# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_aaa
_database_code_depnum_ccdc_archive 'CCDC 1856173'
_audit_update_record             
;
2018-07-15 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;
_audit_creation_date             2015-12-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C30 H20 Cl6 Dy N3 O4'
_chemical_formula_sum            'C30 H20 Cl6 Dy N3 O4'
_chemical_formula_weight         861.69
_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'
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'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.994(8)
_cell_length_b                   10.646(3)
_cell_length_c                   23.517(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.288(5)
_cell_angle_gamma                90.00
_cell_volume                     6331(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4072
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.46
_cell_measurement_theta_min      2.47
_exptl_absorpt_coefficient_mu    2.908
_exptl_absorpt_correction_T_max  0.6226
_exptl_absorpt_correction_T_min  0.5671
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3368
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17782
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.61
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                4438
_reflns_number_total             6306
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6306
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0379
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0538P)²+6.4215P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1096
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C13(H13), C14(H14), C18(H18), C23(H23), C24(H24),
 C28(H28)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Dy1 Dy 0.064595(11) 0.12055(3) 0.478746(12) 0.03466(11) Uani 1 d . . .
Cl1 Cl 0.23604(9) 0.1983(3) 0.83169(9) 0.1122(10) Uani 1 d . . .
Cl2 Cl 0.14169(8) -0.1910(2) 0.67268(10) 0.0764(6) Uani 1 d . . .
Cl3 Cl 0.27276(10) 0.2124(3) 0.38979(14) 0.1202(12) Uani 1 d . . .
Cl4 Cl 0.12045(9) 0.4979(2) 0.38940(12) 0.0851(7) Uani 1 d . . .
Cl5 Cl 0.01652(8) -0.33978(16) 0.40151(9) 0.0621(5) Uani 1 d . . .
Cl6 Cl -0.11053(8) -0.1709(2) 0.15857(8) 0.0757(6) Uani 1 d . . .
O1 O 0.08973(17) 0.0060(4) 0.56924(18) 0.0490(11) Uani 1 d . . .
O2 O 0.09927(16) 0.2725(4) 0.4481(2) 0.0474(11) Uani 1 d . . .
O3 O 0.03456(16) -0.0689(4) 0.43706(17) 0.0424(10) Uani 1 d . . .
O4 O -0.01524(15) 0.1792(4) 0.47307(19) 0.0434(10) Uani 1 d . . .
H4A H -0.0259 0.2488 0.4524 0.065 Uiso 1 d . . GR
H4B H -0.0106 0.1883 0.5117 0.065 Uiso 1 d . . GR
N1 N 0.1027(2) 0.2545(5) 0.5850(2) 0.0428(12) Uani 1 d . . .
N2 N 0.15062(19) 0.0546(5) 0.4772(2) 0.0411(12) Uani 1 d . . .
N3 N -0.00616(19) 0.1265(4) 0.3545(2) 0.0378(11) Uani 1 d . . .
C1 C 0.0777(3) 0.4616(7) 0.5344(4) 0.068(2) Uani 1 d . . .
H1A H 0.1012 0.4888 0.5191 0.101 Uiso 1 calc . . GR
H1B H 0.0641 0.5335 0.5461 0.101 Uiso 1 calc . . GR
H1C H 0.0489 0.4154 0.5006 0.101 Uiso 1 calc . . GR
C2 C 0.1070(3) 0.3791(7) 0.5929(4) 0.0573(18) Uani 1 d . . .
C3 C 0.1387(3) 0.4330(8) 0.6564(4) 0.073(2) Uani 1 d . . .
H3 H 0.1397 0.5198 0.6612 0.087 Uiso 1 calc . . R
C4 C 0.1674(3) 0.3594(8) 0.7100(4) 0.069(2) Uani 1 d . . .
H4 H 0.1891 0.3960 0.7503 0.083 Uiso 1 calc . . R
C5 C 0.1640(3) 0.2300(8) 0.7038(3) 0.0542(19) Uani 1 d . . .
C6 C 0.1301(2) 0.1793(7) 0.6401(3) 0.0440(15) Uani 1 d . . .
C7 C 0.1920(3) 0.1425(9) 0.7544(3) 0.066(2) Uani 1 d . . .
C8 C 0.1845(3) 0.0163(9) 0.7450(3) 0.066(2) Uani 1 d . . .
H8 H 0.2027 -0.0390 0.7796 0.079 Uiso 1 calc . . R
C9 C 0.1491(3) -0.0293(7) 0.6826(3) 0.0534(18) Uani 1 d . . .
C10 C 0.1225(2) 0.0488(7) 0.6296(3) 0.0449(16) Uani 1 d . . .
C11 C 0.1590(4) -0.1567(8) 0.5197(4) 0.088(3) Uani 1 d . . .
H11A H 0.1548 -0.1280 0.5557 0.132 Uiso 1 calc . . GR
H11B H 0.1844 -0.2236 0.5340 0.132 Uiso 1 calc . . GR
H11C H 0.1256 -0.1865 0.4855 0.132 Uiso 1 calc . . GR
C12 C 0.1777(3) -0.0512(7) 0.4949(3) 0.0576(19) Uani 1 d . . .
C13 C 0.2223(3) -0.0717(10) 0.4881(5) 0.099(4) Uani 1 d . . .
H13 H 0.2414 -0.1459 0.5034 0.119 Uiso 1 calc . . R
C14 C 0.2386(3) 0.0202(10) 0.4580(5) 0.086(3) Uani 1 d . . .
H14 H 0.2676 0.0058 0.4522 0.103 Uiso 1 calc . . R
C15 C 0.2102(3) 0.1336(8) 0.4371(4) 0.065(2) Uani 1 d . . .
C16 C 0.1671(2) 0.1471(7) 0.4521(3) 0.0467(17) Uani 1 d . . .
C17 C 0.2218(3) 0.2284(10) 0.4077(4) 0.070(2) Uani 1 d . . .
C18 C 0.1945(3) 0.3377(10) 0.3920(3) 0.070(2) Uani 1 d . . .
H18 H 0.2024 0.4012 0.3710 0.084 Uiso 1 calc . . R
C19 C 0.1535(3) 0.3546(7) 0.4081(3) 0.0563(18) Uani 1 d . . .
C20 C 0.1382(2) 0.2617(6) 0.4365(3) 0.0417(15) Uani 1 d . . .
C21 C -0.0160(3) 0.3538(6) 0.3419(4) 0.067(2) Uani 1 d . . .
H21A H 0.0203 0.3744 0.3564 0.101 Uiso 1 calc . . GR
H21B H -0.0226 0.3583 0.3781 0.101 Uiso 1 calc . . GR
H21C H -0.0386 0.4121 0.3088 0.101 Uiso 1 calc . . GR
C22 C -0.0271(3) 0.2236(6) 0.3146(3) 0.0492(16) Uani 1 d . . .
C23 C -0.0622(3) 0.2091(7) 0.2481(3) 0.0553(19) Uani 1 d . . .
H23 H -0.0762 0.2792 0.2215 0.066 Uiso 1 calc . . R
C24 C -0.0758(3) 0.0919(7) 0.2224(3) 0.0564(19) Uani 1 d . . .
H24 H -0.0991 0.0829 0.1781 0.068 Uiso 1 calc . . R
C25 C -0.0556(2) -0.0157(6) 0.2610(3) 0.0419(15) Uani 1 d . . .
C26 C -0.0200(2) 0.0072(5) 0.3281(2) 0.0335(13) Uani 1 d . . .
C27 C -0.0675(3) -0.1411(6) 0.2403(3) 0.0453(16) Uani 1 d . . .
C28 C -0.0452(2) -0.2381(6) 0.2815(3) 0.0472(16) Uani 1 d . . .
H28 H -0.0524 -0.3204 0.2662 0.057 Uiso 1 calc . . R
C29 C -0.0102(2) -0.2132(6) 0.3487(3) 0.0415(14) Uani 1 d . . .
C30 C 0.0025(2) -0.0938(5) 0.3736(3) 0.0345(13) Uani 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
Dy1 O1 2.243(4) . ?
Dy1 O2 2.204(4) . ?
Dy1 O3 2.225(4) . ?
Dy1 O4 2.337(4) . ?
Dy1 N1 2.607(5) . ?
Dy1 N2 2.608(5) . ?
Dy1 N3 2.624(4) . ?
Cl1 C7 1.736(7) . ?
Cl2 C9 1.736(8) . ?
Cl3 C17 1.732(7) . ?
Cl4 C19 1.740(8) . ?
Cl5 C29 1.737(6) . ?
Cl6 C27 1.734(6) . ?
O1 C10 1.344(7) . ?
O2 C20 1.288(7) . ?
O3 C30 1.343(6) . ?
O4 H4A 0.8562 . ?
O4 H4B 0.8559 . ?
N1 C2 1.336(8) . ?
N1 C6 1.395(8) . ?
N2 C12 1.319(8) . ?
N2 C16 1.350(8) . ?
N3 C22 1.327(7) . ?
N3 C26 1.384(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.497(10) . ?
C2 C3 1.435(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.367(11) . ?
C4 H4 0.9300 . ?
C4 C5 1.383(10) . ?
C5 C6 1.436(8) . ?
C5 C7 1.413(10) . ?
C6 C10 1.409(9) . ?
C7 C8 1.361(11) . ?
C8 H8 0.9300 . ?
C8 C9 1.404(10) . ?
C9 C10 1.378(8) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C11 C12 1.485(12) . ?
C12 C13 1.396(12) . ?
C13 H13 0.9300 . ?
C13 C14 1.417(14) . ?
C14 H14 0.9300 . ?
C14 C15 1.406(12) . ?
C15 C16 1.464(9) . ?
C15 C17 1.354(12) . ?
C16 C20 1.423(9) . ?
C17 C18 1.354(12) . ?
C18 H18 0.9300 . ?
C18 C19 1.422(10) . ?
C19 C20 1.385(9) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C21 C22 1.495(9) . ?
C22 C23 1.396(9) . ?
C23 H23 0.9300 . ?
C23 C24 1.358(10) . ?
C24 H24 0.9300 . ?
C24 C25 1.399(9) . ?
C25 C26 1.422(7) . ?
C25 C27 1.405(8) . ?
C26 C30 1.429(7) . ?
C27 C28 1.345(9) . ?
C28 H28 0.9300 . ?
C28 C29 1.424(8) . ?
C29 C30 1.373(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
O1 Dy1 O4 93.00(15) . . ?
O1 Dy1 N1 66.39(16) . . ?
O1 Dy1 N2 89.87(16) . . ?
O1 Dy1 N3 141.61(15) . . ?
O2 Dy1 O1 136.14(16) . . ?
O2 Dy1 O3 131.60(15) . . ?
O2 Dy1 O4 112.51(15) . . ?
O2 Dy1 N1 82.21(16) . . ?
O2 Dy1 N2 66.46(16) . . ?
O2 Dy1 N3 81.46(15) . . ?
O3 Dy1 O1 78.51(14) . . ?
O3 Dy1 O4 93.08(15) . . ?
O3 Dy1 N1 144.02(15) . . ?
O3 Dy1 N2 85.47(16) . . ?
O3 Dy1 N3 66.85(14) . . ?
O4 Dy1 N1 81.51(15) . . ?
O4 Dy1 N2 176.46(14) . . ?
O4 Dy1 N3 73.57(14) . . ?
N1 Dy1 N2 101.56(15) . . ?
N1 Dy1 N3 142.00(15) . . ?
N2 Dy1 N3 102.90(15) . . ?
C10 O1 Dy1 123.5(4) . . ?
C20 O2 Dy1 126.2(4) . . ?
C30 O3 Dy1 125.3(3) . . ?
Dy1 O4 H4A 109.7 . . ?
Dy1 O4 H4B 109.5 . . ?
H4A O4 H4B 109.2 . . ?
C2 N1 Dy1 130.1(4) . . ?
C2 N1 C6 117.9(6) . . ?
C6 N1 Dy1 111.0(4) . . ?
C12 N2 Dy1 130.7(5) . . ?
C12 N2 C16 118.5(6) . . ?
C16 N2 Dy1 110.8(4) . . ?
C22 N3 Dy1 130.1(4) . . ?
C22 N3 C26 117.8(5) . . ?
C26 N3 Dy1 112.0(3) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
N1 C2 C1 118.8(6) . . ?
N1 C2 C3 120.7(7) . . ?
C3 C2 C1 120.5(7) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 C2 121.4(8) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.6(7) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 117.4(7) . . ?
C4 C5 C7 125.8(7) . . ?
C7 C5 C6 116.7(7) . . ?
N1 C6 C5 122.8(6) . . ?
N1 C6 C10 115.7(5) . . ?
C10 C6 C5 121.4(6) . . ?
C5 C7 Cl1 118.8(7) . . ?
C8 C7 Cl1 119.0(6) . . ?
C8 C7 C5 122.2(6) . . ?
C7 C8 H8 120.4 . . ?
C7 C8 C9 119.2(7) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 Cl2 117.5(6) . . ?
C10 C9 Cl2 120.0(5) . . ?
C10 C9 C8 122.4(7) . . ?
O1 C10 C6 119.2(5) . . ?
O1 C10 C9 123.0(6) . . ?
C9 C10 C6 117.8(6) . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
N2 C12 C11 119.6(7) . . ?
N2 C12 C13 122.7(9) . . ?
C13 C12 C11 117.6(8) . . ?
C12 C13 H13 119.9 . . ?
C12 C13 C14 120.1(8) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 120.4 . . ?
C15 C14 C13 119.2(8) . . ?
C15 C14 H14 120.4 . . ?
C14 C15 C16 114.9(8) . . ?
C17 C15 C14 124.8(8) . . ?
C17 C15 C16 120.2(7) . . ?
N2 C16 C15 124.1(7) . . ?
N2 C16 C20 116.6(5) . . ?
C20 C16 C15 119.2(7) . . ?
C15 C17 Cl3 120.3(8) . . ?
C18 C17 Cl3 118.2(7) . . ?
C18 C17 C15 121.5(7) . . ?
C17 C18 H18 120.4 . . ?
C17 C18 C19 119.3(7) . . ?
C19 C18 H18 120.4 . . ?
C18 C19 Cl4 118.2(6) . . ?
C20 C19 Cl4 118.7(5) . . ?
C20 C19 C18 123.1(7) . . ?
O2 C20 C16 119.3(6) . . ?
O2 C20 C19 124.1(6) . . ?
C19 C20 C16 116.6(6) . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
N3 C22 C21 119.4(6) . . ?
N3 C22 C23 122.5(6) . . ?
C23 C22 C21 118.0(6) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 C22 119.6(6) . . ?
C24 C23 H23 120.2 . . ?
C23 C24 H24 119.1 . . ?
C23 C24 C25 121.7(6) . . ?
C25 C24 H24 119.1 . . ?
C24 C25 C26 115.2(6) . . ?
C24 C25 C27 126.8(6) . . ?
C27 C25 C26 117.9(5) . . ?
N3 C26 C25 123.2(5) . . ?
N3 C26 C30 115.4(5) . . ?
C25 C26 C30 121.3(5) . . ?
C25 C27 Cl6 118.7(5) . . ?
C28 C27 Cl6 119.3(5) . . ?
C28 C27 C25 122.0(5) . . ?
C27 C28 H28 120.5 . . ?
C27 C28 C29 119.1(6) . . ?
C29 C28 H28 120.5 . . ?
C28 C29 Cl5 118.4(5) . . ?
C30 C29 Cl5 118.7(4) . . ?
C30 C29 C28 122.9(6) . . ?
O3 C30 C26 119.8(5) . . ?
O3 C30 C29 123.5(5) . . ?
C29 C30 C26 116.6(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O1 C10 C6 18.9(8) . . . . ?
Dy1 O1 C10 C9 -161.7(5) . . . . ?
Dy1 O2 C20 C16 -8.6(8) . . . . ?
Dy1 O2 C20 C19 169.8(5) . . . . ?
Dy1 O3 C30 C26 -7.6(7) . . . . ?
Dy1 O3 C30 C29 172.1(4) . . . . ?
Dy1 N1 C2 C1 13.1(10) . . . . ?
Dy1 N1 C2 C3 -167.5(5) . . . . ?
Dy1 N1 C6 C5 166.8(5) . . . . ?
Dy1 N1 C6 C10 -12.9(6) . . . . ?
Dy1 N2 C12 C11 0.8(9) . . . . ?
Dy1 N2 C12 C13 177.3(5) . . . . ?
Dy1 N2 C16 C15 -172.0(4) . . . . ?
Dy1 N2 C16 C20 4.5(6) . . . . ?
Dy1 N3 C22 C21 -8.5(9) . . . . ?
Dy1 N3 C22 C23 175.7(5) . . . . ?
Dy1 N3 C26 C25 -176.9(4) . . . . ?
Dy1 N3 C26 C30 5.5(6) . . . . ?
Cl1 C7 C8 C9 -179.7(5) . . . . ?
Cl2 C9 C10 O1 0.9(9) . . . . ?
Cl2 C9 C10 C6 -179.6(5) . . . . ?
Cl3 C17 C18 C19 -178.0(5) . . . . ?
Cl4 C19 C20 O2 2.7(9) . . . . ?
Cl4 C19 C20 C16 -178.8(4) . . . . ?
Cl5 C29 C30 O3 -0.3(8) . . . . ?
Cl5 C29 C30 C26 179.3(4) . . . . ?
Cl6 C27 C28 C29 -179.5(5) . . . . ?
O1 Dy1 O2 C20 70.6(5) . . . . ?
O1 Dy1 O3 C30 170.5(5) . . . . ?
O1 Dy1 N1 C2 -176.4(6) . . . . ?
O1 Dy1 N1 C6 15.6(4) . . . . ?
O1 Dy1 N2 C12 34.0(5) . . . . ?
O1 Dy1 N2 C16 -147.9(4) . . . . ?
O1 Dy1 N3 C22 150.5(5) . . . . ?
O1 Dy1 N3 C26 -33.8(5) . . . . ?
O2 Dy1 O1 C10 29.9(5) . . . . ?
O2 Dy1 O3 C30 -46.0(5) . . . . ?
O2 Dy1 N1 C2 35.0(6) . . . . ?
O2 Dy1 N1 C6 -133.1(4) . . . . ?
O2 Dy1 N2 C12 176.0(5) . . . . ?
O2 Dy1 N2 C16 -6.0(3) . . . . ?
O2 Dy1 N3 C22 -39.6(5) . . . . ?
O2 Dy1 N3 C26 136.1(4) . . . . ?
O3 Dy1 O1 C10 169.9(5) . . . . ?
O3 Dy1 O2 C20 -52.0(5) . . . . ?
O3 Dy1 N1 C2 -162.8(5) . . . . ?
O3 Dy1 N1 C6 29.2(5) . . . . ?
O3 Dy1 N2 C12 -44.5(5) . . . . ?
O3 Dy1 N2 C16 133.6(4) . . . . ?
O3 Dy1 N3 C22 177.8(6) . . . . ?
O3 Dy1 N3 C26 -6.5(3) . . . . ?
O4 Dy1 O1 C10 -97.5(5) . . . . ?
O4 Dy1 O2 C20 -168.5(4) . . . . ?
O4 Dy1 O3 C30 78.0(4) . . . . ?
O4 Dy1 N1 C2 -79.3(6) . . . . ?
O4 Dy1 N1 C6 112.7(4) . . . . ?
O4 Dy1 N2 C12 -110(2) . . . . ?
O4 Dy1 N2 C16 68(3) . . . . ?
O4 Dy1 N3 C22 77.0(5) . . . . ?
O4 Dy1 N3 C26 -107.3(4) . . . . ?
N1 Dy1 O1 C10 -18.2(4) . . . . ?
N1 Dy1 O2 C20 114.1(5) . . . . ?
N1 Dy1 O3 C30 157.8(4) . . . . ?
N1 Dy1 N2 C12 99.9(5) . . . . ?
N1 Dy1 N2 C16 -82.1(4) . . . . ?
N1 Dy1 N3 C22 25.9(7) . . . . ?
N1 Dy1 N3 C26 -158.4(3) . . . . ?
N1 C2 C3 C4 3.3(12) . . . . ?
N1 C6 C10 O1 -1.1(8) . . . . ?
N1 C6 C10 C9 179.4(5) . . . . ?
N2 Dy1 O1 C10 84.5(5) . . . . ?
N2 Dy1 O2 C20 7.8(4) . . . . ?
N2 Dy1 O3 C30 -98.7(4) . . . . ?
N2 Dy1 N1 C2 98.9(6) . . . . ?
N2 Dy1 N1 C6 -69.1(4) . . . . ?
N2 Dy1 N3 C22 -102.9(5) . . . . ?
N2 Dy1 N3 C26 72.8(4) . . . . ?
N2 C12 C13 C14 -3.5(12) . . . . ?
N2 C16 C20 O2 1.4(8) . . . . ?
N2 C16 C20 C19 -177.2(5) . . . . ?
N3 Dy1 O1 C10 -164.6(4) . . . . ?
N3 Dy1 O2 C20 -100.3(5) . . . . ?
N3 Dy1 O3 C30 7.4(4) . . . . ?
N3 Dy1 N1 C2 -30.3(7) . . . . ?
N3 Dy1 N1 C6 161.7(3) . . . . ?
N3 Dy1 N2 C12 -109.5(5) . . . . ?
N3 Dy1 N2 C16 68.6(4) . . . . ?
N3 C22 C23 C24 0.0(11) . . . . ?
N3 C26 C30 O3 0.1(8) . . . . ?
N3 C26 C30 C29 -179.5(5) . . . . ?
C1 C2 C3 C4 -177.4(7) . . . . ?
C2 N1 C6 C5 -2.8(9) . . . . ?
C2 N1 C6 C10 177.4(6) . . . . ?
C2 C3 C4 C5 -3.2(12) . . . . ?
C3 C4 C5 C6 0.3(11) . . . . ?
C3 C4 C5 C7 178.9(7) . . . . ?
C4 C5 C6 N1 2.8(9) . . . . ?
C4 C5 C6 C10 -177.5(6) . . . . ?
C4 C5 C7 Cl1 -1.6(10) . . . . ?
C4 C5 C7 C8 176.8(7) . . . . ?
C5 C6 C10 O1 179.1(5) . . . . ?
C5 C6 C10 C9 -0.4(9) . . . . ?
C5 C7 C8 C9 1.9(11) . . . . ?
C6 N1 C2 C1 -179.6(6) . . . . ?
C6 N1 C2 C3 -0.2(10) . . . . ?
C6 C5 C7 Cl1 177.0(5) . . . . ?
C6 C5 C7 C8 -4.7(10) . . . . ?
C7 C5 C6 N1 -175.9(6) . . . . ?
C7 C5 C6 C10 3.8(9) . . . . ?
C7 C8 C9 Cl2 179.0(6) . . . . ?
C7 C8 C9 C10 1.9(11) . . . . ?
C8 C9 C10 O1 177.9(6) . . . . ?
C8 C9 C10 C6 -2.6(10) . . . . ?
C11 C12 C13 C14 173.0(8) . . . . ?
C12 N2 C16 C15 6.3(9) . . . . ?
C12 N2 C16 C20 -177.2(5) . . . . ?
C12 C13 C14 C15 2.0(13) . . . . ?
C13 C14 C15 C16 2.9(11) . . . . ?
C13 C14 C15 C17 -179.9(8) . . . . ?
C14 C15 C16 N2 -7.4(9) . . . . ?
C14 C15 C16 C20 176.2(6) . . . . ?
C14 C15 C17 Cl3 3.0(10) . . . . ?
C14 C15 C17 C18 -176.4(7) . . . . ?
C15 C16 C20 O2 178.1(5) . . . . ?
C15 C16 C20 C19 -0.5(8) . . . . ?
C15 C17 C18 C19 1.4(11) . . . . ?
C16 N2 C12 C11 -177.1(6) . . . . ?
C16 N2 C12 C13 -0.6(9) . . . . ?
C16 C15 C17 Cl3 -179.9(5) . . . . ?
C16 C15 C17 C18 0.7(11) . . . . ?
C17 C15 C16 N2 175.3(6) . . . . ?
C17 C15 C16 C20 -1.2(9) . . . . ?
C17 C18 C19 Cl4 178.2(6) . . . . ?
C17 C18 C19 C20 -3.2(11) . . . . ?
C18 C19 C20 O2 -175.9(6) . . . . ?
C18 C19 C20 C16 2.6(9) . . . . ?
C21 C22 C23 C24 -175.8(7) . . . . ?
C22 N3 C26 C25 -0.6(8) . . . . ?
C22 N3 C26 C30 -178.2(5) . . . . ?
C22 C23 C24 C25 0.1(11) . . . . ?
C23 C24 C25 C26 -0.5(10) . . . . ?
C23 C24 C25 C27 178.7(6) . . . . ?
C24 C25 C26 N3 0.7(8) . . . . ?
C24 C25 C26 C30 178.2(5) . . . . ?
C24 C25 C27 Cl6 1.4(9) . . . . ?
C24 C25 C27 C28 178.9(6) . . . . ?
C25 C26 C30 O3 -177.6(5) . . . . ?
C25 C26 C30 C29 2.8(8) . . . . ?
C25 C27 C28 C29 3.0(9) . . . . ?
C26 N3 C22 C21 176.0(6) . . . . ?
C26 N3 C22 C23 0.2(9) . . . . ?
C26 C25 C27 Cl6 -179.5(4) . . . . ?
C26 C25 C27 C28 -2.0(9) . . . . ?
C27 C25 C26 N3 -178.5(5) . . . . ?
C27 C25 C26 C30 -1.0(8) . . . . ?
C27 C28 C29 Cl5 177.8(5) . . . . ?
C27 C28 C29 C30 -1.1(9) . . . . ?
C28 C29 C30 O3 178.6(6) . . . . ?
C28 C29 C30 C26 -1.8(9) . . . . ?

