#------------------------------------------------------------------------------ #$Date: 2020-04-05 12:54:22 +0300 (Sun, 05 Apr 2020) $ #$Revision: 250148 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/71/1557174.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_1557174 loop_ _publ_author_name 'Tickner, Ben. J.' 'Semenova, Olga' 'Iali, Wissam' 'Rayner, Peter J.' 'Whitwood, Adrian C.' 'Duckett, Simon B.' _publ_section_title ; Optimisation of pyruvate hyperpolarisation using SABRE by tuning the active magnetisation transfer catalyst ; _journal_issue 5 _journal_name_full 'Catalysis Science & Technology' _journal_page_first 1343 _journal_paper_doi 10.1039/C9CY02498K _journal_volume 10 _journal_year 2020 _chemical_formula_moiety 'C56 H64 Cl2 Ir2 N4 S2, C H4 O' _chemical_formula_sum 'C57 H68 Cl2 Ir2 N4 O S2' _chemical_formula_weight 1344.57 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2019-09-30 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-10-04 deposited with the CCDC. 2019-12-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.2757(13) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.9317(2) _cell_length_b 16.6000(3) _cell_length_c 25.5365(4) _cell_measurement_reflns_used 9511 _cell_measurement_temperature 110.00(10) _cell_measurement_theta_max 70.9880 _cell_measurement_theta_min 6.5490 _cell_volume 5481.76(16) _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (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 N~2~ _diffrn_ambient_temperature 110.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1450 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -13.00 52.00 1.00 1.00 -- 0.00 57.00 -60.00 65 2 \w -51.00 -20.00 1.00 1.00 -- 0.00 124.00 101.00 31 3 \w -13.00 13.00 1.00 3.00 -- 54.00 -57.00-150.00 26 4 \w 27.00 105.00 1.00 3.00 -- 54.00-125.00 120.00 78 5 \w -19.00 98.00 1.00 3.00 -- 54.00 -19.00 -60.00 117 6 \w 40.00 74.00 1.00 3.00 -- 54.00 -57.00 120.00 34 7 \w 92.00 119.00 1.00 3.00 -- 54.00 77.00 -90.00 27 8 \w 39.00 97.00 1.00 3.00 -- 108.00-111.00-120.00 58 9 \w 124.00 176.00 1.00 3.00 -- 108.00 50.00-150.00 52 10 \w 38.00 92.00 1.00 3.00 -- 108.00-111.00 120.00 54 11 \w 77.00 103.00 1.00 3.00 -- 108.00 -50.00 -30.00 26 12 \w 36.00 88.00 1.00 3.00 -- 108.00-111.00-180.00 52 13 \w 38.00 73.00 1.00 3.00 -- 108.00 -50.00 -30.00 35 14 \w 106.00 171.00 1.00 3.00 -- 108.00 63.00 0.00 65 15 \w 77.00 113.00 1.00 3.00 -- 108.00-111.00 -90.00 36 16 \w 90.00 176.00 1.00 3.00 -- 108.00 63.00 120.00 86 17 \w 113.00 139.00 1.00 3.00 -- 108.00 -12.00-150.00 26 18 \w 36.00 73.00 1.00 3.00 -- 108.00 -12.00-150.00 37 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0536477000 _diffrn_orient_matrix_UB_12 -0.0704874000 _diffrn_orient_matrix_UB_13 0.0284325000 _diffrn_orient_matrix_UB_21 -0.0369154000 _diffrn_orient_matrix_UB_22 0.0333776000 _diffrn_orient_matrix_UB_23 0.0530168000 _diffrn_orient_matrix_UB_31 -0.0996791000 _diffrn_orient_matrix_UB_32 -0.0503459000 _diffrn_orient_matrix_UB_33 -0.0047444000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_unetI/netI 0.0331 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 20688 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.076 _diffrn_reflns_theta_max 67.076 _diffrn_reflns_theta_min 3.462 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 11.192 _exptl_absorpt_correction_T_max 0.674 _exptl_absorpt_correction_T_min 0.403 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.629 _exptl_crystal_description block _exptl_crystal_F_000 2664 _exptl_crystal_recrystallization_method 'crystallisation from methanol' _exptl_crystal_size_max 0.149 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.078 _refine_diff_density_max 1.916 _refine_diff_density_min -1.357 _refine_diff_density_rms 0.098 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 650 _refine_ls_number_reflns 9782 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0299 _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^)+(0.0265P)^2^+13.1045P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.0712 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8700 _reflns_number_total 9782 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cy02498k2.cif _cod_data_source_block sbd1906 _cod_depositor_comments 'Adding full bibliography for 1557173--1557174.cif.' _cod_original_cell_volume 5481.76(15) _cod_database_code 1557174 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C57 H64 Cl2 Ir2 N4 O S2' _chemical_oxdiff_usercomment 'Ben Tickner BT Ma1' _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 0.476 _shelx_estimated_absorpt_t_min 0.286 _reflns_odcompleteness_completeness 99.73 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances C46A-Cl1A \\sim Cl1A-C48A with sigma of 0.02 C43A-C44A \\sim C44-C43 with sigma of 0.02 S1-C43 \\sim S1-C43A with sigma of 0.02 C49A-C43A \\sim C43A-C45A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C49A) = Uanis(C49) Uanis(C48) = Uanis(C48A) Uanis(C47A) = Uanis(C47) Uanis(C46A) = Uanis(C46) Uanis(C45A) = Uanis(C45) Uanis(C44A) = Uanis(C44) Uanis(C43A) = Uanis(C43) 4. Others Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)= Sof(H46A)=Sof(C47A)=Sof(C48A)=Sof(H48A)=Sof(C49A)=Sof(H49A)=Sof(Cl1A)=1-FVAR(1) Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)= Sof(C47)=Sof(C48)=Sof(H48)=Sof(C49)=Sof(H49)=Sof(Cl1)=FVAR(1) 5.a Riding coordinates: Ir1(H,HA), Ir2(HB,HC) 5.b Secondary CH2 refined with riding coordinates: C43(H43A,H43B), C43A(H43C,H43D), C50(H50A,H50B) 5.