# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1559076'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-12-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H44 Cu4 I4 N4 O32 Tb4'
_chemical_formula_weight         2346.11

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           129
_space_group_name_H-M_alt        'P 4/n m m'
_space_group_name_Hall           '-P 4a 2a'

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

_cell_length_a                   18.6509(14)
_cell_length_b                   18.6509(14)
_cell_length_c                   12.2593(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4264.5(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    175(2)
_cell_measurement_reflns_used    14908
_cell_measurement_theta_min      2.7445
_cell_measurement_theta_max      24.7825

_exptl_crystal_description       square
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_F_000             2168
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    5.755
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.369
_exptl_absorpt_correction_T_max  0.447
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      175(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'Omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14323
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.544
_diffrn_reflns_theta_max         25.045
_diffrn_reflns_theta_full        25.045
_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             2118
_reflns_number_gt                1759
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1242P)²+82.4982P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2118
_refine_ls_number_parameters     103
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0694
_refine_ls_wR_factor_ref         0.2222
_refine_ls_wR_factor_gt          0.2145
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.002

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
Tb1 Tb 0.43306(5) 0.43306(5) 1.62881(10) 0.0432(4) Uani 0.7 2 d S T P . .
Tb1A Tb 0.47407(16) 0.47407(16) 1.5766(3) 0.0647(10) Uani 0.3 2 d S T P . .
Cu1 Cu 0.2500 0.68066(10) 1.08242(15) 0.0299(5) Uani 1 2 d S T P . .
I1 I 0.2500 0.62220(5) 0.88798(8) 0.0284(4) Uani 1 2 d S T P . .
O1 O 0.3835(5) 0.4887(5) 1.4819(8) 0.057(3) Uani 1 1 d . . . . .
O2 O 0.5611(4) 0.4544(5) 1.6520(8) 0.052(2) Uani 1 1 d . . . . .
O1W O 0.4396(10) 0.4396(10) 1.853(4) 0.220(19) Uani 1 2 d S T P . .
H1WA H 0.4131 0.4131 1.8929 0.264 Uiso 1 2 d R U P . .
H1WB H 0.4687 0.4687 1.8830 0.264 Uiso 1 2 d R U P . .
O2W O 0.351(3) 0.351(3) 1.627(5) 0.382(5) Uani 1 2 d S TU P . .
H2WA H 0.3252 0.3251 1.6684 0.458 Uiso 1 2 d R U P . .
H2WB H 0.3470 0.3469 1.5579 0.458 Uiso 1 2 d R U P . .
O3W O 0.4530(11) 0.3152(11) 1.6939(18) 0.160(7) Uani 1 1 d . U . . .
H3WA H 0.4572 0.3070 1.7618 0.192 Uiso 1 1 d R U . . .
H3WB H 0.4561 0.2809 1.6485 0.192 Uiso 1 1 d R U . . .
N1 N 0.2500 0.6091(7) 1.2063(10) 0.028(3) Uani 1 2 d S T P . .
C1 C 0.3141(6) 0.5430(6) 1.3459(9) 0.036(3) Uani 1 1 d . . . . .
C2 C 0.3116(6) 0.5868(6) 1.2547(9) 0.031(2) Uani 1 1 d . . . . .
H2 H 0.3549 0.6018 1.2247 0.037 Uiso 1 1 calc R U . . .
C3 C 0.2500 0.5208(9) 1.3910(13) 0.034(4) Uani 1 2 d S T P . .
H3 H 0.2500 0.4909 1.4517 0.041 Uiso 1 2 calc R U P . .
C4 C 0.3837(6) 0.5239(7) 1.3967(10) 0.039(3) 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
Tb1 Tb1A 1.257(4) . ?
Tb1 O2W 2.17(7) . ?
Tb1 O1 2.274(8) . ?
Tb1 O1 2.274(8) 16 ?
Tb1 O3W 2.37(2) . ?
Tb1 O3W 2.37(2) 16 ?
Tb1 O2 2.438(8) . ?
Tb1 O2 2.438(8) 16 ?
Tb1 O1W 2.76(5) . ?
Tb1 Tb1A 3.513(4) 9_668 ?
Tb1A O2 1.905(8) . ?
Tb1A O2 1.905(8) 16 ?
Tb1A O1 2.067(9) . ?
Tb1A O1 2.067(9) 16 ?
Tb1A Tb1A 2.323(8) 9_668 ?
Tb1A C4 2.672(12) 8_668 ?
Tb1A C4 2.672(12) 9_668 ?
Tb1A O1 2.837(10) 9_668 ?
Tb1A O1 2.837(10) 8_668 ?
Tb1A C4 2.926(12) 16 ?
Tb1A C4 2.926(12) . ?
Cu1 N1 2.022(13) . ?
Cu1 Cu1 2.587(4) 2_565 ?
Cu1 I1 2.621(2) . ?
Cu1 Cu1 2.726(3) 11_567 ?
Cu1 Cu1 2.726(3) 12_667 ?
Cu1 I1 2.7360(13) 12_667 ?
Cu1 I1 2.7360(13) 11_567 ?
I1 Cu1 2.7361(13) 12_667 ?
I1 Cu1 2.7361(13) 11_567 ?
O1 C4 1.234(15) . ?
O1 Tb1A 2.837(10) 9_668 ?
O2 C4 1.256(15) 9_668 ?
N1 C2 1.359(12) 14_655 ?
N1 C2 1.359(12) . ?
C1 C3 1.381(14) . ?
C1 C2 1.385(15) . ?
C1 C4 1.484(15) . ?
C3 C1 1.380(14) 14_655 ?
C4 O2 1.256(15) 9_668 ?
C4 Tb1A 2.672(12) 9_668 ?

