#------------------------------------------------------------------------------ #$Date: 2020-06-04 04:41:58 +0300 (Thu, 04 Jun 2020) $ #$Revision: 252627 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/06/7240603.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7240603 loop_ _publ_author_name 'Bo, Qi-Bing' 'Wang, Jia-Yin' 'Shi, Yang' 'Tao, Dong-Liang' 'Yin, Guo-Yin' _publ_section_title ; 2D chain layer versus 1D chain: rigid aromatic benzoate disassembling flexible alicyclic dicarboxylate-based lanthanide coordination polymers with enhanced photoluminescence and characteristic behavior of single-molecule magnet. ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00583E _journal_year 2020 _chemical_formula_moiety '0.5(C30 H36 Dy4 O30)' _chemical_formula_sum 'C15 H18 Dy2 O15' _chemical_formula_weight 763.29 _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' _space_group_name_H-M_alt 'P 1 21/m 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_date 2019-11-02 _audit_creation_method ; Olex2 1.2-alpha (compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261) ; _audit_update_record ; 2019-11-02 deposited with the CCDC. 2020-06-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.22(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.759(2) _cell_length_b 7.9677(16) _cell_length_c 12.790(3) _cell_measurement_reflns_used 2334 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.5400 _cell_measurement_theta_min 4.1860 _cell_volume 954.9(4) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _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)' _diffrn_ambient_temperature 293.15 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0355 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 35.00 88.00 1.0000 1.9850 omega____ theta____ kappa____ phi______ frames - 15.8569 178.0000 -60.0000 53 #__ type_ start__ end____ width___ exp.time_ 2 omega 35.00 88.00 1.0000 1.9850 omega____ theta____ kappa____ phi______ frames - 15.8569 178.0000 150.0000 53 #__ type_ start__ end____ width___ exp.time_ 3 omega -51.00 33.00 1.0000 1.9850 omega____ theta____ kappa____ phi______ frames - 15.8569 -57.0000 0.0000 84 #__ type_ start__ end____ width___ exp.time_ 4 omega -14.00 87.00 1.0000 1.9850 omega____ theta____ kappa____ phi______ frames - 15.8569 19.0000 0.0000 101 #__ type_ start__ end____ width___ exp.time_ 5 omega -11.00 24.00 1.0000 1.9850 omega____ theta____ kappa____ phi______ frames - 15.8569 77.0000 60.0000 35 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0261526000 _diffrn_orient_matrix_UB_12 0.0183357000 _diffrn_orient_matrix_UB_13 0.0565472000 _diffrn_orient_matrix_UB_21 -0.0355828000 _diffrn_orient_matrix_UB_22 -0.0720690000 _diffrn_orient_matrix_UB_23 0.0116426000 _diffrn_orient_matrix_UB_31 0.0613910000 _diffrn_orient_matrix_UB_32 -0.0490600000 _diffrn_orient_matrix_UB_33 0.0026529000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.710 _diffrn_reflns_av_R_equivalents 0.1028 _diffrn_reflns_av_unetI/netI 0.0993 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 6076 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.214 _diffrn_reflns_theta_max 26.339 _diffrn_reflns_theta_min 3.314 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 7.848 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.29451 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear whiteish white' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier whiteish _exptl_crystal_colour_primary white _exptl_crystal_density_diffrn 2.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 720 _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.024 _refine_diff_density_max 4.777 _refine_diff_density_min -5.173 _refine_diff_density_rms 0.495 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 89 _refine_ls_number_reflns 2076 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.076 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0963 _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^)+(0.0366P)^2^+120.5462P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2124 _refine_ls_wR_factor_ref 0.2233 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1646 _reflns_number_total 2076 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 150615_BQB_Dy in P2(1)/m CELL 0.71 9.759307 7.96766 12.790435 90 106.2195 90 ZERR 2 0.002392 0.001633 0.003 0 0.0252 0 LATT 1 SYMM -X,0.5+Y,-Z SFAC C H Dy O UNIT 30 36 4 30 EADP O1 O2 C1 C2 C3 EADP O3 C4 C5 C6 EADP O6 O5 C7 C8 C9 EADP O7 O8 O9 L.S. 100 0 0 PLAN 20 SIZE 0.024 0.12 0.38 TEMP 20 htab BOND $H CONF MORE -1 fmap 2 53 acta SHEL 999 0.8 OMIT -2 6 2 OMIT 3 6 2 OMIT -2 4 2 OMIT 0 5 4 OMIT -2 8 2 OMIT -1 5 3 OMIT -1 4 3 REM REM REM WGHT 0.036600 120.546196 FVAR 3.97922 DY1 3 0.490221 0.750000 0.132992 10.50000 0.01268 0.00966 = 0.02761 0.00000 0.00951 0.00000 DY2 3 0.895198 0.250000 0.505004 10.50000 0.01127 0.03099 = 0.02571 0.00000 0.00885 0.00000 O1 4 0.583710 0.569665 0.275324 11.00000 0.02443 0.03587 = 0.06825 0.02020 0.00367 0.00448 O2 4 0.720138 0.426252 0.413631 11.00000 0.02443 0.03587 = 0.06825 0.02020 0.00367 0.00448 O3 4 0.656380 0.931056 0.088433 11.00000 0.01884 0.00748 = 0.03890 0.00425 0.01383 0.00379 O4 4 0.679724 1.041171 -0.066538 11.00000 0.02813 0.02245 = 0.03543 0.00755 0.01029 0.00438 O5 4 0.997551 0.574429 0.598047 11.00000 0.05637 0.01670 = 0.03614 0.00914 0.01824 -0.00113 O6 4 0.844564 0.422863 0.646547 11.00000 0.05637 0.01670 = 0.03614 0.00914 0.01824 -0.00113 O7 4 0.451884 0.750000 -0.063618 10.50000 0.02536 