_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_20180423_lfp_whl_1246aaaa
_database_code_depnum_ccdc_archive 'CCDC 1856175'
_audit_update_record             
;
2018-07-15 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;
_audit_creation_date             2018-06-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C24 H16 Dy N7 O9'
_chemical_formula_sum            'C24 H16 Dy N7 O9'
_chemical_formula_weight         708.94
_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'
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'

_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_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   11.1454(3)
_cell_length_b                   17.8782(3)
_cell_length_c                   13.0034(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.471(2)
_cell_angle_gamma                90.00
_cell_volume                     2547.90(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6359
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3950
_cell_measurement_theta_min      3.8760
_exptl_absorpt_coefficient_mu    3.001
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9332
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.19
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -14.00  85.00   1.00    2.50    --   10.68  38.00 -90.00   99
  2  ω    -61.00  39.00   1.00    2.50    --   10.68 -57.00  90.00  100
  3  ω     35.00  99.00   1.00    2.50    --   10.68 178.00 -30.00   64
  4  ω    -88.00 -63.00   1.00    2.50    --  -11.93 -77.00  60.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0240790000
_diffrn_orient_matrix_UB_12      -0.0324411000
_diffrn_orient_matrix_UB_13      -0.0277286000
_diffrn_orient_matrix_UB_21      0.0571418000
_diffrn_orient_matrix_UB_22      -0.0181698000
_diffrn_orient_matrix_UB_23      0.0146651000
_diffrn_orient_matrix_UB_31      -0.0185941000
_diffrn_orient_matrix_UB_32      -0.0138384000
_diffrn_orient_matrix_UB_33      0.0457410000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2326
_reflns_number_total             2497
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2497
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0211
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0161P)²+2.3481P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0447
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C6(H6), C8(H8), C5(H5), C2(H2), C9(H9), C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Dy1 Dy 0.5000 0.324710(9) 0.7500 0.02738(7) Uani 1 d . . 2 S T P
O1 O 0.67972(19) 0.33488(11) 0.89867(16) 0.0423(5) Uani 1 d . . 1 . . .
O2 O 0.70835(18) 0.36839(11) 0.74588(15) 0.0415(5) Uani 1 d . . 1 . . .
O4 O 0.5138(2) 0.44869(12) 0.83398(18) 0.0546(6) Uani 1 d . . 1 . . .
N2 N 0.5563(2) 0.28077(12) 0.58264(16) 0.0323(5) Uani 1 d . . 1 . . .
N3 N 0.7522(2) 0.35970(13) 0.8428(2) 0.0412(6) Uani 1 d . . 1 . . .
N1 N 0.6292(2) 0.20554(12) 0.76496(17) 0.0317(5) Uani 1 d . . 1 . . .
O3 O 0.8572(2) 0.37571(16) 0.8791(2) 0.0728(7) Uani 1 d . . 1 . . .
N4 N 0.5000 0.4859(2) 0.7500 0.0573(11) Uani 1 d . . 2 S T P
C11 C 0.6064(2) 0.21191(14) 0.5780(2) 0.0294(6) Uani 1 d . . 1 . . .
C1 C 0.6652(3) 0.16866(15) 0.8534(2) 0.0394(7) Uani 1 d . . 1 . . .
H1 H 0.6596 0.1924 0.9160 0.047 Uiso 1 calc . . 1 R . .
C12 C 0.6414(3) 0.17106(14) 0.6740(2) 0.0305(6) Uani 1 d . . 1 . . .
C7 C 0.6249(3) 0.17980(15) 0.4839(2) 0.0365(7) Uani 1 d . . 1 . . .
C10 C 0.5300(3) 0.31948(16) 0.4947(2) 0.0422(7) Uani 1 d . . 1 . . .
H10 H 0.4966 0.3670 0.4971 0.051 Uiso 1 calc . . 1 R . .
O5 O 0.5000 0.55379(18) 0.7500 0.0977(15) Uani 1 d . . 2 S T P
C6 C 0.6724(3) 0.10584(18) 0.4842(3) 0.0546(9) Uani 1 d . . 1 . . .
H6 H 0.6825 0.0841 0.4214 0.066 Uiso 1 calc . . 1 R . .
C4 C 0.6879(3) 0.09839(15) 0.6714(2) 0.0422(7) Uani 1 d . . 1 . . .
C8 C 0.5952(3) 0.22316(19) 0.3931(2) 0.0453(8) Uani 1 d . . 1 . . .
H8 H 0.6066 0.2040 0.3291 0.054 Uiso 1 calc . . 1 R . .
C5 C 0.7028(4) 0.06677(18) 0.5734(3) 0.0593(10) Uani 1 d . . 1 . . .
H5 H 0.7338 0.0186 0.5714 0.071 Uiso 1 calc . . 1 R . .
C2 C 0.7114(3) 0.09604(17) 0.8574(2) 0.0497(8) Uani 1 d . . 1 . . .
H2 H 0.7353 0.0721 0.9213 0.060 Uiso 1 calc . . 1 R . .
C9 C 0.5499(3) 0.29262(19) 0.3988(2) 0.0481(8) Uani 1 d . . 1 . . .
H9 H 0.5322 0.3223 0.3392 0.058 Uiso 1 calc . . 1 R . .
C3 C 0.7208(3) 0.06084(17) 0.7672(3) 0.0538(9) Uani 1 d . . 1 . . .
H3 H 0.7492 0.0119 0.7686 0.065 Uiso 1 calc . . 1 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
Dy1 O1 2.525(2) 2_656 ?
Dy1 O1 2.525(2) . ?
Dy1 O2 2.4598(19) . ?
Dy1 O2 2.4598(19) 2_656 ?
Dy1 O4 2.463(2) . ?
Dy1 O4 2.463(2) 2_656 ?
Dy1 N2 2.499(2) . ?
Dy1 N2 2.499(2) 2_656 ?
Dy1 N3 2.919(3) 2_656 ?
Dy1 N1 2.559(2) . ?
Dy1 N1 2.559(2) 2_656 ?
Dy1 N4 2.882(4) . ?
O1 N3 1.262(3) . ?
O2 N3 1.276(3) . ?
O4 N4 1.264(3) . ?
N2 C11 1.357(3) . ?
N2 C10 1.324(3) . ?
N3 O3 1.213(3) . ?
N1 C1 1.323(3) . ?
N1 C12 1.363(3) . ?
N4 O4 1.264(3) 2_656 ?
N4 O5 1.213(5) . ?
C11 C12 1.437(4) . ?
C11 C7 1.401(4) . ?
C1 H1 0.9300 . ?
C1 C2 1.394(4) . ?
C12 C4 1.401(4) . ?
C7 C6 1.424(4) . ?
C7 C8 1.400(4) . ?
C10 H10 0.9300 . ?
C10 C9 1.391(4) . ?
C6 H6 0.9300 . ?
C6 C5 1.343(4) . ?
C4 C5 1.432(4) . ?
C4 C3 1.403(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.347(4) . ?
C5 H5 0.9300 . ?
C2 H2 0.9300 . ?
C2 C3 1.352(4) . ?
C9 H9 0.9300 . ?
C3 H3 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
O1 Dy1 O1 171.74(9) 2_656 . ?
O1 Dy1 N3 25.51(7) 2_656 2_656 ?
O1 Dy1 N3 150.65(7) . 2_656 ?
O1 Dy1 N1 69.19(7) 2_656 2_656 ?
O1 Dy1 N1 118.37(7) . 2_656 ?
O1 Dy1 N1 69.19(7) . . ?
O1 Dy1 N1 118.37(7) 2_656 . ?
O1 Dy1 N4 85.87(4) 2_656 . ?
O1 Dy1 N4 85.87(4) . . ?
O2 Dy1 O1 125.54(7) . 2_656 ?
O2 Dy1 O1 51.18(6) . . ?
O2 Dy1 O1 125.54(7) 2_656 . ?
O2 Dy1 O1 51.18(6) 2_656 2_656 ?
O2 Dy1 O2 142.98(10) 2_656 . ?
O2 Dy1 O4 74.98(7) . . ?
O2 Dy1 O4 71.81(7) 2_656 . ?
O2 Dy1 O4 71.81(7) . 2_656 ?
O2 Dy1 O4 74.98(7) 2_656 2_656 ?
O2 Dy1 N2 120.42(7) . 2_656 ?
O2 Dy1 N2 72.14(7) 2_656 2_656 ?
O2 Dy1 N2 120.42(7) 2_656 . ?
O2 Dy1 N2 72.14(7) . . ?
O2 Dy1 N3 139.93(6) . 2_656 ?
O2 Dy1 N3 25.67(6) 2_656 2_656 ?
O2 Dy1 N1 75.27(7) 2_656 2_656 ?
O2 Dy1 N1 141.54(7) . 2_656 ?
O2 Dy1 N1 141.54(7) 2_656 . ?
O2 Dy1 N1 75.27(7) . . ?
O2 Dy1 N4 71.49(5) . . ?
O2 Dy1 N4 71.49(5) 2_656 . ?
O4 Dy1 O1 67.60(7) 2_656 2_656 ?
O4 Dy1 O1 104.57(7) . 2_656 ?
O4 Dy1 O1 104.57(7) 2_656 . ?
O4 Dy1 O1 67.60(7) . . ?
O4 Dy1 O4 51.74(11) 2_656 . ?
O4 Dy1 N2 84.38(8) . 2_656 ?
O4 Dy1 N2 131.58(8) . . ?
O4 Dy1 N2 84.38(8) 2_656 . ?
O4 Dy1 N2 131.58(8) 2_656 2_656 ?
O4 Dy1 N3 88.18(7) . 2_656 ?
O4 Dy1 N3 69.27(7) 2_656 2_656 ?
O4 Dy1 N1 136.60(7) 2_656 2_656 ?
O4 Dy1 N1 140.52(7) . 2_656 ?
O4 Dy1 N1 136.60(7) . . ?
O4 Dy1 N1 140.52(7) 2_656 . ?
O4 Dy1 N4 25.87(6) . . ?
O4 Dy1 N4 25.87(6) 2_656 . ?
N2 Dy1 O1 113.55(7) . . ?
N2 Dy1 O1 113.55(7) 2_656 2_656 ?
N2 Dy1 O1 69.25(7) . 2_656 ?
N2 Dy1 O1 69.25(7) 2_656 . ?
N2 Dy1 N2 143.35(10) . 2_656 ?
N2 Dy1 N3 92.97(7) 2_656 2_656 ?
N2 Dy1 N3 94.76(7) . 2_656 ?
N2 Dy1 N1 84.20(7) 2_656 . ?
N2 Dy1 N1 84.20(7) . 2_656 ?
N2 Dy1 N1 65.01(7) . . ?
N2 Dy1 N1 65.01(7) 2_656 2_656 ?
N2 Dy1 N4 108.32(5) . . ?
N2 Dy1 N4 108.32(5) 2_656 . ?
N1 Dy1 N3 70.17(7) 2_656 2_656 ?
N1 Dy1 N3 134.13(7) . 2_656 ?
N1 Dy1 N1 67.26(10) 2_656 . ?
N1 Dy1 N4 146.37(5) . . ?
N1 Dy1 N4 146.37(5) 2_656 . ?
N4 Dy1 N3 77.62(5) . 2_656 ?
N3 O1 Dy1 94.96(16) . . ?
N3 O2 Dy1 97.70(15) . . ?
N4 O4 Dy1 95.90(19) . . ?
C11 N2 Dy1 119.59(16) . . ?
C10 N2 Dy1 122.49(18) . . ?
C10 N2 C11 117.7(2) . . ?
O1 N3 Dy1 59.53(14) . . ?
O1 N3 O2 116.2(2) . . ?
O2 N3 Dy1 56.64(13) . . ?
O3 N3 Dy1 178.1(2) . . ?
O3 N3 O1 122.1(3) . . ?
O3 N3 O2 121.7(3) . . ?
C1 N1 Dy1 123.99(17) . . ?
C1 N1 C12 117.8(2) . . ?
C12 N1 Dy1 117.01(17) . . ?
O4 N4 Dy1 58.23(17) 2_656 . ?
O4 N4 Dy1 58.23(17) . . ?
O4 N4 O4 116.5(3) 2_656 . ?
O5 N4 Dy1 180.000(1) . . ?
O5 N4 O4 121.77(17) . . ?
O5 N4 O4 121.77(17) . 2_656 ?
N2 C11 C12 118.1(2) . . ?
N2 C11 C7 122.5(2) . . ?
C7 C11 C12 119.4(2) . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.3(3) . . ?
C2 C1 H1 118.4 . . ?
N1 C12 C11 118.0(2) . . ?
N1 C12 C4 122.4(2) . . ?
C4 C12 C11 119.6(2) . . ?
C11 C7 C6 119.4(3) . . ?
C8 C7 C11 117.4(3) . . ?
C8 C7 C6 123.2(3) . . ?
N2 C10 H10 118.4 . . ?
N2 C10 C9 123.2(3) . . ?
C9 C10 H10 118.4 . . ?
C7 C6 H6 119.3 . . ?
C5 C6 C7 121.4(3) . . ?
C5 C6 H6 119.3 . . ?
C12 C4 C5 119.4(3) . . ?
C12 C4 C3 117.5(3) . . ?
C3 C4 C5 123.2(3) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 C7 119.9(3) . . ?
C9 C8 H8 120.1 . . ?
C6 C5 C4 120.7(3) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2 120.4 . . ?
C10 C9 H9 120.4 . . ?
C8 C9 C10 119.3(3) . . ?
C8 C9 H9 120.4 . . ?
C4 C3 H3 120.1 . . ?
C2 C3 C4 119.9(3) . . ?
C2 C3 H3 120.1 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.194
_oxdiff_exptl_absorpt_empirical_full_min 0.852
####################################################################### 
# 
# 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_aaa_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1856174'
_audit_update_record             
;
2018-07-15 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;
_audit_creation_date             2017-09-19
_audit_creation_method           
;
  Olex2 1.2-ac2
  (compiled 2012.03.06 svn.r2239, GUI svn.r4109)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         
'4(C30 H20 Br6 Dy N3 O4), C2 H2 Cl6, 0.5(C2 Cl6)'
_chemical_formula_sum            'C123 H82 Br24 Cl9 Dy4 N12 O16'
_chemical_formula_weight         4870.90
_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 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.3670(4)
_cell_length_b                   13.7483(4)
_cell_length_c                   20.9730(6)
_cell_angle_alpha                71.835(3)
_cell_angle_beta                 79.055(3)
_cell_angle_gamma                86.694(3)
_cell_volume                     3595.59(19)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    42056
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.39
_cell_measurement_theta_min      3.7
_exptl_absorpt_coefficient_mu    20.809
_exptl_absorpt_correction_T_max  0.1891
_exptl_absorpt_correction_T_min  0.0427
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.250
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2289
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42056
_diffrn_reflns_theta_full        74.39
_diffrn_reflns_theta_max         74.39
_diffrn_reflns_theta_min         3.70
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                12629
_reflns_number_total             14202
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.093
_refine_diff_density_min         -1.549
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         14202
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0481
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0713P)²+9.4267P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1293
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.88890(2) -0.15909(2) 0.557680(16) 0.03131(9) Uani 1 1 d . . .
Dy2 Dy 0.61732(2) 0.13536(2) 0.926140(15) 0.03139(9) Uani 1 1 d . . .
Br1 Br 0.72029(7) 0.19861(7) 0.55462(5) 0.0721(3) Uani 1 1 d . . .
Br2 Br 0.47017(7) 0.12563(12) 0.38554(6) 0.1269(6) Uani 1 1 d . . .
Br3 Br 1.06116(6) 0.00211(7) 0.70908(4) 0.0598(2) Uani 1 1 d . . .
Br4 Br 1.33602(9) -0.32640(9) 0.73776(8) 0.1110(5) Uani 1 1 d . . .
Br5 Br 0.50045(6) -0.50103(6) 0.83232(4) 0.0629(2) Uani 1 1 d . . .
Br6 Br 0.74689(7) -0.52268(6) 0.58815(5) 0.0669(2) Uani 1 1 d . . .
Br7 Br 0.88335(6) 0.24573(7) 0.69817(4) 0.0623(2) Uani 1 1 d . . .
Br8 Br 0.93596(6) 0.60984(7) 0.75736(5) 0.0708(3) Uani 1 1 d . . .
Br9 Br 0.95200(8) -0.16586(7) 1.17237(6) 0.0817(3) Uani 1 1 d . . .
Br10 Br 0.59743(6) 0.07074(8) 1.19128(4) 0.0634(2) Uani 1 1 d . . .
Br11 Br 0.28817(5) 0.26081(5) 1.05781(4) 0.05250(17) Uani 1 1 d . . .
Br12 Br 0.15662(8) 0.42652(8) 0.80641(6) 0.0914(4) Uani 1 1 d . . .
Cl1 Cl 1.0424(4) -0.3680(5) 1.0272(4) 0.112(2) Uani 0.50 1 d P A 1
Cl1' Cl 1.1609(11) -0.2308(12) 0.9430(7) 0.126(4) Uani 0.50 1 d P A 2
Cl2 Cl 1.0283(13) -0.3107(15) 0.8774(7) 0.154(5) Uani 0.50 1 d P A 1
Cl2' Cl 1.1884(10) -0.3967(10) 0.8994(7) 0.195(5) Uani 0.50 1 d P A 2
Cl3 Cl 1.1740(12) -0.2285(14) 0.9105(7) 0.132(5) Uani 0.50 1 d P A 1
Cl3' Cl 0.9988(14) -0.3401(16) 0.9128(9) 0.178(6) Uani 0.50 1 d P A 2
Cl4 Cl 0.5563(8) -0.3722(9) 0.4674(5) 0.155(3) Uani 0.50 1 d P . 1
Cl5 Cl 0.4313(10) -0.5422(13) 0.5687(6) 0.187(5) Uani 0.50 1 d P . 1
Cl6 Cl 0.4666(10) -0.4537(11) 0.5690(7) 0.185(5) Uani 0.50 1 d P . 2
O1 O 0.6196(3) 0.0856(3) 1.03874(19) 0.0381(9) Uani 1 1 d . . .
O2 O 0.4590(3) 0.1737(3) 0.97093(19) 0.0375(8) Uani 1 1 d . . .
O3 O 0.5731(3) -0.0184(3) 0.9129(2) 0.0394(9) Uani 1 1 d . . .
H3A H 0.5095 -0.0172 0.9128 0.047 Uiso 1 1 d R . .
H3B H 0.5839 -0.0669 0.9476 0.047 Uiso 1 1 d R . .
O4 O 0.7300(3) 0.2005(3) 0.8341(2) 0.0439(10) Uani 1 1 d . . .
O5 O 0.8248(3) 0.0006(3) 0.5348(2) 0.0389(9) Uani 1 1 d . . .
O6 O 0.9848(3) -0.0983(3) 0.6142(2) 0.0366(8) Uani 1 1 d . . .
O7 O 0.8152(3) -0.3085(3) 0.5821(2) 0.0434(9) Uani 1 1 d . . .
O8 O 1.0120(3) -0.1077(3) 0.45713(19) 0.0373(9) Uani 1 1 d . . .
H8A H 1.0674 -0.0962 0.4679 0.045 Uiso 1 1 d R . .
H8B H 0.9928 -0.0513 0.4318 0.045 Uiso 1 1 d R . .
N1 N 1.0495(4) -0.2703(4) 0.5848(3) 0.0401(11) Uani 1 1 d . . .
N2 N 0.7789(4) -0.1153(5) 0.4626(3) 0.0487(13) Uani 1 1 d . . .
N3 N 0.7550(3) -0.2037(4) 0.6695(2) 0.0333(10) Uani 1 1 d . . .
N4 N 0.4909(4) 0.1980(4) 0.8375(3) 0.0429(11) Uani 1 1 d . . .
N5 N 0.6802(4) 0.3126(4) 0.9189(3) 0.0395(11) Uani 1 1 d . . .
N6 N 0.7655(4) 0.0097(4) 0.9621(3) 0.0376(10) Uani 1 1 d . . .
C1 C 0.8274(5) -0.0139(6) 0.8504(3) 0.0500(15) Uani 1 1 d . . .
H1A H 0.7574 -0.0205 0.8477 0.075 Uiso 1 1 calc R . .
H1B H 0.8675 -0.0646 0.8344 0.075 Uiso 1 1 calc R . .
H1C H 0.8518 0.0531 0.8227 0.075 Uiso 1 1 calc R . .
C2 C 0.8361(5) -0.0287(5) 0.9227(3) 0.0419(13) Uani 1 1 d . . .
C3 C 0.9181(5) -0.0860(6) 0.9491(4) 0.0522(16) Uani 1 1 d . . .
H3 H 0.9675 -0.1105 0.9203 0.063 Uiso 1 1 calc R . .
C4 C 0.9265(5) -0.1060(5) 1.0152(4) 0.0526(16) Uani 1 1 d . . .
H4 H 0.9814 -0.1436 1.0317 0.063 Uiso 1 1 calc R . .
C5 C 0.8509(5) -0.0692(5) 1.0589(3) 0.0442(14) Uani 1 1 d . . .
C6 C 0.8480(5) -0.0862(5) 1.1298(4) 0.0480(15) Uani 1 1 d . . .
C7 C 0.7741(5) -0.0454(5) 1.1679(4) 0.0502(16) Uani 1 1 d . . .
H7 H 0.7749 -0.0558 1.2138 0.060 Uiso 1 1 calc R . .
C8 C 0.6966(5) 0.0128(5) 1.1370(3) 0.0414(13) Uani 1 1 d . . .
C9 C 0.6923(4) 0.0318(4) 1.0682(3) 0.0362(12) Uani 1 1 d . . .
C10 C 0.7717(4) -0.0103(5) 1.0294(3) 0.0377(12) Uani 1 1 d . . .
C11 C 0.5761(6) 0.3276(6) 1.0241(4) 0.0551(17) Uani 1 1 d . . .
H11A H 0.5103 0.3545 1.0159 0.083 Uiso 1 1 calc R . .
H11B H 0.5936 0.3476 1.0606 0.083 Uiso 1 1 calc R . .
H11C H 0.5746 0.2543 1.0365 0.083 Uiso 1 1 calc R . .
C12 C 0.6538(5) 0.3688(5) 0.9610(3) 0.0426(13) Uani 1 1 d . . .
C13 C 0.6964(5) 0.4661(5) 0.9472(4) 0.0507(16) Uani 1 1 d . . .
H13 H 0.6768 0.5033 0.9777 0.061 Uiso 1 1 calc R . .
C14 C 0.7667(5) 0.5064(5) 0.8889(4) 0.0500(16) Uani 1 1 d . . .
H14 H 0.7940 0.5711 0.8797 0.060 Uiso 1 1 calc R . .
C15 C 0.7973(5) 0.4495(5) 0.8432(3) 0.0442(14) Uani 1 1 d . . .
C16 C 0.8705(5) 0.4820(5) 0.7811(3) 0.0473(15) Uani 1 1 d . . .
C17 C 0.8945(5) 0.4218(5) 0.7400(3) 0.0505(17) Uani 1 1 d . . .
H17 H 0.9427 0.4440 0.7002 0.061 Uiso 1 1 calc R . .
C18 C 0.8471(5) 0.3262(5) 0.7570(3) 0.0432(14) Uani 1 1 d . . .
C19 C 0.7755(4) 0.2893(5) 0.8164(3) 0.0408(13) Uani 1 1 d . . .
C20 C 0.7509(4) 0.3520(5) 0.8601(3) 0.0390(13) Uani 1 1 d . . .
C21 C 0.5975(6) 0.1515(7) 0.7433(4) 0.064(2) Uani 1 1 d . . .
H21A H 0.6589 0.1865 0.7409 0.097 Uiso 1 1 calc R . .
H21B H 0.5917 0.1513 0.6984 0.097 Uiso 1 1 calc R . .
H21C H 0.5997 0.0822 0.7725 0.097 Uiso 1 1 calc R . .
C22 C 0.5070(5) 0.2054(5) 0.7717(3) 0.0494(15) Uani 1 1 d . . .
C23 C 0.4401(6) 0.2631(6) 0.7291(4) 0.0586(19) Uani 1 1 d . . .
H23 H 0.4538 0.2689 0.6829 0.070 Uiso 1 1 calc R . .
C24 C 0.3573(6) 0.3099(6) 0.7537(4) 0.0595(19) Uani 1 1 d . . .
H24 H 0.3148 0.3482 0.7248 0.071 Uiso 1 1 calc R . .
C25 C 0.3358(5) 0.3001(5) 0.8244(3) 0.0487(15) Uani 1 1 d . . .
C26 C 0.4063(5) 0.2438(5) 0.8635(3) 0.0401(13) Uani 1 1 d . . .
C27 C 0.3928(4) 0.2288(4) 0.9355(3) 0.0372(12) Uani 1 1 d . . .
C28 C 0.3092(5) 0.2755(5) 0.9636(3) 0.0411(13) Uani 1 1 d . . .
C29 C 0.2386(5) 0.3334(5) 0.9250(4) 0.0516(16) Uani 1 1 d . . .
H29 H 0.1829 0.3630 0.9459 0.062 Uiso 1 1 calc R . .
C30 C 0.2519(5) 0.3457(5) 0.8579(4) 0.0530(17) Uani 1 1 d . . .
C31 C 0.8270(7) -0.2610(7) 0.4219(4) 0.068(2) Uani 1 1 d . . .
H31A H 0.8971 -0.2403 0.4066 0.102 Uiso 1 1 calc R . .
H31B H 0.8067 -0.2914 0.3908 0.102 Uiso 1 1 calc R . .
H31C H 0.8189 -0.3100 0.4666 0.102 Uiso 1 1 calc R . .
C32 C 0.7637(6) -0.1720(7) 0.4242(4) 0.061(2) Uani 1 1 d . . .
C33 C 0.6802(7) -0.1446(8) 0.3868(4) 0.074(3) Uani 1 1 d . . .
H33 H 0.6673 -0.1854 0.3612 0.088 Uiso 1 1 calc R . .
C34 C 0.6224(6) -0.0654(8) 0.3875(4) 0.068(2) Uani 1 1 d . . .
H34 H 0.5702 -0.0500 0.3623 0.081 Uiso 1 1 calc R . .
C35 C 0.6391(5) -0.0021(7) 0.4268(4) 0.059(2) Uani 1 1 d . . .
C36 C 0.7210(5) -0.0297(6) 0.4629(3) 0.0496(16) Uani 1 1 d . . .
C37 C 0.7480(4) 0.0297(5) 0.5016(3) 0.0462(15) Uani 1 1 d . . .
C38 C 0.6893(5) 0.1168(6) 0.5035(3) 0.0547(18) Uani 1 1 d . . .
C39 C 0.6063(5) 0.1423(7) 0.4670(4) 0.066(2) Uani 1 1 d . . .
H39 H 0.5677 0.2004 0.4681 0.079 Uiso 1 1 calc R . .
C40 C 0.5835(6) 0.0841(7) 0.4315(4) 0.067(2) Uani 1 1 d . . .
C41 C 0.7027(5) -0.4457(5) 0.6493(3) 0.0433(14) Uani 1 1 d . . .
C42 C 0.6299(5) -0.4904(5) 0.7081(3) 0.0470(15) Uani 1 1 d . . .
H42 H 0.6032 -0.5548 0.7155 0.056 Uiso 1 1 calc R . .
C43 C 0.5994(5) -0.4391(5) 0.7533(3) 0.0441(14) Uani 1 1 d . . .
C44 C 0.6391(4) -0.3411(5) 0.7437(3) 0.0403(13) Uani 1 1 d . . .
C45 C 0.7119(4) -0.2973(4) 0.6835(3) 0.0354(12) Uani 1 1 d . . .
C46 C 0.7463(4) -0.3504(4) 0.6354(3) 0.0368(12) Uani 1 1 d . . .
C47 C 0.6116(5) -0.2813(5) 0.7887(3) 0.0444(14) Uani 1 1 d . . .
H47 H 0.5642 -0.3062 0.8286 0.053 Uiso 1 1 calc R . .
C48 C 0.6544(5) -0.1880(5) 0.7733(3) 0.0434(14) Uani 1 1 d . . .
H48 H 0.6358 -0.1488 0.8026 0.052 Uiso 1 1 calc R . .
C49 C 0.7273(4) -0.1496(4) 0.7130(3) 0.0348(11) Uani 1 1 d . . .
C50 C 0.7729(5) -0.0465(5) 0.6967(3) 0.0463(14) Uani 1 1 d . . .
H50A H 0.8459 -0.0521 0.6897 0.070 Uiso 1 1 calc R . .
H50B H 0.7496 -0.0193 0.7339 0.070 Uiso 1 1 calc R . .
H50C H 0.7528 -0.0017 0.6560 0.070 Uiso 1 1 calc R . .
C51 C 1.0298(6) -0.3851(6) 0.5219(4) 0.064(2) Uani 1 1 d . . .
H51A H 0.9594 -0.4001 0.5419 0.095 Uiso 1 1 calc R . .
H51B H 1.0626 -0.4450 0.5135 0.095 Uiso 1 1 calc R . .
H51C H 1.0344 -0.3305 0.4797 0.095 Uiso 1 1 calc R . .
C52 C 1.0799(5) -0.3542(5) 0.5687(4) 0.0506(16) Uani 1 1 d . . .
C53 C 1.1638(6) -0.4125(6) 0.5961(4) 0.0592(19) Uani 1 1 d . . .
H53 H 1.1839 -0.4723 0.5854 0.071 Uiso 1 1 calc R . .
C54 C 1.2132(6) -0.3824(6) 0.6366(4) 0.0605(19) Uani 1 1 d . . .
H54 H 1.2684 -0.4199 0.6525 0.073 Uiso 1 1 calc R . .
C55 C 1.1818(5) -0.2952(5) 0.6545(3) 0.0487(15) Uani 1 1 d . . .
C56 C 1.0980(4) -0.2390(5) 0.6271(3) 0.0412(13) Uani 1 1 d . . .
C57 C 1.0610(4) -0.1470(5) 0.6415(3) 0.0381(12) Uani 1 1 d . . .
C58 C 1.1082(5) -0.1153(5) 0.6852(3) 0.0445(14) Uani 1 1 d . . .
C59 C 1.1911(5) -0.1698(6) 0.7134(4) 0.0550(18) Uani 1 1 d . . .
H59 H 1.2212 -0.1465 0.7425 0.066 Uiso 1 1 calc R . .
C60 C 1.2261(5) -0.2547(6) 0.6981(4) 0.0558(18) Uani 1 1 d . . .
C61 C 1.1043(13) -0.3449(15) 0.9456(11) 0.146(6) Uani 1 1 d . . .
H61 H 1.1493 -0.4025 0.9417 0.175 Uiso 0.50 1 calc PR A 1
H H 0.94(3) -0.60(3) 1.07(2) 0.175 Uiso 0.50 1 d P B 2
C62 C 0.470(3) -0.461(3) 0.498(2) 0.171(16) Uani 0.50 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
Dy1 O5 2.250(4) . ?
Dy1 O6 2.250(4) . ?
Dy1 O7 2.200(4) . ?
Dy1 O8 2.354(4) . ?
Dy1 N1 2.610(5) . ?
Dy1 N2 2.600(5) . ?
Dy1 N3 2.592(5) . ?
Dy2 O1 2.250(4) . ?
Dy2 O2 2.251(4) . ?
Dy2 O3 2.339(4) . ?
Dy2 O4 2.185(4) . ?
Dy2 N4 2.661(5) . ?
Dy2 N5 2.573(5) . ?
Dy2 N6 2.615(5) . ?
Br1 C38 1.888(9) . ?
Br2 C40 1.913(7) . ?
Br3 C58 1.877(7) . ?
Br4 C60 1.899(6) . ?
Br5 C43 1.907(6) . ?
Br6 C41 1.897(7) . ?
Br7 C18 1.883(7) . ?
Br8 C16 1.889(7) . ?
Br9 C6 1.902(6) . ?
Br10 C8 1.886(7) . ?
Br11 C28 1.890(7) . ?
Br12 C30 1.906(6) . ?
Cl1 C61 1.69(2) . ?
Cl1' C61 1.76(2) . ?
Cl2 C61 1.84(3) . ?
Cl2' C61 1.62(2) . ?
Cl3 C61 1.77(2) . ?
Cl3' C61 1.67(3) . ?
Cl4 Cl5 1.572(19) 2_646 ?
Cl4 C62 1.62(5) . ?
Cl4 C62 2.21(5) 2_646 ?
Cl5 Cl4 1.572(19) 2_646 ?
Cl5 C62 1.57(4) . ?
Cl5 C62 1.72(4) 2_646 ?
Cl6 C62 1.52(5) . ?
Cl6 C62 2.13(5) 2_646 ?
O1 C9 1.316(7) . ?
O2 C27 1.315(6) . ?
O3 H3A 0.8500 . ?
O3 H3B 0.8500 . ?
O4 C19 1.311(7) . ?
O5 C37 1.323(7) . ?
O6 C57 1.311(7) . ?
O7 C46 1.302(7) . ?
O8 H8A 0.8500 . ?
O8 H8B 0.8500 . ?
N1 C52 1.322(9) . ?
N1 C56 1.371(8) . ?
N2 C32 1.331(10) . ?
N2 C36 1.371(10) . ?
N3 C45 1.364(7) . ?
N3 C49 1.337(7) . ?
N4 C22 1.328(8) . ?
N4 C26 1.367(8) . ?
N5 C12 1.333(8) . ?
N5 C20 1.382(7) . ?
N6 C2 1.331(8) . ?
N6 C10 1.370(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.490(9) . ?
C2 C3 1.410(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.353(10) . ?
C4 H4 0.9300 . ?
C4 C5 1.413(10) . ?
C5 C6 1.423(9) . ?
C5 C10 1.413(8) . ?
C6 C7 1.359(10) . ?
C7 H7 0.9300 . ?
C7 C8 1.403(9) . ?
C8 C9 1.396(8) . ?
C9 C10 1.421(9) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C11 C12 1.494(9) . ?
C12 C13 1.408(9) . ?
C13 H13 0.9300 . ?
C13 C14 1.373(10) . ?
C14 H14 0.9300 . ?
C14 C15 1.408(10) . ?
C15 C16 1.433(9) . ?
C15 C20 1.422(9) . ?
C16 C17 1.357(11) . ?
C17 H17 0.9300 . ?
C17 C18 1.405(10) . ?
C18 C19 1.390(8) . ?
C19 C20 1.426(9) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C21 C22 1.506(11) . ?
C22 C23 1.416(10) . ?
C23 H23 0.9300 . ?
C23 C24 1.347(12) . ?
C24 H24 0.9300 . ?
C24 C25 1.420(10) . ?
C25 C26 1.405(8) . ?
C25 C30 1.428(11) . ?
C26 C27 1.435(8) . ?
C27 C28 1.383(8) . ?
C28 C29 1.407(9) . ?
C29 H29 0.9300 . ?
C29 C30 1.343(11) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C31 C32 1.454(12) . ?
C32 C33 1.452(11) . ?
C33 H33 0.9300 . ?
C33 C34 1.301(13) . ?
C34 H34 0.9300 . ?
C34 C35 1.424(13) . ?
C35 C36 1.415(9) . ?
C35 C40 1.382(13) . ?
C36 C37 1.419(10) . ?
C37 C38 1.400(10) . ?
C38 C39 1.432(10) . ?
C39 H39 0.9300 . ?
C39 C40 1.331(13) . ?
C41 C42 1.409(9) . ?
C41 C46 1.389(8) . ?
C42 H42 0.9300 . ?
C42 C43 1.342(10) . ?
C43 C44 1.418(9) . ?
C44 C45 1.424(8) . ?
C44 C47 1.421(9) . ?
C45 C46 1.417(8) . ?
C47 H47 0.9300 . ?
C47 C48 1.354(9) . ?
C48 H48 0.9300 . ?
C48 C49 1.415(8) . ?
C49 C50 1.488(9) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C51 C52 1.459(11) . ?
C52 C53 1.444(10) . ?
C53 H53 0.9300 . ?
C53 C54 1.338(12) . ?
C54 H54 0.9300 . ?
C54 C55 1.386(11) . ?
C55 C56 1.433(8) . ?
C55 C60 1.433(11) . ?
C56 C57 1.431(9) . ?
C57 C58 1.387(8) . ?
C58 C59 1.420(9) . ?
C59 H59 0.9300 . ?
C59 C60 1.341(11) . ?
C61 H61 0.9800 . ?
C62 Cl4 2.21(5) 2_646 ?
C62 Cl5 1.72(4) 2_646 ?
C62 Cl6 2.13(5) 2_646 ?
C62 C62 1.30(7) 2_646 ?

