# 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 
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data_tbnnnno3
_database_code_depnum_ccdc_archive 'CCDC 1817048'
_audit_update_record             
;
2018-01-15 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H25 N10 O9 Tb'
_chemical_formula_weight         684.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 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                   10.8271(5)
_cell_length_b                   14.8273(7)
_cell_length_c                   16.3000(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.757(2)
_cell_angle_gamma                90
_cell_volume                     2603.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9153
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      36.37

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_F_000             1360
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    2.783
_shelx_estimated_absorpt_T_min   0.381
_shelx_estimated_absorpt_T_max   0.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3623
_exptl_absorpt_correction_T_max  0.6070
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus tube'
_diffrn_measurement_device_type  Â
_diffrn_measurement_method\^A    \^A
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34395
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.337
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7590
_reflns_number_gt                6611
_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       APEX3
_computing_cell_refinement\^A    Â
_computing_data_reduction        Â
_computing_structure_solution    Â
_computing_structure_refinement  Â
_computing_molecular_graphics    Â
_computing_publication_material  Â
_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)+(0.0246P)²+0.2842P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7590
_refine_ls_number_parameters     350
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0223
_refine_ls_wR_factor_ref         0.0555
_refine_ls_wR_factor_gt          0.0537
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
Tb1 Tb 0.42008(2) 0.33745(2) 0.66130(2) 0.01117(3) Uani 1 1 d . . . . .
N1 N 0.48865(15) 0.49689(10) 0.67594(10) 0.0134(3) Uani 1 1 d . . . . .
N2 N 0.60463(15) 0.52224(10) 0.70879(9) 0.0128(3) Uani 1 1 d . . . . .
N3 N 0.56157(16) 0.34887(10) 0.79421(10) 0.0131(3) Uani 1 1 d . . . . .
N4 N 0.66649(15) 0.40146(10) 0.80158(9) 0.0130(3) Uani 1 1 d . . . . .
N5 N 0.64047(16) 0.34425(10) 0.62609(10) 0.0137(3) Uani 1 1 d . . . . .
N6 N 0.72779(15) 0.40048(10) 0.66532(10) 0.0134(3) Uani 1 1 d . . . . .
C1 C 0.69855(17) 0.45632(12) 0.73328(11) 0.0125(3) Uani 1 1 d . . . . .
H1A H 0.7758 0.4902 0.7529 0.015 Uiso 1 1 calc R U . . .
C2 C 0.42671(18) 0.57430(14) 0.66149(12) 0.0164(4) Uani 1 1 d . . . . .
C3 C 0.5036(2) 0.64815(12) 0.68543(13) 0.0174(4) Uani 1 1 d . . . . .
H3A H 0.4815 0.7101 0.6816 0.021 Uiso 1 1 calc R U . . .
C4 C 0.61651(19) 0.61345(12) 0.71532(11) 0.0146(4) Uani 1 1 d . . . . .
C5 C 0.2963(2) 0.57729(14) 0.62416(15) 0.0247(4) Uani 1 1 d . . . . .
H5A H 0.2500 0.5270 0.6453 0.037 Uiso 1 1 calc R U . . .
H5B H 0.2943 0.5724 0.5641 0.037 Uiso 1 1 calc R U . . .
H5C H 0.2584 0.6345 0.6384 0.037 Uiso 1 1 calc R U . . .
C6 C 0.7325(2) 0.65888(13) 0.74921(14) 0.0208(4) Uani 1 1 d . . . . .
H6A H 0.8007 0.6405 0.7176 0.031 Uiso 1 1 calc R U . . .
H6B H 0.7519 0.6417 0.8071 0.031 Uiso 1 1 calc R U . . .
H6C H 0.7215 0.7244 0.7453 0.031 Uiso 1 1 calc R U . . .
C7 C 0.56645(18) 0.30394(13) 0.86522(12) 0.0149(4) Uani 1 1 d . . . . .
C8 C 0.6722(2) 0.32685(13) 0.91718(12) 0.0170(4) Uani 1 1 d . . . . .
H8A H 0.6955 0.3039 0.9709 0.020 Uiso 1 1 calc R U . . .
C9 C 0.73582(19) 0.38903(13) 0.87528(12) 0.0156(4) Uani 1 1 d . . . . .
C10 C 0.4668(2) 0.24014(15) 0.88456(12) 0.0214(4) Uani 1 1 d . . . . .
H10A H 0.4295 0.2123 0.8335 0.032 Uiso 1 1 calc R U . . .
H10B H 0.4030 0.2731 0.9109 0.032 Uiso 1 1 calc R U . . .
H10C H 0.5026 0.1932 0.9220 0.032 Uiso 1 1 calc R U . . .
C11 C 0.8540(2) 0.43759(15) 0.89994(13) 0.0239(4) Uani 1 1 d . . . . .
H11A H 0.8411 0.5026 0.8920 0.036 Uiso 1 1 calc R U . . .
H11B H 0.9180 0.4168 0.8659 0.036 Uiso 1 1 calc R U . . .
H11C H 0.8806 0.4254 0.9581 0.036 Uiso 1 1 calc R U . . .
C12 C 0.70080(19) 0.29838(13) 0.57184(11) 0.0163(4) Uani 1 1 d . . . . .
C13 C 0.8254(2) 0.32533(14) 0.57722(13) 0.0199(4) Uani 1 1 d . . . . .
H13A H 0.8873 0.3026 0.5454 0.024 Uiso 1 1 calc R U . . .
C14 C 0.84130(19) 0.39029(13) 0.63676(12) 0.0165(4) Uani 1 1 d . . . . .
C15 C 0.6361(2) 0.22986(14) 0.51543(12) 0.0217(4) Uani 1 1 d . . . . .
H15A H 0.5493 0.2477 0.5020 0.033 Uiso 1 1 calc R U . . .
H15B H 0.6395 0.1709 0.5427 0.033 Uiso 1 1 calc R U . . .
H15C H 0.6772 0.2262 0.4646 0.033 Uiso 1 1 calc R U . . .
C16 C 0.9525(2) 0.44536(16) 0.66641(13) 0.0227(4) Uani 1 1 d . . . . .
H16A H 0.9727 0.4358 0.7257 0.034 Uiso 1 1 calc R U . . .
H16B H 0.9345 0.5093 0.6559 0.034 Uiso 1 1 calc R U . . .
H16C H 1.0231 0.4270 0.6371 0.034 Uiso 1 1 calc R U . . .
O1 O 0.22868(14) 0.36704(11) 0.57252(9) 0.0203(3) Uani 1 1 d . . . . .
O2 O 0.40103(14) 0.38613(10) 0.51885(9) 0.0209(3) Uani 1 1 d . . . . .
O3 O 0.22524(16) 0.40872(11) 0.44434(9) 0.0287(4) Uani 1 1 d . . . . .
N7 N 0.28275(18) 0.38796(11) 0.50905(11) 0.0190(3) Uani 1 1 d . . . . .
O4 O 0.36388(14) 0.19967(10) 0.58532(9) 0.0198(3) Uani 1 1 d . . . . .
O5 O 0.48996(14) 0.18516(10) 0.69521(9) 0.0194(3) Uani 1 1 d . . . . .
O6 O 0.42026(16) 0.06540(10) 0.62845(12) 0.0301(4) Uani 1 1 d . . . . .
N8 N 0.42431(17) 0.14651(12) 0.63617(12) 0.0177(3) Uani 1 1 d . . . . .
O7 O 0.28734(14) 0.41039(9) 0.75178(9) 0.0180(3) Uani 1 1 d . . . . .
O8 O 0.25421(14) 0.26833(9) 0.73250(9) 0.0192(3) Uani 1 1 d . . . . .