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C6(H6), C8(H8), C15(H15), C17(H17), C23(H23), C24(H24), C27(H27), C29(H29), C36(H36), C38(H38), C45A(H45A), C46A(H46A), C48A(H48A), C49A(H49A), C45(H45), C46(H46), C48(H48), C49(H49), C52(H52), C53(H53), C55(H55), C56(H56) 5.d Fitted hexagon refined as free rotating group: C44A(C45A,C46A,C47A,C48A,C49A) 5.e Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B, H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C32(H32A, H32B,H32C), C33(H33A,H33B,H33C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C57(H57A,H57B,H57C) 5.f Idealised tetrahedral OH refined as rotating group: O1(H1) ; _shelx_res_file ; TITL sbd1906_a.res in P2(1)/c sbd1906.res created by SHELXL-2018/3 at 12:17:47 on 30-Sep-2019 REM Old TITL sbd1906 in P21/c #14 REM SHELXT solution in P2(1)/c: R1 0.097, Rweak 0.005, Alpha 0.061 REM 0.535 for 379 systematic absences, Orientation as input REM Formula found by SHELXT: C55 N6 O S4 Ir2 CELL 1.54184 12.931718 16.59997 25.536489 90 90.2757 90 ZERR 4 0.000199 0.0003 0.000382 0 0.0013 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Ir N O S UNIT 228 272 8 8 16 4 8 SADI C46A Cl1A Cl1A C48A SADI C43A C44A C44 C43 SADI S1 C43 S1 C43A SADI C49A C43A C43A C45A EADP C49A C49 EADP C48 C48A EADP C47A C47 EADP C46A C46 EADP C45A C45 EADP C44A C44 EADP C43A C43 L.S. 14 0 0 PLAN 40 SIZE 0.078 0.09 0.149 TEMP -163.15(10) BOND list 4 fmap 2 53 acta REM REM REM WGHT 0.026500 13.104500 FVAR 1.79572 0.80236 C0AA 1 0.242171 0.383941 0.261557 11.00000 0.03806 0.03150 = 0.02342 -0.00365 0.00379 0.00658 C2 1 0.250746 0.405428 0.173440 11.00000 0.06144 0.09683 = 0.01549 0.00252 -0.00061 0.03553 AFIX 43 H2 2 0.277677 0.408767 0.138962 11.00000 -1.20000 AFIX 0 C3 1 0.154435 0.422098 0.187839 11.00000 0.05793 0.12598 = 0.02050 0.00114 -0.00414 0.04507 AFIX 43 H3 2 0.100011 0.440039 0.165607 11.00000 -1.20000 AFIX 0 C4 1 0.412441 0.362300 0.216379 11.00000 0.03546 0.04178 = 0.01393 0.00095 0.00481 0.00295 C5 1 0.440552 0.282167 0.209703 11.00000 0.03817 0.03891 = 0.01240 -0.00344 0.00248 0.00377 C6 1 0.545374 0.264032 0.204756 11.00000 0.04638 0.04852 = 0.01669 -0.00627 0.00224 0.01589 AFIX 43 H6 2 0.566074 0.209398 0.201231 11.00000 -1.20000 AFIX 0 C7 1 0.619811 0.323821 0.204872 11.00000 0.03241 0.07214 = 0.01804 -0.00424 0.00421 0.00398 C8 1 0.588461 0.403282 0.210751 11.00000 0.04954 0.05771 = 0.02213 0.00203 0.00874 -0.01516 AFIX 43 H8 2 0.639251 0.444629 0.211150 11.00000 -1.20000 AFIX 0 C9 1 0.484312 0.424241 0.216103 11.00000 0.05358 0.04494 = 0.01789 0.00471 0.00977 -0.00007 C10 1 0.360244 0.216263 0.206445 11.00000 0.05025 0.04731 = 0.02984 -0.01018 0.00170 -0.00454 AFIX 137 H10A 2 0.330470 0.214991 0.171092 11.00000 -1.50000 H10B 2 0.305451 0.226797 0.231924 11.00000 -1.50000 H10C 2 0.392706 0.164243 0.214207 11.00000 -1.50000 AFIX 0 C11 1 0.732922 0.302179 0.198594 11.00000 0.03834 0.12212 = 0.04014 -0.01364 0.00989 0.01077 AFIX 137 H11A 2 0.751220 0.259435 0.223435 11.00000 -1.50000 H11B 2 0.775646 0.349802 0.205504 11.00000 -1.50000 H11C 2 0.745045 0.283305 0.162783 11.00000 -1.50000 AFIX 0 C12 1 0.452354 0.510495 0.221625 11.00000 0.08760 0.03836 = 0.04324 0.00133 0.01586 0.00024 AFIX 137 H12A 2 0.402020 0.523950 0.194178 11.00000 -1.50000 H12B 2 0.513179 0.545289 0.218247 11.00000 -1.50000 H12C 2 0.420941 0.518706 0.256062 11.00000 -1.50000 AFIX 0 C13 1 0.054703 0.427839 0.269645 11.00000 0.03626 0.05515 = 0.02579 -0.00473 0.00109 0.01572 C14 1 0.037262 0.508678 0.280725 11.00000 0.03868 0.04893 = 0.03290 0.01012 0.00423 0.00444 C15 1 -0.058228 0.529077 0.302383 11.00000 0.04375 0.04127 = 0.04214 -0.00031 0.00611 0.01322 AFIX 43 H15 2 -0.072782 0.584114 0.309394 11.00000 -1.20000 AFIX 0 C16 1 -0.132254 0.471708 0.313945 11.00000 0.03155 0.05128 = 0.04242 -0.00775 0.00455 0.00490 C17 1 -0.110433 0.392110 0.303744 11.00000 0.03345 0.04858 = 0.05497 -0.00760 -0.00385 -0.00105 AFIX 43 H17 2 -0.159562 0.352089 0.313015 11.00000 -1.20000 AFIX 0 C18 1 -0.018105 0.368569 0.280151 11.00000 0.03306 0.04987 = 0.04689 -0.01287 -0.01070 0.00784 C19 1 0.117443 0.571757 0.270473 11.00000 0.05558 0.05952 = 0.07560 0.02251 0.02414 0.00862 AFIX 137 H19A 2 0.136531 0.570623 0.233387 11.00000 -1.50000 H19B 2 0.178760 0.561008 0.292065 11.00000 -1.50000 H19C 2 0.089508 0.624920 0.279257 11.00000 -1.50000 AFIX 0 C20 1 -0.235034 0.495734 0.338024 11.00000 0.04062 0.07068 = 0.07746 -0.01986 0.01775 0.00497 AFIX 137 H20A 2 -0.233793 0.483891 0.375618 11.00000 -1.50000 H20B 2 -0.291023 0.465275 0.321248 11.00000 -1.50000 H20C 2 -0.246536 0.553520 0.332726 11.00000 -1.50000 AFIX 0 C21 1 -0.000039 0.281744 0.265733 11.00000 0.04869 0.05428 = 0.09822 -0.04097 -0.02384 0.01228 AFIX 137 H21A 2 -0.030376 0.270932 0.231201 11.00000 -1.50000 H21B 2 -0.032440 0.246763 0.291854 11.00000 -1.50000 H21C 2 0.074454 0.271042 0.264763 