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 Dy1 O6 82.47(14) . . ?
O5 Dy1 O8 90.30(14) . . ?
O5 Dy1 N1 144.65(15) . . ?
O5 Dy1 N2 66.56(17) . . ?
O5 Dy1 N3 86.64(14) . . ?
O6 Dy1 O8 91.09(14) . . ?
O6 Dy1 N1 66.49(15) . . ?
O6 Dy1 N2 146.58(17) . . ?
O6 Dy1 N3 86.11(14) . . ?
O7 Dy1 O5 131.33(16) . . ?
O7 Dy1 O6 131.70(15) . . ?
O7 Dy1 O8 117.27(15) . . ?
O7 Dy1 N1 83.57(16) . . ?
O7 Dy1 N2 80.62(18) . . ?
O7 Dy1 N3 66.63(15) . . ?
O8 Dy1 N1 74.48(14) . . ?
O8 Dy1 N2 77.38(15) . . ?
O8 Dy1 N3 176.09(15) . . ?
N2 Dy1 N1 136.48(18) . . ?
N3 Dy1 N1 106.77(14) . . ?
N3 Dy1 N2 103.56(15) . . ?
O1 Dy2 O2 77.20(14) . . ?
O1 Dy2 O3 100.65(15) . . ?
O1 Dy2 N4 141.72(15) . . ?
O1 Dy2 N5 88.29(15) . . ?
O1 Dy2 N6 65.91(15) . . ?
O2 Dy2 O3 95.93(15) . . ?
O2 Dy2 N4 65.11(15) . . ?
O2 Dy2 N5 90.09(15) . . ?
O2 Dy2 N6 139.21(15) . . ?
O3 Dy2 N4 77.75(15) . . ?
O3 Dy2 N5 170.12(15) . . ?
O3 Dy2 N6 75.29(14) . . ?
O4 Dy2 O1 134.57(16) . . ?
O4 Dy2 O2 137.14(15) . . ?
O4 Dy2 O3 102.75(15) . . ?
O4 Dy2 N4 81.55(17) . . ?
O4 Dy2 N5 67.68(16) . . ?
O4 Dy2 N6 83.24(16) . . ?
N5 Dy2 N4 97.85(16) . . ?
N5 Dy2 N6 105.05(15) . . ?
N6 Dy2 N4 145.12(16) . . ?
Cl5 Cl4 C62 65.2(19) 2_646 . ?
Cl5 Cl4 C62 45.3(14) 2_646 2_646 ?
C62 Cl4 C62 36(2) . 2_646 ?
Cl4 Cl5 C62 58.9(18) 2_646 2_646 ?
C62 Cl5 Cl4 89(2) . 2_646 ?
C62 Cl5 C62 46(2) . 2_646 ?
C62 Cl6 C62 37(2) . 2_646 ?
C9 O1 Dy2 125.4(4) . . ?
C27 O2 Dy2 124.9(4) . . ?
Dy2 O3 H3A 108.0 . . ?
Dy2 O3 H3B 108.0 . . ?
H3A O3 H3B 107.3 . . ?
C19 O4 Dy2 126.3(4) . . ?
C37 O5 Dy1 122.8(4) . . ?
C57 O6 Dy1 125.1(4) . . ?
C46 O7 Dy1 126.4(4) . . ?
Dy1 O8 H8A 108.0 . . ?
Dy1 O8 H8B 108.0 . . ?
H8A O8 H8B 107.3 . . ?
C52 N1 Dy1 128.1(4) . . ?
C52 N1 C56 119.9(5) . . ?
C56 N1 Dy1 111.6(4) . . ?
C32 N2 Dy1 128.0(5) . . ?
C32 N2 C36 120.3(6) . . ?
C36 N2 Dy1 110.9(4) . . ?
C45 N3 Dy1 111.8(4) . . ?
C49 N3 Dy1 128.9(4) . . ?
C49 N3 C45 119.3(5) . . ?
C22 N4 Dy2 129.1(5) . . ?
C22 N4 C26 118.5(5) . . ?
C26 N4 Dy2 111.4(4) . . ?
C12 N5 Dy2 130.5(4) . . ?
C12 N5 C20 118.5(5) . . ?
C20 N5 Dy2 111.0(4) . . ?
C2 N6 Dy2 128.1(4) . . ?
C2 N6 C10 119.0(5) . . ?
C10 N6 Dy2 112.7(4) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
N6 C2 C1 120.1(6) . . ?
N6 C2 C3 120.6(6) . . ?
C3 C2 C1 119.3(6) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.6(7) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 H4 120.4 . . ?
C3 C4 C5 119.1(6) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 125.6(6) . . ?
C10 C5 C4 116.9(6) . . ?
C10 C5 C6 117.5(6) . . ?
C5 C6 Br9 119.4(5) . . ?
C7 C6 Br9 118.6(5) . . ?
C7 C6 C5 122.0(6) . . ?
C6 C7 H7 120.5 . . ?
C6 C7 C8 119.0(6) . . ?
C8 C7 H7 120.5 . . ?
C7 C8 Br10 117.6(5) . . ?
C9 C8 Br10 119.5(5) . . ?
C9 C8 C7 122.9(6) . . ?
O1 C9 C8 123.5(6) . . ?
O1 C9 C10 119.8(5) . . ?
C8 C9 C10 116.7(5) . . ?
N6 C10 C5 122.8(6) . . ?
N6 C10 C9 115.4(5) . . ?
C5 C10 C9 121.9(6) . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
N5 C12 C11 118.9(6) . . ?
N5 C12 C13 121.9(6) . . ?
C13 C12 C11 119.2(6) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.3(7) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 120.1 . . ?
C13 C14 C15 119.8(6) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 C16 125.4(6) . . ?
C14 C15 C20 116.9(6) . . ?
C20 C15 C16 117.7(6) . . ?
C15 C16 Br8 119.2(6) . . ?
C17 C16 Br8 119.7(5) . . ?
C17 C16 C15 121.0(6) . . ?
C16 C17 H17 119.7 . . ?
C16 C17 C18 120.6(6) . . ?
C18 C17 H17 119.7 . . ?
C17 C18 Br7 118.8(5) . . ?
C19 C18 Br7 119.5(5) . . ?
C19 C18 C17 121.7(6) . . ?
O4 C19 C18 123.4(6) . . ?
O4 C19 C20 118.7(5) . . ?
C18 C19 C20 117.8(6) . . ?
N5 C20 C15 122.6(6) . . ?
N5 C20 C19 116.3(5) . . ?
C15 C20 C19 121.1(5) . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
N4 C22 C21 118.8(6) . . ?
N4 C22 C23 120.5(7) . . ?
C23 C22 C21 120.7(6) . . ?
C22 C23 H23 119.1 . . ?
C24 C23 C22 121.8(7) . . ?
C24 C23 H23 119.1 . . ?
C23 C24 H24 120.5 . . ?
C23 C24 C25 119.1(6) . . ?
C25 C24 H24 120.5 . . ?
C24 C25 C30 125.6(6) . . ?
C26 C25 C24 116.3(7) . . ?
C26 C25 C30 118.0(6) . . ?
N4 C26 C25 123.8(6) . . ?
N4 C26 C27 114.8(5) . . ?
C25 C26 C27 121.4(6) . . ?
O2 C27 C26 119.8(5) . . ?
O2 C27 C28 123.6(5) . . ?
C28 C27 C26 116.6(5) . . ?
C27 C28 Br11 118.8(4) . . ?
C27 C28 C29 122.8(6) . . ?
C29 C28 Br11 118.4(5) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 C28 119.7(7) . . ?
C30 C29 H29 120.1 . . ?
C25 C30 Br12 119.6(5) . . ?
C29 C30 Br12 118.9(6) . . ?
C29 C30 C25 121.5(6) . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
N2 C32 C31 120.8(7) . . ?
N2 C32 C33 118.1(8) . . ?
C33 C32 C31 121.1(8) . . ?
C32 C33 H33 118.6 . . ?
C34 C33 C32 122.7(9) . . ?
C34 C33 H33 118.6 . . ?
C33 C34 H34 120.0 . . ?
C33 C34 C35 120.1(7) . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 116.5(8) . . ?
C40 C35 C34 125.5(7) . . ?
C40 C35 C36 118.0(8) . . ?
N2 C36 C35 122.2(7) . . ?
N2 C36 C37 116.0(5) . . ?
C35 C36 C37 121.8(7) . . ?
O5 C37 C36 119.7(6) . . ?
O5 C37 C38 123.0(7) . . ?
C38 C37 C36 117.3(6) . . ?
C37 C38 Br1 119.5(5) . . ?
C37 C38 C39 119.7(8) . . ?
C39 C38 Br1 120.9(6) . . ?
C38 C39 H39 119.5 . . ?
C40 C39 C38 121.0(8) . . ?
C40 C39 H39 119.5 . . ?
C35 C40 Br2 120.7(7) . . ?
C39 C40 Br2 117.1(7) . . ?
C39 C40 C35 122.2(7) . . ?
C42 C41 Br6 118.0(5) . . ?
C46 C41 Br6 118.6(5) . . ?
C46 C41 C42 123.4(6) . . ?
C41 C42 H42 120.3 . . ?
C43 C42 C41 119.3(6) . . ?
C43 C42 H42 120.3 . . ?
C42 C43 Br5 118.5(5) . . ?
C42 C43 C44 121.6(6) . . ?
C44 C43 Br5 119.8(5) . . ?
C43 C44 C45 117.9(6) . . ?
C43 C44 C47 125.6(6) . . ?
C47 C44 C45 116.5(6) . . ?
N3 C45 C44 122.5(5) . . ?
N3 C45 C46 115.8(5) . . ?
C46 C45 C44 121.6(5) . . ?
O7 C46 C41 124.4(6) . . ?
O7 C46 C45 119.4(5) . . ?
C41 C46 C45 116.1(6) . . ?
C44 C47 H47 120.1 . . ?
C48 C47 C44 119.9(6) . . ?
C48 C47 H47 120.1 . . ?
C47 C48 H48 119.7 . . ?
C47 C48 C49 120.7(6) . . ?
C49 C48 H48 119.7 . . ?
N3 C49 C48 121.0(6) . . ?
N3 C49 C50 119.1(5) . . ?
C48 C49 C50 119.9(5) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C52 C51 H51A 109.5 . . ?
C52 C51 H51B 109.5 . . ?
C52 C51 H51C 109.5 . . ?
N1 C52 C51 119.5(6) . . ?
N1 C52 C53 119.5(7) . . ?
C53 C52 C51 121.0(7) . . ?
C52 C53 H53 119.2 . . ?
C54 C53 C52 121.6(7) . . ?
C54 C53 H53 119.2 . . ?
C53 C54 H54 120.1 . . ?
C53 C54 C55 119.7(7) . . ?
C55 C54 H54 120.1 . . ?
C54 C55 C56 117.7(7) . . ?
C54 C55 C60 126.0(6) . . ?
C56 C55 C60 116.3(7) . . ?
N1 C56 C55 121.6(6) . . ?
N1 C56 C57 116.4(5) . . ?
C57 C56 C55 122.0(6) . . ?
O6 C57 C56 119.2(5) . . ?
O6 C57 C58 123.7(6) . . ?
C58 C57 C56 117.1(5) . . ?
C57 C58 Br3 119.6(5) . . ?
C57 C58 C59 122.1(7) . . ?
C59 C58 Br3 118.3(5) . . ?
C58 C59 H59 120.0 . . ?
C60 C59 C58 120.0(7) . . ?
C60 C59 H59 120.0 . . ?
C55 C60 Br4 118.7(6) . . ?
C59 C60 Br4 118.8(6) . . ?
C59 C60 C55 122.5(6) . . ?
Cl1 C61 Cl1' 94.0(12) . . ?
Cl1 C61 Cl2 118.2(11) . . ?
Cl1 C61 Cl3 115.3(13) . . ?
Cl1 C61 H61 109.9 . . ?
Cl1' C61 Cl2 106.6(13) . . ?
Cl1' C61 Cl3 21.6(7) . . ?
Cl1' C61 H61 117.8 . . ?
Cl2 C61 H61 109.9 . . ?
Cl2' C61 Cl1 140.3(14) . . ?
Cl2' C61 Cl1' 105.3(12) . . ?
Cl2' C61 Cl2 89.4(12) . . ?
Cl2' C61 Cl3 89.2(11) . . ?
Cl2' C61 Cl3' 104.1(15) . . ?
Cl2' C61 H61 30.5 . . ?
Cl3 C61 Cl2 92.5(12) . . ?
Cl3 C61 H61 109.9 . . ?
Cl3' C61 Cl1 95.2(11) . . ?
Cl3' C61 Cl1' 120.0(15) . . ?
Cl3' C61 Cl2 24.7(6) . . ?
Cl3' C61 Cl3 112.0(14) . . ?
Cl3' C61 H61 114.0 . . ?
Cl4 C62 Cl4 144(2) . 2_646 ?
Cl4 C62 Cl5 55.9(16) . 2_646 ?
Cl4 C62 Cl6 95(2) . 2_646 ?
Cl5 C62 Cl4 45.4(14) . 2_646 ?
Cl5 C62 Cl4 97(2) 2_646 2_646 ?
Cl5 C62 Cl4 136(4) . . ?
Cl5 C62 Cl5 134(2) . 2_646 ?
Cl5 C62 Cl6 38.7(11) 2_646 2_646 ?
Cl5 C62 Cl6 106(2) . 2_646 ?
Cl6 C62 Cl4 95(2) . 2_646 ?
Cl6 C62 Cl4 61.6(13) 2_646 2_646 ?
Cl6 C62 Cl4 90(3) . . ?
Cl6 C62 Cl5 132(3) . 2_646 ?
Cl6 C62 Cl5 51.1(17) . . ?
Cl6 C62 Cl6 143(2) . 2_646 ?
C62 C62 Cl4 47(4) 2_646 2_646 ?
C62 C62 Cl4 97(5) 2_646 . ?
C62 C62 Cl5 61(3) 2_646 2_646 ?
C62 C62 Cl5 73(3) 2_646 . ?
C62 C62 Cl6 45(4) 2_646 2_646 ?
C62 C62 Cl6 98(5) 2_646 . ?

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 O5 C37 C36 -17.4(7) . . . . ?
Dy1 O5 C37 C38 161.5(5) . . . . ?
Dy1 O6 C57 C56 9.7(7) . . . . ?
Dy1 O6 C57 C58 -169.3(4) . . . . ?
Dy1 O7 C46 C41 -179.1(4) . . . . ?
Dy1 O7 C46 C45 0.9(8) . . . . ?
Dy1 N1 C52 C51 9.7(9) . . . . ?
Dy1 N1 C52 C53 -171.9(5) . . . . ?
Dy1 N1 C56 C55 173.5(5) . . . . ?
Dy1 N1 C56 C57 -7.2(6) . . . . ?
Dy1 N2 C32 C31 -13.2(10) . . . . ?
Dy1 N2 C32 C33 164.7(5) . . . . ?
Dy1 N2 C36 C35 -166.1(5) . . . . ?
Dy1 N2 C36 C37 13.8(7) . . . . ?
Dy1 N3 C45 C44 177.4(4) . . . . ?
Dy1 N3 C45 C46 -0.7(6) . . . . ?
Dy1 N3 C49 C48 -177.9(4) . . . . ?
Dy1 N3 C49 C50 3.2(7) . . . . ?
Dy2 O1 C9 C8 172.2(4) . . . . ?
Dy2 O1 C9 C10 -7.9(7) . . . . ?
Dy2 O2 C27 C26 18.5(7) . . . . ?
Dy2 O2 C27 C28 -161.0(4) . . . . ?
Dy2 O4 C19 C18 179.7(4) . . . . ?
Dy2 O4 C19 C20 -0.3(8) . . . . ?
Dy2 N4 C22 C21 15.3(9) . . . . ?
Dy2 N4 C22 C23 -164.5(5) . . . . ?
Dy2 N4 C26 C25 168.2(5) . . . . ?
Dy2 N4 C26 C27 -12.8(6) . . . . ?
Dy2 N5 C12 C11 0.5(9) . . . . ?
Dy2 N5 C12 C13 -178.8(5) . . . . ?
Dy2 N5 C20 C15 179.5(4) . . . . ?
Dy2 N5 C20 C19 -0.6(6) . . . . ?
Dy2 N6 C2 C1 -9.4(8) . . . . ?
Dy2 N6 C2 C3 172.3(5) . . . . ?
Dy2 N6 C10 C5 -174.5(5) . . . . ?
Dy2 N6 C10 C9 5.8(6) . . . . ?
Br1 C38 C39 C40 -179.2(6) . . . . ?
Br3 C58 C59 C60 179.2(5) . . . . ?
Br5 C43 C44 C45 -179.3(4) . . . . ?
Br5 C43 C44 C47 -0.1(8) . . . . ?
Br6 C41 C42 C43 178.0(5) . . . . ?
Br6 C41 C46 O7 1.2(8) . . . . ?
Br6 C41 C46 C45 -178.8(4) . . . . ?
Br7 C18 C19 O4 -0.7(8) . . . . ?
Br7 C18 C19 C20 179.3(4) . . . . ?
Br8 C16 C17 C18 179.6(5) . . . . ?
Br9 C6 C7 C8 -179.5(5) . . . . ?
Br10 C8 C9 O1 -2.7(8) . . . . ?
Br10 C8 C9 C10 177.3(4) . . . . ?
Br11 C28 C29 C30 179.5(5) . . . . ?
Cl4 Cl5 C62 Cl4 -128(4) 2_646 . . . ?
Cl4 Cl5 C62 Cl5 -45(5) 2_646 . . 2_646 ?
Cl4 Cl5 C62 Cl6 -160.3(14) 2_646 . . . ?
Cl4 Cl5 C62 Cl6 -14(2) 2_646 . . 2_646 ?
Cl4 Cl5 C62 C62 -45(5) 2_646 . . 2_646 ?
Cl5 Cl4 C62 Cl4 47(5) 2_646 . . 2_646 ?
Cl5 Cl4 C62 Cl5 120(4) 2_646 . . . ?
Cl5 Cl4 C62 Cl6 1.5(10) 2_646 . . 2_646 ?
Cl5 Cl4 C62 Cl6 145(2) 2_646 . . . ?
Cl5 Cl4 C62 C62 47(5) 2_646 . . 2_646 ?
O1 Dy2 O2 C27 169.1(5) . . . . ?
O1 Dy2 O4 C19 -63.3(5) . . . . ?
O1 Dy2 N4 C22 -165.9(5) . . . . ?
O1 Dy2 N4 C26 26.1(5) . . . . ?
O1 Dy2 N5 C12 -40.7(5) . . . . ?
O1 Dy2 N5 C20 140.8(4) . . . . ?
O1 Dy2 N6 C2 178.4(5) . . . . ?
O1 Dy2 N6 C10 -6.8(4) . . . . ?
O1 C9 C10 N6 0.1(8) . . . . ?
O1 C9 C10 C5 -179.6(5) . . . . ?
O2 Dy2 O1 C9 169.9(5) . . . . ?
O2 Dy2 O4 C19 63.9(5) . . . . ?
O2 Dy2 N4 C22 -176.7(6) . . . . ?
O2 Dy2 N4 C26 15.3(4) . . . . ?
O2 Dy2 N5 C12 36.5(5) . . . . ?
O2 Dy2 N5 C20 -142.0(4) . . . . ?
O2 Dy2 N6 C2 151.2(4) . . . . ?
O2 Dy2 N6 C10 -33.9(5) . . . . ?
O2 C27 C28 Br11 0.5(8) . . . . ?
O2 C27 C28 C29 -179.3(6) . . . . ?
O3 Dy2 O1 C9 76.2(4) . . . . ?
O3 Dy2 O2 C27 -91.2(4) . . . . ?
O3 Dy2 O4 C19 177.4(5) . . . . ?
O3 Dy2 N4 C22 -74.2(5) . . . . ?
O3 Dy2 N4 C26 117.9(4) . . . . ?
O3 Dy2 N5 C12 164.2(7) . . . . ?
O3 Dy2 N5 C20 -14.3(11) . . . . ?
O3 Dy2 N6 C2 69.3(5) . . . . ?
O3 Dy2 N6 C10 -115.8(4) . . . . ?
O4 Dy2 O1 C9 -43.9(5) . . . . ?
O4 Dy2 O2 C27 24.7(5) . . . . ?
O4 Dy2 N4 C22 30.9(5) . . . . ?
O4 Dy2 N4 C26 -137.0(4) . . . . ?
O4 Dy2 N5 C12 178.8(6) . . . . ?
O4 Dy2 N5 C20 0.3(4) . . . . ?
O4 Dy2 N6 C2 -35.8(5) . . . . ?
O4 Dy2 N6 C10 139.1(4) . . . . ?
O4 C19 C20 N5 0.6(8) . . . . ?
O4 C19 C20 C15 -179.5(5) . . . . ?
O5 Dy1 O6 C57 -172.3(4) . . . . ?
O5 Dy1 O7 C46 -63.2(5) . . . . ?
O5 Dy1 N1 C52 -148.4(5) . . . . ?
O5 Dy1 N1 C56 38.9(5) . . . . ?
O5 Dy1 N2 C32 174.5(6) . . . . ?
O5 Dy1 N2 C36 -15.8(4) . . . . ?
O5 Dy1 N3 C45 139.0(4) . . . . ?
O5 Dy1 N3 C49 -42.7(4) . . . . ?
O5 C37 C38 Br1 0.6(8) . . . . ?
O5 C37 C38 C39 -179.0(6) . . . . ?
O6 Dy1 O5 C37 -175.5(4) . . . . ?
O6 Dy1 O7 C46 60.2(5) . . . . ?
O6 Dy1 N1 C52 -179.0(6) . . . . ?
O6 Dy1 N1 C56 8.3(4) . . . . ?
O6 Dy1 N2 C32 150.9(5) . . . . ?
O6 Dy1 N2 C36 -39.4(6) . . . . ?
O6 Dy1 N3 C45 -138.3(4) . . . . ?
O6 Dy1 N3 C49 40.0(4) . . . . ?
O6 C57 C58 Br3 1.1(8) . . . . ?
O6 C57 C58 C59 -179.6(6) . . . . ?
O7 Dy1 O5 C37 -34.5(5) . . . . ?
O7 Dy1 O6 C57 47.0(5) . . . . ?
O7 Dy1 N1 C52 39.8(5) . . . . ?
O7 Dy1 N1 C56 -132.9(4) . . . . ?
O7 Dy1 N2 C32 -42.2(6) . . . . ?
O7 Dy1 N2 C36 127.5(4) . . . . ?
O7 Dy1 N3 C45 0.8(3) . . . . ?
O7 Dy1 N3 C49 179.0(5) . . . . ?
O8 Dy1 O5 C37 93.5(4) . . . . ?
O8 Dy1 O6 C57 -82.1(4) . . . . ?
O8 Dy1 O7 C46 179.4(4) . . . . ?
O8 Dy1 N1 C52 -80.8(5) . . . . ?
O8 Dy1 N1 C56 106.5(4) . . . . ?
O8 Dy1 N2 C32 78.6(6) . . . . ?
O8 Dy1 N2 C36 -111.7(4) . . . . ?
O8 Dy1 N3 C45 177.6(18) . . . . ?
O8 Dy1 N3 C49 -4(2) . . . . ?
N1 Dy1 O5 C37 156.4(4) . . . . ?
N1 Dy1 O6 C57 -9.6(4) . . . . ?
N1 Dy1 O7 C46 110.5(5) . . . . ?
N1 Dy1 N2 C32 28.0(7) . . . . ?
N1 Dy1 N2 C36 -162.3(4) . . . . ?
N1 Dy1 N3 C45 -74.3(4) . . . . ?
N1 Dy1 N3 C49 104.0(4) . . . . ?
N1 C52 C53 C54 -1.4(11) . . . . ?
N1 C56 C57 O6 -0.1(8) . . . . ?
N1 C56 C57 C58 178.9(5) . . . . ?
N2 Dy1 O5 C37 17.4(4) . . . . ?
N2 Dy1 O6 C57 -150.5(4) . . . . ?
N2 Dy1 O7 C46 -110.2(5) . . . . ?
N2 Dy1 N1 C52 -29.3(6) . . . . ?
N2 Dy1 N1 C56 158.0(4) . . . . ?
N2 Dy1 N3 C45 74.1(4) . . . . ?
N2 Dy1 N3 C49 -107.6(5) . . . . ?
N2 C32 C33 C34 2.5(12) . . . . ?
N2 C36 C37 O5 -0.3(8) . . . . ?
N2 C36 C37 C38 -179.2(6) . . . . ?
N3 Dy1 O5 C37 -89.0(4) . . . . ?
N3 Dy1 O6 C57 100.6(4) . . . . ?
N3 Dy1 O7 C46 -0.9(4) . . . . ?
N3 Dy1 N1 C52 103.0(5) . . . . ?
N3 Dy1 N1 C56 -69.7(4) . . . . ?
N3 Dy1 N2 C32 -105.2(6) . . . . ?
N3 Dy1 N2 C36 64.4(4) . . . . ?
N3 C45 C46 O7 0.1(8) . . . . ?
N3 C45 C46 C41 -180.0(5) . . . . ?
N4 Dy2 O1 C9 159.8(4) . . . . ?
N4 Dy2 O2 C27 -17.7(4) . . . . ?
N4 Dy2 O4 C19 102.1(5) . . . . ?
N4 Dy2 N5 C12 101.4(5) . . . . ?
N4 Dy2 N5 C20 -77.1(4) . . . . ?
N4 Dy2 N6 C2 28.8(6) . . . . ?
N4 Dy2 N6 C10 -156.3(4) . . . . ?
N4 C22 C23 C24 -1.8(11) . . . . ?
N4 C26 C27 O2 -0.6(8) . . . . ?
N4 C26 C27 C28 178.8(5) . . . . ?
N5 Dy2 O1 C9 -99.6(4) . . . . ?
N5 Dy2 O2 C27 80.9(4) . . . . ?
N5 Dy2 O4 C19 0.0(4) . . . . ?
N5 Dy2 N4 C22 96.8(6) . . . . ?
N5 Dy2 N4 C26 -71.1(4) . . . . ?
N5 Dy2 N6 C2 -100.5(5) . . . . ?
N5 Dy2 N6 C10 74.4(4) . . . . ?
N5 C12 C13 C14 0.4(10) . . . . ?
N6 Dy2 O1 C9 7.7(4) . . . . ?
N6 Dy2 O2 C27 -165.6(4) . . . . ?
N6 Dy2 O4 C19 -109.4(5) . . . . ?
N6 Dy2 N4 C22 -34.2(7) . . . . ?
N6 Dy2 N4 C26 157.9(4) . . . . ?
N6 Dy2 N5 C12 -105.2(5) . . . . ?
N6 Dy2 N5 C20 76.3(4) . . . . ?
N6 C2 C3 C4 1.7(10) . . . . ?
C1 C2 C3 C4 -176.6(7) . . . . ?
C2 N6 C10 C5 0.9(9) . . . . ?
C2 N6 C10 C9 -178.8(5) . . . . ?
C2 C3 C4 C5 0.4(11) . . . . ?
C3 C4 C5 C6 178.3(7) . . . . ?
C3 C4 C5 C10 -1.7(10) . . . . ?
C4 C5 C6 Br9 -0.5(9) . . . . ?
C4 C5 C6 C7 177.9(7) . . . . ?
C4 C5 C10 N6 1.1(9) . . . . ?
C4 C5 C10 C9 -179.2(6) . . . . ?
C5 C6 C7 C8 2.0(10) . . . . ?
C6 C5 C10 N6 -178.8(6) . . . . ?
C6 C5 C10 C9 0.8(9) . . . . ?
C6 C7 C8 Br10 -178.6(5) . . . . ?
C6 C7 C8 C9 -0.7(10) . . . . ?
C7 C8 C9 O1 179.5(6) . . . . ?
C7 C8 C9 C10 -0.5(9) . . . . ?
C8 C9 C10 N6 -179.9(5) . . . . ?
C8 C9 C10 C5 0.4(9) . . . . ?
C10 N6 C2 C1 176.0(6) . . . . ?
C10 N6 C2 C3 -2.3(9) . . . . ?
C10 C5 C6 Br9 179.5(5) . . . . ?
C10 C5 C6 C7 -2.1(10) . . . . ?
C11 C12 C13 C14 -178.9(7) . . . . ?
C12 N5 C20 C15 0.8(9) . . . . ?
C12 N5 C20 C19 -179.3(5) . . . . ?
C12 C13 C14 C15 -0.8(10) . . . . ?
C13 C14 C15 C16 -179.3(6) . . . . ?
C13 C14 C15 C20 1.1(9) . . . . ?
C14 C15 C16 Br8 1.6(9) . . . . ?
C14 C15 C16 C17 -179.6(6) . . . . ?
C14 C15 C20 N5 -1.1(9) . . . . ?
C14 C15 C20 C19 179.0(6) . . . . ?
C15 C16 C17 C18 0.7(10) . . . . ?
C16 C15 C20 N5 179.3(5) . . . . ?
C16 C15 C20 C19 -0.6(9) . . . . ?
C16 C17 C18 Br7 -180.0(5) . . . . ?
C16 C17 C18 C19 -0.9(10) . . . . ?
C17 C18 C19 O4 -179.8(6) . . . . ?
C17 C18 C19 C20 0.2(9) . . . . ?
C18 C19 C20 N5 -179.4(5) . . . . ?
C18 C19 C20 C15 0.5(9) . . . . ?
C20 N5 C12 C11 178.9(6) . . . . ?
C20 N5 C12 C13 -0.4(9) . . . . ?
C20 C15 C16 Br8 -178.8(4) . . . . ?
C20 C15 C16 C17 0.0(9) . . . . ?
C21 C22 C23 C24 178.4(7) . . . . ?
C22 N4 C26 C25 -1.2(9) . . . . ?
C22 N4 C26 C27 177.8(6) . . . . ?
C22 C23 C24 C25 -0.8(12) . . . . ?
C23 C24 C25 C26 2.1(10) . . . . ?
C23 C24 C25 C30 179.3(7) . . . . ?
C24 C25 C26 N4 -1.2(10) . . . . ?
C24 C25 C26 C27 179.8(6) . . . . ?
C24 C25 C30 Br12 0.8(10) . . . . ?
C24 C25 C30 C29 -178.9(7) . . . . ?
C25 C26 C27 O2 178.4(6) . . . . ?
C25 C26 C27 C28 -2.1(9) . . . . ?
C26 N4 C22 C21 -177.4(6) . . . . ?
C26 N4 C22 C23 2.7(9) . . . . ?
C26 C25 C30 Br12 178.0(5) . . . . ?
C26 C25 C30 C29 -1.8(10) . . . . ?
C26 C27 C28 Br11 -179.0(4) . . . . ?
C26 C27 C28 C29 1.2(9) . . . . ?
C27 C28 C29 C30 -0.7(10) . . . . ?
C28 C29 C30 Br12 -178.9(5) . . . . ?
C28 C29 C30 C25 0.9(11) . . . . ?
C30 C25 C26 N4 -178.6(6) . . . . ?
C30 C25 C26 C27 2.4(9) . . . . ?
C31 C32 C33 C34 -179.7(8) . . . . ?
C32 N2 C36 C35 4.5(10) . . . . ?
C32 N2 C36 C37 -175.6(6) . . . . ?
C32 C33 C34 C35 -0.8(13) . . . . ?
C33 C34 C35 C36 0.9(11) . . . . ?
C33 C34 C35 C40 179.7(8) . . . . ?
C34 C35 C36 N2 -2.7(10) . . . . ?
C34 C35 C36 C37 177.3(6) . . . . ?
C34 C35 C40 Br2 2.3(11) . . . . ?
C34 C35 C40 C39 -177.0(7) . . . . ?
C35 C36 C37 O5 179.7(6) . . . . ?
C35 C36 C37 C38 0.7(9) . . . . ?
C36 N2 C32 C31 178.0(7) . . . . ?
C36 N2 C32 C33 -4.2(10) . . . . ?
C36 C35 C40 Br2 -179.0(5) . . . . ?
C36 C35 C40 C39 1.7(11) . . . . ?
C36 C37 C38 Br1 179.5(4) . . . . ?
C36 C37 C38 C39 -0.1(9) . . . . ?
C37 C38 C39 C40 0.4(10) . . . . ?
C38 C39 C40 Br2 179.5(5) . . . . ?
C38 C39 C40 C35 -1.2(11) . . . . ?
C40 C35 C36 N2 178.4(6) . . . . ?
C40 C35 C36 C37 -1.5(10) . . . . ?
C41 C42 C43 Br5 179.8(5) . . . . ?
C41 C42 C43 C44 -0.4(9) . . . . ?
C42 C41 C46 O7 178.6(6) . . . . ?
C42 C41 C46 C45 -1.4(9) . . . . ?
C42 C43 C44 C45 0.9(9) . . . . ?
C42 C43 C44 C47 -179.9(6) . . . . ?
C43 C44 C45 N3 -179.7(5) . . . . ?
C43 C44 C45 C46 -1.8(8) . . . . ?
C43 C44 C47 C48 -179.3(6) . . . . ?
C44 C45 C46 O7 -178.0(5) . . . . ?
C44 C45 C46 C41 1.9(8) . . . . ?
C44 C47 C48 C49 -0.6(9) . . . . ?
C45 N3 C49 C48 0.2(8) . . . . ?
C45 N3 C49 C50 -178.7(5) . . . . ?
C45 C44 C47 C48 -0.2(9) . . . . ?
C46 C41 C42 C43 0.6(10) . . . . ?
C47 C44 C45 N3 1.0(8) . . . . ?
C47 C44 C45 C46 179.0(5) . . . . ?
C47 C48 C49 N3 0.6(9) . . . . ?
C47 C48 C49 C50 179.5(6) . . . . ?
C49 N3 C45 C44 -1.1(8) . . . . ?
C49 N3 C45 C46 -179.2(5) . . . . ?
C51 C52 C53 C54 177.0(7) . . . . ?
C52 N1 C56 C55 0.1(9) . . . . ?
C52 N1 C56 C57 179.4(6) . . . . ?
C52 C53 C54 C55 2.0(11) . . . . ?
C53 C54 C55 C56 -1.5(10) . . . . ?
C53 C54 C55 C60 178.9(7) . . . . ?
C54 C55 C56 N1 0.4(9) . . . . ?
C54 C55 C56 C57 -178.8(6) . . . . ?
C54 C55 C60 Br4 -1.6(10) . . . . ?
C54 C55 C60 C59 -179.8(7) . . . . ?
C55 C56 C57 O6 179.2(5) . . . . ?
C55 C56 C57 C58 -1.8(9) . . . . ?
C56 N1 C52 C51 -178.1(6) . . . . ?
C56 N1 C52 C53 0.3(9) . . . . ?
C56 C55 C60 Br4 178.9(5) . . . . ?
C56 C55 C60 C59 0.7(10) . . . . ?
C56 C57 C58 Br3 -177.9(4) . . . . ?
C56 C57 C58 C59 1.4(9) . . . . ?
C57 C58 C59 C60 0.0(10) . . . . ?
C58 C59 C60 Br4 -179.2(5) . . . . ?
C58 C59 C60 C55 -1.0(11) . . . . ?
C60 C55 C56 N1 -180.0(6) . . . . ?
C60 C55 C56 C57 0.8(9) . . . . ?
C62 Cl4 C62 Cl4 0.000(4) 2_646 . . 2_646 ?
C62 Cl4 C62 Cl5 -47(5) 2_646 . . 2_646 ?
C62 Cl4 C62 Cl5 74(4) 2_646 . . . ?
C62 Cl4 C62 Cl6 98(5) 2_646 . . . ?
C62 Cl4 C62 Cl6 -45(4) 2_646 . . 2_646 ?
C62 Cl5 C62 Cl4 -83(5) 2_646 . . . ?
C62 Cl5 C62 Cl4 45(5) 2_646 . . 2_646 ?
C62 Cl5 C62 Cl5 0.000(7) 2_646 . . 2_646 ?
C62 Cl5 C62 Cl6 32(3) 2_646 . . 2_646 ?
C62 Cl5 C62 Cl6 -115(5) 2_646 . . . ?
C62 Cl6 C62 Cl4 -97(5) 2_646 . . . ?
C62 Cl6 C62 Cl4 47(4) 2_646 . . 2_646 ?
C62 Cl6 C62 Cl5 -57(3) 2_646 . . 2_646 ?
C62 Cl6 C62 Cl5 61(4) 2_646 . . . ?
C62 Cl6 C62 Cl6 0.000(8) 2_646 . . 2_646 ?

