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

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1832851'
_audit_update_record             
;
2018-03-27 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H40 N6 O4'
_chemical_formula_sum            'C26 H40 N6 O4'
_chemical_formula_weight         500.64

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.6859(9)
_cell_length_b                   14.9050(11)
_cell_length_c                   14.1864(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.431(2)
_cell_angle_gamma                90
_cell_volume                     2674.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3307
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      25.6

_exptl_crystal_description       block
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_F_000             1080
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.085
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7088
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_special_details           
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker smart diffractometer equiped with an APEX II CCD Detector,
a graphite monochromator. The crystal-to-detector distance was 
5.0 cm, and the data collection was carried out in 512 x 512 pixel mode.
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BrukerAPEX II with CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            30611
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.075
_diffrn_reflns_theta_max         26.398
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5479
_reflns_number_gt                3307
_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       'APEX2  (Bruker AXS, 2012)'
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2012)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2012)'
_computing_molecular_graphics    ' ORTEP for Windows (Farugia, 1997)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0634P)²+1.8694P] 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         5479
_refine_ls_number_parameters     450
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0618
_refine_ls_wR_factor_ref         0.1759
_refine_ls_wR_factor_gt          0.1482
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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
C1 C 0.47351(18) 0.93349(18) 0.62049(18) 0.0415(6) Uani 1 1 d . . . . .
C2 C 0.46231(18) 0.87827(19) 0.70189(18) 0.0434(6) Uani 1 1 d . . . . .
H2 H 0.439688 0.905532 0.757400 0.052 Uiso 1 1 calc R U . . .
C3 C 0.48243(17) 0.7894(2) 0.70328(18) 0.0456(7) Uani 1 1 d . . . . .
C4 C 0.51450(18) 0.74653(18) 0.61845(18) 0.0432(6) Uani 1 1 d . . . . .
C5 C 0.5375(2) 0.6551(2) 0.6118(2) 0.0572(8) Uani 1 1 d . . . . .
H5 H 0.534109 0.618072 0.665983 0.069 Uiso 1 1 calc R U . . .
C6 C 0.5648(2) 0.6179(2) 0.5290(2) 0.0595(8) Uani 1 1 d . . . . .
H6 H 0.579811 0.555544 0.525993 0.071 Uiso 1 1 calc R U . . .
C7 C 0.57051(19) 0.67145(18) 0.44890(19) 0.0474(7) Uani 1 1 d . . . . .
C8 C 0.55142(18) 0.76163(18) 0.45301(18) 0.0422(6) Uani 1 1 d . . . . .
H8 H 0.557244 0.798249 0.398844 0.051 Uiso 1 1 calc R U . . .
C9 C 0.52327(16) 0.79939(17) 0.53772(18) 0.0397(6) Uani 1 1 d . . . . .
C10 C 0.4715(2) 0.7344(2) 0.7902(2) 0.0591(8) Uani 1 1 d . . . . .
H10A H 0.489359 0.671765 0.777537 0.089 Uiso 0.5 1 calc R U P . .
H10B H 0.519459 0.757493 0.842008 0.089 Uiso 0.5 1 calc R U P . .
H10C H 0.398461 0.737773 0.807977 0.089 Uiso 0.5 1 calc R U P . .
H10D H 0.448827 0.772922 0.840812 0.089 Uiso 0.5 1 calc R U P . .
H10E H 0.418727 0.687195 0.776340 0.089 Uiso 0.5 1 calc R U P . .
H10F H 0.539725 0.706914 0.810371 0.089 Uiso 0.5 1 calc R U P . .
C12 C 0.7051(2) 0.6055(2) 0.3507(2) 0.0625(9) Uani 1 1 d . . . . .
H12A H 0.752863 0.644565 0.391060 0.075 Uiso 1 1 calc R U . . .
H12B H 0.721315 0.614712 0.284221 0.075 Uiso 1 1 calc R U . . .
C13 C 0.7260(2) 0.5083(2) 0.3777(2) 0.0580(8) Uani 1 1 d . . . . .
C14 C 0.8686(2) 0.39727(17) 0.3869(2) 0.0493(7) Uani 1 1 d . . . . .
C15 C 0.8129(3) 0.3303(2) 0.3216(3) 0.0864(12) Uani 1 1 d . . . . .
H15A H 0.841255 0.270225 0.335696 0.130 Uiso 1 1 calc R U . . .
H15B H 0.737019 0.331058 0.330523 0.130 Uiso 1 1 calc R U . . .
H15C H 0.823880 0.345910 0.255995 0.130 Uiso 1 1 calc R U . . .
C16 C 0.8597(3) 0.3751(2) 0.4888(2) 0.0863(12) Uani 1 1 d . . . . .
H16A H 0.887582 0.314701 0.501962 0.129 Uiso 1 1 calc R U . . .
H16B H 0.900340 0.418685 0.528539 0.129 Uiso 1 1 calc R U . . .
H16C H 0.785258 0.377413 0.502754 0.129 Uiso 1 1 calc R U . . .
C17 C 0.9826(3) 0.4073(2) 0.3656(3) 0.0863(12) Uani 1 1 d . . . . .
H17A H 1.019372 0.349982 0.376751 0.129 Uiso 1 1 calc R U . . .
H17B H 0.986054 0.424998 0.299407 0.129 Uiso 1 1 calc R U . . .
H17C H 1.016516 0.453374 0.406864 0.129 Uiso 1 1 calc R U . . .
C18 C 0.5194(3) 0.6015(2) 0.2952(2) 0.0675(9) Uani 1 1 d . . . . .
C19 C 0.4055(2) 0.6177(2) 0.3171(2) 0.0671(9) Uani 1 1 d . . . . .
