# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
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data_2
_audit_block_doi 10.5517/cc1j3ym6
_database_code_depnum_ccdc_archive 'CCDC 1403978'
_audit_update_record
;
2017-05-31 deposited with the CCDC.
2017-06-01 downloaded from the CCDC.
;
_audit_creation_date 2017-04-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C58 H46 Dy2 N12 O12, 2(C2 H3 N)'
_chemical_formula_sum 'C62 H52 Dy2 N14 O12'
_chemical_formula_weight 1510.17
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.3827(6)
_cell_length_b 11.6579(7)
_cell_length_c 13.2869(8)
_cell_angle_alpha 73.8570(10)
_cell_angle_beta 77.6560(10)
_cell_angle_gamma 83.6090(10)
_cell_volume 1506.82(16)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 3160
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 24.22
_cell_measurement_theta_min 2.64
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.536
_exptl_absorpt_correction_T_max 0.587
_exptl_absorpt_correction_T_min 0.564
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details (sadabs;bruker,2000)
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_density_diffrn 1.664
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 750
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.19
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0495
_diffrn_reflns_av_unetI/netI 0.0897
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 9592
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.079
_diffrn_reflns_theta_min 1.821
_diffrn_ambient_temperature 293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4646
_reflns_number_total 5939
_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.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_collection 'Bruker APEX2'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SHELXS-97 (Sheldrick 2008)'
_refine_diff_density_max 1.256
_refine_diff_density_min -0.805
_refine_diff_density_rms 0.153
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.045
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 358
_refine_ls_number_reflns 5939
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0705
_refine_ls_R_factor_gt 0.0499
_refine_ls_restrained_S_all 1.045
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0947
_refine_ls_wR_factor_ref 0.1053
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups, All N(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Others
Sof(H25A)=Sof(H26A)=Sof(C24A)=Sof(C29A)=Sof(H29A)=Sof(C28A)=Sof(H28A)=
Sof(C27A)=Sof(H27A)=1-FVAR(1)
Sof(C24)=Sof(H25)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=
Sof(H29)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C14(H14),
C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
C25(H25A), C26(H26), C26(H26A), C27(H27), C28(H28), C29(H29), C29A(H29A),
C28A(H28A), C27A(H27A)
3.b Fitted hexagon refined as free rotating group:
C10(C11,C12,C13,C14,C15), C17(C18,C19,C20,C21,C22), C24(C25,C26,C27,C28,C29)
3.c X=CH2 refined with riding coordinates:
N3(H3A,H3B), N5(H5A,H5B)
3.d Idealised Me refined as rotating group:
C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7504(7) -0.1033(7) 0.5453(5) 0.0447(18) Uani 1 1 d . . . . .
H1 H 0.8252 -0.0869 0.5657 0.054 Uiso 1 1 calc R . . . .
C2 C 0.6458(7) -0.1488(7) 0.6236(5) 0.049(2) Uani 1 1 d . . . . .
H2 H 0.6494 -0.1624 0.6953 0.059 Uiso 1 1 calc R . . . .
C3 C 0.5366(7) -0.1735(8) 0.5939(6) 0.060(2) Uani 1 1 d . . . . .
H3 H 0.4646 -0.2053 0.6453 0.072 Uiso 1 1 calc R . . . .
C4 C 0.5337(7) -0.1507(7) 0.4856(5) 0.050(2) Uani 1 1 d . . . . .
H4 H 0.4603 -0.1674 0.4636 0.060 Uiso 1 1 calc R . . . .
C5 C 0.6410(6) -0.1032(6) 0.4126(5) 0.0312(15) Uani 1 1 d . . . . .
C6 C 0.6379(6) -0.0668(5) 0.2963(5) 0.0281(14) Uani 1 1 d . . . . .
C7 C 0.5224(6) -0.0506(6) 0.1671(5) 0.0316(15) Uani 1 1 d . . . . .
C8 C 0.7312(6) 0.0102(5) 0.1235(5) 0.0298(14) Uani 1 1 d . . . . .
C9 C 1.1153(6) 0.1385(6) 0.1542(5) 0.0327(15) Uani 1 1 d . . . . .
C10 C 1.2033(4) 0.2038(4) 0.0565(3) 0.0305(14) Uani 1 1 d . . . . .
C11 C 1.1608(3) 0.2400(4) -0.0405(3) 0.0379(16) Uani 1 1 d G . . . .
H11 H 1.0751 0.2272 -0.0436 0.045 Uiso 1 1 calc R . . . .
C12 C 1.2464(4) 0.2954(4) -0.1328(3) 0.0473(19) Uani 1 1 d G . . . .
H12 H 1.2180 0.3196 -0.1976 0.057 Uiso 1 1 calc R . . . .
C13 C 1.3745(4) 0.3145(4) -0.1281(3) 0.0475(19) Uani 1 1 d G . . . .
H13 H 1.4318 0.3516 -0.1898 0.057 Uiso 1 1 calc R . . . .
C14 C 1.4170(3) 0.2783(4) -0.0311(3) 0.0443(18) Uani 1 1 d G . . . .
H14 H 1.5027 0.2912 -0.0279 0.053 Uiso 1 1 calc R . . . .
C15 C 1.3314(4) 0.2230(4) 0.0612(3) 0.0370(16) Uani 1 1 d G . . . .
H15 H 1.3598 0.1988 0.1261 0.044 Uiso 1 1 calc R . . . .
C16 C 1.0419(7) -0.2283(6) 0.2426(5) 0.0340(15) Uani 1 1 d . . . . .
C17 C 1.1050(5) -0.3450(3) 0.2270(4) 0.0380(16) Uani 1 1 d . . . . .
C18 C 1.2345(5) -0.3520(4) 0.1725(4) 0.057(2) Uani 1 1 d G . . . .
H18 H 1.2804 -0.2828 0.1411 0.068 Uiso 1 1 calc R . . . .
C19 C 1.2954(4) -0.4624(5) 0.1647(4) 0.072(3) Uani 1 1 d G . . . .
H19 H 1.3821 -0.4671 0.1282 0.086 Uiso 1 1 calc R . . . .
C20 C 1.2268(6) -0.5658(3) 0.2115(5) 0.063(2) Uani 1 1 d G . . . .
H20 H 1.2676 -0.6397 0.2063 0.076 Uiso 1 1 calc R . . . .
C21 C 1.0973(6) -0.5588(3) 0.2661(5) 0.078(3) Uani 1 1 d G . . . .
H21 H 1.0514 -0.6280 0.2974 0.094 Uiso 1 1 calc R . . . .
C22 C 1.0364(4) -0.4484(4) 0.2738(4) 0.061(2) Uani 1 1 d G . . . .
H22 H 0.9497 -0.4437 0.3103 0.073 Uiso 1 1 calc R . . . .
C23 C 0.8928(6) 0.1691(6) 0.4743(5) 0.0331(15) Uani 1 1 d . . . . .
C24 C 0.7934(10) 0.2736(7) 0.4732(7) 0.030(6) Uiso 0.379(17) 1 d . . P A 1
C25 C 0.7488(6) 0.3302(5) 0.3791(5) 0.0509(19) Uiso 1 1 d G . . . .
H25 H 0.7677 0.2954 0.3222 0.061 Uiso 0.379(17) 1 calc R . P A 1
H25A H 0.7473 0.2831 0.3333 0.061 Uiso 0.621(17) 1 calc R . P A 2
C26 C 0.6759(7) 0.4389(5) 0.3701(5) 0.066(2) Uiso 1 1 d G . . . .
H26 H 0.6461 0.4768 0.3072 0.079 Uiso 0.379(17) 1 calc R . P A 1
H26A H 0.6226 0.4640 0.3191 0.079 Uiso 0.621(17) 1 calc R . P A 2
C27 C 0.6476(12) 0.4909(8) 0.4552(8) 0.087(13) Uiso 0.379(17) 1 d G . P A 1
H27 H 0.5989 0.5636 0.4492 0.104 Uiso 0.379(17) 1 calc R . P A 1
C28 C 0.6922(17) 0.4343(12) 0.5493(8) 0.059(7) Uiso 0.379(17) 1 d G . P A 1
H28 H 0.6733 0.4692 0.6062 0.071 Uiso 0.379(17) 1 calc R . P A 1
C29 C 0.7651(16) 0.3257(12) 0.5582(7) 0.044(6) Uiso 0.379(17) 1 d G . P A 1
H29 H 0.7949 0.2878 0.6212 0.053 Uiso 0.379(17) 1 calc R . P A 1
C30 C 0.8381(10) 0.4049(9) 0.0738(9) 0.093(3) Uani 1 1 d . . . . .
H30A H 0.8312 0.4880 0.0728 0.140 Uiso 1 1 calc GR . . . .
H30B H 0.8721 0.3967 0.0029 0.140 Uiso 1 1 calc GR . . . .
H30C H 0.8968 0.3623 0.1203 0.140 Uiso 1 1 calc GR . . . .
C31 C 0.7103(13) 0.3569(10) 0.1118(8) 0.081(3) Uani 1 1 d . . . . .
Dy1 Dy 0.95526(3) -0.02402(3) 0.31003(2) 0.02841(11) Uani 1 1 d . . . . .
N1 N 0.7501(5) -0.0815(5) 0.4411(4) 0.0319(12) Uani 1 1 d . . . . .
N2 N 0.5261(5) -0.0863(5) 0.2726(4) 0.0328(13) Uani 1 1 d . . . . .
N3 N 0.4106(5) -0.0655(5) 0.1407(4) 0.0394(14) Uani 1 1 d . . . . .
H3A H 0.4027 -0.0442 0.0748 0.047 Uiso 1 1 calc R . . . .
H3B H 0.3458 -0.0965 0.1894 0.047 Uiso 1 1 calc R . . . .
N4 N 0.6222(5) -0.0024(4) 0.0907(4) 0.0304(12) Uani 1 1 d . . . . .
N5 N 0.8326(5) 0.0534(5) 0.0494(4) 0.0420(15) Uani 1 1 d . . . . .
H5A H 0.8267 0.0721 -0.0168 0.050 Uiso 1 1 calc R . . . .
H5B H 0.9048 0.0629 0.0672 0.050 Uiso 1 1 calc R . . . .
N6 N 0.7459(5) -0.0194(4) 0.2290(4) 0.0276(12) Uani 1 1 d . . . . .
N7 N 0.6123(11) 0.3164(11) 0.1433(8) 0.117(4) Uani 1 1 d . . . . .
O1 O 1.1580(4) 0.0892(4) 0.2385(3) 0.0381(11) Uani 1 1 d . . . . .
O2 O 0.9947(4) 0.1304(4) 0.1515(3) 0.0369(11) Uani 1 1 d . . . . .
O3 O 0.9341(4) -0.2267(4) 0.3063(4) 0.0430(12) Uani 1 1 d . . . . .
O4 O 1.0999(5) -0.1327(4) 0.1957(3) 0.0420(12) Uani 1 1 d . . . . .
O5 O 0.9085(4) 0.1230(4) 0.3978(3) 0.0373(11) Uani 1 1 d . . . . .
O6 O 1.0638(4) -0.1248(4) 0.4422(3) 0.0443(12) Uani 1 1 d . . . . .
C24A C 0.8237(13) 0.2941(11) 0.4582(9) 0.030(3) Uiso 0.621(17) 1 d . . P A 2
C29A C 0.8321(14) 0.3663(12) 0.5214(11) 0.056(4) Uiso 0.621(17) 1 d . . P A 2
H29A H 0.8852 0.3425 0.5727 0.067 Uiso 0.621(17) 1 calc R . P A 2
C28A C 0.7584(16) 0.4794(14) 0.5081(13) 0.075(5) Uiso 0.621(17) 1 d . . P A 2
H28A H 0.7635 0.5310 0.5492 0.090 Uiso 0.621(17) 1 calc R . P A 2
C27A C 0.6822(18) 0.5076(14) 0.4347(13) 0.065(5) Uiso 0.621(17) 1 d . . P A 2
H27A H 0.6306 0.5788 0.4279 0.078 Uiso 0.621(17) 1 calc R . P 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
C1 0.034(4) 0.074(5) 0.028(4) -0.014(4) -0.010(3) -0.002(4)
C2 0.052(5) 0.075(6) 0.021(3) -0.012(3) -0.008(3) -0.010(4)
C3 0.045(5) 0.095(7) 0.034(4) -0.002(4) -0.003(3) -0.028(5)
C4 0.041(4) 0.082(6) 0.025(4) -0.006(4) -0.002(3) -0.028(4)
C5 0.029(4) 0.041(4) 0.024(3) -0.009(3) -0.005(3) 0.000(3)
C6 0.022(3) 0.038(4) 0.026(3) -0.011(3) -0.007(3) 0.004(3)
C7 0.027(4) 0.041(4) 0.031(3) -0.015(3) -0.012(3) 0.008(3)
C8 0.029(4) 0.035(4) 0.025(3) -0.008(3) -0.003(3) -0.005(3)
C9 0.036(4) 0.039(4) 0.030(3) -0.016(3) -0.015(3) 0.003(3)
C10 0.032(4) 0.028(3) 0.032(3) -0.013(3) -0.001(3) 0.004(3)
C11 0.036(4) 0.043(4) 0.033(4) -0.006(3) -0.007(3) -0.003(3)
C12 0.052(5) 0.052(5) 0.032(4) 0.001(3) -0.013(3) -0.001(4)
C13 0.044(5) 0.053(5) 0.036(4) -0.006(3) 0.002(3) 0.000(4)
C14 0.030(4) 0.047(4) 0.055(5) -0.016(4) 0.002(3) -0.009(3)
C15 0.032(4) 0.045(4) 0.035(4) -0.014(3) -0.006(3) -0.002(3)
C16 0.033(4) 0.042(4) 0.030(4) -0.012(3) -0.009(3) -0.004(3)
C17 0.048(5) 0.036(4) 0.034(4) -0.013(3) -0.014(3) 0.001(3)
C18 0.066(6) 0.041(4) 0.055(5) -0.017(4) 0.010(4) 0.001(4)
C19 0.081(7) 0.052(5) 0.075(6) -0.024(5) 0.011(5) -0.002(5)
C20 0.083(7) 0.039(5) 0.065(6) -0.019(4) -0.009(5) 0.015(5)
C21 0.080(7) 0.039(5) 0.109(8) -0.019(5) -0.005(6) -0.005(5)
C22 0.050(5) 0.042(5) 0.086(6) -0.013(4) -0.007(4) -0.005(4)
C23 0.027(4) 0.046(4) 0.027(3) -0.008(3) -0.006(3) -0.007(3)
C30 0.092(8) 0.095(8) 0.100(9) -0.039(7) -0.018(7) 0.002(7)
C31 0.105(10) 0.084(8) 0.059(7) -0.024(6) -0.025(6) -0.003(7)
Dy1 0.02622(19) 0.03997(19) 0.01983(15) -0.00868(12) -0.00590(11) -0.00005(13)
N1 0.033(3) 0.047(3) 0.019(3) -0.009(2) -0.009(2) -0.004(3)
N2 0.026(3) 0.050(3) 0.024(3) -0.011(2) -0.007(2) -0.003(3)
N3 0.028(3) 0.062(4) 0.030(3) -0.010(3) -0.011(2) -0.006(3)
N4 0.030(3) 0.040(3) 0.024(3) -0.006(2) -0.011(2) -0.007(3)
N5 0.036(3) 0.070(4) 0.021(3) -0.004(3) -0.007(2) -0.021(3)
N6 0.028(3) 0.037(3) 0.017(2) -0.006(2) -0.005(2) -0.001(2)
N7 0.126(9) 0.161(11) 0.067(6) -0.020(6) -0.018(6) -0.039(8)
O1 0.036(3) 0.056(3) 0.024(2) -0.006(2) -0.0109(19) -0.009(2)
O2 0.032(3) 0.046(3) 0.031(2) -0.001(2) -0.010(2) -0.010(2)
O3 0.030(3) 0.049(3) 0.049(3) -0.015(2) -0.001(2) -0.004(2)
O4 0.055(3) 0.037(3) 0.030(2) -0.010(2) 0.006(2) -0.008(2)
O5 0.044(3) 0.044(3) 0.031(2) -0.020(2) -0.010(2) 0.005(2)
O6 0.047(3) 0.056(3) 0.031(3) -0.009(2) -0.019(2) 0.013(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9300 . ?