####################################################################### 
# 
# 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_aaaa
_database_code_depnum_ccdc_archive 'CCDC 1856182'
_audit_update_record             
;
2018-07-15 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;
_audit_creation_date             2018-06-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C32 H20 Br4 Er N5 O5'
_chemical_formula_sum            'C32 H20 Br4 Er N5 O5'
_chemical_formula_weight         1041.43
_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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   13.552(4)
_cell_length_b                   16.758(5)
_cell_length_c                   14.397(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.625(4)
_cell_angle_gamma                90.00
_cell_volume                     3240.6(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.979
_cell_measurement_theta_min      2.289
_exptl_absorpt_coefficient_mu    7.572
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.135
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39105
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.52
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                5416
_reflns_number_total             6619
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.828
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6619
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0253
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0287P)²+1.9468P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0616
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C16(H16), C10(H10), C19(H19), C6(H6), C29(H29), C15(H15),
 C1(H1), C9(H9), C5(H5), C2(H2), C3(H3), C8(H8)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Er1 Er 0.709094(12) 0.422161(9) 0.282532(10) 0.03219(6) Uani 1 d . . .
Br4 Br 0.89339(4) 0.34179(3) 0.00099(3) 0.05756(12) Uani 1 d . . .
Br3 Br 0.82596(4) 0.65484(3) -0.13629(3) 0.06219(13) Uani 1 d . . .
Br2 Br 0.70353(4) 0.60437(3) 0.56869(3) 0.06497(14) Uani 1 d . . .
Br1 Br 1.03606(4) 0.43795(3) 0.74390(3) 0.07100(15) Uani 1 d . . .
O1 O 0.74152(19) 0.50411(14) 0.40059(16) 0.0389(6) Uani 1 d . . .
O2 O 0.7823(2) 0.40544(14) 0.15771(17) 0.0424(6) Uani 1 d . . .
O4 O 0.5389(2) 0.47681(17) 0.2822(2) 0.0493(7) Uani 1 d . . .
N4 N 0.7096(2) 0.55132(17) 0.1823(2) 0.0331(6) Uani 1 d . . .
N2 N 0.7099(2) 0.27249(17) 0.2702(2) 0.0359(7) Uani 1 d . . .
N3 N 0.8782(2) 0.38983(17) 0.3878(2) 0.0347(7) Uani 1 d . . .
N1 N 0.6317(2) 0.35101(17) 0.4072(2) 0.0366(7) Uani 1 d . . .
O3 O 0.5575(2) 0.37843(19) 0.1920(2) 0.0625(8) Uani 1 d . . .
C27 C 0.7640(3) 0.5975(2) 0.0350(3) 0.0378(8) Uani 1 d . . .
O5 O 0.4099(3) 0.4208(2) 0.2045(3) 0.0869(12) Uani 1 d . . .
N5 N 0.4991(3) 0.4257(2) 0.2262(3) 0.0512(9) Uani 1 d . . .
C14 C 0.9517(3) 0.3389(2) 0.3800(3) 0.0395(9) Uani 1 d . . .
C25 C 0.6839(3) 0.6860(2) 0.1308(3) 0.0528(11) Uani 1 d . . .
H25 H 0.6604 0.7366 0.1427 0.063 Uiso 1 calc . . R
C32 C 0.7542(2) 0.5374(2) 0.1029(2) 0.0322(8) Uani 1 d . . .
C26 C 0.7245(3) 0.6728(2) 0.0518(3) 0.0522(11) Uani 1 d . . .
H26 H 0.7265 0.7136 0.0083 0.063 Uiso 1 calc . . R
C21 C 0.8040(3) 0.48853(19) 0.4753(2) 0.0330(8) Uani 1 d . . .
C22 C 0.8786(3) 0.42885(19) 0.4731(2) 0.0335(8) Uani 1 d . . .
C28 C 0.8128(3) 0.5768(2) -0.0427(3) 0.0420(9) Uani 1 d . . .
C16 C 1.0228(3) 0.3553(2) 0.5400(3) 0.0503(10) Uani 1 d . . .
H16 H 1.0701 0.3416 0.5902 0.060 Uiso 1 calc . . R
C12 C 0.6247(3) 0.2696(2) 0.4060(2) 0.0362(8) Uani 1 d . . .
C30 C 0.8407(3) 0.4448(2) 0.0160(2) 0.0390(8) Uani 1 d . . .
C11 C 0.6669(3) 0.2284(2) 0.3332(2) 0.0354(8) Uani 1 d . . .
C31 C 0.7926(3) 0.4584(2) 0.0939(2) 0.0328(8) Uani 1 d . . .
C10 C 0.7432(3) 0.2337(2) 0.1999(3) 0.0432(9) Uani 1 d . . .
H10 H 0.7697 0.2634 0.1545 0.052 Uiso 1 calc . . R
C19 C 0.8729(3) 0.5128(2) 0.6390(3) 0.0446(9) Uani 1 d . . .
H19 H 0.8703 0.5412 0.6941 0.054 Uiso 1 calc . . R
C24 C 0.6766(3) 0.6243(2) 0.1957(3) 0.0400(9) Uani 1 d . . .
C6 C 0.6132(3) 0.1034(2) 0.3979(3) 0.0538(11) Uani 1 d . . .
H6 H 0.6105 0.0479 0.3963 0.065 Uiso 1 calc . . R
C13 C 0.9591(3) 0.3015(3) 0.2866(3) 0.0530(11) Uani 1 d . . .
H13A H 0.9327 0.2483 0.2855 0.080 Uiso 1 calc . . GR
H13B H 1.0276 0.2997 0.2764 0.080 Uiso 1 calc . . GR
H13C H 0.9217 0.3327 0.2382 0.080 Uiso 1 calc . . GR
C29 C 0.8510(3) 0.5032(2) -0.0512(3) 0.0429(9) Uani 1 d . . .
H29 H 0.8842 0.4913 -0.1019 0.051 Uiso 1 calc . . R
C17 C 0.9503(3) 0.4128(2) 0.5516(3) 0.0395(9) Uani 1 d . . .
C15 C 1.0239(3) 0.3200(2) 0.4563(3) 0.0481(10) Uani 1 d . . .
H15 H 1.0730 0.2827 0.4487 0.058 Uiso 1 calc . . R
C20 C 0.8031(3) 0.5275(2) 0.5605(3) 0.0398(9) Uani 1 d . . .
C1 C 0.5892(3) 0.3903(2) 0.4719(3) 0.0436(9) Uani 1 d . . .
H1 H 0.5935 0.4457 0.4735 0.052 Uiso 1 calc . . R
C7 C 0.6603(3) 0.1451(2) 0.3287(3) 0.0435(9) Uani 1 d . . .
C9 C 0.7403(3) 0.1510(2) 0.1909(3) 0.0494(10) Uani 1 d . . .
H9 H 0.7660 0.1264 0.1413 0.059 Uiso 1 calc . . R
C5 C 0.5733(3) 0.1424(3) 0.4647(3) 0.0579(12) Uani 1 d . . .
H5 H 0.5432 0.1137 0.5084 0.070 Uiso 1 calc . . R
C2 C 0.5382(3) 0.3519(3) 0.5374(3) 0.0517(11) Uani 1 d . . .
H2 H 0.5087 0.3816 0.5808 0.062 Uiso 1 calc . . R
C4 C 0.5759(3) 0.2279(2) 0.4703(3) 0.0448(9) Uani 1 d . . .
C18 C 0.9444(3) 0.4571(2) 0.6346(3) 0.0450(9) Uani 1 d . . .
C3 C 0.5320(3) 0.2716(3) 0.5375(3) 0.0529(11) Uani 1 d . . .
H3 H 0.4990 0.2455 0.5813 0.063 Uiso 1 calc . . R
C8 C 0.6997(3) 0.1066(2) 0.2549(3) 0.0517(11) Uani 1 d . . .
H8 H 0.6980 0.0512 0.2502 0.062 Uiso 1 calc . . R
C23 C 0.6304(3) 0.6429(2) 0.2819(3) 0.0502(10) Uani 1 d . . .
H23A H 0.6594 0.6095 0.3325 0.075 Uiso 1 calc . . GR
H23B H 0.5600 0.6332 0.2701 0.075 Uiso 1 calc . . GR
H23C H 0.6420 0.6979 0.2986 0.075 Uiso 1 calc . . GR


_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
Er1 O1 2.184(2) . ?
Er1 O2 2.183(2) . ?
Er1 O4 2.481(3) . ?
Er1 N4 2.602(3) . ?
Er1 N2 2.514(3) . ?
Er1 N3 2.631(3) . ?
Er1 N1 2.498(3) . ?
Er1 O3 2.397(3) . ?
Er1 N5 2.855(4) . ?
Br4 C30 1.891(4) . ?
Br3 C28 1.903(4) . ?
Br2 C20 1.880(4) . ?
Br1 C18 1.898(4) . ?
O1 C21 1.304(4) . ?
O2 C31 1.298(4) . ?
O4 N5 1.249(4) . ?
N4 C32 1.382(4) . ?
N4 C24 1.325(5) . ?
N2 C11 1.360(4) . ?
N2 C10 1.330(4) . ?
N3 C14 1.327(5) . ?
N3 C22 1.391(4) . ?
N1 C12 1.368(4) . ?
N1 C1 1.332(5) . ?
O3 N5 1.265(4) . ?
C27 C32 1.421(5) . ?
C27 C26 1.405(5) . ?
C27 C28 1.417(5) . ?
O5 N5 1.211(5) . ?
C14 C13 1.499(5) . ?
C14 C15 1.406(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.346(6) . ?
C25 C24 1.405(5) . ?
C32 C31 1.434(5) . ?
C26 H26 0.9300 . ?
C21 C22 1.426(5) . ?
C21 C20 1.391(5) . ?
C22 C17 1.415(5) . ?
C28 C29 1.350(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.402(6) . ?
C16 C15 1.345(6) . ?
C12 C11 1.435(5) . ?
C12 C4 1.394(5) . ?
C30 C31 1.389(5) . ?
C30 C29 1.395(5) . ?
C11 C7 1.399(5) . ?
C10 H10 0.9300 . ?
C10 C9 1.392(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.396(5) . ?
C19 C18 1.352(6) . ?
C24 C23 1.497(5) . ?
C6 H6 0.9300 . ?
C6 C7 1.435(6) . ?
C6 C5 1.335(6) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C29 H29 0.9300 . ?
C17 C18 1.418(6) . ?
C15 H15 0.9300 . ?
C1 H1 0.9300 . ?
C1 C2 1.398(5) . ?
C7 C8 1.407(6) . ?
C9 H9 0.9300 . ?
C9 C8 1.358(6) . ?
C5 H5 0.9300 . ?
C5 C4 1.434(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.348(6) . ?
C4 C3 1.407(6) . ?
C3 H3 0.9300 . ?
C8 H8 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?

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 Er1 O4 81.97(9) . . ?
O1 Er1 N4 83.89(9) . . ?
O1 Er1 N2 132.84(9) . . ?
O1 Er1 N3 67.13(9) . . ?
O1 Er1 N1 78.54(10) . . ?
O1 Er1 O3 133.22(10) . . ?
O1 Er1 N5 107.34(10) . . ?
O2 Er1 O1 130.91(10) . . ?
O2 Er1 O4 124.73(10) . . ?
O2 Er1 N4 67.37(9) . . ?
O2 Er1 N2 78.86(9) . . ?
O2 Er1 N3 89.50(9) . . ?
O2 Er1 N1 144.10(9) . . ?
O2 Er1 O3 87.92(11) . . ?
O2 Er1 N5 108.28(11) . . ?
O4 Er1 N4 76.27(9) . . ?
O4 Er1 N2 112.40(9) . . ?
O4 Er1 N3 144.66(9) . . ?
O4 Er1 N1 72.48(9) . . ?
O4 Er1 N5 25.87(9) . . ?
N4 Er1 N3 115.13(9) . . ?
N4 Er1 N5 84.31(9) . . ?
N2 Er1 N4 142.18(9) . . ?
N2 Er1 N3 79.84(9) . . ?
N2 Er1 N5 90.83(10) . . ?
N3 Er1 N5 158.05(9) . . ?
N1 Er1 N4 145.86(9) . . ?
N1 Er1 N2 65.24(9) . . ?
N1 Er1 N3 84.52(9) . . ?
N1 Er1 N5 73.53(10) . . ?
O3 Er1 O4 51.85(10) . . ?
O3 Er1 N4 91.02(10) . . ?
O3 Er1 N2 70.62(10) . . ?
O3 Er1 N3 150.29(10) . . ?
O3 Er1 N1 80.42(11) . . ?
O3 Er1 N5 26.06(10) . . ?
C21 O1 Er1 123.9(2) . . ?
C31 O2 Er1 126.7(2) . . ?
N5 O4 Er1 94.0(2) . . ?
C32 N4 Er1 110.6(2) . . ?
C24 N4 Er1 131.4(2) . . ?
C24 N4 C32 118.0(3) . . ?
C11 N2 Er1 119.2(2) . . ?
C10 N2 Er1 123.1(2) . . ?
C10 N2 C11 117.4(3) . . ?
C14 N3 Er1 133.6(3) . . ?
C14 N3 C22 117.5(3) . . ?
C22 N3 Er1 108.2(2) . . ?
C12 N1 Er1 120.1(2) . . ?
C1 N1 Er1 121.9(2) . . ?
C1 N1 C12 117.8(3) . . ?
N5 O3 Er1 97.6(2) . . ?
C26 C27 C32 116.5(3) . . ?
C26 C27 C28 125.7(3) . . ?
C28 C27 C32 117.8(3) . . ?
O4 N5 Er1 60.09(19) . . ?
O4 N5 O3 116.2(3) . . ?
O3 N5 Er1 56.32(19) . . ?
O5 N5 Er1 174.7(3) . . ?
O5 N5 O4 123.0(4) . . ?
O5 N5 O3 120.8(4) . . ?
N3 C14 C13 119.0(4) . . ?
N3 C14 C15 122.1(4) . . ?
C15 C14 C13 118.9(3) . . ?
C26 C25 H25 119.5 . . ?
C26 C25 C24 120.9(4) . . ?
C24 C25 H25 119.5 . . ?
N4 C32 C27 122.7(3) . . ?
N4 C32 C31 115.7(3) . . ?
C27 C32 C31 121.6(3) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 C27 120.0(4) . . ?
C25 C26 H26 120.0 . . ?
O1 C21 C22 120.4(3) . . ?
O1 C21 C20 123.5(3) . . ?
C20 C21 C22 116.0(3) . . ?
N3 C22 C21 115.5(3) . . ?
N3 C22 C17 122.5(3) . . ?
C17 C22 C21 121.9(3) . . ?
C27 C28 Br3 119.3(3) . . ?
C29 C28 Br3 119.5(3) . . ?
C29 C28 C27 121.3(3) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C15 C16 C17 120.0(4) . . ?
N1 C12 C11 117.1(3) . . ?
N1 C12 C4 122.0(3) . . ?
C4 C12 C11 120.9(3) . . ?
C31 C30 Br4 117.8(3) . . ?
C31 C30 C29 123.0(3) . . ?
C29 C30 Br4 119.1(3) . . ?
N2 C11 C12 118.3(3) . . ?
N2 C11 C7 122.8(3) . . ?
C7 C11 C12 119.0(3) . . ?
O2 C31 C32 119.5(3) . . ?
O2 C31 C30 124.4(3) . . ?
C30 C31 C32 116.0(3) . . ?
N2 C10 H10 118.3 . . ?
N2 C10 C9 123.3(4) . . ?
C9 C10 H10 118.3 . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C18 C19 C20 119.8(4) . . ?
N4 C24 C25 121.9(3) . . ?
N4 C24 C23 119.9(3) . . ?
C25 C24 C23 118.2(3) . . ?
C7 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C5 C6 C7 121.4(4) . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C28 C29 C30 120.3(3) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C22 C17 C18 117.7(3) . . ?
C16 C17 C22 116.9(4) . . ?
C16 C17 C18 125.4(4) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.8(4) . . ?
C16 C15 H15 119.6 . . ?
C21 C20 Br2 117.9(3) . . ?
C21 C20 C19 123.1(4) . . ?
C19 C20 Br2 119.0(3) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.8(4) . . ?
C2 C1 H1 118.6 . . ?
C11 C7 C6 119.0(4) . . ?
C11 C7 C8 117.7(4) . . ?
C8 C7 C6 123.3(4) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 C10 119.4(4) . . ?
C8 C9 H9 120.3 . . ?
C6 C5 H5 119.3 . . ?
C6 C5 C4 121.4(4) . . ?
C4 C5 H5 119.3 . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.8(4) . . ?
C3 C2 H2 120.1 . . ?
C12 C4 C5 118.2(4) . . ?
C12 C4 C3 118.5(4) . . ?
C3 C4 C5 123.3(4) . . ?
C19 C18 Br1 118.2(3) . . ?
C19 C18 C17 121.4(4) . . ?
C17 C18 Br1 120.4(3) . . ?
C2 C3 C4 119.1(4) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.3(4) . . ?
C9 C8 H8 120.4 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

_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_aaaa_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1856183'
_audit_update_record             
;
2018-07-15 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;
_audit_creation_date             2018-06-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C32 H20 Cl4 N5 O5 Tb'
_chemical_formula_sum            'C32 H20 Cl4 N5 O5 Tb'
_chemical_formula_weight         855.25
_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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   13.221(3)
_cell_length_b                   16.762(4)
_cell_length_c                   14.398(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.620(4)
_cell_angle_gamma                90.00
_cell_volume                     3162.6(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.453
_cell_measurement_theta_min      2.311
_exptl_absorpt_coefficient_mu    2.625
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29050
_diffrn_reflns_theta_full        26.55
_diffrn_reflns_theta_max         26.55
_diffrn_reflns_theta_min         1.87
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                5637
_reflns_number_total             6540
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6540
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0246
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0384P)²+2.5205P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0709
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C10(H10), C3(H3), C8(H8), C6(H6), C29(H29), C16(H16),
 C25(H25), C9(H9), C15(H15), C5(H5), C19(H19), C26(H26)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Tb1 Tb 0.290062(11) 0.425613(8) 0.717386(9) 0.03489(6) Uani 1 d . . .
Cl4 Cl 0.10827(8) 0.34702(6) 0.99933(7) 0.0641(3) Uani 1 d . . .
Cl2 Cl 0.28542(9) 0.60490(6) 0.43152(7) 0.0686(3) Uani 1 d . . .
Cl3 Cl 0.16229(9) 0.64659(7) 1.13227(7) 0.0695(3) Uani 1 d . . .
Cl1 Cl -0.03187(9) 0.43928(8) 0.25916(8) 0.0810(3) Uani 1 d . . .
O1 O 0.25611(17) 0.50777(12) 0.59680(14) 0.0426(5) Uani 1 d . . .
O2 O 0.21437(19) 0.40641(13) 0.84386(15) 0.0460(5) Uani 1 d . . .
N1 N 0.3719(2) 0.35218(15) 0.59142(17) 0.0398(6) Uani 1 d . . .
N4 N 0.28464(19) 0.55517(15) 0.82095(17) 0.0369(5) Uani 1 d . . .
O4 O 0.46723(18) 0.48116(14) 0.71854(17) 0.0525(6) Uani 1 d . . .
N3 N 0.11870(19) 0.39017(15) 0.60662(18) 0.0377(5) Uani 1 d . . .
N2 N 0.29085(18) 0.27413(15) 0.72918(17) 0.0383(6) Uani 1 d . . .
O3 O 0.4505(2) 0.38074(17) 0.80667(19) 0.0650(7) Uani 1 d . . .
C14 C 0.0457(2) 0.33666(18) 0.6127(2) 0.0433(7) Uani 1 d . . .
O5 O 0.6010(2) 0.42168(18) 0.7895(3) 0.0882(11) Uani 1 d . . .
C11 C 0.3337(2) 0.23010(18) 0.6660(2) 0.0367(6) Uani 1 d . . .
C1 C 0.4161(3) 0.3920(2) 0.5267(2) 0.0489(8) Uani 1 d . . .
H1 H 0.4124 0.4474 0.5254 0.059 Uiso 1 calc . . R
C17 C 0.0477(2) 0.41252(19) 0.4420(2) 0.0431(7) Uani 1 d . . .
N5 N 0.5099(2) 0.42770(17) 0.7715(2) 0.0510(7) Uani 1 d . . .
C32 C 0.2393(2) 0.53893(18) 0.90041(19) 0.0349(6) Uani 1 d . . .
C12 C 0.3775(2) 0.27155(18) 0.5930(2) 0.0373(6) Uani 1 d . . .
C21 C 0.1938(2) 0.49133(17) 0.5211(2) 0.0369(6) Uani 1 d . . .
C30 C 0.1537(2) 0.4430(2) 0.9865(2) 0.0436(7) Uani 1 d . . .
C27 C 0.2275(2) 0.5982(2) 0.9687(2) 0.0407(7) Uani 1 d . . .
C24 C 0.3167(2) 0.62893(19) 0.8090(2) 0.0428(7) Uani 1 d . . .
C22 C 0.1191(2) 0.42959(16) 0.5221(2) 0.0360(6) Uani 1 d . . .
C20 C 0.1952(3) 0.53103(18) 0.4367(2) 0.0436(7) Uani 1 d . . .
C31 C 0.2021(2) 0.45947(19) 0.9083(2) 0.0366(6) Uani 1 d . . .
C4 C 0.4269(3) 0.2282(2) 0.5280(2) 0.0470(8) Uani 1 d . . .
C2 C 0.4673(3) 0.3533(2) 0.4616(2) 0.0537(9) Uani 1 d . . .
H2 H 0.4974 0.3827 0.4178 0.064 Uiso 1 calc . . R
C10 C 0.2576(3) 0.2348(2) 0.7995(2) 0.0460(7) Uani 1 d . . .
H10 H 0.2316 0.2642 0.8457 0.055 Uiso 1 calc . . R
C13 C 0.0359(3) 0.2988(2) 0.7054(3) 0.0603(10) Uani 1 d . . .
H13A H 0.0650 0.2463 0.7074 0.090 Uiso 1 calc . . GR
H13B H -0.0349 0.2953 0.7134 0.090 Uiso 1 calc . . GR
H13C H 0.0714 0.3306 0.7548 0.090 Uiso 1 calc . . GR
C3 C 0.4733(3) 0.2730(2) 0.4617(2) 0.0552(9) Uani 1 d . . .
H3 H 0.5078 0.2471 0.4183 0.066 Uiso 1 calc . . R
C7 C 0.3401(3) 0.14607(19) 0.6700(2) 0.0459(8) Uani 1 d . . .
C8 C 0.3010(3) 0.1073(2) 0.7439(3) 0.0524(8) Uani 1 d . . .
H8 H 0.3038 0.0520 0.7488 0.063 Uiso 1 calc . . R
C6 C 0.3885(3) 0.1043(2) 0.5991(3) 0.0545(9) Uani 1 d . . .
H6 H 0.3907 0.0489 0.5998 0.065 Uiso 1 calc . . R
C29 C 0.1409(3) 0.5005(2) 1.0539(2) 0.0500(8) Uani 1 d . . .
H29 H 0.1068 0.4875 1.1044 0.060 Uiso 1 calc . . R
C18 C 0.0535(3) 0.4580(2) 0.3595(2) 0.0507(8) Uani 1 d . . .
C16 C -0.0239(3) 0.3521(2) 0.4498(3) 0.0547(9) Uani 1 d . . .
H16 H -0.0699 0.3370 0.3982 0.066 Uiso 1 calc . . R
C25 C 0.3080(3) 0.6895(2) 0.8753(3) 0.0521(8) Uani 1 d . . .
H25 H 0.3316 0.7405 0.8646 0.062 Uiso 1 calc . . R
C28 C 0.1781(3) 0.5753(2) 1.0463(2) 0.0466(8) Uani 1 d . . .
C9 C 0.2594(3) 0.1510(2) 0.8078(3) 0.0511(8) Uani 1 d . . .
H9 H 0.2323 0.1262 0.8567 0.061 Uiso 1 calc . . R
C15 C -0.0253(3) 0.3159(2) 0.5337(3) 0.0547(9) Uani 1 d . . .
H15 H -0.0737 0.2767 0.5397 0.066 Uiso 1 calc . . R
C5 C 0.4294(3) 0.1435(2) 0.5335(3) 0.0582(9) Uani 1 d . . .
H5 H 0.4606 0.1149 0.4899 0.070 Uiso 1 calc . . R
C19 C 0.1251(3) 0.5154(2) 0.3571(2) 0.0507(8) Uani 1 d . . .
H19 H 0.1277 0.5445 0.3025 0.061 Uiso 1 calc . . R
C26 C 0.2660(3) 0.6748(2) 0.9543(3) 0.0523(8) Uani 1 d . . .
H26 H 0.2626 0.7148 0.9985 0.063 Uiso 1 calc . . R
C23 C 0.3641(3) 0.6485(2) 0.7230(3) 0.0565(9) Uani 1 d . . .
H23A H 0.4368 0.6420 0.7358 0.085 Uiso 1 calc . . GR
H23B H 0.3486 0.7028 0.7050 0.085 Uiso 1 calc . . GR
H23C H 0.3374 0.6134 0.6730 0.085 Uiso 1 calc . . GR


