#------------------------------------------------------------------------------ #$Date: 2019-10-11 06:18:30 +0300 (Fri, 11 Oct 2019) $ #$Revision: 219270 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234538.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_7234538 loop_ _publ_author_name 'Han, Mei-rong' 'Zhang, Han-tao' 'Wang, Jia-nan' 'Feng, Si-si' 'Lu, Li-ping' _publ_section_title ; Three chiral one-dimensional lanthanide--ditoluoyl-tartrate bifunctional polymers exhibiting luminescence and magnetic behaviors ; _journal_issue 55 _journal_name_full 'RSC Advances' _journal_page_first 32288 _journal_paper_doi 10.1039/C9RA06920H _journal_volume 9 _journal_year 2019 _chemical_absolute_configuration rm _chemical_formula_moiety 'C63 H63 Dy O27' _chemical_formula_sum 'C63 H63 Dy O27' _chemical_formula_weight 1414.63 _chemical_name_systematic 2 _space_group_crystal_system trigonal _space_group_IT_number 146 _space_group_name_Hall 'R 3' _space_group_name_H-M_alt 'R 3 :H' _symmetry_space_group_name_Hall 'R 3' _symmetry_space_group_name_H-M 'R 3 :H' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-07-12 deposited with the CCDC. 2019-10-02 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 3 _cell_length_a 27.1659(11) _cell_length_b 27.1659(11) _cell_length_c 7.6520(4) _cell_measurement_reflns_used 8141 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.978 _cell_measurement_theta_min 1.477 _cell_volume 4890.5(4) _computing_cell_refinement 'HKL 2000' _computing_data_collection marccd165 _computing_data_reduction 'HKL 2000' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.948 _diffrn_measurement_device_type marccd165 _diffrn_measurement_method 'oscillation mode' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.700 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_unetI/netI 0.0624 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.948 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 8134 _diffrn_reflns_point_group_measured_fraction_full 0.535 _diffrn_reflns_point_group_measured_fraction_max 0.499 _diffrn_reflns_theta_full 24.835 _diffrn_reflns_theta_max 30.988 _diffrn_reflns_theta_min 2.558 _diffrn_source 'synchrotron, 3W1A at BSRF' _exptl_absorpt_coefficient_mu 1.176 _exptl_absorpt_correction_T_max 0.838 _exptl_absorpt_correction_T_min 0.