# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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 
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data_H2L3_CCDC_1406218
_database_code_depnum_ccdc_archive 'CCDC 1406218'
_audit_update_record             
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_audit_creation_date             2015-02-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C14 H11 Cl N2 O5'
_chemical_formula_sum            'C14 H11 Cl N2 O5'
_chemical_formula_weight         322.70
_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'
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.9697(4)
_cell_length_b                   12.6645(7)
_cell_length_c                   15.0866(8)
_cell_angle_alpha                76.153(5)
_cell_angle_beta                 89.966(5)
_cell_angle_gamma                88.423(5)
_cell_volume                     1292.45(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    173
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.900
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7064
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         71.340
_diffrn_reflns_theta_min         5.222
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3925
_reflns_number_total             4806
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         4806
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0493
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0861P)²+0.1097P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1451
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-H2 = O7-H7
 0.88 with sigma of 0.02
3. Others
 Fixed Sof: H1(0.75) H3B(0.75) H7(0.25) H2(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C8(H8), C10(H10), C13(H13), C17(H17), C18(H18),
 C19(H19), C22(H22), C24(H24), C27(H27)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.38159(9) 0.98265(4) 0.11863(3) 0.03147(17) Uani 1 1 d . . . . .
O1 O 0.4315(3) 0.58558(14) 0.78792(11) 0.0318(4) Uani 1 1 d . . . . .
O2 O 0.4317(3) 0.61811(13) 0.60646(10) 0.0306(4) Uani 1 1 d D . . . .
O3 O 0.3834(3) 0.56291(13) 0.39069(11) 0.0299(4) Uani 1 1 d . . . . .
O4 O 0.3247(4) 0.67767(18) 0.05043(14) 0.0632(7) Uani 1 1 d . . . . .
O5 O 0.4814(4) 0.82334(18) 0.01736(13) 0.0546(6) Uani 1 1 d . . . . .
N1 N 0.3844(3) 0.74587(16) 0.44605(13) 0.0249(4) Uani 1 1 d . . . . .
N2 N 0.3976(3) 0.75398(16) 0.07132(13) 0.0301(4) Uani 1 1 d . . . . .
C1 C 0.4137(4) 0.5694(2) 0.88513(16) 0.0355(5) Uani 1 1 d . . . . .
H1A H 0.2936 0.6040 0.8991 0.053 Uiso 1 1 calc GR . . . .
H1B H 0.5224 0.6020 0.9089 0.053 Uiso 1 1 calc GR . . . .
H1C H 0.4130 0.4913 0.9137 0.053 Uiso 1 1 calc GR . . . .
C2 C 0.4127(3) 0.69069(18) 0.73787(15) 0.0253(4) Uani 1 1 d . . . . .
C3 C 0.3948(3) 0.7810(2) 0.77337(15) 0.0280(5) Uani 1 1 d . . . . .
H3A H 0.3997 0.7726 0.8376 0.034 Uiso 1 1 calc R . . . .
C4 C 0.3691(3) 0.88698(19) 0.71485(17) 0.0300(5) Uani 1 1 d . . . . .
H4 H 0.3564 0.9483 0.7406 0.036 Uiso 1 1 calc R . . . .
C5 C 0.3625(3) 0.90130(18) 0.62305(16) 0.0277(5) Uani 1 1 d . . . . .
H5 H 0.3439 0.9723 0.5849 0.033 Uiso 1 1 calc R . . . .
C6 C 0.3838(3) 0.80936(18) 0.58336(15) 0.0239(4) Uani 1 1 d . . . . .
C7 C 0.4113(3) 0.70128(18) 0.64053(14) 0.0238(4) Uani 1 1 d . . . . .
C8 C 0.3711(3) 0.82603(18) 0.48825(15) 0.0250(4) Uani 1 1 d . . . . .
H8 H 0.3521 0.8983 0.4525 0.030 Uiso 1 1 calc R . . . .
C9 C 0.3802(3) 0.75455(18) 0.35154(14) 0.0236(4) Uani 1 1 d . . . . .
C10 C 0.3781(3) 0.85376(18) 0.28701(15) 0.0247(4) Uani 1 1 d . . . . .
H10 H 0.3725 0.9198 0.3064 0.030 Uiso 1 1 calc R . . . .
C11 C 0.3841(3) 0.85647(18) 0.19474(14) 0.0242(4) Uani 1 1 d . . . . .
C12 C 0.3886(3) 0.75839(19) 0.16773(15) 0.0259(5) Uani 1 1 d . . . . .
C13 C 0.3864(3) 0.65864(18) 0.23177(15) 0.0257(5) Uani 1 1 d . . . . .
H13 H 0.3866 0.5928 0.2121 0.031 Uiso 1 1 calc R . . . .
C14 C 0.3840(3) 0.65586(18) 0.32406(15) 0.0244(4) Uani 1 1 d . . . . .
Cl2 Cl 0.08909(9) 0.47987(4) 0.11973(4) 0.03266(17) Uani 1 1 d . . . . .
O6 O 0.0876(3) 0.09006(14) 0.78897(10) 0.0316(4) Uani 1 1 d . . . . .
O7 O 0.0738(3) 0.11929(13) 0.60769(11) 0.0300(4) Uani 1 1 d D . . . .
O8 O 0.1029(3) 0.05999(13) 0.39096(11) 0.0294(4) Uani 1 1 d . . . . .
O9 O -0.0078(5) 0.1817(2) 0.05284(16) 0.0732(9) Uani 1 1 d . . . . .
O10 O 0.1729(4) 0.31940(19) 0.01571(13) 0.0545(6) Uani 1 1 d . . . . .
N3 N 0.1108(3) 0.24345(16) 0.44617(13) 0.0252(4) Uani 1 1 d . . . . .
N4 N 0.0862(3) 0.25272(17) 0.07184(14) 0.0349(5) Uani 1 1 d . . . . .
C15 C 0.1073(4) 0.0759(2) 0.88632(16) 0.0383(6) Uani 1 1 d . . . . .
H15A H 0.2279 0.1071 0.8998 0.057 Uiso 1 1 calc GR . . . .
H15B H 0.1082 -0.0019 0.9162 0.057 Uiso 1 1 calc GR . . . .
H15C H -0.0007 0.1128 0.9091 0.057 Uiso 1 1 calc GR . . . .
C16 C 0.1028(3) 0.19397(19) 0.73771(15) 0.0249(4) Uani 1 1 d . . . . .
C17 C 0.1242(3) 0.2848(2) 0.77149(16) 0.0286(5) Uani 1 1 d . . . . .
H17 H 0.1234 0.2777 0.8356 0.034 Uiso 1 1 calc R . . . .
C18 C 0.1475(3) 0.38933(19) 0.71176(17) 0.0291(5) Uani 1 1 d . . . . .
H18 H 0.1620 0.4510 0.7365 0.035 Uiso 1 1 calc R . . . .
C19 C 0.1490(3) 0.40161(18) 0.62034(16) 0.0275(5) Uani 1 1 d . . . . .
H19 H 0.1676 0.4714 0.5812 0.033 Uiso 1 1 calc R . . . .
C20 C 0.1226(3) 0.30929(18) 0.58233(15) 0.0244(4) Uani 1 1 d . . . . .
C21 C 0.0976(3) 0.20231(18) 0.64069(15) 0.0235(4) Uani 1 1 d . . . . .
C22 C 0.1287(3) 0.32394(17) 0.48740(15) 0.0244(4) Uani 1 1 d . . . . .
H22 H 0.1467 0.3952 0.4508 0.029 Uiso 1 1 calc R . . . .
C23 C 0.1085(3) 0.25107(18) 0.35212(14) 0.0235(4) Uani 1 1 d . . . . .
C24 C 0.1089(3) 0.35046(18) 0.28746(15) 0.0249(4) Uani 1 1 d . . . . .
H24 H 0.1143 0.4163 0.3069 0.030 Uiso 1 1 calc R . . . .
C25 C 0.1013(3) 0.35363(18) 0.19505(15) 0.0248(4) Uani 1 1 d . . . . .
C26 C 0.0942(3) 0.25556(19) 0.16849(15) 0.0267(5) Uani 1 1 d . . . . .
C27 C 0.0908(3) 0.15587(19) 0.23191(16) 0.0275(5) Uani 1 1 d . . . . .
H27 H 0.0826 0.0903 0.2122 0.033 Uiso 1 1 calc R . . . .
C28 C 0.0997(3) 0.15311(18) 0.32428(15) 0.0246(4) Uani 1 1 d . . . . .
H1 H 0.400(5) 0.686(3) 0.482(3) 0.029 Uiso 0.75 1 d R . P . .
H3B H 0.096(5) 0.182(3) 0.484(3) 0.029 Uiso 0.75 1 d R . P . .
H8A H 0.044(4) 0.011(2) 0.376(2) 0.029 Uiso 1 1 d R . . . .
H3 H 0.439(4) 0.511(3) 0.378(2) 0.029 Uiso 1 1 d R . . . .
H7 H -0.039(8) 0.127(9) 0.582(7) 0.029 Uiso 0.25 1 d DR . P . .
H2 H 0.307(4) 0.618(9) 0.600(8) 0.029 Uiso 0.25 1 d DR . 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
Cl1 C11 1.730(2) . ?
O1 C1 1.437(3) . ?
O1 C2 1.367(3) . ?
O2 C7 1.282(3) . ?
O2 H2 0.88(2) . ?
O3 C14 1.353(3) . ?
O3 H3 0.81(3) . ?
O4 N2 1.210(3) . ?
O5 N2 1.209(3) . ?
N1 C8 1.322(3) . ?
N1 C9 1.404(3) . ?
N1 H1 0.82(4) . ?
N2 C12 1.470(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.377(3) . ?
C2 C7 1.442(3) . ?
C3 H3A 0.9500 . ?
C3 C4 1.426(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.354(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.435(3) . ?
C6 C7 1.440(3) . ?
C6 C8 1.402(3) . ?
C7 H2 1.54(10) . ?
C8 H8 0.9500 . ?
C9 C10 1.393(3) . ?
C9 C14 1.407(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.385(3) . ?
C11 C12 1.396(3) . ?
C12 C13 1.395(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.385(3) . ?
Cl2 C25 1.726(2) . ?
O6 C15 1.442(3) . ?
O6 C16 1.364(3) . ?
O7 C21 1.281(3) . ?
O7 H7 0.87(2) . ?
O8 C28 1.354(3) . ?
O8 H8A 0.82(3) . ?
O9 N4 1.215(3) . ?
O10 N4 1.217(3) . ?
N3 C22 1.324(3) . ?
N3 C23 1.399(3) . ?
N3 H3B 0.85(4) . ?
N4 C26 1.468(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.376(3) . ?
C16 C21 1.443(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.426(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.350(3) . ?
C19 H19 0.9500 . ?
C19 C20 1.436(3) . ?
C20 C21 1.443(3) . ?
C20 C22 1.400(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.396(3) . ?
C23 C28 1.405(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.386(3) . ?
C25 C26 1.395(3) . ?
C26 C27 1.391(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.387(3) . ?

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
C2 O1 C1 116.06(18) . . ?
C7 O2 H2 89(7) . . ?
C14 O3 H3 115(2) . . ?
C8 N1 C9 127.3(2) . . ?
C8 N1 H1 113(3) . . ?
C9 N1 H1 120(3) . . ?
O4 N2 C12 117.5(2) . . ?
O5 N2 O4 122.9(2) . . ?
O5 N2 C12 119.58(19) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 125.4(2) . . ?
O1 C2 C7 113.81(19) . . ?
C3 C2 C7 120.8(2) . . ?
C2 C3 H3A 119.6 . . ?
C2 C3 C4 120.8(2) . . ?
C4 C3 H3A 119.6 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.8(2) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.1(2) . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C7 120.51(19) . . ?
C8 C6 C5 118.9(2) . . ?
C8 C6 C7 120.53(19) . . ?
O2 C7 C2 121.5(2) . . ?
O2 C7 C6 121.51(19) . . ?
O2 C7 H2 35(2) . . ?
C2 C7 H2 120(4) . . ?
C6 C7 C2 116.98(19) . . ?
C6 C7 H2 111(4) . . ?
N1 C8 C6 123.0(2) . . ?
N1 C8 H8 118.5 . . ?
C6 C8 H8 118.5 . . ?
N1 C9 C14 116.12(19) . . ?
C10 C9 N1 123.2(2) . . ?
C10 C9 C14 120.6(2) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.3(2) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 Cl1 117.68(17) . . ?
C10 C11 C12 118.9(2) . . ?
C12 C11 Cl1 123.40(17) . . ?
C11 C12 N2 122.4(2) . . ?
C13 C12 N2 116.4(2) . . ?
C13 C12 C11 121.2(2) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.9(2) . . ?
C14 C13 H13 120.1 . . ?
O3 C14 C9 117.18(19) . . ?
O3 C14 C13 123.8(2) . . ?
C13 C14 C9 119.0(2) . . ?
C16 O6 C15 115.82(18) . . ?
C21 O7 H7 107(8) . . ?
C28 O8 H8A 112(2) . . ?
C22 N3 C23 127.1(2) . . ?
C22 N3 H3B 112(3) . . ?
C23 N3 H3B 121(3) . . ?
O9 N4 O10 123.6(2) . . ?
O9 N4 C26 116.9(2) . . ?
O10 N4 C26 119.5(2) . . ?
O6 C15 H15A 109.5 . . ?
O6 C15 H15B 109.5 . . ?
O6 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O6 C16 C17 125.5(2) . . ?
O6 C16 C21 113.52(19) . . ?
C17 C16 C21 120.9(2) . . ?
C16 C17 H17 119.5 . . ?
C16 C17 C18 121.0(2) . . ?
C18 C17 H17 119.5 . . ?
C17 C18 H18 119.7 . . ?
C19 C18 C17 120.6(2) . . ?
C19 C18 H18 119.7 . . ?
C18 C19 H19 120.0 . . ?
C18 C19 C20 120.0(2) . . ?
C20 C19 H19 120.0 . . ?
C19 C20 C21 120.9(2) . . ?
C22 C20 C19 118.8(2) . . ?
C22 C20 C21 120.26(19) . . ?
O7 C21 C16 122.0(2) . . ?
O7 C21 C20 121.50(19) . . ?
C16 C21 C20 116.46(19) . . ?
N3 C22 C20 123.3(2) . . ?
N3 C22 H22 118.4 . . ?
C20 C22 H22 118.4 . . ?
N3 C23 C28 116.91(19) . . ?
C24 C23 N3 122.7(2) . . ?
C24 C23 C28 120.4(2) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 C23 120.4(2) . . ?
C25 C24 H24 119.8 . . ?
C24 C25 Cl2 117.55(17) . . ?
C24 C25 C26 118.5(2) . . ?
C26 C25 Cl2 123.84(17) . . ?
C25 C26 N4 121.5(2) . . ?
C27 C26 N4 116.6(2) . . ?
C27 C26 C25 121.9(2) . . ?
C26 C27 H27 120.3 . . ?
C28 C27 C26 119.3(2) . . ?
C28 C27 H27 120.3 . . ?
O8 C28 C23 116.88(19) . . ?
O8 C28 C27 123.7(2) . . ?
C27 C28 C23 119.5(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl1 C11 C12 N2 2.0(3) . . . . ?
Cl1 C11 C12 C13 -178.64(18) . . . . ?
O1 C2 C3 C4 -177.7(2) . . . . ?
O1 C2 C7 O2 -1.8(3) . . . . ?
O1 C2 C7 C6 177.43(19) . . . . ?
O4 N2 C12 C11 -150.3(3) . . . . ?
O4 N2 C12 C13 30.2(3) . . . . ?
O5 N2 C12 C11 32.1(4) . . . . ?
O5 N2 C12 C13 -147.4(2) . . . . ?
N1 C9 C10 C11 176.6(2) . . . . ?
N1 C9 C14 O3 2.6(3) . . . . ?
N1 C9 C14 C13 -177.9(2) . . . . ?
N2 C12 C13 C14 178.0(2) . . . . ?
C1 O1 C2 C3 5.8(3) . . . . ?
C1 O1 C2 C7 -173.8(2) . . . . ?
C2 C3 C4 C5 -0.3(4) . . . . ?
C3 C2 C7 O2 178.6(2) . . . . ?
C3 C2 C7 C6 -2.1(3) . . . . ?
C3 C4 C5 C6 -0.7(4) . . . . ?
C4 C5 C6 C7 0.3(3) . . . . ?
C4 C5 C6 C8 178.2(2) . . . . ?
C5 C6 C7 O2 -179.6(2) . . . . ?
C5 C6 C7 C2 1.1(3) . . . . ?
C5 C6 C8 N1 -178.4(2) . . . . ?
C7 C2 C3 C4 1.8(4) . . . . ?
C7 C6 C8 N1 -0.4(3) . . . . ?
C8 N1 C9 C10 6.0(4) . . . . ?
C8 N1 C9 C14 -175.9(2) . . . . ?
C8 C6 C7 O2 2.4(3) . . . . ?
C8 C6 C7 C2 -176.8(2) . . . . ?
C9 N1 C8 C6 -177.6(2) . . . . ?
C9 C10 C11 Cl1 -179.88(17) . . . . ?
C9 C10 C11 C12 1.2(3) . . . . ?
C10 C9 C14 O3 -179.2(2) . . . . ?
C10 C9 C14 C13 0.2(3) . . . . ?
C10 C11 C12 N2 -179.2(2) . . . . ?
C10 C11 C12 C13 0.2(3) . . . . ?
C11 C12 C13 C14 -1.4(4) . . . . ?
C12 C13 C14 O3 -179.5(2) . . . . ?
C12 C13 C14 C9 1.2(3) . . . . ?
C14 C9 C10 C11 -1.4(3) . . . . ?
Cl2 C25 C26 N4 3.5(3) . . . . ?
Cl2 C25 C26 C27 -175.35(18) . . . . ?
O6 C16 C17 C18 177.1(2) . . . . ?
O6 C16 C21 O7 2.4(3) . . . . ?
O6 C16 C21 C20 -176.97(19) . . . . ?
O9 N4 C26 C25 -145.2(3) . . . . ?
O9 N4 C26 C27 33.6(4) . . . . ?
O10 N4 C26 C25 35.3(4) . . . . ?
O10 N4 C26 C27 -145.8(2) . . . . ?
N3 C23 C24 C25 -178.3(2) . . . . ?
N3 C23 C28 O8 -2.9(3) . . . . ?
N3 C23 C28 C27 178.0(2) . . . . ?
N4 C26 C27 C28 179.5(2) . . . . ?
C15 O6 C16 C17 -3.8(3) . . . . ?
C15 O6 C16 C21 175.2(2) . . . . ?
C16 C17 C18 C19 0.0(4) . . . . ?
C17 C16 C21 O7 -178.5(2) . . . . ?
C17 C16 C21 C20 2.1(3) . . . . ?
C17 C18 C19 C20 1.4(4) . . . . ?
C18 C19 C20 C21 -1.1(3) . . . . ?
C18 C19 C20 C22 -178.7(2) . . . . ?
C19 C20 C21 O7 180.0(2) . . . . ?
C19 C20 C21 C16 -0.7(3) . . . . ?
C19 C20 C22 N3 178.3(2) . . . . ?
C21 C16 C17 C18 -1.8(4) . . . . ?
C21 C20 C22 N3 0.6(3) . . . . ?
C22 N3 C23 C24 -5.8(4) . . . . ?
C22 N3 C23 C28 176.2(2) . . . . ?
C22 C20 C21 O7 -2.4(3) . . . . ?
C22 C20 C21 C16 176.9(2) . . . . ?
C23 N3 C22 C20 177.6(2) . . . . ?
C23 C24 C25 Cl2 176.55(17) . . . . ?
C23 C24 C25 C26 -0.3(3) . . . . ?
C24 C23 C28 O8 179.0(2) . . . . ?
C24 C23 C28 C27 -0.1(3) . . . . ?
C24 C25 C26 N4 -180.0(2) . . . . ?
C24 C25 C26 C27 1.2(4) . . . . ?
C25 C26 C27 C28 -1.6(4) . . . . ?
C26 C27 C28 O8 -178.0(2) . . . . ?
C26 C27 C28 C23 1.1(3) . . . . ?
C28 C23 C24 C25 -0.3(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_H2L19_CCDC_1406219
_database_code_depnum_ccdc_archive 'CCDC 1406219'
_audit_update_record             
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_audit_creation_date             2014-06-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C20 H16 Br N O3, C H4 O'
_chemical_formula_sum            'C21 H20 Br N O4'
_chemical_formula_weight         430.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         C52H92Si4Ti2Se2
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'

_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                   7.5662(4)
_cell_length_b                   8.5456(4)
_cell_length_c                   14.8304(8)
_cell_angle_alpha                84.747(4)
_cell_angle_beta                 84.775(4)
_cell_angle_gamma                82.090(4)
_cell_volume                     942.80(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5562
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.4480
_cell_measurement_theta_min      3.1630
_exptl_absorpt_coefficient_mu    2.207
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21895
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.68
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.8628
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0526163000
_diffrn_orient_matrix_UB_12      -0.0021442000
_diffrn_orient_matrix_UB_13      -0.0420795000
_diffrn_orient_matrix_UB_21      -0.0236143000
_diffrn_orient_matrix_UB_22      -0.0759093000
_diffrn_orient_matrix_UB_23      -0.0053894000
_diffrn_orient_matrix_UB_31      -0.0754245000
_diffrn_orient_matrix_UB_32      0.0360659000
_diffrn_orient_matrix_UB_33      -0.0228419000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3890
_reflns_number_total             4630
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4630
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0373
_refine_ls_restrained_S_all      1.049
_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)+(0.0264P)²+0.4331P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0768
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 H2-O2
 0.88 with sigma of 0.02
 H2-N1
 2.2 with sigma of 0.02
3. Others
 Sof(H2)=1-FVAR(1)
 Sof(H1)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C17(H17), C3(H3A), C16(H16), C13(H13), C8(H8), C18(H18), C12(H12),
 C20(H20), C5(H5), C19(H19), C10(H10)
4.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C1(H1A,H1B,H1C)
4.c Idealised tetrahedral OH refined as rotating group:
 O4(H4), O3(H3)
;
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 1.02460(3) -0.29134(3) 1.300723(16) 0.02978(8) Uani 1 1 d . . .
O1 O 0.7789(2) 0.31606(16) 1.27407(10) 0.0253(3) Uani 1 1 d . . .
O4 O 0.7925(3) -0.32512(19) 0.94482(13) 0.0450(5) Uani 1 1 d . . .
H4 H 0.7132 -0.3614 0.9810 0.068 Uiso 1 1 calc R . .
O2 O 0.6822(2) 0.30374(17) 1.10658(11) 0.0263(3) Uani 1 1 d D . .
O3 O 0.4756(2) 0.41259(17) 0.91416(10) 0.0286(4) Uani 1 1 d . . .
H3 H 0.4266 0.4978 0.8892 0.043 Uiso 1 1 calc R . .
N1 N 0.6672(2) 0.1477(2) 0.96915(11) 0.0201(4) Uani 1 1 d D . .
H1 H 0.6429 0.2346 0.9980 0.024 Uiso 0.79(4) 1 calc PR A 1
C17 C 0.6772(3) -0.3444(3) 0.64148(17) 0.0313(5) Uani 1 1 d . . .
H17 H 0.6733 -0.4523 0.6626 0.038 Uiso 1 1 calc R . .
C4 C 0.9280(3) -0.1032(2) 1.23457(14) 0.0221(4) Uani 1 1 d . . .
C3 C 0.8973(3) 0.0380(2) 1.27921(14) 0.0216(4) Uani 1 1 d . . .
H3A H 0.9327 0.0383 1.3390 0.026 Uiso 1 1 calc R . .
C16 C 0.6353(3) -0.2271(2) 0.70165(15) 0.0254(5) Uani 1 1 d . . .
H16 H 0.6036 -0.2555 0.7639 0.030 Uiso 1 1 calc R . .
C13 C 0.4530(3) 0.3233(2) 0.76583(15) 0.0248(5) Uani 1 1 d . . .
H13 H 0.3848 0.4202 0.7462 0.030 Uiso 1 1 calc R . .
C11 C 0.5936(3) 0.0590(2) 0.73526(14) 0.0203(4) Uani 1 1 d . . .
C21 C 0.8845(4) -0.4475(3) 0.89412(19) 0.0407(6) Uani 1 1 d . . .
H21A H 0.8046 -0.4781 0.8523 0.061 Uiso 1 1 calc R . .
H21B H 0.9235 -0.5393 0.9355 0.061 Uiso 1 1 calc R . .
H21C H 0.9892 -0.4101 0.8594 0.061 Uiso 1 1 calc R . .
C1 C 0.8082(4) 0.3166(3) 1.36731(16) 0.0376(6) Uani 1 1 d . . .
H1A H 0.9358 0.2868 1.3755 0.056 Uiso 1 1 calc R . .
H1B H 0.7392 0.2405 1.4034 0.056 Uiso 1 1 calc R . .
H1C H 0.7696 0.4229 1.3874 0.056 Uiso 1 1 calc R . .
C2 C 0.8171(3) 0.1740(2) 1.23677(14) 0.0207(4) Uani 1 1 d . . .
C8 C 0.7516(3) 0.0251(2) 1.01357(14) 0.0203(4) Uani 1 1 d . . .
H8 H 0.7797 -0.0718 0.9855 0.024 Uiso 1 1 calc R . .
C18 C 0.7247(3) -0.3048(3) 0.55111(17) 0.0356(6) Uani 1 1 d . . .
H18 H 0.7537 -0.3853 0.5101 0.043 Uiso 1 1 calc R . .
C12 C 0.4950(3) 0.2038(2) 0.70794(15) 0.0240(5) Uani 1 1 d . . .
H12 H 0.4561 0.2200 0.6483 0.029 Uiso 1 1 calc R . .
C6 C 0.8024(3) 0.0327(2) 1.10222(14) 0.0196(4) Uani 1 1 d . . .
C20 C 0.6877(3) -0.0311(3) 0.58037(15) 0.0304(5) Uani 1 1 d . . .
H20 H 0.6920 0.0765 0.5586 0.037 Uiso 1 1 calc R . .
C9 C 0.6102(3) 0.1581(2) 0.88075(14) 0.0194(4) Uani 1 1 d . . .
C5 C 0.8850(3) -0.1078(2) 1.14852(14) 0.0211(4) Uani 1 1 d . . .
H5 H 0.9097 -0.2037 1.1193 0.025 Uiso 1 1 calc R . .
C19 C 0.7298(4) -0.1483(3) 0.52055(16) 0.0370(6) Uani 1 1 d . . .
H19 H 0.7624 -0.1207 0.4583 0.044 Uiso 1 1 calc R . .
C7 C 0.7633(3) 0.1774(2) 1.14597(14) 0.0193(4) Uani 1 1 d . . .
C14 C 0.5105(3) 0.3016(2) 0.85241(14) 0.0211(4) Uani 1 1 d . . .
C15 C 0.6393(3) -0.0681(2) 0.67166(14) 0.0208(4) Uani 1 1 d . . .
C10 C 0.6491(3) 0.0373(2) 0.82269(14) 0.0194(4) Uani 1 1 d . . .
H10 H 0.7142 -0.0608 0.8429 0.023 Uiso 1 1 calc R . .
H2 H 0.75(2) 0.32(2) 1.056(6) 0.15(11) Uiso 0.21(4) 1 d PD A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C4 1.897(2) . ?
O1 C1 1.421(3) . ?
O1 C2 1.364(2) . ?
O4 H4 0.8400 . ?
O4 C21 1.411(3) . ?
O2 C7 1.285(2) . ?
O2 H2 0.88(2) . ?
O3 H3 0.8400 . ?
O3 C14 1.362(2) . ?
N1 H1 0.8800 . ?
N1 C8 1.306(2) . ?
N1 C9 1.408(3) . ?
C17 H17 0.9500 . ?
C17 C16 1.388(3) . ?
C17 C18 1.379(4) . ?
C4 C3 1.410(3) . ?
C4 C5 1.351(3) . ?
C3 H3A 0.9500 . ?
C3 C2 1.362(3) . ?
C16 H16 0.9500 . ?
C16 C15 1.395(3) . ?
C13 H13 0.9500 . ?
C13 C12 1.380(3) . ?
C13 C14 1.382(3) . ?
C11 C12 1.400(3) . ?
C11 C15 1.488(3) . ?
C11 C10 1.388(3) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C7 1.438(3) . ?
C8 H8 0.9500 . ?
C8 C6 1.412(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.377(3) . ?
C12 H12 0.9500 . ?
C6 C5 1.423(3) . ?
C6 C7 1.432(3) . ?
C20 H20 0.9500 . ?
C20 C19 1.384(3) . ?
C20 C15 1.389(3) . ?
C9 C14 1.399(3) . ?
C9 C10 1.387(3) . ?
C5 H5 0.9500 . ?
C19 H19 0.9500 . ?
C10 H10 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 O1 C1 116.74(16) . . ?
C21 O4 H4 109.5 . . ?
C7 O2 H2 102(10) . . ?
C14 O3 H3 109.5 . . ?
C8 N1 H1 116.0 . . ?
C8 N1 C9 128.03(18) . . ?
C9 N1 H1 116.0 . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C18 C17 C16 120.2(2) . . ?
C3 C4 Br1 117.92(15) . . ?
C5 C4 Br1 120.18(16) . . ?
C5 C4 C3 121.86(19) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 C4 120.18(19) . . ?
C2 C3 H3A 119.9 . . ?
C17 C16 H16 119.7 . . ?
C17 C16 C15 120.6(2) . . ?
C15 C16 H16 119.7 . . ?
C12 C13 H13 120.1 . . ?
C12 C13 C14 119.76(19) . . ?
C14 C13 H13 120.1 . . ?
C12 C11 C15 120.72(18) . . ?
C10 C11 C12 118.49(19) . . ?
C10 C11 C15 120.79(18) . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C7 113.86(17) . . ?
C3 C2 O1 124.97(18) . . ?
C3 C2 C7 121.17(18) . . ?
N1 C8 H8 119.1 . . ?
N1 C8 C6 121.80(18) . . ?
C6 C8 H8 119.1 . . ?
C17 C18 H18 120.1 . . ?
C19 C18 C17 119.8(2) . . ?
C19 C18 H18 120.1 . . ?
C13 C12 C11 121.41(19) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C8 C6 C5 118.74(18) . . ?
C8 C6 C7 120.34(18) . . ?
C5 C6 C7 120.84(18) . . ?
C19 C20 H20 119.4 . . ?
C19 C20 C15 121.1(2) . . ?
C15 C20 H20 119.4 . . ?
C14 C9 N1 115.84(18) . . ?
C10 C9 N1 123.93(18) . . ?
C10 C9 C14 120.23(19) . . ?
C4 C5 C6 119.20(19) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 H5 120.4 . . ?
C18 C19 C20 120.1(2) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
O2 C7 C2 121.59(18) . . ?
O2 C7 C6 121.72(18) . . ?
C6 C7 C2 116.69(17) . . ?
O3 C14 C13 123.91(18) . . ?
O3 C14 C9 116.43(18) . . ?
C13 C14 C9 119.66(19) . . ?
C16 C15 C11 121.23(19) . . ?
C20 C15 C16 118.1(2) . . ?
C20 C15 C11 120.67(19) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 C11 120.43(18) . . ?
C9 C10 H10 119.8 . . ?

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
Br1 C4 C3 C2 -175.60(16) . . . . ?
Br1 C4 C5 C6 176.09(15) . . . . ?
O1 C2 C7 O2 -1.9(3) . . . . ?
O1 C2 C7 C6 178.89(17) . . . . ?
N1 C8 C6 C5 176.49(19) . . . . ?
N1 C8 C6 C7 -0.5(3) . . . . ?
N1 C9 C14 O3 -1.9(3) . . . . ?
N1 C9 C14 C13 178.41(19) . . . . ?
N1 C9 C10 C11 -177.58(19) . . . . ?
C17 C16 C15 C11 179.6(2) . . . . ?
C17 C16 C15 C20 -0.5(3) . . . . ?
C17 C18 C19 C20 0.1(4) . . . . ?
C4 C3 C2 O1 179.02(19) . . . . ?
C4 C3 C2 C7 -0.5(3) . . . . ?
C3 C4 C5 C6 -1.6(3) . . . . ?
C3 C2 C7 O2 177.65(19) . . . . ?
C3 C2 C7 C6 -1.5(3) . . . . ?
C16 C17 C18 C19 -0.2(4) . . . . ?
C1 O1 C2 C3 -7.1(3) . . . . ?
C1 O1 C2 C7 172.5(2) . . . . ?
C8 N1 C9 C14 175.5(2) . . . . ?
C8 N1 C9 C10 -5.3(3) . . . . ?
C8 C6 C5 C4 -177.52(19) . . . . ?
C8 C6 C7 O2 -0.2(3) . . . . ?
C8 C6 C7 C2 179.00(19) . . . . ?
C18 C17 C16 C15 0.4(3) . . . . ?
C12 C13 C14 O3 -180.0(2) . . . . ?
C12 C13 C14 C9 -0.3(3) . . . . ?
C12 C11 C15 C16 -141.0(2) . . . . ?
C12 C11 C15 C20 39.1(3) . . . . ?
C12 C11 C10 C9 -1.2(3) . . . . ?
C9 N1 C8 C6 179.31(19) . . . . ?
C5 C4 C3 C2 2.2(3) . . . . ?
C5 C6 C7 O2 -177.13(19) . . . . ?
C5 C6 C7 C2 2.1(3) . . . . ?
C19 C20 C15 C16 0.4(3) . . . . ?
C19 C20 C15 C11 -179.7(2) . . . . ?
C7 C6 C5 C4 -0.5(3) . . . . ?
C14 C13 C12 C11 0.7(3) . . . . ?
C14 C9 C10 C11 1.6(3) . . . . ?
C15 C11 C12 C13 -179.4(2) . . . . ?
C15 C11 C10 C9 178.20(19) . . . . ?
C15 C20 C19 C18 -0.2(4) . . . . ?
C10 C11 C12 C13 0.0(3) . . . . ?
C10 C11 C15 C16 39.6(3) . . . . ?
C10 C11 C15 C20 -140.3(2) . . . . ?
C10 C9 C14 O3 178.86(18) . . . . ?
C10 C9 C14 C13 -0.9(3) . . . . ?