_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 2.215(2) . ?
Tb1 O2 2.215(2) . ?
Tb1 N1 2.549(3) . ?
Tb1 N4 2.641(3) . ?
Tb1 O4 2.519(2) . ?
Tb1 N3 2.659(3) . ?
Tb1 N2 2.545(3) . ?
Tb1 O3 2.448(3) . ?
Tb1 N5 2.908(3) . ?
Cl4 C30 1.736(4) . ?
Cl2 C20 1.728(3) . ?
Cl3 C28 1.754(3) . ?
Cl1 C18 1.739(3) . ?
O1 C21 1.306(4) . ?
O2 C31 1.311(4) . ?
N1 C1 1.342(4) . ?
N1 C12 1.354(4) . ?
N4 C32 1.387(4) . ?
N4 C24 1.326(4) . ?
O4 N5 1.260(4) . ?
N3 C14 1.329(4) . ?
N3 C22 1.386(4) . ?
N2 C11 1.353(4) . ?
N2 C10 1.331(4) . ?
O3 N5 1.264(4) . ?
C14 C13 1.499(5) . ?
C14 C15 1.418(5) . ?
O5 N5 1.203(4) . ?
C11 C12 1.444(4) . ?
C11 C7 1.412(4) . ?
C1 H1 0.9300 . ?
C1 C2 1.388(5) . ?
C17 C22 1.419(4) . ?
C17 C18 1.422(5) . ?
C17 C16 1.402(5) . ?
C32 C27 1.421(4) . ?
C32 C31 1.430(4) . ?
C12 C4 1.411(4) . ?
C21 C22 1.432(4) . ?
C21 C20 1.388(4) . ?
C30 C31 1.394(4) . ?
C30 C29 1.395(5) . ?
C27 C28 1.419(5) . ?
C27 C26 1.407(5) . ?
C24 C25 1.408(5) . ?
C24 C23 1.497(5) . ?
C20 C19 1.400(5) . ?
C4 C3 1.416(5) . ?
C4 C5 1.422(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.348(5) . ?
C10 H10 0.9300 . ?
C10 C9 1.410(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C3 H3 0.9300 . ?
C7 C8 1.403(5) . ?
C7 C6 1.455(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.348(5) . ?
C6 H6 0.9300 . ?
C6 C5 1.323(6) . ?
C29 H29 0.9300 . ?
C29 C28 1.356(5) . ?
C18 C19 1.354(5) . ?
C16 H16 0.9300 . ?
C16 C15 1.354(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.352(5) . ?
C9 H9 0.9300 . ?
C15 H15 0.9300 . ?
C5 H5 0.9300 . ?
C19 H19 0.9300 . ?
C26 H26 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?

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 N1 78.67(8) . . ?
O1 Tb1 N4 85.04(8) . . ?
O1 Tb1 O4 82.35(8) . . ?
O1 Tb1 N3 66.47(8) . . ?
O1 Tb1 N2 132.17(8) . . ?
O1 Tb1 O3 132.38(8) . . ?
O1 Tb1 N5 107.10(9) . . ?
O2 Tb1 O1 131.93(9) . . ?
O2 Tb1 N1 142.72(8) . . ?
O2 Tb1 N4 66.80(8) . . ?
O2 Tb1 O4 124.72(8) . . ?
O2 Tb1 N3 91.07(8) . . ?
O2 Tb1 N2 78.37(8) . . ?
O2 Tb1 O3 88.74(9) . . ?
O2 Tb1 N5 109.02(9) . . ?
N1 Tb1 N4 147.66(8) . . ?
N1 Tb1 N3 82.74(8) . . ?
N1 Tb1 N5 72.12(8) . . ?
N4 Tb1 N3 115.96(8) . . ?
N4 Tb1 N5 86.54(8) . . ?
O4 Tb1 N1 72.61(8) . . ?
O4 Tb1 N4 77.71(8) . . ?
O4 Tb1 N3 143.53(8) . . ?
O4 Tb1 N2 111.89(8) . . ?
O4 Tb1 N5 25.59(8) . . ?
N3 Tb1 N5 154.86(8) . . ?
N2 Tb1 N1 64.36(8) . . ?
N2 Tb1 N4 141.54(8) . . ?
N2 Tb1 N3 79.21(8) . . ?
N2 Tb1 N5 89.94(8) . . ?
O3 Tb1 N1 78.78(9) . . ?
O3 Tb1 N4 92.44(9) . . ?
O3 Tb1 O4 50.94(8) . . ?
O3 Tb1 N3 148.89(9) . . ?
O3 Tb1 N2 70.29(9) . . ?
O3 Tb1 N5 25.50(8) . . ?
C21 O1 Tb1 124.26(18) . . ?
C31 O2 Tb1 126.55(19) . . ?
C1 N1 Tb1 121.3(2) . . ?
C1 N1 C12 118.7(3) . . ?
C12 N1 Tb1 119.85(19) . . ?
C32 N4 Tb1 110.57(18) . . ?
C24 N4 Tb1 131.4(2) . . ?
C24 N4 C32 118.1(3) . . ?
N5 O4 Tb1 94.71(18) . . ?
C14 N3 Tb1 132.8(2) . . ?
C14 N3 C22 117.8(3) . . ?
C22 N3 Tb1 108.56(18) . . ?
C11 N2 Tb1 119.86(19) . . ?
C10 N2 Tb1 123.1(2) . . ?
C10 N2 C11 116.8(3) . . ?
N5 O3 Tb1 98.0(2) . . ?
N3 C14 C13 119.6(3) . . ?
N3 C14 C15 121.4(3) . . ?
C15 C14 C13 119.0(3) . . ?
N2 C11 C12 118.1(3) . . ?
N2 C11 C7 123.0(3) . . ?
C7 C11 C12 118.8(3) . . ?
N1 C1 H1 118.9 . . ?
N1 C1 C2 122.2(3) . . ?
C2 C1 H1 118.9 . . ?
C22 C17 C18 117.9(3) . . ?
C16 C17 C22 117.6(3) . . ?
C16 C17 C18 124.5(3) . . ?
O4 N5 Tb1 59.69(16) . . ?
O4 N5 O3 115.7(3) . . ?
O3 N5 Tb1 56.49(17) . . ?
O5 N5 Tb1 173.7(3) . . ?
O5 N5 O4 123.0(3) . . ?
O5 N5 O3 121.3(3) . . ?
N4 C32 C27 122.2(3) . . ?
N4 C32 C31 116.1(3) . . ?
C27 C32 C31 121.7(3) . . ?
N1 C12 C11 117.8(3) . . ?
N1 C12 C4 122.1(3) . . ?
C4 C12 C11 120.0(3) . . ?
O1 C21 C22 120.3(3) . . ?
O1 C21 C20 123.3(3) . . ?
C20 C21 C22 116.4(3) . . ?
C31 C30 Cl4 118.2(3) . . ?
C31 C30 C29 122.4(3) . . ?
C29 C30 Cl4 119.4(3) . . ?
C28 C27 C32 117.4(3) . . ?
C26 C27 C32 117.4(3) . . ?
C26 C27 C28 125.2(3) . . ?
N4 C24 C25 121.9(3) . . ?
N4 C24 C23 119.2(3) . . ?
C25 C24 C23 118.9(3) . . ?
N3 C22 C17 122.6(3) . . ?
N3 C22 C21 115.8(3) . . ?
C17 C22 C21 121.5(3) . . ?
C21 C20 Cl2 118.1(2) . . ?
C21 C20 C19 122.9(3) . . ?
C19 C20 Cl2 119.0(3) . . ?
O2 C31 C32 119.9(3) . . ?
O2 C31 C30 123.4(3) . . ?
C30 C31 C32 116.7(3) . . ?
C12 C4 C3 117.0(3) . . ?
C12 C4 C5 119.1(3) . . ?
C3 C4 C5 123.9(3) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.0(3) . . ?
C3 C2 H2 120.0 . . ?
N2 C10 H10 118.2 . . ?
N2 C10 C9 123.6(3) . . ?
C9 C10 H10 118.2 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 120.0(3) . . ?
C2 C3 H3 120.0 . . ?
C11 C7 C6 118.8(3) . . ?
C8 C7 C11 117.8(3) . . ?
C8 C7 C6 123.4(3) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 C7 119.3(3) . . ?
C9 C8 H8 120.3 . . ?
C7 C6 H6 119.3 . . ?
C5 C6 C7 121.4(3) . . ?
C5 C6 H6 119.3 . . ?
C30 C29 H29 119.9 . . ?
C28 C29 C30 120.2(3) . . ?
C28 C29 H29 119.9 . . ?
C17 C18 Cl1 119.8(3) . . ?
C19 C18 Cl1 119.1(3) . . ?
C19 C18 C17 121.2(3) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 C17 119.0(3) . . ?
C15 C16 H16 120.5 . . ?
C24 C25 H25 119.4 . . ?
C26 C25 C24 121.2(3) . . ?
C26 C25 H25 119.4 . . ?
C27 C28 Cl3 118.8(3) . . ?
C29 C28 Cl3 119.6(3) . . ?
C29 C28 C27 121.6(3) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 C10 119.2(3) . . ?
C8 C9 H9 120.4 . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.4(3) . . ?
C16 C15 H15 119.3 . . ?
C4 C5 H5 119.1 . . ?
C6 C5 C4 121.8(3) . . ?
C6 C5 H5 119.1 . . ?
C20 C19 H19 119.9 . . ?
C18 C19 C20 120.1(3) . . ?
C18 C19 H19 119.9 . . ?
C27 C26 H26 120.4 . . ?
C25 C26 C27 119.2(3) . . ?
C25 C26 H26 120.4 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

_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_aaaa_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1856178'
_audit_update_record             
;
2018-07-15 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;
_audit_creation_date             2018-06-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C32 H20 Cl4 Ho N5 O5'
_chemical_formula_sum            'C32 H20 Cl4 Ho N5 O5'
_chemical_formula_weight         861.26
_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'
Ho Ho -0.2175 4.6783 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   13.2312(18)
_cell_length_b                   16.689(2)
_cell_length_c                   14.3530(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.769(2)
_cell_angle_gamma                90.00
_cell_volume                     3140.3(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.389
_cell_measurement_theta_min      2.313
_exptl_absorpt_coefficient_mu    2.911
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37976
_diffrn_reflns_theta_full        26.53
_diffrn_reflns_theta_max         26.53
_diffrn_reflns_theta_min         1.55
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                5530
_reflns_number_total             6486
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6486
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0222
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0355P)²+0.8047P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0637
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C3(H3), C2(H2), C19(H19), C29(H29), C8(H8), C25(H25),
 C16(H16), C15(H15), C9(H9), C26(H26), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Ho1 Ho 0.710312(10) 0.425308(7) 0.282654(8) 0.03432(5) Uani 1 d . . .
Cl4 Cl 0.89224(7) 0.34692(5) 0.00202(6) 0.0623(2) Uani 1 d . . .
Cl3 Cl 0.83561(8) 0.64707(6) -0.13183(6) 0.0672(3) Uani 1 d . . .
Cl2 Cl 0.71418(8) 0.60498(6) 0.56776(7) 0.0684(3) Uani 1 d . . .
Cl1 Cl 1.03109(9) 0.43865(7) 0.74086(7) 0.0796(3) Uani 1 d . . .
O1 O 0.74367(16) 0.50797(11) 0.40175(13) 0.0427(5) Uani 1 d . . .
O2 O 0.78660(17) 0.40649(12) 0.15823(14) 0.0447(5) Uani 1 d . . .
O4 O 0.53552(16) 0.48137(13) 0.28117(15) 0.0507(5) Uani 1 d . . .
N1 N 0.62902(18) 0.35385(14) 0.40832(16) 0.0388(5) Uani 1 d . . .
N4 N 0.71494(18) 0.55480(13) 0.18033(16) 0.0361(5) Uani 1 d . . .
N3 N 0.88074(17) 0.39016(14) 0.39198(17) 0.0369(5) Uani 1 d . . .
N2 N 0.70988(17) 0.27441(14) 0.27072(15) 0.0372(5) Uani 1 d . . .
O3 O 0.55244(18) 0.38063(15) 0.19333(17) 0.0628(6) Uani 1 d . . .
O5 O 0.4015(2) 0.42167(15) 0.2103(3) 0.0845(9) Uani 1 d . . .
C17 C 0.9521(2) 0.41226(17) 0.5575(2) 0.0431(7) Uani 1 d . . .
C11 C 0.6668(2) 0.23037(16) 0.33457(19) 0.0365(6) Uani 1 d . . .
C32 C 0.7603(2) 0.53892(16) 0.10119(18) 0.0334(6) Uani 1 d . . .
N5 N 0.4928(2) 0.42781(15) 0.2278(2) 0.0511(7) Uani 1 d . . .
C14 C 0.9541(2) 0.33641(17) 0.3859(2) 0.0440(7) Uani 1 d . . .
C12 C 0.6230(2) 0.27240(16) 0.40700(18) 0.0365(6) Uani 1 d . . .
C1 C 0.5848(2) 0.3934(2) 0.4725(2) 0.0457(7) Uani 1 d . . .
H1 H 0.5884 0.4490 0.4735 0.055 Uiso 1 calc . . R
C22 C 0.8806(2) 0.42935(15) 0.4771(2) 0.0360(6) Uani 1 d . . .
C30 C 0.8462(2) 0.44291(18) 0.0153(2) 0.0414(7) Uani 1 d . . .
C21 C 0.8059(2) 0.49141(15) 0.47793(19) 0.0372(6) Uani 1 d . . .
C27 C 0.7713(2) 0.59821(18) 0.0319(2) 0.0397(6) Uani 1 d . . .
C31 C 0.7978(2) 0.45910(17) 0.09280(19) 0.0362(6) Uani 1 d . . .
C24 C 0.6820(2) 0.62868(17) 0.1927(2) 0.0408(6) Uani 1 d . . .
C20 C 0.8045(2) 0.53121(17) 0.5623(2) 0.0431(7) Uani 1 d . . .
C4 C 0.5736(2) 0.22950(19) 0.4723(2) 0.0447(7) Uani 1 d . . .
C7 C 0.6600(2) 0.14618(17) 0.3304(2) 0.0430(7) Uani 1 d . . .
C10 C 0.7437(2) 0.23506(18) 0.2006(2) 0.0447(7) Uani 1 d . . .
H10 H 0.7710 0.2645 0.1550 0.054 Uiso 1 calc . . R
C3 C 0.5280(3) 0.2741(2) 0.5380(2) 0.0529(8) Uani 1 d . . .
H3 H 0.4938 0.2480 0.5817 0.063 Uiso 1 calc . . R
C2 C 0.5335(3) 0.3550(2) 0.5381(2) 0.0525(8) Uani 1 d . . .
H2 H 0.5032 0.3847 0.5817 0.063 Uiso 1 calc . . R
C19 C 0.8748(3) 0.51530(19) 0.6427(2) 0.0489(8) Uani 1 d . . .
H19 H 0.8723 0.5444 0.6976 0.059 Uiso 1 calc . . R
C29 C 0.8584(2) 0.5010(2) -0.0529(2) 0.0469(7) Uani 1 d . . .
H29 H 0.8924 0.4879 -0.1035 0.056 Uiso 1 calc . . R
C8 C 0.6992(2) 0.10721(19) 0.2569(2) 0.0509(8) Uani 1 d . . .
H8 H 0.6972 0.0516 0.2524 0.061 Uiso 1 calc . . R
C18 C 0.9456(2) 0.4578(2) 0.6400(2) 0.0494(8) Uani 1 d . . .
C25 C 0.6909(3) 0.68976(18) 0.1256(2) 0.0509(8) Uani 1 d . . .
H25 H 0.6671 0.7410 0.1360 0.061 Uiso 1 calc . . R
C16 C 1.0237(2) 0.3515(2) 0.5485(3) 0.0542(8) Uani 1 d . . .
H16 H 1.0700 0.3363 0.6001 0.065 Uiso 1 calc . . R
C28 C 0.8210(2) 0.57546(19) -0.0457(2) 0.0459(7) Uani 1 d . . .
C13 C 0.9643(3) 0.2990(2) 0.2928(3) 0.0595(9) Uani 1 d . . .
H13A H 0.9375 0.2455 0.2911 0.089 Uiso 1 calc . . GR
H13B H 1.0350 0.2973 0.2842 0.089 Uiso 1 calc . . GR
H13C H 0.9271 0.3302 0.2434 0.089 Uiso 1 calc . . GR
C15 C 1.0249(2) 0.3156(2) 0.4649(3) 0.0535(8) Uani 1 d . . .
H15 H 1.0733 0.2761 0.4589 0.064 Uiso 1 calc . . R
C9 C 0.7403(2) 0.15169(18) 0.1918(2) 0.0496(8) Uani 1 d . . .
H9 H 0.7659 0.1268 0.1419 0.059 Uiso 1 calc . . R
C26 C 0.7329(2) 0.67502(19) 0.0472(2) 0.0503(8) Uani 1 d . . .
H26 H 0.7367 0.7154 0.0032 0.060 Uiso 1 calc . . R
C5 C 0.5715(3) 0.1442(2) 0.4671(2) 0.0553(8) Uani 1 d . . .
H5 H 0.5407 0.1155 0.5111 0.066 Uiso 1 calc . . R
C6 C 0.6123(3) 0.1046(2) 0.4009(2) 0.0543(8) Uani 1 d . . .
H6 H 0.6101 0.0489 0.4002 0.065 Uiso 1 calc . . R
C23 C 0.6359(3) 0.64906(19) 0.2791(2) 0.0555(9) Uani 1 d . . .
H23A H 0.5634 0.6411 0.2673 0.083 Uiso 1 calc . . GR
H23B H 0.6501 0.7041 0.2955 0.083 Uiso 1 calc . . GR
H23C H 0.6645 0.6151 0.3299 0.083 Uiso 1 calc . . GR


_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
Ho1 O1 2.1946(19) . ?
Ho1 O2 2.1895(19) . ?
Ho1 O4 2.492(2) . ?
Ho1 N1 2.521(2) . ?
Ho1 N4 2.618(2) . ?
Ho1 N3 2.633(2) . ?
Ho1 N2 2.524(2) . ?
Ho1 O3 2.416(2) . ?
Ho1 N5 2.879(3) . ?
Cl4 C30 1.734(3) . ?
Cl3 C28 1.749(3) . ?
Cl2 C20 1.725(3) . ?
Cl1 C18 1.742(3) . ?
O1 C21 1.307(3) . ?
O2 C31 1.309(3) . ?
O4 N5 1.260(3) . ?
N1 C12 1.362(4) . ?
N1 C1 1.331(4) . ?
N4 C32 1.381(3) . ?
N4 C24 1.327(4) . ?
N3 C14 1.334(4) . ?
N3 C22 1.386(4) . ?
N2 C11 1.359(3) . ?
N2 C10 1.329(4) . ?
O3 N5 1.262(3) . ?
O5 N5 1.205(4) . ?
C17 C22 1.418(4) . ?
C17 C18 1.419(5) . ?
C17 C16 1.405(5) . ?
C11 C12 1.439(4) . ?
C11 C7 1.409(4) . ?
C32 C27 1.424(4) . ?
C32 C31 1.432(4) . ?
C14 C13 1.497(5) . ?
C14 C15 1.413(5) . ?
C12 C4 1.409(4) . ?
C1 H1 0.9300 . ?
C1 C2 1.390(4) . ?
C22 C21 1.433(4) . ?
C30 C31 1.383(4) . ?
C30 C29 1.402(4) . ?
C21 C20 1.383(4) . ?
C27 C28 1.419(4) . ?
C27 C26 1.407(4) . ?
C24 C25 1.418(4) . ?
C24 C23 1.493(4) . ?
C20 C19 1.406(4) . ?
C4 C3 1.400(5) . ?
C4 C5 1.425(4) . ?
C7 C8 1.397(4) . ?
C7 C6 1.441(5) . ?
C10 H10 0.9300 . ?
C10 C9 1.397(4) . ?
C3 H3 0.9300 . ?
C3 C2 1.352(5) . ?
C2 H2 0.9300 . ?
C19 H19 0.9300 . ?
C19 C18 1.346(5) . ?
C29 H29 0.9300 . ?
C29 C28 1.347(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.363(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.344(4) . ?
C16 H16 0.9300 . ?
C16 C15 1.344(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C15 H15 0.9300 . ?
C9 H9 0.9300 . ?
C26 H26 0.9300 . ?
C5 H5 0.9300 . ?
C5 C6 1.331(5) . ?
C6 H6 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?

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 Ho1 O4 81.91(7) . . ?
O1 Ho1 N1 78.49(8) . . ?
O1 Ho1 N4 84.29(7) . . ?
O1 Ho1 N3 67.05(7) . . ?
O1 Ho1 N2 132.72(7) . . ?
O1 Ho1 O3 132.50(8) . . ?
O1 Ho1 N5 106.98(8) . . ?
O2 Ho1 O1 131.23(8) . . ?
O2 Ho1 O4 125.20(8) . . ?
O2 Ho1 N1 143.50(7) . . ?
O2 Ho1 N4 67.21(7) . . ?
O2 Ho1 N3 90.12(8) . . ?
O2 Ho1 N2 78.38(7) . . ?
O2 Ho1 O3 89.07(8) . . ?
O2 Ho1 N5 109.46(9) . . ?
O4 Ho1 N1 72.46(7) . . ?
O4 Ho1 N4 77.13(7) . . ?
O4 Ho1 N3 143.86(7) . . ?
O4 Ho1 N2 112.36(7) . . ?
O4 Ho1 N5 25.86(7) . . ?
N1 Ho1 N4 146.75(7) . . ?
N1 Ho1 N3 83.23(7) . . ?
N1 Ho1 N2 65.12(7) . . ?
N1 Ho1 N5 72.25(8) . . ?
N4 Ho1 N3 115.79(7) . . ?
N4 Ho1 N5 86.16(7) . . ?
N3 Ho1 N5 155.48(8) . . ?
N2 Ho1 N4 141.76(7) . . ?
N2 Ho1 N3 79.17(7) . . ?
N2 Ho1 N5 90.17(7) . . ?
O3 Ho1 O4 51.44(8) . . ?
O3 Ho1 N1 79.16(8) . . ?
O3 Ho1 N4 92.36(8) . . ?
O3 Ho1 N3 148.94(8) . . ?
O3 Ho1 N2 70.26(8) . . ?
O3 Ho1 N5 25.72(8) . . ?
C21 O1 Ho1 123.82(16) . . ?
C31 O2 Ho1 126.76(17) . . ?
N5 O4 Ho1 94.48(17) . . ?
C12 N1 Ho1 119.48(18) . . ?
C1 N1 Ho1 122.0(2) . . ?
C1 N1 C12 118.3(3) . . ?
C32 N4 Ho1 110.41(17) . . ?
C24 N4 Ho1 131.20(18) . . ?
C24 N4 C32 118.4(2) . . ?
C14 N3 Ho1 133.1(2) . . ?
C14 N3 C22 117.6(3) . . ?
C22 N3 Ho1 108.51(17) . . ?
C11 N2 Ho1 119.42(17) . . ?
C10 N2 Ho1 123.13(19) . . ?
C10 N2 C11 117.3(3) . . ?
N5 O3 Ho1 98.08(18) . . ?
C22 C17 C18 117.5(3) . . ?
C16 C17 C22 117.0(3) . . ?
C16 C17 C18 125.5(3) . . ?
N2 C11 C12 118.0(2) . . ?
N2 C11 C7 122.7(3) . . ?
C7 C11 C12 119.2(3) . . ?
N4 C32 C27 122.5(3) . . ?
N4 C32 C31 116.2(2) . . ?
C27 C32 C31 121.2(3) . . ?
O4 N5 Ho1 59.66(15) . . ?
O4 N5 O3 115.4(3) . . ?
O3 N5 Ho1 56.20(15) . . ?
O5 N5 Ho1 173.2(2) . . ?
O5 N5 O4 122.8(3) . . ?
O5 N5 O3 121.8(3) . . ?
N3 C14 C13 119.6(3) . . ?
N3 C14 C15 121.4(3) . . ?
C15 C14 C13 118.9(3) . . ?
N1 C12 C11 117.9(2) . . ?
N1 C12 C4 122.0(3) . . ?
C4 C12 C11 120.1(3) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.8(3) . . ?
C2 C1 H1 118.6 . . ?
N3 C22 C17 122.8(3) . . ?
N3 C22 C21 115.5(2) . . ?
C17 C22 C21 121.6(3) . . ?
C31 C30 Cl4 118.5(2) . . ?
C31 C30 C29 122.4(3) . . ?
C29 C30 Cl4 119.1(2) . . ?
O1 C21 C22 120.3(2) . . ?
O1 C21 C20 123.3(3) . . ?
C20 C21 C22 116.4(3) . . ?
C28 C27 C32 117.6(3) . . ?
C26 C27 C32 116.8(3) . . ?
C26 C27 C28 125.5(3) . . ?
O2 C31 C32 119.3(2) . . ?
O2 C31 C30 123.8(3) . . ?
C30 C31 C32 116.9(3) . . ?
N4 C24 C25 121.2(3) . . ?
N4 C24 C23 120.1(3) . . ?
C25 C24 C23 118.7(3) . . ?
C21 C20 Cl2 118.3(2) . . ?
C21 C20 C19 122.9(3) . . ?
C19 C20 Cl2 118.8(2) . . ?
C12 C4 C5 118.7(3) . . ?
C3 C4 C12 117.3(3) . . ?
C3 C4 C5 124.1(3) . . ?
C11 C7 C6 118.8(3) . . ?
C8 C7 C11 117.9(3) . . ?
C8 C7 C6 123.2(3) . . ?
N2 C10 H10 118.3 . . ?
N2 C10 C9 123.4(3) . . ?
C9 C10 H10 118.3 . . ?
C4 C3 H3 119.8 . . ?
C2 C3 C4 120.3(3) . . ?
C2 C3 H3 119.8 . . ?
C1 C2 H2 120.3 . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 H2 120.3 . . ?
C20 C19 H19 120.1 . . ?
C18 C19 C20 119.7(3) . . ?
C18 C19 H19 120.1 . . ?
C30 C29 H29 119.8 . . ?
C28 C29 C30 120.4(3) . . ?
C28 C29 H29 119.8 . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.2(3) . . ?
C9 C8 H8 120.4 . . ?
C17 C18 Cl1 119.3(3) . . ?
C19 C18 Cl1 118.8(3) . . ?
C19 C18 C17 121.8(3) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 C24 121.2(3) . . ?
C26 C25 H25 119.4 . . ?
C17 C16 H16 120.2 . . ?
C15 C16 C17 119.6(3) . . ?
C15 C16 H16 120.2 . . ?
C27 C28 Cl3 118.6(2) . . ?
C29 C28 Cl3 120.0(2) . . ?
C29 C28 C27 121.4(3) . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.4(3) . . ?
C16 C15 H15 119.3 . . ?
C10 C9 H9 120.3 . . ?
C8 C9 C10 119.4(3) . . ?
C8 C9 H9 120.3 . . ?
C27 C26 H26 120.1 . . ?
C25 C26 C27 119.8(3) . . ?
C25 C26 H26 120.1 . . ?
C4 C5 H5 119.1 . . ?
C6 C5 C4 121.9(3) . . ?
C6 C5 H5 119.1 . . ?
C7 C6 H6 119.3 . . ?
C5 C6 C7 121.3(3) . . ?
C5 C6 H6 119.3 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

