# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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 973518'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-04-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H22 Cl3 Cu3 Dy N3 O8, H2 O'
_chemical_formula_sum            'C24 H24 Cl3 Cu3 Dy N3 O9'
_chemical_formula_weight         957.96
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7527(10)
_cell_length_b                   13.1156(14)
_cell_length_c                   13.1419(14)
_cell_angle_alpha                96.9510(10)
_cell_angle_beta                 107.5630(10)
_cell_angle_gamma                98.2930(10)
_cell_volume                     1561.6(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5751
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.399
_cell_measurement_theta_min      1.651
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.690
_exptl_absorpt_correction_T_max  0.391
_exptl_absorpt_correction_T_min  0.337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.037
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8218
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.399
_diffrn_reflns_theta_min         1.651
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5054
_reflns_number_total             5751
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Apex2 (Bruker, 2005)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'Apex2 (Bruker, 2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.919
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5646
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0336
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0372P)²+2.6034P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0835
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Cu3B) = Uanis(Cu3A)
3. Others
 Sof(O3WB)=Sof(H3WA)=Sof(H3WB)=1-FVAR(1)
 Sof(O3WA)=Sof(H3WC)=Sof(H3WD)=FVAR(1)
 Sof(Cu3B)=1-FVAR(2)
 Sof(Cu3A)=FVAR(2)
4.a Free rotating group:
 O3WB(H3WA,H3WB), O3WA(H3WC,H3WD)
4.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C10(H10), C11(H11), C3(H3), C18(H18), C19(H19), C24(H24), C21(H21),
 C22(H22), C16(H16), C23(H23), C13(H13), C7(H7), C6(H6), C5(H5), C8(H8),
 C15(H15), C14(H14)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Dy1 Dy 0.75879(2) 0.51855(2) 0.50802(2) 0.02558(10) Uani 1 1 d . . . A 1
Cu1 Cu -0.17033(10) 0.21701(7) -0.20527(7) 0.0712(3) Uani 1 1 d . . . B 1
Cu2 Cu 0.11149(8) 0.11538(8) 0.02080(8) 0.0718(3) Uani 1 1 d . . . C 1
Cu3B Cu 0.06534(18) 0.00763(19) 0.1997(2) 0.0854(6) Uani 0.725(4) 1 d . . P C 2
Cl2 Cl 0.1259(2) 0.18078(15) 0.20908(15) 0.0752(5) Uani 1 1 d . . . . .
Cl3 Cl 0.0056(2) -0.08834(16) 0.31260(18) 0.0828(6) Uani 1 1 d . . . . .
Cl1 Cl -0.12676(15) 0.08809(12) -0.06132(12) 0.0495(3) Uani 1 1 d . . . . .
O1W O 0.8985(4) 0.6625(3) 0.4608(3) 0.0409(9) Uani 1 1 d . . . . .
H1WA H 0.8517 0.6741 0.3966 0.061 Uiso 1 1 d GR . . A .
H1WB H 0.9829 0.6480 0.4600 0.061 Uiso 1 1 d GR . . . .
O1 O 0.6031(3) 0.3420(3) 0.4408(3) 0.0339(8) Uani 1 1 d . . . . .
O2 O 0.8236(3) 0.3522(3) 0.5568(3) 0.0354(8) Uani 1 1 d . . . . .
O2W O 0.6872(4) 0.6824(3) 0.5615(3) 0.0391(8) Uani 1 1 d . . . . .
H2WA H 0.7471 0.7154 0.6254 0.059 Uiso 1 1 d GR . . A .
H2WB H 0.5980 0.6705 0.5657 0.059 Uiso 1 1 d GR . . . .
O5 O 0.8610(4) 0.4508(3) 0.3847(3) 0.0398(8) Uani 1 1 d . . . . .
O4 O 0.5817(4) 0.5390(3) 0.3544(3) 0.0403(8) Uani 1 1 d . . . . .
O6 O 1.0474(3) 0.4148(3) 0.3332(3) 0.0393(8) Uani 1 1 d . . . . .
N2 N 0.0014(5) 0.3234(4) -0.1371(4) 0.0502(13) Uani 1 1 d . . . . .
N3 N 0.3111(5) 0.1516(4) 0.0170(4) 0.0527(13) Uani 1 1 d . . . . .
N1 N 0.3683(5) -0.1511(4) 0.2885(4) 0.0500(12) Uani 1 1 d . . . . .
C1 C 0.7054(5) 0.2981(4) 0.4908(4) 0.0307(10) Uani 1 1 d . . . . .
C2 C 0.6886(6) 0.1830(4) 0.4706(4) 0.0381(12) Uani 1 1 d . . . . .
H2 H 0.7652 0.1529 0.5079 0.046 Uiso 1 1 calc R . . . .
C17 C 0.9116(5) 0.4034(4) 0.3211(4) 0.0300(10) Uani 1 1 d . . . . .
C10 C 0.3838(6) 0.4974(4) 0.1948(4) 0.0394(12) Uani 1 1 d . . . . .
H10 H 0.4470 0.5169 0.1569 0.047 Uiso 1 1 calc R . . . .
C11 C 0.2474(5) 0.4551(4) 0.1383(4) 0.0377(12) Uani 1 1 d . . . . .
H11 H 0.1818 0.4425 0.1761 0.045 Uiso 1 1 calc R . . . .
C3 C 0.5698(6) 0.1214(4) 0.4021(4) 0.0380(12) Uani 1 1 d . . . . .
H3 H 0.4941 0.1537 0.3675 0.046 Uiso 1 1 calc R . . . .
C18 C 0.8127(5) 0.3288(4) 0.2243(4) 0.0386(12) Uani 1 1 d . . . . .
H18 H 0.8535 0.2952 0.1775 0.046 Uiso 1 1 calc R . . . .
C19 C 0.6687(5) 0.3079(4) 0.2015(4) 0.0380(12) Uani 1 1 d . . . . .
H19 H 0.6312 0.3414 0.2506 0.046 Uiso 1 1 calc R . . . .
C24 C 0.4160(5) 0.2155(4) 0.0999(4) 0.0439(13) Uani 1 1 d . . . . .
H24 H 0.3892 0.2474 0.1562 0.053 Uiso 1 1 calc R . . . .
C20 C 0.5622(6) 0.2370(4) 0.1066(4) 0.0419(13) Uani 1 1 d . . . . .
C21 C 0.6005(7) 0.1878(7) 0.0237(6) 0.081(3) Uani 1 1 d . . . . .
H21 H 0.6975 0.1987 0.0253 0.097 Uiso 1 1 calc R . . . .
C22 C 0.4927(8) 0.1220(8) -0.0618(7) 0.113(4) Uani 1 1 d . . . . .
H22 H 0.5169 0.0877 -0.1183 0.136 Uiso 1 1 calc R . . . .
C16 C 0.0577(6) 0.3591(4) -0.0298(4) 0.0437(13) Uani 1 1 d . . . . .
H16 H 0.0039 0.3373 0.0139 0.052 Uiso 1 1 calc R . . . .
C23 C 0.3497(8) 0.1072(7) -0.0635(6) 0.081(2) Uani 1 1 d . . . . .
H23 H 0.2778 0.0646 -0.1229 0.097 Uiso 1 1 calc R . . . .
C4 C 0.5447(6) 0.0071(4) 0.3748(4) 0.0394(12) Uani 1 1 d . . . . .
C12 C 0.1904(6) 0.4262(4) 0.0191(4) 0.0399(12) Uani 1 1 d . . . . .
C13 C 0.2676(6) 0.4597(5) -0.0479(5) 0.0533(16) Uani 1 1 d . . . . .
H13 H 0.3565 0.5065 -0.0185 0.064 Uiso 1 1 calc R . . . .
C7 C 0.4747(8) -0.2050(5) 0.3186(6) 0.0639(19) Uani 1 1 d . . . . .
H7 H 0.4513 -0.2775 0.3001 0.077 Uiso 1 1 calc R . . . .
C6 C 0.6174(8) -0.1587(5) 0.3756(7) 0.079(2) Uani 1 1 d . . . . .
H6 H 0.6886 -0.1994 0.3949 0.094 Uiso 1 1 calc R . . . .
C5 C 0.6537(7) -0.0513(5) 0.4039(6) 0.0637(19) Uani 1 1 d . . . . .
H5 H 0.7500 -0.0185 0.4420 0.076 Uiso 1 1 calc R . . . .
C8 C 0.4055(6) -0.0468(4) 0.3177(5) 0.0446(13) Uani 1 1 d . . . . .
H8 H 0.3318 -0.0083 0.2980 0.054 Uiso 1 1 calc R . . . .
C15 C 0.0787(7) 0.3551(5) -0.1999(5) 0.0587(18) Uani 1 1 d . . . . .
H15 H 0.0414 0.3302 -0.2741 0.070 Uiso 1 1 calc R . . . .
C14 C 0.2119(7) 0.4234(6) -0.1585(5) 0.0627(19) Uani 1 1 d . . . . .
H14 H 0.2632 0.4445 -0.2040 0.075 Uiso 1 1 calc R . . . .
O3WB O 0.984(6) 0.155(3) 0.399(6) 0.127(16) Uani 0.44(7) 1 d . . P D 2
H3WA H 0.9248 0.1937 0.4090 0.191 Uiso 0.44(7) 1 d G . P D 2
H3WB H 0.9349 0.0964 0.3603 0.191 Uiso 0.44(7) 1 d G . P D 2
C9 C 0.4446(5) 0.5163(4) 0.3152(4) 0.0287(10) Uani 1 1 d . . . . .
O3 O 0.3593(4) 0.5085(3) 0.3684(3) 0.0464(9) Uani 1 1 d . . . . .
O3WA O 1.031(3) 0.1294(18) 0.466(4) 0.110(9) Uani 0.56(7) 1 d . . P D 1
H3WC H 0.9935 0.0783 0.4892 0.165 Uiso 0.56(7) 1 d G . P D 1
H3WD H 1.0617 0.1063 0.4153 0.165 Uiso 0.56(7) 1 d G . P D 1
Cu3A Cu 0.0569(6) 0.0408(5) 0.2504(6) 0.0854(6) Uani 0.275(4) 1 d . . P C 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1W 2.420(3) . ?
Dy1 O1 2.476(3) . ?
Dy1 O2 2.462(3) . ?
Dy1 O2W 2.442(3) . ?
Dy1 O5 2.300(3) . ?
Dy1 O4 2.300(3) . ?
Dy1 O6 2.322(3) 2_766 ?
Dy1 O3 2.290(4) 2_666 ?
Cu1 Cl1 2.6673(18) . ?
Cu1 N2 1.916(4) . ?
Cu1 N1 1.920(5) 2 ?
Cu2 Cl2 2.474(2) . ?
Cu2 Cl1 2.2012(16) . ?
Cu2 N3 1.953(5) . ?
Cu3B Cl2 2.241(3) . ?
Cu3B Cl3 2.210(3) . ?
Cu3B Cl1 2.359(4) 2 ?
Cl2 Cu3A 2.055(7) . ?
Cl3 Cu3A 2.031(7) . ?
Cl1 Cu3B 2.359(4) 2 ?
O1W H1WA 0.8737 . ?
O1W H1WB 0.8726 . ?
O1 C1 1.273(6) . ?
O2 C1 1.264(5) . ?
O2W H2WA 0.8819 . ?
O2W H2WB 0.8810 . ?
O5 C17 1.242(6) . ?
O4 C9 1.255(5) . ?
O6 Dy1 2.322(3) 2_766 ?
O6 C17 1.269(5) . ?
N2 C16 1.344(7) . ?
N2 C15 1.339(8) . ?
N3 C24 1.340(7) . ?
N3 C23 1.325(9) . ?
N1 Cu1 1.920(5) 2 ?
N1 C7 1.328(8) . ?
N1 C8 1.339(7) . ?
C1 C2 1.476(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.315(7) . ?
C17 C18 1.481(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.311(7) . ?
C10 C9 1.487(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.475(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.465(7) . ?
C18 H18 0.9300 . ?
C18 C19 1.323(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.469(7) . ?
C24 H24 0.9300 . ?
C24 C20 1.386(7) . ?
C20 C21 1.374(8) . ?
C21 H21 0.9300 . ?
C21 C22 1.380(9) . ?
C22 H22 0.9300 . ?
C22 C23 1.373(10) . ?
C16 H16 0.9300 . ?
C16 C12 1.377(7) . ?
C23 H23 0.9300 . ?
C4 C5 1.388(8) . ?
C4 C8 1.373(7) . ?
C12 C13 1.390(8) . ?
C13 H13 0.9300 . ?
C13 C14 1.384(8) . ?
C7 H7 0.9300 . ?
C7 C6 1.372(9) . ?
C6 H6 0.9300 . ?
C6 C5 1.377(9) . ?
C5 H5 0.9300 . ?
C8 H8 0.9300 . ?
C15 H15 0.9300 . ?
C15 C14 1.381(8) . ?
C14 H14 0.9300 . ?
O3WB H3WA 0.8503 . ?
O3WB H3WB 0.8501 . ?
C9 O3 1.238(6) . ?
O3 Dy1 2.290(4) 2_666 ?
O3WA H3WC 0.8499 . ?
O3WA H3WD 0.8498 . ?

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
O1W Dy1 O1 145.13(12) . . ?
O1W Dy1 O2 130.27(12) . . ?
O1W Dy1 O2W 70.04(12) . . ?
O2 Dy1 O1 53.01(10) . . ?
O2W Dy1 O1 128.18(11) . . ?
O2W Dy1 O2 147.60(12) . . ?
O5 Dy1 O1W 71.71(13) . . ?
O5 Dy1 O1 78.98(12) . . ?
O5 Dy1 O2 72.71(13) . . ?
O5 Dy1 O2W 138.36(13) . . ?
O5 Dy1 O4 82.93(13) . . ?
O5 Dy1 O6 105.90(12) . 2_766 ?
O4 Dy1 O1W 81.63(12) . . ?
O4 Dy1 O1 76.33(12) . . ?
O4 Dy1 O2 126.55(12) . . ?
O4 Dy1 O2W 75.90(12) . . ?
O4 Dy1 O6 151.95(14) . 2_766 ?
O6 Dy1 O1W 76.31(13) 2_766 . ?
O6 Dy1 O1 131.07(12) 2_766 . ?
O6 Dy1 O2 81.34(12) 2_766 . ?
O6 Dy1 O2W 80.39(12) 2_766 . ?
O3 Dy1 O1W 138.44(13) 2_666 . ?
O3 Dy1 O1 74.36(13) 2_666 . ?
O3 Dy1 O2 78.48(13) 2_666 . ?
O3 Dy1 O2W 72.33(13) 2_666 . ?
O3 Dy1 O5 148.87(14) 2_666 . ?
O3 Dy1 O4 105.69(13) 2_666 . ?
O3 Dy1 O6 80.70(13) 2_666 2_766 ?
N2 Cu1 Cl1 99.41(15) . . ?
N2 Cu1 N1 160.5(2) . 2 ?
N1 Cu1 Cl1 97.05(15) 2 . ?
Cl1 Cu2 Cl2 100.68(7) . . ?
N3 Cu2 Cl2 105.38(16) . . ?
N3 Cu2 Cl1 149.93(16) . . ?
Cl2 Cu3B Cl1 112.10(12) . 2 ?
Cl3 Cu3B Cl2 132.61(17) . . ?
Cl3 Cu3B Cl1 113.79(12) . 2 ?
Cu3A Cl2 Cu2 98.7(2) . . ?
Cu2 Cl1 Cu1 106.25(6) . . ?
Dy1 O1W H1WA 110.8 . . ?
Dy1 O1W H1WB 110.2 . . ?
H1WA O1W H1WB 108.2 . . ?
C1 O1 Dy1 92.4(3) . . ?
C1 O2 Dy1 93.3(3) . . ?
Dy1 O2W H2WA 111.0 . . ?
Dy1 O2W H2WB 110.7 . . ?
H2WA O2W H2WB 107.9 . . ?
C17 O5 Dy1 172.8(3) . . ?
C9 O4 Dy1 136.9(3) . . ?
C17 O6 Dy1 127.2(3) . 2_766 ?
C16 N2 Cu1 124.7(4) . . ?
C15 N2 Cu1 116.9(4) . . ?
C15 N2 C16 118.0(5) . . ?
C24 N3 Cu2 121.0(4) . . ?
C23 N3 Cu2 121.0(4) . . ?
C23 N3 C24 117.7(5) . . ?
C7 N1 Cu1 122.5(4) . 2 ?
C7 N1 C8 116.8(5) . . ?
C8 N1 Cu1 120.7(4) . 2 ?
O1 C1 C2 120.3(4) . . ?
O2 C1 O1 120.6(4) . . ?
O2 C1 C2 119.0(4) . . ?
C1 C2 H2 118.7 . . ?
C3 C2 C1 122.7(5) . . ?
C3 C2 H2 118.7 . . ?
O5 C17 O6 123.7(4) . . ?
O5 C17 C18 120.4(4) . . ?
O6 C17 C18 116.0(4) . . ?
C11 C10 H10 117.6 . . ?
C11 C10 C9 124.7(5) . . ?
C9 C10 H10 117.6 . . ?
C10 C11 H11 117.6 . . ?
C10 C11 C12 124.8(5) . . ?
C12 C11 H11 117.6 . . ?
C2 C3 H3 116.7 . . ?
C2 C3 C4 126.6(5) . . ?
C4 C3 H3 116.7 . . ?
C17 C18 H18 118.6 . . ?
C19 C18 C17 122.9(5) . . ?
C19 C18 H18 118.6 . . ?
C18 C19 H19 116.7 . . ?
C18 C19 C20 126.6(5) . . ?
C20 C19 H19 116.7 . . ?
N3 C24 H24 118.0 . . ?
N3 C24 C20 123.9(5) . . ?
C20 C24 H24 118.0 . . ?
C24 C20 C19 119.5(5) . . ?
C21 C20 C19 123.1(5) . . ?
C21 C20 C24 117.4(5) . . ?
C20 C21 H21 120.5 . . ?
C20 C21 C22 118.9(6) . . ?
C22 C21 H21 120.5 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.0(7) . . ?
C23 C22 H22 120.0 . . ?
N2 C16 H16 118.1 . . ?
N2 C16 C12 123.8(5) . . ?
C12 C16 H16 118.1 . . ?
N3 C23 C22 122.1(6) . . ?
N3 C23 H23 119.0 . . ?
C22 C23 H23 119.0 . . ?
C5 C4 C3 123.9(5) . . ?
C8 C4 C3 119.0(5) . . ?
C8 C4 C5 117.1(5) . . ?
C16 C12 C11 119.6(5) . . ?
C16 C12 C13 117.2(5) . . ?
C13 C12 C11 123.2(5) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 119.9(5) . . ?
C14 C13 H13 120.0 . . ?
N1 C7 H7 118.4 . . ?
N1 C7 C6 123.2(6) . . ?
C6 C7 H7 118.4 . . ?
C7 C6 H6 120.4 . . ?
C7 C6 C5 119.2(6) . . ?
C5 C6 H6 120.4 . . ?
C4 C5 H5 120.5 . . ?
C6 C5 C4 119.0(6) . . ?
C6 C5 H5 120.5 . . ?
N1 C8 C4 124.7(5) . . ?
N1 C8 H8 117.6 . . ?
C4 C8 H8 117.6 . . ?
N2 C15 H15 118.8 . . ?
N2 C15 C14 122.4(5) . . ?
C14 C15 H15 118.8 . . ?
C13 C14 H14 120.7 . . ?
C15 C14 C13 118.6(6) . . ?
C15 C14 H14 120.7 . . ?
H3WA O3WB H3WB 109.4 . . ?
O4 C9 C10 115.6(4) . . ?
O3 C9 O4 125.3(4) . . ?
O3 C9 C10 119.1(4) . . ?
C9 O3 Dy1 167.7(4) . 2_666 ?
H3WC O3WA H3WD 109.5 . . ?
Cl3 Cu3A Cl2 172.1(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O1 C1 O2 7.8(5) . . . . ?
Dy1 O1 C1 C2 -170.8(4) . . . . ?
Dy1 O2 C1 O1 -7.9(5) . . . . ?
Dy1 O2 C1 C2 170.8(4) . . . . ?
Dy1 O4 C9 C10 -150.8(4) . . . . ?
Dy1 O4 C9 O3 29.1(8) . . . . ?
Dy1 O6 C17 O5 19.9(7) 2_766 . . . ?
Dy1 O6 C17 C18 -160.4(3) 2_766 . . . ?
Cu1 N2 C16 C12 171.9(4) . . . . ?
Cu1 N2 C15 C14 -173.4(6) . . . . ?
Cu1 N1 C7 C6 178.2(6) 2 . . . ?
Cu1 N1 C8 C4 -178.4(5) 2 . . . ?
Cu2 N3 C24 C20 174.1(5) . . . . ?
Cu2 N3 C23 C22 -172.3(8) . . . . ?
O1 C1 C2 C3 -0.4(8) . . . . ?
O2 C1 C2 C3 -179.1(5) . . . . ?
O5 C17 C18 C19 -1.0(8) . . . . ?
O4 C9 O3 Dy1 -33(2) . . . 2_666 ?
O6 C17 C18 C19 179.3(5) . . . . ?
N2 C16 C12 C11 -175.8(5) . . . . ?
N2 C16 C12 C13 1.4(9) . . . . ?
N2 C15 C14 C13 0.4(11) . . . . ?
N3 C24 C20 C19 -179.6(6) . . . . ?
N3 C24 C20 C21 -1.2(10) . . . . ?
N1 C7 C6 C5 0.2(13) . . . . ?
C1 C2 C3 C4 178.3(5) . . . . ?
C2 C3 C4 C5 -11.7(10) . . . . ?
C2 C3 C4 C8 167.8(6) . . . . ?
C17 C18 C19 C20 178.6(5) . . . . ?
C10 C11 C12 C16 163.4(6) . . . . ?
C10 C11 C12 C13 -13.6(9) . . . . ?
C10 C9 O3 Dy1 146.5(14) . . . 2_666 ?
C11 C10 C9 O4 167.3(5) . . . . ?
C11 C10 C9 O3 -12.6(8) . . . . ?
C11 C12 C13 C14 175.4(6) . . . . ?
C3 C4 C5 C6 178.9(7) . . . . ?
C3 C4 C8 N1 -179.6(5) . . . . ?
C18 C19 C20 C24 173.7(6) . . . . ?
C18 C19 C20 C21 -4.7(10) . . . . ?
C19 C20 C21 C22 179.6(8) . . . . ?
C24 N3 C23 C22 2.4(13) . . . . ?
C24 C20 C21 C22 1.2(12) . . . . ?
C20 C21 C22 C23 0.4(16) . . . . ?
C21 C22 C23 N3 -2.3(17) . . . . ?
C16 N2 C15 C14 -0.8(10) . . . . ?
C16 C12 C13 C14 -1.7(9) . . . . ?
C23 N3 C24 C20 -0.6(10) . . . . ?
C12 C13 C14 C15 0.8(11) . . . . ?
C7 N1 C8 C4 0.8(9) . . . . ?
C7 C6 C5 C4 0.6(13) . . . . ?
C5 C4 C8 N1 0.0(10) . . . . ?
C8 N1 C7 C6 -0.9(11) . . . . ?
C8 C4 C5 C6 -0.7(11) . . . . ?
C15 N2 C16 C12 -0.2(9) . . . . ?
C9 C10 C11 C12 -173.3(5) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 973519'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H24 Cl3 Cu3 Eu N3 O8, O'
_chemical_formula_sum            'C24 H24 Cl3 Cu3 Eu N3 O9'
_chemical_formula_weight         947.43
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7558(13)
_cell_length_b                   13.1043(17)
_cell_length_c                   13.1554(17)
_cell_angle_alpha                97.247(2)
_cell_angle_beta                 98.245(2)
_cell_angle_gamma                107.215(2)
_cell_volume                     1564.4(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2576
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.31
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.297
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'

_exptl_special_details           
; 
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1068 before and 0.0360 after correction.
The Ratio of minimum to maximum transmission is 0.7228.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.007
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   0.423
_exptl_transmission_factor_min   0.371
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8136
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.398
_diffrn_reflns_theta_min         1.653
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4591
_reflns_number_total             5759
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker, 2000-2003)'
_refine_diff_density_max         1.557
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5598
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0490
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0689P)²+1.7509P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1285
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C5) = Uanis(C6)
3. Others
 Sof(Cu3B)=1-FVAR(1)
 Sof(Cu3A)=FVAR(1)
 Sof(O3WB)=1-FVAR(2)
 Sof(O3WA)=FVAR(2)
4.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C8(H8), C7(H7), C16(H16), C13(H13), C14(H14), C15(H15),
 C24(H24), C23(H23), C22(H22), C21(H21), C10(H10), C11(H11), C2(H2), C3(H3),
 C18(H18), C19(H19)
4.c Fitted hexagon refined as free rotating group:
 C6(C5,C4,C8,N1,C7), C16(C12,C13,C14,C15,N2), C24(N3,C23,C22,C21,C20)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Cu3A Cu 0.9309(12) 0.3060(7) 0.4979(9) 0.034(5) Uani 0.125(13) 1 d . . P A 1
Cu3B Cu 0.9403(4) 0.2764(8) 0.4815(5) 0.203(2) Uani 0.875(13) 1 d . . P A 2
C6 C 0.5055(7) 0.5637(5) 0.3830(6) 0.107(3) Uani 1 1 d . . . . .
H6 H 0.4796 0.6202 0.4164 0.129 Uiso 1 1 calc R . . . .
C5 C 0.3995(5) 0.4772(5) 0.3156(6) 0.107(3) Uani 1 1 d G . . . .
H5 H 0.3026 0.4757 0.3039 0.129 Uiso 1 1 calc R . . . .
C4 C 0.4383(4) 0.3928(4) 0.2657(5) 0.0510(19) Uani 1 1 d G . . . .
C8 C 0.5832(5) 0.3951(4) 0.2832(4) 0.052(2) Uani 1 1 d G . . . .
H8 H 0.6091 0.3386 0.2497 0.062 Uiso 1 1 calc R . . . .
N1 N 0.6892(4) 0.4816(5) 0.3506(5) 0.068(2) Uani 1 1 d G . . . .
C7 C 0.6504(6) 0.5659(4) 0.4005(5) 0.107(3) Uani 1 1 d G . . . .
H7 H 0.7214 0.6239 0.4456 0.129 Uiso 1 1 calc R . . . .
C16 C 0.6003(4) 0.1860(4) 0.5433(3) 0.053(2) Uani 1 1 d . . . . .
H16 H 0.6723 0.2065 0.5037 0.064 Uiso 1 1 calc R . . . .
C12 C 0.4575(5) 0.1271(5) 0.4943(3) 0.0441(17) Uani 1 1 d G . . . .
C13 C 0.3500(4) 0.0964(5) 0.5535(4) 0.074(3) Uani 1 1 d G . . . .
H13 H 0.2545 0.0570 0.5207 0.088 Uiso 1 1 calc R . . . .
C14 C 0.3853(6) 0.1244(6) 0.6617(4) 0.087(3) Uani 1 1 d G . . . .
H14 H 0.3134 0.1039 0.7013 0.104 Uiso 1 1 calc R . . . .
C15 C 0.5281(6) 0.1833(5) 0.7107(3) 0.073(3) Uani 1 1 d G . . . .
H15 H 0.5517 0.2020 0.7831 0.087 Uiso 1 1 calc R . . . .
N2 N 0.6356(5) 0.2140(4) 0.6515(3) 0.0615(19) Uani 1 1 d G . . . .
C24 C 1.0588(5) 0.4754(3) 0.8595(4) 0.0500(19) Uani 1 1 d . . . . .
H24 H 1.0077 0.5211 0.8380 0.060 Uiso 1 1 calc R . . . .
N3 N 1.0013(4) 0.3642(4) 0.8230(4) 0.0548(17) Uani 1 1 d G . . . .
C23 C 1.0776(6) 0.2959(3) 0.8551(4) 0.063(2) Uani 1 1 d G . . . .
H23 H 1.0392 0.2215 0.8307 0.075 Uiso 1 1 calc R . . . .
C22 C 1.2114(6) 0.3389(4) 0.9236(5) 0.065(2) Uani 1 1 d G . . . .
H22 H 1.2625 0.2932 0.9451 0.078 Uiso 1 1 calc R . . . .
C21 C 1.2688(4) 0.4501(4) 0.9600(4) 0.057(2) Uani 1 1 d G . . . .
H21 H 1.3584 0.4789 1.0059 0.068 Uiso 1 1 calc R . . . .
C20 C 1.1925(5) 0.5184(3) 0.9280(4) 0.0464(18) Uani 1 1 d G . . . .
Eu1 Eu 0.23909(3) -0.00937(3) -0.01858(3) 0.03053(13) Uani 1 1 d . . . . .
Cu2 Cu 0.83207(14) 0.29759(11) 0.71652(10) 0.0828(4) Uani 1 1 d . . . . .
Cu1 Cu 0.88764(13) 0.47667(14) 0.38616(12) 0.0954(5) Uani 1 1 d . . . . .
Cl2 Cl 0.8772(2) 0.4397(2) 0.58941(18) 0.0659(6) Uani 1 1 d . . . . .
Cl1 Cl 0.8750(4) 0.2880(3) 0.3214(3) 0.1020(10) Uani 1 1 d . . . . .
Cl3 Cl 0.9944(4) 0.1863(3) 0.5891(3) 0.1095(11) Uani 1 1 d . . . . .
O4 O 0.3959(5) 0.0608(4) 0.1607(4) 0.0373(11) Uani 1 1 d . . . . .
O3 O 0.1771(5) -0.0562(4) 0.1514(4) 0.0404(11) Uani 1 1 d . . . . .
O1 O 0.1335(5) 0.1164(4) 0.0501(4) 0.0440(12) Uani 1 1 d . . . . .
O1W O 0.0966(5) 0.0352(4) -0.1658(4) 0.0444(12) Uani 1 1 d . . . . .
H1WA H 0.1485 0.0935 -0.1851 0.067 Uiso 1 1 d GR . . . .
H1WB H 0.0190 0.0469 -0.1481 0.067 Uiso 1 1 d GR . . . .
O2W O 0.3152(5) -0.0632(4) -0.1834(4) 0.0458(12) Uani 1 1 d . . . . .
H2WA H 0.2596 -0.1288 -0.2148 0.069 Uiso 1 1 d GR . . . .
H2WB H 0.4061 -0.0632 -0.1711 0.069 Uiso 1 1 d GR . . . .
O5 O 1.3663(6) 0.8691(5) 1.0109(4) 0.0543(14) Uani 1 1 d . . . . .
C9 C 0.2949(7) 0.0117(6) 0.2046(5) 0.0354(15) Uani 1 1 d . . . . .
O6 O 1.5854(5) 0.8505(4) 1.0394(4) 0.0473(13) Uani 1 1 d . . . . .
C10 C 0.3135(8) 0.0319(6) 0.3199(5) 0.0412(17) Uani 1 1 d . . . . .
H10 H 0.2383 -0.0060 0.3504 0.049 Uiso 1 1 calc R . . . .
C11 C 0.4303(8) 0.1001(7) 0.3803(6) 0.0452(18) Uani 1 1 d . . . . .
H11 H 0.5045 0.1355 0.3477 0.054 Uiso 1 1 calc R . . . .
C2 C 0.1890(8) 0.2791(6) 0.1717(6) 0.0451(18) Uani 1 1 d . . . . .
H2 H 0.1503 0.3277 0.2056 0.054 Uiso 1 1 calc R . . . .
C3 C 0.3303(7) 0.2995(6) 0.1925(6) 0.0413(17) Uani 1 1 d . . . . .
H3 H 0.3669 0.2500 0.1576 0.050 Uiso 1 1 calc R . . . .
C1 C 0.0860(7) 0.1833(5) 0.0971(5) 0.0317(14) Uani 1 1 d . . . . .
C17 C 1.4475(7) 0.8142(5) 1.0174(5) 0.0312(14) Uani 1 1 d . . . . .
C18 C 1.3870(8) 0.6929(6) 0.9979(6) 0.0427(17) Uani 1 1 d . . . . .
H18 H 1.4502 0.6542 1.0155 0.051 Uiso 1 1 calc R . . . .
C19 C 1.2481(8) 0.6373(6) 0.9568(6) 0.0442(17) Uani 1 1 d . . . . .
H19 H 1.1826 0.6758 0.9457 0.053 Uiso 1 1 calc R . . . .
O3WB O 0.972(3) 0.037(4) 0.3714(19) 0.162(18) Uani 0.74(7) 1 d . . P B 2
O2 O -0.0474(5) 0.1753(4) 0.0858(4) 0.0473(13) Uani 1 1 d . . . . .
O3WA O 1.025(9) 0.109(6) 0.340(4) 0.15(2) Uani 0.26(7) 1 d . . P B 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu3A Cu1 2.924(12) . ?
Cu3A Cu1 2.952(8) 2_766 ?
Cu3A Cl2 2.233(9) . ?
Cu3A Cl1 2.273(12) . ?
Cu3A Cl3 2.263(13) . ?
C6 H6 0.9300 . ?
C6 C5 1.3900 . ?
C6 C7 1.3900 . ?
C5 H5 0.9300 . ?
C5 C4 1.3900 . ?
C4 C8 1.3900 . ?
C4 C3 1.478(8) . ?
C8 H8 0.9300 . ?
C8 N1 1.3900 . ?
N1 C7 1.3900 . ?
N1 Cu1 1.947(4) . ?
C7 H7 0.9300 . ?
C16 H16 0.9300 . ?
C16 C12 1.3900 . ?
C16 N2 1.3900 . ?
C12 C13 1.3900 . ?
C12 C11 1.463(8) . ?
C13 H13 0.9300 . ?
C13 C14 1.3900 . ?
C14 H14 0.9300 . ?
C14 C15 1.3900 . ?
C15 H15 0.9300 . ?
C15 N2 1.3900 . ?
N2 Cu2 1.912(4) . ?
C24 H24 0.9300 . ?
C24 N3 1.3900 . ?
C24 C20 1.3900 . ?
N3 C23 1.3900 . ?
N3 Cu2 1.904(3) . ?
C23 H23 0.9300 . ?
C23 C22 1.3900 . ?
C22 H22 0.9300 . ?
C22 C21 1.3900 . ?
C21 H21 0.9300 . ?
C21 C20 1.3900 . ?
C20 C19 1.469(8) . ?
Eu1 O4 2.517(4) . ?
Eu1 O3 2.501(5) . ?
Eu1 O1 2.343(5) . ?
Eu1 O1W 2.453(5) . ?
Eu1 O2W 2.476(5) . ?
Eu1 O5 2.328(5) 1_444 ?
Eu1 O6 2.347(5) 2_766 ?
Eu1 C1 3.241(6) 2 ?
Eu1 O2 2.375(5) 2 ?
Cu2 Cl2 2.640(3) . ?
Cu1 Cu3A 2.952(8) 2_766 ?
Cu1 Cl2 2.186(3) 2_766 ?
Cu1 Cl1 2.472(4) . ?
Cl2 Cu1 2.186(3) 2_766 ?
O4 C9 1.265(8) . ?
O3 C9 1.269(8) . ?
O1 C1 1.245(8) . ?
O1W H1WA 0.8731 . ?
O1W H1WB 0.8719 . ?
O2W H2WA 0.8798 . ?
O2W H2WB 0.8789 . ?
O5 Eu1 2.328(5) 1_666 ?
O5 C17 1.218(8) . ?
C9 C10 1.482(10) . ?
O6 Eu1 2.347(5) 2_766 ?
O6 C17 1.263(8) . ?
C10 H10 0.9300 . ?
C10 C11 1.299(10) . ?
C11 H11 0.9300 . ?
C2 H2 0.9300 . ?
C2 C3 1.305(9) . ?
C2 C1 1.486(9) . ?
C3 H3 0.9300 . ?
C1 Eu1 3.241(6) 2 ?
C1 O2 1.260(7) . ?
C17 C18 1.497(10) . ?
C18 H18 0.9300 . ?
C18 C19 1.328(10) . ?
C19 H19 0.9300 . ?
O2 Eu1 2.375(5) 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
Cu1 Cu3A Cu1 68.8(2) . 2_766 ?
Cl2 Cu3A Cu1 47.41(16) . 2_766 ?
Cl2 Cu3A Cu1 63.8(3) . . ?
Cl2 Cu3A Cl1 115.8(5) . . ?
Cl2 Cu3A Cl3 116.3(5) . . ?
Cl1 Cu3A Cu1 116.6(4) . 2_766 ?
Cl1 Cu3A Cu1 55.1(3) . . ?
Cl3 Cu3A Cu1 105.7(4) . 2_766 ?
Cl3 Cu3A Cu1 172.8(5) . . ?
Cl3 Cu3A Cl1 126.9(4) . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C4 C8 120.0 . . ?
C5 C4 C3 122.3(4) . . ?
C8 C4 C3 117.7(4) . . ?
C4 C8 H8 120.0 . . ?
N1 C8 C4 120.0 . . ?
N1 C8 H8 120.0 . . ?
C8 N1 C7 120.0 . . ?
C8 N1 Cu1 119.7(3) . . ?
C7 N1 Cu1 120.0(3) . . ?
C6 C7 H7 120.0 . . ?
N1 C7 C6 120.0 . . ?
N1 C7 H7 120.0 . . ?
C12 C16 H16 120.0 . . ?
C12 C16 N2 120.0 . . ?
N2 C16 H16 120.0 . . ?
C16 C12 C13 120.0 . . ?
C16 C12 C11 116.4(4) . . ?
C13 C12 C11 123.6(4) . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 120.0 . . ?
C13 C14 C15 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 H15 120.0 . . ?
N2 C15 C14 120.0 . . ?
N2 C15 H15 120.0 . . ?
C16 N2 Cu2 119.0(3) . . ?
C15 N2 C16 120.0 . . ?
C15 N2 Cu2 120.9(3) . . ?
N3 C24 H24 120.0 . . ?
N3 C24 C20 120.0 . . ?
C20 C24 H24 120.0 . . ?
C24 N3 Cu2 123.9(3) . . ?
C23 N3 C24 120.0 . . ?
C23 N3 Cu2 115.7(3) . . ?
N3 C23 H23 120.0 . . ?
C22 C23 N3 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C22 H22 120.0 . . ?
C23 C22 C21 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C21 H21 120.0 . . ?
C20 C21 C22 120.0 . . ?
C20 C21 H21 120.0 . . ?
C24 C20 C19 115.8(4) . . ?
C21 C20 C24 120.0 . . ?
C21 C20 C19 124.1(4) . . ?
O4 Eu1 C1 131.37(15) . 2 ?
O3 Eu1 O4 52.13(15) . . ?
O3 Eu1 C1 79.25(15) . 2 ?
O1 Eu1 O4 78.65(16) . . ?
O1 Eu1 O3 72.60(17) . . ?
O1 Eu1 O1W 72.47(17) . . ?
O1 Eu1 O2W 138.52(18) . . ?
O1 Eu1 O6 81.89(18) . 2_766 ?
O1 Eu1 C1 88.76(16) . 2 ?
O1 Eu1 O2 107.39(17) . 2 ?
O1W Eu1 O4 145.65(17) . . ?
O1W Eu1 O3 131.09(15) . . ?
O1W Eu1 O2W 69.80(16) . . ?
O1W Eu1 C1 66.88(16) . 2 ?
O2W Eu1 O4 127.84(15) . . ?
O2W Eu1 O3 147.94(17) . . ?
O2W Eu1 C1 91.86(16) . 2 ?
O5 Eu1 O4 73.59(17) 1_444 . ?
O5 Eu1 O3 78.61(18) 1_444 . ?
O5 Eu1 O1 148.46(19) 1_444 . ?
O5 Eu1 O1W 138.44(18) 1_444 . ?
O5 Eu1 O2W 72.26(18) 1_444 . ?
O5 Eu1 O6 105.47(19) 1_444 2_766 ?
O5 Eu1 C1 98.39(18) 1_444 2 ?
O5 Eu1 O2 80.56(18) 1_444 2 ?
O6 Eu1 O4 76.55(17) 2_766 . ?
O6 Eu1 O3 125.65(18) 2_766 . ?
O6 Eu1 O1W 81.27(17) 2_766 . ?
O6 Eu1 O2W 76.03(18) 2_766 . ?
O6 Eu1 C1 148.14(17) 2_766 2 ?
O6 Eu1 O2 152.2(2) 2_766 2 ?
O2 Eu1 O4 130.44(17) 2 . ?
O2 Eu1 O3 82.01(17) 2 . ?
O2 Eu1 O1W 77.00(18) 2 . ?
O2 Eu1 O2W 80.31(17) 2 . ?
O2 Eu1 C1 18.97(16) 2 2 ?
N2 Cu2 Cl2 97.85(17) . . ?
N3 Cu2 N2 159.6(2) . . ?
N3 Cu2 Cl2 99.77(17) . . ?
Cu3A Cu1 Cu3A 111.2(2) . 2_766 ?
N1 Cu1 Cu3A 106.8(3) . 2_766 ?
N1 Cu1 Cu3A 117.7(3) . . ?
N1 Cu1 Cl2 148.6(2) . 2_766 ?
N1 Cu1 Cl1 105.91(19) . . ?
Cl2 Cu1 Cu3A 48.8(2) 2_766 2_766 ?
Cl2 Cu1 Cu3A 92.2(2) 2_766 . ?
Cl2 Cu1 Cl1 101.12(12) 2_766 . ?
Cl1 Cu1 Cu3A 48.9(2) . . ?
Cl1 Cu1 Cu3A 147.2(2) . 2_766 ?
Cu3A Cl2 Cu2 80.6(3) . . ?
Cu1 Cl2 Cu3A 83.8(3) 2_766 . ?
Cu1 Cl2 Cu2 108.07(10) 2_766 . ?
Cu3A Cl1 Cu1 75.9(2) . . ?
C9 O4 Eu1 92.8(4) . . ?
C9 O3 Eu1 93.4(4) . . ?
C1 O1 Eu1 173.0(5) . . ?
Eu1 O1W H1WA 110.6 . . ?
Eu1 O1W H1WB 110.3 . . ?
H1WA O1W H1WB 108.3 . . ?
Eu1 O2W H2WA 110.9 . . ?
Eu1 O2W H2WB 110.7 . . ?
H2WA O2W H2WB 108.0 . . ?
C17 O5 Eu1 169.9(5) . 1_666 ?
O4 C9 O3 121.0(6) . . ?
O4 C9 C10 120.2(6) . . ?
O3 C9 C10 118.9(6) . . ?
C17 O6 Eu1 134.2(4) . 2_766 ?
C9 C10 H10 118.5 . . ?
C11 C10 C9 122.9(7) . . ?
C11 C10 H10 118.5 . . ?
C12 C11 H11 116.5 . . ?
C10 C11 C12 126.9(7) . . ?
C10 C11 H11 116.5 . . ?
C3 C2 H2 118.0 . . ?
C3 C2 C1 124.1(7) . . ?
C1 C2 H2 118.0 . . ?
C4 C3 H3 116.6 . . ?
C2 C3 C4 126.7(6) . . ?
C2 C3 H3 116.6 . . ?
O1 C1 Eu1 87.8(4) . 2 ?
O1 C1 C2 119.9(6) . . ?
O1 C1 O2 123.8(6) . . ?
C2 C1 Eu1 149.8(5) . 2 ?
O2 C1 Eu1 37.8(3) . 2 ?
O2 C1 C2 116.2(6) . . ?
O5 C17 O6 125.5(7) . . ?
O5 C17 C18 120.7(6) . . ?
O6 C17 C18 113.7(6) . . ?
C17 C18 H18 118.1 . . ?
C19 C18 C17 123.7(7) . . ?
C19 C18 H18 118.1 . . ?
C20 C19 H19 118.3 . . ?
C18 C19 C20 123.4(6) . . ?
C18 C19 H19 118.3 . . ?
C1 O2 Eu1 123.2(4) . 2 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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 973520'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H24 Cl3 Cu3 Gd N3 O8, O'
_chemical_formula_sum            'C24 H24 Cl3 Cu3 Gd N3 O9'
_chemical_formula_weight         952.68
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.750(2)
_cell_length_b                   13.103(3)
_cell_length_c                   13.133(3)
_cell_angle_alpha                97.405(3)
_cell_angle_beta                 98.215(3)
_cell_angle_gamma                107.290(3)
_cell_volume                     1559.3(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2531
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.72
_cell_measurement_theta_min      2.48
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.427
_exptl_absorpt_correction_T_max  25.394
_exptl_absorpt_correction_T_min  1.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   0.413
_exptl_transmission_factor_min   0.359
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8109
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.394
_diffrn_reflns_theta_min         1.655
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4573
_reflns_number_total             5741
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker, 2000-2003)'
_refine_diff_density_max         1.749
_refine_diff_density_min         -2.060
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         5566
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0561
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0899P)²+1.2491P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1547
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C18(H18), C19(H19), C15(H15), C13(H13), C16(H16), C14(H14),
 C23(H23), C22(H22), C7(H7), C6(H6), C8(H8), C10(H10), C11(H11), C5(H5),
 C21(H21), C24(H24)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Gd1 Gd 0.76040(4) 0.50903(3) 0.51894(3) 0.03232(16) Uani 1 1 d . . . . .
Cu1 Cu 0.16778(18) 0.20212(13) -0.21599(13) 0.0903(5) Uani 1 1 d . . . . .
Cu3 Cu 0.11156(16) 0.02197(18) 0.11296(15) 0.1048(6) Uani 1 1 d . . . . .
Cu2 Cu 0.0622(3) 0.2162(3) 0.0149(3) 0.1980(16) Uani 1 1 d . . . . .
Cl1 Cl 0.1221(3) 0.0601(3) -0.0896(2) 0.0757(8) Uani 1 1 d . . . . .
Cl2 Cl 0.1251(5) 0.2124(3) 0.1789(3) 0.1123(13) Uani 1 1 d . . . . .
Cl3 Cl 0.0071(5) 0.3146(4) -0.0886(4) 0.1194(14) Uani 1 1 d . . . . .
O2W O 0.6858(6) 0.5641(5) 0.6824(5) 0.0477(14) Uani 1 1 d . . . . .
H2WA H 0.7536 0.6217 0.7196 0.072 Uiso 1 1 d GR . . . .
H2WB H 0.6723 0.5125 0.7196 0.072 Uiso 1 1 d GR . . . .
O5 O -0.5836(6) -0.3519(4) -0.5399(5) 0.0443(14) Uani 1 1 d . . . . .
O2 O 0.8233(6) 0.5557(4) 0.3503(4) 0.0415(13) Uani 1 1 d . . . . .
O3 O 0.6046(6) 0.4386(4) 0.3400(4) 0.0416(13) Uani 1 1 d . . . . .
O3W O 0.9007(6) 0.4619(5) 0.6637(5) 0.0499(15) Uani 1 1 d . . . . .
H3WA H 0.9084 0.5053 0.7219 0.075 Uiso 1 1 d GR . . . .
H3WB H 0.9883 0.4674 0.6526 0.075 Uiso 1 1 d GR . . . .
O1 O 0.9526(6) 0.6736(5) 0.5866(5) 0.0509(15) Uani 1 1 d . . . . .
O4 O 0.8653(7) 0.3838(5) 0.4504(5) 0.0489(15) Uani 1 1 d . . . . .
N1 N 1.6889(9) 0.9819(8) 0.8486(8) 0.074(3) Uani 1 1 d . . . . .
N3 N -0.0022(9) 0.1362(6) -0.3220(7) 0.061(2) Uani 1 1 d . . . . .
N2 N 0.3681(10) 0.2850(7) -0.1498(7) 0.062(2) Uani 1 1 d . . . . .
C17 C -0.4478(8) -0.3152(6) -0.5173(6) 0.0352(17) Uani 1 1 d . . . . .
C2 C 1.1903(8) 0.7795(6) 0.6717(7) 0.046(2) Uani 1 1 d . . . . .
H2 H 1.1514 0.8280 0.7056 0.055 Uiso 1 1 calc R . . . .
C3 C 1.3319(9) 0.8002(6) 0.6926(7) 0.045(2) Uani 1 1 d . . . . .
H3 H 1.3683 0.7502 0.6584 0.054 Uiso 1 1 calc R . . . .
C18 C -0.3857(9) -0.1935(7) -0.4982(7) 0.046(2) Uani 1 1 d . . . . .
H18 H -0.4485 -0.1551 -0.5174 0.055 Uiso 1 1 calc R . . . .
C19 C -0.2506(10) -0.1382(7) -0.4569(7) 0.050(2) Uani 1 1 d . . . . .
H19 H -0.1853 -0.1767 -0.4452 0.060 Uiso 1 1 calc R . . . .
C15 C 0.4674(15) 0.3172(10) -0.2044(8) 0.082(4) Uani 1 1 d . . . . .
H15 H 0.4414 0.3009 -0.2770 0.098 Uiso 1 1 calc R . . . .
C13 C 0.6486(12) 0.4028(9) -0.0547(8) 0.069(3) Uani 1 1 d . . . . .
H13 H 0.7450 0.4415 -0.0228 0.082 Uiso 1 1 calc R . . . .
C16 C 0.4045(11) 0.3153(8) -0.0466(8) 0.057(2) Uani 1 1 d . . . . .
H16 H 0.3315 0.2957 -0.0076 0.069 Uiso 1 1 calc R . . . .
C14 C 0.6117(14) 0.3752(10) -0.1587(9) 0.084(4) Uani 1 1 d . . . . .
H14 H 0.6818 0.3946 -0.2000 0.101 Uiso 1 1 calc R . . . .
C23 C -0.0764(13) 0.1996(8) -0.3548(9) 0.070(3) Uani 1 1 d . . . . .
H23 H -0.0360 0.2742 -0.3313 0.084 Uiso 1 1 calc R . . . .
C22 C -0.2125(11) 0.1599(8) -0.4230(9) 0.068(3) Uani 1 1 d . . . . .
H22 H -0.2645 0.2058 -0.4421 0.082 Uiso 1 1 calc R . . . .
C7 C 1.6499(15) 1.0635(11) 0.8967(14) 0.108(6) Uani 1 1 d . . . . .
H7 H 1.7209 1.1221 0.9414 0.130 Uiso 1 1 calc R . . . .
C6 C 1.5099(19) 1.0611(12) 0.8809(16) 0.147(9) Uani 1 1 d . . . . .
H6 H 1.4858 1.1183 0.9150 0.177 Uiso 1 1 calc R . . . .
C4 C 1.4388(9) 0.8932(7) 0.7637(9) 0.056(2) Uani 1 1 d . . . . .
C8 C 1.5844(9) 0.9005(8) 0.7867(8) 0.054(2) Uani 1 1 d . . . . .
H8 H 1.6109 0.8431 0.7559 0.065 Uiso 1 1 calc R . . . .
C12 C 0.5427(10) 0.3734(7) 0.0055(7) 0.049(2) Uani 1 1 d . . . . .
C9 C 0.7045(8) 0.4896(6) 0.2974(6) 0.0368(17) Uani 1 1 d . . . . .
C10 C 0.6866(10) 0.4675(7) 0.1816(7) 0.047(2) Uani 1 1 d . . . . .
H10 H 0.7625 0.5048 0.1512 0.057 Uiso 1 1 calc R . . . .
C11 C 0.5695(10) 0.3981(7) 0.1202(7) 0.046(2) Uani 1 1 d . . . . .
H11 H 0.4960 0.3607 0.1524 0.055 Uiso 1 1 calc R . . . .
C1 C 1.0861(8) 0.6819(6) 0.5959(6) 0.0388(18) Uani 1 1 d . . . . .
C5 C 1.4025(14) 0.9775(10) 0.8165(13) 0.115(7) Uani 1 1 d . . . . .
H5 H 1.3058 0.9765 0.8078 0.138 Uiso 1 1 calc R . . . .
C20 C -0.1933(10) -0.0194(7) -0.4273(7) 0.050(2) Uani 1 1 d . . . . .
C21 C -0.2657(10) 0.0490(7) -0.4604(9) 0.060(3) Uani 1 1 d . . . . .
H21 H -0.3527 0.0202 -0.5093 0.071 Uiso 1 1 calc R . . . .
C24 C -0.0587(10) 0.0280(8) -0.3577(8) 0.054(2) Uani 1 1 d . . . . .
H24 H -0.0065 -0.0166 -0.3354 0.065 Uiso 1 1 calc R . . . .
O1W O 0.0216(19) 0.456(2) 0.1305(13) 0.283(14) Uani 1 1 d . . . . .
O6 O -0.3662(7) -0.3697(5) -0.5100(6) 0.0584(17) 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
Gd1 O2W 2.453(5) . ?
Gd1 O5 2.336(5) 2 ?
Gd1 O2 2.484(6) . ?
Gd1 O3 2.504(6) . ?
Gd1 O3W 2.435(6) . ?
Gd1 O1 2.362(5) . ?
Gd1 O4 2.330(5) . ?
Gd1 C9 2.846(8) . ?
Gd1 O6 2.319(6) 1_666 ?
Cu1 Cl1 2.633(3) . ?
Cu1 N3 1.900(8) . ?
Cu1 N2 1.939(9) . ?
Cu3 Cl1 2.168(3) 2 ?
Cu3 Cl2 2.492(4) . ?
Cu3 N1 1.956(9) 2_766 ?
Cu2 Cl1 2.574(6) . ?
Cu2 Cl2 2.164(6) . ?
Cu2 Cl3 2.111(6) . ?
Cl1 Cu3 2.168(3) 2 ?
O2W H2WA 0.8726 . ?
O2W H2WB 0.8739 . ?
O5 Gd1 2.336(5) 2 ?
O5 C17 1.242(9) . ?
O2 C9 1.262(9) . ?
O3 C9 1.254(9) . ?
O3W H3WA 0.8708 . ?
O3W H3WB 0.8705 . ?
O1 C1 1.260(9) . ?
O4 C1 1.235(9) 2_766 ?
N1 Cu3 1.956(9) 2_766 ?
N1 C7 1.351(16) . ?
N1 C8 1.315(12) . ?
N3 C23 1.327(13) . ?
N3 C24 1.350(12) . ?
N2 C15 1.290(15) . ?
N2 C16 1.327(13) . ?
C17 C18 1.500(11) . ?
C17 O6 1.220(9) . ?
C2 H2 0.9300 . ?
C2 C3 1.306(11) . ?
C2 C1 1.506(11) . ?
C3 H3 0.9300 . ?
C3 C4 1.454(12) . ?
C18 H18 0.9300 . ?
C18 C19 1.297(12) . ?
C19 H19 0.9300 . ?
C19 C20 1.467(12) . ?
C15 H15 0.9300 . ?
C15 C14 1.386(17) . ?
C13 H13 0.9300 . ?
C13 C14 1.335(16) . ?
C13 C12 1.383(13) . ?
C16 H16 0.9300 . ?
C16 C12 1.362(13) . ?
C14 H14 0.9300 . ?
C23 H23 0.9300 . ?
C23 C22 1.402(15) . ?
C22 H22 0.9300 . ?
C22 C21 1.385(13) . ?
C7 H7 0.9300 . ?
C7 C6 1.341(19) . ?
C6 H6 0.9300 . ?
C6 C5 1.356(17) . ?
C4 C8 1.380(12) . ?
C4 C5 1.390(15) . ?
C8 H8 0.9300 . ?
C12 C11 1.468(12) . ?
C9 C10 1.487(12) . ?
C10 H10 0.9300 . ?
C10 C11 1.308(12) . ?
C11 H11 0.9300 . ?
C1 O4 1.235(9) 2_766 ?
C5 H5 0.9300 . ?
C20 C21 1.372(13) . ?
C20 C24 1.403(12) . ?
C21 H21 0.9300 . ?
C24 H24 0.9300 . ?
O6 Gd1 2.319(6) 1_444 ?

