# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_da1012_mecn_0m_a
_audit_block_doi 10.5517/ccdc.csd.cc210f2l
_database_code_depnum_ccdc_archive 'CCDC 1877238'
loop_
_audit_author_name
_audit_author_address
'Dimitrios Alexandropoulos'
;Texas A&M University
United States of America
;
_audit_update_record
;
2018-11-05 deposited with the CCDC. 2019-05-09 downloaded from the CCDC.
;
_audit_creation_date 2018-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'C30 H44 B2 Dy N12, C15 H22 B Cl3 Dy N6, C H2 Cl2'
_chemical_formula_sum 'C46 H68 B3 Cl5 Dy2 N18'
_chemical_formula_weight 1407.86
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 10.2885(5)
_cell_length_b 36.2677(19)
_cell_length_c 16.0699(9)
_cell_angle_alpha 90
_cell_angle_beta 92.5040(16)
_cell_angle_gamma 90
_cell_volume 5990.6(5)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9387
_cell_measurement_temperature 110
_cell_measurement_theta_max 25.722
_cell_measurement_theta_min 2.398
_shelx_estimated_absorpt_T_max 0.853
_shelx_estimated_absorpt_T_min 0.610
_exptl_absorpt_coefficient_mu 2.747
_exptl_absorpt_correction_T_max 0.7453
_exptl_absorpt_correction_T_min 0.6342
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0851 before and 0.0634 after correction. The Ratio of minimum to maximum transmission is 0.8509. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear whiteish colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier whiteish
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.561
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2808
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.19
_exptl_crystal_size_min 0.06
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0483
_diffrn_reflns_av_unetI/netI 0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 44
_diffrn_reflns_limit_k_min -44
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 195830
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.790
_diffrn_reflns_theta_max 25.790
_diffrn_reflns_theta_min 2.059
_diffrn_ambient_temperature 110.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device 'three-circle diffractometer'
_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 10111
_reflns_number_total 11476
_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 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_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 ?
_refine_diff_density_max 0.765
_refine_diff_density_min -0.685
_refine_diff_density_rms 0.090
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.099
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 685
_refine_ls_number_reflns 11476
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0326
_refine_ls_R_factor_gt 0.0244
_refine_ls_restrained_S_all 1.099
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0093P)^2^+12.5212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0438
_refine_ls_wR_factor_ref 0.0459
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All B(H) groups, All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
B1(H1), B2(H2), B3(H3A)
2.b Secondary CH2 refined with riding coordinates:
C46(H46A,H46B)
2.c Aromatic/amide H refined with riding coordinates:
C3(H3), C8(H8), C13(H13), C18(H18), C23(H23), C28(H28), C33(H33), C38(H38),
C43(H43)
2.d Idealised Me refined as rotating group:
C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C20(H20A,H20B,
H20C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C30(H30A,
H30B,H30C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C45(H45A,H45B,H45C)
;
_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
Dy1 Dy 0.50669(2) 0.42126(2) 0.67303(2) 0.01129(4) Uani 1 1 d . . . . .
N1 N 0.3345(2) 0.40502(6) 0.76054(14) 0.0154(5) Uani 1 1 d . . . . .
N2 N 0.2498(2) 0.37749(6) 0.73452(14) 0.0153(5) Uani 1 1 d . . . . .
N3 N 0.5142(2) 0.35703(6) 0.64748(14) 0.0153(5) Uani 1 1 d . . . . .
N4 N 0.3985(2) 0.33780(6) 0.64972(14) 0.0136(5) Uani 1 1 d . . . . .
N5 N 0.3306(2) 0.41529(6) 0.57355(14) 0.0125(5) Uani 1 1 d . . . . .
N6 N 0.2501(2) 0.38514(6) 0.57798(14) 0.0128(5) Uani 1 1 d . . . . .
N7 N 0.6718(2) 0.41650(6) 0.78117(14) 0.0160(5) Uani 1 1 d . . . . .
N8 N 0.7652(2) 0.44395(6) 0.78835(14) 0.0145(5) Uani 1 1 d . . . . .
N9 N 0.5288(2) 0.48527(6) 0.70129(14) 0.0126(5) Uani 1 1 d . . . . .
N10 N 0.6499(2) 0.49910(6) 0.72384(14) 0.0120(5) Uani 1 1 d . . . . .
N11 N 0.6874(2) 0.43785(6) 0.59497(14) 0.0128(5) Uani 1 1 d . . . . .
N12 N 0.7865(2) 0.45776(6) 0.63486(14) 0.0139(5) Uani 1 1 d . . . . .
C1 C 0.3698(4) 0.44538(9) 0.8833(2) 0.0301(8) Uani 1 1 d . . . . .
H1A H 0.448350 0.434807 0.910421 0.045 Uiso 1 1 calc GR . . . .
H1B H 0.314466 0.455716 0.925571 0.045 Uiso 1 1 calc GR . . . .
H1C H 0.394281 0.464921 0.844861 0.045 Uiso 1 1 calc GR . . . .
C2 C 0.2969(3) 0.41593(8) 0.83588(18) 0.0196(7) Uani 1 1 d . . . . .
C3 C 0.1897(3) 0.39562(9) 0.85781(19) 0.0251(7) Uani 1 1 d . . . . .
H3 H 0.144205 0.397759 0.907777 0.030 Uiso 1 1 calc R . . . .
C4 C 0.1621(3) 0.37181(9) 0.79313(19) 0.0218(7) Uani 1 1 d . . . . .
C5 C 0.0559(3) 0.34373(11) 0.7838(2) 0.0367(9) Uani 1 1 d . . . . .
H5A H 0.006203 0.347860 0.731267 0.055 Uiso 1 1 calc GR . . . .
H5B H -0.002003 0.345966 0.830393 0.055 Uiso 1 1 calc GR . . . .
H5C H 0.094070 0.318969 0.783797 0.055 Uiso 1 1 calc GR . . . .
C6 C 0.7489(3) 0.34238(9) 0.6420(2) 0.0327(8) Uani 1 1 d . . . . .
H6A H 0.768570 0.348497 0.584542 0.049 Uiso 1 1 calc GR . . . .
H6B H 0.804088 0.321834 0.661562 0.049 Uiso 1 1 calc GR . . . .
H6C H 0.765695 0.363906 0.677760 0.049 Uiso 1 1 calc GR . . . .
C7 C 0.6091(3) 0.33154(8) 0.64549(18) 0.0185(6) Uani 1 1 d . . . . .
C8 C 0.5564(3) 0.29660(8) 0.64700(19) 0.0228(7) Uani 1 1 d . . . . .
H8 H 0.602297 0.273881 0.646345 0.027 Uiso 1 1 calc R . . . .
C9 C 0.4237(3) 0.30132(8) 0.64967(18) 0.0186(6) Uani 1 1 d . . . . .
C10 C 0.3205(3) 0.27277(8) 0.6511(2) 0.0307(8) Uani 1 1 d . . . . .
H10A H 0.266111 0.277098 0.698694 0.046 Uiso 1 1 calc GR . . . .
H10B H 0.360617 0.248325 0.656100 0.046 Uiso 1 1 calc GR . . . .
H10C H 0.266535 0.274041 0.599360 0.046 Uiso 1 1 calc GR . . . .
C11 C 0.3648(3) 0.46771(8) 0.47995(18) 0.0201(7) Uani 1 1 d . . . . .
H11A H 0.303760 0.488456 0.480243 0.030 Uiso 1 1 calc GR . . . .
H11B H 0.398472 0.465013 0.424171 0.030 Uiso 1 1 calc GR . . . .
H11C H 0.437127 0.472348 0.520289 0.030 Uiso 1 1 calc GR . . . .
C12 C 0.2963(3) 0.43324(8) 0.50298(18) 0.0153(6) Uani 1 1 d . . . . .
C13 C 0.1942(3) 0.41474(8) 0.46183(18) 0.0204(7) Uani 1 1 d . . . . .
H13 H 0.151336 0.421487 0.410513 0.025 Uiso 1 1 calc R . . . .
C14 C 0.1676(3) 0.38462(8) 0.51060(18) 0.0183(6) Uani 1 1 d . . . . .
C15 C 0.0676(3) 0.35534(10) 0.4952(2) 0.0309(8) Uani 1 1 d . . . . .
H15A H 0.110391 0.331251 0.492791 0.046 Uiso 1 1 calc GR . . . .
H15B H 0.019844 0.360156 0.442223 0.046 Uiso 1 1 calc GR . . . .
H15C H 0.006845 0.355393 0.540514 0.046 Uiso 1 1 calc GR . . . .
C16 C 0.9472(3) 0.46395(9) 0.8859(2) 0.0285(8) Uani 1 1 d . . . . .
H16A H 1.013288 0.464442 0.843769 0.043 Uiso 1 1 calc GR . . . .
H16B H 0.986672 0.455395 0.938997 0.043 Uiso 1 1 calc GR . . . .
H16C H 0.911943 0.488811 0.892805 0.043 Uiso 1 1 calc GR . . . .
C17 C 0.8401(3) 0.43839(8) 0.85843(18) 0.0187(6) Uani 1 1 d . . . . .
C18 C 0.7968(3) 0.40706(8) 0.89643(18) 0.0216(7) Uani 1 1 d . . . . .
H18 H 0.831603 0.396323 0.946524 0.026 Uiso 1 1 calc R . . . .
C19 C 0.6926(3) 0.39423(8) 0.84741(18) 0.0183(6) Uani 1 1 d . . . . .
C20 C 0.6104(3) 0.36091(8) 0.86006(19) 0.0250(7) Uani 1 1 d . . . . .
H20A H 0.521137 0.365863 0.839244 0.037 Uiso 1 1 calc GR . . . .
H20B H 0.610409 0.355014 0.919570 0.037 Uiso 1 1 calc GR . . . .
H20C H 0.645653 0.340014 0.829655 0.037 Uiso 1 1 calc GR . . . .
C21 C 0.7514(3) 0.55771(8) 0.77747(19) 0.0207(7) Uani 1 1 d . . . . .
H21A H 0.785793 0.547793 0.830712 0.031 Uiso 1 1 calc GR . . . .
H21B H 0.722969 0.583225 0.785275 0.031 Uiso 1 1 calc GR . . . .
H21C H 0.819481 0.557089 0.736718 0.031 Uiso 1 1 calc GR . . . .
C22 C 0.6386(3) 0.53495(8) 0.74659(17) 0.0147(6) Uani 1 1 d . . . . .
C23 C 0.5083(3) 0.54432(8) 0.73679(17) 0.0156(6) Uani 1 1 d . . . . .
H23 H 0.470749 0.567717 0.747036 0.019 Uiso 1 1 calc R . . . .
C24 C 0.4439(3) 0.51295(8) 0.70919(17) 0.0146(6) Uani 1 1 d . . . . .
C25 C 0.3023(3) 0.50744(8) 0.68811(19) 0.0204(7) Uani 1 1 d . . . . .
H25A H 0.289398 0.503101 0.628124 0.031 Uiso 1 1 calc GR . . . .
H25B H 0.253992 0.529498 0.703652 0.031 Uiso 1 1 calc GR . . . .
H25C H 0.270686 0.486107 0.718722 0.031 Uiso 1 1 calc GR . . . .
C26 C 1.0143(3) 0.47711(12) 0.6111(2) 0.0401(10) Uani 1 1 d . . . . .
H26A H 0.998028 0.503011 0.624642 0.060 Uiso 1 1 calc GR . . . .
H26B H 1.074218 0.475738 0.565505 0.060 Uiso 1 1 calc GR . . . .
H26C H 1.052853 0.464575 0.660280 0.060 Uiso 1 1 calc GR . . . .
C27 C 0.8889(3) 0.45885(9) 0.58526(19) 0.0204(7) Uani 1 1 d . . . . .
C28 C 0.8561(3) 0.44009(9) 0.51249(19) 0.0218(7) Uani 1 1 d . . . . .
H28 H 0.909082 0.436584 0.466160 0.026 Uiso 1 1 calc R . . . .
C29 C 0.7309(3) 0.42750(8) 0.52087(17) 0.0149(6) Uani 1 1 d . . . . .
C30 C 0.6476(3) 0.40533(8) 0.46089(18) 0.0206(7) Uani 1 1 d . . . . .
H30A H 0.593478 0.388343 0.491805 0.031 Uiso 1 1 calc GR . . . .
H30B H 0.703082 0.391215 0.424440 0.031 Uiso 1 1 calc GR . . . .
H30C H 0.591597 0.421909 0.427122 0.031 Uiso 1 1 calc GR . . . .
B1 B 0.2645(3) 0.35730(9) 0.65063(19) 0.0141(7) Uani 1 1 d . . . . .
H1 H 0.194366 0.338319 0.643854 0.017 Uiso 1 1 calc R . . . .
B2 B 0.7729(3) 0.47468(9) 0.7224(2) 0.0150(7) Uani 1 1 d . . . . .
H2 H 0.850987 0.490305 0.736188 0.018 Uiso 1 1 calc R . . . .
Dy2 Dy 0.90394(2) 0.35372(2) 1.16998(2) 0.01088(4) Uani 1 1 d . . . . .
Cl1 Cl 1.08519(7) 0.30894(2) 1.22359(5) 0.02601(17) Uani 1 1 d . . . . .
Cl2 Cl 0.90305(7) 0.39881(2) 1.29563(4) 0.02235(16) Uani 1 1 d . . . . .
Cl3 Cl 1.03312(7) 0.39606(2) 1.07382(4) 0.01738(15) Uani 1 1 d . . . . .
N13 N 0.7393(2) 0.31257(6) 1.22747(14) 0.0138(5) Uani 1 1 d . . . . .
N14 N 0.6375(2) 0.29884(6) 1.17803(14) 0.0130(5) Uani 1 1 d . . . . .
N15 N 0.8524(2) 0.31229(6) 1.05311(14) 0.0134(5) Uani 1 1 d . . . . .
N16 N 0.7266(2) 0.30120(6) 1.03380(14) 0.0121(5) Uani 1 1 d . . . . .
N17 N 0.7018(2) 0.37786(6) 1.10646(14) 0.0127(5) Uani 1 1 d . . . . .
N18 N 0.5982(2) 0.35467(6) 1.08810(14) 0.0135(5) Uani 1 1 d . . . . .
C31 C 0.8218(3) 0.30551(9) 1.37361(18) 0.0234(7) Uani 1 1 d . . . . .
H31A H 0.910886 0.300644 1.357331 0.035 Uiso 1 1 calc GR . . . .
H31B H 0.802229 0.290060 1.421498 0.035 Uiso 1 1 calc GR . . . .
H31C H 0.813405 0.331555 1.388702 0.035 Uiso 1 1 calc GR . . . .
C32 C 0.7288(3) 0.29679(8) 1.30251(18) 0.0173(6) Uani 1 1 d . . . . .
C33 C 0.6228(3) 0.27311(8) 1.30140(18) 0.0183(6) Uani 1 1 d . . . . .
H33 H 0.594885 0.258435 1.346203 0.022 Uiso 1 1 calc R . . . .
C34 C 0.5663(3) 0.27518(8) 1.22222(18) 0.0158(6) Uani 1 1 d . . . . .
C35 C 0.4480(3) 0.25598(9) 1.1868(2) 0.0247(7) Uani 1 1 d . . . . .
H35A H 0.381116 0.274257 1.171259 0.037 Uiso 1 1 calc GR . . . .
H35B H 0.414733 0.239119 1.228466 0.037 Uiso 1 1 calc GR . . . .
H35C H 0.470583 0.241961 1.137292 0.037 Uiso 1 1 calc GR . . . .
C36 C 1.0711(3) 0.30204(9) 0.9983(2) 0.0249(7) Uani 1 1 d . . . . .
H36A H 1.091209 0.328326 0.992965 0.037 Uiso 1 1 calc GR . . . .
H36B H 1.107814 0.288460 0.952082 0.037 Uiso 1 1 calc GR . . . .