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4_CCDC_1406220
_database_code_depnum_ccdc_archive 'CCDC 1406220'
_audit_update_record             
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_audit_creation_date             2015-01-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C28 H20 Co N4 O10, 2(C H4 O), C6 H16 N'
_chemical_formula_sum            'C36 H44 Co N5 O12'
_chemical_formula_weight         797.69
_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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.8624(5)
_cell_length_b                   17.0300(4)
_cell_length_c                   25.6461(18)
_cell_angle_alpha                90
_cell_angle_beta                 108.353(8)
_cell_angle_gamma                90
_cell_volume                     7819.2(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    100
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3344
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            61781
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.052
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11644
_reflns_number_total             17458
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.400
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.098
_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     955
_refine_ls_number_reflns         17458
_refine_ls_number_restraints     93
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0855
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1081P)²+18.2835P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2181
_refine_ls_wR_factor_ref         0.2379
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C18-N206
 1.42 with sigma of 0.02
 N3-C18
 1.42 with sigma of 0.02
 N29-C162
 1.51 with sigma of 0.02
 C8-N1
 1.51 with sigma of 0.02
 N1-C1
 1.51 with sigma of 0.02
 C6-C1
 1.51 with sigma of 0.02
 C2-N1
 1.51 with sigma of 0.02
 C4-C2
 1.51 with sigma of 0.02
 C5-C8
 1.51 with sigma of 0.02
3. Rigid bond restraints
 N1, C1, C2, C4, C5, C6, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim C2 \\sim C4 \\sim C5 \\sim C6 \\sim C8: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C19) = Uanis(C18) = Uanis(C17) = Uanis(C16) = Uanis(C21) = Uanis(C20)
5. Rigid body (RIGU) restrains
 N1, C1, C2, C4, C5, C6, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O5(0.5) O78(0.5) O78A(0.5) O104(0.5) N3(0.5) N206(0.5)
7.a Riding coordinates:
 C2AA(H2AA,H2AB,H2AC), C8(H8A,H8B)
7.b Ternary CH refined with riding coordinates:
 N1(H1), N29(H29)
7.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C68(H68A,H68B), C125(H12A,H12B), C162(H16A,H16B)
7.d Me refined with riding coordinates:
 C0AA(H0AA,H0AB,H0AC), C121(H12D,H12E,H12F)
7.e Aromatic/amide H refined with riding coordinates:
 C31(H31), C33(H33), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
 C45(H45), C47(H47), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C3(H3),
 C5AA(H5AA), C7AA(H7AA), C10(H10), C11(H11), C12(H12), C13(H13), C17(H17),
 C19(H19), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27)
7.f Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C43(H43A,H43B,H43C), C15(H15A,H15B,H15C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C),
 C6AA(H6AA,H6AB,H6AC), C210(H21A,H21B,H21C), C226(H22A,H22B,H22C)
7.g Idealised tetrahedral OH refined as rotating group:
 O82(H82), O74(H74), O12(H12C), O14(H14)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co2 Co 0.65583(3) 0.87373(3) 0.54013(2) 0.02553(15) Uani 1 1 d . . . . .
O4 O 0.25223(19) 0.7940(3) 0.43411(19) 0.0637(12) Uani 1 1 d . . . . .
O8 O 0.91530(17) 0.95320(19) 0.38445(14) 0.0365(7) Uani 1 1 d . . . . .
O19 O 0.54379(17) 0.7020(2) 0.40906(14) 0.0386(8) Uani 1 1 d . . . . .
O33 O 0.26704(19) 0.7156(2) 0.37186(16) 0.0523(10) Uani 1 1 d . . . . .
O39 O 0.62979(17) 1.06075(18) 0.41488(13) 0.0342(7) Uani 1 1 d . . . . .
O48 O 0.84956(18) 1.0532(2) 0.34350(13) 0.0397(8) Uani 1 1 d . . . . .
O49 O 0.59931(15) 0.80303(17) 0.48558(12) 0.0282(6) Uani 1 1 d . . . . .
O65 O 0.65230(15) 0.94763(17) 0.48399(12) 0.0285(6) Uani 1 1 d . . . . .
O102 O 0.65672(16) 0.80107(17) 0.59627(12) 0.0306(7) Uani 1 1 d . . . . .
O108 O 0.71489(16) 0.94466(17) 0.59307(13) 0.0325(7) Uani 1 1 d . . . . .
N13 N 0.57210(19) 0.9238(2) 0.55219(14) 0.0276(7) Uani 1 1 d . . . . .
N79 N 0.2925(2) 0.7601(3) 0.41164(19) 0.0452(10) Uani 1 1 d . . . . .
N98 N 0.8603(2) 0.9965(2) 0.37550(15) 0.0311(8) Uani 1 1 d . . . . .
N207 N 0.74486(19) 0.8225(2) 0.53779(14) 0.0268(7) Uani 1 1 d . . . . .
C29 C 0.6134(3) 1.1221(3) 0.3743(3) 0.0559(16) Uani 1 1 d . . . . .
H29A H 0.6060 1.0992 0.3379 0.084 Uiso 1 1 calc GR . . . .
H29B H 0.6552 1.1592 0.3828 0.084 Uiso 1 1 calc GR . . . .
H29C H 0.5679 1.1497 0.3745 0.084 Uiso 1 1 calc GR . . . .
C30 C 0.6936(2) 1.0180(2) 0.42110(17) 0.0276(9) Uani 1 1 d . . . . .
C31 C 0.7445(2) 1.0323(3) 0.39450(17) 0.0283(9) Uani 1 1 d . . . . .
H31 H 0.7382 1.0752 0.3698 0.034 Uiso 1 1 calc R . . . .
C32 C 0.8066(2) 0.9821(3) 0.40445(16) 0.0275(9) Uani 1 1 d . . . . .
C33 C 0.8174(2) 0.9202(2) 0.43956(16) 0.0264(9) Uani 1 1 d . . . . .
H33 H 0.8594 0.8867 0.4447 0.032 Uiso 1 1 calc R . . . .
C34 C 0.7664(2) 0.9060(2) 0.46818(17) 0.0258(8) Uani 1 1 d . . . . .
C35 C 0.7029(2) 0.9548(2) 0.46008(16) 0.0247(8) Uani 1 1 d . . . . .
C36 C 0.7834(2) 0.8415(2) 0.50606(17) 0.0268(9) Uani 1 1 d . . . . .
H36 H 0.8261 0.8106 0.5080 0.032 Uiso 1 1 calc R . . . .
C37 C 0.7664(2) 0.7633(2) 0.57807(18) 0.0289(9) Uani 1 1 d . . . . .
C38 C 0.8300(2) 0.7154(3) 0.58901(19) 0.0337(10) Uani 1 1 d . . . . .
H38 H 0.8629 0.7207 0.5678 0.040 Uiso 1 1 calc R . . . .
C39 C 0.8445(3) 0.6606(3) 0.6309(2) 0.0392(11) Uani 1 1 d . . . . .
H39 H 0.8872 0.6277 0.6383 0.047 Uiso 1 1 calc R . . . .
C40 C 0.7964(3) 0.6537(3) 0.6622(2) 0.0395(11) Uani 1 1 d . . . . .
H40 H 0.8072 0.6166 0.6913 0.047 Uiso 1 1 calc R . . . .
C41 C 0.7331(3) 0.7002(3) 0.65175(19) 0.0349(10) Uani 1 1 d . . . . .
H41 H 0.7010 0.6948 0.6735 0.042 Uiso 1 1 calc R . . . .
C42 C 0.7165(2) 0.7557(2) 0.60850(18) 0.0289(9) Uani 1 1 d . . . . .
C43 C 0.5158(3) 0.6410(4) 0.3694(3) 0.0593(17) Uani 1 1 d . . . . .
H43A H 0.4814 0.6637 0.3358 0.089 Uiso 1 1 calc GR . . . .
H43B H 0.4893 0.6020 0.3844 0.089 Uiso 1 1 calc GR . . . .
H43C H 0.5576 0.6158 0.3609 0.089 Uiso 1 1 calc GR . . . .
C44 C 0.4933(2) 0.7398(3) 0.42870(18) 0.0307(9) Uani 1 1 d . . . . .
C45 C 0.4178(2) 0.7276(3) 0.4104(2) 0.0358(10) Uani 1 1 d . . . . .
H45 H 0.3967 0.6893 0.3829 0.043 Uiso 1 1 calc R . . . .
C46 C 0.3721(2) 0.7722(3) 0.4327(2) 0.0352(10) Uani 1 1 d . . . . .
C47 C 0.4003(2) 0.8291(3) 0.47171(19) 0.0327(10) Uani 1 1 d . . . . .
H47 H 0.3679 0.8594 0.4855 0.039 Uiso 1 1 calc R . . . .
C48 C 0.4782(2) 0.8418(2) 0.49104(17) 0.0268(9) Uani 1 1 d . . . . .
C49 C 0.5269(2) 0.7966(2) 0.47028(17) 0.0272(9) Uani 1 1 d . . . . .
C50 C 0.5027(2) 0.9039(3) 0.53001(17) 0.0287(9) Uani 1 1 d . . . . .
H50 H 0.4659 0.9325 0.5403 0.034 Uiso 1 1 calc R . . . .
C51 C 0.5949(2) 0.9844(2) 0.59268(18) 0.0297(9) Uani 1 1 d . . . . .
C52 C 0.5485(3) 1.0317(3) 0.61222(18) 0.0332(10) Uani 1 1 d . . . . .
H52 H 0.4958 1.0254 0.5987 0.040 Uiso 1 1 calc R . . . .
C53 C 0.5800(3) 1.0878(3) 0.6515(2) 0.0367(10) Uani 1 1 d . . . . .
H53 H 0.5489 1.1204 0.6651 0.044 Uiso 1 1 calc R . . . .
C54 C 0.6575(3) 1.0968(3) 0.6714(2) 0.0386(11) Uani 1 1 d . . . . .
H54 H 0.6786 1.1356 0.6984 0.046 Uiso 1 1 calc R . . . .
C55 C 0.7038(3) 1.0500(3) 0.6521(2) 0.0374(11) Uani 1 1 d . . . . .
H55 H 0.7565 1.0569 0.6658 0.045 Uiso 1 1 calc R . . . .
C56 C 0.6728(2) 0.9924(3) 0.61243(18) 0.0312(9) Uani 1 1 d . . . . .
Co4 Co 0.85140(3) 0.62253(3) 0.42691(3) 0.02929(16) Uani 1 1 d . . . . .
O5_b O 0.6167(4) 0.4997(5) 0.6095(3) 0.0512(19) Uiso 0.5 1 d . . P A 2
O26 O 0.96003(17) 0.82739(18) 0.52993(14) 0.0372(7) Uani 1 1 d . . . . .
O27 O 0.85388(17) 0.45982(19) 0.56465(14) 0.0372(8) Uani 1 1 d . . . . .
O32 O 1.2323(2) 0.7659(2) 0.61970(17) 0.0545(10) Uani 1 1 d . . . . .
O45 O 1.24804(19) 0.6528(2) 0.58746(18) 0.0566(11) Uani 1 1 d . . . . .
O64 O 0.84504(16) 0.56032(18) 0.48708(14) 0.0351(7) Uani 1 1 d . . . . .
O69 O 0.90518(15) 0.70088(17) 0.47672(12) 0.0290(6) Uani 1 1 d . . . . .
O78_a O 0.5369(6) 0.5404(6) 0.5287(4) 0.078(3) Uiso 0.5 1 d . . P B 1
O78A_b O 0.5684(5) 0.6068(5) 0.5661(3) 0.058(2) Uiso 0.5 1 d . . P A 2
O104_a O 0.6014(5) 0.4581(5) 0.5910(4) 0.057(2) Uiso 0.5 1 d . . P B 1
O111 O 0.86123(16) 0.68478(18) 0.36821(13) 0.0325(7) Uani 1 1 d . . . . .
O112 O 0.79589(17) 0.54685(18) 0.37650(15) 0.0383(8) Uani 1 1 d . . . . .
N3_b N 0.6158(5) 0.5538(5) 0.5757(3) 0.0424(19) Uiso 0.5 1 d D . P A 2
N31 N 0.9368(2) 0.5621(2) 0.42840(16) 0.0301(8) Uani 1 1 d . . . . .
N35 N 0.76201(19) 0.6793(2) 0.41871(15) 0.0296(8) Uani 1 1 d . . . . .
N115 N 1.2082(2) 0.7087(3) 0.59038(19) 0.0433(10) Uani 1 1 d . . . . .
N206_a N 0.5970(5) 0.5058(6) 0.5528(4) 0.054(2) Uiso 0.5 1 d D . P B 1
C0AA C 0.9913(3) 0.9033(3) 0.5471(2) 0.0440(12) Uani 1 1 d . . . . .
H0AA H 1.0236 0.9185 0.5254 0.066 Uiso 1 1 calc R . . . .
H0AB H 1.0207 0.9017 0.5861 0.066 Uiso 1 1 calc R . . . .
H0AC H 0.9510 0.9418 0.5415 0.066 Uiso 1 1 calc R . . . .
C1AA C 1.0100(2) 0.7682(3) 0.53190(19) 0.0310(9) Uani 1 1 d . . . . .
C3 C 1.0842(2) 0.7717(3) 0.56126(19) 0.0326(10) Uani 1 1 d . . . . .
H3 H 1.1047 0.8166 0.5827 0.039 Uiso 1 1 calc R . . . .
C3AA C 1.1298(2) 0.7063(3) 0.5587(2) 0.0363(10) Uani 1 1 d . . . . .
C4AA C 1.0264(2) 0.6386(3) 0.49728(19) 0.0317(9) Uani 1 1 d . . . . .
C5AA C 1.1025(3) 0.6420(3) 0.5277(2) 0.0349(10) Uani 1 1 d . . . . .
H5AA H 1.1347 0.5995 0.5266 0.042 Uiso 1 1 calc R . . . .
C7 C 0.9767(2) 0.7005(3) 0.50043(18) 0.0290(9) Uani 1 1 d . . . . .
C7AA C 1.0036(2) 0.5719(3) 0.46213(19) 0.0325(10) Uani 1 1 d . . . . .
H7AA H 1.0397 0.5324 0.4636 0.039 Uiso 1 1 calc R . . . .
C9 C 0.9173(3) 0.4989(2) 0.39031(19) 0.0313(9) Uani 1 1 d . . . . .
C10 C 0.9665(3) 0.4454(3) 0.3792(2) 0.0368(11) Uani 1 1 d . . . . .
H10 H 1.0186 0.4485 0.3980 0.044 Uiso 1 1 calc R . . . .
C11 C 0.9382(3) 0.3874(3) 0.3404(2) 0.0402(11) Uani 1 1 d . . . . .
H11 H 0.9711 0.3504 0.3325 0.048 Uiso 1 1 calc R . . . .
C12 C 0.8622(3) 0.3832(3) 0.3130(2) 0.0462(13) Uani 1 1 d . . . . .
H12 H 0.8437 0.3435 0.2862 0.055 Uiso 1 1 calc R . . . .
C13 C 0.8127(3) 0.4360(3) 0.3240(2) 0.0401(11) Uani 1 1 d . . . . .
H13 H 0.7606 0.4322 0.3052 0.048 Uiso 1 1 calc R . . . .
C14 C 0.8404(2) 0.4949(3) 0.3633(2) 0.0337(10) Uani 1 1 d . . . . .
C15 C 0.8595(3) 0.4004(4) 0.6044(3) 0.0611(17) Uani 1 1 d . . . . .
H15A H 0.8205 0.3610 0.5896 0.092 Uiso 1 1 calc GR . . . .
H15B H 0.8533 0.4238 0.6376 0.092 Uiso 1 1 calc GR . . . .
H15C H 0.9087 0.3754 0.6135 0.092 Uiso 1 1 calc GR . . . .
C16 C 0.7884(3) 0.5002(4) 0.5456(2) 0.0488(6) Uani 1 1 d . . . . .
C17 C 0.7292(3) 0.4893(4) 0.5647(2) 0.0488(6) Uani 1 1 d . . . . .
H17 H 0.7298 0.4492 0.5906 0.059 Uiso 1 1 calc R . . . .
C18 C 0.6674(3) 0.5395(4) 0.5447(2) 0.0488(6) Uani 1 1 d D . . . .
C19 C 0.6644(3) 0.5970(4) 0.5067(2) 0.0488(6) Uani 1 1 d . . . . .
H19 H 0.6225 0.6310 0.4953 0.059 Uiso 1 1 calc R . . . .
C20 C 0.7232(3) 0.6056(4) 0.4845(2) 0.0488(6) Uani 1 1 d . . . . .
C21 C 0.7871(3) 0.5570(4) 0.5036(2) 0.0488(6) Uani 1 1 d . . . . .
C22 C 0.7154(2) 0.6664(3) 0.44503(19) 0.0334(10) Uani 1 1 d . . . . .
H22 H 0.6729 0.6996 0.4377 0.040 Uiso 1 1 calc R . . . .
C23 C 0.7502(2) 0.7377(2) 0.37738(19) 0.0315(10) Uani 1 1 d . . . . .
C24 C 0.6904(3) 0.7906(3) 0.3613(2) 0.0373(11) Uani 1 1 d . . . . .
H24 H 0.6519 0.7893 0.3779 0.045 Uiso 1 1 calc R . . . .
C25 C 0.6886(3) 0.8447(3) 0.3209(2) 0.0389(11) Uani 1 1 d . . . . .
H25 H 0.6486 0.8812 0.3097 0.047 Uiso 1 1 calc R . . . .
C26 C 0.7448(3) 0.8463(3) 0.2965(2) 0.0405(11) Uani 1 1 d . . . . .
H26 H 0.7429 0.8842 0.2689 0.049 Uiso 1 1 calc R . . . .
C27 C 0.8035(3) 0.7936(3) 0.31184(19) 0.0364(10) Uani 1 1 d . . . . .
H27 H 0.8415 0.7954 0.2948 0.044 Uiso 1 1 calc R . . . .
C28 C 0.8069(2) 0.7380(3) 0.35218(19) 0.0324(10) Uani 1 1 d . . . . .
O82 O 0.6523(2) 0.5155(3) 0.3438(2) 0.0785(15) Uani 1 1 d . . . . .
H82 H 0.6975 0.5201 0.3624 0.118 Uiso 1 1 calc GR . . . .
C2AA C 0.6378(4) 0.5588(6) 0.2947(3) 0.094(3) Uani 1 1 d . . . . .
H2AA H 0.5858 0.5506 0.2719 0.141 Uiso 1 1 d R . . . .
H2AB H 0.6713 0.5411 0.2747 0.141 Uiso 1 1 d R . . . .
H2AC H 0.6462 0.6147 0.3034 0.141 Uiso 1 1 d R . . . .
O74 O 0.8583(2) 0.9735(2) 0.61099(18) 0.0538(10) Uani 1 1 d . . . . .
H74 H 0.8126 0.9650 0.6054 0.081 Uiso 1 1 calc GR . . . .
C58 C 0.8672(4) 1.0449(4) 0.5854(3) 0.0670(18) Uani 1 1 d . . . . .
H58A H 0.8376 1.0431 0.5464 0.100 Uiso 1 1 calc GR . . . .
H58B H 0.9201 1.0522 0.5889 0.100 Uiso 1 1 calc GR . . . .
H58C H 0.8502 1.0887 0.6032 0.100 Uiso 1 1 calc GR . . . .
O12 O 0.5531(2) 0.7142(4) 0.14476(19) 0.0810(16) Uani 1 1 d . . . . .
H12C H 0.5828 0.7210 0.1267 0.122 Uiso 1 1 calc GR . . . .
C59 C 0.5885(4) 0.6725(5) 0.1922(3) 0.076(2) Uani 1 1 d . . . . .
H59A H 0.6161 0.6285 0.1834 0.115 Uiso 1 1 calc GR . . . .
H59B H 0.5511 0.6524 0.2081 0.115 Uiso 1 1 calc GR . . . .
H59C H 0.6232 0.7072 0.2188 0.115 Uiso 1 1 calc GR . . . .
O14 O 0.9891(2) 0.7090(2) 0.3466(2) 0.0600(11) Uani 1 1 d . . . . .
H14 H 0.9449 0.7078 0.3474 0.090 Uiso 1 1 calc GR . . . .
C121 C 1.0256(4) 0.7771(4) 0.3749(3) 0.0713(19) Uani 1 1 d . . . . .
H12D H 1.0669 0.7915 0.3613 0.107 Uiso 1 1 calc R . . . .
H12E H 1.0451 0.7661 0.4143 0.107 Uiso 1 1 calc R . . . .
H12F H 0.9898 0.8206 0.3685 0.107 Uiso 1 1 calc R . . . .
N1 N 0.5600(5) 0.3751(5) 0.3632(4) 0.140(3) Uani 1 1 d D U . . .
H1 H 0.5958 0.4194 0.3662 0.168 Uiso 1 1 calc R . . . .
C1 C 0.5926(5) 0.3377(5) 0.4268(5) 0.113(3) Uani 1 1 d D U . . .
H1A H 0.5519 0.3116 0.4369 0.135 Uiso 1 1 calc R . . . .
H1B H 0.6322 0.2985 0.4288 0.135 Uiso 1 1 calc R . . . .
C2 C 0.5772(5) 0.3252(7) 0.3189(5) 0.137(4) Uani 1 1 d D U . . .
H2A H 0.6228 0.3514 0.3164 0.164 Uiso 1 1 calc R . . . .
H2B H 0.5956 0.2763 0.3396 0.164 Uiso 1 1 calc R . . . .
C4 C 0.5472(6) 0.2956(11) 0.2652(5) 0.181(6) Uani 1 1 d D U . . .
H4A H 0.5179 0.3367 0.2412 0.271 Uiso 1 1 calc GR . . . .
H4B H 0.5149 0.2507 0.2654 0.271 Uiso 1 1 calc GR . . . .
H4C H 0.5879 0.2789 0.2516 0.271 Uiso 1 1 calc GR . . . .
C5_a C 0.4756(7) 0.4675(7) 0.2768(5) 0.151(4) Uani 1 1 d D U . C 1
H5A_a H 0.4294 0.4980 0.2693 0.226 Uiso 1 1 calc GR . . C 1
H5B_a H 0.4729 0.4340 0.2452 0.226 Uiso 1 1 calc GR . . C 1
H5C_a H 0.5182 0.5034 0.2835 0.226 Uiso 1 1 calc GR . . C 1
C6 C 0.6207(7) 0.3982(8) 0.4613(6) 0.164(4) Uani 1 1 d D U . . .
H6A H 0.6632 0.4211 0.4526 0.246 Uiso 1 1 calc GR . . . .
H6B H 0.6371 0.3791 0.4993 0.246 Uiso 1 1 calc GR . . . .
H6C H 0.5819 0.4383 0.4571 0.246 Uiso 1 1 calc GR . . . .
C8 C 0.4858(7) 0.4149(7) 0.3290(6) 0.186(5) Uani 1 1 d D U . . .
H8A H 0.4502 0.3713 0.3151 0.223 Uiso 1 1 d R . . C .
H8B H 0.4662 0.4448 0.3547 0.223 Uiso 1 1 d R . . . .
N29 N 0.9356(3) 0.6010(3) 0.2104(2) 0.0555(12) Uani 1 1 d D . . . .
H29 H 0.9057 0.5681 0.1787 0.067 Uiso 1 1 calc R . . . .
C6AA C 1.0192(4) 0.4853(4) 0.2402(3) 0.081(2) Uani 1 1 d . . . . .
H6AA H 0.9904 0.4586 0.2063 0.121 Uiso 1 1 calc GR . . . .
H6AB H 1.0364 0.4467 0.2698 0.121 Uiso 1 1 calc GR . . . .
H6AC H 1.0623 0.5116 0.2345 0.121 Uiso 1 1 calc GR . . . .
C68 C 0.9698(4) 0.5460(4) 0.2557(2) 0.0598(16) Uani 1 1 d . . . . .
H68A H 0.9299 0.5187 0.2661 0.072 Uiso 1 1 calc R . . . .
H68B H 1.0002 0.5760 0.2881 0.072 Uiso 1 1 calc R . . . .
C125 C 0.9931(4) 0.6457(5) 0.1903(3) 0.0707(19) Uani 1 1 d . . . . .
H12A H 1.0222 0.6073 0.1764 0.085 Uiso 1 1 calc R . . . .
H12B H 0.9660 0.6799 0.1592 0.085 Uiso 1 1 calc R . . . .
C162 C 0.8827(4) 0.6578(4) 0.2215(3) 0.0633(16) Uani 1 1 d D . . . .
H16A H 0.8657 0.6948 0.1903 0.076 Uiso 1 1 calc R . . . .
H16B H 0.9090 0.6886 0.2547 0.076 Uiso 1 1 calc R . . . .
C210 C 0.8143(3) 0.6179(3) 0.2301(2) 0.0427(12) Uani 1 1 d . . . . .
H21A H 0.7903 0.5840 0.1986 0.064 Uiso 1 1 calc GR . . . .
H21B H 0.7788 0.6581 0.2335 0.064 Uiso 1 1 calc GR . . . .
H21C H 0.8301 0.5862 0.2637 0.064 Uiso 1 1 calc GR . . . .
C226 C 1.0460(5) 0.6950(5) 0.2335(4) 0.101(3) Uani 1 1 d . . . . .
H22A H 1.0822 0.7196 0.2184 0.151 Uiso 1 1 calc GR . . . .
H22B H 1.0723 0.6620 0.2648 0.151 Uiso 1 1 calc GR . . . .
H22C H 1.0180 0.7359 0.2455 0.151 Uiso 1 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
Co2 O49 1.898(3) . ?
Co2 O65 1.898(3) . ?
Co2 O102 1.894(3) . ?
Co2 O108 1.895(3) . ?
Co2 N13 1.904(3) . ?
Co2 N207 1.910(3) . ?
O4 N79 1.232(5) . ?
O8 N98 1.235(5) . ?
O19 C43 1.433(6) . ?
O19 C44 1.370(5) . ?
O33 N79 1.240(5) . ?
O39 C29 1.438(5) . ?
O39 C30 1.372(5) . ?
O48 N98 1.242(5) . ?
O49 C49 1.302(5) . ?
O65 C35 1.292(5) . ?
O102 C42 1.320(5) . ?
O108 C56 1.336(5) . ?
N13 C50 1.297(5) . ?
N13 C51 1.431(6) . ?
N79 C46 1.441(6) . ?
N98 C32 1.452(5) . ?
N207 C36 1.292(5) . ?
N207 C37 1.410(5) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.364(6) . ?
C30 C35 1.441(6) . ?
C31 H31 0.9500 . ?
C31 C32 1.407(6) . ?
C32 C33 1.359(6) . ?
C33 H33 0.9500 . ?
C33 C34 1.403(6) . ?
C34 C35 1.419(6) . ?
C34 C36 1.434(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.403(6) . ?
C37 C42 1.405(6) . ?
C38 H38 0.9500 . ?
C38 C39 1.384(6) . ?
C39 H39 0.9500 . ?
C39 C40 1.393(7) . ?
C40 H40 0.9500 . ?
C40 C41 1.387(6) . ?
C41 H41 0.9500 . ?
C41 C42 1.415(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.367(6) . ?
C44 C49 1.432(6) . ?
C45 H45 0.9500 . ?
C45 C46 1.401(7) . ?
C46 C47 1.374(6) . ?
C47 H47 0.9500 . ?
C47 C48 1.411(6) . ?
C48 C49 1.424(6) . ?
C48 C50 1.429(6) . ?
C50 H50 0.9500 . ?
C51 C52 1.394(6) . ?
C51 C56 1.403(6) . ?
C52 H52 0.9500 . ?
C52 C53 1.381(7) . ?
C53 H53 0.9500 . ?
C53 C54 1.396(7) . ?
C54 H54 0.9500 . ?
C54 C55 1.383(7) . ?
C55 H55 0.9500 . ?
C55 C56 1.403(6) . ?
Co4 O64 1.906(3) . ?
Co4 O69 1.904(3) . ?
Co4 O111 1.897(3) . ?
Co4 O112 1.891(3) . ?
Co4 N31 1.902(3) . ?
Co4 N35 1.897(3) . ?
O5_b N3_b 1.262(11) . ?
O26 C0AA 1.432(6) . ?
O26 C1AA 1.371(5) . ?
O27 C15 1.416(6) . ?
O27 C16 1.363(6) . ?
O32 N115 1.227(5) . ?
O45 N115 1.231(5) . ?
O64 C21 1.292(5) . ?
O69 C7 1.294(5) . ?
O78_a N206_a 1.256(13) . ?
O78A_b N3_b 1.239(11) . ?
O104_a N206_a 1.256(12) . ?
O111 C28 1.332(5) . ?
O112 C14 1.336(5) . ?
N3_b C18 1.457(9) . ?
N31 C7AA 1.295(6) . ?
N31 C9 1.422(6) . ?
N35 C22 1.285(6) . ?
N35 C23 1.419(6) . ?
N115 C3AA 1.446(6) . ?
N206_a C18 1.519(10) . ?
C0AA H0AA 0.9800 . ?
C0AA H0AB 0.9800 . ?
C0AA H0AC 0.9800 . ?
C1AA C3 1.366(6) . ?
C1AA C7 1.433(6) . ?
C3 H3 0.9500 . ?
C3 C3AA 1.421(7) . ?
C3AA C5AA 1.356(7) . ?
C4AA C5AA 1.403(6) . ?
C4AA C7 1.429(6) . ?
C4AA C7AA 1.430(6) . ?
C5AA H5AA 0.9500 . ?
C7AA H7AA 0.9500 . ?
C9 C10 1.393(6) . ?
C9 C14 1.397(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.384(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.385(8) . ?
C12 H12 0.9500 . ?
C12 C13 1.389(7) . ?
C13 H13 0.9500 . ?
C13 C14 1.400(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.365(7) . ?
C16 C21 1.442(8) . ?
C17 H17 0.9500 . ?
C17 C18 1.406(7) . ?
C18 C19 1.369(8) . ?
C19 H19 0.9500 . ?
C19 C20 1.405(7) . ?
C20 C21 1.417(7) . ?
C20 C22 1.423(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.401(6) . ?
C23 C28 1.414(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.378(7) . ?
C25 H25 0.9500 . ?
C25 C26 1.392(7) . ?
C26 H26 0.9500 . ?
C26 C27 1.383(7) . ?
C27 H27 0.9500 . ?
C27 C28 1.389(7) . ?
O82 H82 0.8400 . ?
O82 C2AA 1.410(10) . ?
C2AA H2AA 0.9800 . ?
C2AA H2AB 0.9802 . ?
C2AA H2AC 0.9800 . ?
O74 H74 0.8400 . ?
O74 C58 1.417(8) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
O12 H12C 0.8400 . ?
O12 C59 1.386(9) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
O14 H14 0.8400 . ?
O14 C121 1.425(8) . ?
C121 H12D 0.9800 . ?
C121 H12E 0.9800 . ?
C121 H12F 0.9800 . ?
N1 H1 1.0000 . ?
N1 C1 1.676(11) . ?
N1 C2 1.534(11) . ?
N1 C8 1.554(12) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C6 1.353(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C4 1.405(12) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5_a H5A_a 0.9800 . ?
C5_a H5B_a 0.9800 . ?
C5_a H5C_a 0.9800 . ?
C5_a C8 1.571(12) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C8 H8A 0.9899 . ?
C8 H8B 0.9900 . ?
N29 H29 1.0000 . ?
N29 C68 1.474(7) . ?
N29 C125 1.541(8) . ?
N29 C162 1.480(7) . ?
C6AA H6AA 0.9800 . ?
C6AA H6AB 0.9800 . ?
C6AA H6AC 0.9800 . ?
C6AA C68 1.527(9) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C125 H12A 0.9900 . ?
C125 H12B 0.9900 . ?
C125 C226 1.494(10) . ?
C162 H16A 0.9900 . ?
C162 H16B 0.9900 . ?
C162 C210 1.534(8) . ?
C210 H21A 0.9800 . ?
C210 H21B 0.9800 . ?
C210 H21C 0.9800 . ?
C226 H22A 0.9800 . ?
C226 H22B 0.9800 . ?
C226 H22C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O49 Co2 N13 95.85(14) . . ?
O49 Co2 N207 88.99(13) . . ?
O65 Co2 O49 89.09(13) . . ?
O65 Co2 N13 89.62(13) . . ?
O65 Co2 N207 95.74(14) . . ?
O102 Co2 O49 90.82(13) . . ?
O102 Co2 O65 178.38(12) . . ?
O102 Co2 O108 90.53(13) . . ?
O102 Co2 N13 88.78(14) . . ?
O102 Co2 N207 85.88(14) . . ?
O108 Co2 O49 177.81(13) . . ?
O108 Co2 O65 89.61(13) . . ?
O108 Co2 N13 85.90(14) . . ?
O108 Co2 N207 89.39(14) . . ?
N13 Co2 N207 172.85(15) . . ?
C44 O19 C43 117.2(4) . . ?
C30 O39 C29 116.8(3) . . ?
C49 O49 Co2 124.6(3) . . ?
C35 O65 Co2 124.6(3) . . ?
C42 O102 Co2 111.4(3) . . ?
C56 O108 Co2 111.7(3) . . ?
C50 N13 Co2 125.8(3) . . ?
C50 N13 C51 122.5(4) . . ?
C51 N13 Co2 111.5(3) . . ?
O4 N79 O33 122.3(4) . . ?
O4 N79 C46 118.7(4) . . ?
O33 N79 C46 119.0(4) . . ?
O8 N98 O48 122.6(4) . . ?
O8 N98 C32 119.0(4) . . ?
O48 N98 C32 118.4(3) . . ?
C36 N207 Co2 125.5(3) . . ?
C36 N207 C37 123.5(4) . . ?
C37 N207 Co2 110.9(3) . . ?
O39 C29 H29A 109.5 . . ?
O39 C29 H29B 109.5 . . ?
O39 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O39 C30 C35 112.8(4) . . ?
C31 C30 O39 125.3(4) . . ?
C31 C30 C35 121.9(4) . . ?
C30 C31 H31 120.7 . . ?
C30 C31 C32 118.6(4) . . ?
C32 C31 H31 120.7 . . ?
C31 C32 N98 118.6(4) . . ?
C33 C32 N98 119.1(4) . . ?
C33 C32 C31 122.3(4) . . ?
C32 C33 H33 120.1 . . ?
C32 C33 C34 119.7(4) . . ?
C34 C33 H33 120.1 . . ?
C33 C34 C35 120.6(4) . . ?
C33 C34 C36 116.3(4) . . ?
C35 C34 C36 123.1(4) . . ?
O65 C35 C30 116.9(3) . . ?
O65 C35 C34 126.2(4) . . ?
C34 C35 C30 116.9(4) . . ?
N207 C36 C34 124.6(4) . . ?
N207 C36 H36 117.7 . . ?
C34 C36 H36 117.7 . . ?
C38 C37 N207 126.4(4) . . ?
C38 C37 C42 121.1(4) . . ?
C42 C37 N207 112.6(4) . . ?
C37 C38 H38 120.2 . . ?
C39 C38 C37 119.6(4) . . ?
C39 C38 H38 120.2 . . ?
C38 C39 H39 120.0 . . ?
C38 C39 C40 119.9(4) . . ?
C40 C39 H39 120.0 . . ?
C39 C40 H40 119.4 . . ?
C41 C40 C39 121.1(4) . . ?
C41 C40 H40 119.4 . . ?
C40 C41 H41 120.1 . . ?
C40 C41 C42 119.9(4) . . ?
C42 C41 H41 120.1 . . ?
O102 C42 C37 119.1(4) . . ?
O102 C42 C41 122.6(4) . . ?
C37 C42 C41 118.3(4) . . ?
O19 C43 H43A 109.5 . . ?
O19 C43 H43B 109.5 . . ?
O19 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O19 C44 C49 113.3(4) . . ?
C45 C44 O19 124.8(4) . . ?
C45 C44 C49 121.9(4) . . ?
C44 C45 H45 120.5 . . ?
C44 C45 C46 119.0(4) . . ?
C46 C45 H45 120.5 . . ?
C45 C46 N79 118.2(4) . . ?
C47 C46 N79 119.5(4) . . ?
C47 C46 C45 122.2(4) . . ?
C46 C47 H47 120.5 . . ?
C46 C47 C48 119.1(4) . . ?
C48 C47 H47 120.5 . . ?
C47 C48 C49 120.6(4) . . ?
C47 C48 C50 115.6(4) . . ?
C49 C48 C50 123.8(4) . . ?
O49 C49 C44 117.3(4) . . ?
O49 C49 C48 125.5(4) . . ?
C48 C49 C44 117.2(4) . . ?
N13 C50 C48 124.1(4) . . ?
N13 C50 H50 118.0 . . ?
C48 C50 H50 118.0 . . ?
C52 C51 N13 126.7(4) . . ?
C52 C51 C56 121.3(4) . . ?
C56 C51 N13 111.9(4) . . ?
C51 C52 H52 120.4 . . ?
C53 C52 C51 119.1(4) . . ?
C53 C52 H52 120.4 . . ?
C52 C53 H53 119.9 . . ?
C52 C53 C54 120.2(4) . . ?
C54 C53 H53 119.9 . . ?
C53 C54 H54 119.6 . . ?
C55 C54 C53 120.9(4) . . ?
C55 C54 H54 119.6 . . ?
C54 C55 H55 120.1 . . ?
C54 C55 C56 119.7(4) . . ?
C56 C55 H55 120.1 . . ?
O108 C56 C51 119.0(4) . . ?
O108 C56 C55 122.4(4) . . ?
C51 C56 C55 118.7(4) . . ?
O69 Co4 O64 90.14(14) . . ?
O111 Co4 O64 178.08(13) . . ?
O111 Co4 O69 88.64(13) . . ?
O111 Co4 N31 91.40(14) . . ?
O112 Co4 O64 90.70(15) . . ?
O112 Co4 O69 178.38(14) . . ?
O112 Co4 O111 90.56(14) . . ?
O112 Co4 N31 85.89(15) . . ?
O112 Co4 N35 89.43(14) . . ?
N31 Co4 O64 87.25(14) . . ?
N31 Co4 O69 95.55(14) . . ?
N35 Co4 O64 95.31(15) . . ?
N35 Co4 O69 89.10(13) . . ?
N35 Co4 O111 86.15(15) . . ?
N35 Co4 N31 174.69(16) . . ?
C1AA O26 C0AA 116.2(3) . . ?
C16 O27 C15 118.2(4) . . ?
C21 O64 Co4 124.5(3) . . ?
C7 O69 Co4 124.6(3) . . ?
C28 O111 Co4 111.5(3) . . ?
C14 O112 Co4 111.6(3) . . ?
O5_b N3_b C18 112.7(7) . . ?
O78A_b N3_b O5_b 121.4(9) . . ?
O78A_b N3_b C18 125.2(8) . . ?
C7AA N31 Co4 125.7(3) . . ?
C7AA N31 C9 123.0(4) . . ?
C9 N31 Co4 111.1(3) . . ?
C22 N35 Co4 125.9(3) . . ?
C22 N35 C23 122.6(4) . . ?
C23 N35 Co4 111.4(3) . . ?
O32 N115 O45 122.4(4) . . ?
O32 N115 C3AA 118.9(4) . . ?
O45 N115 C3AA 118.7(4) . . ?
O78_a N206_a C18 116.6(9) . . ?
O104_a N206_a O78_a 121.0(10) . . ?
O104_a N206_a C18 120.5(8) . . ?
O26 C0AA H0AA 109.5 . . ?
O26 C0AA H0AB 109.5 . . ?
O26 C0AA H0AC 109.5 . . ?
H0AA C0AA H0AB 109.5 . . ?
H0AA C0AA H0AC 109.5 . . ?
H0AB C0AA H0AC 109.5 . . ?
O26 C1AA C7 113.4(4) . . ?
C3 C1AA O26 124.1(4) . . ?
C3 C1AA C7 122.5(4) . . ?
C1AA C3 H3 121.0 . . ?
C1AA C3 C3AA 118.0(4) . . ?
C3AA C3 H3 121.0 . . ?
C3 C3AA N115 118.6(4) . . ?
C5AA C3AA N115 118.9(4) . . ?
C5AA C3AA C3 122.5(4) . . ?
C5AA C4AA C7 120.9(4) . . ?
C5AA C4AA C7AA 115.8(4) . . ?
C7 C4AA C7AA 123.3(4) . . ?
C3AA C5AA C4AA 119.4(4) . . ?
C3AA C5AA H5AA 120.3 . . ?
C4AA C5AA H5AA 120.3 . . ?
O69 C7 C1AA 117.8(4) . . ?
O69 C7 C4AA 125.7(4) . . ?
C4AA C7 C1AA 116.5(4) . . ?
N31 C7AA C4AA 124.1(4) . . ?
N31 C7AA H7AA 118.0 . . ?
C4AA C7AA H7AA 118.0 . . ?
C10 C9 N31 126.1(4) . . ?
C10 C9 C14 121.4(4) . . ?
C14 C9 N31 112.5(4) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 C9 118.8(4) . . ?
C11 C10 H10 120.6 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.4(4) . . ?
C12 C11 H11 119.8 . . ?
C11 C12 H12 119.4 . . ?
C11 C12 C13 121.2(5) . . ?
C13 C12 H12 119.4 . . ?
C12 C13 H13 120.5 . . ?
C12 C13 C14 119.1(5) . . ?
C14 C13 H13 120.5 . . ?
O112 C14 C9 118.6(4) . . ?
O112 C14 C13 122.3(4) . . ?
C9 C14 C13 119.1(4) . . ?
O27 C15 H15A 109.5 . . ?
O27 C15 H15B 109.5 . . ?
O27 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O27 C16 C17 123.7(5) . . ?
O27 C16 C21 113.9(4) . . ?
C17 C16 C21 122.4(5) . . ?
C16 C17 H17 121.1 . . ?
C16 C17 C18 117.7(5) . . ?
C18 C17 H17 121.1 . . ?
C17 C18 N3_b 121.5(5) . . ?
C17 C18 N206_a 112.3(6) . . ?
C19 C18 N3_b 112.6(5) . . ?
C19 C18 N206_a 121.7(5) . . ?
C19 C18 C17 122.5(5) . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.2(5) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 C21 119.5(5) . . ?
C19 C20 C22 116.5(4) . . ?
C21 C20 C22 123.9(4) . . ?
O64 C21 C16 117.3(4) . . ?
O64 C21 C20 125.2(5) . . ?
C20 C21 C16 117.5(4) . . ?
N35 C22 C20 124.3(4) . . ?
N35 C22 H22 117.9 . . ?
C20 C22 H22 117.9 . . ?
C24 C23 N35 126.4(4) . . ?
C24 C23 C28 121.2(4) . . ?
C28 C23 N35 112.4(4) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 C23 118.6(5) . . ?
C25 C24 H24 120.7 . . ?
C24 C25 H25 119.7 . . ?
C24 C25 C26 120.6(4) . . ?
C26 C25 H25 119.7 . . ?
C25 C26 H26 119.5 . . ?
C27 C26 C25 121.0(5) . . ?
C27 C26 H26 119.5 . . ?
C26 C27 H27 120.0 . . ?
C26 C27 C28 119.9(5) . . ?
C28 C27 H27 120.0 . . ?
O111 C28 C23 118.4(4) . . ?
O111 C28 C27 122.9(4) . . ?
C27 C28 C23 118.6(4) . . ?
C2AA O82 H82 109.5 . . ?
O82 C2AA H2AA 109.5 . . ?
O82 C2AA H2AB 109.4 . . ?
O82 C2AA H2AC 109.4 . . ?
H2AA C2AA H2AB 109.5 . . ?
H2AA C2AA H2AC 109.5 . . ?
H2AB C2AA H2AC 109.5 . . ?
C58 O74 H74 109.5 . . ?
O74 C58 H58A 109.5 . . ?
O74 C58 H58B 109.5 . . ?
O74 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C59 O12 H12C 109.5 . . ?
O12 C59 H59A 109.5 . . ?
O12 C59 H59B 109.5 . . ?
O12 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C121 O14 H14 109.5 . . ?
O14 C121 H12D 109.5 . . ?
O14 C121 H12E 109.5 . . ?
O14 C121 H12F 109.5 . . ?
H12D C121 H12E 109.5 . . ?
H12D C121 H12F 109.5 . . ?
H12E C121 H12F 109.5 . . ?
C1 N1 H1 100.3 . . ?
C2 N1 H1 100.3 . . ?
C2 N1 C1 114.3(7) . . ?
C2 N1 C8 100.7(8) . . ?
C8 N1 H1 100.3 . . ?
C8 N1 C1 134.8(8) . . ?
N1 C1 H1A 110.3 . . ?
N1 C1 H1B 110.3 . . ?
H1A C1 H1B 108.5 . . ?
C6 C1 N1 107.2(10) . . ?
C6 C1 H1A 110.3 . . ?
C6 C1 H1B 110.3 . . ?
N1 C2 H2A 100.9 . . ?
N1 C2 H2B 100.9 . . ?
H2A C2 H2B 104.4 . . ?
C4 C2 N1 144.1(9) . . ?
C4 C2 H2A 100.9 . . ?
C4 C2 H2B 100.9 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
H5A_a C5_a H5B_a 109.5 . . ?
H5A_a C5_a H5C_a 109.5 . . ?
H5B_a C5_a H5C_a 109.5 . . ?
C8 C5_a H5A_a 109.5 . . ?
C8 C5_a H5B_a 109.5 . . ?
C8 C5_a H5C_a 109.5 . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C8 C5_a 125.2(10) . . ?
N1 C8 H8A 105.3 . . ?
N1 C8 H8B 107.9 . . ?
C5_a C8 H8A 103.5 . . ?
C5_a C8 H8B 107.6 . . ?
H8A C8 H8B 105.8 . . ?
C68 N29 H29 106.3 . . ?
C68 N29 C125 113.5(5) . . ?
C68 N29 C162 114.7(5) . . ?
C125 N29 H29 106.3 . . ?
C162 N29 H29 106.3 . . ?
C162 N29 C125 109.2(5) . . ?
H6AA C6AA H6AB 109.5 . . ?
H6AA C6AA H6AC 109.5 . . ?
H6AB C6AA H6AC 109.5 . . ?
C68 C6AA H6AA 109.5 . . ?
C68 C6AA H6AB 109.5 . . ?
C68 C6AA H6AC 109.5 . . ?
N29 C68 C6AA 112.1(5) . . ?
N29 C68 H68A 109.2 . . ?
N29 C68 H68B 109.2 . . ?
C6AA C68 H68A 109.2 . . ?
C6AA C68 H68B 109.2 . . ?
H68A C68 H68B 107.9 . . ?
N29 C125 H12A 108.8 . . ?
N29 C125 H12B 108.8 . . ?
H12A C125 H12B 107.7 . . ?
C226 C125 N29 114.0(6) . . ?
C226 C125 H12A 108.8 . . ?
C226 C125 H12B 108.8 . . ?
N29 C162 H16A 109.0 . . ?
N29 C162 H16B 109.0 . . ?
N29 C162 C210 112.7(5) . . ?
H16A C162 H16B 107.8 . . ?
C210 C162 H16A 109.0 . . ?
C210 C162 H16B 109.0 . . ?
C162 C210 H21A 109.5 . . ?
C162 C210 H21B 109.5 . . ?
C162 C210 H21C 109.5 . . ?
H21A C210 H21B 109.5 . . ?
H21A C210 H21C 109.5 . . ?
H21B C210 H21C 109.5 . . ?
C125 C226 H22A 109.5 . . ?
C125 C226 H22B 109.5 . . ?
C125 C226 H22C 109.5 . . ?
H22A C226 H22B 109.5 . . ?
H22A C226 H22C 109.5 . . ?
H22B C226 H22C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co2 O49 C49 C44 -179.6(3) . . . . ?
Co2 O49 C49 C48 0.9(6) . . . . ?
Co2 O65 C35 C30 -175.6(3) . . . . ?
Co2 O65 C35 C34 5.0(6) . . . . ?
Co2 O102 C42 C37 -3.6(5) . . . . ?
Co2 O102 C42 C41 175.5(3) . . . . ?
Co2 O108 C56 C51 0.3(5) . . . . ?
Co2 O108 C56 C55 180.0(4) . . . . ?
Co2 N13 C50 C48 -2.2(6) . . . . ?
Co2 N13 C51 C52 -178.6(4) . . . . ?
Co2 N13 C51 C56 1.0(4) . . . . ?
Co2 N207 C36 C34 1.7(6) . . . . ?
Co2 N207 C37 C38 -178.2(4) . . . . ?
Co2 N207 C37 C42 1.4(4) . . . . ?
O4 N79 C46 C45 173.9(5) . . . . ?
O4 N79 C46 C47 -9.3(7) . . . . ?
O8 N98 C32 C31 179.3(4) . . . . ?
O8 N98 C32 C33 -1.6(6) . . . . ?
O19 C44 C45 C46 -177.8(4) . . . . ?
O19 C44 C49 O49 -2.7(6) . . . . ?
O19 C44 C49 C48 176.8(4) . . . . ?
O33 N79 C46 C45 -5.6(7) . . . . ?
O33 N79 C46 C47 171.2(5) . . . . ?
O39 C30 C31 C32 -178.8(4) . . . . ?
O39 C30 C35 O65 -1.1(5) . . . . ?
O39 C30 C35 C34 178.4(4) . . . . ?
O48 N98 C32 C31 0.8(6) . . . . ?
O48 N98 C32 C33 179.9(4) . . . . ?
O49 Co2 O65 C35 -93.3(3) . . . . ?
O49 Co2 O102 C42 92.3(3) . . . . ?
O65 Co2 O49 C49 -93.7(3) . . . . ?
O65 Co2 O108 C56 89.9(3) . . . . ?
O102 Co2 O49 C49 84.7(3) . . . . ?
O102 Co2 O108 C56 -88.5(3) . . . . ?
O108 Co2 O65 C35 85.0(3) . . . . ?
O108 Co2 O102 C42 -85.9(3) . . . . ?
N13 Co2 O49 C49 -4.2(3) . . . . ?
N13 Co2 O65 C35 170.9(3) . . . . ?
N13 Co2 O102 C42 -171.8(3) . . . . ?
N13 Co2 O108 C56 0.2(3) . . . . ?
N13 C51 C52 C53 -179.9(4) . . . . ?
N13 C51 C56 O108 -0.9(6) . . . . ?
N13 C51 C56 C55 179.4(4) . . . . ?
N79 C46 C47 C48 -178.4(4) . . . . ?
N98 C32 C33 C34 179.4(4) . . . . ?
N207 Co2 O49 C49 170.6(3) . . . . ?
N207 Co2 O65 C35 -4.4(3) . . . . ?
N207 Co2 O102 C42 3.4(3) . . . . ?
N207 Co2 O108 C56 -174.4(3) . . . . ?
N207 C37 C38 C39 178.7(4) . . . . ?
N207 C37 C42 O102 1.5(6) . . . . ?
N207 C37 C42 C41 -177.7(4) . . . . ?
C29 O39 C30 C31 4.3(7) . . . . ?
C29 O39 C30 C35 -176.3(4) . . . . ?
C30 C31 C32 N98 179.1(4) . . . . ?
C30 C31 C32 C33 0.0(6) . . . . ?
C31 C30 C35 O65 178.3(4) . . . . ?
C31 C30 C35 C34 -2.2(6) . . . . ?
C31 C32 C33 C34 -1.5(6) . . . . ?
C32 C33 C34 C35 1.1(6) . . . . ?
C32 C33 C34 C36 -177.5(4) . . . . ?
C33 C34 C35 O65 -179.9(4) . . . . ?
C33 C34 C35 C30 0.7(6) . . . . ?
C33 C34 C36 N207 176.3(4) . . . . ?
C35 C30 C31 C32 1.9(6) . . . . ?
C35 C34 C36 N207 -2.3(7) . . . . ?
C36 N207 C37 C38 -1.7(7) . . . . ?
C36 N207 C37 C42 177.8(4) . . . . ?
C36 C34 C35 O65 -1.4(7) . . . . ?
C36 C34 C35 C30 179.2(4) . . . . ?
C37 N207 C36 C34 -174.2(4) . . . . ?
C37 C38 C39 C40 -0.6(7) . . . . ?
C38 C37 C42 O102 -178.9(4) . . . . ?
C38 C37 C42 C41 1.9(7) . . . . ?
C38 C39 C40 C41 1.1(8) . . . . ?
C39 C40 C41 C42 0.0(8) . . . . ?
C40 C41 C42 O102 179.4(4) . . . . ?
C40 C41 C42 C37 -1.5(7) . . . . ?
C42 C37 C38 C39 -0.9(7) . . . . ?
C43 O19 C44 C45 -5.0(7) . . . . ?
C43 O19 C44 C49 176.7(4) . . . . ?
C44 C45 C46 N79 178.1(5) . . . . ?
C44 C45 C46 C47 1.4(7) . . . . ?
C45 C44 C49 O49 178.9(4) . . . . ?
C45 C44 C49 C48 -1.6(6) . . . . ?
C45 C46 C47 C48 -1.7(7) . . . . ?
C46 C47 C48 C49 0.3(7) . . . . ?
C46 C47 C48 C50 177.8(4) . . . . ?
C47 C48 C49 O49 -179.3(4) . . . . ?
C47 C48 C49 C44 1.3(6) . . . . ?
C47 C48 C50 N13 179.9(4) . . . . ?
C49 C44 C45 C46 0.3(7) . . . . ?
C49 C48 C50 N13 -2.8(7) . . . . ?
C50 N13 C51 C52 -2.7(7) . . . . ?
C50 N13 C51 C56 177.0(4) . . . . ?
C50 C48 C49 O49 3.5(7) . . . . ?
C50 C48 C49 C44 -176.0(4) . . . . ?
C51 N13 C50 C48 -177.5(4) . . . . ?
C51 C52 C53 C54 0.0(7) . . . . ?
C52 C51 C56 O108 178.8(4) . . . . ?
C52 C51 C56 C55 -0.9(7) . . . . ?
C52 C53 C54 C55 0.0(7) . . . . ?
C53 C54 C55 C56 -0.4(7) . . . . ?
C54 C55 C56 O108 -178.8(4) . . . . ?
C54 C55 C56 C51 0.8(7) . . . . ?
C56 C51 C52 C53 0.5(7) . . . . ?
Co4 O64 C21 C16 173.0(4) . . . . ?
Co4 O64 C21 C20 -8.2(8) . . . . ?
Co4 O69 C7 C1AA 173.0(3) . . . . ?
Co4 O69 C7 C4AA -5.8(6) . . . . ?
Co4 O111 C28 C23 -3.6(5) . . . . ?
Co4 O111 C28 C27 176.5(3) . . . . ?
Co4 O112 C14 C9 5.1(5) . . . . ?
Co4 O112 C14 C13 -175.9(4) . . . . ?
Co4 N31 C7AA C4AA -11.6(6) . . . . ?
Co4 N31 C9 C10 177.1(4) . . . . ?
Co4 N31 C9 C14 -2.6(5) . . . . ?
Co4 N35 C22 C20 -1.0(7) . . . . ?
Co4 N35 C23 C24 -179.1(4) . . . . ?
Co4 N35 C23 C28 1.0(4) . . . . ?
O5_b N3_b C18 N206_a 64.8(9) . . . . ?
O5_b N3_b C18 C17 -22.7(11) . . . . ?
O5_b N3_b C18 C19 177.9(7) . . . . ?
O26 C1AA C3 C3AA -178.9(4) . . . . ?
O26 C1AA C7 O69 -3.3(6) . . . . ?
O26 C1AA C7 C4AA 175.5(4) . . . . ?
O27 C16 C17 C18 174.8(5) . . . . ?
O27 C16 C21 O64 3.5(8) . . . . ?
O27 C16 C21 C20 -175.4(5) . . . . ?
O32 N115 C3AA C3 2.3(7) . . . . ?
O32 N115 C3AA C5AA -177.8(5) . . . . ?
O45 N115 C3AA C3 -178.6(5) . . . . ?
O45 N115 C3AA C5AA 1.2(7) . . . . ?
O64 Co4 O112 C14 -92.3(3) . . . . ?
O64 Co4 N35 C22 -5.9(4) . . . . ?
O64 Co4 N35 C23 176.4(3) . . . . ?
O69 Co4 O111 C28 -86.0(3) . . . . ?
O69 Co4 N35 C22 -96.0(4) . . . . ?
O69 Co4 N35 C23 86.4(3) . . . . ?
O78_a N206_a C18 N3_b 77.9(11) . . . . ?
O78_a N206_a C18 C17 -169.2(8) . . . . ?
O78_a N206_a C18 C19 -9.6(12) . . . . ?
O78A_b N3_b C18 N206_a -105.9(12) . . . . ?
O78A_b N3_b C18 C17 166.6(8) . . . . ?
O78A_b N3_b C18 C19 7.2(12) . . . . ?
O104_a N206_a C18 N3_b -86.3(11) . . . . ?
O104_a N206_a C18 C17 26.6(12) . . . . ?
O104_a N206_a C18 C19 -173.9(8) . . . . ?
O111 Co4 O112 C14 86.2(3) . . . . ?
O111 Co4 N35 C22 175.3(4) . . . . ?
O111 Co4 N35 C23 -2.3(3) . . . . ?
O112 Co4 O111 C28 92.6(3) . . . . ?
O112 Co4 N35 C22 84.7(4) . . . . ?
O112 Co4 N35 C23 -92.9(3) . . . . ?
N3_b C18 C19 C20 161.7(6) . . . . ?
N31 Co4 O111 C28 178.5(3) . . . . ?
N31 Co4 O112 C14 -5.1(3) . . . . ?
N31 C9 C10 C11 -179.4(4) . . . . ?
N31 C9 C14 O112 -1.6(6) . . . . ?
N31 C9 C14 C13 179.4(4) . . . . ?
N35 Co4 O111 C28 3.2(3) . . . . ?
N35 Co4 O112 C14 172.4(3) . . . . ?
N35 C23 C24 C25 178.7(4) . . . . ?
N35 C23 C28 O111 1.7(6) . . . . ?
N35 C23 C28 C27 -178.4(4) . . . . ?
N115 C3AA C5AA C4AA 179.4(4) . . . . ?
N206_a C18 C19 C20 -154.9(7) . . . . ?
C0AA O26 C1AA C3 17.5(7) . . . . ?
C0AA O26 C1AA C7 -163.3(4) . . . . ?
C1AA C3 C3AA N115 -178.9(4) . . . . ?
C1AA C3 C3AA C5AA 1.3(7) . . . . ?
C3 C1AA C7 O69 175.9(4) . . . . ?
C3 C1AA C7 C4AA -5.2(6) . . . . ?
C3 C3AA C5AA C4AA -0.8(7) . . . . ?
C5AA C4AA C7 O69 -175.6(4) . . . . ?
C5AA C4AA C7 C1AA 5.6(6) . . . . ?
C5AA C4AA C7AA N31 -175.1(4) . . . . ?
C7 C1AA C3 C3AA 1.9(7) . . . . ?
C7 C4AA C5AA C3AA -2.8(7) . . . . ?
C7 C4AA C7AA N31 2.5(7) . . . . ?
C7AA N31 C9 C10 -7.8(7) . . . . ?
C7AA N31 C9 C14 172.4(4) . . . . ?
C7AA C4AA C5AA C3AA 174.9(4) . . . . ?
C7AA C4AA C7 O69 6.9(7) . . . . ?
C7AA C4AA C7 C1AA -171.9(4) . . . . ?
C9 N31 C7AA C4AA 174.1(4) . . . . ?
C9 C10 C11 C12 0.2(7) . . . . ?
C10 C9 C14 O112 178.6(4) . . . . ?
C10 C9 C14 C13 -0.4(7) . . . . ?
C10 C11 C12 C13 -0.7(8) . . . . ?
C11 C12 C13 C14 0.5(8) . . . . ?
C12 C13 C14 O112 -179.0(5) . . . . ?
C12 C13 C14 C9 0.0(7) . . . . ?
C14 C9 C10 C11 0.3(7) . . . . ?
C15 O27 C16 C17 3.4(9) . . . . ?
C15 O27 C16 C21 -177.5(5) . . . . ?
C16 C17 C18 N3_b -156.3(7) . . . . ?
C16 C17 C18 N206_a 160.5(6) . . . . ?
C16 C17 C18 C19 1.1(9) . . . . ?
C17 C16 C21 O64 -177.4(6) . . . . ?
C17 C16 C21 C20 3.8(9) . . . . ?
C17 C18 C19 C20 2.5(10) . . . . ?
C18 C19 C20 C21 -3.0(9) . . . . ?
C18 C19 C20 C22 179.6(5) . . . . ?
C19 C20 C21 O64 -178.8(6) . . . . ?
C19 C20 C21 C16 0.0(9) . . . . ?
C19 C20 C22 N35 -176.1(5) . . . . ?
C21 C16 C17 C18 -4.3(9) . . . . ?
C21 C20 C22 N35 6.6(9) . . . . ?
C22 N35 C23 C24 3.2(7) . . . . ?
C22 N35 C23 C28 -176.7(4) . . . . ?
C22 C20 C21 O64 -1.6(10) . . . . ?
C22 C20 C21 C16 177.2(5) . . . . ?
C23 N35 C22 C20 176.3(5) . . . . ?
C23 C24 C25 C26 0.3(7) . . . . ?
C24 C23 C28 O111 -178.2(4) . . . . ?
C24 C23 C28 C27 1.7(6) . . . . ?
C24 C25 C26 C27 0.4(7) . . . . ?
C25 C26 C27 C28 0.0(7) . . . . ?
C26 C27 C28 O111 178.9(4) . . . . ?
C26 C27 C28 C23 -1.0(7) . . . . ?
C28 C23 C24 C25 -1.4(7) . . . . ?
C1 N1 C2 C4 137(2) . . . . ?
C1 N1 C8 C5_a 160.8(11) . . . . ?
C2 N1 C1 C6 138.8(10) . . . . ?
C2 N1 C8 C5_a -57.9(15) . . . . ?
C8 N1 C1 C6 -83.6(14) . . . . ?
C8 N1 C2 C4 -13(2) . . . . ?
C68 N29 C125 C226 -60.4(8) . . . . ?
C68 N29 C162 C210 -63.3(7) . . . . ?
C125 N29 C68 C6AA -57.8(7) . . . . ?
C125 N29 C162 C210 168.1(5) . . . . ?
C162 N29 C68 C6AA 175.8(6) . . . . ?
C162 N29 C125 C226 68.9(8) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.251 0.837 0.770 126.7 11.5 ?
2 0.251 0.663 0.270 126.7 11.5 ?
3 0.199 0.651 0.017 9.9 0.5 ?
4 0.199 0.849 0.517 9.9 0.4 ?
5 0.749 0.163 0.230 126.7 11.5 ?
6 0.749 0.337 0.730 126.7 11.5 ?
7 0.801 0.151 0.483 9.9 0.4 ?
8 0.801 0.349 0.983 9.9 0.4 ?

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

data_5_CCDC_1406221
_database_code_depnum_ccdc_archive 'CCDC 1406221'
_audit_update_record             
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_audit_creation_date             2015-11-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C36 H24 Br2 Co N2 O6, C6 H16 N, 3(C H4 O)'
_chemical_formula_sum            'C45 H52 Br2 Co N3 O9'
_chemical_formula_weight         997.64
_chemical_melting_point          ?
_chemical_oxdiff_formula         Co4C80H88N8O32
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.0590(8)
_cell_length_b                   22.7258(11)
_cell_length_c                   15.4472(13)
_cell_angle_alpha                90
_cell_angle_beta                 109.616(8)
_cell_angle_gamma                90
_cell_volume                     4318.3(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3201
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.8380
_cell_measurement_theta_min      2.8660
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.307
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13404
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.440
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -87.00    3.00   1.0000  150.4700
omega____ theta____ kappa____ phi______ frames
    -      -18.0128  -57.0000   30.0000 90