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
O2W Gd1 O2 147.5(2) . . ?
O2W Gd1 O3 128.05(18) . . ?
O2W Gd1 C9 145.7(2) . . ?
O5 Gd1 O2W 76.0(2) 2 . ?
O5 Gd1 O2 126.1(2) 2 . ?
O5 Gd1 O3 76.56(19) 2 . ?
O5 Gd1 O3W 80.9(2) 2 . ?
O5 Gd1 O1 152.0(2) 2 . ?
O5 Gd1 C9 100.9(2) 2 . ?
O2 Gd1 O3 52.33(17) . . ?
O2 Gd1 C9 26.28(19) . . ?
O3 Gd1 C9 26.12(19) . . ?
O3W Gd1 O2W 70.6(2) . . ?
O3W Gd1 O2 130.72(18) . . ?
O3W Gd1 O3 144.6(2) . . ?
O3W Gd1 C9 143.5(2) . . ?
O1 Gd1 O2W 80.0(2) . . ?
O1 Gd1 O2 81.9(2) . . ?
O1 Gd1 O3 130.7(2) . . ?
O1 Gd1 O3W 77.5(2) . . ?
O1 Gd1 C9 107.1(2) . . ?
O4 Gd1 O2W 138.9(2) . . ?
O4 Gd1 O5 82.5(2) . 2 ?
O4 Gd1 O2 72.5(2) . . ?
O4 Gd1 O3 78.5(2) . . ?
O4 Gd1 O3W 71.7(2) . . ?
O4 Gd1 O1 107.1(2) . . ?
O4 Gd1 C9 72.4(2) . . ?
O6 Gd1 O2W 71.9(2) 1_666 . ?
O6 Gd1 O5 104.9(2) 1_666 2 ?
O6 Gd1 O2 78.8(2) 1_666 . ?
O6 Gd1 O3 73.8(2) 1_666 . ?
O6 Gd1 O3W 139.2(2) 1_666 . ?
O6 Gd1 O1 80.9(2) 1_666 . ?
O6 Gd1 O4 148.5(2) 1_666 . ?
O6 Gd1 C9 76.2(2) 1_666 . ?
N3 Cu1 Cl1 99.7(3) . . ?
N3 Cu1 N2 160.0(4) . . ?
N2 Cu1 Cl1 97.4(3) . . ?
Cl1 Cu3 Cl2 100.77(16) 2 . ?
N1 Cu3 Cl1 148.8(3) 2_766 2 ?
N1 Cu3 Cl2 105.2(3) 2_766 . ?
Cl2 Cu2 Cl1 106.89(19) . . ?
Cl3 Cu2 Cl1 108.9(2) . . ?
Cl3 Cu2 Cl2 142.9(3) . . ?
Cu3 Cl1 Cu1 108.18(14) 2 . ?
Cu3 Cl1 Cu2 83.80(13) 2 . ?
Cu2 Cl1 Cu1 79.78(12) . . ?
Cu2 Cl2 Cu3 83.96(18) . . ?
Gd1 O2W H2WA 109.9 . . ?
Gd1 O2W H2WB 111.1 . . ?
H2WA O2W H2WB 108.2 . . ?
C17 O5 Gd1 135.0(5) . 2 ?
C9 O2 Gd1 93.1(5) . . ?
C9 O3 Gd1 92.4(5) . . ?
Gd1 O3W H3WA 110.4 . . ?
Gd1 O3W H3WB 110.4 . . ?
H3WA O3W H3WB 108.4 . . ?
C1 O1 Gd1 123.6(5) . . ?
C1 O4 Gd1 173.5(6) 2_766 . ?
C7 N1 Cu3 119.8(8) . 2_766 ?
C8 N1 Cu3 122.2(8) . 2_766 ?
C8 N1 C7 117.4(10) . . ?
C23 N3 Cu1 117.4(7) . . ?
C23 N3 C24 118.6(8) . . ?
C24 N3 Cu1 123.7(7) . . ?
C15 N2 Cu1 121.4(8) . . ?
C15 N2 C16 118.1(10) . . ?
C16 N2 Cu1 120.4(7) . . ?
O5 C17 C18 114.8(7) . . ?
O6 C17 O5 125.3(7) . . ?
O6 C17 C18 120.0(7) . . ?
C3 C2 H2 118.0 . . ?
C3 C2 C1 124.0(7) . . ?
C1 C2 H2 118.0 . . ?
C2 C3 H3 116.5 . . ?
C2 C3 C4 126.9(8) . . ?
C4 C3 H3 116.5 . . ?
C17 C18 H18 117.7 . . ?
C19 C18 C17 124.6(8) . . ?
C19 C18 H18 117.7 . . ?
C18 C19 H19 117.6 . . ?
C18 C19 C20 124.7(9) . . ?
C20 C19 H19 117.6 . . ?
N2 C15 H15 118.8 . . ?
N2 C15 C14 122.3(10) . . ?
C14 C15 H15 118.8 . . ?
C14 C13 H13 120.2 . . ?
C14 C13 C12 119.6(10) . . ?
C12 C13 H13 120.2 . . ?
N2 C16 H16 118.1 . . ?
N2 C16 C12 123.8(9) . . ?
C12 C16 H16 118.1 . . ?
C15 C14 H14 120.4 . . ?
C13 C14 C15 119.2(10) . . ?
C13 C14 H14 120.4 . . ?
N3 C23 H23 118.3 . . ?
N3 C23 C22 123.4(9) . . ?
C22 C23 H23 118.3 . . ?
C23 C22 H22 121.7 . . ?
C21 C22 C23 116.7(10) . . ?
C21 C22 H22 121.7 . . ?
N1 C7 H7 119.6 . . ?
C6 C7 N1 120.8(12) . . ?
C6 C7 H7 119.6 . . ?
C7 C6 H6 119.1 . . ?
C7 C6 C5 121.7(13) . . ?
C5 C6 H6 119.1 . . ?
C8 C4 C3 121.3(8) . . ?
C8 C4 C5 115.3(9) . . ?
C5 C4 C3 123.4(9) . . ?
N1 C8 C4 125.5(10) . . ?
N1 C8 H8 117.2 . . ?
C4 C8 H8 117.2 . . ?
C13 C12 C11 124.8(9) . . ?
C16 C12 C13 116.8(9) . . ?
C16 C12 C11 118.3(8) . . ?
O2 C9 Gd1 60.6(4) . . ?
O2 C9 C10 118.7(7) . . ?
O3 C9 Gd1 61.5(4) . . ?
O3 C9 O2 121.9(7) . . ?
O3 C9 C10 119.3(7) . . ?
C10 C9 Gd1 171.6(6) . . ?
C9 C10 H10 118.4 . . ?
C11 C10 C9 123.3(8) . . ?
C11 C10 H10 118.4 . . ?
C12 C11 H11 116.8 . . ?
C10 C11 C12 126.4(8) . . ?
C10 C11 H11 116.8 . . ?
O1 C1 C2 115.6(7) . . ?
O4 C1 O1 125.0(8) 2_766 . ?
O4 C1 C2 119.4(7) 2_766 . ?
C6 C5 C4 119.2(12) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C21 C20 C19 124.0(8) . . ?
C21 C20 C24 117.3(8) . . ?
C24 C20 C19 118.6(8) . . ?
C22 C21 H21 119.2 . . ?
C20 C21 C22 121.6(9) . . ?
C20 C21 H21 119.2 . . ?
N3 C24 C20 122.3(9) . . ?
N3 C24 H24 118.8 . . ?
C20 C24 H24 118.8 . . ?
C17 O6 Gd1 170.1(6) . 1_444 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 973522'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H24 Cl3 Cu3 N3 O8 Tb, O'
_chemical_formula_sum            'C24 H24 Cl3 Cu3 N3 O9 Tb'
_chemical_formula_weight         954.33
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7468(13)
_cell_length_b                   13.1256(17)
_cell_length_c                   13.1381(17)
_cell_angle_alpha                97.029(2)
_cell_angle_beta                 98.260(2)
_cell_angle_gamma                107.433(2)
_cell_volume                     1562.4(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5752
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.396
_cell_measurement_theta_min      2.083
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.559
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       green
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   0.402
_exptl_transmission_factor_min   0.348
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8231
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.396
_diffrn_reflns_theta_min         2.083
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4999
_reflns_number_total             5752
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Apex2 (Bruker, 2005)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'Apex2 (Bruker, 2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker, 2000-2003)'
_refine_diff_density_max         1.697
_refine_diff_density_min         -2.714
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         5650
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0453
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0606P)²+5.9457P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1200
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Sof(O3WB)=1-FVAR(1)
 Sof(O3WA)=FVAR(1)
3.a Free rotating group:
 O3WB(O3WA)
3.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C2(H2), C3(H3), C16(H16), C18(H18), C19(H19), C24(H24),
 C23(H23), C6(H6), C8(H8), C15(H15), C13(H13), C14(H14), C5(H5), C7(H7),
 C21(H21), C22(H22)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.75926(3) 1.00835(2) 0.51847(2) 0.02640(12) Uani 1 1 d . . . A 1
Cu2 Cu 0.06340(18) 0.7113(2) 0.01435(18) 0.1433(9) Uani 1 1 d . . . A 1
Cu1 Cu 0.16959(14) 0.70440(10) -0.21676(9) 0.0737(4) Uani 1 1 d . . . A 1
Cu3 Cu -0.11183(12) 0.47824(12) -0.11485(11) 0.0774(4) Uani 1 1 d . . . A 1
Cl1 Cl 0.1256(2) 0.56111(18) -0.08831(16) 0.0535(5) Uani 1 1 d . . . A 1
Cl3 Cl 0.1258(3) 0.7102(2) 0.1801(2) 0.0823(8) Uani 1 1 d . . . A 1
Cl2 Cl 0.0059(4) 0.8132(3) -0.0883(2) 0.0892(8) Uani 1 1 d . . . A 1
O1W O 0.6863(5) 1.0631(4) 0.6818(4) 0.0407(11) Uani 1 1 d . . . A 1
H1WA H 0.7503 1.1231 0.7160 0.061 Uiso 1 1 d GR . . A 1
H1WB H 0.6801 1.0137 0.7204 0.061 Uiso 1 1 d GR . . A 1
O1 O 0.9518(5) 1.1689(4) 0.5853(4) 0.0401(11) Uani 1 1 d . . . A 1
O2W O 0.8989(5) 0.9598(4) 0.6631(4) 0.0406(11) Uani 1 1 d . . . A 1
H2WA H 0.9149 1.0068 0.7224 0.061 Uiso 1 1 d GR . . A 1
H2WB H 0.9863 0.9591 0.6504 0.061 Uiso 1 1 d GR . . A 1
O3 O 0.6037(5) 0.9403(4) 0.3411(3) 0.0355(10) Uani 1 1 d . . . A 1
O4 O 0.8235(5) 1.0561(4) 0.3513(3) 0.0355(10) Uani 1 1 d . . . A 1
O5 O -0.5830(5) 0.1472(4) -0.5390(4) 0.0416(11) Uani 1 1 d . . . A 1
O6 O -0.3617(6) 0.1317(4) -0.5097(4) 0.0487(13) Uani 1 1 d . . . A 1
N3 N -0.0023(7) 0.6361(5) -0.3226(5) 0.0512(17) Uani 1 1 d . . . A 1
N1 N 1.6896(7) 1.4829(6) 0.8482(6) 0.0566(18) Uani 1 1 d . . . A 1
N2 N 0.3671(7) 0.7881(5) -0.1514(5) 0.0521(17) Uani 1 1 d . . . A 1
C9 C 0.7047(7) 0.9903(5) 0.2969(5) 0.0326(14) Uani 1 1 d . . . A 1
C17 C -0.4454(7) 0.1854(5) -0.5168(5) 0.0278(13) Uani 1 1 d . . . A 1
C10 C 0.6877(8) 0.9700(6) 0.1825(5) 0.0390(16) Uani 1 1 d . . . A 1
H10 H 0.7637 1.0081 0.1524 0.047 Uiso 1 1 calc R . . A 1
C11 C 0.5701(8) 0.9006(6) 0.1208(5) 0.0394(16) Uani 1 1 d . . . A 1
H11 H 0.4958 0.8642 0.1531 0.047 Uiso 1 1 calc R . . A 1
C12 C 0.5435(8) 0.8742(6) 0.0063(5) 0.0401(16) Uani 1 1 d . . . A 1
O2 O 1.1369(5) 1.1154(4) 0.5493(4) 0.0406(11) Uani 1 1 d . . . A 1
C2 C 1.1880(7) 1.2772(5) 0.6708(6) 0.0397(16) Uani 1 1 d . . . A 1
H2 H 1.1483 1.3255 0.7035 0.048 Uiso 1 1 calc R . . A 1
C3 C 1.3310(7) 1.2980(5) 0.6920(5) 0.0379(16) Uani 1 1 d . . . A 1
H3 H 1.3679 1.2479 0.6592 0.045 Uiso 1 1 calc R . . A 1
C4 C 1.4377(8) 1.3930(6) 0.7629(6) 0.0450(18) Uani 1 1 d . . . A 1
C16 C 0.4038(8) 0.8154(6) -0.0466(6) 0.0465(18) Uani 1 1 d . . . A 1
H16 H 0.3309 0.7935 -0.0078 0.056 Uiso 1 1 calc R . . A 1
C18 C -0.3854(7) 0.3056(5) -0.4973(6) 0.0374(15) Uani 1 1 d . . . A 1
H18 H -0.4491 0.3437 -0.5156 0.045 Uiso 1 1 calc R . . A 1
C19 C -0.2474(8) 0.3622(5) -0.4558(6) 0.0404(16) Uani 1 1 d . . . A 1
H19 H -0.1814 0.3243 -0.4444 0.049 Uiso 1 1 calc R . . A 1
C20 C -0.1917(8) 0.4809(6) -0.4264(6) 0.0416(16) Uani 1 1 d . . . A 1
C24 C -0.0582(8) 0.5295(6) -0.3580(6) 0.0458(18) Uani 1 1 d . . . A 1
H24 H -0.0051 0.4854 -0.3357 0.055 Uiso 1 1 calc R . . A 1
C23 C -0.0780(10) 0.6997(6) -0.3556(7) 0.057(2) Uani 1 1 d . . . A 1
H23 H -0.0392 0.7741 -0.3319 0.069 Uiso 1 1 calc R . . A 1
C6 C 1.5081(13) 1.5621(10) 0.8785(12) 0.124(6) Uani 1 1 d . . . A 1
H6 H 1.4846 1.6197 0.9114 0.149 Uiso 1 1 calc R . . A 1
C8 C 1.5841(7) 1.3989(6) 0.7844(6) 0.0449(17) Uani 1 1 d . . . A 1
H8 H 1.6107 1.3420 0.7532 0.054 Uiso 1 1 calc R . . A 1
C15 C 0.4726(11) 0.8166(8) -0.2054(6) 0.066(3) Uani 1 1 d . . . A 1
H15 H 0.4492 0.7962 -0.2778 0.079 Uiso 1 1 calc R . . A 1
C13 C 0.6528(10) 0.9028(8) -0.0520(7) 0.067(3) Uani 1 1 d . . . A 1
H13 H 0.7493 0.9401 -0.0194 0.080 Uiso 1 1 calc R . . A 1
C14 C 0.6150(11) 0.8746(9) -0.1599(7) 0.079(3) Uani 1 1 d . . . A 1
H14 H 0.6855 0.8949 -0.2010 0.095 Uiso 1 1 calc R . . A 1
C5 C 1.4007(11) 1.4771(8) 0.8135(9) 0.084(4) Uani 1 1 d . . . A 1
H5 H 1.3038 1.4760 0.8035 0.101 Uiso 1 1 calc R . . A 1
C7 C 1.6501(11) 1.5620(8) 0.8949(10) 0.089(4) Uani 1 1 d . . . A 1
H7 H 1.7212 1.6196 0.9403 0.107 Uiso 1 1 calc R . . A 1
C21 C -0.2672(9) 0.5484(7) -0.4601(7) 0.057(2) Uani 1 1 d . . . A 1
H21 H -0.3555 0.5194 -0.5075 0.068 Uiso 1 1 calc R . . A 1
C22 C -0.2116(10) 0.6590(6) -0.4234(7) 0.061(2) Uani 1 1 d . . . A 1
H22 H -0.2629 0.7047 -0.4440 0.074 Uiso 1 1 calc R . . A 1
C1 C 1.0872(7) 1.1798(5) 0.5965(5) 0.0304(13) Uani 1 1 d . . . A 1
O3WB O 0.975(3) 0.037(4) 0.8682(16) 0.130(13) Uani 0.66(6) 1 d . . P B 2
O3WA O 1.023(6) 0.112(4) 0.855(3) 0.16(2) Uani 0.34(6) 1 d G . P B 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1W 2.448(4) . ?
Tb1 O1 2.331(4) . ?
Tb1 O2W 2.437(5) . ?
Tb1 O3 2.489(4) . ?
Tb1 O4 2.472(5) . ?
Tb1 O5 2.315(5) 2_565 ?
Tb1 O6 2.305(5) 1_666 ?
Tb1 O2 2.312(4) 2_776 ?
Cu2 Cl1 2.524(4) . ?
Cu2 Cl3 2.178(4) . ?
Cu2 Cl2 2.144(4) . ?
Cu1 Cl1 2.659(2) . ?
Cu1 N3 1.915(6) . ?
Cu1 N2 1.917(6) . ?
Cu3 Cl1 2.197(2) . ?
Cu3 Cl3 2.474(3) 2_565 ?
Cu3 N1 1.948(7) 1_344 ?
Cl3 Cu3 2.474(3) 2_565 ?
O1W H1WA 0.8654 . ?
O1W H1WB 0.8643 . ?
O1 C1 1.269(8) . ?
O2W H2WA 0.8950 . ?
O2W H2WB 0.8942 . ?
O3 C9 1.267(8) . ?
O4 C9 1.269(8) . ?
O5 Tb1 2.315(5) 2_565 ?
O5 C17 1.258(8) . ?
O6 Tb1 2.305(5) 1_444 ?
O6 C17 1.228(8) . ?
N3 C24 1.335(9) . ?
N3 C23 1.340(11) . ?
N1 Cu3 1.948(7) 1_766 ?
N1 C8 1.350(9) . ?
N1 C7 1.324(12) . ?
N2 C16 1.347(10) . ?
N2 C15 1.322(11) . ?
C9 C10 1.471(9) . ?
C17 C18 1.485(9) . ?
C10 H10 0.9300 . ?
C10 C11 1.315(10) . ?
C11 H11 0.9300 . ?
C11 C12 1.468(10) . ?
C12 C16 1.378(10) . ?
C12 C13 1.388(11) . ?
O2 Tb1 2.312(4) 2_776 ?
O2 C1 1.241(8) . ?
C2 H2 0.9300 . ?
C2 C3 1.318(9) . ?
C2 C1 1.489(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.472(9) . ?
C4 C8 1.391(10) . ?
C4 C5 1.385(11) . ?
C16 H16 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.323(9) . ?
C19 H19 0.9300 . ?
C19 C20 1.469(9) . ?
C20 C24 1.391(10) . ?
C20 C21 1.384(11) . ?
C24 H24 0.9300 . ?
C23 H23 0.9300 . ?
C23 C22 1.381(12) . ?
C6 H6 0.9300 . ?
C6 C5 1.370(13) . ?
C6 C7 1.370(15) . ?
C8 H8 0.9300 . ?
C15 H15 0.9300 . ?
C15 C14 1.372(13) . ?
C13 H13 0.9300 . ?
C13 C14 1.386(12) . ?
C14 H14 0.9300 . ?
C5 H5 0.9300 . ?
C7 H7 0.9300 . ?
C21 H21 0.9300 . ?
C21 C22 1.383(11) . ?
C22 H22 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1W Tb1 O3 128.12(15) . . ?
O1W Tb1 O4 147.41(17) . . ?
O1 Tb1 O1W 80.00(16) . . ?
O1 Tb1 O2W 77.06(17) . . ?
O1 Tb1 O3 130.89(17) . . ?
O1 Tb1 O4 81.70(16) . . ?
O2W Tb1 O1W 70.44(16) . . ?
O2W Tb1 O3 144.72(16) . . ?
O2W Tb1 O4 130.55(16) . . ?
O4 Tb1 O3 52.64(14) . . ?
O5 Tb1 O1W 76.36(17) 2_565 . ?
O5 Tb1 O1 151.94(18) 2_565 . ?
O5 Tb1 O2W 80.92(17) 2_565 . ?
O5 Tb1 O3 76.49(17) 2_565 . ?
O5 Tb1 O4 126.19(16) 2_565 . ?
O6 Tb1 O1W 72.05(18) 1_666 . ?
O6 Tb1 O1 80.58(18) 1_666 . ?
O6 Tb1 O2W 138.93(18) 1_666 . ?
O6 Tb1 O3 74.12(17) 1_666 . ?
O6 Tb1 O4 78.52(18) 1_666 . ?
O6 Tb1 O5 105.87(19) 1_666 2_565 ?
O6 Tb1 O2 148.67(19) 1_666 2_776 ?
O2 Tb1 O1W 138.81(18) 2_776 . ?
O2 Tb1 O1 106.32(17) 2_776 . ?
O2 Tb1 O2W 71.56(17) 2_776 . ?
O2 Tb1 O3 78.89(16) 2_776 . ?
O2 Tb1 O4 72.52(17) 2_776 . ?
O2 Tb1 O5 82.57(18) 2_776 2_565 ?
Cl3 Cu2 Cl1 108.34(13) . . ?
Cl2 Cu2 Cl1 109.73(14) . . ?
Cl2 Cu2 Cl3 140.58(18) . . ?
N3 Cu1 Cl1 99.2(2) . . ?
N3 Cu1 N2 160.5(3) . . ?
N2 Cu1 Cl1 97.4(2) . . ?
Cl1 Cu3 Cl3 100.96(10) . 2_565 ?
N1 Cu3 Cl1 149.1(2) 1_344 . ?
N1 Cu3 Cl3 105.6(2) 1_344 2_565 ?
Cu2 Cl1 Cu1 80.34(8) . . ?
Cu3 Cl1 Cu2 83.37(9) . . ?
Cu3 Cl1 Cu1 106.81(9) . . ?
Cu2 Cl3 Cu3 82.62(11) . 2_565 ?
Tb1 O1W H1WA 110.1 . . ?
Tb1 O1W H1WB 110.3 . . ?
H1WA O1W H1WB 108.7 . . ?
C1 O1 Tb1 125.9(4) . . ?
Tb1 O2W H2WA 111.5 . . ?
Tb1 O2W H2WB 111.6 . . ?
H2WA O2W H2WB 107.2 . . ?
C9 O3 Tb1 92.9(4) . . ?
C9 O4 Tb1 93.7(4) . . ?
C17 O5 Tb1 136.0(4) . 2_565 ?
C17 O6 Tb1 168.2(5) . 1_444 ?
C24 N3 Cu1 124.7(5) . . ?
C24 N3 C23 118.3(7) . . ?
C23 N3 Cu1 116.8(5) . . ?
C8 N1 Cu3 120.8(6) . 1_766 ?
C7 N1 Cu3 120.8(6) . 1_766 ?
C7 N1 C8 117.9(7) . . ?
C16 N2 Cu1 120.1(6) . . ?
C15 N2 Cu1 122.2(5) . . ?
C15 N2 C16 117.6(7) . . ?
O3 C9 O4 120.3(6) . . ?
O3 C9 C10 120.5(6) . . ?
O4 C9 C10 119.2(6) . . ?
O5 C17 C18 114.8(5) . . ?
O6 C17 O5 125.4(6) . . ?
O6 C17 C18 119.8(6) . . ?
C9 C10 H10 118.5 . . ?
C11 C10 C9 123.0(7) . . ?
C11 C10 H10 118.5 . . ?
C10 C11 H11 116.5 . . ?
C10 C11 C12 127.0(7) . . ?
C12 C11 H11 116.5 . . ?
C16 C12 C11 118.7(7) . . ?
C16 C12 C13 117.8(7) . . ?
C13 C12 C11 123.5(7) . . ?
C1 O2 Tb1 172.9(5) . 2_776 ?
C3 C2 H2 118.6 . . ?
C3 C2 C1 122.9(6) . . ?
C1 C2 H2 118.6 . . ?
C2 C3 H3 117.0 . . ?
C2 C3 C4 126.1(6) . . ?
C4 C3 H3 117.0 . . ?
C8 C4 C3 119.3(7) . . ?
C5 C4 C3 123.8(7) . . ?
C5 C4 C8 116.9(7) . . ?
N2 C16 C12 123.6(7) . . ?
N2 C16 H16 118.2 . . ?
C12 C16 H16 118.2 . . ?
C17 C18 H18 117.8 . . ?
C19 C18 C17 124.3(6) . . ?
C19 C18 H18 117.8 . . ?
C18 C19 H19 117.9 . . ?
C18 C19 C20 124.2(7) . . ?
C20 C19 H19 117.9 . . ?
C24 C20 C19 119.0(7) . . ?
C21 C20 C19 123.7(7) . . ?
C21 C20 C24 117.2(7) . . ?
N3 C24 C20 123.4(7) . . ?
N3 C24 H24 118.3 . . ?
C20 C24 H24 118.3 . . ?
N3 C23 H23 118.7 . . ?
N3 C23 C22 122.6(7) . . ?
C22 C23 H23 118.7 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C7 C6 C5 120.0(10) . . ?
N1 C8 C4 123.4(7) . . ?
N1 C8 H8 118.3 . . ?
C4 C8 H8 118.3 . . ?
N2 C15 H15 118.5 . . ?
N2 C15 C14 123.1(8) . . ?
C14 C15 H15 118.5 . . ?
C12 C13 H13 120.7 . . ?
C14 C13 C12 118.6(8) . . ?
C14 C13 H13 120.7 . . ?
C15 C14 C13 119.2(8) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C4 C5 H5 120.3 . . ?
C6 C5 C4 119.5(9) . . ?
C6 C5 H5 120.3 . . ?
N1 C7 C6 122.3(9) . . ?
N1 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
C20 C21 H21 119.9 . . ?
C22 C21 C20 120.2(7) . . ?
C22 C21 H21 119.9 . . ?
C23 C22 C21 118.4(8) . . ?
C23 C22 H22 120.8 . . ?
C21 C22 H22 120.8 . . ?
O1 C1 C2 116.1(6) . . ?
O2 C1 O1 123.7(6) . . ?
O2 C1 C2 120.2(6) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 973523'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C24 H22 Cu Dy I N3 O8), H2 O'
_chemical_formula_sum            'C48 H46 Cu2 Dy2 I2 N6 O17'
_chemical_formula_weight         1684.81
_chemical_melting_point          ?
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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.007(3)
_cell_length_b                   9.3047(12)
_cell_length_c                   29.380(5)
_cell_angle_alpha                90
_cell_angle_beta                 110.4860(10)
_cell_angle_gamma                90
_cell_volume                     5635.6(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6736
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.880
_cell_measurement_theta_min      1.480
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.533
_exptl_absorpt_correction_T_max  0.404
_exptl_absorpt_correction_T_min  0.350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            16519
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.880
_diffrn_reflns_theta_min         1.480
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5358
_reflns_number_total             6736
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Apex2 (Bruker, 2005)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'Apex2 (Bruker, 2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker, 2000-2003)'
_refine_diff_density_max         1.143
_refine_diff_density_min         -1.207
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6418
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0321
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0375P)²+5.7283P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0836
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O3W-H3WA = O3W-H3WB = O3B-H3BA = O3B-H3BB = O1W-H1WA = O1W-H1WB = O2W-H2WA =
 O2W-H2WB
 0.82 with sigma of 0.01
 H3WA-H3WB = H3BA-H3BB = H1WA-H1WB = H2WA-H2WB
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O3W \\sim O3B: within 3.8A with sigma of 0.02 and sigma for terminal atoms of
0.04
4. Others
 Sof(O3B)=Sof(H3BA)=Sof(H3BB)=0.5*(1-FVAR(2))
 Sof(O3W)=Sof(H3WA)=Sof(H3WB)=0.5*FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
  C24(H24)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Dy1 Dy 0.22972(2) 0.01597(2) 0.48763(2) 0.02791(7) Uani 1 1 d . . . . .
Cu1 Cu 0.06145(3) 0.81872(7) 0.25189(2) 0.04412(15) Uani 1 1 d . . . . .
I1 I -0.03420(2) 0.88217(4) 0.16951(2) 0.04581(10) Uani 1 1 d . . . . .
O1W O 0.21156(15) -0.1420(3) 0.41324(11) 0.0358(7) Uani 1 1 d D . . . .
H1WA H 0.1733(8) -0.137(4) 0.3959(16) 0.054 Uiso 1 1 d DR . . . .
H1WB H 0.2254(18) -0.225(2) 0.4199(17) 0.054 Uiso 1 1 d DR . . . .
O1 O 0.31402(14) -0.1430(3) 0.50881(11) 0.0394(7) Uani 1 1 d . . . . .
O2 O 0.35876(14) -0.3589(3) 0.52143(11) 0.0367(7) Uani 1 1 d . . . . .
O2W O 0.28914(16) 0.1109(3) 0.43894(12) 0.0395(7) Uani 1 1 d D . . . .
H2WA H 0.296(2) 0.1977(13) 0.4395(19) 0.059 Uiso 1 1 d DR . . . .
H2WB H 0.313(2) 0.062(4) 0.429(2) 0.059 Uiso 1 1 d DR . . . .
O3 O 0.19685(14) 0.3063(3) 0.46304(10) 0.0350(7) Uani 1 1 d . . . . .
O4 O 0.14546(15) 0.1223(3) 0.42064(11) 0.0387(7) Uani 1 1 d . . . A 1
O5 O 0.17439(15) 0.8907(3) 0.04122(11) 0.0367(7) Uani 1 1 d . . . B 1
O6 O 0.24220(15) 1.0688(3) 0.07260(10) 0.0362(7) Uani 1 1 d . . . B 1
N1 N 0.6190(2) 0.0374(5) 0.58798(16) 0.0501(11) Uani 1 1 d . . . C 1
N2 N 0.07582(19) 0.5989(4) 0.24837(13) 0.0381(9) Uani 1 1 d . . . A 1
N3 N 0.14407(19) 0.9262(5) 0.25338(13) 0.0408(9) Uani 1 1 d . . . B 1
C1 C 0.36179(19) -0.2250(4) 0.52197(13) 0.0279(8) Uani 1 1 d . . . C 1
C2 C 0.4282(2) -0.1605(5) 0.54069(16) 0.0373(10) Uani 1 1 d . . . C 1
H2 H 0.4637 -0.2221 0.5512 0.045 Uiso 1 1 calc R . . C 1
C3 C 0.4390(2) -0.0208(5) 0.54310(17) 0.0364(10) Uani 1 1 d . . . C 1
H3 H 0.4027 0.0388 0.5329 0.044 Uiso 1 1 calc R . . C 1
C4 C 0.5026(2) 0.0499(5) 0.56037(16) 0.0377(10) Uani 1 1 d . . . C 1
C5 C 0.5063(3) 0.1985(6) 0.5642(2) 0.0519(13) Uani 1 1 d . . . C 1
H5 H 0.4688 0.2538 0.5562 0.062 Uiso 1 1 calc R . . C 1
C6 C 0.5673(3) 0.2634(6) 0.5801(2) 0.0619(16) Uani 1 1 d . . . C 1
H6 H 0.5710 0.3627 0.5832 0.074 Uiso 1 1 calc R . . C 1
C7 C 0.6211(3) 0.1803(6) 0.5911(2) 0.0568(15) Uani 1 1 d . . . C 1
H7 H 0.6614 0.2252 0.6012 0.068 Uiso 1 1 calc R . . C 1
C8 C 0.5602(2) -0.0232(6) 0.57322(18) 0.0436(12) Uani 1 1 d . . . C 1
H8 H 0.5582 -0.1230 0.5716 0.052 Uiso 1 1 calc R . . C 1
C9 C 0.16018(18) 0.2522(4) 0.42356(13) 0.0284(8) Uani 1 1 d . . . A 1
C10 C 0.1382(2) 0.3442(5) 0.37967(15) 0.0352(10) Uani 1 1 d . . . A 1
H10 H 0.1426 0.4433 0.3833 0.042 Uiso 1 1 calc R . . A 1
C11 C 0.1129(2) 0.2908(5) 0.33606(15) 0.0384(10) Uani 1 1 d . . . A 1
H11 H 0.1052 0.1923 0.3337 0.046 Uiso 1 1 calc R . . A 1
C12 C 0.0953(2) 0.3716(5) 0.29006(15) 0.0375(10) Uani 1 1 d . . . A 1
C13 C 0.0808(3) 0.3000(6) 0.24609(18) 0.0582(15) Uani 1 1 d . . . A 1
H13 H 0.0815 0.2002 0.2449 0.070 Uiso 1 1 calc R . . A 1
C14 C 0.0650(3) 0.3819(7) 0.20364(18) 0.0636(17) Uani 1 1 d . . . A 1
H14 H 0.0557 0.3369 0.1737 0.076 Uiso 1 1 calc R . . A 1
C15 C 0.0632(3) 0.5272(6) 0.20629(17) 0.0506(13) Uani 1 1 d . . . A 1
H15 H 0.0528 0.5798 0.1777 0.061 Uiso 1 1 calc R . . A 1
C16 C 0.0914(2) 0.5197(5) 0.28869(16) 0.0364(10) Uani 1 1 d . . . A 1
H16 H 0.1002 0.5679 0.3180 0.044 Uiso 1 1 calc R . . A 1
C17 C 0.2027(2) 0.9738(5) 0.07632(16) 0.0346(10) Uani 1 1 d . . . B 1
C18 C 0.1902(2) 0.9543(5) 0.12207(17) 0.0399(11) Uani 1 1 d . . . B 1
H18 H 0.1586 0.8884 0.1224 0.048 Uiso 1 1 calc R . . B 1
C19 C 0.2209(2) 1.0239(5) 0.16228(17) 0.0411(11) Uani 1 1 d . . . B 1
H19 H 0.2525 1.0887 0.1613 0.049 Uiso 1 1 calc R . . B 1
C20 C 0.2106(2) 1.0105(5) 0.20866(17) 0.0396(11) Uani 1 1 d . . . B 1
C21 C 0.2550(3) 1.0618(8) 0.2509(2) 0.0662(17) Uani 1 1 d . . . B 1
H21 H 0.2919 1.1095 0.2505 0.079 Uiso 1 1 calc R . . B 1
C22 C 0.2444(3) 1.0417(9) 0.2947(2) 0.077(2) Uani 1 1 d . . . B 1
H22 H 0.2745 1.0741 0.3238 0.092 Uiso 1 1 calc R . . B 1
C23 C 0.1895(3) 0.9745(7) 0.29398(18) 0.0547(14) Uani 1 1 d . . . B 1
H23 H 0.1830 0.9611 0.3233 0.066 Uiso 1 1 calc R . . B 1
C24 C 0.1553(2) 0.9456(5) 0.21167(16) 0.0399(11) Uani 1 1 d . . . B 1
H24 H 0.1240 0.9136 0.1830 0.048 Uiso 1 1 calc R . . B 1
O3W O 0.049(2) 0.900(5) 0.032(3) 0.187(14) Uani 0.157(10) 1 d D U P D 1
H3WA H 0.022(13) 0.94(5) 0.041(10) 0.281 Uiso 0.157(10) 1 d DR . P D 1
H3WB H 0.053(15) 0.93(5) 0.007(7) 0.281 Uiso 0.157(10) 1 d DR . P D 1
O3B O -0.0187(12) 0.982(2) 0.0467(11) 0.175(11) Uani 0.343(10) 1 d D U P D 2
H3BA H -0.040(14) 1.03(3) 0.024(8) 0.263 Uiso 0.343(10) 1 d DR . P D 2
H3BB H 0.013(10) 0.94(3) 0.044(12) 0.263 Uiso 0.343(10) 1 d DR . P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1W 2.547(3) . ?
Dy1 O1 2.282(3) . ?
Dy1 O2 2.374(3) 7_546 ?
Dy1 O2W 2.418(3) . ?
Dy1 O3 2.824(3) . ?
Dy1 O3 2.410(3) 7_556 ?
Dy1 O4 2.395(3) . ?
Dy1 O5 2.461(3) 6_566 ?
Dy1 O6 2.540(3) 6_566 ?
Dy1 C9 2.949(4) . ?
Dy1 C17 2.869(4) 6_566 ?
Cu1 Cu1 2.6677(12) 2 ?
Cu1 I1 2.6592(7) . ?
Cu1 I1 2.6475(8) 2 ?
Cu1 N2 2.078(4) . ?
Cu1 N3 2.062(4) . ?
I1 Cu1 2.6475(7) 2 ?
O1W H1WA 0.818(10) . ?
O1W H1WB 0.829(10) . ?
O1 C1 1.246(5) . ?
O2 Dy1 2.374(3) 7_546 ?
O2 C1 1.247(5) . ?
O2W H2WA 0.820(10) . ?
O2W H2WB 0.825(10) . ?
O3 Dy1 2.410(3) 7_556 ?
O3 C9 1.263(4) . ?
O4 C9 1.246(5) . ?
O5 Dy1 2.461(3) 6_565 ?
O5 C17 1.264(5) . ?
O6 Dy1 2.540(3) 6_565 ?
O6 C17 1.271(5) . ?
N1 C7 1.333(7) . ?
N1 C8 1.337(6) . ?
N2 C15 1.346(6) . ?
N2 C16 1.334(5) . ?
N3 C23 1.337(6) . ?
N3 C24 1.344(5) . ?
C1 C2 1.495(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.319(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.468(6) . ?
C4 C5 1.388(7) . ?
C4 C8 1.369(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.395(7) . ?
C6 H6 0.9300 . ?
C6 C7 1.355(8) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.481(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.304(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.475(6) . ?
C12 C13 1.388(6) . ?
C12 C16 1.381(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.398(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.355(8) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 Dy1 2.869(4) 6_565 ?
C17 C18 1.474(6) . ?
C18 H18 0.9300 . ?
C18 C19 1.309(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.462(6) . ?
C20 C21 1.369(7) . ?
C20 C24 1.390(7) . ?
C21 H21 0.9300 . ?
C21 C22 1.398(8) . ?
C22 H22 0.9300 . ?
C22 C23 1.355(8) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
O3W H3WA 0.820(10) . ?
O3W H3WB 0.820(11) . ?
O3B H3BA 0.820(10) . ?
O3B H3BB 0.820(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1W Dy1 O3 112.54(9) . . ?
O1W Dy1 C9 89.53(11) . . ?
O1W Dy1 C17 141.11(11) . 6_566 ?
O1 Dy1 O1W 74.24(11) . . ?
O1 Dy1 O2 100.84(11) . 7_546 ?
O1 Dy1 O2W 80.90(11) . . ?
O1 Dy1 O3 143.19(10) . . ?
O1 Dy1 O3 88.33(11) . 7_556 ?
O1 Dy1 O4 144.43(11) . . ?
O1 Dy1 O5 126.24(11) . 6_566 ?
O1 Dy1 O6 74.49(11) . 6_566 ?
O1 Dy1 C9 147.95(11) . . ?
O1 Dy1 C17 100.42(13) . 6_566 ?
O2 Dy1 O1W 70.86(10) 7_546 . ?
O2 Dy1 O2W 138.66(11) 7_546 . ?
O2 Dy1 O3 115.70(9) 7_546 . ?
O2 Dy1 O3 147.26(10) 7_546 7_556 ?
O2 Dy1 O4 78.08(10) 7_546 . ?
O2 Dy1 O5 73.68(10) 7_546 6_566 ?
O2 Dy1 O6 73.82(10) 7_546 6_566 ?
O2 Dy1 C9 99.51(11) 7_546 . ?
O2 Dy1 C17 72.55(11) 7_546 6_566 ?
O2W Dy1 O1W 70.01(10) . . ?
O2W Dy1 O3 69.03(10) . . ?
O2W Dy1 O5 137.79(10) . 6_566 ?
O2W Dy1 O6 143.15(11) . 6_566 ?
O2W Dy1 C9 67.50(11) . . ?
O2W Dy1 C17 148.39(11) . 6_566 ?
O3 Dy1 O1W 141.53(10) 7_556 . ?
O3 Dy1 O2W 73.57(10) 7_556 . ?
O3 Dy1 O3 63.59(10) 7_556 . ?
O3 Dy1 O5 75.58(10) 7_556 6_566 ?
O3 Dy1 O6 78.64(9) 7_556 6_566 ?
O3 Dy1 C9 87.79(11) 7_556 . ?
O3 Dy1 C9 25.15(9) . . ?
O3 Dy1 C17 94.85(11) . 6_566 ?
O3 Dy1 C17 74.90(11) 7_556 6_566 ?
O4 Dy1 O1W 71.90(10) . . ?
O4 Dy1 O2W 77.66(11) . . ?
O4 Dy1 O3 111.96(10) . 7_556 ?
O4 Dy1 O3 48.65(9) . . ?
O4 Dy1 O5 88.05(11) . 6_566 ?
O4 Dy1 O6 136.26(11) . 6_566 ?
O4 Dy1 C9 24.24(10) . . ?
O4 Dy1 C17 112.69(13) . 6_566 ?
O5 Dy1 O1W 142.04(10) 6_566 . ?
O5 Dy1 O3 71.73(9) 6_566 . ?
O5 Dy1 O6 52.29(10) 6_566 6_566 ?
O5 Dy1 C9 83.29(10) 6_566 . ?
O5 Dy1 C17 26.03(12) 6_566 6_566 ?
O6 Dy1 O1W 126.49(9) 6_566 . ?
O6 Dy1 O3 118.59(9) 6_566 . ?
O6 Dy1 C9 135.43(11) 6_566 . ?
O6 Dy1 C17 26.28(11) 6_566 6_566 ?
C17 Dy1 C9 109.20(12) 6_566 . ?
I1 Cu1 Cu1 60.04(2) 2 2 ?
I1 Cu1 Cu1 59.60(2) . 2 ?
I1 Cu1 I1 113.30(3) 2 . ?
N2 Cu1 Cu1 99.65(11) . 2 ?
N2 Cu1 I1 105.01(11) . . ?
N2 Cu1 I1 110.36(10) . 2 ?
N3 Cu1 Cu1 150.98(12) . 2 ?
N3 Cu1 I1 109.91(11) . 2 ?
N3 Cu1 I1 108.84(10) . . ?
N3 Cu1 N2 109.27(16) . . ?
Cu1 I1 Cu1 60.36(3) 2 . ?
Dy1 O1W H1WA 109(3) . . ?
Dy1 O1W H1WB 114(3) . . ?
H1WA O1W H1WB 114.2(19) . . ?
C1 O1 Dy1 176.9(3) . . ?
C1 O2 Dy1 130.9(3) . 7_546 ?
Dy1 O2W H2WA 119(3) . . ?
Dy1 O2W H2WB 124(3) . . ?
H2WA O2W H2WB 114.6(19) . . ?
Dy1 O3 Dy1 116.41(10) 7_556 . ?
C9 O3 Dy1 83.0(2) . . ?
C9 O3 Dy1 154.7(3) . 7_556 ?
C9 O4 Dy1 103.7(2) . . ?
C17 O5 Dy1 95.3(3) . 6_565 ?
C17 O6 Dy1 91.5(3) . 6_565 ?
C7 N1 C8 116.7(5) . . ?
C15 N2 Cu1 123.2(3) . . ?
C16 N2 Cu1 119.7(3) . . ?
C16 N2 C15 116.6(4) . . ?
C23 N3 Cu1 124.0(3) . . ?
C23 N3 C24 116.7(4) . . ?
C24 N3 Cu1 119.2(3) . . ?
O1 C1 O2 124.9(4) . . ?
O1 C1 C2 118.6(4) . . ?
O2 C1 C2 116.5(4) . . ?
C1 C2 H2 118.3 . . ?
C3 C2 C1 123.4(4) . . ?
C3 C2 H2 118.3 . . ?
C2 C3 H3 116.8 . . ?
C2 C3 C4 126.3(5) . . ?
C4 C3 H3 116.8 . . ?
C5 C4 C3 119.8(5) . . ?
C8 C4 C3 123.5(4) . . ?
C8 C4 C5 116.8(4) . . ?
C4 C5 H5 120.6 . . ?
C4 C5 C6 118.7(5) . . ?
C6 C5 H5 120.6 . . ?
C5 C6 H6 120.3 . . ?
C7 C6 C5 119.4(5) . . ?
C7 C6 H6 120.3 . . ?
N1 C7 C6 123.1(5) . . ?
N1 C7 H7 118.5 . . ?
C6 C7 H7 118.5 . . ?
N1 C8 C4 125.2(5) . . ?
N1 C8 H8 117.4 . . ?
C4 C8 H8 117.4 . . ?
O3 C9 Dy1 71.9(2) . . ?
O3 C9 C10 118.6(4) . . ?
O4 C9 Dy1 52.1(2) . . ?
O4 C9 O3 121.1(4) . . ?
O4 C9 C10 120.2(4) . . ?
C10 C9 Dy1 157.7(3) . . ?
C9 C10 H10 118.9 . . ?
C11 C10 C9 122.2(4) . . ?
C11 C10 H10 118.9 . . ?
C10 C11 H11 116.9 . . ?
C10 C11 C12 126.2(4) . . ?
C12 C11 H11 116.9 . . ?
C13 C12 C11 120.6(4) . . ?
C16 C12 C11 122.0(4) . . ?
C16 C12 C13 117.4(4) . . ?
C12 C13 H13 120.9 . . ?
C12 C13 C14 118.2(5) . . ?
C14 C13 H13 120.9 . . ?
C13 C14 H14 120.1 . . ?
C15 C14 C13 119.7(5) . . ?
C15 C14 H14 120.1 . . ?
N2 C15 C14 123.1(4) . . ?
N2 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
N2 C16 C12 124.8(4) . . ?
N2 C16 H16 117.6 . . ?
C12 C16 H16 117.6 . . ?
O5 C17 Dy1 58.6(2) . 6_565 ?
O5 C17 O6 120.8(4) . . ?
O5 C17 C18 118.2(4) . . ?
O6 C17 Dy1 62.2(2) . 6_565 ?
O6 C17 C18 121.0(4) . . ?
C18 C17 Dy1 174.7(3) . 6_565 ?
C17 C18 H18 117.9 . . ?
C19 C18 C17 124.1(5) . . ?
C19 C18 H18 117.9 . . ?
C18 C19 H19 116.5 . . ?
C18 C19 C20 126.9(5) . . ?
C20 C19 H19 116.5 . . ?
C21 C20 C19 121.5(5) . . ?
C21 C20 C24 117.2(4) . . ?
C24 C20 C19 121.4(4) . . ?
C20 C21 H21 120.2 . . ?
C20 C21 C22 119.5(5) . . ?
C22 C21 H21 120.2 . . ?
C21 C22 H22 120.6 . . ?
C23 C22 C21 118.9(5) . . ?
C23 C22 H22 120.6 . . ?
N3 C23 C22 123.6(5) . . ?
N3 C23 H23 118.2 . . ?
C22 C23 H23 118.2 . . ?
N3 C24 C20 124.1(4) . . ?
N3 C24 H24 117.9 . . ?
C20 C24 H24 117.9 . . ?
H3WA O3W H3WB 116(2) . . ?
H3BA O3B H3BB 116(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA I1 0.818(10) 2.997(11) 3.815(3) 179(5) 2_545
O1W H1WB O6 0.829(10) 2.030(13) 2.855(4) 173(5) 4_535
O2W H2WA O5 0.820(10) 1.927(18) 2.727(4) 165(5) 4_545
O2W H2WB N1 0.825(10) 1.963(14) 2.782(5) 171(5) 5_656
C6 H6 O3W 0.93 2.61 3.40(5) 142.3 8_566

