#------------------------------------------------------------------------------ #$Date: 2026-06-05 20:10:59 +0100 (Fri, 05 Jun 2026) $ #$Revision: 306440 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/10/7721004.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_7721004 loop_ _publ_author_name 'Amrutha, P. R.' 'Kundu, Gargi' 'Ganesh, Vemuri Lakshmi' 'Gonnade, Rajesh G.' 'Gopakumar, Gopinadhanpillai' 'Sen, Sakya S.' _publ_section_title ; Reactions of saturated NHC·boranes with electron-deficient alkynes and alkenes. Borirane formation, their reactivities, and coupling of tetracyanoethylene. ; _journal_issue 21 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 8356 _journal_page_last 8365 _journal_paper_doi 10.1039/d6dt00852f _journal_volume 55 _journal_year 2026 _chemical_formula_moiety 'C45.50 H63 Al B Cl4 N3 O4' _chemical_formula_sum 'C45.5 H63 Al B Cl4 N3 O4' _chemical_formula_weight 895.58 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2025-09-02 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2025-10-07 deposited with the CCDC. 2026-05-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 98.076(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.5696(10) _cell_length_b 21.6410(14) _cell_length_c 15.5770(11) _cell_measurement_reflns_used 65282 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.311 _cell_measurement_theta_min 2.024 _cell_volume 4862.7(6) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'SAINT (Bruker, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Photon II CPAD Area Detector' _diffrn_detector_area_resol_mean 7.39 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multilayer mirrors' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1472 _diffrn_reflns_av_unetI/netI 0.0916 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 93554 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.311 _diffrn_reflns_theta_min 2.024 _diffrn_source 'micro-focus sealed tube' _diffrn_source_type 'Incoatech I\mS HB' _exptl_absorpt_coefficient_mu 0.304 _exptl_absorpt_correction_T_max 0.0962 _exptl_absorpt_correction_T_min 0.0616 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.223 _exptl_crystal_description plate _exptl_crystal_F_000 1900 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.450 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.074 _refine_ls_extinction_coef 0.0019(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 708 _refine_ls_number_reflns 12077 _refine_ls_number_restraints 321 _refine_ls_restrained_S_all 1.107 _refine_ls_R_factor_all 0.1781 _refine_ls_R_factor_gt 0.1101 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+21.7309P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2199 _refine_ls_wR_factor_ref 0.2504 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6862 _reflns_number_total 12077 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00852f2.cif _cod_data_source_block mo_APR_5Bor_AlCl3_0m_a _cod_depositor_comments 'Adding full bibliography for 7721003--7721010.cif.' _cod_original_formula_sum 'C45.50 H63 Al B Cl4 N3 O4' _cod_database_code 7721004 _shelx_shelxl_version_number 2018/3 _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 0.991 _shelx_estimated_absorpt_t_min 0.964 _olex2_refinement_description ; 1. Restrained distances C1-B1 1.5 with sigma of 0.02 C1-B1' 1.5 with sigma of 0.02 C28-C31 1.5 with sigma of 0.02 C28'-C31' 1.5 with sigma of 0.02 B1'-N3' 1.4 with sigma of 0.02 C30-H30 1 with sigma of 0.02 C30'-C34 1.5 with sigma of 0.02 2. Restrained planarity with sigma of 0.1 3. Uiso/Uaniso restraints and constraints : within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A All non-hydrogen atoms have similar U: within 1A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1A Uanis(B1) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34') \\sim Ueq, Uanis(O4') \\sim Ueq, Uanis(O3') \\sim Ueq, Uanis(C35') \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006 Uanis(N3) \\sim Ueq, Uanis(N3') \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006 Uanis(B1) \\sim Ueq, Uanis(B1') \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006 4. Rigid body (RIGU) restrains with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Same fragment restrains 6. Others Fixed Sof: B1(0.5) H1(0.5) N3(0.6) H3(0.6) C28(0.5) C29(0.55) H29(0.55) C30(0.4) H30(0.4) O1(0.5) C31(0.6) H31A(0.6) H31B(0.6) H31C(0.6) C32(0.5) O2(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C34'(0.4) O4'(0.45) O3'(0.4) C35'(0.4) H35D(0.4) H35E(0.4) H35F(0.4) B1'(0.5) H1'(0.5) N3'(0.4) H3'(0.4) C28'(0.5) C29'(0.45) H29'(0.45) C30'(0.6) H30'(0.6) O1'(0.5) C31'(0.4) H31D(0.4) H31E(0.4) H31F(0.4) C32'(0.5) O2'(0.5) C33'(0.5) H33D(0.5) H33E(0.5) H33F(0.5) C34(0.6) O3(0.6) O4(0.55) C35(0.6) H35A(0.6) H35B(0.6) H35C(0.6) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) C7(0.5) H7(0.5) 7.a Ternary CH refined with riding coordinates: C10(H10), C13(H13), C22(H22), C25(H25), B1(H1), C29(H29), B1'(H1'), C29'(H29') 7.