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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_Compound_1
_database_code_depnum_ccdc_archive 'CCDC 1579341'
_audit_update_record             
;
2018-01-04 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;
_audit_creation_date             2018-01-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1(C82 H90 Co3 La3 N3 O27), 1(Cl1 O4)'
_chemical_formula_sum            'C82 H90 Cl Co3 La3 N3 O31'
_chemical_formula_weight         2242.56
_chemical_absolute_configuration ?
_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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   18.6310(11)
_cell_length_b                   18.6310(11)
_cell_length_c                   54.176(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     16286(2)
_cell_formula_units_Z            5.99994
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      2.19
_shelx_estimated_absorpt_T_max   0.750
_shelx_estimated_absorpt_T_min   0.677
_exptl_absorpt_coefficient_mu    1.694
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.5902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6720
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0999
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            55571
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         1.469
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.975
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                6632
_reflns_number_total             7901
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.898
_refine_diff_density_min         -0.969
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7901
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0525
_refine_ls_restrained_S_all      1.024
_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)+(0.0905P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1335
_refine_special_details          SQUEEZE
_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. Uiso/Uaniso restraints and constraints
Uanis(C00N) = Uanis(C018)
3.a Secondary CH2 refined with riding coordinates:
 C00S(H00A,H00B), C00X(H00F,H00G), C00Z(H00M,H00N)
3.b Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00L(H00L), C00O(H00O), C00R(H00R), C00V(H00V), C012(H012)
3.c Idealised Me refined as rotating group:
 C00T(H00C,H00D,H00E), C00Y(H00I,H00J,H00K), C010(H01A,H01B,H01C), C013(H01D,
 H01E,H01F), C016(H01G,H01H,H01I), C018(H01J,H01K,H01L)
;
_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
La1 La 0.59635(3) 0.18239(3) 0.50045(2) 0.02258(15) Uani 1 1 d . . . . .
Co1 Co 0.42052(8) 0.19843(7) 0.51121(2) 0.0226(3) Uani 1 1 d . . . . .
O4 O 0.4759(4) 0.4552(4) 0.50611(12) 0.0316(15) Uani 1 1 d . . . . .
O1 O 0.4474(4) 0.1210(4) 0.49371(11) 0.0254(13) Uani 1 1 d . . . . .
O7 O 0.5505(4) 0.2716(4) 0.52079(12) 0.0252(13) Uani 1 1 d . . . . .
O5 O 0.3996(4) 0.1687(4) 0.54646(11) 0.0324(14) Uani 1 1 d . . . . .
O3 O 0.4364(4) 0.3032(4) 0.49586(12) 0.0288(14) Uani 1 1 d . . . . .
O8 O 0.7065(4) 0.2937(4) 0.47196(12) 0.0283(14) Uani 1 1 d . . . . .
O9 O 0.5696(4) 0.1435(5) 0.54663(14) 0.0357(16) Uani 1 1 d . . . . .
O6 O 0.4272(5) 0.0739(5) 0.57701(14) 0.0461(19) Uani 1 1 d . . . . .
O2 O 0.5376(4) 0.1101(4) 0.45857(13) 0.0347(15) Uani 1 1 d . . . . .
C00E C 0.666667 0.333333 0.4707(3) 0.027(3) Uani 1 3 d S T P . .
C00F C 0.4083(6) 0.0819(5) 0.47233(17) 0.0263(19) Uani 1 1 d . . . . .
C00G C 0.3946(6) 0.4019(6) 0.50193(19) 0.034(2) Uani 1 1 d . . . . .
C00H C 0.4173(6) 0.0368(6) 0.43148(18) 0.034(2) Uani 1 1 d . . . . .
H00H H 0.450186 0.033059 0.418674 0.041 Uiso 1 1 calc R . . . .
C00I C 0.2925(6) 0.2612(6) 0.49046(18) 0.030(2) Uani 1 1 d . . . . .
C00J C 0.3740(5) 0.3194(6) 0.49615(17) 0.0267(18) Uani 1 1 d . . . . .
C00K C 0.3363(6) 0.0952(6) 0.55194(18) 0.035(2) Uani 1 1 d . . . . .
C00L C 0.3307(6) 0.4213(6) 0.50302(19) 0.033(2) Uani 1 1 d . . . . .
H00L H 0.343764 0.476160 0.507008 0.040 Uiso 1 1 calc R . . . .
N1 N 0.2932(5) 0.1295(5) 0.50080(16) 0.0279(17) Uani 1 1 d . . . . .
C00N C 0.4551(8) 0.0759(9) 0.4534(2) 0.052(2) Uani 1 1 d . . . . .
C00O C 0.2313(6) 0.2833(6) 0.49203(19) 0.036(2) Uani 1 1 d . . . . .
H00O H 0.175617 0.242386 0.488557 0.043 Uiso 1 1 calc R . . . .
C00P C 0.2478(6) 0.3606(7) 0.4983(2) 0.039(2) Uani 1 1 d . . . . .
C00Q C 0.3230(6) 0.0478(5) 0.46912(18) 0.031(2) Uani 1 1 d . . . . .
C00R C 0.2867(7) 0.0097(6) 0.44649(19) 0.037(2) Uani 1 1 d . . . . .
H00R H 0.229035 -0.011851 0.444095 0.045 Uiso 1 1 calc R . . . .
C00S C 0.2707(6) 0.0466(6) 0.49039(19) 0.035(2) Uani 1 1 d . . . . .
H00A H 0.212196 0.019046 0.484926 0.042 Uiso 1 1 calc R . . . .
H00B H 0.274557 0.012451 0.503756 0.042 Uiso 1 1 calc R . . . .
C00T C 0.1817(7) 0.3836(9) 0.4997(3) 0.051(3) Uani 1 1 d . . . . .
H00C H 0.148484 0.359546 0.514656 0.076 Uiso 1 1 calc GR . . . .
H00D H 0.145868 0.362269 0.485160 0.076 Uiso 1 1 calc GR . . . .
H00E H 0.207331 0.444074 0.500293 0.076 Uiso 1 1 calc GR . . . .
C00U C 0.3329(7) 0.0029(7) 0.4278(2) 0.043(3) Uani 1 1 d . . . . .
C00V C 0.1917(8) -0.0121(7) 0.5488(2) 0.048(3) Uani 1 1 d . . . . .
H00V H 0.138354 -0.030021 0.541971 0.058 Uiso 1 1 calc R . . . .
C00W C 0.2574(6) 0.0653(6) 0.54236(19) 0.038(2) Uani 1 1 d . . . . .
C00X C 0.2437(7) 0.1174(6) 0.5240(2) 0.036(2) Uani 1 1 d . . . . .
H00F H 0.260112 0.172109 0.531383 0.043 Uiso 1 1 calc R . . . .
H00G H 0.184027 0.090258 0.519807 0.043 Uiso 1 1 calc R . . . .
C00Y C 0.4386(10) 0.0298(11) 0.5970(3) 0.076(4) Uani 1 1 d . . . . .
H00I H 0.412049 -0.029263 0.592821 0.114 Uiso 1 1 calc GR . . . .
H00J H 0.413521 0.036752 0.612015 0.114 Uiso 1 1 calc GR . . . .
H00K H 0.497968 0.051682 0.599688 0.114 Uiso 1 1 calc GR . . . .
C00Z C 0.2723(6) 0.1757(6) 0.48225(19) 0.033(2) Uani 1 1 d . . . . .
H00M H 0.212321 0.142924 0.478496 0.039 Uiso 1 1 calc R . . . .
H00N H 0.302832 0.180803 0.466793 0.039 Uiso 1 1 calc R . . . .
C010 C 0.4979(7) 0.5354(7) 0.5155(2) 0.046(3) Uani 1 1 d . . . . .
H01A H 0.474724 0.529722 0.532140 0.069 Uiso 1 1 calc GR . . . .
H01B H 0.475657 0.561625 0.504651 0.069 Uiso 1 1 calc GR . . . .
H01C H 0.558404 0.569876 0.516292 0.069 Uiso 1 1 calc GR . . . .
C012 C 0.2823(9) -0.0357(7) 0.5749(2) 0.053(3) Uani 1 1 d . . . . .
H012 H 0.291837 -0.070301 0.585725 0.064 Uiso 1 1 calc R . . . .
C013 C 0.1313(10) -0.1447(9) 0.5732(4) 0.082(5) Uani 1 1 d . . . . .
H01D H 0.095669 -0.134481 0.584240 0.124 Uiso 1 1 calc GR . . . .
H01E H 0.151572 -0.177163 0.581927 0.124 Uiso 1 1 calc GR . . . .
H01F H 0.099384 -0.175570 0.558682 0.124 Uiso 1 1 calc GR . . . .
C014 C 0.3484(7) 0.0435(6) 0.56885(19) 0.040(2) Uani 1 1 d . . . . .
C015 C 0.2027(8) -0.0644(7) 0.5653(2) 0.055(3) Uani 1 1 d . . . . .
C016 C 0.2912(9) -0.0378(8) 0.4032(2) 0.057(3) Uani 1 1 d . . . . .
H01G H 0.271124 -0.004138 0.395120 0.085 Uiso 1 1 calc GR . . . .
H01H H 0.244446 -0.093427 0.406401 0.085 Uiso 1 1 calc GR . . . .
H01I H 0.331467 -0.041712 0.392511 0.085 Uiso 1 1 calc GR . . . .
C018 C 0.5903(7) 0.1042(8) 0.4407(2) 0.052(2) Uani 1 1 d . . . . .
H01J H 0.590870 0.133978 0.425690 0.079 Uiso 1 1 calc GR . . . .
H01K H 0.569652 0.045792 0.436686 0.079 Uiso 1 1 calc GR . . . .
H01L H 0.646627 0.128777 0.447310 0.079 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.000000 0.000000 0.48474(15) 0.0619(15) Uani 1 3 d S T P . .
O10 O 0.0471(9) -0.0319(8) 0.4760(4) 0.134(7) Uani 1 1 d . . . . .
O11 O 0.000000 0.000000 0.5109(6) 0.18(2) Uani 1 3 d S T 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
La1 Co1 3.5604(13) 2_655 ?
La1 Co1 3.4844(13) . ?
La1 O4 2.682(6) 2_655 ?
La1 O1 2.443(6) . ?
La1 O7 2.466(6) 2_655 ?
La1 O7 2.475(6) . ?
La1 O3 2.473(6) 2_655 ?
La1 O8 2.655(6) 3_665 ?
La1 O8 2.577(6) . ?
La1 O9 2.583(7) . ?
La1 O2 2.586(7) . ?
La1 C00E 2.921(10) . ?
Co1 O1 1.988(6) . ?
Co1 O7 2.165(7) . ?
Co1 O5 1.972(6) . ?
Co1 O3 2.003(6) . ?
Co1 N1 2.133(8) . ?
O4 C00G 1.352(11) . ?
O4 C010 1.432(13) . ?
O1 C00F 1.369(11) . ?
O5 C00K 1.319(12) . ?
O3 C00J 1.340(11) . ?
O8 C00E 1.285(7) . ?
O6 C00Y 1.437(14) . ?
O6 C014 1.356(13) . ?
O2 C00N 1.365(14) . ?
O2 C018 1.423(13) . ?
C00F C00N 1.387(14) . ?
C00F C00Q 1.396(13) . ?
C00G C00J 1.420(13) . ?
C00G C00L 1.408(13) . ?
C00H H00H 0.9500 . ?
C00H C00N 1.387(14) . ?
C00H C00U 1.386(15) . ?
C00I C00J 1.390(13) . ?
C00I C00O 1.394(13) . ?
C00I C00Z 1.509(14) . ?
C00K C00W 1.386(15) . ?
C00K C014 1.428(15) . ?
C00L H00L 0.9500 . ?
C00L C00P 1.410(14) . ?
N1 C00S 1.494(12) . ?
N1 C00X 1.507(13) . ?
N1 C00Z 1.496(13) . ?
C00O H00O 0.9500 . ?
C00O C00P 1.357(15) . ?
C00P C00T 1.495(14) . ?
C00Q C00R 1.408(13) . ?
C00Q C00S 1.502(14) . ?
C00R H00R 0.9500 . ?
C00R C00U 1.375(16) . ?
C00S H00A 0.9900 . ?
C00S H00B 0.9900 . ?
C00T H00C 0.9800 . ?
C00T H00D 0.9800 . ?
C00T H00E 0.9800 . ?
C00U C016 1.535(15) . ?
C00V H00V 0.9500 . ?
C00V C00W 1.392(15) . ?
C00V C015 1.410(17) . ?
C00W C00X 1.499(14) . ?
C00X H00F 0.9900 . ?
C00X H00G 0.9900 . ?
C00Y H00I 0.9800 . ?
C00Y H00J 0.9800 . ?
C00Y H00K 0.9800 . ?
C00Z H00M 0.9900 . ?
C00Z H00N 0.9900 . ?
C010 H01A 0.9800 . ?
C010 H01B 0.9800 . ?
C010 H01C 0.9800 . ?
C012 H012 0.9500 . ?
C012 C014 1.409(15) . ?
C012 C015 1.403(19) . ?
C013 H01D 0.9800 . ?
C013 H01E 0.9800 . ?
C013 H01F 0.9800 . ?
C013 C015 1.485(16) . ?
C016 H01G 0.9800 . ?
C016 H01H 0.9800 . ?
C016 H01I 0.9800 . ?
C018 H01J 0.9800 . ?
C018 H01K 0.9800 . ?
C018 H01L 0.9800 . ?
Cl1 O10 1.366(17) 2 ?
Cl1 O10 1.366(17) . ?
Cl1 O10 1.366(17) 3 ?
Cl1 O11 1.42(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
Co1 La1 Co1 155.89(4) . 2_655 ?
O4 La1 Co1 104.66(14) 2_655 . ?
O4 La1 Co1 87.64(14) 2_655 2_655 ?
O4 La1 C00E 151.7(3) 2_655 . ?
O1 La1 Co1 166.44(15) . 2_655 ?
O1 La1 Co1 33.75(15) . . ?
O1 La1 O4 78.8(2) . 2_655 ?
O1 La1 O7 153.4(2) . 2_655 ?
O1 La1 O7 71.8(2) . . ?
O1 La1 O3 134.8(2) . 2_655 ?
O1 La1 O8 77.1(2) . 3_665 ?
O1 La1 O8 123.3(2) . . ?
O1 La1 O9 89.9(2) . . ?
O1 La1 O2 62.5(2) . . ?
O1 La1 C00E 103.07(18) . . ?
O7 La1 Co1 120.07(16) 2_655 . ?
O7 La1 Co1 118.89(16) . 2_655 ?
O7 La1 Co1 38.07(16) . . ?
O7 La1 Co1 36.75(16) 2_655 2_655 ?
O7 La1 O4 130.8(2) . 2_655 ?
O7 La1 O4 115.7(2) 2_655 2_655 ?
