# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_cl041
_database_code_depnum_ccdc_archive 'CCDC 1055605'
_audit_update_record             
;
2015-03-23 deposited with the CCDC.
2015-06-10 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT026_cl041               
;
PROBLEM: Ratio Observed / Unique Reflections too Low ....         39 %     
RESPONSE: Weakly diffracting crystal with a very thin dimension responsible.
;
_vrf_PLAT029_cl041               
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.958 Note  
RESPONSE: Weakly diffracting crystal with a very thin dimension responsible.
;
_audit_creation_date             2015-02-12
_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[NiL26a]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H24 N4 Ni O6'
_chemical_formula_sum            'C26 H24 N4 Ni O6'
_chemical_formula_weight         547.20

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'
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'
Ni Ni 0.3393 1.1124 '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                   4.084(1)
_cell_length_b                   12.918(3)
_cell_length_c                   22.854(6)
_cell_angle_alpha                101.906(19)
_cell_angle_beta                 91.824(20)
_cell_angle_gamma                93.995(20)
_cell_volume                     1175.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    6147
_cell_measurement_theta_min      1.7
_cell_measurement_theta_max      27.71

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_F_000             568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.059
_exptl_absorpt_coefficient_mu    0.877
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  STOE-STADIVARI
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number            8045
_diffrn_reflns_av_unetI/netI     0.2422
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.681
_diffrn_reflns_theta_max         27.821
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measured_fraction_theta_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_point_group_measured_fraction_full 0.958
_reflns_number_total             4136
_reflns_number_gt                1620
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000


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

_computing_data_collection       X-AREA-STOE
_computing_cell_refinement       X-AREA-STOE
_computing_data_reduction        X-AREA-STOE
_computing_structure_solution    SIR97
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  PLATON