O9 O 0.14570(15) 0.34326(10) 0.81532(10) 0.0238(3) Uani 1 1 d . . . . .
N9 N 0.22554(16) 0.34047(11) 0.76828(10) 0.0154(3) Uani 1 1 d . . . . .
N1S N 0.6180(2) 0.58583(18) 0.94062(19) 0.0497(7) Uani 1 1 d . . . . .
C1S C 0.5169(2) 0.57751(16) 0.91654(15) 0.0287(5) Uani 1 1 d . . . . .
C2S C 0.3885(2) 0.56773(19) 0.88524(16) 0.0360(6) Uani 1 1 d . . . . .
H2S1 H 0.3578 0.6249 0.8608 0.054 Uiso 1 1 calc R U . . .
H2S2 H 0.3397 0.5514 0.9305 0.054 Uiso 1 1 calc R U . . .
H2S3 H 0.3807 0.5203 0.8432 0.054 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O7 2.4157(14) . ?
Tb1 O2 2.4204(14) . ?
Tb1 O5 2.4276(15) . ?
Tb1 O4 2.4344(14) . ?
Tb1 O1 2.4452(15) . ?
Tb1 O8 2.4578(14) . ?
Tb1 N1 2.4822(15) . ?
Tb1 N5 2.5117(17) . ?
Tb1 N3 2.5306(17) . ?
Tb1 N8 2.8616(17) . ?
Tb1 N7 2.8618(18) . ?
Tb1 N9 2.8663(17) . ?
N1 C2 1.338(2) . ?
N1 N2 1.367(2) . ?
N2 C4 1.362(2) . ?
N2 C1 1.438(2) . ?
N3 C7 1.332(2) . ?
N3 N4 1.373(2) . ?
N4 C9 1.364(2) . ?
N4 C1 1.449(2) . ?
N5 C12 1.337(2) . ?
N5 N6 1.370(2) . ?
N6 C14 1.366(2) . ?
N6 C1 1.443(2) . ?
C1 H1A 1.0000 . ?
C2 C3 1.407(3) . ?
C2 C5 1.481(3) . ?
C3 C4 1.370(3) . ?
C3 H3A 0.9500 . ?
C4 C6 1.482(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.396(3) . ?
C7 C10 1.492(3) . ?
C8 C9 1.373(3) . ?
C8 H8A 0.9500 . ?
C9 C11 1.488(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.401(3) . ?
C12 C15 1.496(3) . ?
C13 C14 1.366(3) . ?
C13 H13A 0.9500 . ?
C14 C16 1.494(3) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O1 N7 1.277(2) . ?
O2 N7 1.275(2) . ?
O3 N7 1.210(2) . ?
O4 N8 1.276(2) . ?
O5 N8 1.274(2) . ?
O6 N8 1.210(2) . ?
O7 N9 1.277(2) . ?
O8 N9 1.272(2) . ?
O9 N9 1.212(2) . ?
N1S C1S 1.131(4) . ?
C1S C2S 1.439(4) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 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
O7 Tb1 O2 116.97(5) . . ?
O7 Tb1 O5 117.93(5) . . ?
O2 Tb1 O5 119.37(5) . . ?
O7 Tb1 O4 123.55(5) . . ?
O2 Tb1 O4 76.67(5) . . ?
O5 Tb1 O4 52.52(5) . . ?
O7 Tb1 O1 76.12(5) . . ?
O2 Tb1 O1 52.64(5) . . ?
O5 Tb1 O1 121.87(5) . . ?
O4 Tb1 O1 72.29(5) . . ?
O7 Tb1 O8 52.46(5) . . ?
O2 Tb1 O8 125.55(5) . . ?
O5 Tb1 O8 74.36(5) . . ?
O4 Tb1 O8 74.52(5) . . ?
O1 Tb1 O8 74.83(5) . . ?
O7 Tb1 N1 72.87(5) . . ?
O2 Tb1 N1 78.70(5) . . ?
O5 Tb1 N1 141.32(5) . . ?
O4 Tb1 N1 154.86(5) . . ?
O1 Tb1 N1 96.52(5) . . ?
O8 Tb1 N1 125.27(5) . . ?
O7 Tb1 N5 139.34(5) . . ?
O2 Tb1 N5 76.13(5) . . ?
O5 Tb1 N5 78.92(5) . . ?
O4 Tb1 N5 96.44(5) . . ?
O1 Tb1 N5 128.74(5) . . ?
O8 Tb1 N5 151.72(5) . . ?
N1 Tb1 N5 72.65(5) . . ?
O7 Tb1 N3 78.08(5) . . ?
O2 Tb1 N3 141.94(5) . . ?
O5 Tb1 N3 73.69(5) . . ?
O4 Tb1 N3 126.20(5) . . ?
O1 Tb1 N3 154.03(5) . . ?
O8 Tb1 N3 91.83(5) . . ?
N1 Tb1 N3 72.81(5) . . ?
N5 Tb1 N3 71.67(5) . . ?
O7 Tb1 N8 123.32(5) . . ?
O2 Tb1 N8 99.14(5) . . ?
O5 Tb1 N8 26.26(5) . . ?
O4 Tb1 N8 26.33(5) . . ?
O1 Tb1 N8 96.75(5) . . ?
O8 Tb1 N8 71.22(5) . . ?
N1 Tb1 N8 161.28(5) . . ?
N5 Tb1 N8 88.73(5) . . ?
N3 Tb1 N8 99.89(5) . . ?
O7 Tb1 N7 97.07(5) . . ?
O2 Tb1 N7 26.27(5) . . ?
O5 Tb1 N7 124.32(5) . . ?
O4 Tb1 N7 72.35(5) . . ?
O1 Tb1 N7 26.38(5) . . ?
O8 Tb1 N7 100.25(5) . . ?
N1 Tb1 N7 87.62(5) . . ?
N5 Tb1 N7 102.37(5) . . ?
N3 Tb1 N7 160.42(5) . . ?
N8 Tb1 N7 98.58(5) . . ?
O7 Tb1 N9 26.25(4) . . ?
O2 Tb1 N9 125.58(5) . . ?
O5 Tb1 N9 96.16(5) . . ?
O4 Tb1 N9 99.28(5) . . ?
O1 Tb1 N9 74.12(5) . . ?
O8 Tb1 N9 26.22(4) . . ?
N1 Tb1 N9 99.07(5) . . ?
N5 Tb1 N9 155.69(5) . . ?
N3 Tb1 N9 84.08(5) . . ?
N8 Tb1 N9 97.23(5) . . ?
N7 Tb1 N9 100.02(5) . . ?
C2 N1 N2 104.92(15) . . ?
C2 N1 Tb1 131.31(13) . . ?
N2 N1 Tb1 123.60(11) . . ?
C4 N2 N1 112.29(15) . . ?
C4 N2 C1 126.50(17) . . ?
N1 N2 C1 121.20(15) . . ?
C7 N3 N4 104.34(15) . . ?
C7 N3 Tb1 132.72(13) . . ?
N4 N3 Tb1 122.50(11) . . ?
C9 N4 N3 112.19(15) . . ?
C9 N4 C1 126.85(16) . . ?
N3 N4 C1 120.76(15) . . ?
C12 N5 N6 104.97(16) . . ?
C12 N5 Tb1 132.00(13) . . ?
N6 N5 Tb1 123.01(11) . . ?
C14 N6 N5 112.09(16) . . ?
C14 N6 C1 126.82(17) . . ?
N5 N6 C1 120.88(15) . . ?
N2 C1 N6 112.36(15) . . ?
N2 C1 N4 112.19(15) . . ?
N6 C1 N4 110.83(14) . . ?
N2 C1 H1A 107.0 . . ?
N6 C1 H1A 107.0 . . ?
N4 C1 H1A 107.0 . . ?
N1 C2 C3 110.27(18) . . ?
N1 C2 C5 122.56(18) . . ?
C3 C2 C5 127.16(18) . . ?
C4 C3 C2 106.76(17) . . ?
C4 C3 H3A 126.6 . . ?
C2 C3 H3A 126.6 . . ?
N2 C4 C3 105.75(17) . . ?
N2 C4 C6 123.39(18) . . ?
C3 C4 C6 130.86(18) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 C8 111.35(17) . . ?
N3 C7 C10 122.29(18) . . ?
C8 C7 C10 126.32(18) . . ?
C9 C8 C7 106.47(17) . . ?
C9 C8 H8A 126.8 . . ?
C7 C8 H8A 126.8 . . ?
N4 C9 C8 105.64(17) . . ?
N4 C9 C11 123.71(17) . . ?
C8 C9 C11 130.64(18) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N5 C12 C13 110.17(18) . . ?
N5 C12 C15 121.49(18) . . ?
C13 C12 C15 128.35(17) . . ?
C14 C13 C12 107.30(17) . . ?
C14 C13 H13A 126.3 . . ?
C12 C13 H13A 126.3 . . ?
N6 C14 C13 105.47(18) . . ?
N6 C14 C16 123.55(18) . . ?
C13 C14 C16 130.93(18) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 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 . . ?
N7 O1 Tb1 95.33(12) . . ?
N7 O2 Tb1 96.57(10) . . ?
O3 N7 O1 122.04(19) . . ?
O3 N7 O2 122.51(18) . . ?
O1 N7 O2 115.44(16) . . ?
O3 N7 Tb1 179.42(15) . . ?
O1 N7 Tb1 58.29(10) . . ?
O2 N7 Tb1 57.16(9) . . ?
N8 O4 Tb1 95.87(11) . . ?
N8 O5 Tb1 96.25(11) . . ?
O6 N8 O5 122.52(19) . . ?
O6 N8 O4 122.40(19) . . ?
O5 N8 O4 115.08(16) . . ?
O6 N8 Tb1 176.07(15) . . ?
O5 N8 Tb1 57.49(9) . . ?
O4 N8 Tb1 57.80(9) . . ?
N9 O7 Tb1 96.98(10) . . ?
N9 O8 Tb1 95.13(10) . . ?
O9 N9 O8 122.76(16) . . ?
O9 N9 O7 121.82(16) . . ?
O8 N9 O7 115.42(16) . . ?
O9 N9 Tb1 177.94(15) . . ?
O8 N9 Tb1 58.65(9) . . ?
O7 N9 Tb1 56.78(9) . . ?
N1S C1S C2S 179.3(3) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?