O7 La1 O7 82.3(3) 2_655 . ?
O7 La1 O3 69.6(2) 2_655 2_655 ?
O7 La1 O8 63.7(2) . 3_665 ?
O7 La1 O8 65.0(2) 2_655 . ?
O7 La1 O8 97.5(2) . . ?
O7 La1 O8 97.0(2) 2_655 3_665 ?
O7 La1 O9 75.7(2) 2_655 . ?
O7 La1 O9 71.0(2) . . ?
O7 La1 O2 122.8(2) . . ?
O7 La1 O2 141.3(2) 2_655 . ?
O7 La1 C00E 74.8(3) . . ?
O7 La1 C00E 75.0(3) 2_655 . ?
O3 La1 Co1 32.92(15) 2_655 2_655 ?
O3 La1 Co1 165.15(15) 2_655 . ?
O3 La1 O4 60.5(2) 2_655 2_655 ?
O3 La1 O7 150.8(2) 2_655 . ?
O3 La1 O8 125.9(2) 2_655 3_665 ?
O3 La1 O8 78.0(2) 2_655 . ?
O3 La1 O9 94.0(2) 2_655 . ?
O3 La1 O2 85.5(2) 2_655 . ?
O3 La1 C00E 104.06(18) 2_655 . ?
O8 La1 Co1 65.81(16) . 2_655 ?
O8 La1 Co1 66.46(15) 3_665 . ?
O8 La1 Co1 114.48(16) 3_665 2_655 ?
O8 La1 Co1 115.85(16) . . ?
O8 La1 O4 144.6(2) 3_665 2_655 ?
O8 La1 O4 131.8(2) . 2_655 ?
O8 La1 O8 50.2(3) . 3_665 ?
O8 La1 O9 140.4(2) . . ?
O8 La1 O2 81.6(2) . . ?
O8 La1 C00E 26.08(17) 3_665 . ?
O8 La1 C00E 26.07(18) . . ?
O9 La1 Co1 78.72(13) . . ?
O9 La1 Co1 86.33(14) . 2_655 ?
O9 La1 O4 70.3(2) . 2_655 ?
O9 La1 O8 134.7(2) . 3_665 ?
O9 La1 O2 137.0(2) . . ?
O9 La1 C00E 137.3(3) . . ?
O2 La1 Co1 91.14(15) . . ?
O2 La1 Co1 112.53(15) . 2_655 ?
O2 La1 O4 72.2(2) . 2_655 ?
O2 La1 O8 73.8(2) . 3_665 ?
O2 La1 C00E 83.5(3) . . ?
C00E La1 Co1 88.40(7) . 2_655 ?
C00E La1 Co1 89.88(6) . . ?
La1 Co1 La1 73.62(3) . 3_665 ?
O1 Co1 La1 107.70(19) . 3_665 ?
O1 Co1 La1 43.06(18) . . ?
O1 Co1 O7 87.9(2) . . ?
O1 Co1 O3 122.7(3) . . ?
O1 Co1 N1 92.6(3) . . ?
O7 Co1 La1 42.94(15) . 3_665 ?
O7 Co1 La1 44.82(16) . . ?
O5 Co1 La1 113.8(2) . 3_665 ?
O5 Co1 La1 101.5(2) . . ?
O5 Co1 O1 110.1(3) . . ?
O5 Co1 O7 86.9(3) . . ?
O5 Co1 O3 126.0(3) . . ?
O5 Co1 N1 94.8(3) . . ?
O3 Co1 La1 109.06(19) . . ?
O3 Co1 La1 42.16(19) . 3_665 ?
O3 Co1 O7 85.0(2) . . ?
O3 Co1 N1 93.1(3) . . ?
N1 Co1 La1 135.1(2) . 3_665 ?
N1 Co1 La1 135.6(2) . . ?
N1 Co1 O7 178.0(3) . . ?
C00G O4 La1 119.6(6) . 3_665 ?
C00G O4 C010 117.2(8) . . ?
C010 O4 La1 122.9(6) . 3_665 ?
Co1 O1 La1 103.2(3) . . ?
C00F O1 La1 123.6(5) . . ?
C00F O1 Co1 122.0(5) . . ?
La1 O7 La1 117.4(3) 3_665 . ?
Co1 O7 La1 97.1(2) . . ?
Co1 O7 La1 100.3(2) . 3_665 ?
C00K O5 Co1 117.2(6) . . ?
Co1 O3 La1 104.9(3) . 3_665 ?
C00J O3 La1 127.2(5) . 3_665 ?
C00J O3 Co1 119.5(6) . . ?
La1 O8 La1 107.6(2) . 2_655 ?
C00E O8 La1 88.6(5) . 2_655 ?
C00E O8 La1 92.1(6) . . ?
C014 O6 C00Y 116.4(10) . . ?
C00N O2 La1 120.5(6) . . ?
C00N O2 C018 118.9(8) . . ?
C018 O2 La1 120.6(6) . . ?
La1 C00E La1 92.6(4) . 2_655 ?
La1 C00E La1 92.6(4) 2_655 3_665 ?
La1 C00E La1 92.6(4) . 3_665 ?
O8 C00E La1 61.8(5) . . ?
O8 C00E La1 143.6(11) 3_665 2_655 ?
O8 C00E La1 143.6(11) . 3_665 ?
O8 C00E La1 65.3(5) 3_665 . ?
O8 C00E La1 61.8(5) 2_655 2_655 ?
O8 C00E La1 143.6(11) 2_655 . ?
O8 C00E La1 61.8(5) 3_665 3_665 ?
O8 C00E La1 65.3(5) . 2_655 ?
O8 C00E La1 65.3(5) 2_655 3_665 ?
O8 C00E O8 119.73(16) 3_665 2_655 ?
O8 C00E O8 119.74(16) . 3_665 ?
O8 C00E O8 119.74(16) . 2_655 ?
O1 C00F C00N 118.7(9) . . ?
O1 C00F C00Q 122.0(8) . . ?
C00N C00F C00Q 119.4(9) . . ?
O4 C00G C00J 115.5(8) . . ?
O4 C00G C00L 125.8(9) . . ?
C00L C00G C00J 118.8(9) . . ?
C00N C00H H00H 119.1 . . ?
C00U C00H H00H 119.1 . . ?
C00U C00H C00N 121.7(10) . . ?
C00J C00I C00O 119.5(9) . . ?
C00J C00I C00Z 119.1(8) . . ?
C00O C00I C00Z 121.4(9) . . ?
O3 C00J C00G 116.8(8) . . ?
O3 C00J C00I 123.7(8) . . ?
C00I C00J C00G 119.5(8) . . ?
O5 C00K C00W 123.5(9) . . ?
O5 C00K C014 118.9(10) . . ?
C00W C00K C014 117.6(9) . . ?
C00G C00L H00L 119.5 . . ?
C00G C00L C00P 121.0(9) . . ?
C00P C00L H00L 119.5 . . ?
C00S N1 Co1 112.0(6) . . ?
C00S N1 C00X 109.0(7) . . ?
C00S N1 C00Z 108.8(8) . . ?
C00X N1 Co1 106.4(6) . . ?
C00Z N1 Co1 111.3(5) . . ?
C00Z N1 C00X 109.3(7) . . ?
O2 C00N C00F 114.6(9) . . ?
O2 C00N C00H 125.3(9) . . ?
C00H C00N C00F 120.1(10) . . ?
C00I C00O H00O 118.5 . . ?
C00P C00O C00I 123.0(9) . . ?
C00P C00O H00O 118.5 . . ?
C00L C00P C00T 119.4(10) . . ?
C00O C00P C00L 118.2(9) . . ?
C00O C00P C00T 122.4(10) . . ?
C00F C00Q C00R 119.2(9) . . ?
C00F C00Q C00S 119.5(9) . . ?
C00R C00Q C00S 121.1(9) . . ?
C00Q C00R H00R 119.2 . . ?
C00U C00R C00Q 121.6(10) . . ?
C00U C00R H00R 119.2 . . ?
N1 C00S C00Q 115.5(8) . . ?
N1 C00S H00A 108.4 . . ?
N1 C00S H00B 108.4 . . ?
C00Q C00S H00A 108.4 . . ?
C00Q C00S H00B 108.4 . . ?
H00A C00S H00B 107.5 . . ?
C00P C00T H00C 109.5 . . ?
C00P C00T H00D 109.5 . . ?
C00P C00T H00E 109.5 . . ?
H00C C00T H00D 109.5 . . ?
H00C C00T H00E 109.5 . . ?
H00D C00T H00E 109.5 . . ?
C00H C00U C016 121.9(11) . . ?
C00R C00U C00H 118.1(9) . . ?
C00R C00U C016 119.9(11) . . ?
C00W C00V H00V 119.4 . . ?
C00W C00V C015 121.2(12) . . ?
C015 C00V H00V 119.4 . . ?
C00K C00W C00V 122.0(10) . . ?
C00K C00W C00X 118.6(9) . . ?
C00V C00W C00X 119.4(10) . . ?
N1 C00X H00F 109.4 . . ?
N1 C00X H00G 109.4 . . ?
C00W C00X N1 111.1(8) . . ?
C00W C00X H00F 109.4 . . ?
C00W C00X H00G 109.4 . . ?
H00F C00X H00G 108.0 . . ?
O6 C00Y H00I 109.5 . . ?
O6 C00Y H00J 109.5 . . ?
O6 C00Y H00K 109.5 . . ?
H00I C00Y H00J 109.5 . . ?
H00I C00Y H00K 109.5 . . ?
H00J C00Y H00K 109.5 . . ?
C00I C00Z H00M 108.7 . . ?
C00I C00Z H00N 108.7 . . ?
N1 C00Z C00I 114.2(8) . . ?
N1 C00Z H00M 108.7 . . ?
N1 C00Z H00N 108.7 . . ?
H00M C00Z H00N 107.6 . . ?
O4 C010 H01A 109.5 . . ?
O4 C010 H01B 109.5 . . ?
O4 C010 H01C 109.5 . . ?
H01A C010 H01B 109.5 . . ?
H01A C010 H01C 109.5 . . ?
H01B C010 H01C 109.5 . . ?
C014 C012 H012 119.5 . . ?
C015 C012 H012 119.5 . . ?
C015 C012 C014 121.0(12) . . ?
H01D C013 H01E 109.5 . . ?
H01D C013 H01F 109.5 . . ?
H01E C013 H01F 109.5 . . ?
C015 C013 H01D 109.5 . . ?
C015 C013 H01E 109.5 . . ?
C015 C013 H01F 109.5 . . ?
O6 C014 C00K 115.5(9) . . ?
O6 C014 C012 123.9(11) . . ?
C012 C014 C00K 120.4(11) . . ?
C00V C015 C013 120.9(13) . . ?
C012 C015 C00V 117.7(11) . . ?
C012 C015 C013 121.3(12) . . ?
C00U C016 H01G 109.5 . . ?
C00U C016 H01H 109.5 . . ?
C00U C016 H01I 109.5 . . ?
H01G C016 H01H 109.5 . . ?
H01G C016 H01I 109.5 . . ?
H01H C016 H01I 109.5 . . ?
O2 C018 H01J 109.5 . . ?
O2 C018 H01K 109.5 . . ?
O2 C018 H01L 109.5 . . ?
H01J C018 H01K 109.5 . . ?
H01J C018 H01L 109.5 . . ?
H01K C018 H01L 109.5 . . ?
O10 Cl1 O10 108.8(10) 2 . ?
O10 Cl1 O10 108.8(10) 3 2 ?
O10 Cl1 O10 108.8(10) 3 . ?
O10 Cl1 O11 110.2(10) 3 . ?
O10 Cl1 O11 110.2(10) . . ?
O10 Cl1 O11 110.2(10) 2 . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_Compound_5
_database_code_depnum_ccdc_archive 'CCDC 1579345'
_audit_update_record             
;
2018-01-04 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;
_audit_creation_date             2018-01-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C82 H90 Co3 Ho3 N3 O27, Cl1 O4'
_chemical_formula_sum            'C82 H90 Cl Co3 Ho3 N3 O31'
_chemical_formula_weight         2320.59
_chemical_absolute_configuration ?
_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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   18.1503(18)
_cell_length_b                   18.1503(18)
_cell_length_c                   53.697(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     15320(3)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    8891
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.28
_cell_measurement_theta_min      2.24
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.870
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1532 before and 0.0587 after correction. The Ratio of minimum to maximum transmission is 0.8413. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   SADABS
_exptl_crystal_colour            magenta
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6900
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            52018
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.633
_diffrn_reflns_theta_min         1.501
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.956
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                5837
_reflns_number_total             7754
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.730
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details 
;
 Flack x determined using 2387 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_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     376
_refine_ls_number_reflns         7754
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0518
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0770P)²+152.7420P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1453
_refine_special_details          SQUEEZE
_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.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C9(H9A,H9B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C7(H7), C4(H4), C16(H16), C25(H25), C22(H22)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C),
 C21(H21A,H21B,H21C), C24(H24A,H24B,H24C)
;
_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
Ho1 Ho 0.41101(3) 0.59741(3) 0.50306(2) 0.02773(17) Uani 1 1 d . . . . .
Co1 Co 0.57576(11) 0.79737(10) 0.49181(3) 0.0249(4) Uani 1 1 d . . . . .
O3 O 0.3290(5) 0.4532(5) 0.50912(15) 0.0253(18) Uani 1 1 d . . . . .
N1 N 0.7046(7) 0.8654(6) 0.5031(2) 0.027(2) Uani 1 1 d . . . . .
O5 O 0.5986(6) 0.8294(6) 0.45673(16) 0.033(2) Uani 1 1 d . . . . .
O9 O 0.4265(5) 0.5714(6) 0.45963(17) 0.033(2) Uani 1 1 d . . . . .
O4 O 0.4336(6) 0.5507(6) 0.54346(17) 0.036(2) Uani 1 1 d . . . . .
C27 C 0.7591(9) 0.8806(8) 0.4799(3) 0.036(3) Uani 1 1 d . . . . .
H27A H 0.819877 0.909256 0.484674 0.043 Uiso 1 1 calc R . . . .
H27B H 0.744075 0.825362 0.472132 0.043 Uiso 1 1 calc R . . . .
C9 C 0.7233(8) 0.8173(8) 0.5221(2) 0.030(3) Uani 1 1 d . . . . .
H9A H 0.690497 0.811859 0.537423 0.036 Uiso 1 1 calc R . . . .
H9B H 0.784531 0.849978 0.526431 0.036 Uiso 1 1 calc R . . . .
O2 O 0.5132(5) 0.5336(6) 0.49725(18) 0.033(2) Uani 1 1 d . . . . .
O8 O 0.2906(6) 0.5832(7) 0.5310(2) 0.047(3) Uani 1 1 d . . . . .
O7 O 0.2810(5) 0.5569(6) 0.48367(17) 0.0290(19) Uani 1 1 d . . . . .