H36C H 1.108968 0.292737 1.051228 0.037 Uiso 1 1 calc GR . . . .
C37 C 0.9268(3) 0.29684(8) 0.99607(18) 0.0170(6) Uani 1 1 d . . . . .
C38 C 0.8495(3) 0.27621(8) 0.93984(18) 0.0195(6) Uani 1 1 d . . . . .
H38 H 0.877826 0.262768 0.893224 0.023 Uiso 1 1 calc R . . . .
C39 C 0.7244(3) 0.27923(8) 0.96538(17) 0.0165(6) Uani 1 1 d . . . . .
C40 C 0.6031(3) 0.26194(9) 0.92878(19) 0.0239(7) Uani 1 1 d . . . . .
H40A H 0.565909 0.245510 0.969925 0.036 Uiso 1 1 calc GR . . . .
H40B H 0.623749 0.247713 0.879218 0.036 Uiso 1 1 calc GR . . . .
H40C H 0.539973 0.281246 0.913186 0.036 Uiso 1 1 calc GR . . . .
C41 C 0.7414(3) 0.44535(8) 1.1097(2) 0.0234(7) Uani 1 1 d . . . . .
H41A H 0.801791 0.441559 1.157749 0.035 Uiso 1 1 calc GR . . . .
H41B H 0.687586 0.467121 1.119154 0.035 Uiso 1 1 calc GR . . . .
H41C H 0.790734 0.449063 1.059560 0.035 Uiso 1 1 calc GR . . . .
C42 C 0.6561(3) 0.41230(8) 1.09832(17) 0.0158(6) Uani 1 1 d . . . . .
C43 C 0.5236(3) 0.41124(8) 1.07653(18) 0.0198(7) Uani 1 1 d . . . . .
H43 H 0.467669 0.431830 1.067529 0.024 Uiso 1 1 calc R . . . .
C44 C 0.4896(3) 0.37482(8) 1.07058(17) 0.0174(6) Uani 1 1 d . . . . .
C45 C 0.3600(3) 0.35779(9) 1.0508(2) 0.0267(7) Uani 1 1 d . . . . .
H45A H 0.363973 0.343212 0.999593 0.040 Uiso 1 1 calc GR . . . .
H45B H 0.294469 0.377222 1.042921 0.040 Uiso 1 1 calc GR . . . .
H45C H 0.336501 0.341725 1.096790 0.040 Uiso 1 1 calc GR . . . .
B3 B 0.6132(3) 0.31243(9) 1.0881(2) 0.0138(7) Uani 1 1 d . . . . .
H3A H 0.530972 0.301120 1.064447 0.017 Uiso 1 1 calc R . . . .
Cl4 Cl 0.41193(10) 0.32342(2) 0.44501(5) 0.0397(2) Uani 1 1 d . . . . .
Cl5 Cl 0.45732(9) 0.35840(2) 0.28578(6) 0.0390(2) Uani 1 1 d . . . . .
C46 C 0.3471(4) 0.33702(16) 0.3490(2) 0.0637(15) Uani 1 1 d . . . . .
H46A H 0.274127 0.354193 0.357733 0.076 Uiso 1 1 calc R . . . .
H46B H 0.310977 0.315071 0.319600 0.076 Uiso 1 1 calc R . . . .
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 0.01139(7) 0.01029(7) 0.01205(7) 0.00039(5) -0.00116(5) -0.00254(5)
N1 0.0200(13) 0.0156(12) 0.0109(12) -0.0004(10) 0.0037(10) -0.0005(10)
N2 0.0124(12) 0.0166(13) 0.0171(13) 0.0029(10) 0.0009(10) -0.0014(10)
N3 0.0133(12) 0.0143(12) 0.0184(13) -0.0003(10) 0.0003(10) -0.0027(10)
N4 0.0164(12) 0.0105(12) 0.0139(12) -0.0009(9) 0.0008(10) -0.0052(10)
N5 0.0122(12) 0.0112(12) 0.0140(12) 0.0018(9) 0.0006(9) -0.0025(9)
N6 0.0103(12) 0.0156(12) 0.0124(12) 0.0010(10) 0.0007(9) -0.0037(9)
N7 0.0171(13) 0.0160(13) 0.0147(12) 0.0036(10) -0.0030(10) -0.0004(10)
N8 0.0133(12) 0.0153(12) 0.0147(12) -0.0007(10) -0.0041(10) 0.0005(10)
N9 0.0107(12) 0.0123(12) 0.0146(12) -0.0011(10) -0.0019(9) -0.0023(9)
N10 0.0125(12) 0.0114(12) 0.0120(12) -0.0009(9) -0.0020(9) -0.0035(9)
N11 0.0129(12) 0.0127(12) 0.0127(12) 0.0003(10) -0.0017(10) -0.0030(9)
N12 0.0110(12) 0.0163(12) 0.0143(12) 0.0007(10) -0.0014(10) -0.0022(10)
C1 0.049(2) 0.0254(18) 0.0160(16) -0.0037(14) 0.0027(15) 0.0039(16)
C2 0.0238(16) 0.0214(16) 0.0136(15) 0.0031(12) 0.0013(12) 0.0082(13)
C3 0.0252(17) 0.0358(19) 0.0149(16) 0.0044(14) 0.0092(13) 0.0082(14)
C4 0.0165(16) 0.0307(18) 0.0186(16) 0.0082(14) 0.0056(13) 0.0023(13)
C5 0.0223(18) 0.058(3) 0.030(2) 0.0063(18) 0.0104(15) -0.0145(17)
C6 0.0185(17) 0.0261(19) 0.054(2) 0.0023(17) 0.0034(16) 0.0049(14)
C7 0.0178(15) 0.0187(16) 0.0189(15) 0.0000(12) -0.0008(12) 0.0031(12)
C8 0.0295(18) 0.0130(15) 0.0260(17) 0.0019(13) 0.0015(14) 0.0062(13)
C9 0.0284(17) 0.0117(15) 0.0157(15) 0.0009(12) 0.0005(13) -0.0031(12)
C10 0.035(2) 0.0142(16) 0.043(2) 0.0049(15) 0.0018(16) -0.0080(14)
C11 0.0225(16) 0.0222(16) 0.0153(15) 0.0068(13) -0.0017(13) -0.0032(13)
C12 0.0147(15) 0.0150(15) 0.0162(15) 0.0026(12) 0.0006(12) 0.0022(11)
C13 0.0199(16) 0.0257(17) 0.0150(15) 0.0055(13) -0.0064(12) -0.0041(13)
C14 0.0140(15) 0.0222(16) 0.0185(15) -0.0004(13) -0.0027(12) -0.0035(12)
C15 0.0282(18) 0.037(2) 0.0270(18) 0.0043(16) -0.0095(15) -0.0148(16)
C16 0.0276(18) 0.0310(19) 0.0254(18) -0.0015(15) -0.0160(14) 0.0000(15)
C17 0.0184(15) 0.0226(16) 0.0146(15) -0.0034(13) -0.0051(12) 0.0069(13)
C18 0.0245(17) 0.0261(17) 0.0135(15) 0.0023(13) -0.0055(13) 0.0083(13)
C19 0.0251(16) 0.0167(15) 0.0133(15) 0.0019(12) 0.0015(12) 0.0057(13)
C20 0.0329(18) 0.0233(17) 0.0187(16) 0.0090(13) 0.0011(14) -0.0007(14)
C21 0.0213(16) 0.0143(15) 0.0260(17) -0.0071(13) -0.0043(13) -0.0065(12)
C22 0.0202(15) 0.0121(14) 0.0116(14) 0.0004(11) -0.0012(12) -0.0025(12)
C23 0.0193(15) 0.0133(14) 0.0141(15) -0.0015(12) -0.0010(12) 0.0020(12)
C24 0.0158(15) 0.0160(15) 0.0119(14) 0.0003(12) -0.0007(11) -0.0001(12)
C25 0.0152(15) 0.0221(16) 0.0238(17) -0.0042(13) -0.0016(13) 0.0006(12)
C26 0.0184(18) 0.070(3) 0.032(2) -0.0178(19) 0.0067(15) -0.0177(18)
C27 0.0120(15) 0.0276(17) 0.0219(16) -0.0014(13) 0.0020(12) -0.0040(12)
C28 0.0165(16) 0.0313(18) 0.0180(16) -0.0035(14) 0.0041(13) -0.0018(13)
C29 0.0172(15) 0.0125(14) 0.0151(15) 0.0002(11) 0.0006(12) 0.0016(11)
C30 0.0195(16) 0.0241(17) 0.0182(16) -0.0054(13) 0.0026(13) -0.0017(13)
B1 0.0115(15) 0.0161(17) 0.0144(16) 0.0002(13) -0.0025(13) -0.0055(13)
B2 0.0114(16) 0.0148(17) 0.0184(17) -0.0015(13) -0.0033(13) -0.0037(13)
Dy2 0.00961(6) 0.01213(7) 0.01080(7) -0.00086(5) -0.00067(5) -0.00043(5)
Cl1 0.0196(4) 0.0260(4) 0.0317(4) 0.0029(3) -0.0072(3) 0.0068(3)
Cl2 0.0300(4) 0.0231(4) 0.0139(4) -0.0055(3) 0.0013(3) -0.0007(3)
Cl3 0.0139(3) 0.0226(4) 0.0157(3) 0.0015(3) 0.0017(3) -0.0034(3)
N13 0.0121(12) 0.0153(12) 0.0138(12) 0.0009(10) -0.0012(10) 0.0002(9)
N14 0.0104(12) 0.0143(12) 0.0143(12) 0.0008(10) -0.0001(9) 0.0000(9)
N15 0.0097(12) 0.0138(12) 0.0165(12) -0.0031(10) -0.0009(10) -0.0002(9)
N16 0.0110(12) 0.0127(12) 0.0127(12) -0.0002(10) -0.0002(9) -0.0021(9)
N17 0.0128(12) 0.0144(12) 0.0108(12) 0.0000(10) 0.0004(9) 0.0001(10)
N18 0.0105(11) 0.0180(12) 0.0122(12) 0.0004(10) 0.0005(9) 0.0006(10)
C31 0.0252(17) 0.0277(18) 0.0170(16) 0.0076(13) -0.0040(13) -0.0029(14)
C32 0.0194(15) 0.0147(15) 0.0176(15) 0.0015(12) 0.0012(12) 0.0043(12)
C33 0.0210(16) 0.0158(15) 0.0186(16) 0.0043(12) 0.0060(12) -0.0032(12)
C34 0.0151(14) 0.0128(14) 0.0199(15) 0.0015(12) 0.0051(12) -0.0005(11)
C35 0.0191(16) 0.0256(18) 0.0295(18) 0.0026(14) 0.0017(14) -0.0086(13)
C36 0.0181(16) 0.0299(18) 0.0272(18) -0.0114(15) 0.0056(13) 0.0028(13)
C37 0.0175(15) 0.0145(15) 0.0191(15) -0.0013(12) 0.0033(12) 0.0005(12)
C38 0.0240(16) 0.0175(16) 0.0172(15) -0.0066(12) 0.0032(13) 0.0012(13)
C39 0.0222(16) 0.0134(15) 0.0138(15) -0.0024(12) -0.0007(12) -0.0004(12)
C40 0.0267(17) 0.0246(17) 0.0199(16) -0.0084(13) -0.0041(13) -0.0068(14)
C41 0.0314(18) 0.0126(15) 0.0263(17) -0.0013(13) 0.0027(14) 0.0053(13)
C42 0.0222(16) 0.0174(15) 0.0081(14) 0.0000(11) 0.0033(12) 0.0061(12)
C43 0.0227(16) 0.0228(17) 0.0139(15) -0.0002(12) -0.0006(12) 0.0128(13)
C44 0.0130(14) 0.0278(17) 0.0114(14) -0.0007(12) 0.0010(11) 0.0073(12)
C45 0.0143(15) 0.037(2) 0.0281(18) -0.0001(15) -0.0036(13) 0.0069(14)
B3 0.0118(16) 0.0142(17) 0.0151(16) -0.0018(13) -0.0018(13) -0.0023(13)
Cl4 0.0585(6) 0.0318(5) 0.0300(5) -0.0014(4) 0.0143(4) -0.0034(4)
Cl5 0.0504(6) 0.0272(5) 0.0397(5) 0.0125(4) 0.0056(4) 0.0019(4)
C46 0.031(2) 0.139(5) 0.021(2) 0.000(2) 0.0007(17) -0.012(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
Dy1 N1 2.383(2) . ?
Dy1 N3 2.367(2) . ?
Dy1 N5 2.373(2) . ?
Dy1 N7 2.383(2) . ?
Dy1 N9 2.375(2) . ?
Dy1 N11 2.366(2) . ?
N1 N2 1.378(3) . ?
N1 C2 1.347(4) . ?
N2 C4 1.348(4) . ?
N2 B1 1.547(4) . ?
N3 N4 1.382(3) . ?
N3 C7 1.346(4) . ?
N4 C9 1.348(4) . ?
N4 B1 1.550(4) . ?
N5 N6 1.375(3) . ?
N5 C12 1.341(4) . ?
N6 C14 1.346(4) . ?
N6 B1 1.546(4) . ?
N7 N8 1.385(3) . ?
N7 C19 1.346(4) . ?
N8 C17 1.352(4) . ?
N8 B2 1.542(4) . ?
N9 N10 1.377(3) . ?
N9 C24 1.340(4) . ?
N10 C22 1.357(4) . ?
N10 B2 1.546(4) . ?
N11 N12 1.384(3) . ?
N11 C29 1.344(4) . ?
N12 C27 1.349(4) . ?
N12 B2 1.547(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.494(4) . ?
C2 C3 1.385(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.371(5) . ?
C4 C5 1.496(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 C7 1.494(4) . ?
C7 C8 1.379(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.379(4) . ?
C9 C10 1.484(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C11 C12 1.490(4) . ?
C12 C13 1.390(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.379(4) . ?
C14 C15 1.492(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16 C17 1.492(4) . ?
C17 C18 1.373(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.383(4) . ?
C19 C20 1.494(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C21 C22 1.491(4) . ?
C22 C23 1.385(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.380(4) . ?
C24 C25 1.494(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C26 C27 1.493(4) . ?
C27 C28 1.382(4) . ?
C28 H28 0.9500 . ?
C28 C29 1.379(4) . ?
C29 C30 1.496(4) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
B1 H1 1.0000 . ?
B2 H2 1.0000 . ?
Dy2 Cl1 2.5917(7) . ?
Dy2 Cl2 2.5989(7) . ?
Dy2 Cl3 2.5869(7) . ?
Dy2 N13 2.467(2) . ?
Dy2 N15 2.445(2) . ?
Dy2 N17 2.439(2) . ?
N13 N14 1.379(3) . ?
N13 C32 1.343(4) . ?
N14 C34 1.350(4) . ?
N14 B3 1.538(4) . ?
N15 N16 1.378(3) . ?
N15 C37 1.342(4) . ?
N16 C39 1.357(4) . ?
N16 B3 1.541(4) . ?
N17 N18 1.379(3) . ?
N17 C42 1.339(4) . ?
N18 C44 1.355(4) . ?
N18 B3 1.539(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C31 C32 1.492(4) . ?
C32 C33 1.388(4) . ?
C33 H33 0.9500 . ?
C33 C34 1.378(4) . ?
C34 C35 1.494(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C36 C37 1.496(4) . ?
C37 C38 1.395(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.372(4) . ?
C39 C40 1.495(4) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C41 C42 1.492(4) . ?
C42 C43 1.393(4) . ?
C43 H43 0.9500 . ?
C43 C44 1.369(4) . ?
C44 C45 1.491(4) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
B3 H3A 1.0000 . ?
Cl4 C46 1.725(4) . ?
Cl5 C46 1.738(4) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Dy1 N1 83.68(8) . . ?
N3 Dy1 N5 79.81(8) . . ?
