#------------------------------------------------------------------------------ #$Date: 2021-03-07 03:40:06 +0200 (Sun, 07 Mar 2021) $ #$Revision: 262821 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/80/7128006.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_7128006 loop_ _publ_author_name 'Jia, Kexin' 'Meng, Xixi' 'Wang, Mengmeng' 'Gou, Xiaoshuang' 'Wang, Yu-Xia' 'Xu, Na' 'Shi, Wei' 'Cheng, Peng' _publ_section_title ; Enhancing the energy barrier and hysteresis temperature in two benchtop-stable Ho(III) single-ion magnets ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D1CC00582K _journal_year 2021 _chemical_formula_moiety 'C24 H60 Cl3 Ho N6 O8 P2' _chemical_formula_sum 'C24 H60 Cl3 Ho N6 O8 P2' _chemical_formula_weight 894.00 _chemical_name_systematic 'Ho(tppo)2(H2O)5Cl3 H2O' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2020-10-29 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2021-01-29 deposited with the CCDC. 2021-03-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 9.9663(3) _cell_length_b 26.9370(9) _cell_length_c 30.2924(9) _cell_measurement_reflns_used 9137 _cell_measurement_temperature 293 _cell_measurement_theta_max 24.9670 _cell_measurement_theta_min 2.2730 _cell_volume 8132.4(4) _computing_cell_refinement 'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)' _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 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 32.00 109.00 0.50 12.00 -- 20.00 54.00-180.00 154 2 \w -55.00 -29.00 0.50 12.00 -- 20.00 54.00 30.00 52 3 \w -27.00 0.00 0.50 12.00 -- 20.00 54.00 30.00 54 4 \w 69.00 100.00 0.50 12.00 -- 20.00 54.00 30.00 62 5 \w -72.00 106.00 0.50 12.00 -- 20.00 54.00 0.00 356 6 \w -67.00 -42.00 0.50 12.00 -- 20.00 54.00 90.00 50 7 \w 12.00 55.00 0.50 12.00 -- 20.00 54.00 90.00 86 8 \w 1.00 26.00 0.50 12.00 -- 20.00 54.00-180.00 50 ; _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Mini II' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0095712000 _diffrn_orient_matrix_UB_12 -0.0258824000 _diffrn_orient_matrix_UB_13 0.0030054000 _diffrn_orient_matrix_UB_21 -0.0222672000 _diffrn_orient_matrix_UB_22 0.0043354000 _diffrn_orient_matrix_UB_23 0.0219047000 _diffrn_orient_matrix_UB_31 -0.0668983000 _diffrn_orient_matrix_UB_32 0.0022385000 _diffrn_orient_matrix_UB_33 -0.0077072000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_unetI/netI 0.0456 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 43248 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 1.655 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 2.267 _exptl_absorpt_correction_T_max 0.69235 _exptl_absorpt_correction_T_min 0.62499 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear pinkish pink' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier pinkish _exptl_crystal_colour_primary pink _exptl_crystal_density_diffrn 1.460 _exptl_crystal_description hexagonal _exptl_crystal_F_000 3664 _exptl_crystal_preparation NONE _exptl_crystal_recrystallization_method NONE _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 2.627 _refine_diff_density_min -1.467 _refine_diff_density_rms 0.120 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 428 _refine_ls_number_reflns 7173 _refine_ls_number_restraints 171 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0546 _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^)+(0.0601P)^2^+39.5145P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1327 _refine_ls_wR_factor_ref 0.1461 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4953 _reflns_number_total 7173 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1cc00582k2.cif _cod_data_source_block 1 _cod_database_code 7128006 _shelx_shelxl_version_number 2017/1 _chemical_oxdiff_usercomment '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. ; _reflns_odcompleteness_completeness 86.62 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All O(H) groups, All O(H,H) groups 2. Restrained distances O5-H5b \\sim O1-H1a with sigma of 0.02 3. Rigid bond restraints All non-hydrogen atoms with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002 4. Uiso/Uaniso