# Electronic Supplementary Material (ESI) for Catalysis Science & Technology. # This journal is © The Royal Society of Chemistry 2024 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_yyk_crii_20230721_auto _database_code_depnum_ccdc_archive 'CCDC 2286290' loop_ _audit_author_name _audit_author_address 'Yuya Kakiuchi' ;ETH Zurich Switzerland ; _audit_update_record ; 2023-08-02 deposited with the CCDC. 2024-05-20 downloaded from the CCDC. ; _audit_creation_date 2023-07-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic Cr(OSi(tBu)3)2(XyNC)4 _chemical_formula_moiety 'C60 H90 Cr N4 O8 Si2' _chemical_formula_sum 'C60 H90 Cr N4 O8 Si2' _chemical_formula_weight 1103.53 _chemical_melting_point ? _chemical_oxdiff_formula CrNCHOSi _chemical_oxdiff_usercomment 'recry pentane' 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' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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' _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. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3465(2) _cell_length_b 12.5357(2) _cell_length_c 13.0549(2) _cell_angle_alpha 109.944(2) _cell_angle_beta 101.7450(10) _cell_angle_gamma 105.8320(10) _cell_volume 1586.41(5) _cell_formula_units_Z 1 _cell_measurement_reflns_used 15182 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 79.5210 _cell_measurement_theta_min 3.8010 _shelx_estimated_absorpt_T_max 0.895 _shelx_estimated_absorpt_T_min 0.661 _exptl_absorpt_coefficient_mu 2.258 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.76272 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour red _exptl_crystal_colour_lustre . _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 594 _exptl_crystal_preparation 'recrystallization from pentane' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: n-pentane' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_unetI/netI 0.0263 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 24416 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.975 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.269 _diffrn_reflns_theta_min 3.813 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.975 _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 -69.00 -40.00 0.50 0.58 -- -49.60 89.00 27.00 58 2 \w -37.00 20.00 0.50 0.58 -- -49.60 89.00 27.00 114 3 \w -18.00 65.00 0.50 0.58 -- 49.60 -89.00 -88.00 166 4 \w -73.00 -48.00 0.50 2.32 -- -90.00 89.00 27.00 50 5 \w -144.00-119.00 0.50 2.32 -- -90.00 -89.00 -88.00 50 6 \w 60.00 87.00 0.50 2.32 -- 111.50 -89.00 -88.00 54 7 \w -11.00 24.00 0.50 0.58 -- -49.60 19.00 120.00 70 8 \w -114.00 -74.00 0.50 0.58 -- -49.60-125.00 30.00 80 9 \w -26.00 3.00 0.50 0.58 -- -49.60 19.00-180.00 58 10 \w -108.00 -76.00 0.50 0.58 -- -49.60-125.00 -30.00 64 11 \w -26.00 -1.00 0.50 0.58 -- -49.60 19.00 60.00 50 12 \w 49.00 76.00 0.50 0.58 -- 49.60 38.00 60.00 54 13 \w -22.00 26.00 0.50 0.58 -- 49.60 -19.00 0.00 96 14 \w -20.00 60.00 0.50 0.58 -- 49.60 -57.00 -60.00 160 15 \w 92.00 117.00 0.50 0.58 -- 49.60 38.00 60.00 50 16 \w -50.00 -22.00 0.50 2.32 -- -90.00 45.00-120.00 56 17 \w -48.00 -18.00 0.50 2.32 -- -90.00 45.00 -30.00 60 18 \w -145.00-119.00 0.50 2.32 -- -90.00 -45.00 120.00 52 19 \w -50.00 -18.00 0.50 2.32 -- -90.00 45.00-150.00 64 20 \w 104.00 166.00 0.50 2.32 -- 111.50 15.00 0.00 124 21 \w 54.00 105.00 0.50 2.32 -- 111.50 -95.00-120.00 102 22 \w 77.00 111.00 0.50 2.32 -- 111.50-125.00-180.00 68 23 \w 44.00 70.00 0.50 2.32 -- 111.50 -61.00 90.00 52 24 \w 136.00 162.00 0.50 2.32 -- 111.50 125.00 150.00 52 25 \w 43.00 68.00 0.50 2.32 -- 111.50-125.00-180.00 50 26 \w 41.00 71.00 0.50 2.32 -- 111.50 -61.00 60.00 60 27 \w 109.00 176.00 0.50 2.32 -- 111.50 45.00 -90.00 134 28 \w 43.00 69.00 0.50 2.32 -- 111.50 -61.00 120.00 52 29 \w 108.00 134.00 0.50 2.32 -- 111.50 30.00-120.00 52 30 \w 45.00 70.00 0.50 2.32 -- 111.50-125.00-150.00 50 31 \w 44.00 71.00 0.50 2.32 -- 111.50 -61.00 -60.00 54 32 \w 112.00 167.00 0.50 2.32 -- 111.50 30.00 30.00 110 33 \w 42.00 104.00 0.50 2.32 -- 111.50 -95.00 -60.00 124 34 \w 43.00 95.00 0.50 2.32 -- 111.50 -95.00 60.00 104 35 \w 44.00 71.00 0.50 2.32 -- 111.50 -61.00-150.00 54 36 \w 49.00 105.00 0.50 2.32 -- 111.50 -95.00 30.00 112 37 \w 48.00 77.00 0.50 2.32 -- 111.50-125.00 150.00 58 38 \w 109.00 149.00 0.50 2.32 -- 111.50 125.00-150.00 80 39 \w 53.00 108.00 0.50 2.32 -- 111.50-109.00-130.90 110 40 \w 77.00 103.00 0.50 2.32 -- 111.50 -95.00 150.00 52 41 \w 51.00 105.00 0.50 2.32 -- 111.50 -96.00 -25.36 108 42 \w 41.00 67.00 0.50 2.32 -- 111.50 -95.00 150.00 52 43 \w 41.00 89.00 0.50 2.32 -- 111.50 -95.00-180.00 96 44 \w 41.00 71.00 0.50 2.32 -- 111.50 -61.00 -30.00 60 45 \w 106.00 175.00 0.50 2.32 -- 111.50 30.00-150.00 138 46 \w 86.00 111.00 0.50 2.32 -- 111.50-125.00 150.00 50 47 \w 114.00 140.00 0.50 2.32 -- 111.50 15.00 120.00 52 48 \w 75.00 100.00 0.50 2.32 -- 111.50 -95.00 -90.00 50 49 \w 80.00 105.00 0.50 2.32 -- 111.50 -95.00 0.00 50 50 \w 52.00 78.00 0.50 2.32 -- 111.50 -95.00 0.00 52 51 \w 54.00 100.00 0.50 2.32 -- 111.50 -95.00-150.00 92 52 \w 77.00 105.00 0.50 2.32 -- 111.50 -95.00 90.00 56 53 \w 113.00 175.00 0.50 2.32 -- 111.50 15.00 -30.00 124 54 \w 138.00 172.00 0.50 2.32 -- 111.50 30.00-120.00 68 55 \w 105.00 175.00 0.50 2.32 -- 111.50 89.00 27.00 140 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0497757000 _diffrn_orient_matrix_UB_12 -0.0208463000 _diffrn_orient_matrix_UB_13 -0.1037793000 _diffrn_orient_matrix_UB_21 0.0988201000 _diffrn_orient_matrix_UB_22 0.1326897000 _diffrn_orient_matrix_UB_23 0.0610375000 _diffrn_orient_matrix_UB_31 0.1003737000 _diffrn_orient_matrix_UB_32 -0.0423489000 _diffrn_orient_matrix_UB_33 0.0562395000 _diffrn_oxdiff_digest_frames ; 01f83ef9ae2eb155e55d108397d7d6912f000311194 ; _diffrn_oxdiff_digest_hkl ; 015c58ec8883bba03244b94f5b8a078ed4111a ; _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6592 _reflns_number_total 6771 _reflns_odcompleteness_completeness 99.60 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)' _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)' _refine_diff_density_max 0.328 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.053 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 520 _refine_ls_number_reflns 6771 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0322 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1089 _refine_ls_wR_factor_ref 0.1118 _refine_special_details ? _olex2_refinement_description ; ; _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Cr01 Cr 0.500000 0.500000 0.500000 0.01321(9) Uani 1 2 d S T P . . Si02 Si 0.43773(3) 0.25102(3) 0.25269(2) 0.01685(10) Uani 1 1 d . . . . . O003 O 0.50150(8) 0.37388(7) 0.36521(7) 0.01923(17) Uani 1 1 d . . . . . O004 O 0.32966(8) 0.26448(8) 0.15784(7) 0.02206(18) Uani 1 1 d . . . . . O005 O 0.54720(8) 0.21535(8) 0.19786(7) 0.02138(18) Uani 1 1 d . . . . . O006 O 0.35729(8) 0.13109(8) 0.26862(7) 0.02304(18) Uani 1 1 d . . . . . N007 N 0.25676(10) 0.31019(9) 0.51222(9) 0.0205(2) Uani 1 1 d . . . . . N008 N 0.30674(10) 0.55688(9) 0.33103(9) 0.0210(2) Uani 1 1 d . . . . . C009 C 0.34700(11) 0.37901(10) 0.50897(9) 0.0176(2) Uani 1 1 d . . . . . C00A C 0.37623(11) 0.53671(10) 0.39462(10) 0.0183(2) Uani 1 1 d . . . . . C00B C 0.23824(11) 0.58658(10) 0.25047(10) 0.0203(2) Uani 1 1 d . . . . . C00C C 0.12431(12) 0.60462(11) 0.26114(10) 0.0231(2) Uani 1 1 d . . . . . C00D C 0.28736(12) 0.59641(12) 0.16251(11) 0.0263(3) Uani 1 1 d . . . . . C00E C 0.67360(12) 0.29496(12) 0.21322(10) 0.0224(2) Uani 1 1 d . . . . . C00F C 0.10535(12) 0.20178(11) 0.58175(11) 0.0239(2) Uani 1 1 d . . . . . C00G C 0.39997(12) 0.05999(11) 0.32326(11) 0.0250(3) Uani 1 1 d . . . . . C00H C 0.13150(11) 0.23300(10) 0.49325(11) 0.0204(2) Uani 1 1 d . . . . . C00I C 0.25246(13) 0.18406(13) 0.03951(10) 0.0275(3) Uani 1 1 d . . . . . C00J C 0.03798(12) 0.19143(11) 0.38550(11) 0.0235(2) Uani 1 1 d . . . . . C00K C -0.08722(12) 0.11689(12) 0.36864(12) 0.0278(3) Uani 1 1 d . . . . . C00L C -0.02187(13) 0.12905(13) 0.56110(13) 0.0296(3) Uani 1 1 d . . . . . C00M C 0.66616(13) 0.40514(13) 0.19052(12) 0.0276(3) Uani 1 1 d . . . . . C00N C -0.11696(12) 0.08749(12) 0.45629(14) 0.0311(3) Uani 1 1 d . . . . . C00O C 0.07752(15) 0.59293(15) 0.35798(13) 0.0325(3) Uani 1 1 d . . . . . C00P C 0.21050(14) 0.24386(14) 0.69377(13) 0.0308(3) Uani 1 1 d . . . . . C00Q C 0.07286(14) 0.22682(13) 0.29342(12) 0.0299(3) Uani 1 1 d . . . . . C00R C 0.21752(15) 0.62624(14) 0.08323(12) 0.0320(3) Uani 1 1 d . . . . . C00S C 0.50568(14) 0.14301(13) 0.43954(13) 0.0319(3) Uani 1 1 d . . . . . C00T C 0.05822(13) 0.63448(13) 0.17924(12) 0.0292(3) Uani 1 1 d . . . . . C00U C 0.76255(13) 0.33770(14) 0.33598(12) 0.0285(3) Uani 1 1 d . . . . . C00V C 0.72128(15) 0.21771(15) 0.12558(13) 0.0332(3) Uani 1 1 d . . . . . C00W C 0.14737(15) 0.23359(15) 0.01030(13) 0.0360(3) Uani 1 1 d . . . . . C00X C 0.27997(15) -0.01275(14) 0.34033(14) 0.0359(3) Uani 1 1 d . . . . . C00Y C 0.10441(15) 0.64531(13) 0.09169(12) 0.0331(3) Uani 1 1 d . . . . . C00Z C 0.44832(19) -0.02616(15) 0.24409(16) 0.0401(4) Uani 1 1 d . . . . . C010 C 0.18951(15) 0.05307(14) 0.02448(13) 0.0363(3) Uani 1 1 d . . . . . C011 C 0.41058(15) 0.57558(18) 0.15669(15) 0.0389(3) Uani 1 1 d . . . . . C012 C 0.33688(16) 0.18905(19) -0.03685(12) 0.0424(4) Uani 1 1 d . . . . . H00P H 0.584(2) 0.191(2) 0.4273(18) 0.045(5) Uiso 1 1 d . . . . . H00A H 0.6055(19) 0.3776(18) 0.1121(17) 0.037(5) Uiso 1 1 d . . . . . H00B H 0.6326(18) 0.4510(17) 0.2457(16) 0.033(4) Uiso 1 1 d . . . . . H00D H -0.001(2) 0.600(2) 0.3504(18) 0.046(5) Uiso 1 1 d . . . . . H00K H -0.1501(16) 0.0929(15) 0.2976(15) 0.024(4) Uiso 1 1 d . . . . . H00X H 0.807(2) 0.2643(19) 0.1285(17) 0.041(5) Uiso 1 1 d . . . . . H00J H -0.0006(19) 0.1956(18) 0.2293(17) 0.035(5) Uiso 1 1 d . . . . . H00N H -0.202(2) 0.0388(19) 0.4445(17) 0.042(5) Uiso 1 1 d . . . . . H00Y H 0.7204(19) 0.142(2) 0.1391(17) 0.041(5) Uiso 1 1 d . . . . . H00Q H 0.478(2) 0.202(2) 0.4898(19) 0.046(5) Uiso 1 1 d . . . . . H01A H 0.257(2) 0.014(2) 0.039(2) 0.056(6) Uiso 1 1 d . . . . . H00C H 0.7566(17) 0.4564(17) 0.2000(15) 0.028(4) Uiso 1 1 d . . . . . H0AA H 0.054(2) 0.663(2) 0.0343(18) 0.045(5) Uiso 1 1 d . . . . . H00T H -0.020(2) 0.6465(19) 0.1882(18) 0.040(5) Uiso 1 1 d . . . . . H00R H 0.2477(19) 0.6342(18) 0.0213(17) 0.038(5) Uiso 1 1 d . . . . . H H 0.669(2) 0.189(2) 0.049(2) 0.050(6) Uiso 1 1 d . . . . . H00Z H 0.088(2) 0.181(2) -0.0711(18) 0.045(5) Uiso 1 1 d . . . . . H1AA H 0.380(2) -0.076(2) 0.175(2) 0.049(6) Uiso 1 1 d . . . . . H00G H 0.274(2) 0.205(2) 0.6812(18) 0.044(5) Uiso 1 1 d . . . . . H00L H -0.039(2) 0.1073(19) 0.6191(18) 0.040(5) Uiso 1 1 d . . . . . H00U H 0.7635(19) 0.2702(19) 0.3518(17) 0.038(5) Uiso 1 1 d . . . . . H01G H 0.374(2) 0.270(2) -0.0322(18) 0.045(5) Uiso 1 1 d . . . . . H01H H 0.404(2) 0.159(2) -0.0160(19) 0.050(6) Uiso 1 1 d . . . . . H01I H 0.285(2) 0.142(2) -0.1165(19) 0.044(5) Uiso 1 1 d . . . . . H00 H 0.253(2) 0.051(2) 0.397(2) 0.057(6) Uiso 1 1 d . . . . . HA H 0.186(2) 0.317(2) 0.0170(18) 0.041(5) Uiso 1 1 d . . . . . H00S H 0.531(2) 0.094(2) 0.4771(18) 0.044(5) Uiso 1 1 d . . . . . HB H 0.301(2) -0.063(2) 0.3751(19) 0.049(6) Uiso 1 1 d . . . . . HC H 0.468(2) -0.080(2) 0.277(2) 0.054(6) Uiso 1 1 d . . . . . H00E H 0.132(2) 0.659(2) 0.432(2) 0.050(6) Uiso 1 1 d . . . . . HD H 0.092(2) 0.228(2) 0.0618(18) 0.043(5) Uiso 1 1 d . . . . . HE H 0.212(2) -0.065(2) 0.2645(19) 0.046(5) Uiso 1 1 d . . . . . H00M H 0.1079(19) 0.318(2) 0.3229(17) 0.041(5) Uiso 1 1 d . . . . . H01D H 0.483(2) 0.639(2) 0.221(2) 0.057(6) Uiso 1 1 d . . . . . H00F H 0.074(2) 0.520(2) 0.3606(19) 0.049(6) Uiso 1 1 d . . . . . H00V H 0.851(2) 0.389(2) 0.3448(17) 0.041(5) Uiso 1 1 d . . . . . H00H H 0.255(2) 0.332(2) 0.7297(19) 0.051(6) Uiso 1 1 d . . . . . H00O H 0.138(2) 0.201(2) 0.2732(19) 0.049(6) Uiso 1 1 d . . . . . H00W H 0.7314(18) 0.3877(18) 0.3939(16) 0.034(4) Uiso 1 1 d . . . . . H01B H 0.135(2) 0.005(2) -0.0520(19) 0.045(5) Uiso 1 1 d . . . . . H01C H 0.141(2) 0.045(2) 0.080(2) 0.051(6) Uiso 1 1 d . . . . . HF H 0.523(2) 0.018(2) 0.2308(18) 0.046(5) Uiso 1 1 d . . . . . H01E H 0.4089(19) 0.4955(19) 0.1600(17) 0.038(5) Uiso 1 1 d . . . . . H01F H 0.429(3) 0.581(3) 0.093(3) 0.074(8) Uiso 1 1 d . . . . . H00I H 0.179(2) 0.213(2) 0.749(2) 0.061(7) Uiso 1 1 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 Cr01 0.01304(14) 0.01446(14) 0.01219(13) 0.00570(10) 0.00434(9) 0.00494(10) Si02 0.01868(16) 0.01677(16) 0.01441(15) 0.00570(12) 0.00558(11) 0.00657(12) O003 0.0206(4) 0.0190(4) 0.0171(4) 0.0055(3) 0.0074(3) 0.0077(3) O004 0.0240(4) 0.0229(4) 0.0167(4) 0.0064(3) 0.0034(3) 0.0098(3) O005 0.0249(4) 0.0215(4) 0.0196(4) 0.0077(3) 0.0102(3) 0.0105(3) O006 0.0233(4) 0.0207(4) 0.0232(4) 0.0105(3) 0.0059(3) 0.0050(3) N007 0.0199(5) 0.0191(5) 0.0226(5) 0.0083(4) 0.0089(4) 0.0062(4) N008 0.0209(5) 0.0212(5) 0.0204(5) 0.0088(4) 0.0040(4) 0.0089(4) C009 0.0189(5) 0.0185(5) 0.0159(5) 0.0071(4) 0.0058(4) 0.0079(4) C00A 0.0188(5) 0.0172(5) 0.0186(5) 0.0066(4) 0.0083(4) 0.0059(4) C00B 0.0200(5) 0.0188(5) 0.0196(5) 0.0087(4) 0.0011(4) 0.0066(4) C00C 0.0219(5) 0.0210(5) 0.0235(6) 0.0083(5) 0.0033(4) 0.0086(4) C00D 0.0266(6) 0.0273(6) 0.0274(6) 0.0145(5) 0.0083(5) 0.0098(5) C00E 0.0232(5) 0.0275(6) 0.0238(5) 0.0131(5) 0.0130(4) 0.0132(5) C00F 0.0219(6) 0.0225(6) 0.0319(6) 0.0145(5) 0.0120(5) 0.0089(5) C00G 0.0296(6) 0.0202(5) 0.0272(6) 0.0127(5) 0.0097(5) 0.0081(5) C00H 0.0174(5) 0.0167(5) 0.0277(6) 0.0095(4) 0.0099(4) 0.0052(4) C00I 0.0269(6) 0.0316(7) 0.0172(5) 0.0057(5) 0.0011(5) 0.0113(5) C00J 0.0223(6) 0.0198(5) 0.0275(6) 0.0078(5) 0.0087(5) 0.0090(4) C00K 0.0202(6) 0.0226(6) 0.0358(7) 0.0097(5) 0.0052(5) 0.0073(5) C00L 0.0269(6) 0.0286(6) 0.0419(7) 0.0214(6) 0.0182(6) 0.0093(5) C00M 0.0290(6) 0.0313(6) 0.0308(6) 0.0184(5) 0.0149(5) 0.0129(5) C00N 0.0194(6) 0.0245(6) 0.0492(8) 0.0163(6) 0.0132(5) 0.0055(5) C00O 0.0314(7) 0.0419(8) 0.0371(7) 0.0218(6) 0.0170(6) 0.0217(6) C00P 0.0298(6) 0.0337(7) 0.0326(7) 0.0200(6) 0.0120(5) 0.0084(6) C00Q 0.0277(6) 0.0324(7) 0.0242(6) 0.0102(5) 0.0064(5) 0.0070(5) C00R 0.0411(8) 0.0338(7) 0.0272(6) 0.0181(6) 0.0113(6) 0.0159(6) C00S 0.0350(7) 0.0277(6) 0.0315(7) 0.0173(6) 0.0034(5) 0.0089(5) C00T 0.0261(6) 0.0306(6) 0.0302(6) 0.0120(5) 0.0026(5) 0.0153(5) C00U 0.0232(6) 0.0392(7) 0.0271(6) 0.0160(6) 0.0097(5) 0.0137(5) C00V 0.0386(8) 0.0463(8) 0.0308(7) 0.0192(6) 0.0223(6) 0.0276(7) C00W 0.0332(7) 0.0399(8) 0.0287(7) 0.0119(6) -0.0011(6) 0.0160(6) C00X 0.0354(7) 0.0294(7) 0.0438(8) 0.0218(6) 0.0139(6) 0.0046(6) C00Y 0.0405(7) 0.0327(7) 0.0273(6) 0.0155(6) 0.0016(5) 0.0189(6) C00Z 0.0587(10) 0.0280(7) 0.0453(9) 0.0179(7) 0.0274(8) 0.0224(7) C010 0.0380(7) 0.0282(7) 0.0254(6) 0.0012(5) -0.0027(6) 0.0098(6) C011 0.0335(7) 0.0571(10) 0.0439(8) 0.0314(8) 0.0218(7) 0.0233(7) C012 0.0369(8) 0.0645(11) 0.0196(6) 0.0127(7) 0.0072(6) 0.0176(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cr01 O003 1.9301(8) . ? Cr01 O003 1.9301(8) 2_666 ? Cr01 C009 2.0237(11) 2_666 ? Cr01 C009 2.0237(11) . ? Cr01 C00A 2.0186(12) 2_666 ? Cr01 C00A 2.0186(12) . ? Si02 O003 1.5714(8) . ? Si02 O004 1.6440(8) . ? Si02 O005 1.6436(9) . ? Si02 O006 1.6366(9) . ? O004 C00I 1.4405(14) . ? O005 C00E 1.4348(15) . ? O006 C00G 1.4376(14) . ? N007 C009 1.1640(16) . ? N007 C00H 1.4002(15) . ? N008 C00A 1.1664(16) . ? N008 C00B 1.3931(15) . ? C00B C00C 1.3976(17) . ? C00B C00D 1.4013(18) . ? C00C C00O 1.5029(19) . ? C00C C00T 1.3948(17) . ? C00D C00R 1.3895(18) . ? C00D C011 1.5026(19) . ? C00E C00M 1.5282(17) . ? C00E C00U 1.5279(17) . ? C00E C00V 1.5236(17) . ? C00F C00H 1.4002(17) . ? C00F C00L 1.3941(17) . ? C00F C00P 1.5034(19) . ? C00G C00S 1.5251(18) . ? C00G C00X 1.5231(19) . ? C00G C00Z 1.526(2) . ? C00H C00J 1.4024(17) . ? C00I C00W 1.5274(19) . ? C00I C010 1.526(2) . ? C00I C012 1.521(2) . ? C00J C00K 1.3956(18) . ? C00J C00Q 1.5034(18) . ? C00K C00N 1.391(2) . ? C00L C00N 1.383(2) . ? C00R C00Y 1.387(2) . ? C00T C00Y 1.382(2) . ? 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 O003 Cr01 O003 180.00(5) . 2_666 ? O003 Cr01 C009 89.28(4) 2_666 . ? O003 Cr01 C009 90.72(4) 2_666 2_666 ? O003 Cr01 C009 90.72(4) . . ? O003 Cr01 C009 89.28(4) . 