# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_5
_database_code_depnum_ccdc_archive 'CCDC 1888677'
_audit_update_record
;
2019-01-30 deposited with the CCDC. 2019-03-06 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 'C58 H54 Dy2 F6 N6 O12 S2'
_chemical_formula_weight 1530.19
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_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, -y, -z'
_cell_length_a 11.1327(9)
_cell_length_b 11.7050(11)
_cell_length_c 12.3830(10)
_cell_angle_alpha 99.306(7)
_cell_angle_beta 96.452(7)
_cell_angle_gamma 105.332(7)
_cell_volume 1515.2(2)
_cell_formula_units_Z 1
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 5627
_cell_measurement_theta_min 0.73398
_cell_measurement_theta_max 1.00000
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.677
_exptl_crystal_F_000 758
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.110
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_min 0.100
_exptl_absorpt_coefficient_mu 2.599
_shelx_estimated_absorpt_T_min 0.763
_shelx_estimated_absorpt_T_max 0.781
_exptl_absorpt_correction_type ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using
spherical harmonics,
implemented in SCALE3 ABSPACK
scaling algorithm.
;
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source '\w scans'
_diffrn_measurement_device_type 'Xcalibur, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 17350
_diffrn_reflns_av_unetI/netI 0.0963
_diffrn_reflns_av_R_equivalents 0.0847
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_theta_min 3.022
_diffrn_reflns_theta_max 27.484
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total 6919
_reflns_number_gt 5158
_reflns_threshold_expression 'I > 2\s(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 'CrysAlis PRO (Agilent, 2011)'
_computing_cell_refinement 'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction 'CrysAlis PRO (Agilent, 2011)'
_computing_structure_solution 'CrysAlis PRO (Agilent, 2011)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker 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/[\s^2^(Fo^2^)+(0.0590P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 6919
_refine_ls_number_parameters 394
_refine_ls_number_restraints 10
_refine_ls_R_factor_all 0.0804
_refine_ls_R_factor_gt 0.0536
_refine_ls_wR_factor_ref 0.1369
_refine_ls_wR_factor_gt 0.1208
_refine_ls_goodness_of_fit_ref 1.015
_refine_ls_restrained_S_all 1.016
_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
Dy01 Dy 0.50854(3) 0.62541(2) 0.41407(2) 0.03685(12) Uani 1 1 d D . . . .
S1 S 0.2963(2) 0.2965(3) 0.0780(2) 0.0906(8) Uani 1 1 d . . . . .
O5 O 0.6230(4) 0.5536(4) 0.5512(3) 0.0375(10) Uani 1 1 d . . . . .
O4 O 0.6915(4) 0.6493(4) 0.3396(4) 0.0543(12) Uani 1 1 d . . . . .
O3 O 0.4684(4) 0.4821(4) 0.2495(4) 0.0523(12) Uani 1 1 d . . . . .
O1 O 0.4021(4) 0.6989(4) 0.5557(4) 0.0531(12) Uani 1 1 d D . . . .
H1 H 0.432(4) 0.771(3) 0.594(5) 0.080 Uiso 1 1 d D U . . .
O2 O 0.3572(5) 0.6651(4) 0.2892(4) 0.0525(12) Uani 1 1 d . . . . .
N008 N 0.6845(5) 0.7869(4) 0.5399(4) 0.0374(12) Uani 1 1 d . . . . .
N009 N 0.5330(5) 0.8438(5) 0.3955(4) 0.0410(12) Uani 1 1 d . . . . .
N00A N 0.4457(5) 0.8709(5) 0.3235(5) 0.0463(14) Uani 1 1 d . . . . .
O6 O 0.4742(7) 0.8974(5) 0.7144(5) 0.0756(17) Uani 1 1 d . . . . .
H6 H 0.5106 0.9652 0.7059 0.113 Uiso 1 1 calc R U . . .
C16 C 0.7335(6) 0.6245(6) 0.6097(5) 0.0383(14) Uani 1 1 d . . . . .
C19 C 0.7280(6) 0.5928(6) 0.2587(6) 0.0469(17) Uani 1 1 d . . . . .
C7 C 0.3590(6) 0.7702(6) 0.2735(6) 0.0433(15) Uani 1 1 d . . . . .
C6 C 0.2597(6) 0.7778(6) 0.1849(6) 0.0447(15) Uani 1 1 d . . . . .
C23 C 0.4902(7) 0.3155(6) -0.0270(5) 0.0418(15) Uani 1 1 d . U . . .
H23A H 0.5706 0.3385 -0.0456 0.050 Uiso 1 1 calc R U . . .
C15 C 0.8164(6) 0.5843(6) 0.6722(6) 0.0443(15) Uani 1 1 d . . . . .
H15 H 0.7957 0.5035 0.6784 0.053 Uiso 1 1 calc R U . . .
C17 C 0.7687(6) 0.7494(6) 0.6030(5) 0.0387(14) Uani 1 1 d . . . . .
C20 C 0.6570(7) 0.5001(6) 0.1757(6) 0.0499(17) Uani 1 1 d . . . . .
H20 H 0.6958 0.4679 0.1204 0.060 Uiso 1 1 calc R U . . .
F3 F 0.9133(5) 0.7502(5) 0.2690(7) 0.132(3) Uani 1 1 d . . . . .
C21 C 0.5267(7) 0.4524(6) 0.1722(6) 0.0470(16) Uani 1 1 d . . . . .
C8 C 0.6257(7) 0.9311(6) 0.4513(6) 0.0507(17) Uani 1 1 d . . . . .
H8 H 0.6343 1.0105 0.4437 0.061 Uiso 1 1 calc R U . . .
C14 C 0.9324(7) 0.6638(7) 0.7268(6) 0.0533(18) Uani 1 1 d . . . . .
H14 H 0.9869 0.6339 0.7690 0.064 Uiso 1 1 calc R U . . .
C9 C 0.7158(6) 0.9014(6) 0.5260(6) 0.0453(16) Uani 1 1 d . . . . .
C13 C 0.9692(6) 0.7827(6) 0.7211(6) 0.0528(18) Uani 1 1 d . . . . .
H13 H 1.0469 0.8332 0.7587 0.063 Uiso 1 1 calc R U . . .
C12 C 0.8868(6) 0.8269(6) 0.6571(6) 0.0459(16) Uani 1 1 d . . . . .
C22 C 0.4515(7) 0.3608(6) 0.0759(6) 0.0489(17) Uani 1 1 d . . . . .
C5 C 0.2363(7) 0.8872(7) 0.1760(6) 0.0556(18) Uani 1 1 d . . . . .
H5 H 0.2831 0.9574 0.2260 0.067 Uiso 1 1 calc R U . . .
C1 C 0.1908(7) 0.6750(7) 0.1093(6) 0.0576(19) Uani 1 1 d . . . . .
H1A H 0.2053 0.6011 0.1135 0.069 Uiso 1 1 calc R U . . .
C10 C 0.8322(7) 0.9847(6) 0.5774(6) 0.059(2) Uani 1 1 d . . . . .
H10 H 0.8517 1.0641 0.5671 0.070 Uiso 1 1 calc R U . . .
C11 C 0.9159(7) 0.9484(6) 0.6421(7) 0.058(2) Uani 1 1 d . . . . .
H11 H 0.9926 1.0033 0.6768 0.070 Uiso 1 1 calc R U . . .
C26 C 0.2743(7) 0.6478(7) 0.5771(7) 0.063(2) Uani 1 1 d D . . . .
H26A H 0.2745 0.6582 0.6564 0.075 Uiso 1 1 calc R U . . .
H26B H 0.2455 0.5619 0.5455 0.075 Uiso 1 1 calc R U . . .
F1 F 0.9097(6) 0.5842(7) 0.1785(8) 0.159(4) Uani 1 1 d . . . . .
C2 C 0.0998(8) 0.6826(9) 0.0271(7) 0.070(2) Uani 1 1 d . . . . .
H2 H 0.0531 0.6132 -0.0240 0.084 Uiso 1 1 calc R U . . .
C4 C 0.1452(8) 0.8927(8) 0.0944(7) 0.066(2) Uani 1 1 d . . . . .
H4 H 0.1298 0.9663 0.0902 0.080 Uiso 1 1 calc R U . . .
C3 C 0.0774(8) 0.7918(9) 0.0199(7) 0.069(2) Uani 1 1 d . . . . .
H3 H 0.0163 0.7961 -0.0358 0.083 Uiso 1 1 calc R U . . .
C24 C 0.3843(9) 0.2317(8) -0.0921(8) 0.078(2) Uani 1 1 d . U . . .
H24 H 0.3875 0.1913 -0.1624 0.094 Uiso 1 1 calc R U . . .
F2 F 0.9298(6) 0.6100(10) 0.3471(8) 0.173(4) Uani 1 1 d . . . . .
C18 C 0.8710(8) 0.6354(10) 0.2649(9) 0.077(3) Uani 1 1 d . . . . .
C25 C 0.2783(10) 0.2116(8) -0.0495(8) 0.082(3) Uani 1 1 d . . . . .
H25 H 0.2023 0.1567 -0.0861 0.099 Uiso 1 1 calc R U . . .
C28 C 0.4691(10) 0.8997(11) 0.8283(10) 0.101(4) Uani 1 1 d . . . . .
H28A H 0.5093 0.8412 0.8508 0.122 Uiso 1 1 calc R U . . .
H28B H 0.5194 0.9789 0.8694 0.122 Uiso 1 1 calc R U . . .
C27 C 0.1876(9) 0.7083(9) 0.5279(9) 0.091(3) Uani 1 1 d . . . . .
H27A H 0.1949 0.7062 0.4511 0.136 Uiso 1 1 calc R U . . .
H27B H 0.2090 0.7907 0.5666 0.136 Uiso 1 1 calc R U . . .
H27C H 0.1025 0.6672 0.5339 0.136 Uiso 1 1 calc R U . . .
C29 C 0.3496(12) 0.8756(12) 0.8603(12) 0.137(5) Uani 1 1 d . . . . .
H29A H 0.3036 0.9252 0.8302 0.206 Uiso 1 1 calc R U . . .
H29B H 0.3589 0.8932 0.9398 0.206 Uiso 1 1 calc R U . . .
H29C H 0.3043 0.7919 0.8329 0.206 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy01 0.03934(19) 0.03346(17) 0.03573(18) 0.01163(13) 0.00447(12) 0.00493(12)
S1 0.0759(16) 0.0972(19) 0.0757(17) -0.0119(15) 0.0153(13) 0.0019(14)
O5 0.033(2) 0.036(2) 0.040(2) 0.0140(19) -0.0017(18) 0.0040(18)
O4 0.046(3) 0.060(3) 0.050(3) 0.005(3) 0.013(2) 0.004(2)
O3 0.048(3) 0.056(3) 0.044(3) 0.003(2) 0.013(2) 0.002(2)
O1 0.048(3) 0.045(3) 0.063(3) 0.005(2) 0.018(2) 0.007(2)
O2 0.059(3) 0.042(3) 0.052(3) 0.018(2) -0.004(2) 0.009(2)
N008 0.042(3) 0.035(3) 0.034(3) 0.012(2) 0.005(2) 0.006(2)
N009 0.044(3) 0.034(3) 0.041(3) 0.010(2) 0.000(2) 0.005(2)
N00A 0.052(3) 0.046(3) 0.044(3) 0.023(3) 0.003(3) 0.011(3)
O6 0.123(5) 0.037(3) 0.059(4) 0.013(3) 0.009(3) 0.011(3)
C16 0.039(3) 0.043(3) 0.034(3) 0.013(3) 0.011(3) 0.008(3)
C19 0.041(4) 0.053(4) 0.054(4) 0.028(4) 0.015(3) 0.012(3)
C7 0.047(4) 0.040(4) 0.046(4) 0.019(3) 0.009(3) 0.010(3)
C6 0.042(4) 0.053(4) 0.045(4) 0.021(3) 0.010(3) 0.014(3)
C23 0.058(4) 0.035(3) 0.032(3) 0.005(3) 0.004(3) 0.014(3)
C15 0.040(4) 0.044(4) 0.051(4) 0.018(3) 0.009(3) 0.010(3)
C17 0.038(3) 0.040(3) 0.034(3) 0.008(3) 0.004(3) 0.004(3)
C20 0.052(4) 0.053(4) 0.048(4) 0.012(4) 0.019(3) 0.015(4)
F3 0.073(4) 0.082(4) 0.220(9) 0.013(5) 0.048(5) -0.016(3)
C21 0.062(5) 0.042(4) 0.040(4) 0.013(3) 0.012(3) 0.016(3)
C8 0.064(5) 0.034(3) 0.054(4) 0.016(3) 0.000(4) 0.013(3)
C14 0.044(4) 0.058(4) 0.061(5) 0.025(4) 0.001(3) 0.015(3)
C9 0.048(4) 0.036(3) 0.047(4) 0.008(3) 0.003(3) 0.004(3)
C13 0.038(4) 0.053(4) 0.059(5) 0.010(4) -0.006(3) 0.005(3)
C12 0.042(4) 0.044(4) 0.046(4) 0.008(3) 0.003(3) 0.005(3)
C22 0.058(4) 0.045(4) 0.046(4) 0.016(3) 0.009(3) 0.015(3)
C5 0.059(5) 0.057(5) 0.049(4) 0.015(4) 0.001(4) 0.014(4)
C1 0.054(4) 0.060(5) 0.055(5) 0.020(4) 0.005(4) 0.005(4)
C10 0.063(5) 0.037(4) 0.063(5) 0.018(4) -0.006(4) -0.005(3)
C11 0.054(4) 0.046(4) 0.059(5) 0.014(4) -0.008(4) -0.005(3)
C26 0.064(5) 0.057(5) 0.066(5) 0.004(4) 0.025(4) 0.016(4)
F1 0.081(5) 0.169(7) 0.192(8) -0.041(6) 0.079(5) 0.000(4)
C2 0.062(5) 0.088(6) 0.052(5) 0.021(5) 0.002(4) 0.008(5)
C4 0.071(6) 0.081(6) 0.064(5) 0.032(5) 0.007(4) 0.041(5)
C3 0.064(5) 0.106(7) 0.044(4) 0.031(5) 0.001(4) 0.027(5)
C24 0.089(4) 0.074(4) 0.068(4) 0.010(3) 0.017(4) 0.018(3)
F2 0.059(4) 0.294(12) 0.172(8) 0.112(8) -0.005(4) 0.034(5)
C18 0.052(5) 0.089(7) 0.077(7) 0.011(6) 0.017(5) 0.004(5)
C25 0.085(7) 0.065(6) 0.073(6) -0.014(5) -0.007(5) 0.004(5)
C28 0.085(7) 0.113(9) 0.100(9) 0.056(7) 0.005(6) 0.002(6)
C27 0.080(7) 0.102(8) 0.098(8) 0.026(7) 0.014(6) 0.035(6)
C29 0.113(10) 0.144(12) 0.152(13) 0.004(10) 0.062(10) 0.030(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy01 O4 2.298(5) . ?
Dy01 O3 2.337(5) . ?
Dy01 O2 2.347(5) . ?
Dy01 O5 2.352(4) 2_666 ?
Dy01 O1 2.395(5) . ?
Dy01 O5 2.399(4) . ?
Dy01 N008 2.498(5) . ?
Dy01 N009 2.549(5) . ?
Dy01 Dy01 3.8732(6) 2_666 ?
S1 C25 1.685(9) . ?
S1 C22 1.697(8) . ?
O5 C16 1.339(7) . ?
O5 Dy01 2.352(4) 2_666 ?
O4 C19 1.275(8) . ?
O3 C21 1.269(8) . ?
O1 C26 1.463(8) . ?
O2 C7 1.271(7) . ?
N008 C9 1.337(8) . ?
N008 C17 1.359(8) . ?
N009 C8 1.280(8) . ?
N009 N00A 1.378(7) . ?
N00A C7 1.316(8) . ?
O6 C28 1.414(12) . ?
C16 C15 1.364(9) . ?
C16 C17 1.429(8) . ?
C19 C20 1.365(10) . ?
C19 C18 1.526(11) . ?
C7 C6 1.498(9) . ?
C6 C1 1.378(10) . ?
C6 C5 1.391(9) . ?
C23 C24 1.386(11) . ?
C23 C22 1.455(9) . ?
C15 C14 1.398(9) . ?
C17 C12 1.406(9) . ?
C20 C21 1.403(10) . ?
F3 C18 1.292(11) . ?
C21 C22 1.470(10) . ?
C8 C9 1.436(9) . ?
C14 C13 1.359(10) . ?
C9 C10 1.408(9) . ?
C13 C12 1.399(9) . ?
C12 C11 1.420(9) . ?
C5 C4 1.371(10) . ?
C1 C2 1.384(11) . ?
C10 C11 1.357(10) . ?
C26 C27 1.473(12) . ?
F1 C18 1.312(11) . ?
C2 C3 1.380(11) . ?
C4 C3 1.356(12) . ?
C24 C25 1.326(13) . ?
F2 C18 1.267(12) . ?
C28 C29 1.402(14) . ?
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
O4 Dy01 O3 71.57(16) . . ?
O4 Dy01 O2 108.18(18) . . ?
O3 Dy01 O2 71.91(17) . . ?
O4 Dy01 O5 127.77(16) . 2_666 ?
O3 Dy01 O5 74.06(16) . 2_666 ?
O2 Dy01 O5 96.83(15) . 2_666 ?
O4 Dy01 O1 147.46(17) . . ?
O3 Dy01 O1 140.76(17) . . ?
O2 Dy01 O1 85.67(18) . . ?
O5 Dy01 O1 77.27(15) 2_666 . ?
O4 Dy01 O5 82.78(16) . . ?
O3 Dy01 O5 106.53(16) . . ?
O2 Dy01 O5 167.18(15) . . ?
O5 Dy01 O5 70.76(15) 2_666 . ?
O1 Dy01 O5 88.32(16) . . ?
O4 Dy01 N008 69.86(16) . . ?
O3 Dy01 N008 141.33(17) . . ?
O2 Dy01 N008 123.52(16) . . ?
O5 Dy01 N008 130.09(15) 2_666 . ?
O1 Dy01 N008 77.91(16) . . ?
O5 Dy01 N008 65.90(15) . . ?
O4 Dy01 N009 84.54(18) . . ?
O3 Dy01 N009 116.83(17) . . ?
O2 Dy01 N009 61.54(16) . . ?
O5 Dy01 N009 146.88(16) 2_666 . ?
O1 Dy01 N009 76.39(17) . . ?
O5 Dy01 N009 127.76(15) . . ?
N008 Dy01 N009 62.13(16) . . ?
O4 Dy01 Dy01 107.09(13) . 2_666 ?
O3 Dy01 Dy01 90.54(12) . 2_666 ?
O2 Dy01 Dy01 132.54(12) . 2_666 ?
O5 Dy01 Dy01 35.79(10) 2_666 2_666 ?
O1 Dy01 Dy01 81.26(12) . 2_666 ?
O5 Dy01 Dy01 34.98(9) . 2_666 ?
N008 Dy01 Dy01 97.94(11) . 2_666 ?
N009 Dy01 Dy01 152.59(12) . 2_666 ?
C25 S1 C22 91.3(4) . . ?
C16 O5 Dy01 128.9(4) . 2_666 ?
C16 O5 Dy01 120.4(4) . . ?
Dy01 O5 Dy01 109.24(15) 2_666 . ?
C19 O4 Dy01 136.1(4) . . ?
C21 O3 Dy01 138.4(5) . . ?
C26 O1 Dy01 129.3(4) . . ?
C7 O2 Dy01 124.1(4) . . ?
C9 N008 C17 119.0(6) . . ?
C9 N008 Dy01 122.0(4) . . ?
C17 N008 Dy01 116.6(4) . . ?
C8 N009 N00A 118.0(5) . . ?
C8 N009 Dy01 121.8(4) . . ?
N00A N009 Dy01 120.2(4) . . ?
C7 N00A N009 109.1(5) . . ?
O5 C16 C15 124.2(6) . . ?
O5 C16 C17 117.8(6) . . ?
C15 C16 C17 118.0(6) . . ?
O4 C19 C20 128.3(6) . . ?
O4 C19 C18 112.0(7) . . ?
C20 C19 C18 119.6(7) . . ?
O2 C7 N00A 125.1(6) . . ?
O2 C7 C6 116.8(6) . . ?
N00A C7 C6 117.9(6) . . ?
C1 C6 C5 118.9(7) . . ?
C1 C6 C7 119.7(6) . . ?
C5 C6 C7 121.4(6) . . ?
C24 C23 C22 106.8(7) . . ?
C16 C15 C14 120.3(6) . . ?
N008 C17 C12 122.7(6) . . ?
N008 C17 C16 116.7(5) . . ?
C12 C17 C16 120.5(6) . . ?
C19 C20 C21 121.2(6) . . ?
O3 C21 C20 123.7(7) . . ?
O3 C21 C22 116.8(6) . . ?
C20 C21 C22 119.5(6) . . ?
N009 C8 C9 117.3(6) . . ?
C13 C14 C15 123.1(7) . . ?
N008 C9 C10 121.7(6) . . ?
N008 C9 C8 115.5(6) . . ?
C10 C9 C8 122.8(6) . . ?
C14 C13 C12 118.1(7) . . ?
C13 C12 C17 119.9(6) . . ?
C13 C12 C11 123.4(7) . . ?
C17 C12 C11 116.6(6) . . ?
C23 C22 C21 129.0(7) . . ?
C23 C22 S1 112.3(5) . . ?
C21 C22 S1 118.7(5) . . ?
C4 C5 C6 120.7(8) . . ?
C6 C1 C2 119.6(8) . . ?
C11 C10 C9 119.5(6) . . ?
C10 C11 C12 120.3(7) . . ?
O1 C26 C27 110.2(7) . . ?
C3 C2 C1 120.8(8) . . ?
C3 C4 C5 120.5(8) . . ?
C4 C3 C2 119.6(8) . . ?
C25 C24 C23 117.0(9) . . ?
F2 C18 F3 108.2(10) . . ?
F2 C18 F1 104.5(10) . . ?
F3 C18 F1 105.2(9) . . ?
F2 C18 C19 112.7(8) . . ?
F3 C18 C19 112.7(8) . . ?
F1 C18 C19 113.0(8) . . ?
C24 C25 S1 112.5(8) . . ?
C29 C28 O6 117.3(11) . . ?
_refine_diff_density_max 2.508
_refine_diff_density_min -1.510
_refine_diff_density_rms 0.159
_shelx_res_file
;
yzf-247-666.res created by SHELXL-2014/7
TITL yzf-247-666_a.res in P-1
REM Old TITL yzf-247-666 in P1
REM SHELXT solution in P-1
REM R1 0.128, Rweak 0.004, Alpha 0.045, Orientation as input
REM Formula found by SHELXT: C27 N6 O4 Dy S F4
CELL 0.71073 11.1327 11.705 12.383 99.306 96.452 105.332
ZERR 1 0.0009 0.0011 0.001 0.007 0.007 0.007
LATT 1
SFAC C H Dy F N O S
UNIT 58 54 2 6 6 12 2
DFIX 0.85 0.01 O1 H1
DANG 1.923173 0.02 C26 H1
DANG 2.940276 0.02 Dy01 H1
L.S. 5
PLAN 5
SIZE 0.1 0.11 0.1
TEMP 19.85
list 4
fmap 2
ACTA
delu 0.01 0.005 c23 c24
isor 0.005 c24
WGHT 0.059000
FVAR 0.35096
DY01 3 0.508539 0.625408 0.414066 11.00000 0.03934 0.03346 =
0.03573 0.01163 0.00447 0.00493
S1 7 0.296303 0.296520 0.078047 11.00000 0.07587 0.09721 =
0.07573 -0.01194 0.01527 0.00188
O5 6 0.622964 0.553615 0.551215 11.00000 0.03293 0.03640 =
0.03996 0.01402 -0.00169 0.00404
O4 6 0.691521 0.649314 0.339604 11.00000 0.04627 0.05964 =
0.04995 0.00502 0.01332 0.00435
O3 6 0.468364 0.482067 0.249471 11.00000 0.04794 0.05599 =
0.04392 0.00345 0.01275 0.00153
O1 6 0.402088 0.698950 0.555654 11.00000 0.04768 0.04477 =
0.06313 0.00466 0.01793 0.00692
H1 2 0.431580 0.770817 0.593970 11.00000 -1.50000
O2 6 0.357219 0.665147 0.289191 11.00000 0.05947 0.04230 =
0.05199 0.01794 -0.00400 0.00867
N008 5 0.684472 0.786904 0.539903 11.00000 0.04190 0.03500 =
0.03387 0.01231 0.00503 0.00571
N009 5 0.533010 0.843810 0.395518 11.00000 0.04354 0.03401 =
0.04099 0.00988 0.00001 0.00476
N00A 5 0.445689 0.870867 0.323523 11.00000 0.05177 0.04580 =
0.04365 0.02289 0.00335 0.01125
O6 6 0.474189 0.897356 0.714357 11.00000 0.12349 0.03695 =
0.05901 0.01297 0.00925 0.01079
AFIX 147
H6 2 0.510605 0.965199 0.705858 11.00000 -1.50000
AFIX 0
C16 1 0.733519 0.624489 0.609697 11.00000 0.03897 0.04254 =
0.03423 0.01291 0.01078 0.00817
C19 1 0.727981 0.592834 0.258690 11.00000 0.04086 0.05342 =
0.05367 0.02830 0.01511 0.01243
C7 1 0.358974 0.770181 0.273495 11.00000 0.04700 0.04013 =
0.04558 0.01852 0.00937 0.01040
C6 1 0.259670 0.777806 0.184887 11.00000 0.04208 0.05250 =
0.04450 0.02140 0.01040 0.01397
C23 1 0.490223 0.315532 -0.027005 11.00000 0.05750 0.03466 =
0.03249 0.00503 0.00417 0.01425
AFIX 43
H23A 2 0.570607 0.338452 -0.045571 11.00000 -1.20000
AFIX 0
C15 1 0.816428 0.584251 0.672152 11.00000 0.04007 0.04436 =
0.05098 0.01818 0.00893 0.01046
AFIX 43
H15 2 0.795749 0.503517 0.678448 11.00000 -1.20000
AFIX 0
C17 1 0.768691 0.749425 0.603050 11.00000 0.03819 0.03976 =
0.03353 0.00786 0.00415 0.00360
C20 1 0.657046 0.500080 0.175675 11.00000 0.05239 0.05282 =
0.04761 0.01202 0.01868 0.01487
AFIX 43
H20 2 0.695781 0.467911 0.120411 11.00000 -1.20000
AFIX 0
F3 4 0.913295 0.750228 0.269004 11.00000 0.07283 0.08185 =
0.22018 0.01256 0.04830 -0.01557
C21 1 0.526732 0.452388 0.172211 11.00000 0.06198 0.04182 =
0.04040 0.01259 0.01190 0.01623
C8 1 0.625662 0.931072 0.451262 11.00000 0.06358 0.03412 =
0.05369 0.01552 0.00043 0.01279
AFIX 43
H8 2 0.634294 1.010469 0.443654 11.00000 -1.20000
AFIX 0
C14 1 0.932400 0.663775 0.726785 11.00000 0.04372 0.05798 =
0.06100 0.02475 0.00125 0.01475
AFIX 43
H14 2 0.986934 0.633852 0.769003 11.00000 -1.20000
AFIX 0
C9 1 0.715751 0.901429 0.526032 11.00000 0.04782 0.03576 =
0.04661 0.00790 0.00289 0.00439
C13 1 0.969205 0.782670 0.721130 11.00000 0.03845 0.05314 =
0.05852 0.00996 -0.00585 0.00527
AFIX 43
H13 2 1.046914 0.833203 0.758736 11.00000 -1.20000
AFIX 0
C12 1 0.886846 0.826911 0.657108 11.00000 0.04212 0.04402 =
0.04606 0.00775 0.00337 0.00542
C22 1 0.451470 0.360802 0.075923 11.00000 0.05813 0.04523 =
0.04630 0.01626 0.00931 0.01520
C5 1 0.236343 0.887231 0.176011 11.00000 0.05881 0.05742 =
0.04894 0.01492 0.00095 0.01439
AFIX 43
H5 2 0.283056 0.957388 0.225954 11.00000 -1.20000
AFIX 0
C1 1 0.190753 0.675033 0.109273 11.00000 0.05381 0.05978 =
0.05459 0.01992 0.00529 0.00499
AFIX 43
H1A 2 0.205289 0.601082 0.113473 11.00000 -1.20000
AFIX 0
C10 1 0.832206 0.984723 0.577422 11.00000 0.06264 0.03709 =
0.06334 0.01781 -0.00640 -0.00503
AFIX 43
H10 2 0.851677 1.064121 0.567130 11.00000 -1.20000
AFIX 0
C11 1 0.915883 0.948362 0.642101 11.00000 0.05409 0.04647 =
0.05945 0.01368 -0.00759 -0.00498
AFIX 43
H11 2 0.992608 1.003271 0.676753 11.00000 -1.20000
AFIX 0
C26 1 0.274253 0.647838 0.577051 11.00000 0.06409 0.05669 =
0.06650 0.00357 0.02486 0.01582
AFIX 23
H26A 2 0.274548 0.658161 0.656407 11.00000 -1.20000
H26B 2 0.245523 0.561937 0.545463 11.00000 -1.20000
AFIX 0
F1 4 0.909690 0.584237 0.178474 11.00000 0.08142 0.16913 =
0.19216 -0.04051 0.07924 -0.00034
C2 1 0.099776 0.682568 0.027051 11.00000 0.06196 0.08763 =
0.05239 0.02144 0.00223 0.00796
AFIX 43
H2 2 0.053149 0.613220 -0.023950 11.00000 -1.20000
AFIX 0
C4 1 0.145206 0.892747 0.094407 11.00000 0.07109 0.08097 =
0.06389 0.03245 0.00694 0.04136
AFIX 43
H4 2 0.129765 0.966325 0.090172 11.00000 -1.20000
AFIX 0
C3 1 0.077440 0.791760 0.019856 11.00000 0.06382 0.10639 =
0.04359 0.03143 0.00065 0.02729
AFIX 43
H3 2 0.016276 0.796059 -0.035790 11.00000 -1.20000
AFIX 0
C24 1 0.384299 0.231679 -0.092067 11.00000 0.08920 0.07361 =
0.06775 0.00967 0.01708 0.01838
AFIX 43
H24 2 0.387451 0.191334 -0.162376 11.00000 -1.20000
AFIX 0
F2 4 0.929812 0.610039 0.347128 11.00000 0.05931 0.29441 =
0.17223 0.11219 -0.00472 0.03370
C18 1 0.870992 0.635360 0.264880 11.00000 0.05244 0.08926 =
0.07749 0.01082 0.01725 0.00355
C25 1 0.278256 0.211569 -0.049546 11.00000 0.08467 0.06516 =
0.07291 -0.01379 -0.00654 0.00435
AFIX 43
H25 2 0.202339 0.156664 -0.086097 11.00000 -1.20000
AFIX 0
C28 1 0.469141 0.899656 0.828253 11.00000 0.08542 0.11329 =
0.09957 0.05599 0.00486 0.00234
AFIX 23
H28A 2 0.509270 0.841229 0.850845 11.00000 -1.20000
H28B 2 0.519351 0.978858 0.869428 11.00000 -1.20000
AFIX 0
C27 1 0.187638 0.708258 0.527884 11.00000 0.08002 0.10219 =
0.09779 0.02621 0.01388 0.03534
AFIX 137
H27A 2 0.194946 0.706242 0.451132 11.00000 -1.50000
H27B 2 0.209023 0.790730 0.566608 11.00000 -1.50000
H27C 2 0.102480 0.667189 0.533858 11.00000 -1.50000
AFIX 0
C29 1 0.349559 0.875587 0.860319 11.00000 0.11343 0.14404 =
0.15165 0.00356 0.06205 0.03048
AFIX 137
H29A 2 0.303601 0.925171 0.830226 11.00000 -1.50000
H29B 2 0.358898 0.893208 0.939781 11.00000 -1.50000
H29C 2 0.304303 0.791902 0.832903 11.00000 -1.50000
AFIX 0
HKLF 4
REM yzf-247-666_a.res in P-1
REM R1 = 0.0536 for 5158 Fo > 4sig(Fo) and 0.0804 for all 6919 data
REM 394 parameters refined using 10 restraints
END
WGHT 0.0590 0.0000
REM Highest difference peak 2.508, deepest hole -1.510, 1-sigma level 0.159
Q1 1 0.5271 0.8756 0.2440 11.00000 0.05 2.51
Q2 1 0.5991 0.6332 0.4117 11.00000 0.05 1.71
Q3 1 0.4371 0.6432 0.4548 11.00000 0.05 1.60
Q4 1 0.4249 0.6020 0.3801 11.00000 0.05 1.55
Q5 1 0.4399 0.5848 0.3593 11.00000 0.05 1.43
;
_shelx_res_checksum 35263
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_6
_database_code_depnum_ccdc_archive 'CCDC 1888679'
_audit_update_record
;
2019-01-30 deposited with the CCDC. 2019-03-06 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 'C68 H56 Dy2 N6 O10'
_chemical_formula_weight 1442.18
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 24.7131(14)
_cell_length_b 18.3426(8)
_cell_length_c 27.265(3)
_cell_angle_alpha 90
_cell_angle_beta 101.707(7)
_cell_angle_gamma 90
_cell_volume 12102.0(14)
_cell_formula_units_Z 8
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 8107
_cell_measurement_theta_min 3.0029
_cell_measurement_theta_max 29.2094
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.583
_exptl_crystal_F_000 5744
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.150
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_min 0.100
_exptl_absorpt_coefficient_mu 2.516
_shelx_estimated_absorpt_T_min 0.58010
_shelx_estimated_absorpt_T_max 1.00000
_exptl_absorpt_correction_type ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using
spherical harmonics,
implemented in SCALE3 ABSPACK
scaling algorithm.
;
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source '\w scans'
_diffrn_measurement_device_type 'Xcalibur, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 70013
_diffrn_reflns_av_unetI/netI 0.1046
_diffrn_reflns_av_R_equivalents 0.0585
_diffrn_reflns_limit_h_min -33
_diffrn_reflns_limit_h_max 33
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_limit_l_max 34
_diffrn_reflns_theta_min 3.009
_diffrn_reflns_theta_max 29.274
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total 28333
_reflns_number_gt 15417
_reflns_threshold_expression 'I > 2\s(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 'CrysAlis PRO (Agilent, 2011)'
_computing_cell_refinement 'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction 'CrysAlis PRO (Agilent, 2011)'
_computing_structure_solution 'CrysAlis PRO (Agilent, 2011)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker 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/[\s^2^(Fo^2^)+(0.0608P)^2^+59.5499P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 28333
_refine_ls_number_parameters 1564
_refine_ls_number_restraints 2706
_refine_ls_R_factor_all 0.1431
_refine_ls_R_factor_gt 0.0733
_refine_ls_wR_factor_ref 0.2009
_refine_ls_wR_factor_gt 0.1546
_refine_ls_goodness_of_fit_ref 1.027
_refine_ls_restrained_S_all 1.006
_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 0.68982(2) 0.51186(2) 0.41723(2) 0.03888(12) Uani 1 1 d D . . . .