N3 Dy1 N7 91.59(8) . . ?
N3 Dy1 N9 172.60(8) . . ?
N5 Dy1 N1 79.02(8) . . ?
N5 Dy1 N7 169.63(8) . . ?
N5 Dy1 N9 106.38(8) . . ?
N7 Dy1 N1 94.38(8) . . ?
N9 Dy1 N1 101.32(8) . . ?
N9 Dy1 N7 82.64(8) . . ?
N11 Dy1 N1 175.85(8) . . ?
N11 Dy1 N3 97.24(8) . . ?
N11 Dy1 N5 105.12(8) . . ?
N11 Dy1 N7 81.56(8) . . ?
N11 Dy1 N9 77.39(8) . . ?
N2 N1 Dy1 118.46(16) . . ?
C2 N1 Dy1 135.1(2) . . ?
C2 N1 N2 106.4(2) . . ?
N1 N2 B1 121.5(2) . . ?
C4 N2 N1 109.4(2) . . ?
C4 N2 B1 129.1(2) . . ?
N4 N3 Dy1 117.24(16) . . ?
C7 N3 Dy1 135.16(19) . . ?
C7 N3 N4 106.3(2) . . ?
N3 N4 B1 122.5(2) . . ?
C9 N4 N3 109.2(2) . . ?
C9 N4 B1 128.2(2) . . ?
N6 N5 Dy1 118.76(16) . . ?
C12 N5 Dy1 133.61(18) . . ?
C12 N5 N6 107.1(2) . . ?
N5 N6 B1 121.4(2) . . ?
C14 N6 N5 109.2(2) . . ?
C14 N6 B1 129.4(2) . . ?
N8 N7 Dy1 118.60(16) . . ?
C19 N7 Dy1 134.8(2) . . ?
C19 N7 N8 106.2(2) . . ?
N7 N8 B2 121.2(2) . . ?
C17 N8 N7 109.3(2) . . ?
C17 N8 B2 129.5(2) . . ?
N10 N9 Dy1 118.99(16) . . ?
C24 N9 Dy1 133.86(18) . . ?
C24 N9 N10 106.7(2) . . ?
N9 N10 B2 121.3(2) . . ?
C22 N10 N9 109.5(2) . . ?
C22 N10 B2 129.2(2) . . ?
N12 N11 Dy1 117.87(16) . . ?
C29 N11 Dy1 134.31(18) . . ?
C29 N11 N12 106.8(2) . . ?
N11 N12 B2 122.3(2) . . ?
C27 N12 N11 108.7(2) . . ?
C27 N12 B2 129.1(2) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
N1 C2 C1 120.7(3) . . ?
N1 C2 C3 109.6(3) . . ?
C3 C2 C1 129.7(3) . . ?
C2 C3 H3 126.8 . . ?
C4 C3 C2 106.4(3) . . ?
C4 C3 H3 126.8 . . ?
N2 C4 C3 108.1(3) . . ?
N2 C4 C5 122.8(3) . . ?
C3 C4 C5 129.1(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
N3 C7 C6 121.4(3) . . ?
N3 C7 C8 110.1(3) . . ?
C8 C7 C6 128.5(3) . . ?
C7 C8 H8 127.0 . . ?
C7 C8 C9 106.1(3) . . ?
C9 C8 H8 126.9 . . ?
N4 C9 C8 108.2(3) . . ?
N4 C9 C10 123.2(3) . . ?
C8 C9 C10 128.6(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
N5 C12 C11 120.5(2) . . ?
N5 C12 C13 109.5(2) . . ?
C13 C12 C11 130.0(3) . . ?
C12 C13 H13 127.0 . . ?
C14 C13 C12 106.0(3) . . ?
C14 C13 H13 127.0 . . ?
N6 C14 C13 108.2(2) . . ?
N6 C14 C15 123.3(3) . . ?
C13 C14 C15 128.5(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 C16 H16A 109.5 . . ?
C17 C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
N8 C17 C16 122.7(3) . . ?
N8 C17 C18 108.1(3) . . ?
C18 C17 C16 129.2(3) . . ?
C17 C18 H18 126.8 . . ?
C17 C18 C19 106.5(3) . . ?
C19 C18 H18 126.8 . . ?
N7 C19 C18 109.9(3) . . ?
N7 C19 C20 121.4(3) . . ?
C18 C19 C20 128.6(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
N10 C22 C21 123.1(3) . . ?
N10 C22 C23 107.3(2) . . ?
C23 C22 C21 129.6(3) . . ?
C22 C23 H23 126.8 . . ?
C24 C23 C22 106.5(2) . . ?
C24 C23 H23 126.8 . . ?
N9 C24 C23 110.0(2) . . ?
N9 C24 C25 120.8(2) . . ?
C23 C24 C25 129.3(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C27 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
C27 C26 H26C 109.5 . . ?
N12 C27 C26 122.4(3) . . ?
N12 C27 C28 108.6(3) . . ?
C28 C27 C26 129.0(3) . . ?
C27 C28 H28 127.0 . . ?
C29 C28 C27 105.9(3) . . ?
C29 C28 H28 127.0 . . ?
N11 C29 C28 110.0(3) . . ?
N11 C29 C30 121.2(2) . . ?
C28 C29 C30 128.8(3) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N2 B1 N4 110.2(2) . . ?
N2 B1 H1 108.8 . . ?
N4 B1 H1 108.8 . . ?
N6 B1 N2 109.8(2) . . ?
N6 B1 N4 110.3(2) . . ?
N6 B1 H1 108.8 . . ?
N8 B2 N10 109.7(2) . . ?
N8 B2 N12 110.4(2) . . ?
N8 B2 H2 108.8 . . ?
N10 B2 N12 110.3(2) . . ?
N10 B2 H2 108.8 . . ?
N12 B2 H2 108.8 . . ?
Cl1 Dy2 Cl2 99.38(3) . . ?
Cl3 Dy2 Cl1 100.93(2) . . ?
Cl3 Dy2 Cl2 96.31(2) . . ?
N13 Dy2 Cl1 89.57(6) . . ?
N13 Dy2 Cl2 93.67(6) . . ?
N13 Dy2 Cl3 164.12(5) . . ?
N15 Dy2 Cl1 89.94(6) . . ?
N15 Dy2 Cl2 167.30(5) . . ?
N15 Dy2 Cl3 90.33(6) . . ?
N15 Dy2 N13 77.68(8) . . ?
N17 Dy2 Cl1 162.20(6) . . ?
N17 Dy2 Cl2 93.87(6) . . ?
N17 Dy2 Cl3 89.30(6) . . ?
N17 Dy2 N13 77.70(7) . . ?
N17 Dy2 N15 75.34(7) . . ?
N14 N13 Dy2 121.26(16) . . ?
C32 N13 Dy2 132.60(19) . . ?
C32 N13 N14 106.0(2) . . ?
N13 N14 B3 120.9(2) . . ?
C34 N14 N13 110.0(2) . . ?
C34 N14 B3 128.9(2) . . ?
N16 N15 Dy2 121.48(16) . . ?
C37 N15 Dy2 132.10(18) . . ?
C37 N15 N16 106.4(2) . . ?
N15 N16 B3 121.5(2) . . ?
C39 N16 N15 109.6(2) . . ?
C39 N16 B3 128.9(2) . . ?
N18 N17 Dy2 120.48(16) . . ?
C42 N17 Dy2 131.72(19) . . ?
C42 N17 N18 106.4(2) . . ?
N17 N18 B3 122.0(2) . . ?
C44 N18 N17 109.8(2) . . ?
C44 N18 B3 128.2(2) . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
N13 C32 C31 121.6(3) . . ?
N13 C32 C33 110.2(3) . . ?
C33 C32 C31 128.2(3) . . ?
C32 C33 H33 126.9 . . ?
C34 C33 C32 106.1(3) . . ?
C34 C33 H33 126.9 . . ?
N14 C34 C33 107.7(2) . . ?
N14 C34 C35 123.2(3) . . ?
C33 C34 C35 129.1(3) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C37 C36 H36A 109.5 . . ?
C37 C36 H36B 109.5 . . ?
C37 C36 H36C 109.5 . . ?
N15 C37 C36 121.7(3) . . ?
N15 C37 C38 109.9(3) . . ?
C38 C37 C36 128.3(3) . . ?
C37 C38 H38 126.9 . . ?
C39 C38 C37 106.2(3) . . ?
C39 C38 H38 126.9 . . ?
N16 C39 C38 107.9(2) . . ?
N16 C39 C40 123.3(3) . . ?
C38 C39 C40 128.8(3) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
N17 C42 C41 122.3(3) . . ?
N17 C42 C43 109.6(3) . . ?
C43 C42 C41 128.1(3) . . ?
C42 C43 H43 126.6 . . ?
C44 C43 C42 106.8(3) . . ?
C44 C43 H43 126.6 . . ?
N18 C44 C43 107.4(3) . . ?
N18 C44 C45 122.9(3) . . ?
C43 C44 C45 129.7(3) . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N14 B3 N16 110.5(2) . . ?
N14 B3 N18 109.3(2) . . ?
N14 B3 H3A 109.0 . . ?
N16 B3 H3A 109.0 . . ?
N18 B3 N16 110.0(2) . . ?
N18 B3 H3A 109.0 . . ?
Cl4 C46 Cl5 114.4(2) . . ?
Cl4 C46 H46A 108.7 . . ?
Cl4 C46 H46B 108.7 . . ?
Cl5 C46 H46A 108.7 . . ?
Cl5 C46 H46B 108.7 . . ?
H46A C46 H46B 107.6 . . ?
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 N1 N2 C4 178.46(18) . . . . ?
Dy1 N1 N2 B1 0.0(3) . . . . ?
Dy1 N1 C2 C1 1.0(4) . . . . ?
Dy1 N1 C2 C3 -177.9(2) . . . . ?
Dy1 N3 N4 C9 -168.53(18) . . . . ?
Dy1 N3 N4 B1 12.3(3) . . . . ?
Dy1 N3 C7 C6 -14.5(4) . . . . ?
Dy1 N3 C7 C8 165.6(2) . . . . ?
Dy1 N5 N6 C14 -172.40(18) . . . . ?
Dy1 N5 N6 B1 5.8(3) . . . . ?
Dy1 N5 C12 C11 -9.6(4) . . . . ?
Dy1 N5 C12 C13 170.9(2) . . . . ?
Dy1 N7 N8 C17 173.09(18) . . . . ?
Dy1 N7 N8 B2 -7.0(3) . . . . ?
Dy1 N7 C19 C18 -172.0(2) . . . . ?
Dy1 N7 C19 C20 8.5(4) . . . . ?
Dy1 N9 N10 C22 -172.81(17) . . . . ?
Dy1 N9 N10 B2 6.3(3) . . . . ?
Dy1 N9 C24 C23 172.10(19) . . . . ?
Dy1 N9 C24 C25 -8.7(4) . . . . ?
Dy1 N11 N12 C27 169.39(18) . . . . ?
Dy1 N11 N12 B2 -10.2(3) . . . . ?
Dy1 N11 C29 C28 -167.4(2) . . . . ?
Dy1 N11 C29 C30 12.3(4) . . . . ?
N1 N2 C4 C3 -0.1(3) . . . . ?
N1 N2 C4 C5 179.8(3) . . . . ?
N1 N2 B1 N4 60.2(3) . . . . ?
N1 N2 B1 N6 -61.5(3) . . . . ?
N1 C2 C3 C4 -0.2(3) . . . . ?
N2 N1 C2 C1 179.0(3) . . . . ?
N2 N1 C2 C3 0.1(3) . . . . ?
N3 N4 C9 C8 -0.3(3) . . . . ?
N3 N4 C9 C10 -179.5(3) . . . . ?
N3 N4 B1 N2 -68.9(3) . . . . ?
N3 N4 B1 N6 52.5(3) . . . . ?
N3 C7 C8 C9 0.3(3) . . . . ?
N4 N3 C7 C6 179.5(3) . . . . ?
N4 N3 C7 C8 -0.4(3) . . . . ?
N5 N6 C14 C13 -0.1(3) . . . . ?
N5 N6 C14 C15 179.4(3) . . . . ?
N5 N6 B1 N2 58.0(3) . . . . ?
N5 N6 B1 N4 -63.7(3) . . . . ?
N5 C12 C13 C14 0.0(3) . . . . ?
N6 N5 C12 C11 179.4(2) . . . . ?
N6 N5 C12 C13 0.0(3) . . . . ?
N7 N8 C17 C16 -177.8(3) . . . . ?
N7 N8 C17 C18 0.8(3) . . . . ?
N7 N8 B2 N10 66.0(3) . . . . ?
N7 N8 B2 N12 -55.8(3) . . . . ?
N8 N7 C19 C18 0.2(3) . . . . ?
N8 N7 C19 C20 -179.3(3) . . . . ?
N8 C17 C18 C19 -0.6(3) . . . . ?
N9 N10 C22 C21 177.7(2) . . . . ?
N9 N10 C22 C23 -1.2(3) . . . . ?
N9 N10 B2 N8 -65.7(3) . . . . ?
N9 N10 B2 N12 56.0(3) . . . . ?
N10 N9 C24 C23 -0.2(3) . . . . ?
N10 N9 C24 C25 179.0(2) . . . . ?
N10 C22 C23 C24 1.0(3) . . . . ?
N11 N12 C27 C26 -177.7(3) . . . . ?
N11 N12 C27 C28 0.8(3) . . . . ?
N11 N12 B2 N8 67.5(3) . . . . ?
N11 N12 B2 N10 -53.9(3) . . . . ?
N12 N11 C29 C28 0.4(3) . . . . ?
N12 N11 C29 C30 -179.9(2) . . . . ?
N12 C27 C28 C29 -0.5(4) . . . . ?
C1 C2 C3 C4 -179.0(3) . . . . ?
C2 N1 N2 C4 0.0(3) . . . . ?
C2 N1 N2 B1 -178.5(2) . . . . ?
C2 C3 C4 N2 0.2(3) . . . . ?
C2 C3 C4 C5 -179.7(3) . . . . ?
C4 N2 B1 N4 -118.0(3) . . . . ?
C4 N2 B1 N6 120.3(3) . . . . ?
C6 C7 C8 C9 -179.7(3) . . . . ?
C7 N3 N4 C9 0.4(3) . . . . ?
C7 N3 N4 B1 -178.7(2) . . . . ?
C7 C8 C9 N4 0.0(3) . . . . ?
C7 C8 C9 C10 179.2(3) . . . . ?
C9 N4 B1 N2 112.1(3) . . . . ?
C9 N4 B1 N6 -126.5(3) . . . . ?
C11 C12 C13 C14 -179.5(3) . . . . ?
C12 N5 N6 C14 0.1(3) . . . . ?
C12 N5 N6 B1 178.3(2) . . . . ?
C12 C13 C14 N6 0.1(3) . . . . ?
C12 C13 C14 C15 -179.4(3) . . . . ?
C14 N6 B1 N2 -124.3(3) . . . . ?
C14 N6 B1 N4 114.1(3) . . . . ?
C16 C17 C18 C19 177.9(3) . . . . ?
C17 N8 B2 N10 -114.1(3) . . . . ?
C17 N8 B2 N12 124.2(3) . . . . ?
C17 C18 C19 N7 0.3(3) . . . . ?
C17 C18 C19 C20 179.7(3) . . . . ?
C19 N7 N8 C17 -0.6(3) . . . . ?
C19 N7 N8 B2 179.3(2) . . . . ?
C21 C22 C23 C24 -177.8(3) . . . . ?
C22 N10 B2 N8 113.1(3) . . . . ?
C22 N10 B2 N12 -125.1(3) . . . . ?
C22 C23 C24 N9 -0.5(3) . . . . ?
C22 C23 C24 C25 -179.6(3) . . . . ?
C24 N9 N10 C22 0.9(3) . . . . ?
