# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_compound6
_database_code_depnum_ccdc_archive 'CCDC 1522627'
_audit_update_record             
;
2017-03-11 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            
Poly{dihydrogenphosphato-tris(mu-1,2-di(4-pyridyl)ethylene)-bis(mu-pyrazole-3,5-dicarboxylato))pentacopper(II)}
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H34 Cu5 N10 O16 P2'
_chemical_formula_weight         1362.47

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'
P P 0.1023 0.0942 '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                   9.8788(4)
_cell_length_b                   11.1243(4)
_cell_length_c                   13.8420(6)
_cell_angle_alpha                69.7760(10)
_cell_angle_beta                 79.7190(10)
_cell_angle_gamma                64.4060(10)
_cell_volume                     1286.56(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9982
_cell_measurement_theta_min      3.004
_cell_measurement_theta_max      26.009

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_F_000             683
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    2.175
_shelx_estimated_absorpt_T_min   0.812
_shelx_estimated_absorpt_T_max   0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6839
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  
;
Bruker D8 QUEST PHOTON 100
;
_diffrn_measurement_method       '\fandω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            53391
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.004
_diffrn_reflns_theta_max         26.458
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5294
_reflns_number_gt                3845
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       BrukerAPEX2
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0307P)²+2.8291P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5294
_refine_ls_number_parameters     389
_refine_ls_number_restraints     129
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.0903
_refine_ls_wR_factor_gt          0.0801
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.16780(5) 0.87738(5) 0.48234(3) 0.02426(13) Uani 1 1 d . . . . .
Cu2 Cu 0.07142(5) 0.72087(5) 0.80689(4) 0.02936(13) Uani 1 1 d . . . . .
Cu3 Cu 0.0000 0.5000 0.5000 0.02409(16) Uani 1 2 d S . P . .
P1 P -0.05923(11) 0.74867(11) 0.60156(8) 0.0296(2) Uani 1 1 d . . . . .
O1 O 0.3747(3) 0.8639(3) 0.43382(19) 0.0393(7) Uani 1 1 d . . . . .
O2 O 0.5864(3) 0.8463(3) 0.4836(2) 0.0421(7) Uani 1 1 d . . . . .
O3 O 0.1787(3) 0.7182(3) 0.9130(2) 0.0423(7) Uani 1 1 d . . . . .
O4 O 0.3605(4) 0.7710(5) 0.9367(2) 0.0716(12) Uani 1 1 d . . . . .
O5 O -0.0282(3) 0.8789(3) 0.54133(18) 0.0237(5) Uani 1 1 d . . . . .
O6 O 0.0094(3) 0.6756(3) 0.7068(2) 0.0397(7) Uani 1 1 d . . . . .
O7 O -0.0072(4) 0.6501(4) 0.5384(3) 0.0705(12) Uani 1 1 d . . . . .
O8 O -0.2324(3) 0.7972(4) 0.6260(3) 0.0423(8) Uani 1 1 d . . . . .
H10A H -0.276(5) 0.818(4) 0.582(3) 0.029(13) Uiso 1 1 d . . . . .
N1 N 0.2583(3) 0.8148(3) 0.6161(2) 0.0230(7) Uani 1 1 d . . . . .
N2 N 0.2145(3) 0.7895(3) 0.7161(2) 0.0235(7) Uani 1 1 d . . . . .
N3 N 0.1246(4) 0.9063(3) 0.3376(2) 0.0323(8) Uani 1 1 d . . . . .
N4 N 0.1708(4) 0.5221(3) 0.3999(2) 0.0318(8) Uani 1 1 d . . . . .
N5 N -0.0809(4) 0.6798(4) 0.9154(3) 0.0466(10) Uani 1 1 d . . . . .
C1 C 0.3889(4) 0.8296(4) 0.6070(3) 0.0250(8) Uani 1 1 d . . . . .
C2 C 0.4301(4) 0.8150(4) 0.7020(3) 0.0328(9) Uani 1 1 d . . . . .
H2 H 0.5145 0.8209 0.7175 0.039 Uiso 1 1 calc R U . . .
C3 C 0.3175(4) 0.7897(4) 0.7683(3) 0.0286(9) Uani 1 1 d . . . . .
C4 C 0.4575(4) 0.8498(4) 0.5016(3) 0.0299(9) Uani 1 1 d . . . . .
C5 C 0.2864(5) 0.7585(5) 0.8810(3) 0.0396(11) Uani 1 1 d . . . . .
C6 C 0.2081(5) 0.9525(5) 0.2585(3) 0.0479(12) Uani 1 1 d . . . . .
H6 H 0.2866 0.9679 0.2730 0.058 Uiso 1 1 calc R U . . .
C7 C 0.1839(7) 0.9785(5) 0.1574(3) 0.0637(16) Uani 1 1 d . . . . .
H7 H 0.2455 1.0104 0.1056 0.076 Uiso 1 1 calc R U . . .
C8 C 0.0709(7) 0.9580(5) 0.1324(4) 0.0575(13) Uani 1 1 d . U . . .
C9 C -0.0183(6) 0.9101(5) 0.2135(4) 0.0584(13) Uani 1 1 d . U . . .
H9 H -0.0972 0.8946 0.1999 0.070 Uiso 1 1 calc R U . . .
C10 C 0.0116(5) 0.8857(4) 0.3154(3) 0.0437(11) Uani 1 1 d . . . . .
H10 H -0.0486 0.8544 0.3687 0.052 Uiso 1 1 calc R U . . .
C12 C 0.2874(5) 0.5263(6) 0.4309(4) 0.0619(15) Uani 1 1 d . . . . .
H12 H 0.2925 0.5136 0.5004 0.074 Uiso 1 1 calc R U . . .
C13 C 0.4020(6) 0.5489(7) 0.3640(6) 0.084(2) Uani 1 1 d . . . . .
H13 H 0.4815 0.5507 0.3898 0.100 Uiso 1 1 calc R U . . .
C14 C 0.4012(7) 0.5685(5) 0.2620(5) 0.0693(16) Uani 1 1 d . U . . .
C15 C 0.2789(7) 0.5664(5) 0.2309(4) 0.0680(18) Uani 1 1 d . . . . .
H15 H 0.2703 0.5816 0.1614 0.082 Uiso 1 1 calc R U . . .
C16 C 0.1674(6) 0.5421(5) 0.3008(4) 0.0484(12) Uani 1 1 d . . . . .
H16 H 0.0868 0.5397 0.2767 0.058 Uiso 1 1 calc R U . . .
C19 C -0.0784(6) 0.6767(5) 1.0125(4) 0.0660(16) Uani 1 1 d . . . . .
H19 H -0.0023 0.6920 1.0306 0.079 Uiso 1 1 calc R U . . .
C20 C -0.1854(8) 0.6516(6) 1.0873(5) 0.089(2) Uani 1 1 d . . . . .
H20 H -0.1809 0.6518 1.1538 0.107 Uiso 1 1 calc R U . . .
C21 C -0.2987(7) 0.6262(6) 1.0630(6) 0.083(2) Uani 1 1 d . U . . .
C22 C -0.2996(6) 0.6290(6) 0.9641(6) 0.085(2) Uani 1 1 d . . . . .
H22 H -0.3738 0.6126 0.9445 0.102 Uiso 1 1 calc R U . . .
C23 C -0.1907(5) 0.6562(5) 0.8918(5) 0.0645(16) Uani 1 1 d . . . . .
H23 H -0.1946 0.6581 0.8247 0.077 Uiso 1 1 calc R U . . .
C17A C 0.5432(12) 0.5880(10) 0.2109(8) 0.057(2) Uani 0.6 1 d . U P A 1
H17A H 0.6100 0.5931 0.2473 0.069 Uiso 0.6 1 calc R U P A 1
C18A C -0.4347(11) 0.5966(9) 1.1175(7) 0.052(2) Uani 0.6 1 d . U P B 1
H18A H -0.4985 0.5855 1.0826 0.062 Uiso 0.6 1 calc R U P B 1
C11A C 0.0614(9) 0.9948(7) 0.0194(6) 0.0284(14) Uani 0.6 1 d . U P C 1
H11A H 0.1389 1.0108 -0.0245 0.034 Uiso 0.6 1 calc R U P C 1
C17B C 0.4900(13) 0.5952(13) 0.1603(11) 0.040(2) Uani 0.4 1 d . U P A 2
H17B H 0.4584 0.6046 0.0977 0.048 Uiso 0.4 1 calc R U P A 2
C18B C -0.3816(13) 0.6036(12) 1.1702(11) 0.040(2) Uani 0.4 1 d . U P B 2
H18B H -0.3479 0.5971 1.2312 0.048 Uiso 0.4 1 calc R U P B 2
C11B C -0.0271(18) 0.9777(12) 0.0406(10) 0.046(2) Uani 0.4 1 d . U P C 2
H11B H -0.1115 0.9574 0.0501 0.055 Uiso 0.4 1 calc R U P C 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O5 1.957(2) . ?
Cu1 N1 1.968(3) . ?
Cu1 O1 1.991(3) . ?
Cu1 N3 2.010(3) . ?
Cu1 O5 2.382(2) 2_576 ?
Cu2 O6 1.898(3) . ?
Cu2 O3 1.944(3) . ?
Cu2 N2 1.948(3) . ?
Cu2 N5 2.011(3) . ?
Cu3 O7 1.890(3) 2_566 ?
Cu3 O7 1.890(3) . ?
Cu3 N4 2.029(3) 2_566 ?
Cu3 N4 2.029(3) . ?
P1 O7 1.499(3) . ?
P1 O6 1.516(3) . ?
P1 O5 1.532(3) . ?
P1 O8 1.566(3) . ?
O1 C4 1.279(4) . ?
O2 C4 1.239(4) . ?
O3 C5 1.278(5) . ?
O4 C5 1.230(5) . ?
O5 Cu1 2.382(2) 2_576 ?
O8 H10A 0.72(4) . ?
N1 N2 1.343(4) . ?
N1 C1 1.348(4) . ?
N2 C3 1.350(5) . ?
N3 C10 1.336(5) . ?
N3 C6 1.342(5) . ?
N4 C16 1.316(5) . ?
N4 C12 1.323(6) . ?
N5 C23 1.336(7) . ?
N5 C19 1.336(7) . ?
C1 C2 1.382(5) . ?
C1 C4 1.480(5) . ?
C2 C3 1.373(5) . ?
C2 H2 0.9300 . ?
C3 C5 1.482(5) . ?
C6 C7 1.371(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.353(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.400(8) . ?
C8 C11A 1.482(9) . ?
C8 C11B 1.631(17) . ?
C9 C10 1.401(6) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C12 C13 1.383(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.353(9) . ?
C13 H13 0.9300 . ?
C14 C15 1.365(9) . ?
C14 C17A 1.522(11) . ?
C14 C17B 1.529(14) . ?
C15 C16 1.385(6) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C19 C20 1.390(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.385(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.360(10) . ?
C21 C18A 1.527(10) . ?
C21 C18B 1.556(13) . ?
C22 C23 1.392(7) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C17A C18A 1.249(14) 1_654 ?
C17A H17A 0.9300 . ?
C18A C17A 1.249(14) 1_456 ?
C18A H18A 0.9300 . ?
C11A C11A 1.358(14) 2_575 ?
C11A H11A 0.9300 . ?
C17B C18B 1.346(17) 1_654 ?
C17B H17B 0.9300 . ?
C18B C17B 1.346(17) 1_456 ?
C18B H18B 0.9300 . ?
C11B C11B 1.19(3) 2_575 ?
C11B H11B 0.9300 . ?

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 Cu1 N1 95.01(10) . . ?
O5 Cu1 O1 175.05(11) . . ?
N1 Cu1 O1 80.46(11) . . ?
O5 Cu1 N3 95.35(12) . . ?
N1 Cu1 N3 165.77(12) . . ?
O1 Cu1 N3 88.78(12) . . ?
O5 Cu1 O5 79.52(10) . 2_576 ?
N1 Cu1 O5 101.82(11) . 2_576 ?
O1 Cu1 O5 103.29(11) . 2_576 ?
N3 Cu1 O5 89.64(11) . 2_576 ?
O6 Cu2 O3 164.58(12) . . ?
O6 Cu2 N2 95.87(12) . . ?
O3 Cu2 N2 82.49(12) . . ?
O6 Cu2 N5 94.75(15) . . ?
O3 Cu2 N5 88.87(15) . . ?
N2 Cu2 N5 167.75(15) . . ?
O7 Cu3 O7 180.0(2) 2_566 . ?
O7 Cu3 N4 87.21(12) 2_566 2_566 ?
O7 Cu3 N4 92.79(12) . 2_566 ?
O7 Cu3 N4 92.79(12) 2_566 . ?
O7 Cu3 N4 87.21(12) . . ?
N4 Cu3 N4 180.0 2_566 . ?
O7 P1 O6 111.0(2) . . ?
O7 P1 O5 109.66(17) . . ?
O6 P1 O5 113.45(14) . . ?
O7 P1 O8 110.70(18) . . ?
O6 P1 O8 103.98(17) . . ?
O5 P1 O8 107.88(17) . . ?
C4 O1 Cu1 115.7(2) . . ?
C5 O3 Cu2 115.8(2) . . ?
P1 O5 Cu1 125.06(15) . . ?
P1 O5 Cu1 133.58(13) . 2_576 ?
Cu1 O5 Cu1 100.48(10) . 2_576 ?
P1 O6 Cu2 138.28(18) . . ?
P1 O7 Cu3 155.3(2) . . ?
P1 O8 H10A 114(3) . . ?
N2 N1 C1 107.6(3) . . ?
N2 N1 Cu1 137.8(2) . . ?
C1 N1 Cu1 112.7(2) . . ?
N1 N2 C3 108.1(3) . . ?
N1 N2 Cu2 138.1(2) . . ?
C3 N2 Cu2 112.6(2) . . ?
C10 N3 C6 117.4(4) . . ?
C10 N3 Cu1 122.8(3) . . ?
C6 N3 Cu1 119.7(3) . . ?
C16 N4 C12 116.7(4) . . ?
C16 N4 Cu3 122.4(3) . . ?
C12 N4 Cu3 120.8(3) . . ?
C23 N5 C19 117.4(4) . . ?
C23 N5 Cu2 120.4(4) . . ?
C19 N5 Cu2 122.2(4) . . ?
N1 C1 C2 110.3(3) . . ?
N1 C1 C4 114.4(3) . . ?
C2 C1 C4 135.2(3) . . ?
C3 C2 C1 103.8(3) . . ?
C3 C2 H2 128.1 . . ?
C1 C2 H2 128.1 . . ?
N2 C3 C2 110.2(3) . . ?
N2 C3 C5 114.2(3) . . ?
C2 C3 C5 135.6(4) . . ?
O2 C4 O1 124.2(3) . . ?
O2 C4 C1 121.9(3) . . ?
O1 C4 C1 113.8(3) . . ?
O4 C5 O3 124.6(4) . . ?
O4 C5 C3 121.3(4) . . ?
O3 C5 C3 114.2(4) . . ?
N3 C6 C7 123.6(5) . . ?
N3 C6 H6 118.2 . . ?
C7 C6 H6 118.2 . . ?
C8 C7 C6 120.4(5) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 117.2(4) . . ?
C7 C8 C11A 112.1(6) . . ?
C9 C8 C11A 130.7(6) . . ?
C7 C8 C11B 146.8(7) . . ?
C9 C8 C11B 95.7(7) . . ?
C8 C9 C10 119.9(5) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
N3 C10 C9 121.6(5) . . ?
N3 C10 H10 119.2 . . ?
C9 C10 H10 119.2 . . ?
N4 C12 C13 122.6(5) . . ?
N4 C12 H12 118.7 . . ?
C13 C12 H12 118.7 . . ?
C14 C13 C12 121.7(6) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C13 C14 C15 115.1(5) . . ?
C13 C14 C17A 108.6(7) . . ?
C15 C14 C17A 136.3(7) . . ?
C13 C14 C17B 143.3(8) . . ?
C15 C14 C17B 101.6(7) . . ?
C14 C15 C16 121.2(5) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
N4 C16 C15 122.7(5) . . ?
N4 C16 H16 118.6 . . ?
C15 C16 H16 118.6 . . ?
N5 C19 C20 122.5(6) . . ?
N5 C19 H19 118.8 . . ?
C20 C19 H19 118.8 . . ?
C21 C20 C19 120.1(6) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C22 C21 C20 116.9(5) . . ?
C22 C21 C18A 105.6(7) . . ?
C20 C21 C18A 137.6(8) . . ?
C22 C21 C18B 143.9(8) . . ?
C20 C21 C18B 99.3(8) . . ?
C21 C22 C23 120.7(7) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
N5 C23 C22 122.4(6) . . ?
N5 C23 H23 118.8 . . ?
C22 C23 H23 118.8 . . ?
C18A C17A C14 116.5(11) 1_654 . ?
C18A C17A H17A 121.7 1_654 . ?
C14 C17A H17A 121.7 . . ?
C17A C18A C21 117.4(11) 1_456 . ?
C17A C18A H18A 121.3 1_456 . ?
C21 C18A H18A 121.3 . . ?
C11A C11A C8 119.5(10) 2_575 . ?
C11A C11A H11A 120.2 2_575 . ?
C8 C11A H11A 120.2 . . ?
C18B C17B C14 113.4(13) 1_654 . ?
C18B C17B H17B 123.3 1_654 . ?
C14 C17B H17B 123.3 . . ?
C17B C18B C21 108.8(13) 1_456 . ?
C17B C18B H18B 125.6 1_456 . ?
C21 C18B H18B 125.6 . . ?
C11B C11B C8 109(2) 2_575 . ?
C11B C11B H11B 125.6 2_575 . ?
C8 C11B H11B 125.6 . . ?