Dy2 Dy 0.55646(2) 0.46195(2) 0.32502(2) 0.03764(12) Uani 1 1 d D . . . .
Dy3 Dy 0.80140(2) 0.03651(2) 0.57040(2) 0.04284(13) Uani 1 1 d D . . . .
Dy4 Dy 0.93692(2) -0.00007(2) 0.66411(2) 0.04698(14) Uani 1 1 d D . . . .
O7 O 0.6284(2) 0.5482(3) 0.3425(2) 0.0401(14) Uani 1 1 d . . . . .
O2 O 0.6226(2) 0.4197(3) 0.3953(2) 0.0400(14) Uani 1 1 d . . . . .
O12 O 0.8752(2) -0.0466(3) 0.5925(2) 0.0468(16) Uani 1 1 d . . . . .
O5 O 0.7012(3) 0.5050(3) 0.5030(2) 0.0520(17) Uani 1 1 d . . . . .
O10 O 0.6194(2) 0.3907(3) 0.2933(2) 0.0456(15) Uani 1 1 d . . . . .
O4 O 0.6254(2) 0.5892(3) 0.4436(2) 0.0438(15) Uani 1 1 d . . . . .
O13 O 0.7766(3) -0.0079(4) 0.6471(2) 0.0573(17) Uani 1 1 d D U . . .
H13 H 0.792(3) -0.045(3) 0.6634(15) 0.086 Uiso 1 1 d D U . . .
O6 O 0.5011(3) 0.3628(3) 0.3252(3) 0.0530(17) Uani 1 1 d . . . . .
O11 O 0.7438(3) 0.1341(3) 0.5681(3) 0.0548(18) Uani 1 1 d . . . . .
O9 O 0.5366(3) 0.4703(4) 0.2399(2) 0.0563(18) Uani 1 1 d . . . . .
O17 O 0.8669(2) 0.0876(3) 0.6385(2) 0.0491(16) Uani 1 1 d . . . . .
O19 O 0.8726(2) -0.0719(3) 0.6951(3) 0.0534(17) Uani 1 1 d . . . . .
O8 O 0.5310(3) 0.5134(4) 0.4002(3) 0.0625(18) Uani 1 1 d D U . . .
H8 H 0.548(3) 0.549(3) 0.417(2) 0.094 Uiso 1 1 d D U . . .
O1 O 0.7405(3) 0.6150(3) 0.4209(3) 0.0606(19) Uani 1 1 d . . . . .
O16 O 0.9888(3) -0.1022(3) 0.6750(3) 0.063(2) Uani 1 1 d . . . . .
O20 O 0.9526(3) 0.0147(3) 0.7502(3) 0.0569(18) Uani 1 1 d . . . . .
O14 O 0.8640(3) 0.1019(3) 0.5338(2) 0.0539(17) Uani 1 1 d . . . . .
N8 N 0.6989(3) 0.0137(4) 0.5499(3) 0.0454(19) Uani 1 1 d . . . . .
N4 N 0.5243(3) 0.5881(4) 0.3057(3) 0.0423(18) Uani 1 1 d . . . . .
O18 O 0.9666(3) 0.0364(4) 0.5877(3) 0.075(2) Uani 1 1 d D U . . .
H18 H 0.942(2) 0.024(6) 0.5626(5) 0.113 Uiso 1 1 d D U . . .
N7 N 0.7728(3) -0.0900(4) 0.5559(3) 0.0465(19) Uani 1 1 d . . . . .
O15 O 0.7780(3) 0.0223(4) 0.4844(3) 0.063(2) Uani 1 1 d . . . . .
N5 N 0.4539(3) 0.4817(4) 0.3029(3) 0.0413(18) Uani 1 1 d . . . . .
N10 N 0.9708(3) 0.1246(4) 0.6782(3) 0.053(2) Uani 1 1 d . . . . .
O3 O 0.7213(3) 0.4615(5) 0.3443(3) 0.073(2) Uani 1 1 d D U . . .
H3 H 0.703(3) 0.480(5) 0.3168(6) 0.110 Uiso 1 1 d D U . . .
N6 N 0.4176(3) 0.4236(4) 0.3059(3) 0.050(2) Uani 1 1 d . . . . .
N9 N 0.6621(3) 0.0701(4) 0.5501(3) 0.0479(19) Uani 1 1 d . . . . .
N3 N 0.8257(3) 0.5628(4) 0.4519(3) 0.059(2) Uani 1 1 d . . . . .
C34 C 0.6196(4) 0.6175(5) 0.3259(4) 0.0539(13) Uani 1 1 d . U . . .
C33 C 0.5639(4) 0.6389(5) 0.3078(4) 0.0536(12) Uani 1 1 d . U . . .
N11 N 1.0394(3) 0.0153(4) 0.6937(3) 0.055(2) Uani 1 1 d . . . . .
N1 N 0.7260(3) 0.3898(4) 0.4427(3) 0.0451(19) Uani 1 1 d . . . . .
N2 N 0.7922(3) 0.5021(4) 0.4501(3) 0.050(2) Uani 1 1 d . . . . .
C66 C 0.8670(4) -0.1171(5) 0.5787(4) 0.0592(13) Uani 1 1 d . U . . .
C75 C 0.6907(5) 0.1302(6) 0.5609(4) 0.0670(13) Uani 1 1 d . U . . .
C58 C 0.6217(4) 0.3618(5) 0.2512(4) 0.0514(12) Uani 1 1 d . U . . .
C55 C 0.5237(4) 0.4727(5) 0.1525(4) 0.0486(12) Uani 1 1 d . U . . .
C101 C 0.9340(4) 0.1792(6) 0.6658(4) 0.0663(12) Uani 1 1 d . U . . .
C38 C 0.5498(4) 0.7117(5) 0.2924(4) 0.0549(13) Uani 1 1 d . U . . .
C59 C 0.6572(4) 0.2954(5) 0.2531(4) 0.0536(13) Uani 1 1 d . U . . .
C87 C 0.7632(5) 0.0119(6) 0.3984(4) 0.0633(13) Uani 1 1 d . U . . .
C44 C 0.4192(5) 0.2976(6) 0.3291(4) 0.0679(15) Uani 1 1 d . U . . .
C26 C 0.6255(4) 0.6244(5) 0.4834(4) 0.0507(12) Uani 1 1 d . U . . .
C56 C 0.5523(4) 0.4430(5) 0.2029(4) 0.0482(12) Uani 1 1 d . U . . .
C23 C 0.7203(4) 0.5233(5) 0.5892(4) 0.0522(13) Uani 1 1 d . U . . .
C24 C 0.6910(4) 0.5423(5) 0.5379(4) 0.0519(12) Uani 1 1 d . U . . .
C27 C 0.5945(4) 0.6943(5) 0.4788(4) 0.0526(13) Uani 1 1 d . U . . .
C49 C 0.4489(5) 0.2335(6) 0.3376(4) 0.0692(15) Uani 1 1 d . U . . .
H49 H 0.4863 0.2334 0.3366 0.083 Uiso 1 1 calc R U . . .
C90 C 0.8667(4) 0.1251(6) 0.4894(4) 0.0629(12) Uani 1 1 d . U . . .
C74 C 0.6801(4) -0.0502(5) 0.5380(4) 0.0592(14) Uani 1 1 d . U . . .
H74 H 0.6424 -0.0585 0.5278 0.071 Uiso 1 1 calc R U . . .
C35 C 0.6596(4) 0.6680(5) 0.3244(4) 0.0564(14) Uani 1 1 d . U . . .
H35 H 0.6966 0.6547 0.3333 0.068 Uiso 1 1 calc R U . . .
C43 C 0.4486(5) 0.3653(6) 0.3192(4) 0.0682(14) Uani 1 1 d . U . . .
C37 C 0.5927(4) 0.7620(5) 0.2947(4) 0.0564(13) Uani 1 1 d . U . . .
H37 H 0.5849 0.8104 0.2859 0.068 Uiso 1 1 calc R U . . .
C25 C 0.6546(4) 0.6027(5) 0.5304(4) 0.0504(12) Uani 1 1 d . U . . .
H25 H 0.6498 0.6293 0.5583 0.060 Uiso 1 1 calc R U . . .
C54 C 0.5501(4) 0.4781(5) 0.1119(4) 0.0489(12) Uani 1 1 d . U . . .
H54 H 0.5856 0.4598 0.1138 0.059 Uiso 1 1 calc R U . . .
C57 C 0.5911(4) 0.3871(5) 0.2060(4) 0.0508(11) Uani 1 1 d . U . . .
H57 H 0.5967 0.3658 0.1765 0.061 Uiso 1 1 calc R U . . .
C1 C 0.6344(5) 0.3505(5) 0.4103(4) 0.0624(12) Uani 1 1 d . U . . .
C73 C 0.7199(4) -0.1097(5) 0.5410(4) 0.0573(14) Uani 1 1 d . U . . .
C22 C 0.6953(4) 0.5262(5) 0.6298(4) 0.0546(13) Uani 1 1 d . U . . .
H22 H 0.6591 0.5426 0.6261 0.066 Uiso 1 1 calc R U . . .
C53 C 0.5223(4) 0.5112(5) 0.0693(4) 0.0513(13) Uani 1 1 d . U . . .
H53 H 0.5399 0.5158 0.0424 0.062 Uiso 1 1 calc R U . . .
N12 N 1.0733(4) -0.0457(5) 0.7024(4) 0.069(3) Uani 1 1 d . . . . .
C11 C 0.7938(5) 0.6183(6) 0.4339(5) 0.0776(16) Uani 1 1 d . U . . .
C50 C 0.4702(4) 0.5010(5) 0.1482(4) 0.0514(12) Uani 1 1 d . U . . .
H50 H 0.4523 0.4991 0.1750 0.062 Uiso 1 1 calc R U . . .
C97 C 0.8779(4) 0.1592(6) 0.6466(4) 0.0659(13) Uani 1 1 d . U . . .
C122 C 0.8745(4) -0.1044(6) 0.7356(4) 0.0644(14) Uani 1 1 d . U . . .
C52 C 0.4712(4) 0.5372(5) 0.0645(4) 0.0523(14) Uani 1 1 d . U . . .
H52 H 0.4538 0.5591 0.0347 0.063 Uiso 1 1 calc R U . . .
C36 C 0.6454(4) 0.7399(5) 0.3095(4) 0.0576(14) Uani 1 1 d . U . . .
H36 H 0.6736 0.7737 0.3100 0.069 Uiso 1 1 calc R U . . .
C88 C 0.7937(5) 0.0450(6) 0.4461(4) 0.0623(12) Uani 1 1 d . U . . .
C32 C 0.5890(4) 0.7336(5) 0.4353(4) 0.0555(13) Uani 1 1 d . U . . .
H32 H 0.6018 0.7140 0.4083 0.067 Uiso 1 1 calc R U . . .
C41 C 0.4715(4) 0.6037(5) 0.2902(4) 0.0553(13) Uani 1 1 d . U . . .
C51 C 0.4446(4) 0.5317(5) 0.1033(4) 0.0528(13) Uani 1 1 d . U . . .
H51 H 0.4086 0.5489 0.0996 0.063 Uiso 1 1 calc R U . . .
C65 C 0.8120(4) -0.1415(5) 0.5605(4) 0.0602(12) Uani 1 1 d . U . . .
C96 C 0.9264(4) 0.2246(6) 0.5311(5) 0.0665(11) Uani 1 1 d . U . . .
H96 H 0.9203 0.2072 0.5616 0.080 Uiso 1 1 calc R U . . .
C91 C 0.9039(4) 0.1871(6) 0.4876(4) 0.0644(11) Uani 1 1 d . U . . .
C89 C 0.8343(4) 0.0961(5) 0.4465(4) 0.0631(11) Uani 1 1 d . U . . .
H89 H 0.8404 0.1124 0.4158 0.076 Uiso 1 1 calc R U . . .
C20 C 0.7771(4) 0.4807(5) 0.6819(4) 0.0577(14) Uani 1 1 d . U . . .
H20 H 0.7958 0.4664 0.7136 0.069 Uiso 1 1 calc R U . . .
C9 C 0.7784(5) 0.3802(6) 0.4643(4) 0.0635(12) Uani 1 1 d . U . . .
C2 C 0.5977(5) 0.2951(5) 0.4035(4) 0.0644(13) Uani 1 1 d . U . . .
H2 H 0.5612 0.3043 0.3881 0.077 Uiso 1 1 calc R U . . .
C12 C 0.8188(5) 0.6887(6) 0.4253(5) 0.0807(17) Uani 1 1 d . U . . .
C21 C 0.7241(4) 0.5046(5) 0.6756(4) 0.0565(13) Uani 1 1 d . U . . .
H21 H 0.7070 0.5063 0.7030 0.068 Uiso 1 1 calc R U . . .
C40 C 0.4547(4) 0.6740(5) 0.2735(4) 0.0582(14) Uani 1 1 d . U . . .
H40 H 0.4175 0.6846 0.2619 0.070 Uiso 1 1 calc R U . . .
C120 C 0.9436(5) -0.0230(6) 0.7869(5) 0.0689(14) Uani 1 1 d . U . . .
C119 C 0.9779(5) -0.0050(6) 0.8365(5) 0.0712(15) Uani 1 1 d . U . . .
C121 C 0.9065(4) -0.0823(6) 0.7811(4) 0.0660(13) Uani 1 1 d . U . . .
H121 H 0.9033 -0.1083 0.8097 0.079 Uiso 1 1 calc R U . . .
C123 C 0.8425(4) -0.1738(6) 0.7336(5) 0.0661(14) Uani 1 1 d . U . . .
C102 C 0.9479(4) 0.2536(6) 0.6747(4) 0.0679(13) Uani 1 1 d . U . . .
C42 C 0.4331(4) 0.5438(5) 0.2901(4) 0.0585(14) Uani 1 1 d . U . . .
H42 H 0.3950 0.5506 0.2811 0.070 Uiso 1 1 calc R U . . .
C5 C 0.6903(4) 0.3349(6) 0.4345(4) 0.0615(11) Uani 1 1 d . U . . .
C39 C 0.4941(4) 0.7267(5) 0.2746(4) 0.0574(13) Uani 1 1 d . U . . .
H39 H 0.4835 0.7733 0.2632 0.069 Uiso 1 1 calc R U . . .
C67 C 0.9096(4) -0.1671(5) 0.5816(4) 0.0618(15) Uani 1 1 d . U . . .
H67 H 0.9462 -0.1524 0.5921 0.074 Uiso 1 1 calc R U . . .
C10 C 0.8128(5) 0.4428(6) 0.4686(4) 0.0663(13) Uani 1 1 d . U . . .
H10 H 0.8497 0.4402 0.4847 0.080 Uiso 1 1 calc R U . . .
C82 C 0.7114(5) -0.0184(6) 0.3960(4) 0.0656(14) Uani 1 1 d . U . . .
H82 H 0.6955 -0.0171 0.4242 0.079 Uiso 1 1 calc R U . . .
C18 C 0.7747(4) 0.4985(5) 0.5958(4) 0.0550(13) Uani 1 1 d . U . . .
H18A H 0.7917 0.4961 0.5684 0.066 Uiso 1 1 calc R U . . .
C76 C 0.6608(5) 0.1990(6) 0.5672(4) 0.0670(13) Uani 1 1 d . U . . .
C19 C 0.8034(4) 0.4776(5) 0.6422(4) 0.0578(13) Uani 1 1 d . U . . .
H19 H 0.8398 0.4617 0.6465 0.069 Uiso 1 1 calc R U . . .
C30 C 0.5454(4) 0.8308(5) 0.4695(4) 0.0581(14) Uani 1 1 d . U . . .
H30 H 0.5293 0.8769 0.4664 0.070 Uiso 1 1 calc R U . . .
C86 C 0.7869(5) 0.0068(6) 0.3556(4) 0.0649(14) Uani 1 1 d . U . . .
H86 H 0.8217 0.0262 0.3560 0.078 Uiso 1 1 calc R U . . .
C106 C 1.0606(5) 0.0782(6) 0.7052(4) 0.0702(14) Uani 1 1 d . U . . .
H106 H 1.0980 0.0838 0.7189 0.084 Uiso 1 1 calc R U . . .
C60 C 0.6734(4) 0.2671(5) 0.2118(4) 0.0568(13) Uani 1 1 d . U . . .
H60 H 0.6644 0.2912 0.1812 0.068 Uiso 1 1 calc R U . . .
C105 C 1.0239(5) 0.1402(6) 0.6959(5) 0.0676(13) Uani 1 1 d . U . . .
C28 C 0.5735(4) 0.7255(5) 0.5171(4) 0.0550(13) Uani 1 1 d . U . . .
H28 H 0.5759 0.7000 0.5469 0.066 Uiso 1 1 calc R U . . .
C64 C 0.6731(4) 0.2597(5) 0.2975(4) 0.0588(11) Uani 1 1 d . U . . .
H64 H 0.6641 0.2796 0.3262 0.071 Uiso 1 1 calc R U . . .
C31 C 0.5648(4) 0.8022(5) 0.4309(4) 0.0583(14) Uani 1 1 d . U . . .
H31 H 0.5619 0.8284 0.4013 0.070 Uiso 1 1 calc R U . . .
C114 C 1.0283(5) 0.0283(6) 0.8394(5) 0.0732(15) Uani 1 1 d . U . . .
H114 H 1.0402 0.0390 0.8100 0.088 Uiso 1 1 calc R U . . .
C107 C 1.0412(5) -0.1035(7) 0.6906(5) 0.0815(17) Uani 1 1 d . U . . .
C85 C 0.7580(5) -0.0273(6) 0.3134(4) 0.0668(14) Uani 1 1 d . U . . .
H85 H 0.7740 -0.0319 0.2854 0.080 Uiso 1 1 calc R U . . .
C116 C 1.0433(5) 0.0290(6) 0.9275(5) 0.0772(16) Uani 1 1 d . U . . .
H116 H 1.0652 0.0404 0.9585 0.093 Uiso 1 1 calc R U . . .
C45 C 0.3637(5) 0.2968(6) 0.3314(4) 0.0700(15) Uani 1 1 d . U . . .
H45 H 0.3430 0.3394 0.3256 0.084 Uiso 1 1 calc R U . . .
C62 C 0.7170(4) 0.1681(6) 0.2600(4) 0.0605(14) Uani 1 1 d . U . . .
H62 H 0.7371 0.1249 0.2623 0.073 Uiso 1 1 calc R U . . .
C17 C 0.7859(5) 0.7491(6) 0.4147(5) 0.0826(17) Uani 1 1 d . U . . .
H17 H 0.7480 0.7444 0.4126 0.099 Uiso 1 1 calc R U . . .
C29 C 0.5490(4) 0.7936(5) 0.5122(4) 0.0570(14) Uani 1 1 d . U . . .
H29 H 0.5351 0.8134 0.5385 0.068 Uiso 1 1 calc R U . . .
C72 C 0.7050(4) -0.1810(5) 0.5278(4) 0.0610(14) Uani 1 1 d . U . . .
H72 H 0.6680 -0.1931 0.5165 0.073 Uiso 1 1 calc R U . . .
C83 C 0.6827(5) -0.0509(6) 0.3520(4) 0.0673(14) Uani 1 1 d . U . . .
H83 H 0.6475 -0.0701 0.3504 0.081 Uiso 1 1 calc R U . . .
C113 C 1.0684(5) -0.1755(7) 0.6991(5) 0.0843(18) Uani 1 1 d . U . . .
C81 C 0.6897(5) 0.2640(5) 0.5733(4) 0.0678(12) Uani 1 1 d . U . . .
H81 H 0.7272 0.2643 0.5729 0.081 Uiso 1 1 calc R U . . .
C6 C 0.7059(5) 0.2622(6) 0.4507(4) 0.0634(11) Uani 1 1 d . U . . .
C98 C 0.8399(5) 0.2131(5) 0.6356(4) 0.0691(15) Uani 1 1 d . U . . .
H98 H 0.8033 0.2013 0.6222 0.083 Uiso 1 1 calc R U . . .
C84 C 0.7069(5) -0.0540(6) 0.3118(4) 0.0684(15) Uani 1 1 d . U . . .
H84 H 0.6877 -0.0751 0.2823 0.082 Uiso 1 1 calc R U . . .
C118 C 0.9608(5) -0.0210(6) 0.8807(5) 0.0744(15) Uani 1 1 d . U . . .
H118 H 0.9268 -0.0433 0.8801 0.089 Uiso 1 1 calc R U . . .
C115 C 1.0618(5) 0.0462(6) 0.8846(5) 0.0754(16) Uani 1 1 d . U . . .
H115 H 1.0957 0.0691 0.8861 0.090 Uiso 1 1 calc R U . . .
C4 C 0.6667(4) 0.2074(6) 0.4408(4) 0.0647(11) Uani 1 1 d . U . . .
H4 H 0.6769 0.1595 0.4490 0.078 Uiso 1 1 calc R U . . .
C95 C 0.9576(4) 0.2869(6) 0.5308(5) 0.0675(14) Uani 1 1 d . U . . .
H95 H 0.9714 0.3120 0.5604 0.081 Uiso 1 1 calc R U . . .
C70 C 0.8006(4) -0.2156(5) 0.5480(4) 0.0608(13) Uani 1 1 d . U . . .
C124 C 0.8196(4) -0.1982(6) 0.7730(5) 0.0681(14) Uani 1 1 d . U . . .
H124 H 0.8214 -0.1694 0.8014 0.082 Uiso 1 1 calc R U . . .
C48 C 0.4235(5) 0.1697(6) 0.3474(4) 0.0716(15) Uani 1 1 d . U . . .
H48 H 0.4432 0.1262 0.3514 0.086 Uiso 1 1 calc R U . . .
C3 C 0.6136(5) 0.2231(6) 0.4192(4) 0.0647(13) Uani 1 1 d . U . . .
H3B H 0.5873 0.1862 0.4147 0.078 Uiso 1 1 calc R U . . .
C100 C 0.9084(4) 0.3070(6) 0.6621(4) 0.0702(14) Uani 1 1 d . U . . .
H100 H 0.9180 0.3560 0.6658 0.084 Uiso 1 1 calc R U . . .
C61 C 0.7033(4) 0.2026(5) 0.2157(4) 0.0595(14) Uani 1 1 d . U . . .
H61 H 0.7138 0.1830 0.1875 0.071 Uiso 1 1 calc R U . . .
C92 C 0.9158(4) 0.2129(6) 0.4437(4) 0.0680(12) Uani 1 1 d . U . . .
H92 H 0.9020 0.1890 0.4137 0.082 Uiso 1 1 calc R U . . .
C126 C 0.7905(5) -0.3061(6) 0.7297(5) 0.0715(16) Uani 1 1 d . U . . .
H126 H 0.7728 -0.3511 0.7281 0.086 Uiso 1 1 calc R U . . .
C127 C 0.8122(4) -0.2843(6) 0.6893(5) 0.0704(15) Uani 1 1 d . U . . .
H127 H 0.8097 -0.3138 0.6612 0.084 Uiso 1 1 calc R U . . .
C69 C 0.8442(4) -0.2641(5) 0.5523(4) 0.0621(13) Uani 1 1 d . U . . .
H69 H 0.8375 -0.3129 0.5442 0.075 Uiso 1 1 calc R U . . .
C71 C 0.7445(4) -0.2328(5) 0.5313(4) 0.0607(13) Uani 1 1 d . U . . .
H71 H 0.7343 -0.2806 0.5225 0.073 Uiso 1 1 calc R U . . .
C7 C 0.7606(4) 0.2550(6) 0.4751(4) 0.0643(10) Uani 1 1 d . U . . .
H7 H 0.7731 0.2090 0.4864 0.077 Uiso 1 1 calc R U . . .
C128 C 0.8379(4) -0.2167(6) 0.6921(4) 0.0670(12) Uani 1 1 d . U . . .
H128 H 0.8523 -0.2004 0.6651 0.080 Uiso 1 1 calc R U . . .
C103 C 1.0047(4) 0.2676(6) 0.6951(4) 0.0692(13) Uani 1 1 d . U . . .
H103 H 1.0169 0.3154 0.7014 0.083 Uiso 1 1 calc R U . . .
C112 C 1.0364(5) -0.2374(6) 0.6924(5) 0.0856(18) Uani 1 1 d . U . . .
H112 H 0.9985 -0.2331 0.6809 0.103 Uiso 1 1 calc R U . . .
C63 C 0.7021(4) 0.1955(5) 0.3013(4) 0.0591(14) Uani 1 1 d . U . . .
H63 H 0.7113 0.1712 0.3318 0.071 Uiso 1 1 calc R U . . .
C104 C 1.0404(5) 0.2127(6) 0.7054(4) 0.0693(14) Uani 1 1 d . U . . .
H104 H 1.0772 0.2227 0.7191 0.083 Uiso 1 1 calc R U . . .
C68 C 0.8972(4) -0.2398(5) 0.5686(4) 0.0639(14) Uani 1 1 d . U . . .
H68 H 0.9260 -0.2730 0.5711 0.077 Uiso 1 1 calc R U . . .
C125 C 0.7935(4) -0.2668(6) 0.7699(5) 0.0713(15) Uani 1 1 d . U . . .
H125 H 0.7785 -0.2838 0.7964 0.086 Uiso 1 1 calc R U . . .
C94 C 0.9676(5) 0.3108(6) 0.4867(4) 0.0701(15) Uani 1 1 d . U . . .
H94 H 0.9880 0.3533 0.4863 0.084 Uiso 1 1 calc R U . . .
C47 C 0.3693(5) 0.1713(6) 0.3512(4) 0.0732(16) Uani 1 1 d . U . . .
H47 H 0.3529 0.1290 0.3601 0.088 Uiso 1 1 calc R U . . .
C8 C 0.7961(5) 0.3100(5) 0.4832(4) 0.0659(11) Uani 1 1 d . U . . .
H8A H 0.8320 0.3028 0.5010 0.079 Uiso 1 1 calc R U . . .
C46 C 0.3390(5) 0.2331(6) 0.3423(4) 0.0720(15) Uani 1 1 d . U . . .
H46 H 0.3017 0.2326 0.3435 0.086 Uiso 1 1 calc R U . . .
C77 C 0.6046(5) 0.2018(6) 0.5667(4) 0.0709(14) Uani 1 1 d . U . . .
H77 H 0.5839 0.1592 0.5609 0.085 Uiso 1 1 calc R U . . .
C80 C 0.6636(5) 0.3279(6) 0.5797(4) 0.0714(14) Uani 1 1 d . U . . .
H80 H 0.6836 0.3713 0.5835 0.086 Uiso 1 1 calc R U . . .
C111 C 1.0591(5) -0.3051(7) 0.7021(5) 0.0869(18) Uani 1 1 d . U . . .
H111 H 1.0363 -0.3460 0.6976 0.104 Uiso 1 1 calc R U . . .
C93 C 0.9492(4) 0.2759(6) 0.4440(5) 0.0697(14) Uani 1 1 d . U . . .
H93 H 0.9581 0.2926 0.4144 0.084 Uiso 1 1 calc R U . . .
C117 C 0.9952(5) -0.0032(6) 0.9257(5) 0.0770(16) Uani 1 1 d . U . . .
H117 H 0.9842 -0.0142 0.9555 0.092 Uiso 1 1 calc R U . . .
C99 C 0.8548(5) 0.2867(6) 0.6440(4) 0.0691(13) Uani 1 1 d . U . . .
H99 H 0.8277 0.3225 0.6371 0.083 Uiso 1 1 calc R U . . .
C79 C 0.6089(5) 0.3287(6) 0.5805(4) 0.0730(15) Uani 1 1 d . U . . .
H79 H 0.5916 0.3725 0.5851 0.088 Uiso 1 1 calc R U . . .
C133 C 0.7685(4) 0.4209(6) 0.3336(5) 0.0699(16) Uani 1 1 d D U . . .
H13I H 0.7823 0.3867 0.3603 0.084 Uiso 1 1 calc R U . . .
H13J H 0.7581 0.3942 0.3024 0.084 Uiso 1 1 calc R U . . .
C108 C 1.1253(5) -0.1848(7) 0.7122(5) 0.0868(18) Uani 1 1 d . U . . .
H108 H 1.1488 -0.1449 0.7140 0.104 Uiso 1 1 calc R U . . .
C16 C 0.8071(5) 0.8158(7) 0.4071(5) 0.0853(17) Uani 1 1 d . U . . .
H16 H 0.7846 0.8568 0.4025 0.102 Uiso 1 1 calc R U . . .
C131 C 1.0123(4) 0.0639(6) 0.5704(5) 0.0755(16) Uani 1 1 d D U . . .
H13A H 0.9999 0.0874 0.5382 0.091 Uiso 1 1 calc R U . . .
H13B H 1.0310 0.1000 0.5938 0.091 Uiso 1 1 calc R U . . .
C78 C 0.5787(5) 0.2650(6) 0.5745(4) 0.0724(14) Uani 1 1 d . U . . .
H78 H 0.5414 0.2652 0.5757 0.087 Uiso 1 1 calc R U . . .
C110 C 1.1136(5) -0.3133(7) 0.7182(5) 0.0892(19) Uani 1 1 d . U . . .
H110 H 1.1286 -0.3594 0.7262 0.107 Uiso 1 1 calc R U . . .
C132 C 1.0490(6) 0.0079(8) 0.5656(6) 0.115(4) Uani 1 1 d . U . . .
H13C H 1.0665 0.0182 0.5380 0.173 Uiso 1 1 calc R U . . .
H13D H 1.0291 -0.0373 0.5596 0.173 Uiso 1 1 calc R U . . .
H13E H 1.0765 0.0041 0.5959 0.173 Uiso 1 1 calc R U . . .
C134 C 0.8087(6) 0.4735(8) 0.3300(6) 0.111(4) Uani 1 1 d . U . . .
H13K H 0.8218 0.4663 0.2995 0.167 Uiso 1 1 calc R U . . .
H13L H 0.8390 0.4690 0.3581 0.167 Uiso 1 1 calc R U . . .
H13M H 0.7928 0.5213 0.3299 0.167 Uiso 1 1 calc R U . . .
C109 C 1.1468(5) -0.2543(7) 0.7227(5) 0.0887(18) Uani 1 1 d . U . . .
H109 H 1.1848 -0.2602 0.7330 0.106 Uiso 1 1 calc R U . . .
C15 C 0.8625(5) 0.8214(7) 0.4064(5) 0.0884(18) Uani 1 1 d . U . . .
H15 H 0.8767 0.8654 0.3979 0.106 Uiso 1 1 calc R U . . .
C14 C 0.8967(5) 0.7624(6) 0.4182(5) 0.0868(17) Uani 1 1 d . U . . .
H14 H 0.9344 0.7672 0.4192 0.104 Uiso 1 1 calc R U . . .
C13 C 0.8756(5) 0.6959(7) 0.4287(5) 0.0846(17) Uani 1 1 d . U . . .
H13N H 0.8989 0.6563 0.4379 0.101 Uiso 1 1 calc R U . . .
C130 C 0.7164(7) -0.0088(9) 0.7032(7) 0.129(4) Uani 1 1 d . U . . .
H13F H 0.6853 -0.0226 0.6777 0.193 Uiso 1 1 calc R U . . .
H13G H 0.7036 0.0170 0.7293 0.193 Uiso 1 1 calc R U . . .
H13H H 0.7360 -0.0518 0.7169 0.193 Uiso 1 1 calc R U . . .
C129 C 0.7513(6) 0.0357(7) 0.6826(5) 0.085(2) Uani 1 1 d D U . . .
H12A H 0.7799 0.0554 0.7089 0.102 Uiso 1 1 calc R U . . .
H12B H 0.7305 0.0761 0.6651 0.102 Uiso 1 1 calc R U . . .
C135 C 0.4923(6) 0.4747(7) 0.4317(5) 0.093(2) Uani 1 1 d D U . . .
H13P H 0.4746 0.5097 0.4499 0.112 Uiso 1 1 calc R U . . .
H13Q H 0.4644 0.4452 0.4106 0.112 Uiso 1 1 calc R U . . .
C136 C 0.5299(6) 0.4319(8) 0.4639(5) 0.112(3) Uani 1 1 d D U . . .
H13O H 0.5110 0.4050 0.4856 0.168 Uiso 1 1 calc R U . . .
H13R H 0.5474 0.3986 0.4448 0.168 Uiso 1 1 calc R U . . .
