#------------------------------------------------------------------------------ #$Date: 2019-10-11 06:18:30 +0300 (Fri, 11 Oct 2019) $ #$Revision: 219270 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234540.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_7234540 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 Ho O27' _chemical_formula_sum 'C63 H63 Ho O27' _chemical_formula_weight 1417.06 _chemical_name_systematic 3 _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-2014/7 _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 27.0729(11) _cell_length_b 27.0729(11) _cell_length_c 7.6370(4) _cell_measurement_reflns_used 9141 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 31.449 _cell_measurement_theta_min 2.639 _cell_volume 4847.6(4) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT, SADABS and XPREP' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type marccd165 _diffrn_measurement_method 'oscillation mode' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.720 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_unetI/netI 0.0259 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 9141 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.595 _diffrn_reflns_theta_max 31.249 _diffrn_reflns_theta_min 2.640 _diffrn_source 'synchrotron, 3W1A at BSRF' _exptl_absorpt_coefficient_mu 1.347 _exptl_absorpt_correction_T_max 0.817 _exptl_absorpt_correction_T_min 0.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour 'light pink' _exptl_crystal_density_diffrn 1.456 _exptl_crystal_description needle-shaped _exptl_crystal_F_000 2172 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _refine_diff_density_max 2.361 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.243 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.42(5) _refine_ls_extinction_coef 0.044(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 279 _refine_ls_number_reflns 3590 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.128 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0615 _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^)+(0.1337P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1504 _refine_ls_wR_factor_ref 0.1504 _reflns_Friedel_coverage 1.000 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.998 _reflns_number_gt 3590 _reflns_number_total 3590 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ra06920h2.cif _cod_data_source_block 3 _cod_original_cell_volume 4847.6(5) _cod_database_code 7234540 _shelx_shelxl_version_number 2014/7 _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 0.688 _shelx_estimated_absorpt_t_max 0.774 _shelx_res_file ; 3.res created by SHELXL-2014/7 TITL 3 in R3 New: R3 CELL 0.7200 27.0729 27.0729 7.6370 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 Ho DISP C 0.003 0.002 11.6 DISP H 0.000 0.000 0.7 DISP Ho -0.155 4.803 20096.9 DISP O 0.011 0.006 33.1 UNIT 189 189 81 3 L.S. 20 ACTA BOND $H FMAP 2 PLAN 5 SIZE 0.3 0.2 0.2 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 0.133700 EXTI 0.043772 BASF 0.42287 FVAR 0.13049 HO1 4 0.000000 0.000000 -0.416490 10.33330 0.03399 0.03399 = 0.01946 0.00000 0.00000 0.01699 C1 1 0.114647 0.049134 -0.151030 11.00000 0.03598 0.07792 = 0.02219 -0.01011 -0.00483 0.02097 C2 1 0.115545 0.034675 0.043711 11.00000 0.04314 0.05346 = 0.03378 -0.00525 -0.00119 0.02147 AFIX 13 H2 2 0.076626 0.006662 0.079364 11.00000 -1.20000 AFIX 0 C3 1 0.135871 0.089056 0.155210 11.00000 0.05140 0.05536 = 0.03154 -0.00542 -0.00277 0.02718 AFIX 13 H3 2 0.114224 0.107742 0.121944 11.00000 -1.20000 AFIX 0 C4 1 0.123505 0.070420 0.348261 11.00000 0.04387 0.06601 = 0.02894 -0.00417 0.00886 0.01699 C5 1 0.137578 -0.036232 0.033270 11.00000 0.05083 0.07440 = 0.05489 0.02832 0.01167 0.01717 C6 1 0.178532 -0.057518 0.094085 11.00000 0.06794 0.05181 = 0.05753 0.00704 0.01012 0.03184 C7 1 0.162638 -0.115127 0.076937 11.00000 0.10606 0.06261 = 0.07440 0.00048 0.00504 0.03877 AFIX 43 H7 2 0.128711 -0.140739 0.021794 11.00000 -1.20000 AFIX 0 C8 1 0.198098 -0.132810 0.143034 11.00000 0.17368 0.06904 = 0.08914 -0.00230 -0.00891 0.07946 AFIX 43 H8 2 0.187382 -0.171163 0.134950 11.00000 -1.20000 AFIX 0 C9 1 0.250919 -0.094305 0.223848 11.00000 0.13441 0.09618 = 0.06971 0.01317 0.00308 0.08610 C10 1 0.264458 -0.037915 0.237342 11.00000 0.08336 0.07643 = 0.08081 -0.00100 -0.00925 0.05119 AFIX 43 H10 2 0.298647 -0.011711 0.289971 11.00000 -1.20000 AFIX 0 C11 1 0.227921 -0.019280 0.173648 11.00000 0.07618 0.06348 = 0.05863 0.00078 -0.00509 0.04491 AFIX 43 H11 2 0.237367 0.018633 0.185713 11.00000 -1.20000 AFIX 0 C12 1 0.287849 -0.115867 0.294274 11.00000 0.19548 0.17644 = 0.10948 0.03253 -0.00049 0.15457 AFIX 137 H12A 2 0.284865 -0.118103 0.419616 11.00000 -1.50000 H12B 2 0.326743 -0.090333 0.261433 11.00000 -1.50000 H12C 2 0.275771 -0.153080 0.247217 11.00000 -1.50000 AFIX 0 C13 1 0.213647 0.180110 0.173553 11.00000 0.04435 0.06762 = 0.04826 0.00880 0.00721 0.01531 C14 1 0.275367 0.214462 0.138465 11.00000 0.05280 0.06273 = 0.05227 -0.00210 0.00424 0.02203 C15 1 0.304166 0.194713 0.039566 11.00000 0.05143 0.05350 = 0.07269 0.00219 0.00279 0.02592 AFIX 43 H15 2 0.285384 0.157143 0.000505 11.00000 -1.20000 