# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

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

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1415098'
_audit_update_record             
;
2016-10-19 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H21 Co Dy N9 O12'
_chemical_formula_weight         812.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   15.0503(2)
_cell_length_b                   15.0503(2)
_cell_length_c                   10.29970(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2020.44(6)
_cell_formula_units_Z            3
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    6983
_cell_measurement_theta_min      8.04
_cell_measurement_theta_max      72.06

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_F_000             1197
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    20.224
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.269
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6533
_diffrn_reflns_av_unetI/netI     0.0838
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         8.047
_diffrn_reflns_theta_max         64.691
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.928
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.928
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.912
_reflns_number_total             1486
_reflns_number_gt                1445
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.966
_reflns_Friedel_fraction_max     0.963
_reflns_Friedel_fraction_full    0.896

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0140P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 662 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1486
_refine_ls_number_parameters     134
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0715
_refine_ls_wR_factor_gt          0.0713
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy Dy 0.0000 1.0000 0.84370(2) 0.0179(3) Uani 1 3 d S T P . .
Co Co 0.0000 1.0000 1.2113(2) 0.0126(6) Uani 1 3 d S T P . .
O1 O 0.0468(5) 0.9148(5) 0.9952(6) 0.0212(15) Uani 1 1 d . . . . .
N1 N -0.1015(5) 0.8831(6) 1.3112(7) 0.0153(18) Uani 1 1 d . . . . .
N2 N -0.0032(5) 0.8947(5) 1.1078(7) 0.0161(18) Uani 1 1 d . . . . .
C1 C -0.1551(7) 0.8830(7) 1.4160(9) 0.022(2) Uani 1 1 d . . . . .
H1 H -0.1459 0.9466 1.4469 0.029 Uiso 1 1 calc R U . . .
C2 C -0.2222(7) 0.7951(7) 1.4795(10) 0.028(2) Uani 1 1 d . . . . .
H2 H -0.2583 0.7973 1.5540 0.036 Uiso 1 1 calc R U . . .
C3 C -0.2365(8) 0.7029(8) 1.4329(11) 0.038(3) Uani 1 1 d . . . . .
H3 H -0.2832 0.6408 1.4752 0.049 Uiso 1 1 calc R U . . .
C4 C -0.1834(7) 0.7006(7) 1.3259(9) 0.027(2) Uani 1 1 d . . . . .
H4 H -0.1926 0.6374 1.2936 0.037 Uiso 1 1 calc R U . . .
C5 C -0.1162(7) 0.7925(7) 1.2661(9) 0.019(2) Uani 1 1 d . . . . .
C6 C -0.0587(7) 0.8007(6) 1.1470(9) 0.018(2) Uani 1 1 d . . . . .
C7 C -0.0683(8) 0.7104(7) 1.0742(10) 0.035(3) Uani 1 1 d . . . . .
H7A H -0.0547 0.7276 0.9819 0.049 Uiso 1 1 calc R U . . .
H7B H -0.1379 0.6520 1.0849 0.049 Uiso 1 1 calc R U . . .
H7C H -0.0186 0.6923 1.1082 0.049 Uiso 1 1 calc R U . . .
N11 N -0.0786(6) 0.8024(6) 0.7211(8) 0.0243(19) Uani 1 1 d . . . . .
O11 O -0.1301(5) 0.8161(5) 0.8071(6) 0.0291(16) Uani 1 1 d . . . . .
O12 O 0.0039(5) 0.8825(5) 0.6852(6) 0.0264(17) Uani 1 1 d . . . . .
O13 O -0.1043(6) 0.7178(5) 0.6744(8) 0.0400(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
Dy O1 2.340(6) . ?
Dy O1 2.340(6) 2_675 ?
Dy O1 2.340(6) 3_465 ?
Dy O12 2.429(6) 3_465 ?
Dy O12 2.429(6) 2_675 ?
Dy O12 2.429(6) . ?
Dy O11 2.493(6) . ?
Dy O11 2.493(6) 2_675 ?
Dy O11 2.493(6) 3_465 ?
Dy N11 2.885(8) . ?
Dy N11 2.885(8) 2_675 ?
Dy N11 2.885(8) 3_465 ?
Co N2 1.890(7) 3_465 ?
Co N2 1.890(7) . ?
Co N2 1.890(7) 2_675 ?
Co N1 1.950(7) 2_675 ?
