# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_p
_database_code_depnum_ccdc_archive 'CCDC 969850'
_audit_update_record             
;
2015-04-24 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H40 Cl2 Fe2 N6 O6'
_chemical_formula_weight         907.40

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 1.000 0.500 184 47 ' '
2 0.500 0.500 0.000 184 47 ' '
_platon_squeeze_details          
;
;

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'
Fe Fe 0.3463 0.8444 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   8.736(4)
_cell_length_b                   20.255(9)
_cell_length_c                   12.610(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.847(15)
_cell_angle_gamma                90.00
_cell_volume                     2219.7(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2406
_cell_measurement_theta_min      2.550
_cell_measurement_theta_max      23.660

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.6645
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11635
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3858
_reflns_number_gt                2746
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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     
'calc w=1/[σ²(Fo²)+(0.0412P)²+0.0000P] 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         3858
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.0952
_refine_ls_wR_factor_gt          0.0871
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.44684(4) 0.108726(19) 1.04897(3) 0.03176(15) Uani 1 1 d . . .
Cl1 Cl 0.54300(9) 0.20233(4) 1.16393(6) 0.0466(2) Uani 1 1 d . . .
O1 O 0.3500(2) 0.03163(9) 0.94361(14) 0.0370(5) Uani 1 1 d . . .
O2 O 0.4592(2) -0.04233(9) 0.84653(14) 0.0459(5) Uani 1 1 d . . .
O3 O 0.3406(3) 0.17163(11) 0.49010(16) 0.0656(7) Uani 1 1 d . . .
N1 N 0.3142(2) 0.17909(11) 0.93506(17) 0.0344(6) Uani 1 1 d . . .
N2 N 0.2197(3) 0.11428(11) 1.10467(18) 0.0375(6) Uani 1 1 d . . .
N3 N 0.6036(2) 0.13326(11) 0.93292(17) 0.0325(6) Uani 1 1 d . . .
C1 C 0.1595(3) 0.07008(15) 1.1671(2) 0.0431(8) Uani 1 1 d . . .
H1A H 0.2200 0.0347 1.1930 0.052 Uiso 1 1 calc R . .
C2 C 0.0119(4) 0.07483(17) 1.1945(2) 0.0544(9) Uani 1 1 d . . .
H2A H -0.0269 0.0432 1.2380 0.065 Uiso 1 1 calc R . .
C3 C -0.0776(4) 0.12713(19) 1.1566(3) 0.0567(10) Uani 1 1 d . . .
H3A H -0.1775 0.1318 1.1749 0.068 Uiso 1 1 calc R . .
C4 C -0.0178(3) 0.17219(16) 1.0918(2) 0.0453(8) Uani 1 1 d . . .
H4A H -0.0771 0.2076 1.0645 0.054 Uiso 1 1 calc R . .
C5 C 0.1315(3) 0.16472(15) 1.0673(2) 0.0388(7) Uani 1 1 d . . .
C6 C 0.2093(3) 0.21329(14) 1.0011(2) 0.0432(8) Uani 1 1 d . . .
H6A H 0.1324 0.2374 0.9555 0.052 Uiso 1 1 calc R . .
H6B H 0.2670 0.2448 1.0474 0.052 Uiso 1 1 calc R . .
C7 C 0.5689(3) 0.18662(14) 0.8739(2) 0.0360(7) Uani 1 1 d . . .
C8 C 0.6591(4) 0.20701(16) 0.7965(2) 0.0508(9) Uani 1 1 d . . .
H8A H 0.6346 0.2451 0.7573 0.061 Uiso 1 1 calc R . .
C9 C 0.7859(4) 0.17000(18) 0.7783(3) 0.0585(9) Uani 1 1 d . . .
H9A H 0.8493 0.1831 0.7272 0.070 Uiso 1 1 calc R . .
C10 C 0.8174(3) 0.11394(16) 0.8361(2) 0.0475(8) Uani 1 1 d . . .
H10A H 0.9004 0.0874 0.8232 0.057 Uiso 1 1 calc R . .
C11 C 0.7254(3) 0.09716(14) 0.9131(2) 0.0391(7) Uani 1 1 d . . .
H11A H 0.7485 0.0593 0.9533 0.047 Uiso 1 1 calc R . .
C12 C 0.4286(3) 0.22424(13) 0.8976(2) 0.0429(8) Uani 1 1 d . . .
H12A H 0.4570 0.2572 0.9518 0.051 Uiso 1 1 calc R . .
H12B H 0.3847 0.2468 0.8338 0.051 Uiso 1 1 calc R . .
C13 C 0.2181(3) 0.14622(14) 0.8458(2) 0.0384(7) Uani 1 1 d . . .
H13A H 0.1444 0.1782 0.8143 0.046 Uiso 1 1 calc R . .
H13B H 0.1601 0.1112 0.8757 0.046 Uiso 1 1 calc R . .
C14 C 0.3015(3) 0.11720(14) 0.7581(2) 0.0334(7) Uani 1 1 d . . .
C15 C 0.2914(3) 0.15329(14) 0.6646(2) 0.0417(8) Uani 1 1 d . . .
H15A H 0.2375 0.1930 0.6607 0.050 Uiso 1 1 calc R . .
C16 C 0.3596(4) 0.13154(15) 0.5769(2) 0.0458(8) Uani 1 1 d . . .
C17 C 0.4391(4) 0.07305(16) 0.5822(2) 0.0515(9) Uani 1 1 d . . .
H17A H 0.4871 0.0583 0.5241 0.062 Uiso 1 1 calc R . .
C18 C 0.4471(4) 0.03654(15) 0.6742(2) 0.0461(8) Uani 1 1 d . . .
H18A H 0.4995 -0.0035 0.6766 0.055 Uiso 1 1 calc R . .
C19 C 0.3804(3) 0.05687(13) 0.7631(2) 0.0333(7) Uani 1 1 d . . .
C20 C 0.3970(3) 0.01300(14) 0.8588(2) 0.0356(7) Uani 1 1 d . . .
C21 C 0.3921(5) 0.14771(18) 0.3940(2) 0.0823(13) Uani 1 1 d . . .
H21A H 0.3776 0.1812 0.3400 0.124 Uiso 1 1 calc R . .
H21B H 0.3343 0.1091 0.3710 0.124 Uiso 1 1 calc R . .
H21C H 0.4994 0.1367 0.4061 0.124 Uiso 1 1 calc R . .


_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
Fe1 O2 2.000(2) 3_657 ?
Fe1 N3 2.162(2) . ?
Fe1 O1 2.166(2) . ?
Fe1 N2 2.175(2) . ?
Fe1 N1 2.258(2) . ?
Fe1 Cl1 2.4806(11) . ?
O1 C20 1.243(3) . ?
O2 C20 1.262(3) . ?
O2 Fe1 2.000(2) 3_657 ?
O3 C16 1.359(3) . ?
O3 C21 1.420(4) . ?
N1 C12 1.468(3) . ?
N1 C6 1.472(3) . ?
N1 C13 1.490(3) . ?
N2 C1 1.335(3) . ?
N2 C5 1.336(3) . ?
N3 C7 1.329(3) . ?
N3 C11 1.336(3) . ?
C1 C2 1.372(4) . ?
C2 C3 1.373(4) . ?
C3 C4 1.364(4) . ?
C4 C5 1.379(4) . ?
C5 C6 1.497(4) . ?
C7 C8 1.379(4) . ?
C7 C12 1.499(4) . ?
C8 C9 1.376(4) . ?
C9 C10 1.362(4) . ?
C10 C11 1.365(4) . ?
C13 C14 1.504(4) . ?
C14 C15 1.383(4) . ?
C14 C19 1.401(4) . ?
C15 C16 1.381(4) . ?
C16 C17 1.371(4) . ?
C17 C18 1.371(4) . ?
C18 C19 1.379(4) . ?
C19 C20 1.493(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
O2 Fe1 N3 110.79(9) 3_657 . ?
O2 Fe1 O1 91.59(8) 3_657 . ?
N3 Fe1 O1 89.15(8) . . ?
O2 Fe1 N2 98.56(9) 3_657 . ?
N3 Fe1 N2 150.32(9) . . ?
O1 Fe1 N2 85.60(8) . . ?
O2 Fe1 N1 173.40(8) 3_657 . ?
N3 Fe1 N1 75.15(9) . . ?
O1 Fe1 N1 85.52(8) . . ?
N2 Fe1 N1 75.32(9) . . ?
O2 Fe1 Cl1 92.12(7) 3_657 . ?
N3 Fe1 Cl1 91.13(6) . . ?
O1 Fe1 Cl1 175.91(5) . . ?
N2 Fe1 Cl1 92.16(7) . . ?
N1 Fe1 Cl1 90.61(7) . . ?
C20 O1 Fe1 127.19(18) . . ?
C20 O2 Fe1 132.04(19) . 3_657 ?
C16 O3 C21 117.4(2) . . ?
C12 N1 C6 111.9(2) . . ?
C12 N1 C13 112.6(2) . . ?
C6 N1 C13 107.6(2) . . ?
C12 N1 Fe1 105.99(17) . . ?
C6 N1 Fe1 104.22(16) . . ?
C13 N1 Fe1 114.28(16) . . ?
C1 N2 C5 118.2(3) . . ?
C1 N2 Fe1 125.7(2) . . ?
C5 N2 Fe1 115.97(19) . . ?
C7 N3 C11 118.8(2) . . ?
C7 N3 Fe1 116.21(18) . . ?
C11 N3 Fe1 124.92(19) . . ?
N2 C1 C2 122.6(3) . . ?
C3 C2 C1 118.9(3) . . ?
C2 C3 C4 119.1(3) . . ?
C3 C4 C5 119.3(3) . . ?
N2 C5 C4 122.0(3) . . ?
N2 C5 C6 114.9(3) . . ?
C4 C5 C6 123.1(3) . . ?
N1 C6 C5 110.5(2) . . ?
N3 C7 C8 121.7(3) . . ?
N3 C7 C12 116.5(2) . . ?
C8 C7 C12 121.8(3) . . ?
C9 C8 C7 118.9(3) . . ?
C10 C9 C8 119.1(3) . . ?
C9 C10 C11 119.2(3) . . ?
N3 C11 C10 122.3(3) . . ?
N1 C12 C7 110.2(2) . . ?
N1 C13 C14 116.9(2) . . ?
C15 C14 C19 119.2(3) . . ?
C15 C14 C13 115.3(2) . . ?
C19 C14 C13 125.5(3) . . ?
C14 C15 C16 121.3(3) . . ?
O3 C16 C17 125.1(3) . . ?
O3 C16 C15 115.3(3) . . ?
C17 C16 C15 119.6(3) . . ?
C16 C17 C18 119.3(3) . . ?
C17 C18 C19 122.5(3) . . ?
C18 C19 C14 118.1(3) . . ?
C18 C19 C20 117.7(3) . . ?
C14 C19 C20 124.2(3) . . ?
O1 C20 O2 124.0(3) . . ?
O1 C20 C19 120.1(3) . . ?
O2 C20 C19 115.9(3) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.054
####################################################################### 
# 
# 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_p
_database_code_depnum_ccdc_archive 'CCDC 969851'
_audit_update_record             
;
2015-04-24 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H43 Cl Fe2 N6 O9'
_chemical_formula_weight         946.99