_refine_diff_density_max         0.711
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.091



####################################################################### 
# 
# 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_compound5
_database_code_depnum_ccdc_archive 'CCDC 1522626'
_audit_update_record             
;
2017-03-11 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            
Poly{hexakis(mu-1,2-di(4-pyridyl)ethylene)-tetrakis(mu3-pyrazole-3,5-dicarboxylato)tetracopper(I)tetracopper(II)}
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C184 H128 Cu16 N40 O32'
_chemical_formula_weight         4427.90

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   16.3570(7)
_cell_length_b                   26.4808(12)
_cell_length_c                   21.4340(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.7730(10)
_cell_angle_gamma                90
_cell_volume                     9263.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9830
_cell_measurement_theta_min      2.932
_cell_measurement_theta_max      24.237

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_F_000             4464
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.876
_shelx_estimated_absorpt_T_min   0.806
_shelx_estimated_absorpt_T_max   0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6773
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  
;
Bruker D8 QUEST PHOTON 100
;
_diffrn_measurement_method       '\fandω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            267493
_diffrn_reflns_av_unetI/netI     0.1063
_diffrn_reflns_av_R_equivalents  0.097
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.836
_diffrn_reflns_theta_max         26.435
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             18998
_reflns_number_gt                10197
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       BrukerAPEX2
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0615P)²+5.3176P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18998
_refine_ls_number_parameters     1225
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0634
_refine_ls_wR_factor_ref         0.1417
_refine_ls_wR_factor_gt          0.1152
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5725(3) 0.45480(19) 0.4005(2) 0.0297(13) Uani 1 1 d . . . . .
C2 C 0.5225(4) 0.4970(2) 0.3917(3) 0.0434(16) Uani 1 1 d . . . . .
H2 H 0.4662 0.4977 0.3823 0.052 Uiso 1 1 calc R U . . .
C3 C 0.5756(3) 0.5381(2) 0.4001(2) 0.0325(13) Uani 1 1 d . . . . .
C4 C 0.5670(4) 0.3987(2) 0.3969(2) 0.0338(13) Uani 1 1 d . . . . .
C5 C 0.5739(4) 0.5941(2) 0.3937(3) 0.0410(15) Uani 1 1 d . . . . .
C6 C 0.8937(3) 0.4493(2) 0.3940(2) 0.0301(13) Uani 1 1 d . . . . .
C7 C 0.9429(3) 0.4899(2) 0.3794(3) 0.0390(14) Uani 1 1 d . . . . .
H7 H 0.9958 0.4889 0.3661 0.047 Uiso 1 1 calc R U . . .
C8 C 0.8956(3) 0.53215(19) 0.3892(2) 0.0292(13) Uani 1 1 d . . . . .
C9 C 0.8943(4) 0.3931(2) 0.3909(2) 0.0335(14) Uani 1 1 d . . . . .
C10 C 0.8990(4) 0.5880(2) 0.3790(3) 0.0417(15) Uani 1 1 d . . . . .
C11 C 0.6161(3) 0.5544(2) 1.0995(2) 0.0310(13) Uani 1 1 d . . . . .
C12 C 0.5630(3) 0.5159(2) 1.1141(3) 0.0405(15) Uani 1 1 d . . . . .
H12 H 0.5112 0.5189 1.1291 0.049 Uiso 1 1 calc R U . . .
C13 C 0.6047(3) 0.4718(2) 1.1011(2) 0.0342(14) Uani 1 1 d . . . . .
C14 C 0.6190(4) 0.6103(2) 1.1068(2) 0.0306(13) Uani 1 1 d . . . . .
C15 C 0.5959(4) 0.4157(2) 1.1099(3) 0.0440(15) Uani 1 1 d . . . . .
C16 C 0.9323(3) 0.5382(2) 1.0882(2) 0.0340(14) Uani 1 1 d . . . . .
C17 C 0.9789(3) 0.4944(2) 1.0988(3) 0.0401(15) Uani 1 1 d . . . . .
H17 H 1.0347 0.4919 1.1098 0.048 Uiso 1 1 calc R U . . .
C18 C 0.9226(3) 0.4555(2) 1.0891(2) 0.0327(13) Uani 1 1 d . . . . .
C19 C 0.9424(4) 0.5940(2) 1.0942(3) 0.0390(14) Uani 1 1 d . . . . .
C20 C 0.9195(4) 0.3995(2) 1.0961(2) 0.0337(14) Uani 1 1 d . . . . .
C21 C 0.6794(3) 0.4218(2) 0.5607(2) 0.0355(14) Uani 1 1 d . . . . .
H21 H 0.6280 0.4233 0.5397 0.043 Uiso 1 1 calc R U . . .
C22 C 0.6842(3) 0.4243(2) 0.6253(2) 0.0358(14) Uani 1 1 d . . . . .
H22 H 0.6366 0.4274 0.6465 0.043 Uiso 1 1 calc R U . . .
C23 C 0.7599(3) 0.42243(19) 0.6584(2) 0.0305(13) Uani 1 1 d . . . . .
C24 C 0.8282(3) 0.4192(2) 0.6230(2) 0.0422(15) Uani 1 1 d . . . . .
H24 H 0.8806 0.4190 0.6427 0.051 Uiso 1 1 calc R U . . .
C25 C 0.8178(4) 0.4163(2) 0.5586(3) 0.0442(16) Uani 1 1 d . . . . .
H25 H 0.8642 0.4136 0.5360 0.053 Uiso 1 1 calc R U . . .
C26 C 0.7700(3) 0.4239(2) 0.7266(2) 0.0378(14) Uani 1 1 d . . . . .
H26 H 0.8234 0.4263 0.7441 0.045 Uiso 1 1 calc R U . . .
C27 C 0.7114(4) 0.4220(2) 0.7660(2) 0.0377(14) Uani 1 1 d . . . . .
H27 H 0.6577 0.4205 0.7488 0.045 Uiso 1 1 calc R U . . .
C28 C 0.6672(4) 0.4176(2) 0.9345(3) 0.0419(15) Uani 1 1 d . . . . .
H28 H 0.6214 0.4143 0.9576 0.050 Uiso 1 1 calc R U . . .
C29 C 0.6554(3) 0.4173(2) 0.8702(3) 0.0427(15) Uani 1 1 d . . . . .
H29 H 0.6030 0.4139 0.8510 0.051 Uiso 1 1 calc R U . . .
C30 C 0.7229(3) 0.4222(2) 0.8342(2) 0.0339(13) Uani 1 1 d . . . . .
C31 C 0.7990(3) 0.4272(2) 0.8664(2) 0.0389(15) Uani 1 1 d . . . . .
H31 H 0.8461 0.4309 0.8447 0.047 Uiso 1 1 calc R U . . .
C32 C 0.8040(3) 0.4267(2) 0.9311(2) 0.0393(15) Uani 1 1 d . . . . .
H32 H 0.8556 0.4297 0.9518 0.047 Uiso 1 1 calc R U . . .
C33 C 0.6876(3) 0.5736(2) 0.5570(3) 0.0398(15) Uani 1 1 d . . . . .
H33 H 0.6358 0.5749 0.5363 0.048 Uiso 1 1 calc R U . . .
C34 C 0.6926(4) 0.5716(2) 0.6216(3) 0.0410(15) Uani 1 1 d . . . . .
H34 H 0.6452 0.5711 0.6433 0.049 Uiso 1 1 calc R U . . .
C35 C 0.7693(4) 0.5701(2) 0.6539(2) 0.0397(15) Uani 1 1 d . . . . .
C36 C 0.8362(4) 0.5719(2) 0.6181(3) 0.0443(16) Uani 1 1 d . . . . .
H36 H 0.8887 0.5725 0.6376 0.053 Uiso 1 1 calc R U . . .
C37 C 0.8259(4) 0.5729(2) 0.5539(3) 0.0444(16) Uani 1 1 d . . . . .
H37 H 0.8723 0.5727 0.5311 0.053 Uiso 1 1 calc R U . . .
C38 C 0.7825(4) 0.5698(2) 0.7229(3) 0.0441(15) Uani 1 1 d . . . . .
H38 H 0.8363 0.5721 0.7395 0.053 Uiso 1 1 calc R U . . .
C39 C 0.7262(4) 0.5666(2) 0.7620(3) 0.0465(16) Uani 1 1 d . . . . .
H39 H 0.6726 0.5622 0.7457 0.056 Uiso 1 1 calc R U . . .
C40 C 0.6866(4) 0.5715(2) 0.9314(3) 0.0431(15) Uani 1 1 d . . . . .
H40 H 0.6413 0.5687 0.9553 0.052 Uiso 1 1 calc R U . . .
C41 C 0.6734(4) 0.5665(2) 0.8680(3) 0.0463(16) Uani 1 1 d . . . . .
H41 H 0.6208 0.5614 0.8500 0.056 Uiso 1 1 calc R U . . .
C42 C 0.7402(4) 0.5693(2) 0.8307(2) 0.0397(15) Uani 1 1 d . . . . .
C43 C 0.8169(4) 0.5771(2) 0.8615(3) 0.0412(15) Uani 1 1 d . . . . .
H43 H 0.8635 0.5788 0.8389 0.049 Uiso 1 1 calc R U . . .
C44 C 0.8231(4) 0.5821(2) 0.9265(3) 0.0393(14) Uani 1 1 d . . . . .
H44 H 0.8747 0.5872 0.9464 0.047 Uiso 1 1 calc R U . . .
C45 C 0.3980(3) 0.3115(2) 0.2780(2) 0.0345(14) Uani 1 1 d . . . . .
H45 H 0.4096 0.3451 0.2874 0.041 Uiso 1 1 calc R U . . .
C46 C 0.3439(3) 0.3010(2) 0.2277(2) 0.0345(14) Uani 1 1 d . . . . .
H46 H 0.3198 0.3274 0.2045 0.041 Uiso 1 1 calc R U . . .
C47 C 0.3251(3) 0.2519(2) 0.2114(2) 0.0288(12) Uani 1 1 d . . . . .
C48 C 0.3647(3) 0.2150(2) 0.2480(2) 0.0313(13) Uani 1 1 d . . . . .
H48 H 0.3552 0.1812 0.2387 0.038 Uiso 1 1 calc R U . . .
C49 C 0.4175(3) 0.2278(2) 0.2976(2) 0.0330(13) Uani 1 1 d . . . . .
H49 H 0.4426 0.2020 0.3211 0.040 Uiso 1 1 calc R U . . .
C50 C 0.2683(3) 0.2379(2) 0.1593(2) 0.0307(13) Uani 1 1 d . . . . .
H50 H 0.2582 0.2036 0.1538 0.037 Uiso 1 1 calc R U . . .
C51 C 0.2291(3) 0.2691(2) 0.1185(2) 0.0321(13) Uani 1 1 d . . . . .
H51 H 0.2383 0.3035 0.1239 0.038 Uiso 1 1 calc R U . . .
C52 C 0.0999(3) 0.2727(2) -0.0320(2) 0.0282(12) Uani 1 1 d . . . . .
H52 H 0.0866 0.2961 -0.0634 0.034 Uiso 1 1 calc R U . . .
C53 C 0.1510(3) 0.28755(19) 0.0174(2) 0.0293(13) Uani 1 1 d . . . . .
H53 H 0.1715 0.3203 0.0189 0.035 Uiso 1 1 calc R U . . .
C54 C 0.1727(3) 0.2536(2) 0.0659(2) 0.0262(12) Uani 1 1 d . . . . .
C55 C 0.1383(3) 0.20629(19) 0.0600(2) 0.0292(13) Uani 1 1 d . . . . .
H55 H 0.1502 0.1822 0.0909 0.035 Uiso 1 1 calc R U . . .
C56 C 0.0868(3) 0.1942(2) 0.0096(2) 0.0318(13) Uani 1 1 d . . . . .
H56 H 0.0638 0.1621 0.0078 0.038 Uiso 1 1 calc R U . . .
C57 C 1.0791(3) 0.3045(2) 0.4653(2) 0.0348(14) Uani 1 1 d . . . . .
H57 H 1.0670 0.3379 0.4548 0.042 Uiso 1 1 calc R U . . .
C58 C 1.1345(3) 0.2953(2) 0.5149(2) 0.0360(14) Uani 1 1 d . . . . .
H58 H 1.1587 0.3222 0.5371 0.043 Uiso 1 1 calc R U . . .
C59 C 1.1544(3) 0.2462(2) 0.5319(2) 0.0256(12) Uani 1 1 d . . . . .
C60 C 1.1163(3) 0.2084(2) 0.4961(2) 0.0341(14) Uani 1 1 d . . . . .
H60 H 1.1280 0.1747 0.5055 0.041 Uiso 1 1 calc R U . . .
C61 C 1.0615(3) 0.2200(2) 0.4469(2) 0.0362(14) Uani 1 1 d . . . . .
H61 H 1.0370 0.1939 0.4235 0.043 Uiso 1 1 calc R U . . .
C62 C 1.2120(3) 0.2326(2) 0.5861(2) 0.0220(11) Uani 1 1 d . . . . .
H62 H 1.2215 0.1985 0.5939 0.026 Uiso 1 1 calc R U . . .
C63 C 1.2495(3) 0.2644(2) 0.6227(2) 0.0372(15) Uani 1 1 d . . . . .
H63 H 1.2416 0.2986 0.6142 0.045 Uiso 1 1 calc R U . . .
C64 C 1.3871(3) 0.2765(2) 0.7682(2) 0.0389(15) Uani 1 1 d . . . . .
H64 H 1.4105 0.3026 0.7922 0.047 Uiso 1 1 calc R U . . .
C65 C 1.3404(3) 0.2885(2) 0.7141(3) 0.0407(15) Uani 1 1 d . . . . .
H65 H 1.3330 0.3220 0.7023 0.049 Uiso 1 1 calc R U . . .
C66 C 1.3048(3) 0.2504(2) 0.6777(2) 0.0304(13) Uani 1 1 d . . . . .
C67 C 1.3209(3) 0.2009(2) 0.6965(2) 0.0368(14) Uani 1 1 d . . . . .
H67 H 1.3002 0.1741 0.6723 0.044 Uiso 1 1 calc R U . . .
C68 C 1.3678(3) 0.1918(2) 0.7512(2) 0.0358(14) Uani 1 1 d . . . . .
H68 H 1.3773 0.1585 0.7635 0.043 Uiso 1 1 calc R U . . .
C69 C 0.8932(3) 0.30370(19) 0.9888(2) 0.0277(12) Uani 1 1 d . . . . .
H69 H 0.9135 0.3365 0.9918 0.033 Uiso 1 1 calc R U . . .
C70 C 0.8406(3) 0.29168(19) 0.9387(2) 0.0298(13) Uani 1 1 d . . . . .
H70 H 0.8259 0.3161 0.9088 0.036 Uiso 1 1 calc R U . . .
C71 C 0.8090(3) 0.2431(2) 0.9321(2) 0.0270(13) Uani 1 1 d . . . . .
C72 C 0.8369(3) 0.20820(19) 0.9771(2) 0.0268(12) Uani 1 1 d . . . . .
H72 H 0.8202 0.1747 0.9737 0.032 Uiso 1 1 calc R U . . .
C73 C 0.8888(3) 0.2230(2) 1.0262(2) 0.0258(12) Uani 1 1 d . . . . .
H73 H 0.9055 0.1989 1.0559 0.031 Uiso 1 1 calc R U . . .
C74 C 0.7503(3) 0.2281(2) 0.8810(2) 0.0310(13) Uani 1 1 d . . . . .
H74 H 0.7425 0.1937 0.8740 0.037 Uiso 1 1 calc R U . . .
C75 C 0.7069(3) 0.2602(2) 0.8436(2) 0.0319(14) Uani 1 1 d . . . . .
H75 H 0.7140 0.2944 0.8519 0.038 Uiso 1 1 calc R U . . .