H13S H 0.5575 0.4625 0.4838 0.168 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.0426(2) 0.0335(2) 0.0380(2) 0.00015(17) 0.00234(18) 0.00852(19)
Dy2 0.0419(2) 0.0351(2) 0.0345(2) 0.00075(17) 0.00470(18) 0.00721(18)
Dy3 0.0423(2) 0.0416(2) 0.0411(3) -0.00273(18) 0.00003(19) -0.0120(2)
Dy4 0.0459(3) 0.0405(2) 0.0487(3) 0.00014(19) -0.0042(2) -0.0129(2)
O7 0.043(3) 0.037(3) 0.038(3) 0.001(3) 0.002(3) 0.004(3)
O2 0.056(4) 0.033(3) 0.032(3) -0.001(2) 0.010(3) 0.004(3)
O12 0.046(4) 0.035(3) 0.055(4) -0.001(3) -0.001(3) -0.007(3)
O5 0.071(4) 0.047(4) 0.034(3) 0.002(3) 0.001(3) 0.025(3)
O10 0.050(4) 0.048(3) 0.036(3) -0.009(3) 0.004(3) 0.021(3)
O4 0.046(3) 0.046(3) 0.039(3) -0.012(3) 0.005(3) 0.014(3)
O13 0.060(4) 0.059(4) 0.048(4) 0.009(3) 0.001(3) -0.008(3)
O6 0.045(4) 0.036(3) 0.072(5) -0.008(3) 0.001(3) 0.008(3)
O11 0.049(4) 0.036(3) 0.070(5) 0.004(3) -0.010(3) -0.009(3)
O9 0.066(4) 0.065(4) 0.037(4) 0.001(3) 0.008(3) 0.025(4)
O17 0.041(3) 0.036(3) 0.062(4) -0.004(3) -0.008(3) -0.007(3)
O19 0.047(4) 0.050(4) 0.060(4) 0.015(3) 0.004(3) -0.010(3)
O8 0.057(4) 0.070(5) 0.058(4) -0.021(3) 0.007(3) 0.010(3)
O1 0.054(4) 0.045(4) 0.076(5) 0.004(3) -0.004(4) 0.006(3)
O16 0.058(4) 0.041(4) 0.083(5) 0.005(3) -0.004(4) -0.012(3)
O20 0.069(5) 0.045(4) 0.052(4) -0.005(3) 0.000(4) -0.010(3)
O14 0.050(4) 0.058(4) 0.050(4) 0.004(3) 0.003(3) -0.017(3)
N8 0.054(5) 0.034(4) 0.044(4) -0.010(3) 0.000(4) -0.013(4)
N4 0.038(4) 0.039(4) 0.048(5) 0.001(3) 0.004(3) 0.019(3)
O18 0.064(4) 0.085(5) 0.066(5) 0.008(4) -0.012(3) -0.028(4)
N7 0.040(4) 0.041(4) 0.054(5) 0.000(4) 0.001(4) -0.016(4)
O15 0.056(4) 0.081(5) 0.047(4) -0.005(4) 0.001(3) -0.020(4)
N5 0.045(4) 0.030(3) 0.051(5) -0.005(3) 0.016(4) 0.013(3)
N10 0.055(5) 0.040(4) 0.055(5) -0.002(4) -0.005(4) -0.019(4)
O3 0.075(5) 0.107(6) 0.038(4) 0.005(4) 0.012(4) 0.029(4)
N6 0.051(5) 0.040(4) 0.057(5) -0.003(4) 0.006(4) 0.003(4)
N9 0.044(4) 0.041(4) 0.057(5) -0.001(4) 0.004(4) 0.003(4)
N3 0.044(5) 0.046(5) 0.080(7) 0.005(4) -0.005(4) 0.004(4)
C34 0.059(3) 0.039(2) 0.063(3) 0.013(2) 0.011(2) 0.005(2)
C33 0.058(2) 0.038(2) 0.065(3) 0.013(2) 0.014(2) 0.005(2)
N11 0.050(5) 0.049(5) 0.060(5) -0.003(4) -0.001(4) -0.017(4)
N1 0.040(4) 0.038(4) 0.055(5) 0.008(3) 0.002(4) 0.022(3)
N2 0.045(4) 0.045(4) 0.060(5) 0.006(4) 0.012(4) 0.006(4)
C66 0.053(2) 0.047(2) 0.073(3) -0.009(2) 0.002(2) -0.006(2)
C75 0.071(2) 0.051(2) 0.076(2) 0.000(2) 0.007(2) 0.001(2)
C58 0.055(2) 0.043(2) 0.055(2) -0.005(2) 0.009(2) 0.009(2)
C55 0.056(2) 0.041(2) 0.047(2) -0.003(2) 0.006(2) 0.001(2)
C101 0.062(2) 0.049(2) 0.083(2) -0.009(2) 0.002(2) -0.008(2)
C38 0.060(3) 0.039(2) 0.066(3) 0.014(2) 0.012(2) 0.006(2)
C59 0.058(2) 0.045(2) 0.057(2) -0.006(2) 0.008(2) 0.011(2)
C87 0.069(2) 0.056(2) 0.061(2) -0.001(2) 0.004(2) 0.000(2)
C44 0.076(3) 0.051(3) 0.073(3) 0.006(3) 0.007(3) 0.000(3)
C26 0.054(2) 0.040(2) 0.055(3) -0.004(2) 0.004(2) 0.009(2)
C56 0.054(2) 0.041(2) 0.047(2) -0.002(2) 0.007(2) 0.002(2)
C23 0.061(2) 0.043(2) 0.050(2) 0.000(2) 0.004(2) 0.007(2)
C24 0.059(2) 0.042(2) 0.051(2) 0.000(2) 0.004(2) 0.007(2)
C27 0.056(3) 0.040(2) 0.058(3) -0.005(2) 0.002(2) 0.011(2)
C49 0.077(3) 0.051(3) 0.075(3) 0.008(3) 0.007(3) 0.000(3)
C90 0.065(2) 0.054(2) 0.068(2) 0.003(2) 0.009(2) -0.002(2)
C74 0.054(3) 0.047(2) 0.074(3) -0.009(2) 0.005(2) -0.007(2)
C35 0.060(3) 0.042(3) 0.066(3) 0.015(2) 0.010(3) 0.004(2)
C43 0.077(3) 0.053(2) 0.073(3) 0.007(2) 0.012(3) 0.001(2)
C37 0.062(3) 0.040(2) 0.067(3) 0.015(2) 0.011(2) 0.005(2)
C25 0.057(2) 0.041(2) 0.051(2) -0.002(2) 0.005(2) 0.010(2)
C54 0.057(2) 0.041(2) 0.047(2) -0.002(2) 0.007(2) 0.000(2)
C57 0.057(2) 0.044(2) 0.050(2) -0.004(2) 0.008(2) 0.006(2)
C1 0.069(2) 0.048(2) 0.069(2) 0.007(2) 0.010(2) 0.005(2)
C73 0.052(2) 0.044(2) 0.073(3) -0.010(2) 0.005(2) -0.007(2)
C22 0.061(2) 0.046(2) 0.053(2) 0.000(2) 0.004(2) 0.007(2)
C53 0.059(3) 0.044(2) 0.049(3) -0.002(2) 0.006(2) -0.001(2)
N12 0.054(5) 0.056(5) 0.087(7) -0.001(5) -0.011(5) -0.001(5)
C11 0.066(3) 0.060(3) 0.100(3) 0.009(3) 0.001(3) -0.005(3)
C50 0.058(2) 0.045(2) 0.050(2) -0.001(2) 0.006(2) 0.002(2)
C97 0.062(2) 0.048(2) 0.082(3) -0.010(2) 0.002(2) -0.007(2)
C122 0.061(3) 0.058(3) 0.071(3) 0.009(2) 0.005(2) -0.001(2)
C52 0.061(3) 0.044(3) 0.049(3) -0.001(2) 0.005(2) 0.001(2)
C36 0.062(3) 0.042(2) 0.068(3) 0.015(2) 0.011(2) 0.004(2)
C88 0.067(2) 0.055(2) 0.062(2) 0.000(2) 0.006(2) 0.000(2)
C32 0.059(3) 0.044(2) 0.059(3) -0.003(2) 0.003(2) 0.011(2)
C41 0.058(3) 0.039(2) 0.069(3) 0.012(2) 0.014(2) 0.007(2)
C51 0.058(3) 0.046(2) 0.052(3) 0.000(2) 0.003(2) 0.002(2)
C65 0.054(2) 0.047(2) 0.075(2) -0.009(2) 0.001(2) -0.007(2)
C96 0.066(2) 0.0558(19) 0.075(2) 0.0021(18) 0.0081(19) -0.0051(18)
C91 0.066(2) 0.055(2) 0.070(2) 0.0048(19) 0.010(2) -0.0028(19)
C89 0.067(2) 0.054(2) 0.066(2) 0.001(2) 0.008(2) -0.001(2)
C20 0.065(3) 0.050(3) 0.054(3) 0.002(2) 0.001(3) 0.006(3)
C9 0.067(2) 0.050(2) 0.072(2) 0.007(2) 0.012(2) 0.007(2)
C2 0.070(2) 0.050(2) 0.071(2) 0.009(2) 0.010(2) 0.004(2)
C12 0.067(3) 0.062(3) 0.106(4) 0.013(3) -0.001(3) -0.007(3)
C21 0.064(3) 0.049(2) 0.053(3) 0.000(2) 0.004(2) 0.005(2)
C40 0.060(3) 0.041(2) 0.072(3) 0.014(2) 0.011(2) 0.008(2)
C120 0.071(3) 0.063(3) 0.067(3) 0.000(2) 0.001(3) 0.004(2)
C119 0.074(3) 0.066(3) 0.067(3) 0.000(3) 0.001(3) 0.005(3)
C121 0.065(2) 0.060(2) 0.069(3) 0.005(2) 0.005(2) 0.002(2)
C123 0.061(3) 0.059(3) 0.075(3) 0.012(2) 0.005(2) -0.004(2)
C102 0.064(2) 0.049(2) 0.085(3) -0.011(2) 0.002(2) -0.007(2)
C42 0.061(3) 0.042(2) 0.073(3) 0.011(2) 0.013(3) 0.008(2)
C5 0.066(2) 0.047(2) 0.070(2) 0.0075(19) 0.011(2) 0.005(2)
C39 0.061(2) 0.041(2) 0.070(3) 0.014(2) 0.012(2) 0.008(2)
C67 0.053(3) 0.049(3) 0.077(3) -0.013(3) 0.001(3) -0.006(2)
C10 0.065(2) 0.055(2) 0.077(2) 0.006(2) 0.009(2) 0.006(2)
C82 0.071(3) 0.059(2) 0.063(3) -0.003(2) 0.003(2) 0.000(2)
C18 0.061(2) 0.048(2) 0.053(2) 0.001(2) 0.005(2) 0.006(2)
C76 0.070(2) 0.050(2) 0.077(2) 0.002(2) 0.005(2) 0.002(2)
C19 0.063(2) 0.048(2) 0.059(2) -0.002(2) 0.003(2) 0.009(2)
C30 0.060(3) 0.045(3) 0.064(3) -0.005(2) 0.002(3) 0.013(2)
C86 0.072(3) 0.058(2) 0.061(3) -0.001(2) 0.004(2) 0.000(2)
C106 0.063(3) 0.055(2) 0.088(3) -0.008(2) 0.003(2) -0.009(2)
C60 0.061(2) 0.049(2) 0.059(2) -0.005(2) 0.008(2) 0.011(2)
C105 0.062(2) 0.052(2) 0.085(3) -0.008(2) 0.005(2) -0.010(2)
C28 0.057(3) 0.045(2) 0.059(3) -0.004(2) 0.003(2) 0.010(2)
C64 0.063(2) 0.050(2) 0.062(2) -0.0029(19) 0.0090(19) 0.0105(19)
C31 0.061(3) 0.047(2) 0.063(3) -0.001(2) 0.001(2) 0.009(2)
C114 0.076(3) 0.069(3) 0.069(3) -0.002(3) 0.000(3) 0.005(3)
C107 0.073(3) 0.063(3) 0.101(4) 0.001(3) -0.001(3) 0.002(3)
C85 0.074(3) 0.060(3) 0.062(3) -0.002(2) 0.004(3) 0.000(3)
C116 0.081(3) 0.073(3) 0.070(3) -0.002(3) -0.002(3) 0.006(3)
C45 0.078(3) 0.053(3) 0.076(3) 0.006(3) 0.007(3) 0.000(3)
C62 0.064(3) 0.051(3) 0.064(3) -0.006(2) 0.008(3) 0.013(2)
C17 0.069(3) 0.063(3) 0.107(4) 0.013(3) 0.000(3) -0.008(3)
C29 0.059(3) 0.046(2) 0.062(3) -0.007(2) 0.003(2) 0.012(2)
C72 0.054(3) 0.048(2) 0.077(3) -0.011(2) 0.002(2) -0.009(2)
C83 0.072(3) 0.061(3) 0.064(3) -0.003(2) 0.002(3) -0.001(3)
C113 0.077(3) 0.064(3) 0.104(4) 0.004(3) -0.001(3) 0.005(3)
C81 0.072(2) 0.051(2) 0.077(2) 0.002(2) 0.006(2) 0.003(2)
C6 0.069(2) 0.0485(19) 0.071(2) 0.0070(19) 0.0102(19) 0.0041(19)
C98 0.065(3) 0.049(3) 0.087(3) -0.012(3) 0.000(3) -0.006(3)
C84 0.075(3) 0.061(3) 0.063(3) -0.002(3) 0.000(3) 0.000(3)
C118 0.077(3) 0.070(3) 0.070(3) -0.001(3) 0.000(3) 0.004(3)
C115 0.077(3) 0.072(3) 0.071(3) -0.003(3) 0.000(3) 0.004(3)
C4 0.070(2) 0.0490(19) 0.073(2) 0.0071(19) 0.0096(19) 0.0031(19)
C95 0.068(3) 0.059(2) 0.073(3) 0.005(2) 0.009(2) -0.007(2)
C70 0.054(2) 0.047(2) 0.076(3) -0.011(2) 0.002(2) -0.007(2)
C124 0.063(3) 0.062(3) 0.076(3) 0.010(2) 0.006(2) -0.004(2)
C48 0.080(3) 0.054(3) 0.078(3) 0.007(3) 0.007(3) -0.001(3)
C3 0.071(2) 0.049(2) 0.072(2) 0.009(2) 0.009(2) 0.002(2)
C100 0.066(3) 0.051(2) 0.087(3) -0.012(2) 0.001(2) -0.007(2)
C61 0.063(3) 0.052(2) 0.062(3) -0.007(2) 0.008(2) 0.014(2)
C92 0.070(2) 0.059(2) 0.074(2) 0.003(2) 0.010(2) -0.006(2)
C126 0.065(3) 0.063(3) 0.082(3) 0.012(3) 0.004(3) -0.008(3)
C127 0.065(3) 0.062(3) 0.079(3) 0.010(3) 0.003(3) -0.007(3)
C69 0.056(2) 0.048(2) 0.078(3) -0.013(2) 0.001(2) -0.006(2)
C71 0.055(2) 0.046(2) 0.076(3) -0.011(2) 0.003(2) -0.008(2)
C7 0.0683(19) 0.0506(18) 0.0724(19) 0.0069(17) 0.0106(18) 0.0042(17)
C128 0.061(2) 0.059(2) 0.076(2) 0.007(2) 0.004(2) -0.006(2)
C103 0.064(2) 0.051(2) 0.087(3) -0.010(2) 0.003(2) -0.009(2)
C112 0.077(3) 0.066(3) 0.105(4) 0.004(3) -0.001(3) 0.005(3)
C63 0.064(3) 0.051(2) 0.061(3) -0.004(2) 0.008(2) 0.014(2)
C104 0.063(3) 0.052(2) 0.087(3) -0.011(2) 0.003(3) -0.010(2)
C68 0.057(3) 0.051(2) 0.079(3) -0.013(2) 0.001(2) -0.004(2)
C125 0.064(3) 0.065(3) 0.080(3) 0.013(3) 0.006(3) -0.006(3)
C94 0.070(3) 0.061(3) 0.077(3) 0.005(3) 0.010(3) -0.009(3)
C47 0.081(3) 0.055(3) 0.079(3) 0.008(3) 0.007(3) -0.003(3)
C8 0.068(2) 0.0533(19) 0.074(2) 0.0072(19) 0.009(2) 0.0028(19)
C46 0.078(3) 0.056(3) 0.078(3) 0.008(3) 0.008(3) -0.002(3)
C77 0.073(3) 0.053(2) 0.082(3) 0.000(2) 0.004(3) 0.003(3)
C80 0.075(3) 0.053(2) 0.082(3) -0.001(2) 0.005(3) 0.001(3)
C111 0.079(3) 0.066(3) 0.107(4) 0.003(3) -0.001(3) 0.004(3)
C93 0.071(3) 0.062(2) 0.075(3) 0.005(2) 0.012(2) -0.008(2)
C117 0.081(3) 0.073(3) 0.071(3) -0.002(3) 0.000(3) 0.005(3)
C99 0.066(2) 0.051(2) 0.085(3) -0.011(2) 0.001(2) -0.004(2)
C79 0.076(3) 0.053(3) 0.084(3) -0.002(3) 0.003(3) 0.004(3)
C133 0.069(3) 0.064(3) 0.077(3) -0.004(3) 0.017(3) 0.009(3)
C108 0.078(3) 0.066(3) 0.107(4) 0.003(3) -0.002(3) 0.005(3)
C16 0.072(3) 0.065(3) 0.110(4) 0.013(3) -0.001(3) -0.006(3)
C131 0.068(3) 0.066(3) 0.091(3) -0.002(3) 0.013(3) -0.008(3)
C78 0.073(3) 0.056(2) 0.083(3) -0.001(2) 0.005(3) 0.003(2)
C110 0.082(4) 0.067(3) 0.109(4) 0.005(3) -0.002(3) 0.006(3)
C132 0.101(8) 0.109(8) 0.133(9) -0.019(7) 0.020(7) 0.025(7)
C134 0.116(8) 0.114(8) 0.109(8) -0.021(7) 0.035(7) -0.022(7)
C109 0.079(3) 0.069(3) 0.109(4) 0.003(3) -0.002(3) 0.005(3)
C15 0.074(3) 0.069(3) 0.114(4) 0.015(3) -0.001(3) -0.008(3)
C14 0.072(3) 0.068(3) 0.112(4) 0.013(3) -0.001(3) -0.007(3)
C13 0.070(3) 0.066(3) 0.109(4) 0.013(3) 0.000(3) -0.007(3)
C130 0.120(9) 0.127(9) 0.138(9) -0.017(8) 0.025(8) -0.007(8)
C129 0.097(5) 0.073(4) 0.087(5) -0.004(4) 0.023(4) 0.004(4)
C135 0.107(4) 0.091(4) 0.085(4) 0.007(3) 0.025(3) 0.000(3)
C136 0.121(5) 0.103(5) 0.109(5) 0.006(4) 0.018(4) 0.018(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.260(7) . ?
Dy1 O5 2.302(6) . ?
Dy1 O4 2.352(5) . ?
Dy1 O2 2.361(6) . ?
Dy1 O7 2.375(5) . ?
Dy1 N1 2.457(6) . ?
Dy1 O3 2.459(7) . ?
Dy1 N2 2.514(7) . ?
Dy1 Dy2 3.8287(6) . ?
Dy2 O6 2.276(6) . ?
Dy2 O9 2.278(6) . ?
Dy2 O10 2.329(6) . ?
Dy2 O7 2.355(6) . ?
Dy2 O2 2.382(5) . ?
Dy2 O8 2.452(7) . ?
Dy2 N4 2.468(7) . ?
Dy2 N5 2.510(7) . ?
Dy3 O11 2.280(6) . ?
Dy3 O15 2.312(7) . ?
Dy3 O14 2.334(6) . ?
Dy3 O12 2.360(6) . ?
Dy3 O17 2.393(6) . ?
Dy3 N7 2.435(7) . ?
Dy3 O13 2.436(7) . ?
Dy3 N8 2.515(7) . ?
Dy3 Dy4 3.8370(7) . ?
Dy4 O16 2.255(7) . ?
Dy4 O20 2.317(7) . ?
Dy4 O19 2.350(6) . ?
Dy4 O17 2.361(6) . ?
Dy4 O12 2.379(6) . ?
Dy4 N10 2.438(7) . ?
Dy4 O18 2.439(8) . ?
Dy4 N11 2.513(8) . ?
O7 C34 1.352(10) . ?
O2 C1 1.345(11) . ?
O12 C66 1.351(10) . ?
O5 C24 1.237(11) . ?
O10 C58 1.275(11) . ?
O4 C26 1.264(10) . ?
O13 C129 1.488(14) . ?
O13 H13 0.856(10) . ?
O6 C43 1.275(12) . ?
O11 C75 1.290(12) . ?
O9 C56 1.256(11) . ?
O17 C97 1.350(11) . ?
O19 C122 1.248(12) . ?
O8 C135 1.578(14) . ?
O8 H8 0.856(10) . ?
O1 C11 1.294(12) . ?
O16 C107 1.278(13) . ?
O20 C120 1.271(13) . ?
O14 C90 1.300(12) . ?
N8 C74 1.278(11) . ?
N8 N9 1.379(10) . ?
N4 C41 1.319(11) . ?
N4 C33 1.345(11) . ?
O18 C131 1.403(12) . ?
O18 H18 0.851(10) . ?
N7 C73 1.338(11) . ?
N7 C65 1.342(12) . ?
O15 C88 1.257(13) . ?
N5 C42 1.269(11) . ?
N5 N6 1.405(10) . ?
N10 C105 1.334(12) . ?
N10 C101 1.349(12) . ?
O3 C133 1.461(12) . ?
O3 H3 0.856(10) . ?
N6 C43 1.323(12) . ?
N9 C75 1.310(12) . ?
N3 C11 1.320(13) . ?
N3 N2 1.381(10) . ?
C34 C35 1.360(13) . ?
C34 C33 1.420(13) . ?
C33 C38 1.422(12) . ?
N11 C106 1.280(12) . ?
N11 N12 1.389(11) . ?
N1 C9 1.323(12) . ?
N1 C5 1.326(12) . ?
N2 C10 1.261(12) . ?
C66 C67 1.387(13) . ?
C66 C65 1.423(13) . ?
C75 C76 1.490(14) . ?
C58 C57 1.388(13) . ?
C58 C59 1.497(12) . ?
C55 C54 1.398(13) . ?
C55 C50 1.404(13) . ?
C55 C56 1.513(13) . ?
C101 C102 1.415(14) . ?
C101 C97 1.429(14) . ?
C38 C39 1.391(13) . ?
C38 C37 1.397(13) . ?
C59 C64 1.362(13) . ?
C59 C60 1.371(13) . ?
C87 C82 1.385(15) . ?
C87 C86 1.410(15) . ?
C87 C88 1.492(14) . ?
C44 C49 1.380(14) . ?
C44 C45 1.386(15) . ?
C44 C43 1.491(15) . ?
C26 C25 1.393(12) . ?
C26 C27 1.485(12) . ?
C56 C57 1.394(12) . ?
C23 C22 1.376(14) . ?
C23 C18 1.394(13) . ?
C23 C24 1.479(13) . ?
C24 C25 1.417(12) . ?
C27 C32 1.371(13) . ?
C27 C28 1.380(13) . ?
C49 C48 1.379(14) . ?
C49 H49 0.9300 . ?
C90 C89 1.383(14) . ?
C90 C91 1.469(14) . ?
C74 C73 1.460(13) . ?
C74 H74 0.9300 . ?
C35 C36 1.404(12) . ?
C35 H35 0.9300 . ?
C37 C36 1.345(13) . ?
C37 H37 0.9300 . ?
C25 H25 0.9300 . ?
C54 C53 1.366(12) . ?
C54 H54 0.9300 . ?
C57 H57 0.9300 . ?
C1 C2 1.349(14) . ?
C1 C5 1.436(14) . ?
C73 C72 1.385(12) . ?
C22 C21 1.365(13) . ?
C22 H22 0.9300 . ?
C53 C52 1.332(13) . ?
C53 H53 0.9300 . ?
N12 C107 1.324(14) . ?
C11 C12 1.471(15) . ?
C50 C51 1.378(13) . ?
C50 H50 0.9300 . ?
C97 C98 1.355(14) . ?
C122 C121 1.390(14) . ?
C122 C123 1.493(14) . ?
C52 C51 1.357(13) . ?
C52 H52 0.9300 . ?
C36 H36 0.9300 . ?
C88 C89 1.372(14) . ?
C32 C31 1.388(12) . ?
C32 H32 0.9300 . ?
C41 C40 1.402(12) . ?
C41 C42 1.452(13) . ?
C51 H51 0.9300 . ?
C65 C70 1.415(13) . ?
C96 C95 1.379(14) . ?
C96 C91 1.388(14) . ?
C96 H96 0.9300 . ?
C91 C92 1.374(15) . ?
C89 H89 0.9300 . ?
C20 C21 1.359(13) . ?
C20 C19 1.374(14) . ?
C20 H20 0.9300 . ?
C9 C10 1.418(14) . ?
C9 C8 1.422(13) . ?
C2 C3 1.420(13) . ?
C2 H2 0.9300 . ?
C12 C17 1.369(15) . ?
C12 C13 1.393(15) . ?
C21 H21 0.9300 . ?
C40 C39 1.368(13) . ?
C40 H40 0.9300 . ?
C120 C121 1.410(15) . ?
C120 C119 1.481(15) . ?
C119 C114 1.375(16) . ?
C119 C118 1.388(16) . ?
C121 H121 0.9300 . ?
C123 C128 1.363(15) . ?
C123 C124 1.387(15) . ?
C102 C100 1.376(14) . ?
C102 C103 1.425(14) . ?
C42 H42 0.9300 . ?
C5 C6 1.433(13) . ?
C39 H39 0.9300 . ?
C67 C68 1.398(13) . ?
C67 H67 0.9300 . ?
C10 H10 0.9300 . ?
C82 C83 1.398(14) . ?
C82 H82 0.9300 . ?
C18 C19 1.373(13) . ?
C18 H18A 0.9300 . ?
C76 C81 1.383(14) . ?
C76 C77 1.387(15) . ?
C19 H19 0.9300 . ?
C30 C29 1.337(14) . ?
C30 C31 1.347(14) . ?
C30 H30 0.9300 . ?
C86 C85 1.376(14) . ?
C86 H86 0.9300 . ?
C106 C105 1.444(14) . ?
C106 H106 0.9300 . ?
C60 C61 1.388(13) . ?
C60 H60 0.9300 . ?
C105 C104 1.399(13) . ?
C28 C29 1.383(12) . ?
C28 H28 0.9300 . ?
C64 C63 1.372(13) . ?
C64 H64 0.9300 . ?
C31 H31 0.9300 . ?
C114 C115 1.378(15) . ?
C114 H114 0.9300 . ?
C107 C113 1.479(16) . ?
C85 C84 1.348(15) . ?
C85 H85 0.9300 . ?
C116 C117 1.319(15) . ?
C116 C115 1.376(16) . ?
C116 H116 0.9300 . ?
C45 C46 1.377(14) . ?
C45 H45 0.9300 . ?
C62 C61 1.345(14) . ?
C62 C63 1.351(14) . ?
C62 H62 0.9300 . ?
C17 C16 1.364(15) . ?
C17 H17 0.9300 . ?
C29 H29 0.9300 . ?
C72 C71 1.351(13) . ?
C72 H72 0.9300 . ?
C83 C84 1.353(15) . ?
C83 H83 0.9300 . ?
C113 C112 1.374(16) . ?
C113 C108 1.391(15) . ?
C81 C80 1.365(14) . ?
C81 H81 0.9300 . ?
C6 C4 1.384(14) . ?
C6 C7 1.386(14) . ?
C98 C99 1.406(13) . ?
C98 H98 0.9300 . ?
C84 H84 0.9300 . ?
C118 C117 1.383(15) . ?
C118 H118 0.9300 . ?
C115 H115 0.9300 . ?
C4 C3 1.355(13) . ?
C4 H4 0.9300 . ?
C95 C94 1.348(15) . ?
C95 H95 0.9300 . ?
C70 C69 1.383(13) . ?
C70 C71 1.404(13) . ?
C124 C125 1.408(14) . ?
C124 H124 0.9300 . ?
C48 C47 1.366(15) . ?
C48 H48 0.9300 . ?
C3 H3B 0.9300 . ?
C100 C99 1.367(13) . ?
C100 H100 0.9300 . ?
C61 H61 0.9300 . ?
C92 C93 1.418(14) . ?
C92 H92 0.9300 . ?
C126 C125 1.302(15) . ?
C126 C127 1.378(15) . ?
C126 H126 0.9300 . ?
C127 C128 1.387(14) . ?
C127 H127 0.9300 . ?
C69 C68 1.369(13) . ?
C69 H69 0.9300 . ?
C71 H71 0.9300 . ?
C7 C8 1.325(13) . ?
C7 H7 0.9300 . ?
C128 H128 0.9300 . ?
C103 C104 1.331(14) . ?
C103 H103 0.9300 . ?
C112 C111 1.366(15) . ?
C112 H112 0.9300 . ?
C63 H63 0.9300 . ?
C104 H104 0.9300 . ?
C68 H68 0.9300 . ?
C125 H125 0.9300 . ?
C94 C93 1.328(15) . ?
C94 H94 0.9300 . ?
C47 C46 1.354(14) . ?
C47 H47 0.9300 . ?
C8 H8A 0.9300 . ?
C46 H46 0.9300 . ?
C77 C78 1.361(14) . ?
C77 H77 0.9300 . ?
C80 C79 1.358(14) . ?
C80 H80 0.9300 . ?
C111 C110 1.339(15) . ?
C111 H111 0.9300 . ?
C93 H93 0.9300 . ?
C117 H117 0.9300 . ?
C99 H99 0.9300 . ?
C79 C78 1.378(14) . ?
C79 H79 0.9300 . ?
C133 C134 1.402(16) . ?
C133 H13I 0.9700 . ?
C133 H13J 0.9700 . ?
C108 C109 1.387(15) . ?
C108 H108 0.9300 . ?
C16 C15 1.376(16) . ?
C16 H16 0.9300 . ?
C131 C132 1.393(16) . ?
C131 H13A 0.9700 . ?
C131 H13B 0.9700 . ?
C78 H78 0.9300 . ?
C110 C109 1.349(16) . ?
C110 H110 0.9300 . ?
C132 H13C 0.9600 . ?
C132 H13D 0.9600 . ?
C132 H13E 0.9600 . ?
C134 H13K 0.9600 . ?
C134 H13L 0.9600 . ?
C134 H13M 0.9600 . ?
C109 H109 0.9300 . ?
C15 C14 1.371(15) . ?
C15 H15 0.9300 . ?
C14 C13 1.379(15) . ?
C14 H14 0.9300 . ?
C13 H13N 0.9300 . ?
C130 C129 1.387(18) . ?
C130 H13F 0.9600 . ?
C130 H13G 0.9600 . ?
C130 H13H 0.9600 . ?
C129 H12A 0.9700 . ?
C129 H12B 0.9700 . ?
C135 C136 1.386(13) . ?
C135 H13P 0.9700 . ?
C135 H13Q 0.9700 . ?
C136 H13O 0.9600 . ?
C136 H13R 0.9600 . ?
C136 H13S 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O5 92.7(2) . . ?
O1 Dy1 O4 83.4(2) . . ?
O5 Dy1 O4 70.9(2) . . ?
O1 Dy1 O2 165.0(2) . . ?
O5 Dy1 O2 98.8(2) . . ?
O4 Dy1 O2 91.4(2) . . ?
O1 Dy1 O7 93.2(2) . . ?
O5 Dy1 O7 144.3(2) . . ?
O4 Dy1 O7 74.8(2) . . ?
O2 Dy1 O7 71.89(19) . . ?
O1 Dy1 N1 125.7(2) . . ?
O5 Dy1 N1 72.6(2) . . ?
O4 Dy1 N1 133.9(2) . . ?
O2 Dy1 N1 67.4(2) . . ?
O7 Dy1 N1 129.1(2) . . ?
O1 Dy1 O3 95.0(3) . . ?
O5 Dy1 O3 143.9(2) . . ?
O4 Dy1 O3 145.0(2) . . ?
O2 Dy1 O3 81.2(2) . . ?
O7 Dy1 O3 70.4(2) . . ?
N1 Dy1 O3 74.3(3) . . ?
O1 Dy1 N2 62.3(2) . . ?
O5 Dy1 N2 74.2(3) . . ?
O4 Dy1 N2 129.0(2) . . ?
O2 Dy1 N2 130.2(2) . . ?
O7 Dy1 N2 138.4(2) . . ?
N1 Dy1 N2 63.4(2) . . ?
O3 Dy1 N2 78.5(3) . . ?
O1 Dy1 Dy2 128.67(16) . . ?
O5 Dy1 Dy2 124.44(17) . . ?
O4 Dy1 Dy2 78.37(14) . . ?
O2 Dy1 Dy2 36.36(13) . . ?
O7 Dy1 Dy2 35.78(14) . . ?
N1 Dy1 Dy2 100.53(17) . . ?
O3 Dy1 Dy2 75.57(18) . . ?
N2 Dy1 Dy2 152.55(18) . . ?
O6 Dy2 O9 92.9(2) . . ?
O6 Dy2 O10 90.0(2) . . ?
O9 Dy2 O10 71.4(2) . . ?
O6 Dy2 O7 164.9(2) . . ?
O9 Dy2 O7 99.1(2) . . ?
O10 Dy2 O7 85.3(2) . . ?
O6 Dy2 O2 93.1(2) . . ?
O9 Dy2 O2 144.3(2) . . ?
O10 Dy2 O2 73.43(19) . . ?
O7 Dy2 O2 71.88(19) . . ?
O6 Dy2 O8 92.9(2) . . ?
O9 Dy2 O8 141.9(2) . . ?
O10 Dy2 O8 146.2(2) . . ?
O7 Dy2 O8 83.3(2) . . ?
O2 Dy2 O8 72.8(2) . . ?
O6 Dy2 N4 125.5(2) . . ?
O9 Dy2 N4 74.1(2) . . ?
O10 Dy2 N4 131.1(2) . . ?
O7 Dy2 N4 67.1(2) . . ?
O2 Dy2 N4 128.0(2) . . ?
O8 Dy2 N4 72.0(3) . . ?
O6 Dy2 N5 62.5(2) . . ?
O9 Dy2 N5 75.4(2) . . ?
O10 Dy2 N5 135.2(2) . . ?
O7 Dy2 N5 129.5(2) . . ?
O2 Dy2 N5 137.4(2) . . ?
O8 Dy2 N5 74.2(2) . . ?
N4 Dy2 N5 63.1(2) . . ?
O6 Dy2 Dy1 128.88(16) . . ?
O9 Dy2 Dy1 129.14(18) . . ?
O10 Dy2 Dy1 80.05(14) . . ?
O7 Dy2 Dy1 36.14(13) . . ?
O2 Dy2 Dy1 35.99(13) . . ?
O8 Dy2 Dy1 72.02(16) . . ?
N4 Dy2 Dy1 96.50(16) . . ?
N5 Dy2 Dy1 144.73(16) . . ?
O11 Dy3 O15 92.0(3) . . ?
O11 Dy3 O14 92.8(2) . . ?
O15 Dy3 O14 71.1(2) . . ?
O11 Dy3 O12 163.8(2) . . ?
O15 Dy3 O12 101.9(2) . . ?
O14 Dy3 O12 84.0(2) . . ?
O11 Dy3 O17 92.0(2) . . ?
O15 Dy3 O17 145.2(2) . . ?
O14 Dy3 O17 74.2(2) . . ?
O12 Dy3 O17 71.9(2) . . ?
O11 Dy3 N7 125.8(2) . . ?
O15 Dy3 N7 73.9(3) . . ?
O14 Dy3 N7 128.0(3) . . ?
O12 Dy3 N7 67.1(2) . . ?
O17 Dy3 N7 128.9(2) . . ?
O11 Dy3 O13 91.3(2) . . ?
O15 Dy3 O13 141.1(2) . . ?
O14 Dy3 O13 147.4(2) . . ?