AFIX 0 C16 1 0.362097 0.230998 -0.003341 11.00000 0.05485 0.06824 = 0.06308 0.00381 0.01365 0.03097 AFIX 43 H16 2 0.380460 0.217868 -0.076794 11.00000 -1.20000 AFIX 0 C17 1 0.391518 0.285222 0.061851 11.00000 0.04340 0.07349 = 0.06555 -0.00153 0.00686 0.01648 C18 1 0.362302 0.304203 0.167409 11.00000 0.05529 0.06981 = 0.09998 -0.02478 -0.00212 0.02137 AFIX 43 H18 2 0.381512 0.340993 0.212836 11.00000 -1.20000 AFIX 0 C19 1 0.305500 0.269232 0.205122 11.00000 0.06430 0.07511 = 0.08225 -0.02341 0.01189 0.02025 AFIX 43 H19 2 0.286970 0.282633 0.276792 11.00000 -1.20000 AFIX 0 C20 1 0.455023 0.325171 0.026717 11.00000 0.05317 0.09155 = 0.07275 0.01117 0.01241 0.02768 AFIX 137 H20A 2 0.474489 0.340376 0.135592 11.00000 -1.50000 H20B 2 0.459807 0.355862 -0.047595 11.00000 -1.50000 H20C 2 0.470641 0.304357 -0.029904 11.00000 -1.50000 AFIX 0 C21 1 -0.154871 -0.095551 -0.531099 11.00000 0.05542 0.05357 = 0.10993 -0.00062 0.01280 0.02919 AFIX 137 H21A 2 -0.137907 -0.097220 -0.639700 11.00000 -1.50000 H21B 2 -0.177974 -0.078337 -0.550400 11.00000 -1.50000 H21C 2 -0.178212 -0.133452 -0.486151 11.00000 -1.50000 AFIX 0 O1 3 0.070570 0.044068 -0.204120 11.00000 0.04576 0.08109 = 0.03780 -0.00355 0.00068 0.03074 O2 3 0.159096 0.061538 -0.241331 11.00000 0.04235 0.08875 = 0.04067 -0.00305 0.00142 0.02851 AFIX 3 H2A 2 0.162815 0.071659 -0.345732 11.00000 -1.50000 AFIX 0 O3 3 0.165400 0.086827 0.450046 11.00000 0.04081 0.07576 = 0.02252 -0.00241 0.00177 0.01748 O4 3 0.072212 0.040457 0.380781 11.00000 0.04456 0.07735 = 0.03615 -0.00358 -0.00083 0.02698 O5 3 0.152803 0.012116 0.085705 11.00000 0.04671 0.08174 = 0.03061 0.00180 0.00258 0.03815 O6 3 0.094358 -0.067755 -0.055235 11.00000 0.06626 0.06385 = 0.05961 -0.01422 -0.00386 0.02996 O7 3 0.193015 0.124934 0.116616 11.00000 0.05689 0.06363 = 0.03234 -0.00723 -0.00145 0.01560 O8 3 0.185310 0.197118 0.241946 11.00000 0.06109 0.07182 = 0.06688 -0.01013 0.00413 0.02987 O9 3 -0.108586 -0.060451 -0.400857 11.00000 0.03203 0.08897 = 0.04041 -0.00416 0.00083 0.01672 AFIX 3 H9A 2 -0.129509 -0.060748 -0.307246 11.00000 -1.50000 AFIX 0 HKLF 4 1 0 1 0 1 0 0 0 0 -1 REM 3 in R3 New: R3 REM R1 = 0.0615 for 3590 Fo > 4sig(Fo) and 0.0615 for all 3590 data REM 279 parameters refined using 1 restraints END WGHT 0.1337 0.0000 REM Highest difference peak 2.361, deepest hole -0.632, 1-sigma level 0.243 Q1 1 0.0390 0.0149 -0.4268 11.00000 0.05 2.36 Q2 1 0.0294 0.0379 -0.4149 11.00000 0.05 2.28 Q3 1 0.0133 -0.0246 -0.4921 11.00000 0.05 1.73 Q4 1 -0.0195 -0.0368 -0.3328 11.00000 0.05 1.55 Q5 1 0.1911 0.0651 0.1149 11.00000 0.05 