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B) 7.c Aromatic/amide H refined with riding coordinates: C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), N3(H3), N3'(H3'), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7) 7.d Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B, H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A, H27B,H27C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C35'(H35D,H35E,H35F), C31'(H31D,H31E,H31F), C33'(H33D,H33E,H33F), C35(H35A,H35B,H35C), C42(H42A,H42B, H42C), C1(H1A,H1B,H1C) ; _shelx_res_file ; TITL mo_APR_5Bor_AlCl3_0m_a.res in P2(1)/n mo_APR_5Bor_AlCl3_0m_a.res created by SHELXL-2018/3 at 12:11:08 on 02-Sep-2025 REM Old TITL mo_APR_5Bor_AlCl3_0m in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.305, Rweak 0.078, Alpha 0.085 REM 0.513 for 285 systematic absences, Orientation as input REM Formula found by SHELXT: C51 Al Cl4 N3 O CELL 0.71073 14.5696 21.6410 15.5770 90.000 98.076 90.000 ZERR 4.000 0.0010 0.0014 0.0011 0.000 0.002 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H AL B CL N O UNIT 182 252 4 4 16 12 16 SADI_TOL C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 C7 C2 SADI_TOL 0.04 C2 C6 C2 C4 C7 C5 C3 C7 C4 C6 C3 C5 SADI_TOL 0.02 C1 C2 SADI_TOL 0.04 C1 C7 C1 C3 FLAT_TOL C1 > C7 SIMU_TOL C1 > C7 RIGU_TOL C1 > C7 SAME_TOL C1 > C7 SIMU 0.04 0.08 1 OMIT 0 4 0 OMIT 0 2 1 OMIT 1 0 9 OMIT 1 0 1 OMIT -1 3 3 ACTA CONF SIZE 0.12 0.08 0.03 TEMP -173.150 L.S. 10 DFIX 1.50 C1 B1 DFIX 1.50 C1 B1' DFIX 1.50 C28 C31 DFIX 1.50 C28' C31' DFIX 1.40 B1' N3' DFIX 1.00 C30 H30 FREE C30 C32 FREE C30' C34' DFIX 1.50 C30' C34 ISOR 0.003 B1 > C35' ISOR 0.003 N3 N3' ISOR 0.003 B1 B1' BOND LIST 6 FMAP 2 PLAN 20 WGHT 0.000000 21.730904 EXTI 0.001945 FVAR 0.30807 MOLE 1 CL1 5 -0.091053 0.699747 0.209867 11.00000 0.06844 0.07916 = 0.04778 -0.01640 0.00832 -0.00748 CL2 5 -0.076324 0.704720 0.433164 11.00000 0.09036 0.07364 = 0.05102 0.00485 0.02133 0.03800 CL3 5 -0.003179 0.829580 0.319823 11.00000 0.05021 0.06064 = 0.12100 -0.01688 0.01293 -0.01122 CL4 5 -0.240492 0.794428 0.307588 11.00000 0.04580 0.07043 = 0.06941 0.01300 0.01102 0.00364 AL1 3 -0.103607 0.758343 0.317521 11.00000 0.04591 0.04932 = 0.04858 -0.00345 0.00792 -0.00283 MOLE 2 N1 6 0.187404 0.595570 0.357157 11.00000 0.03455 0.04287 = 0.05238 -0.00546 0.02769 -0.00578 N2 6 0.261288 0.669179 0.298904 11.00000 0.03441 0.03830 = 0.05309 -0.00746 0.02632 -0.00300 C1 1 0.270404 0.614311 0.340161 11.00000 0.04341 0.03650 = 0.06386 -0.00515 0.03934 -0.00512 C2 1 0.112296 0.638234 0.321135 11.00000 0.03234 0.06470 = 0.05839 0.00077 0.02305 -0.00212 AFIX 23 H2A 2 0.075050 0.651590 0.366294 11.00000 -1.20000 H2B 2 0.070891 0.618814 0.272786 11.00000 -1.20000 AFIX 0 C3 1 0.165369 0.691935 0.289527 11.00000 0.03675 0.04882 = 0.05987 -0.01030 0.02760 -0.00222 AFIX 23 H3A 2 0.142198 0.701905 0.228285 11.00000 -1.20000 H3B 2 0.160480 0.729176 0.325516 11.00000 -1.20000 AFIX 0 C4 1 0.167939 0.546713 0.414823 11.00000 0.02878 0.04704 = 0.05103 -0.00184 0.02379 -0.00774 C5 1 0.179344 0.559855 0.504731 11.00000 0.04689 0.05155 = 0.06095 -0.01370 0.03719 -0.01532 C6 1 0.157514 0.513060 0.558618 11.00000 0.05488 0.06768 = 0.04511 -0.00980 0.02960 -0.01874 AFIX 43 H6 2 0.165605 0.519999 0.619434 11.00000 -1.20000 AFIX 0 C7 1 0.124283 0.456460 0.527020 11.00000 0.04588 0.05746 = 0.04990 0.00260 0.01775 -0.01512 AFIX 43 H7 2 0.109508 0.425265 0.565748 11.00000 -1.20000 AFIX 0 C8 1 0.112643 0.445482 0.438521 11.00000 0.02945 0.05247 = 0.05525 -0.00007 0.01376 -0.01397 AFIX 43 H8 2 0.089521 0.406607 0.416934 11.00000 -1.20000 AFIX 0 C9 1 0.134204 0.490334 0.380904 11.00000 0.02463 0.05088 = 0.04368 -0.00244 0.01336 -0.01066 C10 1 0.210811 0.621571 0.541190 11.00000 0.07715 0.06114 = 0.06475 -0.02435 0.05426 -0.02855 AFIX 13 H10 2 0.219064 0.649552 0.491760 11.00000 -1.20000 AFIX 0 C11 1 0.304216 0.616927 0.600681 11.00000 0.05135 0.09975 = 0.11850 -0.06599 0.04576 -0.03027 AFIX 137 H11A 2 0.323059 0.658058 0.622862 11.00000 -1.50000 H11B 2 0.351301 0.600440 0.567724 11.00000 -1.50000 H11C 2 0.297793 0.589324 0.649356 11.00000 -1.50000 AFIX 0 C12 1 0.138880 0.651149 0.592512 11.00000 0.06668 0.06606 = 0.05280 -0.02041 0.03441 -0.01163 AFIX 137 H12A 2 0.157094 0.693824 0.607498 11.00000 -1.50000 H12B 2 0.136059 0.627476 0.645710 11.00000 -1.50000 H12C 2 0.077818 0.650926 0.556912 11.00000 -1.50000 AFIX 0 C13 1 0.116624 0.477100 0.284783 11.00000 0.03873 0.05917 = 0.04475 0.00274 0.01121 -0.01940 AFIX 13 H13 2 0.142484 0.512343 0.254262 11.00000 -1.20000 AFIX 0 C14 1 0.164683 0.418130 0.260671 11.00000 0.07981 0.06138 = 0.05310 -0.02103 0.02205 -0.02964 AFIX 137 H14A 2 0.152109 0.411871 0.197807 11.00000 -1.50000 H14B 2 0.141087 0.382779 0.290258 11.00000 -1.50000 