O12 Dy3 O13 83.2(2) . . ?
O17 Dy3 O13 73.3(2) . . ?
N7 Dy3 O13 72.9(2) . . ?
O11 Dy3 N8 61.9(2) . . ?
O15 Dy3 N8 73.9(2) . . ?
O14 Dy3 N8 135.6(2) . . ?
O12 Dy3 N8 129.8(2) . . ?
O17 Dy3 N8 136.8(2) . . ?
N7 Dy3 N8 63.8(2) . . ?
O13 Dy3 N8 73.6(2) . . ?
O11 Dy3 Dy4 127.69(15) . . ?
O15 Dy3 Dy4 131.32(18) . . ?
O14 Dy3 Dy4 79.04(15) . . ?
O12 Dy3 Dy4 36.11(14) . . ?
O17 Dy3 Dy4 35.91(14) . . ?
N7 Dy3 Dy4 97.32(17) . . ?
O13 Dy3 Dy4 72.99(15) . . ?
N8 Dy3 Dy4 145.32(17) . . ?
O16 Dy4 O20 89.5(3) . . ?
O16 Dy4 O19 84.0(2) . . ?
O20 Dy4 O19 71.7(2) . . ?
O16 Dy4 O17 165.3(2) . . ?
O20 Dy4 O17 100.5(2) . . ?
O19 Dy4 O17 88.8(2) . . ?
O16 Dy4 O12 93.6(2) . . ?
O20 Dy4 O12 145.2(2) . . ?
O19 Dy4 O12 74.2(2) . . ?
O17 Dy4 O12 72.1(2) . . ?
O16 Dy4 N10 126.2(3) . . ?
O20 Dy4 N10 75.5(2) . . ?
O19 Dy4 N10 134.8(3) . . ?
O17 Dy4 N10 67.4(2) . . ?
O12 Dy4 N10 127.5(2) . . ?
O16 Dy4 O18 94.5(3) . . ?
O20 Dy4 O18 144.8(2) . . ?
O19 Dy4 O18 143.5(2) . . ?
O17 Dy4 O18 83.7(3) . . ?
O12 Dy4 O18 69.5(2) . . ?
N10 Dy4 O18 74.0(3) . . ?
O16 Dy4 N11 62.7(2) . . ?
O20 Dy4 N11 73.2(3) . . ?
O19 Dy4 N11 131.2(2) . . ?
O17 Dy4 N11 130.5(2) . . ?
O12 Dy4 N11 137.7(3) . . ?
N10 Dy4 N11 63.5(3) . . ?
O18 Dy4 N11 77.7(3) . . ?
O16 Dy4 Dy3 128.98(17) . . ?
O20 Dy4 Dy3 126.73(17) . . ?
O19 Dy4 Dy3 77.01(15) . . ?
O17 Dy4 Dy3 36.47(14) . . ?
O12 Dy4 Dy3 35.76(14) . . ?
N10 Dy4 Dy3 99.58(18) . . ?
O18 Dy4 Dy3 75.86(17) . . ?
N11 Dy4 Dy3 151.76(19) . . ?
C34 O7 Dy2 120.0(5) . . ?
C34 O7 Dy1 125.6(6) . . ?
Dy2 O7 Dy1 108.1(2) . . ?
C1 O2 Dy1 120.0(6) . . ?
C1 O2 Dy2 128.4(6) . . ?
Dy1 O2 Dy2 107.7(2) . . ?
C66 O12 Dy3 118.9(6) . . ?
C66 O12 Dy4 127.4(6) . . ?
Dy3 O12 Dy4 108.1(2) . . ?
C24 O5 Dy1 138.4(6) . . ?
C58 O10 Dy2 136.2(6) . . ?
C26 O4 Dy1 133.4(6) . . ?
C129 O13 Dy3 126.2(7) . . ?
C129 O13 H13 107.0(19) . . ?
Dy3 O13 H13 122.9(19) . . ?
C43 O6 Dy2 124.6(6) . . ?
C75 O11 Dy3 124.9(6) . . ?
C56 O9 Dy2 138.9(6) . . ?
C97 O17 Dy4 120.2(6) . . ?
C97 O17 Dy3 126.1(6) . . ?
Dy4 O17 Dy3 107.6(2) . . ?
C122 O19 Dy4 132.9(6) . . ?
C135 O8 Dy2 124.6(6) . . ?
C135 O8 H8 110.2(18) . . ?
Dy2 O8 H8 123.7(18) . . ?
C11 O1 Dy1 125.1(7) . . ?
C107 O16 Dy4 124.8(7) . . ?
C120 O20 Dy4 135.5(7) . . ?
C90 O14 Dy3 137.0(6) . . ?
C74 N8 N9 118.9(8) . . ?
C74 N8 Dy3 120.5(7) . . ?
N9 N8 Dy3 120.7(5) . . ?
C41 N4 C33 121.8(8) . . ?
C41 N4 Dy2 121.8(6) . . ?
C33 N4 Dy2 116.1(5) . . ?
C131 O18 Dy4 141.9(7) . . ?
C131 O18 H18 108.9(17) . . ?
Dy4 O18 H18 108.7(15) . . ?
C73 N7 C65 118.7(8) . . ?
C73 N7 Dy3 122.8(6) . . ?
C65 N7 Dy3 118.4(6) . . ?
C88 O15 Dy3 138.7(7) . . ?
C42 N5 N6 117.9(8) . . ?
C42 N5 Dy2 122.0(7) . . ?
N6 N5 Dy2 120.1(5) . . ?
C105 N10 C101 119.6(8) . . ?
C105 N10 Dy4 122.6(7) . . ?
C101 N10 Dy4 117.7(6) . . ?
C133 O3 Dy1 138.5(6) . . ?
C133 O3 H3 108.4(17) . . ?
Dy1 O3 H3 111.6(16) . . ?
C43 N6 N5 106.8(8) . . ?
C75 N9 N8 107.9(8) . . ?
C11 N3 N2 107.5(8) . . ?
O7 C34 C35 125.6(9) . . ?
O7 C34 C33 117.0(8) . . ?
C35 C34 C33 117.4(8) . . ?
N4 C33 C34 118.0(8) . . ?
N4 C33 C38 120.4(9) . . ?
C34 C33 C38 121.6(9) . . ?
C106 N11 N12 118.8(8) . . ?
C106 N11 Dy4 121.0(7) . . ?
N12 N11 Dy4 119.9(5) . . ?
C9 N1 C5 122.1(8) . . ?
C9 N1 Dy1 121.0(6) . . ?
C5 N1 Dy1 116.9(6) . . ?
C10 N2 N3 119.4(8) . . ?
C10 N2 Dy1 119.9(7) . . ?
N3 N2 Dy1 120.5(5) . . ?
O12 C66 C67 123.2(9) . . ?
O12 C66 C65 118.5(9) . . ?
C67 C66 C65 118.2(9) . . ?
O11 C75 N9 124.5(10) . . ?
O11 C75 C76 116.7(10) . . ?
N9 C75 C76 118.8(10) . . ?
O10 C58 C57 123.0(9) . . ?
O10 C58 C59 116.1(8) . . ?
C57 C58 C59 120.8(9) . . ?
C54 C55 C50 119.3(9) . . ?
C54 C55 C56 122.5(9) . . ?
C50 C55 C56 118.0(9) . . ?
N10 C101 C102 123.1(9) . . ?
N10 C101 C97 117.1(9) . . ?
C102 C101 C97 119.7(10) . . ?
C39 C38 C37 125.0(9) . . ?
C39 C38 C33 117.0(9) . . ?
C37 C38 C33 118.0(9) . . ?
C64 C59 C60 117.9(9) . . ?
C64 C59 C58 118.9(10) . . ?
C60 C59 C58 123.1(9) . . ?
C82 C87 C86 118.0(10) . . ?
C82 C87 C88 120.1(11) . . ?
C86 C87 C88 121.8(10) . . ?
C49 C44 C45 118.8(11) . . ?
C49 C44 C43 118.5(11) . . ?
C45 C44 C43 122.7(10) . . ?
O4 C26 C25 123.8(8) . . ?
O4 C26 C27 117.1(8) . . ?
C25 C26 C27 119.0(9) . . ?
O9 C56 C57 124.4(9) . . ?
O9 C56 C55 114.9(8) . . ?
C57 C56 C55 120.6(9) . . ?
C22 C23 C18 119.2(9) . . ?
C22 C23 C24 122.6(9) . . ?
C18 C23 C24 118.2(10) . . ?
O5 C24 C25 123.0(9) . . ?
O5 C24 C23 117.3(8) . . ?
C25 C24 C23 119.7(9) . . ?
C32 C27 C28 116.7(9) . . ?
C32 C27 C26 119.1(10) . . ?
C28 C27 C26 124.0(9) . . ?
C48 C49 C44 120.5(12) . . ?
C48 C49 H49 119.8 . . ?
C44 C49 H49 119.8 . . ?
O14 C90 C89 122.1(10) . . ?
O14 C90 C91 115.8(10) . . ?
C89 C90 C91 122.0(11) . . ?
N8 C74 C73 117.7(9) . . ?
N8 C74 H74 121.1 . . ?
C73 C74 H74 121.1 . . ?
C34 C35 C36 120.6(9) . . ?
C34 C35 H35 119.7 . . ?
C36 C35 H35 119.7 . . ?
O6 C43 N6 125.5(10) . . ?
O6 C43 C44 117.9(10) . . ?
N6 C43 C44 116.6(10) . . ?
C36 C37 C38 119.6(9) . . ?
C36 C37 H37 120.2 . . ?
C38 C37 H37 120.2 . . ?
C26 C25 C24 123.4(9) . . ?
C26 C25 H25 118.3 . . ?
C24 C25 H25 118.3 . . ?
C53 C54 C55 118.0(9) . . ?
C53 C54 H54 121.0 . . ?
C55 C54 H54 121.0 . . ?
C58 C57 C56 122.8(9) . . ?
C58 C57 H57 118.6 . . ?
C56 C57 H57 118.6 . . ?
O2 C1 C2 124.8(10) . . ?
O2 C1 C5 117.1(9) . . ?
C2 C1 C5 118.0(9) . . ?
N7 C73 C72 121.7(9) . . ?
N7 C73 C74 114.8(8) . . ?
C72 C73 C74 123.4(9) . . ?
C21 C22 C23 119.3(10) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C52 C53 C54 123.1(10) . . ?
C52 C53 H53 118.4 . . ?
C54 C53 H53 118.4 . . ?
C107 N12 N11 106.9(8) . . ?
O1 C11 N3 124.3(10) . . ?
O1 C11 C12 115.8(10) . . ?
N3 C11 C12 119.9(11) . . ?
C51 C50 C55 118.7(10) . . ?
C51 C50 H50 120.6 . . ?
C55 C50 H50 120.6 . . ?
O17 C97 C98 124.6(9) . . ?
O17 C97 C101 117.3(9) . . ?
C98 C97 C101 118.0(10) . . ?
O19 C122 C121 124.2(10) . . ?
O19 C122 C123 116.7(10) . . ?
C121 C122 C123 119.0(11) . . ?
C53 C52 C51 119.7(10) . . ?
C53 C52 H52 120.1 . . ?
C51 C52 H52 120.1 . . ?
C37 C36 C35 122.6(10) . . ?
C37 C36 H36 118.7 . . ?
C35 C36 H36 118.7 . . ?
O15 C88 C89 124.5(11) . . ?
O15 C88 C87 113.9(10) . . ?
C89 C88 C87 121.6(11) . . ?
C27 C32 C31 121.1(10) . . ?
C27 C32 H32 119.5 . . ?
C31 C32 H32 119.5 . . ?
N4 C41 C40 120.9(9) . . ?
N4 C41 C42 116.1(8) . . ?
C40 C41 C42 123.0(9) . . ?
C52 C51 C50 121.0(10) . . ?
C52 C51 H51 119.5 . . ?
C50 C51 H51 119.5 . . ?
N7 C65 C70 123.3(9) . . ?
N7 C65 C66 115.6(8) . . ?
C70 C65 C66 121.1(10) . . ?
C95 C96 C91 122.2(12) . . ?
C95 C96 H96 118.9 . . ?
C91 C96 H96 118.9 . . ?
C92 C91 C96 117.1(11) . . ?
C92 C91 C90 122.8(11) . . ?
C96 C91 C90 120.1(11) . . ?
C88 C89 C90 124.6(11) . . ?
C88 C89 H89 117.7 . . ?
C90 C89 H89 117.7 . . ?
C21 C20 C19 120.7(10) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
N1 C9 C10 116.4(9) . . ?
N1 C9 C8 118.9(10) . . ?
C10 C9 C8 124.7(10) . . ?
C1 C2 C3 121.5(10) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 H2 119.2 . . ?
C17 C12 C13 119.0(11) . . ?
C17 C12 C11 119.5(11) . . ?
C13 C12 C11 121.5(11) . . ?
C20 C21 C22 121.4(11) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C39 C40 C41 118.6(9) . . ?
C39 C40 H40 120.7 . . ?
C41 C40 H40 120.7 . . ?
O20 C120 C121 123.0(11) . . ?
O20 C120 C119 116.0(11) . . ?
C121 C120 C119 120.8(11) . . ?
C114 C119 C118 118.5(11) . . ?
C114 C119 C120 119.7(12) . . ?
C118 C119 C120 121.8(12) . . ?
C122 C121 C120 124.4(11) . . ?
C122 C121 H121 117.8 . . ?
C120 C121 H121 117.8 . . ?
C128 C123 C124 118.6(11) . . ?
C128 C123 C122 118.6(11) . . ?
C124 C123 C122 122.8(11) . . ?
C100 C102 C101 120.5(10) . . ?
C100 C102 C103 124.2(10) . . ?
C101 C102 C103 115.3(10) . . ?
N5 C42 C41 116.8(9) . . ?
N5 C42 H42 121.6 . . ?
C41 C42 H42 121.6 . . ?
N1 C5 C6 121.8(9) . . ?
N1 C5 C1 118.1(9) . . ?
C6 C5 C1 120.0(10) . . ?
C40 C39 C38 121.3(9) . . ?
C40 C39 H39 119.4 . . ?
C38 C39 H39 119.4 . . ?
C66 C67 C68 119.4(9) . . ?
C66 C67 H67 120.3 . . ?
C68 C67 H67 120.3 . . ?
N2 C10 C9 118.7(10) . . ?
N2 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C87 C82 C83 121.0(12) . . ?
C87 C82 H82 119.5 . . ?
C83 C82 H82 119.5 . . ?
C19 C18 C23 121.0(11) . . ?
C19 C18 H18A 119.5 . . ?
C23 C18 H18A 119.5 . . ?
C81 C76 C77 117.4(10) . . ?
C81 C76 C75 119.2(11) . . ?
C77 C76 C75 123.3(10) . . ?
C18 C19 C20 118.5(10) . . ?
C18 C19 H19 120.8 . . ?
C20 C19 H19 120.8 . . ?
C29 C30 C31 120.6(10) . . ?
C29 C30 H30 119.7 . . ?
C31 C30 H30 119.7 . . ?
C85 C86 C87 119.4(11) . . ?
C85 C86 H86 120.3 . . ?
C87 C86 H86 120.3 . . ?
N11 C106 C105 117.1(10) . . ?
N11 C106 H106 121.4 . . ?
C105 C106 H106 121.4 . . ?
C59 C60 C61 120.0(10) . . ?
C59 C60 H60 120.0 . . ?
C61 C60 H60 120.0 . . ?
N10 C105 C104 119.9(10) . . ?
N10 C105 C106 115.5(9) . . ?
C104 C105 C106 124.5(10) . . ?
C27 C28 C29 121.7(10) . . ?
C27 C28 H28 119.1 . . ?
C29 C28 H28 119.1 . . ?
C59 C64 C63 122.2(10) . . ?
C59 C64 H64 118.9 . . ?
C63 C64 H64 118.9 . . ?
C30 C31 C32 120.1(10) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C119 C114 C115 122.0(13) . . ?
C119 C114 H114 119.0 . . ?
C115 C114 H114 119.0 . . ?
O16 C107 N12 125.7(11) . . ?
O16 C107 C113 117.8(11) . . ?
N12 C107 C113 116.5(11) . . ?
C84 C85 C86 121.1(12) . . ?
C84 C85 H85 119.5 . . ?
C86 C85 H85 119.5 . . ?
C117 C116 C115 121.5(13) . . ?
C117 C116 H116 119.3 . . ?
C115 C116 H116 119.3 . . ?
C46 C45 C44 120.3(11) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C61 C62 C63 120.9(10) . . ?
C61 C62 H62 119.6 . . ?
C63 C62 H62 119.6 . . ?
C16 C17 C12 121.8(12) . . ?
C16 C17 H17 119.1 . . ?
C12 C17 H17 119.1 . . ?
C30 C29 C28 119.7(10) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C71 C72 C73 119.7(9) . . ?
C71 C72 H72 120.1 . . ?
C73 C72 H72 120.1 . . ?
C84 C83 C82 118.9(11) . . ?
C84 C83 H83 120.6 . . ?
C82 C83 H83 120.6 . . ?
C112 C113 C108 117.2(12) . . ?
C112 C113 C107 119.2(11) . . ?
C108 C113 C107 123.6(12) . . ?
C80 C81 C76 120.7(11) . . ?
C80 C81 H81 119.7 . . ?
C76 C81 H81 119.7 . . ?
C4 C6 C7 127.0(10) . . ?
C4 C6 C5 118.8(10) . . ?
C7 C6 C5 114.2(10) . . ?
C97 C98 C99 121.3(10) . . ?
C97 C98 H98 119.4 . . ?
C99 C98 H98 119.4 . . ?
C85 C84 C83 121.6(11) . . ?
C85 C84 H84 119.2 . . ?
C83 C84 H84 119.2 . . ?
C117 C118 C119 118.6(12) . . ?
C117 C118 H118 120.7 . . ?
C119 C118 H118 120.7 . . ?
C116 C115 C114 117.6(12) . . ?
C116 C115 H115 121.2 . . ?
C114 C115 H115 121.2 . . ?
C3 C4 C6 120.6(10) . . ?
C3 C4 H4 119.7 . . ?
C6 C4 H4 119.7 . . ?
C94 C95 C96 118.6(12) . . ?
C94 C95 H95 120.7 . . ?
C96 C95 H95 120.7 . . ?
C69 C70 C71 125.7(9) . . ?
C69 C70 C65 118.9(9) . . ?
C71 C70 C65 115.4(10) . . ?
C123 C124 C125 119.7(12) . . ?
C123 C124 H124 120.1 . . ?
C125 C124 H124 120.1 . . ?
C47 C48 C49 119.3(11) . . ?
C47 C48 H48 120.3 . . ?
C49 C48 H48 120.3 . . ?
C4 C3 C2 120.8(10) . . ?
C4 C3 H3B 119.6 . . ?
C2 C3 H3B 119.6 . . ?
C99 C100 C102 118.8(10) . . ?
C99 C100 H100 120.6 . . ?
C102 C100 H100 120.6 . . ?
C62 C61 C60 120.2(11) . . ?
C62 C61 H61 119.9 . . ?
C60 C61 H61 119.9 . . ?
C91 C92 C93 120.2(11) . . ?
C91 C92 H92 119.9 . . ?
C93 C92 H92 119.9 . . ?
C125 C126 C127 123.1(12) . . ?
C125 C126 H126 118.5 . . ?
C127 C126 H126 118.5 . . ?
C126 C127 C128 117.7(12) . . ?
C126 C127 H127 121.1 . . ?
C128 C127 H127 121.1 . . ?
C68 C69 C70 119.8(9) . . ?
C68 C69 H69 120.1 . . ?
C70 C69 H69 120.1 . . ?
C72 C71 C70 121.1(9) . . ?
C72 C71 H71 119.5 . . ?
C70 C71 H71 119.5 . . ?
C8 C7 C6 123.8(10) . . ?
C8 C7 H7 118.1 . . ?
C6 C7 H7 118.1 . . ?
C123 C128 C127 121.4(12) . . ?
C123 C128 H128 119.3 . . ?
C127 C128 H128 119.3 . . ?
C104 C103 C102 120.2(10) . . ?
C104 C103 H103 119.9 . . ?
C102 C103 H103 119.9 . . ?
C111 C112 C113 121.6(12) . . ?
C111 C112 H112 119.2 . . ?
C113 C112 H112 119.2 . . ?
C62 C63 C64 118.8(10) . . ?
C62 C63 H63 120.6 . . ?
C64 C63 H63 120.6 . . ?
C103 C104 C105 121.7(10) . . ?
C103 C104 H104 119.2 . . ?
C105 C104 H104 119.2 . . ?
C69 C68 C67 122.6(10) . . ?
C69 C68 H68 118.7 . . ?
C67 C68 H68 118.7 . . ?
C126 C125 C124 119.5(12) . . ?
C126 C125 H125 120.2 . . ?
C124 C125 H125 120.2 . . ?
C93 C94 C95 122.3(12) . . ?
C93 C94 H94 118.8 . . ?
C95 C94 H94 118.8 . . ?
C46 C47 C48 121.3(12) . . ?
C46 C47 H47 119.4 . . ?
C48 C47 H47 119.4 . . ?
C7 C8 C9 119.0(10) . . ?
C7 C8 H8A 120.5 . . ?
C9 C8 H8A 120.5 . . ?
C47 C46 C45 119.7(12) . . ?
C47 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C78 C77 C76 122.1(11) . . ?
C78 C77 H77 118.9 . . ?
C76 C77 H77 118.9 . . ?
C79 C80 C81 120.6(11) . . ?
C79 C80 H80 119.7 . . ?
C81 C80 H80 119.7 . . ?
C110 C111 C112 120.7(13) . . ?
C110 C111 H111 119.6 . . ?
C112 C111 H111 119.6 . . ?
C94 C93 C92 119.5(12) . . ?
C94 C93 H93 120.2 . . ?
C92 C93 H93 120.2 . . ?
C116 C117 C118 121.8(14) . . ?
C116 C117 H117 119.1 . . ?
C118 C117 H117 119.1 . . ?
C100 C99 C98 121.5(11) . . ?
C100 C99 H99 119.3 . . ?
C98 C99 H99 119.3 . . ?
C80 C79 C78 120.4(11) . . ?
C80 C79 H79 119.8 . . ?
C78 C79 H79 119.8 . . ?
C134 C133 O3 105.6(10) . . ?
C134 C133 H13I 110.6 . . ?
O3 C133 H13I 110.6 . . ?
C134 C133 H13J 110.6 . . ?
O3 C133 H13J 110.6 . . ?
H13I C133 H13J 108.8 . . ?
C109 C108 C113 119.4(12) . . ?
C109 C108 H108 120.3 . . ?
C113 C108 H108 120.3 . . ?
C17 C16 C15 118.9(12) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C132 C131 O18 110.6(11) . . ?
C132 C131 H13A 109.5 . . ?
O18 C131 H13A 109.5 . . ?
C132 C131 H13B 109.5 . . ?
O18 C131 H13B 109.5 . . ?
H13A C131 H13B 108.1 . . ?
C77 C78 C79 118.7(12) . . ?
C77 C78 H78 120.7 . . ?
C79 C78 H78 120.7 . . ?
C111 C110 C109 119.5(12) . . ?
C111 C110 H110 120.2 . . ?
C109 C110 H110 120.2 . . ?
C131 C132 H13C 109.5 . . ?
C131 C132 H13D 109.5 . . ?
H13C C132 H13D 109.5 . . ?
C131 C132 H13E 109.5 . . ?
H13C C132 H13E 109.5 . . ?
H13D C132 H13E 109.5 . . ?
C133 C134 H13K 109.5 . . ?
C133 C134 H13L 109.5 . . ?
H13K C134 H13L 109.5 . . ?
C133 C134 H13M 109.5 . . ?
H13K C134 H13M 109.5 . . ?
H13L C134 H13M 109.5 . . ?
C110 C109 C108 121.3(12) . . ?
C110 C109 H109 119.4 . . ?
C108 C109 H109 119.4 . . ?
C14 C15 C16 120.4(12) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C14 C13 120.3(12) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C13 C12 119.2(12) . . ?
C14 C13 H13N 120.4 . . ?
C12 C13 H13N 120.4 . . ?
C129 C130 H13F 109.5 . . ?
C129 C130 H13G 109.5 . . ?
H13F C130 H13G 109.5 . . ?
C129 C130 H13H 109.5 . . ?
H13F C130 H13H 109.5 . . ?
H13G C130 H13H 109.5 . . ?
C130 C129 O13 108.9(12) . . ?
C130 C129 H12A 109.9 . . ?
O13 C129 H12A 109.9 . . ?
C130 C129 H12B 109.9 . . ?
O13 C129 H12B 109.9 . . ?
H12A C129 H12B 108.3 . . ?
C136 C135 O8 101.4(11) . . ?
C136 C135 H13P 111.5 . . ?
O8 C135 H13P 111.5 . . ?
C136 C135 H13Q 111.5 . . ?
O8 C135 H13Q 111.5 . . ?
H13P C135 H13Q 109.3 . . ?
C135 C136 H13O 109.5 . . ?
C135 C136 H13R 109.5 . . ?
H13O C136 H13R 109.5 . . ?
C135 C136 H13S 109.5 . . ?
H13O C136 H13S 109.5 . . ?
H13R C136 H13S 109.5 . . ?