11.00000 -1.50000 AFIX 0 C22 1 0.255598 0.286909 0.490851 11.00000 0.03313 0.03715 = 0.01731 -0.00074 0.00564 0.00255 C23 1 0.157626 0.337342 0.556260 11.00000 0.05088 0.04728 = 0.02783 -0.00271 0.01850 0.00889 AFIX 43 H23 2 0.115030 0.373239 0.575500 11.00000 -1.20000 AFIX 0 C24 1 0.188882 0.264633 0.571861 11.00000 0.05011 0.04986 = 0.02360 0.00236 0.01887 0.00045 AFIX 43 H24 2 0.173285 0.238867 0.604088 11.00000 -1.20000 AFIX 0 C25 1 0.181779 0.426837 0.480696 11.00000 0.05396 0.03256 = 0.02511 -0.00400 0.01421 0.01043 C26 1 0.255951 0.486232 0.487376 11.00000 0.06469 0.03851 = 0.03328 -0.01246 0.02048 0.00042 C27 1 0.235167 0.559728 0.462852 11.00000 0.08260 0.03965 = 0.05810 -0.01969 0.03460 -0.00727 AFIX 43 H27 2 0.283280 0.602659 0.466369 11.00000 -1.20000 AFIX 0 C28 1 0.145737 0.571521 0.433424 11.00000 0.07938 0.04228 = 0.05002 -0.00425 0.02445 0.01720 C29 1 0.075648 0.510700 0.428771 11.00000 0.06838 0.04274 = 0.03948 -0.00100 0.01570 0.01646 AFIX 43 H29 2 0.014352 0.519570 0.408943 11.00000 -1.20000 AFIX 0 C30 1 0.090921 0.436807 0.451914 11.00000 0.05557 0.03625 = 0.03333 -0.00518 0.01894 0.01813 C31 1 0.353845 0.471920 0.518915 11.00000 0.05897 0.06545 = 0.05269 -0.02440 0.01671 -0.01675 AFIX 137 H31A 2 0.335789 0.450978 0.553567 11.00000 -1.50000 H31B 2 0.391540 0.522790 0.522863 11.00000 -1.50000 H31C 2 0.397494 0.432740 0.500704 11.00000 -1.50000 AFIX 0 C32 1 0.128264 0.653244 0.408074 11.00000 0.14277 0.03901 = 0.09550 0.01310 0.04958 0.02266 AFIX 137 H32A 2 0.089472 0.646320 0.375320 11.00000 -1.50000 H32B 2 0.195162 0.678399 0.400638 11.00000 -1.50000 H32C 2 0.088889 0.687719 0.431914 11.00000 -1.50000 AFIX 0 C33 1 0.011872 0.371466 0.445696 11.00000 0.04702 0.05725 = 0.04326 -0.01448 0.00525 0.00637 AFIX 137 H33A 2 0.044672 0.323458 0.430845 11.00000 -1.50000 H33B 2 -0.043384 0.389946 0.422206 11.00000 -1.50000 H33C 2 -0.017375 0.358259 0.479971 11.00000 -1.50000 AFIX 0 C34 1 0.297507 0.156730 0.536635 11.00000 0.04386 0.03985 = 0.01536 0.00130 0.00994 0.00606 C35 1 0.398006 0.152859 0.556310 11.00000 0.04113 0.04849 = 0.01424 0.00669 0.00346 -0.00330 C36 1 0.439207 0.076880 0.565395 11.00000 0.03776 0.06246 = 0.02253 0.00995 0.00150 0.00668 AFIX 43 H36 2 0.507100 0.072824 0.579524 11.00000 -1.20000 AFIX 0 C37 1 0.384862 0.006504 0.554597 11.00000 0.05428 0.04596 = 0.02269 0.00732 0.01288 0.00710 C38 1 0.285457 0.013157 0.535508 11.00000 0.04764 0.04074 = 0.02861 0.00666 0.00781 -0.00341 AFIX 43 H38 2 0.247003 -0.034488 0.528664 11.00000 -1.20000 AFIX 0 C39 1 0.239795 0.087414 0.525971 11.00000 0.03943 0.04230 = 0.02620 0.00343 0.00876 -0.00217 C40 1 0.460429 0.227269 0.567816 11.00000 0.05096 0.06280 = 0.02757 0.00379 -0.00507 -0.01349 AFIX 137 H40A 2 0.490103 0.247913 0.535225 11.00000 -1.50000 H40B 2 0.516238 0.213974 0.592433 11.00000 -1.50000 H40C 2 0.415625 0.268410 0.583286 11.00000 -1.50000 AFIX 0 C41 1 0.434981 -0.074209 0.563753 11.00000 0.06547 0.05452 = 0.04085 0.01575 0.01627 0.01985 AFIX 137 H41A 2 0.502317 -0.075614 0.546333 11.00000 -1.50000 H41B 2 0.390628 -0.116805 0.549447 11.00000 -1.50000 H41C 2 0.444611 -0.082727 0.601437 11.00000 -1.50000 AFIX 0 C42 1 0.131207 0.093717 0.504696 11.00000 0.03435 0.05998 = 0.05925 -0.00011 0.00514 -0.00539 AFIX 137 H42A 2 0.088956 0.125724 0.528719 11.00000 -1.50000 H42B 2 0.101487 0.039661 0.501232 11.00000 -1.50000 H42C 2 0.132556 0.119865 0.470299 11.00000 -1.50000 AFIX 0 PART 1 C43 1 0.212579 0.158642 0.326788 21.00000 0.04720 0.03754 = 0.03072 -0.01082 0.00982 -0.00546 AFIX 23 H43A 2 0.164998 0.159028 0.296303 21.00000 -1.20000 H43B 2 0.283955 0.163214 0.313262 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C43A 1 0.218743 0.164941 0.322659 -21.00000 0.04720 0.03754 = 0.03072 -0.01082 0.00982 -0.00546 AFIX 23 H43C 2 0.181325 0.170914 0.288969 -21.00000 -1.20000 H43D 2 0.293987 0.164602 0.315697 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C44 1 0.202151 0.080725 0.354115 21.00000 0.02953 0.03093 = 0.03828 -0.01401 0.00382 -0.00326 PART 0 PART 2 AFIX 66 C44A 1 0.187342 0.090279 0.349348 -21.00000 0.02953 0.03093 = 0.03828 -0.01401 0.00382 -0.00326 C45A 1 0.083176 0.070676 0.353333 -21.00000 0.04019 0.04987 = 0.06400 0.01830 -0.01982 -0.01320 AFIX 43 H45A 2 0.032081 0.106502 0.340089 -21.00000 -1.20000 AFIX 65 C46A 1 0.053770 -0.001346 0.376695 -21.00000 0.06537 0.06226 = 0.08103 0.03669 -0.03824 -0.03661 AFIX 43 H46A 2 -0.017423 -0.014744 0.379419 -21.00000 -1.20000 AFIX 65 C47A 1 0.128529 -0.053766 0.396073 -21.00000 0.06705 0.03531 = 0.05342 -0.00030 -0.00514 -0.00980 C48A 1 0.232695 -0.034164 0.392089 -21.00000 0.04072 0.04522 = 0.04733 -0.00818 -0.00491 0.01683 AFIX 43 H48A 2 0.283790 -0.069991 0.405332 -21.00000 -1.20000 AFIX 65 C49A 1 0.262103 0.037858 0.368727 -21.00000 0.03287 0.03545 = 0.04344 -0.01550 0.00389 -0.00279 AFIX 43 H49A 2 0.333296 0.051255 0.366003 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C45 1 0.106962 0.040649 0.357617 21.00000 0.04019 0.04987 = 0.06400 0.01830 -0.01982 -0.01320 AFIX 43 H45 2 0.048445 0.063121 0.340373 21.00000 -1.20000 AFIX 0 C46 1 0.095342 -0.029203 0.384793 21.00000 0.06537 0.06226 = 0.08103 0.03669 -0.03824 -0.03661 AFIX 43 H46 2 0.030027 -0.055345 0.385730 21.00000 -1.20000 AFIX 0 C47 1 0.177624 -0.061379 0.410582 21.00000 0.06705 0.03531 = 0.05342 -0.00030 -0.00514 -0.00980 C48 1 0.272669 -0.026825 0.407684 21.00000 0.04072 0.04522 = 0.04733 -0.00818 -0.00491 0.01683 AFIX 43 H48 2 0.330394 -0.051465 0.424346 21.00000 -1.20000 AFIX 0 C49 1 0.284901 0.044498 0.380311 21.00000 0.03287 0.03545 = 0.04344 -0.01550 0.00389 -0.00279 AFIX 43 H49 2 0.351059 0.069316 0.379339 21.00000 -1.20000 AFIX 0 PART 0 C50 1 0.538987 0.327343 0.345952 11.00000 0.02938 0.03341 = 0.02471 0.00278 0.00444 -0.00112 AFIX 23 H50A 2 0.555275 0.350275 0.311168 11.00000 -1.20000 H50B 2 0.525970 0.372798 0.370138 11.00000 -1.20000 AFIX 0 C51 1 0.631091 0.280645 0.365428 11.00000 0.02418 0.03679 = 0.02997 0.00383 0.00758 -0.00380 C52 1 0.677946 0.301071 0.412983 11.00000 0.04355 0.04111 = 0.04254 -0.00018 -0.00369 -0.00633 AFIX 43 H52 2 0.650135 0.343537 0.433497 11.00000 -1.20000 AFIX 0 C53 1 0.764566 0.259960 0.430476 11.00000 0.04605 0.05662 = 0.06691 0.00931 -0.01930 -0.01215 AFIX 43 H53 2 0.796827 0.274239 0.462663 11.00000 -1.20000 AFIX 0 C54 1 0.803239 0.198106 0.400547 11.00000 0.02932 0.06220 = 0.07865 0.02899 -0.00263 0.00226 C55 1 0.756551 0.175492 0.354368 11.00000 0.04515 0.05478 = 0.06179 0.00204 0.02458 0.01083 AFIX 43 H55 2 0.783271 0.131802 0.334577 11.00000 -1.20000 AFIX 0 C56 1 0.670487 0.216929 0.337082 11.00000 0.03966 0.05041 = 0.03276 0.00031 0.01231 0.00443 AFIX 43 H56 2 0.637866 0.201414 0.305233 11.00000 -1.20000 AFIX 0 PART 1 CL1 3 0.161158 -0.149518 0.446705 21.00000 0.14361 0.03912 = 0.08141 0.01273 -0.01405 -0.02092 PART 0 PART 2 CL1A 3 0.092437 -0.145380 0.415028 -21.00000 0.18092 0.04228 = 0.21526 0.01486 0.13030 0.00104 PART 0 CL2 3 0.914031 0.146767 0.420326 11.00000 0.03419 0.09410 = 0.16903 0.05310 -0.01211 0.00945 IR1 4 0.279728 0.364127 0.335246 11.00000 0.03009 0.02852 = 0.01748 -0.00153 0.00447 0.00266 AFIX 3 1.6500 H 2 0.358988 0.439517 0.322706 11.00000 0.06807 HA 2 0.183988 0.428027 0.344966 11.00000 0.04671 AFIX 0 IR2 4 0.335468 0.273001 0.422939 11.00000 0.03040 0.02897 = 0.01741 -0.00064 0.00703 0.00272 AFIX 3 1.6500 HB 2 0.439088 0.324491 0.440569 11.00000 0.09803 HC 2 0.389488 0.193161 0.450159 11.00000 0.07875 AFIX 0 N1 5 0.304491 0.382328 0.217916 11.00000 0.04021 0.04721 = 0.01853 -0.00079 0.00481 0.00947 N2 5 0.148074 0.408439 0.241399 11.00000 0.03936 0.07479 = 0.02295 -0.00362 -0.00103 0.02009 N3 5 0.198341 0.351234 0.506976 11.00000 0.04032 0.03862 = 0.02308 -0.00422 0.01174 0.00491 N4 5 0.249067 0.234072 0.531328 11.00000 0.03899 0.03722 = 0.02090 -0.00014 0.01011 0.00322 S1 7 0.184912 0.247862 0.367885 11.00000 0.03171 0.03489 = 0.02707 -0.00666 0.00808 -0.00260 S2 7 0.421708 0.266898 0.340482 11.00000 0.02850 0.03184 = 0.01823 -0.00048 0.00745 0.00083 C57 1 0.454492 0.566451 0.377320 11.00000 0.08655 0.05630 = 0.06657 0.00073 -0.00555 -0.03285 AFIX 137 H57A 2 0.501637 0.540637 0.352511 11.00000 -1.50000 H57B 2 0.441631 0.529931 0.406730 11.00000 -1.50000 H57C 2 0.485733 0.616383 0.390393 11.00000 -1.50000 AFIX 0 O1 6 0.359755 0.584381 0.351766 11.00000 0.08331 0.04323 = 0.05829 0.00117 0.00625 -0.00821 AFIX 147 H1 2 0.331515 0.541376 0.341897 11.00000 -1.50000 AFIX 0 HKLF 4 REM sbd1906_a.res in P2(1)/c REM wR2 = 0.0712, GooF = S = 1.036, Restrained GooF = 1.036 for all data REM R1 = 0.0299 for 8700 Fo > 4sig(Fo) and 0.0357 for all 9782 data REM 650 parameters refined using 4 restraints END WGHT 0.0265 13.0995 REM Highest difference peak 1.916, deepest hole -1.357, 1-sigma level 0.098 Q1 1 0.3600 0.3174 0.4332 11.00000 0.05 1.92 Q2 1 0.2899 0.4179 0.3409 11.00000 0.05 1.55 Q3 1 0.9024 0.1395 0.4582 11.00000 0.05 0.93 Q4 1 0.3316 0.1970 0.4216 11.00000 0.05 0.73 Q5 1 0.3806 0.4921 0.3379 11.00000 0.05 0.68 Q6 1 0.2851 0.3795 0.4049 11.00000 0.05 0.67 Q7 1 0.9076 0.1032 0.4005 11.00000 0.05 0.58 Q8 1 0.2170 0.3014 0.3545 11.00000 0.05 0.56 Q9 1 0.2324 -0.1481 0.4396 11.00000 0.05 0.54 Q10 1 0.3346 0.3791 0.4013 11.00000 0.05 0.52 Q11 1 0.2996 0.3012 0.3394 11.00000 0.05 0.44 Q12 1 0.3361 0.4455 0.4201 11.00000 0.05 0.43 Q13 1 0.1346 0.0464 0.3175 11.00000 0.05 0.43 Q14 1 0.3280 0.1496 0.4353 11.00000 0.05 0.41 Q15 1 0.2593 0.3181 0.4253 11.00000 0.05 0.41 Q16 1 0.2580 0.2179 0.4260 11.00000 0.05 0.41 Q17 1 0.4581 0.3041 0.3542 11.00000 0.05 0.38 Q18 1 0.4216 0.2366 0.4210 11.00000 0.05 0.38 Q19 1 0.2745 0.1788 0.3255 11.00000 0.05 0.38 Q20 1 0.9277 0.1687 0.4216 11.00000 0.05 0.37 Q21 1 0.2807 0.3789 0.2397 11.00000 0.05 0.37 Q22 1 0.3076 0.5782 0.4751 11.00000 0.05 0.37 Q23 1 0.2076 0.5933 0.4381 11.00000 0.05 0.37 Q24 1 0.3902 0.1825 0.5178 11.00000 0.05 0.37 Q25 1 0.2094 0.6774 0.4124 11.00000 0.05 0.35 Q26 1 0.2075 0.3545 0.4053 11.00000 0.05 0.35 Q27 1 0.1403 0.3318 0.2764 11.00000 0.05 0.35 Q28 1 0.2253 0.4548 0.2456 11.00000 0.05 0.34 Q29 1 0.4140 0.2383 0.4565 11.00000 0.05 0.34 Q30 1 0.2368 0.3169 0.2982 11.00000 0.05 0.33 Q31 1 0.2618 0.1594 0.4044 11.00000 0.05 0.33 Q32 1 0.1529 0.3616 0.1921 11.00000 0.05 0.32 Q33 1 0.3202 0.7168 0.4168 11.00000 0.05 0.32 Q34 1 0.4437 0.5570 0.2006 11.00000 0.05 0.31 Q35 1 0.1184 -0.0169 0.3541 