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.441 _exptl_crystal_description needle-shaped _exptl_crystal_F_000 2169 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _refine_diff_density_max 1.547 _refine_diff_density_min -1.651 _refine_diff_density_rms 0.123 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.51(3) _refine_ls_extinction_coef 0.0059(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 279 _refine_ls_number_reflns 3629 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0425 _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^)+(0.0562P)^2^+8.6128P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1037 _refine_ls_wR_factor_ref 0.1042 _reflns_Friedel_coverage 0.053 _reflns_Friedel_fraction_full 0.071 _reflns_Friedel_fraction_max 0.050 _reflns_number_gt 3615 _reflns_number_total 3629 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ra06920h2.cif _cod_data_source_block 2 _cod_original_cell_volume 4890.5(5) _cod_database_code 7234538 _shelx_shelxl_version_number 2018/3 _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_min 0.719 _shelx_estimated_absorpt_t_max 0.799 _shelx_res_file ; TITL 2 in R3 New: R3 2.res created by SHELXL-2018/3 at 18:15:35 on 25-Jun-2019 CELL 0.7000 27.1659 27.1659 7.6520 90.000 90.000 120.000 ZERR 3 0.0011 0.0011 0.0004 0 0 0 LATT -3 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SFAC C H O Dy DISP C 0.003 0.002 11.0 DISP H 0.000 0.000 0.7 DISP Dy -0.127 4.317 17597.6 DISP O 0.010 0.006 30.8 UNIT 189 189 81 3 OMIT -1 5 0 OMIT -1 1 1 OMIT -1 4 1 OMIT 1 1 0 L.S. 10 ACTA BOND $H FMAP 2 PLAN 5 SIZE 0.30 0.20 0.20 CONF TWIN -1 0 0 0 -1 0 0 0 -1 2 EQIV $1 -y, x-y, z-1 EQIV $2 x, y, z-1 EQIV $3 -x+y, -x, z HTAB C21 O8_$1 HTAB O2 O3_$2 HTAB O9 O6_$3 WGHT 0.056200 8.612801 EXTI 0.005892 BASF 0.50923 FVAR 0.07126 DY1 4 0.000000 0.000000 0.583516 10.33330 0.02200 0.02200 = 0.01442 0.00000 0.00000 0.01100 C1 1 0.115119 0.048487 0.849495 11.00000 0.02281 0.03802 = 0.01900 -0.00549 -0.00523 0.01483 C2 1 0.116149 0.035323 1.044370 11.00000 0.02086 0.03013 = 0.01856 -0.00110 -0.00171 0.01076 AFIX 13 H2 2 0.077659 0.006930 1.081024 11.00000 -1.20000 AFIX 0 C3 1 0.135986 0.088958 1.153127 11.00000 0.02769 0.02665 = 0.02062 -0.00101 0.00486 0.01303 AFIX 13 H3 2 0.114874 0.107823 1.117359 11.00000 -1.20000 AFIX 0 C4 1 0.123445 0.071840 1.346174 11.00000 0.02763 0.03198 = 0.02364 -0.00514 0.00192 0.01539 C5 1 0.138260 -0.038928 1.029145 11.00000 0.03594 0.03474 = 0.02072 0.00098 -0.00036 0.01570 C6 1 0.178050 -0.057085 1.091268 11.00000 0.04463 0.03535 = 0.03093 0.00136 0.00164 0.02307 C7 1 0.164446 -0.113106 1.073988 11.00000 0.08018 0.03817 = 0.05236 -0.00220 -0.00761 