_refine_diff_density_max         1.163
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.101

####################################################################### 
# 
# 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_dynnncl
_database_code_depnum_ccdc_archive 'CCDC 1817052'
_audit_update_record             
;
2018-01-15 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H22 Cl3 Dy N6, 2(C2 H3 N)'
_chemical_formula_sum            'C20 H28 Cl3 Dy N8'
_chemical_formula_weight         649.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   9.4983(3)
_cell_length_b                   16.2661(4)
_cell_length_c                   17.1262(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.3140(10)
_cell_angle_gamma                90
_cell_volume                     2638.51(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9673
_cell_measurement_theta_min      2.83
_cell_measurement_theta_max      35.75

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_F_000             1284
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    3.159
_shelx_estimated_absorpt_T_min   0.318
_shelx_estimated_absorpt_T_max   0.451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.303
_exptl_absorpt_correction_T_max  0.438
_exptl_absorpt_process_details   
;
SADABS 2016/2: L. Krause et al., J. Appl. Cryst., 2015, 48, 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus tube'
_diffrn_measurement_device_type  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            52459
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.379
_diffrn_reflns_theta_max         35.771
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12269
_reflns_number_gt                11311
_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       APEX3
_computing_cell_refinement       'SAINT (8.37A)'
_computing_data_reduction        'SAINT (8.37A)'
_computing_structure_solution    'SHELXT (2014/5)'
_computing_structure_refinement  'SHELXL (2017/1)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_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)+(0.0240P)²+3.6000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12269
_refine_ls_number_parameters     297
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0602
_refine_ls_wR_factor_gt          0.0587
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.003
_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
Dy1 Dy 0.50712(2) 0.43398(2) 0.24704(2) 0.00922(2) Uani 1 1 d . . . . .
Cl1 Cl 0.37120(4) 0.56914(2) 0.25070(3) 0.01748(7) Uani 1 1 d . . . . .
Cl2 Cl 0.40358(4) 0.36205(2) 0.36288(2) 0.01570(6) Uani 1 1 d . . . . .
Cl3 Cl 0.37603(4) 0.36362(3) 0.12926(2) 0.01683(7) Uani 1 1 d . . . . .
C1 C 0.87933(15) 0.43710(8) 0.24377(8) 0.0095(2) Uani 1 1 d . . . . .
H1A H 0.984453 0.437686 0.242719 0.011 Uiso 1 1 calc R U . . .
N1 N 0.68004(13) 0.49405(8) 0.16307(7) 0.0112(2) Uani 1 1 d . . . . .
N2 N 0.82250(13) 0.48076(8) 0.17523(7) 0.0104(2) Uani 1 1 d . . . . .
C2 C 0.66510(17) 0.54261(10) 0.09995(9) 0.0133(2) Uani 1 1 d . . . . .
C3 C 0.79707(18) 0.55937(10) 0.07172(9) 0.0159(3) Uani 1 1 d . . . . .
H3A H 0.814445 0.591627 0.027207 0.019 Uiso 1 1 calc R U . . .
C4 C 0.89620(16) 0.52007(10) 0.12096(9) 0.0128(2) Uani 1 1 d . . . . .
C5 C 0.52474(19) 0.57542(12) 0.07002(10) 0.0193(3) Uani 1 1 d . . . . .
H5A H 0.451858 0.533985 0.077037 0.029 Uiso 1 1 calc R U . . .
H5B H 0.526440 0.588586 0.014262 0.029 Uiso 1 1 calc R U . . .
H5C H 0.503633 0.625263 0.099096 0.029 Uiso 1 1 calc R U . . .
C6 C 1.05269(17) 0.51731(12) 0.12067(11) 0.0189(3) Uani 1 1 d . . . . .
H6A H 1.083833 0.459972 0.118551 0.028 Uiso 1 1 calc R U . . .
H6B H 1.095201 0.543202 0.168456 0.028 Uiso 1 1 calc R U . . .
H6C H 1.082142 0.546949 0.074815 0.028 Uiso 1 1 calc R U . . .
N3 N 0.69671(13) 0.33152(8) 0.24592(8) 0.0113(2) Uani 1 1 d . . . . .
N4 N 0.83616(13) 0.35223(8) 0.24378(8) 0.01021(19) Uani 1 1 d . . . . .
C7 C 0.69562(16) 0.24898(9) 0.24758(9) 0.0130(2) Uani 1 1 d . . . . .
C8 C 0.83298(17) 0.21792(9) 0.24653(10) 0.0147(3) Uani 1 1 d . . . . .
H8A H 0.859967 0.161672 0.247189 0.018 Uiso 1 1 calc R U . . .
C9 C 0.92143(16) 0.28504(9) 0.24437(9) 0.0128(2) Uani 1 1 d . . . . .
C10 C 0.56126(19) 0.20163(11) 0.24948(12) 0.0205(3) Uani 1 1 d . . . . .
H10A H 0.514310 0.216488 0.296524 0.031 Uiso 1 1 calc R U . . .
H10B H 0.582117 0.142622 0.250327 0.031 Uiso 1 1 calc R U . . .
H10C H 0.499150 0.214713 0.202841 0.031 Uiso 1 1 calc R U . . .
C11 C 1.07743(18) 0.29064(11) 0.24353(12) 0.0204(3) Uani 1 1 d . . . . .
H11A H 1.116186 0.318825 0.290949 0.031 Uiso 1 1 calc R U . . .
H11B H 1.101562 0.321583 0.197283 0.031 Uiso 1 1 calc R U . . .
H11C H 1.117451 0.235194 0.241788 0.031 Uiso 1 1 calc R U . . .
N5 N 0.70796(13) 0.49178(8) 0.33014(7) 0.0112(2) Uani 1 1 d . . . . .
N6 N 0.84569(13) 0.47896(8) 0.31470(7) 0.0104(2) Uani 1 1 d . . . . .
C12 C 0.71452(17) 0.53595(10) 0.39615(9) 0.0131(2) Uani 1 1 d . . . . .
C13 C 0.85562(18) 0.55017(10) 0.42313(9) 0.0152(3) Uani 1 1 d . . . . .
H13A H 0.888232 0.579448 0.468969 0.018 Uiso 1 1 calc R U . . .
C14 C 0.93744(16) 0.51333(10) 0.37008(9) 0.0127(2) Uani 1 1 d . . . . .
C15 C 0.5844(2) 0.56643(12) 0.43020(11) 0.0202(3) Uani 1 1 d . . . . .
H15A H 0.509371 0.525270 0.422155 0.030 Uiso 1 1 calc R U . . .
H15B H 0.553929 0.617902 0.404413 0.030 Uiso 1 1 calc R U . . .
H15C H 0.604354 0.576170 0.486411 0.030 Uiso 1 1 calc R U . . .
C16 C 1.09329(18) 0.50812(12) 0.36846(11) 0.0197(3) Uani 1 1 d . . . . .
H16A H 1.122323 0.534869 0.320972 0.029 Uiso 1 1 calc R U . . .
H16B H 1.122120 0.450268 0.368663 0.029 Uiso 1 1 calc R U . . .
H16C H 1.138277 0.535789 0.414660 0.029 Uiso 1 1 calc R U . . .
N1S N 0.9432(2) 0.32792(13) 0.43357(12) 0.0311(4) Uani 1 1 d . . . . .
C1S C 0.8399(2) 0.31406(12) 0.46037(13) 0.0255(4) Uani 1 1 d . . . . .
C2S C 0.7090(3) 0.29791(19) 0.4966(2) 0.0452(7) Uani 1 1 d . . . . .
H2SA H 0.718545 0.247073 0.527288 0.068 Uiso 1 1 calc R U . . .
H2SB H 0.631559 0.292016 0.455870 0.068 Uiso 1 1 calc R U . . .
H2SC H 0.688711 0.343762 0.531173 0.068 Uiso 1 1 calc R U . . .
N2S N 0.9595(2) 0.33390(14) 0.04535(14) 0.0362(4) Uani 1 1 d . . . . .
C3S C 0.8502(2) 0.30614(12) 0.03938(12) 0.0241(3) Uani 1 1 d . . . . .
C4S C 0.7098(3) 0.26979(17) 0.03287(19) 0.0402(6) Uani 1 1 d . . . . .
H4SA H 0.710424 0.218966 0.063613 0.060 Uiso 1 1 calc R U . . .
H4SB H 0.682375 0.257378 -0.022174 0.060 Uiso 1 1 calc R U . . .
H4SC H 0.642124 0.308561 0.052782 0.060 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 N3 2.4548(13) . ?
Dy1 N1 2.4648(13) . ?
Dy1 N5 2.4778(13) . ?
Dy1 Cl1 2.5527(4) . ?
Dy1 Cl3 2.5596(4) . ?
Dy1 Cl2 2.5623(4) . ?
C1 N4 1.4401(18) . ?
C1 N2 1.4416(19) . ?
C1 N6 1.4492(19) . ?
C1 H1A 1.0000 . ?
N1 C2 1.3379(19) . ?
N1 N2 1.3706(18) . ?
N2 C4 1.3642(19) . ?
C2 C3 1.404(2) . ?
C2 C5 1.491(2) . ?
C3 C4 1.374(2) . ?
C3 H3A 0.9500 . ?
C4 C6 1.487(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N3 C7 1.3430(19) . ?
N3 N4 1.3698(17) . ?
N4 C9 1.3598(19) . ?
C7 C8 1.400(2) . ?
C7 C10 1.493(2) . ?
C8 C9 1.380(2) . ?
C8 H8A 0.9500 . ?
C9 C11 1.486(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
N5 C12 1.3370(19) . ?
N5 N6 1.3700(18) . ?
N6 C14 1.3591(19) . ?
C12 C13 1.404(2) . ?
C12 C15 1.491(2) . ?
C13 C14 1.376(2) . ?
C13 H13A 0.9500 . ?
C14 C16 1.485(2) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N1S C1S 1.136(3) . ?
C1S C2S 1.455(3) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
N2S C3S 1.129(3) . ?
C3S C4S 1.455(3) . ?
C4S H4SA 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SC 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
N3 Dy1 N1 75.12(4) . . ?
N3 Dy1 N5 74.25(4) . . ?
N1 Dy1 N5 70.53(4) . . ?
N3 Dy1 Cl1 163.25(3) . . ?
N1 Dy1 Cl1 91.91(3) . . ?
N5 Dy1 Cl1 91.61(3) . . ?
N3 Dy1 Cl3 90.22(3) . . ?
N1 Dy1 Cl3 91.34(3) . . ?
N5 Dy1 Cl3 158.46(3) . . ?
Cl1 Dy1 Cl3 100.807(14) . . ?
N3 Dy1 Cl2 91.18(3) . . ?
N1 Dy1 Cl2 160.76(3) . . ?
N5 Dy1 Cl2 93.00(3) . . ?
Cl1 Dy1 Cl2 98.625(13) . . ?
Cl3 Dy1 Cl2 102.338(13) . . ?
N4 C1 N2 112.53(12) . . ?
N4 C1 N6 111.69(12) . . ?
N2 C1 N6 111.00(12) . . ?
N4 C1 H1A 107.1 . . ?
N2 C1 H1A 107.1 . . ?
N6 C1 H1A 107.1 . . ?
C2 N1 N2 105.03(12) . . ?
C2 N1 Dy1 132.12(10) . . ?
N2 N1 Dy1 122.85(9) . . ?
C4 N2 N1 111.96(12) . . ?
C4 N2 C1 127.28(13) . . ?
N1 N2 C1 120.42(12) . . ?
N1 C2 C3 110.48(14) . . ?
N1 C2 C5 121.80(14) . . ?
C3 C2 C5 127.65(14) . . ?
C4 C3 C2 106.67(13) . . ?
C4 C3 H3A 126.7 . . ?
C2 C3 H3A 126.7 . . ?
N2 C4 C3 105.86(13) . . ?
N2 C4 C6 123.52(14) . . ?
C3 C4 C6 130.62(14) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 N3 N4 104.80(12) . . ?
C7 N3 Dy1 132.20(10) . . ?
N4 N3 Dy1 123.00(9) . . ?
C9 N4 N3 112.26(12) . . ?
C9 N4 C1 126.93(13) . . ?
N3 N4 C1 120.78(12) . . ?
N3 C7 C8 110.59(13) . . ?
N3 C7 C10 121.61(14) . . ?
C8 C7 C10 127.80(14) . . ?
C9 C8 C7 106.53(13) . . ?
C9 C8 H8A 126.7 . . ?
C7 C8 H8A 126.7 . . ?
N4 C9 C8 105.82(13) . . ?
N4 C9 C11 123.00(14) . . ?
C8 C9 C11 131.18(14) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 N5 N6 105.10(12) . . ?
C12 N5 Dy1 132.41(10) . . ?
N6 N5 Dy1 122.45(9) . . ?
C14 N6 N5 111.98(12) . . ?
C14 N6 C1 127.45(13) . . ?
N5 N6 C1 120.48(12) . . ?
N5 C12 C13 110.46(14) . . ?
N5 C12 C15 121.49(14) . . ?
C13 C12 C15 128.00(14) . . ?
C14 C13 C12 106.47(14) . . ?
C14 C13 H13A 126.8 . . ?
C12 C13 H13A 126.8 . . ?
N6 C14 C13 105.99(13) . . ?
N6 C14 C16 123.45(14) . . ?
C13 C14 C16 130.56(15) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 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 . . ?
N1S C1S C2S 178.3(3) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
N2S C3S C4S 179.1(3) . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?

_refine_diff_density_max         0.730
_refine_diff_density_min         -2.170
_refine_diff_density_rms         0.140

####################################################################### 
# 
# 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_dynnnno3
_database_code_depnum_ccdc_archive 'CCDC 1817049'
_audit_update_record             
;
2018-01-15 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H22 Dy N9 O9, C2 H3 N'
_chemical_formula_sum            'C18 H25 Dy N10 O9'
_chemical_formula_weight         687.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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                   10.8339(3)
_cell_length_b                   14.8275(4)
_cell_length_c                   16.3088(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.8810(10)
_cell_angle_gamma                90
_cell_volume                     2606.05(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9789
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      36.22