restraints and constraints C0AA \\sim C18 \\sim C20: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C10) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 5.a Free rotating group: O8(H8c,H8d) 5.b Rotating group: O1(H1a), O2(H2a), O3(H3a), O5(H5a) 5.c Secondary CH2 refined with riding coordinates: C1(H1c,H1d), C2(H2c,H2d), C3(H3c,H3d), C4(H4c,H4d), C5(H5c,H5d), C6(H6a,H6b), C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C11(H11a,H11b), C12(H12a,H12b), C13(H13a,H13b), C14(H14a,H14b), C15(H15a,H15b), C16(H16a,H16b), C17(H17a,H17b), C18(H18a,H18b), C20(H20a,H20b), C21(H21a,H21b), C22(H22a, H22b), C23(H23a,H23b), C24(H24a,H24b), C0AA(H0Aa,H0Ab) ; _shelx_res_file ; TITL c20201013c_a.res in Pbca c20201013c.res created by SHELXL-2017/1 at 12:12:38 on 29-Oct-2020 REM Old TITL C20201013C in Pbca REM SHELXT solution in Pbca REM R1 0.154, Rweak 0.004, Alpha 0.054, Orientation as input REM Formula found by SHELXT: C20 N12 O11 I CELL 0.71073 9.9663 26.937 30.2924 90 90 90 ZERR 8 0.0003 0.0009 0.0009 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Cl Ho N O P UNIT 192 480 24 8 48 64 16 SADI O5 H5b O1 H1a DELU 0.001 0.002 SIMU 0.01 0.02 3.8 C0AA C18 C20 ISOR 0.01 0.02 C3 C5 ISOR 0.01 0.02 C10 C16 C18 L.S. 10 PLAN 50 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.060100 39.514500 FVAR 0.09390 HO1 4 0.393522 0.744923 0.625786 11.00000 0.03627 0.03342 = 0.02710 0.00109 0.00010 -0.00054 P1 7 0.252804 0.871524 0.628989 11.00000 0.04369 0.03743 = 0.04963 -0.00093 -0.00175 0.00446 P2 7 0.534723 0.618446 0.625764 11.00000 0.04390 0.03825 = 0.05490 0.00330 0.00331 0.00476 O1 6 0.392665 0.745949 0.547687 11.00000 0.05444 0.08000 = 0.02673 0.00069 0.00118 -0.01199 AFIX 7 H1A 2 0.320533 0.731413 0.537167 11.00000 -1.50000 AFIX 0 O2 6 0.593749 0.781548 0.601577 11.00000 0.04532 0.06720 = 0.04000 0.00347 0.00373 -0.01637 AFIX 7 H2A 2 0.589979 0.786617 0.573736 11.00000 -1.50000 AFIX 0 O3 6 0.514956 0.768623 0.688582 11.00000 0.05331 0.06451 = 0.03267 -0.00134 -0.00663 -0.01577 AFIX 7 H3A 2 0.575305 0.790375 0.681781 11.00000 -1.50000 AFIX 0 O4 6 0.272636 0.719044 0.688524 11.00000 0.05278 0.06529 = 0.03042 0.00480 0.00405 -0.01489 O5 6 0.190154 0.709848 0.601368 11.00000 0.04784 0.06865 = 0.03675 0.00521 -0.00790 -0.01850 AFIX 7 H5A 2 0.146404 0.697627 0.623518 11.00000 -1.50000 AFIX 0 O6 6 0.296458 0.818449 0.627453 11.00000 0.06244 0.03954 = 0.05676 0.00268 0.00268 0.01052 O7 6 0.493536 0.671512 0.626578 11.00000 0.06162 0.03889 = 0.06083 0.00007 0.00069 0.00913 N1 5 0.135928 0.877902 0.592965 11.00000 0.06045 0.05491 = 0.09194 0.00129 -0.03058 0.00265 N2 5 0.365968 0.912954 0.616401 11.00000 0.05134 0.04795 = 0.04297 0.00687 -0.00494 -0.00199 N3 5 0.210884 0.884709 0.679879 11.00000 0.07815 0.04455 = 0.06042 -0.00367 0.02137 -0.00239 N4 5 0.420192 0.578220 0.611980 11.00000 0.06090 0.04705 = 0.05639 -0.00366 0.00258 -0.00486 N5 5 0.652019 0.613270 0.589363 11.00000 0.06653 0.06099 = 0.09845 0.00084 0.03555 0.00727 N6 5 0.575881 0.601701 0.675684 11.00000 0.07909 0.05362 = 0.06749 0.01113 -0.01789 0.00258 C1 1 0.481053 0.922103 0.646382 11.00000 0.06154 0.08399 = 0.08413 0.01410 -0.02498 -0.02125 AFIX 23 H1C 2 0.458084 0.946825 0.668405 11.00000 -1.20000 H1D 2 0.507167 0.891741 0.661302 11.00000 -1.20000 AFIX 0 C2 1 0.591035 0.940205 0.617645 11.00000 0.05326 0.15395 = 0.15518 0.04228 -0.00621 -0.02250 AFIX 23 H2C 2 0.603873 0.975594 0.621792 11.00000 -1.20000 H2D 2 0.674204 0.923388 0.624925 11.00000 -1.20000 AFIX 0 C3 1 0.554781 0.930171 0.573516 11.00000 0.09974 0.15348 = 0.13334 0.00301 0.05741 -0.02476 AFIX 23 H3C 2 0.608869 0.902995 0.562348 11.00000 -1.20000 H3D 2 0.572614 0.959177 0.555471 11.00000 -1.20000 AFIX 0 C4 1 0.414075 0.917236 0.570249 11.00000 0.10361 0.07868 = 0.05416 0.00596 0.01983 -0.01254 AFIX 23 H4C 2 0.402945 0.886005 0.554734 11.00000 -1.20000 H4D 2 0.364815 0.942826 0.554600 11.00000 -1.20000 AFIX 0 C5 1 0.057609 0.924284 0.587402 11.00000 0.11347 0.08190 = 0.15541 -0.00754 -0.07270 0.03763 AFIX 23 H5C 2 0.023816 0.935544 0.615713 11.00000 -1.20000 H5D 2 0.113818 0.950177 0.575024 11.00000 -1.20000 