2_666 ? O003 Cr01 C00A 88.57(4) . . ? O003 Cr01 C00A 88.57(4) 2_666 2_666 ? O003 Cr01 C00A 91.43(4) . 2_666 ? O003 Cr01 C00A 91.43(4) 2_666 . ? C009 Cr01 C009 180.0 2_666 . ? C00A Cr01 C009 90.46(4) . 2_666 ? C00A Cr01 C009 89.54(4) 2_666 2_666 ? C00A Cr01 C009 90.46(4) 2_666 . ? C00A Cr01 C009 89.54(4) . . ? C00A Cr01 C00A 180.00(5) . 2_666 ? O003 Si02 O004 109.19(4) . . ? O003 Si02 O005 111.36(5) . . ? O003 Si02 O006 115.41(5) . . ? O005 Si02 O004 110.18(4) . . ? O006 Si02 O004 104.59(5) . . ? O006 Si02 O005 105.82(5) . . ? Si02 O003 Cr01 154.26(5) . . ? C00I O004 Si02 131.74(8) . . ? C00E O005 Si02 128.28(7) . . ? C00G O006 Si02 131.67(8) . . ? C009 N007 C00H 165.29(12) . . ? C00A N008 C00B 172.16(12) . . ? N007 C009 Cr01 178.16(10) . . ? N008 C00A Cr01 177.74(10) . . ? N008 C00B C00C 118.54(11) . . ? N008 C00B C00D 118.03(11) . . ? C00C C00B C00D 123.43(11) . . ? C00B C00C C00O 120.55(11) . . ? C00T C00C C00B 117.09(12) . . ? C00T C00C C00O 122.35(12) . . ? C00B C00D C011 120.33(12) . . ? C00R C00D C00B 117.03(12) . . ? C00R C00D C011 122.64(13) . . ? O005 C00E C00M 110.75(10) . . ? O005 C00E C00U 109.40(10) . . ? O005 C00E C00V 105.36(11) . . ? C00U C00E C00M 110.05(11) . . ? C00V C00E C00M 110.52(11) . . ? C00V C00E C00U 110.67(11) . . ? C00H C00F C00P 121.32(11) . . ? C00L C00F C00H 117.20(12) . . ? C00L C00F C00P 121.48(12) . . ? O006 C00G C00S 110.69(10) . . ? O006 C00G C00X 105.01(11) . . ? O006 C00G C00Z 109.66(11) . . ? C00S C00G C00Z 110.86(13) . . ? C00X C00G C00S 110.13(12) . . ? C00X C00G C00Z 110.35(12) . . ? N007 C00H C00J 117.60(11) . . ? C00F C00H N007 119.04(11) . . ? C00F C00H C00J 123.36(11) . . ? O004 C00I C00W 105.32(11) . . ? O004 C00I C010 111.43(10) . . ? O004 C00I C012 109.46(11) . . ? C010 C00I C00W 109.58(12) . . ? C012 C00I C00W 110.50(13) . . ? C012 C00I C010 110.44(13) . . ? C00H C00J C00Q 120.73(11) . . ? C00K C00J C00H 117.04(12) . . ? C00K C00J C00Q 122.23(12) . . ? C00N C00K C00J 120.85(13) . . ? C00N C00L C00F 120.99(13) . . ? C00L C00N C00K 120.52(12) . . ? C00Y C00R C00D 121.00(13) . . ? C00Y C00T C00C 120.87(13) . . ? C00T C00Y C00R 120.58(12) . . ? _shelx_res_file ; TITL yyk_crii_20230721_auto_a.res in P-1 yyk_crii_20230721_auto.res created by SHELXL-2018/3 at 21:16:54 on 24-Jul-2023 REM Old TITL YYK_CrII_20230721_auto in P-1 REM SHELXT solution in P-1: R1 0.115, Rweak 0.011, Alpha 0.052 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C60 N4 O8 Si2 Cr CELL 1.54184 11.3465 12.5357 13.0549 109.944 101.745 105.832 ZERR 1 0.0002 0.0002 0.0002 0.002 0.001 0.001 LATT 1 SFAC C H Cr N O Si UNIT 60 90 1 4 8 2 L.S. 4 0 0 PLAN 20 SIZE 0.2 0.2 0.05 TEMP -173 BOND list 4 fmap 2 53 ACTA REM REM REM WGHT 0.100000 FVAR 0.75645 CR01 3 0.500000 0.500000 0.500000 10.50000 0.01304 0.01446 = 0.01219 0.00570 0.00434 0.00494 SI02 6 0.437734 0.251015 0.252687 11.00000 0.01868 0.01677 = 0.01441 0.00570 0.00558 0.00657 O003 5 0.501503 0.373880 0.365209 11.00000 0.02059 0.01896 = 0.01713 0.00547 0.00743 0.00768 O004 5 0.329662 0.264478 0.157844 11.00000 0.02402 0.02290 = 0.01668 0.00644 0.00339 0.00979 O005 5 0.547200 0.215349 0.197858 11.00000 0.02490 0.02149 = 0.01962 0.00769 0.01019 0.01048 O006 5 0.357287 0.131093 0.268622 11.00000 0.02331 0.02073 = 0.02316 0.01052 0.00592 0.00499 N007 4 0.256765 0.310186 0.512217 11.00000 0.01986 0.01906 = 0.02259 0.00832 0.00887 0.00624 N008 4 0.306737 0.556883 0.331025 11.00000 0.02089 0.02115 = 0.02038 0.00879 0.00404 0.00887 C009 1 0.346995 0.379014 0.508974 11.00000 0.01888 0.01852 = 0.01594 0.00712 0.00578 0.00786 C00A 1 0.376233 0.536713 0.394620 11.00000 0.01883 0.01719 = 0.01864 0.00664 0.00835 0.00585 C00B 1 0.238243 0.586582 0.250467 11.00000 0.01998 0.01878 = 0.01961 0.00871 0.00114 0.00656 C00C 1 0.124306 0.604616 0.261144 11.00000 0.02195 0.02102 = 0.02355 0.00827 0.00330 0.00858 C00D 1 0.287356 0.596405 0.162510 11.00000 0.02656 0.02732 = 0.02739 0.01454 0.00833 0.00978 C00E 1 0.673603 0.294958 0.213221 11.00000 0.02322 0.02752 = 0.02377 0.01310 0.01297 0.01322 C00F 1 0.105352 0.201779 0.581748 11.00000 0.02191 0.02250 = 0.03193 0.01450 0.01199 0.00887 C00G 1 0.399974 0.059987 0.323263 11.00000 0.02957 0.02023 = 0.02715 0.01272 0.00971 0.00809 C00H 1 0.131500 0.232996 0.493251 11.00000 0.01735 0.01667 = 0.02774 0.00951 0.00995 0.00523 C00I 1 0.252464 0.184063 0.039509 11.00000 0.02691 0.03162 = 0.01715 0.00575 0.00111 0.01125 C00J 1 0.037983 0.191430 0.385505 11.00000 0.02230 0.01976 = 0.02747 0.00777 0.00874 0.00897 C00K 1 -0.087220 0.116893 0.368639 11.00000 0.02024 0.02263 = 0.03581 0.00969 0.00516 0.00733 C00L 1 -0.021874 0.129054 0.561104 11.00000 0.02687 0.02856 = 0.04194 0.02138 0.01817 0.00927 C00M 1 0.666158 0.405139 0.190516 11.00000 0.02899 0.03133 = 0.03080 0.01841 0.01492 0.01289 C00N 1 -0.116957 0.087494 0.456288 11.00000 0.01937 0.02453 = 0.04924 0.01629 0.01317 0.00555 C00O 1 0.077517 0.592925 0.357979 11.00000 0.03145 0.04191 = 0.03708 0.02183 0.01704 0.02170 C00P 1 0.210496 0.243865 0.693770 11.00000 0.02979 0.03371 = 0.03263 0.01997 0.01199 0.00839 C00Q 1 0.072859 0.226821 0.293425 11.00000 0.02770 0.03238 = 0.02424 0.01021 0.00636 0.00697 C00R 1 0.217518 0.626238 0.083232 11.00000 0.04106 0.03378 = 0.02723 0.01810 0.01128 0.01594 C00S 1 0.505680 0.143011 0.439539 11.00000 0.03500 0.02767 = 0.03149 0.01727 0.00336 0.00892 C00T 1 0.058221 0.634480 0.179243 11.00000 0.02606 0.03057 = 0.03022 0.01202 0.00262 0.01528 C00U 1 0.762554 0.337702 0.335976 11.00000 0.02322 0.03921 = 0.02713 0.01603 0.00971 0.01373 C00V 1 0.721275 0.217705 0.125577 11.00000 0.03862 0.04628 = 0.03084 0.01920 0.02233 0.02759 C00W 1 0.147374 0.233591 0.010302 11.00000 0.03320 0.03988 = 0.02873 0.01187 -0.00110 0.01601 C00X 1 0.279968 -0.012753 0.340328 11.00000 0.03538 0.02940 = 0.04379 0.02179 0.01394 0.00457 C00Y 1 0.104406 0.645307 0.091691 11.00000 0.04046 0.03275 = 0.02731 0.01547 0.00163 0.01890 C00Z 1 0.448324 -0.026163 0.244088 11.00000 0.05868 0.02804 = 0.04528 0.01791 0.02739 0.02244 C010 1 0.189512 0.053073 0.024477 11.00000 0.03801 0.02824 = 0.02542 0.00119 -0.00273 0.00976 C011 1 0.410583 0.575577 0.156689 11.00000 0.03352 0.05710 = 0.04395 0.03144 0.02180 0.02331 C012 1 0.336880 0.189046 -0.036846 11.00000 0.03690 0.06453 = 0.01958 0.01273 0.00722 0.01757 H00P 2 0.583871 0.191400 0.427301 11.00000 0.04457 H00A 2 0.605539 0.377570 0.112059 11.00000 0.03727 H00B 2 0.632582 0.450974 0.245685 11.00000 0.03257 H00D 2 -0.001148 0.599967 0.350361 11.00000 0.04644 H00K 2 -0.150057 0.092870 0.297579 11.00000 0.02365 H00X 2 0.807437 0.264337 0.128502 11.00000 0.04070 H00J 2 -0.000559 0.195632 0.229273 11.00000 0.03494 H00N 2 -0.202104 0.038827 0.444462 11.00000 0.04219 H00Y 2 0.720427 0.141831 0.139124 11.00000 0.04053 H00Q 2 0.477656 0.202074 0.489833 11.00000 0.04618 H01A 2 0.257402 0.013761 0.038652 11.00000 0.05630 H00C 2 0.756599 0.456382 0.200034 11.00000 0.02848 H0AA 2 0.053931 0.662857 0.034295 11.00000 0.04481 H00T 2 -0.020397 0.646501 0.188166 11.00000 0.04014 H00R 2 0.247746 0.634232 0.021332 11.00000 0.03834 H 2 0.668666 0.188929 0.049030 11.00000 0.04980 H00Z 2 0.088363 0.181321 -0.071137 11.00000 0.04465 H1AA 2 0.380223 -0.076423 0.174573 11.00000 0.04880 H00G 2 0.273971 0.205488 0.681243 11.00000 0.04420 H00L 2 -0.038571 0.107295 0.619139 11.00000 0.03980 H00U 2 0.763454 0.270185 0.351802 11.00000 0.03774 H01G 2 0.373614 0.270144 -0.032210 11.00000 0.04467 H01H 2 0.403865 0.158967 -0.016019 11.00000 0.04974 H01I 2 0.285252 0.142322 -0.116470 11.00000 0.04443 H00 2 0.252855 0.050508 0.396550 11.00000 0.05697 HA 2 0.186345 0.316776 0.017022 11.00000 0.04104 H00S 2 0.530759 0.094323 0.477125 11.00000 0.04356 HB 2 0.300977 -0.063231 0.375142 11.00000 0.04932 HC 2 0.467861 -0.080403 0.276555 11.00000 0.05428 H00E 2 0.132047 0.659230 0.432352 11.00000 0.04996 HD 2 0.091667 0.227545 0.061797 11.00000 0.04296 HE 2 0.212251 -0.064793 0.264462 11.00000 0.04565 H00M 2 0.107918 0.317505 0.322918 11.00000 0.04116 H01D 2 0.482785 0.639406 0.220826 11.00000 0.05696 H00F 2 0.073914 0.519558 0.360595 11.00000 0.04913 H00V 2 0.851370 0.389015 0.344840 11.00000 0.04123 H00H 2 0.254514 0.331530 0.729727 11.00000 0.05117 H00O 2 0.137726 0.201102 0.273152 11.00000 0.04901 H00W 2 0.731428 0.387719 0.393934 11.00000 0.03392 H01B 2 0.134903 0.005024 -0.051958 11.00000 0.04452 H01C 2 0.140963 0.045152 0.079800 11.00000 0.05115 HF 2 0.523300 0.018362 0.230812 11.00000 0.04602 H01E 2 0.408913 0.495527 0.159970 11.00000 0.03772 H01F 2 0.429074 0.581401 0.093481 11.00000 0.07439 H00I 2 0.179398 0.213321 0.748634 11.00000 0.06053 HKLF 4 REM yyk_crii_20230721_auto_a.res in P-1 REM wR2 = 0.1118, GooF = S = 0.996, Restrained GooF = 0.996 for all data REM R1 = 0.0322 for 6592 Fo > 4sig(Fo) and 0.0336 for all 6771 data REM 520 parameters refined using 0 restraints END WGHT 0.0716 0.1697 REM Highest difference peak 0.328, deepest hole -0.519, 1-sigma level 0.053 Q1 1 0.4230 0.5208 0.4526 11.00000 0.05 0.33 Q2 1 0.0913 0.6215 0.2237 11.00000 0.05 0.32 Q3 1 0.3768 0.2583 0.1945 11.00000 0.05 0.29 Q4 1 0.1957 0.2047 0.0193 11.00000 0.05 0.28 Q5 1 0.2603 0.5842 0.2025 11.00000 0.05 0.27 Q6 1 0.1862 0.5963 0.2607 11.00000 0.05 0.27 Q7 1 0.3786 0.0988 0.2956 11.00000 0.05 0.26 Q8 1 0.2582 0.6137 0.1284 11.00000 0.05 0.24 Q9 1 0.3388 0.0274 0.3366 11.00000 0.05 0.24 Q10 1 0.0538 0.2134 0.3429 11.00000 0.05 0.23 Q11 1 0.4479 0.0943 0.3830 11.00000 0.05 0.23 Q12 1 0.3808 0.4563 0.4958 11.00000 0.05 0.23 Q13 1 0.0987 0.5993 0.3018 11.00000 0.05 0.23 Q14 1 -0.0553 0.0885 0.4934 11.00000 0.05 0.23 Q15 1 0.6633 0.3404 0.1970 11.00000 0.05 0.23 Q16 1 0.1139 0.2179 0.5374 11.00000 0.05 0.22 Q17 1 0.1679 0.6379 0.0975 11.00000 0.05 0.21 Q18 1 0.2672 0.5666 0.2799 11.00000 0.05 0.21 Q19 1 0.4283 0.0166 0.2829 11.00000 0.05 0.21 Q20 1 0.7221 0.3201 0.2776 11.00000 0.05 0.21 ; _shelx_res_checksum 9293 _olex2_exptl_crystal_mounting_method loop _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 1.319 _oxdiff_exptl_absorpt_empirical_full_min 0.835 _chemical_properties_physical Air-sensitive,Moisture-sensitive,Oxygen-sensitive ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_yyk190_croar2_xync2_auto _database_code_depnum_ccdc_archive 'CCDC 2286291' loop_ _audit_author_name _audit_author_address 'Yuya Kakiuchi' ;ETH Zurich Switzerland ; _audit_update_record ; 2023-08-02 deposited with the CCDC. 2024-05-20 downloaded from the CCDC. ; _audit_creation_date 2023-07-07 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic Cr(O(tBu)2C6H3)2(XyNC)2 _chemical_formula_moiety 'C46 H60 Cr N2 O2' _chemical_formula_sum 'C46 H60 Cr N2 O2' _chemical_formula_weight 724.96 _chemical_melting_point ? _chemical_oxdiff_formula CrNCHO _chemical_oxdiff_usercomment 'yellow needle-like plate, acetonitrile at -30 deg' 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' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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' _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. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' 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' _cell_length_a 10.9280(4) _cell_length_b 28.6868(10) _cell_length_c 14.0779(6) _cell_angle_alpha 90 _cell_angle_beta 110.037(5) _cell_angle_gamma 90 _cell_volume 4146.1(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 24728 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 78.5410 _cell_measurement_theta_min 2.9850 _shelx_estimated_absorpt_T_max 0.883 _shelx_estimated_absorpt_T_min 0.515 _exptl_absorpt_coefficient_mu 2.550 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.62029 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.61a (Rigaku Oxford Diffraction, 2022) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_lustre . _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1560 _exptl_crystal_preparation 'recrystallization from DCM' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: dichloromethane' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_unetI/netI 0.0292 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 61380 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.840 _diffrn_reflns_theta_min 3.081 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.985 _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 -82.00 -8.00 0.50 10.70 -- -49.62 113.00 114.00 148 2 \w 38.00 72.00 0.50 10.70 -- 49.62-113.00 23.00 68 3 \w -144.00-119.00 0.50 14.40 -- -90.00-113.00 23.00 50 4 \w -76.00 -51.00 0.50 14.40 -- -90.00 113.00 114.00 50 5 \w 79.00 108.00 0.50 14.40 -- 111.50-113.00 23.00 58 6 \w 103.00 155.00 0.50 14.40 -- 111.50 113.00 114.00 104 7 \w -115.00 -73.00 0.50 10.70 -- -49.62-125.00 120.00 84 8 \w -115.00 -75.00 0.50 10.70 -- -49.62-125.00 60.00 80 9 \w -117.00 -73.00 0.50 10.70 -- -49.62-125.00-150.00 88 10 \w -116.00 -76.00 0.50 10.70 -- -49.62-125.00-120.00 80 11 \w -43.00 22.00 0.50 10.70 -- -49.62 38.00 150.00 130 12 \w -19.00 62.00 0.50 10.70 -- 49.62 -57.00 -60.00 162 13 \w 52.00 78.00 0.50 10.70 -- 49.62 -99.00-150.00 52 14 \w 5.00 32.00 0.50 10.70 -- 49.62 -99.00-150.00 54 15 \w -47.00 -19.00 0.50 14.40 -- -90.00 45.00 -60.00 56 16 \w -46.00 -20.00 0.50 14.40 -- -90.00 45.00 60.00 52 17 \w -158.00-104.00 0.50 14.40 -- -90.00 -30.00 -90.00 108 18 \w 106.00 159.00 0.50 14.40 -- 111.50 125.00-180.00 106 19 \w 44.00 74.00 0.50 14.40 -- 111.50-125.00-180.00 60 20 \w 105.00 173.00 0.50 14.40 -- 111.50 30.00 120.00 136 21 \w 45.00 71.00 0.50 14.40 -- 111.50 -61.00 0.00 52 22 \w 73.00 108.00 0.50 14.40 -- 111.50-111.00 104.83 70 23 \w 74.00 104.00 0.50 14.40 -- 111.50 -95.00-180.00 60 24 \w 118.00 166.00 0.50 14.40 -- 111.50 30.00 90.00 96 25 \w 148.00 173.00 0.50 14.40 -- 111.50 30.00 -30.00 50 26 \w 119.00 177.00 0.50 14.40 -- 111.50 45.00 60.00 116 27 \w 111.00 137.00 0.50 14.40 -- 111.50 30.00 -30.00 52 28 \w 71.00 104.00 0.50 14.40 -- 111.50 -95.00-150.00 66 29 \w 42.00 74.00 0.50 14.40 -- 111.50 -77.00 0.00 64 30 \w 126.00 176.00 0.50 14.40 -- 111.50 30.00 30.00 100 31 \w 43.00 83.00 0.50 14.40 -- 111.50-125.00 150.00 80 32 \w 105.00 177.00 0.50 14.40 -- 111.50 45.00 -60.00 144 33 \w 77.00 102.00 0.50 14.40 -- 111.50 -95.00 150.00 50 34 \w 67.00 94.00 0.50 14.40 -- 111.50 -95.00 -30.00 54 35 \w 43.00 68.00 0.50 14.40 -- 111.50 -95.00-180.00 50 36 \w 75.00 103.00 0.50 14.40 -- 111.50 -95.00-120.00 56 37 \w 47.00 110.00 0.50 14.40 -- 111.50-125.00 -30.00 126 38 \w 43.00 68.00 0.50 14.40 -- 111.50 -61.00 150.00 50 39 \w 139.00 167.00 0.50 14.40 -- 111.50 30.00 -90.00 56 40 \w 56.00 95.00 0.50 14.40 -- 111.50-125.00 0.00 78 41 \w 71.00 103.00 0.50 14.40 -- 111.50 -95.00 0.00 64 42 \w 97.00 148.00 0.50 14.40 -- 111.50 61.00-150.00 102 43 \w 153.00 178.00 0.50 14.40 -- 111.50 61.00-150.00 50 44 \w 111.00 177.00 0.50 14.40 -- 111.50 15.00 0.00 132 45 \w 41.00 67.00 0.50 14.40 -- 111.50 -95.00 0.00 52 46 \w 104.00 130.00 0.50 14.40 -- 111.50 30.00 -90.00 52 47 \w 41.00 94.00 0.50 14.40 -- 111.50 -95.00 60.00 106 48 \w 42.00 68.00 0.50 14.40 -- 111.50-105.00 142.56 52 49 \w 71.00 107.00 0.50 14.40 -- 111.50-105.00 142.56 72 50 \w 78.00 103.00 0.50 14.40 -- 111.50 -95.00 30.00 50 51 \w 49.00 75.00 0.50 14.40 -- 111.50 -95.00 90.00 52 52 \w 78.00 103.00 0.50 14.40 -- 111.50 -95.00 90.00 50 53 \w 113.00 148.00 0.50 14.40 -- 111.50 30.00 150.00 70 54 \w 69.00 103.00 0.50 14.40 -- 111.50 -95.00 -90.00 68 55 \w 45.00 70.00 0.50 14.40 -- 111.50 -61.00 120.00 50 56 \w 110.00 135.00 0.50 14.40 -- 111.50 45.00 -30.00 50 57 \w 104.00 131.00 0.50 14.40 -- 111.50 30.00-150.00 54 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0629829000 _diffrn_orient_matrix_UB_12 -0.0189204000 _diffrn_orient_matrix_UB_13 -0.1083533000 _diffrn_orient_matrix_UB_21 -0.0032511000 _diffrn_orient_matrix_UB_22 -0.0492557000 _diffrn_orient_matrix_UB_23 0.0426604000 _diffrn_orient_matrix_UB_31 -0.1360539000 _diffrn_orient_matrix_UB_32 0.0099383000 _diffrn_orient_matrix_UB_33 0.0051658000 _diffrn_oxdiff_digest_frames ; 01c8e9bc48dae11a120cfb99860a1ff71900025d207 ; _diffrn_oxdiff_digest_hkl ; 01afc570dd15094cefe99d6c2cb905afc2ac0c ; _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8043 _reflns_number_total 8955 _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)' _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 'olex2.solve (Bourhis et al., 2015)' _refine_diff_density_max 0.758 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.068 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 700 _refine_ls_number_reflns 8955 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0612 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+8.7780P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1456 _refine_ls_wR_factor_ref 0.1488 _refine_special_details ? _olex2_refinement_description ; 1. Restrained distances C00X-H00X \\sim C00D-H00D \\sim C013-H013 \\sim C00V-H00V \\sim C00Y-H00Y \\sim C010-H010 with sigma of 0.02 ; _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary iterative _atom_sites_solution_secondary ? 