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0092P)²] 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         4136
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1498
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.0884
_refine_ls_wR_factor_gt          0.0720
_refine_ls_goodness_of_fit_ref   0.680
_refine_ls_restrained_S_all      0.680
_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
C1 C 1.2132(15) 0.2203(5) 0.0750(3) 0.0280(15) Uani 1 1 d . . . . .
C2 C 1.3546(13) 0.3221(5) 0.1037(2) 0.0230(14) Uani 1 1 d . . . . .
C3 C 1.2800(14) 0.3702(5) 0.1620(2) 0.0247(15) Uani 1 1 d . . . . .
H3 H 1.3843 0.4388 0.1778 0.030 Uiso 1 1 calc R U . . .
C4 C 1.0236(12) 0.3889(5) 0.2547(2) 0.0255(14) Uani 1 1 d . . . . .
C5 C 1.1341(13) 0.4912(5) 0.2809(3) 0.0325(15) Uani 1 1 d . . . . .
H5 H 1.2637 0.5321 0.2588 0.039 Uiso 1 1 calc R U . . .
C6 C 1.0606(13) 0.5365(5) 0.3393(3) 0.0277(14) Uani 1 1 d . . . . .
C7 C 1.0960(13) 0.6781(5) 0.4197(3) 0.0339(15) Uani 1 1 d . . . . .
C8 C 1.2028(14) 0.7827(5) 0.4483(3) 0.0391(17) Uani 1 1 d . . . . .
H8 H 1.3320 0.8255 0.4272 0.047 Uiso 1 1 calc R U . . .
C9 C 1.1264(14) 0.8238(5) 0.5050(3) 0.0393(16) Uani 1 1 d . . . . .
H9 H 1.2046 0.8945 0.5231 0.047 Uiso 1 1 calc R U . . .
C10 C 0.9305(15) 0.7629(5) 0.5379(3) 0.0411(16) Uani 1 1 d . . . . .
H10 H 0.8771 0.7931 0.5776 0.049 Uiso 1 1 calc R U . . .
C11 C 0.8185(14) 0.6604(5) 0.5123(3) 0.0366(16) Uani 1 1 d . . . . .
H11 H 0.6891 0.6194 0.5343 0.044 Uiso 1 1 calc R U . . .
C12 C 0.8964(15) 0.6163(5) 0.4530(3) 0.0310(16) Uani 1 1 d . . . . .
C13 C 0.8621(13) 0.4759(5) 0.3728(3) 0.0260(14) Uani 1 1 d . . . . .
C14 C 0.7439(13) 0.3700(5) 0.3446(2) 0.0287(13) Uani 1 1 d . . . . .
H14 H 0.6150 0.3281 0.3662 0.034 Uiso 1 1 calc R U . . .
C15 C 0.8132(12) 0.3297(4) 0.2882(2) 0.0240(13) Uani 1 1 d . . . . .
C16 C 0.5044(14) 0.1640(5) 0.2761(3) 0.0253(14) Uani 1 1 d . . . . .
H16 H 0.4528 0.1876 0.3167 0.030 Uiso 1 1 calc R U . . .
C17 C 0.3627(13) 0.0636(4) 0.2465(3) 0.0235(14) Uani 1 1 d . . . . .
C18 C 0.4221(14) 0.0206(5) 0.1870(3) 0.0248(15) Uani 1 1 d . . . . .
C19 C 1.2808(14) 0.1644(4) 0.0131(2) 0.0356(15) Uani 1 1 d . . . . .
H19A H 1.1444 0.0972 0.0026 0.053 Uiso 1 1 calc R U . . .
H19B H 1.5133 0.1503 0.0112 0.053 Uiso 1 1 calc R U . . .
H19C H 1.2290 0.2091 -0.0153 0.053 Uiso 1 1 calc R U . . .
C20 C 1.5809(14) 0.3826(5) 0.0710(3) 0.0279(16) Uani 1 1 d . . . . .
C21 C 1.8879(12) 0.5448(4) 0.0736(2) 0.0265(14) Uani 1 1 d . . . . .
H21A H 1.7539 0.5643 0.0412 0.032 Uiso 1 1 calc R U . . .
H21B H 2.0737 0.5064 0.0555 0.032 Uiso 1 1 calc R U . . .
C22 C 2.0155(14) 0.6436(4) 0.1187(2) 0.0375(15) Uani 1 1 d . . . . .
H22A H 1.8298 0.6797 0.1372 0.056 Uiso 1 1 calc R U . . .
H22B H 2.1444 0.6913 0.0984 0.056 Uiso 1 1 calc R U . . .
H22C H 2.1547 0.6237 0.1497 0.056 Uiso 1 1 calc R U . . .
C23 C 0.2735(13) -0.0833(4) 0.1513(2) 0.0348(14) Uani 1 1 d . . . . .
H23A H 0.3638 -0.0968 0.1115 0.052 Uiso 1 1 calc R U . . .
H23B H 0.0346 -0.0811 0.1474 0.052 Uiso 1 1 calc R U . . .
H23C H 0.3248 -0.1403 0.1718 0.052 Uiso 1 1 calc R U . . .
C24 C 0.1554(15) 0.0143(5) 0.2870(3) 0.0322(16) Uani 1 1 d . . . . .
C25 C -0.1554(14) -0.1385(5) 0.3037(3) 0.0336(15) Uani 1 1 d . . . . .
H25A H -0.3355 -0.0952 0.3199 0.040 Uiso 1 1 calc R U . . .
H25B H -0.0097 -0.1467 0.3377 0.040 Uiso 1 1 calc R U . . .
C26 C -0.2941(14) -0.2452(5) 0.2699(3) 0.0413(16) Uani 1 1 d . . . . .
H26A H -0.4429 -0.2364 0.2371 0.062 Uiso 1 1 calc R U . . .
H26B H -0.4154 -0.2819 0.2969 0.062 Uiso 1 1 calc R U . . .
H26C H -0.1146 -0.2872 0.2535 0.062 Uiso 1 1 calc R U . . .
N1 N 1.0818(11) 0.3303(4) 0.1969(2) 0.0242(11) Uani 1 1 d . . . . .
N2 N 0.7004(11) 0.2278(4) 0.25303(19) 0.0238(11) Uani 1 1 d . . . . .
N3 N 1.1733(11) 0.6375(4) 0.3637(2) 0.0298(12) Uani 1 1 d . . . . .
N4 N 0.7805(11) 0.5152(4) 0.4290(2) 0.0345(13) Uani 1 1 d . . . . .
O1 O 1.0109(9) 0.1662(3) 0.10129(16) 0.0276(9) Uani 1 1 d . . . . .
O2 O 0.6179(9) 0.0686(3) 0.15704(16) 0.0278(10) Uani 1 1 d . . . . .