Cl1 Cl 0.000000 0.000000 0.5194(2) 0.066(2) Uani 1 3 d S T P . .
C11 C 0.3867(8) 0.4663(9) 0.5489(2) 0.035(3) Uani 1 1 d . . . . .
C19 C 0.6653(9) 0.9062(8) 0.4517(2) 0.035(3) Uani 1 1 d . . . . .
C14 C 0.3404(9) 0.3435(10) 0.5756(3) 0.041(3) Uani 1 1 d . . . . .
C17 C 0.2780(8) 0.3270(9) 0.5342(3) 0.034(3) Uani 1 1 d . . . . .
C26 C 0.7451(9) 0.9344(9) 0.4617(3) 0.038(3) Uani 1 1 d . . . . .
C13 C 0.3912(9) 0.4294(10) 0.5717(2) 0.037(3) Uani 1 1 d . . . . .
H13 H 0.429459 0.464168 0.584327 0.045 Uiso 1 1 calc R . . . .
C10 C 0.3301(8) 0.4145(8) 0.5301(2) 0.028(3) Uani 1 1 d . . . . .
O1 O 0.5562(5) 0.6894(5) 0.50708(16) 0.0259(18) Uani 1 1 d . . . . .
C8 C 0.7014(8) 0.7282(8) 0.5133(2) 0.031(3) Uani 1 1 d . . . . .
C7 C 0.7654(8) 0.7066(8) 0.5112(2) 0.033(3) Uani 1 1 d . . . . .
H7 H 0.822952 0.747736 0.514654 0.040 Uiso 1 1 calc R . . . .
C18 C 0.7286(8) 0.9528(8) 0.5138(3) 0.033(3) Uani 1 1 d . . . . .
H18A H 0.787748 0.979830 0.520084 0.040 Uiso 1 1 calc R . . . .
H18B H 0.727288 0.988868 0.500198 0.040 Uiso 1 1 calc R . . . .
C2 C 0.5990(8) 0.5865(8) 0.5012(2) 0.030(3) Uani 1 1 d . . . . .
C4 C 0.6615(9) 0.5660(9) 0.4998(3) 0.040(4) Uani 1 1 d . . . . .
H4 H 0.647850 0.509627 0.495776 0.048 Uiso 1 1 calc R . . . .
C28 C 0.333333 0.666667 0.5331(7) 0.055(8) Uani 1 3 d S T P . .
O11 O 0.000000 0.000000 0.4914(9) 0.18(2) Uani 1 3 d S T P . .
C16 C 0.2839(9) 0.2921(10) 0.5571(3) 0.039(3) Uani 1 1 d . . . . .
H16 H 0.248921 0.232734 0.559918 0.046 Uiso 1 1 calc R . . . .
C25 C 0.8131(11) 1.0165(10) 0.4558(3) 0.053(4) Uani 1 1 d . . . . .
H25 H 0.867738 1.034933 0.462744 0.064 Uiso 1 1 calc R . . . .
C22 C 0.7218(12) 1.0435(9) 0.4306(3) 0.055(5) Uani 1 1 d . . . . .
H22 H 0.713782 1.081567 0.420336 0.066 Uiso 1 1 calc R . . . .
C15 C 0.3440(12) 0.3036(12) 0.6003(3) 0.058(5) Uani 1 1 d . . . . .
H15A H 0.403090 0.319779 0.603972 0.087 Uiso 1 1 calc GR . . . .
H15B H 0.309415 0.241552 0.599102 0.087 Uiso 1 1 calc GR . . . .
H15C H 0.321872 0.323993 0.613639 0.087 Uiso 1 1 calc GR . . . .
C20 C 0.6513(11) 0.9611(9) 0.4357(3) 0.045(4) Uani 1 1 d . . . . .
C23 C 0.8018(12) 1.0692(10) 0.4404(3) 0.051(4) Uani 1 1 d . . . . .
C6 C 0.8151(9) 0.6016(11) 0.5028(4) 0.046(4) Uani 1 1 d . . . . .
H6A H 0.852677 0.630384 0.488666 0.069 Uiso 1 1 calc GR . . . .
H6B H 0.788246 0.539860 0.500668 0.069 Uiso 1 1 calc GR . . . .
H6C H 0.848531 0.618389 0.518255 0.069 Uiso 1 1 calc GR . . . .
C1 C 0.6186(8) 0.6697(8) 0.5075(2) 0.027(3) Uani 1 1 d . . . . .
C3 C 0.4880(9) 0.4515(8) 0.4863(3) 0.036(3) Uani 1 1 d . . . . .
H3A H 0.517419 0.459466 0.470378 0.055 Uiso 1 1 calc GR . . . .
H3B H 0.426376 0.420546 0.483531 0.055 Uiso 1 1 calc GR . . . .
H3C H 0.503162 0.418741 0.497615 0.055 Uiso 1 1 calc GR . . . .
C5 C 0.7447(9) 0.6274(9) 0.5043(3) 0.038(3) Uani 1 1 d . . . . .
O6 O 0.5722(7) 0.9309(7) 0.42749(19) 0.046(3) Uani 1 1 d . . . . .
O13 O 0.0832(10) 0.0446(9) 0.5288(4) 0.115(8) Uani 1 1 d . . . . .
C12 C 0.4943(12) 0.6057(10) 0.5617(3) 0.065(6) Uani 1 1 d . . . . .
H12A H 0.464056 0.609030 0.576412 0.097 Uiso 1 1 calc GR . . . .
H12B H 0.529055 0.662681 0.554616 0.097 Uiso 1 1 calc GR . . . .
H12C H 0.531035 0.582884 0.566541 0.097 Uiso 1 1 calc GR . . . .
C21 C 0.5596(15) 0.9783(15) 0.4087(4) 0.087(7) Uani 1 1 d . . . . .
H21A H 0.570727 1.032941 0.415577 0.131 Uiso 1 1 calc GR . . . .
H21B H 0.500776 0.946392 0.402730 0.131 Uiso 1 1 calc GR . . . .
H21C H 0.598628 0.988341 0.394844 0.131 Uiso 1 1 calc GR . . . .
C24 C 0.8782(16) 1.1545(12) 0.4335(4) 0.086(7) Uani 1 1 d . . . . .
H24A H 0.905887 1.147678 0.418715 0.129 Uiso 1 1 calc GR . . . .
H24B H 0.918701 1.175290 0.447399 0.129 Uiso 1 1 calc GR . . . .
H24C H 0.859431 1.195482 0.429977 0.129 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
Ho1 Co1 3.4098(19) . ?
Ho1 Co1 3.3552(18) 3_565 ?
Ho1 O3 2.297(8) . ?
Ho1 O9 2.423(9) . ?
Ho1 O4 2.438(9) . ?
Ho1 O2 2.650(9) . ?
Ho1 O8 2.457(10) 2_665 ?
Ho1 O8 2.555(10) . ?
Ho1 O7 2.336(8) . ?
Ho1 O7 2.317(8) 2_665 ?
Ho1 O1 2.319(8) . ?
Ho1 C28 2.82(2) . ?
Co1 O3 1.979(8) 2_665 ?
Co1 N1 2.114(11) . ?
Co1 O5 1.954(8) . ?
Co1 O7 2.135(10) 2_665 ?
Co1 O1 1.986(9) . ?
O3 C10 1.332(14) . ?
N1 C27 1.526(16) . ?
N1 C9 1.491(16) . ?
N1 C18 1.531(15) . ?
O5 C19 1.338(15) . ?
O4 C11 1.360(17) . ?
O4 C12 1.439(17) . ?
C27 C26 1.49(2) . ?
C9 C8 1.535(18) . ?
O2 C2 1.378(15) . ?
O2 C3 1.448(16) . ?
O8 C28 1.317(12) . ?
Cl1 O11 1.50(5) . ?
Cl1 O13 1.401(17) 2 ?
Cl1 O13 1.402(17) . ?
Cl1 O13 1.402(17) 3 ?
C11 C13 1.419(18) . ?
C11 C10 1.411(19) . ?
C19 C26 1.38(2) . ?
C19 C20 1.43(2) . ?
C14 C13 1.37(2) . ?
C14 C16 1.40(2) . ?
C14 C15 1.528(19) . ?
C17 C10 1.401(18) . ?
C17 C18 1.477(19) 3_565 ?
C17 C16 1.411(18) . ?
C26 C25 1.42(2) . ?
O1 C1 1.349(15) . ?
C8 C7 1.405(18) . ?
C8 C1 1.372(18) . ?
C7 C5 1.343(19) . ?
C2 C4 1.361(18) . ?
C2 C1 1.408(18) . ?
C4 C5 1.38(2) . ?
C25 C23 1.35(2) . ?
C22 C20 1.43(2) . ?
C22 C23 1.39(3) . ?
C20 O6 1.33(2) . ?
C23 C24 1.52(2) . ?
C6 C5 1.569(17) . ?
O6 C21 1.42(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Co1 Ho1 Co1 155.19(6) 3_565 . ?
O3 Ho1 Co1 35.1(2) . 3_565 ?
O3 Ho1 Co1 164.1(2) . . ?
O3 Ho1 O9 89.2(3) . . ?
O3 Ho1 O4 66.6(3) . . ?
O3 Ho1 O2 73.4(3) . . ?
O3 Ho1 O8 125.4(3) . 2_665 ?
O3 Ho1 O8 76.6(3) . . ?
O3 Ho1 O7 74.2(3) . . ?
O3 Ho1 O7 153.2(3) . 2_665 ?
O3 Ho1 O1 131.5(3) . . ?
O3 Ho1 C28 104.1(3) . . ?
O9 Ho1 Co1 84.9(2) . . ?
O9 Ho1 Co1 78.97(19) . 3_565 ?
O9 Ho1 O4 137.1(4) . . ?
O9 Ho1 O2 68.1(3) . . ?
O9 Ho1 O8 141.6(3) . 2_665 ?
O9 Ho1 O8 136.2(3) . . ?
O9 Ho1 C28 140.4(7) . . ?
O4 Ho1 Co1 108.5(2) . . ?
O4 Ho1 Co1 96.1(2) . 3_565 ?
O4 Ho1 O2 71.1(3) . . ?
O4 Ho1 O8 78.1(3) . 2_665 ?
O4 Ho1 O8 74.1(3) . . ?
O4 Ho1 C28 81.7(7) . . ?
O2 Ho1 Co1 90.7(2) . . ?
O2 Ho1 Co1 100.5(2) . 3_565 ?
O2 Ho1 C28 151.4(6) . . ?
O8 Ho1 Co1 65.6(3) . 3_565 ?
O8 Ho1 Co1 117.5(3) . . ?
O8 Ho1 Co1 65.5(3) 2_665 . ?
O8 Ho1 Co1 118.6(3) 2_665 3_565 ?
O8 Ho1 O2 132.2(3) 2_665 . ?
O8 Ho1 O2 140.8(3) . . ?
O8 Ho1 O8 53.9(5) 2_665 . ?
O8 Ho1 C28 27.9(3) 2_665 . ?
O8 Ho1 C28 27.8(3) . . ?
O7 Ho1 Co1 118.7(2) 2_665 3_565 ?
O7 Ho1 Co1 38.1(2) 2_665 . ?
O7 Ho1 Co1 117.8(2) . . ?
O7 Ho1 Co1 39.1(2) . 3_565 ?
O7 Ho1 O9 73.0(3) . . ?
O7 Ho1 O9 76.4(3) 2_665 . ?
O7 Ho1 O4 127.3(3) . . ?
O7 Ho1 O4 138.0(3) 2_665 . ?
O7 Ho1 O2 119.8(3) 2_665 . ?
O7 Ho1 O2 128.9(3) . . ?
O7 Ho1 O8 65.2(3) 2_665 2_665 ?
O7 Ho1 O8 63.3(3) . . ?
O7 Ho1 O8 98.8(3) . 2_665 ?
O7 Ho1 O8 98.1(3) 2_665 . ?
O7 Ho1 O7 79.9(5) 2_665 . ?
O7 Ho1 O1 72.3(3) 2_665 . ?
O7 Ho1 C28 75.1(5) . . ?
O7 Ho1 C28 75.4(5) 2_665 . ?
O1 Ho1 Co1 162.6(2) . 3_565 ?
O1 Ho1 Co1 34.3(2) . . ?
O1 Ho1 O9 91.7(3) . . ?
O1 Ho1 O4 80.8(3) . . ?
O1 Ho1 O2 62.2(3) . . ?
O1 Ho1 O8 77.7(4) . 2_665 ?
O1 Ho1 O8 128.7(3) . . ?
O1 Ho1 O7 150.8(3) . . ?
O1 Ho1 C28 105.5(3) . . ?
C28 Ho1 Co1 90.81(14) . 3_565 ?
C28 Ho1 Co1 89.69(14) . . ?
Ho1 Co1 Ho1 72.55(4) 2_665 . ?
O3 Co1 Ho1 106.0(3) 2_665 . ?
O3 Co1 Ho1 41.8(2) 2_665 2_665 ?
O3 Co1 N1 93.4(4) 2_665 . ?
O3 Co1 O7 85.5(3) 2_665 2_665 ?
O3 Co1 O1 122.4(4) 2_665 . ?
N1 Co1 Ho1 135.1(3) . 2_665 ?
N1 Co1 Ho1 134.1(3) . . ?
N1 Co1 O7 174.9(4) . 2_665 ?
O5 Co1 Ho1 115.5(3) . . ?
O5 Co1 Ho1 102.5(3) . 2_665 ?
O5 Co1 O3 109.4(4) . 2_665 ?
O5 Co1 N1 95.4(4) . . ?
O5 Co1 O7 89.6(4) . 2_665 ?
O5 Co1 O1 126.8(4) . . ?
O7 Co1 Ho1 42.0(2) 2_665 . ?
O7 Co1 Ho1 43.7(2) 2_665 2_665 ?
O1 Co1 Ho1 41.2(2) . . ?
O1 Co1 Ho1 107.4(2) . 2_665 ?
O1 Co1 N1 93.3(4) . . ?
O1 Co1 O7 83.1(3) . 2_665 ?
Co1 O3 Ho1 103.1(4) 3_565 . ?
C10 O3 Ho1 123.3(8) . . ?
C10 O3 Co1 121.9(7) . 3_565 ?
C27 N1 Co1 107.4(8) . . ?
C27 N1 C18 107.3(10) . . ?
C9 N1 Co1 111.3(7) . . ?
C9 N1 C27 110.4(10) . . ?
C9 N1 C18 108.5(10) . . ?
C18 N1 Co1 111.8(7) . . ?
C19 O5 Co1 116.7(8) . . ?
C11 O4 Ho1 117.5(7) . . ?
C11 O4 C12 117.9(11) . . ?
C12 O4 Ho1 124.6(9) . . ?
C26 C27 N1 110.3(10) . . ?