H19A H 0.396324 0.682792 0.327542 0.081 Uiso 0.592(5) 1 calc R U P A 1
H19B H 0.393821 0.586946 0.377308 0.081 Uiso 0.592(5) 1 calc R U P A 1
H19C H 0.381065 0.571243 0.360327 0.081 Uiso 0.408(5) 1 calc R U P A 2
H19D H 0.396884 0.677638 0.345550 0.081 Uiso 0.408(5) 1 calc R U P A 2
C20A C 0.2595(3) 0.6604(3) 0.1950(3) 0.0469(13) Uani 0.592(5) 1 d . . P A 1
H20A H 0.198797 0.635782 0.155136 0.056 Uiso 0.592(5) 1 calc R U P A 1
H20B H 0.231592 0.700268 0.242989 0.056 Uiso 0.592(5) 1 calc R U P A 1
C21A C 0.3286(10) 0.7127(9) 0.1352(9) 0.074(4) Uani 0.592(5) 1 d . . P A 1
H21A H 0.285354 0.761780 0.105327 0.088 Uiso 0.592(5) 1 calc R U P A 1
H21B H 0.384364 0.741100 0.177890 0.088 Uiso 0.592(5) 1 calc R U P A 1
C22A C 0.3076(4) 0.6408(4) -0.0183(4) 0.0629(16) Uani 0.592(5) 1 d . . P A 1
H22A H 0.291014 0.693385 -0.059428 0.075 Uiso 0.592(5) 1 calc R U P A 1
H22B H 0.240703 0.618928 0.004981 0.075 Uiso 0.592(5) 1 calc R U P A 1
C23A C 0.3550(11) 0.5680(6) -0.0753(10) 0.061(3) Uani 0.592(5) 1 d . . P A 1
H23A H 0.305848 0.553950 -0.131039 0.073 Uiso 0.592(5) 1 calc R U P A 1
H23B H 0.421894 0.589936 -0.098599 0.073 Uiso 0.592(5) 1 calc R U P A 1
C24A C 0.2839(7) 0.4281(5) -0.0181(6) 0.0639(19) Uani 0.592(5) 1 d . . P A 1
H24A H 0.220202 0.465237 -0.011459 0.077 Uiso 0.592(5) 1 calc R U P A 1
H24B H 0.273602 0.395708 -0.079064 0.077 Uiso 0.592(5) 1 calc R U P A 1
C25A C 0.2925(10) 0.3639(6) 0.0567(9) 0.063(4) Uani 0.592(5) 1 d . . P A 1
H25A H 0.349544 0.320689 0.045634 0.075 Uiso 0.592(5) 1 calc R U P A 1
H25B H 0.225439 0.330023 0.057427 0.075 Uiso 0.592(5) 1 calc R U P A 1
C26A C 0.2223(5) 0.4505(4) 0.1882(4) 0.0558(15) Uani 0.592(5) 1 d . . P A 1
H26A H 0.174110 0.402338 0.206288 0.067 Uiso 0.592(5) 1 calc R U P A 1
H26B H 0.185275 0.485806 0.136581 0.067 Uiso 0.592(5) 1 calc R U P A 1
C27A C 0.2495(12) 0.5113(14) 0.2729(11) 0.064(5) Uani 0.592(5) 1 d . . P A 1
H27A H 0.184043 0.536115 0.296302 0.077 Uiso 0.592(5) 1 calc R U P A 1
H27B H 0.287147 0.476612 0.324688 0.077 Uiso 0.592(5) 1 calc R U P A 1
N10A N 0.3192(5) 0.5867(5) 0.2422(4) 0.0401(13) Uani 0.592(5) 1 d . . P A 1
N11 N 0.3796(5) 0.6682(4) 0.0622(4) 0.0555(14) Uani 0.592(5) 1 d . . P A 1
H11 H 0.448116 0.658165 0.065330 0.067 Uiso 0.592(5) 1 calc R U P A 1
N12A N 0.3756(3) 0.4876(3) -0.0212(3) 0.0456(12) Uani 0.592(5) 1 d . . P A 1
N13 N 0.3173(4) 0.4107(3) 0.1547(4) 0.0488(12) Uani 0.592(5) 1 d . . P A 1
N1 N 0.50358(15) 0.89013(14) 0.54227(15) 0.0416(5) Uani 1 1 d . . . . .
H0 H 0.510909 0.922319 0.491186 0.050 Uiso 1 1 calc R U . . .
N2 N 0.59576(18) 0.63174(16) 0.36108(17) 0.0543(6) Uani 1 1 d . . . . .
O0 O 0.45891(14) 1.01613(13) 0.61872(13) 0.0498(5) Uani 1 1 d . . . . .
O2 O 0.5436(2) 0.5634(2) 0.22424(18) 0.1013(10) Uani 1 1 d . . . . .
O3 O 0.66267(18) 0.45810(15) 0.4066(2) 0.0960(9) Uani 1 1 d . . . . .
O4 O 0.82652(13) 0.48867(12) 0.36651(13) 0.0506(5) Uani 1 1 d . . . . .
C28B C 0.2461(7) 0.5804(5) 0.2485(5) 0.0384(17) Uani 0.408(5) 1 d . . P A 2
H28A H 0.221241 0.613476 0.303160 0.046 Uiso 0.408(5) 1 calc R U P A 2
H28B H 0.196252 0.592761 0.192826 0.046 Uiso 0.408(5) 1 calc R U P A 2
N12B N 0.3479(6) 0.4193(7) 0.0182(5) 0.063(2) Uani 0.408(5) 1 d . . P A 2
C24B C 0.2978(8) 0.4862(12) -0.0448(7) 0.095(5) Uani 0.408(5) 1 d . . P A 2
H24C H 0.231455 0.506654 -0.019136 0.114 Uiso 0.408(5) 1 calc R U P A 2
H24D H 0.279295 0.458721 -0.107390 0.114 Uiso 0.408(5) 1 calc R U P A 2
N10B N 0.3528(7) 0.6120(6) 0.2297(8) 0.040(2) Uani 0.408(5) 1 d . . P A 2
N11B N 0.4042(5) 0.6129(7) 0.0322(7) 0.070(3) Uani 0.408(5) 1 d . . P A 2
N13B N 0.2904(5) 0.4213(4) 0.2094(6) 0.0468(18) Uani 0.408(5) 1 d . . P A 2
H13B H 0.354610 0.398966 0.218386 0.056 Uiso 0.408(5) 1 calc R U P A 2
C21B C 0.3445(18) 0.6949(14) 0.1754(14) 0.100(8) Uani 0.408(5) 1 d . . P A 2
H21C H 0.411388 0.729243 0.184423 0.120 Uiso 0.408(5) 1 calc R U P A 2
H21D H 0.286660 0.732563 0.196781 0.120 Uiso 0.408(5) 1 calc R U P A 2
C22B C 0.3216(9) 0.6702(10) 0.0698(11) 0.089(5) Uani 0.408(5) 1 d . . P A 2
H22C H 0.252976 0.638400 0.061796 0.107 Uiso 0.408(5) 1 calc R U P A 2
H22D H 0.315056 0.726075 0.032144 0.107 Uiso 0.408(5) 1 calc R U P A 2
C25B C 0.2765(16) 0.3640(15) 0.0659(16) 0.110(9) Uani 0.408(5) 1 d . . P A 2
H25C H 0.228818 0.335322 0.016204 0.132 Uiso 0.408(5) 1 calc R U P A 2
H25D H 0.319372 0.315380 0.097057 0.132 Uiso 0.408(5) 1 calc R U P A 2
C26B C 0.2142(5) 0.3970(5) 0.1315(6) 0.052(2) Uani 0.408(5) 1 d . . P A 2
H26C H 0.164076 0.350934 0.151085 0.062 Uiso 0.408(5) 1 calc R U P A 2
H26D H 0.173849 0.450111 0.107068 0.062 Uiso 0.408(5) 1 calc R U P A 2
C27B C 0.2474(13) 0.4852(19) 0.2684(19) 0.058(6) Uani 0.408(5) 1 d . . P A 2
H27C H 0.284742 0.477792 0.331827 0.070 Uiso 0.408(5) 1 calc R U P A 2
H27D H 0.173046 0.467311 0.274399 0.070 Uiso 0.408(5) 1 calc R U P A 2
C23B C 0.3708(16) 0.568(2) -0.0567(17) 0.124(11) Uani 0.408(5) 1 d . . P A 2
H23C H 0.434395 0.547997 -0.087103 0.149 Uiso 0.408(5) 1 calc R U P A 2
H23D H 0.333128 0.611980 -0.099556 0.149 Uiso 0.408(5) 1 calc R U P A 2
HN3A H 0.360(3) 0.459(3) 0.159(3) 0.031(12) Uiso 0.592(5) 1 d . . P A 1
HN2A H 0.427(5) 0.458(4) -0.044(4) 0.079(19) Uiso 0.592(5) 1 d . . P A 1
H1B H 0.418(5) 0.577(5) 0.091(5) 0.049(19) Uiso 0.408(5) 1 d . . P A 2
H2B H 0.399(7) 0.372(6) -0.001(6) 0.08(3) Uiso 0.408(5) 1 d . . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O0 1.246(3) . ?