C1 C2 1.372(9) . ?
C1 N1 1.337(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.361(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.395(9) . ?
C4 H4 0.9300 . ?
C4 C5 1.366(8) . ?
C5 C6 1.490(8) . ?
C5 N1 1.338(7) . ?
C6 N2 1.325(7) . ?
C6 N6 1.340(7) . ?
C7 N2 1.355(7) . ?
C7 N3 1.325(7) . ?
C7 N4 1.334(8) . ?
C8 N4 1.333(7) . ?
C8 N5 1.315(7) . ?
C8 N6 1.385(7) . ?
C9 C10 1.482(7) . ?
C9 Dy1 2.773(7) . ?
C9 O1 1.256(7) . ?
C9 O2 1.276(7) . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 H11 0.9300 . ?
C11 C12 1.3900 . ?
C12 H12 0.9300 . ?
C12 C13 1.3900 . ?
C13 H13 0.9300 . ?
C13 C14 1.3900 . ?
C14 H14 0.9300 . ?
C14 C15 1.3900 . ?
C15 H15 0.9300 . ?
C16 C17 1.490(7) . ?
C16 Dy1 2.766(7) . ?
C16 O3 1.253(7) . ?
C16 O4 1.264(7) . ?
C17 C18 1.3900 . ?
C17 C22 1.3900 . ?
C18 H18 0.9300 . ?
C18 C19 1.3900 . ?
C19 H19 0.9300 . ?
C19 C20 1.3900 . ?
C20 H20 0.9300 . ?
C20 C21 1.3900 . ?
C21 H21 0.9300 . ?
C21 C22 1.3900 . ?
C22 H22 0.9300 . ?
C23 C24 1.506(9) . ?
C23 O5 1.250(7) . ?
C23 O6 1.242(7) 2_756 ?
C23 C24A 1.531(12) . ?
C24 C25 1.3900 . ?
C24 C29 1.3900 . ?
C25 H25 0.9300 . ?
C25 H25A 0.9300 . ?
C25 C26 1.3900 . ?
C25 C24A 1.385(12) . ?
C26 H26 0.9300 . ?
C26 H26A 0.9300 . ?
C26 C27 1.3900 . ?
C26 C27A 1.341(15) . ?
C27 H27 0.9300 . ?
C27 C28 1.3900 . ?
C28 H28 0.9300 . ?
C28 C29 1.3900 . ?
C29 H29 0.9300 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C30 C31 1.432(14) . ?
C31 N7 1.117(13) . ?
Dy1 N1 2.470(5) . ?
Dy1 N6 2.613(5) . ?
Dy1 O1 2.478(4) . ?
Dy1 O2 2.352(4) . ?
Dy1 O3 2.412(5) . ?
Dy1 O4 2.416(4) . ?
Dy1 O5 2.284(4) . ?
Dy1 O6 2.267(4) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
O6 C23 1.242(7) 2_756 ?
C24A C29A 1.365(15) . ?
C29A H29A 0.9300 . ?
C29A C28A 1.435(17) . ?
C28A H28A 0.9300 . ?
C28A C27A 1.334(18) . ?
C27A H27A 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
C2 C1 H1 118.4 . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.2(6) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 C1 118.5(6) . . ?
C3 C2 H2 120.8 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.4(7) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 120.7 . . ?
C5 C4 C3 118.5(6) . . ?
C5 C4 H4 120.7 . . ?
C4 C5 C6 120.5(6) . . ?
N1 C5 C4 122.5(6) . . ?
N1 C5 C6 116.9(5) . . ?
N2 C6 C5 114.5(5) . . ?
N2 C6 N6 127.9(5) . . ?
N6 C6 C5 117.6(5) . . ?
N3 C7 N2 116.0(6) . . ?
N3 C7 N4 119.5(6) . . ?
N4 C7 N2 124.5(6) . . ?
N4 C8 N6 125.0(5) . . ?
N5 C8 N4 117.1(5) . . ?
N5 C8 N6 117.9(5) . . ?
C10 C9 Dy1 166.4(4) . . ?
O1 C9 C10 121.3(5) . . ?
O1 C9 Dy1 63.3(3) . . ?
O1 C9 O2 119.6(6) . . ?
O2 C9 C10 119.1(5) . . ?
O2 C9 Dy1 57.7(3) . . ?
C11 C10 C9 120.4(3) . . ?
C11 C10 C15 120.0 . . ?
C15 C10 C9 119.5(3) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C10 C15 H15 120.0 . . ?
C14 C15 C10 120.0 . . ?
C14 C15 H15 120.0 . . ?
C17 C16 Dy1 166.9(4) . . ?
O3 C16 C17 119.4(6) . . ?
O3 C16 Dy1 60.6(3) . . ?
O3 C16 O4 120.4(6) . . ?
O4 C16 C17 120.1(5) . . ?
O4 C16 Dy1 60.8(3) . . ?
C18 C17 C16 120.5(4) . . ?
C18 C17 C22 120.0 . . ?
C22 C17 C16 119.4(4) . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C19 C20 H20 120.0 . . ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C20 C21 H21 120.0 . . ?
C20 C21 C22 120.0 . . ?
C22 C21 H21 120.0 . . ?
C17 C22 H22 120.0 . . ?
C21 C22 C17 120.0 . . ?
C21 C22 H22 120.0 . . ?
O5 C23 C24 116.6(6) . . ?
O5 C23 C24A 116.2(6) . . ?
O6 C23 C24 117.4(6) 2_756 . ?
O6 C23 O5 125.0(6) 2_756 . ?
O6 C23 C24A 118.6(6) 2_756 . ?
C25 C24 C23 119.0(6) . . ?
C25 C24 C29 120.0 . . ?
C29 C24 C23 120.0(6) . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 120.0 . . ?
C26 C25 H25 120.0 . . ?
C26 C25 H25A 120.9 . . ?
C24A C25 H25A 120.9 . . ?
C24A C25 C26 118.1(7) . . ?
C25 C26 H26 120.0 . . ?
C25 C26 H26A 119.9 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26 120.0 . . ?
C27A C26 C25 120.3(8) . . ?
C27A C26 H26A 119.9 . . ?
C26 C27 H27 120.0 . . ?
C26 C27 C28 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 120.0 . . ?
C27 C28 C29 120.0 . . ?
C29 C28 H28 120.0 . . ?
C24 C29 H29 120.0 . . ?
C28 C29 C24 120.0 . . ?
C28 C29 H29 120.0 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C31 C30 H30C 109.5 . . ?
N7 C31 C30 177.9(14) . . ?
C16 Dy1 C9 99.24(19) . . ?
N1 Dy1 C9 153.40(18) . . ?
N1 Dy1 C16 103.77(18) . . ?
N1 Dy1 N6 64.54(15) . . ?
N1 Dy1 O1 153.14(16) . . ?
N6 Dy1 C9 103.96(16) . . ?
N6 Dy1 C16 87.06(17) . . ?
O1 Dy1 C9 26.94(15) . . ?
O1 Dy1 C16 99.31(17) . . ?
O1 Dy1 N6 130.88(14) . . ?
O2 Dy1 C9 27.28(15) . . ?
O2 Dy1 C16 103.30(17) . . ?
O2 Dy1 N1 131.21(16) . . ?
O2 Dy1 N6 77.24(14) . . ?
O2 Dy1 O1 53.81(14) . . ?
O2 Dy1 O3 121.19(16) . . ?
O2 Dy1 O4 80.38(15) . . ?
O3 Dy1 C9 124.73(17) . . ?
O3 Dy1 C16 26.90(16) . . ?
O3 Dy1 N1 76.93(16) . . ?
O3 Dy1 N6 73.86(15) . . ?
O3 Dy1 O1 125.72(15) . . ?
O3 Dy1 O4 53.78(15) . . ?
O4 Dy1 C9 72.20(16) . . ?
O4 Dy1 C16 27.17(16) . . ?
O4 Dy1 N1 130.64(16) . . ?
O4 Dy1 N6 96.05(16) . . ?
O4 Dy1 O1 74.03(15) . . ?
O5 Dy1 C9 85.49(16) . . ?
O5 Dy1 C16 166.58(17) . . ?
O5 Dy1 N1 75.14(16) . . ?
O5 Dy1 N6 104.08(15) . . ?
O5 Dy1 O1 79.20(15) . . ?
O5 Dy1 O2 86.68(15) . . ?
O5 Dy1 O3 149.64(16) . . ?
O5 Dy1 O4 153.02(16) . . ?
O6 Dy1 C9 110.91(17) . . ?
O6 Dy1 C16 80.14(17) . . ?
O6 Dy1 N1 86.27(16) . . ?
O6 Dy1 N6 144.29(16) . . ?
O6 Dy1 O1 84.30(15) . . ?
O6 Dy1 O2 138.10(16) . . ?
O6 Dy1 O3 80.06(16) . . ?
O6 Dy1 O4 87.56(16) . . ?
O6 Dy1 O5 86.44(16) . . ?
C1 N1 C5 117.9(5) . . ?
C1 N1 Dy1 119.5(4) . . ?
C5 N1 Dy1 122.3(4) . . ?
C6 N2 C7 114.4(5) . . ?
C7 N3 H3A 120.0 . . ?
C7 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C8 N4 C7 116.0(5) . . ?
C8 N5 H5A 120.0 . . ?
C8 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C6 N6 C8 112.1(5) . . ?
C6 N6 Dy1 117.0(4) . . ?
C8 N6 Dy1 130.2(4) . . ?
C9 O1 Dy1 89.7(4) . . ?
C9 O2 Dy1 95.1(4) . . ?
C16 O3 Dy1 92.5(4) . . ?
C16 O4 Dy1 92.0(4) . . ?
C23 O5 Dy1 157.5(4) . . ?
C23 O6 Dy1 168.6(4) 2_756 . ?
C25 C24A C23 117.6(8) . . ?
C29A C24A C23 121.4(9) . . ?
C29A C24A C25 120.9(10) . . ?
C24A C29A H29A 120.3 . . ?
C24A C29A C28A 119.4(13) . . ?
C28A C29A H29A 120.3 . . ?
C29A C28A H28A 121.2 . . ?
C27A C28A C29A 117.5(14) . . ?
C27A C28A H28A 121.2 . . ?
C26 C27A H27A 118.2 . . ?
C28A C27A C26 123.6(14) . . ?
C28A C27A H27A 118.2 . . ?
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
C1 C2 C3 C4 -0.8(13) . . . . ?
C2 C1 N1 C5 1.3(11) . . . . ?
C2 C1 N1 Dy1 -172.3(6) . . . . ?
C2 C3 C4 C5 -0.4(13) . . . . ?
C3 C4 C5 C6 -174.3(7) . . . . ?
C3 C4 C5 N1 2.2(12) . . . . ?
C4 C5 C6 N2 -1.0(9) . . . . ?
C4 C5 C6 N6 179.2(6) . . . . ?
C4 C5 N1 C1 -2.6(10) . . . . ?
C4 C5 N1 Dy1 170.8(5) . . . . ?
C5 C6 N2 C7 178.6(5) . . . . ?
C5 C6 N6 C8 179.7(5) . . . . ?
C5 C6 N6 Dy1 7.7(7) . . . . ?
C6 C5 N1 C1 174.0(6) . . . . ?
C6 C5 N1 Dy1 -12.6(8) . . . . ?
C9 C10 C11 C12 -176.5(4) . . . . ?
C9 C10 C15 C14 176.5(4) . . . . ?
C10 C9 O1 Dy1 -165.3(5) . . . . ?
C10 C9 O2 Dy1 164.6(4) . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C10 C15 C14 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 C10 0.0 . . . . ?
C15 C10 C11 C12 0.0 . . . . ?
C16 C17 C18 C19 175.5(5) . . . . ?
C16 C17 C22 C21 -175.6(5) . . . . ?
C17 C16 O3 Dy1 164.9(5) . . . . ?
C17 C16 O4 Dy1 -164.9(5) . . . . ?
C17 C18 C19 C20 0.0 . . . . ?
C18 C17 C22 C21 0.0 . . . . ?
C18 C19 C20 C21 0.0 . . . . ?
C19 C20 C21 C22 0.0 . . . . ?
C20 C21 C22 C17 0.0 . . . . ?
C22 C17 C18 C19 0.0 . . . . ?
C23 C24 C25 C26 -168.6(9) . . . . ?
C23 C24 C29 C28 168.4(9) . . . . ?
C23 C24A C29A C28A -175.7(11) . . . . ?
C24 C23 O5 Dy1 -150.0(10) . . . . ?
C24 C25 C26 C27 0.0 . . . . ?
C25 C24 C29 C28 0.0 . . . . ?
C25 C26 C27 C28 0.0 . . . . ?
C25 C26 C27A C28A 2(2) . . . . ?
C25 C24A C29A C28A 2(2) . . . . ?
C26 C25 C24A C23 174.2(7) . . . . ?
C26 C25 C24A C29A -3.9(16) . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
C27 C28 C29 C24 0.0 . . . . ?
C29 C24 C25 C26 0.0 . . . . ?
Dy1 C9 C10 C11 62.7(18) . . . . ?
Dy1 C9 C10 C15 -113.8(16) . . . . ?
Dy1 C16 C17 C18 -82.0(19) . . . . ?
Dy1 C16 C17 C22 93.6(19) . . . . ?
N1 C1 C2 C3 0.4(12) . . . . ?
N1 C5 C6 N2 -177.7(6) . . . . ?
N1 C5 C6 N6 2.4(9) . . . . ?
N2 C6 N6 C8 -0.1(9) . . . . ?
N2 C6 N6 Dy1 -172.1(5) . . . . ?
N2 C7 N4 C8 -0.1(9) . . . . ?
N3 C7 N2 C6 -178.1(5) . . . . ?
N3 C7 N4 C8 179.7(6) . . . . ?
N4 C7 N2 C6 1.7(9) . . . . ?
N4 C8 N6 C6 2.0(9) . . . . ?
N4 C8 N6 Dy1 172.6(4) . . . . ?
N5 C8 N4 C7 177.5(6) . . . . ?
N5 C8 N6 C6 -177.4(6) . . . . ?
N5 C8 N6 Dy1 -6.8(8) . . . . ?
N6 C6 N2 C7 -1.6(9) . . . . ?
N6 C8 N4 C7 -1.9(9) . . . . ?
O1 C9 C10 C11 168.9(5) . . . . ?
O1 C9 C10 C15 -7.6(7) . . . . ?
O1 C9 O2 Dy1 -13.9(6) . . . . ?
O2 C9 C10 C11 -9.6(7) . . . . ?
O2 C9 C10 C15 174.0(4) . . . . ?
O2 C9 O1 Dy1 13.1(6) . . . . ?
O3 C16 C17 C18 -168.2(5) . . . . ?
O3 C16 C17 C22 7.3(7) . . . . ?
O3 C16 O4 Dy1 11.7(6) . . . . ?
O4 C16 C17 C18 8.4(8) . . . . ?