C24 N9 N10 B2 179.9(2) . . . . ?
C26 C27 C28 C29 177.9(3) . . . . ?
C27 N12 B2 N8 -112.0(3) . . . . ?
C27 N12 B2 N10 126.6(3) . . . . ?
C27 C28 C29 N11 0.0(3) . . . . ?
C27 C28 C29 C30 -179.6(3) . . . . ?
C29 N11 N12 C27 -0.8(3) . . . . ?
C29 N11 N12 B2 179.6(2) . . . . ?
B1 N2 C4 C3 178.2(3) . . . . ?
B1 N2 C4 C5 -1.9(5) . . . . ?
B1 N4 C9 C8 178.8(3) . . . . ?
B1 N4 C9 C10 -0.4(5) . . . . ?
B1 N6 C14 C13 -178.1(3) . . . . ?
B1 N6 C14 C15 1.5(5) . . . . ?
B2 N8 C17 C16 2.2(5) . . . . ?
B2 N8 C17 C18 -179.1(3) . . . . ?
B2 N10 C22 C21 -1.3(4) . . . . ?
B2 N10 C22 C23 179.9(3) . . . . ?
B2 N12 C27 C26 1.8(5) . . . . ?
B2 N12 C27 C28 -179.6(3) . . . . ?
Dy2 N13 N14 C34 175.81(17) . . . . ?
Dy2 N13 N14 B3 -7.7(3) . . . . ?
Dy2 N13 C32 C31 6.0(4) . . . . ?
Dy2 N13 C32 C33 -174.62(19) . . . . ?
Dy2 N15 N16 C39 178.37(17) . . . . ?
Dy2 N15 N16 B3 -3.8(3) . . . . ?
Dy2 N15 C37 C36 3.2(4) . . . . ?
Dy2 N15 C37 C38 -177.73(19) . . . . ?
Dy2 N17 N18 C44 166.88(17) . . . . ?
Dy2 N17 N18 B3 -13.8(3) . . . . ?
Dy2 N17 C42 C41 16.4(4) . . . . ?
Dy2 N17 C42 C43 -165.08(18) . . . . ?
N13 N14 C34 C33 -0.6(3) . . . . ?
N13 N14 C34 C35 179.1(3) . . . . ?
N13 N14 B3 N16 65.5(3) . . . . ?
N13 N14 B3 N18 -55.7(3) . . . . ?
N13 C32 C33 C34 -0.7(3) . . . . ?
N14 N13 C32 C31 -179.0(3) . . . . ?
N14 N13 C32 C33 0.4(3) . . . . ?
N15 N16 C39 C38 -0.3(3) . . . . ?
N15 N16 C39 C40 178.9(3) . . . . ?
N15 N16 B3 N14 -58.8(3) . . . . ?
N15 N16 B3 N18 62.0(3) . . . . ?
N15 C37 C38 C39 -0.8(3) . . . . ?
N16 N15 C37 C36 -178.5(3) . . . . ?
N16 N15 C37 C38 0.6(3) . . . . ?
N17 N18 C44 C43 0.8(3) . . . . ?
N17 N18 C44 C45 -178.1(3) . . . . ?
N17 N18 B3 N14 70.0(3) . . . . ?
N17 N18 B3 N16 -51.5(3) . . . . ?
N17 C42 C43 C44 -0.7(3) . . . . ?
N18 N17 C42 C41 -177.3(2) . . . . ?
N18 N17 C42 C43 1.2(3) . . . . ?
C31 C32 C33 C34 178.6(3) . . . . ?
C32 N13 N14 C34 0.1(3) . . . . ?
C32 N13 N14 B3 176.6(2) . . . . ?
C32 C33 C34 N14 0.8(3) . . . . ?
C32 C33 C34 C35 -178.9(3) . . . . ?
C34 N14 B3 N16 -118.7(3) . . . . ?
C34 N14 B3 N18 120.1(3) . . . . ?
C36 C37 C38 C39 178.3(3) . . . . ?
C37 N15 N16 C39 -0.1(3) . . . . ?
C37 N15 N16 B3 177.7(2) . . . . ?
C37 C38 C39 N16 0.7(3) . . . . ?
C37 C38 C39 C40 -178.5(3) . . . . ?
C39 N16 B3 N14 118.6(3) . . . . ?
C39 N16 B3 N18 -120.6(3) . . . . ?
C41 C42 C43 C44 177.7(3) . . . . ?
C42 N17 N18 C44 -1.2(3) . . . . ?
C42 N17 N18 B3 178.1(2) . . . . ?
C42 C43 C44 N18 -0.1(3) . . . . ?
C42 C43 C44 C45 178.7(3) . . . . ?
C44 N18 B3 N14 -110.8(3) . . . . ?
C44 N18 B3 N16 127.7(3) . . . . ?
B3 N14 C34 C33 -176.7(3) . . . . ?
B3 N14 C34 C35 3.0(4) . . . . ?
B3 N16 C39 C38 -178.0(3) . . . . ?
B3 N16 C39 C40 1.2(4) . . . . ?
B3 N18 C44 C43 -178.5(3) . . . . ?
B3 N18 C44 C45 2.6(4) . . . . ?
_shelx_res_file
;
TITL da1012_MeCN_0m_a.res in P2(1)/n
da1012_mecn_0m_a.res
created by SHELXL-2017/1 at 16:04:24 on 08-Sep-2018
REM Old TITL da1012_MeCN_0m in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.070, Rweak 0.005, Alpha 0.113, Orientation as input
REM Formula found by SHELXT: C56 Cl5 Dy2 N11
CELL 0.71073 10.2885 36.2677 16.0699 90 92.504 90
ZERR 4 0.0005 0.0019 0.0009 0 0.0016 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H B Cl Dy N
UNIT 184 272 12 20 8 72
L.S. 30
PLAN 20
SIZE 0.2 0.19 0.06
TEMP -163.15
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
REM
REM
REM
WGHT 0.009300 12.521201
FVAR 0.05764
DY1 5 0.506687 0.421257 0.673026 11.00000 0.01139 0.01029 =
0.01205 0.00039 -0.00116 -0.00254
N1 6 0.334497 0.405017 0.760539 11.00000 0.01995 0.01557 =
0.01087 -0.00037 0.00370 -0.00051
N2 6 0.249760 0.377488 0.734519 11.00000 0.01242 0.01655 =
0.01706 0.00295 0.00089 -0.00143
N3 6 0.514187 0.357029 0.647481 11.00000 0.01334 0.01427 =
0.01839 -0.00027 0.00030 -0.00272
N4 6 0.398472 0.337796 0.649719 11.00000 0.01640 0.01046 =
0.01394 -0.00087 0.00079 -0.00516
N5 6 0.330552 0.415288 0.573553 11.00000 0.01223 0.01117 =
0.01396 0.00175 0.00065 -0.00247
N6 6 0.250148 0.385137 0.577976 11.00000 0.01029 0.01560 =
0.01243 0.00101 0.00069 -0.00372
N7 6 0.671798 0.416505 0.781169 11.00000 0.01708 0.01601 =
0.01470 0.00362 -0.00299 -0.00036
N8 6 0.765196 0.443951 0.788349 11.00000 0.01327 0.01526 =
0.01466 -0.00075 -0.00406 0.00054
N9 6 0.528801 0.485267 0.701285 11.00000 0.01068 0.01234 =
0.01457 -0.00115 -0.00193 -0.00234
N10 6 0.649892 0.499101 0.723837 11.00000 0.01247 0.01136 =
0.01203 -0.00092 -0.00197 -0.00352
N11 6 0.687444 0.437854 0.594967 11.00000 0.01286 0.01273 =
0.01275 0.00026 -0.00171 -0.00295
N12 6 0.786532 0.457764 0.634857 11.00000 0.01096 0.01628 =
0.01429 0.00075 -0.00139 -0.00221
C1 1 0.369763 0.445377 0.883259 11.00000 0.04904 0.02536 =
0.01600 -0.00371 0.00271 0.00393
AFIX 137
H1A 2 0.448350 0.434807 0.910421 11.00000 -1.50000
H1B 2 0.314466 0.455716 0.925571 11.00000 -1.50000
H1C 2 0.394281 0.464921 0.844861 11.00000 -1.50000
AFIX 0
C2 1 0.296868 0.415931 0.835875 11.00000 0.02381 0.02139 =
0.01361 0.00312 0.00135 0.00819
C3 1 0.189669 0.395622 0.857806 11.00000 0.02525 0.03585 =
0.01486 0.00445 0.00924 0.00817
AFIX 43
H3 2 0.144205 0.397759 0.907777 11.00000 -1.20000
AFIX 0
C4 1 0.162100 0.371813 0.793130 11.00000 0.01650 0.03069 =
0.01860 0.00820 0.00560 0.00231
C5 1 0.055937 0.343730 0.783846 11.00000 0.02228 0.05808 =
0.03048 0.00632 0.01044 -0.01453
AFIX 137
H5A 2 0.006203 0.347860 0.731267 11.00000 -1.50000
H5B 2 -0.002003 0.345966 0.830393 11.00000 -1.50000
H5C 2 0.094070 0.318969 0.783797 11.00000 -1.50000
AFIX 0
C6 1 0.748892 0.342376 0.642041 11.00000 0.01852 0.02605 =
0.05355 0.00229 0.00340 0.00490
AFIX 137
H6A 2 0.768570 0.348497 0.584542 11.00000 -1.50000
H6B 2 0.804088 0.321834 0.661562 11.00000 -1.50000
H6C 2 0.765695 0.363906 0.677760 11.00000 -1.50000
AFIX 0
C7 1 0.609113 0.331538 0.645487 11.00000 0.01776 0.01869 =
0.01894 -0.00004 -0.00080 0.00315
C8 1 0.556425 0.296605 0.647003 11.00000 0.02947 0.01299 =
0.02602 0.00188 0.00146 0.00620
AFIX 43
H8 2 0.602297 0.273881 0.646345 11.00000 -1.20000
AFIX 0
C9 1 0.423655 0.301321 0.649666 11.00000 0.02842 0.01169 =
0.01571 0.00090 0.00046 -0.00309
C10 1 0.320471 0.272773 0.651074 11.00000 0.03540 0.01422 =
0.04255 0.00485 0.00184 -0.00800
AFIX 137
H10A 2 0.266111 0.277098 0.698694 11.00000 -1.50000
H10B 2 0.360617 0.248325 0.656100 11.00000 -1.50000
H10C 2 0.266535 0.274041 0.599360 11.00000 -1.50000
AFIX 0
C11 1 0.364778 0.467712 0.479951 11.00000 0.02252 0.02219 =
0.01535 0.00680 -0.00173 -0.00324
AFIX 137
H11A 2 0.303760 0.488456 0.480243 11.00000 -1.50000
H11B 2 0.398472 0.465013 0.424171 11.00000 -1.50000
H11C 2 0.437127 0.472348 0.520289 11.00000 -1.50000
AFIX 0
C12 1 0.296339 0.433237 0.502978 11.00000 0.01466 0.01501 =
0.01616 0.00260 0.00056 0.00220
C13 1 0.194184 0.414744 0.461832 11.00000 0.01991 0.02571 =
0.01503 0.00553 -0.00642 -0.00407
AFIX 43
H13 2 0.151336 0.421487 0.410513 11.00000 -1.20000
AFIX 0
C14 1 0.167631 0.384623 0.510604 11.00000 0.01398 0.02222 =
0.01854 -0.00044 -0.00274 -0.00346
C15 1 0.067597 0.355344 0.495213 11.00000 0.02821 0.03652 =
0.02697 0.00429 -0.00955 -0.01476
AFIX 137
H15A 2 0.110391 0.331251 0.492791 11.00000 -1.50000
H15B 2 0.019844 0.360156 0.442223 11.00000 -1.50000
H15C 2 0.006845 0.355393 0.540514 11.00000 -1.50000
AFIX 0
C16 1 0.947184 0.463951 0.885852 11.00000 0.02759 0.03104 =
0.02542 -0.00149 -0.01603 0.00002
AFIX 137
H16A 2 1.013288 0.464442 0.843769 11.00000 -1.50000
H16B 2 0.986672 0.455395 0.938997 11.00000 -1.50000
H16C 2 0.911943 0.488811 0.892805 11.00000 -1.50000
AFIX 0
C17 1 0.840102 0.438388 0.858434 11.00000 0.01836 0.02257 =
0.01458 -0.00339 -0.00512 0.00687
C18 1 0.796828 0.407061 0.896432 11.00000 0.02454 0.02611 =
0.01345 0.00233 -0.00545 0.00831
AFIX 43
H18 2 0.831603 0.396323 0.946524 11.00000 -1.20000
AFIX 0
C19 1 0.692644 0.394225 0.847407 11.00000 0.02508 0.01667 =
0.01331 0.00189 0.00149 0.00566
C20 1 0.610385 0.360914 0.860057 11.00000 0.03294 0.02326 =
0.01874 0.00903 0.00107 -0.00074
AFIX 137
H20A 2 0.521137 0.365863 0.839244 11.00000 -1.50000
H20B 2 0.610409 0.355014 0.919570 11.00000 -1.50000
H20C 2 0.645653 0.340014 0.829655 11.00000 -1.50000
AFIX 0
C21 1 0.751380 0.557715 0.777470 11.00000 0.02130 0.01432 =
0.02603 -0.00706 -0.00435 -0.00650
AFIX 137
H21A 2 0.785793 0.547793 0.830712 11.00000 -1.50000
H21B 2 0.722969 0.583225 0.785275 11.00000 -1.50000
H21C 2 0.819481 0.557089 0.736718 11.00000 -1.50000
AFIX 0
C22 1 0.638628 0.534947 0.746591 11.00000 0.02018 0.01207 =
0.01162 0.00041 -0.00122 -0.00250
C23 1 0.508332 0.544316 0.736788 11.00000 0.01927 0.01332 =
0.01413 -0.00154 -0.00102 0.00199
AFIX 43
H23 2 0.470749 0.567717 0.747036 11.00000 -1.20000
AFIX 0
C24 1 0.443879 0.512946 0.709193 11.00000 0.01578 0.01602 =
0.01193 0.00035 -0.00070 -0.00012
C25 1 0.302306 0.507439 0.688108 11.00000 0.01522 0.02209 =
0.02375 -0.00415 -0.00161 0.00065
AFIX 137
H25A 2 0.289398 0.503101 0.628124 11.00000 -1.50000
H25B 2 0.253992 0.529498 0.703652 11.00000 -1.50000
H25C 2 0.270686 0.486107 0.718722 11.00000 -1.50000
AFIX 0
C26 1 1.014266 0.477112 0.611145 11.00000 0.01837 0.07045 =
0.03206 -0.01776 0.00666 -0.01769
AFIX 137
H26A 2 0.998028 0.503011 0.624642 11.00000 -1.50000
H26B 2 1.074218 0.475738 0.565505 11.00000 -1.50000
H26C 2 1.052853 0.464575 0.660280 11.00000 -1.50000
AFIX 0
C27 1 0.888865 0.458845 0.585255 11.00000 0.01198 0.02760 =
0.02185 -0.00142 0.00201 -0.00400
C28 1 0.856145 0.440090 0.512488 11.00000 0.01645 0.03133 =
0.01798 -0.00351 0.00408 -0.00184
AFIX 43
H28 2 0.909082 0.436584 0.466160 11.00000 -1.20000
AFIX 0
C29 1 0.730908 0.427501 0.520874 11.00000 0.01716 0.01246 =
0.01510 0.00018 0.00063 0.00156
C30 1 0.647579 0.405330 0.460886 11.00000 0.01947 0.02413 =
0.01824 -0.00545 0.00259 -0.00166
AFIX 137
H30A 2 0.593478 0.388343 0.491805 11.00000 -1.50000
H30B 2 0.703082 0.391215 0.424440 11.00000 -1.50000
H30C 2 0.591597 0.421909 0.427122 11.00000 -1.50000
AFIX 0
B1 3 0.264525 0.357302 0.650626 11.00000 0.01151 0.01609 =
0.01440 0.00023 -0.00250 -0.00548
AFIX 13
H1 2 0.194366 0.338319 0.643854 11.00000 -1.20000
AFIX 0
B2 3 0.772907 0.474679 0.722408 11.00000 0.01145 0.01482 =
0.01837 -0.00152 -0.00330 -0.00369
AFIX 13
H2 2 0.850987 0.490305 0.736188 11.00000 -1.20000
AFIX 0
DY2 5 0.903937 0.353719 1.169981 11.00000 0.00961 0.01213 =
0.01080 -0.00086 -0.00067 -0.00043
CL1 4 1.085187 0.308938 1.223591 11.00000 0.01957 0.02603 =
0.03171 0.00286 -0.00718 0.00680
CL2 4 0.903051 0.398815 1.295635 11.00000 0.03000 0.02312 =
0.01395 -0.00554 0.00129 -0.00068
CL3 4 1.033122 0.396060 1.073825 11.00000 0.01386 0.02264 =
0.01573 0.00150 0.00168 -0.00344
N13 6 0.739264 0.312575 1.227468 11.00000 0.01209 0.01532 =