N1 C9 C8 112.9(11) . . ?
C2 O2 Ho1 118.2(7) . . ?
C2 O2 C3 116.4(10) . . ?
C3 O2 Ho1 124.6(7) . . ?
Ho1 O8 Ho1 106.0(4) 3_565 . ?
C28 O8 Ho1 91.4(11) . 3_565 ?
C28 O8 Ho1 87.2(11) . . ?
Ho1 O7 Ho1 118.7(4) 3_565 . ?
Co1 O7 Ho1 99.9(4) 3_565 3_565 ?
Co1 O7 Ho1 97.1(3) 3_565 . ?
O13 Cl1 O11 111.0(11) . . ?
O13 Cl1 O11 111.0(11) 3 . ?
O13 Cl1 O11 111.0(11) 2 . ?
O13 Cl1 O13 107.9(12) 2 3 ?
O13 Cl1 O13 107.9(12) . 3 ?
O13 Cl1 O13 107.9(12) 2 . ?
O4 C11 C13 124.4(13) . . ?
O4 C11 C10 115.8(11) . . ?
C10 C11 C13 119.9(13) . . ?
O5 C19 C26 123.0(13) . . ?
O5 C19 C20 117.5(13) . . ?
C26 C19 C20 119.5(13) . . ?
C13 C14 C16 120.1(12) . . ?
C13 C14 C15 120.4(15) . . ?
C16 C14 C15 119.5(15) . . ?
C10 C17 C18 120.0(12) . 3_565 ?
C10 C17 C16 119.1(13) . . ?
C16 C17 C18 120.7(13) . 3_565 ?
C19 C26 C27 120.1(12) . . ?
C19 C26 C25 120.4(15) . . ?
C25 C26 C27 119.5(14) . . ?
C14 C13 C11 120.2(13) . . ?
O3 C10 C11 116.8(12) . . ?
O3 C10 C17 123.4(12) . . ?
C17 C10 C11 119.8(12) . . ?
Co1 O1 Ho1 104.5(4) . . ?
C1 O1 Ho1 127.9(8) . . ?
C1 O1 Co1 120.7(7) . . ?
C7 C8 C9 120.2(11) . . ?
C1 C8 C9 119.5(11) . . ?
C1 C8 C7 120.3(13) . . ?
C5 C7 C8 119.5(13) . . ?
C17 C18 N1 114.8(11) 2_665 . ?
O2 C2 C1 112.1(11) . . ?
C4 C2 O2 127.4(12) . . ?
C4 C2 C1 120.5(12) . . ?
C2 C4 C5 119.7(13) . . ?
Ho1 C28 Ho1 90.5(9) 2_665 3_565 ?
Ho1 C28 Ho1 90.5(9) 2_665 . ?
Ho1 C28 Ho1 90.5(9) 3_565 . ?
O8 C28 Ho1 140(2) 3_565 . ?
O8 C28 Ho1 140(2) 2_665 3_565 ?
O8 C28 Ho1 64.9(9) 2_665 2_665 ?
O8 C28 Ho1 60.7(9) 2_665 . ?
O8 C28 Ho1 64.9(9) . . ?
O8 C28 Ho1 140(2) . 2_665 ?
O8 C28 Ho1 60.7(9) 3_565 2_665 ?
O8 C28 Ho1 64.9(10) 3_565 3_565 ?
O8 C28 Ho1 60.7(9) . 3_565 ?
O8 C28 O8 119.3(5) 2_665 . ?
O8 C28 O8 119.3(5) 3_565 . ?
O8 C28 O8 119.3(5) 3_565 2_665 ?
C14 C16 C17 121.0(14) . . ?
C23 C25 C26 121.3(17) . . ?
C23 C22 C20 121.2(16) . . ?
C22 C20 C19 117.8(16) . . ?
O6 C20 C19 116.3(13) . . ?
O6 C20 C22 125.8(15) . . ?
C25 C23 C22 119.7(15) . . ?
C25 C23 C24 119.0(18) . . ?
C22 C23 C24 121.2(16) . . ?
O1 C1 C8 122.5(12) . . ?
O1 C1 C2 118.9(11) . . ?
C8 C1 C2 118.5(12) . . ?
C7 C5 C4 121.4(13) . . ?
C7 C5 C6 120.0(13) . . ?
C4 C5 C6 118.4(14) . . ?
C20 O6 C21 117.0(14) . . ?

_olex2_submission_special_instructions 'No special instructions were received'

#
_vrf_PLAT342_Compound_5          
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02121 Ang.
RESPONSE: This is due to nonavailability of enough high precision data.
;
# end Validation Reply Form
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_Compound_4
_database_code_depnum_ccdc_archive 'CCDC 1579344'
_audit_update_record             
;
2018-01-04 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;
_audit_creation_date             2018-01-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1(C82 H90 Co3 Dy3 N3 O27), 1(Cl1 O4)'
_chemical_formula_sum            'C82 H90 Cl Co3 Dy3 N3 O31'
_chemical_formula_weight         2313.33
_chemical_absolute_configuration ?
_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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   18.149(2)
_cell_length_b                   18.149(2)
_cell_length_c                   53.851(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     15362(5)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    6792
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.92
_cell_measurement_theta_min      2.24
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.733
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.4917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1246 before and 0.0774 after correction.
The Ratio of minimum to maximum transmission is 0.6600.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   SADABS
_exptl_crystal_colour            magenta
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6882
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            53588
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.178
_diffrn_reflns_theta_max         24.178
_diffrn_reflns_theta_min         1.500
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                3971
_reflns_number_total             5403
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 
;
 Flack x determined using 1700 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5403
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0434
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0642P)²+86.9916P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1241
_refine_special_details          SQUEEZE
_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. Rigid bond restraints
 C23, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C9(H9A,H9B), C28(H28A,H28B)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C16(H16), C4(H4), C7(H7), C26(H26), C23(H23)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C12(H12A,H12B,H12C), C3(H3A,H3B,H3C), C25(H25A,H25B,
 H25C), C6(H6A,H6B,H6C), C22(H22A,H22B,H22C)
;
_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 0.25574(4) 0.51967(5) 0.44125(2) 0.0419(2) Uani 1 1 d . . . . .
Co1 Co 0.44414(13) 0.53570(13) 0.45259(4) 0.0427(5) Uani 1 1 d . . . . .
O7 O 0.3857(6) 0.6093(6) 0.4609(2) 0.042(3) Uani 1 1 d . . . . .
C29 C 0.333333 0.666667 0.4125(5) 0.047(7) Uani 1 3 d S T P . .
O1 O 0.1111(7) 0.4678(7) 0.4375(2) 0.049(3) Uani 1 1 d . . . . .
O9 O 0.2407(7) 0.4783(8) 0.4849(2) 0.058(3) Uani 1 1 d . . . . .
O2 O 0.1537(7) 0.3553(7) 0.4466(2) 0.058(3) Uani 1 1 d . . . . .
O8 O 0.2536(7) 0.6252(7) 0.41354(19) 0.050(3) Uani 1 1 d . . . . .
C15 C -0.1452(13) 0.1229(14) 0.4409(6) 0.093(7) Uani 1 1 d . . . . .
H15A H -0.181527 0.114169 0.454886 0.139 Uiso 1 1 calc GR . . . .
H15B H -0.117710 0.089790 0.443028 0.139 Uiso 1 1 calc GR . . . .
H15C H -0.178542 0.105523 0.425990 0.139 Uiso 1 1 calc GR . . . .
C11 C 0.0691(11) 0.3238(10) 0.4425(3) 0.054(5) Uani 1 1 d . . . . .
C20 C -0.0341(11) 0.3629(11) 0.4314(3) 0.056(5) Uani 1 1 d . . . . .
C18 C -0.0555(10) 0.4284(10) 0.4225(3) 0.049(4) Uani 1 1 d . . . . .
H18A H -0.022971 0.455329 0.407611 0.059 Uiso 1 1 calc R . . . .
H18B H -0.115398 0.400462 0.418188 0.059 Uiso 1 1 calc R . . . .
C13 C 0.0073(11) 0.2398(11) 0.4437(4) 0.064(5) Uani 1 1 d . . . . .
H13 H 0.020631 0.197793 0.447427 0.077 Uiso 1 1 calc R . . . .
C16 C -0.0960(11) 0.2775(11) 0.4324(3) 0.055(5) Uani 1 1 d . . . . .
H16 H -0.151935 0.260921 0.428344 0.066 Uiso 1 1 calc R . . . .
C14 C -0.0762(12) 0.2195(11) 0.4391(4) 0.066(6) Uani 1 1 d . . . . .
C12 C 0.1783(12) 0.2953(12) 0.4560(4) 0.073(6) Uani 1 1 d . . . . .
H12A H 0.150470 0.272517 0.471568 0.110 Uiso 1 1 calc GR . . . .
H12B H 0.238811 0.324047 0.458284 0.110 Uiso 1 1 calc GR . . . .
H12C H 0.161707 0.249860 0.444257 0.110 Uiso 1 1 calc GR . . . .
C9 C 0.4408(11) 0.3817(10) 0.4308(3) 0.053(4) Uani 1 1 d . . . . .
H9A H 0.471091 0.353704 0.424854 0.063 Uiso 1 1 calc R . . . .
H9B H 0.402972 0.346938 0.443962 0.063 Uiso 1 1 calc R . . . .
C2 C 0.2823(10) 0.4140(10) 0.3955(3) 0.046(4) Uani 1 1 d . . . . .
C1 C 0.3361(10) 0.4193(10) 0.4140(3) 0.043(4) Uani 1 1 d . . . . .
C4 C 0.2800(12) 0.3735(10) 0.3737(3) 0.057(5) Uani 1 1 d . . . . .
H4 H 0.242181 0.369376 0.361375 0.069 Uiso 1 1 calc R . . . .
C8 C 0.3892(11) 0.3856(10) 0.4103(4) 0.056(5) Uani 1 1 d . . . . .
C7 C 0.3837(12) 0.3436(10) 0.3878(3) 0.057(5) Uani 1 1 d . . . . .
H7 H 0.416696 0.318184 0.385403 0.068 Uiso 1 1 calc R . . . .
C3 C 0.1803(15) 0.4513(16) 0.3810(4) 0.093(8) Uani 1 1 d . . . . .
H3A H 0.189983 0.428188 0.366179 0.140 Uiso 1 1 calc GR . . . .
H3B H 0.193245 0.508674 0.378022 0.140 Uiso 1 1 calc GR . . . .
H3C H 0.121786 0.417421 0.385912 0.140 Uiso 1 1 calc GR . . . .
C5 C 0.3295(13) 0.3400(12) 0.3694(4) 0.068(5) Uani 1 1 d . . . . .
O3 O 0.3378(6) 0.4581(6) 0.4349(2) 0.042(3) Uani 1 1 d . . . . .
C28 C 0.5421(10) 0.4526(10) 0.4645(4) 0.056(4) Uani 1 1 d . . . . .
H28A H 0.573571 0.424399 0.459896 0.067 Uiso 1 1 calc R . . . .
H28B H 0.581793 0.506739 0.471992 0.067 Uiso 1 1 calc R . . . .
C19 C 0.4253(12) 0.4280(11) 0.4924(3) 0.056(4) Uani 1 1 d . . . . .
C26 C 0.4649(15) 0.3199(14) 0.4886(3) 0.077(6) Uani 1 1 d . . . . .
H26 H 0.500142 0.301716 0.481788 0.092 Uiso 1 1 calc R . . . .
C27 C 0.4795(12) 0.4021(11) 0.4822(4) 0.060(5) Uani 1 1 d . . . . .
O4 O 0.2348(7) 0.4507(8) 0.40084(19) 0.051(3) Uani 1 1 d . . . . .
O5 O 0.4332(8) 0.5016(8) 0.4870(2) 0.057(3) Uani 1 1 d . . . . .
N1 N 0.5053(8) 0.4683(8) 0.4415(3) 0.047(3) Uani 1 1 d . . . . .
C10 C 0.0495(10) 0.3855(10) 0.4369(3) 0.044(4) Uani 1 1 d . . . . .
C21 C 0.3609(15) 0.3743(12) 0.5082(4) 0.073(6) Uani 1 1 d . . . . .
C23 C 0.3474(15) 0.2904(13) 0.5134(4) 0.085(6) Uani 1 1 d . U . . .
H23 H 0.301054 0.252882 0.523023 0.102 Uiso 1 1 calc R . . . .
C25 C 0.395(3) 0.1813(15) 0.5100(7) 0.161(15) Uani 1 1 d . . . . .
H25A H 0.337573 0.139948 0.514028 0.241 Uiso 1 1 calc GR . . . .
H25B H 0.431568 0.187621 0.523762 0.241 Uiso 1 1 calc GR . . . .
H25C H 0.412973 0.162689 0.495651 0.241 Uiso 1 1 calc GR . . . .
C24 C 0.4012(16) 0.2658(14) 0.5045(4) 0.087(7) Uani 1 1 d . U . . .
O6 O 0.3083(9) 0.4008(9) 0.5166(3) 0.078(4) Uani 1 1 d . . . . .
C6 C 0.3227(15) 0.2930(14) 0.3454(4) 0.091(7) Uani 1 1 d . . . . .
H6A H 0.313576 0.321738 0.331759 0.137 Uiso 1 1 calc GR . . . .
H6B H 0.275772 0.235828 0.346446 0.137 Uiso 1 1 calc GR . . . .
H6C H 0.374374 0.291837 0.342692 0.137 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.666667 0.333333 0.4226(4) 0.141(6) Uani 1 3 d S T P . .
C22 C 0.255(2) 0.360(2) 0.5354(6) 0.172(15) Uani 1 1 d . . . . .
H22A H 0.203021 0.361210 0.533007 0.257 Uiso 1 1 calc GR . . . .
H22B H 0.280566 0.386997 0.550784 0.257 Uiso 1 1 calc GR . . . .
H22C H 0.242201 0.301778 0.535726 0.257 Uiso 1 1 calc GR . . . .
O10 O 0.666667 0.333333 0.4574(17) 0.36(6) Uani 1 3 d S T P . .
O11 O 0.589(2) 0.2980(17) 0.4141(8) 0.249(19) 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 Co1 3.340(2) . ?
Dy1 Co1 3.412(2) 3_565 ?
Dy1 O7 2.343(10) . ?
Dy1 O7 2.325(10) 3_565 ?
Dy1 C29 2.783(16) . ?
Dy1 O1 2.313(10) . ?
Dy1 O9 2.440(11) . ?
Dy1 O2 2.625(11) . ?
Dy1 O8 2.555(10) 2_665 ?
Dy1 O8 2.444(10) . ?
Dy1 O3 2.290(10) . ?
Dy1 O4 2.444(10) . ?
Co1 O7 2.128(12) . ?
Co1 O1 1.975(11) 2_665 ?
Co1 O3 1.974(10) . ?