O3 O 1.6604(9) 0.3535(3) 0.02004(17) 0.0323(10) Uani 1 1 d . . . . .
O4 O 1.6891(8) 0.4783(3) 0.10498(16) 0.0288(10) Uani 1 1 d . . . . .
O5 O 0.1001(10) 0.0568(3) 0.33729(18) 0.0414(12) Uani 1 1 d . . . . .
O6 O 0.0293(9) -0.0861(3) 0.26338(17) 0.0301(10) Uani 1 1 d . . . . .
Ni1 Ni 0.8533(2) 0.19932(7) 0.17766(4) 0.0276(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.287(6) . ?
C1 C2 1.417(8) . ?
C1 C19 1.493(8) . ?
C2 C3 1.402(8) . ?
C2 C20 1.485(8) . ?
C3 N1 1.308(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(7) . ?
C4 N1 1.417(7) . ?
C4 C15 1.451(7) . ?
C5 C6 1.393(8) . ?
C5 H5 0.9500 . ?
C6 N3 1.351(7) . ?
C6 C13 1.432(7) . ?
C7 N3 1.336(7) . ?
C7 C8 1.407(8) . ?
C7 C12 1.442(8) . ?
C8 C9 1.349(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.421(8) . ?
C9 H9 0.9500 . ?
C10 C11 1.372(8) . ?
C10 H10 0.9500 . ?
C11 C12 1.412(8) . ?
C11 H11 0.9500 . ?
C12 N4 1.354(7) . ?
C13 N4 1.342(7) . ?
C13 C14 1.429(7) . ?
C14 C15 1.334(7) . ?
C14 H14 0.9500 . ?
C15 N2 1.431(7) . ?
C16 N2 1.308(6) . ?
C16 C17 1.408(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.394(8) . ?
C17 C24 1.483(8) . ?
C18 O2 1.278(6) . ?
C18 C23 1.496(7) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 O3 1.210(6) . ?
C20 O4 1.354(7) . ?
C21 O4 1.452(5) . ?
C21 C22 1.514(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 O5 1.203(7) . ?
C24 O6 1.356(7) . ?
C25 O6 1.451(6) . ?
C25 C26 1.498(8) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
N1 Ni1 1.836(5) . ?
N2 Ni1 1.825(4) . ?
O1 Ni1 1.856(4) . ?
O2 Ni1 1.847(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
O1 C1 C2 121.8(5) . . ?
O1 C1 C19 113.3(6) . . ?
C2 C1 C19 124.9(6) . . ?
C3 C2 C1 122.0(6) . . ?
C3 C2 C20 118.1(6) . . ?
C1 C2 C20 119.9(5) . . ?
N1 C3 C2 126.7(6) . . ?
N1 C3 H3 116.7 . . ?
C2 C3 H3 116.7 . . ?
C5 C4 N1 128.7(5) . . ?
C5 C4 C15 118.4(5) . . ?
N1 C4 C15 112.9(5) . . ?
C4 C5 C6 121.4(5) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
N3 C6 C5 119.8(5) . . ?
N3 C6 C13 120.5(5) . . ?
C5 C6 C13 119.7(6) . . ?
N3 C7 C8 121.5(6) . . ?
N3 C7 C12 121.1(6) . . ?
C8 C7 C12 117.4(6) . . ?
C9 C8 C7 121.7(6) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C8 C9 C10 120.9(6) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 120.0(6) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 119.7(6) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
N4 C12 C11 118.2(6) . . ?
N4 C12 C7 121.6(5) . . ?
C11 C12 C7 120.2(6) . . ?
N4 C13 C14 119.0(5) . . ?
N4 C13 C6 122.5(6) . . ?
C14 C13 C6 118.4(5) . . ?
C15 C14 C13 120.5(5) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 N2 127.2(5) . . ?
C14 C15 C4 121.5(5) . . ?
N2 C15 C4 111.3(5) . . ?
N2 C16 C17 126.2(5) . . ?
N2 C16 H16 116.9 . . ?
C17 C16 H16 116.9 . . ?
C18 C17 C16 121.9(5) . . ?
C18 C17 C24 127.1(6) . . ?
C16 C17 C24 110.9(6) . . ?
O2 C18 C17 121.7(6) . . ?
O2 C18 C23 112.7(5) . . ?
C17 C18 C23 125.7(5) . . ?
C1 C19 H19A 109.5 . . ?
C1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O3 C20 O4 122.3(6) . . ?
O3 C20 C2 125.9(6) . . ?
O4 C20 C2 111.7(5) . . ?
O4 C21 C22 107.7(4) . . ?
O4 C21 H21A 110.2 . . ?
C22 C21 H21A 110.2 . . ?
O4 C21 H21B 110.2 . . ?
C22 C21 H21B 110.2 . . ?
H21A C21 H21B 108.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O5 C24 O6 120.7(6) . . ?
O5 C24 C17 124.5(6) . . ?
O6 C24 C17 114.7(6) . . ?
O6 C25 C26 108.8(5) . . ?
O6 C25 H25A 109.9 . . ?
C26 C25 H25A 109.9 . . ?
O6 C25 H25B 109.9 . . ?
C26 C25 H25B 109.9 . . ?
H25A C25 H25B 108.3 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C3 N1 C4 120.7(5) . . ?
C3 N1 Ni1 125.4(4) . . ?
C4 N1 Ni1 113.9(4) . . ?
C16 N2 C15 119.6(4) . . ?
C16 N2 Ni1 125.8(4) . . ?
C15 N2 Ni1 114.7(3) . . ?
C7 N3 C6 117.9(5) . . ?
C13 N4 C12 116.4(5) . . ?
C1 O1 Ni1 129.9(4) . . ?
C18 O2 Ni1 130.9(4) . . ?
C20 O4 C21 114.1(4) . . ?
C24 O6 C25 115.5(5) . . ?
N2 Ni1 N1 87.1(2) . . ?
N2 Ni1 O2 93.44(19) . . ?
N1 Ni1 O2 178.7(2) . . ?
N2 Ni1 O1 178.3(2) . . ?
N1 Ni1 O1 94.15(19) . . ?
O2 Ni1 O1 85.33(18) . . ?

