6A 89.6(15) . . ?
O8A Cl2A O7A 92.7(14) . . ?
O10 Cl3 O9 104.1(12) . . ?
O10 Cl3 O11 104.0(12) . . ?
O10 Cl3 O12 110.3(14) . . ?
O11 Cl3 O9 114.8(15) . . ?
O12 Cl3 O9 113.3(13) . . ?
O12 Cl3 O11 109.7(13) . . ?
O9A Cl3A O10A 106.7(16) . . ?
O11A Cl3A O9A 105(2) . . ?
O11A Cl3A O10A 109.1(16) . . ?
O12A Cl3A O9A 111.2(16) . . ?
O12A Cl3A O10A 113.4(16) . . ?
O12A Cl3A O11A 111.3(16) . . ?
Cl3A O9A O10A 163(2) . 2_554 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C13 C14 O14 1(2) . . . . ?
Br1 C13 C14 C15 174.8(15) . . . . ?
Br2 C23 C24 O24 2(3) . . . . ?
Br2 C23 C24 C25 176(2) . . . . ?
Br1A C13A C14A O14 -4.0(18) . . . . ?
Br1A C13A C14A C15A -179.4(13) . . . . ?
Br2A C23A C24A O24 -1.2(15) . . . . ?
Br2A C23A C24A C25A -177.0(12) . . . . ?
Cu1 O14 C14 C13 146.6(14) . . . . ?
Cu1 O14 C14 C15 -26.6(16) . . . . ?
Cu1 O14 C14A C13A 149.6(9) . . . . ?
Cu1 O14 C14A C15A -35.4(14) . . . . ?
Cu1 O24 C24 C23 127.7(19) . . . . ?
Cu1 O24 C24 C25 -46(2) . . . . ?
Cu1 O24 C24A C23A 132.8(8) . . . . ?
Cu1 O24 C24A C25A -51.8(14) . . . . ?
Cu1 N1 C1 C2 180.0(4) . . . 3_665 ?
Cu1 N1 C2 C1 -180.0(4) . . . 3_665 ?
Cu1 N3 C4 C5 177.9(5) . . . . ?
Cu1 N3 C8 C7 -177.5(5) . . . . ?
Cu1 N6 C5 C4 -176.3(5) 1_565 . . . ?
Cu1 N6 C7 C8 176.5(5) 1_565 . . . ?
O14 C14 C15 C16 177.9(16) . . . . ?
O14 C14A C15A C16A -176.0(11) . . . . ?
O24 C24 C25 C26 180(3) . . . . ?
O24 C24A C25A C26A -177.8(11) . . . . ?
N3 C4 C5 N6 -1.0(10) . . . . ?
N6 C7 C8 N3 0.4(10) . . . . ?
N11 C12 C13 Br1 -176.9(15) . . . . ?
N11 C12 C13 C14 3(3) . . . . ?
N21 C22 C23 Br2 -177(2) . . . . ?
N21 C22 C23 C24 5(4) . . . . ?
N11A C12A C13A Br1A 179.0(11) . . . . ?
N11A C12A C13A C14A -1(2) . . . . ?
N21A C22A C23A Br2A 178.1(9) . . . . ?
N21A C22A C23A C24A -2.5(19) . . . . ?
C1 N1 C2 C1 0.8(10) . . . 3_665 ?
C2 N1 C1 C2 -0.8(10) . . . 3_665 ?
C4 N3 C8 C7 0.2(9) . . . . ?
C5 N6 C7 C8 -1.2(9) . . . . ?
C7 N6 C5 C4 1.5(9) . . . . ?
C8 N3 C4 C5 0.1(9) . . . . ?
C12 N11 C16 C15 -3(3) . . . . ?
C12 C13 C14 O14 -178.7(15) . . . . ?
C12 C13 C14 C15 -5(3) . . . . ?
C13 C14 C15 C16 4(3) . . . . ?
C14 C15 C16 N11 0(3) . . . . ?
C16 N11 C12 C13 1(3) . . . . ?
C22 N21 C26 C25 0(4) . . . . ?
C22 C23 C24 O24 179.3(19) . . . . ?
C22 C23 C24 C25 -6(4) . . . . ?
C23 C24 C25 C26 5(4) . . . . ?
C24 C25 C26 N21 -2(5) . . . . ?
C26 N21 C22 C23 -2(4) . . . . ?
C12A N11A C16A C15A -3(2) . . . . ?
C12A C13A C14A O14 176.3(12) . . . . ?
C12A C13A C14A C15A 1(2) . . . . ?
C13A C14A C15A C16A -1(2) . . . . ?
C14A C15A C16A N11A 2(2) . . . . ?
C16A N11A C12A C13A 2(2) . . . . ?
C22A N21A C26A C25A 1.5(19) . . . . ?
C22A C23A C24A O24 179.5(10) . . . . ?
C22A C23A C24A C25A 3.7(19) . . . . ?
C23A C24A C25A C26A -2(2) . . . . ?
C24A C25A C26A N21A 0(2) . . . . ?
C26A N21A C22A C23A -0.1(18) . . . . ?
O5A Cl2A O7A Cl2A -100(2) . . . 3_575 ?
O5A Cl2A O7A O7A -100(2) . . . 3_575 ?
O6A Cl2A O7A Cl2A 174.5(19) . . . 3_575 ?
O6A Cl2A O7A O7A 174.5(19) . . . 3_575 ?
O7A Cl2A O7A Cl2A 0.002(2) 3_575 . . 3_575 ?
O8A Cl2A O7A Cl2A 83(2) . . . 3_575 ?
O8A Cl2A O7A O7A 83(2) . . . 3_575 ?
O9A Cl3A O10A O9A 175(3) . . . 2_544 ?