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
Tb1A Tb1 O2W 148.7(16) . . ?
Tb1A Tb1 O1 64.3(3) . . ?
O2W Tb1 O1 91.5(13) . . ?
Tb1A Tb1 O1 64.3(3) . 16 ?
O2W Tb1 O1 91.5(13) . 16 ?
O1 Tb1 O1 75.2(5) . 16 ?
Tb1A Tb1 O3W 129.9(5) . . ?
O2W Tb1 O3W 57.2(8) . . ?
O1 Tb1 O3W 139.0(6) . . ?
O1 Tb1 O3W 79.5(6) 16 . ?
Tb1A Tb1 O3W 129.9(5) . 16 ?
O2W Tb1 O3W 57.2(8) . 16 ?
O1 Tb1 O3W 79.5(6) . 16 ?
O1 Tb1 O3W 139.0(6) 16 16 ?
O3W Tb1 O3W 100.3(10) . 16 ?
Tb1A Tb1 O2 50.5(3) . . ?
O2W Tb1 O2 144.0(4) . . ?
O1 Tb1 O2 114.6(3) . . ?
O1 Tb1 O2 73.2(4) 16 . ?
O3W Tb1 O2 87.6(6) . . ?
O3W Tb1 O2 147.6(6) 16 . ?
Tb1A Tb1 O2 50.5(3) . 16 ?
O2W Tb1 O2 144.0(4) . 16 ?
O1 Tb1 O2 73.2(4) . 16 ?
O1 Tb1 O2 114.6(3) 16 16 ?
O3W Tb1 O2 147.6(6) . 16 ?
O3W Tb1 O2 87.6(6) 16 16 ?
O2 Tb1 O2 70.5(5) . 16 ?
Tb1A Tb1 O1W 117.1(6) . . ?
O2W Tb1 O1W 94.3(17) . . ?
O1 Tb1 O1W 142.0(3) . . ?
O1 Tb1 O1W 142.0(3) 16 . ?
O3W Tb1 O1W 72.4(6) . . ?
O3W Tb1 O1W 72.4(6) 16 . ?
O2 Tb1 O1W 80.4(5) . . ?
O2 Tb1 O1W 80.4(5) 16 . ?
Tb1A Tb1 Tb1A 15.2(3) . 9_668 ?
O2W Tb1 Tb1A 133.5(16) . 9_668 ?
O1 Tb1 Tb1A 53.7(2) . 9_668 ?
O1 Tb1 Tb1A 53.7(2) 16 9_668 ?
O3W Tb1 Tb1A 128.5(5) . 9_668 ?
O3W Tb1 Tb1A 128.4(5) 16 9_668 ?
O2 Tb1 Tb1A 61.3(2) . 9_668 ?
O2 Tb1 Tb1A 61.3(2) 16 9_668 ?
O1W Tb1 Tb1A 132.2(6) . 9_668 ?
Tb1 Tb1A O2 98.9(3) . . ?
Tb1 Tb1A O2 98.9(3) . 16 ?
O2 Tb1A O2 95.3(7) . 16 ?
Tb1 Tb1A O1 82.5(3) . . ?
O2 Tb1A O1 174.1(5) . . ?
O2 Tb1A O1 90.2(4) 16 . ?
Tb1 Tb1A O1 82.5(3) . 16 ?
O2 Tb1A O1 90.2(4) . 16 ?
O2 Tb1A O1 174.1(5) 16 16 ?
O1 Tb1A O1 84.3(6) . 16 ?
Tb1 Tb1A Tb1A 156.7(4) . 9_668 ?
O2 Tb1A Tb1A 96.8(3) . 9_668 ?
O2 Tb1A Tb1A 96.8(3) 16 9_668 ?
O1 Tb1A Tb1A 80.3(3) . 9_668 ?
O1 Tb1A Tb1A 80.3(3) 16 9_668 ?
Tb1 Tb1A C4 123.4(3) . 8_668 ?
O2 Tb1A C4 96.9(5) . 8_668 ?
O2 Tb1A C4 25.4(4) 16 8_668 ?
O1 Tb1A C4 87.1(4) . 8_668 ?
O1 Tb1A C4 151.4(4) 16 8_668 ?
Tb1A Tb1A C4 71.3(3) 9_668 8_668 ?
Tb1 Tb1A C4 123.4(3) . 9_668 ?
O2 Tb1A C4 25.4(4) . 9_668 ?
O2 Tb1A C4 96.9(5) 16 9_668 ?
O1 Tb1A C4 151.4(4) . 9_668 ?
O1 Tb1A C4 87.1(4) 16 9_668 ?
Tb1A Tb1A C4 71.3(3) 9_668 9_668 ?
C4 Tb1A C4 87.6(6) 8_668 9_668 ?
Tb1 Tb1A O1 147.9(2) . 9_668 ?
O2 Tb1A O1 51.1(3) . 9_668 ?
O2 Tb1A O1 95.4(4) 16 9_668 ?
O1 Tb1A O1 126.2(3) . 9_668 ?
O1 Tb1A O1 86.2(5) 16 9_668 ?
Tb1A Tb1A O1 45.9(2) 9_668 9_668 ?
C4 Tb1A O1 77.0(4) 8_668 9_668 ?
C4 Tb1A O1 25.7(3) 9_668 9_668 ?
Tb1 Tb1A O1 147.9(2) . 8_668 ?
O2 Tb1A O1 95.4(4) . 8_668 ?
O2 Tb1A O1 51.1(3) 16 8_668 ?
O1 Tb1A O1 86.2(5) . 8_668 ?
O1 Tb1A O1 126.2(3) 16 8_668 ?
Tb1A Tb1A O1 45.9(2) 9_668 8_668 ?
C4 Tb1A O1 25.7(3) 8_668 8_668 ?
C4 Tb1A O1 77.0(4) 9_668 8_668 ?
O1 Tb1A O1 58.5(4) 9_668 8_668 ?
Tb1 Tb1A C4 103.1(3) . 16 ?
O2 Tb1A C4 89.1(4) . 16 ?
O2 Tb1A C4 156.6(4) 16 16 ?
O1 Tb1A C4 85.0(4) . 16 ?
O1 Tb1A C4 20.7(4) 16 16 ?
Tb1A Tb1A C4 59.9(3) 9_668 16 ?
C4 Tb1A C4 131.2(2) 8_668 16 ?
C4 Tb1A C4 77.6(5) 9_668 16 ?
O1 Tb1A C4 69.7(4) 9_668 16 ?
O1 Tb1A C4 105.7(3) 8_668 16 ?
Tb1 Tb1A C4 103.1(3) . . ?
O2 Tb1A C4 156.6(4) . . ?
O2 Tb1A C4 89.1(4) 16 . ?
O1 Tb1A C4 20.7(4) . . ?
O1 Tb1A C4 85.0(4) 16 . ?
Tb1A Tb1A C4 59.9(3) 9_668 . ?
C4 Tb1A C4 77.6(5) 8_668 . ?
C4 Tb1A C4 131.2(2) 9_668 . ?
O1 Tb1A C4 105.7(3) 9_668 . ?
O1 Tb1A C4 69.7(4) 8_668 . ?
C4 Tb1A C4 78.4(5) 16 . ?
N1 Cu1 Cu1 131.3(4) . 2_565 ?
N1 Cu1 I1 114.1(4) . . ?
Cu1 Cu1 I1 114.58(5) 2_565 . ?
N1 Cu1 Cu1 150.47(10) . 11_567 ?
Cu1 Cu1 Cu1 61.67(4) 2_565 11_567 ?
I1 Cu1 Cu1 61.52(7) . 11_567 ?
N1 Cu1 Cu1 150.47(10) . 12_667 ?
Cu1 Cu1 Cu1 61.67(4) 2_565 12_667 ?
I1 Cu1 Cu1 61.52(7) . 12_667 ?
Cu1 Cu1 Cu1 56.65(8) 11_567 12_667 ?
N1 Cu1 I1 102.27(18) . 12_667 ?
Cu1 Cu1 I1 61.79(4) 2_565 12_667 ?
I1 Cu1 I1 108.49(4) . 12_667 ?
Cu1 Cu1 I1 106.70(4) 11_567 12_667 ?
Cu1 Cu1 I1 57.36(6) 12_667 12_667 ?
N1 Cu1 I1 102.27(18) . 11_567 ?
Cu1 Cu1 I1 61.79(4) 2_565 11_567 ?
I1 Cu1 I1 108.49(4) . 11_567 ?
Cu1 Cu1 I1 57.36(6) 11_567 11_567 ?
Cu1 Cu1 I1 106.70(4) 12_667 11_567 ?
I1 Cu1 I1 121.19(8) 12_667 11_567 ?
Cu1 I1 Cu1 61.12(7) . 12_667 ?
Cu1 I1 Cu1 61.12(6) . 11_567 ?
Cu1 I1 Cu1 56.42(7) 12_667 11_567 ?
C4 O1 Tb1A 122.9(9) . . ?
C4 O1 Tb1 155.7(9) . . ?
Tb1A O1 Tb1 33.23(17) . . ?
C4 O1 Tb1A 69.7(7) . 9_668 ?
Tb1A O1 Tb1A 53.8(3) . 9_668 ?
Tb1 O1 Tb1A 86.1(3) . 9_668 ?
C4 O2 Tb1A 113.9(8) 9_668 . ?
C4 O2 Tb1 143.0(8) 9_668 . ?
Tb1A O2 Tb1 30.62(18) . . ?
C2 N1 C2 115.6(13) 14_655 . ?
C2 N1 Cu1 122.0(6) 14_655 . ?
C2 N1 Cu1 122.0(7) . . ?
C3 C1 C2 118.1(11) . . ?
C3 C1 C4 121.2(11) . . ?
C2 C1 C4 120.6(11) . . ?
N1 C2 C1 124.1(10) . . ?
C1 C3 C1 119.9(14) 14_655 . ?
O1 C4 O2 125.2(11) . 9_668 ?
O1 C4 C1 118.7(11) . . ?
O2 C4 C1 116.1(11) 9_668 . ?
O1 C4 Tb1A 84.7(7) . 9_668 ?
O2 C4 Tb1A 40.7(5) 9_668 9_668 ?
C1 C4 Tb1A 156.5(9) . 9_668 ?
O1 C4 Tb1A 36.4(6) . . ?
O2 C4 Tb1A 89.4(7) 9_668 . ?
C1 C4 Tb1A 153.7(9) . . ?
Tb1A C4 Tb1A 48.8(2) 9_668 . ?