Co N1 1.950(7) 3_465 ?
Co N1 1.950(8) . ?
O1 N2 1.333(8) . ?
N1 C1 1.348(10) . ?
N1 C5 1.350(11) . ?
N2 C6 1.295(10) . ?
C1 C2 1.365(12) . ?
C1 H1 0.9500 . ?
C2 C3 1.379(12) . ?
C2 H2 0.9500 . ?
C3 C4 1.372(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(12) . ?
C4 H4 0.9500 . ?
C5 C6 1.470(12) . ?
C6 C7 1.494(11) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N11 O13 1.228(10) . ?
N11 O11 1.261(9) . ?
N11 O12 1.278(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy O1 80.4(2) . 2_675 ?
O1 Dy O1 80.4(2) . 3_465 ?
O1 Dy O1 80.4(2) 2_675 3_465 ?
O1 Dy O12 149.7(2) . 3_465 ?
O1 Dy O12 123.7(2) 2_675 3_465 ?
O1 Dy O12 85.7(2) 3_465 3_465 ?
O1 Dy O12 123.7(2) . 2_675 ?
O1 Dy O12 85.7(2) 2_675 2_675 ?
O1 Dy O12 149.7(2) 3_465 2_675 ?
O12 Dy O12 79.8(2) 3_465 2_675 ?
O1 Dy O12 85.7(2) . . ?
O1 Dy O12 149.7(2) 2_675 . ?
O1 Dy O12 123.7(2) 3_465 . ?
O12 Dy O12 79.8(2) 3_465 . ?
O12 Dy O12 79.8(2) 2_675 . ?
O1 Dy O11 77.1(2) . . ?
O1 Dy O11 146.7(2) 2_675 . ?
O1 Dy O11 71.9(2) 3_465 . ?
O12 Dy O11 73.0(2) 3_465 . ?
O12 Dy O11 127.3(2) 2_675 . ?
O12 Dy O11 51.8(2) . . ?
O1 Dy O11 71.9(2) . 2_675 ?
O1 Dy O11 77.1(2) 2_675 2_675 ?
O1 Dy O11 146.7(2) 3_465 2_675 ?
O12 Dy O11 127.3(2) 3_465 2_675 ?
O12 Dy O11 51.8(2) 2_675 2_675 ?
O12 Dy O11 73.0(2) . 2_675 ?
O11 Dy O11 117.75(8) . 2_675 ?
O1 Dy O11 146.7(2) . 3_465 ?
O1 Dy O11 71.9(2) 2_675 3_465 ?
O1 Dy O11 77.1(2) 3_465 3_465 ?
O12 Dy O11 51.8(2) 3_465 3_465 ?
O12 Dy O11 73.0(2) 2_675 3_465 ?
O12 Dy O11 127.3(2) . 3_465 ?
O11 Dy O11 117.75(8) . 3_465 ?
O11 Dy O11 117.75(8) 2_675 3_465 ?
O1 Dy N11 78.9(2) . . ?
O1 Dy N11 159.2(2) 2_675 . ?
O1 Dy N11 97.6(2) 3_465 . ?
O12 Dy N11 76.4(2) 3_465 . ?
O12 Dy N11 104.5(2) 2_675 . ?
O12 Dy N11 26.1(2) . . ?
O11 Dy N11 25.8(2) . . ?
O11 Dy N11 94.8(2) 2_675 . ?
O11 Dy N11 128.1(2) 3_465 . ?
O1 Dy N11 97.6(2) . 2_675 ?
O1 Dy N11 78.9(2) 2_675 2_675 ?
O1 Dy N11 159.2(2) 3_465 2_675 ?
O12 Dy N11 104.5(2) 3_465 2_675 ?
O12 Dy N11 26.1(2) 2_675 2_675 ?
O12 Dy N11 76.4(2) . 2_675 ?
O11 Dy N11 128.1(2) . 2_675 ?
O11 Dy N11 25.8(2) 2_675 2_675 ?
O11 Dy N11 94.8(2) 3_465 2_675 ?
N11 Dy N11 102.3(2) . 2_675 ?
O1 Dy N11 159.2(2) . 3_465 ?
O1 Dy N11 97.6(2) 2_675 3_465 ?
O1 Dy N11 78.9(2) 3_465 3_465 ?
O12 Dy N11 26.1(2) 3_465 3_465 ?
O12 Dy N11 76.4(2) 2_675 3_465 ?
O12 Dy N11 104.5(2) . 3_465 ?
O11 Dy N11 94.8(2) . 3_465 ?
O11 Dy N11 128.1(2) 2_675 3_465 ?
O11 Dy N11 25.8(2) 3_465 3_465 ?
N11 Dy N11 102.3(2) . 3_465 ?
N11 Dy N11 102.3(2) 2_675 3_465 ?
N2 Co N2 91.4(3) 3_465 . ?
N2 Co N2 91.4(3) 3_465 2_675 ?
N2 Co N2 91.4(3) . 2_675 ?
N2 Co N1 172.5(3) 3_465 2_675 ?
N2 Co N1 92.3(3) . 2_675 ?
N2 Co N1 82.0(3) 2_675 2_675 ?
N2 Co N1 82.0(3) 3_465 3_465 ?
N2 Co N1 172.5(3) . 3_465 ?
N2 Co N1 92.3(3) 2_675 3_465 ?
N1 Co N1 94.7(3) 2_675 3_465 ?
N2 Co N1 92.3(3) 3_465 . ?
N2 Co N1 82.0(3) . . ?
N2 Co N1 172.5(3) 2_675 . ?
N1 Co N1 94.7(3) 2_675 . ?
N1 Co N1 94.7(3) 3_465 . ?
N2 O1 Dy 114.5(5) . . ?
C1 N1 C5 118.6(8) . . ?
C1 N1 Co 128.5(6) . . ?
C5 N1 Co 112.9(6) . . ?
C6 N2 O1 120.1(7) . . ?
C6 N2 Co 118.2(6) . . ?
O1 N2 Co 121.6(5) . . ?
N1 C1 C2 122.5(9) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C1 C2 C3 118.5(10) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 120.4(10) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 118.4(10) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
N1 C5 C4 121.7(9) . . ?
N1 C5 C6 114.2(8) . . ?
C4 C5 C6 124.1(8) . . ?
N2 C6 C5 112.5(8) . . ?
N2 C6 C7 123.6(9) . . ?
C5 C6 C7 123.8(8) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O13 N11 O11 123.0(9) . . ?
O13 N11 O12 121.2(9) . . ?
O11 N11 O12 115.8(8) . . ?
O13 N11 Dy 173.8(6) . . ?
O11 N11 Dy 59.5(4) . . ?
O12 N11 Dy 56.6(4) . . ?
N11 O11 Dy 94.7(5) . . ?
N11 O12 Dy 97.3(5) . . ?