0.03435 AFIX 43 H7 2 0.131282 -0.138435 1.015590 11.00000 -1.20000 AFIX 0 C8 1 0.198174 -0.132029 1.139914 11.00000 0.09718 0.04333 = 0.06871 -0.00251 -0.01663 0.05083 AFIX 43 H8 2 0.186732 -0.170428 1.131266 11.00000 -1.20000 AFIX 0 C9 1 0.250392 -0.094681 1.221586 11.00000 0.08248 0.05115 = 0.05403 0.00594 -0.00060 0.04913 C10 1 0.265264 -0.037451 1.235428 11.00000 0.06247 0.05157 = 0.06112 -0.00057 -0.01036 0.03989 AFIX 43 H10 2 0.299680 -0.011546 1.286625 11.00000 -1.20000 AFIX 0 C11 1 0.228755 -0.018775 1.172818 11.00000 0.04477 0.03618 = 0.04410 -0.00358 -0.00646 0.02465 AFIX 43 H11 2 0.238441 0.019056 1.185827 11.00000 -1.20000 AFIX 0 C12 1 0.289449 -0.114512 1.292094 11.00000 0.12612 0.08445 = 0.07588 0.00154 -0.01876 0.08625 AFIX 137 H12A 2 0.279417 -0.126726 1.410986 11.00000 -1.50000 H12B 2 0.328032 -0.083794 1.287459 11.00000 -1.50000 H12C 2 0.285735 -0.145629 1.222678 11.00000 -1.50000 AFIX 0 C13 1 0.215539 0.179781 1.176433 11.00000 0.02796 0.04057 = 0.02426 0.00426 0.00248 0.01270 C14 1 0.276690 0.214082 1.141868 11.00000 0.03355 0.04082 = 0.02901 -0.00014 0.00394 0.01583 C15 1 0.305501 0.194579 1.039230 11.00000 0.02912 0.03446 = 0.04709 0.00100 0.00014 0.01647 AFIX 43 H15 2 0.286894 0.157392 0.998010 11.00000 -1.20000 AFIX 0 C16 1 0.362079 0.230768 0.998537 11.00000 0.03990 0.04156 = 0.04606 0.00215 0.01059 0.02100 AFIX 43 H16 2 0.380550 0.217994 0.924774 11.00000 -1.20000 AFIX 0 C17 1 0.391750 0.285124 1.064212 11.00000 0.02613 0.04550 = 0.04339 -0.00195 0.00244 0.01162 C18 1 0.363069 0.304011 1.168553 11.00000 0.04015 0.04608 = 0.05992 -0.01095 -0.00137 0.01227 AFIX 43 H18 2 0.382185 0.340874 1.212367 11.00000 -1.20000 AFIX 0 C19 1 0.305852 0.268548 1.209049 11.00000 0.03816 0.04463 = 0.04682 -0.01478 0.00398 0.01217 AFIX 43 H19 2 0.287274 0.281569 1.281407 11.00000 -1.20000 AFIX 0 C20 1 0.454597 0.324608 1.026496 11.00000 0.03413 0.05193 = 0.05030 0.00030 0.00873 0.01131 AFIX 137 H20A 2 0.464965 0.362790 1.058112 11.00000 -1.50000 H20B 2 0.461692 0.323163 0.904228 11.00000 -1.50000 H20C 2 0.476766 0.312770 1.093364 11.00000 -1.50000 AFIX 0 C21 1 -0.154115 -0.095534 0.477651 11.00000 0.03852 0.04297 = 0.03791 -0.00486 -0.00517 0.02264 AFIX 137 H21A 2 -0.162884 -0.070985 0.410856 11.00000 -1.50000 H21B 2 -0.187160 -0.122194 0.541853 11.00000 -1.50000 H21C 2 -0.142617 -0.115743 0.400211 11.00000 -1.50000 AFIX 0 O1 3 0.070805 0.045771 0.797848 11.00000 0.02679 0.03802 = 0.02173 -0.00661 -0.00374 0.01699 O2 3 0.158926 0.061456 