_refine_diff_density_max         2.322
_refine_diff_density_min         -2.850
_refine_diff_density_rms         0.259



loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.026 0.119 0.000 1521.3 267.7
2 0.250 0.750 0.500 188.1 43.3
3 0.750 0.250 0.500 188.1 43.4
_platon_squeeze_details          
; ?
;
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1559077'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-12-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H44 Cu4 I4 N4 O32 Y4'
_chemical_formula_weight         2066.07

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           129
_space_group_name_H-M_alt        'P 4/n m m'
_space_group_name_Hall           '-P 4a 2a'

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

_cell_length_a                   18.529(4)
_cell_length_b                   18.529(4)
_cell_length_c                   12.303(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4224.2(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    175(2)
_cell_measurement_reflns_used    17556
_cell_measurement_theta_min      2.752
_cell_measurement_theta_max      25.7545

_exptl_crystal_description       square
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_F_000             1960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.126
_exptl_absorpt_coefficient_mu    5.223
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.401
_exptl_absorpt_correction_T_max  0.518
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      175(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'Omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13995
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.554
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2088
_reflns_number_gt                1702
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1300P)²+12.0108P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2088
_refine_ls_number_parameters     107
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0537
_refine_ls_wR_factor_ref         0.1808
_refine_ls_wR_factor_gt          0.1746
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.004
_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
Cu3 Cu 1.18028(7) 0.7500 -1.41846(9) 0.0369(4) Uani 1 2 d S T P . .
N1 N 1.1083(4) 0.7500 -1.2938(7) 0.0322(18) Uani 1 2 d S T P . .
O1 O 0.9897(3) 0.6146(3) -1.0192(5) 0.0639(18) Uani 1 1 d . . . . .
C1 C 1.0422(4) 0.6853(4) -1.1558(6) 0.0398(17) Uani 1 1 d . . . . .
C2 C 1.0217(6) 0.7500 -1.1107(8) 0.042(2) Uani 1 2 d S T P . .
H2 H 0.9934 0.7500 -1.0483 0.050 Uiso 1 2 calc R U P . .
C3 C 1.0252(5) 0.6153(5) -1.1051(7) 0.052(2) Uani 1 1 d . . . . .
C4 C 1.0862(4) 0.6877(4) -1.2481(5) 0.0371(16) Uani 1 1 d . . . . .
H4 H 1.1009 0.6444 -1.2793 0.045 Uiso 1 1 calc R U . . .
I1 I 1.12148(3) 0.7500 -1.61232(5) 0.0351(3) Uani 1 2 d S T P . .
O3 O 1.0464(4) 0.5592(3) -1.1536(5) 0.0607(16) Uani 1 1 d . . . . .
O3W O 1.0610(5) 0.4390(5) -1.3189(13) 0.149(6) Uani 1 2 d S T P . .
H3WA H 1.0551 0.4781 -1.3520 0.179 Uiso 0.5 1 d R U P . .
H3WB H 1.0660 0.3994 -1.3549 0.179 Uiso 0.5 1 d R U P . .
O1W O 1.062(3) 0.3437(5) -1.1766(17) 0.61(7) Uani 0.5 1 d . . P . .
H1WA H 1.0601 0.3361 -1.2446 0.729 Uiso 1 1 d R U . . .
H1WB H 1.0591 0.3085 -1.1324 0.729 Uiso 1 1 d DR U . . .
O2W O 1.1551(13) 0.3449(13) -1.115(2) 0.262(7) Uani 1 2 d S TU P . .
H2WA H 1.1714 0.3286 -1.1751 0.314 Uiso 1 2 d R U P . .
H2WB H 1.1713 0.3287 -1.0554 0.314 Uiso 1 2 d R U P . .
Y1 Y 1.06460(6) 0.43540(6) -1.12366(11) 0.0371(4) Uani 0.7 2 d S T P . .
Y2 Y 1.02635(14) 0.47365(14) -1.0800(3) 0.0389(8) Uani 0.3 2 d S T P . .
O1WA O 1.0476(8) 0.3168(7) -1.1953(13) 0.067(4) Uiso 0.5 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
Cu3 N1 2.033(8) . ?
Cu3 Cu3 2.584(3) 2_765 ?
Cu3 I1 2.6222(14) . ?
Cu3 Cu3 2.714(2) 12_752 ?
Cu3 Cu3 2.714(2) 11_672 ?
Cu3 I1 2.7355(10) 11_672 ?
Cu3 I1 2.7355(10) 12_752 ?
N1 C4 1.347(8) . ?
N1 C4 1.347(8) 13_575 ?
O1 C3 1.245(10) . ?
O1 Y2 2.063(6) 9_763 ?
O1 Y1 2.228(5) 9_763 ?
O1 Y2 2.801(7) . ?
C1 C2 1.374(9) . ?
C1 C4 1.399(9) . ?
C1 C3 1.473(11) . ?
C2 C1 1.373(9) 13_575 ?
C3 O3 1.262(11) . ?
C3 Y2 2.644(10) . ?
C3 Y2 2.970(9) 9_763 ?
I1 Cu3 2.7355(10) 11_672 ?
I1 Cu3 2.7355(10) 12_752 ?
O3 Y2 1.863(6) . ?
O3 Y1 2.348(6) . ?
O3W Y1 2.404(16) . ?
O1W O1WA 0.61(3) . ?
O1W Y1 1.820(12) . ?
O1W Y2 2.76(2) . ?
O2W Y1 2.37(3) . ?
Y1 Y2 1.137(4) . ?
Y1 O1W 1.820(12) 15_775 ?
Y1 O1 2.228(5) 7_543 ?
Y1 O1 2.228(5) 9_763 ?
Y1 O3 2.348(6) 15_775 ?
Y1 O1WA 2.388(15) . ?
Y1 O1WA 2.388(15) 15_775 ?
Y1 Y2 3.458(4) 9_763 ?
Y2 O3 1.863(6) 15_775 ?
Y2 O1 2.063(6) 7_543 ?
Y2 O1 2.063(6) 9_763 ?
Y2 Y2 2.405(7) 9_763 ?
Y2 C3 2.644(10) 15_775 ?
Y2 O1W 2.76(2) 15_775 ?
Y2 O1 2.801(7) 15_775 ?