#__ type_ start__ end____ width___ exp.time_
  2 omega  -44.00   31.00   1.0000  150.4700
omega____ theta____ kappa____ phi______ frames
    -      -18.0128   77.0000  150.0000 75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0287118000
_diffrn_orient_matrix_UB_12      0.0166250000
_diffrn_orient_matrix_UB_13      -0.0395587000
_diffrn_orient_matrix_UB_21      -0.0254367000
_diffrn_orient_matrix_UB_22      -0.0260680000
_diffrn_orient_matrix_UB_23      -0.0223367000
_diffrn_orient_matrix_UB_31      -0.0430939000
_diffrn_orient_matrix_UB_32      0.0043186000
_diffrn_orient_matrix_UB_33      0.0176033000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5589
_reflns_number_total             8410
_reflns_odcompleteness_completeness 95.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         8410
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0590
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0486P)²+4.6912P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1182
_refine_ls_wR_factor_ref         0.1402
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H45A,H45B,H45C} of C45, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, {H1A,H1B,H1C} of C1, {H19A,H19B,H19C} of C19, {H40A,H40B,
  H40C} of C40, {H38A,H38B,H38C} of C38, {H44A,H44B,H44C} of C44, {H43A,H43B,
  H43C} of C43, {H42A,H42B,H42C} of C42
2.a Riding coordinates:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C38(H38A,H38B,H38C), C40(H40A,H40B,
 H40C), C42(H42A,H42B,H42C), O9(H9), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C)
2.b Ternary CH refined with riding coordinates:
 N3(H3A)
2.c Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B)
2.d Me refined with riding coordinates:
 C44(H44A,H44B,H44C)
2.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15),
 C17(H17), C21(H21), C23(H23), C26(H26), C28(H28), C30(H30), C31(H31), C32(H32),
  C33(H33), C35(H35)
2.f Idealised tetrahedral OH refined as rotating group:
 O7(H7), O8(H8A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.59129(4) 0.72058(2) 1.19700(4) 0.04473(17) Uani 1 1 d . . . . .
Br2 Br 0.04016(5) 0.22905(3) 1.07193(5) 0.05398(19) Uani 1 1 d . . . . .
Co10 Co 0.21244(5) 0.50267(3) 0.91398(4) 0.02599(17) Uani 1 1 d . . . . .
O1 O 0.2184(2) 0.61425(15) 1.1523(2) 0.0376(9) Uani 1 1 d . . . . .
O2 O 0.2300(2) 0.55015(14) 1.0181(2) 0.0302(8) Uani 1 1 d . . . . .
O3 O 0.1890(2) 0.45195(14) 0.8118(2) 0.0351(8) Uani 1 1 d . . . . .
O4 O 0.3858(2) 0.35129(15) 1.0797(3) 0.0406(9) Uani 1 1 d . . . . .
O5 O 0.2735(2) 0.43877(13) 0.9918(2) 0.0332(8) Uani 1 1 d . . . . .
O6 O 0.1580(2) 0.56841(13) 0.8372(2) 0.0301(8) Uani 1 1 d . . . . .
N1 N 0.3507(3) 0.51880(16) 0.9033(3) 0.0280(9) Uani 1 1 d . . . . .
N2 N 0.0665(3) 0.48879(16) 0.9060(2) 0.0251(8) Uani 1 1 d . . . . .
C1 C 0.2067(4) 0.6515(3) 1.2221(4) 0.0493(15) Uani 1 1 d . . . . .
H1A H 0.2083 0.6927 1.2039 0.074 Uiso 1 1 d R . . . .
H1B H 0.2664 0.6443 1.2796 0.074 Uiso 1 1 d R . . . .
H1C H 0.1372 0.6432 1.2308 0.074 Uiso 1 1 d R . . . .
C2 C 0.3102(4) 0.6209(2) 1.1287(3) 0.0302(11) Uani 1 1 d . . . . .
C3 C 0.3919(4) 0.6604(2) 1.1703(4) 0.0341(12) Uani 1 1 d . . . . .
H3 H 0.3874 0.6849 1.2187 0.041 Uiso 1 1 calc R . . . .
C4 C 0.4817(4) 0.6640(2) 1.1402(4) 0.0342(12) Uani 1 1 d . . . . .
C5 C 0.4910(4) 0.6290(2) 1.0726(3) 0.0314(11) Uani 1 1 d . . . . .
H5 H 0.5538 0.6315 1.0548 0.038 Uiso 1 1 calc R . . . .
C6 C 0.4068(3) 0.5885(2) 1.0278(3) 0.0277(11) Uani 1 1 d . . . . .
C7 C 0.3136(3) 0.5841(2) 1.0544(3) 0.0272(11) Uani 1 1 d . . . . .
C8 C 0.4210(4) 0.5552(2) 0.9537(3) 0.0308(11) Uani 1 1 d . . . . .
H8 H 0.4867 0.5604 0.9411 0.037 Uiso 1 1 calc R . . . .
C9 C 0.3625(4) 0.48988(19) 0.8257(3) 0.0295(11) Uani 1 1 d . . . . .
C10 C 0.4468(4) 0.4958(2) 0.7921(3) 0.0343(12) Uani 1 1 d . . . . .
H10 H 0.5070 0.5201 0.8232 0.041 Uiso 1 1 calc R . . . .
C11 C 0.4444(4) 0.4656(2) 0.7109(4) 0.0383(13) Uani 1 1 d . . . . .
C12 C 0.5257(5) 0.4731(3) 0.6703(4) 0.0545(16) Uani 1 1 d . . . . .
H12 H 0.5862 0.4980 0.6988 0.065 Uiso 1 1 calc R . . . .
C13 C 0.5176(5) 0.4446(2) 0.5900(4) 0.0503(15) Uani 1 1 d . . . . .
H13 H 0.5718 0.4509 0.5626 0.060 Uiso 1 1 calc R . . . .
C14 C 0.4328(5) 0.4074(3) 0.5484(4) 0.0497(15) Uani 1 1 d . . . . .
H14 H 0.4285 0.3887 0.4923 0.060 Uiso 1 1 calc R . . . .
C15 C 0.3555(5) 0.3971(2) 0.5865(4) 0.0488(15) Uani 1 1 d . . . . .
H15 H 0.2992 0.3697 0.5584 0.059 Uiso 1 1 calc R . . . .
C16 C 0.3569(4) 0.4265(2) 0.6679(4) 0.0385(13) Uani 1 1 d . . . . .
C17 C 0.2727(4) 0.4203(2) 0.7049(4) 0.0406(13) Uani 1 1 d . . . . .
H17 H 0.2151 0.3935 0.6774 0.049 Uiso 1 1 calc R . . . .
C18 C 0.2724(4) 0.4525(2) 0.7807(3) 0.0323(11) Uani 1 1 d . . . . .
C19 C 0.4494(4) 0.3021(2) 1.1224(5) 0.0551(17) Uani 1 1 d . . . . .
H19A H 0.4303 0.2682 1.0808 0.083 Uiso 1 1 d R . . . .
H19B H 0.4353 0.2927 1.1793 0.083 Uiso 1 1 d R . . . .
H19C H 0.5266 0.3114 1.1367 0.083 Uiso 1 1 d R . . . .
C20 C 0.2748(4) 0.3449(2) 1.0531(4) 0.0329(11) Uani 1 1 d . . . . .
C21 C 0.2232(4) 0.2969(2) 1.0722(4) 0.0364(12) Uani 1 1 d . . . . .
H21 H 0.2637 0.2639 1.1033 0.044 Uiso 1 1 calc R . . . .
C22 C 0.1098(4) 0.2971(2) 1.0452(4) 0.0362(12) Uani 1 1 d . . . . .
C23 C 0.0493(4) 0.3436(2) 1.0016(3) 0.0335(12) Uani 1 1 d . . . . .
H23 H -0.0276 0.3427 0.9854 0.040 Uiso 1 1 calc R . . . .
C24 C 0.1011(4) 0.3934(2) 0.9804(3) 0.0278(11) Uani 1 1 d . . . . .
C25 C 0.2164(4) 0.3952(2) 1.0057(3) 0.0302(11) Uani 1 1 d . . . . .
C26 C 0.0329(3) 0.4407(2) 0.9345(3) 0.0279(11) Uani 1 1 d . . . . .
H26 H -0.0428 0.4370 0.9238 0.034 Uiso 1 1 calc R . . . .
C27 C -0.0046(3) 0.53321(19) 0.8544(3) 0.0269(11) Uani 1 1 d . . . . .
C28 C -0.1132(4) 0.5376(2) 0.8391(3) 0.0319(11) Uani 1 1 d . . . . .
H28 H -0.1484 0.5096 0.8650 0.038 Uiso 1 1 calc R . . . .
C29 C -0.1730(4) 0.5837(2) 0.7848(3) 0.0325(12) Uani 1 1 d . . . . .
C30 C -0.2867(4) 0.5897(3) 0.7655(4) 0.0426(14) Uani 1 1 d . . . . .
H30 H -0.3234 0.5630 0.7924 0.051 Uiso 1 1 calc R . . . .
C31 C -0.3439(5) 0.6332(3) 0.7088(4) 0.0519(16) Uani 1 1 d . . . . .
H31 H -0.4202 0.6361 0.6955 0.062 Uiso 1 1 calc R . . . .
C32 C -0.2916(4) 0.6727(3) 0.6709(4) 0.0536(17) Uani 1 1 d . . . . .
H32 H -0.3329 0.7024 0.6309 0.064 Uiso 1 1 calc R . . . .
C33 C -0.1823(4) 0.6706(2) 0.6893(4) 0.0465(14) Uani 1 1 d . . . . .
H33 H -0.1478 0.6993 0.6638 0.056 Uiso 1 1 calc R . . . .
C34 C -0.1199(4) 0.6256(2) 0.7463(4) 0.0361(12) Uani 1 1 d . . . . .
C35 C -0.0063(4) 0.6211(2) 0.7666(4) 0.0361(12) Uani 1 1 d . . . . .
H35 H 0.0306 0.6498 0.7432 0.043 Uiso 1 1 calc R . . . .
C36 C 0.0514(3) 0.5758(2) 0.8196(3) 0.0285(11) Uani 1 1 d . . . . .
N3 N 0.2048(4) 0.5810(2) 0.5419(3) 0.0562(13) Uani 1 1 d . . . . .
H3A H 0.1404 0.6037 0.5023 0.067 Uiso 1 1 calc R . . . .
C37 C 0.3063(6) 0.6199(3) 0.5614(6) 0.078(2) Uani 1 1 d . . . . .
H37A H 0.3695 0.5989 0.6042 0.093 Uiso 1 1 calc R . . . .
H37B H 0.3211 0.6264 0.5033 0.093 Uiso 1 1 calc R . . . .
C38 C 0.2946(7) 0.6775(3) 0.6015(6) 0.089(3) Uani 1 1 d . . . . .
H38A H 0.2250 0.6953 0.5655 0.133 Uiso 1 1 d R . . . .
H38B H 0.3542 0.7034 0.6005 0.133 Uiso 1 1 d R . . . .
H38C H 0.2970 0.6719 0.6650 0.133 Uiso 1 1 d R . . . .
C39 C 0.1868(5) 0.5658(3) 0.6297(4) 0.0616(17) Uani 1 1 d . . . . .
H39A H 0.1853 0.6025 0.6638 0.074 Uiso 1 1 calc R . . . .
H39B H 0.2486 0.5417 0.6679 0.074 Uiso 1 1 calc R . . . .
C40 C 0.0789(5) 0.5312(3) 0.6147(4) 0.0625(18) Uani 1 1 d . . . . .
H40A H 0.0180 0.5528 0.5717 0.094 Uiso 1 1 d R . . . .
H40B H 0.0668 0.5269 0.6736 0.094 Uiso 1 1 d R . . . .
H40C H 0.0841 0.4922 0.5894 0.094 Uiso 1 1 d R . . . .
C41 C 0.2195(6) 0.5266(3) 0.4886(5) 0.0657(19) Uani 1 1 d . . . . .
H41A H 0.2966 0.5141 0.5127 0.079 Uiso 1 1 calc R . . . .
H41B H 0.1750 0.4940 0.4996 0.079 Uiso 1 1 calc R . . . .
C42 C 0.1887(6) 0.5365(3) 0.3890(5) 0.083(2) Uani 1 1 d . . . . .
H42A H 0.1893 0.4990 0.3578 0.124 Uiso 1 1 d R . . . .
H42B H 0.2408 0.5636 0.3769 0.124 Uiso 1 1 d R . . . .
H42C H 0.1157 0.5537 0.3658 0.124 Uiso 1 1 d R . . . .
O9 O -0.0284(4) 0.3570(2) 0.5588(3) 0.0864(16) Uani 1 1 d . . . . .
H9 H -0.0166 0.3544 0.6279 0.130 Uiso 1 1 d R . . . .
C44 C 0.0403(6) 0.3319(3) 0.5169(5) 0.078(2) Uani 1 1 d . . . . .
H44A H 0.0062 0.3343 0.4500 0.117 Uiso 1 1 calc R . . . .
H44B H 0.0535 0.2906 0.5355 0.117 Uiso 1 1 calc R . . . .
H44C H 0.1095 0.3533 0.5358 0.117 Uiso 1 1 calc R . . . .
O7 O 0.2623(3) 0.6728(2) 0.8284(3) 0.0624(12) Uani 1 1 d . . . . .
H7 H 0.2279 0.6410 0.8232 0.094 Uiso 1 1 calc GR . . . .
C43 C 0.2488(6) 0.7061(3) 0.9007(5) 0.071(2) Uani 1 1 d . . . . .
H43A H 0.2509 0.7481 0.8869 0.107 Uiso 1 1 d R . . . .
H43B H 0.3074 0.6970 0.9582 0.107 Uiso 1 1 d R . . . .
H43C H 0.1785 0.6966 0.9073 0.107 Uiso 1 1 d R . . . .
O8 O 0.0493(3) 0.36494(16) 0.7401(3) 0.0451(9) Uani 1 1 d . . . . .
H8A H 0.0881 0.3944 0.7624 0.068 Uiso 1 1 calc GR . . . .
C45 C 0.1013(5) 0.3132(2) 0.7856(4) 0.0553(16) Uani 1 1 d . . . . .
H45A H 0.1755 0.3114 0.7836 0.066 Uiso 1 1 d R . . . .
H45B H 0.0606 0.2785 0.7550 0.066 Uiso 1 1 d R . . . .
H45C H 0.1039 0.3141 0.8497 0.066 Uiso 1 1 d R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C4 1.905(5) . ?
Br2 C22 1.908(5) . ?
Co10 O2 1.886(3) . ?
Co10 O3 1.895(3) . ?
Co10 O5 1.883(3) . ?
Co10 O6 1.891(3) . ?
Co10 N1 1.903(4) . ?
Co10 N2 1.895(4) . ?
O1 C1 1.418(6) . ?
O1 C2 1.373(5) . ?
O2 C7 1.300(5) . ?
O3 C18 1.328(5) . ?
O4 C19 1.417(6) . ?
O4 C20 1.376(5) . ?
O5 C25 1.300(5) . ?
O6 C36 1.337(5) . ?
N1 C8 1.285(6) . ?
N1 C9 1.421(6) . ?
N2 C26 1.309(6) . ?
N2 C27 1.421(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9799 . ?
C1 H1C 0.9799 . ?
C2 C3 1.377(6) . ?
C2 C7 1.433(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.401(6) . ?
C4 C5 1.350(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.423(6) . ?
C6 C7 1.412(6) . ?
C6 C8 1.435(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.373(6) . ?
C9 C18 1.428(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.420(7) . ?
C11 C12 1.413(7) . ?
C11 C16 1.423(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.371(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.370(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.348(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.420(7) . ?
C16 C17 1.406(7) . ?
C17 H17 0.9500 . ?
C17 C18 1.382(7) . ?
C19 H19A 0.9801 . ?
C19 H19B 0.9799 . ?
C19 H19C 0.9800 . ?
C20 C21 1.366(6) . ?
C20 C25 1.431(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.396(7) . ?
C22 C23 1.356(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.412(6) . ?
C24 C25 1.424(6) . ?
C24 C26 1.424(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.361(6) . ?
C27 C36 1.424(6) . ?
C28 H28 0.9500 . ?
C28 C29 1.403(7) . ?
C29 C30 1.419(6) . ?
C29 C34 1.421(7) . ?
C30 H30 0.9500 . ?
C30 C31 1.365(8) . ?
C31 H31 0.9500 . ?
C31 C32 1.373(8) . ?
C32 H32 0.9500 . ?
C32 C33 1.360(7) . ?
C33 H33 0.9500 . ?
C33 C34 1.415(7) . ?
C34 C35 1.413(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.372(7) . ?
N3 H3A 1.0000 . ?
N3 C37 1.535(8) . ?
N3 C39 1.493(7) . ?
N3 C41 1.534(8) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.479(9) . ?
C38 H38A 0.9798 . ?
C38 H38B 0.9795 . ?
C38 H38C 0.9797 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.561(8) . ?
C40 H40A 0.9801 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9798 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.472(9) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9801 . ?
C42 H42C 0.9799 . ?
O9 H9 1.0264 . ?
O9 C44 1.393(7) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
O7 H7 0.8400 . ?
O7 C43 1.408(8) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9801 . ?
C43 H43C 0.9800 . ?
O8 H8A 0.8400 . ?
O8 C45 1.420(7) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9801 . ?
C45 H45C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co10 O3 176.47(13) . . ?
O2 Co10 O6 89.73(14) . . ?
O2 Co10 N1 96.66(14) . . ?
O2 Co10 N2 89.01(14) . . ?
O3 Co10 N1 86.42(15) . . ?
O5 Co10 O2 89.59(14) . . ?
O5 Co10 O3 88.72(15) . . ?
O5 Co10 O6 177.19(13) . . ?
O5 Co10 N1 89.58(15) . . ?
O5 Co10 N2 96.58(15) . . ?
O6 Co10 O3 92.10(15) . . ?
O6 Co10 N1 87.79(15) . . ?
O6 Co10 N2 86.14(15) . . ?
N2 Co10 O3 88.11(14) . . ?
N2 Co10 N1 171.67(16) . . ?
C2 O1 C1 117.5(4) . . ?
C7 O2 Co10 123.5(3) . . ?
C18 O3 Co10 111.8(3) . . ?
C20 O4 C19 116.7(4) . . ?
C25 O5 Co10 123.3(3) . . ?
C36 O6 Co10 112.0(3) . . ?
C8 N1 Co10 125.2(3) . . ?
C8 N1 C9 123.5(4) . . ?
C9 N1 Co10 111.0(3) . . ?
C26 N2 Co10 124.1(3) . . ?
C26 N2 C27 123.6(4) . . ?
C27 N2 Co10 111.8(3) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.3 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 123.8(4) . . ?
O1 C2 C7 114.4(4) . . ?
C3 C2 C7 121.8(4) . . ?
C2 C3 H3 120.4 . . ?
C2 C3 C4 119.2(5) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 Br1 118.0(4) . . ?
C5 C4 Br1 120.3(4) . . ?
C5 C4 C3 121.7(4) . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.1(4) . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C8 116.3(4) . . ?
C7 C6 C5 120.3(4) . . ?
C7 C6 C8 123.3(4) . . ?
O2 C7 C2 116.4(4) . . ?
O2 C7 C6 126.7(4) . . ?
C6 C7 C2 116.9(4) . . ?
N1 C8 C6 124.5(4) . . ?
N1 C8 H8 117.8 . . ?
C6 C8 H8 117.8 . . ?
N1 C9 C18 112.4(4) . . ?
C10 C9 N1 127.0(4) . . ?
C10 C9 C18 120.6(5) . . ?
C9 C10 H10 119.9 . . ?
C9 C10 C11 120.3(5) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 C16 119.3(5) . . ?
C12 C11 C10 122.4(5) . . ?
C12 C11 C16 118.3(5) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.1(5) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 119.3 . . ?
C14 C13 C12 121.4(5) . . ?
C14 C13 H13 119.3 . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.6(6) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 H15 119.5 . . ?
C14 C15 C16 121.0(5) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 C11 118.5(5) . . ?
C17 C16 C11 119.2(5) . . ?
C17 C16 C15 122.2(5) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 C16 121.1(5) . . ?
C18 C17 H17 119.5 . . ?
O3 C18 C9 118.1(4) . . ?
O3 C18 C17 122.4(4) . . ?
C17 C18 C9 119.4(4) . . ?
O4 C19 H19A 109.5 . . ?
O4 C19 H19B 109.5 . . ?
O4 C19 H19C 109.4 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O4 C20 C25 113.2(4) . . ?
C21 C20 O4 124.5(4) . . ?
C21 C20 C25 122.2(4) . . ?
C20 C21 H21 120.6 . . ?
C20 C21 C22 118.9(5) . . ?
C22 C21 H21 120.6 . . ?
C21 C22 Br2 117.9(4) . . ?
C23 C22 Br2 119.9(4) . . ?
C23 C22 C21 122.3(5) . . ?
C22 C23 H23 120.2 . . ?
C22 C23 C24 119.6(4) . . ?
C24 C23 H23 120.2 . . ?
C23 C24 C25 120.4(4) . . ?
C23 C24 C26 116.9(4) . . ?
C25 C24 C26 122.8(4) . . ?
O5 C25 C20 117.2(4) . . ?
O5 C25 C24 126.1(4) . . ?
C24 C25 C20 116.7(4) . . ?
N2 C26 C24 125.1(4) . . ?
N2 C26 H26 117.5 . . ?
C24 C26 H26 117.5 . . ?
N2 C27 C36 111.9(4) . . ?
C28 C27 N2 126.6(4) . . ?
C28 C27 C36 121.4(4) . . ?
C27 C28 H28 120.1 . . ?
C27 C28 C29 119.9(5) . . ?
C29 C28 H28 120.1 . . ?
C28 C29 C30 122.0(5) . . ?
C28 C29 C34 119.9(4) . . ?
C30 C29 C34 118.1(5) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 C29 120.8(6) . . ?
C31 C30 H30 119.6 . . ?
C30 C31 H31 119.9 . . ?
C30 C31 C32 120.3(5) . . ?
C32 C31 H31 119.9 . . ?
C31 C32 H32 119.2 . . ?
C33 C32 C31 121.7(6) . . ?
C33 C32 H32 119.2 . . ?
C32 C33 H33 120.0 . . ?
C32 C33 C34 120.0(6) . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C29 119.0(5) . . ?
C35 C34 C29 118.8(5) . . ?
C35 C34 C33 122.2(5) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 C34 120.8(5) . . ?
C36 C35 H35 119.6 . . ?
O6 C36 C27 118.0(4) . . ?
O6 C36 C35 122.8(4) . . ?
C35 C36 C27 119.1(4) . . ?
C37 N3 H3A 108.5 . . ?
C39 N3 H3A 108.5 . . ?
C39 N3 C37 110.1(5) . . ?
C39 N3 C41 112.7(5) . . ?
C41 N3 H3A 108.5 . . ?
C41 N3 C37 108.3(5) . . ?
N3 C37 H37A 109.0 . . ?
N3 C37 H37B 109.0 . . ?
H37A C37 H37B 107.8 . . ?
C38 C37 N3 112.8(6) . . ?
C38 C37 H37A 109.0 . . ?
C38 C37 H37B 109.0 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.4 . . ?
C37 C38 H38C 109.4 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N3 C39 H39A 109.0 . . ?
N3 C39 H39B 109.0 . . ?
N3 C39 C40 113.1(5) . . ?
H39A C39 H39B 107.8 . . ?
C40 C39 H39A 109.0 . . ?
C40 C39 H39B 109.0 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.3 . . ?
C39 C40 H40C 109.6 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N3 C41 H41A 108.9 . . ?
N3 C41 H41B 108.9 . . ?
H41A C41 H41B 107.7 . . ?
C42 C41 N3 113.4(6) . . ?
C42 C41 H41A 108.9 . . ?
C42 C41 H41B 108.9 . . ?
C41 C42 H42A 109.6 . . ?
C41 C42 H42B 109.3 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.4 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 O9 H9 124.3 . . ?
O9 C44 H44A 109.5 . . ?
O9 C44 H44B 109.5 . . ?
O9 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 O7 H7 109.5 . . ?
O7 C43 H43A 109.2 . . ?
O7 C43 H43B 109.7 . . ?
O7 C43 H43C 109.6 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 O8 H8A 109.5 . . ?
O8 C45 H45A 109.4 . . ?
O8 C45 H45B 109.7 . . ?
O8 C45 H45C 109.3 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br1 C4 C5 C6 -177.4(4) . . . . ?
Br2 C22 C23 C24 -178.8(4) . . . . ?
Co10 O2 C7 C2 175.1(3) . . . . ?
Co10 O2 C7 C6 -4.8(7) . . . . ?
Co10 O3 C18 C9 -0.8(5) . . . . ?
Co10 O3 C18 C17 -178.1(4) . . . . ?
Co10 O5 C25 C20 169.2(3) . . . . ?
Co10 O5 C25 C24 -12.5(7) . . . . ?
Co10 O6 C36 C27 -3.7(5) . . . . ?
Co10 O6 C36 C35 179.0(4) . . . . ?
Co10 N1 C8 C6 1.6(7) . . . . ?
Co10 N1 C9 C10 173.6(4) . . . . ?
Co10 N1 C9 C18 -5.0(5) . . . . ?
Co10 N2 C26 C24 4.0(6) . . . . ?
Co10 N2 C27 C28 -177.1(4) . . . . ?
Co10 N2 C27 C36 1.8(5) . . . . ?
O1 C2 C3 C4 -179.4(4) . . . . ?
O1 C2 C7 O2 0.9(6) . . . . ?
O1 C2 C7 C6 -179.2(4) . . . . ?
O2 Co10 O5 C25 104.6(4) . . . . ?
O2 Co10 O6 C36 -85.3(3) . . . . ?
O2 Co10 N2 C26 -101.1(4) . . . . ?
O2 Co10 N2 C27 86.8(3) . . . . ?
O3 Co10 O5 C25 -72.3(4) . . . . ?
O3 Co10 O6 C36 91.7(3) . . . . ?
O3 Co10 N2 C26 76.9(4) . . . . ?
O3 Co10 N2 C27 -95.3(3) . . . . ?
O4 C20 C21 C22 176.9(5) . . . . ?
O4 C20 C25 O5 1.8(6) . . . . ?
O4 C20 C25 C24 -176.6(4) . . . . ?
O5 Co10 O2 C7 95.0(3) . . . . ?
O5 Co10 O3 C18 -91.4(3) . . . . ?
O5 Co10 N2 C26 -11.6(4) . . . . ?
O5 Co10 N2 C27 176.3(3) . . . . ?
O6 Co10 O2 C7 -82.2(3) . . . . ?
O6 Co10 O3 C18 85.9(3) . . . . ?
O6 Co10 N2 C26 169.1(4) . . . . ?
O6 Co10 N2 C27 -3.0(3) . . . . ?
N1 Co10 O2 C7 5.5(4) . . . . ?
N1 Co10 O3 C18 -1.8(3) . . . . ?
N1 Co10 O5 C25 -158.7(4) . . . . ?
N1 Co10 O6 C36 178.0(3) . . . . ?
N1 C9 C10 C11 -177.3(5) . . . . ?
N1 C9 C18 O3 3.9(6) . . . . ?
N1 C9 C18 C17 -178.7(4) . . . . ?
N2 Co10 O2 C7 -168.4(4) . . . . ?
N2 Co10 O3 C18 171.9(3) . . . . ?
N2 Co10 O5 C25 15.6(4) . . . . ?
N2 Co10 O6 C36 3.7(3) . . . . ?
N2 C27 C28 C29 -178.7(4) . . . . ?
N2 C27 C36 O6 1.3(6) . . . . ?
N2 C27 C36 C35 178.7(4) . . . . ?
C1 O1 C2 C3 1.6(7) . . . . ?
C1 O1 C2 C7 -176.7(4) . . . . ?
C2 C3 C4 Br1 178.3(4) . . . . ?
C2 C3 C4 C5 -1.1(8) . . . . ?
C3 C2 C7 O2 -177.5(4) . . . . ?
C3 C2 C7 C6 2.4(7) . . . . ?
C3 C4 C5 C6 1.9(8) . . . . ?
C4 C5 C6 C7 -0.6(7) . . . . ?
C4 C5 C6 C8 177.0(4) . . . . ?
C5 C6 C7 O2 178.4(4) . . . . ?
C5 C6 C7 C2 -1.5(7) . . . . ?
C5 C6 C8 N1 -176.6(4) . . . . ?
C7 C2 C3 C4 -1.2(7) . . . . ?
C7 C6 C8 N1 0.9(8) . . . . ?
C8 N1 C9 C10 -0.4(8) . . . . ?
C8 N1 C9 C18 -179.0(4) . . . . ?
C8 C6 C7 O2 0.9(8) . . . . ?
C8 C6 C7 C2 -179.0(4) . . . . ?
C9 N1 C8 C6 174.7(4) . . . . ?
C9 C10 C11 C12 175.9(5) . . . . ?
C9 C10 C11 C16 -3.6(8) . . . . ?
C10 C9 C18 O3 -174.8(4) . . . . ?
C10 C9 C18 C17 2.6(7) . . . . ?
C10 C11 C12 C13 -177.5(5) . . . . ?
C10 C11 C16 C15 179.6(5) . . . . ?
C10 C11 C16 C17 2.2(8) . . . . ?
C11 C12 C13 C14 -1.6(10) . . . . ?
C11 C16 C17 C18 1.6(8) . . . . ?
C12 C11 C16 C15 0.0(8) . . . . ?
C12 C11 C16 C17 -177.3(5) . . . . ?
C12 C13 C14 C15 -0.9(10) . . . . ?
C13 C14 C15 C16 3.0(9) . . . . ?
C14 C15 C16 C11 -2.5(8) . . . . ?
C14 C15 C16 C17 174.7(6) . . . . ?
C15 C16 C17 C18 -175.6(5) . . . . ?
C16 C11 C12 C13 2.0(9) . . . . ?
C16 C17 C18 O3 173.2(5) . . . . ?
C16 C17 C18 C9 -4.1(8) . . . . ?
C18 C9 C10 C11 1.2(7) . . . . ?
C19 O4 C20 C21 5.9(8) . . . . ?
C19 O4 C20 C25 -176.5(5) . . . . ?
C20 C21 C22 Br2 179.5(4) . . . . ?
C20 C21 C22 C23 -0.8(8) . . . . ?
C21 C20 C25 O5 179.4(5) . . . . ?
C21 C20 C25 C24 1.0(7) . . . . ?
C21 C22 C23 C24 1.5(8) . . . . ?
C22 C23 C24 C25 -0.9(7) . . . . ?
C22 C23 C24 C26 179.9(5) . . . . ?
C23 C24 C25 O5 -178.5(4) . . . . ?
C23 C24 C25 C20 -0.3(7) . . . . ?
C23 C24 C26 N2 -176.7(4) . . . . ?
C25 C20 C21 C22 -0.5(8) . . . . ?
C25 C24 C26 N2 4.1(7) . . . . ?
C26 N2 C27 C28 10.8(7) . . . . ?
C26 N2 C27 C36 -170.4(4) . . . . ?
C26 C24 C25 O5 0.6(8) . . . . ?
C26 C24 C25 C20 178.8(4) . . . . ?
C27 N2 C26 C24 175.2(4) . . . . ?
C27 C28 C29 C30 178.9(5) . . . . ?
C27 C28 C29 C34 -0.1(7) . . . . ?
C28 C27 C36 O6 -179.8(4) . . . . ?
C28 C27 C36 C35 -2.4(7) . . . . ?
C28 C29 C30 C31 -176.7(5) . . . . ?
C28 C29 C34 C33 177.9(5) . . . . ?
C28 C29 C34 C35 -2.4(7) . . . . ?
C29 C30 C31 C32 -1.3(9) . . . . ?
C29 C34 C35 C36 2.5(7) . . . . ?
C30 C29 C34 C33 -1.1(7) . . . . ?
C30 C29 C34 C35 178.5(5) . . . . ?
C30 C31 C32 C33 -0.9(9) . . . . ?
C31 C32 C33 C34 2.1(9) . . . . ?
C32 C33 C34 C29 -1.0(8) . . . . ?
C32 C33 C34 C35 179.3(5) . . . . ?
C33 C34 C35 C36 -177.8(5) . . . . ?
C34 C29 C30 C31 2.3(8) . . . . ?
C34 C35 C36 O6 177.1(4) . . . . ?
C34 C35 C36 C27 -0.2(7) . . . . ?
C36 C27 C28 C29 2.6(7) . . . . ?
C37 N3 C39 C40 174.6(5) . . . . ?
C37 N3 C41 C42 -83.9(7) . . . . ?
C39 N3 C37 C38 -64.1(8) . . . . ?
C39 N3 C41 C42 154.0(6) . . . . ?
C41 N3 C37 C38 172.2(6) . . . . ?
C41 N3 C39 C40 -64.3(7) . . . . ?

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

data_6_CCDC_1406222
_database_code_depnum_ccdc_archive 'CCDC 1406222'
_audit_update_record             
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_audit_creation_date             2015-11-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C118 H110 Dy2 N4 Ni2 O20, 5(C0.5 H Cl)'
_chemical_formula_sum            'C120.50 H115 Cl5 Dy2 N4 Ni2 O20'
_chemical_formula_weight         2558.83
_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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.1776(15)
_cell_length_b                   18.8940(11)
_cell_length_c                   27.8333(11)
_cell_angle_alpha                90
_cell_angle_beta                 100.127(4)
_cell_angle_gamma                90
_cell_volume                     11481.1(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    173
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.795
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             5196
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.1362
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_number            ?
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.316
_diffrn_reflns_theta_min         2.782
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7112
_reflns_number_total             12896
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.475
_refine_diff_density_min         -2.562
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         12896
_refine_ls_number_restraints     264
_refine_ls_R_factor_all          0.1828
_refine_ls_R_factor_gt           0.1138
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1504P)²+133.4705P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2803
_refine_ls_wR_factor_ref         0.3192
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 Cl3-C58
 1.78 with sigma of 0.02
 C25-C38
 1.24 with sigma of 0.02
 C8-C7
 1.24 with sigma of 0.02
 C15-C7
 1.45 with sigma of 0.02
 C50-C15
 1.53 with sigma of 0.02
 C39-C38
 1.31 with sigma of 0.02
 O10-H10
 0.87 with sigma of 0.01
 C61-H10
 1.927776 with sigma of 0.02
 Ni1-H10
 2.669128 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C25 \\sim C38: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C23)
Uanis(C25) = Uanis(C38)
Uanis(C7) = Uanis(C15) = Uanis(C48) = Uanis(C49) = Uanis(C50) = Uanis(C51) =
Uanis(C52) = Uanis(C53) = Uanis(C54) = Uanis(C8)
Uanis(C2) = Uanis(C4AA) = Uanis(C4) = Uanis(C3) = Uanis(C5) = Uanis(C6) =
Uanis(C25) = Uanis(C38)
Uanis(C4) = Uanis(C3) = Uanis(C5) = Uanis(C25) = Uanis(C38) = Uanis(C39)
Uanis(C7) = Uanis(C8) = Uanis(C15) = Uanis(C48) = Uanis(C49) = Uanis(C50) =
Uanis(C51) = Uanis(C52) = Uanis(C53) = Uanis(C54)
5. Rigid body (RIGU) restrains
 C25, C38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C8, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Cl3(0.5) C58(0.25) H58A(0.25) H58B(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C25(H25A,H25B), C31(H31A,H31B), C61(H61A,H61B), C58(H58A,
 H58B), C9(H9A,H9B)
7.b Me refined with riding coordinates:
 C0AA(H0AA,H0AB,H0AC), C24(H24A,H24B,H24C), C47(H47A,H47B,H47C), C62(H62A,H62B,
 H62C)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C2AA(H2AA), C3AA(H3AA), C7(H7), C11(H11), C13(H13), C16(H16),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C28(H28), C32(H32),
  C34(H34), C36(H36), C38(H38), C5AA(H5AA), C42(H42), C43(H43), C44(H44),
 C45(H45), C46(H46), C49(H49), C51(H51), C54(H54)
7.d Fitted hexagon refined as free rotating group:
 C2(C4AA,C4,C3,C5,C6)
7.e X=CH2 refined with riding coordinates:
 C8(H8A,H8B), C33(H33A,H33B), C39(H39A,H39B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.47500(2) 0.50837(3) 0.38637(2) 0.0397(2) Uani 1 1 d . U . . .
Ni1 Ni 0.57021(6) 0.48419(7) 0.49850(4) 0.0310(3) Uani 1 1 d D U . . .
O1 O 0.3524(6) 0.6055(6) 0.2498(4) 0.084(3) Uani 1 1 d . U . . .
O2 O 0.4044(4) 0.5301(4) 0.3240(3) 0.0477(19) Uani 1 1 d . U . . .
O3 O 0.4846(3) 0.4482(4) 0.4648(2) 0.0304(14) Uani 1 1 d . U . . .
O4 O 0.5041(4) 0.6364(5) 0.3761(3) 0.0497(19) Uani 1 1 d . U . . .
O5 O 0.5587(3) 0.5493(4) 0.4404(3) 0.0391(16) Uani 1 1 d . U . . .
O6 O 0.5907(3) 0.4346(4) 0.5653(2) 0.0365(16) Uani 1 1 d . U . . .
O7 O 0.5469(5) 0.2744(6) 0.3858(4) 0.070(3) Uani 1 1 d . U . . .
O8 O 0.5298(4) 0.4115(5) 0.3760(3) 0.0497(18) Uani 1 1 d . U . . .
O9 O 0.5316(5) 0.5278(5) 0.3201(3) 0.061(2) Uani 1 1 d . U . . .
O10 O 0.6070(4) 0.4025(4) 0.4614(3) 0.0483(19) Uani 1 1 d D U . . .
H10 H 0.589(3) 0.361(2) 0.458(4) 0.072 Uiso 1 1 d DR . . . .
N1 N 0.3988(5) 0.4115(5) 0.3853(3) 0.043(2) Uani 1 1 d . U . . .
N2 N 0.6529(4) 0.5268(5) 0.5215(3) 0.0383(19) Uani 1 1 d . U . . .
C0AA C 0.3321(10) 0.6369(12) 0.2024(6) 0.117(8) Uani 1 1 d . U . . .
H0AA H 0.3230 0.5994 0.1779 0.176 Uiso 1 1 calc R . . . .
H0AB H 0.3644 0.6676 0.1942 0.176 Uiso 1 1 calc R . . . .
H0AC H 0.2950 0.6649 0.2030 0.176 Uiso 1 1 calc R . . . .
C1AA C 0.5582(6) 0.6592(7) 0.4009(4) 0.052(3) Uani 1 1 d . U . . .
C2 C 0.3485(4) 0.5106(6) 0.3022(4) 0.0862(18) Uani 1 1 d . U . . .
C4AA C 0.3211(5) 0.5475(6) 0.2609(4) 0.0862(18) Uani 1 1 d G U . . .
C4 C 0.2648(5) 0.5255(6) 0.2351(3) 0.0862(18) Uani 1 1 d G U . . .
H4 H 0.2460 0.5508 0.2069 0.103 Uiso 1 1 calc R . . . .
C3 C 0.2358(4) 0.4667(6) 0.2507(4) 0.0862(18) Uani 1 1 d G U . . .
C5 C 0.2632(5) 0.4298(6) 0.2920(4) 0.0862(18) Uani 1 1 d G U . . .
H5 H 0.2434 0.3896 0.3026 0.103 Uiso 1 1 calc R . . . .
C6 C 0.3195(5) 0.4518(6) 0.3178(3) 0.0862(18) Uani 1 1 d G U . . .
C2AA C 0.7445(6) 0.3958(8) 0.6282(4) 0.055(3) Uani 1 1 d . U . . .
H2AA H 0.7646 0.3643 0.6525 0.066 Uiso 1 1 calc R . . . .
C3AA C 0.4685(6) 0.2592(6) 0.4897(4) 0.043(3) Uani 1 1 d . U . . .
H3AA H 0.4850 0.2257 0.5140 0.052 Uiso 1 1 calc R . . . .
C7 C 0.6365(12) 0.2226(10) 0.2187(7) 0.145(4) Uani 1 1 d D U . . .
H7 H 0.6755 0.2385 0.2349 0.174 Uiso 1 1 calc R . . . .
C8 C 0.6266(14) 0.1621(10) 0.1996(7) 0.145(4) Uani 1 1 d D U . . .
H8A H 0.5865 0.1494 0.1840 0.174 Uiso 1 1 calc R . . . .
H8B H 0.6593 0.1293 0.2008 0.174 Uiso 1 1 calc R . . . .
C11 C 0.3461(6) 0.4067(7) 0.3577(4) 0.046(3) Uani 1 1 d . U . . .
H11 H 0.3213 0.3683 0.3646 0.055 Uiso 1 1 calc R . . . .
C12 C 0.4181(5) 0.3584(6) 0.4201(3) 0.033(2) Uani 1 1 d . U . . .
C13 C 0.3998(5) 0.2887(6) 0.4171(3) 0.038(2) Uani 1 1 d . U . . .
H13 H 0.3703 0.2745 0.3898 0.046 Uiso 1 1 calc R . . . .
C14 C 0.4227(6) 0.2372(6) 0.4523(4) 0.042(2) Uani 1 1 d . U . . .
C15 C 0.5827(12) 0.2635(11) 0.2132(6) 0.145(4) Uani 1 1 d D U . . .
H15A H 0.5460 0.2328 0.2058 0.174 Uiso 1 1 calc R . . . .
H15B H 0.5817 0.2982 0.1864 0.174 Uiso 1 1 calc R . . . .
C16 C 0.4912(5) 0.3273(6) 0.4936(4) 0.039(3) Uani 1 1 d . U . . .
H16 H 0.5247 0.3393 0.5185 0.047 Uiso 1 1 calc R . . . .
C17 C 0.4646(5) 0.3780(5) 0.4605(4) 0.034(2) Uani 1 1 d . U . . .
C18 C 0.3976(8) 0.1664(8) 0.4488(7) 0.0780(19) Uani 1 1 d . U . . .
C19 C 0.3355(8) 0.1522(8) 0.4299(6) 0.0780(19) Uani 1 1 d . U . . .
H19 H 0.3091 0.1901 0.4176 0.094 Uiso 1 1 calc R . . . .
C20 C 0.3128(8) 0.0851(8) 0.4288(6) 0.0780(19) Uani 1 1 d . U . . .
H20 H 0.2709 0.0770 0.4157 0.094 Uiso 1 1 calc R . . . .
C21 C 0.3485(8) 0.0304(9) 0.4460(7) 0.0780(19) Uani 1 1 d . U . . .
H21 H 0.3317 -0.0159 0.4446 0.094 Uiso 1 1 calc R . . . .
C22 C 0.4094(8) 0.0404(9) 0.4658(6) 0.0780(19) Uani 1 1 d . U . . .
H22 H 0.4337 0.0010 0.4786 0.094 Uiso 1 1 calc R . . . .
C23 C 0.4356(8) 0.1072(8) 0.4673(6) 0.0780(19) Uani 1 1 d . U . . .
H23 H 0.4778 0.1138 0.4802 0.094 Uiso 1 1 calc R . . . .
C24 C 0.4766(7) 0.6774(9) 0.3353(5) 0.080(5) Uani 1 1 d . U . . .
H24A H 0.5012 0.6737 0.3093 0.120 Uiso 1 1 calc R . . . .
H24B H 0.4746 0.7271 0.3450 0.120 Uiso 1 1 calc R . . . .
H24C H 0.4352 0.6598 0.3232 0.120 Uiso 1 1 calc R . . . .
C25 C 0.1741(8) 0.4430(9) 0.2234(5) 0.0862(18) Uani 1 1 d D U . . .
H25A H 0.1477 0.4303 0.2472 0.103 Uiso 1 1 calc R . . . .
H25B H 0.1545 0.4829 0.2035 0.103 Uiso 1 1 calc R . . . .
C26 C 0.5829(8) 0.7252(8) 0.3968(5) 0.075(5) Uani 1 1 d . U . . .
H26 H 0.5640 0.7565 0.3719 0.090 Uiso 1 1 calc R . . . .
C27 C 0.6361(8) 0.7469(9) 0.4293(5) 0.077(5) Uani 1 1 d . U . . .
C28 C 0.6637(8) 0.6987(8) 0.4616(5) 0.077(5) Uani 1 1 d . U . . .
H28 H 0.7006 0.7125 0.4822 0.092 Uiso 1 1 calc R . . . .
C29 C 0.6424(6) 0.6300(7) 0.4671(4) 0.055(3) Uani 1 1 d . U . . .
C30 C 0.5853(5) 0.6122(6) 0.4361(4) 0.040(2) Uani 1 1 d . U . . .
C31 C 0.6570(9) 0.8235(9) 0.4241(6) 0.089(5) Uani 1 1 d . U . . .
H31A H 0.6208 0.8546 0.4156 0.107 Uiso 1 1 calc R . . . .
H31B H 0.6811 0.8399 0.4555 0.107 Uiso 1 1 calc R . . . .
C32 C 0.6937(10) 0.8270(10) 0.3867(8) 0.104(7) Uani 1 1 d . U . . .
H32 H 0.7029 0.8728 0.3759 0.125 Uiso 1 1 calc R . . . .
C33 C 0.7152(11) 0.7747(10) 0.3666(9) 0.116(7) Uani 1 1 d . U . . .
H33A H 0.7072 0.7278 0.3762 0.140 Uiso 1 1 calc R . . . .
H33B H 0.7392 0.7823 0.3420 0.140 Uiso 1 1 calc R . . . .
C34 C 0.6721(6) 0.5865(7) 0.5064(4) 0.050(3) Uani 1 1 d . U . . .
H34 H 0.7104 0.6032 0.5234 0.060 Uiso 1 1 calc R . . . .
C35 C 0.6875(5) 0.4849(6) 0.5582(4) 0.042(2) Uani 1 1 d . U . . .
C36 C 0.7508(5) 0.4891(7) 0.5722(4) 0.047(3) Uani 1 1 d . U . . .
H36 H 0.7741 0.5209 0.5564 0.057 Uiso 1 1 calc R . . . .
C37 C 0.7791(6) 0.4455(8) 0.6098(4) 0.054(3) Uani 1 1 d . U . . .
C38 C 0.1779(8) 0.3892(8) 0.1951(6) 0.0862(18) Uani 1 1 d D U . . .
H38 H 0.1881 0.4015 0.1644 0.103 Uiso 1 1 calc R . . . .
C5AA C 0.6833(6) 0.3891(7) 0.6136(4) 0.049(3) Uani 1 1 d . U . . .
H5AA H 0.6617 0.3531 0.6273 0.059 Uiso 1 1 calc R . . . .
C40 C 0.6513(5) 0.4353(6) 0.5780(4) 0.037(2) Uani 1 1 d . U . . .
C41 C 0.8459(6) 0.4530(8) 0.6282(5) 0.061(3) Uani 1 1 d . U . . .
C42 C 0.8703(8) 0.4429(10) 0.6751(6) 0.078(5) Uani 1 1 d . U . . .
H42 H 0.8442 0.4298 0.6972 0.094 Uiso 1 1 calc R . . . .
C43 C 0.9345(9) 0.4511(14) 0.6931(7) 0.111(7) Uani 1 1 d . U . . .
H43 H 0.9509 0.4400 0.7262 0.134 Uiso 1 1 calc R . . . .
C44 C 0.9720(8) 0.4749(12) 0.6626(8) 0.101(6) Uani 1 1 d . U . . .
H44 H 1.0142 0.4831 0.6748 0.121 Uiso 1 1 calc R . . . .
C45 C 0.9489(8) 0.4869(11) 0.6144(8) 0.095(6) Uani 1 1 d . U . . .
H45 H 0.9755 0.5016 0.5930 0.114 Uiso 1 1 calc R . . . .
C46 C 0.8859(7) 0.4774(9) 0.5963(6) 0.072(4) Uani 1 1 d . U . . .
H46 H 0.8700 0.4873 0.5630 0.087 Uiso 1 1 calc R . . . .
C47 C 0.5537(9) 0.1997(9) 0.3914(6) 0.085(5) Uani 1 1 d . U . . .
H47A H 0.5239 0.1758 0.3664 0.127 Uiso 1 1 calc R . . . .
H47B H 0.5465 0.1859 0.4239 0.127 Uiso 1 1 calc R . . . .
H47C H 0.5953 0.1860 0.3878 0.127 Uiso 1 1 calc R . . . .
C48 C 0.5595(14) 0.3040(11) 0.3448(8) 0.145(4) Uani 1 1 d . U . . .
C49 C 0.5775(14) 0.2676(12) 0.3061(8) 0.145(4) Uani 1 1 d . U . . .
H49 H 0.5853 0.2182 0.3092 0.174 Uiso 1 1 calc R . . . .
C50 C 0.5844(14) 0.3019(11) 0.2625(7) 0.145(4) Uani 1 1 d D U . . .
C51 C 0.5802(14) 0.3753(11) 0.2619(8) 0.145(4) Uani 1 1 d . U . . .
H51 H 0.5886 0.4002 0.2342 0.174 Uiso 1 1 calc R . . . .
C52 C 0.5645(14) 0.4129(12) 0.2995(8) 0.145(4) Uani 1 1 d . U . . .
C53 C 0.5507(14) 0.3755(12) 0.3411(8) 0.145(4) Uani 1 1 d . U . . .
C54 C 0.5543(15) 0.4885(11) 0.2954(9) 0.145(4) Uani 1 1 d . U . . .
H54 H 0.5681 0.5101 0.2684 0.174 Uiso 1 1 calc R . . . .
C61 C 0.6685(8) 0.3936(14) 0.4497(7) 0.112(8) Uani 1 1 d D U . . .
H61A H 0.6980 0.3979 0.4807 0.135 Uiso 1 1 calc R . . . .
H61B H 0.6714 0.3444 0.4382 0.135 Uiso 1 1 calc R . . . .
C62 C 0.6886(11) 0.4364(19) 0.4170(9) 0.182(15) Uani 1 1 d . U . . .
H62A H 0.6698 0.4222 0.3839 0.272 Uiso 1 1 calc R . . . .
H62B H 0.7333 0.4326 0.4206 0.272 Uiso 1 1 calc R . . . .
H62C H 0.6774 0.4855 0.4227 0.272 Uiso 1 1 calc R . . . .
Cl3 Cl 0.5563(15) 0.8295(17) 0.2775(11) 0.284(13) Uiso 0.5 1 d D U . . .
C58 C 0.5000 0.891(3) 0.2500 0.42(11) Uiso 0.5 2 d DS TU P . .
H58A H 0.4849 0.9210 0.2745 0.499 Uiso 0.25 1 calc R . . . .
H58B H 0.5151 0.9210 0.2255 0.499 Uiso 0.25 1 calc R . . . .
Cl1 Cl 0.6839(5) 0.1815(6) 0.4878(4) 0.208(4) Uiso 1 1 d . U . . .
Cl2 Cl 0.6134(5) 0.1969(6) 0.5655(4) 0.223(4) Uiso 1 1 d . U . . .
C9 C 0.6462(14) 0.2378(17) 0.5218(11) 0.166(12) Uiso 1 1 d . U . . .
H9A H 0.6757 0.2735 0.5377 0.200 Uiso 1 1 calc R . . . .
H9B H 0.6138 0.2632 0.4993 0.200 Uiso 1 1 calc R . . . .
C39 C 0.1701(8) 0.3181(9) 0.2010(6) 0.0862(18) Uani 1 1 d D U . . .
H39A H 0.1599 0.3006 0.2305 0.103 Uiso 1 1 calc R . . . .
H39B H 0.1749 0.2862 0.1755 0.103 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Ni1 3.4770(13) . ?
Dy1 O2 2.162(8) . ?
Dy1 O3 2.438(6) . ?
Dy1 O4 2.533(8) . ?
Dy1 O5 2.307(7) . ?
Dy1 O6 2.404(7) 5_666 ?
Dy1 O8 2.242(9) . ?
Dy1 O9 2.436(8) . ?
Dy1 N1 2.487(9) . ?
Ni1 O3 2.143(7) 5_666 ?
Ni1 O3 2.078(7) . ?
Ni1 O5 2.012(7) . ?
Ni1 O6 2.061(7) . ?
Ni1 O10 2.100(8) . ?
Ni1 N2 2.001(9) . ?
O1 C0AA 1.445(17) . ?
O1 C4AA 1.362(13) . ?
O2 C2 1.333(11) . ?
O3 Ni1 2.143(7) 5_666 ?
O3 C17 1.397(12) . ?
O4 C1AA 1.345(14) . ?
O4 C24 1.422(14) . ?
O5 C30 1.343(13) . ?
O6 Dy1 2.404(7) 5_666 ?
O6 C40 1.328(13) . ?
O7 C47 1.426(19) . ?
O7 C48 1.34(2) . ?
O8 C53 1.336(19) . ?
O9 C54 1.18(2) . ?
O10 H10 0.874(10) . ?
O10 C61 1.468(17) . ?
N1 C11 1.284(14) . ?
N1 C12 1.408(14) . ?
N2 C34 1.303(15) . ?
N2 C35 1.409(15) . ?
C0AA H0AA 0.9800 . ?
C0AA H0AB 0.9800 . ?
C0AA H0AC 0.9800 . ?
C1AA C26 1.375(18) . ?
C1AA C30 1.379(16) . ?
C2 C4AA 1.3900 . ?
C2 C6 1.3900 . ?
C4AA C4 1.3900 . ?
C4 H4 0.9500 . ?
C4 C3 1.3900 . ?
C3 C5 1.3900 . ?
C3 C25 1.511(17) . ?
C5 H5 0.9500 . ?
C5 C6 1.3900 . ?
C6 C11 1.441(13) . ?
C2AA H2AA 0.9500 . ?
C2AA C37 1.369(19) . ?
C2AA C5AA 1.353(17) . ?
C3AA H3AA 0.9500 . ?
C3AA C14 1.384(16) . ?
C3AA C16 1.379(16) . ?
C7 H7 0.9500 . ?
C7 C8 1.263(16) . ?
C7 C15 1.409(18) . ?
C8 H8A 0.9500 . ?
C8 H8B 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.377(15) . ?
C12 C17 1.435(13) . ?
C13 H13 0.9500 . ?
C13 C14 1.410(15) . ?
C14 C18 1.446(19) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C50 1.546(16) . ?
C16 H16 0.9500 . ?
C16 C17 1.386(14) . ?
C18 C19 1.41(2) . ?
C18 C23 1.44(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.36(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.34(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.38(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.39(2) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C38 1.298(15) . ?
C26 H26 0.9500 . ?
C26 C27 1.417(19) . ?
C27 C28 1.35(2) . ?
C27 C31 1.53(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.400(18) . ?
C29 C30 1.440(16) . ?
C29 C34 1.432(17) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.43(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.27(3) . ?
C33 H33A 0.9500 . ?
C33 H33B 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.391(16) . ?
C35 C40 1.408(16) . ?
C36 H36 0.9500 . ?
C36 C37 1.391(17) . ?
C37 C41 1.487(18) . ?
C38 H38 0.9500 . ?
C38 C39 1.368(15) . ?
C5AA H5AA 0.9500 . ?
C5AA C40 1.415(15) . ?
C41 C42 1.334(19) . ?
C41 C46 1.44(2) . ?
C42 H42 0.9500 . ?
C42 C43 1.43(2) . ?
C43 H43 0.9500 . ?
C43 C44 1.37(3) . ?
C44 H44 0.9500 . ?
C44 C45 1.37(3) . ?
C45 H45 0.9500 . ?
C45 C46 1.41(2) . ?
C46 H46 0.9500 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C49 1.40(2) . ?
C48 C53 1.37(3) . ?
C49 H49 0.9500 . ?
C49 C50 1.41(3) . ?
C50 C51 1.39(3) . ?
C51 H51 0.9500 . ?
C51 C52 1.36(2) . ?
C52 C53 1.43(3) . ?
C52 C54 1.45(3) . ?
C54 H54 0.9500 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.35(3) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
Cl3 C58 1.77(2) . ?
C58 Cl3 1.77(2) 2_655 ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
Cl1 C9 1.73(3) . ?
Cl2 C9 1.71(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C39 H39A 0.9500 . ?
C39 H39B 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 Ni1 170.1(2) . . ?
O2 Dy1 O3 138.1(3) . . ?
O2 Dy1 O4 83.8(3) . . ?
O2 Dy1 O5 147.7(3) . . ?
O2 Dy1 O6 86.5(3) . 5_666 ?
O2 Dy1 O8 112.6(3) . . ?
O2 Dy1 O9 76.1(3) . . ?
O2 Dy1 N1 74.6(3) . . ?
O3 Dy1 Ni1 36.00(17) . . ?
O3 Dy1 O4 124.2(2) . . ?
O3 Dy1 N1 67.7(3) . . ?
O4 Dy1 Ni1 95.73(18) . . ?
O5 Dy1 Ni1 33.58(18) . . ?
O5 Dy1 O3 68.8(2) . . ?
O5 Dy1 O4 64.0(3) . . ?
O5 Dy1 O6 89.0(3) . 5_666 ?
O5 Dy1 O9 88.9(3) . . ?
O5 Dy1 N1 136.2(3) . . ?
O6 Dy1 Ni1 83.63(16) 5_666 . ?
O6 Dy1 O3 71.0(2) 5_666 . ?
O6 Dy1 O4 80.0(3) 5_666 . ?
O6 Dy1 O9 143.1(3) 5_666 . ?
O6 Dy1 N1 82.0(3) 5_666 . ?
O8 Dy1 Ni1 75.6(2) . . ?
O8 Dy1 O3 76.7(3) . . ?
O8 Dy1 O4 127.6(3) . . ?
O8 Dy1 O5 88.0(3) . . ?
O8 Dy1 O6 146.4(3) . 5_666 ?
O8 Dy1 O9 70.3(3) . . ?
O8 Dy1 N1 77.3(3) . . ?
O9 Dy1 Ni1 112.8(2) . . ?
O9 Dy1 O3 140.7(3) . . ?
O9 Dy1 O4 66.1(3) . . ?
O9 Dy1 N1 122.8(3) . . ?
N1 Dy1 Ni1 102.6(2) . . ?
N1 Dy1 O4 152.6(3) . . ?
O3 Ni1 Dy1 92.47(17) 5_666 . ?
O3 Ni1 Dy1 43.61(18) . . ?
O3 Ni1 O3 82.0(3) . 5_666 ?
O3 Ni1 O10 86.6(3) . . ?
O5 Ni1 Dy1 39.4(2) . . ?
O5 Ni1 O3 82.0(3) . . ?
O5 Ni1 O3 90.9(3) . 5_666 ?
O5 Ni1 O6 168.6(3) . . ?
O5 Ni1 O10 93.5(3) . . ?
O6 Ni1 Dy1 150.7(2) . . ?
O6 Ni1 O3 84.0(3) . 5_666 ?
O6 Ni1 O3 107.3(3) . . ?
O6 Ni1 O10 93.8(3) . . ?
O10 Ni1 Dy1 83.3(2) . . ?
O10 Ni1 O3 167.1(3) . 5_666 ?
N2 Ni1 Dy1 127.7(3) . . ?
N2 Ni1 O3 99.9(3) . 5_666 ?
N2 Ni1 O3 171.4(3) . . ?
N2 Ni1 O5 89.5(3) . . ?
N2 Ni1 O6 81.4(3) . . ?
N2 Ni1 O10 92.3(4) . . ?
C4AA O1 C0AA 116.6(13) . . ?
C2 O2 Dy1 142.9(6) . . ?
Ni1 O3 Dy1 100.4(3) . . ?
Ni1 O3 Dy1 100.4(3) 5_666 . ?
Ni1 O3 Ni1 98.0(3) . 5_666 ?
C17 O3 Dy1 112.9(5) . . ?
C17 O3 Ni1 114.1(6) . 5_666 ?
C17 O3 Ni1 126.9(6) . . ?
C1AA O4 Dy1 118.0(7) . . ?
C1AA O4 C24 117.0(10) . . ?
C24 O4 Dy1 121.9(8) . . ?
Ni1 O5 Dy1 107.0(3) . . ?
C30 O5 Dy1 123.7(6) . . ?
C30 O5 Ni1 128.1(7) . . ?
Ni1 O6 Dy1 104.0(3) . 5_666 ?
C40 O6 Dy1 122.0(6) . 5_666 ?
C40 O6 Ni1 106.7(6) . . ?
C48 O7 C47 118.2(13) . . ?
C53 O8 Dy1 140.8(13) . . ?
C54 O9 Dy1 132.4(12) . . ?
Ni1 O10 H10 120.7(19) . . ?
C61 O10 Ni1 130.5(10) . . ?
C61 O10 H10 107(2) . . ?
C11 N1 Dy1 127.2(8) . . ?
C11 N1 C12 119.6(10) . . ?
C12 N1 Dy1 113.1(7) . . ?
C34 N2 Ni1 125.4(8) . . ?
C34 N2 C35 123.6(10) . . ?
C35 N2 Ni1 111.0(7) . . ?
O1 C0AA H0AA 109.5 . . ?
O1 C0AA H0AB 109.5 . . ?
O1 C0AA H0AC 109.5 . . ?
H0AA C0AA H0AB 109.5 . . ?
H0AA C0AA H0AC 109.5 . . ?
H0AB C0AA H0AC 109.5 . . ?
O4 C1AA C26 125.4(12) . . ?
O4 C1AA C30 113.4(10) . . ?
C26 C1AA C30 120.9(12) . . ?
O2 C2 C4AA 118.3(8) . . ?
O2 C2 C6 121.5(8) . . ?
C4AA C2 C6 120.0 . . ?
O1 C4AA C2 115.2(8) . . ?
O1 C4AA C4 124.8(8) . . ?
C2 C4AA C4 120.0 . . ?
C4AA C4 H4 120.0 . . ?
C3 C4 C4AA 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C3 C5 120.0 . . ?
C4 C3 C25 120.5(9) . . ?
C5 C3 C25 119.5(9) . . ?
C3 C5 H5 120.0 . . ?
C6 C5 C3 120.0 . . ?
C6 C5 H5 120.0 . . ?
C2 C6 C11 124.3(8) . . ?
C5 C6 C2 120.0 . . ?
C5 C6 C11 115.5(8) . . ?
C37 C2AA H2AA 118.3 . . ?
C5AA C2AA H2AA 118.3 . . ?
C5AA C2AA C37 123.3(12) . . ?
C14 C3AA H3AA 118.4 . . ?
C16 C3AA H3AA 118.4 . . ?
C16 C3AA C14 123.3(11) . . ?
C8 C7 H7 124.2 . . ?
C8 C7 C15 112(2) . . ?
C15 C7 H7 124.2 . . ?
C7 C8 H8A 120.0 . . ?
C7 C8 H8B 120.0 . . ?
H8A C8 H8B 120.0 . . ?
N1 C11 C6 128.6(11) . . ?
N1 C11 H11 115.7 . . ?
C6 C11 H11 115.7 . . ?
N1 C12 C17 116.5(9) . . ?
C13 C12 N1 126.1(9) . . ?
C13 C12 C17 117.2(10) . . ?
C12 C13 H13 118.3 . . ?
C12 C13 C14 123.5(10) . . ?
C14 C13 H13 118.3 . . ?
C3AA C14 C13 116.3(10) . . ?
C3AA C14 C18 123.5(12) . . ?
C13 C14 C18 120.2(12) . . ?
C7 C15 H15A 110.6 . . ?
C7 C15 H15B 110.6 . . ?
C7 C15 C50 105.9(19) . . ?
H15A C15 H15B 108.7 . . ?
C50 C15 H15A 110.6 . . ?
C50 C15 H15B 110.6 . . ?
C3AA C16 H16 120.5 . . ?
C3AA C16 C17 119.0(10) . . ?
C17 C16 H16 120.5 . . ?
O3 C17 C12 119.0(9) . . ?
C16 C17 O3 120.5(9) . . ?
C16 C17 C12 120.4(10) . . ?
C19 C18 C14 122.7(15) . . ?
C19 C18 C23 117.2(14) . . ?
C23 C18 C14 120.0(15) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 C18 121.2(17) . . ?
C20 C19 H19 119.4 . . ?
C19 C20 H20 119.4 . . ?
C21 C20 C19 121.2(18) . . ?
C21 C20 H20 119.4 . . ?
C20 C21 H21 119.5 . . ?
C20 C21 C22 121.0(16) . . ?
C22 C21 H21 119.5 . . ?
C21 C22 H22 119.6 . . ?
C21 C22 C23 120.7(17) . . ?
C23 C22 H22 119.6 . . ?
C18 C23 H23 120.6 . . ?
C22 C23 C18 118.7(16) . . ?
C22 C23 H23 120.6 . . ?
O4 C24 H24A 109.5 . . ?
O4 C24 H24B 109.5 . . ?
O4 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C3 C25 H25A 109.0 . . ?
C3 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
C38 C25 C3 112.8(16) . . ?
C38 C25 H25A 109.0 . . ?
C38 C25 H25B 109.0 . . ?
C1AA C26 H26 119.7 . . ?
C1AA C26 C27 120.6(12) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 C31 116.4(13) . . ?
C28 C27 C26 117.4(13) . . ?
C28 C27 C31 126.2(14) . . ?
C27 C28 H28 117.4 . . ?
C27 C28 C29 125.3(13) . . ?
C29 C28 H28 117.4 . . ?
C28 C29 C30 115.4(12) . . ?
C28 C29 C34 119.8(11) . . ?
C34 C29 C30 124.2(11) . . ?
O5 C30 C1AA 119.3(10) . . ?
O5 C30 C29 120.5(10) . . ?
C1AA C30 C29 120.2(11) . . ?
C27 C31 H31A 109.8 . . ?
C27 C31 H31B 109.8 . . ?
H31A C31 H31B 108.2 . . ?
C32 C31 C27 109.4(17) . . ?
C32 C31 H31A 109.8 . . ?
C32 C31 H31B 109.8 . . ?
C31 C32 H32 116.9 . . ?
C33 C32 C31 126.1(19) . . ?
C33 C32 H32 116.9 . . ?
C32 C33 H33A 120.0 . . ?
C32 C33 H33B 120.0 . . ?
H33A C33 H33B 120.0 . . ?
N2 C34 C29 127.6(11) . . ?
N2 C34 H34 116.2 . . ?
C29 C34 H34 116.2 . . ?
C36 C35 N2 124.4(11) . . ?
C36 C35 C40 123.1(11) . . ?
C40 C35 N2 112.4(10) . . ?
C35 C36 H36 120.8 . . ?
C37 C36 C35 118.4(12) . . ?
C37 C36 H36 120.8 . . ?
C2AA C37 C36 118.8(12) . . ?
C2AA C37 C41 121.6(12) . . ?
C36 C37 C41 119.6(13) . . ?
C25 C38 H38 113.8 . . ?
C25 C38 C39 132.3(18) . . ?
C39 C38 H38 113.8 . . ?
C2AA C5AA H5AA 119.8 . . ?
C2AA C5AA C40 120.5(13) . . ?
C40 C5AA H5AA 119.8 . . ?
O6 C40 C35 121.6(10) . . ?
O6 C40 C5AA 122.7(11) . . ?
C35 C40 C5AA 115.7(11) . . ?
C42 C41 C37 122.3(14) . . ?
C42 C41 C46 117.4(14) . . ?
C46 C41 C37 120.2(13) . . ?
C41 C42 H42 118.8 . . ?
C41 C42 C43 122.4(17) . . ?
C43 C42 H42 118.8 . . ?
C42 C43 H43 120.2 . . ?
C44 C43 C42 119.5(18) . . ?
C44 C43 H43 120.2 . . ?
C43 C44 H44 119.9 . . ?
C43 C44 C45 120.1(17) . . ?
C45 C44 H44 119.9 . . ?
C44 C45 H45 119.8 . . ?
C44 C45 C46 120.3(19) . . ?
C46 C45 H45 119.8 . . ?
C41 C46 H46 120.0 . . ?
C45 C46 C41 120.0(16) . . ?
C45 C46 H46 120.0 . . ?
O7 C47 H47A 109.5 . . ?
O7 C47 H47B 109.5 . . ?
O7 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O7 C48 C49 125.5(19) . . ?
O7 C48 C53 115.3(15) . . ?
C53 C48 C49 119.1(18) . . ?
C48 C49 H49 119.1 . . ?
C48 C49 C50 122(2) . . ?
C50 C49 H49 119.1 . . ?
C49 C50 C15 123.9(18) . . ?
C51 C50 C15 117.9(18) . . ?
C51 C50 C49 117.0(15) . . ?
C50 C51 H51 118.7 . . ?
C52 C51 C50 122.5(18) . . ?
C52 C51 H51 118.7 . . ?
C51 C52 C53 119(2) . . ?
C51 C52 C54 120.8(19) . . ?
C53 C52 C54 119.8(17) . . ?
O8 C53 C48 120.8(16) . . ?
O8 C53 C52 119.1(19) . . ?
C48 C53 C52 120.0(17) . . ?
O9 C54 C52 130.5(18) . . ?
O9 C54 H54 114.7 . . ?
C52 C54 H54 114.7 . . ?
O10 C61 H61A 107.1 . . ?
O10 C61 H61B 107.1 . . ?
H61A C61 H61B 106.8 . . ?
C62 C61 O10 121(2) . . ?
C62 C61 H61A 107.1 . . ?
C62 C61 H61B 107.1 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
Cl3 C58 Cl3 99(4) 2_655 . ?
Cl3 C58 H58A 112.1 2_655 . ?
Cl3 C58 H58A 112.1 . . ?
Cl3 C58 H58B 112.1 2_655 . ?
Cl3 C58 H58B 112.1 . . ?
H58A C58 H58B 109.7 . . ?
Cl1 C9 H9A 108.6 . . ?
Cl1 C9 H9B 108.6 . . ?
Cl2 C9 Cl1 114.7(19) . . ?
Cl2 C9 H9A 108.6 . . ?
Cl2 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C38 C39 H39A 120.0 . . ?
C38 C39 H39B 120.0 . . ?
H39A C39 H39B 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O2 C2 C4AA 176.6(9) . . . . ?
Dy1 O2 C2 C6 -8.1(18) . . . . ?
Dy1 O3 C17 C12 -28.2(12) . . . . ?
Dy1 O3 C17 C16 148.9(9) . . . . ?
Dy1 O4 C1AA C26 175.0(13) . . . . ?
Dy1 O4 C1AA C30 -11.8(15) . . . . ?
Dy1 O5 C30 C1AA 7.4(15) . . . . ?
Dy1 O5 C30 C29 -171.1(9) . . . . ?
Dy1 O6 C40 C35 -96.9(10) 5_666 . . . ?
Dy1 O6 C40 C5AA 80.2(12) 5_666 . . . ?
Dy1 O8 C53 C48 -151(2) . . . . ?
Dy1 O8 C53 C52 30(4) . . . . ?
Dy1 O9 C54 C52 -10(5) . . . . ?
Dy1 N1 C11 C6 6.2(19) . . . . ?
Dy1 N1 C12 C13 -153.6(9) . . . . ?
Dy1 N1 C12 C17 21.3(12) . . . . ?
Ni1 O3 C17 C12 -152.5(8) . . . . ?
Ni1 O3 C17 C12 85.6(10) 5_666 . . . ?
Ni1 O3 C17 C16 24.6(14) . . . . ?
Ni1 O3 C17 C16 -97.3(11) 5_666 . . . ?
Ni1 O5 C30 C1AA -159.0(9) . . . . ?
Ni1 O5 C30 C29 22.5(16) . . . . ?
Ni1 O6 C40 C35 22.1(12) . . . . ?
Ni1 O6 C40 C5AA -160.8(9) . . . . ?
Ni1 O10 C61 C62 -69(2) . . . . ?
Ni1 N2 C34 C29 -8(2) . . . . ?
Ni1 N2 C35 C36 161.9(10) . . . . ?
Ni1 N2 C35 C40 -15.3(12) . . . . ?
O1 C4AA C4 C3 -177.7(14) . . . . ?
O2 C2 C4AA O1 -6.7(13) . . . . ?
O2 C2 C4AA C4 175.4(12) . . . . ?
O2 C2 C6 C5 -175.2(13) . . . . ?
O2 C2 C6 C11 -0.3(14) . . . . ?
O4 C1AA C26 C27 171.5(15) . . . . ?
O4 C1AA C30 O5 3.7(18) . . . . ?
O4 C1AA C30 C29 -177.7(11) . . . . ?
O7 C48 C49 C50 174(3) . . . . ?
O7 C48 C53 O8 -1(4) . . . . ?
O7 C48 C53 C52 178(3) . . . . ?
N1 C12 C13 C14 177.4(11) . . . . ?
N1 C12 C17 O3 4.3(15) . . . . ?
N1 C12 C17 C16 -172.8(10) . . . . ?
N2 C35 C36 C37 178.6(11) . . . . ?
N2 C35 C40 O6 -5.4(15) . . . . ?
N2 C35 C40 C5AA 177.3(10) . . . . ?
C0AA O1 C4AA C2 168.1(14) . . . . ?
C0AA O1 C4AA C4 -14(2) . . . . ?
C1AA C26 C27 C28 5(3) . . . . ?
C1AA C26 C27 C31 -175.3(17) . . . . ?
C2 C4AA C4 C3 0.0 . . . . ?
C2 C6 C11 N1 -0.2(19) . . . . ?
C4AA C2 C6 C5 0.0 . . . . ?
C4AA C2 C6 C11 174.9(13) . . . . ?
C4AA C4 C3 C5 0.0 . . . . ?
C4AA C4 C3 C25 179.1(13) . . . . ?
C4 C3 C5 C6 0.0 . . . . ?
C4 C3 C25 C38 101.4(16) . . . . ?
C3 C5 C6 C2 0.0 . . . . ?
C3 C5 C6 C11 -175.3(12) . . . . ?
C3 C25 C38 C39 98(2) . . . . ?
C5 C3 C25 C38 -79.4(17) . . . . ?
C5 C6 C11 N1 174.9(11) . . . . ?
C6 C2 C4AA O1 177.9(13) . . . . ?
C6 C2 C4AA C4 0.0 . . . . ?
C2AA C37 C41 C42 -36(2) . . . . ?
C2AA C37 C41 C46 149.8(15) . . . . ?
C2AA C5AA C40 O6 -174.5(11) . . . . ?
C2AA C5AA C40 C35 2.8(17) . . . . ?
C3AA C14 C18 C19 145.5(16) . . . . ?
C3AA C14 C18 C23 -31(2) . . . . ?
C3AA C16 C17 O3 176.9(10) . . . . ?
C3AA C16 C17 C12 -6.0(17) . . . . ?
C7 C15 C50 C49 -69(3) . . . . ?
C7 C15 C50 C51 124(3) . . . . ?
C8 C7 C15 C50 138.9(18) . . . . ?
C11 N1 C12 C13 27.4(18) . . . . ?
C11 N1 C12 C17 -157.7(11) . . . . ?
C12 N1 C11 C6 -175.0(12) . . . . ?
C12 C13 C14 C3AA -4.0(18) . . . . ?
C12 C13 C14 C18 174.8(13) . . . . ?
C13 C12 C17 O3 179.7(9) . . . . ?
C13 C12 C17 C16 2.7(16) . . . . ?
C13 C14 C18 C19 -33(2) . . . . ?
C13 C14 C18 C23 150.1(15) . . . . ?
C14 C3AA C16 C17 4.5(19) . . . . ?
C14 C18 C19 C20 -177.4(16) . . . . ?
C14 C18 C23 C22 176.5(15) . . . . ?
C15 C50 C51 C52 162(3) . . . . ?
C16 C3AA C14 C13 0.4(19) . . . . ?
C16 C3AA C14 C18 -178.4(14) . . . . ?
C17 C12 C13 C14 2.5(17) . . . . ?
C18 C19 C20 C21 0(3) . . . . ?
C19 C18 C23 C22 0(3) . . . . ?
C19 C20 C21 C22 1(3) . . . . ?
C20 C21 C22 C23 -2(3) . . . . ?
C21 C22 C23 C18 2(3) . . . . ?
C23 C18 C19 C20 -1(3) . . . . ?
C24 O4 C1AA C26 14(2) . . . . ?
C24 O4 C1AA C30 -172.5(13) . . . . ?
C25 C3 C5 C6 -179.1(13) . . . . ?
C26 C1AA C30 O5 177.3(14) . . . . ?
C26 C1AA C30 C29 -4(2) . . . . ?
C26 C27 C28 C29 -3(3) . . . . ?
C26 C27 C31 C32 -84(2) . . . . ?
C27 C28 C29 C30 -2(3) . . . . ?
C27 C28 C29 C34 -173.0(17) . . . . ?
C27 C31 C32 C33 -12(3) . . . . ?
C28 C27 C31 C32 95(2) . . . . ?
C28 C29 C30 O5 -175.8(13) . . . . ?
C28 C29 C30 C1AA 6(2) . . . . ?
C28 C29 C34 N2 168.0(15) . . . . ?
C30 C1AA C26 C27 -1(3) . . . . ?
C30 C29 C34 N2 -2(2) . . . . ?
C31 C27 C28 C29 177.1(18) . . . . ?
C34 N2 C35 C36 -20.3(18) . . . . ?
C34 N2 C35 C40 162.4(12) . . . . ?
C34 C29 C30 O5 -5(2) . . . . ?
C34 C29 C30 C1AA 176.2(13) . . . . ?
C35 N2 C34 C29 174.9(13) . . . . ?
C35 C36 C37 C2AA 6.2(19) . . . . ?
C35 C36 C37 C41 -175.0(12) . . . . ?
C36 C35 C40 O6 177.2(11) . . . . ?
C36 C35 C40 C5AA 0.0(17) . . . . ?
C36 C37 C41 C42 145.7(16) . . . . ?
C36 C37 C41 C46 -29(2) . . . . ?
C37 C2AA C5AA C40 -1(2) . . . . ?
C37 C41 C42 C43 -179.0(17) . . . . ?
C37 C41 C46 C45 177.7(16) . . . . ?
C5AA C2AA C37 C36 -4(2) . . . . ?
C5AA C2AA C37 C41 177.5(13) . . . . ?
C40 C35 C36 C37 -4.4(19) . . . . ?
C41 C42 C43 C44 5(3) . . . . ?
C42 C41 C46 C45 3(2) . . . . ?
C42 C43 C44 C45 -4(4) . . . . ?
C43 C44 C45 C46 2(3) . . . . ?
C44 C45 C46 C41 -2(3) . . . . ?
C46 C41 C42 C43 -4(3) . . . . ?
C47 O7 C48 C49 2(4) . . . . ?
C47 O7 C48 C53 179(2) . . . . ?
C48 C49 C50 C15 -159(3) . . . . ?
C48 C49 C50 C51 8(5) . . . . ?
C49 C48 C53 O8 176(3) . . . . ?
C49 C48 C53 C52 -5(5) . . . . ?
C49 C50 C51 C52 -6(5) . . . . ?
C50 C51 C52 C53 -1(5) . . . . ?
C50 C51 C52 C54 -173(3) . . . . ?
C51 C52 C53 O8 -174(3) . . . . ?
C51 C52 C53 C48 7(5) . . . . ?
C51 C52 C54 O9 167(3) . . . . ?
C53 C48 C49 C50 -3(5) . . . . ?
C53 C52 C54 O9 -6(6) . . . . ?
C54 C52 C53 O8 -1(5) . . . . ?
C54 C52 C53 C48 179(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_7_CCDC_1406223
_database_code_depnum_ccdc_archive 'CCDC 1406223'
_audit_update_record             
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_audit_creation_date             2014-07-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C110 H118 Dy2 N10 Ni2 O18, 4(C3 H7 N O), 2(Cl O4)'
_chemical_formula_sum            'C122 H146 Cl2 Dy2 N14 Ni2 O30'
_chemical_formula_weight         2801.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         Ni2Dy2C124H130N10O40
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.5403(7)
_cell_length_b                   14.7915(10)
_cell_length_c                   18.880(2)
_cell_angle_alpha                100.291(8)
_cell_angle_beta                 106.198(7)
_cell_angle_gamma                105.143(5)
_cell_volume                     3124.5(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    3730
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.6500
_cell_measurement_theta_min      2.6630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1438
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9418
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.037
_diffrn_reflns_theta_min         2.478
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -44.00   52.00   1.0000   14.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.0128   38.0000   90.0000 96