O10A Cl3A O9A O10A -5(9) . . . 2_554 ?
O11A Cl3A O9A O10A 111(8) . . . 2_554 ?
O11A Cl3A O10A O9A 62(4) . . . 2_544 ?
O12A Cl3A O9A O10A -129(8) . . . 2_554 ?
O12A Cl3A O10A O9A -63(4) . . . 2_544 ?


# start Validation Reply Form
_vrf_PLAT242_jcmaa               
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Cl1 Check 
RESPONSE: Cl1 is part of a perchlorate anion. As such, this is not a case
of misassigned atom-type.
;
_vrf_PLAT341_jcmaa               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.009 Ang.  
RESPONSE: Noted. All geometries are included with associated standard
uncertainties.
;
_vrf_PLAT906_jcmaa               
;
PROBLEM: Large K Value in the Analysis of Variance ......      4.955 Check 
RESPONSE: This value of K is associated with the weakest Fc/Fc(max) group 
(0.000 - 0.014). The next largest value of K was associated with the next
weakest Fc/Fc(max) group (1.591 for 0.014 - 0.027). All other values of
K ranged from 0.998 to 1.199.
;
_vrf_PLAT910_jcmaa               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).          9 Note  
RESPONSE: These may have been partially obstructed by the beamstop. They
represent a very small number of reflections compared with the total 
number that were collected.
;
_vrf_PLAT971_jcmaa               
;
PROBLEM: Check Calcd Resid. Dens.  0.63A   From O10A            1.64 eA-3  
RESPONSE: This is in the area of a badly disordered perchlorate anion,
and may indicate an additional disorder component.
;
_vrf_PLAT977_jcmaa               
;
PROBLEM: Check Negative Difference Density on H11A             -0.31 eA-3  
RESPONSE: This is a partial occupancy hydrogen atom, which is required
for charge balance. It is consistent with other supporting 
characterizations.
;
_vrf_PLAT002_jcmaa               
;
PROBLEM: Number of Distance or Angle Restraints on AtSite         50 Note   
RESPONSE: Two fully disordered ligands, and one disordered perchlorate anion
 were present. These were modeled using distance restraints and displacement 
constraints. 
;
_vrf_PLAT004_jcmaa               
;
PROBLEM: Polymeric Structure Found with Maximum Dimension          1 Info   
RESPONSE: This is confirmed. 
;
_vrf_PLAT007_jcmaa               
;
PROBLEM: Number of Unrefined Donor-H Atoms ..............          4 Report   
RESPONSE: Since the hydrogen atoms were associated with the fully disordered
ligands, these were introduced in calculated positions and refined on a 
riding model. 
;
_vrf_PLAT042_jcmaa               
;
PROBLEM: Calc. and Reported MoietyFormula Strings  Differ     Please Check   
RESPONSE: The reported formula differentiates the perchlorate anions from
the rest of the structure, with associatedi integer values.
;
_vrf_PLAT083_jcmaa               
;
PROBLEM: SHELXL Second Parameter in WGHT  Unusually Large      33.62 Why ?  
RESPONSE: This may have been due to the inclusion of some weak, high angle
data.
;
_vrf_PLAT168_jcmaa               
;
PROBLEM: The CIF-Embedded .res File Contains EXYZ Records          2 Report 
RESPONSE: The model includes two fully disordered ligands. The atoms on the 
"pivot" site for the disorder (C14A and C24A) were split, with refined 
occupancy. The atoms were constrained to have the same positions as 
their minor disorder components (C14 and C24). 
;
_vrf_PLAT171_jcmaa               
;
PROBLEM: The CIF-Embedded .res File Contains EADP Records          6 Report
RESPONSE: The model includes two fully disordered ligands and one disordered
perchlorate anion. The atoms in these groups were contrained to have 
identical anisotropic displacements.
;
_vrf_PLAT176_jcmaa               
;
PROBLEM: The CIF-Embedded .res File Contains SADI Records          12 Report
RESPONSE: The model includes two fully disordered ligands and one disordered
perchlorate anion. The atoms in these groups were treated with similar 
distance restraints on bonds.
;
_vrf_PLAT301_jcmaa               
;
PROBLEM: Main Residue  Disorder ..............(Resd  1  )        45% Note
RESPONSE: This is consistent with the presence of two fully disordered 
ligands.
;
_vrf_PLAT302_jcmaa               
;
PROBLEM: Anion/Solvent/Minor-Residue Disorder (Resd  2  )       100% Note 
RESPONSE: This is consistent with the presence of one fully disordered 
perchlorate anion (where PLATON appears to consider the other as coordinated
to the main residue).
;
_vrf_PLAT395_jcmaa               
;
PROBLEM: Deviating  X-O-Y    Angle From 120
RESPONSE: This is a bit of an odd alert, since there are no X-O-Y
species present in the structure. It is likely associated with
misinterpretation of the disorder model for the perchlorate anion.
;
_vrf_PLAT811_jcmaa               
;
PROBLEM: No ADDSYM Analysis: Too Many Excluded Atoms ....          ! Info 
RESPONSE: This is noted.
;
_vrf_PLAT860_jcmaa               
;
PROBLEM: Number of Least-Squares Restraints .............         202 Note   
RESPONSE: Two fully disordered ligands and one perchlorate anion were 
present. These were modeled using distance restraints and displacement 
constraints. 
;
_vrf_PLAT941_jcmaa               
;
PROBLEM: Average HKL Measurement Multiplicity ...........        3.2 Low
RESPONSE: This is noted.
;
_vrf_PLAT978_jcmaa               
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          7 Info
RESPONSE: This is consistent with a good model.