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_F_000             1364
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    2.933
_shelx_estimated_absorpt_T_min   0.592
_shelx_estimated_absorpt_T_max   0.739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_T_max  0.735
_exptl_absorpt_process_details   'SADABS 2016/2'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus tube'
_diffrn_measurement_device_type  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37341
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.336
_diffrn_reflns_theta_max         29.961
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7574
_reflns_number_gt                6936
_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       APEX3
_computing_cell_refinement       'SAINT (8.37A)'
_computing_data_reduction        'SAINT (8.37A)'
_computing_structure_solution    'SHELXT (2014/5)'
_computing_structure_refinement  'SHELXL (2017/1)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_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)+(0.0180P)²+1.6100P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7574
_refine_ls_number_parameters     350
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0161
_refine_ls_wR_factor_ref         0.0385
_refine_ls_wR_factor_gt          0.0374
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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
Dy1 Dy 0.42085(2) 0.33760(2) 0.66135(2) 0.01007(2) Uani 1 1 d . . . . .
C1 C 0.69835(13) 0.45584(10) 0.73306(9) 0.0119(2) Uani 1 1 d . . . . .
H1A H 0.775576 0.489708 0.752712 0.014 Uiso 1 1 calc R U . . .
N1 N 0.48804(11) 0.49663(8) 0.67552(7) 0.0123(2) Uani 1 1 d . . . . .
N2 N 0.60435(11) 0.52183(8) 0.70847(7) 0.0120(2) Uani 1 1 d . . . . .
C2 C 0.42685(14) 0.57432(10) 0.66135(9) 0.0149(3) Uani 1 1 d . . . . .
C3 C 0.50302(15) 0.64796(10) 0.68553(10) 0.0166(3) Uani 1 1 d . . . . .
H3A H 0.480684 0.709907 0.682130 0.020 Uiso 1 1 calc R U . . .
C4 C 0.61597(14) 0.61316(10) 0.71501(9) 0.0136(3) Uani 1 1 d . . . . .
C5 C 0.29562(15) 0.57732(11) 0.62384(12) 0.0241(3) Uani 1 1 d . . . . .
H5A H 0.248405 0.528893 0.647069 0.036 Uiso 1 1 calc R U . . .
H5B H 0.293077 0.569307 0.564044 0.036 Uiso 1 1 calc R U . . .
H5C H 0.259041 0.635725 0.635731 0.036 Uiso 1 1 calc R U . . .
C6 C 0.73238(16) 0.65850(11) 0.74909(11) 0.0202(3) Uani 1 1 d . . . . .
H6A H 0.799896 0.641595 0.716489 0.030 Uiso 1 1 calc R U . . .
H6B H 0.753284 0.639794 0.806469 0.030 Uiso 1 1 calc R U . . .
H6C H 0.720729 0.724032 0.746804 0.030 Uiso 1 1 calc R U . . .
N3 N 0.56194(11) 0.34844(8) 0.79385(7) 0.0121(2) Uani 1 1 d . . . . .
N4 N 0.66656(11) 0.40108(8) 0.80123(7) 0.0119(2) Uani 1 1 d . . . . .
C7 C 0.56610(14) 0.30333(10) 0.86527(9) 0.0136(3) Uani 1 1 d . . . . .
C8 C 0.67287(14) 0.32635(10) 0.91697(9) 0.0158(3) Uani 1 1 d . . . . .
H8A H 0.696922 0.303311 0.970589 0.019 Uiso 1 1 calc R U . . .
C9 C 0.73592(14) 0.38872(10) 0.87497(9) 0.0148(3) Uani 1 1 d . . . . .
C10 C 0.46722(15) 0.23949(11) 0.88437(10) 0.0202(3) Uani 1 1 d . . . . .
H10A H 0.430632 0.211052 0.833323 0.030 Uiso 1 1 calc R U . . .
H10B H 0.402774 0.272349 0.910067 0.030 Uiso 1 1 calc R U . . .
H10C H 0.503044 0.192964 0.922328 0.030 Uiso 1 1 calc R U . . .
C11 C 0.85439(15) 0.43712(12) 0.89963(10) 0.0231(3) Uani 1 1 d . . . . .
H11A H 0.841035 0.502248 0.893571 0.035 Uiso 1 1 calc R U . . .
H11B H 0.917398 0.417795 0.864316 0.035 Uiso 1 1 calc R U . . .
H11C H 0.882678 0.423151 0.957235 0.035 Uiso 1 1 calc R U . . .
N5 N 0.63994(12) 0.34378(8) 0.62585(7) 0.0126(2) Uani 1 1 d . . . . .
N6 N 0.72738(11) 0.40010(8) 0.66499(7) 0.0125(2) Uani 1 1 d . . . . .
C12 C 0.69996(14) 0.29795(10) 0.57159(9) 0.0154(3) Uani 1 1 d . . . . .
C13 C 0.82498(15) 0.32454(11) 0.57703(10) 0.0193(3) Uani 1 1 d . . . . .
H13A H 0.886896 0.301553 0.545429 0.023 Uiso 1 1 calc R U . . .
C14 C 0.84068(14) 0.38986(11) 0.63648(9) 0.0159(3) Uani 1 1 d . . . . .
C15 C 0.63593(16) 0.22907(12) 0.51531(10) 0.0208(3) Uani 1 1 d . . . . .
H15A H 0.550136 0.248028 0.499507 0.031 Uiso 1 1 calc R U . . .
H15B H 0.636139 0.170817 0.543720 0.031 Uiso 1 1 calc R U . . .
H15C H 0.679566 0.223215 0.465831 0.031 Uiso 1 1 calc R U . . .
C16 C 0.95225(14) 0.44494(12) 0.66604(10) 0.0214(3) Uani 1 1 d . . . . .
H16A H 0.973435 0.434818 0.725190 0.032 Uiso 1 1 calc R U . . .
H16B H 0.934018 0.508994 0.656156 0.032 Uiso 1 1 calc R U . . .
H16C H 1.022320 0.427082 0.636127 0.032 Uiso 1 1 calc R U . . .
O1 O 0.23009(10) 0.36783(8) 0.57336(7) 0.0193(2) Uani 1 1 d . . . . .
O2 O 0.40267(11) 0.38574(8) 0.51957(7) 0.0193(2) Uani 1 1 d . . . . .
O3 O 0.22655(12) 0.40889(9) 0.44473(7) 0.0277(3) Uani 1 1 d . . . . .
N7 N 0.28431(13) 0.38822(9) 0.50973(8) 0.0177(3) Uani 1 1 d . . . . .
O4 O 0.36456(11) 0.20073(8) 0.58485(7) 0.0186(2) Uani 1 1 d . . . . .
O5 O 0.49078(10) 0.18621(8) 0.69521(7) 0.0180(2) Uani 1 1 d . . . . .
O6 O 0.42102(12) 0.06612(8) 0.62816(9) 0.0279(3) Uani 1 1 d . . . . .
N8 N 0.42491(12) 0.14750(9) 0.63597(9) 0.0168(3) Uani 1 1 d . . . . .
O7 O 0.28914(10) 0.41024(7) 0.75128(7) 0.0173(2) Uani 1 1 d . . . . .
O8 O 0.25620(10) 0.26801(7) 0.73220(7) 0.0180(2) Uani 1 1 d . . . . .
O9 O 0.14705(11) 0.34306(8) 0.81451(8) 0.0229(2) Uani 1 1 d . . . . .
N9 N 0.22733(12) 0.34026(9) 0.76767(8) 0.0150(2) Uani 1 1 d . . . . .
N1S N 0.61840(18) 0.58492(14) 0.93999(15) 0.0490(5) Uani 1 1 d . . . . .
C1S C 0.51666(18) 0.57731(12) 0.91616(12) 0.0273(4) Uani 1 1 d . . . . .
C2S C 0.38717(18) 0.56828(15) 0.88553(12) 0.0333(4) Uani 1 1 d . . . . .
H2S1 H 0.356070 0.626103 0.862813 0.050 Uiso 1 1 calc R U . . .
H2S2 H 0.339405 0.550418 0.930763 0.050 Uiso 1 1 calc R U . . .
H2S3 H 0.378311 0.522188 0.842257 0.050 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O7 2.4034(11) . ?
Dy1 O2 2.4085(11) . ?
Dy1 O5 2.4150(11) . ?
Dy1 O4 2.4272(11) . ?
Dy1 O1 2.4339(11) . ?
Dy1 O8 2.4504(11) . ?
Dy1 N1 2.4716(12) . ?
Dy1 N5 2.5018(13) . ?
Dy1 N3 2.5209(12) . ?
Dy1 N7 2.8488(13) . ?
Dy1 N8 2.8500(13) . ?
Dy1 N9 2.8546(13) . ?
C1 N2 1.4393(18) . ?
C1 N6 1.4442(18) . ?
C1 N4 1.4466(18) . ?
C1 H1A 1.0000 . ?
N1 C2 1.3374(18) . ?
N1 N2 1.3702(16) . ?
N2 C4 1.3631(18) . ?
C2 C3 1.401(2) . ?
C2 C5 1.490(2) . ?
C3 C4 1.369(2) . ?
C3 H3A 0.9500 . ?
C4 C6 1.486(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N3 C7 1.3399(18) . ?
N3 N4 1.3713(16) . ?
N4 C9 1.3635(18) . ?
C7 C8 1.402(2) . ?
C7 C10 1.486(2) . ?
C8 C9 1.374(2) . ?
C8 H8A 0.9500 . ?
C9 C11 1.489(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
N5 C12 1.3363(18) . ?
N5 N6 1.3706(17) . ?
N6 C14 1.3649(18) . ?
C12 C13 1.405(2) . ?
C12 C15 1.495(2) . ?
C13 C14 1.369(2) . ?
C13 H13A 0.9500 . ?
C14 C16 1.497(2) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O1 N7 1.2799(18) . ?
O2 N7 1.2763(17) . ?
O3 N7 1.2140(17) . ?
O4 N8 1.2782(17) . ?
O5 N8 1.2770(17) . ?
O6 N8 1.2136(18) . ?
O7 N9 1.2780(16) . ?
O8 N9 1.2717(16) . ?
O9 N9 1.2157(17) . ?
N1S C1S 1.136(3) . ?
C1S C2S 1.446(3) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 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
O7 Dy1 O2 117.24(4) . . ?
O7 Dy1 O5 117.97(4) . . ?
O2 Dy1 O5 119.20(4) . . ?
O7 Dy1 O4 123.70(4) . . ?
O2 Dy1 O4 76.28(4) . . ?
O5 Dy1 O4 52.90(4) . . ?
O7 Dy1 O1 75.87(4) . . ?
O2 Dy1 O1 53.02(4) . . ?
O5 Dy1 O1 122.24(4) . . ?
O4 Dy1 O1 72.39(4) . . ?
O7 Dy1 O8 52.74(4) . . ?
O2 Dy1 O8 125.84(4) . . ?
O5 Dy1 O8 74.17(4) . . ?
O4 Dy1 O8 74.55(4) . . ?
O1 Dy1 O8 74.95(4) . . ?
O7 Dy1 N1 72.72(4) . . ?
O2 Dy1 N1 78.54(4) . . ?
O5 Dy1 N1 141.53(4) . . ?
O4 Dy1 N1 154.40(4) . . ?
O1 Dy1 N1 95.95(4) . . ?
O8 Dy1 N1 125.40(4) . . ?
O7 Dy1 N5 139.59(4) . . ?
O2 Dy1 N5 75.71(4) . . ?
O5 Dy1 N5 78.71(4) . . ?
O4 Dy1 N5 96.09(4) . . ?
O1 Dy1 N5 128.70(4) . . ?
O8 Dy1 N5 151.44(4) . . ?
N1 Dy1 N5 73.10(4) . . ?
O7 Dy1 N3 78.12(4) . . ?
O2 Dy1 N3 141.89(4) . . ?
O5 Dy1 N3 73.43(4) . . ?
O4 Dy1 N3 126.32(4) . . ?
O1 Dy1 N3 153.81(4) . . ?
O8 Dy1 N3 91.68(4) . . ?
N1 Dy1 N3 73.27(4) . . ?
N5 Dy1 N3 71.93(4) . . ?
O7 Dy1 N7 97.10(4) . . ?
O2 Dy1 N7 26.44(4) . . ?
O5 Dy1 N7 124.48(4) . . ?
O4 Dy1 N7 72.14(4) . . ?
O1 Dy1 N7 26.58(4) . . ?
O8 Dy1 N7 100.48(4) . . ?
N1 Dy1 N7 87.23(4) . . ?
N5 Dy1 N7 102.13(4) . . ?
N3 Dy1 N7 160.48(4) . . ?
O7 Dy1 N8 123.42(4) . . ?
O2 Dy1 N8 98.90(4) . . ?
O5 Dy1 N8 26.46(4) . . ?
O4 Dy1 N8 26.51(4) . . ?
O1 Dy1 N8 96.97(4) . . ?
O8 Dy1 N8 71.02(4) . . ?
N1 Dy1 N8 161.51(4) . . ?
N5 Dy1 N8 88.48(4) . . ?
N3 Dy1 N8 99.82(4) . . ?
N7 Dy1 N8 98.56(4) . . ?
O7 Dy1 N9 26.39(4) . . ?
O2 Dy1 N9 125.88(4) . . ?
O5 Dy1 N9 96.12(4) . . ?
O4 Dy1 N9 99.34(4) . . ?
O1 Dy1 N9 73.94(4) . . ?
O8 Dy1 N9 26.35(4) . . ?
N1 Dy1 N9 99.07(4) . . ?
N5 Dy1 N9 155.97(4) . . ?
N3 Dy1 N9 84.09(4) . . ?
N7 Dy1 N9 100.09(4) . . ?
N8 Dy1 N9 97.19(4) . . ?
N2 C1 N6 112.24(11) . . ?
N2 C1 N4 112.23(11) . . ?
N6 C1 N4 110.94(12) . . ?
N2 C1 H1A 107.0 . . ?
N6 C1 H1A 107.0 . . ?
N4 C1 H1A 107.0 . . ?
C2 N1 N2 104.63(12) . . ?
C2 N1 Dy1 132.03(10) . . ?
N2 N1 Dy1 123.16(9) . . ?
C4 N2 N1 112.05(12) . . ?
C4 N2 C1 126.62(12) . . ?
N1 N2 C1 121.32(11) . . ?
N1 C2 C3 110.82(13) . . ?
N1 C2 C5 122.14(14) . . ?
C3 C2 C5 127.03(14) . . ?
C4 C3 C2 106.54(13) . . ?
C4 C3 H3A 126.7 . . ?
C2 C3 H3A 126.7 . . ?
N2 C4 C3 105.96(13) . . ?
N2 C4 C6 123.15(13) . . ?
C3 C4 C6 130.89(14) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 N3 N4 104.71(11) . . ?
C7 N3 Dy1 132.60(10) . . ?
N4 N3 Dy1 122.32(8) . . ?
C9 N4 N3 112.14(12) . . ?
C9 N4 C1 126.88(12) . . ?
N3 N4 C1 120.78(11) . . ?
N3 C7 C8 110.70(13) . . ?
N3 C7 C10 122.64(13) . . ?
C8 C7 C10 126.65(13) . . ?
C9 C8 C7 106.60(13) . . ?
C9 C8 H8A 126.7 . . ?
C7 C8 H8A 126.7 . . ?
N4 C9 C8 105.85(13) . . ?
N4 C9 C11 123.73(13) . . ?
C8 C9 C11 130.42(14) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 N5 N6 104.97(12) . . ?
C12 N5 Dy1 132.24(10) . . ?
N6 N5 Dy1 122.78(9) . . ?
C14 N6 N5 112.11(12) . . ?
C14 N6 C1 126.86(13) . . ?
N5 N6 C1 120.81(11) . . ?
N5 C12 C13 110.30(14) . . ?
N5 C12 C15 121.82(14) . . ?
C13 C12 C15 127.89(14) . . ?
C14 C13 C12 107.00(13) . . ?
C14 C13 H13A 126.5 . . ?
C12 C13 H13A 126.5 . . ?
N6 C14 C13 105.62(13) . . ?
N6 C14 C16 123.66(14) . . ?
C13 C14 C16 130.68(14) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 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 . . ?
N7 O1 Dy1 95.10(8) . . ?
N7 O2 Dy1 96.40(8) . . ?
O3 N7 O2 122.57(14) . . ?
O3 N7 O1 121.96(14) . . ?
O2 N7 O1 115.46(12) . . ?
O3 N7 Dy1 179.26(12) . . ?
O2 N7 Dy1 57.16(7) . . ?
O1 N7 Dy1 58.32(7) . . ?
N8 O4 Dy1 95.52(8) . . ?
N8 O5 Dy1 96.14(8) . . ?
O6 N8 O5 122.48(14) . . ?
O6 N8 O4 122.38(14) . . ?
O5 N8 O4 115.13(12) . . ?
O6 N8 Dy1 176.12(12) . . ?
O5 N8 Dy1 57.41(7) . . ?
O4 N8 Dy1 57.96(7) . . ?
N9 O7 Dy1 96.91(8) . . ?
N9 O8 Dy1 94.85(8) . . ?
O9 N9 O8 122.67(13) . . ?
O9 N9 O7 121.84(13) . . ?
O8 N9 O7 115.49(12) . . ?
O9 N9 Dy1 178.07(11) . . ?
O8 N9 Dy1 58.80(7) . . ?
O7 N9 Dy1 56.70(7) . . ?
N1S C1S C2S 179.6(2) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?

