#------------------------------------------------------------------------------ #$Date: 2021-09-23 01:11:52 +0300 (Thu, 23 Sep 2021) $ #$Revision: 269243 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/47/1564702.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1564702 loop_ _publ_author_name 'Yi, Xiaofeng' 'Wang, Di' 'Li, Fan' 'Zhang, Jian' 'Zhang, Lei' _publ_section_title ; Molecular Bixbyite-Like In12-Oxo Clusters with Tunable Functionalization Sites for Lithography Patterning Applications ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC04491E _journal_year 2021 _chemical_formula_moiety 'C36 H84 Cl4 In12 N8 O26, 2(Cl)' _chemical_formula_sum 'C36 H84 Cl6 In12 N8 O26' _chemical_formula_weight 2635.65 _chemical_name_systematic InOC-1 _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'I 2y' _space_group_name_H-M_alt 'I 1 2 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-01-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-04-19 deposited with the CCDC. 2021-09-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.1940(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 16.05120(10) _cell_length_b 11.42060(10) _cell_length_c 20.21170(10) _cell_measurement_reflns_used 38558 _cell_measurement_temperature 297.99(16) _cell_measurement_theta_max 64.0050 _cell_measurement_theta_min 3.7910 _cell_volume 3705.07(4) _computing_cell_refinement 'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment air _diffrn_ambient_temperature 297.99(16) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.991 _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 -15.00 73.00 0.50 0.05 -- -0.94 38.00 -30.00 176 2 \w -74.00 14.00 0.50 0.05 -- -0.94 -38.00 60.00 176 3 \w -17.00 72.00 0.50 0.05 -- -0.94 57.00-150.00 178 4 \w 8.00 106.00 0.50 0.05 -- 80.41 -99.00 30.00 196 5 \w 20.00 111.00 0.50 0.05 -- 80.41-125.00-180.00 182 6 \w 8.00 104.00 0.50 0.05 -- 80.41 -77.00-180.00 192 7 \w 8.00 106.00 0.50 0.05 -- 80.41 -99.00-180.00 196 8 \w 8.00 66.00 0.50 0.05 -- 80.41 -57.00 60.00 116 9 \w 20.00 111.00 0.50 0.05 -- 80.41-125.00 30.00 182 10 \w 7.00 43.00 0.50 0.05 -- 80.41 -38.00 -60.00 72 11 \w 20.00 111.00 0.50 0.05 -- 80.41-125.00 -60.00 182 12 \w -66.00 -9.00 0.50 0.05 -- -82.29 57.00 0.00 114 13 \w -156.00 -68.00 0.50 0.05 -- -82.29 -38.00 -90.00 176 14 \w -66.00 -9.00 0.50 0.05 -- -82.29 57.00 30.00 114 15 \w -43.00 -9.00 0.50 0.05 -- -82.29 38.00 -30.00 68 16 \w -66.00 -9.00 0.50 0.05 -- -82.29 57.00 60.00 114 17 \w -156.00 -68.00 0.50 0.05 -- -82.29 -38.00-120.00 176 18 \w -43.00 -9.00 0.50 0.05 -- -82.29 38.00-150.00 68 19 \w -43.00 -9.00 0.50 0.05 -- -82.29 38.00 150.00 68 20 \w -111.00 -20.00 0.50 0.05 -- -82.29 125.00 60.00 182 21 \w -43.00 -9.00 0.50 0.05 -- -82.29 38.00-120.00 68 22 \w -43.00 -9.00 0.50 0.05 -- -82.29 38.00-180.00 68 23 \w -155.00 -66.00 0.50 0.05 -- -82.29 -57.00 60.00 178 24 \w -111.00 -20.00 0.50 0.05 -- -82.29 125.00 -90.00 182 25 \w -16.00 75.00 0.50 0.05 -- -0.94 19.00 -60.00 182 26 \w -16.00 75.00 0.50 0.05 -- -0.94 19.00 120.00 182 27 \w -73.00 15.00 0.50 0.05 -- -0.94 -57.00 0.00 176 28 \w -24.00 72.00 0.50 0.05 -- -0.94 77.00 150.00 192 29 \w -156.00 -68.00 0.50 0.05 -- -82.29 -38.00 0.00 176 30 \w -156.00 -68.00 0.50 0.05 -- -82.29 -38.00 90.00 176 31 \w -156.00 -68.00 0.50 0.05 -- -82.29 -38.00 150.00 176 32 \w -155.00-126.00 0.50 0.05 -- -82.29 -57.00-150.00 58 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'ROD, Synergy Custom system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0418250000 _diffrn_orient_matrix_UB_12 -0.0908042000 _diffrn_orient_matrix_UB_13 0.0256141000 _diffrn_orient_matrix_UB_21 -0.0240010000 _diffrn_orient_matrix_UB_22 0.0316553000 _diffrn_orient_matrix_UB_23 0.0608306000 _diffrn_orient_matrix_UB_31 -0.0681228000 _diffrn_orient_matrix_UB_32 -0.0669659000 _diffrn_orient_matrix_UB_33 -0.0060433000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.3405 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_unetI/netI 0.0361 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 43834 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 53.543 _diffrn_reflns_theta_max 64.142 _diffrn_reflns_theta_min 3.803 _diffrn_source 'micro-focus metaljet' _exptl_absorpt_coefficient_mu 21.288 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.22240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour light _exptl_crystal_colour_modifier light _exptl_crystal_density_diffrn 2.362 _exptl_crystal_description block _exptl_crystal_F_000 2508 _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.7 _exptl_crystal_size_min 0.6 _refine_diff_density_max 1.128 _refine_diff_density_min -1.335 _refine_diff_density_rms 0.174 _refine_ls_abs_structure_details ; Flack x determined using 3964 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.001(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 400 _refine_ls_number_reflns 9088 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0335 _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^)+(0.0595P)^2^+8.9904P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0911 _refine_ls_wR_factor_ref 0.0915 _reflns_Friedel_coverage 0.865 _reflns_Friedel_fraction_full 0.989 _reflns_Friedel_fraction_max 0.946 _reflns_number_gt 8895 _reflns_number_total 9088 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc04491e2.cif _cod_data_source_block InOC-1 _cod_database_code 1564702 _shelx_shelxl_version_number 2017/1 _chemical_oxdiff_formula In12CHONCl _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.028 _shelx_estimated_absorpt_t_min 0.021 _diffrn_oxdiff_digest_frames ; 01315327b64b33652a1d32372b9f7deff10474266a6 ; _diffrn_oxdiff_digest_hkl ; 01e81091a91d4acab5403871708933a4397708 ; _reflns_odcompleteness_completeness 99.90 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 56.82 _olex2_refinement_description ; 1. Others Fixed U12: O5(0) O11(0) Fixed U23: O5(0) O11(0) Fixed Uiso: H1(0.053) H2(0.049) H3(0.044) H4(0.05) H1A(0.071) H1B(0.071) H2A(0.06) H2B(0.06) H3A(0.045) H3B(0.045) H4A(0.081) H4B(0.081) H5A(0.062) H5B(0.062) H6A(0.051) H6B(0.051) H7A(0.048) H7B(0.048) H8A(0.054) H8B(0.054) H9A(0.045) H9B(0.045) H10A(0.068) H10B(0.068) H11A(0.058) H11B(0.058) H12A(0.089) H12B(0.089) H12C(0.089) H13A(0.057) H13B(0.057) H14A(0.066) H14B(0.066) H15A(0.071) H15B(0.071) H16A(0.065) H16B(0.065) H17A(0.069) H17B(0.069) H18A(0.093) H18B(0.093) H18C(0.093) Fixed X: O5(0.5) O11(0.5) H1(0.43115) H2(0.13273) H3(0.098789) H4(0.505382) H1A(0.469381) H1B(0.470138) H2A(0.307497) H2B(0.322064) H3A(0.351929) H3B(0.269919) H4A(0.295354) H4B(0.332628) H5A(0.202791) H5B(0.170891) H6A(0.101569) H6B(0.080145) H7A(0.054817) H7B(0.146061) H8A(0.107292) H8B(0.162177) H9A(0.245999) H9B(0.221895) H10A(0.185358) H10B(0.208023) H11A(0.344538) H11B(0.323997) H12A(0.316303) H12B(0.224576) H12C(0.258678) H13A(0.430851) H13B(0.340836) H14A(0.38242) H14B(0.433023) H15A(0.573457) H15B(0.625611) H16A(0.662866) H16B(0.570138) H17A(0.413009) H17B(0.392511) H18A(0.564166) H18B(0.473303) H18C(0.489778) Fixed Y: H1(0.385631) H2(0.773941) H3(0.599925) H4(0.215388) H1A(0.615148) H1B(0.558249) H2A(0.413043) H2B(0.525804) H3A(0.63556) H3B(0.566802) H4A(0.831833) H4B(0.88106) H5A(0.928165) H5B(0.816651) H6A(0.408479) H6B(0.538648) H7A(0.421469) H7B(0.371667) H8A(0.465313) H8B(0.578006) H9A(0.421915) H9B(0.354483) H10A(0.82466) H10B(0.934923) H11A(0.872992) H11B(0.865506) H12A(0.119242) H12B(0.15937) H12C(0.157883) H13A(0.114624) H13B(0.145352) H14A(0.168762) H14B(0.059011) H15A(0.058822) H15B(0.16818) H16A(0.133462) H16B(0.116783) H17A(0.446935) H17B(0.578773) H18A(0.835014) H18B(0.835284) H18C(0.877215) Fixed Z: O5(0.5) O11(0.5) H1(0.180931) H2(0.504372) H3(0.558247) H4(0.789358) H1A(0.213793) H1B(0.143049) H2A(0.226518) H2B(0.183808) H3A(0.27515) H3B(0.291749) H4A(0.366577) H4B(0.432716) H5A(0.443731) H5B(0.406369) H6A(0.41979) H6B(0.438338) H7A(0.529692) H7B(0.52705) H8A(0.646383) H8B(0.655482) H9A(0.683339) H9B(0.618199) H10A(0.600028) H10B(0.557395) H11A(0.545794) H11B(0.621581) H12A(0.488233) H12B(0.474004) H12C(0.546772) H13A(0.623747) H13B(0.64842) H14A(0.752581) H14B(0.729364) H15A(0.730201) H15B(0.751989) H16A(0.647616) H16B(0.624543) H17A(0.829714) H17B(0.814207) H18A(0.691018) H18B(0.719218) H18C(0.646575) ; _shelx_res_file ; TITL r4-3_a.res in I2 r4-3.res created by SHELXL-2017/1 at 21:38:55 on 24-Jan-2021 REM Old TITL R4-3 in I2/m REM SHELXT solution in I2 REM R1 0.075, Rweak 0.016, Alpha 0.110, Orientation as input REM Flack x = 0.144 ( 0.007 ) from Parsons' quotients REM Formula found by SHELXT: C13 N7 O14 Cl5 In6 CELL 1.3405 16.0512 11.4206 20.2117 90 90.194 90 ZERR 2 0.0001 0.0001 0.0001 0 0.001 0 LATT -2 SYMM -X,+Y,-Z SFAC C H Cl In N O DISP C 0.0147 0.007 57.608 DISP Cl 0.3292 0.5397 4076.816 DISP H -0 0 0.6481 DISP In 0.1337 3.9104 30156.1191 DISP N 0.0253 0.0135 110.2408 DISP O 0.0412 0.025 193.4765 UNIT 72 168 12 24 16 52 L.S. 10 0 49 PLAN 2 SIZE 0.6 0.7 0.8 BOND $H list 4 conf fmap 2 53 acta OMIT -4 0 2 OMIT -2 1 3 OMIT 0 0 4 OMIT 0 1 7 REM REM REM WGHT 0.059500 8.990399 FVAR 0.11445 IN01 4 0.564391 0.616883 0.582879 11.00000 0.01783 0.02124 = 0.01961 -0.00107 0.00031 -0.00187 IN02 4 0.396266 0.378156 0.549013 11.00000 0.01953 0.01953 = 0.01931 -0.00061 0.00292 -0.00215 IN03 4 0.510297 0.382980 0.688056 11.00000 0.03337 0.02916 = 0.01807 0.00385 0.00141 0.00054 IN04 4 0.297324 0.387769 0.402387 11.00000 0.02193 0.02940 = 0.02861 -0.00809 -0.00187 -0.00275 IN05 4 0.380420 0.608938 0.659010 11.00000 0.02564 0.03018 = 0.02310 -0.00748 0.00588 0.00106 IN06 4 0.261234 0.609033 0.508952 11.00000 0.01709 0.02655 = 0.03353 -0.00650 0.00363 0.00183 CL1 3 0.199199 0.289037 0.330486 11.00000 0.05115 0.08270 = 0.08266 -0.04609 -0.02142 -0.00953 CL2 3 0.296888 0.719247 0.735957 11.00000 0.06222 0.07804 = 0.04823 -0.02458 0.01958 0.01977 O00J 6 0.330640 0.711151 0.578075 11.00000 0.04447 0.02460 = 0.03745 -0.00836 -0.00746 0.00410 O1 6 0.368537 0.507742 0.338812 11.00000 0.02633 0.03503 = 0.02053 -0.00147 -0.00788 0.00070 O2 6 0.201599 0.508282 0.432229 11.00000 0.01663 0.04092 = 0.04162 -0.00819 -0.00211 -0.00016 O3 6 0.299598 0.285169 0.494216 11.00000 0.03277 0.04169 = 0.02838 -0.00286 0.00001 -0.01050 O4 6 0.363300 0.497512 0.474133 11.00000 0.01739 0.02019 = 0.01897 0.00126 0.00157 -0.00141 O5 6 0.500000 0.299330 0.500000 10.50000 0.02634 0.02756 = 0.05103 0.00000 0.02645 0.00000 O6 6 0.300144 0.486166 0.603071 11.00000 0.02202 0.03099 = 0.02773 -0.00539 0.00708 -0.00148 O7 6 0.411701 0.279739 0.636102 11.00000 0.04278 0.03038 = 0.02822 0.01158 0.00075 -0.00932 O8 6 0.412398 0.483440 0.733791 11.00000 0.05440 0.05191 = 0.01693 0.00084 0.01069 0.00590 O9 6 0.495072 0.709105 0.657765 11.00000 0.02880 0.03849 = 0.03638 -0.01421 0.00333 -0.00188 O10 6 0.470433 0.496248 0.606883 11.00000 0.02177 0.01950 = 0.01504 -0.00243 0.00245 -0.00455 O11 6 0.500000 0.694303 0.500000 10.50000 0.04869 0.02197 = 0.02010 0.00000 -0.01593 0.00000 O12 6 0.675199 0.713217 0.570079 11.00000 0.02707 0.03227 = 0.04170 -0.00591 0.00510 -0.01099 O13 6 0.601910 0.282653 0.636674 11.00000 0.03868 0.02765 = 0.04750 0.00873 0.01513 0.00257 N1 5 0.429149 0.449498 0.213269 11.00000 0.05898 0.05346 = 0.02047 -0.00647 -0.00263 0.00453 AFIX 13 H1 2 0.431150 0.385631 0.180931 11.00000 -1.20000 AFIX 0 N2 5 0.192830 0.788414 0.502060 11.00000 0.02324 0.03609 = 0.06330 -0.00439 0.00509 0.00692 AFIX 13 H2 2 0.132730 0.773941 0.504372 11.00000 -1.20000 AFIX 0 N3 5 0.141140 0.538169 0.559828 11.00000 0.01824 0.04316 = 0.04978 -0.00777 0.00731 0.00362 AFIX 13 H3 2 0.098789 0.599925 0.558247 11.00000 -1.20000 AFIX 0 N4 5 0.504913 0.202265 0.741442 11.00000 0.05755 0.04043 = 0.02669 0.01122 0.00307 0.00111 AFIX 13 H4 2 0.505382 0.215388 0.789358 11.00000 -1.20000 AFIX 0 C1 1 0.481703 0.544019 0.189493 11.00000 0.08707 0.06711 = 0.02220 0.01366 -0.00084 -0.00152 AFIX 23 H1A 2 0.469381 0.615148 0.213793 11.00000 -1.20000 H1B 2 0.470138 0.558249 0.143049 11.00000 -1.20000 AFIX 0 C2 1 0.341153 0.483213 0.222515 11.00000 0.06780 0.05488 = 0.02687 -0.00593 -0.01752 0.01190 AFIX 23 H2A 2 0.307497 0.413043 0.226518 11.00000 -1.20000 H2B 2 0.322064 0.525804 0.183808 11.00000 -1.20000 AFIX 0 C3 1 0.329005 0.558254 0.283070 11.00000 0.04897 0.03929 = 0.02451 0.00224 -0.01225 0.00911 AFIX 23 H3A 2 0.351929 0.635560 0.275150 11.00000 -1.20000 H3B 2 0.269919 0.566802 0.291749 11.00000 -1.20000 AFIX 0 C4 1 0.295262 0.822715 0.414292 11.00000 0.07215 0.06536 = 0.06608 0.02556 0.01137 0.03442 AFIX 23 H4A 2 0.295354 0.831833 0.366577 11.00000 -1.20000 H4B 2 0.332628 0.881060 0.432716 11.00000 -1.20000 AFIX 0 C5 1 0.210696 0.844380 0.439011 11.00000 0.04863 0.04584 = 0.06156 0.01301 -0.00936 0.01355 AFIX 23 H5A 2 0.202791 0.928165 0.443731 11.00000 -1.20000 H5B 2 0.170891 0.816651 0.406369 11.00000 -1.20000 AFIX 0 C6 1 0.117811 0.474150 0.447399 11.00000 0.01890 0.06085 = 0.04826 -0.00481 -0.00395 -0.00522 AFIX 23 H6A 2 0.101569 0.408479 0.419790 11.00000 -1.20000 H6B 2 0.080145 0.538648 0.438338 11.00000 -1.20000 AFIX 0 C7 1 0.112049 0.440341 0.518720 11.00000 0.01904 0.05127 = 0.05029 0.00046 0.00015 -0.00955 AFIX 23 H7A 2 0.054817 0.421469 0.529692 11.00000 -1.20000 H7B 2 0.146061 0.371667 0.527050 11.00000 -1.20000 AFIX 0 C8 1 0.155359 0.507148 0.629563 11.00000 0.02741 0.05828 = 0.04858 -0.01168 0.01932 -0.00584 AFIX 23 H8A 2 0.107292 0.465313 0.646383 11.00000 -1.20000 H8B 2 0.162177 0.578006 0.655482 11.00000 -1.20000 AFIX 0 C9 1 0.232289 0.431373 0.636868 11.00000 0.03033 0.04202 = 0.03913 0.00243 0.01224 -0.00848 AFIX 23 H9A 2 0.245999 0.421915 0.683339 11.00000 -1.20000 H9B 2 0.221895 0.354483 0.618199 11.00000 -1.20000 AFIX 0 C10 1 0.218513 0.851874 0.563056 11.00000 0.06063 0.03629 = 0.07404 -0.01806 0.00268 0.01528 AFIX 23 H10A 2 0.185358 0.824660 0.600028 11.00000 -1.20000 H10B 2 0.208023 0.934923 0.557395 11.00000 -1.20000 AFIX 0 C11 1 0.310956 0.832758 0.578493 11.00000 0.06659 0.02692 = 0.05158 -0.00511 -0.00479 0.00002 AFIX 23 H11A 2 0.344538 0.872992 0.545794 11.00000 -1.20000 H11B 2 0.323997 0.865506 0.621581 11.00000 -1.20000 AFIX 0 C12 1 0.272780 0.171934 0.501340 11.00000 0.06756 0.05456 = 0.05540 -0.00112 0.00085 -0.02323 AFIX 137 H12A 2 0.316303 0.119242 0.488233 11.00000 -1.50000 H12B 2 0.224576 0.159370 0.474004 11.00000 -1.50000 H12C 2 0.258678 0.157883 0.546772 11.00000 -1.50000 AFIX 0 C13 1 0.399378 0.164711 0.653286 11.00000 0.04959 0.04244 = 0.05001 0.01576 0.00764 -0.01232 AFIX 23 H13A 2 0.430851 0.114624 0.623747 11.00000 -1.20000 H13B 2 0.340836 0.145352 0.648420 11.00000 -1.20000 AFIX 0 C14 1 0.426147 0.142652 0.723039 11.00000 0.06908 0.04751 = 0.04844 0.02434 0.00901 -0.00604 AFIX 23 H14A 2 0.382420 0.168762 0.752581 11.00000 -1.20000 H14B 2 0.433023 0.059011 0.729364 11.00000 -1.20000 AFIX 0 C15 1 0.580968 0.142140 0.723063 11.00000 0.06586 0.04226 = 0.06901 0.02630 0.00098 0.00845 AFIX 23 H15A 2 0.573457 0.058822 0.730201 11.00000 -1.20000 H15B 2 0.625611 0.168180 0.751989 11.00000 -1.20000 AFIX 0 C16 1 0.606317 0.161304 0.653708 11.00000 0.06747 0.02935 = 0.06671 0.00659 0.01889 -0.00080 AFIX 23 H16A 2 0.662866 0.133462 0.647616 11.00000 -1.20000 H16B 2 0.570138 0.116783 0.624543 11.00000 -1.20000 AFIX 0 C17 1 0.427123 0.512853 0.801640 11.00000 0.08185 0.07362 = 0.01804 -0.00406 0.01745 0.00884 AFIX 23 H17A 2 0.413009 0.446935 0.829714 11.00000 -1.20000 H17B 2 0.392511 0.578773 0.814207 11.00000 -1.20000 AFIX 0 C18 1 0.506461 0.822965 