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 Cu3 Cu3 131.0(2) . 2_765 ?
N1 Cu3 I1 114.4(3) . . ?
Cu3 Cu3 I1 114.55(3) 2_765 . ?
N1 Cu3 Cu3 150.50(6) . 12_752 ?
Cu3 Cu3 Cu3 61.57(3) 2_765 12_752 ?
I1 Cu3 Cu3 61.65(4) . 12_752 ?
N1 Cu3 Cu3 150.50(6) . 11_672 ?
Cu3 Cu3 Cu3 61.57(3) 2_765 11_672 ?
I1 Cu3 Cu3 61.66(4) . 11_672 ?
Cu3 Cu3 Cu3 56.85(6) 12_752 11_672 ?
N1 Cu3 I1 101.86(12) . 11_672 ?
Cu3 Cu3 I1 61.82(2) 2_765 11_672 ?
I1 Cu3 I1 108.79(3) . 11_672 ?
Cu3 Cu3 I1 106.97(3) 12_752 11_672 ?
Cu3 Cu3 I1 57.53(4) 11_672 11_672 ?
N1 Cu3 I1 101.86(12) . 12_752 ?
Cu3 Cu3 I1 61.82(2) 2_765 12_752 ?
I1 Cu3 I1 108.79(3) . 12_752 ?
Cu3 Cu3 I1 57.53(4) 12_752 12_752 ?
Cu3 Cu3 I1 106.97(3) 11_672 12_752 ?
I1 Cu3 I1 121.04(5) 11_672 12_752 ?
C4 N1 C4 117.9(8) . 13_575 ?
C4 N1 Cu3 120.9(4) . . ?
C4 N1 Cu3 120.9(4) 13_575 . ?
C3 O1 Y2 125.9(6) . 9_763 ?
C3 O1 Y1 155.9(6) . 9_763 ?
Y2 O1 Y1 30.43(13) 9_763 9_763 ?
C3 O1 Y2 69.8(5) . . ?
Y2 O1 Y2 56.9(2) 9_763 . ?
Y1 O1 Y2 86.10(19) 9_763 . ?
C2 C1 C4 117.5(7) . . ?
C2 C1 C3 122.6(7) . . ?
C4 C1 C3 119.7(7) . . ?
C1 C2 C1 121.5(9) 13_575 . ?
O1 C3 O3 123.9(8) . . ?
O1 C3 C1 118.8(9) . . ?
O3 C3 C1 117.3(7) . . ?
O1 C3 Y2 84.0(5) . . ?
O3 C3 Y2 40.0(4) . . ?
C1 C3 Y2 157.3(6) . . ?
O1 C3 Y2 34.2(4) . 9_763 ?
O3 C3 Y2 90.3(5) . 9_763 ?
C1 C3 Y2 151.9(6) . 9_763 ?
Y2 C3 Y2 50.3(2) . 9_763 ?
N1 C4 C1 122.8(7) . . ?
Cu3 I1 Cu3 60.82(4) . 11_672 ?
Cu3 I1 Cu3 60.82(4) . 12_752 ?
Cu3 I1 Cu3 56.36(5) 11_672 12_752 ?
C3 O3 Y2 114.1(5) . . ?
C3 O3 Y1 140.9(5) . . ?
Y2 O3 Y1 28.48(14) . . ?
O1WA O1W Y1 155(8) . . ?
O1WA O1W Y2 140(7) . . ?
Y1 O1W Y2 16.2(7) . . ?
Y2 Y1 O1W 137(2) . 15_775 ?
Y2 Y1 O1W 137(2) . . ?
O1W Y1 O1W 86(4) 15_775 . ?
Y2 Y1 O1 66.7(2) . 7_543 ?
O1W Y1 O1 83.2(12) 15_775 7_543 ?
O1W Y1 O1 135.7(12) . 7_543 ?
Y2 Y1 O1 66.7(2) . 9_763 ?
O1W Y1 O1 135.7(12) 15_775 9_763 ?
O1W Y1 O1 83.2(12) . 9_763 ?
O1 Y1 O1 75.7(4) 7_543 9_763 ?
Y2 Y1 O3 51.37(19) . 15_775 ?
O1W Y1 O3 148.4(8) 15_775 15_775 ?
O1W Y1 O3 93(2) . 15_775 ?
O1 Y1 O3 117.8(2) 7_543 15_775 ?
O1 Y1 O3 75.1(2) 9_763 15_775 ?
Y2 Y1 O3 51.37(19) . . ?
O1W Y1 O3 93(2) 15_775 . ?
O1W Y1 O3 148.4(8) . . ?
O1 Y1 O3 75.1(2) 7_543 . ?
O1 Y1 O3 117.8(2) 9_763 . ?
O3 Y1 O3 72.2(3) 15_775 . ?
Y2 Y1 O2W 149.3(7) . . ?
O1W Y1 O2W 51.3(18) 15_775 . ?
O1W Y1 O2W 51.3(18) . . ?
O1 Y1 O2W 89.5(6) 7_543 . ?
O1 Y1 O2W 89.5(6) 9_763 . ?
O3 Y1 O2W 143.0(2) 15_775 . ?
O3 Y1 O2W 143.0(2) . . ?
Y2 Y1 O1WA 131.7(3) . . ?
O1W Y1 O1WA 90.9(18) 15_775 . ?
O1W Y1 O1WA 6(2) . . ?
O1 Y1 O1WA 139.6(4) 7_543 . ?
O1 Y1 O1WA 81.3(4) 9_763 . ?
O3 Y1 O1WA 86.8(4) 15_775 . ?
O3 Y1 O1WA 145.3(4) . . ?
O2W Y1 O1WA 57.3(5) . . ?
Y2 Y1 O1WA 131.7(3) . 15_775 ?
O1W Y1 O1WA 6(2) 15_775 15_775 ?
O1W Y1 O1WA 90.9(18) . 15_775 ?
O1 Y1 O1WA 81.3(4) 7_543 15_775 ?