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
O1 C1 C2 C3 -0.6(8) . . . . ?
C19 C1 C2 C3 179.9(5) . . . . ?
O1 C1 C2 C20 -178.6(5) . . . . ?
C19 C1 C2 C20 1.9(8) . . . . ?
C1 C2 C3 N1 0.5(9) . . . . ?
C20 C2 C3 N1 178.5(5) . . . . ?
N1 C4 C5 C6 -178.3(5) . . . . ?
C15 C4 C5 C6 2.9(7) . . . . ?
C4 C5 C6 N3 -179.9(5) . . . . ?
C4 C5 C6 C13 -0.8(8) . . . . ?
N3 C7 C8 C9 -179.8(5) . . . . ?
C12 C7 C8 C9 0.9(8) . . . . ?
C7 C8 C9 C10 -0.7(9) . . . . ?
C8 C9 C10 C11 0.6(8) . . . . ?
C9 C10 C11 C12 -0.5(8) . . . . ?
C10 C11 C12 N4 -179.6(5) . . . . ?
C10 C11 C12 C7 0.7(8) . . . . ?
N3 C7 C12 N4 0.1(8) . . . . ?
C8 C7 C12 N4 179.5(5) . . . . ?
N3 C7 C12 C11 179.8(6) . . . . ?
C8 C7 C12 C11 -0.9(7) . . . . ?
N3 C6 C13 N4 -0.3(7) . . . . ?
C5 C6 C13 N4 -179.5(6) . . . . ?
N3 C6 C13 C14 178.9(5) . . . . ?
C5 C6 C13 C14 -0.3(7) . . . . ?
N4 C13 C14 C15 178.2(5) . . . . ?
C6 C13 C14 C15 -1.1(7) . . . . ?
C13 C14 C15 N2 -176.6(4) . . . . ?
C13 C14 C15 C4 3.4(7) . . . . ?
C5 C4 C15 C14 -4.3(7) . . . . ?
N1 C4 C15 C14 176.7(5) . . . . ?
C5 C4 C15 N2 175.7(4) . . . . ?
N1 C4 C15 N2 -3.3(5) . . . . ?
N2 C16 C17 C18 0.3(9) . . . . ?
N2 C16 C17 C24 179.8(5) . . . . ?
C16 C17 C18 O2 2.6(8) . . . . ?
C24 C17 C18 O2 -176.8(5) . . . . ?
C16 C17 C18 C23 -177.7(5) . . . . ?
C24 C17 C18 C23 2.9(9) . . . . ?
C3 C2 C20 O3 -177.5(5) . . . . ?
C1 C2 C20 O3 0.5(8) . . . . ?
C3 C2 C20 O4 1.2(6) . . . . ?
C1 C2 C20 O4 179.3(5) . . . . ?
C18 C17 C24 O5 -176.5(6) . . . . ?
C16 C17 C24 O5 4.1(8) . . . . ?
C18 C17 C24 O6 4.2(8) . . . . ?
C16 C17 C24 O6 -175.3(5) . . . . ?
C2 C3 N1 C4 -178.6(5) . . . . ?
C2 C3 N1 Ni1 0.5(7) . . . . ?
C5 C4 N1 C3 4.6(8) . . . . ?
C15 C4 N1 C3 -176.5(4) . . . . ?
C5 C4 N1 Ni1 -174.7(4) . . . . ?
C15 C4 N1 Ni1 4.2(5) . . . . ?
C17 C16 N2 C15 177.2(5) . . . . ?
C17 C16 N2 Ni1 -3.0(8) . . . . ?
C14 C15 N2 C16 0.7(8) . . . . ?
C4 C15 N2 C16 -179.2(4) . . . . ?
C14 C15 N2 Ni1 -179.0(4) . . . . ?
C4 C15 N2 Ni1 1.0(5) . . . . ?
C8 C7 N3 C6 -179.8(5) . . . . ?
C12 C7 N3 C6 -0.5(7) . . . . ?
C5 C6 N3 C7 179.7(5) . . . . ?
C13 C6 N3 C7 0.6(7) . . . . ?
C14 C13 N4 C12 -179.2(5) . . . . ?
C6 C13 N4 C12 0.0(7) . . . . ?
C11 C12 N4 C13 -179.5(5) . . . . ?
C7 C12 N4 C13 0.1(8) . . . . ?
C2 C1 O1 Ni1 -0.3(8) . . . . ?
C19 C1 O1 Ni1 179.3(4) . . . . ?
C17 C18 O2 Ni1 -2.6(8) . . . . ?
C23 C18 O2 Ni1 177.7(3) . . . . ?
O3 C20 O4 C21 4.0(7) . . . . ?
C2 C20 O4 C21 -174.8(4) . . . . ?
C22 C21 O4 C20 -174.7(4) . . . . ?
O5 C24 O6 C25 -3.5(8) . . . . ?
C17 C24 O6 C25 175.9(4) . . . . ?
C26 C25 O6 C24 176.6(5) . . . . ?
C16 N2 Ni1 N1 -178.6(4) . . . . ?
C15 N2 Ni1 N1 1.1(3) . . . . ?
C16 N2 Ni1 O2 2.5(4) . . . . ?
C15 N2 Ni1 O2 -177.8(3) . . . . ?
C3 N1 Ni1 N2 177.8(4) . . . . ?
C4 N1 Ni1 N2 -3.0(4) . . . . ?
C3 N1 Ni1 O1 -1.0(4) . . . . ?
C4 N1 Ni1 O1 178.2(3) . . . . ?
C18 O2 Ni1 N2 0.2(4) . . . . ?
C18 O2 Ni1 O1 179.0(4) . . . . ?
C1 O1 Ni1 N1 0.9(4) . . . . ?
C1 O1 Ni1 O2 179.8(4) . . . . ?