C76 C 0.5605(3) 0.2724(2) 0.7031(2) 0.0288(12) Uani 1 1 d . . . . .
H76 H 0.5365 0.2986 0.6794 0.035 Uiso 1 1 calc R U . . .
C77 C 0.6116(3) 0.28420(19) 0.7547(2) 0.0298(13) Uani 1 1 d . . . . .
H77 H 0.6208 0.3179 0.7653 0.036 Uiso 1 1 calc R U . . .
C78 C 0.6493(3) 0.2467(2) 0.7908(2) 0.0279(12) Uani 1 1 d . . . . .
C79 C 0.6297(3) 0.1973(2) 0.7741(2) 0.0349(14) Uani 1 1 d . . . . .
H79 H 0.6515 0.1706 0.7979 0.042 Uiso 1 1 calc R U . . .
C80 C 0.5779(3) 0.1879(2) 0.7221(2) 0.0323(13) Uani 1 1 d . . . . .
H80 H 0.5659 0.1545 0.7118 0.039 Uiso 1 1 calc R U . . .
C81 C 0.8053(3) 0.7780(2) 1.1708(2) 0.0364(14) Uani 1 1 d . . . . .
H81 H 0.7838 0.8038 1.1452 0.044 Uiso 1 1 calc R U . . .
C82 C 0.8574(3) 0.7905(2) 1.2210(2) 0.0336(13) Uani 1 1 d . . . . .
H82 H 0.8700 0.8243 1.2290 0.040 Uiso 1 1 calc R U . . .
C83 C 0.8912(3) 0.7535(2) 1.2598(2) 0.0264(12) Uani 1 1 d . . . . .
C84 C 0.8697(3) 0.7039(2) 1.2447(2) 0.0362(14) Uani 1 1 d . . . . .
H84 H 0.8908 0.6775 1.2695 0.043 Uiso 1 1 calc R U . . .
C85 C 0.8175(3) 0.6939(2) 1.1936(2) 0.0358(14) Uani 1 1 d . . . . .
H85 H 0.8049 0.6605 1.1841 0.043 Uiso 1 1 calc R U . . .
C86 C 0.9456(3) 0.7672(2) 1.3143(2) 0.0285(13) Uani 1 1 d . . . . .
H86 H 0.9523 0.8014 1.3231 0.034 Uiso 1 1 calc R U . . .
C87 C 0.9858(3) 0.7349(2) 1.3520(2) 0.0304(13) Uani 1 1 d . . . . .
H87 H 0.9778 0.7007 1.3436 0.036 Uiso 1 1 calc R U . . .
C88 C 1.1109(3) 0.8050(2) 1.4758(2) 0.0324(13) Uani 1 1 d . . . . .
H88 H 1.1221 0.8383 1.4872 0.039 Uiso 1 1 calc R U . . .
C89 C 1.0601(3) 0.79674(19) 1.4235(2) 0.0295(13) Uani 1 1 d . . . . .
H89 H 1.0382 0.8238 1.4004 0.035 Uiso 1 1 calc R U . . .
C90 C 1.0415(3) 0.7478(2) 1.4054(2) 0.0255(12) Uani 1 1 d . . . . .
C91 C 1.0783(3) 0.7095(2) 1.4417(2) 0.0305(13) Uani 1 1 d . . . . .
H91 H 1.0684 0.6759 1.4310 0.037 Uiso 1 1 calc R U . . .
C92 C 1.1294(3) 0.7211(2) 1.4931(2) 0.0325(13) Uani 1 1 d . . . . .
H92 H 1.1538 0.6948 1.5162 0.039 Uiso 1 1 calc R U . . .
N1 N 0.6500(3) 0.47018(16) 0.41385(19) 0.0308(11) Uani 1 1 d . . . . .
N2 N 0.6515(3) 0.52030(15) 0.41345(19) 0.0305(11) Uani 1 1 d . . . . .
N3 N 0.8213(3) 0.46698(16) 0.41128(18) 0.0285(10) Uani 1 1 d . . . . .
N4 N 0.8226(3) 0.51752(16) 0.40826(19) 0.0307(11) Uani 1 1 d . . . . .
N5 N 0.6843(3) 0.53407(17) 1.07906(18) 0.0303(11) Uani 1 1 d . . . . .
N6 N 0.6778(3) 0.48401(16) 1.08011(19) 0.0311(11) Uani 1 1 d . . . . .
N7 N 0.8546(3) 0.52442(16) 1.07276(19) 0.0313(11) Uani 1 1 d . . . . .
N8 N 0.8482(3) 0.47490(16) 1.07356(19) 0.0325(11) Uani 1 1 d . . . . .
N9 N 0.7448(3) 0.41718(16) 0.52710(19) 0.0325(11) Uani 1 1 d . . . . .
N10 N 0.7398(3) 0.42225(17) 0.96556(19) 0.0349(11) Uani 1 1 d . . . . .
N11 N 0.7528(3) 0.57396(16) 0.52279(19) 0.0344(11) Uani 1 1 d . . . . .
N12 N 0.7586(3) 0.58005(17) 0.96148(19) 0.0350(11) Uani 1 1 d . . . . .
N13 N 0.4348(2) 0.27568(17) 0.31411(19) 0.0292(10) Uani 1 1 d . . . . .
N14 N 0.0677(2) 0.22637(16) -0.03776(18) 0.0248(10) Uani 1 1 d . . . . .
N15 N 1.0417(2) 0.26803(17) 0.43118(18) 0.0287(10) Uani 1 1 d . . . . .
N16 N 1.4001(2) 0.22893(18) 0.78734(19) 0.0309(11) Uani 1 1 d . . . . .
N17 N 0.9171(2) 0.27035(16) 1.03431(18) 0.0251(10) Uani 1 1 d . . . . .
N18 N 0.5437(2) 0.22444(16) 0.68544(18) 0.0254(10) Uani 1 1 d . . . . .
N19 N 0.7839(2) 0.73031(18) 1.15678(18) 0.0301(11) Uani 1 1 d . . . . .
N20 N 1.1456(2) 0.76839(17) 1.51144(18) 0.0281(10) Uani 1 1 d . . . . .
O1 O 0.6355(2) 0.37575(13) 0.40321(16) 0.0334(9) Uani 1 1 d . . . . .
O2 O 0.4997(2) 0.37715(14) 0.38714(19) 0.0512(11) Uani 1 1 d . . . . .
O3 O 0.6449(2) 0.61523(13) 0.40163(17) 0.0367(9) Uani 1 1 d . . . . .
O4 O 0.5096(3) 0.61673(15) 0.3815(2) 0.0680(14) Uani 1 1 d . . . . .
O5 O 0.8265(2) 0.37147(13) 0.40276(15) 0.0318(9) Uani 1 1 d . . . . .
O6 O 0.9565(2) 0.36990(14) 0.37672(18) 0.0446(10) Uani 1 1 d . . . . .
O7 O 0.8334(2) 0.61170(13) 0.39080(17) 0.0377(9) Uani 1 1 d . . . . .
O8 O 0.9606(3) 0.60793(16) 0.3583(2) 0.0726(15) Uani 1 1 d . . . . .
O9 O 0.6888(2) 0.62952(13) 1.09176(15) 0.0343(9) Uani 1 1 d . . . . .
O10 O 0.5620(2) 0.63484(15) 1.12523(19) 0.0500(11) Uani 1 1 d . . . . .
O11 O 0.6582(2) 0.38984(13) 1.09445(17) 0.0401(10) Uani 1 1 d . . . . .
O12 O 0.5339(3) 0.39845(17) 1.1311(2) 0.0752(15) Uani 1 1 d . . . . .
O13 O 0.8754(2) 0.61887(13) 1.08176(17) 0.0393(10) Uani 1 1 d . . . . .
O14 O 1.0082(3) 0.61334(16) 1.1114(2) 0.0683(14) Uani 1 1 d . . . . .
O15 O 0.8472(2) 0.38032(13) 1.08875(15) 0.0342(9) Uani 1 1 d . . . . .
O16 O 0.9830(2) 0.37443(14) 1.10748(18) 0.0456(10) Uani 1 1 d . . . . .
Cu1 Cu 0.73462(4) 0.41943(2) 0.42194(3) 0.02812(17) Uani 1 1 d . . . . .
Cu2 Cu 0.74021(4) 0.56876(2) 0.41714(3) 0.02906(17) Uani 1 1 d . . . . .
Cu3 Cu 0.77466(4) 0.57851(2) 1.06632(3) 0.02935(17) Uani 1 1 d . . . . .
Cu4 Cu 0.75523(4) 0.42986(2) 1.07004(3) 0.02971(17) Uani 1 1 d . . . . .
Cu5 Cu 0.50423(4) 0.29311(3) 0.38724(3) 0.03567(19) Uani 1 1 d . . . . .
Cu6 Cu 0.96455(4) 0.28417(3) 0.36326(3) 0.0426(2) Uani 1 1 d . . . . .
Cu7 Cu 0.97736(4) 0.29140(3) 1.10993(3) 0.03290(18) Uani 1 1 d . . . . .
Cu8 Cu 0.70929(4) 0.71704(3) 1.08671(3) 0.0402(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 N1 1.344(6) . ?
C1 C2 1.391(7) . ?
C1 C4 1.491(7) . ?
C2 C3 1.396(7) . ?
C2 H2 0.9300 . ?
C3 N2 1.342(6) . ?
C3 C5 1.490(7) . ?
C4 O2 1.245(6) . ?
C4 O1 1.274(6) . ?
C5 O4 1.223(6) . ?
C5 O3 1.289(6) . ?
C6 N3 1.347(6) . ?
C6 C7 1.391(7) . ?
C6 C9 1.489(7) . ?
C7 C8 1.384(7) . ?
C7 H7 0.9300 . ?
C8 N4 1.344(6) . ?
C8 C10 1.497(8) . ?
C9 O6 1.243(6) . ?
C9 O5 1.289(6) . ?
C10 O8 1.245(6) . ?
C10 O7 1.282(6) . ?
C11 N5 1.337(6) . ?
C11 C12 1.389(7) . ?
C11 C14 1.490(7) . ?
C12 C13 1.390(7) . ?
C12 H12 0.9300 . ?
C13 N6 1.345(6) . ?
C13 C15 1.504(8) . ?
C14 O10 1.224(6) . ?
C14 O9 1.309(6) . ?
C15 O12 1.227(7) . ?
C15 O11 1.290(7) . ?
C16 N7 1.343(6) . ?
C16 C17 1.398(7) . ?
C16 C19 1.491(7) . ?
C17 C18 1.390(7) . ?
C17 H17 0.9300 . ?
C18 N8 1.342(6) . ?
C18 C20 1.491(7) . ?
C19 O14 1.226(6) . ?
C19 O13 1.291(6) . ?
C20 O16 1.244(6) . ?
C20 O15 1.286(6) . ?
C21 N9 1.334(6) . ?
C21 C22 1.381(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.387(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.394(7) . ?
C23 C26 1.461(7) . ?
C24 C25 1.381(7) . ?
C24 H24 0.9300 . ?
C25 N9 1.332(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.321(7) . ?
C26 H26 0.9300 . ?
C27 C30 1.461(7) . ?
C27 H27 0.9300 . ?
C28 N10 1.328(7) . ?
C28 C29 1.380(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.393(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.390(7) . ?
C31 C32 1.384(7) . ?
C31 H31 0.9300 . ?
C32 N10 1.328(7) . ?
C32 H32 0.9300 . ?
C33 N11 1.334(6) . ?
C33 C34 1.382(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.393(8) . ?
C34 H34 0.9300 . ?
C35 C36 1.377(8) . ?
C35 C38 1.481(7) . ?
C36 C37 1.376(7) . ?
C36 H36 0.9300 . ?
C37 N11 1.331(7) . ?
C37 H37 0.9300 . ?
C38 C39 1.287(8) . ?
C38 H38 0.9300 . ?
C39 C42 1.477(7) . ?
C39 H39 0.9300 . ?
C40 N12 1.325(7) . ?
C40 C41 1.369(7) . ?
C40 H40 0.9300 . ?
C41 C42 1.399(8) . ?
C41 H41 0.9300 . ?
C42 C43 1.393(8) . ?
C43 C44 1.398(7) . ?
C43 H43 0.9300 . ?
C44 N12 1.334(6) . ?
C44 H44 0.9300 . ?
C45 N13 1.343(6) . ?
C45 C46 1.377(7) . ?
C45 H45 0.9300 . ?
C46 C47 1.375(7) . ?
C46 H46 0.9300 . ?
C47 C48 1.386(7) . ?
C47 C50 1.454(7) . ?
C48 C49 1.367(7) . ?
C48 H48 0.9300 . ?
C49 N13 1.341(6) . ?
C49 H49 0.9300 . ?
C50 C51 1.335(7) . ?
C50 H50 0.9300 . ?
C51 C54 1.469(7) . ?
C51 H51 0.9300 . ?
C52 N14 1.337(6) . ?
C52 C53 1.363(6) . ?
C52 H52 0.9300 . ?
C53 C54 1.403(7) . ?
C53 H53 0.9300 . ?
C54 C55 1.375(7) . ?
C55 C56 1.363(7) . ?
C55 H55 0.9300 . ?
C56 N14 1.345(6) . ?
C56 H56 0.9300 . ?
C57 N15 1.335(6) . ?
C57 C58 1.372(7) . ?
C57 H57 0.9300 . ?
C58 C59 1.386(7) . ?
C58 H58 0.9300 . ?
C59 C60 1.384(7) . ?
C59 C62 1.491(6) . ?
C60 C61 1.374(7) . ?
C60 H60 0.9300 . ?
C61 N15 1.348(7) . ?
C61 H61 0.9300 . ?
C62 C63 1.278(7) . ?
C62 H62 0.9300 . ?
C63 C66 1.487(7) . ?
C63 H63 0.9300 . ?
C64 N16 1.338(7) . ?
C64 C65 1.382(7) . ?
C64 H64 0.9300 . ?
C65 C66 1.380(7) . ?
C65 H65 0.9300 . ?
C66 C67 1.392(7) . ?
C67 C68 1.379(7) . ?
C67 H67 0.9300 . ?
C68 N16 1.339(6) . ?
C68 H68 0.9300 . ?
C69 N17 1.354(6) . ?
C69 C70 1.370(6) . ?
C69 H69 0.9300 . ?
C70 C71 1.389(7) . ?
C70 H70 0.9300 . ?
C71 C72 1.391(7) . ?
C71 C74 1.464(7) . ?
C72 C73 1.366(6) . ?
C72 H72 0.9300 . ?
C73 N17 1.344(6) . ?
C73 H73 0.9300 . ?
C74 C75 1.338(7) . ?
C74 H74 0.9300 . ?
C75 C78 1.467(7) . ?
C75 H75 0.9300 . ?
C76 N18 1.349(6) . ?
C76 C77 1.378(6) . ?
C76 H76 0.9300 . ?
C77 C78 1.379(7) . ?
C77 H77 0.9300 . ?
C78 C79 1.390(7) . ?
C79 C80 1.378(6) . ?
C79 H79 0.9300 . ?
C80 N18 1.344(6) . ?
C80 H80 0.9300 . ?
C81 N19 1.340(7) . ?
C81 C82 1.370(7) . ?
C81 H81 0.9300 . ?
C82 C83 1.377(7) . ?
C82 H82 0.9300 . ?
C83 C84 1.392(7) . ?
C83 C86 1.466(6) . ?
C84 C85 1.369(7) . ?
C84 H84 0.9300 . ?
C85 N19 1.340(6) . ?
C85 H85 0.9300 . ?
C86 C87 1.321(7) . ?
C86 H86 0.9300 . ?
C87 C90 1.456(6) . ?
C87 H87 0.9300 . ?
C88 N20 1.338(6) . ?
C88 C89 1.368(7) . ?
C88 H88 0.9300 . ?
C89 C90 1.382(7) . ?
C89 H89 0.9300 . ?
C90 C91 1.391(7) . ?
C91 C92 1.374(6) . ?
C91 H91 0.9300 . ?
C92 N20 1.334(6) . ?
C92 H92 0.9300 . ?
N1 N2 1.327(6) . ?
N1 Cu1 1.929(4) . ?
N2 Cu2 1.934(4) . ?
N3 N4 1.340(5) . ?
N3 Cu1 1.921(4) . ?
N4 Cu2 1.931(4) . ?
N5 N6 1.330(5) . ?
N5 Cu3 1.923(4) . ?
N6 Cu4 1.934(4) . ?
N7 N8 1.316(6) . ?
N7 Cu3 1.938(4) . ?
N8 Cu4 1.931(4) . ?
N9 Cu1 2.250(4) . ?
N10 Cu4 2.246(4) . ?
N11 Cu2 2.264(4) . ?
N12 Cu3 2.246(4) . ?
N13 Cu5 1.930(4) . ?
N14 Cu5 1.926(4) 4_565 ?
N15 Cu6 1.912(4) . ?
N16 Cu6 1.911(4) 4_666 ?
N17 Cu7 1.923(4) . ?
N18 Cu7 1.935(4) 4_565 ?
N19 Cu8 1.905(4) . ?
N20 Cu8 1.901(4) 4_676 ?
O1 Cu1 2.010(3) . ?
O2 Cu5 2.227(4) . ?
O3 Cu2 1.997(3) . ?
O5 Cu1 2.030(3) . ?
O6 Cu6 2.293(4) . ?
O7 Cu2 2.012(4) . ?
O9 Cu3 2.048(4) . ?
O9 Cu8 2.345(4) . ?
O11 Cu4 2.006(4) . ?
O13 Cu3 1.974(4) . ?
O15 Cu4 2.016(4) . ?
O16 Cu7 2.201(4) . ?
Cu5 N14 1.926(4) 4_666 ?
Cu6 N16 1.911(4) 4_565 ?
Cu7 N18 1.935(4) 4_666 ?
Cu8 N20 1.901(4) 4_575 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 108.9(5) . . ?
N1 C1 C4 111.5(5) . . ?
C2 C1 C4 139.5(5) . . ?
C1 C2 C3 104.6(5) . . ?
C1 C2 H2 127.7 . . ?
C3 C2 H2 127.7 . . ?
N2 C3 C2 108.3(5) . . ?