0.759567 11.00000 0.02890 0.05273 = 0.02069 -0.00225 0.00142 0.01753 AFIX 3 H2A 2 0.162645 0.071577 0.655168 11.00000 -1.50000 AFIX 0 O3 3 0.165063 0.088613 1.449560 11.00000 0.02946 0.03976 = 0.01773 0.00069 0.00152 0.01222 O4 3 0.071808 0.041499 1.379658 11.00000 0.03121 0.04137 = 0.02741 -0.00370 0.00219 0.01668 O5 3 0.154126 0.014563 1.083879 11.00000 0.02592 0.02951 = 0.02051 -0.00045 -0.00205 0.01332 O6 3 0.095431 -0.067026 0.940644 11.00000 0.03990 0.03299 = 0.04347 -0.01570 -0.00363 0.01255 O7 3 0.194251 0.125150 1.117650 11.00000 0.02839 0.03138 = 0.02150 -0.00276 0.00188 0.00982 O8 3 0.186054 0.196495 1.244112 11.00000 0.04132 0.04024 = 0.03742 -0.00836 0.00219 0.01763 O9 3 -0.109028 -0.062336 0.596683 11.00000 0.03096 0.04439 = 0.02358 -0.00011 0.00155 0.01589 AFIX 3 H9A 2 -0.129952 -0.062633 0.690294 11.00000 -1.50000 AFIX 0 HKLF 4 1 0 1 0 1 0 0 0 0 -1 REM 2 in R3 New: R3 REM wR2 = 0.1042, GooF = S = 1.084, Restrained GooF = 1.084 for all data REM R1 = 0.0425 for 3615 Fo > 4sig(Fo) and 0.0428 for all 3629 data REM 279 parameters refined using 1 restraints END WGHT 0.0563 8.5319 REM Highest difference peak 1.547, deepest hole -1.651, 1-sigma level 0.123 Q1 1 0.0000 0.0000 0.4391 10.33333 0.05 1.55 Q2 1 0.0000 0.0000 0.7291 10.33333 0.05 1.49 Q3 1 -0.0371 -0.0002 0.5088 11.00000 0.05 1.09 Q4 1 0.0378 0.0476 0.6032 11.00000 0.05 0.98 Q5 1 -0.0115 0.0367 0.5475 11.00000 0.05 0.98 ; _shelx_res_checksum 75086 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 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 Dy1 Dy 0.000000 0.000000 0.58352(2) 0.01947(12) Uani 1 3 d S T P C1 C 0.1151(2) 0.0485(3) 0.8495(7) 0.0268(10) Uani 1 1 d . . . C2 C 0.1161(2) 0.0353(2) 1.0444(7) 0.0241(9) Uani 1 1 d . . . H2 H 0.077659 0.006930 1.081024 0.029 Uiso 1 1 calc R U . C3 C 0.1360(2) 0.0890(2) 1.1531(7) 0.0252(10) Uani 1 1 d . . . H3 H 0.114874 0.107823 1.117359 0.030 Uiso 1 1 calc R U . C4 C 0.1234(2) 0.0718(2) 1.3462(8) 0.0275(10) Uani 1 1 d . . . C5 C 0.1383(3) -0.0389(3) 1.0291(8) 0.0313(12) Uani 1 1 d . . . C6 C 0.1781(3) -0.0571(3) 1.0913(9) 0.0356(13) Uani 1 1 d . . . C7 C 0.1644(5) -0.1131(4) 1.0740(13) 0.055(2) Uani 1 1 d . . . H7 H 0.131282 -0.138435 1.015590 0.066 Uiso 1 1 calc R U . C8 C 0.1982(5) -0.1320(4) 1.1399(16) 0.063(3) Uani 1 1 d . . . H8 H 0.186732 -0.170428 1.131266 0.075 Uiso 1 1 calc R U . C9 C 0.2504(5) -0.0947(4) 1.2216(14) 0.056(2) Uani 1 1 d . . . C10 C 0.2653(4) -0.0375(4) 1.2354(14) 0.053(2) Uani 1 1 d . . . H10 H 0.299680 -0.011546 1.286625 0.064 Uiso 1 1 calc R U . C11 C 0.2288(3) -0.0188(3) 1.1728(11) 0.0397(14) Uani 1 1 d . . . H11 H 0.238441 0.019056 1.185827 0.048 Uiso 1 1 calc R U . C12 C 0.2894(6) -0.1145(6) 1.2921(18) 0.081(4) Uani 1 1 d . . . H12A H 0.279417 -0.126726 1.410986 0.121 Uiso 1 1 calc R U . H12B H 0.328032 -0.083794 1.287459 0.121 Uiso 1 1 calc R U . H12C H 0.285735 -0.145629 1.222678 0.121 Uiso 1 1 calc R U . C13 C 0.2155(3) 0.1798(3) 1.1764(8) 0.0329(12) Uani 1 1 d . . . C14 C 0.2767(3) 0.2141(3) 1.1419(9) 0.0357(13) Uani 1 1 d . . . C15 C 0.3055(3) 0.1946(3) 1.0392(11) 0.0366(14) Uani 1 1 d . . . H15 H 0.286894 0.157392 0.998010 0.044 Uiso 1 1 calc R U . C16 C 0.3621(3) 0.2308(3) 0.9985(11) 0.0422(15) Uani 1 1 d . . . H16 H 0.380550 0.217994 0.924774 0.051 Uiso 1 1 calc R U . C17 C 0.3918(3) 0.2851(3) 1.0642(11) 0.0411(15) Uani 1 1 d . . . C18 C 0.3631(4) 0.3040(4) 1.1686(13) 0.053(2) Uani 1 1 d . . . H18 H 0.382185 0.340874 1.212367 0.063 Uiso 1 1 calc R U . C19 C 0.3059(3) 0.2685(3) 1.2090(12) 0.0470(17) Uani 1 1 d . . . H19 H 0.287274 0.281569 1.281407 0.056 Uiso 1 1 calc R U . C20 C 0.4546(3) 0.3246(4) 1.0265(13) 0.0500(18) Uani 1 1 d . . . H20A H 0.464965 0.362790 1.058112 0.075 Uiso 1 1 calc R U . H20B H 0.461692 0.323163 0.904228 0.075 Uiso 1 1 calc R U . H20C H 0.476766 0.312770 1.093364 0.075 Uiso 1 1 calc R U . C21 C -0.1541(3) -0.0955(3) 0.4777(10) 0.0388(14) Uani 1 1 d . . . H21A H -0.162884 -0.070985 0.410856 0.058 Uiso 1 1 calc R U . H21B H -0.187160 -0.122194 0.541853 0.058 Uiso 1 1 calc R U . H21C H -0.142617 -0.115743 0.400211 0.058 Uiso 1 1 calc R U . O1 O 0.07080(18) 0.04577(19) 0.7978(6) 0.0285(8) Uani 1 1 d . . . O2 O 0.15893(19) 0.0615(2) 0.7596(6) 0.0354(10) Uani 1 1 d . . . H2A H 0.162645 0.071577 0.655168 0.053 Uiso 1 1 d R U . O3 O 0.16506(18) 0.0886(2) 1.4496(6) 0.0312(9) Uani 1 1 d . . . O4 O 0.0718(2) 0.0415(2) 1.3797(6) 0.0340(9) Uani 1 1 d . . . O5 O 0.15413(17) 0.01456(17) 1.0839(5) 0.0256(7) Uani 1 1 d . . . O6 O 0.0954(2) -0.0670(2) 0.9406(8) 0.0413(11) Uani 1 1 d . . . O7 O 0.19425(19) 0.1251(2) 1.1176(6) 0.0294(8) Uani 1 1 d . . . O8 O 0.1861(2) 0.1965(2) 1.2441(7) 0.0409(11) Uani 1 1 d . . . O9 O -0.1090(2) -0.0623(2) 0.5967(6) 0.0343(9) Uani 1 1 d . . . H9A H -0.129952 -0.062633 0.690294 0.051 Uiso 1 1 d R U . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02200(13) 0.02200(13) 0.01442(14) 0.000 0.000 0.01100(7) C1 0.023(2) 0.038(3) 0.019(2) -0.005(2) -0.0052(18) 0.015(2) C2 0.021(2) 0.030(2) 0.019(2) -0.0011(18) -0.0017(17) 0.0108(18) C3 0.028(2) 0.027(2) 0.021(2) -0.001(2) 0.005(2) 0.013(2) C4 0.028(2) 0.032(3) 0.024(2) -0.005(2) 0.002(2) 0.015(2) C5 0.036(3) 0.035(3) 0.021(2) 0.001(2) 0.000(2) 0.016(3) C6 0.045(3) 0.035(3) 0.031(3) 0.001(2) 0.002(3) 0.023(3) C7 0.080(6) 0.038(4) 0.052(5) -0.002(4) -0.008(5) 0.034(4) C8 0.097(8) 0.043(5) 0.069(6) -0.003(4) -0.017(6) 0.051(5) C9 0.082(6) 0.051(5) 0.054(5) 0.006(4) -0.001(5) 0.049(5) C10 0.062(5) 0.052(4) 0.061(5) -0.001(4) -0.010(4) 0.040(4) C11 0.045(3) 0.036(3) 0.044(4) -0.004(3) -0.006(3) 0.025(3) C12 0.126(10) 0.084(7) 0.076(7) 0.002(6) -0.019(7) 0.086(8) C13 0.028(3) 0.041(3) 0.024(3) 0.004(2) 0.002(2) 0.013(2) C14 0.034(3) 0.041(3) 0.029(3) 0.000(3) 0.004(2) 0.016(3) C15 0.029(3) 0.034(3) 0.047(4) 0.001(3) 0.000(3) 0.016(3) C16 0.040(4) 0.042(3) 0.046(4) 0.002(3) 0.011(3) 0.021(3) C17 0.026(3) 0.045(3) 0.043(4) -0.002(3) 0.002(3) 0.012(3) C18 0.040(4) 0.046(4) 0.060(5) -0.011(4) -0.001(4) 0.012(3) C19 0.038(3) 0.045(4) 0.047(4) -0.015(3) 0.004(3) 0.012(3) C20 0.034(3) 0.052(4) 0.050(4) 0.000(4) 0.009(3) 0.011(3) C21 0.039(3) 0.043(3) 0.038(3) -0.005(3) -0.005(3) 0.023(3) O1 0.0268(18) 0.038(2) 0.0217(18) -0.0066(16) -0.0037(15) 0.0170(16) O2 0.029(2) 0.053(3) 0.0207(18) -0.0022(19) 0.0014(16) 0.0175(19) O3 0.0295(19) 0.040(2) 0.0177(17) 0.0007(16) 0.0015(15) 0.0122(17) O4 0.031(2) 0.041(2) 0.027(2) -0.0037(18) 0.0022(17) 0.0167(18) O5 0.0259(17) 0.0295(18) 0.0205(17) -0.0004(15) -0.0021(14) 0.0133(15) O6 0.040(2) 0.033(2) 0.043(3) -0.016(2) -0.004(2) 0.0126(19) O7 0.028(2) 0.031(2) 0.0215(18) -0.0028(16) 0.0019(16) 0.0098(17) O8 0.041(2) 0.040(2) 0.037(3) -0.008(2) 0.002(2) 0.018(2) O9 0.031(2) 0.044(2) 0.0236(19) -0.0001(18) 0.0016(17) 0.0159(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0100 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1270 4.3170 '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 O4 Dy1 O4 79.20(19) 3_554 2_554 O4 Dy1 O4 79.20(19) 3_554 1_554 O4 Dy1 O4 79.20(19) 2_554 1_554 O4 Dy1 O1 134.36(17) 3_554 2 O4 Dy1 O1 86.85(16) 2_554 2 O4 Dy1 O1 140.38(16) 1_554 2 O4 Dy1 O1 140.38(16) 3_554 . O4 Dy1 O1 134.36(17) 2_554 . O4 Dy1 O1 86.85(16) 1_554 . O1 Dy1 O1 76.83(17) 2 . O4 Dy1 O1 86.84(16) 3_554 3 O4 Dy1 O1 140.38(16) 2_554 3 O4 Dy1 O1 134.36(17) 1_554 3 O1 Dy1 O1 76.83(17) 2 3 O1 Dy1 O1 76.83(17) . 3 O4 Dy1 O9 139.64(17) 3_554 3 O4 Dy1 O9 70.32(16) 2_554 3 O4 Dy1 O9 69.77(16) 1_554 3 O1 Dy1 O9 70.62(15) 2 3 O1 Dy1 O9 64.08(15) . 