_refine_diff_density_max         0.369
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.082



####################################################################### 
# 
# 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_cl043
_database_code_depnum_ccdc_archive 'CCDC 1055606'
_audit_update_record             
;
2015-03-23 deposited with the CCDC.
2015-06-10 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_cl043               
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.958 Note  
RESPONSE: small crystal badly diffracting.
;
_audit_creation_date             2015-02-12
_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[CuL26a(EtOH)]2CHCl3'
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H32 Cl6 Cu N4 O7'
_chemical_formula_sum            'C30 H32 Cl6 Cu N4 O7'
_chemical_formula_weight         836.83

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

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

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

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

_cell_length_a                   8.651(1)
_cell_length_b                   11.798(2)
_cell_length_c                   18.199(3)
_cell_angle_alpha                71.833(11)
_cell_angle_beta                 86.734(12)
_cell_angle_gamma                88.122(12)
_cell_volume                     1761.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9058
_cell_measurement_theta_min      1.18
_cell_measurement_theta_max      27.25

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_F_000             854
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.084
_exptl_absorpt_coefficient_mu    1.126
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  STOE-STADIVARI
_diffrn_measurement_method       omega-scan
_diffrn_detector_area_resol_mean 9
_diffrn_reflns_number            14806
_diffrn_reflns_av_unetI/netI     0.1677
_diffrn_reflns_av_R_equivalents  0.1731
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.179
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measured_fraction_theta_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_point_group_measured_fraction_full 0.958
_reflns_number_total             7594
_reflns_number_gt                3682
_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       X-AREA-STOE
_computing_cell_refinement       X-AREA-STOE
_computing_data_reduction        X-AREA-STOE
_computing_structure_solution    SIR97
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ORTEP-III
_computing_publication_material  PLATON