11.00000 0.05 0.31 Q36 1 0.1035 -0.0342 0.3261 11.00000 0.05 0.31 Q37 1 0.1333 0.3478 0.3780 11.00000 0.05 0.30 Q38 1 0.2645 0.2675 0.3975 11.00000 0.05 0.30 Q39 1 0.2631 0.3399 0.4984 11.00000 0.05 0.30 Q40 1 0.0623 0.1981 0.3374 11.00000 0.05 0.30 ; _shelx_res_checksum 89407 _olex2_date_sample_data_collection 2019-09-20 _olex2_date_sample_submission 2019-09-19 _olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount' _olex2_submission_original_sample_id 'BT Ma1' _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 1.277 _oxdiff_exptl_absorpt_empirical_full_min 0.810 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C0AA C 0.2422(4) 0.3839(3) 0.26156(17) 0.0310(10) Uani 1 1 d . . . . C2 C 0.2507(5) 0.4054(4) 0.17344(19) 0.0579(18) Uani 1 1 d . . . . H2 H 0.277677 0.408767 0.138962 0.070 Uiso 1 1 calc R . . . C3 C 0.1544(5) 0.4221(5) 0.1878(2) 0.068(2) Uani 1 1 d . . . . H3 H 0.100011 0.440039 0.165607 0.082 Uiso 1 1 calc R . . . C4 C 0.4124(4) 0.3623(3) 0.21638(16) 0.0304(10) Uani 1 1 d . . . . C5 C 0.4406(4) 0.2822(3) 0.20970(15) 0.0298(10) Uani 1 1 d . . . . C6 C 0.5454(4) 0.2640(3) 0.20476(17) 0.0372(11) Uani 1 1 d . . . . H6 H 0.566074 0.209398 0.201231 0.045 Uiso 1 1 calc R . . . C7 C 0.6198(4) 0.3238(4) 0.20487(17) 0.0409(12) Uani 1 1 d . . . . C8 C 0.5885(4) 0.4033(4) 0.21075(18) 0.0431(13) Uani 1 1 d . . . . H8 H 0.639251 0.444629 0.211150 0.052 Uiso 1 1 calc R . . . C9 C 0.4843(4) 0.4242(3) 0.21610(17) 0.0388(12) Uani 1 1 d . . . . C10 C 0.3602(4) 0.2163(3) 0.20645(19) 0.0425(12) Uani 1 1 d . . . . H10A H 0.330470 0.214991 0.171092 0.064 Uiso 1 1 calc GR . . . H10B H 0.305451 0.226797 0.231924 0.064 Uiso 1 1 calc GR . . . H10C H 0.392706 0.164243 0.214207 0.064 Uiso 1 1 calc GR . . . C11 C 0.7329(4) 0.3022(5) 0.1986(2) 0.067(2) Uani 1 1 d . . . . H11A H 0.751220 0.259435 0.223435 0.100 Uiso 1 1 calc GR . . . H11B H 0.775646 0.349802 0.205504 0.100 Uiso 1 1 calc GR . . . H11C H 0.745045 0.283305 0.162783 0.100 Uiso 1 1 calc GR . . . C12 C 0.4524(5) 0.5105(3) 0.2216(2) 0.0564(16) Uani 1 1 d . . . . H12A H 0.402020 0.523950 0.194178 0.085 Uiso 1 1 calc GR . . . H12B H 0.513179 0.545289 0.218247 0.085 Uiso 1 1 calc GR . . . H12C H 0.420941 0.518706 0.256062 0.085 Uiso 1 1 calc GR . . . C13 C 0.0547(4) 0.4278(3) 0.26964(18) 0.0391(12) Uani 1 1 d . . . . C14 C 0.0373(4) 0.5087(3) 0.28073(19) 0.0402(12) Uani 1 1 d . . . . C15 C -0.0582(4) 0.5291(3) 0.3024(2) 0.0424(12) Uani 1 1 d . . . . H15 H -0.072782 0.584114 0.309394 0.051 Uiso 1 1 calc R . . . C16 C -0.1323(4) 0.4717(3) 0.3139(2) 0.0417(12) Uani 1 1 d . . . . C17 C -0.1104(4) 0.3921(3) 0.3037(2) 0.0457(13) Uani 1 1 d . . . . H17 H -0.159562 0.352089 0.313015 0.055 Uiso 1 1 calc R . . . C18 C -0.0181(4) 0.3686(3) 0.2802(2) 0.0433(13) Uani 1 1 d . . . . C19 C 0.1174(5) 0.5718(4) 0.2705(3) 0.0635(18) Uani 1 1 d . . . . H19A H 0.136531 0.570623 0.233387 0.095 Uiso 1 1 calc GR . . . H19B H 0.178760 0.561008 0.292065 0.095 Uiso 1 1 calc GR . . . H19C H 0.089508 0.624920 0.279257 0.095 Uiso 1 1 calc GR . . . C20 C -0.2350(4) 0.4957(4) 0.3380(3) 0.0629(17) Uani 1 1 d . . . . H20A H -0.233793 0.483891 0.375618 0.094 Uiso 1 1 calc GR . . . H20B H -0.291023 0.465275 0.321248 0.094 Uiso 1 1 calc GR . . . H20C H -0.246536 0.553520 0.332726 0.094 Uiso 1 1 calc GR . . . C21 C 0.0000(5) 0.2817(4) 0.2657(3) 0.067(2) Uani 1 1 d . . . . H21A H -0.030376 0.270932 0.231201 0.101 Uiso 1 1 calc GR . . . H21B H -0.032440 0.246763 0.291854 0.101 Uiso 1 1 calc GR . . . H21C H 0.074454 0.271042 0.264763 0.101 Uiso 1 1 calc GR . . . C22 C 0.2556(3) 0.2869(3) 0.49085(16) 0.0292(10) Uani 1 1 d . . . . C23 C 0.1576(4) 0.3373(3) 0.55626(19) 0.0419(12) Uani 1 1 d . . . . H23 H 0.115030 0.373239 0.575500 0.050 Uiso 1 1 calc R . . . C24 C 0.1889(4) 0.2646(3) 0.57186(18) 0.0411(12) Uani 1 1 d . . . . H24 H 0.173285 0.238867 0.604088 0.049 Uiso 1 1 calc R . . . C25 C 0.1818(4) 0.4268(3) 0.48070(18) 0.0372(11) Uani 1 1 d . . . . C26 C 0.2560(5) 0.4862(3) 0.4874(2) 0.0454(13) Uani 1 1 d . . . . C27 C 0.2352(5) 0.5597(4) 0.4629(2) 0.0600(18) Uani 1 1 d . . . . H27 H 0.283280 0.602659 0.466369 0.072 Uiso 1 1 calc R . . . C28 C 0.1457(6) 0.5715(4) 0.4334(2) 0.0572(16) Uani 1 1 d . . . . C29 C 0.0756(5) 0.5107(3) 0.4288(2) 0.0502(14) Uani 1 1 d . . . . H29 H 0.014352 0.519570 0.408943 0.060 Uiso 1 1 calc R . . . C30 C 0.0909(4) 0.4368(3) 0.45191(19) 0.0417(12) Uani 1 1 d . . . . C31 C 0.3538(5) 0.4719(4) 0.5189(2) 0.0590(17) Uani 1 1 d . . . . H31A H 0.335789 0.450978 0.553567 0.088 Uiso 1 1 calc GR . . . H31B H 0.391540 0.522790 0.522863 0.088 Uiso 1 1 calc GR . . . H31C H 0.397494 0.432740 0.500704 0.088 Uiso 1 1 calc GR . . . C32 C 0.1283(7) 0.6532(4) 0.4081(3) 0.092(3) Uani 1 1 d . . . . H32A H 0.089472 0.646320 0.375320 0.138 Uiso 1 1 calc GR . . . H32B H 0.195162 0.678399 0.400638 0.138 Uiso 1 1 calc GR . . . H32C H 0.088889 0.687719 0.431914 0.138 Uiso 1 1 calc GR . . . C33 C 0.0119(4) 0.3715(4) 0.4457(2) 0.0492(14) Uani 1 1 d . . . . H33A H 0.044672 0.323458 0.430845 0.074 Uiso 1 1 calc GR . . . H33B H -0.043384 0.389946 0.422206 0.074 Uiso 1 1 calc GR . . . H33C H -0.017375 0.358259 0.479971 0.074 Uiso 1 1 calc GR . . . C34 C 