_refine_diff_density_max         1.519
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.102

_shelxl_version_number           2014/6

# start Validation Reply Form
_vrf_PLAT090_shelxl              
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.64 Note  
RESPONSE: This is most probably a false alert; the actual data / parameter
ratio is larger than 10.
;
_vrf_PLAT973_shelxl              
;
PROBLEM: Check Calcd Positive Residual Density on      Dy       1.73 eA-3  
RESPONSE: The high value for the residual density close to Dy atom should 
result from absorption correction effects. We have tried to determine the
shape of the crystal as accurate as possible. Due to their small size it
is possible that it has not been defined accurately. The data used for 
the final refinement are the best among several attempts.
;
# end Validation Reply Form

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

data_shelxl_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1415101'
_audit_update_record             
;
2016-10-19 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H27 Co Dy N9 O12'
_chemical_formula_weight         999.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c :H'
_space_group_name_Hall           'R 3 -2"c'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-y, -x, z+1/2'
'-x+y, -x, z'
'x, x-y, z+1/2'
'-x+y, y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, -x+1/3, z+1/3'
'x+2/3, x-y+1/3, z+5/6'
'-x+y+2/3, 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'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, -x+2/3, z+2/3'
'x+1/3, x-y+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'

_cell_length_a                   11.2364(2)
_cell_length_b                   11.2364(2)
_cell_length_c                   55.6273(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6082.4(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    31250
_cell_measurement_theta_min      7.16
_cell_measurement_theta_max      71.96

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_F_000             2970
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    13.570
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.167
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30781
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_theta_min         7.831
_diffrn_reflns_theta_max         64.916
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.901
_reflns_number_total             2228
_reflns_number_gt                2145
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_max     0.933
_reflns_Friedel_fraction_full    0.872

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0806P)²+4.3217P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 989 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2228
_refine_ls_number_parameters     178
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1145
_refine_ls_wR_factor_gt          0.1126
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.3333 0.6667 0.89757(5) 0.0204(5) Uani 1 3 d S T P . .
Dy Dy 0.3333 0.6667 0.82903(3) 0.0225(3) Uani 1 3 d S T P . .
O1 O 0.4060(5) 0.8424(6) 0.85740(11) 0.0258(12) Uani 1 1 d . . . . .
N1 N 0.2096(5) 0.7042(5) 0.91661(10) 0.0255(10) Uani 1 1 d . . . . .
N2 N 0.3446(4) 0.8120(4) 0.87837(10) 0.0245(10) Uani 1 1 d . . . . .
C1 C 0.1339(6) 0.6371(7) 0.93616(12) 0.0345(13) Uani 1 1 d . . . . .
H1 H 0.1350 0.5576 0.9417 0.045 Uiso 1 1 calc R U . . .
C2 C 0.0562(7) 0.6800(7) 0.94813(14) 0.0405(15) Uani 1 1 d . . . . .
H2 H 0.0051 0.6317 0.9619 0.053 Uiso 1 1 calc R U . . .
C3 C 0.0521(6) 0.7937(7) 0.94007(13) 0.0407(16) Uani 1 1 d . . . . .
H3 H -0.0045 0.8223 0.9479 0.053 Uiso 1 1 calc R U . . .
C4 C 0.1298(7) 0.8653(7) 0.92073(19) 0.034(2) Uani 1 1 d . . . . .
H4 H 0.1295 0.9453 0.9153 0.044 Uiso 1 1 calc R U . . .
C5 C 0.2096(7) 0.8198(7) 0.90902(16) 0.0265(16) Uani 1 1 d . . . . .
C6 C 0.2913(6) 0.8824(6) 0.88744(11) 0.0260(11) Uani 1 1 d . . . . .
C7 C 0.3111(7) 1.0133(6) 0.87754(12) 0.0323(14) Uani 1 1 d . . . . .
C8 C 0.2621(10) 1.0217(8) 0.85515(15) 0.053(2) Uani 1 1 d . . . . .
H8 H 0.2153 0.9419 0.8454 0.070 Uiso 1 1 calc R U . . .
C9 C 0.281(2) 1.1465(12) 0.8470(3) 0.072(5) Uani 1 1 d . . . . .
H9 H 0.2500 1.1525 0.8314 0.093 Uiso 1 1 calc R U . . .
C10 C 0.3454(12) 1.2612(8) 0.86110(18) 0.065(2) Uani 1 1 d . . . . .
H10 H 0.3549 1.3457 0.8557 0.084 Uiso 1 1 calc R U . . .
C11 C 0.3956(10) 1.2539(8) 0.88314(19) 0.055(2) Uani 1 1 d . . . . .
H11 H 0.4434 1.3346 0.8926 0.071 Uiso 1 1 calc R U . . .
C12 C 0.3775(9) 1.1303(8) 0.89180(17) 0.0430(19) Uani 1 1 d . . . . .
H12 H 0.4102 1.1255 0.9073 0.056 Uiso 1 1 calc R U . . .
N11 N 0.3372(6) 0.4430(6) 0.80393(12) 0.0443(14) Uani 1 1 d . . . . .
O11 O 0.2544(6) 0.4236(5) 0.82015(10) 0.0405(11) Uani 1 1 d . . . . .
O12 O 0.4200(7) 0.5704(7) 0.7991(2) 0.076(4) Uani 1 1 d . . . . .
O13 O 0.3388(6) 0.3522(6) 0.79254(13) 0.0686(18) 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
Co N2 1.902(5) 2_665 ?
Co N2 1.902(5) 4_565 ?
Co N2 1.902(5) . ?
Co N1 1.954(5) 4_565 ?
Co N1 1.954(5) 2_665 ?
Co N1 1.954(5) . ?
Dy O1 2.333(6) . ?
Dy O1 2.333(6) 4_565 ?
Dy O1 2.333(6) 2_665 ?
Dy O12 2.436(9) . ?
Dy O12 2.436(9) 4_565 ?
Dy O12 2.436(9) 2_665 ?
Dy O11 2.463(5) . ?
Dy O11 2.463(5) 4_565 ?
Dy O11 2.463(5) 2_665 ?
Dy N11 2.894(6) 4_565 ?
Dy N11 2.894(6) 2_665 ?
Dy N11 2.894(6) . ?
O1 N2 1.311(8) . ?
N1 C1 1.354(8) . ?
N1 C5 1.366(9) . ?
N2 C6 1.308(7) . ?
C1 C2 1.364(9) . ?
C1 H1 0.9500 . ?
C2 C3 1.376(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.365(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.396(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.461(10) . ?
C6 C7 1.480(8) . ?
C7 C8 1.384(10) . ?
C7 C12 1.390(10) . ?
C8 C9 1.385(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.367(16) . ?
C9 H9 0.9500 . ?
C10 C11 1.369(14) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(14) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
N11 O13 1.209(8) . ?
N11 O11 1.235(8) . ?
N11 O12 1.286(9) . ?