O4 C16 C17 C22 -176.0(5) . . . . ?
O4 C16 O3 Dy1 -11.7(6) . . . . ?
O5 C23 C24 C25 -14.9(11) . . . . ?
O5 C23 C24 C29 176.6(6) . . . . ?
O5 C23 C24A C25 19.9(14) . . . . ?
O5 C23 C24A C29A -162.0(10) . . . . ?
O6 C23 C24 C25 176.0(6) 2_756 . . . ?
O6 C23 C24 C29 7.5(8) 2_756 . . . ?
O6 C23 O5 Dy1 18.1(15) 2_756 . . . ?
O6 C23 C24A C25 -164.7(8) 2_756 . . . ?
O6 C23 C24A C29A 13.4(16) 2_756 . . . ?
C24A C23 O5 Dy1 -166.9(10) . . . . ?
C24A C25 C26 C27A 2.0(15) . . . . ?
C24A C29A C28A C27A 1(2) . . . . ?
C29A C28A C27A C26 -3(3) . . . . ?
_iucr_refine_instructions_details
;
1.res created by SHELXL-2014/7
TITL 1 in P1 New: P-1
CELL 0.71073 10.3827 11.6579 13.2869 73.857 77.656 83.609
ZERR 1 0.0006 0.0007 0.0008 0.001 0.001 0.001
LATT 1
SFAC C H Dy N O
UNIT 62 52 2 14 12
L.S. 50
PLAN 30
BOND $H
CONF
fmap 2
acta
REM
REM
REM
WGHT 0.037600
FVAR 0.12738 0.37872
C1 1 0.750418 -0.103319 0.545321 11.00000 0.03410 0.07429 =
0.02817 -0.01440 -0.01012 -0.00207
AFIX 43
H1 2 0.825197 -0.086883 0.565716 11.00000 -1.20000
AFIX 0
C2 1 0.645803 -0.148780 0.623609 11.00000 0.05239 0.07525 =
0.02114 -0.01224 -0.00769 -0.00951
AFIX 43
H2 2 0.649409 -0.162393 0.695345 11.00000 -1.20000
AFIX 0
C3 1 0.536603 -0.173503 0.593883 11.00000 0.04528 0.09504 =
0.03351 -0.00220 -0.00257 -0.02824
AFIX 43
H3 2 0.464628 -0.205324 0.645265 11.00000 -1.20000
AFIX 0
C4 1 0.533682 -0.150651 0.485587 11.00000 0.04129 0.08155 =
0.02510 -0.00619 -0.00173 -0.02790
AFIX 43
H4 2 0.460252 -0.167363 0.463571 11.00000 -1.20000
AFIX 0
C5 1 0.641037 -0.103191 0.412588 11.00000 0.02854 0.04122 =
0.02354 -0.00878 -0.00523 0.00014
C6 1 0.637928 -0.066764 0.296315 11.00000 0.02178 0.03767 =
0.02594 -0.01078 -0.00653 0.00394
C7 1 0.522429 -0.050569 0.167056 11.00000 0.02682 0.04083 =
0.03104 -0.01474 -0.01167 0.00812
C8 1 0.731220 0.010228 0.123495 11.00000 0.02945 0.03458 =
0.02524 -0.00807 -0.00342 -0.00450
C9 1 1.115327 0.138512 0.154200 11.00000 0.03612 0.03902 =
0.02975 -0.01557 -0.01478 0.00278
AFIX 66
C10 1 1.203285 0.203817 0.056517 11.00000 0.03161 0.02763 =
0.03211 -0.01330 -0.00109 0.00370
C11 1 1.160812 0.240010 -0.040463 11.00000 0.03590 0.04263 =
0.03294 -0.00625 -0.00665 -0.00268
AFIX 43
H11 2 1.075105 0.227189 -0.043601 11.00000 -1.20000
AFIX 65
C12 1 1.246440 0.295364 -0.132753 11.00000 0.05172 0.05231 =
0.03240 0.00075 -0.01283 -0.00094
AFIX 43
H12 2 1.218023 0.319579 -0.197639 11.00000 -1.20000
AFIX 65
C13 1 1.374541 0.314526 -0.128063 11.00000 0.04388 0.05343 =
0.03608 -0.00558 0.00232 -0.00038
AFIX 43
H13 2 1.431831 0.351562 -0.189811 11.00000 -1.20000
AFIX 65
C14 1 1.417015 0.278333 -0.031084 11.00000 0.02973 0.04710 =
0.05484 -0.01625 0.00180 -0.00891
AFIX 43
H14 2 1.502723 0.291154 -0.027946 11.00000 -1.20000
AFIX 65
C15 1 1.331388 0.222979 0.061207 11.00000 0.03236 0.04512 =
0.03518 -0.01409 -0.00562 -0.00178
AFIX 43
H15 2 1.359806 0.198764 0.126092 11.00000 -1.20000
AFIX 0
C16 1 1.041897 -0.228321 0.242593 11.00000 0.03312 0.04172 =
0.03038 -0.01161 -0.00915 -0.00410
AFIX 66
C17 1 1.104958 -0.344974 0.226992 11.00000 0.04835 0.03553 =
0.03426 -0.01307 -0.01350 0.00135
C18 1 1.234480 -0.351982 0.172450 11.00000 0.06580 0.04064 =
0.05494 -0.01713 0.01011 0.00117
AFIX 43
H18 2 1.280374 -0.282796 0.141133 11.00000 -1.20000
AFIX 65
C19 1 1.295409 -0.462395 0.164715 11.00000 0.08083 0.05234 =
0.07470 -0.02385 0.01123 -0.00228
AFIX 43
H19 2 1.382068 -0.467083 0.128223 11.00000 -1.20000
AFIX 65
C20 1 1.226816 -0.565802 0.211522 11.00000 0.08282 0.03870 =
0.06474 -0.01912 -0.00935 0.01516
AFIX 43
H20 2 1.267581 -0.639675 0.206347 11.00000 -1.20000
AFIX 65
C21 1 1.097293 -0.558796 0.266064 11.00000 0.08048 0.03929 =
0.10938 -0.01904 -0.00487 -0.00487
AFIX 43
H21 2 1.051400 -0.627982 0.297381 11.00000 -1.20000
AFIX 65
C22 1 1.036364 -0.448383 0.273800 11.00000 0.05009 0.04170 =
0.08627 -0.01302 -0.00687 -0.00510
AFIX 43
H22 2 0.949705 -0.443696 0.310292 11.00000 -1.20000
AFIX 0
C23 1 0.892821 0.169097 0.474348 11.00000 0.02744 0.04607 =
0.02656 -0.00840 -0.00591 -0.00722
PART 1
AFIX 66
C24 1 0.793379 0.273648 0.473157 21.00000 0.02954
PART 0
C25 1 0.748807 0.330243 0.379100 11.00000 0.05088
PART 1
AFIX 43
H25 2 0.767743 0.295419 0.322177 21.00000 -1.20000
AFIX 43
PART 0
PART 2
H25A 2 0.747302 0.283136 0.333255 -21.00000 -1.20000
AFIX 65
PART 0
C26 1 0.675935 0.438886 0.370121 11.00000 0.06597
PART 1
AFIX 43
H26 2 0.646114 0.476752 0.307190 21.00000 -1.20000
AFIX 43
PART 0
PART 2
H26A 2 0.622618 0.464049 0.319146 -21.00000 -1.20000
AFIX 65
PART 0
PART 1
C27 1 0.647633 0.490935 0.455199 21.00000 0.08682
AFIX 43
H27 2 0.598876 0.563625 0.449191 21.00000 -1.20000
AFIX 65
C28 1 0.692203 0.434341 0.549257 21.00000 0.05910
AFIX 43
H28 2 0.673267 0.469166 0.606180 21.00000 -1.20000
AFIX 65
C29 1 0.765077 0.325698 0.558237 21.00000 0.04378
AFIX 43
H29 2 0.794897 0.287833 0.621168 21.00000 -1.20000
AFIX 0
PART 0
C30 1 0.838118 0.404942 0.073834 11.00000 0.09188 0.09499 =
0.09961 -0.03884 -0.01790 0.00205
AFIX 137
H30A 2 0.831150 0.488046 0.072824 11.00000 -1.50000
H30B 2 0.872053 0.396678 0.002945 11.00000 -1.50000
H30C 2 0.896807 0.362329 0.120265 11.00000 -1.50000
AFIX 0
C31 1 0.710318 0.356857 0.111834 11.00000 0.10518 0.08440 =
0.05917 -0.02421 -0.02518 -0.00313
DY1 3 0.955261 -0.024018 0.310026 11.00000 0.02622 0.03997 =
0.01983 -0.00868 -0.00590 -0.00005
N1 4 0.750125 -0.081480 0.441094 11.00000 0.03298 0.04694 =
0.01869 -0.00935 -0.00936 -0.00367
N2 4 0.526063 -0.086306 0.272624 11.00000 0.02587 0.05000 =
0.02427 -0.01092 -0.00653 -0.00330
N3 4 0.410583 -0.065472 0.140681 11.00000 0.02835 0.06224 =
0.03007 -0.01025 -0.01100 -0.00647
AFIX 93
H3A 2 0.402703 -0.044167 0.074810 11.00000 -1.20000
H3B 2 0.345842 -0.096454 0.189426 11.00000 -1.20000
AFIX 0
N4 4 0.622176 -0.002416 0.090750 11.00000 0.02978 0.04032 =
0.02373 -0.00587 -0.01136 -0.00676
N5 4 0.832601 0.053376 0.049417 11.00000 0.03565 0.06989 =
0.02072 -0.00417 -0.00672 -0.02083
AFIX 93
H5A 2 0.826683 0.072053 -0.016833 11.00000 -1.20000
H5B 2 0.904819 0.062915 0.067222 11.00000 -1.20000
AFIX 0
N6 4 0.745902 -0.019367 0.228981 11.00000 0.02786 0.03734 =
0.01701 -0.00567 -0.00509 -0.00133
N7 4 0.612338 0.316376 0.143316 11.00000 0.12560 0.16069 =
0.06721 -0.02037 -0.01785 -0.03929
O1 5 1.157990 0.089168 0.238454 11.00000 0.03560 0.05574 =
0.02408 -0.00610 -0.01092 -0.00893
O2 5 0.994661 0.130373 0.151504 11.00000 0.03166 0.04579 =
0.03142 -0.00100 -0.01014 -0.00973
O3 5 0.934127 -0.226709 0.306348 11.00000 0.02978 0.04913 =
0.04902 -0.01537 -0.00078 -0.00433
O4 5 1.099895 -0.132651 0.195714 11.00000 0.05458 0.03721 =
0.02989 -0.01028 0.00636 -0.00849
O5 5 0.908549 0.123017 0.397814 11.00000 0.04404 0.04357 =
0.03063 -0.02046 -0.01020 0.00463
O6 5 1.063764 -0.124788 0.442194 11.00000 0.04670 0.05561 =
0.03071 -0.00865 -0.01910 0.01294
PART 2
C24A 1 0.823732 0.294097 0.458236 -21.00000 0.02978
C29A 1 0.832145 0.366304 0.521439 -21.00000 0.05610
AFIX 43
H29A 2 0.885199 0.342452 0.572662 -21.00000 -1.20000
AFIX 0
C28A 1 0.758386 0.479353 0.508131 -21.00000 0.07489
AFIX 43
H28A 2 0.763489 0.531018 0.549164 -21.00000 -1.20000
AFIX 0
C27A 1 0.682218 0.507577 0.434700 -21.00000 0.06469
AFIX 43
H27A 2 0.630613 0.578817 0.427897 -21.00000 -1.20000
AFIX 0
HKLF 4
REM 1 in P1 New: P-1
REM R1 = 0.0499 for 4646 Fo > 4sig(Fo) and 0.0705 for all 5939 data
REM 358 parameters refined using 0 restraints
END
WGHT 0.0376 0.0000
REM Highest difference peak 1.256, deepest hole -0.805, 1-sigma level 0.153
Q1 1 1.1367 0.0754 0.0644 11.00000 0.05 1.26
Q2 1 0.9893 0.0672 0.3026 11.00000 0.05 0.81
Q3 1 0.6721 0.4721 0.3981 11.00000 0.05 0.76
Q4 1 0.8214 -0.0413 0.3486 11.00000 0.05 0.75
Q5 1 0.8199 0.4856 0.5045 11.00000 0.05 0.75
Q6 1 0.6993 0.4602 0.5073 11.00000 0.05 0.67
Q7 1 0.8950 0.3910 0.5111 11.00000 0.05 0.65
Q8 1 1.0001 0.2003 0.1598 11.00000 0.05 0.64
Q9 1 0.9573 0.0791 0.1997 11.00000 0.05 0.62
Q10 1 0.5282 -0.1853 0.3019 11.00000 0.05 0.62
Q11 1 0.9337 -0.1355 0.3149 11.00000 0.05 0.62
Q12 1 0.6921 0.5172 0.4711 11.00000 0.05 0.62
Q13 1 0.9633 -0.0933 0.3845 11.00000 0.05 0.59
Q14 1 1.0138 -0.1393 0.3371 11.00000 0.05 0.57
Q15 1 0.6800 0.4129 0.3406 11.00000 0.05 0.57
Q16 1 1.5416 0.3719 0.0012 11.00000 0.05 0.56
Q17 1 0.8958 -0.0611 0.4057 11.00000 0.05 0.56
Q18 1 0.8243 0.2432 0.4608 11.00000 0.05 0.55
Q19 1 1.0919 -0.0808 0.3202 11.00000 0.05 0.54
Q20 1 0.9903 -0.0280 0.2992 11.00000 0.05 0.54
Q21 1 0.7515 0.3606 0.3970 11.00000 0.05 0.53
Q22 1 0.8844 0.0508 0.3752 11.00000 0.05 0.53
Q23 1 1.1992 -0.5868 0.3379 11.00000 0.05 0.53
Q24 1 0.7019 0.6981 0.4251 11.00000 0.05 0.53
Q25 1 0.5835 -0.1022 0.2904 11.00000 0.05 0.53
Q26 1 0.7454 0.2678 0.6028 11.00000 0.05 0.51
Q27 1 0.8526 0.1621 0.3598 11.00000 0.05 0.51
Q28 1 0.9215 -0.3433 0.4214 11.00000 0.05 0.50
Q29 1 0.5835 -0.0935 0.1429 11.00000 0.05 0.50
Q30 1 1.2983 -0.5783 0.2825 11.00000 0.05 0.50
REM The information below was added by Olex2.
REM
REM R1 = 0.0499 for 4646 Fo > 4sig(Fo) and 0.0705 for all 9592 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 1.26, deepest hole -0.80
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0705
REM R1_gt = 0.0499
REM wR_ref = 0.1053
REM GOOF = 1.045
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 9592
REM Reflections_gt = 4646
REM Parameters = n/a
REM Hole = -0.80
REM Peak = 1.26
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# 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
_audit_block_doi 10.5517/cc1j3yn7
_database_code_depnum_ccdc_archive 'CCDC 1403979'
_audit_update_record
;
2017-05-31 deposited with the CCDC.
