#------------------------------------------------------------------------------ #$Date: 2020-02-04 22:05:34 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247598 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/57/7125701.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_7125701 loop_ _publ_author_name 'Tsoureas, Nikolaos' 'Mansikkam\"aki, Akseli' 'Layfield, Richard A.' _publ_section_title ; Uranium(iv) cyclobutadienyl sandwich compounds: synthesis, structure and chemical bonding. ; _journal_issue 6 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 944 _journal_page_last 947 _journal_paper_doi 10.1039/c9cc09018e _journal_volume 56 _journal_year 2020 _chemical_formula_moiety 'C24 H64 B3 K O2 Si4 U' _chemical_formula_sum 'C24 H64 B3 K O2 Si4 U' _chemical_formula_weight 794.57 _chemical_name_systematic 2 _chemical_properties_physical Air-sensitive,Moisture-sensitive,Oxygen-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-11-19 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-12-10 deposited with the CCDC. 2019-12-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.572(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.5143(5) _cell_length_b 15.8092(8) _cell_length_c 16.0534(5) _cell_measurement_reflns_used 5660 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 67.3540 _cell_measurement_theta_min 3.9760 _cell_volume 3903.1(3) _computing_cell_refinement 'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.37a (Rigaku OD, 2019)' _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 n/a (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'Rigaku Saturn724+' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _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 -71.00 88.00 0.50 1.00 -- 0.00 10.00-120.00 318 2 \w -19.00 6.00 0.50 1.00 -- 5.00 36.00 -89.00 50 3 \w -106.00 -73.00 0.50 4.00 -- -90.00 36.00 -89.00 66 4 \w -175.00-128.00 0.50 4.00 -- -90.00 36.00 -89.00 94 5 \w -68.00 -22.00 0.50 4.00 -- -90.00 39.00 30.00 92 6 \w -179.00-107.00 0.50 4.00 -- -90.00 30.00 0.00 144 7 \w -88.00 -2.00 0.50 4.00 -- -90.00 30.00 0.00 172 8 \w -121.00 -3.00 0.50 4.00 -- -90.00 39.00-180.00 236 9 \w -178.00-148.00 0.50 4.00 -- -90.00 10.00-180.00 60 10 \w -178.00 -2.00 0.50 4.00 -- -90.00 49.00 150.00 352 11 \w -106.00 -80.00 0.50 4.00 -- -90.00 10.00-180.00 52 12 \w -61.00 -2.00 0.50 4.00 -- -90.00 10.00-180.00 118 13 \w -178.00-149.00 0.50 4.00 -- -90.00 49.00 120.00 58 14 \w -105.00 -64.00 0.50 4.00 -- -90.00 49.00 120.00 82 15 \w -111.00 -85.00 0.50 4.00 -- -90.00 0.00-180.00 52 16 \w -179.00-102.00 0.50 4.00 -- -90.00 39.00 30.00 154 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC11 (RCD3): quarter-chi single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0005830000 _diffrn_orient_matrix_UB_12 0.0570368000 _diffrn_orient_matrix_UB_13 -0.0779094000 _diffrn_orient_matrix_UB_21 -0.1001817000 _diffrn_orient_matrix_UB_22 -0.0000172000 _diffrn_orient_matrix_UB_23 -0.0120411000 _diffrn_orient_matrix_UB_31 0.0003850000 _diffrn_orient_matrix_UB_32 0.0789825000 _diffrn_orient_matrix_UB_33 0.0561992000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_unetI/netI 0.0706 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 14621 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.359 _diffrn_reflns_theta_min 2.873 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 13.959 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.32972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour brown _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.352 _exptl_crystal_description plate _exptl_crystal_F_000 1576 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: n-pentane' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.01 _refine_diff_density_max 3.600 _refine_diff_density_min -1.152 _refine_diff_density_rms 0.217 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 369 _refine_ls_number_reflns 14621 _refine_ls_number_restraints 887 _refine_ls_restrained_S_all 0.976 _refine_ls_R_factor_all 0.1552 _refine_ls_R_factor_gt 0.0991 _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^)+(0.1969P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2690 _refine_ls_wR_factor_ref 0.3009 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7876 _reflns_number_total 14621 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc09018e2.cif _cod_data_source_block 2 _cod_depositor_comments 'Adding full bibliography for 7125700--7125702.cif.' _cod_database_code 7125701 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'C96 H228 B12 K4 O8 Si16 U4 ' _chemical_oxdiff_usercomment NTL12p63 _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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.5120(19) 0.4880(19) 2. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances H16B-H5A -1.8 with sigma of 0.02 C17-C18 \\sim C18-C19 \\sim C19-C20 with sigma of 0.02 O2-C17 \\sim O2-C20 with sigma of 0.02 O2-C18 \\sim O2-C19 with sigma of 0.04 C18-C20 \\sim C17-C19 with sigma of 0.04 C0AA-C1AA \\sim C1AA-C7AA \\sim C7AA-C8AA with sigma of 0.02 O1-C0AA \\sim O1-C8AA with sigma of 0.02 O1-C1AA \\sim O1-C7AA with sigma of 0.04 C1AA-C8AA \\sim C0AA-C7AA with sigma of 0.04 K1-O1 \\sim K1-O1A with sigma of 0.02 O1-C0AA \\sim O1A-C1A with sigma of 0.02 O1-C8AA \\sim O1A-C9A with sigma of 0.02 C0AA-C1AA \\sim C1A-C2A with sigma of 0.02 C1AA-C7AA \\sim C2A-C7A with sigma of 0.02 C7AA-C8AA \\sim C7A-C9A with sigma of 0.02 K1-C0AA \\sim K1-C1A with sigma of 0.04 K1-C8AA \\sim K1-C9A with sigma of 0.04 O1-C1AA \\sim O1A-C2A with sigma of 0.04 O1-C7AA \\sim O1A-C7A with sigma of 0.04 C0AA-C7AA \\sim C1A-C7A with sigma of 0.04 C0AA-C8AA \\sim C1A-C9A with sigma of 0.04 C1AA-C8AA \\sim C2A-C9A with sigma of 0.04 C4-C15 \\sim C4-C14 \\sim C4-C16 \\sim C15-C14 \\sim C15-C16 \\sim C14-C16 with sigma of 0.04 Si3-C4 \\sim Si3-C15 \\sim Si3-C14 \\sim Si3-C16 with sigma of 0.02 4. Rigid bond restraints All non-hydrogen atoms with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 6. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 7. Others Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(O1A)=Sof(C1A)=Sof(H1AC)=Sof(H1AD)=Sof(C2A)= Sof(H2AA)=Sof(H2AB)=Sof(C7A)=Sof(H7AC)=Sof(H7AD)=1-FVAR(1) Sof(O1)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(C7AA)= Sof(H7AA)=Sof(H7AB)=Sof(C8AA)=Sof(H8AA)=Sof(H8AB)=FVAR(1) 8.a Secondary CH2 refined with riding coordinates: C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C0AA(H0AA, H0AB), C1AA(H1AA,H1AB), C7AA(H7AA,H7AB), C8AA(H8AA,H8AB), C9A(H9AA,H9AB), C1A(H1AC,H1AD), C2A(H2AA,H2AB), C7A(H7AC,H7AD) 8.b Me refined with riding coordinates: C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C5(H5A,H5B,H5C) 8.c Idealised Me refined as rotating group: C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C7(H7A,H7B, H7C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C) ; _shelx_res_file ; 2019ncs0032z_twin1_hklf4.res created by SHELXL-2014/7 TITL 2019ncs0032z_twin1_hklf4_a.res in P2(1)/c REM Old TITL 2019ncs0032z_twin1_hklf4 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.220, Rweak 0.062, Alpha 0.175 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C5 O4 Si4 K U CELL 1.54184 15.5143 15.8092 16.0534 90 97.572 90 ZERR 4 0.0005 0.0008 0.0005 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B K O Si U UNIT 96 208 12 4 8 16 4 EQIV $1 1-X,1-Y,1-Z DFIX -1.8 H16b H5a SADI C17 C18 C18 C19 C19 C20 SADI O2 C17 O2 C20 SADI 0.04 O2 C18 O2 C19 SADI 0.04 C18 C20 C17 C19 SADI C0AA C1AA C1AA C7AA C7AA C8AA SADI O1 C0AA O1 C8AA SADI 0.04 O1 C1AA O1 C7AA SADI 0.04 C1AA C8AA C0AA C7AA SADI K1 O1 K1 O1A SADI O1 C0AA O1A C1A SADI O1 C8AA O1A C9A SADI C0AA C1AA C1A C2A SADI C1AA C7AA C2A C7A SADI C7AA C8AA C7A C9A SADI 0.04 K1 C0AA K1 C1A SADI 0.04 K1 C8AA K1 C9A SADI 0.04 O1 C1AA O1A C2A SADI 0.04 O1 C7AA O1A C7A SADI 0.04 C0AA C7AA C1A C7A SADI 0.04 C0AA C8AA C1A C9A SADI 0.04 C1AA C8AA C2A C9A SADI 0.04 C4 C15 C4 C14 C4 C16 C15 C14 C15 C16 C14 C16 SADI Si3 C4 Si3 C15 Si3 C14 Si3 C16 DELU SIMU RIGU L.S. 18 0 0 PLAN 5 BIND B2 K1 BIND K1 B3_$1 FREE K1 C0AA FREE C20 C17 CONF BOND $H MORE -1 list 4 fmap 2 53 acta REM REM REM WGHT 0.196900 BASF 0.48801 FVAR 0.58347 0.43147 U1 7 0.338162 0.461152 0.317207 11.00000 0.06994 0.11008 = 0.07398 0.01093 0.00150 0.01427 K1 4 0.612382 0.639330 0.355193 11.00000 0.15561 0.14521 = 0.15549 -0.05093 0.03032 -0.00045 SI3 6 0.214248 0.631486 0.158028 11.00000 0.18094 0.09592 = 0.08919 0.02980 0.00468 0.00413 SI1 6 0.164641 0.618628 0.394132 11.00000 0.14728 0.10271 = 0.10644 -0.01561 0.03816 0.02253 SI4 6 