0.00869 = 0.05437 0.00000 0.01822 0.00000 AFIX 3 0.8600 H7A 2 0.407344 0.828820 -0.105438 10.50000 -1.50000 H7B 2 0.405634 0.672120 -0.105388 10.50000 -1.50000 AFIX 0 O8 4 0.321392 0.750000 0.238918 10.50000 0.02536 0.00869 = 0.05437 0.00000 0.01822 0.00000 AFIX 3 0.8600 H8A 2 0.309902 0.822510 0.285558 10.50000 -1.50000 H8B 2 0.256772 0.677290 0.240228 10.50000 -1.50000 AFIX 0 O9 4 1.134190 0.250000 0.615316 10.50000 0.02536 0.00869 = 0.05437 0.00000 0.01822 0.00000 AFIX 3 0.8600 H9A 2 1.166850 0.174400 0.663876 10.50000 -1.50000 H9B 2 1.211420 0.295120 0.608726 10.50000 -1.50000 AFIX 0 C1 1 0.599680 0.452035 0.341132 11.00000 0.02443 0.03587 = 0.06825 0.02020 0.00367 0.00448 C2 1 0.473763 0.347127 0.343463 11.00000 0.02443 0.03587 = 0.06825 0.02020 0.00367 0.00448 AFIX 13 H2 2 0.382357 0.396100 0.302649 11.00000 -1.20000 AFIX 0 C3 1 0.465431 0.250000 0.441625 10.50000 0.02443 0.03587 = 0.06825 0.02020 0.00367 0.00448 AFIX 23 H3A 2 0.375067 0.249998 0.459357 10.50000 -1.20000 H3B 2 0.548977 0.250001 0.504205 10.50000 -1.20000 AFIX 0 C4 1 0.718081 0.945007 0.013880 11.00000 0.01884 0.00748 = 0.03890 0.00425 0.01383 0.00379 C5 1 0.850795 0.846402 0.021794 11.00000 0.01884 0.00748 = 0.03890 0.00425 0.01383 0.00379 AFIX 13 H5 2 0.914895 0.897015 -0.016227 11.00000 -1.20000 AFIX 0 C6 1 0.926040 0.750000 0.123372 10.50000 0.01884 0.00748 = 0.03890 0.00425 0.01383 0.00379 AFIX 23 H6A 2 1.029552 0.750001 0.145190 10.50000 -1.20000 H6B 2 0.882975 0.749998 0.183157 10.50000 -1.20000 AFIX 0 C7 1 0.923474 0.551007 0.661097 11.00000 0.05637 0.01670 = 0.03614 0.00914 0.01824 -0.00113 C8 1 0.925420 0.655915 0.755310 11.00000 0.05637 0.01670 = 0.03614 0.00914 0.01824 -0.00113 AFIX 13 H8 2 0.877280 0.605738 0.805463 11.00000 -1.20000 AFIX 0 C9 1 1.061054 0.750000 0.811248 10.50000 0.05637 0.01670 = 0.03614 0.00914 0.01824 -0.00113 AFIX 23 H9C 2 1.091818 0.750001 0.890216 10.50000 -1.20000 H9D 2 1.137644 0.749999 0.776555 10.50000 -1.20000 AFIX 0 HKLF 4 REM 150615_BQB_Dy in P2(1)/m REM R1 = 0.0963 for 1646 Fo > 4sig(Fo) and 0.1100 for all 2076 data REM 89 parameters refined using 0 restraints END WGHT 0.0366 120.5649 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y+2, -z HTAB O7 O3_$1 EQIV $2 -x+1, y-1/2, -z HTAB O7 O3_$2 EQIV $3 -x+1, y+1/2, -z+1 HTAB O8 O6_$3 EQIV $4 -x+1, -y+1, -z+1 HTAB O8 O6_$4 EQIV $5 -x+2, y-1/2, -z+1 HTAB O9 O1_$5 HTAB O9 O2_$5 EQIV $6 -x+2, -y+1, -z+1 HTAB O9 O1_$6 HTAB O9 O2_$6 REM Highest difference peak 4.777, deepest hole -5.173, 1-sigma level 0.495 Q1 1 0.8860 0.2500 0.5801 10.50000 0.05 4.78 Q2 1 0.4990 0.7500 0.0669 10.50000 0.05 4.72 Q3 1 0.9139 0.2500 0.4408 10.50000 0.05 4.63 Q4 1 0.4494 0.7500 0.0614 10.50000 0.05 4.02 Q5 1 0.5442 0.7500 0.2034 10.50000 0.05 4.01 Q6 1 