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
Dy1 O2 C1 O1 -13.9(6) 7_546 . . . ?
Dy1 O2 C1 C2 165.1(3) 7_546 . . . ?
Dy1 O3 C9 Dy1 142.1(6) 7_556 . . . ?
Dy1 O3 C9 O4 159.8(4) 7_556 . . . ?
Dy1 O3 C9 O4 17.7(4) . . . . ?
Dy1 O3 C9 C10 -158.4(4) . . . . ?
Dy1 O3 C9 C10 -16.3(9) 7_556 . . . ?
Dy1 O4 C9 O3 -21.5(5) . . . . ?
Dy1 O4 C9 C10 154.6(3) . . . . ?
Dy1 O5 C17 O6 3.0(4) 6_565 . . . ?
Dy1 O5 C17 C18 -175.2(3) 6_565 . . . ?
Dy1 O6 C17 O5 -2.9(4) 6_565 . . . ?
Dy1 O6 C17 C18 175.2(4) 6_565 . . . ?
Dy1 C9 C10 C11 51.3(10) . . . . ?
Cu1 N2 C15 C14 -171.6(5) . . . . ?
Cu1 N2 C16 C12 172.7(4) . . . . ?
Cu1 N3 C23 C22 178.3(5) . . . . ?
Cu1 N3 C24 C20 -177.0(4) . . . . ?
O1 C1 C2 C3 -1.4(7) . . . . ?
O2 C1 C2 C3 179.5(4) . . . . ?
O3 C9 C10 C11 164.4(4) . . . . ?
O4 C9 C10 C11 -11.7(7) . . . . ?
O5 C17 C18 C19 173.4(5) . . . . ?
O6 C17 C18 C19 -4.7(7) . . . . ?
C1 C2 C3 C4 -179.1(4) . . . . ?
C2 C3 C4 C5 -175.3(5) . . . . ?
C2 C3 C4 C8 4.9(8) . . . . ?
C3 C4 C5 C6 -179.3(5) . . . . ?
C3 C4 C8 N1 178.3(5) . . . . ?
C4 C5 C6 C7 0.6(8) . . . . ?
C5 C4 C8 N1 -1.5(8) . . . . ?
C5 C6 C7 N1 -0.9(9) . . . . ?
C7 N1 C8 C4 1.2(8) . . . . ?
C8 N1 C7 C6 0.1(8) . . . . ?
C8 C4 C5 C6 0.6(7) . . . . ?
C9 C10 C11 C12 -173.9(4) . . . . ?
C10 C11 C12 C13 167.2(5) . . . . ?
C10 C11 C12 C16 -14.0(8) . . . . ?
C11 C12 C13 C14 -179.4(5) . . . . ?
C11 C12 C16 N2 179.9(4) . . . . ?
C12 C13 C14 C15 -1.0(9) . . . . ?
C13 C12 C16 N2 -1.2(8) . . . . ?
C13 C14 C15 N2 -0.3(9) . . . . ?
C15 N2 C16 C12 0.0(7) . . . . ?
C16 N2 C15 C14 0.9(8) . . . . ?
C16 C12 C13 C14 1.7(8) . . . . ?
C17 C18 C19 C20 179.5(4) . . . . ?
C18 C19 C20 C21 164.3(6) . . . . ?
C18 C19 C20 C24 -15.9(8) . . . . ?
C19 C20 C21 C22 -177.6(6) . . . . ?
C19 C20 C24 N3 177.8(5) . . . . ?
C20 C21 C22 C23 -1.4(11) . . . . ?
C21 C20 C24 N3 -2.4(8) . . . . ?
C21 C22 C23 N3 -0.4(11) . . . . ?
C23 N3 C24 C20 0.6(8) . . . . ?
C24 N3 C23 C22 0.8(9) . . . . ?
C24 C20 C21 C22 2.7(10) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 973524'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '2(C24 H23 Cu Gd I N3 O8), O'
_chemical_formula_sum            'C48 H46 Cu2 Gd2 I2 N6 O17'
_chemical_formula_weight         1674.29
_chemical_melting_point          ?
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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.998(2)
_cell_length_b                   9.2967(9)
_cell_length_c                   29.381(4)
_cell_angle_alpha                90
_cell_angle_beta                 110.4250(10)
_cell_angle_gamma                90
_cell_volume                     5631.1(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5202
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.40
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.239
_exptl_absorpt_correction_T_max  0.428
_exptl_absorpt_correction_T_min  0.376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_special_details           
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1357 before and 0.0406 after correction.
The Ratio of minimum to maximum transmission is 0.5385.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            14263
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.399
_diffrn_reflns_theta_min         1.479
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4584
_reflns_number_total             5202
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.791
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5192
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0273
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0328P)²+9.4077P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0669
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid bond restraints
 Gd1, O6
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
3. Others
 Fixed Sof: O3W(0.5)
4.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C24(H24), C16(H16), C11(H11), C15(H15), C13(H13), C23(H23),
 C21(H21), C3(H3), C2(H2), C19(H19), C22(H22), C18(H18), C8(H8), C5(H5),
 C14(H14), C7(H7), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Gd1 Gd 0.27042(2) 0.51614(2) 0.01234(2) 0.02642(7) Uani 1 1 d . U . . .
I1 I 0.46608(2) 1.38266(4) 0.16944(2) 0.04774(10) Uani 1 1 d . . . . .
Cu1 Cu 0.43868(3) 1.31931(6) 0.24808(2) 0.04597(15) Uani 1 1 d . . . . .
O2W O 0.20965(15) 0.6099(3) 0.06059(11) 0.0417(7) Uani 1 1 d . . . . .
H2WA H 0.1954 0.6945 0.0506 0.063 Uiso 1 1 d GR . . . .
H2WB H 0.2343 0.6152 0.0906 0.063 Uiso 1 1 d GR . . . .
O1W O 0.28844(14) 0.3580(3) 0.08672(10) 0.0384(7) Uani 1 1 d . . . . .
H1WA H 0.3296 0.3541 0.1044 0.058 Uiso 1 1 d GR . . . .
H1WB H 0.2749 0.2705 0.0778 0.058 Uiso 1 1 d GR . . . .
C9 C 0.33936(17) 0.7517(4) 0.07683(14) 0.0293(8) Uani 1 1 d . . . . .
O1 O 0.18635(13) 0.3570(3) -0.00873(11) 0.0410(7) Uani 1 1 d . . . . .
C1 C 0.13781(18) 0.2764(4) -0.02220(13) 0.0295(8) Uani 1 1 d . . . . .
C10 C 0.3618(2) 0.8442(4) 0.12030(15) 0.0357(9) Uani 1 1 d . . . . .
H10 H 0.3579 0.9434 0.1165 0.043 Uiso 1 1 calc R . . . .
N3 N 0.35597(18) 1.4268(4) 0.24644(13) 0.0439(9) Uani 1 1 d . . . . .
C24 C 0.3450(2) 1.4452(5) 0.28763(16) 0.0419(10) Uani 1 1 d . . . . .
H24 H 0.3763 1.4124 0.3161 0.050 Uiso 1 1 calc R . . . .
C16 C 0.4090(2) 1.0199(4) 0.21113(15) 0.0387(10) Uani 1 1 d . . . . .
H16 H 0.4002 1.0683 0.1818 0.046 Uiso 1 1 calc R . . . .
N2 N 0.42462(17) 1.0984(4) 0.25168(12) 0.0396(8) Uani 1 1 d . . . . .
C11 C 0.3871(2) 0.7906(5) 0.16392(15) 0.0411(10) Uani 1 1 d . . . . .
H11 H 0.3945 0.6919 0.1663 0.049 Uiso 1 1 calc R . . . .
C12 C 0.4049(2) 0.8715(5) 0.20982(15) 0.0407(10) Uani 1 1 d . . . . .
C15 C 0.4367(3) 1.0281(6) 0.29368(16) 0.0528(13) Uani 1 1 d . . . . .
H15 H 0.4470 1.0812 0.3222 0.063 Uiso 1 1 calc R . . . .
C13 C 0.4193(3) 0.8009(6) 0.25404(17) 0.0593(14) Uani 1 1 d . . . . .
H13 H 0.4186 0.7009 0.2552 0.071 Uiso 1 1 calc R . . . .
C20 C 0.2895(2) 1.5108(5) 0.29109(16) 0.0428(11) Uani 1 1 d . . . . .
C23 C 0.3108(2) 1.4747(6) 0.20598(17) 0.0576(14) Uani 1 1 d . . . . .
H23 H 0.3173 1.4609 0.1767 0.069 Uiso 1 1 calc R . . . .
C21 C 0.2447(3) 1.5613(8) 0.24866(19) 0.0688(17) Uani 1 1 d . . . . .
H21 H 0.2074 1.6074 0.2491 0.083 Uiso 1 1 calc R . . . .
O3 O 0.30250(13) 0.8064(3) 0.03700(9) 0.0373(7) Uani 1 1 d . . . . .
O4 O 0.35446(14) 0.6212(3) 0.07971(10) 0.0419(7) Uani 1 1 d . . . . .
C3 C 0.0609(2) 0.4790(5) -0.04318(15) 0.0377(10) Uani 1 1 d . . . . .
H3 H 0.0974 0.5377 -0.0328 0.045 Uiso 1 1 calc R . . . .
C2 C 0.07142(19) 0.3399(4) -0.04080(16) 0.0375(10) Uani 1 1 d . . . . .
H2 H 0.0359 0.2782 -0.0511 0.045 Uiso 1 1 calc R . . . .
C19 C 0.2791(2) 1.5242(5) 0.33765(16) 0.0426(11) Uani 1 1 d . . . . .
H19 H 0.2475 1.5891 0.3389 0.051 Uiso 1 1 calc R . . . .
C22 C 0.2554(3) 1.5431(8) 0.20518(19) 0.080(2) Uani 1 1 d . . . . .
H22 H 0.2256 1.5767 0.1762 0.096 Uiso 1 1 calc R . . . .
C17 C 0.2976(2) 1.4736(4) 0.42393(15) 0.0341(9) Uani 1 1 d . . . . .
C18 C 0.3100(2) 1.4534(5) 0.37765(16) 0.0421(10) Uani 1 1 d . . . . .
H18 H 0.3414 1.3871 0.3771 0.051 Uiso 1 1 calc R . . . .
C8 C -0.0605(2) 0.4776(5) -0.07310(17) 0.0446(11) Uani 1 1 d . . . . .
H8 H -0.0587 0.3778 -0.0710 0.053 Uiso 1 1 calc R . . . .
C4 C -0.0021(2) 0.5519(5) -0.06046(15) 0.0389(10) Uani 1 1 d . . . . .
C5 C -0.0059(2) 0.7005(5) -0.06349(19) 0.0541(13) Uani 1 1 d . . . . .
H5 H 0.0316 0.7558 -0.0551 0.065 Uiso 1 1 calc R . . . .
C14 C 0.4347(3) 0.8805(6) 0.29636(18) 0.0648(16) Uani 1 1 d . . . . .
H14 H 0.4435 0.8350 0.3262 0.078 Uiso 1 1 calc R . . . .
C7 C -0.1203(2) 0.6827(6) -0.0905(2) 0.0597(15) Uani 1 1 d . . . . .
H7 H -0.1605 0.7279 -0.1006 0.072 Uiso 1 1 calc R . . . .
C6 C -0.0667(3) 0.7660(6) -0.0793(2) 0.0638(15) Uani 1 1 d . . . . .
H6 H -0.0703 0.8655 -0.0821 0.077 Uiso 1 1 calc R . . . .
N1 N -0.11875(18) 0.5390(5) -0.08801(15) 0.0511(10) Uani 1 1 d . . . . .
O5 O 0.25818(14) 1.5681(3) 0.42749(10) 0.0378(7) Uani 1 1 d . . . . .
O6 O 0.32606(14) 1.3900(3) 0.45893(10) 0.0384(7) Uani 1 1 d . U . . .
O2 O 0.14135(13) 0.1409(3) -0.02111(11) 0.0379(7) Uani 1 1 d . . . . .
O3W O 1.0060(16) 0.037(3) 0.9557(10) 0.41(2) Uani 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
Gd1 O2W 2.425(3) . ?
Gd1 O1W 2.547(3) . ?
Gd1 O1 2.279(3) . ?
Gd1 O3 2.403(3) 7_565 ?
Gd1 O3 2.819(3) . ?
Gd1 O4 2.395(3) . ?
Gd1 C17 2.863(4) 6_575 ?
Gd1 O5 2.536(3) 6_575 ?
Gd1 O6 2.462(3) 6_575 ?
Gd1 O2 2.370(3) 7 ?
I1 Cu1 2.6581(7) 2_655 ?
I1 Cu1 2.6498(7) . ?
Cu1 I1 2.6581(6) 2_655 ?
Cu1 Cu1 2.6605(12) 2_655 ?
Cu1 N3 2.061(4) . ?
Cu1 N2 2.085(4) . ?
C9 C10 1.474(5) . ?
C9 O3 1.274(4) . ?
C9 O4 1.253(5) . ?
O1 C1 1.250(5) . ?
C1 C2 1.491(5) . ?
C1 O2 1.262(5) . ?
C10 C11 1.305(6) . ?
N3 C24 1.325(5) . ?
N3 C23 1.332(6) . ?
C24 C20 1.401(6) . ?
C16 N2 1.336(5) . ?
C16 C12 1.382(6) . ?
N2 C15 1.338(6) . ?
C11 C12 1.473(6) . ?
C12 C13 1.390(6) . ?
C15 C14 1.376(7) . ?
C13 C14 1.384(7) . ?
C20 C21 1.374(7) . ?
C20 C19 1.469(6) . ?
C23 C22 1.368(7) . ?
C21 C22 1.388(7) . ?
O3 Gd1 2.403(3) 7_565 ?
C3 C2 1.311(6) . ?
C3 C4 1.466(6) . ?
C19 C18 1.311(6) . ?
C17 Gd1 2.863(4) 6_576 ?
C17 C18 1.490(6) . ?
C17 O5 1.263(5) . ?
C17 O6 1.267(5) . ?
C8 C4 1.391(6) . ?
C8 N1 1.329(5) . ?
C4 C5 1.385(6) . ?
C5 C6 1.393(6) . ?
C7 C6 1.351(7) . ?
C7 N1 1.338(7) . ?
O5 Gd1 2.536(3) 6_576 ?
O6 Gd1 2.462(3) 6_576 ?
O2 Gd1 2.370(3) 7 ?