1.43 ; _shelx_res_checksum 31181 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 Ho1 Ho 0.0000 0.0000 -0.41649(2) 0.0291(2) Uani 1 3 d S T P C1 C 0.1146(3) 0.0491(5) -0.1510(12) 0.049(2) Uani 1 1 d . . . C2 C 0.1155(4) 0.0347(4) 0.0437(14) 0.0447(16) Uani 1 1 d . . . H2 H 0.0766 0.0067 0.0794 0.054 Uiso 1 1 calc R U . C3 C 0.1359(4) 0.0891(4) 0.1552(14) 0.0459(17) Uani 1 1 d . . . H3 H 0.1142 0.1077 0.1219 0.055 Uiso 1 1 calc R U . C4 C 0.1235(4) 0.0704(5) 0.3483(14) 0.051(2) Uani 1 1 d . . . C5 C 0.1376(5) -0.0362(8) 0.033(2) 0.066(3) Uani 1 1 d . . . C6 C 0.1785(6) -0.0575(5) 0.094(2) 0.058(2) Uani 1 1 d . . . C7 C 0.1626(11) -0.1151(7) 0.077(3) 0.083(5) Uani 1 1 d . . . H7 H 0.1287 -0.1407 0.0218 0.099 Uiso 1 1 calc R U . C8 C 0.1981(15) -0.1328(9) 0.143(4) 0.102(9) Uani 1 1 d . . . H8 H 0.1874 -0.1712 0.1349 0.123 Uiso 1 1 calc R U . C9 C 0.2509(11) -0.0943(10) 0.224(3) 0.087(6) Uani 1 1 d . . . C10 C 0.2645(8) -0.0379(8) 0.237(3) 0.075(4) Uani 1 1 d . . . H10 H 0.2986 -0.0117 0.2900 0.090 Uiso 1 1 calc R U . C11 C 0.2279(7) -0.0193(6) 0.174(2) 0.062(3) Uani 1 1 d . . . H11 H 0.2374 0.0186 0.1857 0.074 Uiso 1 1 calc R U . C12 C 0.2878(19) -0.1159(18) 0.294(5) 0.133(13) Uani 1 1 d . . . H12A H 0.2849 -0.1181 0.4196 0.200 Uiso 1 1 calc R U . H12B H 0.3267 -0.0903 0.2614 0.200 Uiso 1 1 calc R U . H12C H 0.2758 -0.1531 0.2472 0.200 Uiso 1 1 calc R U . C13 C 0.2136(5) 0.1801(6) 0.1736(18) 0.059(3) Uani 1 1 d . . . C14 C 0.2754(5) 0.2145(6) 0.138(2) 0.059(2) Uani 1 1 d . . . C15 C 0.3042(6) 0.1947(5) 0.040(2) 0.059(3) Uani 1 1 d . . . H15 H 0.2854 0.1571 0.0005 0.071 Uiso 1 1 calc R U . C16 C 0.3621(6) 0.2310(6) -0.003(2) 0.062(3) Uani 1 1 d . . . H16 H 0.3805 0.2179 -0.0768 0.074 Uiso 1 1 calc R U . C17 C 0.3915(5) 0.2852(7) 0.062(2) 0.066(3) Uani 1 1 d . . . C18 C 0.3623(6) 0.3042(7) 0.167(3) 0.079(5) Uani 1 1 d . . . H18 H 0.3815 0.3410 0.2128 0.095 Uiso 1 1 calc R U . C19 C 0.3055(7) 0.2692(8) 0.205(3) 0.080(5) Uani 1 1 d . . . H19 H 0.2870 0.2826 0.2768 0.096 Uiso 1 1 calc R U . C20 C 0.4550(6) 0.3252(9) 0.027(3) 0.076(4) Uani 1 1 d . . . H20A H 0.4745 0.3404 0.1356 0.114 Uiso 1 1 calc R U . H20B H 0.4598 0.3559 -0.0476 0.114 Uiso 1 1 calc R U . H20C H 0.4706 0.3044 -0.0299 0.114 Uiso 1 1 calc R U . C21 C -0.1549(6) -0.0956(6) -0.531(3) 0.072(4) Uani 1 1 d . . . H21A H -0.1379 -0.0972 -0.6397 0.108 Uiso 1 1 calc R U . H21B H -0.1780 -0.0783 -0.5504 0.108 Uiso 1 1 calc R U . H21C H -0.1782 -0.1335 -0.4862 0.108 Uiso 1 1 calc R U . O1 O 0.0706(3) 0.0441(4) -0.2041(12) 0.0553(17) Uani 1 1 d . . . O2 O 0.1591(3) 0.0615(5) -0.2413(13) 