0.2975(4) 0.1567(3) 0.53664(16) 0.0330(10) Uani 1 1 d . . . . C35 C 0.3980(4) 0.1529(3) 0.55631(16) 0.0346(11) Uani 1 1 d . . . . C36 C 0.4392(4) 0.0769(3) 0.56540(18) 0.0409(12) Uani 1 1 d . . . . H36 H 0.507100 0.072824 0.579524 0.049 Uiso 1 1 calc R . . . C37 C 0.3849(4) 0.0065(3) 0.55460(18) 0.0409(12) Uani 1 1 d . . . . C38 C 0.2855(4) 0.0132(3) 0.53551(18) 0.0390(11) Uani 1 1 d . . . . H38 H 0.247003 -0.034488 0.528664 0.047 Uiso 1 1 calc R . . . C39 C 0.2398(4) 0.0874(3) 0.52597(18) 0.0359(11) Uani 1 1 d . . . . C40 C 0.4604(4) 0.2273(4) 0.5678(2) 0.0471(13) Uani 1 1 d . . . . H40A H 0.490103 0.247913 0.535225 0.071 Uiso 1 1 calc GR . . . H40B H 0.516238 0.213974 0.592433 0.071 Uiso 1 1 calc GR . . . H40C H 0.415625 0.268410 0.583286 0.071 Uiso 1 1 calc GR . . . C41 C 0.4350(5) -0.0742(4) 0.5638(2) 0.0536(15) Uani 1 1 d . . . . H41A H 0.502317 -0.075614 0.546333 0.080 Uiso 1 1 calc GR . . . H41B H 0.390628 -0.116805 0.549447 0.080 Uiso 1 1 calc GR . . . H41C H 0.444611 -0.082727 0.601437 0.080 Uiso 1 1 calc GR . . . C42 C 0.1312(4) 0.0937(4) 0.5047(2) 0.0512(14) Uani 1 1 d . . . . H42A H 0.088956 0.125724 0.528719 0.077 Uiso 1 1 calc GR . . . H42B H 0.101487 0.039661 0.501232 0.077 Uiso 1 1 calc GR . . . H42C H 0.132556 0.119865 0.470299 0.077 Uiso 1 1 calc GR . . . C43 C 0.2126(10) 0.1586(4) 0.3268(4) 0.0385(13) Uani 0.802(10) 1 d D P A 1 H43A H 0.164998 0.159028 0.296303 0.046 Uiso 0.802(10) 1 calc R P A 1 H43B H 0.283955 0.163214 0.313262 0.046 Uiso 0.802(10) 1 calc R P A 1 C43A C 0.219(4) 0.1649(13) 0.3227(13) 0.0385(13) Uani 0.198(10) 1 d D P A 2 H43C H 0.181325 0.170914 0.288969 0.046 Uiso 0.198(10) 1 calc R P A 2 H43D H 0.293987 0.164602 0.315697 0.046 Uiso 0.198(10) 1 calc R P A 2 C44 C 0.2022(6) 0.0807(5) 0.3541(4) 0.0329(15) Uani 0.802(10) 1 d D P A 1 C44A C 0.187(2) 0.0903(17) 0.3493(15) 0.0329(15) Uani 0.198(10) 1 d D P A 2 C45A C 0.083(2) 0.0707(16) 0.3533(14) 0.051(2) Uani 0.198(10) 1 d DG P A 2 H45A H 0.032081 0.106502 0.340089 0.062 Uiso 0.198(10) 1 calc R P A 2 C46A C 0.0538(16) -0.0013(15) 0.3767(11) 0.070(3) Uani 0.198(10) 1 d DG P A 2 H46A H -0.017423 -0.014744 0.379419 0.084 Uiso 0.198(10) 1 calc R P A 2 C47A C 0.1285(17) -0.0538(13) 0.3961(11) 0.052(2) Uani 0.198(10) 1 d G P A 2 C48A C 0.2327(16) -0.0342(15) 0.3921(11) 0.0444(17) Uani 0.198(10) 1 d DG P A 2 H48A H 0.283790 -0.069991 0.405332 0.053 Uiso 0.198(10) 1 calc R P A 2 C49A C 0.2621(17) 0.0379(17) 0.3687(13) 0.0372(17) Uani 0.198(10) 1 d DG P A 2 H49A H 0.333296 0.051255 0.366003 0.045 Uiso 0.198(10) 1 calc R P A 2 C45 C 0.1070(6) 0.0406(5) 0.3576(4) 0.051(2) Uani 0.802(10) 1 d . P A 1 H45 H 0.048445 0.063121 0.340373 0.062 Uiso 0.802(10) 1 calc R P A 1 C46 C 0.0953(7) -0.0292(6) 0.3848(4) 0.070(3) Uani 0.802(10) 1 d . P A 1 H46 H 0.030027 -0.055345 0.385730 0.084 Uiso 0.802(10) 1 calc R P A 1 C47 C 0.1776(7) -0.0614(4) 0.4106(3) 0.052(2) Uani 0.802(10) 1 d . P A 1 C48 C 0.2727(6) -0.0268(4) 0.4077(3) 0.0444(17) Uani 0.802(10) 1 d . P A 1 H48 H 0.330394 -0.051465 0.424346 0.053 Uiso 0.802(10) 1 calc R P A 1 C49 C 0.2849(6) 0.0445(5) 0.3803(3) 0.0372(17) Uani 0.802(10) 1 d . P A 1 H49 H 0.351059 0.069316 0.379339 0.045 Uiso 0.802(10) 1 calc R P A 1 C50 C 0.5390(3) 0.3273(3) 0.34595(17) 0.0292(9) Uani 1 1 d . . . . H50A H 0.555275 0.350275 0.311168 0.035 Uiso 1 1 calc R . . . H50B H 0.525970 0.372798 0.370138 0.035 Uiso 1 1 calc R . . . C51 C 0.6311(3) 0.2806(3) 0.36543(17) 0.0303(10) Uani 1 1 d . . . . C52 C 0.6779(4) 0.3011(3) 0.4130(2) 0.0424(12) Uani 1 1 d . . . . H52 H 0.650135 0.343537 0.433497 0.051 Uiso 1 1 calc R . . . C53 C 0.7646(5) 0.2600(4) 0.4305(3) 0.0566(16) Uani 1 1 d . . . . H53 H 0.796827 0.274239 0.462663 0.068 Uiso 1 1 calc R . . . C54 C 0.8032(4) 0.1981(4) 0.4005(3) 0.0567(16) Uani 1 1 d . . . . C55 C 0.7566(4) 0.1755(4) 0.3544(2) 0.0538(15) Uani 1 1 d . . . . H55 H 0.783271 0.131802 0.334577 0.065 Uiso 1 1 calc R . . . C56 C 0.6705(4) 0.2169(3) 0.3371(2) 0.0409(12) Uani 1 1 d . . . . H56 H 0.637866 0.201414 0.305233 0.049 Uiso 1 1 calc R . . . Cl1 Cl 0.1612(4) -0.14952(16) 0.44671(12) 0.0881(11) Uani 0.802(10) 1 d . P A 1 Cl1A Cl 0.092(2) -0.1454(7) 0.4150(12) 0.146(14) Uani 0.198(10) 1 d D P A 2 Cl2 Cl 0.91403(12) 0.14677(13) 0.42033(11) 0.0991(8) Uani 1 1 d . . . . Ir1 Ir 0.27973(2) 0.36413(2) 0.33525(2) 0.02535(6) Uani 1 1 d . . . . H H 0.358988 0.439517 0.322706 0.068(19) Uiso 1 1 d R . . . HA H 0.183988 0.428027 0.344966 0.047(15) Uiso 1 1 d R . . . Ir2 Ir 0.33547(2) 0.27300(2) 0.42294(2) 0.02557(6) Uani 1 1 d . . . . HB H 0.439088 0.324491 0.440569 0.10(2) Uiso 1 1 d R . . . HC H 0.389488 0.193161 0.450159 0.08(2) Uiso 1 1 d R . . . N1 N 0.3045(3) 0.3823(3) 0.21792(14) 0.0353(9) Uani 1 1 d . . . . N2 N 0.1481(3) 0.4084(3) 0.24140(15) 0.0457(11) Uani 1 1 d . . . . N3 N 0.1983(3) 0.3512(2) 0.50698(14) 0.0340(9) Uani 1 1 d . . . . N4 N 0.2491(3) 0.2341(2) 0.53133(14) 0.0323(9) Uani 1 1 d . . . . S1 S 0.18491(9) 0.24786(7) 0.36789(4) 0.0312(2) Uani 1 1 d D . . . S2 S 0.42171(8) 0.26690(6) 0.34048(4) 0.0262(2) Uani 1 1 d . . . . C57 C 0.4545(6) 0.5665(4) 0.3773(3) 0.070(2) Uani 1 1 d . . . . H57A H 0.501637 0.540637 0.352511 0.105 Uiso 1 1 calc GR . . . H57B H 0.441631 0.529931 0.406730 0.105 Uiso 1 1 calc GR . . . H57C H 0.485733 0.616383 0.390393 0.105 Uiso 1 1 calc GR . . . O1 O 0.3598(4) 0.5844(2) 0.35177(17) 0.0616(11) Uani 1 1 d . . . . H1 H 0.331515 0.541376 0.341897 0.092 Uiso 1 1 calc GR . . . 