2017-06-01 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 'C30 H42 Dy2 N12 O14'
_chemical_formula_sum 'C30 H42 Dy2 N12 O14'
_chemical_formula_weight 1119.75
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 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 8.2957(12)
_cell_length_b 9.8138(14)
_cell_length_c 12.7158(18)
_cell_angle_alpha 101.220(3)
_cell_angle_beta 103.232(3)
_cell_angle_gamma 104.948(3)
_cell_volume 937.6(2)
_cell_formula_units_Z 1
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 1740
_cell_measurement_theta_min 2.42
_cell_measurement_theta_max 25.76
_exptl_crystal_description block
_exptl_crystal_colour colorless
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_density_diffrn 1.983
_exptl_crystal_F_000 550
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.21
_exptl_absorpt_coefficient_mu 4.038
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.411
_exptl_absorpt_correction_T_max 0.428
_exptl_absorpt_process_details (sadabs;bruker,2000)
_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 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 5900
_diffrn_reflns_av_unetI/netI 0.1209
_diffrn_reflns_av_R_equivalents 0.0652
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 9
_diffrn_reflns_theta_min 1.708
_diffrn_reflns_theta_max 26.110
_diffrn_reflns_theta_full 25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total 3683
_reflns_number_gt 2955
_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 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)'
_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^)+(0.0407P)^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 3683
_refine_ls_number_parameters 267
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0753
_refine_ls_R_factor_gt 0.0572
_refine_ls_wR_factor_ref 0.1192
_refine_ls_wR_factor_gt 0.1099
_refine_ls_goodness_of_fit_ref 1.006
_refine_ls_restrained_S_all 1.006
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8191(11) 0.2572(10) 0.2724(8) 0.018(2) Uani 1 1 d . . . . .
H1 H 0.7314 0.2381 0.2060 0.021 Uiso 1 1 calc R U . . .
C2 C 0.7968(12) 0.1634(10) 0.3412(8) 0.019(2) Uani 1 1 d . . . . .
H2 H 0.6966 0.0829 0.3208 0.023 Uiso 1 1 calc R U . . .
C3 C 0.9259(11) 0.1924(10) 0.4394(7) 0.019(2) Uani 1 1 d . . . . .
H3 H 0.9154 0.1300 0.4856 0.022 Uiso 1 1 calc R U . . .
C4 C 1.0700(11) 0.3134(11) 0.4693(8) 0.019(2) Uani 1 1 d . . . . .
H4 H 1.1568 0.3355 0.5367 0.022 Uiso 1 1 calc R U . . .
C5 C 1.0848(11) 0.4030(10) 0.3969(7) 0.015(2) Uani 1 1 d . . . . .
C6 C 1.2310(10) 0.5405(10) 0.4307(7) 0.014(2) Uani 1 1 d . . . . .
C7 C 1.4724(11) 0.6997(10) 0.5650(8) 0.017(2) Uani 1 1 d . . . . .
C8 C 1.3512(11) 0.7689(10) 0.4146(7) 0.0132(19) Uani 1 1 d . . . . .
C9 C 0.6524(12) 0.7217(12) 0.2753(8) 0.026(2) Uani 1 1 d . . . . .
H9A H 0.5581 0.7118 0.2114 0.039 Uiso 1 1 calc R U . . .
H9B H 0.7101 0.8236 0.3133 0.039 Uiso 1 1 calc R U . . .
H9C H 0.6073 0.6722 0.3256 0.039 Uiso 1 1 calc R U . . .
C10 C 0.7799(11) 0.6555(10) 0.2375(7) 0.013(2) Uani 1 1 d . . . . .
C11 C 0.6417(11) 0.6851(10) -0.0354(8) 0.020(2) Uani 1 1 d . . . . .
H11A H 0.6949 0.7405 0.0416 0.029 Uiso 1 1 calc R U . . .
H11B H 0.5339 0.6129 -0.0425 0.029 Uiso 1 1 calc R U . . .
H11C H 0.6189 0.7496 -0.0807 0.029 Uiso 1 1 calc R U . . .
C12 C 0.7631(10) 0.6101(9) -0.0744(7) 0.0123(19) Uani 1 1 d . . . . .
C13 C 0.6263(12) 0.0783(10) -0.0887(8) 0.025(2) Uani 1 1 d . . . . .
H13A H 0.6464 0.0322 -0.0291 0.037 Uiso 1 1 calc R U . . .
H13B H 0.6368 0.0200 -0.1553 0.037 Uiso 1 1 calc R U . . .
H13C H 0.5111 0.0870 -0.1032 0.037 Uiso 1 1 calc R U . . .
C14 C 0.7605(10) 0.2299(10) -0.0550(7) 0.0121(19) Uani 1 1 d . . . . .
C15 C 0.0059(13) 0.0214(11) 0.1421(8) 0.028(2) Uani 1 1 d . . . . .
H15A H -0.1156 0.0071 0.1343 0.041 Uiso 1 1 calc R U . . .
H15B H 0.0176 -0.0552 0.0875 0.041 Uiso 1 1 calc R U . . .
H15C H 0.0581 0.1145 0.1304 0.041 Uiso 1 1 calc R U . . .
Dy1 Dy 1.00721(5) 0.52476(5) 0.16021(3) 0.01110(14) Uani 1 1 d . . . . .
N1 N 0.9624(9) 0.3740(8) 0.2985(6) 0.0162(17) Uani 1 1 d . . . . .
N2 N 1.2278(9) 0.6330(8) 0.3659(6) 0.0149(17) Uani 1 1 d . . . . .
N3 N 1.3450(9) 0.8734(8) 0.3626(6) 0.0156(17) Uani 1 1 d . . . . .
H3A H 1.4169 0.9605 0.3931 0.019 Uiso 1 1 calc R U . . .
H3B H 1.2690 0.8538 0.2986 0.019 Uiso 1 1 calc R U . . .
N4 N 1.4725(9) 0.8071(8) 0.5138(6) 0.0149(17) Uani 1 1 d . . . . .
N5 N 1.5974(9) 0.7302(9) 0.6603(6) 0.0189(18) Uani 1 1 d . . . . .
H5A H 1.6740 0.8159 0.6866 0.023 Uiso 1 1 calc R U . . .
H5B H 1.6020 0.6644 0.6957 0.023 Uiso 1 1 calc R U . . .
N6 N 1.3466(9) 0.5649(8) 0.5289(6) 0.0138(16) Uani 1 1 d . . . . .
O1 O 0.9313(7) 0.7360(7) 0.2476(5) 0.0168(14) Uani 1 1 d . . . . .
O2 O 0.7334(7) 0.5192(7) 0.1951(5) 0.0206(15) Uani 1 1 d . . . . .
O3 O 0.8613(7) 0.5682(6) -0.0044(5) 0.0144(14) Uani 1 1 d . . . . .
O4 O 0.7672(7) 0.5897(6) -0.1743(5) 0.0137(13) Uani 1 1 d . . . . .
O5 O 0.8242(8) 0.2935(7) 0.0467(5) 0.0175(14) Uani 1 1 d . . . . .
O6 O 0.7951(8) 0.2790(7) -0.1356(5) 0.0177(14) Uani 1 1 d . . . . .
O7 O 0.0906(8) 0.0182(8) 0.2505(5) 0.0239(16) Uani 1 1 d . . . . .
H7 H 0.0491 -0.0626 0.2594 0.036 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
C1 0.019(5) 0.018(5) 0.013(5) -0.001(4) 0.001(4) 0.008(4)
C2 0.019(5) 0.016(5) 0.023(5) 0.009(4) 0.008(4) 0.006(4)
C3 0.026(5) 0.019(5) 0.011(5) 0.006(4) 0.006(4) 0.006(4)
C4 0.017(5) 0.024(6) 0.014(5) 0.004(4) 0.002(4) 0.008(4)
C5 0.014(4) 0.017(5) 0.013(5) 0.002(4) 0.005(4) 0.007(4)
C6 0.010(4) 0.023(6) 0.014(5) 0.007(4) 0.007(4) 0.007(4)
C7 0.018(5) 0.017(5) 0.017(5) 0.001(4) 0.005(4) 0.009(4)
C8 0.015(4) 0.015(5) 0.011(4) 0.005(4) 0.006(4) 0.004(4)
C9 0.021(5) 0.032(7) 0.026(6) 0.005(5) 0.008(5) 0.010(5)
C10 0.015(4) 0.021(6) 0.006(4) 0.007(4) 0.000(4) 0.010(4)
C11 0.015(4) 0.021(6) 0.025(5) 0.012(5) 0.003(4) 0.005(4)
C12 0.010(4) 0.005(5) 0.013(5) -0.003(4) -0.005(4) 0.000(4)
C13 0.033(6) 0.024(6) 0.020(5) 0.007(5) 0.009(5) 0.012(5)
C14 0.011(4) 0.015(5) 0.014(5) 0.010(4) 0.001(4) 0.007(4)
C15 0.028(5) 0.031(6) 0.018(5) 0.009(5) -0.003(5) 0.008(5)
Dy1 0.0103(2) 0.0126(2) 0.0090(2) 0.00268(17) -0.00069(16) 0.00451(17)
N1 0.012(4) 0.016(4) 0.017(4) 0.004(4) 0.002(3) 0.001(3)
N2 0.010(3) 0.017(4) 0.008(4) -0.001(3) -0.004(3) -0.001(3)
N3 0.014(4) 0.011(4) 0.014(4) 0.004(3) -0.005(3) 0.000(3)
N4 0.018(4) 0.011(4) 0.011(4) 0.001(3) 0.003(3) 0.001(3)
N5 0.024(4) 0.020(5) 0.010(4) 0.008(3) -0.003(3) 0.006(4)
N6 0.014(4) 0.015(4) 0.015(4) 0.006(3) 0.004(3) 0.007(3)
O1 0.015(3) 0.017(4) 0.021(3) 0.004(3) 0.004(3) 0.011(3)
O2 0.013(3) 0.020(4) 0.025(4) 0.006(3) 0.002(3) 0.002(3)
O3 0.012(3) 0.015(3) 0.012(3) 0.003(3) -0.007(3) 0.006(3)
O4 0.014(3) 0.013(3) 0.011(3) 0.000(3) -0.001(3) 0.004(3)
O5 0.023(3) 0.019(4) 0.008(3) 0.004(3) 0.000(3) 0.006(3)
O6 0.018(3) 0.018(4) 0.009(3) 0.001(3) -0.002(3) 0.001(3)
O7 0.022(3) 0.026(4) 0.015(3) 0.005(3) -0.005(3) 0.002(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.344(11) . ?
C1 C2 1.395(12) . ?
C1 H1 0.9300 . ?
C2 C3 1.371(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.366(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.396(12) . ?
C4 H4 0.9300 . ?
C5 N1 1.345(10) . ?
C5 C6 1.473(12) . ?
C6 N6 1.324(10) . ?
C6 N2 1.341(11) . ?
C7 N5 1.325(10) . ?
C7 N4 1.342(11) . ?
C7 N6 1.372(11) . ?
C8 N3 1.329(11) . ?
C8 N4 1.336(10) . ?
C8 N2 1.376(11) . ?
C9 C10 1.496(13) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O2 1.260(11) . ?
C10 O1 1.262(10) . ?
C10 Dy1 2.788(9) . ?
C11 C12 1.507(12) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 O4 1.257(10) . ?
C12 O3 1.267(10) . ?
C12 Dy1 2.874(9) 2_765 ?
C13 C14 1.522(12) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 O5 1.242(10) . ?
C14 O6 1.273(10) . ?
C15 O7 1.407(10) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
Dy1 O6 2.310(6) 2_765 ?
Dy1 O5 2.342(6) . ?
Dy1 O3 2.342(5) . ?
Dy1 O2 2.402(6) . ?
Dy1 O4 2.409(6) 2_765 ?
Dy1 O1 2.454(6) . ?
Dy1 N1 2.539(7) . ?
Dy1 O3 2.598(6) 2_765 ?
Dy1 N2 2.654(7) . ?
Dy1 C12 2.874(9) 2_765 ?
Dy1 Dy1 3.9784(10) 2_765 ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N5 H5A 0.8600 . ?
N5 H5B 0.8600 . ?
O3 Dy1 2.598(6) 2_765 ?
O4 Dy1 2.409(6) 2_765 ?
O6 Dy1 2.310(6) 2_765 ?
O7 H7 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
N1 C1 C2 122.5(8) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C3 C2 C1 118.5(8) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C4 C3 C2 119.9(8) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 118.9(8) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 122.2(8) . . ?
N1 C5 C6 117.4(7) . . ?
C4 C5 C6 120.2(8) . . ?
N6 C6 N2 126.5(8) . . ?
N6 C6 C5 115.0(7) . . ?
N2 C6 C5 118.3(7) . . ?
N5 C7 N4 117.1(8) . . ?
N5 C7 N6 118.4(8) . . ?
N4 C7 N6 124.4(8) . . ?
N3 C8 N4 116.7(8) . . ?
N3 C8 N2 118.1(8) . . ?
N4 C8 N2 125.1(7) . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C10 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O2 C10 O1 120.9(8) . . ?
O2 C10 C9 119.1(8) . . ?
O1 C10 C9 120.1(8) . . ?
O2 C10 Dy1 59.2(5) . . ?
O1 C10 Dy1 61.6(5) . . ?
C9 C10 Dy1 177.9(7) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O4 C12 O3 120.7(8) . . ?
O4 C12 C11 120.6(7) . . ?
O3 C12 C11 118.7(8) . . ?
O4 C12 Dy1 56.0(4) . 2_765 ?
O3 C12 Dy1 64.6(5) . 2_765 ?
C11 C12 Dy1 176.4(6) . 2_765 ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O5 C14 O6 126.6(8) . . ?
O5 C14 C13 117.9(7) . . ?
O6 C14 C13 115.6(8) . . ?
O7 C15 H15A 109.5 . . ?
O7 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O7 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O6 Dy1 O5 135.5(2) 2_765 . ?
O6 Dy1 O3 74.75(19) 2_765 . ?
O5 Dy1 O3 75.0(2) . . ?
O6 Dy1 O2 126.7(2) 2_765 . ?
O5 Dy1 O2 78.1(2) . . ?
O3 Dy1 O2 79.7(2) . . ?
O6 Dy1 O4 86.7(2) 2_765 2_765 ?
O5 Dy1 O4 84.4(2) . 2_765 ?
O3 Dy1 O4 124.6(2) . 2_765 ?
O2 Dy1 O4 145.0(2) . 2_765 ?
O6 Dy1 O1 76.8(2) 2_765 . ?
O5 Dy1 O1 129.5(2) . . ?
O3 Dy1 O1 82.0(2) . . ?
O2 Dy1 O1 53.7(2) . . ?
O4 Dy1 O1 143.76(19) 2_765 . ?
O6 Dy1 N1 142.2(2) 2_765 . ?
O5 Dy1 N1 76.0(2) . . ?
O3 Dy1 N1 142.6(2) . . ?
O2 Dy1 N1 71.5(2) . . ?
O4 Dy1 N1 75.0(2) 2_765 . ?
O1 Dy1 N1 98.9(2) . . ?
O6 Dy1 O3 70.5(2) 2_765 2_765 ?
O5 Dy1 O3 69.8(2) . 2_765 ?
O3 Dy1 O3 72.8(2) . 2_765 ?
O2 Dy1 O3 141.9(2) . 2_765 ?
O4 Dy1 O3 51.80(18) 2_765 2_765 ?
O1 Dy1 O3 142.80(19) . 2_765 ?
N1 Dy1 O3 117.8(2) . 2_765 ?
O6 Dy1 N2 79.6(2) 2_765 . ?
O5 Dy1 N2 136.5(2) . . ?
O3 Dy1 N2 148.3(2) . . ?
O2 Dy1 N2 101.7(2) . . ?
O4 Dy1 N2 71.2(2) 2_765 . ?
O1 Dy1 N2 74.2(2) . . ?
N1 Dy1 N2 63.4(2) . . ?
O3 Dy1 N2 115.5(2) 2_765 . ?
O6 Dy1 C10 101.9(2) 2_765 . ?
O5 Dy1 C10 103.8(2) . . ?
O3 Dy1 C10 79.5(2) . . ?