O1 Y1 O1WA 139.6(4) 9_763 15_775 ?
O3 Y1 O1WA 145.3(4) 15_775 15_775 ?
O3 Y1 O1WA 86.8(4) . 15_775 ?
O2W Y1 O1WA 57.3(5) . 15_775 ?
O1WA Y1 O1WA 96.1(7) . 15_775 ?
Y2 Y1 O3W 115.9(4) . . ?
O1W Y1 O3W 70.6(7) 15_775 . ?
O1W Y1 O3W 70.6(7) . . ?
O1 Y1 O3W 141.95(18) 7_543 . ?
O1 Y1 O3W 141.95(18) 9_763 . ?
O3 Y1 O3W 79.2(3) 15_775 . ?
O3 Y1 O3W 79.2(3) . . ?
O2W Y1 O3W 94.7(8) . . ?
O1WA Y1 O3W 69.7(4) . . ?
O1WA Y1 O3W 69.7(4) 15_775 . ?
Y2 Y1 Y2 18.3(2) . 9_763 ?
O1W Y1 Y2 134.5(16) 15_775 9_763 ?
O1W Y1 Y2 134.5(16) . 9_763 ?
O1 Y1 Y2 53.90(17) 7_543 9_763 ?
O1 Y1 Y2 53.90(17) 9_763 9_763 ?
O3 Y1 Y2 64.39(16) 15_775 9_763 ?
O3 Y1 Y2 64.39(16) . 9_763 ?
O2W Y1 Y2 131.1(7) . 9_763 ?
O1WA Y1 Y2 130.7(4) . 9_763 ?
O1WA Y1 Y2 130.7(4) 15_775 9_763 ?
O3W Y1 Y2 134.2(3) . 9_763 ?
Y1 Y2 O3 100.1(3) . 15_775 ?
Y1 Y2 O3 100.1(3) . . ?
O3 Y2 O3 95.9(4) 15_775 . ?
Y1 Y2 O1 82.8(2) . 7_543 ?
O3 Y2 O1 172.4(3) 15_775 7_543 ?
O3 Y2 O1 90.4(3) . 7_543 ?
Y1 Y2 O1 82.8(2) . 9_763 ?
O3 Y2 O1 90.4(3) 15_775 9_763 ?
O3 Y2 O1 172.4(3) . 9_763 ?
O1 Y2 O1 83.0(4) 7_543 9_763 ?
Y1 Y2 Y2 153.2(3) . 9_763 ?
O3 Y2 Y2 97.7(3) 15_775 9_763 ?
O3 Y2 Y2 97.7(3) . 9_763 ?
O1 Y2 Y2 77.2(2) 7_543 9_763 ?
O1 Y2 Y2 77.2(2) 9_763 9_763 ?
Y1 Y2 C3 124.7(2) . . ?
O3 Y2 C3 97.7(3) 15_775 . ?
O3 Y2 C3 25.8(3) . . ?
O1 Y2 C3 86.1(3) 7_543 . ?
O1 Y2 C3 148.8(3) 9_763 . ?
Y2 Y2 C3 71.9(2) 9_763 . ?
Y1 Y2 C3 124.7(2) . 15_775 ?
O3 Y2 C3 25.8(3) 15_775 15_775 ?
O3 Y2 C3 97.7(3) . 15_775 ?
O1 Y2 C3 148.8(3) 7_543 15_775 ?
O1 Y2 C3 86.1(3) 9_763 15_775 ?
Y2 Y2 C3 71.9(2) 9_763 15_775 ?
C3 Y2 C3 88.3(4) . 15_775 ?
Y1 Y2 O1W 26.6(12) . 15_775 ?
O3 Y2 O1W 119.0(7) 15_775 15_775 ?
O3 Y2 O1W 79.6(12) . 15_775 ?
O1 Y2 O1W 66.3(6) 7_543 15_775 ?
O1 Y2 O1W 101.0(12) 9_763 15_775 ?
Y2 Y2 O1W 143.3(7) 9_763 15_775 ?
C3 Y2 O1W 101.2(13) . 15_775 ?
C3 Y2 O1W 144.7(7) 15_775 15_775 ?
Y1 Y2 O1W 26.6(12) . . ?
O3 Y2 O1W 79.6(12) 15_775 . ?
O3 Y2 O1W 119.0(7) . . ?
O1 Y2 O1W 101.0(12) 7_543 . ?
O1 Y2 O1W 66.3(6) 9_763 . ?
Y2 Y2 O1W 143.3(7) 9_763 . ?
C3 Y2 O1W 144.7(7) . . ?
C3 Y2 O1W 101.2(13) 15_775 . ?
O1W Y2 O1W 53(2) 15_775 . ?
Y1 Y2 O1 149.15(14) . 15_775 ?
O3 Y2 O1 52.0(2) 15_775 15_775 ?
O3 Y2 O1 96.3(3) . 15_775 ?
O1 Y2 O1 123.1(2) 7_543 15_775 ?
O1 Y2 O1 84.2(3) 9_763 15_775 ?
Y2 Y2 O1 45.92(16) 9_763 15_775 ?
C3 Y2 O1 77.5(3) . 15_775 ?
C3 Y2 O1 26.2(2) 15_775 15_775 ?
O1W Y2 O1 170.0(4) 15_775 15_775 ?
O1W Y2 O1 123.2(13) . 15_775 ?
Y1 Y2 O1 149.15(14) . . ?
O3 Y2 O1 96.3(3) 15_775 . ?
O3 Y2 O1 52.0(2) . . ?
O1 Y2 O1 84.2(3) 7_543 . ?
O1 Y2 O1 123.1(2) 9_763 . ?
Y2 Y2 O1 45.92(16) 9_763 . ?
C3 Y2 O1 26.2(2) . . ?
C3 Y2 O1 77.5(3) 15_775 . ?
O1W Y2 O1 123.2(13) 15_775 . ?
O1W Y2 O1 170.0(4) . . ?
O1 Y2 O1 58.5(3) 15_775 . ?
O1W O1WA Y1 18(6) . . ?