0.059(2) Uani 1 1 d . . . H2A H 0.1628 0.0717 -0.3457 0.089 Uiso 1 1 d R U . O3 O 0.1654(3) 0.0868(4) 0.4500(10) 0.0515(17) Uani 1 1 d . . . O4 O 0.0722(3) 0.0405(4) 0.3808(12) 0.0542(17) Uani 1 1 d . . . O5 O 0.1528(3) 0.0121(4) 0.0857(10) 0.0503(16) Uani 1 1 d . . . O6 O 0.0944(5) -0.0678(5) -0.0552(17) 0.064(2) Uani 1 1 d . . . O7 O 0.1930(4) 0.1249(4) 0.1166(12) 0.0574(19) Uani 1 1 d . . . O8 O 0.1853(5) 0.1971(5) 0.2419(17) 0.068(2) Uani 1 1 d . . . O9 O -0.1086(3) -0.0605(5) -0.4009(12) 0.060(2) Uani 1 1 d . . . H9A H -0.1295 -0.0607 -0.3072 0.090 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 Ho1 0.0340(2) 0.0340(2) 0.0195(2) 0.000 0.000 0.01699(11) C1 0.036(3) 0.078(6) 0.022(3) -0.010(3) -0.005(3) 0.021(3) C2 0.043(3) 0.053(4) 0.034(4) -0.005(3) -0.001(3) 0.021(3) C3 0.051(4) 0.055(4) 0.032(4) -0.005(3) -0.003(3) 0.027(4) C4 0.044(4) 0.066(5) 0.029(4) -0.004(4) 0.009(3) 0.017(4) C5 0.051(5) 0.074(8) 0.055(7) 0.028(6) 0.012(5) 0.017(5) C6 0.068(6) 0.052(4) 0.058(7) 0.007(5) 0.010(5) 0.032(4) C7 0.106(14) 0.063(7) 0.074(11) 0.000(7) 0.005(10) 0.039(8) C8 0.17(3) 0.069(9) 0.089(14) -0.002(9) -0.009(16) 0.079(14) C9 0.134(17) 0.096(13) 0.070(10) 0.013(9) 0.003(11) 0.086(13) C10 0.083(9) 0.076(8) 0.081(11) -0.001(8) -0.009(8) 0.051(7) C11 0.076(7) 0.063(6) 0.059(7) 0.001(5) -0.005(6) 0.045(5) C12 0.20(3) 0.18(3) 0.11(2) 0.03(2) 0.00(2) 0.15(3) C13 0.044(4) 0.068(6) 0.048(6) 0.009(5) 0.007(4) 0.015(4) C14 0.053(5) 0.063(5) 0.052(6) -0.002(5) 0.004(4) 0.022(4) C15 0.051(5) 0.054(5) 0.073(8) 0.002(5) 0.003(5) 0.026(4) C16 0.055(5) 0.068(6) 0.063(8) 0.004(6) 0.014(5) 0.031(5) C17 0.043(4) 0.073(7) 0.066(8) -0.002(6) 0.007(5) 0.016(4) C18 0.055(6) 0.070(7) 0.100(14) -0.025(8) -0.002(7) 0.021(5) C19 0.064(7) 0.075(8) 0.082(11) -0.023(8) 0.012(7) 0.020(6) C20 0.053(5) 0.092(10) 0.073(10) 0.011(8) 0.012(6) 0.028(6) C21 0.055(5) 0.054(5) 0.110(13) -0.001(6) 0.013(7) 0.029(4) O1 0.046(3) 0.081(5) 0.038(4) -0.004(3) 0.001(3) 0.031(3) O2 0.042(3) 0.089(6) 0.041(4) -0.003(4) 0.001(3) 0.029(3) O3 0.041(3) 0.076(4) 0.023(3) -0.002(3) 0.002(2) 0.017(3) O4 0.045(3) 0.077(5) 0.036(3) -0.004(3) -0.001(3) 0.027(3) O5 0.047(3) 0.082(5) 0.031(3) 0.002(3) 0.003(2) 0.038(3) O6 0.066(5) 0.064(5) 0.060(5) -0.014(4) -0.004(4) 0.030(4) O7 0.057(4) 0.064(4) 0.032(4) -0.007(3) -0.001(3) 0.016(4) O8 0.061(4) 0.072(5) 0.067(6) -0.010(5) 0.004(4) 0.030(4) O9 0.032(2) 0.089(6) 0.040(4) -0.004(4) 0.001(2) 0.017(3) 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 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.1550 4.8030 '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 Ho1 O4 79.6(3) 3_554 2_554 O4 Ho1 O4 79.6(3) 3_554 1_554 O4 Ho1 O4 79.6(3) 2_554 1_554 O4 Ho1 O1 140.1(4) 3_554 . O4 Ho1 O1 134.4(4) 2_554 . O4 Ho1 O1 86.6(3) 1_554 . O4 Ho1 O1 134.4(4) 3_554 2 O4 Ho1 O1 86.6(3) 2_554 2 O4 Ho1 O1 140.1(4) 1_554 2 O1 Ho1 O1 76.9(3) . 