H14C 2 0.231680 0.421913 0.278480 11.00000 -1.50000 AFIX 0 C15 1 0.011821 0.474065 0.253212 11.00000 0.04348 0.11291 = 0.05993 0.02753 -0.00087 -0.03176 AFIX 137 H15A 2 0.001420 0.465539 0.190812 11.00000 -1.50000 H15B 2 -0.016800 0.513666 0.264574 11.00000 -1.50000 H15C 2 -0.015918 0.441056 0.284138 11.00000 -1.50000 AFIX 0 C16 1 0.336901 0.707063 0.277979 11.00000 0.03059 0.02851 = 0.05866 -0.00124 0.02483 0.00071 C17 1 0.348442 0.712994 0.190084 11.00000 0.03711 0.03201 = 0.05304 -0.00006 0.02319 0.00189 C18 1 0.423089 0.748486 0.170655 11.00000 0.03709 0.03888 = 0.06773 0.00162 0.03042 -0.00226 AFIX 43 H18 2 0.432510 0.753211 0.111891 11.00000 -1.20000 AFIX 0 C19 1 0.482757 0.776508 0.234449 11.00000 0.03929 0.03493 = 0.06022 0.01319 0.02253 -0.00236 AFIX 43 H19 2 0.534295 0.799145 0.219948 11.00000 -1.20000 AFIX 0 C20 1 0.468034 0.771902 0.321213 11.00000 0.03539 0.03624 = 0.05220 0.00561 0.01196 -0.00154 AFIX 43 H20 2 0.508794 0.792440 0.365047 11.00000 -1.20000 AFIX 0 C21 1 0.394103 0.737448 0.343875 11.00000 0.03090 0.02901 = 0.05480 0.00428 0.02088 0.00717 C22 1 0.282407 0.685565 0.115583 11.00000 0.04381 0.05999 = 0.04157 -0.01219 0.02526 -0.01173 AFIX 13 H22 2 0.240224 0.656386 0.140894 11.00000 -1.20000 AFIX 0 C23 1 0.332912 0.648704 0.051603 11.00000 0.05855 0.06289 = 0.06824 -0.02431 0.03812 -0.01890 AFIX 137 H23A 2 0.287164 0.629213 0.007776 11.00000 -1.50000 H23B 2 0.371608 0.616755 0.083216 11.00000 -1.50000 H23C 2 0.372067 0.676715 0.023148 11.00000 -1.50000 AFIX 0 C24 1 0.222441 0.736038 0.067580 11.00000 0.03748 0.08633 = 0.05380 -0.00429 0.01308 -0.00657 AFIX 137 H24A 2 0.177247 0.717213 0.022621 11.00000 -1.50000 H24B 2 0.261907 0.764746 0.040648 11.00000 -1.50000 H24C 2 0.189685 0.758545 0.108666 11.00000 -1.50000 AFIX 0 C25 1 0.376621 0.737963 0.437510 11.00000 0.03234 0.03909 = 0.05856 0.01167 0.01885 0.00495 AFIX 13 H25 2 0.336226 0.701755 0.446042 11.00000 -1.20000 AFIX 0 C26 1 0.464987 0.731559 0.500923 11.00000 0.04149 0.04658 = 0.05927 0.00579 0.01690 -0.00382 AFIX 137 H26A 2 0.449452 0.725743 0.559592 11.00000 -1.50000 H26B 2 0.502503 0.769015 0.499279 11.00000 -1.50000 H26C 2 0.500167 0.695778 0.484916 11.00000 -1.50000 AFIX 0 C27 1 0.323296 0.797137 0.456001 11.00000 0.05190 0.05625 = 0.05562 -0.00320 0.01605 0.01690 AFIX 137 H27A 2 0.311287 0.796725 0.516343 11.00000 -1.50000 H27B 2 0.264287 0.798675 0.417145 11.00000 -1.50000 H27C 2 0.360507 0.833527 0.446239 11.00000 -1.50000 AFIX 0 PART 1 B1 4 0.372061 0.583674 0.379120 10.50000 0.03426 0.03437 = 0.03995 -0.00539 0.01212 -0.00167 AFIX 13 H1 2 0.400431 0.609212 0.429455 10.50000 -1.20000 AFIX 0 N3 6 0.369520 0.510732 0.411023 10.60000 0.03291 0.03541 = 0.03625 0.00683 0.00830 0.00211 AFIX 43 H3 2 0.335572 0.495454 0.448427 10.60000 -1.20000 AFIX 0 C28 1 0.427354 0.480268 0.370199 10.50000 0.02653 0.02851 = 0.02678 -0.00046 0.00314 -0.00013 C29 1 0.480572 0.512690 0.307745 10.55000 0.02830 0.03090 = 0.02679 0.00011 0.00430 0.00144 AFIX 13 H29 2 0.483734 0.494647 0.249132 10.55000 -1.20000 AFIX 0 C30 1 0.450241 0.571926 0.315477 10.40000 0.02665 0.02665 = 0.02792 -0.00095 0.00527 -0.00141 H30 2 0.443247 0.591713 0.256895 10.40000 -1.50000 O1 7 0.605214 0.523454 0.426083 10.50000 0.03531 0.03652 = 0.03420 0.00070 0.00174 0.00159 C31 1 0.447600 0.415714 0.402261 10.60000 0.03463 0.03570 = 0.03358 -0.00004 0.00728 0.00260 AFIX 137 H31A 2 0.455591 0.388817 0.353242 10.60000 -1.50000 H31B 2 0.395904 0.400569 0.430447 10.60000 -1.50000 H31C 2 0.504542 0.415551 0.444058 10.60000 -1.50000 AFIX 0 C32 1 0.564592 0.543365 0.357580 10.50000 0.02224 0.02395 = 0.02298 -0.00022 0.00594 0.00050 O2 7 0.591990 0.592332 0.317018 10.50000 0.02755 0.02922 = 0.03088 0.00331 0.00325 -0.00588 C33 1 0.675713 0.624187 0.360034 10.50000 0.04145 0.04510 = 0.04457 0.00378 0.00618 -0.00477 AFIX 137 H33A 2 0.691558 0.658235 0.323317 10.50000 -1.50000 H33B 2 0.727424 0.594871 0.369288 10.50000 -1.50000 H33C 2 0.663696 0.640589 0.416031 10.50000 -1.50000 AFIX 0 C34' 1 0.360719 0.495511 0.209659 10.40000 0.02535 0.02629 = 0.02757 0.00111 0.00630 -0.00223 O4' 7 0.375582 0.448406 0.161579 10.45000 0.03887 0.04060 = 0.04240 -0.00186 0.00618 0.00050 O3' 7 0.296178 0.529312 0.194481 10.40000 0.03224 0.03757 = 0.03926 0.00297 0.00544 0.00302 C35' 1 0.311242 0.435712 0.084394 10.40000 0.05113 0.05224 = 0.04946 -0.00160 0.00717 -0.00052 AFIX 137 H35D 2 0.321560 0.393738 0.064158 10.40000 -1.50000 H35E 2 0.320849 0.465463 0.039067 10.40000 -1.50000 H35F 2 0.247629 0.439316 0.097547 10.40000 -1.50000 AFIX 0 PART 2 B1' 4 0.361663 0.579089 0.347750 10.50000 0.02853 0.02834 = 0.02530 -0.00108 0.00587 -0.00273 AFIX 13 H1' 2 0.407825 0.604562 0.386088 10.50000 -1.20000 AFIX 0 N3' 6 0.361370 0.516914 0.389823 10.40000 0.01908 0.02237 = 0.01847 0.00448 0.00276 -0.00127 AFIX 43 H3' 2 0.329889 0.511782 0.433548 10.40000 -1.20000 AFIX 0 C28' 1 