_refine_diff_density_max         1.611
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.154




loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.250 0.750 0.000 189.5 31.3
2 0.750 0.250 0.000 189.5 31.3
3 0.238 0.241 0.500 1387.6 341.3
_platon_squeeze_details          
; ?
;
####################################################################### 
# 
# 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_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1559078'
_audit_update_record             
;
2017-06-28 deposited with the CCDC.
2017-12-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H44 Cu4 Eu4 I4 N4 O32'
_chemical_formula_weight         2318.27

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           129
_space_group_name_H-M_alt        'P 4/n m m'
_space_group_name_Hall           '-P 4a 2a'

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

_cell_length_a                   18.6210(9)
_cell_length_b                   18.6210(9)
_cell_length_c                   12.3194(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4271.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    175(2)
_cell_measurement_reflns_used    14511
_cell_measurement_theta_min      2.742
_cell_measurement_theta_max      24.9605

_exptl_crystal_description       square
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_F_000             2152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.132
_exptl_absorpt_coefficient_mu    5.371
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_T_max  0.492
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      175(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'Omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14062
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.547
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_full        25.023
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2118
_reflns_number_gt                1801
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1315P)²+67.9684P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2118
_refine_ls_number_parameters     103
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0697
_refine_ls_wR_factor_ref         0.2223
_refine_ls_wR_factor_gt          0.2167
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.059
_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
Eu1 Eu 0.06597(5) 0.06597(5) 1.62665(9) 0.0395(4) Uani 0.7 2 d S T P . .
Eu1A Eu 0.02545(19) 0.02545(19) 1.5776(4) 0.0835(13) Uani 0.3 2 d S T P . .
Cu1 Cu 0.2500 -0.18065(10) 1.08205(14) 0.0345(5) Uani 1 2 d S T P . .
I1 I 0.2500 -0.12187(5) 0.88844(7) 0.0323(4) Uani 1 2 d S T P . .
O1 O 0.1164(5) 0.0106(5) 1.4788(7) 0.066(3) Uani 1 1 d . . . . .
O2 O -0.0611(4) 0.0471(5) 1.6531(8) 0.062(2) Uani 1 1 d . . . . .
O1W O 0.1845(9) 0.0510(10) 1.6922(15) 0.145(6) Uani 1 1 d . U . . .
H1WA H 0.1930 0.0486 1.7599 0.174 Uiso 1 1 d R U . . .
H1WB H 0.2188 0.0482 1.6469 0.174 Uiso 1 1 d R U . . .
O2W O 0.0626(9) 0.0626(9) 1.836(3) 0.199(15) Uani 1 2 d S T P . .
H2WA H 0.0229 0.0558 1.8689 0.239 Uiso 0.5 1 d R U P . .
H2WB H 0.1011 0.0673 1.8728 0.239 Uiso 0.5 1 d R U P . .
O3W O 0.153(2) 0.153(2) 1.639(4) 0.363(9) Uani 1 2 d S TU P . .
H3WA H 0.1742 0.1741 1.6915 0.436 Uiso 1 2 d R U P . .
H3WB H 0.1643 0.1643 1.5739 0.436 Uiso 1 2 d R U P . .
N1 N 0.2500 -0.1090(7) 1.2058(10) 0.034(3) Uani 1 2 d S T P . .
C1 C 0.2500 -0.0210(8) 1.3903(12) 0.038(3) Uani 1 2 d S TU P . .
H1 H 0.2500 0.0071 1.4527 0.045 Uiso 1 2 calc R U P . .
C2 C 0.1868(6) -0.0428(6) 1.3421(9) 0.039(2) Uani 1 1 d . . . . .
C3 C 0.1888(5) -0.0873(6) 1.2523(8) 0.035(2) Uani 1 1 d . . . . .
H3 H 0.1455 -0.1028 1.2228 0.042 Uiso 1 1 calc R U . . .
C4 C 0.1162(7) -0.0241(7) 1.3953(10) 0.048(3) 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
Eu1 Eu1A 1.226(5) . ?
Eu1 O1 2.293(8) . ?
Eu1 O1 2.293(8) 16 ?
Eu1 O3W 2.31(6) . ?
Eu1 O1W 2.367(17) . ?
Eu1 O1W 2.367(17) 16 ?
Eu1 O2 2.415(8) . ?
Eu1 O2 2.415(8) 16 ?
Eu1 O2W 2.58(4) . ?
Eu1 Eu1A 3.482(5) 9_558 ?
Eu1A O2 1.905(8) . ?
Eu1A O2 1.905(8) 16 ?
Eu1A O1 2.103(9) . ?
Eu1A O1 2.103(9) 16 ?
Eu1A Eu1A 2.335(10) 9_558 ?
Eu1A C4 2.659(13) 8_558 ?
Eu1A C4 2.659(13) 9_558 ?
Eu1A O1 2.812(10) 9_558 ?
Eu1A O1 2.812(10) 8_558 ?
Eu1A C4 2.958(12) . ?
Eu1A C4 2.958(12) 16 ?
Cu1 N1 2.026(12) . ?
Cu1 Cu1 2.583(4) 2_545 ?
Cu1 I1 2.624(2) . ?
Cu1 Cu1 2.724(3) 12_557 ?
Cu1 Cu1 2.724(3) 11_657 ?
Cu1 I1 2.7372(12) 12_557 ?
Cu1 I1 2.7372(12) 11_657 ?
I1 Cu1 2.7371(12) 12_557 ?
I1 Cu1 2.7371(12) 11_657 ?
O1 C4 1.215(14) . ?
O1 Eu1A 2.812(10) 9_558 ?
O2 C4 1.262(15) 9_558 ?
N1 C3 1.338(12) 14_655 ?
N1 C3 1.338(12) . ?
C1 C2 1.378(13) 14_655 ?
C1 C2 1.378(13) . ?
C2 C3 1.383(14) . ?
C2 C4 1.510(15) . ?
C4 O2 1.262(15) 9_558 ?
C4 Eu1A 2.659(13) 9_558 ?