N2 C3 C5 112.3(5) . . ?
C2 C3 C5 139.2(5) . . ?
O2 C4 O1 124.2(5) . . ?
O2 C4 C1 121.0(5) . . ?
O1 C4 C1 114.8(5) . . ?
O4 C5 O3 124.7(5) . . ?
O4 C5 C3 121.1(5) . . ?
O3 C5 C3 114.1(5) . . ?
N3 C6 C7 109.0(5) . . ?
N3 C6 C9 111.6(5) . . ?
C7 C6 C9 139.1(5) . . ?
C8 C7 C6 104.7(5) . . ?
C8 C7 H7 127.7 . . ?
C6 C7 H7 127.7 . . ?
N4 C8 C7 109.2(5) . . ?
N4 C8 C10 111.8(5) . . ?
C7 C8 C10 138.7(5) . . ?
O6 C9 O5 123.8(5) . . ?
O6 C9 C6 120.9(5) . . ?
O5 C9 C6 115.3(5) . . ?
O8 C10 O7 124.8(6) . . ?
O8 C10 C8 120.6(6) . . ?
O7 C10 C8 114.6(5) . . ?
N5 C11 C12 109.0(5) . . ?
N5 C11 C14 114.4(5) . . ?
C12 C11 C14 136.3(5) . . ?
C11 C12 C13 104.5(5) . . ?
C11 C12 H12 127.8 . . ?
C13 C12 H12 127.8 . . ?
N6 C13 C12 108.9(5) . . ?
N6 C13 C15 112.0(5) . . ?
C12 C13 C15 138.7(5) . . ?
O10 C14 O9 124.8(5) . . ?
O10 C14 C11 122.8(5) . . ?
O9 C14 C11 112.5(5) . . ?
O12 C15 O11 125.7(6) . . ?
O12 C15 C13 120.2(6) . . ?
O11 C15 C13 114.1(5) . . ?
N7 C16 C17 108.1(5) . . ?
N7 C16 C19 112.9(5) . . ?
C17 C16 C19 138.7(5) . . ?
C18 C17 C16 104.0(5) . . ?
C18 C17 H17 128.0 . . ?
C16 C17 H17 128.0 . . ?
N8 C18 C17 109.5(5) . . ?
N8 C18 C20 111.7(5) . . ?
C17 C18 C20 138.5(5) . . ?
O14 C19 O13 124.4(5) . . ?
O14 C19 C16 122.0(5) . . ?
O13 C19 C16 113.6(5) . . ?
O16 C20 O15 124.3(5) . . ?
O16 C20 C18 121.1(5) . . ?
O15 C20 C18 114.6(5) . . ?
N9 C21 C22 123.5(5) . . ?
N9 C21 H21 118.3 . . ?
C22 C21 H21 118.3 . . ?
C21 C22 C23 120.0(5) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C24 116.4(5) . . ?
C22 C23 C26 123.4(5) . . ?
C24 C23 C26 120.2(5) . . ?
C25 C24 C23 119.7(5) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
N9 C25 C24 123.6(5) . . ?
N9 C25 H25 118.2 . . ?
C24 C25 H25 118.2 . . ?
C27 C26 C23 126.9(5) . . ?
C27 C26 H26 116.5 . . ?
C23 C26 H26 116.5 . . ?
C26 C27 C30 126.1(5) . . ?
C26 C27 H27 117.0 . . ?
C30 C27 H27 117.0 . . ?
N10 C28 C29 124.3(5) . . ?
N10 C28 H28 117.8 . . ?
C29 C28 H28 117.8 . . ?
C28 C29 C30 119.2(5) . . ?
C28 C29 H29 120.4 . . ?
C30 C29 H29 120.4 . . ?
C31 C30 C29 116.8(5) . . ?
C31 C30 C27 123.3(5) . . ?
C29 C30 C27 119.9(5) . . ?
C32 C31 C30 119.2(5) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 H31 120.4 . . ?
N10 C32 C31 124.2(5) . . ?
N10 C32 H32 117.9 . . ?
C31 C32 H32 117.9 . . ?
N11 C33 C34 123.6(5) . . ?
N11 C33 H33 118.2 . . ?
C34 C33 H33 118.2 . . ?
C33 C34 C35 119.4(5) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C36 C35 C34 116.5(5) . . ?
C36 C35 C38 119.1(5) . . ?
C34 C35 C38 124.3(5) . . ?
C37 C36 C35 120.5(5) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
N11 C37 C36 123.3(5) . . ?
N11 C37 H37 118.4 . . ?
C36 C37 H37 118.4 . . ?
C39 C38 C35 125.9(6) . . ?
C39 C38 H38 117.0 . . ?
C35 C38 H38 117.0 . . ?
C38 C39 C42 125.1(6) . . ?
C38 C39 H39 117.4 . . ?
C42 C39 H39 117.4 . . ?
N12 C40 C41 125.2(5) . . ?
N12 C40 H40 117.4 . . ?
C41 C40 H40 117.4 . . ?
C40 C41 C42 119.0(6) . . ?
C40 C41 H41 120.5 . . ?
C42 C41 H41 120.5 . . ?
C43 C42 C41 116.7(5) . . ?
C43 C42 C39 123.7(5) . . ?
C41 C42 C39 119.5(6) . . ?
C42 C43 C44 119.4(5) . . ?
C42 C43 H43 120.3 . . ?
C44 C43 H43 120.3 . . ?
N12 C44 C43 123.2(5) . . ?
N12 C44 H44 118.4 . . ?
C43 C44 H44 118.4 . . ?
N13 C45 C46 123.4(5) . . ?
N13 C45 H45 118.3 . . ?
C46 C45 H45 118.3 . . ?
C47 C46 C45 120.7(5) . . ?
C47 C46 H46 119.7 . . ?
C45 C46 H46 119.7 . . ?
C46 C47 C48 115.8(5) . . ?
C46 C47 C50 123.9(5) . . ?
C48 C47 C50 120.3(5) . . ?
C49 C48 C47 120.8(5) . . ?
C49 C48 H48 119.6 . . ?
C47 C48 H48 119.6 . . ?
N13 C49 C48 123.5(5) . . ?
N13 C49 H49 118.3 . . ?
C48 C49 H49 118.3 . . ?
C51 C50 C47 126.9(5) . . ?
C51 C50 H50 116.6 . . ?
C47 C50 H50 116.6 . . ?
C50 C51 C54 125.5(5) . . ?
C50 C51 H51 117.2 . . ?
C54 C51 H51 117.2 . . ?
N14 C52 C53 123.6(5) . . ?
N14 C52 H52 118.2 . . ?
C53 C52 H52 118.2 . . ?
C52 C53 C54 120.2(5) . . ?
C52 C53 H53 119.9 . . ?
C54 C53 H53 119.9 . . ?
C55 C54 C53 115.7(4) . . ?
C55 C54 C51 123.9(5) . . ?
C53 C54 C51 120.4(5) . . ?
C56 C55 C54 120.9(5) . . ?
C56 C55 H55 119.6 . . ?
C54 C55 H55 119.6 . . ?
N14 C56 C55 123.4(5) . . ?
N14 C56 H56 118.3 . . ?
C55 C56 H56 118.3 . . ?
N15 C57 C58 123.4(5) . . ?
N15 C57 H57 118.3 . . ?
C58 C57 H57 118.3 . . ?
C57 C58 C59 120.2(5) . . ?
C57 C58 H58 119.9 . . ?
C59 C58 H58 119.9 . . ?
C60 C59 C58 116.3(5) . . ?
C60 C59 C62 119.8(5) . . ?
C58 C59 C62 123.9(5) . . ?
C61 C60 C59 120.7(5) . . ?
C61 C60 H60 119.7 . . ?
C59 C60 H60 119.7 . . ?
N15 C61 C60 122.5(5) . . ?
N15 C61 H61 118.8 . . ?
C60 C61 H61 118.8 . . ?
C63 C62 C59 124.9(5) . . ?
C63 C62 H62 117.5 . . ?
C59 C62 H62 117.5 . . ?
C62 C63 C66 124.4(5) . . ?
C62 C63 H63 117.8 . . ?
C66 C63 H63 117.8 . . ?
N16 C64 C65 122.8(5) . . ?
N16 C64 H64 118.6 . . ?
C65 C64 H64 118.6 . . ?
C66 C65 C64 119.7(5) . . ?
C66 C65 H65 120.1 . . ?
C64 C65 H65 120.1 . . ?
C65 C66 C67 117.4(5) . . ?
C65 C66 C63 118.6(5) . . ?
C67 C66 C63 124.0(5) . . ?
C68 C67 C66 119.7(5) . . ?
C68 C67 H67 120.2 . . ?
C66 C67 H67 120.2 . . ?
N16 C68 C67 122.7(5) . . ?
N16 C68 H68 118.7 . . ?
C67 C68 H68 118.7 . . ?
N17 C69 C70 123.4(5) . . ?
N17 C69 H69 118.3 . . ?
C70 C69 H69 118.3 . . ?
C69 C70 C71 120.3(5) . . ?
C69 C70 H70 119.9 . . ?
C71 C70 H70 119.9 . . ?
C70 C71 C72 116.3(4) . . ?
C70 C71 C74 123.3(5) . . ?
C72 C71 C74 120.5(5) . . ?
C73 C72 C71 120.1(5) . . ?
C73 C72 H72 119.9 . . ?
C71 C72 H72 119.9 . . ?
N17 C73 C72 124.0(5) . . ?
N17 C73 H73 118.0 . . ?
C72 C73 H73 118.0 . . ?
C75 C74 C71 124.9(5) . . ?
C75 C74 H74 117.6 . . ?
C71 C74 H74 117.6 . . ?
C74 C75 C78 126.6(5) . . ?
C74 C75 H75 116.7 . . ?
C78 C75 H75 116.7 . . ?
N18 C76 C77 122.6(5) . . ?
N18 C76 H76 118.7 . . ?
C77 C76 H76 118.7 . . ?
C76 C77 C78 120.9(5) . . ?
C76 C77 H77 119.5 . . ?
C78 C77 H77 119.5 . . ?
C77 C78 C79 116.4(5) . . ?
C77 C78 C75 120.0(5) . . ?
C79 C78 C75 123.6(5) . . ?
C80 C79 C78 119.9(5) . . ?
C80 C79 H79 120.0 . . ?
C78 C79 H79 120.0 . . ?
N18 C80 C79 123.5(5) . . ?
N18 C80 H80 118.2 . . ?
C79 C80 H80 118.2 . . ?
N19 C81 C82 123.0(5) . . ?
N19 C81 H81 118.5 . . ?
C82 C81 H81 118.5 . . ?
C81 C82 C83 120.5(5) . . ?
C81 C82 H82 119.8 . . ?
C83 C82 H82 119.8 . . ?
C82 C83 C84 116.4(5) . . ?
C82 C83 C86 120.3(5) . . ?
C84 C83 C86 123.2(5) . . ?
C85 C84 C83 120.2(5) . . ?
C85 C84 H84 119.9 . . ?
C83 C84 H84 119.9 . . ?
N19 C85 C84 122.8(5) . . ?
N19 C85 H85 118.6 . . ?
C84 C85 H85 118.6 . . ?
C87 C86 C83 125.4(5) . . ?
C87 C86 H86 117.3 . . ?
C83 C86 H86 117.3 . . ?
C86 C87 C90 126.1(5) . . ?
C86 C87 H87 116.9 . . ?
C90 C87 H87 116.9 . . ?
N20 C88 C89 124.3(5) . . ?
N20 C88 H88 117.9 . . ?
C89 C88 H88 117.9 . . ?
C88 C89 C90 119.5(5) . . ?
C88 C89 H89 120.3 . . ?
C90 C89 H89 120.3 . . ?
C89 C90 C91 116.6(4) . . ?
C89 C90 C87 123.8(5) . . ?
C91 C90 C87 119.6(5) . . ?
C92 C91 C90 120.2(5) . . ?
C92 C91 H91 119.9 . . ?
C90 C91 H91 119.9 . . ?
N20 C92 C91 123.0(5) . . ?
N20 C92 H92 118.5 . . ?
C91 C92 H92 118.5 . . ?
N2 N1 C1 108.6(4) . . ?
N2 N1 Cu1 133.1(3) . . ?
C1 N1 Cu1 118.0(3) . . ?
N1 N2 C3 109.6(4) . . ?
N1 N2 Cu2 132.6(3) . . ?
C3 N2 Cu2 117.2(3) . . ?
N4 N3 C6 108.4(4) . . ?
N4 N3 Cu1 132.4(3) . . ?
C6 N3 Cu1 118.3(4) . . ?
N3 N4 C8 108.7(4) . . ?
N3 N4 Cu2 133.1(3) . . ?
C8 N4 Cu2 117.9(4) . . ?
N6 N5 C11 109.1(4) . . ?
N6 N5 Cu3 132.4(4) . . ?
C11 N5 Cu3 117.7(4) . . ?
N5 N6 C13 108.6(4) . . ?
N5 N6 Cu4 133.1(4) . . ?
C13 N6 Cu4 117.5(4) . . ?
N8 N7 C16 110.0(4) . . ?
N8 N7 Cu3 133.2(4) . . ?
C16 N7 Cu3 116.1(4) . . ?
N7 N8 C18 108.3(4) . . ?
N7 N8 Cu4 132.7(4) . . ?
C18 N8 Cu4 118.1(4) . . ?
C25 N9 C21 116.8(5) . . ?
C25 N9 Cu1 120.9(4) . . ?
C21 N9 Cu1 122.0(3) . . ?
C28 N10 C32 116.3(5) . . ?
C28 N10 Cu4 123.1(4) . . ?
C32 N10 Cu4 120.4(4) . . ?
C37 N11 C33 116.7(5) . . ?
C37 N11 Cu2 121.3(4) . . ?
C33 N11 Cu2 121.7(4) . . ?
C40 N12 C44 116.4(5) . . ?
C40 N12 Cu3 121.6(4) . . ?
C44 N12 Cu3 121.2(4) . . ?
C49 N13 C45 115.8(4) . . ?
C49 N13 Cu5 122.9(3) . . ?
C45 N13 Cu5 121.2(4) . . ?
C52 N14 C56 116.1(4) . . ?
C52 N14 Cu5 120.7(3) . 4_565 ?
C56 N14 Cu5 123.1(4) . 4_565 ?
C57 N15 C61 116.9(4) . . ?
C57 N15 Cu6 120.7(4) . . ?
C61 N15 Cu6 122.4(3) . . ?
C64 N16 C68 117.7(5) . . ?
C64 N16 Cu6 120.0(4) . 4_666 ?
C68 N16 Cu6 122.3(4) . 4_666 ?
C73 N17 C69 115.7(4) . . ?
C73 N17 Cu7 122.2(3) . . ?
C69 N17 Cu7 121.7(4) . . ?
C80 N18 C76 116.5(4) . . ?
C80 N18 Cu7 121.4(4) . 4_565 ?
C76 N18 Cu7 122.1(3) . 4_565 ?
C81 N19 C85 117.0(4) . . ?
C81 N19 Cu8 119.7(3) . . ?
C85 N19 Cu8 123.3(4) . . ?
C92 N20 C88 116.4(4) . . ?
C92 N20 Cu8 121.8(3) . 4_676 ?
C88 N20 Cu8 121.7(4) . 4_676 ?
C4 O1 Cu1 116.1(3) . . ?
C4 O2 Cu5 115.3(4) . . ?
C5 O3 Cu2 116.2(3) . . ?
C9 O5 Cu1 114.8(3) . . ?
C9 O6 Cu6 125.1(4) . . ?
C10 O7 Cu2 116.0(4) . . ?
C14 O9 Cu3 115.7(3) . . ?
C14 O9 Cu8 121.6(3) . . ?
Cu3 O9 Cu8 122.50(17) . . ?
C15 O11 Cu4 116.0(4) . . ?
C19 O13 Cu3 116.5(3) . . ?
C20 O15 Cu4 115.8(3) . . ?
C20 O16 Cu7 120.1(4) . . ?
N3 Cu1 N1 93.62(18) . . ?
N3 Cu1 O1 160.93(16) . . ?
N1 Cu1 O1 79.56(16) . . ?
N3 Cu1 O5 79.87(16) . . ?
N1 Cu1 O5 162.55(16) . . ?
O1 Cu1 O5 101.38(15) . . ?
N3 Cu1 N9 97.46(16) . . ?
N1 Cu1 N9 96.56(17) . . ?
O1 Cu1 N9 100.99(15) . . ?
O5 Cu1 N9 100.32(15) . . ?
N4 Cu2 N2 93.22(18) . . ?
N4 Cu2 O3 163.56(16) . . ?
N2 Cu2 O3 80.03(16) . . ?
N4 Cu2 O7 79.80(17) . . ?
N2 Cu2 O7 160.62(16) . . ?
O3 Cu2 O7 101.69(15) . . ?
N4 Cu2 N11 97.09(17) . . ?
N2 Cu2 N11 95.72(17) . . ?
O3 Cu2 N11 98.48(15) . . ?
O7 Cu2 N11 103.04(16) . . ?
N5 Cu3 N7 93.37(19) . . ?
N5 Cu3 O13 161.58(16) . . ?
N7 Cu3 O13 80.59(17) . . ?
N5 Cu3 O9 79.57(17) . . ?
N7 Cu3 O9 159.98(15) . . ?
O13 Cu3 O9 100.23(15) . . ?
N5 Cu3 N12 96.49(17) . . ?
N7 Cu3 N12 96.80(17) . . ?
O13 Cu3 N12 101.48(16) . . ?
O9 Cu3 N12 102.57(15) . . ?
N8 Cu4 N6 93.29(19) . . ?
N8 Cu4 O11 161.98(16) . . ?
N6 Cu4 O11 80.08(17) . . ?
N8 Cu4 O15 79.55(16) . . ?
N6 Cu4 O15 160.97(16) . . ?
O11 Cu4 O15 101.36(15) . . ?
N8 Cu4 N10 97.52(17) . . ?
N6 Cu4 N10 98.42(17) . . ?
O11 Cu4 N10 100.01(16) . . ?
O15 Cu4 N10 99.98(15) . . ?
N14 Cu5 N13 150.46(19) 4_666 . ?
N14 Cu5 O2 106.54(16) 4_666 . ?
N13 Cu5 O2 102.73(17) . . ?
N16 Cu6 N15 155.1(2) 4_565 . ?
N16 Cu6 O6 104.70(17) 4_565 . ?
N15 Cu6 O6 99.57(17) . . ?
N17 Cu7 N18 150.51(19) . 4_666 ?
N17 Cu7 O16 106.83(16) . . ?
N18 Cu7 O16 102.36(16) 4_666 . ?
N20 Cu8 N19 156.7(2) 4_575 . ?
N20 Cu8 O9 99.66(16) 4_575 . ?
N19 Cu8 O9 103.40(16) . . ?