_refine_diff_density_max 2.228
_refine_diff_density_min -1.573
_refine_diff_density_rms 0.163
_shelx_res_file
;
YZF-232-1.res created by SHELXL-2014/7
TITL yzf-232-1_a.res in P2(1)/c
REM Old TITL YZF-232-1 in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.181, Rweak 0.015, Alpha 0.085, Orientation as input
REM Formula found by SHELXT: C121 O24 N9 Dy4
CELL 0.71073 24.7131 18.3426 27.2646 90 101.707 90
ZERR 8 0.0014 0.0008 0.0025 0 0.007 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Dy N O
UNIT 544 448 16 48 80
DFIX 0.85 0.01 O13 H13
DFIX 0.85 0.01 O18 H18
DFIX 0.85 0.01 O3 H3
DFIX 0.85 0.01 O8 H8
DANG 1.943296 0.02 C129 H13
DANG 3.009485 0.02 Dy3 H13
DANG 1.87433 0.02 C131 H18
DANG 2.830427 0.02 Dy4 H18
DANG 1.936157 0.02 C133 H3
DANG 2.908616 0.02 Dy1 H3
DANG 2.060962 0.02 C135 H8
DANG 3.027473 0.02 Dy2 H8
DELU 0.0001 0.0001 C135 C136
L.S. 4 0 0
PLAN 30
BOND $H
list 4
fmap 2 53
acta
delu 0.001 0.01 o8 c135
dfix 1.45 c135 c136
isor 0.05 c135
isor 0.05 O8
simu 0.005 0.01 3.8 $c
delu 0.001 0.01 o3 c133
delu 0.001 0.01 o13 c129
delu 0.001 0.01 o18 c131
REM
REM
REM
WGHT 0.060800 59.549900
FVAR 0.06769
DY1 3 0.689824 0.511862 0.417225 11.00000 0.04264 0.03349 =
0.03803 0.00015 0.00234 0.00852
DY2 3 0.556455 0.461950 0.325021 11.00000 0.04195 0.03514 =
0.03453 0.00075 0.00470 0.00721
DY3 3 0.801405 0.036511 0.570397 11.00000 0.04230 0.04156 =
0.04109 -0.00273 0.00003 -0.01196
DY4 3 0.936922 -0.000065 0.664113 11.00000 0.04586 0.04052 =
0.04872 0.00014 -0.00424 -0.01290
O7 5 0.628386 0.548187 0.342525 11.00000 0.04311 0.03674 =
0.03809 0.00069 0.00250 0.00405
O2 5 0.622615 0.419655 0.395278 11.00000 0.05561 0.03340 =
0.03154 -0.00088 0.01035 0.00363
O12 5 0.875220 -0.046590 0.592461 11.00000 0.04590 0.03453 =
0.05530 -0.00099 -0.00086 -0.00693
O5 5 0.701210 0.505002 0.503028 11.00000 0.07085 0.04686 =
0.03424 0.00157 0.00134 0.02477
O10 5 0.619419 0.390716 0.293269 11.00000 0.05040 0.04825 =
0.03636 -0.00882 0.00440 0.02068
O4 5 0.625356 0.589227 0.443556 11.00000 0.04579 0.04555 =
0.03881 -0.01238 0.00536 0.01408
O13 5 0.776589 -0.007917 0.647115 11.00000 0.05989 0.05935 =
0.04837 0.00936 0.00082 -0.00801
H13 2 0.792327 -0.044610 0.663437 11.00000 -1.50000
O6 5 0.501087 0.362815 0.325153 11.00000 0.04550 0.03650 =
0.07233 -0.00819 0.00126 0.00787
O11 5 0.743800 0.134098 0.568082 11.00000 0.04867 0.03627 =
0.07020 0.00433 -0.01004 -0.00868
O9 5 0.536648 0.470314 0.239874 11.00000 0.06574 0.06466 =
0.03732 0.00128 0.00792 0.02512
O17 5 0.866894 0.087558 0.638533 11.00000 0.04133 0.03619 =
0.06208 -0.00376 -0.00783 -0.00669
O19 5 0.872614 -0.071914 0.695140 11.00000 0.04729 0.05002 =
0.05978 0.01471 0.00368 -0.00954
O8 5 0.531041 0.513424 0.400205 11.00000 0.05750 0.06988 =
0.05816 -0.02140 0.00703 0.01015
H8 2 0.547813 0.549403 0.416621 11.00000 -1.50000
O1 5 0.740486 0.615034 0.420931 11.00000 0.05367 0.04463 =
0.07633 0.00394 -0.00403 0.00634
O16 5 0.988826 -0.102152 0.674974 11.00000 0.05766 0.04106 =
0.08298 0.00491 -0.00406 -0.01170
O20 5 0.952570 0.014701 0.750238 11.00000 0.06884 0.04508 =
0.05188 -0.00543 0.00036 -0.00999
O14 5 0.863975 0.101879 0.533828 11.00000 0.05026 0.05791 =
0.05030 0.00419 0.00258 -0.01719
N8 4 0.698922 0.013700 0.549883 11.00000 0.05381 0.03443 =
0.04365 -0.01049 -0.00002 -0.01347
N4 4 0.524263 0.588075 0.305694 11.00000 0.03790 0.03897 =
0.04801 0.00114 0.00428 0.01928
O18 5 0.966552 0.036448 0.587650 11.00000 0.06431 0.08496 =
0.06559 0.00807 -0.01203 -0.02837
H18 2 0.941885 0.023725 0.562585 11.00000 -1.50000
N7 4 0.772755 -0.089974 0.555875 11.00000 0.04041 0.04104 =
0.05419 0.00042 0.00078 -0.01643
O15 5 0.778027 0.022329 0.484433 11.00000 0.05631 0.08141 =
0.04718 -0.00510 0.00137 -0.01973
N5 4 0.453887 0.481692 0.302852 11.00000 0.04519 0.03049 =
0.05080 -0.00537 0.01599 0.01305
N10 4 0.970777 0.124590 0.678240 11.00000 0.05529 0.04021 =
0.05533 -0.00239 -0.00497 -0.01857
O3 5 0.721339 0.461494 0.344276 11.00000 0.07465 0.10694 =
0.03810 0.00450 0.01220 0.02882
H3 2 0.703395 0.479618 0.316802 11.00000 -1.50000
N6 4 0.417635 0.423603 0.305911 11.00000 0.05077 0.03983 =
0.05683 -0.00313 0.00568 0.00267
N9 4 0.662093 0.070116 0.550072 11.00000 0.04391 0.04075 =
0.05663 -0.00058 0.00446 0.00262
N3 4 0.825683 0.562760 0.451895 11.00000 0.04441 0.04606 =
0.08030 0.00513 -0.00495 0.00387
C34 1 0.619626 0.617481 0.325855 11.00000 0.05882 0.03911 =
0.06341 0.01317 0.01135 0.00462
C33 1 0.563912 0.638896 0.307821 11.00000 0.05787 0.03836 =
0.06504 0.01339 0.01358 0.00472
N11 4 1.039396 0.015267 0.693726 11.00000 0.05023 0.04896 =
0.05954 -0.00274 -0.00063 -0.01748
N1 4 0.725969 0.389843 0.442679 11.00000 0.03980 0.03753 =
0.05467 0.00756 0.00189 0.02175
N2 4 0.792241 0.502128 0.450114 11.00000 0.04487 0.04499 =
0.05958 0.00632 0.01205 0.00621
C66 1 0.867008 -0.117090 0.578657 11.00000 0.05304 0.04658 =
0.07329 -0.00901 0.00189 -0.00598
C75 1 0.690661 0.130247 0.560876 11.00000 0.07110 0.05069 =
0.07596 0.00007 0.00693 0.00059
C58 1 0.621659 0.361826 0.251195 11.00000 0.05536 0.04338 =
0.05454 -0.00487 0.00864 0.00860
C55 1 0.523749 0.472740 0.152529 11.00000 0.05566 0.04135 =
0.04681 -0.00250 0.00606 0.00112
C101 1 0.934015 0.179249 0.665827 11.00000 0.06218 0.04899 =
0.08262 -0.00893 0.00231 -0.00792
C38 1 0.549841 0.711728 0.292395 11.00000 0.05952 0.03926 =
0.06558 0.01424 0.01203 0.00629
C59 1 0.657160 0.295359 0.253098 11.00000 0.05757 0.04504 =
0.05687 -0.00559 0.00822 0.01057
C87 1 0.763247 0.011854 0.398412 11.00000 0.06892 0.05598 =
0.06093 -0.00064 0.00384 -0.00032
C44 1 0.419199 0.297583 0.329096 11.00000 0.07640 0.05101 =
0.07288 0.00642 0.00717 -0.00011
C26 1 0.625533 0.624426 0.483449 11.00000 0.05435 0.04018 =
0.05455 -0.00372 0.00425 0.00926
C56 1 0.552327 0.442986 0.202888 11.00000 0.05422 0.04145 =
0.04740 -0.00241 0.00678 0.00236
C23 1 0.720320 0.523295 0.589154 11.00000 0.06060 0.04291 =
0.05005 -0.00048 0.00432 0.00735
C24 1 0.691036 0.542294 0.537886 11.00000 0.05896 0.04249 =
0.05118 -0.00014 0.00423 0.00735
C27 1 0.594519 0.694274 0.478808 11.00000 0.05559 0.04036 =
0.05787 -0.00506 0.00194 0.01091
C49 1 0.448913 0.233513 0.337562 11.00000 0.07735 0.05148 =
0.07512 0.00833 0.00659 -0.00017
AFIX 43
H49 2 0.486323 0.233351 0.336631 11.00000 -1.20000
AFIX 0
C90 1 0.866689 0.125125 0.489352 11.00000 0.06543 0.05369 =
0.06765 0.00305 0.00900 -0.00196
C74 1 0.680099 -0.050206 0.538015 11.00000 0.05377 0.04675 =
0.07358 -0.00878 0.00451 -0.00661
AFIX 43
H74 2 0.642364 -0.058497 0.527810 11.00000 -1.20000
AFIX 0
C35 1 0.659570 0.667966 0.324400 11.00000 0.05977 0.04210 =
0.06605 0.01498 0.00977 0.00417
AFIX 43
H35 2 0.696587 0.654712 0.333336 11.00000 -1.20000
AFIX 0
C43 1 0.448607 0.365267 0.319201 11.00000 0.07678 0.05336 =
0.07286 0.00710 0.01151 0.00150
C37 1 0.592719 0.761996 0.294662 11.00000 0.06177 0.03975 =
0.06680 0.01472 0.01121 0.00528
AFIX 43
H37 2 0.584894 0.810444 0.285949 11.00000 -1.20000
AFIX 0
C25 1 0.654565 0.602731 0.530405 11.00000 0.05665 0.04075 =
0.05104 -0.00249 0.00468 0.00970
AFIX 43
H25 2 0.649773 0.629260 0.558279 11.00000 -1.20000
AFIX 0
C54 1 0.550133 0.478145 0.111920 11.00000 0.05680 0.04093 =
0.04728 -0.00202 0.00663 0.00049
AFIX 43
H54 2 0.585576 0.459769 0.113848 11.00000 -1.20000
AFIX 0
C57 1 0.591100 0.387083 0.205972 11.00000 0.05690 0.04359 =
0.05048 -0.00422 0.00762 0.00582
AFIX 43
H57 2 0.596735 0.365794 0.176458 11.00000 -1.20000
AFIX 0
C1 1 0.634359 0.350547 0.410266 11.00000 0.06867 0.04787 =
0.06909 0.00694 0.01022 0.00531
C73 1 0.719855 -0.109741 0.541027 11.00000 0.05150 0.04416 =
0.07287 -0.01019 0.00489 -0.00709
C22 1 0.695256 0.526176 0.629788 11.00000 0.06149 0.04626 =
0.05284 0.00029 0.00399 0.00663
AFIX 43
H22 2 0.659062 0.542650 0.626081 11.00000 -1.20000
AFIX 0
C53 1 0.522307 0.511225 0.069312 11.00000 0.05946 0.04369 =
0.04870 -0.00182 0.00613 -0.00051
AFIX 43
H53 2 0.539890 0.515784 0.042370 11.00000 -1.20000
AFIX 0
N12 4 1.073326 -0.045708 0.702404 11.00000 0.05407 0.05626 =
0.08658 -0.00131 -0.01095 -0.00099
C11 1 0.793794 0.618321 0.433896 11.00000 0.06601 0.06034 =
0.09988 0.00912 0.00129 -0.00500
C50 1 0.470200 0.501040 0.148168 11.00000 0.05779 0.04477 =
0.04962 -0.00104 0.00614 0.00192
AFIX 43
H50 2 0.452322 0.499102 0.175046 11.00000 -1.20000
AFIX 0
C97 1 0.877861 0.159154 0.646596 11.00000 0.06243 0.04799 =
0.08201 -0.01022 0.00200 -0.00654
C122 1 0.874470 -0.104436 0.735645 11.00000 0.06068 0.05774 =
0.07140 0.00899 0.00519 -0.00130
C52 1 0.471202 0.537249 0.064531 11.00000 0.06105 0.04416 =
0.04886 -0.00091 0.00464 0.00103
AFIX 43
H52 2 0.453780 0.559122 0.034721 11.00000 -1.20000
AFIX 0
C36 1 0.645413 0.739916 0.309526 11.00000 0.06167 0.04235 =
0.06779 0.01451 0.01079 0.00424
AFIX 43
H36 2 0.673591 0.773666 0.309966 11.00000 -1.20000
AFIX 0
C88 1 0.793669 0.044969 0.446057 11.00000 0.06739 0.05459 =
0.06198 -0.00038 0.00586 -0.00023
C32 1 0.589045 0.733608 0.435305 11.00000 0.05912 0.04417 =
0.05935 -0.00339 0.00256 0.01084
AFIX 43
H32 2 0.601795 0.714023 0.408293 11.00000 -1.20000
AFIX 0
C41 1 0.471473 0.603727 0.290229 11.00000 0.05829 0.03921 =
0.06874 0.01156 0.01374 0.00701
C51 1 0.444642 0.531732 0.103320 11.00000 0.05765 0.04557 =
0.05175 -0.00014 0.00299 0.00225
AFIX 43
H51 2 0.408635 0.548934 0.099570 11.00000 -1.20000
AFIX 0
C65 1 0.811956 -0.141543 0.560485 11.00000 0.05395 0.04693 =
0.07484 -0.00925 0.00136 -0.00680
C96 1 0.926435 0.224649 0.531141 11.00000 0.06589 0.05578 =
0.07519 0.00205 0.00809 -0.00507
AFIX 43
H96 2 0.920339 0.207173 0.561580 11.00000 -1.20000
AFIX 0
C91 1 0.903870 0.187130 0.487580 11.00000 0.06634 0.05492 =
0.07025 0.00477 0.01007 -0.00284
C89 1 0.834260 0.096107 0.446483 11.00000 0.06723 0.05394 =
0.06568 0.00140 0.00756 -0.00137
AFIX 43
H89 2 0.840399 0.112406 0.415775 11.00000 -1.20000
AFIX 0
C20 1 0.777070 0.480748 0.681948 11.00000 0.06471 0.04986 =
0.05392 0.00157 0.00135 0.00598
AFIX 43
H20 2 0.795772 0.466370 0.713573 11.00000 -1.20000
AFIX 0
C9 1 0.778443 0.380238 0.464278 11.00000 0.06719 0.05018 =
0.07216 0.00655 0.01201 0.00697
C2 1 0.597724 0.295106 0.403470 11.00000 0.07015 0.05018 =
0.07095 0.00879 0.01006 0.00439
AFIX 43
H2 2 0.561206 0.304285 0.388105 11.00000 -1.20000
AFIX 0
C12 1 0.818801 0.688714 0.425288 11.00000 0.06673 0.06226 =
0.10558 0.01259 -0.00050 -0.00724
C21 1 0.724058 0.504611 0.675592 11.00000 0.06426 0.04923 =
0.05277 0.00018 0.00418 0.00461
AFIX 43
H21 2 0.707047 0.506282 0.703029 11.00000 -1.20000
AFIX 0
C40 1 0.454661 0.674013 0.273501 11.00000 0.06046 0.04082 =
0.07206 0.01432 0.01074 0.00796
AFIX 43
H40 2 0.417464 0.684635 0.261918 11.00000 -1.20000
AFIX 0
C120 1 0.943621 -0.023019 0.786871 11.00000 0.07117 0.06340 =
0.06666 0.00031 0.00096 0.00444
C119 1 0.977928 -0.005029 0.836500 11.00000 0.07436 0.06615 =
0.06750 -0.00041 0.00083 0.00505
C121 1 0.906539 -0.082270 0.781112 11.00000 0.06533 0.05976 =
0.06921 0.00540 0.00515 0.00155
AFIX 43
H121 2 0.903319 -0.108277 0.809661 11.00000 -1.20000
AFIX 0
C123 1 0.842480 -0.173828 0.733553 11.00000 0.06072 0.05874 =
0.07537 0.01218 0.00534 -0.00409
C102 1 0.947903 0.253596 0.674673 11.00000 0.06357 0.04936 =
0.08530 -0.01093 0.00188 -0.00737
C42 1 0.433062 0.543767 0.290116 11.00000 0.06066 0.04229 =
0.07255 0.01143 0.01346 0.00776
AFIX 43
H42 2 0.395041 0.550551 0.281142 11.00000 -1.20000
AFIX 0
C5 1 0.690331 0.334947 0.434534 11.00000 0.06584 0.04736 =
0.07023 0.00752 0.01112 0.00521
C39 1 0.494115 0.726656 0.274569 11.00000 0.06094 0.04122 =
0.06963 0.01368 0.01249 0.00752
AFIX 43
H39 2 0.483481 0.773309 0.263162 11.00000 -1.20000
AFIX 0
C67 1 0.909649 -0.167123 0.581570 11.00000 0.05339 0.04919 =
0.07736 -0.01253 0.00065 -0.00605
AFIX 43
H67 2 0.946186 -0.152438 0.592068 11.00000 -1.20000
AFIX 0
C10 1 0.812771 0.442802 0.468570 11.00000 0.06500 0.05452 =
0.07696 0.00610 0.00884 0.00579
AFIX 43
H10 2 0.849688 0.440156 0.484672 11.00000 -1.20000
AFIX 0
C82 1 0.711443 -0.018420 0.396039 11.00000 0.07081 0.05885 =
0.06291 -0.00342 0.00344 -0.00009
AFIX 43
H82 2 0.695547 -0.017126 0.424159 11.00000 -1.20000
AFIX 0
C18 1 0.774656 0.498496 0.595790 11.00000 0.06092 0.04815 =
0.05309 0.00125 0.00502 0.00629
AFIX 43
H18A 2 0.791701 0.496063 0.568397 11.00000 -1.20000
AFIX 0
C76 1 0.660765 0.199016 0.567219 11.00000 0.07044 0.04980 =
0.07685 0.00194 0.00543 0.00222
C19 1 0.803357 0.477625 0.642156 11.00000 0.06268 0.04828 =
0.05867 -0.00230 0.00330 0.00891
AFIX 43
H19 2 0.839759 0.461734 0.646542 11.00000 -1.20000
AFIX 0
C30 1 0.545384 0.830790 0.469486 11.00000 0.06047 0.04504 =
0.06428 -0.00481 0.00163 0.01262
AFIX 43
H30 2 0.529324 0.876852 0.466363 11.00000 -1.20000
AFIX 0
C86 1 0.786923 0.006757 0.355628 11.00000 0.07175 0.05754 =
0.06144 -0.00053 0.00415 -0.00048
AFIX 43
H86 2 0.821749 0.026212 0.355972 11.00000 -1.20000
AFIX 0
C106 1 1.060577 0.078234 0.705185 11.00000 0.06271 0.05519 =
0.08773 -0.00775 0.00330 -0.00881
AFIX 43
H106 2 1.097994 0.083827 0.718883 11.00000 -1.20000
AFIX 0
C60 1 0.673384 0.267124 0.211812 11.00000 0.06087 0.04905 =
0.05896 -0.00509 0.00821 0.01131
AFIX 43
H60 2 0.664388 0.291215 0.181225 11.00000 -1.20000
AFIX 0
C105 1 1.023873 0.140194 0.695928 11.00000 0.06224 0.05158 =
0.08487 -0.00828 0.00504 -0.01006
C28 1 0.573509 0.725452 0.517070 11.00000 0.05748 0.04468 =
0.05898 -0.00421 0.00298 0.01038
AFIX 43
H28 2 0.575889 0.699982 0.546926 11.00000 -1.20000
AFIX 0
C64 1 0.673118 0.259706 0.297513 11.00000 0.06302 0.05014 =
0.06166 -0.00292 0.00903 0.01048
AFIX 43
H64 2 0.664061 0.279564 0.326185 11.00000 -1.20000
AFIX 0
C31 1 0.564791 0.802157 0.430935 11.00000 0.06085 0.04689 =
0.06253 -0.00089 0.00139 0.00906
AFIX 43
H31 2 0.561925 0.828392 0.401331 11.00000 -1.20000
AFIX 0
C114 1 1.028327 0.028260 0.839402 11.00000 0.07553 0.06921 =
0.06870 -0.00170 0.00016 0.00546
AFIX 43
H114 2 1.040184 0.039005 0.809952 11.00000 -1.20000
AFIX 0
C107 1 1.041182 -0.103469 0.690619 11.00000 0.07335 0.06254 =
0.10075 0.00135 -0.00081 0.00181
C85 1 0.758009 -0.027279 0.313359 11.00000 0.07449 0.05993 =
0.06168 -0.00164 0.00394 -0.00020
AFIX 43
H85 2 0.774015 -0.031921 0.285449 11.00000 -1.20000
AFIX 0
C116 1 1.043315 0.029036 0.927549 11.00000 0.08135 0.07273 =
0.07004 -0.00243 -0.00216 0.00620
AFIX 43
H116 2 1.065215 0.040416 0.958541 11.00000 -1.20000
AFIX 0
C45 1 0.363693 0.296765 0.331419 11.00000 0.07781 0.05289 =
0.07563 0.00617 0.00706 -0.00040
AFIX 43
H45 2 0.343021 0.339401 0.325594 11.00000 -1.20000
AFIX 0
C62 1 0.717039 0.168118 0.260024 11.00000 0.06445 0.05116 =
0.06356 -0.00558 0.00773 0.01265
AFIX 43
H62 2 0.737106 0.124930 0.262268 11.00000 -1.20000
AFIX 0
C17 1 0.785898 0.749080 0.414690 11.00000 0.06940 0.06334 =
0.10746 0.01298 -0.00026 -0.00781
AFIX 43
H17 2 0.748023 0.744433 0.412590 11.00000 -1.20000
AFIX 0
C29 1 0.549008 0.793571 0.512188 11.00000 0.05909 0.04644 =
0.06158 -0.00687 0.00285 0.01155
AFIX 43
H29 2 0.535112 0.813403 0.538501 11.00000 -1.20000
AFIX 0
C72 1 0.704996 -0.180980 0.527770 11.00000 0.05374 0.04753 =
0.07703 -0.01056 0.00221 -0.00860
AFIX 43
H72 2 0.668020 -0.193090 0.516493 11.00000 -1.20000
AFIX 0
C83 1 0.682671 -0.050904 0.352005 11.00000 0.07219 0.06110 =
0.06378 -0.00316 0.00232 -0.00102
AFIX 43
H83 2 0.647512 -0.070054 0.350409 11.00000 -1.20000
AFIX 0
C113 1 1.068360 -0.175523 0.699099 11.00000 0.07657 0.06396 =
0.10424 0.00369 -0.00084 0.00506
C81 1 0.689656 0.264049 0.573259 11.00000 0.07180 0.05056 =
0.07739 0.00165 0.00630 0.00306
AFIX 43
H81 2 0.727215 0.264267 0.572942 11.00000 -1.20000
AFIX 0
C6 1 0.705903 0.262193 0.450700 11.00000 0.06877 0.04849 =
0.07135 0.00699 0.01016 0.00413
C98 1 0.839934 0.213136 0.635586 11.00000 0.06504 0.04925 =
0.08653 -0.01184 0.00000 -0.00644
AFIX 43
H98 2 0.803323 0.201282 0.622219 11.00000 -1.20000
AFIX 0
C84 1 0.706863 -0.053995 0.311758 11.00000 0.07545 0.06139 =
0.06253 -0.00243 -0.00003 -0.00025
AFIX 43
H84 2 0.687738 -0.075066 0.282271 11.00000 -1.20000
AFIX 0
C118 1 0.960768 -0.021018 0.880696 11.00000 0.07721 0.06991 =
0.06985 -0.00065 0.00034 0.00369
AFIX 43
H118 2 0.926817 -0.043258 0.880071 11.00000 -1.20000
AFIX 0
C115 1 1.061802 0.046184 0.884627 11.00000 0.07706 0.07183 =
0.07106 -0.00308 0.00032 0.00418
AFIX 43
H115 2 1.095679 0.069053 0.886093 11.00000 -1.20000
AFIX 0
C4 1 0.666683 0.207428 0.440792 11.00000 0.07050 0.04898 =
0.07268 0.00708 0.00960 0.00309
AFIX 43
H4 2 0.676855 0.159455 0.449015 11.00000 -1.20000
AFIX 0
C95 1 0.957576 0.286941 0.530823 11.00000 0.06801 0.05854 =
0.07348 0.00472 0.00876 -0.00709
AFIX 43
H95 2 0.971402 0.311954 0.560380 11.00000 -1.20000
AFIX 0
C70 1 0.800563 -0.215603 0.547959 11.00000 0.05424 0.04684 =
0.07634 -0.01119 0.00177 -0.00665
C124 1 0.819558 -0.198245 0.772992 11.00000 0.06291 0.06169 =
0.07638 0.01004 0.00630 -0.00390
AFIX 43
H124 2 0.821431 -0.169450 0.801362 11.00000 -1.20000
AFIX 0
C48 1 0.423547 0.169747 0.347389 11.00000 0.07986 0.05361 =
0.07751 0.00743 0.00688 -0.00075
AFIX 43
H48 2 0.443168 0.126155 0.351362 11.00000 -1.20000
AFIX 0
C3 1 0.613614 0.223055 0.419229 11.00000 0.07095 0.04883 =
0.07199 0.00911 0.00904 0.00150
AFIX 43
H3B 2 0.587263 0.186151 0.414688 11.00000 -1.20000
AFIX 0
C100 1 0.908413 0.306995 0.662051 11.00000 0.06632 0.05084 =
0.08731 -0.01238 0.00085 -0.00723
AFIX 43
H100 2 0.918001 0.356008 0.665755 11.00000 -1.20000
AFIX 0
C61 1 0.703252 0.202550 0.215684 11.00000 0.06292 0.05185 =
0.06185 -0.00676 0.00806 0.01357
AFIX 43
H61 2 0.713757 0.183045 0.187543 11.00000 -1.20000
AFIX 0
C92 1 0.915820 0.212885 0.443660 11.00000 0.06952 0.05929 =
0.07351 0.00334 0.01021 -0.00577
AFIX 43
H92 2 0.901998 0.188961 0.413660 11.00000 -1.20000
AFIX 0
C126 1 0.790453 -0.306127 0.729698 11.00000 0.06512 0.06307 =
0.08153 0.01184 0.00357 -0.00785
AFIX 43
H126 2 0.772821 -0.351108 0.728142 11.00000 -1.20000
AFIX 0
C127 1 0.812174 -0.284266 0.689337 11.00000 0.06492 0.06240 =
0.07901 0.01015 0.00330 -0.00651
AFIX 43
H127 2 0.809676 -0.313772 0.661227 11.00000 -1.20000
AFIX 0
C69 1 0.844162 -0.264061 0.552291 11.00000 0.05611 0.04757 =
0.07759 -0.01256 0.00144 -0.00587
AFIX 43
H69 2 0.837499 -0.312933 0.544174 11.00000 -1.20000
AFIX 0
C71 1 0.744460 -0.232783 0.531295 11.00000 0.05493 0.04619 =
0.07644 -0.01144 0.00295 -0.00805
AFIX 43
H71 2 0.734309 -0.280601 0.522544 11.00000 -1.20000
AFIX 0
C7 1 0.760598 0.255050 0.475080 11.00000 0.06825 0.05055 =
0.07239 0.00693 0.01057 0.00417
AFIX 43
H7 2 0.773115 0.209026 0.486404 11.00000 -1.20000
AFIX 0
C128 1 0.837891 -0.216741 0.692084 11.00000 0.06147 0.05863 =
0.07639 0.00683 0.00357 -0.00551
AFIX 43
H128 2 0.852298 -0.200407 0.665082 11.00000 -1.20000
AFIX 0
C103 1 1.004691 0.267648 0.695130 11.00000 0.06439 0.05089 =
0.08683 -0.01046 0.00265 -0.00920
AFIX 43
H103 2 1.016873 0.315369 0.701354 11.00000 -1.20000
AFIX 0
C112 1 1.036429 -0.237430 0.692369 11.00000 0.07737 0.06573 =
0.10529 0.00400 -0.00117 0.00466
AFIX 43
H112 2 0.998475 -0.233141 0.680876 11.00000 -1.20000
AFIX 0
C63 1 0.702114 0.195460 0.301339 11.00000 0.06368 0.05087 =
0.06056 -0.00383 0.00759 0.01370
AFIX 43
H63 2 0.711330 0.171168 0.331835 11.00000 -1.20000
AFIX 0
C104 1 1.040375 0.212677 0.705367 11.00000 0.06347 0.05246 =
0.08695 -0.01070 0.00328 -0.00967
AFIX 43
H104 2 1.077211 0.222711 0.719144 11.00000 -1.20000
AFIX 0
C68 1 0.897172 -0.239806 0.568577 11.00000 0.05671 0.05074 =
0.07910 -0.01251 0.00139 -0.00378
AFIX 43
H68 2 0.926031 -0.273030 0.571093 11.00000 -1.20000
AFIX 0
C125 1 0.793456 -0.266781 0.769889 11.00000 0.06446 0.06528 =
0.08041 0.01345 0.00552 -0.00643
AFIX 43
H125 2 0.778462 -0.283827 0.796370 11.00000 -1.20000
AFIX 0
C94 1 0.967553 0.310813 0.486735 11.00000 0.07030 0.06113 =
0.07684 0.00482 0.00981 -0.00876
AFIX 43
H94 2 0.988026 0.353258 0.486272 11.00000 -1.20000
AFIX 0
C47 1 0.369307 0.171258 0.351228 11.00000 0.08118 0.05527 =
0.07904 0.00810 0.00678 -0.00332
AFIX 43
H47 2 0.352872 0.128995 0.360135 11.00000 -1.20000
AFIX 0
C8 1 0.796081 0.310043 0.483181 11.00000 0.06785 0.05328 =
0.07428 0.00718 0.00926 0.00280
AFIX 43
H8A 2 0.831976 0.302833 0.500961 11.00000 -1.20000
AFIX 0
C46 1 0.339006 0.233128 0.342311 11.00000 0.07847 0.05612 =
0.07797 0.00782 0.00787 -0.00235
AFIX 43
H46 2 0.301673 0.232644 0.343538 11.00000 -1.20000
AFIX 0
C77 1 0.604587 0.201826 0.566747 11.00000 0.07311 0.05311 =
0.08157 -0.00029 0.00391 0.00289
AFIX 43
H77 2 0.583945 0.159164 0.560937 11.00000 -1.20000
AFIX 0
C80 1 0.663631 0.327909 0.579680 11.00000 0.07503 0.05256 =
0.08194 -0.00084 0.00478 0.00148
AFIX 43
H80 2 0.683561 0.371259 0.583528 11.00000 -1.20000
AFIX 0
C111 1 1.059069 -0.305133 0.702148 11.00000 0.07942 0.06637 =
0.10652 0.00339 -0.00121 0.00437
AFIX 43
H111 2 1.036330 -0.346003 0.697598 11.00000 -1.20000
AFIX 0
C93 1 0.949182 0.275860 0.443958 11.00000 0.07085 0.06166 =
0.07537 0.00533 0.01216 -0.00755
AFIX 43
H93 2 0.958127 0.292556 0.414390 11.00000 -1.20000
AFIX 0
C117 1 0.995210 -0.003191 0.925704 11.00000 0.08099 0.07280 =
0.07078 -0.00161 0.00014 0.00458
AFIX 43
H117 2 0.984156 -0.014224 0.955485 11.00000 -1.20000
AFIX 0
C99 1 0.854850 0.286736 0.643976 11.00000 0.06566 0.05055 =
0.08492 -0.01062 0.00092 -0.00362
AFIX 43
H99 2 0.827656 0.322451 0.637072 11.00000 -1.20000
AFIX 0
C79 1 0.608866 0.328688 0.580497 11.00000 0.07627 0.05343 =
0.08399 -0.00169 0.00343 0.00444
AFIX 43
H79 2 0.591624 0.372493 0.585126 11.00000 -1.20000
AFIX 0
C133 1 0.768500 0.420949 0.333567 11.00000 0.06898 0.06421 =
0.07731 -0.00376 0.01694 0.00927
AFIX 23
H13I 2 0.782299 0.386728 0.360306 11.00000 -1.20000
H13J 2 0.758093 0.394193 0.302389 11.00000 -1.20000
AFIX 0
C108 1 1.125335 -0.184838 0.712235 11.00000 0.07801 0.06609 =
0.10730 0.00345 -0.00233 0.00452
AFIX 43
H108 2 1.148809 -0.144877 0.713972 11.00000 -1.20000
AFIX 0
C16 1 0.807110 0.815807 0.407129 11.00000 0.07184 0.06540 =
0.11023 0.01280 -0.00120 -0.00592
AFIX 43
H16 2 0.784551 0.856849 0.402536 11.00000 -1.20000
AFIX 0
C131 1 1.012329 0.063850 0.570409 11.00000 0.06763 0.06628 =
0.09114 -0.00187 0.01288 -0.00786
AFIX 23
H13A 2 0.999940 0.087373 0.538224 11.00000 -1.20000
H13B 2 1.031039 0.100046 0.593774 11.00000 -1.20000
AFIX 0
C78 1 0.578688 0.264984 0.574509 11.00000 0.07348 0.05556 =
0.08339 -0.00128 0.00471 0.00319
AFIX 43
H78 2 0.541358 0.265154 0.575749 11.00000 -1.20000
AFIX 0
C110 1 1.113642 -0.313324 0.718214 11.00000 0.08231 0.06726 =
0.10887 0.00526 -0.00242 0.00629
AFIX 43
H110 2 1.128567 -0.359389 0.726208 11.00000 -1.20000
AFIX 0
C132 1 1.048951 0.007863 0.565584 11.00000 0.10123 0.10894 =
0.13341 -0.01903 0.01951 0.02476
AFIX 137
H13C 2 1.066498 0.018233 0.538012 11.00000 -1.50000
H13D 2 1.029099 -0.037312 0.559557 11.00000 -1.50000
H13E 2 1.076502 0.004073 0.595856 11.00000 -1.50000
AFIX 0
C134 1 0.808657 0.473546 0.329955 11.00000 0.11595 0.11444 =
0.10926 -0.02115 0.03541 -0.02212
AFIX 137
H13K 2 0.821751 0.466304 0.299485 11.00000 -1.50000
H13L 2 0.838956 0.469037 0.358052 11.00000 -1.50000
H13M 2 0.792764 0.521316 0.329854 11.00000 -1.50000
AFIX 0
C109 1 1.146799 -0.254251 0.722712 11.00000 0.07942 0.06868 =
0.10908 0.00333 -0.00230 0.00524
AFIX 43
H109 2 1.184780 -0.260197 0.733038 11.00000 -1.20000
AFIX 0
C15 1 0.862460 0.821373 0.406412 11.00000 0.07425 0.06892 =
0.11351 0.01458 -0.00105 -0.00767
AFIX 43
H15 2 0.876744 0.865419 0.397871 11.00000 -1.20000
AFIX 0
C14 1 0.896699 0.762357 0.418218 11.00000 0.07190 0.06850 =
0.11168 0.01274 -0.00090 -0.00673
AFIX 43
H14 2 0.934359 0.767197 0.419177 11.00000 -1.20000
AFIX 0
C13 1 0.875564 0.695888 0.428673 11.00000 0.07037 0.06637 =
0.10911 0.01280 -0.00041 -0.00653
AFIX 43
H13N 2 0.898928 0.656299 0.437878 11.00000 -1.20000
AFIX 0
C130 1 0.716366 -0.008842 0.703195 11.00000 0.12007 0.12709 =
0.13824 -0.01686 0.02464 -0.00682
AFIX 137
H13F 2 0.685289 -0.022637 0.677659 11.00000 -1.50000
H13G 2 0.703621 0.017022 0.729295 11.00000 -1.50000
H13H 2 0.736035 -0.051755 0.716887 11.00000 -1.50000
AFIX 0
C129 1 0.751253 0.035713 0.682602 11.00000 0.09711 0.07341 =
0.08692 -0.00428 0.02251 0.00444
AFIX 23
H12A 2 0.779929 0.055365 0.708927 11.00000 -1.20000
H12B 2 0.730527 0.076124 0.665071 11.00000 -1.20000
AFIX 0
C135 1 0.492338 0.474659 0.431691 11.00000 0.10745 0.09061 =
0.08475 0.00722 0.02531 0.00033
AFIX 23
H13P 2 0.474559 0.509737 0.449864 11.00000 -1.20000
H13Q 2 0.464353 0.445161 0.410577 11.00000 -1.20000
AFIX 0
C136 1 0.529939 0.431889 0.463939 11.00000 0.12133 0.10268 =
0.10890 0.00608 0.01820 0.01805
AFIX 33
H13O 2 0.511022 0.404969 0.485557 11.00000 -1.50000
H13R 2 0.547366 0.398550 0.444840 11.00000 -1.50000
H13S 2 0.557477 0.462520 0.483760 11.00000 -1.50000
AFIX 0
HKLF 4
REM yzf-232-1_a.res in P2(1)/c
REM R1 = 0.0733 for 15417 Fo > 4sig(Fo) and 0.1431 for all 28333 data
REM 1564 parameters refined using 2706 restraints
END
WGHT 0.0608 59.6954
REM Highest difference peak 2.228, deepest hole -1.573, 1-sigma level 0.163
Q1 1 0.9380 0.0790 0.6610 11.00000 0.05 2.23
Q2 1 0.5582 0.5580 0.3228 11.00000 0.05 1.68
Q3 1 0.6982 0.4204 0.4216 11.00000 0.05 1.65
Q4 1 0.4219 0.5021 0.2351 11.00000 0.05 1.53
Q5 1 0.8007 -0.0399 0.5687 11.00000 0.05 1.41
Q6 1 1.0775 0.0393 0.7607 11.00000 0.05 1.35
Q7 1 0.6628 -0.0054 0.4778 11.00000 0.05 1.34
Q8 1 0.8193 0.0027 0.5885 11.00000 0.05 1.31
Q9 1 0.4200 0.4201 0.2356 11.00000 0.05 1.30
Q10 1 1.0736 -0.0435 0.7577 11.00000 0.05 1.18
Q11 1 0.7822 0.0390 0.5175 11.00000 0.05 1.18
Q12 1 0.9563 -0.0386 0.6818 11.00000 0.05 1.14
Q13 1 0.8206 0.5579 0.5042 11.00000 0.05 1.14
Q14 1 0.6632 0.0811 0.4775 11.00000 0.05 1.14
Q15 1 0.4997 0.4606 0.2999 11.00000 0.05 1.10
Q16 1 0.5607 0.4619 0.3545 11.00000 0.05 1.10
Q17 1 0.5410 0.4609 0.2784 11.00000 0.05 1.08
Q18 1 0.8192 0.4657 0.5011 11.00000 0.05 1.06
Q19 1 0.7185 0.5142 0.4796 11.00000 0.05 1.04
Q20 1 0.5360 0.4811 0.4446 11.00000 0.05 0.98
Q21 1 0.6805 0.5139 0.3807 11.00000 0.05 0.96
Q22 1 0.9218 -0.0023 0.6168 11.00000 0.05 0.95
Q23 1 0.7795 -0.0002 0.5426 11.00000 0.05 0.89
Q24 1 0.8194 0.0390 0.6214 11.00000 0.05 0.88
Q25 1 0.6412 0.5457 0.3770 11.00000 0.05 0.87
Q26 1 0.7006 0.5093 0.4614 11.00000 0.05 0.86
Q27 1 0.5360 0.5045 0.2991 11.00000 0.05 0.84
Q28 1 0.7409 0.5066 0.4387 11.00000 0.05 0.83
Q29 1 0.9589 -0.0005 0.7206 11.00000 0.05 0.82
Q30 1 0.5998 0.4607 0.3377 11.00000 0.05 0.82
;
_shelx_res_checksum 99724
#######################################################################
#
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1888737'
_audit_update_record
;
2019-01-30 deposited with the CCDC. 2019-03-06 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 'C38 H30 Cl4 Dy2 N8 O4'
_chemical_formula_weight 1129.50
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'
O O 0.0106 0.0060 '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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_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, -y, -z'
_cell_length_a 9.0284(6)
_cell_length_b 10.4527(7)
_cell_length_c 11.2508(7)
_cell_angle_alpha 99.014(5)
_cell_angle_beta 104.323(5)
_cell_angle_gamma 98.006(5)
_cell_volume 998.31(11)
_cell_formula_units_Z 1
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 4155
_cell_measurement_theta_min 3.0262
_cell_measurement_theta_max 28.9618
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.879
_exptl_crystal_F_000 546
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.12
_exptl_absorpt_coefficient_mu 4.032
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.64832
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using
spherical harmonics,
implemented in SCALE3 ABSPACK
scaling algorithm.
;
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Xcalibur, Eos'
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 7869
_diffrn_reflns_av_unetI/netI 0.0598
_diffrn_reflns_av_R_equivalents 0.0444
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_theta_min 3.032
_diffrn_reflns_theta_max 29.026
_diffrn_reflns_theta_full 26.000
_diffrn_measured_fraction_theta_max 0.835
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.835
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total 4464
_reflns_number_gt 3897
_reflns_threshold_expression 'I > 2\s(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 'CrysAlis PRO (Agilent, 2011)'
_computing_cell_refinement 'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction 'CrysAlis PRO (Agilent, 2011)'
_computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker 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/[\s^2^(Fo^2^)+(0.0215P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 4464
_refine_ls_number_parameters 254
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0415
_refine_ls_R_factor_gt 0.0330
_refine_ls_wR_factor_ref 0.0698
_refine_ls_wR_factor_gt 0.0650
_refine_ls_goodness_of_fit_ref 1.027
_refine_ls_restrained_S_all 1.027
_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
Dy1 Dy 0.43688(2) 0.42292(2) 0.32941(2) 0.02948(8) Uani 1 1 d . . . . .
Cl1 Cl 0.52381(16) 0.20042(12) 0.35442(12) 0.0522(3) Uani 1 1 d . . . . .
O1 O 0.1909(4) 0.3053(3) 0.2025(3) 0.0469(9) Uani 1 1 d . . . . .
C16 C -0.2558(6) 0.0958(5) 0.0305(5) 0.0552(14) Uani 1 1 d . . . . .
H16 H -0.3258 0.0806 0.0773 0.066 Uiso 1 1 calc R U . . .
C7 C 0.9328(5) 0.5428(4) 0.1849(4) 0.0388(11) Uani 1 1 d . . . . .
H7 H 1.0226 0.5639 0.1600 0.047 Uiso 1 1 calc R U . . .
N1 N 0.6660(4) 0.4739(3) 0.2570(3) 0.0280(8) Uani 1 1 d . . . . .
N3 N 0.2706(4) 0.2648(3) 0.0306(3) 0.0360(9) Uani 1 1 d . . . . .
H3 H 0.2537 0.2303 -0.0472 0.043 Uiso 1 1 calc R U . . .
C6 C 0.9331(5) 0.5902(4) 0.3102(4) 0.0338(10) Uani 1 1 d . . . . .