;

# end Validation Reply Form
####################################################################### 
# 
# 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_jcmaa_sq
_database_code_depnum_ccdc_archive 'CCDC 2099943'
loop_
_audit_author_name
_audit_author_address
'Louise N. Dawe'
;Wilfrid Laurier University
Canada
;
_audit_update_record             
;
2021-07-28 deposited with the CCDC.	2022-02-24 downloaded from the CCDC.
;
_audit_creation_date             2021-02-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H14 Br2 Cu N5 O2, Cl O4'
_chemical_formula_sum            'C16 H14 Br2 Cl Cu N5 O6'
_chemical_formula_weight         631.13
_chemical_melting_point          ?

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'
Br Br -0.2901 2.4595 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_symmetry_space_group_name_H-M_alt 'P 1 21/c 1'
_cell_length_a                   21.4129(7)
_cell_length_b                   6.8466(2)
_cell_length_c                   16.6158(6)
_cell_angle_alpha                90
_cell_angle_beta                 99.172(3)
_cell_angle_gamma                90
_cell_volume                     2404.83(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6490
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      28.7500
_cell_measurement_theta_min      3.5190
_cell_oxdiff_angle_alpha         89.986(3)
_cell_oxdiff_angle_beta          99.114(3)
_cell_oxdiff_angle_gamma         90.029(3)
_cell_oxdiff_length_a            21.4211(8)
_cell_oxdiff_length_b            6.8510(3)
_cell_oxdiff_length_c            16.6064(8)
_cell_oxdiff_measurement_reflns_used 4876
_cell_oxdiff_volume              2406.33(17)
_shelx_estimated_absorpt_T_max   0.779
_shelx_estimated_absorpt_T_min   0.490
_exptl_absorpt_coefficient_mu    4.382
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1236
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 0 0.0213
-3 -4 2 0.0723
3 1 1 0.0514
3 0 -1 0.0460
-3 -4 -1 0.0968
3 0 2 0.0674
2 -2 5 0.0813
0 1 -5 0.0552
-3 2 2 0.0648
3 -2 1 0.0742
1 0 0 0.0382
-1 0 5 0.0865

_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.06
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.5003 -0.0001 -0.0002 0.0156 0.0025 -0.0058
-2.5012 -4.0020 2.0018 0.2200 -0.0583 0.3634
2.5009 1.0011 1.0014 -0.1131 -0.0597 -0.0667
2.5019 0.0001 -0.9999 -0.0780 0.0307 0.0272
-2.5001 -4.0027 -1.0006 0.2195 0.0714 0.3584
2.5008 0.0008 2.0025 -0.0774 -0.0990 0.0322
2.0000 -1.9996 5.0052 0.0096 -0.2184 0.2258
-0.4988 0.9992 -5.0044 -0.0208 0.2148 -0.1113
-2.5027 2.0012 2.0002 0.0072 -0.0818 -0.2200
2.5017 -2.0005 1.0022 -0.0066 -0.0479 0.2250
0.5003 0.0001 0.0002 -0.0156 -0.0025 0.0058
-1.0023 0.0011 5.0037 0.0320 -0.2112 -0.0033

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14764
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         3.308
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00 100.00   1.00   32.79    --   11.05 178.00-120.00   65
  2  ω    -84.00  13.00   1.00   32.79    --  -11.98 -57.00 -90.00   97
  3  ω     -5.00  29.00   1.00   32.79    --  -11.98 -99.00 120.00   34
  4  ω    -85.00 -56.00   1.00   32.79    --  -11.98 -37.00-120.00   29
  5  ω     -7.00  41.00   1.00   32.79    --  -11.98  37.00-120.00   48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0310892000
_diffrn_orient_matrix_UB_12      -0.0354658000
_diffrn_orient_matrix_UB_13      0.0001786000
_diffrn_orient_matrix_UB_21      -0.0049890000
_diffrn_orient_matrix_UB_22      -0.0039223000
_diffrn_orient_matrix_UB_23      -0.0432101000
_diffrn_orient_matrix_UB_31      0.0115460000
_diffrn_orient_matrix_UB_32      -0.0971675000
_diffrn_orient_matrix_UB_33      0.0016839000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3895
_reflns_number_total             4577
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4577
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0469
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0071P)²+14.9175P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0961
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Shared sites
{C24A, C24}
{C14A, C14}
3. Restrained distances
 Br1A-C13A \\sim Br1-C13
 with sigma of 0.02
 C13A-C12A \\sim C14A-C13A \\sim C15A-C14A \\sim C16A-C15A \\sim C13-C12 \\sim
C14-C13 \\sim C15-C14 ~
 C16-C15
 with sigma of 0.02
 N11-C16 \\sim N11A-C16A \\sim N11-C12 \\sim N11A-C12A
 with sigma of 0.02
 Br2A-C23A \\sim Br2-C23
 with sigma of 0.02
 C24A-C23A \\sim C25A-C24A \\sim C26-C25 \\sim C23-C22 \\sim C23A-C22A \\sim
C24-C23 \\sim C25-C24 ~
 C26A-C25A
 with sigma of 0.02
 N21A-C22A \\sim N21-C22 \\sim N21A-C26A \\sim N21-C26
 with sigma of 0.02
 O24-C24A \\sim O24-C24
 with sigma of 0.02
 O14-C14 \\sim O14-C14A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Br1A) = Uanis(Br1)
Uanis(C12A) = Uanis(C13A) = Uanis(C14A) = Uanis(C15) = Uanis(C16) = Uanis(N11)
= Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15A) = Uanis(C16A) = Uanis(N11A)
Uanis(Br2A) = Uanis(Br2)
Uanis(C23A) = Uanis(C24A) = Uanis(C25A) = Uanis(C26) = Uanis(N21) = Uanis(C22)
= Uanis(C23) = Uanis(C22A) = Uanis(C24) = Uanis(C25) = Uanis(C26A) = Uanis(N21A)
5. Others
 Sof(Br1A)=Sof(N11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(C14A)=
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=1-FVAR(1)
 Sof(Br1)=Sof(N11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(C14)=Sof(C15)=
 Sof(H15)=Sof(C16)=Sof(H16)=FVAR(1)
 Sof(Br2A)=Sof(N21A)=Sof(H21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(C24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=1-FVAR(2)
 Sof(Br2)=Sof(N21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(C24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), N11(H11), N21(H21), C12(H12),
 C15(H15), C16(H16), C22(H22), C25(H25), C26(H26), N11A(H11A), N21A(H21A),
 C12A(H12A), C15A(H15A), C16A(H16A), C22A(H22A), C25A(H25A), C26A(H26A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.36783(2) 0.49544(7) 0.09165(3) 0.00851(12) Uani 1 1 d . . . . .