0.4815 0.7500 0.2083 10.50000 0.05 3.91 Q7 1 0.9529 0.2500 0.5793 10.50000 0.05 3.69 Q8 1 0.7503 0.2500 0.5613 10.50000 0.05 2.98 Q9 1 0.9272 0.3304 0.5180 11.00000 0.05 2.56 Q10 1 0.3086 0.3243 0.1512 11.00000 0.05 2.53 Q11 1 0.9103 0.6751 0.7780 11.00000 0.05 2.46 Q12 1 0.8293 0.2500 0.4191 10.50000 0.05 2.39 Q13 1 0.3116 0.7500 0.1822 10.50000 0.05 2.15 Q14 1 0.7783 0.2500 0.6380 10.50000 0.05 2.05 Q15 1 0.3882 0.7500 0.2737 10.50000 0.05 1.98 Q16 1 1.0286 0.2500 0.6605 10.50000 0.05 1.87 Q17 1 0.9937 0.3427 0.6263 11.00000 0.05 1.83 Q18 1 1.1214 0.6715 0.6383 11.00000 0.05 1.78 Q19 1 0.5162 0.8369 0.1395 11.00000 0.05 1.71 Q20 1 0.2955 0.2500 0.2983 10.50000 0.05 1.67 REM The information below was added by Olex2. REM REM R1 = 0.0963 for 1646 Fo > 4sig(Fo) and 0.1100 for all 6614 data REM n/a parameters refined using n/a restraints REM Highest difference peak 4.78, deepest hole -5.17 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1100 REM R1_gt = 0.0963 REM wR_ref = 0.2233 REM GOOF = 1.076 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 6614 REM Reflections_gt = 1646 REM Parameters = n/a REM Hole = -5.17 REM Peak = 4.78 REM Flack = n/a ; _cod_data_source_file d0ce00583e2.cif _cod_data_source_block cpdc-Dy _cod_original_cell_volume 955.0(4) _cod_database_code 7240603 _shelxl_version_number 2013-2 _chemical_oxdiff_formula 'C H O Dy' _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. ; _shelx_estimated_absorpt_t_max 0.834 _shelx_estimated_absorpt_t_min 0.154 _reflns_odcompleteness_completeness 99.38 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(O1) = Uanis(O2) = Uanis(C1) = Uanis(C2) = Uanis(C3) Uanis(O3) = Uanis(C4) = Uanis(C5) = Uanis(C6) Uanis(O6) = Uanis(O5) = Uanis(C7) = Uanis(C8) = Uanis(C9) Uanis(O7) = Uanis(O8) = Uanis(O9) 3. Others Fixed Sof: H7A(0.5) H7B(0.5) H8A(0.5) H8B(0.5) H9A(0.5) H9B(0.5) 4.a Riding coordinates: O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B) 4.b Ternary CH refined with riding coordinates: C2(H2), C5(H5), C8(H8) 4.c Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C6(H6A,H6B), C9(H9C,H9D) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' 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 0.49022(13) 0.7500 0.13299(11) 0.0159(4) Uani 1 2 d S T P . . Dy2 Dy 0.89520(13) 0.2500 0.50500(11) 0.0219(4) Uani 1 2 d S T P . . O1 O 0.5837(16) 0.570(2) 0.2753(15) 0.045(3) Uani 1 1 d . . . . . O2 O 0.7201(16) 0.426(2) 0.4136(15) 0.045(3) Uani 1 1 d . . . . . O3 O 0.6564(13) 0.9311(17) 0.0884(12) 0.021(2) Uani 1 1 d . . . . . O4 O 0.6797(15) 1.041(2) -0.0665(12) 0.028(3) Uani 1 1 d . . . . . O5 O 0.9976(18) 0.574(2) 0.5980(13) 0.035(2) Uani 1 1 d . . . . . O6 O 0.8446(18) 0.423(2) 0.6465(13) 0.035(2) Uani 1 1 d . . . . . O7 O 0.452(2) 