C1 N1 1.364(3) . ?
C1 C2 1.434(4) . ?
C2 C3 1.349(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.448(4) . ?
C3 C10 1.496(4) . ?
C4 C5 1.398(4) . ?
C4 C9 1.402(3) . ?
C5 C6 1.368(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.395(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.368(4) . ?
C7 N2 1.438(4) . ?
C8 C9 1.398(4) . ?
C8 H8 0.9500 . ?
C9 N1 1.378(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 H10D 0.9800 . ?
C10 H10E 0.9800 . ?
C10 H10F 0.9800 . ?
C12 N2 1.460(3) . ?
C12 C13 1.517(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 O3 1.194(3) . ?
C13 O4 1.330(3) . ?
C14 O4 1.484(3) . ?
C14 C16 1.496(4) . ?
C14 C15 1.501(4) . ?
C14 C17 1.507(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O2 1.215(4) . ?
C18 N2 1.370(4) . ?
C18 C19 1.521(4) . ?
C19 N10B 1.365(11) . ?
C19 N10A 1.537(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 H19C 0.9900 . ?
C19 H19D 0.9900 . ?
C20A C21A 1.487(13) . ?
C20A N10A 1.466(8) . ?
C20A H20A 0.9900 . ?
C20A H20B 0.9900 . ?
C21A N11 1.426(13) . ?
C21A H21A 0.9900 . ?
C21A H21B 0.9900 . ?
C22A N11 1.465(9) . ?
C22A C23A 1.506(12) . ?
C22A H22A 0.9900 . ?
C22A H22B 0.9900 . ?
C23A N12A 1.437(13) . ?
C23A H23A 0.9900 . ?
C23A H23B 0.9900 . ?
C24A C25A 1.428(14) . ?
C24A N12A 1.466(10) . ?
C24A H24A 0.9900 . ?
C24A H24B 0.9900 . ?
C25A N13 1.565(12) . ?
C25A H25A 0.9900 . ?
C25A H25B 0.9900 . ?
C26A N13 1.455(7) . ?
C26A C27A 1.523(18) . ?
C26A H26A 0.9900 . ?
C26A H26B 0.9900 . ?
C27A N10A 1.515(17) . ?
C27A H27A 0.9900 . ?
C27A H27B 0.9900 . ?
N11 H11 0.8800 . ?
N12A HN2A 0.87(7) . ?
N13 HN3A 0.91(4) . ?
N1 H0 0.8800 . ?
C28B C27B 1.45(3) . ?
C28B N10B 1.478(9) . ?
C28B H28A 0.9900 . ?
C28B H28B 0.9900 . ?
N12B C25B 1.43(2) . ?
N12B C24B 1.453(16) . ?
N12B H2B 1.00(9) . ?
C24B C23B 1.55(3) . ?
C24B H24C 0.9900 . ?
C24B H24D 0.9900 . ?
N10B C21B 1.46(2) . ?
N11B C23B 1.46(3) . ?
N11B C22B 1.483(16) . ?
N11B H1B 0.99(7) . ?
N13B C27B 1.41(3) . ?
N13B C26B 1.458(10) . ?
N13B H13B 0.8800 . ?
C21B C22B 1.55(3) . ?
C21B H21C 0.9900 . ?
C21B H21D 0.9900 . ?
C22B H22C 0.9900 . ?
C22B H22D 0.9900 . ?
C25B C26B 1.36(2) . ?
C25B H25C 0.9900 . ?
C25B H25D 0.9900 . ?
C26B H26C 0.9900 . ?
C26B H26D 0.9900 . ?
C27B H27C 0.9900 . ?
C27B H27D 0.9900 . ?
C23B H23C 0.9900 . ?
C23B H23D 0.9900 . ?

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
O0 C1 N1 120.2(2) . . ?
O0 C1 C2 124.1(2) . . ?
N1 C1 C2 115.8(2) . . ?
C3 C2 C1 123.0(3) . . ?
C3 C2 H2 118.5 . . ?
C1 C2 H2 118.5 . . ?
C2 C3 C4 119.1(2) . . ?
C2 C3 C10 121.4(3) . . ?
C4 C3 C10 119.5(3) . . ?
C5 C4 C9 117.6(3) . . ?
C5 C4 C3 124.0(2) . . ?
C9 C4 C3 118.4(2) . . ?
C6 C5 C4 121.4(3) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C7 120.0(3) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 120.5(3) . . ?
C8 C7 N2 119.6(2) . . ?
C6 C7 N2 119.9(2) . . ?
C7 C8 C9 119.3(2) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
N1 C9 C8 119.6(2) . . ?
N1 C9 C4 119.2(2) . . ?
C8 C9 C4 121.2(2) . . ?
C3 C10 H10A 109.5 . . ?
C3 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C3 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H10D C10 H10E 109.5 . . ?
H10D C10 H10F 109.5 . . ?
H10E C10 H10F 109.5 . . ?
N2 C12 C13 112.3(2) . . ?
N2 C12 H12A 109.1 . . ?
C13 C12 H12A 109.1 . . ?
N2 C12 H12B 109.1 . . ?
C13 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
O3 C13 O4 125.5(3) . . ?
O3 C13 C12 125.2(3) . . ?
O4 C13 C12 109.3(2) . . ?
O4 C14 C16 109.8(2) . . ?
O4 C14 C15 110.2(2) . . ?
C16 C14 C15 112.5(3) . . ?