0.167308 0.385271 0.130224 11.00000 0.16425 0.13474 = 0.09943 -0.03183 -0.02066 -0.01922 SI2 6 0.120977 0.371993 0.370511 11.00000 0.15877 0.12586 = 0.13123 0.00101 0.06609 -0.04078 C4 1 0.214443 0.544974 0.234242 11.00000 0.09718 0.07874 = 0.06861 0.00465 0.00725 0.01222 C2 1 0.179198 0.447675 0.310658 11.00000 0.08869 0.07738 = 0.07973 0.00212 0.01894 0.01279 C1 1 0.197439 0.538167 0.319999 11.00000 0.09962 0.07890 = 0.07209 0.00595 0.01274 0.01092 C3 1 0.194695 0.454563 0.222365 11.00000 0.09746 0.08711 = 0.07557 0.00131 0.00930 0.01013 C15 1 0.100217 0.659053 0.118326 11.00000 0.20035 0.16195 = 0.15964 0.07562 -0.00213 0.03217 AFIX 137 H15A 2 0.068970 0.608708 0.099451 11.00000 -1.50000 H15B 2 0.099236 0.698031 0.072356 11.00000 -1.50000 H15C 2 0.073328 0.684713 0.162588 11.00000 -1.50000 AFIX 0 C10 1 0.131683 0.260235 0.349744 11.00000 0.20717 0.11261 = 0.23130 0.01291 0.06509 -0.03935 AFIX 137 H10A 2 0.175430 0.252020 0.313431 11.00000 -1.50000 H10B 2 0.077119 0.238583 0.323071 11.00000 -1.50000 H10C 2 0.148181 0.230816 0.401715 11.00000 -1.50000 AFIX 0 C6 1 0.181432 0.593268 0.506790 11.00000 0.20725 0.23538 = 0.10361 -0.02687 0.04291 0.06954 AFIX 33 H6A 2 0.160957 0.536996 0.515155 11.00000 -1.50000 H6B 2 0.242270 0.596763 0.527473 11.00000 -1.50000 H6C 2 0.149842 0.632792 0.536608 11.00000 -1.50000 AFIX 0 C14 1 0.265708 0.598714 0.064740 11.00000 0.24112 0.17607 = 0.11616 0.05571 0.04423 0.02402 AFIX 137 H14A 2 0.324764 0.581942 0.082389 11.00000 -1.50000 H14B 2 0.264861 0.645282 0.026261 11.00000 -1.50000 H14C 2 0.234045 0.552014 0.037450 11.00000 -1.50000 AFIX 0 B2 3 0.451404 0.553464 0.250098 11.00000 0.11690 0.16478 = 0.12956 0.01373 0.02791 -0.00830 C7 1 0.043554 0.638885 0.361579 11.00000 0.16646 0.15167 = 0.14904 -0.00703 0.04432 0.05949 AFIX 137 H7A 2 0.026666 0.617365 0.305901 11.00000 -1.50000 H7B 2 0.032434 0.698596 0.362371 11.00000 -1.50000 H7C 2 0.010683 0.610879 0.400099 11.00000 -1.50000 AFIX 0 B1 3 0.380403 0.306357 0.298510 11.00000 0.14791 0.12267 = 0.14420 0.02189 0.02463 0.06130 B3 3 0.372624 0.484258 0.473166 11.00000 0.13403 0.19135 = 0.08623 0.00543 -0.00964 0.02386 C12 1 0.181608 0.270876 0.153606 11.00000 0.26005 0.12461 = 0.20766 -0.04006 -0.01576 -0.01168 AFIX 137 H12A 2 0.238230 0.261359 0.184181 11.00000 -1.50000 H12B 2 0.176016 0.239557 0.101942 11.00000 -1.50000 H12C 2 0.137981 0.252490 0.186800 11.00000 -1.50000 AFIX 0 C8 1 0.108156 0.396003 0.474836 11.00000 0.26519 0.22437 = 0.16675 -0.00448 0.12054 -0.06997 AFIX 33 H8A 2 0.163962 0.395814 0.508736 11.00000 -1.50000 H8B 2 0.082149 0.450912 0.477123 11.00000 -1.50000 H8C 2 0.071339 0.354424 0.495750 11.00000 -1.50000 AFIX 0 C16 1 0.278905 0.723428 0.196730 11.00000 0.30232 0.13865 = 0.18704 0.03222 -0.01099 -0.06163 AFIX 33 H16A 2 0.275578 0.765718 0.153510 11.00000 -1.50000 H16B 2 0.256708 0.746153 0.245119 11.00000 -1.50000 H16C 2 0.338389 0.706704 0.211887 11.00000 -1.50000 AFIX 0 C11 1 0.047887 0.372769 0.125399 11.00000 0.17883 0.19776 = 0.21149 -0.05359 -0.03923 -0.02863 AFIX 33 H11A 2 0.034508 0.349923 0.177599 11.00000 -1.50000 H11B 2 0.020305 0.426884 0.115732 11.00000 -1.50000 H11C 2 0.027035 0.335029 0.080367 11.00000 -1.50000 AFIX 0 C13 1 0.187919 0.425844 0.036583 11.00000 0.34349 0.19628 = 0.10784 -0.04514 0.02132 -0.05705 AFIX 33 H13A 2 0.171601 0.385345 -0.007221 11.00000 -1.50000 H13B 2 0.154962 0.476835 0.024786 11.00000 -1.50000 H13C 2 0.248813 0.438225 0.039397 11.00000 -1.50000 AFIX 0 C9 1 0.007484 0.383914 0.355538 11.00000 0.16209 0.17821 = 0.27810 0.00516 0.09210 -0.03896 AFIX 137 H9A 2 -0.014015 0.376271 0.297165 11.00000 -1.50000 H9B 2 -0.007365 0.439551 0.372927 11.00000 -1.50000 H9C 2 -0.018228 0.342439 0.388334 11.00000 -1.50000 AFIX 0 C5 1 0.203182 0.720322 0.385455 11.00000 0.25731 0.12464 = 0.25364 -0.05570 0.10869 -0.01421 AFIX 33 H5A 2 0.195896 0.736813 0.327399 11.00000 -1.50000 H5B 2 0.171322 0.758351 0.416639 11.00000 -1.50000 H5C 2 0.263750 0.722322 0.407504 11.00000 -1.50000 AFIX 0 O2 5 0.717552 0.548930 0.280894 11.00000 0.14834 0.15452 = 0.18666 -0.08160 0.03383 -0.02077 C17 1 0.708449 0.466624 0.250636 11.00000 0.21072 0.17139 = 0.23562 -0.09797 0.08440 -0.03065 AFIX 23 H17A 2 0.647641 0.454047 0.232687 11.00000 -1.20000 H17B 2 0.730463 0.426776 0.294260 11.00000 -1.20000 AFIX 0 C18 1 0.758999 0.459994 0.178337 11.00000 0.20832 0.19596 = 0.21127 -0.08531 0.07121 -0.00867 AFIX 23 H18A 2 0.784312 0.404175 0.175138 11.00000 -1.20000 H18B 2 0.723047 0.472484 0.125660 11.00000 -1.20000 AFIX 0 C19 1 0.826950 0.525222 0.198998 11.00000 0.20022 0.21815 = 0.19943 -0.06030 0.06559 -0.01492 AFIX 23 H19A 2 0.820525 0.571847 0.159387 11.00000 -1.20000 H19B 2 0.885033 0.501755 0.201835 11.00000 -1.20000 AFIX 0 C20 1 0.805963 0.550866 0.283540 11.00000 0.16192 0.17384 = 0.18894 -0.05021 0.04549 -0.00917 AFIX 23 H20A 2 0.832885 0.512198 0.326157 11.00000 -1.20000 H20B 2 0.827677 0.607401 0.297196 11.00000 -1.20000 AFIX 0 PART 1 O1 5 0.541083 0.756906 0.439207 21.00000 0.22025 0.16140 = 0.13622 -0.02082 0.04328 0.04182 C0AA 1 0.588906 0.807442 0.509269 21.00000 0.23531 0.14813 = 0.12805 -0.01526 0.03761 0.04311 AFIX 23 H0AA 2 0.618308 0.770782 0.552437 21.00000 -1.20000 H0AB 2 0.631395 0.844363 0.488755 21.00000 -1.20000 AFIX 0 C1AA 1 0.523800 0.854136 0.540003 21.00000 0.24539 0.16353 = 0.12734 -0.01137 0.04062 0.05180 AFIX 23 H1AA 2 0.547785 0.898542 0.577852 21.00000 -1.20000 H1AB 2 0.486011 0.818408 0.568393 21.00000 -1.20000 AFIX 0 C7AA 1 0.480528 0.887122 0.465272 21.00000 0.23862 0.16472 = 0.12504 -0.01098 0.04272 0.05238 AFIX 23 H7AA 2 0.425598 0.912530 0.474268 21.00000 -1.20000 H7AB 2 0.515827 0.929243 0.441716 21.00000 -1.20000 AFIX 0 C8AA 1 0.467508 0.817263 0.413423 21.00000 0.22910 0.16985 = 0.13184 -0.01566 0.04254 0.04952 AFIX 23 H8AA 2 0.466992 0.833852 0.355187 21.00000 -1.20000 H8AB 2 0.412296 0.790729 0.419453 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C9A 1 0.469882 0.834017 0.375497 -21.00000 0.20440 0.15977 = 0.10937 0.00072 0.05045 0.04038 AFIX 23 H9AA 2 0.493056 0.853310 0.325560 -21.00000 -1.20000 H9AB 2 0.408723 0.820922 0.360502 -21.00000 -1.20000 AFIX 0 O1A 5 0.518014 0.758089 0.410967 -21.00000 0.21657 0.15797 = 0.11603 -0.00347 0.04203 0.04488 C1A 1 0.510694 0.772984 0.501865 -21.00000 0.23859 0.16205 = 0.11386 -0.00104 0.04468 0.05188 AFIX 23 H1AC 2 0.454883 0.753841 0.515660 -21.00000 -1.20000 H1AD 2 0.556627 0.743902 0.537623 -21.00000 -1.20000 AFIX 0 C2A 1 0.518856 0.859428 0.510810 -21.00000 0.25217 0.16421 = 0.11653 -0.00331 0.03432 0.05007 AFIX 23 H2AA 2 0.490289 0.878633 0.557614 -21.00000 -1.20000 H2AB 2 0.579756 0.875126 0.521437 -21.00000 -1.20000 AFIX 0 C7A 1 0.480485 0.895539 0.437115 -21.00000 0.22253 0.16080 = 0.10842 -0.00159 0.04883 0.04949 AFIX 23 H7AC 2 0.516829 0.940807 0.420497 -21.00000 -1.20000 H7AD 2 0.424458 0.919221 0.445019 -21.00000 -1.20000 AFIX 0 HKLF 5 REM 2019ncs0032z_twin1_hklf4_a.res in P2(1)/c REM R1 = 0.0991 for 7876 Fo > 4sig(Fo) and 0.1552 for all 14621 data REM 369 parameters refined using 887 restraints END WGHT 0.1970 0.0000 REM Highest difference peak 3.600, deepest hole -1.152, 1-sigma level 0.217 Q1 1 0.3216 0.4033 0.2976 11.00000 0.05 3.60 Q2 1 0.3519 0.4620 0.2665 11.00000 0.05 3.39 Q3 1 0.2685 0.3717 0.0570 11.00000 0.05 1.10 Q4 1 0.6956 0.5467 0.1787 11.00000 0.05 1.06 Q5 1 0.2051 0.3545 0.4906 11.00000 0.05 1.04 ; _shelx_res_checksum 90384 _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 4.580 _oxdiff_exptl_absorpt_empirical_full_min 0.185 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 _twin_special_details ; Component 2 rotated by 15.7246\% around [0.96 -0.13 -0.23] (reciprocal) or [0.99 -0.13 -0.09] (direct) ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 U1 U 0.33816(4) 0.46115(4) 0.31721(3) 0.0854(3) Uani 1 1 d . U . . . K1 K 0.6124(5) 0.6393(4) 0.3552(4) 0.151(2) Uani 1 1 d D U . . . Si3 Si 0.2142(5) 0.6315(4) 0.1580(4) 0.123(2) Uani 1 1 d D U . . . Si1 Si 0.1646(5) 0.6186(4) 0.3941(4) 0.117(2) Uani 1 1 d . U . . . Si4 Si 0.1673(6) 0.3853(5) 0.1302(4) 0.136(3) Uani 1 1 d . U . . . Si2 Si 0.1210(6) 0.3720(5) 0.3705(5) 0.134(2) Uani 1 1 d . U . . . C4 C 0.2144(12) 0.5450(10) 0.2342(10) 0.082(3) Uani 1 1 d D U . . . C2 C 0.1792(12) 0.4477(11) 0.3107(11) 0.081(3) Uani 1 1 d . U . . . C1 C 0.1974(13) 0.5382(11) 0.3200(11) 0.083(3) Uani 1 1 d . U . . . C3 C 0.1947(14) 0.4546(12) 0.2224(11) 0.087(3) Uani 1 1 d . U . . . C15 C 0.1002(15) 0.6591(18) 0.1183(18) 0.176(9) Uani 1 1 d D U . . . H15A H 0.0690 0.6087 0.0995 0.264 Uiso 1 1 calc GR . . . . H15B H 0.0992 0.6980 