Co1 O5 1.933(11) . ?
Co1 N1 2.107(13) . ?
C29 O8 1.255(12) 2_665 ?
C29 O8 1.255(12) 3_565 ?
C29 O8 1.255(12) . ?
O1 C10 1.346(18) . ?
O2 C11 1.36(2) . ?
O2 C12 1.46(2) . ?
C15 C14 1.57(2) . ?
C11 C13 1.37(2) . ?
C11 C10 1.37(2) . ?
C20 C18 1.50(2) . ?
C20 C16 1.39(2) . ?
C20 C10 1.39(2) . ?
C18 N1 1.49(2) 3_565 ?
C13 C14 1.39(3) . ?
C16 C14 1.32(2) . ?
C9 C8 1.47(2) . ?
C9 N1 1.529(19) . ?
C2 C1 1.36(2) . ?
C2 C4 1.37(2) . ?
C2 O4 1.357(19) . ?
C1 C8 1.39(2) . ?
C1 O3 1.322(19) . ?
C4 C5 1.33(3) . ?
C8 C7 1.41(2) . ?
C7 C5 1.37(3) . ?
C3 O4 1.46(2) . ?
C5 C6 1.52(3) . ?
C28 C27 1.41(2) . ?
C28 N1 1.50(2) . ?
C19 C27 1.40(3) . ?
C19 O5 1.305(19) . ?
C19 C21 1.38(3) . ?
C26 C27 1.42(3) . ?
C26 C24 1.38(3) . ?
C21 C23 1.44(3) . ?
C21 O6 1.35(2) . ?
C23 C24 1.35(3) . ?
C25 C24 1.51(3) . ?
O6 C22 1.34(3) . ?
Cl1 O10 1.87(9) . ?
Cl1 O11 1.31(3) . ?
Cl1 O11 1.31(3) 2_655 ?
Cl1 O11 1.31(3) 3_665 ?

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
Co1 Dy1 Co1 154.85(8) . 3_565 ?
O7 Dy1 Co1 37.9(3) 3_565 3_565 ?
O7 Dy1 Co1 118.5(3) 3_565 . ?
O7 Dy1 Co1 39.3(3) . . ?
O7 Dy1 Co1 117.3(3) . 3_565 ?
O7 Dy1 O7 79.6(6) 3_565 . ?
O7 Dy1 C29 74.6(5) . . ?
O7 Dy1 C29 74.8(5) 3_565 . ?
O7 Dy1 O9 72.4(4) . . ?
O7 Dy1 O9 76.0(4) 3_565 . ?
O7 Dy1 O2 129.3(4) . . ?
O7 Dy1 O2 119.7(4) 3_565 . ?
O7 Dy1 O8 97.8(4) . . ?
O7 Dy1 O8 63.8(3) . 2_665 ?
O7 Dy1 O8 97.0(4) 3_565 2_665 ?
O7 Dy1 O8 65.8(3) 3_565 . ?
O7 Dy1 O4 138.7(4) 3_565 . ?
O7 Dy1 O4 127.0(4) . . ?
C29 Dy1 Co1 89.26(11) . 3_565 ?
C29 Dy1 Co1 90.74(11) . . ?
O1 Dy1 Co1 34.0(3) . 3_565 ?
O1 Dy1 Co1 162.9(3) . . ?
O1 Dy1 O7 150.0(4) . . ?
O1 Dy1 O7 71.8(4) . 3_565 ?
O1 Dy1 C29 105.6(3) . . ?
O1 Dy1 O9 91.7(4) . . ?
O1 Dy1 O2 62.3(4) . . ?
O1 Dy1 O8 78.8(4) . . ?
O1 Dy1 O8 127.8(4) . 2_665 ?
O1 Dy1 O4 82.0(4) . . ?
O9 Dy1 Co1 78.6(3) . . ?
O9 Dy1 Co1 85.0(3) . 3_565 ?
O9 Dy1 C29 139.1(6) . . ?
O9 Dy1 O2 68.7(4) . . ?
O9 Dy1 O8 141.8(4) . . ?
O9 Dy1 O8 136.2(4) . 2_665 ?
O9 Dy1 O4 137.3(4) . . ?
O2 Dy1 Co1 90.7(3) . 3_565 ?
O2 Dy1 Co1 100.9(3) . . ?
O2 Dy1 C29 151.9(5) . . ?
O8 Dy1 Co1 117.4(3) . . ?
O8 Dy1 Co1 66.8(3) 2_665 . ?
O8 Dy1 Co1 66.5(3) . 3_565 ?
O8 Dy1 Co1 116.0(3) 2_665 3_565 ?
O8 Dy1 C29 26.8(3) . . ?
O8 Dy1 C29 26.8(3) 2_665 . ?
O8 Dy1 O2 132.8(4) . . ?
O8 Dy1 O2 141.8(4) 2_665 . ?
O8 Dy1 O8 51.5(5) . 2_665 ?
O3 Dy1 Co1 35.2(3) . . ?
O3 Dy1 Co1 164.6(3) . 3_565 ?
O3 Dy1 O7 74.4(4) . . ?
O3 Dy1 O7 153.1(4) . 3_565 ?
O3 Dy1 C29 104.1(3) . . ?
O3 Dy1 O1 132.2(4) . . ?
O3 Dy1 O9 89.6(4) . . ?
O3 Dy1 O2 73.9(4) . . ?
O3 Dy1 O8 77.6(4) . 2_665 ?
O3 Dy1 O8 124.1(4) . . ?
O3 Dy1 O4 65.8(4) . . ?
O4 Dy1 Co1 109.3(2) . 3_565 ?
O4 Dy1 Co1 95.6(2) . . ?
O4 Dy1 C29 82.5(6) . . ?
O4 Dy1 O2 71.0(4) . . ?
O4 Dy1 O8 78.4(4) . . ?
O4 Dy1 O8 74.3(4) . 2_665 ?
Dy1 Co1 Dy1 72.73(5) . 2_665 ?
O7 Co1 Dy1 44.2(3) . . ?
O7 Co1 Dy1 42.2(3) . 2_665 ?
O1 Co1 Dy1 40.9(3) 2_665 2_665 ?
O1 Co1 Dy1 107.3(3) 2_665 . ?
O1 Co1 O7 82.9(4) 2_665 . ?
O1 Co1 N1 93.3(5) 2_665 . ?
O3 Co1 Dy1 105.8(3) . 2_665 ?
O3 Co1 Dy1 41.9(3) . . ?
O3 Co1 O7 86.1(4) . . ?
O3 Co1 O1 121.7(5) . 2_665 ?
O3 Co1 N1 93.5(5) . . ?
O5 Co1 Dy1 116.5(4) . 2_665 ?
O5 Co1 Dy1 102.2(4) . . ?
O5 Co1 O7 89.8(4) . . ?
O5 Co1 O1 127.8(5) . 2_665 ?
O5 Co1 O3 109.1(5) . . ?
O5 Co1 N1 94.8(5) . . ?
N1 Co1 Dy1 135.4(3) . . ?
N1 Co1 Dy1 133.8(4) . 2_665 ?
N1 Co1 O7 175.2(5) . . ?
Dy1 O7 Dy1 118.1(4) 2_665 . ?
Co1 O7 Dy1 96.6(4) . . ?
Co1 O7 Dy1 99.9(4) . 2_665 ?
Dy1 C29 Dy1 92.0(7) . 3_565 ?
Dy1 C29 Dy1 92.0(7) . 2_665 ?
Dy1 C29 Dy1 92.0(7) 3_565 2_665 ?
O8 C29 Dy1 143.5(18) 3_565 . ?
O8 C29 Dy1 61.4(8) 2_665 2_665 ?
O8 C29 Dy1 66.4(8) 3_565 2_665 ?
O8 C29 Dy1 61.4(8) . . ?
O8 C29 Dy1 61.4(8) 3_565 3_565 ?
O8 C29 Dy1 66.4(8) 2_665 . ?
O8 C29 Dy1 66.4(8) . 3_565 ?
O8 C29 Dy1 143.5(18) 2_665 3_565 ?
O8 C29 Dy1 143.5(18) . 2_665 ?
O8 C29 O8 119.8(2) 3_565 . ?
O8 C29 O8 119.8(2) . 2_665 ?
O8 C29 O8 119.8(2) 3_565 2_665 ?
Co1 O1 Dy1 105.1(5) 3_565 . ?
C10 O1 Dy1 126.6(10) . . ?
C10 O1 Co1 121.5(10) . 3_565 ?
C11 O2 Dy1 117.7(10) . . ?
C11 O2 C12 116.4(13) . . ?
C12 O2 Dy1 125.6(10) . . ?
Dy1 O8 Dy1 106.4(4) . 3_565 ?
C29 O8 Dy1 86.8(9) . 3_565 ?
C29 O8 Dy1 91.8(10) . . ?
O2 C11 C13 125.7(17) . . ?
O2 C11 C10 113.1(14) . . ?
C10 C11 C13 121.2(17) . . ?
C16 C20 C18 120.7(16) . . ?
C16 C20 C10 118.4(17) . . ?
C10 C20 C18 120.6(15) . . ?
N1 C18 C20 112.2(14) 3_565 . ?
C11 C13 C14 117.6(18) . . ?
C14 C16 C20 120.7(17) . . ?
C13 C14 C15 116.1(19) . . ?
C16 C14 C15 122(2) . . ?
C16 C14 C13 122.1(17) . . ?
C8 C9 N1 114.4(14) . . ?
C1 C2 C4 119.4(16) . . ?
O4 C2 C1 114.8(14) . . ?
O4 C2 C4 125.9(15) . . ?
C2 C1 C8 119.7(16) . . ?
O3 C1 C2 119.0(14) . . ?
O3 C1 C8 121.3(16) . . ?
C5 C4 C2 122.9(18) . . ?
C1 C8 C9 120.8(17) . . ?
C1 C8 C7 118.9(18) . . ?
C7 C8 C9 119.6(16) . . ?
C5 C7 C8 120.1(17) . . ?
C4 C5 C7 118.9(17) . . ?
C4 C5 C6 121(2) . . ?
C7 C5 C6 120(2) . . ?
Co1 O3 Dy1 102.9(4) . . ?
C1 O3 Dy1 122.7(9) . . ?
C1 O3 Co1 123.0(9) . . ?
C27 C28 N1 112.9(14) . . ?
O5 C19 C27 121.3(16) . . ?
O5 C19 C21 118.8(18) . . ?
C21 C19 C27 119.8(18) . . ?
C24 C26 C27 123(2) . . ?
C28 C27 C26 120.8(18) . . ?
C19 C27 C28 121.5(16) . . ?
C19 C27 C26 117.5(19) . . ?
C2 O4 Dy1 117.8(9) . . ?
C2 O4 C3 116.6(13) . . ?
C3 O4 Dy1 125.4(10) . . ?
C19 O5 Co1 118.9(11) . . ?
C18 N1 Co1 111.3(10) 2_665 . ?
C18 N1 C9 108.5(13) 2_665 . ?
C18 N1 C28 111.9(12) 2_665 . ?
C9 N1 Co1 110.4(9) . . ?
C28 N1 Co1 107.0(10) . . ?
C28 N1 C9 107.6(12) . . ?
O1 C10 C11 119.5(15) . . ?
O1 C10 C20 120.7(16) . . ?
C11 C10 C20 119.7(15) . . ?
C19 C21 C23 120(2) . . ?
O6 C21 C19 117.3(17) . . ?
O6 C21 C23 122(2) . . ?
C24 C23 C21 121(2) . . ?
C26 C24 C25 117(3) . . ?
C23 C24 C26 118(2) . . ?
C23 C24 C25 125(2) . . ?
C22 O6 C21 120(2) . . ?
O11 Cl1 O10 111(2) 3_665 . ?
O11 Cl1 O10 111(2) 2_655 . ?
O11 Cl1 O10 111(2) . . ?
O11 Cl1 O11 108(2) 2_655 . ?
O11 Cl1 O11 108(2) 3_665 . ?
O11 Cl1 O11 108(2) 2_655 3_665 ?

_olex2_submission_special_instructions 'No special instructions were received'

#
_vrf_PLAT342_Compound_4          
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02958 Ang.
RESPONSE: This is due to nonavailability of enough high precision data.
;
_vrf_PLAT412_Compound_4          
;
PROBLEM: Short Intra XH3 .. XHn   H3A      ..H4        ..       1.76 Ang.
            
RESPONSE: This alert is arising due to conformational complexity.
;
# end Validation Reply Form

_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_Compound_2
_database_code_depnum_ccdc_archive 'CCDC 1579342'
_audit_update_record             
;
2018-01-04 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;
_audit_creation_date             2018-01-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C82 H90 Co3 Gd3 N3 O27, Cl1 O4'
_chemical_formula_sum            'C82 H90 Cl Co3 Gd3 N3 O31'
_chemical_formula_weight         2297.55
_chemical_absolute_configuration ?
_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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   18.4477(11)
_cell_length_b                   18.4477(11)
_cell_length_c                   53.653(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     15813(2)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.869
_cell_measurement_theta_min      2.21
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.416
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.5268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1240 before and 0.0633 after correction. The Ratio of minimum to maximum transmission is 0.7071. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   SADABS
_exptl_crystal_colour            magenta
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6846
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   0.7450
_exptl_transmission_factor_min   0.5268
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            42348
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        23.962
_diffrn_reflns_theta_max         23.962
_diffrn_reflns_theta_min         1.484
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                4918
_reflns_number_total             5475
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         2.259
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 
;
 Flack x determined using 2307 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5475
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0539
_refine_ls_restrained_S_all      1.055
_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)+(0.0756P)²+470.2268P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1486
_refine_special_details          SQUEEZE
_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.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C27(H27A,H27B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C4(H4), C16(H16), C25(H25), C22(H22), C7(H7)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C),
 C24(H24A,H24B,H24C), C21(H21A,H21B,H21C)
;
_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
Gd1 Gd 0.25436(4) 0.52059(5) 0.07848(2) 0.0303(3) Uani 1 1 d . . . . .
Co1 Co 0.09298(14) 0.55945(14) 0.08975(4) 0.0300(5) Uani 1 1 d . . . . .
O1 O 0.1099(7) 0.4710(7) 0.0744(2) 0.034(3) Uani 1 1 d . . . . .
O3 O 0.3350(7) 0.4572(7) 0.0722(2) 0.031(3) Uani 1 1 d . . . . .
O2 O 0.1504(8) 0.3586(7) 0.0842(2) 0.039(3) Uani 1 1 d . . . . .
O8 O 0.2526(9) 0.6257(7) 0.0505(2) 0.042(3) Uani 1 1 d . . . . .
O7 O 0.2230(8) 0.6162(7) 0.0984(2) 0.030(2) Uani 1 1 d . . . . .
O4 O 0.2324(7) 0.4510(8) 0.0377(2) 0.038(3) Uani 1 1 d . . . . .