O4 C14 C17 101.9(2) . . ?
C16 C14 C17 111.2(3) . . ?
C15 C14 C17 110.8(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O2 C18 N2 120.6(3) . . ?
O2 C18 C19 123.2(3) . . ?
N2 C18 C19 116.1(3) . . ?
N10B C19 C18 102.1(5) . . ?
C18 C19 N10A 116.6(3) . . ?
C18 C19 H19A 108.1 . . ?
N10A C19 H19A 108.1 . . ?
C18 C19 H19B 108.1 . . ?
N10A C19 H19B 108.1 . . ?
H19A C19 H19B 107.3 . . ?
N10B C19 H19C 111.3 . . ?
C18 C19 H19C 111.3 . . ?
N10B C19 H19D 111.3 . . ?
C18 C19 H19D 111.3 . . ?
H19C C19 H19D 109.2 . . ?
C21A C20A N10A 110.3(6) . . ?
C21A C20A H20A 109.6 . . ?
N10A C20A H20A 109.6 . . ?
C21A C20A H20B 109.6 . . ?
N10A C20A H20B 109.6 . . ?
H20A C20A H20B 108.1 . . ?
N11 C21A C20A 119.4(10) . . ?
N11 C21A H21A 107.5 . . ?
C20A C21A H21A 107.5 . . ?
N11 C21A H21B 107.5 . . ?
C20A C21A H21B 107.5 . . ?
H21A C21A H21B 107.0 . . ?
N11 C22A C23A 111.7(7) . . ?
N11 C22A H22A 109.3 . . ?
C23A C22A H22A 109.3 . . ?
N11 C22A H22B 109.3 . . ?
C23A C22A H22B 109.3 . . ?
H22A C22A H22B 107.9 . . ?
N12A C23A C22A 112.2(10) . . ?
N12A C23A H23A 109.2 . . ?
C22A C23A H23A 109.2 . . ?
N12A C23A H23B 109.2 . . ?
C22A C23A H23B 109.2 . . ?
H23A C23A H23B 107.9 . . ?
C25A C24A N12A 114.3(9) . . ?
C25A C24A H24A 108.7 . . ?
N12A C24A H24A 108.7 . . ?
C25A C24A H24B 108.7 . . ?
N12A C24A H24B 108.7 . . ?
H24A C24A H24B 107.6 . . ?
C24A C25A N13 111.1(7) . . ?
C24A C25A H25A 109.4 . . ?
N13 C25A H25A 109.4 . . ?
C24A C25A H25B 109.4 . . ?
N13 C25A H25B 109.4 . . ?
H25A C25A H25B 108.0 . . ?
N13 C26A C27A 110.9(8) . . ?
N13 C26A H26A 109.5 . . ?
C27A C26A H26A 109.5 . . ?
N13 C26A H26B 109.5 . . ?
C27A C26A H26B 109.5 . . ?
H26A C26A H26B 108.0 . . ?
N10A C27A C26A 108.4(10) . . ?
N10A C27A H27A 110.0 . . ?
C26A C27A H27A 110.0 . . ?
N10A C27A H27B 110.0 . . ?
C26A C27A H27B 110.0 . . ?
H27A C27A H27B 108.4 . . ?
C20A N10A C27A 113.3(8) . . ?
C20A N10A C19 114.0(5) . . ?
C27A N10A C19 115.1(7) . . ?
C21A N11 C22A 114.0(8) . . ?
C21A N11 H11 123.0 . . ?
C22A N11 H11 123.0 . . ?
C23A N12A C24A 114.1(7) . . ?
C23A N12A HN2A 110(4) . . ?
C24A N12A HN2A 108(4) . . ?
C26A N13 C25A 110.9(6) . . ?
C26A N13 HN3A 99(3) . . ?
C25A N13 HN3A 120(3) . . ?
C1 N1 C9 124.5(2) . . ?
C1 N1 H0 117.8 . . ?
C9 N1 H0 117.8 . . ?
C18 N2 C7 122.3(2) . . ?
C18 N2 C12 118.0(3) . . ?
C7 N2 C12 118.4(2) . . ?
C13 O4 C14 120.9(2) . . ?
C27B C28B N10B 110.5(9) . . ?
C27B C28B H28A 109.5 . . ?
N10B C28B H28A 109.5 . . ?
C27B C28B H28B 109.5 . . ?
N10B C28B H28B 109.5 . . ?
H28A C28B H28B 108.1 . . ?
C25B N12B C24B 115.0(12) . . ?
C25B N12B H2B 100(5) . . ?
C24B N12B H2B 125(5) . . ?
N12B C24B C23B 111.8(13) . . ?
N12B C24B H24C 109.3 . . ?
C23B C24B H24C 109.3 . . ?
N12B C24B H24D 109.3 . . ?
C23B C24B H24D 109.3 . . ?
H24C C24B H24D 107.9 . . ?
C19 N10B C28B 104.3(7) . . ?
C19 N10B C21B 116.0(11) . . ?
C28B N10B C21B 109.6(12) . . ?
C23B N11B C22B 114.1(12) . . ?
C23B N11B H1B 120(4) . . ?
C22B N11B H1B 95(4) . . ?
C27B N13B C26B 110.8(11) . . ?
C27B N13B H13B 124.6 . . ?
C26B N13B H13B 124.6 . . ?
N10B C21B C22B 108.1(15) . . ?
N10B C21B H21C 110.1 . . ?
C22B C21B H21C 110.1 . . ?
N10B C21B H21D 110.1 . . ?
C22B C21B H21D 110.1 . . ?
H21C C21B H21D 108.4 . . ?
N11B C22B C21B 113.6(11) . . ?
N11B C22B H22C 108.8 . . ?
C21B C22B H22C 108.8 . . ?
N11B C22B H22D 108.8 . . ?
C21B C22B H22D 108.8 . . ?
H22C C22B H22D 107.7 . . ?
C26B C25B N12B 122.6(17) . . ?
C26B C25B H25C 106.7 . . ?
N12B C25B H25C 106.7 . . ?
C26B C25B H25D 106.7 . . ?
N12B C25B H25D 106.7 . . ?
H25C C25B H25D 106.6 . . ?
C25B C26B N13B 102.8(11) . . ?
C25B C26B H26C 111.2 . . ?
N13B C26B H26C 111.2 . . ?
C25B C26B H26D 111.2 . . ?
N13B C26B H26D 111.2 . . ?
H26C C26B H26D 109.1 . . ?
N13B C27B C28B 123.2(18) . . ?
N13B C27B H27C 106.5 . . ?
C28B C27B H27C 106.5 . . ?
N13B C27B H27D 106.5 . . ?
C28B C27B H27D 106.5 . . ?
H27C C27B H27D 106.5 . . ?
N11B C23B C24B 113.6(17) . . ?
N11B C23B H23C 108.8 . . ?