0.680395 11.00000 0.04931 0.04691 = 0.09055 -0.03464 0.00403 0.00211 AFIX 137 H18A 2 0.564166 0.835014 0.691018 11.00000 -1.50000 H18B 2 0.473303 0.835284 0.719218 11.00000 -1.50000 H18C 2 0.489778 0.877215 0.646575 11.00000 -1.50000 AFIX 0 CL3 3 0.497065 0.250693 0.901561 11.00000 0.05162 0.07019 = 0.04012 0.01574 -0.00033 -0.00785 HKLF 4 REM r4-3_a.res in I2 REM R1 = 0.0335 for 8895 Fo > 4sig(Fo) and 0.0340 for all 9088 data REM 400 parameters refined using 1 restraints END WGHT 0.0595 8.9903 REM Highest difference peak 1.128, deepest hole -1.335, 1-sigma level 0.174 Q1 1 0.5208 0.5477 0.0033 11.00000 0.05 1.13 Q2 1 0.3379 0.3831 0.5585 11.00000 0.05 0.99 ; _shelx_res_checksum 42847 _shelx_hkl_file ; 0 0 2 1177.37 15.56 0 0 2 1154.70 15.47 0 0 4 49.80 2.29 0 0 -4 53.57 2.25 0 0 4 46.90 2.15 0 0 -4 52.45 1.83 0 0 4 58.03 2.48 0 0 6 38.82 2.51 0 0 6 33.49 2.42 0 0 -6 43.28 1.97 0 0 -6 43.13 2.44 0 0 6 48.72 2.87 0 0 8 209.41 7.38 0 0 -8 266.67 6.83 0 0 8 225.48 7.62 0 0 -8 253.97 6.08 0 0 -8 222.78 7.32 0 0 8 312.23 9.04 0 0 -8 263.55 7.52 0 0 -10 286.18 9.07 0 0 10 329.03 10.57 0 0 10 279.35 9.98 0 0 10 263.82 9.46 0 0 -10 312.08 8.48 0 0 -10 320.28 9.49 0 0 10 402.18 11.80 0 0 -10 274.48 9.22 0 0 -10 302.25 7.50 0 0 -10 336.24 9.17 0 0 -10 335.47 8.73 0 0 12 1621.88 29.36 0 0 12 1279.00 27.83 0 0 -12 1528.01 25.46 0 0 12 1329.84 28.85 0 0 -12 1665.20 27.05 0 0 -12 1257.68 21.40 0 0 -12 1386.45 20.85 0 0 -12 1585.30 27.88 0 0 -12 1349.91 26.98 0 0 -12 1466.88 23.23 0 0 12 1379.97 28.05 0 0 -12 1627.94 25.82 0 0 14 3.35 1.71 0 0 -14 3.56 1.44 0 0 -14 5.72 1.19 0 0 -14 3.99 1.27 0 0 16 38.35 4.47 0 0 -16 37.50 4.19 0 0 -16 32.56 3.51 0 0 -18 17.57 3.30 0 0 -18 20.29 3.06 0 0 20 366.37 15.34 0 0 -20 321.37 14.32 0 0 -20 334.49 13.09 0 0 22 218.67 11.57 0 0 -22 185.58 10.76 0 0 -22 188.60 9.63 0 0 24 0.91 1.69 0 0 -24 2.57 1.77 0 0 -24 1.25 1.05 0 0 26 46.39 4.43 0 0 -26 39.70 4.18 0 0 26 41.23 4.26 0 1 3 280.43 5.69 0 1 -3 300.65 5.35 0 1 3 245.56 5.97 0 -1 -3 329.80 5.70 0 -1 -3 307.89 6.43 0 1 3 265.15 5.61 0 1 -3 298.97 5.75 0 1 3 266.20 5.81 0 -1 3 321.32 5.71 0 -1 3 349.26 6.79 0 1 -3 264.83 5.84 0 1 -5 221.99 5.25 0 -1 -5 276.46 6.02 0 1 5 208.74 5.75 0 -1 -5 240.85 6.53 0 -1 5 232.75 5.99 0 1 -5 231.05 5.72 0 -1 5 279.99 7.06 0 -1 -5 252.65 6.51 0 -1 -5 197.76 3.81 0 1 5 202.89 5.72 0 -1 5 231.99 5.65 0 -1 -5 250.84 6.13 0 1 -5 214.38 5.09 0 1 5 239.47 5.98 0 1 7 15.88 1.78 0 1 -7 16.59 1.54 0 -1 -7 2.23 0.60 0 -1 -7 4.69 0.96 0 -1 7 2.55 0.88 0 1 7 24.81 2.29 0 1 7 16.92 1.78 0 -1 -7 4.72 0.73 0 -1 7 3.01 0.98 0 1 -7 16.91 1.44 0 -1 -7 4.25 1.08 0 -1 -7 3.89 0.97 0 1 -7 17.45 1.72 0 1 7 14.43 1.69 0 -1 -7 2.46 0.46 0 -1 7 3.37 0.86 0 -1 -9 122.77 5.43 0 -1 9 134.27 6.34 0 1 9 145.66 6.51 0 -1 9 111.45 5.65 0 1 9 138.28 6.37 0 -1 -9 131.33 4.86 0 1 9 134.70 6.25 0 -1 9 116.23 5.64 0 1 -9 137.38 5.74 0 1 -9 150.93 5.47 0 -1 -9 145.11 6.01 0 -1 -9 139.00 6.22 0 1 9 141.04 6.17 0 1 -9 168.04 5.35 0 -1 -9 145.72 5.50 0 -1 -9 134.86 4.24 0 -1 -9 112.69 3.33 0 -1 9 168.03 7.25 0 1 -9 152.48 5.94 0 -1 9 119.29 5.50 0 1 9 179.68 6.87 0 1 -9 158.52 5.54 0 -1 -11 718.02 16.70 0 1 11 853.12 18.65 0 -1 11 790.30 18.71 0 1 11 707.64 18.45 0 1 11 676.55 17.97 0 -1 11 569.18 16.32 0 -1 11 649.44 17.56 0 -1 -11 750.62 15.15 0 1 -11 894.82 17.95 0 1 -11 844.05 15.13 0 1 -11 728.06 16.70 0 -1 -11 718.55 11.37 0 -1 11 661.88 16.65 0 1 11 760.02 18.19 0 -1 11 928.26 20.87 0 -1 -11 663.20 10.57 0 1 -11 882.21 16.88 0 -1 -11 793.91 17.50 0 -1 -11 764.04 18.00 0 -1 -11 703.18 13.16 0 -1 -11 778.88 15.22 0 1 11 843.29 15.20 0 1 -11 899.15 16.60 0 1 13 1721.39 30.49 0 -1 -13 1549.61 28.73 0 -1 13 1724.11 31.88 0 -1 13 1161.92 27.90 0 -1 -13 1434.41 22.84 0 1 -13 1585.50 27.86 0 1 -13 1355.21 22.52 0 1 -13 1395.56 24.30 0 -1 -13 1632.88 26.62 0 1 -13 1598.51 27.14 0 1 15 106.52 6.90 0 -1 15 100.51 7.20 0 1 -15 96.20 6.28 0 -1 -15 92.81 5.55 0 1 -15 98.32 5.98 0 -1 17 61.41 6.07 0 1 17 64.12 5.76 0 1 -17 60.48 5.53 0 1 -17 63.90 5.26 0 -1 -17 60.25 4.85 0 -1 19 48.20 5.61 0 1 19 47.23 5.21 0 1 -19 43.55 5.13 0 -1 -19 42.97 4.41 0 1 -19 43.69 4.63 0 1 21 409.51 16.03 0 1 -21 364.89 15.45 0 1 -21 371.27 14.27 0 -1 -21 419.12 14.44 0 1 23 3.22 1.90 0 -1 23 5.46 2.27 0 1 -23 4.23 2.10 0 -1 -23 5.15 1.70 0 -1 23 6.70 2.61 0 1 -23 5.64 1.91 0 -1 25 130.22 8.09 0 1 25 137.34 7.90 0 -1 -25 110.07 10.29 0 1 -25 114.11 7.41 0 -1 25 130.50 8.18 0 1 -25 114.99 6.57 0 1 -27 0.86 1.39 0 -1 -27 2.67 1.85 0 1 -27 1.18 1.09 0 1 27 2.96 1.33 0 2 0 35.92 1.61 0 2 0 30.92 1.54 0 -2 0 38.27 0.98 0 2 0 33.44 0.96 0 2 -2 3.90 0.64 0 2 2 10.51 0.69 0 -2 2 14.27 1.15 0 2 2 3.92 0.89 0 -2 -2 14.21 1.05 0 2 2 4.63 0.63 0 2 -2 7.19 0.63 0 2 4 148.31 2.61 0 2 4 152.70 4.41 0 2 -4 139.82 4.57 0 2 4 140.05 4.81 0 -2 4 167.80 4.58 0 -2 4 161.38 4.64 0 2 4 140.12 5.06 0 -2 -4 178.29 5.61 0 2 -4 162.79 4.09 0 2 4 142.98 4.64 0 -2 4 160.67 4.61 0 -2 -4 181.89 4.44 0 2 6 349.99 9.26 0 -2 6 426.38 10.66 0 -2 6 385.39 8.76 0 -2 -6 339.89 9.02 0 2 -6 341.87 8.79 0 2 -6 433.97 8.70 0 2 6 427.28 9.27 0 -2 6 344.50 8.53 0 2 -6 449.71 9.47 0 -2 -6 423.98 8.64 0 -2 -6 384.56 7.41 0 -2 -6 388.69 9.93 0 2 -6 416.83 8.37 0 2 6 361.19 9.14 0 -2 8 1110.34 20.55 0 2 -8 1393.92 21.90 0 2 8 1165.39 22.08 0 2 -8 1317.16 20.14 0 -2 8 1080.22 20.54 0 2 8 1496.99 22.57 0 -2 -8 1053.82 21.48 0 -2 8 1339.94 24.32 0 -2 -8 1220.82 18.89 0 2 -8 1275.87 20.05 0 2 8 1037.83 21.22 0 -2 -8 1297.17 20.55 0 2 10 59.87 4.28 0 -2 -10 51.68 3.83 0 -2 10 61.80 4.63 0 2 10 44.72 4.11 0 -2 10 48.39 3.84 0 2 -10 56.96 3.51 0 2 10 47.74 4.09 0 -2 -10 60.92 3.35 0 -2 -10 59.64 2.78 0 2 -10 69.51 4.31 0 2 -10 58.42 3.61 0 -2 -10 60.34 4.48 0 -2 10 77.58 5.46 0 2 -10 56.47 3.38 0 2 10 72.59 4.59 0 2 10 50.28 4.13 0 -2 -10 59.36 3.76 0 -2 -10 55.51 3.78 0 -2 10 50.47 3.76 0 2 12 1963.69 32.64 0 -2 12 1771.49 33.45 0 -2 -12 1578.38 30.32 0 -2 -12 1741.14 27.92 0 -2 -12 1630.76 27.58 0 2 12 1520.65 32.92 0 -2 -12 1562.15 24.50 0 -2 -12 1840.05 30.21 0 -2 12 1387.38 29.68 0 -2 -12 1647.15 32.19 0 2 -12 1952.25 30.33 0 2 -12 1776.46 28.30 0 2 -12 2018.27 32.36 0 -2 -12 1786.56 27.78 0 2 12 1969.88 28.11 0 2 14 1411.68 27.96 0 -2 -14 1296.18 27.48 0 -2 14 1424.71 30.59 0 -2 -14 1280.15 23.16 0 -2 -14 1387.02 26.77 0 2 -14 1335.88 26.21 0 -2 -14 1350.83 24.36 0 2 16 248.08 10.95 0 -2 -16 251.44 11.16 0 -2 16 268.63 12.85 0 2 -16 217.46 10.16 0 -2 -16 259.86 10.92 0 -2 -16 254.66 9.56 0 2 -16 224.01 9.87 0 -2 18 6.25 2.72 0 2 18 4.65 1.92 0 -2 -18 3.96 1.86 0 2 -18 3.13 1.75 0 -2 -18 3.50 1.39 0 2 -18 3.84 1.66 0 2 20 161.37 9.48 0 -2 20 197.86 11.85 0 2 -20 147.98 9.46 0 -2 -20 184.96 10.41 0 2 -20 162.11 9.39 0 -2 -20 175.67 8.74 0 -2 22 325.34 15.04 0 2 22 281.98 12.67 0 -2 -22 273.89 12.90 0 2 -22 253.54 12.49 0 -2 22 340.34 15.56 0 2 -22 250.05 11.69 0 -2 -24 224.55 15.46 0 2 24 242.61 10.87 0 -2 24 240.37 11.93 0 -2 -24 194.71 10.18 0 2 -24 233.32 11.08 0 -2 24 231.40 11.81 0 2 -24 205.28 9.78 0 2 -26 59.79 6.64 0 -2 26 66.51 5.35 0 2 26 74.18 5.24 0 -2 -26 69.92 7.47 0 -2 -26 63.45 5.00 0 2 -26 69.09 5.12 0 -2 26 69.72 5.54 0 2 -26 63.13 4.45 0 3 1 1028.10 14.50 0 3 1 979.31 13.63 0 -3 -1 818.41 13.91 0 3 -1 1052.20 15.09 0 -3 1 893.64 15.12 0 3 -1 1007.28 12.73 0 -3 -1 873.47 13.20 0 -3 -1 787.78 15.16 0 3 1 885.67 15.12 0 3 -3 90.58 3.81 0 -3 -3 112.22 3.50 0 3 3 120.84 2.99 0 -3 3 108.62 4.04 0 -3 -3 105.51 4.18 0 3 -3 116.61 4.02 0 3 -3 115.54 3.22 0 -3 -3 109.47 3.40 0 3 3 88.92 4.29 0 -3 -5 298.05 8.02 0 3 5 314.02 4.79 0 -3 5 259.04 6.98 0 3 5 327.85 7.60 0 3 -5 272.65 7.64 0 -3 5 281.27 7.59 0 -3 -5 274.12 6.25 0 -3 -5 305.02 5.52 0 3 5 252.41 7.26 0 -3 -5 316.00 6.83 0 -3 5 287.13 7.50 0 3 -5 333.59 6.99 0 3 5 269.49 8.48 0 -3 7 