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
N2 Co N2 91.5(3) 2_665 4_565 ?
N2 Co N2 91.5(3) 2_665 . ?
N2 Co N2 91.5(3) 4_565 . ?
N2 Co N1 172.50(19) 2_665 4_565 ?
N2 Co N1 82.4(2) 4_565 4_565 ?
N2 Co N1 93.07(19) . 4_565 ?
N2 Co N1 82.4(2) 2_665 2_665 ?
N2 Co N1 93.06(19) 4_565 2_665 ?
N2 Co N1 172.5(2) . 2_665 ?
N1 Co N1 93.4(3) 4_565 2_665 ?
N2 Co N1 93.07(19) 2_665 . ?
N2 Co N1 172.5(2) 4_565 . ?
N2 Co N1 82.42(19) . . ?
N1 Co N1 93.4(3) 4_565 . ?
N1 Co N1 93.4(3) 2_665 . ?
O1 Dy O1 79.2(2) . 4_565 ?
O1 Dy O1 79.2(2) . 2_665 ?
O1 Dy O1 79.2(2) 4_565 2_665 ?
O1 Dy O12 142.08(19) . . ?
O1 Dy O12 85.9(4) 4_565 . ?
O1 Dy O12 131.9(2) 2_665 . ?
O1 Dy O12 131.9(2) . 4_565 ?
O1 Dy O12 142.08(19) 4_565 4_565 ?
O1 Dy O12 85.9(4) 2_665 4_565 ?
O12 Dy O12 78.6(5) . 4_565 ?
O1 Dy O12 85.9(4) . 2_665 ?
O1 Dy O12 131.9(2) 4_565 2_665 ?
O1 Dy O12 142.08(19) 2_665 2_665 ?
O12 Dy O12 78.6(5) . 2_665 ?
O12 Dy O12 78.6(5) 4_565 2_665 ?
O1 Dy O11 148.6(2) . . ?
O1 Dy O11 73.39(18) 4_565 . ?
O1 Dy O11 80.75(19) 2_665 . ?
O12 Dy O11 51.2(2) . . ?
O12 Dy O11 69.88(18) 4_565 . ?
O12 Dy O11 124.1(4) 2_665 . ?
O1 Dy O11 80.74(18) . 4_565 ?
O1 Dy O11 148.6(2) 4_565 4_565 ?
O1 Dy O11 73.39(18) 2_665 4_565 ?
O12 Dy O11 124.1(4) . 4_565 ?
O12 Dy O11 51.2(2) 4_565 4_565 ?
O12 Dy O11 69.88(18) 2_665 4_565 ?
O11 Dy O11 116.09(9) . 4_565 ?
O1 Dy O11 73.39(18) . 2_665 ?
O1 Dy O11 80.74(19) 4_565 2_665 ?
O1 Dy O11 148.6(2) 2_665 2_665 ?
O12 Dy O11 69.88(18) . 2_665 ?
O12 Dy O11 124.1(4) 4_565 2_665 ?
O12 Dy O11 51.2(2) 2_665 2_665 ?
O11 Dy O11 116.09(9) . 2_665 ?
O11 Dy O11 116.09(9) 4_565 2_665 ?
O1 Dy N11 105.78(17) . 4_565 ?
O1 Dy N11 155.54(19) 4_565 4_565 ?
O1 Dy N11 78.29(19) 2_665 4_565 ?
O12 Dy N11 102.1(3) . 4_565 ?
O12 Dy N11 26.15(19) 4_565 4_565 ?
O12 Dy N11 72.5(2) 2_665 4_565 ?
O11 Dy N11 93.49(18) . 4_565 ?
O11 Dy N11 25.04(17) 4_565 4_565 ?
O11 Dy N11 123.7(2) 2_665 4_565 ?
O1 Dy N11 78.3(2) . 2_665 ?
O1 Dy N11 105.78(18) 4_565 2_665 ?
O1 Dy N11 155.54(18) 2_665 2_665 ?
O12 Dy N11 72.5(2) . 2_665 ?
O12 Dy N11 102.1(3) 4_565 2_665 ?
O12 Dy N11 26.15(19) 2_665 2_665 ?
O11 Dy N11 123.7(2) . 2_665 ?
O11 Dy N11 93.49(18) 4_565 2_665 ?
O11 Dy N11 25.04(17) 2_665 2_665 ?
N11 Dy N11 98.67(19) 4_565 2_665 ?
O1 Dy N11 155.54(18) . . ?
O1 Dy N11 78.29(19) 4_565 . ?
O1 Dy N11 105.78(18) 2_665 . ?
O12 Dy N11 26.15(19) . . ?
O12 Dy N11 72.5(2) 4_565 . ?
O12 Dy N11 102.1(3) 2_665 . ?
O11 Dy N11 25.04(17) . . ?
O11 Dy N11 123.7(2) 4_565 . ?
O11 Dy N11 93.49(18) 2_665 . ?
N11 Dy N11 98.67(19) 4_565 . ?
N11 Dy N11 98.67(19) 2_665 . ?
N2 O1 Dy 117.8(4) . . ?
C1 N1 C5 118.7(6) . . ?
C1 N1 Co 129.1(4) . . ?
C5 N1 Co 112.1(5) . . ?
C6 N2 O1 121.8(5) . . ?
C6 N2 Co 116.6(4) . . ?
O1 N2 Co 121.6(4) . . ?
N1 C1 C2 122.0(6) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C1 C2 C3 119.6(6) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 119.7(7) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 119.4(8) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 120.6(7) . . ?
N1 C5 C6 114.4(7) . . ?
C4 C5 C6 124.9(7) . . ?
N2 C6 C5 113.2(6) . . ?
N2 C6 C7 124.8(5) . . ?
C5 C6 C7 122.0(6) . . ?
C8 C7 C12 119.5(7) . . ?
C8 C7 C6 122.4(6) . . ?
C12 C7 C6 118.1(6) . . ?
C7 C8 C9 119.9(9) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 120.5(12) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 119.8(8) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C10 C11 C12 120.9(8) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C11 C12 C7 119.3(8) . . ?
C11 C12 H12 120.3 . . ?
C7 C12 H12 120.3 . . ?
O13 N11 O11 124.2(6) . . ?
O13 N11 O12 121.5(7) . . ?
O11 N11 O12 114.2(6) . . ?
O13 N11 Dy 177.3(6) . . ?
O11 N11 Dy 57.6(3) . . ?
O12 N11 Dy 56.6(5) . . ?
N11 O11 Dy 97.4(4) . . ?
N11 O12 Dy 97.2(5) . . ?