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
O2W Gd1 O1W 70.02(9) . . ?
O2W Gd1 O3 69.23(9) . . ?
O2W Gd1 C17 148.27(10) . 6_575 ?
O2W Gd1 O5 142.62(10) . 6_575 ?
O2W Gd1 O6 138.01(9) . 6_575 ?
O1W Gd1 O3 112.45(8) . . ?
O1W Gd1 C17 141.12(10) . 6_575 ?
O1 Gd1 O2W 80.30(10) . . ?
O1 Gd1 O1W 74.15(10) . . ?
O1 Gd1 O3 88.53(10) . 7_565 ?
O1 Gd1 O3 142.93(9) . . ?
O1 Gd1 O4 143.94(11) . . ?
O1 Gd1 C17 100.47(12) . 6_575 ?
O1 Gd1 O5 74.63(10) . 6_575 ?
O1 Gd1 O6 126.43(10) . 6_575 ?
O1 Gd1 O2 100.71(10) . 7 ?
O3 Gd1 O2W 73.60(10) 7_565 . ?
O3 Gd1 O1W 141.73(9) 7_565 . ?
O3 Gd1 O3 63.40(10) 7_565 . ?
O3 Gd1 C17 95.07(10) . 6_575 ?
O3 Gd1 C17 74.71(10) 7_565 6_575 ?
O3 Gd1 O5 78.43(9) 7_565 6_575 ?
O3 Gd1 O6 75.39(10) 7_565 6_575 ?
O4 Gd1 O2W 78.13(10) . . ?
O4 Gd1 O1W 71.46(10) . . ?
O4 Gd1 O3 112.27(9) . 7_565 ?
O4 Gd1 O3 49.12(8) . . ?
O4 Gd1 C17 113.02(12) . 6_575 ?
O4 Gd1 O5 136.46(10) . 6_575 ?
O4 Gd1 O6 88.29(10) . 6_575 ?
O5 Gd1 O1W 126.62(9) 6_575 . ?
O5 Gd1 O3 118.63(9) 6_575 . ?
O5 Gd1 C17 26.18(10) 6_575 6_575 ?
O6 Gd1 O1W 142.01(9) 6_575 . ?
O6 Gd1 O3 71.87(8) 6_575 . ?
O6 Gd1 C17 26.16(11) 6_575 6_575 ?
O6 Gd1 O5 52.33(9) 6_575 6_575 ?
O2 Gd1 O2W 139.08(10) 7 . ?
O2 Gd1 O1W 71.03(9) 7 . ?
O2 Gd1 O3 116.08(9) 7 . ?
O2 Gd1 O3 146.88(10) 7 7_565 ?
O2 Gd1 O4 78.14(10) 7 . ?
O2 Gd1 C17 72.36(10) 7 6_575 ?
O2 Gd1 O5 73.66(9) 7 6_575 ?
O2 Gd1 O6 73.57(10) 7 6_575 ?
Cu1 I1 Cu1 60.16(2) . 2_655 ?
I1 Cu1 I1 113.51(2) . 2_655 ?
I1 Cu1 Cu1 59.76(2) 2_655 2_655 ?
I1 Cu1 Cu1 60.07(2) . 2_655 ?
N3 Cu1 I1 108.81(10) . 2_655 ?
N3 Cu1 I1 109.84(11) . . ?
N3 Cu1 Cu1 151.00(11) . 2_655 ?
N3 Cu1 N2 109.46(15) . . ?
N2 Cu1 I1 110.25(10) . . ?
N2 Cu1 I1 104.81(10) . 2_655 ?
N2 Cu1 Cu1 99.45(10) . 2_655 ?
O3 C9 C10 118.5(3) . . ?
O4 C9 C10 120.3(3) . . ?
O4 C9 O3 121.1(3) . . ?
C1 O1 Gd1 175.9(3) . . ?
O1 C1 C2 119.9(4) . . ?
O1 C1 O2 123.5(3) . . ?
O2 C1 C2 116.6(3) . . ?
C11 C10 C9 121.8(4) . . ?
C24 N3 Cu1 118.8(3) . . ?
C24 N3 C23 117.1(4) . . ?
C23 N3 Cu1 124.1(3) . . ?
N3 C24 C20 124.3(4) . . ?
N2 C16 C12 124.4(4) . . ?
C16 N2 Cu1 119.3(3) . . ?
C16 N2 C15 117.5(4) . . ?
C15 N2 Cu1 122.9(3) . . ?
C10 C11 C12 126.2(4) . . ?
C16 C12 C11 122.0(4) . . ?
C16 C12 C13 117.0(4) . . ?
C13 C12 C11 121.0(4) . . ?
N2 C15 C14 122.7(4) . . ?
C14 C13 C12 119.4(5) . . ?
C24 C20 C19 121.9(4) . . ?
C21 C20 C24 116.7(4) . . ?
C21 C20 C19 121.4(4) . . ?
N3 C23 C22 123.6(5) . . ?
C20 C21 C22 119.7(5) . . ?
Gd1 O3 Gd1 116.60(10) 7_565 . ?
C9 O3 Gd1 82.9(2) . . ?
C9 O3 Gd1 154.8(3) . 7_565 ?
C9 O4 Gd1 103.2(2) . . ?
C2 C3 C4 127.0(4) . . ?
C3 C2 C1 122.8(4) . . ?
C18 C19 C20 126.3(4) . . ?
C23 C22 C21 118.5(5) . . ?
C18 C17 Gd1 174.5(3) . 6_576 ?
O5 C17 Gd1 62.3(2) . 6_576 ?
O5 C17 C18 120.9(4) . . ?
O5 C17 O6 121.3(4) . . ?
O6 C17 Gd1 59.0(2) . 6_576 ?
O6 C17 C18 117.8(4) . . ?
C19 C18 C17 123.5(4) . . ?
N1 C8 C4 124.7(4) . . ?
C8 C4 C3 122.5(4) . . ?
C5 C4 C3 120.8(4) . . ?
C5 C4 C8 116.7(4) . . ?
C4 C5 C6 119.1(5) . . ?
C15 C14 C13 119.0(5) . . ?
N1 C7 C6 123.7(4) . . ?
C7 C6 C5 119.0(5) . . ?
C8 N1 C7 116.8(4) . . ?
C17 O5 Gd1 91.5(2) . 6_576 ?
C17 O6 Gd1 94.8(2) . 6_576 ?
C1 O2 Gd1 131.2(3) . 7 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 973525'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(C24 H22 Cu I N3 O8 Sm), H2 O'
_chemical_formula_sum            'C48 H46 Cu2 I2 N6 O17 Sm2'
_chemical_formula_weight         1660.53
_chemical_melting_point          ?
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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.069(4)
_cell_length_b                   9.2855(15)
_cell_length_c                   29.444(5)
_cell_angle_alpha                90
_cell_angle_beta                 110.419(2)
_cell_angle_gamma                90
_cell_volume                     5654.6(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6892
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.083
_cell_measurement_theta_min      1.969
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.952
_exptl_absorpt_correction_T_max  0.454
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.950
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            16700
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.083
_diffrn_reflns_theta_min         1.969
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5146
_reflns_number_total             6892
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Apex2 (Bruker, 2005)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'Apex2 (Bruker, 2005)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker, 2000-2003)'
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6538
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0229P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0639
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O3W-H3WA = O3W-H3WB = O3B-H3BA = O3B-H3BB = O1W-H1WA = O1W-H1WB = O2W-H2WA =
 O2W-H2WB
 0.82 with sigma of 0.01
 H3WA-H3WB = H3BA-H3BB = H1WA-H1WB = H2WA-H2WB
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O3W \\sim O3B: within 3.8A with sigma of 0.02 and sigma for terminal atoms of
0.04
4. Others
 Sof(O3B)=Sof(H3BA)=Sof(H3BB)=0.5*(1-FVAR(2))
 Sof(O3W)=Sof(H3WA)=Sof(H3WB)=0.5*FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
  C24(H24)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Sm1 Sm 0.22933(2) 0.01664(2) 0.48763(2) 0.02762(6) Uani 1 1 d . . . . .
Cu1 Cu 0.06147(3) 0.82038(6) 0.25221(2) 0.04769(14) Uani 1 1 d . . . . .
I1 I -0.03338(2) 0.88320(3) 0.16966(2) 0.04929(9) Uani 1 1 d . . . . .
O1W O 0.21072(14) -0.1438(3) 0.41273(10) 0.0406(7) Uani 1 1 d D . . . .
H1WA H 0.1716(6) -0.139(4) 0.3974(14) 0.061 Uiso 1 1 d DR . . . .
H1WB H 0.2251(16) -0.2268(19) 0.4172(15) 0.061 Uiso 1 1 d DR . . . .
O1 O 0.31443(13) -0.1432(3) 0.50897(10) 0.0420(7) Uani 1 1 d . . . . .
O2 O 0.35989(13) -0.3582(3) 0.52094(9) 0.0391(6) Uani 1 1 d . . . . .
O2W O 0.28958(15) 0.1111(3) 0.43830(11) 0.0450(7) Uani 1 1 d D . . . .
H2WA H 0.3016(19) 0.1950(17) 0.4441(15) 0.067 Uiso 1 1 d DR . . . .
H2WB H 0.3113(18) 0.063(3) 0.4263(16) 0.067 Uiso 1 1 d DR . . . .
O3 O 0.19684(13) 0.3029(3) 0.46257(8) 0.0360(6) Uani 1 1 d . . . . .
O4 O 0.14399(14) 0.1208(3) 0.41940(9) 0.0426(7) Uani 1 1 d . . . A 1
O5 O 0.17406(14) 0.8898(3) 0.04237(9) 0.0406(7) Uani 1 1 d . . . B 1
O6 O 0.24204(13) 1.0682(3) 0.07330(9) 0.0387(6) Uani 1 1 d . . . B 1
N1 N 0.61867(18) 0.0390(4) 0.58768(13) 0.0522(10) Uani 1 1 d . . . C 1
N2 N 0.07576(17) 0.6003(3) 0.24852(11) 0.0419(8) Uani 1 1 d . . . A 1
N3 N 0.14386(18) 0.9274(4) 0.25403(12) 0.0450(9) Uani 1 1 d . . . B 1
C1 C 0.36280(18) -0.2236(4) 0.52190(12) 0.0299(8) Uani 1 1 d . . . C 1
C2 C 0.4286(2) -0.1587(4) 0.54051(14) 0.0396(9) Uani 1 1 d . . . C 1
H2 H 0.4640 -0.2204 0.5509 0.047 Uiso 1 1 calc R . . C 1
C3 C 0.4396(2) -0.0199(4) 0.54313(14) 0.0390(9) Uani 1 1 d . . . C 1
H3 H 0.4034 0.0394 0.5327 0.047 Uiso 1 1 calc R . . C 1
C4 C 0.5023(2) 0.0526(4) 0.56064(14) 0.0394(10) Uani 1 1 d . . . C 1
C5 C 0.5064(2) 0.2018(5) 0.56382(17) 0.0565(12) Uani 1 1 d . . . C 1
H5 H 0.4692 0.2578 0.5554 0.068 Uiso 1 1 calc R . . C 1
C6 C 0.5667(3) 0.2652(5) 0.57961(19) 0.0662(14) Uani 1 1 d . . . C 1
H6 H 0.5704 0.3648 0.5828 0.079 Uiso 1 1 calc R . . C 1
C7 C 0.6203(2) 0.1832(5) 0.59050(17) 0.0612(14) Uani 1 1 d . . . C 1
H7 H 0.6603 0.2288 0.6005 0.073 Uiso 1 1 calc R . . C 1
C8 C 0.5604(2) -0.0219(5) 0.57303(15) 0.0466(11) Uani 1 1 d . . . C 1
H8 H 0.5584 -0.1219 0.5709 0.056 Uiso 1 1 calc R . . C 1
C9 C 0.15990(18) 0.2507(4) 0.42255(13) 0.0326(8) Uani 1 1 d . . . A 1
C10 C 0.1380(2) 0.3448(4) 0.37923(13) 0.0375(9) Uani 1 1 d . . . A 1
H10 H 0.1426 0.4441 0.3832 0.045 Uiso 1 1 calc R . . A 1
C11 C 0.1125(2) 0.2920(4) 0.33568(13) 0.0414(10) Uani 1 1 d . . . A 1
H11 H 0.1048 0.1934 0.3333 0.050 Uiso 1 1 calc R . . A 1
C12 C 0.0946(2) 0.3726(4) 0.29002(14) 0.0412(10) Uani 1 1 d . . . A 1
C13 C 0.0803(3) 0.3034(5) 0.24574(15) 0.0611(14) Uani 1 1 d . . . A 1
H13 H 0.0809 0.2033 0.2444 0.073 Uiso 1 1 calc R . . A 1
C14 C 0.0653(3) 0.3829(5) 0.20375(16) 0.0677(16) Uani 1 1 d . . . A 1
H14 H 0.0566 0.3376 0.1740 0.081 Uiso 1 1 calc R . . A 1
C15 C 0.0635(2) 0.5293(5) 0.20667(15) 0.0543(12) Uani 1 1 d . . . A 1
H15 H 0.0532 0.5824 0.1782 0.065 Uiso 1 1 calc R . . A 1
C16 C 0.0912(2) 0.5212(4) 0.28894(13) 0.0390(9) Uani 1 1 d . . . A 1
H16 H 0.1002 0.5694 0.3182 0.047 Uiso 1 1 calc R . . A 1
C17 C 0.2029(2) 0.9736(4) 0.07697(14) 0.0365(9) Uani 1 1 d . . . B 1
C18 C 0.1903(2) 0.9536(4) 0.12303(14) 0.0441(10) Uani 1 1 d . . . B 1
H18 H 0.1587 0.8879 0.1234 0.053 Uiso 1 1 calc R . . B 1
C19 C 0.2214(2) 1.0238(4) 0.16317(14) 0.0427(10) Uani 1 1 d . . . B 1
H19 H 0.2534 1.0877 0.1622 0.051 Uiso 1 1 calc R . . B 1
C20 C 0.2105(2) 1.0110(4) 0.20967(14) 0.0420(10) Uani 1 1 d . . . B 1
C21 C 0.2551(3) 1.0634(7) 0.25176(16) 0.0715(16) Uani 1 1 d . . . B 1
H21 H 0.2920 1.1109 0.2512 0.086 Uiso 1 1 calc R . . B 1
C22 C 0.2445(3) 1.0444(7) 0.29527(17) 0.0835(19) Uani 1 1 d . . . B 1
H22 H 0.2745 1.0772 0.3243 0.100 Uiso 1 1 calc R . . B 1
C23 C 0.1890(2) 0.9767(5) 0.29459(15) 0.0587(13) Uani 1 1 d . . . B 1
H23 H 0.1823 0.9642 0.3238 0.070 Uiso 1 1 calc R . . B 1
C24 C 0.1555(2) 0.9475(4) 0.21257(14) 0.0425(10) Uani 1 1 d . . . B 1
H24 H 0.1242 0.9165 0.1839 0.051 Uiso 1 1 calc R . . B 1
O3W O 0.052(2) 0.889(4) 0.033(2) 0.219(13) Uani 0.164(8) 1 d D U P D 1
H3WA H 0.027(12) 0.93(4) 0.044(10) 0.328 Uiso 0.164(8) 1 d DR . P D 1
H3WB H 0.063(14) 0.93(4) 0.014(9) 0.328 Uiso 0.164(8) 1 d DR . P D 1
O3B O -0.0177(11) 0.981(2) 0.0455(9) 0.208(10) Uani 0.336(8) 1 d D U P D 2
H3BA H -0.049(9) 0.99(4) 0.021(6) 0.312 Uiso 0.336(8) 1 d DR . P D 2
H3BB H 0.012(9) 0.93(3) 0.043(12) 0.312 Uiso 0.336(8) 1 d DR . P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O1W 2.573(3) . ?
Sm1 O1 2.302(3) . ?
Sm1 O2 2.400(3) 7_546 ?
Sm1 O2W 2.448(3) . ?
Sm1 O3 2.784(2) . ?
Sm1 O3 2.439(2) 7_556 ?
Sm1 O4 2.425(3) . ?
Sm1 O5 2.493(3) 6_566 ?
Sm1 O6 2.563(2) 6_566 ?
Sm1 C9 2.949(4) . ?
Sm1 C17 2.888(4) 6_566 ?
Cu1 Cu1 2.6708(12) 2 ?
Cu1 I1 2.6609(7) . ?
Cu1 I1 2.6482(7) 2 ?
Cu1 N2 2.076(3) . ?
Cu1 N3 2.056(4) . ?
I1 Cu1 2.6481(7) 2 ?
O1W H1WA 0.825(10) . ?
O1W H1WB 0.826(10) . ?
O1 C1 1.248(4) . ?
O2 Sm1 2.400(2) 7_546 ?
O2 C1 1.251(4) . ?
O2W H2WA 0.821(10) . ?
O2W H2WB 0.821(10) . ?
O3 Sm1 2.438(2) 7_556 ?
O3 C9 1.272(4) . ?
O4 C9 1.250(4) . ?
O5 Sm1 2.493(3) 6_565 ?
O5 C17 1.263(5) . ?
O6 Sm1 2.563(2) 6_565 ?
O6 C17 1.262(5) . ?
N1 C7 1.342(6) . ?
N1 C8 1.332(5) . ?
N2 C15 1.339(5) . ?
N2 C16 1.338(4) . ?
N3 C23 1.341(5) . ?
N3 C24 1.345(5) . ?
C1 C2 1.490(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.309(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.461(5) . ?
C4 C5 1.389(6) . ?
C4 C8 1.389(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.379(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.349(7) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.481(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.303(5) . ?
C11 H11 0.9300 . ?
C11 C12 1.467(5) . ?
C12 C13 1.387(5) . ?
C12 C16 1.382(5) . ?
C13 H13 0.9300 . ?
C13 C14 1.378(6) . ?
C14 H14 0.9300 . ?
C14 C15 1.363(6) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 Sm1 2.888(4) 6_565 ?
C17 C18 1.488(5) . ?
C18 H18 0.9300 . ?
C18 C19 1.314(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.476(5) . ?
C20 C21 1.375(6) . ?
C20 C24 1.379(6) . ?
C21 H21 0.9300 . ?
C21 C22 1.392(6) . ?
C22 H22 0.9300 . ?
C22 C23 1.371(7) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
O3W H3WA 0.820(10) . ?
O3W H3WB 0.820(10) . ?
O3B H3BA 0.820(10) . ?
O3B H3BB 0.820(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1W Sm1 O3 112.11(8) . . ?
O1W Sm1 C9 88.77(9) . . ?
O1W Sm1 C17 140.92(9) . 6_566 ?
O1 Sm1 O1W 74.44(9) . . ?
O1 Sm1 O2 101.22(9) . 7_546 ?
O1 Sm1 O2W 80.37(10) . . ?
O1 Sm1 O3 142.92(8) . . ?
O1 Sm1 O3 88.21(9) . 7_556 ?
O1 Sm1 O4 143.82(9) . . ?
O1 Sm1 O5 125.78(9) . 6_566 ?
O1 Sm1 O6 74.61(9) . 6_566 ?
O1 Sm1 C9 147.35(10) . . ?
O1 Sm1 C17 100.15(11) . 6_566 ?
O2 Sm1 O1W 71.03(9) 7_546 . ?
O2 Sm1 O2W 138.83(9) 7_546 . ?
O2 Sm1 O3 115.56(8) 7_546 . ?
O2 Sm1 O3 146.74(8) 7_546 7_556 ?
O2 Sm1 O4 77.64(9) 7_546 . ?
O2 Sm1 O5 73.32(9) 7_546 6_566 ?
O2 Sm1 O6 73.69(9) 7_546 6_566 ?
O2 Sm1 C9 99.34(10) 7_546 . ?
O2 Sm1 C17 72.30(9) 7_546 6_566 ?
O2W Sm1 O1W 69.90(9) . . ?
O2W Sm1 O3 69.14(8) . . ?
O2W Sm1 O5 138.46(8) . 6_566 ?
O2W Sm1 O6 142.97(10) . 6_566 ?
O2W Sm1 C9 67.49(10) . . ?
O2W Sm1 C17 148.57(10) . 6_566 ?
O3 Sm1 O1W 141.89(9) 7_556 . ?
O3 Sm1 O2W 73.94(9) 7_556 . ?
O3 Sm1 O3 63.87(10) 7_556 . ?
O3 Sm1 O5 75.33(9) 7_556 6_566 ?
O3 Sm1 O6 78.38(8) 7_556 6_566 ?
O3 Sm1 C9 88.33(10) 7_556 . ?
O3 Sm1 C9 25.43(8) . . ?
O3 Sm1 C17 95.52(9) . 6_566 ?
O3 Sm1 C17 74.67(9) 7_556 6_566 ?
O4 Sm1 O1W 71.05(9) . . ?
O4 Sm1 O2W 77.95(10) . . ?
O4 Sm1 O3 112.76(8) . 7_556 ?
O4 Sm1 O3 49.14(7) . . ?
O4 Sm1 O5 89.02(9) . 6_566 ?
O4 Sm1 O6 136.45(9) . 6_566 ?
O4 Sm1 C9 24.51(9) . . ?
O4 Sm1 C17 113.39(11) . 6_566 ?
O5 Sm1 O1W 142.02(9) 6_566 . ?
O5 Sm1 O3 72.53(8) 6_566 . ?
O5 Sm1 O6 51.73(8) 6_566 6_566 ?
O5 Sm1 C9 84.42(9) 6_566 . ?
O5 Sm1 C17 25.84(10) 6_566 6_566 ?
O6 Sm1 O1W 126.56(8) 6_566 . ?
O6 Sm1 O3 118.92(8) 6_566 . ?
O6 Sm1 C9 136.03(9) 6_566 . ?
O6 Sm1 C17 25.91(10) 6_566 6_566 ?
C17 Sm1 C9 110.16(11) 6_566 . ?
I1 Cu1 Cu1 60.034(19) 2 2 ?
I1 Cu1 Cu1 59.56(2) . 2 ?
I1 Cu1 I1 113.41(2) 2 . ?
N2 Cu1 Cu1 99.66(10) . 2 ?
N2 Cu1 I1 104.68(9) . . ?
N2 Cu1 I1 110.37(9) . 2 ?
N3 Cu1 Cu1 151.09(10) . 2 ?
N3 Cu1 I1 110.11(9) . 2 ?
N3 Cu1 I1 108.95(9) . . ?
N3 Cu1 N2 109.14(14) . . ?
Cu1 I1 Cu1 60.41(2) 2 . ?
Sm1 O1W H1WA 105(3) . . ?
Sm1 O1W H1WB 118(3) . . ?
H1WA O1W H1WB 114.2(18) . . ?
C1 O1 Sm1 176.4(3) . . ?
C1 O2 Sm1 130.4(2) . 7_546 ?
Sm1 O2W H2WA 115(3) . . ?
Sm1 O2W H2WB 125(3) . . ?
H2WA O2W H2WB 114.7(19) . . ?
Sm1 O3 Sm1 116.13(10) 7_556 . ?
C9 O3 Sm1 84.5(2) . . ?
C9 O3 Sm1 153.7(2) . 7_556 ?
C9 O4 Sm1 101.9(2) . . ?
C17 O5 Sm1 94.8(2) . 6_565 ?
C17 O6 Sm1 91.6(2) . 6_565 ?
C8 N1 C7 116.5(4) . . ?
C15 N2 Cu1 123.2(3) . . ?
C16 N2 Cu1 119.3(3) . . ?
C16 N2 C15 117.1(3) . . ?
C23 N3 Cu1 124.3(3) . . ?
C23 N3 C24 116.3(4) . . ?
C24 N3 Cu1 119.4(3) . . ?
O1 C1 O2 124.0(3) . . ?
O1 C1 C2 119.4(3) . . ?
O2 C1 C2 116.6(3) . . ?
C1 C2 H2 118.1 . . ?
C3 C2 C1 123.8(4) . . ?
C3 C2 H2 118.1 . . ?
C2 C3 H3 116.3 . . ?
C2 C3 C4 127.4(4) . . ?
C4 C3 H3 116.3 . . ?
C5 C4 C3 121.0(4) . . ?
C8 C4 C3 122.5(4) . . ?
C8 C4 C5 116.5(4) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 C4 118.8(5) . . ?
C6 C5 H5 120.6 . . ?
C5 C6 H6 119.9 . . ?
C7 C6 C5 120.1(5) . . ?
C7 C6 H6 119.9 . . ?
N1 C7 C6 123.1(4) . . ?
N1 C7 H7 118.4 . . ?
C6 C7 H7 118.4 . . ?
N1 C8 C4 124.9(4) . . ?
N1 C8 H8 117.5 . . ?
C4 C8 H8 117.5 . . ?
O3 C9 Sm1 70.05(19) . . ?
O3 C9 C10 119.0(3) . . ?
O4 C9 Sm1 53.57(18) . . ?
O4 C9 O3 120.6(3) . . ?
O4 C9 C10 120.4(3) . . ?
C10 C9 Sm1 159.1(3) . . ?
C9 C10 H10 119.2 . . ?
C11 C10 C9 121.6(3) . . ?
C11 C10 H10 119.2 . . ?
C10 C11 H11 116.7 . . ?
C10 C11 C12 126.6(4) . . ?
C12 C11 H11 116.7 . . ?
C13 C12 C11 121.7(4) . . ?
C16 C12 C11 121.7(3) . . ?
C16 C12 C13 116.6(4) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 120.6 . . ?
C15 C14 C13 118.7(4) . . ?
C15 C14 H14 120.6 . . ?
N2 C15 C14 123.2(4) . . ?
N2 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
N2 C16 C12 124.3(4) . . ?
N2 C16 H16 117.9 . . ?
C12 C16 H16 117.9 . . ?
O5 C17 Sm1 59.33(19) . 6_565 ?
O5 C17 C18 117.1(4) . . ?
O6 C17 Sm1 62.53(18) . 6_565 ?
O6 C17 O5 121.8(3) . . ?
O6 C17 C18 121.0(4) . . ?
C18 C17 Sm1 174.6(3) . 6_565 ?
C17 C18 H18 118.2 . . ?
C19 C18 C17 123.5(4) . . ?
C19 C18 H18 118.2 . . ?
C18 C19 H19 116.9 . . ?
C18 C19 C20 126.2(4) . . ?
C20 C19 H19 116.9 . . ?
C21 C20 C19 120.7(4) . . ?
C21 C20 C24 117.7(4) . . ?
C24 C20 C19 121.6(4) . . ?
C20 C21 H21 120.4 . . ?
C20 C21 C22 119.1(5) . . ?
C22 C21 H21 120.4 . . ?
C21 C22 H22 120.6 . . ?
C23 C22 C21 118.8(5) . . ?
C23 C22 H22 120.6 . . ?
N3 C23 C22 123.5(4) . . ?
N3 C23 H23 118.2 . . ?
C22 C23 H23 118.2 . . ?
N3 C24 C20 124.5(4) . . ?
N3 C24 H24 117.8 . . ?
C20 C24 H24 117.8 . . ?
H3WA O3W H3WB 116(2) . . ?
H3BA O3B H3BB 116(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA I1 0.825(10) 3.007(12) 3.826(3) 173(4) 2_545
O1W H1WB O6 0.826(10) 2.022(11) 2.848(4) 178(4) 4_535
O2W H2WA O5 0.821(10) 1.890(10) 2.711(3) 178(4) 4_545
O2W H2WB N1 0.821(10) 1.973(16) 2.776(5) 166(5) 5_656
C2 H2 O3W 0.93 2.68 3.52(4) 151.4 8_556
C16 H16 I1 0.93 3.34 3.936(4) 124.0 2

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
Sm1 O2 C1 O1 -14.6(5) 7_546 . . . ?
Sm1 O2 C1 C2 164.4(2) 7_546 . . . ?
Sm1 O3 C9 Sm1 143.6(5) 7_556 . . . ?
Sm1 O3 C9 O4 162.2(4) 7_556 . . . ?
Sm1 O3 C9 O4 18.5(4) . . . . ?
Sm1 O3 C9 C10 -159.2(3) . . . . ?
Sm1 O3 C9 C10 -15.5(8) 7_556 . . . ?
Sm1 O4 C9 O3 -21.8(4) . . . . ?
Sm1 O4 C9 C10 155.9(3) . . . . ?
Sm1 O5 C17 O6 3.0(4) 6_565 . . . ?
Sm1 O5 C17 C18 -175.3(3) 6_565 . . . ?
Sm1 O6 C17 O5 -2.9(4) 6_565 . . . ?
Sm1 O6 C17 C18 175.3(3) 6_565 . . . ?
Sm1 C9 C10 C11 53.9(9) . . . . ?
Cu1 N2 C15 C14 -171.8(4) . . . . ?
Cu1 N2 C16 C12 172.4(3) . . . . ?
Cu1 N3 C23 C22 178.2(4) . . . . ?
Cu1 N3 C24 C20 -176.5(3) . . . . ?
O1 C1 C2 C3 -1.9(6) . . . . ?
O2 C1 C2 C3 179.1(4) . . . . ?
O3 C9 C10 C11 164.7(4) . . . . ?
O4 C9 C10 C11 -13.0(6) . . . . ?
O5 C17 C18 C19 173.4(4) . . . . ?
O6 C17 C18 C19 -4.9(6) . . . . ?
C1 C2 C3 C4 -179.8(4) . . . . ?
C2 C3 C4 C5 -176.4(4) . . . . ?
C2 C3 C4 C8 6.2(6) . . . . ?
C3 C4 C5 C6 -178.7(4) . . . . ?
C3 C4 C8 N1 177.7(4) . . . . ?
C4 C5 C6 C7 1.7(7) . . . . ?
C5 C4 C8 N1 0.3(6) . . . . ?
C5 C6 C7 N1 -1.3(8) . . . . ?
C7 N1 C8 C4 0.1(6) . . . . ?
C8 N1 C7 C6 0.4(7) . . . . ?
C8 C4 C5 C6 -1.2(6) . . . . ?
C9 C10 C11 C12 -173.9(4) . . . . ?
C10 C11 C12 C13 166.5(5) . . . . ?
C10 C11 C12 C16 -13.6(7) . . . . ?
C11 C12 C13 C14 -178.4(5) . . . . ?
C11 C12 C16 N2 179.4(4) . . . . ?
C12 C13 C14 C15 -1.4(8) . . . . ?
C13 C12 C16 N2 -0.7(7) . . . . ?
C13 C14 C15 N2 0.2(8) . . . . ?
C15 N2 C16 C12 -0.5(6) . . . . ?
C16 N2 C15 C14 0.8(7) . . . . ?
C16 C12 C13 C14 1.7(7) . . . . ?
C17 C18 C19 C20 178.8(4) . . . . ?
C18 C19 C20 C21 164.9(5) . . . . ?
C18 C19 C20 C24 -15.6(7) . . . . ?
C19 C20 C21 C22 -177.5(5) . . . . ?
C19 C20 C24 N3 177.2(4) . . . . ?
C20 C21 C22 C23 -1.4(9) . . . . ?
C21 C20 C24 N3 -3.3(7) . . . . ?
C21 C22 C23 N3 -0.2(9) . . . . ?
C23 N3 C24 C20 1.7(6) . . . . ?
C24 N3 C23 C22 0.1(7) . . . . ?
C24 C20 C21 C22 3.0(8) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 973526'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.25(C192 H176 Cu8 I8 N24 O64 Tb8), H2 O'
_chemical_formula_sum            'C48 H46 Cu2 I2 N6 O17 Tb2'
_chemical_formula_weight         1677.67
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.9956(15)
_cell_length_b                   9.2876(6)
_cell_length_c                   29.387(3)
_cell_angle_alpha                90
_cell_angle_beta                 110.5140(10)
_cell_angle_gamma                90
_cell_volume                     5622.7(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6757
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.947
_cell_measurement_theta_min      1.977
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.402
_exptl_absorpt_correction_T_max  0.415
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3224
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            16623
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.947
_diffrn_reflns_theta_min         1.977
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4852
_reflns_number_total             6486
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6486
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0331
_refine_ls_restrained_S_all      0.993
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0239P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0653
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O3W-H3WA = O3W-H3WB = O3B-H3BA = O3B-H3BB = O1W-H1WA = O1W-H1WB = O2W-H2WA =
 O2W-H2WB
 0.82 with sigma of 0.01
 H3WA-H3WB = H3BA-H3BB = H1WA-H1WB = H2WA-H2WB
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O3W \\sim O3B: within 3.8A with sigma of 0.02 and sigma for terminal atoms of
0.04
4. Others
 Sof(O3B)=Sof(H3BA)=Sof(H3BB)=0.5*(1-FVAR(2))
 Sof(O3W)=Sof(H3WA)=Sof(H3WB)=0.5*FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
  C24(H24)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.23012(2) 0.01405(2) 0.48757(2) 0.03026(6) Uani 1 1 d . . . . .
Cu1 Cu 0.06139(3) 0.81695(6) 0.25151(2) 0.04931(16) Uani 1 1 d . . . . .
I1 I -0.03468(2) 0.88142(4) 0.16956(2) 0.05067(10) Uani 1 1 d . . . . .
O1W O 0.21172(15) -0.1411(3) 0.41339(11) 0.0406(7) Uani 1 1 d D . . . .
H1WA H 0.1728(7) -0.139(4) 0.3968(15) 0.061 Uiso 1 1 d DR . . . .
H1WB H 0.2280(16) -0.222(2) 0.4177(17) 0.061 Uiso 1 1 d DR . . . .
O1 O 0.31348(13) -0.1443(3) 0.50824(11) 0.0439(8) Uani 1 1 d . . . . .
O2 O 0.35865(13) -0.3598(3) 0.52167(11) 0.0412(7) Uani 1 1 d . . . . .
O2W O 0.28901(15) 0.1107(3) 0.43943(13) 0.0447(8) Uani 1 1 d D . . . .
H2WA H 0.3033(19) 0.1935(18) 0.4441(17) 0.067 Uiso 1 1 d DR . . . .
H2WB H 0.3103(19) 0.056(3) 0.4287(18) 0.067 Uiso 1 1 d DR . . . .
O3 O 0.19705(14) 0.3111(3) 0.46378(10) 0.0421(8) Uani 1 1 d . . . . .
O4 O 0.14717(14) 0.1234(3) 0.42190(11) 0.0443(8) Uani 1 1 d . . . A 1
O5 O 0.17487(15) 0.8912(3) 0.04043(11) 0.0421(7) Uani 1 1 d . . . B 1
O6 O 0.24217(14) 1.0692(3) 0.07220(10) 0.0401(7) Uani 1 1 d . . . B 1
N1 N 0.61931(18) 0.0355(5) 0.58813(16) 0.0552(11) Uani 1 1 d . . . C 1
N2 N 0.07525(18) 0.5962(4) 0.24812(13) 0.0429(9) Uani 1 1 d . . . A 1
N3 N 0.14406(18) 0.9241(4) 0.25284(14) 0.0452(9) Uani 1 1 d . . . B 1
C1 C 0.36222(19) -0.2251(4) 0.52204(14) 0.0309(9) Uani 1 1 d . . . C 1
C2 C 0.4279(2) -0.1616(5) 0.54033(17) 0.0435(12) Uani 1 1 d . . . C 1
H2 H 0.4634 -0.2236 0.5508 0.052 Uiso 1 1 calc R . . C 1
C3 C 0.4389(2) -0.0231(5) 0.54265(16) 0.0418(11) Uani 1 1 d . . . C 1
H3 H 0.4026 0.0362 0.5317 0.050 Uiso 1 1 calc R . . C 1
C4 C 0.5025(2) 0.0498(5) 0.56061(16) 0.0407(11) Uani 1 1 d . . . C 1
C5 C 0.5065(2) 0.1993(5) 0.5640(2) 0.0567(14) Uani 1 1 d . . . C 1
H5 H 0.4691 0.2551 0.5556 0.068 Uiso 1 1 calc R . . C 1
C6 C 0.5672(3) 0.2634(6) 0.5799(2) 0.0669(16) Uani 1 1 d . . . C 1
H6 H 0.5712 0.3629 0.5832 0.080 Uiso 1 1 calc R . . C 1
C7 C 0.6215(3) 0.1785(6) 0.5909(2) 0.0624(16) Uani 1 1 d . . . C 1
H7 H 0.6618 0.2232 0.6007 0.075 Uiso 1 1 calc R . . C 1
C8 C 0.5607(2) -0.0252(5) 0.57305(18) 0.0480(12) Uani 1 1 d . . . C 1
H8 H 0.5586 -0.1251 0.5707 0.058 Uiso 1 1 calc R . . C 1
C9 C 0.16122(19) 0.2548(4) 0.42427(15) 0.0321(10) Uani 1 1 d . . . A 1
C10 C 0.1377(2) 0.3451(4) 0.38024(15) 0.0371(10) Uani 1 1 d . . . A 1
H10 H 0.1401 0.4447 0.3838 0.045 Uiso 1 1 calc R . . A 1
C11 C 0.1135(2) 0.2911(4) 0.33654(16) 0.0429(11) Uani 1 1 d . . . A 1
H11 H 0.1068 0.1921 0.3345 0.051 Uiso 1 1 calc R . . A 1
C12 C 0.0957(2) 0.3695(5) 0.29007(16) 0.0402(11) Uani 1 1 d . . . A 1
C13 C 0.0805(3) 0.2995(6) 0.24631(18) 0.0613(15) Uani 1 1 d . . . A 1
H13 H 0.0804 0.1994 0.2453 0.074 Uiso 1 1 calc R . . A 1
C14 C 0.0653(3) 0.3776(6) 0.20388(19) 0.0687(17) Uani 1 1 d . . . A 1
H14 H 0.0567 0.3314 0.1742 0.082 Uiso 1 1 calc R . . A 1
C15 C 0.0632(2) 0.5251(6) 0.20646(17) 0.0563(14) Uani 1 1 d . . . A 1
H15 H 0.0529 0.5778 0.1778 0.068 Uiso 1 1 calc R . . A 1
C16 C 0.0912(2) 0.5191(5) 0.28893(16) 0.0408(11) Uani 1 1 d . . . A 1
H16 H 0.0997 0.5678 0.3182 0.049 Uiso 1 1 calc R . . A 1
C17 C 0.2029(2) 0.9743(4) 0.07554(16) 0.0379(10) Uani 1 1 d . . . B 1
C18 C 0.1901(2) 0.9540(5) 0.12167(17) 0.0442(11) Uani 1 1 d . . . B 1
H18 H 0.1584 0.8882 0.1219 0.053 Uiso 1 1 calc R . . B 1
C19 C 0.2210(2) 1.0235(5) 0.16177(17) 0.0448(11) Uani 1 1 d . . . B 1
H19 H 0.2527 1.0886 0.1610 0.054 Uiso 1 1 calc R . . B 1
C20 C 0.2099(2) 1.0081(5) 0.20824(17) 0.0448(11) Uani 1 1 d . . . B 1
C21 C 0.2549(3) 1.0597(7) 0.2507(2) 0.0706(17) Uani 1 1 d . . . B 1
H21 H 0.2919 1.1071 0.2501 0.085 Uiso 1 1 calc R . . B 1
C22 C 0.2450(3) 1.0410(7) 0.2940(2) 0.080(2) Uani 1 1 d . . . B 1
H22 H 0.2753 1.0738 0.3229 0.096 Uiso 1 1 calc R . . B 1
C23 C 0.1892(2) 0.9725(6) 0.29364(18) 0.0580(14) Uani 1 1 d . . . B 1
H23 H 0.1826 0.9595 0.3230 0.070 Uiso 1 1 calc R . . B 1
C24 C 0.1551(2) 0.9438(5) 0.21138(17) 0.0441(11) Uani 1 1 d . . . B 1
H24 H 0.1237 0.9122 0.1827 0.053 Uiso 1 1 calc R . . B 1
O3W O 0.0489(18) 0.891(4) 0.033(2) 0.192(13) Uani 0.152(8) 1 d D U P D 1
H3WA H 0.019(10) 0.91(5) 0.042(9) 0.288 Uiso 0.152(8) 1 d DR . P D 1
H3WB H 0.055(15) 0.95(3) 0.013(9) 0.288 Uiso 0.152(8) 1 d DR . P D 1
O3B O -0.0179(9) 0.9812(18) 0.0473(9) 0.190(10) Uani 0.348(8) 1 d D U P D 2
H3BA H -0.045(11) 1.00(3) 0.021(6) 0.284 Uiso 0.348(8) 1 d DR . P D 2
H3BB H 0.010(9) 0.93(3) 0.046(11) 0.284 Uiso 0.348(8) 1 d DR . P D 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1W 2.525(3) . ?
Tb1 O1 2.261(3) . ?
Tb1 O2 2.359(3) 7_546 ?
Tb1 O2W 2.402(3) . ?
Tb1 O3 2.876(3) . ?
Tb1 O3 2.375(3) 7_556 ?
Tb1 O4 2.370(3) . ?
Tb1 O5 2.447(3) 6_566 ?
Tb1 O6 2.528(3) 6_566 ?
Tb1 C9 2.963(4) . ?
Tb1 C17 2.853(5) 6_566 ?
Cu1 Cu1 2.6708(12) 2 ?
Cu1 I1 2.6566(7) . ?
Cu1 I1 2.6530(7) 2 ?
Cu1 N2 2.080(4) . ?
Cu1 N3 2.061(4) . ?
I1 Cu1 2.6529(7) 2 ?
O1W H1WA 0.824(10) . ?
O1W H1WB 0.822(10) . ?
O1 C1 1.254(4) . ?
O2 Tb1 2.359(3) 7_546 ?
O2 C1 1.254(4) . ?
O2W H2WA 0.824(10) . ?
O2W H2WB 0.825(10) . ?
O3 Tb1 2.375(3) 7_556 ?
O3 C9 1.265(5) . ?
O4 C9 1.255(4) . ?
O5 Tb1 2.447(3) 6_565 ?
O5 C17 1.263(5) . ?
O6 Tb1 2.528(3) 6_565 ?
O6 C17 1.262(5) . ?
N1 C7 1.331(6) . ?
N1 C8 1.333(5) . ?
N2 C15 1.333(6) . ?
N2 C16 1.334(5) . ?
N3 C23 1.338(6) . ?
N3 C24 1.336(5) . ?
C1 C2 1.477(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.307(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.474(6) . ?
C4 C5 1.392(6) . ?
C4 C8 1.389(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.386(6) . ?
C6 H6 0.9300 . ?
C6 C7 1.370(7) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.475(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.306(6) . ?
C11 H11 0.9300 . ?
C11 C12 1.474(6) . ?
C12 C13 1.374(6) . ?
C12 C16 1.393(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.378(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.374(7) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 Tb1 2.853(5) 6_565 ?
C17 C18 1.490(6) . ?
C18 H18 0.9300 . ?
C18 C19 1.306(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.475(6) . ?
C20 C21 1.379(7) . ?
C20 C24 1.378(6) . ?
C21 H21 0.9300 . ?
C21 C22 1.373(7) . ?
C22 H22 0.9300 . ?
C22 C23 1.380(7) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
O3W H3WA 0.820(10) . ?
O3W H3WB 0.820(10) . ?
O3B H3BA 0.821(10) . ?
O3B H3BB 0.820(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1W Tb1 O3 112.78(9) . . ?
O1W Tb1 O6 127.20(9) . 6_566 ?
O1W Tb1 C9 89.81(11) . . ?
O1W Tb1 C17 141.56(10) . 6_566 ?
O1 Tb1 O1W 74.35(10) . . ?
O1 Tb1 O2 101.34(10) . 7_546 ?
O1 Tb1 O2W 81.21(11) . . ?
O1 Tb1 O3 88.31(10) . 7_556 ?
O1 Tb1 O3 143.26(9) . . ?
O1 Tb1 O4 144.88(11) . . ?
O1 Tb1 O5 126.85(11) . 6_566 ?
O1 Tb1 O6 75.00(11) . 6_566 ?
O1 Tb1 C9 147.95(11) . . ?
O1 Tb1 C17 100.90(13) . 6_566 ?
O2 Tb1 O1W 71.24(10) 7_546 . ?
O2 Tb1 O2W 138.97(11) 7_546 . ?
O2 Tb1 O3 115.20(9) 7_546 . ?
O2 Tb1 O3 147.22(11) 7_546 7_556 ?
O2 Tb1 O4 78.26(10) 7_546 . ?
O2 Tb1 O5 73.53(10) 7_546 6_566 ?
O2 Tb1 O6 74.03(10) 7_546 6_566 ?
O2 Tb1 C9 99.51(10) 7_546 . ?
O2 Tb1 C17 72.51(11) 7_546 6_566 ?
O2W Tb1 O1W 70.18(10) . . ?
O2W Tb1 O3 68.98(9) . . ?
O2W Tb1 O5 136.87(9) . 6_566 ?
O2W Tb1 O6 143.26(11) . 6_566 ?
O2W Tb1 C9 67.12(11) . . ?
O2W Tb1 C17 147.92(11) . 6_566 ?
O3 Tb1 O1W 141.27(10) 7_556 . ?
O3 Tb1 O2W 73.13(11) 7_556 . ?
O3 Tb1 O3 63.27(10) 7_556 . ?
O3 Tb1 O5 75.65(10) 7_556 6_566 ?
O3 Tb1 O6 78.52(9) 7_556 6_566 ?
O3 Tb1 C9 87.17(11) 7_556 . ?
O3 Tb1 C9 24.97(9) . . ?
O3 Tb1 C17 74.93(11) 7_556 6_566 ?
O4 Tb1 O1W 72.36(10) . . ?
O4 Tb1 O2W 77.32(11) . . ?
O4 Tb1 O3 111.18(10) . 7_556 ?
O4 Tb1 O3 48.24(8) . . ?
O4 Tb1 O5 87.18(11) . 6_566 ?
O4 Tb1 O6 135.85(10) . 6_566 ?
O4 Tb1 C9 24.08(10) . . ?
O4 Tb1 C17 112.05(13) . 6_566 ?
O5 Tb1 O1W 142.05(10) 6_566 . ?
O5 Tb1 O3 70.71(9) 6_566 . ?
O5 Tb1 O6 52.39(9) 6_566 6_566 ?
O5 Tb1 C9 82.44(11) 6_566 . ?
O5 Tb1 C17 26.16(11) 6_566 6_566 ?
O6 Tb1 O3 117.58(9) 6_566 . ?
O6 Tb1 C9 134.64(11) 6_566 . ?
O6 Tb1 C17 26.25(11) 6_566 6_566 ?
C17 Tb1 O3 93.91(11) 6_566 . ?
C17 Tb1 C9 108.46(13) 6_566 . ?
I1 Cu1 Cu1 59.87(2) 2 2 ?
I1 Cu1 Cu1 59.73(2) . 2 ?
I1 Cu1 I1 113.09(2) 2 . ?
N2 Cu1 Cu1 99.31(10) . 2 ?
N2 Cu1 I1 105.19(10) . . ?
N2 Cu1 I1 110.21(11) . 2 ?
N3 Cu1 Cu1 151.13(11) . 2 ?
N3 Cu1 I1 109.80(11) . 2 ?
N3 Cu1 I1 108.94(11) . . ?
N3 Cu1 N2 109.48(15) . . ?
Cu1 I1 Cu1 60.40(2) 2 . ?
Tb1 O1W H1WA 108(3) . . ?
Tb1 O1W H1WB 117(3) . . ?
H1WA O1W H1WB 114.9(19) . . ?
C1 O1 Tb1 175.6(3) . . ?
C1 O2 Tb1 130.8(3) . 7_546 ?
Tb1 O2W H2WA 120(3) . . ?
Tb1 O2W H2WB 119(3) . . ?
H2WA O2W H2WB 113.9(19) . . ?
Tb1 O3 Tb1 116.72(10) 7_556 . ?
C9 O3 Tb1 81.4(2) . . ?
C9 O3 Tb1 155.0(3) . 7_556 ?
C9 O4 Tb1 105.5(2) . . ?
C17 O5 Tb1 95.2(3) . 6_565 ?
C17 O6 Tb1 91.4(3) . 6_565 ?
C7 N1 C8 116.9(4) . . ?
C15 N2 Cu1 123.2(3) . . ?
C15 N2 C16 117.7(4) . . ?
C16 N2 Cu1 118.9(3) . . ?
C23 N3 Cu1 123.5(3) . . ?
C24 N3 Cu1 119.4(3) . . ?
C24 N3 C23 117.2(4) . . ?
O1 C1 O2 123.4(4) . . ?
O1 C1 C2 119.8(4) . . ?
O2 C1 C2 116.8(4) . . ?
C1 C2 H2 118.3 . . ?
C3 C2 C1 123.4(4) . . ?
C3 C2 H2 118.3 . . ?
C2 C3 H3 116.4 . . ?
C2 C3 C4 127.3(4) . . ?
C4 C3 H3 116.4 . . ?
C5 C4 C3 120.8(4) . . ?
C8 C4 C3 122.3(4) . . ?
C8 C4 C5 116.9(4) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 C4 118.8(5) . . ?
C6 C5 H5 120.6 . . ?
C5 C6 H6 120.4 . . ?
C7 C6 C5 119.3(5) . . ?
C7 C6 H6 120.4 . . ?
N1 C7 C6 123.4(4) . . ?
N1 C7 H7 118.3 . . ?
C6 C7 H7 118.3 . . ?
N1 C8 C4 124.8(4) . . ?
N1 C8 H8 117.6 . . ?
C4 C8 H8 117.6 . . ?
O3 C9 Tb1 73.7(2) . . ?
O3 C9 C10 119.0(4) . . ?
O4 C9 Tb1 50.4(2) . . ?
O4 C9 O3 121.0(4) . . ?
O4 C9 C10 120.0(4) . . ?
C10 C9 Tb1 157.6(3) . . ?
C9 C10 H10 118.6 . . ?
C11 C10 C9 122.8(4) . . ?
C11 C10 H10 118.6 . . ?
C10 C11 H11 116.3 . . ?
C10 C11 C12 127.3(4) . . ?
C12 C11 H11 116.3 . . ?
C13 C12 C11 122.1(4) . . ?
C13 C12 C16 117.3(4) . . ?
C16 C12 C11 120.6(4) . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.0(5) . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 120.8 . . ?
C15 C14 C13 118.5(5) . . ?
C15 C14 H14 120.8 . . ?
N2 C15 C14 123.0(5) . . ?
N2 C15 H15 118.5 . . ?
C14 C15 H15 118.5 . . ?
N2 C16 C12 123.4(4) . . ?
N2 C16 H16 118.3 . . ?
C12 C16 H16 118.3 . . ?
O5 C17 Tb1 58.7(2) . 6_565 ?
O5 C17 C18 118.2(4) . . ?
O6 C17 Tb1 62.4(2) . 6_565 ?
O6 C17 O5 121.0(4) . . ?
O6 C17 C18 120.8(4) . . ?
C18 C17 Tb1 174.8(3) . 6_565 ?
C17 C18 H18 118.2 . . ?
C19 C18 C17 123.7(5) . . ?
C19 C18 H18 118.2 . . ?
C18 C19 H19 117.1 . . ?
C18 C19 C20 125.8(5) . . ?
C20 C19 H19 117.1 . . ?
C21 C20 C19 120.4(4) . . ?
C24 C20 C19 122.4(4) . . ?
C24 C20 C21 117.2(5) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 C20 119.8(5) . . ?
C22 C21 H21 120.1 . . ?
C21 C22 H22 120.6 . . ?
C21 C22 C23 118.8(5) . . ?
C23 C22 H22 120.6 . . ?
N3 C23 C22 122.7(5) . . ?
N3 C23 H23 118.7 . . ?
C22 C23 H23 118.7 . . ?
N3 C24 C20 124.3(4) . . ?
N3 C24 H24 117.8 . . ?
C20 C24 H24 117.8 . . ?
H3WA O3W H3WB 116(2) . . ?
H3BA O3B H3BB 116(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA I1 0.824(10) 2.986(11) 3.808(3) 175(4) 2_545
O1W H1WB O6 0.822(10) 2.036(12) 2.854(4) 173(4) 4_535
O2W H2WA O5 0.824(10) 1.912(11) 2.728(4) 170(4) 4_545
O2W H2WB N1 0.825(10) 1.975(17) 2.777(5) 164(4) 5_656
C2 H2 O3W 0.93 2.64 3.48(4) 150.9 8_556
C16 H16 I1 0.93 3.32 3.926(4) 124.9 2