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.094 245 99 ' '
2 0.000 0.500 0.344 245 98 ' '
3 0.000 0.000 0.594 245 98 ' '
4 0.000 0.500 0.844 245 99 ' '
5 0.500 0.000 0.344 245 99 ' '
6 0.500 0.000 0.844 245 98 ' '
7 0.500 0.500 0.094 245 98 ' '
8 0.500 0.500 0.594 245 99 ' '
_platon_squeeze_details          
;
;

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)cd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x, -y, z+1/2'
'-x+1/2, y+1/2, z'
'-y, -x+1/2, z+3/4'
'y+1/2, x, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'
'x+1/2, -y+1/2, z+1'
'-x+1, y+1, z+1/2'
'-y+1/2, -x+1, z+5/4'
'y+1, x+1/2, z+3/4'

_cell_length_a                   16.545(5)
_cell_length_b                   16.545(5)
_cell_length_c                   36.72(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10052(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2779
_cell_measurement_theta_min      2.454
_cell_measurement_theta_max      20.342

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3920
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.6641
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26254
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         24.99
_reflns_number_total             4245
_reflns_number_gt                2730
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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     
'calc w=1/[σ²(Fo²)+(0.1415P)²+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_number_reflns         4245
_refine_ls_number_parameters     282
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0757
_refine_ls_wR_factor_ref         0.2150
_refine_ls_wR_factor_gt          0.1976
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.996
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe -0.00163(5) 0.90127(5) 0.76649(6) 0.0563(3) Uani 1 1 d . . .
Cl Cl 0.0000 1.0000 0.94799(8) 0.0696(8) Uani 1 2 d S . .
O1 O -0.1144(3) 0.8645(3) 0.77467(17) 0.0686(14) Uani 1 1 d . . .
O2 O -0.2447(3) 0.8485(3) 0.7689(2) 0.0887(18) Uani 1 1 d . . .
O3 O -0.1424(5) 0.7531(6) 0.6098(3) 0.125(3) Uani 1 1 d . . .
O4 O -0.0213(3) 0.9362(3) 0.71400(17) 0.0687(14) Uani 1 1 d . . .
O5 O 0.0000 1.0000 0.7874(2) 0.0574(17) Uani 1 2 d S . .
N1 N 0.0244(4) 0.7741(3) 0.7439(2) 0.0625(16) Uani 1 1 d . . .
N2 N 0.0305(4) 0.8347(4) 0.8137(2) 0.0706(18) Uani 1 1 d . . .
N3 N 0.1247(3) 0.8989(4) 0.7499(2) 0.0647(17) Uani 1 1 d . . .
C1 C 0.0677(5) 0.7257(4) 0.7726(3) 0.076(2) Uani 1 1 d . . .
H1A H 0.0519 0.6693 0.7708 0.092 Uiso 1 1 calc R . .
H1B H 0.1256 0.7290 0.7687 0.092 Uiso 1 1 calc R . .
C2 C 0.0473(5) 0.7573(5) 0.8098(3) 0.074(2) Uani 1 1 d . . .
C3 C 0.0533(6) 0.7065(6) 0.8415(4) 0.105(4) Uani 1 1 d . . .
H3A H 0.0668 0.6522 0.8392 0.126 Uiso 1 1 calc R . .
C4 C 0.0389(10) 0.7385(7) 0.8745(4) 0.120(4) Uani 1 1 d . . .
H4A H 0.0390 0.7047 0.8948 0.144 Uiso 1 1 calc R . .
C5 C 0.0249(8) 0.8147(7) 0.8791(3) 0.098(3) Uani 1 1 d . . .
H5B H 0.0196 0.8369 0.9023 0.117 Uiso 1 1 calc R . .
C6 C 0.0179(6) 0.8620(7) 0.8480(3) 0.091(3) Uani 1 1 d . . .
H6A H 0.0037 0.9160 0.8509 0.109 Uiso 1 1 calc R . .
C7 C 0.0810(5) 0.7879(4) 0.7132(2) 0.070(2) Uani 1 1 d . . .
H7A H 0.1057 0.7371 0.7062 0.083 Uiso 1 1 calc R . .
H7B H 0.0514 0.8087 0.6924 0.083 Uiso 1 1 calc R . .
C8 C 0.1445(5) 0.8459(5) 0.7236(3) 0.070(2) Uani 1 1 d . . .
C9 C 0.2209(5) 0.8465(5) 0.7091(3) 0.075(2) Uani 1 1 d . . .
H9A H 0.2351 0.8092 0.6912 0.090 Uiso 1 1 calc R . .
C10 C 0.2773(5) 0.9033(5) 0.7212(3) 0.073(2) Uani 1 1 d . . .
H10A H 0.3288 0.9047 0.7111 0.087 Uiso 1 1 calc R . .
C11 C 0.2566(4) 0.9566(5) 0.7479(3) 0.081(3) Uani 1 1 d . . .
H11A H 0.2934 0.9952 0.7560 0.098 Uiso 1 1 calc R . .
C12 C 0.1788(4) 0.9522(4) 0.7629(3) 0.073(2) Uani 1 1 d . . .
H12A H 0.1645 0.9863 0.7821 0.087 Uiso 1 1 calc R . .
C13 C -0.0496(4) 0.7296(4) 0.7331(3) 0.075(3) Uani 1 1 d D . .
H13A H -0.0331 0.6784 0.7227 0.090 Uiso 1 1 calc R . .
H13B H -0.0798 0.7176 0.7551 0.090 Uiso 1 1 calc R . .
C14 C -0.1048(5) 0.7686(4) 0.7074(2) 0.069(2) Uani 1 1 d D . .
C15 C -0.1025(5) 0.7439(5) 0.6700(3) 0.075(2) Uani 1 1 d . . .
H15A H -0.0667 0.7034 0.6630 0.090 Uiso 1 1 calc R . .
C16 C -0.1509(6) 0.7778(7) 0.6448(3) 0.091(3) Uani 1 1 d . . .
C17 C -0.2090(6) 0.8310(6) 0.6551(3) 0.090(3) Uani 1 1 d U . .
H17A H -0.2427 0.8542 0.6377 0.108 Uiso 1 1 calc R . .
C18 C -0.2184(5) 0.8514(5) 0.6928(3) 0.071(2) Uani 1 1 d U . .
H18A H -0.2602 0.8852 0.7003 0.085 Uiso 1 1 calc R . .
C19 C -0.1661(4) 0.8209(4) 0.7173(2) 0.066(2) Uani 1 1 d . . .
C20 C -0.1751(4) 0.8465(4) 0.7558(3) 0.069(2) Uani 1 1 d . . .
C21 C -0.1957(10) 0.7792(10) 0.5818(4) 0.137(5) Uani 1 1 d . . .
H21A H -0.1792 0.7561 0.5590 0.205 Uiso 1 1 calc R . .
H21B H -0.1942 0.8370 0.5802 0.205 Uiso 1 1 calc R . .
H21C H -0.2497 0.7620 0.5874 0.205 Uiso 1 1 calc R . .
C22 C 0.0000 1.0000 0.6983(4) 0.064(3) Uani 1 2 d S . .
C23 C 0.0000 1.0000 0.6579(4) 0.078(3) Uani 1 2 d S . .
H23A H 0.0181 1.0516 0.6492 0.117 Uiso 0.50 1 calc PR . .
H23B H -0.0538 0.9899 0.6492 0.117 Uiso 0.50 1 calc PR . .
H23C H 0.0357 0.9585 0.6492 0.117 Uiso 0.50 1 calc PR . .


_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
Fe1 O5 1.804(3) . ?
Fe1 O1 1.985(5) . ?
Fe1 O4 2.039(7) . ?
Fe1 N2 2.122(8) . ?
Fe1 N3 2.177(6) . ?
Fe1 N1 2.303(6) . ?
O1 C20 1.254(9) . ?
O2 C20 1.250(9) . ?
O3 C16 1.357(14) . ?
O3 C21 1.420(14) . ?
O4 C22 1.253(9) . ?
O5 Fe1 1.804(3) 10_464 ?
N1 C7 1.482(10) . ?
N1 C13 1.483(9) . ?
N1 C1 1.506(10) . ?
N2 C2 1.319(10) . ?
N2 C6 1.353(13) . ?
N3 C12 1.345(9) . ?
N3 C8 1.344(11) . ?
C1 C2 1.500(13) . ?
C2 C3 1.440(14) . ?
C3 C4 1.344(17) . ?
C4 C5 1.293(16) . ?
C5 C6 1.390(14) . ?
C7 C8 1.472(11) . ?
C8 C9 1.374(11) . ?
C9 C10 1.397(12) . ?
C10 C11 1.362(12) . ?
C11 C12 1.404(11) . ?
C13 C14 1.463(10) . ?
C14 C19 1.383(11) . ?
C14 C15 1.433(13) . ?
C15 C16 1.347(13) . ?
C16 C17 1.357(14) . ?
C17 C18 1.434(14) . ?
C18 C19 1.346(12) . ?
C19 C20 1.484(12) . ?
C22 O4 1.253(9) 10_464 ?
C22 C23 1.485(19) . ?

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
O5 Fe1 O1 103.12(16) . . ?
O5 Fe1 O4 98.5(3) . . ?
O1 Fe1 O4 94.6(2) . . ?
O5 Fe1 N2 96.8(3) . . ?
O1 Fe1 N2 87.3(3) . . ?
O4 Fe1 N2 163.7(3) . . ?
O5 Fe1 N3 96.94(18) . . ?
O1 Fe1 N3 159.9(2) . . ?
O4 Fe1 N3 83.9(3) . . ?
N2 Fe1 N3 88.8(3) . . ?
O5 Fe1 N1 167.81(18) . . ?
O1 Fe1 N1 87.2(2) . . ?
O4 Fe1 N1 87.0(2) . . ?
N2 Fe1 N1 76.9(3) . . ?
N3 Fe1 N1 72.7(2) . . ?
C20 O1 Fe1 137.8(6) . . ?
C16 O3 C21 121.9(10) . . ?
C22 O4 Fe1 129.0(7) . . ?
Fe1 O5 Fe1 129.8(4) . 10_464 ?
C7 N1 C13 113.3(7) . . ?
C7 N1 C1 108.3(6) . . ?
C13 N1 C1 108.4(6) . . ?
C7 N1 Fe1 104.6(4) . . ?
C13 N1 Fe1 113.2(4) . . ?
C1 N1 Fe1 108.8(5) . . ?
C2 N2 C6 117.3(8) . . ?
C2 N2 Fe1 117.9(6) . . ?
C6 N2 Fe1 123.2(6) . . ?
C12 N3 C8 121.4(7) . . ?
C12 N3 Fe1 121.8(5) . . ?
C8 N3 Fe1 116.5(5) . . ?
C2 C1 N1 110.2(6) . . ?
N2 C2 C3 119.5(9) . . ?
N2 C2 C1 119.0(7) . . ?
C3 C2 C1 121.2(8) . . ?
C4 C3 C2 119.2(9) . . ?
C5 C4 C3 122.3(11) . . ?
C4 C5 C6 117.2(11) . . ?
N2 C6 C5 124.3(11) . . ?
C8 C7 N1 110.7(7) . . ?
N3 C8 C9 119.9(8) . . ?
N3 C8 C7 115.9(7) . . ?
C9 C8 C7 124.1(8) . . ?
C8 C9 C10 119.7(9) . . ?
C11 C10 C9 119.9(8) . . ?
C10 C11 C12 118.7(8) . . ?
N3 C12 C11 120.3(8) . . ?
C14 C13 N1 117.9(6) . . ?
C19 C14 C15 116.8(8) . . ?
C19 C14 C13 124.3(8) . . ?
C15 C14 C13 118.4(7) . . ?
C16 C15 C14 121.6(9) . . ?
C15 C16 O3 117.7(9) . . ?
C15 C16 C17 120.0(10) . . ?
O3 C16 C17 122.2(9) . . ?
C16 C17 C18 119.9(9) . . ?
C19 C18 C17 119.2(8) . . ?
C18 C19 C14 122.0(9) . . ?
C18 C19 C20 117.8(7) . . ?
C14 C19 C20 120.2(8) . . ?
O2 C20 O1 121.3(9) . . ?
O2 C20 C19 117.8(8) . . ?
O1 C20 C19 120.9(7) . . ?
O4 C22 O4 125.2(13) 10_464 . ?
O4 C22 C23 117.4(7) 10_464 . ?
O4 C22 C23 117.4(7) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.321
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.110
####################################################################### 
# 
# 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_p
_database_code_depnum_ccdc_archive 'CCDC 969852'
_audit_update_record             
;
2015-04-24 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H40 Cl2 Co2 N6 O6'
_chemical_formula_weight         913.56

