# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_xzh3-81d_a
_database_code_depnum_ccdc_archive 'CCDC 2227207'
loop_
_audit_author_name
_audit_author_address
'Simon J. Teat'
;Advanced Light Source, Lawrence Berkeley National Laboratory
United States of America
;
_audit_update_record             
;
2022-12-17 deposited with the CCDC.	2023-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H48 Cu6 I8 N18 O2'
_chemical_formula_weight         2233.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
H H 0.0000 0.0000
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
N N 0.0065 0.0035
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
O O 0.0115 0.0064
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
Cu Cu 0.3203 1.3289
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
I I -0.3993 1.9038
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'

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

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

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

_cell_length_a                   10.3781(4)
_cell_length_b                   10.8319(5)
_cell_length_c                   15.0528(6)
_cell_angle_alpha                71.647(2)
_cell_angle_beta                 72.550(2)
_cell_angle_gamma                74.302(2)
_cell_volume                     1502.90(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9872
_cell_measurement_theta_min      2.5175
_cell_measurement_theta_max      31.4286

_exptl_crystal_description       Rod
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.468
_exptl_crystal_F_000             1040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.005
_exptl_absorpt_coefficient_mu    6.628
_shelx_estimated_absorpt_T_min   0.692
_shelx_estimated_absorpt_T_max   0.968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_process_details   'SADABS 2016/2 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source beamline 12.2.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTONII detector'
_diffrn_measurement_method       'ω/θ shutterless scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            54702
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.150
_diffrn_reflns_theta_max         31.436
_diffrn_reflns_theta_full        25.930
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9209
_reflns_number_gt                8236
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40a'
_computing_data_reduction        'Bruker SAINT v8.40a'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;
 All non-hydrogen atoms were refined anisotropically. Hydrogen
 atoms were found in the fourier difference map constrained were
 refined using a riding model. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0224P)²+2.5184P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Dual space'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9209
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_ref         0.0567
_refine_ls_wR_factor_gt          0.0546
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.004
_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 0.44479(3) 0.62599(3) 0.69818(2) 0.01667(6) Uani 1 1 d . . . . .
Cu2 Cu 0.36156(3) 0.59761(3) 0.54254(2) 0.02182(7) Uani 1 1 d . . . . .
Cu3 Cu 0.18481(3) 0.71416(3) 0.78579(2) 0.02089(7) Uani 1 1 d . . . . .
I1 I 0.61095(2) 0.62105(2) 0.52404(2) 0.01549(4) Uani 1 1 d . . . . .
I2 I 0.23622(2) 0.50548(2) 0.72489(2) 0.01894(4) Uani 1 1 d . . . . .
I3 I 0.34305(2) 0.87829(2) 0.69264(2) 0.01832(4) Uani 1 1 d . . . . .
I4 I -0.02174(2) 0.74963(2) 0.91845(2) 0.02323(4) Uani 1 1 d . . . . .
N1 N 0.5522(2) 0.5319(2) 0.80105(15) 0.0150(4) Uani 1 1 d . . . . .
N2 N 0.6801(2) 0.5421(2) 0.78261(15) 0.0149(4) Uani 1 1 d . . . . .
N3 N 0.7345(2) 0.4593(2) 0.85620(14) 0.0141(4) Uani 1 1 d . . . . .
C1 C 0.5210(2) 0.4401(2) 0.88826(17) 0.0141(4) Uani 1 1 d . . . . .
C2 C 0.3986(3) 0.3951(2) 0.94103(18) 0.0170(5) Uani 1 1 d . . . . .
H2A H 0.316515 0.427603 0.918338 0.020 Uiso 1 1 calc R U . . .
C3 C 0.4031(3) 0.3018(3) 1.02707(19) 0.0200(5) Uani 1 1 d . . . . .
H3A H 0.322138 0.268675 1.064307 0.024 Uiso 1 1 calc R U . . .
C4 C 0.5242(3) 0.2536(3) 1.06195(19) 0.0202(5) Uani 1 1 d . . . . .
H4A H 0.522101 0.189506 1.122103 0.024 Uiso 1 1 calc R U . . .
C5 C 0.6451(3) 0.2967(2) 1.01131(18) 0.0180(5) Uani 1 1 d . . . . .
H5A H 0.726902 0.264324 1.034361 0.022 Uiso 1 1 calc R U . . .
N6 N 0.9614(2) 0.1774(2) 0.57167(15) 0.0147(4) Uani 1 1 d . . . . .
C7 C 0.8807(2) 0.4370(2) 0.84789(18) 0.0155(4) Uani 1 1 d . . . . .
H7A H 0.898813 0.413037 0.912755 0.019 Uiso 1 1 calc R U . . .
H7B H 0.915342 0.519398 0.810118 0.019 Uiso 1 1 calc R U . . .
N4 N 0.9529(2) 0.3301(2) 0.80031(15) 0.0138(4) Uani 1 1 d . . . . .
C8 C 0.9849(2) 0.3433(2) 0.70551(17) 0.0139(4) Uani 1 1 d . . . . .
N5 N 1.0389(2) 0.2220(2) 0.69184(15) 0.0146(4) Uani 1 1 d . . . . .
C9 C 1.0380(3) 0.1291(3) 0.77997(18) 0.0182(5) Uani 1 1 d . . . . .
H9A H 1.068883 0.035902 0.790299 0.022 Uiso 1 1 calc R U . . .
C10 C 0.9843(3) 0.1976(2) 0.84814(19) 0.0180(5) Uani 1 1 d . . . . .
H10A H 0.970700 0.161839 0.915809 0.022 Uiso 1 1 calc R U . . .
C11 C 0.9621(3) 0.4664(2) 0.62974(18) 0.0176(5) Uani 1 1 d . . . . .
H11A H 1.042582 0.467574 0.575137 0.026 Uiso 1 1 calc R U . . .
H11B H 0.948283 0.542933 0.655334 0.026 Uiso 1 1 calc R U . . .
H11C H 0.880375 0.470513 0.608311 0.026 Uiso 1 1 calc R U . . .
C12 C 1.0790(2) 0.1891(3) 0.59872(17) 0.0155(4) Uani 1 1 d . . . . .
H12A H 1.123963 0.259067 0.548687 0.019 Uiso 1 1 calc R U . . .
H12B H 1.146554 0.104359 0.602431 0.019 Uiso 1 1 calc R U . . .
C6 C 0.6398(2) 0.3912(2) 0.92381(17) 0.0146(4) Uani 1 1 d . . . . .
N7 N 0.8866(2) 0.2862(2) 0.52376(15) 0.0166(4) Uani 1 1 d . . . . .
N8 N 0.7788(2) 0.2542(2) 0.51639(15) 0.0168(4) Uani 1 1 d . . . . .
C13 C 0.8999(2) 0.0704(2) 0.59685(17) 0.0145(4) Uani 1 1 d . . . . .
C14 C 0.9356(3) -0.0621(3) 0.64606(19) 0.0196(5) Uani 1 1 d . . . . .
H14A H 1.016129 -0.095065 0.670514 0.024 Uiso 1 1 calc R U . . .
C15 C 0.8457(3) -0.1413(3) 0.6566(2) 0.0239(5) Uani 1 1 d . . . . .
H15A H 0.864745 -0.232231 0.689677 0.029 Uiso 1 1 calc R U . . .
C16 C 0.7260(3) -0.0924(3) 0.6199(2) 0.0230(5) Uani 1 1 d . . . . .
H16A H 0.667405 -0.151412 0.629000 0.028 Uiso 1 1 calc R U . . .
C17 C 0.6919(3) 0.0387(3) 0.57132(19) 0.0197(5) Uani 1 1 d . . . . .
H17A H 0.611162 0.071514 0.547014 0.024 Uiso 1 1 calc R U . . .
C18 C 0.7826(2) 0.1206(2) 0.55977(17) 0.0154(4) Uani 1 1 d . . . . .
O1S O 0.7377(2) 0.2746(2) 0.73342(14) 0.0238(4) Uani 1 1 d . . . . .
C1S C 0.6255(3) 0.2558(3) 0.7371(2) 0.0224(5) Uani 1 1 d . . . . .
H1SA H 0.573549 0.319382 0.694553 0.027 Uiso 1 1 calc R U . . .
N1S N 0.5700(3) 0.1536(2) 0.79583(19) 0.0262(5) Uani 1 1 d . . . . .
C2S C 0.6452(4) 0.0525(3) 0.8611(3) 0.0393(8) Uani 1 1 d . . . . .
H2SA H 0.589992 -0.015220 0.899006 0.059 Uiso 1 1 calc R U . . .
H2SB H 0.732202 0.011491 0.824088 0.059 Uiso 1 1 calc R U . . .
H2SC H 0.664350 0.092907 0.904431 0.059 Uiso 1 1 calc R U . . .
C3S C 0.4368(4) 0.1365(4) 0.7960(3) 0.0454(9) Uani 1 1 d . . . . .
H3SA H 0.415117 0.055261 0.844422 0.068 Uiso 1 1 calc R U . . .
H3SB H 0.366693 0.212740 0.811486 0.068 Uiso 1 1 calc R U . . .