N2 N 0.4135(4) 0.3346(3) 0.1021(3) 0.0312(8) Uani 1 1 d . . . . .
C5 C 0.7931(5) 0.5511(4) 0.3422(4) 0.0276(9) Uani 1 1 d . . . . .
C3 C 1.0459(5) 0.7079(5) 0.5176(4) 0.0492(14) Uani 1 1 d . . . . .
H3A H 1.1307 0.7611 0.5782 0.059 Uiso 1 1 calc R U . . .
C4 C 1.0604(5) 0.6700(5) 0.4024(4) 0.0435(12) Uani 1 1 d . . . . .
H4 H 1.1534 0.6962 0.3838 0.052 Uiso 1 1 calc R U . . .
C11 C 0.1582(5) 0.2537(4) 0.0905(4) 0.0339(10) Uani 1 1 d . . . . .
C9 C 0.6712(5) 0.4333(4) 0.1400(4) 0.0328(10) Uani 1 1 d . . . . .
C12 C 0.0014(5) 0.1817(4) 0.0206(4) 0.0354(10) Uani 1 1 d . . . . .
C1 C 0.7807(5) 0.5907(4) 0.4650(4) 0.0313(10) Uani 1 1 d . . . . .
C8 C 0.8045(5) 0.4676(5) 0.1011(4) 0.0389(11) Uani 1 1 d . . . . .
H8 H 0.8046 0.4390 0.0186 0.047 Uiso 1 1 calc R U . . .
C2 C 0.9094(5) 0.6711(5) 0.5510(4) 0.0476(13) Uani 1 1 d . . . . .
H2 H 0.9050 0.7011 0.6321 0.057 Uiso 1 1 calc R U . . .
C17 C -0.1047(6) 0.1596(5) 0.0895(5) 0.0491(13) Uani 1 1 d . . . . .
H17 H -0.0736 0.1881 0.1760 0.059 Uiso 1 1 calc R U . . .
C13 C -0.0468(6) 0.1406(5) -0.1061(4) 0.0498(13) Uani 1 1 d . . . . .
H13 H 0.0226 0.1557 -0.1534 0.060 Uiso 1 1 calc R U . . .
C15 C -0.3023(6) 0.0553(5) -0.0963(5) 0.0579(15) Uani 1 1 d . . . . .
H15 H -0.4044 0.0132 -0.1363 0.070 Uiso 1 1 calc R U . . .
C10 C 0.5273(5) 0.3562(4) 0.0551(4) 0.0335(10) Uani 1 1 d . . . . .
H10 H 0.5185 0.3243 -0.0287 0.040 Uiso 1 1 calc R U . . .
O2 O 0.6462(3) 0.5494(3) 0.4910(2) 0.0325(7) Uani 1 1 d . . . . .
C14 C -0.1981(6) 0.0766(6) -0.1650(5) 0.0634(17) Uani 1 1 d . . . . .
H14 H -0.2295 0.0479 -0.2515 0.076 Uiso 1 1 calc R U . . .
Cl2 Cl 0.36240(14) 0.62830(12) 0.24025(11) 0.0443(3) Uani 1 1 d . . . . .
N4 N 0.2762(6) 0.1490(5) -0.2214(4) 0.0748(16) Uani 1 1 d . . . . .
C18 C 0.2960(7) 0.1186(5) -0.3143(5) 0.0593(15) Uani 1 1 d . . . . .
C19 C 0.3266(9) 0.0845(6) -0.4338(6) 0.093(2) Uani 1 1 d . . . . .
H19A H 0.2492 0.1088 -0.4972 0.140 Uiso 1 1 calc R U . . .
H19B H 0.3233 -0.0088 -0.4534 0.140 Uiso 1 1 calc R U . . .
H19C H 0.4276 0.1306 -0.4304 0.140 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.02401(12) 0.03886(13) 0.02375(11) 0.00452(9) 0.00894(8) -0.00253(9)
Cl1 0.0557(8) 0.0431(7) 0.0548(7) 0.0136(6) 0.0094(6) 0.0058(6)
O1 0.036(2) 0.067(2) 0.0280(16) -0.0037(16) 0.0114(14) -0.0129(17)
C16 0.038(3) 0.054(3) 0.069(4) 0.013(3) 0.014(3) -0.005(3)
C7 0.034(3) 0.048(3) 0.043(2) 0.014(2) 0.023(2) 0.008(2)
N1 0.0282(19) 0.0309(18) 0.0274(17) 0.0085(15) 0.0115(15) 0.0039(15)
N3 0.036(2) 0.037(2) 0.0267(17) 0.0000(16) 0.0033(16) -0.0036(17)
C6 0.030(2) 0.040(2) 0.038(2) 0.014(2) 0.0178(19) 0.0038(19)
N2 0.026(2) 0.042(2) 0.0252(17) 0.0082(16) 0.0074(15) 0.0029(16)
C5 0.021(2) 0.031(2) 0.033(2) 0.0104(18) 0.0104(17) 0.0036(17)
C3 0.029(3) 0.062(3) 0.046(3) -0.003(3) 0.011(2) -0.015(2)
C4 0.025(3) 0.057(3) 0.047(3) 0.013(2) 0.013(2) -0.006(2)
C11 0.032(3) 0.035(2) 0.035(2) 0.007(2) 0.0112(19) 0.0024(19)
C9 0.030(2) 0.042(3) 0.031(2) 0.012(2) 0.0121(18) 0.0076(19)
C12 0.031(3) 0.031(2) 0.039(2) 0.005(2) 0.0048(19) 0.0002(19)
C1 0.027(2) 0.037(2) 0.033(2) 0.011(2) 0.0139(18) 0.0019(19)
C8 0.033(3) 0.056(3) 0.032(2) 0.009(2) 0.017(2) 0.006(2)
C2 0.034(3) 0.066(3) 0.035(2) 0.001(2) 0.010(2) -0.011(2)
C17 0.037(3) 0.054(3) 0.045(3) 0.000(2) 0.007(2) -0.008(2)
C13 0.042(3) 0.056(3) 0.045(3) 0.004(3) 0.008(2) 0.002(3)
C15 0.031(3) 0.052(3) 0.075(4) 0.003(3) 0.000(3) -0.007(2)
C10 0.034(3) 0.040(2) 0.027(2) 0.0049(19) 0.0110(18) 0.005(2)
O2 0.0267(16) 0.0440(18) 0.0258(14) 0.0051(13) 0.0122(12) -0.0035(13)
C14 0.047(4) 0.073(4) 0.049(3) 0.000(3) -0.007(3) -0.006(3)
Cl2 0.0470(7) 0.0518(7) 0.0421(6) 0.0164(6) 0.0198(5) 0.0144(6)
N4 0.075(4) 0.093(4) 0.056(3) 0.001(3) 0.031(3) 0.005(3)
C18 0.078(4) 0.057(3) 0.051(3) 0.014(3) 0.028(3) 0.016(3)
C19 0.166(8) 0.081(5) 0.068(4) 0.032(4) 0.067(5) 0.056(5)
_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 O2 2.315(3) 2_666 ?
Dy1 O2 2.340(3) . ?
Dy1 O1 2.367(3) . ?
Dy1 N1 2.427(3) . ?
Dy1 N2 2.525(3) . ?
Dy1 Cl1 2.5901(13) . ?
Dy1 Cl2 2.6096(12) . ?
Dy1 Dy1 3.7438(4) 2_666 ?
O1 C11 1.235(5) . ?
C16 C15 1.362(7) . ?
C16 C17 1.381(6) . ?
C16 H16 0.9300 . ?
C7 C8 1.350(6) . ?
C7 C6 1.419(6) . ?
C7 H7 0.9300 . ?
N1 C9 1.333(5) . ?
N1 C5 1.357(5) . ?
N3 C11 1.351(5) . ?
N3 N2 1.373(4) . ?
N3 H3 0.8600 . ?
C6 C4 1.401(6) . ?
C6 C5 1.422(5) . ?
N2 C10 1.276(5) . ?
C5 C1 1.415(6) . ?
C3 C4 1.339(6) . ?
C3 C2 1.397(6) . ?
C3 H3A 0.9300 . ?
C4 H4 0.9300 . ?
C11 C12 1.468(6) . ?
C9 C8 1.399(6) . ?
C9 C10 1.450(6) . ?
C12 C13 1.363(6) . ?
C12 C17 1.391(6) . ?
C1 O2 1.347(4) . ?
C1 C2 1.382(6) . ?
C8 H8 0.9300 . ?
C2 H2 0.9300 . ?
C17 H17 0.9300 . ?
C13 C14 1.383(6) . ?
C13 H13 0.9300 . ?
C15 C14 1.374(8) . ?
C15 H15 0.9300 . ?
C10 H10 0.9300 . ?
O2 Dy1 2.315(3) 2_666 ?
C14 H14 0.9300 . ?
N4 C18 1.108(7) . ?
C18 C19 1.440(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O2 72.91(10) 2_666 . ?
O2 Dy1 O1 93.31(10) 2_666 . ?
O2 Dy1 O1 165.98(10) . . ?
O2 Dy1 N1 141.38(10) 2_666 . ?
O2 Dy1 N1 68.52(10) . . ?
O1 Dy1 N1 125.32(10) . . ?
O2 Dy1 N2 155.68(10) 2_666 . ?
O2 Dy1 N2 131.34(10) . . ?
O1 Dy1 N2 62.55(10) . . ?
N1 Dy1 N2 62.82(10) . . ?
O2 Dy1 Cl1 95.59(8) 2_666 . ?
O2 Dy1 Cl1 94.67(8) . . ?
O1 Dy1 Cl1 89.10(9) . . ?
N1 Dy1 Cl1 85.80(8) . . ?
N2 Dy1 Cl1 81.96(9) . . ?
O2 Dy1 Cl2 100.83(8) 2_666 . ?
O2 Dy1 Cl2 93.09(8) . . ?
O1 Dy1 Cl2 86.91(9) . . ?
N1 Dy1 Cl2 83.31(8) . . ?
N2 Dy1 Cl2 81.81(8) . . ?
Cl1 Dy1 Cl2 163.30(4) . . ?
O2 Dy1 Dy1 36.68(6) 2_666 2_666 ?
O2 Dy1 Dy1 36.23(6) . 2_666 ?
O1 Dy1 Dy1 129.94(7) . 2_666 ?
N1 Dy1 Dy1 104.73(8) . 2_666 ?
N2 Dy1 Dy1 167.48(8) . 2_666 ?
Cl1 Dy1 Dy1 96.37(3) . 2_666 ?
Cl2 Dy1 Dy1 98.62(3) . 2_666 ?
C11 O1 Dy1 126.6(3) . . ?
C15 C16 C17 120.0(5) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C8 C7 C6 121.1(4) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C9 N1 C5 119.7(3) . . ?
C9 N1 Dy1 123.8(3) . . ?
C5 N1 Dy1 116.5(2) . . ?
C11 N3 N2 115.7(3) . . ?
C11 N3 H3 122.2 . . ?
N2 N3 H3 122.2 . . ?
C4 C6 C7 124.7(4) . . ?
C4 C6 C5 119.0(4) . . ?
C7 C6 C5 116.3(4) . . ?
C10 N2 N3 121.6(3) . . ?
C10 N2 Dy1 121.9(3) . . ?
N3 N2 Dy1 116.5(2) . . ?
N1 C5 C1 117.1(3) . . ?
N1 C5 C6 121.7(4) . . ?
C1 C5 C6 121.2(4) . . ?
C4 C3 C2 123.0(4) . . ?
C4 C3 H3A 118.5 . . ?
C2 C3 H3A 118.5 . . ?
C3 C4 C6 118.9(4) . . ?
C3 C4 H4 120.5 . . ?
C6 C4 H4 120.5 . . ?
O1 C11 N3 118.7(4) . . ?
O1 C11 C12 122.1(4) . . ?
N3 C11 C12 119.2(4) . . ?
N1 C9 C8 122.1(4) . . ?
N1 C9 C10 115.2(4) . . ?
C8 C9 C10 122.6(4) . . ?
C13 C12 C17 118.9(4) . . ?
C13 C12 C11 124.2(4) . . ?
C17 C12 C11 116.9(4) . . ?
O2 C1 C2 124.2(4) . . ?
O2 C1 C5 118.9(4) . . ?
C2 C1 C5 116.9(4) . . ?
C7 C8 C9 119.2(4) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C1 C2 C3 120.8(4) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C16 C17 C12 120.5(5) . . ?
C16 C17 H17 119.8 . . ?
C12 C17 H17 119.7 . . ?
C12 C13 C14 120.5(5) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C16 C15 C14 119.9(5) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
N2 C10 C9 116.2(4) . . ?
N2 C10 H10 121.9 . . ?
C9 C10 H10 121.9 . . ?
C1 O2 Dy1 134.0(2) . 2_666 ?
C1 O2 Dy1 118.9(2) . . ?
Dy1 O2 Dy1 107.09(10) 2_666 . ?
C15 C14 C13 120.3(5) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
N4 C18 C19 177.4(7) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 C7 C6 C4 -179.1(5) . . . . ?
C8 C7 C6 C5 1.6(7) . . . . ?
C11 N3 N2 C10 -177.3(4) . . . . ?
C11 N3 N2 Dy1 1.1(5) . . . . ?
C9 N1 C5 C1 -179.8(4) . . . . ?
Dy1 N1 C5 C1 1.7(5) . . . . ?
C9 N1 C5 C6 -0.1(6) . . . . ?
Dy1 N1 C5 C6 -178.6(3) . . . . ?
C4 C6 C5 N1 180.0(4) . . . . ?
C7 C6 C5 N1 -0.7(6) . . . . ?
C4 C6 C5 C1 -0.3(7) . . . . ?
C7 C6 C5 C1 179.0(4) . . . . ?
C2 C3 C4 C6 0.3(9) . . . . ?
C7 C6 C4 C3 -179.8(5) . . . . ?
C5 C6 C4 C3 -0.5(7) . . . . ?
Dy1 O1 C11 N3 -0.9(6) . . . . ?
Dy1 O1 C11 C12 179.5(3) . . . . ?
N2 N3 C11 O1 -0.3(6) . . . . ?
N2 N3 C11 C12 179.4(4) . . . . ?
C5 N1 C9 C8 0.0(7) . . . . ?
Dy1 N1 C9 C8 178.3(3) . . . . ?
C5 N1 C9 C10 -177.4(4) . . . . ?
Dy1 N1 C9 C10 0.9(5) . . . . ?
O1 C11 C12 C13 169.6(5) . . . . ?
N3 C11 C12 C13 -10.1(7) . . . . ?
O1 C11 C12 C17 -7.8(7) . . . . ?
N3 C11 C12 C17 172.5(4) . . . . ?
N1 C5 C1 O2 0.7(6) . . . . ?
C6 C5 C1 O2 -179.0(4) . . . . ?
N1 C5 C1 C2 -179.0(4) . . . . ?
C6 C5 C1 C2 1.4(7) . . . . ?
C6 C7 C8 C9 -1.7(7) . . . . ?
N1 C9 C8 C7 0.9(7) . . . . ?
C10 C9 C8 C7 178.2(4) . . . . ?
O2 C1 C2 C3 178.8(5) . . . . ?
C5 C1 C2 C3 -1.6(8) . . . . ?
C4 C3 C2 C1 0.8(9) . . . . ?
C15 C16 C17 C12 -0.7(9) . . . . ?
C13 C12 C17 C16 0.7(8) . . . . ?
C11 C12 C17 C16 178.2(5) . . . . ?
C17 C12 C13 C14 -0.8(8) . . . . ?
C11 C12 C13 C14 -178.1(5) . . . . ?
C17 C16 C15 C14 0.7(9) . . . . ?
N3 N2 C10 C9 178.9(4) . . . . ?
Dy1 N2 C10 C9 0.5(5) . . . . ?
N1 C9 C10 N2 -0.9(6) . . . . ?
C8 C9 C10 N2 -178.3(4) . . . . ?
C2 C1 O2 Dy1 -2.3(7) . . . 2_666 ?
C5 C1 O2 Dy1 178.1(3) . . . 2_666 ?
C2 C1 O2 Dy1 176.7(4) . . . . ?
C5 C1 O2 Dy1 -2.9(5) . . . . ?
C16 C15 C14 C13 -0.8(9) . . . . ?
C12 C13 C14 C15 0.9(9) . . . . ?
_refine_diff_density_max 0.987
_refine_diff_density_min -0.644
_refine_diff_density_rms 0.123
_shelx_res_file
;
1.res created by SHELXL-2014/7
TITL CF solution in P-1
CELL 0.71073 9.028434 10.45275 11.250752 99.014 104.3226 98.0057
ZERR 1 0.000556 0.000657 0.000684 0.0052 0.0053 0.0052
LATT 1
SFAC C H O N Dy Cl
UNIT 38 30 4 8 2 4
L.S. 4
PLAN 5
BOND $H
CONF
HTAB
fmap 2
acta 52
REM
REM
REM
WGHT 0.021500
FVAR 3.05824
DY1 5 0.436882 0.422924 0.329406 11.00000 0.02401 0.03886 =
0.02375 0.00452 0.00894 -0.00253
CL1 6 0.523807 0.200419 0.354420 11.00000 0.05569 0.04311 =
0.05479 0.01357 0.00944 0.00583
O1 3 0.190937 0.305278 0.202487 11.00000 0.03591 0.06710 =
0.02797 -0.00371 0.01143 -0.01294
C16 1 -0.255802 0.095830 0.030500 11.00000 0.03814 0.05406 =
0.06903 0.01266 0.01367 -0.00468
AFIX 43
H16 2 -0.325795 0.080568 0.077300 11.00000 -1.20000
AFIX 0
C7 1 0.932828 0.542797 0.184878 11.00000 0.03412 0.04771 =
0.04278 0.01357 0.02294 0.00752
AFIX 43
H7 2 1.022567 0.563882 0.160019 11.00000 -1.20000
AFIX 0
N1 4 0.665993 0.473914 0.256991 11.00000 0.02818 0.03093 =
0.02739 0.00853 0.01147 0.00388
N3 4 0.270632 0.264774 0.030634 11.00000 0.03565 0.03748 =
0.02666 -0.00002 0.00335 -0.00360
AFIX 43
H3 2 0.253720 0.230292 -0.047196 11.00000 -1.20000
AFIX 0
C6 1 0.933062 0.590162 0.310199 11.00000 0.02972 0.03964 =
0.03785 0.01352 0.01776 0.00378
N2 4 0.413523 0.334598 0.102095 11.00000 0.02645 0.04162 =
0.02524 0.00822 0.00740 0.00285
C5 1 0.793085 0.551102 0.342202 11.00000 0.02112 0.03129 =
0.03291 0.01036 0.01041 0.00364
C3 1 1.045903 0.707865 0.517598 11.00000 0.02873 0.06181 =
0.04573 -0.00287 0.01094 -0.01469
AFIX 43
H3A 2 1.130677 0.761119 0.578216 11.00000 -1.20000
AFIX 0
C4 1 1.060369 0.669960 0.402356 11.00000 0.02452 0.05686 =
0.04740 0.01294 0.01291 -0.00643
AFIX 43
H4 2 1.153387 0.696157 0.383757 11.00000 -1.20000
AFIX 0
C11 1 0.158243 0.253717 0.090492 11.00000 0.03153 0.03464 =
0.03545 0.00682 0.01116 0.00236
C9 1 0.671227 0.433270 0.139965 11.00000 0.02955 0.04224 =
0.03072 0.01233 0.01213 0.00759
C12 1 0.001441 0.181684 0.020620 11.00000 0.03097 0.03124 =
0.03890 0.00481 0.00484 0.00019
C1 1 0.780670 0.590742 0.464979 11.00000 0.02725 0.03726 =
0.03258 0.01077 0.01392 0.00187
C8 1 0.804474 0.467620 0.101119 11.00000 0.03281 0.05593 =
0.03194 0.00941 0.01718 0.00557
AFIX 43
H8 2 0.804649 0.439027 0.018613 11.00000 -1.20000
AFIX 0
C2 1 0.909373 0.671116 0.550975 11.00000 0.03363 0.06591 =
0.03452 0.00095 0.01037 -0.01119
AFIX 43
H2 2 0.905021 0.701126 0.632122 11.00000 -1.20000
AFIX 0
C17 1 -0.104669 0.159629 0.089524 11.00000 0.03737 0.05397 =
0.04510 0.00019 0.00677 -0.00834
AFIX 43
H17 2 -0.073617 0.188061 0.176008 11.00000 -1.20000
AFIX 0
C13 1 -0.046788 0.140617 -0.106136 11.00000 0.04192 0.05632 =
0.04490 0.00357 0.00817 0.00248
AFIX 43
H13 2 0.022646 0.155750 -0.153429 11.00000 -1.20000
AFIX 0
C15 1 -0.302332 0.055255 -0.096299 11.00000 0.03137 0.05171 =
0.07476 0.00259 -0.00020 -0.00698
AFIX 43
H15 2 -0.404399 0.013184 -0.136266 11.00000 -1.20000
AFIX 0
C10 1 0.527333 0.356171 0.055136 11.00000 0.03360 0.04040 =
0.02697 0.00487 0.01103 0.00522
AFIX 43
H10 2 0.518509 0.324260 -0.028741 11.00000 -1.20000
AFIX 0
O2 3 0.646189 0.549405 0.490951 11.00000 0.02669 0.04398 =
0.02575 0.00511 0.01218 -0.00347
C14 1 -0.198117 0.076629 -0.165024 11.00000 0.04713 0.07311 =
0.04939 -0.00033 -0.00686 -0.00599
AFIX 43
H14 2 -0.229501 0.047942 -0.251480 11.00000 -1.20000
AFIX 0
CL2 6 0.362403 0.628299 0.240250 11.00000 0.04697 0.05179 =
0.04211 0.01642 0.01981 0.01438
N4 4 0.276222 0.149005 -0.221412 11.00000 0.07493 0.09310 =
0.05553 0.00088 0.03120 0.00490
C18 1 0.295966 0.118591 -0.314255 11.00000 0.07774 0.05697 =
0.05081 0.01391 0.02782 0.01622
C19 1 0.326556 0.084465 -0.433775 11.00000 0.16586 0.08058 =
0.06786 0.03213 0.06729 0.05595
AFIX 137
H19A 2 0.249169 0.108839 -0.497159 11.00000 -1.50000
H19B 2 0.323259 -0.008815 -0.453449 11.00000 -1.50000
H19C 2 0.427639 0.130616 -0.430416 11.00000 -1.50000
AFIX 0
HKLF 4
REM CF solution in P-1
REM R1 = 0.0330 for 3897 Fo > 4sig(Fo) and 0.0415 for all 4464 data
REM 254 parameters refined using 0 restraints
END
WGHT 0.0215 0.0000
REM Instructions for potential hydrogen bonds
HTAB N3 N4
EQIV $1 -x+1, -y+1, -z
HTAB C8 Cl2_$1
EQIV $2 -x+1, -y+1, -z+1
HTAB C2 O1_$2
HTAB C10 Cl2_$1
EQIV $3 -x+1, -y, -z
HTAB C19 Cl1_$3
EQIV $4 x, y, z-1
HTAB C19 Cl1_$4
REM Highest difference peak 0.987, deepest hole -0.644, 1-sigma level 0.123
Q1 1 0.4821 0.3121 0.3302 11.00000 0.05 0.99
Q2 1 0.4025 0.5380 0.3174 11.00000 0.05 0.85
Q3 1 0.5191 0.3925 0.4059 11.00000 0.05 0.83
Q4 1 0.3624 0.4578 0.2517 11.00000 0.05 0.70
Q5 1 0.3625 0.3229 0.2610 11.00000 0.05 0.62
;
_shelx_res_checksum 55842
#######################################################################
#
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1888736'
_audit_update_record
;
2019-01-30 deposited with the CCDC. 2019-03-06 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 'C42 H40 Cl4 Dy2 N12 O4'
_chemical_formula_weight 1243.66
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 2/c'
_space_group_name_Hall '-C 2yc'
_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, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 20.3353(12)
_cell_length_b 15.0093(13)
_cell_length_c 15.7056(9)
_cell_angle_alpha 90
_cell_angle_beta 106.012(6)
_cell_angle_gamma 90
_cell_volume 4607.7(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 3487
_cell_measurement_theta_min 2.9367
_cell_measurement_theta_max 28.8068
_exptl_crystal_description block
_exptl_crystal_colour 'clear red'
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.793
_exptl_crystal_F_000 2432
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.15
_exptl_absorpt_coefficient_mu 3.506
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.84357
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using
spherical harmonics,
implemented in SCALE3 ABSPACK
scaling algorithm.
;
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Xcalibur, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 10707
_diffrn_reflns_av_unetI/netI 0.0821
_diffrn_reflns_av_R_equivalents 0.0557
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 27
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 2.943
_diffrn_reflns_theta_max 28.870
_diffrn_reflns_theta_full 26.000
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total 5231
_reflns_number_gt 3639
_reflns_threshold_expression 'I > 2\s(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 'CrysAlis PRO (Agilent, 2011)'
_computing_cell_refinement 'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction 'CrysAlis PRO (Agilent, 2011)'
_computing_structure_solution 'CrysAlis PRO (Agilent, 2011)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker 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/[\s^2^(Fo^2^)+(0.0434P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 5231
_refine_ls_number_parameters 289
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0820
_refine_ls_R_factor_gt 0.0509
_refine_ls_wR_factor_ref 0.1193
_refine_ls_wR_factor_gt 0.1063
_refine_ls_goodness_of_fit_ref 1.051
_refine_ls_restrained_S_all 1.053
_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
Dy01 Dy 0.56322(2) 0.62848(2) 0.86264(2) 0.03052(12) Uani 1 1 d . . . . .
Cl2 Cl 0.58287(9) 0.45576(13) 0.85625(12) 0.0422(4) Uani 1 1 d . . . . .
Cl1 Cl 0.57270(11) 0.79784(14) 0.89843(14) 0.0538(5) Uani 1 1 d . . . . .
O1 O 0.4480(2) 0.6324(3) 0.7908(3) 0.0316(10) Uani 1 1 d . . . . .
O2 O 0.4549(2) 0.6033(3) 0.4993(3) 0.0402(13) Uani 1 1 d . . . . .
N2 N 0.3316(3) 0.6241(4) 0.5057(4) 0.0334(13) Uani 1 1 d . . . . .
N1 N 0.3265(3) 0.6416(4) 0.6682(3) 0.0324(13) Uani 1 1 d . . . . .
N4 N 0.4230(3) 0.5900(4) 0.3513(4) 0.0523(18) Uani 1 1 d . . . . .
H4A H 0.4646 0.5834 0.3495 0.063 Uiso 1 1 calc R U . . .
H4B H 0.3903 0.5892 0.3030 0.063 Uiso 1 1 calc R U . . .
N3 N 0.3425(3) 0.6111(4) 0.4249(4) 0.0491(17) Uani 1 1 d . . . . .
H3 H 0.3098 0.6091 0.3766 0.059 Uiso 1 1 calc R U . . .
C9 C 0.2666(3) 0.6459(5) 0.6045(5) 0.0408(18) Uani 1 1 d . . . . .
C1 C 0.3907(3) 0.6380(5) 0.8196(5) 0.0353(16) Uani 1 1 d . . . . .
C5 C 0.3262(3) 0.6441(5) 0.7546(5) 0.0364(17) Uani 1 1 d . . . . .
C11 C 0.4097(3) 0.6013(5) 0.4269(5) 0.0372(17) Uani 1 1 d . . . . .
N5 N 0.2395(3) 0.5993(5) 0.2618(5) 0.0553(19) Uani 1 1 d . . . . .
C10 C 0.2720(3) 0.6344(5) 0.5156(5) 0.0438(19) Uani 1 1 d . . . . .
H10 H 0.2334 0.6346 0.4672 0.053 Uiso 1 1 calc R U . . .
C2 C 0.3900(4) 0.6364(5) 0.9059(5) 0.048(2) Uani 1 1 d . . . . .
H2 H 0.4311 0.6297 0.9497 0.058 Uiso 1 1 calc R U . . .
C6 C 0.2641(4) 0.6527(5) 0.7791(5) 0.0445(19) Uani 1 1 d . . . . .
C3 C 0.3301(4) 0.6445(6) 0.9307(5) 0.061(3) Uani 1 1 d . . . . .
H3A H 0.3325 0.6436 0.9907 0.073 Uiso 1 1 calc R U . . .
C4 C 0.2670(4) 0.6538(7) 0.8700(5) 0.060(3) Uani 1 1 d . . . . .
H4 H 0.2276 0.6605 0.8883 0.072 Uiso 1 1 calc R U . . .
N6 N -0.0046(6) 0.6781(8) 0.9012(7) 0.110(4) Uani 1 1 d . . . . .
H6 H -0.0304 0.7156 0.9182 0.132 Uiso 1 1 calc R U . . .
C8 C 0.2038(4) 0.6577(7) 0.6244(5) 0.064(3) Uani 1 1 d . . . . .
H8 H 0.1633 0.6628 0.5793 0.077 Uiso 1 1 calc R U . . .
C7 C 0.2033(4) 0.6616(7) 0.7100(5) 0.061(3) Uani 1 1 d . . . . .
H7 H 0.1621 0.6704 0.7237 0.073 Uiso 1 1 calc DR U . . .
C17 C 0.0484(6) 0.7064(8) 0.8696(8) 0.095(4) Uani 1 1 d . . . . .
H17 H 0.0536 0.7674 0.8635 0.114 Uiso 1 1 calc R U . . .
C16 C 0.1764(5) 0.6200(7) 0.2590(7) 0.070(3) Uani 1 1 d . . . . .
H16 H 0.1669 0.6289 0.3130 0.085 Uiso 1 1 calc R U . . .
C18 C 0.0893(7) 0.6567(11) 0.8489(9) 0.096(5) Uani 1 1 d . . . . .
H18 H 0.1268 0.6805 0.8338 0.115 Uiso 1 1 calc DR U . . .
C15 C 0.1238(5) 0.6296(7) 0.1856(8) 0.082(3) Uani 1 1 d . . . . .
H15 H 0.0803 0.6445 0.1893 0.098 Uiso 1 1 calc R U . . .
C21 C -0.0147(6) 0.5908(9) 0.9047(8) 0.091(4) Uani 1 1 d . . . . .
H21 H -0.0507 0.5678 0.9238 0.109 Uiso 1 1 calc R U . . .
C20 C 0.0300(8) 0.5370(7) 0.8790(10) 0.116(5) Uani 1 1 d . . . . .
H20 H 0.0269 0.4753 0.8817 0.140 Uiso 1 1 calc R U . . .
C14 C 0.1360(6) 0.6174(8) 0.1088(8) 0.101(4) Uani 1 1 d . . . . .
H14 H 0.1010 0.6248 0.0569 0.121 Uiso 1 1 calc R U . . .
C13 C 0.2000(6) 0.5937(9) 0.1046(7) 0.101(4) Uani 1 1 d . . . . .
H13 H 0.2094 0.5840 0.0507 0.121 Uiso 1 1 calc R U . . .
C12 C 0.2502(5) 0.5849(8) 0.1842(7) 0.088(4) Uani 1 1 d . . . . .
H12 H 0.2938 0.5680 0.1826 0.105 Uiso 1 1 calc R U . . .
C19 C 0.0812(8) 0.5783(15) 0.8481(10) 0.131(7) Uani 1 1 d . . . . .
H19 H 0.1100 0.5425 0.8260 0.157 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy01 0.02265(17) 0.0458(2) 0.02120(17) -0.00056(16) 0.00285(11) -0.00096(17)
Cl2 0.0428(10) 0.0467(11) 0.0380(11) 0.0034(9) 0.0127(8) 0.0027(9)
Cl1 0.0594(12) 0.0494(12) 0.0528(13) -0.0058(11) 0.0155(10) -0.0012(11)
O1 0.025(2) 0.047(3) 0.022(2) -0.001(2) 0.0047(18) -0.001(2)
O2 0.028(2) 0.068(4) 0.026(3) -0.007(2) 0.010(2) 0.003(3)
N2 0.031(3) 0.044(3) 0.025(3) 0.001(3) 0.006(2) 0.004(3)
N1 0.025(3) 0.050(4) 0.019(3) 0.002(3) 0.000(2) 0.001(3)
N4 0.045(4) 0.085(5) 0.027(4) -0.007(4) 0.009(3) 0.007(4)
N3 0.041(3) 0.081(5) 0.024(3) -0.005(3) 0.007(3) -0.009(4)
C9 0.025(3) 0.065(5) 0.031(4) 0.002(4) 0.006(3) 0.001(4)
C1 0.033(3) 0.045(4) 0.029(4) 0.001(3) 0.010(3) 0.002(4)
C5 0.026(3) 0.050(5) 0.036(4) 0.001(3) 0.013(3) 0.001(3)
C11 0.034(4) 0.045(4) 0.032(4) 0.001(3) 0.008(3) 0.002(3)
N5 0.046(4) 0.073(5) 0.041(4) -0.001(4) 0.001(3) 0.013(4)
C10 0.024(3) 0.078(6) 0.023(4) 0.012(4) -0.004(3) 0.000(4)
C2 0.032(4) 0.083(6) 0.027(4) 0.008(4) 0.005(3) 0.006(4)
C6 0.034(4) 0.067(5) 0.032(4) 0.008(4) 0.007(3) 0.004(4)
C3 0.038(4) 0.112(8) 0.033(5) 0.007(5) 0.012(3) 0.009(5)
C4 0.036(4) 0.114(8) 0.035(5) 0.008(5) 0.018(3) 0.007(5)
N6 0.107(8) 0.113(9) 0.113(9) 0.011(7) 0.036(7) 0.052(8)
C8 0.021(3) 0.133(9) 0.036(5) 0.013(5) 0.002(3) 0.010(5)
C7 0.027(4) 0.119(8) 0.037(5) 0.011(5) 0.009(3) 0.014(5)
C17 0.079(8) 0.081(9) 0.119(11) 0.036(8) 0.017(8) -0.023(7)
C16 0.053(5) 0.091(8) 0.066(7) -0.005(6) 0.016(5) 0.002(6)
C18 0.062(8) 0.122(12) 0.126(12) -0.013(10) 0.061(8) -0.020(9)
C15 0.045(5) 0.102(9) 0.083(9) -0.007(8) -0.007(5) 0.009(6)
C21 0.062(7) 0.082(8) 0.122(11) 0.030(8) 0.016(7) -0.018(7)
C20 0.141(12) 0.035(6) 0.139(14) -0.013(7) -0.019(10) 0.026(8)
C14 0.079(8) 0.116(10) 0.070(9) 0.022(8) -0.042(6) -0.008(8)
C13 0.086(8) 0.163(13) 0.041(7) 0.009(7) -0.004(5) 0.001(9)
C12 0.054(6) 0.143(11) 0.067(8) -0.017(7) 0.019(5) 0.012(7)
C19 0.087(11) 0.20(2) 0.107(12) -0.056(14) 0.033(9) 0.038(14)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy01 O1 2.304(4) . ?