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
Tb1 O2 C1 O1 -13.8(6) 7_546 . . . ?
Tb1 O2 C1 C2 165.6(3) 7_546 . . . ?
Tb1 O3 C9 Tb1 138.7(6) 7_556 . . . ?
Tb1 O3 C9 O4 156.8(5) 7_556 . . . ?
Tb1 O3 C9 O4 18.1(4) . . . . ?
Tb1 O3 C9 C10 -159.9(4) . . . . ?
Tb1 O3 C9 C10 -21.2(9) 7_556 . . . ?
Tb1 O4 C9 O3 -22.7(5) . . . . ?
Tb1 O4 C9 C10 155.2(3) . . . . ?
Tb1 O5 C17 O6 2.8(4) 6_565 . . . ?
Tb1 O5 C17 C18 -175.3(3) 6_565 . . . ?
Tb1 O6 C17 O5 -2.7(4) 6_565 . . . ?
Tb1 O6 C17 C18 175.3(3) 6_565 . . . ?
Tb1 C9 C10 C11 43.9(10) . . . . ?
Cu1 N2 C15 C14 -172.4(4) . . . . ?
Cu1 N2 C16 C12 173.9(3) . . . . ?
Cu1 N3 C23 C22 178.4(4) . . . . ?
Cu1 N3 C24 C20 -177.0(4) . . . . ?
O1 C1 C2 C3 -0.8(7) . . . . ?
O2 C1 C2 C3 179.8(4) . . . . ?
O3 C9 C10 C11 163.9(4) . . . . ?
O4 C9 C10 C11 -14.1(7) . . . . ?
O5 C17 C18 C19 173.0(4) . . . . ?
O6 C17 C18 C19 -5.0(7) . . . . ?
C1 C2 C3 C4 179.5(4) . . . . ?
C2 C3 C4 C5 -175.6(5) . . . . ?
C2 C3 C4 C8 7.0(8) . . . . ?
C3 C4 C5 C6 -178.4(5) . . . . ?
C3 C4 C8 N1 178.0(4) . . . . ?
C4 C5 C6 C7 1.5(8) . . . . ?
C5 C4 C8 N1 0.6(7) . . . . ?
C5 C6 C7 N1 -1.6(9) . . . . ?
C7 N1 C8 C4 -0.6(8) . . . . ?
C8 N1 C7 C6 1.2(8) . . . . ?
C8 C4 C5 C6 -0.9(7) . . . . ?
C9 C10 C11 C12 -172.3(4) . . . . ?
C10 C11 C12 C13 169.3(5) . . . . ?
C10 C11 C12 C16 -13.3(8) . . . . ?
C11 C12 C13 C14 -178.8(5) . . . . ?
C11 C12 C16 N2 -179.9(4) . . . . ?
C12 C13 C14 C15 -2.7(9) . . . . ?
C13 C12 C16 N2 -2.5(7) . . . . ?
C13 C14 C15 N2 0.1(9) . . . . ?
C15 N2 C16 C12 0.0(7) . . . . ?
C16 N2 C15 C14 1.3(8) . . . . ?
C16 C12 C13 C14 3.8(8) . . . . ?
C17 C18 C19 C20 179.7(4) . . . . ?
C18 C19 C20 C21 164.4(5) . . . . ?
C18 C19 C20 C24 -16.2(8) . . . . ?
C19 C20 C21 C22 -178.2(5) . . . . ?
C19 C20 C24 N3 178.0(4) . . . . ?
C20 C21 C22 C23 -1.1(10) . . . . ?
C21 C20 C24 N3 -2.5(8) . . . . ?
C21 C22 C23 N3 -0.3(10) . . . . ?
C23 N3 C24 C20 1.2(7) . . . . ?
C24 N3 C23 C22 0.3(8) . . . . ?
C24 C20 C21 C22 2.4(9) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_10
_database_code_depnum_ccdc_archive 'CCDC 973527'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-04-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C24 H24 Br Cu Eu N3 O8, O'
_chemical_formula_sum            'C24 H24 Br Cu Eu N3 O9'
_chemical_formula_weight         793.88
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.078(2)
_cell_length_b                   9.3534(9)
_cell_length_c                   28.855(4)
_cell_angle_alpha                90
_cell_angle_beta                 109.7880(10)
_cell_angle_gamma                90
_cell_volume                     5606.8(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1728
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.93
_cell_measurement_theta_min      2.39
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.455
_exptl_absorpt_correction_T_max  0.410
_exptl_absorpt_correction_T_min  0.357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0911 before and 0.0543 after correction.
The Ratio of minimum to maximum transmission is 0.8094.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   'Apex2 (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            14348
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.398
_diffrn_reflns_theta_min         1.500
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3625
_reflns_number_total             5186
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5167
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0476
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0424P)²+12.4284P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1144
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Sof(O3WB)=1-FVAR(1)
 Sof(O3WA)=FVAR(1)
3.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C2(H2), C7(H7), C10(H10), C11(H11), C6(H6), C5(H5), C16(H16),
 C23(H23), C24(H24), C21(H21), C22(H22), C14(H14), C15(H15), C13(H13), C19(H19),
  C18(H18)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.49125(2) 0.26610(4) 0.51240(2) 0.02915(13) Uani 1 1 d . . . . .
Br1 Br 0.52535(5) 1.10890(12) 0.82278(3) 0.0684(3) Uani 1 1 d . . . . .
Cu3 Cu 0.56778(6) 1.05100(13) 0.75530(4) 0.0619(3) Uani 1 1 d . . . . .
O1W O 0.5957(2) 0.3643(5) 0.56022(19) 0.0438(14) Uani 1 1 d . . . . .
H1WA H 0.6024 0.4410 0.5468 0.066 Uiso 1 1 d GR . . . .
H1WB H 0.6248 0.3035 0.5612 0.066 Uiso 1 1 d GR . . . .
O1 O 0.4128(2) 0.1088(5) 0.52378(19) 0.0418(13) Uani 1 1 d . . . . .
O2W O 0.5450(2) 0.1073(5) 0.58716(18) 0.0429(13) Uani 1 1 d . . . . .
H2WA H 0.5196 0.0975 0.6038 0.064 Uiso 1 1 d GR . . . .
H2WB H 0.5802 0.1455 0.6055 0.064 Uiso 1 1 d GR . . . .
O2 O 0.4469(2) -0.1055(5) 0.5117(2) 0.0457(14) Uani 1 1 d . . . . .
O3 O 0.4825(2) 0.5545(5) 0.53851(18) 0.0400(13) Uani 1 1 d . . . . .
C3 C 0.3510(3) -0.2279(8) 0.5441(3) 0.0361(18) Uani 1 1 d . . . . .
H3 H 0.3781 -0.2875 0.5342 0.043 Uiso 1 1 calc R . . . .
C8 C 0.2571(4) -0.2220(8) 0.5740(3) 0.042(2) Uani 1 1 d . . . . .
H8 H 0.2585 -0.1227 0.5727 0.050 Uiso 1 1 calc R . . . .
C4 C 0.3028(3) -0.2996(8) 0.5606(3) 0.0379(19) Uani 1 1 d . . . . .
N1 N 0.2117(3) -0.2819(7) 0.5885(3) 0.0480(18) Uani 1 1 d . . . . .
C2 C 0.3606(4) -0.0915(8) 0.5416(3) 0.042(2) Uani 1 1 d . . . . .
H2 H 0.3343 -0.0304 0.5518 0.050 Uiso 1 1 calc R . . . .
C7 C 0.2101(4) -0.4238(10) 0.5895(4) 0.060(3) Uani 1 1 d . . . . .
H7 H 0.1779 -0.4676 0.5985 0.072 Uiso 1 1 calc R . . . .
C10 C 0.5059(4) 0.5883(8) 0.6237(3) 0.044(2) Uani 1 1 d . . . . .
H10 H 0.5050 0.6872 0.6202 0.053 Uiso 1 1 calc R . . . .
C9 C 0.4840(4) 0.4993(8) 0.5797(3) 0.0342(18) Uani 1 1 d . . . . .
C11 C 0.5267(4) 0.5331(9) 0.6681(3) 0.051(2) Uani 1 1 d . . . . .
H11 H 0.5224 0.4347 0.6703 0.061 Uiso 1 1 calc R . . . .
O4 O 0.4702(3) 0.3700(5) 0.58151(19) 0.0438(14) Uani 1 1 d . . . . .
C6 C 0.2530(4) -0.5083(10) 0.5779(4) 0.068(3) Uani 1 1 d . . . . .
H6 H 0.2512 -0.6072 0.5805 0.082 Uiso 1 1 calc R . . . .
C5 C 0.2989(4) -0.4452(9) 0.5624(3) 0.054(2) Uani 1 1 d . . . . .
H5 H 0.3274 -0.5017 0.5530 0.064 Uiso 1 1 calc R . . . .
N2 N 0.5796(3) 0.8356(8) 0.7584(3) 0.0492(18) Uani 1 1 d . . . . .
C16 C 0.5555(4) 0.7581(9) 0.7171(3) 0.045(2) Uani 1 1 d . . . . .
H16 H 0.5367 0.8072 0.6877 0.054 Uiso 1 1 calc R . . . .
C12 C 0.5566(4) 0.6111(9) 0.7151(3) 0.048(2) Uani 1 1 d . . . . .
N3 N 0.6448(3) 1.1657(8) 0.7536(3) 0.0510(19) Uani 1 1 d . . . . .
C20 C 0.7527(4) 1.2511(10) 0.7944(3) 0.052(2) Uani 1 1 d . . . . .
C23 C 0.6489(4) 1.2178(11) 0.7121(3) 0.067(3) Uani 1 1 d . . . . .
H23 H 0.6141 1.2060 0.6832 0.080 Uiso 1 1 calc R . . . .
C24 C 0.6968(4) 1.1838(10) 0.7942(3) 0.055(2) Uani 1 1 d . . . . .
H24 H 0.6950 1.1490 0.8239 0.066 Uiso 1 1 calc R . . . .
C21 C 0.7551(4) 1.3054(13) 0.7519(4) 0.080(3) Uani 1 1 d . . . . .
H21 H 0.7916 1.3531 0.7510 0.096 Uiso 1 1 calc R . . . .
C22 C 0.7027(5) 1.2890(13) 0.7100(4) 0.086(4) Uani 1 1 d . . . . .
H22 H 0.7033 1.3256 0.6802 0.103 Uiso 1 1 calc R . . . .
C14 C 0.6127(5) 0.6180(12) 0.8019(3) 0.076(3) Uani 1 1 d . . . . .
H14 H 0.6341 0.5718 0.8315 0.091 Uiso 1 1 calc R . . . .
C15 C 0.6085(4) 0.7630(11) 0.7999(3) 0.065(3) Uani 1 1 d . . . . .
H15 H 0.6267 0.8143 0.8289 0.077 Uiso 1 1 calc R . . . .
C13 C 0.5845(5) 0.5399(11) 0.7590(3) 0.068(3) Uani 1 1 d . . . . .
H13 H 0.5844 0.4405 0.7599 0.082 Uiso 1 1 calc R . . . .
C19 C 0.8097(4) 1.2659(10) 0.8403(3) 0.057(2) Uani 1 1 d . . . . .
H19 H 0.8414 1.3301 0.8393 0.068 Uiso 1 1 calc R . . . .
C18 C 0.8192(4) 1.2009(10) 0.8800(4) 0.060(3) Uani 1 1 d . . . . .
H18 H 0.7879 1.1365 0.8816 0.072 Uiso 1 1 calc R . . . .
C17 C 0.8787(4) 1.2200(9) 0.9259(4) 0.049(2) Uani 1 1 d . . . . .
O6 O 0.8853(2) 1.1406(6) 0.9612(2) 0.0489(15) Uani 1 1 d . . . . .
O5 O 0.9210(3) 1.3127(6) 0.9267(2) 0.0481(15) Uani 1 1 d . . . . .
O3WB O 0.321(3) 0.157(9) 0.603(2) 0.12(3) Uiso 0.17(4) 1 d . . P A 2
C1 C 0.4097(3) -0.0242(8) 0.5241(3) 0.0311(17) Uani 1 1 d . . . . .
O3WA O 0.3417(7) 0.2224(17) 0.5897(5) 0.117(6) Uiso 0.83(4) 1 d . . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 Eu1 4.4714(8) 5_666 ?
Eu1 O1W 2.431(5) . ?
Eu1 O1 2.379(5) . ?
Eu1 O2W 2.556(5) . ?
Eu1 O2 2.291(5) 5_656 ?
Eu1 O3 2.427(5) 5_666 ?
Eu1 O3 2.825(5) . ?
Eu1 O4 2.401(5) . ?
Eu1 C17 2.868(9) 8_465 ?
Eu1 O6 2.465(5) 8_465 ?
Eu1 O5 2.542(5) 8_465 ?
Br1 Cu3 2.4892(15) . ?
Br1 Cu3 2.5418(16) 2_656 ?
Cu3 Br1 2.5418(16) 2_656 ?
Cu3 Cu3 2.903(2) 2_656 ?
Cu3 N2 2.030(8) . ?
Cu3 N3 2.024(7) . ?
O1 C1 1.246(8) . ?
O2 Eu1 2.291(5) 5_656 ?
O2 C1 1.256(8) . ?
O3 Eu1 2.427(5) 5_666 ?
O3 C9 1.284(8) . ?
C3 C4 1.467(10) . ?
C3 C2 1.300(9) . ?
C8 C4 1.399(11) . ?
C8 N1 1.335(9) . ?
C4 C5 1.366(10) . ?
N1 C7 1.329(10) . ?
C2 C1 1.482(10) . ?
C7 C6 1.359(12) . ?
C10 C9 1.458(10) . ?
C10 C11 1.311(10) . ?
C9 O4 1.253(8) . ?
C11 C12 1.484(11) . ?
C6 C5 1.373(11) . ?
N2 C16 1.342(10) . ?
N2 C15 1.334(11) . ?
C16 C12 1.376(11) . ?
C12 C13 1.379(12) . ?
N3 C23 1.324(11) . ?
N3 C24 1.345(10) . ?
C20 C24 1.384(12) . ?
C20 C21 1.345(13) . ?
C20 C19 1.493(11) . ?
C23 C22 1.380(13) . ?
C21 C22 1.372(12) . ?
C14 C15 1.360(13) . ?
C14 C13 1.390(13) . ?
C19 C18 1.248(12) . ?
C18 C17 1.528(12) . ?
C17 Eu1 2.868(9) 8_566 ?
C17 O6 1.228(10) . ?
C17 O5 1.269(10) . ?
O6 Eu1 2.465(5) 8_566 ?
O5 Eu1 2.542(5) 8_566 ?

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
O1W Eu1 Eu1 66.69(12) . 5_666 ?
O1W Eu1 O2W 70.17(16) . . ?
O1W Eu1 O3 67.99(16) . . ?
O1W Eu1 C17 148.52(19) . 8_465 ?
O1W Eu1 O6 137.02(18) . 8_465 ?
O1W Eu1 O5 144.17(18) . 8_465 ?
O1 Eu1 Eu1 137.19(12) . 5_666 ?
O1 Eu1 O1W 138.64(18) . . ?
O1 Eu1 O2W 71.09(17) . . ?
O1 Eu1 O3 115.77(16) . . ?
O1 Eu1 O3 147.74(17) . 5_666 ?
O1 Eu1 O4 77.34(18) . . ?
O1 Eu1 C17 72.0(2) . 8_465 ?
O1 Eu1 O6 73.39(18) . 8_465 ?
O1 Eu1 O5 73.83(18) . 8_465 ?
O2W Eu1 Eu1 131.54(12) . 5_666 ?
O2W Eu1 O3 112.58(16) . . ?
O2W Eu1 C17 141.14(19) . 8_465 ?
O2 Eu1 Eu1 120.02(13) 5_656 5_666 ?
O2 Eu1 O1W 82.65(18) 5_656 . ?
O2 Eu1 O1 99.98(18) 5_656 . ?
O2 Eu1 O2W 73.82(18) 5_656 . ?
O2 Eu1 O3 143.98(16) 5_656 . ?
O2 Eu1 O3 88.87(18) 5_656 5_666 ?
O2 Eu1 O4 145.15(19) 5_656 . ?
O2 Eu1 C17 101.3(3) 5_656 8_465 ?
O2 Eu1 O6 126.3(2) 5_656 8_465 ?
O2 Eu1 O5 75.2(2) 5_656 8_465 ?
O3 Eu1 Eu1 29.04(10) . 5_666 ?
O3 Eu1 Eu1 34.41(12) 5_666 5_666 ?
O3 Eu1 O1W 72.97(17) 5_666 . ?
O3 Eu1 O2W 140.82(16) 5_666 . ?
O3 Eu1 O3 63.45(19) 5_666 . ?
O3 Eu1 C17 75.88(19) 5_666 8_465 ?
O3 Eu1 C17 94.1(2) . 8_465 ?
O3 Eu1 O6 76.39(17) 5_666 8_465 ?
O3 Eu1 O5 78.70(17) 5_666 8_465 ?
O4 Eu1 Eu1 77.79(12) . 5_666 ?
O4 Eu1 O1W 77.81(18) . . ?
O4 Eu1 O2W 72.50(17) . . ?
O4 Eu1 O3 48.85(16) . . ?
O4 Eu1 O3 112.09(17) . 5_666 ?
O4 Eu1 C17 110.5(3) . 8_465 ?
O4 Eu1 O6 86.8(2) . 8_465 ?
O4 Eu1 O5 134.33(19) . 8_465 ?
C17 Eu1 Eu1 84.99(16) 8_465 5_666 ?
O6 Eu1 Eu1 70.94(12) 8_465 5_666 ?
O6 Eu1 O2W 141.90(17) 8_465 . ?
O6 Eu1 O3 71.66(16) 8_465 . ?
O6 Eu1 C17 25.2(2) 8_465 8_465 ?
O6 Eu1 O5 51.44(19) 8_465 8_465 ?
O5 Eu1 Eu1 100.69(13) 8_465 5_666 ?
O5 Eu1 O2W 127.44(18) 8_465 . ?
O5 Eu1 O3 117.51(17) 8_465 . ?
O5 Eu1 C17 26.3(2) 8_465 8_465 ?
Cu3 Br1 Cu3 70.48(5) . 2_656 ?
Br1 Cu3 Br1 103.96(6) . 2_656 ?
Br1 Cu3 Cu3 53.91(4) 2_656 2_656 ?
Br1 Cu3 Cu3 55.61(4) . 2_656 ?
N2 Cu3 Br1 104.9(2) . . ?
N2 Cu3 Br1 107.72(19) . 2_656 ?
N2 Cu3 Cu3 96.73(19) . 2_656 ?
N3 Cu3 Br1 116.4(2) . . ?
N3 Cu3 Br1 107.4(2) . 2_656 ?
N3 Cu3 Cu3 147.3(2) . 2_656 ?
N3 Cu3 N2 115.5(3) . . ?
C1 O1 Eu1 131.4(5) . . ?
C1 O2 Eu1 175.7(5) . 5_656 ?
Eu1 O3 Eu1 116.55(19) 5_666 . ?
C9 O3 Eu1 83.1(4) . . ?
C9 O3 Eu1 154.3(5) . 5_666 ?
C2 C3 C4 128.1(8) . . ?
N1 C8 C4 123.9(7) . . ?
C8 C4 C3 121.5(7) . . ?
C5 C4 C3 122.0(8) . . ?
C5 C4 C8 116.5(7) . . ?
C7 N1 C8 117.0(8) . . ?
C3 C2 C1 126.0(7) . . ?
N1 C7 C6 123.4(8) . . ?
C11 C10 C9 122.0(7) . . ?
O3 C9 C10 118.2(7) . . ?
O4 C9 O3 119.8(7) . . ?
O4 C9 C10 121.8(7) . . ?
C10 C11 C12 126.9(8) . . ?
C9 O4 Eu1 103.7(4) . . ?
C7 C6 C5 118.9(8) . . ?
C4 C5 C6 120.3(8) . . ?
C16 N2 Cu3 119.4(6) . . ?
C15 N2 Cu3 124.1(6) . . ?
C15 N2 C16 116.5(8) . . ?
N2 C16 C12 124.8(8) . . ?
C16 C12 C11 121.4(8) . . ?
C16 C12 C13 116.9(8) . . ?
C13 C12 C11 121.6(8) . . ?
C23 N3 Cu3 122.2(6) . . ?
C23 N3 C24 116.2(8) . . ?
C24 N3 Cu3 121.5(6) . . ?
C24 C20 C19 122.0(9) . . ?
C21 C20 C24 118.5(8) . . ?
C21 C20 C19 119.5(8) . . ?
N3 C23 C22 122.8(9) . . ?
N3 C24 C20 124.0(8) . . ?
C20 C21 C22 118.7(9) . . ?
C21 C22 C23 119.8(10) . . ?
C15 C14 C13 118.8(9) . . ?
N2 C15 C14 123.5(9) . . ?
C12 C13 C14 119.4(9) . . ?
C18 C19 C20 126.7(10) . . ?
C19 C18 C17 124.5(10) . . ?
C18 C17 Eu1 175.9(6) . 8_566 ?
O6 C17 Eu1 58.7(4) . 8_566 ?
O6 C17 C18 118.4(9) . . ?
O6 C17 O5 121.1(8) . . ?
O5 C17 Eu1 62.4(4) . 8_566 ?
O5 C17 C18 120.5(9) . . ?
C17 O6 Eu1 96.1(5) . 8_566 ?
C17 O5 Eu1 91.4(5) . 8_566 ?
O1 C1 O2 124.1(7) . . ?
O1 C1 C2 118.2(7) . . ?
O2 C1 C2 117.6(7) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 973528'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'O, C24 H24 Br Cu La N3 O8'
_chemical_formula_sum            'C24 H24 Br Cu La N3 O9'
_chemical_formula_weight         780.82
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.315(4)
_cell_length_b                   9.4268(17)
_cell_length_c                   29.048(5)
_cell_angle_alpha                90
_cell_angle_beta                 110.025(2)
_cell_angle_gamma                90
_cell_volume                     5741.0(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1672
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.79
_cell_measurement_theta_min      2.58
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.654
_exptl_absorpt_correction_T_max  0.482
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   0.482
_exptl_transmission_factor_min   0.420
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            14597
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.397
_diffrn_reflns_theta_min         1.492
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3452
_reflns_number_total             5277
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         1.486
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         5277
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0483
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0457P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1165
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C10-C11
 1.32 with sigma of 0.01
3. Rigid bond restraints
 C11, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9, C10
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C7)
5. Others
 Sof(O3WB)=1-FVAR(1)
 Sof(O3W)=FVAR(1)
6.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C8(H8), C7(H7), C6(H6), C5(H5), C15(H15), C13(H13), C14(H14),
 C23(H23), C16(H16), C22(H22), C24(H24), C21(H21), C19(H19), C18(H18), C11(H11),
  C10(H10)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
O3W O 0.8345(5) 0.2124(12) 0.0897(5) 0.133(6) Uani 0.717(14) 1 d . . P A 1
O3WB O 0.7189(13) 0.196(4) 0.0094(16) 0.23(3) Uani 0.283(14) 1 d . . P A 2
La1 La 0.99063(2) 1.26534(4) 1.01265(2) 0.03502(14) Uani 1 1 d . . . . .
Br1 Br 1.02989(5) 0.88590(12) 0.82291(3) 0.0800(3) Uani 1 1 d . . . . .
Cu1 Cu 0.93526(6) 0.94259(13) 0.74850(4) 0.0775(4) Uani 1 1 d . . . . .
O2W O 1.0982(2) 1.3671(5) 1.06525(17) 0.0544(14) Uani 1 1 d . . . . .
H2WA H 1.1111 1.4680 1.0557 0.082 Uiso 1 1 d GR . . . .
H2WB H 1.1374 1.3073 1.0653 0.082 Uiso 1 1 d GR . . . .
O1 O 0.9061(2) 1.1079(5) 1.02168(18) 0.0529(13) Uani 1 1 d . . . . .
O1W O 1.0423(2) 1.1056(5) 1.09042(16) 0.0486(13) Uani 1 1 d . . . . .
H1WA H 1.0496 1.0087 1.0832 0.073 Uiso 1 1 d GR . . . .
H1WB H 1.0160 1.0978 1.1102 0.073 Uiso 1 1 d GR . . . .
C3 C 0.8497(3) 0.7732(8) 1.0439(3) 0.0461(18) Uani 1 1 d . . . . .
H3 H 0.8760 0.7138 1.0338 0.055 Uiso 1 1 calc R . . . .
C1 C 0.9052(3) 0.9755(8) 1.0219(3) 0.0427(18) Uani 1 1 d . . . . .
C2 C 0.8580(4) 0.9082(8) 1.0411(3) 0.054(2) Uani 1 1 d . . . . .
H2 H 0.8325 0.9682 1.0519 0.065 Uiso 1 1 calc R . . . .
N1 N 0.7115(3) 0.7225(7) 1.0889(3) 0.0631(15) Uani 1 1 d . . . . .
C8 C 0.7567(3) 0.7795(8) 1.0739(3) 0.051(2) Uani 1 1 d . . . . .
H8 H 0.7576 0.8778 1.0715 0.062 Uiso 1 1 calc R . . . .
C7 C 0.7113(4) 0.5841(9) 1.0922(3) 0.0631(15) Uani 1 1 d . . . . .
H7 H 0.6808 0.5424 1.1031 0.076 Uiso 1 1 calc R . . . .
C4 C 0.8019(3) 0.7041(9) 1.0617(3) 0.050(2) Uani 1 1 d . . . . .
C6 C 0.7537(4) 0.4953(9) 1.0806(3) 0.075(3) Uani 1 1 d . . . . .
H6 H 0.7516 0.3973 1.0833 0.090 Uiso 1 1 calc R . . . .
C5 C 0.7988(4) 0.5584(9) 1.0650(3) 0.063(2) Uani 1 1 d . . . . .
H5 H 0.8276 0.5021 1.0564 0.076 Uiso 1 1 calc R . . . .
N2 N 0.8588(3) 0.8274(8) 0.7489(2) 0.0621(19) Uani 1 1 d . . . . .
C15 C 0.8538(4) 0.7737(10) 0.7898(3) 0.076(3) Uani 1 1 d . . . . .
H15 H 0.8880 0.7846 0.8188 0.092 Uiso 1 1 calc R . . . .
C13 C 0.7488(5) 0.6925(15) 0.7498(4) 0.110(4) Uani 1 1 d . . . . .
H13 H 0.7119 0.6479 0.7504 0.132 Uiso 1 1 calc R . . . .
C14 C 0.8006(5) 0.7029(14) 0.7915(3) 0.106(4) Uani 1 1 d . . . . .
H14 H 0.8001 0.6628 0.8206 0.128 Uiso 1 1 calc R . . . .
N3 N 0.9220(3) 1.1568(7) 0.7452(2) 0.0595(19) Uani 1 1 d . . . . .
C23 C 0.8929(4) 1.2258(11) 0.7041(3) 0.079(3) Uani 1 1 d . . . . .
H23 H 0.8748 1.1730 0.6757 0.095 Uiso 1 1 calc R . . . .
C12 C 0.7511(5) 0.7470(11) 0.7077(4) 0.080(3) Uani 1 1 d . U . . .
C16 C 0.8069(5) 0.8129(10) 0.7082(3) 0.074(3) Uani 1 1 d . . . . .
H16 H 0.8086 0.8492 0.6789 0.089 Uiso 1 1 calc R . . . .
C22 C 0.8876(5) 1.3707(13) 0.7008(3) 0.101(4) Uani 1 1 d . . . . .
H22 H 0.8658 1.4141 0.6710 0.121 Uiso 1 1 calc R . . . .
C24 C 0.9474(4) 1.2365(9) 0.7852(3) 0.057(2) Uani 1 1 d . . . . .
H24 H 0.9681 1.1902 0.8146 0.069 Uiso 1 1 calc R . . . .
C21 C 0.9151(4) 1.4503(10) 0.7422(3) 0.077(3) Uani 1 1 d . . . . .
H21 H 0.9135 1.5488 0.7407 0.093 Uiso 1 1 calc R . . . .
C20 C 0.9448(4) 1.3826(9) 0.7859(3) 0.057(2) Uani 1 1 d . . . . .
O2 O 0.9419(2) 0.8977(5) 1.0091(2) 0.0597(15) Uani 1 1 d . . . . .
C19 C 0.9756(4) 1.4621(8) 0.8317(3) 0.057(2) Uani 1 1 d . . . . .
H19 H 0.9804 1.5592 0.8286 0.068 Uiso 1 1 calc R . . . .
C18 C 0.9968(4) 1.4106(8) 0.8763(3) 0.054(2) Uani 1 1 d . . . . .
H18 H 0.9975 1.3128 0.8806 0.065 Uiso 1 1 calc R . . . .
C17 C 1.0199(3) 1.5038(8) 0.9203(3) 0.0417(18) Uani 1 1 d . . . . .
O3 O 1.0199(2) 1.4534(5) 0.96123(15) 0.0423(12) Uani 1 1 d . . . . .
O4 O 1.0347(3) 1.6304(5) 0.91607(17) 0.0564(14) Uani 1 1 d . . . . .
C9 C 0.6186(5) 0.7698(12) 0.5813(4) 0.094(5) Uani 1 1 d . U . . .
O5 O 0.6162(2) 0.8541(6) 0.5474(2) 0.0690(18) Uani 1 1 d . . . . .
O6 O 0.5766(3) 0.6768(6) 0.5760(2) 0.0721(19) Uani 1 1 d . . . . .
C11 C 0.6908(6) 0.7258(13) 0.6632(4) 0.114(5) Uani 1 1 d D U . . .
H11 H 0.6600 0.6614 0.6649 0.137 Uiso 1 1 calc R . . . .
C10 C 0.6824(6) 0.7938(12) 0.6247(4) 0.105(4) Uani 1 1 d D U . . .
H10 H 0.7130 0.8567 0.6219 0.126 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 O2W 2.551(5) . ?
La1 O1 2.484(5) . ?
La1 O1W 2.630(4) . ?
La1 O2 2.382(5) 5_777 ?
La1 C17 2.982(7) 5_787 ?
La1 O3 2.544(4) . ?
La1 O3 2.790(5) 5_787 ?
La1 O4 2.524(5) 5_787 ?
La1 C9 2.973(9) 4_656 ?
La1 O5 2.565(5) 4_656 ?
La1 O6 2.632(5) 4_656 ?
Br1 Cu1 2.5081(15) . ?
Br1 Cu1 2.5096(15) 2_756 ?
Cu1 Br1 2.5095(15) 2_756 ?
Cu1 Cu1 2.861(2) 2_756 ?
Cu1 N2 2.026(7) . ?
Cu1 N3 2.038(7) . ?
O1 C1 1.249(8) . ?
C3 C2 1.292(9) . ?
C3 C4 1.485(10) . ?
C1 C2 1.493(10) . ?
C1 O2 1.248(8) . ?
N1 C8 1.341(9) . ?
N1 C7 1.309(10) . ?
C8 C4 1.376(10) . ?
C7 C6 1.388(11) . ?
C4 C5 1.380(10) . ?
C6 C5 1.374(10) . ?
N2 C15 1.331(11) . ?
N2 C16 1.349(10) . ?
C15 C14 1.376(13) . ?
C13 C14 1.363(12) . ?
C13 C12 1.341(14) . ?
N3 C23 1.318(10) . ?
N3 C24 1.336(9) . ?
C23 C22 1.372(13) . ?
C12 C16 1.387(13) . ?
C12 C11 1.526(13) . ?
C22 C21 1.372(12) . ?
C24 C20 1.379(10) . ?
C21 C20 1.372(10) . ?
C20 C19 1.475(10) . ?
O2 La1 2.382(5) 5_777 ?
C19 C18 1.311(9) . ?
C18 C17 1.491(9) . ?
C17 La1 2.982(7) 5_787 ?
C17 O3 1.279(7) . ?
C17 O4 1.256(8) . ?
O3 La1 2.790(5) 5_787 ?
O4 La1 2.524(5) 5_787 ?
C9 La1 2.973(9) 4_646 ?
C9 O5 1.253(13) . ?
C9 O6 1.254(13) . ?
C9 C10 1.560(14) . ?
O5 La1 2.565(5) 4_646 ?
O6 La1 2.632(5) 4_646 ?
C11 C10 1.247(8) . ?