AFIX 0 C6 1 -0.049173 0.913739 0.558837 11.00000 0.08430 0.14462 = 0.12344 -0.00720 -0.04686 0.04404 AFIX 23 H6A 2 -0.039059 0.932577 0.531750 11.00000 -1.20000 H6B 2 -0.133217 0.923339 0.572545 11.00000 -1.20000 AFIX 0 C7 1 -0.051203 0.861189 0.548921 11.00000 0.09795 0.13352 = 0.14042 0.02213 -0.07084 -0.02659 AFIX 23 H7A 2 -0.040874 0.855969 0.517420 11.00000 -1.20000 H7B 2 -0.135886 0.846760 0.558113 11.00000 -1.20000 AFIX 0 C8 1 0.060516 0.837801 0.572971 11.00000 0.06676 0.08237 = 0.07839 -0.00578 -0.02053 -0.01597 AFIX 23 H8A 2 0.026617 0.815451 0.595464 11.00000 -1.20000 H8B 2 0.116879 0.819075 0.552866 11.00000 -1.20000 AFIX 0 C9 1 0.186206 0.935150 0.696162 11.00000 0.18795 0.05239 = 0.10735 -0.01647 0.08756 -0.00277 AFIX 23 H9A 2 0.269257 0.950717 0.705498 11.00000 -1.20000 H9B 2 0.145035 0.955475 0.673464 11.00000 -1.20000 AFIX 0 C10 1 0.095120 0.928566 0.733622 11.00000 0.15705 0.08154 = 0.12168 -0.01251 0.08555 0.00918 AFIX 23 H10A 2 0.138590 0.940117 0.760367 11.00000 -1.20000 H10B 2 0.015190 0.948458 0.729047 11.00000 -1.20000 AFIX 0 C11 1 0.058538 0.878753 0.738734 11.00000 0.08823 0.09733 = 0.06601 -0.01320 0.02866 -0.01678 AFIX 23 H11A 2 -0.035845 0.874446 0.731919 11.00000 -1.20000 H11B 2 0.073618 0.868249 0.768958 11.00000 -1.20000 AFIX 0 C12 1 0.142566 0.848421 0.707841 11.00000 0.07119 0.06050 = 0.05792 0.00587 0.01043 -0.00681 AFIX 23 H12A 2 0.207004 0.828544 0.724073 11.00000 -1.20000 H12B 2 0.086785 0.826546 0.690229 11.00000 -1.20000 AFIX 0 C13 1 0.726899 0.654695 0.570437 11.00000 0.07994 0.09320 = 0.08371 0.00402 0.03241 -0.01727 AFIX 23 H13A 2 0.761067 0.676220 0.593515 11.00000 -1.20000 H13B 2 0.670265 0.674070 0.550908 11.00000 -1.20000 AFIX 0 C14 1 0.837834 0.631782 0.545760 11.00000 0.09779 0.16858 = 0.14613 -0.03520 0.07451 -0.03222 AFIX 23 H14A 2 0.830530 0.639941 0.514664 11.00000 -1.20000 H14B 2 0.923075 0.644210 0.556564 11.00000 -1.20000 AFIX 0 C15 1 0.830848 0.578665 0.551710 11.00000 0.11670 0.17266 = 0.13462 0.02331 0.06085 0.07868 AFIX 23 H15A 2 0.812920 0.562643 0.523646 11.00000 -1.20000 H15B 2 0.915776 0.566348 0.562875 11.00000 -1.20000 AFIX 0 C16 1 0.727811 0.567732 0.581769 11.00000 0.12398 0.09205 = 0.16477 -0.00151 0.07049 0.04467 AFIX 23 H16A 2 0.765467 0.555745 0.609305 11.00000 -1.20000 H16B 2 0.669530 0.542215 0.569818 11.00000 -1.20000 AFIX 0 C17 1 0.642699 0.636479 0.706221 11.00000 0.08787 0.07055 = 0.05589 0.00206 -0.01075 0.00225 AFIX 23 H17A 2 0.576836 0.655698 0.722461 11.00000 -1.20000 H17B 2 0.700422 0.659116 0.690112 11.00000 -1.20000 AFIX 0 C18 1 0.724236 0.604615 0.737276 11.00000 0.14095 0.09571 = 0.10321 0.01665 -0.06184 -0.00147 AFIX 23 H18A 2 0.819488 0.608944 0.731942 11.00000 -1.20000 H18B 2 0.705105 0.613034 0.767767 11.00000 -1.20000 AFIX 0 C20 1 0.600189 0.550608 0.690327 11.00000 0.16975 0.06206 = 0.11970 0.02666 -0.07794 0.00168 AFIX 23 H20A 2 0.516651 0.534325 0.698095 11.00000 -1.20000 H20B 2 0.644405 0.531520 0.667400 11.00000 -1.20000 AFIX 0 C21 1 0.299962 0.572225 0.640620 11.00000 0.05699 0.06010 = 0.09527 0.00028 0.01227 -0.01265 AFIX 23 H21A 2 0.317801 0.548702 0.664143 11.00000 -1.20000 H21B 2 0.274632 0.603761 0.653640 11.00000 -1.20000 AFIX 0 C22 1 0.192344 0.553623 0.611386 11.00000 0.06235 0.10741 = 0.15221 -0.02678 -0.00878 -0.01244 AFIX 23 H22A 2 0.186320 0.517731 0.613066 11.00000 -1.20000 H22B 2 0.106437 0.567686 0.619761 11.00000 -1.20000 AFIX 0 C23 1 0.228791 0.569060 0.567381 11.00000 0.11856 0.11953 = 0.14346 0.01813 -0.07063 -0.02787 AFIX 23 H23A 2 0.186774 0.600610 0.560512 11.00000 -1.20000 H23B 2 0.198366 0.544688 0.546039 11.00000 -1.20000 AFIX 0 C24 1 0.377079 0.573976 0.565218 11.00000 0.12447 0.10049 = 0.06500 -0.00583 -0.01846 -0.03580 AFIX 23 H24A 2 0.416988 0.545053 0.551381 11.00000 -1.20000 H24B 2 0.402511 0.603315 0.548644 11.00000 -1.20000 AFIX 0 CL1 3 0.637748 0.791912 0.500115 11.00000 0.05257 0.12689 = 0.03790 0.00442 0.01414 -0.00256 CL2 3 0.777718 0.824968 0.670442 11.00000 0.05449 0.10758 = 0.06084 0.00661 -0.01029 -0.02653 CL3 3 0.010987 0.662368 0.670440 11.00000 0.05932 0.10074 = 0.05784 -0.00650 0.01291 -0.02275 AFIX 6 O8 6 0.395710 0.743820 0.766207 11.00000 0.07590 0.08977 = 0.03073 0.00217 0.00303 -0.00573 H8C 2 0.369667 0.763494 0.786404 11.00000 -1.50000 H8D 2 0.413527 0.716932 0.779681 11.00000 -1.50000 AFIX 0 C0AA 1 0.684673 0.555678 0.728022 11.00000 0.17912 0.08664 = 0.13166 0.03016 -0.09031 0.00305 AFIX 23 H0AA 2 0.637873 0.542507 0.753538 11.00000 -1.20000 H0AB 2 0.764448 0.535669 0.723558 11.00000 -1.20000 AFIX 0 H1B 2 0.453798 0.755324 0.528339 11.00000 0.04208 H4A 2 0.194341 0.702475 0.690080 11.00000 0.10251 H2B 2 0.683025 0.788633 0.612103 11.00000 0.13998 H3B 2 0.509699 0.761140 0.715003 11.00000 0.10193 H4B 2 0.288348 0.732018 0.709981 11.00000 0.08318 H5B 2 0.157056 0.711815 0.574836 11.00000 0.16056 HKLF 4 REM c20201013c_a.res in Pbca REM R1 = 0.0546 for 4953 Fo > 4sig(Fo) and 0.0833 for all 7173 data REM 428 parameters refined using 171 restraints END WGHT 0.0601 39.5227 REM Highest difference peak 2.627, deepest hole -1.467, 1-sigma level 0.120 Q1 1 0.3925 0.7838 0.6259 11.00000 0.05 2.63 Q2 1 0.3925 0.7067 0.6254 11.00000 0.05 2.06 Q3 1 0.6123 0.7503 0.7268 11.00000 0.05 1.27 Q4 1 -0.0319 0.7519 0.6253 11.00000 0.05 1.26 Q5 1 0.6150 0.7508 0.5238 11.00000 0.05 1.24 Q6 1 0.7649 0.7403 0.6107 11.00000 0.05 0.71 Q7 1 0.3219 0.7514 0.6185 11.00000 0.05 0.69 Q8 1 0.3868 0.8307 0.6246 11.00000 0.05 0.68 Q9 1 0.3383 0.7468 0.8539 11.00000 0.05 0.66 Q10 1 0.3921 0.6427 0.6236 11.00000 0.05 0.66 Q11 1 0.2634 0.8321 0.6269 11.00000 0.05 0.64 Q12 1 0.4803 0.7532 0.6228 11.00000 0.05 0.63 Q13 1 0.1094 0.9239 0.5609 11.00000 0.05 0.63 Q14 1 0.3613 0.8837 0.6238 11.00000 0.05 0.55 Q15 1 0.7918 0.7899 0.6657 11.00000 0.05 0.54 Q16 1 0.7682 0.5603 0.7086 11.00000 0.05 0.49 Q17 1 0.5851 0.7537 0.6041 11.00000 0.05 0.45 Q18 1 0.0190 0.9221 0.7151 11.00000 0.05 0.45 Q19 1 0.6855 0.5689 0.5536 11.00000 0.05 0.44 Q20 1 0.0095 0.6961 0.6667 11.00000 0.05 0.43 Q21 1 0.5111 0.7141 0.6274 11.00000 0.05 0.43 Q22 1 0.2529 0.6171 0.6281 11.00000 0.05 0.43 Q23 1 0.2923 0.7530 0.6800 11.00000 0.05 0.43 Q24 1 0.5263 0.8703 0.6279 11.00000 0.05 0.42 Q25 1 0.6949 0.5608 0.6726 11.00000 0.05 0.42 Q26 1 0.6833 0.7355 0.5974 11.00000 0.05 0.41 Q27 1 0.2218 0.7520 0.6024 11.00000 0.05 0.40 Q28 1 0.5528 0.7407 0.6215 11.00000 0.05 0.39 Q29 1 0.6249 0.8795 0.6055 11.00000 0.05 0.39 Q30 1 0.7435 0.7473 0.5765 11.00000 0.05 0.37 Q31 1 0.4060 0.6097 0.6223 11.00000 0.05 0.37 Q32 1 0.6167 0.6034 0.6634 11.00000 0.05 0.37 Q33 1 0.6341 0.7531 0.6819 11.00000 0.05 0.37 Q34 1 0.3434 0.9388 0.6225 11.00000 0.05 0.36 Q35 1 -0.0336 0.9303 0.6954 11.00000 0.05 0.36 Q36 1 -0.0566 0.7619 0.5875 11.00000 0.05 0.36 Q37 1 0.7574 0.8730 0.6752 11.00000 0.05 0.36 Q38 1 0.1631 0.9305 0.7472 11.00000 0.05 0.35 Q39 1 -0.0437 0.8435 0.6233 11.00000 0.05 0.35 Q40 1 0.0029 0.8290 0.6718 11.00000 0.05 0.35 Q41 1 0.6622 0.7569 0.6038 11.00000 0.05 0.35 Q42 1 0.6321 0.6146 0.5686 11.00000 0.05 0.34 Q43 1 0.0577 0.9303 0.6781 11.00000 0.05 0.34 Q44 1 0.1435 0.7794 0.5019 11.00000 0.05 0.34 Q45 1 0.1732 0.7279 0.6390 11.00000 0.05 0.33 Q46 1 0.5574 0.5303 0.6699 11.00000 0.05 0.33 Q47 1 0.6689 0.7618 0.6473 11.00000 0.05 0.33 Q48 1 0.3100 0.6824 0.6825 11.00000 0.05 0.32 Q49 1 0.6044 0.8803 0.6409 11.00000 0.05 0.32 Q50 1 0.1237 0.8798 0.6656 11.00000 0.05 0.32 ; _shelx_res_checksum 37579 _olex2_exptl_crystal_mounting_method 293 _olex2_submission_original_sample_id Ho-Cl _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.524 _oxdiff_exptl_absorpt_empirical_full_min 0.786 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, 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 Ho1 Ho 0.39352(3) 0.74492(2) 0.62579(2) 0.03226(13) Uani 1 1 d . U . . . P1 P 0.2528(2) 0.87152(7) 0.62899(7) 0.0436(4) Uani 1 1 d . U . . . P2 P 0.5347(2) 0.61845(7) 0.62576(7) 0.0457(5) Uani 1 1 d . U . . . O1 O 0.3927(7) 0.7459(2) 0.54769(17) 0.0537(12) Uani 1 1 d D U . . . H1A H 0.320533 0.731413 0.537167 0.081 Uiso 1 1 d DGR . . . . O2 O 0.5937(6) 0.7815(2) 0.60158(17) 0.0508(11) Uani 1 1 d . U . . . H2A H 0.589979 0.786617 0.573736 0.076 Uiso 1 1 d GR . . . . O3 O 0.5150(6) 0.7686(2) 0.68858(18) 