H3SC H 0.438144 0.129792 0.732318 0.068 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.027(2) . ?
Cu1 I3 2.6341(4) . ?
Cu1 I1 2.6786(4) . ?
Cu1 Cu3 2.6825(5) . ?
Cu1 I2 2.6884(4) . ?
Cu1 Cu2 2.8533(5) . ?
Cu2 N8 2.024(2) 2_666 ?
Cu2 I1 2.5922(4) . ?
Cu2 I2 2.6568(4) . ?
Cu2 I1 2.7664(4) 2_666 ?
Cu3 I4 2.4901(4) . ?
Cu3 I3 2.5402(4) . ?
Cu3 I2 2.5677(4) . ?
N1 N2 1.300(3) . ?
N1 C1 1.384(3) . ?
N2 N3 1.351(3) . ?
N3 C6 1.366(3) . ?
N3 C7 1.443(3) . ?
C1 C6 1.396(3) . ?
C1 C2 1.403(3) . ?
C2 C3 1.374(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.413(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.376(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.396(3) . ?
C5 H5A 0.9500 . ?
N6 N7 1.348(3) . ?
N6 C13 1.368(3) . ?
N6 C12 1.445(3) . ?
C7 N4 1.465(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N4 C8 1.334(3) . ?
N4 C10 1.386(3) . ?
C8 N5 1.337(3) . ?
C8 C11 1.472(3) . ?
N5 C9 1.389(3) . ?
N5 C12 1.466(3) . ?
C9 C10 1.352(4) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N7 N8 1.302(3) . ?
N8 C18 1.383(3) . ?
C13 C18 1.395(3) . ?
C13 C14 1.397(3) . ?
C14 C15 1.375(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.414(4) . ?
C15 H15A 0.9500 . ?
C16 C17 1.380(4) . ?
C16 H16A 0.9500 . ?
C17 C18 1.401(3) . ?
C17 H17A 0.9500 . ?
O1S C1S 1.218(3) . ?
C1S N1S 1.328(4) . ?
C1S H1SA 0.9500 . ?
N1S C3S 1.443(4) . ?
N1S C2S 1.446(4) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 I3 113.58(6) . . ?
N1 Cu1 I1 109.75(6) . . ?
I3 Cu1 I1 105.834(12) . . ?
N1 Cu1 Cu3 107.97(6) . . ?
I3 Cu1 Cu3 57.074(11) . . ?
I1 Cu1 Cu3 142.276(15) . . ?
N1 Cu1 I2 110.34(6) . . ?
I3 Cu1 I2 108.405(12) . . ?
I1 Cu1 I2 108.744(12) . . ?
Cu3 Cu1 I2 57.121(11) . . ?
N1 Cu1 Cu2 144.63(6) . . ?
I3 Cu1 Cu2 101.729(13) . . ?
I1 Cu1 Cu2 55.778(10) . . ?
Cu3 Cu1 Cu2 92.467(14) . . ?
I2 Cu1 Cu2 57.202(10) . . ?
N8 Cu2 I1 123.16(6) 2_666 . ?
N8 Cu2 I2 106.20(6) 2_666 . ?
I1 Cu2 I2 112.417(13) . . ?
N8 Cu2 I1 108.25(6) 2_666 2_666 ?
I1 Cu2 I1 105.339(13) . 2_666 ?
I2 Cu2 I1 98.673(12) . 2_666 ?
N8 Cu2 Cu1 118.37(6) 2_666 . ?
I1 Cu2 Cu1 58.697(10) . . ?
I2 Cu2 Cu1 58.276(10) . . ?
I1 Cu2 Cu1 131.816(14) 2_666 . ?
I4 Cu3 I3 125.406(16) . . ?
I4 Cu3 I2 118.999(15) . . ?
I3 Cu3 I2 115.379(14) . . ?
I4 Cu3 Cu1 159.249(16) . . ?
I3 Cu3 Cu1 60.503(11) . . ?
I2 Cu3 Cu1 61.555(11) . . ?
Cu2 I1 Cu1 65.524(11) . . ?
Cu2 I1 Cu2 74.662(13) . 2_666 ?
Cu1 I1 Cu2 117.014(12) . 2_666 ?
Cu3 I2 Cu2 99.892(13) . . ?
Cu3 I2 Cu1 61.324(11) . . ?
Cu2 I2 Cu1 64.522(11) . . ?
Cu3 I3 Cu1 62.423(11) . . ?
N2 N1 C1 109.1(2) . . ?
N2 N1 Cu1 118.84(16) . . ?
C1 N1 Cu1 131.46(16) . . ?
N1 N2 N3 108.17(19) . . ?
N2 N3 C6 111.0(2) . . ?
N2 N3 C7 119.6(2) . . ?
C6 N3 C7 128.5(2) . . ?
N1 C1 C6 107.8(2) . . ?
N1 C1 C2 131.9(2) . . ?
C6 C1 C2 120.3(2) . . ?
C3 C2 C1 116.8(2) . . ?
C3 C2 H2A 121.6 . . ?
C1 C2 H2A 121.6 . . ?
C2 C3 C4 122.1(2) . . ?
C2 C3 H3A 118.9 . . ?
C4 C3 H3A 118.9 . . ?
C5 C4 C3 121.9(2) . . ?
C5 C4 H4A 119.0 . . ?
C3 C4 H4A 119.0 . . ?
C4 C5 C6 115.6(2) . . ?
C4 C5 H5A 122.2 . . ?
C6 C5 H5A 122.2 . . ?
N7 N6 C13 110.7(2) . . ?
N7 N6 C12 119.7(2) . . ?
C13 N6 C12 129.2(2) . . ?
N3 C7 N4 110.13(19) . . ?
N3 C7 H7A 109.6 . . ?
N4 C7 H7A 109.6 . . ?
N3 C7 H7B 109.6 . . ?
N4 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
C8 N4 C10 110.0(2) . . ?
C8 N4 C7 125.2(2) . . ?
C10 N4 C7 124.5(2) . . ?
N4 C8 N5 106.8(2) . . ?
N4 C8 C11 127.2(2) . . ?
N5 C8 C11 125.9(2) . . ?
C8 N5 C9 110.0(2) . . ?
C8 N5 C12 125.2(2) . . ?
C9 N5 C12 124.5(2) . . ?
C10 C9 N5 106.4(2) . . ?
C10 C9 H9A 126.8 . . ?
N5 C9 H9A 126.8 . . ?
C9 C10 N4 106.8(2) . . ?
C9 C10 H10A 126.6 . . ?
N4 C10 H10A 126.6 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N6 C12 N5 111.47(19) . . ?
N6 C12 H12A 109.3 . . ?
N5 C12 H12A 109.3 . . ?
N6 C12 H12B 109.3 . . ?
N5 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
N3 C6 C1 103.9(2) . . ?
N3 C6 C5 132.8(2) . . ?
C1 C6 C5 123.3(2) . . ?
N8 N7 N6 108.6(2) . . ?
N7 N8 C18 108.7(2) . . ?
N7 N8 Cu2 117.34(16) . 2_666 ?
C18 N8 Cu2 133.73(17) . 2_666 ?
N6 C13 C18 103.9(2) . . ?
N6 C13 C14 132.8(2) . . ?
C18 C13 C14 123.3(2) . . ?
C15 C14 C13 115.2(2) . . ?
C15 C14 H14A 122.4 . . ?
C13 C14 H14A 122.4 . . ?
C14 C15 C16 122.4(3) . . ?
C14 C15 H15A 118.8 . . ?
C16 C15 H15A 118.8 . . ?
C17 C16 C15 121.9(2) . . ?
C17 C16 H16A 119.1 . . ?
C15 C16 H16A 119.1 . . ?
C16 C17 C18 116.4(2) . . ?
C16 C17 H17A 121.8 . . ?
C18 C17 H17A 121.8 . . ?
N8 C18 C13 108.0(2) . . ?
N8 C18 C17 131.2(2) . . ?
C13 C18 C17 120.8(2) . . ?
O1S C1S N1S 125.1(3) . . ?
O1S C1S H1SA 117.4 . . ?
N1S C1S H1SA 117.4 . . ?
C1S N1S C3S 122.4(3) . . ?
C1S N1S C2S 119.9(3) . . ?
C3S N1S C2S 117.6(3) . . ?
N1S C2S H2SA 109.5 . . ?
N1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
N1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
N1S C3S H3SA 109.5 . . ?
N1S C3S H3SB 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
N1S C3S H3SC 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 N2 N3 -0.3(3) . . . . ?
Cu1 N1 N2 N3 -172.71(15) . . . . ?
N1 N2 N3 C6 1.1(3) . . . . ?
N1 N2 N3 C7 171.3(2) . . . . ?
N2 N1 C1 C6 -0.6(3) . . . . ?
Cu1 N1 C1 C6 170.51(17) . . . . ?
N2 N1 C1 C2 178.6(3) . . . . ?
Cu1 N1 C1 C2 -10.3(4) . . . . ?
N1 C1 C2 C3 -179.6(2) . . . . ?
C6 C1 C2 C3 -0.5(4) . . . . ?
C1 C2 C3 C4 0.6(4) . . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C3 C4 C5 C6 0.2(4) . . . . ?
N2 N3 C7 N4 -86.4(3) . . . . ?
C6 N3 C7 N4 81.7(3) . . . . ?
N3 C7 N4 C8 80.0(3) . . . . ?
N3 C7 N4 C10 -92.5(3) . . . . ?
C10 N4 C8 N5 -1.3(3) . . . . ?
C7 N4 C8 N5 -174.8(2) . . . . ?
C10 N4 C8 C11 177.1(2) . . . . ?
C7 N4 C8 C11 3.6(4) . . . . ?
N4 C8 N5 C9 1.6(3) . . . . ?
C11 C8 N5 C9 -176.8(2) . . . . ?
N4 C8 N5 C12 175.2(2) . . . . ?
C11 C8 N5 C12 -3.2(4) . . . . ?
C8 N5 C9 C10 -1.3(3) . . . . ?
C12 N5 C9 C10 -174.9(2) . . . . ?
N5 C9 C10 N4 0.4(3) . . . . ?
C8 N4 C10 C9 0.6(3) . . . . ?
C7 N4 C10 C9 174.0(2) . . . . ?
N7 N6 C12 N5 86.9(3) . . . . ?
C13 N6 C12 N5 -84.7(3) . . . . ?
C8 N5 C12 N6 -80.5(3) . . . . ?
C9 N5 C12 N6 92.2(3) . . . . ?
N2 N3 C6 C1 -1.5(3) . . . . ?
C7 N3 C6 C1 -170.5(2) . . . . ?
N2 N3 C6 C5 -179.6(3) . . . . ?
C7 N3 C6 C5 11.3(4) . . . . ?
N1 C1 C6 N3 1.2(3) . . . . ?
C2 C1 C6 N3 -178.1(2) . . . . ?
N1 C1 C6 C5 179.6(2) . . . . ?
C2 C1 C6 C5 0.3(4) . . . . ?
C4 C5 C6 N3 177.7(3) . . . . ?
C4 C5 C6 C1 -0.2(4) . . . . ?
C13 N6 N7 N8 -0.2(3) . . . . ?
C12 N6 N7 N8 -173.3(2) . . . . ?
N6 N7 N8 C18 -0.5(3) . . . . ?
N6 N7 N8 Cu2 174.83(15) . . . 2_666 ?
N7 N6 C13 C18 0.8(3) . . . . ?
C12 N6 C13 C18 173.1(2) . . . . ?
N7 N6 C13 C14 179.9(3) . . . . ?
C12 N6 C13 C14 -7.8(4) . . . . ?
N6 C13 C14 C15 -179.4(3) . . . . ?
C18 C13 C14 C15 -0.5(4) . . . . ?
C13 C14 C15 C16 0.2(4) . . . . ?
C14 C15 C16 C17 -0.2(4) . . . . ?
C15 C16 C17 C18 0.3(4) . . . . ?
N7 N8 C18 C13 1.0(3) . . . . ?
Cu2 N8 C18 C13 -173.24(18) 2_666 . . . ?
N7 N8 C18 C17 179.9(3) . . . . ?
Cu2 N8 C18 C17 5.6(4) 2_666 . . . ?
N6 C13 C18 N8 -1.1(3) . . . . ?
C14 C13 C18 N8 179.7(2) . . . . ?
N6 C13 C18 C17 179.9(2) . . . . ?
C14 C13 C18 C17 0.7(4) . . . . ?
C16 C17 C18 N8 -179.3(3) . . . . ?
C16 C17 C18 C13 -0.6(4) . . . . ?
O1S C1S N1S C3S -179.4(3) . . . . ?
O1S C1S N1S C2S -1.0(5) . . . . ?