0.403873 0.472841 0.364993 10.50000 0.04074 0.03111 = 0.03285 0.00478 0.01308 -0.00847 C29' 1 0.434977 0.503162 0.286902 10.45000 0.03495 0.03389 = 0.03179 -0.00545 0.00930 -0.00547 AFIX 13 H29' 2 0.494926 0.488498 0.269795 10.45000 -1.20000 AFIX 0 C30' 1 0.410582 0.560393 0.266314 10.60000 0.02546 0.03515 = 0.03481 0.00226 0.01650 0.00254 H30' 2 0.437211 0.607422 0.234211 10.60000 -1.50000 O1' 7 0.589667 0.542202 0.406589 10.50000 0.02440 0.03783 = 0.06309 -0.00046 0.01339 -0.00028 C31' 1 0.407857 0.404659 0.379964 10.40000 0.03054 0.02742 = 0.05575 -0.00015 0.00540 -0.00658 AFIX 137 H31D 2 0.388184 0.383130 0.325115 10.40000 -1.50000 H31E 2 0.366504 0.393514 0.421984 10.40000 -1.50000 H31F 2 0.471496 0.392599 0.402616 10.40000 -1.50000 AFIX 0 C32' 1 0.546435 0.580043 0.357657 10.50000 0.03394 0.04766 = 0.03570 -0.01369 0.01628 -0.01292 O2' 7 0.578289 0.635176 0.340437 10.50000 0.03036 0.04900 = 0.05447 0.01626 0.01341 -0.00795 C33' 1 0.669687 0.647749 0.376965 10.50000 0.02692 0.06330 = 0.05899 0.00400 0.00932 -0.01038 AFIX 137 H33D 2 0.686347 0.689706 0.361205 10.50000 -1.50000 H33E 2 0.711503 0.618006 0.355055 10.50000 -1.50000 H33F 2 0.675219 0.644339 0.440217 10.50000 -1.50000 AFIX 0 C34 1 0.342103 0.530446 0.195085 10.60000 0.02962 0.04158 = 0.02653 -0.00042 0.01629 -0.00778 O3 7 0.265574 0.549550 0.171632 10.60000 0.04002 0.04286 = 0.02922 -0.00196 0.00536 -0.00052 O4 7 0.374427 0.480584 0.159810 10.55000 0.02863 0.04004 = 0.03162 -0.00387 -0.00331 0.00366 C35 1 0.315852 0.452806 0.086365 10.60000 0.03578 0.05114 = 0.03059 -0.01316 0.00244 0.00027 AFIX 137 H35A 2 0.342000 0.412904 0.072518 10.60000 -1.50000 H35B 2 0.312847 0.480270 0.036025 10.60000 -1.50000 H35C 2 0.253322 0.446565 0.101167 10.60000 -1.50000 AFIX 0 PART 0 MOLE 3 C36 1 0.645786 0.590223 0.128438 11.00000 0.05185 0.04891 = 0.06619 -0.01200 0.03053 -0.00072 C37 1 0.575981 0.548048 0.105155 11.00000 0.03408 0.07734 = 0.07558 -0.00562 0.02332 0.00733 AFIX 43 H37 2 0.515843 0.562392 0.082392 11.00000 -1.20000 AFIX 0 C38 1 0.591567 0.485686 0.114184 11.00000 0.04685 0.06843 = 0.06501 -0.01676 0.02435 -0.01428 AFIX 43 H38 2 0.542380 0.457497 0.097187 11.00000 -1.20000 AFIX 0 C39 1 0.676607 0.463918 0.147173 11.00000 0.05959 0.05104 = 0.06226 0.00080 0.02925 -0.00012 AFIX 43 H39 2 0.686672 0.420666 0.153169 11.00000 -1.20000 AFIX 0 C40 1 0.746889 0.503629 0.171470 11.00000 0.04552 0.07639 = 0.06249 0.00130 0.00890 0.00867 AFIX 43 H40 2 0.806199 0.488428 0.195289 11.00000 -1.20000 AFIX 0 C41 1 0.732002 0.567696 0.161389 11.00000 0.04361 0.06723 = 0.06344 -0.01496 0.01284 -0.00720 AFIX 43 H41 2 0.781811 0.595587 0.177441 11.00000 -1.20000 AFIX 0 C42 1 0.627937 0.658804 0.118609 11.00000 0.08934 0.05524 = 0.11412 -0.00151 0.05341 0.01720 AFIX 137 H42A 2 0.686986 0.681132 0.128739 11.00000 -1.50000 H42B 2 0.588207 0.672260 0.160874 11.00000 -1.50000 H42C 2 0.597040 0.667504 0.059837 11.00000 -1.50000 AFIX 0 MOLE 4 RESI TOL 1 PART -1 10.5 C1 1 -0.053702 0.407313 -0.058220 10.50000 0.08582 0.05912 = 0.06153 -0.01216 -0.00814 -0.01143 AFIX 137 H1A 2 -0.101609 0.415360 -0.107700 10.50000 -1.50000 H1B 2 -0.079717 0.381896 -0.015478 10.50000 -1.50000 H1C 2 -0.001744 0.385399 -0.078152 10.50000 -1.50000 AFIX 0 C2 1 -0.019903 0.467763 -0.017180 10.50000 0.03808 0.05372 = 0.03792 -0.00082 0.00502 -0.00458 C3 1 -0.082145 0.505452 0.017092 10.50000 0.04112 0.06530 = 0.04795 0.00853 0.01402 0.00413 AFIX 43 H3 2 -0.144905 0.492913 0.015030 10.50000 -1.20000 AFIX 0 C4 1 -0.053464 0.560958 0.054099 10.50000 0.06473 0.06138 = 0.05804 0.00380 0.02111 0.01050 AFIX 43 H4 2 -0.097494 0.587077 0.075521 10.50000 -1.20000 AFIX 0 C5 1 0.037352 0.579697 0.060940 10.50000 0.07107 0.05267 = 0.05213 0.00144 -0.00133 -0.00343 AFIX 43 H5 2 0.057061 0.617233 0.089355 10.50000 -1.20000 AFIX 0 C6 1 0.098881 0.542724 0.025607 10.50000 0.04888 0.06069 = 0.07630 0.00452 0.00572 -0.01125 AFIX 43 H6 2 0.161384 0.555687 0.027114 10.50000 -1.20000 AFIX 0 C7 1 0.070714 0.486863 -0.012102 10.50000 0.03280 0.06082 = 0.06006 0.00533 0.00019 0.00079 AFIX 43 H7 2 0.114522 0.461292 -0.034835 10.50000 -1.20000 PART 0 RESI 0 AFIX 0 HKLF 4 REM mo_APR_5Bor_AlCl3_0m_a.res in P2(1)/n REM wR2 = 0.250395, GooF = S = 1.11568, Restrained GooF = 1.10711 for all data REM R1 = 0.110138 for 6862 Fo > 4sig(Fo) and 0.178139 for all 12077 data REM 708 parameters refined using 321 restraints END WGHT 0.0000 21.7393 REM Highest difference peak 0.450, deepest hole -0.425, 1-sigma level 0.074 Q1 1 -0.0087 0.7217 0.4585 11.00000 0.05 0.45 Q2 1 0.3884 0.5764 0.4036 11.00000 0.05 0.39 Q3 1 0.5035 0.4686 0.2613 11.00000 0.05 0.37 Q4 1 0.0192 0.8009 0.2817 11.00000 0.05 0.36 Q5 1 -0.1546 0.6686 0.2027 11.00000 0.05 0.35 Q6 1 0.1792 0.4787 0.5436 11.00000 0.05 0.34 Q7 1 0.3275 0.6002 0.3324 11.00000 0.05 0.34 Q8 1 -0.2014 0.7739 0.2825 11.00000 0.05 0.32 Q9 1 -0.3211 0.8274 0.2988 