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 Cr01 Cr 0.72195(4) 0.37620(2) 0.43104(3) 0.01681(12) Uani 1 1 d . . . . . O002 O 0.89600(17) 0.36250(6) 0.52120(13) 0.0193(4) Uani 1 1 d . . . . . O003 O 0.54583(18) 0.38400(6) 0.33865(14) 0.0208(4) Uani 1 1 d . . . . . N2 N 0.5950(2) 0.35915(8) 0.60840(18) 0.0230(5) Uani 1 1 d . . . . . N1 N 0.8491(2) 0.39920(8) 0.25559(18) 0.0237(5) Uani 1 1 d . . . . . C006 C 0.9568(2) 0.35020(9) 0.61716(19) 0.0167(5) Uani 1 1 d . . . . . C21 C 0.6421(3) 0.36578(9) 0.5470(2) 0.0219(5) Uani 1 1 d . . . . . C008 C 0.4832(2) 0.39562(9) 0.24291(19) 0.0180(5) Uani 1 1 d . . . . . C009 C 0.9721(2) 0.30201(9) 0.6441(2) 0.0205(5) Uani 1 1 d . . . . . C00A C 1.0706(3) 0.37073(10) 0.7921(2) 0.0225(5) Uani 1 1 d . . . . . C00B C 1.0783(3) 0.32447(10) 0.8197(2) 0.0250(6) Uani 1 1 d . . . . . C00C C 1.0133(2) 0.38519(9) 0.6919(2) 0.0186(5) Uani 1 1 d . . . . . C00D C 0.4176(3) 0.34070(11) 0.8199(2) 0.0296(6) Uani 1 1 d D . . . . C00E C 0.5352(3) 0.35194(9) 0.6811(2) 0.0216(5) Uani 1 1 d . . . . . C00F C 0.4496(2) 0.44304(9) 0.2163(2) 0.0184(5) Uani 1 1 d . . . . . C00G C 0.4420(3) 0.36031(9) 0.1667(2) 0.0213(5) Uani 1 1 d . . . . . C00H C 0.3914(3) 0.45436(10) 0.1140(2) 0.0236(6) Uani 1 1 d . . . . . C00I C 0.4713(3) 0.48096(9) 0.2977(2) 0.0225(5) Uani 1 1 d . . . . . C20 C 0.8031(3) 0.39170(10) 0.3171(2) 0.0229(5) Uani 1 1 d . . . . . C00K C 0.3990(3) 0.34972(10) 0.6459(2) 0.0262(6) Uani 1 1 d . . . . . C00L C 1.0794(3) 0.44189(10) 0.5814(2) 0.0265(6) Uani 1 1 d . . . . . C00M C 0.6155(3) 0.34846(9) 0.7825(2) 0.0251(6) Uani 1 1 d . . . . . C00N C 1.0160(3) 0.43676(9) 0.6632(2) 0.0216(5) Uani 1 1 d . . . . . C00O C 0.3590(3) 0.42071(11) 0.0395(2) 0.0262(6) Uani 1 1 d . . . . . C00P C 0.3812(3) 0.37447(11) 0.0666(2) 0.0271(6) Uani 1 1 d . . . . . C00Q C 0.8258(3) 0.42782(10) 0.0900(2) 0.0261(6) Uani 1 1 d . . . . . C00R C 1.0400(3) 0.40043(10) 0.2090(2) 0.0259(6) Uani 1 1 d . . . . . C00S C 0.9061(3) 0.40923(9) 0.1822(2) 0.0220(5) Uani 1 1 d . . . . . C00T C 1.0324(3) 0.29051(10) 0.7463(2) 0.0230(6) Uani 1 1 d . . . . . C00U C 0.9275(3) 0.26309(9) 0.5639(2) 0.0255(6) Uani 1 1 d . . . . . C00V C 1.0185(3) 0.43159(12) 0.0433(2) 0.0306(7) Uani 1 1 d D . . . . C00W C 0.3219(3) 0.35359(12) 0.5384(3) 0.0324(7) Uani 1 1 d . . . . . C00X C 0.3405(3) 0.34306(11) 0.7188(2) 0.0305(7) Uani 1 1 d D . . . . C00Y C 1.0946(3) 0.41144(11) 0.1348(2) 0.0301(6) Uani 1 1 d D . . . . C00Z C 0.6167(3) 0.48969(11) 0.3545(3) 0.0301(6) Uani 1 1 d . . . . . C010 C 0.8875(3) 0.43846(12) 0.0206(2) 0.0317(7) Uani 1 1 d D . . . . C011 C 0.4026(3) 0.46720(11) 0.3717(2) 0.0279(6) Uani 1 1 d . . . . . C012 C 0.4127(4) 0.52801(11) 0.2516(3) 0.0365(7) Uani 1 1 d . . . . . C013 C 0.5510(3) 0.34232(11) 0.8517(2) 0.0304(6) Uani 1 1 d D . . . . C014 C 0.8796(3) 0.45783(11) 0.6263(3) 0.0301(6) Uani 1 1 d . . . . . C015 C 0.6843(3) 0.43617(13) 0.0689(3) 0.0329(7) Uani 1 1 d . . . . . C016 C 1.1166(3) 0.38045(12) 0.3071(3) 0.0327(7) Uani 1 1 d . . . . . C017 C 0.6049(4) 0.29488(11) 0.2290(3) 0.0351(7) Uani 1 1 d . . . . . C018 C 0.9696(4) 0.21454(11) 0.6099(3) 0.0381(8) Uani 1 1 d . . . . . C019 C 0.4605(3) 0.30808(10) 0.1928(2) 0.0301(6) Uani 1 1 d . . . . . C01A C 0.7602(3) 0.35093(13) 0.8123(3) 0.0332(7) Uani 1 1 d . . . . . C01B C 0.7786(3) 0.26152(11) 0.5167(3) 0.0295(6) Uani 1 1 d . . . . . C01C C 0.4010(4) 0.29548(12) 0.2743(3) 0.0379(8) Uani 1 1 d . . . . . C01D C 1.0982(3) 0.46604(11) 0.7538(2) 0.0317(7) Uani 1 1 d . . . . . C01E C 0.9878(3) 0.26993(12) 0.4814(3) 0.0343(7) Uani 1 1 d . . . . . C01F C 0.3921(5) 0.27748(13) 0.1002(3) 0.0480(10) Uani 1 1 d . . . . . H1AA H 0.430(4) 0.2802(13) 0.048(3) 0.037(10) Uiso 1 1 d . . . . . H01Y H 0.739(4) 0.2585(13) 0.568(3) 0.040(10) Uiso 1 1 d . . . . . H00Y H 1.186(2) 0.4060(10) 0.148(2) 0.020(8) Uiso 1 1 d D . . . . H01M H 1.210(3) 0.3771(11) 0.311(2) 0.024(8) Uiso 1 1 d . . . . . H00X H 0.246(2) 0.3416(12) 0.698(3) 0.033(9) Uiso 1 1 d D . . . . H H 0.299(5) 0.2839(15) 0.073(3) 0.055(13) Uiso 1 1 d . . . . . H01P H 0.645(4) 0.3024(15) 0.183(3) 0.055(13) Uiso 1 1 d . . . . . H00G H 0.232(4) 0.3522(12) 0.530(3) 0.034(9) Uiso 1 1 d . . . . . H01A H 0.308(4) 0.4626(13) 0.340(3) 0.040(10) Uiso 1 1 d . . . . . H00D H 0.373(4) 0.3377(14) 0.867(3) 0.054(12) Uiso 1 1 d D . . . . H01J H 0.668(5) 0.4645(18) 0.103(4) 0.070(15) Uiso 1 1 d . . . . . H01D H 0.461(4) 0.5398(15) 0.209(3) 0.053(12) Uiso 1 1 d . . . . . H00T H 1.047(3) 0.2576(11) 0.766(2) 0.019(7) Uiso 1 1 d . . . . . H01S H 0.926(3) 0.2071(12) 0.659(3) 0.031(9) Uiso 1 1 d . . . . . H01V H 0.800(4) 0.3496(13) 0.887(3) 0.043(10) Uiso 1 1 d . . . . . H01 H 1.099(3) 0.4986(13) 0.731(3) 0.035(9) Uiso 1 1 d . . . . . H00B H 1.115(3) 0.3164(12) 0.887(3) 0.029(9) Uiso 1 1 d . . . . . H00I H 0.336(4) 0.3819(13) 0.510(3) 0.038(10) Uiso 1 1 d . . . . . H01Q H 0.655(3) 0.3090(13) 0.296(3) 0.035(9) Uiso 1 1 d . . . . . H01Z H 0.302(4) 0.3018(13) 0.253(3) 0.044(11) Uiso 1 1 d . . . . . H00C H 1.168(4) 0.4296(13) 0.605(3) 0.042(10) Uiso 1 1 d . . . . . H01B H 0.438(3) 0.4386(12) 0.408(3) 0.029(9) Uiso 1 1 d . . . . . H01G H 0.837(4) 0.4551(14) 0.674(3) 0.049(11) Uiso 1 1 d . . . . . H01E H 0.315(4) 0.5260(13) 0.218(3) 0.041(10) Uiso 1 1 d . . . . . H00H H 0.375(3) 0.4865(12) 0.097(2) 0.024(8) Uiso 1 1 d . . . . . H01H H 0.826(4) 0.4430(14) 0.564(3) 0.044(11) Uiso 1 1 d . . . . . H00E H 1.083(4) 0.4758(14) 0.565(3) 0.042(10) Uiso 1 1 d . . . . . HA H 0.414(4) 0.2608(16) 0.289(3) 0.059(13) Uiso 1 1 d . . . . . HB H 1.189(4) 0.4545(12) 0.782(3) 0.031(9) Uiso 1 1 d . . . . . H0AA H 1.088(4) 0.2683(13) 0.508(3) 0.042(10) Uiso 1 1 d . . . . . H01R H 0.613(4) 0.2609(15) 0.238(3) 0.047(11) Uiso 1 1 d . . . . . HC H 0.750(4) 0.2360(14) 0.466(3) 0.040(10) Uiso 1 1 d . . . . . H00V H 1.062(4) 0.4383(15) -0.002(3) 0.058(12) Uiso 1 1 d D . . . . HD H 0.966(4) 0.2992(16) 0.445(3) 0.053(12) Uiso 1 1 d . . . . . H01N H 1.114(4) 0.4003(15) 0.361(3) 0.053(12) Uiso 1 1 d . . . . . H01W H 0.791(4) 0.3788(15) 0.786(3) 0.054(12) Uiso 1 1 d . . . . . HE H 1.059(3) 0.4667(12) 0.808(3) 0.033(9) Uiso 1 1 d . . . . . HF H 0.441(4) 0.3122(14) 0.337(3) 0.043(11) Uiso 1 1 d . . . . . H00K H 0.630(4) 0.5174(14) 0.408(3) 0.043(10) Uiso 1 1 d . . . . . H01K H 0.639(4) 0.4394(14) -0.006(3) 0.045(11) Uiso 1 1 d . . . . . H013 H 0.607(3) 0.3413(12) 0.9217(17) 0.036(9) Uiso 1 1 d D . . . . H00L H 0.656(4) 0.4622(14) 0.393(3) 0.040(10) Uiso 1 1 d . . . . . H00P H 0.354(3) 0.3516(11) 0.014(2) 0.020(8) Uiso 1 1 d . . . . . H00O H 0.323(4) 0.4283(13) -0.029(3) 0.038(10) Uiso 1 1 d . . . . . H01I H 0.884(3) 0.4919(13) 0.612(3) 0.032(9) Uiso 1 1 d . . . . . H00M H 0.661(4) 0.4972(13) 0.309(3) 0.040(10) Uiso 1 1 d . . . . . H00F H 1.031(4) 0.4254(14) 0.519(3) 0.048(11) Uiso 1 1 d . . . . . HG H 0.405(4) 0.2456(17) 0.119(3) 0.062(13) Uiso 1 1 d . . . . . H00A H 1.106(3) 0.3930(11) 0.845(2) 0.023(8) Uiso 1 1 d . . . . . HH H 0.961(4) 0.2457(15) 0.430(3) 0.051(11) Uiso 1 1 d . . . . . HI H 0.743(4) 0.2899(14) 0.479(3) 0.043(10) Uiso 1 1 d . . . . . H01C H 0.412(4) 0.4917(13) 0.423(3) 0.040(10) Uiso 1 1 d . . . . . H01T H 1.066(4) 0.2133(15) 0.640(3) 0.056(12) Uiso 1 1 d . . . . . H01F H 0.427(4) 0.5506(13) 0.307(3) 0.039(10) Uiso 1 1 d . . . . . H01O H 1.083(4) 0.3499(15) 0.321(3) 0.053(12) Uiso 1 1 d . . . . . H01L H 0.642(4) 0.4102(17) 0.093(3) 0.066(14) Uiso 1 1 d . . . . . H01X H 0.793(4) 0.3271(16) 0.778(3) 0.061(13) Uiso 1 1 d . . . . . H01U H 0.946(4) 0.1906(15) 0.552(3) 0.053(12) Uiso 1 1 d . . . . . H010 H 0.837(4) 0.4511(14) -0.044(2) 0.056(12) Uiso 1 1 d D . . . . H00J H 0.353(4) 0.3313(14) 0.500(3) 0.044(11) Uiso 1 1 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 Cr01 0.0136(2) 0.0203(2) 0.0166(2) 0.00285(16) 0.00545(15) 0.00139(16) O002 0.0174(9) 0.0209(9) 0.0178(9) 0.0015(7) 0.0036(7) 0.0004(7) O003 0.0194(9) 0.0221(9) 0.0189(9) 0.0029(7) 0.0039(7) 0.0010(7) N2 0.0225(12) 0.0220(11) 0.0256(12) 0.0011(9) 0.0098(10) 0.0013(9) N1 0.0226(12) 0.0247(12) 0.0249(12) 0.0010(9) 0.0096(10) 0.0001(9) C006 0.0125(11) 0.0209(12) 0.0178(12) 0.0011(9) 0.0068(9) 0.0012(9) C21 0.0200(13) 0.0234(13) 0.0224(13) 0.0024(10) 0.0074(11) 0.0015(10) C008 0.0145(12) 0.0212(12) 0.0189(12) 0.0012(10) 0.0068(10) 0.0011(9) C009 0.0147(12) 0.0196(12) 0.0273(14) 0.0016(10) 0.0073(10) 0.0005(9) C00A 0.0182(13) 0.0279(14) 0.0208(13) -0.0036(11) 0.0059(10) -0.0032(11) C00B 0.0186(13) 0.0325(15) 0.0221(14) 0.0072(11) 0.0045(11) -0.0025(11) C00C 0.0150(12) 0.0200(12) 0.0216(13) 0.0000(10) 0.0072(10) 0.0000(9) C00D 0.0287(15) 0.0394(17) 0.0285(15) -0.0015(12) 0.0199(13) 0.0053(13) C00E 0.0252(14) 0.0196(12) 0.0242(13) 0.0007(10) 0.0138(11) 0.0007(10) C00F 0.0139(12) 0.0204(12) 0.0212(12) 0.0007(10) 0.0066(10) -0.0013(9) C00G 0.0178(12) 0.0223(13) 0.0245(13) -0.0020(10) 0.0082(10) -0.0007(10) C00H 0.0192(13) 0.0249(14) 0.0266(14) 0.0058(11) 0.0076(11) 0.0023(11) C00I 0.0219(13) 0.0197(12) 0.0254(14) -0.0020(10) 0.0076(11) 0.0014(10) C20 0.0208(13) 0.0260(13) 0.0221(13) 0.0023(11) 0.0074(11) 0.0011(11) C00K 0.0282(15) 0.0198(13) 0.0374(16) -0.0027(11) 0.0198(13) -0.0007(11) C00L 0.0259(15) 0.0238(14) 0.0310(15) 0.0037(12) 0.0113(12) -0.0017(11) C00M 0.0310(15) 0.0188(12) 0.0269(14) 0.0011(11) 0.0119(12) 0.0021(11) C00N 0.0197(13) 0.0199(12) 0.0253(13) -0.0012(10) 0.0078(11) -0.0001(10) C00O 0.0223(14) 0.0355(16) 0.0189(13) 0.0031(11) 0.0046(11) -0.0012(12) C00P 0.0253(14) 0.0323(15) 0.0229(14) -0.0059(12) 0.0071(11) -0.0042(12) C00Q 0.0258(14) 0.0284(14) 0.0259(14) 0.0010(11) 0.0111(12) -0.0025(11) C00R 0.0268(14) 0.0215(13) 0.0351(16) -0.0052(11) 0.0180(12) -0.0051(11) C00S 0.0246(14) 0.0214(12) 0.0233(13) -0.0008(10) 0.0125(11) -0.0027(10) C00T 0.0190(13) 0.0219(13) 0.0288(14) 0.0059(11) 0.0090(11) 0.0005(10) C00U 0.0241(14) 0.0185(13) 0.0318(15) -0.0010(11) 0.0070(12) 0.0018(11) C00V 0.0256(15) 0.0455(18) 0.0267(15) 0.0060(13) 0.0166(12) 0.0010(13) C00W 0.0227(15) 0.0338(17) 0.0458(19) 0.0068(14) 0.0182(14) 0.0023(13) C00X 0.0301(16) 0.0308(15) 0.0390(17) 0.0043(13) 0.0226(14) 0.0066(12) C00Y 0.0242(15) 0.0393(17) 0.0313(16) -0.0024(13) 0.0153(13) -0.0033(13) C00Z 0.0236(15) 0.0289(15) 0.0382(17) -0.0064(13) 0.0112(13) -0.0070(12) C010 0.0319(16) 0.0392(17) 0.0263(15) 0.0054(13) 0.0129(13) 0.0000(13) C011 0.0247(15) 0.0295(15) 0.0313(16) -0.0043(13) 0.0119(12) 0.0016(12) C012 0.047(2) 0.0212(14) 0.0395(18) 0.0007(13) 0.0131(16) 0.0092(14) C013 0.0383(17) 0.0306(15) 0.0242(14) 0.0023(12) 0.0130(13) 0.0048(13) C014 0.0261(15) 0.0233(14) 0.0419(18) -0.0007(13) 0.0129(14) 0.0023(12) C015 0.0238(15) 0.0429(18) 0.0328(17) 0.0081(14) 0.0107(13) 0.0008(13) C016 0.0242(15) 0.0395(18) 0.0351(17) -0.0007(14) 0.0111(13) -0.0009(13) C017 0.0403(19) 0.0229(15) 0.0413(19) -0.0026(13) 0.0129(16) 0.0073(13) C018 0.041(2) 0.0196(14) 0.045(2) -0.0005(14) 0.0040(16) 0.0049(13) C019 0.0384(17) 0.0191(13) 0.0332(16) -0.0035(12) 0.0125(13) -0.0041(12) C01A 0.0288(16) 0.0382(18) 0.0303(17) 0.0037(14) 0.0072(13) 0.0001(13) C01B 0.0254(15) 0.0227(14) 0.0369(17) -0.0018(13) 0.0062(13) -0.0031(12) C01C 0.043(2) 0.0254(16) 0.048(2) 0.0033(14) 0.0191(16) -0.0075(14) C01D 0.0371(18) 0.0238(15) 0.0322(16) -0.0059(12) 0.0093(14) -0.0081(13) C01E 0.0341(18) 0.0311(16) 0.0411(19) -0.0101(14) 0.0173(15) 0.0029(13) C01F 0.066(3) 0.0243(17) 0.044(2) -0.0092(15) 0.007(2) -0.0083(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cr01 O002 1.9310(18) . ? Cr01 O003 1.9315(18) . ? Cr01 C21 2.119(3) . ? Cr01 C20 2.128(3) . ? O002 C006 1.333(3) . ? O003 C008 1.328(3) . ? N2 C21 1.163(4) . ? N2 C00E 1.405(3) . ? N1 C20 1.162(4) . ? N1 C00S 1.406(3) . ? C006 C009 1.428(4) . ? C006 C00C 1.432(4) . ? C008 C00F 1.425(4) . ? C008 C00G 1.431(4) . ? C009 C00T 1.401(4) . ? C009 C00U 1.544(4) . ? C00A C00B 1.378(4) . ? C00A C00C 1.396(4) . ? C00B C00T 1.383(4) . ? C00C C00N 1.536(4) . ? C00D C00X 1.385(5) . ? C00D C013 1.371(4) . ? C00E C00K 1.400(4) . ? C00E C00M 1.400(4) . ? C00F C00H 1.400(4) . ? C00F C00I 1.538(4) . ? C00G C00P 1.397(4) . ? C00G C019 1.539(4) . ? C00H C00O 1.379(4) . ? C00I C00Z 1.535(4) . ? C00I C011 1.530(4) . ? C00I C012 1.539(4) . ? C00K C00W 1.462(5) . ? C00K C00X 1.396(4) . ? C00L C00N 1.541(4) . ? C00M C013 1.395(4) . ? C00M C01A 1.492(4) . ? C00N C014 1.526(4) . ? C00N C01D 1.535(4) . ? C00O C00P 1.379(4) . ? C00Q C00S 1.400(4) . ? C00Q C010 1.398(4) . ? C00Q C015 1.490(4) . ? C00R C00S 1.404(4) . ? C00R C00Y 1.404(4) . ? C00R C016 1.465(4) . ? C00U C018 1.538(4) . ? C00U C01B 1.533(4) . ? C00U C01E 1.532(5) . ? C00V C00Y 1.396(4) . ? C00V C010 1.370(4) . ? C017 C019 1.530(5) . ? C019 C01C 1.543(5) . ? C019 C01F 1.537(5) . ? 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 O002 Cr01 O003 174.88(8) . . ? O002 Cr01 C21 92.15(9) . . ? O002 Cr01 C20 88.12(9) . . ? O003 Cr01 C21 87.53(9) . . ? O003 Cr01 C20 92.56(9) . . ? C21 Cr01 C20 176.01(11) . . ? C006 O002 Cr01 139.18(16) . . ? C008 O003 Cr01 139.50(17) . . ? C21 N2 C00E 178.4(3) . . ? C20 N1 C00S 178.7(3) . . ? O002 C006 C009 119.9(2) . . ? O002 C006 C00C 119.9(2) . . ? C009 C006 C00C 120.1(2) . . ? N2 C21 Cr01 177.7(2) . . ? O003 C008 C00F 120.2(2) . . ? O003 C008 C00G 120.2(2) . . ? C00F C008 C00G 119.5(2) . . ? C006 C009 C00U 121.8(2) . . ? C00T C009 C006 118.2(2) . . ? C00T C009 C00U 120.0(2) . . ? C00B C00A C00C 122.3(3) . . ? C00A C00B C00T 119.7(3) . . ? C006 C00C C00N 121.6(2) . . ? C00A C00C C006 117.7(2) . . ? C00A C00C C00N 120.6(2) . . ? C013 C00D C00X 122.6(3) . . ? C00K C00E N2 116.9(2) . . ? C00K C00E C00M 125.2(3) . . ? C00M C00E N2 117.9(3) . . ? C008 C00F C00I 121.3(2) . . ? C00H C00F C008 118.5(2) . . ? C00H C00F C00I 120.2(2) . . ? C008 C00G C019 121.9(2) . . ? C00P C00G C008 118.0(2) . . ? C00P C00G C019 120.1(2) . . ? C00O C00H C00F 121.9(3) . . ? C00F C00I C012 111.8(2) . . ? C00Z C00I C00F 111.8(2) . . ? C00Z C00I C012 106.5(3) . . ? C011 C00I C00F 109.8(2) . . ? C011 C00I C00Z 110.4(2) . . ? C011 C00I C012 106.5(3) . . ? N1 C20 Cr01 178.4(2) . . ? C00E C00K C00W 121.9(3) . . ? C00X C00K C00E 116.4(3) . . ? C00X C00K C00W 121.6(3) . . ? C00E C00M C01A 121.1(3) . . ? C013 C00M C00E 115.6(3) . . ? C013 C00M C01A 123.4(3) . . ? C00C C00N C00L 110.0(2) . . ? C014 C00N C00C 111.5(2) . . ? C014 C00N C00L 110.2(2) . . ? C014 C00N C01D 106.9(2) . . ? C01D C00N C00C 111.5(2) . . ? C01D C00N C00L 106.5(2) . . ? C00P C00O C00H 119.2(3) . . ? C00O C00P C00G 122.5(3) . . ? C00S C00Q C015 121.6(3) . . ? C010 C00Q C00S 115.6(3) . . ? C010 C00Q C015 122.8(3) . . ? C00S C00R C00Y 115.4(3) . . ? C00S C00R C016 122.0(3) . . ? C00Y C00R C016 122.6(3) . . ? C00Q C00S N1 117.7(2) . . ? C00Q C00S C00R 125.6(3) . . ? C00R C00S N1 116.7(2) . . ? C00B C00T C009 121.6(3) . . ? C018 C00U C009 111.9(2) . . ? C01B C00U C009 111.1(2) . . ? C01B C00U C018 106.0(3) . . ? C01E C00U C009 110.6(2) . . ? C01E C00U C018 106.9(3) . . ? C01E C00U C01B 110.1(3) . . ? C010 C00V C00Y 121.3(3) . . ? C00D C00X C00K 119.4(3) . . ? C00V C00Y C00R 120.6(3) . . ? C00V C010 C00Q 121.4(3) . . ? C00D C013 C00M 120.7(3) . . ? C00G C019 C01C 110.5(3) . . ? C017 C019 C00G 110.9(2) . . ? C017 C019 C01C 110.1(3) . . ? C017 C019 C01F 106.7(3) . . ? C01F C019 C00G 111.6(3) . . ? C01F C019 C01C 106.9(3) . . ? _shelx_res_file ; TITL yyk190_croar2_xync2_auto_a.res in P2(1)/c yyk190_croar2_xync2_auto.res created by SHELXL-2018/3 at 14:58:45 on 07-Jul-2023 REM Old TITL YYK190_CrOAr2_XyNC2_auto in P21/c #14 