_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_lfp_whl_1242aaaa
_database_code_depnum_ccdc_archive 'CCDC 1856180'

_audit_update_record             
;
2018-07-15 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;
_audit_creation_date             2018-06-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H20 Cl4 Er N5 O5'
_chemical_formula_sum            'C32 H20 Cl4 Er N5 O5'
_chemical_formula_weight         863.59
_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'
Er Er -0.2586 4.9576 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   13.2305(3)
_cell_length_b                   16.6540(3)
_cell_length_c                   14.3223(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.802(2)
_cell_angle_gamma                90.00
_cell_volume                     3126.57(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11843
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9390
_cell_measurement_theta_min      3.9020
_exptl_absorpt_coefficient_mu    3.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           ?
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22262
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.31
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -22.00  87.00   1.00    5.00    --   10.68  77.00  30.00  109
  2  ω    -48.00  28.00   1.00    5.00    --   10.68 -77.00  60.00   76
  3  ω    -82.00  12.00   1.00    5.00    --  -11.93 -57.00 150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0469025000
_diffrn_orient_matrix_UB_12      -0.0100949000
_diffrn_orient_matrix_UB_13      -0.0158745000
_diffrn_orient_matrix_UB_21      -0.0131506000
_diffrn_orient_matrix_UB_22      -0.0412592000
_diffrn_orient_matrix_UB_23      0.0004563000
_diffrn_orient_matrix_UB_31      -0.0235753000
_diffrn_orient_matrix_UB_32      0.0029755000
_diffrn_orient_matrix_UB_33      -0.0474047000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                5233
_reflns_number_total             6131
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.065
_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     426
_refine_ls_number_reflns         6131
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0237
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0201P)²+1.8862P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0529
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1), C29(H29), C3(H3), C2(H2), C9(H9), C8(H8), C15(H15),
 C19(H19), C25(H25), C16(H16), C26(H26), C6(H6), C5(H5)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Er1 Er 0.289557(10) 0.574931(8) 0.717093(9) 0.03567(5) Uani 1 d . . .
Cl3 Cl 0.16507(8) 0.35320(6) 1.13174(6) 0.0684(3) Uani 1 d . . .
Cl4 Cl 0.10761(7) 0.65322(6) 0.99717(6) 0.0639(2) Uani 1 d . . .
Cl2 Cl 0.28586(8) 0.39485(6) 0.43275(7) 0.0688(3) Uani 1 d . . .
Cl1 Cl -0.03082(8) 0.56147(7) 0.25907(7) 0.0796(3) Uani 1 d . . .
O1 O 0.25633(15) 0.49210(12) 0.59910(13) 0.0429(5) Uani 1 d . . .
O2 O 0.21321(16) 0.59375(12) 0.84103(14) 0.0462(5) Uani 1 d . . .
O4 O 0.46354(16) 0.51850(13) 0.71860(15) 0.0514(5) Uani 1 d . . .
N4 N 0.28516(17) 0.44553(14) 0.81882(16) 0.0366(5) Uani 1 d . . .
N1 N 0.37068(18) 0.64573(14) 0.59204(16) 0.0391(6) Uani 1 d . . .
N2 N 0.28938(17) 0.72500(14) 0.72926(16) 0.0378(6) Uani 1 d . . .
N3 N 0.11933(18) 0.61011(14) 0.60846(17) 0.0379(5) Uani 1 d . . .
O3 O 0.44586(18) 0.61922(15) 0.80683(16) 0.0627(6) Uani 1 d . . .
O5 O 0.5973(2) 0.57801(16) 0.7903(2) 0.0853(9) Uani 1 d . . .
N5 N 0.5061(2) 0.57198(17) 0.7726(2) 0.0508(7) Uani 1 d . . .
C32 C 0.2399(2) 0.46121(17) 0.89832(19) 0.0345(6) Uani 1 d . . .
C11 C 0.3327(2) 0.76907(17) 0.6654(2) 0.0371(6) Uani 1 d . . .
C31 C 0.2019(2) 0.54084(18) 0.90623(19) 0.0373(7) Uani 1 d . . .
C14 C 0.0462(2) 0.66361(18) 0.6145(2) 0.0447(7) Uani 1 d . . .
C10 C 0.2561(2) 0.76456(18) 0.7996(2) 0.0444(7) Uani 1 d . . .
H10 H 0.2294 0.7351 0.8456 0.053 Uiso 1 calc . . R
C22 C 0.1192(2) 0.57058(16) 0.5233(2) 0.0373(7) Uani 1 d . . .
C1 C 0.4146(2) 0.6059(2) 0.5277(2) 0.0469(8) Uani 1 d . . .
H1 H 0.4106 0.5501 0.5267 0.056 Uiso 1 calc . . R
C12 C 0.3764(2) 0.72718(18) 0.59301(19) 0.0370(6) Uani 1 d . . .
C17 C 0.0483(2) 0.58779(18) 0.4427(2) 0.0442(8) Uani 1 d . . .
C30 C 0.1541(2) 0.55698(19) 0.9846(2) 0.0426(7) Uani 1 d . . .
C21 C 0.1940(2) 0.50876(16) 0.5227(2) 0.0383(7) Uani 1 d . . .
C24 C 0.3177(2) 0.37144(18) 0.8067(2) 0.0431(7) Uani 1 d . . .
C27 C 0.2291(2) 0.40209(19) 0.9674(2) 0.0409(7) Uani 1 d . . .
C20 C 0.1954(2) 0.46892(17) 0.4381(2) 0.0432(7) Uani 1 d . . .
C7 C 0.3393(2) 0.85340(18) 0.6695(2) 0.0438(7) Uani 1 d . . .
C29 C 0.1420(2) 0.4996(2) 1.0530(2) 0.0485(8) Uani 1 d . . .
H29 H 0.1083 0.5127 1.1038 0.058 Uiso 1 calc . . R
C3 C 0.4722(2) 0.7254(2) 0.4619(2) 0.0525(8) Uani 1 d . . .
H3 H 0.5069 0.7515 0.4184 0.063 Uiso 1 calc . . R
C2 C 0.4663(2) 0.6443(2) 0.4620(2) 0.0532(9) Uani 1 d . . .
H2 H 0.4965 0.6145 0.4184 0.064 Uiso 1 calc . . R
C9 C 0.2591(2) 0.84792(19) 0.8081(2) 0.0505(8) Uani 1 d . . .
H9 H 0.2332 0.8728 0.8580 0.061 Uiso 1 calc . . R
C8 C 0.2999(3) 0.8926(2) 0.7435(2) 0.0531(8) Uani 1 d . . .
H8 H 0.3018 0.9483 0.7481 0.064 Uiso 1 calc . . R
C15 C -0.0247(2) 0.6843(2) 0.5354(3) 0.0537(9) Uani 1 d . . .
H15 H -0.0733 0.7237 0.5415 0.064 Uiso 1 calc . . R
C13 C 0.0357(3) 0.7011(2) 0.7080(2) 0.0588(9) Uani 1 d . . .
H13A H 0.0741 0.6705 0.7574 0.088 Uiso 1 calc . . GR
H13B H -0.0349 0.7017 0.7170 0.088 Uiso 1 calc . . GR
H13C H 0.0611 0.7551 0.7093 0.088 Uiso 1 calc . . GR
C18 C 0.0547(2) 0.5426(2) 0.3604(2) 0.0499(8) Uani 1 d . . .
C19 C 0.1258(3) 0.4847(2) 0.3576(2) 0.0504(8) Uani 1 d . . .
H19 H 0.1284 0.4556 0.3026 0.060 Uiso 1 calc . . R
C28 C 0.1793(2) 0.4246(2) 1.0452(2) 0.0454(8) Uani 1 d . . .
C25 C 0.3092(3) 0.31049(19) 0.8736(2) 0.0519(8) Uani 1 d . . .
H25 H 0.3330 0.2591 0.8631 0.062 Uiso 1 calc . . R
C4 C 0.4260(2) 0.7701(2) 0.5275(2) 0.0463(8) Uani 1 d . . .
C16 C -0.0237(2) 0.6484(2) 0.4512(3) 0.0547(9) Uani 1 d . . .
H16 H -0.0701 0.6636 0.3995 0.066 Uiso 1 calc . . R
C23 C 0.3645(3) 0.35116(19) 0.7205(2) 0.0559(9) Uani 1 d . . .
H23A H 0.3366 0.3855 0.6696 0.084 Uiso 1 calc . . GR
H23B H 0.3499 0.2962 0.7036 0.084 Uiso 1 calc . . GR
H23C H 0.4370 0.3587 0.7329 0.084 Uiso 1 calc . . GR
C26 C 0.2672(2) 0.3256(2) 0.9523(2) 0.0525(8) Uani 1 d . . .
H26 H 0.2636 0.2852 0.9966 0.063 Uiso 1 calc . . R
C6 C 0.3876(3) 0.8950(2) 0.5994(2) 0.0532(8) Uani 1 d . . .
H6 H 0.3902 0.9508 0.6004 0.064 Uiso 1 calc . . R
C5 C 0.4286(3) 0.8552(2) 0.5332(2) 0.0566(9) Uani 1 d . . .
H5 H 0.4598 0.8840 0.4894 0.068 Uiso 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
Er1 O1 2.1795(19) . ?
Er1 O2 2.1809(19) . ?
Er1 O4 2.484(2) . ?
Er1 N4 2.606(2) . ?
Er1 N1 2.504(2) . ?
Er1 N2 2.505(2) . ?
Er1 N3 2.624(2) . ?
Er1 O3 2.398(2) . ?
Er1 N5 2.868(3) . ?
Cl3 C28 1.747(3) . ?
Cl4 C30 1.735(3) . ?
Cl2 C20 1.728(3) . ?
Cl1 C18 1.743(3) . ?
O1 C21 1.308(3) . ?
O2 C31 1.307(3) . ?
O4 N5 1.261(3) . ?
N4 C32 1.381(3) . ?
N4 C24 1.326(4) . ?
N1 C1 1.331(4) . ?
N1 C12 1.358(4) . ?
N2 C11 1.359(4) . ?
N2 C10 1.328(4) . ?
N3 C14 1.327(4) . ?
N3 C22 1.386(4) . ?
O3 N5 1.266(3) . ?
O5 N5 1.203(4) . ?
C32 C31 1.428(4) . ?
C32 C27 1.416(4) . ?
C11 C12 1.435(4) . ?
C11 C7 1.408(4) . ?
C31 C30 1.387(4) . ?
C14 C15 1.413(4) . ?
C14 C13 1.500(4) . ?
C10 H10 0.9300 . ?
C10 C9 1.394(4) . ?
C22 C17 1.415(4) . ?
C22 C21 1.429(4) . ?
C1 H1 0.9300 . ?
C1 C2 1.393(4) . ?
C12 C4 1.410(4) . ?
C17 C18 1.411(5) . ?
C17 C16 1.406(4) . ?
C30 C29 1.394(4) . ?
C21 C20 1.384(4) . ?
C24 C25 1.411(4) . ?
C24 C23 1.492(4) . ?
C27 C28 1.420(4) . ?
C27 C26 1.397(4) . ?
C20 C19 1.399(4) . ?
C7 C8 1.403(4) . ?
C7 C6 1.439(4) . ?
C29 H29 0.9300 . ?
C29 C28 1.352(4) . ?
C3 H3 0.9300 . ?
C3 C2 1.353(5) . ?
C3 C4 1.402(4) . ?
C2 H2 0.9300 . ?
C9 H9 0.9300 . ?
C9 C8 1.356(5) . ?
C8 H8 0.9300 . ?
C15 H15 0.9300 . ?
C15 C16 1.347(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C18 C19 1.351(5) . ?
C19 H19 0.9300 . ?
C25 H25 0.9300 . ?
C25 C26 1.347(4) . ?
C4 C5 1.421(5) . ?
C16 H16 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C26 H26 0.9300 . ?
C6 H6 0.9300 . ?
C6 C5 1.331(5) . ?
C5 H5 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
O1 Er1 O2 130.93(8) . . ?
O1 Er1 O4 81.74(7) . . ?
O1 Er1 N4 83.84(7) . . ?
O1 Er1 N1 78.72(8) . . ?
O1 Er1 N2 133.10(7) . . ?
O1 Er1 N3 67.36(7) . . ?
O1 Er1 O3 132.74(8) . . ?
O1 Er1 N5 107.02(8) . . ?
O2 Er1 O4 125.34(8) . . ?
O2 Er1 N4 67.41(7) . . ?
O2 Er1 N1 143.63(7) . . ?
O2 Er1 N2 78.18(7) . . ?
O2 Er1 N3 89.74(8) . . ?
O2 Er1 O3 88.89(8) . . ?
O2 Er1 N5 109.43(8) . . ?
O4 Er1 N4 76.90(7) . . ?
O4 Er1 N1 72.41(7) . . ?
O4 Er1 N2 112.74(7) . . ?
O4 Er1 N3 144.05(7) . . ?
O4 Er1 N5 26.00(7) . . ?
N4 Er1 N3 115.69(7) . . ?
N4 Er1 N5 85.89(7) . . ?
N1 Er1 N4 146.44(7) . . ?
N1 Er1 N2 65.46(7) . . ?
N1 Er1 N3 83.54(7) . . ?
N1 Er1 N5 72.37(8) . . ?
N2 Er1 N4 141.78(7) . . ?
N2 Er1 N3 79.03(7) . . ?
N2 Er1 N5 90.47(8) . . ?
N3 Er1 N5 155.91(7) . . ?
O3 Er1 O4 51.75(8) . . ?
O3 Er1 N4 92.16(8) . . ?
O3 Er1 N1 79.42(8) . . ?
O3 Er1 N2 70.42(8) . . ?
O3 Er1 N3 149.03(8) . . ?
O3 Er1 N5 25.89(7) . . ?
C21 O1 Er1 123.54(17) . . ?
C31 O2 Er1 126.51(18) . . ?
N5 O4 Er1 94.27(17) . . ?
C32 N4 Er1 110.46(17) . . ?
C24 N4 Er1 131.58(19) . . ?
C24 N4 C32 118.0(2) . . ?
C1 N1 Er1 122.0(2) . . ?
C1 N1 C12 118.5(3) . . ?
C12 N1 Er1 119.42(18) . . ?
C11 N2 Er1 119.18(18) . . ?
C10 N2 Er1 123.5(2) . . ?
C10 N2 C11 117.1(3) . . ?
C14 N3 Er1 133.3(2) . . ?
C14 N3 C22 117.6(3) . . ?
C22 N3 Er1 108.31(17) . . ?
N5 O3 Er1 98.27(19) . . ?
O4 N5 Er1 59.73(15) . . ?
O4 N5 O3 115.1(3) . . ?
O3 N5 Er1 55.84(15) . . ?
O5 N5 Er1 173.1(2) . . ?
O5 N5 O4 122.7(3) . . ?
O5 N5 O3 122.2(3) . . ?
N4 C32 C31 115.9(2) . . ?
N4 C32 C27 122.7(3) . . ?
C27 C32 C31 121.4(3) . . ?
N2 C11 C12 118.2(3) . . ?
N2 C11 C7 122.7(3) . . ?
C7 C11 C12 119.1(3) . . ?
O2 C31 C32 119.6(2) . . ?
O2 C31 C30 123.8(3) . . ?
C30 C31 C32 116.6(3) . . ?
N3 C14 C15 121.5(3) . . ?
N3 C14 C13 119.7(3) . . ?
C15 C14 C13 118.9(3) . . ?
N2 C10 H10 118.2 . . ?
N2 C10 C9 123.5(3) . . ?
C9 C10 H10 118.2 . . ?
N3 C22 C17 122.9(3) . . ?
N3 C22 C21 115.4(3) . . ?
C17 C22 C21 121.6(3) . . ?
N1 C1 H1 118.7 . . ?
N1 C1 C2 122.6(3) . . ?
C2 C1 H1 118.7 . . ?
N1 C12 C11 117.8(3) . . ?
N1 C12 C4 121.9(3) . . ?
C4 C12 C11 120.3(3) . . ?
C18 C17 C22 117.8(3) . . ?
C16 C17 C22 117.2(3) . . ?
C16 C17 C18 125.0(3) . . ?
C31 C30 Cl4 118.1(2) . . ?
C31 C30 C29 123.0(3) . . ?
C29 C30 Cl4 119.0(2) . . ?
O1 C21 C22 120.4(3) . . ?
O1 C21 C20 123.3(3) . . ?
C20 C21 C22 116.2(3) . . ?
N4 C24 C25 121.5(3) . . ?
N4 C24 C23 119.8(3) . . ?
C25 C24 C23 118.6(3) . . ?
C32 C27 C28 117.7(3) . . ?
C26 C27 C32 117.0(3) . . ?
C26 C27 C28 125.3(3) . . ?
C21 C20 Cl2 118.2(2) . . ?
C21 C20 C19 123.1(3) . . ?
C19 C20 Cl2 118.7(2) . . ?
C11 C7 C6 118.8(3) . . ?
C8 C7 C11 117.9(3) . . ?
C8 C7 C6 123.2(3) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 C30 119.8(3) . . ?
C28 C29 H29 120.1 . . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.8(3) . . ?
C4 C3 H3 120.1 . . ?
C1 C2 H2 120.2 . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 H2 120.2 . . ?
C10 C9 H9 120.1 . . ?
C8 C9 C10 119.7(3) . . ?
C8 C9 H9 120.1 . . ?
C7 C8 H8 120.6 . . ?
C9 C8 C7 118.9(3) . . ?
C9 C8 H8 120.6 . . ?
C14 C15 H15 119.2 . . ?
C16 C15 C14 121.6(3) . . ?
C16 C15 H15 119.2 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C17 C18 Cl1 119.6(3) . . ?
C19 C18 Cl1 118.7(3) . . ?
C19 C18 C17 121.7(3) . . ?
C20 C19 H19 120.2 . . ?
C18 C19 C20 119.5(3) . . ?
C18 C19 H19 120.2 . . ?
C27 C28 Cl3 118.9(3) . . ?
C29 C28 Cl3 119.6(2) . . ?
C29 C28 C27 121.5(3) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 C24 120.9(3) . . ?
C26 C25 H25 119.5 . . ?
C12 C4 C5 118.5(3) . . ?
C3 C4 C12 117.6(3) . . ?
C3 C4 C5 124.0(3) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 C17 119.1(3) . . ?
C15 C16 H16 120.5 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C27 C26 H26 120.1 . . ?
C25 C26 C27 119.9(3) . . ?
C25 C26 H26 120.1 . . ?
C7 C6 H6 119.4 . . ?
C5 C6 C7 121.3(3) . . ?
C5 C6 H6 119.4 . . ?
C4 C5 H5 119.0 . . ?
C6 C5 C4 122.0(3) . . ?
C6 C5 H5 119.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.540
_oxdiff_exptl_absorpt_empirical_full_min 0.751

####################################################################### 
# 
# 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_aaaa_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1856179'
_audit_update_record             
;
2018-07-15 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;
_audit_creation_date             2018-06-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C32 H20 Br4 N5 O5 Tb'
_chemical_formula_sum            'C32 H20 Br4 N5 O5 Tb'
_chemical_formula_weight         1033.09
_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'
Br Br -0.2901 2.4595 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   13.5432(11)
_cell_length_b                   16.8109(13)
_cell_length_c                   14.4543(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.5140(10)
_cell_angle_gamma                90.00
_cell_volume                     3262.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9572
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.62
_cell_measurement_theta_min      2.29
_exptl_absorpt_coefficient_mu    7.116
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39266
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.52
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                5279
_reflns_number_total             6691
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6691
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0280
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0217P)²+4.7139P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0623
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C16(H16), C19(H19), C10(H10), C5(H5), C15(H15), C29(H29),
 C6(H6), C1(H1), C2(H2), C9(H9), C3(H3), C8(H8)
2.b Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C23(H23a,H23b,H23c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Tb1 Tb 0.708731(14) 0.577241(11) 0.282274(12) 0.03341(6) Uani 1 d . . .
Br4 Br 0.89266(4) 0.65792(3) -0.00066(3) 0.05939(14) Uani 1 d . . .
Br3 Br 0.82840(4) 0.34517(3) -0.13677(3) 0.06446(15) Uani 1 d . . .
Br2 Br 0.70396(4) 0.39606(3) 0.57003(4) 0.06673(15) Uani 1 d . . .
Br1 Br 1.03746(4) 0.56148(4) 0.74370(4) 0.07355(17) Uani 1 d . . .
O1 O 0.7415(2) 0.49616(15) 0.40279(17) 0.0397(6) Uani 1 d . . .
O2 O 0.7812(2) 0.59429(15) 0.15506(18) 0.0432(7) Uani 1 d . . .
O4 O 0.5356(2) 0.52303(18) 0.2824(2) 0.0519(7) Uani 1 d . . .
N4 N 0.7101(2) 0.44799(18) 0.1803(2) 0.0344(7) Uani 1 d . . .
N2 N 0.7082(2) 0.72865(18) 0.2702(2) 0.0365(7) Uani 1 d . . .
N3 N 0.8790(2) 0.60980(18) 0.3896(2) 0.0350(7) Uani 1 d . . .
N1 N 0.6298(2) 0.65042(19) 0.4079(2) 0.0388(8) Uani 1 d . . .
C27 C 0.7647(3) 0.4024(2) 0.0333(3) 0.0389(9) Uani 1 d . . .
N5 N 0.4952(3) 0.5749(2) 0.2266(3) 0.0519(9) Uani 1 d . . .
O3 O 0.5539(2) 0.6215(2) 0.1922(2) 0.0656(9) Uani 1 d . . .
O5 O 0.4059(3) 0.5795(2) 0.2061(3) 0.0909(13) Uani 1 d . . .
C32 C 0.7547(3) 0.4624(2) 0.1005(2) 0.0317(8) Uani 1 d . . .
C14 C 0.9518(3) 0.6609(2) 0.3812(3) 0.0402(9) Uani 1 d . . .
C25 C 0.6851(3) 0.3139(2) 0.1289(3) 0.0518(11) Uani 1 d . . .
H25 H 0.6611 0.2636 0.1403 0.062 Uiso 1 calc . . R
C21 C 0.8045(3) 0.5116(2) 0.4775(3) 0.0349(8) Uani 1 d . . .
C12 C 0.6234(3) 0.7309(2) 0.4062(3) 0.0366(9) Uani 1 d . . .
C26 C 0.7266(3) 0.3266(3) 0.0505(3) 0.0518(11) Uani 1 d . . .
H26 H 0.7301 0.2855 0.0079 0.062 Uiso 1 calc . . R
C22 C 0.8797(3) 0.5712(2) 0.4740(3) 0.0337(8) Uani 1 d . . .
C31 C 0.7931(3) 0.5408(2) 0.0916(2) 0.0343(8) Uani 1 d . . .
C24 C 0.6772(3) 0.3751(2) 0.1939(3) 0.0405(9) Uani 1 d . . .
C16 C 1.0234(3) 0.6442(3) 0.5411(3) 0.0508(11) Uani 1 d . . .
H16 H 1.0709 0.6578 0.5910 0.061 Uiso 1 calc . . R
C19 C 0.8735(3) 0.4872(2) 0.6395(3) 0.0456(10) Uani 1 d . . .
H19 H 0.8707 0.4587 0.6943 0.055 Uiso 1 calc . . R
C30 C 0.8407(3) 0.5548(2) 0.0145(3) 0.0394(9) Uani 1 d . . .
C17 C 0.9510(3) 0.5868(2) 0.5531(3) 0.0406(9) Uani 1 d . . .
C20 C 0.8036(3) 0.4725(2) 0.5611(3) 0.0409(9) Uani 1 d . . .
C10 C 0.7422(3) 0.7672(2) 0.2004(3) 0.0433(10) Uani 1 d . . .
H10 H 0.7690 0.7376 0.1553 0.052 Uiso 1 calc . . R
C28 C 0.8143(3) 0.4235(3) -0.0438(3) 0.0444(10) Uani 1 d . . .
C11 C 0.6661(3) 0.7724(2) 0.3330(3) 0.0367(9) Uani 1 d . . .
C5 C 0.5724(4) 0.8590(3) 0.4642(3) 0.0567(12) Uani 1 d . . .
H5 H 0.5420 0.8879 0.5075 0.068 Uiso 1 calc . . R
C15 C 1.0246(3) 0.6797(3) 0.4578(3) 0.0500(11) Uani 1 d . . .
H15 H 1.0736 0.7170 0.4504 0.060 Uiso 1 calc . . R
C4 C 0.5750(3) 0.7739(3) 0.4699(3) 0.0470(10) Uani 1 d . . .
C29 C 0.8522(3) 0.4967(3) -0.0529(3) 0.0462(10) Uani 1 d . . .
H29 H 0.8857 0.5086 -0.1033 0.055 Uiso 1 calc . . R
C13 C 0.9593(3) 0.6983(3) 0.2896(3) 0.0561(12) Uani 1 d . . .
H13A H 0.9205 0.6684 0.2413 0.084 Uiso 1 calc . . GR
H13B H 1.0276 0.6991 0.2786 0.084 Uiso 1 calc . . GR
H13C H 0.9344 0.7518 0.2896 0.084 Uiso 1 calc . . GR
C7 C 0.6593(3) 0.8557(2) 0.3287(3) 0.0442(10) Uani 1 d . . .
C6 C 0.6129(4) 0.8977(3) 0.3978(3) 0.0563(12) Uani 1 d . . .
H6 H 0.6110 0.9529 0.3963 0.068 Uiso 1 calc . . R
C18 C 0.9452(3) 0.5430(3) 0.6354(3) 0.0475(11) Uani 1 d . . .
C1 C 0.5871(3) 0.6121(3) 0.4726(3) 0.0471(10) Uani 1 d . . .
H1 H 0.5909 0.5569 0.4744 0.057 Uiso 1 calc . . R
C2 C 0.5371(3) 0.6507(3) 0.5376(3) 0.0552(12) Uani 1 d . . .
H2 H 0.5077 0.6212 0.5812 0.066 Uiso 1 calc . . R
C9 C 0.7394(3) 0.8498(3) 0.1917(3) 0.0509(11) Uani 1 d . . .
H9 H 0.7654 0.8744 0.1426 0.061 Uiso 1 calc . . R
C3 C 0.5310(3) 0.7309(3) 0.5377(3) 0.0536(12) Uani 1 d . . .
H3 H 0.4984 0.7572 0.5815 0.064 Uiso 1 calc . . R
C8 C 0.6989(3) 0.8939(3) 0.2549(3) 0.0536(12) Uani 1 d . . .
H8 H 0.6971 0.9490 0.2499 0.064 Uiso 1 calc . . R
C23 C 0.6309(4) 0.3567(3) 0.2798(3) 0.0526(11) Uani 1 d . . .
H23A H 0.6617 0.3885 0.3307 0.079 Uiso 1 calc . . GR
H23B H 0.6402 0.3014 0.2950 0.079 Uiso 1 calc . . GR
H23C H 0.5609 0.3683 0.2688 0.079 Uiso 1 calc . . GR


_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 2.211(2) . ?
Tb1 O2 2.213(3) . ?
Tb1 O4 2.515(3) . ?
Tb1 N4 2.627(3) . ?
Tb1 N2 2.551(3) . ?
Tb1 N3 2.663(3) . ?
Tb1 N1 2.542(3) . ?
Tb1 N5 2.898(4) . ?
Tb1 O3 2.435(3) . ?
Br4 C30 1.894(4) . ?
Br3 C28 1.909(4) . ?
Br2 C20 1.880(4) . ?
Br1 C18 1.897(4) . ?
O1 C21 1.311(4) . ?
O2 C31 1.309(4) . ?
O4 N5 1.263(5) . ?
N4 C32 1.392(5) . ?
N4 C24 1.327(5) . ?
N2 C10 1.331(5) . ?
N2 C11 1.350(5) . ?
N3 C14 1.325(5) . ?
N3 C22 1.380(5) . ?
N1 C12 1.356(5) . ?
N1 C1 1.329(5) . ?
C27 C32 1.419(5) . ?
C27 C26 1.408(6) . ?
C27 C28 1.419(5) . ?
N5 O3 1.263(5) . ?
N5 O5 1.210(5) . ?
C32 C31 1.429(5) . ?
C14 C15 1.418(6) . ?
C14 C13 1.481(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.346(6) . ?
C25 C24 1.406(6) . ?
C21 C22 1.435(5) . ?
C21 C20 1.377(5) . ?
C12 C11 1.449(5) . ?
C12 C4 1.399(5) . ?
C26 H26 0.9300 . ?
C22 C17 1.422(5) . ?
C31 C30 1.380(5) . ?
C24 C23 1.495(5) . ?
C16 H16 0.9300 . ?
C16 C17 1.403(6) . ?
C16 C15 1.345(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.400(6) . ?
C19 C18 1.357(6) . ?
C30 C29 1.402(6) . ?
C17 C18 1.411(6) . ?
C10 H10 0.9300 . ?
C10 C9 1.395(6) . ?
C28 C29 1.347(6) . ?
C11 C7 1.405(5) . ?
C5 H5 0.9300 . ?
C5 C4 1.434(6) . ?
C5 C6 1.334(7) . ?
C15 H15 0.9300 . ?
C4 C3 1.410(6) . ?
C29 H29 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C7 C6 1.433(6) . ?
C7 C8 1.409(6) . ?
C6 H6 0.9300 . ?
C1 H1 0.9300 . ?
C1 C2 1.389(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.351(7) . ?
C9 H9 0.9300 . ?
C9 C8 1.347(6) . ?
C3 H3 0.9300 . ?
C8 H8 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?