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
O2W La1 O1W 69.84(15) . . ?
O2W La1 C17 66.59(18) . 5_787 ?
O2W La1 O3 68.25(15) . 5_787 ?
O2W La1 C9 148.5(2) . 4_656 ?
O2W La1 O5 138.57(17) . 4_656 ?
O2W La1 O6 144.02(18) . 4_656 ?
O1 La1 O2W 138.99(16) . . ?
O1 La1 O1W 72.08(15) . . ?
O1 La1 C17 97.74(18) . 5_787 ?
O1 La1 O3 113.64(14) . 5_787 ?
O1 La1 O3 146.68(15) . . ?
O1 La1 O4 75.80(16) . 5_787 ?
O1 La1 C9 72.0(2) . 4_656 ?
O1 La1 O5 72.76(17) . 4_656 ?
O1 La1 O6 73.44(17) . 4_656 ?
O1W La1 C17 88.07(17) . 5_787 ?
O1W La1 O3 111.32(14) . 5_787 ?
O1W La1 C9 141.0(2) . 4_656 ?
O1W La1 O6 126.43(17) . 4_656 ?
O2 La1 O2W 81.42(17) 5_777 . ?
O2 La1 O1 102.37(17) 5_777 . ?
O2 La1 O1W 74.18(17) 5_777 . ?
O2 La1 C17 147.31(19) 5_777 5_787 ?
O2 La1 O3 143.61(16) 5_777 5_787 ?
O2 La1 O3 88.93(16) 5_777 . ?
O2 La1 O4 143.84(18) 5_777 5_787 ?
O2 La1 C9 99.2(3) 5_777 4_656 ?
O2 La1 O5 123.7(2) 5_777 4_656 ?
O2 La1 O6 74.7(2) 5_777 4_656 ?
O3 La1 O2W 73.21(15) . . ?
O3 La1 O1W 141.12(14) . . ?
O3 La1 C17 25.32(15) 5_787 5_787 ?
O3 La1 C17 88.18(18) . 5_787 ?
O3 La1 O3 63.90(16) . 5_787 ?
O3 La1 C9 75.27(19) . 4_656 ?
O3 La1 C9 96.7(3) 5_787 4_656 ?
O3 La1 O5 74.90(16) . 4_656 ?
O3 La1 O6 79.72(16) . 4_656 ?
O4 La1 O2W 77.95(17) 5_787 . ?
O4 La1 O1W 70.95(16) 5_787 . ?
O4 La1 C17 24.60(16) 5_787 5_787 ?
O4 La1 O3 112.64(15) 5_787 . ?
O4 La1 O3 48.96(14) 5_787 5_787 ?
O4 La1 C9 113.8(3) 5_787 4_656 ?
O4 La1 O5 90.8(2) 5_787 4_656 ?
O4 La1 O6 135.5(2) 5_787 4_656 ?
C9 La1 C17 111.5(3) 4_656 5_787 ?
O5 La1 O1W 143.38(17) 4_656 . ?
O5 La1 C17 86.7(2) 4_656 5_787 ?
O5 La1 O3 74.31(17) 4_656 5_787 ?
O5 La1 C9 24.8(3) 4_656 4_656 ?
O5 La1 O6 49.7(2) 4_656 4_656 ?
O6 La1 C17 136.4(2) 4_656 5_787 ?
O6 La1 O3 119.63(17) 4_656 5_787 ?
O6 La1 C9 24.9(3) 4_656 4_656 ?
Cu1 Br1 Cu1 69.52(5) . 2_756 ?
Br1 Cu1 Br1 105.02(6) . 2_756 ?
Br1 Cu1 Cu1 55.27(4) . 2_756 ?
Br1 Cu1 Cu1 55.22(4) 2_756 2_756 ?
N2 Cu1 Br1 113.0(2) . 2_756 ?
N2 Cu1 Br1 110.1(2) . . ?
N2 Cu1 Cu1 147.5(2) . 2_756 ?
N2 Cu1 N3 115.0(3) . . ?
N3 Cu1 Br1 108.52(19) . . ?
N3 Cu1 Br1 104.6(2) . 2_756 ?
N3 Cu1 Cu1 97.47(19) . 2_756 ?
C1 O1 La1 127.7(5) . . ?
C2 C3 C4 126.1(7) . . ?
O1 C1 C2 116.2(7) . . ?
O2 C1 O1 124.9(7) . . ?
O2 C1 C2 118.8(7) . . ?
C3 C2 C1 125.2(7) . . ?
C7 N1 C8 116.4(7) . . ?
N1 C8 C4 125.2(8) . . ?
N1 C7 C6 124.3(8) . . ?
C8 C4 C3 122.6(7) . . ?
C8 C4 C5 116.0(7) . . ?
C5 C4 C3 121.3(8) . . ?
C5 C6 C7 117.2(8) . . ?
C6 C5 C4 120.8(8) . . ?
C15 N2 Cu1 122.5(6) . . ?
C15 N2 C16 115.7(8) . . ?
C16 N2 Cu1 121.4(7) . . ?
N2 C15 C14 123.6(8) . . ?
C12 C13 C14 119.8(10) . . ?
C13 C14 C15 118.8(10) . . ?
C23 N3 Cu1 123.4(6) . . ?
C23 N3 C24 116.1(8) . . ?
C24 N3 Cu1 120.3(6) . . ?
N3 C23 C22 124.0(8) . . ?
C13 C12 C16 118.4(9) . . ?
C13 C12 C11 115.1(11) . . ?
C16 C12 C11 126.5(10) . . ?
N2 C16 C12 123.6(9) . . ?
C23 C22 C21 118.7(9) . . ?
N3 C24 C20 124.5(8) . . ?
C22 C21 C20 119.1(9) . . ?
C24 C20 C19 120.8(7) . . ?
C21 C20 C24 117.4(8) . . ?
C21 C20 C19 121.7(8) . . ?
C1 O2 La1 175.7(5) . 5_777 ?
C18 C19 C20 127.0(8) . . ?
C19 C18 C17 122.1(7) . . ?
C18 C17 La1 155.4(5) . 5_787 ?
O3 C17 La1 68.9(4) . 5_787 ?
O3 C17 C18 118.0(6) . . ?
O4 C17 La1 56.8(3) . 5_787 ?
O4 C17 C18 120.0(6) . . ?
O4 C17 O3 121.8(6) . . ?
La1 O3 La1 116.10(16) . 5_787 ?
C17 O3 La1 152.3(4) . . ?
C17 O3 La1 85.8(4) . 5_787 ?
C17 O4 La1 98.6(4) . 5_787 ?
O5 C9 La1 59.1(4) . 4_646 ?
O5 C9 O6 121.1(8) . . ?
O5 C9 C10 109.0(11) . . ?
O6 C9 La1 62.1(4) . 4_646 ?
O6 C9 C10 129.7(11) . . ?
C10 C9 La1 167.9(10) . 4_646 ?
C9 O5 La1 96.2(6) . 4_646 ?
C9 O6 La1 92.9(6) . 4_646 ?
C10 C11 C12 120.8(13) . . ?
C11 C10 C9 117.8(13) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_12
_database_code_depnum_ccdc_archive 'CCDC 973529'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C24 H23 Br Cu N3 Nd O8), O'
_chemical_formula_sum            'C48 H46 Br2 Cu2 N6 Nd2 O17'
_chemical_formula_weight         1554.29
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.175(4)
_cell_length_b                   9.3814(17)
_cell_length_c                   28.994(5)
_cell_angle_alpha                90
_cell_angle_beta                 110.156(2)
_cell_angle_gamma                90
_cell_volume                     5662.2(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3795
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.976
_cell_measurement_theta_min      1.957
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.027
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0914 before and 0.0438 after correction.
The Ratio of minimum to maximum transmission is 0.7788.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.447
_exptl_transmission_factor_min   0.396
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            16730
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.976
_diffrn_reflns_theta_min         1.957
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4898
_reflns_number_total             6832
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker, 2000-2003)'
_refine_diff_density_max         1.356
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         6553
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0409
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0491P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1025
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O3W(0.5)
3.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C7(H7), C8(H8), C24(H24), C21(H21), C11(H11), C16(H16),
 C15(H15), C5(H5), C14(H14), C23(H23), C22(H22), C13(H13), C10(H10), C18(H18),
 C19(H19), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Nd1 Nd 0.49113(2) 0.73277(2) 1.01259(2) 0.02849(9) Uani 1 1 d . . . . .
Cu3 Cu 0.06612(4) 0.55557(9) 0.75297(3) 0.0662(2) Uani 1 1 d . . . . .
O2 O 0.40991(16) 0.8925(3) 1.02229(13) 0.0434(8) Uani 1 1 d . . . . .
O1W O 0.59755(16) 0.6354(4) 1.06196(13) 0.0470(9) Uani 1 1 d . . . . .
H1WA H 0.6042 0.5564 1.0491 0.071 Uiso 1 1 d GR . . . .
H1WB H 0.5991 0.6188 1.0917 0.071 Uiso 1 1 d GR . . . .
C1 C 0.4077(2) 1.0263(5) 1.02283(16) 0.0338(10) Uani 1 1 d . . . . .
O2W O 0.54419(16) 0.8914(4) 1.08855(12) 0.0433(8) Uani 1 1 d . . . . .
H2WA H 0.5222 0.8893 1.1093 0.065 Uiso 1 1 d GR . . . .
H2WB H 0.5460 0.9822 1.0798 0.065 Uiso 1 1 d GR . . . .
C3 C 0.3506(2) 1.2263(5) 1.04387(18) 0.0383(11) Uani 1 1 d . . . . .
H3 H 0.3775 1.2857 1.0340 0.046 Uiso 1 1 calc R . . . .
C4 C 0.3023(2) 1.2972(5) 1.06091(18) 0.0396(11) Uani 1 1 d . . . . .
C2 C 0.3592(2) 1.0918(5) 1.0412(2) 0.0444(12) Uani 1 1 d . . . . .
H2 H 0.3332 1.0308 1.0515 0.053 Uiso 1 1 calc R . . . .
N1 N 0.2124(2) 1.2779(5) 1.08895(18) 0.0517(12) Uani 1 1 d . . . . .
C7 C 0.2112(3) 1.4195(7) 1.0913(2) 0.0610(17) Uani 1 1 d . . . . .
H7 H 0.1798 1.4625 1.1010 0.073 Uiso 1 1 calc R . . . .
C8 C 0.2574(2) 1.2203(6) 1.07357(19) 0.0430(12) Uani 1 1 d . . . . .
H8 H 0.2584 1.1216 1.0713 0.052 Uiso 1 1 calc R . . . .
C24 C 0.0532(3) 0.2617(6) 0.7152(2) 0.0518(14) Uani 1 1 d . . . . .
H24 H 0.0328 0.3099 0.6859 0.062 Uiso 1 1 calc R . . . .
C21 C 0.0849(3) 0.0443(8) 0.7581(2) 0.0681(18) Uani 1 1 d . . . . .
H21 H 0.0862 -0.0548 0.7594 0.082 Uiso 1 1 calc R . . . .
C20 C 0.0549(3) 0.1142(6) 0.71375(19) 0.0479(13) Uani 1 1 d . . . . .
N2 N 0.1432(2) 0.6695(5) 0.75190(16) 0.0534(12) Uani 1 1 d . . . . .
C11 C 0.3092(4) 0.7682(7) 0.8387(3) 0.0703(19) Uani 1 1 d . . . . .
H11 H 0.3411 0.8306 0.8374 0.084 Uiso 1 1 calc R . . . .
C12 C 0.2510(3) 0.7540(7) 0.7933(2) 0.0654(19) Uani 1 1 d . . . . .
C16 C 0.1950(3) 0.6869(7) 0.7920(2) 0.0593(16) Uani 1 1 d . . . . .
H16 H 0.1933 0.6510 0.8214 0.071 Uiso 1 1 calc R . . . .
C15 C 0.1470(3) 0.7241(7) 0.7107(2) 0.0639(18) Uani 1 1 d . . . . .
H15 H 0.1122 0.7127 0.6817 0.077 Uiso 1 1 calc R . . . .
C5 C 0.3000(3) 1.4436(6) 1.0639(2) 0.0548(15) Uani 1 1 d . . . . .
H5 H 0.3287 1.5009 1.0553 0.066 Uiso 1 1 calc R . . . .
C14 C 0.2007(4) 0.7973(10) 0.7088(3) 0.095(3) Uani 1 1 d . . . . .
H14 H 0.2007 0.8356 0.6793 0.114 Uiso 1 1 calc R . . . .
N3 N 0.0793(2) 0.3398(5) 0.75639(16) 0.0539(12) Uani 1 1 d . . . . .
C23 C 0.1079(3) 0.2686(8) 0.7976(2) 0.0662(19) Uani 1 1 d . . . . .
H23 H 0.1259 0.3201 0.8266 0.079 Uiso 1 1 calc R . . . .
C22 C 0.1124(4) 0.1235(9) 0.7998(2) 0.085(2) Uani 1 1 d . . . . .
H22 H 0.1341 0.0785 0.8295 0.102 Uiso 1 1 calc R . . . .
C13 C 0.2522(4) 0.8125(11) 0.7495(3) 0.095(3) Uani 1 1 d . . . . .
H13 H 0.2883 0.8613 0.7486 0.113 Uiso 1 1 calc R . . . .
Br2 Br 0.02873(3) 0.61279(8) 0.82328(2) 0.0690(2) Uani 1 1 d . . . . .
C10 C 0.3180(4) 0.7060(7) 0.8765(3) 0.074(2) Uani 1 1 d . . . . .
H10 H 0.2864 0.6434 0.8786 0.088 Uiso 1 1 calc R . . . .
C18 C 0.0044(3) 0.0882(5) 0.62327(18) 0.0466(13) Uani 1 1 d . . . . .
H18 H 0.0038 0.1867 0.6193 0.056 Uiso 1 1 calc R . . . .
C19 C 0.0251(3) 0.0359(6) 0.66795(18) 0.0468(13) Uani 1 1 d . . . . .
H19 H 0.0203 -0.0618 0.6708 0.056 Uiso 1 1 calc R . . . .
C9 C 0.3797(3) 0.7250(6) 0.9224(2) 0.0554(16) Uani 1 1 d . . . . .
O4 O 0.38440(17) 0.6423(4) 0.95675(15) 0.0541(10) Uani 1 1 d . . . . .
O3 O 0.4219(2) 0.8169(4) 0.92498(13) 0.0569(10) Uani 1 1 d . . . . .
O5 O -0.01846(15) 0.0487(3) 0.53862(11) 0.0381(8) Uani 1 1 d . . . . .
O6 O -0.03227(18) -0.1303(4) 0.58294(12) 0.0476(9) Uani 1 1 d . . . . .
C17 C -0.0179(2) -0.0015(5) 0.57954(16) 0.0349(11) Uani 1 1 d . . . . .
O1 O 0.44437(17) 1.1058(4) 1.01030(14) 0.0496(9) Uani 1 1 d . . . . .
O3W O 0.3369(4) 0.7863(9) 0.0884(4) 0.078(3) Uani 0.5 1 d . . P . .
C6 C 0.2535(3) 1.5029(6) 1.0800(2) 0.0652(17) Uani 1 1 d . . . . .
H6 H 0.2515 1.6013 1.0831 0.078 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 O2 2.433(3) . ?
Nd1 O1W 2.475(3) . ?
Nd1 O2W 2.581(3) . ?
Nd1 O4 2.511(4) . ?
Nd1 O3 2.597(4) . ?
Nd1 O5 2.485(3) 4_556 ?
Nd1 O5 2.774(3) 8_556 ?
Nd1 O6 2.467(3) 8_556 ?
Nd1 C17 2.963(4) 8_556 ?
Nd1 O1 2.331(3) 5_677 ?
Cu3 Cu3 2.8775(17) 2_556 ?
Cu3 N2 2.024(5) . ?
Cu3 N3 2.043(5) . ?
Cu3 Br2 2.5290(11) 2_556 ?
Cu3 Br2 2.5092(10) . ?
O2 C1 1.256(5) . ?
C1 C2 1.489(6) . ?
C1 O1 1.246(5) . ?
C3 C4 1.482(7) . ?
C3 C2 1.283(6) . ?
C4 C8 1.377(7) . ?
C4 C5 1.378(7) . ?
N1 C7 1.330(7) . ?
N1 C8 1.338(6) . ?
C7 C6 1.343(8) . ?
C24 C20 1.385(7) . ?
C24 N3 1.350(7) . ?
C21 C20 1.392(7) . ?
C21 C22 1.371(9) . ?
C20 C19 1.461(7) . ?
N2 C16 1.332(7) . ?
N2 C15 1.330(7) . ?
C11 C12 1.498(9) . ?
C11 C10 1.197(9) . ?
C12 C16 1.381(9) . ?
C12 C13 1.391(11) . ?
C15 C14 1.391(10) . ?
C5 C6 1.388(7) . ?
C14 C13 1.339(9) . ?
N3 C23 1.325(7) . ?
C23 C22 1.365(9) . ?
Br2 Cu3 2.5288(11) 2_556 ?
C10 C9 1.557(9) . ?
C18 C19 1.312(7) . ?
C18 C17 1.459(6) . ?
C9 O4 1.238(7) . ?
C9 O3 1.255(8) . ?
O5 Nd1 2.774(3) 8_455 ?
O5 Nd1 2.485(3) 4_546 ?
O5 C17 1.272(5) . ?
O6 Nd1 2.467(3) 8_455 ?
O6 C17 1.262(5) . ?
C17 Nd1 2.963(4) 8_455 ?
O1 Nd1 2.331(3) 5_677 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Nd1 O1W 139.19(12) . . ?
O2 Nd1 O2W 71.58(11) . . ?
O2 Nd1 O4 73.26(12) . . ?
O2 Nd1 O3 73.40(12) . . ?
O2 Nd1 O5 147.14(11) . 4_556 ?
O2 Nd1 O5 115.19(10) . 8_556 ?
O2 Nd1 O6 76.67(11) . 8_556 ?
O2 Nd1 C17 98.95(12) . 8_556 ?
O1W Nd1 O2W 69.87(11) . . ?
O1W Nd1 O4 138.36(12) . . ?
O1W Nd1 O3 143.36(12) . . ?
O1W Nd1 O5 73.07(11) . 4_556 ?
O1W Nd1 O5 68.81(11) . 8_556 ?
O1W Nd1 C17 67.47(13) . 8_556 ?
O2W Nd1 O3 126.97(11) . . ?
O2W Nd1 O5 111.82(10) . 8_556 ?
O2W Nd1 C17 88.67(12) . 8_556 ?
O4 Nd1 O2W 142.78(11) . . ?
O4 Nd1 O3 50.49(14) . . ?
O4 Nd1 O5 73.14(11) . 8_556 ?
O4 Nd1 C17 85.04(14) . 8_556 ?
O3 Nd1 O5 118.71(12) . 8_556 ?
O3 Nd1 C17 135.45(14) . 8_556 ?
O5 Nd1 O2W 141.00(11) 4_556 . ?
O5 Nd1 O4 75.49(11) 4_556 . ?
O5 Nd1 O3 79.07(11) 4_556 . ?
O5 Nd1 O5 63.79(11) 4_556 8_556 ?
O5 Nd1 C17 25.35(10) 8_556 8_556 ?
O5 Nd1 C17 88.16(12) 4_556 8_556 ?
O6 Nd1 O1W 78.94(12) 8_556 . ?
O6 Nd1 O2W 71.52(12) 8_556 . ?
O6 Nd1 O4 88.92(14) 8_556 . ?
O6 Nd1 O3 134.86(14) 8_556 . ?
O6 Nd1 O5 112.78(10) 8_556 4_556 ?
O6 Nd1 O5 49.18(10) 8_556 8_556 ?
O6 Nd1 C17 24.77(11) 8_556 8_556 ?
O1 Nd1 O2 100.61(12) 5_677 . ?
O1 Nd1 O1W 81.27(12) 5_677 . ?
O1 Nd1 O2W 74.01(12) 5_677 . ?
O1 Nd1 O4 124.80(14) 5_677 . ?
O1 Nd1 O3 74.82(14) 5_677 . ?
O1 Nd1 O5 88.94(11) 5_677 4_556 ?
O1 Nd1 O5 143.88(11) 5_677 8_556 ?
O1 Nd1 O6 144.42(13) 5_677 8_556 ?
O1 Nd1 C17 148.05(13) 5_677 8_556 ?
N2 Cu3 Cu3 147.88(14) . 2_556 ?
N2 Cu3 N3 114.6(2) . . ?
N2 Cu3 Br2 114.60(13) . . ?
N2 Cu3 Br2 109.06(14) . 2_556 ?
N3 Cu3 Cu3 97.39(13) . 2_556 ?
N3 Cu3 Br2 108.34(13) . 2_556 ?
N3 Cu3 Br2 104.74(13) . . ?
Br2 Cu3 Cu3 55.49(3) . 2_556 ?
Br2 Cu3 Cu3 54.85(3) 2_556 2_556 ?
Br2 Cu3 Br2 104.88(4) . 2_556 ?
C1 O2 Nd1 130.5(3) . . ?
O2 C1 C2 116.9(4) . . ?
O1 C1 O2 124.3(4) . . ?
O1 C1 C2 118.8(4) . . ?
C2 C3 C4 126.9(5) . . ?
C8 C4 C3 121.7(5) . . ?
C8 C4 C5 117.4(5) . . ?
C5 C4 C3 120.9(5) . . ?
C3 C2 C1 124.6(5) . . ?
C7 N1 C8 116.8(5) . . ?
N1 C7 C6 122.7(5) . . ?
N1 C8 C4 124.5(5) . . ?
N3 C24 C20 124.2(5) . . ?
C22 C21 C20 119.0(7) . . ?
C24 C20 C21 116.9(5) . . ?
C24 C20 C19 121.4(5) . . ?
C21 C20 C19 121.7(5) . . ?
C16 N2 Cu3 122.0(4) . . ?
C15 N2 Cu3 122.2(4) . . ?
C15 N2 C16 115.7(5) . . ?
C10 C11 C12 125.5(8) . . ?
C16 C12 C11 124.0(7) . . ?
C16 C12 C13 117.0(6) . . ?
C13 C12 C11 119.0(7) . . ?
N2 C16 C12 125.3(6) . . ?
N2 C15 C14 123.0(6) . . ?
C4 C5 C6 117.9(5) . . ?
C13 C14 C15 120.0(7) . . ?
C24 N3 Cu3 119.0(4) . . ?
C23 N3 Cu3 124.0(4) . . ?
C23 N3 C24 116.8(5) . . ?
N3 C23 C22 123.3(6) . . ?
C23 C22 C21 119.8(6) . . ?
C14 C13 C12 118.9(7) . . ?
Cu3 Br2 Cu3 69.66(4) . 2_556 ?
C11 C10 C9 123.0(8) . . ?
C19 C18 C17 122.7(5) . . ?
C18 C19 C20 127.2(5) . . ?
O4 C9 C10 114.9(6) . . ?
O4 C9 O3 122.0(5) . . ?
O3 C9 C10 123.2(6) . . ?
C9 O4 Nd1 96.0(4) . . ?
C9 O3 Nd1 91.5(3) . . ?
Nd1 O5 Nd1 116.21(11) 4_546 8_455 ?
C17 O5 Nd1 85.7(3) . 8_455 ?
C17 O5 Nd1 152.6(3) . 4_546 ?
C17 O6 Nd1 100.2(3) . 8_455 ?
C18 C17 Nd1 155.9(4) . 8_455 ?
O5 C17 Nd1 69.0(2) . 8_455 ?
O5 C17 C18 119.2(4) . . ?
O6 C17 Nd1 55.0(2) . 8_455 ?
O6 C17 C18 120.2(4) . . ?
O6 C17 O5 120.4(4) . . ?
C1 O1 Nd1 176.3(3) . 5_677 ?
C7 C6 C5 120.7(6) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_11
_database_code_depnum_ccdc_archive 'CCDC 973530'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '2(C24 H23 Br Cu N3 O8 Sm), O'
_chemical_formula_sum            'C48 H46 Br2 Cu2 N6 O17 Sm2'
_chemical_formula_weight         1566.51
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.121(3)
_cell_length_b                   9.3741(9)
_cell_length_c                   28.944(3)
_cell_angle_alpha                90
_cell_angle_beta                 110.003(2)
_cell_angle_gamma                90
_cell_volume                     5639.8(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5209
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.53
_cell_measurement_theta_min      2.38
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.285
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1417 before and 0.0406 after correction.
The Ratio of minimum to maximum transmission is 0.5586.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   0.424
_exptl_transmission_factor_min   0.372
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            14129
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.395
_diffrn_reflns_theta_min         2.383
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4416
_reflns_number_total             5209
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker, 2000-2003)'
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0328
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0382P)²+9.2119P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0789
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O3W(0.5)
3.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C14(H14), C13(H13), C15(H15), C11(H11), C10(H10), C3(H3), C2(H2),
 C8(H8), C5(H5), C7(H7), C6(H6), C23(H23), C24(H24), C22(H22), C21(H21),
 C19(H19), C18(H18)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Sm1 Sm -0.00878(2) 0.73336(2) 0.01245(2) 0.02700(8) Uani 1 1 d . . . . .
Br1 Br 0.02670(3) -0.11035(7) 0.32307(2) 0.06201(18) Uani 1 1 d . . . . .
Cu3 Cu 0.06703(4) -0.05268(8) 0.25422(3) 0.0611(2) Uani 1 1 d . . . . .
O2W O 0.09648(15) 0.6361(3) 0.06015(12) 0.0436(8) Uani 1 1 d . . . . .
H2WA H 0.0985 0.5473 0.0527 0.065 Uiso 1 1 d GR . . . .
H2WB H 0.1027 0.6420 0.0913 0.065 Uiso 1 1 d GR . . . .
O3 O -0.01779(15) 0.4478(3) 0.03847(10) 0.0375(7) Uani 1 1 d . . . . .
O1 O 0.05369(16) 0.8942(3) -0.01118(12) 0.0451(8) Uani 1 1 d . . . . .
N2 N 0.0796(2) 0.1634(5) 0.25709(15) 0.0490(11) Uani 1 1 d . . . . .
C16 C 0.0541(3) 0.2411(5) 0.21606(18) 0.0450(12) Uani 1 1 d . . . . .
H16 H 0.0338 0.1925 0.1868 0.054 Uiso 1 1 calc R . . . .
C12 C 0.0557(3) 0.3873(6) 0.21428(17) 0.0478(13) Uani 1 1 d . . . . .
C14 C 0.1124(3) 0.3797(8) 0.3008(2) 0.078(2) Uani 1 1 d . . . . .
H14 H 0.1334 0.4248 0.3306 0.094 Uiso 1 1 calc R . . . .
C13 C 0.0853(3) 0.4595(7) 0.2584(2) 0.0689(18) Uani 1 1 d . . . . .
H13 H 0.0868 0.5587 0.2593 0.083 Uiso 1 1 calc R . . . .
C15 C 0.1082(3) 0.2354(7) 0.2985(2) 0.0659(17) Uani 1 1 d . . . . .
H15 H 0.1263 0.1838 0.3274 0.079 Uiso 1 1 calc R . . . .
C11 C 0.0263(3) 0.4656(5) 0.16763(18) 0.0469(12) Uani 1 1 d . . . . .
H11 H 0.0220 0.5638 0.1700 0.056 Uiso 1 1 calc R . . . .
C10 C 0.0056(3) 0.4112(5) 0.12345(17) 0.0430(12) Uani 1 1 d . . . . .
H10 H 0.0049 0.3126 0.1199 0.052 Uiso 1 1 calc R . . . .
O1W O 0.04533(15) 0.8903(3) 0.08783(11) 0.0393(7) Uani 1 1 d . . . . .
H1WA H 0.0228 0.8903 0.1065 0.059 Uiso 1 1 d GR . . . .
H1WB H 0.0484 0.9751 0.0784 0.059 Uiso 1 1 d GR . . . .
C9 C -0.0165(2) 0.5004(5) 0.07925(15) 0.0330(10) Uani 1 1 d . . . . .
C1 C 0.0907(2) 0.9736(4) -0.02373(15) 0.0307(9) Uani 1 1 d . . . . .
C3 C 0.1492(2) 0.7724(5) -0.04367(17) 0.0368(10) Uani 1 1 d . . . . .
H3 H 0.1224 0.7132 -0.0335 0.044 Uiso 1 1 calc R . . . .
C2 C 0.1404(2) 0.9089(5) -0.04153(18) 0.0417(11) Uani 1 1 d . . . . .
H2 H 0.1666 0.9699 -0.0517 0.050 Uiso 1 1 calc R . . . .
C8 C 0.2430(2) 0.7797(5) -0.07334(18) 0.0428(12) Uani 1 1 d . . . . .
H8 H 0.2421 0.8787 -0.0715 0.051 Uiso 1 1 calc R . . . .
C5 C 0.2001(3) 0.5563(6) -0.0633(2) 0.0528(14) Uani 1 1 d . . . . .
H5 H 0.1712 0.4998 -0.0545 0.063 Uiso 1 1 calc R . . . .
C4 C 0.1976(2) 0.7023(5) -0.06068(17) 0.0351(10) Uani 1 1 d . . . . .
N1 N 0.2881(2) 0.7194(5) -0.08811(17) 0.0499(11) Uani 1 1 d . . . . .
C7 C 0.2893(3) 0.5790(6) -0.0904(2) 0.0557(15) Uani 1 1 d . . . . .
H7 H 0.3208 0.5360 -0.1002 0.067 Uiso 1 1 calc R . . . .
C6 C 0.2465(3) 0.4945(6) -0.0791(2) 0.0649(16) Uani 1 1 d . . . . .
H6 H 0.2483 0.3959 -0.0820 0.078 Uiso 1 1 calc R . . . .
O3W O 0.6618(4) 0.2832(8) 0.4119(3) 0.068(2) Uani 0.5 1 d . . P . .
O2 O 0.08852(15) 1.1074(3) -0.02289(11) 0.0399(8) Uani 1 1 d . . . . .
N3 N 0.1443(2) -0.1681(5) 0.25268(15) 0.0503(11) Uani 1 1 d . . . . .
C20 C 0.2522(3) -0.2534(6) 0.2941(2) 0.0573(15) Uani 1 1 d . . . . .
C23 C 0.1485(3) -0.2210(7) 0.2111(2) 0.0607(16) Uani 1 1 d . . . . .
H23 H 0.1140 -0.2076 0.1821 0.073 Uiso 1 1 calc R . . . .
C24 C 0.1963(3) -0.1852(6) 0.29344(19) 0.0533(14) Uani 1 1 d . . . . .
H24 H 0.1947 -0.1490 0.3229 0.064 Uiso 1 1 calc R . . . .
C22 C 0.2012(3) -0.2940(9) 0.2092(2) 0.089(2) Uani 1 1 d . . . . .
H22 H 0.2012 -0.3327 0.1796 0.107 Uiso 1 1 calc R . . . .
C21 C 0.2535(3) -0.3101(9) 0.2504(2) 0.080(2) Uani 1 1 d . . . . .
H21 H 0.2896 -0.3585 0.2492 0.096 Uiso 1 1 calc R . . . .
C19 C 0.3095(3) -0.2681(6) 0.3394(2) 0.0579(15) Uani 1 1 d . . . . .
H19 H 0.3413 -0.3312 0.3381 0.069 Uiso 1 1 calc R . . . .
C18 C 0.3192(3) -0.2027(6) 0.3798(2) 0.0597(15) Uani 1 1 d . . . . .
H18 H 0.2877 -0.1396 0.3817 0.072 Uiso 1 1 calc R . . . .
C17 C 0.3787(2) -0.2208(5) 0.4249(2) 0.0452(13) Uani 1 1 d . . . . .
O6 O 0.38460(15) -0.1403(3) 0.46000(13) 0.0461(8) Uani 1 1 d . . . . .
O5 O 0.42092(18) -0.3149(4) 0.42591(12) 0.0503(9) Uani 1 1 d . . . . .
O4 O -0.03021(17) 0.6299(3) 0.08197(11) 0.0442(8) 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
Sm1 O2W 2.442(3) . ?
Sm1 O3 2.807(3) . ?
Sm1 O3 2.448(3) 5_565 ?
Sm1 O1 2.302(3) . ?
Sm1 O1W 2.563(3) . ?
Sm1 O2 2.407(3) 5_575 ?
Sm1 C17 2.884(5) 8_455 ?
Sm1 O6 2.486(3) 8_455 ?
Sm1 O5 2.571(3) 8_455 ?
Sm1 O4 2.422(3) . ?
Br1 Cu3 2.5055(9) . ?
Br1 Cu3 2.5343(10) 2 ?
Cu3 Br1 2.5342(10) 2 ?
Cu3 Cu3 2.8914(15) 2 ?
Cu3 N2 2.042(5) . ?
Cu3 N3 2.035(4) . ?
O3 Sm1 2.448(3) 5_565 ?
O3 C9 1.270(5) . ?
O1 C1 1.248(5) . ?
N2 C16 1.342(6) . ?
N2 C15 1.331(7) . ?
C16 C12 1.373(7) . ?
C12 C13 1.395(7) . ?
C12 C11 1.478(7) . ?
C14 C13 1.387(8) . ?
C14 C15 1.356(9) . ?
C11 C10 1.305(6) . ?
C10 C9 1.465(6) . ?
C9 O4 1.261(5) . ?
C1 C2 1.494(6) . ?
C1 O2 1.256(5) . ?
C3 C2 1.299(6) . ?
C3 C4 1.476(6) . ?
C8 C4 1.387(7) . ?
C8 N1 1.338(6) . ?
C5 C4 1.373(6) . ?
C5 C6 1.386(7) . ?
N1 C7 1.318(6) . ?
C7 C6 1.358(8) . ?
O2 Sm1 2.407(3) 5_575 ?
N3 C23 1.334(7) . ?
N3 C24 1.347(6) . ?
C20 C24 1.386(8) . ?
C20 C21 1.382(9) . ?
C20 C19 1.487(8) . ?
C23 C22 1.370(9) . ?
C22 C21 1.355(8) . ?
C19 C18 1.271(8) . ?
C18 C17 1.513(7) . ?
C17 Sm1 2.884(5) 8_556 ?
C17 O6 1.237(6) . ?
C17 O5 1.278(6) . ?
O6 Sm1 2.486(3) 8_556 ?
O5 Sm1 2.571(3) 8_556 ?

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
O2W Sm1 O3 72.69(10) . 5_565 ?
O2W Sm1 O3 68.49(10) . . ?
O2W Sm1 O1W 69.86(10) . . ?
O2W Sm1 C17 148.34(12) . 8_455 ?
O2W Sm1 O6 137.42(10) . 8_455 ?
O2W Sm1 O5 143.51(11) . 8_455 ?
O3 Sm1 O3 63.49(11) 5_565 . ?
O3 Sm1 O1W 140.54(10) 5_565 . ?
O3 Sm1 C17 75.84(11) 5_565 8_455 ?
O3 Sm1 C17 94.46(13) . 8_455 ?
O3 Sm1 O6 76.23(10) 5_565 8_455 ?
O3 Sm1 O5 79.02(10) 5_565 8_455 ?
O1 Sm1 O2W 81.91(11) . . ?
O1 Sm1 O3 89.04(11) . 5_565 ?
O1 Sm1 O3 144.05(10) . . ?
O1 Sm1 O1W 73.97(11) . . ?
O1 Sm1 O2 99.86(11) . 5_575 ?
O1 Sm1 C17 101.01(15) . 8_455 ?
O1 Sm1 O6 126.10(12) . 8_455 ?
O1 Sm1 O5 74.94(13) . 8_455 ?
O1 Sm1 O4 144.80(12) . . ?
O1W Sm1 O3 111.99(9) . . ?
O1W Sm1 C17 141.52(11) . 8_455 ?
O1W Sm1 O5 127.52(10) . 8_455 ?
O2 Sm1 O2W 139.35(11) 5_575 . ?
O2 Sm1 O3 115.82(9) 5_575 . ?
O2 Sm1 O3 147.43(10) 5_575 5_565 ?
O2 Sm1 O1W 71.71(10) 5_575 . ?
O2 Sm1 C17 71.73(12) 5_575 8_455 ?
O2 Sm1 O6 73.23(10) 5_575 8_455 ?
O2 Sm1 O5 73.32(11) 5_575 8_455 ?
O2 Sm1 O4 77.52(10) 5_575 . ?
O6 Sm1 O3 71.91(10) 8_455 . ?
O6 Sm1 O1W 142.24(10) 8_455 . ?
O6 Sm1 C17 25.26(13) 8_455 8_455 ?
O6 Sm1 O5 51.55(12) 8_455 8_455 ?
O5 Sm1 O3 118.05(10) 8_455 . ?
O5 Sm1 C17 26.30(14) 8_455 8_455 ?
O4 Sm1 O2W 78.49(11) . . ?
O4 Sm1 O3 48.94(9) . . ?
O4 Sm1 O3 112.21(10) . 5_565 ?
O4 Sm1 O1W 71.93(11) . . ?
O4 Sm1 C17 111.01(15) . 8_455 ?
O4 Sm1 O6 87.27(12) . 8_455 ?
O4 Sm1 O5 134.70(12) . 8_455 ?
Cu3 Br1 Cu3 70.02(3) . 2 ?
Br1 Cu3 Br1 104.46(3) . 2 ?
Br1 Cu3 Cu3 54.52(3) 2 2 ?
Br1 Cu3 Cu3 55.46(3) . 2 ?
N2 Cu3 Br1 107.83(12) . 2 ?
N2 Cu3 Br1 105.18(12) . . ?
N2 Cu3 Cu3 97.15(12) . 2 ?
N3 Cu3 Br1 107.86(13) . 2 ?
N3 Cu3 Br1 115.63(12) . . ?
N3 Cu3 Cu3 147.40(13) . 2 ?
N3 Cu3 N2 115.15(18) . . ?
Sm1 O3 Sm1 116.51(11) 5_565 . ?
C9 O3 Sm1 153.5(3) . 5_565 ?
C9 O3 Sm1 84.1(2) . . ?
C1 O1 Sm1 175.5(3) . . ?
C16 N2 Cu3 119.5(4) . . ?
C15 N2 Cu3 123.8(4) . . ?
C15 N2 C16 116.6(5) . . ?
N2 C16 C12 124.5(5) . . ?
C16 C12 C13 117.4(5) . . ?
C16 C12 C11 121.4(5) . . ?
C13 C12 C11 121.1(5) . . ?
C15 C14 C13 119.5(6) . . ?
C14 C13 C12 118.3(6) . . ?
N2 C15 C14 123.7(5) . . ?
C10 C11 C12 126.7(5) . . ?
C11 C10 C9 122.2(4) . . ?
O3 C9 C10 119.0(4) . . ?
O4 C9 O3 120.2(4) . . ?
O4 C9 C10 120.7(4) . . ?
O1 C1 C2 119.5(4) . . ?
O1 C1 O2 123.9(4) . . ?
O2 C1 C2 116.7(4) . . ?
C2 C3 C4 126.3(4) . . ?
C3 C2 C1 123.8(4) . . ?
N1 C8 C4 123.4(5) . . ?
C4 C5 C6 119.0(5) . . ?
C8 C4 C3 121.9(4) . . ?
C5 C4 C3 120.7(4) . . ?
C5 C4 C8 117.4(4) . . ?
C7 N1 C8 117.9(5) . . ?
N1 C7 C6 122.9(5) . . ?
C7 C6 C5 119.4(5) . . ?
C1 O2 Sm1 131.0(3) . 5_575 ?
C23 N3 Cu3 122.4(4) . . ?
C23 N3 C24 116.3(5) . . ?
C24 N3 Cu3 121.1(4) . . ?
C24 C20 C19 122.8(6) . . ?
C21 C20 C24 117.6(5) . . ?
C21 C20 C19 119.6(6) . . ?
N3 C23 C22 123.0(5) . . ?
N3 C24 C20 123.9(5) . . ?
C21 C22 C23 120.2(6) . . ?
C22 C21 C20 118.9(6) . . ?
C18 C19 C20 126.3(6) . . ?
C19 C18 C17 124.3(6) . . ?
C18 C17 Sm1 175.8(4) . 8_556 ?
O6 C17 Sm1 59.1(3) . 8_556 ?
O6 C17 C18 117.2(5) . . ?
O6 C17 O5 122.1(5) . . ?
O5 C17 Sm1 63.1(2) . 8_556 ?
O5 C17 C18 120.7(5) . . ?
C17 O6 Sm1 95.7(3) . 8_556 ?
C17 O5 Sm1 90.6(3) . 8_556 ?
C9 O4 Sm1 102.4(2) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_13
_database_code_depnum_ccdc_archive 'CCDC 1445871'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H16 Cu2 Eu I2 N2 O8, 2(H2 O)'
_chemical_formula_sum            'C17 H20 Cu2 Eu I2 N2 O10'
_chemical_formula_weight         945.22
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 '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'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.1814(11)
_cell_length_b                   8.2858(11)
_cell_length_c                   18.974(3)
_cell_angle_alpha                86.452(3)
_cell_angle_beta                 84.078(2)
_cell_angle_gamma                79.676(2)
_cell_volume                     1257.4(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1519
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      2.54
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.647
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1113 before and 0.0378 after correction.
The Ratio of minimum to maximum transmission is 0.6797.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.497
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             886
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   0.265
_exptl_transmission_factor_min   0.221
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6600
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.400
_diffrn_reflns_theta_min         1.080
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3533
_reflns_number_total             4611
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker, 2000-2003)'
_refine_diff_density_max         1.388
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.221
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4566
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0451
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0544P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1207
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O5W(H5WA,H5WB), O6W(H6WA,H6WB), O9W(H9WA,H9WB), O10W(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C13(H13), C1(H1), C2(H2), C3(H3), C5(H5), C6(H6),
 C7(H7), C14(H14), C15(H15)
2.c Fitted hexagon refined as free rotating group:
 C9(C10,C11,C12,C13,N2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C9 C 0.9353(8) 0.6004(7) 0.6213(3) 0.043(3) Uani 1 1 d . . . . .
H9 H 1.0003 0.5495 0.5831 0.051 Uiso 1 1 calc R . . . .
C10 C 0.9112(8) 0.5122(6) 0.6852(4) 0.044(3) Uani 1 1 d G . . . .
H10 H 0.9602 0.4022 0.6897 0.053 Uiso 1 1 calc R . . . .
C11 C 0.8139(8) 0.5883(7) 0.7423(3) 0.038(3) Uani 1 1 d G . . . .
H11 H 0.7978 0.5293 0.7850 0.045 Uiso 1 1 calc R . . . .
C12 C 0.7407(8) 0.7527(7) 0.7356(3) 0.035(2) Uani 1 1 d G . . . .
C13 C 0.7647(8) 0.8409(5) 0.6717(3) 0.038(3) Uani 1 1 d G . . . .
H13 H 0.7157 0.9509 0.6672 0.046 Uiso 1 1 calc R . . . .
N2 N 0.8620(8) 0.7648(7) 0.6146(3) 0.035(2) Uani 1 1 d G . . . .
C1 C 1.4879(13) 0.5908(13) 0.6170(6) 0.042(3) Uani 1 1 d . . . . .
H1 H 1.5561 0.5534 0.5769 0.050 Uiso 1 1 calc R . . . .
C2 C 1.4836(13) 0.4876(13) 0.6762(7) 0.045(3) Uani 1 1 d . . . . .
H2 H 1.5491 0.3835 0.6760 0.054 Uiso 1 1 calc R . . . .
C3 C 1.3833(12) 0.5381(12) 0.7353(5) 0.033(2) Uani 1 1 d . . . . .
H3 H 1.3800 0.4691 0.7758 0.039 Uiso 1 1 calc R . . . .
C4 C 1.2850(11) 0.6949(11) 0.7346(5) 0.029(2) Uani 1 1 d . . . . .
C5 C 1.2982(13) 0.7936(13) 0.6721(6) 0.037(3) Uani 1 1 d . . . . .
H5 H 1.2348 0.8986 0.6708 0.044 Uiso 1 1 calc R . . . .
N1 N 1.3988(11) 0.7428(11) 0.6140(5) 0.041(2) Uani 1 1 d . . . . .
C6 C 1.1650(11) 0.7548(12) 0.7930(5) 0.031(2) Uani 1 1 d . . . . .
H6 H 1.1340 0.8678 0.7965 0.037 Uiso 1 1 calc R . . . .
C7 C 1.0972(11) 0.6594(12) 0.8414(5) 0.029(2) Uani 1 1 d . . . . .
H7 H 1.1393 0.5474 0.8417 0.035 Uiso 1 1 calc R . . . .
C8 C 0.9593(10) 0.7181(11) 0.8951(5) 0.025(2) Uani 1 1 d . . . . .
C14 C 0.6554(11) 0.8360(12) 0.7984(5) 0.031(2) Uani 1 1 d . . . . .
H14 H 0.6353 0.7704 0.8388 0.037 Uiso 1 1 calc R . . . .
C15 C 0.6040(12) 0.9964(12) 0.8030(5) 0.031(2) Uani 1 1 d . . . . .
H15 H 0.6216 1.0645 0.7631 0.037 Uiso 1 1 calc R . . . .
C16 C 0.5193(11) 1.0724(11) 0.8692(5) 0.026(2) Uani 1 1 d . . . . .
C17 C 0.4374(10) 1.5524(10) 0.9778(5) 0.023(2) Uani 1 1 d . . . . .
Cu1 Cu 1.39553(17) 0.88922(17) 0.52301(8) 0.0445(4) Uani 1 1 d . . . . .
Cu2 Cu 0.88467(17) 0.89771(17) 0.52011(8) 0.0434(4) Uani 1 1 d . . . . .
Eu1 Eu 0.30259(5) 1.20340(5) 0.99143(3) 0.02019(15) Uani 1 1 d . . . . .
I1 I 1.17315(8) 0.78942(8) 0.44936(4) 0.0411(2) Uani 1 1 d . . . . .
I2 I 1.32639(8) 1.19755(8) 0.56129(4) 0.0368(2) Uani 1 1 d . . . . .
O1 O 0.8716(7) 0.6131(7) 0.9240(4) 0.0316(16) Uani 1 1 d . . . . .
O2 O 0.9254(7) 0.8658(7) 0.9144(3) 0.0294(15) Uani 1 1 d . . . . .
O3 O 0.5551(7) 1.0077(7) 0.9294(3) 0.0238(14) Uani 1 1 d . . . . .
O4 O 0.4128(8) 1.2012(8) 0.8647(4) 0.0340(16) Uani 1 1 d . . . . .
O5W O 0.0500(8) 1.3011(8) 0.9367(4) 0.0359(17) Uani 1 1 d . . . . .
H5WA H -0.0179 1.3905 0.9434 0.043 Uiso 1 1 d R . . . .
H5WB H -0.0062 1.2284 0.9288 0.043 Uiso 1 1 d R . . . .
O6W O 0.2145(8) 0.9640(7) 0.9520(4) 0.0345(17) Uani 1 1 d . . . . .
H6WA H 0.1300 0.9269 0.9416 0.041 Uiso 1 1 d R . . . .
H6WB H 0.3001 0.8906 0.9433 0.041 Uiso 1 1 d R . . . .
O7 O 0.3242(7) 1.4920(7) 0.9566(4) 0.0281(15) Uani 1 1 d . . . . .
O8 O 0.5391(7) 1.2991(7) 1.0348(4) 0.0285(16) Uani 1 1 d . . . . .
O9W O 0.8068(12) 0.8176(12) 0.2436(5) 0.084(3) Uani 1 1 d . . . . .
H9WA H 0.7370 0.8170 0.2135 0.100 Uiso 1 1 d R . . . .
H9WB H 0.7604 0.7943 0.2842 0.100 Uiso 1 1 d R . . . .
O10W O 0.1010(11) 0.8214(10) 0.1601(5) 0.073(3) Uani 1 1 d . . . . .
H10A H 0.1229 0.9182 0.1579 0.088 Uiso 1 1 d R . . . .
H10B H 0.0332 0.8125 0.1966 0.088 Uiso 1 1 d R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C9 H9 0.9300 . ?
C9 C10 1.3900 . ?
C9 N2 1.3900 . ?
C10 H10 0.9300 . ?
C10 C11 1.3900 . ?
C11 H11 0.9300 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C12 C14 1.464(10) . ?
C13 H13 0.9300 . ?
C13 N2 1.3900 . ?
N2 Cu2 2.055(5) . ?
C1 H1 0.9300 . ?
C1 C2 1.371(15) . ?
C1 N1 1.338(13) . ?
C2 H2 0.9300 . ?
C2 C3 1.361(14) . ?
C3 H3 0.9300 . ?
C3 C4 1.400(13) . ?
C4 C5 1.403(14) . ?
C4 C6 1.452(13) . ?
C5 H5 0.9300 . ?
C5 N1 1.348(13) . ?
N1 Cu1 2.047(9) . ?
C6 H6 0.9300 . ?
C6 C7 1.318(13) . ?
C7 H7 0.9300 . ?
C7 C8 1.475(13) . ?
C8 Eu1 2.893(9) 2_677 ?
C8 O1 1.286(10) . ?
C8 O2 1.274(10) . ?
C14 H14 0.9300 . ?
C14 C15 1.326(13) . ?
C15 H15 0.9300 . ?
C15 C16 1.490(13) . ?
C16 O3 1.270(11) . ?
C16 O4 1.255(11) . ?
C17 C17 1.510(17) 2_687 ?
C17 O7 1.240(10) . ?
C17 O8 1.283(10) 2_687 ?
Cu1 Cu1 2.770(3) 2_876 ?
Cu1 Cu2 2.793(2) 2_776 ?
Cu1 I1 2.6746(16) . ?
Cu1 I2 2.6460(16) . ?
Cu1 I2 2.6563(15) 2_876 ?
Cu2 Cu1 2.793(2) 2_776 ?
Cu2 Cu2 2.776(3) 2_776 ?
Cu2 I1 2.6400(15) 2_776 ?
Cu2 I1 2.6294(15) . ?
Cu2 I2 2.6795(16) 2_776 ?
Eu1 C8 2.893(9) 2_677 ?
Eu1 Eu1 4.2520(10) 2_677 ?
Eu1 O1 2.444(6) 2_677 ?
Eu1 O2 2.563(6) 2_677 ?
Eu1 O3 2.445(6) 2_677 ?
Eu1 O3 2.611(6) . ?
Eu1 O4 2.479(7) . ?
Eu1 O5W 2.396(6) . ?
Eu1 O6W 2.413(6) . ?
Eu1 H6WB 2.8048 . ?
Eu1 O7 2.473(6) . ?
Eu1 O8 2.452(6) . ?
I1 Cu2 2.6400(15) 2_776 ?
I2 Cu1 2.6563(15) 2_876 ?
I2 Cu2 2.6795(16) 2_776 ?
O1 Eu1 2.444(6) 2_677 ?
O2 Eu1 2.563(6) 2_677 ?
O3 Eu1 2.445(6) 2_677 ?
O5W H5WA 0.8500 . ?
O5W H5WB 0.8500 . ?
O6W H6WA 0.8500 . ?
O6W H6WB 0.8501 . ?
O8 C17 1.283(10) 2_687 ?
O9W H9WA 0.8500 . ?
O9W H9WB 0.8501 . ?
O10W H10A 0.8499 . ?
O10W H10B 0.8501 . ?

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
C10 C9 H9 120.0 . . ?
C10 C9 N2 120.0 . . ?
N2 C9 H9 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 C14 119.2(6) . . ?
C13 C12 C11 120.0 . . ?
C13 C12 C14 120.4(6) . . ?
C12 C13 H13 120.0 . . ?
C12 C13 N2 120.0 . . ?
N2 C13 H13 120.0 . . ?
C9 N2 Cu2 121.5(3) . . ?
C13 N2 C9 120.0 . . ?
C13 N2 Cu2 118.4(3) . . ?
C2 C1 H1 118.4 . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.2(10) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.7(10) . . ?
C3 C2 H2 120.1 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.3(10) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C5 117.4(9) . . ?
C3 C4 C6 123.3(9) . . ?
C5 C4 C6 119.2(9) . . ?
C4 C5 H5 118.6 . . ?
N1 C5 C4 122.8(10) . . ?
N1 C5 H5 118.6 . . ?
C1 N1 C5 117.5(9) . . ?
C1 N1 Cu1 122.5(7) . . ?
C5 N1 Cu1 119.8(7) . . ?
C4 C6 H6 117.9 . . ?
C7 C6 C4 124.3(9) . . ?
C7 C6 H6 117.9 . . ?
C6 C7 H7 117.7 . . ?
C6 C7 C8 124.5(9) . . ?
C8 C7 H7 117.7 . . ?
C7 C8 Eu1 173.5(7) . 2_677 ?
O1 C8 C7 117.7(8) . . ?
O1 C8 Eu1 57.0(5) . 2_677 ?
O2 C8 C7 123.1(8) . . ?
O2 C8 Eu1 62.3(5) . 2_677 ?
O2 C8 O1 119.2(8) . . ?
C12 C14 H14 117.0 . . ?
C15 C14 C12 126.0(9) . . ?
C15 C14 H14 117.0 . . ?
C14 C15 H15 118.6 . . ?
C14 C15 C16 122.8(9) . . ?
C16 C15 H15 118.6 . . ?
O3 C16 C15 120.2(8) . . ?
O4 C16 C15 119.1(9) . . ?
O4 C16 O3 120.6(9) . . ?
O7 C17 C17 119.7(9) . 2_687 ?
O7 C17 O8 125.6(8) . 2_687 ?
O8 C17 C17 114.6(10) 2_687 2_687 ?
N1 Cu1 Cu1 128.0(3) . 2_876 ?
N1 Cu1 Cu2 124.9(3) . 2_776 ?
N1 Cu1 I1 104.6(3) . . ?
N1 Cu1 I2 110.3(3) . 2_876 ?
N1 Cu1 I2 107.2(3) . . ?
Cu1 Cu1 Cu2 92.24(7) 2_876 2_776 ?
I1 Cu1 Cu1 126.98(8) . 2_876 ?
I1 Cu1 Cu2 57.70(5) . 2_776 ?
I2 Cu1 Cu1 58.69(5) . 2_876 ?
I2 Cu1 Cu1 58.32(5) 2_876 2_876 ?
I2 Cu1 Cu2 58.96(4) . 2_776 ?
I2 Cu1 Cu2 123.67(6) 2_876 2_776 ?
I2 Cu1 I1 116.52(6) . . ?
I2 Cu1 I1 100.51(5) 2_876 . ?
I2 Cu1 I2 117.01(5) . 2_876 ?
N2 Cu2 Cu1 118.62(18) . 2_776 ?
N2 Cu2 Cu2 126.71(19) . 2_776 ?
N2 Cu2 I1 109.89(18) . . ?
N2 Cu2 I1 106.84(18) . 2_776 ?
N2 Cu2 I2 105.65(18) . 2_776 ?
Cu2 Cu2 Cu1 97.09(8) 2_776 2_776 ?
I1 Cu2 Cu1 130.45(7) . 2_776 ?
I1 Cu2 Cu1 58.91(5) 2_776 2_776 ?
I1 Cu2 Cu2 58.40(5) . 2_776 ?
I1 Cu2 Cu2 58.02(5) 2_776 2_776 ?
I1 Cu2 I1 116.42(5) . 2_776 ?
I1 Cu2 I2 116.56(6) 2_776 2_776 ?
I1 Cu2 I2 100.93(5) . 2_776 ?
I2 Cu2 Cu1 57.79(5) 2_776 2_776 ?
I2 Cu2 Cu2 127.22(8) 2_776 2_776 ?
C8 Eu1 Eu1 122.08(18) 2_677 2_677 ?
C8 Eu1 H6WB 110.2 2_677 . ?
Eu1 Eu1 H6WB 55.7 2_677 . ?
O1 Eu1 C8 26.2(2) 2_677 2_677 ?
O1 Eu1 Eu1 134.50(16) 2_677 2_677 ?
O1 Eu1 O2 52.28(19) 2_677 2_677 ?
O1 Eu1 O3 101.6(2) 2_677 2_677 ?
O1 Eu1 O3 162.3(2) 2_677 . ?
O1 Eu1 O4 140.1(2) 2_677 . ?
O1 Eu1 H6WB 136.0 2_677 . ?
O1 Eu1 O7 70.1(2) 2_677 . ?
O1 Eu1 O8 85.7(2) 2_677 . ?
O2 Eu1 C8 26.1(2) 2_677 2_677 ?
O2 Eu1 Eu1 103.62(14) 2_677 2_677 ?
O2 Eu1 O3 129.17(19) 2_677 . ?
O2 Eu1 H6WB 84.6 2_677 . ?
O3 Eu1 C8 152.4(2) . 2_677 ?
O3 Eu1 C8 88.7(2) 2_677 2_677 ?
O3 Eu1 Eu1 31.57(13) . 2_677 ?
O3 Eu1 Eu1 33.99(14) 2_677 2_677 ?
O3 Eu1 O2 74.64(19) 2_677 2_677 ?
O3 Eu1 O3 65.6(2) 2_677 . ?
O3 Eu1 O4 116.5(2) 2_677 . ?
O3 Eu1 H6WB 70.0 2_677 . ?
O3 Eu1 H6WB 53.4 . . ?
O3 Eu1 O7 135.11(19) 2_677 . ?
O3 Eu1 O8 70.05(19) 2_677 . ?
O4 Eu1 C8 152.7(2) . 2_677 ?
O4 Eu1 Eu1 82.55(14) . 2_677 ?
O4 Eu1 O2 147.2(2) . 2_677 ?
O4 Eu1 O3 51.0(2) . . ?
O4 Eu1 H6WB 72.3 . . ?
O5W Eu1 C8 73.2(2) . 2_677 ?
O5W Eu1 Eu1 143.66(16) . 2_677 ?
O5W Eu1 O1 74.8(2) . 2_677 ?
O5W Eu1 O2 76.6(2) . 2_677 ?
O5W Eu1 O3 145.4(2) . 2_677 ?
O5W Eu1 O3 122.7(2) . . ?
O5W Eu1 O4 79.8(2) . . ?
O5W Eu1 O6W 73.8(2) . . ?
O5W Eu1 H6WB 88.6 . . ?
O5W Eu1 O7 77.0(2) . . ?
O5W Eu1 O8 141.8(2) . . ?
O6W Eu1 C8 98.0(2) . 2_677 ?
O6W Eu1 Eu1 71.56(15) . 2_677 ?
O6W Eu1 O1 122.4(2) . 2_677 ?
O6W Eu1 O2 74.0(2) . 2_677 ?
O6W Eu1 O3 69.2(2) . . ?
O6W Eu1 O3 80.1(2) . 2_677 ?
O6W Eu1 O4 77.7(2) . . ?
O6W Eu1 H6WB 16.7 . . ?
O6W Eu1 O7 142.6(2) . . ?
O6W Eu1 O8 143.0(2) . . ?
O7 Eu1 C8 95.3(2) . 2_677 ?
O7 Eu1 Eu1 127.86(14) . 2_677 ?
O7 Eu1 O2 120.9(2) . 2_677 ?
O7 Eu1 O3 109.64(19) . . ?
O7 Eu1 O4 74.6(2) . . ?
O7 Eu1 H6WB 145.7 . . ?
O8 Eu1 C8 102.6(2) . 2_677 ?
O8 Eu1 Eu1 71.44(13) . 2_677 ?
O8 Eu1 O2 116.5(2) . 2_677 ?
O8 Eu1 O3 78.5(2) . . ?
O8 Eu1 O4 96.1(2) . . ?
O8 Eu1 H6WB 126.7 . . ?
O8 Eu1 O7 65.44(19) . . ?
Cu2 I1 Cu1 103.78(5) . . ?
Cu2 I1 Cu1 63.40(5) 2_776 . ?
Cu2 I1 Cu2 63.58(5) . 2_776 ?
Cu1 I2 Cu1 62.99(5) . 2_876 ?
Cu1 I2 Cu2 63.25(5) . 2_776 ?
Cu1 I2 Cu2 97.43(5) 2_876 2_776 ?
C8 O1 Eu1 96.8(5) . 2_677 ?
C8 O2 Eu1 91.6(5) . 2_677 ?
C16 O3 Eu1 90.3(5) . . ?
C16 O3 Eu1 154.4(6) . 2_677 ?
Eu1 O3 Eu1 114.4(2) 2_677 . ?
C16 O4 Eu1 96.9(6) . . ?
Eu1 O5W H5WA 128.0 . . ?
Eu1 O5W H5WB 115.8 . . ?
H5WA O5W H5WB 107.7 . . ?
Eu1 O6W H6WA 143.4 . . ?
Eu1 O6W H6WB 108.8 . . ?
H6WA O6W H6WB 107.7 . . ?
C17 O7 Eu1 119.1(5) . . ?
C17 O8 Eu1 121.1(5) 2_687 . ?
H9WA O9W H9WB 107.7 . . ?
H10A O10W H10B 107.7 . . ?