Dy01 O2 2.329(4) 2_656 ?
Dy01 O1 2.359(4) 2_656 ?
Dy01 N1 2.429(5) 2_656 ?
Dy01 N2 2.532(5) 2_656 ?
Dy01 Cl1 2.599(2) . ?
Dy01 Cl2 2.6291(19) . ?
Dy01 Dy01 3.7564(6) 2_656 ?
O1 C1 1.364(7) . ?
O1 Dy01 2.359(4) 2_656 ?
O2 C11 1.250(8) . ?
O2 Dy01 2.329(4) 2_656 ?
N2 C10 1.272(8) . ?
N2 N3 1.362(8) . ?
N2 Dy01 2.532(5) 2_656 ?
N1 C9 1.347(8) . ?
N1 C5 1.359(8) . ?
N1 Dy01 2.429(5) 2_656 ?
N4 C11 1.301(9) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N3 C11 1.366(9) . ?
N3 H3 0.8600 . ?
C9 C8 1.408(9) . ?
C9 C10 1.442(10) . ?
C1 C2 1.360(9) . ?
C1 C5 1.425(9) . ?
C5 C6 1.425(9) . ?
N5 C16 1.309(10) . ?
N5 C12 1.313(11) . ?
C10 H10 0.9300 . ?
C2 C3 1.381(10) . ?
C2 H2 0.9300 . ?
C6 C7 1.409(10) . ?
C6 C4 1.413(10) . ?
C3 C4 1.379(11) . ?
C3 H3A 0.9300 . ?
C4 H4 0.9300 . ?
N6 C21 1.330(14) . ?
N6 C17 1.371(13) . ?
N6 H6 0.8600 . ?
C8 C7 1.348(11) . ?
C8 H8 0.9300 . ?
C7 H7 0.9300 . ?
C17 C18 1.227(15) . ?
C17 H17 0.9300 . ?
C16 C15 1.345(13) . ?
C16 H16 0.9300 . ?
C18 C19 1.19(2) . ?
C18 H18 0.9300 . ?
C15 C14 1.309(15) . ?
C15 H15 0.9300 . ?
C21 C20 1.358(15) . ?
C21 H21 0.9300 . ?
C20 C19 1.41(2) . ?
C20 H20 0.9300 . ?
C14 C13 1.367(16) . ?
C14 H14 0.9300 . ?
C13 C12 1.384(13) . ?
C13 H13 0.9300 . ?
C12 H12 0.9300 . ?
C19 H19 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy01 O2 93.37(15) . 2_656 ?
O1 Dy01 O1 72.58(16) . 2_656 ?
O2 Dy01 O1 163.80(16) 2_656 2_656 ?
O1 Dy01 N1 140.42(16) . 2_656 ?
O2 Dy01 N1 126.21(17) 2_656 2_656 ?
O1 Dy01 N1 68.21(16) 2_656 2_656 ?
O1 Dy01 N2 156.36(16) . 2_656 ?
O2 Dy01 N2 63.30(16) 2_656 2_656 ?
O1 Dy01 N2 131.06(16) 2_656 2_656 ?
N1 Dy01 N2 63.03(17) 2_656 2_656 ?
O1 Dy01 Cl1 94.89(12) . . ?
O2 Dy01 Cl1 88.79(14) 2_656 . ?
O1 Dy01 Cl1 100.19(12) 2_656 . ?
N1 Dy01 Cl1 86.93(14) 2_656 . ?
N2 Dy01 Cl1 81.55(14) 2_656 . ?
O1 Dy01 Cl2 98.72(12) . . ?
O2 Dy01 Cl2 86.57(14) 2_656 . ?
O1 Dy01 Cl2 87.64(12) 2_656 . ?
N1 Dy01 Cl2 85.06(14) 2_656 . ?
N2 Dy01 Cl2 84.42(13) 2_656 . ?
Cl1 Dy01 Cl2 165.85(7) . . ?
O1 Dy01 Dy01 36.82(10) . 2_656 ?
O2 Dy01 Dy01 129.34(11) 2_656 2_656 ?
O1 Dy01 Dy01 35.83(10) 2_656 2_656 ?
N1 Dy01 Dy01 104.01(12) 2_656 2_656 ?
N2 Dy01 Dy01 166.77(12) 2_656 2_656 ?
Cl1 Dy01 Dy01 101.21(5) . 2_656 ?
Cl2 Dy01 Dy01 92.05(4) . 2_656 ?
C1 O1 Dy01 133.3(4) . . ?
C1 O1 Dy01 119.3(4) . 2_656 ?
Dy01 O1 Dy01 107.34(16) . 2_656 ?
C11 O2 Dy01 125.8(4) . 2_656 ?
C10 N2 N3 122.3(6) . . ?
C10 N2 Dy01 121.1(4) . 2_656 ?
N3 N2 Dy01 116.6(4) . 2_656 ?
C9 N1 C5 119.2(6) . . ?
C9 N1 Dy01 123.5(4) . 2_656 ?
C5 N1 Dy01 117.3(4) . 2_656 ?
C11 N4 H4A 120.0 . . ?
C11 N4 H4B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
N2 N3 C11 114.3(6) . . ?
N2 N3 H3 122.8 . . ?
C11 N3 H3 122.8 . . ?
N1 C9 C8 122.1(7) . . ?
N1 C9 C10 114.7(6) . . ?
C8 C9 C10 123.1(6) . . ?
C2 C1 O1 125.1(6) . . ?
C2 C1 C5 117.1(6) . . ?
O1 C1 C5 117.8(6) . . ?
N1 C5 C6 121.4(6) . . ?
N1 C5 C1 117.3(6) . . ?
C6 C5 C1 121.4(7) . . ?
O2 C11 N4 123.2(7) . . ?
O2 C11 N3 120.0(6) . . ?
N4 C11 N3 116.9(7) . . ?
C16 N5 C12 114.8(8) . . ?
N2 C10 C9 117.5(6) . . ?
N2 C10 H10 121.3 . . ?
C9 C10 H10 121.3 . . ?
C1 C2 C3 122.1(7) . . ?
C1 C2 H2 118.9 . . ?
C3 C2 H2 118.9 . . ?
C7 C6 C4 124.1(7) . . ?
C7 C6 C5 117.1(7) . . ?
C4 C6 C5 118.8(7) . . ?
C4 C3 C2 122.6(7) . . ?
C4 C3 H3A 118.7 . . ?
C2 C3 H3A 118.7 . . ?
C3 C4 C6 118.0(7) . . ?
C3 C4 H4 121.0 . . ?
C6 C4 H4 121.0 . . ?
C21 N6 C17 117.7(10) . . ?
C21 N6 H6 121.1 . . ?
C17 N6 H6 121.1 . . ?
C7 C8 C9 118.9(7) . . ?
C7 C8 H8 120.6 . . ?
C9 C8 H8 120.6 . . ?
C8 C7 C6 121.2(7) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C18 C17 N6 124.5(12) . . ?
C18 C17 H17 117.7 . . ?
N6 C17 H17 117.7 . . ?
N5 C16 C15 126.4(10) . . ?
N5 C16 H16 116.8 . . ?
C15 C16 H16 116.8 . . ?
C19 C18 C17 120.1(14) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C14 C15 C16 117.8(10) . . ?
C14 C15 H15 121.1 . . ?
C16 C15 H15 121.1 . . ?
N6 C21 C20 116.8(11) . . ?
N6 C21 H21 121.6 . . ?
C20 C21 H21 121.6 . . ?
C21 C20 C19 117.4(11) . . ?
C21 C20 H20 121.3 . . ?
C19 C20 H20 121.3 . . ?
C15 C14 C13 120.3(10) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C13 C12 117.1(10) . . ?
C14 C13 H13 121.4 . . ?
C12 C13 H13 121.4 . . ?
N5 C12 C13 123.5(10) . . ?
N5 C12 H12 118.2 . . ?
C13 C12 H12 118.2 . . ?
C18 C19 C20 123.1(14) . . ?
C18 C19 H19 118.5 . . ?
C20 C19 H19 118.5 . . ?
_refine_diff_density_max 1.348
_refine_diff_density_min -0.954
_refine_diff_density_rms 0.161
_shelx_res_file
;
2.res created by SHELXL-2014/7
TITL 2_a.res in C2/c
REM Old TITL 2 in Cc
REM SHELXT solution in C2/c
REM R1 0.137, Rweak 0.037, Alpha 0.073, Orientation as input
REM Formula found by SHELXT: C12 N5 O3 Dy F2 S2
CELL 0.71073 20.3353 15.0093 15.7056 90 106.012 90
ZERR 4 0.0012 0.0013 0.0009 0 0.006 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Cl Dy N O
UNIT 168 160 16 8 48 16
L.S. 10
PLAN 20
TEMP 19.85
BOND $H
list 4
fmap 2
acta 52
dfix 2.15 H7 H18
REM
REM
REM
WGHT 0.043400
FVAR 0.08907
DY01 4 0.563224 0.628484 0.862636 11.00000 0.02265 0.04580 =
0.02120 -0.00056 0.00285 -0.00096
CL2 3 0.582873 0.455764 0.856252 11.00000 0.04282 0.04667 =
0.03804 0.00338 0.01266 0.00272
CL1 3 0.572697 0.797843 0.898430 11.00000 0.05937 0.04936 =
0.05276 -0.00578 0.01550 -0.00123
O1 6 0.447994 0.632447 0.790842 11.00000 0.02495 0.04669 =
0.02211 -0.00066 0.00470 -0.00142
O2 6 0.454933 0.603276 0.499293 11.00000 0.02778 0.06797 =
0.02634 -0.00722 0.00973 0.00303
N2 5 0.331623 0.624132 0.505745 11.00000 0.03054 0.04381 =
0.02484 0.00149 0.00607 0.00396
N1 5 0.326498 0.641586 0.668159 11.00000 0.02493 0.04978 =
0.01909 0.00192 0.00042 0.00106
N4 5 0.423031 0.590037 0.351258 11.00000 0.04466 0.08507 =
0.02654 -0.00735 0.00851 0.00678
AFIX 93
H4A 2 0.464640 0.583448 0.349469 11.00000 -1.20000
H4B 2 0.390253 0.589151 0.303034 11.00000 -1.20000
AFIX 0
N3 5 0.342453 0.611071 0.424862 11.00000 0.04129 0.08100 =
0.02411 -0.00550 0.00749 -0.00943
AFIX 43
H3 2 0.309751 0.609114 0.376597 11.00000 -1.20000
AFIX 0
C9 1 0.266626 0.645850 0.604546 11.00000 0.02480 0.06470 =
0.03143 0.00218 0.00552 0.00146
C1 1 0.390696 0.638013 0.819627 11.00000 0.03309 0.04503 =
0.02860 0.00082 0.01011 0.00188
C5 1 0.326243 0.644056 0.754559 11.00000 0.02582 0.04967 =
0.03619 0.00053 0.01275 0.00054
C11 1 0.409678 0.601341 0.426899 11.00000 0.03385 0.04468 =
0.03242 0.00057 0.00788 0.00200
N5 5 0.239458 0.599278 0.261780 11.00000 0.04610 0.07292 =
0.04069 -0.00078 0.00141 0.01257
C10 1 0.272045 0.634437 0.515558 11.00000 0.02411 0.07755 =
0.02336 0.01207 -0.00409 -0.00002
AFIX 43
H10 2 0.233437 0.634604 0.467163 11.00000 -1.20000
AFIX 0
C2 1 0.389973 0.636404 0.905922 11.00000 0.03200 0.08309 =
0.02717 0.00796 0.00470 0.00581
AFIX 43
H2 2 0.431099 0.629659 0.949680 11.00000 -1.20000
AFIX 0
C6 1 0.264119 0.652739 0.779082 11.00000 0.03393 0.06669 =
0.03173 0.00816 0.00693 0.00363
C3 1 0.330142 0.644462 0.930703 11.00000 0.03818 0.11224 =
0.03300 0.00686 0.01185 0.00946
AFIX 43
H3A 2 0.332519 0.643566 0.990686 11.00000 -1.20000
AFIX 0
C4 1 0.267041 0.653780 0.869993 11.00000 0.03575 0.11370 =
0.03466 0.00768 0.01768 0.00741
AFIX 43
H4 2 0.227576 0.660550 0.888335 11.00000 -1.20000
AFIX 0
N6 5 -0.004619 0.678139 0.901208 11.00000 0.10710 0.11297 =
0.11331 0.01105 0.03620 0.05233
AFIX 43
H6 2 -0.030422 0.715613 0.918156 11.00000 -1.20000
AFIX 0
C8 1 0.203769 0.657710 0.624423 11.00000 0.02080 0.13295 =
0.03553 0.01292 0.00186 0.00999
AFIX 43
H8 2 0.163264 0.662752 0.579266 11.00000 -1.20000
AFIX 0
C7 1 0.203293 0.661633 0.710022 11.00000 0.02670 0.11852 =
0.03724 0.01103 0.00893 0.01414
AFIX 43
H7 2 0.162085 0.670364 0.723704 11.00000 -1.20000
AFIX 0
C17 1 0.048357 0.706369 0.869643 11.00000 0.07894 0.08111 =
0.11871 0.03560 0.01704 -0.02293
AFIX 43
H17 2 0.053599 0.767386 0.863547 11.00000 -1.20000
AFIX 0
C16 1 0.176354 0.619977 0.258980 11.00000 0.05320 0.09131 =
0.06644 -0.00520 0.01600 0.00179
AFIX 43
H16 2 0.166901 0.628896 0.313009 11.00000 -1.20000
AFIX 0
C18 1 0.089311 0.656727 0.848890 11.00000 0.06173 0.12189 =
0.12590 -0.01259 0.06092 -0.01967
AFIX 43
H18 2 0.126789 0.680526 0.833754 11.00000 -1.20000
AFIX 0
C15 1 0.123834 0.629613 0.185618 11.00000 0.04496 0.10189 =
0.08330 -0.00732 -0.00737 0.00934
AFIX 43
H15 2 0.080314 0.644479 0.189335 11.00000 -1.20000
AFIX 0
C21 1 -0.014732 0.590847 0.904716 11.00000 0.06240 0.08221 =
0.12207 0.03005 0.01574 -0.01792
AFIX 43
H21 2 -0.050664 0.567790 0.923835 11.00000 -1.20000
AFIX 0
C20 1 0.029957 0.537009 0.879025 11.00000 0.14097 0.03473 =
0.13917 -0.01281 -0.01883 0.02630
AFIX 43
H20 2 0.026861 0.475309 0.881746 11.00000 -1.20000
AFIX 0
C14 1 0.135999 0.617376 0.108823 11.00000 0.07861 0.11624 =
0.07027 0.02222 -0.04178 -0.00804
AFIX 43
H14 2 0.100964 0.624791 0.056877 11.00000 -1.20000
AFIX 0
C13 1 0.199978 0.593744 0.104639 11.00000 0.08605 0.16260 =
0.04092 0.00876 -0.00373 0.00093
AFIX 43
H13 2 0.209369 0.584009 0.050693 11.00000 -1.20000
AFIX 0
C12 1 0.250166 0.584939 0.184196 11.00000 0.05399 0.14287 =
0.06718 -0.01658 0.01861 0.01217
AFIX 43
H12 2 0.293796 0.567962 0.182614 11.00000 -1.20000
AFIX 0
C19 1 0.081200 0.578285 0.848085 11.00000 0.08672 0.20201 =
0.10678 -0.05605 0.03320 0.03813
AFIX 43
H19 2 0.110022 0.542473 0.826001 11.00000 -1.20000
AFIX 0
HKLF 4
REM 2_a.res in C2/c
REM R1 = 0.0509 for 3639 Fo > 4sig(Fo) and 0.0820 for all 5231 data
REM 289 parameters refined using 1 restraints
END
WGHT 0.0434 0.0000
REM Highest difference peak 1.348, deepest hole -0.954, 1-sigma level 0.161
Q1 1 0.5924 0.5759 0.8594 11.00000 0.05 1.35
Q2 1 0.5334 0.6848 0.8563 11.00000 0.05 1.28
Q3 1 0.5866 0.6773 0.8599 11.00000 0.05 1.11
Q4 1 0.5097 0.6257 0.8039 11.00000 0.05 1.08
Q5 1 0.5382 0.5764 0.8673 11.00000 0.05 1.05
Q6 1 0.5970 0.6266 0.9207 11.00000 0.05 0.96
Q7 1 0.5887 0.6993 0.8971 11.00000 0.05 0.88
Q8 1 0.6024 0.7411 0.8993 11.00000 0.05 0.80
Q9 1 0.5578 0.5025 0.8537 11.00000 0.05 0.75
Q10 1 0.3878 0.6306 0.7125 11.00000 0.05 0.74
Q11 1 0.6103 0.5084 0.8832 11.00000 0.05 0.70
Q12 1 0.5787 0.7396 0.9833 11.00000 0.05 0.59
Q13 1 0.0555 0.6163 0.8480 11.00000 0.05 0.59
Q14 1 0.0771 0.6804 0.8608 11.00000 0.05 0.59
Q15 1 0.6058 0.4601 0.8998 11.00000 0.05 0.58
Q16 1 0.5593 0.4565 0.8816 11.00000 0.05 0.56
Q17 1 0.2203 0.6221 0.3424 11.00000 0.05 0.55
Q18 1 0.4624 0.5815 0.8210 11.00000 0.05 0.54
Q19 1 0.5516 0.7425 0.9090 11.00000 0.05 0.54
Q20 1 0.4377 0.5759 0.5688 11.00000 0.05 0.54
;
_shelx_res_checksum 51043
#######################################################################
#
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1888735'
_audit_update_record
;
2019-01-30 deposited with the CCDC. 2019-03-06 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C12 H14 Cl3 Dy N4 O3'
_chemical_formula_weight 531.12
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'
O O 0.0106 0.0060 '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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/n'
loop_
_symmetry_equiv_pos_as_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 8.02653(15)
_cell_length_b 19.3019(4)
_cell_length_c 11.1247(2)
_cell_angle_alpha 90.00
_cell_angle_beta 95.6771(19)
_cell_angle_gamma 90.00
_cell_volume 1715.07(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 6017
_cell_measurement_theta_min 3.1598
_cell_measurement_theta_max 29.1563
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.057
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1020
_exptl_absorpt_coefficient_mu 4.841
_exptl_absorpt_correction_type ?
_exptl_absorpt_correction_T_min 0.423
_exptl_absorpt_correction_T_max 0.484
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using
spherical harmonics,
implemented in SCALE3 ABSPACK
scaling algorithm.
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Xcalibur, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 13903
_diffrn_reflns_av_R_equivalents 0.0329
_diffrn_reflns_av_sigmaI/netI 0.0318
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 3.17
_diffrn_reflns_theta_max 29.22
_reflns_number_total 4105
_reflns_number_gt 3643
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrysAlis PRO (Agilent, 2011)'
_computing_cell_refinement 'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction 'CrysAlis PRO (Agilent, 2011)'
_computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.6131P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4105
_refine_ls_number_parameters 218
_refine_ls_number_restraints 23
_refine_ls_R_factor_all 0.0337
_refine_ls_R_factor_gt 0.0278
_refine_ls_wR_factor_ref 0.0698
_refine_ls_wR_factor_gt 0.0666
_refine_ls_goodness_of_fit_ref 1.097
_refine_ls_restrained_S_all 1.102
_refine_ls_shift/su_max 0.073
_refine_ls_shift/su_mean 0.004
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.764177(18) 0.359699(8) 0.358286(14) 0.02184(7) Uani 1 1 d . . .
O2 O 1.0139(3) 0.32659(14) 0.4659(2) 0.0320(6) Uani 1 1 d . . .
N4 N 1.2885(4) 0.33738(19) 0.5294(3) 0.0354(7) Uani 1 1 d . . .
H4A H 1.2735 0.2947 0.5567 0.053 Uiso 1 1 calc R . .
H4B H 1.3223 0.3650 0.5911 0.053 Uiso 1 1 calc R . .
H4C H 1.3658 0.3366 0.4773 0.053 Uiso 1 1 calc R . .
O1 O 0.4839(3) 0.37036(14) 0.2589(2) 0.0330(6) Uani 1 1 d . . .
C7 C 0.6264(5) 0.5990(2) 0.1470(3) 0.0383(9) Uani 1 1 d . . .
H7 H 0.6022 0.6417 0.1108 0.046 Uiso 1 1 calc R . .
N2 N 0.9975(3) 0.44606(16) 0.3691(2) 0.0247(6) Uani 1 1 d . . .
C3 C 0.2303(5) 0.5026(3) 0.0877(4) 0.0465(11) Uani 1 1 d . . .
H3 H 0.1227 0.5084 0.0496 0.056 Uiso 1 1 calc R . .
C10 C 0.9807(4) 0.50574(19) 0.3193(3) 0.0278(8) Uani 1 1 d . . .
H10 H 1.0688 0.5372 0.3225 0.033 Uiso 1 1 calc R . .
N1 N 0.7027(3) 0.47222(15) 0.2573(2) 0.0237(6) Uani 1 1 d . . .
N3 N 1.1468(3) 0.42593(16) 0.4274(3) 0.0281(6) Uani 1 1 d . . .
H3A H 1.2339 0.4521 0.4336 0.034 Uiso 1 1 calc R . .
C5 C 0.5478(4) 0.48415(19) 0.2007(3) 0.0255(7) Uani 1 1 d . . .
C2 C 0.2720(5) 0.4390(3) 0.1447(3) 0.0394(10) Uani 1 1 d . . .
H2 H 0.1930 0.4038 0.1441 0.047 Uiso 1 1 calc R . .
C9 C 0.8166(4) 0.52206(19) 0.2573(3) 0.0264(7) Uani 1 1 d . . .
C6 C 0.5034(5) 0.5479(2) 0.1439(3) 0.0323(8) Uani 1 1 d . . .
C8 C 0.7829(5) 0.5863(2) 0.2033(3) 0.0342(8) Uani 1 1 d . . .
H8 H 0.8655 0.6202 0.2055 0.041 Uiso 1 1 calc R . .
C1 C 0.4290(4) 0.4295(2) 0.2008(3) 0.0285(8) Uani 1 1 d . . .
C4 C 0.3404(5) 0.5556(2) 0.0860(3) 0.0424(10) Uani 1 1 d . . .
H4 H 0.3087 0.5968 0.0470 0.051 Uiso 1 1 calc R . .
C11 C 1.1469(4) 0.36066(18) 0.4752(3) 0.0259(8) Uani 1 1 d . . .
Cl1 Cl 0.64565(12) 0.24479(5) 0.43348(9) 0.0362(2) Uani 1 1 d . . .
Cl3 Cl 0.64759(11) 0.42814(5) 0.54017(8) 0.03059(19) Uani 1 1 d . . .
Cl2 Cl 0.85924(13) 0.32194(6) 0.15284(9) 0.0442(3) Uani 1 1 d . . .
C12 C 0.2437(6) 0.2169(3) 0.2690(5) 0.0608(13) Uani 1 1 d DU . .
H12A H 0.2624 0.1745 0.2271 0.091 Uiso 1 1 d R A .
H12B H 0.1265 0.2217 0.2778 0.091 Uiso 1 1 d R . .
H12C H 0.3056 0.2159 0.3474 0.091 Uiso 1 1 d R . .
O3 O 0.326(3) 0.2613(12) 0.1917(11) 0.071(4) Uani 0.56(5) 1 d PDU A 1
H3B H 0.3672 0.2941 0.2308 0.107 Uiso 0.56(5) 1 calc PR A 1
O3' O 0.264(3) 0.2803(8) 0.217(2) 0.051(5) Uani 0.44(5) 1 d PDU A 2
H3'A H 0.3469 0.2995 0.2510 0.077 Uiso 0.44(5) 1 calc PR A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.01881(10) 0.01895(10) 0.02756(10) -0.00099(6) 0.00133(7) -0.00199(6)
O2 0.0219(12) 0.0256(14) 0.0473(15) 0.0078(12) -0.0022(11) -0.0034(11)
N4 0.0243(15) 0.0372(19) 0.0440(19) 0.0017(15) -0.0008(14) 0.0025(14)
O1 0.0219(13) 0.0347(15) 0.0407(15) 0.0032(12) -0.0048(11) -0.0061(11)
C7 0.054(3) 0.024(2) 0.037(2) 0.0045(16) 0.0046(18) 0.0077(19)
N2 0.0202(13) 0.0255(16) 0.0283(14) -0.0020(12) 0.0013(11) -0.0008(12)
C3 0.035(2) 0.066(3) 0.035(2) 0.002(2) -0.0093(17) 0.016(2)
C10 0.0283(18) 0.0243(19) 0.0311(18) -0.0008(15) 0.0040(15) -0.0068(15)
N1 0.0246(14) 0.0245(15) 0.0219(13) -0.0005(11) 0.0021(11) 0.0015(12)
N3 0.0183(13) 0.0285(17) 0.0363(16) 0.0020(13) -0.0034(12) -0.0060(12)
C5 0.0249(17) 0.033(2) 0.0178(15) -0.0007(14) 0.0007(13) 0.0047(15)
C2 0.0261(18) 0.057(3) 0.035(2) -0.0040(18) 0.0008(16) -0.0020(19)
C9 0.0300(18) 0.0235(18) 0.0261(17) 0.0001(14) 0.0040(14) 0.0001(15)
C6 0.036(2) 0.040(2) 0.0215(17) 0.0020(16) 0.0036(15) 0.0109(18)
C8 0.041(2) 0.024(2) 0.037(2) 0.0024(16) 0.0050(17) -0.0034(17)
C1 0.0248(17) 0.038(2) 0.0222(16) -0.0009(15) 0.0021(13) 0.0015(16)
C4 0.044(2) 0.048(3) 0.033(2) 0.0068(19) -0.0039(18) 0.016(2)
C11 0.0216(17) 0.028(2) 0.0275(18) -0.0033(14) 0.0006(14) 0.0008(14)
Cl1 0.0373(5) 0.0233(5) 0.0477(5) 0.0022(4) 0.0031(4) -0.0071(4)
Cl3 0.0305(4) 0.0271(5) 0.0347(4) -0.0076(4) 0.0057(4) -0.0047(4)
Cl2 0.0491(6) 0.0473(6) 0.0375(5) -0.0109(5) 0.0109(4) 0.0036(5)
C12 0.061(3) 0.045(3) 0.073(3) -0.004(2) -0.012(3) -0.014(2)
O3 0.082(8) 0.072(7) 0.056(5) -0.006(4) -0.012(5) -0.041(6)
O3' 0.043(7) 0.045(6) 0.061(7) 0.005(4) -0.025(5) -0.026(4)
_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 O2 2.321(2) . ?
Dy1 O1 2.415(2) . ?
Dy1 N1 2.472(3) . ?
Dy1 N2 2.501(3) . ?
Dy1 Cl2 2.5849(10) . ?
Dy1 Cl1 2.5849(9) . ?
Dy1 Cl3 2.6626(9) . ?
O2 C11 1.249(4) . ?
N4 C11 1.313(5) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?
O1 C1 1.364(4) . ?
C7 C8 1.369(6) . ?
C7 C6 1.393(6) . ?
C7 H7 0.9300 . ?
N2 C10 1.279(5) . ?
N2 N3 1.361(4) . ?
C3 C4 1.354(6) . ?
C3 C2 1.406(7) . ?
C3 H3 0.9300 . ?
C10 C9 1.459(5) . ?
C10 H10 0.9300 . ?
N1 C9 1.327(4) . ?
N1 C5 1.357(4) . ?
N3 C11 1.367(5) . ?
N3 H3A 0.8600 . ?
C5 C6 1.413(5) . ?
C5 C1 1.421(5) . ?
C2 C1 1.363(5) . ?
C2 H2 0.9300 . ?
C9 C8 1.393(5) . ?
C6 C4 1.407(5) . ?
C8 H8 0.9300 . ?
C4 H4 0.9300 . ?
C12 O3' 1.372(11) . ?
C12 O3 1.421(11) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9599 . ?
C12 H12C 0.9600 . ?
O3 H3B 0.8200 . ?
O3' H3'A 0.8200 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O1 167.83(9) . . ?
O2 Dy1 N1 126.85(9) . . ?
O1 Dy1 N1 65.31(9) . . ?
O2 Dy1 N2 63.53(9) . . ?
O1 Dy1 N2 128.63(9) . . ?
N1 Dy1 N2 63.33(9) . . ?
O2 Dy1 Cl2 93.62(7) . . ?
O1 Dy1 Cl2 87.85(7) . . ?
N1 Dy1 Cl2 84.79(7) . . ?
N2 Dy1 Cl2 86.87(7) . . ?
O2 Dy1 Cl1 85.61(6) . . ?
O1 Dy1 Cl1 82.25(7) . . ?
N1 Dy1 Cl1 146.87(7) . . ?
N2 Dy1 Cl1 148.66(7) . . ?
Cl2 Dy1 Cl1 101.22(3) . . ?
O2 Dy1 Cl3 95.46(7) . . ?
O1 Dy1 Cl3 85.64(7) . . ?
N1 Dy1 Cl3 80.79(7) . . ?
N2 Dy1 Cl3 87.16(7) . . ?
Cl2 Dy1 Cl3 165.57(3) . . ?
Cl1 Dy1 Cl3 90.66(3) . . ?
C11 O2 Dy1 125.8(2) . . ?
C11 N4 H4A 109.5 . . ?
C11 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
C11 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
C1 O1 Dy1 122.1(2) . . ?
C8 C7 C6 120.1(4) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C10 N2 N3 120.9(3) . . ?
C10 N2 Dy1 122.2(2) . . ?
N3 N2 Dy1 116.9(2) . . ?
C4 C3 C2 122.6(4) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
N2 C10 C9 116.8(3) . . ?
N2 C10 H10 121.6 . . ?
C9 C10 H10 121.6 . . ?
C9 N1 C5 118.5(3) . . ?
C9 N1 Dy1 122.0(2) . . ?
C5 N1 Dy1 119.5(2) . . ?
N2 N3 C11 114.5(3) . . ?
N2 N3 H3A 122.7 . . ?
C11 N3 H3A 122.7 . . ?
N1 C5 C6 122.3(3) . . ?
N1 C5 C1 117.2(3) . . ?
C6 C5 C1 120.5(3) . . ?
C1 C2 C3 119.5(4) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
N1 C9 C8 122.8(3) . . ?
N1 C9 C10 115.7(3) . . ?
C8 C9 C10 121.6(3) . . ?
C7 C6 C4 124.1(4) . . ?
C7 C6 C5 117.3(3) . . ?
C4 C6 C5 118.6(4) . . ?
C7 C8 C9 119.1(4) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C2 C1 O1 124.8(4) . . ?
C2 C1 C5 119.3(4) . . ?
O1 C1 C5 115.9(3) . . ?
C3 C4 C6 119.5(4) . . ?
C3 C4 H4 120.2 . . ?
C6 C4 H4 120.2 . . ?
O2 C11 N4 123.5(3) . . ?
O2 C11 N3 119.0(3) . . ?
N4 C11 N3 117.5(3) . . ?
O3' C12 O3 28.9(5) . . ?
O3' C12 H12A 121.7 . . ?
O3 C12 H12A 96.7 . . ?
O3' C12 H12B 96.6 . . ?
O3 C12 H12B 121.4 . . ?
H12A C12 H12B 109.5 . . ?
O3' C12 H12C 109.1 . . ?
O3 C12 H12C 109.4 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C12 O3 H3B 109.4 . . ?
C12 O3' H3'A 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.883
_diffrn_reflns_theta_full 26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 1.015
_refine_diff_density_min -1.100
_refine_diff_density_rms 0.145
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_4
_database_code_depnum_ccdc_archive 'CCDC 1888678'
_audit_update_record
;
2019-01-30 deposited with the CCDC. 2019-03-06 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 'C42 H34 Dy2 F12 N6 O18 S4'
_chemical_formula_weight 1591.99
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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 11.5623(12)
_cell_length_b 11.9207(13)
_cell_length_c 19.877(3)
_cell_angle_alpha 90
_cell_angle_beta 96.515(12)
_cell_angle_gamma 90
_cell_volume 2722.0(6)
_cell_formula_units_Z 2
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 2834
_cell_measurement_theta_min 3.3328
_cell_measurement_theta_max 27.9481
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.942
_exptl_crystal_F_000 1552
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.16
_exptl_absorpt_coefficient_mu 2.994
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type ?
_exptl_absorpt_correction_T_min 0.39071
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using
spherical harmonics,
implemented in SCALE3 ABSPACK
scaling algorithm.
;
_exptl_absorpt_special_details ?
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_source ?
_diffrn_measurement_device_type 'Xcalibur, Eos'
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 20931
_diffrn_reflns_av_unetI/netI 0.0817
_diffrn_reflns_av_R_equivalents 0.0813
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_theta_min 3.340
_diffrn_reflns_theta_max 28.010
_diffrn_reflns_theta_full 26.000
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total 6131
_reflns_number_gt 4129
_reflns_threshold_expression 'I > 2\s(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 'CrysAlis PRO (Agilent, 2011)'
_computing_cell_refinement 'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction 'CrysAlis PRO (Agilent, 2011)'
_computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker 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/[\s^2^(Fo^2^)+(0.0511P)^2^+3.5275P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 6131
_refine_ls_number_parameters 380
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0952
_refine_ls_R_factor_gt 0.0584
_refine_ls_wR_factor_ref 0.1419
_refine_ls_wR_factor_gt 0.1195
_refine_ls_goodness_of_fit_ref 1.056
_refine_ls_restrained_S_all 1.056
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.58788(3) 0.45264(3) 0.58093(2) 0.03916(14) Uani 1 1 d . . . . .
S1 S 0.5927(2) 0.50760(19) 0.76116(11) 0.0574(5) Uani 1 1 d . . . . .
S2 S 0.72614(18) 0.26745(19) 0.46655(11) 0.0559(5) Uani 1 1 d . . . . .
O2 O 0.4018(4) 0.4640(4) 0.5267(2) 0.0381(11) Uani 1 1 d . . . . .
O1 O 0.7816(4) 0.4820(4) 0.6250(3) 0.0441(12) Uani 1 1 d . . . . .
N1 N 0.4715(5) 0.2913(5) 0.6050(3) 0.0380(13) Uani 1 1 d . . . . .