0.0502(12) Uani 1 1 d . U . . . H3A H 0.575305 0.790375 0.681781 0.075 Uiso 1 1 d GR . . . . O4 O 0.2726(7) 0.7190(2) 0.68852(19) 0.0495(12) Uani 1 1 d . U . . . O5 O 0.1902(6) 0.7098(2) 0.60137(18) 0.0511(11) Uani 1 1 d D U . . . H5A H 0.146404 0.697627 0.623518 0.077 Uiso 1 1 d GR . . . . O6 O 0.2965(6) 0.81845(18) 0.62745(16) 0.0529(11) Uani 1 1 d . U . . . O7 O 0.4935(6) 0.67151(18) 0.62658(17) 0.0538(11) Uani 1 1 d . U . . . N1 N 0.1359(7) 0.8779(3) 0.5930(3) 0.0691(18) Uani 1 1 d . U . . . N2 N 0.3660(7) 0.9130(2) 0.6164(2) 0.0474(13) Uani 1 1 d . U . . . N3 N 0.2109(8) 0.8847(2) 0.6799(2) 0.0610(17) Uani 1 1 d . U . . . N4 N 0.4202(7) 0.5782(2) 0.6120(2) 0.0548(14) Uani 1 1 d . U . . . N5 N 0.6520(8) 0.6133(3) 0.5894(3) 0.075(2) Uani 1 1 d . U . . . N6 N 0.5759(8) 0.6017(3) 0.6757(2) 0.0667(18) Uani 1 1 d . U . . . C1 C 0.4811(10) 0.9221(4) 0.6464(3) 0.077(3) Uani 1 1 d . U . . . H1C H 0.458084 0.946825 0.668405 0.092 Uiso 1 1 calc R . . . . H1D H 0.507167 0.891741 0.661302 0.092 Uiso 1 1 calc R . . . . C2 C 0.5910(12) 0.9402(6) 0.6176(4) 0.121(5) Uani 1 1 d . U . . . H2C H 0.603873 0.975594 0.621792 0.145 Uiso 1 1 calc R . . . . H2D H 0.674204 0.923388 0.624925 0.145 Uiso 1 1 calc R . . . . C3 C 0.5548(14) 0.9302(6) 0.5735(5) 0.129(4) Uani 1 1 d . U . . . H3C H 0.608869 0.902995 0.562348 0.155 Uiso 1 1 calc R . . . . H3D H 0.572614 0.959177 0.555471 0.155 Uiso 1 1 calc R . . . . C4 C 0.4141(11) 0.9172(4) 0.5702(3) 0.079(3) Uani 1 1 d . U . . . H4C H 0.402945 0.886005 0.554734 0.095 Uiso 1 1 calc R . . . . H4D H 0.364815 0.942826 0.554600 0.095 Uiso 1 1 calc R . . . . C5 C 0.0576(13) 0.9243(4) 0.5874(5) 0.117(4) Uani 1 1 d . U . . . H5C H 0.023816 0.935544 0.615713 0.140 Uiso 1 1 calc R . . . . H5D H 0.113818 0.950177 0.575024 0.140 Uiso 1 1 calc R . . . . C6 C -0.0492(13) 0.9137(5) 0.5588(4) 0.117(4) Uani 1 1 d . U . . . H6A H -0.039059 0.932577 0.531750 0.141 Uiso 1 1 calc R . . . . H6B H -0.133217 0.923339 0.572545 0.141 Uiso 1 1 calc R . . . . C7 C -0.0512(13) 0.8612(5) 0.5489(5) 0.124(5) Uani 1 1 d . U . . . H7A H -0.040874 0.855969 0.517420 0.149 Uiso 1 1 calc R . . . . H7B H -0.135886 0.846760 0.558113 0.149 Uiso 1 1 calc R . . . . C8 C 0.0605(10) 0.8378(4) 0.5730(3) 0.076(3) Uani 1 1 d . U . . . H8A H 0.026617 0.815451 0.595464 0.091 Uiso 1 1 calc R . . . . H8B H 0.116879 0.819075 0.552866 0.091 Uiso 1 1 calc R . . . . C9 C 0.1862(15) 0.9352(4) 0.6962(4) 0.116(5) Uani 1 1 d . U . . . H9A H 0.269257 0.950717 0.705498 0.139 Uiso 1 1 calc R . . . . H9B H 0.145035 0.955475 0.673464 0.139 Uiso 1 1 calc R . . . . C10 C 0.0951(14) 0.9286(4) 0.7336(4) 0.120(4) Uani 1 1 d . U . . . H10A H 0.138590 0.940117 0.760367 0.144 Uiso 1 1 calc R . . . . H10B H 0.015190 0.948458 0.729047 0.144 Uiso 1 1 calc R . . . . C11 C 0.0585(11) 0.8788(4) 0.7387(3) 0.084(3) Uani 1 1 d . U . . . H11A H -0.035845 0.874446 0.731919 0.101 Uiso 1 1 calc R . . . . H11B H 0.073618 0.868249 0.768958 0.101 Uiso 1 1 calc R . . . . C12 C 0.1426(10) 0.8484(3) 0.7078(3) 0.063(2) Uani 1 1 d . U . . . H12A H 0.207004 0.828544 0.724073 0.076 Uiso 1 1 calc R . . . . H12B H 0.086785 0.826546 0.690229 0.076 Uiso 1 1 calc R . . . . C13 C 0.7269(11) 0.6547(4) 0.5704(4) 0.086(3) Uani 1 1 d . U . . . H13A H 0.761067 0.676220 0.593515 0.103 Uiso 1 1 calc R . . . . H13B H 0.670265 0.674070 0.550908 0.103 Uiso 1 1 calc R . . . . C14 C 0.8378(14) 0.6318(6) 0.5458(5) 0.137(5) Uani 1 1 d . U . . . H14A H 0.830530 0.639941 0.514664 0.165 Uiso 1 1 calc R . . . . H14B H 0.923075 0.644210 0.556564 0.165 Uiso 1 1 calc R . . . . C15 C 0.8308(15) 0.5787(6) 0.5517(5) 0.141(6) Uani 1 1 d . U . . . H15A H 0.812920 0.562643 0.523646 0.170 Uiso 1 1 calc R . . . . H15B H 0.915776 0.566348 0.562875 0.170 Uiso 1 1 calc R . . . . C16 C 0.7278(14) 0.5677(4) 0.5818(5) 0.127(4) Uani 1 1 d . U . . . H16A H 0.765467 0.555745 0.609305 0.152 Uiso 1 1 calc R . . . . H16B H 0.669530 0.542215 0.569818 0.152 Uiso 1 1 calc R . . . . C17 C 0.6427(11) 0.6365(3) 0.7062(3) 0.071(2) Uani 1 1 d . U . . . H17A H 0.576836 0.655698 0.722461 0.086 Uiso 1 1 calc R . . . . H17B H 0.700422 0.659116 0.690112 0.086 