11.00000 0.05 0.31 Q10 1 -0.0565 0.6622 0.5206 11.00000 0.05 0.31 Q11 1 -0.1617 0.7771 0.3905 11.00000 0.05 0.30 Q12 1 0.0157 0.8152 0.3820 11.00000 0.05 0.30 Q13 1 -0.2332 0.7931 0.3855 11.00000 0.05 0.29 Q14 1 0.1979 0.5320 0.5320 11.00000 0.05 0.29 Q15 1 0.2602 0.6332 0.3223 11.00000 0.05 0.28 Q16 1 -0.0874 0.6896 0.2752 11.00000 0.05 0.27 Q17 1 -0.0729 0.7087 0.5032 11.00000 0.05 0.27 Q18 1 -0.0760 0.6685 0.2364 11.00000 0.05 0.26 Q19 1 0.4866 0.7915 0.0791 11.00000 0.05 0.26 Q20 1 -0.0864 0.7561 0.3833 11.00000 0.05 0.26 ; _shelx_res_checksum 35854 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' '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 Cl1 Cl -0.09105(13) 0.69975(9) 0.20987(11) 0.0651(5) Uani 1 1 d . . . . . Cl2 Cl -0.07632(14) 0.70472(9) 0.43316(11) 0.0706(6) Uani 1 1 d . . . . . Cl3 Cl -0.00318(13) 0.82958(8) 0.31982(15) 0.0772(6) Uani 1 1 d . . . . . Cl4 Cl -0.24049(11) 0.79443(8) 0.30759(12) 0.0616(5) Uani 1 1 d . . . . . Al1 Al -0.10361(13) 0.75834(8) 0.31752(12) 0.0478(4) Uani 1 1 d . . . . . N1 N 0.1874(3) 0.5956(2) 0.3572(3) 0.0412(11) Uani 1 1 d . . . . . N2 N 0.2613(3) 0.6692(2) 0.2989(3) 0.0400(11) Uani 1 1 d . . . . . C1 C 0.2704(4) 0.6143(2) 0.3402(4) 0.0449(14) Uani 1 1 d D . . . . C2 C 0.1123(4) 0.6382(3) 0.3211(4) 0.0502(15) Uani 1 1 d . . . . . H2A H 0.075050 0.651590 0.366294 0.060 Uiso 1 1 calc R U . . . H2B H 0.070891 0.618814 0.272786 0.060 Uiso 1 1 calc R U . . . C3 C 0.1654(4) 0.6919(3) 0.2895(4) 0.0465(14) Uani 1 1 d . . . . . H3A H 0.142198 0.701905 0.228285 0.056 Uiso 1 1 calc R U . . . H3B H 0.160480 0.729176 0.325516 0.056 Uiso 1 1 calc R U . . . C4 C 0.1679(4) 0.5467(3) 0.4148(4) 0.0405(13) Uani 1 1 d . . . . . C5 C 0.1793(4) 0.5599(3) 0.5047(4) 0.0503(16) Uani 1 1 d . . . . . C6 C 0.1575(4) 0.5131(3) 0.5586(4) 0.0537(16) Uani 1 1 d . . . . . H6 H 0.165605 0.519999 0.619434 0.064 Uiso 1 1 calc R U . . . C7 C 0.1243(4) 0.4565(3) 0.5270(4) 0.0500(15) Uani 1 1 d . . . . . H7 H 0.109508 0.425265 0.565748 0.060 Uiso 1 1 calc R U . . . C8 C 0.1126(4) 0.4455(3) 0.4385(4) 0.0450(14) Uani 1 1 d . . . . . H8 H 0.089521 0.406607 0.416934 0.054 Uiso 1 1 calc R U . . . C9 C 0.1342(3) 0.4903(3) 0.3809(4) 0.0389(12) Uani 1 1 d . . . . . C10 C 0.2108(5) 0.6216(3) 0.5412(4) 0.063(2) Uani 1 1 d . . . . . H10 H 0.219064 0.649552 0.491760 0.076 Uiso 1 1 calc R U . . . C11 C 0.3042(5) 0.6169(4) 0.6007(6) 0.087(3) Uani 1 1 d . . . . . H11A H 0.323059 0.658058 0.622862 0.130 Uiso 1 1 calc R U . . . H11B H 0.351301 0.600440 0.567724 0.130 Uiso 1 1 calc R U . . . H11C H 0.297793 0.589324 0.649356 0.130 Uiso 1 1 calc R U . . . C12 C 0.1389(5) 0.6511(3) 0.5925(4) 0.0594(18) Uani 1 1 d . . . . . H12A H 0.157094 0.693824 0.607498 0.089 Uiso 1 1 calc R U . . . H12B H 0.136059 0.627476 0.645710 0.089 Uiso 1 1 calc R U . . . H12C H 0.077818 0.650926 0.556912 0.089 Uiso 1 1 calc R U . . . C13 C 0.1166(4) 0.4771(3) 0.2848(4) 0.0470(14) Uani 1 1 d . . . . . H13 H 0.142484 0.512343 0.254262 0.056 Uiso 1 1 calc R U . . . C14 C 0.1647(5) 0.4181(3) 0.2607(4) 0.0635(19) Uani 1 1 d . . . . . H14A H 0.152109 0.411871 0.197807 0.095 Uiso 1 1 calc R U . . . H14B H 0.141087 0.382779 0.290258 0.095 Uiso 1 1 calc R U . . . H14C H 0.231680 0.421913 0.278480 0.095 Uiso 1 1 calc R U . . . C15 C 0.0118(5) 0.4741(4) 0.2532(5) 0.073(2) Uani 1 1 d . . . . . H15A H 0.001420 0.465539 0.190812 0.109 Uiso 1 1 calc R U . . . H15B H -0.016800 0.513666 0.264574 0.109 Uiso 1 1 calc R U . . . H15C H -0.015918 0.441056 0.284138 0.109 Uiso 1 1 calc R U . . . C16 C 0.3369(3) 0.7071(2) 0.2780(4) 0.0375(12) Uani 1 1 d . . . . . C17 C 0.3484(4) 0.7130(2) 0.1901(4) 0.0391(12) Uani 1 1 d . . . . . C18 C 0.4231(4) 0.7485(2) 0.1707(4) 0.0457(14) Uani 1 1 d . . . . . H18 H 0.432510 0.753211 0.111891 0.055 Uiso 1 1 calc R U . . . C19 C 0.4828(4) 0.7765(2) 0.2344(4) 0.0433(14) Uani 1 1 d . . . . . H19 H 0.534295 0.799145 0.219948 0.052 Uiso 1 1 calc R U . . . C20 C 0.4680(4) 0.7719(2) 0.3212(4) 0.0407(12) Uani 1 1 d . . . . . H20 H 0.508794 0.792440 0.365047 0.049 Uiso 1 1 calc R U . . . C21 C 0.3941(4) 0.7374(2) 0.3439(4) 0.0368(12) Uani 1 1 d . . . . . C22 C 0.2824(4) 0.6856(3) 0.1156(4) 0.0466(14) Uani 1 1 d . . . . . H22 H 0.240224 0.656386 0.140894 0.056 Uiso 1 1 calc R U . . . C23 C 0.3329(5) 0.6487(3) 0.0516(4) 0.0604(19) Uani 1 1 d . . . . . H23A H 0.287164 0.629213 0.007776 0.091 Uiso 1 1 calc R U . . . H23B H 0.371608 0.616755 0.083216 0.091 Uiso 1 1 calc R U . . . H23C H 0.372067 0.676715 0.023148 0.091 Uiso 1 1 calc R U . . . C24 C 0.2224(4) 0.7360(3) 0.0676(4) 0.0586(17) Uani 1 1 d . . . . . H24A H 0.177247 0.717213 0.022621 0.088 Uiso 1 1 calc R U . . . H24B H 0.261907 0.764746 0.040648 0.088 Uiso 1 1 calc R U . . . H24C H 0.189685 0.758545 0.108666 0.088 Uiso 1 1 calc R U . . . C25 C 0.3766(4) 0.7380(3) 0.4375(4) 0.0421(13) Uani 1 1 d . . . . . H25 H 0.336226 0.701755 0.446042 0.051 