2 O4 Ho1 O1 86.6(3) 3_554 3 O4 Ho1 O1 140.1(4) 2_554 3 O4 Ho1 O1 134.4(4) 1_554 3 O1 Ho1 O1 76.9(3) . 3 O1 Ho1 O1 76.9(3) 2 3 O4 Ho1 O9 70.1(4) 3_554 2 O4 Ho1 O9 140.3(3) 2_554 2 O4 Ho1 O9 70.4(3) 1_554 2 O1 Ho1 O9 70.0(3) . 2 O1 Ho1 O9 133.0(3) 2 2 O1 Ho1 O9 64.0(4) 3 2 O4 Ho1 O9 70.4(3) 3_554 . O4 Ho1 O9 70.1(4) 2_554 . O4 Ho1 O9 140.3(3) 1_554 . O1 Ho1 O9 133.0(3) . . O1 Ho1 O9 64.0(4) 2 . O1 Ho1 O9 70.0(3) 3 . O9 Ho1 O9 119.78(4) 2 . O4 Ho1 O9 140.3(3) 3_554 3 O4 Ho1 O9 70.4(3) 2_554 3 O4 Ho1 O9 70.1(4) 1_554 3 O1 Ho1 O9 64.0(4) . 3 O1 Ho1 O9 70.0(3) 2 3 O1 Ho1 O9 133.0(3) 3 3 O9 Ho1 O9 119.79(4) 2 3 O9 Ho1 O9 119.78(3) . 3 O1 C1 O2 126.8(10) . . O1 C1 C2 115.9(8) . . O2 C1 C2 117.1(9) . . O5 C2 C1 115.0(8) . . O5 C2 C3 106.7(8) . . C1 C2 C3 109.5(9) . . O5 C2 H2 108.5 . . C1 C2 H2 108.5 . . C3 C2 H2 108.5 . . O7 C3 C4 114.6(9) . . O7 C3 C2 107.0(8) . . C4 C3 C2 107.5(9) . . O7 C3 H3 109.2 . . C4 C3 H3 109.2 . . C2 C3 H3 109.2 . . O4 C4 O3 128.8(10) . . O4 C4 C3 113.4(10) . . O3 C4 C3 117.8(8) . . O5 C5 O6 127.4(16) . . O5 C5 C6 112.1(12) . . O6 C5 C6 120.5(17) . . C11 C6 C7 121.8(16) . . C11 C6 C5 117.6(11) . . C7 C6 C5 120.4(16) . . C8 C7 C6 118(2) . . C8 C7 H7 120.8 . . C6 C7 H7 120.8 . . C7 C8 C9 121.9(18) . . C7 C8 H8 119.0 . . C9 C8 H8 119.0 . . C10 C9 C8 117.1(18) . . C10 C9 C12 123(3) . . C8 C9 C12 120(2) . . C9 C10 C11 121.7(18) . . C9 C10 H10 119.2 . . C11 C10 H10 119.2 . . C6 C11 C10 118.9(13) . . C6 C11 H11 120.5 . . C10 C11 H11 120.5 . . 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 124.4(11) . . O8 C13 C14 125.4(13) . . O7 C13 C14 110.1(12) . . C15 C14 C19 118.4(13) . . C15 C14 C13 122.7(13) . . C19 C14 C13 119.0(13) . . C14 C15 C16 120.5(12) . . C14 C15 H15 119.8 . . C16 C15 H15 119.8 . . C17 C16 C15 120.7(13) . . C17 C16 H16 119.6 . . C15 C16 H16 119.6 . . C16 C17 C18 118.2(12) . . C16 C17 C20 122.8(15) . . C18 C17 C20 119.0(15) . . C19 C18 C17 120.8(14) . . C19 C18 H18 119.6 . . C17 C18 H18 119.6 . . C18 C19 C14 121.2(15) . . C18 C19 H19 119.4 . . C14 C19 H19 119.4 . . 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 Ho1 143.8(8) . . C1 O2 H2A 123.1 . . C4 O4 Ho1 149.2(8) . 