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
Eu1A Eu1 O1 65.4(3) . . ?
Eu1A Eu1 O1 65.4(3) . 16 ?
O1 Eu1 O1 74.8(5) . 16 ?
Eu1A Eu1 O3W 154.2(13) . . ?
O1 Eu1 O3W 94.6(11) . . ?
O1 Eu1 O3W 94.6(11) 16 . ?
Eu1A Eu1 O1W 132.0(4) . . ?
O1 Eu1 O1W 80.6(5) . . ?
O1 Eu1 O1W 137.6(5) 16 . ?
O3W Eu1 O1W 53.3(6) . . ?
Eu1A Eu1 O1W 132.0(4) . 16 ?
O1 Eu1 O1W 137.6(5) . 16 ?
O1 Eu1 O1W 80.6(5) 16 16 ?
O3W Eu1 O1W 53.3(6) . 16 ?
O1W Eu1 O1W 95.9(9) . 16 ?
Eu1A Eu1 O2 51.2(3) . . ?
O1 Eu1 O2 116.3(3) . . ?
O1 Eu1 O2 74.1(4) 16 . ?
O3W Eu1 O2 141.8(5) . . ?
O1W Eu1 O2 148.3(5) . . ?
O1W Eu1 O2 88.5(5) 16 . ?
Eu1A Eu1 O2 51.2(3) . 16 ?
O1 Eu1 O2 74.1(4) . 16 ?
O1 Eu1 O2 116.3(3) 16 16 ?
O3W Eu1 O2 141.8(5) . 16 ?
O1W Eu1 O2 88.5(5) . 16 ?
O1W Eu1 O2 148.3(5) 16 16 ?
O2 Eu1 O2 72.3(5) . 16 ?
Eu1A Eu1 O2W 117.6(6) . . ?
O1 Eu1 O2W 142.4(3) . . ?
O1 Eu1 O2W 142.4(3) 16 . ?
O3W Eu1 O2W 88.2(14) . . ?
O1W Eu1 O2W 71.2(5) . . ?
O1W Eu1 O2W 71.2(5) 16 . ?
O2 Eu1 O2W 80.7(5) . . ?
O2 Eu1 O2W 80.7(5) 16 . ?
Eu1A Eu1 Eu1A 16.7(3) . 9_558 ?
O1 Eu1 Eu1A 53.6(2) . 9_558 ?
O1 Eu1 Eu1A 53.6(2) 16 9_558 ?
O3W Eu1 Eu1A 137.5(13) . 9_558 ?
O1W Eu1 Eu1A 130.2(4) . 9_558 ?
O1W Eu1 Eu1A 130.2(4) 16 9_558 ?
O2 Eu1 Eu1A 63.1(2) . 9_558 ?
O2 Eu1 Eu1A 63.1(2) 16 9_558 ?
O2W Eu1 Eu1A 134.3(5) . 9_558 ?
Eu1 Eu1A O2 98.6(4) . . ?
Eu1 Eu1A O2 98.6(4) . 16 ?
O2 Eu1A O2 96.8(7) . 16 ?
Eu1 Eu1A O1 82.6(3) . . ?
O2 Eu1A O1 172.7(5) . . ?
O2 Eu1A O1 90.1(4) 16 . ?
Eu1 Eu1A O1 82.6(3) . 16 ?
O2 Eu1A O1 90.1(4) . 16 ?
O2 Eu1A O1 172.7(5) 16 16 ?
O1 Eu1A O1 83.0(6) . 16 ?
Eu1 Eu1A Eu1A 154.6(5) . 9_558 ?
O2 Eu1A Eu1A 98.2(4) . 9_558 ?
O2 Eu1A Eu1A 98.2(4) 16 9_558 ?
O1 Eu1A Eu1A 78.5(3) . 9_558 ?
O1 Eu1A Eu1A 78.5(3) 16 9_558 ?
Eu1 Eu1A C4 123.7(3) . 8_558 ?
O2 Eu1A C4 98.1(5) . 8_558 ?
O2 Eu1A C4 26.0(4) 16 8_558 ?
O1 Eu1A C4 87.1(4) . 8_558 ?
O1 Eu1A C4 150.5(4) 16 8_558 ?
Eu1A Eu1A C4 72.3(3) 9_558 8_558 ?
Eu1 Eu1A C4 123.7(3) . 9_558 ?
O2 Eu1A C4 26.0(4) . 9_558 ?
O2 Eu1A C4 98.1(5) 16 9_558 ?
O1 Eu1A C4 150.5(4) . 9_558 ?
O1 Eu1A C4 87.1(4) 16 9_558 ?
Eu1A Eu1A C4 72.3(3) 9_558 9_558 ?
C4 Eu1A C4 88.0(6) 8_558 9_558 ?
Eu1 Eu1A O1 147.8(2) . 9_558 ?
O2 Eu1A O1 51.4(3) . 9_558 ?
O2 Eu1A O1 96.7(4) 16 9_558 ?
O1 Eu1A O1 125.6(3) . 9_558 ?
O1 Eu1A O1 85.7(5) 16 9_558 ?
Eu1A Eu1A O1 47.1(2) 9_558 9_558 ?
C4 Eu1A O1 77.6(4) 8_558 9_558 ?
C4 Eu1A O1 25.5(3) 9_558 9_558 ?
Eu1 Eu1A O1 147.8(2) . 8_558 ?
O2 Eu1A O1 96.7(4) . 8_558 ?
O2 Eu1A O1 51.4(3) 16 8_558 ?
O1 Eu1A O1 85.7(5) . 8_558 ?
O1 Eu1A O1 125.6(3) 16 8_558 ?
Eu1A Eu1A O1 47.1(2) 9_558 8_558 ?