Uiso 1 1 calc R U . . . C26 C 0.4650(4) 0.7316(3) 0.5009(4) 0.0482(14) Uani 1 1 d . . . . . H26A H 0.449452 0.725743 0.559592 0.072 Uiso 1 1 calc R U . . . H26B H 0.502503 0.769015 0.499279 0.072 Uiso 1 1 calc R U . . . H26C H 0.500167 0.695778 0.484916 0.072 Uiso 1 1 calc R U . . . C27 C 0.3233(4) 0.7971(3) 0.4560(4) 0.0538(16) Uani 1 1 d . . . . . H27A H 0.311287 0.796725 0.516343 0.081 Uiso 1 1 calc R U . . . H27B H 0.264287 0.798675 0.417145 0.081 Uiso 1 1 calc R U . . . H27C H 0.360507 0.833527 0.446239 0.081 Uiso 1 1 calc R U . . . B1 B 0.3721(9) 0.5837(6) 0.3791(10) 0.036(3) Uani 0.5 1 d D U P A 1 H1 H 0.400431 0.609212 0.429455 0.043 Uiso 0.5 1 calc R U P A 1 N3 N 0.3695(8) 0.5107(5) 0.4110(7) 0.035(3) Uani 0.6 1 d . U P A 1 H3 H 0.335572 0.495454 0.448427 0.041 Uiso 0.6 1 calc R U P A 1 C28 C 0.4274(12) 0.4803(7) 0.3702(15) 0.027(4) Uani 0.5 1 d D U P A 1 C29 C 0.4806(7) 0.5127(4) 0.3077(6) 0.029(2) Uani 0.55 1 d . U P A 1 H29 H 0.483734 0.494647 0.249132 0.034 Uiso 0.55 1 calc R U P A 1 C30 C 0.4502(9) 0.5719(5) 0.3155(8) 0.027(2) Uani 0.4 1 d D U P A 1 H30 H 0.443(14) 0.592(8) 0.257(5) 0.040 Uiso 0.4 1 d D U P B 1 O1 O 0.6052(10) 0.5235(5) 0.4261(9) 0.036(3) Uani 0.5 1 d . U P A 1 C31 C 0.4476(7) 0.4157(4) 0.4023(7) 0.034(2) Uani 0.6 1 d D U P A 1 H31A H 0.455591 0.388817 0.353242 0.052 Uiso 0.6 1 calc R U P A 1 H31B H 0.395904 0.400569 0.430447 0.052 Uiso 0.6 1 calc R U P A 1 H31C H 0.504542 0.415551 0.444058 0.052 Uiso 0.6 1 calc R U P A 1 C32 C 0.5646(8) 0.5434(6) 0.3576(7) 0.023(2) Uani 0.5 1 d . U P A 1 O2 O 0.5920(5) 0.5923(3) 0.3170(4) 0.0293(14) Uani 0.5 1 d . U P A 1 C33 C 0.6757(13) 0.6242(7) 0.3600(12) 0.044(4) Uani 0.5 1 d . U P A 1 H33A H 0.691558 0.658235 0.323317 0.066 Uiso 0.5 1 calc R U P A 1 H33B H 0.727424 0.594871 0.369288 0.066 Uiso 0.5 1 calc R U P A 1 H33C H 0.663696 0.640589 0.416031 0.066 Uiso 0.5 1 calc R U P A 1 C34' C 0.3607(9) 0.4955(7) 0.2097(9) 0.026(3) Uani 0.4 1 d . U P C 1 O4' O 0.3756(7) 0.4484(5) 0.1616(7) 0.041(3) Uani 0.45 1 d . U P C 1 O3' O 0.2962(10) 0.5293(6) 0.1945(9) 0.036(3) Uani 0.4 1 d . U P C 1 C35' C 0.311(3) 0.4357(15) 0.084(3) 0.051(9) Uani 0.4 1 d . U P C 1 H35D H 0.321560 0.393738 0.064158 0.076 Uiso 0.4 1 calc R U P C 1 H35E H 0.320849 0.465463 0.039067 0.076 Uiso 0.4 1 calc R U P C 1 H35F H 0.247629 0.439316 0.097547 0.076 Uiso 0.4 1 calc R U P C 1 B1' B 0.3617(8) 0.5791(5) 0.3477(9) 0.027(3) Uani 0.5 1 d D U P A 2 H1' H 0.407825 0.604562 0.386088 0.033 Uiso 0.5 1 calc R U P A 2 N3' N 0.3614(11) 0.5169(6) 0.3898(9) 0.020(3) Uani 0.4 1 d D U P A 2 H3' H 0.329889 0.511782 0.433548 0.024 Uiso 0.4 1 calc R U P A 2 C28' C 0.4039(13) 0.4728(7) 0.3650(14) 0.034(4) Uani 0.5 1 d D U P A 2 C29' C 0.4350(9) 0.5032(5) 0.2869(8) 0.033(3) Uani 0.45 1 d . U P A 2 H29' H 0.494926 0.488498 0.269795 0.040 Uiso 0.45 1 calc R U P A 2 C30' C 0.4106(6) 0.5604(4) 0.2663(6) 0.0306(18) Uani 0.6 1 d D U P A 2 H30' H 0.437(9) 0.607(5) 0.234(7) 0.046 Uiso 0.6 1 d . U P D 2 O1' O 0.5897(9) 0.5422(6) 0.4066(10) 0.041(3) Uani 0.5 1 d . U P E 2 C31' C 0.4079(11) 0.4047(6) 0.3800(11) 0.038(4) Uani 0.4 1 d D U P A 2 H31D H 0.388184 0.383130 0.325115 0.057 Uiso 0.4 1 calc R U P A 2 H31E H 0.366504 0.393514 0.421984 0.057 Uiso 0.4 1 calc R U P A 2 H31F H 0.471496 0.392599 0.402616 0.057 Uiso 0.4 1 calc R U P A 2 C32' C 0.5464(8) 0.5800(6) 0.3577(7) 0.038(2) Uani 0.5 1 d . U P E 2 O2' O 0.5783(5) 0.6352(4) 0.3404(5) 0.0439(19) Uani 0.5 1 d . . P E 2 C33' C 0.6697(11) 0.6477(8) 0.3770(12) 0.049(4) Uani 0.5 1 d . U P E 2 H33D H 0.686347 0.689706 0.361205 0.074 Uiso 0.5 1 calc R U P E 2 H33E H 0.711503 0.618006 0.355055 0.074 Uiso 0.5 1 calc R U P E 2 H33F H 0.675219 0.644339 0.440217 0.074 Uiso 0.5 1 calc R U P E 2 C34 C 0.3421(8) 0.5304(5) 0.1951(6) 0.031(2) Uani 0.6 1 d D U P A 2 O3 O 0.2656(5) 0.5495(3) 0.1716(5) 0.0373(17) Uani 0.6 1 d . U P A 2 O4 O 0.3744(5) 0.4806(4) 0.1598(5) 0.0342(15) Uani 0.55 1 d . U P A 2 C35 C 0.3159(14) 0.4528(10) 0.0864(13) 0.039(3) Uani 0.6 1 d . U P A 2 H35A H 0.342000 0.412904 0.072518 0.059 Uiso 0.6 1 calc R U P A 2 H35B H 0.312847 0.480270 0.036025 0.059 Uiso 0.6 1 calc R U P A 2 H35C H 0.253322 0.446565 0.101167 0.059 Uiso 0.6 1 calc R U P A 2 C36 C 0.6458(5) 0.5902(3) 0.1284(4) 0.0535(16) Uani 1 1 d . . . . . C37 C 0.5760(4) 0.5480(3) 0.1052(5) 0.0608(18) Uani 1 1 d . . . . . H37 H 0.515843 0.562392 0.082392 0.073 Uiso 1 1 calc R U . . . C38 C 0.5916(5) 0.4857(3) 0.1142(4) 0.0585(17) Uani 1 1 d . . . . . H38 H 0.542380 0.457497 0.097187 0.070 Uiso 1 1 calc R U . . . C39 C 0.6766(5) 0.4639(3) 0.1472(4) 0.0557(16) Uani 1 1 d . . . . . H39 H 0.686672 0.420666 0.153169 0.067 Uiso 1 1 calc R U . . . C40 C 0.7469(5) 0.5036(3) 0.1715(4) 0.0613(18) Uani 1 1 d . . . . . H40 H 0.806199 0.488428 0.195289 0.074 Uiso 1 1 calc R U . . . C41 C 0.7320(5) 0.5677(3) 0.1614(4) 0.0576(17) Uani 1 1 d . . . . . H41 H 0.781811 