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] 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         7594
_refine_ls_number_parameters     434
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1779
_refine_ls_R_factor_gt           0.1176
_refine_ls_wR_factor_ref         0.3478
_refine_ls_wR_factor_gt          0.2963
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_restrained_S_all      0.988
_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
C1 C 0.6727(9) 0.9328(7) 0.4072(5) 0.0435(18) Uani 1 1 d . . . . .
C2 C 0.7582(9) 0.8867(6) 0.3530(4) 0.0377(15) Uani 1 1 d . . . . .
C3 C 0.9050(9) 0.8321(6) 0.3688(4) 0.0391(16) Uani 1 1 d . . . . .
H3 H 0.9544 0.8047 0.3293 0.047 Uiso 1 1 calc R U . . .
C4 C 1.1309(8) 0.7667(6) 0.4378(4) 0.0363(15) Uani 1 1 d . . . . .
C5 C 1.2100(9) 0.7220(7) 0.3846(5) 0.0427(17) Uani 1 1 d . . . . .
H5 H 1.1617 0.7219 0.3391 0.051 Uiso 1 1 calc R U . . .
C6 C 1.3639(9) 0.6761(6) 0.3977(5) 0.0390(16) Uani 1 1 d . . . . .
C7 C 1.5828(9) 0.5960(7) 0.3570(5) 0.0421(17) Uani 1 1 d . . . . .
C8 C 1.6674(9) 0.5540(6) 0.3006(5) 0.0430(17) Uani 1 1 d . . . . .
H8 H 1.6217 0.5560 0.2539 0.052 Uiso 1 1 calc R U . . .
C9 C 1.8132(10) 0.5114(7) 0.3145(5) 0.051(2) Uani 1 1 d . . . . .
H9 H 1.8672 0.4799 0.2781 0.061 Uiso 1 1 calc R U . . .
C10 C 1.8886(10) 0.5120(6) 0.3815(5) 0.0459(18) Uani 1 1 d . . . . .
H10 H 1.9925 0.4837 0.3886 0.055 Uiso 1 1 calc R U . . .
C11 C 1.8111(9) 0.5538(6) 0.4364(5) 0.0436(17) Uani 1 1 d . . . . .
H11 H 1.8603 0.5525 0.4820 0.052 Uiso 1 1 calc R U . . .
C12 C 1.6567(9) 0.5988(6) 0.4244(5) 0.0403(17) Uani 1 1 d . . . . .
C13 C 1.4365(9) 0.6823(6) 0.4643(5) 0.0402(16) Uani 1 1 d . . . . .
C14 C 1.3530(9) 0.7275(6) 0.5190(4) 0.0383(16) Uani 1 1 d . . . . .
H14 H 1.4011 0.7295 0.5643 0.046 Uiso 1 1 calc R U . . .
C15 C 1.2062(8) 0.7676(6) 0.5070(4) 0.0357(15) Uani 1 1 d . . . . .
C16 C 1.1544(9) 0.8003(7) 0.6289(4) 0.0403(16) Uani 1 1 d . . . . .
H16 H 1.2535 0.7654 0.6424 0.048 Uiso 1 1 calc R U . . .
C17 C 1.0684(9) 0.8380(7) 0.6847(5) 0.0438(18) Uani 1 1 d . . . . .
C18 C 0.9235(9) 0.8993(6) 0.6716(5) 0.0405(17) Uani 1 1 d . . . . .
C19 C 0.5217(10) 0.9997(7) 0.3877(5) 0.0487(19) Uani 1 1 d . . . . .
H19A H 0.4396 0.9431 0.3901 0.073 Uiso 1 1 calc R U . . .
H19B H 0.5314 1.0564 0.3353 0.073 Uiso 1 1 calc R U . . .
H19C H 0.4959 1.0430 0.4248 0.073 Uiso 1 1 calc R U . . .
C20 C 0.6897(10) 0.8906(7) 0.2796(5) 0.0480(19) Uani 1 1 d . . . . .
C23 C 0.8405(11) 0.9521(7) 0.7285(5) 0.0493(19) Uani 1 1 d . . . . .
H23A H 0.7600 1.0082 0.7025 0.074 Uiso 1 1 calc R U . . .
H23B H 0.9146 0.9942 0.7490 0.074 Uiso 1 1 calc R U . . .
H23C H 0.7929 0.8881 0.7712 0.074 Uiso 1 1 calc R U . . .
C24 C 1.1369(10) 0.8173(8) 0.7604(5) 0.0484(19) Uani 1 1 d . . . . .
C25 C 1.3608(13) 0.7472(11) 0.8349(6) 0.071(3) Uani 1 1 d . . . . .
H25A H 1.3227 0.8021 0.8636 0.086 Uiso 1 1 calc R U . . .
H25B H 1.4739 0.7574 0.8247 0.086 Uiso 1 1 calc R U . . .
C26 C 1.3279(16) 0.6224(13) 0.8818(8) 0.093(4) Uani 1 1 d . . . . .
H26A H 1.2162 0.6091 0.8846 0.140 Uiso 1 1 calc R U . . .
H26B H 1.3636 0.6077 0.9342 0.140 Uiso 1 1 calc R U . . .
H26C H 1.3821 0.5677 0.8577 0.140 Uiso 1 1 calc R U . . .
C51 C 0.7638(12) 0.6193(8) 0.6688(7) 0.066(3) Uani 1 1 d . . . . .
H51A H 0.7516 0.5324 0.6798 0.079 Uiso 1 1 calc R U . . .
H51B H 0.8576 0.6317 0.6939 0.079 Uiso 1 1 calc R U . . .
C52 C 0.6304(12) 0.6672(10) 0.7010(7) 0.072(3) Uani 1 1 d . . . . .
H52A H 0.6353 0.7544 0.6844 0.107 Uiso 1 1 calc R U . . .
H52B H 0.6293 0.6364 0.7577 0.107 Uiso 1 1 calc R U . . .
H52C H 0.5358 0.6432 0.6830 0.107 Uiso 1 1 calc R U . . .
C61 C 1.3039(14) 0.7400(12) 1.1685(7) 0.081(3) Uani 1 1 d . . . . .
H61 H 1.3594 0.7291 1.2170 0.097 Uiso 1 1 calc R U . . .
C71 C 0.8371(15) 0.7212(11) 0.9457(7) 0.076(3) Uani 1 1 d . . . . .
H71 H 0.9015 0.7799 0.9049 0.092 Uiso 1 1 calc R U . . .
N1 N 0.9820(7) 0.8145(5) 0.4322(4) 0.0381(13) Uani 1 1 d . . . . .
N2 N 1.1097(7) 0.8090(5) 0.5590(4) 0.0352(13) Uani 1 1 d . . . . .
N3 N 1.4358(7) 0.6351(5) 0.3438(4) 0.0407(14) Uani 1 1 d . . . . .
N4 N 1.5814(7) 0.6392(5) 0.4794(4) 0.0386(13) Uani 1 1 d . . . . .
O1 O 0.7220(6) 0.9284(4) 0.4737(3) 0.0458(13) Uani 1 1 d . . . . .
O2 O 0.8573(6) 0.9200(4) 0.6078(3) 0.0411(12) Uani 1 1 d . . . . .
O3 O 0.5592(8) 0.9114(8) 0.2638(4) 0.075(2) Uani 1 1 d . . . . .
O4 O 0.7951(8) 0.8666(8) 0.2304(4) 0.077(2) Uani 1 1 d . . . . .
O5 O 1.0738(8) 0.8304(6) 0.8176(4) 0.0654(18) Uani 1 1 d . . . . .
O6 O 1.2837(8) 0.7759(7) 0.7610(4) 0.0665(18) Uani 1 1 d . . . . .
O51 O 0.7838(6) 0.6755(4) 0.5858(3) 0.0431(12) Uani 1 1 d . . . . .
H51 H 0.7444 0.6328 0.5628 0.065 Uiso 1 1 calc R U . . .
Cl61 Cl 1.3956(5) 0.6529(4) 1.1189(2) 0.1080(12) Uani 1 1 d . . . . .
Cl62 Cl 1.3088(5) 0.8905(3) 1.1147(3) 0.1148(13) Uani 1 1 d . . . . .
Cl63 Cl 1.1100(4) 0.6942(4) 1.19498(18) 0.0968(11) Uani 1 1 d . . . . .
Cl71 Cl 0.9385(6) 0.6779(4) 1.0289(3) 0.1260(15) Uani 1 1 d . . . . .
Cl72 Cl 0.8034(6) 0.6001(4) 0.9120(3) 0.1272(16) Uani 1 1 d . . . . .
Cl73 Cl 0.6637(4) 0.7913(4) 0.9587(3) 0.1054(12) Uani 1 1 d . . . . .
Cu1 Cu 0.90770(11) 0.85944(8) 0.52139(5) 0.0388(3) Uani 1 1 d . . . . .