0.7500 -0.0636(19) 0.028(3) Uani 1 2 d S T P . . H7A H 0.4073 0.8288 -0.1054 0.042 Uiso 0.5 1 d R . . . . H7B H 0.4056 0.6721 -0.1054 0.042 Uiso 0.5 1 d R . . . . O8 O 0.321(2) 0.7500 0.2389(19) 0.028(3) Uani 1 2 d S T P . . H8A H 0.3099 0.8225 0.2856 0.042 Uiso 0.5 1 d R . . . . H8B H 0.2568 0.6773 0.2402 0.042 Uiso 0.5 1 d R . . . . O9 O 1.134(2) 0.2500 0.6153(19) 0.028(3) Uani 1 2 d S T P . . H9A H 1.1669 0.1744 0.6639 0.042 Uiso 0.5 1 d R . . . . H9B H 1.2114 0.2951 0.6087 0.042 Uiso 0.5 1 d R . . . . C1 C 0.600(2) 0.452(4) 0.341(2) 0.045(3) Uani 1 1 d . . . . . C2 C 0.474(2) 0.347(3) 0.343(2) 0.045(3) Uani 1 1 d . . . . . H2 H 0.3824 0.3961 0.3026 0.054 Uiso 1 1 calc R . . . . C3 C 0.465(4) 0.2500 0.442(3) 0.045(3) Uani 1 2 d S T P . . H3A H 0.3751 0.2500 0.4594 0.054 Uiso 1 2 calc RS T P . . H3B H 0.5490 0.2500 0.5042 0.054 Uiso 1 2 calc RS T P . . C4 C 0.718(2) 0.945(2) 0.0139(17) 0.021(2) Uani 1 1 d . . . . . C5 C 0.8508(19) 0.846(2) 0.0218(17) 0.021(2) Uani 1 1 d . . . . . H5 H 0.9149 0.8970 -0.0162 0.025 Uiso 1 1 calc R . . . . C6 C 0.926(3) 0.7500 0.123(3) 0.021(2) Uani 1 2 d S T P . . H6A H 1.0296 0.7500 0.1452 0.025 Uiso 1 2 calc RS T P . . H6B H 0.8830 0.7500 0.1832 0.025 Uiso 1 2 calc RS T P . . C7 C 0.923(3) 0.551(3) 0.6611(19) 0.035(2) Uani 1 1 d . . . . . C8 C 0.925(3) 0.656(3) 0.7553(19) 0.035(2) Uani 1 1 d . . . . . H8 H 0.8773 0.6057 0.8055 0.042 Uiso 1 1 calc R . . . . C9 C 1.061(4) 0.7500 0.811(3) 0.035(2) Uani 1 2 d S T P . . H9C H 1.0918 0.7500 0.8902 0.042 Uiso 1 2 calc RS T P . . H9D H 1.1376 0.7500 0.7766 0.042 Uiso 1 2 calc RS 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 0.0127(6) 0.0097(6) 0.0276(7) 0.000 0.0095(5) 0.000 Dy2 0.0113(6) 0.0310(8) 0.0257(7) 0.000 0.0088(5) 0.000 O1 0.024(4) 0.036(6) 0.068(7) 0.020(6) 0.004(4) 0.004(5) O2 0.024(4) 0.036(6) 0.068(7) 0.020(6) 0.004(4) 0.004(5) O3 0.019(4) 0.007(4) 0.039(5) 0.004(4) 0.014(4) 0.004(4) O4 0.028(7) 0.022(8) 0.035(8) 0.008(7) 0.010(6) 0.004(7) O5 0.056(6) 0.017(4) 0.036(5) 0.009(4) 0.018(4) -0.001(4) O6 0.056(6) 0.017(4) 0.036(5) 0.009(4) 0.018(4) -0.001(4) O7 0.025(6) 0.009(6) 0.054(8) 0.000 0.018(6) 0.000 O8 0.025(6) 0.009(6) 0.054(8) 0.000 0.018(6) 0.000 O9 0.025(6) 0.009(6) 0.054(8) 0.000 0.018(6) 0.000 C1 0.024(4) 0.036(6) 0.068(7) 0.020(6) 0.004(4) 0.004(5) C2 0.024(4) 0.036(6) 0.068(7) 0.020(6) 0.004(4) 0.004(5) C3 0.024(4) 0.036(6) 0.068(7) 0.020(6) 0.004(4) 0.004(5) C4 0.019(4) 0.007(4) 0.039(5) 0.004(4) 0.014(4) 0.004(4) C5 0.019(4) 0.007(4) 0.039(5) 0.004(4) 0.014(4) 0.004(4) C6 0.019(4) 0.007(4) 0.039(5) 0.004(4) 0.014(4) 0.004(4) C7 0.056(6) 0.017(4) 0.036(5) 0.009(4) 0.018(4) -0.001(4) C8 0.056(6) 0.017(4) 0.036(5) 0.009(4) 0.018(4) -0.001(4) C9 0.056(6) 0.017(4) 0.036(5) 0.009(4) 0.018(4) -0.001(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Dy1 O1 77.4(10) . 