_refine_diff_density_max         1.513
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.112



####################################################################### 
# 
# 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_compound4
_database_code_depnum_ccdc_archive 'CCDC 1522625'
_audit_update_record             
;
2016-12-14 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            
'Poly{bis(mu-1,2-di(4-pyridyl)ethylene)-mu5-pyrazole-3,5-dicarboxylato)dicopper(II) thiocyanate}'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H21 Cu2 N7 O4 S'
_chemical_formula_weight         702.68

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'
S S 0.1246 0.1234 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.7346(9)
_cell_length_b                   26.731(2)
_cell_length_c                   8.4383(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2872.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3102
_cell_measurement_theta_min      2.896
_cell_measurement_theta_max      23.506

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_F_000             1424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.604
_shelx_estimated_absorpt_T_min   0.882
_shelx_estimated_absorpt_T_max   0.953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6458
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  
;
Bruker D8 QUEST PHOTON 100
;
_diffrn_measurement_method       '\fandω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43633
_diffrn_reflns_av_unetI/netI     0.0905
_diffrn_reflns_av_R_equivalents  0.1777
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.896
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2886
_reflns_number_gt                1755
_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       BrukerAPEX2
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0890P)²+12.7369P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2886
_refine_ls_number_parameters     215
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.0687
_refine_ls_wR_factor_ref         0.1944
_refine_ls_wR_factor_gt          0.1630
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.82138(9) 0.2500 0.47040(14) 0.0208(4) Uani 1 2 d S T P . .
Cu2 Cu 1.12427(9) 0.2500 1.60795(14) 0.0166(3) Uani 1 2 d S T P . .
O1 O 0.9316(5) 0.2500 0.6323(7) 0.0217(15) Uani 1 2 d S T P . .
O2 O 0.8119(5) 0.2500 0.8267(9) 0.0348(19) Uani 1 2 d S T P . .
O3 O 1.0954(5) 0.2500 1.3769(7) 0.0204(15) Uani 1 2 d S T P . .
O4 O 1.2508(5) 0.2500 1.2510(8) 0.0203(15) Uani 1 2 d S T P . .
N1 N 0.8371(5) 0.3243(2) 0.4500(7) 0.0252(14) Uani 1 1 d . . . . .
N2 N 0.8617(5) 0.67492(19) 0.4022(7) 0.0229(13) Uani 1 1 d . . . . .
N3 N 1.0922(6) 0.2500 0.8404(9) 0.0154(18) Uani 1 2 d S T P . .
N4 N 1.1568(6) 0.2500 0.9662(9) 0.0176(17) Uani 1 2 d S T P . .
C1 C 0.7764(8) 0.3563(3) 0.5264(12) 0.059(3) Uani 1 1 d . . . . .
H1 H 0.7242 0.3440 0.5928 0.071 Uiso 1 1 calc R U . . .
C2 C 0.7878(9) 0.4074(3) 0.5112(13) 0.068(3) Uani 1 1 d . . . . .
H2 H 0.7437 0.4284 0.5683 0.081 Uiso 1 1 calc R U . . .
C3 C 0.8626(7) 0.4278(3) 0.4138(10) 0.040(2) Uani 1 1 d . . . . .
C4 C 0.9253(7) 0.3941(3) 0.3349(10) 0.041(2) Uani 1 1 d . . . . .
H4 H 0.9774 0.4053 0.2664 0.049 Uiso 1 1 calc R U . . .
C5 C 0.9106(6) 0.3441(3) 0.3578(10) 0.039(2) Uani 1 1 d . . . . .
H5 H 0.9553 0.3222 0.3049 0.047 Uiso 1 1 calc R U . . .
C6 C 0.8787(7) 0.4822(3) 0.3907(10) 0.043(2) Uani 1 1 d . . . . .
H6 H 0.9325 0.4922 0.3232 0.051 Uiso 1 1 calc R U . . .
C7 C 0.8236(8) 0.5166(3) 0.4573(12) 0.057(3) Uani 1 1 d . . . . .
H7 H 0.7701 0.5066 0.5252 0.069 Uiso 1 1 calc R U . . .
C8 C 0.7854(7) 0.6554(3) 0.4921(10) 0.040(2) Uani 1 1 d . . . . .
H8 H 0.7399 0.6768 0.5452 0.048 Uiso 1 1 calc R U . . .
C9 C 0.7722(8) 0.6046(3) 0.5086(12) 0.060(3) Uani 1 1 d . . . . .
H9 H 0.7175 0.5925 0.5708 0.071 Uiso 1 1 calc R U . . .
C10 C 0.8391(7) 0.5711(3) 0.4337(11) 0.044(2) Uani 1 1 d . . . . .
C11 C 0.9162(7) 0.5917(3) 0.3392(10) 0.038(2) Uani 1 1 d . . . . .
H11 H 0.9620 0.5711 0.2837 0.045 Uiso 1 1 calc R U . . .
C12 C 0.9251(6) 0.6428(3) 0.3272(9) 0.0285(18) Uani 1 1 d . . . . .
H12 H 0.9781 0.6558 0.2634 0.034 Uiso 1 1 calc R U . . .
C13 C 0.9922(7) 0.2500 0.8919(11) 0.0147(19) Uani 1 2 d S T P . .
C14 C 0.9901(7) 0.2500 1.0580(11) 0.017(2) Uani 1 2 d S T P . .
H14 H 0.9320 0.2500 1.1247 0.021 Uiso 1 2 calc R U P . .
C15 C 1.0967(7) 0.2500 1.0998(11) 0.017(2) Uani 1 2 d S T P . .
C16 C 0.9031(7) 0.2500 0.7785(11) 0.017(2) Uani 1 2 d S T P . .
C17 C 1.1510(7) 0.2500 1.2520(12) 0.017(2) Uani 1 2 d S T P . .
S1 S 1.0401(13) 0.4815(6) 0.039(2) 0.220(6) Uiso 0.5 1 d D . P A -1
N5 N 0.872(2) 0.4968(14) -0.169(4) 0.220(6) Uiso 0.5 1 d D . P A -1
C18 C 0.934(3) 0.4824(18) -0.066(5) 0.220(6) Uiso 0.5 1 d D . P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.959(6) . ?
Cu1 N1 2.002(5) 7_565 ?
Cu1 N1 2.002(5) . ?
Cu1 O4 2.073(7) 6_557 ?
Cu1 N4 2.163(8) 6_557 ?
Cu2 O3 1.984(6) . ?
Cu2 N3 2.003(7) 1_556 ?
Cu2 N2 2.017(5) 5_767 ?
Cu2 N2 2.017(5) 3_747 ?
O1 C16 1.286(11) . ?
O2 C16 1.230(11) . ?
O3 C17 1.269(11) . ?
O4 C17 1.272(10) . ?
O4 Cu1 2.073(7) 6_657 ?
N1 C1 1.322(10) . ?
N1 C5 1.327(10) . ?
N2 C12 1.338(9) . ?
N2 C8 1.339(9) . ?
N2 Cu2 2.017(5) 5_767 ?
N3 N4 1.343(10) . ?
N3 C13 1.345(11) . ?
N3 Cu2 2.003(7) 1_554 ?
N4 C15 1.363(12) . ?
N4 Cu1 2.163(8) 6_657 ?
C1 C2 1.379(12) . ?
C1 H1 0.9300 . ?
C2 C3 1.372(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.376(11) . ?
C3 C6 1.482(11) . ?
C4 C5 1.363(10) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.286(12) . ?
C6 H6 0.9300 . ?
C7 C10 1.483(11) . ?
C7 H7 0.9300 . ?
C8 C9 1.374(11) . ?
C8 H8 0.9300 . ?
C9 C10 1.389(12) . ?
C9 H9 0.9300 . ?
C10 C11 1.380(12) . ?
C11 C12 1.374(10) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.402(12) . ?
C13 C16 1.485(13) . ?
C14 C15 1.402(13) . ?
C14 H14 0.9300 . ?
C15 C17 1.459(13) . ?
S1 C18 1.617(10) . ?
N5 C18 1.240(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N1 89.32(17) . 7_565 ?
O1 Cu1 N1 89.32(17) . . ?
N1 Cu1 N1 164.8(4) 7_565 . ?
O1 Cu1 O4 159.9(3) . 6_557 ?
N1 Cu1 O4 88.05(17) 7_565 6_557 ?
N1 Cu1 O4 88.05(17) . 6_557 ?
O1 Cu1 N4 121.4(3) . 6_557 ?
N1 Cu1 N4 96.80(18) 7_565 6_557 ?
N1 Cu1 N4 96.80(18) . 6_557 ?
O4 Cu1 N4 78.6(3) 6_557 6_557 ?
O3 Cu2 N3 157.6(3) . 1_556 ?
O3 Cu2 N2 88.55(16) . 5_767 ?
N3 Cu2 N2 93.42(16) 1_556 5_767 ?
O3 Cu2 N2 88.55(16) . 3_747 ?
N3 Cu2 N2 93.42(16) 1_556 3_747 ?
N2 Cu2 N2 168.7(3) 5_767 3_747 ?
C16 O1 Cu1 117.8(6) . . ?
C17 O3 Cu2 135.4(6) . . ?
C17 O4 Cu1 116.1(6) . 6_657 ?
C1 N1 C5 116.1(6) . . ?
C1 N1 Cu1 122.8(5) . . ?
C5 N1 Cu1 121.1(5) . . ?
C12 N2 C8 117.1(6) . . ?
C12 N2 Cu2 124.4(5) . 5_767 ?
C8 N2 Cu2 118.5(5) . 5_767 ?
N4 N3 C13 108.9(7) . . ?
N4 N3 Cu2 130.5(6) . 1_554 ?
C13 N3 Cu2 120.6(6) . 1_554 ?
N3 N4 C15 108.0(8) . . ?
N3 N4 Cu1 142.1(6) . 6_657 ?
C15 N4 Cu1 109.9(6) . 6_657 ?
N1 C1 C2 122.3(8) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C3 C2 C1 121.6(8) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C2 C3 C4 115.5(7) . . ?
C2 C3 C6 124.5(8) . . ?
C4 C3 C6 120.0(8) . . ?
C5 C4 C3 119.7(8) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
N1 C5 C4 124.8(8) . . ?
N1 C5 H5 117.6 . . ?
C4 C5 H5 117.6 . . ?
C7 C6 C3 124.6(9) . . ?
C7 C6 H6 117.7 . . ?
C3 C6 H6 117.7 . . ?
C6 C7 C10 124.7(9) . . ?
C6 C7 H7 117.6 . . ?
C10 C7 H7 117.6 . . ?
N2 C8 C9 122.1(8) . . ?
N2 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C8 C9 C10 121.1(8) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 116.2(7) . . ?
C11 C10 C7 124.4(8) . . ?
C9 C10 C7 119.4(8) . . ?
C12 C11 C10 119.9(7) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
N2 C12 C11 123.6(7) . . ?
N2 C12 H12 118.2 . . ?
C11 C12 H12 118.2 . . ?
N3 C13 C14 110.0(8) . . ?
N3 C13 C16 121.0(8) . . ?
C14 C13 C16 129.0(8) . . ?
C15 C14 C13 103.5(8) . . ?
C15 C14 H14 128.3 . . ?
C13 C14 H14 128.3 . . ?
N4 C15 C14 109.6(8) . . ?
N4 C15 C17 117.5(8) . . ?
C14 C15 C17 132.8(9) . . ?
O2 C16 O1 125.7(9) . . ?
O2 C16 C13 120.6(8) . . ?
O1 C16 C13 113.7(8) . . ?
O3 C17 O4 124.3(9) . . ?
O3 C17 C15 117.8(8) . . ?
O4 C17 C15 117.9(9) . . ?
N5 C18 S1 157(3) . . ?