0.01385 0.00089 -0.00119 0.00016
N14 6 0.637545 0.298844 1.178033 11.00000 0.01038 0.01427 =
0.01427 0.00077 -0.00006 0.00005
N15 6 0.852445 0.312291 1.053107 11.00000 0.00974 0.01376 =
0.01652 -0.00308 -0.00094 -0.00021
N16 6 0.726589 0.301198 1.033796 11.00000 0.01099 0.01265 =
0.01272 -0.00019 -0.00020 -0.00210
N17 6 0.701827 0.377861 1.106457 11.00000 0.01285 0.01436 =
0.01084 0.00002 0.00040 0.00006
N18 6 0.598236 0.354669 1.088105 11.00000 0.01047 0.01800 =
0.01218 0.00037 0.00054 0.00061
C31 1 0.821811 0.305510 1.373607 11.00000 0.02521 0.02772 =
0.01697 0.00762 -0.00396 -0.00286
AFIX 137
H31A 2 0.910886 0.300644 1.357331 11.00000 -1.50000
H31B 2 0.802229 0.290060 1.421498 11.00000 -1.50000
H31C 2 0.813405 0.331555 1.388702 11.00000 -1.50000
AFIX 0
C32 1 0.728831 0.296792 1.302512 11.00000 0.01941 0.01473 =
0.01765 0.00149 0.00125 0.00432
C33 1 0.622845 0.273112 1.301403 11.00000 0.02097 0.01578 =
0.01859 0.00431 0.00602 -0.00324
AFIX 43
H33 2 0.594885 0.258435 1.346203 11.00000 -1.20000
AFIX 0
C34 1 0.566343 0.275178 1.222222 11.00000 0.01506 0.01281 =
0.01989 0.00147 0.00513 -0.00053
C35 1 0.448021 0.255978 1.186761 11.00000 0.01905 0.02564 =
0.02945 0.00256 0.00167 -0.00858
AFIX 137
H35A 2 0.381116 0.274257 1.171259 11.00000 -1.50000
H35B 2 0.414733 0.239119 1.228466 11.00000 -1.50000
H35C 2 0.470583 0.241961 1.137292 11.00000 -1.50000
AFIX 0
C36 1 1.071143 0.302038 0.998277 11.00000 0.01806 0.02987 =
0.02724 -0.01137 0.00564 0.00275
AFIX 137
H36A 2 1.091209 0.328326 0.992965 11.00000 -1.50000
H36B 2 1.107814 0.288460 0.952082 11.00000 -1.50000
H36C 2 1.108968 0.292737 1.051228 11.00000 -1.50000
AFIX 0
C37 1 0.926803 0.296837 0.996070 11.00000 0.01753 0.01455 =
0.01914 -0.00127 0.00328 0.00046
C38 1 0.849536 0.276208 0.939837 11.00000 0.02402 0.01747 =
0.01720 -0.00661 0.00322 0.00119
AFIX 43
H38 2 0.877826 0.262768 0.893224 11.00000 -1.20000
AFIX 0
C39 1 0.724434 0.279230 0.965379 11.00000 0.02219 0.01345 =
0.01381 -0.00240 -0.00072 -0.00038
C40 1 0.603067 0.261936 0.928775 11.00000 0.02668 0.02459 =
0.01994 -0.00842 -0.00408 -0.00680
AFIX 137
H40A 2 0.565909 0.245510 0.969925 11.00000 -1.50000
H40B 2 0.623749 0.247713 0.879218 11.00000 -1.50000
H40C 2 0.539973 0.281246 0.913186 11.00000 -1.50000
AFIX 0
C41 1 0.741361 0.445345 1.109670 11.00000 0.03144 0.01256 =
0.02633 -0.00132 0.00273 0.00535
AFIX 137
H41A 2 0.801791 0.441559 1.157749 11.00000 -1.50000
H41B 2 0.687586 0.467121 1.119154 11.00000 -1.50000
H41C 2 0.790734 0.449063 1.059560 11.00000 -1.50000
AFIX 0
C42 1 0.656058 0.412296 1.098320 11.00000 0.02223 0.01739 =
0.00806 -0.00005 0.00334 0.00606
C43 1 0.523612 0.411241 1.076529 11.00000 0.02275 0.02276 =
0.01389 -0.00021 -0.00063 0.01283
AFIX 43
H43 2 0.467669 0.431830 1.067529 11.00000 -1.20000
AFIX 0
C44 1 0.489574 0.374822 1.070577 11.00000 0.01298 0.02781 =
0.01138 -0.00074 0.00100 0.00732
C45 1 0.360034 0.357786 1.050774 11.00000 0.01433 0.03732 =
0.02806 -0.00013 -0.00359 0.00695
AFIX 137
H45A 2 0.363973 0.343212 0.999593 11.00000 -1.50000
H45B 2 0.294469 0.377222 1.042921 11.00000 -1.50000
H45C 2 0.336501 0.341725 1.096790 11.00000 -1.50000
AFIX 0
B3 3 0.613200 0.312434 1.088055 11.00000 0.01179 0.01423 =
0.01510 -0.00180 -0.00181 -0.00228
AFIX 13
H3A 2 0.530972 0.301120 1.064447 11.00000 -1.20000
AFIX 0
CL4 4 0.411934 0.323419 0.445013 11.00000 0.05852 0.03183 =
0.02995 -0.00140 0.01428 -0.00336
CL5 4 0.457317 0.358397 0.285785 11.00000 0.05036 0.02724 =
0.03971 0.01246 0.00562 0.00192
C46 1 0.347084 0.337017 0.349049 11.00000 0.03077 0.13915 =
0.02120 -0.00043 0.00071 -0.01193
AFIX 23
H46A 2 0.274127 0.354193 0.357733 11.00000 -1.20000
H46B 2 0.310977 0.315071 0.319600 11.00000 -1.20000
AFIX 0
HKLF 4
REM da1012_MeCN_0m_a.res in P2(1)/n
REM R1 = 0.0244 for 10111 Fo > 4sig(Fo) and 0.0326 for all 11476 data
REM 685 parameters refined using 0 restraints
END
WGHT 0.0093 12.5212
REM Highest difference peak 0.765, deepest hole -0.685, 1-sigma level 0.090
Q1 1 0.3409 0.3178 0.4151 11.00000 0.05 0.77
Q2 1 0.3558 0.3621 0.3587 11.00000 0.05 0.57
Q3 1 0.9467 0.4735 0.5920 11.00000 0.05 0.43
Q4 1 0.4240 0.3723 0.3146 11.00000 0.05 0.41
Q5 1 0.3073 0.4254 0.5392 11.00000 0.05 0.40
Q6 1 0.6476 0.5125 0.7579 11.00000 0.05 0.37
Q7 1 0.2626 0.4816 0.6592 11.00000 0.05 0.37
Q8 1 0.5657 0.5415 0.7731 11.00000 0.05 0.36
Q9 1 0.1220 0.2997 0.7759 11.00000 0.05 0.36
Q10 1 0.4425 0.4525 0.8720 11.00000 0.05 0.36
Q11 1 0.8805 0.3272 1.1007 11.00000 0.05 0.35
Q12 1 0.8884 0.2771 0.9782 11.00000 0.05 0.35
Q13 1 0.7633 0.3668 0.6349 11.00000 0.05 0.34
Q14 1 1.0242 0.4888 0.6621 11.00000 0.05 0.34
Q15 1 0.4928 0.3034 1.0622 11.00000 0.05 0.34
Q16 1 0.8862 0.5109 0.8268 11.00000 0.05 0.33
Q17 1 0.4200 0.3190 0.9406 11.00000 0.05 0.33
Q18 1 1.0700 0.4676 0.5791 11.00000 0.05 0.33
Q19 1 0.2387 0.3747 0.6982 11.00000 0.05 0.32
Q20 1 0.3151 0.4522 0.5014 11.00000 0.05 0.32
;
_shelx_res_checksum 97394
_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_da1063_0m_a
_audit_block_doi 10.5517/ccdc.csd.cc210f4n
_database_code_depnum_ccdc_archive 'CCDC 1877240'
loop_
_audit_author_name
_audit_author_address
'Dimitrios Alexandropoulos'
;Texas A&M University
United States of America
;
_audit_update_record
;
2018-11-05 deposited with the CCDC. 2019-05-09 downloaded from the CCDC.
;
_audit_creation_date 2018-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C30 H44 B2 Dy N12, I'
_chemical_formula_sum 'C30 H44 B2 Dy I N12'
_chemical_formula_weight 883.79
_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'
B B 0.0013 0.0007 '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'
I I -0.4742 1.8119 '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'
_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 12
_space_group_name_H-M_alt 'C 1 2/m 1'
_space_group_name_Hall '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
_cell_length_a 16.4584(11)
_cell_length_b 12.8987(8)
_cell_length_c 8.4033(6)
_cell_angle_alpha 90
_cell_angle_beta 91.810(3)
_cell_angle_gamma 90
_cell_volume 1783.1(2)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 9583
_cell_measurement_temperature 100
_cell_measurement_theta_max 25.741
_cell_measurement_theta_min 2.425
_shelx_estimated_absorpt_T_max 0.864
_shelx_estimated_absorpt_T_min 0.571
_exptl_absorpt_coefficient_mu 3.001
_exptl_absorpt_correction_T_max 0.7453
_exptl_absorpt_correction_T_min 0.6132
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1487 before and 0.0724 after correction. The Ratio of minimum to maximum transmission is 0.8228. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear whiteish colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier whiteish
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.646
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 874
_exptl_crystal_preparation ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.05
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0635
_diffrn_reflns_av_unetI/netI 0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 10
_diffrn_reflns_limit_l_min -10
_diffrn_reflns_number 33794
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.742
_diffrn_reflns_theta_max 25.742
_diffrn_reflns_theta_min 2.425
_diffrn_ambient_temperature 100.42
_diffrn_detector 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\ms'
_diffrn_special_details ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 1647
_reflns_number_total 1791
_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 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max 0.565
_refine_diff_density_min -0.768
_refine_diff_density_rms 0.105
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.109
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 124
_refine_ls_number_reflns 1791
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0300
_refine_ls_R_factor_gt 0.0253
_refine_ls_restrained_S_all 1.109
_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^)+(0.0062P)^2^+9.8949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0458
_refine_ls_wR_factor_ref 0.0473
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All B(H) groups, All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Others
Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
3.a Ternary CH refined with riding coordinates:
B1(H1)
3.b Aromatic/amide H refined with riding coordinates:
C3(H3), C8(H8)
3.c Idealised Me refined as rotating group:
C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C)
;
_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 0.500000 0.500000 0.500000 0.00910(9) Uani 1 4 d S T P . .
N1 N 0.6313(2) 0.500000 0.6405(4) 0.0114(7) Uani 1 2 d S T P . .
N2 N 0.70117(19) 0.500000 0.5544(4) 0.0091(7) Uani 1 2 d S T P . .
N3 N 0.57164(14) 0.38441(19) 0.3347(3) 0.0114(5) Uani 1 1 d . . . . .
N4 N 0.65303(13) 0.40108(19) 0.3107(3) 0.0094(5) Uani 1 1 d . . . . .
C1 C 0.5946(3) 0.500000 0.9226(5) 0.0209(10) Uani 1 2 d S T P . .
H1A H 0.609034 0.553106 1.001950 0.031 Uiso 0.5 1 calc GR . . A -1
H1B H 0.593901 0.431816 0.974007 0.031 Uiso 0.5 1 calc GR . . A -1
H1C H 0.540601 0.515078 0.875591 0.031 Uiso 0.5 1 calc GR . . A -1
C2 C 0.6555(3) 0.500000 0.7954(5) 0.0145(9) Uani 1 2 d S T P . .
C3 C 0.7396(3) 0.500000 0.8081(5) 0.0145(9) Uani 1 2 d S T P . .
H3 H 0.772092 0.500000 0.903545 0.017 Uiso 1 2 calc RS T P . .
C4 C 0.7669(3) 0.500000 0.6538(5) 0.0129(9) Uani 1 2 d S T P . .
C5 C 0.8520(2) 0.500000 0.5975(5) 0.0164(10) Uani 1 2 d S T P . .
H5A H 0.889778 0.487019 0.687786 0.025 Uiso 0.5 1 calc GR . . B -1
H5B H 0.864103 0.567498 0.550251 0.025 Uiso 0.5 1 calc GR . . B -1
H5C H 0.857990 0.445483 0.517502 0.025 Uiso 0.5 1 calc GR . . B -1
C6 C 0.46937(18) 0.2484(3) 0.2747(4) 0.0247(8) Uani 1 1 d . . . . .
H6A H 0.433202 0.299746 0.321243 0.037 Uiso 1 1 calc GR . . . .
H6B H 0.469616 0.185160 0.339349 0.037 Uiso 1 1 calc GR . . . .
H6C H 0.450051 0.232112 0.166072 0.037 Uiso 1 1 calc GR . . . .
C7 C 0.55325(18) 0.2912(2) 0.2709(4) 0.0144(6) Uani 1 1 d . . . . .
C8 C 0.62233(18) 0.2478(2) 0.2063(4) 0.0168(7) Uani 1 1 d . . . . .
H8 H 0.626186 0.182901 0.153464 0.020 Uiso 1 1 calc R . . . .
C9 C 0.68415(17) 0.3186(2) 0.2350(3) 0.0130(6) Uani 1 1 d . . . . .
C10 C 0.77218(18) 0.3095(3) 0.1995(4) 0.0223(8) Uani 1 1 d . . . . .
H10A H 0.787368 0.365608 0.127546 0.033 Uiso 1 1 calc GR . . . .
H10B H 0.782173 0.242516 0.148813 0.033 Uiso 1 1 calc GR . . . .
H10C H 0.804773 0.314554 0.298816 0.033 Uiso 1 1 calc GR . . . .
B1 B 0.6972(3) 0.500000 0.3718(6) 0.0101(9) Uani 1 2 d S T P . .
H1 H 0.753884 0.500000 0.332118 0.012 Uiso 1 2 calc RS T P . .
I1 I 0.500000 0.000000 0.000000 0.03014(14) Uani 1 4 d S T P . .