0.0724 0.264 Uiso 1 1 calc GR . . . . H15C H 0.0733 0.6847 0.1626 0.264 Uiso 1 1 calc GR . . . . C10 C 0.132(2) 0.2602(16) 0.350(2) 0.180(10) Uani 1 1 d . U . . . H10A H 0.1754 0.2520 0.3134 0.271 Uiso 1 1 calc GR . . . . H10B H 0.0771 0.2386 0.3231 0.271 Uiso 1 1 calc GR . . . . H10C H 0.1482 0.2308 0.4017 0.271 Uiso 1 1 calc GR . . . . C6 C 0.181(2) 0.593(2) 0.5068(16) 0.180(10) Uani 1 1 d . U . . . H6A H 0.1610 0.5370 0.5152 0.270 Uiso 1 1 calc R . . . . H6B H 0.2423 0.5968 0.5275 0.270 Uiso 1 1 calc R . . . . H6C H 0.1498 0.6328 0.5366 0.270 Uiso 1 1 calc R . . . . C14 C 0.266(2) 0.5987(18) 0.0647(14) 0.176(9) Uani 1 1 d D U . . . H14A H 0.3248 0.5819 0.0824 0.264 Uiso 1 1 calc GR . . . . H14B H 0.2649 0.6453 0.0263 0.264 Uiso 1 1 calc GR . . . . H14C H 0.2340 0.5520 0.0374 0.264 Uiso 1 1 calc GR . . . . B2 B 0.451(2) 0.553(2) 0.250(2) 0.136(7) Uani 1 1 d . U . . . C7 C 0.044(2) 0.6389(18) 0.3616(18) 0.154(8) Uani 1 1 d . U . . . H7A H 0.0267 0.6174 0.3059 0.230 Uiso 1 1 calc GR . . . . H7B H 0.0324 0.6986 0.3624 0.230 Uiso 1 1 calc GR . . . . H7C H 0.0107 0.6109 0.4001 0.230 Uiso 1 1 calc GR . . . . B1 B 0.380(2) 0.306(2) 0.299(2) 0.138(8) Uani 1 1 d . U . . . B3 B 0.373(2) 0.484(3) 0.4732(17) 0.139(8) Uani 1 1 d . U . . . C12 C 0.182(3) 0.271(2) 0.154(2) 0.202(11) Uani 1 1 d . U . . . H12A H 0.2382 0.2614 0.1842 0.302 Uiso 1 1 calc GR . . . . H12B H 0.1760 0.2396 0.1019 0.302 Uiso 1 1 calc GR . . . . H12C H 0.1380 0.2525 0.1868 0.302 Uiso 1 1 calc GR . . . . C8 C 0.108(3) 0.396(2) 0.475(2) 0.211(11) Uani 1 1 d . U . . . H8A H 0.1640 0.3958 0.5087 0.316 Uiso 1 1 calc R . . . . H8B H 0.0821 0.4509 0.4771 0.316 Uiso 1 1 calc R . . . . H8C H 0.0713 0.3544 0.4958 0.316 Uiso 1 1 calc R . . . . C16 C 0.279(2) 0.7234(16) 0.1967(17) 0.213(11) Uani 1 1 d D U . . . H16A H 0.2756 0.7657 0.1535 0.320 Uiso 1 1 calc R . . . . H16B H 0.2567 0.7462 0.2451 0.320 Uiso 1 1 calc DR . . . . H16C H 0.3384 0.7067 0.2119 0.320 Uiso 1 1 calc R . . . . C11 C 0.048(2) 0.373(2) 0.125(2) 0.202(10) Uani 1 1 d . U . . . H11A H 0.0345 0.3499 0.1776 0.303 Uiso 1 1 calc R . . . . H11B H 0.0203 0.4269 0.1157 0.303 Uiso 1 1 calc R . . . . H11C H 0.0270 0.3350 0.0804 0.303 Uiso 1 1 calc R . . . . C13 C 0.188(3) 0.426(2) 0.0366(19) 0.217(12) Uani 1 1 d . U . . . H13A H 0.1716 0.3853 -0.0072 0.325 Uiso 1 1 calc R . . . . H13B H 0.1550 0.4768 0.0248 0.325 Uiso 1 1 calc R . . . . H13C H 0.2488 0.4382 0.0394 0.325 Uiso 1 1 calc R . . . . C9 C 0.007(2) 0.384(2) 0.356(3) 0.200(9) Uani 1 1 d . U . . . H9A H -0.0140 0.3763 0.2972 0.301 Uiso 1 1 calc GR . . . . H9B H -0.0074 0.4396 0.3729 0.301 Uiso 1 1 calc GR . . . . H9C H -0.0182 0.3424 0.3883 0.301 Uiso 1 1 calc GR . . . . C5 C 0.203(3) 0.7203(19) 0.385(2) 0.205(10) Uani 1 1 d . U . . . H5A H 0.1959 0.7368 0.3274 0.308 Uiso 1 1 calc DR . . . . H5B H 0.1713 0.7584 0.4166 0.308 Uiso 1 1 calc R . . . . H5C H 0.2638 0.7223 0.4075 0.308 Uiso 1 1 calc R . . . . O2 O 0.7176(14) 0.5489(12) 0.2809(14) 0.162(7) Uani 1 1 d D U . . . C17 C 0.708(3) 0.4666(19) 0.251(3) 0.201(11) Uani 1 1 d D U . . . H17A H 0.6476 0.4540 0.2327 0.241 Uiso 1 1 calc R . . . . H17B H 0.7305 0.4268 0.2943 0.241 Uiso 1 1 calc R . . . . C18 C 0.759(3) 0.460(2) 0.178(2) 0.201(12) Uani 1 1 d D U . . . H18A H 0.7843 0.4042 0.1751 0.242 Uiso 1 1 calc R . . . . H18B H 0.7230 0.4725 0.1257 0.242 Uiso 1 1 calc R . . . . C19 C 0.827(3) 0.525(2) 0.199(2) 0.202(12) Uani 1 1 d D U . . . H19A H 0.8205 0.5718 0.1594 0.243 Uiso 1 1 calc R . . . . H19B H 0.8850 0.5018 0.2018 0.243 Uiso 1 1 calc R . . . . C20 C 0.806(2) 0.551(2) 0.284(2) 0.173(9) Uani 1 1 d D U . . . H20A H 0.8329 0.5122 0.3262 0.207 Uiso 1 1 calc R . . . . H20B H 0.8277 0.6074 0.2972 0.207 Uiso 1 1 calc R . . . . O1 O 0.541(4) 0.757(3) 0.439(3) 0.171(11) Uani 0.43(4) 1 d D U P A 1 C0AA C 0.589(4) 0.807(4) 0.509(3) 0.169(12) Uani 0.43(4) 1 d D U P A 1 H0AA H 0.6183 0.7708 0.5524 0.203 Uiso 0.43(4) 1 calc R . P A 1 H0AB H 0.6314 0.8444 0.4888 0.203 Uiso 0.43(4) 1 calc R . P A 1 C1AA C 0.524(6) 0.854(4) 0.540(3) 0.177(12) Uani 0.43(4) 1 d D U P A 1 H1AA H 0.5478 0.8985 0.5779 0.213 Uiso 0.43(4) 1 calc R . P A 1 H1AB H 0.4860 0.8184 0.5684 0.213 Uiso 0.43(4) 1 calc R . P A 1 C7AA C 0.481(6) 0.887(4) 0.465(4) 0.174(13) Uani 0.43(4) 1 d D U P A 1 H7AA H 0.4256 0.9125 0.4743 