0.595587 0.177441 0.069 Uiso 1 1 calc R U . . . C42 C 0.6279(6) 0.6588(3) 0.1186(6) 0.082(3) Uani 1 1 d . . . . . H42A H 0.686986 0.681132 0.128739 0.124 Uiso 1 1 calc R U . . . H42B H 0.588207 0.672260 0.160874 0.124 Uiso 1 1 calc R U . . . H42C H 0.597040 0.667504 0.059837 0.124 Uiso 1 1 calc R U . . . C1_1 C -0.0537(14) 0.4073(9) -0.0582(13) 0.071(6) Uani 0.5 1 d D U P F -1 H1A_1 H -0.101609 0.415360 -0.107700 0.106 Uiso 0.5 1 calc R U P F -1 H1B_1 H -0.079717 0.381896 -0.015478 0.106 Uiso 0.5 1 calc R U P F -1 H1C_1 H -0.001744 0.385399 -0.078152 0.106 Uiso 0.5 1 calc R U P F -1 C2_1 C -0.0199(7) 0.4678(5) -0.0172(7) 0.043(2) Uani 0.5 1 d D U P F -1 C3_1 C -0.0821(12) 0.5055(8) 0.0171(14) 0.051(4) Uani 0.5 1 d D U P F -1 H3_1 H -0.144905 0.492913 0.015030 0.061 Uiso 0.5 1 calc R U P F -1 C4_1 C -0.0535(9) 0.5610(6) 0.0541(8) 0.060(3) Uani 0.5 1 d D U P F -1 H4_1 H -0.097494 0.587077 0.075521 0.072 Uiso 0.5 1 calc R U P F -1 C5_1 C 0.0374(10) 0.5797(8) 0.0609(14) 0.060(5) Uani 0.5 1 d D U P F -1 H5_1 H 0.057061 0.617233 0.089355 0.071 Uiso 0.5 1 calc R U P F -1 C6_1 C 0.0989(9) 0.5427(5) 0.0256(9) 0.062(3) Uani 0.5 1 d D U P F -1 H6_1 H 0.161384 0.555687 0.027114 0.075 Uiso 0.5 1 calc R U P F -1 C7_1 C 0.0707(11) 0.4869(8) -0.0121(16) 0.052(5) Uani 0.5 1 d D U P F -1 H7_1 H 0.114522 0.461292 -0.034835 0.062 Uiso 0.5 1 calc R U P F -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0684(11) 0.0792(12) 0.0478(9) -0.0164(8) 0.0083(8) -0.0075(9) Cl2 0.0904(14) 0.0736(11) 0.0510(9) 0.0049(8) 0.0213(9) 0.0380(10) Cl3 0.0502(10) 0.0606(11) 0.1210(17) -0.0169(11) 0.0129(10) -0.0112(8) Cl4 0.0458(9) 0.0704(11) 0.0694(11) 0.0130(9) 0.0110(8) 0.0036(8) Al1 0.0459(10) 0.0493(10) 0.0486(10) -0.0035(8) 0.0079(8) -0.0028(8) N1 0.035(2) 0.043(3) 0.052(3) -0.005(2) 0.028(2) -0.0058(19) N2 0.034(2) 0.038(2) 0.053(3) -0.007(2) 0.026(2) -0.0030(19) C1 0.043(3) 0.036(3) 0.064(4) -0.005(3) 0.039(3) -0.005(2) C2 0.032(3) 0.065(4) 0.058(4) 0.001(3) 0.023(3) -0.002(3) C3 0.037(3) 0.049(3) 0.060(4) -0.010(3) 0.028(3) -0.002(2) C4 0.029(3) 0.047(3) 0.051(3) -0.002(3) 0.024(2) -0.008(2) C5 0.047(3) 0.052(3) 0.061(4) -0.014(3) 0.037(3) -0.015(3) C6 0.055(4) 0.068(4) 0.045(3) -0.010(3) 0.030(3) -0.019(3) C7 0.046(3) 0.057(4) 0.050(4) 0.003(3) 0.018(3) -0.015(3) C8 0.029(3) 0.052(3) 0.055(4) 0.000(3) 0.014(3) -0.014(2) C9 0.025(3) 0.051(3) 0.044(3) -0.002(2) 0.013(2) -0.011(2) C10 0.077(5) 0.061(4) 0.065(4) -0.024(3) 0.054(4) -0.029(3) C11 0.051(4) 0.100(6) 0.118(7) -0.066(5) 0.046(5) -0.030(4) C12 0.067(4) 0.066(4) 0.053(4) -0.020(3) 0.034(3) -0.012(3) C13 0.039(3) 0.059(4) 0.045(3) 0.003(3) 0.011(3) -0.019(3) C14 0.080(5) 0.061(4) 0.053(4) -0.021(3) 0.022(4) -0.030(4) C15 0.043(4) 0.113(6) 0.060(4) 0.028(4) -0.001(3) -0.032(4) C16 0.031(3) 0.029(2) 0.059(3) -0.001(2) 0.025(2) 0.001(2) C17 0.037(3) 0.032(3) 0.053(3) 0.000(2) 0.023(3) 0.002(2) C18 0.037(3) 0.039(3) 0.068(4) 0.002(3) 0.030(3) -0.002(2) C19 0.039(3) 0.035(3) 0.060(4) 0.013(3) 0.023(3) -0.002(2) C20 0.035(3) 0.036(3) 0.052(3) 0.006(2) 0.012(3) -0.002(2) C21 0.031(3) 0.029(2) 0.055(3) 0.004(2) 0.021(2) 0.007(2) C22 0.044(3) 0.060(4) 0.042(3) -0.012(3) 0.025(3) -0.012(3) C23 0.059(4) 0.063(4) 0.068(4) -0.024(3) 0.038(4) -0.019(3) C24 0.037(3) 0.086(5) 0.054(4) -0.004(3) 0.013(3) -0.007(3) C25 0.032(3) 0.039(3) 0.059(4) 0.012(3) 0.019(3) 0.005(2) C26 0.041(3) 0.047(3) 0.059(4) 0.006(3) 0.017(3) -0.004(3) C27 0.052(4) 0.056(4) 0.056(4) -0.003(3) 0.016(3) 0.017(3) B1 0.034(4) 0.034(4) 0.040(4) -0.005(3) 0.012(3) -0.002(3) N3 0.033(3) 0.035(3) 0.036(4) 0.007(3) 0.008(3) 0.002(2) C28 0.027(5) 0.029(5) 0.027(5) 0.000(3) 0.003(3) 0.000(3) C29 0.028(3) 0.031(3) 0.027(3) 0.000(2) 0.004(2) 0.001(2) C30 0.027(3) 0.027(3) 0.028(3) -0.001(3) 0.005(3) -0.001(3) O1 0.035(5) 0.037(5) 0.034(5) 0.001(4) 0.002(4) 0.002(4) C31 0.035(4) 0.036(4) 0.034(4) 0.000(3) 0.007(4) 0.003(4) C32 0.022(3) 0.024(3) 0.023(3) 0.000(3) 0.006(2) 0.001(2) O2 0.028(2) 0.029(2) 0.031(2) 0.003(2) 0.003(2) -0.006(2) C33 0.041(6) 0.045(6) 0.045(6) 0.004(5) 0.006(4) -0.005(5) C34' 0.025(4) 0.026(3) 0.028(4) 0.001(3) 0.006(3) -0.002(3) O4' 0.039(3) 0.041(3) 0.042(3) -0.002(3) 0.006(2) 0.000(3) O3' 0.032(5) 0.038(5) 0.039(5) 0.003(4) 0.005(4) 0.003(5) C35' 0.051(10) 0.052(11) 0.049(10) -0.002(6) 0.007(6) -0.001(6) B1' 0.029(4) 0.028(4) 0.025(4) -0.001(3) 0.006(3) -0.003(3) N3' 0.019(4) 0.022(4) 0.018(4) 0.004(3) 0.003(3) -0.001(3) C28' 0.041(10) 0.031(7) 0.033(7) 0.005(5) 0.013(7) -0.008(6) C29' 0.035(7) 0.034(6) 0.032(6) -0.005(5) 0.009(5) -0.005(5) C30' 0.025(4) 0.035(4) 0.035(5) 0.002(4) 0.017(4) 0.003(3) O1' 0.024(6) 0.038(7) 0.063(10) 0.000(6) 0.013(6) 0.000(5) C31' 0.031(8) 0.027(7) 0.056(10) 0.000(7) 0.005(7) -0.007(6) C32' 0.034(6) 0.048(7) 0.036(6) -0.014(5) 0.016(5) -0.013(5) O2' 0.030(4) 0.049(5) 0.054(5) 0.016(4) 0.013(4) -0.008(3) C33' 0.027(7) 0.063(11) 0.059(10) 