O2 Dy1 C10 26.8(2) . . ?
O4 Dy1 C10 155.9(2) 2_765 . ?
O1 Dy1 C10 26.9(2) . . ?
N1 Dy1 C10 85.0(2) . . ?
O3 Dy1 C10 152.3(2) 2_765 . ?
N2 Dy1 C10 88.0(2) . . ?
O6 Dy1 C12 77.8(2) 2_765 2_765 ?
O5 Dy1 C12 75.5(2) . 2_765 ?
O3 Dy1 C12 99.0(2) . 2_765 ?
O2 Dy1 C12 152.9(2) . 2_765 ?
O4 Dy1 C12 25.6(2) 2_765 2_765 ?
O1 Dy1 C12 153.3(2) . 2_765 ?
N1 Dy1 C12 96.2(2) . 2_765 ?
O3 Dy1 C12 26.2(2) 2_765 2_765 ?
N2 Dy1 C12 93.4(2) . 2_765 ?
C10 Dy1 C12 178.4(2) . 2_765 ?
O6 Dy1 Dy1 68.11(15) 2_765 2_765 ?
O5 Dy1 Dy1 67.83(14) . 2_765 ?
O3 Dy1 Dy1 38.59(15) . 2_765 ?
O2 Dy1 Dy1 114.11(15) . 2_765 ?
O4 Dy1 Dy1 86.01(14) 2_765 2_765 ?
O1 Dy1 Dy1 116.02(14) . 2_765 ?
N1 Dy1 Dy1 140.52(18) . 2_765 ?
O3 Dy1 Dy1 34.22(12) 2_765 2_765 ?
N2 Dy1 Dy1 141.49(16) . 2_765 ?
C10 Dy1 Dy1 118.07(16) . 2_765 ?
C12 Dy1 Dy1 60.37(16) 2_765 2_765 ?
C1 N1 C5 117.9(7) . . ?
C1 N1 Dy1 120.6(6) . . ?
C5 N1 Dy1 121.3(5) . . ?
C6 N2 C8 113.7(7) . . ?
C6 N2 Dy1 116.6(6) . . ?
C8 N2 Dy1 129.5(5) . . ?
C8 N3 H3A 120.0 . . ?
C8 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C8 N4 C7 115.1(7) . . ?
C7 N5 H5A 120.0 . . ?
C7 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C6 N6 C7 114.6(7) . . ?
C10 O1 Dy1 91.5(5) . . ?
C10 O2 Dy1 94.0(5) . . ?
C12 O3 Dy1 163.5(6) . . ?
C12 O3 Dy1 89.2(5) . 2_765 ?
Dy1 O3 Dy1 107.2(2) . 2_765 ?
C12 O4 Dy1 98.3(5) . 2_765 ?
C14 O5 Dy1 138.0(6) . . ?
C14 O6 Dy1 138.2(6) . 2_765 ?
C15 O7 H7 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
N1 C1 C2 C3 0.5(15) . . . . ?
C1 C2 C3 C4 1.7(14) . . . . ?
C2 C3 C4 C5 -1.8(15) . . . . ?
C3 C4 C5 N1 -0.4(15) . . . . ?
C3 C4 C5 C6 175.0(8) . . . . ?
N1 C5 C6 N6 179.1(8) . . . . ?
C4 C5 C6 N6 3.6(13) . . . . ?
N1 C5 C6 N2 4.5(13) . . . . ?
C4 C5 C6 N2 -171.0(9) . . . . ?
C2 C1 N1 C5 -2.5(14) . . . . ?
C2 C1 N1 Dy1 173.8(7) . . . . ?
C4 C5 N1 C1 2.5(14) . . . . ?
C6 C5 N1 C1 -173.0(8) . . . . ?
C4 C5 N1 Dy1 -173.9(7) . . . . ?
C6 C5 N1 Dy1 10.7(11) . . . . ?
N6 C6 N2 C8 -5.4(14) . . . . ?
C5 C6 N2 C8 168.4(8) . . . . ?
N6 C6 N2 Dy1 169.8(7) . . . . ?
C5 C6 N2 Dy1 -16.3(11) . . . . ?
N3 C8 N2 C6 -172.2(8) . . . . ?
N4 C8 N2 C6 4.0(13) . . . . ?
N3 C8 N2 Dy1 13.3(12) . . . . ?
N4 C8 N2 Dy1 -170.5(6) . . . . ?
N3 C8 N4 C7 178.6(9) . . . . ?
N2 C8 N4 C7 2.3(13) . . . . ?
N5 C7 N4 C8 175.9(8) . . . . ?
N6 C7 N4 C8 -8.2(13) . . . . ?
N2 C6 N6 C7 0.4(13) . . . . ?
C5 C6 N6 C7 -173.7(8) . . . . ?
N5 C7 N6 C6 -177.1(8) . . . . ?
N4 C7 N6 C6 7.0(13) . . . . ?
O2 C10 O1 Dy1 1.1(8) . . . . ?
C9 C10 O1 Dy1 -178.5(7) . . . . ?
O1 C10 O2 Dy1 -1.1(8) . . . . ?
C9 C10 O2 Dy1 178.5(7) . . . . ?
O4 C12 O3 Dy1 175.4(14) . . . . ?
C11 C12 O3 Dy1 -4(2) . . . . ?
Dy1 C12 O3 Dy1 174.1(19) 2_765 . . . ?
O4 C12 O3 Dy1 1.3(8) . . . 2_765 ?
C11 C12 O3 Dy1 -178.6(7) . . . 2_765 ?
O3 C12 O4 Dy1 -1.4(8) . . . 2_765 ?
C11 C12 O4 Dy1 178.5(7) . . . 2_765 ?
O6 C14 O5 Dy1 6.9(15) . . . . ?
C13 C14 O5 Dy1 -172.6(6) . . . . ?
O5 C14 O6 Dy1 8.9(15) . . . 2_765 ?
C13 C14 O6 Dy1 -171.5(6) . . . 2_765 ?
_refine_diff_density_max 2.258
_refine_diff_density_min -2.030
_refine_diff_density_rms 0.271
_shelx_res_file
;
1.res created by SHELXL-2014/7
TITL 1 in P1 New: P-1
CELL 0.71073 8.2957 9.8138 12.7158 101.220 103.232 104.948
ZERR 1 0.0012 0.0014 0.0018 0.003 0.003 0.003
LATT 1
SFAC C H Dy N O
UNIT 30 42 2 12 14
L.S. 50
ACTA
BOND $H
FMAP 2
PLAN 5
CONF
WGHT 0.040700
FVAR 0.16515
C1 1 0.819080 0.257165 0.272432 11.00000 0.01932 0.01751 =
0.01310 -0.00132 0.00070 0.00771
AFIX 43
H1 2 0.731386 0.238140 0.206000 11.00000 -1.20000
AFIX 0
C2 1 0.796809 0.163377 0.341179 11.00000 0.01937 0.01620 =
0.02341 0.00926 0.00796 0.00561
AFIX 43
H2 2 0.696620 0.082900 0.320837 11.00000 -1.20000
AFIX 0
C3 1 0.925895 0.192434 0.439434 11.00000 0.02628 0.01888 =
0.01146 0.00623 0.00610 0.00597
AFIX 43
H3 2 0.915363 0.129953 0.485641 11.00000 -1.20000
AFIX 0
C4 1 1.070019 0.313360 0.469315 11.00000 0.01682 0.02417 =
0.01364 0.00430 0.00172 0.00783
AFIX 43
H4 2 1.156814 0.335550 0.536747 11.00000 -1.20000
AFIX 0
C5 1 1.084770 0.403040 0.396901 11.00000 0.01412 0.01724 =
0.01321 0.00229 0.00458 0.00669
C6 1 1.231046 0.540542 0.430701 11.00000 0.01000 0.02255 =
0.01378 0.00670 0.00749 0.00669
C7 1 1.472421 0.699695 0.565017 11.00000 0.01761 0.01655 =
0.01689 0.00071 0.00511 0.00906
C8 1 1.351228 0.768865 0.414629 11.00000 0.01531 0.01477 =
0.01083 0.00454 0.00586 0.00433
C9 1 0.652424 0.721728 0.275317 11.00000 0.02138 0.03200 =
0.02603 0.00543 0.00837 0.01031
AFIX 137
H9A 2 0.558113 0.711817 0.211363 11.00000 -1.50000
H9B 2 0.710050 0.823637 0.313278 11.00000 -1.50000
H9C 2 0.607299 0.672214 0.325595 11.00000 -1.50000
AFIX 0
C10 1 0.779892 0.655537 0.237478 11.00000 0.01462 0.02108 =
0.00569 0.00666 -0.00023 0.01005
C11 1 0.641680 0.685070 -0.035444 11.00000 0.01468 0.02082 =
0.02455 0.01217 0.00344 0.00545
AFIX 137
H11A 2 0.694868 0.740502 0.041616 11.00000 -1.50000
H11B 2 0.533907 0.612852 -0.042458 11.00000 -1.50000
H11C 2 0.618918 0.749636 -0.080664 11.00000 -1.50000
AFIX 0
C12 1 0.763109 0.610059 -0.074421 11.00000 0.00973 0.00512 =
0.01343 -0.00347 -0.00511 0.00010
C13 1 0.626327 0.078285 -0.088750 11.00000 0.03332 0.02390 =
0.01976 0.00737 0.00931 0.01230
AFIX 137
H13A 2 0.646356 0.032235 -0.029100 11.00000 -1.50000
H13B 2 0.636817 0.020018 -0.155292 11.00000 -1.50000
H13C 2 0.511148 0.086951 -0.103178 11.00000 -1.50000
AFIX 0
C14 1 0.760517 0.229898 -0.054955 11.00000 0.01070 0.01489 =
0.01350 0.00966 0.00078 0.00670
C15 1 0.005944 0.021393 0.142063 11.00000 0.02835 0.03097 =
0.01828 0.00852 -0.00259 0.00779
AFIX 137
H15A 2 -0.115552 0.007110 0.134340 11.00000 -1.50000
H15B 2 0.017609 -0.055227 0.087485 11.00000 -1.50000
H15C 2 0.058052 0.114455 0.130377 11.00000 -1.50000
AFIX 0
DY1 3 1.007207 0.524763 0.160210 11.00000 0.01029 0.01260 =
0.00896 0.00268 -0.00069 0.00451
N1 4 0.962362 0.373961 0.298481 11.00000 0.01236 0.01568 =
0.01695 0.00403 0.00198 0.00075
N2 4 1.227762 0.633016 0.365886 11.00000 0.01036 0.01741 =
0.00813 -0.00064 -0.00421 -0.00092
N3 4 1.344958 0.873362 0.362625 11.00000 0.01414 0.01141 =
0.01396 0.00392 -0.00471 -0.00049
AFIX 93
H3A 2 1.416886 0.960520 0.393056 11.00000 -1.20000
H3B 2 1.268973 0.853804 0.298552 11.00000 -1.20000
AFIX 0
N4 4 1.472530 0.807073 0.513840 11.00000 0.01847 0.01093 =
0.01115 0.00102 0.00258 0.00069
N5 4 1.597426 0.730248 0.660257 11.00000 0.02428 0.01965 =
0.00984 0.00799 -0.00284 0.00583
AFIX 93
H5A 2 1.673992 0.815882 0.686638 11.00000 -1.20000
H5B 2 1.602004 0.664448 0.695697 11.00000 -1.20000
AFIX 0
N6 4 1.346594 0.564888 0.528914 11.00000 0.01433 0.01487 =
0.01460 0.00552 0.00421 0.00733
O1 5 0.931303 0.735960 0.247599 11.00000 0.01488 0.01677 =
0.02126 0.00450 0.00416 0.01079
O2 5 0.733354 0.519235 0.195074 11.00000 0.01281 0.02033 =
0.02454 0.00625 0.00162 0.00181
O3 5 0.861257 0.568232 -0.004421 11.00000 0.01223 0.01480 =
0.01158 0.00342 -0.00687 0.00572
O4 5 0.767220 0.589692 -0.174329 11.00000 0.01363 0.01271 =
0.01106 0.00039 -0.00096 0.00419
O5 5 0.824232 0.293521 0.046673 11.00000 0.02341 0.01874 =
0.00783 0.00379 0.00018 0.00640
O6 5 0.795141 0.278955 -0.135569 11.00000 0.01818 0.01849 =
0.00946 0.00095 -0.00156 0.00127
O7 5 0.090554 0.018226 0.250509 11.00000 0.02163 0.02607 =
0.01471 0.00454 -0.00478 0.00166
AFIX 147
H7 2 0.049100 -0.062584 0.259449 11.00000 -1.50000
AFIX 0
HKLF 4
REM 1 in P1 New: P-1
REM R1 = 0.0572 for 2955 Fo > 4sig(Fo) and 0.0753 for all 3683 data
REM 267 parameters refined using 0 restraints
END
WGHT 0.0407 0.0000
REM Highest difference peak 2.258, deepest hole -2.030, 1-sigma level 0.271
Q1 1 0.8937 0.5193 0.1738 11.00000 0.05 2.26
Q2 1 1.1132 0.5240 0.1410 11.00000 0.05 2.21
Q3 1 0.9425 0.5656 0.0935 11.00000 0.05 1.60
Q4 1 1.0499 0.4634 0.1993 11.00000 0.05 1.33
Q5 1 1.0490 0.5714 0.2457 11.00000 0.05 1.26
;
_shelx_res_checksum 27042
#######################################################################
#
# 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
_audit_block_doi 10.5517/cc1j3z2p
_database_code_depnum_ccdc_archive 'CCDC 1403992'
_audit_update_record
;
2017-05-31 deposited with the CCDC.
2017-06-01 downloaded from the CCDC.
;
_audit_creation_date 2017-04-26
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C32 H54 Dy2 F12 N4 O20 S4'
_chemical_formula_sum 'C32 H54 Dy2 F12 N4 O20 S4'
_chemical_formula_weight 1496.03
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
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 22.3484(16)
_cell_length_b 14.1037(10)
_cell_length_c 21.8136(16)
_cell_angle_alpha 90
_cell_angle_beta 109.759(2)
_cell_angle_gamma 90
_cell_volume 6470.7(8)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 7859
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 25.89
_cell_measurement_theta_min 2.16
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 2.514
_exptl_absorpt_correction_T_max 0.590
_exptl_absorpt_correction_T_min 0.567
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details (sadabs;bruker,2000)
_exptl_absorpt_special_details ?
_exptl_crystal_colour colorless
_exptl_crystal_density_diffrn 1.536
_exptl_crystal_density_meas .
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2952
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.21
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0484
_diffrn_reflns_av_unetI/netI 0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 27
_diffrn_reflns_limit_h_min -26
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_number 19862
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 26.019
_diffrn_reflns_theta_min 1.738
_diffrn_ambient_temperature 296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4942
_reflns_number_total 6377
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'Bruker SMART'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max 0.879
_refine_diff_density_min -0.800
_refine_diff_density_rms 0.109
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.039
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 334
_refine_ls_number_reflns 6377
_refine_ls_number_restraints 137
_refine_ls_R_factor_all 0.0544
_refine_ls_R_factor_gt 0.0412
_refine_ls_restrained_S_all 1.106
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+4.2788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0959
_refine_ls_wR_factor_ref 0.1015
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
C4-C5 = C9-C10
1.48 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq,
Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim
Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
F3, C1, N1, N11, F1, C1, F2, C1, O7, C3, O7, C6, C3, C4, C5, C6
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C4A)=Sof(H4AA)=
Sof(H4AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=1-FVAR(1)
Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=
Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
C9(H9A,H9B), C10(H10A,H10B), C6A(H6AA,H6AB), C5A(H5AA,H5AB), C4A(H4AA,H4AB),
C3A(H3AA,H3AB)
6.b X=CH2 refined with riding coordinates:
C17(H17A,H17B)
6.c Idealised Me refined as rotating group:
C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.31022(2) 0.35473(2) -0.00134(2) 0.03610(10) Uani 1 1 d . . . . .