O14 O 0.30046(13) 0.4738(5) 0.15647(18) 0.0145(7) Uani 1 1 d D . . . .
O24 O 0.30502(13) 0.5005(5) -0.02683(17) 0.0148(6) Uani 1 1 d D . . . .
N1 N 0.44663(16) 0.4973(5) 0.0372(2) 0.0102(7) Uani 1 1 d . . . . .
N3 N 0.37179(16) 0.7917(5) 0.0959(2) 0.0082(7) Uani 1 1 d . . . . .
N6 N 0.37229(16) 1.1968(5) 0.0960(2) 0.0092(7) Uani 1 1 d . . . . .
C1 C 0.50414(19) 0.4997(6) 0.0814(3) 0.0118(9) Uani 1 1 d . . . . .
H1 H 0.508631 0.500246 0.139248 0.014 Uiso 1 1 calc R U . . .
C2 C 0.4424(2) 0.4986(6) -0.0441(3) 0.0126(9) Uani 1 1 d . . . . .
H2 H 0.401785 0.498280 -0.076977 0.015 Uiso 1 1 calc R U . . .
C4 C 0.3724(2) 0.8938(6) 0.0274(3) 0.0114(9) Uani 1 1 d . . . . .
H4 H 0.372469 0.826030 -0.022488 0.014 Uiso 1 1 calc R U . . .
C5 C 0.3730(2) 1.0946(6) 0.0276(3) 0.0113(9) Uani 1 1 d . . . . .
H5 H 0.374031 1.162367 -0.022094 0.014 Uiso 1 1 calc R U . . .
C7 C 0.3723(2) 1.0959(6) 0.1645(3) 0.0124(9) Uani 1 1 d . . . . .
H7 H 0.372673 1.164294 0.214325 0.015 Uiso 1 1 calc R U . . .
C8 C 0.3718(2) 0.8929(7) 0.1648(3) 0.0137(9) Uani 1 1 d . . . . .
H8 H 0.371370 0.825037 0.214601 0.016 Uiso 1 1 calc R U . . .
Br1 Br 0.2154(3) 0.2043(9) 0.2312(5) 0.0362(6) Uani 0.442(7) 1 d D . P A 1
Br2 Br 0.2323(3) 0.8121(10) -0.1314(4) 0.0392(6) Uani 0.319(11) 1 d D . P B 1
N11 N 0.1166(5) 0.6643(15) 0.1231(7) 0.0242(7) Uani 0.442(7) 1 d D . P A 1
H11 H 0.077326 0.707070 0.116845 0.029 Uiso 0.442(7) 1 calc R U P A 1
N21 N 0.1185(7) 0.365(2) -0.0849(10) 0.0242(6) Uani 0.319(11) 1 d D . P B 1
H21 H 0.078281 0.332293 -0.097246 0.029 Uiso 0.319(11) 1 calc R U P B 1
C12 C 0.1314(5) 0.499(2) 0.1658(8) 0.0242(7) Uani 0.442(7) 1 d D . P A 1
H12 H 0.099736 0.428530 0.187831 0.029 Uiso 0.442(7) 1 calc R U P A 1
C13 C 0.1929(5) 0.433(2) 0.1771(10) 0.0242(7) Uani 0.442(7) 1 d D . P A 1
C14 C 0.2429(2) 0.5307(7) 0.1490(3) 0.0242(7) Uani 0.442(7) 1 d D . P A 1
C15 C 0.2220(7) 0.700(2) 0.1012(9) 0.0242(7) Uani 0.442(7) 1 d D . P A 1
H15 H 0.252193 0.770228 0.076515 0.029 Uiso 0.442(7) 1 calc R U P A 1
C16 C 0.1599(5) 0.7675(19) 0.0893(8) 0.0242(7) Uani 0.442(7) 1 d D . P A 1
H16 H 0.148164 0.882229 0.058339 0.029 Uiso 0.442(7) 1 calc R U P A 1
C22 C 0.1381(7) 0.530(3) -0.1158(11) 0.0242(6) Uani 0.319(11) 1 d D . P B 1
H22 H 0.109292 0.608421 -0.151281 0.029 Uiso 0.319(11) 1 calc R U P B 1
C23 C 0.2005(6) 0.584(3) -0.0957(13) 0.0242(6) Uani 0.319(11) 1 d D . P B 1
C24 C 0.2464(2) 0.4681(7) -0.0494(3) 0.0242(6) Uani 0.319(11) 1 d D . P B 1
C25 C 0.2200(9) 0.300(3) -0.0177(14) 0.0242(6) Uani 0.319(11) 1 d D . P B 1
H25 H 0.247505 0.219035 0.018552 0.029 Uiso 0.319(11) 1 calc R U P B 1
C26 C 0.1573(7) 0.246(3) -0.0359(12) 0.0242(6) Uani 0.319(11) 1 d D . P B 1
H26 H 0.142224 0.129444 -0.014597 0.029 Uiso 0.319(11) 1 calc R U P B 1
Br1A Br 0.2299(2) 0.1666(7) 0.2387(3) 0.0362(6) Uani 0.558(7) 1 d D . P A 2
Br2A Br 0.2485(2) 0.8328(5) -0.13967(19) 0.0392(6) Uani 0.681(11) 1 d D . P B 2