0.209 Uiso 0.43(4) 1 calc R . P A 1 H7AB H 0.5158 0.9292 0.4417 0.209 Uiso 0.43(4) 1 calc R . P A 1 C8AA C 0.468(5) 0.817(4) 0.413(5) 0.175(12) Uani 0.43(4) 1 d D U P A 1 H8AA H 0.4670 0.8339 0.3552 0.210 Uiso 0.43(4) 1 calc R . P A 1 H8AB H 0.4123 0.7907 0.4195 0.210 Uiso 0.43(4) 1 calc R . P A 1 C9A C 0.470(4) 0.834(3) 0.375(3) 0.155(11) Uani 0.57(4) 1 d D U P A 2 H9AA H 0.4931 0.8533 0.3256 0.186 Uiso 0.57(4) 1 calc R . P A 2 H9AB H 0.4087 0.8209 0.3605 0.186 Uiso 0.57(4) 1 calc R . P A 2 O1A O 0.518(3) 0.758(2) 0.411(2) 0.162(9) Uani 0.57(4) 1 d D U P A 2 C1A C 0.511(5) 0.773(3) 0.502(2) 0.170(10) Uani 0.57(4) 1 d D U P A 2 H1AC H 0.4549 0.7538 0.5157 0.203 Uiso 0.57(4) 1 calc R . P A 2 H1AD H 0.5566 0.7439 0.5376 0.203 Uiso 0.57(4) 1 calc R . P A 2 C2A C 0.519(5) 0.859(3) 0.511(3) 0.177(12) Uani 0.57(4) 1 d D U P A 2 H2AA H 0.4903 0.8786 0.5576 0.212 Uiso 0.57(4) 1 calc R . P A 2 H2AB H 0.5798 0.8751 0.5214 0.212 Uiso 0.57(4) 1 calc R . P A 2 C7A C 0.480(5) 0.896(3) 0.437(3) 0.162(12) Uani 0.57(4) 1 d D U P A 2 H7AC H 0.5168 0.9408 0.4205 0.194 Uiso 0.57(4) 1 calc R . P A 2 H7AD H 0.4245 0.9192 0.4450 0.194 Uiso 0.57(4) 1 calc R . P A 2 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 U1 0.0699(4) 0.1101(6) 0.0740(4) 0.0109(3) 0.0015(3) 0.0143(3) K1 0.156(5) 0.145(5) 0.155(5) -0.051(4) 0.030(4) 0.000(4) Si3 0.181(7) 0.096(4) 0.089(3) 0.030(3) 0.005(4) 0.004(4) Si1 0.147(5) 0.103(4) 0.106(4) -0.016(3) 0.038(4) 0.023(4) Si4 0.164(6) 0.135(5) 0.099(4) -0.032(4) -0.021(4) -0.019(5) Si2 0.159(6) 0.126(5) 0.131(5) 0.001(4) 0.066(5) -0.041(5) C4 0.097(8) 0.079(6) 0.069(6) 0.005(4) 0.007(5) 0.012(6) C2 0.089(7) 0.077(6) 0.080(6) 0.002(5) 0.019(6) 0.013(6) C1 0.100(8) 0.079(6) 0.072(6) 0.006(5) 0.013(6) 0.011(5) C3 0.097(8) 0.087(6) 0.076(6) 0.001(5) 0.009(5) 0.010(6) C15 0.200(12) 0.16(2) 0.160(19) 0.076(16) -0.002(11) 0.032(12) C10 0.21(2) 0.113(9) 0.23(3) 0.013(11) 0.07(2) -0.039(11) C6 0.21(2) 0.24(2) 0.104(8) -0.027(10) 0.043(10) 0.07(2) C14 0.24(2) 0.18(2) 0.116(12) 0.056(11) 0.044(13) 0.024(17) B2 0.117(8) 0.165(15) 0.130(14) 0.014(11) 0.028(9) -0.008(10) C7 0.166(11) 0.152(19) 0.149(16) -0.007(15) 0.044(11) 0.059(10) B1 0.148(18) 0.123(10) 0.144(18) 0.022(11) 0.025(15) 0.061(11) B3 0.134(17) 0.19(2) 0.086(8) 0.005(10) -0.010(8) 0.024(15) C12 0.26(3) 0.125(9) 0.21(2) -0.040(10) -0.02(2) -0.012(13) C8 0.27(2) 0.22(2) 0.167(11) -0.004(13) 0.121(12) -0.07(2) C16 0.30(2) 0.139(14) 0.19(2) 0.032(12) -0.011(19) -0.062(16) C11 0.179(11) 0.20(2) 0.21(2) -0.054(18) -0.039(12) -0.029(12) C13 0.34(3) 0.20(2) 0.108(10) -0.045(11) 0.021(15) -0.06(2) C9 0.162(10) 0.18(2) 0.28(2) 0.005(19) 0.092(12) -0.039(11) C5 0.26(2) 0.125(10) 0.25(2) -0.056(11) 0.11(2) -0.014(13) O2 0.148(9) 0.155(12) 0.187(15) -0.082(11) 0.034(11) -0.021(9) C17 0.211(19) 0.171(14) 0.24(2) -0.098(15) 0.084(18) -0.031(13) C18 0.21(2) 0.20(2) 0.21(2) -0.085(17) 0.071(18) -0.009(16) C19 0.20(2) 0.22(3) 0.20(2) -0.060(17) 0.066(17) -0.015(16) C20 0.162(11) 0.17(2) 0.189(19) -0.050(15) 0.045(13) -0.009(12) O1 0.22(2) 0.161(16) 0.14(2) -0.021(14) 0.043(17) 0.042(14) C0AA 0.24(2) 0.15(2) 0.13(2) -0.015(14) 0.038(19) 0.043(16) C1AA 0.25(3) 0.16(2) 0.13(2) -0.011(15) 0.041(19) 0.052(19) C7AA 0.24(2) 0.165(17) 0.13(2) -0.011(16) 0.04(2) 0.052(16) C8AA 0.23(2) 0.170(19) 0.13(2) -0.016(16) 0.043(19) 0.050(15) C9A 0.20(2) 0.160(16) 0.109(17) 0.001(13) 0.050(18) 0.040(15) O1A 0.22(2) 0.158(14) 0.116(16) -0.003(11) 0.042(15) 0.045(12) C1A 0.24(3) 0.162(16) 0.114(16) -0.001(12) 0.045(16) 0.052(16) C2A 0.25(3) 0.164(17) 0.117(18) -0.003(13) 0.034(19) 0.050(16) C7A 0.22(3) 0.161(15) 0.108(19) -0.002(13) 0.05(2) 0.049(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -4.3638 13.4090 '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_3 C4 U1 B2 89.7(9) . C4 U1 B1 128.3(9) . C2 U1 C4 49.0(6) . C2 U1 C1 34.2(5) . C2 U1 C3 34.3(6) . C2 U1 B2 138.7(9) . C2 U1 B1 100.5(10) . C2 U1 B3 97.8(10) . C1 U1 C4 33.0(5) . C1 U1 C3 48.0(6) . C1 U1 B2 111.7(9) . C1 U1 B1 134.7(10) . C1 U1 B3 89.0(9) . C3 U1 C4 33.6(5) . C3 U1 B2 111.1(9) . C3 U1 B1 96.2(9) . B1 U1 B2 106.7(11) . B3 U1 C4 119.3(9) . B3 U1 C3 131.3(9) . B3 U1 B2 105.2(12) . B3 U1 B1 103.4(11) . B2 K1 B3 98.8(9) 3_666 O2 K1 B2 91.1(8) . O2 K1 B3 94.4(9) 3_666 O2 K1 O1 165.0(16) . O2 K1 O1A 167.3(12) . O1 