C24B C23B H23C 108.8 . . ?
N11B C23B H23D 108.8 . . ?
C24B C23B H23D 108.8 . . ?
H23C C23B H23D 107.7 . . ?

_refine_diff_density_max         0.254
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.041

####################################################################### 
# 
# 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_ao_keb_dk_dy_glyme_1_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1833918'
_audit_update_record             
;
2018-06-07 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;
_audit_creation_date             2018-06-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H41 Dy N6 O11'
_chemical_formula_sum            'C30 H41 Dy N6 O11'
_chemical_formula_weight         824.19
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.7962(2)
_cell_length_b                   14.4010(4)
_cell_length_c                   17.6620(5)
_cell_angle_alpha                100.1990(10)
_cell_angle_beta                 98.0780(10)
_cell_angle_gamma                107.4760(10)
_cell_volume                     2055.13(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.34
_cell_measurement_theta_min      2.39
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.873
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1018 before and 0.0506 after correction.
The Ratio of minimum to maximum transmission is 0.8053.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             834
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46688
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.877
_diffrn_reflns_theta_min         1.706
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_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         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10870
_reflns_number_total             12686
_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       'APEX2  (Bruker AXS, 2012)'
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         1.630
_refine_diff_density_min         -1.251
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         12686
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0318
_refine_ls_restrained_S_all      0.998
_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)+(0.0346P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0708
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-H3A = O3-H3B
 0.95 with sigma of 0.1
3. Others
 Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(H14A)=Sof(H14B)=Sof(C15B)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C28(H28A,H28B), C24(H24A,H24B), C30(H30A,H30B), C27(H27A,
 H27B), C22(H22A,H22B), C26(H26A,H26B), C20(H20A,H20B), C25(H25A,H25B),
 C23(H23A,H23B), C19(H19A,H19B), C12(H12A,H12B), C32(H32A,H32B), C14(H14A,H14B),
  C14(H14C,H14D)
4.b Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C15B(H15A,H15B,H15C), C15A(H15D,H15E,H15F)
4.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C5(H5), C8(H8), C6(H6)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy01 Dy 0.86438(2) 0.69280(2) 0.63056(2) 0.01256(3) Uani 1 1 d . . . . .
O8 O 1.2373(2) 0.60089(12) 0.52886(10) 0.0210(4) Uani 1 1 d . . . . .
O6 O 0.60271(19) 0.64598(12) 0.65162(10) 0.0175(3) Uani 1 1 d . . . . .
O4 O 1.06831(19) 0.63017(12) 0.60424(10) 0.0179(3) Uani 1 1 d . . . . .
O3 O 0.7647(2) 0.51199(13) 0.61390(11) 0.0184(4) Uani 1 1 d D . . . .
O7 O 0.91966(19) 0.65647(12) 0.75838(10) 0.0177(3) Uani 1 1 d . . . . .
O5 O 0.7533(2) 0.62386(12) 0.49712(10) 0.0186(3) Uani 1 1 d . . . . .
O10 O 0.4282(2) 0.64210(13) 0.73185(11) 0.0237(4) Uani 1 1 d . . . . .
O9 O 0.5695(2) 0.59975(13) 0.38995(11) 0.0263(4) Uani 1 1 d . . . . .
O0 O 0.4212(2) 0.27315(13) 0.90289(11) 0.0269(4) Uani 1 1 d . . . . .
O1 O 0.5865(2) 0.19667(13) 1.04114(11) 0.0244(4) Uani 1 1 d . . . . .
N11 N 1.0559(2) 0.79570(14) 0.55106(12) 0.0150(4) Uani 1 1 d . . . . .
O2 O 0.3172(2) 0.14646(13) 1.03076(12) 0.0303(4) Uani 1 1 d . . . . .
N12 N 0.7296(2) 0.80345(14) 0.56347(12) 0.0157(4) Uani 1 1 d . . . . .
N13 N 0.8133(2) 0.82929(14) 0.73700(12) 0.0171(4) Uani 1 1 d . . . . .
N10 N 1.1377(2) 0.81901(14) 0.72326(11) 0.0157(4) Uani 1 1 d . . . . .
N2 N 1.0872(2) 0.68530(14) 0.87679(12) 0.0173(4) Uani 1 1 d . . . . .
H2 H 1.1884 0.7164 0.9025 0.021 Uiso 1 1 calc R . . . .
N1 N 0.6252(2) 0.40958(15) 0.89692(12) 0.0203(4) Uani 1 1 d . . . . .
H1 H 0.6013 0.3902 0.8453 0.024 Uiso 1 1 calc R . . . .
C29 C 1.1447(3) 0.64613(17) 0.54966(14) 0.0168(5) Uani 1 1 d . . . . .
C31 C 0.6448(3) 0.64745(17) 0.45767(15) 0.0188(5) Uani 1 1 d . . . . .
C21 C 1.1921(3) 0.88023(18) 0.60417(14) 0.0198(5) Uani 1 1 d . . . . .
H21A H 1.1526 0.9366 0.6208 0.024 Uiso 1 1 calc R . . . .
H21B H 1.2792 0.9032 0.5750 0.024 Uiso 1 1 calc R . . . .
C28 C 1.1204(3) 0.72432(18) 0.50680(15) 0.0191(5) Uani 1 1 d . . . . .
H28A H 1.2260 0.7620 0.4958 0.023 Uiso 1 1 calc R . . . .
H28B H 1.0442 0.6902 0.4557 0.023 Uiso 1 1 calc R . . . .
C24 C 0.6535(3) 0.85632(18) 0.61947(15) 0.0208(5) Uani 1 1 d . . . . .
H24A H 0.5518 0.8081 0.6259 0.025 Uiso 1 1 calc R . . . .
H24B H 0.6248 0.9089 0.5974 0.025 Uiso 1 1 calc R . . . .
C30 C 0.6010(3) 0.73493(18) 0.49656(15) 0.0198(5) Uani 1 1 d . . . . .
H30A H 0.5799 0.7729 0.4571 0.024 Uiso 1 1 calc R . . . .
H30B H 0.4991 0.7094 0.5155 0.024 Uiso 1 1 calc R . . . .
C27 C 1.1131(3) 0.90891(17) 0.76858(15) 0.0200(5) Uani 1 1 d . . . . .
H27A H 1.1087 0.9557 0.7341 0.024 Uiso 1 1 calc R . . . .
H27B H 1.2074 0.9434 0.8129 0.024 Uiso 1 1 calc R . . . .
C22 C 0.9636(3) 0.83626(17) 0.49593(14) 0.0171(5) Uani 1 1 d . . . . .
H22A H 0.9004 0.7822 0.4492 0.020 Uiso 1 1 calc R . . . .
H22B H 1.0411 0.8892 0.4780 0.020 Uiso 1 1 calc R . . . .