_refine_diff_density_max         0.417
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.077

####################################################################### 
# 
# 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_tbnnncl
_database_code_depnum_ccdc_archive 'CCDC 1817051'
_audit_update_record             
;
2018-01-15 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H28 Cl3 N8 Tb'
_chemical_formula_weight         645.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 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                   9.5146(6)
_cell_length_b                   16.2693(10)
_cell_length_c                   17.1333(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.245(3)
_cell_angle_gamma                90
_cell_volume                     2644.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9800
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      30.72

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_F_000             1280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    3.000
_shelx_estimated_absorpt_T_min   0.403
_shelx_estimated_absorpt_T_max   0.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3628
_exptl_absorpt_correction_T_max  0.6300
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus tube'
_diffrn_measurement_device_type  Â
_diffrn_measurement_method\^A    \^A
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35546
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.377
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             7698
_reflns_number_gt                7120
_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       APEX3
_computing_cell_refinement\^A    Â
_computing_data_reduction        Â
_computing_structure_solution    Â
_computing_structure_refinement  Â
_computing_molecular_graphics    Â
_computing_publication_material  Â
_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)+(0.0113P)²+26.5431P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7698
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0932
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_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
Tb1 Tb 0.00589(2) 0.93376(2) 0.24709(2) 0.01080(5) Uani 1 1 d . . . . .
Cl1 Cl -0.13017(10) 1.06982(6) 0.25082(6) 0.02004(19) Uani 1 1 d . . . . .
Cl2 Cl -0.09739(10) 0.86146(6) 0.36357(6) 0.01739(17) Uani 1 1 d . . . . .
Cl3 Cl -0.12432(10) 0.86296(6) 0.12876(6) 0.01873(18) Uani 1 1 d . . . . .
N1 N 0.1974(3) 0.83118(19) 0.2460(2) 0.0125(6) Uani 1 1 d . . . . .
N2 N 0.3366(3) 0.85201(19) 0.24400(19) 0.0106(5) Uani 1 1 d . . . . .
N3 N 0.2078(3) 0.9918(2) 0.33006(19) 0.0121(6) Uani 1 1 d . . . . .
N4 N 0.3454(3) 0.97906(19) 0.31491(19) 0.0118(6) Uani 1 1 d . . . . .
N5 N 0.1803(3) 0.9941(2) 0.16312(19) 0.0127(6) Uani 1 1 d . . . . .
N6 N 0.3227(3) 0.98097(19) 0.17528(19) 0.0116(6) Uani 1 1 d . . . . .
C1 C 0.3794(4) 0.9375(2) 0.2439(2) 0.0108(6) Uani 1 1 d . . . . .
H1A H 0.4843 0.9383 0.2429 0.013 Uiso 1 1 calc R U . . .
C2 C 0.1968(4) 0.7488(2) 0.2476(2) 0.0143(7) Uani 1 1 d . . . . .
C3 C 0.3364(4) 0.7164(2) 0.2469(2) 0.0144(7) Uani 1 1 d . . . . .
H3A H 0.3644 0.6604 0.2479 0.017 Uiso 1 1 calc R U . . .
C4 C 0.4216(4) 0.7853(2) 0.2446(2) 0.0141(7) Uani 1 1 d . . . . .
C5 C 0.0649(4) 0.7017(2) 0.2495(3) 0.0201(8) Uani 1 1 d . . . . .
H5A H 0.0863 0.6428 0.2505 0.030 Uiso 1 1 calc R U . . .
H5B H 0.0177 0.7165 0.2964 0.030 Uiso 1 1 calc R U . . .
H5C H 0.0030 0.7145 0.2028 0.030 Uiso 1 1 calc R U . . .
C6 C 0.5778(4) 0.7912(3) 0.2435(3) 0.0226(9) Uani 1 1 d . . . . .
H6A H 0.6185 0.7359 0.2442 0.034 Uiso 1 1 calc R U . . .
H6B H 0.6016 0.8200 0.1960 0.034 Uiso 1 1 calc R U . . .
H6C H 0.6160 0.8218 0.2896 0.034 Uiso 1 1 calc R U . . .
C7 C 0.2141(4) 1.0361(2) 0.3963(2) 0.0149(7) Uani 1 1 d . . . . .
C8 C 0.3548(4) 1.0502(2) 0.4229(2) 0.0169(7) Uani 1 1 d . . . . .
H8A H 0.3874 1.0798 0.4685 0.020 Uiso 1 1 calc R U . . .
C9 C 0.4366(4) 1.0132(2) 0.3702(2) 0.0134(7) Uani 1 1 d . . . . .
C10 C 0.0843(5) 1.0663(3) 0.4301(3) 0.0217(8) Uani 1 1 d . . . . .
H10A H 0.0096 1.0251 0.4222 0.033 Uiso 1 1 calc R U . . .
H10B H 0.0537 1.1177 0.4042 0.033 Uiso 1 1 calc R U . . .
H10C H 0.1040 1.0762 0.4863 0.033 Uiso 1 1 calc R U . . .
C11 C 0.5924(4) 1.0083(3) 0.3685(3) 0.0209(8) Uani 1 1 d . . . . .
H11A H 0.6217 0.9506 0.3694 0.031 Uiso 1 1 calc R U . . .
H11B H 0.6371 1.0367 0.4143 0.031 Uiso 1 1 calc R U . . .
H11C H 0.6211 1.0346 0.3207 0.031 Uiso 1 1 calc R U . . .
C12 C 0.1660(4) 1.0426(2) 0.1002(2) 0.0143(7) Uani 1 1 d . . . . .
C13 C 0.2975(4) 1.0591(3) 0.0717(2) 0.0178(7) Uani 1 1 d . . . . .
H13A H 0.3146 1.0912 0.0271 0.021 Uiso 1 1 calc R U . . .
C14 C 0.3968(4) 1.0200(2) 0.1209(2) 0.0146(7) Uani 1 1 d . . . . .
C15 C 0.0255(5) 1.0753(3) 0.0703(3) 0.0220(8) Uani 1 1 d . . . . .
H15A H -0.0470 1.0337 0.0772 0.033 Uiso 1 1 calc R U . . .
H15B H 0.0273 1.0887 0.0146 0.033 Uiso 1 1 calc R U . . .
H15C H 0.0041 1.1250 0.0995 0.033 Uiso 1 1 calc R U . . .
C16 C 0.5521(4) 1.0170(3) 0.1207(3) 0.0204(8) Uani 1 1 d . . . . .
H16A H 0.5829 0.9596 0.1189 0.031 Uiso 1 1 calc R U . . .
H16B H 0.5945 1.0432 0.1683 0.031 Uiso 1 1 calc R U . . .
H16C H 0.5817 1.0462 0.0746 0.031 Uiso 1 1 calc R U . . .
N1S N 0.4434(5) 0.8278(3) 0.4339(3) 0.0335(10) Uani 1 1 d . . . . .
N2S N 0.4603(5) 0.8336(3) 0.0457(3) 0.0379(11) Uani 1 1 d . . . . .
C1S C 0.3407(5) 0.8144(3) 0.4607(3) 0.0283(10) Uani 1 1 d . . . . .
C2S C 0.2092(6) 0.7979(4) 0.4965(5) 0.0488(17) Uani 1 1 d . . . . .
H2S1 H 0.2201 0.7486 0.5292 0.073 Uiso 1 1 calc R U . . .
H2S2 H 0.1335 0.7891 0.4554 0.073 Uiso 1 1 calc R U . . .
H2S3 H 0.1857 0.8449 0.5288 0.073 Uiso 1 1 calc R U . . .
C3S C 0.3505(5) 0.8062(3) 0.0387(3) 0.0270(9) Uani 1 1 d . . . . .
C4S C 0.2108(6) 0.7699(4) 0.0317(4) 0.0446(15) Uani 1 1 d . . . . .
H4S1 H 0.1849 0.7566 -0.0233 0.067 Uiso 1 1 calc R U . . .
H4S2 H 0.1426 0.8090 0.0504 0.067 Uiso 1 1 calc R U . . .
H4S3 H 0.2105 0.7196 0.0631 0.067 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 N1 2.472(3) . ?
Tb1 N5 2.478(3) . ?
Tb1 N3 2.490(3) . ?
Tb1 Cl1 2.5675(10) . ?
Tb1 Cl3 2.5690(10) . ?
Tb1 Cl2 2.5734(10) . ?
N1 C2 1.341(5) . ?
N1 N2 1.369(4) . ?
N2 C4 1.354(5) . ?
N2 C1 1.449(5) . ?
N3 C7 1.342(5) . ?
N3 N4 1.369(4) . ?
N4 C9 1.356(5) . ?
N4 C1 1.449(5) . ?
N5 C12 1.334(5) . ?
N5 N6 1.372(4) . ?
N6 C14 1.366(5) . ?
N6 C1 1.443(5) . ?
C2 C3 1.430(5) . ?
C2 C5 1.472(5) . ?
C3 C4 1.385(5) . ?
C4 C6 1.491(5) . ?
C7 C8 1.402(6) . ?
C7 C10 1.486(6) . ?
C8 C9 1.374(5) . ?
C9 C11 1.487(6) . ?
C12 C13 1.402(5) . ?
C12 C15 1.494(6) . ?
C13 C14 1.374(6) . ?
C14 C16 1.479(6) . ?
N1S C1S 1.131(7) . ?
N2S C3S 1.134(7) . ?
C1S C2S 1.458(8) . ?
C3S C4S 1.451(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Tb1 N5 74.76(11) . . ?
N1 Tb1 N3 73.87(11) . . ?
N5 Tb1 N3 70.11(10) . . ?
N1 Tb1 Cl1 162.84(8) . . ?
N5 Tb1 Cl1 91.92(8) . . ?
N3 Tb1 Cl1 91.61(8) . . ?
N1 Tb1 Cl3 90.23(8) . . ?
N5 Tb1 Cl3 91.37(8) . . ?
N3 Tb1 Cl3 158.01(8) . . ?
Cl1 Tb1 Cl3 101.05(3) . . ?
N1 Tb1 Cl2 91.23(8) . . ?
N5 Tb1 Cl2 160.37(8) . . ?
N3 Tb1 Cl2 93.05(8) . . ?
Cl1 Tb1 Cl2 98.78(3) . . ?
Cl3 Tb1 Cl2 102.57(3) . . ?
C2 N1 N2 104.7(3) . . ?
C2 N1 Tb1 132.1(3) . . ?
N2 N1 Tb1 123.2(2) . . ?
C4 N2 N1 112.3(3) . . ?
C4 N2 C1 127.0(3) . . ?
N1 N2 C1 120.7(3) . . ?
C7 N3 N4 105.0(3) . . ?
C7 N3 Tb1 132.1(3) . . ?
N4 N3 Tb1 122.9(2) . . ?
C9 N4 N3 112.2(3) . . ?
C9 N4 C1 127.4(3) . . ?
N3 N4 C1 120.4(3) . . ?
C12 N5 N6 104.8(3) . . ?
C12 N5 Tb1 132.1(3) . . ?
N6 N5 Tb1 123.1(2) . . ?
C14 N6 N5 112.2(3) . . ?
C14 N6 C1 127.1(3) . . ?
N5 N6 C1 120.4(3) . . ?
N6 C1 N2 112.5(3) . . ?
N6 C1 N4 111.2(3) . . ?
N2 C1 N4 111.5(3) . . ?
N1 C2 C3 111.2(3) . . ?
N1 C2 C5 121.7(4) . . ?
C3 C2 C5 127.0(3) . . ?
C4 C3 C2 104.4(3) . . ?
N2 C4 C3 107.3(3) . . ?
N2 C4 C6 122.9(3) . . ?
C3 C4 C6 129.7(4) . . ?
N3 C7 C8 110.2(3) . . ?
N3 C7 C10 121.4(4) . . ?
C8 C7 C10 128.3(4) . . ?
C9 C8 C7 106.8(3) . . ?
N4 C9 C8 105.9(3) . . ?
N4 C9 C11 123.5(4) . . ?
C8 C9 C11 130.6(4) . . ?
N5 C12 C13 110.8(3) . . ?
N5 C12 C15 121.5(4) . . ?
C13 C12 C15 127.6(4) . . ?
C14 C13 C12 106.7(3) . . ?
N6 C14 C13 105.5(3) . . ?
N6 C14 C16 123.5(4) . . ?
C13 C14 C16 131.0(4) . . ?
N1S C1S C2S 179.0(7) . . ?
N2S C3S C4S 178.5(6) . . ?