N11A N 0.1181(4) 0.6232(13) 0.1541(5) 0.0242(7) Uani 0.558(7) 1 d D . P A 2
H11A H 0.078576 0.655217 0.155957 0.029 Uiso 0.558(7) 1 calc R U P A 2
N21A N 0.1184(3) 0.4175(12) -0.1085(5) 0.0242(6) Uani 0.681(11) 1 d D . P B 2
H21A H 0.077737 0.400535 -0.125656 0.029 Uiso 0.681(11) 1 calc R U P B 2
C12A C 0.1415(4) 0.4541(15) 0.1884(6) 0.0242(7) Uani 0.558(7) 1 d D . P A 2
H12A H 0.114956 0.369406 0.213147 0.029 Uiso 0.558(7) 1 calc R U P A 2
C13A C 0.2032(4) 0.4046(16) 0.1875(8) 0.0242(7) Uani 0.558(7) 1 d D . P A 2
C14A C 0.2429(2) 0.5307(7) 0.1490(3) 0.0242(7) Uani 0.558(7) 1 d D . P A 2
C15A C 0.2169(6) 0.7041(18) 0.1139(8) 0.0242(7) Uani 0.558(7) 1 d D . P A 2
H15A H 0.242055 0.792106 0.088485 0.029 Uiso 0.558(7) 1 calc R U P A 2
C16A C 0.1549(4) 0.7450(16) 0.1167(6) 0.0242(7) Uani 0.558(7) 1 d D . P A 2
H16A H 0.136916 0.861445 0.092021 0.029 Uiso 0.558(7) 1 calc R U P A 2
C22A C 0.1468(4) 0.5784(13) -0.1306(5) 0.0242(6) Uani 0.681(11) 1 d D . P B 2
H22A H 0.123336 0.672839 -0.164760 0.029 Uiso 0.681(11) 1 calc R U P B 2
C23A C 0.2106(3) 0.6060(13) -0.1034(6) 0.0242(6) Uani 0.681(11) 1 d D . P B 2
C24A C 0.2464(2) 0.4681(7) -0.0494(3) 0.0242(6) Uani 0.681(11) 1 d D . P B 2
C25A C 0.2136(4) 0.3016(16) -0.0301(7) 0.0242(6) Uani 0.681(11) 1 d D . P B 2
H25A H 0.235075 0.203237 0.003946 0.029 Uiso 0.681(11) 1 calc R U P B 2
C26A C 0.1508(4) 0.2810(13) -0.0604(5) 0.0242(6) Uani 0.681(11) 1 d D . P B 2
H26A H 0.129248 0.166974 -0.047134 0.029 Uiso 0.681(11) 1 calc R U P B 2
Cl1 Cl 0.43272(5) 0.49220(16) 0.32166(6) 0.0134(2) Uani 1 1 d . . . . .
O1 O 0.44199(16) 0.4893(5) 0.23698(19) 0.0222(7) Uani 1 1 d . . . . .
O2 O 0.40262(19) 0.6720(5) 0.3377(2) 0.0296(9) Uani 1 1 d . . . . .
O3 O 0.39285(17) 0.3322(5) 0.3370(2) 0.0263(8) Uani 1 1 d . . . . .
O4 O 0.49218(16) 0.4764(7) 0.3741(2) 0.0419(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O14 1.939(3) . ?
Cu1 O24 2.200(3) . ?
Cu1 N1 2.038(3) . ?
Cu1 N3 2.031(3) . ?
Cu1 N6 2.048(4) 1_545 ?
O14 C14 1.280(5) . ?
O14 C14A 1.280(5) . ?
O24 C24 1.271(5) . ?
O24 C24A 1.271(5) . ?
N1 C1 1.330(5) . ?
N1 C2 1.340(5) . ?
N3 C4 1.338(5) . ?
N3 C8 1.338(6) . ?
N6 C5 1.337(6) . ?
N6 C7 1.332(5) . ?
C1 H1 0.9500 . ?
C1 C2 1.387(6) 3_665 ?
C2 H2 0.9500 . ?
C4 H4 0.9500 . ?
C4 C5 1.375(6) . ?
C5 H5 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.390(6) . ?
C8 H8 0.9500 . ?
Br1 C13 1.828(11) . ?
Br2 C23 1.839(13) . ?
N11 H11 0.8800 . ?
N11 C12 1.348(12) . ?
N11 C16 1.357(11) . ?
N21 H21 0.8800 . ?
N21 C22 1.337(13) . ?
N21 C26 1.341(13) . ?
C12 H12 0.9500 . ?
C12 C13 1.379(11) . ?
C13 C14 1.405(10) . ?
C14 C15 1.436(11) . ?
C15 H15 0.9500 . ?
C15 C16 1.391(11) . ?
C16 H16 0.9500 . ?
C22 H22 0.9500 . ?
C22 C23 1.377(13) . ?
C23 C24 1.395(12) . ?
C24 C25 1.420(13) . ?
C25 H25 0.9500 . ?
C25 C26 1.380(13) . ?
C26 H26 0.9500 . ?
Br1A C13A 1.884(9) . ?
Br2A C23A 1.894(7) . ?