S1 S 0.29078(9) 0.26692(13) 0.14587(7) 0.0661(5) Uani 1 1 d . . . . .
S2 S 0.47707(7) 0.28379(13) 0.02391(9) 0.0629(4) Uani 1 1 d . . . . .
F1 F 0.3304(3) 0.1537(5) 0.2438(3) 0.179(3) Uani 1 1 d . U . . .
F2 F 0.4011(3) 0.2487(6) 0.2333(3) 0.200(3) Uani 1 1 d . U . . .
F3 F 0.3715(4) 0.1283(5) 0.1688(4) 0.172(3) Uani 1 1 d . U . . .
F4 F 0.4977(3) 0.2880(5) 0.1479(3) 0.145(2) Uani 1 1 d . U . . .
F5 F 0.4761(4) 0.1534(5) 0.1059(3) 0.156(3) Uani 1 1 d . U . . .
F6 F 0.5661(2) 0.2114(5) 0.1212(3) 0.144(2) Uani 1 1 d . U . . .
O1 O 0.2452(2) 0.1963(3) 0.11083(18) 0.0620(11) Uani 1 1 d . . . . .
O0AA O 0.2698(4) 0.3275(4) 0.1853(3) 0.128(3) Uani 1 1 d . . . . .
O3 O 0.3245(2) 0.3119(3) 0.10756(18) 0.0684(12) Uani 1 1 d . . . . .
O4 O 0.41037(17) 0.3002(3) 0.0140(2) 0.0583(11) Uani 1 1 d . . . . .
O5 O 0.4865(3) 0.2124(4) -0.0171(3) 0.1068(19) Uani 1 1 d . . . . .
O6 O 0.5128(3) 0.3685(4) 0.0309(4) 0.125(2) Uani 1 1 d . . . . .
O7 O 0.37342(19) 0.4787(3) 0.0674(2) 0.0609(11) Uani 1 1 d . U . . .
O8 O 0.33328(18) 0.4585(3) -0.07755(19) 0.0563(10) Uani 1 1 d . . . . .
O9 O 0.24234(17) 0.4753(3) -0.0043(2) 0.0565(10) Uani 1 1 d . . . . .
N1 N 0.1879(2) 0.4589(3) 0.0027(2) 0.0542(12) Uani 1 1 d . U . . .
O2 O 0.20827(15) 0.3128(2) 0.00005(17) 0.0410(8) Uani 1 1 d . . . . .
C1 C 0.3550(5) 0.1937(9) 0.2031(5) 0.125(3) Uani 1 1 d . U . . .
C2 C 0.5062(4) 0.2315(7) 0.1033(4) 0.090(2) Uani 1 1 d . U . . .
C3 C 0.4158(8) 0.4740(12) 0.1321(7) 0.093(5) Uiso 0.535(11) 1 d . U P A 1
H3A H 0.4427 0.4183 0.1387 0.112 Uiso 0.535(11) 1 calc R . P A 1
H3B H 0.3929 0.4725 0.1628 0.112 Uiso 0.535(11) 1 calc R . P A 1
C4 C 0.4549(8) 0.5647(11) 0.1397(9) 0.102(5) Uiso 0.535(11) 1 d D U P A 1
H4A H 0.4826 0.5637 0.1138 0.122 Uiso 0.535(11) 1 calc R . P A 1
H4B H 0.4794 0.5782 0.1848 0.122 Uiso 0.535(11) 1 calc R . P A 1
C5 C 0.3989(9) 0.6327(13) 0.1123(10) 0.120(7) Uiso 0.535(11) 1 d D U P A 1
H5A H 0.4120 0.6973 0.1085 0.144 Uiso 0.535(11) 1 calc R . P A 1
H5B H 0.3692 0.6309 0.1359 0.144 Uiso 0.535(11) 1 calc R . P A 1
C6 C 0.3733(7) 0.5782(10) 0.0436(7) 0.078(4) Uiso 0.535(11) 1 d . U P A 1
H6A H 0.3310 0.5988 0.0175 0.093 Uiso 0.535(11) 1 calc R . P A 1
H6B H 0.4018 0.5857 0.0189 0.093 Uiso 0.535(11) 1 calc R . P A 1
C7 C 0.3815(4) 0.4400(6) -0.1069(4) 0.092(2) Uani 1 1 d . U . . .
H7A H 0.3825 0.3733 -0.1172 0.110 Uiso 1 1 calc R . . . .
H7B H 0.4232 0.4586 -0.0778 0.110 Uiso 1 1 calc R . . . .
C8 C 0.3622(6) 0.4995(8) -0.1685(5) 0.137(4) Uani 1 1 d . U . . .
H8A H 0.3987 0.5326 -0.1727 0.164 Uiso 1 1 calc R . . . .
H8B H 0.3440 0.4599 -0.2067 0.164 Uiso 1 1 calc R . . . .
C9 C 0.3173(6) 0.5638(10) -0.1621(6) 0.172(5) Uani 1 1 d D U . . .
H9A H 0.2842 0.5731 -0.2039 0.207 Uiso 1 1 calc R . . . .
H9B H 0.3374 0.6245 -0.1473 0.207 Uiso 1 1 calc R . . . .
C10 C 0.2898(4) 0.5276(6) -0.1156(4) 0.114(3) Uani 1 1 d D U . . .
H10A H 0.2841 0.5783 -0.0881 0.136 Uiso 1 1 calc R . . . .
H10B H 0.2487 0.4989 -0.1380 0.136 Uiso 1 1 calc R . . . .
N11 N 0.1674(2) 0.3765(3) 0.0053(2) 0.0491(12) Uani 1 1 d . U . . .
C12 C 0.1475(3) 0.5455(4) 0.0055(4) 0.073(2) Uani 1 1 d . U . . .
C13 C 0.0893(4) 0.5120(6) 0.0208(5) 0.122(4) Uani 1 1 d . U . . .
H13A H 0.1023 0.4681 0.0566 0.184 Uiso 1 1 calc GR . . . .
H13B H 0.0603 0.4812 -0.0167 0.184 Uiso 1 1 calc GR . . . .
H13C H 0.0688 0.5655 0.0323 0.184 Uiso 1 1 calc GR . . . .
C14 C 0.1286(5) 0.5903(6) -0.0618(5) 0.123(3) Uani 1 1 d . U . . .
H14A H 0.1051 0.6475 -0.0623 0.184 Uiso 1 1 calc GR . . . .
H14B H 0.1026 0.5468 -0.0935 0.184 Uiso 1 1 calc GR . . . .
H14C H 0.1661 0.6050 -0.0720 0.184 Uiso 1 1 calc GR . . . .
C15 C 0.1877(4) 0.6041(6) 0.0607(5) 0.089(2) Uani 1 1 d . U . . .
C16 C 0.1973(6) 0.6979(6) 0.0493(7) 0.160(5) Uani 1 1 d . U . . .
H16A H 0.1890 0.7073 0.0036 0.240 Uiso 1 1 calc GR . . . .
H16B H 0.2406 0.7150 0.0731 0.240 Uiso 1 1 calc GR . . . .
H16C H 0.1692 0.7369 0.0633 0.240 Uiso 1 1 calc GR . . . .
C17 C 0.2120(6) 0.5623(8) 0.1236(5) 0.157(5) Uani 1 1 d . U . . .
H17A H 0.2356 0.5986 0.1591 0.189 Uiso 1 1 calc R . . . .
H17B H 0.2044 0.4986 0.1292 0.189 Uiso 1 1 calc R . . . .
C6A C 0.3687(10) 0.5125(14) 0.1299(9) 0.101(6) Uiso 0.465(11) 1 d . U P A 2
H6AA H 0.3294 0.5475 0.1217 0.121 Uiso 0.465(11) 1 calc R . P A 2
H6AB H 0.3681 0.4587 0.1573 0.121 Uiso 0.465(11) 1 calc R . P A 2
C5A C 0.4209(10) 0.5715(14) 0.1620(9) 0.097(6) Uiso 0.465(11) 1 d . U P A 2
H5AA H 0.4572 0.5348 0.1884 0.116 Uiso 0.465(11) 1 calc R . P A 2
H5AB H 0.4100 0.6179 0.1894 0.116 Uiso 0.465(11) 1 calc R . P A 2
C4A C 0.4344(11) 0.6210(14) 0.1019(9) 0.096(6) Uiso 0.465(11) 1 d . U P A 2
H4AA H 0.4034 0.6694 0.0811 0.115 Uiso 0.465(11) 1 calc R . P A 2
H4AB H 0.4771 0.6465 0.1135 0.115 Uiso 0.465(11) 1 calc R . P A 2
C3A C 0.4256(9) 0.5317(12) 0.0626(9) 0.092(6) Uiso 0.465(11) 1 d . U P A 2
H3AA H 0.4181 0.5475 0.0173 0.110 Uiso 0.465(11) 1 calc R . P A 2
H3AB H 0.4639 0.4937 0.0782 0.110 Uiso 0.465(11) 1 calc R . P 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 0.03441(15) 0.03247(14) 0.04298(15) 0.00002(11) 0.01514(11) 0.00053(11)
S1 0.0814(12) 0.0772(11) 0.0394(8) -0.0062(8) 0.0200(8) -0.0261(10)
S2 0.0371(8) 0.0725(11) 0.0799(11) 0.0077(9) 0.0207(8) 0.0062(8)
F1 0.168(5) 0.241(7) 0.101(4) 0.088(4) 0.012(3) -0.063(5)
F2 0.156(5) 0.272(7) 0.108(4) 0.068(4) -0.039(4) -0.103(5)
F3 0.143(6) 0.173(6) 0.183(6) 0.069(4) 0.031(5) 0.024(4)
F4 0.138(5) 0.194(6) 0.086(4) -0.028(4) 0.017(3) 0.047(4)
F5 0.171(6) 0.152(5) 0.120(5) 0.064(4) 0.018(4) -0.002(4)
F6 0.077(3) 0.208(6) 0.116(4) 0.013(4) -0.008(3) 0.058(4)
O1 0.073(3) 0.068(3) 0.044(2) 0.003(2) 0.018(2) -0.028(2)
O0AA 0.187(7) 0.108(4) 0.129(5) -0.059(4) 0.105(5) -0.052(5)
O3 0.077(3) 0.079(3) 0.041(2) -0.004(2) 0.010(2) -0.041(3)
O4 0.032(2) 0.055(2) 0.086(3) 0.001(2) 0.0187(19) 0.0061(18)
O5 0.094(4) 0.141(5) 0.089(4) -0.015(4) 0.036(3) 0.052(4)
O6 0.062(3) 0.115(5) 0.187(7) 0.037(4) 0.028(4) -0.029(3)
O7 0.062(3) 0.055(2) 0.066(3) -0.015(2) 0.023(2) -0.015(2)
O8 0.061(3) 0.051(2) 0.062(3) 0.0166(19) 0.028(2) -0.001(2)
O9 0.046(2) 0.035(2) 0.099(3) 0.002(2) 0.039(2) 0.0017(17)
N1 0.043(3) 0.039(2) 0.083(4) 0.001(2) 0.025(2) 0.008(2)
O2 0.0333(19) 0.0314(18) 0.063(2) -0.0008(17) 0.0228(17) 0.0055(15)
C1 0.112(6) 0.150(7) 0.092(5) 0.045(5) 0.008(4) -0.043(5)
C2 0.072(5) 0.095(5) 0.094(5) 0.006(5) 0.015(4) 0.018(4)
C7 0.098(5) 0.103(5) 0.093(5) 0.026(4) 0.057(4) 0.009(4)
C8 0.176(8) 0.152(7) 0.109(6) 0.036(6) 0.083(6) 0.018(6)
C9 0.171(8) 0.202(9) 0.161(8) 0.085(7) 0.078(7) 0.023(7)
C10 0.121(6) 0.106(6) 0.125(6) 0.062(5) 0.057(5) 0.028(5)
N11 0.040(2) 0.036(2) 0.076(3) 0.000(2) 0.027(2) 0.005(2)
C12 0.060(4) 0.048(3) 0.117(5) -0.010(4) 0.037(4) 0.019(3)
C13 0.084(6) 0.074(5) 0.228(11) -0.027(6) 0.078(6) 0.016(5)
C14 0.122(7) 0.092(6) 0.146(8) 0.022(6) 0.035(6) 0.061(6)
C15 0.089(5) 0.060(4) 0.128(6) -0.020(4) 0.050(5) 0.009(4)
C16 0.161(10) 0.065(6) 0.255(13) -0.045(7) 0.072(9) 0.002(6)
C17 0.211(12) 0.122(8) 0.121(8) -0.030(7) 0.032(8) 0.017(8)
_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 2.399(4) 7 ?
Dy1 O3 2.366(4) . ?
Dy1 O4 2.281(3) . ?
Dy1 O7 2.422(4) . ?
Dy1 O8 2.398(3) . ?
Dy1 O9 2.265(4) . ?
Dy1 O2 2.364(3) . ?
Dy1 O2 2.401(3) 7 ?
S1 O1 1.445(4) . ?
S1 O0AA 1.402(6) . ?
S1 O3 1.447(4) . ?
S1 C1 1.864(11) . ?
S2 O4 1.451(4) . ?
S2 O5 1.409(5) . ?
S2 O6 1.416(5) . ?
S2 C2 1.790(9) . ?
F1 C1 1.318(11) . ?
F2 C1 1.279(11) . ?
F3 C1 1.317(14) . ?
F4 C2 1.319(9) . ?
F5 C2 1.302(10) . ?
F6 C2 1.293(9) . ?
O1 Dy1 2.399(4) 7 ?
O7 C3 1.411(15) . ?
O7 C6 1.496(14) . ?
O7 C6A 1.481(19) . ?
O7 C3A 1.417(17) . ?
O8 C7 1.452(7) . ?
O8 C10 1.428(8) . ?
O9 N1 1.298(5) . ?
N1 N11 1.257(6) . ?
N1 C12 1.531(7) . ?
O2 Dy1 2.401(3) 7 ?
O2 N11 1.313(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.53(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.529(16) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.61(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.518(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.395(13) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.445(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 C13 1.524(10) . ?
C12 C14 1.520(11) . ?
C12 C15 1.487(11) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.377(12) . ?
C15 C17 1.421(13) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9300 . ?
C17 H17B 0.9300 . ?
C6A H6AA 0.9700 . ?
C6A H6AB 0.9700 . ?
C6A C5A 1.41(2) . ?
C5A H5AA 0.9700 . ?
C5A H5AB 0.9700 . ?
C5A C4A 1.60(3) . ?
C4A H4AA 0.9700 . ?
C4A H4AB 0.9700 . ?
C4A C3A 1.50(2) . ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?
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 O7 146.03(14) 7 . ?
O1 Dy1 O2 71.54(13) 7 7 ?
O3 Dy1 O1 140.52(13) . 7 ?
O3 Dy1 O7 73.18(14) . . ?
O3 Dy1 O8 149.81(14) . . ?
O3 Dy1 O2 72.67(13) . 7 ?
O4 Dy1 O1 101.30(15) . 7 ?
O4 Dy1 O3 88.50(16) . . ?
O4 Dy1 O7 79.29(14) . . ?
O4 Dy1 O8 82.96(14) . . ?
O4 Dy1 O2 80.26(12) . 7 ?
O4 Dy1 O2 144.66(13) . . ?