3 O1 Dy1 O9 133.40(15) 3 3 O4 Dy1 O9 69.77(16) 3_554 2 O4 Dy1 O9 139.64(17) 2_554 2 O4 Dy1 O9 70.32(16) 1_554 2 O1 Dy1 O9 133.40(15) 2 2 O1 Dy1 O9 70.62(15) . 2 O1 Dy1 O9 64.08(15) 3 2 O9 Dy1 O9 119.848(15) 3 2 O4 Dy1 O9 70.32(16) 3_554 . O4 Dy1 O9 69.77(16) 2_554 . O4 Dy1 O9 139.64(17) 1_554 . O1 Dy1 O9 64.08(15) 2 . O1 Dy1 O9 133.40(15) . . O1 Dy1 O9 70.62(15) 3 . O9 Dy1 O9 119.850(14) 3 . O9 Dy1 O9 119.847(15) 2 . O1 C1 O2 126.7(5) . . O1 C1 C2 115.3(5) . . O2 C1 C2 118.0(5) . . O5 C2 C3 106.3(4) . . O5 C2 C1 113.4(4) . . C3 C2 C1 110.3(5) . . O5 C2 H2 108.9 . . C3 C2 H2 108.9 . . C1 C2 H2 108.9 . . O7 C3 C2 107.4(4) . . O7 C3 C4 113.5(5) . . C2 C3 C4 108.5(4) . . O7 C3 H3 109.1 . . C2 C3 H3 109.1 . . C4 C3 H3 109.1 . . O4 C4 O3 128.1(6) . . O4 C4 C3 113.8(5) . . O3 C4 C3 118.1(5) . . O6 C5 O5 122.0(6) . . O6 C5 C6 126.6(7) . . O5 C5 C6 111.4(5) . . C7 C6 C11 119.1(7) . . C7 C6 C5 120.1(7) . . C11 C6 C5 120.8(6) . . C8 C7 C6 121.6(9) . . C8 C7 H7 119.2 . . C6 C7 H7 119.2 . . C7 C8 C9 121.3(9) . . C7 C8 H8 119.3 . . C9 C8 H8 119.3 . . C10 C9 C8 117.4(8) . . C10 C9 C12 120.3(10) . . C8 C9 C12 122.3(9) . . C9 C10 C11 120.7(9) . . C9 C10 H10 119.6 . . C11 C10 H10 119.6 . . C6 C11 C10 119.8(7) . . C6 C11 H11 120.1 . . C10 C11 H11 120.1 . . C9 C12 H12A 109.5 . . C9 C12 H12B 109.5 . . H12A C12 H12B 109.5 . . C9 C12 H12C 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . O8 C13 O7 122.9(6) . . O8 C13 C14 126.0(6) . . O7 C13 C14 111.1(6) . . C19 C14 C15 119.3(7) . . C19 C14 C13 118.3(6) . . C15 C14 C13 122.4(7) . . C16 C15 C14 119.6(7) . . C16 C15 H15 120.2 . . C14 C15 H15 120.2 . . C17 C16 C15 121.8(7) . . C17 C16 H16 119.1 . . C15 C16 H16 119.1 . . C16 C17 C18 118.2(7) . . C16 C17 C20 122.4(7) . . C18 C17 C20 119.3(7) . . C17 C18 C19 120.9(7) . . C17 C18 H18 119.6 . . C19 C18 H18 119.6 . . C14 C19 C18 120.1(7) . . C14 C19 H19 119.9 . . C18 C19 H19 119.9 . . C17 C20 H20A 109.5 . . C17 C20 H20B 109.5 . . H20A C20 H20B 109.5 . . C17 C20 H20C 109.5 . . H20A C20 H20C 109.5 . . H20B C20 H20C 109.5 . . O9 C21 H21A 109.5 . . O9 C21 H21B 109.5 . . H21A C21 H21B 109.5 . . O9 C21 H21C 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . C1 O1 Dy1 140.3(4) . . C1 O2 H2A 123.8 . . C4 O4 Dy1 149.2(4) . 