#__ type_ start__ end____ width___ exp.time_
  2 omega    8.00   60.00   1.0000   14.5000
omega____ theta____ kappa____ phi______ frames
    -       18.3253  -99.0000  120.0000 52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0367260000
_diffrn_orient_matrix_UB_12      0.0488734000
_diffrn_orient_matrix_UB_13      0.0185765000
_diffrn_orient_matrix_UB_21      -0.0048156000
_diffrn_orient_matrix_UB_22      0.0092625000
_diffrn_orient_matrix_UB_23      -0.0361627000
_diffrn_orient_matrix_UB_31      -0.0501744000
_diffrn_orient_matrix_UB_32      0.0137674000
_diffrn_orient_matrix_UB_33      -0.0002509000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6754
_reflns_number_total             7781
_reflns_odcompleteness_completeness 56.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         7781
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0437
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0527P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1165
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9-C10 = C32-C33A
 1.29 with sigma of 0.02
 C32-C33
 1.29 with sigma of 0.02
 C33A-C32A
 1.29 with sigma of 0.02
 C33-C32
 1.29 with sigma of 0.02
 C8-C9 = C31A-C32A
 1.49 with sigma of 0.02
 C31-C32
 1.49 with sigma of 0.02
 C31A-C27
 1.49 with sigma of 0.02
 C31-C27
 1.49 with sigma of 0.02
 C31A-C27
 1.53 with sigma of 0.02
 C31-C27
 1.53 with sigma of 0.02
3. Rigid bond restraints
 C33, C33A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C32A, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31A, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31, C31A, C32, C32A, C33A, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C33 \\sim C33A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C32A \\sim C32: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C31A \\sim C31: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C31 \\sim C31A \\sim C32 \\sim C32A \\sim C33A \\sim C33: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uiso(C33) = Uiso(C33A)
Uiso(C32A) = Uiso(C32)
Uiso(C31) = Uiso(C31A)
Uiso(C31) = Uiso(C31A) = Uiso(C32) = Uiso(C32A) = Uiso(C33A) = Uiso(C33)
5. Others
 Fixed Sof: C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32(0.5) C33(0.5) H33A(0.5)
 H33B(0.5) C33A(0.5) H33C(0.5) H33D(0.5) C32A(0.5) H32A(0.5) C31A(0.5)
 H31C(0.5) H31D(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C31(H31A,H31B), C31A(H31C,H31D)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11), C13(H13), C15(H15), C16(H16), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C28(H28), C32(H32), C34(H34),
  C36(H36), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44), C45(H45),
 C46(H46), C47(H47), C50(H50), C53(H53), C56(H56), C59(H59), C32A(H32A)
6.c X=CH2 refined with riding coordinates:
 C10(H10A,H10B), C33(H33A,H33B), C33A(H33C,H33D)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C24(H24A,H24B,H24C), C49(H49A,H49B,H49C), C51(H51A,H51B,
 H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,
 H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C),
 C48(H48A,H48B,H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.18632(2) 0.66304(2) 0.64420(2) 0.02359(12) Uani 1 1 d . . . . .
Ni1 Ni 0.07771(5) 0.43256(5) 0.51349(5) 0.0208(2) Uani 1 1 d . . . . .
O1 O 0.3215(3) 0.7407(3) 0.5759(3) 0.0270(12) Uani 1 1 d . . . . .
O2 O 0.2181(3) 0.5574(3) 0.5539(3) 0.0258(12) Uani 1 1 d . . . . .
O3 O 0.0558(3) 0.6982(2) 0.5437(3) 0.0246(11) Uani 1 1 d . . . . .
O4 O 0.3518(4) 0.9969(3) 0.7531(4) 0.0444(16) Uani 1 1 d . . . . .
O5 O 0.2330(3) 0.8106(3) 0.7126(3) 0.0298(12) Uani 1 1 d . . . . .
O6 O 0.0140(3) 0.5203(2) 0.5780(3) 0.0223(11) Uani 1 1 d . . . . .
O7 O 0.3879(4) 0.6930(3) 0.7165(3) 0.0431(15) Uani 1 1 d . . . . .
O8 O 0.1995(3) 0.5674(3) 0.7338(3) 0.0334(12) Uani 1 1 d . . . . .
O9 O 0.1270(3) 0.3698(3) 0.6004(3) 0.0302(12) Uani 1 1 d . . . . .
O10 O 0.3589(6) 0.9216(6) 1.0999(6) 0.090(3) Uani 1 1 d . . . . .
O11 O -0.1099(5) 0.7430(5) 0.8643(5) 0.080(2) Uani 1 1 d . . . . .
N1 N 0.1671(3) 0.3678(3) 0.4607(3) 0.0219(13) Uani 1 1 d . . . . .
N2 N 0.0287(4) 0.6628(3) 0.6975(3) 0.0282(15) Uani 1 1 d . . . . .
N3 N 0.5799(5) 0.7722(4) 0.7807(5) 0.059(2) Uani 1 1 d . . . . .
N4 N 0.2221(5) 0.5238(4) 0.8446(4) 0.0437(18) Uani 1 1 d . . . . .
N5 N 0.2488(4) 0.3379(4) 0.6982(4) 0.0418(18) Uani 1 1 d . . . . .
N6 N 0.3550(6) 0.9086(6) 0.9766(6) 0.068(3) Uani 1 1 d . . . . .
N7 N -0.0236(5) 0.6912(5) 0.9643(5) 0.065(2) Uani 1 1 d . . . . .
C1 C 0.3892(5) 0.8435(4) 0.6013(5) 0.039(2) Uani 1 1 d . . . . .
H1A H 0.3618 0.8771 0.6386 0.059 Uiso 1 1 calc GR . . . .
H1B H 0.3791 0.8708 0.5572 0.059 Uiso 1 1 calc GR . . . .
H1C H 0.4726 0.8521 0.6253 0.059 Uiso 1 1 calc GR . . . .
C2 C 0.3581(4) 0.6802(4) 0.5324(4) 0.0246(17) Uani 1 1 d . . . . .
C3 C 0.4399(4) 0.7097(4) 0.4976(4) 0.0275(17) Uani 1 1 d . . . . .
H3 H 0.4790 0.7772 0.5068 0.033 Uiso 1 1 calc R . . . .
C4 C 0.4656(4) 0.6436(4) 0.4503(5) 0.033(2) Uani 1 1 d . . . . .
C5 C 0.4054(5) 0.5442(4) 0.4348(5) 0.033(2) Uani 1 1 d . . . . .
H5 H 0.4212 0.4980 0.4009 0.040 Uiso 1 1 calc R . . . .
C6 C 0.3213(4) 0.5120(4) 0.4694(4) 0.0244(17) Uani 1 1 d . . . . .
C7 C 0.2969(4) 0.5794(4) 0.5190(4) 0.0240(17) Uani 1 1 d . . . . .
C8 C 0.5516(5) 0.6754(4) 0.4095(5) 0.0340(19) Uani 1 1 d D . . . .
H8A H 0.6327 0.6925 0.4456 0.041 Uiso 1 1 calc R . . . .
H8B H 0.5389 0.6201 0.3663 0.041 Uiso 1 1 calc R . . . .
C9 C 0.5398(5) 0.7610(5) 0.3794(5) 0.037(2) Uani 1 1 d D . . . .
H9 H 0.4700 0.7505 0.3380 0.045 Uiso 1 1 calc R . . . .
C10 C 0.6155(7) 0.8472(5) 0.4043(6) 0.059(3) Uani 1 1 d D . . . .
H10A H 0.6866 0.8612 0.4455 0.071 Uiso 1 1 calc R . . . .
H10B H 0.6003 0.8969 0.3815 0.071 Uiso 1 1 calc R . . . .
C11 C 0.2600(4) 0.4077(4) 0.4464(4) 0.0257(17) Uani 1 1 d . . . . .
H11 H 0.2906 0.3666 0.4192 0.031 Uiso 1 1 calc R . . . .
C12 C 0.1120(4) 0.2650(4) 0.4404(4) 0.0254(17) Uani 1 1 d . . . . .
C13 C 0.1655(5) 0.1963(4) 0.4228(4) 0.0266(17) Uani 1 1 d . . . . .
H13 H 0.2423 0.2176 0.4201 0.032 Uiso 1 1 calc R . . . .
C14 C 0.1091(5) 0.0986(4) 0.4093(4) 0.0270(17) Uani 1 1 d . . . . .
C15 C -0.0050(5) 0.0693(4) 0.4114(4) 0.0337(19) Uani 1 1 d . . . . .
H15 H -0.0454 0.0020 0.4019 0.040 Uiso 1 1 calc R . . . .
C16 C -0.0602(5) 0.1354(4) 0.4270(4) 0.0307(18) Uani 1 1 d . . . . .
H16 H -0.1381 0.1132 0.4277 0.037 Uiso 1 1 calc R . . . .
C17 C -0.0028(4) 0.2356(4) 0.4418(4) 0.0249(17) Uani 1 1 d . . . . .
C18 C 0.1693(5) 0.0276(4) 0.3929(5) 0.036(2) Uani 1 1 d . . . . .
C19 C 0.2468(6) 0.0428(5) 0.3536(6) 0.049(3) Uani 1 1 d . . . . .
H19 H 0.2583 0.0973 0.3331 0.059 Uiso 1 1 calc R . . . .
C20 C 0.3088(6) -0.0219(5) 0.3437(8) 0.074(4) Uani 1 1 d . . . . .
H20 H 0.3632 -0.0102 0.3173 0.089 Uiso 1 1 calc R . . . .
C21 C 0.2921(7) -0.1014(5) 0.3715(8) 0.076(4) Uani 1 1 d . . . . .
H21 H 0.3336 -0.1454 0.3638 0.091 Uiso 1 1 calc R . . . .
C22 C 0.2144(6) -0.1172(5) 0.4107(6) 0.055(3) Uani 1 1 d . . . . .
H22 H 0.2029 -0.1724 0.4304 0.066 Uiso 1 1 calc R . . . .
C23 C 0.1526(5) -0.0535(4) 0.4219(5) 0.043(2) Uani 1 1 d . . . . .
H23 H 0.0993 -0.0652 0.4491 0.051 Uiso 1 1 calc R . . . .
C24 C 0.4174(6) 1.0975(5) 0.7777(6) 0.053(3) Uani 1 1 d . . . . .
H24A H 0.3714 1.1328 0.7504 0.079 Uiso 1 1 calc GR . . . .
H24B H 0.4910 1.1074 0.7668 0.079 Uiso 1 1 calc GR . . . .
H24C H 0.4353 1.1217 0.8329 0.079 Uiso 1 1 calc GR . . . .
C25 C 0.2447(5) 0.9722(4) 0.7639(5) 0.042(2) Uani 1 1 d . . . . .
C26 C 0.1937(6) 1.0358(4) 0.7909(5) 0.040(2) Uani 1 1 d . . . . .
H26 H 0.2341 1.1037 0.8038 0.048 Uiso 1 1 calc R . . . .
C27 C 0.0847(6) 1.0046(5) 0.8001(5) 0.042(2) Uani 1 1 d D . . . .
C28 C 0.0280(6) 0.9063(5) 0.7812(5) 0.041(2) Uani 1 1 d . . . . .
H28 H -0.0454 0.8840 0.7885 0.050 Uiso 1 1 calc R . . . .
C29 C 0.0735(5) 0.8375(4) 0.7517(4) 0.0301(18) Uani 1 1 d . . . . .
C30 C 0.1833(5) 0.8699(4) 0.7422(4) 0.0311(18) Uani 1 1 d . . . . .
C31_a C 0.030(3) 1.079(2) 0.8244(17) 0.073(2) Uiso 0.5 1 d D U P A 1
H31A_a H 0.0847 1.1450 0.8339 0.087 Uiso 0.5 1 calc R . P A 1
H31B_a H -0.0431 1.0701 0.7821 0.087 Uiso 0.5 1 calc R . P A 1
C32_a C 0.0013(15) 1.0707(17) 0.8934(12) 0.073(2) Uiso 0.5 1 d D U P A 1
H32_a H 0.0594 1.0664 0.9362 0.087 Uiso 0.5 1 calc R . P A 1
C33_a C -0.1012(13) 1.0692(13) 0.8985(14) 0.073(2) Uiso 0.5 1 d D U P A 1
H33A_a H -0.1605 1.0734 0.8563 0.087 Uiso 0.5 1 calc R . P A 1
H33B_a H -0.1163 1.0638 0.9445 0.087 Uiso 0.5 1 calc R . P A 1
C34 C 0.0046(5) 0.7359(4) 0.7310(4) 0.0316(19) Uani 1 1 d . . . . .
H34 H -0.0655 0.7208 0.7430 0.038 Uiso 1 1 calc R . . . .
C35 C -0.0454(4) 0.5650(4) 0.6852(4) 0.0257(18) Uani 1 1 d . . . . .
C36 C -0.1062(4) 0.5402(4) 0.7354(4) 0.0232(16) Uani 1 1 d . . . . .
H36 H -0.1045 0.5896 0.7759 0.028 Uiso 1 1 calc R . . . .
C37 C -0.1685(4) 0.4434(4) 0.7254(4) 0.0250(17) Uani 1 1 d . . . . .
C38 C -0.1701(4) 0.3740(4) 0.6650(4) 0.0270(18) Uani 1 1 d . . . . .
H38 H -0.2142 0.3079 0.6569 0.032 Uiso 1 1 calc R . . . .
C39 C -0.1092(4) 0.3974(4) 0.6155(4) 0.0249(17) Uani 1 1 d . . . . .
H39 H -0.1112 0.3476 0.5751 0.030 Uiso 1 1 calc R . . . .
C40 C -0.0456(4) 0.4943(4) 0.6256(4) 0.0219(17) Uani 1 1 d . . . . .
C41 C -0.2301(5) 0.4147(4) 0.7781(4) 0.0320(18) Uani 1 1 d . . . . .
C42 C -0.2827(5) 0.4732(5) 0.8120(5) 0.044(2) Uani 1 1 d . . . . .
H42 H -0.2775 0.5346 0.8020 0.053 Uiso 1 1 calc R . . . .
C43 C -0.3427(6) 0.4442(6) 0.8601(6) 0.056(3) Uani 1 1 d . . . . .
H43 H -0.3776 0.4857 0.8827 0.067 Uiso 1 1 calc R . . . .
C44 C -0.3515(6) 0.3546(6) 0.8751(5) 0.054(3) Uani 1 1 d . . . . .
H44 H -0.3940 0.3339 0.9070 0.064 Uiso 1 1 calc R . . . .
C45 C -0.2981(6) 0.2956(6) 0.8433(5) 0.045(2) Uani 1 1 d . . . . .
H45 H -0.3031 0.2346 0.8543 0.054 Uiso 1 1 calc R . . . .
C46 C -0.2370(5) 0.3248(5) 0.7954(5) 0.038(2) Uani 1 1 d . . . . .
H46 H -0.2000 0.2840 0.7742 0.045 Uiso 1 1 calc R . . . .
C47 C 0.4678(6) 0.7664(6) 0.7550(5) 0.043(2) Uani 1 1 d . . . . .
H47 H 0.4492 0.8241 0.7678 0.052 Uiso 1 1 calc R . . . .
C49 C 0.6731(6) 0.8561(6) 0.8260(7) 0.068(3) Uani 1 1 d . . . . .
H49A H 0.6437 0.9111 0.8332 0.102 Uiso 1 1 calc GR . . . .
H49B H 0.7315 0.8698 0.8006 0.102 Uiso 1 1 calc GR . . . .
H49C H 0.7096 0.8465 0.8759 0.102 Uiso 1 1 calc GR . . . .
C50 C 0.2519(5) 0.5795(5) 0.8018(5) 0.038(2) Uani 1 1 d . . . . .
H50 H 0.3210 0.6347 0.8260 0.046 Uiso 1 1 calc R . . . .
C51 C 0.1169(6) 0.4389(5) 0.8128(5) 0.046(2) Uani 1 1 d . . . . .
H51A H 0.0625 0.4461 0.8403 0.069 Uiso 1 1 calc GR . . . .
H51B H 0.1380 0.3806 0.8184 0.069 Uiso 1 1 calc GR . . . .
H51C H 0.0790 0.4325 0.7584 0.069 Uiso 1 1 calc GR . . . .
C52 C 0.2907(8) 0.5454(7) 0.9259(6) 0.083(4) Uani 1 1 d . . . . .
H52A H 0.3564 0.6062 0.9409 0.124 Uiso 1 1 calc GR . . . .
H52B H 0.3214 0.4923 0.9346 0.124 Uiso 1 1 calc GR . . . .
H52C H 0.2403 0.5521 0.9565 0.124 Uiso 1 1 calc GR . . . .
C53 C 0.2239(5) 0.3926(4) 0.6516(4) 0.0325(18) Uani 1 1 d . . . . .
H53 H 0.2827 0.4518 0.6577 0.039 Uiso 1 1 calc R . . . .
C54 C 0.3604(6) 0.3679(6) 0.7599(5) 0.059(3) Uani 1 1 d . . . . .
H54A H 0.4042 0.3241 0.7495 0.089 Uiso 1 1 calc GR . . . .
H54B H 0.3464 0.3653 0.8082 0.089 Uiso 1 1 calc GR . . . .
H54C H 0.4060 0.4346 0.7639 0.089 Uiso 1 1 calc GR . . . .
C55 C 0.1642(7) 0.2437(5) 0.6869(6) 0.068(3) Uani 1 1 d . . . . .
H55A H 0.0894 0.2363 0.6482 0.101 Uiso 1 1 calc GR . . . .
H55B H 0.1520 0.2390 0.7353 0.101 Uiso 1 1 calc GR . . . .
H55C H 0.1941 0.1921 0.6694 0.101 Uiso 1 1 calc GR . . . .
C56 C 0.3819(8) 0.8867(7) 1.0444(7) 0.067(3) Uani 1 1 d . . . . .
H56 H 0.4218 0.8405 1.0495 0.080 Uiso 1 1 calc R . . . .
C57 C 0.2958(9) 0.9795(8) 0.9659(8) 0.089(4) Uani 1 1 d . . . . .
H57A H 0.2605 0.9892 1.0057 0.134 Uiso 1 1 calc GR . . . .
H57B H 0.2340 0.9560 0.9154 0.134 Uiso 1 1 calc GR . . . .
H57C H 0.3526 1.0414 0.9695 0.134 Uiso 1 1 calc GR . . . .
C58 C 0.3869(11) 0.8632(9) 0.9147(9) 0.106(5) Uani 1 1 d . . . . .
H58A H 0.4414 0.8292 0.9342 0.159 Uiso 1 1 calc GR . . . .
H58B H 0.4249 0.9132 0.8935 0.159 Uiso 1 1 calc GR . . . .
H58C H 0.3160 0.8165 0.8744 0.159 Uiso 1 1 calc GR . . . .
C59 C -0.1090(7) 0.7150(6) 0.9235(7) 0.065(3) Uani 1 1 d . . . . .
H59 H -0.1751 0.7109 0.9395 0.078 Uiso 1 1 calc R . . . .
C60 C 0.0839(8) 0.7068(10) 0.9470(10) 0.129(6) Uani 1 1 d . . . . .
H60A H 0.0711 0.7201 0.8968 0.194 Uiso 1 1 calc GR . . . .
H60B H 0.1073 0.6485 0.9461 0.194 Uiso 1 1 calc GR . . . .
H60C H 0.1462 0.7624 0.9863 0.194 Uiso 1 1 calc GR . . . .
C61 C -0.0310(10) 0.6543(12) 1.0268(11) 0.152(8) Uani 1 1 d . . . . .
H61A H -0.1082 0.6481 1.0317 0.229 Uiso 1 1 calc GR . . . .
H61B H 0.0308 0.6988 1.0737 0.229 Uiso 1 1 calc GR . . . .
H61C H -0.0206 0.5903 1.0187 0.229 Uiso 1 1 calc GR . . . .
C33A_b C -0.0574(15) 1.0625(13) 0.9382(12) 0.073(2) Uiso 0.5 1 d D U P A 2
H33C_b H -0.1330 1.0526 0.9031 0.087 Uiso 0.5 1 calc R . P A 2
H33D_b H -0.0476 1.0628 0.9900 0.087 Uiso 0.5 1 calc R . P A 2
C32A_b C 0.0352(15) 1.0759(17) 0.9148(13) 0.073(2) Uiso 0.5 1 d D U P A 2
H32A_b H 0.1089 1.0855 0.9520 0.087 Uiso 0.5 1 calc R . P A 2
C31A_b C 0.034(3) 1.077(2) 0.8356(16) 0.073(2) Uiso 0.5 1 d D U P A 2
H31C_b H 0.0799 1.1436 0.8370 0.087 Uiso 0.5 1 calc R . P A 2
H31D_b H -0.0479 1.0632 0.8021 0.087 Uiso 0.5 1 calc R . P A 2
Cl1 Cl 0.6307(2) 0.7094(2) 1.0150(2) 0.0781(10) Uani 1 1 d . . . . .
O12 O 0.7204(9) 0.6966(8) 1.0718(10) 0.202(8) Uani 1 1 d . . . . .
C48 C 0.6083(8) 0.6861(7) 0.7645(10) 0.140(8) Uani 1 1 d . . . . .
H48A H 0.6467 0.6731 0.8126 0.210 Uiso 1 1 calc GR . . . .
H48B H 0.6618 0.6941 0.7351 0.210 Uiso 1 1 calc GR . . . .
H48C H 0.5363 0.6314 0.7345 0.210 Uiso 1 1 calc GR . . . .
O13 O 0.5465(8) 0.7390(7) 1.0360(9) 0.170(7) Uani 1 1 d . . . . .
O14 O 0.6981(11) 0.7973(8) 1.0042(9) 0.182(6) Uani 1 1 d . . . . .
O15 O 0.5899(10) 0.6319(9) 0.9587(14) 0.332(17) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.566(4) . ?
Dy1 O2 2.293(5) . ?
Dy1 O3 2.369(3) . ?
Dy1 O5 2.163(4) . ?
Dy1 O6 2.420(3) . ?
Dy1 O7 2.392(4) . ?
Dy1 O8 2.389(4) . ?
Dy1 N2 2.456(5) . ?
Ni1 O2 2.034(3) . ?
Ni1 O3 2.065(4) 2_566 ?
Ni1 O6 2.080(4) . ?
Ni1 O6 2.129(3) 2_566 ?
Ni1 O9 2.053(4) . ?
Ni1 N1 2.003(5) . ?
O1 C1 1.450(6) . ?
O1 C2 1.360(8) . ?
O2 C7 1.338(7) . ?
O3 Ni1 2.065(4) 2_566 ?
O3 C17 1.350(6) 2_566 ?
O4 C24 1.417(7) . ?
O4 C25 1.379(8) . ?
O5 C30 1.332(8) . ?
O6 Ni1 2.129(3) 2_566 ?
O6 C40 1.364(7) . ?
O7 C47 1.206(8) . ?
O8 C50 1.225(9) . ?
O9 C53 1.240(7) . ?
O10 C56 1.226(13) . ?
O11 C59 1.258(13) . ?
N1 C11 1.285(7) . ?
N1 C12 1.425(6) . ?
N2 C34 1.300(9) . ?
N2 C35 1.438(6) . ?
N3 C47 1.328(8) . ?
N3 C49 1.393(10) . ?
N3 C48 1.415(10) . ?
N4 C50 1.310(9) . ?
N4 C51 1.450(8) . ?
N4 C52 1.464(11) . ?
N5 C53 1.328(7) . ?
N5 C54 1.447(8) . ?
N5 C55 1.452(8) . ?
N6 C56 1.349(13) . ?
N6 C57 1.446(10) . ?
N6 C58 1.449(16) . ?
N7 C59 1.303(10) . ?
N7 C60 1.445(13) . ?
N7 C61 1.400(15) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.386(9) . ?
C2 C7 1.427(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.368(10) . ?
C4 C5 1.401(7) . ?
C4 C8 1.517(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.414(9) . ?
C6 C7 1.395(10) . ?
C6 C11 1.454(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.503(7) . ?
C9 H9 0.9500 . ?
C9 C10 1.285(8) . ?
C10 H10A 0.9500 . ?
C10 H10B 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.397(8) . ?
C12 C17 1.401(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.375(7) . ?
C14 C15 1.397(8) . ?
C14 C18 1.482(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.374(8) . ?
C16 H16 0.9500 . ?
C16 C17 1.405(7) . ?
C17 O3 1.350(6) 2_566 ?
C18 C19 1.377(11) . ?
C18 C23 1.397(8) . ?
C19 H19 0.9500 . ?
C19 C20 1.400(9) . ?
C20 H20 0.9500 . ?
C20 C21 1.361(11) . ?
C21 H21 0.9500 . ?
C21 C22 1.378(14) . ?
C22 H22 0.9500 . ?
C22 C23 1.391(9) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.371(10) . ?
C25 C30 1.429(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.393(10) . ?
C27 C28 1.372(9) . ?
C27 C31_a 1.512(13) . ?
C27 C31A_b 1.530(13) . ?
C28 H28 0.9500 . ?
C28 C29 1.396(10) . ?
C29 C30 1.408(9) . ?
C29 C34 1.443(8) . ?
C31_a H31A_a 0.9900 . ?
C31_a H31B_a 0.9900 . ?
C31_a C32_a 1.460(18) . ?
C32_a H32_a 0.9500 . ?
C32_a C33_a 1.312(12) . ?
C33_a H33A_a 0.9500 . ?
C33_a H33B_a 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.413(9) . ?
C35 C40 1.391(10) . ?
C36 H36 0.9500 . ?
C36 C37 1.391(7) . ?
C37 C38 1.383(10) . ?
C37 C41 1.475(9) . ?
C38 H38 0.9500 . ?
C38 C39 1.397(9) . ?
C39 H39 0.9500 . ?
C39 C40 1.396(7) . ?
C41 C42 1.389(11) . ?
C41 C46 1.411(7) . ?
C42 H42 0.9500 . ?
C42 C43 1.388(12) . ?
C43 H43 0.9500 . ?
C43 C44 1.387(10) . ?
C44 H44 0.9500 . ?
C44 C45 1.382(12) . ?
C45 H45 0.9500 . ?
C45 C46 1.396(10) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50 0.9500 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53 0.9500 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59 0.9500 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C33A_b H33C_b 0.9500 . ?
C33A_b H33D_b 0.9500 . ?
C33A_b C32A_b 1.334(16) . ?
C32A_b H32A_b 0.9500 . ?
C32A_b C31A_b 1.496(18) . ?
C31A_b H31C_b 0.9900 . ?
C31A_b H31D_b 0.9900 . ?
Cl1 O12 1.400(10) . ?
Cl1 O13 1.369(10) . ?
Cl1 O14 1.436(9) . ?
Cl1 O15 1.289(15) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O1 63.90(12) . . ?
O2 Dy1 O3 88.86(14) . . ?
O2 Dy1 O6 68.59(13) . . ?
O2 Dy1 O7 84.36(17) . . ?
O2 Dy1 O8 94.82(15) . . ?
O2 Dy1 N2 136.38(15) . . ?
O3 Dy1 O1 77.21(12) . . ?
O3 Dy1 O6 70.78(11) . . ?
O3 Dy1 O7 145.41(14) . . ?
O3 Dy1 O8 144.67(12) . . ?
O3 Dy1 N2 80.99(15) . . ?
O5 Dy1 O1 84.51(16) . . ?
O5 Dy1 O2 148.01(14) . . ?
O5 Dy1 O3 88.86(14) . . ?
O5 Dy1 O6 139.41(14) . . ?
O5 Dy1 O7 79.62(15) . . ?
O5 Dy1 O8 105.19(17) . . ?
O5 Dy1 N2 74.51(16) . . ?
O6 Dy1 O1 122.21(15) . . ?
O6 Dy1 N2 68.00(16) . . ?
O7 Dy1 O1 69.35(15) . . ?
O7 Dy1 O6 135.69(12) . . ?
O7 Dy1 N2 125.72(19) . . ?
O8 Dy1 O1 135.34(12) . . ?
O8 Dy1 O6 77.95(13) . . ?
O8 Dy1 O7 69.84(14) . . ?
O8 Dy1 N2 72.21(13) . . ?
N2 Dy1 O1 149.91(12) . . ?
O2 Ni1 O3 170.14(19) . 2_566 ?
O2 Ni1 O6 93.36(13) . 2_566 ?
O2 Ni1 O6 80.47(16) . . ?
O2 Ni1 O9 98.20(15) . . ?
O3 Ni1 O6 107.96(14) 2_566 . ?
O3 Ni1 O6 82.78(13) 2_566 2_566 ?
O6 Ni1 O6 83.40(18) . 2_566 ?
O9 Ni1 O3 86.85(15) . 2_566 ?
O9 Ni1 O6 91.68(17) . . ?
O9 Ni1 O6 166.53(14) . 2_566 ?
N1 Ni1 O2 89.23(18) . . ?
N1 Ni1 O3 82.46(17) . 2_566 ?
N1 Ni1 O6 169.54(16) . . ?
N1 Ni1 O6 99.13(18) . 2_566 ?
N1 Ni1 O9 87.97(18) . . ?
C1 O1 Dy1 122.0(4) . . ?
C2 O1 Dy1 117.0(3) . . ?
C2 O1 C1 117.7(4) . . ?
Ni1 O2 Dy1 107.86(17) . . ?
C7 O2 Dy1 126.8(3) . . ?
C7 O2 Ni1 123.4(4) . . ?
Ni1 O3 Dy1 104.82(12) 2_566 . ?
C17 O3 Dy1 121.5(4) 2_566 . ?
C17 O3 Ni1 106.1(3) 2_566 2_566 ?
C25 O4 C24 115.8(6) . . ?
C30 O5 Dy1 140.0(4) . . ?
Ni1 O6 Dy1 101.91(13) . . ?
Ni1 O6 Dy1 101.11(11) 2_566 . ?
Ni1 O6 Ni1 96.60(18) . 2_566 ?
C40 O6 Dy1 111.5(4) . . ?
C40 O6 Ni1 126.7(3) . . ?
C40 O6 Ni1 115.3(3) . 2_566 ?
C47 O7 Dy1 132.7(4) . . ?
C50 O8 Dy1 137.7(4) . . ?
C53 O9 Ni1 129.0(3) . . ?
C11 N1 Ni1 128.3(4) . . ?
C11 N1 C12 122.7(5) . . ?
C12 N1 Ni1 109.0(3) . . ?
C34 N2 Dy1 129.4(4) . . ?
C34 N2 C35 119.9(5) . . ?
C35 N2 Dy1 110.8(4) . . ?
C47 N3 C49 125.3(7) . . ?
C47 N3 C48 118.3(7) . . ?
C49 N3 C48 116.4(6) . . ?
C50 N4 C51 120.6(7) . . ?
C50 N4 C52 122.0(7) . . ?
C51 N4 C52 117.4(6) . . ?
C53 N5 C54 122.0(6) . . ?
C53 N5 C55 120.0(6) . . ?
C54 N5 C55 117.9(5) . . ?
C56 N6 C57 119.9(11) . . ?
C56 N6 C58 120.7(8) . . ?
C57 N6 C58 119.5(9) . . ?
C59 N7 C60 119.4(9) . . ?
C59 N7 C61 121.8(9) . . ?
C61 N7 C60 118.7(8) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 125.2(5) . . ?
O1 C2 C7 114.0(5) . . ?
C3 C2 C7 120.6(6) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 C2 121.4(5) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 119.3(6) . . ?
C3 C4 C8 121.7(5) . . ?
C5 C4 C8 118.9(6) . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.5(6) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C11 115.8(6) . . ?
C7 C6 C5 120.2(5) . . ?
C7 C6 C11 123.9(5) . . ?
O2 C7 C2 116.7(6) . . ?
O2 C7 C6 125.3(5) . . ?
C6 C7 C2 118.0(5) . . ?
C4 C8 H8A 108.9 . . ?
C4 C8 H8B 108.9 . . ?
H8A C8 H8B 107.8 . . ?
C9 C8 C4 113.2(5) . . ?
C9 C8 H8A 108.9 . . ?
C9 C8 H8B 108.9 . . ?
C8 C9 H9 117.0 . . ?
C10 C9 C8 126.0(7) . . ?
C10 C9 H9 117.0 . . ?
C9 C10 H10A 120.0 . . ?
C9 C10 H10B 120.0 . . ?
H10A C10 H10B 120.0 . . ?
N1 C11 C6 124.1(6) . . ?
N1 C11 H11 118.0 . . ?
C6 C11 H11 118.0 . . ?
C13 C12 N1 124.9(5) . . ?
C13 C12 C17 120.7(5) . . ?
C17 C12 N1 114.4(5) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 C12 121.1(5) . . ?
C14 C13 H13 119.4 . . ?
C13 C14 C15 118.2(5) . . ?
C13 C14 C18 120.0(5) . . ?
C15 C14 C18 121.9(5) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 C14 121.6(5) . . ?
C16 C15 H15 119.2 . . ?
C15 C16 H16 119.6 . . ?
C15 C16 C17 120.7(5) . . ?
C17 C16 H16 119.6 . . ?
O3 C17 C12 120.6(4) 2_566 . ?
O3 C17 C16 121.7(5) 2_566 . ?
C12 C17 C16 117.6(5) . . ?
C19 C18 C14 121.5(5) . . ?
C19 C18 C23 119.1(6) . . ?
C23 C18 C14 119.4(7) . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.2(7) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 119.6 . . ?
C21 C20 C19 120.8(9) . . ?
C21 C20 H20 119.6 . . ?
C20 C21 H21 120.3 . . ?
C20 C21 C22 119.4(7) . . ?
C22 C21 H21 120.3 . . ?
C21 C22 H22 119.5 . . ?
C21 C22 C23 120.9(7) . . ?
C23 C22 H22 119.5 . . ?
C18 C23 H23 120.2 . . ?
C22 C23 C18 119.6(8) . . ?
C22 C23 H23 120.2 . . ?
O4 C24 H24A 109.5 . . ?
O4 C24 H24B 109.5 . . ?
O4 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O4 C25 C30 114.4(6) . . ?
C26 C25 O4 126.2(5) . . ?
C26 C25 C30 119.4(6) . . ?
C25 C26 H26 118.8 . . ?
C25 C26 C27 122.5(6) . . ?
C27 C26 H26 118.8 . . ?
C26 C27 C31_a 119.5(15) . . ?
C26 C27 C31A_b 121.1(16) . . ?
C28 C27 C26 117.8(6) . . ?
C28 C27 C31_a 122.6(16) . . ?
C28 C27 C31A_b 121.0(15) . . ?
C27 C28 H28 118.6 . . ?
C27 C28 C29 122.8(6) . . ?
C29 C28 H28 118.6 . . ?
C28 C29 C30 118.9(5) . . ?
C28 C29 C34 118.3(6) . . ?
C30 C29 C34 122.7(6) . . ?
O5 C30 C25 117.7(6) . . ?
O5 C30 C29 123.7(5) . . ?
C29 C30 C25 118.6(6) . . ?
C27 C31_a H31A_a 109.1 . . ?
C27 C31_a H31B_a 109.1 . . ?
H31A_a C31_a H31B_a 107.9 . . ?
C32_a C31_a C27 112.4(15) . . ?
C32_a C31_a H31A_a 109.1 . . ?
C32_a C31_a H31B_a 109.1 . . ?
C31_a C32_a H32_a 118.7 . . ?
C33_a C32_a C31_a 123(2) . . ?
C33_a C32_a H32_a 118.7 . . ?
C32_a C33_a H33A_a 120.0 . . ?
C32_a C33_a H33B_a 120.0 . . ?
H33A_a C33_a H33B_a 120.0 . . ?
N2 C34 C29 126.7(6) . . ?
N2 C34 H34 116.6 . . ?
C29 C34 H34 116.6 . . ?
C36 C35 N2 121.7(7) . . ?
C40 C35 N2 116.6(5) . . ?
C40 C35 C36 121.5(5) . . ?
C35 C36 H36 120.1 . . ?
C37 C36 C35 119.9(7) . . ?
C37 C36 H36 120.1 . . ?
C36 C37 C41 121.3(7) . . ?
C38 C37 C36 118.2(5) . . ?
C38 C37 C41 120.6(5) . . ?
C37 C38 H38 118.7 . . ?
C37 C38 C39 122.6(5) . . ?
C39 C38 H38 118.7 . . ?
C38 C39 H39 120.2 . . ?
C40 C39 C38 119.6(7) . . ?
C40 C39 H39 120.2 . . ?
O6 C40 C35 120.2(5) . . ?
O6 C40 C39 121.4(6) . . ?
C35 C40 C39 118.3(5) . . ?
C42 C41 C37 122.3(5) . . ?
C42 C41 C46 117.9(6) . . ?
C46 C41 C37 119.8(6) . . ?
C41 C42 H42 119.2 . . ?
C43 C42 C41 121.6(7) . . ?
C43 C42 H42 119.2 . . ?
C42 C43 H43 120.0 . . ?
C44 C43 C42 119.9(8) . . ?
C44 C43 H43 120.0 . . ?
C43 C44 H44 120.1 . . ?
C45 C44 C43 119.8(7) . . ?
C45 C44 H44 120.1 . . ?
C44 C45 H45 119.8 . . ?
C44 C45 C46 120.5(7) . . ?
C46 C45 H45 119.8 . . ?
C41 C46 H46 119.9 . . ?
C45 C46 C41 120.3(7) . . ?
C45 C46 H46 119.9 . . ?
O7 C47 N3 124.5(7) . . ?
O7 C47 H47 117.7 . . ?
N3 C47 H47 117.7 . . ?
N3 C49 H49A 109.5 . . ?
N3 C49 H49B 109.5 . . ?
N3 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O8 C50 N4 126.4(7) . . ?
O8 C50 H50 116.8 . . ?
N4 C50 H50 116.8 . . ?
N4 C51 H51A 109.5 . . ?
N4 C51 H51B 109.5 . . ?
N4 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N4 C52 H52A 109.5 . . ?
N4 C52 H52B 109.5 . . ?
N4 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O9 C53 N5 122.8(5) . . ?
O9 C53 H53 118.6 . . ?
N5 C53 H53 118.6 . . ?
N5 C54 H54A 109.5 . . ?
N5 C54 H54B 109.5 . . ?
N5 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N5 C55 H55A 109.5 . . ?
N5 C55 H55B 109.5 . . ?
N5 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
O10 C56 N6 125.2(9) . . ?
O10 C56 H56 117.4 . . ?
N6 C56 H56 117.4 . . ?
N6 C57 H57A 109.5 . . ?
N6 C57 H57B 109.5 . . ?
N6 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
N6 C58 H58A 109.5 . . ?
N6 C58 H58B 109.5 . . ?
N6 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
O11 C59 N7 124.4(10) . . ?
O11 C59 H59 117.8 . . ?
N7 C59 H59 117.8 . . ?
N7 C60 H60A 109.5 . . ?
N7 C60 H60B 109.5 . . ?
N7 C60 H60C 109.5 . . ?
H60A C60 H60B 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
N7 C61 H61A 109.5 . . ?
N7 C61 H61B 109.5 . . ?
N7 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
H33C_b C33A_b H33D_b 120.0 . . ?
C32A_b C33A_b H33C_b 120.0 . . ?
C32A_b C33A_b H33D_b 120.0 . . ?
C33A_b C32A_b H32A_b 116.8 . . ?
C33A_b C32A_b C31A_b 126(2) . . ?
C31A_b C32A_b H32A_b 116.8 . . ?
C27 C31A_b H31C_b 108.7 . . ?
C27 C31A_b H31D_b 108.7 . . ?
C32A_b C31A_b C27 114.3(16) . . ?
C32A_b C31A_b H31C_b 108.7 . . ?
C32A_b C31A_b H31D_b 108.7 . . ?
H31C_b C31A_b H31D_b 107.6 . . ?
O12 Cl1 O14 98.5(7) . . ?
O13 Cl1 O12 118.2(11) . . ?
O13 Cl1 O14 100.9(7) . . ?
O15 Cl1 O12 106.6(11) . . ?
O15 Cl1 O13 114.5(8) . . ?
O15 Cl1 O14 117.5(14) . . ?
N3 C48 H48A 109.5 . . ?
N3 C48 H48B 109.5 . . ?
N3 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O1 C2 C3 -173.3(4) . . . . ?
Dy1 O1 C2 C7 11.8(6) . . . . ?
Dy1 O2 C7 C2 -7.9(6) . . . . ?
Dy1 O2 C7 C6 173.9(4) . . . . ?
Dy1 O5 C30 C25 -160.6(5) . . . . ?
Dy1 O5 C30 C29 18.1(10) . . . . ?
Dy1 O6 C40 C35 31.4(5) . . . . ?
Dy1 O6 C40 C39 -149.5(4) . . . . ?
Dy1 O7 C47 N3 -167.7(6) . . . . ?
Dy1 O8 C50 N4 159.3(5) . . . . ?
Dy1 N2 C34 C29 -6.4(10) . . . . ?
Dy1 N2 C35 C36 151.7(4) . . . . ?
Dy1 N2 C35 C40 -22.5(5) . . . . ?
Ni1 O2 C7 C2 154.2(3) . . . . ?
Ni1 O2 C7 C6 -24.1(6) . . . . ?
Ni1 O6 C40 C35 156.2(3) . . . . ?
Ni1 O6 C40 C35 -83.1(5) 2_566 . . . ?
Ni1 O6 C40 C39 -24.7(6) . . . . ?
Ni1 O6 C40 C39 96.0(4) 2_566 . . . ?
Ni1 O9 C53 N5 -170.5(5) . . . . ?
Ni1 N1 C11 C6 2.0(8) . . . . ?
Ni1 N1 C12 C13 -161.1(6) . . . . ?
Ni1 N1 C12 C17 16.6(6) . . . . ?
O1 C2 C3 C4 -175.3(5) . . . . ?
O1 C2 C7 O2 -3.8(7) . . . . ?
O1 C2 C7 C6 174.5(5) . . . . ?
O4 C25 C26 C27 179.9(7) . . . . ?
O4 C25 C30 O5 -1.7(9) . . . . ?
O4 C25 C30 C29 179.5(6) . . . . ?
N1 C12 C13 C14 175.2(6) . . . . ?
N1 C12 C17 O3 4.4(8) . . . 2_566 ?
N1 C12 C17 C16 -176.3(5) . . . . ?
N2 C35 C36 C37 -174.3(4) . . . . ?
N2 C35 C40 O6 -5.7(6) . . . . ?
N2 C35 C40 C39 175.1(4) . . . . ?
C1 O1 C2 C3 -13.5(8) . . . . ?
C1 O1 C2 C7 171.6(5) . . . . ?
C2 C3 C4 C5 1.9(9) . . . . ?
C2 C3 C4 C8 177.6(5) . . . . ?
C3 C2 C7 O2 -179.0(5) . . . . ?
C3 C2 C7 C6 -0.6(7) . . . . ?
C3 C4 C5 C6 -1.8(8) . . . . ?
C3 C4 C8 C9 -40.2(9) . . . . ?
C4 C5 C6 C7 0.4(8) . . . . ?
C4 C5 C6 C11 177.1(5) . . . . ?
C4 C8 C9 C10 111.5(8) . . . . ?
C5 C4 C8 C9 135.4(6) . . . . ?
C5 C6 C7 O2 179.0(5) . . . . ?
C5 C6 C7 C2 0.7(8) . . . . ?
C5 C6 C11 N1 -166.7(5) . . . . ?
C7 C2 C3 C4 -0.8(8) . . . . ?
C7 C6 C11 N1 9.8(9) . . . . ?
C8 C4 C5 C6 -177.6(5) . . . . ?
C11 N1 C12 C13 18.1(9) . . . . ?
C11 N1 C12 C17 -164.1(6) . . . . ?
C11 C6 C7 O2 2.6(8) . . . . ?
C11 C6 C7 C2 -175.6(5) . . . . ?
C12 N1 C11 C6 -177.1(5) . . . . ?
C12 C13 C14 C15 1.8(9) . . . . ?
C12 C13 C14 C18 -178.3(7) . . . . ?
C13 C12 C17 O3 -177.7(6) . . . 2_566 ?
C13 C12 C17 C16 1.6(9) . . . . ?
C13 C14 C15 C16 -0.4(10) . . . . ?
C13 C14 C18 C19 -33.4(11) . . . . ?
C13 C14 C18 C23 142.7(7) . . . . ?
C14 C15 C16 C17 -0.4(11) . . . . ?
C14 C18 C19 C20 175.4(8) . . . . ?
C14 C18 C23 C22 -176.1(7) . . . . ?
C15 C14 C18 C19 146.4(8) . . . . ?
C15 C14 C18 C23 -37.5(10) . . . . ?
C15 C16 C17 O3 179.2(6) . . . 2_566 ?
C15 C16 C17 C12 -0.2(9) . . . . ?
C17 C12 C13 C14 -2.5(10) . . . . ?
C18 C14 C15 C16 179.7(7) . . . . ?
C18 C19 C20 C21 1.1(15) . . . . ?
C19 C18 C23 C22 0.1(12) . . . . ?
C19 C20 C21 C22 -1.0(16) . . . . ?
C20 C21 C22 C23 0.3(15) . . . . ?
C21 C22 C23 C18 0.1(13) . . . . ?
C23 C18 C19 C20 -0.7(13) . . . . ?
C24 O4 C25 C26 4.8(10) . . . . ?
C24 O4 C25 C30 -177.0(6) . . . . ?
C25 C26 C27 C28 0.1(11) . . . . ?
C25 C26 C27 C31_a -175.4(15) . . . . ?
C25 C26 C27 C31A_b 175.7(14) . . . . ?
C26 C25 C30 O5 176.6(7) . . . . ?
C26 C25 C30 C29 -2.2(10) . . . . ?
C26 C27 C28 C29 -1.7(11) . . . . ?
C26 C27 C31_a C32_a -124(2) . . . . ?
C26 C27 C31A_b C32A_b -108(2) . . . . ?
C27 C28 C29 C30 1.3(11) . . . . ?
C27 C28 C29 C34 -177.7(7) . . . . ?
C27 C31_a C32_a C33_a -132(3) . . . . ?
C28 C27 C31_a C32_a 60(3) . . . . ?
C28 C27 C31A_b C32A_b 68(3) . . . . ?
C28 C29 C30 O5 -178.0(7) . . . . ?
C28 C29 C30 C25 0.7(10) . . . . ?
C28 C29 C34 N2 174.4(7) . . . . ?
C30 C25 C26 C27 1.8(12) . . . . ?
C30 C29 C34 N2 -4.6(10) . . . . ?
C31_a C27 C28 C29 173.6(14) . . . . ?
C31_a C27 C31A_b C32A_b 172(24) . . . . ?
C34 N2 C35 C36 -30.3(8) . . . . ?
C34 N2 C35 C40 155.6(5) . . . . ?
C34 C29 C30 O5 0.9(10) . . . . ?
C34 C29 C30 C25 179.6(6) . . . . ?
C35 N2 C34 C29 176.0(6) . . . . ?
C35 C36 C37 C38 -1.0(7) . . . . ?
C35 C36 C37 C41 178.2(5) . . . . ?
C36 C35 C40 O6 -179.9(4) . . . . ?
C36 C35 C40 C39 0.9(7) . . . . ?
C36 C37 C38 C39 1.8(7) . . . . ?
C36 C37 C41 C42 34.2(9) . . . . ?
C36 C37 C41 C46 -146.0(6) . . . . ?
C37 C38 C39 C40 -1.2(7) . . . . ?
C37 C41 C42 C43 178.5(7) . . . . ?
C37 C41 C46 C45 -178.1(6) . . . . ?
C38 C37 C41 C42 -146.6(6) . . . . ?
C38 C37 C41 C46 33.2(8) . . . . ?
C38 C39 C40 O6 -179.4(4) . . . . ?
C38 C39 C40 C35 -0.2(7) . . . . ?
C40 C35 C36 C37 -0.3(7) . . . . ?
C41 C37 C38 C39 -177.4(5) . . . . ?
C41 C42 C43 C44 -0.3(13) . . . . ?
C42 C41 C46 C45 1.8(10) . . . . ?
C42 C43 C44 C45 1.5(13) . . . . ?
C43 C44 C45 C46 -1.0(12) . . . . ?
C44 C45 C46 C41 -0.6(11) . . . . ?
C46 C41 C42 C43 -1.4(11) . . . . ?
C49 N3 C47 O7 -179.2(9) . . . . ?
C51 N4 C50 O8 -1.1(13) . . . . ?
C52 N4 C50 O8 -179.4(8) . . . . ?
C54 N5 C53 O9 -177.0(7) . . . . ?
C55 N5 C53 O9 4.6(12) . . . . ?
C57 N6 C56 O10 0.9(15) . . . . ?
C58 N6 C56 O10 179.7(11) . . . . ?
C60 N7 C59 O11 6.9(17) . . . . ?
C61 N7 C59 O11 -175.6(14) . . . . ?
C33A_b C32A_b C31A_b C27 -124(3) . . . . ?
C31A_b C27 C28 C29 -177.3(14) . . . . ?
C31A_b C27 C31_a C32_a -20(19) . . . . ?
C48 N3 C47 O7 -2.3(15) . . . . ?