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 186 42 ' '
2 0.500 0.000 0.500 186 42 ' '
_platon_squeeze_details          
;
;


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'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   8.726(5)
_cell_length_b                   20.348(11)
_cell_length_c                   12.677(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.148(10)
_cell_angle_gamma                90.00
_cell_volume                     2238(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1785
_cell_measurement_theta_min      2.552
_cell_measurement_theta_max      22.202

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             940
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.6598
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12698
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3939
_reflns_number_gt                2933
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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     
'calc w=1/[σ²(Fo²)+(0.0327P)²+0.0000P] 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         3939
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0808
_refine_ls_wR_factor_gt          0.0762
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.94717(4) 0.110228(15) 0.04647(3) 0.03171(12) Uani 1 1 d . . .
Cl1 Cl 1.04582(8) 0.20095(3) 0.16392(5) 0.04530(19) Uani 1 1 d . . .
O1 O 0.85186(19) 0.03246(7) -0.05330(13) 0.0361(4) Uani 1 1 d . . .
O2 O 0.9556(2) -0.04302(8) -0.15133(13) 0.0443(5) Uani 1 1 d . . .
O3 O 0.8469(3) 0.17223(9) -0.50771(15) 0.0628(6) Uani 1 1 d . . .
N1 N 0.8181(2) 0.17954(9) -0.06185(16) 0.0348(5) Uani 1 1 d . . .
N2 N 0.7270(2) 0.11360(10) 0.10734(17) 0.0371(5) Uani 1 1 d . . .
N3 N 1.1081(2) 0.13221(9) -0.06378(16) 0.0335(5) Uani 1 1 d . . .
C1 C 0.7125(3) 0.21330(12) 0.0045(2) 0.0423(7) Uani 1 1 d . . .
H9A H 0.6342 0.2368 -0.0406 0.051 Uiso 1 1 calc R . .
H9B H 0.7699 0.2450 0.0503 0.051 Uiso 1 1 calc R . .
C2 C 0.6368(3) 0.16418(12) 0.0713(2) 0.0382(6) Uani 1 1 d . . .
C3 C 0.4863(3) 0.17103(14) 0.0967(2) 0.0453(7) Uani 1 1 d . . .
H11A H 0.4261 0.2064 0.0707 0.054 Uiso 1 1 calc R . .
C4 C 0.4278(3) 0.12496(16) 0.1607(2) 0.0562(8) Uani 1 1 d . . .
H12A H 0.3278 0.1289 0.1789 0.067 Uiso 1 1 calc R . .
C5 C 0.5192(3) 0.07295(15) 0.1976(2) 0.0543(8) Uani 1 1 d . . .
H13A H 0.4816 0.0409 0.2404 0.065 Uiso 1 1 calc R . .
C6 C 0.6681(3) 0.06912(13) 0.1697(2) 0.0437(7) Uani 1 1 d . . .
H14A H 0.7299 0.0342 0.1953 0.052 Uiso 1 1 calc R . .
C7 C 0.9344(3) 0.22443(12) -0.0990(2) 0.0420(7) Uani 1 1 d . . .
H15A H 0.9637 0.2571 -0.0448 0.050 Uiso 1 1 calc R . .
H15B H 0.8906 0.2472 -0.1624 0.050 Uiso 1 1 calc R . .
C8 C 1.0749(3) 0.18634(12) -0.1229(2) 0.0378(6) Uani 1 1 d . . .
C9 C 1.1667(3) 0.20606(14) -0.1998(2) 0.0492(7) Uani 1 1 d . . .
H17A H 1.1431 0.2442 -0.2386 0.059 Uiso 1 1 calc R . .
C10 C 1.2929(3) 0.16892(15) -0.2185(2) 0.0566(8) Uani 1 1 d . . .
H18A H 1.3567 0.1819 -0.2689 0.068 Uiso 1 1 calc R . .
C11 C 1.3224(3) 0.11238(14) -0.1610(2) 0.0478(7) Uani 1 1 d . . .
H19A H 1.4045 0.0855 -0.1742 0.057 Uiso 1 1 calc R . .
C12 C 1.2299(3) 0.09552(12) -0.0836(2) 0.0387(6) Uani 1 1 d . . .
H21A H 1.2524 0.0576 -0.0440 0.046 Uiso 1 1 calc R . .
C13 C 0.7218(3) 0.14695(12) -0.1517(2) 0.0390(6) Uani 1 1 d . . .
H8A H 0.6477 0.1789 -0.1828 0.047 Uiso 1 1 calc R . .
H8B H 0.6639 0.1119 -0.1224 0.047 Uiso 1 1 calc R . .
C14 C 0.8043(3) 0.11821(11) -0.2400(2) 0.0339(6) Uani 1 1 d . . .
C15 C 0.7960(3) 0.15396(12) -0.3333(2) 0.0422(7) Uani 1 1 d . . .
H7A H 0.7435 0.1938 -0.3373 0.051 Uiso 1 1 calc R . .
C16 C 0.8638(3) 0.13212(12) -0.4207(2) 0.0452(7) Uani 1 1 d . . .
C17 C 0.9409(3) 0.07268(13) -0.4160(2) 0.0494(7) Uani 1 1 d . . .
H3A H 0.9869 0.0574 -0.4742 0.059 Uiso 1 1 calc R . .
C18 C 0.9485(3) 0.03646(12) -0.3238(2) 0.0440(7) Uani 1 1 d . . .
H4A H 1.0007 -0.0034 -0.3209 0.053 Uiso 1 1 calc R . .
C19 C 0.8815(3) 0.05701(11) -0.23497(19) 0.0333(6) Uani 1 1 d . . .
C20 C 0.8968(3) 0.01287(12) -0.1386(2) 0.0335(6) Uani 1 1 d . . .
C21 C 0.8974(5) 0.14828(16) -0.6038(2) 0.0787(11) Uani 1 1 d . . .
H1A H 0.8823 0.1816 -0.6575 0.118 Uiso 1 1 calc R . .
H1B H 0.8390 0.1099 -0.6266 0.118 Uiso 1 1 calc R . .
H1C H 1.0048 0.1372 -0.5921 0.118 Uiso 1 1 calc R . .


_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
Co1 O2 2.0287(18) 3_755 ?
Co1 N3 2.132(2) . ?
Co1 O1 2.1379(18) . ?
Co1 N2 2.146(2) . ?
Co1 N1 2.194(2) . ?
Co1 Cl1 2.4680(11) . ?
O1 C20 1.254(3) . ?
O2 C20 1.265(3) . ?
O2 Co1 2.0287(18) 3_755 ?
O3 C16 1.367(3) . ?
O3 C21 1.425(3) . ?
N1 C7 1.479(3) . ?
N1 C1 1.482(3) . ?
N1 C13 1.496(3) . ?
N2 C6 1.340(3) . ?
N2 C2 1.346(3) . ?
N3 C8 1.346(3) . ?
N3 C12 1.345(3) . ?
C1 C2 1.507(3) . ?
C2 C3 1.393(4) . ?
C3 C4 1.373(4) . ?
C4 C5 1.376(4) . ?
C5 C6 1.385(4) . ?
C7 C8 1.508(4) . ?
C8 C9 1.386(4) . ?
C9 C10 1.377(4) . ?
C10 C11 1.371(4) . ?
C11 C12 1.379(4) . ?
C13 C14 1.512(3) . ?
C14 C15 1.384(3) . ?
C14 C19 1.414(3) . ?
C15 C16 1.385(4) . ?
C16 C17 1.382(4) . ?
C17 C18 1.378(4) . ?
C18 C19 1.388(3) . ?
C19 C20 1.511(3) . ?

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
O2 Co1 N3 108.20(8) 3_755 . ?
O2 Co1 O1 89.86(8) 3_755 . ?
N3 Co1 O1 90.53(7) . . ?
O2 Co1 N2 96.52(8) 3_755 . ?
N3 Co1 N2 155.03(8) . . ?
O1 Co1 N2 85.98(7) . . ?
O2 Co1 N1 173.86(8) 3_755 . ?
N3 Co1 N1 77.57(8) . . ?
O1 Co1 N1 87.96(8) . . ?
N2 Co1 N1 77.60(8) . . ?
O2 Co1 Cl1 90.83(6) 3_755 . ?
N3 Co1 Cl1 91.54(6) . . ?
O1 Co1 Cl1 177.49(5) . . ?
N2 Co1 Cl1 91.54(6) . . ?
N1 Co1 Cl1 91.10(7) . . ?
C20 O1 Co1 127.41(15) . . ?
C20 O2 Co1 132.02(17) . 3_755 ?
C16 O3 C21 118.0(2) . . ?
C7 N1 C1 112.58(19) . . ?
C7 N1 C13 112.3(2) . . ?
C1 N1 C13 107.8(2) . . ?
C7 N1 Co1 105.81(15) . . ?
C1 N1 Co1 104.55(15) . . ?
C13 N1 Co1 113.61(14) . . ?
C6 N2 C2 118.0(2) . . ?
C6 N2 Co1 127.24(17) . . ?
C2 N2 Co1 114.59(17) . . ?
C8 N3 C12 118.5(2) . . ?
C8 N3 Co1 114.77(17) . . ?
C12 N3 Co1 126.55(17) . . ?
N1 C1 C2 110.38(19) . . ?
N2 C2 C3 122.0(2) . . ?
N2 C2 C1 115.0(2) . . ?
C3 C2 C1 123.0(2) . . ?
C4 C3 C2 119.2(3) . . ?
C3 C4 C5 119.2(3) . . ?
C4 C5 C6 118.8(3) . . ?
N2 C6 C5 122.9(3) . . ?
N1 C7 C8 110.28(19) . . ?
N3 C8 C9 121.5(2) . . ?
N3 C8 C7 116.1(2) . . ?
C9 C8 C7 122.4(2) . . ?
C10 C9 C8 119.7(3) . . ?
C11 C10 C9 118.5(3) . . ?
C10 C11 C12 119.7(3) . . ?
N3 C12 C11 122.0(3) . . ?
N1 C13 C14 117.5(2) . . ?
C15 C14 C19 118.8(2) . . ?
C15 C14 C13 116.4(2) . . ?
C19 C14 C13 124.7(2) . . ?
C14 C15 C16 121.9(2) . . ?
O3 C16 C17 124.5(2) . . ?
O3 C16 C15 115.8(2) . . ?
C17 C16 C15 119.6(2) . . ?
C16 C17 C18 118.9(3) . . ?
C17 C18 C19 122.8(2) . . ?
C18 C19 C14 118.0(2) . . ?
C18 C19 C20 117.9(2) . . ?
C14 C19 C20 124.1(2) . . ?
O1 C20 O2 124.3(2) . . ?
O1 C20 C19 120.0(2) . . ?
O2 C20 C19 115.7(2) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.050
####################################################################### 
# 
# 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_p
_database_code_depnum_ccdc_archive 'CCDC 969853'
_audit_update_record             
;
2015-04-24 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H48 Cl2 N6 Ni2 O8'
_chemical_formula_weight         977.20
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.267 0.108 0.403 61 17 ' '
2 0.267 0.392 0.903 61 17 ' '
3 0.733 0.608 0.097 61 17 ' '
4 0.733 0.892 0.597 61 17 ' '
_platon_squeeze_details          
;
;