_refine_diff_density_max         0.983
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.095

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_shelxl_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1415100'
_audit_update_record             
;
2016-10-19 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H15 Co Dy N9 O12'
_chemical_formula_weight         770.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   14.1257(3)
_cell_length_b                   14.1257(3)
_cell_length_c                   20.6905(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3575.37(17)
_cell_formula_units_Z            6
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    9611
_cell_measurement_theta_min      7.55
_cell_measurement_theta_max      71.23

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.148
_exptl_crystal_F_000             2250
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    22.812
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.289
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10087
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         7.552
_diffrn_reflns_theta_max         64.995
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.941
_reflns_number_total             1348
_reflns_number_gt                1283
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0465P)²+15.5519P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1348
_refine_ls_number_parameters     124
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0348
_refine_ls_wR_factor_ref         0.0880
_refine_ls_wR_factor_gt          0.0856
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

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
Co Co 0.0000 0.0000 0.31023(5) 0.0072(3) Uani 1 3 d S T P . .
Dy Dy 0.0000 0.0000 0.12377(2) 0.00979(17) Uani 1 3 d S T P . .
N1 N 0.0551(3) -0.0785(3) 0.36180(17) 0.0096(8) Uani 1 1 d . . . . .
N2 N -0.0559(3) -0.1276(3) 0.25818(17) 0.0100(8) Uani 1 1 d . . . . .
O1 O -0.0992(2) -0.1349(2) 0.20103(14) 0.0106(7) Uani 1 1 d . . . . .
C1 C 0.1197(4) -0.0453(4) 0.4144(2) 0.0129(10) Uani 1 1 d . . . . .
H1 H 0.1509 0.0286 0.4280 0.017 Uiso 1 1 calc R U . . .
C2 C 0.1422(4) -0.1155(4) 0.4494(2) 0.0162(10) Uani 1 1 d . . . . .
H2 H 0.1884 -0.0900 0.4863 0.021 Uiso 1 1 calc R U . . .
C3 C 0.0964(4) -0.2232(4) 0.4299(2) 0.0180(11) Uani 1 1 d . . . . .
H3 H 0.1089 -0.2732 0.4539 0.023 Uiso 1 1 calc R U . . .
C4 C 0.0324(4) -0.2572(4) 0.3752(2) 0.0153(10) Uani 1 1 d . . . . .
H4 H 0.0019 -0.3305 0.3606 0.020 Uiso 1 1 calc R U . . .
C5 C 0.0127(3) -0.1839(3) 0.3417(2) 0.0101(9) Uani 1 1 d . . . . .
C6 C -0.0486(4) -0.2085(4) 0.2821(2) 0.0139(10) Uani 1 1 d . . . . .
H6 H -0.0810 -0.2783 0.2621 0.018 Uiso 1 1 calc R U . . .
N11 N -0.2155(3) -0.1393(3) 0.07318(18) 0.0163(9) Uani 1 1 d . . . . .
O11 O -0.1961(3) -0.0594(3) 0.10913(15) 0.0175(7) Uani 1 1 d . . . . .
O12 O -0.1344(3) -0.1483(3) 0.05605(16) 0.0214(8) Uani 1 1 d . . . . .
O13 O -0.3092(3) -0.2066(3) 0.0574(2) 0.0318(9) 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
Co N2 1.900(4) . ?
Co N2 1.900(4) 3 ?
Co N2 1.900(4) 2 ?
Co N1 1.959(4) 2 ?
Co N1 1.959(4) 3 ?
Co N1 1.959(4) . ?
Dy O1 2.341(3) . ?
Dy O1 2.341(3) 2 ?
Dy O1 2.341(3) 3 ?
Dy O12 2.445(3) 3 ?
Dy O12 2.445(3) 2 ?
Dy O12 2.445(3) . ?
Dy O11 2.479(3) . ?
Dy O11 2.479(3) 3 ?
Dy O11 2.479(3) 2 ?
Dy N11 2.871(4) 3 ?
Dy N11 2.871(4) 2 ?
Dy N11 2.871(4) . ?
N1 C1 1.346(5) . ?
N1 C5 1.361(5) . ?
N2 C6 1.296(6) . ?
N2 O1 1.312(4) . ?
C1 C2 1.386(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.383(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.375(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.446(6) . ?
C6 H6 0.9500 . ?