_refine_diff_density_max         1.661
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.132



####################################################################### 
# 
# 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_XZH3-77a_a
_database_code_depnum_ccdc_archive 'CCDC 2227210'
loop_
_audit_author_name
_audit_author_address
'Simon J. Teat'
;Advanced Light Source, Lawrence Berkeley National Laboratory
United States of America
;
_audit_update_record             
;
2022-12-17 deposited with the CCDC.	2023-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H15 Cu3 I4 N8'
_chemical_formula_weight         1029.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
H H 0.0000 0.0000
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
N N 0.0065 0.0035
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
Cu Cu 0.3203 1.3289
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
I I -0.3993 1.9038
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'

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

_cell_length_a                   13.6626(8)
_cell_length_b                   13.9283(8)
_cell_length_c                   13.6877(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2604.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9401
_cell_measurement_theta_min      2.6294
_cell_measurement_theta_max      31.4274

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.625
_exptl_crystal_F_000             1888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    7.632
_shelx_estimated_absorpt_T_min   0.273
_shelx_estimated_absorpt_T_max   0.803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_process_details   'SADABS 2016/2 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source beamline 12.2.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTONII detector'
_diffrn_measurement_method       'ω/θ shutterless scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            70439
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.629
_diffrn_reflns_theta_max         31.427
_diffrn_reflns_theta_full        25.930
_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             3992
_reflns_number_gt                3796
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40a'
_computing_data_reduction        'Bruker SAINT v8.40a'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;
 All non-hydrogen atoms were refined anisotropically. Hydrogen
 atoms were found were placed geometrically
 constrained and refined using a riding model. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0172P)²+4.4456P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Dual space'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3992
_refine_ls_number_parameters     146
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0199
_refine_ls_R_factor_gt           0.0184
_refine_ls_wR_factor_ref         0.0453
_refine_ls_wR_factor_gt          0.0446
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.47129(3) 0.250000 0.750000 0.01807(8) Uani 1 2 d S T P . .
Cu2 Cu 0.49499(2) 0.42169(2) 0.56488(2) 0.01665(6) Uani 1 1 d . . . . .
I1 I 0.57325(2) 0.40931(2) 0.74009(2) 0.01677(4) Uani 1 1 d . . . . .
I2 I 0.62491(2) 0.43187(2) 0.42856(2) 0.01552(4) Uani 1 1 d . . . . .
N1 N 0.38301(13) 0.24933(13) 0.62985(13) 0.0162(3) Uani 1 1 d . . . . .
N2 N 0.39895(13) 0.30485(13) 0.55482(12) 0.0140(3) Uani 1 1 d . . . . .
N3 N 0.32700(12) 0.28997(13) 0.48824(12) 0.0139(3) Uani 1 1 d . . . . .
C1 C 0.29868(15) 0.19761(15) 0.61384(15) 0.0160(4) Uani 1 1 d . . . . .
C2 C 0.24803(17) 0.13370(17) 0.67437(16) 0.0217(4) Uani 1 1 d . . . . .
H2A H 0.272156 0.116263 0.736997 0.026 Uiso 1 1 calc R U . . .
C3 C 0.16183(19) 0.09751(18) 0.63871(19) 0.0254(5) Uani 1 1 d . . . . .
H3A H 0.124996 0.054275 0.677815 0.030 Uiso 1 1 calc R U . . .
C4 C 0.12635(18) 0.12299(18) 0.54503(19) 0.0248(5) Uani 1 1 d . . . . .
H4A H 0.066795 0.095322 0.522872 0.030 Uiso 1 1 calc R U . . .
C5 C 0.17473(16) 0.18617(17) 0.48497(16) 0.0204(4) Uani 1 1 d . . . . .
H5A H 0.150482 0.203357 0.422312 0.024 Uiso 1 1 calc R U . . .
C6 C 0.26210(15) 0.22348(15) 0.52231(14) 0.0153(4) Uani 1 1 d . . . . .
C7 C 0.32135(15) 0.34703(15) 0.40032(14) 0.0150(4) Uani 1 1 d . . . . .
H7A H 0.361997 0.405371 0.408076 0.018 Uiso 1 1 calc R U . . .
H7B H 0.252803 0.367563 0.389667 0.018 Uiso 1 1 calc R U . . .
N4 N 0.35523(12) 0.29275(13) 0.31548(12) 0.0149(3) Uani 1 1 d . . . . .
C8 C 0.45175(18) 0.2771(3) 0.2906(2) 0.0401(8) Uani 1 1 d . . . . .
H8A H 0.507663 0.300242 0.324464 0.048 Uiso 1 1 calc R U . . .
C9 C 0.2983(2) 0.250000 0.250000 0.0141(5) Uani 1 2 d S T P . .
H9A H 0.228757 0.250001 0.250001 0.017 Uiso 1 2 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.0395(18) 4_556 ?
Cu1 N1 2.0395(18) . ?
Cu1 I1 2.6234(3) 4_556 ?
Cu1 I1 2.6235(3) . ?
Cu2 N2 2.0950(18) . ?
Cu2 I2 2.5792(3) . ?
Cu2 I2 2.6176(3) 5_666 ?
Cu2 I1 2.6315(3) . ?
Cu2 Cu2 2.8165(5) 5_666 ?
N1 N2 1.304(2) . ?
N1 C1 1.376(3) . ?
N2 N3 1.356(2) . ?
N3 C6 1.364(3) . ?
N3 C7 1.444(3) . ?
C1 C6 1.396(3) . ?
C1 C2 1.399(3) . ?
C2 C3 1.371(3) . ?
C2 H2A 0.9500 . ?
C3 C4 1.416(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.374(3) . ?
C4 H4A 0.9500 . ?
C5 C6 1.399(3) . ?
C5 H5A 0.9500 . ?
C7 N4 1.461(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N4 C9 1.328(2) . ?
N4 C8 1.379(3) . ?
C8 C8 1.343(5) 4 ?
C8 H8A 0.9500 . ?
C9 H9A 0.9500 . ?

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 Cu1 N1 107.49(10) 4_556 . ?
N1 Cu1 I1 106.03(5) 4_556 4_556 ?
N1 Cu1 I1 110.60(5) . 4_556 ?
N1 Cu1 I1 110.60(5) 4_556 . ?
N1 Cu1 I1 106.03(5) . . ?
I1 Cu1 I1 115.856(16) 4_556 . ?
N2 Cu2 I2 115.23(5) . . ?
N2 Cu2 I2 102.45(5) . 5_666 ?
I2 Cu2 I2 114.371(11) . 5_666 ?
N2 Cu2 I1 105.28(5) . . ?
I2 Cu2 I1 112.533(11) . . ?
I2 Cu2 I1 105.908(11) 5_666 . ?
N2 Cu2 Cu2 126.21(5) . 5_666 ?
I2 Cu2 Cu2 57.843(10) . 5_666 ?
I2 Cu2 Cu2 56.528(10) 5_666 5_666 ?
I1 Cu2 Cu2 127.278(16) . 5_666 ?
Cu1 I1 Cu2 83.498(8) . . ?
Cu2 I2 Cu2 65.629(11) . 5_666 ?
N2 N1 C1 108.95(17) . . ?
N2 N1 Cu1 122.25(14) . . ?
C1 N1 Cu1 128.75(14) . . ?
N1 N2 N3 108.51(16) . . ?
N1 N2 Cu2 120.90(14) . . ?
N3 N2 Cu2 128.08(13) . . ?
N2 N3 C6 110.19(16) . . ?
N2 N3 C7 120.97(17) . . ?
C6 N3 C7 128.57(17) . . ?
N1 C1 C6 107.91(18) . . ?
N1 C1 C2 130.7(2) . . ?
C6 C1 C2 121.2(2) . . ?
C3 C2 C1 116.6(2) . . ?
C3 C2 H2A 121.7 . . ?
C1 C2 H2A 121.7 . . ?
C2 C3 C4 121.6(2) . . ?
C2 C3 H3A 119.2 . . ?
C4 C3 H3A 119.2 . . ?
C5 C4 C3 122.5(2) . . ?
C5 C4 H4A 118.7 . . ?
C3 C4 H4A 118.7 . . ?
C4 C5 C6 115.5(2) . . ?
C4 C5 H5A 122.3 . . ?
C6 C5 H5A 122.3 . . ?
N3 C6 C1 104.43(17) . . ?
N3 C6 C5 133.00(19) . . ?
C1 C6 C5 122.5(2) . . ?
N3 C7 N4 111.14(17) . . ?
N3 C7 H7A 109.4 . . ?
N4 C7 H7A 109.4 . . ?
N3 C7 H7B 109.4 . . ?
N4 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C9 N4 C8 108.81(19) . . ?
C9 N4 C7 125.65(18) . . ?
C8 N4 C7 125.53(18) . . ?
C8 C8 N4 107.05(12) 4 . ?
C8 C8 H8A 126.5 4 . ?
N4 C8 H8A 126.5 . . ?
N4 C9 N4 108.3(2) . 4 ?
N4 C9 H9A 125.9 . . ?
N4 C9 H9A 125.9 4 . ?

_refine_diff_density_max         0.791
_refine_diff_density_min         -0.933
_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_xZH3-128f_a
_database_code_depnum_ccdc_archive 'CCDC 2227209'
loop_
_audit_author_name
_audit_author_address
'Simon J. Teat'
;Advanced Light Source, Lawrence Berkeley National Laboratory
United States of America
;
_audit_update_record             
;
2022-12-17 deposited with the CCDC.	2023-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H17 Cu3 I4 N8'
_chemical_formula_weight         1043.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
H H 0.0000 0.0000
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
N N 0.0065 0.0035
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
Cu Cu 0.3203 1.3289
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
I I -0.3993 1.9038
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'

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

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

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

_cell_length_a                   10.3623(3)
_cell_length_b                   17.4990(6)
_cell_length_c                   14.4300(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.578(2)
_cell_angle_gamma                90
_cell_volume                     2553.79(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9611
_cell_measurement_theta_min      2.5602
_cell_measurement_theta_max      31.3982