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 O2 132.02(10) . . ?
O1 Tb1 O4 82.38(10) . . ?
O1 Tb1 N4 85.23(9) . . ?
O1 Tb1 N2 131.86(10) . . ?
O1 Tb1 N3 66.31(9) . . ?
O1 Tb1 N1 78.19(10) . . ?
O1 Tb1 N5 107.50(11) . . ?
O1 Tb1 O3 132.83(10) . . ?
O2 Tb1 O4 124.17(10) . . ?
O2 Tb1 N4 66.70(9) . . ?
O2 Tb1 N2 79.14(10) . . ?
O2 Tb1 N3 90.76(10) . . ?
O2 Tb1 N1 143.55(10) . . ?
O2 Tb1 N5 107.78(11) . . ?
O2 Tb1 O3 87.73(11) . . ?
O4 Tb1 N4 77.03(10) . . ?
O4 Tb1 N2 111.55(10) . . ?
O4 Tb1 N3 144.14(10) . . ?
O4 Tb1 N1 72.31(10) . . ?
O4 Tb1 N5 25.75(10) . . ?
N4 Tb1 N3 115.34(9) . . ?
N4 Tb1 N5 85.00(10) . . ?
N2 Tb1 N4 141.91(9) . . ?
N2 Tb1 N3 80.16(10) . . ?
N2 Tb1 N5 90.05(11) . . ?
N3 Tb1 N5 157.10(10) . . ?
N1 Tb1 N4 146.69(10) . . ?
N1 Tb1 N2 64.42(10) . . ?
N1 Tb1 N3 84.10(10) . . ?
N1 Tb1 N5 73.00(10) . . ?
O3 Tb1 O4 51.23(10) . . ?
O3 Tb1 N4 91.24(11) . . ?
O3 Tb1 N2 70.36(11) . . ?
O3 Tb1 N3 150.24(11) . . ?
O3 Tb1 N1 79.68(11) . . ?
O3 Tb1 N5 25.56(10) . . ?
C21 O1 Tb1 124.7(2) . . ?
C31 O2 Tb1 127.0(2) . . ?
N5 O4 Tb1 94.3(2) . . ?
C32 N4 Tb1 110.9(2) . . ?
C24 N4 Tb1 130.8(2) . . ?
C24 N4 C32 118.3(3) . . ?
C10 N2 Tb1 122.6(3) . . ?
C10 N2 C11 117.6(3) . . ?
C11 N2 Tb1 119.6(2) . . ?
C14 N3 Tb1 132.7(3) . . ?
C14 N3 C22 117.8(3) . . ?
C22 N3 Tb1 108.8(2) . . ?
C12 N1 Tb1 120.2(2) . . ?
C1 N1 Tb1 122.1(3) . . ?
C1 N1 C12 117.6(4) . . ?
C32 C27 C28 117.2(4) . . ?
C26 C27 C32 116.9(4) . . ?
C26 C27 C28 125.9(4) . . ?
O4 N5 Tb1 59.9(2) . . ?
O4 N5 O3 115.9(4) . . ?
O3 N5 Tb1 56.3(2) . . ?
O5 N5 Tb1 175.2(3) . . ?
O5 N5 O4 122.4(4) . . ?
O5 N5 O3 121.7(4) . . ?
N5 O3 Tb1 98.2(2) . . ?
N4 C32 C27 122.3(3) . . ?
N4 C32 C31 115.9(3) . . ?
C27 C32 C31 121.8(3) . . ?
N3 C14 C15 121.5(4) . . ?
N3 C14 C13 119.7(4) . . ?
C15 C14 C13 118.8(4) . . ?
C26 C25 H25 119.2 . . ?
C26 C25 C24 121.6(4) . . ?
C24 C25 H25 119.2 . . ?
O1 C21 C22 119.8(3) . . ?
O1 C21 C20 123.3(4) . . ?
C20 C21 C22 116.9(3) . . ?
N1 C12 C11 117.5(3) . . ?
N1 C12 C4 122.5(4) . . ?
C4 C12 C11 119.9(4) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 C27 119.6(4) . . ?
C25 C26 H26 120.2 . . ?
N3 C22 C21 115.9(3) . . ?
N3 C22 C17 123.3(3) . . ?
C17 C22 C21 120.8(4) . . ?
O2 C31 C32 119.4(3) . . ?
O2 C31 C30 124.2(4) . . ?
C30 C31 C32 116.3(3) . . ?
N4 C24 C25 121.3(4) . . ?
N4 C24 C23 120.0(4) . . ?
C25 C24 C23 118.7(4) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C15 C16 C17 120.3(4) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C18 C19 C20 119.9(4) . . ?
C31 C30 Br4 118.0(3) . . ?
C31 C30 C29 123.2(4) . . ?
C29 C30 Br4 118.8(3) . . ?
C16 C17 C22 116.2(4) . . ?
C16 C17 C18 125.5(4) . . ?
C18 C17 C22 118.3(4) . . ?
C21 C20 Br2 118.4(3) . . ?
C21 C20 C19 122.9(4) . . ?
C19 C20 Br2 118.7(3) . . ?
N2 C10 H10 118.5 . . ?
N2 C10 C9 123.0(4) . . ?
C9 C10 H10 118.5 . . ?
C27 C28 Br3 118.8(3) . . ?
C29 C28 Br3 119.1(3) . . ?
C29 C28 C27 122.1(4) . . ?
N2 C11 C12 118.3(3) . . ?
N2 C11 C7 122.9(4) . . ?
C7 C11 C12 118.8(4) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C6 C5 C4 121.2(4) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.8(4) . . ?
C16 C15 H15 119.6 . . ?
C12 C4 C5 119.1(4) . . ?
C12 C4 C3 118.0(4) . . ?
C3 C4 C5 122.9(4) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 C30 119.4(4) . . ?
C28 C29 H29 120.3 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C7 C6 119.5(4) . . ?
C11 C7 C8 117.3(4) . . ?
C8 C7 C6 123.2(4) . . ?
C5 C6 C7 121.4(4) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C19 C18 Br1 118.4(3) . . ?
C19 C18 C17 121.1(4) . . ?
C17 C18 Br1 120.4(3) . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.1(4) . . ?
C2 C1 H1 118.4 . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.1(4) . . ?
C3 C2 H2 120.0 . . ?
C10 C9 H9 120.1 . . ?
C8 C9 C10 119.7(4) . . ?
C8 C9 H9 120.1 . . ?
C4 C3 H3 120.7 . . ?
C2 C3 C4 118.7(4) . . ?
C2 C3 H3 120.7 . . ?
C7 C8 H8 120.3 . . ?
C9 C8 C7 119.4(4) . . ?
C9 C8 H8 120.3 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

_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_lfp_whl_10238aaaa
_database_code_depnum_ccdc_archive 'CCDC 1856176'
_audit_update_record             
;
2018-07-15 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;
_audit_creation_date             2018-06-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C32 H20 Br4 Ho N5 O5'
_chemical_formula_sum            'C32 H20 Br4 Ho N5 O5'
_chemical_formula_weight         1039.10
_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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   13.5558(2)
_cell_length_b                   16.7642(2)
_cell_length_c                   14.3978(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.6210(10)
_cell_angle_gamma                90.00
_cell_volume                     3243.03(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10496
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0720
_cell_measurement_theta_min      3.4160
_exptl_absorpt_coefficient_mu    7.418
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.128
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21530
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.27
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  52.00   1.00   15.00    --   10.68 -19.00-120.00  121
  2  ω    -20.00  23.00   1.00   15.00    --   10.68 -99.00-150.00   43
  3  ω    -15.00  65.00   1.00   15.00    --   10.68  57.00  60.00   80
  4  ω    -17.00  16.00   1.00   15.00    --  -11.93 -99.00 150.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0381215000
_diffrn_orient_matrix_UB_12      -0.0262500000
_diffrn_orient_matrix_UB_13      0.0102837000
_diffrn_orient_matrix_UB_21      -0.0348847000
_diffrn_orient_matrix_UB_22      0.0317240000
_diffrn_orient_matrix_UB_23      -0.0062078000
_diffrn_orient_matrix_UB_31      -0.0108718000
_diffrn_orient_matrix_UB_32      -0.0096665000
_diffrn_orient_matrix_UB_33      -0.0482363000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4792
_reflns_number_total             5687
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5687
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0242
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0210P)²+2.3004P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0523
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C25(H25), C10(H10), C19(H19), C29(H29), C16(H16), C1(H1), C5(H5),
 C2(H2), C15(H15), C9(H9), C3(H3), C8(H8), C6(H6)
2.b Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C23(H23a,H23b,H23c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Ho1 Ho 0.708970(12) 0.577669(10) 0.282311(10) 0.03445(6) Uani 1 d . . .
Br4 Br 0.89320(3) 0.65805(3) 0.00035(3) 0.05931(13) Uani 1 d . . .
Br3 Br 0.82654(4) 0.34498(3) -0.13665(3) 0.06382(13) Uani 1 d . . .
Br2 Br 0.70371(4) 0.39581(3) 0.56927(3) 0.06623(14) Uani 1 d . . .
Br1 Br 1.03668(4) 0.56201(3) 0.74397(3) 0.07267(15) Uani 1 d . . .
O1 O 0.74147(18) 0.49587(14) 0.40140(15) 0.0401(6) Uani 1 d . . .
O2 O 0.78210(19) 0.59456(14) 0.15671(15) 0.0434(6) Uani 1 d . . .
O4 O 0.5382(2) 0.52319(16) 0.28193(18) 0.0519(7) Uani 1 d . . .
N4 N 0.7097(2) 0.44856(17) 0.18138(18) 0.0344(7) Uani 1 d . . .
N2 N 0.7094(2) 0.72791(17) 0.27025(19) 0.0370(7) Uani 1 d . . .
N3 N 0.8784(2) 0.61014(17) 0.38846(18) 0.0362(7) Uani 1 d . . .
N1 N 0.6308(2) 0.64945(18) 0.40733(19) 0.0400(7) Uani 1 d . . .
O3 O 0.5563(2) 0.62183(19) 0.19245(19) 0.0644(8) Uani 1 d . . .
N5 N 0.4977(3) 0.5745(2) 0.2263(2) 0.0521(8) Uani 1 d . . .
C27 C 0.7638(3) 0.4024(2) 0.0346(2) 0.0395(9) Uani 1 d . . .
C32 C 0.7543(2) 0.4627(2) 0.1024(2) 0.0329(8) Uani 1 d . . .
O5 O 0.4084(2) 0.5792(2) 0.2054(3) 0.0878(11) Uani 1 d . . .
C14 C 0.9512(3) 0.6611(2) 0.3803(3) 0.0426(9) Uani 1 d . . .
C12 C 0.6245(3) 0.7306(2) 0.4061(2) 0.0377(8) Uani 1 d . . .
C26 C 0.7253(3) 0.3267(2) 0.0511(3) 0.0517(10) Uani 1 d . . .
H26 H 0.7285 0.2857 0.0082 0.062 Uiso 1 calc . . R
C31 C 0.7927(2) 0.5412(2) 0.0932(2) 0.0348(8) Uani 1 d . . .
C21 C 0.8044(3) 0.5117(2) 0.4758(2) 0.0353(8) Uani 1 d . . .
C25 C 0.6836(3) 0.3141(2) 0.1303(3) 0.0532(10) Uani 1 d . . .
H25 H 0.6593 0.2637 0.1419 0.064 Uiso 1 calc . . R
C11 C 0.6666(3) 0.7719(2) 0.3335(2) 0.0366(8) Uani 1 d . . .
C22 C 0.8791(2) 0.5710(2) 0.4736(2) 0.0345(8) Uani 1 d . . .
C30 C 0.8405(3) 0.5549(2) 0.0153(2) 0.0405(9) Uani 1 d . . .
C24 C 0.6764(3) 0.3756(2) 0.1950(2) 0.0407(9) Uani 1 d . . .
C17 C 0.9509(3) 0.5871(2) 0.5522(2) 0.0402(9) Uani 1 d . . .
C10 C 0.7430(3) 0.7668(2) 0.2003(3) 0.0466(9) Uani 1 d . . .
H10 H 0.7699 0.7373 0.1550 0.056 Uiso 1 calc . . R
C28 C 0.8128(3) 0.4234(2) -0.0432(2) 0.0449(9) Uani 1 d . . .
C13 C 0.9597(3) 0.6987(3) 0.2875(3) 0.0561(11) Uani 1 d . . .
H13A H 0.9228 0.6678 0.2386 0.084 Uiso 1 calc . . GR
H13B H 1.0284 0.7005 0.2779 0.084 Uiso 1 calc . . GR
H13C H 0.9334 0.7519 0.2864 0.084 Uiso 1 calc . . GR
C19 C 0.8736(3) 0.4874(2) 0.6393(2) 0.0457(9) Uani 1 d . . .
H19 H 0.8709 0.4591 0.6945 0.055 Uiso 1 calc . . R
C29 C 0.8512(3) 0.4967(2) -0.0520(2) 0.0448(9) Uani 1 d . . .
H29 H 0.8846 0.5085 -0.1027 0.054 Uiso 1 calc . . R
C16 C 1.0229(3) 0.6449(2) 0.5402(3) 0.0520(10) Uani 1 d . . .
H16 H 1.0701 0.6590 0.5904 0.062 Uiso 1 calc . . R
C1 C 0.5884(3) 0.6106(2) 0.4716(2) 0.0452(9) Uani 1 d . . .
H1 H 0.5925 0.5553 0.4733 0.054 Uiso 1 calc . . R
C4 C 0.5759(3) 0.7732(2) 0.4704(3) 0.0468(10) Uani 1 d . . .
C20 C 0.8037(3) 0.4723(2) 0.5607(2) 0.0416(9) Uani 1 d . . .
C5 C 0.5733(3) 0.8582(3) 0.4648(3) 0.0583(11) Uani 1 d . . .
H5 H 0.5433 0.8870 0.5087 0.070 Uiso 1 calc . . R
C2 C 0.5378(3) 0.6492(3) 0.5369(3) 0.0542(11) Uani 1 d . . .
H2 H 0.5082 0.6196 0.5804 0.065 Uiso 1 calc . . R
C15 C 1.0238(3) 0.6797(2) 0.4565(3) 0.0506(10) Uani 1 d . . .
H15 H 1.0731 0.7167 0.4487 0.061 Uiso 1 calc . . R
C18 C 0.9447(3) 0.5428(2) 0.6350(2) 0.0451(9) Uani 1 d . . .
C9 C 0.7398(3) 0.8496(2) 0.1915(3) 0.0504(10) Uani 1 d . . .
H9 H 0.7655 0.8743 0.1421 0.060 Uiso 1 calc . . R
C3 C 0.5319(3) 0.7294(3) 0.5369(3) 0.0559(11) Uani 1 d . . .
H3 H 0.4989 0.7555 0.5807 0.067 Uiso 1 calc . . R
C23 C 0.6305(3) 0.3570(2) 0.2817(3) 0.0516(10) Uani 1 d . . .
H23A H 0.6605 0.3898 0.3324 0.077 Uiso 1 calc . . GR
H23B H 0.6414 0.3018 0.2977 0.077 Uiso 1 calc . . GR
H23C H 0.5603 0.3675 0.2705 0.077 Uiso 1 calc . . GR
C8 C 0.6994(3) 0.8937(2) 0.2550(3) 0.0521(10) Uani 1 d . . .
H8 H 0.6978 0.9490 0.2502 0.063 Uiso 1 calc . . R
C7 C 0.6598(3) 0.8555(2) 0.3284(3) 0.0447(9) Uani 1 d . . .
C6 C 0.6129(3) 0.8974(3) 0.3977(3) 0.0565(11) Uani 1 d . . .
H6 H 0.6100 0.9528 0.3960 0.068 Uiso 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
Ho1 O1 2.194(2) . ?
Ho1 O2 2.193(2) . ?
Ho1 O4 2.488(3) . ?
Ho1 N4 2.608(3) . ?
Ho1 N2 2.525(3) . ?
Ho1 N3 2.641(3) . ?
Ho1 N1 2.514(3) . ?
Ho1 O3 2.407(3) . ?
Ho1 N5 2.871(3) . ?
Br4 C30 1.894(4) . ?
Br3 C28 1.909(4) . ?
Br2 C20 1.881(4) . ?
Br1 C18 1.898(3) . ?
O1 C21 1.305(4) . ?
O2 C31 1.300(4) . ?
O4 N5 1.251(4) . ?
N4 C32 1.377(4) . ?
N4 C24 1.328(4) . ?
N2 C11 1.361(4) . ?
N2 C10 1.330(4) . ?
N3 C14 1.323(4) . ?
N3 C22 1.390(4) . ?
N1 C12 1.364(4) . ?
N1 C1 1.323(4) . ?
O3 N5 1.266(4) . ?
N5 O5 1.211(4) . ?
C27 C32 1.423(5) . ?
C27 C26 1.403(5) . ?
C27 C28 1.420(5) . ?
C32 C31 1.428(5) . ?
C14 C13 1.496(5) . ?
C14 C15 1.408(5) . ?
C12 C11 1.434(5) . ?
C12 C4 1.401(5) . ?
C26 H26 0.9300 . ?
C26 C25 1.354(5) . ?
C31 C30 1.387(5) . ?
C21 C22 1.424(5) . ?
C21 C20 1.390(5) . ?
C25 H25 0.9300 . ?
C25 C24 1.402(5) . ?
C11 C7 1.404(5) . ?
C22 C17 1.416(5) . ?
C30 C29 1.396(5) . ?
C24 C23 1.499(5) . ?
C17 C16 1.402(5) . ?
C17 C18 1.416(5) . ?
C10 H10 0.9300 . ?
C10 C9 1.394(5) . ?
C28 C29 1.348(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C19 H19 0.9300 . ?
C19 C20 1.399(5) . ?
C19 C18 1.346(5) . ?
C29 H29 0.9300 . ?
C16 H16 0.9300 . ?
C16 C15 1.340(5) . ?
C1 H1 0.9300 . ?
C1 C2 1.394(5) . ?
C4 C5 1.427(6) . ?
C4 C3 1.401(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.337(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.348(6) . ?
C15 H15 0.9300 . ?
C9 H9 0.9300 . ?
C9 C8 1.347(5) . ?
C3 H3 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C8 H8 0.9300 . ?
C8 C7 1.402(5) . ?
C7 C6 1.437(5) . ?
C6 H6 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
O1 Ho1 O4 82.11(9) . . ?
O1 Ho1 N4 84.35(8) . . ?
O1 Ho1 N2 132.47(9) . . ?
O1 Ho1 N3 66.89(9) . . ?
O1 Ho1 N1 78.44(9) . . ?
O1 Ho1 O3 132.96(9) . . ?
O1 Ho1 N5 107.29(10) . . ?
O2 Ho1 O1 131.25(9) . . ?
O2 Ho1 O4 124.60(9) . . ?
O2 Ho1 N4 67.17(8) . . ?
O2 Ho1 N2 78.99(9) . . ?
O2 Ho1 N3 89.83(9) . . ?
O2 Ho1 N1 143.95(9) . . ?
O2 Ho1 O3 88.13(10) . . ?
O2 Ho1 N5 108.31(10) . . ?
O4 Ho1 N4 76.50(9) . . ?
O4 Ho1 N2 112.13(9) . . ?
O4 Ho1 N3 144.53(8) . . ?
O4 Ho1 N1 72.34(9) . . ?
O4 Ho1 N5 25.74(9) . . ?
N4 Ho1 N3 115.22(8) . . ?
N4 Ho1 N5 84.58(9) . . ?
N2 Ho1 N4 142.13(8) . . ?
N2 Ho1 N3 79.88(9) . . ?
N2 Ho1 N5 90.61(9) . . ?
N3 Ho1 N5 157.64(9) . . ?
N1 Ho1 N4 146.06(9) . . ?
N1 Ho1 N2 64.96(9) . . ?
N1 Ho1 N3 84.48(9) . . ?
N1 Ho1 N5 73.16(9) . . ?
O3 Ho1 O4 51.57(9) . . ?
O3 Ho1 N4 91.28(10) . . ?
O3 Ho1 N2 70.48(10) . . ?
O3 Ho1 N3 150.14(10) . . ?
O3 Ho1 N1 79.84(10) . . ?
O3 Ho1 N5 25.89(9) . . ?
C21 O1 Ho1 123.8(2) . . ?
C31 O2 Ho1 126.5(2) . . ?
N5 O4 Ho1 94.5(2) . . ?
C32 N4 Ho1 110.6(2) . . ?
C24 N4 Ho1 131.0(2) . . ?
C24 N4 C32 118.4(3) . . ?
C11 N2 Ho1 119.4(2) . . ?
C10 N2 Ho1 123.0(2) . . ?
C10 N2 C11 117.4(3) . . ?
C14 N3 Ho1 133.1(2) . . ?
C14 N3 C22 117.7(3) . . ?
C22 N3 Ho1 108.5(2) . . ?
C12 N1 Ho1 120.0(2) . . ?
C1 N1 Ho1 121.9(3) . . ?
C1 N1 C12 117.9(3) . . ?
N5 O3 Ho1 98.0(2) . . ?
O4 N5 Ho1 59.76(18) . . ?
O4 N5 O3 115.6(3) . . ?
O3 N5 Ho1 56.11(18) . . ?
O5 N5 Ho1 174.8(3) . . ?
O5 N5 O4 123.0(4) . . ?
O5 N5 O3 121.4(4) . . ?
C26 C27 C32 117.2(3) . . ?
C26 C27 C28 125.5(3) . . ?
C28 C27 C32 117.3(3) . . ?
N4 C32 C27 122.2(3) . . ?
N4 C32 C31 116.1(3) . . ?
C27 C32 C31 121.6(3) . . ?
N3 C14 C13 119.9(3) . . ?
N3 C14 C15 121.7(3) . . ?
C15 C14 C13 118.4(3) . . ?
N1 C12 C11 117.5(3) . . ?
N1 C12 C4 122.3(3) . . ?
C4 C12 C11 120.2(4) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 C27 119.3(3) . . ?
C25 C26 H26 120.3 . . ?
O2 C31 C32 119.5(3) . . ?
O2 C31 C30 124.2(3) . . ?
C30 C31 C32 116.3(3) . . ?
O1 C21 C22 120.9(3) . . ?
O1 C21 C20 123.1(3) . . ?
C20 C21 C22 116.0(3) . . ?
C26 C25 H25 119.4 . . ?
C26 C25 C24 121.2(4) . . ?
C24 C25 H25 119.4 . . ?
N2 C11 C12 118.2(3) . . ?
N2 C11 C7 122.5(3) . . ?
C7 C11 C12 119.3(3) . . ?
N3 C22 C21 115.3(3) . . ?
N3 C22 C17 122.6(3) . . ?
C17 C22 C21 122.1(3) . . ?
C31 C30 Br4 117.8(3) . . ?
C31 C30 C29 123.3(3) . . ?
C29 C30 Br4 118.9(3) . . ?
N4 C24 C25 121.6(3) . . ?
N4 C24 C23 120.1(3) . . ?
C25 C24 C23 118.3(3) . . ?
C16 C17 C22 116.7(3) . . ?
C16 C17 C18 125.9(4) . . ?
C18 C17 C22 117.5(3) . . ?
N2 C10 H10 118.4 . . ?
N2 C10 C9 123.1(4) . . ?
C9 C10 H10 118.4 . . ?
C27 C28 Br3 119.0(3) . . ?
C29 C28 Br3 119.1(3) . . ?
C29 C28 C27 121.9(3) . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C18 C19 C20 120.0(3) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 C30 119.6(3) . . ?
C28 C29 H29 120.2 . . ?
C17 C16 H16 120.0 . . ?
C15 C16 C17 120.0(4) . . ?
C15 C16 H16 120.0 . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.9(4) . . ?
C2 C1 H1 118.6 . . ?
C12 C4 C5 118.8(4) . . ?
C3 C4 C12 117.7(4) . . ?
C3 C4 C5 123.5(4) . . ?
C21 C20 Br2 118.0(3) . . ?
C21 C20 C19 122.8(3) . . ?
C19 C20 Br2 119.1(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.5(4) . . ?
C6 C5 H5 119.3 . . ?
C1 C2 H2 120.1 . . ?
C3 C2 C1 119.8(4) . . ?
C3 C2 H2 120.1 . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.1(4) . . ?
C16 C15 H15 119.5 . . ?
C17 C18 Br1 120.1(3) . . ?
C19 C18 Br1 118.4(3) . . ?
C19 C18 C17 121.6(3) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 C10 119.7(4) . . ?
C8 C9 H9 120.1 . . ?
C4 C3 H3 120.2 . . ?
C2 C3 C4 119.5(4) . . ?
C2 C3 H3 120.2 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C9 C8 H8 120.3 . . ?
C9 C8 C7 119.4(4) . . ?
C7 C8 H8 120.3 . . ?
C11 C7 C6 118.9(4) . . ?
C8 C7 C11 117.8(4) . . ?
C8 C7 C6 123.3(4) . . ?
C5 C6 C7 121.2(4) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.666
_oxdiff_exptl_absorpt_empirical_full_min 0.794
####################################################################### 
# 
# 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_mo_1113_2_0m
_database_code_depnum_ccdc_archive 'CCDC 1856181'