REM SHELXT solution in P2(1)/c: R1 0.122, Rweak 0.019, Alpha 0.059 REM 1.543 for 193 systematic absences, Orientation as input REM Formula found by SHELXT: C46 N2 O2 Cr CELL 1.54184 10.928 28.6868 14.0779 90 110.037 90 ZERR 4 0.0004 0.001 0.0006 0 0.005 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cr N O UNIT 184 240 4 8 8 SADI C00X H00X C00D H00D C013 H013 C00V H00V C00Y H00Y C010 H010 L.S. 4 0 0 PLAN 72 SIZE 0.3 0.2 0.05 TEMP -173 BOND list 4 fmap 2 53 acta OMIT -9 0 2 OMIT -9 3 3 OMIT -9 17 1 OMIT -9 1 2 OMIT -8 2 2 REM REM REM WGHT 0.041600 8.778000 FVAR 0.26202 CR01 3 0.721954 0.376204 0.431038 11.00000 0.01365 0.02034 = 0.01664 0.00285 0.00545 0.00139 O002 5 0.895998 0.362501 0.521201 11.00000 0.01736 0.02093 = 0.01782 0.00146 0.00357 0.00042 O003 5 0.545827 0.384001 0.338650 11.00000 0.01936 0.02209 = 0.01892 0.00294 0.00392 0.00105 N2 4 0.595041 0.359150 0.608405 11.00000 0.02248 0.02200 = 0.02562 0.00105 0.00979 0.00126 N1 4 0.849140 0.399195 0.255591 11.00000 0.02258 0.02473 = 0.02488 0.00103 0.00959 0.00014 C006 1 0.956771 0.350204 0.617162 11.00000 0.01253 0.02095 = 0.01777 0.00107 0.00675 0.00122 C21 1 0.642146 0.365781 0.546993 11.00000 0.01999 0.02340 = 0.02245 0.00245 0.00742 0.00153 C008 1 0.483228 0.395616 0.242907 11.00000 0.01454 0.02124 = 0.01890 0.00117 0.00677 0.00113 C009 1 0.972130 0.302014 0.644144 11.00000 0.01467 0.01957 = 0.02731 0.00161 0.00725 0.00050 C00A 1 1.070608 0.370733 0.792070 11.00000 0.01819 0.02788 = 0.02085 -0.00358 0.00587 -0.00318 C00B 1 1.078275 0.324469 0.819726 11.00000 0.01864 0.03247 = 0.02206 0.00715 0.00446 -0.00246 C00C 1 1.013335 0.385190 0.691858 11.00000 0.01499 0.01995 = 0.02158 -0.00002 0.00715 0.00000 C00D 1 0.417635 0.340695 0.819876 11.00000 0.02870 0.03942 = 0.02848 -0.00146 0.01985 0.00527 C00E 1 0.535223 0.351942 0.681071 11.00000 0.02515 0.01963 = 0.02416 0.00071 0.01383 0.00071 C00F 1 0.449561 0.443042 0.216326 11.00000 0.01385 0.02043 = 0.02122 0.00071 0.00656 -0.00131 C00G 1 0.442024 0.360309 0.166737 11.00000 0.01785 0.02232 = 0.02447 -0.00203 0.00822 -0.00069 C00H 1 0.391367 0.454364 0.113959 11.00000 0.01921 0.02489 = 0.02656 0.00582 0.00755 0.00232 C00I 1 0.471268 0.480964 0.297666 11.00000 0.02192 0.01973 = 0.02539 -0.00205 0.00755 0.00136 C20 1 0.803064 0.391703 0.317136 11.00000 0.02081 0.02596 = 0.02210 0.00226 0.00741 0.00109 C00K 1 0.398987 0.349717 0.645855 11.00000 0.02820 0.01984 = 0.03736 -0.00267 0.01983 -0.00066 C00L 1 1.079428 0.441895 0.581358 11.00000 0.02594 0.02381 = 0.03103 0.00371 0.01126 -0.00171 C00M 1 0.615463 0.348459 0.782535 11.00000 0.03098 0.01884 = 0.02691 0.00106 0.01186 0.00207 C00N 1 1.016035 0.436758 0.663172 11.00000 0.01974 0.01987 = 0.02526 -0.00118 0.00781 -0.00013 C00O 1 0.358983 0.420708 0.039492 11.00000 0.02232 0.03554 = 0.01894 0.00310 0.00461 -0.00118 C00P 1 0.381186 0.374468 0.066580 11.00000 0.02529 0.03232 = 0.02287 -0.00589 0.00710 -0.00416 C00Q 1 0.825762 0.427822 0.089971 11.00000 0.02580 0.02843 = 0.02592 0.00103 0.01109 -0.00253 C00R 1 1.040037 0.400429 0.209012 11.00000 0.02675 0.02155 = 0.03507 -0.00518 0.01801 -0.00508 C00S 1 0.906067 0.409228 0.182234 11.00000 0.02460 0.02140 = 0.02326 -0.00078 0.01249 -0.00275 C00T 1 1.032447 0.290511 0.746332 11.00000 0.01899 0.02192 = 0.02878 0.00593 0.00902 0.00049 C00U 1 0.927529 0.263089 0.563881 11.00000 0.02412 0.01851 = 0.03183 -0.00095 0.00702 0.00184 C00V 1 1.018538 0.431589 0.043341 11.00000 0.02557 0.04552 = 0.02668 0.00595 0.01665 0.00098 C00W 1 0.321856 0.353594 0.538382 11.00000 0.02267 0.03382 = 0.04576 0.00684 0.01824 0.00234 C00X 1 0.340491 0.343059 0.718811 11.00000 0.03012 0.03084 = 0.03896 0.00426 0.02264 0.00656 C00Y 1 1.094557 0.411440 0.134810 11.00000 0.02424 0.03933 = 0.03129 -0.00241 0.01532 -0.00334 C00Z 1 0.616678 0.489685 0.354508 11.00000 0.02361 0.02888 = 0.03820 -0.00642 0.01122 -0.00699 C010 1 0.887522 0.438464 0.020567 11.00000 0.03186 0.03918 = 0.02633 0.00544 0.01286 0.00001 C011 1 0.402625 0.467196 0.371746 11.00000 0.02465 0.02950 = 0.03129 -0.00433 0.01194 0.00161 C012 1 0.412693 0.528007 0.251597 11.00000 0.04733 0.02117 = 0.03953 0.00074 0.01308 0.00918 C013 1 0.550989 0.342316 0.851701 11.00000 0.03826 0.03055 = 0.02421 0.00226 0.01299 0.00479 C014 1 0.879584 0.457834 0.626261 11.00000 0.02612 0.02333 = 0.04185 -0.00069 0.01285 0.00226 C015 1 0.684344 0.436167 0.068891 11.00000 0.02375 0.04293 = 0.03284 0.00806 0.01071 0.00080 C016 1 1.116645 0.380448 0.307127 11.00000 0.02421 0.03946 = 0.03507 -0.00066 0.01112 -0.00086 C017 1 0.604862 0.294881 0.228973 11.00000 0.04029 0.02295 = 0.04130 -0.00260 0.01289 0.00732 C018 1 0.969577 0.214538 0.609874 11.00000 0.04147 0.01955 = 0.04478 -0.00054 0.00400 0.00490 C019 1 0.460545 0.308076 0.192803 11.00000 0.03838 0.01906 = 0.03320 -0.00352 0.01252 -0.00407 C01A 1 0.760153 0.350927 0.812317 11.00000 0.02881 0.03824 = 0.03031 0.00375 0.00721 0.00015 C01B 1 0.778624 0.261517 0.516710 11.00000 0.02541 0.02266 = 0.03689 -0.00178 0.00618 -0.00315 C01C 1 0.400978 0.295483 0.274270 11.00000 0.04333 0.02539 = 0.04768 0.00325 0.01907 -0.00751 C01D 1 1.098222 0.466036 0.753824 11.00000 0.03715 0.02380 = 0.03220 -0.00595 0.00934 -0.00814 C01E 1 0.987813 0.269929 0.481358 11.00000 0.03409 0.03109 = 0.04110 -0.01015 0.01727 0.00293 C01F 1 0.392093 0.277478 0.100207 11.00000 0.06588 0.02432 = 0.04436 -0.00918 0.00658 -0.00829 H1AA 2 0.430448 0.280216 0.047582 11.00000 0.03744 H01Y 2 0.738770 0.258469 0.567504 11.00000 0.04034 H00Y 2 1.185620 0.405981 0.147868 11.00000 0.02015 H01M 2 1.210122 0.377145 0.311377 11.00000 0.02399 H00X 2 0.246394 0.341588 0.697685 11.00000 0.03316 H 2 0.299050 0.283948 0.072970 11.00000 0.05517 H01P 2 0.644971 0.302358 0.183198 11.00000 0.05537 H00G 2 0.231978 0.352176 0.529511 11.00000 0.03447 H01A 2 0.307875 0.462647 0.339771 11.00000 0.04005 H00D 2 0.373145 0.337655 0.866678 11.00000 0.05359 H01J 2 0.667645 0.464482 0.103083 11.00000 0.07036 H01D 2 0.460928 0.539769 0.209022 11.00000 0.05300 H00T 2 1.047288 0.257587 0.766373 11.00000 0.01935 H01S 2 0.926083 0.207129 0.658917 11.00000 0.03115 H01V 2 0.799794 0.349641 0.887358 11.00000 0.04294 H01 2 1.098828 0.498552 0.731104 11.00000 0.03516 H00B 2 1.115105 0.316364 0.886764 11.00000 0.02916 H00I 2 0.336454 0.381948 0.509738 11.00000 0.03801 H01Q 2 0.655475 0.309031 0.295715 11.00000 0.03467 H01Z 2 0.301613 0.301836 0.253153 11.00000 0.04421 H00C 2 1.167922 0.429583 0.604904 11.00000 0.04239 H01B 2 0.437579 0.438573 0.408218 11.00000 0.02874 H01G 2 0.836680 0.455103 0.673925 11.00000 0.04933 H01E 2 0.315311 0.525971 0.217721 11.00000 0.04055 H00H 2 0.374821 0.486500 0.096947 11.00000 0.02412 H01H 2 0.825661 0.442953 0.563603 11.00000 0.04358 H00E 2 1.083110 0.475776 0.564537 11.00000 0.04231 HA 2 0.414319 0.260809 0.289355 11.00000 0.05884 HB 2 1.189357 0.454506 0.782220 11.00000 0.03097 H0AA 2 1.087522 0.268340 0.508057 11.00000 0.04232 H01R 2 0.613049 0.260890 0.238063 11.00000 0.04675 HC 2 0.749923 0.236017 0.466115 11.00000 0.04040 H00V 2 1.062362 0.438344 -0.002244 11.00000 0.05762 HD 2 0.966365 0.299238 0.445140 11.00000 0.05327 H01N 2 1.113546 0.400318 0.360729 11.00000 0.05257 H01W 2 0.790608 0.378841 0.786136 11.00000 0.05371 HE 2 1.058756 0.466653 0.808218 11.00000 0.03327 HF 2 0.441195 0.312196 0.336997 11.00000 0.04302 H00K 2 0.629835 0.517377 0.407544 11.00000 0.04347 H01K 2 0.638767 0.439441 -0.006127 11.00000 0.04484 H013 2 0.607449 0.341326 0.921722 11.00000 0.03564 H00L 2 0.655903 0.462226 0.393072 11.00000 0.03992 H00P 2 0.353639 0.351580 0.013639 11.00000 0.01990 H00O 2 0.323290 0.428268 -0.028522 11.00000 0.03785 H01I 2 0.883580 0.491876 0.612434 11.00000 0.03184 H00M 2 0.661339 0.497155 0.308679 11.00000 0.04040 H00F 2 1.031349 0.425356 0.519358 11.00000 0.04830 HG 2 0.404539 0.245588 0.119299 11.00000 0.06184 H00A 2 1.105578 0.393031 0.845304 11.00000 0.02262 HH 2 0.961080 0.245745 0.429632 11.00000 0.05060 HI 2 0.743075 0.289856 0.478762 11.00000 0.04271 H01C 2 0.412260 0.491688 0.423415 11.00000 0.03999 H01T 2 1.066006 0.213271 0.639595 11.00000 0.05613 H01F 2 0.426924 0.550590 0.307407 11.00000 0.03925 H01O 2 1.082668 0.349886 0.321344 11.00000 0.05322 H01L 2 0.642292 0.410210 0.093211 11.00000 0.06556 H01X 2 0.793261 0.327058 0.778113 11.00000 0.06062 H01U 2 0.946412 0.190597 0.552491 11.00000 0.05253 H010 2 0.837185 0.451059 -0.044438 11.00000 0.05559 H00J 2 0.352554 0.331308 0.499535 11.00000 0.04386 HKLF 4 REM yyk190_croar2_xync2_auto_a.res in P2(1)/c REM wR2 = 0.1488, GooF = S = 1.108, Restrained GooF = 1.107 for all data REM R1 = 0.0612 for 8043 Fo > 4sig(Fo) and 0.0680 for all 8955 data REM 700 parameters refined using 15 restraints END WGHT 0.0414 8.7831 REM Highest difference peak 0.758, deepest hole -0.528, 1-sigma level 0.068 Q1 1 0.3555 0.3595 0.5986 11.00000 0.05 0.76 Q2 1 1.0796 0.3987 0.2585 11.00000 0.05 0.64 Q3 1 0.8167 0.3790 0.4256 11.00000 0.05 0.64 Q4 1 0.6212 0.3790 0.4405 11.00000 0.05 0.53 Q5 1 0.7602 0.3989 0.2395 11.00000 0.05 0.52 Q6 1 0.6970 0.3610 0.6431 11.00000 0.05 0.44 Q7 1 0.6975 0.3826 0.3421 11.00000 0.05 0.40 Q8 1 0.7348 0.3677 0.5254 11.00000 0.05 0.38 Q9 1 0.9499 0.3783 0.4383 11.00000 0.05 0.38 Q10 1 0.3968 0.3576 0.8010 11.00000 0.05 0.35 Q11 1 1.0413 0.4577 0.0608 11.00000 0.05 0.33 Q12 1 0.4513 0.3802 0.3279 11.00000 0.05 0.30 Q13 1 0.4873 0.3776 0.4223 11.00000 0.05 0.29 Q14 1 0.8216 0.3643 0.5242 11.00000 0.05 0.28 Q15 1 0.7542 0.3772 0.3376 11.00000 0.05 0.27 Q16 1 0.6971 0.3362 0.4781 11.00000 0.05 0.26 Q17 1 0.7230 0.4152 0.1241 11.00000 0.05 0.26 Q18 1 0.3599 0.3581 0.5143 11.00000 0.05 0.25 Q19 1 0.3573 0.3811 0.2579 11.00000 0.05 0.24 Q20 1 1.0124 0.4426 0.6044 11.00000 0.05 0.24 Q21 1 0.9078 0.2613 0.5020 11.00000 0.05 0.24 Q22 1 0.4607 0.4607 0.2617 11.00000 0.05 0.24 Q23 1 0.3279 0.3795 0.4386 11.00000 0.05 0.24 Q24 1 1.0637 0.3794 0.4329 11.00000 0.05 0.23 Q25 1 0.5263 0.3589 0.1623 11.00000 0.05 0.23 Q26 1 0.4467 0.2992 0.2378 11.00000 0.05 0.23 Q27 1 0.2219 0.4221 0.0392 11.00000 0.05 0.22 Q28 1 0.5331 0.5385 0.2425 11.00000 0.05 0.22 Q29 1 0.7618 0.3442 0.7014 11.00000 0.05 0.22 Q30 1 0.3963 0.3004 0.1993 11.00000 0.05 0.22 Q31 1 0.5367 0.3624 0.3252 11.00000 0.05 0.22 Q32 1 1.3365 0.3827 0.3279 11.00000 0.05 0.22 Q33 1 0.3859 0.3768 0.4215 11.00000 0.05 0.21 Q34 1 1.0162 0.3608 0.5179 11.00000 0.05 0.21 Q35 1 1.0180 0.2586 0.5465 11.00000 0.05 0.21 Q36 1 0.4498 0.3389 0.1770 11.00000 0.05 0.21 Q37 1 0.5343 0.3431 0.7956 11.00000 0.05 0.21 Q38 1 0.6035 0.3829 0.3417 11.00000 0.05 0.21 Q39 1 0.9819 0.3809 0.5354 11.00000 0.05 0.21 Q40 1 0.4762 0.3810 0.1983 11.00000 0.05 0.21 Q41 1 0.3151 0.3427 0.6648 11.00000 0.05 0.21 Q42 1 0.7400 0.3587 0.7550 11.00000 0.05 0.20 Q43 1 0.5655 0.3580 0.5442 11.00000 0.05 0.20 Q44 1 0.1984 0.3574 0.6191 11.00000 0.05 0.20 Q45 1 0.4807 0.4177 0.2328 11.00000 0.05 0.20 Q46 1 0.8380 0.3824 0.1181 11.00000 0.05 0.20 Q47 1 0.9163 0.3624 0.5628 11.00000 0.05 0.20 Q48 1 0.5183 0.4391 0.2079 11.00000 0.05 0.20 Q49 1 0.9392 0.3795 0.3442 11.00000 0.05 0.20 Q50 1 0.7779 0.3844 0.6956 11.00000 0.05 0.20 Q51 1 0.5082 0.3646 0.5175 11.00000 0.05 0.20 Q52 1 0.7832 0.4407 0.5985 11.00000 0.05 0.20 Q53 1 0.7026 0.2208 0.6043 11.00000 0.05 0.19 Q54 1 1.1651 0.3780 0.4346 11.00000 0.05 0.19 Q55 1 0.9620 0.2589 0.7802 11.00000 0.05 0.19 Q56 1 0.2984 0.3985 0.7104 11.00000 0.05 0.19 Q57 1 1.0619 0.3785 0.0710 11.00000 0.05 0.18 Q58 1 1.0740 0.3414 0.7971 11.00000 0.05 0.18 Q59 1 0.7592 0.3732 0.5781 11.00000 0.05 0.18 Q60 1 0.7017 0.3422 0.7392 11.00000 0.05 0.18 Q61 1 0.9368 0.3360 0.3849 11.00000 0.05 0.18 Q62 1 0.3760 0.4809 0.3085 11.00000 0.05 0.18 Q63 1 0.8428 0.3391 0.3558 11.00000 0.05 0.18 Q64 1 0.5311 0.3036 0.2087 11.00000 0.05 0.18 Q65 1 0.4006 0.4164 0.2524 11.00000 0.05 0.18 Q66 1 0.8491 0.3014 0.6520 11.00000 0.05 0.18 Q67 1 1.2052 0.3821 0.1459 11.00000 0.05 0.18 Q68 1 1.1661 0.3436 0.7797 11.00000 0.05 0.18 Q69 1 0.8293 0.3193 0.3768 11.00000 0.05 0.17 Q70 1 0.3585 0.4018 0.4874 11.00000 0.05 0.17 Q71 1 0.8945 0.3024 0.4279 11.00000 0.05 0.17 Q72 1 1.0022 0.3386 0.8203 11.00000 0.05 0.17 ; _shelx_res_checksum 85398 _olex2_exptl_crystal_mounting_method Loop _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 1.426 _oxdiff_exptl_absorpt_empirical_full_min 0.631 _chemical_properties_physical Air-sensitive,Moisture-sensitive,Oxygen-sensitive ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_yyk_criii_crtbos3xync2_auto _database_code_depnum_ccdc_archive 'CCDC 2286292' loop_ _audit_author_name _audit_author_address 'Yuya Kakiuchi' ;ETH Zurich Switzerland ; _audit_update_record ; 2023-08-02 deposited with the CCDC. 2024-05-20 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT213_yyk_criii_crtbos3xync2_auto ; PROBLEM: Atom C7 has ADP max/min Ratio ..... 4.3 oblate RESPONSE: The compound includes highly flexible -OSi(OtBu)3 ligand, which keeps its mobility even at 100K causing the disorder. ; # Added during the CSD deposition process: Wednesday 02 August 2023 03:53 PM # end Validation Reply Form _audit_creation_date 2023-07-25 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic Cr(OSi(tBu)3)3(XyNC)2 _chemical_formula_moiety 'C54 H99 Cr N2 O12 Si3' _chemical_formula_sum 'C54 H99 Cr N2 O12 Si3' _chemical_formula_weight 1104.62 _chemical_absolute_configuration ? _chemical_melting_point ? _chemical_oxdiff_formula CrNCHOSi _chemical_oxdiff_usercomment 'pentane, -30 deg, half year' 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' Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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' _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. ; _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' 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' _cell_length_a 13.1907(3) _cell_length_b 20.8362(5) _cell_length_c 23.4449(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6443.7(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 27244 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 80.0280 _cell_measurement_theta_min 2.7300 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 2.429 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.76106 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.61a (Rigaku Oxford Diffraction, 2022) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour blue _exptl_crystal_colour_lustre . _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 2396 _exptl_crystal_preparation 'recrystallization from pentane' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: n-pentane' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_unetI/netI 0.0430 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 47345 _diffrn_reflns_point_group_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.953 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.871 _diffrn_reflns_theta_min 2.837 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.984 _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 -99.00 -41.00 0.50 0.69 -- -49.62 -48.00-100.00 116 2 \w -54.00 -29.00 0.50 2.77 -- -90.00 48.00 47.00 50 3 \w -151.00-124.00 0.50 2.77 -- -90.00 -97.00 39.00 54 4 \w 105.00 138.00 0.50 2.77 -- 111.50 83.00-104.00 66 5 \w 111.00 146.00 0.50 2.77 -- 111.50 48.00 47.00 70 6 \w 144.00 178.00 0.50 2.77 -- 111.50 83.00-104.00 68 7 \w -114.00 -87.00 0.50 0.69 -- -49.62-125.00-150.00 54 8 \w -43.00 20.00 0.50 0.69 -- -49.62 48.00 47.00 126 9 \w -118.00 -73.00 0.50 0.69 -- -49.62-125.00 60.00 90 10 \w 45.00 70.00 0.50 2.77 -- 111.50 -61.00 30.00 50 11 \w 45.00 70.00 0.50 2.77 -- 111.50 -61.00 0.00 50 12 \w 117.00 156.00 0.50 2.77 -- 111.50 30.00 90.00 78 13 \w 123.00 175.00 0.50 2.77 -- 111.50 15.00 0.00 104 14 \w 60.00 87.00 0.50 2.77 -- 111.50 -95.00 60.00 54 15 \w 45.00 70.00 0.50 2.77 -- 111.50 -61.00 -90.00 50 16 \w 42.00 71.00 0.50 2.77 -- 111.50 -77.00-150.00 58 17 \w 60.00 85.00 0.50 2.77 -- 111.50 -77.00 0.00 50 18 \w 98.00 125.00 0.50 2.77 -- 111.50 61.00-120.00 54 19 \w 151.00 178.00 0.50 2.77 -- 111.50 61.00-120.00 54 20 \w 41.00 66.00 0.50 2.77 -- 111.50 -61.00 -30.00 50 21 \w 119.00 164.00 0.50 2.77 -- 111.50 30.00 150.00 90 22 \w 130.00 177.00 0.50 2.77 -- 111.50 125.00 -60.00 94 23 \w 105.00 136.00 0.50 2.77 -- 111.50 30.00 -30.00 62 24 \w 105.00 131.00 0.50 2.77 -- 111.50 15.00 60.00 52 25 \w 136.00 170.00 0.50 2.77 -- 111.50 15.00 60.00 68 26 \w 43.00 68.00 0.50 2.77 -- 111.50 -61.00 120.00 50 27 \w 80.00 105.00 0.50 2.77 -- 111.50 -77.00 30.00 50 28 \w 55.00 80.00 0.50 2.77 -- 111.50-125.00 0.00 50 29 \w 81.00 111.00 0.50 2.77 -- 111.50-125.00 150.00 60 30 \w 138.00 164.00 0.50 2.77 -- 111.50 15.00 -30.00 52 31 \w 143.00 177.00 0.50 2.77 -- 111.50 77.00 -60.00 68 32 \w 150.00 176.00 0.50 2.77 -- 111.50 48.00 47.00 52 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0622349000 _diffrn_orient_matrix_UB_12 -0.0046166000 _diffrn_orient_matrix_UB_13 -0.0554552000 _diffrn_orient_matrix_UB_21 0.0306297000 _diffrn_orient_matrix_UB_22 0.0691575000 _diffrn_orient_matrix_UB_23 -0.0154480000 _diffrn_orient_matrix_UB_31 0.0939671000 _diffrn_orient_matrix_UB_32 -0.0256475000 _diffrn_orient_matrix_UB_33 -0.0317369000 _diffrn_oxdiff_digest_frames ; 01f3be118ff862737a9b17d4c565a76fbf000319b15 ; _diffrn_oxdiff_digest_hkl ; 01d8c79c2a07a808d96d0eb674ed752f03327a ; _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _reflns_Friedel_coverage 0.769 _reflns_Friedel_fraction_full 0.969 _reflns_Friedel_fraction_max 0.915 _reflns_number_gt 13046 _reflns_number_total 13511 _reflns_odcompleteness_completeness 98.14 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 80.95 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. Completness statistics refer to single and composite reflections containing twin component 1 only. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)' _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 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.402 _refine_diff_density_min -1.074 _refine_diff_density_rms 0.098 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.068(11) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 804 _refine_ls_number_reflns 13511 _refine_ls_number_restraints 773 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0835 _refine_ls_restrained_S_all 1.084 _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^)+31.7748P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1905 _refine_ls_wR_factor_ref 0.1915 _refine_special_details ; Refined as a 2-component inversion twin. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.932(11) 0.068(11) 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 3. Rigid body (RIGU) restrains C7, C8, C11, C4AA, O2, Si18 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O8, C0AA, C1Q, C1P, C1O, Si32 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C16, C18, C1A, C19, O1, Si18 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 C1M, C1L, C1J, C1K, O6, Si7 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C1G, C1H, C1I, C1F, O5, Si7 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O3, C1AA, C1D, C1B, C1C, Si7 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O7, C3AA, C1N, C10, C9 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C2AA, C1E, C17, C5AA, O4, Si7 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C7, C18, C19 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 All non-hydrogen atoms with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 C18, C7 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 4. Others Sof(O1)=Sof(C16)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)= Sof(H19B)=Sof(H19C)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1) Sof(O2)=Sof(C4AA)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)= Sof(H8B)=Sof(H8C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(1) Sof(O4)=Sof(C2AA)=Sof(C5AA)=Sof(H5AA)=Sof(H5AB)=Sof(H5AC)=Sof(C17)=Sof(H17A)= Sof(H17B)=Sof(H17C)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(H1EC)=Sof(O6)=Sof(C1J)= Sof(C1K)=Sof(H1KA)=Sof(H1KB)=Sof(H1KC)=Sof(C1L)=Sof(H1LA)=Sof(H1LB)=Sof(H1LC)= Sof(C1M)=Sof(H1MA)=Sof(H1MB)=Sof(H1MC)=1-FVAR(2) Sof(O3)=Sof(C1AA)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C1C)=Sof(H1CA)= Sof(H1CB)=Sof(H1CC)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=Sof(O5)=Sof(C1F)= Sof(C1G)=Sof(H1GA)=Sof(H1GB)=Sof(H1GC)=Sof(C1H)=Sof(H1HA)=Sof(H1HB)=Sof(H1HC)= Sof(C1I)=Sof(H1IA)=Sof(H1IB)=Sof(H1IC)=FVAR(2) Sof(O8)=Sof(C0AA)=Sof(C1O)=Sof(H1OA)=Sof(H1OB)=Sof(H1OC)=Sof(C1P)=Sof(H1PA)= Sof(H1PB)=Sof(H1PC)=Sof(C1Q)=Sof(H1QA)=Sof(H1QB)=Sof(H1QC)=1-FVAR(3) Sof(O7)=Sof(C3AA)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)= Sof(H10B)=Sof(H10C)=Sof(C1N)=Sof(H1NA)=Sof(H1NB)=Sof(H1NC)=FVAR(3) 5.a Free rotating group: O2(C4AA,C7,C8,C11), O1(C16,C18,C19,C1A), O3(C1AA,C1B,C1C,C1D), O4(C2AA,C5AA, C17,C1E), O5(C1F,C1G,C1H,C1I), O6(C1J,C1K,C1L,C1M), O7(C3AA,C9,C10,C1N), O8(C0AA,C1O,C1P,C1Q) 5.b Aromatic/amide H refined with riding coordinates: C62(H62), C60(H60), C51(H51), C52(H52), C50(H50), C61(H61) 5.c Idealised Me refined as rotating group: C73(H73A,H73B,H73C), C40(H40A,H40B,H40C), C21(H21A,H21B,H21C), C67(H67A,H67B, H67C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C15(H15A, H15B,H15C), C43(H43A,H43B,H43C), C66(H66A,H66B,H66C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C45(H45A,H45B,H45C), C24(H24A,H24B,H24C), C57(H57A,H57B, H57C), C28(H28A,H28B,H28C), C35(H35A,H35B,H35C), C46(H46A,H46B,H46C), C44(H44A, H44B,H44C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C18(H18A, H18B,H18C), C19(H19A,H19B,H19C), C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C1D(H1DA,H1DB,H1DC), C5AA(H5AA,H5AB,H5AC), C17(H17A,H17B, H17C), C1E(H1EA,H1EB,H1EC), C1G(H1GA,H1GB,H1GC), C1H(H1HA,H1HB,H1HC), C1I(H1IA, H1IB,H1IC), C1K(H1KA,H1KB,H1KC), C1L(H1LA,H1LB,H1LC), C1M(H1MA,H1MB,H1MC), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C1N(H1NA,H1NB,H1NC), C1O(H1OA,H1OB,H1OC), C1P(H1PA,H1PB,H1PC), C1Q(H1QA,H1QB,H1QC) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? 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 Cr1 Cr 0.34545(8) 0.51238(5) 0.61027(5) 0.0222(2) Uani 1 1 d . U . . . Si7 Si 0.47746(16) 0.54982(10) 0.52458(9) 0.0268(4) Uani 1 1 d . U . . . Si18 Si 0.21733(15) 0.62446(9) 0.68054(8) 0.0245(4) Uani 1 1 d . U . . . Si32 Si 0.23142(15) 0.36957(9) 0.64618(8) 0.0234(4) Uani 1 1 d . U . . . O33 O 0.2676(4) 0.3128(2) 0.6021(2) 0.0305(11) Uani 1 1 d . U . . . O16 O 0.4136(4) 0.5853(2) 0.5714(2) 0.0275(10) Uani 1 1 d . U . . . O19 O 0.2310(4) 0.6839(2) 0.6364(2) 0.0242(9) Uani 1 1 d . U . . . O31 O 0.2811(4) 0.5618(2) 0.6669(2) 0.0243(10) Uani 1 1 d . U . . . O47 O 0.3006(4) 0.4293(2) 0.6343(2) 0.0262(10) Uani 1 1 d . U . . . O41 O 0.1108(4) 0.3794(3) 0.6335(2) 0.0320(11) Uani 1 1 d . U . . . O22 O 0.0974(4) 0.6059(3) 0.6770(3) 0.0353(12) Uani 1 1 d . U . . . N54 N 0.5457(4) 0.5017(3) 0.6936(3) 0.0307(14) Uani 1 1 d . U . . . O52 O 0.4386(5) 0.4759(3) 0.5384(3) 0.0421(14) Uani 1 1 d . U . . . N66 N 0.1589(5) 0.5284(3) 0.5202(3) 0.0307(13) Uani 1 1 d . U . . . C58 C 0.0868(6) 0.5346(4) 0.4772(3) 0.0297(14) Uani 1 1 d . U . . . C20 C 0.3070(5) 0.7334(3) 0.6306(3) 0.0239(13) Uani 1 1 d . U . . . C69 C 0.4762(5) 0.5031(4) 0.6646(4) 0.0304(15) Uani 1 1 d . U . . . C59 C 0.0661(6) 0.5952(4) 0.4546(3) 0.0311(15) Uani 1 1 d . U . . . C48 C 0.6270(5) 0.5037(4) 0.7318(3) 0.0277(13) Uani 1 1 d . U . . . C73 C 0.6712(6) 0.3905(4) 0.7024(4) 0.0367(18) Uani 1 1 d . U . . . H73A H 0.603288 0.373580 0.710316 0.055 Uiso 1 1 calc GR . . . . H73B H 0.722007 0.357874 0.712041 0.055 Uiso 1 1 calc GR . . . . H73C H 0.676677 0.401374 0.661899 0.055 Uiso 1 1 calc GR . . . . C53 C 0.6892(5) 0.4499(4) 0.7380(3) 0.0290(14) Uani 1 1 d . U . . . C63 C 0.0410(6) 0.4783(4) 0.4572(3) 0.0320(15) Uani 1 1 d . U . . . C62 C -0.0296(6) 0.4850(4) 0.4127(3) 0.0350(16) Uani 1 1 d . U . . . H62 H -0.063006 0.447972 0.398227 0.042 Uiso 1 1 calc R . . . . C40 C 0.1721(7) 0.2211(4) 0.6384(4) 0.0432(19) Uani 1 1 d . U . . . H40A H 0.221666 0.212692 0.668643 0.065 Uiso 1 1 calc GR . . . . H40B H 0.140708 0.180650 0.626528 0.065 Uiso 1 1 calc GR . . . . H40C H 0.119746 0.250316 0.652736 0.065 Uiso 1 1 calc GR . . . . C68 C 0.2226(6) 0.5217(4) 0.5539(3) 0.0283(14) Uani 1 1 d . U . . . C60 C -0.0034(6) 0.5995(4) 0.4102(3) 0.0357(16) Uani 1 1 d . U . . . H60 H -0.018450 0.640024 0.393675 0.043 Uiso 1 1 calc R . . . . C21 C 0.4069(6) 0.7121(4) 0.6565(5) 0.043(2) Uani 1 1 d . U . . . H21A H 0.397487 0.703432 0.697251 0.065 Uiso 1 1 calc GR . . . . H21B H 0.457551 0.746062 0.651623 0.065 Uiso 1 1 calc GR . . . . H21C H 0.430241 0.672968 0.637362 0.065 Uiso 1 1 calc GR . . . . C67 C 0.0671(8) 0.4139(4) 0.4811(4) 0.043(2) Uani 1 1 d . U . . . H67A H 0.138069 0.403851 0.472410 0.064 Uiso 1 1 calc GR . . . . H67B H 0.023117 0.381222 0.463922 0.064 Uiso 1 1 calc GR . . . . H67C H 0.057266 0.414232 0.522485 0.064 Uiso 1 1 calc GR . . . . C25 C 0.0176(7) 0.7088(4) 0.7022(4) 0.0380(18) Uani 1 1 d . U . . . H25A H 0.028504 0.701606 0.743010 0.057 Uiso 1 1 calc GR . . . . H25B H -0.044496 0.733855 0.696631 0.057 Uiso 1 1 calc GR . . . . H25C H 0.075397 0.732300 0.686273 0.057 Uiso 1 1 calc GR . . . . C27 C 0.2682(7) 0.7930(4) 0.6596(4) 0.0386(19) Uani 1 1 d . U . . . H27A H 0.205338 0.806929 0.641166 0.058 Uiso 1 1 calc GR . . . . H27B H 0.319113 0.827071 0.656699 0.058 Uiso 1 1 calc GR . . . . H27C H 0.254962 0.783660 0.699921 0.058 Uiso 1 1 calc GR . . . . C26 C -0.0140(6) 0.6550(4) 0.6090(4) 0.0387(17) Uani 1 1 d . U . . . H26A H 0.041395 0.679776 0.591935 0.058 Uiso 1 1 calc GR . . . . H26B H -0.077839 0.678464 0.604493 0.058 Uiso 1 1 calc GR . . . . H26C H -0.019211 0.613283 0.589811 0.058 Uiso 1 1 calc GR . . . . C51 C 0.7822(7) 0.5092(5) 0.8094(4) 0.0442(18) Uani 1 1 d . U . . . H51 H 0.834405 0.510590 0.837287 0.053 Uiso 1 1 calc R . . . . C23 C 0.0073(6) 0.6446(4) 0.6721(4) 0.0320(15) Uani 1 1 d . U . . . C12 C 0.4600(7) 0.4142(4) 0.5116(4) 0.0365(17) Uani 1 1 d . U . . . C52 C 0.7664(6) 0.4528(4) 0.7771(3) 0.0338(15) Uani 1 1 d . U . . . H52 H 0.809407 0.416735 0.782526 0.041 Uiso 1 1 calc R . . . . C50 C 0.7228(7) 0.5614(5) 0.8004(4) 0.0459(19) Uani 1 1 d . U . . . H50 H 0.736100 0.599385 0.821532 0.055 Uiso 1 1 calc R . . . . C61 C -0.0512(6) 0.5442(4) 0.3898(4) 0.0372(16) Uani 1 1 d . U . . . H61 H -0.099231 0.547522 0.359747 0.045 Uiso 1 1 calc R . . . . C49 C 0.6439(6) 0.5615(4) 0.7620(4) 0.0378(16) Uani 1 1 d . U . . . C15 C 0.3617(7) 0.3893(4) 0.4895(4) 0.0411(18) Uani 1 1 d . U . . . H15A H 0.312731 0.386609 0.520869 0.062 Uiso 1 1 calc GR . . . . H15B H 0.371935 0.346595 0.473066 0.062 Uiso 1 1 calc GR . . . . H15C H 0.335754 0.418442 0.460114 0.062 Uiso 1 1 calc GR . . . . C43 C 0.0673(8) 0.4522(4) 0.7114(4) 0.047(2) Uani 1 1 d . U . . . H43A H 0.120398 0.434135 0.735807 0.071 Uiso 1 1 calc GR . . . . H43B H 0.010961 0.467280 0.735079 0.071 Uiso 1 1 calc GR . . . . H43C H 0.094989 0.488214 0.689492 0.071 Uiso 1 1 calc GR . . . . C34 C 0.2258(9) 0.2520(4) 0.5872(4) 0.0456(19) Uani 1 1 d . U . . . C66 C 0.1188(8) 0.6556(4) 0.4763(4) 0.046(2) Uani 1 1 d . U . . . H66A H 0.144220 0.648073 0.514986 0.069 Uiso 1 1 calc GR . . . . H66B H 0.070531 0.691293 0.476711 0.069 Uiso 1 1 calc GR . . . . H66C H 0.175695 0.666134 0.451048 0.069 Uiso 1 1 calc GR . . . . C13 C 0.5029(7) 0.3711(5) 0.5597(4) 0.045(2) Uani 1 1 d . U . . . H13A H 0.575450 0.379777 0.564433 0.068 Uiso 1 1 calc GR . . . . H13B H 0.493105 0.325914 0.549553 0.068 Uiso 1 1 calc GR . . . . H13C H 0.467363 0.380400 0.595430 0.068 Uiso 1 1 calc GR . . . . C14 C 0.5366(8) 0.4224(5) 0.4635(4) 0.050(2) Uani 1 1 d . U . . . H14A H 0.507609 0.449819 0.433727 0.076 Uiso 1 1 calc GR . . . . H14B H 0.553034 0.380261 0.447315 0.076 Uiso 1 1 calc GR . . . . H14C H 0.598440 0.442256 0.478477 0.076 Uiso 1 1 calc GR . . . . C42 C 0.0295(7) 0.4011(4) 0.6708(5) 0.046(2) Uani 1 1 d . U . . . C45 C -0.0116(8) 0.3431(5) 0.7013(6) 0.063(3) Uani 1 1 d . U . . . H45A H -0.035640 0.311722 0.673281 0.094 Uiso 1 1 calc GR . . . . H45B H -0.068040 0.356058 0.725954 0.094 Uiso 1 1 calc GR . . . . H45C H 0.042057 0.323827 0.724590 0.094 Uiso 1 1 calc GR . . . . C24 C -0.0776(7) 0.6052(5) 0.6998(5) 0.052(3) Uani 1 1 d . U . . . H24A H -0.090299 0.566597 0.676957 0.077 Uiso 1 1 calc GR . . . . H24B H -0.139605 0.631066 0.701594 0.077 Uiso 1 1 calc GR . . . . H24C H -0.057296 0.592737 0.738397 0.077 Uiso 1 1 calc GR . . . . C57 C 0.5808(8) 0.6199(5) 0.7496(6) 0.060(3) Uani 1 1 d . U . . . H57A H 0.508811 0.608536 0.751069 0.091 Uiso 1 1 calc GR . . . . H57B H 0.597497 0.636294 0.711559 0.091 Uiso 1 1 calc GR . . . . H57C H 0.595117 0.653091 0.778153 0.091 Uiso 1 1 calc GR . . . . C28 C 0.3192(8) 0.7433(5) 0.5673(4) 0.045(2) Uani 1 1 d . U . . . H28A H 0.354345 0.706236 0.550736 0.068 Uiso 1 1 calc GR . . . . H28B H 0.359019 0.782220 0.560343 0.068 Uiso 1 1 calc GR . . . . H28C H 0.252292 0.747752 0.549604 0.068 Uiso 1 1 calc GR . . . . C35 C 0.1482(12) 0.2633(5) 0.5388(5) 0.076(4) Uani 1 1 d . U . . . H35A H 0.092519 0.290033 0.552984 0.114 Uiso 1 1 calc GR . . . . H35B H 0.121314 0.221985 0.525790 0.114 Uiso 1 1 calc GR . . . . H35C H 0.181616 0.285135 0.506859 0.114 Uiso 1 1 calc GR . . . . C46 C 0.3136(11) 0.2111(4) 0.5674(5) 0.065(3) Uani 1 1 d . U . . . H46A H 0.345947 0.231385 0.534337 0.098 Uiso 1 1 calc GR . . . . H46B H 0.288706 0.168476 0.556615 0.098 Uiso 1 1 calc GR . . . . H46C H 0.363118 0.206924 0.598317 0.098 Uiso 1 1 calc GR . . . . C44 C -0.0499(7) 0.4294(5) 0.6296(6) 0.065(3) Uani 1 1 d . U . . . H44A H -0.022501 0.468215 0.611750 0.097 Uiso 1 1 calc GR . . . . H44B H -0.111502 0.440264 0.650928 0.097 Uiso 1 1 calc GR . . . . H44C H -0.066172 0.397765 0.600112 0.097 Uiso 1 1 calc GR . . . . O2 O 0.2509(12) 0.6536(6) 0.7439(4) 0.039(3) Uani 0.62(2) 1 d . U P A 2 C4AA C 0.2554(9) 0.6268(5) 0.8004(3) 0.053(4) Uani 0.62(2) 1 d G U P A 2 C7 C 0.1445(10) 0.6192(11) 0.8184(6) 0.093(8) Uani 0.62(2) 1 d G U P A 2 H7A H 0.111760 0.661418 0.819220 0.140 Uiso 0.62(2) 1 calc GR . P A 2 H7B H 0.141476 0.599907 0.856520 0.140 Uiso 0.62(2) 1 calc GR . P A 2 H7C H 0.109302 0.591430 0.791138 0.140 Uiso 0.62(2) 1 calc GR . P A 2 C8 C 0.3090(13) 0.5614(6) 0.7983(6) 0.062(5) Uani 0.62(2) 1 d G U P A 2 H8A H 0.274218 0.533408 0.771023 0.093 Uiso 0.62(2) 1 calc GR . P A 2 H8B H 0.307397 0.541695 0.836265 0.093 Uiso 0.62(2) 1 calc GR . P A 2 H8C H 0.379547 0.567391 0.786365 0.093 Uiso 0.62(2) 1 calc GR . P A 2 C11 C 0.3114(18) 0.6733(7) 0.8403(5) 0.095(9) Uani 0.62(2) 1 d G U P A 2 H11A H 0.384166 0.672173 0.831879 0.143 Uiso 0.62(2) 1 calc GR . P A 2 H11B H 0.300078 0.660549 0.879987 0.143 Uiso 0.62(2) 1 calc GR . P A 2 H11C H 0.285720 0.716972 0.834385 0.143 Uiso 0.62(2) 1 calc GR . P A 2 O1 O 0.2325(18) 0.6522(10) 0.7416(5) 0.037(4) Uani 0.38(2) 1 d . U P A 1 C16 C 0.2329(11) 0.6306(6) 0.7999(5) 0.037(4) Uani 0.38(2) 1 d G U P A 1 C18 C 0.1468(14) 0.5815(9) 0.8032(8) 0.039(5) Uani 0.38(2) 1 d G U P A 1 H18A H 0.081550 0.603548 0.799281 0.058 Uiso 0.38(2) 1 calc GR . P A 1 H18B H 0.149328 0.559449 0.840136 0.058 Uiso 0.38(2) 1 calc GR . P A 1 H18C H 0.154352 0.550037 0.772450 0.058 Uiso 0.38(2) 1 calc GR . P A 1 C19 C 0.3354(12) 0.5991(11) 0.8135(9) 0.046(6) Uani 0.38(2) 1 d G U P A 1 H19A H 0.330837 0.552762 0.806713 0.070 Uiso 0.38(2) 1 calc GR . P A 1 H19B H 0.352640 0.606873 0.853577 0.070 Uiso 0.38(2) 1 calc GR . P A 1 H19C H 0.387989 0.617502 0.788966 0.070 Uiso 0.38(2) 1 calc GR . P A 1 C1A C 0.2126(19) 0.6877(8) 0.8397(8) 0.045(6) Uani 0.38(2) 1 d G U P A 1 H1AA H 0.258984 0.722856 0.830343 0.068 Uiso 0.38(2) 1 calc GR . P A 1 H1AB H 0.223446 0.674403 0.879386 0.068 Uiso 0.38(2) 1 calc GR . P A 1 H1AC H 0.142440 0.702154 0.834957 0.068 Uiso 0.38(2) 1 calc GR . P A 1 O3 O 0.5998(6) 0.5365(5) 0.5482(4) 0.034(2) Uani 0.510(8) 1 d . U P B 2 C1AA C 0.6910(7) 0.5744(5) 0.5462(4) 0.043(4) Uani 0.510(8) 1 d G U P B 2 C1B C 0.7601(9) 0.5449(10) 0.5916(7) 0.068(6) Uani 0.510(8) 1 d G U P B 2 H1BA H 0.733186 0.554719 0.629585 0.103 Uiso 0.510(8) 1 calc GR . P B 2 H1BB H 0.828413 0.562951 0.587928 0.103 Uiso 0.510(8) 1 calc GR . P B 2 H1BC H 0.762927 0.498319 0.586377 0.103 Uiso 0.510(8) 1 calc GR . P B 2 C1C C 0.7390(10) 0.5690(9) 0.4867(5) 0.053(5) Uani 0.510(8) 1 d G U P B 2 H1CA H 0.752663 0.523786 0.478082 0.079 Uiso 0.510(8) 1 calc GR . P B 2 H1CB H 0.802645 0.593221 0.485868 0.079 Uiso 0.510(8) 1 