Uiso 1 1 calc R . . . . C18 C 0.7242(14) 0.6046(4) 0.7373(4) 0.113(3) Uani 1 1 d . U . . . H18A H 0.819488 0.608944 0.731942 0.136 Uiso 1 1 calc R . . . . H18B H 0.705105 0.613034 0.767767 0.136 Uiso 1 1 calc R . . . . C20 C 0.6002(15) 0.5506(4) 0.6903(4) 0.117(3) Uani 1 1 d . U . . . H20A H 0.516651 0.534325 0.698095 0.141 Uiso 1 1 calc R . . . . H20B H 0.644405 0.531520 0.667400 0.141 Uiso 1 1 calc R . . . . C21 C 0.3000(9) 0.5722(4) 0.6406(4) 0.071(2) Uani 1 1 d . U . . . H21A H 0.317801 0.548702 0.664143 0.085 Uiso 1 1 calc R . . . . H21B H 0.274632 0.603761 0.653640 0.085 Uiso 1 1 calc R . . . . C22 C 0.1923(12) 0.5536(5) 0.6114(5) 0.107(4) Uani 1 1 d . U . . . H22A H 0.186320 0.517731 0.613066 0.129 Uiso 1 1 calc R . . . . H22B H 0.106437 0.567686 0.619761 0.129 Uiso 1 1 calc R . . . . C23 C 0.2288(14) 0.5691(5) 0.5674(5) 0.127(5) Uani 1 1 d . U . . . H23A H 0.186774 0.600610 0.560512 0.153 Uiso 1 1 calc R . . . . H23B H 0.198366 0.544688 0.546039 0.153 Uiso 1 1 calc R . . . . C24 C 0.3771(12) 0.5740(4) 0.5652(3) 0.097(3) Uani 1 1 d . U . . . H24A H 0.416988 0.545053 0.551381 0.116 Uiso 1 1 calc R . . . . H24B H 0.402511 0.603315 0.548644 0.116 Uiso 1 1 calc R . . . . Cl1 Cl 0.6377(2) 0.79191(11) 0.50012(7) 0.0725(7) Uani 1 1 d . U . . . Cl2 Cl 0.7777(2) 0.82497(10) 0.67044(8) 0.0743(7) Uani 1 1 d . U . . . Cl3 Cl 0.0110(2) 0.66237(10) 0.67044(8) 0.0726(7) Uani 1 1 d . U . . . O8 O 0.3957(8) 0.7438(3) 0.76621(18) 0.0655(18) Uani 1 1 d . U . . . H8C H 0.369667 0.763494 0.786404 0.098 Uiso 1 1 d G . . . . H8D H 0.413527 0.716932 0.779681 0.098 Uiso 1 1 d G . . . . C0AA C 0.6847(16) 0.5557(4) 0.7280(4) 0.132(3) Uani 1 1 d . U . . . H0AA H 0.637873 0.542507 0.753538 0.159 Uiso 1 1 calc R . . . . H0AB H 0.764448 0.535669 0.723558 0.159 Uiso 1 1 calc R . . . . H1B H 0.454(8) 0.755(2) 0.528(3) 0.04(2) Uiso 1 1 d . . . . . H4A H 0.194(11) 0.702(4) 0.690(3) 0.10(4) Uiso 1 1 d . . . . . H2B H 0.683(13) 0.789(5) 0.612(4) 0.14(5) Uiso 1 1 d . . . . . H3B H 0.510(11) 0.761(4) 0.715(4) 0.10(4) Uiso 1 1 d . . . . . H4B H 0.288(10) 0.732(4) 0.710(3) 0.08(4) Uiso 1 1 d . . . . . H5B H 0.157(12) 0.712(5) 0.5748(18) 0.16(5) Uiso 1 1 d D . . . . 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 0.0363(2) 0.03342(18) 0.02710(19) 0.00109(12) 0.00010(18) -0.00054(13) P1 0.0437(11) 0.0374(8) 0.0496(11) -0.0009(9) -0.0018(9) 0.0045(7) P2 0.0439(11) 0.0382(8) 0.0549(12) 0.0033(9) 0.0033(9) 0.0048(8) O1 0.054(3) 0.080(4) 0.0267(9) 0.0007(16) 0.0012(16) -0.012(3) O2 0.045(2) 0.067(3) 0.040(2) 0.003(3) 0.0037(19) -0.016(2) O3 0.053(3) 0.065(3) 0.0327(17) -0.001(2) -0.0066(17) -0.016(2) O4 0.053(3) 0.065(3) 0.0304(17) 0.005(2) 0.0040(17) -0.015(2) O5 0.048(2) 0.069(3) 0.037(2) 0.005(3) -0.0079(19) -0.019(2) O6 0.062(3) 0.0395(12) 0.057(3) 0.0027(17) 0.003(2) 0.0105(14) O7 0.062(3) 0.0389(12) 0.061(3) 0.0001(16) 0.001(2) 0.0091(14) N1 0.060(4) 0.055(3) 0.092(4) 0.001(4) -0.031(3) 0.003(2) N2 0.051(3) 0.048(2) 0.043(3) 0.007(3) -0.005(2) -0.002(2) N3 0.078(5) 0.045(3) 0.060(2) -0.004(2) 0.021(2) -0.002(3) N4 0.061(3) 0.047(3) 0.056(3) -0.004(3) 0.003(2) -0.005(2) N5 0.067(4) 0.061(3) 0.098(4) 0.001(4) 0.036(3) 0.007(3) N6 0.079(5) 0.054(3) 0.067(2) 0.011(3) -0.018(3) 0.003(3) C1 0.062(5) 0.084(7) 0.084(4) 0.014(6) -0.025(3) -0.021(4) C2 0.053(5) 0.154(13) 0.155(8) 0.042(9) -0.006(5) -0.022(7) C3 0.100(5) 0.153(9) 0.133(5) 0.003(7) 0.057(5) -0.025(7) C4 0.104(6) 0.079(6) 0.054(3) 0.006(4) 0.020(3) -0.013(5) C5 0.113(7) 0.082(4) 0.155(8) -0.008(5) -0.073(6) 0.038(4) C6 0.084(8) 0.145(7) 0.123(10) -0.007(8) -0.047(6) 0.044(7) C7 0.098(9) 0.134(7) 0.140(12) 0.022(8) -0.071(7) -0.027(7) C8 0.067(6) 0.082(4) 0.078(7) -0.006(5) -0.021(4) -0.016(4) C9 0.188(13) 0.052(3) 0.107(7) -0.016(4) 0.088(8) -0.003(6) C10 0.157(8) 0.082(4) 0.122(7) -0.013(5) 0.086(6) 0.009(6) C11 0.088(8) 0.097(5) 0.066(6) -0.013(5) 0.029(4) -0.017(5) C12 0.071(6) 0.060(3) 0.058(4) 0.006(3) 0.010(4) -0.007(4) C13 0.080(7) 0.093(4) 0.084(7) 0.004(5) 0.032(5) -0.017(4) C14 0.098(9) 0.169(8) 0.146(13) -0.035(10) 0.075(8) -0.032(8) C15 0.117(11) 0.173(8) 0.135(12) 0.023(10) 0.061(8) 0.079(9) C16 