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 0.00733(14) 0.01004(16) 0.01004(16) 0.000 0.00171(11) 0.000
N1 0.0083(17) 0.0142(18) 0.0118(18) 0.000 0.0024(14) 0.000
N2 0.0072(17) 0.0102(17) 0.0100(18) 0.000 0.0010(14) 0.000
N3 0.0053(11) 0.0126(13) 0.0164(13) -0.0029(11) 0.0026(10) -0.0003(10)
N4 0.0067(11) 0.0120(13) 0.0095(12) -0.0001(10) 0.0012(9) 0.0001(10)
C1 0.017(2) 0.035(3) 0.011(2) 0.000 0.0011(18) 0.000
C2 0.018(2) 0.016(2) 0.010(2) 0.000 -0.0001(18) 0.000
C3 0.013(2) 0.020(2) 0.010(2) 0.000 -0.0048(18) 0.000
C4 0.015(2) 0.010(2) 0.014(2) 0.000 -0.0013(18) 0.000
C5 0.006(2) 0.030(3) 0.013(2) 0.000 -0.0006(17) 0.000
C6 0.0147(16) 0.0212(18) 0.038(2) -0.0122(16) 0.0058(15) -0.0057(14)
C7 0.0146(15) 0.0128(16) 0.0158(16) -0.0024(13) -0.0011(12) -0.0010(12)
C8 0.0157(16) 0.0124(16) 0.0222(17) -0.0058(13) -0.0009(13) 0.0012(13)
C9 0.0130(15) 0.0128(15) 0.0131(15) -0.0002(13) -0.0008(12) 0.0041(12)
C10 0.0140(16) 0.0215(18) 0.032(2) -0.0114(15) 0.0034(14) 0.0028(14)
B1 0.009(2) 0.012(2) 0.009(2) 0.000 0.0023(18) 0.000
I1 0.0524(3) 0.0115(2) 0.0251(3) 0.000 -0.0217(2) 0.000
_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 N1 2.430(3) 5_666 ?
Dy1 N1 2.430(3) . ?
Dy1 N3 2.376(2) . ?
Dy1 N3 2.376(2) 5_666 ?
Dy1 N3 2.376(2) 6_565 ?
Dy1 N3 2.376(2) 2_656 ?
N1 N2 1.378(5) . ?
N1 C2 1.349(5) . ?
N2 C4 1.346(5) . ?
N2 B1 1.534(6) . ?
N3 N4 1.378(3) . ?
N3 C7 1.347(4) . ?
N4 C9 1.349(4) . ?
N4 B1 1.548(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.489(6) . ?
C2 C3 1.384(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.385(6) . ?
C4 C5 1.493(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 C7 1.488(4) . ?
C7 C8 1.393(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.383(4) . ?
C9 C10 1.493(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
B1 H1 1.0000 . ?
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 Dy1 N1 180.00(7) . 5_666 ?
N3 Dy1 N1 80.44(8) 2_656 5_666 ?
N3 Dy1 N1 99.56(8) 6_565 5_666 ?
N3 Dy1 N1 80.44(8) . . ?
N3 Dy1 N1 99.56(8) 2_656 . ?
N3 Dy1 N1 99.56(8) . 5_666 ?
N3 Dy1 N1 80.44(8) 5_666 5_666 ?
N3 Dy1 N1 80.44(8) 6_565 . ?
N3 Dy1 N1 99.56(8) 5_666 . ?
N3 Dy1 N3 102.27(12) . 2_656 ?
N3 Dy1 N3 77.73(12) 5_666 2_656 ?
N3 Dy1 N3 102.27(12) 5_666 6_565 ?
N3 Dy1 N3 180.0 . 5_666 ?
N3 Dy1 N3 180.00(9) 6_565 2_656 ?
N3 Dy1 N3 77.73(12) . 6_565 ?
N2 N1 Dy1 119.3(2) . . ?
C2 N1 Dy1 134.4(3) . . ?
C2 N1 N2 106.3(3) . . ?
N1 N2 B1 121.1(3) . . ?
C4 N2 N1 110.0(3) . . ?
C4 N2 B1 129.0(3) . . ?
N4 N3 Dy1 119.37(17) . . ?
C7 N3 Dy1 133.11(19) . . ?
C7 N3 N4 106.7(2) . . ?
N3 N4 B1 121.9(3) . . ?
C9 N4 N3 109.4(2) . . ?
C9 N4 B1 128.7(3) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
N1 C2 C1 120.5(4) . . ?
N1 C2 C3 109.8(4) . . ?
C3 C2 C1 129.8(4) . . ?
C2 C3 H3 126.8 . . ?
C2 C3 C4 106.3(4) . . ?
C4 C3 H3 126.8 . . ?
N2 C4 C3 107.6(4) . . ?
N2 C4 C5 123.2(4) . . ?
C3 C4 C5 129.2(4) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
N3 C7 C6 121.3(3) . . ?
N3 C7 C8 109.8(3) . . ?
C8 C7 C6 128.9(3) . . ?
C7 C8 H8 127.1 . . ?
C9 C8 C7 105.7(3) . . ?
C9 C8 H8 127.1 . . ?
N4 C9 C8 108.4(3) . . ?
N4 C9 C10 122.8(3) . . ?
C8 C9 C10 128.8(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 B1 N4 109.6(2) . 6_565 ?
N2 B1 N4 109.6(2) . . ?
N2 B1 H1 108.8 . . ?
N4 B1 N4 111.0(3) . 6_565 ?
N4 B1 H1 108.8 6_565 . ?
N4 B1 H1 108.8 . . ?
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 N1 N2 C4 180.000(1) . . . . ?
Dy1 N1 N2 B1 0.000(1) . . . . ?
Dy1 N1 C2 C1 0.000(1) . . . . ?
Dy1 N1 C2 C3 180.000(1) . . . . ?
Dy1 N3 N4 C9 170.49(18) . . . . ?
Dy1 N3 N4 B1 -7.3(3) . . . . ?
Dy1 N3 C7 C6 10.8(5) . . . . ?
Dy1 N3 C7 C8 -169.4(2) . . . . ?
N1 N2 C4 C3 0.000(1) . . . . ?
N1 N2 C4 C5 180.000(1) . . . . ?
N1 N2 B1 N4 61.1(2) . . . 6_565 ?
N1 N2 B1 N4 -61.1(2) . . . . ?
N1 C2 C3 C4 0.000(1) . . . . ?
N2 N1 C2 C1 180.000(1) . . . . ?
N2 N1 C2 C3 0.000(1) . . . . ?
N3 N4 C9 C8 1.1(3) . . . . ?
N3 N4 C9 C10 -176.4(3) . . . . ?
N3 N4 B1 N2 66.9(4) . . . . ?
N3 N4 B1 N4 -54.4(4) . . . 6_565 ?
N3 C7 C8 C9 0.5(4) . . . . ?
N4 N3 C7 C6 -179.6(3) . . . . ?
N4 N3 C7 C8 0.1(3) . . . . ?
C1 C2 C3 C4 180.000(1) . . . . ?
C2 N1 N2 C4 0.000(1) . . . . ?
C2 N1 N2 B1 180.000(1) . . . . ?
C2 C3 C4 N2 0.000(1) . . . . ?
C2 C3 C4 C5 180.000(1) . . . . ?
C4 N2 B1 N4 -118.9(2) . . . 6_565 ?
C4 N2 B1 N4 118.9(2) . . . . ?
C6 C7 C8 C9 -179.7(3) . . . . ?
C7 N3 N4 C9 -0.7(3) . . . . ?
C7 N3 N4 B1 -178.6(3) . . . . ?
C7 C8 C9 N4 -1.0(3) . . . . ?
C7 C8 C9 C10 176.3(3) . . . . ?
C9 N4 B1 N2 -110.5(4) . . . . ?
C9 N4 B1 N4 128.2(3) . . . 6_565 ?
B1 N2 C4 C3 180.000(1) . . . . ?
B1 N2 C4 C5 0.000(1) . . . . ?
B1 N4 C9 C8 178.7(3) . . . . ?
B1 N4 C9 C10 1.3(5) . . . . ?
_shelx_res_file
;
TITL da1063_0m_a.res in C2/m
da1063_0m_a.res
created by SHELXL-2017/1 at 15:49:37 on 08-Sep-2018
REM Old TITL da1063_0m in C2/m
REM SHELXT solution in C2/m
REM R1 0.117, Rweak 0.017, Alpha 0.081, Orientation as input
REM Formula found by SHELXT: C38 Dy I N6
CELL 0.71073 16.4584 12.8987 8.4033 90 91.81 90
ZERR 2 0.0011 0.0008 0.0006 0 0.003 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H B Dy I N
UNIT 60 88 4 2 2 24
L.S. 10
PLAN 20
SIZE 0.21 0.13 0.05
TEMP -172.73
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
REM
REM
REM
WGHT 0.006200 9.894900
FVAR 0.08591
DY1 4 0.500000 0.500000 0.500000 10.25000 0.00733 0.01004 =
0.01004 0.00000 0.00171 0.00000
N1 6 0.631334 0.500000 0.640539 10.50000 0.00830 0.01421 =
0.01181 0.00000 0.00245 0.00000
N2 6 0.701174 0.500000 0.554410 10.50000 0.00718 0.01024 =
0.01001 0.00000 0.00099 0.00000
N3 6 0.571640 0.384412 0.334725 11.00000 0.00534 0.01261 =
0.01637 -0.00289 0.00257 -0.00033
N4 6 0.653029 0.401075 0.310688 11.00000 0.00672 0.01196 =
0.00950 -0.00013 0.00118 0.00009
C1 1 0.594557 0.500000 0.922616 10.50000 0.01711 0.03494 =
0.01082 0.00000 0.00114 0.00000
PART -1
AFIX 137
H1A 2 0.609034 0.553106 1.001950 10.50000 -1.50000
H1B 2 0.593901 0.431816 0.974007 10.50000 -1.50000
H1C 2 0.540601 0.515078 0.875591 10.50000 -1.50000
AFIX 0
PART 0
C2 1 0.655547 0.500000 0.795423 10.50000 0.01767 0.01556 =
0.01023 0.00000 -0.00007 0.00000
C3 1 0.739595 0.500000 0.808080 10.50000 0.01306 0.01956 =
0.01048 0.00000 -0.00475 0.00000
AFIX 43
H3 2 0.772092 0.500000 0.903545 10.50000 -1.20000
AFIX 0
C4 1 0.766897 0.500000 0.653833 10.50000 0.01513 0.00965 =
0.01368 0.00000 -0.00132 0.00000
C5 1 0.851998 0.500000 0.597508 10.50000 0.00595 0.03022 =
0.01299 0.00000 -0.00057 0.00000
PART -1
AFIX 137
H5A 2 0.889778 0.487019 0.687786 10.50000 -1.50000
H5B 2 0.864103 0.567498 0.550251 10.50000 -1.50000
H5C 2 0.857990 0.445483 0.517502 10.50000 -1.50000
AFIX 0
PART 0
C6 1 0.469368 0.248406 0.274715 11.00000 0.01467 0.02119 =
0.03849 -0.01221 0.00579 -0.00567
AFIX 137
H6A 2 0.433202 0.299746 0.321243 11.00000 -1.50000
H6B 2 0.469616 0.185160 0.339349 11.00000 -1.50000
H6C 2 0.450051 0.232112 0.166072 11.00000 -1.50000
AFIX 0
C7 1 0.553249 0.291233 0.270886 11.00000 0.01458 0.01284 =
0.01577 -0.00240 -0.00107 -0.00096
C8 1 0.622334 0.247757 0.206267 11.00000 0.01572 0.01237 =
0.02219 -0.00576 -0.00089 0.00123
AFIX 43
H8 2 0.626186 0.182901 0.153464 11.00000 -1.20000
AFIX 0
C9 1 0.684154 0.318637 0.234961 11.00000 0.01301 0.01279 =
0.01314 -0.00022 -0.00084 0.00412
C10 1 0.772177 0.309548 0.199487 11.00000 0.01397 0.02147 =
0.03151 -0.01138 0.00344 0.00277
AFIX 137
H10A 2 0.787368 0.365608 0.127546 11.00000 -1.50000
H10B 2 0.782173 0.242516 0.148813 11.00000 -1.50000
H10C 2 0.804773 0.314554 0.298816 11.00000 -1.50000
AFIX 0
B1 3 0.697231 0.500000 0.371762 10.50000 0.00917 0.01211 =
0.00905 0.00000 0.00227 0.00000
AFIX 13
H1 2 0.753884 0.500000 0.332118 10.50000 -1.20000
AFIX 0
I1 5 0.500000 0.000000 0.000000 10.25000 0.05237 0.01152 =
0.02508 0.00000 -0.02174 0.00000
HKLF 4
REM da1063_0m_a.res in C2/m
REM R1 = 0.0253 for 1647 Fo > 4sig(Fo) and 0.0300 for all 1791 data
REM 124 parameters refined using 0 restraints
END
WGHT 0.0062 9.8949
REM Highest difference peak 0.565, deepest hole -0.768, 1-sigma level 0.105
Q1 1 0.5400 0.5000 0.9319 10.50000 0.05 0.57
Q2 1 0.4251 0.0000 0.0860 10.50000 0.05 0.46
Q3 1 0.4439 0.0000 -0.1203 10.50000 0.05 0.42
Q4 1 0.4642 0.1751 0.2349 11.00000 0.05 0.41
Q5 1 0.4872 0.0000 0.1136 10.50000 0.05 0.40
Q6 1 0.7934 0.5000 0.3412 10.50000 0.05 0.39
Q7 1 0.6531 0.5000 0.5846 10.50000 0.05 0.38
Q8 1 0.4919 0.5000 0.7391 10.50000 0.05 0.37
Q9 1 0.4996 0.5000 0.3843 10.50000 0.05 0.37
Q10 1 0.5290 0.4151 0.3450 11.00000 0.05 0.37
Q11 1 0.5883 0.5000 0.6351 10.50000 0.05 0.37
Q12 1 0.8116 0.5000 0.6534 10.50000 0.05 0.35
Q13 1 0.5823 0.2730 0.2195 11.00000 0.05 0.35
Q14 1 0.6705 0.3759 0.2367 11.00000 0.05 0.34
Q15 1 0.8766 0.5000 0.5024 10.50000 0.05 0.34
Q16 1 0.7720 0.5293 0.7354 11.00000 0.05 0.34
Q17 1 0.4416 0.2528 0.4016 11.00000 0.05 0.34
Q18 1 0.6321 0.5000 0.8649 10.50000 0.05 0.34
Q19 1 0.6428 0.5000 0.7182 10.50000 0.05 0.33
Q20 1 0.6695 0.4426 0.3539 11.00000 0.05 0.32
;
_shelx_res_checksum 29761
_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_da1029_0m_a
_audit_block_doi 10.5517/ccdc.csd.cc210f3m
_database_code_depnum_ccdc_archive 'CCDC 1877239'
loop_
_audit_author_name
_audit_author_address
'Dimitrios Alexandropoulos'
;Texas A&M University
United States of America
;
_audit_update_record
;
2018-11-05 deposited with the CCDC. 2019-05-09 downloaded from the CCDC.
;
_audit_creation_date 2018-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2017/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C15 H22 B Cl3 Dy N6, C4 H12 N'
_chemical_formula_sum 'C19 H34 B Cl3 Dy N7'
_chemical_formula_weight 640.19
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 9.499(3)
_cell_length_b 31.346(8)
_cell_length_c 10.016(3)
_cell_angle_alpha 90
_cell_angle_beta 118.040(8)
_cell_angle_gamma 90
_cell_volume 2632.2(13)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9745
_cell_measurement_temperature 110
_cell_measurement_theta_max 25.75
_cell_measurement_theta_min 2.39
_shelx_estimated_absorpt_T_max 0.743
_shelx_estimated_absorpt_T_min 0.364
_exptl_absorpt_coefficient_mu 3.163
_exptl_absorpt_correction_T_max 0.7453
_exptl_absorpt_correction_T_min 0.4820
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1104 before and 0.0526 after correction.
The Ratio of minimum to maximum transmission is 0.6467.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear whiteish colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier whiteish
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.615
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 1276
_exptl_crystal_preparation ?