_audit_update_record             
;
2018-07-15 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;
_audit_creation_date             2018-06-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H20 Cl4 Dy N5 O5'
_chemical_formula_sum            'C32 H20 Cl4 Dy N5 O5'
_chemical_formula_weight         858.83
_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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   13.0622(6)
_cell_length_b                   16.6648(8)
_cell_length_c                   14.2828(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.7270(10)
_cell_angle_gamma                90.00
_cell_volume                     3080.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.322
_cell_measurement_theta_min      2.330
_exptl_absorpt_coefficient_mu    2.824
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0661 before and 0.0570 after correction.
The Ratio of minimum to maximum transmission is 0.8864.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1684
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           ?
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            50449
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         2.33
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                5053
_reflns_number_total             6328
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.519
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0284
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0233P)²+4.2844P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0619
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C8(H8), C16(H16), C29(H29), C3(H3), C25(H25), C26(H26),
 C9(H9), C10(H10), C15(H15), C6(H6), C19(H19), C5(H5)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Dy1 Dy 0.289364(13) 0.573984(10) 0.719865(11) 0.01715(5) Uani 1 d . . .
Cl4 Cl 0.10445(8) 0.65167(6) 1.00263(7) 0.0301(2) Uani 1 d . . .
Cl2 Cl 0.28506(8) 0.39429(6) 0.43198(7) 0.0324(2) Uani 1 d . . .
Cl3 Cl 0.16276(8) 0.35029(6) 1.13631(6) 0.0324(2) Uani 1 d . . .
Cl1 Cl -0.03698(8) 0.56205(7) 0.25899(7) 0.0382(3) Uani 1 d . . .
O1 O 0.25618(19) 0.49205(14) 0.59869(16) 0.0212(5) Uani 1 d . . .
O2 O 0.21346(19) 0.59343(14) 0.84666(16) 0.0219(6) Uani 1 d . . .
O4 O 0.46684(19) 0.51694(15) 0.71881(17) 0.0244(6) Uani 1 d . . .
N1 N 0.3718(2) 0.64696(17) 0.59384(19) 0.0202(6) Uani 1 d . . .
N3 N 0.1179(2) 0.61119(17) 0.6086(2) 0.0192(6) Uani 1 d . . .
O5 O 0.6049(2) 0.57787(18) 0.7873(2) 0.0394(7) Uani 1 d . . .
N4 N 0.2863(2) 0.44469(16) 0.82373(19) 0.0177(6) Uani 1 d . . .
O3 O 0.4508(2) 0.61931(16) 0.80779(18) 0.0300(6) Uani 1 d . . .
N2 N 0.2899(2) 0.72560(17) 0.73242(19) 0.0182(6) Uani 1 d . . .
C11 C 0.3328(3) 0.7700(2) 0.6678(2) 0.0177(7) Uani 1 d . . .
N5 N 0.5112(2) 0.57118(19) 0.7718(2) 0.0236(7) Uani 1 d . . .
C12 C 0.3772(3) 0.7284(2) 0.5947(2) 0.0188(7) Uani 1 d . . .
C14 C 0.0444(3) 0.6655(2) 0.6149(3) 0.0216(8) Uani 1 d . . .
C7 C 0.3381(3) 0.8549(2) 0.6718(2) 0.0222(8) Uani 1 d . . .
C22 C 0.1175(3) 0.5717(2) 0.5233(2) 0.0178(7) Uani 1 d . . .
C1 C 0.4170(3) 0.6068(2) 0.5292(2) 0.0239(8) Uani 1 d . . .
H1 H 0.4141 0.5499 0.5287 0.029 Uiso 1 calc . . R
C17 C 0.0454(3) 0.5893(2) 0.4426(2) 0.0199(8) Uani 1 d . . .
C2 C 0.4684(3) 0.6458(2) 0.4622(2) 0.0243(8) Uani 1 d . . .
H2 H 0.5000 0.6156 0.4174 0.029 Uiso 1 calc . . R
C8 C 0.2989(3) 0.8939(2) 0.7466(3) 0.0251(8) Uani 1 d . . .
H8 H 0.3007 0.9507 0.7513 0.030 Uiso 1 calc . . R
C13 C 0.0349(3) 0.7039(2) 0.7087(3) 0.0296(9) Uani 1 d . . .
H13A H 0.0744 0.6727 0.7594 0.044 Uiso 1 calc . . GR
H13B H -0.0380 0.7052 0.7184 0.044 Uiso 1 calc . . GR
H13C H 0.0619 0.7588 0.7095 0.044 Uiso 1 calc . . GR
C4 C 0.4260(3) 0.7721(2) 0.5283(2) 0.0225(8) Uani 1 d . . .
C32 C 0.2401(3) 0.4597(2) 0.9032(2) 0.0175(7) Uani 1 d . . .
C16 C -0.0271(3) 0.6503(2) 0.4511(3) 0.0269(9) Uani 1 d . . .
H16 H -0.0755 0.6654 0.3983 0.032 Uiso 1 calc . . R
C29 C 0.1399(3) 0.4973(2) 1.0582(2) 0.0234(8) Uani 1 d . . .
H29 H 0.1050 0.5105 1.1104 0.028 Uiso 1 calc . . R
C3 C 0.4727(3) 0.7272(2) 0.4620(3) 0.0274(9) Uani 1 d . . .
H3 H 0.5074 0.7541 0.4169 0.033 Uiso 1 calc . . R
C20 C 0.1931(3) 0.4686(2) 0.4373(2) 0.0208(8) Uani 1 d . . .
C30 C 0.1521(3) 0.5555(2) 0.9896(2) 0.0217(8) Uani 1 d . . .
C25 C 0.3119(3) 0.3089(2) 0.8778(3) 0.0256(8) Uani 1 d . . .
H25 H 0.3369 0.2567 0.8669 0.031 Uiso 1 calc . . R
C26 C 0.2689(3) 0.3237(2) 0.9574(3) 0.0238(8) Uani 1 d . . .
H26 H 0.2656 0.2823 1.0027 0.029 Uiso 1 calc . . R
C9 C 0.2583(3) 0.8488(2) 0.8122(3) 0.0249(8) Uani 1 d . . .
H9 H 0.2316 0.8740 0.8635 0.030 Uiso 1 calc . . R
C21 C 0.1928(3) 0.5090(2) 0.5222(2) 0.0179(7) Uani 1 d . . .
C10 C 0.2561(3) 0.7649(2) 0.8034(3) 0.0228(8) Uani 1 d . . .
H10 H 0.2290 0.7345 0.8507 0.027 Uiso 1 calc . . R
C31 C 0.2012(3) 0.5396(2) 0.9118(2) 0.0174(7) Uani 1 d . . .
C15 C -0.0270(3) 0.6873(2) 0.5358(3) 0.0262(8) Uani 1 d . . .
H15 H -0.0759 0.7285 0.5419 0.031 Uiso 1 calc . . R
C27 C 0.2295(3) 0.4001(2) 0.9727(2) 0.0204(8) Uani 1 d . . .
C24 C 0.3200(3) 0.3704(2) 0.8107(2) 0.0214(8) Uani 1 d . . .
C6 C 0.3851(3) 0.8969(2) 0.5999(3) 0.0257(8) Uani 1 d . . .
H6 H 0.3860 0.9539 0.6001 0.031 Uiso 1 calc . . R
C28 C 0.1779(3) 0.4221(2) 1.0501(2) 0.0226(8) Uani 1 d . . .
C19 C 0.1222(3) 0.4843(2) 0.3568(2) 0.0249(8) Uani 1 d . . .
H19 H 0.1243 0.4542 0.3006 0.030 Uiso 1 calc . . R
C5 C 0.4273(3) 0.8573(2) 0.5330(3) 0.0279(9) Uani 1 d . . .
H5 H 0.4589 0.8868 0.4877 0.033 Uiso 1 calc . . R
C18 C 0.0502(3) 0.5431(2) 0.3596(3) 0.0237(8) Uani 1 d . . .
C23 C 0.3676(3) 0.3502(2) 0.7241(3) 0.0266(9) Uani 1 d . . .
H23A H 0.3360 0.3832 0.6712 0.040 Uiso 1 calc . . GR
H23B H 0.3558 0.2933 0.7087 0.040 Uiso 1 calc . . GR
H23C H 0.4420 0.3608 0.7356 0.040 Uiso 1 calc . . GR


_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 O1 2.201(2) . ?
Dy1 O2 2.202(2) . ?
Dy1 O4 2.508(3) . ?
Dy1 N1 2.530(3) . ?
Dy1 N3 2.640(3) . ?
Dy1 N4 2.619(3) . ?
Dy1 O3 2.426(3) . ?
Dy1 N2 2.533(3) . ?
Dy1 N5 2.894(3) . ?
Cl4 C30 1.739(4) . ?
Cl2 C20 1.734(4) . ?
Cl3 C28 1.748(4) . ?
Cl1 C18 1.738(4) . ?
O1 C21 1.310(4) . ?
O2 C31 1.317(4) . ?
O4 N5 1.268(4) . ?
N1 C12 1.358(4) . ?
N1 C1 1.340(4) . ?
N3 C14 1.331(4) . ?
N3 C22 1.384(4) . ?
O5 N5 1.219(4) . ?
N4 C32 1.377(4) . ?
N4 C24 1.336(4) . ?
O3 N5 1.280(4) . ?
N2 C11 1.360(4) . ?
N2 C10 1.331(4) . ?
C11 C12 1.439(5) . ?
C11 C7 1.417(5) . ?
C12 C4 1.414(5) . ?
C14 C13 1.505(5) . ?
C14 C15 1.413(5) . ?
C7 C8 1.404(5) . ?
C7 C6 1.446(5) . ?
C22 C17 1.418(5) . ?
C22 C21 1.437(5) . ?
C1 C2 1.400(5) . ?
C17 C16 1.405(5) . ?
C17 C18 1.422(5) . ?
C2 C3 1.359(5) . ?
C8 C9 1.363(5) . ?
C4 C3 1.407(5) . ?
C4 C5 1.421(5) . ?
C32 C31 1.436(5) . ?
C32 C27 1.425(5) . ?
C16 C15 1.358(5) . ?
C29 C30 1.403(5) . ?
C29 C28 1.358(5) . ?
C20 C21 1.387(5) . ?
C20 C19 1.401(5) . ?
C30 C31 1.381(5) . ?
C25 C26 1.356(5) . ?
C25 C24 1.416(5) . ?
C26 C27 1.403(5) . ?
C9 C10 1.403(5) . ?
C27 C28 1.417(5) . ?
C24 C23 1.495(5) . ?
C6 C5 1.340(5) . ?
C19 C18 1.363(5) . ?

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 Dy1 O2 132.45(9) . . ?
O1 Dy1 O4 81.06(8) . . ?
O1 Dy1 N1 78.25(9) . . ?
O1 Dy1 N3 67.12(9) . . ?
O1 Dy1 N4 85.33(9) . . ?
O1 Dy1 O3 131.74(9) . . ?
O1 Dy1 N2 132.28(9) . . ?
O1 Dy1 N5 106.03(9) . . ?
O2 Dy1 O4 125.42(8) . . ?
O2 Dy1 N1 142.75(9) . . ?
O2 Dy1 N3 91.20(9) . . ?
O2 Dy1 N4 67.20(9) . . ?
O2 Dy1 O3 89.12(9) . . ?
O2 Dy1 N2 78.01(9) . . ?
O2 Dy1 N5 109.73(9) . . ?
O4 Dy1 N1 72.29(9) . . ?
O4 Dy1 N3 142.73(8) . . ?
O4 Dy1 N4 77.06(8) . . ?
O4 Dy1 N2 112.63(9) . . ?
O4 Dy1 N5 25.91(8) . . ?
N1 Dy1 N3 82.33(9) . . ?
N1 Dy1 N4 147.02(9) . . ?
N1 Dy1 N2 64.74(9) . . ?
N1 Dy1 N5 71.51(9) . . ?
N3 Dy1 N5 153.85(8) . . ?
N4 Dy1 N3 117.24(9) . . ?
N4 Dy1 N5 86.14(8) . . ?
O3 Dy1 O4 51.75(8) . . ?
O3 Dy1 N1 78.18(9) . . ?
O3 Dy1 N3 147.86(9) . . ?
O3 Dy1 N4 92.38(9) . . ?
O3 Dy1 N2 70.04(9) . . ?
O3 Dy1 N5 25.99(8) . . ?
N2 Dy1 N3 78.61(9) . . ?
N2 Dy1 N4 141.31(8) . . ?
N2 Dy1 N5 90.27(9) . . ?
C21 O1 Dy1 123.9(2) . . ?
C31 O2 Dy1 126.2(2) . . ?
N5 O4 Dy1 94.30(19) . . ?
C12 N1 Dy1 120.0(2) . . ?
C1 N1 Dy1 121.3(2) . . ?
C1 N1 C12 118.5(3) . . ?
C14 N3 Dy1 132.9(2) . . ?
C14 N3 C22 117.7(3) . . ?
C22 N3 Dy1 108.7(2) . . ?
C32 N4 Dy1 111.0(2) . . ?
C24 N4 Dy1 130.8(2) . . ?
C24 N4 C32 118.2(3) . . ?
N5 O3 Dy1 97.87(19) . . ?
C11 N2 Dy1 119.4(2) . . ?
C10 N2 Dy1 123.1(2) . . ?
C10 N2 C11 117.3(3) . . ?
N2 C11 C12 118.3(3) . . ?
N2 C11 C7 122.5(3) . . ?
C7 C11 C12 119.2(3) . . ?
O4 N5 Dy1 59.79(16) . . ?
O4 N5 O3 115.4(3) . . ?
O5 N5 Dy1 172.5(2) . . ?
O5 N5 O4 122.7(3) . . ?
O5 N5 O3 121.9(3) . . ?
O3 N5 Dy1 56.14(16) . . ?
N1 C12 C11 117.5(3) . . ?
N1 C12 C4 122.4(3) . . ?
C4 C12 C11 120.0(3) . . ?
N3 C14 C13 119.7(3) . . ?
N3 C14 C15 121.7(3) . . ?
C15 C14 C13 118.6(3) . . ?
C11 C7 C6 118.5(3) . . ?
C8 C7 C11 118.2(3) . . ?
C8 C7 C6 123.3(3) . . ?
N3 C22 C17 122.8(3) . . ?
N3 C22 C21 115.7(3) . . ?
C17 C22 C21 121.4(3) . . ?
N1 C1 C2 122.4(4) . . ?
C22 C17 C18 117.9(3) . . ?
C16 C17 C22 117.4(3) . . ?
C16 C17 C18 124.7(3) . . ?
C3 C2 C1 119.2(4) . . ?
C9 C8 C7 118.9(3) . . ?
C12 C4 C5 119.1(3) . . ?
C3 C4 C12 116.9(3) . . ?
C3 C4 C5 124.0(3) . . ?
N4 C32 C31 116.0(3) . . ?
N4 C32 C27 122.8(3) . . ?
C27 C32 C31 121.2(3) . . ?
C15 C16 C17 119.1(3) . . ?
C28 C29 C30 120.0(3) . . ?
C2 C3 C4 120.6(3) . . ?
C21 C20 Cl2 117.9(3) . . ?
C21 C20 C19 123.2(3) . . ?
C19 C20 Cl2 118.9(3) . . ?
C29 C30 Cl4 119.1(3) . . ?
C31 C30 Cl4 118.3(3) . . ?
C31 C30 C29 122.6(3) . . ?
C26 C25 C24 120.9(3) . . ?
C25 C26 C27 119.8(3) . . ?
C8 C9 C10 119.5(3) . . ?
O1 C21 C22 120.3(3) . . ?
O1 C21 C20 123.2(3) . . ?
C20 C21 C22 116.5(3) . . ?
N2 C10 C9 123.6(3) . . ?
O2 C31 C32 119.5(3) . . ?
O2 C31 C30 123.5(3) . . ?
C30 C31 C32 117.0(3) . . ?
C16 C15 C14 121.2(4) . . ?
C26 C27 C32 116.9(3) . . ?
C26 C27 C28 125.4(3) . . ?
C28 C27 C32 117.7(3) . . ?
N4 C24 C25 121.3(3) . . ?
N4 C24 C23 120.4(3) . . ?
C25 C24 C23 118.3(3) . . ?
C5 C6 C7 121.5(4) . . ?
C29 C28 Cl3 119.6(3) . . ?
C29 C28 C27 121.5(3) . . ?
C27 C28 Cl3 118.9(3) . . ?
C18 C19 C20 119.5(3) . . ?
C6 C5 C4 121.5(4) . . ?
C17 C18 Cl1 119.6(3) . . ?
C19 C18 Cl1 119.0(3) . . ?
C19 C18 C17 121.5(3) . . ?

_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_aaaa_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1856177'

_audit_update_record             
;
2018-07-15 deposited with the CCDC.
2018-10-17 downloaded from the CCDC.
;
_audit_creation_date             2018-06-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H20 Br4 Dy N5 O5'
_chemical_formula_sum            'C32 H20 Br4 Dy N5 O5'
_chemical_formula_weight         1036.67
_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'
Br Br -0.2901 2.4595 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   13.583(3)
_cell_length_b                   16.809(4)
_cell_length_c                   14.442(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.666(4)
_cell_angle_gamma                90.00
_cell_volume                     3267.7(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7504
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.71
_cell_measurement_theta_min      2.28
_exptl_absorpt_coefficient_mu    7.227
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.107
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           ?
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39265
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.51
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_reflns_number_gt                4986
_reflns_number_total             6658
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0303
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0394P)²+0.0317P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0767
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C1(H1), C19(H19), C10(H10), C26(H26), C16(H16), C8(H8), C2(H2),
 C29(H29), C15(H15), C6(H6), C3(H3), C5(H5), C9(H9)
2.b Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C23(H23a,H23b,H23c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Dy1 Dy 0.708885(16) 0.577449(12) 0.282148(13) 0.03303(7) Uani 1 d . . .
Br4 Br 0.89279(4) 0.65809(3) -0.00032(4) 0.05782(15) Uani 1 d . . .
Br3 Br 0.82772(5) 0.34504(3) -0.13681(4) 0.06262(17) Uani 1 d . . .
Br2 Br 0.70381(5) 0.39603(3) 0.56969(4) 0.06532(17) Uani 1 d . . .
Br1 Br 1.03739(5) 0.56170(4) 0.74398(4) 0.07175(19) Uani 1 d . . .
O1 O 0.7413(2) 0.49642(17) 0.40203(19) 0.0382(7) Uani 1 d . . .
O2 O 0.7814(2) 0.59443(17) 0.1555(2) 0.0425(8) Uani 1 d . . .
O4 O 0.5370(2) 0.5227(2) 0.2821(2) 0.0498(8) Uani 1 d . . .
N3 N 0.8783(3) 0.6100(2) 0.3891(2) 0.0341(8) Uani 1 d . . .
N4 N 0.7094(3) 0.4481(2) 0.1806(2) 0.0342(8) Uani 1 d . . .
N2 N 0.7089(3) 0.7285(2) 0.2696(2) 0.0358(8) Uani 1 d . . .
N1 N 0.6300(3) 0.6498(2) 0.4079(2) 0.0382(9) Uani 1 d . . .
N5 N 0.4961(3) 0.5744(2) 0.2267(3) 0.0486(10) Uani 1 d . . .
O3 O 0.5551(3) 0.6217(2) 0.1921(2) 0.0624(10) Uani 1 d . . .
C14 C 0.9516(3) 0.6610(3) 0.3806(3) 0.0397(11) Uani 1 d . . .
C27 C 0.7650(3) 0.4025(3) 0.0342(3) 0.0400(11) Uani 1 d . . .
O5 O 0.4071(3) 0.5792(2) 0.2057(4) 0.0898(14) Uani 1 d . . .
C12 C 0.6241(3) 0.7305(3) 0.4060(3) 0.0365(10) Uani 1 d . . .
C30 C 0.8406(3) 0.5548(3) 0.0148(3) 0.0390(11) Uani 1 d . . .
C28 C 0.8134(4) 0.4232(3) -0.0438(3) 0.0454(11) Uani 1 d . . .
C21 C 0.8043(3) 0.5113(2) 0.4762(3) 0.0328(9) Uani 1 d . . .
C32 C 0.7548(3) 0.4623(3) 0.1011(3) 0.0322(9) Uani 1 d . . .
C11 C 0.6666(3) 0.7727(3) 0.3328(3) 0.0361(10) Uani 1 d . . .
C31 C 0.7923(3) 0.5411(3) 0.0921(3) 0.0346(10) Uani 1 d . . .
C7 C 0.6596(4) 0.8558(3) 0.3281(3) 0.0430(11) Uani 1 d . . .
C25 C 0.6844(4) 0.3140(3) 0.1296(3) 0.0492(12) Uani 1 d . . .
H25 H 0.6600 0.2638 0.1411 0.059 Uiso 1 calc . . R
C1 C 0.5874(4) 0.6110(3) 0.4722(3) 0.0434(11) Uani 1 d . . .
H1 H 0.5914 0.5558 0.4737 0.052 Uiso 1 calc . . R
C19 C 0.8736(4) 0.4874(3) 0.6396(3) 0.0451(12) Uani 1 d . . .
H19 H 0.8706 0.4595 0.6947 0.054 Uiso 1 calc . . R
C20 C 0.8041(4) 0.4722(2) 0.5615(3) 0.0416(11) Uani 1 d . . .
C24 C 0.6773(3) 0.3750(3) 0.1940(3) 0.0394(11) Uani 1 d . . .
C10 C 0.7422(3) 0.7673(3) 0.2005(3) 0.0421(11) Uani 1 d . . .
H10 H 0.7691 0.7379 0.1554 0.051 Uiso 1 calc . . R
C22 C 0.8800(3) 0.5709(2) 0.4737(3) 0.0340(10) Uani 1 d . . .
C26 C 0.7261(4) 0.3265(3) 0.0506(3) 0.0514(13) Uani 1 d . . .
H26 H 0.7292 0.2856 0.0078 0.062 Uiso 1 calc . . R
C16 C 1.0234(4) 0.6443(3) 0.5409(4) 0.0529(13) Uani 1 d . . .
H16 H 1.0710 0.6577 0.5908 0.063 Uiso 1 calc . . R
C17 C 0.9512(3) 0.5873(3) 0.5523(3) 0.0386(10) Uani 1 d . . .
C8 C 0.6994(4) 0.8940(3) 0.2552(4) 0.0525(13) Uani 1 d . . .
H8 H 0.6985 0.9492 0.2507 0.063 Uiso 1 calc . . R
C2 C 0.5370(4) 0.6493(3) 0.5375(3) 0.0514(13) Uani 1 d . . .
H2 H 0.5075 0.6198 0.5809 0.062 Uiso 1 calc . . R
C29 C 0.8523(3) 0.4970(3) -0.0523(3) 0.0461(12) Uani 1 d . . .
H29 H 0.8864 0.5089 -0.1023 0.055 Uiso 1 calc . . R
C15 C 1.0238(3) 0.6799(3) 0.4571(4) 0.0486(12) Uani 1 d . . .
H15 H 1.0725 0.7174 0.4496 0.058 Uiso 1 calc . . R
C4 C 0.5759(4) 0.7735(3) 0.4705(3) 0.0453(12) Uani 1 d . . .
C18 C 0.9448(4) 0.5422(3) 0.6353(3) 0.0437(12) Uani 1 d . . .
C6 C 0.6125(4) 0.8978(3) 0.3977(4) 0.0535(13) Uani 1 d . . .
H6 H 0.6098 0.9531 0.3961 0.064 Uiso 1 calc . . R
C13 C 0.9594(4) 0.6986(3) 0.2877(4) 0.0559(13) Uani 1 d . . .
H13A H 0.9211 0.6683 0.2392 0.084 Uiso 1 calc . . GR
H13B H 1.0277 0.6995 0.2772 0.084 Uiso 1 calc . . GR
H13C H 0.9344 0.7520 0.2872 0.084 Uiso 1 calc . . GR
C23 C 0.6315(4) 0.3569(3) 0.2810(3) 0.0501(13) Uani 1 d . . .
H23A H 0.6606 0.3905 0.3309 0.075 Uiso 1 calc . . GR
H23B H 0.6434 0.3022 0.2980 0.075 Uiso 1 calc . . GR
H23C H 0.5612 0.3664 0.2694 0.075 Uiso 1 calc . . GR
C3 C 0.5313(4) 0.7296(3) 0.5373(3) 0.0536(13) Uani 1 d . . .
H3 H 0.4982 0.7558 0.5807 0.064 Uiso 1 calc . . R
C5 C 0.5727(4) 0.8588(3) 0.4643(4) 0.0585(14) Uani 1 d . . .
H5 H 0.5422 0.8875 0.5076 0.070 Uiso 1 calc . . R
C9 C 0.7391(4) 0.8497(3) 0.1917(4) 0.0511(13) Uani 1 d . . .
H9 H 0.7644 0.8742 0.1421 0.061 Uiso 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
Dy1 O1 2.201(3) . ?
Dy1 O2 2.208(3) . ?
Dy1 O4 2.509(3) . ?
Dy1 N3 2.652(4) . ?
Dy1 N4 2.624(3) . ?
Dy1 N2 2.546(3) . ?
Dy1 N1 2.538(4) . ?
Dy1 N5 2.894(4) . ?
Dy1 O3 2.426(4) . ?
Br4 C30 1.898(4) . ?
Br3 C28 1.907(5) . ?
Br2 C20 1.885(5) . ?
Br1 C18 1.905(4) . ?
O1 C21 1.304(5) . ?
O2 C31 1.304(5) . ?
O4 N5 1.259(5) . ?
N3 C14 1.332(5) . ?
N3 C22 1.385(5) . ?
N4 C32 1.395(5) . ?
N4 C24 1.327(5) . ?
N2 C11 1.361(5) . ?
N2 C10 1.321(5) . ?
N1 C12 1.359(5) . ?
N1 C1 1.328(5) . ?
N5 O3 1.277(5) . ?
N5 O5 1.210(5) . ?
C14 C15 1.411(7) . ?
C14 C13 1.500(6) . ?
C27 C28 1.422(6) . ?
C27 C32 1.414(6) . ?
C27 C26 1.413(6) . ?
C12 C11 1.455(6) . ?
C12 C4 1.408(6) . ?
C30 C31 1.388(6) . ?
C30 C29 1.397(6) . ?
C28 C29 1.362(7) . ?
C21 C20 1.395(6) . ?
C21 C22 1.439(6) . ?
C32 C31 1.431(6) . ?
C11 C7 1.401(6) . ?
C7 C8 1.403(7) . ?
C7 C6 1.445(7) . ?
C25 H25 0.9300 . ?
C25 C24 1.395(6) . ?
C25 C26 1.357(6) . ?
C1 H1 0.9300 . ?
C1 C2 1.395(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.394(6) . ?
C19 C18 1.343(7) . ?
C24 C23 1.506(6) . ?
C10 H10 0.9300 . ?
C10 C9 1.392(6) . ?
C22 C17 1.416(6) . ?
C26 H26 0.9300 . ?
C16 H16 0.9300 . ?
C16 C17 1.396(7) . ?
C16 C15 1.350(7) . ?
C17 C18 1.431(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.348(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.353(7) . ?
C29 H29 0.9300 . ?
C15 H15 0.9300 . ?
C4 C3 1.413(7) . ?
C4 C5 1.436(7) . ?
C6 H6 0.9300 . ?
C6 C5 1.337(7) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C3 H3 0.9300 . ?
C5 H5 0.9300 . ?
C9 H9 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
O1 Dy1 O2 131.85(12) . . ?
O1 Dy1 O4 82.04(11) . . ?
O1 Dy1 N3 66.57(10) . . ?
O1 Dy1 N4 84.93(11) . . ?
O1 Dy1 N2 132.17(11) . . ?
O1 Dy1 N1 78.04(11) . . ?
O1 Dy1 N5 107.09(12) . . ?
O1 Dy1 O3 132.76(12) . . ?
O2 Dy1 O4 124.40(11) . . ?
O2 Dy1 N3 90.44(11) . . ?
O2 Dy1 N4 67.01(10) . . ?
O2 Dy1 N2 78.93(11) . . ?
O2 Dy1 N1 143.90(11) . . ?
O2 Dy1 N5 108.21(12) . . ?
O2 Dy1 O3 87.92(12) . . ?
O4 Dy1 N3 144.16(11) . . ?
O4 Dy1 N4 76.60(11) . . ?
O4 Dy1 N2 111.98(11) . . ?
O4 Dy1 N1 72.18(11) . . ?
O4 Dy1 N5 25.69(10) . . ?
N3 Dy1 N5 157.15(11) . . ?
N4 Dy1 N3 115.44(11) . . ?
N4 Dy1 N5 84.72(11) . . ?
N2 Dy1 N3 80.07(11) . . ?
N2 Dy1 N4 141.92(10) . . ?
N2 Dy1 N5 90.42(12) . . ?
N1 Dy1 N3 84.31(11) . . ?
N1 Dy1 N4 146.09(11) . . ?
N1 Dy1 N2 64.98(11) . . ?
N1 Dy1 N5 72.84(12) . . ?
O3 Dy1 O4 51.50(12) . . ?
O3 Dy1 N3 150.17(12) . . ?
O3 Dy1 N4 91.20(12) . . ?
O3 Dy1 N2 70.38(12) . . ?
O3 Dy1 N1 79.69(12) . . ?
O3 Dy1 N5 25.90(11) . . ?
C21 O1 Dy1 124.6(2) . . ?
C31 O2 Dy1 126.7(3) . . ?
N5 O4 Dy1 94.5(3) . . ?
C14 N3 Dy1 132.9(3) . . ?
C14 N3 C22 117.5(4) . . ?
C22 N3 Dy1 109.1(3) . . ?
C32 N4 Dy1 110.6(2) . . ?
C24 N4 Dy1 131.4(3) . . ?
C24 N4 C32 118.0(4) . . ?
C11 N2 Dy1 119.5(3) . . ?
C10 N2 Dy1 123.3(3) . . ?
C10 N2 C11 117.1(4) . . ?
C12 N1 Dy1 119.6(3) . . ?
C1 N1 Dy1 122.0(3) . . ?
C1 N1 C12 118.2(4) . . ?
O4 N5 Dy1 59.8(2) . . ?
O4 N5 O3 115.6(4) . . ?
O3 N5 Dy1 56.1(2) . . ?
O5 N5 Dy1 175.0(4) . . ?
O5 N5 O4 123.1(4) . . ?
O5 N5 O3 121.3(5) . . ?
N5 O3 Dy1 98.0(3) . . ?
N3 C14 C15 121.5(4) . . ?
N3 C14 C13 119.8(4) . . ?
C15 C14 C13 118.7(4) . . ?
C32 C27 C28 117.7(4) . . ?
C26 C27 C28 125.2(4) . . ?
C26 C27 C32 117.1(4) . . ?
N1 C12 C11 118.2(4) . . ?
N1 C12 C4 122.1(4) . . ?
C4 C12 C11 119.7(4) . . ?
C31 C30 Br4 118.0(3) . . ?
C31 C30 C29 123.5(4) . . ?
C29 C30 Br4 118.5(3) . . ?
C27 C28 Br3 119.4(4) . . ?
C29 C28 Br3 119.1(3) . . ?
C29 C28 C27 121.4(4) . . ?
O1 C21 C20 123.8(4) . . ?
O1 C21 C22 120.4(4) . . ?
C20 C21 C22 115.8(4) . . ?
N4 C32 C27 122.3(4) . . ?
N4 C32 C31 115.8(4) . . ?
C27 C32 C31 121.9(4) . . ?
N2 C11 C12 117.7(4) . . ?
N2 C11 C7 122.9(4) . . ?
C7 C11 C12 119.3(4) . . ?
O2 C31 C30 124.1(4) . . ?
O2 C31 C32 119.9(4) . . ?
C30 C31 C32 116.0(4) . . ?
C11 C7 C8 117.5(4) . . ?
C11 C7 C6 119.2(5) . . ?
C8 C7 C6 123.3(4) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C26 C25 C24 121.3(4) . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 123.1(5) . . ?
C2 C1 H1 118.5 . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.1(4) . . ?
C21 C20 Br2 117.5(3) . . ?
C19 C20 Br2 119.3(3) . . ?
C19 C20 C21 123.2(4) . . ?
N4 C24 C25 122.0(4) . . ?
N4 C24 C23 119.3(4) . . ?
C25 C24 C23 118.7(4) . . ?
N2 C10 H10 118.3 . . ?
N2 C10 C9 123.4(4) . . ?
C9 C10 H10 118.3 . . ?
N3 C22 C21 115.1(4) . . ?
N3 C22 C17 122.9(4) . . ?
C17 C22 C21 122.0(4) . . ?
C27 C26 H26 120.4 . . ?
C25 C26 C27 119.2(4) . . ?
C25 C26 H26 120.4 . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C15 C16 C17 119.8(5) . . ?
C22 C17 C18 117.2(4) . . ?
C16 C17 C22 117.0(4) . . ?
C16 C17 C18 125.8(4) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.2(4) . . ?
C9 C8 H8 120.4 . . ?
C1 C2 H2 120.3 . . ?
C3 C2 C1 119.4(5) . . ?
C3 C2 H2 120.3 . . ?
C30 C29 H29 120.3 . . ?
C28 C29 C30 119.3(4) . . ?
C28 C29 H29 120.3 . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.0(5) . . ?
C16 C15 H15 119.5 . . ?
C12 C4 C3 117.6(4) . . ?
C12 C4 C5 119.0(5) . . ?
C3 C4 C5 123.4(5) . . ?
C19 C18 Br1 118.7(4) . . ?
C19 C18 C17 121.8(4) . . ?
C17 C18 Br1 119.5(4) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 C7 121.3(5) . . ?
C5 C6 H6 119.4 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C2 C3 C4 119.5(5) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.5(5) . . ?
C6 C5 H5 119.3 . . ?
C10 C9 H9 120.1 . . ?
C8 C9 C10 119.8(5) . . ?
C8 C9 H9 120.1 . . ?

_olex2_submission_special_instructions 'No special instructions were received'