1_556 C5 O5 C2 116.7(4) . . C13 O7 C3 114.2(5) . . C21 O9 Dy1 137.0(4) . . C21 O9 H9A 99.3 . . Dy1 O9 H9A 122.9 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Dy1 O4 2.304(5) 3_554 Dy1 O4 2.304(5) 2_554 Dy1 O4 2.304(5) 1_554 Dy1 O1 2.355(4) 2 Dy1 O1 2.355(4) . Dy1 O1 2.355(4) 3 Dy1 O9 2.576(5) 3 Dy1 O9 2.576(5) 2 Dy1 O9 2.576(5) . C1 O1 1.234(6) . C1 O2 1.263(7) . C1 C2 1.537(8) . C2 O5 1.434(6) . C2 C3 1.523(8) . C2 H2 0.9800 . C3 O7 1.410(7) . C3 C4 1.535(8) . C3 H3 0.9800 . C4 O4 1.248(7) . C4 O3 1.264(7) . C5 O6 1.228(8) . C5 O5 1.359(8) . C5 C6 1.473(10) . C6 C7 1.381(10) . C6 C11 1.392(10) . C7 C8 1.352(14) . C7 H7 0.9300 . C8 C9 1.412(16) . C8 H8 0.9300 . C9 C10 1.401(12) . C9 C12 1.510(12) . C10 C11 1.405(10) . C10 H10 0.9300 . C11 H11 0.9300 . C12 H12A 0.9600 . C12 H12B 0.9600 . C12 H12C 0.9600 . C13 O8 1.216(8) . C13 O7 1.372(8) . C13 C14 1.466(9) . C14 C19 1.382(10) . C14 C15 1.387(11) . C15 C16 1.384(10) . C15 H15 0.9300 . C16 C17 1.376(11) . C16 H16 0.9300 . C17 C18 1.381(12) . C17 C20 1.522(10) . C18 C19 1.394(11) . C18 H18 0.9300 . C19 H19 0.9300 . C20 H20A 0.9600 . C20 H20B 0.9600 . C20 H20C 0.9600 . C21 O9 1.428(8) . C21 H21A 0.9600 . C21 H21B 0.9600 . C21 H21C 0.9600 . O2 H2A 0.8344 . O9 H9A 0.9120 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C21 H21A O8 0.96 2.58 3.539(9) 174.3 2_554 yes O2 H2A O3 0.83 1.63 2.465(6) 176.0 1_554 yes O9 H9A O6 0.91 2.11 2.922(8) 147.5 3 yes 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_4 O1 C1 C2 O5 154.2(5) . O2 C1 C2 O5 -26.6(7) . O1 C1 C2 C3 -86.8(6) . O2 C1 C2 C3 92.4(6) . O5 C2 C3 O7 53.4(6) . C1 C2 C3 O7 -69.9(6) . O5 C2 C3 C4 -69.6(5) . C1 C2 C3 C4 167.1(4) . O7 C3 C4 O4 177.5(5) . C2 C3 C4 O4 -63.2(6) . O7 C3 C4 O3 -3.6(7) . C2 C3 C4 O3 115.7(6) . O6 C5 C6 C7 -9.9(12) . O5 C5 C6 C7 169.4(7) . O6 C5 C6 C11 172.2(7) . O5 C5 C6 C11 -8.5(9) . C11 C6 C7 C8 2.4(14) . C5 C6 C7 C8 -175.5(9) . C6 C7 C8 C9 -3.3(18) . C7 C8 C9 C10 1.5(17) . C7 C8 C9 C12 -178.4(11) . C8 C9 C10 C11 1.1(15) . C12 C9 C10 C11 -178.9(10) . C7 C6 C11 C10 0.2(12) . C5 C6 C11 C10 178.2(8) . C9 C10 C11 C6 -2.0(14) . O8 C13 C14 C19 8.2(11) . O7 C13 C14 C19 -173.4(7) . O8 C13 C14 C15 -169.3(7) . O7 C13 C14 C15 9.1(9) . C19 C14 C15 C16 -3.2(12) . C13 C14 C15 C16 174.2(7) . C14 C15 C16 C17 3.3(13) . C15 C16 C17 C18 -2.2(13) . C15 C16 C17 C20 177.5(8) . C16 C17 C18 C19 1.2(14) . C20 C17 C18 C19 -178.5(9) . C15 C14 C19 C18 2.3(13) . C13 C14 C19 C18 -175.3(8) . C17 C18 C19 C14 -1.3(15) . O2 C1 O1 Dy1 56.2(10) . C2 C1 O1 Dy1 -124.7(5) . O3 C4 O4 Dy1 13.0(13) 1_556 C3 C4 O4 Dy1 -168.3(6) 1_556 O6 C5 O5 C2 4.5(9) . C6 C5 O5 C2 -174.9(5) . C3 C2 O5 C5 167.3(5) . C1 C2 O5 C5 -71.4(6) . O8 C13 O7 C3 -4.1(9) . C14 C13 O7 C3 177.5(5) . C2 C3 O7 C13 166.9(5) . C4 C3 O7 C13 -73.2(6) .