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0310
_diffrn_reflns_av_unetI/netI 0.0106
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 38
_diffrn_reflns_limit_k_min -38
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_number 108352
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.803
_diffrn_reflns_theta_max 25.803
_diffrn_reflns_theta_min 2.394
_diffrn_ambient_temperature 110
_diffrn_detector 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_source_type 'Incoatec I\ms'
_diffrn_special_details ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4713
_reflns_number_total 5062
_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 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_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 1.043
_refine_diff_density_min -1.495
_refine_diff_density_rms 0.089
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.167
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 290
_refine_ls_number_reflns 5062
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0270
_refine_ls_R_factor_gt 0.0237
_refine_ls_restrained_S_all 1.167
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0162P)^2^+6.1012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0527
_refine_ls_wR_factor_ref 0.0542
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All B(H) groups, All C(H) groups
At 1.5 times of:
All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
C8(H8), C3(H3), C13(H13)
2.c Idealised Me refined as rotating group:
C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C6(H6A,H6B,H6C), C10(H10A,H10B,
H10C), C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C19(H19A,H19B,
H19C), C15(H15A,H15B,H15C), C11(H11A,H11B,H11C)
;
_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 0.54421(2) 0.36706(2) 0.36817(2) 0.01967(5) Uani 1 1 d . . . . .
Cl1 Cl 0.45903(13) 0.40562(3) 0.11271(9) 0.0436(2) Uani 1 1 d . . . . .
Cl2 Cl 0.70639(16) 0.30986(3) 0.31083(11) 0.0531(3) Uani 1 1 d . . . . .
Cl3 Cl 0.27138(12) 0.33255(3) 0.29371(15) 0.0688(4) Uani 1 1 d . . . . .
N2 N 0.7104(3) 0.35923(8) 0.7468(3) 0.0210(5) Uani 1 1 d . . . . .
N5 N 0.7872(3) 0.40781(8) 0.5178(3) 0.0188(5) Uani 1 1 d . . . . .
N1 N 0.6435(3) 0.33501(8) 0.6169(3) 0.0195(5) Uani 1 1 d . . . . .
N4 N 0.5649(3) 0.42924(8) 0.6499(3) 0.0203(5) Uani 1 1 d . . . . .
N7 N 0.2369(3) 0.32224(8) 0.7408(3) 0.0242(6) Uani 1 1 d . . . . .
N6 N 0.8329(3) 0.41840(8) 0.6655(3) 0.0203(5) Uani 1 1 d . . . . .
N3 N 0.4751(3) 0.42204(8) 0.4971(3) 0.0199(5) Uani 1 1 d . . . . .
C9 C 0.4979(4) 0.46067(10) 0.6940(4) 0.0272(7) Uani 1 1 d . . . . .
C14 C 0.9704(4) 0.44099(10) 0.7223(4) 0.0339(9) Uani 1 1 d . . . . .
C4 C 0.7546(4) 0.33349(12) 0.8687(4) 0.0306(8) Uani 1 1 d . . . . .
C2 C 0.6476(4) 0.29449(10) 0.6605(4) 0.0270(7) Uani 1 1 d . . . . .
C8 C 0.3635(4) 0.47434(11) 0.5671(4) 0.0325(8) Uani 1 1 d . . . . .
H8 H 0.292354 0.496304 0.562218 0.039 Uiso 1 1 calc R . . . .
C3 C 0.7160(4) 0.29243(12) 0.8170(4) 0.0325(8) Uani 1 1 d . . . . .
H3 H 0.732693 0.267508 0.876571 0.039 Uiso 1 1 calc R . . . .
C16 C 0.3647(4) 0.30133(11) 0.8785(4) 0.0348(8) Uani 1 1 d . . . . .
H16A H 0.456324 0.294973 0.861914 0.052 Uiso 1 1 calc GR . . . .
H16B H 0.323658 0.274769 0.898677 0.052 Uiso 1 1 calc GR . . . .
H16C H 0.398089 0.320547 0.965363 0.052 Uiso 1 1 calc GR . . . .
C7 C 0.3532(4) 0.44959(11) 0.4481(4) 0.0268(7) Uani 1 1 d . . . . .
C12 C 0.8982(4) 0.42419(11) 0.4857(5) 0.0333(8) Uani 1 1 d . . . . .
C17 C 0.3013(4) 0.36248(11) 0.7091(4) 0.0338(8) Uani 1 1 d . . . . .
H17A H 0.336183 0.381780 0.795826 0.051 Uiso 1 1 calc GR . . . .
H17B H 0.217687 0.376328 0.618900 0.051 Uiso 1 1 calc GR . . . .
H17C H 0.392055 0.355616 0.691749 0.051 Uiso 1 1 calc GR . . . .
C6 C 0.2312(4) 0.45104(13) 0.2860(4) 0.0410(10) Uani 1 1 d . . . . .
H6A H 0.283256 0.457174 0.223719 0.062 Uiso 1 1 calc GR . . . .
H6B H 0.153243 0.473460 0.271052 0.062 Uiso 1 1 calc GR . . . .
H6C H 0.176663 0.423435 0.256312 0.062 Uiso 1 1 calc GR . . . .
C10 C 0.5612(5) 0.47480(12) 0.8539(4) 0.0429(10) Uani 1 1 d . . . . .
H10A H 0.539473 0.452854 0.911412 0.064 Uiso 1 1 calc GR . . . .
H10B H 0.509340 0.501534 0.856958 0.064 Uiso 1 1 calc GR . . . .
H10C H 0.676621 0.479328 0.898496 0.064 Uiso 1 1 calc GR . . . .
C5 C 0.8287(6) 0.35006(16) 1.0269(4) 0.0559(13) Uani 1 1 d . . . . .
H5A H 0.935563 0.361072 1.054792 0.084 Uiso 1 1 calc GR . . . .
H5B H 0.836734 0.326926 1.095973 0.084 Uiso 1 1 calc GR . . . .
H5C H 0.762595 0.373049 1.033901 0.084 Uiso 1 1 calc GR . . . .
C13 C 1.0135(4) 0.44514(11) 0.6112(5) 0.0440(11) Uani 1 1 d . . . . .
H13 H 1.104713 0.459572 0.618400 0.053 Uiso 1 1 calc R . . . .
C1 C 0.5875(5) 0.25847(11) 0.5513(5) 0.0456(10) Uani 1 1 d . . . . .
H1A H 0.497896 0.268251 0.456519 0.068 Uiso 1 1 calc GR . . . .
H1B H 0.551889 0.235321 0.594017 0.068 Uiso 1 1 calc GR . . . .
H1C H 0.673224 0.248095 0.531427 0.068 Uiso 1 1 calc GR . . . .
B1 B 0.7282(4) 0.40768(12) 0.7408(4) 0.0226(7) Uani 1 1 d . . . . .
H1 H 0.780137 0.419225 0.846253 0.027 Uiso 1 1 calc R . . . .
C18 C 0.1860(6) 0.29294(13) 0.6092(5) 0.0566(12) Uani 1 1 d . . . . .
H18A H 0.277071 0.286909 0.591413 0.085 Uiso 1 1 calc GR . . . .
H18B H 0.100787 0.306382 0.519177 0.085 Uiso 1 1 calc GR . . . .
H18C H 0.146794 0.266223 0.630523 0.085 Uiso 1 1 calc GR . . . .
C19 C 0.0997(5) 0.33230(15) 0.7683(6) 0.0576(13) Uani 1 1 d . . . . .
H19A H 0.056015 0.305777 0.785526 0.086 Uiso 1 1 calc GR . . . .
H19B H 0.017032 0.347078 0.680070 0.086 Uiso 1 1 calc GR . . . .
H19C H 0.135759 0.350669 0.857607 0.086 Uiso 1 1 calc GR . . . .
C15 C 1.0563(5) 0.45553(14) 0.8833(5) 0.0611(15) Uani 1 1 d . . . . .
H15A H 0.984174 0.472696 0.906297 0.092 Uiso 1 1 calc GR . . . .
H15B H 1.148788 0.472797 0.898805 0.092 Uiso 1 1 calc GR . . . .
H15C H 1.092256 0.430637 0.950287 0.092 Uiso 1 1 calc GR . . . .
C11 C 0.8885(6) 0.41849(16) 0.3345(6) 0.0573(13) Uani 1 1 d . . . . .
H11A H 0.950829 0.393398 0.335978 0.086 Uiso 1 1 calc GR . . . .
H11B H 0.931498 0.443853 0.309093 0.086 Uiso 1 1 calc GR . . . .
H11C H 0.776956 0.414462 0.258458 0.086 Uiso 1 1 calc GR . . . .
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 0.02670(8) 0.01565(8) 0.00893(7) -0.00145(5) 0.00198(6) -0.00462(6)
Cl1 0.0749(7) 0.0345(5) 0.0162(4) 0.0090(3) 0.0171(4) 0.0134(4)
Cl2 0.1075(9) 0.0255(4) 0.0370(5) 0.0038(4) 0.0429(6) 0.0222(5)
Cl3 0.0345(5) 0.0396(6) 0.0785(8) 0.0147(5) -0.0180(5) -0.0238(4)
N2 0.0197(12) 0.0309(14) 0.0121(11) 0.0036(10) 0.0071(10) 0.0067(10)
N5 0.0184(12) 0.0187(12) 0.0233(13) -0.0033(10) 0.0131(11) -0.0021(10)
N1 0.0194(12) 0.0218(13) 0.0156(12) 0.0034(10) 0.0068(10) -0.0002(10)
N4 0.0224(13) 0.0246(13) 0.0173(12) -0.0008(10) 0.0122(11) 0.0046(10)
N7 0.0226(13) 0.0192(13) 0.0321(14) 0.0002(11) 0.0138(12) -0.0023(10)
N6 0.0123(11) 0.0212(13) 0.0211(13) -0.0091(10) 0.0027(10) -0.0011(10)
N3 0.0154(12) 0.0273(14) 0.0168(12) 0.0049(10) 0.0074(10) 0.0012(10)
C9 0.0384(19) 0.0221(16) 0.0381(19) 0.0039(14) 0.0321(16) 0.0041(14)
C14 0.0127(15) 0.0194(16) 0.053(2) -0.0128(15) 0.0020(15) -0.0012(12)
C4 0.0244(16) 0.052(2) 0.0181(15) 0.0156(15) 0.0125(13) 0.0163(15)
C2 0.0183(15) 0.0276(17) 0.0331(18) 0.0128(14) 0.0103(14) 0.0011(13)
C8 0.0348(19) 0.0260(17) 0.056(2) 0.0178(16) 0.0369(18) 0.0137(14)
C3 0.0243(17) 0.041(2) 0.0345(19) 0.0255(16) 0.0158(15) 0.0115(15)
C16 0.0281(18) 0.0289(18) 0.041(2) 0.0047(15) 0.0109(16) 0.0018(14)
C7 0.0169(15) 0.0316(17) 0.0372(19) 0.0184(14) 0.0171(14) 0.0039(13)
C12 0.0308(18) 0.0260(17) 0.058(2) 0.0080(16) 0.0333(18) 0.0027(14)
C17 0.039(2) 0.0231(17) 0.047(2) 0.0020(15) 0.0275(18) -0.0041(15)
C6 0.0185(16) 0.056(2) 0.044(2) 0.0292(19) 0.0108(16) 0.0078(16)
C10 0.073(3) 0.0302(19) 0.047(2) -0.0056(16) 0.047(2) 0.0065(18)
C5 0.065(3) 0.084(3) 0.0156(17) 0.0146(19) 0.0159(19) 0.033(3)
C13 0.0197(17) 0.0222(18) 0.092(3) -0.0003(19) 0.027(2) -0.0034(14)
C1 0.048(2) 0.0228(18) 0.050(2) 0.0104(17) 0.0102(19) -0.0096(16)
B1 0.0233(17) 0.0293(19) 0.0107(15) -0.0047(13) 0.0043(13) 0.0049(14)
C18 0.084(3) 0.037(2) 0.039(2) -0.0098(18) 0.021(2) -0.023(2)
C19 0.043(2) 0.052(3) 0.101(4) 0.034(3) 0.053(3) 0.018(2)
C15 0.026(2) 0.041(2) 0.068(3) -0.031(2) -0.018(2) 0.0037(17)
C11 0.064(3) 0.067(3) 0.077(3) 0.023(2) 0.062(3) 0.012(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
Dy1 Cl1 2.5916(10) . ?
Dy1 Cl2 2.5979(11) . ?
Dy1 Cl3 2.5740(12) . ?
Dy1 N5 2.440(2) . ?
Dy1 N1 2.429(2) . ?
Dy1 N3 2.422(3) . ?
N2 N1 1.377(3) . ?
N2 C4 1.355(4) . ?
N2 B1 1.532(5) . ?
N5 N6 1.372(3) . ?
N5 C12 1.341(4) . ?
N1 C2 1.337(4) . ?
N4 N3 1.376(3) . ?
N4 C9 1.354(4) . ?
N4 B1 1.537(4) . ?
N7 C16 1.494(4) . ?
N7 C17 1.499(4) . ?
N7 C18 1.488(5) . ?
N7 C19 1.487(4) . ?
N6 C14 1.354(4) . ?
N6 B1 1.542(4) . ?
N3 C7 1.339(4) . ?
C9 C8 1.379(5) . ?
C9 C10 1.489(5) . ?
C14 C13 1.360(6) . ?
C14 C15 1.496(5) . ?
C4 C3 1.371(5) . ?
C4 C5 1.493(5) . ?
C2 C3 1.388(5) . ?
C2 C1 1.486(5) . ?
C8 H8 0.9500 . ?
C8 C7 1.386(5) . ?
C3 H3 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C7 C6 1.488(5) . ?
C12 C13 1.385(6) . ?
C12 C11 1.484(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C13 H13 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
B1 H1 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Dy1 Cl2 92.64(3) . . ?
Cl3 Dy1 Cl1 96.05(4) . . ?
Cl3 Dy1 Cl2 105.48(5) . . ?
N5 Dy1 Cl1 97.38(6) . . ?
N5 Dy1 Cl2 90.52(7) . . ?
N5 Dy1 Cl3 158.57(7) . . ?
N1 Dy1 Cl1 175.11(6) . . ?
N1 Dy1 Cl2 87.53(6) . . ?
N1 Dy1 Cl3 88.61(6) . . ?
N1 Dy1 N5 77.73(8) . . ?
N3 Dy1 Cl1 99.06(6) . . ?
N3 Dy1 Cl2 161.17(6) . . ?
N3 Dy1 Cl3 88.00(7) . . ?
N3 Dy1 N5 73.45(8) . . ?
N3 Dy1 N1 79.57(8) . . ?
N1 N2 B1 121.4(2) . . ?
C4 N2 N1 109.4(3) . . ?
C4 N2 B1 129.2(3) . . ?
N6 N5 Dy1 121.16(17) . . ?
C12 N5 Dy1 132.6(2) . . ?
C12 N5 N6 106.3(3) . . ?
N2 N1 Dy1 121.68(18) . . ?
C2 N1 Dy1 131.7(2) . . ?
C2 N1 N2 106.6(2) . . ?
N3 N4 B1 120.8(2) . . ?
C9 N4 N3 109.9(3) . . ?
C9 N4 B1 128.7(3) . . ?
C16 N7 C17 109.2(3) . . ?
C18 N7 C16 109.4(3) . . ?
C18 N7 C17 109.1(3) . . ?
C19 N7 C16 108.9(3) . . ?
C19 N7 C17 109.9(3) . . ?
C19 N7 C18 110.3(3) . . ?
N5 N6 B1 121.7(2) . . ?
C14 N6 N5 109.5(3) . . ?
C14 N6 B1 128.7(3) . . ?
N4 N3 Dy1 121.86(17) . . ?
C7 N3 Dy1 131.9(2) . . ?
C7 N3 N4 106.2(3) . . ?
N4 C9 C8 107.4(3) . . ?
N4 C9 C10 123.5(3) . . ?
C8 C9 C10 129.0(3) . . ?
N6 C14 C13 108.0(3) . . ?
N6 C14 C15 122.8(4) . . ?
C13 C14 C15 129.1(4) . . ?
N2 C4 C3 107.7(3) . . ?