0.124(7) 0.092(4) 0.165(8) -0.002(6) 0.070(6) 0.045(5) C17 0.088(7) 0.071(3) 0.056(4) 0.002(4) -0.011(4) 0.002(4) C18 0.141(7) 0.096(4) 0.103(5) 0.017(4) -0.062(4) -0.001(5) C20 0.170(8) 0.062(3) 0.120(6) 0.027(4) -0.078(5) 0.002(5) C21 0.057(4) 0.060(5) 0.095(4) 0.000(5) 0.012(3) -0.013(4) C22 0.062(4) 0.107(9) 0.152(8) -0.027(8) -0.009(5) -0.012(6) C23 0.119(7) 0.120(10) 0.143(7) 0.018(9) -0.071(6) -0.028(9) C24 0.124(7) 0.100(8) 0.065(3) -0.006(5) -0.018(4) -0.036(7) Cl1 0.0526(14) 0.127(2) 0.0379(11) 0.0044(12) 0.0141(10) -0.0026(13) Cl2 0.0545(15) 0.108(2) 0.0608(14) 0.0066(13) -0.0103(12) -0.0265(13) Cl3 0.0593(15) 0.1007(19) 0.0578(14) -0.0065(12) 0.0129(12) -0.0227(13) O8 0.076(5) 0.090(5) 0.031(3) 0.002(3) 0.003(3) -0.006(4) C0AA 0.179(8) 0.087(4) 0.132(7) 0.030(5) -0.090(5) 0.003(6) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 O2 Ho1 O1 71.7(2) . . ? O2 Ho1 O4 144.3(2) . . ? O2 Ho1 O5 143.44(19) . . ? O3 Ho1 O1 144.1(2) . . ? O3 Ho1 O2 72.52(19) . . ? O3 Ho1 O4 71.9(2) . . ? O3 Ho1 O5 144.0(2) . . ? O4 Ho1 O1 143.9(2) . . ? O5 Ho1 O1 71.8(2) . . ? O5 Ho1 O4 72.2(2) . . ? O6 Ho1 O1 90.6(2) . . ? O6 Ho1 O2 90.1(2) . . ? O6 Ho1 O3 87.9(2) . . ? O6 Ho1 O4 91.3(2) . . ? O6 Ho1 O5 89.4(2) . . ? O6 Ho1 O7 177.94(19) . . ? O7 Ho1 O1 91.3(2) . . ? O7 Ho1 O2 89.8(2) . . ? O7 Ho1 O3 90.1(2) . . ? O7 Ho1 O4 87.5(2) . . ? O7 Ho1 O5 91.9(2) . . ? O6 P1 N1 107.0(4) . . ? O6 P1 N2 116.5(4) . . ? O6 P1 N3 108.1(3) . . ? N1 P1 N2 105.6(4) . . ? N1 P1 N3 115.6(4) . . ? N2 P1 N3 104.4(4) . . ? O7 P2 N4 116.8(4) . . ? O7 P2 N5 107.1(4) . . ? O7 P2 N6 108.7(4) . . ? N4 P2 N6 103.3(4) . . ? N5 P2 N4 106.0(4) . . ? N5 P2 N6 115.3(4) . . ? Ho1 O1 H1A 111.1 . . ? Ho1 O1 H1B 132(5) . . ? H1A O1 H1B 116.9 . . ? Ho1 O2 H2A 109.8 . . ? Ho1 O2 H2B 140(7) . . ? H2A O2 H2B 109.6 . . ? Ho1 O3 H3A 110.5 . . ? Ho1 O3 H3B 133(8) . . ? H3A O3 H3B 116.1 . . ? Ho1 O4 H4A 129(6) . . ? Ho1 O4 H4B 117(8) . . ? H4A O4 H4B 111(9) . . ? Ho1 O5 H5A 110.0 . . ? Ho1 O5 H5B 126(9) . . ? H5A O5 H5B 123.2 . . ? P1 O6 Ho1 170.9(4) . . ? P2 O7 Ho1 169.2(4) . . ? C5 N1 P1 123.3(7) . . ? C8 N1 P1 125.5(6) . . ? C8 N1 C5 107.9(8) . . ? C1 N2 P1 120.3(5) . . ? C4 N2 P1 119.8(6) . . ? C4 N2 C1 108.3(7) . . ? C9 N3 P1 124.1(6) . . ? C12 N3 P1 121.3(6) . . ? C12 N3 C9 110.3(7) . . ? C21 N4 P2 119.2(6) . . ? C24 N4 P2 119.9(6) . . ? C24 N4 C21 108.4(8) . . ? C13 N5 P2 125.0(7) . . ? C16 N5 P2 123.8(7) . . ? C16 N5 C13 108.4(8) . . ? C17 N6 P2 121.3(6) . . ? C20 N6 P2 125.6(7) . . ? C20 N6 C17 109.4(7) . . ? N2 C1 H1C 110.6 . . ? N2 C1 H1D 110.6 . . ? H1C C1 H1D 108.8 . . ? C2 C1 N2 105.5(8) . . ? C2 C1 H1C 110.6 . . ? C2 C1 H1D 110.6 . . ? C1 C2 H2C 110.2 . . ? C1 C2 H2D 110.2 . . ? H2C C2 H2D 108.5 . . ? C3 C2 C1 107.7(11) . . ? C3 C2 H2C 110.2 . . ? C3 C2 H2D 110.2 . . ? C2 C3 H3C 109.4 . . ? C2 C3 H3D 109.4 . . ? C2 C3 C4 111.0(11) . . ? H3C C3 H3D 108.0 . . ? C4 C3 H3C 109.4 . . ? C4 C3 H3D 109.4 . . ? N2 C4 H4C 110.6 . . ? N2 C4 H4D 110.6 . . ? C3 C4 N2 105.5(9) . . ? C3 C4 H4C 110.6 . . ? C3 C4 H4D 110.6 . . ? H4C C4 H4D 108.8 . . ? N1 C5 H5C 110.2 . . ? N1 C5 H5D 110.2 . . ? H5C C5 H5D 108.5 . . ? C6 C5 N1 107.4(10) . . ? C6 C5 H5C 110.2 . . ? C6 C5 H5D 110.2 . . ? C5 C6 H6A 109.7 . . ? C5 C6 H6B 109.7 . . ? C5 C6 C7 109.7(10) . . ? H6A C6 H6B 108.2 . . ? C7 C6 H6A 109.7 . . ? C7 C6 H6B 109.7 . . ? C6 C7 H7A 110.2 . . ? C6 C7 H7B 110.2 . . ? C6 C7 C8 107.8(10) . . ? H7A C7 H7B 108.5 . . ? C8 C7 H7A 110.2 . . ? C8 C7 H7B 110.2 . . ? N1 C8 C7 106.3(9) . . ? N1 C8 H8A 110.5 . . ? N1 C8 H8B 110.5 . . ? C7 C8 H8A 110.5 . . ? C7 C8 H8B 110.5 . . ? H8A C8 H8B 108.7 . . ? N3 C9 H9A 110.8 . . ? N3 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? C10 C9 N3 104.6(8) . . ? C10 C9 H9A 110.8 . . ? C10 C9 H9B 110.8 . . ? C9 C10 H10A 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C11 C10 C9 111.3(9) . . ? C11 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C10 C11 H11A 110.1 . . ? C10 C11 H11B 110.1 . . ? C10 C11 C12 108.0(8) . . ? H11A C11 H11B 108.4 . . ? C12 C11 H11A 110.1 . . ? C12 C11 H11B 110.1 . . ? N3 C12 C11 104.9(7) . . ? N3 C12 H12A 110.8 . . ? N3 C12 