calc GR . P B 2 H1CC H 0.692273 0.586517 0.458161 0.079 Uiso 0.510(8) 1 calc GR . P B 2 C1D C 0.6659(15) 0.6445(5) 0.5606(9) 0.068(6) Uani 0.510(8) 1 d G U P B 2 H1DA H 0.624939 0.663113 0.529850 0.101 Uiso 0.510(8) 1 calc GR . P B 2 H1DB H 0.728979 0.669002 0.564570 0.101 Uiso 0.510(8) 1 calc GR . P B 2 H1DC H 0.627867 0.646266 0.596426 0.101 Uiso 0.510(8) 1 calc GR . P B 2 O4 O 0.5867(6) 0.5659(5) 0.5107(4) 0.028(2) Uani 0.490(8) 1 d . U P B 1 C2AA C 0.6759(7) 0.5840(6) 0.5421(4) 0.039(4) Uani 0.490(8) 1 d G U P B 1 C5AA C 0.7009(11) 0.5254(11) 0.5789(8) 0.077(7) Uani 0.490(8) 1 d G U P B 1 H5AA H 0.645184 0.517473 0.605631 0.115 Uiso 0.490(8) 1 calc GR . P B 1 H5AB H 0.763487 0.533369 0.600202 0.115 Uiso 0.490(8) 1 calc GR . P B 1 H5AC H 0.709909 0.487770 0.554285 0.115 Uiso 0.490(8) 1 calc GR . P B 1 C17 C 0.7625(8) 0.5987(10) 0.5003(6) 0.048(5) Uani 0.490(8) 1 d G U P B 1 H17A H 0.791297 0.558315 0.486132 0.072 Uiso 0.490(8) 1 calc GR . P B 1 H17B H 0.815350 0.623308 0.519895 0.072 Uiso 0.490(8) 1 calc GR . P B 1 H17C H 0.736260 0.623698 0.468134 0.072 Uiso 0.490(8) 1 calc GR . P B 1 C1E C 0.6523(15) 0.6427(10) 0.5796(9) 0.090(9) Uani 0.490(8) 1 d G U P B 1 H1EA H 0.635953 0.679435 0.555184 0.135 Uiso 0.490(8) 1 calc GR . P B 1 H1EB H 0.711512 0.652889 0.603095 0.135 Uiso 0.490(8) 1 calc GR . P B 1 H1EC H 0.594331 0.633036 0.604280 0.135 Uiso 0.490(8) 1 calc GR . P B 1 O5 O 0.5013(6) 0.5748(5) 0.4612(4) 0.031(2) Uani 0.510(8) 1 d . U P B 2 C1F C 0.4375(6) 0.6081(4) 0.4211(4) 0.025(3) Uani 0.510(8) 1 d G U P B 2 C1G C 0.4832(10) 0.5931(8) 0.3626(3) 0.041(4) Uani 0.510(8) 1 d G U P B 2 H1GA H 0.553455 0.608347 0.361349 0.061 Uiso 0.510(8) 1 calc GR . P B 2 H1GB H 0.443619 0.614694 0.332911 0.061 Uiso 0.510(8) 1 calc GR . P B 2 H1GC H 0.481811 0.546641 0.356142 0.061 Uiso 0.510(8) 1 calc GR . P B 2 C1H C 0.3286(5) 0.5824(8) 0.4255(6) 0.046(4) Uani 0.510(8) 1 d G U P B 2 H1HA H 0.328779 0.535863 0.419530 0.068 Uiso 0.510(8) 1 calc GR . P B 2 H1HB H 0.286325 0.602947 0.396415 0.068 Uiso 0.510(8) 1 calc GR . P B 2 H1HC H 0.301300 0.592022 0.463453 0.068 Uiso 0.510(8) 1 calc GR . P B 2 C1I C 0.4409(14) 0.6805(4) 0.4334(7) 0.057(7) Uani 0.510(8) 1 d G U P B 2 H1IA H 0.421759 0.688256 0.473224 0.085 Uiso 0.510(8) 1 calc GR . P B 2 H1IB H 0.393508 0.702801 0.408112 0.085 Uiso 0.510(8) 1 calc GR . P B 2 H1IC H 0.509767 0.696563 0.426823 0.085 Uiso 0.510(8) 1 calc GR . P B 2 O6 O 0.4163(7) 0.5548(4) 0.4618(3) 0.025(2) Uani 0.490(8) 1 d . U P B 1 C1J C 0.4255(6) 0.5943(4) 0.4117(3) 0.026(3) Uani 0.490(8) 1 d G U P B 1 C1K C 0.5210(7) 0.5699(7) 0.3816(5) 0.034(3) Uani 0.490(8) 1 d G U P B 1 H1KA H 0.578774 0.572598 0.407774 0.051 Uiso 0.490(8) 1 calc GR . P B 1 H1KB H 0.534343 0.596424 0.347890 0.051 Uiso 0.490(8) 1 calc GR . P B 1 H1KC H 0.511001 0.525240 0.369906 0.051 Uiso 0.490(8) 1 calc GR . P B 1 C1L C 0.3316(8) 0.5853(7) 0.3738(4) 0.032(3) Uani 0.490(8) 1 d G U P B 1 H1LA H 0.327201 0.540368 0.361574 0.048 Uiso 0.490(8) 1 calc GR . P B 1 H1LB H 0.337003 0.613054 0.340219 0.048 Uiso 0.490(8) 1 calc GR . P B 1 H1LC H 0.270566 0.596602 0.395431 0.048 Uiso 0.490(8) 1 calc GR . P B 1 C1M C 0.4375(12) 0.6648(4) 0.4295(6) 0.029(4) Uani 0.490(8) 1 d G U P B 1 H1MA H 0.376190 0.679093 0.449364 0.044 Uiso 0.490(8) 1 calc GR . P B 1 H1MB H 0.448042 0.691363 0.395455 0.044 Uiso 0.490(8) 1 calc GR . P B 1 H1MC H 0.496074 0.669099 0.454931 0.044 Uiso 0.490(8) 1 calc GR . P B 1 O7 O 0.2446(10) 0.3415(7) 0.7116(7) 0.025(3) Uani 0.60(4) 1 d . U P C 2 C3AA C 0.3337(9) 0.3283(5) 0.7450(4) 0.024(3) Uani 0.60(4) 1 d G U P C 2 C9 C 0.2978(14) 0.2821(7) 0.7915(7) 0.032(4) Uani 0.60(4) 1 d G U P C 2 H9A H 0.244009 0.302539 0.813926 0.049 Uiso 0.60(4) 1 calc GR . P C 2 H9B H 0.354766 0.271329 0.816554 0.049 Uiso 0.60(4) 1 calc GR . P C 2 H9C H 0.271496 0.242852 0.773847 0.049 Uiso 0.60(4) 1 calc GR . P C 2 C10 C 0.4146(9) 0.2966(8) 0.7071(6) 0.030(3) Uani 0.60(4) 1 d G U P C 2 H10A H 0.386191 0.258132 0.689216 0.045 Uiso 0.60(4) 1 calc GR . P C 2 H10B H 0.473196 0.284659 0.730535 0.045 Uiso 0.60(4) 1 calc GR . P C 2 H10C H 0.436038 0.326903 0.677500 0.045 Uiso 0.60(4) 1 calc GR . P C 2 C1N C 0.3736(16) 0.3910(7) 0.7711(5) 0.039(5) Uani 0.60(4) 1 d G U P C 2 H1NA H 0.392313 0.420811 0.740501 0.058 Uiso 0.60(4) 1 calc GR . P C 2 H1NB H 0.433348 0.381840 0.794601 0.058 Uiso 0.60(4) 1 calc GR . P C 2 H1NC H 0.320744 0.410429 0.794841 0.058 Uiso 0.60(4) 1 calc GR . P C 2 O8 O 0.2280(15) 0.3447(12) 0.7123(11) 0.028(4) Uani 0.40(4) 1 d . U P C 1 C0AA C 0.3090(13) 0.3455(9) 0.7534(7) 0.027(5) Uani 0.40(4) 1 d G U P C 1 C1O C 0.276(2) 0.2984(11) 0.7998(11) 0.035(6) Uani 0.40(4) 1 d G U P C 1 H1OA H 0.204717 0.306444 0.809747 0.052 Uiso 0.40(4) 1 calc GR . P C 1 H1OB H 0.318279 0.304211 0.833687 0.052 Uiso 0.40(4) 1 calc GR . P C 1 H1OC H 0.282978 0.254357 0.785711 0.052 Uiso 0.40(4) 1 calc GR . P C 1 C1P C 0.4077(13) 0.3231(14) 0.7249(11) 0.037(6) Uani 0.40(4) 1 d G U P C 1 H1PA H 0.402570 0.277372 0.715555 0.056 Uiso 0.40(4) 1 calc GR . P C 1 H1PB H 0.464686 0.329909 0.751022 0.056 Uiso 0.40(4) 1 calc GR . P C 1 H1PC H 0.418953 0.347749 0.689818 0.056 Uiso 0.40(4) 1 calc GR . P C 1 C1Q C 0.321(2) 0.4136(10) 0.7777(9) 0.037(6) Uani 0.40(4) 1 d G U P C 1 H1QA H 0.345103 0.442471 0.747703 0.055 Uiso 0.40(4) 1 calc GR . P C 1 H1QB H 0.369475 0.412968 0.809216 0.055 Uiso 0.40(4) 1 calc GR . P C 1 H1QC H 0.254904 0.428779 0.791702 0.055 Uiso 0.40(4) 1 calc GR . P C 1 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 Cr1 0.0170(5) 0.0210(5) 0.0285(6) -0.0010(5) 0.0026(5) 0.0003(4) Si7 0.0294(10) 0.0295(10) 0.0216(9) 0.0011(8) 0.0042(8) 0.0011(8) Si18 0.0277(10) 0.0226(9) 0.0232(9) -0.0001(7) 0.0046(8) 0.0005(8) Si32 0.0220(9) 0.0218(9) 0.0262(9) 0.0005(7) -0.0023(7) -0.0004(7) O33 0.038(3) 0.023(2) 0.031(3) -0.0035(19) -0.007(2) 0.001(2) O16 0.026(2) 0.021(2) 0.036(3) -0.001(2) 0.007(2) -0.0028(19) O19 0.023(2) 0.024(2) 0.025(2) 0.0026(18) 0.002(2) -0.0032(19) O31 0.021(2) 0.025(2) 0.027(2) 0.0003(18) -0.0036(19) -0.0005(18) O47 0.024(2) 0.023(2) 0.031(3) -0.0015(19) -0.002(2) -0.0008(18) O41 0.024(2) 0.031(3) 0.042(3) 0.007(2) -0.003(2) 0.000(2) O22 0.028(2) 0.027(3) 0.052(3) 0.008(2) 0.014(2) 0.0060(19) N54 0.019(2) 0.031(3) 0.043(3) 0.000(3) 0.001(2) 0.000(2) O52 0.047(3) 0.028(2) 0.051(3) -0.008(2) 0.033(3) -0.002(2) N66 0.033(3) 0.034(3) 0.025(3) 0.001(2) -0.004(2) -0.003(3) C58 0.029(3) 0.036(3) 0.024(3) 0.002(3) -0.003(3) -0.004(3) C20 0.023(3) 0.022(3) 0.027(3) -0.002(2) 0.002(2) -0.005(2) C69 0.021(3) 0.027(4) 0.043(4) -0.002(3) 0.000(3) 0.000(3) C59 0.032(4) 0.033(3) 0.028(3) 0.002(3) 0.009(3) 0.004(3) C48 0.021(3) 0.035(3) 0.027(3) 0.001(3) 0.004(2) -0.008(2) C73 0.027(4) 0.039(4) 0.044(4) -0.004(3) -0.009(3) 0.001(3) C53 0.020(3) 0.036(3) 0.031(3) 0.003(3) 0.005(2) -0.007(2) C63 0.034(4) 0.037(3) 0.026(3) 0.002(3) -0.007(3) -0.007(3) C62 0.030(4) 0.045(4) 0.030(3) -0.005(3) -0.006(3) 0.000(3) C40 0.052(5) 0.023(4) 0.055(5) 0.002(3) -0.017(4) -0.007(3) C68 0.033(3) 0.028(4) 0.023(3) 0.001(3) -0.004(2) -0.002(3) C60 0.034(4) 0.044(4) 0.029(4) 0.005(3) 0.007(3) 0.006(3) C21 0.030(4) 0.027(4) 0.073(6) 0.001(4) -0.017(4) -0.004(3) C67 0.054(5) 0.038(4) 0.036(5) 0.008(4) -0.017(4) -0.007(4) C25 0.033(4) 0.036(4) 0.045(5) -0.005(3) 0.007(4) 0.013(3) C27 0.040(4) 0.023(3) 0.053(5) -0.007(3) 0.011(4) -0.005(3) C26 0.034(4) 0.039(4) 0.043(4) -0.003(3) 0.005(3) 0.004(3) C51 0.034(4) 0.056(4) 0.043(4) -0.004(3) -0.002(3) -0.019(3) C23 0.028(3) 0.027(3) 0.042(4) 0.003(3) 0.010(3) 0.008(3) C12 0.046(4) 0.028(3) 0.036(4) -0.003(3) 0.011(3) 0.009(3) C52 0.028(3) 0.046(4) 0.028(3) 0.006(3) -0.001(3) -0.008(3) C50 0.042(4) 0.046(4) 0.050(5) -0.006(4) 0.002(3) -0.021(3) C61 0.032(4) 0.049(4) 0.030(4) 0.001(3) 0.001(3) 0.006(3) C49 0.033(4) 0.036(3) 0.044(4) -0.006(3) 0.011(3) -0.014(3) C15 0.057(4) 0.030(4) 0.035(4) -0.004(3) 0.003(3) 0.004(3) C43 0.055(5) 0.033(4) 0.054(5) 0.010(3) 0.030(4) 0.004(4) C34 0.066(5) 0.022(3) 0.049(4) -0.003(3) -0.012(4) -0.006(3) C66 0.063(6) 0.040(4) 0.035(4) -0.003(4) 0.004(4) -0.006(4) C13 0.052(5) 0.046(5) 0.038(4) -0.005(4) 0.007(4) 0.025(4) C14 0.054(5) 0.044(5) 0.053(5) -0.009(4) 0.029(4) 0.009(4) C42 0.028(4) 0.033(4) 0.077(6) 0.013(3) 0.016(3) 0.003(3) C45 0.040(5) 0.043(5) 0.106(9) 0.024(5) 0.029(5) 0.001(4) C24 0.028(4) 0.045(5) 0.081(7) 0.022(5) 0.020(4) 0.008(3) C57 0.039(5) 0.040(4) 0.102(9) -0.015(5) 0.006(5) -0.004(4) C28 0.057(6) 0.049(5) 0.030(3) 0.005(3) 0.005(3) -0.031(4) C35 0.125(9) 0.037(5) 0.067(6) 0.010(5) -0.054(7) -0.037(6) C46 0.112(8) 0.019(4) 0.064(7) -0.011(4) 0.018(6) 0.006(5) C44 0.033(4) 0.052(6) 0.110(9) 0.025(6) 0.000(5) 0.007(4) O2 0.067(8) 0.025(6) 0.024(4) -0.002(3) 0.002(4) -0.009(5) C4AA 0.093(10) 0.043(7) 0.022(5) -0.002(5) 0.008(6) 0.007(7) C7 0.104(11) 0.15(2) 0.021(8) 0.011(11) 0.034(8) 0.019(11) C8 0.090(13) 0.044(8) 0.052(10) 0.007(6) -0.014(9) 0.005(8) C11 0.18(2) 0.065(11) 0.043(9) -0.018(9) -0.022(12) -0.001(13) O1 0.061(10) 0.026(8) 0.023(3) 0.001(4) 0.005(4) -0.007(7) C16 0.044(8) 0.044(9) 0.023(5) 0.003(5) 0.004(5) -0.003(6) C18 0.053(9) 0.052(10) 0.011(9) 0.016(7) -0.007(7) -0.010(9) C19 0.048(8) 0.056(13) 0.036(10) 0.004(10) 0.001(7) 0.002(8) C1A 0.066(15) 0.047(9) 0.023(6) 0.002(7) 0.001(9) 0.003(8) O3 0.024(3) 0.053(6) 0.026(5) 0.003(5) 0.006(3) 0.004(4) C1AA 0.025(6) 0.059(8) 0.045(8) 0.006(7) -0.002(6) -0.001(6) C1B 0.034(9) 0.094(15) 0.077(11) 0.038(12) -0.018(8) -0.017(9) C1C 0.014(7) 0.086(15) 0.058(9) 0.014(9) 0.012(7) 0.002(9) C1D 0.043(13) 0.064(8) 0.096(18) -0.021(10) -0.006(13) -0.004(8) O4 0.018(3) 0.042(6) 0.025(5) 0.004(4) -0.003(3) 0.003(3) C2AA 0.023(6) 0.068(10) 0.026(8) 0.005(6) -0.008(5) -0.006(6) C5AA 0.039(11) 0.122(16) 0.069(14) 0.055(12) -0.020(9) -0.005(11) C17 0.033(7) 0.085(16) 0.026(8) 0.001(8) -0.007(6) -0.022(9) C1E 0.039(14) 0.127(15) 0.105(19) -0.069(14) -0.021(12) -0.001(13) O5 0.020(5) 0.042(6) 0.032(4) 0.005(4) 0.003(3) 0.008(4) C1F 0.017(5) 0.036(7) 0.024(5) -0.004(5) 0.001(4) 0.004(5) C1G 0.046(9) 0.046(10) 0.030(6) 0.000(6) 0.016(6) 0.004(8) C1H 0.022(6) 0.069(11) 0.045(10) 0.012(9) 0.001(6) -0.004(7) C1I 0.083(18) 0.035(7) 0.053(14) -0.010(8) -0.006(13) 0.006(7) O6 0.023(5) 0.030(5) 0.022(4) 0.005(3) 0.003(3) -0.001(4) C1J 0.036(7) 0.029(6) 0.012(5) 0.003(4) 0.001(4) 0.002(5) C1K 0.037(7) 0.042(9) 0.024(7) 0.008(6) 0.007(6) 0.006(6) C1L 0.032(6) 0.047(9) 0.017(6) 0.004(6) 0.004(5) -0.004(6) C1M 0.044(11) 0.027(6) 0.017(8) 0.005(5) 0.004(7) 0.005(6) O7 0.021(5) 0.023(6) 0.032(4) 0.003(4) -0.004(4) -0.001(4) C3AA 0.020(5) 0.030(6) 0.024(5) 0.000(4) -0.001(4) -0.006(5) C9 0.039(9) 0.033(8) 0.026(7) 0.007(6) -0.001(6) 0.003(7) C10 0.028(6) 0.038(8) 0.025(7) 0.002(6) -0.001(5) 0.002(5) C1N 0.041(11) 0.038(7) 0.037(7) -0.006(5) -0.006(6) -0.012(7) O8 0.027(7) 0.031(10) 0.025(4) 0.001(5) -0.006(5) 0.000(6) C0AA 0.025(8) 0.031(9) 0.024(8) 0.005(6) -0.006(6) 0.000(7) C1O 0.038(13) 0.037(11) 0.029(10) 0.008(9) -0.001(8) 0.003(10) C1P 0.026(8) 0.056(16) 0.030(12) 0.005(10) -0.004(7) 0.003(9) C1Q 0.029(13) 0.035(9) 0.046(12) -0.003(8) -0.016(9) -0.001(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cr1 Si7 2.771(2) . ? Cr1 O16 1.987(5) . ? Cr1 O31 1.882(5) . ? Cr1 O47 1.915(5) . ? Cr1 O52 2.220(5) . ? Cr1 C69 2.154(8) . ? Cr1 C68 2.101(7) . ? Si7 O16 1.569(5) . ? Si7 O52 1.654(6) . ? Si7 O3 1.729(9) . ? Si7 O4 1.514(9) . ? Si7 O5 1.606(9) . ? Si7 O6 1.682(8) . ? Si18 O19 1.623(5) . ? Si18 O31 1.586(5) . ? Si18 O22 1.631(6) . ? Si18 O2 1.665(11) . ? Si18 O1 1.557(17) . ? Si32 O33 1.641(5) . ? Si32 O47 1.568(5) . ? Si32 O41 1.631(5) . ? Si32 O7 1.650(17) . ? Si32 O8 1.64(3) . ? O33 C34 1.426(10) . ? O19 C20 1.446(8) . ? O41 C42 1.455(11) . ? O22 C23 1.441(9) . ? N54 C69 1.141(10) . ? N54 C48 1.398(9) . ? O52 C12 1.459(9) . ? N66 C58 1.393(10) . ? N66 C68 1.160(10) . ? C58 C59 1.396(11) . ? C58 C63 1.400(11) . ? C20 C21 1.517(11) . ? C20 C27 1.504(10) . ? C20 C28 1.508(11) . ? C59 C60 1.390(12) . ? C59 C66 1.525(12) . ? C48 C53 1.396(11) . ? C48 C49 1.415(11) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C73 C53 1.513(11) . ? C53 C52 1.371(11) . ? C63 C62 1.405(10) . ? C63 C67 1.496(12) . ? C62 H62 0.9500 . ? C62 C61 1.375(12) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C40 C34 1.536(14) . ? C60 H60 0.9500 . ? C60 C61 1.398(13) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C25 C23 1.517(11) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 C23 1.521(12) . ? C51 H51 0.9500 . ? C51 C52 1.413(12) . ? C51 C50 1.357(14) . ? C23 C24 1.534(11) . ? C12 C15 1.489(13) . ? C12 C13 1.548(12) . ? C12 C14 1.524(12) . ? C52 H52 0.9500 . ? C50 H50 0.9500 . ? C50 C49 1.377(13) . ? C61 H61 0.9500 . ? C49 C57 1.502(14) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C43 C42 1.512(14) . ? C34 C35 1.547(14) . ? C34 C46 1.511(16) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C42 C45 1.505(12) . ? C42 C44 1.542(14) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? O2 C4AA 1.4388 . ? C4AA C7 1.5307 . ? C4AA C8 1.5362 . ? C4AA C11 1.5362 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? O1 C16 1.4384 . ? C16 C18 1.5309 . ? C16 C19 1.5361 . ? C16 C1A 1.5364 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? O3 C1AA 1.4391 . ? C1AA C1B 1.5300 . ? C1AA C1C 1.5361 . ? C1AA C1D 1.5360 . ? C1B H1BA 0.9800 . ? C1B H1BB 0.9800 . ? C1B H1BC 0.9800 . ? C1C H1CA 0.9800 . ? C1C H1CB 0.9800 . ? C1C H1CC 0.9800 . ? C1D H1DA 0.9800 . ? C1D H1DB 0.9800 . ? C1D H1DC 0.9800 . ? O4 C2AA 1.4384 . ? C2AA C5AA 1.5306 . ? C2AA C17 1.5369 . ? C2AA C1E 1.5366 . ? C5AA H5AA 0.9800 . ? C5AA H5AB 0.9800 . ? C5AA H5AC 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C1E H1EA 0.9800 . ? C1E H1EB 0.9800 . ? C1E H1EC 0.9800 . ? O5 C1F 1.4392 . ? C1F C1G 1.5309 . ? C1F C1H 1.5364 . ? C1F C1I 1.5359 . ? C1G H1GA 0.9800 . ? C1G H1GB 0.9800 . ? C1G H1GC 0.9800 . ? C1H H1HA 0.9800 . ? C1H H1HB 0.9800 . ? C1H H1HC 0.9800 . ? C1I H1IA 0.9800 . ? C1I H1IB 0.9800 . ? C1I H1IC 0.9800 . ? O6 C1J 1.4391 . ? C1J C1K 1.5303 . ? C1J C1L 1.5358 . ? C1J C1M 1.5366 . ? C1K H1KA 0.9800 . ? C1K H1KB 0.9800 . ? C1K H1KC 0.9800 . ? C1L H1LA 0.9800 . ? C1L H1LB 0.9800 . ? C1L H1LC 0.9800 . ? C1M H1MA 0.9800 . ? C1M H1MB 0.9800 . ? C1M H1MC 0.9800 . ? O7 C3AA 1.4391 . ? C3AA C9 1.5300 . ? C3AA C10 1.5366 . ? C3AA C1N 1.5364 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C1N H1NA 0.9800 . ? C1N H1NB 0.9800 . ? C1N H1NC 0.9800 . ? O8 C0AA 1.4380 . ? C0AA C1O 1.5300 . ? C0AA C1P 1.5371 . ? C0AA C1Q 1.5364 . ? C1O H1OA 0.9800 . ? C1O H1OB 0.9800 . ? C1O H1OC 0.9800 . ? C1P H1PA 0.9800 . ? C1P H1PB 0.9800 . ? C1P H1PC 0.9800 . ? C1Q H1QA 0.9800 . ? C1Q H1QB 0.9800 . ? C1Q H1QC 0.9800 . ? 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 O16 Cr1 Si7 33.67(15) . . ? O16 Cr1 O52 70.3(2) . . ? O16 Cr1 C69 88.7(3) . . ? O16 Cr1 C68 89.4(3) . . ? O31 Cr1 Si7 129.87(16) . . ? O31 Cr1 O16 96.3(2) . . ? O31 Cr1 O47 98.5(2) . . ? O31 Cr1 O52 166.5(2) . . ? O31 Cr1 C69 89.6(3) . . ? O31 Cr1 C68 92.6(3) . . ? O47 Cr1 Si7 131.46(17) . . ? O47 Cr1 O16 165.1(2) . . ? O47 Cr1 O52 94.9(2) . . ? O47 Cr1 C69 89.5(3) . . ? O47 Cr1 C68 91.8(3) . . ? O52 Cr1 Si7 36.66(15) . . ? C69 Cr1 Si7 87.2(2) . . ? C69 Cr1 O52 88.6(3) . . ? C68 Cr1 Si7 90.1(2) . . ? C68 Cr1 O52 88.9(3) . . ? C68 Cr1 C69 177.3(3) . . ? O16 Si7 Cr1 44.59(19) . . ? O16 Si7 O52 97.8(3) . . ? O16 Si7 O3 110.7(4) . . ? O16 Si7 O5 126.9(4) . . ? O16 Si7 O6 109.0(4) . . ? O52 Si7 Cr1 53.24(19) . . ? O52 Si7 O3 94.4(4) . . ? O52 Si7 O6 94.6(4) . . ? O3 Si7 Cr1 108.0(3) . . ? O4 Si7 Cr1 144.7(4) . . ? O4 Si7 O16 123.8(5) . . ? O4 Si7 O52 122.9(5) . . ? O4 Si7 O6 104.7(5) . . ? O5 Si7 Cr1 152.3(3) . . ? O5 Si7 O52 122.9(5) . . ? O5 Si7 O3 99.5(4) . . ? O6 Si7 Cr1 110.5(3) . . ? O19 Si18 O22 104.9(3) . . ? O19 Si18 O2 105.1(5) . . ? O31 Si18 O19 116.1(3) . . ? O31 Si18 O22 108.0(3) . . ? O31 Si18 O2 109.9(5) . . ? O22 Si18 O2 112.9(6) . . ? O1 Si18 O19 106.8(7) . . ? O1 Si18 O31 115.1(9) . . ? O1 Si18 O22 105.0(9) . . ? O33 Si32 O7 107.4(5) . . ? O47 Si32 O33 106.9(3) . . ? O47 Si32 O41 115.8(3) . . ? O47 Si32 O7 112.7(5) . . ? O47 Si32 O8 115.9(7) . . ? O41 Si32 O33 105.0(3) . . ? O41 Si32 O7 108.5(5) . . ? O41 Si32 O8 100.7(7) . . ? O8 Si32 O33 112.1(8) . . ? C34 O33 Si32 133.1(6) . . ? Si7 O16 Cr1 101.7(3) . . ? C20 O19 Si18 132.9(5) . . ? Si18 O31 Cr1 146.3(3) . . ? Si32 O47 Cr1 161.8(3) . . ? C42 O41 Si32 130.4(6) . . ? C23 O22 Si18 132.1(5) . . ? C69 N54 C48 175.5(8) . . ? Si7 O52 Cr1 90.1(2) . . ? C12 O52 Cr1 137.3(5) . . ? C12 O52 Si7 132.6(5) . . ? C68 N66 C58 176.2(8) . . ? N66 C58 C59 119.5(7) . . ? N66 C58 C63 117.4(7) . . ? C59 C58 C63 123.1(7) . . ? O19 C20 C21 110.8(6) . . ? O19 C20 C27 108.1(6) . . ? O19 C20 C28 105.3(6) . . ? C27 C20 C21 110.9(7) . . ? C27 C20 C28 111.7(7) . . ? C28 C20 C21 109.9(7) . . ? N54 C69 Cr1 176.2(7) . . ? C58 C59 C66 122.0(8) . . ? C60 C59 C58 118.2(8) . . ? C60 C59 C66 119.8(8) . . ? N54 C48 C49 117.7(7) . . ? C53 C48 N54 119.7(7) . . ? C53 C48 C49 122.6(7) . . ? H73A C73 H73B 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C53 C73 H73A 109.5 . . ? C53 C73 H73B 109.5 . . ? C53 C73 H73C 109.5 . . ? C48 C53 C73 120.5(7) . . ? C52 C53 C48 118.2(8) . . ? C52 C53 C73 121.4(7) . . ? C58 C63 C62 116.9(8) . . ? C58 C63 C67 121.8(7) . . ? C62 C63 C67 121.2(8) . . ? C63 C62 H62 119.5 . . ? C61 C62 C63 121.0(8) . . ? C61 C62 H62 119.