C26 C 0.9591(3) 0.88360(18) 0.80052(15) 0.0205(5) Uani 1 1 d . . . . .
H26A H 0.9671 0.8417 0.8387 0.025 Uiso 1 1 calc R . . . .
H26B H 0.9472 0.9461 0.8287 0.025 Uiso 1 1 calc R . . . .
C33 C 0.5590(3) 0.68048(17) 0.71339(15) 0.0167(5) Uani 1 1 d . . . . .
C5 C 0.9280(3) 0.61545(18) 1.04644(15) 0.0204(5) Uani 1 1 d . . . . .
H5 H 0.9553 0.6403 1.1019 0.024 Uiso 1 1 calc R . . . .
C1 C 0.5322(3) 0.35299(18) 0.93776(15) 0.0204(5) Uani 1 1 d . . . . .
C18 C 1.0545(3) 0.69660(16) 0.80372(14) 0.0149(4) Uani 1 1 d . . . . .
C20 C 1.2624(3) 0.85190(18) 0.67653(14) 0.0189(5) Uani 1 1 d . . . . .
H20A H 1.3058 0.7972 0.6603 0.023 Uiso 1 1 calc R . . . .
H20B H 1.3538 0.9102 0.7095 0.023 Uiso 1 1 calc R . . . .
C4 C 0.7914(3) 0.52912(17) 1.01304(14) 0.0176(5) Uani 1 1 d . . . . .
C25 C 0.7668(3) 0.90358(17) 0.69894(15) 0.0212(5) Uani 1 1 d . . . . .
H25A H 0.8666 0.9536 0.6925 0.025 Uiso 1 1 calc R . . . .
H25B H 0.7130 0.9392 0.7337 0.025 Uiso 1 1 calc R . . . .
C7 C 0.9812(3) 0.62990(17) 0.91892(14) 0.0163(5) Uani 1 1 d . . . . .
C9 C 0.7555(3) 0.49597(17) 0.93114(14) 0.0175(5) Uani 1 1 d . . . . .
C2 C 0.5680(3) 0.38824(18) 1.02292(14) 0.0193(5) Uani 1 1 d . . . . .
C23 C 0.8496(3) 0.87894(17) 0.53435(15) 0.0201(5) Uani 1 1 d . . . . .
H23A H 0.9138 0.9358 0.5790 0.024 Uiso 1 1 calc R . . . .
H23B H 0.7902 0.9050 0.4960 0.024 Uiso 1 1 calc R . . . .
C8 C 0.8483(3) 0.54635(17) 0.88319(14) 0.0175(5) Uani 1 1 d . . . . .
H8 H 0.8201 0.5234 0.8276 0.021 Uiso 1 1 calc R . . . .
C13 C 0.4626(3) 0.21608(18) 1.04257(14) 0.0204(5) Uani 1 1 d . . . . .
C3 C 0.6917(3) 0.47367(18) 1.05978(15) 0.0194(5) Uani 1 1 d . . . . .
C19 C 1.1948(3) 0.76375(18) 0.77748(14) 0.0178(5) Uani 1 1 d . . . . .
H19A H 1.2724 0.8120 0.8241 0.021 Uiso 1 1 calc R . . . .
H19B H 1.2529 0.7228 0.7509 0.021 Uiso 1 1 calc R . . . .
C12 C 0.4557(3) 0.32027(18) 1.06220(16) 0.0226(5) Uani 1 1 d . . . . .
H12A H 0.4873 0.3469 1.1199 0.027 Uiso 1 1 calc R . . . .
H12B H 0.3427 0.3186 1.0448 0.027 Uiso 1 1 calc R . . . .
C6 C 1.0223(3) 0.66430(18) 1.00070(14) 0.0194(5) Uani 1 1 d . . . . .
H6 H 1.1155 0.7215 1.0245 0.023 Uiso 1 1 calc R . . . .
C32 C 0.6784(3) 0.77401(18) 0.76988(15) 0.0213(5) Uani 1 1 d . . . . .
H32A H 0.6184 0.8192 0.7875 0.026 Uiso 1 1 calc R . . . .
H32B H 0.7248 0.7550 0.8168 0.026 Uiso 1 1 calc R . . . .
C10 C 0.7317(3) 0.5140(2) 1.14682(15) 0.0276(6) Uani 1 1 d . . . . .
H10A H 0.8251 0.5762 1.1606 0.041 Uiso 1 1 calc R . . . .
H10B H 0.6375 0.5276 1.1638 0.041 Uiso 1 1 calc R . . . .
H10C H 0.7586 0.4648 1.1730 0.041 Uiso 1 1 calc R . . . .
C14 C 0.3134(4) 0.0426(2) 1.0090(3) 0.0546(11) Uani 1 1 d . . . . .
H14A H 0.3412 0.0303 0.9566 0.066 Uiso 0.528(7) 1 calc R . P A -1
H14B H 0.3973 0.0327 1.0473 0.066 Uiso 0.528(7) 1 calc R . P A -1
H14C H 0.2174 0.0050 0.9661 0.066 Uiso 0.472(7) 1 calc R . P A 1
H14D H 0.4117 0.0422 0.9879 0.066 Uiso 0.472(7) 1 calc R . P A 1
C15B C 0.1560(7) -0.0297(4) 1.0069(4) 0.0377(17) Uani 0.528(7) 1 d . . P A -1
H15A H 0.1604 -0.0976 0.9921 0.057 Uiso 0.528(7) 1 calc R . P A -1
H15B H 0.1287 -0.0191 1.0589 0.057 Uiso 0.528(7) 1 calc R . P A -1
H15C H 0.0726 -0.0214 0.9682 0.057 Uiso 0.528(7) 1 calc R . P A -1
C15A C 0.3074(9) -0.0024(5) 1.0628(4) 0.042(2) Uani 0.472(7) 1 d . . P A 1
H15D H 0.3053 -0.0708 1.0425 0.063 Uiso 0.472(7) 1 calc R . P A 1
H15E H 0.4034 0.0326 1.1051 0.063 Uiso 0.472(7) 1 calc R . P A 1
H15F H 0.2087 -0.0046 1.0832 0.063 Uiso 0.472(7) 1 calc R . P A 1
H3A H 0.768(3) 0.483(2) 0.5751(17) 0.020(8) Uiso 1 1 d D . . . .
H3B H 0.677(4) 0.492(2) 0.6162(18) 0.027(9) Uiso 1 1 d 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
Dy01 O6 2.2996(15) . ?
Dy01 O4 2.3032(15) . ?
Dy01 O3 2.4331(17) . ?
Dy01 O7 2.4227(16) . ?
Dy01 O5 2.3316(17) . ?
Dy01 N11 2.6282(18) . ?
Dy01 N12 2.5996(19) . ?