_exptl_crystal_description       block
_exptl_crystal_colour            Tan
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.714
_exptl_crystal_F_000             1920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    7.786
_shelx_estimated_absorpt_T_min   0.481
_shelx_estimated_absorpt_T_max   0.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.560
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_process_details   'SADABS 2016/2 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source beamline 12.2.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTONII detector'
_diffrn_measurement_method       'ω/θ shutterless scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            90192
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.385
_diffrn_reflns_theta_max         31.420
_diffrn_reflns_theta_full        25.930
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7822
_reflns_number_gt                7154
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40a'
_computing_data_reduction        'Bruker SAINT v8.40a'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;
 All non-hydrogen atoms were refined anisotropically. Hydrogen
 atoms were found in the fourier difference map constrained were
 refined using a riding model. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0141P)²+3.5358P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Dual space'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7822
_refine_ls_number_parameters     299
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0178
_refine_ls_wR_factor_ref         0.0400
_refine_ls_wR_factor_gt          0.0389
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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
I1 I 0.15300(2) 0.30403(2) 0.90212(2) 0.01558(3) Uani 1 1 d . . . . .
Cu1 Cu 0.36157(3) 0.23114(2) 0.99827(2) 0.01740(5) Uani 1 1 d . . . . .
N1 N 0.52338(18) 0.30047(10) 1.01366(13) 0.0158(3) Uani 1 1 d . . . . .
C1 C 0.5485(2) 0.37011(12) 1.05852(14) 0.0144(4) Uani 1 1 d . . . . .
I2 I 0.41788(2) 0.11534(2) 0.89763(2) 0.01616(3) Uani 1 1 d . . . . .
Cu2 Cu 0.26621(3) 0.21624(2) 0.79031(2) 0.01944(6) Uani 1 1 d . . . . .
N2 N 0.62219(17) 0.28199(11) 0.97577(13) 0.0158(3) Uani 1 1 d . . . . .
C2 C 0.4740(2) 0.41246(13) 1.11012(16) 0.0196(4) Uani 1 1 d . . . . .
H2A H 0.391477 0.394770 1.120265 0.023 Uiso 1 1 calc R U . . .
I3 I 0.37354(2) 0.31006(2) 0.68014(2) 0.01518(3) Uani 1 1 d . . . . .
Cu3 Cu 0.15083(3) 0.25849(2) 0.57269(2) 0.01689(5) Uani 1 1 d . . . . .
N3 N 0.71361(17) 0.33831(10) 0.99555(12) 0.0144(3) Uani 1 1 d . . . . .
C3 C 0.5271(2) 0.48122(14) 1.14531(17) 0.0222(5) Uani 1 1 d . . . . .
H3A H 0.479804 0.511832 1.181030 0.027 Uiso 1 1 calc R U . . .
I4 I 0.08117(2) 0.14309(2) 0.66921(2) 0.01699(3) Uani 1 1 d . . . . .
N4 N 0.80048(17) 0.36933(10) 0.86046(12) 0.0137(3) Uani 1 1 d . . . . .
C4 C 0.6494(2) 0.50800(14) 1.13028(16) 0.0219(5) Uani 1 1 d . . . . .
H4A H 0.680166 0.556804 1.154234 0.026 Uiso 1 1 calc R U . . .
N5 N 0.73675(17) 0.38957(10) 0.71114(12) 0.0140(3) Uani 1 1 d . . . . .
C5 C 0.7256(2) 0.46564(13) 1.08200(15) 0.0189(4) Uani 1 1 d . . . . .
H5A H 0.809154 0.482795 1.073420 0.023 Uiso 1 1 calc R U . . .
N6 N 0.80654(18) 0.37597(11) 0.56607(13) 0.0159(3) Uani 1 1 d . . . . .
C6 C 0.6712(2) 0.39556(12) 1.04646(14) 0.0152(4) Uani 1 1 d . . . . .
N7 N 0.90244(18) 0.32459(11) 0.59881(13) 0.0174(4) Uani 1 1 d . . . . .
C7 C 0.8277(2) 0.33338(13) 0.95385(15) 0.0159(4) Uani 1 1 d . . . . .
H7A H 0.851263 0.279057 0.947825 0.019 Uiso 1 1 calc R U . . .
H7B H 0.903716 0.359088 0.995644 0.019 Uiso 1 1 calc R U . . .
N8 N 0.99148(18) 0.32988(10) 0.54790(13) 0.0155(3) Uani 1 1 d . . . . .
C8 C 0.75743(19) 0.33407(12) 0.77686(14) 0.0139(4) Uani 1 1 d . . . . .
C9 C 0.7427(2) 0.25067(13) 0.76178(17) 0.0209(4) Uani 1 1 d . . . . .
H9A H 0.684551 0.240701 0.699718 0.031 Uiso 1 1 calc R U . . .
H9B H 0.704154 0.228190 0.811781 0.031 Uiso 1 1 calc R U . . .
H9C H 0.829630 0.227826 0.763835 0.031 Uiso 1 1 calc R U . . .
C10 C 0.8093(2) 0.44738(12) 0.84695(15) 0.0170(4) Uani 1 1 d . . . . .
H10A H 0.837782 0.484814 0.894699 0.020 Uiso 1 1 calc R U . . .
C11 C 0.7698(2) 0.45979(12) 0.75343(15) 0.0163(4) Uani 1 1 d . . . . .
H11A H 0.765346 0.507792 0.722131 0.020 Uiso 1 1 calc R U . . .
C12 C 0.6930(2) 0.37959(13) 0.60905(14) 0.0171(4) Uani 1 1 d . . . . .
H12A H 0.640932 0.331891 0.595488 0.020 Uiso 1 1 calc R U . . .
H12B H 0.635642 0.422889 0.581826 0.020 Uiso 1 1 calc R U . . .
C13 C 0.8323(2) 0.41568(12) 0.49055(15) 0.0155(4) Uani 1 1 d . . . . .
C14 C 0.7674(2) 0.47432(13) 0.43352(15) 0.0182(4) Uani 1 1 d . . . . .
H14A H 0.686019 0.495058 0.441972 0.022 Uiso 1 1 calc R U . . .
C15 C 0.8288(2) 0.50011(13) 0.36440(16) 0.0212(4) Uani 1 1 d . . . . .
H15A H 0.789198 0.540529 0.324111 0.025 Uiso 1 1 calc R U . . .
C16 C 0.9489(2) 0.46858(13) 0.35108(16) 0.0209(4) Uani 1 1 d . . . . .
H16A H 0.986536 0.487803 0.301310 0.025 Uiso 1 1 calc R U . . .
C17 C 1.0132(2) 0.41111(13) 0.40762(16) 0.0185(4) Uani 1 1 d . . . . .
H17A H 1.094344 0.390336 0.398705 0.022 Uiso 1 1 calc R U . . .
C18 C 0.9524(2) 0.38492(12) 0.47906(15) 0.0153(4) 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
I1 Cu1 2.6300(3) . ?
I1 Cu2 2.6765(3) . ?
I1 Cu3 2.6982(3) 4_566 ?
Cu1 N1 2.0421(18) . ?
Cu1 I2 2.6314(3) . ?
Cu1 Cu3 2.6414(4) 4_566 ?
Cu1 I3 2.6983(3) 4_566 ?
Cu1 Cu2 2.9593(4) . ?
N1 N2 1.302(2) . ?
N1 C1 1.378(3) . ?
C1 C6 1.393(3) . ?
C1 C2 1.397(3) . ?
I2 Cu2 2.6317(3) . ?
Cu2 I4 2.6286(3) . ?
Cu2 I3 2.6888(3) . ?
N2 N3 1.354(2) . ?
C2 C3 1.373(3) . ?
C2 H2A 0.9500 . ?
I3 Cu3 2.6431(3) . ?
Cu3 N8 2.0390(18) 1_455 ?
Cu3 I4 2.6413(3) . ?
N3 C6 1.370(3) . ?
N3 C7 1.441(3) . ?
C3 C4 1.412(3) . ?
C3 H3A 0.9500 . ?
N4 C8 1.342(3) . ?
N4 C10 1.385(3) . ?
N4 C7 1.458(3) . ?
C4 C5 1.377(3) . ?
C4 H4A 0.9500 . ?
N5 C8 1.342(3) . ?
N5 C11 1.381(3) . ?
N5 C12 1.455(3) . ?
C5 C6 1.400(3) . ?
C5 H5A 0.9500 . ?
N6 N7 1.347(2) . ?
N6 C13 1.367(3) . ?
N6 C12 1.446(3) . ?
N7 N8 1.302(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
N8 C18 1.379(3) . ?
C8 C9 1.479(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.340(3) . ?
C10 H10A 0.9500 . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.393(3) . ?
C13 C18 1.399(3) . ?
C14 C15 1.371(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.413(3) . ?
C15 H15A 0.9500 . ?
C16 C17 1.373(3) . ?
C16 H16A 0.9500 . ?
C17 C18 1.397(3) . ?
C17 H17A 0.9500 . ?

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
Cu1 I1 Cu2 67.784(9) . . ?
Cu1 I1 Cu3 59.419(9) . 4_566 ?
Cu2 I1 Cu3 114.140(10) . 4_566 ?
N1 Cu1 I1 109.28(5) . . ?
N1 Cu1 I2 104.01(5) . . ?
I1 Cu1 I2 109.746(11) . . ?
N1 Cu1 Cu3 130.31(5) . 4_566 ?
I1 Cu1 Cu3 61.575(9) . 4_566 ?
I2 Cu1 Cu3 125.422(12) . 4_566 ?
N1 Cu1 I3 100.96(5) . 4_566 ?
I1 Cu1 I3 120.073(11) . 4_566 ?
I2 Cu1 I3 111.239(11) . 4_566 ?
Cu3 Cu1 I3 59.325(9) 4_566 4_566 ?
N1 Cu1 Cu2 104.33(5) . . ?
I1 Cu1 Cu2 56.854(8) . . ?
I2 Cu1 Cu2 55.791(8) . . ?
Cu3 Cu1 Cu2 107.175(13) 4_566 . ?
I3 Cu1 Cu2 153.790(12) 4_566 . ?
N2 N1 C1 109.35(17) . . ?
N2 N1 Cu1 120.59(14) . . ?
C1 N1 Cu1 130.03(14) . . ?
N1 C1 C6 107.96(18) . . ?
N1 C1 C2 130.5(2) . . ?
C6 C1 C2 121.5(2) . . ?
Cu1 I2 Cu2 68.427(9) . . ?
I4 Cu2 I2 108.674(11) . . ?
I4 Cu2 I1 109.161(11) . . ?
I2 Cu2 I1 108.323(11) . . ?
I4 Cu2 I3 103.887(10) . . ?
I2 Cu2 I3 119.124(11) . . ?
I1 Cu2 I3 107.334(11) . . ?
I4 Cu2 Cu1 138.692(12) . . ?
I2 Cu2 Cu1 55.783(8) . . ?
I1 Cu2 Cu1 55.362(8) . . ?
I3 Cu2 Cu1 117.128(12) . . ?
N1 N2 N3 108.00(17) . . ?
C3 C2 C1 116.0(2) . . ?
C3 C2 H2A 122.0 . . ?
C1 C2 H2A 122.0 . . ?
Cu3 I3 Cu2 73.599(9) . . ?
Cu3 I3 Cu1 59.263(9) . 4_565 ?
Cu2 I3 Cu1 118.333(10) . 4_565 ?
N8 Cu3 I4 104.90(5) 1_455 . ?
N8 Cu3 Cu1 126.60(5) 1_455 4_565 ?
I4 Cu3 Cu1 127.731(12) . 4_565 ?
N8 Cu3 I3 117.65(5) 1_455 . ?
I4 Cu3 I3 104.813(10) . . ?
Cu1 Cu3 I3 61.411(9) 4_565 . ?
N8 Cu3 I1 104.81(5) 1_455 4_565 ?
I4 Cu3 I1 103.209(10) . 4_565 ?
Cu1 Cu3 I1 59.007(9) 4_565 4_565 ?
I3 Cu3 I1 119.598(11) . 4_565 ?
N2 N3 C6 110.71(17) . . ?
N2 N3 C7 117.93(17) . . ?
C6 N3 C7 130.99(18) . . ?
C2 C3 C4 122.3(2) . . ?
C2 C3 H3A 118.8 . . ?
C4 C3 H3A 118.8 . . ?
Cu2 I4 Cu3 74.616(10) . . ?
C8 N4 C10 110.24(18) . . ?
C8 N4 C7 126.30(18) . . ?
C10 N4 C7 123.37(18) . . ?
C5 C4 C3 122.1(2) . . ?
C5 C4 H4A 118.9 . . ?
C3 C4 H4A 118.9 . . ?
C8 N5 C11 110.22(17) . . ?
C8 N5 C12 126.55(19) . . ?
C11 N5 C12 123.15(18) . . ?
C4 C5 C6 115.3(2) . . ?
C4 C5 H5A 122.3 . . ?
C6 C5 H5A 122.3 . . ?
N7 N6 C13 111.20(17) . . ?
N7 N6 C12 119.07(18) . . ?
C13 N6 C12 129.65(18) . . ?
N3 C6 C1 103.97(18) . . ?
N3 C6 C5 133.3(2) . . ?
C1 C6 C5 122.7(2) . . ?
N8 N7 N6 108.30(17) . . ?
N3 C7 N4 110.43(17) . . ?
N3 C7 H7A 109.6 . . ?
N4 C7 H7A 109.6 . . ?
N3 C7 H7B 109.6 . . ?
N4 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
N7 N8 C18 108.84(17) . . ?
N7 N8 Cu3 120.25(14) . 1_655 ?
C18 N8 Cu3 130.81(14) . 1_655 ?
N5 C8 N4 105.86(18) . . ?
N5 C8 C9 127.96(19) . . ?
N4 C8 C9 126.13(19) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 N4 106.65(19) . . ?
C11 C10 H10A 126.7 . . ?
N4 C10 H10A 126.7 . . ?
C10 C11 N5 107.01(19) . . ?
C10 C11 H11A 126.5 . . ?
N5 C11 H11A 126.5 . . ?
N6 C12 N5 109.66(17) . . ?
N6 C12 H12A 109.7 . . ?
N5 C12 H12A 109.7 . . ?
N6 C12 H12B 109.7 . . ?
N5 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
N6 C13 C14 133.8(2) . . ?
N6 C13 C18 103.43(18) . . ?
C14 C13 C18 122.7(2) . . ?
C15 C14 C13 115.6(2) . . ?
C15 C14 H14A 122.2 . . ?
C13 C14 H14A 122.2 . . ?
C14 C15 C16 122.2(2) . . ?
C14 C15 H15A 118.9 . . ?
C16 C15 H15A 118.9 . . ?
C17 C16 C15 122.2(2) . . ?
C17 C16 H16A 118.9 . . ?
C15 C16 H16A 118.9 . . ?
C16 C17 C18 116.1(2) . . ?
C16 C17 H17A 121.9 . . ?
C18 C17 H17A 121.9 . . ?
N8 C18 C17 130.6(2) . . ?
N8 C18 C13 108.22(18) . . ?
C17 C18 C13 121.1(2) . . ?