N11 O13 1.227(5) . ?
N11 O11 1.262(5) . ?
N11 O12 1.265(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
N2 Co N2 91.02(15) . 3 ?
N2 Co N2 91.03(15) . 2 ?
N2 Co N2 91.03(15) 3 2 ?
N2 Co N1 171.66(15) . 2 ?
N2 Co N1 94.08(15) 3 2 ?
N2 Co N1 82.29(15) 2 2 ?
N2 Co N1 94.08(15) . 3 ?
N2 Co N1 82.29(15) 3 3 ?
N2 Co N1 171.66(15) 2 3 ?
N1 Co N1 93.15(14) 2 3 ?
N2 Co N1 82.30(15) . . ?
N2 Co N1 171.66(15) 3 . ?
N2 Co N1 94.08(15) 2 . ?
N1 Co N1 93.15(14) 2 . ?
N1 Co N1 93.15(14) 3 . ?
O1 Dy O1 78.48(11) . 2 ?
O1 Dy O1 78.49(11) . 3 ?
O1 Dy O1 78.48(11) 2 3 ?
O1 Dy O12 140.84(11) . 3 ?
O1 Dy O12 126.67(11) 2 3 ?
O1 Dy O12 78.56(11) 3 3 ?
O1 Dy O12 126.67(11) . 2 ?
O1 Dy O12 78.56(11) 2 2 ?
O1 Dy O12 140.84(11) 3 2 ?
O12 Dy O12 90.42(12) 3 2 ?
O1 Dy O12 78.56(11) . . ?
O1 Dy O12 140.84(11) 2 . ?
O1 Dy O12 126.67(11) 3 . ?
O12 Dy O12 90.42(12) 3 . ?
O12 Dy O12 90.42(12) 2 . ?
O1 Dy O11 72.23(10) . . ?
O1 Dy O11 143.88(10) 2 . ?
O1 Dy O11 75.39(10) 3 . ?
O12 Dy O11 71.51(11) 3 . ?
O12 Dy O11 136.44(11) 2 . ?
O12 Dy O11 51.86(11) . . ?
O1 Dy O11 143.88(10) . 3 ?
O1 Dy O11 75.39(10) 2 3 ?
O1 Dy O11 72.23(10) 3 3 ?
O12 Dy O11 51.86(11) 3 3 ?
O12 Dy O11 71.51(11) 2 3 ?
O12 Dy O11 136.44(11) . 3 ?
O11 Dy O11 118.53(3) . 3 ?
O1 Dy O11 75.39(10) . 2 ?
O1 Dy O11 72.23(10) 2 2 ?
O1 Dy O11 143.88(10) 3 2 ?
O12 Dy O11 136.44(11) 3 2 ?
O12 Dy O11 51.86(11) 2 2 ?
O12 Dy O11 71.51(11) . 2 ?
O11 Dy O11 118.53(3) . 2 ?
O11 Dy O11 118.53(3) 3 2 ?
O1 Dy N11 150.03(11) . 3 ?
O1 Dy N11 100.82(11) 2 3 ?
O1 Dy N11 72.12(10) 3 3 ?
O12 Dy N11 25.97(11) 3 3 ?
O12 Dy N11 81.61(11) 2 3 ?
O12 Dy N11 114.72(11) . 3 ?
O11 Dy N11 94.44(11) . 3 ?
O11 Dy N11 25.99(10) 3 3 ?
O11 Dy N11 133.46(10) 2 3 ?
O1 Dy N11 100.82(11) . 2 ?
O1 Dy N11 72.12(10) 2 2 ?
O1 Dy N11 150.03(11) 3 2 ?
O12 Dy N11 114.72(11) 3 2 ?
O12 Dy N11 25.97(11) 2 2 ?
O12 Dy N11 81.60(11) . 2 ?
O11 Dy N11 133.46(10) . 2 ?
O11 Dy N11 94.44(11) 3 2 ?
O11 Dy N11 25.99(10) 2 2 ?
N11 Dy N11 107.50(8) 3 2 ?
O1 Dy N11 72.12(10) . . ?
O1 Dy N11 150.03(11) 2 . ?
O1 Dy N11 100.82(11) 3 . ?
O12 Dy N11 81.61(11) 3 . ?
O12 Dy N11 114.72(11) 2 . ?
O12 Dy N11 25.97(11) . . ?
O11 Dy N11 25.99(10) . . ?
O11 Dy N11 133.46(10) 3 . ?
O11 Dy N11 94.44(11) 2 . ?
N11 Dy N11 107.50(8) 3 . ?
N11 Dy N11 107.50(8) 2 . ?
C1 N1 C5 118.6(4) . . ?
C1 N1 Co 129.5(3) . . ?
C5 N1 Co 111.7(3) . . ?
C6 N2 O1 121.0(4) . . ?
C6 N2 Co 116.2(3) . . ?
O1 N2 Co 122.8(3) . . ?
N2 O1 Dy 119.1(2) . . ?
N1 C1 C2 122.1(4) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
C4 C3 C2 119.3(4) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 119.5(4) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 121.4(4) . . ?
N1 C5 C6 114.0(4) . . ?
C4 C5 C6 124.5(4) . . ?
N2 C6 C5 114.6(4) . . ?
N2 C6 H6 122.7 . . ?
C5 C6 H6 122.7 . . ?
O13 N11 O11 121.2(4) . . ?
O13 N11 O12 121.9(4) . . ?
O11 N11 O12 116.9(4) . . ?
O13 N11 Dy 172.7(3) . . ?
O11 N11 Dy 59.4(2) . . ?
O12 N11 Dy 57.8(2) . . ?
N11 O11 Dy 94.6(3) . . ?
N11 O12 Dy 96.2(2) . . ?

_refine_diff_density_max         1.410
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.128

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1415099'
_audit_update_record             
;
2017-09-14 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H30 Co Dy N12 O15'
_chemical_formula_weight         912.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'

_cell_length_a                   16.51370(10)
_cell_length_b                   16.51370(10)
_cell_length_c                   20.9946(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4958.23(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    36323
_cell_measurement_theta_min      6.54
_cell_measurement_theta_max      71.98