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
C13 N3 N4 C15 0.000(2) . . . . ?
Cu2 N3 N4 C15 180.000(2) 1_554 . . . ?
C13 N3 N4 Cu1 180.000(2) . . . 6_657 ?
Cu2 N3 N4 Cu1 0.000(3) 1_554 . . 6_657 ?
C5 N1 C1 C2 0.3(15) . . . . ?
Cu1 N1 C1 C2 -179.8(8) . . . . ?
N1 C1 C2 C3 0.7(18) . . . . ?
C1 C2 C3 C4 -0.6(16) . . . . ?
C1 C2 C3 C6 179.5(10) . . . . ?
C2 C3 C4 C5 -0.4(13) . . . . ?
C6 C3 C4 C5 179.5(8) . . . . ?
C1 N1 C5 C4 -1.5(13) . . . . ?
Cu1 N1 C5 C4 178.7(6) . . . . ?
C3 C4 C5 N1 1.6(13) . . . . ?
C2 C3 C6 C7 -1.0(16) . . . . ?
C4 C3 C6 C7 179.1(10) . . . . ?
C3 C6 C7 C10 -179.6(8) . . . . ?
C12 N2 C8 C9 0.4(12) . . . . ?
Cu2 N2 C8 C9 -178.4(7) 5_767 . . . ?
N2 C8 C9 C10 1.0(15) . . . . ?
C8 C9 C10 C11 -2.1(15) . . . . ?
C8 C9 C10 C7 178.7(9) . . . . ?
C6 C7 C10 C11 -1.2(17) . . . . ?
C6 C7 C10 C9 178.0(11) . . . . ?
C9 C10 C11 C12 1.8(13) . . . . ?
C7 C10 C11 C12 -179.0(8) . . . . ?
C8 N2 C12 C11 -0.6(11) . . . . ?
Cu2 N2 C12 C11 178.0(6) 5_767 . . . ?
C10 C11 C12 N2 -0.5(13) . . . . ?
N4 N3 C13 C14 0.000(2) . . . . ?
Cu2 N3 C13 C14 180.000(2) 1_554 . . . ?
N4 N3 C13 C16 180.000(2) . . . . ?
Cu2 N3 C13 C16 0.000(2) 1_554 . . . ?
N3 C13 C14 C15 0.000(3) . . . . ?
C16 C13 C14 C15 180.000(2) . . . . ?
N3 N4 C15 C14 0.000(2) . . . . ?
Cu1 N4 C15 C14 180.000(2) 6_657 . . . ?
N3 N4 C15 C17 180.000(2) . . . . ?
Cu1 N4 C15 C17 0.000(3) 6_657 . . . ?
C13 C14 C15 N4 0.000(2) . . . . ?
C13 C14 C15 C17 180.000(3) . . . . ?
Cu1 O1 C16 O2 0.000(2) . . . . ?
Cu1 O1 C16 C13 180.000(1) . . . . ?
N3 C13 C16 O2 180.000(2) . . . . ?
C14 C13 C16 O2 0.000(3) . . . . ?
N3 C13 C16 O1 0.000(2) . . . . ?
C14 C13 C16 O1 180.000(2) . . . . ?
Cu2 O3 C17 O4 0.000(5) . . . . ?
Cu2 O3 C17 C15 180.000(3) . . . . ?
Cu1 O4 C17 O3 180.000(2) 6_657 . . . ?
Cu1 O4 C17 C15 0.000(3) 6_657 . . . ?
N4 C15 C17 O3 180.000(2) . . . . ?
C14 C15 C17 O3 0.000(4) . . . . ?
N4 C15 C17 O4 0.000(3) . . . . ?
C14 C15 C17 O4 180.000(3) . . . . ?

_refine_diff_density_max         1.578
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.162

####################################################################### 
# 
# 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_compound1
_database_code_depnum_ccdc_archive 'CCDC 1522622'
_audit_update_record             
;
2016-12-14 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            
'Poly{bis(mu-1,2-di(4-pyridyl)ethylene)-mu5-pyrazole-3,5-dicarboxylato)dicopper(II) nitrate}'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H21 Cu2 N7 O7'
_chemical_formula_weight         706.61

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.4115(7)
_cell_length_b                   26.8057(16)
_cell_length_c                   8.4121(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2798.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4859
_cell_measurement_theta_min      2.9255
_cell_measurement_theta_max      27.708


_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_F_000             1432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    1.582
_shelx_estimated_absorpt_T_min   0.871
_shelx_estimated_absorpt_T_max   0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6929
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  
;
Bruker D8 QUEST PHOTON 100
;
_diffrn_measurement_method       '\fandω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26502
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.925
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3145
_reflns_number_gt                2409
_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       BrukerAPEX2
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+12.2555P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3145
_refine_ls_number_parameters     242
_refine_ls_number_restraints     221
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0511
_refine_ls_wR_factor_ref         0.1004
_refine_ls_wR_factor_gt          0.0926
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.34135(5) 0.2500 0.54113(8) 0.00627(17) Uani 1 2 d S T P . .
Cu2 Cu 0.63919(5) 0.2500 0.38829(8) 0.00624(16) Uani 1 2 d S T P . .
O1 O 0.4444(3) 0.2500 0.3663(4) 0.0104(8) Uani 1 2 d S TU P . .
O2 O 0.3202(3) 0.2500 0.1731(5) 0.0184(9) Uani 1 2 d S TU P . .
O3 O 0.7678(3) 0.2500 -0.2584(4) 0.0062(7) Uani 1 2 d S TU P . .
O4 O 0.6062(3) 0.2500 -0.3802(4) 0.0089(8) Uani 1 2 d S TU P . .
N1 N 0.3568(2) 0.32467(12) 0.5633(4) 0.0120(7) Uani 1 1 d . U . . .
N2 N 0.3489(2) 0.67470(12) 0.6047(4) 0.0104(7) Uani 1 1 d . U . . .
N3 N 0.6081(3) 0.2500 0.1573(5) 0.0078(9) Uani 1 2 d S TU P . .
N4 N 0.6733(3) 0.2500 0.0314(5) 0.0065(8) Uani 1 2 d S TU P . .
C1 C 0.4339(3) 0.34511(15) 0.6522(5) 0.0134(8) Uani 1 1 d . U . . .
H1 H 0.4847 0.3237 0.7022 0.016 Uiso 1 1 calc R U . . .
C2 C 0.4435(3) 0.39586(14) 0.6749(5) 0.0135(8) Uani 1 1 d . U . . .
H2 H 0.5000 0.4087 0.7392 0.016 Uiso 1 1 calc R U . . .
C3 C 0.3707(4) 0.42830(15) 0.6041(5) 0.0182(9) Uani 1 1 d . U . . .
C4 C 0.2901(4) 0.40684(16) 0.5112(6) 0.0362(13) Uani 1 1 d . U . . .
H4 H 0.2382 0.4273 0.4600 0.043 Uiso 1 1 calc R U . . .
C5 C 0.2862(4) 0.35575(16) 0.4941(6) 0.0305(11) Uani 1 1 d . U . . .
H5 H 0.2308 0.3418 0.4300 0.037 Uiso 1 1 calc R U . . .
C6 C 0.3827(3) 0.48240(15) 0.6251(5) 0.0187(9) Uani 1 1 d . U . . .
H6 H 0.4447 0.4939 0.6801 0.022 Uiso 1 1 calc R U . . .
C7 C 0.3138(4) 0.51642(16) 0.5735(6) 0.0295(11) Uani 1 1 d . U . . .
H7 H 0.2509 0.5047 0.5213 0.035 Uiso 1 1 calc R U . . .
C8 C 0.4176(3) 0.64405(14) 0.6794(5) 0.0116(8) Uani 1 1 d . U . . .
H8 H 0.4748 0.6584 0.7387 0.014 Uiso 1 1 calc R U . . .
C9 C 0.4098(3) 0.59299(15) 0.6748(5) 0.0144(8) Uani 1 1 d . U . . .
H9 H 0.4610 0.5730 0.7292 0.017 Uiso 1 1 calc R U . . .
C10 C 0.3260(4) 0.57071(15) 0.5897(5) 0.0213(9) Uani 1 1 d . U . . .
C11 C 0.2534(4) 0.60272(16) 0.5144(6) 0.0277(11) Uani 1 1 d . U . . .
H11 H 0.1943 0.5894 0.4565 0.033 Uiso 1 1 calc R U . . .
C12 C 0.2674(3) 0.65387(15) 0.5238(5) 0.0203(9) Uani 1 1 d . U . . .
H12 H 0.2175 0.6750 0.4710 0.024 Uiso 1 1 calc R U . . .
C13 C 0.5032(4) 0.2500 0.1030(7) 0.0065(10) Uani 1 2 d S TU P . .
C14 C 0.5018(4) 0.2500 -0.0615(6) 0.0080(11) Uani 1 2 d S TU P . .
H14 H 0.4411 0.2500 -0.1302 0.010 Uiso 1 2 calc R U P . .
C15 C 0.6096(4) 0.2500 -0.1021(7) 0.0077(10) Uani 1 2 d S TU P . .
C16 C 0.4152(4) 0.2500 0.2199(6) 0.0085(11) Uani 1 2 d S TU P . .
C17 C 0.6657(4) 0.2500 -0.2554(7) 0.0080(10) Uani 1 2 d S TU P . .
N5 N 0.5190(8) 0.5027(3) 0.9629(11) 0.026(2) Uani 0.5 1 d D . P A -1
O5 O 0.5819(6) 0.5130(4) 0.8544(11) 0.067(3) Uani 0.5 1 d D . P A -1
O6 O 0.5011(15) 0.4586(4) 0.9986(19) 0.068(7) Uani 0.5 1 d D . P A -1
O7 O 0.4587(14) 0.5357(5) 1.016(2) 0.064(6) Uani 0.5 1 d D . P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.949(4) . ?
Cu1 N1 2.019(3) 7_565 ?
Cu1 N1 2.019(3) . ?
Cu1 O3 2.043(4) 6_556 ?
Cu1 N4 2.173(4) 6_556 ?
Cu2 N3 1.981(5) . ?
Cu2 O4 1.990(4) 1_556 ?
Cu2 N2 2.025(3) 5_666 ?
Cu2 N2 2.025(3) 3_646 ?
Cu2 O2 2.305(4) 6_656 ?
Cu2 O1 2.425(4) . ?
O1 C16 1.284(7) . ?
O2 C16 1.243(6) . ?
O2 Cu2 2.305(4) 6_556 ?
O3 C17 1.267(6) . ?
O3 Cu1 2.043(4) 6_656 ?
O4 C17 1.284(6) . ?
O4 Cu2 1.990(4) 1_554 ?
N1 C1 1.333(5) . ?
N1 C5 1.341(5) . ?
N2 C8 1.340(5) . ?
N2 C12 1.341(5) . ?
N2 Cu2 2.025(3) 5_666 ?
N3 N4 1.333(6) . ?
N3 C13 1.380(6) . ?
N4 C15 1.373(7) . ?
N4 Cu1 2.173(4) 6_656 ?
C1 C2 1.379(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.388(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.393(6) . ?
C3 C6 1.468(5) . ?
C4 C5 1.378(6) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.323(6) . ?
C6 H6 0.9500 . ?
C7 C10 1.469(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.373(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.397(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.396(6) . ?
C11 C12 1.384(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.384(8) . ?
C13 C16 1.470(7) . ?
C14 C15 1.381(7) . ?
C14 H14 0.9500 . ?
C15 C17 1.465(8) . ?
N5 O5 1.232(8) . ?
N5 O6 1.240(10) . ?
N5 O7 1.243(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 N1 90.44(9) . 7_565 ?
O1 Cu1 N1 90.44(9) . . ?
N1 Cu1 N1 164.79(18) 7_565 . ?
O1 Cu1 O3 165.54(14) . 6_556 ?
N1 Cu1 O3 87.68(9) 7_565 6_556 ?
N1 Cu1 O3 87.68(9) . 6_556 ?
O1 Cu1 N4 114.71(16) . 6_556 ?
N1 Cu1 N4 96.71(9) 7_565 6_556 ?
N1 Cu1 N4 96.71(9) . 6_556 ?
O3 Cu1 N4 79.75(15) 6_556 6_556 ?
N3 Cu2 O4 156.89(15) . 1_556 ?
N3 Cu2 N2 92.44(9) . 5_666 ?
O4 Cu2 N2 89.23(9) 1_556 5_666 ?
N3 Cu2 N2 92.44(9) . 3_646 ?
O4 Cu2 N2 89.23(9) 1_556 3_646 ?
N2 Cu2 N2 171.00(18) 5_666 3_646 ?
N3 Cu2 O2 88.30(16) . 6_656 ?
O4 Cu2 O2 114.81(14) 1_556 6_656 ?
N2 Cu2 O2 86.30(9) 5_666 6_656 ?
N2 Cu2 O2 86.30(9) 3_646 6_656 ?
N3 Cu2 O1 74.38(15) . . ?
O4 Cu2 O1 82.51(13) 1_556 . ?
N2 Cu2 O1 94.30(9) 5_666 . ?
N2 Cu2 O1 94.30(9) 3_646 . ?
O2 Cu2 O1 162.68(14) 6_656 . ?
C16 O1 Cu1 122.6(3) . . ?
C16 O1 Cu2 110.8(3) . . ?
Cu1 O1 Cu2 126.63(18) . . ?
C16 O2 Cu2 174.5(4) . 6_556 ?
C17 O3 Cu1 115.4(3) . 6_656 ?
C17 O4 Cu2 133.0(3) . 1_554 ?
C1 N1 C5 117.2(4) . . ?
C1 N1 Cu1 121.8(3) . . ?
C5 N1 Cu1 120.9(3) . . ?
C8 N2 C12 117.5(3) . . ?
C8 N2 Cu2 123.5(3) . 5_666 ?
C12 N2 Cu2 119.0(3) . 5_666 ?
N4 N3 C13 108.1(4) . . ?
N4 N3 Cu2 131.4(3) . . ?
C13 N3 Cu2 120.6(4) . . ?
N3 N4 C15 107.4(4) . . ?
N3 N4 Cu1 143.7(3) . 6_656 ?
C15 N4 Cu1 108.9(3) . 6_656 ?
N1 C1 C2 123.0(4) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C1 C2 C3 120.2(4) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C2 C3 C4 116.7(4) . . ?
C2 C3 C6 120.1(4) . . ?
C4 C3 C6 123.2(4) . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
N1 C5 C4 123.3(4) . . ?
N1 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
C7 C6 C3 125.2(4) . . ?
C7 C6 H6 117.4 . . ?
C3 C6 H6 117.4 . . ?
C6 C7 C10 125.9(4) . . ?
C6 C7 H7 117.1 . . ?
C10 C7 H7 117.1 . . ?
N2 C8 C9 123.6(4) . . ?
N2 C8 H8 118.2 . . ?
C9 C8 H8 118.2 . . ?
C8 C9 C10 119.6(4) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C11 C10 C9 116.8(4) . . ?
C11 C10 C7 120.0(4) . . ?
C9 C10 C7 123.2(4) . . ?
C12 C11 C10 120.1(4) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
N2 C12 C11 122.4(4) . . ?
N2 C12 H12 118.8 . . ?
C11 C12 H12 118.8 . . ?
N3 C13 C14 110.0(4) . . ?
N3 C13 C16 118.7(5) . . ?
C14 C13 C16 131.3(5) . . ?
C15 C14 C13 103.6(5) . . ?
C15 C14 H14 128.2 . . ?
C13 C14 H14 128.2 . . ?
N4 C15 C14 110.8(5) . . ?
N4 C15 C17 116.5(4) . . ?
C14 C15 C17 132.7(5) . . ?
O2 C16 O1 124.9(5) . . ?
O2 C16 C13 119.5(5) . . ?
O1 C16 C13 115.6(4) . . ?
O3 C17 O4 123.9(5) . . ?
O3 C17 C15 119.5(5) . . ?
O4 C17 C15 116.5(4) . . ?
O5 N5 O6 120.5(10) . . ?
O5 N5 O7 119.2(11) . . ?
O6 N5 O7 118.9(12) . . ?