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   13.6889(7)
_cell_length_b                   13.9132(7)
_cell_length_c                   15.1302(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 123.009(3)
_cell_angle_gamma                90.00
_cell_volume                     2416.5(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7708
_cell_measurement_theta_min      2.172
_cell_measurement_theta_max      27.019

_exptl_crystal_description       block
_exptl_crystal_colour            light-blue
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1016
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.6689
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21800
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4255
_reflns_number_gt                3883
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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     
'calc w=1/[σ²(Fo²)+(0.0330P)²+1.7202P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4255
_refine_ls_number_parameters     283
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0758
_refine_ls_wR_factor_gt          0.0729
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.34625(2) 0.607348(17) 0.448485(18) 0.02891(9) Uani 1 1 d . . .
O1 O 0.37496(11) 0.46581(10) 0.43007(10) 0.0336(3) Uani 1 1 d . . .
O2 O 0.50178(12) 0.35509(10) 0.53751(12) 0.0402(3) Uani 1 1 d . . .
O4 O 0.32787(13) 0.75563(11) 0.47006(13) 0.0460(4) Uani 1 1 d D . .
H4B H 0.278(2) 0.7884(19) 0.4218(19) 0.055 Uiso 1 1 d D . .
O3 O 0.11421(14) 0.26855(13) 0.63036(15) 0.0588(5) Uani 1 1 d . . .
N1 N 0.17953(13) 0.57535(12) 0.41702(12) 0.0315(3) Uani 1 1 d . . .
N2 N 0.24795(15) 0.62263(13) 0.28556(13) 0.0379(4) Uani 1 1 d . . .
N3 N 0.38849(14) 0.58944(12) 0.60183(13) 0.0321(4) Uani 1 1 d . . .
C1 C 0.09591(17) 0.62971(16) 0.31961(17) 0.0402(5) Uani 1 1 d . . .
H1A H 0.0941 0.6965 0.3370 0.048 Uiso 1 1 calc R . .
H1B H 0.0183 0.6033 0.2883 0.048 Uiso 1 1 calc R . .
C2 C 0.13248(18) 0.62305(16) 0.24249(17) 0.0418(5) Uani 1 1 d . . .
C3 C 0.0537(2) 0.6199(2) 0.1351(2) 0.0641(7) Uani 1 1 d . . .
H3A H -0.0259 0.6197 0.1068 0.077 Uiso 1 1 calc R . .
C4 C 0.0954(3) 0.6171(3) 0.0702(2) 0.0777(9) Uani 1 1 d . . .
H4A H 0.0439 0.6152 -0.0026 0.093 Uiso 1 1 calc R . .
C5 C 0.2130(3) 0.6173(2) 0.1135(2) 0.0671(8) Uani 1 1 d . . .
H5A H 0.2423 0.6158 0.0707 0.081 Uiso 1 1 calc R . .
C6 C 0.2871(2) 0.61964(18) 0.22155(18) 0.0479(6) Uani 1 1 d . . .
H6A H 0.3671 0.6191 0.2510 0.057 Uiso 1 1 calc R . .
C7 C 0.17825(18) 0.60872(16) 0.50893(17) 0.0403(5) Uani 1 1 d . . .
H7A H 0.1181 0.5748 0.5117 0.048 Uiso 1 1 calc R . .
H7B H 0.1602 0.6768 0.5017 0.048 Uiso 1 1 calc R . .
C8 C 0.29530(18) 0.59132(15) 0.61001(17) 0.0382(5) Uani 1 1 d . . .
C9 C 0.3059(2) 0.5793(2) 0.7050(2) 0.0574(7) Uani 1 1 d . . .
H9A H 0.2405 0.5810 0.7090 0.069 Uiso 1 1 calc R . .
C10 C 0.4154(3) 0.5646(2) 0.7946(2) 0.0663(8) Uani 1 1 d . . .
H10A H 0.4245 0.5569 0.8597 0.080 Uiso 1 1 calc R . .
C11 C 0.5109(2) 0.56153(19) 0.78669(18) 0.0519(6) Uani 1 1 d . . .
H11A H 0.5852 0.5512 0.8460 0.062 Uiso 1 1 calc R . .
C12 C 0.49412(18) 0.57396(15) 0.68951(16) 0.0381(5) Uani 1 1 d . . .
H12A H 0.5585 0.5716 0.6840 0.046 Uiso 1 1 calc R . .
C13 C 0.15007(16) 0.47064(14) 0.39373(15) 0.0341(4) Uani 1 1 d . . .
H13A H 0.1671 0.4510 0.3420 0.041 Uiso 1 1 calc R . .
H13B H 0.0668 0.4633 0.3615 0.041 Uiso 1 1 calc R . .
C14 C 0.21183(16) 0.40270(14) 0.48614(15) 0.0312(4) Uani 1 1 d . . .
C15 C 0.14566(17) 0.36513(16) 0.52216(18) 0.0398(5) Uani 1 1 d . . .
H15A H 0.0686 0.3847 0.4900 0.048 Uiso 1 1 calc R . .
C16 C 0.19014(18) 0.29980(16) 0.60395(18) 0.0408(5) Uani 1 1 d . . .
C17 C 0.30491(19) 0.27020(17) 0.65308(18) 0.0447(5) Uani 1 1 d . . .
H17A H 0.3368 0.2276 0.7095 0.054 Uiso 1 1 calc R . .
C18 C 0.37120(18) 0.30531(16) 0.61645(17) 0.0406(5) Uani 1 1 d . . .
H18A H 0.4477 0.2842 0.6485 0.049 Uiso 1 1 calc R . .
C19 C 0.32854(16) 0.37046(14) 0.53418(15) 0.0314(4) Uani 1 1 d . . .
C22 C 0.4242(2) 0.81281(19) 0.5419(2) 0.0645(7) Uani 1 1 d . . .
H20A H 0.3987 0.8774 0.5403 0.097 Uiso 1 1 calc R . .
H20B H 0.4803 0.8129 0.5224 0.097 Uiso 1 1 calc R . .
H20C H 0.4593 0.7870 0.6116 0.097 Uiso 1 1 calc R . .
C21 C 0.1510(2) 0.1907(2) 0.7032(2) 0.0659(8) Uani 1 1 d . . .
H21A H 0.0908 0.1758 0.7153 0.099 Uiso 1 1 calc R . .
H21B H 0.2206 0.2086 0.7685 0.099 Uiso 1 1 calc R . .
H21C H 0.1663 0.1354 0.6746 0.099 Uiso 1 1 calc R . .
C20 C 0.40711(16) 0.40054(13) 0.49811(15) 0.0305(4) Uani 1 1 d . . .
Cl1 Cl 0.13160(5) 0.88763(5) 0.32270(6) 0.06069(18) 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
Ni1 O2 2.0410(13) 3_666 ?
Ni1 O1 2.0565(13) . ?
Ni1 N3 2.0779(16) . ?
Ni1 N2 2.0781(17) . ?
Ni1 N1 2.1094(15) . ?
Ni1 O4 2.1249(16) . ?
O1 C20 1.259(2) . ?
O2 C20 1.262(2) . ?
O2 Ni1 2.0410(13) 3_666 ?
O4 C22 1.411(3) . ?
O3 C16 1.372(2) . ?
O3 C21 1.427(3) . ?
N1 C7 1.475(3) . ?
N1 C1 1.489(2) . ?
N1 C13 1.502(3) . ?
N2 C6 1.339(3) . ?
N2 C2 1.342(3) . ?
N3 C12 1.344(3) . ?
N3 C8 1.347(3) . ?
C1 C2 1.502(3) . ?
C2 C3 1.377(3) . ?
C3 C4 1.378(4) . ?
C4 C5 1.367(4) . ?
C5 C6 1.377(3) . ?
C7 C8 1.515(3) . ?
C8 C9 1.374(3) . ?
C9 C10 1.383(4) . ?
C10 C11 1.376(4) . ?
C11 C12 1.370(3) . ?
C13 C14 1.508(3) . ?
C14 C15 1.389(3) . ?
C14 C19 1.420(3) . ?
C15 C16 1.381(3) . ?
C16 C17 1.385(3) . ?
C17 C18 1.385(3) . ?
C18 C19 1.386(3) . ?
C19 C20 1.506(3) . ?