1_556 C5 O5 C2 116.3(10) . . C13 O7 C3 113.5(10) . . C21 O9 Ho1 134.5(8) . . C21 O9 H9A 101.3 . . Ho1 O9 H9A 123.7 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ho1 O4 2.297(8) 3_554 Ho1 O4 2.297(8) 2_554 Ho1 O4 2.297(8) 1_554 Ho1 O1 2.329(9) . Ho1 O1 2.329(9) 2 Ho1 O1 2.329(9) 3 Ho1 O9 2.554(7) 2 Ho1 O9 2.554(7) . Ho1 O9 2.554(7) 3 C1 O1 1.201(12) . C1 O2 1.278(11) . C1 C2 1.541(14) . C2 O5 1.452(12) . C2 C3 1.544(14) . C2 H2 0.9800 . C3 O7 1.386(13) . C3 C4 1.540(15) . C3 H3 0.9800 . C4 O4 1.234(12) . C4 O3 1.259(13) . C5 O5 1.23(2) . C5 O6 1.247(19) . C5 C6 1.55(2) . C6 C11 1.36(2) . C6 C7 1.40(2) . C7 C8 1.37(4) . C7 H7 0.9300 . C8 C9 1.42(4) . C8 H8 0.9300 . C9 C10 1.38(3) . C9 C12 1.49(3) . C10 C11 1.403(19) . C10 H10 0.9300 . C11 H11 0.9300 . C12 H12A 0.9600 . C12 H12B 0.9600 . C12 H12C 0.9600 . C13 O8 1.194(18) . C13 O7 1.378(18) . C13 C14 1.475(16) . C14 C15 1.37(2) . C14 C19 1.38(2) . C15 C16 1.411(18) . C15 H15 0.9300 . C16 C17 1.37(2) . C16 H16 0.9300 . C17 C18 1.39(2) . C17 C20 1.529(18) . C18 C19 1.37(2) . C18 H18 0.9300 . C19 H19 0.9300 . C20 H20A 0.9600 . C20 H20B 0.9600 . C20 H20C 0.9600 . C21 O9 1.51(2) . C21 H21A 0.9600 . C21 H21B 0.9600 . C21 H21C 0.9600 . O2 H2A 0.8327 . O4 Ho1 2.297(8) 1_556 O9 H9A 0.9097 . 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 C21 H21B O8 0.96 2.64 3.47(2) 145.3 2_554 O2 H2A O3 0.83 1.61 2.436(12) 175.6 1_554 O9 H9A O6 0.91 2.12 2.929(15) 147.1 3 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 149.3(11) . O2 C1 C2 O5 -26.3(15) . O1 C1 C2 C3 -90.6(12) . O2 C1 C2 C3 93.8(12) . O5 C2 C3 O7 56.3(10) . C1 C2 C3 O7 -68.8(10) . O5 C2 C3 C4 -67.3(10) . C1 C2 C3 C4 167.7(8) . O7 C3 C4 O4 177.2(11) . C2 C3 C4 O4 -64.1(13) . O7 C3 C4 O3 -3.0(16) . C2 C3 C4 O3 115.7(11) . O5 C5 C6 C11 -8.4(18) . O6 C5 C6 C11 173.1(14) . O5 C5 C6 C7 167.5(15) . O6 C5 C6 C7 -11(2) . C11 C6 C7 C8 0(3) . C5 C6 C7 C8 -176(2) . C6 C7 C8 C9 -2(4) . C7 C8 C9 C10 2(4) . C7 C8 C9 C12 180(3) . C8 C9 C10 C11 0(3) . C12 C9 C10 C11 -178(2) . C7 C6 C11 C10 1(3) . C5 C6 C11 C10 177.0(15) . C9 C10 C11 C6 -1(3) . O8 C13 C14 C15 -171.3(16) . O7 C13 C14 C15 9(2) . O8 C13 C14 C19 8(3) . O7 C13 C14 C19 -172.2(16) . C19 C14 C15 C16 -5(3) . C13 C14 C15 C16 174.3(15) . C14 C15 C16 C17 4(3) . C15 C16 C17 C18 -2(3) . C15 C16 C17 C20 176.9(17) . C16 C17 C18 C19 0(3) . C20 C17 C18 C19 -179(2) . C17 C18 C19 C14 -1(4) . C15 C14 C19 C18 3(3) . C13 C14 C19 C18 -176(2) . O2 C1 O1 Ho1 50(2) . C2 C1 O1 Ho1 -124.6(11) . O3 C4 O4 Ho1 15(3) 1_556 C3 C4 O4 Ho1 -165.2(12) 1_556 O6 C5 O5 C2 1.7(19) . C6 C5 O5 C2 -176.8(9) . C1 C2 O5 C5 -70.5(12) . C3 C2 O5 C5 167.9(10) . O8 C13 O7 C3 -3.6(19) . C14 C13 O7 C3 176.1(11) . C4 C3 O7 C13 -75.5(13) . C2 C3 O7 C13 165.5(10) .