C11 C 0.2796(10) 0.4141(11) 0.0317(3) 0.038(4) Uani 1 1 d . . . . .
C10 C 0.3330(10) 0.4177(10) 0.0508(3) 0.036(4) Uani 1 1 d . . . . .
C13 C 0.2756(12) 0.3750(11) 0.0093(3) 0.042(4) Uani 1 1 d . . . . .
H13 H 0.239240 0.372362 -0.003124 0.051 Uiso 1 1 calc R . . . .
N1 N -0.0344(8) 0.5021(10) 0.0786(3) 0.035(3) Uani 1 1 d . . . . .
O5 O 0.0704(7) 0.5688(7) 0.1248(2) 0.038(3) Uani 1 1 d . . . . .
C4 C 0.0031(12) 0.2438(10) 0.0814(4) 0.040(4) Uani 1 1 d . . . . .
H4 H 0.015714 0.202165 0.085148 0.048 Uiso 1 1 calc R . . . .
C28 C 0.333333 0.666667 0.0489(6) 0.042(8) Uani 1 3 d S T P . .
C2 C 0.0657(11) 0.3278(11) 0.0805(4) 0.046(5) Uani 1 1 d . . . . .
C9 C -0.0539(10) 0.4345(11) 0.0599(3) 0.035(4) Uani 1 1 d . . . . .
H9A H -0.112971 0.407344 0.055764 0.041 Uiso 1 1 calc R . . . .
H9B H -0.022622 0.459934 0.044731 0.041 Uiso 1 1 calc R . . . .
C8 C -0.0338(10) 0.3695(11) 0.0685(3) 0.039(4) Uani 1 1 d . . . . .
C27 C -0.0877(12) 0.4629(12) 0.1021(4) 0.045(5) Uani 1 1 d . . . . .
H27A H -0.146577 0.432351 0.097691 0.054 Uiso 1 1 calc R . . . .
H27B H -0.073242 0.423956 0.109610 0.054 Uiso 1 1 calc R . . . .
C14 C 0.3252(12) 0.3402(11) 0.0055(3) 0.048(5) Uani 1 1 d . . . . .
C16 C 0.3794(12) 0.3440(10) 0.0240(3) 0.042(4) Uani 1 1 d . . . . .
H16 H 0.413186 0.320568 0.021359 0.050 Uiso 1 1 calc R . . . .
C17 C 0.3833(11) 0.3831(10) 0.0468(3) 0.038(4) Uani 1 1 d . . . . .
C15 C 0.3210(15) 0.2992(14) -0.0201(4) 0.062(6) Uani 1 1 d . . . . .
H15A H 0.264312 0.256742 -0.023533 0.093 Uiso 1 1 calc GR . . . .
H15B H 0.356047 0.274460 -0.019803 0.093 Uiso 1 1 calc GR . . . .
H15C H 0.340129 0.341137 -0.032945 0.093 Uiso 1 1 calc GR . . . .
C19 C 0.0067(11) 0.5805(12) 0.1300(3) 0.038(4) Uani 1 1 d . . . . .
C26 C -0.0716(12) 0.5312(13) 0.1202(3) 0.045(5) Uani 1 1 d . . . . .
C25 C -0.1374(13) 0.5472(15) 0.1262(3) 0.057(6) Uani 1 1 d . . . . .
H25 H -0.189428 0.514370 0.118778 0.068 Uiso 1 1 calc R . . . .
C22 C -0.0468(15) 0.6598(14) 0.1519(4) 0.058(6) Uani 1 1 d . . . . .
H22 H -0.037975 0.703749 0.162372 0.070 Uiso 1 1 calc R . . . .
C23 C -0.1276(16) 0.6076(17) 0.1420(5) 0.068(7) Uani 1 1 d . . . . .
C20 C 0.0201(13) 0.6473(13) 0.1465(3) 0.047(5) Uani 1 1 d . . . . .
O6 O 0.0984(9) 0.6940(9) 0.1546(2) 0.054(4) Uani 1 1 d . . . . .
C1 C 0.0472(10) 0.3925(11) 0.0739(3) 0.034(4) Uani 1 1 d . . . . .
C7 C -0.0968(11) 0.2849(12) 0.0701(3) 0.043(4) Uani 1 1 d . . . . .
H7 H -0.151891 0.270218 0.066625 0.052 Uiso 1 1 calc R . . . .
C6 C -0.1468(12) 0.1314(12) 0.0790(4) 0.047(5) Uani 1 1 d . . . . .
H6A H -0.121351 0.097107 0.077973 0.071 Uiso 1 1 calc GR . . . .
H6B H -0.186846 0.116665 0.065727 0.071 Uiso 1 1 calc GR . . . .
H6C H -0.174644 0.122606 0.094719 0.071 Uiso 1 1 calc GR . . . .
C5 C -0.0789(12) 0.2242(11) 0.0765(3) 0.046(5) Uani 1 1 d . . . . .
C18 C -0.0557(12) 0.5643(12) 0.0672(3) 0.041(4) Uani 1 1 d . . . . .
H18A H -0.112567 0.533736 0.060922 0.049 Uiso 1 1 calc R . . . .
H18B H -0.054614 0.601078 0.080356 0.049 Uiso 1 1 calc R . . . .
C3 C 0.1745(14) 0.3024(13) 0.0951(4) 0.055(5) Uani 1 1 d . . . . .
H3A H 0.145767 0.281580 0.110629 0.083 Uiso 1 1 calc GR . . . .
H3B H 0.233804 0.331735 0.097898 0.083 Uiso 1 1 calc GR . . . .
H3C H 0.159894 0.256407 0.083923 0.083 Uiso 1 1 calc GR . . . .
C12 C 0.1732(16) 0.4439(17) 0.0201(4) 0.068(7) Uani 1 1 d . . . . .
H12A H 0.201386 0.479892 0.006159 0.102 Uiso 1 1 calc GR . . . .
H12B H 0.136065 0.460084 0.027510 0.102 Uiso 1 1 calc GR . . . .
H12C H 0.141584 0.387035 0.014410 0.102 Uiso 1 1 calc GR . . . .
O9 O 0.2384(7) 0.4792(8) 0.1227(2) 0.034(3) Uani 1 1 d . . . . .
Cl1 Cl 0.666667 0.333333 0.0634(3) 0.076(3) Uani 1 3 d S T P . .
C24 C -0.200(2) 0.619(3) 0.1494(6) 0.110(13) Uani 1 1 d . . . . .
H24A H -0.229409 0.619862 0.134770 0.165 Uiso 1 1 calc GR . . . .
H24B H -0.179120 0.671187 0.158190 0.165 Uiso 1 1 calc GR . . . .
H24C H -0.237129 0.573853 0.160037 0.165 Uiso 1 1 calc GR . . . .
O11 O 0.7002(15) 0.2883(15) 0.0549(8) 0.170(17) Uani 1 1 d . . . . .
C21 C 0.1155(19) 0.7563(18) 0.1729(5) 0.095(9) Uani 1 1 d . . . . .
H21A H 0.086729 0.785941 0.168624 0.143 Uiso 1 1 calc GR . . . .
H21B H 0.174644 0.794905 0.173489 0.143 Uiso 1 1 calc GR . . . .
H21C H 0.096668 0.730280 0.188882 0.143 Uiso 1 1 calc GR . . . .
O12 O 0.666667 0.333333 0.0892(11) 0.36(7) Uani 1 3 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 Co1 3.446(2) . ?
Gd1 Co1 3.376(2) 2_665 ?
Gd1 O1 2.356(11) . ?
Gd1 O3 2.331(11) . ?
Gd1 O2 2.640(12) . ?
Gd1 O8 2.580(12) 2_665 ?
Gd1 O8 2.464(11) . ?
Gd1 O7 2.368(10) . ?
Gd1 O7 2.360(10) 2_665 ?
Gd1 O4 2.464(11) . ?
Gd1 C28 2.825(18) . ?
Gd1 O9 2.465(11) . ?
Co1 O1 1.985(12) . ?
Co1 O3 1.979(11) 3_565 ?
Co1 O7 2.134(13) . ?
Co1 N1 2.124(13) . ?
Co1 O5 1.953(11) . ?
O1 C1 1.33(2) . ?
O3 C10 1.35(2) . ?
O2 C2 1.38(2) . ?
O2 C3 1.44(2) . ?
O8 C28 1.292(14) . ?
O4 C11 1.38(2) . ?
O4 C12 1.40(2) . ?
C11 C10 1.40(2) . ?
C11 C13 1.38(2) . ?
C10 C17 1.38(2) . ?
C13 C14 1.37(3) . ?
N1 C9 1.50(2) . ?
N1 C27 1.54(2) . ?
N1 C18 1.52(2) . ?
O5 C19 1.33(2) . ?
C4 C2 1.40(2) . ?
C4 C5 1.39(3) . ?
C2 C1 1.44(3) . ?
C9 C8 1.50(3) . ?
C8 C1 1.36(2) . ?
C8 C7 1.41(2) . ?
C27 C26 1.50(3) . ?
C14 C16 1.39(3) . ?
C14 C15 1.55(2) . ?
C16 C17 1.40(2) . ?
C17 C18 1.48(3) 2_665 ?
C19 C26 1.37(3) . ?
C19 C20 1.44(3) . ?
C26 C25 1.42(3) . ?
C25 C23 1.34(3) . ?
C22 C23 1.42(3) . ?
C22 C20 1.39(3) . ?
C23 C24 1.50(3) . ?
C20 O6 1.33(2) . ?
O6 C21 1.42(3) . ?
C7 C5 1.36(3) . ?
C6 C5 1.54(2) . ?
Cl1 O11 1.34(3) 2_655 ?
Cl1 O11 1.34(3) 3_665 ?
Cl1 O11 1.34(3) . ?
Cl1 O12 1.38(6) . ?

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
Co1 Gd1 Co1 155.22(8) 2_665 . ?
O1 Gd1 Co1 33.9(3) . . ?
O1 Gd1 Co1 163.2(3) . 2_665 ?
O1 Gd1 O2 62.0(4) . . ?
O1 Gd1 O8 78.0(4) . . ?
O1 Gd1 O8 128.0(4) . 2_665 ?
O1 Gd1 O7 71.4(4) . . ?
O1 Gd1 O7 150.5(4) . 2_665 ?
O1 Gd1 O4 81.8(4) . . ?
O1 Gd1 C28 105.2(3) . . ?
O1 Gd1 O9 91.8(4) . . ?
O3 Gd1 Co1 34.9(3) . 2_665 ?
O3 Gd1 Co1 164.6(3) . . ?
O3 Gd1 O1 132.4(4) . . ?
O3 Gd1 O2 74.5(4) . . ?
O3 Gd1 O8 77.2(4) . 2_665 ?
O3 Gd1 O8 124.7(4) . . ?
O3 Gd1 O7 73.7(4) . 2_665 ?
O3 Gd1 O7 153.4(4) . . ?
O3 Gd1 O4 65.8(4) . . ?
O3 Gd1 C28 104.1(3) . . ?
O3 Gd1 O9 89.5(4) . . ?
O2 Gd1 Co1 90.1(3) . . ?
O2 Gd1 Co1 101.3(3) . 2_665 ?
O2 Gd1 C28 151.8(6) . . ?
O8 Gd1 Co1 65.8(3) . . ?
O8 Gd1 Co1 116.5(3) 2_665 . ?
O8 Gd1 Co1 66.1(3) 2_665 2_665 ?
O8 Gd1 Co1 117.8(3) . 2_665 ?
O8 Gd1 O2 132.3(4) . . ?
O8 Gd1 O2 142.2(4) 2_665 . ?
O8 Gd1 O8 52.5(6) . 2_665 ?
O8 Gd1 O4 78.9(4) . . ?
O8 Gd1 C28 27.2(4) . . ?
O8 Gd1 C28 27.2(3) 2_665 . ?
O8 Gd1 O9 141.6(4) . . ?
O7 Gd1 Co1 117.9(3) 2_665 . ?
O7 Gd1 Co1 37.6(3) . . ?
O7 Gd1 Co1 38.8(3) 2_665 2_665 ?
O7 Gd1 Co1 119.0(3) . 2_665 ?
O7 Gd1 O2 128.9(4) 2_665 . ?
O7 Gd1 O2 118.8(4) . . ?
O7 Gd1 O8 98.7(4) 2_665 . ?
O7 Gd1 O8 97.5(4) . 2_665 ?
O7 Gd1 O8 63.6(4) 2_665 2_665 ?
O7 Gd1 O8 65.4(4) . . ?
O7 Gd1 O7 80.6(6) 2_665 . ?
O7 Gd1 O4 126.8(4) 2_665 . ?
O7 Gd1 O4 138.6(4) . . ?
O7 Gd1 C28 75.3(5) 2_665 . ?
O7 Gd1 C28 75.2(5) . . ?
O7 Gd1 O9 72.4(4) 2_665 . ?
O7 Gd1 O9 76.2(4) . . ?
O4 Gd1 Co1 95.3(3) . 2_665 ?
O4 Gd1 Co1 109.3(3) . . ?
O4 Gd1 O2 71.1(4) . . ?
O4 Gd1 O8 74.7(4) . 2_665 ?
O4 Gd1 C28 82.6(6) . . ?
O4 Gd1 O9 136.9(4) . . ?
C28 Gd1 Co1 90.69(12) . 2_665 ?
C28 Gd1 Co1 89.27(12) . . ?
O9 Gd1 Co1 85.1(2) . . ?
O9 Gd1 Co1 79.0(2) . 2_665 ?
O9 Gd1 O2 68.4(4) . . ?
O9 Gd1 O8 136.0(4) . 2_665 ?
O9 Gd1 C28 139.6(6) . . ?
Gd1 Co1 Gd1 72.75(5) 3_565 . ?
O1 Co1 Gd1 41.4(3) . . ?
O1 Co1 Gd1 107.7(3) . 3_565 ?
O1 Co1 O7 83.9(4) . . ?
O1 Co1 N1 93.6(5) . . ?
O3 Co1 Gd1 42.3(3) 3_565 3_565 ?
O3 Co1 Gd1 106.4(3) 3_565 . ?
O3 Co1 O1 122.3(5) 3_565 . ?
O3 Co1 O7 86.2(4) 3_565 . ?
O3 Co1 N1 92.6(5) 3_565 . ?
O7 Co1 Gd1 42.6(3) . . ?
O7 Co1 Gd1 43.9(3) . 3_565 ?
N1 Co1 Gd1 134.8(4) . 3_565 ?
N1 Co1 Gd1 134.6(4) . . ?
N1 Co1 O7 176.1(5) . . ?
O5 Co1 Gd1 102.6(4) . 3_565 ?
O5 Co1 Gd1 115.6(4) . . ?
O5 Co1 O1 126.8(5) . . ?
O5 Co1 O3 109.6(5) . 3_565 ?