N2 C4 C5 122.8(4) . . ?
C3 C4 C5 129.5(3) . . ?
N1 C2 C3 109.8(3) . . ?
N1 C2 C1 122.6(3) . . ?
C3 C2 C1 127.6(3) . . ?
C9 C8 H8 126.9 . . ?
C9 C8 C7 106.2(3) . . ?
C7 C8 H8 126.9 . . ?
C4 C3 C2 106.4(3) . . ?
C4 C3 H3 126.8 . . ?
C2 C3 H3 126.8 . . ?
N7 C16 H16A 109.5 . . ?
N7 C16 H16B 109.5 . . ?
N7 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C7 C8 110.3(3) . . ?
N3 C7 C6 121.0(3) . . ?
C8 C7 C6 128.7(3) . . ?
N5 C12 C13 109.8(3) . . ?
N5 C12 C11 121.4(4) . . ?
C13 C12 C11 128.8(3) . . ?
N7 C17 H17A 109.5 . . ?
N7 C17 H17B 109.5 . . ?
N7 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C14 C13 C12 106.5(3) . . ?
C14 C13 H13 126.8 . . ?
C12 C13 H13 126.8 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N2 B1 N4 111.1(3) . . ?
N2 B1 N6 110.1(2) . . ?
N2 B1 H1 109.0 . . ?
N4 B1 N6 108.5(2) . . ?
N4 B1 H1 109.0 . . ?
N6 B1 H1 109.0 . . ?
N7 C18 H18A 109.5 . . ?
N7 C18 H18B 109.5 . . ?
N7 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N7 C19 H19A 109.5 . . ?
N7 C19 H19B 109.5 . . ?
N7 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 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
Dy1 N5 N6 C14 -179.75(19) . . . . ?
Dy1 N5 N6 B1 -4.0(3) . . . . ?
Dy1 N5 C12 C13 179.5(2) . . . . ?
Dy1 N5 C12 C11 -1.0(5) . . . . ?
Dy1 N1 C2 C3 -179.6(2) . . . . ?
Dy1 N1 C2 C1 1.1(5) . . . . ?
Dy1 N3 C7 C8 178.4(2) . . . . ?
Dy1 N3 C7 C6 -2.1(4) . . . . ?
N2 N1 C2 C3 0.2(3) . . . . ?
N2 N1 C2 C1 -179.1(3) . . . . ?
N2 C4 C3 C2 0.1(4) . . . . ?
N5 N6 C14 C13 0.2(4) . . . . ?
N5 N6 C14 C15 -176.9(3) . . . . ?
N5 N6 B1 N2 63.0(3) . . . . ?
N5 N6 B1 N4 -58.8(3) . . . . ?
N5 C12 C13 C14 0.3(4) . . . . ?
N1 N2 C4 C3 0.0(3) . . . . ?
N1 N2 C4 C5 -178.9(3) . . . . ?
N1 N2 B1 N4 60.4(3) . . . . ?
N1 N2 B1 N6 -59.9(3) . . . . ?
N1 C2 C3 C4 -0.2(4) . . . . ?
N4 N3 C7 C8 0.0(3) . . . . ?
N4 N3 C7 C6 179.5(3) . . . . ?
N4 C9 C8 C7 0.7(4) . . . . ?
N6 N5 C12 C13 -0.2(4) . . . . ?
N6 N5 C12 C11 179.3(3) . . . . ?
N6 C14 C13 C12 -0.3(4) . . . . ?
N3 N4 C9 C8 -0.7(3) . . . . ?
N3 N4 C9 C10 176.9(3) . . . . ?
N3 N4 B1 N2 -66.0(3) . . . . ?
N3 N4 B1 N6 55.1(4) . . . . ?
C9 N4 N3 Dy1 -178.15(19) . . . . ?
C9 N4 N3 C7 0.4(3) . . . . ?
C9 N4 B1 N2 123.9(3) . . . . ?
C9 N4 B1 N6 -115.0(3) . . . . ?
C9 C8 C7 N3 -0.5(4) . . . . ?
C9 C8 C7 C6 -179.9(3) . . . . ?
C14 N6 B1 N2 -122.1(3) . . . . ?
C14 N6 B1 N4 116.1(3) . . . . ?
C4 N2 N1 Dy1 179.70(19) . . . . ?
C4 N2 N1 C2 -0.2(3) . . . . ?
C4 N2 B1 N4 -120.5(3) . . . . ?
C4 N2 B1 N6 119.3(3) . . . . ?
C12 N5 N6 C14 0.0(3) . . . . ?
C12 N5 N6 B1 175.8(3) . . . . ?
C10 C9 C8 C7 -176.8(3) . . . . ?
C5 C4 C3 C2 179.0(4) . . . . ?
C1 C2 C3 C4 179.1(3) . . . . ?
B1 N2 N1 Dy1 -1.0(3) . . . . ?
B1 N2 N1 C2 179.1(3) . . . . ?
B1 N2 C4 C3 -179.2(3) . . . . ?
B1 N2 C4 C5 1.9(5) . . . . ?
B1 N4 N3 Dy1 10.1(3) . . . . ?
B1 N4 N3 C7 -171.4(3) . . . . ?
B1 N4 C9 C8 170.3(3) . . . . ?
B1 N4 C9 C10 -12.1(5) . . . . ?
B1 N6 C14 C13 -175.2(3) . . . . ?
B1 N6 C14 C15 7.7(5) . . . . ?
C15 C14 C13 C12 176.5(4) . . . . ?
C11 C12 C13 C14 -179.1(4) . . . . ?
_shelx_res_file
;
TITL da1029_0m_a.res in P2(1)/n
da1029_0m_a.res
created by SHELXL-2017/1 at 16:25:35 on 08-Sep-2018
REM Old TITL da1029_0m in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.154, Rweak 0.006, Alpha 0.035, Orientation as input
REM Formula found by SHELXT: C22 Cl3 Dy N5
CELL 0.71073 9.4991 31.346 10.0158 90 118.04 90
ZERR 4 0.0029 0.0083 0.0029 0 0.008 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H B Cl Dy N
UNIT 76 136 4 12 4 28
L.S. 30
PLAN 20
SIZE 0.4 0.2 0.1
TEMP -163.15
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
OMIT 0 4 0
REM
REM
REM
WGHT 0.016200 6.101200
FVAR 0.09396
DY1 5 0.544210 0.367056 0.368168 11.00000 0.02670 0.01565 =
0.00893 -0.00145 0.00198 -0.00462
CL1 4 0.459030 0.405623 0.112706 11.00000 0.07488 0.03451 =
0.01618 0.00896 0.01715 0.01345
CL2 4 0.706392 0.309864 0.310826 11.00000 0.10751 0.02552 =
0.03704 0.00375 0.04287 0.02218
CL3 4 0.271383 0.332548 0.293713 11.00000 0.03453 0.03964 =
0.07846 0.01473 -0.01799 -0.02377
N2 6 0.710431 0.359232 0.746794 11.00000 0.01972 0.03089 =
0.01212 0.00356 0.00714 0.00665
N5 6 0.787193 0.407812 0.517824 11.00000 0.01844 0.01867 =
0.02333 -0.00327 0.01305 -0.00207
N1 6 0.643455 0.335005 0.616948 11.00000 0.01937 0.02180 =
0.01560 0.00339 0.00678 -0.00023
N4 6 0.564919 0.429244 0.649906 11.00000 0.02242 0.02462 =
0.01729 -0.00079 0.01222 0.00458
N7 6 0.236895 0.322240 0.740754 11.00000 0.02259 0.01919 =
0.03213 0.00016 0.01383 -0.00232
N6 6 0.832884 0.418402 0.665482 11.00000 0.01229 0.02118 =
0.02107 -0.00910 0.00266 -0.00111
N3 6 0.475094 0.422045 0.497141 11.00000 0.01543 0.02733 =
0.01678 0.00494 0.00737 0.00124
C9 1 0.497905 0.460672 0.693957 11.00000 0.03842 0.02213 =
0.03806 0.00387 0.03214 0.00406
C14 1 0.970376 0.440986 0.722260 11.00000 0.01269 0.01944 =
0.05336 -0.01280 0.00201 -0.00118
C4 1 0.754618 0.333490 0.868653 11.00000 0.02438 0.05242 =
0.01807 0.01560 0.01254 0.01630
C2 1 0.647609 0.294492 0.660491 11.00000 0.01830 0.02762 =
0.03306 0.01281 0.01035 0.00107
C8 1 0.363527 0.474339 0.567091 11.00000 0.03484 0.02595 =
0.05561 0.01777 0.03689 0.01367
AFIX 43
H8 2 0.292354 0.496304 0.562218 11.00000 -1.20000
AFIX 0
C3 1 0.715976 0.292432 0.817005 11.00000 0.02434 0.04106 =
0.03449 0.02545 0.01579 0.01152
AFIX 43
H3 2 0.732693 0.267508 0.876571 11.00000 -1.20000
AFIX 0
C16 1 0.364742 0.301333 0.878533 11.00000 0.02811 0.02888 =
0.04086 0.00469 0.01086 0.00183
AFIX 137
H16A 2 0.456324 0.294973 0.861914 11.00000 -1.50000
H16B 2 0.323658 0.274769 0.898677 11.00000 -1.50000
H16C 2 0.398089 0.320547 0.965363 11.00000 -1.50000
AFIX 0
C7 1 0.353203 0.449585 0.448144 11.00000 0.01688 0.03162 =
0.03722 0.01838 0.01714 0.00394
C12 1 0.898192 0.424185 0.485668 11.00000 0.03080 0.02596 =
0.05802 0.00802 0.03325 0.00272
C17 1 0.301280 0.362475 0.709063 11.00000 0.03942 0.02306 =
0.04736 0.00202 0.02746 -0.00413
AFIX 137
H17A 2 0.336183 0.381780 0.795826 11.00000 -1.50000
H17B 2 0.217687 0.376328 0.618900 11.00000 -1.50000
H17C 2 0.392055 0.355616 0.691749 11.00000 -1.50000
AFIX 0
C6 1 0.231177 0.451037 0.285966 11.00000 0.01853 0.05647 =
0.04360 0.02920 0.01084 0.00782
AFIX 137
H6A 2 0.283256 0.457174 0.223719 11.00000 -1.50000
H6B 2 0.153243 0.473460 0.271052 11.00000 -1.50000
H6C 2 0.176663 0.423435 0.256312 11.00000 -1.50000
AFIX 0
C10 1 0.561249 0.474805 0.853876 11.00000 0.07330 0.03024 =
0.04749 -0.00564 0.04689 0.00648
AFIX 137
H10A 2 0.539473 0.452854 0.911412 11.00000 -1.50000
H10B 2 0.509340 0.501534 0.856958 11.00000 -1.50000
H10C 2 0.676621 0.479328 0.898496 11.00000 -1.50000
AFIX 0
C5 1 0.828745 0.350057 1.026926 11.00000 0.06454 0.08409 =
0.01559 0.01455 0.01594 0.03298
AFIX 137
H5A 2 0.935563 0.361072 1.054792 11.00000 -1.50000
H5B 2 0.836734 0.326926 1.095973 11.00000 -1.50000
H5C 2 0.762595 0.373049 1.033901 11.00000 -1.50000
AFIX 0
C13 1 1.013474 0.445138 0.611231 11.00000 0.01966 0.02216 =
0.09171 -0.00032 0.02742 -0.00343
AFIX 43
H13 2 1.104713 0.459572 0.618400 11.00000 -1.20000
AFIX 0
C1 1 0.587538 0.258472 0.551314 11.00000 0.04829 0.02285 =
0.05010 0.01039 0.01015 -0.00958
AFIX 137
H1A 2 0.497896 0.268251 0.456519 11.00000 -1.50000
H1B 2 0.551889 0.235321 0.594017 11.00000 -1.50000
H1C 2 0.673224 0.248095 0.531427 11.00000 -1.50000
AFIX 0
B1 3 0.728161 0.407679 0.740801 11.00000 0.02328 0.02926 =
0.01073 -0.00472 0.00434 0.00490
AFIX 13
H1 2 0.780137 0.419225 0.846253 11.00000 -1.20000
AFIX 0
C18 1 0.186048 0.292938 0.609244 11.00000 0.08431 0.03677 =
0.03878 -0.00982 0.02077 -0.02326
AFIX 137
H18A 2 0.277071 0.286909 0.591413 11.00000 -1.50000
H18B 2 0.100787 0.306382 0.519177 11.00000 -1.50000
H18C 2 0.146794 0.266223 0.630523 11.00000 -1.50000
AFIX 0
C19 1 0.099730 0.332299 0.768342 11.00000 0.04290 0.05228 =
0.10086 0.03435 0.05298 0.01848
AFIX 137
H19A 2 0.056015 0.305777 0.785526 11.00000 -1.50000
H19B 2 0.017032 0.347078 0.680070 11.00000 -1.50000
H19C 2 0.135759 0.350669 0.857607 11.00000 -1.50000
AFIX 0
C15 1 1.056308 0.455533 0.883298 11.00000 0.02628 0.04107 =
0.06786 -0.03113 -0.01776 0.00367
AFIX 137
H15A 2 0.984174 0.472696 0.906297 11.00000 -1.50000
H15B 2 1.148788 0.472797 0.898805 11.00000 -1.50000
H15C 2 1.092256 0.430637 0.950287 11.00000 -1.50000
AFIX 0
C11 1 0.888550 0.418491 0.334452 11.00000 0.06358 0.06651 =
0.07692 0.02269 0.06202 0.01223
AFIX 137
H11A 2 0.950829 0.393398 0.335978 11.00000 -1.50000
H11B 2 0.931498 0.443853 0.309093 11.00000 -1.50000
H11C 2 0.776956 0.414462 0.258458 11.00000 -1.50000
AFIX 0
HKLF 4
REM da1029_0m_a.res in P2(1)/n
REM R1 = 0.0237 for 4713 Fo > 4sig(Fo) and 0.0270 for all 5062 data
REM 290 parameters refined using 0 restraints
END
WGHT 0.0162 6.1007
REM Highest difference peak 1.043, deepest hole -1.495, 1-sigma level 0.089
Q1 1 0.3177 0.3218 0.2603 11.00000 0.05 1.03
Q2 1 0.8321 0.4345 0.2663 11.00000 0.05 0.43
Q3 1 0.7586 0.3058 0.3032 11.00000 0.05 0.36
Q4 1 0.6557 0.2950 0.3205 11.00000 0.05 0.35
Q5 1 0.6159 0.3579 0.3826 11.00000 0.05 0.31
Q6 1 0.8473 0.3943 0.2981 11.00000 0.05 0.30
Q7 1 0.2639 0.3421 0.4377 11.00000 0.05 0.30
Q8 1 0.9688 0.4200 0.3535 11.00000 0.05 0.30
Q9 1 0.9037 0.3402 1.1168 11.00000 0.05 0.29
Q10 1 0.6458 0.3282 0.2804 11.00000 0.05 0.29
Q11 1 0.7619 0.3465 0.3237 11.00000 0.05 0.29
Q12 1 0.7030 0.3519 1.0328 11.00000 0.05 0.27
Q13 1 0.9818 0.4289 0.5526 11.00000 0.05 0.27
Q14 1 0.0511 0.3269 0.5465 11.00000 0.05 0.27
Q15 1 0.6245 0.3030 0.2418 11.00000 0.05 0.27
Q16 1 0.3976 0.3696 0.3809 11.00000 0.05 0.27
Q17 1 0.8151 0.3732 0.2850 11.00000 0.05 0.26
Q18 1 0.7869 0.4180 0.6910 11.00000 0.05 0.26
Q19 1 0.7838 0.3388 0.9464 11.00000 0.05 0.26
Q20 1 0.9736 0.4676 0.9591 11.00000 0.05 0.26
;
_shelx_res_checksum 61011
_olex2_submission_special_instructions 'No special instructions were received'