O8 Dy1 O1 69.67(13) . 7 ?
O8 Dy1 O7 76.78(14) . . ?
O8 Dy1 O2 133.39(13) . 7 ?
O9 Dy1 O1 94.66(16) . 7 ?
O9 Dy1 O3 94.72(16) . . ?
O9 Dy1 O4 150.61(13) . . ?
O9 Dy1 O7 73.78(14) . . ?
O9 Dy1 O8 79.67(14) . . ?
O9 Dy1 O2 63.20(12) . . ?
O9 Dy1 O2 128.54(12) . 7 ?
O2 Dy1 O1 76.26(13) . 7 ?
O2 Dy1 O3 74.12(13) . . ?
O2 Dy1 O7 140.35(13) 7 . ?
O2 Dy1 O7 122.38(13) . . ?
O2 Dy1 O8 126.55(12) . . ?
O2 Dy1 O2 65.37(13) . 7 ?
O1 S1 O3 114.1(2) . . ?
O1 S1 C1 102.6(4) . . ?
O0AA S1 O1 115.0(3) . . ?
O0AA S1 O3 115.8(3) . . ?
O0AA S1 C1 105.5(6) . . ?
O3 S1 C1 101.3(4) . . ?
O4 S2 C2 103.2(3) . . ?
O5 S2 O4 112.8(3) . . ?
O5 S2 O6 118.1(4) . . ?
O5 S2 C2 103.7(4) . . ?
O6 S2 O4 113.2(3) . . ?
O6 S2 C2 103.6(4) . . ?
S1 O1 Dy1 140.1(2) . 7 ?
S1 O3 Dy1 140.5(2) . . ?
S2 O4 Dy1 169.5(3) . . ?
C3 O7 Dy1 129.7(7) . . ?
C3 O7 C6 108.2(9) . . ?
C6 O7 Dy1 122.0(6) . . ?
C6A O7 Dy1 126.5(8) . . ?
C3A O7 Dy1 131.1(7) . . ?
C3A O7 C6A 102.3(10) . . ?
C7 O8 Dy1 124.2(4) . . ?
C10 O8 Dy1 123.8(4) . . ?
C10 O8 C7 109.1(5) . . ?
N1 O9 Dy1 120.6(3) . . ?
O9 N1 C12 116.8(4) . . ?
N11 N1 O9 122.7(4) . . ?
N11 N1 C12 120.5(5) . . ?
Dy1 O2 Dy1 114.63(13) . 7 ?
N11 O2 Dy1 123.0(3) . 7 ?
N11 O2 Dy1 122.1(3) . . ?
F1 C1 S1 106.6(8) . . ?
F2 C1 S1 108.2(8) . . ?
F2 C1 F1 111.1(10) . . ?
F2 C1 F3 112.8(12) . . ?
F3 C1 S1 107.9(8) . . ?
F3 C1 F1 110.1(10) . . ?
F4 C2 S2 111.6(6) . . ?
F5 C2 S2 111.5(6) . . ?
F5 C2 F4 105.9(8) . . ?
F6 C2 S2 112.5(7) . . ?
F6 C2 F4 107.6(8) . . ?
F6 C2 F5 107.4(8) . . ?
O7 C3 H3A 111.0 . . ?
O7 C3 H3B 111.0 . . ?
O7 C3 C4 103.6(12) . . ?
H3A C3 H3B 109.0 . . ?
C4 C3 H3A 111.0 . . ?
C4 C3 H3B 111.0 . . ?
C3 C4 H4A 112.4 . . ?
C3 C4 H4B 112.4 . . ?
C3 C4 C5 96.9(14) . . ?
H4A C4 H4B 109.9 . . ?
C5 C4 H4A 112.4 . . ?
C5 C4 H4B 112.4 . . ?
C4 C5 H5A 113.1 . . ?
C4 C5 H5B 113.1 . . ?
C4 C5 C6 92.9(13) . . ?
H5A C5 H5B 110.5 . . ?
C6 C5 H5A 113.1 . . ?
C6 C5 H5B 113.1 . . ?
O7 C6 C5 99.6(10) . . ?
O7 C6 H6A 111.8 . . ?
O7 C6 H6B 111.8 . . ?
C5 C6 H6A 111.8 . . ?
C5 C6 H6B 111.8 . . ?
H6A C6 H6B 109.6 . . ?
O8 C7 H7A 110.7 . . ?
O8 C7 H7B 110.7 . . ?
O8 C7 C8 105.1(7) . . ?
H7A C7 H7B 108.8 . . ?
C8 C7 H7A 110.7 . . ?
C8 C7 H7B 110.7 . . ?
C7 C8 H8A 110.6 . . ?
C7 C8 H8B 110.6 . . ?
H8A C8 H8B 108.8 . . ?
C9 C8 C7 105.5(8) . . ?
C9 C8 H8A 110.6 . . ?
C9 C8 H8B 110.6 . . ?
C8 C9 H9A 109.8 . . ?
C8 C9 H9B 109.8 . . ?
C8 C9 C10 109.5(10) . . ?
H9A C9 H9B 108.2 . . ?
C10 C9 H9A 109.8 . . ?
C10 C9 H9B 109.8 . . ?
O8 C10 C9 106.3(8) . . ?
O8 C10 H10A 110.5 . . ?
O8 C10 H10B 110.5 . . ?
C9 C10 H10A 110.5 . . ?
C9 C10 H10B 110.5 . . ?
H10A C10 H10B 108.7 . . ?
N1 N11 O2 110.8(4) . . ?
C13 C12 N1 108.6(5) . . ?
C14 C12 N1 105.6(6) . . ?
C14 C12 C13 111.2(7) . . ?
C15 C12 N1 105.9(6) . . ?
C15 C12 C13 108.7(7) . . ?
C15 C12 C14 116.5(7) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C12 118.4(9) . . ?
C16 C15 C17 122.8(10) . . ?
C17 C15 C12 118.7(8) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 120.0 . . ?
C15 C17 H17B 120.0 . . ?
H17A C17 H17B 120.0 . . ?
O7 C6A H6AA 109.6 . . ?
O7 C6A H6AB 109.6 . . ?
H6AA C6A H6AB 108.1 . . ?
C5A C6A O7 110.1(15) . . ?
C5A C6A H6AA 109.6 . . ?
C5A C6A H6AB 109.6 . . ?
C6A C5A H5AA 111.4 . . ?
C6A C5A H5AB 111.4 . . ?
C6A C5A C4A 101.7(15) . . ?
H5AA C5A H5AB 109.3 . . ?
C4A C5A H5AA 111.4 . . ?
C4A C5A H5AB 111.4 . . ?
C5A C4A H4AA 112.8 . . ?
C5A C4A H4AB 112.8 . . ?
H4AA C4A H4AB 110.3 . . ?
C3A C4A C5A 94.4(15) . . ?
C3A C4A H4AA 112.8 . . ?
C3A C4A H4AB 112.8 . . ?
O7 C3A C4A 110.8(14) . . ?
O7 C3A H3AA 109.5 . . ?
O7 C3A H3AB 109.5 . . ?
C4A C3A H3AA 109.5 . . ?
C4A C3A H3AB 109.5 . . ?
H3AA C3A H3AB 108.1 . . ?
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
Dy1 O7 C3 C4 162.9(8) . . . . ?
Dy1 O7 C6 C5 159.4(8) . . . . ?
Dy1 O7 C6A C5A 168.4(11) . . . . ?
Dy1 O7 C3A C4A 160.5(10) . . . . ?
Dy1 O8 C7 C8 158.2(6) . . . . ?
Dy1 O8 C10 C9 -171.0(7) . . . . ?
Dy1 O9 N1 N11 -6.9(7) . . . . ?
Dy1 O9 N1 C12 175.2(4) . . . . ?
Dy1 O2 N11 N1 6.5(6) . . . . ?
Dy1 O2 N11 N1 -179.5(3) 7 . . . ?
O1 S1 O3 Dy1 30.1(6) . . . . ?
O1 S1 C1 F1 -65.9(9) . . . . ?
O1 S1 C1 F2 174.5(8) . . . . ?
O1 S1 C1 F3 52.2(8) . . . . ?
O0AA S1 O1 Dy1 121.4(5) . . . 7 ?
O0AA S1 O3 Dy1 -106.8(6) . . . . ?
O0AA S1 C1 F1 54.8(9) . . . . ?
O0AA S1 C1 F2 -64.7(10) . . . . ?
O0AA S1 C1 F3 173.0(7) . . . . ?
O3 S1 O1 Dy1 -15.9(6) . . . 7 ?
O3 S1 C1 F1 176.0(8) . . . . ?
O3 S1 C1 F2 56.4(10) . . . . ?
O3 S1 C1 F3 -65.9(8) . . . . ?
O4 S2 C2 F4 -58.9(7) . . . . ?
O4 S2 C2 F5 59.3(7) . . . . ?
O4 S2 C2 F6 -179.9(7) . . . . ?
O5 S2 O4 Dy1 -134.1(15) . . . . ?
O5 S2 C2 F4 -176.7(6) . . . . ?
O5 S2 C2 F5 -58.5(8) . . . . ?
O5 S2 C2 F6 62.2(8) . . . . ?
O6 S2 O4 Dy1 3.4(17) . . . . ?
O6 S2 C2 F4 59.4(7) . . . . ?
O6 S2 C2 F5 177.6(7) . . . . ?
O6 S2 C2 F6 -61.7(8) . . . . ?
O7 C3 C4 C5 49.0(17) . . . . ?
O7 C6A C5A C4A 33(2) . . . . ?
O8 C7 C8 C9 15.0(12) . . . . ?
O9 N1 N11 O2 0.2(8) . . . . ?
O9 N1 C12 C13 -174.2(6) . . . . ?
O9 N1 C12 C14 66.5(8) . . . . ?
O9 N1 C12 C15 -57.7(8) . . . . ?
N1 C12 C15 C16 126.1(8) . . . . ?
N1 C12 C15 C17 -56.7(10) . . . . ?
C1 S1 O1 Dy1 -124.5(6) . . . 7 ?
C1 S1 O3 Dy1 139.6(6) . . . . ?
C2 S2 O4 Dy1 114.7(16) . . . . ?
C3 O7 C6 C5 -21.8(14) . . . . ?
C3 C4 C5 C6 -58.5(16) . . . . ?
C4 C5 C6 O7 49.6(15) . . . . ?
C6 O7 C3 C4 -15.7(14) . . . . ?
C7 O8 C10 C9 -9.7(11) . . . . ?
C7 C8 C9 C10 -21.6(15) . . . . ?
C8 C9 C10 O8 20.0(15) . . . . ?
C10 O8 C7 C8 -3.0(10) . . . . ?
N11 N1 C12 C13 7.9(9) . . . . ?
N11 N1 C12 C14 -111.5(7) . . . . ?
N11 N1 C12 C15 124.4(7) . . . . ?
C12 N1 N11 O2 178.0(5) . . . . ?
C13 C12 C15 C16 -117.4(9) . . . . ?
C13 C12 C15 C17 59.8(10) . . . . ?
C14 C12 C15 C16 9.1(11) . . . . ?
C14 C12 C15 C17 -173.8(8) . . . . ?
C6A O7 C3A C4A -23.8(17) . . . . ?
C6A C5A C4A C3A -42(2) . . . . ?
C5A C4A C3A O7 41.0(19) . . . . ?
C3A O7 C6A C5A -7.5(18) . . . . ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.356 0.250 361.6 91.2 ?
2 0.000 0.644 0.750 361.6 90.9 ?
3 0.500 0.144 0.750 361.6 90.9 ?
4 0.500 0.856 0.250 361.6 91.2 ?