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 C0AA 0.038(3) 0.032(2) 0.023(2) -0.0036(18) 0.0038(18) 0.007(2) C2 0.061(4) 0.097(5) 0.015(2) 0.003(3) -0.001(2) 0.036(4) C3 0.058(4) 0.126(6) 0.020(2) 0.001(3) -0.004(2) 0.045(4) C4 0.035(2) 0.042(3) 0.0139(19) 0.0009(18) 0.0048(17) 0.003(2) C5 0.038(2) 0.039(3) 0.0124(19) -0.0034(18) 0.0025(17) 0.004(2) C6 0.046(3) 0.049(3) 0.017(2) -0.006(2) 0.0022(19) 0.016(2) C7 0.032(3) 0.072(4) 0.018(2) -0.004(2) 0.0042(18) 0.004(3) C8 0.050(3) 0.058(3) 0.022(2) 0.002(2) 0.009(2) -0.015(3) C9 0.054(3) 0.045(3) 0.018(2) 0.005(2) 0.010(2) 0.000(2) C10 0.050(3) 0.047(3) 0.030(3) -0.010(2) 0.002(2) -0.005(2) C11 0.038(3) 0.122(6) 0.040(3) -0.014(4) 0.010(2) 0.011(4) C12 0.088(5) 0.038(3) 0.043(3) 0.001(3) 0.016(3) 0.000(3) C13 0.036(3) 0.055(3) 0.026(2) -0.005(2) 0.0011(19) 0.016(2) C14 0.039(3) 0.049(3) 0.033(3) 0.010(2) 0.004(2) 0.004(2) C15 0.044(3) 0.041(3) 0.042(3) 0.000(2) 0.006(2) 0.013(2) C16 0.032(3) 0.051(3) 0.042(3) -0.008(2) 0.005(2) 0.005(2) C17 0.033(3) 0.049(3) 0.055(3) -0.008(3) -0.004(2) -0.001(2) C18 0.033(3) 0.050(3) 0.047(3) -0.013(3) -0.011(2) 0.008(2) C19 0.056(4) 0.060(4) 0.076(4) 0.023(3) 0.024(3) 0.009(3) C20 0.041(3) 0.071(4) 0.077(4) -0.020(4) 0.018(3) 0.005(3) C21 0.049(3) 0.054(4) 0.098(5) -0.041(4) -0.024(3) 0.012(3) C22 0.033(2) 0.037(3) 0.017(2) -0.0007(18) 0.0056(17) 0.0025(19) C23 0.051(3) 0.047(3) 0.028(2) -0.003(2) 0.018(2) 0.009(2) C24 0.050(3) 0.050(3) 0.024(2) 0.002(2) 0.019(2) 0.000(2) C25 0.054(3) 0.033(3) 0.025(2) -0.0040(19) 0.014(2) 0.010(2) C26 0.065(4) 0.039(3) 0.033(3) -0.012(2) 0.020(2) 0.000(3) C27 0.083(5) 0.040(3) 0.058(4) -0.020(3) 0.035(3) -0.007(3) C28 0.079(4) 0.042(3) 0.050(3) -0.004(3) 0.024(3) 0.017(3) C29 0.068(4) 0.043(3) 0.039(3) -0.001(2) 0.016(3) 0.016(3) C30 0.056(3) 0.036(3) 0.033(3) -0.005(2) 0.019(2) 0.018(2) C31 0.059(4) 0.065(4) 0.053(4) -0.024(3) 0.017(3) -0.017(3) C32 0.143(8) 0.039(4) 0.096(6) 0.013(4) 0.050(5) 0.023(4) C33 0.047(3) 0.057(4) 0.043(3) -0.014(3) 0.005(2) 0.006(3) C34 0.044(3) 0.040(3) 0.015(2) 0.0013(18) 0.0099(18) 0.006(2) C35 0.041(3) 0.048(3) 0.014(2) 0.0067(19) 0.0035(18) -0.003(2) C36 0.038(3) 0.062(4) 0.023(2) 0.010(2) 0.0015(19) 0.007(2) C37 0.054(3) 0.046(3) 0.023(2) 0.007(2) 0.013(2) 0.007(3) C38 0.048(3) 0.041(3) 0.029(2) 0.007(2) 0.008(2) -0.003(2) C39 0.039(3) 0.042(3) 0.026(2) 0.003(2) 0.0088(19) -0.002(2) C40 0.051(3) 0.063(4) 0.028(3) 0.004(2) -0.005(2) -0.013(3) C41 0.065(4) 0.055(4) 0.041(3) 0.016(3) 0.016(3) 0.020(3) C42 0.034(3) 0.060(4) 0.059(4) 0.000(3) 0.005(2) -0.005(3) C43 0.047(3) 0.038(3) 0.031(3) -0.011(2) 0.010(2) -0.005(2) C43A 0.047(3) 0.038(3) 0.031(3) -0.011(2) 0.010(2) -0.005(2) C44 0.030(3) 0.031(3) 0.038(3) -0.014(2) 0.004(3) -0.003(3) C44A 0.030(3) 0.031(3) 0.038(3) -0.014(2) 0.004(3) -0.003(3) C45A 0.040(4) 0.050(5) 0.064(4) 0.018(4) -0.020(3) -0.013(4) C46A 0.065(6) 0.062(6) 0.081(6) 0.037(5) -0.038(5) -0.037(5) C47A 0.067(6) 0.035(4) 0.053(5) 0.000(3) -0.005(4) -0.010(4) C48A 0.041(4) 0.045(4) 0.047(4) -0.008(3) -0.005(3) 0.017(3) C49A 0.033(4) 0.035(3) 0.043(5) -0.015(3) 0.004(3) -0.003(3) C45 0.040(4) 0.050(5) 0.064(4) 0.018(4) -0.020(3) -0.013(4) C46 0.065(6) 0.062(6) 0.081(6) 0.037(5) -0.038(5) -0.037(5) C47 0.067(6) 0.035(4) 0.053(5) 0.000(3) -0.005(4) -0.010(4) C48 0.041(4) 0.045(4) 0.047(4) -0.008(3) -0.005(3) 0.017(3) C49 0.033(4) 0.035(3) 0.043(5) -0.015(3) 0.004(3) -0.003(3) C50 0.029(2) 0.033(2) 0.025(2) 0.0028(19) 0.0044(17) -0.0011(19) C51 0.024(2) 0.037(3) 0.030(2) 0.0038(19) 0.0076(18) -0.0038(19) C52 0.044(3) 0.041(3) 0.043(3) 0.000(2) -0.004(2) -0.006(2) C53 0.046(3) 0.057(4) 0.067(4) 0.009(3) -0.019(3) -0.012(3) C54 0.029(3) 0.062(4) 0.079(4) 0.029(3) -0.003(3) 0.002(3) C55 0.045(3) 0.055(4) 0.062(4) 0.002(3) 0.025(3) 0.011(3) C56 0.040(3) 0.050(3) 0.033(3) 0.000(2) 0.012(2) 0.004(2) Cl1 0.144(3) 0.0391(12) 0.0814(18) 0.0127(11) -0.0141(18) -0.0209(14) Cl1A 0.18(2) 0.042(6) 0.22(3) 0.015(9) 0.13(2) 0.001(8) Cl2 0.0342(8) 0.0941(14) 0.169(2) 0.0531(15) -0.0121(10) 0.0094(8) Ir1 0.03009(10) 0.02852(10) 0.01748(9) -0.00153(7) 0.00447(7) 0.00266(7) Ir2 0.03040(10) 0.02897(10) 0.01741(9) -0.00064(7) 0.00703(7) 0.00272(7) N1 0.040(2) 0.047(2) 0.0185(18) -0.0008(17) 0.0048(16) 0.0095(19) N2 0.039(2) 0.075(3) 0.023(2) -0.004(2) -0.0010(17) 0.020(2) N3 0.040(2) 0.039(2) 0.0231(19) -0.0042(16) 0.0117(16) 0.0049(18) N4 0.039(2) 0.037(2) 0.0209(18) -0.0001(16) 0.0101(16) 0.0032(17) S1 0.0317(6) 0.0349(6) 0.0271(5) -0.0067(5) 0.0081(4) -0.0026(5) S2 0.0285(5) 0.0318(6) 0.0182(5) -0.0005(4) 0.0075(4) 0.0008(4) C57 0.087(5) 0.056(4) 0.067(4) 0.001(3) -0.006(4) -0.033(4) O1 0.083(3) 0.043(2) 0.058(3) 0.001(2) 0.006(2) -0.008(2) 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 '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' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0444 -1 1 2 0.0518 1 1 -5 0.0332 -1 -1 0 0.0661 -2 -1 -2 