N11A H11A 0.8800 . ?
N11A C12A 1.351(10) . ?
N11A C16A 1.363(10) . ?
N21A H21A 0.8800 . ?
N21A C22A 1.338(9) . ?
N21A C26A 1.347(9) . ?
C12A H12A 0.9500 . ?
C12A C13A 1.366(10) . ?
C13A C14A 1.433(9) . ?
C14A C15A 1.398(10) . ?
C15A H15A 0.9500 . ?
C15A C16A 1.366(10) . ?
C16A H16A 0.9500 . ?
C22A H22A 0.9500 . ?
C22A C23A 1.381(9) . ?
C23A C24A 1.437(8) . ?
C24A C25A 1.402(9) . ?
C25A H25A 0.9500 . ?
C25A C26A 1.367(9) . ?
C26A H26A 0.9500 . ?
Cl1 O1 1.452(3) . ?
Cl1 O2 1.434(4) . ?
Cl1 O3 1.436(3) . ?
Cl1 O4 1.428(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O14 Cu1 O24 95.47(12) . . ?
O14 Cu1 N1 171.60(13) . . ?
O14 Cu1 N3 95.02(13) . . ?
O14 Cu1 N6 86.50(13) . 1_545 ?
N1 Cu1 O24 91.96(12) . . ?
N1 Cu1 N6 89.11(14) . 1_545 ?
N3 Cu1 O24 91.81(13) . . ?
N3 Cu1 N1 88.65(14) . . ?
N3 Cu1 N6 174.06(13) . 1_545 ?
N6 Cu1 O24 93.76(13) 1_545 . ?
C14 O14 Cu1 135.5(3) . . ?
C14A O14 Cu1 135.5(3) . . ?
C24 O24 Cu1 134.1(3) . . ?
C24A O24 Cu1 134.1(3) . . ?
C1 N1 Cu1 120.9(3) . . ?
C1 N1 C2 117.7(4) . . ?
C2 N1 Cu1 121.3(3) . . ?
C4 N3 Cu1 119.9(3) . . ?
C8 N3 Cu1 122.8(3) . . ?
C8 N3 C4 117.3(4) . . ?
C5 N6 Cu1 120.0(3) . 1_565 ?
C7 N6 Cu1 122.8(3) . 1_565 ?
C7 N6 C5 117.2(4) . . ?
N1 C1 H1 119.6 . . ?
N1 C1 C2 120.7(4) . 3_665 ?
C2 C1 H1 119.6 3_665 . ?
N1 C2 C1 121.5(4) . 3_665 ?
N1 C2 H2 119.2 . . ?
C1 C2 H2 119.2 3_665 . ?
N3 C4 H4 119.3 . . ?
N3 C4 C5 121.5(4) . . ?
C5 C4 H4 119.3 . . ?
N6 C5 C4 121.6(4) . . ?
N6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
N6 C7 H7 119.2 . . ?
N6 C7 C8 121.5(4) . . ?
C8 C7 H7 119.2 . . ?
N3 C8 C7 120.9(4) . . ?
N3 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C12 N11 H11 118.8 . . ?
C12 N11 C16 122.5(10) . . ?
C16 N11 H11 118.8 . . ?
C22 N21 H21 118.6 . . ?
C22 N21 C26 122.9(14) . . ?
C26 N21 H21 118.6 . . ?
N11 C12 H12 120.4 . . ?
N11 C12 C13 119.2(10) . . ?
C13 C12 H12 120.4 . . ?
C12 C13 Br1 121.3(8) . . ?
C12 C13 C14 124.1(9) . . ?
C14 C13 Br1 114.7(7) . . ?
O14 C14 C13 126.5(6) . . ?
O14 C14 C15 120.7(7) . . ?
C13 C14 C15 112.5(8) . . ?
C14 C15 H15 118.2 . . ?
C16 C15 C14 123.6(12) . . ?
C16 C15 H15 118.2 . . ?
N11 C16 C15 118.0(12) . . ?
N11 C16 H16 121.0 . . ?
C15 C16 H16 121.0 . . ?
N21 C22 H22 120.4 . . ?
N21 C22 C23 119.2(13) . . ?
C23 C22 H22 120.4 . . ?
C22 C23 Br2 123.1(10) . . ?
C22 C23 C24 123.4(12) . . ?
C24 C23 Br2 113.4(8) . . ?
O24 C24 C23 129.7(7) . . ?
O24 C24 C25 117.7(8) . . ?
C23 C24 C25 112.3(10) . . ?
C24 C25 H25 117.7 . . ?
C26 C25 C24 124.5(15) . . ?
C26 C25 H25 117.7 . . ?
N21 C26 C25 117.3(15) . . ?
N21 C26 H26 121.3 . . ?
C25 C26 H26 121.3 . . ?
C12A N11A H11A 119.5 . . ?
C12A N11A C16A 121.0(8) . . ?
C16A N11A H11A 119.5 . . ?
C22A N21A H21A 119.3 . . ?
C22A N21A C26A 121.4(7) . . ?
C26A N21A H21A 119.3 . . ?
N11A C12A H12A 119.9 . . ?
N11A C12A C13A 120.1(8) . . ?
C13A C12A H12A 119.9 . . ?
C12A C13A Br1A 115.8(7) . . ?
C12A C13A C14A 119.9(8) . . ?
C14A C13A Br1A 124.3(6) . . ?
O14 C14A C13A 113.8(5) . . ?
O14 C14A C15A 127.7(6) . . ?
C15A C14A C13A 118.3(7) . . ?
C14A C15A H15A 120.5 . . ?
C16A C15A C14A 118.9(10) . . ?
C16A C15A H15A 120.5 . . ?
N11A C16A C15A 121.8(9) . . ?