_refine_diff_density_max         2.613
_refine_diff_density_min         -4.224
_refine_diff_density_rms         0.170

####################################################################### 
# 
# 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_ernnnno3
_database_code_depnum_ccdc_archive 'CCDC 1817050'
_audit_update_record             
;
2018-01-15 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H25 Er N10 O9'
_chemical_formula_weight         692.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 '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                   10.8169(3)
_cell_length_b                   14.8226(5)
_cell_length_c                   16.2864(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.0506(11)
_cell_angle_gamma                90
_cell_volume                     2596.73(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9475
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      36.17

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_F_000             1372
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    3.298
_shelx_estimated_absorpt_T_min   0.391
_shelx_estimated_absorpt_T_max   0.638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4303
_exptl_absorpt_correction_T_max  0.5989
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus tube'
_diffrn_measurement_device_type  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56351
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.339
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6275
_reflns_number_gt                5984
_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       APEX3
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_structure_solution    SHELXT-2014/4
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_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)+(0.0180P)²+1.6100P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6275
_refine_ls_number_parameters     350
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0148
_refine_ls_R_factor_gt           0.0137
_refine_ls_wR_factor_ref         0.0350
_refine_ls_wR_factor_gt          0.0346
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_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
Er1 Er 0.42198(2) 0.33811(2) 0.66166(2) 0.01000(3) Uani 1 1 d . . . . .
C1 C 0.69803(13) 0.45562(10) 0.73269(9) 0.0119(3) Uani 1 1 d . . . . .
H1A H 0.7755 0.4895 0.7523 0.014 Uiso 1 1 calc R U . . .
N1 N 0.48694(11) 0.49628(8) 0.67522(7) 0.0124(2) Uani 1 1 d . . . . .
N2 N 0.60380(11) 0.52159(8) 0.70807(7) 0.0117(2) Uani 1 1 d . . . . .
C2 C 0.42542(13) 0.57385(10) 0.66131(9) 0.0151(3) Uani 1 1 d . . . . .
C3 C 0.50185(15) 0.64763(10) 0.68552(10) 0.0164(3) Uani 1 1 d . . . . .
H3A H 0.4794 0.7096 0.6822 0.020 Uiso 1 1 calc R U . . .
C4 C 0.61523(14) 0.61288(10) 0.71492(9) 0.0139(3) Uani 1 1 d . . . . .
C5 C 0.29372(15) 0.57716(11) 0.62424(12) 0.0239(3) Uani 1 1 d . . . . .
H5A H 0.2467 0.5286 0.6474 0.036 Uiso 1 1 calc R U . . .
H5B H 0.2904 0.5695 0.5643 0.036 Uiso 1 1 calc R U . . .
H5C H 0.2574 0.6355 0.6366 0.036 Uiso 1 1 calc R U . . .
C6 C 0.73198(15) 0.65841(10) 0.74872(11) 0.0195(3) Uani 1 1 d . . . . .
H6A H 0.7995 0.6410 0.7163 0.029 Uiso 1 1 calc R U . . .
H6B H 0.7530 0.6403 0.8064 0.029 Uiso 1 1 calc R U . . .
H6C H 0.7204 0.7240 0.7458 0.029 Uiso 1 1 calc R U . . .
N3 N 0.56153(12) 0.34830(8) 0.79350(8) 0.0122(2) Uani 1 1 d . . . . .
N4 N 0.66653(11) 0.40091(8) 0.80102(7) 0.0122(2) Uani 1 1 d . . . . .
C7 C 0.56652(13) 0.30301(10) 0.86495(9) 0.0138(3) Uani 1 1 d . . . . .
C8 C 0.67343(14) 0.32611(10) 0.91684(9) 0.0160(3) Uani 1 1 d . . . . .
H8A H 0.6977 0.3031 0.9706 0.019 Uiso 1 1 calc R U . . .
C9 C 0.73619(14) 0.38849(10) 0.87485(9) 0.0148(3) Uani 1 1 d . . . . .
C10 C 0.46738(15) 0.23908(11) 0.88430(10) 0.0199(3) Uani 1 1 d . . . . .
H10A H 0.4310 0.2101 0.8333 0.030 Uiso 1 1 calc R U . . .
H10B H 0.4026 0.2721 0.9095 0.030 Uiso 1 1 calc R U . . .
H10C H 0.5033 0.1929 0.9228 0.030 Uiso 1 1 calc R U . . .
C11 C 0.85514(15) 0.43697(12) 0.89947(10) 0.0230(3) Uani 1 1 d . . . . .
H11A H 0.8418 0.5021 0.8933 0.034 Uiso 1 1 calc R U . . .
H11B H 0.9181 0.4175 0.8641 0.034 Uiso 1 1 calc R U . . .
H11C H 0.8837 0.4231 0.9572 0.034 Uiso 1 1 calc R U . . .
N5 N 0.63864(12) 0.34343(8) 0.62548(8) 0.0127(2) Uani 1 1 d . . . . .
N6 N 0.72656(11) 0.39977(8) 0.66456(7) 0.0125(2) Uani 1 1 d . . . . .
C12 C 0.69848(14) 0.29730(10) 0.57124(9) 0.0159(3) Uani 1 1 d . . . . .
C13 C 0.82357(15) 0.32383(11) 0.57658(10) 0.0195(3) Uani 1 1 d . . . . .
H13A H 0.8854 0.3006 0.5450 0.023 Uiso 1 1 calc R U . . .
C14 C 0.83977(13) 0.38941(11) 0.63587(9) 0.0160(3) Uani 1 1 d . . . . .
C15 C 0.63434(15) 0.22849(12) 0.51488(10) 0.0212(3) Uani 1 1 d . . . . .
H15A H 0.5481 0.2471 0.4995 0.032 Uiso 1 1 calc R U . . .
H15B H 0.6354 0.1701 0.5431 0.032 Uiso 1 1 calc R U . . .
H15C H 0.6774 0.2231 0.4651 0.032 Uiso 1 1 calc R U . . .
C16 C 0.95144(14) 0.44438(12) 0.66529(10) 0.0219(3) Uani 1 1 d . . . . .
H16A H 0.9733 0.4341 0.7245 0.033 Uiso 1 1 calc R U . . .
H16B H 0.9330 0.5085 0.6556 0.033 Uiso 1 1 calc R U . . .
H16C H 1.0213 0.4267 0.6351 0.033 Uiso 1 1 calc R U . . .
O1 O 0.23237(10) 0.36879(8) 0.57498(7) 0.0188(2) Uani 1 1 d . . . . .
O2 O 0.40448(10) 0.38553(8) 0.52086(7) 0.0189(2) Uani 1 1 d . . . . .
O3 O 0.22797(12) 0.40899(9) 0.44575(7) 0.0271(3) Uani 1 1 d . . . . .
N7 N 0.28610(13) 0.38847(9) 0.51097(8) 0.0176(3) Uani 1 1 d . . . . .
O4 O 0.36569(10) 0.20283(7) 0.58505(7) 0.0182(2) Uani 1 1 d . . . . .
O5 O 0.49222(10) 0.18821(8) 0.69550(7) 0.0174(2) Uani 1 1 d . . . . .
O6 O 0.42182(12) 0.06806(8) 0.62820(9) 0.0271(3) Uani 1 1 d . . . . .
N8 N 0.42616(12) 0.14954(9) 0.63606(9) 0.0164(3) Uani 1 1 d . . . . .
O7 O 0.29190(10) 0.41014(7) 0.75106(7) 0.0169(2) Uani 1 1 d . . . . .