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
C13 N3 N4 C15 0.000(0) . . . . ?
Cu2 N3 N4 C15 180.000(0) . . . . ?
C13 N3 N4 Cu1 180.0 . . . 6_656 ?
Cu2 N3 N4 Cu1 0.000(0) . . . 6_656 ?
C5 N1 C1 C2 0.1(6) . . . . ?
Cu1 N1 C1 C2 -177.1(3) . . . . ?
N1 C1 C2 C3 0.1(6) . . . . ?
C1 C2 C3 C4 -0.1(6) . . . . ?
C1 C2 C3 C6 -178.4(4) . . . . ?
C2 C3 C4 C5 0.0(8) . . . . ?
C6 C3 C4 C5 178.2(5) . . . . ?
C1 N1 C5 C4 -0.2(7) . . . . ?
Cu1 N1 C5 C4 177.0(4) . . . . ?
C3 C4 C5 N1 0.2(9) . . . . ?
C2 C3 C6 C7 -174.6(5) . . . . ?
C4 C3 C6 C7 7.2(8) . . . . ?
C3 C6 C7 C10 -178.2(4) . . . . ?
C12 N2 C8 C9 1.2(6) . . . . ?
Cu2 N2 C8 C9 -180.0(3) 5_666 . . . ?
N2 C8 C9 C10 -0.5(6) . . . . ?
C8 C9 C10 C11 -0.6(6) . . . . ?
C8 C9 C10 C7 177.6(4) . . . . ?
C6 C7 C10 C11 172.8(5) . . . . ?
C6 C7 C10 C9 -5.4(8) . . . . ?
C9 C10 C11 C12 1.1(7) . . . . ?
C7 C10 C11 C12 -177.2(5) . . . . ?
C8 N2 C12 C11 -0.6(6) . . . . ?
Cu2 N2 C12 C11 -179.5(4) 5_666 . . . ?
C10 C11 C12 N2 -0.5(8) . . . . ?
N4 N3 C13 C14 0.000(0) . . . . ?
Cu2 N3 C13 C14 180.000(0) . . . . ?
N4 N3 C13 C16 180.000(0) . . . . ?
Cu2 N3 C13 C16 0.000(0) . . . . ?
N3 C13 C14 C15 0.000(0) . . . . ?
C16 C13 C14 C15 180.000(0) . . . . ?
N3 N4 C15 C14 0.000(0) . . . . ?
Cu1 N4 C15 C14 180.0 6_656 . . . ?
N3 N4 C15 C17 180.000(0) . . . . ?
Cu1 N4 C15 C17 0.000(0) 6_656 . . . ?
C13 C14 C15 N4 0.000(0) . . . . ?
C13 C14 C15 C17 180.000(0) . . . . ?
Cu1 O1 C16 O2 0.000(0) . . . . ?
Cu2 O1 C16 O2 180.000(0) . . . . ?
Cu1 O1 C16 C13 180.000(0) . . . . ?
Cu2 O1 C16 C13 0.000(0) . . . . ?
N3 C13 C16 O2 180.000(0) . . . . ?
C14 C13 C16 O2 0.000(0) . . . . ?
N3 C13 C16 O1 0.000(0) . . . . ?
C14 C13 C16 O1 180.000(0) . . . . ?
Cu1 O3 C17 O4 180.000(0) 6_656 . . . ?
Cu1 O3 C17 C15 0.000(0) 6_656 . . . ?
Cu2 O4 C17 O3 0.000(1) 1_554 . . . ?
Cu2 O4 C17 C15 180.000(0) 1_554 . . . ?
N4 C15 C17 O3 0.000(0) . . . . ?
C14 C15 C17 O3 180.000(0) . . . . ?
N4 C15 C17 O4 180.000(0) . . . . ?
C14 C15 C17 O4 0.000(0) . . . . ?

_refine_diff_density_max         0.650
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.119

####################################################################### 
# 
# 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_compound2
_database_code_depnum_ccdc_archive 'CCDC 1522623'
_audit_update_record             
;
2016-12-14 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            
'Poly{bis(mu-1,2-di(4-pyridyl)ethylene)-mu5-pyrazole-3,5-dicarboxylato)dicopper(II) perchlorate}'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H21 Cl Cu2 N6 O8'
_chemical_formula_weight         744.05

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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.8632(8)
_cell_length_b                   26.6997(18)
_cell_length_c                   8.4942(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2917.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4532
_cell_measurement_theta_min      2.9735
_cell_measurement_theta_max      23.535

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_F_000             1504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.613
_shelx_estimated_absorpt_T_min   0.882
_shelx_estimated_absorpt_T_max   0.953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  
;
Bruker D8 QUEST PHOTON 100
;
_diffrn_measurement_method       '\fandω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            61930
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_av_R_equivalents  0.1430
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.874
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3055
_reflns_number_gt                2031
_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       BrukerAPEX2
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0621P)²+29.7712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3055
_refine_ls_number_parameters     251
_refine_ls_number_restraints     130
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0769
_refine_ls_wR_factor_ref         0.2085
_refine_ls_wR_factor_gt          0.1887
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_restrained_S_all      1.191
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.31890(10) 0.2500 -0.02395(16) 0.0180(4) Uani 1 2 d S T P . .
Cu2 Cu 0.62414(10) 0.2500 0.10495(15) 0.0143(4) Uani 1 2 d S T P . .
O1 O 0.4312(6) 0.2500 0.1316(8) 0.0211(18) Uani 1 2 d S T P . .
O2 O 0.3130(6) 0.2500 0.3236(10) 0.036(2) Uani 1 2 d S T P . .
O3 O 0.7489(5) 0.2500 0.7500(9) 0.0178(16) Uani 1 2 d S T P . .
O4 O 0.5924(6) 0.2500 0.8709(9) 0.0236(18) Uani 1 2 d S T P . .
N1 N 0.5918(6) 0.2500 0.3362(10) 0.0101(18) Uani 1 2 d S T P . .
N2 N 0.6561(7) 0.2500 0.4632(10) 0.016(2) Uani 1 2 d S T P . .
N3 N 0.6419(5) 0.3247(2) 0.0943(8) 0.0223(15) Uani 1 1 d . . . . .
N4 N 0.6656(5) 0.6757(2) 0.0446(8) 0.0253(16) Uani 1 1 d . . . . .
C1 C 0.4903(8) 0.2500 0.3900(13) 0.017(2) Uani 1 2 d S TU P . .
C2 C 0.4900(8) 0.2500 0.5544(11) 0.0126(19) Uani 1 2 d S TU P . .
H2 H 0.4328 0.2500 0.6213 0.015 Uiso 1 2 calc R U P . .
C3 C 0.5979(8) 0.2500 0.5968(12) 0.0151(19) Uani 1 2 d S TU P . .
C4 C 0.4061(8) 0.2500 0.2772(12) 0.012(2) Uani 1 2 d S TU P . .
C5 C 0.6529(8) 0.2500 0.7464(12) 0.012(2) Uani 1 2 d S TU P . .
C6 C 0.7186(9) 0.3439(3) 0.0092(11) 0.045(2) Uani 1 1 d . U . . .
H6 H 0.7647 0.3220 -0.0397 0.054 Uiso 1 1 calc R U . . .
C7 C 0.7332(10) 0.3944(4) -0.0102(13) 0.057(2) Uani 1 1 d . U . . .
H7 H 0.7880 0.4060 -0.0716 0.068 Uiso 1 1 calc R U . . .
C8 C 0.6667(10) 0.4283(3) 0.0614(12) 0.051(2) Uani 1 1 d . U . . .
C9 C 0.5885(8) 0.4084(3) 0.1539(11) 0.0346(19) Uani 1 1 d . U . . .
H9 H 0.5427 0.4295 0.2066 0.042 Uiso 1 1 calc R U . . .
C10 C 0.5786(7) 0.3569(3) 0.1680(10) 0.0274(18) Uani 1 1 d . U . . .
H10 H 0.5258 0.3442 0.2312 0.033 Uiso 1 1 calc R U . . .
C11 C 0.6823(11) 0.4823(4) 0.0396(14) 0.065(3) Uani 1 1 d . U . . .
H11 H 0.7400 0.4922 -0.0185 0.078 Uiso 1 1 calc R U . . .
C12 C 0.6215(11) 0.5181(4) 0.0955(13) 0.060(3) Uani 1 1 d . U . . .
H12 H 0.5628 0.5085 0.1518 0.072 Uiso 1 1 calc R U . . .
C13 C 0.7245(12) 0.6439(4) -0.0339(15) 0.076(4) Uani 1 1 d . U . . .
H13 H 0.7757 0.6567 -0.1000 0.092 Uiso 1 1 calc R U . . .
C14 C 0.7136(11) 0.5928(4) -0.0225(15) 0.076(3) Uani 1 1 d . U . . .
H14 H 0.7566 0.5720 -0.0816 0.091 Uiso 1 1 calc R U . . .
C15 C 0.6405(10) 0.5721(3) 0.0746(12) 0.050(2) Uani 1 1 d . U . . .
C16 C 0.5767(7) 0.6053(3) 0.1550(11) 0.0357(19) Uani 1 1 d . U . . .
H16 H 0.5247 0.5935 0.2213 0.043 Uiso 1 1 calc R U . . .
C17 C 0.5915(7) 0.6564(3) 0.1350(11) 0.033(2) Uani 1 1 d . U . . .
H17 H 0.5472 0.6782 0.1877 0.040 Uiso 1 1 calc R U . . .
Cl1 Cl 0.5377(5) 0.4995(3) 0.5365(7) 0.0613(16) Uani 0.5 1 d D . P A -1
O5 O 0.479(4) 0.5419(14) 0.516(5) 0.31(5) Uani 0.5 1 d D . P A -1
O6 O 0.6086(15) 0.4968(16) 0.419(2) 0.109(9) Uani 0.5 1 d D . P A -1
O7 O 0.5804(13) 0.5014(10) 0.6827(17) 0.135(11) Uani 0.5 1 d D . P A -1
O8 O 0.472(4) 0.4591(14) 0.528(4) 0.21(3) Uani 0.5 1 d D . P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.957(7) . ?
Cu1 N4 2.003(6) 3_645 ?
Cu1 N4 2.003(6) 5_665 ?
Cu1 O3 2.121(8) 6_556 ?
Cu1 N2 2.157(9) 6_556 ?
Cu2 N1 2.008(8) . ?
Cu2 N3 2.008(6) . ?
Cu2 N3 2.008(6) 7_565 ?
Cu2 O4 2.030(8) 1_554 ?
O1 C4 1.278(12) . ?
O2 C4 1.261(13) . ?
O3 C5 1.236(12) . ?
O3 Cu1 2.121(8) 6_656 ?
O4 C5 1.313(12) . ?
O4 Cu2 2.030(8) 1_556 ?
N1 N2 1.360(12) . ?
N1 C1 1.384(13) . ?
N2 C3 1.359(14) . ?
N2 Cu1 2.157(9) 6_656 ?
N3 C6 1.326(11) . ?
N3 C10 1.340(10) . ?
N4 C13 1.317(12) . ?
N4 C17 1.329(11) . ?
N4 Cu1 2.003(6) 5_665 ?
C1 C2 1.396(14) . ?
C1 C4 1.446(15) . ?
C2 C3 1.433(14) . ?
C2 H2 0.9300 . ?
C3 C5 1.455(15) . ?
C6 C7 1.373(12) . ?
C6 H6 0.9300 . ?
C7 C8 1.385(15) . ?
C7 H7 0.9300 . ?
C8 C9 1.382(14) . ?
C8 C11 1.467(13) . ?
C9 C10 1.387(11) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.323(16) . ?
C11 H11 0.9300 . ?
C12 C15 1.473(12) . ?
C12 H12 0.9300 . ?
C13 C14 1.375(14) . ?
C13 H13 0.9300 . ?
C14 C15 1.368(15) . ?
C14 H14 0.9300 . ?
C15 C16 1.388(13) . ?
C16 C17 1.386(11) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
Cl1 O6 1.352(14) . ?
Cl1 O7 1.359(13) . ?
Cl1 O8 1.371(15) . ?
Cl1 O5 1.372(16) . ?