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

data_8_CCDC_1406224
_database_code_depnum_ccdc_archive 'CCDC 1406224'
_audit_update_record             
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_audit_creation_date             2015-01-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C100 H78 Br6 Dy2 N4 Ni2 O20, 6(C2 H6 O)'
_chemical_formula_sum            'C112 H114 Br6 Dy2 N4 Ni2 O26'
_chemical_formula_weight         2848.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   20.4620(7)
_cell_length_b                   20.8069(7)
_cell_length_c                   27.3553(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.444(3)
_cell_angle_gamma                90
_cell_volume                     11520.3(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    173
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.754
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22076
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.133
_diffrn_reflns_theta_min         2.530
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9196
_reflns_number_total             12759
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         2.772
_refine_diff_density_min         -3.539
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         12759
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0501
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0805P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1310
_refine_ls_wR_factor_ref         0.1431
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O11-C49
 1.43 with sigma of 0.02
 O12-C51
 1.43 with sigma of 0.02
 C51-C52
 1.54 with sigma of 0.02
 C50-C49
 1.54 with sigma of 0.02
 O10-H10
 0.87 with sigma of 0.01
 C4-H10
 1.877518 with sigma of 0.02
 Ni1-H10
 2.650389 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C4) = Uanis(O10)
4.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C51(H51A,H51B)
4.b Me refined with riding coordinates:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C50(H50A,H50B,H50C), C52(H52A,H52B,
 H52C), C1(H1A,H1B,H1C)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C10(H10A), C12(H12), C13(H13), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C23(H23), C25(H25), C28(H28), C30(H30), C32(H32),
  C33(H33), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C43(H43),
 C45(H45), C48(H48), C4(H4)
4.d Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC)
4.e Idealised tetrahedral OH refined as rotating group:
 O11(H11), O12(H12A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.52523(2) -0.00392(2) 0.61513(2) 0.02335(9) Uani 1 1 d . . . . .
Br1 Br 0.88342(4) 0.03678(4) 0.76476(3) 0.0692(2) Uani 1 1 d . . . . .
Br2 Br 0.29349(3) -0.28567(3) 0.59668(3) 0.05253(19) Uani 1 1 d . . . . .
Br3 Br 0.37934(8) 0.24544(5) 0.78541(4) 0.1192(5) Uani 1 1 d . . . . .
Ni1 Ni 0.42494(3) 0.01673(3) 0.50188(2) 0.02160(15) Uani 1 1 d D . . . .
O1 O 0.6606(2) -0.0934(2) 0.74966(15) 0.0457(11) Uani 1 1 d . . . . .
O2 O 0.60262(18) -0.02150(17) 0.67801(12) 0.0290(8) Uani 1 1 d . . . . .
O3 O 0.51781(17) 0.04800(15) 0.53497(11) 0.0221(7) Uani 1 1 d . . . . .
O4 O 0.48994(18) -0.11922(17) 0.62809(13) 0.0301(8) Uani 1 1 d . . . . .
O5 O 0.43509(17) -0.04026(16) 0.56246(11) 0.0240(7) Uani 1 1 d . . . . .
O6 O 0.40608(18) 0.06000(16) 0.43353(12) 0.0261(8) Uani 1 1 d . . . . .
O7 O 0.4481(3) 0.2106(2) 0.60931(17) 0.0629(15) Uani 1 1 d . . . . .
O8 O 0.46714(19) 0.08775(17) 0.62349(12) 0.0304(8) Uani 1 1 d . . . . .
O9 O 0.4620(2) -0.01527(19) 0.68348(14) 0.0379(10) Uani 1 1 d . . . . .
O10 O 0.3840(3) 0.0937(2) 0.53585(18) 0.0607(10) Uani 1 1 d D . . . .
H10 H 0.4084(9) 0.115(2) 0.5586(16) 0.091 Uiso 1 1 d DR . . . .
O11 O 0.5175(6) 0.3174(4) 0.3154(4) 0.151(4) Uani 1 1 d D . . . .
H11 H 0.4884 0.3243 0.2909 0.226 Uiso 1 1 calc GR . . . .
O12 O 0.0912(6) 0.2189(5) 0.7463(5) 0.165(4) Uani 1 1 d D . . . .
H12A H 0.0860 0.2503 0.7646 0.248 Uiso 1 1 calc GR . . . .
N1 N 0.6102(2) 0.08121(19) 0.61246(14) 0.0253(9) Uani 1 1 d . . . . .
N2 N 0.3336(2) -0.0194(2) 0.48141(14) 0.0236(9) Uani 1 1 d . . . . .
C0AA C 0.6871(4) -0.1266(4) 0.7943(3) 0.076(3) Uani 1 1 d . . . . .
H0AA H 0.7306 -0.1442 0.7909 0.114 Uiso 1 1 calc GR . . . .
H0AB H 0.6573 -0.1618 0.8002 0.114 Uiso 1 1 calc GR . . . .
H0AC H 0.6913 -0.0966 0.8222 0.114 Uiso 1 1 calc GR . . . .
C2 C 0.6979(3) -0.0441(3) 0.7346(2) 0.0352(13) Uani 1 1 d . . . . .
C3 C 0.7614(3) -0.0306(3) 0.7546(2) 0.0462(16) Uani 1 1 d . . . . .
H3 H 0.7829 -0.0554 0.7814 0.055 Uiso 1 1 calc R . . . .
C1AA C 0.7950(3) 0.0200(3) 0.7354(2) 0.0450(15) Uani 1 1 d . . . . .
C5 C 0.7650(3) 0.0571(3) 0.6979(2) 0.0358(13) Uani 1 1 d . . . . .
H5 H 0.7884 0.0916 0.6856 0.043 Uiso 1 1 calc R . . . .
C6 C 0.6980(3) 0.0441(3) 0.67696(18) 0.0290(11) Uani 1 1 d . . . . .
C7 C 0.6631(3) -0.0069(2) 0.69490(19) 0.0275(11) Uani 1 1 d . . . . .
C8 C 0.6691(3) 0.0856(3) 0.63692(18) 0.0289(11) Uani 1 1 d . . . . .
H8 H 0.6961 0.1193 0.6277 0.035 Uiso 1 1 calc R . . . .
C9 C 0.5878(3) 0.1293(2) 0.57566(17) 0.0231(10) Uani 1 1 d . . . . .
C10 C 0.6108(3) 0.1921(2) 0.57827(18) 0.0272(11) Uani 1 1 d . . . . .
H10A H 0.6439 0.2045 0.6047 0.033 Uiso 1 1 calc R . . . .
C11 C 0.5856(3) 0.2380(2) 0.54222(18) 0.0261(11) Uani 1 1 d . . . . .
C12 C 0.5363(3) 0.2177(2) 0.50530(19) 0.0300(12) Uani 1 1 d . . . . .
H12 H 0.5176 0.2478 0.4811 0.036 Uiso 1 1 calc R . . . .
C13 C 0.5133(2) 0.1551(2) 0.50253(17) 0.0251(11) Uani 1 1 d . . . . .
H13 H 0.4797 0.1428 0.4765 0.030 Uiso 1 1 calc R . . . .
C14 C 0.5392(2) 0.1101(2) 0.53765(17) 0.0223(10) Uani 1 1 d . . . . .
C15 C 0.6103(3) 0.3055(2) 0.54422(19) 0.0300(12) Uani 1 1 d . . . . .
C16 C 0.6384(3) 0.3340(3) 0.5876(2) 0.0406(14) Uani 1 1 d . . . . .
H16 H 0.6425 0.3102 0.6176 0.049 Uiso 1 1 calc R . . . .
C17 C 0.6611(3) 0.3976(3) 0.5885(3) 0.0479(16) Uani 1 1 d . . . . .
H17 H 0.6819 0.4161 0.6186 0.057 Uiso 1 1 calc R . . . .
C18 C 0.6532(3) 0.4328(3) 0.5460(3) 0.0478(17) Uani 1 1 d . . . . .
H18 H 0.6672 0.4763 0.5464 0.057 Uiso 1 1 calc R . . . .
C19 C 0.6245(3) 0.4045(3) 0.5024(3) 0.0491(16) Uani 1 1 d . . . . .
H19 H 0.6188 0.4287 0.4727 0.059 Uiso 1 1 calc R . . . .
C20 C 0.6047(3) 0.3430(3) 0.5018(2) 0.0420(14) Uani 1 1 d . . . . .
H20 H 0.5861 0.3244 0.4711 0.050 Uiso 1 1 calc R . . . .
C21 C 0.5174(3) -0.1560(3) 0.6710(2) 0.0467(16) Uani 1 1 d . . . . .
H21A H 0.4863 -0.1561 0.6950 0.070 Uiso 1 1 calc R . . . .
H21B H 0.5592 -0.1367 0.6859 0.070 Uiso 1 1 calc R . . . .
H21C H 0.5251 -0.2003 0.6611 0.070 Uiso 1 1 calc R . . . .
C22 C 0.4291(3) -0.1378(2) 0.60405(17) 0.0250(11) Uani 1 1 d . . . . .
C23 C 0.3979(3) -0.1950(2) 0.61214(19) 0.0308(12) Uani 1 1 d . . . . .
H23 H 0.4173 -0.2245 0.6365 0.037 Uiso 1 1 calc R . . . .
C24 C 0.3377(3) -0.2080(3) 0.5838(2) 0.0312(12) Uani 1 1 d . . . . .
C25 C 0.3100(3) -0.1680(3) 0.54724(19) 0.0311(12) Uani 1 1 d . . . . .
H25 H 0.2697 -0.1798 0.5274 0.037 Uiso 1 1 calc R . . . .
C26 C 0.3403(2) -0.1095(2) 0.53857(17) 0.0225(10) Uani 1 1 d . . . . .
C27 C 0.4010(3) -0.0938(2) 0.56714(17) 0.0243(11) Uani 1 1 d . . . . .
C28 C 0.3086(3) -0.0691(2) 0.49815(18) 0.0263(11) Uani 1 1 d . . . . .
H28 H 0.2655 -0.0811 0.4831 0.032 Uiso 1 1 calc R . . . .
C29 C 0.2996(3) 0.0209(2) 0.44432(19) 0.0257(11) Uani 1 1 d . . . . .
C30 C 0.2312(3) 0.0240(3) 0.4330(2) 0.0325(12) Uani 1 1 d . . . . .
H30 H 0.2050 -0.0032 0.4502 0.039 Uiso 1 1 calc R . . . .
C31 C 0.2000(3) 0.0657(3) 0.3972(2) 0.0358(13) Uani 1 1 d . . . . .
C32 C 0.2411(3) 0.1064(3) 0.37404(19) 0.0336(12) Uani 1 1 d . . . . .
H32 H 0.2212 0.1356 0.3495 0.040 Uiso 1 1 calc R . . . .
C33 C 0.3097(3) 0.1056(3) 0.38559(18) 0.0308(12) Uani 1 1 d . . . . .
H33 H 0.3357 0.1338 0.3691 0.037 Uiso 1 1 calc R . . . .
C34 C 0.3403(3) 0.0629(2) 0.42196(17) 0.0259(11) Uani 1 1 d . . . . .
C35 C 0.1276(3) 0.0675(3) 0.3852(2) 0.0399(14) Uani 1 1 d . . . . .
C36 C 0.0881(3) 0.0608(3) 0.4222(3) 0.0461(16) Uani 1 1 d . . . . .
H36 H 0.1080 0.0561 0.4556 0.055 Uiso 1 1 calc R . . . .
C37 C 0.0192(4) 0.0609(3) 0.4103(3) 0.0568(19) Uani 1 1 d . . . . .
H37 H -0.0072 0.0579 0.4360 0.068 Uiso 1 1 calc R . . . .
C38 C -0.0105(4) 0.0650(4) 0.3630(3) 0.070(2) Uani 1 1 d . . . . .
H38 H -0.0573 0.0627 0.3556 0.085 Uiso 1 1 calc R . . . .
C39 C 0.0269(4) 0.0726(5) 0.3258(3) 0.083(3) Uani 1 1 d . . . . .
H39 H 0.0059 0.0765 0.2925 0.099 Uiso 1 1 calc R . . . .
C40 C 0.0973(4) 0.0746(4) 0.3369(3) 0.0580(19) Uani 1 1 d . . . . .
H40 H 0.1232 0.0809 0.3111 0.070 Uiso 1 1 calc R . . . .
C41 C 0.4419(6) 0.2776(4) 0.6011(4) 0.113(5) Uani 1 1 d . . . . .
H41A H 0.4523 0.2878 0.5681 0.169 Uiso 1 1 calc R . . . .
H41B H 0.4725 0.3005 0.6261 0.169 Uiso 1 1 calc R . . . .
H41C H 0.3965 0.2910 0.6033 0.169 Uiso 1 1 calc R . . . .
C42 C 0.4366(4) 0.1869(3) 0.6531(2) 0.0483(17) Uani 1 1 d . . . . .
C43 C 0.4169(4) 0.2237(3) 0.6904(3) 0.062(2) Uani 1 1 d . . . . .
H43 H 0.4113 0.2689 0.6867 0.074 Uiso 1 1 calc R . . . .
C44 C 0.4055(5) 0.1922(4) 0.7344(3) 0.070(2) Uani 1 1 d . . . . .
C45 C 0.4116(4) 0.1282(3) 0.7409(2) 0.0538(18) Uani 1 1 d . . . . .
H45 H 0.4020 0.1086 0.7704 0.065 Uiso 1 1 calc R . . . .
C46 C 0.4330(3) 0.0903(3) 0.7024(2) 0.0379(14) Uani 1 1 d . . . . .
C47 C 0.4468(3) 0.1199(3) 0.6592(2) 0.0352(13) Uani 1 1 d . . . . .
C48 C 0.4385(3) 0.0226(3) 0.7101(2) 0.0419(15) Uani 1 1 d . . . . .
H48 H 0.4226 0.0057 0.7384 0.050 Uiso 1 1 calc R . . . .
C49 C 0.5304(8) 0.3769(6) 0.3441(7) 0.157(6) Uani 1 1 d D . . . .
H49A H 0.5249 0.4151 0.3223 0.188 Uiso 1 1 calc R . . . .
H49B H 0.5758 0.3770 0.3627 0.188 Uiso 1 1 calc R . . . .
C50 C 0.4767(9) 0.3764(9) 0.3808(6) 0.185(8) Uani 1 1 d D . . . .
H50A H 0.4886 0.3437 0.4064 0.278 Uiso 1 1 calc R . . . .
H50B H 0.4332 0.3663 0.3623 0.278 Uiso 1 1 calc R . . . .
H50C H 0.4753 0.4187 0.3963 0.278 Uiso 1 1 calc R . . . .
C51 C 0.1621(8) 0.2120(7) 0.7420(6) 0.155(6) Uani 1 1 d D . . . .
H51A H 0.1715 0.1658 0.7381 0.186 Uiso 1 1 calc R . . . .
H51B H 0.1881 0.2264 0.7734 0.186 Uiso 1 1 calc R . . . .
C52 C 0.1860(10) 0.2475(8) 0.7010(5) 0.209(9) Uani 1 1 d D . . . .
H52A H 0.1864 0.2937 0.7080 0.314 Uiso 1 1 calc R . . . .
H52B H 0.1566 0.2390 0.6700 0.314 Uiso 1 1 calc R . . . .
H52C H 0.2308 0.2333 0.6978 0.314 Uiso 1 1 calc R . . . .
C1 C 0.2658(4) 0.0676(4) 0.5651(3) 0.0607(10) Uani 1 1 d . . . . .
H1A H 0.2557 0.0286 0.5454 0.091 Uiso 1 1 calc R . . . .
H1B H 0.2276 0.0965 0.5602 0.091 Uiso 1 1 calc R . . . .
H1C H 0.2759 0.0561 0.6001 0.091 Uiso 1 1 calc R . . . .
C4 C 0.3190(4) 0.0976(4) 0.5507(3) 0.0607(10) Uani 1 1 d D . . . .
H4 H 0.3085 0.1421 0.5501 0.073 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Ni1 3.4824(7) . ?
Dy1 O2 2.191(4) . ?
Dy1 O3 2.429(3) . ?
Dy1 O4 2.545(3) . ?
Dy1 O5 2.295(3) . ?
Dy1 O6 2.379(3) 5_656 ?
Dy1 O8 2.276(4) . ?
Dy1 O9 2.436(4) . ?
Dy1 N1 2.490(4) . ?
Br1 C1AA 1.902(6) . ?
Br2 C24 1.911(5) . ?
Br3 C44 1.918(6) . ?
Ni1 O3 2.085(3) . ?
Ni1 O3 2.133(3) 5_656 ?
Ni1 O5 2.024(3) . ?
Ni1 O6 2.060(3) . ?
Ni1 O10 2.088(5) . ?
Ni1 N2 2.015(4) . ?
O1 C0AA 1.438(7) . ?
O1 C2 1.376(7) . ?
O2 C7 1.293(7) . ?
O3 Ni1 2.133(3) 5_656 ?
O3 C14 1.364(5) . ?
O4 C21 1.444(6) . ?
O4 C22 1.375(6) . ?
O5 C27 1.330(6) . ?
O6 Dy1 2.379(3) 5_656 ?
O6 C34 1.338(6) . ?
O7 C41 1.415(8) . ?
O7 C42 1.348(7) . ?
O8 C47 1.301(6) . ?
O9 C48 1.220(7) . ?
O10 H10 0.867(10) . ?
O10 C4 1.448(9) . ?
O11 H11 0.8400 . ?
O11 C49 1.471(13) . ?
O12 H12A 0.8400 . ?
O12 C51 1.479(13) . ?
N1 C8 1.293(7) . ?
N1 C9 1.445(6) . ?
N2 C28 1.269(6) . ?
N2 C29 1.417(7) . ?
C0AA H0AA 0.9800 . ?
C0AA H0AB 0.9800 . ?
C0AA H0AC 0.9800 . ?
C2 C3 1.364(9) . ?
C2 C7 1.434(7) . ?
C3 H3 0.9500 . ?
C3 C1AA 1.400(9) . ?
C1AA C5 1.355(8) . ?
C5 H5 0.9500 . ?
C5 C6 1.433(7) . ?
C6 C7 1.407(7) . ?
C6 C8 1.450(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.387(7) . ?
C9 C14 1.388(7) . ?
C10 H10A 0.9500 . ?
C10 C11 1.414(7) . ?
C11 C12 1.385(7) . ?
C11 C15 1.490(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.384(7) . ?
C13 H13 0.9500 . ?
C13 C14 1.389(7) . ?
C15 C16 1.377(8) . ?
C15 C20 1.390(7) . ?
C16 H16 0.9500 . ?
C16 C17 1.401(8) . ?
C17 H17 0.9500 . ?
C17 C18 1.364(9) . ?
C18 H18 0.9500 . ?
C18 C19 1.381(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.342(8) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.383(7) . ?
C22 C27 1.420(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.382(8) . ?
C24 C25 1.359(7) . ?
C25 H25 0.9500 . ?
C25 C26 1.401(7) . ?
C26 C27 1.406(7) . ?
C26 C28 1.463(7) . ?
C28 H28 0.9500 . ?
C29 C30 1.391(7) . ?
C29 C34 1.408(7) . ?
C30 H30 0.9500 . ?
C30 C31 1.393(8) . ?
C31 C32 1.408(8) . ?
C31 C35 1.470(8) . ?
C32 H32 0.9500 . ?
C32 C33 1.393(8) . ?
C33 H33 0.9500 . ?
C33 C34 1.411(7) . ?
C35 C36 1.391(9) . ?
C35 C40 1.383(9) . ?
C36 H36 0.9500 . ?
C36 C37 1.400(9) . ?
C37 H37 0.9500 . ?
C37 C38 1.348(11) . ?
C38 H38 0.9500 . ?
C38 C39 1.370(12) . ?
C39 H39 0.9500 . ?
C39 C40 1.428(11) . ?
C40 H40 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.381(8) . ?
C42 C47 1.416(8) . ?
C43 H43 0.9500 . ?
C43 C44 1.421(10) . ?
C44 C45 1.345(10) . ?
C45 H45 0.9500 . ?
C45 C46 1.435(8) . ?
C46 C47 1.399(7) . ?
C46 C48 1.426(9) . ?
C48 H48 0.9500 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.595(15) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C52 1.484(14) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C4 1.362(9) . ?
C4 H4 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 Ni1 169.30(9) . . ?
O2 Dy1 O3 136.48(12) . . ?
O2 Dy1 O4 85.44(12) . . ?
O2 Dy1 O5 149.24(13) . . ?
O2 Dy1 O6 86.51(13) . 5_656 ?
O2 Dy1 O8 112.89(14) . . ?
O2 Dy1 O9 77.60(14) . . ?
O2 Dy1 N1 73.42(13) . . ?
O3 Dy1 Ni1 36.05(8) . . ?
O3 Dy1 O4 124.30(11) . . ?
O3 Dy1 O9 140.01(13) . . ?
O3 Dy1 N1 66.96(12) . . ?
O4 Dy1 Ni1 95.63(8) . . ?
O5 Dy1 Ni1 33.70(8) . . ?
O5 Dy1 O3 69.02(11) . . ?
O5 Dy1 O4 63.81(11) . . ?
O5 Dy1 O6 88.48(12) . 5_656 ?
O5 Dy1 O9 88.95(13) . . ?
O5 Dy1 N1 135.71(12) . . ?
O6 Dy1 Ni1 83.23(8) 5_656 . ?
O6 Dy1 O3 71.14(11) 5_656 . ?
O6 Dy1 O4 79.55(11) 5_656 . ?
O6 Dy1 O9 143.70(12) 5_656 . ?
O6 Dy1 N1 81.95(12) 5_656 . ?
O8 Dy1 Ni1 74.80(9) . . ?
O8 Dy1 O3 75.74(11) . . ?
O8 Dy1 O4 127.79(12) . . ?
O8 Dy1 O5 87.47(13) . . ?
O8 Dy1 O6 145.81(11) . 5_656 ?
O8 Dy1 O9 70.14(12) . . ?
O8 Dy1 N1 77.53(13) . . ?
O9 Dy1 Ni1 112.64(11) . . ?
O9 Dy1 O4 66.94(12) . . ?
O9 Dy1 N1 122.89(13) . . ?
N1 Dy1 Ni1 102.05(9) . . ?
N1 Dy1 O4 152.63(13) . . ?
O3 Ni1 Dy1 43.27(8) . . ?
O3 Ni1 Dy1 92.85(9) 5_656 . ?
O3 Ni1 O3 82.73(13) . 5_656 ?
O3 Ni1 O10 88.14(17) . . ?
O5 Ni1 Dy1 39.00(10) . . ?
O5 Ni1 O3 81.36(13) . . ?
O5 Ni1 O3 91.12(13) . 5_656 ?
O5 Ni1 O6 169.26(14) . . ?
O5 Ni1 O10 94.85(17) . . ?
O6 Ni1 Dy1 150.32(10) . . ?
O6 Ni1 O3 107.16(13) . . ?
O6 Ni1 O3 83.67(13) . 5_656 ?
O6 Ni1 O10 92.00(17) . . ?
O10 Ni1 Dy1 85.49(15) . . ?
O10 Ni1 O3 168.23(17) . 5_656 ?
N2 Ni1 Dy1 127.03(11) . . ?
N2 Ni1 O3 170.21(14) . . ?
N2 Ni1 O3 100.62(15) . 5_656 ?
N2 Ni1 O5 89.34(15) . . ?
N2 Ni1 O6 82.44(15) . . ?
N2 Ni1 O10 89.60(19) . . ?
C2 O1 C0AA 117.2(5) . . ?
C7 O2 Dy1 141.8(3) . . ?
Ni1 O3 Dy1 100.68(12) . . ?
Ni1 O3 Dy1 100.36(13) 5_656 . ?
Ni1 O3 Ni1 97.27(13) . 5_656 ?
C14 O3 Dy1 113.3(3) . . ?
C14 O3 Ni1 115.4(3) . 5_656 ?
C14 O3 Ni1 125.8(3) . . ?
C21 O4 Dy1 121.9(3) . . ?
C22 O4 Dy1 117.0(3) . . ?
C22 O4 C21 117.1(4) . . ?
Ni1 O5 Dy1 107.30(14) . . ?
C27 O5 Dy1 126.8(3) . . ?
C27 O5 Ni1 125.3(3) . . ?
Ni1 O6 Dy1 104.25(14) . 5_656 ?
C34 O6 Dy1 123.1(3) . 5_656 ?
C34 O6 Ni1 106.4(3) . . ?
C42 O7 C41 118.5(5) . . ?
C47 O8 Dy1 137.4(3) . . ?
C48 O9 Dy1 134.1(4) . . ?
Ni1 O10 H10 119.6(18) . . ?
C4 O10 Ni1 127.8(4) . . ?
C4 O10 H10 103.1(17) . . ?
C49 O11 H11 109.5 . . ?
C51 O12 H12A 109.5 . . ?
C8 N1 Dy1 129.5(3) . . ?
C8 N1 C9 119.2(4) . . ?
C9 N1 Dy1 111.2(3) . . ?
C28 N2 Ni1 127.6(4) . . ?
C28 N2 C29 123.9(5) . . ?
C29 N2 Ni1 108.4(3) . . ?
O1 C0AA H0AA 109.5 . . ?
O1 C0AA H0AB 109.5 . . ?
O1 C0AA H0AC 109.5 . . ?
H0AA C0AA H0AB 109.5 . . ?
H0AA C0AA H0AC 109.5 . . ?
H0AB C0AA H0AC 109.5 . . ?
O1 C2 C7 113.2(5) . . ?
C3 C2 O1 124.8(5) . . ?
C3 C2 C7 122.0(5) . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C1AA 119.7(6) . . ?
C1AA C3 H3 120.2 . . ?
C3 C1AA Br1 117.9(5) . . ?
C5 C1AA Br1 120.7(5) . . ?
C5 C1AA C3 121.3(6) . . ?
C1AA C5 H5 120.2 . . ?
C1AA C5 C6 119.7(5) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C8 116.8(5) . . ?
C7 C6 C5 120.5(5) . . ?
C7 C6 C8 122.8(5) . . ?
O2 C7 C2 119.1(5) . . ?
O2 C7 C6 124.1(5) . . ?
C6 C7 C2 116.8(5) . . ?
N1 C8 C6 126.5(5) . . ?
N1 C8 H8 116.8 . . ?
C6 C8 H8 116.8 . . ?
C10 C9 N1 123.1(4) . . ?
C10 C9 C14 120.6(4) . . ?
C14 C9 N1 116.2(4) . . ?
C9 C10 H10A 119.5 . . ?
C9 C10 C11 121.0(5) . . ?
C11 C10 H10A 119.5 . . ?
C10 C11 C15 121.6(5) . . ?
C12 C11 C10 117.0(5) . . ?
C12 C11 C15 121.4(5) . . ?
C11 C12 H12 118.9 . . ?
C13 C12 C11 122.2(5) . . ?
C13 C12 H12 118.9 . . ?
C12 C13 H13 119.9 . . ?
C12 C13 C14 120.3(5) . . ?
C14 C13 H13 119.9 . . ?
O3 C14 C9 120.1(4) . . ?
O3 C14 C13 121.0(5) . . ?
C9 C14 C13 118.9(4) . . ?
C16 C15 C11 122.3(5) . . ?
C16 C15 C20 116.8(5) . . ?
C20 C15 C11 120.8(5) . . ?
C15 C16 H16 119.4 . . ?
C15 C16 C17 121.2(6) . . ?
C17 C16 H16 119.4 . . ?
C16 C17 H17 120.2 . . ?
C18 C17 C16 119.6(6) . . ?
C18 C17 H17 120.2 . . ?
C17 C18 H18 120.3 . . ?
C17 C18 C19 119.4(5) . . ?
C19 C18 H18 120.3 . . ?
C18 C19 H19 119.8 . . ?
C20 C19 C18 120.5(6) . . ?
C20 C19 H19 119.8 . . ?
C15 C20 H20 118.8 . . ?
C19 C20 C15 122.5(6) . . ?
C19 C20 H20 118.8 . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C22 C23 124.9(5) . . ?
O4 C22 C27 113.7(4) . . ?
C23 C22 C27 121.4(5) . . ?
C22 C23 H23 120.9 . . ?
C24 C23 C22 118.2(5) . . ?
C24 C23 H23 120.9 . . ?
C23 C24 Br2 118.0(4) . . ?
C25 C24 Br2 119.7(4) . . ?
C25 C24 C23 122.3(5) . . ?
C24 C25 H25 119.7 . . ?
C24 C25 C26 120.5(5) . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C27 119.0(4) . . ?
C25 C26 C28 118.0(5) . . ?
C27 C26 C28 122.9(4) . . ?
O5 C27 C22 116.5(5) . . ?
O5 C27 C26 125.0(4) . . ?
C26 C27 C22 118.5(4) . . ?
N2 C28 C26 125.7(5) . . ?
N2 C28 H28 117.1 . . ?
C26 C28 H28 117.1 . . ?
C30 C29 N2 124.0(5) . . ?
C30 C29 C34 121.0(5) . . ?
C34 C29 N2 114.7(5) . . ?
C29 C30 H30 119.0 . . ?
C29 C30 C31 121.9(5) . . ?
C31 C30 H30 119.0 . . ?
C30 C31 C32 116.7(5) . . ?
C30 C31 C35 121.1(5) . . ?
C32 C31 C35 122.2(5) . . ?
C31 C32 H32 118.7 . . ?
C33 C32 C31 122.7(5) . . ?
C33 C32 H32 118.7 . . ?
C32 C33 H33 120.1 . . ?
C32 C33 C34 119.7(5) . . ?
C34 C33 H33 120.1 . . ?
O6 C34 C29 120.5(4) . . ?
O6 C34 C33 121.5(5) . . ?
C29 C34 C33 117.9(5) . . ?
C36 C35 C31 120.6(6) . . ?
C40 C35 C31 120.8(6) . . ?
C40 C35 C36 118.6(6) . . ?
C35 C36 H36 119.9 . . ?
C35 C36 C37 120.2(7) . . ?
C37 C36 H36 119.9 . . ?
C36 C37 H37 119.3 . . ?
C38 C37 C36 121.3(7) . . ?
C38 C37 H37 119.3 . . ?
C37 C38 H38 120.1 . . ?
C37 C38 C39 119.9(7) . . ?
C39 C38 H38 120.1 . . ?
C38 C39 H39 119.9 . . ?
C38 C39 C40 120.1(8) . . ?
C40 C39 H39 119.9 . . ?
C35 C40 C39 119.7(7) . . ?
C35 C40 H40 120.1 . . ?
C39 C40 H40 120.1 . . ?
O7 C41 H41A 109.5 . . ?
O7 C41 H41B 109.5 . . ?
O7 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O7 C42 C43 124.2(6) . . ?
O7 C42 C47 114.9(5) . . ?
C43 C42 C47 120.9(5) . . ?
C42 C43 H43 120.9 . . ?
C42 C43 C44 118.1(6) . . ?
C44 C43 H43 120.9 . . ?
C43 C44 Br3 116.6(6) . . ?
C45 C44 Br3 120.4(5) . . ?
C45 C44 C43 123.0(6) . . ?
C44 C45 H45 120.7 . . ?
C44 C45 C46 118.6(6) . . ?
C46 C45 H45 120.7 . . ?
C47 C46 C45 120.0(6) . . ?
C47 C46 C48 122.6(5) . . ?
C48 C46 C45 117.4(5) . . ?
O8 C47 C42 118.5(5) . . ?
O8 C47 C46 122.3(5) . . ?
C46 C47 C42 119.2(5) . . ?
O9 C48 C46 125.4(5) . . ?
O9 C48 H48 117.3 . . ?
C46 C48 H48 117.3 . . ?
O11 C49 H49A 110.9 . . ?
O11 C49 H49B 110.9 . . ?
O11 C49 C50 104.1(12) . . ?
H49A C49 H49B 109.0 . . ?
C50 C49 H49A 110.9 . . ?
C50 C49 H49B 110.9 . . ?
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 . . ?
O12 C51 H51A 108.1 . . ?
O12 C51 H51B 108.1 . . ?
O12 C51 C52 116.6(13) . . ?
H51A C51 H51B 107.3 . . ?
C52 C51 H51A 108.1 . . ?
C52 C51 H51B 108.1 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C1 H1A 109.5 . . ?
C4 C1 H1B 109.5 . . ?
C4 C1 H1C 109.5 . . ?
O10 C4 H4 105.3 . . ?
C1 C4 O10 149.3(7) . . ?
C1 C4 H4 105.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O2 C7 C2 -165.4(4) . . . . ?
Dy1 O2 C7 C6 15.0(9) . . . . ?
Dy1 O3 C14 C9 29.6(5) . . . . ?
Dy1 O3 C14 C13 -150.7(4) . . . . ?
Dy1 O4 C22 C23 -170.3(4) . . . . ?
Dy1 O4 C22 C27 12.8(5) . . . . ?
Dy1 O5 C27 C22 -10.4(6) . . . . ?
Dy1 O5 C27 C26 169.5(3) . . . . ?
Dy1 O6 C34 C29 97.7(5) 5_656 . . . ?
Dy1 O6 C34 C33 -79.3(5) 5_656 . . . ?
Dy1 O8 C47 C42 153.4(5) . . . . ?
Dy1 O8 C47 C46 -28.4(9) . . . . ?
Dy1 O9 C48 C46 11.3(11) . . . . ?
Dy1 N1 C8 C6 -7.5(8) . . . . ?
Dy1 N1 C9 C10 154.3(4) . . . . ?
Dy1 N1 C9 C14 -23.2(5) . . . . ?
Br1 C1AA C5 C6 -179.0(4) . . . . ?
Br2 C24 C25 C26 177.4(4) . . . . ?
Br3 C44 C45 C46 -178.4(5) . . . . ?
Ni1 O3 C14 C9 153.6(3) . . . . ?
Ni1 O3 C14 C9 -85.4(4) 5_656 . . . ?
Ni1 O3 C14 C13 -26.7(6) . . . . ?
Ni1 O3 C14 C13 94.3(5) 5_656 . . . ?
Ni1 O5 C27 C22 159.6(3) . . . . ?
Ni1 O5 C27 C26 -20.5(6) . . . . ?
Ni1 O6 C34 C29 -22.1(5) . . . . ?
Ni1 O6 C34 C33 160.8(4) . . . . ?
Ni1 O10 C4 C1 26.5(16) . . . . ?
Ni1 N2 C28 C26 3.6(7) . . . . ?
Ni1 N2 C29 C30 -158.1(4) . . . . ?
Ni1 N2 C29 C34 16.4(5) . . . . ?
O1 C2 C3 C1AA 178.6(6) . . . . ?
O1 C2 C7 O2 0.9(7) . . . . ?
O1 C2 C7 C6 -179.5(5) . . . . ?
O4 C22 C23 C24 -177.8(5) . . . . ?
O4 C22 C27 O5 -3.0(6) . . . . ?
O4 C22 C27 C26 177.0(4) . . . . ?
O7 C42 C43 C44 178.9(8) . . . . ?
O7 C42 C47 O8 1.4(9) . . . . ?
O7 C42 C47 C46 -176.8(6) . . . . ?
N1 C9 C10 C11 -177.7(4) . . . . ?
N1 C9 C14 O3 -3.6(6) . . . . ?
N1 C9 C14 C13 176.8(4) . . . . ?
N2 C29 C30 C31 178.0(5) . . . . ?
N2 C29 C34 O6 4.5(7) . . . . ?
N2 C29 C34 C33 -178.3(4) . . . . ?
C0AA O1 C2 C3 9.8(9) . . . . ?
C0AA O1 C2 C7 -170.0(6) . . . . ?
C2 C3 C1AA Br1 179.9(5) . . . . ?
C2 C3 C1AA C5 1.6(10) . . . . ?
C3 C2 C7 O2 -178.9(5) . . . . ?
C3 C2 C7 C6 0.7(8) . . . . ?
C3 C1AA C5 C6 -0.7(10) . . . . ?
C1AA C5 C6 C7 -0.2(8) . . . . ?
C1AA C5 C6 C8 -179.8(5) . . . . ?
C5 C6 C7 O2 179.8(5) . . . . ?
C5 C6 C7 C2 0.2(7) . . . . ?
C5 C6 C8 N1 178.5(5) . . . . ?
C7 C2 C3 C1AA -1.6(9) . . . . ?
C7 C6 C8 N1 -1.2(8) . . . . ?
C8 N1 C9 C10 -28.6(7) . . . . ?
C8 N1 C9 C14 154.0(5) . . . . ?
C8 C6 C7 O2 -0.6(8) . . . . ?
C8 C6 C7 C2 179.8(5) . . . . ?
C9 N1 C8 C6 176.0(5) . . . . ?
C9 C10 C11 C12 1.6(7) . . . . ?
C9 C10 C11 C15 -179.3(4) . . . . ?
C10 C9 C14 O3 178.9(4) . . . . ?
C10 C9 C14 C13 -0.8(7) . . . . ?
C10 C11 C12 C13 -1.7(7) . . . . ?
C10 C11 C15 C16 -24.7(8) . . . . ?
C10 C11 C15 C20 156.4(5) . . . . ?
C11 C12 C13 C14 0.6(7) . . . . ?
C11 C15 C16 C17 -179.9(5) . . . . ?
C11 C15 C20 C19 178.0(6) . . . . ?
C12 C11 C15 C16 154.3(6) . . . . ?
C12 C11 C15 C20 -24.6(8) . . . . ?
C12 C13 C14 O3 -179.0(4) . . . . ?
C12 C13 C14 C9 0.7(7) . . . . ?
C14 C9 C10 C11 -0.4(7) . . . . ?
C15 C11 C12 C13 179.2(5) . . . . ?
C15 C16 C17 C18 2.4(10) . . . . ?
C16 C15 C20 C19 -1.0(9) . . . . ?
C16 C17 C18 C19 -1.8(10) . . . . ?
C17 C18 C19 C20 -0.1(10) . . . . ?
C18 C19 C20 C15 1.5(11) . . . . ?
C20 C15 C16 C17 -1.0(9) . . . . ?
C21 O4 C22 C23 -12.2(7) . . . . ?
C21 O4 C22 C27 170.9(5) . . . . ?
C22 C23 C24 Br2 -177.9(4) . . . . ?
C22 C23 C24 C25 2.9(8) . . . . ?
C23 C22 C27 O5 179.9(4) . . . . ?
C23 C22 C27 C26 0.0(7) . . . . ?
C23 C24 C25 C26 -3.4(8) . . . . ?
C24 C25 C26 C27 2.2(8) . . . . ?
C24 C25 C26 C28 179.0(5) . . . . ?
C25 C26 C27 O5 179.6(4) . . . . ?
C25 C26 C27 C22 -0.5(7) . . . . ?
C25 C26 C28 N2 -170.3(5) . . . . ?
C27 C22 C23 C24 -1.1(7) . . . . ?
C27 C26 C28 N2 6.4(8) . . . . ?
C28 N2 C29 C30 21.3(8) . . . . ?
C28 N2 C29 C34 -164.2(5) . . . . ?
C28 C26 C27 O5 2.9(7) . . . . ?
C28 C26 C27 C22 -177.1(4) . . . . ?
C29 N2 C28 C26 -175.8(5) . . . . ?
C29 C30 C31 C32 -2.0(8) . . . . ?
C29 C30 C31 C35 179.0(5) . . . . ?
C30 C29 C34 O6 179.2(5) . . . . ?
C30 C29 C34 C33 -3.6(7) . . . . ?
C30 C31 C32 C33 0.2(8) . . . . ?
C30 C31 C35 C36 37.9(8) . . . . ?
C30 C31 C35 C40 -140.7(6) . . . . ?
C31 C32 C33 C34 -0.1(8) . . . . ?
C31 C35 C36 C37 -178.3(6) . . . . ?
C31 C35 C40 C39 176.4(7) . . . . ?
C32 C31 C35 C36 -141.0(6) . . . . ?
C32 C31 C35 C40 40.4(9) . . . . ?
C32 C33 C34 O6 178.9(5) . . . . ?
C32 C33 C34 C29 1.8(7) . . . . ?
C34 C29 C30 C31 3.8(8) . . . . ?
C35 C31 C32 C33 179.2(5) . . . . ?
C35 C36 C37 C38 2.5(11) . . . . ?
C36 C35 C40 C39 -2.2(10) . . . . ?
C36 C37 C38 C39 -3.3(13) . . . . ?
C37 C38 C39 C40 1.4(14) . . . . ?
C38 C39 C40 C35 1.4(13) . . . . ?
C40 C35 C36 C37 0.3(9) . . . . ?
C41 O7 C42 C43 2.1(12) . . . . ?
C41 O7 C42 C47 -177.3(8) . . . . ?
C42 C43 C44 Br3 179.2(6) . . . . ?
C42 C43 C44 C45 -1.3(14) . . . . ?
C43 C42 C47 O8 -178.0(7) . . . . ?
C43 C42 C47 C46 3.7(11) . . . . ?
C43 C44 C45 C46 2.2(13) . . . . ?
C44 C45 C46 C47 -0.1(11) . . . . ?
C44 C45 C46 C48 -179.5(8) . . . . ?
C45 C46 C47 O8 179.0(6) . . . . ?
C45 C46 C47 C42 -2.8(10) . . . . ?
C45 C46 C48 O9 -172.3(7) . . . . ?
C47 C42 C43 C44 -1.7(12) . . . . ?
C47 C46 C48 O9 8.3(11) . . . . ?
C48 C46 C47 O8 -1.6(10) . . . . ?
C48 C46 C47 C42 176.6(7) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.669 -0.669 0.000 763.5 25.0 ?
2 -0.789 -0.789 0.500 763.5 25.0 ?
3 0.000 0.175 0.250 9.1 0.0 ?
4 0.000 0.825 0.750 9.1 0.0 ?
5 0.500 0.325 0.750 9.1 0.0 ?
6 0.500 0.675 0.250 9.1 0.0 ?