N11A C16A H16A 119.1 . . ?
C15A C16A H16A 119.1 . . ?
N21A C22A H22A 120.3 . . ?
N21A C22A C23A 119.5(7) . . ?
C23A C22A H22A 120.3 . . ?
C22A C23A Br2A 117.4(5) . . ?
C22A C23A C24A 121.0(6) . . ?
C24A C23A Br2A 121.6(5) . . ?
O24 C24A C23A 118.2(5) . . ?
O24 C24A C25A 125.6(5) . . ?
C25A C24A C23A 116.1(5) . . ?
C24A C25A H25A 120.0 . . ?
C26A C25A C24A 120.0(8) . . ?
C26A C25A H25A 120.0 . . ?
N21A C26A C25A 122.0(8) . . ?
N21A C26A H26A 119.0 . . ?
C25A C26A H26A 119.0 . . ?
O2 Cl1 O1 109.0(2) . . ?
O2 Cl1 O3 108.9(2) . . ?
O3 Cl1 O1 109.8(2) . . ?
O4 Cl1 O1 110.1(2) . . ?
O4 Cl1 O2 109.6(3) . . ?
O4 Cl1 O3 109.3(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O14 C14 C13 146.7(10) . . . . ?
Cu1 O14 C14 C15 -26.7(11) . . . . ?
Cu1 O14 C14A C13A 149.6(7) . . . . ?
Cu1 O14 C14A C15A -35.5(10) . . . . ?
Cu1 O24 C24 C23 127.2(14) . . . . ?
Cu1 O24 C24 C25 -45.6(15) . . . . ?
Cu1 O24 C24A C23A 132.7(6) . . . . ?
Cu1 O24 C24A C25A -51.4(10) . . . . ?
Cu1 N1 C1 C2 -179.8(3) . . . 3_665 ?
Cu1 N1 C2 C1 179.8(3) . . . 3_665 ?
Cu1 N3 C4 C5 177.9(3) . . . . ?
Cu1 N3 C8 C7 -177.7(3) . . . . ?
Cu1 N6 C5 C4 -176.3(3) 1_565 . . . ?
Cu1 N6 C7 C8 176.3(3) 1_565 . . . ?
O14 C14 C15 C16 178.6(11) . . . . ?
O14 C14A C15A C16A -175.5(8) . . . . ?
O24 C24 C25 C26 179.5(19) . . . . ?
O24 C24A C25A C26A -177.9(8) . . . . ?
N3 C4 C5 N6 -0.8(7) . . . . ?
N6 C7 C8 N3 0.6(7) . . . . ?
C1 N1 C2 C1 0.7(7) . . . 3_665 ?
C2 N1 C1 C2 -0.7(7) . . . 3_665 ?
C4 N3 C8 C7 0.1(6) . . . . ?
C5 N6 C7 C8 -1.3(6) . . . . ?
C7 N6 C5 C4 1.4(6) . . . . ?
C8 N3 C4 C5 0.0(6) . . . . ?
Br1 C13 C14 O14 1.3(17) . . . . ?
Br1 C13 C14 C15 175.2(11) . . . . ?
Br2 C23 C24 O24 3(2) . . . . ?
Br2 C23 C24 C25 175.8(16) . . . . ?
N11 C12 C13 Br1 -177.6(11) . . . . ?
N11 C12 C13 C14 2(2) . . . . ?
N21 C22 C23 Br2 -177.7(15) . . . . ?
N21 C22 C23 C24 5(3) . . . . ?
C12 N11 C16 C15 -1.4(18) . . . . ?
C12 C13 C14 O14 -178.5(11) . . . . ?
C12 C13 C14 C15 -5(2) . . . . ?
C13 C14 C15 C16 4(2) . . . . ?
C14 C15 C16 N11 -2(2) . . . . ?
C16 N11 C12 C13 1.2(19) . . . . ?
C22 N21 C26 C25 0(3) . . . . ?
C22 C23 C24 O24 179.9(14) . . . . ?
C22 C23 C24 C25 -7(3) . . . . ?
C23 C24 C25 C26 6(3) . . . . ?
C24 C25 C26 N21 -2(3) . . . . ?
C26 N21 C22 C23 -1(3) . . . . ?
Br1A C13A C14A O14 -4.1(13) . . . . ?
Br1A C13A C14A C15A -179.4(9) . . . . ?
Br2A C23A C24A O24 -0.7(11) . . . . ?
Br2A C23A C24A C25A -177.1(8) . . . . ?
N11A C12A C13A Br1A 179.2(8) . . . . ?
N11A C12A C13A C14A -1.0(17) . . . . ?
N21A C22A C23A Br2A 178.1(7) . . . . ?
N21A C22A C23A C24A -2.2(14) . . . . ?
C12A N11A C16A C15A -1.5(15) . . . . ?
C12A C13A C14A O14 176.1(9) . . . . ?
C12A C13A C14A C15A 0.8(17) . . . . ?
C13A C14A C15A C16A -0.9(16) . . . . ?
C14A C15A C16A N11A 1.2(17) . . . . ?
C16A N11A C12A C13A 1.4(15) . . . . ?
C22A N21A C26A C25A 1.7(13) . . . . ?
C22A C23A C24A O24 179.5(8) . . . . ?
C22A C23A C24A C25A 3.2(14) . . . . ?
C23A C24A C25A C26A -1.9(15) . . . . ?
C24A C25A C26A N21A -0.5(16) . . . . ?
C26A N21A C22A C23A -0.3(12) . . . . ?

# start Validation Reply Form
_vrf_PLAT242_jcmaa_sq            
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Cl1 Check 
RESPONSE: Cl1 is part of a perchlorate anion. As such, this is not a case
of misassigned atom-type.