4_575 ? O1 Dy1 O3 115.2(5) . . ? O1 Dy1 O3 70.2(6) 4_575 . ? O1 Dy1 O3 115.2(5) 4_575 4_575 ? O1 Dy1 O3 70.2(6) . 4_575 ? O1 Dy1 O4 85.8(6) . 2_645 ? O1 Dy1 O4 144.9(6) 4_575 2_645 ? O1 Dy1 O4 144.9(6) . 3_675 ? O1 Dy1 O4 85.8(6) 4_575 3_675 ? O1 Dy1 O7 136.9(5) . . ? O1 Dy1 O7 136.9(5) 4_575 . ? O1 Dy1 O8 74.8(6) . . ? O1 Dy1 O8 74.7(6) 4_575 . ? O3 Dy1 O3 75.5(6) 4_575 . ? O3 Dy1 O7 70.6(5) 4_575 . ? O3 Dy1 O7 70.6(5) . . ? O3 Dy1 O8 139.6(4) 4_575 . ? O3 Dy1 O8 139.6(4) . . ? O4 Dy1 O3 144.6(5) 3_675 4_575 ? O4 Dy1 O3 144.6(5) 2_645 . ? O4 Dy1 O3 86.7(5) 2_645 4_575 ? O4 Dy1 O3 86.7(5) 3_675 . ? O4 Dy1 O4 90.9(8) 2_645 3_675 ? O4 Dy1 O7 74.7(5) 3_675 . ? O4 Dy1 O7 74.7(5) 2_645 . ? O4 Dy1 O8 71.1(5) 2_645 . ? O4 Dy1 O8 71.1(5) 3_675 . ? O8 Dy1 O7 130.4(7) . . ? O2 Dy2 O2 76.5(9) 4_565 . ? O2 Dy2 O5 77.5(6) 4_565 4_565 ? O2 Dy2 O5 117.9(7) 4_565 3_766 ? O2 Dy2 O5 152.4(6) . 4_565 ? O2 Dy2 O5 74.5(6) 4_565 2_746 ? O2 Dy2 O5 74.5(6) . 3_766 ? O2 Dy2 O5 77.5(6) . . ? O2 Dy2 O5 117.9(7) . 2_746 ? O2 Dy2 O5 152.4(6) 4_565 . ? O2 Dy2 O6 75.7(6) 4_565 4_565 ? O2 Dy2 O6 117.0(6) . 4_565 ? O2 Dy2 O6 117.0(6) 4_565 . ? O2 Dy2 O6 75.7(6) . . ? O2 Dy2 O9 141.5(5) . . ? O2 Dy2 O9 141.5(5) 4_565 . ? O5 Dy2 O5 127.0(3) 3_766 4_565 ? O5 Dy2 O5 63.0(6) 3_766 . ? O5 Dy2 O5 72.8(8) 2_746 3_766 ? O5 Dy2 O5 63.0(6) 2_746 4_565 ? O5 Dy2 O5 127.0(3) 2_746 . ? O5 Dy2 O5 125.8(6) . 4_565 ? O5 Dy2 O6 107.1(5) 3_766 . ? O5 Dy2 O6 165.0(6) 3_766 4_565 ? O5 Dy2 O6 107.1(5) 2_746 4_565 ? O5 Dy2 O6 165.0(6) 2_746 . ? O5 Dy2 O9 79.4(6) 2_746 . ? O5 Dy2 O9 79.4(6) 3_766 . ? O6 Dy2 O5 46.3(5) 4_565 4_565 ? O6 Dy2 O5 108.5(5) 4_565 . ? O6 Dy2 O5 46.3(5) . . ? O6 Dy2 O5 108.5(5) . 4_565 ? O6 Dy2 O6 69.0(7) . 4_565 ? O9 Dy2 O5 65.6(3) . 4_565 ? O9 Dy2 O5 65.6(4) . . ? O9 Dy2 O6 85.8(6) . . ? O9 Dy2 O6 85.8(6) . 4_565 ? C1 O1 Dy1 163.1(16) . . ? C1 O2 Dy2 150.5(19) . . ? C4 O3 Dy1 137.7(13) . . ? C4 O4 Dy1 138.9(13) . 3_675 ? Dy2 O5 Dy2 117.0(6) 3_766 . ? C7 O5 Dy2 86.3(15) . . ? C7 O5 Dy2 152.2(16) . 3_766 ? C7 O6 Dy2 109.0(15) . . ? Dy1 O7 H7A 123.2 . . ? Dy1 O7 H7B 122.9 . . ? H7A O7 H7B 93.1 . . ? Dy1 O8 H8A 129.2 . . ? Dy1 O8 H8B 129.2 . . ? H8A O8 H8B 101.6 . . ? Dy2 O9 H9A 122.4 . . ? Dy2 O9 H9B 133.4 . . ? H9A O9 H9B 101.9 . . ? O1 C1 O2 122(2) . . ? O1 C1 C2 119(2) . . ? O2 C1 C2 119(2) . . ? C1 C2 C2 124.0(14) . 4_565 ? C1 C2 H2 113.5 . . ? C1 C2 C3 123(2) . . ? C2 C2 H2 113.5 4_565 . ? C3 C2 C2 58.9(14) . 4_565 ? C3 C2 H2 113.5 . . ? C2 C3 C2 62(3) . 4_565 ? C2 C3 H3A 117.5 . . ? C2 C3 H3A 117.5 4_565 . ? C2 C3 H3B 117.5 . . ? C2 C3 H3B 117.5 4_565 . ? H3A C3 H3B 114.6 . . ? O3 C4 C5 119.2(17) . . ? O4 C4 O3 125.1(18) . . ? O4 C4 C5 115.6(17) . . ? C4 C5 C5 121.7(10) . 