# start Validation Reply Form
_vrf_CHEMW03_kg04040414          
;
PROBLEM:The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    4
           From the CIF: _chemical_formula_weight          2848.01
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01  108.00 1297.19
           H         1.01  102.00  102.82
           N        14.01    4.00   56.03
           O        16.00   24.00  383.98
           Ni       58.69    2.00  117.38
           Dy      162.50    2.00  325.00
           Br       79.90    6.00  479.42

           Calculated formula weight             2761.81
RESPONSE: The sample diffracted very weakly at high angles and the
reflections were completely absent. Therefore PLATON / SQUEEZE
programm as used to remove those disordered solvent molecules and 
obtained the total electron count of 50 per unit cell and was 
assigned to two EtOH molecules. The reported formula, molecular weight, 
F000, density etc include the contribution of disordered solvents 
(2 EtOH) which were removed by SQUEEZE.
;
# end Validation Reply Form

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

data_9_CCDC_1406225
_database_code_depnum_ccdc_archive 'CCDC 1406225'
_audit_update_record             
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_audit_creation_date             2015-01-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C110 H102 Dy2 N4 Ni2 O20, 2(C4 H8 O) 2(C2 H6 O)'
_chemical_formula_sum            'C122 H130 Dy2 N4 Ni2 O24'
_chemical_formula_weight         2478.64
_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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   38.159(3)
_cell_length_b                   38.159(3)
_cell_length_c                   18.7654(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     23664(4)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    100
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.832
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             10962
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56666
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.496
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9239
_reflns_number_total             11972
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.455
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         11972
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0408
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0768P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1157
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O23-H23
 0.85 with sigma of 0.01
 C728-H23
 1.886514 with sigma of 0.02
 Ni13-H23
 2.587601 with sigma of 0.02
3. Rigid bond restraints
 O3, C8, C10, C5, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
H126 \\sim O3 \\sim C8 \\sim C10 \\sim C5 \\sim C6: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C755) = Uanis(C2) = Uanis(C551)
Uanis(C4) = Uanis(C53) = Uanis(C9)
Uanis(C212) = Uanis(C307) = Uanis(C58)
5. Rigid body (RIGU) restrains
 O3, C8, C10, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C5(H5A,H5B), C6(H6A,H6B)
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C212(H21A,H21B), C551(H55A,H55B), C728(H72A,H72B)
6.c Aromatic/amide H refined with riding coordinates:
 C80(H80), C239(H239), C16(H16), C29(H29), C53(H53), C110(H110), C126(H126),
 C2(H2), C18(H18), C46(H46), C59(H59), C168(H168), C1(H1), C307(H307),
 C321(H321), C360(H360), C379(H379), C411(H411), C422(H422), C469(H469),
 C504(H504), C635(H635), C716(H716), C757(H757)
6.d X=CH2 refined with riding coordinates:
 C58(H58A,H58B), C755(H75A,H75B)
6.e Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C345(H34A,H34B,H34C), C674(H67A,H67B,H67C), C7(H7A,H7B,
 H7C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy18 Dy 0.43934(2) 0.53143(2) 0.47252(2) 0.03553(7) Uani 1 1 d . . . . .
Ni13 Ni 0.46737(2) 0.46535(2) 0.54959(2) 0.03405(11) Uani 1 1 d D . . . .
C4 C 0.5145(3) 0.7437(2) 0.3386(4) 0.1086(14) Uani 1 1 d . . . . .
H4A H 0.5416 0.7581 0.3609 0.130 Uiso 1 1 calc R . . . .
H4B H 0.5181 0.7454 0.2863 0.130 Uiso 1 1 calc R . . . .
O23 O 0.43488(7) 0.46898(8) 0.63653(14) 0.0407(6) Uani 1 1 d D . . . .
H23 H 0.4300(12) 0.4885(9) 0.6322(11) 0.061 Uiso 1 1 d DR . . . .
O63 O 0.40609(10) 0.60122(11) 0.3026(2) 0.0769(11) Uani 1 1 d . . . . .
C80 C 0.42188(14) 0.30127(14) 0.7292(3) 0.0566(10) Uani 1 1 d . . . . .
H80 H 0.3970 0.2814 0.7089 0.068 Uiso 1 1 calc R . . . .
O101 O 0.43852(7) 0.54823(8) 0.72112(14) 0.0408(6) Uani 1 1 d . . . . .
O113 O 0.41945(7) 0.52571(7) 0.58852(14) 0.0404(5) Uani 1 1 d . . . . .
O136 O 0.36733(7) 0.51229(8) 0.47656(15) 0.0465(6) Uani 1 1 d . . . . .
O141 O 0.43252(7) 0.57687(8) 0.41335(15) 0.0438(6) Uani 1 1 d . . . . .
O160 O 0.50735(7) 0.45627(7) 0.60927(13) 0.0385(5) Uani 1 1 d . . . . .
O184 O 0.40038(7) 0.48565(7) 0.37286(14) 0.0424(6) Uani 1 1 d . . . . .
C212 C 0.33421(18) 0.34551(15) 0.2778(3) 0.0774(9) Uani 1 1 d . . . . .
H21A H 0.3547 0.3498 0.2412 0.093 Uiso 1 1 calc R . . . .
H21B H 0.3235 0.3179 0.2971 0.093 Uiso 1 1 calc R . . . .
C239 C 0.55404(11) 0.56769(12) 0.7731(2) 0.0439(8) Uani 1 1 d . . . . .
H239 H 0.5542 0.5430 0.7779 0.053 Uiso 1 1 calc R . . . .
O248 O 0.49328(6) 0.52816(7) 0.53657(13) 0.0344(5) Uani 1 1 d . . . . .
C16 C 0.43728(16) 0.29112(16) 0.7861(3) 0.0671(13) Uani 1 1 d . . . . .
H16 H 0.4236 0.2644 0.8045 0.081 Uiso 1 1 calc R . . . .
C29 C 0.37880(10) 0.55576(10) 0.7350(2) 0.0390(8) Uani 1 1 d . . . . .
H29 H 0.3850 0.5635 0.7835 0.047 Uiso 1 1 calc R . . . .
C53 C 0.4914(3) 0.7634(2) 0.3596(4) 0.1086(14) Uani 1 1 d . . . . .
H53 H 0.4884 0.7646 0.4097 0.130 Uiso 1 1 calc R . . . .
C58 C 0.30385(18) 0.36106(14) 0.1755(3) 0.0774(9) Uani 1 1 d . . . . .
H58A H 0.3278 0.3695 0.1486 0.093 Uiso 1 1 calc R . . . .
H58B H 0.2816 0.3620 0.1550 0.093 Uiso 1 1 calc R . . . .
C88 C 0.39287(10) 0.39470(10) 0.4503(2) 0.0379(8) Uani 1 1 d . . . . .
C110 C 0.33531(11) 0.54231(11) 0.6355(2) 0.0441(9) Uani 1 1 d . . . . .
H110 H 0.3118 0.5406 0.6146 0.053 Uiso 1 1 calc R . . . .
C126 C 0.56774(12) 0.59485(12) 0.8273(2) 0.0498(9) Uani 1 1 d . . . . .
H126 H 0.5768 0.5886 0.8700 0.060 Uiso 1 1 calc R U . . .
O135 O 0.42602(7) 0.46586(7) 0.48310(13) 0.0372(5) Uani 1 1 d . . . . .
C139 C 0.53933(10) 0.57592(10) 0.7087(2) 0.0379(7) Uani 1 1 d . . . . .
C2 C 0.34049(15) 0.60724(14) 0.7770(3) 0.0618(7) Uani 1 1 d . . . . .
H2 H 0.3477 0.6283 0.7432 0.074 Uiso 1 1 calc R . . . .
C18 C 0.42781(11) 0.35178(12) 0.6396(2) 0.0444(8) Uani 1 1 d . . . . .
H18 H 0.4031 0.3322 0.6182 0.053 Uiso 1 1 calc R . . . .
C31 C 0.44955(12) 0.56034(13) 0.7936(2) 0.0480(9) Uani 1 1 d . . . . .
H31A H 0.4534 0.5875 0.8006 0.072 Uiso 1 1 calc GR . . . .
H31B H 0.4748 0.5606 0.8046 0.072 Uiso 1 1 calc GR . . . .
H31C H 0.4280 0.5412 0.8252 0.072 Uiso 1 1 calc GR . . . .
C46 C 0.47378(16) 0.32082(18) 0.8171(3) 0.0745(15) Uani 1 1 d . . . . .
H46 H 0.4845 0.3138 0.8567 0.089 Uiso 1 1 calc R . . . .
C59 C 0.40802(10) 0.38127(11) 0.5084(2) 0.0380(8) Uani 1 1 d . . . . .
H59 H 0.3967 0.3529 0.5144 0.046 Uiso 1 1 calc R . . . .
C91 C 0.53986(10) 0.61327(11) 0.7020(2) 0.0395(8) Uani 1 1 d . . . . .
C123 C 0.34401(11) 0.55361(11) 0.7050(2) 0.0416(8) Uani 1 1 d . . . . .
N142 N 0.43557(8) 0.40440(9) 0.55291(16) 0.0372(6) Uani 1 1 d . . . . .
C168 C 0.49398(14) 0.35945(16) 0.7913(3) 0.0627(12) Uani 1 1 d . . . . .
H168 H 0.5183 0.3790 0.8138 0.075 Uiso 1 1 calc R . . . .
C172 C 0.36068(10) 0.53295(11) 0.5934(2) 0.0393(8) Uani 1 1 d . . . . .
C177 C 0.44230(12) 0.34092(12) 0.6998(2) 0.0479(9) Uani 1 1 d . . . . .
C214 C 0.35520(11) 0.37569(12) 0.3379(2) 0.0467(9) Uani 1 1 d . . . . .
C1 C 0.52395(10) 0.62077(10) 0.6395(2) 0.0395(8) Uani 1 1 d . . . . .
H1 H 0.5237 0.6454 0.6351 0.047 Uiso 1 1 calc R . . . .
N246 N 0.48987(8) 0.59719(9) 0.52260(17) 0.0381(6) Uani 1 1 d . . . . .
C257 C 0.39556(10) 0.53511(10) 0.6236(2) 0.0379(8) Uani 1 1 d . . . . .
C307 C 0.30137(18) 0.34764(14) 0.2436(3) 0.0774(9) Uani 1 1 d . . . . .
H307 H 0.2771 0.3393 0.2696 0.093 Uiso 1 1 calc R . . . .
C321 C 0.50610(13) 0.68530(12) 0.4175(2) 0.0497(9) Uani 1 1 d . . . . .
H321 H 0.5296 0.7041 0.4428 0.060 Uiso 1 1 calc R . . . .
C345 C 0.39262(12) 0.44933(12) 0.7422(2) 0.0508(9) Uani 1 1 d . . . . .
H34A H 0.3717 0.4254 0.7172 0.076 Uiso 1 1 calc GR . . . .
H34B H 0.3871 0.4717 0.7369 0.076 Uiso 1 1 calc GR . . . .
H34C H 0.3925 0.4431 0.7928 0.076 Uiso 1 1 calc GR . . . .
C360 C 0.52375(10) 0.54758(10) 0.65202(19) 0.0363(7) Uani 1 1 d . . . . .
H360 H 0.5239 0.5228 0.6560 0.044 Uiso 1 1 calc R . . . .
C363 C 0.50882(10) 0.59283(11) 0.58479(19) 0.0370(7) Uani 1 1 d . . . . .
C378 C 0.43820(13) 0.63042(13) 0.3416(3) 0.0565(11) Uani 1 1 d . . . . .
C379 C 0.56876(12) 0.63238(12) 0.8211(2) 0.0520(10) Uani 1 1 d . . . . .
H379 H 0.5787 0.6513 0.8592 0.062 Uiso 1 1 calc R . . . .
C396 C 0.48594(11) 0.64421(11) 0.4381(2) 0.0430(8) Uani 1 1 d . . . . .
C411 C 0.36836(10) 0.36571(11) 0.3984(2) 0.0440(9) Uani 1 1 d . . . . .
H411 H 0.3607 0.3382 0.4059 0.053 Uiso 1 1 calc R . . . .
C422 C 0.55534(11) 0.64119(12) 0.7596(2) 0.0472(9) Uani 1 1 d . . . . .
H422 H 0.5564 0.6665 0.7554 0.057 Uiso 1 1 calc R . . . .
C454 C 0.40399(10) 0.54704(10) 0.6966(2) 0.0368(7) Uani 1 1 d . . . . .
C459 C 0.47916(12) 0.37067(13) 0.7315(2) 0.0482(9) Uani 1 1 d . . . . .
C469 C 0.36464(10) 0.41606(12) 0.3284(2) 0.0421(8) Uani 1 1 d . . . . .
H469 H 0.3551 0.4235 0.2876 0.051 Uiso 1 1 calc R . . . .
C504 C 0.50237(11) 0.63320(11) 0.4970(2) 0.0427(8) Uani 1 1 d . . . . .
H504 H 0.5251 0.6548 0.5201 0.051 Uiso 1 1 calc R . . . .
C512 C 0.50860(9) 0.55523(10) 0.59192(19) 0.0351(7) Uani 1 1 d . . . . .
C544 C 0.40298(9) 0.43533(11) 0.4399(2) 0.0377(8) Uani 1 1 d . . . . .
C551 C 0.31739(15) 0.56402(14) 0.7505(3) 0.0618(7) Uani 1 1 d . . . . .
H55A H 0.2939 0.5602 0.7220 0.074 Uiso 1 1 calc R . . . .
H55B H 0.3070 0.5454 0.7918 0.074 Uiso 1 1 calc R . . . .
C574 C 0.44863(10) 0.39005(11) 0.6109(2) 0.0389(8) Uani 1 1 d . . . . .
C583 C 0.45129(11) 0.61555(12) 0.3995(2) 0.0443(8) Uani 1 1 d . . . . .
C627 C 0.49245(14) 0.69867(12) 0.3619(2) 0.0556(10) Uani 1 1 d . . . . .
C635 C 0.50020(12) 0.41026(13) 0.7013(2) 0.0462(9) Uani 1 1 d . . . . .
H635 H 0.5243 0.4304 0.7235 0.055 Uiso 1 1 calc R . . . .
C670 C 0.38778(10) 0.44470(11) 0.3783(2) 0.0378(7) Uani 1 1 d . . . . .
C674 C 0.38530(12) 0.49822(13) 0.3140(2) 0.0469(9) Uani 1 1 d . . . . .
H67A H 0.3556 0.4835 0.3151 0.070 Uiso 1 1 calc GR . . . .
H67B H 0.3946 0.4924 0.2692 0.070 Uiso 1 1 calc GR . . . .
H67C H 0.3953 0.5273 0.3174 0.070 Uiso 1 1 calc GR . . . .
C713 C 0.48659(11) 0.41978(11) 0.6415(2) 0.0401(8) Uani 1 1 d . . . . .
C716 C 0.45792(14) 0.67101(14) 0.3239(3) 0.0601(11) Uani 1 1 d . . . . .
H716 H 0.4481 0.6802 0.2860 0.072 Uiso 1 1 calc R . . . .
C728 C 0.43423(13) 0.46164(14) 0.7102(2) 0.0542(10) Uani 1 1 d D . . . .
H72A H 0.4552 0.4864 0.7343 0.065 Uiso 1 1 calc R . . . .
H72B H 0.4406 0.4398 0.7184 0.065 Uiso 1 1 calc R . . . .
C755 C 0.35128(15) 0.61770(15) 0.8437(3) 0.0618(7) Uani 1 1 d . . . . .
H75A H 0.3446 0.5975 0.8790 0.074 Uiso 1 1 calc R . . . .
H75B H 0.3658 0.6455 0.8566 0.074 Uiso 1 1 calc R . . . .
C757 C 0.34883(11) 0.52062(11) 0.5214(2) 0.0461(9) Uani 1 1 d . . . . .
H757 H 0.3241 0.5186 0.5064 0.055 Uiso 1 1 calc R . . . .
O3 O 0.45394(18) 0.44754(19) 0.9854(3) 0.1308(18) Uani 1 1 d . U . . .
C7 C 0.3940(3) 0.6117(3) 0.2375(5) 0.130(3) Uani 1 1 d . . . . .
H7A H 0.4176 0.6261 0.2062 0.195 Uiso 1 1 calc GR . . . .
H7B H 0.3827 0.6293 0.2479 0.195 Uiso 1 1 calc GR . . . .
H7C H 0.3735 0.5871 0.2137 0.195 Uiso 1 1 calc GR . . . .
C8_a C 0.4747(3) 0.4254(3) 0.9930(5) 0.140(3) Uani 1 1 d . U . A 1
H8A_a H 0.4928 0.4336 1.0337 0.168 Uiso 1 1 d R . . A 1
H8B_a H 0.4559 0.3965 0.9953 0.168 Uiso 1 1 d R . . A 1
C9 C 0.4746(3) 0.7793(2) 0.3229(4) 0.1086(14) Uani 1 1 d . . . . .
H9A H 0.4758 0.7795 0.2734 0.130 Uiso 1 1 d R . . . .
H9B H 0.4610 0.7906 0.3461 0.130 Uiso 1 1 d R . . . .
C10_a C 0.4645(4) 0.4697(4) 0.9183(6) 0.169(4) Uani 1 1 d . U . A 1
H10A_a H 0.4423 0.4566 0.8848 0.202 Uiso 1 1 d R . . A 1
H10B_a H 0.4703 0.4971 0.9271 0.202 Uiso 1 1 d R . . A 1
C5_a C 0.4990(4) 0.4665(5) 0.8963(8) 0.197(4) Uani 1 1 d . U . A 1
H5A_a H 0.4979 0.4655 0.8446 0.237 Uiso 1 1 d R . . A 1
H5B_a H 0.5232 0.4909 0.9114 0.237 Uiso 1 1 d R . . A 1
C6_a C 0.4953(4) 0.4279(5) 0.9257(8) 0.197(4) Uani 1 1 d . U . A 1
H6A_a H 0.5230 0.4343 0.9338 0.236 Uiso 1 1 d R . . A 1
H6B_a H 0.4824 0.4059 0.8919 0.236 Uiso 1 1 d R . . A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy18 O113 2.280(3) . ?
Dy18 O136 2.466(2) . ?
Dy18 O141 2.181(3) . ?
Dy18 O160 2.400(2) 10_666 ?
Dy18 O184 2.482(2) . ?
Dy18 O248 2.440(2) . ?
Dy18 O135 2.299(2) . ?
Dy18 N246 2.461(3) . ?
Ni13 O23 2.095(2) . ?
Ni13 O160 2.057(2) . ?
Ni13 O248 2.101(2) . ?
Ni13 O248 2.135(2) 10_666 ?
Ni13 O135 2.019(2) . ?
Ni13 N142 2.016(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C53 1.469(10) . ?
C4 C627 1.551(8) . ?
O23 H23 0.858(9) . ?
O23 C728 1.408(5) . ?
O63 C378 1.383(6) . ?
O63 C7 1.432(8) . ?
C80 H80 0.9500 . ?
C80 C16 1.364(7) . ?
C80 C177 1.422(6) . ?
O101 C31 1.430(5) . ?
O101 C454 1.375(4) . ?
O113 C257 1.312(4) . ?
O136 C757 1.238(5) . ?
O141 C583 1.305(4) . ?
O160 Dy18 2.400(2) 10_666 ?
O160 C713 1.353(4) . ?
O184 C670 1.390(4) . ?
O184 C674 1.435(5) . ?
C212 H21A 0.9900 . ?
C212 H21B 0.9900 . ?
C212 C214 1.522(6) . ?
C212 C307 1.446(7) . ?
C239 H239 0.9500 . ?
C239 C126 1.356(5) . ?
C239 C139 1.432(5) . ?
O248 Ni13 2.135(2) 10_666 ?
O248 C512 1.372(4) . ?
C16 H16 0.9500 . ?
C16 C46 1.409(8) . ?
C29 H29 0.9500 . ?
C29 C123 1.406(5) . ?
C29 C454 1.368(5) . ?
C53 H53 0.9500 . ?
C53 C9 1.282(9) . ?
C58 H58A 0.9500 . ?
C58 H58B 0.9500 . ?
C58 C307 1.361(8) . ?
C88 C59 1.443(5) . ?
C88 C411 1.419(5) . ?
C88 C544 1.412(5) . ?
C110 H110 0.9500 . ?
C110 C123 1.362(6) . ?
C110 C172 1.427(5) . ?
C126 H126 0.9500 . ?
C126 C379 1.418(6) . ?
O135 C544 1.328(4) . ?
C139 C91 1.421(5) . ?
C139 C360 1.418(5) . ?
C2 H2 0.9500 . ?
C2 C551 1.513(7) . ?
C2 C755 1.315(7) . ?
C18 H18 0.9500 . ?
C18 C177 1.409(6) . ?
C18 C574 1.376(5) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C46 H46 0.9500 . ?
C46 C168 1.365(7) . ?
C59 H59 0.9500 . ?
C59 N142 1.285(5) . ?
C91 C1 1.414(5) . ?
C91 C422 1.423(5) . ?
C123 C551 1.524(6) . ?
N142 C574 1.416(5) . ?
C168 H168 0.9500 . ?
C168 C459 1.416(6) . ?
C172 C257 1.411(5) . ?
C172 C757 1.426(6) . ?
C177 C459 1.423(6) . ?
C214 C411 1.370(6) . ?
C214 C469 1.407(6) . ?
C1 H1 0.9500 . ?
C1 C363 1.381(5) . ?
N246 C363 1.426(5) . ?
N246 C504 1.300(5) . ?
C257 C454 1.428(5) . ?
C307 H307 0.9500 . ?
C321 H321 0.9500 . ?
C321 C396 1.411(5) . ?
C321 C627 1.374(6) . ?
C345 H34A 0.9800 . ?
C345 H34B 0.9800 . ?
C345 H34C 0.9800 . ?
C345 C728 1.535(6) . ?
C360 H360 0.9500 . ?
C360 C512 1.364(5) . ?
C363 C512 1.437(5) . ?
C378 C583 1.427(6) . ?
C378 C716 1.382(6) . ?
C379 H379 0.9500 . ?
C379 C422 1.370(6) . ?
C396 C504 1.434(6) . ?
C396 C583 1.422(5) . ?
C411 H411 0.9500 . ?
C422 H422 0.9500 . ?
C459 C635 1.426(6) . ?
C469 H469 0.9500 . ?
C469 C670 1.374(5) . ?
C504 H504 0.9500 . ?
C544 C670 1.416(5) . ?
C551 H55A 0.9900 . ?
C551 H55B 0.9900 . ?
C574 C713 1.439(5) . ?
C627 C716 1.402(7) . ?
C635 H635 0.9500 . ?
C635 C713 1.360(5) . ?
C674 H67A 0.9800 . ?
C674 H67B 0.9800 . ?
C674 H67C 0.9800 . ?
C716 H716 0.9500 . ?
C728 H72A 0.9900 . ?
C728 H72B 0.9900 . ?
C755 H75A 0.9500 . ?
C755 H75B 0.9500 . ?
C757 H757 0.9500 . ?
O3 C8_a 1.425(10) . ?
O3 C10_a 1.456(12) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8_a H8A_a 0.9699 . ?
C8_a H8B_a 0.9702 . ?
C8_a C6_a 1.464(15) . ?
C9 H9A 0.9300 . ?
C9 H9B 0.9307 . ?
C10_a H10A_a 0.9699 . ?
C10_a H10B_a 0.9703 . ?
C10_a C5_a 1.442(17) . ?
C5_a H5A_a 0.9699 . ?
C5_a H5B_a 0.9702 . ?
C5_a C6_a 1.511(19) . ?
C6_a H6A_a 0.9701 . ?
C6_a H6B_a 0.9697 . ?

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
O113 Dy18 O136 70.98(9) . . ?
O113 Dy18 O160 146.98(8) . 10_666 ?
O113 Dy18 O184 126.76(9) . . ?
O113 Dy18 O248 76.92(8) . . ?
O113 Dy18 O135 86.07(9) . . ?
O113 Dy18 N246 77.68(9) . . ?
O136 Dy18 O184 68.17(9) . . ?
O141 Dy18 O113 113.33(9) . . ?
O141 Dy18 O136 72.13(9) . . ?
O141 Dy18 O160 86.87(9) . 10_666 ?
O141 Dy18 O184 84.74(9) . . ?
O141 Dy18 O248 136.92(8) . . ?
O141 Dy18 O135 149.27(9) . . ?
O141 Dy18 N246 74.22(10) . . ?
O160 Dy18 O136 141.96(9) 10_666 . ?
O160 Dy18 O184 78.85(8) 10_666 . ?
O160 Dy18 O248 70.78(8) 10_666 . ?
O160 Dy18 N246 83.65(9) 10_666 . ?
O248 Dy18 O136 144.40(9) . . ?
O248 Dy18 O184 123.97(8) . . ?
O248 Dy18 N246 67.24(9) . . ?
O135 Dy18 O136 93.88(9) . . ?
O135 Dy18 O160 88.42(8) . 10_666 ?
O135 Dy18 O184 64.56(8) . . ?
O135 Dy18 O248 68.59(8) . . ?
O135 Dy18 N246 135.28(9) . . ?
N246 Dy18 O136 118.63(9) . . ?
N246 Dy18 O184 153.29(10) . . ?
O23 Ni13 O248 88.37(9) . . ?
O23 Ni13 O248 170.80(9) . 10_666 ?
O160 Ni13 O23 95.76(10) . . ?
O160 Ni13 O248 83.91(9) . 10_666 ?
O160 Ni13 O248 106.86(9) . . ?
O248 Ni13 O248 82.95(9) . 10_666 ?
O135 Ni13 O23 89.39(10) . . ?
O135 Ni13 O160 170.77(9) . . ?
O135 Ni13 O248 80.87(9) . . ?
O135 Ni13 O248 92.21(9) . 10_666 ?
N142 Ni13 O23 91.00(11) . . ?
N142 Ni13 O160 81.85(11) . . ?
N142 Ni13 O248 98.04(10) . 10_666 ?
N142 Ni13 O248 171.29(11) . . ?
N142 Ni13 O135 90.43(11) . . ?
H4A C4 H4B 108.0 . . ?
C53 C4 H4A 109.4 . . ?
C53 C4 H4B 109.4 . . ?
C53 C4 C627 111.0(7) . . ?
C627 C4 H4A 109.4 . . ?
C627 C4 H4B 109.4 . . ?
Ni13 O23 H23 112.1(14) . . ?
C728 O23 Ni13 134.7(2) . . ?
C728 O23 H23 106.0(14) . . ?
C378 O63 C7 120.3(5) . . ?
C16 C80 H80 119.3 . . ?
C16 C80 C177 121.4(5) . . ?
C177 C80 H80 119.3 . . ?
C454 O101 C31 116.8(3) . . ?
C257 O113 Dy18 134.2(2) . . ?
C757 O136 Dy18 129.7(2) . . ?
C583 O141 Dy18 141.7(2) . . ?
Ni13 O160 Dy18 104.27(11) . 10_666 ?
C713 O160 Dy18 119.4(2) . 10_666 ?
C713 O160 Ni13 108.4(2) . . ?
C670 O184 Dy18 119.0(2) . . ?
C670 O184 C674 117.5(3) . . ?
C674 O184 Dy18 123.0(2) . . ?
H21A C212 H21B 107.5 . . ?
C214 C212 H21A 108.4 . . ?
C214 C212 H21B 108.4 . . ?
C307 C212 H21A 108.4 . . ?
C307 C212 H21B 108.4 . . ?
C307 C212 C214 115.4(5) . . ?
C126 C239 H239 119.7 . . ?
C126 C239 C139 120.6(4) . . ?
C139 C239 H239 119.7 . . ?
Ni13 O248 Dy18 100.57(10) 10_666 . ?
Ni13 O248 Dy18 100.83(8) . . ?
Ni13 O248 Ni13 97.06(9) . 10_666 ?
C512 O248 Dy18 112.79(18) . . ?
C512 O248 Ni13 118.39(19) . 10_666 ?
C512 O248 Ni13 123.4(2) . . ?
C80 C16 H16 120.4 . . ?
C80 C16 C46 119.2(5) . . ?
C46 C16 H16 120.4 . . ?
C123 C29 H29 118.9 . . ?
C454 C29 H29 118.9 . . ?
C454 C29 C123 122.2(4) . . ?
C4 C53 H53 114.0 . . ?
C9 C53 C4 131.9(8) . . ?
C9 C53 H53 114.0 . . ?
H58A C58 H58B 120.0 . . ?
C307 C58 H58A 120.0 . . ?
C307 C58 H58B 120.0 . . ?
C411 C88 C59 117.9(3) . . ?
C544 C88 C59 123.8(3) . . ?
C544 C88 C411 118.2(3) . . ?
C123 C110 H110 119.3 . . ?
C123 C110 C172 121.4(3) . . ?
C172 C110 H110 119.3 . . ?
C239 C126 H126 119.5 . . ?
C239 C126 C379 121.1(4) . . ?
C379 C126 H126 119.5 . . ?
Ni13 O135 Dy18 108.37(10) . . ?
C544 O135 Dy18 126.2(2) . . ?
C544 O135 Ni13 123.1(2) . . ?
C91 C139 C239 119.0(3) . . ?
C360 C139 C239 121.8(3) . . ?
C360 C139 C91 119.2(3) . . ?
C551 C2 H2 117.7 . . ?
C755 C2 H2 117.7 . . ?
C755 C2 C551 124.5(5) . . ?
C177 C18 H18 119.2 . . ?
C574 C18 H18 119.2 . . ?
C574 C18 C177 121.5(4) . . ?
O101 C31 H31A 109.5 . . ?
O101 C31 H31B 109.5 . . ?
O101 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C16 C46 H46 119.3 . . ?
C168 C46 C16 121.3(5) . . ?
C168 C46 H46 119.3 . . ?
C88 C59 H59 117.2 . . ?
N142 C59 C88 125.6(3) . . ?
N142 C59 H59 117.2 . . ?
C1 C91 C139 119.0(3) . . ?
C1 C91 C422 122.6(3) . . ?
C422 C91 C139 118.4(4) . . ?
C29 C123 C551 119.6(4) . . ?
C110 C123 C29 118.4(3) . . ?
C110 C123 C551 122.0(4) . . ?
C59 N142 Ni13 125.9(3) . . ?
C59 N142 C574 123.9(3) . . ?
C574 N142 Ni13 110.2(2) . . ?
C46 C168 H168 119.6 . . ?
C46 C168 C459 120.8(5) . . ?
C459 C168 H168 119.6 . . ?
C257 C172 C110 120.0(4) . . ?
C257 C172 C757 122.3(3) . . ?
C757 C172 C110 117.7(3) . . ?
C18 C177 C80 122.5(4) . . ?
C18 C177 C459 118.5(4) . . ?
C459 C177 C80 118.9(4) . . ?
C411 C214 C212 122.1(4) . . ?
C411 C214 C469 118.7(3) . . ?
C469 C214 C212 119.0(4) . . ?
C91 C1 H1 119.5 . . ?
C363 C1 C91 121.1(3) . . ?
C363 C1 H1 119.5 . . ?
C363 N246 Dy18 112.2(2) . . ?
C504 N246 Dy18 128.5(3) . . ?
C504 N246 C363 119.1(3) . . ?
O113 C257 C172 123.1(3) . . ?
O113 C257 C454 119.5(3) . . ?
C172 C257 C454 117.4(3) . . ?
C212 C307 H307 118.7 . . ?
C58 C307 C212 122.6(6) . . ?
C58 C307 H307 118.7 . . ?
C396 C321 H321 119.2 . . ?
C627 C321 H321 119.2 . . ?
C627 C321 C396 121.5(4) . . ?
H34A C345 H34B 109.5 . . ?
H34A C345 H34C 109.5 . . ?
H34B C345 H34C 109.5 . . ?
C728 C345 H34A 109.5 . . ?
C728 C345 H34B 109.5 . . ?
C728 C345 H34C 109.5 . . ?
C139 C360 H360 119.4 . . ?
C512 C360 C139 121.2(3) . . ?
C512 C360 H360 119.4 . . ?
C1 C363 N246 124.0(3) . . ?
C1 C363 C512 119.5(3) . . ?
N246 C363 C512 116.3(3) . . ?
O63 C378 C583 115.3(4) . . ?
O63 C378 C716 122.9(4) . . ?
C716 C378 C583 121.7(4) . . ?
C126 C379 H379 120.3 . . ?
C422 C379 C126 119.5(4) . . ?
C422 C379 H379 120.3 . . ?
C321 C396 C504 117.4(4) . . ?
C321 C396 C583 119.7(4) . . ?
C583 C396 C504 122.8(3) . . ?
C88 C411 H411 118.6 . . ?
C214 C411 C88 122.9(4) . . ?
C214 C411 H411 118.6 . . ?
C91 C422 H422 119.3 . . ?
C379 C422 C91 121.5(4) . . ?
C379 C422 H422 119.3 . . ?
O101 C454 C257 113.0(3) . . ?
C29 C454 O101 126.5(3) . . ?
C29 C454 C257 120.5(3) . . ?
C168 C459 C177 118.4(4) . . ?
C168 C459 C635 122.5(4) . . ?
C177 C459 C635 119.2(4) . . ?
C214 C469 H469 120.1 . . ?
C670 C469 C214 119.7(4) . . ?
C670 C469 H469 120.1 . . ?
N246 C504 C396 127.7(4) . . ?
N246 C504 H504 116.2 . . ?
C396 C504 H504 116.2 . . ?
O248 C512 C363 117.9(3) . . ?
C360 C512 O248 122.1(3) . . ?
C360 C512 C363 120.0(3) . . ?
C88 C544 C670 117.9(3) . . ?
O135 C544 C88 125.2(3) . . ?
O135 C544 C670 116.8(3) . . ?
C2 C551 C123 111.6(4) . . ?
C2 C551 H55A 109.3 . . ?
C2 C551 H55B 109.3 . . ?
C123 C551 H55A 109.3 . . ?
C123 C551 H55B 109.3 . . ?
H55A C551 H55B 108.0 . . ?
C18 C574 N142 125.6(3) . . ?
C18 C574 C713 120.0(4) . . ?
N142 C574 C713 114.3(3) . . ?
O141 C583 C378 119.9(4) . . ?
O141 C583 C396 122.8(4) . . ?
C396 C583 C378 117.3(4) . . ?
C321 C627 C4 121.9(5) . . ?
C321 C627 C716 119.6(4) . . ?
C716 C627 C4 118.4(5) . . ?
C459 C635 H635 119.2 . . ?
C713 C635 C459 121.5(4) . . ?
C713 C635 H635 119.2 . . ?
O184 C670 C544 112.9(3) . . ?
C469 C670 O184 124.6(3) . . ?
C469 C670 C544 122.5(3) . . ?
O184 C674 H67A 109.5 . . ?
O184 C674 H67B 109.5 . . ?
O184 C674 H67C 109.5 . . ?
H67A C674 H67B 109.5 . . ?
H67A C674 H67C 109.5 . . ?
H67B C674 H67C 109.5 . . ?
O160 C713 C574 118.2(3) . . ?
O160 C713 C635 122.6(3) . . ?
C635 C713 C574 119.2(4) . . ?
C378 C716 C627 120.1(4) . . ?
C378 C716 H716 119.9 . . ?
C627 C716 H716 119.9 . . ?
O23 C728 C345 110.9(3) . . ?
O23 C728 H72A 109.5 . . ?
O23 C728 H72B 109.5 . . ?
C345 C728 H72A 109.5 . . ?
C345 C728 H72B 109.5 . . ?
H72A C728 H72B 108.0 . . ?
C2 C755 H75A 120.0 . . ?
C2 C755 H75B 120.0 . . ?
H75A C755 H75B 120.0 . . ?
O136 C757 C172 126.9(3) . . ?
O136 C757 H757 116.5 . . ?
C172 C757 H757 116.5 . . ?
C8_a O3 C10_a 110.8(9) . . ?
O63 C7 H7A 109.5 . . ?
O63 C7 H7B 109.5 . . ?
O63 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C8_a H8A_a 113.7 . . ?
O3 C8_a H8B_a 111.3 . . ?
O3 C8_a C6_a 108.3(10) . . ?
H8A_a C8_a H8B_a 109.5 . . ?
C6_a C8_a H8A_a 112.7 . . ?
C6_a C8_a H8B_a 100.5 . . ?
C53 C9 H9A 120.3 . . ?
C53 C9 H9B 119.7 . . ?
H9A C9 H9B 120.0 . . ?
O3 C10_a H10A_a 110.1 . . ?
O3 C10_a H10B_a 109.2 . . ?
H10A_a C10_a H10B_a 109.5 . . ?
C5_a C10_a O3 101.5(11) . . ?
C5_a C10_a H10A_a 111.8 . . ?
C5_a C10_a H10B_a 114.5 . . ?
C10_a C5_a H5A_a 105.5 . . ?
C10_a C5_a H5B_a 107.8 . . ?
C10_a C5_a C6_a 109.4(12) . . ?
H5A_a C5_a H5B_a 109.5 . . ?
C6_a C5_a H5A_a 110.2 . . ?
C6_a C5_a H5B_a 114.1 . . ?
C8_a C6_a C5_a 99.5(12) . . ?
C8_a C6_a H6A_a 111.3 . . ?
C8_a C6_a H6B_a 119.0 . . ?
C5_a C6_a H6A_a 104.7 . . ?
C5_a C6_a H6B_a 111.5 . . ?
H6A_a C6_a H6B_a 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy18 O113 C257 C172 33.6(5) . . . . ?
Dy18 O113 C257 C454 -148.3(3) . . . . ?
Dy18 O136 C757 C172 -20.8(6) . . . . ?
Dy18 O141 C583 C378 164.3(3) . . . . ?
Dy18 O141 C583 C396 -13.0(6) . . . . ?
Dy18 O160 C713 C574 -96.5(3) 10_666 . . . ?
Dy18 O160 C713 C635 83.4(4) 10_666 . . . ?
Dy18 O184 C670 C469 177.1(3) . . . . ?
Dy18 O184 C670 C544 -5.9(4) . . . . ?
Dy18 O248 C512 C360 149.2(3) . . . . ?
Dy18 O248 C512 C363 -31.5(3) . . . . ?
Dy18 O135 C544 C88 -175.2(2) . . . . ?
Dy18 O135 C544 C670 5.4(4) . . . . ?
Dy18 N246 C363 C1 -151.0(3) . . . . ?
Dy18 N246 C363 C512 23.7(3) . . . . ?
Dy18 N246 C504 C396 9.3(5) . . . . ?
Ni13 O23 C728 C345 -152.5(3) . . . . ?
Ni13 O160 C713 C574 22.5(4) . . . . ?
Ni13 O160 C713 C635 -157.6(3) . . . . ?
Ni13 O248 C512 C360 -93.8(3) 10_666 . . . ?
Ni13 O248 C512 C360 27.8(4) . . . . ?
Ni13 O248 C512 C363 85.5(3) 10_666 . . . ?
Ni13 O248 C512 C363 -152.9(2) . . . . ?
Ni13 O135 C544 C88 23.9(4) . . . . ?
Ni13 O135 C544 C670 -155.6(2) . . . . ?
Ni13 N142 C574 C18 163.4(3) . . . . ?
Ni13 N142 C574 C713 -14.8(3) . . . . ?
C4 C627 C716 C378 177.9(5) . . . . ?
O63 C378 C583 O141 -1.6(6) . . . . ?
O63 C378 C583 C396 175.9(4) . . . . ?
O63 C378 C716 C627 -174.5(4) . . . . ?
C80 C16 C46 C168 -0.1(8) . . . . ?
C80 C177 C459 C168 0.0(6) . . . . ?
C80 C177 C459 C635 178.7(4) . . . . ?
O113 C257 C454 O101 1.8(4) . . . . ?
O113 C257 C454 C29 -177.9(3) . . . . ?
C212 C214 C411 C88 170.9(4) . . . . ?
C212 C214 C469 C670 -172.3(4) . . . . ?
C239 C126 C379 C422 0.6(6) . . . . ?
C239 C139 C91 C1 -177.7(3) . . . . ?
C239 C139 C91 C422 0.5(5) . . . . ?
C239 C139 C360 C512 177.8(3) . . . . ?
C16 C80 C177 C18 177.6(4) . . . . ?
C16 C80 C177 C459 -1.2(6) . . . . ?
C16 C46 C168 C459 -1.2(8) . . . . ?
C29 C123 C551 C2 60.8(5) . . . . ?
C53 C4 C627 C321 -107.0(7) . . . . ?
C53 C4 C627 C716 73.9(7) . . . . ?
C88 C59 N142 Ni13 -4.2(5) . . . . ?
C88 C59 N142 C574 177.7(3) . . . . ?
C88 C544 C670 O184 -178.7(3) . . . . ?
C88 C544 C670 C469 -1.6(5) . . . . ?
C110 C123 C551 C2 -119.0(5) . . . . ?
C110 C172 C257 O113 177.8(3) . . . . ?
C110 C172 C257 C454 -0.3(5) . . . . ?
C110 C172 C757 O136 178.1(4) . . . . ?
C126 C239 C139 C91 0.9(5) . . . . ?
C126 C239 C139 C360 -178.2(3) . . . . ?
C126 C379 C422 C91 0.8(6) . . . . ?
O135 C544 C670 O184 0.9(4) . . . . ?
O135 C544 C670 C469 178.0(3) . . . . ?
C139 C239 C126 C379 -1.5(6) . . . . ?
C139 C91 C1 C363 -1.4(5) . . . . ?
C139 C91 C422 C379 -1.3(6) . . . . ?
C139 C360 C512 O248 -179.8(3) . . . . ?
C139 C360 C512 C363 0.9(5) . . . . ?
C18 C177 C459 C168 -178.9(4) . . . . ?
C18 C177 C459 C635 -0.2(6) . . . . ?
C18 C574 C713 O160 176.0(3) . . . . ?
C18 C574 C713 C635 -3.9(5) . . . . ?
C31 O101 C454 C29 -1.0(5) . . . . ?
C31 O101 C454 C257 179.3(3) . . . . ?
C46 C168 C459 C177 1.2(7) . . . . ?
C46 C168 C459 C635 -177.5(5) . . . . ?
C59 C88 C411 C214 -174.3(3) . . . . ?
C59 C88 C544 O135 -3.0(5) . . . . ?
C59 C88 C544 C670 176.5(3) . . . . ?
C59 N142 C574 C18 -18.2(5) . . . . ?
C59 N142 C574 C713 163.7(3) . . . . ?
C91 C139 C360 C512 -1.2(5) . . . . ?
C91 C1 C363 N246 175.6(3) . . . . ?
C91 C1 C363 C512 1.0(5) . . . . ?
C123 C29 C454 O101 -179.9(3) . . . . ?
C123 C29 C454 C257 -0.2(5) . . . . ?
C123 C110 C172 C257 0.3(5) . . . . ?
C123 C110 C172 C757 178.8(3) . . . . ?
N142 C574 C713 O160 -5.7(4) . . . . ?
N142 C574 C713 C635 174.4(3) . . . . ?
C168 C459 C635 C713 176.4(4) . . . . ?
C172 C110 C123 C29 -0.3(5) . . . . ?
C172 C110 C123 C551 179.5(4) . . . . ?
C172 C257 C454 O101 -180.0(3) . . . . ?
C172 C257 C454 C29 0.3(5) . . . . ?
C177 C80 C16 C46 1.3(7) . . . . ?
C177 C18 C574 N142 -176.6(3) . . . . ?
C177 C18 C574 C713 1.4(5) . . . . ?
C177 C459 C635 C713 -2.3(6) . . . . ?
C214 C212 C307 C58 110.6(6) . . . . ?
C214 C469 C670 O184 177.0(3) . . . . ?
C214 C469 C670 C544 0.3(5) . . . . ?
C1 C91 C422 C379 176.7(4) . . . . ?
C1 C363 C512 O248 179.9(3) . . . . ?
C1 C363 C512 C360 -0.8(5) . . . . ?
N246 C363 C512 O248 5.0(4) . . . . ?
N246 C363 C512 C360 -175.8(3) . . . . ?
C257 C172 C757 O136 -3.4(6) . . . . ?
C307 C212 C214 C411 142.1(5) . . . . ?
C307 C212 C214 C469 -43.7(7) . . . . ?
C321 C396 C504 N246 -176.7(4) . . . . ?
C321 C396 C583 O141 176.4(4) . . . . ?
C321 C396 C583 C378 -1.0(5) . . . . ?
C321 C627 C716 C378 -1.2(7) . . . . ?
C360 C139 C91 C1 1.4(5) . . . . ?
C360 C139 C91 C422 179.5(3) . . . . ?
C363 N246 C504 C396 -176.0(3) . . . . ?
C396 C321 C627 C4 -179.6(5) . . . . ?
C396 C321 C627 C716 -0.6(6) . . . . ?
C411 C88 C59 N142 168.0(3) . . . . ?
C411 C88 C544 O135 -179.0(3) . . . . ?
C411 C88 C544 C670 0.4(5) . . . . ?
C411 C214 C469 C670 2.1(6) . . . . ?
C422 C91 C1 C363 -179.4(3) . . . . ?
C454 C29 C123 C110 0.2(5) . . . . ?
C454 C29 C123 C551 -179.5(3) . . . . ?
C459 C635 C713 O160 -175.6(3) . . . . ?
C459 C635 C713 C574 4.3(5) . . . . ?
C469 C214 C411 C88 -3.3(6) . . . . ?
C504 N246 C363 C1 33.5(5) . . . . ?
C504 N246 C363 C512 -151.8(3) . . . . ?
C504 C396 C583 O141 -2.2(6) . . . . ?
C504 C396 C583 C378 -179.5(4) . . . . ?
C544 C88 C59 N142 -8.1(5) . . . . ?
C544 C88 C411 C214 2.0(5) . . . . ?
C574 C18 C177 C80 -178.3(4) . . . . ?
C574 C18 C177 C459 0.6(6) . . . . ?
C583 C378 C716 C627 1.9(7) . . . . ?
C583 C396 C504 N246 1.9(6) . . . . ?
C627 C4 C53 C9 -116.7(9) . . . . ?
C627 C321 C396 C504 -179.7(4) . . . . ?
C627 C321 C396 C583 1.7(6) . . . . ?
C674 O184 C670 C469 5.6(5) . . . . ?
C674 O184 C670 C544 -177.4(3) . . . . ?
C716 C378 C583 O141 -178.2(4) . . . . ?
C716 C378 C583 C396 -0.8(6) . . . . ?
C755 C2 C551 C123 -109.5(5) . . . . ?
C757 C172 C257 O113 -0.6(5) . . . . ?
C757 C172 C257 C454 -178.7(3) . . . . ?
O3 C8_a C6_a C5_a 23.8(13) . . . . ?
O3 C10_a C5_a C6_a 28.6(15) . . . . ?
C7 O63 C378 C583 -171.1(6) . . . . ?
C7 O63 C378 C716 5.5(9) . . . . ?
C8_a O3 C10_a C5_a -12.7(12) . . . . ?
C10_a O3 C8_a C6_a -8.0(12) . . . . ?
C10_a C5_a C6_a C8_a -33.0(15) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 7.2 0.4 ?
2 0.000 0.000 0.500 330.0 13.6 ?
3 0.030 0.213 0.269 8.0 0.4 ?
4 -0.030 0.787 0.731 8.0 0.4 ?
5 0.093 0.889 0.528 7.2 0.0 ?
6 0.111 0.204 0.528 7.2 0.0 ?
7 0.120 0.484 0.935 8.0 0.4 ?
8 0.130 0.574 0.194 7.2 0.0 ?
9 0.150 0.697 0.398 8.0 0.4 ?
10 0.183 0.970 0.269 8.0 0.4 ?
11 0.204 0.093 0.472 7.2 0.0 ?
12 0.213 0.183 0.731 8.0 0.4 ?
13 0.222 0.463 0.139 7.2 0.0 ?
14 0.333 0.667 0.167 330.0 13.6 ?
15 0.241 0.778 0.139 7.2 0.0 ?
16 0.303 0.454 0.398 8.0 0.4 ?
17 0.333 0.667 0.667 7.2 0.4 ?
18 0.363 0.880 0.935 8.0 0.4 ?
19 0.426 0.556 0.194 7.2 0.0 ?
20 0.444 0.870 0.194 7.2 0.0 ?
21 0.454 0.150 0.602 8.0 0.4 ?
22 0.463 0.241 0.861 7.2 0.0 ?
23 0.484 0.363 0.065 8.0 0.4 ?
24 0.516 0.637 0.935 8.0 0.4 ?
25 0.537 0.759 0.139 7.2 0.0 ?
26 0.546 0.850 0.398 8.0 0.4 ?
27 0.556 0.130 0.806 7.2 0.0 ?
28 0.667 0.333 -0.167 330.0 13.6 ?
29 0.574 0.444 0.806 7.2 0.0 ?
30 0.637 0.120 0.065 8.0 0.4 ?
31 0.667 0.333 0.333 7.2 0.4 ?
32 0.697 0.546 0.602 8.0 0.4 ?
33 0.759 0.222 0.861 7.2 0.0 ?
34 0.778 0.537 0.861 7.2 0.0 ?
35 0.787 0.817 0.269 8.0 0.4 ?
36 0.796 0.907 0.528 7.2 0.0 ?
37 0.817 0.030 0.731 8.0 0.4 ?
38 0.850 0.303 0.602 8.0 0.4 ?
39 0.870 0.426 0.806 7.2 0.0 ?
40 0.880 0.516 0.065 8.0 0.4 ?
41 0.889 0.796 0.472 7.2 0.0 ?
42 0.907 0.111 0.472 7.2 0.0 ?