_refine_diff_density_max         2.087
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.115



####################################################################### 
# 
# 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_XZH4-48d_a
_database_code_depnum_ccdc_archive 'CCDC 2227208'
loop_
_audit_author_name
_audit_author_address
'Simon J. Teat'
;Advanced Light Source, Lawrence Berkeley National Laboratory
United States of America
;
_audit_update_record             
;
2022-12-17 deposited with the CCDC.	2023-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H17.25 Cu2 I3 N8 O0.12'
_chemical_formula_weight         855.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
H H 0.0000 0.0000
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
N N 0.0065 0.0035
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
O O 0.0115 0.0064
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
Cu Cu 0.3203 1.3289
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
I I -0.3993 1.9038
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'

_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                   12.9449(13)
_cell_length_b                   13.5810(13)
_cell_length_c                   13.8160(13)
_cell_angle_alpha                90
_cell_angle_beta                 91.192(4)
_cell_angle_gamma                90
_cell_volume                     2428.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9425
_cell_measurement_theta_min      2.7125
_cell_measurement_theta_max      37.4116

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.340
_exptl_crystal_F_000             1597
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    5.929
_shelx_estimated_absorpt_T_min   0.891
_shelx_estimated_absorpt_T_max   0.943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_process_details   'SADABS 2016/2 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source beamline 12.2.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTONII detector'
_diffrn_measurement_method       'ω/θ shutterless scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            110299
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.188
_diffrn_reflns_theta_max         37.501
_diffrn_reflns_theta_full        25.930
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11805
_reflns_number_gt                10453
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40a'
_computing_data_reduction        'Bruker SAINT v8.40a'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;
 All non-hydrogen atoms were refined anisotropically. Hydrogen
 atoms were placed geometrically on the carbon atoms, constrained and
 refined using a riding model. An isolated electron density peak was
 refined as water, the hydrogens of which could neither be found nor
 placed and where therefore omitted from the refinement but not the
 chemical formula.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0125P)²+2.2808P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Dual space'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11805
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0493
_refine_ls_wR_factor_gt          0.0478
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.48810(2) 0.23394(2) 0.76102(2) 0.01789(4) Uani 1 1 d . . . . .
Cu2 Cu 0.51678(2) 0.42254(2) -0.05888(2) 0.01474(4) Uani 1 1 d . . . . .
I1 I 0.60356(2) 0.07969(2) 0.74698(2) 0.02092(3) Uani 1 1 d . . . . .
I2 I 0.65041(2) 0.46195(2) 0.07782(2) 0.01389(3) Uani 0.9584(5) 1 d . . P A 1
I2' I 0.6728(2) 0.4935(3) 0.0558(2) 0.01389(3) Uani 0.0416(5) 1 d . . P A 2
I3 I 0.58264(2) 0.40991(2) -0.23452(2) 0.01484(2) Uani 1 1 d . . . . .
N1 N 0.39909(12) 0.23840(12) 0.63780(10) 0.0176(3) Uani 1 1 d . . . . .
N2 N 0.41515(11) 0.17974(12) 0.56499(10) 0.0169(3) Uani 1 1 d . . . . .
N3 N 0.34164(11) 0.19799(11) 0.49624(10) 0.0150(2) Uani 1 1 d . . . . .
C1 C 0.31356(13) 0.29569(13) 0.61753(12) 0.0162(3) Uani 1 1 d . . . . .
C2 C 0.26397(15) 0.36748(14) 0.67312(13) 0.0199(3) Uani 1 1 d . . . . .
H2A H 0.289910 0.386642 0.735133 0.024 Uiso 1 1 calc R U . . .
C3 C 0.17568(16) 0.40869(14) 0.63297(15) 0.0231(4) Uani 1 1 d . . . . .
H3A H 0.139901 0.457483 0.668383 0.028 Uiso 1 1 calc R U . . .
C4 C 0.13672(16) 0.38049(15) 0.54056(15) 0.0247(4) Uani 1 1 d . . . . .
H4A H 0.075406 0.410673 0.515941 0.030 Uiso 1 1 calc R U . . .
C5 C 0.18529(15) 0.31035(15) 0.48511(13) 0.0214(3) Uani 1 1 d . . . . .
H5A H 0.159330 0.291180 0.423112 0.026 Uiso 1 1 calc R U . . .
C6 C 0.27495(13) 0.26948(13) 0.52610(12) 0.0155(3) Uani 1 1 d . . . . .
C7 C 0.33688(13) 0.13710(13) 0.41050(11) 0.0151(3) Uani 1 1 d . . . . .
H7A H 0.263914 0.120470 0.395097 0.018 Uiso 1 1 calc R U . . .
H7B H 0.374631 0.074874 0.423182 0.018 Uiso 1 1 calc R U . . .
N4 N 0.38183(11) 0.18694(11) 0.32763(10) 0.0144(2) Uani 1 1 d . . . . .
C8 C 0.32669(13) 0.23877(13) 0.26265(11) 0.0153(3) Uani 1 1 d . . . . .
H8A H 0.253962 0.248181 0.262292 0.018 Uiso 1 1 calc R U . . .
N5 N 0.39187(11) 0.27478(11) 0.19863(10) 0.0146(2) Uani 1 1 d . . . . .
C9 C 0.49177(14) 0.24531(14) 0.22356(13) 0.0176(3) Uani 1 1 d . . . . .
H9A H 0.552837 0.261303 0.189989 0.021 Uiso 1 1 calc R U . . .
C10 C 0.48593(13) 0.18937(14) 0.30486(12) 0.0167(3) Uani 1 1 d . . . . .
C11 C 0.56689(14) 0.13566(15) 0.36286(13) 0.0214(3) Uani 1 1 d . . . . .
H11A H 0.558824 0.150342 0.431734 0.032 Uiso 1 1 calc R U . . .
H11B H 0.635518 0.156796 0.342590 0.032 Uiso 1 1 calc R U . . .
H11C H 0.559364 0.064651 0.352237 0.032 Uiso 1 1 calc R U . . .
C12 C 0.36110(14) 0.33750(13) 0.11673(11) 0.0157(3) Uani 1 1 d . . . . .
H12A H 0.293091 0.367583 0.129590 0.019 Uiso 1 1 calc R U . . .
H12B H 0.412019 0.391342 0.110115 0.019 Uiso 1 1 calc R U . . .
N6 N 0.35452(11) 0.28243(11) 0.02707(10) 0.0141(2) Uani 1 1 d . . . . .
N7 N 0.42874(11) 0.29189(11) -0.04021(10) 0.0136(2) Uani 1 1 d . . . . .
N8 N 0.40153(11) 0.24070(10) -0.11682(10) 0.0139(2) Uani 1 1 d . . . . .
C13 C 0.27594(13) 0.22448(13) -0.00813(12) 0.0149(3) Uani 1 1 d . . . . .
C14 C 0.18159(14) 0.19429(14) 0.02998(13) 0.0202(3) Uani 1 1 d . . . . .
H14A H 0.160636 0.212865 0.092895 0.024 Uiso 1 1 calc R U . . .
C15 C 0.12118(15) 0.13577(15) -0.03003(14) 0.0228(4) Uani 1 1 d . . . . .
H15A H 0.056942 0.112480 -0.007128 0.027 Uiso 1 1 calc R U . . .
C16 C 0.15121(15) 0.10911(14) -0.12434(14) 0.0216(3) Uani 1 1 d . . . . .
H16A H 0.106416 0.069226 -0.163029 0.026 Uiso 1 1 calc R U . . .
C17 C 0.24374(14) 0.13956(13) -0.16139(13) 0.0180(3) Uani 1 1 d . . . . .
H17A H 0.263755 0.122105 -0.224892 0.022 Uiso 1 1 calc R U . . .
C18 C 0.30714(13) 0.19773(12) -0.10068(11) 0.0140(3) Uani 1 1 d . . . . .
O1W O -0.1269(13) 0.0907(12) -0.1044(12) 0.044(4) Uiso 0.125 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 2.0368(15) . ?
Cu1 N8 2.0472(14) 1_556 ?
Cu1 I1 2.5831(3) . ?
Cu1 I3 2.6851(3) 1_556 ?
Cu2 N7 2.1274(14) . ?
Cu2 I2 2.5902(3) . ?
Cu2 I3 2.5945(3) . ?
Cu2 I2 2.6814(3) 3_665 ?
Cu2 Cu2 2.7004(5) 3_665 ?
Cu2 I2' 2.708(3) 3_665 ?
Cu2 I2' 2.717(3) . ?
N1 N2 1.303(2) . ?
N1 C1 1.377(2) . ?
N2 N3 1.353(2) . ?
N3 C6 1.368(2) . ?
N3 C7 1.445(2) . ?
C1 C6 1.395(2) . ?
C1 C2 1.405(3) . ?
C2 C3 1.379(3) . ?
C3 C4 1.416(3) . ?
C4 C5 1.382(3) . ?
C5 C6 1.396(3) . ?
C7 N4 1.461(2) . ?
N4 C8 1.336(2) . ?
N4 C10 1.391(2) . ?
C8 N5 1.328(2) . ?
N5 C9 1.390(2) . ?
N5 C12 1.465(2) . ?
C9 C10 1.359(2) . ?
C10 C11 1.496(3) . ?
C12 N6 1.448(2) . ?
N6 N7 1.3567(19) . ?
N6 C13 1.368(2) . ?
N7 N8 1.3085(19) . ?
N8 C18 1.376(2) . ?
C13 C18 1.397(2) . ?
C13 C14 1.401(2) . ?
C14 C15 1.380(3) . ?
C15 C16 1.415(3) . ?
C16 C17 1.376(3) . ?
C17 C18 1.404(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N8 112.20(6) . 1_556 ?
N1 Cu1 I1 106.23(5) . . ?
N8 Cu1 I1 115.20(4) 1_556 . ?
N1 Cu1 I3 104.03(5) . 1_556 ?
N8 Cu1 I3 101.43(4) 1_556 1_556 ?
I1 Cu1 I3 117.346(11) . 1_556 ?
N7 Cu2 I2 115.80(4) . . ?
N7 Cu2 I3 104.22(4) . . ?
I2 Cu2 I3 117.916(11) . . ?
N7 Cu2 I2 93.81(4) . 3_665 ?
I2 Cu2 I2 118.402(9) . 3_665 ?
I3 Cu2 I2 103.158(9) . 3_665 ?
N7 Cu2 Cu2 118.91(4) . 3_665 ?
I2 Cu2 Cu2 60.864(9) . 3_665 ?
I3 Cu2 Cu2 132.463(13) . 3_665 ?
I2 Cu2 Cu2 57.539(9) 3_665 3_665 ?
N7 Cu2 I2' 82.03(10) . 3_665 ?
I2 Cu2 I2' 119.55(6) . 3_665 ?
I3 Cu2 I2' 110.99(7) . 3_665 ?
I2 Cu2 I2' 12.84(9) 3_665 3_665 ?
Cu2 Cu2 I2' 60.33(6) 3_665 3_665 ?
N7 Cu2 I2' 128.22(9) . . ?
I3 Cu2 I2' 108.29(8) . . ?
Cu2 Cu2 I2' 59.97(6) 3_665 . ?
I2' Cu2 I2' 120.30(6) 3_665 . ?
Cu2 I2 Cu2 61.599(9) . 3_665 ?
Cu2 I2' Cu2 59.71(6) 3_665 . ?
Cu2 I3 Cu1 85.513(8) . 1_554 ?
N2 N1 C1 109.21(14) . . ?
N2 N1 Cu1 122.03(12) . . ?
C1 N1 Cu1 128.69(12) . . ?
N1 N2 N3 107.97(14) . . ?
N2 N3 C6 110.93(13) . . ?
N2 N3 C7 119.20(14) . . ?
C6 N3 C7 129.55(14) . . ?
N1 C1 C6 108.13(15) . . ?
N1 C1 C2 130.97(16) . . ?
C6 C1 C2 120.87(17) . . ?
C3 C2 C1 116.50(17) . . ?
C2 C3 C4 121.99(18) . . ?
C5 C4 C3 121.92(18) . . ?
C4 C5 C6 115.68(17) . . ?
N3 C6 C1 103.75(15) . . ?
N3 C6 C5 133.18(16) . . ?
C1 C6 C5 123.03(17) . . ?
N3 C7 N4 111.49(13) . . ?
C8 N4 C10 110.02(14) . . ?
C8 N4 C7 123.69(14) . . ?
C10 N4 C7 126.29(14) . . ?
N5 C8 N4 107.67(15) . . ?
C8 N5 C9 109.24(14) . . ?
C8 N5 C12 124.20(15) . . ?
C9 N5 C12 126.55(14) . . ?
C10 C9 N5 107.35(15) . . ?
C9 C10 N4 105.72(15) . . ?
C9 C10 C11 131.66(16) . . ?
N4 C10 C11 122.60(15) . . ?
N6 C12 N5 111.76(14) . . ?
N7 N6 C13 110.06(13) . . ?
N7 N6 C12 120.48(13) . . ?
C13 N6 C12 129.17(14) . . ?
N8 N7 N6 108.75(13) . . ?
N8 N7 Cu2 118.74(11) . . ?
N6 N7 Cu2 123.42(11) . . ?
N7 N8 C18 108.61(13) . . ?
N7 N8 Cu1 123.23(11) . 1_554 ?
C18 N8 Cu1 128.14(11) . 1_554 ?
N6 C13 C18 104.36(14) . . ?
N6 C13 C14 133.03(16) . . ?
C18 C13 C14 122.60(16) . . ?
C15 C14 C13 115.48(17) . . ?
C14 C15 C16 122.53(17) . . ?
C17 C16 C15 121.59(17) . . ?
C16 C17 C18 116.70(16) . . ?
N8 C18 C13 108.22(14) . . ?
N8 C18 C17 130.64(15) . . ?
C13 C18 C17 121.09(16) . . ?