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 Cu1 N4 89.2(2) . 3_645 ?
O1 Cu1 N4 89.2(2) . 5_665 ?
N4 Cu1 N4 164.8(4) 3_645 5_665 ?
O1 Cu1 O3 157.6(3) . 6_556 ?
N4 Cu1 O3 87.9(2) 3_645 6_556 ?
N4 Cu1 O3 87.9(2) 5_665 6_556 ?
O1 Cu1 N2 123.7(3) . 6_556 ?
N4 Cu1 N2 96.7(2) 3_645 6_556 ?
N4 Cu1 N2 96.7(2) 5_665 6_556 ?
O3 Cu1 N2 78.7(3) 6_556 6_556 ?
N1 Cu2 N3 93.87(19) . . ?
N1 Cu2 N3 93.87(19) . 7_565 ?
N3 Cu2 N3 165.9(4) . 7_565 ?
N1 Cu2 O4 156.4(3) . 1_554 ?
N3 Cu2 O4 88.79(19) . 1_554 ?
N3 Cu2 O4 88.79(19) 7_565 1_554 ?
C4 O1 Cu1 117.8(7) . . ?
C5 O3 Cu1 113.7(7) . 6_656 ?
C5 O4 Cu2 132.0(7) . 1_556 ?
N2 N1 C1 108.2(8) . . ?
N2 N1 Cu2 130.6(6) . . ?
C1 N1 Cu2 121.2(7) . . ?
C3 N2 N1 109.1(8) . . ?
C3 N2 Cu1 109.6(7) . 6_656 ?
N1 N2 Cu1 141.3(7) . 6_656 ?
C6 N3 C10 117.3(7) . . ?
C6 N3 Cu2 119.5(6) . . ?
C10 N3 Cu2 123.2(5) . . ?
C13 N4 C17 117.1(8) . . ?
C13 N4 Cu1 122.4(7) . 5_665 ?
C17 N4 Cu1 120.4(6) . 5_665 ?
N1 C1 C2 109.4(9) . . ?
N1 C1 C4 119.2(9) . . ?
C2 C1 C4 131.4(10) . . ?
C1 C2 C3 104.4(9) . . ?
C1 C2 H2 127.8 . . ?
C3 C2 H2 127.8 . . ?
N2 C3 C2 108.9(9) . . ?
N2 C3 C5 117.4(9) . . ?
C2 C3 C5 133.6(9) . . ?
O2 C4 O1 122.8(10) . . ?
O2 C4 C1 120.3(10) . . ?
O1 C4 C1 116.9(9) . . ?
O3 C5 O4 124.9(10) . . ?
O3 C5 C3 120.5(9) . . ?
O4 C5 C3 114.5(8) . . ?
N3 C6 C7 123.2(9) . . ?
N3 C6 H6 118.4 . . ?
C7 C6 H6 118.4 . . ?
C6 C7 C8 120.3(9) . . ?
C6 C7 H7 119.8 . . ?
C8 C7 H7 119.8 . . ?
C9 C8 C7 116.6(8) . . ?
C9 C8 C11 123.3(10) . . ?
C7 C8 C11 120.1(10) . . ?
C8 C9 C10 119.8(9) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
N3 C10 C9 122.8(8) . . ?
N3 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
C12 C11 C8 125.8(11) . . ?
C12 C11 H11 117.1 . . ?
C8 C11 H11 117.1 . . ?
C11 C12 C15 124.5(11) . . ?
C11 C12 H12 117.7 . . ?
C15 C12 H12 117.7 . . ?
N4 C13 C14 123.0(10) . . ?
N4 C13 H13 118.5 . . ?
C14 C13 H13 118.5 . . ?
C15 C14 C13 120.9(10) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C16 116.4(9) . . ?
C14 C15 C12 125.6(10) . . ?
C16 C15 C12 118.0(10) . . ?
C17 C16 C15 119.2(9) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
N4 C17 C16 123.4(8) . . ?
N4 C17 H17 118.3 . . ?
C16 C17 H17 118.3 . . ?
O6 Cl1 O7 113.7(10) . . ?
O6 Cl1 O8 109.6(13) . . ?
O7 Cl1 O8 108.9(12) . . ?
O6 Cl1 O5 108.8(14) . . ?
O7 Cl1 O5 108.1(13) . . ?
O8 Cl1 O5 107.7(14) . . ?

_refine_diff_density_max         0.768
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.177

####################################################################### 
# 
# 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_compound3
_database_code_depnum_ccdc_archive 'CCDC 1522624'
_audit_update_record             
;
2016-12-14 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            
'Poly{bis(mu-1,2-di(4-pyridyl)ethylene)-mu5-pyrazole-3,5-dicarboxylato)dicopper(II) tetrafluoroborate}'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H21 B Cu2 F4 N6 O4'
_chemical_formula_weight         731.41

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.7573(6)
_cell_length_b                   26.7175(13)
_cell_length_c                   8.4773(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2889.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6379
_cell_measurement_theta_min      2.984
_cell_measurement_theta_max      26.888

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_F_000             1472
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.546
_shelx_estimated_absorpt_T_min   0.899
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6853
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  
;
Bruker D8 QUEST PHOTON 100
;
_diffrn_measurement_method       '\fandω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16481
_diffrn_reflns_av_unetI/netI     0.1181
_diffrn_reflns_av_R_equivalents  0.1274
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.984
_diffrn_reflns_theta_max         28.296
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3659
_reflns_number_gt                2168
_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       BrukerAPEX2
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0461P)²+13.3725P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3659
_refine_ls_number_parameters     251
_refine_ls_number_restraints     195
_refine_ls_R_factor_all          0.1487
_refine_ls_R_factor_gt           0.0697
_refine_ls_wR_factor_ref         0.1589
_refine_ls_wR_factor_gt          0.1352
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.67697(7) 0.7500 -0.02753(11) 0.0158(3) Uani 1 2 d S T P . .
Cu2 Cu 0.37293(7) 0.7500 1.10669(11) 0.0133(2) Uani 1 2 d S T P . .
O1 O 0.5661(4) 0.7500 0.1314(6) 0.0184(12) Uani 1 2 d S T P . .
O2 O 0.6852(4) 0.7500 0.3250(7) 0.0342(16) Uani 1 2 d S T P . .
O3 O 0.4047(4) 0.7500 0.8724(6) 0.0201(13) Uani 1 2 d S T P . .
O4 O 0.2478(4) 0.7500 0.7504(6) 0.0168(12) Uani 1 2 d S T P . .
N1 N 0.6612(4) 0.67552(16) -0.0483(6) 0.0243(11) Uani 1 1 d . . . . .
N2 N 0.6429(4) 0.32492(16) -0.0963(5) 0.0192(10) Uani 1 1 d . . . . .
N3 N 0.4052(4) 0.7500 0.3371(7) 0.0112(13) Uani 1 2 d S T P . .
N4 N 0.3414(5) 0.7500 0.4636(7) 0.0139(13) Uani 1 2 d S T P . .
C1 C 0.7225(7) 0.6442(3) 0.0290(10) 0.062(2) Uani 1 1 d . U . . .
H1 H 0.7738 0.6570 0.0956 0.074 Uiso 1 1 calc R U . . .
C2 C 0.7126(7) 0.5929(3) 0.0140(10) 0.067(2) Uani 1 1 d . U . . .
H2 H 0.7581 0.5721 0.0692 0.080 Uiso 1 1 calc R U . . .
C3 C 0.6376(6) 0.5722(2) -0.0800(8) 0.0432(16) Uani 1 1 d . U . . .
C4 C 0.5730(5) 0.6051(2) -0.1570(8) 0.0342(14) Uani 1 1 d . U . . .
H4 H 0.5200 0.5933 -0.2224 0.041 Uiso 1 1 calc R U . . .
C5 C 0.5868(5) 0.6559(2) -0.1372(8) 0.0328(15) Uani 1 1 d . U . . .
H5 H 0.5412 0.6775 -0.1892 0.039 Uiso 1 1 calc R U . . .
C6 C 0.6199(7) 0.5182(2) -0.1000(9) 0.0474(16) Uani 1 1 d . U . . .
H6 H 0.5608 0.5083 -0.1560 0.057 Uiso 1 1 calc R U . . .
C7 C 0.6817(7) 0.4829(3) -0.0444(9) 0.0545(18) Uani 1 1 d . U . . .
H7 H 0.7397 0.4930 0.0139 0.065 Uiso 1 1 calc R U . . .
C8 C 0.7199(6) 0.3442(2) -0.0106(8) 0.0395(17) Uani 1 1 d . U . . .
H8 H 0.7658 0.3226 0.0407 0.047 Uiso 1 1 calc R U . . .
C9 C 0.7346(6) 0.3952(3) 0.0054(9) 0.0509(18) Uani 1 1 d . U . . .
H9 H 0.7905 0.4071 0.0651 0.061 Uiso 1 1 calc R U . . .
C10 C 0.6669(6) 0.4289(2) -0.0665(8) 0.0418(15) Uani 1 1 d . U . . .
C11 C 0.5893(5) 0.4082(2) -0.1578(7) 0.0287(13) Uani 1 1 d . U . . .
H11 H 0.5432 0.4289 -0.2121 0.034 Uiso 1 1 calc R U . . .
C12 C 0.5791(4) 0.3570(2) -0.1695(7) 0.0227(13) Uani 1 1 d . U . . .
H12 H 0.5252 0.3442 -0.2313 0.027 Uiso 1 1 calc R U . . .
C13 C 0.5062(6) 0.7500 0.3909(9) 0.0157(16) Uani 1 2 d S T P . .
C14 C 0.5082(6) 0.7500 0.5559(8) 0.0130(16) Uani 1 2 d S T P . .
H14 H 0.5662 0.7500 0.6224 0.016 Uiso 1 2 calc R U P . .
C15 C 0.4012(6) 0.7500 0.5970(9) 0.0163(16) Uani 1 2 d S T P . .
C16 C 0.5922(6) 0.7500 0.2770(9) 0.0140(16) Uani 1 2 d S T P . .
C17 C 0.3464(5) 0.7500 0.7489(9) 0.0132(16) Uani 1 2 d S T P . .
B1 B 0.4711(10) 0.4988(5) 0.5363(14) 0.055(5) Uani 0.5 1 d D . P A -1
F1 F 0.5422(19) 0.5363(10) 0.532(2) 0.159(8) Uani 0.5 1 d D U P A -1
F2 F 0.3988(9) 0.5058(7) 0.4259(13) 0.101(4) Uani 0.5 1 d D U P A -1
F3 F 0.525(2) 0.4568(8) 0.501(3) 0.177(9) Uani 0.5 1 d D U P A -1
F4 F 0.4280(9) 0.4965(5) 0.6796(12) 0.120(5) Uani 0.5 1 d D U P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.954(5) . ?
Cu1 N1 2.008(4) . ?
Cu1 N1 2.008(4) 7_575 ?
Cu1 O4 2.094(5) 6_656 ?
Cu1 N4 2.167(6) 6_656 ?
Cu2 N3 1.996(6) 1_556 ?
Cu2 N2 2.014(4) 5_666 ?
Cu2 N2 2.014(4) 3_656 ?
Cu2 O3 2.027(5) . ?
O1 C16 1.279(9) . ?
O2 C16 1.255(9) . ?
O3 C17 1.284(9) . ?
O4 C17 1.258(8) . ?
O4 Cu1 2.094(5) 6_556 ?
N1 C1 1.319(8) . ?
N1 C5 1.321(8) . ?
N2 C8 1.326(7) . ?
N2 C12 1.336(7) . ?
N2 Cu2 2.014(4) 5_666 ?
N3 N4 1.346(8) . ?
N3 C13 1.366(9) . ?
N3 Cu2 1.996(6) 1_554 ?
N4 C15 1.364(10) . ?
N4 Cu1 2.167(6) 6_556 ?
C1 C2 1.383(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.363(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.371(9) . ?
C3 C6 1.469(8) . ?
C4 C5 1.379(8) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C7 1.318(10) . ?
C6 H6 0.9300 . ?
C7 C10 1.468(9) . ?
C7 H7 0.9300 . ?
C8 C9 1.382(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.388(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.372(9) . ?
C11 C12 1.376(8) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.399(10) . ?
C13 C16 1.462(11) . ?
C14 C15 1.409(10) . ?
C14 H14 0.9300 . ?
C15 C17 1.465(10) . ?
B1 F2 1.327(10) . ?
B1 F4 1.335(10) . ?
B1 F3 1.351(11) . ?
B1 F1 1.352(11) . ?

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 Cu1 N1 89.32(14) . . ?
O1 Cu1 N1 89.32(14) . 7_575 ?
N1 Cu1 N1 164.7(3) . 7_575 ?
O1 Cu1 O4 159.2(2) . 6_656 ?
N1 Cu1 O4 87.93(14) . 6_656 ?
N1 Cu1 O4 87.93(14) 7_575 6_656 ?
O1 Cu1 N4 121.9(2) . 6_656 ?
N1 Cu1 N4 96.82(15) . 6_656 ?
N1 Cu1 N4 96.82(15) 7_575 6_656 ?
O4 Cu1 N4 78.9(2) 6_656 6_656 ?
N3 Cu2 N2 93.64(13) 1_556 5_666 ?
N3 Cu2 N2 93.64(13) 1_556 3_656 ?
N2 Cu2 N2 167.4(3) 5_666 3_656 ?
N3 Cu2 O3 156.6(2) 1_556 . ?
N2 Cu2 O3 88.70(13) 5_666 . ?
N2 Cu2 O3 88.70(13) 3_656 . ?
C16 O1 Cu1 118.5(5) . . ?
C17 O3 Cu2 133.1(5) . . ?
C17 O4 Cu1 115.0(5) . 6_556 ?
C1 N1 C5 117.3(5) . . ?
C1 N1 Cu1 121.7(5) . . ?
C5 N1 Cu1 121.0(4) . . ?
C8 N2 C12 117.1(5) . . ?
C8 N2 Cu2 119.0(4) . 5_666 ?
C12 N2 Cu2 123.8(4) . 5_666 ?
N4 N3 C13 107.7(6) . . ?
N4 N3 Cu2 130.9(4) . 1_554 ?
C13 N3 Cu2 121.4(5) . 1_554 ?
N3 N4 C15 108.8(6) . . ?
N3 N4 Cu1 141.7(5) . 6_556 ?
C15 N4 Cu1 109.5(5) . 6_556 ?
N1 C1 C2 121.9(7) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C3 C2 C1 121.3(7) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C2 C3 C4 116.1(6) . . ?
C2 C3 C6 125.0(7) . . ?
C4 C3 C6 118.9(6) . . ?
C3 C4 C5 119.9(6) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 123.4(6) . . ?
N1 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
C7 C6 C3 124.8(7) . . ?
C7 C6 H6 117.6 . . ?
C3 C6 H6 117.6 . . ?
C6 C7 C10 125.6(7) . . ?
C6 C7 H7 117.2 . . ?
C10 C7 H7 117.2 . . ?
N2 C8 C9 122.6(6) . . ?
N2 C8 H8 118.7 . . ?
C9 C8 H8 118.7 . . ?
C8 C9 C10 120.7(6) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C11 C10 C9 115.9(6) . . ?
C11 C10 C7 124.1(6) . . ?
C9 C10 C7 120.0(6) . . ?
C10 C11 C12 120.6(6) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
N2 C12 C11 123.1(5) . . ?
N2 C12 H12 118.4 . . ?
C11 C12 H12 118.4 . . ?
N3 C13 C14 110.6(7) . . ?
N3 C13 C16 119.1(7) . . ?
C14 C13 C16 130.3(7) . . ?
C13 C14 C15 103.2(7) . . ?
C13 C14 H14 128.4 . . ?
C15 C14 H14 128.4 . . ?
N4 C15 C14 109.7(6) . . ?
N4 C15 C17 117.5(6) . . ?
C14 C15 C17 132.8(7) . . ?
O2 C16 O1 124.0(7) . . ?
O2 C16 C13 119.7(7) . . ?
O1 C16 C13 116.3(7) . . ?
O4 C17 O3 124.8(7) . . ?
O4 C17 C15 119.1(7) . . ?
O3 C17 C15 116.1(6) . . ?
F2 B1 F4 111.3(10) . . ?
F2 B1 F3 108.4(11) . . ?
F4 B1 F3 111.8(12) . . ?
F2 B1 F1 110.1(11) . . ?
F4 B1 F1 109.5(11) . . ?
F3 B1 F1 105.5(11) . . ?

_refine_diff_density_max         0.797
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.135