O8 O 0.25902(10) 0.26801(7) 0.73122(7) 0.0180(2) Uani 1 1 d . . . . .
O9 O 0.14892(11) 0.34283(8) 0.81331(8) 0.0228(3) Uani 1 1 d . . . . .
N9 N 0.22973(12) 0.34020(8) 0.76684(8) 0.0148(2) Uani 1 1 d . . . . .
N1S N 0.61846(17) 0.58443(14) 0.93928(14) 0.0478(5) Uani 1 1 d . . . . .
C1S C 0.51627(18) 0.57772(12) 0.91601(12) 0.0273(4) Uani 1 1 d . . . . .
C2S C 0.38620(18) 0.56918(15) 0.88571(12) 0.0335(4) Uani 1 1 d . . . . .
H2S1 H 0.3552 0.6271 0.8630 0.050 Uiso 1 1 calc R U . . .
H2S2 H 0.3388 0.5515 0.9312 0.050 Uiso 1 1 calc R U . . .
H2S3 H 0.3765 0.5231 0.8424 0.050 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O7 2.3815(11) . ?
Er1 O2 2.3868(11) . ?
Er1 O5 2.3937(11) . ?
Er1 O4 2.4059(11) . ?
Er1 O1 2.4075(11) . ?
Er1 O8 2.4272(11) . ?
Er1 N1 2.4508(12) . ?
Er1 N5 2.4773(13) . ?
Er1 N3 2.4957(13) . ?
Er1 N7 2.8250(13) . ?
Er1 N8 2.8272(13) . ?
Er1 N9 2.8304(13) . ?
C1 N2 1.4386(18) . ?
C1 N6 1.4436(18) . ?
C1 N4 1.4464(18) . ?
C1 H1A 1.0000 . ?
N1 C2 1.3358(19) . ?
N1 N2 1.3719(16) . ?
N2 C4 1.3623(18) . ?
C2 C3 1.402(2) . ?
C2 C5 1.488(2) . ?
C3 C4 1.369(2) . ?
C3 H3A 0.9500 . ?
C4 C6 1.486(2) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N3 C7 1.3396(19) . ?
N3 N4 1.3726(16) . ?
N4 C9 1.3625(18) . ?
C7 C8 1.401(2) . ?
C7 C10 1.489(2) . ?
C8 C9 1.372(2) . ?
C8 H8A 0.9500 . ?
C9 C11 1.491(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
N5 C12 1.3370(19) . ?
N5 N6 1.3708(17) . ?
N6 C14 1.3646(18) . ?
C12 C13 1.403(2) . ?
C12 C15 1.493(2) . ?
C13 C14 1.368(2) . ?
C13 H13A 0.9500 . ?
C14 C16 1.494(2) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O1 N7 1.2796(17) . ?
O2 N7 1.2743(17) . ?
O3 N7 1.2145(17) . ?
O4 N8 1.2757(17) . ?
O5 N8 1.2769(17) . ?
O6 N8 1.2149(18) . ?
O7 N9 1.2765(16) . ?
O8 N9 1.2730(16) . ?
O9 N9 1.2157(17) . ?
N1S C1S 1.134(3) . ?
C1S C2S 1.447(3) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 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
O7 Er1 O2 117.59(4) . . ?
O7 Er1 O5 117.97(4) . . ?
O2 Er1 O5 119.06(4) . . ?
O7 Er1 O4 123.86(4) . . ?
O2 Er1 O4 75.94(4) . . ?
O5 Er1 O4 53.32(4) . . ?
O7 Er1 O1 75.65(4) . . ?
O2 Er1 O1 53.46(4) . . ?
O5 Er1 O1 122.71(4) . . ?
O4 Er1 O1 72.54(4) . . ?
O7 Er1 O8 53.24(4) . . ?
O2 Er1 O8 125.91(4) . . ?
O5 Er1 O8 73.96(4) . . ?
O4 Er1 O8 74.26(4) . . ?
O1 Er1 O8 74.86(4) . . ?
O7 Er1 N1 72.44(4) . . ?
O2 Er1 N1 78.34(4) . . ?
O5 Er1 N1 141.83(4) . . ?
O4 Er1 N1 153.97(4) . . ?
O1 Er1 N1 95.20(4) . . ?
O8 Er1 N1 125.65(4) . . ?
O7 Er1 N5 139.99(4) . . ?
O2 Er1 N5 75.13(4) . . ?
O5 Er1 N5 78.41(4) . . ?
O4 Er1 N5 95.58(4) . . ?
O1 Er1 N5 128.56(4) . . ?
O8 Er1 N5 151.22(4) . . ?
N1 Er1 N5 73.83(4) . . ?
O7 Er1 N3 77.85(4) . . ?
O2 Er1 N3 142.03(4) . . ?
O5 Er1 N3 73.11(4) . . ?
O4 Er1 N3 126.42(4) . . ?
O1 Er1 N3 153.34(4) . . ?
O8 Er1 N3 91.57(4) . . ?
N1 Er1 N3 73.91(4) . . ?
N5 Er1 N3 72.61(4) . . ?
O7 Er1 N7 97.23(4) . . ?
O2 Er1 N7 26.64(4) . . ?
O5 Er1 N7 124.67(4) . . ?
O4 Er1 N7 71.92(4) . . ?
O1 Er1 N7 26.82(4) . . ?
O8 Er1 N7 100.47(4) . . ?
N1 Er1 N7 86.76(4) . . ?
N5 Er1 N7 101.75(4) . . ?
N3 Er1 N7 160.66(4) . . ?
O7 Er1 N8 123.58(4) . . ?
O2 Er1 N8 98.65(4) . . ?
O5 Er1 N8 26.69(4) . . ?
O4 Er1 N8 26.70(4) . . ?
O1 Er1 N8 97.25(4) . . ?
O8 Er1 N8 70.69(4) . . ?
N1 Er1 N8 161.84(4) . . ?
N5 Er1 N8 88.06(4) . . ?
N3 Er1 N8 99.73(4) . . ?
N7 Er1 N8 98.52(4) . . ?
O7 Er1 N9 26.61(4) . . ?
O2 Er1 N9 126.11(4) . . ?
O5 Er1 N9 96.11(4) . . ?
O4 Er1 N9 99.27(4) . . ?
O1 Er1 N9 73.62(4) . . ?
O8 Er1 N9 26.63(4) . . ?
N1 Er1 N9 99.03(4) . . ?
N5 Er1 N9 156.56(4) . . ?
N3 Er1 N9 83.97(4) . . ?
N7 Er1 N9 100.06(4) . . ?
N8 Er1 N9 97.14(4) . . ?
N2 C1 N6 112.22(11) . . ?
N2 C1 N4 112.22(11) . . ?
N6 C1 N4 110.89(12) . . ?
N2 C1 H1A 107.1 . . ?
N6 C1 H1A 107.1 . . ?
N4 C1 H1A 107.1 . . ?
C2 N1 N2 104.65(12) . . ?
C2 N1 Er1 132.46(10) . . ?
N2 N1 Er1 122.71(9) . . ?
C4 N2 N1 112.05(12) . . ?
C4 N2 C1 126.64(12) . . ?
N1 N2 C1 121.29(11) . . ?
N1 C2 C3 110.80(13) . . ?
N1 C2 C5 122.39(14) . . ?
C3 C2 C5 126.81(14) . . ?
C4 C3 C2 106.54(13) . . ?
C4 C3 H3A 126.7 . . ?
C2 C3 H3A 126.7 . . ?
N2 C4 C3 105.95(13) . . ?
N2 C4 C6 123.22(13) . . ?
C3 C4 C6 130.83(14) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 N3 N4 104.48(12) . . ?
C7 N3 Er1 133.03(10) . . ?
N4 N3 Er1 122.07(9) . . ?
C9 N4 N3 112.18(12) . . ?
C9 N4 C1 126.98(12) . . ?
N3 N4 C1 120.64(11) . . ?
N3 C7 C8 110.89(13) . . ?
N3 C7 C10 122.59(13) . . ?
C8 C7 C10 126.50(13) . . ?
C9 C8 C7 106.52(13) . . ?
C9 C8 H8A 126.7 . . ?
C7 C8 H8A 126.7 . . ?
N4 C9 C8 105.93(13) . . ?
N4 C9 C11 123.60(13) . . ?
C8 C9 C11 130.47(14) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 N5 N6 104.94(12) . . ?
C12 N5 Er1 132.60(10) . . ?
N6 N5 Er1 122.44(9) . . ?
C14 N6 N5 112.10(12) . . ?
C14 N6 C1 126.87(13) . . ?
N5 N6 C1 120.81(11) . . ?
N5 C12 C13 110.28(14) . . ?
N5 C12 C15 121.98(14) . . ?
C13 C12 C15 127.75(14) . . ?
C14 C13 C12 107.09(14) . . ?
C14 C13 H13A 126.5 . . ?
C12 C13 H13A 126.5 . . ?
N6 C14 C13 105.59(13) . . ?
N6 C14 C16 123.60(14) . . ?
C13 C14 C16 130.78(14) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 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 . . ?
N7 O1 Er1 95.09(8) . . ?
N7 O2 Er1 96.23(8) . . ?
O3 N7 O2 122.67(14) . . ?
O3 N7 O1 122.13(14) . . ?
O2 N7 O1 115.20(12) . . ?
O3 N7 Er1 179.13(11) . . ?
O2 N7 Er1 57.13(7) . . ?
O1 N7 Er1 58.09(7) . . ?
N8 O4 Er1 95.39(8) . . ?
N8 O5 Er1 95.94(8) . . ?
O6 N8 O4 122.37(14) . . ?
O6 N8 O5 122.58(14) . . ?
O4 N8 O5 115.04(12) . . ?
O6 N8 Er1 175.84(11) . . ?
O4 N8 Er1 57.91(7) . . ?
O5 N8 Er1 57.37(7) . . ?
N9 O7 Er1 96.70(8) . . ?
N9 O8 Er1 94.63(8) . . ?
O9 N9 O8 122.72(12) . . ?
O9 N9 O7 121.86(13) . . ?
O8 N9 O7 115.42(12) . . ?
O9 N9 Er1 178.25(11) . . ?
O8 N9 Er1 58.73(7) . . ?
O7 N9 Er1 56.69(7) . . ?
N1S C1S C2S 179.6(2) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?