984.49 20.25 0 -3 7 1094.52 20.40 0 -3 -7 1352.65 19.63 0 -3 -7 1260.31 17.55 0 3 7 1024.03 21.54 0 -3 -7 1252.83 22.77 0 3 -7 1304.56 19.38 0 3 7 1029.45 20.72 0 -3 -7 1261.74 21.32 0 3 -7 1369.01 20.42 0 3 -7 1057.88 20.21 0 3 7 1395.21 21.09 0 -3 7 1087.76 20.15 0 -3 7 1073.03 19.66 0 3 7 1158.99 21.69 0 -3 -7 1083.92 17.50 0 -3 -9 72.29 4.59 0 -3 9 77.77 5.01 0 3 9 57.40 3.99 0 3 -9 62.58 3.61 0 -3 -9 88.40 4.51 0 -3 -9 100.38 4.55 0 3 9 52.32 4.24 0 -3 9 64.68 4.47 0 -3 -9 87.54 3.65 0 -3 -9 94.87 5.73 0 3 -9 64.11 3.67 0 -3 -9 96.93 5.24 0 -3 9 66.82 4.19 0 -3 -9 97.30 4.59 0 -3 -9 81.85 4.54 0 3 -9 73.72 3.98 0 3 9 75.64 4.41 0 3 9 62.66 4.58 0 -3 9 72.17 4.47 0 -3 -9 74.03 4.58 0 3 -9 62.75 3.70 0 3 11 422.28 12.40 0 -3 -11 342.74 11.52 0 -3 11 384.02 13.15 0 3 11 319.63 12.55 0 3 11 351.76 12.93 0 -3 -11 367.81 9.46 0 -3 11 285.07 11.51 0 -3 11 395.37 11.92 0 -3 -11 386.19 10.77 0 3 -11 426.44 11.13 0 -3 -11 332.52 7.69 0 3 11 519.67 13.54 0 -3 -11 361.76 11.23 0 -3 -11 408.56 11.22 0 3 -11 404.62 10.75 0 -3 11 296.24 10.61 0 3 11 345.77 12.62 0 3 -11 436.18 11.39 0 -3 -11 386.80 9.27 0 3 13 1652.55 31.90 0 -3 13 1888.49 36.65 0 -3 -13 1627.48 32.31 0 -3 -13 1685.94 28.57 0 -3 -13 1720.03 29.55 0 3 -13 1707.58 30.61 0 -3 -13 1789.06 31.26 0 3 -13 1778.83 31.02 0 -3 -13 1735.92 28.05 0 -3 15 67.65 6.54 0 -3 -15 60.16 5.41 0 3 15 70.56 5.57 0 -3 -15 58.18 4.26 0 3 -15 57.74 4.94 0 -3 -15 58.23 4.94 0 3 15 61.25 5.42 0 -3 -15 58.62 4.18 0 3 17 50.48 4.98 0 -3 17 55.44 6.38 0 -3 -17 45.54 5.01 0 -3 -17 46.65 4.79 0 3 -17 46.78 4.81 0 -3 -17 44.47 3.97 0 3 19 5.96 2.17 0 -3 19 7.40 2.89 0 3 -19 3.28 1.98 0 -3 -19 6.17 2.20 0 -3 19 10.74 3.41 0 3 -19 5.90 2.07 0 -3 21 676.83 22.96 0 -3 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16.23 -5 4 -3 792.13 15.27 5 -4 5 66.98 4.98 -5 -4 -5 51.86 5.37 -5 -4 -5 50.25 4.48 -5 -4 -5 55.50 3.59 -5 -4 -5 48.58 3.85 -5 -4 -5 58.51 4.95 -5 -4 -5 56.11 4.72 5 -4 5 51.97 3.43 -5 -4 -5 55.52 4.09 5 4 5 51.02 4.03 5 4 5 57.23 2.28 -5 -4 -5 62.80 4.66 -5 4 -5 62.62 3.75 5 4 5 53.47 2.38 5 4 5 51.91 3.12 -5 -4 -5 58.17 2.91 -5 -4 -5 60.23 3.78 5 -4 5 49.08 3.49 -5 4 -5 59.37 3.85 5 4 5 51.52 1.49 -5 4 -5 58.00 3.75 -5 4 -5 55.96 3.58 -5 4 -5 53.58 3.89 -5 -4 -5 50.62 3.12 5 -4 5 54.39 3.61 -5 -4 -7 8.53 2.18 5 -4 7 10.01 2.31 -5 -4 -7 13.83 2.76 -5 -4 -7 9.55 1.80 5 4 7 17.55 2.05 -5 -4 -7 9.84 2.69 5 4 7 10.19 2.22 -5 -4 -7 9.47 2.34 -5 -4 -7 8.76 1.17 -5 -4 -7 7.65 1.66 -5 -4 -7 10.15 2.08 5 4 7 13.62 1.36 -5 4 -7 11.96 2.48 5 -4 7 10.18 1.67 -5 4 -7 17.24 2.13 5 4 7 17.87 2.31 5 -4 7 9.76 1.69 -5 -4 -7 10.48 1.72 -5 4 -7 14.86 2.03 -5 -4 -7 9.63 1.47 5 4 7 17.83 1.18 -5 4 -7 15.30 2.01 -5 4 -7 11.85 1.97 5 -4 7 9.17 1.74 -5 4 -7 15.78 2.07 -5 -4 -7 9.40 1.45 -5 -4 -9 1629.00 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-4 -15 45.78 4.49 -5 4 -15 38.92 4.08 5 4 15 43.34 4.89 5 -4 15 40.30 5.21 5 4 17 30.27 3.76 -5 -4 -17 12.66 4.64 -5 -4 -17 15.19 3.35 -5 -4 -17 16.32 3.16 -5 4 -17 26.54 3.47 5 4 17 29.71 4.38 5 -4 17 30.69 4.84 5 4 19 10.39 2.35 -5 -4 -19 11.61 4.84 -5 -4 -19 9.83 2.68 -5 -4 -19 11.36 2.79 -5 4 -19 11.30 2.31 5 -4 19 15.92 3.87 5 4 19 10.36 2.69 5 4 21 192.56 8.93 -5 -4 -21 182.42 15.10 -5 -4 -21 180.63 9.72 -5 4 -21 171.78 9.68 5 4 21 180.35 9.87 5 -4 21 214.97 12.34 -5 -4 -23 20.80 5.20 5 -4 23 20.24 3.70 5 4 23 29.27 3.79 -5 4 -23 27.91 3.67 -5 -4 -25 53.94 6.51 -5 4 -25 54.50 4.74 5 -4 25 63.18 5.35 -5 4 -25 50.42 4.09 5 4 25 60.10 4.58 5 -5 -24 287.54 10.22 -5 5 24 302.70 10.34 5 5 -24 292.92 10.20 5 -5 -22 9.65 2.29 5 5 -22 13.25 2.52 -5 5 22 13.04 2.59 -5 -5 22 14.50 3.88 5 -5 -20 86.29 5.97 5 -5 -20 109.19 10.27 5 -5 -20 95.47 6.86 -5 -5 20 97.36 8.43 -5 5 20 84.31 6.57 5 5 -20 77.22 6.22 -5 -5 18 351.40 19.00 5 -5 -18 361.76 13.07 -5 5 18 353.51 14.34 5 -5 -18 357.91 13.86 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-2 577.59 14.59 5 -5 -2 536.30 14.33 5 -5 -2 357.95 9.47 5 5 -2 521.64 12.11 5 -5 -2 337.21 11.64 -5 5 2 498.03 12.33 -5 -5 2 396.74 10.80 5 -5 -2 419.15 10.62 5 -5 -2 391.20 11.68 5 5 -2 478.31 9.38 -5 5 2 542.57 12.31 -5 -5 2 452.26 11.06 -5 -5 2 400.39 11.05 -5 5 2 456.47 10.97 -5 -5 0 25.02 2.56 -5 -5 0 32.17 3.91 -5 -5 0 20.38 2.60 -5 -5 0 36.02 3.94 -5 -5 0 40.42 3.59 5 -5 0 36.46 3.55 5 5 0 30.44 1.49 5 5 0 30.11 1.82 -5 -5 0 29.96 3.18 -5 -5 0 32.21 3.98 5 -5 0 37.02 3.60 5 -5 0 25.58 2.26 -5 -5 0 24.77 2.81 -5 -5 0 30.78 2.76 5 5 0 33.69 2.56 -5 5 0 26.56 2.75 5 5 0 26.93 1.74 5 -5 0 27.49 2.89 -5 5 0 27.25 2.64 -5 -5 0 26.65 2.47 -5 -5 0 26.90 2.45 -5 5 0 27.25 2.36 5 -5 2 1318.95 21.72 -5 -5 -2 1177.23 22.37 -5 -5 -2 1365.63 29.28 -5 -5 -2 1306.71 27.31 -5 -5 -2 1224.74 24.68 -5 5 -2 1523.68 22.45 -5 -5 -2 1278.94 28.02 5 -5 2 1582.20 27.13 5 5 2 1272.02 20.91 5 5 2 1177.29 15.90 -5 -5 -2 1266.70 25.18 5 -5 2 1130.72 21.02 -5 -5 -2 1212.97 25.04 -5 5 -2 1353.92 23.29 5 5 2 1178.30 20.65 5 -5 2 1126.89 23.27 5 5 2 1435.41 20.63 -5 5 -2 1425.64 24.46 5 -5 2 1393.55 24.86 5 5 2 1238.51 17.59 -5 5 -2 1368.66 22.95 -5 -5 -2 1283.86 21.86 -5 5 -2 1280.08 21.72 -5 -5 -2 1147.10 21.12 5 -5 4 50.37 4.69 -5 -5 -4 51.67 4.63 -5 -5 -4 46.70 3.78 -5 -5 -4 47.16 3.34 -5 -5 -4 49.24 5.35 -5 -5 -4 50.21 4.77 -5 -5 -4 62.21 5.44 5 -5 4 39.89 3.13 -5 -5 -4 50.86 4.23 -5 5 -4 62.82 3.81 -5 -5 -4 51.22 4.60 5 5 4 54.54 3.94 5 5 4 54.21 2.04 -5 -5 -4 50.65 2.42 -5 -5 -4 53.73 3.84 5 5 4 59.20 3.05 5 -5 4 42.67 3.62 5 5 4 65.74 2.61 5 5 4 67.80 2.29 -5 5 -4 60.85 4.06 -5 5 -4 56.71 4.02 -5 5 -4 65.23 3.98 5 -5 4 52.69 3.74 -5 -5 -4 49.57 3.38 5 -5 6 17.88 3.16 -5 -5 -6 18.36 3.16 -5 -5 -6 17.15 3.02 -5 -5 -6 18.29 2.79 -5 -5 -6 17.84 2.35 -5 -5 -6 14.79 3.41 -5 -5 -6 20.83 2.96 -5 -5 -6 16.91 2.52 5 -5 6 15.33 2.14 -5 -5 -6 13.25 2.53 -5 5 -6 22.28 2.43 5 5 6 16.32 2.66 -5 5 -6 12.65 2.10 -5 -5 -6 15.01 2.17 -5 -5 -6 16.79 1.74 5 -5 6 12.91 2.13 -5 5 -6 18.59 2.39 -5 5 -6 20.11 2.62 5 -5 6 17.64 1.94 -5 5 -6 19.50 2.30 5 -5 6 18.50 2.45 5 -5 8 115.25 8.20 -5 -5 -8 108.80 6.39 -5 -5 -8 112.03 8.07 -5 -5 -8 105.48 7.61 5 5 8 137.56 6.28 -5 -5 -8 96.11 8.71 -5 -5 -8 102.16 6.25 -5 -5 -8 103.98 6.81 -5 -5 -8 96.56 7.20 -5 -5 -8 114.95 6.08 -5 5 -8 144.75 6.95 -5 -5 -8 105.27 5.22 5 -5 8 107.39 5.27 5 -5 8 99.34 6.23 -5 5 -8 154.34 6.90 -5 -5 -10 2099.19 42.93 -5 -5 -10 2193.15 40.76 -5 -5 -10 2110.93 50.41 5 5 10 2481.85 39.02 -5 -5 -10 2168.21 40.82 -5 -5 -10 2275.46 44.24 -5 5 -10 2374.43 39.18 -5 -5 -10 2381.69 38.74 5 -5 10 2283.02 41.48 5 -5 10 2375.43 37.41 -5 5 -10 2373.28 38.94 -5 -5 -12 64.66 5.96 -5 -5 -12 63.92 8.14 5 5 12 54.07 4.62 -5 5 -12 43.60 5.03 -5 -5 -12 53.41 5.82 -5 -5 -12 66.03 5.60 -5 -5 -12 52.46 4.11 -5 5 -12 47.07 4.37 -5 -5 -12 70.50 5.08 5 -5 12 63.42 6.01 5 -5 12 60.63 4.76 -5 5 -12 42.46 4.28 -5 -5 -14 304.22 14.12 5 5 14 297.91 11.42 -5 -5 -14 278.56 18.12 -5 -5 -14 284.21 13.82 -5 -5 -14 282.83 11.93 -5 -5 -14 291.49 10.94 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109.71 6.29 -8 -6 -2 22.14 4.54 -8 -6 -2 27.70 4.32 -8 -6 -2 25.88 4.14 -8 -6 -2 33.43 4.08 -8 -6 -2 27.50 4.95 -8 -6 -2 26.43 3.43 -8 6 -2 22.34 3.01 -8 -6 -2 32.57 3.43 -8 6 -2 29.72 3.48 -8 -6 -2 25.51 3.02 8 -6 4 67.87 6.35 -8 -6 -4 62.68 6.02 -8 -6 -4 50.31 6.78 -8 -6 -4 54.38 6.87 -8 -6 -4 58.90 5.49 -8 -6 -4 66.04 7.44 -8 -6 -4 70.35 6.37 -8 -6 -4 48.91 5.74 -8 -6 -4 46.58 5.96 -8 6 -4 70.38 5.38 -8 -6 -4 55.51 4.87 -8 6 -4 70.69 5.41 -8 6 -4 65.90 4.96 8 -6 6 673.27 21.27 -8 -6 -6 693.06 22.43 -8 -6 -6 606.23 24.15 -8 -6 -6 535.43 23.73 -8 -6 -6 610.44 19.86 -8 -6 -6 642.33 22.51 -8 -6 -6 574.49 22.52 -8 6 -6 756.31 19.55 8 -6 6 618.22 20.00 -8 -6 -6 633.20 18.13 -8 -6 -6 627.18 16.58 -8 6 -6 681.20 18.76 -8 6 -6 673.85 17.64 8 -6 8 816.02 24.75 -8 -6 -8 944.83 28.14 -8 -6 -8 803.52 28.51 -8 -6 -8 726.26 28.68 -8 -6 -8 764.11 22.33 -8 -6 -8 708.33 23.80 -8 6 -8 587.48 22.28 -8 -6 -8 725.05 26.31 -8 -6 -8 787.91 20.68 -8 6 -8 828.66 20.89 -8 6 -8 747.32 20.62 8 -6 8 804.96 20.18 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3.87 8 -8 -2 28.34 3.64 -8 8 2 36.52 4.48 -8 8 2 36.09 3.96 -8 -8 2 40.85 4.62 -8 -8 2 33.55 4.28 -8 -8 0 117.88 8.40 -8 -8 0 113.11 10.85 -8 -8 0 114.48 8.00 -8 -8 0 118.33 10.89 -8 -8 0 100.64 10.33 -8 -8 0 110.40 9.06 -8 -8 0 96.24 8.17 -8 -8 0 82.48 6.69 -8 -8 0 114.50 7.63 -8 8 0 112.37 7.57 8 -8 0 124.56 7.64 8 -8 0 129.40 8.85 -8 -8 0 138.44 8.33 -8 8 0 126.19 7.48 -8 -8 0 113.78 7.63 8 -8 2 77.55 8.19 -8 -8 -2 77.44 7.27 -8 -8 -2 69.30 8.69 -8 -8 -2 78.45 6.86 -8 -8 -2 82.05 9.37 -8 -8 -2 72.15 7.37 -8 -8 -2 69.76 7.30 -8 -8 -2 55.19 6.21 -8 8 -2 78.54 6.33 8 -8 2 70.99 6.06 8 -8 2 69.21 6.69 -8 -8 -2 66.42 5.96 -8 8 -2 70.59 5.74 -8 -8 -2 82.14 6.42 8 -8 4 71.44 7.80 -8 -8 -4 64.38 7.02 -8 -8 -4 49.19 7.65 -8 -8 -4 61.01 8.18 -8 -8 -4 67.64 6.85 -8 -8 -4 52.26 6.62 -8 -8 -4 63.54 8.15 -8 -8 -4 49.14 6.53 -8 -8 -4 56.64 5.64 8 -8 4 68.35 6.96 -8 8 -4 48.67 4.85 -8 -8 -4 72.99 6.01 8 -8 6 446.99 20.00 -8 -8 -6 513.78 20.80 -8 -8 -6 345.58 20.94 8 -8 6 444.05 14.37 -8 -8 -6 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106.35 7.25 -8 -8 -18 129.79 11.99 -8 8 -18 108.75 6.83 -8 8 -18 109.62 6.94 -8 -8 -20 29.35 5.38 -8 8 -20 20.78 2.87 -8 9 19 106.70 5.94 8 9 -19 105.58 6.05 8 -9 -17 90.46 5.91 -8 9 17 87.17 6.08 8 9 -17 91.01 6.45 -8 -9 17 103.47 9.17 8 -9 -15 20.97 3.17 -8 9 15 19.07 3.31 -8 -9 15 23.42 5.98 8 -9 -15 21.23 3.04 8 9 -15 19.30 3.42 8 -9 -15 26.34 3.65 -8 -9 15 28.14 5.52 -8 9 15 19.91 2.82 -8 -9 13 70.80 6.79 -8 9 13 84.32 6.96 -8 -9 13 78.01 10.42 8 -9 -13 83.65 6.03 8 9 -13 81.26 6.78 8 -9 -13 90.27 6.69 8 -9 -13 84.17 6.45 -8 -9 13 93.29 9.36 8 -9 -13 81.85 6.39 -8 9 13 77.91 5.89 -8 -9 11 21.92 4.09 -8 9 11 30.21 4.41 -8 -9 11 33.48 7.18 8 -9 -11 30.41 3.84 8 9 -11 27.69 4.02 8 -9 -11 26.56 4.03 -8 -9 11 29.18 5.45 -8 -9 9 18.08 5.28 -8 -9 9 12.71 3.35 -8 9 9 10.53 2.92 -8 -9 9 17.48 5.50 8 -9 -9 12.53 2.69 8 9 -9 12.13 2.72 8 -9 -9 14.26 3.16 -8 9 9 12.91 2.57 -8 -9 9 17.39 4.24 -8 -9 7 1306.82 40.55 -8 -9 7 1144.48 30.49 -8 -9 7 1149.62 40.37 -8 9 7 1215.82 28.91 8 -9 -7 1273.05 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2.34 8 -11 3 15.01 3.81 -8 -11 -3 11.46 2.99 8 -11 5 79.13 9.98 -8 -11 -5 109.27 10.51 -8 -11 -5 84.79 11.91 -8 -11 -5 89.81 11.74 -8 11 -5 94.03 7.27 8 -11 5 86.13 8.39 8 -11 5 91.73 8.85 -8 -11 -7 677.75 32.75 -8 -11 -7 651.62 30.44 -8 -11 -7 599.72 20.73 -8 11 -7 559.25 18.43 8 -11 7 634.33 23.95 8 -11 7 599.50 23.52 -8 11 -7 551.67 17.02 8 -11 9 24.91 4.91 -8 -11 -9 26.99 7.39 -8 -11 -9 29.20 6.62 -8 -11 -9 34.34 4.83 8 -11 9 24.88 5.16 -8 11 -9 21.50 3.32 -8 -11 -11 14.98 5.33 8 -11 11 5.48 3.10 8 -11 11 9.10 3.66 -8 11 -11 6.36 1.87 -8 -11 -11 9.90 2.75 -8 -11 -13 14.90 4.90 8 -11 13 8.27 2.97 -8 11 -13 9.03 2.21 -8 11 -13 10.01 2.19 -8 -11 -13 12.10 2.73 -8 11 -15 136.89 6.89 8 -12 -12 130.51 11.47 8 -12 -12 134.06 7.50 -8 12 12 121.41 6.77 -8 -12 12 163.97 14.16 8 -12 -12 109.05 6.63 8 -12 -12 123.65 6.96 -8 -12 12 167.76 11.36 8 -12 -10 29.94 6.47 -8 12 10 22.32 3.36 -8 -12 10 31.17 6.90 8 -12 -10 29.65 3.98 8 -12 -10 27.39 3.62 -8 -12 10 40.05 6.17 8 -12 -10 29.50 3.92 8 -12 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4.77 -19 5 -2 26.44 4.78 19 -5 2 21.91 2.70 -19 5 -2 24.27 3.26 -19 -5 -2 28.82 3.76 -19 5 -4 134.76 10.20 -19 -5 -4 182.96 11.11 -19 -5 -4 186.17 11.52 -19 5 -4 130.43 9.63 19 -5 4 102.10 5.86 -19 5 -6 214.49 12.42 -19 -5 -6 259.87 12.33 -19 -5 -6 280.85 13.83 -19 5 -6 210.20 11.29 19 -5 6 157.02 7.37 -19 6 7 128.71 8.23 -19 -6 7 134.61 9.64 -19 -6 7 133.36 7.33 -19 -6 5 6.26 2.53 -19 6 5 2.51 1.82 -19 6 5 2.10 2.00 -19 -6 5 4.74 2.73 19 -6 -5 4.16 1.55 -19 6 5 4.12 1.59 -19 -6 3 36.43 5.28 -19 6 3 24.32 3.88 -19 6 3 23.79 4.39 -19 -6 3 31.72 5.35 -19 6 3 20.88 3.06 -19 -6 3 27.54 3.77 -19 -6 1 189.90 11.67 -19 6 1 162.85 9.11 -19 6 1 162.02 8.08 -19 -6 1 182.19 9.29 -19 6 -1 66.90 6.89 -19 6 -1 84.62 7.80 -19 6 -1 77.51 5.49 -19 -6 -1 82.28 6.08 -19 6 -3 174.21 11.09 -19 -6 -3 226.20 12.29 -19 -6 -3 229.17 11.87 -19 6 -3 191.02 11.06 19 -6 3 130.55 6.49 -19 6 -3 163.06 7.73 -19 -6 -3 179.38 8.52 -19 6 -5 146.11 10.02 -19 -6 -5 208.60 11.10 -19 -6 -5 208.05 11.27 -19 6 -5 137.46 8.93 -19 6 -7 122.25 8.54 -19 7 2 56.66 4.44 -19 -7 0 181.47 10.69 -19 7 0 158.07 9.92 -19 -7 0 173.75 8.62 -19 7 -2 94.11 7.45 -20 0 8 95.41 7.48 -20 0 8 76.31 5.13 -20 0 6 19.55 2.79 -20 0 4 25.82 4.53 -20 0 2 185.96 11.66 -20 0 2 164.31 10.53 -20 0 0 101.96 8.59 -20 0 0 95.78 8.38 -20 0 -2 0.74 1.85 -20 0 -2 0.21 2.08 -20 0 -4 3.00 1.92 -20 0 -6 36.23 4.83 -20 0 -6 34.57 5.20 -20 0 -8 66.08 6.39 -20 0 -8 64.74 6.35 -20 -1 9 43.59 4.87 -20 1 9 44.19 4.98 -20 -1 9 35.13 3.50 -20 -1 7 76.37 6.88 -20 1 7 73.39 6.84 -20 1 7 46.51 3.93 -20 -1 7 52.69 4.42 -20 1 5 115.32 8.95 -20 -1 5 83.09 5.71 -20 -1 3 118.37 9.33 -20 1 3 121.54 9.27 -20 1 3 121.11 8.82 -20 -1 3 96.96 6.06 -20 -1 1 201.22 12.28 -20 1 1 196.62 11.78 -20 -1 1 208.26 11.90 -20 1 1 192.87 11.76 -20 -1 -1 35.94 5.23 -20 1 -1 39.56 5.26 -20 -1 -1 40.03 5.65 -20 1 -1 32.49 5.29 -20 -1 -3 11.33 3.16 -20 1 -3 13.00 3.08 -20 -1 -3 11.81 3.52 -20 1 -5 41.45 5.32 -20 -1 -5 42.76 4.89 -20 1 -5 30.92 4.04 -20 1 -5 45.68 5.82 -20 -1 -7 22.51 3.80 -20 1 -7 16.09 3.50 -20 -1 -7 19.17 3.86 -20 1 -7 18.65 3.74 -20 1 -9 106.94 7.84 -20 -1 -9 105.70 7.70 -20 1 -9 107.53 7.42 -20 -2 8 21.38 3.72 -20 -2 8 16.08 2.55 20 -2 -6 26.90 2.80 -20 -2 6 33.80 3.72 -20 2 4 376.55 15.96 -20 2 4 370.63 14.91 -20 2 2 21.94 4.13 -20 -2 2 16.83 3.97 -20 2 2 17.48 3.81 -20 -2 2 15.17 2.66 -20 -2 0 284.44 14.48 -20 2 0 244.24 12.63 -20 -2 0 294.92 14.11 -20 2 0 232.22 13.08 -20 -2 -2 13.47 3.57 -20 2 -2 14.81 3.23 -20 -2 -2 14.78 3.73 -20 2 -4 54.47 6.05 -20 -2 -4 56.41 5.94 -20 2 -4 42.71 4.67 -20 -2 -4 67.34 7.07 -20 2 -4 52.90 6.24 -20 2 -6 8.22 2.80 -20 -2 -6 5.67 2.07 -20 2 -6 6.56 2.53 -20 2 -8 53.20 5.83 -20 -2 -8 64.05 6.32 -20 2 -8 57.51 5.64 -20 -3 7 10.58 2.85 -20 3 7 11.12 2.88 -20 -3 7 8.22 2.02 -20 -3 5 174.37 10.55 -20 3 5 173.65 10.27 20 -3 -5 112.62 5.88 -20 -3 5 131.50 7.28 -20 3 3 139.26 9.29 -20 3 3 125.07 8.97 -20 -3 3 111.80 6.75 -20 -3 1 153.76 10.48 -20 3 1 151.49 9.56 -20 3 1 160.43 10.49 -20 -3 1 129.19 7.22 -20 -3 -1 50.34 6.16 -20 3 -1 36.32 4.63 -20 -3 -1 42.07 5.50 -20 3 -1 40.98 5.58 -20 3 -3 6.77 2.41 -20 -3 -3 5.79 2.45 -20 3 -3 6.36 2.01 -20 -3 -3 5.48 2.47 -20 3 -3 7.49 2.69 -20 3 -5 9.19 2.77 -20 -3 -5 14.61 3.22 -20 -3 -5 15.92 3.64 -20 3 -5 12.54 3.18 -20 3 -7 31.19 4.58 -20 3 -7 27.90 4.10 -20 -4 6 5.99 2.29 -20 4 6 4.54 2.08 20 -4 -6 3.27 1.22 -20 -4 6 3.78 1.62 -20 -4 4 52.86 5.94 -20 4 4 48.87 5.43 -20 4 4 52.78 5.57 20 -4 -4 34.24 3.32 -20 -4 4 46.70 4.46 -20 4 2 118.65 8.12 -20 4 2 116.93 8.66 -20 -4 2 127.27 7.22 -20 -4 0 27.55 4.69 -20 4 0 17.32 3.22 -20 4 0 17.06 3.71 -20 -4 0 23.79 3.14 -20 -4 -2 2.35 2.04 -20 -4 -2 3.06 2.15 -20 4 -2 0.73 1.64 -20 4 -4 5.31 2.19 -20 -4 -4 3.74 2.18 -20 -4 -4 3.77 2.15 -20 4 -4 3.88 2.11 -20 4 -6 61.08 6.05 -20 -4 -6 68.55 6.44 -20 4 -6 51.42 5.36 -20 -5 3 104.01 7.89 -20 5 3 89.34 7.13 -20 -5 3 87.03 5.85 -20 5 1 90.49 7.44 -20 -5 1 93.78 6.05 -20 -5 -1 30.88 4.62 -20 -5 -3 17.95 3.53 -20 5 -3 14.58 3.13 -21 0 3 246.76 11.94 -21 0 1 95.46 7.43 -21 0 1 96.34 7.21 -21 0 -1 17.43 3.41 -21 0 -1 20.73 3.76 -21 0 -3 37.18 4.35 -21 0 -3 38.71 4.93 -21 1 4 204.26 10.55 -21 -1 2 167.21 9.78 -21 1 2 148.15 9.07 -21 1 2 144.08 8.63 -21 -1 0 22.79 3.82 -21 1 0 17.68 3.36 -21 -1 0 20.98 3.63 -21 1 0 18.68 3.50 -21 -1 -2 7.56 2.43 -21 1 -2 4.75 1.98 -21 -1 -2 8.92 2.63 -21 1 -2 6.40 2.41 -21 -1 -4 86.48 7.04 -21 2 5 191.84 9.82 -21 2 3 177.32 9.62 -21 -2 1 31.14 4.50 -21 2 1 28.46 4.01 -21 2 1 32.97 4.34 -21 -2 -1 0.31 1.59 -21 -2 -1 1.58 1.65 -21 2 -1 0.31 1.44 -21 -2 -3 14.61 2.97 -21 -2 -3 17.65 3.35 -21 -3 0 6.11 2.46 -21 3 0 5.11 2.10 0 0 0 0.00 0.00 TITL R4-3 in I2/m REM I2/m (#12 in standard setting) CELL 1.34050 16.051242 11.420609 20.211658 90.0000 90.1944 90.0000 ZERR 13.00 0.000113 0.000082 0.000145 0.0000 0.0007 0.0000 LATT 2 SYMM -x, y,-z SFAC C H N O Cl In UNIT 13.00 13.00 13.00 13.00 13.00 156.