4_575 ? C4 C5 H5 114.3 . . ? C4 C5 C6 122.0(19) . . ? C5 C5 H5 114.3 4_575 . ? C6 C5 C5 59.5(9) . 4_575 ? C6 C5 H5 114.3 . . ? C5 C6 C5 61.1(18) 4_575 . ? C5 C6 H6A 117.7 . . ? C5 C6 H6A 117.7 4_575 . ? C5 C6 H6B 117.7 4_575 . ? C5 C6 H6B 117.7 . . ? H6A C6 H6B 114.8 . . ? O5 C7 O6 118(2) . . ? O5 C7 C8 125(2) . . ? O6 C7 C8 117(2) . . ? C7 C8 C8 124.9(12) . 4_575 ? C7 C8 H8 114.1 . . ? C7 C8 C9 119(2) . . ? C8 C8 H8 114.1 4_575 . ? C8 C8 C9 60.4(11) 4_575 . ? C9 C8 H8 114.1 . . ? C8 C9 C8 59(2) 4_575 . ? C8 C9 H9C 117.8 4_575 . ? C8 C9 H9C 117.8 . . ? C8 C9 H9D 117.8 . . ? C8 C9 H9D 117.8 4_575 . ? H9C C9 H9D 115.0 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O1 2.299(17) . ? Dy1 O1 2.299(17) 4_575 ? Dy1 O3 2.356(13) . ? Dy1 O3 2.356(13) 4_575 ? Dy1 O4 2.335(15) 3_675 ? Dy1 O4 2.335(15) 2_645 ? Dy1 O7 2.44(2) . ? Dy1 O8 2.41(2) . ? Dy2 O2 2.267(16) 4_565 ? Dy2 O2 2.267(16) . ? Dy2 O5 2.358(16) 2_746 ? Dy2 O5 2.358(16) 3_766 ? Dy2 O5 2.904(17) . ? Dy2 O5 2.904(17) 4_565 ? Dy2 O6 2.433(17) . ? Dy2 O6 2.433(17) 4_565 ? Dy2 O9 2.36(2) . ? O1 C1 1.24(3) . ? O2 C1 1.29(3) . ? O3 C4 1.27(2) . ? O4 Dy1 2.335(15) 3_675 ? O4 C4 1.25(2) . ? O5 Dy2 2.358(16) 3_766 ? O5 C7 1.24(3) . ? O6 C7 1.26(3) . ? O7 H7A 0.8600 . ? O7 H7B 0.8599 . ? O8 H8A 0.8600 . ? O8 H8B 0.8600 . ? O9 H9A 0.8600 . ? O9 H9B 0.8602 . ? C1 C2 1.49(3) . ? C2 C2 1.55(5) 4_565 ? C2 H2 0.9800 . ? C2 C3 1.50(4) . ? C3 C2 1.50(4) 4_565 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.49(2) . ? C5 C5 1.54(4) 4_575 ? C5 H5 0.9800 . ? C5 C6 1.51(3) . ? C6 C5 1.51(3) 4_575 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.46(3) . ? C8 C8 1.50(4) 4_575 ? C8 H8 0.9800 . ? C8 C9 1.52(4) . ? C9 C8 1.52(4) 4_575 ? C9 H9C 0.9700 . ? C9 H9D 0.9700 . ? 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 O1 C1 O2 174(5) . . . . ? Dy1 O1 C1 C2 -12(9) . . . . ? Dy1 O3 C4 O4 98(2) . . . . ? Dy1 O3 C4 C5 -84(2) . . . . ? Dy1 O4 C4 O3 5(4) 3_675 . . . ? Dy1 O4 C4 C5 -172.6(14) 3_675 . . . ? Dy2 O2 C1 O1 -135(3) . . . . ? Dy2 O2 C1 C2 51(5) . . . . ? Dy2 O5 C7 O6 143(3) 3_766 . . . ? Dy2 O5 C7 O6 -5(2) . . . . ? Dy2 O5 C7 C8 171(2) . . . . ? Dy2 O5 C7 C8 -40(5) 3_766 . . . ? Dy2 O6 C7 O5 7(3) . . . . ? Dy2 O6 C7 C8 -170.2(17) . . . . ? O1 C1 C2 C2 132(2) . . . 4_565 ? O1 C1 C2 C3 -156(3) . . . . ? O2 C1 C2 C2 -54(3) . . . 4_565 ? O2 C1 C2 C3 19(4) . . . . ? O3 C4 C5 C5 62(2) . . . 4_575 ? O3 C4 C5 C6 -9(3) . . . . ? O4 C4 C5 C5 -120.1(15) . . . 4_575 ? O4 C4 C5 C6 168.5(17) . . . . ? O5 C7 C8 C8 44(3) . . . 4_575 ? O5 C7 C8 C9 -28(3) . . . . ? O6 C7 C8 C8 -138.9(16) . . . 4_575 ? O6 C7 C8 C9 149(2) . . . . ? C1 C2 C3 C2 -113(2) . . . 4_565 ? C4 C5 C6 C5 110.6(16) . . . 4_575 ? C7 C8 C9 C8 116.0(18) . . . 4_575 ?