H12B 110.8 . . ? C11 C12 H12A 110.8 . . ? C11 C12 H12B 110.8 . . ? H12A C12 H12B 108.8 . . ? N5 C13 H13A 110.7 . . ? N5 C13 H13B 110.7 . . ? N5 C13 C14 105.3(10) . . ? H13A C13 H13B 108.8 . . ? C14 C13 H13A 110.7 . . ? C14 C13 H13B 110.7 . . ? C13 C14 H14A 110.0 . . ? C13 C14 H14B 110.0 . . ? H14A C14 H14B 108.4 . . ? C15 C14 C13 108.4(11) . . ? C15 C14 H14A 110.0 . . ? C15 C14 H14B 110.0 . . ? C14 C15 H15A 109.9 . . ? C14 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? C16 C15 C14 108.9(11) . . ? C16 C15 H15A 109.9 . . ? C16 C15 H15B 109.9 . . ? N5 C16 H16A 110.2 . . ? N5 C16 H16B 110.2 . . ? C15 C16 N5 107.7(11) . . ? C15 C16 H16A 110.2 . . ? C15 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? N6 C17 H17A 110.6 . . ? N6 C17 H17B 110.6 . . ? N6 C17 C18 105.8(8) . . ? H17A C17 H17B 108.7 . . ? C18 C17 H17A 110.6 . . ? C18 C17 H17B 110.6 . . ? C17 C18 H18A 110.8 . . ? C17 C18 H18B 110.8 . . ? H18A C18 H18B 108.8 . . ? C0AA C18 C17 105.0(9) . . ? C0AA C18 H18A 110.8 . . ? C0AA C18 H18B 110.8 . . ? N6 C20 H20A 110.9 . . ? N6 C20 H20B 110.9 . . ? H20A C20 H20B 108.9 . . ? C0AA C20 N6 104.5(9) . . ? C0AA C20 H20A 110.9 . . ? C0AA C20 H20B 110.9 . . ? N4 C21 H21A 110.6 . . ? N4 C21 H21B 110.6 . . ? H21A C21 H21B 108.7 . . ? C22 C21 N4 105.8(9) . . ? C22 C21 H21A 110.6 . . ? C22 C21 H21B 110.6 . . ? C21 C22 H22A 110.6 . . ? C21 C22 H22B 110.6 . . ? H22A C22 H22B 108.7 . . ? C23 C22 C21 105.8(10) . . ? C23 C22 H22A 110.6 . . ? C23 C22 H22B 110.6 . . ? C22 C23 H23A 110.0 . . ? C22 C23 H23B 110.0 . . ? C22 C23 C24 108.5(11) . . ? H23A C23 H23B 108.4 . . ? C24 C23 H23A 110.0 . . ? C24 C23 H23B 110.0 . . ? N4 C24 C23 104.6(10) . . ? N4 C24 H24A 110.8 . . ? N4 C24 H24B 110.8 . . ? C23 C24 H24A 110.8 . . ? C23 C24 H24B 110.8 . . ? H24A C24 H24B 108.9 . . ? H8C O8 H8D 104.4 . . ? C18 C0AA C20 114.6(10) . . ? C18 C0AA H0AA 108.6 . . ? C18 C0AA H0AB 108.6 . . ? C20 C0AA H0AA 108.6 . . ? C20 C0AA H0AB 108.6 . . ? H0AA C0AA H0AB 107.6 . . ? 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 Ho1 O1 2.366(5) . ? Ho1 O2 2.344(5) . ? Ho1 O3 2.343(5) . ? Ho1 O4 2.356(5) . ? Ho1 O5 2.355(5) . ? Ho1 O6 2.205(5) . ? Ho1 O7 2.215(5) . ? P1 O6 1.495(5) . ? P1 N1 1.605(7) . ? P1 N2 1.632(7) . ? P1 N3 1.636(7) . ? P2 O7 1.487(5) . ? P2 N4 1.628(7) . ? P2 N5 1.613(8) . ? P2 N6 1.630(7) . ? O1 H1A 0.8784 . ? O1 H1B 0.88(8) . ? O2 H2A 0.8552 . ? O2 H2B 0.96(13) . ? O3 H3A 0.8646 . ? O3 H3B 0.83(11) . ? O4 H4A 0.90(11) . ? O4 H4B 0.75(10) . ? O5 H5A 0.8653 . ? O5 H5B 0.87(2) . ? N1 C5 1.483(12) . ? N1 C8 1.449(11) . ? N2 C1 1.484(11) . ? N2 C4 1.482(10) . ? N3 C9 1.466(11) . ? N3 C12 1.462(10) . ? N4 C21 1.488(11) . ? N4 C24 1.485(12) . ? N5 C13 1.460(11) . ? N5 C16 1.459(12) . ? N6 C17 1.475(11) . ? N6 C20 1.466(11) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C1 C2 1.482(14) . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C2 C3 1.411(16) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C3 C4 1.448(15) . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 H5C 0.9700 . ? C5 H5D 0.9700 . ? C5 C6 1.401(14) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C7 1.447(16) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.472(14) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 C10 1.464(14) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C11 1.399(13) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C12 1.498(12) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.470(15) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.444(17) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 C16 1.404(16) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C18 1.511(13) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 C0AA 1.404(14) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 C0AA 1.425(14) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 C22 1.478(14) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 C23 1.443(17) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 C24 1.485(17) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? O8 H8C 0.8500 . ? O8 H8D 0.8501 . ? C0AA H0AA 0.9700 . ? C0AA H0AB 0.9700 . ?