# start Validation Reply Form
_vrf_CHEMW03_shelx               
;
PROBLEM:The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.99 <> 1.01
           From the CIF: _cell_formula_units_Z                    9
           From the CIF: _chemical_formula_weight          2478.64
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01  118.00 1417.30
           H         1.01  118.00  118.94
           Dy      162.50    2.00  325.00
           N        14.01    4.00   56.03
           Ni       58.69    2.00  117.38
           O        16.00   22.00  351.98

           Calculated formula weight             2386.63
RESPONSE: The sample diffracted very weakly at high angles and the
reflections were completely absent. Therefore PLATON / SQUEEZE
programm as used to remove those disordered solvent molecules and 
obtained the total electron count of 49.4 per unit cell and was 
assigned to two EtOH molecules. The reported formula, molecular weight, 
F000, density etc include the contribution of disordered solvents 
(2 EtOH) which were removed by SQUEEZE.
;
# end Validation Reply Form

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

data_10_CCDC_1406226
_database_code_depnum_ccdc_archive 'CCDC 1406226'
_audit_update_record             
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_audit_creation_date             2014-07-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C102 H110 Dy2 N10 Ni2 O18, 2(Cl O4)'
_chemical_formula_sum            'C102 H110 Cl2 Dy2 N10 Ni2 O26'
_chemical_formula_weight         2405.31
_chemical_melting_point          ?
_chemical_oxdiff_formula         Ni2Dy2C120H150N14O30
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.8855(6)
_cell_length_b                   17.2105(11)
_cell_length_c                   20.5903(11)
_cell_angle_alpha                90
_cell_angle_beta                 96.747(4)
_cell_angle_gamma                90
_cell_volume                     5590.3(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.7690
_cell_measurement_theta_min      2.9240
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2444
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13138
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.188
_diffrn_reflns_theta_min         2.536
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -38.00   50.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -18.1690   57.0000  -30.0000 88

#__ type_ start__ end____ width___ exp.time_
  2 omega  -32.00   43.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -18.1690   57.0000   90.0000 75

#__ type_ start__ end____ width___ exp.time_
  3 omega   26.00   51.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -18.1690   57.0000  150.0000 25

#__ type_ start__ end____ width___ exp.time_
  4 omega  -36.00   10.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -18.1690   57.0000  150.0000 46

#__ type_ start__ end____ width___ exp.time_
  5 omega  -89.00  -53.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -18.1690  178.0000  120.0000 36

#__ type_ start__ end____ width___ exp.time_
  6 omega  -80.00  -43.00   1.0000    2.5400
omega____ theta____ kappa____ phi______ frames
    -      -18.1690 -178.0000  -60.0000 37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0073669000
_diffrn_orient_matrix_UB_12      0.0271064000
_diffrn_orient_matrix_UB_13      -0.0259709000
_diffrn_orient_matrix_UB_21      0.0372428000
_diffrn_orient_matrix_UB_22      -0.0128569000
_diffrn_orient_matrix_UB_23      -0.0125947000
_diffrn_orient_matrix_UB_31      -0.0240314000
_diffrn_orient_matrix_UB_32      -0.0282308000
_diffrn_orient_matrix_UB_33      -0.0191528000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9655
_reflns_number_total             13129
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.236
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         13129
_refine_ls_number_restraints     446
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0464
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0578P)²+3.7604P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1220
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O13-Cl1
 1.43 with sigma of 0.02
 O11-Cl1
 1.43 with sigma of 0.02
 O14-Cl1
 1.43 with sigma of 0.02
 O12-Cl1
 1.43 with sigma of 0.02
 Cl1-O15
 1.43 with sigma of 0.02
 C43-N3
 1.32 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Fixed Sof: O13(0.5) O12(0.5) O11(0.5) O15(0.5) O11A(0.5) O13A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C29(H29A,H29B)
5.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C5(H5), C39(H39), C37(H37), C3(H3), C20(H20), C9(H9), C13(H13),
 C36(H36), C17(H17), C11(H11), C34(H34), C26(H26), C16(H16), C38(H38), C32(H32),
  C15(H15), C46(H46), C24(H24), C41(H41), C49(H49), C43(H43), C18(H18)
5.c X=CH2 refined with riding coordinates:
 C10(H10A,H10B), C31(H31A,H31B)
5.d Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C22(H22A,H22B,H22C), C51(H51A,H51B,H51C), C50(H50A,H50B,
 H50C), C48(H48A,H48B,H48C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C1(H1A,
 H1B,H1C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.47165(2) 0.88624(2) 0.38333(2) 0.03094(7) Uani 1 1 d . . . . .
Ni1 Ni 0.53791(3) 1.06190(3) 0.45518(2) 0.02669(12) Uani 1 1 d . . . . .
C47 C 0.5784(6) 0.5779(4) 0.4796(6) 0.165(5) Uani 1 1 d . . . . .
H47A H 0.6160 0.5525 0.4515 0.247 Uiso 1 1 calc GR . . . .
H47B H 0.5195 0.5636 0.4650 0.247 Uiso 1 1 calc GR . . . .
H47C H 0.5934 0.5610 0.5249 0.247 Uiso 1 1 calc GR . . . .
O5 O 0.48128(18) 0.87297(18) 0.27986(15) 0.0417(7) Uani 1 1 d . . . . .
O4 O 0.4132(2) 0.8799(3) 0.15913(18) 0.0708(12) Uani 1 1 d . . . . .
O3 O 0.48095(15) 1.02130(15) 0.36683(13) 0.0291(6) Uani 1 1 d . . . . .
O7 O 0.3848(2) 0.77375(18) 0.36221(18) 0.0526(9) Uani 1 1 d . . . . .
C22 C 0.3717(5) 0.8866(5) 0.0949(3) 0.097(3) Uani 1 1 d . . . . .
H22A H 0.3953 0.8486 0.0666 0.145 Uiso 1 1 calc GR . . . .
H22B H 0.3800 0.9392 0.0784 0.145 Uiso 1 1 calc GR . . . .
H22C H 0.3110 0.8768 0.0951 0.145 Uiso 1 1 calc GR . . . .
C51 C 0.5866(7) 1.3614(5) 0.4078(7) 0.188(6) Uani 1 1 d . . . . .
H51A H 0.6187 1.3700 0.3706 0.282 Uiso 1 1 calc GR . . . .
H51B H 0.6260 1.3547 0.4478 0.282 Uiso 1 1 calc GR . . . .
H51C H 0.5500 1.4063 0.4128 0.282 Uiso 1 1 calc GR . . . .
O8 O 0.53978(18) 0.77755(16) 0.43570(17) 0.0443(8) Uani 1 1 d . . . . .
C8 C 0.9701(3) 1.0637(3) 0.5886(3) 0.0590(14) Uani 1 1 d . . . . .
H8A H 0.9839 1.0162 0.6148 0.071 Uiso 1 1 calc R . . . .
H8B H 0.9973 1.0595 0.5479 0.071 Uiso 1 1 calc R . . . .
N1 N 0.6355(2) 1.07751(19) 0.40325(16) 0.0312(7) Uani 1 1 d . . . . .
N2 N 0.6246(2) 0.89711(19) 0.37171(17) 0.0331(8) Uani 1 1 d . . . . .
N4 N 0.5881(3) 0.6624(2) 0.4755(3) 0.0673(14) Uani 1 1 d . . . . .
C30 C 0.6963(5) 0.8832(6) 0.0366(4) 0.102(3) Uani 1 1 d . . . . .
H30 H 0.7197 0.8965 -0.0023 0.123 Uiso 1 1 calc R . . . .
C5 C 0.8365(3) 1.0754(3) 0.5086(2) 0.0400(10) Uani 1 1 d . . . . .
H5 H 0.8711 1.0754 0.4740 0.048 Uiso 1 1 calc R . . . .
C39 C 0.8053(3) 0.8745(3) 0.6239(2) 0.0438(11) Uani 1 1 d . . . . .
H39 H 0.7782 0.8886 0.6609 0.053 Uiso 1 1 calc R . . . .
C50 C 0.4705(5) 1.2933(4) 0.3404(4) 0.099(2) Uani 1 1 d . . . . .
H50A H 0.4238 1.3273 0.3496 0.148 Uiso 1 1 calc GR . . . .
H50B H 0.4490 1.2405 0.3319 0.148 Uiso 1 1 calc GR . . . .
H50C H 0.4950 1.3127 0.3020 0.148 Uiso 1 1 calc GR . . . .
O9 O 0.50056(17) 1.17290(16) 0.42685(14) 0.0364(6) Uani 1 1 d . . . . .
C4 C 0.8746(3) 1.0693(3) 0.5715(2) 0.0427(11) Uani 1 1 d . . . . .
O6 O 0.55194(15) 0.94190(14) 0.47839(13) 0.0265(6) Uani 1 1 d . . . . .
C37 C 0.9278(3) 0.8287(4) 0.5778(3) 0.0635(15) Uani 1 1 d . . . . .
H37 H 0.9852 0.8120 0.5836 0.076 Uiso 1 1 calc R . . . .
N5 N 0.5351(3) 1.2925(3) 0.3964(3) 0.0732(15) Uani 1 1 d . . . . .
C12 C 0.6045(2) 1.0842(2) 0.3361(2) 0.0343(9) Uani 1 1 d . . . . .
C3 C 0.8234(3) 1.0690(2) 0.6226(2) 0.0387(10) Uani 1 1 d . . . . .
H3 H 0.8485 1.0636 0.6666 0.046 Uiso 1 1 calc R . . . .
C21 C 0.5198(3) 1.0561(2) 0.3195(2) 0.0330(9) Uani 1 1 d . . . . .
N3 N 0.2563(3) 0.7341(2) 0.3207(2) 0.0562(11) Uani 1 1 d D . . . .
C33 C 0.6751(2) 0.8941(2) 0.4340(2) 0.0297(8) Uani 1 1 d . . . . .
C20 C 0.4825(3) 1.0643(2) 0.2570(2) 0.0352(9) Uani 1 1 d . . . . .
H20 H 0.4259 1.0467 0.2459 0.042 Uiso 1 1 calc R . . . .
C9 C 1.0055(4) 1.1341(5) 0.6272(3) 0.0773(19) Uani 1 1 d . . . . .
H9 H 0.9899 1.1831 0.6082 0.093 Uiso 1 1 calc R . . . .
C48 C 0.6636(4) 0.6929(3) 0.5090(4) 0.084(2) Uani 1 1 d . . . . .
H48A H 0.6778 0.6646 0.5501 0.126 Uiso 1 1 calc GR . . . .
H48B H 0.6555 0.7481 0.5184 0.126 Uiso 1 1 calc GR . . . .
H48C H 0.7098 0.6873 0.4817 0.126 Uiso 1 1 calc GR . . . .
C29 C 0.6869(4) 0.9488(4) 0.0842(3) 0.083(2) Uani 1 1 d . . . . .
H29A H 0.7440 0.9651 0.1041 0.100 Uiso 1 1 calc R . . . .
H29B H 0.6603 0.9938 0.0598 0.100 Uiso 1 1 calc R . . . .
C13 C 0.6467(3) 1.1194(3) 0.2898(2) 0.0445(11) Uani 1 1 d . . . . .
H13 H 0.7020 1.1395 0.3018 0.053 Uiso 1 1 calc R . . . .
C44 C 0.1963(4) 0.7135(5) 0.2657(4) 0.107(3) Uani 1 1 d . . . . .
H44A H 0.1845 0.6577 0.2670 0.160 Uiso 1 1 calc GR . . . .
H44B H 0.2198 0.7261 0.2251 0.160 Uiso 1 1 calc GR . . . .
H44C H 0.1436 0.7426 0.2676 0.160 Uiso 1 1 calc GR . . . .
C36 C 0.8862(3) 0.8336(3) 0.5164(3) 0.0513(12) Uani 1 1 d . . . . .
H36 H 0.9141 0.8185 0.4800 0.062 Uiso 1 1 calc R . . . .
C17 C 0.5317(4) 1.1389(4) 0.0955(3) 0.0655(16) Uani 1 1 d . . . . .
H17 H 0.5057 1.1438 0.0518 0.079 Uiso 1 1 calc R . . . .
C11 C 0.7146(2) 1.0836(2) 0.4254(2) 0.0350(9) Uani 1 1 d . . . . .
H11 H 0.7538 1.0901 0.3944 0.042 Uiso 1 1 calc R . . . .
C34 C 0.7566(3) 0.8674(2) 0.4431(2) 0.0373(10) Uani 1 1 d . . . . .
H34 H 0.7837 0.8528 0.4061 0.045 Uiso 1 1 calc R . . . .
C40 C 0.7598(3) 0.8814(2) 0.5610(2) 0.0327(9) Uani 1 1 d . . . . .
C35 C 0.8014(3) 0.8609(3) 0.5060(2) 0.0377(10) Uani 1 1 d . . . . .
C26 C 0.6689(3) 0.9247(3) 0.2028(2) 0.0548(13) Uani 1 1 d . . . . .
H26 H 0.7277 0.9347 0.2136 0.066 Uiso 1 1 calc R . . . .
C16 C 0.6148(4) 1.1651(4) 0.1123(3) 0.0711(17) Uani 1 1 d . . . . .
H16 H 0.6449 1.1872 0.0796 0.085 Uiso 1 1 calc R . . . .
C38 C 0.8874(3) 0.8480(3) 0.6333(3) 0.0579(13) Uani 1 1 d . . . . .
H38 H 0.9165 0.8427 0.6761 0.070 Uiso 1 1 calc R . . . .
C32 C 0.6597(3) 0.9075(3) 0.3193(2) 0.0379(10) Uani 1 1 d . . . . .
H32 H 0.7191 0.9164 0.3248 0.046 Uiso 1 1 calc R . . . .
C15 C 0.6530(4) 1.1592(4) 0.1750(3) 0.0666(16) Uani 1 1 d . . . . .
H15 H 0.7094 1.1775 0.1856 0.080 Uiso 1 1 calc R . . . .
C27 C 0.6185(3) 0.9072(3) 0.2534(2) 0.0445(11) Uani 1 1 d . . . . .
C46 C 0.5317(3) 0.7074(3) 0.4437(3) 0.0508(12) Uani 1 1 d . . . . .
H46 H 0.4802 0.6841 0.4252 0.061 Uiso 1 1 calc R . . . .
C6 C 0.7481(2) 1.0815(2) 0.4933(2) 0.0316(9) Uani 1 1 d . . . . .
C24 C 0.5471(4) 0.9124(4) 0.1228(3) 0.0639(15) Uani 1 1 d . . . . .
H24 H 0.5226 0.9153 0.0785 0.077 Uiso 1 1 calc R . . . .
C25 C 0.6343(4) 0.9277(4) 0.1381(2) 0.0635(15) Uani 1 1 d . . . . .
C7 C 0.6977(2) 1.0845(2) 0.5447(2) 0.0302(8) Uani 1 1 d . . . . .
C14 C 0.6093(3) 1.1260(3) 0.2247(2) 0.0488(12) Uani 1 1 d . . . . .
C2 C 0.7372(3) 1.0764(2) 0.6090(2) 0.0337(9) Uani 1 1 d . . . . .
C19 C 0.5259(3) 1.0984(3) 0.2079(2) 0.0439(11) Uani 1 1 d . . . . .
C45 C 0.2281(4) 0.7216(4) 0.3845(3) 0.0775(18) Uani 1 1 d . . . . .
H45A H 0.1749 0.7496 0.3869 0.116 Uiso 1 1 calc GR . . . .
H45B H 0.2713 0.7408 0.4186 0.116 Uiso 1 1 calc GR . . . .
H45C H 0.2191 0.6659 0.3909 0.116 Uiso 1 1 calc GR . . . .
C23 C 0.4971(3) 0.8936(3) 0.1697(2) 0.0558(14) Uani 1 1 d . . . . .
C41 C 0.6754(2) 0.9076(2) 0.5506(2) 0.0297(8) Uani 1 1 d . . . . .
H41 H 0.6469 0.9206 0.5872 0.036 Uiso 1 1 calc R . . . .
C49 C 0.5446(3) 1.2306(3) 0.4333(3) 0.0525(13) Uani 1 1 d . . . . .
H49 H 0.5896 1.2308 0.4681 0.063 Uiso 1 1 calc R . . . .
C43 C 0.3326(3) 0.7580(3) 0.3142(3) 0.0500(12) Uani 1 1 d D . . . .
H43 H 0.3489 0.7637 0.2715 0.060 Uiso 1 1 calc R . . . .
C28 C 0.5320(3) 0.8905(3) 0.2369(2) 0.0419(10) Uani 1 1 d . . . . .
C42 C 0.6336(2) 0.9145(2) 0.4893(2) 0.0267(8) Uani 1 1 d . . . . .
C18 C 0.4876(4) 1.1063(3) 0.1422(2) 0.0530(13) Uani 1 1 d . . . . .
H18 H 0.4311 1.0888 0.1305 0.064 Uiso 1 1 calc R . . . .
C10 C 1.0510(6) 1.1366(6) 0.6790(5) 0.119(3) Uani 1 1 d . . . . .
H10A H 1.0691 1.0898 0.7008 0.143 Uiso 1 1 calc R . . . .
H10B H 1.0684 1.1853 0.6976 0.143 Uiso 1 1 calc R . . . .
C31 C 0.6757(7) 0.8095(7) 0.0431(5) 0.142(4) Uani 1 1 d . . . . .
H31A H 0.6520 0.7929 0.0811 0.171 Uiso 1 1 calc R . . . .
H31B H 0.6845 0.7731 0.0099 0.171 Uiso 1 1 calc R . . . .
Cl1 Cl 0.3590(2) 0.53168(11) 0.35340(13) 0.1532(14) Uani 1 1 d D . . . .
O2 O 0.61329(16) 1.09284(16) 0.53629(14) 0.0320(6) Uani 1 1 d . . . . .
O1 O 0.68094(17) 1.07514(17) 0.65508(14) 0.0360(6) Uani 1 1 d . . . . .
C1 C 0.7147(3) 1.0620(3) 0.7216(2) 0.0471(11) Uani 1 1 d . . . . .
H1A H 0.7619 1.0977 0.7337 0.071 Uiso 1 1 calc GR . . . .
H1B H 0.7349 1.0083 0.7267 0.071 Uiso 1 1 calc GR . . . .
H1C H 0.6703 1.0709 0.7501 0.071 Uiso 1 1 calc GR . . . .
O13_a O 0.3567(7) 0.5699(6) 0.4224(5) 0.080(3) Uiso 0.5 1 d D . P A 1
O14 O 0.3487(6) 0.4542(3) 0.3532(5) 0.165(3) Uani 1 1 d D . . . .
O12 O 0.3578(6) 0.5750(4) 0.2969(4) 0.072(2) Uani 0.5 1 d D . P A .
O11_a O 0.3019(16) 0.4822(16) 0.3710(15) 0.255(11) Uiso 0.5 1 d D . P A 1
O15 O 0.4596(8) 0.5115(8) 0.3513(7) 0.146(5) Uani 0.5 1 d D . P A .
O11A_b O 0.2478(7) 0.5407(6) 0.3469(5) 0.102(3) Uiso 0.5 1 d . . P A 2
O13A_b O 0.3843(8) 0.5748(7) 0.4009(6) 0.099(4) Uiso 0.5 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 Ni1 3.4743(6) . ?
Dy1 Ni1 3.4635(6) 3_676 ?
Dy1 O5 2.166(3) . ?
Dy1 O3 2.356(3) . ?
Dy1 O7 2.387(3) . ?
Dy1 O8 2.358(3) . ?
Dy1 N2 2.476(3) . ?
Dy1 O6 2.406(3) . ?
Dy1 O2 2.283(3) 3_676 ?
Dy1 O1 2.548(3) 3_676 ?
Ni1 Dy1 3.4634(6) 3_676 ?
Ni1 O3 2.057(3) . ?
Ni1 N1 2.002(3) . ?
Ni1 O9 2.064(3) . ?
Ni1 O6 2.126(2) . ?
Ni1 O6 2.091(2) 3_676 ?
Ni1 O2 2.009(3) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C47 N4 1.466(8) . ?
O5 C28 1.300(5) . ?
O4 C22 1.411(7) . ?
O4 C23 1.347(6) . ?
O3 C21 1.352(5) . ?
O7 C43 1.242(6) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C51 N5 1.444(8) . ?
O8 C46 1.227(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C4 1.521(6) . ?
C8 C9 1.519(9) . ?
N1 C12 1.417(5) . ?
N1 C11 1.289(5) . ?
N2 C33 1.431(5) . ?
N2 C32 1.283(5) . ?
N4 C48 1.413(7) . ?
N4 C46 1.301(6) . ?
C30 H30 0.9500 . ?
C30 C29 1.515(10) . ?
C30 C31 1.321(11) . ?
C5 H5 0.9500 . ?
C5 C4 1.366(6) . ?
C5 C6 1.408(5) . ?
C39 H39 0.9500 . ?
C39 C40 1.411(6) . ?
C39 C38 1.375(7) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C50 N5 1.451(8) . ?
O9 C49 1.213(5) . ?
C4 C3 1.403(6) . ?
O6 Ni1 2.091(2) 3_676 ?
O6 C42 1.374(4) . ?
C37 H37 0.9500 . ?
C37 C36 1.360(7) . ?
C37 C38 1.414(7) . ?
N5 C49 1.308(6) . ?
C12 C21 1.432(6) . ?
C12 C13 1.370(6) . ?
C3 H3 0.9500 . ?
C3 C2 1.372(6) . ?
C21 C20 1.361(6) . ?
N3 C44 1.435(7) . ?
N3 C45 1.453(8) . ?
N3 C43 1.302(6) . ?
C33 C34 1.367(6) . ?
C33 C42 1.426(5) . ?
C20 H20 0.9500 . ?
C20 C19 1.416(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.217(10) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C25 1.510(7) . ?
C13 H13 0.9500 . ?
C13 C14 1.405(7) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C36 H36 0.9500 . ?
C36 C35 1.419(6) . ?
C17 H17 0.9500 . ?
C17 C16 1.399(8) . ?
C17 C18 1.374(7) . ?
C11 H11 0.9500 . ?
C11 C6 1.438(6) . ?
C34 H34 0.9500 . ?
C34 C35 1.407(6) . ?
C40 C35 1.422(6) . ?
C40 C41 1.407(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.419(6) . ?
C26 C25 1.379(7) . ?
C16 H16 0.9500 . ?
C16 C15 1.365(8) . ?
C38 H38 0.9500 . ?
C32 H32 0.9500 . ?
C32 C27 1.436(6) . ?
C15 H15 0.9500 . ?
C15 C14 1.423(7) . ?
C27 C28 1.406(7) . ?
C46 H46 0.9500 . ?
C6 C7 1.400(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.409(8) . ?
C24 C23 1.359(8) . ?
C7 C2 1.403(6) . ?
C7 O2 1.339(4) . ?
C14 C19 1.412(7) . ?
C2 O1 1.378(5) . ?
C19 C18 1.423(7) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C23 C28 1.430(7) . ?
C41 H41 0.9500 . ?
C41 C42 1.360(6) . ?
C49 H49 0.9500 . ?
C43 H43 0.9500 . ?
C18 H18 0.9500 . ?
C10 H10A 0.9500 . ?
C10 H10B 0.9500 . ?
C31 H31A 0.9500 . ?
C31 H31B 0.9500 . ?
Cl1 O13_a 1.570(10) . ?
Cl1 O14 1.344(6) . ?
Cl1 O12 1.380(7) . ?
Cl1 O11_a 1.325(17) . ?
Cl1 O15 1.640(12) . ?
Cl1 O11A_b 1.763(11) . ?
Cl1 O13A_b 1.256(13) . ?
O2 Dy1 2.283(3) 3_676 ?
O1 Dy1 2.548(3) 3_676 ?
O1 C1 1.429(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
O14 O11_a 0.99(3) . ?

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
Ni1 Dy1 Ni1 53.996(14) 3_676 . ?
O5 Dy1 Ni1 117.24(8) . . ?
O5 Dy1 Ni1 171.00(8) . 3_676 ?
O5 Dy1 O3 87.09(11) . . ?
O5 Dy1 O7 80.88(12) . . ?
O5 Dy1 O8 106.54(11) . . ?
O5 Dy1 N2 74.30(11) . . ?
O5 Dy1 O6 138.61(10) . . ?
O5 Dy1 O2 147.74(10) . 3_676 ?
O5 Dy1 O1 84.07(10) . 3_676 ?
O3 Dy1 Ni1 35.11(6) . . ?
O3 Dy1 Ni1 83.96(6) . 3_676 ?
O3 Dy1 O7 144.92(10) . . ?
O3 Dy1 O8 144.62(10) . . ?
O3 Dy1 N2 80.37(10) . . ?
O3 Dy1 O6 71.84(9) . . ?
O3 Dy1 O1 76.79(9) . 3_676 ?
O7 Dy1 Ni1 157.35(9) . . ?
O7 Dy1 Ni1 107.11(9) . 3_676 ?
O7 Dy1 N2 126.60(11) . . ?
O7 Dy1 O6 135.30(11) . . ?
O7 Dy1 O1 69.31(10) . 3_676 ?
O8 Dy1 Ni1 113.31(8) . . ?
O8 Dy1 Ni1 80.49(8) . 3_676 ?
O8 Dy1 O7 70.39(11) . . ?
O8 Dy1 N2 72.62(11) . . ?
O8 Dy1 O6 76.86(9) . . ?
O8 Dy1 O1 135.87(10) . 3_676 ?
N2 Dy1 Ni1 103.15(8) . 3_676 ?
N2 Dy1 Ni1 73.96(8) . . ?
N2 Dy1 O1 149.17(10) . 3_676 ?
O6 Dy1 Ni1 36.41(6) . 3_676 ?
O6 Dy1 Ni1 37.06(6) . . ?
O6 Dy1 N2 67.43(10) . . ?
O6 Dy1 O1 122.87(9) . 3_676 ?
O2 Dy1 Ni1 74.30(7) 3_676 . ?
O2 Dy1 Ni1 33.61(7) 3_676 3_676 ?
O2 Dy1 O3 90.08(9) 3_676 . ?
O2 Dy1 O7 83.22(11) 3_676 . ?
O2 Dy1 O8 94.14(10) 3_676 . ?
O2 Dy1 N2 136.73(11) 3_676 . ?
O2 Dy1 O6 69.48(9) 3_676 . ?
O2 Dy1 O1 64.04(9) 3_676 3_676 ?
O1 Dy1 Ni1 97.75(7) 3_676 . ?
O1 Dy1 Ni1 94.78(7) 3_676 3_676 ?
Dy1 Ni1 Dy1 126.004(14) 3_676 . ?
O3 Ni1 Dy1 150.74(7) . 3_676 ?
O3 Ni1 Dy1 41.23(7) . . ?
O3 Ni1 O9 88.99(12) . . ?
O3 Ni1 O6 83.82(10) . . ?
O3 Ni1 O6 107.75(10) . 3_676 ?
N1 Ni1 Dy1 95.99(10) . . ?
N1 Ni1 Dy1 127.02(10) . 3_676 ?
N1 Ni1 O3 82.01(12) . . ?
N1 Ni1 O9 86.55(12) . . ?
N1 Ni1 O6 100.56(11) . . ?
N1 Ni1 O6 169.92(13) . 3_676 ?
N1 Ni1 O2 89.15(13) . . ?
O9 Ni1 Dy1 89.38(8) . 3_676 ?
O9 Ni1 Dy1 128.49(9) . . ?
O9 Ni1 O6 169.06(11) . . ?
O9 Ni1 O6 91.04(10) . 3_676 ?
O6 Ni1 Dy1 43.02(7) . . ?
O6 Ni1 Dy1 92.85(7) . 3_676 ?
O6 Ni1 Dy1 93.17(7) 3_676 . ?
O6 Ni1 Dy1 43.09(7) 3_676 3_676 ?
O6 Ni1 O6 83.34(10) 3_676 . ?
O2 Ni1 Dy1 134.89(8) . . ?
O2 Ni1 Dy1 38.98(7) . 3_676 ?
O2 Ni1 O3 169.31(10) . . ?
O2 Ni1 O9 96.49(12) . . ?
O2 Ni1 O6 91.95(11) . . ?
O2 Ni1 O6 81.40(10) . 3_676 ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N4 C47 H47A 109.5 . . ?
N4 C47 H47B 109.5 . . ?
N4 C47 H47C 109.5 . . ?
C28 O5 Dy1 140.0(3) . . ?
C23 O4 C22 118.8(5) . . ?
Ni1 O3 Dy1 103.66(11) . . ?
C21 O3 Dy1 125.6(2) . . ?
C21 O3 Ni1 107.2(2) . . ?
C43 O7 Dy1 129.7(3) . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N5 C51 H51A 109.5 . . ?
N5 C51 H51B 109.5 . . ?
N5 C51 H51C 109.5 . . ?
C46 O8 Dy1 142.4(3) . . ?
H8A C8 H8B 108.0 . . ?
C4 C8 H8A 109.3 . . ?
C4 C8 H8B 109.3 . . ?
C9 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
C9 C8 C4 111.6(5) . . ?
C12 N1 Ni1 109.2(2) . . ?
C11 N1 Ni1 127.3(3) . . ?
C11 N1 C12 123.5(3) . . ?
C33 N2 Dy1 111.4(2) . . ?
C32 N2 Dy1 128.3(3) . . ?
C32 N2 C33 120.3(4) . . ?
C48 N4 C47 115.4(5) . . ?
C46 N4 C47 123.3(5) . . ?
C46 N4 C48 121.3(4) . . ?
C29 C30 H30 116.4 . . ?
C31 C30 H30 116.4 . . ?
C31 C30 C29 127.2(7) . . ?
C4 C5 H5 118.8 . . ?
C4 C5 C6 122.4(4) . . ?
C6 C5 H5 118.8 . . ?
C40 C39 H39 118.9 . . ?
C38 C39 H39 118.9 . . ?
C38 C39 C40 122.1(5) . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N5 C50 H50A 109.5 . . ?
N5 C50 H50B 109.5 . . ?
N5 C50 H50C 109.5 . . ?
C49 O9 Ni1 125.7(3) . . ?
C5 C4 C8 122.9(4) . . ?
C5 C4 C3 118.7(4) . . ?
C3 C4 C8 118.4(4) . . ?
Ni1 O6 Dy1 100.51(9) 3_676 . ?
Ni1 O6 Dy1 99.92(10) . . ?
Ni1 O6 Ni1 96.65(10) 3_676 . ?
C42 O6 Dy1 113.4(2) . . ?
C42 O6 Ni1 125.9(2) . 3_676 ?
C42 O6 Ni1 116.2(2) . . ?
C36 C37 H37 119.3 . . ?
C36 C37 C38 121.3(5) . . ?
C38 C37 H37 119.3 . . ?
C51 N5 C50 117.1(6) . . ?
C49 N5 C51 123.4(6) . . ?
C49 N5 C50 119.5(5) . . ?
N1 C12 C21 114.5(3) . . ?
C13 C12 N1 124.9(4) . . ?
C13 C12 C21 120.5(4) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 C4 119.9(4) . . ?
C2 C3 H3 120.0 . . ?
O3 C21 C12 118.3(4) . . ?
O3 C21 C20 122.9(4) . . ?
C20 C21 C12 118.9(4) . . ?
C44 N3 C45 115.4(5) . . ?
C43 N3 C44 122.6(6) . . ?
C43 N3 C45 121.9(5) . . ?
C34 C33 N2 123.9(4) . . ?
C34 C33 C42 119.5(4) . . ?
C42 C33 N2 116.4(3) . . ?
C21 C20 H20 119.2 . . ?
C21 C20 C19 121.6(4) . . ?
C19 C20 H20 119.2 . . ?
C8 C9 H9 115.4 . . ?
C10 C9 C8 129.2(8) . . ?
C10 C9 H9 115.4 . . ?
N4 C48 H48A 109.5 . . ?
N4 C48 H48B 109.5 . . ?
N4 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C30 C29 H29A 108.8 . . ?
C30 C29 H29B 108.8 . . ?
H29A C29 H29B 107.7 . . ?
C25 C29 C30 113.7(6) . . ?
C25 C29 H29A 108.8 . . ?
C25 C29 H29B 108.8 . . ?
C12 C13 H13 119.6 . . ?
C12 C13 C14 120.8(4) . . ?
C14 C13 H13 119.6 . . ?
N3 C44 H44A 109.5 . . ?
N3 C44 H44B 109.5 . . ?
N3 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C37 C36 H36 119.7 . . ?
C37 C36 C35 120.7(5) . . ?
C35 C36 H36 119.7 . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C18 C17 C16 120.2(5) . . ?
N1 C11 H11 117.4 . . ?
N1 C11 C6 125.2(4) . . ?
C6 C11 H11 117.4 . . ?
C33 C34 H34 119.3 . . ?
C33 C34 C35 121.4(4) . . ?
C35 C34 H34 119.3 . . ?
C39 C40 C35 118.3(4) . . ?
C41 C40 C39 122.9(4) . . ?
C41 C40 C35 118.8(4) . . ?
C36 C35 C40 119.0(4) . . ?
C34 C35 C36 122.2(4) . . ?
C34 C35 C40 118.8(4) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C25 C26 C27 121.4(5) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 C17 120.8(5) . . ?
C15 C16 H16 119.6 . . ?
C39 C38 C37 118.5(5) . . ?
C39 C38 H38 120.7 . . ?
C37 C38 H38 120.7 . . ?
N2 C32 H32 116.6 . . ?
N2 C32 C27 126.8(4) . . ?
C27 C32 H32 116.6 . . ?
C16 C15 H15 119.7 . . ?
C16 C15 C14 120.6(6) . . ?
C14 C15 H15 119.7 . . ?
C26 C27 C32 117.4(4) . . ?
C28 C27 C26 119.0(4) . . ?
C28 C27 C32 123.6(4) . . ?
O8 C46 N4 125.2(5) . . ?
O8 C46 H46 117.4 . . ?
N4 C46 H46 117.4 . . ?
C5 C6 C11 117.7(4) . . ?
C7 C6 C5 118.6(4) . . ?
C7 C6 C11 123.7(4) . . ?
C25 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C23 C24 C25 121.8(5) . . ?
C26 C25 C29 121.8(5) . . ?
C26 C25 C24 118.6(5) . . ?
C24 C25 C29 119.6(5) . . ?
C6 C7 C2 118.5(4) . . ?
O2 C7 C6 123.9(4) . . ?
O2 C7 C2 117.6(3) . . ?
C13 C14 C15 122.1(5) . . ?
C13 C14 C19 119.1(4) . . ?
C19 C14 C15 118.8(5) . . ?
C3 C2 C7 121.8(4) . . ?
C3 C2 O1 124.8(4) . . ?
O1 C2 C7 113.4(3) . . ?
C20 C19 C18 121.9(5) . . ?
C14 C19 C20 119.1(4) . . ?
C14 C19 C18 119.1(4) . . ?
N3 C45 H45A 109.5 . . ?
N3 C45 H45B 109.5 . . ?
N3 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O4 C23 C24 125.3(5) . . ?
O4 C23 C28 114.4(5) . . ?
C24 C23 C28 120.2(5) . . ?
C40 C41 H41 119.3 . . ?
C42 C41 C40 121.5(4) . . ?
C42 C41 H41 119.3 . . ?
O9 C49 N5 125.3(5) . . ?
O9 C49 H49 117.3 . . ?
N5 C49 H49 117.3 . . ?
O7 C43 N3 122.0(5) . . ?
O7 C43 H43 119.0 . . ?
N3 C43 H43 119.0 . . ?
O5 C28 C27 123.3(4) . . ?
O5 C28 C23 117.8(4) . . ?
C27 C28 C23 118.9(4) . . ?
O6 C42 C33 118.0(3) . . ?
C41 C42 O6 122.0(3) . . ?
C41 C42 C33 119.9(3) . . ?
C17 C18 C19 120.5(5) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C9 C10 H10A 120.0 . . ?
C9 C10 H10B 120.0 . . ?
H10A C10 H10B 120.0 . . ?
C30 C31 H31A 120.0 . . ?
C30 C31 H31B 120.0 . . ?
H31A C31 H31B 120.0 . . ?
O13_a Cl1 O15 103.8(6) . . ?
O14 Cl1 O13_a 113.8(6) . . ?
O14 Cl1 O12 123.0(6) . . ?
O14 Cl1 O15 84.8(7) . . ?
O14 Cl1 O11A_b 88.1(6) . . ?
O12 Cl1 O13_a 122.4(5) . . ?
O12 Cl1 O15 90.5(6) . . ?
O12 Cl1 O11A_b 88.6(5) . . ?
O11_a Cl1 O13_a 86.1(15) . . ?
O11_a Cl1 O14 43.6(12) . . ?
O11_a Cl1 O12 129.5(15) . . ?
O11_a Cl1 O15 124.8(15) . . ?
O15 Cl1 O11A_b 170.8(7) . . ?
O13A_b Cl1 O14 128.1(7) . . ?
O13A_b Cl1 O12 107.9(7) . . ?
O13A_b Cl1 O15 85.5(8) . . ?
O13A_b Cl1 O11A_b 103.5(7) . . ?
Ni1 O2 Dy1 107.40(11) . 3_676 ?
C7 O2 Dy1 126.2(2) . 3_676 ?
C7 O2 Ni1 124.7(2) . . ?
C2 O1 Dy1 116.9(2) . 3_676 ?
C2 O1 C1 117.6(3) . . ?
C1 O1 Dy1 125.1(2) . 3_676 ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O11_a O14 Cl1 67.2(12) . . ?
O14 O11_a Cl1 69.2(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O5 C28 C27 21.6(7) . . . . ?
Dy1 O5 C28 C23 -157.9(3) . . . . ?
Dy1 O3 C21 C12 -97.7(4) . . . . ?
Dy1 O3 C21 C20 81.2(4) . . . . ?
Dy1 O7 C43 N3 -130.6(4) . . . . ?
Dy1 O8 C46 N4 176.3(4) . . . . ?
Dy1 N2 C33 C34 152.1(3) . . . . ?
Dy1 N2 C33 C42 -22.5(4) . . . . ?
Dy1 N2 C32 C27 -7.2(7) . . . . ?
Dy1 O6 C42 C33 32.3(4) . . . . ?
Dy1 O6 C42 C41 -148.5(3) . . . . ?
Ni1 O3 C21 C12 24.0(4) . . . . ?
Ni1 O3 C21 C20 -157.1(3) . . . . ?
Ni1 N1 C12 C21 -17.6(4) . . . . ?
Ni1 N1 C12 C13 157.6(4) . . . . ?
Ni1 N1 C11 C6 -1.0(6) . . . . ?
Ni1 O9 C49 N5 153.1(5) . . . . ?
Ni1 O6 C42 C33 156.3(3) 3_676 . . . ?
Ni1 O6 C42 C33 -82.6(4) . . . . ?
Ni1 O6 C42 C41 96.6(4) . . . . ?
Ni1 O6 C42 C41 -24.5(5) 3_676 . . . ?
C47 N4 C46 O8 -175.2(7) . . . . ?
O4 C23 C28 O5 2.1(7) . . . . ?
O4 C23 C28 C27 -177.4(4) . . . . ?
O3 C21 C20 C19 -177.6(4) . . . . ?
C22 O4 C23 C24 -1.3(9) . . . . ?
C22 O4 C23 C28 175.9(5) . . . . ?
C51 N5 C49 O9 177.0(8) . . . . ?
C8 C4 C3 C2 178.0(4) . . . . ?
N1 C12 C21 O3 -5.0(5) . . . . ?
N1 C12 C21 C20 176.0(4) . . . . ?
N1 C12 C13 C14 -177.4(4) . . . . ?
N1 C11 C6 C5 169.1(4) . . . . ?
N1 C11 C6 C7 -10.3(7) . . . . ?
N2 C33 C34 C35 -175.7(4) . . . . ?
N2 C33 C42 O6 -5.7(5) . . . . ?
N2 C33 C42 C41 175.1(3) . . . . ?
N2 C32 C27 C26 176.2(5) . . . . ?
N2 C32 C27 C28 -3.7(8) . . . . ?
C30 C29 C25 C26 114.9(7) . . . . ?
C30 C29 C25 C24 -66.8(8) . . . . ?
C5 C4 C3 C2 -1.5(7) . . . . ?
C5 C6 C7 C2 -3.9(6) . . . . ?
C5 C6 C7 O2 177.8(4) . . . . ?
C39 C40 C35 C36 0.7(6) . . . . ?
C39 C40 C35 C34 179.9(4) . . . . ?
C39 C40 C41 C42 179.2(4) . . . . ?
C50 N5 C49 O9 -3.6(10) . . . . ?
C4 C8 C9 C10 127.9(8) . . . . ?
C4 C5 C6 C11 -177.0(4) . . . . ?
C4 C5 C6 C7 2.5(6) . . . . ?
C4 C3 C2 C7 -0.1(6) . . . . ?
C4 C3 C2 O1 178.6(4) . . . . ?
C37 C36 C35 C34 179.4(5) . . . . ?
C37 C36 C35 C40 -1.4(8) . . . . ?
C12 N1 C11 C6 176.4(4) . . . . ?
C12 C21 C20 C19 1.3(6) . . . . ?
C12 C13 C14 C15 -177.2(5) . . . . ?
C12 C13 C14 C19 2.3(7) . . . . ?
C3 C2 O1 Dy1 169.6(3) . . . 3_676 ?
C3 C2 O1 C1 -2.7(6) . . . . ?
C21 C12 C13 C14 -2.4(7) . . . . ?
C21 C20 C19 C14 -1.3(7) . . . . ?
C21 C20 C19 C18 179.2(4) . . . . ?
C33 N2 C32 C27 175.9(4) . . . . ?
C33 C34 C35 C36 -179.7(4) . . . . ?
C33 C34 C35 C40 1.1(6) . . . . ?
C20 C19 C18 C17 -179.3(5) . . . . ?
C9 C8 C4 C5 115.0(6) . . . . ?
C9 C8 C4 C3 -64.5(6) . . . . ?
C48 N4 C46 O8 5.1(10) . . . . ?
C13 C12 C21 O3 179.6(4) . . . . ?
C13 C12 C21 C20 0.6(6) . . . . ?
C13 C14 C19 C20 -0.5(7) . . . . ?
C13 C14 C19 C18 179.0(4) . . . . ?
C44 N3 C43 O7 -178.0(6) . . . . ?
C36 C37 C38 C39 -2.1(9) . . . . ?
C17 C16 C15 C14 0.3(10) . . . . ?
C11 N1 C12 C21 164.6(4) . . . . ?
C11 N1 C12 C13 -20.2(7) . . . . ?
C11 C6 C7 C2 175.5(4) . . . . ?
C11 C6 C7 O2 -2.8(6) . . . . ?
C34 C33 C42 O6 179.4(3) . . . . ?
C34 C33 C42 C41 0.2(6) . . . . ?
C40 C39 C38 C37 1.3(8) . . . . ?
C40 C41 C42 O6 -178.3(3) . . . . ?
C40 C41 C42 C33 0.9(6) . . . . ?
C35 C40 C41 C42 -1.0(6) . . . . ?
C26 C27 C28 O5 179.2(4) . . . . ?
C26 C27 C28 C23 -1.4(7) . . . . ?
C16 C17 C18 C19 -0.2(9) . . . . ?
C16 C15 C14 C13 -179.8(5) . . . . ?
C16 C15 C14 C19 0.6(9) . . . . ?
C38 C39 C40 C35 -0.6(7) . . . . ?
C38 C39 C40 C41 179.2(4) . . . . ?
C38 C37 C36 C35 2.2(9) . . . . ?
C32 N2 C33 C34 -30.6(6) . . . . ?
C32 N2 C33 C42 154.8(4) . . . . ?
C32 C27 C28 O5 -0.9(7) . . . . ?
C32 C27 C28 C23 178.6(4) . . . . ?
C15 C14 C19 C20 179.1(5) . . . . ?
C15 C14 C19 C18 -1.4(7) . . . . ?
C27 C26 C25 C29 178.0(6) . . . . ?
C27 C26 C25 C24 -0.3(9) . . . . ?
C6 C5 C4 C8 -179.2(4) . . . . ?
C6 C5 C4 C3 0.2(7) . . . . ?
C6 C7 C2 C3 2.8(6) . . . . ?
C6 C7 C2 O1 -176.0(3) . . . . ?
C6 C7 O2 Dy1 -171.6(3) . . . 3_676 ?
C6 C7 O2 Ni1 25.1(5) . . . . ?
C24 C23 C28 O5 179.3(5) . . . . ?
C24 C23 C28 C27 -0.1(7) . . . . ?
C25 C26 C27 C32 -178.4(5) . . . . ?
C25 C26 C27 C28 1.6(8) . . . . ?
C25 C24 C23 O4 178.5(6) . . . . ?
C25 C24 C23 C28 1.5(9) . . . . ?
C7 C2 O1 Dy1 -11.6(4) . . . 3_676 ?
C7 C2 O1 C1 176.0(4) . . . . ?
C14 C19 C18 C17 1.2(7) . . . . ?
C2 C7 O2 Dy1 10.0(5) . . . 3_676 ?
C2 C7 O2 Ni1 -153.2(3) . . . . ?
C45 N3 C43 O7 -2.2(8) . . . . ?
C23 C24 C25 C29 -179.6(6) . . . . ?
C23 C24 C25 C26 -1.3(10) . . . . ?
C41 C40 C35 C36 -179.2(4) . . . . ?
C41 C40 C35 C34 0.0(6) . . . . ?
C42 C33 C34 C35 -1.2(6) . . . . ?
C18 C17 C16 C15 -0.6(10) . . . . ?
C31 C30 C29 C25 -11.3(13) . . . . ?
O2 C7 C2 C3 -178.8(4) . . . . ?
O2 C7 C2 O1 2.4(5) . . . . ?
O13_a Cl1 O14 O11_a 55(2) . . . . ?
O13_a Cl1 O11_a O14 -131.0(19) . . . . ?
O12 Cl1 O14 O11_a -115(2) . . . . ?
O12 Cl1 O11_a O14 99(2) . . . . ?
O15 Cl1 O14 O11_a 158(2) . . . . ?
O15 Cl1 O11_a O14 -27(3) . . . . ?
O11A_b Cl1 O14 O11_a -28(2) . . . . ?
O11A_b Cl1 O11_a O14 143(3) . . . . ?
O13A_b Cl1 O14 O11_a 78(2) . . . . ?
O13A_b Cl1 O11_a O14 -125.2(17) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.137 0.142 0.257 173.3 1.0 ?
2 0.137 -0.142 0.743 173.3 2.8 ?
3 0.363 0.358 0.757 173.3 3.4 ?
4 0.637 0.642 0.243 173.3 0.5 ?