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_F_000             1812
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    11.104
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48920
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         6.822
_diffrn_reflns_theta_max         64.981
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.940
_reflns_number_total             2819
_reflns_number_gt                2431
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0445P)²+3.1629P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2819
_refine_ls_number_parameters     171
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0309
_refine_ls_wR_factor_ref         0.0891
_refine_ls_wR_factor_gt          0.0866
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.6667 0.3333 0.05616(3) 0.01550(19) Uani 1 3 d S T P . .
Dy Dy 0.6667 0.3333 -0.12365(2) 0.01865(12) Uani 1 3 d S T P . .
O1 O 0.54349(14) 0.26847(12) -0.05240(8) 0.0203(4) Uani 1 1 d . . . . .
N1 N 0.63423(15) 0.22094(16) 0.10525(10) 0.0184(5) Uani 1 1 d . . . . .
N2 N 0.56625(14) 0.24699(15) 0.00516(9) 0.0184(5) Uani 1 1 d . . . . .
N3 N 0.45280(17) 0.09099(16) -0.01074(10) 0.0299(6) Uani 1 1 d . . . . .
H3A H 0.4353 0.1037 -0.0472 0.036 Uiso 1 1 calc R U . . .
H3B H 0.4251 0.0332 0.0036 0.036 Uiso 1 1 calc R U . . .
C1 C 0.6756(2) 0.2133(2) 0.15786(12) 0.0234(6) Uani 1 1 d . . . . .
C2 C 0.6434(2) 0.1292(2) 0.18941(13) 0.0299(7) Uani 1 1 d . . . . .
C3 C 0.5648(2) 0.0507(2) 0.16689(14) 0.0336(7) Uani 1 1 d . . . . .
C4 C 0.5203(2) 0.0574(2) 0.11267(14) 0.0273(7) Uani 1 1 d . . . . .
C5 C 0.55737(18) 0.1433(2) 0.08264(12) 0.0197(6) Uani 1 1 d . . . . .
C6 C 0.52182(18) 0.15982(18) 0.02304(11) 0.0198(6) Uani 1 1 d . . . . .
N11 N 0.82723(18) 0.48080(17) -0.18964(11) 0.0338(6) Uani 1 1 d . . . . .
O11 O 0.83705(15) 0.43401(14) -0.14620(9) 0.0304(5) Uani 1 1 d . . . . .
O12 O 0.74327(16) 0.45934(19) -0.20171(11) 0.0435(6) Uani 1 1 d . . . . .
O13 O 0.89285(17) 0.54242(18) -0.21818(13) 0.0633(8) Uani 1 1 d . . . . .
O1M O 0.41272(18) 0.31847(16) -0.02649(12) 0.0467(6) Uani 1 1 d . . . . .
C1M C 0.3473(3) 0.2421(3) 0.0097(2) 0.0745(13) Uani 1 1 d . . . . .
H1MA H 0.3783 0.2354 0.0465 0.097 Uiso 1 1 d . U . . .
H1MB H 0.3233 0.1864 -0.0159 0.097 Uiso 1 1 d . U . . .
H1MC H 0.2979 0.2521 0.0225 0.097 Uiso 1 1 d . U . . .
H1 H 0.727(2) 0.266(2) 0.1736(15) 0.026(9) Uiso 1 1 d . . . . .
H2 H 0.681(2) 0.125(2) 0.2241(15) 0.043(9) Uiso 1 1 d . . . . .
H3 H 0.537(2) -0.008(2) 0.1874(14) 0.041(9) Uiso 1 1 d . . . . .
H4 H 0.463(2) 0.008(2) 0.0978(12) 0.024(7) Uiso 1 1 d . . . . .
H1OM H 0.457(3) 0.306(3) -0.0319(19) 0.074(14) Uiso 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
Co N2 1.888(2) 2_655 ?
Co N2 1.888(2) 3_665 ?
Co N2 1.888(2) . ?
Co N1 1.949(2) . ?
Co N1 1.949(2) 2_655 ?
Co N1 1.949(2) 3_665 ?
Dy O1 2.3116(19) 3_665 ?
Dy O1 2.3116(19) . ?
Dy O1 2.3117(19) 2_655 ?
Dy O12 2.446(2) 3_665 ?
Dy O12 2.446(2) 2_655 ?
Dy O12 2.446(2) . ?
Dy O11 2.495(2) . ?
Dy O11 2.495(2) 3_665 ?
Dy O11 2.495(2) 2_655 ?
Dy N11 2.902(2) 3_665 ?
Dy N11 2.902(2) 2_655 ?
Dy N11 2.902(2) . ?
O1 N2 1.364(3) . ?
N1 C1 1.338(3) . ?
N1 C5 1.362(4) . ?
N2 C6 1.302(3) . ?
N3 C6 1.341(3) . ?
N3 H3A 0.8800 . ?
N3 H3B 0.8800 . ?
C1 C2 1.383(4) . ?
C1 H1 0.92(3) . ?
C2 C3 1.381(4) . ?
C2 H2 0.98(3) . ?
C3 C4 1.389(4) . ?
C3 H3 0.94(3) . ?
C4 C5 1.384(4) . ?
C4 H4 0.94(3) . ?
C5 C6 1.465(3) . ?
N11 O13 1.211(3) . ?
N11 O11 1.257(3) . ?
N11 O12 1.273(3) . ?
O1M C1M 1.404(4) . ?
O1M H1OM 0.86(4) . ?
C1M H1MA 0.9630 . ?
C1M H1MB 0.9622 . ?
C1M H1MC 0.9490 . ?