C21 C 0.7463(13) 0.8688(17) 0.1548(7) 0.096(5) Uani 1 1 d . . . . .
H21A H 0.6349 0.8903 0.1504 0.115 Uiso 1 1 calc R U . . .
H21B H 0.7618 0.7889 0.1484 0.115 Uiso 1 1 calc R U . . .
C22 C 0.840(3) 0.9591(12) 0.0931(8) 0.145(9) Uani 1 1 d . . . . .
H22A H 0.8520 1.0305 0.1087 0.218 Uiso 1 1 calc R U . . .
H22B H 0.7875 0.9806 0.0443 0.218 Uiso 1 1 calc R U . . .
H22C H 0.9428 0.9249 0.0860 0.218 Uiso 1 1 calc R 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
C1 O1 1.292(10) . ?
C1 C2 1.428(10) . ?
C1 C19 1.505(11) . ?
C2 C3 1.409(11) . ?
C2 C20 1.479(12) . ?
C3 N1 1.323(10) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(9) . ?
C4 N1 1.385(9) . ?
C4 C15 1.453(11) . ?
C5 C6 1.425(11) . ?
C5 H5 0.9500 . ?
C6 N3 1.338(9) . ?
C6 C13 1.419(11) . ?
C7 N3 1.348(10) . ?
C7 C12 1.425(11) . ?
C7 C8 1.430(9) . ?
C8 C9 1.351(12) . ?
C8 H8 0.9500 . ?
C9 C10 1.417(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.377(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.424(11) . ?
C11 H11 0.9500 . ?
C12 N4 1.362(9) . ?
C13 N4 1.347(10) . ?
C13 C14 1.423(9) . ?
C14 C15 1.346(10) . ?
C14 H14 0.9500 . ?
C15 N2 1.415(8) . ?
C16 N2 1.323(10) . ?
C16 C17 1.397(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.421(11) . ?
C17 C24 1.478(12) . ?
C18 O2 1.275(10) . ?
C18 C23 1.505(10) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 O3 1.180(11) . ?
C20 O4 1.328(10) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 O5 1.197(10) . ?
C24 O6 1.345(10) . ?
C25 O6 1.473(12) . ?
C25 C26 1.481(18) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C51 C52 1.443(14) . ?
C51 O51 1.450(13) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C61 Cl61 1.715(11) . ?
C61 Cl62 1.740(14) . ?
C61 Cl63 1.773(13) . ?
C61 H61 1.0000 . ?
C71 Cl71 1.721(13) . ?
C71 Cl73 1.729(12) . ?
C71 Cl72 1.760(12) . ?
C71 H71 1.0000 . ?
N1 Cu1 1.930(6) . ?
N2 Cu1 1.921(6) . ?
O1 Cu1 1.905(6) . ?
O2 Cu1 1.943(5) . ?
O4 C21 1.453(13) . ?
O51 Cu1 2.378(5) . ?
O51 H51 0.8400 . ?
C21 C22 1.51(2) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 123.6(7) . . ?
O1 C1 C19 114.6(7) . . ?
C2 C1 C19 121.6(8) . . ?
C3 C2 C1 121.8(7) . . ?
C3 C2 C20 118.2(6) . . ?
C1 C2 C20 120.0(7) . . ?
N1 C3 C2 127.4(7) . . ?
N1 C3 H3 116.3 . . ?
C2 C3 H3 116.3 . . ?
C5 C4 N1 126.3(7) . . ?
C5 C4 C15 119.5(7) . . ?
N1 C4 C15 114.2(6) . . ?
C4 C5 C6 120.3(7) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
N3 C6 C13 123.2(7) . . ?
N3 C6 C5 117.8(7) . . ?
C13 C6 C5 118.9(6) . . ?
N3 C7 C12 121.7(6) . . ?
N3 C7 C8 118.7(7) . . ?
C12 C7 C8 119.6(7) . . ?
C9 C8 C7 119.0(8) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C8 C9 C10 122.4(7) . . ?
C8 C9 H9 118.8 . . ?
C10 C9 H9 118.8 . . ?
C11 C10 C9 119.9(8) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 119.7(8) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
N4 C12 C11 119.0(7) . . ?
N4 C12 C7 121.7(7) . . ?
C11 C12 C7 119.3(7) . . ?
N4 C13 C6 121.0(6) . . ?
N4 C13 C14 118.7(7) . . ?
C6 C13 C14 120.1(7) . . ?
C15 C14 C13 120.3(7) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 N2 125.2(7) . . ?
C14 C15 C4 120.8(6) . . ?
N2 C15 C4 113.9(6) . . ?
N2 C16 C17 125.7(8) . . ?
N2 C16 H16 117.2 . . ?
C17 C16 H16 117.2 . . ?
C16 C17 C18 124.0(8) . . ?
C16 C17 C24 117.5(7) . . ?
C18 C17 C24 118.5(7) . . ?
O2 C18 C17 121.9(6) . . ?
O2 C18 C23 114.3(7) . . ?
C17 C18 C23 123.6(8) . . ?
C1 C19 H19A 109.5 . . ?
C1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O3 C20 O4 121.7(9) . . ?
O3 C20 C2 126.9(8) . . ?
O4 C20 C2 111.4(7) . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O5 C24 O6 120.9(8) . . ?
O5 C24 C17 126.8(8) . . ?
O6 C24 C17 112.3(7) . . ?
O6 C25 C26 109.6(11) . . ?
O6 C25 H25A 109.7 . . ?
C26 C25 H25A 109.7 . . ?
O6 C25 H25B 109.7 . . ?
C26 C25 H25B 109.7 . . ?
H25A C25 H25B 108.2 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C52 C51 O51 111.7(9) . . ?
C52 C51 H51A 109.3 . . ?
O51 C51 H51A 109.3 . . ?
C52 C51 H51B 109.3 . . ?
O51 C51 H51B 109.3 . . ?
H51A C51 H51B 107.9 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
Cl61 C61 Cl62 111.6(7) . . ?
Cl61 C61 Cl63 110.5(8) . . ?
Cl62 C61 Cl63 110.4(6) . . ?
Cl61 C61 H61 108.1 . . ?
Cl62 C61 H61 108.1 . . ?
Cl63 C61 H61 108.1 . . ?
Cl71 C71 Cl73 111.7(6) . . ?
Cl71 C71 Cl72 111.8(7) . . ?
Cl73 C71 Cl72 110.0(7) . . ?
Cl71 C71 H71 107.7 . . ?
Cl73 C71 H71 107.7 . . ?
Cl72 C71 H71 107.7 . . ?
C3 N1 C4 121.3(6) . . ?
C3 N1 Cu1 124.8(5) . . ?
C4 N1 Cu1 113.8(5) . . ?
C16 N2 C15 121.0(6) . . ?
C16 N2 Cu1 125.6(5) . . ?
C15 N2 Cu1 113.1(5) . . ?
C6 N3 C7 116.0(7) . . ?
C13 N4 C12 116.2(7) . . ?
C1 O1 Cu1 129.8(5) . . ?
C18 O2 Cu1 129.6(5) . . ?
C20 O4 C21 118.1(8) . . ?
C24 O6 C25 116.8(7) . . ?
C51 O51 Cu1 126.7(5) . . ?
C51 O51 H51 109.5 . . ?
Cu1 O51 H51 123.8 . . ?
O1 Cu1 N2 171.8(2) . . ?
O1 Cu1 N1 92.5(3) . . ?
N2 Cu1 N1 84.8(3) . . ?
O1 Cu1 O2 90.7(2) . . ?
N2 Cu1 O2 90.9(2) . . ?
N1 Cu1 O2 171.9(2) . . ?
O1 Cu1 O51 91.8(2) . . ?
N2 Cu1 O51 96.1(2) . . ?
N1 Cu1 O51 95.3(2) . . ?
O2 Cu1 O51 92.0(2) . . ?
O4 C21 C22 109.0(12) . . ?
O4 C21 H21A 109.9 . . ?
C22 C21 H21A 109.9 . . ?
O4 C21 H21B 109.9 . . ?
C22 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