_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_11_CCDC_1406227
_database_code_depnum_ccdc_archive 'CCDC 1406227'
_audit_update_record             
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_audit_creation_date             2014-12-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.12.23 svn.r3114 for OlexSys, GUI svn.r4973)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '2(Cl O4), C64 H72 Dy2 N4 Ni2 O18'
_chemical_formula_sum            'C64 H72 Cl2 Dy2 N4 Ni2 O26'
_chemical_formula_weight         1826.57
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.1724(12)
_cell_length_b                   14.1352(15)
_cell_length_c                   19.123(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.425(11)
_cell_angle_gamma                90
_cell_volume                     3245.9(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    173
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.019
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1031
_diffrn_reflns_av_unetI/netI     0.2047
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.831
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12310
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.029
_diffrn_reflns_theta_min         2.592
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.831
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4079
_reflns_number_total             7192
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.348
_refine_diff_density_min         -1.823
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         7192
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1319
_refine_ls_R_factor_gt           0.0650
_refine_ls_restrained_S_all      0.872
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1300
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O7-H7
 0.87 with sigma of 0.01
 O8-H8
 0.87 with sigma of 0.01
 C29-H7
 1.907074 with sigma of 0.02
 Dy1-H7
 2.944961 with sigma of 0.02
 Dy1-H8
 2.916097 with sigma of 0.02
3.a Rotating group:
 O9(H9A,H9B)
3.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C1A(H1AA,H1AB)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11), C12(H12), C25(H25), C17(H17), C24(H24), C8(H8A), C26(H26),
 C22(H22), C5(H5), C19(H19), C10(H10), C18(H18), C13(H13), C27(H27), C4(H4)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O13 O 0.5479(6) 0.2297(7) 0.5829(5) 0.068(3) Uani 1 1 d . . . . .
Dy1 Dy 0.00541(3) 0.29388(3) 0.44163(3) 0.01550(13) Uani 1 1 d D . . . .
Cl1 Cl 0.4349(2) 0.2526(2) 0.56507(17) 0.0345(7) Uani 1 1 d . . . . .
O4 O -0.1811(5) 0.0940(5) 0.2525(4) 0.0257(17) Uani 1 1 d . . . . .
O10 O 0.4203(6) 0.3527(6) 0.5637(5) 0.057(3) Uani 1 1 d . . . . .
O5 O -0.0928(4) 0.1855(4) 0.3781(3) 0.0177(15) Uani 1 1 d . . . . .
O7 O 0.1669(5) 0.1899(5) 0.4290(4) 0.0256(17) Uani 1 1 d D . . . .
H7 H 0.208(5) 0.177(6) 0.4694(9) 0.038 Uiso 1 1 d DR . . . .
O1 O 0.0765(5) 0.3294(5) 0.3289(3) 0.0232(16) Uani 1 1 d . . . . .
O11 O 0.3765(6) 0.2165(7) 0.6178(6) 0.076(4) Uani 1 1 d . . . . .
C3 C 0.2272(7) 0.4003(7) 0.2784(5) 0.021(2) Uani 1 1 d . . . . .
H3 H 0.2051 0.3699 0.2341 0.025 Uiso 1 1 calc R . . . .
C11 C 0.4517(7) 0.6909(7) 0.6656(6) 0.029(3) Uani 1 1 d . . . . .
H11 H 0.5249 0.7159 0.6768 0.034 Uiso 1 1 calc R . . . .
O9 O 0.2184(5) 0.3960(4) 0.6090(4) 0.0232(17) Uani 1 1 d . . . . .
H9A H 0.2892 0.3850 0.6003 0.035 Uiso 1 1 d GR . . . .
H9B H 0.1838 0.3385 0.6073 0.035 Uiso 1 1 d GR . . . .
O3 O 0.1287(5) 0.5943(4) 0.6113(3) 0.0176(15) Uani 1 1 d . . . . .
O8 O 0.1091(5) 0.2360(5) 0.5531(4) 0.0267(17) Uani 1 1 d D . . . .
H8 H 0.120(7) 0.278(2) 0.5870(17) 0.040 Uiso 1 1 d DR . . . .
Ni1 Ni 0.12747(9) 0.49389(9) 0.53390(7) 0.0152(3) Uani 1 1 d . . . . .
O12 O 0.3904(8) 0.2150(9) 0.5002(6) 0.098(4) Uani 1 1 d . . . . .
C14 C 0.2351(7) 0.6237(6) 0.6312(5) 0.012(2) Uani 1 1 d . . . . .
N2 N -0.1390(6) 0.2520(5) 0.5108(4) 0.0172(18) Uani 1 1 d . . . . .
C12 C 0.3767(7) 0.7071(7) 0.7117(6) 0.026(2) Uani 1 1 d . . . . .
H12 H 0.3987 0.7411 0.7545 0.031 Uiso 1 1 calc R . . . .
N1 N 0.2743(5) 0.5517(5) 0.5253(4) 0.0118(16) Uani 1 1 d . . . . .
O6 O -0.0174(4) 0.4127(4) 0.5299(3) 0.0148(14) Uani 1 1 d . . . . .
C25 C -0.1499(7) 0.3046(7) 0.7007(5) 0.023(2) Uani 1 1 d . . . . .
H25 H -0.1831 0.2814 0.7389 0.027 Uiso 1 1 calc R . . . .
C1 C 0.0255(7) 0.2970(7) 0.2590(5) 0.025(2) Uani 1 1 d . . . . .
H1A H 0.0789 0.2583 0.2385 0.038 Uiso 1 1 calc GR . . . .
H1B H 0.0037 0.3517 0.2284 0.038 Uiso 1 1 calc GR . . . .
H1C H -0.0406 0.2590 0.2630 0.038 Uiso 1 1 calc GR . . . .
C17 C -0.3227(7) 0.0312(7) 0.3105(5) 0.022(2) Uani 1 1 d . . . . .
H17 H -0.3477 -0.0047 0.2689 0.026 Uiso 1 1 calc R . . . .
C23 C -0.1261(7) 0.2962(7) 0.5788(5) 0.017(2) Uani 1 1 d . . . . .
C16 C -0.2276(7) 0.0855(7) 0.3143(5) 0.019(2) Uani 1 1 d . . . . .
C24 C -0.1707(7) 0.2611(7) 0.6367(5) 0.020(2) Uani 1 1 d . . . . .
H24 H -0.2162 0.2061 0.6310 0.025 Uiso 1 1 calc R . . . .
C28 C -0.0579(7) 0.3778(6) 0.5879(5) 0.013(2) Uani 1 1 d . . . . .
C8 C 0.3268(7) 0.5455(7) 0.4720(6) 0.023(2) Uani 1 1 d . . . . .
H8A H 0.3946 0.5798 0.4748 0.028 Uiso 1 1 calc R . . . .
O2 O 0.1411(4) 0.4072(4) 0.4512(3) 0.0172(15) Uani 1 1 d . . . . .
C26 C -0.0796(7) 0.3837(7) 0.7104(5) 0.019(2) Uani 1 1 d . . . . .
H26 H -0.0642 0.4136 0.7555 0.023 Uiso 1 1 calc R . . . .
C22 C -0.2248(7) 0.1962(7) 0.4934(5) 0.018(2) Uani 1 1 d . . . . .
H22 H -0.2752 0.1924 0.5263 0.021 Uiso 1 1 calc R . . . .
C5 C 0.3494(8) 0.5067(7) 0.3521(6) 0.026(3) Uani 1 1 d . . . . .
H5 H 0.4118 0.5480 0.3582 0.032 Uiso 1 1 calc R . . . .
C19 C -0.3491(8) 0.0847(7) 0.4236(5) 0.024(2) Uani 1 1 d . . . . .
H19 H -0.3931 0.0868 0.4602 0.029 Uiso 1 1 calc R . . . .
C10 C 0.4232(8) 0.6405(7) 0.6049(6) 0.025(3) Uani 1 1 d . . . . .
H10 H 0.4768 0.6280 0.5751 0.031 Uiso 1 1 calc R . . . .
C18 C -0.3829(7) 0.0283(7) 0.3669(5) 0.023(2) Uani 1 1 d . . . . .
H18 H -0.4457 -0.0120 0.3655 0.028 Uiso 1 1 calc R . . . .
C20 C -0.2515(7) 0.1405(6) 0.4308(5) 0.014(2) Uani 1 1 d . . . . .
C13 C 0.2698(7) 0.6729(7) 0.6942(6) 0.024(2) Uani 1 1 d . . . . .
H13 H 0.2184 0.6831 0.7258 0.029 Uiso 1 1 calc R . . . .
C21 C -0.1872(7) 0.1382(6) 0.3742(5) 0.017(2) Uani 1 1 d . . . . .
C7 C 0.2013(7) 0.4288(6) 0.3999(5) 0.014(2) Uani 1 1 d . . . . .
C27 C -0.0323(7) 0.4184(6) 0.6540(5) 0.015(2) Uani 1 1 d . . . . .
H27 H 0.0179 0.4703 0.6611 0.018 Uiso 1 1 calc R . . . .
C2 C 0.1716(7) 0.3842(7) 0.3346(5) 0.020(2) Uani 1 1 d . . . . .
C9 C 0.3145(7) 0.6072(6) 0.5866(5) 0.015(2) Uani 1 1 d . . . . .
C29 C 0.2129(9) 0.1450(8) 0.3730(6) 0.036(3) Uani 1 1 d D . . . .
H29A H 0.2721 0.1855 0.3592 0.043 Uiso 1 1 calc R . . . .
H29B H 0.1540 0.1372 0.3311 0.043 Uiso 1 1 calc R . . . .
C4 C 0.3183(8) 0.4638(8) 0.2892(6) 0.031(3) Uani 1 1 d . . . . .
H4 H 0.3581 0.4764 0.2514 0.037 Uiso 1 1 calc R . . . .
C6 C 0.2917(7) 0.4916(7) 0.4093(5) 0.016(2) Uani 1 1 d . . . . .
C15 C -0.0767(7) 0.0463(8) 0.2561(6) 0.035(3) Uani 1 1 d . . . . .
H15A H -0.0453 0.0597 0.2132 0.052 Uiso 1 1 calc GR . . . .
H15B H -0.0881 -0.0220 0.2600 0.052 Uiso 1 1 calc GR . . . .
H15C H -0.0253 0.0685 0.2977 0.052 Uiso 1 1 calc GR . . . .
C1A C 0.1163(11) 0.1494(10) 0.5899(8) 0.068(5) Uani 1 1 d . . . . .
H1AA H 0.1938 0.1264 0.5934 0.081 Uiso 1 1 calc R . . . .
H1AB H 0.1039 0.1628 0.6388 0.081 Uiso 1 1 calc R . . . .
C1B C 0.0493(12) 0.0786(11) 0.5652(10) 0.098(6) Uani 1 1 d . . . . .
H1BA H 0.0379 0.0790 0.5133 0.147 Uiso 1 1 calc GR . . . .
H1BB H -0.0225 0.0862 0.5814 0.147 Uiso 1 1 calc GR . . . .
H1BC H 0.0831 0.0184 0.5828 0.147 Uiso 1 1 calc GR . . . .
C1C C 0.2616(9) 0.0480(8) 0.3968(7) 0.054(4) Uani 1 1 d . . . . .
H1CA H 0.3028 0.0229 0.3610 0.081 Uiso 1 1 calc GR . . . .
H1CB H 0.2010 0.0045 0.4026 0.081 Uiso 1 1 calc GR . . . .
H1CC H 0.3120 0.0546 0.4421 0.081 Uiso 1 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
O13 Cl1 1.401(7) . ?
Dy1 O5 2.185(6) . ?
Dy1 O7 2.498(6) . ?
Dy1 O1 2.501(6) . ?
Dy1 O3 2.375(6) 3_566 ?
Dy1 O8 2.434(7) . ?
Dy1 Ni1 3.4760(13) 3_566 ?
Dy1 N2 2.440(7) . ?
Dy1 O6 2.429(6) . ?
Dy1 O2 2.287(6) . ?
Cl1 O10 1.426(8) . ?
Cl1 O11 1.420(8) . ?
Cl1 O12 1.377(10) . ?
O4 C16 1.397(10) . ?
O4 C15 1.430(10) . ?
O5 C21 1.321(9) . ?
O7 H7 0.868(9) . ?
O7 C29 1.434(10) . ?
O1 C1 1.452(11) . ?
O1 C2 1.383(10) . ?
C3 H3 0.9500 . ?
C3 C2 1.379(11) . ?
C3 C4 1.415(13) . ?
C11 H11 0.9500 . ?
C11 C12 1.388(13) . ?
C11 C10 1.358(13) . ?
O9 H9A 0.9164 . ?
O9 H9B 0.9135 . ?
O9 Ni1 2.164(6) . ?
O3 Dy1 2.375(6) 3_566 ?
O3 Ni1 2.049(6) . ?
O3 C14 1.354(10) . ?
O8 H8 0.869(10) . ?
O8 C1A 1.409(13) . ?
Ni1 Dy1 3.4760(13) 3_566 ?
Ni1 N1 1.996(7) . ?
Ni1 O6 2.095(6) . ?
Ni1 O6 2.119(6) 3_566 ?
Ni1 O2 2.028(6) . ?
C14 C13 1.396(13) . ?
C14 C9 1.408(11) . ?
N2 C23 1.429(11) . ?
N2 C22 1.308(11) . ?
C12 H12 0.9500 . ?
C12 C13 1.376(12) . ?
N1 C8 1.292(11) . ?
N1 C9 1.430(11) . ?
O6 Ni1 2.119(6) 3_566 ?
O6 C28 1.377(10) . ?
C25 H25 0.9500 . ?
C25 C24 1.356(13) . ?
C25 C26 1.403(12) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C17 H17 0.9500 . ?
C17 C16 1.381(12) . ?
C17 C18 1.401(12) . ?
C23 C24 1.401(12) . ?
C23 C28 1.415(12) . ?
C16 C21 1.388(13) . ?
C24 H24 0.9500 . ?
C28 C27 1.376(12) . ?
C8 H8A 0.9500 . ?
C8 C6 1.426(13) . ?
O2 C7 1.351(9) . ?
C26 H26 0.9500 . ?
C26 C27 1.393(11) . ?
C22 H22 0.9500 . ?
C22 C20 1.425(12) . ?
C5 H5 0.9500 . ?
C5 C4 1.346(14) . ?
C5 C6 1.409(12) . ?
C19 H19 0.9500 . ?
C19 C18 1.353(13) . ?
C19 C20 1.414(12) . ?
C10 H10 0.9500 . ?
C10 C9 1.393(12) . ?
C18 H18 0.9500 . ?
C20 C21 1.437(12) . ?
C13 H13 0.9500 . ?
C7 C2 1.393(13) . ?
C7 C6 1.403(12) . ?
C27 H27 0.9500 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C1C 1.533(14) . ?
C4 H4 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C1A C1B 1.327(17) . ?
C1B H1BA 0.9800 . ?
C1B H1BB 0.9800 . ?
C1B H1BC 0.9800 . ?
C1C H1CA 0.9800 . ?
C1C H1CB 0.9800 . ?
C1C H1CC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Dy1 O7 84.3(2) . . ?
O5 Dy1 O1 84.1(2) . . ?
O5 Dy1 O3 87.4(2) . 3_566 ?
O5 Dy1 O8 114.2(2) . . ?
O5 Dy1 Ni1 117.10(15) . 3_566 ?
O5 Dy1 N2 75.8(2) . . ?
O5 Dy1 O6 139.16(19) . . ?
O5 Dy1 O2 149.1(2) . . ?
O7 Dy1 O1 69.3(2) . . ?
O7 Dy1 Ni1 155.78(16) . 3_566 ?
O1 Dy1 Ni1 100.19(16) . 3_566 ?
O3 Dy1 O7 147.9(2) 3_566 . ?
O3 Dy1 O1 79.0(2) 3_566 . ?
O3 Dy1 O8 144.9(2) 3_566 . ?
O3 Dy1 Ni1 35.00(15) 3_566 3_566 ?
O3 Dy1 N2 83.5(2) 3_566 . ?
O3 Dy1 O6 71.8(2) 3_566 . ?
O8 Dy1 O7 65.4(2) . . ?
O8 Dy1 O1 128.3(2) . . ?
O8 Dy1 Ni1 110.98(15) . 3_566 ?
O8 Dy1 N2 76.1(2) . . ?
N2 Dy1 O7 123.9(2) . . ?
N2 Dy1 O1 153.8(2) . . ?
N2 Dy1 Ni1 75.17(18) . 3_566 ?
O6 Dy1 O7 131.0(2) . . ?
O6 Dy1 O1 123.7(2) . . ?
O6 Dy1 O8 74.1(2) . . ?
O6 Dy1 Ni1 36.95(15) . 3_566 ?
O6 Dy1 N2 67.5(2) . . ?
O2 Dy1 O7 81.4(2) . . ?
O2 Dy1 O1 65.3(2) . . ?
O2 Dy1 O3 90.3(2) . 3_566 ?
O2 Dy1 O8 84.3(2) . . ?
O2 Dy1 Ni1 74.38(15) . 3_566 ?
O2 Dy1 N2 134.6(2) . . ?
O2 Dy1 O6 67.86(19) . . ?
O13 Cl1 O10 110.4(5) . . ?
O13 Cl1 O11 109.3(6) . . ?
O11 Cl1 O10 107.1(5) . . ?
O12 Cl1 O13 110.8(6) . . ?
O12 Cl1 O10 109.7(7) . . ?
O12 Cl1 O11 109.5(7) . . ?
C16 O4 C15 113.4(8) . . ?
C21 O5 Dy1 141.0(6) . . ?
Dy1 O7 H7 112.5(14) . . ?
C29 O7 Dy1 137.9(6) . . ?
C29 O7 H7 109.6(14) . . ?
C1 O1 Dy1 125.0(5) . . ?
C2 O1 Dy1 116.6(5) . . ?
C2 O1 C1 118.4(7) . . ?
C2 C3 H3 121.1 . . ?
C2 C3 C4 117.7(10) . . ?
C4 C3 H3 121.1 . . ?
C12 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C10 C11 C12 121.8(9) . . ?
H9A O9 H9B 106.6 . . ?
Ni1 O9 H9A 112.4 . . ?
Ni1 O9 H9B 111.2 . . ?
Ni1 O3 Dy1 103.3(3) . 3_566 ?
C14 O3 Dy1 118.4(5) . 3_566 ?
C14 O3 Ni1 108.0(5) . . ?
Dy1 O8 H8 115(2) . . ?
C1A O8 Dy1 135.3(7) . . ?
C1A O8 H8 103(3) . . ?
O9 Ni1 Dy1 131.42(18) . 3_566 ?
O3 Ni1 Dy1 41.68(18) . 3_566 ?
O3 Ni1 O9 91.2(3) . . ?
O3 Ni1 O6 85.0(2) . 3_566 ?
O3 Ni1 O6 108.2(2) . . ?
N1 Ni1 Dy1 95.8(2) . 3_566 ?
N1 Ni1 O9 87.1(3) . . ?
N1 Ni1 O3 82.8(3) . . ?
N1 Ni1 O6 168.8(3) . . ?
N1 Ni1 O6 100.8(3) . 3_566 ?
N1 Ni1 O2 89.7(3) . . ?
O6 Ni1 Dy1 94.02(16) . 3_566 ?
O6 Ni1 Dy1 43.57(16) 3_566 3_566 ?
O6 Ni1 O9 170.7(2) 3_566 . ?
O6 Ni1 O9 90.6(2) . . ?
O6 Ni1 O6 82.6(2) . 3_566 ?
O2 Ni1 Dy1 136.52(19) . 3_566 ?
O2 Ni1 O9 91.9(3) . . ?
O2 Ni1 O3 171.7(2) . . ?
O2 Ni1 O6 79.4(2) . . ?
O2 Ni1 O6 93.0(2) . 3_566 ?
O3 C14 C13 122.4(7) . . ?
O3 C14 C9 120.0(8) . . ?
C13 C14 C9 117.6(8) . . ?
C23 N2 Dy1 114.0(5) . . ?
C22 N2 Dy1 128.6(6) . . ?
C22 N2 C23 117.4(7) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 C11 118.8(10) . . ?
C13 C12 H12 120.6 . . ?
C8 N1 Ni1 127.1(7) . . ?
C8 N1 C9 122.4(8) . . ?
C9 N1 Ni1 110.4(5) . . ?
Ni1 O6 Dy1 102.3(2) . . ?
Ni1 O6 Dy1 99.5(2) 3_566 . ?
Ni1 O6 Ni1 97.4(2) . 3_566 ?
C28 O6 Dy1 114.1(5) . . ?
C28 O6 Ni1 125.2(6) . . ?
C28 O6 Ni1 114.3(5) . 3_566 ?
C24 C25 H25 119.9 . . ?
C24 C25 C26 120.1(9) . . ?
C26 C25 H25 119.9 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C16 C17 H17 119.5 . . ?
C16 C17 C18 121.0(9) . . ?
C18 C17 H17 119.5 . . ?
C24 C23 N2 124.4(8) . . ?
C24 C23 C28 119.2(9) . . ?
C28 C23 N2 116.3(8) . . ?
C17 C16 O4 117.1(9) . . ?
C17 C16 C21 121.5(8) . . ?
C21 C16 O4 121.0(8) . . ?
C25 C24 C23 120.9(9) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
O6 C28 C23 118.2(8) . . ?
C27 C28 O6 122.2(8) . . ?
C27 C28 C23 119.5(8) . . ?
N1 C8 H8A 117.3 . . ?
N1 C8 C6 125.5(9) . . ?
C6 C8 H8A 117.3 . . ?
Ni1 O2 Dy1 109.6(2) . . ?
C7 O2 Dy1 124.7(6) . . ?
C7 O2 Ni1 123.5(5) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 C25 119.9(9) . . ?
C27 C26 H26 120.1 . . ?
N2 C22 H22 116.2 . . ?
N2 C22 C20 127.6(8) . . ?
C20 C22 H22 116.2 . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.6(9) . . ?
C6 C5 H5 119.2 . . ?
C18 C19 H19 118.4 . . ?
C18 C19 C20 123.2(9) . . ?
C20 C19 H19 118.4 . . ?
C11 C10 H10 120.3 . . ?
C11 C10 C9 119.3(9) . . ?
C9 C10 H10 120.3 . . ?
C17 C18 H18 120.9 . . ?
C19 C18 C17 118.1(9) . . ?
C19 C18 H18 120.9 . . ?
C22 C20 C21 124.6(8) . . ?
C19 C20 C22 117.6(8) . . ?
C19 C20 C21 117.8(9) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 C14 121.7(9) . . ?
C12 C13 H13 119.2 . . ?
O5 C21 C16 120.4(8) . . ?
O5 C21 C20 121.5(8) . . ?
C16 C21 C20 118.1(8) . . ?
O2 C7 C2 117.2(8) . . ?
O2 C7 C6 123.8(9) . . ?
C2 C7 C6 119.0(8) . . ?
C28 C27 C26 120.3(9) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
O1 C2 C7 114.5(7) . . ?
C3 C2 O1 122.9(9) . . ?
C3 C2 C7 122.4(9) . . ?
C14 C9 N1 114.2(7) . . ?
C10 C9 C14 120.7(9) . . ?
C10 C9 N1 125.1(8) . . ?
O7 C29 H29A 109.5 . . ?
O7 C29 H29B 109.5 . . ?
O7 C29 C1C 110.7(9) . . ?
H29A C29 H29B 108.1 . . ?
C1C C29 H29A 109.5 . . ?
C1C C29 H29B 109.5 . . ?
C3 C4 H4 119.5 . . ?
C5 C4 C3 120.9(9) . . ?
C5 C4 H4 119.5 . . ?
C5 C6 C8 116.9(9) . . ?
C7 C6 C8 124.5(8) . . ?
C7 C6 C5 118.4(9) . . ?
O4 C15 H15A 109.5 . . ?
O4 C15 H15B 109.5 . . ?
O4 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O8 C1A H1AA 107.4 . . ?
O8 C1A H1AB 107.4 . . ?
H1AA C1A H1AB 107.0 . . ?
C1B C1A O8 119.5(13) . . ?
C1B C1A H1AA 107.4 . . ?
C1B C1A H1AB 107.4 . . ?
C1A C1B H1BA 109.5 . . ?
C1A C1B H1BB 109.5 . . ?
C1A C1B H1BC 109.5 . . ?
H1BA C1B H1BB 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
C29 C1C H1CA 109.5 . . ?
C29 C1C H1CB 109.5 . . ?
C29 C1C H1CC 109.5 . . ?
H1CA C1C H1CB 109.5 . . ?
H1CA C1C H1CC 109.5 . . ?
H1CB C1C H1CC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O5 C21 C16 167.7(7) . . . . ?
Dy1 O5 C21 C20 -11.6(14) . . . . ?
Dy1 O7 C29 C1C -144.1(8) . . . . ?
Dy1 O1 C2 C3 172.4(7) . . . . ?
Dy1 O1 C2 C7 -13.1(10) . . . . ?
Dy1 O3 C14 C13 80.0(10) 3_566 . . . ?
Dy1 O3 C14 C9 -98.1(8) 3_566 . . . ?
Dy1 O8 C1A C1B -5(2) . . . . ?
Dy1 N2 C23 C24 -156.6(7) . . . . ?
Dy1 N2 C23 C28 19.7(10) . . . . ?
Dy1 N2 C22 C20 4.6(14) . . . . ?
Dy1 O6 C28 C23 -27.8(9) . . . . ?
Dy1 O6 C28 C27 150.7(7) . . . . ?
Dy1 O2 C7 C2 5.6(11) . . . . ?
Dy1 O2 C7 C6 -173.2(6) . . . . ?
O4 C16 C21 O5 -11.3(14) . . . . ?
O4 C16 C21 C20 168.0(8) . . . . ?
C11 C12 C13 C14 -0.7(15) . . . . ?
C11 C10 C9 C14 -1.4(15) . . . . ?
C11 C10 C9 N1 -178.5(9) . . . . ?
O3 C14 C13 C12 -176.1(9) . . . . ?
O3 C14 C9 N1 -5.3(12) . . . . ?
O3 C14 C9 C10 177.2(8) . . . . ?
Ni1 O3 C14 C13 -163.2(8) . . . . ?
Ni1 O3 C14 C9 18.7(9) . . . . ?
Ni1 N1 C8 C6 -3.2(14) . . . . ?
Ni1 N1 C9 C14 -11.6(9) . . . . ?
Ni1 N1 C9 C10 165.7(8) . . . . ?
Ni1 O6 C28 C23 -154.8(6) . . . . ?
Ni1 O6 C28 C23 85.7(8) 3_566 . . . ?
Ni1 O6 C28 C27 -95.7(9) 3_566 . . . ?
Ni1 O6 C28 C27 23.7(11) . . . . ?
Ni1 O2 C7 C2 -156.1(7) . . . . ?
Ni1 O2 C7 C6 25.1(11) . . . . ?
N2 C23 C24 C25 176.5(9) . . . . ?
N2 C23 C28 O6 5.3(12) . . . . ?
N2 C23 C28 C27 -173.3(8) . . . . ?
N2 C22 C20 C19 179.6(9) . . . . ?
N2 C22 C20 C21 -1.4(15) . . . . ?
C12 C11 C10 C9 2.8(16) . . . . ?
N1 C8 C6 C5 169.2(9) . . . . ?
N1 C8 C6 C7 -7.6(16) . . . . ?
O6 C28 C27 C26 176.7(7) . . . . ?
C25 C26 C27 C28 2.7(13) . . . . ?
C1 O1 C2 C3 -7.6(13) . . . . ?
C1 O1 C2 C7 166.9(8) . . . . ?
C17 C16 C21 O5 176.3(8) . . . . ?
C17 C16 C21 C20 -4.4(14) . . . . ?
C23 N2 C22 C20 -176.1(9) . . . . ?
C23 C28 C27 C26 -4.7(13) . . . . ?
C16 C17 C18 C19 3.9(15) . . . . ?
C24 C25 C26 C27 0.9(14) . . . . ?
C24 C23 C28 O6 -178.2(8) . . . . ?
C24 C23 C28 C27 3.2(13) . . . . ?
C28 C23 C24 C25 0.4(14) . . . . ?
C8 N1 C9 C14 165.7(8) . . . . ?
C8 N1 C9 C10 -17.0(14) . . . . ?
O2 C7 C2 O1 5.8(12) . . . . ?
O2 C7 C2 C3 -179.7(8) . . . . ?
O2 C7 C6 C8 -4.7(14) . . . . ?
O2 C7 C6 C5 178.6(8) . . . . ?
C26 C25 C24 C23 -2.4(14) . . . . ?
C22 N2 C23 C24 24.0(13) . . . . ?
C22 N2 C23 C28 -159.8(8) . . . . ?
C22 C20 C21 O5 3.6(14) . . . . ?
C22 C20 C21 C16 -175.7(9) . . . . ?
C19 C20 C21 O5 -177.4(8) . . . . ?
C19 C20 C21 C16 3.3(13) . . . . ?
C10 C11 C12 C13 -1.7(16) . . . . ?
C18 C17 C16 O4 -171.8(8) . . . . ?
C18 C17 C16 C21 0.8(15) . . . . ?
C18 C19 C20 C22 -179.5(10) . . . . ?
C18 C19 C20 C21 1.4(15) . . . . ?
C20 C19 C18 C17 -5.0(16) . . . . ?
C13 C14 C9 N1 176.5(8) . . . . ?
C13 C14 C9 C10 -0.9(14) . . . . ?
C2 C3 C4 C5 0.1(16) . . . . ?
C2 C7 C6 C8 176.5(9) . . . . ?
C2 C7 C6 C5 -0.3(13) . . . . ?
C9 C14 C13 C12 2.0(14) . . . . ?
C9 N1 C8 C6 180.0(9) . . . . ?
C4 C3 C2 O1 174.9(9) . . . . ?
C4 C3 C2 C7 0.9(15) . . . . ?
C4 C5 C6 C8 -175.7(10) . . . . ?
C4 C5 C6 C7 1.3(15) . . . . ?
C6 C5 C4 C3 -1.2(16) . . . . ?
C6 C7 C2 O1 -175.3(8) . . . . ?
C6 C7 C2 C3 -0.8(14) . . . . ?
C15 O4 C16 C17 -110.8(10) . . . . ?
C15 O4 C16 C21 76.5(11) . . . . ?

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

data_12_CCDC_1406228
_database_code_depnum_ccdc_archive 'CCDC 1406228'
_audit_update_record             
;
2015-11-15 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_audit_creation_date             2015-11-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'C74 H86 Dy2 N10 Ni2 O18, 2(C F3 O3 S), 2(C3 H7 N O)'
_chemical_formula_sum            'C82 H100 Dy2 F6 N12 Ni2 O26 S2'
_chemical_formula_weight         2290.27
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C80 H60 N12 O16 Ni2 Dy2'
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'
F F 0.0171 0.0103 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.6632(4)
_cell_length_b                   18.8674(3)
_cell_length_c                   15.7017(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.993(3)
_cell_angle_gamma                90
_cell_volume                     4638.96(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6213
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.9660
_cell_measurement_theta_min      3.7630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.130
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17646
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.381
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -42.00   24.00   1.0000    7.7450
omega____ theta____ kappa____ phi______ frames
    -      -16.1295   77.0000   60.0000 66

#__ type_ start__ end____ width___ exp.time_
  2 omega  -37.00   44.00   1.0000    7.7450
omega____ theta____ kappa____ phi______ frames
    -      -16.1295   77.0000 -180.0000 81

#__ type_ start__ end____ width___ exp.time_
  3 omega  -20.00   26.00   1.0000    7.7450
omega____ theta____ kappa____ phi______ frames
    -      -16.1295   77.0000  -30.0000 46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0247390000
_diffrn_orient_matrix_UB_12      -0.0185588000
_diffrn_orient_matrix_UB_13      0.0215678000
_diffrn_orient_matrix_UB_21      0.0293711000
_diffrn_orient_matrix_UB_22      -0.0286367000
_diffrn_orient_matrix_UB_23      0.0091623000
_diffrn_orient_matrix_UB_31      0.0240724000
_diffrn_orient_matrix_UB_32      0.0157714000
_diffrn_orient_matrix_UB_33      0.0419494000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7897
_reflns_number_total             9384
_reflns_odcompleteness_completeness 98.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.026
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.104
_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     599
_refine_ls_number_reflns         9384
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0382
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0367P)²+10.1517P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0976
_refine_special_details          
;
 ?
;
_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. Uiso/Uaniso restraints and constraints
Uanis(C37) = Uanis(C36)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18), C19(H19), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C32(H32), C35(H35), C38(H38)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.67939(2) 0.51451(2) 0.64866(2) 0.02314(7) Uani 1 1 d . . . . .
Ni1 Ni 0.54067(3) 0.52207(2) 0.42614(3) 0.02074(12) Uani 1 1 d . . . . .
O1 O 0.8143(3) 0.5645(2) 0.9533(2) 0.0572(11) Uani 1 1 d . . . . .
O2 O 0.7445(2) 0.50744(16) 0.7942(2) 0.0335(7) Uani 1 1 d . . . . .
O3 O 0.56571(17) 0.45188(14) 0.53395(17) 0.0219(6) Uani 1 1 d . . . . .
O4 O 0.67434(19) 0.64707(15) 0.67785(19) 0.0303(7) Uani 1 1 d . . . . .
O5 O 0.62050(17) 0.58397(14) 0.52353(18) 0.0248(6) Uani 1 1 d . . . . .
O6 O 0.44702(18) 0.47749(14) 0.31618(18) 0.0237(6) Uani 1 1 d . . . . .
O7 O 0.63153(18) 0.47052(15) 0.38589(19) 0.0288(6) Uani 1 1 d . . . . .
O8 O 0.75641(18) 0.44514(16) 0.57891(19) 0.0316(7) Uani 1 1 d . . . . .
O9 O 0.81395(19) 0.57108(18) 0.6682(2) 0.0384(8) Uani 1 1 d . . . . .
N1 N 0.6659(2) 0.38939(17) 0.6896(2) 0.0235(7) Uani 1 1 d . . . . .
N2 N 0.5337(2) 0.59879(18) 0.3350(2) 0.0246(7) Uani 1 1 d . . . . .
N3 N 0.6774(3) 0.4501(3) 0.2694(3) 0.0491(11) Uani 1 1 d . . . . .
N4 N 0.8319(2) 0.4099(2) 0.4921(3) 0.0354(9) Uani 1 1 d . . . . .
N5 N 0.9335(3) 0.6315(3) 0.7445(4) 0.0681(16) Uani 1 1 d . . . . .
C1 C 0.8392(4) 0.6003(4) 1.0368(4) 0.0676(18) Uani 1 1 d . . . . .
H1A H 0.8388 0.6515 1.0263 0.101 Uiso 1 1 calc GR . . . .
H1B H 0.8968 0.5853 1.0740 0.101 Uiso 1 1 calc GR . . . .
H1C H 0.7992 0.5890 1.0684 0.101 Uiso 1 1 calc GR . . . .
C2 C 0.7937(3) 0.4942(3) 0.9522(3) 0.0385(11) Uani 1 1 d . . . . .
C3 C 0.8064(3) 0.4526(3) 1.0277(3) 0.0442(12) Uani 1 1 d . . . . .
H3 H 0.8342 0.4718 1.0863 0.053 Uiso 1 1 calc R . . . .
C4 C 0.7787(3) 0.3820(3) 1.0187(3) 0.0405(11) Uani 1 1 d . . . . .
H4 H 0.7871 0.3536 1.0710 0.049 Uiso 1 1 calc R . . . .
C5 C 0.7394(3) 0.3544(3) 0.9342(3) 0.0348(10) Uani 1 1 d . . . . .
H5 H 0.7203 0.3066 0.9285 0.042 Uiso 1 1 calc R . . . .
C6 C 0.7265(3) 0.3951(2) 0.8552(3) 0.0272(9) Uani 1 1 d . . . . .
C7 C 0.7547(3) 0.4657(2) 0.8636(3) 0.0299(9) Uani 1 1 d . . . . .
C8 C 0.6841(3) 0.3616(2) 0.7692(3) 0.0273(9) Uani 1 1 d . . . . .
H8 H 0.6678 0.3136 0.7711 0.033 Uiso 1 1 calc R . . . .
C9 C 0.6297(3) 0.3463(2) 0.6116(3) 0.0238(8) Uani 1 1 d . . . . .
C10 C 0.6441(3) 0.2735(2) 0.6095(3) 0.0288(9) Uani 1 1 d . . . . .
H10 H 0.6771 0.2497 0.6633 0.035 Uiso 1 1 calc R . . . .
C11 C 0.6106(3) 0.2360(2) 0.5298(3) 0.0321(10) Uani 1 1 d . . . . .
H11 H 0.6198 0.1864 0.5293 0.038 Uiso 1 1 calc R . . . .
C12 C 0.5634(3) 0.2703(2) 0.4503(3) 0.0308(9) Uani 1 1 d . . . . .
H12 H 0.5408 0.2443 0.3955 0.037 Uiso 1 1 calc R . . . .
C13 C 0.5493(3) 0.3427(2) 0.4512(3) 0.0265(9) Uani 1 1 d . . . . .
H13 H 0.5174 0.3663 0.3966 0.032 Uiso 1 1 calc R . . . .
C14 C 0.5813(3) 0.3810(2) 0.5310(3) 0.0235(8) Uani 1 1 d . . . . .
C15 C 0.7094(4) 0.6794(3) 0.7656(3) 0.0534(15) Uani 1 1 d . . . . .
H15A H 0.7235 0.6426 0.8125 0.080 Uiso 1 1 calc GR . . . .
H15B H 0.6674 0.7121 0.7749 0.080 Uiso 1 1 calc GR . . . .
H15C H 0.7613 0.7057 0.7694 0.080 Uiso 1 1 calc GR . . . .
C16 C 0.6564(3) 0.6909(2) 0.6035(3) 0.0271(9) Uani 1 1 d . . . . .
C17 C 0.6650(3) 0.7636(2) 0.6080(3) 0.0334(10) Uani 1 1 d . . . . .
H17 H 0.6882 0.7869 0.6648 0.040 Uiso 1 1 calc R . . . .
C18 C 0.6390(3) 0.8023(2) 0.5272(3) 0.0387(11) Uani 1 1 d . . . . .
H18 H 0.6449 0.8524 0.5291 0.046 Uiso 1 1 calc R . . . .
C19 C 0.6050(3) 0.7688(2) 0.4452(3) 0.0344(10) Uani 1 1 d . . . . .
H19 H 0.5870 0.7962 0.3912 0.041 Uiso 1 1 calc R . . . .
C20 C 0.5962(3) 0.6943(2) 0.4394(3) 0.0288(9) Uani 1 1 d . . . . .
C21 C 0.6240(3) 0.6544(2) 0.5202(3) 0.0257(9) Uani 1 1 d . . . . .
C22 C 0.5575(3) 0.6638(2) 0.3510(3) 0.0278(9) Uani 1 1 d . . . . .
H22 H 0.5488 0.6940 0.3002 0.033 Uiso 1 1 calc R . . . .
C23 C 0.5000(3) 0.5698(2) 0.2466(3) 0.0251(9) Uani 1 1 d . . . . .
C24 C 0.5123(3) 0.5987(2) 0.1701(3) 0.0311(10) Uani 1 1 d . . . . .
H24 H 0.5437 0.6414 0.1749 0.037 Uiso 1 1 calc R . . . .
C25 C 0.4789(3) 0.5651(3) 0.0875(3) 0.0347(10) Uani 1 1 d . . . . .
H25 H 0.4866 0.5850 0.0353 0.042 Uiso 1 1 calc R . . . .
C26 C 0.4342(3) 0.5022(2) 0.0808(3) 0.0341(10) Uani 1 1 d . . . . .
H26 H 0.4098 0.4798 0.0235 0.041 Uiso 1 1 calc R . . . .
C27 C 0.4248(3) 0.4718(2) 0.1571(3) 0.0305(9) Uani 1 1 d . . . . .
H27 H 0.3962 0.4276 0.1521 0.037 Uiso 1 1 calc R . . . .
C28 C 0.4566(3) 0.5050(2) 0.2414(3) 0.0265(9) Uani 1 1 d . . . . .
C29 C 0.6653(3) 0.4906(3) 0.3317(3) 0.0327(10) Uani 1 1 d . . . . .
H29 H 0.6838 0.5385 0.3352 0.039 Uiso 1 1 calc R . . . .
C30 C 0.6457(5) 0.3784(4) 0.2568(5) 0.081(2) Uani 1 1 d . . . . .
H30A H 0.6936 0.3455 0.2681 0.121 Uiso 1 1 calc GR . . . .
H30B H 0.6063 0.3725 0.1945 0.121 Uiso 1 1 calc GR . . . .
H30C H 0.6155 0.3686 0.2992 0.121 Uiso 1 1 calc GR . . . .
C31 C 0.7168(5) 0.4770(5) 0.2067(4) 0.088(3) Uani 1 1 d . . . . .
H31A H 0.7322 0.5269 0.2204 0.132 Uiso 1 1 calc GR . . . .
H31B H 0.6765 0.4729 0.1445 0.132 Uiso 1 1 calc GR . . . .
H31C H 0.7683 0.4495 0.2127 0.132 Uiso 1 1 calc GR . . . .
C32 C 0.8035(3) 0.4583(3) 0.5346(3) 0.0322(10) Uani 1 1 d . . . . .
H32 H 0.8199 0.5062 0.5312 0.039 Uiso 1 1 calc R . . . .
C33 C 0.8059(4) 0.3365(3) 0.4914(4) 0.0572(16) Uani 1 1 d . . . . .
H33A H 0.8486 0.3107 0.5404 0.086 Uiso 1 1 calc GR . . . .
H33B H 0.8009 0.3149 0.4331 0.086 Uiso 1 1 calc GR . . . .
H33C H 0.7505 0.3343 0.5003 0.086 Uiso 1 1 calc GR . . . .
C34 C 0.8911(3) 0.4272(3) 0.4439(4) 0.0480(13) Uani 1 1 d . . . . .
H34A H 0.8974 0.4788 0.4420 0.072 Uiso 1 1 calc GR . . . .
H34B H 0.8685 0.4087 0.3819 0.072 Uiso 1 1 calc GR . . . .
H34C H 0.9469 0.4058 0.4756 0.072 Uiso 1 1 calc GR . . . .
C35 C 0.8691(3) 0.5921(3) 0.7385(4) 0.0506(13) Uani 1 1 d . . . . .
H35 H 0.8630 0.5777 0.7940 0.061 Uiso 1 1 calc R . . . .
C36 C 0.9957(6) 0.6552(6) 0.8284(6) 0.123(3) Uani 1 1 d . . . . .
H36A H 0.9929 0.7069 0.8325 0.185 Uiso 1 1 calc GR . . . .
H36B H 1.0530 0.6412 0.8305 0.185 Uiso 1 1 calc GR . . . .
H36C H 0.9835 0.6336 0.8795 0.185 Uiso 1 1 calc GR . . . .
C37 C 0.9348(6) 0.6660(6) 0.6588(6) 0.123(3) Uani 1 1 d . . . . .
H37A H 0.8934 0.6424 0.6065 0.185 Uiso 1 1 calc GR . . . .
H37B H 0.9921 0.6618 0.6550 0.185 Uiso 1 1 calc GR . . . .
H37C H 0.9197 0.7161 0.6591 0.185 Uiso 1 1 calc GR . . . .
S1 S 0.84293(14) 0.65991(11) 0.38119(14) 0.0808(5) Uani 1 1 d . . . . .
F1 F 0.8980(4) 0.5784(4) 0.2834(4) 0.148(2) Uani 1 1 d . . . . .
F2 F 0.8859(4) 0.6850(4) 0.2439(4) 0.139(2) Uani 1 1 d . . . . .
F3 F 0.9883(4) 0.6533(4) 0.3583(4) 0.155(3) Uani 1 1 d . . . . .
O11 O 0.8695(4) 0.6065(3) 0.4465(4) 0.1072(19) Uani 1 1 d . . . . .
O12 O 0.8641(4) 0.7302(3) 0.4152(4) 0.1037(19) Uani 1 1 d . . . . .
O13 O 0.7582(3) 0.6501(3) 0.3170(4) 0.0934(16) Uani 1 1 d . . . . .
C41 C 0.8928(6) 0.6409(4) 0.3185(5) 0.090(3) Uani 1 1 d . . . . .
O10 O 0.8359(3) 0.2147(3) 0.7758(3) 0.0798(14) Uani 1 1 d . . . . .
N6 N 0.9045(3) 0.3197(3) 0.8160(3) 0.0584(13) Uani 1 1 d . . . . .
C38 C 0.8538(4) 0.2740(4) 0.7591(4) 0.0630(17) Uani 1 1 d . . . . .
H38 H 0.8286 0.2893 0.6981 0.076 Uiso 1 1 calc R . . . .
C39 C 0.9427(4) 0.3014(5) 0.9126(4) 0.084(2) Uani 1 1 d . . . . .
H39A H 0.9186 0.3319 0.9482 0.127 Uiso 1 1 calc GR . . . .
H39B H 1.0046 0.3082 0.9324 0.127 Uiso 1 1 calc GR . . . .
H39C H 0.9302 0.2517 0.9215 0.127 Uiso 1 1 calc GR . . . .
C40 C 0.9172(4) 0.3908(4) 0.7898(5) 0.078(2) Uani 1 1 d . . . . .
H40A H 0.8810 0.3988 0.7267 0.117 Uiso 1 1 calc GR . . . .
H40B H 0.9773 0.3972 0.7957 0.117 Uiso 1 1 calc GR . . . .
H40C H 0.9022 0.4247 0.8291 0.117 Uiso 1 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 Ni1 3.4710(5) . ?
Dy1 O2 2.172(3) . ?
Dy1 O3 2.428(3) . ?
Dy1 O4 2.549(3) . ?
Dy1 O5 2.285(3) . ?
Dy1 O6 2.358(3) 3_666 ?
Dy1 O8 2.350(3) . ?
Dy1 O9 2.406(3) . ?
Dy1 N1 2.477(3) . ?
Ni1 O3 2.076(3) . ?
Ni1 O3 2.130(3) 3_666 ?
Ni1 O5 2.020(3) . ?
Ni1 O6 2.069(3) . ?
Ni1 O7 2.072(3) . ?
Ni1 N2 2.011(3) . ?
O1 C1 1.406(6) . ?
O1 C2 1.369(6) . ?
O2 C7 1.308(5) . ?
O3 Ni1 2.130(3) 3_666 ?
O3 C14 1.366(5) . ?
O4 C15 1.436(5) . ?
O4 C16 1.378(5) . ?
O5 C21 1.331(5) . ?
O6 Dy1 2.358(3) 3_666 ?
O6 C28 1.343(5) . ?
O7 C29 1.230(5) . ?
O8 C32 1.239(5) . ?
O9 C35 1.235(6) . ?
N1 C8 1.291(5) . ?
N1 C9 1.422(5) . ?
N2 C22 1.287(5) . ?
N2 C23 1.417(5) . ?
N3 C29 1.309(6) . ?
N3 C30 1.440(8) . ?
N3 C31 1.450(7) . ?
N4 C32 1.312(6) . ?
N4 C33 1.451(6) . ?
N4 C34 1.470(5) . ?
N5 C35 1.283(7) . ?
N5 C36 1.442(9) . ?
N5 C37 1.501(11) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.376(7) . ?
C2 C7 1.425(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.400(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.366(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.411(6) . ?
C6 C7 1.405(6) . ?
C6 C8 1.438(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.396(6) . ?
C9 C14 1.408(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.378(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.386(6) . ?
C12 H12 0.9500 . ?
C12 C13 1.388(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.385(6) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.378(6) . ?
C16 C21 1.413(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.398(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.371(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.413(6) . ?
C20 C21 1.410(6) . ?
C20 C22 1.436(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.397(5) . ?
C23 C28 1.408(6) . ?
C24 H24 0.9500 . ?
C24 C25 1.378(6) . ?
C25 H25 0.9500 . ?
C25 C26 1.386(7) . ?
C26 H26 0.9500 . ?
C26 C27 1.385(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.394(6) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35 0.9500 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
S1 O11 1.397(5) . ?
S1 O12 1.429(5) . ?
S1 O13 1.439(5) . ?
S1 C41 1.533(9) . ?
F1 C41 1.317(9) . ?
F2 C41 1.408(9) . ?
F3 C41 1.515(11) . ?
O10 C38 1.210(8) . ?
N6 C38 1.318(8) . ?
N6 C39 1.471(8) . ?
N6 C40 1.440(8) . ?
C38 H38 0.9500 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 Ni1 169.21(8) . . ?
O2 Dy1 O3 137.10(10) . . ?
O2 Dy1 O4 84.63(10) . . ?
O2 Dy1 O5 148.50(10) . . ?
O2 Dy1 O6 85.55(11) . 3_666 ?
O2 Dy1 O8 107.47(11) . . ?
O2 Dy1 O9 77.57(11) . . ?
O2 Dy1 N1 74.06(11) . . ?
O3 Dy1 Ni1 36.02(6) . . ?
O3 Dy1 O4 123.06(9) . . ?
O3 Dy1 N1 67.15(10) . . ?
O4 Dy1 Ni1 95.12(7) . . ?
O5 Dy1 Ni1 33.76(7) . . ?
O5 Dy1 O3 69.18(9) . . ?
O5 Dy1 O4 63.97(9) . . ?
O5 Dy1 O6 90.53(9) . 3_666 ?
O5 Dy1 O8 93.50(10) . . ?
O5 Dy1 O9 87.87(11) . . ?
O5 Dy1 N1 136.00(10) . . ?
O6 Dy1 Ni1 83.82(7) 3_666 . ?
O6 Dy1 O3 70.85(9) 3_666 . ?
O6 Dy1 O4 78.94(9) 3_666 . ?
O6 Dy1 O9 144.08(10) 3_666 . ?
O6 Dy1 N1 80.34(10) 3_666 . ?
O8 Dy1 Ni1 80.54(7) . . ?
O8 Dy1 O3 78.18(9) . . ?
O8 Dy1 O4 133.41(10) . . ?
O8 Dy1 O6 144.97(10) . 3_666 ?
O8 Dy1 O9 70.91(11) . . ?
O8 Dy1 N1 72.72(10) . . ?
O9 Dy1 Ni1 112.40(8) . . ?
O9 Dy1 O3 140.10(9) . . ?
O9 Dy1 O4 68.19(10) . . ?
O9 Dy1 N1 123.58(11) . . ?
N1 Dy1 Ni1 102.25(8) . . ?
N1 Dy1 O4 151.24(10) . . ?
O3 Ni1 Dy1 43.45(7) . . ?
O3 Ni1 Dy1 92.76(7) 3_666 . ?
O3 Ni1 O3 82.11(11) . 3_666 ?
O5 Ni1 Dy1 38.95(8) . . ?
O5 Ni1 O3 81.65(11) . . ?
O5 Ni1 O3 92.45(11) . 3_666 ?
O5 Ni1 O6 168.58(11) . . ?
O5 Ni1 O7 98.14(12) . . ?
O6 Ni1 Dy1 151.16(7) . . ?
O6 Ni1 O3 107.76(10) . . ?
O6 Ni1 O3 82.71(10) . 3_666 ?
O6 Ni1 O7 88.62(11) . . ?
O7 Ni1 Dy1 89.04(8) . . ?
O7 Ni1 O3 165.17(11) . 3_666 ?
O7 Ni1 O3 89.16(10) . . ?
N2 Ni1 Dy1 127.06(10) . . ?
N2 Ni1 O3 170.45(13) . . ?
N2 Ni1 O3 101.06(12) . 3_666 ?
N2 Ni1 O5 89.17(12) . . ?
N2 Ni1 O6 81.66(12) . . ?
N2 Ni1 O7 89.50(12) . . ?
C2 O1 C1 118.0(4) . . ?
C7 O2 Dy1 142.1(3) . . ?
Ni1 O3 Dy1 100.53(10) . . ?
Ni1 O3 Dy1 100.73(10) 3_666 . ?
Ni1 O3 Ni1 97.89(11) . 3_666 ?
C14 O3 Dy1 113.1(2) . . ?
C14 O3 Ni1 115.0(2) . 3_666 ?
C14 O3 Ni1 125.7(2) . . ?
C15 O4 Dy1 124.2(3) . . ?
C16 O4 Dy1 116.6(2) . . ?
C16 O4 C15 117.2(3) . . ?
Ni1 O5 Dy1 107.29(11) . . ?
C21 O5 Dy1 126.5(2) . . ?
C21 O5 Ni1 125.0(3) . . ?
Ni1 O6 Dy1 104.95(10) . 3_666 ?
C28 O6 Dy1 124.3(2) . 3_666 ?
C28 O6 Ni1 106.9(2) . . ?
C29 O7 Ni1 128.5(3) . . ?
C32 O8 Dy1 134.6(3) . . ?
C35 O9 Dy1 129.2(3) . . ?
C8 N1 Dy1 128.7(3) . . ?
C8 N1 C9 119.5(3) . . ?
C9 N1 Dy1 111.7(2) . . ?
C22 N2 Ni1 127.4(3) . . ?
C22 N2 C23 123.5(3) . . ?
C23 N2 Ni1 109.1(3) . . ?
C29 N3 C30 120.5(5) . . ?
C29 N3 C31 121.6(6) . . ?
C30 N3 C31 117.8(5) . . ?
C32 N4 C33 120.6(4) . . ?
C32 N4 C34 122.0(4) . . ?
C33 N4 C34 117.4(4) . . ?
C35 N5 C36 124.6(6) . . ?
C35 N5 C37 117.0(6) . . ?
C36 N5 C37 117.3(6) . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 125.3(4) . . ?
O1 C2 C7 114.0(4) . . ?
C3 C2 C7 120.7(5) . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.5(5) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 120.2 . . ?
C5 C4 C3 119.5(4) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.6(4) . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C8 117.8(4) . . ?
C7 C6 C5 119.2(4) . . ?
C7 C6 C8 123.0(4) . . ?
O2 C7 C2 118.2(4) . . ?
O2 C7 C6 123.3(4) . . ?
C6 C7 C2 118.4(4) . . ?
N1 C8 C6 127.5(4) . . ?
N1 C8 H8 116.3 . . ?
C6 C8 H8 116.3 . . ?
C10 C9 N1 123.9(4) . . ?
C10 C9 C14 119.1(4) . . ?
C14 C9 N1 116.9(3) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.4(4) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 119.8 . . ?
C10 C11 C12 120.5(4) . . ?
C12 C11 H11 119.8 . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.7(4) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.6(4) . . ?
C14 C13 H13 119.7 . . ?
O3 C14 C9 118.8(3) . . ?
O3 C14 C13 121.5(4) . . ?
C13 C14 C9 119.7(4) . . ?
O4 C15 H15A 109.5 . . ?
O4 C15 H15B 109.5 . . ?
O4 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O4 C16 C21 113.3(4) . . ?
C17 C16 O4 124.5(4) . . ?
C17 C16 C21 122.2(4) . . ?
C16 C17 H17 120.7 . . ?
C16 C17 C18 118.6(4) . . ?
C18 C17 H17 120.7 . . ?
C17 C18 H18 119.6 . . ?
C19 C18 C17 120.8(4) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 H19 119.4 . . ?
C18 C19 C20 121.3(4) . . ?
C20 C19 H19 119.4 . . ?
C19 C20 C22 117.6(4) . . ?
C21 C20 C19 118.6(4) . . ?
C21 C20 C22 123.7(4) . . ?
O5 C21 C16 117.3(4) . . ?
O5 C21 C20 124.3(4) . . ?
C20 C21 C16 118.4(4) . . ?
N2 C22 C20 125.3(4) . . ?
N2 C22 H22 117.3 . . ?
C20 C22 H22 117.3 . . ?
C24 C23 N2 124.5(4) . . ?
C24 C23 C28 120.8(4) . . ?
C28 C23 N2 114.5(3) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 119.9(4) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 120.0(4) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 119.8 . . ?
C27 C26 C25 120.3(4) . . ?
C27 C26 H26 119.8 . . ?
C26 C27 H27 119.5 . . ?
C26 C27 C28 121.1(4) . . ?
C28 C27 H27 119.5 . . ?
O6 C28 C23 119.8(4) . . ?
O6 C28 C27 122.3(4) . . ?
C27 C28 C23 117.8(4) . . ?
O7 C29 N3 124.1(5) . . ?
O7 C29 H29 117.9 . . ?
N3 C29 H29 117.9 . . ?
N3 C30 H30A 109.5 . . ?
N3 C30 H30B 109.5 . . ?
N3 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N3 C31 H31A 109.5 . . ?
N3 C31 H31B 109.5 . . ?
N3 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O8 C32 N4 123.7(4) . . ?
O8 C32 H32 118.2 . . ?
N4 C32 H32 118.2 . . ?
N4 C33 H33A 109.5 . . ?
N4 C33 H33B 109.5 . . ?
N4 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N4 C34 H34A 109.5 . . ?
N4 C34 H34B 109.5 . . ?
N4 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O9 C35 N5 126.8(6) . . ?
O9 C35 H35 116.6 . . ?
N5 C35 H35 116.6 . . ?
N5 C36 H36A 109.5 . . ?
N5 C36 H36B 109.5 . . ?
N5 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N5 C37 H37A 109.5 . . ?
N5 C37 H37B 109.5 . . ?
N5 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O11 S1 O12 114.8(4) . . ?
O11 S1 O13 114.3(4) . . ?
O11 S1 C41 101.4(4) . . ?
O12 S1 O13 116.0(4) . . ?
O12 S1 C41 109.8(4) . . ?
O13 S1 C41 97.9(4) . . ?
F1 C41 S1 127.2(8) . . ?
F1 C41 F2 100.4(7) . . ?
F1 C41 F3 95.8(7) . . ?
F2 C41 S1 119.2(6) . . ?
F2 C41 F3 91.7(7) . . ?
F3 C41 S1 115.0(6) . . ?
C38 N6 C39 119.8(6) . . ?
C38 N6 C40 122.5(6) . . ?
C40 N6 C39 117.3(6) . . ?
O10 C38 N6 127.3(6) . . ?
O10 C38 H38 116.4 . . ?
N6 C38 H38 116.4 . . ?
N6 C39 H39A 109.5 . . ?
N6 C39 H39B 109.5 . . ?
N6 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N6 C40 H40A 109.5 . . ?
N6 C40 H40B 109.5 . . ?
N6 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Dy1 O2 C7 C2 -167.4(3) . . . . ?
Dy1 O2 C7 C6 10.3(7) . . . . ?
Dy1 O3 C14 C9 30.9(4) . . . . ?
Dy1 O3 C14 C13 -150.3(3) . . . . ?
Dy1 O4 C16 C17 -168.6(3) . . . . ?
Dy1 O4 C16 C21 14.0(4) . . . . ?
Dy1 O5 C21 C16 -9.7(5) . . . . ?
Dy1 O5 C21 C20 171.5(3) . . . . ?
Dy1 O6 C28 C23 100.7(4) 3_666 . . . ?
Dy1 O6 C28 C27 -79.2(4) 3_666 . . . ?
Dy1 O8 C32 N4 -171.2(3) . . . . ?
Dy1 O9 C35 N5 -168.5(5) . . . . ?
Dy1 N1 C8 C6 -7.7(6) . . . . ?
Dy1 N1 C9 C10 154.0(3) . . . . ?
Dy1 N1 C9 C14 -21.9(4) . . . . ?
Ni1 O3 C14 C9 154.4(3) . . . . ?
Ni1 O3 C14 C9 -84.1(4) 3_666 . . . ?
Ni1 O3 C14 C13 -26.7(5) . . . . ?
Ni1 O3 C14 C13 94.7(4) 3_666 . . . ?
Ni1 O5 C21 C16 155.9(3) . . . . ?
Ni1 O5 C21 C20 -22.9(5) . . . . ?
Ni1 O6 C28 C23 -21.5(4) . . . . ?
Ni1 O6 C28 C27 158.6(3) . . . . ?
Ni1 O7 C29 N3 -136.2(4) . . . . ?
Ni1 N2 C22 C20 1.3(6) . . . . ?
Ni1 N2 C23 C24 -157.2(3) . . . . ?
Ni1 N2 C23 C28 18.5(4) . . . . ?
O1 C2 C3 C4 176.5(5) . . . . ?
O1 C2 C7 O2 1.6(6) . . . . ?
O1 C2 C7 C6 -176.2(4) . . . . ?
O4 C16 C17 C18 -175.7(4) . . . . ?
O4 C16 C21 O5 -4.3(5) . . . . ?
O4 C16 C21 C20 174.5(3) . . . . ?
N1 C9 C10 C11 -176.4(4) . . . . ?
N1 C9 C14 O3 -5.5(5) . . . . ?
N1 C9 C14 C13 175.6(3) . . . . ?
N2 C23 C24 C25 178.0(4) . . . . ?
N2 C23 C28 O6 2.7(5) . . . . ?
N2 C23 C28 C27 -177.4(4) . . . . ?
C1 O1 C2 C3 -9.5(8) . . . . ?
C1 O1 C2 C7 169.2(5) . . . . ?
C2 C3 C4 C5 0.6(8) . . . . ?
C3 C2 C7 O2 -179.7(4) . . . . ?
C3 C2 C7 C6 2.5(7) . . . . ?
C3 C4 C5 C6 0.5(7) . . . . ?
C4 C5 C6 C7 0.0(7) . . . . ?
C4 C5 C6 C8 -179.7(4) . . . . ?
C5 C6 C7 O2 -179.2(4) . . . . ?
C5 C6 C7 C2 -1.5(6) . . . . ?
C5 C6 C8 N1 179.6(4) . . . . ?
C7 C2 C3 C4 -2.1(8) . . . . ?
C7 C6 C8 N1 -0.1(7) . . . . ?
C8 N1 C9 C10 -28.3(6) . . . . ?
C8 N1 C9 C14 155.9(4) . . . . ?
C8 C6 C7 O2 0.5(7) . . . . ?
C8 C6 C7 C2 178.2(4) . . . . ?
C9 N1 C8 C6 175.0(4) . . . . ?
C9 C10 C11 C12 1.1(6) . . . . ?
C10 C9 C14 O3 178.4(3) . . . . ?
C10 C9 C14 C13 -0.5(6) . . . . ?
C10 C11 C12 C13 -0.5(6) . . . . ?
C11 C12 C13 C14 -0.6(6) . . . . ?
C12 C13 C14 O3 -177.8(4) . . . . ?
C12 C13 C14 C9 1.1(6) . . . . ?
C14 C9 C10 C11 -0.6(6) . . . . ?
C15 O4 C16 C17 -4.0(6) . . . . ?
C15 O4 C16 C21 178.6(4) . . . . ?
C16 C17 C18 C19 0.4(7) . . . . ?
C17 C16 C21 O5 178.2(4) . . . . ?
C17 C16 C21 C20 -2.9(6) . . . . ?
C17 C18 C19 C20 -0.9(7) . . . . ?
C18 C19 C20 C21 -0.6(7) . . . . ?
C18 C19 C20 C22 178.1(4) . . . . ?
C19 C20 C21 O5 -178.8(4) . . . . ?
C19 C20 C21 C16 2.4(6) . . . . ?
C19 C20 C22 N2 -169.4(4) . . . . ?
C21 C16 C17 C18 1.5(6) . . . . ?
C21 C20 C22 N2 9.2(7) . . . . ?
C22 N2 C23 C24 20.8(6) . . . . ?
C22 N2 C23 C28 -163.4(4) . . . . ?
C22 C20 C21 O5 2.6(6) . . . . ?
C22 C20 C21 C16 -176.2(4) . . . . ?
C23 N2 C22 C20 -176.4(4) . . . . ?
C23 C24 C25 C26 -0.8(6) . . . . ?
C24 C23 C28 O6 178.6(4) . . . . ?
C24 C23 C28 C27 -1.5(6) . . . . ?
C24 C25 C26 C27 -1.8(7) . . . . ?
C25 C26 C27 C28 2.9(7) . . . . ?
C26 C27 C28 O6 178.7(4) . . . . ?
C26 C27 C28 C23 -1.2(6) . . . . ?
C28 C23 C24 C25 2.5(6) . . . . ?
C30 N3 C29 O7 4.1(8) . . . . ?
C31 N3 C29 O7 179.3(5) . . . . ?
C33 N4 C32 O8 2.8(7) . . . . ?
C34 N4 C32 O8 -176.9(4) . . . . ?
C36 N5 C35 O9 179.3(7) . . . . ?
C37 N5 C35 O9 11.4(10) . . . . ?
O11 S1 C41 F1 49.4(9) . . . . ?
O11 S1 C41 F2 -177.5(7) . . . . ?
O11 S1 C41 F3 -70.2(7) . . . . ?
O12 S1 C41 F1 171.2(8) . . . . ?
O12 S1 C41 F2 -55.7(8) . . . . ?
O12 S1 C41 F3 51.6(7) . . . . ?
O13 S1 C41 F1 -67.5(8) . . . . ?
O13 S1 C41 F2 65.7(8) . . . . ?
O13 S1 C41 F3 173.0(6) . . . . ?
C39 N6 C38 O10 -3.0(10) . . . . ?
C40 N6 C38 O10 -176.0(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