C4 Eu1A O1 25.5(3) 8_558 8_558 ?
C4 Eu1A O1 77.6(4) 9_558 8_558 ?
O1 Eu1A O1 59.4(4) 9_558 8_558 ?
Eu1 Eu1A C4 102.4(4) . . ?
O2 Eu1A C4 157.0(4) . . ?
O2 Eu1A C4 89.2(4) 16 . ?
O1 Eu1A C4 19.9(4) . . ?
O1 Eu1A C4 83.5(4) 16 . ?
Eu1A Eu1A C4 58.9(3) 9_558 . ?
C4 Eu1A C4 77.9(5) 8_558 . ?
C4 Eu1A C4 131.2(3) 9_558 . ?
O1 Eu1A C4 105.9(3) 9_558 . ?
O1 Eu1A C4 69.9(4) 8_558 . ?
Eu1 Eu1A C4 102.4(4) . 16 ?
O2 Eu1A C4 89.2(4) . 16 ?
O2 Eu1A C4 157.0(4) 16 16 ?
O1 Eu1A C4 83.5(4) . 16 ?
O1 Eu1A C4 19.9(4) 16 16 ?
Eu1A Eu1A C4 58.9(3) 9_558 16 ?
C4 Eu1A C4 131.2(3) 8_558 16 ?
C4 Eu1A C4 77.9(5) 9_558 16 ?
O1 Eu1A C4 69.9(4) 9_558 16 ?
O1 Eu1A C4 105.9(3) 8_558 16 ?
C4 Eu1A C4 77.3(5) . 16 ?
N1 Cu1 Cu1 131.2(4) . 2_545 ?
N1 Cu1 I1 114.1(4) . . ?
Cu1 Cu1 I1 114.65(4) 2_545 . ?
N1 Cu1 Cu1 150.52(10) . 12_557 ?
Cu1 Cu1 Cu1 61.71(4) 2_545 12_557 ?
I1 Cu1 Cu1 61.52(6) . 12_557 ?
N1 Cu1 Cu1 150.52(10) . 11_657 ?
Cu1 Cu1 Cu1 61.71(4) 2_545 11_657 ?
I1 Cu1 Cu1 61.52(6) . 11_657 ?
Cu1 Cu1 Cu1 56.58(8) 12_557 11_657 ?
N1 Cu1 I1 102.18(17) . 12_557 ?
Cu1 Cu1 I1 61.85(4) 2_545 12_557 ?
I1 Cu1 I1 108.51(4) . 12_557 ?
Cu1 Cu1 I1 57.44(5) 12_557 12_557 ?
Cu1 Cu1 I1 106.74(4) 11_657 12_557 ?
N1 Cu1 I1 102.18(17) . 11_657 ?
Cu1 Cu1 I1 61.85(4) 2_545 11_657 ?
I1 Cu1 I1 108.51(4) . 11_657 ?
Cu1 Cu1 I1 106.74(4) 12_557 11_657 ?
Cu1 Cu1 I1 57.44(5) 11_657 11_657 ?
I1 Cu1 I1 121.30(7) 12_557 11_657 ?
Cu1 I1 Cu1 61.04(6) . 12_557 ?
Cu1 I1 Cu1 61.04(6) . 11_657 ?
Cu1 I1 Cu1 56.30(7) 12_557 11_657 ?
C4 O1 Eu1A 123.9(9) . . ?
C4 O1 Eu1 155.6(9) . . ?
Eu1A O1 Eu1 32.02(18) . . ?
C4 O1 Eu1A 70.2(7) . 9_558 ?
Eu1A O1 Eu1A 54.4(3) . 9_558 ?
Eu1 O1 Eu1A 85.4(3) . 9_558 ?
C4 O2 Eu1A 112.7(7) 9_558 . ?
C4 O2 Eu1 141.5(8) 9_558 . ?
Eu1A O2 Eu1 30.1(2) . . ?
C3 N1 C3 116.8(12) 14_655 . ?
C3 N1 Cu1 121.4(6) 14_655 . ?
C3 N1 Cu1 121.4(6) . . ?
C2 C1 C2 117.1(13) 14_655 . ?
C1 C2 C3 119.9(10) . . ?
C1 C2 C4 119.2(10) . . ?
C3 C2 C4 120.5(10) . . ?
N1 C3 C2 123.1(10) . . ?
O1 C4 O2 125.7(11) . 9_558 ?
O1 C4 C2 119.2(12) . . ?
O2 C4 C2 115.1(10) 9_558 . ?
O1 C4 Eu1A 84.3(7) . 9_558 ?
O2 C4 Eu1A 41.4(5) 9_558 9_558 ?
C2 C4 Eu1A 156.4(9) . 9_558 ?
O1 C4 Eu1A 36.2(6) . . ?
O2 C4 Eu1A 90.0(7) 9_558 . ?
C2 C4 Eu1A 154.0(8) . . ?
Eu1A C4 Eu1A 48.8(3) 9_558 . ?

_refine_diff_density_max         2.266
_refine_diff_density_min         -3.897
_refine_diff_density_rms         0.258



loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.006 -0.006 0.000 1573.8 364.6
2 0.250 0.750 0.500 186.9 33.5
3 0.750 0.250 0.500 187.0 33.5
_platon_squeeze_details          
; ?
;