_shelx_fab_file
;
-27 1 5 -0.3485 -0.6061
-27 1 6 -1.5824 -0.0124
-27 1 7 0.3468 0.0757
-27 1 8 2.3796 -0.0857
-27 1 9 1.9085 -0.0294
-27 1 10 -2.5558 0.3011
-27 1 11 -1.2216 -0.1595
-27 1 12 -3.1782 -0.3750
-27 1 13 -2.1907 -0.4884
-27 3 7 -1.3286 -0.6075
-27 3 8 1.1960 0.9220
-27 3 9 2.0139 0.3575
-27 3 10 1.9552 0.8939
-27 3 11 -0.5649 -0.3246
-26 0 2 -0.5260 -1.0910
-26 0 4 -0.8705 0.8570
-26 0 6 3.8774 0.2988
-26 0 8 -5.9785 -0.2405
-26 0 10 7.0291 0.0232
-26 0 12 -0.4608 -0.0470
-26 0 14 -3.5565 0.1336
-26 0 16 -2.9276 -1.1619
-26 2 1 0.6171 0.6000
-26 2 2 4.8624 0.8939
-26 2 3 0.5460 -0.9166
-26 2 4 -2.9339 -0.5544
-26 2 5 -2.8288 0.4625
-26 2 6 -0.9420 0.3271
-26 2 7 2.5693 0.0024
-26 2 8 0.5327 -0.3020
-26 2 9 -2.9744 0.0252
-26 2 10 1.3584 -0.2959
-26 2 11 0.9946 0.5148
-26 2 12 -1.8255 0.4217
-26 2 13 3.7046 0.0451
-26 2 14 1.2136 0.1402
-26 2 15 -0.0845 -0.2873
-26 2 16 -0.0756 0.3162
-26 4 3 2.8340 -0.1041
-26 4 4 -0.7651 1.2480
-26 4 5 -0.2197 -0.0655
-26 4 6 1.4047 -0.2113
-26 4 7 -0.2275 0.3504
-26 4 8 1.3137 -0.5481
-26 4 9 -0.1875 -0.1796
-26 4 10 -4.9272 -0.4992
-26 4 11 -0.1357 -0.5493
-26 4 12 3.9881 0.7916
-26 4 13 -1.3662 -0.0218
-26 4 14 -1.6007 1.1920
-25 1 1 0.6051 0.6032
-25 1 2 -2.0821 -0.7475
-25 1 3 1.3595 -0.1682
-25 1 4 1.9489 -0.3060
-25 1 5 2.8699 -0.4729
-25 1 6 -1.4784 0.3705
-25 1 7 -5.5676 0.3483
-25 1 8 1.8700 -0.0430
-25 1 9 3.6742 -0.1477
-25 1 10 -4.2444 0.2383
-25 1 11 -0.3633 -0.2553
-25 1 12 3.4678 0.1129
-25 1 13 -3.6915 -0.1540
-25 1 14 -1.5867 -0.4124
-25 1 15 2.6456 -0.2939
-25 1 16 4.2199 0.1778
-25 1 17 1.9796 2.1965
-25 1 18 -4.2720 -0.2478
-25 3 1 0.6933 0.0137
-25 3 2 -3.8915 0.4668
-25 3 3 -2.5192 -0.2518
-25 3 4 0.7595 -0.1610
-25 3 5 0.4168 0.2710
-25 3 6 3.8061 0.0369
-25 3 7 1.1475 -0.1177
-25 3 8 -3.0203 0.2467
-25 3 9 1.8576 -0.0954
-25 3 10 0.5593 0.0871
-25 3 11 -4.5525 -0.1865
-25 3 12 1.5880 -0.7654
-25 3 13 4.6322 0.0153
-25 3 14 -2.2579 -0.3154
-25 3 15 -4.0004 0.4843
-25 3 16 -2.6013 0.6731
-25 3 17 2.9170 0.3050
-25 5 1 1.6516 -1.2991
-25 5 2 2.6910 0.0337
-25 5 3 -3.1234 0.5926
-25 5 4 -1.4249 -0.5100
-25 5 5 2.1444 -0.4516
-25 5 6 -1.0199 -0.0091
-25 5 7 0.2041 0.0120
-25 5 8 -0.4994 0.3506
-25 5 9 -2.1926 0.3875
-25 5 10 1.4264 0.2913
-25 5 11 2.5360 0.2293
-25 5 12 -0.5665 -0.1988
-25 5 13 -0.2391 0.4163
-25 5 14 0.9057 -0.2866
-25 5 15 -1.5335 -2.3556
-25 5 16 1.1185 -0.2176
-25 7 5 0.4862 0.1262
-25 7 6 0.9870 0.0062
-25 7 7 -1.9914 -0.0590
-25 7 8 2.7474 -0.1514
-25 7 9 2.8231 -0.3941
-25 7 10 -1.5807 0.1953
-25 7 11 -3.4485 -0.2297
-24 0 2 1.1904 3.3692
-24 0 4 0.3537 -0.9793
-24 0 6 0.5191 -0.6484
-24 0 8 -1.5453 0.4131
-24 0 10 2.4450 0.0711
-24 0 12 -2.0221 -0.0845
-24 0 14 -0.1606 -0.1761
-24 0 16 -0.9711 -0.2967
-24 0 18 0.7109 0.2847
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21 7 3 -9.6389 -0.5258
21 7 4 -1.1797 -1.2224
21 7 5 4.4546 0.9708
21 9 0 0.0821 0.2398
21 9 1 -3.2991 -0.3679
21 9 2 -1.8112 -0.0650
22 0 0 7.1388 -1.5193
22 0 2 -12.4458 0.1393
22 0 4 8.4876 0.5753
22 0 6 -2.6620 0.2151
22 2 0 0.6722 0.3706
22 2 1 3.8160 0.1239
22 2 2 3.8251 0.2633
22 2 3 -1.5119 -0.1144
22 2 4 -1.3295 0.6096
22 2 5 -0.3146 -0.7260
22 2 6 -1.7943 -0.9128
22 2 7 0.3065 0.9384
22 4 0 -0.8533 0.0392
22 4 1 -1.0142 -0.3347
22 4 2 -0.2759 -0.4120
22 4 3 1.8859 0.4763
22 4 4 0.1740 0.0219
22 4 5 -0.5308 -0.3042
22 4 6 -2.0101 0.2652
22 6 0 0.8985 0.2163
22 6 1 -1.4987 -0.2538
22 6 2 -0.1258 -1.0117
22 6 3 3.3952 1.3637
22 6 4 0.3553 0.7971
22 6 5 0.4585 -2.0089
22 8 0 1.9217 -0.3969
22 8 1 -2.3096 1.1913
22 8 2 -3.4921 -0.5737
23 1 0 -2.4600 -0.4833
23 1 1 -6.3128 -0.8285
23 1 2 1.2024 -0.0826
23 1 3 3.7521 0.5724
23 1 4 0.5157 -0.7148
23 1 5 1.5882 0.3966
23 1 6 -0.3665 0.7527
23 3 0 0.9254 -0.4342
23 3 1 -0.5500 -0.4038
23 3 2 -0.8326 0.7638
23 3 3 -0.4258 -0.2796
23 3 4 -2.8222 -0.6668
23 3 5 -2.2156 0.5646
23 5 0 -1.1519 -0.1512
23 5 1 1.4057 0.2218
23 5 2 0.3562 0.6661
23 5 3 -1.7525 -0.5967
23 5 4 1.9319 -0.5709
23 7 0 -0.0573 -0.3352
23 7 1 -0.8581 -0.9374
24 0 0 -3.0434 2.5553
24 0 2 4.2670 -0.5260
24 0 4 -4.2629 1.1410
24 2 0 0.0069 -0.3242
24 2 1 1.6941 0.5055
24 2 2 -0.2746 0.1935
24 2 3 0.7425 -0.1642
24 2 4 1.8454 -0.2782
24 4 0 -0.8067 0.4552
24 4 1 0.1100 0.9316
24 4 2 1.2224 -1.0306
24 4 3 -1.7131 -0.1129
24 6 0 2.3243 0.2191
24 6 1 0.1042 0.6853
25 1 0 2.8579 -0.8648
25 1 1 3.7861 -1.5790
25 1 2 -2.9947 0.1901
25 3 0 2.2000 -0.0613
25 3 1 -1.7028 -0.2371
0 0 0 0.0 0.0
;
_iucr_refine_instructions_details
;
1.res created by SHELXL-2014/7
TITL 1 in C2/c New: C2/c
CELL 0.71073 22.3484 14.1037 21.8136 90 109.759 90
ZERR 4 0.0016 0.001 0.0016 0 0.002 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H Dy F N O S
UNIT 128 216 8 48 16 80 16
DFIX 1.48 C4 C5 C9 C10
RIGU F3 C1 N1 N11 F1 C1 F2 C1 O7 C3 O7 C6 C3 C4 C5 C6
ISOR 0.01 0.02 $c $f O7
L.S. 100
PLAN 10
TEMP 23
BOND $H
CONF
ABIN
fmap 2
acta
OMIT -2 0 1
OMIT 8 0 5
OMIT 18 0 7
OMIT -10 0 9
OMIT -10 0 9
OMIT 16 10 8
OMIT -2 12 12
OMIT -4 0 2
OMIT 1 1 2
REM
REM
REM
WGHT 0.048100 4.278800
FVAR 0.04183 0.53468
DY1 3 0.310220 0.354730 -0.001345 11.00000 0.03441 0.03247 =
0.04298 0.00002 0.01514 0.00053
S1 7 0.290782 0.266924 0.145871 11.00000 0.08142 0.07719 =
0.03936 -0.00616 0.02000 -0.02615
S2 7 0.477074 0.283789 0.023909 11.00000 0.03709 0.07248 =
0.07994 0.00768 0.02074 0.00623
F1 4 0.330364 0.153741 0.243764 11.00000 0.16827 0.24095 =
0.10116 0.08819 0.01177 -0.06265
F2 4 0.401118 0.248692 0.233310 11.00000 0.15578 0.27218 =
0.10799 0.06847 -0.03864 -0.10308
F3 4 0.371458 0.128260 0.168812 11.00000 0.14253 0.17336 =
0.18257 0.06888 0.03134 0.02407
F4 4 0.497718 0.288021 0.147883 11.00000 0.13791 0.19434 =
0.08594 -0.02807 0.01744 0.04749
F5 4 0.476078 0.153427 0.105948 11.00000 0.17064 0.15162 =
0.12041 0.06408 0.01770 -0.00210
F6 4 0.566105 0.211432 0.121238 11.00000 0.07681 0.20756 =
0.11634 0.01293 -0.00789 0.05806
O1 6 0.245187 0.196308 0.110834 11.00000 0.07259 0.06783 =
0.04407 0.00287 0.01790 -0.02844
O0AA 6 0.269774 0.327500 0.185344 11.00000 0.18684 0.10819 =
0.12917 -0.05851 0.10486 -0.05228
O3 6 0.324481 0.311889 0.107560 11.00000 0.07711 0.07924 =
0.04111 -0.00379 0.00993 -0.04119
O4 6 0.410369 0.300244 0.014049 11.00000 0.03237 0.05514 =
0.08637 0.00073 0.01873 0.00606
O5 6 0.486545 0.212424 -0.017062 11.00000 0.09357 0.14126 =
0.08918 -0.01539 0.03573 0.05167
O6 6 0.512810 0.368491 0.030948 11.00000 0.06249 0.11455 =
0.18724 0.03689 0.02798 -0.02861
O7 6 0.373416 0.478683 0.067356 11.00000 0.06216 0.05528 =
0.06602 -0.01544 0.02268 -0.01516
O8 6 0.333285 0.458494 -0.077552 11.00000 0.06112 0.05104 =
0.06207 0.01656 0.02797 -0.00101
O9 6 0.242341 0.475297 -0.004345 11.00000 0.04595 0.03523 =
0.09920 0.00181 0.03867 0.00170
N1 5 0.187891 0.458944 0.002700 11.00000 0.04293 0.03897 =
0.08339 0.00068 0.02475 0.00841
O2 6 0.208266 0.312806 0.000055 11.00000 0.03334 0.03136 =
0.06315 -0.00079 0.02285 0.00553
C1 1 0.355031 0.193712 0.203133 11.00000 0.11222 0.14951 =
0.09179 0.04461 0.00751 -0.04295
C2 1 0.506202 0.231545 0.103322 11.00000 0.07236 0.09480 =
0.09393 0.00559 0.01494 0.01788
PART 1
C3 1 0.415779 0.473974 0.132115 21.00000 0.09311
AFIX 23
H3A 2 0.442690 0.418280 0.138714 21.00000 -1.20000
H3B 2 0.392872 0.472533 0.162764 21.00000 -1.20000
AFIX 0
C4 1 0.454875 0.564666 0.139697 21.00000 0.10168
AFIX 23
H4A 2 0.482631 0.563711 0.113803 21.00000 -1.20000
H4B 2 0.479378 0.578171 0.184829 21.00000 -1.20000
AFIX 0
C5 1 0.398884 0.632667 0.112261 21.00000 0.12023
AFIX 23
H5A 2 0.411979 0.697343 0.108468 21.00000 -1.20000
H5B 2 0.369161 0.630910 0.135947 21.00000 -1.20000
AFIX 0
C6 1 0.373324 0.578158 0.043581 21.00000 0.07759
AFIX 23
H6A 2 0.330965 0.598828 0.017481 21.00000 -1.20000
H6B 2 0.401845 0.585745 0.018861 21.00000 -1.20000
AFIX 0
PART 0
C7 1 0.381540 0.440036 -0.106936 11.00000 0.09839 0.10283 =
0.09282 0.02602 0.05666 0.00932
AFIX 23
H7A 2 0.382514 0.373258 -0.117197 11.00000 -1.20000
H7B 2 0.423228 0.458643 -0.077766 11.00000 -1.20000
AFIX 0
C8 1 0.362240 0.499477 -0.168543 11.00000 0.17588 0.15230 =
0.10860 0.03572 0.08339 0.01798
AFIX 23
H8A 2 0.398714 0.532638 -0.172670 11.00000 -1.20000
H8B 2 0.343964 0.459868 -0.206669 11.00000 -1.20000
AFIX 0
C9 1 0.317308 0.563757 -0.162052 11.00000 0.17139 0.20168 =
0.16055 0.08524 0.07825 0.02330
AFIX 23
H9A 2 0.284240 0.573109 -0.203906 11.00000 -1.20000
H9B 2 0.337437 0.624450 -0.147280 11.00000 -1.20000
AFIX 0
C10 1 0.289754 0.527594 -0.115605 11.00000 0.12093 0.10648 =
0.12531 0.06192 0.05690 0.02846
AFIX 23
H10A 2 0.284070 0.578348 -0.088070 11.00000 -1.20000
H10B 2 0.248709 0.498867 -0.137957 11.00000 -1.20000
AFIX 0
N11 5 0.167409 0.376527 0.005258 11.00000 0.04002 0.03600 =
0.07642 0.00022 0.02654 0.00544
C12 1 0.147546 0.545490 0.005464 11.00000 0.06027 0.04824 =
0.11727 -0.00981 0.03733 0.01940
C13 1 0.089340 0.511966 0.020841 11.00000 0.08393 0.07375 =
0.22835 -0.02678 0.07757 0.01556
AFIX 137
H13A 2 0.102284 0.468124 0.056590 11.00000 -1.50000
H13B 2 0.060300 0.481191 -0.016729 11.00000 -1.50000
H13C 2 0.068775 0.565468 0.032347 11.00000 -1.50000
AFIX 0
C14 1 0.128585 0.590327 -0.061768 11.00000 0.12196 0.09233 =
0.14585 0.02244 0.03513 0.06092
AFIX 137
H14A 2 0.105102 0.647488 -0.062266 11.00000 -1.50000
H14B 2 0.102583 0.546819 -0.093510 11.00000 -1.50000
H14C 2 0.166092 0.604995 -0.071994 11.00000 -1.50000
AFIX 0
C15 1 0.187699 0.604122 0.060742 11.00000 0.08870 0.05961 =
0.12832 -0.01986 0.04966 0.00925
C16 1 0.197346 0.697932 0.049308 11.00000 0.16111 0.06478 =
0.25497 -0.04527 0.07200 0.00222
AFIX 137
H16A 2 0.188971 0.707319 0.003573 11.00000 -1.50000
H16B 2 0.240593 0.714956 0.073057 11.00000 -1.50000
H16C 2 0.169202 0.736932 0.063322 11.00000 -1.50000
AFIX 0
C17 1 0.212039 0.562317 0.123594 11.00000 0.21068 0.12166 =
0.12081 -0.03018 0.03225 0.01736
AFIX 93
H17A 2 0.235597 0.598647 0.159139 11.00000 -1.20000
H17B 2 0.204413 0.498626 0.129186 11.00000 -1.20000
AFIX 0
PART 2
C6A 1 0.368728 0.512524 0.129863 -21.00000 0.10074
AFIX 23
H6AA 2 0.329429 0.547523 0.121682 -21.00000 -1.20000
H6AB 2 0.368135 0.458679 0.157317 -21.00000 -1.20000
AFIX 0
C5A 1 0.420903 0.571516 0.162038 -21.00000 0.09658
AFIX 23
H5AA 2 0.457224 0.534844 0.188357 -21.00000 -1.20000
H5AB 2 0.409959 0.617879 0.189351 -21.00000 -1.20000
AFIX 0
C4A 1 0.434404 0.621022 0.101913 -21.00000 0.09590
AFIX 23
H4AA 2 0.403378 0.669445 0.081058 -21.00000 -1.20000
H4AB 2 0.477128 0.646452 0.113542 -21.00000 -1.20000
AFIX 0
C3A 1 0.425552 0.531707 0.062604 -21.00000 0.09154
AFIX 23
H3AA 2 0.418146 0.547472 0.017349 -21.00000 -1.20000
H3AB 2 0.463914 0.493701 0.078202 -21.00000 -1.20000
AFIX 0
HKLF 4
REM 1 in C2/c New: C2/c
REM R1 = 0.0412 for 4942 Fo > 4sig(Fo) and 0.0544 for all 6377 data
REM 334 parameters refined using 137 restraints
END
WGHT 0.0481 4.2857
REM Highest difference peak 0.879, deepest hole -0.800, 1-sigma level 0.109
Q1 1 0.2986 0.4975 -0.1910 11.00000 0.05 0.88
Q2 1 0.3710 0.3520 0.0010 11.00000 0.05 0.66
Q3 1 0.2495 0.3568 -0.0052 11.00000 0.05 0.62
Q4 1 0.3104 0.3478 0.0397 11.00000 0.05 0.62
Q5 1 0.3968 0.4781 0.1463 11.00000 0.05 0.61
Q6 1 0.4046 0.6447 0.0890 11.00000 0.05 0.61
Q7 1 0.3425 0.3528 0.0406 11.00000 0.05 0.60
Q8 1 0.4498 0.5551 0.1681 11.00000 0.05 0.60
Q9 1 0.2771 0.3394 -0.0378 11.00000 0.05 0.59
Q10 1 0.3700 0.3106 0.2486 11.00000 0.05 0.57
REM The information below was added by Olex2.
REM
REM R1 = 0.0412 for 4942 Fo > 4sig(Fo) and 0.0544 for all 20330 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.88, deepest hole -0.80
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0544
REM R1_gt = 0.0412
REM wR_ref = 0.1015
REM GOOF = 1.039
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 20330
REM Reflections_gt = 4942
REM Parameters = n/a
REM Hole = -0.80
REM Peak = 0.88
REM Flack = n/a
;
_olex2_submission_special_instructions 'No special instructions were received'
#===END