_refine_diff_density_max         0.392
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.076

####################################################################### 
# 
# 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_ernnncl
_database_code_depnum_ccdc_archive 'CCDC 1817053'
_audit_update_record             
;
2018-01-15 deposited with the CCDC.
2018-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H28 Cl3 Er N8'
_chemical_formula_weight         654.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   9.4683(3)
_cell_length_b                   16.2801(5)
_cell_length_c                   17.1285(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.4690(10)
_cell_angle_gamma                90
_cell_volume                     2632.24(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9751
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      42.00

_exptl_crystal_description       stick
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_F_000             1292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    3.516
_shelx_estimated_absorpt_T_min   0.570
_shelx_estimated_absorpt_T_max   0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5116
_exptl_absorpt_correction_T_max  0.7589
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus tube'
_diffrn_measurement_device_type  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            57788
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.494
_diffrn_reflns_theta_max         27.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             6292
_reflns_number_gt                5756
_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       APEX3
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_structure_solution    SHELXT-2014/4
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_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)+(0.0427P)²+9.0822P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6292
_refine_ls_number_parameters     297
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0832
_refine_ls_wR_factor_gt          0.0822
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_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
Er1 Er 0.49028(2) 0.56558(2) 0.75293(2) 0.00935(6) Uani 1 1 d . . . . .
Cl1 Cl 0.62598(9) 0.43162(6) 0.74943(6) 0.01746(18) Uani 1 1 d . . . . .
Cl2 Cl 0.59374(9) 0.63653(6) 0.63817(5) 0.01545(17) Uani 1 1 d . . . . .
Cl3 Cl 0.62288(9) 0.63502(6) 0.86940(5) 0.01626(17) Uani 1 1 d . . . . .
N1 N 0.1536(3) 0.52100(19) 0.68536(17) 0.0109(6) Uani 1 1 d . . . . .
N2 N 0.2919(3) 0.50831(19) 0.66998(17) 0.0105(6) Uani 1 1 d . . . . .
N3 N 0.1774(3) 0.51935(19) 0.82484(17) 0.0108(6) Uani 1 1 d . . . . .
N4 N 0.3204(3) 0.50602(19) 0.83663(17) 0.0110(6) Uani 1 1 d . . . . .
N5 N 0.1638(3) 0.64801(18) 0.75630(17) 0.0085(5) Uani 1 1 d . . . . .
N6 N 0.3043(3) 0.66876(18) 0.75379(17) 0.0108(6) Uani 1 1 d . . . . .
C1 C 0.1201(4) 0.5629(2) 0.7566(2) 0.0114(6) Uani 1 1 d . . . . .
H1A H 0.0147 0.5623 0.7577 0.014 Uiso 1 1 calc R U . . .
C2 C 0.0618(4) 0.4865(2) 0.6295(2) 0.0120(7) Uani 1 1 d . . . . .
C3 C 0.1436(4) 0.4502(2) 0.5768(2) 0.0143(7) Uani 1 1 d . . . . .
H3A H 0.1107 0.4212 0.5307 0.017 Uiso 1 1 calc R U . . .
C4 C 0.2855(4) 0.4639(2) 0.6038(2) 0.0134(7) Uani 1 1 d . . . . .
C5 C -0.0944(4) 0.4918(3) 0.6316(2) 0.0207(8) Uani 1 1 d . . . . .
H5A H -0.1403 0.4649 0.5851 0.031 Uiso 1 1 calc R U . . .
H5B H -0.1231 0.5496 0.6323 0.031 Uiso 1 1 calc R U . . .
H5C H -0.1230 0.4644 0.6788 0.031 Uiso 1 1 calc R U . . .
C6 C 0.4155(4) 0.4338(3) 0.5696(2) 0.0200(8) Uani 1 1 d . . . . .
H6A H 0.3943 0.4226 0.5137 0.030 Uiso 1 1 calc R U . . .
H6B H 0.4482 0.3832 0.5963 0.030 Uiso 1 1 calc R U . . .
H6C H 0.4898 0.4757 0.5762 0.030 Uiso 1 1 calc R U . . .
C7 C 0.1034(4) 0.4801(2) 0.8789(2) 0.0142(7) Uani 1 1 d . . . . .
C8 C 0.2039(4) 0.4409(2) 0.9284(2) 0.0158(7) Uani 1 1 d . . . . .
H8A H 0.1870 0.4089 0.9731 0.019 Uiso 1 1 calc R U . . .
C9 C 0.3355(4) 0.4577(2) 0.9001(2) 0.0130(7) Uani 1 1 d . . . . .
C10 C -0.0532(4) 0.4825(3) 0.8796(2) 0.0182(8) Uani 1 1 d . . . . .
H10A H -0.0817 0.4546 0.9266 0.027 Uiso 1 1 calc R U . . .
H10B H -0.0963 0.4547 0.8329 0.027 Uiso 1 1 calc R U . . .
H10C H -0.0851 0.5398 0.8798 0.027 Uiso 1 1 calc R U . . .
C11 C 0.4767(4) 0.4250(3) 0.9304(2) 0.0197(8) Uani 1 1 d . . . . .
H11A H 0.4749 0.4118 0.9861 0.030 Uiso 1 1 calc R U . . .
H11B H 0.5497 0.4664 0.9235 0.030 Uiso 1 1 calc R U . . .
H11C H 0.4981 0.3752 0.9014 0.030 Uiso 1 1 calc R U . . .
C12 C 0.0786(4) 0.7150(2) 0.7553(2) 0.0137(7) Uani 1 1 d . . . . .
C13 C 0.1658(4) 0.7837(2) 0.7528(2) 0.0122(7) Uani 1 1 d . . . . .
H13A H 0.1384 0.8399 0.7517 0.015 Uiso 1 1 calc R U . . .
C14 C 0.3056(4) 0.7510(2) 0.7525(2) 0.0124(7) Uani 1 1 d . . . . .
C15 C -0.0778(4) 0.7099(3) 0.7564(3) 0.0223(8) Uani 1 1 d . . . . .
H15A H -0.1175 0.7655 0.7579 0.033 Uiso 1 1 calc R U . . .
H15B H -0.1019 0.6793 0.8028 0.033 Uiso 1 1 calc R U . . .
H15C H -0.1174 0.6816 0.7091 0.033 Uiso 1 1 calc R U . . .
C16 C 0.4406(4) 0.7980(2) 0.7506(3) 0.0198(8) Uani 1 1 d . . . . .
H16A H 0.4210 0.8569 0.7548 0.030 Uiso 1 1 calc R U . . .
H16B H 0.4828 0.7871 0.7012 0.030 Uiso 1 1 calc R U . . .
H16C H 0.5065 0.7809 0.7946 0.030 Uiso 1 1 calc R U . . .
N1S N 0.0400(5) 0.6657(3) 0.9546(3) 0.0360(10) Uani 1 1 d . . . . .
C1S C 0.1497(5) 0.6940(3) 0.9603(3) 0.0250(9) Uani 1 1 d . . . . .
C2S C 0.2906(5) 0.7306(4) 0.9666(4) 0.0418(13) Uani 1 1 d . . . . .
H2SA H 0.3592 0.6909 0.9490 0.063 Uiso 1 1 calc R U . . .
H2SB H 0.3167 0.7455 1.0212 0.063 Uiso 1 1 calc R U . . .
H2SC H 0.2907 0.7798 0.9337 0.063 Uiso 1 1 calc R U . . .
N2S N 0.0572(4) 0.6720(3) 0.5670(2) 0.0312(9) Uani 1 1 d . . . . .
C3S C 0.1591(5) 0.6861(3) 0.5396(3) 0.0266(9) Uani 1 1 d . . . . .
C4S C 0.2909(5) 0.7033(4) 0.5036(4) 0.0464(15) Uani 1 1 d . . . . .
H4SA H 0.3154 0.6563 0.4715 0.070 Uiso 1 1 calc R U . . .
H4SB H 0.3671 0.7129 0.5447 0.070 Uiso 1 1 calc R U . . .
H4SC H 0.2786 0.7523 0.4705 0.070 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 N6 2.435(3) . ?
Er1 N4 2.437(3) . ?
Er1 N2 2.450(3) . ?
Er1 Cl1 2.5344(9) . ?
Er1 Cl3 2.5384(9) . ?
Er1 Cl2 2.5413(9) . ?
N1 C2 1.362(4) . ?
N1 N2 1.371(4) . ?
N1 C1 1.454(4) . ?
N2 C4 1.342(4) . ?
N3 C7 1.363(4) . ?
N3 N4 1.371(4) . ?
N3 C1 1.437(4) . ?
N4 C9 1.340(4) . ?
N5 C12 1.356(4) . ?
N5 N6 1.376(4) . ?
N5 C1 1.446(4) . ?
N6 C14 1.339(5) . ?
C1 H1A 1.0000 . ?
C2 C3 1.370(5) . ?
C2 C5 1.485(5) . ?
C3 C4 1.405(5) . ?
C3 H3A 0.9500 . ?
C4 C6 1.487(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.381(5) . ?
C7 C10 1.485(5) . ?
C8 C9 1.398(5) . ?
C8 H8A 0.9500 . ?
C9 C11 1.495(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.393(5) . ?
C12 C15 1.485(6) . ?
C13 C14 1.427(5) . ?
C13 H13A 0.9500 . ?
C14 C16 1.492(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
N1S C1S 1.134(6) . ?
C1S C2S 1.457(7) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
N2S C3S 1.130(6) . ?
C3S C4S 1.461(7) . ?
C4S H4SA 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SC 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
N6 Er1 N4 76.13(10) . . ?
N6 Er1 N2 75.16(10) . . ?
N4 Er1 N2 71.25(10) . . ?
N6 Er1 Cl1 164.19(8) . . ?
N4 Er1 Cl1 91.75(8) . . ?
N2 Er1 Cl1 91.48(7) . . ?
N6 Er1 Cl3 90.10(7) . . ?
N4 Er1 Cl3 91.35(7) . . ?
N2 Er1 Cl3 159.28(7) . . ?
Cl1 Er1 Cl3 100.44(3) . . ?
N6 Er1 Cl2 90.78(7) . . ?
N4 Er1 Cl2 161.36(7) . . ?
N2 Er1 Cl2 92.79(7) . . ?
Cl1 Er1 Cl2 98.40(3) . . ?
Cl3 Er1 Cl2 102.04(3) . . ?
C2 N1 N2 111.7(3) . . ?
C2 N1 C1 127.8(3) . . ?
N2 N1 C1 120.4(3) . . ?
C4 N2 N1 105.2(3) . . ?
C4 N2 Er1 132.6(2) . . ?
N1 N2 Er1 122.1(2) . . ?
C7 N3 N4 112.3(3) . . ?
C7 N3 C1 127.0(3) . . ?
N4 N3 C1 120.3(3) . . ?
C9 N4 N3 104.7(3) . . ?
C9 N4 Er1 132.6(2) . . ?
N3 N4 Er1 122.7(2) . . ?
C12 N5 N6 112.2(3) . . ?
C12 N5 C1 126.9(3) . . ?
N6 N5 C1 120.8(3) . . ?
C14 N6 N5 104.9(3) . . ?
C14 N6 Er1 133.0(2) . . ?
N5 N6 Er1 122.1(2) . . ?
N3 C1 N5 112.7(3) . . ?
N3 C1 N1 111.0(3) . . ?
N5 C1 N1 111.4(3) . . ?
N3 C1 H1A 107.1 . . ?
N5 C1 H1A 107.1 . . ?
N1 C1 H1A 107.1 . . ?
N1 C2 C3 106.2(3) . . ?
N1 C2 C5 122.8(3) . . ?
C3 C2 C5 131.0(3) . . ?
C2 C3 C4 106.8(3) . . ?
C2 C3 H3A 126.6 . . ?
C4 C3 H3A 126.6 . . ?
N2 C4 C3 110.1(3) . . ?
N2 C4 C6 121.8(3) . . ?
C3 C4 C6 128.1(3) . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 C8 105.5(3) . . ?
N3 C7 C10 124.1(3) . . ?
C8 C7 C10 130.4(3) . . ?
C7 C8 C9 106.7(3) . . ?
C7 C8 H8A 126.7 . . ?
C9 C8 H8A 126.7 . . ?
N4 C9 C8 110.8(3) . . ?
N4 C9 C11 121.8(3) . . ?
C8 C9 C11 127.4(3) . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N5 C12 C13 107.0(3) . . ?
N5 C12 C15 123.2(3) . . ?
C13 C12 C15 129.7(3) . . ?
C12 C13 C14 104.6(3) . . ?
C12 C13 H13A 127.7 . . ?
C14 C13 H13A 127.7 . . ?
N6 C14 C13 111.3(3) . . ?
N6 C14 C16 121.5(3) . . ?
C13 C14 C16 127.2(3) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 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 . . ?
N1S C1S C2S 179.2(5) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
N2S C3S C4S 179.3(6) . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?

_refine_diff_density_max         2.113
_refine_diff_density_min         -3.296
_refine_diff_density_rms         0.142