K1 B2 102.9(15) . O1 K1 B3 88.8(15) 3_666 O1A K1 B2 93.0(14) . O1A K1 B3 96.8(11) 3_666 C4 Si3 C15 108.8(10) . C4 Si3 C14 111.5(10) . C15 Si3 C14 106.3(12) . C16 Si3 C4 114.4(10) . C16 Si3 C15 112.7(13) . C16 Si3 C14 102.7(13) . C1 Si1 C7 106.4(11) . C6 Si1 C1 117.8(12) . C6 Si1 C7 108.2(14) . C5 Si1 C1 117.3(12) . C5 Si1 C6 106.1(19) . C5 Si1 C7 99.2(18) . C3 Si4 C12 114.1(13) . C3 Si4 C11 102.7(13) . C12 Si4 C11 89.8(18) . C13 Si4 C3 115.7(14) . C13 Si4 C12 121(2) . C13 Si4 C11 108(2) . C10 Si2 C2 118.3(13) . C8 Si2 C2 118.8(13) . C8 Si2 C10 114.3(18) . C8 Si2 C9 83(2) . C9 Si2 C2 114.2(15) . C9 Si2 C10 101.2(17) . Si3 C4 U1 132.0(10) . C1 C4 U1 71.5(9) . C1 C4 Si3 135.2(13) . C1 C4 C3 89.4(13) . C3 C4 U1 72.1(10) . C3 C4 Si3 131.1(13) . Si2 C2 U1 126.2(9) . C1 C2 U1 74.4(11) . C1 C2 Si2 133.1(14) . C1 C2 C3 88.4(14) . C3 C2 U1 75.2(11) . C3 C2 Si2 134.7(14) . Si1 C1 U1 131.1(9) . C4 C1 U1 75.5(10) . C4 C1 Si1 131.4(13) . C4 C1 C2 91.9(14) . C2 C1 U1 71.3(10) . C2 C1 Si1 132.1(14) . Si4 C3 U1 126.8(10) . C4 C3 U1 74.3(11) . C4 C3 Si4 134.7(14) . C4 C3 C2 90.3(14) . C2 C3 U1 70.5(10) . C2 C3 Si4 132.7(15) . Si3 C15 H15A 109.5 . Si3 C15 H15B 109.5 . Si3 C15 H15C 109.5 . H15A C15 H15B 109.5 . H15A C15 H15C 109.5 . H15B C15 H15C 109.5 . Si2 C10 H10A 109.5 . Si2 C10 H10B 109.5 . Si2 C10 H10C 109.5 . H10A C10 H10B 109.5 . H10A C10 H10C 109.5 . H10B C10 H10C 109.5 . Si1 C6 H6A 109.5 . Si1 C6 H6B 109.5 . Si1 C6 H6C 109.5 . H6A C6 H6B 109.5 . H6A C6 H6C 109.5 . H6B C6 H6C 109.5 . Si3 C14 H14A 109.5 . Si3 C14 H14B 109.5 . Si3 C14 H14C 109.5 . H14A C14 H14B 109.5 . H14A C14 H14C 109.5 . H14B C14 H14C 109.5 . U1 B2 K1 123.3(13) . Si1 C7 H7A 109.5 . Si1 C7 H7B 109.5 . Si1 C7 H7C 109.5 . H7A C7 H7B 109.5 . H7A C7 H7C 109.5 . H7B C7 H7C 109.5 . U1 B3 K1 135.6(15) 3_666 Si4 C12 H12A 109.5 . Si4 C12 H12B 109.5 . Si4 C12 H12C 109.5 . H12A C12 H12B 109.5 . H12A C12 H12C 109.5 . H12B C12 H12C 109.5 . Si2 C8 H8A 109.5 . Si2 C8 H8B 109.5 . Si2 C8 H8C 109.5 . H8A C8 H8B 109.5 . H8A C8 H8C 109.5 . H8B C8 H8C 109.5 . Si3 C16 H16A 109.5 . Si3 C16 H16B 109.5 . Si3 C16 H16C 109.5 . H16A C16 H16B 109.5 . H16A C16 H16C 109.5 . H16B C16 H16C 109.5 . Si4 C11 H11A 109.5 . Si4 C11 H11B 109.5 . Si4 C11 H11C 109.5 . H11A C11 H11B 109.5 . H11A C11 H11C 109.5 . H11B C11 H11C 109.5 . Si4 C13 H13A 109.5 . Si4 C13 H13B 109.5 . Si4 C13 H13C 109.5 . H13A C13 H13B 109.5 . H13A C13 H13C 109.5 . H13B C13 H13C 109.5 . Si2 C9 H9A 109.5 . Si2 C9 H9B 109.5 . Si2 C9 H9C 109.5 . H9A C9 H9B 109.5 . H9A C9 H9C 109.5 . H9B C9 H9C 109.5 . Si1 C5 H5A 109.5 . Si1 C5 H5B 109.5 . Si1 C5 H5C 109.5 . H5A C5 H5B 109.5 . H5A C5 H5C 109.5 . H5B C5 H5C 109.5 . C17 O2 K1 129.8(19) . C20 O2 K1 131.8(16) . C20 O2 C17 95(3) . O2 C17 H17A 110.2 . O2 C17 H17B 110.2 . O2 C17 C18 107(2) . H17A C17 H17B 108.5 . C18 C17 H17A 110.2 . C18 C17 H17B 110.2 . C17 C18 H18A 111.4 . C17 C18 H18B 111.4 . H18A C18 H18B 109.2 . C19 C18 C17 102.1(18) . C19 C18 H18A 111.4 . C19 C18 H18B 111.4 . C18 C19 H19A 111.9 . C18 C19 H19B 111.9 . C18 C19 C20 99.1(19) . H19A C19 H19B 109.6 . C20 C19 H19A 111.9 . C20 C19 H19B 111.9 . O2 C20 C19 108(3) . O2 C20 H20A 110.2 . O2 C20 H20B 110.2 . C19 C20 H20A 110.2 . C19 C20 H20B 110.2 . H20A C20 H20B 108.5 . C0AA O1 K1 124(3) . C0AA O1 C8AA 99(3) . C8AA O1 K1 132(3) . O1 C0AA H0AA 111.0 . O1 C0AA H0AB 111.0 . H0AA C0AA H0AB 109.0 . C1AA C0AA O1 104(3) . C1AA C0AA H0AA 111.0 . C1AA C0AA H0AB 111.0 . C0AA C1AA H1AA 111.7 . C0AA C1AA H1AB 111.7 . C0AA C1AA C7AA 101(3) . H1AA C1AA H1AB 109.4 . C7AA C1AA H1AA 111.7 . C7AA C1AA H1AB 111.7 . C1AA C7AA H7AA 111.0 . C1AA C7AA H7AB 111.0 . H7AA C7AA H7AB 109.0 . C8AA C7AA C1AA 104(3) . C8AA C7AA H7AA 111.0 . C8AA C7AA H7AB 111.0 . O1 C8AA H8AA 110.3 . O1 C8AA H8AB 110.3 . C7AA C8AA O1 107(3) . C7AA C8AA H8AA 110.3 . C7AA C8AA H8AB 110.3 . H8AA C8AA H8AB 108.5 . H9AA C9A H9AB 108.6 . O1A C9A H9AA 110.4 . O1A C9A H9AB 110.4 . C7A C9A H9AA 110.4 . C7A C9A H9AB 110.4 . C7A C9A O1A 107(3) . C9A O1A K1 136(2) . C9A O1A C1A 98(3) . C1A O1A K1 124(2) . O1A C1A H1AC 111.0 . O1A C1A H1AD 111.0 . H1AC C1A H1AD 109.0 . C2A C1A O1A 104(3) . C2A C1A H1AC 111.0 . C2A C1A H1AD 111.0 . C1A C2A H2AA 110.2 . C1A C2A H2AB 110.2 . H2AA C2A H2AB 108.5 . C7A C2A C1A 107(3) . C7A C2A H2AA 110.2 . C7A C2A H2AB 110.2 . C9A C7A