_refine_diff_density_max         1.061
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.186



####################################################################### 
# 
# 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_XZH4-121c_a
_database_code_depnum_ccdc_archive 'CCDC 2227211'
loop_
_audit_author_name
_audit_author_address
'Simon J. Teat'
;Advanced Light Source, Lawrence Berkeley National Laboratory
United States of America
;
_audit_update_record             
;
2022-12-17 deposited with the CCDC.	2023-01-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H46 Cu4 I6 N16'
_chemical_formula_weight         1790.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
H H 0.0000 0.0000
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
N N 0.0065 0.0035
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
Cu Cu 0.3203 1.3289
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'
I I -0.3993 1.9038
'XDISP Program in WinGX S.Brennan & P.L.Cowan Rev.Sci.Instrum.63,850 1992'

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

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

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

_cell_length_a                   8.6527(9)
_cell_length_b                   16.0764(17)
_cell_length_c                   38.106(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.414(4)
_cell_angle_gamma                90
_cell_volume                     5300.6(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9921
_cell_measurement_theta_min      2.5484
_cell_measurement_theta_max      27.9214

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.244
_exptl_crystal_F_000             3376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    5.438
_shelx_estimated_absorpt_T_min   0.702
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_process_details   'SADABS 2016/2 Bruker AXS Madison WI USA'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_source                   'Advanced Light Source beamline 12.2.1'
_diffrn_measurement_device_type  'Bruker D8 with PHOTONII detector'
_diffrn_measurement_method       'ω/θ shutterless scans'
_diffrn_detector_area_resol_mean 7.39
_diffrn_reflns_number            131343
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         1.700
_diffrn_reflns_theta_max         27.950
_diffrn_reflns_theta_full        25.930
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11779
_reflns_number_gt                9923
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40a'
_computing_data_reduction        'Bruker SAINT v8.40a'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_refine_special_details          
;
 All non-hydrogen atoms were refined anisotropically. Hydrogen
 atoms were placed geometrically where possible and methyl
 hydrogen atoms were found in the difference map, all were
 constrained and refined using a riding model.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0216P)²+10.1562P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     'Dual space'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11779
_refine_ls_number_parameters     621
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0276
_refine_ls_wR_factor_ref         0.0661
_refine_ls_wR_factor_gt          0.0625
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.004
_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 0.68455(6) 0.43019(3) 0.56444(2) 0.02652(11) Uani 1 1 d . . . . .
Cu2 Cu 0.50911(5) 0.39412(3) 0.51216(2) 0.02661(11) Uani 1 1 d . . . . .
I1 I 0.48290(3) 0.54371(2) 0.55178(2) 0.01952(6) Uani 1 1 d . . . . .
I2 I 0.78840(3) 0.32860(2) 0.52161(2) 0.02698(7) Uani 1 1 d . . . . .
I3 I 0.27563(3) 0.30511(2) 0.52788(2) 0.02260(6) Uani 1 1 d . . . . .
N1 N 0.6950(4) 0.4275(2) 0.61645(8) 0.0239(7) Uani 1 1 d . . . . .
N2 N 0.7490(4) 0.4867(2) 0.63637(8) 0.0218(7) Uani 1 1 d . . . . .
N3 N 0.7097(4) 0.4678(2) 0.66983(8) 0.0216(7) Uani 1 1 d . . . . .
C1 C 0.6173(4) 0.3697(2) 0.63622(10) 0.0217(8) Uani 1 1 d . . . . .
C2 C 0.5370(5) 0.2975(3) 0.62677(11) 0.0298(9) Uani 1 1 d . . . . .
H2A H 0.531555 0.279968 0.602981 0.036 Uiso 1 1 calc R U . . .
C3 C 0.4664(5) 0.2528(3) 0.65264(12) 0.0297(9) Uani 1 1 d . . . . .
C4 C 0.4762(5) 0.2796(3) 0.68869(12) 0.0296(9) Uani 1 1 d . . . . .
C5 C 0.5559(5) 0.3501(3) 0.69803(11) 0.0276(9) Uani 1 1 d . . . . .
H5A H 0.563649 0.367302 0.721829 0.033 Uiso 1 1 calc R U . . .
C6 C 0.6254(4) 0.3958(2) 0.67110(10) 0.0220(8) Uani 1 1 d . . . . .
C7 C 0.3784(6) 0.1747(3) 0.64353(15) 0.0457(12) Uani 1 1 d . . . . .
H7A H 0.377147 0.167143 0.618006 0.069 Uiso 1 1 calc R U . . .
H7B H 0.272134 0.179381 0.652017 0.069 Uiso 1 1 calc R U . . .
H7C H 0.428757 0.126731 0.654638 0.069 Uiso 1 1 calc R U . . .
C8 C 0.3981(6) 0.2286(3) 0.71642(13) 0.0430(12) Uani 1 1 d . . . . .
H8A H 0.408578 0.256509 0.739173 0.064 Uiso 1 1 calc R U . . .
H8B H 0.446455 0.173543 0.717680 0.064 Uiso 1 1 calc R U . . .
H8C H 0.288294 0.222464 0.710488 0.064 Uiso 1 1 calc R U . . .
C9 C 0.7404(4) 0.5291(2) 0.69689(10) 0.0227(8) Uani 1 1 d . . . . .
H9A H 0.833237 0.561810 0.690703 0.027 Uiso 1 1 calc R U . . .
H9B H 0.760825 0.500726 0.719509 0.027 Uiso 1 1 calc R U . . .
N4 N 0.6077(4) 0.5846(2) 0.70041(8) 0.0207(7) Uani 1 1 d . . . . .
C10 C 0.5924(4) 0.6608(2) 0.68695(10) 0.0208(8) Uani 1 1 d . . . . .
H10A H 0.669354 0.690673 0.674547 0.025 Uiso 1 1 calc R U . . .
N5 N 0.4508(4) 0.68747(19) 0.69391(8) 0.0202(7) Uani 1 1 d . . . . .
C11 C 0.3738(5) 0.6262(3) 0.71238(12) 0.0346(10) Uani 1 1 d . . . . .
H11A H 0.270424 0.628530 0.720544 0.041 Uiso 1 1 calc R U . . .
C12 C 0.4725(5) 0.5633(3) 0.71649(12) 0.0375(11) Uani 1 1 d . . . . .
H12A H 0.452614 0.512661 0.728462 0.045 Uiso 1 1 calc R U . . .
C13 C 0.3799(4) 0.7659(2) 0.68229(10) 0.0219(8) Uani 1 1 d . . . . .
H13A H 0.279899 0.773885 0.694287 0.026 Uiso 1 1 calc R U . . .
H13B H 0.448291 0.813054 0.688546 0.026 Uiso 1 1 calc R U . . .
N6 N 0.3555(3) 0.7641(2) 0.64499(8) 0.0206(7) Uani 1 1 d . . . . .
N7 N 0.2627(4) 0.7041(2) 0.63063(9) 0.0230(7) Uani 1 1 d . . . . .
N8 N 0.2727(4) 0.70716(19) 0.59685(8) 0.0212(7) Uani 1 1 d . . . . .
C14 C 0.4285(4) 0.8079(2) 0.61891(9) 0.0167(7) Uani 1 1 d . . . . .
C15 C 0.5270(4) 0.8762(2) 0.61904(10) 0.0200(8) Uani 1 1 d . . . . .
H15A H 0.558835 0.902205 0.640287 0.024 Uiso 1 1 calc R U . . .
C16 C 0.5766(4) 0.9046(2) 0.58666(11) 0.0214(8) Uani 1 1 d . . . . .