N3 N 0.8047(5) 0.3124(5) 0.6706(3) 0.0431(14) Uani 1 1 d . . . . .
H3 H 0.8473 0.2603 0.6903 0.052 Uiso 1 1 calc R U . . .
N2 N 0.6878(5) 0.2991(5) 0.6528(3) 0.0399(14) Uani 1 1 d . . . . .
O4 O 0.5369(5) 0.4754(4) 0.6951(3) 0.0517(13) Uani 1 1 d . . . . .
O3 O 0.5675(4) 0.6493(4) 0.5983(3) 0.0553(14) Uani 1 1 d . . . . .
O8 O 0.6668(5) 0.2598(6) 0.3997(3) 0.0758(18) Uani 1 1 d . . . . .
F2 F 0.7991(7) 0.1205(6) 0.5568(4) 0.134(3) Uani 1 1 d . . . . .
O7 O 0.6507(6) 0.3102(5) 0.5141(3) 0.0712(18) Uani 1 1 d . . . . .
C11 C 0.8481(6) 0.4114(6) 0.6555(4) 0.0407(17) Uani 1 1 d . . . . .
F3 F 0.8171(7) 0.0708(6) 0.4565(4) 0.133(3) Uani 1 1 d . . . . .
C12 C 0.9727(6) 0.4362(6) 0.6750(4) 0.0445(18) Uani 1 1 d . . . . .
C1 C 0.3182(6) 0.3891(6) 0.5411(4) 0.0408(17) Uani 1 1 d . . . . .
F5 F 0.5716(6) 0.4270(6) 0.8805(3) 0.107(2) Uani 1 1 d . . . . .
C2 C 0.2026(6) 0.3974(7) 0.5194(4) 0.0500(19) Uani 1 1 d . . . . .
H2 H 0.1753 0.4593 0.4938 0.060 Uiso 1 1 calc R U . . .
O5 O 0.7157(5) 0.4826(6) 0.7720(3) 0.085(2) Uani 1 1 d . . . . .
C5 C 0.3573(6) 0.2964(6) 0.5818(3) 0.0388(16) Uani 1 1 d . . . . .
C9 C 0.5115(6) 0.2050(6) 0.6433(4) 0.0410(17) Uani 1 1 d . . . . .
F6 F 0.5595(8) 0.3081(5) 0.8034(3) 0.127(3) Uani 1 1 d . . . . .
C17 C 1.0157(7) 0.5339(7) 0.6525(4) 0.056(2) Uani 1 1 d . . . . .
H17 H 0.9666 0.5837 0.6271 0.067 Uiso 1 1 calc R U . . .
O9 O 0.8383(5) 0.3155(6) 0.4730(4) 0.098(2) Uani 1 1 d . . . . .
C8 C 0.4383(7) 0.1178(6) 0.6604(4) 0.052(2) Uani 1 1 d . . . . .
H8 H 0.4680 0.0581 0.6871 0.062 Uiso 1 1 calc R U . . .
C10 C 0.6366(6) 0.2095(7) 0.6669(4) 0.0458(18) Uani 1 1 d . . . . .
H10 H 0.6754 0.1509 0.6906 0.055 Uiso 1 1 calc R U . . .
O6 O 0.5622(6) 0.6133(5) 0.7832(3) 0.086(2) Uani 1 1 d . . . . .
C13 C 1.0465(7) 0.3637(8) 0.7137(5) 0.064(2) Uani 1 1 d . . . . .
H13 H 1.0179 0.2974 0.7301 0.076 Uiso 1 1 calc R U . . .
C14 C 1.1618(7) 0.3903(8) 0.7276(5) 0.075(3) Uani 1 1 d . . . . .
H14 H 1.2113 0.3413 0.7534 0.090 Uiso 1 1 calc R U . . .
F4 F 0.4203(5) 0.4158(8) 0.8140(4) 0.139(3) Uani 1 1 d . . . . .
C15 C 1.2048(7) 0.4855(10) 0.7048(5) 0.076(3) Uani 1 1 d . . . . .
H15 H 1.2838 0.5015 0.7142 0.091 Uiso 1 1 calc R U . . .
C6 C 0.2786(6) 0.2120(6) 0.5977(4) 0.0492(19) Uani 1 1 d . . . . .
C18 C 0.6462(9) 0.7366(8) 0.6242(6) 0.083(3) Uani 1 1 d . . . . .
H18A H 0.6429 0.7435 0.6725 0.100 Uiso 1 1 calc R U . . .
H18B H 0.7249 0.7148 0.6174 0.100 Uiso 1 1 calc R U . . .
C7 C 0.3234(7) 0.1225(7) 0.6371(4) 0.058(2) Uani 1 1 d . . . . .
H7 H 0.2740 0.0651 0.6477 0.070 Uiso 1 1 calc R U . . .
F1 F 0.6493(8) 0.0694(6) 0.4903(5) 0.140(3) Uani 1 1 d . . . . .
C21 C 0.7468(11) 0.1246(9) 0.4950(6) 0.084(3) Uani 1 1 d . . . . .
C3 C 0.1248(7) 0.3155(7) 0.5347(4) 0.060(2) Uani 1 1 d . . . . .
H3A H 0.0465 0.3234 0.5186 0.072 Uiso 1 1 calc R U . . .
C16 C 1.1332(8) 0.5594(9) 0.6676(5) 0.076(3) Uani 1 1 d . . . . .
H16 H 1.1629 0.6262 0.6526 0.092 Uiso 1 1 calc R U . . .
C20 C 0.5330(8) 0.4111(9) 0.8171(5) 0.065(2) Uani 1 1 d . . . . .
C4 C 0.1590(7) 0.2246(7) 0.5721(4) 0.059(2) Uani 1 1 d . . . . .
H4 H 0.1050 0.1704 0.5813 0.070 Uiso 1 1 calc R U . . .
C19 C 0.6226(10) 0.8422(9) 0.5939(6) 0.102(4) Uani 1 1 d . . . . .
H19A H 0.6008 0.8328 0.5462 0.153 Uiso 1 1 calc R U . . .
H19B H 0.6909 0.8885 0.6011 0.153 Uiso 1 1 calc R U . . .
H19C H 0.5601 0.8775 0.6138 0.153 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.0334(2) 0.0372(2) 0.0447(2) 0.00420(16) -0.00533(14) -0.00204(15)
S1 0.0650(14) 0.0526(13) 0.0535(13) -0.0057(11) 0.0013(10) -0.0104(11)
S2 0.0502(12) 0.0614(14) 0.0554(13) -0.0008(11) 0.0033(10) -0.0006(10)
O2 0.032(2) 0.039(3) 0.041(3) 0.011(2) -0.004(2) -0.002(2)
O1 0.035(3) 0.040(3) 0.055(3) 0.003(2) -0.007(2) -0.003(2)
N1 0.032(3) 0.039(3) 0.041(3) 0.000(3) -0.005(3) -0.002(2)
N3 0.033(3) 0.041(4) 0.052(4) 0.007(3) -0.007(3) 0.002(3)
N2 0.037(3) 0.034(3) 0.046(4) 0.001(3) -0.004(3) 0.000(3)
O4 0.057(3) 0.043(3) 0.054(3) -0.009(2) 0.003(3) -0.001(2)
O3 0.047(3) 0.033(3) 0.081(4) 0.006(3) -0.015(3) -0.009(2)
O8 0.071(4) 0.095(5) 0.059(4) -0.004(4) -0.002(3) -0.004(4)
F2 0.190(8) 0.094(5) 0.107(6) 0.012(4) -0.027(5) 0.065(5)
O7 0.097(5) 0.061(4) 0.058(4) 0.007(3) 0.020(3) 0.030(3)
C11 0.030(3) 0.045(4) 0.045(4) -0.004(4) -0.003(3) 0.002(3)
F3 0.154(7) 0.109(5) 0.139(6) -0.032(5) 0.027(5) 0.059(5)
C12 0.032(4) 0.055(5) 0.046(4) -0.006(4) 0.001(3) 0.001(3)
C1 0.040(4) 0.039(4) 0.043(4) 0.002(3) 0.002(3) -0.002(3)
F5 0.116(5) 0.151(6) 0.051(3) 0.011(4) -0.005(3) -0.033(4)
C2 0.040(4) 0.054(5) 0.053(5) 0.012(4) -0.010(4) -0.005(4)
O5 0.055(4) 0.114(6) 0.084(5) -0.020(4) -0.002(3) -0.001(4)
C5 0.036(4) 0.038(4) 0.041(4) -0.003(3) -0.001(3) -0.003(3)
C9 0.043(4) 0.038(4) 0.041(4) 0.003(3) 0.000(3) -0.002(3)
F6 0.213(9) 0.066(4) 0.106(5) 0.020(4) 0.035(5) -0.003(5)
C17 0.040(4) 0.076(6) 0.050(5) 0.016(4) -0.003(4) -0.012(4)
O9 0.051(4) 0.116(6) 0.125(6) 0.013(5) -0.008(4) -0.016(4)
C8 0.059(5) 0.039(4) 0.054(5) 0.008(4) -0.007(4) -0.005(4)
C10 0.039(4) 0.045(4) 0.051(5) 0.011(4) -0.003(3) 0.003(3)
O6 0.129(6) 0.045(4) 0.080(5) -0.010(3) -0.004(4) -0.003(4)
C13 0.045(4) 0.059(5) 0.082(6) -0.005(5) -0.016(4) 0.006(4)
C14 0.039(5) 0.077(7) 0.103(8) -0.006(6) -0.019(5) 0.006(5)
F4 0.062(4) 0.243(9) 0.112(5) 0.061(6) 0.004(4) -0.032(5)
C15 0.033(4) 0.117(9) 0.076(7) -0.011(6) 0.001(4) -0.009(5)
C6 0.046(4) 0.046(5) 0.054(5) 0.002(4) -0.002(4) -0.011(4)
C18 0.084(7) 0.062(6) 0.097(8) -0.005(6) -0.017(6) -0.013(6)
C7 0.057(5) 0.043(5) 0.072(6) 0.010(4) -0.003(4) -0.017(4)
F1 0.141(7) 0.075(5) 0.203(9) 0.026(5) 0.012(7) -0.022(5)
C21 0.091(8) 0.061(7) 0.099(9) -0.022(6) 0.001(7) 0.022(6)
C3 0.033(4) 0.080(6) 0.067(6) 0.015(5) 0.001(4) -0.008(4)
C16 0.057(6) 0.110(8) 0.062(6) 0.019(6) 0.006(5) -0.031(6)
C20 0.057(6) 0.072(6) 0.063(6) 0.003(5) -0.003(5) -0.010(5)
C4 0.043(4) 0.067(6) 0.065(6) 0.005(5) 0.002(4) -0.018(4)
C19 0.112(9) 0.058(7) 0.130(10) 0.004(7) -0.008(8) -0.025(6)
_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 O2 2.299(4) . ?
Dy1 O7 2.322(5) . ?
Dy1 O1 2.337(4) . ?
Dy1 O2 2.375(4) 3_666 ?
Dy1 O3 2.385(5) . ?
Dy1 O4 2.423(5) . ?
Dy1 N1 2.426(5) . ?
Dy1 N2 2.520(6) . ?
Dy1 Dy1 3.7778(8) 3_666 ?
S1 O6 1.392(6) . ?
S1 O5 1.446(6) . ?
S1 O4 1.448(5) . ?
S1 C20 1.792(10) . ?
S2 O9 1.410(6) . ?
S2 O8 1.428(6) . ?
S2 O7 1.450(6) . ?
S2 C21 1.801(11) . ?
O2 C1 1.369(8) . ?
O2 Dy1 2.375(4) 3_666 ?
O1 C11 1.249(8) . ?
N1 C9 1.331(8) . ?
N1 C5 1.349(8) . ?
N3 C11 1.330(9) . ?
N3 N2 1.367(7) . ?
N3 H3 0.8600 . ?
N2 C10 1.268(9) . ?
O3 C18 1.439(10) . ?
F2 C21 1.308(12) . ?
C11 C12 1.479(9) . ?
F3 C21 1.340(12) . ?
C12 C17 1.362(10) . ?
C12 C13 1.386(10) . ?
C1 C2 1.360(9) . ?
C1 C5 1.414(9) . ?
F5 C20 1.302(10) . ?
C2 C3 1.385(10) . ?
C2 H2 0.9300 . ?
C5 C6 1.415(9) . ?
C9 C8 1.406(10) . ?
C9 C10 1.471(9) . ?
F6 C20 1.302(11) . ?
C17 C16 1.392(11) . ?
C17 H17 0.9300 . ?
C8 C7 1.358(11) . ?
C8 H8 0.9300 . ?
C10 H10 0.9300 . ?
C13 C14 1.368(11) . ?
C13 H13 0.9300 . ?
C14 C15 1.340(13) . ?
C14 H14 0.9300 . ?
F4 C20 1.299(10) . ?
C15 C16 1.366(13) . ?
C15 H15 0.9300 . ?
C6 C7 1.390(10) . ?
C6 C4 1.426(10) . ?
C18 C19 1.408(13) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C7 H7 0.9300 . ?
F1 C21 1.300(13) . ?
C3 C4 1.349(11) . ?
C3 H3A 0.9300 . ?
C16 H16 0.9300 . ?
C4 H4 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O7 96.4(2) . . ?
O2 Dy1 O1 166.74(17) . . ?
O7 Dy1 O1 88.6(2) . . ?
O2 Dy1 O2 72.13(18) . 3_666 ?
O7 Dy1 O2 74.94(17) . 3_666 ?
O1 Dy1 O2 97.53(16) . 3_666 ?
O2 Dy1 O3 84.69(16) . . ?
O7 Dy1 O3 147.5(2) . . ?
O1 Dy1 O3 84.53(16) . . ?
O2 Dy1 O3 74.61(18) 3_666 . ?
O2 Dy1 O4 96.77(17) . . ?
O7 Dy1 O4 137.92(18) . . ?
O1 Dy1 O4 87.53(18) . . ?
O2 Dy1 O4 147.05(16) 3_666 . ?
O3 Dy1 O4 73.51(18) . . ?
O2 Dy1 N1 68.17(16) . . ?
O7 Dy1 N1 75.5(2) . . ?
O1 Dy1 N1 125.06(17) . . ?
O2 Dy1 N1 126.54(17) 3_666 . ?
O3 Dy1 N1 133.22(18) . . ?
O4 Dy1 N1 72.83(18) . . ?
O2 Dy1 N2 130.77(17) . . ?
O7 Dy1 N2 68.88(19) . . ?
O1 Dy1 N2 62.49(17) . . ?
O2 Dy1 N2 138.42(17) 3_666 . ?
O3 Dy1 N2 132.72(18) . . ?
O4 Dy1 N2 72.26(18) . . ?
N1 Dy1 N2 62.70(18) . . ?
O2 Dy1 Dy1 36.75(11) . 3_666 ?
O7 Dy1 Dy1 84.54(14) . 3_666 ?
O1 Dy1 Dy1 132.42(12) . 3_666 ?
O2 Dy1 Dy1 35.39(11) 3_666 3_666 ?
O3 Dy1 Dy1 77.11(12) . 3_666 ?
O4 Dy1 Dy1 126.82(12) . 3_666 ?
N1 Dy1 Dy1 98.51(13) . 3_666 ?
N2 Dy1 Dy1 150.17(13) . 3_666 ?
O6 S1 O5 114.8(4) . . ?
O6 S1 O4 115.0(4) . . ?
O5 S1 O4 114.2(4) . . ?
O6 S1 C20 104.9(5) . . ?
O5 S1 C20 102.5(5) . . ?
O4 S1 C20 103.3(4) . . ?
O9 S2 O8 116.8(4) . . ?
O9 S2 O7 114.4(5) . . ?
O8 S2 O7 111.6(4) . . ?
O9 S2 C21 105.5(5) . . ?
O8 S2 C21 105.3(5) . . ?
O7 S2 C21 101.3(5) . . ?
C1 O2 Dy1 120.6(4) . . ?
C1 O2 Dy1 124.7(4) . 3_666 ?
Dy1 O2 Dy1 107.86(18) . 3_666 ?
C11 O1 Dy1 126.2(4) . . ?
C9 N1 C5 119.5(6) . . ?
C9 N1 Dy1 124.1(4) . . ?
C5 N1 Dy1 116.1(4) . . ?
C11 N3 N2 115.6(6) . . ?
C11 N3 H3 122.2 . . ?
N2 N3 H3 122.2 . . ?
C10 N2 N3 120.9(6) . . ?
C10 N2 Dy1 122.8(5) . . ?
N3 N2 Dy1 116.0(4) . . ?
S1 O4 Dy1 138.5(3) . . ?
C18 O3 Dy1 133.9(5) . . ?
S2 O7 Dy1 151.7(4) . . ?
O1 C11 N3 118.7(6) . . ?
O1 C11 C12 121.3(7) . . ?
N3 C11 C12 120.0(6) . . ?
C17 C12 C13 119.4(7) . . ?
C17 C12 C11 117.8(7) . . ?
C13 C12 C11 122.8(7) . . ?
C2 C1 O2 125.3(6) . . ?
C2 C1 C5 118.5(7) . . ?
O2 C1 C5 116.2(6) . . ?
C1 C2 C3 121.2(7) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
N1 C5 C1 117.9(6) . . ?
N1 C5 C6 121.4(6) . . ?
C1 C5 C6 120.7(6) . . ?
N1 C9 C8 122.0(7) . . ?
N1 C9 C10 114.8(6) . . ?
C8 C9 C10 123.1(7) . . ?
C12 C17 C16 120.0(8) . . ?
C12 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C7 C8 C9 118.7(7) . . ?
C7 C8 H8 120.7 . . ?
C9 C8 H8 120.7 . . ?
N2 C10 C9 115.3(7) . . ?
N2 C10 H10 122.4 . . ?
C9 C10 H10 122.4 . . ?
C14 C13 C12 119.5(9) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C15 C14 C13 121.3(9) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 C15 C16 120.3(8) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C7 C6 C5 117.6(7) . . ?
C7 C6 C4 124.4(7) . . ?
C5 C6 C4 117.9(7) . . ?
C19 C18 O3 114.2(8) . . ?
C19 C18 H18A 108.7 . . ?
O3 C18 H18A 108.7 . . ?
C19 C18 H18B 108.7 . . ?
O3 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
C8 C7 C6 120.7(7) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
F1 C21 F2 110.7(12) . . ?
F1 C21 F3 107.1(9) . . ?
F2 C21 F3 105.8(9) . . ?
F1 C21 S2 111.9(8) . . ?
F2 C21 S2 111.2(8) . . ?
F3 C21 S2 110.0(9) . . ?
C4 C3 C2 122.0(7) . . ?
C4 C3 H3A 119.0 . . ?
C2 C3 H3A 119.0 . . ?
C15 C16 C17 119.5(9) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
F4 C20 F6 106.9(9) . . ?
F4 C20 F5 105.8(9) . . ?
F6 C20 F5 106.1(9) . . ?
F4 C20 S1 113.4(7) . . ?
F6 C20 S1 111.0(7) . . ?
F5 C20 S1 113.1(7) . . ?
C3 C4 C6 119.5(7) . . ?
C3 C4 H4 120.2 . . ?
C6 C4 H4 120.2 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C11 N3 N2 C10 -177.5(7) . . . . ?
C11 N3 N2 Dy1 8.5(7) . . . . ?
O6 S1 O4 Dy1 107.1(5) . . . . ?
O5 S1 O4 Dy1 -28.7(6) . . . . ?
C20 S1 O4 Dy1 -139.2(5) . . . . ?
O9 S2 O7 Dy1 31.6(9) . . . . ?
O8 S2 O7 Dy1 -103.8(8) . . . . ?
C21 S2 O7 Dy1 144.5(8) . . . . ?
Dy1 O1 C11 N3 -6.7(10) . . . . ?
Dy1 O1 C11 C12 173.7(5) . . . . ?
N2 N3 C11 O1 -2.1(10) . . . . ?
N2 N3 C11 C12 177.6(6) . . . . ?
O1 C11 C12 C17 -6.8(11) . . . . ?
N3 C11 C12 C17 173.5(7) . . . . ?
O1 C11 C12 C13 174.4(8) . . . . ?
N3 C11 C12 C13 -5.2(11) . . . . ?
Dy1 O2 C1 C2 170.2(6) . . . . ?
Dy1 O2 C1 C2 -42.2(9) 3_666 . . . ?
Dy1 O2 C1 C5 -9.7(8) . . . . ?
Dy1 O2 C1 C5 137.8(5) 3_666 . . . ?
O2 C1 C2 C3 177.9(7) . . . . ?
C5 C1 C2 C3 -2.2(12) . . . . ?
C9 N1 C5 C1 -179.7(6) . . . . ?
Dy1 N1 C5 C1 5.5(8) . . . . ?
C9 N1 C5 C6 0.4(10) . . . . ?
Dy1 N1 C5 C6 -174.5(5) . . . . ?
C2 C1 C5 N1 -177.6(7) . . . . ?
O2 C1 C5 N1 2.3(9) . . . . ?
C2 C1 C5 C6 2.3(11) . . . . ?
O2 C1 C5 C6 -177.8(6) . . . . ?
C5 N1 C9 C8 0.2(10) . . . . ?
Dy1 N1 C9 C8 174.6(5) . . . . ?
C5 N1 C9 C10 -178.6(6) . . . . ?
Dy1 N1 C9 C10 -4.2(9) . . . . ?
C13 C12 C17 C16 1.0(13) . . . . ?
C11 C12 C17 C16 -177.9(8) . . . . ?
N1 C9 C8 C7 -0.2(12) . . . . ?
C10 C9 C8 C7 178.6(8) . . . . ?
N3 N2 C10 C9 -178.4(6) . . . . ?
Dy1 N2 C10 C9 -4.9(9) . . . . ?
N1 C9 C10 N2 5.7(10) . . . . ?
C8 C9 C10 N2 -173.1(7) . . . . ?
C17 C12 C13 C14 -1.3(13) . . . . ?
C11 C12 C13 C14 177.5(8) . . . . ?
C12 C13 C14 C15 0.3(15) . . . . ?
C13 C14 C15 C16 1.0(16) . . . . ?
N1 C5 C6 C7 -1.0(11) . . . . ?
C1 C5 C6 C7 179.1(7) . . . . ?
N1 C5 C6 C4 179.0(7) . . . . ?
C1 C5 C6 C4 -1.0(11) . . . . ?
Dy1 O3 C18 C19 146.9(8) . . . . ?
C9 C8 C7 C6 -0.5(13) . . . . ?
C5 C6 C7 C8 1.1(12) . . . . ?
C4 C6 C7 C8 -178.9(8) . . . . ?
O9 S2 C21 F1 -178.6(9) . . . . ?
O8 S2 C21 F1 -54.5(10) . . . . ?
O7 S2 C21 F1 61.9(10) . . . . ?
O9 S2 C21 F2 57.0(10) . . . . ?
O8 S2 C21 F2 -178.9(8) . . . . ?
O7 S2 C21 F2 -62.5(10) . . . . ?
O9 S2 C21 F3 -59.8(9) . . . . ?
O8 S2 C21 F3 64.3(9) . . . . ?
O7 S2 C21 F3 -179.3(8) . . . . ?
C1 C2 C3 C4 0.7(14) . . . . ?
C14 C15 C16 C17 -1.3(16) . . . . ?
C12 C17 C16 C15 0.3(14) . . . . ?
O6 S1 C20 F4 62.1(9) . . . . ?
O5 S1 C20 F4 -177.6(8) . . . . ?
O4 S1 C20 F4 -58.7(9) . . . . ?
O6 S1 C20 F6 -177.6(7) . . . . ?
O5 S1 C20 F6 -57.3(8) . . . . ?
O4 S1 C20 F6 61.6(8) . . . . ?
O6 S1 C20 F5 -58.4(8) . . . . ?
O5 S1 C20 F5 61.9(8) . . . . ?
O4 S1 C20 F5 -179.2(7) . . . . ?
C2 C3 C4 C6 0.7(13) . . . . ?
C7 C6 C4 C3 179.4(8) . . . . ?
C5 C6 C4 C3 -0.5(12) . . . . ?
_refine_diff_density_max 1.949
_refine_diff_density_min -1.473
_refine_diff_density_rms 0.154
_shelx_res_file
;
exp_13444.res created by SHELXL-2014/7
TITL exp_13444_a.res in P2(1)/n
REM Old TITL exp_13444 in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.189, Rweak 0.059, Alpha 0.066, Orientation as input
REM Formula found by SHELXT: C29 N9 Dy O1
CELL 0.71073 11.5623 11.9207 19.8775 90 96.515 90
ZERR 2 0.0012 0.0013 0.0027 0 0.012 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Dy F N O S
UNIT 84 68 4 24 12 36 8
L.S. 10
PLAN 20
TEMP 19.85
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
REM
REM
REM
WGHT 0.051100 3.527500
FVAR 0.23705
DY1 3 0.587884 0.452641 0.580926 11.00000 0.03336 0.03718 =
0.04471 0.00420 -0.00533 -0.00204
S1 7 0.592651 0.507604 0.761162 11.00000 0.06495 0.05256 =
0.05350 -0.00568 0.00125 -0.01045
S2 7 0.726136 0.267450 0.466547 11.00000 0.05025 0.06137 =
0.05540 -0.00081 0.00329 -0.00055
O2 6 0.401769 0.463968 0.526718 11.00000 0.03221 0.03927 =
0.04097 0.01108 -0.00443 -0.00225
O1 6 0.781619 0.482018 0.625008 11.00000 0.03456 0.03980 =
0.05517 0.00270 -0.00687 -0.00253
N1 5 0.471471 0.291293 0.604997 11.00000 0.03231 0.03860 =
0.04115 -0.00032 -0.00474 -0.00221
N3 5 0.804685 0.312420 0.670626 11.00000 0.03311 0.04105 =
0.05222 0.00748 -0.00723 0.00189
AFIX 43
H3 2 0.847327 0.260255 0.690349 11.00000 -1.20000
AFIX 0
N2 5 0.687803 0.299107 0.652782 11.00000 0.03714 0.03435 =
0.04620 0.00135 -0.00433 -0.00014
O4 6 0.536870 0.475422 0.695071 11.00000 0.05686 0.04326 =
0.05419 -0.00940 0.00323 -0.00120
O3 6 0.567535 0.649328 0.598258 11.00000 0.04744 0.03278 =
0.08050 0.00638 -0.01493 -0.00912
O8 6 0.666784 0.259818 0.399701 11.00000 0.07145 0.09539 =
0.05859 -0.00414 -0.00155 -0.00401
F2 4 0.799138 0.120514 0.556791 11.00000 0.18966 0.09418 =
0.10742 0.01153 -0.02695 0.06533
O7 6 0.650737 0.310155 0.514149 11.00000 0.09723 0.06061 =
0.05834 0.00740 0.01984 0.02990
C11 1 0.848079 0.411351 0.655471 11.00000 0.02953 0.04541 =
0.04543 -0.00368 -0.00328 0.00211
F3 4 0.817114 0.070816 0.456545 11.00000 0.15353 0.10933 =
0.13907 -0.03192 0.02695 0.05939
C12 1 0.972684 0.436223 0.674999 11.00000 0.03206 0.05465 =
0.04609 -0.00555 0.00130 0.00076
C1 1 0.318151 0.389117 0.541051 11.00000 0.03988 0.03926 =
0.04272 0.00181 0.00246 -0.00209
F5 4 0.571641 0.426966 0.880495 11.00000 0.11604 0.15088 =
0.05079 0.01127 -0.00543 -0.03251
C2 1 0.202580 0.397436 0.519382 11.00000 0.03984 0.05357 =
0.05311 0.01201 -0.01005 -0.00477
AFIX 43
H2 2 0.175311 0.459288 0.493818 11.00000 -1.20000
AFIX 0
O5 6 0.715694 0.482592 0.771974 11.00000 0.05481 0.11371 =
0.08366 -0.01971 -0.00220 -0.00114
C5 1 0.357285 0.296384 0.581825 11.00000 0.03599 0.03843 =
0.04070 -0.00344 -0.00083 -0.00255
C9 1 0.511461 0.204998 0.643258 11.00000 0.04292 0.03802 =
0.04090 0.00297 -0.00004 -0.00205
F6 4 0.559455 0.308105 0.803357 11.00000 0.21311 0.06602 =
0.10553 0.01998 0.03459 -0.00307
C17 1 1.015713 0.533941 0.652537 11.00000 0.04012 0.07629 =
0.05023 0.01638 -0.00317 -0.01155
AFIX 43
H17 2 0.966552 0.583668 0.627101 11.00000 -1.20000
AFIX 0
O9 6 0.838295 0.315494 0.472987 11.00000 0.05113 0.11560 =
0.12456 0.01343 -0.00760 -0.01603
C8 1 0.438302 0.117812 0.660371 11.00000 0.05889 0.03939 =
0.05353 0.00799 -0.00656 -0.00470
AFIX 43
H8 2 0.468048 0.058128 0.687079 11.00000 -1.20000
AFIX 0
C10 1 0.636575 0.209547 0.666945 11.00000 0.03913 0.04537 =
0.05111 0.01096 -0.00259 0.00304
AFIX 43
H10 2 0.675394 0.150858 0.690648 11.00000 -1.20000
AFIX 0
O6 6 0.562216 0.613316 0.783204 11.00000 0.12856 0.04528 =
0.08018 -0.00981 -0.00363 -0.00293
C13 1 1.046537 0.363679 0.713714 11.00000 0.04476 0.05899 =
0.08193 -0.00537 -0.01563 0.00624
AFIX 43
H13 2 1.017918 0.297385 0.730121 11.00000 -1.20000
AFIX 0
C14 1 1.161819 0.390292 0.727615 11.00000 0.03935 0.07677 =
0.10289 -0.00585 -0.01866 0.00583
AFIX 43
H14 2 1.211301 0.341318 0.753433 11.00000 -1.20000
AFIX 0
F4 4 0.420264 0.415846 0.814011 11.00000 0.06171 0.24267 =
0.11152 0.06099 0.00388 -0.03231
C15 1 1.204844 0.485544 0.704762 11.00000 0.03339 0.11749 =
0.07553 -0.01067 0.00094 -0.00919
AFIX 43
H15 2 1.283759 0.501458 0.714202 11.00000 -1.20000
AFIX 0
C6 1 0.278625 0.212040 0.597650 11.00000 0.04594 0.04567 =
0.05406 0.00219 -0.00225 -0.01072
C18 1 0.646242 0.736647 0.624180 11.00000 0.08375 0.06200 =
0.09717 -0.00520 -0.01724 -0.01310
AFIX 23
H18A 2 0.642892 0.743474 0.672547 11.00000 -1.20000
H18B 2 0.724908 0.714760 0.617448 11.00000 -1.20000
AFIX 0
C7 1 0.323359 0.122485 0.637128 11.00000 0.05677 0.04285 =
0.07206 0.00966 -0.00253 -0.01704
AFIX 43
H7 2 0.274024 0.065119 0.647746 11.00000 -1.20000
AFIX 0
F1 4 0.649284 0.069396 0.490259 11.00000 0.14052 0.07484 =
0.20333 0.02591 0.01213 -0.02250
C21 1 0.746828 0.124650 0.494964 11.00000 0.09091 0.06101 =
0.09868 -0.02156 0.00068 0.02220
C3 1 0.124765 0.315490 0.534689 11.00000 0.03329 0.07953 =
0.06718 0.01488 0.00122 -0.00796
AFIX 43
H3A 2 0.046454 0.323409 0.518647 11.00000 -1.20000
AFIX 0
C16 1 1.133250 0.559393 0.667645 11.00000 0.05694 0.10964 =
0.06239 0.01912 0.00569 -0.03069
AFIX 43
H16 2 1.162856 0.626225 0.652574 11.00000 -1.20000
AFIX 0
C20 1 0.532958 0.411072 0.817120 11.00000 0.05669 0.07215 =
0.06293 0.00298 -0.00319 -0.00951
C4 1 0.159044 0.224571 0.572136 11.00000 0.04335 0.06682 =
0.06495 0.00524 0.00235 -0.01798
AFIX 43
H4 2 0.105043 0.170428 0.581251 11.00000 -1.20000
AFIX 0
C19 1 0.622623 0.842243 0.593909 11.00000 0.11216 0.05827 =
0.12998 0.00424 -0.00821 -0.02545
AFIX 137
H19A 2 0.600787 0.832762 0.546198 11.00000 -1.50000
H19B 2 0.690911 0.888456 0.601051 11.00000 -1.50000
H19C 2 0.560074 0.877482 0.613847 11.00000 -1.50000
AFIX 0
HKLF 4
REM exp_13444_a.res in P2(1)/n
REM R1 = 0.0584 for 4129 Fo > 4sig(Fo) and 0.0952 for all 6131 data
REM 380 parameters refined using 0 restraints
END
WGHT 0.0511 3.5276
REM Highest difference peak 1.949, deepest hole -1.473, 1-sigma level 0.154
Q1 1 0.7628 0.5482 0.7425 11.00000 0.05 1.95
Q2 1 0.5530 0.3721 0.5909 11.00000 0.05 1.41
Q3 1 0.5204 0.5428 0.7593 11.00000 0.05 1.35
Q4 1 0.6188 0.5319 0.5764 11.00000 0.05 1.29
Q5 1 0.6246 0.3759 0.5799 11.00000 0.05 1.24
Q6 1 0.5525 0.5394 0.5925 11.00000 0.05 1.20
Q7 1 0.6054 0.4676 0.6281 11.00000 0.05 1.20
Q8 1 0.6085 0.5218 0.5430 11.00000 0.05 1.01
Q9 1 0.7599 0.3579 0.7403 11.00000 0.05 1.01
Q10 1 0.6038 0.3766 0.5464 11.00000 0.05 1.00
Q11 1 0.6591 0.4515 0.5547 11.00000 0.05 0.96
Q12 1 0.5655 0.4388 0.5347 11.00000 0.05 0.94
Q13 1 0.5620 0.4091 0.5487 11.00000 0.05 0.93
Q14 1 0.5427 0.5029 0.5568 11.00000 0.05 0.93
Q15 1 0.5838 0.6405 0.5799 11.00000 0.05 0.93
Q16 1 0.6575 0.5639 0.7814 11.00000 0.05 0.82
Q17 1 0.5071 0.4446 0.6123 11.00000 0.05 0.79
Q18 1 0.5044 0.6553 0.6154 11.00000 0.05 0.61
Q19 1 0.5908 0.5956 0.6267 11.00000 0.05 0.60
Q20 1 0.4402 0.5837 0.7780 11.00000 0.05 0.60
;
_shelx_res_checksum 33754