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
C9 C10 C11 C12 0.0 . . . . ?
C10 C9 N2 C13 0.0 . . . . ?
C10 C9 N2 Cu2 -177.1(4) . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C10 C11 C12 C14 -172.8(7) . . . . ?
C11 C12 C13 N2 0.0 . . . . ?
C11 C12 C14 C15 168.3(8) . . . . ?
C12 C13 N2 C9 0.0 . . . . ?
C12 C13 N2 Cu2 177.2(4) . . . . ?
C12 C14 C15 C16 -179.4(8) . . . . ?
C13 C12 C14 C15 -4.5(12) . . . . ?
N2 C9 C10 C11 0.0 . . . . ?
C1 C2 C3 C4 0.3(16) . . . . ?
C2 C1 N1 C5 -1.3(16) . . . . ?
C2 C1 N1 Cu1 -175.9(8) . . . . ?
C2 C3 C4 C5 -1.1(14) . . . . ?
C2 C3 C4 C6 175.2(9) . . . . ?
C3 C4 C5 N1 0.7(15) . . . . ?
C3 C4 C6 C7 -22.1(16) . . . . ?
C4 C5 N1 C1 0.5(16) . . . . ?
C4 C5 N1 Cu1 175.3(7) . . . . ?
C4 C6 C7 C8 -171.5(9) . . . . ?
C5 C4 C6 C7 154.0(10) . . . . ?
N1 C1 C2 C3 0.9(17) . . . . ?
C6 C4 C5 N1 -175.7(9) . . . . ?
C6 C7 C8 O1 158.9(10) . . . . ?
C6 C7 C8 O2 -22.0(15) . . . . ?
C7 C8 O1 Eu1 175.6(7) . . . 2_677 ?
C7 C8 O2 Eu1 -175.7(8) . . . 2_677 ?
C14 C12 C13 N2 172.7(7) . . . . ?
C14 C15 C16 O3 31.5(14) . . . . ?
C14 C15 C16 O4 -148.8(9) . . . . ?
C15 C16 O3 Eu1 -169.7(7) . . . . ?
C15 C16 O3 Eu1 -4.0(18) . . . 2_677 ?
C15 C16 O4 Eu1 169.1(7) . . . . ?
C17 C17 O7 Eu1 2.1(13) 2_687 . . . ?
O1 C8 O2 Eu1 3.4(9) . . . 2_677 ?
O2 C8 O1 Eu1 -3.5(9) . . . 2_677 ?
O3 C16 O4 Eu1 -11.1(9) . . . . ?
O4 C16 O3 Eu1 176.2(8) . . . 2_677 ?
O4 C16 O3 Eu1 10.5(8) . . . . ?
O8 C17 O7 Eu1 -178.3(7) 2_687 . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_14
_database_code_depnum_ccdc_archive 'CCDC 1445872'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C17 H16 Cu2 Gd I2 N2 O8, 2(H2 O)'
_chemical_formula_sum            'C17 H20 Cu2 Gd I2 N2 O10'
_chemical_formula_weight         950.50
_chemical_melting_point          ?
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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.161(3)
_cell_length_b                   8.250(3)
_cell_length_c                   18.961(6)
_cell_angle_alpha                86.444(7)
_cell_angle_beta                 83.969(6)
_cell_angle_gamma                79.622(6)
_cell_volume                     1247.4(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1129
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.51
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.844
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1433 before and 0.0514 after correction.
The Ratio of minimum to maximum transmission is 0.4988.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.530
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   0.254
_exptl_transmission_factor_min   0.211
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.1159
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6611
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.392
_diffrn_reflns_theta_min         2.162
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3042
_reflns_number_total             4587
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         2.188
_refine_diff_density_min         -2.246
_refine_diff_density_rms         0.302
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4524
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0661
_refine_ls_restrained_S_all      0.954
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0829P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1739
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O7W(H7WA,H7WB), O8W(H8WA,H8WB), O9W(H9WA,H9WB), O10W(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C1(H1), C5(H5), C4(H4), C3(H3), C15(H15), C14(H14), C11(H11),
 C12(H12), C13(H13), C9(H9)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Gd1 Gd 0.80301(8) 0.20354(8) 0.49136(3) 0.0260(2) Uani 1 1 d . . . . .
I1 I 0.82605(12) 0.19850(13) 1.06120(5) 0.0417(3) Uani 1 1 d . . . . .
I2 I 0.32641(12) 0.21136(13) 1.05061(6) 0.0456(3) Uani 1 1 d . . . . .
Cu1 Cu 0.6154(2) 0.1027(3) 0.97981(10) 0.0481(5) Uani 1 1 d . . . . .
Cu2 Cu 0.8952(3) -0.1104(3) 1.02311(10) 0.0486(5) Uani 1 1 d . . . . .
O5 O 0.8251(11) 0.4940(11) 0.4572(5) 0.033(2) Uani 1 1 d . . . . .
O1 O 0.9446(11) -0.0081(11) 0.5697(4) 0.028(2) Uani 1 1 d . . . . .
O3 O 0.5752(12) 0.1335(12) 0.5850(5) 0.036(2) Uani 1 1 d . . . . .
O7W O 0.7151(11) -0.0321(11) 0.4513(5) 0.037(2) Uani 1 1 d . . . . .
H7WA H 0.6238 -0.0549 0.4402 0.045 Uiso 1 1 d R . . . .
H7WB H 0.7942 -0.1054 0.4346 0.045 Uiso 1 1 d R . . . .
O8W O 0.5499(11) 0.3015(11) 0.4364(5) 0.037(2) Uani 1 1 d . . . . .
H8WA H 0.4836 0.2438 0.4590 0.045 Uiso 1 1 d R . . . .
H8WB H 0.4950 0.3979 0.4293 0.045 Uiso 1 1 d R . . . .
C8 C 0.9781(16) -0.0738(17) 0.6316(7) 0.029(3) Uani 1 1 d . . . . .
O2 O 1.0835(13) -0.2017(12) 0.6342(5) 0.041(2) Uani 1 1 d . . . . .
C7 C 0.8965(18) 0.0039(19) 0.6959(7) 0.041(4) Uani 1 1 d . . . . .
H7 H 0.8779 -0.0657 0.7353 0.049 Uiso 1 1 calc R . . . .
C6 C 0.8472(17) 0.1611(18) 0.7038(7) 0.036(3) Uani 1 1 d . . . . .
H6 H 0.8738 0.2285 0.6647 0.043 Uiso 1 1 calc R . . . .
C2 C 0.7570(18) 0.2470(19) 0.7643(7) 0.036(3) Uani 1 1 d . . . . .
C1 C 0.7290(18) 0.1654(19) 0.8298(8) 0.041(4) Uani 1 1 d . . . . .
H1 H 0.7773 0.0548 0.8348 0.049 Uiso 1 1 calc R . . . .
N1 N 0.6384(17) 0.2350(16) 0.8851(7) 0.048(3) Uani 1 1 d . . . . .
C5 C 0.570(2) 0.392(2) 0.8775(9) 0.051(4) Uani 1 1 d . . . . .
H5 H 0.5049 0.4415 0.9162 0.062 Uiso 1 1 calc R . . . .
C4 C 0.588(2) 0.486(2) 0.8168(8) 0.048(4) Uani 1 1 d . . . . .
H4 H 0.5384 0.5968 0.8142 0.058 Uiso 1 1 calc R . . . .
C3 C 0.6840(19) 0.412(2) 0.7589(8) 0.043(4) Uani 1 1 d . . . . .
H3 H 0.6992 0.4734 0.7165 0.051 Uiso 1 1 calc R . . . .
O4 O 0.6288(11) 0.3839(12) 0.5765(5) 0.036(2) Uani 1 1 d . . . . .
C16 C 0.5429(16) 0.2808(17) 0.6026(8) 0.033(3) Uani 1 1 d . . . . .
C15 C 0.4059(16) 0.3417(16) 0.6591(7) 0.029(3) Uani 1 1 d . . . . .
H15 H 0.3690 0.4549 0.6612 0.035 Uiso 1 1 calc R . . . .
C14 C 0.3338(19) 0.2426(19) 0.7066(8) 0.041(4) Uani 1 1 d . . . . .
H14 H 0.3606 0.1293 0.7013 0.050 Uiso 1 1 calc R . . . .
C10 C 0.2173(18) 0.3026(18) 0.7652(7) 0.037(3) Uani 1 1 d . . . . .
C11 C 0.1152(18) 0.461(2) 0.7649(7) 0.040(4) Uani 1 1 d . . . . .
H11 H 0.1158 0.5306 0.7243 0.048 Uiso 1 1 calc R . . . .
C12 C 0.0170(18) 0.5106(18) 0.8245(7) 0.039(4) Uani 1 1 d . . . . .
H12 H -0.0481 0.6154 0.8252 0.047 Uiso 1 1 calc R . . . .
C13 C 0.0127(19) 0.408(2) 0.8834(8) 0.043(4) Uani 1 1 d . . . . .
H13 H -0.0560 0.4441 0.9237 0.051 Uiso 1 1 calc R . . . .
N2 N 0.1040(15) 0.2569(15) 0.8851(6) 0.037(3) Uani 1 1 d . . . . .
C9 C 0.200(2) 0.204(2) 0.8276(8) 0.051(4) Uani 1 1 d . . . . .
H9 H 0.2601 0.0972 0.8287 0.061 Uiso 1 1 calc R . . . .
C17 C 0.9393(17) 0.5492(17) 0.4782(7) 0.030(3) Uani 1 1 d . . . . .
O6 O 0.9619(11) 0.7007(11) 0.4655(5) 0.037(2) Uani 1 1 d . . . . .
O9W O 0.4028(17) 0.1770(17) 0.3381(7) 0.084(4) Uani 1 1 d . . . . .
H9WA H 0.4044 0.0790 0.3551 0.101 Uiso 1 1 d R . . . .
H9WB H 0.3068 0.2325 0.3502 0.101 Uiso 1 1 d R . . . .
O10W O 0.305(2) 0.817(2) 0.7427(8) 0.101(5) Uani 1 1 d . . . . .
H10A H 0.2358 0.8098 0.7128 0.122 Uiso 1 1 d R . . . .
H10B H 0.2509 0.8209 0.7837 0.122 Uiso 1 1 d R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O5 2.477(9) . ?
Gd1 O1 2.429(9) . ?
Gd1 O1 2.592(9) 2_756 ?
Gd1 O3 2.551(9) . ?
Gd1 O7W 2.382(8) . ?
Gd1 O8W 2.399(9) . ?
Gd1 C8 2.919(13) 2_756 ?
Gd1 O2 2.462(9) 2_756 ?
Gd1 O4 2.428(9) . ?
Gd1 C16 2.845(15) . ?
Gd1 O6 2.435(8) 2_766 ?
I1 Cu1 2.676(2) . ?
I1 Cu2 2.638(2) . ?
I1 Cu2 2.653(2) 2_757 ?
I2 Cu1 2.625(2) . ?
I2 Cu1 2.638(2) 2_657 ?
I2 Cu2 2.672(2) 2_657 ?
Cu1 I2 2.638(2) 2_657 ?
Cu1 Cu1 2.773(4) 2_657 ?
Cu1 Cu2 2.784(3) . ?
Cu1 N1 2.051(14) . ?
Cu2 I1 2.653(2) 2_757 ?
Cu2 I2 2.672(2) 2_657 ?
Cu2 Cu2 2.761(4) 2_757 ?
Cu2 N2 2.056(12) 2_657 ?
O5 C17 1.221(15) . ?
O1 Gd1 2.592(9) 2_756 ?
O1 C8 1.297(16) . ?
O3 C16 1.255(16) . ?
C8 Gd1 2.919(13) 2_756 ?
C8 O2 1.237(16) . ?
C8 C7 1.453(18) . ?
O2 Gd1 2.462(9) 2_756 ?
C7 C6 1.30(2) . ?
C6 C2 1.448(19) . ?
C2 C1 1.39(2) . ?
C2 C3 1.39(2) . ?
C1 N1 1.318(18) . ?
N1 C5 1.32(2) . ?
C5 C4 1.36(2) . ?
C4 C3 1.38(2) . ?
O4 C16 1.244(16) . ?
C16 C15 1.505(19) . ?
C15 C14 1.340(19) . ?
C14 C10 1.435(19) . ?
C10 C11 1.42(2) . ?
C10 C9 1.40(2) . ?
C11 C12 1.355(19) . ?
C12 C13 1.36(2) . ?
C13 N2 1.331(19) . ?
N2 Cu2 2.057(12) 2_657 ?
N2 C9 1.323(18) . ?
C17 C17 1.46(3) 2_766 ?
C17 O6 1.300(16) . ?
O6 Gd1 2.435(8) 2_766 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Gd1 O1 109.8(3) . 2_756 ?
O5 Gd1 O3 120.9(3) . . ?
O5 Gd1 C8 93.7(3) . 2_756 ?
O5 Gd1 C16 95.3(4) . . ?
O1 Gd1 O5 135.0(3) . . ?
O1 Gd1 O1 65.1(3) . 2_756 ?
O1 Gd1 O3 74.6(3) . . ?
O1 Gd1 C8 91.3(4) . 2_756 ?
O1 Gd1 C8 26.4(3) 2_756 2_756 ?
O1 Gd1 O2 116.0(3) . 2_756 ?
O1 Gd1 C16 89.0(3) . . ?
O1 Gd1 C16 152.3(3) 2_756 . ?
O1 Gd1 O6 70.3(3) . 2_766 ?
O3 Gd1 O1 128.9(3) . 2_756 ?
O3 Gd1 C8 142.6(3) . 2_756 ?
O3 Gd1 C16 26.2(3) . . ?
O7W Gd1 O5 142.3(3) . . ?
O7W Gd1 O1 69.5(3) . 2_756 ?
O7W Gd1 O1 80.5(3) . . ?
O7W Gd1 O3 74.1(3) . . ?
O7W Gd1 O8W 73.2(3) . . ?
O7W Gd1 C8 69.4(3) . 2_756 ?
O7W Gd1 O2 77.7(3) . 2_756 ?
O7W Gd1 O4 122.0(3) . . ?
O7W Gd1 C16 97.9(4) . . ?
O7W Gd1 O6 143.5(3) . 2_766 ?
O8W Gd1 O5 77.3(3) . . ?
O8W Gd1 O1 145.3(3) . . ?
O8W Gd1 O1 122.9(3) . 2_756 ?
O8W Gd1 O3 76.7(3) . . ?
O8W Gd1 C8 99.9(4) . 2_756 ?
O8W Gd1 O2 80.3(3) . 2_756 ?
O8W Gd1 O4 75.2(3) . . ?
O8W Gd1 C16 73.0(3) . . ?
O8W Gd1 O6 141.8(3) . 2_766 ?
O2 Gd1 O5 74.7(3) 2_756 . ?
O2 Gd1 O1 50.9(3) 2_756 2_756 ?
O2 Gd1 O3 147.7(3) 2_756 . ?
O2 Gd1 C8 24.8(3) 2_756 2_756 ?
O2 Gd1 C16 153.0(4) 2_756 . ?
O4 Gd1 O5 70.5(3) . . ?
O4 Gd1 O1 161.8(3) . 2_756 ?
O4 Gd1 O1 101.2(3) . . ?
O4 Gd1 O3 51.9(3) . . ?
O4 Gd1 C8 164.1(3) . 2_756 ?
O4 Gd1 O2 140.9(3) . 2_756 ?
O4 Gd1 C16 25.8(3) . . ?
O4 Gd1 O6 85.7(3) . 2_766 ?
C16 Gd1 C8 167.0(4) . 2_756 ?
O6 Gd1 O5 65.1(3) 2_766 . ?
O6 Gd1 O1 78.4(3) 2_766 2_756 ?
O6 Gd1 O3 116.6(3) 2_766 . ?
O6 Gd1 C8 89.4(3) 2_766 2_756 ?
O6 Gd1 O2 95.5(3) 2_766 2_756 ?
O6 Gd1 C16 102.9(3) 2_766 . ?
Cu2 I1 Cu1 63.18(7) . . ?
Cu2 I1 Cu1 97.28(7) 2_757 . ?
Cu2 I1 Cu2 62.89(8) . 2_757 ?
Cu1 I2 Cu1 63.61(8) . 2_657 ?
Cu1 I2 Cu2 63.25(7) 2_657 2_657 ?
Cu1 I2 Cu2 103.60(7) . 2_657 ?
I1 Cu1 Cu1 127.14(12) . 2_657 ?
I1 Cu1 Cu2 57.75(7) . . ?
I2 Cu1 I1 116.60(9) 2_657 . ?
I2 Cu1 I1 100.84(7) . . ?
I2 Cu1 I2 116.39(8) . 2_657 ?
I2 Cu1 Cu1 57.97(8) 2_657 2_657 ?
I2 Cu1 Cu1 58.42(7) . 2_657 ?
I2 Cu1 Cu2 58.97(7) 2_657 . ?
I2 Cu1 Cu2 130.30(9) . . ?
Cu1 Cu1 Cu2 97.00(12) 2_657 . ?
N1 Cu1 I1 105.8(4) . . ?
N1 Cu1 I2 106.6(3) . 2_657 ?
N1 Cu1 I2 110.1(4) . . ?
N1 Cu1 Cu1 126.6(4) . 2_657 ?
N1 Cu1 Cu2 118.6(4) . . ?
I1 Cu2 I1 117.11(8) . 2_757 ?
I1 Cu2 I2 100.27(7) 2_757 2_657 ?
I1 Cu2 I2 116.71(8) . 2_657 ?
I1 Cu2 Cu1 59.06(7) . . ?
I1 Cu2 Cu1 123.62(9) 2_757 . ?
I1 Cu2 Cu2 58.82(8) . 2_757 ?
I1 Cu2 Cu2 58.28(7) 2_757 2_757 ?
I2 Cu2 Cu1 57.78(7) 2_657 . ?
I2 Cu2 Cu2 126.93(12) 2_657 2_757 ?
Cu2 Cu2 Cu1 92.34(11) 2_757 . ?
N2 Cu2 I1 106.9(3) 2_657 . ?
N2 Cu2 I1 110.7(4) 2_657 2_757 ?
N2 Cu2 I2 104.4(3) 2_657 2_657 ?
N2 Cu2 Cu1 124.4(4) 2_657 . ?
N2 Cu2 Cu2 128.2(4) 2_657 2_757 ?
C17 O5 Gd1 117.6(9) . . ?
Gd1 O1 Gd1 114.9(3) . 2_756 ?
C8 O1 Gd1 153.3(9) . . ?
C8 O1 Gd1 91.0(8) . 2_756 ?
C16 O3 Gd1 90.1(8) . . ?
O1 C8 Gd1 62.6(6) . 2_756 ?
O1 C8 C7 120.5(13) . . ?
O2 C8 Gd1 56.5(6) . 2_756 ?
O2 C8 O1 118.1(12) . . ?
O2 C8 C7 121.3(13) . . ?
C7 C8 Gd1 169.0(9) . 2_756 ?
C8 O2 Gd1 98.8(8) . 2_756 ?
C6 C7 C8 126.4(14) . . ?
C7 C6 C2 129.7(14) . . ?
C1 C2 C6 121.7(14) . . ?
C3 C2 C6 121.8(14) . . ?
C3 C2 C1 116.4(13) . . ?
N1 C1 C2 124.2(16) . . ?
C1 N1 Cu1 120.1(12) . . ?
C1 N1 C5 117.5(15) . . ?
C5 N1 Cu1 122.4(10) . . ?
N1 C5 C4 124.3(15) . . ?
C5 C4 C3 117.9(16) . . ?
C4 C3 C2 119.8(15) . . ?
C16 O4 Gd1 96.2(9) . . ?
O3 C16 Gd1 63.7(7) . . ?
O3 C16 C15 122.5(13) . . ?
O4 C16 Gd1 58.0(7) . . ?
O4 C16 O3 121.5(13) . . ?
O4 C16 C15 115.9(12) . . ?
C15 C16 Gd1 173.6(10) . . ?
C14 C15 C16 123.9(13) . . ?
C15 C14 C10 123.3(14) . . ?
C11 C10 C14 123.6(14) . . ?
C9 C10 C14 120.4(15) . . ?
C9 C10 C11 116.0(13) . . ?
C12 C11 C10 119.1(14) . . ?
C11 C12 C13 120.5(16) . . ?
N2 C13 C12 121.9(14) . . ?
C13 N2 Cu2 120.7(9) . 2_657 ?
C9 N2 Cu2 120.1(11) . 2_657 ?
C9 N2 C13 119.1(14) . . ?
N2 C9 C10 123.2(16) . . ?
O5 C17 C17 122.4(16) . 2_766 ?
O5 C17 O6 123.6(12) . . ?
O6 C17 C17 114.0(15) . 2_766 ?
C17 O6 Gd1 120.8(8) . 2_766 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_15
_database_code_depnum_ccdc_archive 'CCDC 1445873'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H16 Cu2 I2 N2 Nd O8, 2(H2 O)'
_chemical_formula_sum            'C17 H20 Cu2 I2 N2 Nd O10'
_chemical_formula_weight         937.49
_chemical_melting_point          ?
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'
Nd Nd -0.1943 3.0179 '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'

_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.
;
_symmetry_cell_setting           Triclinic
_space_group_IT_number           2
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2377(17)
_cell_length_b                   8.3660(17)
_cell_length_c                   18.956(4)
_cell_angle_alpha                86.420(4)
_cell_angle_beta                 84.477(4)
_cell_angle_gamma                79.549(3)
_cell_volume                     1277.4(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4691
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.398
_cell_measurement_theta_min      2.161
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.121
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.437
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   0.294
_exptl_transmission_factor_min   0.239
_diffrn_reflns_av_R_equivalents  0.1146
_diffrn_reflns_av_unetI/netI     0.1284
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6549
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.398
_diffrn_reflns_theta_min         2.161
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3059
_reflns_number_total             4691
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.750
_refine_diff_density_min         -2.275
_refine_diff_density_rms         0.263
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4558
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0621
_refine_ls_restrained_S_all      0.914
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0527P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1451
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Riding coordinates:
 O7W(H7WA,H7WB), O8W(H8WA,H8WB), O9W(H9WA,H9WB), O10W(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C7(H7), C15(H15), C2(H2), C1(H1), C9(H9), C3(H3), C5(H5), C13(H13),
 C6(H6), C10(H10), C11(H11)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
O5 O 0.3266(9) -0.0102(9) -0.0442(4) 0.034(2) Uani 1 1 d . . . . .
O6 O 0.4577(9) 0.2020(9) -0.0346(5) 0.039(2) Uani 1 1 d . . . . .
C12 C 0.2584(14) 0.7457(16) 0.2655(6) 0.034(3) Uani 1 1 d . . . . .
C14 C 0.3475(14) 0.6660(15) 0.2043(7) 0.039(3) Uani 1 1 d . . . . .
H14 H 0.3686 0.7326 0.1646 0.047 Uiso 1 1 calc R . . . .
C7 C 0.0958(13) 0.1549(15) 0.8396(6) 0.031(3) Uani 1 1 d . . . . .
H7 H 0.1371 0.0439 0.8390 0.038 Uiso 1 1 calc R . . . .
C8 C -0.0402(14) 0.2124(13) 0.8931(7) 0.032(3) Uani 1 1 d . . . . .
C15 C 0.4036(15) 0.5042(14) 0.1986(7) 0.036(3) Uani 1 1 d . . . . .
H15 H 0.3905 0.4359 0.2386 0.044 Uiso 1 1 calc R . . . .
C16 C 0.4846(14) 0.4301(14) 0.1322(6) 0.028(3) Uani 1 1 d . . . . .
Cu1 Cu 0.3959(2) 0.3888(2) 0.52234(9) 0.0486(4) Uani 1 1 d . . . . .
Cu2 Cu 0.1135(2) 0.6022(2) 0.48013(9) 0.0480(5) Uani 1 1 d . . . . .
I1 I 0.17191(10) 0.29185(11) 0.44890(5) 0.0450(3) Uani 1 1 d . . . . .
I2 I 0.32754(10) 0.69435(11) 0.56131(5) 0.0414(3) Uani 1 1 d . . . . .
Nd1 Nd 0.69917(7) 0.29699(7) 0.00841(3) 0.02401(19) Uani 1 1 d . . . . .
O1 O -0.1243(9) 0.1120(9) 0.9230(5) 0.037(2) Uani 1 1 d . . . . .
O2 O -0.0723(9) 0.3588(9) 0.9122(4) 0.0327(19) Uani 1 1 d . . . . .
O3 O 0.5913(10) 0.3014(9) 0.1375(4) 0.036(2) Uani 1 1 d . . . . .
O4 O 0.4484(9) 0.4932(8) 0.0724(4) 0.0255(17) Uani 1 1 d . . . . .
O7W O 0.9565(9) 0.1997(9) 0.0642(4) 0.0331(19) Uani 1 1 d . . . . .
H7WA H 1.0513 0.1699 0.0425 0.040 Uiso 1 1 d R . . . .
H7WB H 0.9631 0.1698 0.1077 0.040 Uiso 1 1 d R . . . .
O8W O 0.7898(9) 0.5393(9) 0.0479(5) 0.042(2) Uani 1 1 d . . . . .
H8WA H 0.8664 0.5696 0.0678 0.051 Uiso 1 1 d R . . . .
H8WB H 0.7043 0.6130 0.0526 0.051 Uiso 1 1 d R . . . .
O9W O 0.1884(14) 0.6797(15) 0.7539(7) 0.093(4) Uani 1 1 d . . . . .
H9WA H 0.2578 0.6838 0.7838 0.112 Uiso 1 1 d R . . . .
H9WB H 0.2427 0.6544 0.7145 0.112 Uiso 1 1 d R . . . .
O10W O 0.8953(13) 0.6746(12) 0.8374(6) 0.077(4) Uani 1 1 d . . . . .
H10A H 0.8536 0.5962 0.8248 0.092 Uiso 1 1 d R . . . .
H10B H 0.9697 0.6931 0.8053 0.092 Uiso 1 1 d R . . . .
N1 N 0.4008(13) 0.2403(12) 0.6150(5) 0.038(3) Uani 1 1 d . . . . .
N2 N 0.1395(13) 0.7334(13) 0.3862(5) 0.043(3) Uani 1 1 d . . . . .
C2 C 0.4807(16) -0.0092(16) 0.6729(8) 0.045(3) Uani 1 1 d . . . . .
H2 H 0.5433 -0.1135 0.6716 0.054 Uiso 1 1 calc R . . . .
C1 C 0.4895(16) 0.0927(16) 0.6155(8) 0.047(4) Uani 1 1 d . . . . .
H1 H 0.5590 0.0584 0.5756 0.056 Uiso 1 1 calc R . . . .
C9 C 0.0680(16) 0.8935(16) 0.3789(7) 0.045(3) Uani 1 1 d . . . . .
H9 H 0.0011 0.9427 0.4166 0.054 Uiso 1 1 calc R . . . .
C3 C 0.3802(14) 0.0370(14) 0.7345(7) 0.038(3) Uani 1 1 d . . . . .
H3 H 0.3782 -0.0321 0.7748 0.045 Uiso 1 1 calc R . . . .
C5 C 0.3004(15) 0.2899(16) 0.6726(7) 0.042(3) Uani 1 1 d . . . . .
H5 H 0.2407 0.3955 0.6713 0.051 Uiso 1 1 calc R . . . .
C4 C 0.2810(14) 0.1952(16) 0.7326(7) 0.039(3) Uani 1 1 d . . . . .
C13 C 0.2295(15) 0.6679(17) 0.3291(8) 0.047(4) Uani 1 1 d . . . . .
H13 H 0.2767 0.5584 0.3335 0.056 Uiso 1 1 calc R . . . .
C6 C 0.1625(15) 0.2524(15) 0.7923(7) 0.040(3) Uani 1 1 d . . . . .
H6 H 0.1323 0.3640 0.7972 0.048 Uiso 1 1 calc R . . . .
C10 C 0.0922(17) 0.9820(16) 0.3179(7) 0.046(3) Uani 1 1 d . . . . .
H10 H 0.0436 1.0913 0.3146 0.055 Uiso 1 1 calc R . . . .
C11 C 0.1890(16) 0.9115(16) 0.2602(7) 0.042(3) Uani 1 1 d . . . . .
H11 H 0.2076 0.9731 0.2186 0.050 Uiso 1 1 calc R . . . .
C17 C 0.4389(12) 0.0542(12) -0.0223(5) 0.021(2) Uani 1 1 d . 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
O5 Nd1 2.494(7) 2_655 ?
O5 C17 1.265(11) . ?
O6 Nd1 2.494(6) . ?
O6 C17 1.278(12) . ?
C12 C14 1.445(16) . ?
C12 C13 1.355(18) . ?
C12 C11 1.402(17) . ?
C14 H14 0.9300 . ?
C14 C15 1.356(16) . ?
C7 H7 0.9300 . ?
C7 C8 1.471(16) . ?
C7 C6 1.321(16) . ?
C8 Nd1 2.937(12) 1_456 ?
C8 O1 1.258(13) . ?
C8 O2 1.273(12) . ?
C15 H15 0.9300 . ?
C15 C16 1.484(16) . ?
C16 O3 1.266(13) . ?
C16 O4 1.258(13) . ?
Cu1 Cu1 2.793(3) 2_666 ?
Cu1 Cu2 2.814(3) . ?
Cu1 I1 2.6795(19) . ?
Cu1 I2 2.652(2) . ?
Cu1 I2 2.6559(19) 2_666 ?
Cu1 N1 2.087(10) . ?
Cu2 Cu2 2.778(3) 2_566 ?
Cu2 I1 2.6474(19) . ?
Cu2 I1 2.6279(19) 2_566 ?
Cu2 I2 2.6899(19) . ?
Cu2 N2 2.045(11) . ?
I1 Cu2 2.6279(19) 2_566 ?
I2 Cu1 2.6559(19) 2_666 ?
Nd1 O5 2.494(7) 2_655 ?
Nd1 C8 2.937(12) 1_654 ?
Nd1 O1 2.485(8) 1_654 ?
Nd1 O2 2.590(8) 1_654 ?
Nd1 O3 2.522(8) . ?
Nd1 O4 2.640(7) . ?
Nd1 O4 2.481(7) 2_665 ?
Nd1 O7W 2.444(7) . ?
Nd1 O8W 2.464(7) . ?
O1 Nd1 2.485(8) 1_456 ?
O2 Nd1 2.590(8) 1_456 ?
O4 Nd1 2.481(7) 2_665 ?
O7W H7WA 0.8499 . ?
O7W H7WB 0.8500 . ?
O8W H8WA 0.8496 . ?
O8W H8WB 0.8499 . ?
O9W H9WA 0.8497 . ?
O9W H9WB 0.8503 . ?
O10W H10A 0.8500 . ?
O10W H10B 0.8498 . ?
N1 C1 1.316(16) . ?
N1 C5 1.344(15) . ?
N2 C9 1.367(16) . ?
N2 C13 1.340(16) . ?
C2 H2 0.9300 . ?
C2 C1 1.345(19) . ?
C2 C3 1.398(18) . ?
C1 H1 0.9300 . ?
C9 H9 0.9300 . ?
C9 C10 1.352(19) . ?
C3 H3 0.9300 . ?
C3 C4 1.424(17) . ?
C5 H5 0.9300 . ?
C5 C4 1.358(18) . ?
C4 C6 1.466(17) . ?
C13 H13 0.9300 . ?
C6 H6 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.387(18) . ?
C11 H11 0.9300 . ?
C17 C17 1.514(19) 2_655 ?

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
C17 O5 Nd1 120.9(6) . 2_655 ?
C17 O6 Nd1 119.9(6) . . ?
C13 C12 C14 123.8(12) . . ?
C13 C12 C11 116.1(12) . . ?
C11 C12 C14 120.0(12) . . ?
C12 C14 H14 116.6 . . ?
C15 C14 C12 126.8(13) . . ?
C15 C14 H14 116.6 . . ?
C8 C7 H7 118.2 . . ?
C6 C7 H7 118.2 . . ?
C6 C7 C8 123.6(11) . . ?
C7 C8 Nd1 174.3(8) . 1_456 ?
O1 C8 C7 118.8(10) . . ?
O1 C8 Nd1 56.9(6) . 1_456 ?
O1 C8 O2 118.7(11) . . ?
O2 C8 C7 122.4(11) . . ?
O2 C8 Nd1 61.8(6) . 1_456 ?
C14 C15 H15 118.2 . . ?
C14 C15 C16 123.6(12) . . ?
C16 C15 H15 118.2 . . ?
O3 C16 C15 117.9(10) . . ?
O4 C16 C15 121.1(10) . . ?
O4 C16 O3 121.1(10) . . ?
Cu1 Cu1 Cu2 92.54(9) 2_666 . ?
I1 Cu1 Cu1 127.61(10) . 2_666 ?
I1 Cu1 Cu2 57.56(5) . . ?
I2 Cu1 Cu1 58.18(6) 2_666 2_666 ?
I2 Cu1 Cu1 58.32(6) . 2_666 ?
I2 Cu1 Cu2 124.24(8) 2_666 . ?
I2 Cu1 Cu2 58.88(5) . . ?
I2 Cu1 I1 116.31(7) . . ?
I2 Cu1 I1 101.49(6) 2_666 . ?
I2 Cu1 I2 116.50(7) . 2_666 ?
N1 Cu1 Cu1 127.5(3) . 2_666 ?
N1 Cu1 Cu2 124.4(3) . . ?
N1 Cu1 I1 104.5(3) . . ?
N1 Cu1 I2 110.3(3) . 2_666 ?
N1 Cu1 I2 107.1(3) . . ?
Cu2 Cu2 Cu1 97.00(9) 2_566 . ?
I1 Cu2 Cu1 130.75(8) 2_566 . ?
I1 Cu2 Cu1 58.67(5) . . ?
I1 Cu2 Cu2 57.88(6) . 2_566 ?
I1 Cu2 Cu2 58.57(6) 2_566 2_566 ?
I1 Cu2 I1 116.45(7) 2_566 . ?
I1 Cu2 I2 116.10(7) . . ?
I1 Cu2 I2 101.49(6) 2_566 . ?
I2 Cu2 Cu1 57.56(5) . . ?
I2 Cu2 Cu2 127.42(10) . 2_566 ?
N2 Cu2 Cu1 117.1(3) . . ?
N2 Cu2 Cu2 127.8(3) . 2_566 ?
N2 Cu2 I1 111.1(3) . 2_566 ?
N2 Cu2 I1 106.6(3) . . ?
N2 Cu2 I2 104.6(3) . . ?
Cu2 I1 Cu1 104.20(6) 2_566 . ?
Cu2 I1 Cu1 63.77(6) . . ?
Cu2 I1 Cu2 63.55(7) 2_566 . ?
Cu1 I2 Cu1 63.50(7) . 2_666 ?
Cu1 I2 Cu2 63.57(6) . . ?
Cu1 I2 Cu2 98.55(6) 2_666 . ?
O5 Nd1 O6 64.8(2) 2_655 . ?
O5 Nd1 C8 95.2(3) 2_655 1_654 ?
O5 Nd1 O2 120.3(3) 2_655 1_654 ?
O5 Nd1 O3 74.6(3) 2_655 . ?
O5 Nd1 O4 108.7(2) 2_655 . ?
O6 Nd1 C8 102.5(3) . 1_654 ?
O6 Nd1 O2 116.3(3) . 1_654 ?
O6 Nd1 O3 96.0(3) . . ?
O6 Nd1 O4 78.6(2) . . ?
O1 Nd1 O5 70.8(3) 1_654 2_655 ?
O1 Nd1 O6 86.7(3) 1_654 . ?
O1 Nd1 C8 25.1(3) 1_654 1_654 ?
O1 Nd1 O2 50.7(2) 1_654 1_654 ?
O1 Nd1 O3 140.2(2) 1_654 . ?
O1 Nd1 O4 163.4(2) 1_654 . ?
O2 Nd1 C8 25.7(3) 1_654 1_654 ?
O2 Nd1 O4 130.6(2) 1_654 . ?
O3 Nd1 C8 152.6(3) . 1_654 ?
O3 Nd1 O2 147.6(3) . 1_654 ?
O3 Nd1 O4 50.3(2) . . ?
O4 Nd1 O5 133.7(2) 2_665 2_655 ?
O4 Nd1 O6 69.3(2) 2_665 . ?
O4 Nd1 C8 89.2(3) 2_665 1_654 ?
O4 Nd1 C8 153.5(3) . 1_654 ?
O4 Nd1 O1 101.7(3) 2_665 1_654 ?
O4 Nd1 O2 75.7(2) 2_665 1_654 ?
O4 Nd1 O3 116.4(2) 2_665 . ?
O4 Nd1 O4 66.1(3) 2_665 . ?
O7W Nd1 O5 78.1(2) . 2_655 ?
O7W Nd1 O6 142.3(2) . . ?
O7W Nd1 C8 73.3(3) . 1_654 ?
O7W Nd1 O1 74.6(2) . 1_654 ?
O7W Nd1 O2 76.2(3) . 1_654 ?
O7W Nd1 O3 79.6(3) . . ?
O7W Nd1 O4 145.8(2) . 2_665 ?
O7W Nd1 O4 121.9(2) . . ?
O7W Nd1 O8W 73.4(2) . . ?
O8W Nd1 O5 143.1(3) . 2_655 ?
O8W Nd1 O6 142.7(2) . . ?
O8W Nd1 C8 98.6(3) . 1_654 ?
O8W Nd1 O1 121.8(3) . 1_654 ?
O8W Nd1 O2 75.0(3) . 1_654 ?
O8W Nd1 O3 77.5(3) . . ?
O8W Nd1 O4 80.7(2) . 2_665 ?
O8W Nd1 O4 69.1(2) . . ?
C8 O1 Nd1 98.0(7) . 1_456 ?
C8 O2 Nd1 92.6(7) . 1_456 ?
C16 O3 Nd1 96.5(7) . . ?
C16 O4 Nd1 154.4(7) . 2_665 ?
C16 O4 Nd1 91.1(6) . . ?
Nd1 O4 Nd1 113.9(3) 2_665 . ?
Nd1 O7W H7WA 125.6 . . ?
Nd1 O7W H7WB 125.3 . . ?
H7WA O7W H7WB 107.7 . . ?
Nd1 O8W H8WA 142.8 . . ?
Nd1 O8W H8WB 107.0 . . ?
H8WA O8W H8WB 107.7 . . ?
H9WA O9W H9WB 107.7 . . ?
H10A O10W H10B 107.7 . . ?
C1 N1 Cu1 120.4(9) . . ?
C1 N1 C5 119.7(12) . . ?
C5 N1 Cu1 119.6(9) . . ?
C9 N2 Cu2 121.7(9) . . ?
C13 N2 Cu2 121.9(9) . . ?
C13 N2 C9 116.4(12) . . ?
C1 C2 H2 119.0 . . ?
C1 C2 C3 121.9(12) . . ?
C3 C2 H2 119.0 . . ?
N1 C1 C2 120.7(12) . . ?
N1 C1 H1 119.7 . . ?
C2 C1 H1 119.7 . . ?
N2 C9 H9 119.2 . . ?
C10 C9 N2 121.5(12) . . ?
C10 C9 H9 119.2 . . ?
C2 C3 H3 121.6 . . ?
C2 C3 C4 116.8(12) . . ?
C4 C3 H3 121.6 . . ?
N1 C5 H5 118.0 . . ?
N1 C5 C4 123.9(12) . . ?
C4 C5 H5 118.0 . . ?
C3 C4 C6 121.5(12) . . ?
C5 C4 C3 116.8(12) . . ?
C5 C4 C6 121.6(12) . . ?
C12 C13 H13 116.8 . . ?
N2 C13 C12 126.4(13) . . ?
N2 C13 H13 116.8 . . ?
C7 C6 C4 124.0(12) . . ?
C7 C6 H6 118.0 . . ?
C4 C6 H6 118.0 . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.6(13) . . ?
C11 C10 H10 119.7 . . ?
C12 C11 H11 120.5 . . ?
C10 C11 C12 118.9(12) . . ?
C10 C11 H11 120.5 . . ?
O5 C17 O6 125.8(9) . . ?
O5 C17 C17 116.7(11) . 2_655 ?
O6 C17 C17 117.5(11) . 2_655 ?