;
_vrf_PLAT420_jcmaa_sq            
;
PROBLEM: D-H Without Acceptor       N11A     --H11A     .     Please Check 
RESPONSE: The model was treated using a solvent mask. As such, acceptor
molecules may have been removed using PLATON SQUEEZE.
;
_vrf_PLAT906_jcmaa_sq            
;
PROBLEM: Large K Value in the Analysis of Variance ......      3.435 Check 
RESPONSE: This value of K is associated with the weakest Fc/Fc(max) group 
(0.000 - 0.014). The next largest value of K was associated with the next
weakest Fc/Fc(max) group (1.632 for 0.014 - 0.025). All other values of
K ranged from 0.996 to 1.129.
;
_vrf_PLAT910_jcmaa_sq            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).          9 Note  
RESPONSE: These may have been partially obstructed by the beamstop. They
represent a very small number of reflections compared with the total 
number that were collected.
;
_vrf_PLAT002_jcmaa_sq            
;
PROBLEM: Number of Distance or Angle Restraints on AtSite         30 Note   
RESPONSE: Two fully disordered ligands were present. These were modeled
using distance restraints and displacement constraints. 
;
_vrf_PLAT004_jcmaa_sq            
;
PROBLEM: Polymeric Structure Found with Maximum Dimension          1 Info   
RESPONSE: This is confirmed. 
;
_vrf_PLAT007_jcmaa_sq            
;
PROBLEM: Number of Unrefined Donor-H Atoms ..............          4 Report   
RESPONSE: Since the hydrogen atoms were associated with the fully disordered
ligands, these were introduced in calculated positions and refined on a 
riding
model. 
;
_vrf_PLAT042_jcmaa_sq            
;
PROBLEM: Calc. and Reported MoietyFormula Strings  Differ     Please Check   
RESPONSE: The reported formula differentiates the perchlorate anion from
the rest of the structure.
;
_vrf_PLAT083_jcmaa_sq            
;
PROBLEM: SHELXL Second Parameter in WGHT  Unusually Large      14.91 Why ?  
RESPONSE: This may have been due to the inclusion of some weak, high angle
data.
;
_vrf_PLAT168_jcmaa_sq            
;
PROBLEM: The CIF-Embedded .res File Contains EXYZ Records          2 Report 
RESPONSE: The model includes two fully disordered ligands. The atoms on the 
"pivot" site for the disorder (C14A and C24A) were split, with refined 
occupancy.
The atoms were constrained to have the same positions as their minor disorder
components (C14 and C24). 
;
_vrf_PLAT171_jcmaa_sq            
;
PROBLEM: The CIF-Embedded .res File Contains EADP Records          4 Report
RESPONSE: The model includes two fully disordered ligands. The atoms in these
groups were contrained to have identical anisotropic displacements.
;
_vrf_PLAT176_jcmaa_sq            
;
PROBLEM: The CIF-Embedded .res File Contains SADI Records          8 Report
RESPONSE: The model includes two fully disordered ligands. The atoms in 
these
groups were treated with similar distance restraints on bonds.
;
_vrf_PLAT301_jcmaa_sq            
;
PROBLEM: Main Residue  Disorder ..............(Resd  1  )        45% Note
RESPONSE: This is consistent with the presence of two fully disordered 
ligands.
;
_vrf_PLAT605_jcmaa_sq            
;
PROBLEM: Largest Solvent Accessible VOID in the Structure        364 A**3
RESPONSE: A badly disordered perchlorate anion was treated using a solvent
maks (PLATON SQUEEZE).
;
_vrf_PLAT811_jcmaa_sq            
;
PROBLEM: No ADDSYM Analysis: Too Many Excluded Atoms ....          ! Info 
RESPONSE: This is noted.
;
_vrf_PLAT860_jcmaa_sq            
;
PROBLEM: Number of Least-Squares Restraints .............         72 Note   
RESPONSE: Two fully disordered ligands were present. These were modeled
using distance restraints and displacement constraints. 
;
_vrf_PLAT869_jcmaa_sq            
;
PROBLEM: ALERTS Related to the Use of SQUEEZE Suppressed           ! Info
RESPONSE: A badly disordered perchlorate anion was treated using a solvent
maks (PLATON SQUEEZE).
;
_vrf_PLAT870_jcmaa_sq            
;
PROBLEM: ALERTS Related to Twinning Effects Suppressed ..          ! Info
RESPONSE: A minor twin contribution was considered (hklf5), but refinement
using the hklf4 file yielded more satisfactory statistics.
;
_vrf_PLAT941_jcmaa_sq            
;
PROBLEM: Average HKL Measurement Multiplicity ...........        3.2 Low
RESPONSE: This is noted.
;
_vrf_PLAT975_jcmaa_sq            
;
PROBLEM: Check Calcd Resid. Dens.  0.97A   From O14             0.45 eA-3  
RESPONSE: This has been examined, and is not consistent with a missed 
hydrogen atom, based on charge balance and other supporting 
characterizations.
;
_vrf_PLAT977_jcmaa_sq            
;
PROBLEM: Check Negative Difference Density on H21A             -0.34 eA-3 
RESPONSE: This is a partial occupancy hydrogen atom, which is required
for charge balance. It is consistent with other supporting 
characterizations.
;
_vrf_PLAT933_jcmaa_sq            
;
PROBLEM: Number of OMIT Records in Embedded .res File ...          1 Note
RESPONSE: One disagreeable reflection was omitted from the refinement.
;
_vrf_PLAT978_jcmaa_sq            
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          8 Info
RESPONSE: This is consistent with a good model.
;
# end Validation Reply Form
_exptl_crystal_preparation       'Magnetic properties'