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 16844 _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 2.931 _oxdiff_exptl_absorpt_empirical_full_min 0.454 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group In01 In 0.56439(3) 0.61688(5) 0.58288(2) 0.01956(10) Uani 1 1 d . . . . . In02 In 0.39627(3) 0.37816(4) 0.54901(2) 0.01945(10) Uani 1 1 d . . . . . In03 In 0.51030(3) 0.38298(5) 0.68806(2) 0.02686(12) Uani 1 1 d . . . . . In04 In 0.29732(3) 0.38777(5) 0.40239(3) 0.02665(12) Uani 1 1 d . . . . . In05 In 0.38042(3) 0.60894(5) 0.65901(2) 0.02630(12) Uani 1 1 d . . . . . In06 In 0.26123(3) 0.60903(5) 0.50895(3) 0.02571(12) Uani 1 1 d . . . . . Cl1 Cl 0.19920(19) 0.2890(3) 0.33049(18) 0.0722(10) Uani 1 1 d . . . . . Cl2 Cl 0.2969(2) 0.7192(3) 0.73596(14) 0.0628(8) Uani 1 1 d . . . . . O00J O 0.3306(4) 0.7112(5) 0.5781(3) 0.0355(13) Uani 1 1 d . . . . . O1 O 0.3685(3) 0.5077(5) 0.3388(3) 0.0273(12) Uani 1 1 d . . . . . O2 O 0.2016(3) 0.5083(6) 0.4322(3) 0.0331(13) Uani 1 1 d . . . . . O3 O 0.2996(4) 0.2852(6) 0.4942(3) 0.0343(13) Uani 1 1 d . . . . . O4 O 0.3633(3) 0.4975(4) 0.4741(2) 0.0188(9) Uani 1 1 d . . . . . O5 O 0.500000 0.2993(7) 0.500000 0.035(2) Uani 1 2 d S T P . . O6 O 0.3001(3) 0.4862(5) 0.6031(3) 0.0269(11) Uani 1 1 d . . . . . O7 O 0.4117(4) 0.2797(5) 0.6361(3) 0.0338(13) Uani 1 1 d . . . . . O8 O 0.4124(5) 0.4834(6) 0.7338(3) 0.0411(16) Uani 1 1 d . . . . . O9 O 0.4951(4) 0.7091(6) 0.6578(3) 0.0345(13) Uani 1 1 d . . . . . O10 O 0.4704(3) 0.4962(4) 0.6069(2) 0.0188(9) Uani 1 1 d . . . . . O11 O 0.500000 0.6943(7) 0.500000 0.0303(18) Uani 1 2 d S T P . . O12 O 0.6752(4) 0.7132(5) 0.5701(3) 0.0337(13) Uani 1 1 d . . . . . O13 O 0.6019(4) 0.2827(5) 0.6367(3) 0.0379(15) Uani 1 1 d . . . . . N1 N 0.4291(6) 0.4495(8) 0.2133(4) 0.0443(19) Uani 1 1 d . . . . . H1 H 0.431150 0.385631 0.180931 0.053 Uiso 1 1 calc R . . . . N2 N 0.1928(5) 0.7884(7) 0.5021(4) 0.0409(18) Uani 1 1 d . . . . . H2 H 0.132730 0.773941 0.504372 0.049 Uiso 1 1 calc R . . . . N3 N 0.1411(4) 0.5382(7) 0.5598(4) 0.0370(17) Uani 1 1 d . . . . . H3 H 0.098789 0.599925 0.558247 0.044 Uiso 1 1 calc R . . . . N4 N 0.5049(5) 0.2023(7) 0.7414(4) 0.0415(18) Uani 1 1 d . . . . . H4 H 0.505382 0.215388 0.789358 0.050 Uiso 1 1 calc R . . . . C1 C 0.4817(9) 0.5440(12) 0.1895(5) 0.059(3) Uani 1 1 d . . . . . H1A H 0.469381 0.615148 0.213793 0.071 Uiso 1 1 calc R . . . . H1B H 0.470138 0.558249 0.143049 0.071 Uiso 1 1 calc R . . . . C2 C 0.3412(7) 0.4832(10) 0.2225(5) 0.050(3) Uani 1 1 d . . . . . H2A H 0.307497 0.413043 0.226518 0.060 Uiso 1 1 calc R . . . . H2B H 0.322064 0.525804 0.183808 0.060 Uiso 1 1 calc R . . . . C3 C 0.3290(6) 0.5583(8) 0.2831(4) 0.038(2) Uani 1 1 d . . . . . H3A H 0.351929 0.635560 0.275150 0.045 Uiso 1 1 calc R . . . . H3B H 0.269919 0.566802 0.291749 0.045 Uiso 1 1 calc R . . . . C4 C 0.2953(9) 0.8227(12) 0.4143(7) 0.068(4) Uani 1 1 d . . . . . H4A H 0.295354 0.831833 0.366577 0.081 Uiso 1 1 calc R . . . . H4B H 0.332628 0.881060 0.432716 0.081 Uiso 1 1 calc R . . . . C5 C 0.2107(7) 0.8444(10) 0.4390(6) 0.052(3) Uani 1 1 d . . . . . H5A H 0.202791 0.928165 0.443731 0.062 Uiso 1 1 calc R . . . . H5B H 0.170891 0.816651 0.406369 0.062 Uiso 1 1 calc R . . . . C6 C 0.1178(5) 0.4742(10) 0.4474(5) 0.043(2) Uani 1 1 d . . . . . H6A H 0.101569 0.408479 0.419790 0.051 Uiso 1 1 calc R . . . . H6B H 0.080145 0.538648 0.438338 0.051 Uiso 1 1 calc R . . . . C7 C 0.1120(5) 0.4403(9) 0.5187(5) 0.040(2) Uani 1 1 d . . . . . H7A H 0.054817 0.421469 0.529692 0.048 Uiso 1 1 calc R . . . . H7B H 0.146061 0.371667 0.527050 0.048 Uiso 1 1 calc R . . . . C8 C 0.1554(6) 0.5071(10) 0.6296(5) 0.045(2) Uani 1 1 d . . . . . H8A H 0.107292 0.465313 0.646383 0.054 Uiso 1 1 calc R . . . . H8B H 0.162177 0.578006 0.655482 0.054 Uiso 1 1 calc R . . . . C9 C 0.2323(5) 0.4314(8) 0.6369(5) 0.0371(19) Uani 1 1 d . . . . . H9A H 0.245999 0.421915 0.683339 0.045 Uiso 1 1 calc R . . . . H9B H 0.221895 0.354483 0.618199 0.045 Uiso 1 1 calc R . . . . C10 C 0.2185(7) 0.8519(9) 0.5631(6) 0.057(3) Uani 1 1 d . . . . . H10A H 0.185358 0.824660 0.600028 0.068 Uiso 1 1 calc R . . . . H10B H 0.208023 0.934923 0.557395 0.068 Uiso 1 1 calc R . . . . C11 C 0.3110(7) 0.8328(8) 0.5785(5) 0.048(2) Uani 1 1 d . . . . . H11A H 0.344538 0.872992 0.545794 0.058 Uiso 1 1 calc R . . . . H11B H 0.323997 0.865506 0.621581 0.058 Uiso 1 1 calc R . . . . C12 C 0.2728(8) 0.1719(11) 0.5013(6) 0.059(3) Uani 1 1 d . . . . . H12A H 0.316303 0.119242 0.488233 0.089 Uiso 1 1 calc GR . . . . H12B H 0.224576 0.159370 0.474004 0.089 Uiso 1 1 calc GR . . . . H12C H 0.258678 0.157883 0.546772 0.089 Uiso 1 1 calc GR . . . . C13 C 0.3994(7) 0.1647(10) 0.6533(5) 0.047(2) Uani 1 1 d . . . . . H13A H 0.430851 0.114624 0.623747 0.057 Uiso 1 1 calc R . . . . H13B H 0.340836 0.145352 0.648420 0.057 Uiso 1 1 calc R . . . . C14 C 0.4261(8) 0.1427(10) 0.7230(5) 0.055(3) Uani 1 1 d . . . . . H14A H 0.382420 0.168762 0.752581 0.066 Uiso 1 1 calc R . . . . H14B H 0.433023 0.059011 0.729364 0.066 Uiso 1 1 calc R . . . . C15 C 0.5810(8) 0.1421(10) 0.7231(6) 0.059(3) Uani 1 1 d . . . . . H15A H 0.573457 0.058822 0.730201 0.071 Uiso 1 1 calc R . . . . H15B H 0.625611 0.168180 0.751989 0.071 Uiso 1 1 calc R . . . . C16 C 0.6063(8) 0.1613(9) 0.6537(6) 0.054(3) Uani 1 1 d . . . . . H16A H 0.662866 0.133462 0.647616 0.065 Uiso 1 1 calc R . . . . H16B H 0.570138 0.116783 0.624543 0.065 Uiso 1 1 calc R . . . . C17 C 0.4271(8) 0.5129(12) 0.8016(4) 0.058(3) Uani 1 1 d . . . . . H17A H 0.413009 0.446935 0.829714 0.069 Uiso 1 1 calc R . . . . H17B H 0.392511 0.578773 0.814207 0.069 Uiso 1 1 calc R . . . . C18 C 0.5065(8) 0.8230(10) 0.6804(7) 0.062(4) Uani 1 1 d . . . . . H18A H 0.564166 0.835014 0.691018 0.093 Uiso 1 1 calc GR . . . . H18B H 0.473303 0.835284 0.719218 0.093 Uiso 1 1 calc GR . . . . H18C H 0.489778 0.877215 0.646575 0.093 Uiso 1 1 calc GR . . . . Cl3 Cl 0.49706(17) 0.2507(3) 0.90156(13) 0.0540(6) Uani 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 In01 0.0178(2) 0.0212(2) 0.01961(19) -0.00107(17) 0.00031(15) -0.00187(17) In02 0.0195(2) 0.0195(2) 0.0193(2) -0.00061(17) 0.00292(15) -0.00215(18) In03 0.0334(3) 0.0292(3) 0.0181(2) 0.0039(2) 0.00141(18) 0.0005(2) In04 0.0219(2) 0.0294(3) 0.0286(2) -0.0081(2) -0.00187(18) -0.0028(2) In05 0.0256(2) 0.0302(3) 0.0231(2) -0.0075(2) 0.00588(18) 0.0011(2) In06 0.0171(2) 0.0265(2) 0.0335(3) -0.0065(2) 0.00363(18) 0.0018(2) Cl1 0.0511(15) 0.083(2) 0.083(2) -0.0461(18) -0.0214(15) -0.0095(14) Cl2 0.0622(16) 0.078(2) 0.0482(14) -0.0246(13) 0.0196(13) 0.0198(15) O00J 0.044(3) 0.025(3) 0.037(3) -0.008(2) -0.007(3) 0.004(2) O1 0.026(3) 0.035(3) 0.021(3) -0.001(2) -0.008(2) 0.001(2) O2 0.017(2) 0.041(3) 0.042(3) -0.008(3) -0.002(2) 0.000(2) O3 0.033(3) 0.042(3) 0.028(3) -0.003(2) 0.000(2) -0.010(3) O4 0.017(2) 0.020(2) 0.019(2) 0.0013(18) 0.0016(18) -0.0014(19) O5 0.026(4) 0.028(4) 0.051(5) 0.000 0.026(4) 0.000 O6 0.022(3) 0.031(3) 0.028(3) -0.005(2) 0.007(2) -0.001(2) O7 0.043(3) 0.030(3) 0.028(3) 0.012(2) 0.001(3) -0.009(2) O8 0.054(4) 0.052(4) 0.017(3) 0.001(3) 0.011(3) 