0.0572 -1 0 -2 0.0535 0 1 -2 0.0254 2 1 -1 0.0654 -1 0 1 0.0657 1 -2 -1 0.0426 2 -2 -1 0.0549 -1 2 1 0.0476 0 2 1 0.0427 0 -2 -1 0.0355 1 1 2 0.0587 0 0 1 0.0395 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 C0AA Ir1 128.8(3) N1 C0AA N2 102.8(4) N2 C0AA Ir1 128.2(3) C3 C2 N1 107.4(4) C2 C3 N2 107.4(5) C5 C4 N1 118.7(4) C9 C4 C5 122.3(4) C9 C4 N1 118.7(4) C4 C5 C6 118.2(4) C4 C5 C10 121.3(4) C6 C5 C10 120.5(4) C7 C6 C5 121.4(5) C6 C7 C8 118.6(5) C6 C7 C11 120.1(6) C8 C7 C11 121.3(6) C7 C8 C9 121.9(5) C4 C9 C8 117.5(5) C4 C9 C12 121.6(5) C8 C9 C12 120.9(5) C14 C13 N2 117.0(5) C18 C13 C14 122.3(5) C18 C13 N2 120.5(5) C13 C14 C15 117.3(5) C13 C14 C19 121.8(5) C15 C14 C19 120.9(5) C16 C15 C14 122.1(5) C15 C16 C20 120.9(5) C17 C16 C15 118.5(5) C17 C16 C20 120.6(5) C16 C17 C18 121.8(5) C13 C18 C17 117.8(5) C13 C18 C21 121.6(5) C17 C18 C21 120.5(5) N3 C22 Ir2 128.6(3) N4 C22 Ir2 127.5(3) N4 C22 N3 103.9(3) C24 C23 N3 107.8(4) C23 C24 N4 106.1(4) C26 C25 C30 124.2(5) C26 C25 N3 117.5(5) C30 C25 N3 118.2(5) C25 C26 C27 115.8(6) C25 C26 C31 122.0(5) C27 C26 C31 122.2(6) C28 C27 C26 121.5(6) C27 C28 C32 118.5(7) C29 C28 C27 119.6(6) C29 C28 C32 121.8(7) C28 C29 C30 122.0(6) C25 C30 C33 122.9(5) C29 C30 C25 116.9(5) C29 C30 C33 120.2(5) C35 C34 C39 121.9(5) C35 C34 N4 118.8(4) C39 C34 N4 119.1(4) C34 C35 C40 122.1(5) C36 C35 C34 117.3(5) C36 C35 C40 120.6(5) C35 C36 C37 122.5(5) C36 C37 C41 120.0(5) C38 C37 C36 118.2(5) C38 C37 C41 121.8(5) C37 C38 C39 121.9(5) C34 C39 C42 120.6(5) C38 C39 C34 118.1(5) C38 C39 C42 121.3(5) C44 C43 S1 114.5(6) C44A C43A S1 106(2) C45 C44 C43 121.9(6) C49 C44 C43 122.2(6) C49 C44 C45 115.9(6) C45A C44A C43A 120.0(8) C45A C44A C49A 120.0 C49A C44A C43A 119.9(8) C44A C45A C46A 120.0 C45A C46A C47A 120.0 C46A C47A Cl1A 118.7(8) C48A C47A C46A 120.0 C48A C47A Cl1A 120.6(7) C49A C48A C47A 120.0 C48A C49A C44A 120.0 C46 C45 C44 122.4(7) C47 C46 C45 119.6(7) C46 C47 C48 121.0(7) C46 C47 Cl1 119.3(6) C48 C47 Cl1 119.7(6) C47 C48 C49 119.6(6) C48 C49 C44 121.4(6) C51 C50 S2 113.5(3) C52 C51 C50 120.1(4) C56 C51 C50 121.0(4) C56 C51 C52 118.8(5) C53 C52 C51 120.5(5) C54 C53 C52 119.0(6) C53 C54 Cl2 120.4(5) C55 C54 C53 121.4(5) C55 C54 Cl2 118.2(5) C54 C55 C56 119.3(5) C55 C56 C51 120.9(5) C0AA Ir1 Ir2 156.63(13) C0AA Ir1 S1 109.70(14) C0AA Ir1 S2 110.11(13) S1 Ir1 Ir2 54.91(3) S1 Ir1 S2 80.65(4) S2 Ir1 Ir2 53.75(2) C22 Ir2 Ir1 119.43(13) C22 Ir2 S1 95.96(13) C22 Ir2 S2 175.02(13) S1 Ir2 Ir1 55.03(3) S2 Ir2 Ir1 55.70(3) S2 Ir2 S1 81.90(4) C0AA N1 C2 111.4(4) C0AA N1 C4 126.8(4) C2 N1 C4 121.8(4) C0AA N2 C3 111.0(4) C0AA N2 C13 128.1(4) C3 N2 C13 120.6(4) C22 N3 C23 110.7(4) C22 N3 C25 128.4(4) C23 N3 C25 120.8(4) C22 N4 C24 111.5(4) C22 N4 C34 128.4(4) C24 N4 C34 120.0(4) C43 S1 Ir1 109.9(3) C43 S1 Ir2 108.0(4) C43A S1 Ir1 104.8(9) C43A S1 Ir2 107.3(15) Ir2 S1 Ir1 70.06(3) C50 S2 Ir1 105.35(15) C50 S2 Ir2 107.50(14) Ir2 S2 Ir1 70.55(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C0AA Ir1 1.969(4) C0AA N1 1.379(6) C0AA N2 1.380(6) C2 C3 1.329(8) C2 N1 1.383(6) C3 N2 1.389(6) C4 C5 1.390(6) C4 C9 1.386(7) C4 N1 1.436(6) C5 C6 1.395(7) C5 C10 1.510(7) C6 C7 1.383(8) C7 C8 1.388(8) C7 C11 1.515(7) C8 C9 1.398(7) C9 C12 1.497(7) C13 C14 1.390(7) C13 C18 1.389(8) C13 N2 1.446(6) C14 C15 1.397(7) C14 C19 1.498(8) C15 C16 1.383(7) C16 C17 1.376(8) C16 C20 1.520(7) C17 C18 1.396(7) C18 C21 1.506(7) C22 Ir2 2.036(4) C22 N3 1.364(6) C22 N4 1.359(6) C23 C24 1.333(7) C23 N3 1.386(6) C24 N4 1.394(6) C25 C26 1.386(8) C25 C30 1.393(7) C25 N3 1.439(6) C26 C27 1.397(8) C26 C31 1.516(8) C27 C28 1.390(9) C28 C29 1.362(9) C28 C32 1.520(9) C29 C30 1.375(7) C30 C33 1.498(8) C34 C35 1.393(7) C34 C39 1.398(7) C34 N4 1.435(6) C35 C36 1.388(7) C35 C40 1.504(7) C36 C37 1.390(8) C37 C38 1.377(7) C37 C41 1.506(7) C38 C39 1.388(7) C39 C42 1.507(7) C43 C44 1.476(8) C43 S1 1.851(6) C43A C44A 1.472(19) C43A S1 1.851(17) C44 C45 1.402(9) C44 C49 1.395(9) C44A C45A 1.3900 C44A C49A 1.3900 C45A C46A 1.3900 C46A C47A 1.3900 C47A C48A 1.3900 C47A Cl1A 1.66(2) C48A C49A 1.3900 C45 C46 1.360(10) C46 C47 1.358(11) C47 C48 1.359(10) C47 Cl1 1.743(8) C48 C49 1.384(10) C50 C51 1.504(6) C50 S2 1.823(4) C51 C52 1.396(7) C51 C56 1.380(7) C52 C53 1.384(8) C53 C54 1.376(9) C54 C55 1.374(9) C54 Cl2 1.740(6) C55 C56 1.379(8) Ir1 Ir2 2.7941(3) Ir1 S1 2.4357(12) Ir1 S2 2.4478(11) Ir2 S1 2.4321(11) Ir2 S2 2.3896(9) C57 O1 1.417(8) loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0002 -0.0010 -1.0002 -0.0284 -0.0531 0.0048 -0.9972 1.0043 2.0004 -0.0674 0.1764 0.0393 0.9993 0.9957 -5.0009 -0.1588 -0.2688 -0.1260 -1.0001 -1.0007 -0.0002 0.0169 0.0035 0.1501 -1.9993 -1.0020 -2.0008 -0.0935 -0.0657 0.2592 -0.9992 -0.0013 -2.0006 -0.1104 -0.0692 0.1092 0.0009 0.9995 -2.0004 -0.1273 -0.0727 -0.0409 1.9988 0.9990 -0.9999 0.0084 -0.0935 -0.2448 -0.9987 0.0018 1.0001 -0.0253 0.0899 0.0947 0.9961 -2.0048 -1.0003 0.1663 -0.1567 0.0064 1.9949 -2.0055 -1.0001 0.2200 -0.1936 -0.0931 -0.9961 2.0048 1.0003 -0.1663 0.1567 -0.0064 0.0027 2.0040 1.0004 -0.1127 0.1198 -0.1059 -0.0027 -2.0040 -1.0004 0.1127 -0.1198 0.1059 1.0005 1.0028 2.0007 0.0399 0.1026 -0.1597 0.0002 0.0010 1.0002 0.0284 0.0531 -0.0048