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C34 C40 H40A 109.5 . . ? C34 C40 H40B 109.5 . . ? C34 C40 H40C 109.5 . . ? N66 C68 Cr1 175.7(7) . . ? C59 C60 H60 120.0 . . ? C59 C60 C61 120.0(8) . . ? C61 C60 H60 120.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C63 C67 H67A 109.5 . . ? C63 C67 H67B 109.5 . . ? C63 C67 H67C 109.5 . . ? H67A C67 H67B 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? C20 C27 H27A 109.5 . . ? C20 C27 H27B 109.5 . . ? C20 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C50 C51 C52 119.9(8) . . ? O22 C23 C25 112.5(7) . . ? O22 C23 C26 108.1(6) . . ? O22 C23 C24 105.5(6) . . ? C25 C23 C26 110.1(7) . . ? C25 C23 C24 109.9(7) . . ? C26 C23 C24 110.7(8) . . ? O52 C12 C15 106.7(7) . . ? O52 C12 C13 105.6(7) . . ? O52 C12 C14 110.4(7) . . ? C15 C12 C13 111.7(8) . . ? C15 C12 C14 111.0(8) . . ? C14 C12 C13 111.2(8) . . ? C53 C52 C51 120.2(8) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C51 C50 H50 118.7 . . ? C51 C50 C49 122.7(9) . . ? C49 C50 H50 118.7 . . ? C62 C61 C60 120.9(8) . . ? C62 C61 H61 119.6 . . ? C60 C61 H61 119.6 . . ? C48 C49 C57 120.5(8) . . ? C50 C49 C48 116.4(8) . . ? C50 C49 C57 123.1(8) . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? H43A C43 H43B 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? O33 C34 C40 111.0(7) . . ? O33 C34 C35 107.5(7) . . ? O33 C34 C46 106.3(9) . . ? C40 C34 C35 109.4(9) . . ? C46 C34 C40 111.0(8) . . ? C46 C34 C35 111.6(10) . . ? C59 C66 H66A 109.5 . . ? C59 C66 H66B 109.5 . . ? C59 C66 H66C 109.5 . . ? H66A C66 H66B 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O41 C42 C43 110.7(7) . . ? O41 C42 C45 107.6(7) . . ? O41 C42 C44 104.1(9) . . ? C43 C42 C44 110.4(8) . . ? C45 C42 C43 112.6(9) . . ? C45 C42 C44 111.1(9) . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C49 C57 H57A 109.5 . . ? C49 C57 H57B 109.5 . . ? C49 C57 H57C 109.5 . . ? H57A C57 H57B 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C20 C28 H28A 109.5 . . ? C20 C28 H28B 109.5 . . ? C20 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C46 H46A 109.5 . . ? C34 C46 H46B 109.5 . . ? C34 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C4AA O2 Si18 133.7(8) . . ? O2 C4AA C7 104.8 . . ? O2 C4AA C8 109.5 . . ? O2 C4AA C11 109.6 . . ? C7 C4AA C8 110.9 . . ? C7 C4AA C11 110.9 . . ? C8 C4AA C11 110.9 . . ? C4AA C7 H7A 109.5 . . ? C4AA C7 H7B 109.5 . . ? C4AA C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4AA C8 H8A 109.5 . . ? C4AA C8 H8B 109.5 . . ? C4AA C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4AA C11 H11A 109.5 . . ? C4AA C11 H11B 109.5 . . ? C4AA C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C16 O1 Si18 139.3(12) . . ? O1 C16 C18 104.8 . . ? O1 C16 C19 109.6 . . ? O1 C16 C1A 109.6 . . ? C18 C16 C19 110.9 . . ? C18 C16 C1A 110.9 . . ? C19 C16 C1A 110.9 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C1A H1AA 109.5 . . ? C16 C1A H1AB 109.5 . . ? C16 C1A H1AC 109.5 . . ? H1AA C1A H1AB 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C1AA O3 Si7 132.9(7) . . ? O3 C1AA C1B 104.8 . . ? O3 C1AA C1C 109.5 . . ? O3 C1AA C1D 109.6 . . ? C1B C1AA C1C 110.9 . . ? C1B C1AA C1D 110.9 . . ? C1D C1AA C1C 111.0 . . ? C1AA C1B H1BA 109.5 . . ? C1AA C1B H1BB 109.5 . . ? C1AA C1B H1BC 109.5 . . ? H1BA C1B H1BB 109.5 . . ? H1BA C1B H1BC 109.5 . . ? H1BB C1B H1BC 109.5 . . ? C1AA C1C H1CA 109.5 . . ? C1AA C1C H1CB 109.5 . . ? C1AA C1C H1CC 109.5 . . ? H1CA C1C H1CB 109.5 . . ? H1CA C1C H1CC 109.5 . . ? H1CB C1C H1CC 109.5 . . ? C1AA C1D H1DA 109.5 . . ? C1AA C1D H1DB 109.5 . . ? C1AA C1D H1DC 109.5 . . ? H1DA C1D H1DB 109.5 . . ? H1DA C1D H1DC 109.5 . . ? H1DB C1D H1DC 109.5 . . ? C2AA O4 Si7 136.6(7) . . ? O4 C2AA C5AA 104.8 . . ? O4 C2AA C17 109.5 . . ? O4 C2AA C1E 109.6 . . ? C5AA C2AA C17 111.0 . . ? C5AA C2AA C1E 110.9 . . ? C1E C2AA C17 110.9 . . ? C2AA C5AA H5AA 109.5 . . ? C2AA C5AA H5AB 109.5 . . ? C2AA C5AA H5AC 109.5 . . ? H5AA C5AA H5AB 109.5 . . ? H5AA C5AA H5AC 109.5 . . ? H5AB C5AA H5AC 109.5 . . ? C2AA C17 H17A 109.5 . . ? C2AA C17 H17B 109.5 . . ? C2AA C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C2AA C1E H1EA 109.5 . . ? C2AA C1E H1EB 109.5 . . ? C2AA C1E H1EC 109.5 . . ? H1EA C1E H1EB 109.5 . . ? H1EA C1E H1EC 109.5 . . ? H1EB C1E H1EC 109.5 . . ? C1F O5 Si7 130.2(6) . . ? O5 C1F C1G 104.8 . . ? O5 C1F C1H 109.5 . . ? O5 C1F C1I 109.5 . . ? C1G C1F C1H 110.9 . . ? C1G C1F C1I 110.9 . . ? C1I C1F C1H 110.9 . . ? C1F C1G H1GA 109.5 . . ? C1F C1G H1GB 109.5 . . ? C1F C1G H1GC 109.5 . . ? H1GA C1G H1GB 109.5 . . ? H1GA C1G H1GC 109.5 . . ? H1GB C1G H1GC 109.5 . . ? C1F C1H H1HA 109.5 . . ? C1F C1H H1HB 109.5 . . ? C1F C1H H1HC 109.5 . . ? H1HA C1H H1HB 109.5 . . ? H1HA C1H H1HC 109.5 . . ? H1HB C1H H1HC 109.5 . . ? C1F C1I H1IA 109.5 . . ? C1F C1I H1IB 109.5 . . ? C1F C1I H1IC 109.5 . . ? H1IA C1I H1IB 109.5 . . ? H1IA C1I H1IC 109.5 . . ? H1IB C1I H1IC 109.5 . . ? C1J O6 Si7 135.2(5) . . ? O6 C1J C1K 104.8 . . ? O6 C1J C1L 109.5 . . ? O6 C1J C1M 109.5 . . ? C1K C1J C1L 110.9 . . ? C1K C1J C1M 110.9 . . ? C1L C1J C1M 111.0 . . ? C1J C1K H1KA 109.5 . . ? C1J C1K H1KB 109.5 . . ? C1J C1K H1KC 109.5 . . ? H1KA C1K H1KB 109.5 . . ? H1KA C1K H1KC 109.5 . . ? H1KB C1K H1KC 109.5 . . ? C1J C1L H1LA 109.5 . . ? C1J C1L H1LB 109.5 . . ? C1J C1L H1LC 109.5 . . ? H1LA C1L H1LB 109.5 . . ? H1LA C1L H1LC 109.5 . . ? H1LB C1L H1LC 109.5 . . ? C1J C1M H1MA 109.5 . . ? C1J C1M H1MB 109.5 . . ? C1J C1M H1MC 109.5 . . ? H1MA C1M H1MB 109.5 . . ? H1MA C1M H1MC 109.5 . . ? H1MB C1M H1MC 109.5 . . ? C3AA O7 Si32 131.3(9) . . ? O7 C3AA C9 104.8 . . ? O7 C3AA C10 109.5 . . ? O7 C3AA C1N 109.5 . . ? C9 C3AA C10 110.9 . . ? C9 C3AA C1N 110.9 . . ? C1N C3AA C10 110.9 . . ? C3AA C9 H9A 109.5 . . ? C3AA C9 H9B 109.5 . . ? C3AA C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C3AA C10 H10A 109.5 . . ? C3AA C10 H10B 109.5 . . ? C3AA C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3AA C1N H1NA 109.5 . . ? C3AA C1N H1NB 109.5 . . ? C3AA C1N H1NC 109.5 . . ? H1NA C1N H1NB 109.5 . . ? H1NA C1N H1NC 109.5 . . ? H1NB C1N H1NC 109.5 . . ? C0AA O8 Si32 127.6(14) . . ? O8 C0AA C1O 104.8 . . ? O8 C0AA C1P 109.5 . . ? O8 C0AA C1Q 109.5 . . ? C1O C0AA C1P 110.9 . . ? C1O C0AA C1Q 110.9 . . ? C1Q C0AA C1P 110.9 . . ? C0AA C1O H1OA 109.5 . . ? C0AA C1O H1OB 109.5 . . ? C0AA C1O H1OC 109.5 . . ? H1OA C1O H1OB 109.5 . . ? H1OA C1O H1OC 109.5 . . ? H1OB C1O H1OC 109.5 . . ? C0AA C1P H1PA 109.5 . . ? C0AA C1P H1PB 109.5 . . ? C0AA C1P H1PC 109.5 . . ? H1PA C1P H1PB 109.5 . . ? H1PA C1P H1PC 109.5 . . ? H1PB C1P H1PC 109.5 . . ? C0AA C1Q H1QA 109.5 . . ? C0AA C1Q H1QB 109.5 . . ? C0AA C1Q H1QC 109.5 . . ? H1QA C1Q H1QB 109.5 . . ? H1QA C1Q H1QC 109.5 . . ? H1QB C1Q H1QC 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cr1 Si7 O52 C12 179.6(9) . . . . ? Cr1 Si7 O3 C1AA -135.0(8) . . . . ? Cr1 Si7 O4 C2AA -18.9(16) . . . . ? Cr1 Si7 O5 C1F 21.5(15) . . . . ? Cr1 Si7 O6 C1J 147.5(6) . . . . ? Cr1 O52 C12 C15 61.4(10) . . . . ? Cr1 O52 C12 C13 -57.6(11) . . . . ? Cr1 O52 C12 C14 -177.8(7) . . . . ? Si7 Cr1 O31 Si18 47.9(6) . . . . ? Si7 O52 C12 C15 -118.0(8) . . . . ? Si7 O52 C12 C13 123.0(8) . . . . ? Si7 O52 C12 C14 2.8(12) . . . . ? Si7 O3 C1AA C1B 161.1(10) . . . . ? Si7 O3 C1AA C1C -79.9(10) . . . . ? Si7 O3 C1AA C1D 42.1(10) . . . . ? Si7 O4 C2AA C5AA 65.2(12) . . . . ? Si7 O4 C2AA C17 -175.7(12) . . . . ? Si7 O4 C2AA C1E -53.8(12) . . . . ? Si7 O5 C1F C1G -156.2(9) . . . . ? Si7 O5 C1F C1H -37.1(9) . . . . ? Si7 O5 C1F C1I 84.8(9) . . . . ? Si7 O6 C1J C1K 73.5(8) . . . . ? Si7 O6 C1J C1L -167.4(8) . . . . ? Si7 O6 C1J C1M -45.5(8) . . . . ? Si18 O19 C20 C21 24.2(9) . . . . ? Si18 O19 C20 C27 -97.6(7) . . . . ? Si18 O19 C20 C28 143.0(6) . . . . ? Si18 O22 C23 C25 -32.9(10) . . . . ? Si18 O22 C23 C26 88.9(9) . . . . ? Si18 O22 C23 C24 -152.7(7) . . . . ? Si18 O2 C4AA C7 -71.5(11) . . . . ? Si18 O2 C4AA C8 47.5(11) . . . . ? Si18 O2 C4AA C11 169.4(11) . . . . ? Si18 O1 C16 C18 -39(2) . . . . ? Si18 O1 C16 C19 80(2) . . . . ? Si18 O1 C16 C1A -158(2) . . . . ? Si32 O33 C34 C40 -33.4(11) . . . . ? Si32 O33 C34 C35 86.2(11) . . . . ? Si32 O33 C34 C46 -154.2(7) . . . . ? Si32 O41 C42 C43 36.0(10) . . . . ? Si32 O41 C42 C45 -87.5(10) . . . . ? Si32 O41 C42 C44 154.5(6) . . . . ? Si32 O7 C3AA C9 -160.4(11) . . . . ? Si32 O7 C3AA C10 -41.4(11) . . . . ? Si32 O7 C3AA C1N 80.5(11) . . . . ? Si32 O8 C0AA C1O -162.4(16) . . . . ? Si32 O8 C0AA C1P -43.3(16) . . . . ? Si32 O8 C0AA C1Q 78.6(16) . . . . ? O33 Si32 O47 Cr1 109.6(11) . . . . ? O33 Si32 O41 C42 151.7(6) . . . . ? O33 Si32 O7 C3AA 71.4(11) . . . . ? O33 Si32 O8 C0AA 88.8(14) . . . . ? O16 Cr1 O31 Si18 45.2(6) . . . . ? O16 Si7 O52 Cr1 -2.3(3) . . . . ? O16 Si7 O52 C12 177.3(8) . . . . ? O16 Si7 O3 C1AA -87.7(9) . . . . ? O16 Si7 O4 C2AA 38.6(13) . . . . ? O16 Si7 O5 C1F -39.4(11) . . . . ? O16 Si7 O6 C1J 100.0(7) . . . . ? O19 Si18 O31 Cr1 -25.7(7) . . . . ? O19 Si18 O22 C23 -38.7(8) . . . . ? O19 Si18 O2 C4AA 179.4(10) . . . . ? O19 Si18 O1 C16 -179.3(17) . . . . ? O31 Si18 O19 C20 -81.4(6) . . . . ? O31 Si18 O22 C23 -163.1(7) . . . . ? O31 Si18 O2 C4AA -55.0(12) . . . . ? O31 Si18 O1 C16 -49(2) . . . . ? O47 Cr1 O31 Si18 -136.6(6) . . . . ? O47 Si32 O33 C34 -169.9(7) . . . . ? O47 Si32 O41 C42 -90.6(7) . . . . ? O47 Si32 O7 C3AA -46.0(11) . . . . ? O47 Si32 O8 C0AA -34.2(16) . . . . ? O41 Si32 O33 C34 -46.3(8) . . . . ? O41 Si32 O47 Cr1 -7.0(12) . . . . ? O41 Si32 O7 C3AA -175.6(9) . . . . ? O41 Si32 O8 C0AA -160.0(13) . . . . ? O22 Si18 O19 C20 159.6(6) . . . . ? O22 Si18 O31 Cr1 91.7(6) . . . . ? O22 Si18 O2 C4AA 65.6(12) . . . . ? O22 Si18 O1 C16 70(2) . . . . ? N54 C48 C53 C73 2.0(11) . . . . ? N54 C48 C53 C52 -178.1(7) . . . . ? N54 C48 C49 C50 178.3(7) . . . . ? N54 C48 C49 C57 -4.6(12) . . . . ? O52 Cr1 O31 Si18 51.6(13) . . . . ? O52 Si7 O16 Cr1 2.7(4) . . . . ? O52 Si7 O3 C1AA 172.3(9) . . . . ? O52 Si7 O4 C2AA -90.2(12) . . . . ? O52 Si7 O5 C1F 94.0(9) . . . . ? O52 Si7 O6 C1J -160.2(7) . . . . ? N66 C58 C59 C60 177.6(7) . . . . ? N66 C58 C59 C66 -1.1(12) . . . . ? N66 C58 C63 C62 -178.3(7) . . . . ? N66 C58 C63 C67 0.6(12) . . . . ? C58 C59 C60 C61 0.7(12) . . . . ? C58 C63 C62 C61 0.8(12) . . . . ? C69 Cr1 O31 Si18 133.9(6) . . . . ? C59 C58 C63 C62 -0.9(12) . . . . ? C59 C58 C63 C67 178.1(8) . . . . ? C59 C60 C61 C62 -0.7(12) . . . . ? C48 C53 C52 C51 -0.7(11) . . . . ? C73 C53 C52 C51 179.3(8) . . . . ? C53 C48 C49 C50 -3.0(11) . . . . ? C53 C48 C49 C57 174.2(8) . . . . ? C63 C58 C59 C60 0.1(12) . . . . ? C63 C58 C59 C66 -178.5(8) . . . . ? C63 C62 C61 C60 0.0(13) . . . . ? C68 Cr1 O31 Si18 -44.4(6) . . . . ? C67 C63 C62 C61 -178.1(8) . . . . ? C51 C50 C49 C48 0.2(13) . . . . ? C51 C50 C49 C57 -176.9(9) . . . . ? C52 C51 C50 C49 2.2(14) . . . . ? C50 C51 C52 C53 -2.0(13) . . . . ? C49 C48 C53 C73 -176.7(7) . . . . ? C49 C48 C53 C52 3.2(11) . . . . ? C66 C59 C60 C61 179.4(8) . . . . ? O2 Si18 O19 C20 40.3(8) . . . . ? O2 Si18 O31 Cr1 -144.7(7) . . . . ? O2 Si18 O22 C23 75.2(9) . . . . ? O1 Si18 O19 C20 48.5(11) . . . . ? O1 Si18 O31 Cr1 -151.4(9) . . . . ? O1 Si18 O22 C23 73.7(10) . . . . ? O3 Si7 O16 Cr1 -95.1(4) . . . . ? O3 Si7 O52 Cr1 109.2(4) . . . . ? O3 Si7 O52 C12 -71.2(9) . . . . ? O3 Si7 O5 C1F -164.4(8) . . . . ? O4 Si7 O16 Cr1 -136.0(5) . . . . ? O4 Si7 O52 Cr1 136.9(4) . . . . ? O4 Si7 O52 C12 -43.5(10) . . . . ? O4 Si7 O6 C1J -34.4(9) . . . . ? O5 Si7 O16 Cr1 144.6(5) . . . . ? O5 Si7 O52 Cr1 -146.4(4) . . . . ? O5 Si7 O52 C12 33.2(10) . . . . ? O5 Si7 O3 C1AA 47.9(10) . . . . ? O6 Si7 O16 Cr1 100.3(4) . . . . ? O6 Si7 O52 Cr1 -112.3(4) . . . . ? O6 Si7 O52 C12 67.3(9) . . . . ? O6 Si7 O4 C2AA 164.2(11) . . . . ? O7 Si32 O33 C34 69.0(9) . . . . ? O7 Si32 O47 Cr1 -132.7(12) . . . . ? O7 Si32 O41 C42 37.2(8) . . . . ? O8 Si32 O33 C34 62.1(10) . . . . ? O8 Si32 O47 Cr1 -124.6(14) . . . . ? O8 Si32 O41 C42 35.2(10) . . . . ? _shelx_res_file ; TITL yyk_criii_crtbos3xync2_auto_a.res in P2(1)2(1)2(1) yyk_criii_crtbos3xync2_auto.res created by SHELXL-2018/3 at 20:32:11 on 25-Jul-2023 REM Old TITL YYK_CrIII_CrTBOS3XyNC2_auto in P2(1)2(1)2 REM SHELXT solution in P2(1)2(1)2(1): R1 0.143, Rweak 0.104, Alpha 0.017 REM 4.994 for 32 systematic absences, Orientation as input REM Flack x = 0.118 ( 0.004 ) from 4385 Parsons' quotients REM Formula found by SHELXT: C58 C68 O22 Si32 Cr CELL 1.54184 13.190684 20.836193 23.444897 90 90 90 ZERR 4 0.000279 0.00049 0.000566 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 Cr N O Si UNIT 216 396 4 8 48 12 RIGU C7 C8 C11 C4AA O2 Si18 RIGU O8 C0AA C1Q C1P C1O Si32 RIGU 0.001 0.001 C16 C18 C1A C19 O1 Si18 RIGU C1M C1L C1J C1K O6 Si7 RIGU C1G C1H C1I C1F O5 Si7 RIGU O3 C1AA C1D C1B C1C Si7 RIGU O7 C3AA C1N C10 C9 RIGU C2AA C1E C17 C5AA O4 Si7 RIGU C7 C18 C19 RIGU 0.002 0.002 RIGU 0.001 0.001 C18 C7 L.S. 20 PLAN 20 TEMP -173 CONF MORE -1 BOND $H fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.000000 31.774799 BASF 0.06800 FVAR 1.87824 0.62283 0.50973 0.60248 CR1 3 0.345454 0.512384 0.610266 11.00000 0.01703 0.02102 = 0.02850 -0.00103 0.00259 0.00028 SI7 6 0.477459 0.549816 0.524580 11.00000 0.02942 0.02948 = 0.02157 0.00108 0.00424 0.00105 SI18 6 0.217329 0.624459 0.680544 11.00000 0.02774 0.02256 = 0.02322 -0.00006 0.00458 0.00051 SI32 6 0.231417 0.369575 0.646182 11.00000 0.02203 0.02179 = 0.02625 0.00052 -0.00231 -0.00036 O33 5 0.267588 0.312813 0.602125 11.00000 0.03757 0.02278 = 0.03118 -0.00346 -0.00674 0.00121 O16 5 0.413621 0.585295 0.571413 11.00000 0.02563 0.02108 = 0.03581 -0.00088 0.00705 -0.00277 O19 5 0.230995 0.683876 0.636414 11.00000 0.02292 0.02446 = 0.02522 0.00264 0.00182 -0.00318 O31 5 0.281081 0.561771 0.666865 11.00000 0.02095 0.02486 = 0.02714 0.00027 -0.00362 -0.00053 O47 5 0.300609 0.429272 0.634301 11.00000 0.02425 0.02341 = 0.03092 -0.00148 -0.00158 -0.00081 O41 5 0.110834 0.379415 0.633525 11.00000 0.02383 0.03057 = 0.04167 0.00699 -0.00348 0.00007 O22 5 0.097354 0.605853 0.677041 11.00000 0.02757 0.02658 = 0.05172 0.00775 0.01405 0.00596 N54 4 0.545686 0.501749 0.693593 11.00000 0.01854 0.03109 = 0.04261 -0.00025 0.00054 -0.00024 O52 5 0.438590 0.475946 0.538372 11.00000 0.04719 0.02804 = 0.05105 -0.00848 0.03275 -0.00205 N66 4 0.158910 0.528419 0.520213 11.00000 0.03309 0.03434 = 0.02460 0.00076 -0.00361 -0.00349 C58 1 0.086764 0.534603 0.477190 11.00000 0.02885 0.03589 = 0.02441 0.00174 -0.00336 -0.00419 C20 1 0.307031 0.733431 0.630639 11.00000 0.02313 0.02197 = 0.02659 -0.00179 0.00244 -0.00455 C69 1 0.476208 0.503082 0.664644 11.00000 0.02123 0.02688 = 0.04303 -0.00153 -0.00009 0.00033 C59 1 0.066068 0.595174 0.454570 11.00000 0.03206 0.03348 = 0.02773 0.00177 0.00868 0.00391 C48 1 0.627038 0.503670 0.731781 11.00000 0.02084 0.03522 = 0.02704 0.00143 0.00369 -0.00787 C73 1 0.671210 0.390451 0.702440 11.00000 0.02717 0.03895 = 0.04413 -0.00429 -0.00926 0.00064 AFIX 137 H73A 2 0.603288 0.373580 0.710316 11.00000 -1.50000 H73B 2 0.722007 0.357874 0.712041 11.00000 -1.50000 H73C 2 0.676677 0.401374 0.661899 11.00000 -1.50000 AFIX 0 C53 1 0.689210 0.449932 0.738046 11.00000 0.01969 0.03601 = 0.03142 0.00301 0.00541 -0.00696 C63 1 0.041011 0.478348 0.457159 11.00000 0.03369 0.03687 = 0.02554 0.00210 -0.00681 -0.00680 C62 1 -0.029645 0.484957 0.412691 11.00000 0.02958 0.04518 = 0.03011 -0.00479 -0.00559 -0.00016 AFIX 43 H62 2 -0.063006 0.447972 0.398227 11.00000 -1.20000 AFIX 0 C40 1 0.172130 0.221121 0.638404 11.00000 0.05187 0.02267 = 0.05494 0.00218 -0.01715 -0.00716 AFIX 137 H40A 2 0.221666 0.212692 0.668643 11.00000 -1.50000 H40B 2 0.140708 0.180650 0.626528 11.00000 -1.50000 H40C 2 0.119746 0.250316 0.652736 11.00000 -1.50000 AFIX 0 C68 1 0.222572 0.521714 0.553852 11.00000 0.03315 0.02850 = 0.02334 0.00108 -0.00386 -0.00150 C60 1 -0.003426 0.599482 0.410175 11.00000 0.03401 0.04408 = 0.02909 0.00475 0.00672 0.00575 AFIX 43 H60 2 -0.018450 0.640024 0.393675 11.00000 -1.20000 AFIX 0 C21 1 0.406919 0.712084 0.656508 11.00000 0.02953 0.02732 = 0.07303 0.00130 -0.01717 -0.00373 AFIX 137 H21A 2 0.397487 0.703432 0.697251 11.00000 -1.50000 H21B 2 0.457551 0.746062 0.651623 11.00000 -1.50000 H21C 2 0.430241 0.672968 0.637362 11.00000 -1.50000 AFIX 0 C67 1 0.067117 0.413851 0.481055 11.00000 0.05424 0.03771 = 0.03641 0.00833 -0.01675 -0.00698 AFIX 137 H67A 2 0.138069 0.403851 0.472410 11.00000 -1.50000 H67B 2 0.023117 0.381222 0.463922 11.00000 -1.50000 H67C 2 0.057266 0.414232 0.522485 11.00000 -1.50000 AFIX 0 C25 1 0.017586 0.708778 0.702158 11.00000 0.03314 0.03570 = 0.04518 -0.00537 0.00688 0.01251 AFIX 137 H25A 2 0.028504 0.701606 0.743010 11.00000 -1.50000 H25B 2 -0.044496 0.733855 0.696631 11.00000 -1.50000 H25C 2 0.075397 0.732300 0.686273 11.00000 -1.50000 AFIX 0 C27 1 0.268231 0.792959 0.659632 11.00000 0.04001 0.02255 = 0.05337 -0.00717 0.01096 -0.00462 AFIX 137 H27A 2 0.205338 0.806929 0.641166 11.00000 -1.50000 H27B 2 0.319113 0.827071 0.656699 11.00000 -1.50000 H27C 2 0.254962 0.783660 0.699921 11.00000 -1.50000 AFIX 0 C26 1 -0.013982 0.654957 0.608964 11.00000 0.03405 0.03859 = 0.04338 -0.00256 0.00531 0.00356 AFIX 137 H26A 2 0.041395 0.679776 0.591935 11.00000 -1.50000 H26B 2 -0.077839 0.678464 0.604493 11.00000 -1.50000 H26C 2 -0.019211 0.613283 0.589811 11.00000 -1.50000 AFIX 0 C51 1 0.782233 0.509204 0.809380 11.00000 0.03364 0.05624 = 0.04263 -0.00369 -0.00160 -0.01851 AFIX 43 H51 2 0.834405 0.510590 0.837287 11.00000 -1.20000 AFIX 0 C23 1 0.007295 0.644633 0.672057 11.00000 0.02762 0.02671 = 0.04160 0.00304 0.00971 0.00776 C12 1 0.460009 0.414222 0.511618 11.00000 0.04630 0.02755 = 0.03578 -0.00329 0.01060 0.00910 C52 1 0.766403 0.452798 0.777119 11.00000 0.02784 0.04561 = 0.02790 0.00556 -0.00101 -0.00767 AFIX 43 H52 2 0.809407 0.416735 0.782526 11.00000 -1.20000 AFIX 0 C50 1 0.722755 0.561398 0.800419 11.00000 0.04154 0.04589 = 0.05016 -0.00567 0.00216 -0.02127 AFIX 43 H50 2 0.736100 0.599385 0.821532 11.00000 -1.20000 AFIX 0 C61 1 -0.051218 0.544167 0.389802 11.00000 0.03248 0.04927 = 0.02984 0.00113 0.00124 0.00649 AFIX 43 H61 2 -0.099231 0.547522 0.359747 11.00000 -1.20000 AFIX 0 C49 1 0.643860 0.561509 0.761965 11.00000 0.03327 0.03622 = 0.04394 -0.00581 0.01088 -0.01373 C15 1 0.361700 0.389339 0.489528 11.00000 0.05742 0.03034 = 0.03544 -0.00378 0.00291 0.00441 AFIX 137 H15A 2 0.312731 0.386609 0.520869 11.00000 -1.50000 H15B 2 0.371935 0.346595 0.473066 11.00000 -1.50000 H15C 2 0.335754 0.418442 0.460114 11.00000 -1.50000 AFIX 0 C43 1 0.067291 0.452170 0.711362 11.00000 0.05457 0.03316 = 0.05425 0.00962 0.02975 0.00436 AFIX 137 H43A 2 0.120398 0.434135 0.735807 11.00000 -1.50000 H43B 2 0.010961 0.467280 0.735079 11.00000 -1.50000 H43C 2 0.094989 0.488214 0.689492 11.00000 -1.50000 AFIX 0 C34 1 0.225827 0.251995 0.587178 11.00000 0.06598 0.02172 = 0.04897 -0.00313 -0.01181 -0.00550 C66 1 0.118846 0.655567 0.476268 11.00000 0.06295 0.03952 = 0.03486 -0.00277 0.00355 -0.00639 AFIX 137 H66A 2 0.144220 0.648073 0.514986 11.00000 -1.50000 H66B 2 0.070531 0.691293 0.476711 11.00000 -1.50000 H66C 2 0.175695 0.666134 0.451048 11.00000 -1.50000 AFIX 0 C13 1 0.502917 0.371126 0.559665 11.00000 0.05207 0.04559 = 0.03828 -0.00529 0.00745 0.02471 AFIX 137 H13A 2 0.575450 0.379777 0.564433 11.00000 -1.50000 H13B 2 0.493105 0.325914 0.549553 11.00000 -1.50000 H13C 2 0.467363 0.380400 0.595430 11.00000 -1.50000 AFIX 0 C14 1 0.536610 0.422366 0.463488 11.00000 0.05428 0.04377 = 0.05345 -0.00903 0.02872 0.00943 AFIX 137 H14A 2 0.507609 0.449819 0.433727 11.00000 -1.50000 H14B 2 0.553034 0.380261 0.447315 11.00000 -1.50000 H14C 2 0.598440 0.442256 0.478477 11.00000 -1.50000 AFIX 0 C42 1 0.029530 0.401073 0.670796 11.00000 0.02762 0.03287 = 0.07731 0.01310 0.01558 0.00301 C45 1 -0.011611 0.343116 0.701317 11.00000 0.03991 0.04293 = 0.10580 0.02393 0.02928 0.00052 AFIX 137 H45A 2 -0.035640 0.311722 0.673281 11.00000 -1.50000 H45B 2 -0.068040 0.356058 0.725954 11.00000 -1.50000 H45C 2 0.042057 0.323827 0.724590 11.00000 -1.50000 AFIX 0 C24 1 -0.077641 0.605200 0.699750 11.00000 0.02823 0.04531 = 0.08120 0.02202 0.02014 0.00823 AFIX 137 H24A 2 -0.090299 0.566597 0.676957 11.00000 -1.50000 H24B 2 -0.139605 0.631066 0.701594 11.00000 -1.50000 H24C 2 -0.057296 0.592737 0.738397 11.00000 -1.50000 AFIX 0 C57 1 0.580845 0.619936 0.749613 11.00000 0.03895 0.04005 = 0.10216 -0.01475 0.00638 -0.00437 AFIX 137 H57A 2 0.508811 0.608536 0.751069 11.00000 -1.50000 H57B 2 0.597497 0.636294 0.711559 11.00000 -1.50000 H57C 2 0.595117 0.653091 0.778153 11.00000 -1.50000 AFIX 0 C28 1 0.319240 0.743271 0.567284 11.00000 0.05707 0.04855 = 0.02997 0.00490 0.00518 -0.03125 AFIX 137 H28A 2 0.354345 0.706236 0.550736 11.00000 -1.50000 H28B 2 0.359019 0.782220 0.560343 11.00000 -1.50000 H28C 2 0.252292 0.747752 0.549604 11.00000 -1.50000 AFIX 0 C35 1 0.148210 0.263325 0.538769 11.00000 0.12528 0.03687 = 0.06676 0.01002 -0.05376 -0.03688 AFIX 137 H35A 2 0.092519 0.290033 0.552984 11.00000 -1.50000 H35B 2 0.121314 0.221985 0.525790 11.00000 -1.50000 H35C 2 0.181616 0.285135 0.506859 11.00000 -1.50000 AFIX 0 C46 1 0.313609 0.211103 0.567372 11.00000 0.11244 0.01908 = 0.06374 -0.01070 0.01807 0.00632 AFIX 137 H46A 2 0.345947 0.231385 0.534337 11.00000 -1.50000 H46B 2 0.288706 0.168476 0.556615 11.00000 -1.50000 H46C 2 0.363118 0.206924 0.598317 11.00000 -1.50000 AFIX 0 C44 1 -0.049896 0.429410 0.629648 11.00000 0.03259 0.05198 = 0.11037 0.02491 0.00020 0.00695 AFIX 137 H44A 2 -0.022501 0.468215 0.611750 11.00000 -1.50000 H44B 2 -0.111502 0.440264 0.650928 11.00000 -1.50000 H44C 2 -0.066172 0.397765 0.600112 11.00000 -1.50000 AFIX 6 PART 2 O2 5 0.250880 0.653645 0.743901 21.00000 0.06728 0.02498 = 0.02444 -0.00230 0.00184 -0.00925 C4AA 1 0.255378 0.626818 0.800391 21.00000 0.09309 0.04321 = 0.02216 -0.00205 0.00779 0.00696 C7 1 0.144507 0.619209 0.818441 21.00000 0.10432 0.15488 = 0.02067 0.01062 0.03370 0.01922 AFIX 137 H7A 2 0.111760 0.661418 0.819220 21.00000 -1.50000 H7B 2 0.141476 0.599907 0.856520 21.00000 -1.50000 H7C 2 0.109302 0.591430 0.791138 21.00000 -1.50000 AFIX 5 C8 1 0.308987 0.561407 0.798324 21.00000 0.09007 0.04401 = 0.05158 0.00676 -0.01355 0.00540 AFIX 137 H8A 2 0.274218 0.533408 0.771023 21.00000 -1.50000 H8B 2 0.307397 0.541695 0.836265 21.00000 -1.50000 H8C 2 0.379547 0.567391 0.786365 21.00000 -1.50000 AFIX 5 C11 1 0.311407 0.673339 0.840271 21.00000 0.17717 0.06507 = 0.04341 -0.01839 -0.02239 -0.00091 AFIX 137 H11A 2 0.384166 0.672173 0.831879 21.00000 -1.50000 H11B 2 0.300078 0.660549 0.879987 21.00000 -1.50000 H11C 2 0.285720 0.716972 0.834385 21.00000 -1.50000 AFIX 6 PART 0 PART 1 O1 5 0.232476 0.652201 0.741598 -21.00000 0.06080 0.02634 = 0.02330 0.00122 0.00513 -0.00728 C16 1 0.232918 0.630590 0.799867 -21.00000 0.04445 0.04370 = 0.02256 0.00336 0.00448 -0.00265 C18 1 0.146789 0.581489 0.803237 -21.00000 0.05276 0.05243 = 0.01147 0.01628 -0.00740 -0.01020 AFIX 137 H18A 2 0.081550 0.603548 0.799281 -21.00000 -1.50000 H18B 2 0.149328 0.559449 0.840136 -21.00000 -1.50000 H18C 2 0.154352 0.550037 0.772450 -21.00000 -1.50000 AFIX 5 C19 1 0.335369 0.599080 0.813516 -21.00000 0.04791 0.05563 = 0.03551 0.00352 0.00125 0.00171 AFIX 137 H19A 2 0.330837 0.552762 0.806713 -21.00000 -1.50000 H19B 2 0.352640 0.606873 0.853577 -21.00000 -1.50000 H19C 2 0.387989 0.617502 0.788966 -21.00000 -1.50000 AFIX 5 C1A 1 0.212608 0.687668 0.839749 -21.00000 0.06599 0.04661 = 0.02303 0.00153 0.00109 0.00293 AFIX 137 H1AA 2 0.258984 0.722856 0.830343 -21.00000 -1.50000 H1AB 2 0.223446 0.674403 0.879386 -21.00000 -1.50000 H1AC 2 0.142440 0.702154 0.834957 -21.00000 -1.50000 AFIX 6 PART 0 PART 2 O3 5 0.599849 0.536482 0.548197 31.00000 0.02445 0.05297 = 0.02573 0.00256 0.00622 0.00365 C1AA 1 0.690981 0.574391 0.546189 31.00000 0.02546 0.05881 = 0.04523 0.00578 -0.00201 -0.00072 C1B 1 0.760087 0.544949 0.591601 31.00000 0.03438 0.09385 = 0.07677 0.03803 -0.01848 -0.01704 AFIX 137 H1BA 2 0.733186 0.554719 0.629585 31.00000 -1.50000 H1BB 2 0.828413 0.562951 0.587928 31.00000 -1.50000 H1BC 2 0.762927 0.498319 0.586377 31.00000 -1.50000 AFIX 5 C1C 1 0.738985 0.568990 0.486690 31.00000 0.01366 0.08553 = 0.05849 0.01434 0.01196 0.00170 AFIX 137 H1CA 2 0.752663 0.523786 0.478082 31.00000 -1.50000 H1CB 2 0.802645 0.593221 0.485868 31.00000 -1.50000 H1CC 2 0.692273 0.586517 0.458161 31.00000 -1.50000 AFIX 5 C1D 1 0.665924 0.644541 0.560559 31.00000 0.04300 0.06355 = 0.09641 -0.02149 -0.00568 -0.00440 AFIX 137 H1DA 2 0.624939 0.663113 0.529850 31.00000 -1.50000 H1DB 2 0.728979 0.669002 0.564570 31.00000 -1.50000 H1DC 2 0.627867 0.646266 0.596426 31.00000 -1.50000 AFIX 6 PART 0 PART 1 O4 5 0.586659 0.565938 0.510702 -31.00000 0.01753 0.04195 = 0.02489 0.00391 -0.00272 0.00339 C2AA 1 0.675880 0.584000 0.542110 -31.00000 0.02298 0.06756 = 0.02647 0.00524 -0.00787 -0.00558 C5AA 1 0.700862 0.525381 0.578862 -31.00000 0.03875 0.12235 = 0.06941 0.05537 -0.01973 -0.00505 AFIX 137 H5AA 2 0.645184 0.517473 0.605631 -31.00000 -1.50000 H5AB 2 0.763487 0.533369 0.600202 -31.00000 -1.50000 H5AC 2 0.709909 0.487770 0.554285 -31.00000 -1.50000 AFIX 5 C17 1 0.762548 0.598658 0.500278 -31.00000 0.03314 0.08505 = 0.02639 0.00088 -0.00692 -0.02176 AFIX 137 H17A 2 0.791297 0.558315 0.486132 -31.00000 -1.50000 H17B 2 0.815350 0.623308 0.519895 -31.00000 -1.50000 H17C 2 0.736260 0.623698 0.468134 -31.00000 -1.50000 AFIX 5 C1E 1 0.652282 0.642651 0.579559 -31.00000 0.03857 0.12736 = 0.10452 -0.06948 -0.02062 -0.00052 AFIX 137 H1EA 2 0.635953 0.679435 0.555184 -31.00000 -1.50000 H1EB 2 0.711512 0.652889 0.603095 -31.00000 -1.50000 H1EC 2 0.594331 0.633036 0.604280 -31.00000 -1.50000 AFIX 6 PART 0 PART 2 O5 5 0.501291 0.574783 0.461182 31.00000 0.02002 0.04238 = 0.03209 0.00544 0.00346 0.00818 C1F 1 0.437509 0.608110 0.421141 31.00000 0.01664 0.03557 = 0.02355 -0.00425 0.00084 0.00440 C1G 1 0.483209 0.593097 0.362621 31.00000 0.04601 0.04624 = 0.02986 0.00013 0.01646 0.00442 AFIX 137 H1GA 2 0.553455 0.608347 0.361349 31.00000 -1.50000 H1GB 2 0.443619 0.614694 0.332911 31.00000 -1.50000 H1GC 2 0.481811 0.546641 0.356142 31.00000 -1.50000 AFIX 5 C1H 1 0.328620 0.582409 0.425532 31.00000 0.02245 0.06920 = 0.04529 0.01185 0.00117 -0.00381 AFIX 137 H1HA 2 0.328779 0.535863 0.419530 31.00000 -1.50000 H1HB 2 0.286325 0.602947 0.396415 31.00000 -1.50000 H1HC 2 0.301300 0.592022 0.463453 31.00000 -1.50000 AFIX 5 C1I 1 0.440947 0.680481 0.433437 31.00000 0.08295 0.03501 = 0.05276 -0.00957 -0.00602 0.00565 AFIX 137 H1IA 2 0.421759 0.688256 0.473224 31.00000 -1.50000 H1IB 2 0.393508 0.702801 0.408112 31.00000 -1.50000 H1IC 2 0.509767 0.696563 0.426823 31.00000 -1.50000 AFIX 6 PART 0 PART 1 O6 5 0.416313 0.554800 0.461791 -31.00000 0.02308 0.02992 = 0.02216 0.00550 0.00333 -0.00148 C1J 1 0.425464 0.594279 0.411691 -31.00000 0.03592 0.02938 = 0.01176 0.00331 0.00067 0.00199 C1K 1 0.520983 0.569948 0.381611 -31.00000 0.03683 0.04159 = 0.02380 0.00772 0.00710 0.00631 AFIX 137 H1KA 2 0.578774 0.572598 0.407774 -31.00000 -1.50000 H1KB 2 0.534343 0.596424 0.347890 -31.00000 -1.50000 H1KC 2 0.511001 0.525240 0.369906 -31.00000 -1.50000 AFIX 5 C1L 1 0.331563 0.585260 0.373801 -31.00000 0.03249 0.04682 = 0.01681 0.00386 0.00396 -0.00374 AFIX 137 H1LA 2 0.327201 0.540368 0.361574 -31.00000 -1.50000 H1LB 2 0.337003 0.613054 0.340219 -31.00000 -1.50000 H1LC 2 0.270566 0.596602 0.395431 -31.00000 -1.50000 AFIX 5 C1M 1 0.437536 0.664849 0.429470 -31.00000 0.04424 0.02687 = 0.01736 0.00473 0.00426 0.00457 AFIX 137 H1MA 2 0.376190 0.679093 0.449364 -31.00000 -1.50000 H1MB 2 0.448042 0.691363 0.395455 -31.00000 -1.50000 H1MC 2 0.496074 0.669099 0.454931 -31.00000 -1.50000 AFIX 6 PART 0 PART 2 O7 5 0.244623 0.341467 0.711566 41.00000 0.02086 0.02279 = 0.03159 0.00335 -0.00362 -0.00135 C3AA 1 0.333731 0.328290 0.744988 41.00000 0.01967 0.02984 = 0.02395 0.00036 -0.00107 -0.00615 C9 1 0.297769 0.282102 0.791509 41.00000 0.03860 0.03261 = 0.02581 0.00657 -0.00121 0.00315 AFIX 137 H9A 2 0.244009 0.302539 0.813926 41.00000 -1.50000 H9B 2 0.354766 0.271329 0.816554 41.00000 -1.50000 H9C 2 0.271496 0.242852 0.773847 41.00000 -1.50000 AFIX 5 C10 1 0.414614 0.296628 0.707131 41.00000 0.02792 0.03796 = 0.02482 0.00231 -0.00141 0.00246 AFIX 137 H10A 2 0.386191 0.258132 0.689216 41.00000 -1.50000 H10B 2 0.473196 0.284659 0.730535 41.00000 -1.50000 H10C 2 0.436038 0.326903 0.677500 41.00000 -1.50000 AFIX 5 C1N 1 0.373648 0.391021 0.771097 41.00000 0.04111 0.03831 = 0.03733 -0.00562 -0.00644 -0.01178 AFIX 137 H1NA 2 0.392313 0.420811 0.740501 41.00000 -1.50000 H1NB 2 0.433348 0.381840 0.794601 41.00000 -1.50000 H1NC 2 0.320744 0.410429 0.794841 41.00000 -1.50000 AFIX 6 PART 0 PART 1 O8 5 0.228006 0.344671 0.712325 -41.00000 0.02718 0.03137 = 0.02538 0.00063 -0.00638 0.00019 C0AA 1 0.308980 0.345530 0.753383 -41.00000 0.02546 0.03126 = 0.02438 0.00540 -0.00620 0.00016 C1O 1 0.275752 0.298400 0.799804 -41.00000 0.03780 0.03708 = 0.02872 0.00840 -0.00132 0.00290 AFIX 137 H1OA 2 0.204717 0.306444 0.809747 -41.00000 -1.50000 H1OB 2 0.318279 0.304211 0.833687 -41.00000 -1.50000 H1OC 2 0.282978 0.254357 0.785711 -41.00000 -1.50000 AFIX 5 C1P 1 0.407746 0.323108 0.724860 -41.00000 0.02551 0.05594 = 0.02970 0.00519 -0.00363 0.00272 AFIX 137 H1PA 2 0.402570 0.277372 0.715555 -41.00000 -1.50000 H1PB 2 0.464686 0.329909 0.751022 -41.00000 -1.50000 H1PC 2 0.418953 0.347749 0.689818 -41.00000 -1.50000 AFIX 5 C1Q 1 0.320674 0.413599 0.777703 -41.00000 0.02875 0.03500 = 0.04629 -0.00296 -0.01624 -0.00063 AFIX 137 H1QA 2 0.345103 0.442471 0.747703 -41.00000 -1.50000 H1QB 2 0.369475 0.412968 0.809216 -41.00000 -1.50000 H1QC 2 0.254904 0.428779 0.791702 -41.00000 -1.50000 AFIX 0 HKLF 4 REM yyk_criii_crtbos3xync2_auto_a.res in P2(1)2(1)2(1) REM wR2 = 0.1915, GooF = S = 1.104, Restrained GooF = 1.084 for all data REM R1 = 0.0835 for 13046 Fo > 4sig(Fo) and 0.0854 for all 13511 data REM 804 parameters refined using 773 restraints END WGHT 0.0000 32.0692 REM Highest difference peak 0.402, deepest hole -1.074, 1-sigma level 0.098 Q1 1 0.0433 0.5649 0.6176 11.00000 0.05 0.40 Q2 1 0.4058 0.4212 0.5719 11.00000 0.05 0.40 Q3 1 0.2801 0.6606 0.7467 11.00000 0.05 0.37 Q4 1 0.1842 0.6822 0.6747 11.00000 0.05 0.37 Q5 1 0.3917 0.5592 0.5748 11.00000 0.05 0.36 Q6 1 0.5987 0.2504 0.5927 11.00000 0.05 0.36 Q7 1 0.2452 0.4155 0.6435 11.00000 0.05 0.35 Q8 1 0.2510 0.5246 0.5811 11.00000 0.05 0.35 Q9 1 0.3063 0.4574 0.6330 11.00000 0.05 0.35 Q10 1 0.2165 0.5794 0.4414 11.00000 0.05 0.34 Q11 1 0.2133 0.4560 0.6235 11.00000 0.05 0.34 Q12 1 0.2662 0.4981 0.4807 11.00000 0.05 0.34 Q13 1 0.3026 0.7937 0.7037 11.00000 0.05 0.33 Q14 1 0.4610 0.5575 0.5611 11.00000 0.05 0.33 Q15 1 0.4338 0.5071 0.6433 11.00000 0.05 0.32 Q16 1 0.0137 0.3203 0.4927 11.00000 0.05 0.32 Q17 1 0.5068 0.3608 0.6499 11.00000 0.05 0.32 Q18 1 0.4326 0.6998 0.3860 11.00000 0.05 0.32 Q19 1 0.8463 0.4757 0.7428 11.00000 0.05 0.32 Q20 1 0.4100 0.2238 0.7663 11.00000 0.05 0.32 ; _shelx_res_checksum 25226 _olex2_exptl_crystal_mounting_method loop _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 1.598 _oxdiff_exptl_absorpt_empirical_full_min 0.525 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.932(11) 2 0.068(11) _chemical_properties_physical Air-sensitive,Moisture-sensitive,Oxygen-sensitive