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
C12 C14 C15 C16 175.8(11) . . . . ?
C14 C12 C13 N2 -175.7(11) . . . . ?
C14 C12 C11 C10 174.6(11) . . . . ?
C14 C15 C16 O3 150.2(11) . . . . ?
C14 C15 C16 O4 -29.8(17) . . . . ?
C7 C8 O1 Nd1 175.5(9) . . . 1_456 ?
C7 C8 O2 Nd1 -175.5(10) . . . 1_456 ?
C8 C7 C6 C4 -170.9(11) . . . . ?
C15 C16 O3 Nd1 -169.3(9) . . . . ?
C15 C16 O4 Nd1 169.8(9) . . . . ?
C15 C16 O4 Nd1 2(2) . . . 2_665 ?
Cu1 N1 C1 C2 -173.5(9) . . . . ?
Cu1 N1 C5 C4 172.4(10) . . . . ?
Cu2 N2 C9 C10 176.6(10) . . . . ?
Cu2 N2 C13 C12 -177.8(10) . . . . ?
Nd1 O5 C17 O6 -176.3(8) 2_655 . . . ?
Nd1 O5 C17 C17 3.6(15) 2_655 . . 2_655 ?
Nd1 O6 C17 O5 -176.4(8) . . . . ?
Nd1 O6 C17 C17 3.8(15) . . . 2_655 ?
O1 C8 O2 Nd1 2.0(11) . . . 1_456 ?
O2 C8 O1 Nd1 -2.1(11) . . . 1_456 ?
O3 C16 O4 Nd1 -177.9(10) . . . 2_665 ?
O3 C16 O4 Nd1 -10.2(11) . . . . ?
O4 C16 O3 Nd1 10.7(11) . . . . ?
N1 C5 C4 C3 3.1(19) . . . . ?
N1 C5 C4 C6 -176.4(11) . . . . ?
N2 C9 C10 C11 1(2) . . . . ?
C2 C3 C4 C5 -3.8(17) . . . . ?
C2 C3 C4 C6 175.7(11) . . . . ?
C1 N1 C5 C4 -1(2) . . . . ?
C1 C2 C3 C4 2.9(19) . . . . ?
C9 N2 C13 C12 1.2(19) . . . . ?
C9 C10 C11 C12 1.4(19) . . . . ?
C3 C2 C1 N1 -1(2) . . . . ?
C3 C4 C6 C7 -23.9(19) . . . . ?
C5 N1 C1 C2 0.1(19) . . . . ?
C5 C4 C6 C7 155.6(13) . . . . ?
C13 C12 C14 C15 5.4(19) . . . . ?
C13 C12 C11 C10 -2.5(17) . . . . ?
C13 N2 C9 C10 -2.4(18) . . . . ?
C6 C7 C8 O1 161.4(11) . . . . ?
C6 C7 C8 O2 -21.1(18) . . . . ?
C11 C12 C14 C15 -171.4(12) . . . . ?
C11 C12 C13 N2 1.2(19) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_16
_database_code_depnum_ccdc_archive 'CCDC 1445874'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H16 Br2 Cu2 Gd N2 O7, H2 O'
_chemical_formula_sum            'C17 H16 Br2 Cu2 Gd N2 O8'
_chemical_formula_weight         820.47
_chemical_melting_point          ?
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'
O O 0.0106 0.0060 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.4390(17)
_cell_length_b                   7.797(2)
_cell_length_c                   21.617(5)
_cell_angle_alpha                86.532(4)
_cell_angle_beta                 87.711(4)
_cell_angle_gamma                65.178(4)
_cell_volume                     1135.7(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    645
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.78
_cell_measurement_theta_min      3.02
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.305
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0820 before and 0.0447 after correction.
The Ratio of minimum to maximum transmission is 0.7465.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.399
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   0.190
_exptl_transmission_factor_min   0.149
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.1172
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            5970
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.395
_diffrn_reflns_theta_min         0.944
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2646
_reflns_number_total             4175
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker, 2000-2003)'
_refine_diff_density_max         1.991
_refine_diff_density_min         -2.157
_refine_diff_density_rms         0.253
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0667
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0737P)²+1.8919P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1738
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O7W(H7WA,H7WB), O8W(H8WA,H8WB)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C9(H9), C13(H13), C3(H3), C2(H2), C1(H1), C5(H5), C7(H7),
 C6(H6), C15(H15), C14(H14)
2.c Fitted hexagon refined as free rotating group:
 C12(C11,C10,C9,N2,C13)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Gd1 Gd 0.25463(10) 0.25959(9) 0.49025(3) 0.0286(2) Uani 1 1 d . . . A 1
O6 O 0.4930(13) 0.6924(12) 0.4536(4) 0.034(2) Uani 1 1 d . . . . .
O4 O 0.4467(13) -0.0447(12) 0.5552(4) 0.032(2) Uani 1 1 d . . . . .
C12 C 0.2887(14) -0.1842(12) 0.7641(3) 0.035(3) Uani 1 1 d . . . . .
C11 C 0.4653(12) -0.3430(13) 0.7743(4) 0.046(4) Uani 1 1 d G . . . .
H11 H 0.5549 -0.3909 0.7417 0.056 Uiso 1 1 calc R . . . .
C10 C 0.5080(11) -0.4301(11) 0.8333(4) 0.046(4) Uani 1 1 d G . . . .
H10 H 0.6261 -0.5363 0.8401 0.055 Uiso 1 1 calc R . . . .
C9 C 0.3741(14) -0.3585(12) 0.8819(3) 0.042(4) Uani 1 1 d G . . . .
H9 H 0.4026 -0.4168 0.9214 0.050 Uiso 1 1 calc R . . . .
N2 N 0.1975(12) -0.1997(12) 0.8717(3) 0.050(3) Uani 1 1 d G . . . .
C13 C 0.1548(11) -0.1126(11) 0.8127(4) 0.044(4) Uani 1 1 d G . . . .
H13 H 0.0366 -0.0064 0.8059 0.053 Uiso 1 1 calc R . . . .
C4 C -0.203(2) 0.638(2) 0.2273(6) 0.037(4) Uani 1 1 d . . . . .
C3 C -0.392(3) 0.774(2) 0.2309(7) 0.055(5) Uani 1 1 d . . . . .
H3 H -0.4611 0.7989 0.2685 0.066 Uiso 1 1 calc R . . . .
C2 C -0.481(2) 0.877(2) 0.1754(7) 0.048(4) Uani 1 1 d . . . . .
H2 H -0.6100 0.9715 0.1761 0.058 Uiso 1 1 calc R . . . .
C1 C -0.373(2) 0.834(2) 0.1195(8) 0.052(4) Uani 1 1 d . . . . .
H1 H -0.4304 0.9009 0.0831 0.062 Uiso 1 1 calc R . . . .
N1 N -0.185(2) 0.6984(19) 0.1177(6) 0.051(4) Uani 1 1 d . . . . .
C5 C -0.105(2) 0.601(2) 0.1711(6) 0.042(4) Uani 1 1 d . . . . .
H5 H 0.0215 0.5033 0.1696 0.051 Uiso 1 1 calc R . . . .
Br1 Br 0.2229(2) 0.7830(2) 0.04266(7) 0.0480(4) Uani 1 1 d . . . . .
Br2 Br 0.2192(3) 0.2843(2) 0.05322(8) 0.0493(5) Uani 1 1 d . . . . .
Cu1 Cu -0.0154(4) 0.6382(3) 0.03905(10) 0.0643(7) Uani 1 1 d . . . . .
Cu2 Cu -0.0008(4) 1.1094(3) 0.05662(10) 0.0672(7) Uani 1 1 d . . . . .
C8 C -0.013(2) 0.4338(19) 0.3912(6) 0.030(3) Uani 1 1 d . . . . .
O2 O -0.0750(14) 0.4733(12) 0.4478(4) 0.035(2) Uani 1 1 d . . . . .
O1 O 0.1591(14) 0.3180(13) 0.3794(4) 0.038(2) Uani 1 1 d . . . . .
C7 C -0.150(2) 0.540(2) 0.3410(6) 0.035(3) Uani 1 1 d . . . . .
H7 H -0.2808 0.6176 0.3509 0.042 Uiso 1 1 calc R . . . .
C6 C -0.091(2) 0.5261(19) 0.2823(6) 0.032(3) Uani 1 1 d . . . . .
H6 H 0.0356 0.4349 0.2743 0.039 Uiso 1 1 calc R . . . .
O3 O 0.1486(15) 0.1359(13) 0.5870(5) 0.047(3) Uani 1 1 d . . . . .
O5 O 0.3408(14) 0.5026(13) 0.4432(4) 0.037(2) Uani 1 1 d . . . . .
C15 C 0.355(2) -0.1250(19) 0.6537(6) 0.039(4) Uani 1 1 d . . . . .
H15 H 0.4689 -0.2376 0.6542 0.047 Uiso 1 1 calc R . . . .
C16 C 0.309(2) -0.0031(18) 0.5968(6) 0.030(3) Uani 1 1 d . . . . .
O7W O 0.1394(18) 0.0335(16) 0.4585(5) 0.065(4) Uani 1 1 d . . . . .
H7WA H 0.2398 -0.0724 0.4579 0.078 Uiso 1 1 d R . . A .
H7WB H 0.0483 0.0242 0.4383 0.078 Uiso 1 1 d R . . . .
C17 C 0.451(2) 0.5569(16) 0.4704(6) 0.027(3) Uani 1 1 d . . . . .
C14 C 0.243(2) -0.083(2) 0.7040(7) 0.043(4) Uani 1 1 d . . . . .
H14 H 0.1218 0.0227 0.7008 0.052 Uiso 1 1 calc R . . . .
O8W O 0.232(3) 0.791(5) 0.3383(12) 0.32(2) Uani 1 1 d . . . . .
H8WA H 0.3190 0.7158 0.3630 0.385 Uiso 1 1 d R . . . .
H8WB H 0.1196 0.7995 0.3517 0.385 Uiso 1 1 d R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O6 2.442(9) 2_666 ?
Gd1 O4 2.368(9) 2_656 ?
Gd1 O4 2.560(8) . ?
Gd1 O2 2.403(9) 2_566 ?
Gd1 O2 2.489(9) . ?
Gd1 O1 2.488(9) . ?
Gd1 O3 2.488(10) . ?
Gd1 O5 2.402(10) . ?
Gd1 O7W 2.403(10) . ?
O6 Gd1 2.442(9) 2_666 ?
O6 C17 1.251(14) . ?
O4 Gd1 2.368(9) 2_656 ?
O4 C16 1.283(15) . ?
C12 C11 1.3900 . ?
C12 C13 1.3900 . ?
C12 C14 1.455(15) . ?
C11 C10 1.3900 . ?
C10 C9 1.3900 . ?
C9 N2 1.3900 . ?
N2 C13 1.3900 . ?
N2 Cu2 2.031(6) 2_566 ?
C4 C3 1.36(2) . ?
C4 C5 1.374(19) . ?
C4 C6 1.486(18) . ?
C3 C2 1.42(2) . ?
C2 C1 1.40(2) . ?
C1 N1 1.353(19) . ?
N1 C5 1.355(17) . ?
N1 Cu1 2.032(13) . ?
Br1 Cu1 2.475(3) . ?
Br1 Cu2 2.416(3) . ?
Br1 Cu2 2.635(3) 2_575 ?
Br2 Cu1 2.443(3) 2_565 ?
Br2 Cu1 2.579(3) . ?
Br2 Cu2 2.528(3) 1_545 ?
Cu1 Br2 2.443(3) 2_565 ?
Cu1 Cu1 2.746(5) 2_565 ?
Cu1 Cu2 2.802(3) 2_575 ?
Cu2 N2 2.03(7) 2_566 ?
Cu2 Br1 2.635(3) 2_575 ?
Cu2 Br2 2.528(3) 1_565 ?
Cu2 Cu1 2.802(3) 2_575 ?
C8 O2 1.297(15) . ?
C8 O1 1.245(15) . ?
C8 C7 1.474(18) . ?
O2 Gd1 2.403(9) 2_566 ?
C7 C6 1.322(18) . ?
O3 C16 1.245(16) . ?
O5 C17 1.248(15) . ?
C15 C16 1.466(18) . ?
C15 C14 1.315(18) . ?
C17 C17 1.53(3) 2_666 ?

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
O6 Gd1 O4 72.5(3) 2_666 . ?
O6 Gd1 O2 134.4(3) 2_666 . ?
O6 Gd1 O1 131.9(3) 2_666 . ?
O6 Gd1 O3 90.9(3) 2_666 . ?
O4 Gd1 O6 77.3(3) 2_656 2_666 ?
O4 Gd1 O4 64.4(3) 2_656 . ?
O4 Gd1 O2 151.1(3) 2_656 2_566 ?
O4 Gd1 O2 133.4(3) 2_656 . ?
O4 Gd1 O1 80.5(3) 2_656 . ?
O4 Gd1 O3 114.8(3) 2_656 . ?
O4 Gd1 O5 85.6(3) 2_656 . ?
O4 Gd1 O7W 81.6(4) 2_656 . ?
O2 Gd1 O6 74.7(3) 2_566 2_666 ?
O2 Gd1 O4 145.0(3) . . ?
O2 Gd1 O4 113.0(3) 2_566 . ?
O2 Gd1 O2 66.6(4) 2_566 . ?
O2 Gd1 O1 113.3(3) 2_566 . ?
O2 Gd1 O3 73.2(3) 2_566 . ?
O1 Gd1 O4 132.2(3) . . ?
O1 Gd1 O2 53.0(3) . . ?
O3 Gd1 O4 51.1(3) . . ?
O3 Gd1 O2 99.9(3) . . ?
O3 Gd1 O1 137.2(4) . . ?
O5 Gd1 O6 66.5(3) . 2_666 ?
O5 Gd1 O4 133.4(3) . . ?
O5 Gd1 O2 76.6(3) . 2_566 ?
O5 Gd1 O2 81.5(3) . . ?
O5 Gd1 O1 69.7(3) . . ?
O5 Gd1 O3 146.2(3) . . ?
O5 Gd1 O7W 138.1(3) . . ?
O7W Gd1 O6 146.0(3) . 2_666 ?
O7W Gd1 O4 74.5(3) . . ?
O7W Gd1 O2 79.0(3) . . ?
O7W Gd1 O2 126.6(4) . 2_566 ?
O7W Gd1 O1 68.9(3) . . ?
O7W Gd1 O3 74.1(4) . . ?
C17 O6 Gd1 119.0(8) . 2_666 ?
Gd1 O4 Gd1 115.6(3) 2_656 . ?
C16 O4 Gd1 92.4(7) . . ?
C16 O4 Gd1 151.5(8) . 2_656 ?
C11 C12 C13 120.0 . . ?
C11 C12 C14 121.9(8) . . ?
C13 C12 C14 118.1(8) . . ?
C10 C11 C12 120.0 . . ?
C11 C10 C9 120.0 . . ?
N2 C9 C10 120.0 . . ?
C9 N2 Cu2 118.3(5) . 2_566 ?
C13 N2 C9 120.0 . . ?
C13 N2 Cu2 121.6(5) . 2_566 ?
N2 C13 C12 120.0 . . ?
C3 C4 C5 120.1(14) . . ?
C3 C4 C6 123.2(13) . . ?
C5 C4 C6 116.6(13) . . ?
C4 C3 C2 118.2(15) . . ?
C1 C2 C3 119.0(15) . . ?
N1 C1 C2 121.3(15) . . ?
C1 N1 C5 118.4(14) . . ?
C1 N1 Cu1 123.2(11) . . ?
C5 N1 Cu1 118.5(11) . . ?
N1 C5 C4 123.0(14) . . ?
Cu1 Br1 Cu2 66.43(8) . 2_575 ?
Cu2 Br1 Cu1 100.61(11) . . ?
Cu2 Br1 Cu2 74.56(10) . 2_575 ?
Cu1 Br2 Cu1 66.23(10) 2_565 . ?
Cu1 Br2 Cu2 68.58(9) 2_565 1_545 ?
Cu2 Br2 Cu1 105.78(10) 1_545 . ?
N1 Cu1 Br1 108.4(4) . . ?
N1 Cu1 Br2 111.4(4) . 2_565 ?
N1 Cu1 Br2 104.9(4) . . ?
N1 Cu1 Cu1 124.4(4) . 2_565 ?
N1 Cu1 Cu2 128.0(4) . 2_575 ?
Br1 Cu1 Br2 100.74(10) . . ?
Br1 Cu1 Cu1 125.00(14) . 2_565 ?
Br1 Cu1 Cu2 59.52(8) . 2_575 ?
Br2 Cu1 Br1 116.61(10) 2_565 . ?
Br2 Cu1 Br2 113.77(10) 2_565 . ?
Br2 Cu1 Cu1 54.51(9) . 2_565 ?
Br2 Cu1 Cu1 59.26(9) 2_565 2_565 ?
Br2 Cu1 Cu2 126.65(11) . 2_575 ?
Br2 Cu1 Cu2 57.15(8) 2_565 2_575 ?
Cu1 Cu1 Cu2 94.47(12) 2_565 2_575 ?
N2 Cu2 Br1 124.4(15) 2_566 . ?
N2 Cu2 Br1 104(2) 2_566 2_575 ?
N2 Cu2 Br2 109(3) 2_566 1_565 ?
N2 Cu2 Cu1 121.2(14) 2_566 2_575 ?
Br1 Cu2 Br1 105.44(10) . 2_575 ?
Br1 Cu2 Br2 104.78(11) . 1_565 ?
Br1 Cu2 Cu1 54.05(8) 2_575 2_575 ?
Br1 Cu2 Cu1 114.39(10) . 2_575 ?
Br2 Cu2 Br1 108.27(10) 1_565 2_575 ?
Br2 Cu2 Cu1 54.27(8) 1_565 2_575 ?
O2 C8 C7 117.5(12) . . ?
O1 C8 O2 121.6(12) . . ?
O1 C8 C7 120.8(12) . . ?
Gd1 O2 Gd1 113.4(4) 2_566 . ?
C8 O2 Gd1 92.0(7) . . ?
C8 O2 Gd1 140.6(8) . 2_566 ?
C8 O1 Gd1 93.4(7) . . ?
C6 C7 C8 121.6(13) . . ?
C7 C6 C4 128.1(13) . . ?
C16 O3 Gd1 96.8(8) . . ?
C17 O5 Gd1 120.4(8) . . ?
C14 C15 C16 123.1(13) . . ?
O4 C16 C15 116.4(12) . . ?
O3 C16 O4 119.0(12) . . ?
O3 C16 C15 124.6(13) . . ?
O6 C17 C17 116.6(15) . 2_666 ?
O5 C17 O6 126.7(12) . . ?
O5 C17 C17 116.7(14) . 2_666 ?
C15 C14 C12 126.4(13) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT973_16                  
;
PROBLEM:  
RESPONSE: The diffractions were collected at room temperature.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_17
_database_code_depnum_ccdc_archive 'CCDC 1445875'
_audit_update_record             
;
2016-06-02 deposited with the CCDC.
2016-06-06 downloaded from the CCDC.
;
_audit_creation_date             2016-05-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C17 H16 Br2 Cu2 N2 O7 Tb, O'
_chemical_formula_sum            'C17 H16 Br2 Cu2 N2 O8 Tb'
_chemical_formula_weight         822.15
_chemical_melting_point          ?
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'
O O 0.0106 0.0060 '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'
Cu Cu 0.3201 1.2651 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.4069(15)
_cell_length_b                   7.7788(15)
_cell_length_c                   21.614(4)
_cell_angle_alpha                86.456(3)
_cell_angle_beta                 87.677(4)
_cell_angle_gamma                65.171(3)
_cell_volume                     1127.9(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5396
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.904
_cell_measurement_theta_min      1.888
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.558
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker, 2005)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   0.181
_exptl_transmission_factor_min   0.140
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.1041
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6718
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.904
_diffrn_reflns_theta_min         1.888
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3219
_reflns_number_total             5396
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.594
_refine_diff_density_min         -1.489
_refine_diff_density_rms         0.229
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4849
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0585
_refine_ls_restrained_S_all      0.946
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0606P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1387
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H,H) groups
2. Restrained distances
 O1W-H1W = O1W-H1WA = O1W-H1WB
 0.82 with sigma of 0.01
 H1W-H1WA = H1W-H1WB
 1.39 with sigma of 0.01
 H1W-Tb1 \\sim H1WA-Tb1 \\sim H1WB-Tb1
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O2W \\sim O2B: within 3.8A with sigma of 0.02 and sigma for terminal atoms of
0.04
4. Others
 Sof(O2B)=1-FVAR(1)
 Sof(O2W)=FVAR(1)
 Fixed Sof: H1WA(0.5) H1WB(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.25481(7) 0.26003(7) 0.49043(2) 0.02662(16) Uani 1 1 d D . . . .
Cu1 Cu 0.9996(3) 0.1099(2) 0.05652(7) 0.0621(5) Uani 1 1 d . . . . .
Cu2 Cu 0.9843(3) 0.6377(2) 0.03902(7) 0.0592(5) Uani 1 1 d . . . . .
Br1 Br 1.22064(18) 0.28421(16) 0.05323(5) 0.0454(3) Uani 1 1 d . . . . .
Br2 Br 1.22455(18) 0.78266(16) 0.04229(6) 0.0460(3) Uani 1 1 d . . . . .
O1 O 0.5513(10) 0.0479(9) 0.4449(3) 0.0298(16) Uani 1 1 d . . . . .
O2 O 0.8508(11) -0.1382(10) 0.4120(3) 0.0412(18) Uani 1 1 d . . . . .
O3 O 0.9286(10) 0.4719(9) 0.4480(3) 0.0316(16) Uani 1 1 d . . . . .
O4 O 1.1588(10) 0.3138(10) 0.3798(3) 0.0340(16) Uani 1 1 d . . . . .
O5 O 0.3381(11) 0.5058(10) 0.4435(3) 0.0388(18) Uani 1 1 d . . . . .
O6 O 0.4956(9) 0.6916(9) 0.4533(3) 0.0327(16) Uani 1 1 d . . . . .
O1W O 0.1408(13) 0.0304(13) 0.4591(4) 0.058(2) Uani 1 1 d D . . . .
H1W H 0.189(11) -0.023(16) 0.427(3) 0.087 Uiso 1 1 d DR . . . .
H1WA H 0.023(5) 0.054(13) 0.466(5) 0.087 Uiso 0.5 1 d DR . P A 1
H1WB H 0.023(5) 0.054(13) 0.466(5) 0.087 Uiso 0.5 1 d DR . P B 2
N1 N 0.8060(14) 0.1969(13) 0.1279(4) 0.043(2) Uani 1 1 d . . . . .
N2 N 0.8159(14) 0.6945(13) 0.1169(4) 0.043(2) Uani 1 1 d . . . . .
C1 C 0.8389(17) 0.1175(16) 0.1856(5) 0.046(3) Uani 1 1 d . . . . .
H1 H 0.9559 0.0095 0.1928 0.056 Uiso 1 1 calc R . . . .
C2 C 0.7097(15) 0.1866(14) 0.2347(5) 0.033(2) Uani 1 1 d . . . . .
C3 C 0.5335(16) 0.3442(15) 0.2240(5) 0.042(3) Uani 1 1 d . . . . .
H3 H 0.4419 0.3935 0.2561 0.050 Uiso 1 1 calc R . . . .
C4 C 0.4954(18) 0.4279(16) 0.1647(5) 0.050(3) Uani 1 1 d . . . . .
H4 H 0.3781 0.5348 0.1565 0.059 Uiso 1 1 calc R . . . .
C5 C 0.6327(17) 0.3512(16) 0.1181(5) 0.044(3) Uani 1 1 d . . . . .
H5 H 0.6056 0.4076 0.0784 0.053 Uiso 1 1 calc R . . . .
C6 C 0.7607(17) 0.0847(15) 0.2958(5) 0.039(3) Uani 1 1 d . . . . .
H6 H 0.8853 -0.0163 0.2996 0.047 Uiso 1 1 calc R . . . .
C7 C 0.6455(17) 0.1249(15) 0.3447(4) 0.041(3) Uani 1 1 d . . . . .
H7 H 0.5274 0.2343 0.3429 0.049 Uiso 1 1 calc R . . . .
C8 C 0.6910(15) 0.0077(14) 0.4027(5) 0.031(2) Uani 1 1 d . . . . .
C9 C 0.8959(16) 0.6012(15) 0.1707(5) 0.039(3) Uani 1 1 d . . . . .
H9 H 1.0248 0.5063 0.1696 0.047 Uiso 1 1 calc R . . . .
C10 C 0.7959(16) 0.6393(15) 0.2279(5) 0.036(2) Uani 1 1 d . . . . .
C11 C 0.6076(18) 0.7772(17) 0.2289(5) 0.048(3) Uani 1 1 d . . . . .
H11 H 0.5363 0.8057 0.2662 0.058 Uiso 1 1 calc R . . . .
C12 C 0.5232(18) 0.8737(17) 0.1755(5) 0.050(3) Uani 1 1 d . . . . .
H12 H 0.3933 0.9668 0.1757 0.060 Uiso 1 1 calc R . . . .
C13 C 0.6323(17) 0.8321(16) 0.1211(5) 0.045(3) Uani 1 1 d . . . . .
H13 H 0.5750 0.9036 0.0852 0.055 Uiso 1 1 calc R . . . .
C14 C 0.9084(16) 0.5305(15) 0.2824(5) 0.039(3) Uani 1 1 d . . . . .
H14 H 1.0376 0.4423 0.2746 0.047 Uiso 1 1 calc R . . . .
C15 C 0.8492(15) 0.5425(14) 0.3407(5) 0.035(2) Uani 1 1 d . . . . .
H15 H 0.7179 0.6205 0.3508 0.042 Uiso 1 1 calc R . . . .
C16 C 0.9889(14) 0.4330(14) 0.3908(4) 0.030(2) Uani 1 1 d . . . . .
C17 C 0.4513(15) 0.5563(14) 0.4697(4) 0.030(2) Uani 1 1 d . . . . .
O2W O 0.225(4) 0.737(4) 0.3311(13) 0.115(10) Uiso 0.53(3) 1 d . U P C 1
O2B O 0.230(5) 0.857(6) 0.3504(16) 0.136(12) Uiso 0.47(3) 1 d . U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.344(7) . ?
Tb1 O1 2.571(6) 2_656 ?
Tb1 O2 2.490(7) 2_656 ?
Tb1 O3 2.405(7) 2_666 ?
Tb1 O3 2.459(6) 1_455 ?
Tb1 O4 2.483(7) 1_455 ?
Tb1 O5 2.401(7) . ?
Tb1 O6 2.420(7) 2_666 ?
Tb1 O1W 2.414(8) . ?
Tb1 C8 2.934(10) 2_656 ?
Tb1 C16 2.844(10) 1_455 ?
Cu1 Cu2 2.794(2) 2_765 ?
Cu1 Br1 2.523(2) . ?
Cu1 Br2 2.417(2) 1_545 ?
Cu1 Br2 2.630(2) 2_765 ?
Cu1 N1 2.007(9) . ?
Cu2 Cu1 2.794(2) 2_765 ?
Cu2 Cu2 2.735(3) 2_765 ?
Cu2 Br1 2.572(2) . ?
Cu2 Br1 2.4433(19) 2_765 ?
Cu2 Br2 2.480(2) . ?
Cu2 N2 2.011(9) . ?
Br1 Cu2 2.4432(19) 2_765 ?
Br2 Cu1 2.417(2) 1_565 ?
Br2 Cu1 2.630(2) 2_765 ?
O1 Tb1 2.571(6) 2_656 ?
O1 C8 1.299(11) . ?
O2 Tb1 2.490(7) 2_656 ?
O2 C8 1.262(11) . ?
O3 Tb1 2.405(7) 2_666 ?
O3 Tb1 2.459(6) 1_655 ?
O3 C16 1.307(11) . ?
O4 Tb1 2.483(7) 1_655 ?
O4 C16 1.234(11) . ?
O5 C17 1.234(12) . ?
O6 Tb1 2.420(7) 2_666 ?
O6 C17 1.255(11) . ?
O1W H1W 0.819(10) . ?
O1W H1WA 0.820(10) . ?
O1W H1WB 0.820(10) . ?
N1 C1 1.342(14) . ?
N1 C5 1.352(14) . ?
N2 C9 1.349(13) . ?
N2 C13 1.335(14) . ?
C1 H1 0.9300 . ?
C1 C2 1.373(14) . ?
C2 C3 1.381(14) . ?
C2 C6 1.475(14) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(14) . ?
C4 H4 0.9300 . ?
C4 C5 1.373(15) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C6 C7 1.300(14) . ?
C7 H7 0.9300 . ?
C7 C8 1.466(13) . ?
C8 Tb1 2.934(10) 2_656 ?
C9 H9 0.9300 . ?
C9 C10 1.398(14) . ?
C10 C11 1.357(15) . ?
C10 C14 1.470(14) . ?
C11 H11 0.9300 . ?
C11 C12 1.358(14) . ?
C12 H12 0.9300 . ?
C12 C13 1.376(15) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C14 C15 1.313(13) . ?
C15 H15 0.9300 . ?
C15 C16 1.485(13) . ?
C16 Tb1 2.844(10) 1_655 ?
C17 C17 1.55(2) 2_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O1 64.5(2) . 2_656 ?
O1 Tb1 O2 115.4(2) . 2_656 ?
O1 Tb1 O3 151.6(2) . 2_666 ?
O1 Tb1 O3 132.9(2) . 1_455 ?
O1 Tb1 O4 80.0(2) . 1_455 ?
O1 Tb1 O5 85.9(2) . . ?
O1 Tb1 O6 77.8(2) . 2_666 ?
O1 Tb1 O1W 81.4(3) . . ?
O1 Tb1 C8 90.6(2) . 2_656 ?
O1 Tb1 C8 26.3(2) 2_656 2_656 ?
O1 Tb1 C16 146.1(2) 2_656 1_455 ?
O1 Tb1 C16 105.6(2) . 1_455 ?
O2 Tb1 O1 51.4(2) 2_656 2_656 ?
O2 Tb1 C8 25.2(2) 2_656 2_656 ?
O2 Tb1 C16 121.8(3) 2_656 1_455 ?
O3 Tb1 O1 113.6(2) 2_666 2_656 ?
O3 Tb1 O1 145.1(2) 1_455 2_656 ?
O3 Tb1 O2 72.6(2) 2_666 2_656 ?
O3 Tb1 O2 100.3(2) 1_455 2_656 ?
O3 Tb1 O3 66.3(2) 2_666 1_455 ?
O3 Tb1 O4 113.6(2) 2_666 1_455 ?
O3 Tb1 O4 52.9(2) 1_455 1_455 ?
O3 Tb1 O6 74.9(2) 2_666 2_666 ?
O3 Tb1 O1W 126.4(3) 2_666 . ?
O3 Tb1 C8 123.8(2) 1_455 2_656 ?
O3 Tb1 C8 92.0(2) 2_666 2_656 ?
O3 Tb1 C16 90.3(3) 2_666 1_455 ?
O3 Tb1 C16 27.3(2) 1_455 1_455 ?
O4 Tb1 O1 131.0(2) 1_455 2_656 ?
O4 Tb1 O2 137.1(2) 1_455 2_656 ?
O4 Tb1 C8 141.8(3) 1_455 2_656 ?
O4 Tb1 C16 25.7(2) 1_455 1_455 ?
O5 Tb1 O1 134.0(2) . 2_656 ?
O5 Tb1 O2 145.3(2) . 2_656 ?
O5 Tb1 O3 80.8(2) . 1_455 ?
O5 Tb1 O3 76.4(2) . 2_666 ?
O5 Tb1 O4 70.5(2) . 1_455 ?
O5 Tb1 O6 66.9(2) . 2_666 ?
O5 Tb1 O1W 138.5(3) . . ?
O5 Tb1 C8 146.1(3) . 2_656 ?
O5 Tb1 C16 73.0(3) . 1_455 ?
O6 Tb1 O1 72.7(2) 2_666 2_656 ?
O6 Tb1 O2 90.0(2) 2_666 2_656 ?
O6 Tb1 O3 134.2(2) 2_666 1_455 ?
O6 Tb1 O4 132.9(2) 2_666 1_455 ?
O6 Tb1 C8 79.4(3) 2_666 2_656 ?
O6 Tb1 C16 139.4(2) 2_666 1_455 ?
O1W Tb1 O1 73.6(3) . 2_656 ?
O1W Tb1 O2 74.5(3) . 2_656 ?
O1W Tb1 O3 79.5(3) . 1_455 ?
O1W Tb1 O4 68.4(3) . 1_455 ?
O1W Tb1 O6 145.6(3) . 2_666 ?
O1W Tb1 C8 73.6(3) . 2_656 ?
O1W Tb1 C16 72.8(3) . 1_455 ?
C16 Tb1 C8 139.7(3) 1_455 2_656 ?
Br1 Cu1 Cu2 54.41(5) . 2_765 ?
Br1 Cu1 Br2 108.66(7) . 2_765 ?
Br2 Cu1 Cu2 114.22(7) 1_545 2_765 ?
Br2 Cu1 Cu2 54.31(5) 2_765 2_765 ?
Br2 Cu1 Br1 104.65(8) 1_545 . ?
Br2 Cu1 Br2 105.33(7) 1_545 2_765 ?
N1 Cu1 Cu2 121.7(3) . 2_765 ?
N1 Cu1 Br1 109.1(3) . . ?
N1 Cu1 Br2 124.0(3) . 1_545 ?
N1 Cu1 Br2 104.4(3) . 2_765 ?
Cu2 Cu2 Cu1 94.28(8) 2_765 2_765 ?
Br1 Cu2 Cu1 57.13(6) 2_765 2_765 ?
Br1 Cu2 Cu1 126.50(8) . 2_765 ?
Br1 Cu2 Cu2 59.24(6) 2_765 2_765 ?
Br1 Cu2 Cu2 54.71(6) . 2_765 ?
Br1 Cu2 Br1 113.95(7) 2_765 . ?
Br1 Cu2 Br2 116.53(7) 2_765 . ?
Br2 Cu2 Cu1 59.46(6) . 2_765 ?
Br2 Cu2 Cu2 124.68(10) . 2_765 ?
Br2 Cu2 Br1 100.41(7) . . ?
N2 Cu2 Cu1 128.6(3) . 2_765 ?
N2 Cu2 Cu2 124.0(3) . 2_765 ?
N2 Cu2 Br1 104.4(3) . . ?
N2 Cu2 Br1 111.3(3) . 2_765 ?
N2 Cu2 Br2 109.0(3) . . ?
Cu1 Br1 Cu2 105.40(7) . . ?
Cu2 Br1 Cu1 68.45(6) 2_765 . ?
Cu2 Br1 Cu2 66.05(7) 2_765 . ?
Cu1 Br2 Cu1 74.67(7) 1_565 2_765 ?
Cu1 Br2 Cu2 100.48(8) 1_565 . ?
Cu2 Br2 Cu1 66.23(6) . 2_765 ?
Tb1 O1 Tb1 115.5(2) . 2_656 ?
C8 O1 Tb1 92.6(6) . 2_656 ?
C8 O1 Tb1 151.3(6) . . ?
C8 O2 Tb1 97.5(6) . 2_656 ?
Tb1 O3 Tb1 113.7(2) 2_666 1_655 ?
C16 O3 Tb1 93.0(6) . 1_655 ?
C16 O3 Tb1 140.1(6) . 2_666 ?
C16 O4 Tb1 93.7(6) . 1_655 ?
C17 O5 Tb1 120.2(7) . . ?
C17 O6 Tb1 119.6(6) . 2_666 ?
Tb1 O1W H1W 117(4) . . ?
Tb1 O1W H1WA 117(4) . . ?
Tb1 O1W H1WB 117(4) . . ?
H1W O1W H1WA 116(2) . . ?
H1W O1W H1WB 116(2) . . ?
C1 N1 Cu1 124.7(8) . . ?
C1 N1 C5 117.1(10) . . ?
C5 N1 Cu1 118.1(7) . . ?
C9 N2 Cu2 119.2(8) . . ?
C13 N2 Cu2 124.6(7) . . ?
C13 N2 C9 115.9(9) . . ?
N1 C1 H1 118.1 . . ?
N1 C1 C2 123.8(10) . . ?
C2 C1 H1 118.1 . . ?
C1 C2 C3 118.4(10) . . ?
C1 C2 C6 118.8(9) . . ?
C3 C2 C6 122.8(9) . . ?
C2 C3 H3 120.6 . . ?
C2 C3 C4 118.9(10) . . ?
C4 C3 H3 120.6 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.3(11) . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 122.5(10) . . ?
N1 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
C2 C6 H6 117.4 . . ?
C7 C6 C2 125.2(10) . . ?
C7 C6 H6 117.4 . . ?
C6 C7 H7 118.1 . . ?
C6 C7 C8 123.8(10) . . ?
C8 C7 H7 118.1 . . ?
O1 C8 Tb1 61.1(5) . 2_656 ?
O1 C8 C7 117.6(9) . . ?
O2 C8 Tb1 57.3(5) . 2_656 ?
O2 C8 O1 118.2(9) . . ?
O2 C8 C7 124.0(9) . . ?
C7 C8 Tb1 170.2(8) . 2_656 ?
N2 C9 H9 118.2 . . ?
N2 C9 C10 123.6(10) . . ?
C10 C9 H9 118.2 . . ?
C9 C10 C14 116.6(10) . . ?
C11 C10 C9 117.7(10) . . ?
C11 C10 C14 125.7(10) . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.0(11) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 120.4 . . ?
C11 C12 C13 119.2(11) . . ?
C13 C12 H12 120.4 . . ?
N2 C13 C12 123.5(10) . . ?
N2 C13 H13 118.2 . . ?
C12 C13 H13 118.2 . . ?
C10 C14 H14 116.0 . . ?
C15 C14 C10 128.1(10) . . ?
C15 C14 H14 116.0 . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.9(9) . . ?
C16 C15 H15 119.6 . . ?
O3 C16 Tb1 59.7(5) . 1_655 ?
O3 C16 C15 117.5(9) . . ?
O4 C16 Tb1 60.6(5) . 1_655 ?
O4 C16 O3 120.2(9) . . ?
O4 C16 C15 122.2(9) . . ?
C15 C16 Tb1 174.0(7) . 1_655 ?
O5 C17 O6 127.2(10) . . ?
O5 C17 C17 117.2(11) . 2_666 ?
O6 C17 C17 115.5(11) . 2_666 ?

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
Tb1 O1 C8 Tb1 169.1(14) . . . 2_656 ?
Tb1 O1 C8 O2 163.7(8) . . . . ?
Tb1 O1 C8 O2 -5.3(10) 2_656 . . . ?
Tb1 O1 C8 C7 -21.9(19) . . . . ?
Tb1 O1 C8 C7 169.0(8) 2_656 . . . ?
Tb1 O2 C8 O1 5.6(10) 2_656 . . . ?
Tb1 O2 C8 C7 -168.4(9) 2_656 . . . ?
Tb1 O3 C16 Tb1 133.7(9) 2_666 . . 1_655 ?
Tb1 O3 C16 O4 137.4(8) 2_666 . . . ?
Tb1 O3 C16 O4 3.7(10) 1_655 . . . ?
Tb1 O3 C16 C15 -174.0(8) 1_655 . . . ?
Tb1 O3 C16 C15 -40.3(14) 2_666 . . . ?
Tb1 O4 C16 O3 -3.6(9) 1_655 . . . ?
Tb1 O4 C16 C15 173.9(9) 1_655 . . . ?
Tb1 O5 C17 O6 -174.0(7) . . . . ?
Tb1 O5 C17 C17 5.0(14) . . . 2_666 ?
Tb1 O6 C17 O5 -174.7(8) 2_666 . . . ?
Tb1 O6 C17 C17 6.2(13) 2_666 . . 2_666 ?
Cu1 N1 C1 C2 175.7(8) . . . . ?
Cu1 N1 C5 C4 -176.4(9) . . . . ?
Cu2 N2 C9 C10 175.5(8) . . . . ?
Cu2 N2 C13 C12 -177.0(9) . . . . ?
N1 C1 C2 C3 1.5(17) . . . . ?
N1 C1 C2 C6 178.9(10) . . . . ?
N2 C9 C10 C11 0.4(16) . . . . ?
N2 C9 C10 C14 -177.2(10) . . . . ?
C1 N1 C5 C4 1.0(17) . . . . ?
C1 C2 C3 C4 -0.9(17) . . . . ?
C1 C2 C6 C7 -174.1(11) . . . . ?
C2 C3 C4 C5 0.5(18) . . . . ?
C2 C6 C7 C8 172.6(10) . . . . ?
C3 C2 C6 C7 3.2(18) . . . . ?
C3 C4 C5 N1 -0.5(18) . . . . ?
C5 N1 C1 C2 -1.5(17) . . . . ?
C6 C2 C3 C4 -178.2(11) . . . . ?
C6 C7 C8 O1 -170.2(11) . . . . ?
C6 C7 C8 O2 3.8(18) . . . . ?
C9 N2 C13 C12 -3.2(17) . . . . ?
C9 C10 C11 C12 -0.5(17) . . . . ?
C9 C10 C14 C15 178.8(11) . . . . ?
C10 C11 C12 C13 -1.2(19) . . . . ?
C10 C14 C15 C16 -174.6(10) . . . . ?
C11 C10 C14 C15 1.5(19) . . . . ?
C11 C12 C13 N2 3.2(19) . . . . ?
C13 N2 C9 C10 1.4(16) . . . . ?
C14 C10 C11 C12 176.9(11) . . . . ?
C14 C15 C16 O3 170.4(10) . . . . ?
C14 C15 C16 O4 -7.2(16) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