H7AC 109.9 . C9A C7A H7AD 109.9 . C2A C7A C9A 109(2) . C2A C7A H7AC 110.0 . C2A C7A H7AD 109.9 . H7AC C7A H7AD 108.3 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 U1 C4 2.557(16) . U1 C2 2.464(19) . U1 C1 2.505(19) . U1 C3 2.53(2) . U1 B2 2.62(3) . U1 B1 2.56(3) . U1 B3 2.52(3) . K1 B2 3.13(4) . K1 B3 3.36(3) 3_666 K1 O2 2.58(2) . K1 O1 2.63(3) . K1 O1A 2.61(2) . Si3 C4 1.835(15) . Si3 C15 1.85(2) . Si3 C14 1.86(2) . Si3 C16 1.83(2) . Si1 C1 1.858(19) . Si1 C6 1.84(3) . Si1 C7 1.91(3) . Si1 C5 1.73(3) . Si4 C3 1.845(19) . Si4 C12 1.85(4) . Si4 C11 1.85(4) . Si4 C13 1.70(4) . Si2 C2 1.84(2) . Si2 C10 1.81(3) . Si2 C8 1.75(3) . Si2 C9 1.76(4) . C4 C1 1.44(2) . C4 C3 1.47(2) . C2 C1 1.46(2) . C2 C3 1.47(3) . C15 H15A 0.9600 . C15 H15B 0.9600 . C15 H15C 0.9600 . C10 H10A 0.9600 . C10 H10B 0.9600 . C10 H10C 0.9600 . C6 H6A 0.9600 . C6 H6B 0.9600 . C6 H6C 0.9600 . C14 H14A 0.9600 . C14 H14B 0.9600 . C14 H14C 0.9600 . C7 H7A 0.9600 . C7 H7B 0.9600 . C7 H7C 0.9600 . B3 K1 3.36(3) 3_666 C12 H12A 0.9600 . C12 H12B 0.9600 . C12 H12C 0.9600 . C8 H8A 0.9600 . C8 H8B 0.9600 . C8 H8C 0.9600 . C16 H16A 0.9600 . C16 H16B 0.9600 . C16 H16C 0.9600 . C11 H11A 0.9600 . C11 H11B 0.9600 . C11 H11C 0.9600 . C13 H13A 0.9600 . C13 H13B 0.9600 . C13 H13C 0.9600 . C9 H9A 0.9600 . C9 H9B 0.9600 . C9 H9C 0.9600 . C5 H5A 0.9600 . C5 H5B 0.9600 . C5 H5C 0.9600 . O2 C17 1.39(2) . O2 C20 1.37(3) . C17 H17A 0.9700 . C17 H17B 0.9700 . C17 C18 1.49(3) . C18 H18A 0.9700 . C18 H18B 0.9700 . C18 C19 1.48(3) . C19 H19A 0.9700 . C19 H19B 0.9700 . C19 C20 1.49(3) . C20 H20A 0.9700 . C20 H20B 0.9700 . O1 C0AA 1.49(3) . O1 C8AA 1.50(3) . C0AA H0AA 0.9700 . C0AA H0AB 0.9700 . C0AA C1AA 1.39(3) . C1AA H1AA 0.9700 . C1AA H1AB 0.9700 . C1AA C7AA 1.40(3) . C7AA H7AA 0.9700 . C7AA H7AB 0.9700 . C7AA C8AA 1.38(3) . C8AA H8AA 0.9700 . C8AA H8AB 0.9700 . C9A H9AA 0.9700 . C9A H9AB 0.9700 . C9A O1A 1.49(3) . C9A C7A 1.38(3) . O1A C1A 1.50(3) . C1A H1AC 0.9700 . C1A H1AD 0.9700 . C1A C2A 1.38(3) . C2A H2AA 0.9700 . C2A H2AB 0.9700 . C2A C7A 1.38(3) . C7A H7AC 0.9700 . C7A H7AD 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 U1 C4 C1 Si1 132.6(18) U1 C4 C1 C2 -70.2(10) U1 C4 C3 Si4 -127(2) U1 C4 C3 C2 69.6(10) U1 C2 C1 Si1 -129.0(16) U1 C2 C1 C4 74.0(11) U1 C2 C3 Si4 122.5(18) U1 C2 C3 C4 -73.2(11) K1 O2 C17 C18 151(3) K1 O2 C20 C19 -147(2) K1 O1 C0AA C1AA -174(5) K1 O1 C8AA C7AA -154(6) K1 O1A C1A C2A 135(5) Si3 C4 C1 U1 -131.6(18) Si3 C4 C1 Si1 1(3) Si3 C4 C1 C2 158.3(18) Si3 C4 C3 U1 130.6(17) Si3 C4 C3 Si4 4(3) Si3 C4 C3 C2 -159.8(16) Si2 C2 C1 U1 125.3(18) Si2 C2 C1 Si1 -4(3) Si2 C2 C1 C4 -160.7(17) Si2 C2 C3 U1 -126.7(18) Si2 C2 C3 Si4 -4(3) Si2 C2 C3 C4 160.1(17) C1 C4 C3 U1 -70.7(10) C1 C4 C3 Si4 162.6(19) C1 C4 C3 C2 -1.1(15) C1 C2 C3 U1 74.3(11) C1 C2 C3 Si4 -163.2(18) C1 C2 C3 C4 1.1(15) C3 C4 C1 U1 71.3(10) C3 C4 C1 Si1 -156.1(17) C3 C4 C1 C2 1.1(15) C3 C2 C1 U1 -75.1(11) C3 C2 C1 Si1 155.9(17) C3 C2 C1 C4 -1.1(15) C15 Si3 C4 U1 177.3(13) C15 Si3 C4 C1 -75(2) C15 Si3 C4 C3 74(2) C10 Si2 C2 U1 -64.7(19) C10 Si2 C2 C1 -168(2) C10 Si2 C2 C3 41(3) C6 Si1 C1 U1 -53(2) C6 Si1 C1 C4 -162(2) C6 Si1 C1 C2 50(3) C14 Si3 C4 U1 60.4(16) C14 Si3 C4 C1 168(2) C14 Si3 C4 C3 -43(2) C7 Si1 C1 U1 -174.1(13) C7 Si1 C1 C4 77(2) C7 Si1 C1 C2 -72(2) C12 Si4 C3 U1 57(2) C12 Si4 C3 C4 162(2) C12 Si4 C3 C2 -40(3) C8 Si2 C2 U1 81(2) C8 Si2 C2 C1 -22(3) C8 Si2 C2 C3 -172(2) C16 Si3 C4 U1 -55.6(17) C16 Si3 C4 C1 52(2) C16 Si3 C4 C3 -159(2) C11 Si4 C3 U1 152.5(16) C11 Si4 C3 C4 -102(2) C11 Si4 C3 C2 56(2) C13 Si4 C3 U1 -90(2) C13 Si4 C3 C4 15(3) C13 Si4 C3 C2 173(2) C9 Si2 C2 U1 176.3(16) C9 Si2 C2 C1 73(2) C9 Si2 C2 C3 -78(2) C5 Si1 C1 U1 76(2) C5 Si1 C1 C4 -33(3) C5 Si1 C1 C2 178(2) O2 C17 C18 C19 27(5) C17 O2 C20 C19 53(4) C17 C18 C19 C20 5(4) C18 C19 C20 O2 -37(4) C20 O2 C17 C18 -48(4) O1 C0AA C1AA C7AA -49(6) C0AA O1 C8AA C7AA 0(7) C0AA C1AA C7AA C8AA 49(7) C1AA C7AA C8AA O1 -30(8) C8AA O1 C0AA C1AA 30(7) C9A O1A C1A C2A -38(6) O1A C9A C7A C2A -9(7) O1A C1A C2A C7A 34(7) C1A C2A C7A C9A -16(8) C7A C9A O1A K1 -143(5) C7A C9A O1A C1A 28(6) loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.5120(19) 31558 730 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.4880(19) 31233 730 nmt 0.9936 0.0216 -0.0384 -0.0674 0.9621 -0.2662 0.0293 0.2664 0.9688