Dy01 N13 2.6570(19) . ?
Dy01 N10 2.6417(19) . ?
O8 C29 1.241(3) . ?
O6 C33 1.275(3) . ?
O4 C29 1.265(3) . ?
O3 H3A 0.74(3) . ?
O3 H3B 0.74(3) . ?
O7 C18 1.241(3) . ?
O5 C31 1.266(3) . ?
O10 C33 1.234(3) . ?
O9 C31 1.247(3) . ?
O0 C1 1.249(3) . ?
O1 C13 1.206(3) . ?
N11 C21 1.484(3) . ?
N11 C28 1.476(3) . ?
N11 C22 1.487(3) . ?
O2 C13 1.329(3) . ?
O2 C14 1.466(4) . ?
N12 C24 1.494(3) . ?
N12 C30 1.480(3) . ?
N12 C23 1.491(3) . ?
N13 C26 1.482(3) . ?
N13 C25 1.484(3) . ?
N13 C32 1.472(3) . ?
N10 C27 1.488(3) . ?
N10 C20 1.480(3) . ?
N10 C19 1.476(3) . ?
N2 H2 0.8800 . ?
N2 C18 1.332(3) . ?
N2 C7 1.420(3) . ?
N1 H1 0.8800 . ?
N1 C1 1.352(3) . ?
N1 C9 1.382(3) . ?
C29 C28 1.513(3) . ?
C31 C30 1.506(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C20 1.515(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.513(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C26 1.509(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.503(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C33 C32 1.514(3) . ?
C5 H5 0.9500 . ?
C5 C4 1.407(3) . ?
C5 C6 1.369(3) . ?
C1 C2 1.456(3) . ?
C18 C19 1.508(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C4 C9 1.399(3) . ?
C4 C3 1.451(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C7 C8 1.376(3) . ?
C7 C6 1.398(3) . ?
C9 C8 1.402(3) . ?
C2 C3 1.354(3) . ?
C2 C12 1.506(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C8 H8 0.9500 . ?
C13 C12 1.501(3) . ?
C3 C10 1.495(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C6 H6 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 H14C 0.9900 . ?
C14 H14D 0.9900 . ?
C14 C15B 1.452(6) . ?
C14 C15A 1.239(7) . ?
C15B H15A 0.9800 . ?
C15B H15B 0.9800 . ?
C15B H15C 0.9800 . ?
C15B C15A 1.443(9) . ?
C15A H15D 0.9800 . ?
C15A H15E 0.9800 . ?
C15A H15F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Dy01 O4 142.36(6) . . ?
O6 Dy01 O3 71.51(6) . . ?
O6 Dy01 O7 81.55(6) . . ?
O6 Dy01 O5 87.53(6) . . ?
O6 Dy01 N11 143.22(6) . . ?
O6 Dy01 N12 75.39(6) . . ?
O6 Dy01 N13 66.84(6) . . ?
O6 Dy01 N10 130.27(6) . . ?
O4 Dy01 O3 70.92(6) . . ?
O4 Dy01 O7 84.98(6) . . ?
O4 Dy01 O5 83.80(6) . . ?
O4 Dy01 N11 67.08(6) . . ?
O4 Dy01 N12 132.30(6) . . ?
O4 Dy01 N13 139.81(6) . . ?
O4 Dy01 N10 73.39(6) . . ?
O3 Dy01 N11 127.46(6) . . ?
O3 Dy01 N12 128.37(6) . . ?
O3 Dy01 N13 127.42(6) . . ?
O3 Dy01 N10 126.39(6) . . ?
O7 Dy01 O3 71.96(6) . . ?
O7 Dy01 N11 131.74(6) . . ?
O7 Dy01 N12 139.57(6) . . ?
O7 Dy01 N13 71.50(6) . . ?
O7 Dy01 N10 66.25(6) . . ?
O5 Dy01 O3 73.19(6) . . ?
O5 Dy01 O7 145.15(6) . . ?
O5 Dy01 N11 72.28(6) . . ?
O5 Dy01 N12 66.83(6) . . ?
O5 Dy01 N13 133.19(6) . . ?
O5 Dy01 N10 139.66(6) . . ?
N11 Dy01 N13 105.08(6) . . ?
N11 Dy01 N10 68.33(6) . . ?
N12 Dy01 N11 68.51(6) . . ?
N12 Dy01 N13 69.02(6) . . ?
N12 Dy01 N10 105.24(6) . . ?
N10 Dy01 N13 67.46(6) . . ?
C33 O6 Dy01 125.24(15) . . ?
C29 O4 Dy01 124.64(15) . . ?
Dy01 O3 H3A 114(2) . . ?
Dy01 O3 H3B 113(2) . . ?
H3A O3 H3B 104(3) . . ?
C18 O7 Dy01 122.08(14) . . ?
C31 O5 Dy01 124.22(15) . . ?
C21 N11 Dy01 111.47(14) . . ?
C21 N11 C22 108.62(17) . . ?
C28 N11 Dy01 105.61(13) . . ?
C28 N11 C21 109.92(18) . . ?
C28 N11 C22 110.19(18) . . ?
C22 N11 Dy01 111.02(12) . . ?
C13 O2 C14 115.7(2) . . ?
C24 N12 Dy01 110.51(14) . . ?
C30 N12 Dy01 106.62(13) . . ?
C30 N12 C24 109.13(18) . . ?
C30 N12 C23 109.76(19) . . ?
C23 N12 Dy01 111.74(13) . . ?
C23 N12 C24 109.04(17) . . ?
C26 N13 Dy01 112.38(13) . . ?
C26 N13 C25 108.31(18) . . ?
C25 N13 Dy01 110.04(14) . . ?
C32 N13 Dy01 105.81(13) . . ?
C32 N13 C26 110.01(19) . . ?
C32 N13 C25 110.29(19) . . ?
C27 N10 Dy01 112.02(13) . . ?
C20 N10 Dy01 110.37(14) . . ?
C20 N10 C27 108.74(18) . . ?
C19 N10 Dy01 106.59(13) . . ?
C19 N10 C27 110.07(19) . . ?
C19 N10 C20 109.00(18) . . ?
C18 N2 H2 115.5 . . ?
C18 N2 C7 128.9(2) . . ?
C7 N2 H2 115.5 . . ?
C1 N1 H1 117.9 . . ?
C1 N1 C9 124.1(2) . . ?
C9 N1 H1 117.9 . . ?
O8 C29 O4 123.9(2) . . ?
O8 C29 C28 118.1(2) . . ?
O4 C29 C28 118.0(2) . . ?
O5 C31 C30 117.7(2) . . ?
O9 C31 O5 123.2(2) . . ?
O9 C31 C30 119.0(2) . . ?
N11 C21 H21A 109.1 . . ?
N11 C21 H21B 109.1 . . ?