O5 Co1 O7 89.1(5) . . ?
O5 Co1 N1 94.8(5) . . ?
Co1 O1 Gd1 104.8(5) . . ?
C1 O1 Gd1 128.7(10) . . ?
C1 O1 Co1 119.8(10) . . ?
Co1 O3 Gd1 102.8(5) 2_665 . ?
C10 O3 Gd1 122.8(10) . . ?
C10 O3 Co1 122.7(10) . 2_665 ?
C2 O2 Gd1 118.7(10) . . ?
C2 O2 C3 117.0(15) . . ?
C3 O2 Gd1 123.5(11) . . ?
Gd1 O8 Gd1 106.7(4) . 3_565 ?
C28 O8 Gd1 92.1(10) . . ?
C28 O8 Gd1 87.0(10) . 3_565 ?
Gd1 O7 Gd1 117.7(4) 3_565 . ?
Co1 O7 Gd1 97.3(4) . 3_565 ?
Co1 O7 Gd1 99.8(5) . . ?
C11 O4 Gd1 119.0(9) . . ?
C11 O4 C12 116.6(14) . . ?
C12 O4 Gd1 124.4(11) . . ?
O4 C11 C10 114.0(15) . . ?
C13 C11 O4 125.3(16) . . ?
C13 C11 C10 120.8(17) . . ?
O3 C10 C11 118.4(16) . . ?
O3 C10 C17 122.5(16) . . ?
C17 C10 C11 119.1(16) . . ?
C14 C13 C11 120.0(18) . . ?
C9 N1 Co1 110.4(9) . . ?
C9 N1 C27 109.1(14) . . ?
C9 N1 C18 108.3(13) . . ?
C27 N1 Co1 107.0(11) . . ?
C18 N1 Co1 112.2(11) . . ?
C18 N1 C27 109.8(13) . . ?
C19 O5 Co1 117.5(10) . . ?
C5 C4 C2 118.1(17) . . ?
Gd1 C28 Gd1 91.5(7) 3_565 2_665 ?
Gd1 C28 Gd1 91.5(7) 2_665 . ?
Gd1 C28 Gd1 91.5(7) 3_565 . ?
O8 C28 Gd1 65.8(9) . 3_565 ?
O8 C28 Gd1 65.8(9) 3_565 2_665 ?
O8 C28 Gd1 142(2) 3_565 . ?
O8 C28 Gd1 60.6(8) 3_565 3_565 ?
O8 C28 Gd1 60.6(8) 2_665 2_665 ?
O8 C28 Gd1 142(2) 2_665 3_565 ?
O8 C28 Gd1 65.8(9) 2_665 . ?
O8 C28 Gd1 142(2) . 2_665 ?
O8 C28 Gd1 60.6(8) . . ?
O8 C28 O8 119.5(4) . 3_565 ?
O8 C28 O8 119.5(4) 3_565 2_665 ?
O8 C28 O8 119.5(4) . 2_665 ?
O2 C2 C4 126.1(17) . . ?
O2 C2 C1 112.5(15) . . ?
C4 C2 C1 121.4(18) . . ?
C8 C9 N1 113.9(14) . . ?
C1 C8 C9 119.2(16) . . ?
C1 C8 C7 120.1(18) . . ?
C7 C8 C9 120.6(15) . . ?
C26 C27 N1 109.0(15) . . ?
C13 C14 C16 120.3(16) . . ?
C13 C14 C15 118.5(19) . . ?
C16 C14 C15 121(2) . . ?
C14 C16 C17 120.0(18) . . ?
C10 C17 C16 119.9(17) . . ?
C10 C17 C18 120.5(16) . 2_665 ?
C16 C17 C18 119.4(16) . 2_665 ?
O5 C19 C26 122.6(16) . . ?
O5 C19 C20 118.8(17) . . ?
C26 C19 C20 118.5(16) . . ?
C19 C26 C27 120.4(16) . . ?
C19 C26 C25 120.2(19) . . ?
C25 C26 C27 119.3(19) . . ?
C23 C25 C26 123(2) . . ?
C20 C22 C23 122(2) . . ?
C25 C23 C22 117.6(19) . . ?
C25 C23 C24 122(3) . . ?
C22 C23 C24 121(2) . . ?
C22 C20 C19 119(2) . . ?
O6 C20 C19 114.9(16) . . ?
O6 C20 C22 126.1(19) . . ?
C20 O6 C21 118.5(19) . . ?
O1 C1 C2 117.4(15) . . ?
O1 C1 C8 124.5(17) . . ?
C8 C1 C2 118.1(16) . . ?
C5 C7 C8 121.4(17) . . ?
C4 C5 C6 116.5(19) . . ?
C7 C5 C4 120.9(16) . . ?
C7 C5 C6 122.7(18) . . ?
C17 C18 N1 115.8(14) 3_565 . ?
O11 Cl1 O11 109.1(19) 2_655 3_665 ?
O11 Cl1 O11 109.1(19) . 2_655 ?
O11 Cl1 O11 109.1(19) . 3_665 ?
O11 Cl1 O12 109.9(19) . . ?
O11 Cl1 O12 109.9(19) 3_665 . ?
O11 Cl1 O12 109.9(19) 2_655 . ?

_olex2_submission_special_instructions 'No special instructions were received'

#
_vrf_THETM01_Compound_2          
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: This is due to the crystal not diffracting at higher Bragg angle.
;
_vrf_PLAT342_Compound_2          
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03167 Ang.
            
RESPONSE: This is due to nonavailability of enough high precision data.
;
# end Validation Reply Form
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_Compound_3
_database_code_depnum_ccdc_archive 'CCDC 1579343'
_audit_update_record             
;
2018-01-04 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;
_audit_creation_date             2018-01-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1(C82 H90 Co3 N3 O27 Tb3), 1(Cl1 O4)'
_chemical_formula_sum            'C82 H90 Cl Co3 N3 O31 Tb3'
_chemical_formula_weight         2302.59
_chemical_absolute_configuration ?
_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'
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           'R 3 -2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'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'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'

_cell_length_a                   18.4775(15)
_cell_length_b                   18.4775(15)
_cell_length_c                   53.567(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     15839(3)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9250
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.22
_cell_measurement_theta_min      2.20
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.537
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1710 before and 0.0626 after correction.
The Ratio of minimum to maximum transmission is 0.6447.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   SADABS
_exptl_crystal_colour            magenta
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6864
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.4804
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            49350
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.336
_diffrn_reflns_theta_min         1.482
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.979
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                5629
_reflns_number_total             6387
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.735
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details 
;
 Flack x determined using 2487 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         6387
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0429
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0583P)²+199.8359P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1142
_refine_special_details          SQUEEZE
_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.a Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C39(H39A,H39B), C47(H47A,H47B)
2.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C45(H45), C54(H54), C51(H51), C37(H37), C34(H34)
2.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C8(H8A,H8B,H8C), C33(H33A,H33B,H33C), C36(H36A,H36B,
 H36C), C53(H53A,H53B,H53C), C50(H50A,H50B,H50C)
;
_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
Tb1 Tb 0.85478(4) 0.93431(3) 0.52198(2) 0.02545(16) Uani 1 1 d . . . . .
Co1 Co 0.86586(10) 0.76074(10) 0.51065(3) 0.0256(4) Uani 1 1 d . . . . .
O3 O 0.8065(6) 1.0288(5) 0.52617(16) 0.0304(19) Uani 1 1 d . . . . .
O1 O 0.7912(5) 0.7911(5) 0.52827(15) 0.0282(18) Uani 1 1 d . . . . .
O4 O 0.6933(6) 0.8759(5) 0.51637(17) 0.033(2) Uani 1 1 d . . . . .
O8 O 0.9604(5) 1.0397(5) 0.54985(15) 0.0309(19) Uani 1 1 d . . . . .
O7 O 0.9502(5) 1.0599(5) 0.50196(15) 0.0259(17) Uani 1 1 d . . . . .
C44 C 0.4681(9) 0.9492(12) 0.5221(4) 0.054(5) Uani 1 1 d . . . . .
H44A H 0.455552 0.976196 0.535390 0.081 Uiso 1 1 calc GR . . . .
H44B H 0.432795 0.889758 0.523562 0.081 Uiso 1 1 calc GR . . . .
H44C H 0.458344 0.967475 0.506345 0.081 Uiso 1 1 calc GR . . . .
C42 C 0.5802(8) 0.9106(9) 0.5191(3) 0.036(3) Uani 1 1 d . . . . .
H42 H 0.538617 0.856695 0.515027 0.043 Uiso 1 1 calc R . . . .
C41 C 0.6633(8) 0.9299(8) 0.5205(2) 0.034(3) Uani 1 1 d . . . . .
C46 C 0.7053(8) 1.0715(8) 0.5323(2) 0.034(3) Uani 1 1 d . . . . .
C45 C 0.6213(8) 1.0508(8) 0.5303(2) 0.035(3) Uani 1 1 d . . . . .
H45 H 0.607068 1.091700 0.533327 0.042 Uiso 1 1 calc R . . . .
C40 C 0.7275(8) 1.0127(8) 0.5268(2) 0.031(3) Uani 1 1 d . . . . .
C43 C 0.5597(8) 0.9719(10) 0.5239(3) 0.040(3) Uani 1 1 d . . . . .
C8 C 0.6369(9) 0.7952(9) 0.5050(3) 0.047(4) Uani 1 1 d . . . . .
H8A H 0.590035 0.763855 0.515892 0.070 Uiso 1 1 calc GR . . . .
H8B H 0.665950 0.764920 0.502466 0.070 Uiso 1 1 calc GR . . . .
H8C H 0.617461 0.803719 0.489284 0.070 Uiso 1 1 calc GR . . . .
C54 C 0.6474(8) 0.5314(9) 0.4740(2) 0.044(3) Uani 1 1 d . . . . .
H54 H 0.627696 0.478847 0.481093 0.053 Uiso 1 1 calc R . . . .
C55 C 0.7287(8) 0.5959(8) 0.4802(3) 0.040(3) Uani 1 1 d . . . . .
C48 C 0.7577(7) 0.6748(8) 0.4702(2) 0.031(3) Uani 1 1 d . . . . .
C49 C 0.7053(9) 0.6886(9) 0.4538(2) 0.038(3) Uani 1 1 d . . . . .
C51 C 0.6263(9) 0.6230(10) 0.4480(3) 0.050(4) Uani 1 1 d . . . . .
H51 H 0.592357 0.632243 0.437212 0.061 Uiso 1 1 calc R . . . .
C52 C 0.5967(9) 0.5433(10) 0.4581(3) 0.053(4) Uani 1 1 d . . . . .
C56 C 0.7795(8) 0.5798(8) 0.4984(2) 0.035(3) Uani 1 1 d . . . . .
H56A H 0.832229 0.592671 0.490765 0.041 Uiso 1 1 calc R . . . .
H56B H 0.750194 0.521252 0.503002 0.041 Uiso 1 1 calc R . . . .
C39 C 0.7132(8) 0.6134(9) 0.5331(2) 0.034(3) Uani 1 1 d . . . . .
H39A H 0.677795 0.614706 0.519923 0.041 Uiso 1 1 calc R . . . .
H39B H 0.686789 0.556695 0.539426 0.041 Uiso 1 1 calc R . . . .
C31 C 0.7523(7) 0.7539(8) 0.5495(2) 0.027(3) Uani 1 1 d . . . . .
C37 C 0.6788(7) 0.6358(8) 0.5763(2) 0.035(3) Uani 1 1 d . . . . .
H37 H 0.655192 0.578584 0.578903 0.042 Uiso 1 1 calc R . . . .
C32 C 0.7499(8) 0.8045(8) 0.5688(2) 0.030(3) Uani 1 1 d . . . . .
C34 C 0.7116(7) 0.7697(8) 0.5912(2) 0.036(3) Uani 1 1 d . . . . .
H34 H 0.710336 0.803737 0.603745 0.044 Uiso 1 1 calc R . . . .
C38 C 0.7168(7) 0.6697(7) 0.5537(2) 0.032(3) Uani 1 1 d . . . . .
C35 C 0.6750(8) 0.6845(10) 0.5950(3) 0.042(3) Uani 1 1 d . . . . .
C33 C 0.7875(11) 0.9433(9) 0.5816(2) 0.053(4) Uani 1 1 d . . . . .
H33A H 0.731153 0.925322 0.586708 0.080 Uiso 1 1 calc GR . . . .
H33B H 0.812443 0.998870 0.574961 0.080 Uiso 1 1 calc GR . . . .
H33C H 0.819149 0.942907 0.595790 0.080 Uiso 1 1 calc GR . . . .
N1 N 0.7959(6) 0.6343(6) 0.5219(2) 0.031(2) Uani 1 1 d . . . . .
O2 O 0.7870(6) 0.8881(5) 0.56304(16) 0.033(2) Uani 1 1 d . . . . .
O5 O 0.8338(5) 0.7382(5) 0.47564(15) 0.034(2) Uani 1 1 d . . . . .
O6 O 0.7361(7) 0.7673(6) 0.44566(17) 0.048(3) Uani 1 1 d . . . . .
C47 C 0.7711(7) 1.1562(7) 0.5404(2) 0.029(3) Uani 1 1 d . . . . .
H47A H 0.744560 1.188557 0.544511 0.035 Uiso 1 1 calc R . . . .
H47B H 0.796578 1.150410 0.555521 0.035 Uiso 1 1 calc R . . . .
C57 C 1.000000 1.000000 0.5510(3) 0.023(4) Uani 1 3 d S T P . .
O9 O 0.8126(6) 0.9083(5) 0.47760(15) 0.0322(19) Uani 1 1 d . . . . .
C36 C 0.6338(10) 0.6487(11) 0.6206(3) 0.055(4) Uani 1 1 d . . . . .
H36A H 0.608175 0.588886 0.620315 0.083 Uiso 1 1 calc GR . . . .
H36B H 0.592036 0.663865 0.623862 0.083 Uiso 1 1 calc GR . . . .
H36C H 0.675532 0.671005 0.633446 0.083 Uiso 1 1 calc GR . . . .
C53 C 0.5135(11) 0.4699(14) 0.4508(4) 0.088(7) Uani 1 1 d . . . . .
H53A H 0.521678 0.437987 0.438095 0.131 Uiso 1 1 calc GR . . . .
H53B H 0.477899 0.489684 0.444511 0.131 Uiso 1 1 calc GR . . . .
H53C H 0.487924 0.435144 0.465139 0.131 Uiso 1 1 calc GR . . . .
C50 C 0.6906(13) 0.7843(13) 0.4281(3) 0.078(6) Uani 1 1 d . . . . .
H50A H 0.685222 0.754001 0.412975 0.118 Uiso 1 1 calc GR . . . .
H50B H 0.719233 0.843160 0.424542 0.118 Uiso 1 1 calc GR . . . .