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
O2 Ni1 O1 90.00(5) 3_666 . ?
O2 Ni1 N3 105.48(6) 3_666 . ?
O1 Ni1 N3 94.53(6) . . ?
O2 Ni1 N2 93.54(6) 3_666 . ?
O1 Ni1 N2 89.15(6) . . ?
N3 Ni1 N2 160.61(7) . . ?
O2 Ni1 N1 173.59(6) 3_666 . ?
O1 Ni1 N1 91.75(6) . . ?
N3 Ni1 N1 80.53(6) . . ?
N2 Ni1 N1 80.33(6) . . ?
O2 Ni1 O4 86.26(6) 3_666 . ?
O1 Ni1 O4 176.21(6) . . ?
N3 Ni1 O4 85.93(7) . . ?
N2 Ni1 O4 91.64(7) . . ?
N1 Ni1 O4 92.03(6) . . ?
C20 O1 Ni1 125.97(12) . . ?
C20 O2 Ni1 130.32(13) . 3_666 ?
C22 O4 Ni1 121.76(14) . . ?
C16 O3 C21 117.43(18) . . ?
C7 N1 C1 112.08(16) . . ?
C7 N1 C13 112.77(16) . . ?
C1 N1 C13 107.29(15) . . ?
C7 N1 Ni1 106.73(12) . . ?
C1 N1 Ni1 105.67(12) . . ?
C13 N1 Ni1 112.14(11) . . ?
C6 N2 C2 118.61(19) . . ?
C6 N2 Ni1 126.80(15) . . ?
C2 N2 Ni1 114.00(14) . . ?
C12 N3 C8 118.41(18) . . ?
C12 N3 Ni1 128.06(14) . . ?
C8 N3 Ni1 113.50(13) . . ?
N1 C1 C2 109.62(16) . . ?
N2 C2 C3 122.0(2) . . ?
N2 C2 C1 115.20(19) . . ?
C3 C2 C1 122.7(2) . . ?
C2 C3 C4 118.7(3) . . ?
C5 C4 C3 119.6(3) . . ?
C4 C5 C6 118.9(3) . . ?
N2 C6 C5 122.2(2) . . ?
N1 C7 C8 110.62(16) . . ?
N3 C8 C9 121.9(2) . . ?
N3 C8 C7 116.36(18) . . ?
C9 C8 C7 121.7(2) . . ?
C8 C9 C10 118.9(2) . . ?
C11 C10 C9 119.6(2) . . ?
C12 C11 C10 118.5(2) . . ?
N3 C12 C11 122.7(2) . . ?
N1 C13 C14 116.57(16) . . ?
C15 C14 C19 118.21(18) . . ?
C15 C14 C13 116.34(17) . . ?
C19 C14 C13 125.34(17) . . ?
C16 C15 C14 122.41(19) . . ?
O3 C16 C15 115.81(18) . . ?
O3 C16 C17 124.6(2) . . ?
C15 C16 C17 119.62(19) . . ?
C18 C17 C16 118.6(2) . . ?
C17 C18 C19 122.88(19) . . ?
C18 C19 C14 118.20(18) . . ?
C18 C19 C20 118.19(17) . . ?
C14 C19 C20 123.58(17) . . ?
O1 C20 O2 124.00(18) . . ?
O1 C20 C19 119.75(16) . . ?
O2 C20 C19 116.22(17) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.044
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 969854'
_audit_update_record             
;
2015-04-24 deposited with the CCDC.
2015-06-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23.50 H28 Cu N3 O7'
_chemical_formula_weight         528.03

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'
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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9928(2)
_cell_length_b                   12.0354(2)
_cell_length_c                   18.6928(3)
_cell_angle_alpha                83.4210(10)
_cell_angle_beta                 78.4230(10)
_cell_angle_gamma                80.3700(10)
_cell_volume                     2380.24(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5138
_cell_measurement_theta_min      2.232
_cell_measurement_theta_max      26.852