0.006(3) O9 0.029(3) 0.038(3) 0.036(3) -0.014(3) 0.003(2) -0.002(2) O10 0.022(2) 0.019(2) 0.015(2) -0.0024(18) 0.0025(18) -0.0046(19) O11 0.049(5) 0.022(4) 0.020(3) 0.000 -0.016(3) 0.000 O12 0.027(3) 0.032(3) 0.042(3) -0.006(2) 0.005(2) -0.011(2) O13 0.039(3) 0.028(3) 0.048(4) 0.009(3) 0.015(3) 0.003(2) N1 0.059(5) 0.053(5) 0.020(3) -0.006(3) -0.003(3) 0.005(4) N2 0.023(3) 0.036(4) 0.063(5) -0.004(4) 0.005(3) 0.007(3) N3 0.018(3) 0.043(4) 0.050(4) -0.008(3) 0.007(3) 0.004(3) N4 0.058(5) 0.040(4) 0.027(3) 0.011(3) 0.003(3) 0.001(4) C1 0.087(9) 0.067(7) 0.022(4) 0.014(4) -0.001(5) -0.002(7) C2 0.068(7) 0.055(6) 0.027(4) -0.006(4) -0.018(4) 0.012(5) C3 0.049(5) 0.039(5) 0.025(4) 0.002(3) -0.012(4) 0.009(4) C4 0.072(8) 0.065(8) 0.066(8) 0.026(6) 0.011(7) 0.034(7) C5 0.049(6) 0.046(6) 0.062(7) 0.013(5) -0.009(5) 0.014(5) C6 0.019(4) 0.061(6) 0.048(5) -0.005(4) -0.004(4) -0.005(4) C7 0.019(4) 0.051(5) 0.050(5) 0.000(4) 0.000(3) -0.010(4) C8 0.027(4) 0.058(6) 0.049(5) -0.012(4) 0.019(4) -0.006(4) C9 0.030(4) 0.042(5) 0.039(5) 0.002(4) 0.012(4) -0.008(4) C10 0.061(7) 0.036(5) 0.074(7) -0.018(5) 0.003(6) 0.015(5) C11 0.067(7) 0.027(4) 0.052(6) -0.005(4) -0.005(5) 0.000(4) C12 0.068(8) 0.055(7) 0.055(7) -0.001(5) 0.001(6) -0.023(6) C13 0.050(6) 0.042(5) 0.050(6) 0.016(4) 0.008(5) -0.012(5) C14 0.069(7) 0.048(6) 0.048(6) 0.024(5) 0.009(5) -0.006(5) C15 0.066(7) 0.042(6) 0.069(7) 0.026(5) 0.001(6) 0.008(5) C16 0.067(7) 0.029(5) 0.067(7) 0.007(5) 0.019(6) -0.001(5) C17 0.082(8) 0.074(8) 0.018(4) -0.004(4) 0.017(4) 0.009(6) C18 0.049(6) 0.047(6) 0.091(10) -0.035(6) 0.004(6) 0.002(5) Cl3 0.0516(14) 0.0702(17) 0.0401(12) 0.0157(12) -0.0003(11) -0.0079(12) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0147 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3292 0.5397 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In 0.1337 3.9104 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0253 0.0135 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag In05 In01 In06 173.246(19) . 2_656 ? O1 In01 In05 94.67(15) 2_656 . ? O1 In01 In06 88.66(15) 2_656 2_656 ? O4 In01 In05 135.77(14) 2_656 . ? O4 In01 In06 39.57(14) 2_656 2_656 ? O4 In01 O1 76.6(2) 2_656 2_656 ? O4 In01 O9 167.2(2) 2_656 . ? O4 In01 O11 95.90(18) 2_656 . ? O9 In01 In05 39.63(16) . . ? O9 In01 In06 146.34(17) . 2_656 ? O9 In01 O1 91.3(2) . 2_656 ? O10 In01 In05 40.38(14) . . ? O10 In01 In06 135.16(14) . 2_656 ? O10 In01 O1 79.6(2) . 2_656 ? O10 In01 O4 95.6(2) . 2_656 ? O10 In01 O9 77.6(2) . . ? O10 In01 O11 96.07(19) . . ? O10 In01 O12 167.8(2) . . ? O11 In01 In05 86.947(19) . . ? O11 In01 In06 88.843(17) . 2_656 ? O11 In01 O1 170.8(2) . 2_656 ? O11 In01 O9 95.6(2) . . ? O12 In01 In05 145.03(17) . . ? O12 In01 In06 40.75(17) . 2_656 ? O12 In01 O1 88.5(2) . 2_656 ? O12 In01 O4 78.8(2) . 2_656 ? O12 In01 O9 105.6(2) . . ? O12 In01 O11 95.3(2) . . ? In03 In02 In04 174.346(19) . . ? O3 In02 In03 145.14(17) . . ? O3 In02 In04 40.01(16) . . ? O3 In02 O6 91.5(2) . . ? O4 In02 In03 136.77(14) . . ? O4 In02 In04 39.37(14) . . ? O4 In02 O3 76.9(2) . . ? O4 In02 O5 97.69(19) . . ? O4 In02 O6 79.8(2) . . ? O4 In02 O10 97.1(2) . . ? O5 In02 In03 88.366(17) . . ? O5 In02 In04 88.373(19) . . ? O5 In02 O3 96.5(2) . . ? O5 In02 O6 170.9(2) . . ? O5 In02 O10 94.92(19) . . ? O6 In02 In03 87.56(15) . . ? O6 In02 In04 95.00(15) . . ? O7 In02 In03 40.86(16) . . ? O7 In02 In04 144.10(17) . . ? O7 In02 O3 104.3(2) . . ? O7 In02 O4 167.9(2) . . ? O7 In02 O5 94.2(2) . . ? O7 In02 O6 88.0(2) . . ? O7 In02 O10 79.4(2) . . ? O10 In02 In03 39.72(14) . . ? O10 In02 In04 136.12(14) . . ? O10 In02 O3 167.7(2) . . ? O10 In02 O6 76.80(19) . . ? In02 In03 In05 61.972(14) . . ? O1 In03 In02 104.67(12) 2_656 . ? O1 In03 In05 90.40(13) 2_656 . ? O7 In03 In02 38.02(14) . . ? O7 In03 In05 83.41(16) . . ? O7 In03 O1 139.26(19) . 2_656 ? O7 In03 N1 149.7(3) . 2_656 ? O7 In03 N4 73.9(3) . . ? O8 In03 In02 88.37(17) . . ? O8 In03 In05 38.32(16) . . ? O8 In03 O1 111.2(2) . 2_656 ? O8 In03 O7 88.1(3) . . ? O8 In03 O10 78.2(2) . . ? O8 In03 N1 76.3(3) . 2_656 ? O8 In03 N4 104.2(3) . . ? O10 In03 In02 38.86(13) . . ? O10 In03 In05 40.13(13) . . ? O10 In03 O1 73.88(18) . 2_656 ? O10 In03 O7 75.76(19) . . ? O10 In03 N1 124.6(2) . 2_656 ? O10 In03 N4 149.5(2) . . ? O13 In03 In02 87.62(19) . . ? O13 In03 In05 138.84(17) . . ? O13 In03 O1 70.1(2) . 2_656 ? O13 In03 O7 88.6(3) . . ? O13 In03 O8 176.0(3) . . ? O13 In03 O10 98.8(2) . . ? O13 In03 N1 107.7(3) . 2_656 ? O13 In03 N4 77.1(3) . . ? N1 In03 In02 160.7(2) 2_656 . ? N1 In03 In05 98.9(2) 2_656 . ? N1 In03 O1 71.1(2) 2_656 2_656 ? N4 In03 In02 110.7(2) . . ? N4 In03 In05 137.3(2) . . ? N4 In03 O1 130.0(2) . 2_656 ? N4 In03 N1 84.8(3) . 2_656 ? In02 In04 In06 62.786(15) . . ? Cl1 In04 In02 145.07(11) . . ? Cl1 In04 In06 128.34(8) . . ? O1 In04 In02 106.89(13) . . ? O1 In04 In06 89.83(15) . . ? O1 In04 Cl1 106.13(17) . . ? O2 In04 In02 96.29(17) . . ? O2 In04 In06 38.44(15) . . ? O2 In04 Cl1 90.14(17) . . ? O2 In04 O1 97.9(2) . . ? O2 In04 O3 96.6(2) . . ? O2 In04 O4 78.0(2) . . ? O2 In04 O13 172.9(3) . 2_656 ? O3 In04 In02 39.66(15) . . ? O3 In04 In06 82.09(17) . . ? O3 In04 Cl1 105.55(19) . . ? O3 In04 O1 145.0(2) . . ? O4 In04 In02 37.58(13) . . ? O4 In04 In06 39.73(13) . . ? O4 In04 Cl1 168.06(16) . . ? O4 In04 O1 77.24(18) . . ? O4 In04 O3 74.9(2) . . ? O13 In04 In02 87.25(18) 2_656 . ? O13 In04 In06 141.13(17) 2_656 . ? O13 In04 Cl1 90.47(19) 2_656 . ? O13 In04 O1 75.1(2) 2_656 . ? O13 In04 O3 90.1(3) 2_656 . ? O13 In04 O4 101.5(2) 2_656 . ? In01 In05 In03 63.437(15) . . ? Cl2 In05 In01 141.09(9) . . ? Cl2 In05 In03 129.27(9) . . ? O00J In05 In01 87.81(18) . . ? O00J In05 In03 140.63(17) . . ? O00J In05 Cl2 90.06(19) . . ? O00J In05 O6 75.1(2) . . ? O00J In05 O9 91.0(3) . . ? O00J In05 O10 101.2(2) . . ? O6 In05 In01 107.25(14) . . ? O6 In05 In03 87.85(15) . . ? O6 In05 Cl2 109.66(16) . . ? O8 In05 In01 97.65(18) . . ? O8 In05 In03 38.58(17) . . ? O8 In05 Cl2 91.54(19) . . ? O8 In05 O00J 169.1(3) . . ? O8 In05 O6 94.3(2) . . ? O8 In05 O9 99.2(3) . . ? O8 In05 O10 77.9(2) . . ? O9 In05 In01 39.39(15) . . ? O9 In05 In03 83.18(17) . . ? O9 In05 Cl2 101.87(18) . . ? O9 In05 O6 145.3(2) . . ? O9 In05 O10 75.2(2) . . ? O10 In05 In01 38.10(13) . . ? O10 In05 In03 39.65(13) . . ? O10 In05 Cl2 168.32(15) . . ? O10 In05 O6 76.55(18) . . ? In01 In06 In04 61.483(14) 2_656 . ? O00J In06 In01 85.01(18) . 2_656 ? O00J In06 In04 137.58(17) . . ? O00J In06 O2 174.1(3) . . ? O00J In06 O4 98.0(2) . . ? O00J In06 O6 70.9(2) . . ? O00J In06 O12 86.5(3) . 2_656 ? O00J In06 N2 78.6(3) . . ? O00J In06 N3 109.4(3) . . ? O2 In06 In01 89.17(16) . 2_656 ? O2 In06 In04 38.39(16) . . ? O2 In06 O4 77.8(2) . . ? O2 In06 O6 111.5(2) . . ? O2 In06 O12 88.4(2) . 2_656 ? O2 In06 N2 102.6(3) . . ? O2 In06 N3 76.5(3) . . ? O4 In06 In01 38.26(13) . 2_656 ? O4 In06 In04 39.61(13) . . ? O4 In06 O6 74.16(18) . . ? O4 In06 O12 74.76(19) . 2_656 ? O4 In06 N2 147.6(2) . . ? O4 In06 N3 124.0(2) . . ? O6 In06 In01 103.52(13) . 2_656 ? O6 In06 In04 91.31(13) . . ? O12 In06 In01 37.90(14) 2_656 2_656 ? O12 In06 In04 82.12(16) 2_656 . ? O12 In06 O6 138.1(2) 2_656 . ? O12 In06 N2 72.9(3) 2_656 . ? O12 In06 N3 151.3(3) 2_656 . ? N2 In06 In01 109.7(2) . 2_656 ? N2 In06 In04 134.7(2) . . ? N2 In06 O6 132.2(3) . . ? N2 In06 N3 86.6(3) . . ? N3 In06 In01 160.49(19) . 2_656 ? N3 In06 In04 99.53(19) . . ? N3 In06 O6 70.5(2) . . ? In06 O00J In05 113.1(3) . . ? C11 O00J In05 127.1(6) . . ? C11 O00J In06 115.0(6) . . ? In01 O1 In03 95.60(19) 2_656 2_656 ? In04 O1 In01 100.4(2) . 2_656 ? In04 O1 In03 100.4(2) . 2_656 ? C3 O1 In01 122.6(5) . 2_656 ? C3 O1 In03 114.3(5) . 