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
O1 C1 C2 C3 0.1(11) . . . . ?
C19 C1 C2 C3 175.1(7) . . . . ?
O1 C1 C2 C20 177.2(7) . . . . ?
C19 C1 C2 C20 -7.8(11) . . . . ?
C1 C2 C3 N1 0.7(12) . . . . ?
C20 C2 C3 N1 -176.4(7) . . . . ?
N1 C4 C5 C6 179.6(7) . . . . ?
C15 C4 C5 C6 0.6(11) . . . . ?
C4 C5 C6 N3 -179.3(7) . . . . ?
C4 C5 C6 C13 -3.0(11) . . . . ?
N3 C7 C8 C9 -178.0(7) . . . . ?
C12 C7 C8 C9 3.7(11) . . . . ?
C7 C8 C9 C10 -3.1(12) . . . . ?
C8 C9 C10 C11 2.0(12) . . . . ?
C9 C10 C11 C12 -1.5(11) . . . . ?
C10 C11 C12 N4 179.7(6) . . . . ?
C10 C11 C12 C7 2.2(11) . . . . ?
N3 C7 C12 N4 1.1(12) . . . . ?
C8 C7 C12 N4 179.3(6) . . . . ?
N3 C7 C12 C11 178.5(7) . . . . ?
C8 C7 C12 C11 -3.3(11) . . . . ?
N3 C6 C13 N4 -4.4(11) . . . . ?
C5 C6 C13 N4 179.5(7) . . . . ?
N3 C6 C13 C14 179.7(6) . . . . ?
C5 C6 C13 C14 3.6(11) . . . . ?
N4 C13 C14 C15 -177.8(7) . . . . ?
C6 C13 C14 C15 -1.8(11) . . . . ?
C13 C14 C15 N2 176.8(6) . . . . ?
C13 C14 C15 C4 -0.7(10) . . . . ?
C5 C4 C15 C14 1.3(10) . . . . ?
N1 C4 C15 C14 -177.8(6) . . . . ?
C5 C4 C15 N2 -176.4(6) . . . . ?
N1 C4 C15 N2 4.5(9) . . . . ?
N2 C16 C17 C18 -4.7(12) . . . . ?
N2 C16 C17 C24 178.3(7) . . . . ?
C16 C17 C18 O2 3.2(12) . . . . ?
C24 C17 C18 O2 -179.8(7) . . . . ?
C16 C17 C18 C23 -172.7(7) . . . . ?
C24 C17 C18 C23 4.4(11) . . . . ?
C3 C2 C20 O3 164.4(9) . . . . ?
C1 C2 C20 O3 -12.7(13) . . . . ?
C3 C2 C20 O4 -15.3(10) . . . . ?
C1 C2 C20 O4 167.5(7) . . . . ?
C16 C17 C24 O5 -170.6(8) . . . . ?
C18 C17 C24 O5 12.2(13) . . . . ?
C16 C17 C24 O6 7.1(11) . . . . ?
C18 C17 C24 O6 -170.1(7) . . . . ?
C2 C3 N1 C4 -175.5(6) . . . . ?
C2 C3 N1 Cu1 0.8(11) . . . . ?
C5 C4 N1 C3 -6.6(11) . . . . ?
C15 C4 N1 C3 172.4(6) . . . . ?
C5 C4 N1 Cu1 176.8(6) . . . . ?
C15 C4 N1 Cu1 -4.2(7) . . . . ?
C17 C16 N2 C15 -179.9(7) . . . . ?
C17 C16 N2 Cu1 -7.2(11) . . . . ?
C14 C15 N2 C16 -6.7(10) . . . . ?
C4 C15 N2 C16 170.9(6) . . . . ?
C14 C15 N2 Cu1 179.8(6) . . . . ?
C4 C15 N2 Cu1 -2.6(7) . . . . ?
C13 C6 N3 C7 1.8(11) . . . . ?
C5 C6 N3 C7 177.9(6) . . . . ?
C12 C7 N3 C6 -0.2(11) . . . . ?
C8 C7 N3 C6 -178.4(7) . . . . ?
C6 C13 N4 C12 5.1(10) . . . . ?
C14 C13 N4 C12 -179.0(6) . . . . ?
C11 C12 N4 C13 179.1(6) . . . . ?
C7 C12 N4 C13 -3.5(10) . . . . ?
C2 C1 O1 Cu1 -2.4(11) . . . . ?
C19 C1 O1 Cu1 -177.7(5) . . . . ?
C17 C18 O2 Cu1 10.2(10) . . . . ?
C23 C18 O2 Cu1 -173.5(5) . . . . ?
O3 C20 O4 C21 1.2(16) . . . . ?
C2 C20 O4 C21 -179.0(10) . . . . ?
O5 C24 O6 C25 0.5(14) . . . . ?
C17 C24 O6 C25 -177.4(8) . . . . ?
C26 C25 O6 C24 87.8(11) . . . . ?
C52 C51 O51 Cu1 83.3(9) . . . . ?
C20 O4 C21 C22 121.3(12) . . . . ?

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
C5 H5 Cl63 0.95 2.80 3.720(8) 162.2 1_554
C19 H19C O1 0.98 2.65 3.484(9) 143.1 2_676
C21 H21A Cl62 0.99 2.93 3.881(12) 161.2 1_454
C22 H22A O5 0.98 2.54 3.484(15) 162.3 2_776
C22 H22B Cl62 0.98 2.97 3.916(15) 162.4 2_776
C61 H61 N3 1.00 2.35 3.297(14) 157.8 1_556
C71 H71 O5 1.00 2.07 3.008(15) 154.7 .
O51 H51 N4 0.84 2.11 2.821(9) 141.8 1_455
C5 H5 Cl63 0.95 2.80 3.720(8) 162.2 1_554
C19 H19C O1 0.98 2.65 3.484(9) 143.1 2_676
C61 H61 N3 1.00 2.35 3.297(14) 157.8 1_556
C71 H71 O5 1.00 2.07 3.008(15) 154.7 .
O51 H51 N4 0.84 2.11 2.821(9) 141.8 1_455

_refine_diff_density_max         1.649
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.188

_shelxl_version_number           2014-3