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1100
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.6396
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16089
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8346
_reflns_number_gt                6656
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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     
'calc w=1/[σ²(Fo²)+(0.0520P)²+0.6184P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8346
_refine_ls_number_parameters     664
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0966
_refine_ls_wR_factor_gt          0.0912
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.007
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.33814(2) 0.49810(2) 0.808514(14) 0.03113(9) Uani 1 1 d . . .
O1 O 0.23228(15) 0.52578(15) 0.72235(9) 0.0432(4) Uani 1 1 d . . .
O2 O 0.15290(18) 0.65275(18) 0.64294(10) 0.0613(5) Uani 1 1 d . . .
O3 O 0.70457(19) 0.63579(17) 0.47093(10) 0.0578(5) Uani 1 1 d . . .
O4 O 0.20022(15) 0.56863(14) 0.87930(9) 0.0424(4) Uani 1 1 d . . .
O5 O 0.3156(13) 0.535(2) 0.9678(14) 0.060(3) Uani 0.50 1 d PD . .
O5' O 0.3297(13) 0.558(2) 0.9553(13) 0.063(4) Uani 0.50 1 d PD . .
N1 N 0.49732(17) 0.41814(15) 0.74701(10) 0.0308(4) Uani 1 1 d . . .
N2 N 0.42981(18) 0.63032(15) 0.78583(10) 0.0337(4) Uani 1 1 d . . .
N3 N 0.30474(19) 0.34034(16) 0.84019(11) 0.0389(5) Uani 1 1 d . . .
C1 C 0.6003(2) 0.48466(19) 0.74620(13) 0.0353(5) Uani 1 1 d . . .
H1A H 0.6610 0.4759 0.7010 0.042 Uiso 1 1 calc R . .
H1B H 0.6430 0.4560 0.7867 0.042 Uiso 1 1 calc R . .
C2 C 0.5497(2) 0.6079(2) 0.75243(12) 0.0351(5) Uani 1 1 d . . .
C3 C 0.6235(3) 0.6927(2) 0.73003(14) 0.0490(7) Uani 1 1 d . . .
H3A H 0.7067 0.6758 0.7067 0.059 Uiso 1 1 calc R . .
C4 C 0.5716(3) 0.8024(2) 0.74291(16) 0.0601(8) Uani 1 1 d . . .
H4A H 0.6198 0.8605 0.7291 0.072 Uiso 1 1 calc R . .
C5 C 0.4475(3) 0.8254(2) 0.77640(17) 0.0594(8) Uani 1 1 d . . .
H5A H 0.4107 0.8993 0.7846 0.071 Uiso 1 1 calc R . .
C6 C 0.3792(3) 0.7384(2) 0.79741(14) 0.0461(6) Uani 1 1 d . . .
H6A H 0.2956 0.7540 0.8203 0.055 Uiso 1 1 calc R . .
C7 C 0.5225(2) 0.30287(19) 0.78477(13) 0.0394(6) Uani 1 1 d . . .
H7A H 0.5717 0.3054 0.8221 0.047 Uiso 1 1 calc R . .
H7B H 0.5708 0.2514 0.7496 0.047 Uiso 1 1 calc R . .
C8 C 0.4023(2) 0.26028(19) 0.81946(13) 0.0379(5) Uani 1 1 d . . .
C9 C 0.3928(3) 0.1468(2) 0.83373(15) 0.0514(7) Uani 1 1 d . . .
H9A H 0.4607 0.0923 0.8183 0.062 Uiso 1 1 calc R . .
C10 C 0.2807(3) 0.1159(2) 0.87137(17) 0.0638(8) Uani 1 1 d . . .
H10B H 0.2723 0.0398 0.8818 0.077 Uiso 1 1 calc R . .
C11 C 0.1819(3) 0.1975(3) 0.89332(17) 0.0626(8) Uani 1 1 d . . .
H11B H 0.1062 0.1777 0.9195 0.075 Uiso 1 1 calc R . .
C12 C 0.1959(3) 0.3096(2) 0.87618(15) 0.0494(7) Uani 1 1 d . . .
H12B H 0.1282 0.3653 0.8900 0.059 Uiso 1 1 calc R . .
C13 C 0.4768(2) 0.40660(19) 0.67092(12) 0.0351(5) Uani 1 1 d . . .
H13C H 0.3971 0.3797 0.6750 0.042 Uiso 1 1 calc R . .
H13D H 0.5421 0.3495 0.6487 0.042 Uiso 1 1 calc R . .
C14 C 0.4766(2) 0.51423(19) 0.62047(12) 0.0332(5) Uani 1 1 d . . .
C15 C 0.5883(2) 0.5263(2) 0.57108(12) 0.0381(5) Uani 1 1 d . . .
H15B H 0.6577 0.4706 0.5725 0.046 Uiso 1 1 calc R . .
C16 C 0.5986(3) 0.6189(2) 0.51999(13) 0.0439(6) Uani 1 1 d . . .
C17 C 0.4942(3) 0.7009(2) 0.51704(15) 0.0496(7) Uani 1 1 d . . .
H17B H 0.4991 0.7636 0.4832 0.060 Uiso 1 1 calc R . .
C18 C 0.3838(3) 0.6885(2) 0.56447(14) 0.0440(6) Uani 1 1 d . . .
H18B H 0.3143 0.7434 0.5613 0.053 Uiso 1 1 calc R . .
C19 C 0.3712(2) 0.59698(19) 0.61743(12) 0.0356(5) Uani 1 1 d . . .
C20 C 0.2428(2) 0.5914(2) 0.66484(13) 0.0370(6) Uani 1 1 d . . .
C21 C 0.8169(3) 0.5607(3) 0.47768(16) 0.0633(8) Uani 1 1 d . . .
H21D H 0.8864 0.5879 0.4445 0.095 Uiso 1 1 calc R . .
H21E H 0.8093 0.4868 0.4660 0.095 Uiso 1 1 calc R . .
H21F H 0.8310 0.5566 0.5270 0.095 Uiso 1 1 calc R . .
C22 C 0.2211(3) 0.5798(2) 0.94197(14) 0.0431(6) Uani 1 1 d D . .
C23 C 0.1125(3) 0.6377(3) 0.99402(16) 0.0692(9) Uani 1 1 d . . .
H23D H 0.0473 0.6610 0.9673 0.083 Uiso 1 1 d R . .
H23E H 0.1431 0.7002 1.0074 0.083 Uiso 1 1 d R . .
H23F H 0.0896 0.5870 1.0352 0.083 Uiso 1 1 d R . .
Cu1A Cu -0.15944(2) 0.01549(2) 0.807793(14) 0.03115(9) Uani 1 1 d . . .
O1A O -0.28678(15) 0.02412(14) 0.73330(9) 0.0398(4) Uani 1 1 d . . .
O2A O -0.39226(17) 0.11151(18) 0.64896(11) 0.0595(5) Uani 1 1 d . . .
O3A O 0.12986(17) 0.19079(16) 0.46545(9) 0.0513(5) Uani 1 1 d . . .
O4A O -0.29365(16) 0.08731(15) 0.88006(9) 0.0436(4) Uani 1 1 d . . .
O5A O -0.1631(15) 0.0849(11) 0.9577(15) 0.068(3) Uani 0.50 1 d PD . .
O5B O -0.1703(14) 0.0493(11) 0.9608(13) 0.063(3) Uani 0.50 1 d PD . .
N1A N -0.00583(17) -0.06243(15) 0.74130(9) 0.0293(4) Uani 1 1 d . . .
N2A N -0.07255(18) 0.15155(16) 0.77691(10) 0.0350(4) Uani 1 1 d . . .
N3A N -0.18294(19) -0.14363(16) 0.84613(10) 0.0380(5) Uani 1 1 d . . .
C1A C 0.0968(2) 0.0059(2) 0.73550(13) 0.0362(5) Uani 1 1 d . . .
H1 H 0.1551 -0.0052 0.6896 0.043 Uiso 1 1 calc R . .
H2 H 0.1423 -0.0189 0.7753 0.043 Uiso 1 1 calc R . .
C2A C 0.0440(2) 0.13011(19) 0.73882(12) 0.0346(5) Uani 1 1 d . . .
C3A C 0.1136(3) 0.2156(2) 0.70851(14) 0.0478(6) Uani 1 1 d . . .
H6 H 0.1944 0.1990 0.6817 0.057 Uiso 1 1 calc R . .
C4A C 0.0598(3) 0.3259(2) 0.71919(17) 0.0596(8) Uani 1 1 d . . .
H8 H 0.1046 0.3850 0.7000 0.071 Uiso 1 1 calc R . .
C5A C -0.0601(3) 0.3479(2) 0.75819(18) 0.0593(8) Uani 1 1 d . . .
H9 H -0.0976 0.4220 0.7653 0.071 Uiso 1 1 calc R . .
C6A C -0.1237(3) 0.2597(2) 0.78646(15) 0.0479(7) Uani 1 1 d . . .
H5 H -0.2048 0.2749 0.8131 0.058 Uiso 1 1 calc R . .
C7A C 0.0273(2) -0.17841(19) 0.77756(13) 0.0368(5) Uani 1 1 d . . .
H3 H 0.0694 -0.2294 0.7406 0.044 Uiso 1 1 calc R . .
H4 H 0.0846 -0.1755 0.8104 0.044 Uiso 1 1 calc R . .
C8A C -0.0879(2) -0.22219(19) 0.81986(12) 0.0371(5) Uani 1 1 d . . .
C9A C -0.0933(3) -0.3371(2) 0.83570(15) 0.0525(7) Uani 1 1 d . . .
H7 H -0.0272 -0.3908 0.8166 0.063 Uiso 1 1 calc R . .
C10A C -0.1992(3) -0.3691(3) 0.88043(18) 0.0670(9) Uani 1 1 d . . .
H10A H -0.2055 -0.4455 0.8918 0.080 Uiso 1 1 calc R . .
C11A C -0.2956(3) -0.2889(3) 0.90826(18) 0.0679(9) Uani 1 1 d . . .
H11A H -0.3667 -0.3101 0.9394 0.082 Uiso 1 1 calc R . .
C12A C -0.2856(3) -0.1767(2) 0.88943(15) 0.0532(7) Uani 1 1 d . . .
H12A H -0.3518 -0.1221 0.9072 0.064 Uiso 1 1 calc R . .
C13A C -0.0343(2) -0.07550(18) 0.66754(12) 0.0322(5) Uani 1 1 d . . .
H13A H -0.1084 -0.1122 0.6749 0.039 Uiso 1 1 calc R . .
H13B H 0.0351 -0.1251 0.6414 0.039 Uiso 1 1 calc R . .
C14A C -0.0560(2) 0.03358(18) 0.61982(12) 0.0305(5) Uani 1 1 d . . .
C15A C 0.0467(2) 0.06277(19) 0.56738(12) 0.0343(5) Uani 1 1 d . . .
H15A H 0.1245 0.0175 0.5654 0.041 Uiso 1 1 calc R . .
C16A C 0.0343(2) 0.1575(2) 0.51858(13) 0.0391(6) Uani 1 1 d . . .
C17A C -0.0812(3) 0.2244(2) 0.52013(14) 0.0475(7) Uani 1 1 d . . .
H17A H -0.0901 0.2886 0.4877 0.057 Uiso 1 1 calc R . .
C18A C -0.1826(2) 0.1949(2) 0.57025(13) 0.0441(6) Uani 1 1 d . . .
H18A H -0.2606 0.2391 0.5701 0.053 Uiso 1 1 calc R . .
C19A C -0.1733(2) 0.10161(19) 0.62124(12) 0.0327(5) Uani 1 1 d . . .
C20A C -0.2928(2) 0.07676(19) 0.67178(13) 0.0343(5) Uani 1 1 d . . .
C21A C 0.2534(3) 0.1328(2) 0.46637(15) 0.0541(7) Uani 1 1 d . . .
H21A H 0.3117 0.1673 0.4286 0.081 Uiso 1 1 calc R . .
H21B H 0.2570 0.0550 0.4580 0.081 Uiso 1 1 calc R . .
H21C H 0.2749 0.1370 0.5132 0.081 Uiso 1 1 calc R . .
C22A C -0.2702(3) 0.0966(2) 0.94255(14) 0.0467(6) Uani 1 1 d D . .
C23A C -0.3789(3) 0.1473(3) 0.99724(16) 0.0775(10) Uani 1 1 d . . .
H23A H -0.4044 0.0899 1.0347 0.116 Uiso 1 1 calc R . .
H23B H -0.4478 0.1781 0.9729 0.116 Uiso 1 1 calc R . .
H23C H -0.3542 0.2064 1.0190 0.116 Uiso 1 1 calc R . .
O12 O 0.0858(3) 0.3868(3) 0.35138(16) 0.0870(8) Uani 1 1 d D . .
H12D H 0.099(4) 0.340(3) 0.378(2) 0.104 Uiso 1 1 d D . .
H12C H 0.014(3) 0.387(4) 0.345(2) 0.104 Uiso 1 1 d D . .
O13 O 0.5723(3) 0.4317(3) 0.91872(14) 0.0872(9) Uani 1 1 d D . .
H13F H 0.613(4) 0.431(3) 0.954(2) 0.105 Uiso 1 1 d D . .
H13E H 0.507(3) 0.426(4) 0.939(2) 0.105 Uiso 1 1 d D . .
O18 O 0.3834(2) 1.0525(3) 0.6480(2) 0.1107(11) Uani 1 1 d D . .
H18C H 0.457(4) 1.085(4) 0.655(2) 0.133 Uiso 1 1 d D . .
C26 C 0.4149(4) 0.9665(4) 0.6053(2) 0.0983(13) Uani 1 1 d . . .
H26A H 0.3405 0.9379 0.6009 0.147 Uiso 1 1 calc R . .
H26B H 0.4700 0.9075 0.6268 0.147 Uiso 1 1 calc R . .
H26C H 0.4567 0.9924 0.5577 0.147 Uiso 1 1 calc R . .
O16 O 0.9310(3) 0.0705(2) 0.08404(13) 0.0764(7) Uani 1 1 d D . .
H16A H 0.896(3) 0.074(3) 0.0481(19) 0.092 Uiso 1 1 d D . .
H16B H 0.999(3) 0.051(3) 0.066(2) 0.092 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O4 1.9473(16) . ?
Cu1 N2 1.9845(18) . ?
Cu1 N3 1.9947(19) . ?
Cu1 N1 2.0475(18) . ?
Cu1 O1 2.1351(17) . ?
O1 C20 1.256(3) . ?
O2 C20 1.240(3) . ?
O3 C16 1.359(3) . ?
O3 C21 1.422(3) . ?
O4 C22 1.264(3) . ?
O5 C22 1.248(11) . ?
O5' C22 1.247(11) . ?
N1 C1 1.489(3) . ?
N1 C7 1.492(3) . ?
N1 C13 1.509(3) . ?
N2 C2 1.337(3) . ?
N2 C6 1.349(3) . ?
N3 C12 1.337(3) . ?
N3 C8 1.342(3) . ?
C1 C2 1.504(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.385(3) . ?
C3 C4 1.375(4) . ?
C3 H3A 0.9300 . ?
C4 C5 1.378(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.366(4) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C8 1.496(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.378(3) . ?
C9 C10 1.377(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.368(4) . ?
C10 H10B 0.9300 . ?
C11 C12 1.378(4) . ?
C11 H11B 0.9300 . ?
C12 H12B 0.9300 . ?
C13 C14 1.512(3) . ?
C13 H13C 0.9700 . ?
C13 H13D 0.9700 . ?
C14 C15 1.398(3) . ?
C14 C19 1.402(3) . ?
C15 C16 1.387(3) . ?
C15 H15B 0.9300 . ?
C16 C17 1.388(4) . ?
C17 C18 1.371(4) . ?
C17 H17B 0.9300 . ?
C18 C19 1.400(3) . ?
C18 H18B 0.9300 . ?
C19 C20 1.516(3) . ?
C21 H21D 0.9600 . ?
C21 H21E 0.9600 . ?
C21 H21F 0.9600 . ?
C22 C23 1.505(4) . ?
C23 H23D 0.9411 . ?
C23 H23E 0.9503 . ?
C23 H23F 0.9456 . ?
Cu1A O4A 1.9467(16) . ?
Cu1A N2A 2.0031(19) . ?
Cu1A N3A 2.0060(19) . ?
Cu1A N1A 2.0421(18) . ?
Cu1A O1A 2.1471(16) . ?
O1A C20A 1.256(3) . ?
O2A C20A 1.243(3) . ?
O3A C16A 1.371(3) . ?
O3A C21A 1.421(3) . ?
O4A C22A 1.267(3) . ?
O5A C22A 1.247(11) . ?
O5B C22A 1.241(11) . ?
N1A C1A 1.484(3) . ?
N1A C7A 1.501(3) . ?
N1A C13A 1.504(3) . ?
N2A C2A 1.334(3) . ?
N2A C6A 1.345(3) . ?
N3A C12A 1.340(3) . ?
N3A C8A 1.341(3) . ?
C1A C2A 1.514(3) . ?
C1A H1 0.9700 . ?
C1A H2 0.9700 . ?
C2A C3A 1.386(3) . ?
C3A C4A 1.379(4) . ?
C3A H6 0.9300 . ?
C4A C5A 1.371(4) . ?
C4A H8 0.9300 . ?
C5A C6A 1.366(4) . ?
C5A H9 0.9300 . ?
C6A H5 0.9300 . ?
C7A C8A 1.494(3) . ?
C7A H3 0.9700 . ?
C7A H4 0.9700 . ?
C8A C9A 1.389(3) . ?
C9A C10A 1.375(4) . ?
C9A H7 0.9300 . ?
C10A C11A 1.370(4) . ?
C10A H10A 0.9300 . ?
C11A C12A 1.373(4) . ?
C11A H11A 0.9300 . ?
C12A H12A 0.9300 . ?
C13A C14A 1.513(3) . ?
C13A H13A 0.9700 . ?
C13A H13B 0.9700 . ?
C14A C15A 1.403(3) . ?
C14A C19A 1.405(3) . ?
C15A C16A 1.382(3) . ?
C15A H15A 0.9300 . ?
C16A C17A 1.382(3) . ?
C17A C18A 1.373(3) . ?
C17A H17A 0.9300 . ?
C18A C19A 1.391(3) . ?
C18A H18A 0.9300 . ?
C19A C20A 1.508(3) . ?
C21A H21A 0.9600 . ?
C21A H21B 0.9600 . ?
C21A H21C 0.9600 . ?
C22A C23A 1.502(4) . ?
C23A H23A 0.9600 . ?
C23A H23B 0.9600 . ?
C23A H23C 0.9600 . ?
O12 H12D 0.73(3) . ?
O12 H12C 0.83(3) . ?
O13 H13F 0.86(3) . ?
O13 H13E 0.75(3) . ?
O18 C26 1.336(4) . ?
O18 H18C 1.00(3) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
O16 H16A 0.83(3) . ?
O16 H16B 0.77(3) . ?