2_656 ? C3 O1 In04 119.1(5) . . ? In04 O2 In06 103.2(2) . . ? C6 O2 In04 123.9(6) . . ? C6 O2 In06 114.0(5) . . ? In02 O3 In04 100.3(2) . . ? C12 O3 In02 129.0(7) . . ? C12 O3 In04 126.0(6) . . ? In01 O4 In04 105.7(2) 2_656 . ? In01 O4 In06 102.2(2) 2_656 . ? In02 O4 In01 131.9(3) . 2_656 ? In02 O4 In04 103.0(2) . . ? In02 O4 In06 109.4(2) . . ? In04 O4 In06 100.7(2) . . ? In02 O5 In02 130.2(4) 2_656 . ? In02 O6 In06 96.3(2) . . ? In05 O6 In02 101.3(2) . . ? In05 O6 In06 100.4(2) . . ? C9 O6 In02 120.9(5) . . ? C9 O6 In05 118.4(5) . . ? C9 O6 In06 115.4(5) . . ? In02 O7 In03 101.1(2) . . ? C13 O7 In02 134.9(6) . . ? C13 O7 In03 119.3(6) . . ? In05 O8 In03 103.1(2) . . ? C17 O8 In03 114.7(7) . . ? C17 O8 In05 123.9(7) . . ? In01 O9 In05 101.0(2) . . ? C18 O9 In01 128.3(7) . . ? C18 O9 In05 126.9(7) . . ? In01 O10 In02 133.2(2) . . ? In01 O10 In03 110.7(2) . . ? In01 O10 In05 101.5(2) . . ? In02 O10 In03 101.4(2) . . ? In02 O10 In05 105.3(2) . . ? In03 O10 In05 100.2(2) . . ? In01 O11 In01 131.6(4) 2_656 . ? In01 O12 In06 101.4(2) . 2_656 ? C4 O12 In01 137.5(7) 2_656 . ? C4 O12 In06 119.3(7) 2_656 2_656 ? In03 O13 In04 113.3(3) . 2_656 ? C16 O13 In03 115.9(6) . . ? C16 O13 In04 126.1(6) . 2_656 ? In03 N1 H1 108.2 2_656 . ? C1 N1 In03 106.4(6) . 2_656 ? C1 N1 H1 108.2 . . ? C1 N1 C2 113.9(9) . . ? C2 N1 In03 111.8(5) . 2_656 ? C2 N1 H1 108.2 . . ? In06 N2 H2 108.2 . . ? C5 N2 In06 110.2(6) . . ? C5 N2 H2 108.2 . . ? C5 N2 C10 117.2(9) . . ? C10 N2 In06 104.5(6) . . ? C10 N2 H2 108.2 . . ? In06 N3 H3 108.1 . . ? C7 N3 In06 106.0(5) . . ? C7 N3 H3 108.1 . . ? C7 N3 C8 114.0(8) . . ? C8 N3 In06 112.4(5) . . ? C8 N3 H3 108.1 . . ? In03 N4 H4 108.8 . . ? C14 N4 In03 108.9(6) . . ? C14 N4 H4 108.8 . . ? C15 N4 In03 105.6(6) . . ? C15 N4 H4 108.8 . . ? C15 N4 C14 115.9(9) . . ? N1 C1 H1A 109.6 . . ? N1 C1 H1B 109.6 . . ? N1 C1 C17 110.4(10) . 2_656 ? H1A C1 H1B 108.1 . . ? C17 C1 H1A 109.6 2_656 . ? C17 C1 H1B 109.6 2_656 . ? N1 C2 H2A 109.2 . . ? N1 C2 H2B 109.2 . . ? N1 C2 C3 112.2(8) . . ? H2A C2 H2B 107.9 . . ? C3 C2 H2A 109.2 . . ? C3 C2 H2B 109.2 . . ? O1 C3 C2 110.9(7) . . ? O1 C3 H3A 109.5 . . ? O1 C3 H3B 109.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? O12 C4 H4A 108.9 2_656 . ? O12 C4 H4B 108.9 2_656 . ? O12 C4 C5 113.2(11) 2_656 . ? H4A C4 H4B 107.8 . . ? C5 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? N2 C5 C4 114.1(8) . . ? N2 C5 H5A 108.7 . . ? N2 C5 H5B 108.7 . . ? C4 C5 H5A 108.7 . . ? C4 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? O2 C6 H6A 109.7 . . ? O2 C6 H6B 109.7 . . ? O2 C6 C7 109.7(7) . . ? H6A C6 H6B 108.2 . . ? C7 C6 H6A 109.7 . . ? C7 C6 H6B 109.7 . . ? N3 C7 C6 109.2(8) . . ? N3 C7 H7A 109.8 . . ? N3 C7 H7B 109.8 . . ? C6 C7 H7A 109.8 . . ? C6 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? N3 C8 C9 110.8(7) . . ? H8A C8 H8B 108.1 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? O6 C9 C8 109.0(7) . . ? O6 C9 H9A 109.9 . . ? O6 C9 H9B 109.9 . . ? C8 C9 H9A 109.9 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 108.3 . . ? N2 C10 H10A 109.3 . . ? N2 C10 H10B 109.3 . . ? N2 C10 C11 111.4(8) . . ? H10A C10 H10B 108.0 . . ? C11 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? O00J C11 C10 110.7(9) . . ? O00J C11 H11A 109.5 . . ? O00J C11 H11B 109.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? O3 C12 H12A 109.5 . . ? O3 C12 H12B 109.5 . . ? O3 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O7 C13 H13A 109.4 . . ? O7 C13 H13B 109.4 . . ? O7 C13 C14 111.0(9) . . ? H13A C13 H13B 108.0 . . ? C14 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? N4 C14 C13 113.7(8) . . ? N4 C14 H14A 108.8 . . ? N4 C14 H14B 108.8 . . ? C13 C14 H14A 108.8 . . ? C13 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? N4 C15 H15A 108.7 . . ? N4 C15 H15B 108.7 . . ? N4 C15 C16 114.1(9) . . ? H15A C15 H15B 107.6 . . ? C16 C15 H15A 108.7 . . ? C16 C15 H15B 108.7 . . ? O13 C16 C15 111.0(9) . . ? O13 C16 H16A 109.4 . . ? O13 C16 H16B 109.4 . . ? C15 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? O8 C17 C1 108.9(8) . 2_656 ? O8 C17 H17A 109.9 . . ? O8 C17 H17B 109.9 . . ? C1 C17 H17A 109.9 2_656 . ? C1 C17 H17B 109.9 2_656 . ? H17A C17 H17B 108.3 . . ? O9 C18 H18A 109.5 . . ? O9 C18 H18B 109.5 . . ? O9 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? 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 In01 In05 3.3357(6) . ? In01 In06 3.3648(6) 2_656 ? In01 O1 2.282(5) 2_656 ? In01 O4 2.131(5) 2_656 ? In01 O9 2.156(6) . ? In01 O10 2.101(5) . ? In01 O11 2.155(3) . ? In01 O12 2.108(6) . ? In02 In03 3.3490(6) . ? In02 In04 3.3593(6) . ? In02 O3 2.180(6) . ? In02 O4 2.103(5) . ? In02 O5 2.139(4) . ? In02 O6 2.260(5) . ? In02 O7 2.102(5) . ? In02 O10 2.144(5) . ? In03 In05 3.3677(8) . ? In03 O1 2.473(6) 2_656 ? In03 O7 2.233(6) . ? In03 O8 2.156(7) . ? In03 O10 2.183(5) . ? In03 O13 2.136(6) . ? In03 N1 2.342(8) 2_656 ? In03 N4 2.331(7) . ? In04 In06 3.3717(7) . ? In04 Cl1 2.418(2) . ? In04 O1 2.201(6) . ? In04 O2 2.151(6) . ? In04 O3 2.195(6) . ? In04 O4 2.187(5) . ? In04 O13 2.165(6) 2_656 ? In05 Cl2 2.412(2) . ? In05 O00J 2.161(6) . ? In05 O6 2.212(6) . ? In05 O8 2.144(6) . ? In05 O9 2.167(6) . ? In05 O10 2.205(5) . ? In06 O00J 2.131(6) . ? In06 O2 2.153(6) . ? In06 O4 2.193(5) . ? In06 O6 2.443(6) . ? In06 O12 2.240(6) 2_656 ? In06 N2 2.328(7) . ? In06 N3 2.333(7) . ? O00J C11 1.424(11) . ? O1 C3 1.414(9) . ? O2 C6 1.434(10) . ? O3 C12 1.371(13) . ? O6 C9 1.432(9) . ? O7 C13 1.373(11) . ? O8 C17 1.431(11) . ? O9 C18 1.390(12) . ? O12 C4 1.374(13) 2_656 ? O13 C16 1.430(12) . ? N1 H1 0.9800 . ? N1 C1 1.453(15) . ? N1 C2 1.476(14) . ? N2 H2 0.9800 . ? N2 C5 1.455(14) . ? N2 C10 1.487(13) . ? N3 H3 0.9800 . ? N3 C7 1.468(12) . ? N3 C8 1.470(13) . ? N4 H4 0.9800 . ? N4 C14 1.482(14) . ? N4 C15 1.450(14) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C17 1.516(17) 2_656 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C3 1.507(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 C5 1.469(17) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C7 1.495(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C9 1.515(14) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C11 1.531(15) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.494(15) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 C16 1.477(16) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? 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 In01 O1 C3 C2 142.0(7) 2_656 . . . ? In02 O6 C9 C8 -143.9(6) . . . . ? In02 O7 C13 C14 176.7(7) . . . . ? In03 O1 C3 C2 27.4(10) 2_656 . . . ? In03 O7 C13 C14 26.1(12) . . . . ? In03 O8 C17 C1 39.4(12) . . . 2_656 ? In03 O13 C16 C15 -29.6(13) . . . . ? In03 N1 C1 C17 41.6(10) 2_656 . . 2_656 ? In03 N1 C2 C3 46.4(10) 2_656 . . . ? In03 N4 C14 C13 35.5(11) . . . . ? In03 N4 C15 C16 -38.3(12) . . . . ? In04 O1 C3 C2 -91.1(9) . . . . ? In04 O2 C6 C7 87.3(9) . . . . ? In04 O13 C16 C15 124.3(9) 2_656 . . . ? In05 O00J C11 C10 -120.1(8) . . . . ? In05 O6 C9 C8 90.4(8) . . . . ? In05 O8 C17 C1 -88.1(11) . . . 2_656 ? In06 O00J C11 C10 33.4(11) . . . . ? In06 O2 C6 C7 -39.4(10) . . . . ? In06 O6 C9 C8 -28.6(9) . . . . ? In06 N2 C5 C4 -34.6(12) . . . . ? In06 N2 C10 C11 40.5(10) . . . . ? In06 N3 C7 C6 -43.4(8) . . . . ? In06 N3 C8 C9 -48.9(9) . . . . ? O2 C6 C7 N3 56.3(10) . . . . ? O7 C13 C14 N4 -41.2(14) . . . . ? O12 C4 C5 N2 34.3(17) 2_656 . . . ? N1 C2 C3 O1 -49.1(12) . . . . ? N2 C10 C11 O00J -51.0(13) . . . . ? N3 C8 C9 O6 50.5(10) . . . . ? N4 C15 C16 O13 46.7(15) . . . . ? C1 N1 C2 C3 -74.2(10) . . . . ? C2 N1 C1 C17 165.2(8) . . . 2_656 ? C5 N2 C10 C11 -81.7(11) . . . . ? C7 N3 C8 C9 71.8(9) . . . . ? C8 N3 C7 C6 -167.6(7) . . . . ? C10 N2 C5 C4 84.6(13) . . . . ? C14 N4 C15 C16 82.3(12) . . . . ? C15 N4 C14 C13 -83.2(12) . . . . ?