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
N2 Co N2 91.01(9) 2_655 3_665 ?
N2 Co N2 91.01(9) 2_655 . ?
N2 Co N2 91.01(9) 3_665 . ?
N2 Co N1 92.73(9) 2_655 . ?
N2 Co N1 172.15(9) 3_665 . ?
N2 Co N1 82.03(9) . . ?
N2 Co N1 82.03(9) 2_655 2_655 ?
N2 Co N1 92.73(9) 3_665 2_655 ?
N2 Co N1 172.15(9) . 2_655 ?
N1 Co N1 94.63(9) . 2_655 ?
N2 Co N1 172.15(9) 2_655 3_665 ?
N2 Co N1 82.03(9) 3_665 3_665 ?
N2 Co N1 92.73(9) . 3_665 ?
N1 Co N1 94.63(9) . 3_665 ?
N1 Co N1 94.63(9) 2_655 3_665 ?
O1 Dy O1 82.65(7) 3_665 . ?
O1 Dy O1 82.64(7) 3_665 2_655 ?
O1 Dy O1 82.65(7) . 2_655 ?
O1 Dy O12 142.05(7) 3_665 3_665 ?
O1 Dy O12 129.62(7) . 3_665 ?
O1 Dy O12 82.77(8) 2_655 3_665 ?
O1 Dy O12 129.62(7) 3_665 2_655 ?
O1 Dy O12 82.77(8) . 2_655 ?
O1 Dy O12 142.05(7) 2_655 2_655 ?
O12 Dy O12 80.02(10) 3_665 2_655 ?
O1 Dy O12 82.77(8) 3_665 . ?
O1 Dy O12 142.06(7) . . ?
O1 Dy O12 129.62(7) 2_655 . ?
O12 Dy O12 80.02(10) 3_665 . ?
O12 Dy O12 80.02(10) 2_655 . ?
O1 Dy O11 72.64(6) 3_665 . ?
O1 Dy O11 150.38(7) . . ?
O1 Dy O11 78.31(6) 2_655 . ?
O12 Dy O11 70.18(7) 3_665 . ?
O12 Dy O11 125.65(8) 2_655 . ?
O12 Dy O11 51.31(7) . . ?
O1 Dy O11 150.38(7) 3_665 3_665 ?
O1 Dy O11 78.31(6) . 3_665 ?
O1 Dy O11 72.64(6) 2_655 3_665 ?
O12 Dy O11 51.31(7) 3_665 3_665 ?
O12 Dy O11 70.18(7) 2_655 3_665 ?
O12 Dy O11 125.65(8) . 3_665 ?
O11 Dy O11 116.49(3) . 3_665 ?
O1 Dy O11 78.31(6) 3_665 2_655 ?
O1 Dy O11 72.64(6) . 2_655 ?
O1 Dy O11 150.38(7) 2_655 2_655 ?
O12 Dy O11 125.65(8) 3_665 2_655 ?
O12 Dy O11 51.31(7) 2_655 2_655 ?
O12 Dy O11 70.18(7) . 2_655 ?
O11 Dy O11 116.49(3) . 2_655 ?
O11 Dy O11 116.49(3) 3_665 2_655 ?
O1 Dy N11 157.03(6) 3_665 3_665 ?
O1 Dy N11 103.84(7) . 3_665 ?
O1 Dy N11 76.50(6) 2_655 3_665 ?
O12 Dy N11 25.78(7) 3_665 3_665 ?
O12 Dy N11 73.33(7) 2_655 3_665 ?
O12 Dy N11 103.18(8) . 3_665 ?
O11 Dy N11 93.57(7) . 3_665 ?
O11 Dy N11 25.54(6) 3_665 3_665 ?
O11 Dy N11 124.64(7) 2_655 3_665 ?
O1 Dy N11 103.84(7) 3_665 2_655 ?
O1 Dy N11 76.50(6) . 2_655 ?
O1 Dy N11 157.04(6) 2_655 2_655 ?
O12 Dy N11 103.18(8) 3_665 2_655 ?
O12 Dy N11 25.78(7) 2_655 2_655 ?
O12 Dy N11 73.33(7) . 2_655 ?
O11 Dy N11 124.64(7) . 2_655 ?
O11 Dy N11 93.57(7) 3_665 2_655 ?
O11 Dy N11 25.54(6) 2_655 2_655 ?
N11 Dy N11 99.10(6) 3_665 2_655 ?
O1 Dy N11 76.50(6) 3_665 . ?
O1 Dy N11 157.04(6) . . ?
O1 Dy N11 103.84(7) 2_655 . ?
O12 Dy N11 73.33(7) 3_665 . ?
O12 Dy N11 103.18(8) 2_655 . ?
O12 Dy N11 25.78(6) . . ?
O11 Dy N11 25.53(6) . . ?
O11 Dy N11 124.64(7) 3_665 . ?
O11 Dy N11 93.57(7) 2_655 . ?
N11 Dy N11 99.10(6) 3_665 . ?
N11 Dy N11 99.10(6) 2_655 . ?
N2 O1 Dy 113.62(14) . . ?
C1 N1 C5 118.6(2) . . ?
C1 N1 Co 128.1(2) . . ?
C5 N1 Co 113.31(17) . . ?
C6 N2 O1 117.8(2) . . ?
C6 N2 Co 117.91(17) . . ?
O1 N2 Co 123.93(16) . . ?
C6 N3 H3A 120.0 . . ?
C6 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
N1 C1 C2 122.2(3) . . ?
N1 C1 H1 119(2) . . ?
C2 C1 H1 119(2) . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2 121.5(18) . . ?
C1 C2 H2 118.9(19) . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 H3 123.3(19) . . ?
C4 C3 H3 117(2) . . ?
C5 C4 C3 118.4(3) . . ?
C5 C4 H4 118.7(16) . . ?
C3 C4 H4 122.7(16) . . ?
N1 C5 C4 122.2(2) . . ?
N1 C5 C6 113.2(2) . . ?
C4 C5 C6 124.6(3) . . ?
N2 C6 N3 123.7(2) . . ?
N2 C6 C5 113.3(2) . . ?
N3 C6 C5 122.9(2) . . ?
O13 N11 O11 122.6(3) . . ?
O13 N11 O12 121.9(3) . . ?
O11 N11 O12 115.5(2) . . ?
O13 N11 Dy 178.5(2) . . ?
O11 N11 Dy 58.83(14) . . ?
O12 N11 Dy 56.67(14) . . ?
N11 O11 Dy 95.63(16) . . ?
N11 O12 Dy 97.55(16) . . ?
C1M O1M H1OM 103(3) . . ?
O1M C1M H1MA 108.9 . . ?
O1M C1M H1MB 108.8 . . ?
H1MA C1M H1MB 109.0 . . ?
O1M C1M H1MC 109.7 . . ?
H1MA C1M H1MC 110.2 . . ?
H1MB C1M H1MC 110.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1M H1OM O1 0.86(4) 1.87(4) 2.725(3) 172(4) .
N3 H3B O1M 0.88 2.01 2.847(3) 157.6 8
C3 H3 O11 0.94(3) 2.56(3) 3.216(4) 127(2) 9_545
C4 H4 O11 0.94(3) 2.68(3) 3.231(4) 119(2) 9_545

_refine_diff_density_max         0.539
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.065

_shelxl_version_number           2014/6

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.001 2086 372 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?