C17 C 0.5296(4) 0.8643(2) 0.55499(10) 0.0200(8) Uani 1 1 d . . . . .
C18 C 0.4289(4) 0.7977(2) 0.55560(10) 0.0209(8) Uani 1 1 d . . . . .
H18A H 0.396766 0.771173 0.534493 0.025 Uiso 1 1 calc R U . . .
C19 C 0.3758(4) 0.7704(2) 0.58807(10) 0.0186(7) Uani 1 1 d . . . . .
C20 C 0.6785(5) 0.9812(2) 0.58514(11) 0.0272(9) Uani 1 1 d . . . . .
H20A H 0.708804 0.997498 0.608996 0.041 Uiso 1 1 calc R U . . .
H20B H 0.621501 1.026828 0.573957 0.041 Uiso 1 1 calc R U . . .
H20C H 0.771241 0.968755 0.571472 0.041 Uiso 1 1 calc R U . . .
C21 C 0.5902(5) 0.8952(3) 0.52040(10) 0.0247(8) Uani 1 1 d . . . . .
H21A H 0.539917 0.864791 0.501188 0.037 Uiso 1 1 calc R U . . .
H21B H 0.702144 0.886275 0.519474 0.037 Uiso 1 1 calc R U . . .
H21C H 0.567993 0.954746 0.518052 0.037 Uiso 1 1 calc R U . . .
Cu3 Cu 0.05089(6) 0.41814(4) 0.75110(2) 0.03820(15) Uani 1 1 d . . . . .
Cu4 Cu 0.05236(5) 0.35939(3) 0.81205(2) 0.02377(11) Uani 1 1 d . . . . .
I4 I 0.30940(3) 0.42938(2) 0.78630(2) 0.02057(6) Uani 1 1 d . . . . .
I5 I -0.17420(3) 0.46163(2) 0.79185(2) 0.02282(6) Uani 1 1 d . . . . .
I6 I 0.02699(3) 0.21425(2) 0.78036(2) 0.02897(7) Uani 1 1 d . . . . .
N9 N 0.0574(4) 0.4100(2) 0.69943(8) 0.0267(8) Uani 1 1 d . . . . .
N10 N 0.1267(4) 0.4662(2) 0.68001(8) 0.0242(7) Uani 1 1 d . . . . .
N11 N 0.1290(3) 0.43648(19) 0.64669(8) 0.0190(6) Uani 1 1 d . . . . .
C22 C 0.0126(4) 0.3440(3) 0.67867(10) 0.0216(8) Uani 1 1 d . . . . .
C23 C -0.0655(5) 0.2698(3) 0.68656(11) 0.0293(9) Uani 1 1 d . . . . .
H23A H -0.098326 0.258557 0.709814 0.035 Uiso 1 1 calc R U . . .
C24 C -0.0933(5) 0.2141(3) 0.66021(12) 0.0284(9) Uani 1 1 d . . . . .
C25 C -0.0436(5) 0.2316(2) 0.62508(11) 0.0261(9) Uani 1 1 d . . . . .
C26 C 0.0313(4) 0.3043(2) 0.61696(10) 0.0217(8) Uani 1 1 d . . . . .
H26A H 0.062614 0.316274 0.593657 0.026 Uiso 1 1 calc R U . . .
C27 C 0.0594(4) 0.3598(2) 0.64442(9) 0.0189(7) Uani 1 1 d . . . . .
C28 C -0.1753(6) 0.1328(3) 0.66805(15) 0.0453(13) Uani 1 1 d . . . . .
H28A H -0.206052 0.131827 0.692748 0.068 Uiso 1 1 calc R U . . .
H28B H -0.105338 0.086189 0.663417 0.068 Uiso 1 1 calc R U . . .
H28C H -0.267293 0.127887 0.653055 0.068 Uiso 1 1 calc R U . . .
C29 C -0.0761(6) 0.1694(3) 0.59646(14) 0.0403(11) Uani 1 1 d . . . . .
H29A H -0.022842 0.186342 0.575008 0.061 Uiso 1 1 calc R U . . .
H29B H -0.187618 0.166851 0.591950 0.061 Uiso 1 1 calc R U . . .
H29C H -0.038909 0.114432 0.603792 0.061 Uiso 1 1 calc R U . . .
C30 C 0.1991(4) 0.4856(2) 0.61917(10) 0.0226(8) Uani 1 1 d . . . . .
H30A H 0.265402 0.449226 0.604706 0.027 Uiso 1 1 calc R U . . .
H30B H 0.265754 0.528808 0.629942 0.027 Uiso 1 1 calc R U . . .
N12 N 0.0838(3) 0.52570(18) 0.59657(8) 0.0181(6) Uani 1 1 d . . . . .
C31 C 0.0031(4) 0.5932(2) 0.60517(10) 0.0183(7) Uani 1 1 d . . . . .
H31A H 0.008882 0.621946 0.626916 0.022 Uiso 1 1 calc R U . . .
N13 N -0.0870(3) 0.61319(18) 0.57804(8) 0.0163(6) Uani 1 1 d . . . . .
C32 C -0.0633(5) 0.5568(2) 0.55109(10) 0.0239(8) Uani 1 1 d . . . . .
H32A H -0.112624 0.556386 0.528735 0.029 Uiso 1 1 calc R U . . .
C33 C 0.0444(4) 0.5022(2) 0.56302(10) 0.0234(8) Uani 1 1 d . . . . .
H33A H 0.085164 0.456207 0.550483 0.028 Uiso 1 1 calc R U . . .
C34 C -0.2002(4) 0.6808(2) 0.57708(10) 0.0201(8) Uani 1 1 d . . . . .
H34A H -0.229630 0.692768 0.552438 0.024 Uiso 1 1 calc R U . . .
H34B H -0.294407 0.663775 0.589802 0.024 Uiso 1 1 calc R U . . .
N14 N -0.1365(3) 0.75452(18) 0.59302(7) 0.0164(6) Uani 1 1 d . . . . .
N15 N -0.1489(3) 0.76498(19) 0.62811(8) 0.0177(6) Uani 1 1 d . . . . .
N16 N -0.0693(3) 0.83083(18) 0.63709(8) 0.0167(6) Uani 1 1 d . . . . .
C35 C -0.0455(4) 0.8149(2) 0.57857(9) 0.0154(7) Uani 1 1 d . . . . .
C36 C 0.0018(4) 0.8314(2) 0.54433(9) 0.0181(7) Uani 1 1 d . . . . .
H36A H -0.027730 0.796520 0.525294 0.022 Uiso 1 1 calc R U . . .
C37 C 0.0933(4) 0.9005(2) 0.53944(9) 0.0172(7) Uani 1 1 d . . . . .
C38 C 0.1382(4) 0.9529(2) 0.56843(10) 0.0177(7) Uani 1 1 d . . . . .
C39 C 0.0907(4) 0.9345(2) 0.60202(10) 0.0180(7) Uani 1 1 d . . . . .
H39A H 0.120532 0.968624 0.621272 0.022 Uiso 1 1 calc R U . . .
C40 C -0.0028(4) 0.8643(2) 0.60710(9) 0.0170(7) Uani 1 1 d . . . . .
C41 C 0.1519(4) 0.9193(3) 0.50315(10) 0.0230(8) Uani 1 1 d . . . . .
H41A H 0.102979 0.881594 0.486212 0.034 Uiso 1 1 calc R U . . .
H41B H 0.264254 0.911690 0.502648 0.034 Uiso 1 1 calc R U . . .
H41C H 0.126692 0.976976 0.496995 0.034 Uiso 1 1 calc R U . . .
C42 C 0.2380(4) 1.0275(2) 0.56197(11) 0.0240(8) Uani 1 1 d . . . . .
H42A H 0.265038 1.053613 0.584437 0.036 Uiso 1 1 calc R U . . .
H42B H 0.181649 1.067483 0.547274 0.036 Uiso 1 1 calc R U . . .
H42C H 0.332569 1.010237 0.549998 0.036 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.984(3) . ?
Cu1 I2 2.4819(6) . ?
Cu1 Cu2 2.5626(7) . ?
Cu1 I1 2.5682(6) . ?
Cu2 I3 2.5505(6) . ?
Cu2 I1 2.6349(6) 3_666 ?
Cu2 I2 2.6584(6) . ?
Cu2 I1 2.8495(6) . ?
N1 N2 1.302(5) . ?
N1 C1 1.375(5) . ?
N2 N3 1.357(4) . ?
N3 C6 1.369(5) . ?
N3 C9 1.449(5) . ?
C1 C6 1.395(5) . ?
C1 C2 1.399(6) . ?
C2 C3 1.367(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.442(6) . ?
C3 C7 1.508(6) . ?
C4 C5 1.373(6) . ?
C4 C8 1.502(6) . ?
C5 C6 1.401(5) . ?
C5 H5A 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.461(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
N4 C10 1.334(5) . ?
N4 C12 1.368(5) . ?
C10 N5 1.326(5) . ?
C10 H10A 0.9500 . ?
N5 C11 1.384(5) . ?
N5 C13 1.469(5) . ?
C11 C12 1.332(6) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
C13 N6 1.436(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
N6 N7 1.367(4) . ?
N6 C14 1.375(5) . ?
N7 N8 1.292(4) . ?
N8 C19 1.395(5) . ?
C14 C15 1.391(5) . ?
C14 C19 1.394(5) . ?
C15 C16 1.387(5) . ?
C15 H15A 0.9500 . ?
C16 C17 1.427(5) . ?
C16 C20 1.516(5) . ?
C17 C18 1.381(5) . ?
C17 C21 1.506(5) . ?
C18 C19 1.394(5) . ?
C18 H18A 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
Cu3 N9 1.975(3) . ?
Cu3 Cu4 2.5071(7) . ?
Cu3 I5 2.5955(6) . ?
Cu3 I4 2.6060(6) . ?
Cu4 N16 1.996(3) 2_546 ?
Cu4 I6 2.6357(6) . ?
Cu4 I5 2.6675(6) . ?
Cu4 I4 2.6846(6) . ?
N9 N10 1.316(5) . ?
N9 C22 1.377(5) . ?
N10 N11 1.357(4) . ?
N11 C27 1.374(5) . ?
N11 C30 1.449(5) . ?
C22 C27 1.393(5) . ?
C22 C23 1.404(6) . ?
C23 C24 1.365(6) . ?
C23 H23A 0.9500 . ?
C24 C25 1.437(6) . ?
C24 C28 1.518(6) . ?
C25 C26 1.373(5) . ?
C25 C29 1.504(6) . ?
C26 C27 1.396(5) . ?