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
O4 Cu1 N2 95.97(7) . . ?
O4 Cu1 N3 95.17(8) . . ?
N2 Cu1 N3 159.56(8) . . ?
O4 Cu1 N1 171.36(7) . . ?
N2 Cu1 N1 83.24(7) . . ?
N3 Cu1 N1 83.18(8) . . ?
O4 Cu1 O1 93.57(7) . . ?
N2 Cu1 O1 100.19(7) . . ?
N3 Cu1 O1 96.15(8) . . ?
N1 Cu1 O1 95.04(7) . . ?
C20 O1 Cu1 130.44(15) . . ?
C16 O3 C21 117.9(2) . . ?
C22 O4 Cu1 117.96(17) . . ?
C1 N1 C7 111.30(18) . . ?
C1 N1 C13 112.35(17) . . ?
C7 N1 C13 108.76(17) . . ?
C1 N1 Cu1 107.36(13) . . ?
C7 N1 Cu1 106.09(13) . . ?
C13 N1 Cu1 110.80(14) . . ?
C2 N2 C6 119.2(2) . . ?
C2 N2 Cu1 115.18(15) . . ?
C6 N2 Cu1 125.50(17) . . ?
C12 N3 C8 119.4(2) . . ?
C12 N3 Cu1 126.29(18) . . ?
C8 N3 Cu1 114.26(16) . . ?
N1 C1 C2 110.88(18) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C3 121.6(2) . . ?
N2 C2 C1 115.44(19) . . ?
C3 C2 C1 122.8(2) . . ?
C4 C3 C2 118.8(3) . . ?
C4 C3 H3A 120.6 . . ?
C2 C3 H3A 120.6 . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C6 C5 C4 119.2(3) . . ?
C6 C5 H5A 120.4 . . ?
C4 C5 H5A 120.4 . . ?
N2 C6 C5 121.7(3) . . ?
N2 C6 H6A 119.1 . . ?
C5 C6 H6A 119.1 . . ?
N1 C7 C8 110.75(19) . . ?
N1 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
N3 C8 C9 121.6(2) . . ?
N3 C8 C7 115.4(2) . . ?
C9 C8 C7 122.9(2) . . ?
C10 C9 C8 118.7(3) . . ?
C10 C9 H9A 120.7 . . ?
C8 C9 H9A 120.7 . . ?
C11 C10 C9 119.7(3) . . ?
C11 C10 H10B 120.2 . . ?
C9 C10 H10B 120.2 . . ?
C10 C11 C12 119.1(3) . . ?
C10 C11 H11B 120.4 . . ?
C12 C11 H11B 120.4 . . ?
N3 C12 C11 121.5(3) . . ?
N3 C12 H12B 119.2 . . ?
C11 C12 H12B 119.2 . . ?
N1 C13 C14 114.88(18) . . ?
N1 C13 H13C 108.5 . . ?
C14 C13 H13C 108.5 . . ?
N1 C13 H13D 108.5 . . ?
C14 C13 H13D 108.5 . . ?
H13C C13 H13D 107.5 . . ?
C15 C14 C19 119.2(2) . . ?
C15 C14 C13 116.3(2) . . ?
C19 C14 C13 124.4(2) . . ?
C16 C15 C14 121.9(2) . . ?
C16 C15 H15B 119.1 . . ?
C14 C15 H15B 119.1 . . ?
O3 C16 C15 124.7(3) . . ?
O3 C16 C17 116.4(2) . . ?
C15 C16 C17 118.9(2) . . ?
C18 C17 C16 119.4(2) . . ?
C18 C17 H17B 120.3 . . ?
C16 C17 H17B 120.3 . . ?
C17 C18 C19 123.0(2) . . ?
C17 C18 H18B 118.5 . . ?
C19 C18 H18B 118.5 . . ?
C18 C19 C14 117.6(2) . . ?
C18 C19 C20 117.7(2) . . ?
C14 C19 C20 124.6(2) . . ?
O2 C20 O1 123.9(2) . . ?
O2 C20 C19 116.4(2) . . ?
O1 C20 C19 119.7(2) . . ?
O3 C21 H21D 109.5 . . ?
O3 C21 H21E 109.5 . . ?
H21D C21 H21E 109.5 . . ?
O3 C21 H21F 109.5 . . ?
H21D C21 H21F 109.5 . . ?
H21E C21 H21F 109.5 . . ?
O5' C22 O5 17.2(17) . . ?
O5' C22 O4 120.8(13) . . ?
O5 C22 O4 126.4(15) . . ?
O5' C22 C23 122.6(14) . . ?
O5 C22 C23 116.9(14) . . ?
O4 C22 C23 115.9(3) . . ?
C22 C23 H23D 106.3 . . ?
C22 C23 H23E 104.7 . . ?
H23D C23 H23E 111.9 . . ?
C22 C23 H23F 109.6 . . ?
H23D C23 H23F 112.4 . . ?
H23E C23 H23F 111.4 . . ?
O4A Cu1A N2A 96.08(8) . . ?
O4A Cu1A N3A 95.56(8) . . ?
N2A Cu1A N3A 158.73(8) . . ?
O4A Cu1A N1A 173.22(7) . . ?
N2A Cu1A N1A 82.95(7) . . ?
N3A Cu1A N1A 83.39(7) . . ?
O4A Cu1A O1A 90.59(7) . . ?
N2A Cu1A O1A 104.86(7) . . ?
N3A Cu1A O1A 92.74(7) . . ?
N1A Cu1A O1A 96.14(7) . . ?
C20A O1A Cu1A 132.93(14) . . ?
C16A O3A C21A 117.9(2) . . ?
C22A O4A Cu1A 118.07(17) . . ?
C1A N1A C7A 110.98(17) . . ?
C1A N1A C13A 112.05(17) . . ?
C7A N1A C13A 108.08(16) . . ?
C1A N1A Cu1A 107.27(13) . . ?
C7A N1A Cu1A 106.98(13) . . ?
C13A N1A Cu1A 111.37(13) . . ?
C2A N2A C6A 118.8(2) . . ?
C2A N2A Cu1A 114.79(15) . . ?
C6A N2A Cu1A 126.22(17) . . ?
C12A N3A C8A 119.2(2) . . ?
C12A N3A Cu1A 126.44(18) . . ?
C8A N3A Cu1A 114.16(15) . . ?
N1A C1A C2A 110.44(18) . . ?
N1A C1A H1 109.6 . . ?
C2A C1A H1 109.6 . . ?
N1A C1A H2 109.6 . . ?
C2A C1A H2 109.6 . . ?
H1 C1A H2 108.1 . . ?
N2A C2A C3A 122.1(2) . . ?
N2A C2A C1A 114.98(19) . . ?
C3A C2A C1A 122.8(2) . . ?
C4A C3A C2A 118.2(3) . . ?
C4A C3A H6 120.9 . . ?
C2A C3A H6 120.9 . . ?
C5A C4A C3A 119.7(3) . . ?
C5A C4A H8 120.2 . . ?
C3A C4A H8 120.2 . . ?
C6A C5A C4A 119.2(3) . . ?
C6A C5A H9 120.4 . . ?
C4A C5A H9 120.4 . . ?
N2A C6A C5A 122.0(3) . . ?
N2A C6A H5 119.0 . . ?
C5A C6A H5 119.0 . . ?
C8A C7A N1A 110.68(18) . . ?
C8A C7A H3 109.5 . . ?
N1A C7A H3 109.5 . . ?
C8A C7A H4 109.5 . . ?
N1A C7A H4 109.5 . . ?
H3 C7A H4 108.1 . . ?
N3A C8A C9A 121.8(2) . . ?
N3A C8A C7A 115.8(2) . . ?
C9A C8A C7A 122.3(2) . . ?
C10A C9A C8A 118.1(3) . . ?
C10A C9A H7 121.0 . . ?
C8A C9A H7 121.0 . . ?
C11A C10A C9A 120.2(3) . . ?
C11A C10A H10A 119.9 . . ?
C9A C10A H10A 119.9 . . ?
C10A C11A C12A 119.0(3) . . ?
C10A C11A H11A 120.5 . . ?
C12A C11A H11A 120.5 . . ?
N3A C12A C11A 121.8(3) . . ?
N3A C12A H12A 119.1 . . ?
C11A C12A H12A 119.1 . . ?
N1A C13A C14A 115.13(17) . . ?
N1A C13A H13A 108.5 . . ?
C14A C13A H13A 108.5 . . ?
N1A C13A H13B 108.5 . . ?
C14A C13A H13B 108.5 . . ?
H13A C13A H13B 107.5 . . ?
C15A C14A C19A 118.7(2) . . ?
C15A C14A C13A 117.0(2) . . ?
C19A C14A C13A 124.2(2) . . ?
C16A C15A C14A 121.2(2) . . ?
C16A C15A H15A 119.4 . . ?
C14A C15A H15A 119.4 . . ?
O3A C16A C15A 124.5(2) . . ?
O3A C16A C17A 115.5(2) . . ?
C15A C16A C17A 120.0(2) . . ?
C18A C17A C16A 119.1(2) . . ?
C18A C17A H17A 120.4 . . ?
C16A C17A H17A 120.4 . . ?
C17A C18A C19A 122.6(2) . . ?
C17A C18A H18A 118.7 . . ?
C19A C18A H18A 118.7 . . ?
C18A C19A C14A 118.4(2) . . ?
C18A C19A C20A 117.2(2) . . ?
C14A C19A C20A 124.3(2) . . ?
O2A C20A O1A 124.3(2) . . ?
O2A C20A C19A 116.5(2) . . ?
O1A C20A C19A 119.3(2) . . ?
O3A C21A H21A 109.5 . . ?
O3A C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
O3A C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
O5B C22A O5A 20.5(12) . . ?
O5B C22A O4A 121.3(11) . . ?
O5A C22A O4A 125.2(13) . . ?
O5B C22A C23A 121.9(12) . . ?
O5A C22A C23A 118.0(12) . . ?
O4A C22A C23A 115.7(3) . . ?
C22A C23A H23A 109.5 . . ?
C22A C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
C22A C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
H12D O12 H12C 107(4) . . ?
H13F O13 H13E 103(4) . . ?
C26 O18 H18C 113(3) . . ?
O18 C26 H26A 109.5 . . ?
O18 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O18 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
H16A O16 H16B 100(4) . . ?