N11 C21 C20 112.48(19) . . ?
H21A C21 H21B 107.8 . . ?
C20 C21 H21A 109.1 . . ?
C20 C21 H21B 109.1 . . ?
N11 C28 C29 113.49(19) . . ?
N11 C28 H28A 108.9 . . ?
N11 C28 H28B 108.9 . . ?
C29 C28 H28A 108.9 . . ?
C29 C28 H28B 108.9 . . ?
H28A C28 H28B 107.7 . . ?
N12 C24 H24A 109.3 . . ?
N12 C24 H24B 109.3 . . ?
N12 C24 C25 111.64(19) . . ?
H24A C24 H24B 108.0 . . ?
C25 C24 H24A 109.3 . . ?
C25 C24 H24B 109.3 . . ?
N12 C30 C31 113.13(19) . . ?
N12 C30 H30A 109.0 . . ?
N12 C30 H30B 109.0 . . ?
C31 C30 H30A 109.0 . . ?
C31 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
N10 C27 H27A 109.0 . . ?
N10 C27 H27B 109.0 . . ?
N10 C27 C26 112.74(18) . . ?
H27A C27 H27B 107.8 . . ?
C26 C27 H27A 109.0 . . ?
C26 C27 H27B 109.0 . . ?
N11 C22 H22A 109.4 . . ?
N11 C22 H22B 109.4 . . ?
N11 C22 C23 111.36(19) . . ?
H22A C22 H22B 108.0 . . ?
C23 C22 H22A 109.4 . . ?
C23 C22 H22B 109.4 . . ?
N13 C26 C27 111.6(2) . . ?
N13 C26 H26A 109.3 . . ?
N13 C26 H26B 109.3 . . ?
C27 C26 H26A 109.3 . . ?
C27 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
O6 C33 C32 117.70(19) . . ?
O10 C33 O6 125.0(2) . . ?
O10 C33 C32 117.2(2) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C6 C5 C4 121.4(2) . . ?
O0 C1 N1 120.5(2) . . ?
O0 C1 C2 122.0(2) . . ?
N1 C1 C2 117.5(2) . . ?
O7 C18 N2 124.4(2) . . ?
O7 C18 C19 120.2(2) . . ?
N2 C18 C19 115.4(2) . . ?
N10 C20 C21 111.30(19) . . ?
N10 C20 H20A 109.4 . . ?
N10 C20 H20B 109.4 . . ?
C21 C20 H20A 109.4 . . ?
C21 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
C5 C4 C3 122.9(2) . . ?
C9 C4 C5 117.1(2) . . ?
C9 C4 C3 120.0(2) . . ?
N13 C25 C24 112.79(19) . . ?
N13 C25 H25A 109.0 . . ?
N13 C25 H25B 109.0 . . ?
C24 C25 H25A 109.0 . . ?
C24 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
C8 C7 N2 123.3(2) . . ?
C8 C7 C6 121.1(2) . . ?
C6 C7 N2 115.6(2) . . ?
N1 C9 C4 118.4(2) . . ?
N1 C9 C8 119.3(2) . . ?
C4 C9 C8 122.3(2) . . ?
C1 C2 C12 112.9(2) . . ?
C3 C2 C1 121.1(2) . . ?
C3 C2 C12 125.9(2) . . ?
N12 C23 C22 112.43(18) . . ?
N12 C23 H23A 109.1 . . ?
N12 C23 H23B 109.1 . . ?
C22 C23 H23A 109.1 . . ?
C22 C23 H23B 109.1 . . ?
H23A C23 H23B 107.8 . . ?
C7 C8 C9 118.1(2) . . ?
C7 C8 H8 120.9 . . ?
C9 C8 H8 120.9 . . ?
O1 C13 O2 123.1(2) . . ?
O1 C13 C12 124.3(2) . . ?
O2 C13 C12 112.5(2) . . ?
C4 C3 C10 117.9(2) . . ?
C2 C3 C4 118.8(2) . . ?
C2 C3 C10 123.2(2) . . ?
N10 C19 C18 111.26(18) . . ?
N10 C19 H19A 109.4 . . ?
N10 C19 H19B 109.4 . . ?
C18 C19 H19A 109.4 . . ?
C18 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
C2 C12 H12A 109.4 . . ?
C2 C12 H12B 109.4 . . ?
C13 C12 C2 111.0(2) . . ?
C13 C12 H12A 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C5 C6 C7 119.9(2) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
N13 C32 C33 114.5(2) . . ?
N13 C32 H32A 108.6 . . ?
N13 C32 H32B 108.6 . . ?
C33 C32 H32A 108.6 . . ?
C33 C32 H32B 108.6 . . ?
H32A C32 H32B 107.6 . . ?
C3 C10 H10A 109.5 . . ?
C3 C10 H10B 109.5 . . ?
C3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O2 C14 H14A 109.0 . . ?
O2 C14 H14B 109.0 . . ?
O2 C14 H14C 108.4 . . ?
O2 C14 H14D 108.4 . . ?
H14A C14 H14B 107.8 . . ?
H14A C14 H14C 66.6 . . ?
H14A C14 H14D 43.0 . . ?
H14B C14 H14C 141.8 . . ?
H14B C14 H14D 67.5 . . ?
H14C C14 H14D 107.4 . . ?
C15B C14 O2 113.0(3) . . ?
C15B C14 H14A 109.0 . . ?
C15B C14 H14B 109.0 . . ?
C15B C14 H14C 47.3 . . ?
C15B C14 H14D 136.7 . . ?
C15A C14 O2 115.6(4) . . ?
C15A C14 H14A 133.8 . . ?
C15A C14 H14B 46.5 . . ?
C15A C14 H14C 108.4 . . ?
C15A C14 H14D 108.4 . . ?
C15A C14 C15B 64.3(4) . . ?
C14 C15B H15A 109.5 . . ?
C14 C15B H15B 109.5 . . ?
C14 C15B H15C 109.5 . . ?
H15A C15B H15B 109.5 . . ?
H15A C15B H15C 109.5 . . ?
H15B C15B H15C 109.5 . . ?
C15A C15B C14 50.7(3) . . ?
C15A C15B H15A 88.9 . . ?
C15A C15B H15B 74.2 . . ?
C15A C15B H15C 157.8 . . ?
C14 C15A C15B 65.0(5) . . ?
C14 C15A H15D 109.5 . . ?
C14 C15A H15E 109.5 . . ?
C14 C15A H15F 109.5 . . ?
C15B C15A H15D 85.8 . . ?
C15B C15A H15E 164.6 . . ?
C15B C15A H15F 62.0 . . ?
H15D C15A H15E 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.282 0.000 0.500 693.2 196.7 ?

_shelx_SHELXL_version_number     2014/7

_olex2_submission_special_instructions 'No special instructions were received'