C26 H26A 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 N12 1.462(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
N12 C31 1.332(5) . ?
N12 C33 1.373(5) . ?
C31 N13 1.330(5) . ?
C31 H31A 0.9500 . ?
N13 C32 1.387(5) . ?
N13 C34 1.463(5) . ?
C32 C33 1.356(6) . ?
C32 H32A 0.9500 . ?
C33 H33A 0.9500 . ?
C34 N14 1.439(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
N14 N15 1.353(4) . ?
N14 C35 1.368(4) . ?
N15 N16 1.307(4) . ?
N16 C40 1.392(5) . ?
C35 C40 1.394(5) . ?
C35 C36 1.395(5) . ?
C36 C37 1.379(5) . ?
C36 H36A 0.9500 . ?
C37 C38 1.440(5) . ?
C37 C41 1.507(5) . ?
C38 C39 1.380(5) . ?
C38 C42 1.499(5) . ?
C39 C40 1.403(5) . ?
C39 H39A 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 I2 128.93(10) . . ?
N1 Cu1 Cu2 142.60(10) . . ?
I2 Cu1 Cu2 63.581(18) . . ?
N1 Cu1 I1 103.26(10) . . ?
I2 Cu1 I1 126.35(2) . . ?
Cu2 Cu1 I1 67.472(19) . . ?
I3 Cu2 Cu1 114.21(2) . . ?
I3 Cu2 I1 117.14(2) . 3_666 ?
Cu1 Cu2 I1 127.86(2) . 3_666 ?
I3 Cu2 I2 117.82(2) . . ?
Cu1 Cu2 I2 56.731(16) . . ?
I1 Cu2 I2 104.225(19) 3_666 . ?
I3 Cu2 I1 106.432(19) . . ?
Cu1 Cu2 I1 56.359(16) . . ?
I1 Cu2 I1 99.932(19) 3_666 . ?
I2 Cu2 I1 109.774(19) . . ?
Cu1 I1 Cu2 114.898(18) . 3_666 ?
Cu1 I1 Cu2 56.170(16) . . ?
Cu2 I1 Cu2 80.066(19) 3_666 . ?
Cu1 I2 Cu2 59.688(17) . . ?
N2 N1 C1 110.5(3) . . ?
N2 N1 Cu1 125.4(3) . . ?
C1 N1 Cu1 122.9(3) . . ?
N1 N2 N3 107.0(3) . . ?
N2 N3 C6 111.1(3) . . ?
N2 N3 C9 118.1(3) . . ?
C6 N3 C9 130.1(3) . . ?
N1 C1 C6 107.3(3) . . ?
N1 C1 C2 131.6(4) . . ?
C6 C1 C2 121.1(4) . . ?
C3 C2 C1 118.3(4) . . ?
C3 C2 H2A 120.9 . . ?
C1 C2 H2A 120.9 . . ?
C2 C3 C4 120.4(4) . . ?
C2 C3 C7 119.9(4) . . ?
C4 C3 C7 119.6(4) . . ?
C5 C4 C3 121.3(4) . . ?
C5 C4 C8 119.8(4) . . ?
C3 C4 C8 118.9(4) . . ?
C4 C5 C6 117.4(4) . . ?
C4 C5 H5A 121.3 . . ?
C6 C5 H5A 121.3 . . ?
N3 C6 C1 104.1(3) . . ?
N3 C6 C5 134.5(4) . . ?
C1 C6 C5 121.4(4) . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 N4 109.9(3) . . ?
N3 C9 H9A 109.7 . . ?
N4 C9 H9A 109.7 . . ?
N3 C9 H9B 109.7 . . ?
N4 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
C10 N4 C12 108.6(3) . . ?
C10 N4 C9 127.0(3) . . ?
C12 N4 C9 124.3(3) . . ?
N5 C10 N4 108.0(3) . . ?
N5 C10 H10A 126.0 . . ?
N4 C10 H10A 126.0 . . ?
C10 N5 C11 108.7(3) . . ?
C10 N5 C13 127.0(3) . . ?
C11 N5 C13 124.2(3) . . ?
C12 C11 N5 106.8(4) . . ?
C12 C11 H11A 126.6 . . ?
N5 C11 H11A 126.6 . . ?
C11 C12 N4 107.9(4) . . ?
C11 C12 H12A 126.1 . . ?
N4 C12 H12A 126.1 . . ?
N6 C13 N5 109.9(3) . . ?
N6 C13 H13A 109.7 . . ?
N5 C13 H13A 109.7 . . ?
N6 C13 H13B 109.7 . . ?
N5 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
N7 N6 C14 110.1(3) . . ?
N7 N6 C13 119.5(3) . . ?
C14 N6 C13 129.8(3) . . ?
N8 N7 N6 109.2(3) . . ?
N7 N8 C19 108.3(3) . . ?
N6 C14 C15 133.4(3) . . ?
N6 C14 C19 103.8(3) . . ?
C15 C14 C19 122.7(3) . . ?
C16 C15 C14 116.8(3) . . ?
C16 C15 H15A 121.6 . . ?
C14 C15 H15A 121.6 . . ?
C15 C16 C17 121.0(3) . . ?
C15 C16 C20 119.0(4) . . ?
C17 C16 C20 119.9(3) . . ?
C18 C17 C16 121.0(3) . . ?
C18 C17 C21 119.6(4) . . ?
C16 C17 C21 119.4(3) . . ?
C17 C18 C19 118.1(4) . . ?
C17 C18 H18A 121.0 . . ?
C19 C18 H18A 121.0 . . ?
C18 C19 C14 120.3(3) . . ?
C18 C19 N8 131.1(3) . . ?
C14 C19 N8 108.6(3) . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N9 Cu3 Cu4 153.98(11) . . ?
N9 Cu3 I5 129.89(10) . . ?
Cu4 Cu3 I5 63.008(17) . . ?
N9 Cu3 I4 119.16(10) . . ?
Cu4 Cu3 I4 63.307(18) . . ?
I5 Cu3 I4 108.57(2) . . ?
N16 Cu4 Cu3 170.38(9) 2_546 . ?
N16 Cu4 I6 104.28(9) 2_546 . ?
Cu3 Cu4 I6 84.79(2) . . ?
N16 Cu4 I5 118.07(9) 2_546 . ?
Cu3 Cu4 I5 60.115(18) . . ?
I6 Cu4 I5 110.77(2) . . ?
N16 Cu4 I4 113.34(9) 2_546 . ?
Cu3 Cu4 I4 60.143(17) . . ?
I6 Cu4 I4 105.666(19) . . ?
I5 Cu4 I4 104.200(19) . . ?
Cu3 I4 Cu4 56.549(18) . . ?
Cu3 I5 Cu4 56.877(18) . . ?
N10 N9 C22 109.5(3) . . ?
N10 N9 Cu3 122.1(3) . . ?
C22 N9 Cu3 127.9(3) . . ?
N9 N10 N11 107.1(3) . . ?
N10 N11 C27 111.4(3) . . ?
N10 N11 C30 119.6(3) . . ?
C27 N11 C30 129.0(3) . . ?
N9 C22 C27 108.3(3) . . ?
N9 C22 C23 131.7(4) . . ?
C27 C22 C23 120.0(4) . . ?
C24 C23 C22 118.8(4) . . ?
C24 C23 H23A 120.6 . . ?
C22 C23 H23A 120.6 . . ?
C23 C24 C25 120.3(4) . . ?
C23 C24 C28 120.0(4) . . ?
C25 C24 C28 119.7(4) . . ?
C26 C25 C24 121.4(4) . . ?
C26 C25 C29 119.2(4) . . ?
C24 C25 C29 119.3(4) . . ?
C25 C26 C27 117.1(4) . . ?
C25 C26 H26A 121.4 . . ?
C27 C26 H26A 121.4 . . ?
N11 C27 C22 103.6(3) . . ?
N11 C27 C26 134.0(3) . . ?
C22 C27 C26 122.3(4) . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C25 C29 H29A 109.5 . . ?
C25 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C25 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N11 C30 N12 112.3(3) . . ?
N11 C30 H30A 109.1 . . ?
N12 C30 H30A 109.1 . . ?
N11 C30 H30B 109.1 . . ?
N12 C30 H30B 109.1 . . ?
H30A C30 H30B 107.9 . . ?
C31 N12 C33 109.0(3) . . ?
C31 N12 C30 124.8(3) . . ?
C33 N12 C30 126.2(3) . . ?
N13 C31 N12 108.1(3) . . ?
N13 C31 H31A 125.9 . . ?
N12 C31 H31A 125.9 . . ?
C31 N13 C32 109.2(3) . . ?
C31 N13 C34 126.0(3) . . ?
C32 N13 C34 124.8(3) . . ?
C33 C32 N13 106.2(3) . . ?
C33 C32 H32A 126.9 . . ?
N13 C32 H32A 126.9 . . ?
C32 C33 N12 107.5(3) . . ?
C32 C33 H33A 126.3 . . ?
N12 C33 H33A 126.3 . . ?
N14 C34 N13 110.3(3) . . ?
N14 C34 H34A 109.6 . . ?
N13 C34 H34A 109.6 . . ?
N14 C34 H34B 109.6 . . ?
N13 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
N15 N14 C35 111.1(3) . . ?
N15 N14 C34 119.1(3) . . ?
C35 N14 C34 129.4(3) . . ?
N16 N15 N14 108.3(3) . . ?
N15 N16 C40 108.6(3) . . ?
N15 N16 Cu4 118.4(2) . 2_556 ?
C40 N16 Cu4 132.9(2) . 2_556 ?
N14 C35 C40 103.9(3) . . ?
N14 C35 C36 133.1(3) . . ?
C40 C35 C36 122.9(3) . . ?
C37 C36 C35 116.8(3) . . ?
C37 C36 H36A 121.6 . . ?
C35 C36 H36A 121.6 . . ?
C36 C37 C38 121.3(3) . . ?
C36 C37 C41 118.9(3) . . ?
C38 C37 C41 119.7(3) . . ?
C39 C38 C37 120.4(3) . . ?
C39 C38 C42 120.0(3) . . ?
C37 C38 C42 119.6(3) . . ?
C38 C39 C40 118.4(3) . . ?
C38 C39 H39A 120.8 . . ?
C40 C39 H39A 120.8 . . ?
N16 C40 C35 108.1(3) . . ?
N16 C40 C39 131.8(3) . . ?
C35 C40 C39 120.0(3) . . ?
C37 C41 H41A 109.5 . . ?
C37 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C37 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C38 C42 H42A 109.5 . . ?
C38 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C38 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

_refine_diff_density_max         1.371
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.145