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
O4 Cu1 O1 C20 110.1(2) . . . . ?
N2 Cu1 O1 C20 13.4(2) . . . . ?
N3 Cu1 O1 C20 -154.3(2) . . . . ?
N1 Cu1 O1 C20 -70.6(2) . . . . ?
N2 Cu1 O4 C22 -74.74(18) . . . . ?
N3 Cu1 O4 C22 88.09(19) . . . . ?
N1 Cu1 O4 C22 9.5(6) . . . . ?
O1 Cu1 O4 C22 -175.39(18) . . . . ?
O4 Cu1 N1 C1 -64.1(5) . . . . ?
N2 Cu1 N1 C1 21.08(14) . . . . ?
N3 Cu1 N1 C1 -143.61(15) . . . . ?
O1 Cu1 N1 C1 120.78(14) . . . . ?
O4 Cu1 N1 C7 55.0(5) . . . . ?
N2 Cu1 N1 C7 140.19(15) . . . . ?
N3 Cu1 N1 C7 -24.50(15) . . . . ?
O1 Cu1 N1 C7 -120.11(14) . . . . ?
O4 Cu1 N1 C13 172.8(4) . . . . ?
N2 Cu1 N1 C13 -101.94(14) . . . . ?
N3 Cu1 N1 C13 93.38(14) . . . . ?
O1 Cu1 N1 C13 -2.24(14) . . . . ?
O4 Cu1 N2 C2 163.23(16) . . . . ?
N3 Cu1 N2 C2 40.5(3) . . . . ?
N1 Cu1 N2 C2 -8.12(16) . . . . ?
O1 Cu1 N2 C2 -102.05(16) . . . . ?
O4 Cu1 N2 C6 -20.9(2) . . . . ?
N3 Cu1 N2 C6 -143.6(2) . . . . ?
N1 Cu1 N2 C6 167.8(2) . . . . ?
O1 Cu1 N2 C6 73.9(2) . . . . ?
O4 Cu1 N3 C12 21.8(2) . . . . ?
N2 Cu1 N3 C12 144.7(2) . . . . ?
N1 Cu1 N3 C12 -166.7(2) . . . . ?
O1 Cu1 N3 C12 -72.3(2) . . . . ?
O4 Cu1 N3 C8 -161.02(17) . . . . ?
N2 Cu1 N3 C8 -38.2(3) . . . . ?
N1 Cu1 N3 C8 10.45(17) . . . . ?
O1 Cu1 N3 C8 104.81(17) . . . . ?
C7 N1 C1 C2 -145.68(19) . . . . ?
C13 N1 C1 C2 92.1(2) . . . . ?
Cu1 N1 C1 C2 -30.0(2) . . . . ?
C6 N2 C2 C3 0.6(3) . . . . ?
Cu1 N2 C2 C3 176.80(18) . . . . ?
C6 N2 C2 C1 176.3(2) . . . . ?
Cu1 N2 C2 C1 -7.6(3) . . . . ?
N1 C1 C2 N2 25.8(3) . . . . ?
N1 C1 C2 C3 -158.6(2) . . . . ?
N2 C2 C3 C4 0.2(4) . . . . ?
C1 C2 C3 C4 -175.1(2) . . . . ?
C2 C3 C4 C5 -1.1(4) . . . . ?
C3 C4 C5 C6 1.2(5) . . . . ?
C2 N2 C6 C5 -0.5(4) . . . . ?
Cu1 N2 C6 C5 -176.3(2) . . . . ?
C4 C5 C6 N2 -0.4(4) . . . . ?
C1 N1 C7 C8 150.73(19) . . . . ?
C13 N1 C7 C8 -85.0(2) . . . . ?
Cu1 N1 C7 C8 34.3(2) . . . . ?
C12 N3 C8 C9 0.6(4) . . . . ?
Cu1 N3 C8 C9 -176.7(2) . . . . ?
C12 N3 C8 C7 -175.5(2) . . . . ?
Cu1 N3 C8 C7 7.2(3) . . . . ?
N1 C7 C8 N3 -28.7(3) . . . . ?
N1 C7 C8 C9 155.3(2) . . . . ?
N3 C8 C9 C10 -1.2(4) . . . . ?
C7 C8 C9 C10 174.6(3) . . . . ?
C8 C9 C10 C11 0.3(5) . . . . ?
C9 C10 C11 C12 1.0(5) . . . . ?
C8 N3 C12 C11 0.8(4) . . . . ?
Cu1 N3 C12 C11 177.8(2) . . . . ?
C10 C11 C12 N3 -1.6(5) . . . . ?
C1 N1 C13 C14 -44.3(3) . . . . ?
C7 N1 C13 C14 -168.01(19) . . . . ?
Cu1 N1 C13 C14 75.7(2) . . . . ?
N1 C13 C14 C15 99.1(2) . . . . ?
N1 C13 C14 C19 -85.0(3) . . . . ?
C19 C14 C15 C16 1.3(3) . . . . ?
C13 C14 C15 C16 177.4(2) . . . . ?
C21 O3 C16 C15 -7.7(4) . . . . ?
C21 O3 C16 C17 173.0(2) . . . . ?
C14 C15 C16 O3 179.6(2) . . . . ?
C14 C15 C16 C17 -1.2(4) . . . . ?
O3 C16 C17 C18 179.3(2) . . . . ?
C15 C16 C17 C18 0.0(4) . . . . ?
C16 C17 C18 C19 1.1(4) . . . . ?
C17 C18 C19 C14 -1.0(4) . . . . ?
C17 C18 C19 C20 -178.0(2) . . . . ?
C15 C14 C19 C18 -0.1(3) . . . . ?
C13 C14 C19 C18 -175.9(2) . . . . ?
C15 C14 C19 C20 176.6(2) . . . . ?
C13 C14 C19 C20 0.9(3) . . . . ?
Cu1 O1 C20 O2 -134.0(2) . . . . ?
Cu1 O1 C20 C19 46.9(3) . . . . ?
C18 C19 C20 O2 15.8(3) . . . . ?
C14 C19 C20 O2 -161.0(2) . . . . ?
C18 C19 C20 O1 -165.0(2) . . . . ?
C14 C19 C20 O1 18.2(3) . . . . ?
Cu1 O4 C22 O5' 7.7(13) . . . . ?
Cu1 O4 C22 O5 -11.9(12) . . . . ?
Cu1 O4 C22 C23 178.41(19) . . . . ?
O4A Cu1A O1A C20A 114.8(2) . . . . ?
N2A Cu1A O1A C20A 18.3(2) . . . . ?
N3A Cu1A O1A C20A -149.6(2) . . . . ?
N1A Cu1A O1A C20A -66.0(2) . . . . ?
N2A Cu1A O4A C22A -80.28(19) . . . . ?
N3A Cu1A O4A C22A 81.89(19) . . . . ?
N1A Cu1A O4A C22A 1.1(7) . . . . ?
O1A Cu1A O4A C22A 174.71(19) . . . . ?
O4A Cu1A N1A C1A -59.2(6) . . . . ?
N2A Cu1A N1A C1A 22.99(14) . . . . ?
N3A Cu1A N1A C1A -140.67(15) . . . . ?
O1A Cu1A N1A C1A 127.26(14) . . . . ?
O4A Cu1A N1A C7A 60.0(6) . . . . ?
N2A Cu1A N1A C7A 142.13(14) . . . . ?
N3A Cu1A N1A C7A -21.53(14) . . . . ?
O1A Cu1A N1A C7A -113.59(14) . . . . ?
O4A Cu1A N1A C13A 177.9(5) . . . . ?
N2A Cu1A N1A C13A -99.97(14) . . . . ?
N3A Cu1A N1A C13A 96.37(14) . . . . ?
O1A Cu1A N1A C13A 4.31(14) . . . . ?
O4A Cu1A N2A C2A 164.82(16) . . . . ?
N3A Cu1A N2A C2A 42.0(3) . . . . ?
N1A Cu1A N2A C2A -8.42(16) . . . . ?
O1A Cu1A N2A C2A -102.94(16) . . . . ?
O4A Cu1A N2A C6A -20.3(2) . . . . ?
N3A Cu1A N2A C6A -143.2(2) . . . . ?
N1A Cu1A N2A C6A 166.5(2) . . . . ?
O1A Cu1A N2A C6A 71.9(2) . . . . ?
O4A Cu1A N3A C12A 19.2(2) . . . . ?
N2A Cu1A N3A C12A 142.1(2) . . . . ?
N1A Cu1A N3A C12A -167.5(2) . . . . ?
O1A Cu1A N3A C12A -71.7(2) . . . . ?
O4A Cu1A N3A C8A -166.13(17) . . . . ?
N2A Cu1A N3A C8A -43.2(3) . . . . ?
N1A Cu1A N3A C8A 7.13(16) . . . . ?
O1A Cu1A N3A C8A 103.00(17) . . . . ?
C7A N1A C1A C2A -149.53(18) . . . . ?
C13A N1A C1A C2A 89.5(2) . . . . ?
Cu1A N1A C1A C2A -33.0(2) . . . . ?
C6A N2A C2A C3A -0.4(3) . . . . ?
Cu1A N2A C2A C3A 174.93(19) . . . . ?
C6A N2A C2A C1A 175.9(2) . . . . ?
Cu1A N2A C2A C1A -8.8(2) . . . . ?
N1A C1A C2A N2A 28.6(3) . . . . ?
N1A C1A C2A C3A -155.2(2) . . . . ?
N2A C2A C3A C4A 0.7(4) . . . . ?
C1A C2A C3A C4A -175.3(2) . . . . ?
C2A C3A C4A C5A -0.8(4) . . . . ?
C3A C4A C5A C6A 0.6(5) . . . . ?
C2A N2A C6A C5A 0.2(4) . . . . ?
Cu1A N2A C6A C5A -174.5(2) . . . . ?
C4A C5A C6A N2A -0.3(5) . . . . ?
C1A N1A C7A C8A 148.62(19) . . . . ?
C13A N1A C7A C8A -88.1(2) . . . . ?
Cu1A N1A C7A C8A 31.9(2) . . . . ?
C12A N3A C8A C9A 0.6(4) . . . . ?
Cu1A N3A C8A C9A -174.45(19) . . . . ?
C12A N3A C8A C7A -174.8(2) . . . . ?
Cu1A N3A C8A C7A 10.1(3) . . . . ?
N1A C7A C8A N3A -28.8(3) . . . . ?
N1A C7A C8A C9A 155.8(2) . . . . ?
N3A C8A C9A C10A -0.9(4) . . . . ?
C7A C8A C9A C10A 174.3(3) . . . . ?
C8A C9A C10A C11A -0.2(5) . . . . ?
C9A C10A C11A C12A 1.4(5) . . . . ?
C8A N3A C12A C11A 0.7(4) . . . . ?
Cu1A N3A C12A C11A 175.1(2) . . . . ?
C10A C11A C12A N3A -1.7(5) . . . . ?
C1A N1A C13A C14A -51.1(2) . . . . ?
C7A N1A C13A C14A -173.67(18) . . . . ?
Cu1A N1A C13A C14A 69.1(2) . . . . ?
N1A C13A C14A C15A 96.8(2) . . . . ?
N1A C13A C14A C19A -88.2(3) . . . . ?
C19A C14A C15A C16A 1.1(3) . . . . ?
C13A C14A C15A C16A 176.4(2) . . . . ?
C21A O3A C16A C15A -8.5(4) . . . . ?
C21A O3A C16A C17A 173.2(2) . . . . ?
C14A C15A C16A O3A -179.3(2) . . . . ?
C14A C15A C16A C17A -1.1(4) . . . . ?
O3A C16A C17A C18A 178.0(2) . . . . ?
C15A C16A C17A C18A -0.4(4) . . . . ?
C16A C17A C18A C19A 1.8(4) . . . . ?
C17A C18A C19A C14A -1.7(4) . . . . ?
C17A C18A C19A C20A -178.3(2) . . . . ?
C15A C14A C19A C18A 0.2(3) . . . . ?
C13A C14A C19A C18A -174.7(2) . . . . ?
C15A C14A C19A C20A 176.6(2) . . . . ?
C13A C14A C19A C20A 1.6(3) . . . . ?
Cu1A O1A C20A O2A -148.76(19) . . . . ?
Cu1A O1A C20A C19A 30.7(3) . . . . ?
C18A C19A C20A O2A 25.4(3) . . . . ?
C14A C19A C20A O2A -151.0(2) . . . . ?
C18A C19A C20A O1A -154.1(2) . . . . ?
C14A C19A C20A O1A 29.5(3) . . . . ?
Cu1A O4A C22A O5B -8.8(10) . . . . ?
Cu1A O4A C22A O5A 15.3(9) . . . . ?
Cu1A O4A C22A C23A -177.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.049