H50C H 0.636028 0.767547 0.434594 0.118 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.666667 0.333333 0.5359(2) 0.081(3) Uani 1 3 d S T P . .
O11 O 0.6345(11) 0.3781(11) 0.5451(5) 0.146(10) Uani 1 1 d . . . . .
O12 O 0.666667 0.333333 0.5087(9) 0.24(3) Uani 1 3 d S T 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
Tb1 Co1 3.4371(17) 3_675 ?
Tb1 Co1 3.3695(17) . ?
Tb1 O3 2.336(8) . ?
Tb1 O1 2.321(8) . ?
Tb1 O4 2.633(9) . ?
Tb1 O8 2.455(8) . ?
Tb1 O8 2.566(8) 2_765 ?
Tb1 O7 2.362(8) 2_765 ?
Tb1 O7 2.357(8) . ?
Tb1 O2 2.463(8) . ?
Tb1 C57 2.798(10) . ?
Tb1 O9 2.473(8) . ?
Co1 O3 1.992(9) 2_765 ?
Co1 O1 1.970(8) . ?
Co1 O7 2.132(9) 2_765 ?
Co1 N1 2.114(11) . ?
Co1 O5 1.948(8) . ?
O3 C40 1.336(15) . ?
O1 C31 1.339(14) . ?
O4 C41 1.380(15) . ?
O4 C8 1.458(16) . ?
O8 C57 1.271(9) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C44 C43 1.531(18) . ?
C42 H42 0.9300 . ?
C42 C41 1.393(17) . ?
C42 C43 1.386(19) . ?
C41 C40 1.431(19) . ?
C46 C45 1.405(18) . ?
C46 C40 1.372(18) . ?
C46 C47 1.488(18) . ?
C45 H45 0.9300 . ?
C45 C43 1.370(19) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C54 H54 0.9300 . ?
C54 C55 1.413(19) . ?
C54 C52 1.36(2) . ?
C55 C48 1.385(19) . ?
C55 C56 1.481(19) . ?
C48 C49 1.421(18) . ?
C48 O5 1.337(14) . ?
C49 C51 1.39(2) . ?
C49 O6 1.342(17) . ?
C51 H51 0.9300 . ?
C51 C52 1.40(2) . ?
C52 C53 1.51(2) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 N1 1.545(16) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C38 1.495(18) . ?
C39 N1 1.502(15) . ?
C31 C32 1.407(17) . ?
C31 C38 1.373(17) . ?
C37 H37 0.9300 . ?
C37 C38 1.383(17) . ?
C37 C35 1.37(2) . ?
C32 C34 1.376(16) . ?
C32 O2 1.376(14) . ?
C34 H34 0.9300 . ?
C34 C35 1.38(2) . ?
C35 C36 1.545(17) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C33 O2 1.422(15) . ?
N1 C47 1.487(16) 2_765 ?
O6 C50 1.401(18) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
Cl1 O11 1.331(18) . ?
Cl1 O11 1.331(18) 3_665 ?
Cl1 O11 1.331(18) 2_655 ?
Cl1 O12 1.46(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Co1 Tb1 Co1 155.18(6) . 3_675 ?
O3 Tb1 Co1 34.1(2) . 3_675 ?
O3 Tb1 Co1 163.1(2) . . ?
O3 Tb1 O4 62.6(3) . . ?
O3 Tb1 O8 127.6(3) . 2_765 ?
O3 Tb1 O8 78.3(3) . . ?
O3 Tb1 O7 71.6(3) . . ?
O3 Tb1 O7 150.6(3) . 2_765 ?
O3 Tb1 O2 81.7(3) . . ?
O3 Tb1 C57 105.3(2) . . ?
O3 Tb1 O9 92.1(3) . . ?
O1 Tb1 Co1 164.7(2) . 3_675 ?
O1 Tb1 Co1 34.7(2) . . ?
O1 Tb1 O3 132.4(3) . . ?
O1 Tb1 O4 74.1(3) . . ?
O1 Tb1 O8 124.4(3) . . ?
O1 Tb1 O8 77.3(3) . 2_765 ?
O1 Tb1 O7 73.6(3) . 2_765 ?
O1 Tb1 O7 153.1(3) . . ?
O1 Tb1 O2 66.2(3) . . ?
O1 Tb1 C57 104.1(2) . . ?
O1 Tb1 O9 89.3(3) . . ?
O4 Tb1 Co1 100.66(18) . . ?
O4 Tb1 Co1 90.66(19) . 3_675 ?
O4 Tb1 C57 152.3(4) . . ?
O8 Tb1 Co1 66.5(2) 2_765 . ?
O8 Tb1 Co1 66.2(2) . 3_675 ?
O8 Tb1 Co1 116.2(2) 2_765 3_675 ?
O8 Tb1 Co1 117.5(2) . . ?
O8 Tb1 O4 133.0(3) . . ?
O8 Tb1 O4 141.9(3) 2_765 . ?
O8 Tb1 O8 51.9(4) . 2_765 ?
O8 Tb1 O2 78.3(3) . . ?
O8 Tb1 C57 27.0(2) 2_765 . ?
O8 Tb1 C57 27.0(2) . . ?
O8 Tb1 O9 141.9(3) . . ?
O7 Tb1 Co1 117.9(2) 2_765 3_675 ?
O7 Tb1 Co1 118.9(2) . . ?
O7 Tb1 Co1 37.7(2) . 3_675 ?
O7 Tb1 Co1 38.9(2) 2_765 . ?
O7 Tb1 O4 128.4(3) 2_765 . ?
O7 Tb1 O4 119.2(3) . . ?
O7 Tb1 O8 63.9(3) 2_765 2_765 ?
O7 Tb1 O8 97.5(3) . 2_765 ?
O7 Tb1 O8 98.4(3) 2_765 . ?
O7 Tb1 O8 65.7(3) . . ?
O7 Tb1 O7 80.4(4) . 2_765 ?
O7 Tb1 O2 138.4(3) . . ?
O7 Tb1 O2 126.7(3) 2_765 . ?
O7 Tb1 C57 75.1(3) . . ?
O7 Tb1 C57 75.0(3) 2_765 . ?
O7 Tb1 O9 72.3(3) 2_765 . ?
O7 Tb1 O9 76.2(3) . . ?
O2 Tb1 Co1 95.37(19) . . ?
O2 Tb1 Co1 109.21(19) . 3_675 ?
O2 Tb1 O4 71.6(3) . . ?
O2 Tb1 O8 74.1(3) . 2_765 ?
O2 Tb1 C57 82.3(4) . . ?
O2 Tb1 O9 137.3(3) . . ?
C57 Tb1 Co1 90.65(7) . . ?
C57 Tb1 Co1 89.26(8) . 3_675 ?
O9 Tb1 Co1 78.77(19) . . ?
O9 Tb1 Co1 85.21(19) . 3_675 ?
O9 Tb1 O4 68.2(3) . . ?
O9 Tb1 O8 136.2(3) . 2_765 ?
O9 Tb1 C57 139.3(4) . . ?
Tb1 Co1 Tb1 72.63(4) . 2_765 ?
O3 Co1 Tb1 41.0(2) 2_765 2_765 ?
O3 Co1 Tb1 107.2(3) 2_765 . ?
O3 Co1 O7 83.4(3) 2_765 2_765 ?
O3 Co1 N1 93.7(4) 2_765 . ?
O1 Co1 Tb1 42.1(3) . . ?
O1 Co1 Tb1 106.0(3) . 2_765 ?
O1 Co1 O3 121.6(4) . 2_765 ?
O1 Co1 O7 86.2(3) . 2_765 ?
O1 Co1 N1 92.9(4) . . ?
O7 Co1 Tb1 42.5(2) 2_765 2_765 ?
O7 Co1 Tb1 44.1(2) 2_765 . ?
N1 Co1 Tb1 134.9(3) . . ?
N1 Co1 Tb1 134.4(3) . 2_765 ?
N1 Co1 O7 175.9(4) . 2_765 ?
O5 Co1 Tb1 102.7(3) . . ?
O5 Co1 Tb1 115.8(3) . 2_765 ?
O5 Co1 O3 127.2(4) . 2_765 ?
O5 Co1 O1 109.9(4) . . ?
O5 Co1 O7 89.2(3) . 2_765 ?
O5 Co1 N1 94.9(4) . . ?
Co1 O3 Tb1 104.9(4) 3_675 . ?
C40 O3 Tb1 128.2(7) . . ?
C40 O3 Co1 120.0(7) . 3_675 ?
Co1 O1 Tb1 103.2(4) . . ?
C31 O1 Tb1 122.9(7) . . ?
C31 O1 Co1 122.3(7) . . ?
C41 O4 Tb1 118.0(7) . . ?
C41 O4 C8 117.7(10) . . ?
C8 O4 Tb1 123.5(8) . . ?
Tb1 O8 Tb1 106.8(3) . 3_675 ?
C57 O8 Tb1 86.7(6) . 3_675 ?
C57 O8 Tb1 91.7(6) . . ?
Tb1 O7 Tb1 117.4(3) . 3_675 ?
Co1 O7 Tb1 97.0(3) 3_675 3_675 ?
Co1 O7 Tb1 99.8(3) 3_675 . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
C41 C42 H42 120.1 . . ?
C43 C42 H42 120.1 . . ?
C43 C42 C41 119.8(13) . . ?
O4 C41 C42 126.6(12) . . ?
O4 C41 C40 113.0(11) . . ?
C42 C41 C40 120.3(12) . . ?
C45 C46 C47 121.3(11) . . ?
C40 C46 C45 119.7(12) . . ?
C40 C46 C47 119.0(12) . . ?
C46 C45 H45 119.2 . . ?
C43 C45 C46 121.7(12) . . ?
C43 C45 H45 119.2 . . ?
O3 C40 C41 117.6(11) . . ?
O3 C40 C46 123.7(12) . . ?
C46 C40 C41 118.7(12) . . ?
C42 C43 C44 118.8(14) . . ?
C45 C43 C44 121.5(13) . . ?
C45 C43 C42 119.7(12) . . ?
O4 C8 H8A 109.5 . . ?
O4 C8 H8B 109.5 . . ?
O4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C55 C54 H54 118.8 . . ?
C52 C54 H54 118.8 . . ?
C52 C54 C55 122.5(15) . . ?
C54 C55 C56 119.9(13) . . ?
C48 C55 C54 119.1(13) . . ?
C48 C55 C56 121.0(12) . . ?
C55 C48 C49 119.2(12) . . ?
O5 C48 C55 121.5(12) . . ?
O5 C48 C49 119.3(12) . . ?
C51 C49 C48 119.7(13) . . ?
O6 C49 C48 115.9(12) . . ?
O6 C49 C51 124.3(13) . . ?
C49 C51 H51 119.4 . . ?
C49 C51 C52 121.3(14) . . ?
C52 C51 H51 119.4 . . ?
C54 C52 C51 118.3(13) . . ?
C54 C52 C53 119.4(16) . . ?
C51 C52 C53 122.2(16) . . ?
C55 C56 H56A 109.7 . . ?
C55 C56 H56B 109.7 . . ?
C55 C56 N1 110.0(10) . . ?
H56A C56 H56B 108.2 . . ?
N1 C56 H56A 109.7 . . ?
N1 C56 H56B 109.7 . . ?
H39A C39 H39B 107.5 . . ?
C38 C39 H39A 108.4 . . ?
C38 C39 H39B 108.4 . . ?
C38 C39 N1 115.5(11) . . ?
N1 C39 H39A 108.4 . . ?
N1 C39 H39B 108.4 . . ?
O1 C31 C32 118.1(11) . . ?
O1 C31 C38 123.3(11) . . ?
C38 C31 C32 118.6(11) . . ?
C38 C37 H37 119.2 . . ?
C35 C37 H37 119.2 . . ?
C35 C37 C38 121.6(12) . . ?
C34 C32 C31 120.5(12) . . ?
O2 C32 C31 114.7(10) . . ?
O2 C32 C34 124.8(11) . . ?
C32 C34 H34 119.8 . . ?
C32 C34 C35 120.4(12) . . ?
C35 C34 H34 119.8 . . ?
C31 C38 C39 119.9(12) . . ?
C31 C38 C37 120.2(12) . . ?
C37 C38 C39 119.8(11) . . ?
C37 C35 C34 118.7(12) . . ?
C37 C35 C36 122.8(14) . . ?
C34 C35 C36 118.4(13) . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O2 C33 H33A 109.5 . . ?
O2 C33 H33B 109.5 . . ?
O2 C33 H33C 109.5 . . ?
C56 N1 Co1 107.5(8) . . ?
C39 N1 Co1 112.3(8) . . ?
C39 N1 C56 108.4(9) . . ?
C47 N1 Co1 110.3(7) 2_765 . ?
C47 N1 C56 109.5(9) 2_765 . ?
C47 N1 C39 108.9(10) 2_765 . ?
C32 O2 Tb1 118.1(7) . . ?
C32 O2 C33 118.0(10) . . ?
C33 O2 Tb1 123.9(7) . . ?
C48 O5 Co1 118.2(7) . . ?
C49 O6 C50 119.1(13) . . ?
C46 C47 H47A 108.4 . . ?
C46 C47 H47B 108.4 . . ?
N1 C47 C46 115.6(10) 3_675 . ?
N1 C47 H47A 108.4 3_675 . ?
N1 C47 H47B 108.4 3_675 . ?
H47A C47 H47B 107.4 . . ?
Tb1 C57 Tb1 92.2(4) . 3_675 ?
Tb1 C57 Tb1 92.2(4) . 2_765 ?
Tb1 C57 Tb1 92.2(4) 2_765 3_675 ?
O8 C57 Tb1 66.3(5) 2_765 . ?
O8 C57 Tb1 66.3(5) 3_675 2_765 ?
O8 C57 Tb1 61.3(5) 2_765 2_765 ?
O8 C57 Tb1 61.3(5) 3_675 3_675 ?
O8 C57 Tb1 66.3(6) . 3_675 ?
O8 C57 Tb1 143.5(12) 3_675 . ?
O8 C57 Tb1 143.5(12) . 2_765 ?
O8 C57 Tb1 61.3(5) . . ?
O8 C57 Tb1 143.5(12) 2_765 3_675 ?
O8 C57 O8 119.78(16) 3_675 . ?
O8 C57 O8 119.78(16) 2_765 . ?
O8 C57 O8 119.78(16) 2_765 3_675 ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O6 C50 H50A 109.5 . . ?
O6 C50 H50B 109.5 . . ?
O6 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O11 Cl1 O11 107.2(14) 3_665 2_655 ?
O11 Cl1 O11 107.2(14) 3_665 . ?
O11 Cl1 O11 107.2(14) 2_655 . ?
O11 Cl1 O12 111.7(13) 3_665 . ?
O11 Cl1 O12 111.7(13) . . ?
O11 Cl1 O12 111.7(13) 2_655 . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_preparation       'Magnetic properties'