0.004(9) 0.009(6) -0.010(7) C34 0.030(5) 0.042(6) 0.027(4) 0.000(4) 0.016(4) -0.008(5) O3 0.040(4) 0.043(4) 0.029(4) -0.002(3) 0.005(3) -0.001(3) O4 0.029(4) 0.040(4) 0.032(4) -0.004(4) -0.003(3) 0.004(3) C35 0.036(6) 0.051(11) 0.031(6) -0.013(7) 0.002(4) 0.000(7) C36 0.052(4) 0.049(3) 0.066(4) -0.012(3) 0.031(3) -0.001(3) C37 0.034(3) 0.077(5) 0.076(5) -0.006(4) 0.023(3) 0.007(3) C38 0.047(4) 0.068(4) 0.065(4) -0.017(3) 0.024(3) -0.014(3) C39 0.060(4) 0.051(4) 0.062(4) 0.001(3) 0.029(3) 0.000(3) C40 0.046(4) 0.076(5) 0.062(4) 0.001(4) 0.009(3) 0.009(3) C41 0.044(4) 0.067(4) 0.063(4) -0.015(3) 0.013(3) -0.007(3) C42 0.089(6) 0.055(4) 0.114(7) -0.002(4) 0.053(5) 0.017(4) C1_1 0.086(13) 0.059(10) 0.062(13) -0.012(9) -0.008(10) -0.011(8) C2_1 0.038(5) 0.054(6) 0.038(6) -0.001(5) 0.005(4) -0.005(4) C3_1 0.041(7) 0.065(8) 0.048(10) 0.009(7) 0.014(7) 0.004(6) C4_1 0.065(7) 0.061(7) 0.058(8) 0.004(6) 0.021(6) 0.010(6) C5_1 0.071(8) 0.053(9) 0.052(11) 0.001(7) -0.001(8) -0.003(7) C6_1 0.049(7) 0.061(7) 0.076(9) 0.005(6) 0.006(6) -0.011(5) C7_1 0.033(6) 0.061(8) 0.060(12) 0.005(8) 0.000(7) 0.001(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cl1 Al1 Cl2 108.33(11) . . ? Cl3 Al1 Cl1 108.08(11) . . ? Cl3 Al1 Cl2 109.56(12) . . ? Cl3 Al1 Cl4 111.82(11) . . ? Cl4 Al1 Cl1 110.15(11) . . ? Cl4 Al1 Cl2 108.83(10) . . ? C1 N1 C2 112.1(4) . . ? C1 N1 C4 127.5(5) . . ? C4 N1 C2 119.6(4) . . ? C1 N2 C3 111.8(4) . . ? C1 N2 C16 125.4(5) . . ? C16 N2 C3 122.1(4) . . ? N1 C1 N2 109.3(5) . . ? N1 C1 B1 126.3(6) . . ? N1 C1 B1' 129.6(6) . . ? N2 C1 B1 123.4(6) . . ? N2 C1 B1' 120.3(6) . . ? N1 C2 C3 102.6(4) . . ? N2 C3 C2 103.4(5) . . ? C5 C4 N1 117.6(5) . . ? C9 C4 N1 119.8(5) . . ? C9 C4 C5 122.5(5) . . ? C4 C5 C10 122.8(5) . . ? C6 C5 C4 116.7(5) . . ? C6 C5 C10 120.5(6) . . ? C5 C6 C7 122.2(6) . . ? C6 C7 C8 119.6(5) . . ? C7 C8 C9 121.1(5) . . ? C4 C9 C13 123.0(5) . . ? C8 C9 C4 117.9(5) . . ? C8 C9 C13 119.1(5) . . ? C5 C10 C11 111.6(6) . . ? C5 C10 C12 111.9(5) . . ? C11 C10 C12 108.8(5) . . ? C9 C13 C14 112.5(5) . . ? C9 C13 C15 110.3(5) . . ? C14 C13 C15 110.8(6) . . ? C17 C16 N2 118.0(5) . . ? C21 C16 N2 119.8(5) . . ? C21 C16 C17 122.2(5) . . ? C16 C17 C22 123.9(5) . . ? C18 C17 C16 117.6(5) . . ? C18 C17 C22 118.5(5) . . ? C19 C18 C17 121.4(6) . . ? C18 C19 C20 120.1(5) . . ? C21 C20 C19 120.7(5) . . ? C16 C21 C20 118.0(5) . . ? C16 C21 C25 123.3(5) . . ? C20 C21 C25 118.7(5) . . ? C17 C22 C23 112.8(5) . . ? C17 C22 C24 110.6(5) . . ? C24 C22 C23 110.2(5) . . ? C21 C25 C27 110.0(4) . . ? C26 C25 C21 112.6(4) . . ? C26 C25 C27 111.0(5) . . ? N3 B1 C1 115.7(9) . . ? C30 B1 C1 120.3(10) . . ? C30 B1 N3 94.6(9) . . ? C28 N3 B1 107.0(11) . . ? N3 C28 C29 120.5(12) . . ? N3 C28 C31 114.8(15) . . ? C31 C28 C29 123.8(14) . . ? C28 C29 C32 109.2(11) . . ? C30 C29 C28 100.3(10) . . ? C30 C29 C32 77.9(9) . . ? C29 C30 B1 117.5(10) . . ? O1 C32 C29 123.5(11) . . ? O1 C32 O2 123.8(12) . . ? O2 C32 C29 112.6(10) . . ? C32 O2 C33 116.2(10) . . ? O3' C34' O4' 124.0(14) . . ? C34' O4' C35' 119.2(17) . . ? C1 B1' C30' 123.3(9) . . ? N3' B1' C1 115.3(10) . . ? N3' B1' C30' 98.6(9) . . ? C28' N3' B1' 121.8(14) . . ? N3' C28' C29' 97.9(12) . . ? N3' C28' C31' 136.7(18) . . ? C31' C28' C29' 123.1(16) . . ? C28' C29' C34 118.4(11) . . ? C30' C29' C28' 120.3(11) . . ? C30' C29' C34 52.5(7) . . ? C29' C30' B1' 100.4(8) . . ? C29' C30' C34 84.5(9) . . ? C34 C30' B1' 111.5(8) . . ? O1' C32' O2' 124.3(11) . . ? C32' O2' C33' 115.7(11) . . ? C30' C34 C29' 43.0(5) . . ? O3 C34 C29' 149.6(8) . . ? O3 C34 C30' 124.1(9) . . ? O3 C34 O4 121.6(9) . . ? O4 C34 C29' 78.7(8) . . ? O4 C34 C30' 114.3(10) . . ? C34 O4 C35 117.2(11) . . ? C37 C36 C41 117.7(6) . . ? C37 C36 C42 121.0(7) . . ? C41 C36 C42 121.4(6) . . ? C38 C37 C36 121.3(6) . . ? C39 C38 C37 120.6(6) . . ? C40 C39 C38 120.1(7) . . ? C39 C40 C41 119.8(7) . . ? C36 C41 C40 120.5(6) . . ? C3_1 C2_1 C1_1 118.9(11) . . ? C7_1 C2_1 C1_1 122.6(11) . . ? C7_1 C2_1 C3_1 118.5(10) . . ? C4_1 C3_1 C2_1 120.1(12) . . ? C3_1 C4_1 C5_1 121.6(12) . . ? C6_1 C5_1 C4_1 118.2(12) . . ? C5_1 C6_1 C7_1 120.6(12) . . ? C2_1 C7_1 C6_1 120.9(12) . . ? 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 Cl1 Al1 2.131(2) . ? Cl2 Al1 2.133(3) . ? Cl3 Al1 2.122(3) . ? Cl4 Al1 2.127(2) . ? N1 C1 1.337(6) . ? N1 C2 1.481(7) . ? N1 C4 1.441(7) . ? N2 C1 1.348(7) . ? N2 C3 1.470(7) . ? N2 C16 1.447(6) . ? C1 B1 1.658(13) . ? C1 B1' 1.523(11) . ? C2 C3 1.516(8) . ? C4 C5 1.416(8) . ? C4 C9 1.392(7) . ? C5 C6 1.381(8) . ? C5 C10 1.498(8) . ? C6 C7 1.382(8) . ? C7 C8 1.386(8) . ? C8 C9 1.388(7) . ? C9 C13 1.511(8) . ? C10 C11 1.538(11) . ? C10 C12 1.544(8) . ? C13 C14 1.528(9) . ? C13 C15 1.538(8) . ? C16 C17 1.409(7) . ? C16 C21 1.393(8) . ? C17 C18 1.399(7) . ? C17 C22 1.520(8) . ? C18 C19 1.367(8) . ? C19 C20 1.401(8) . ? C20 C21 1.396(7) . ? C21 C25 1.516(7) . ? C22 C23 1.542(7) . ? C22 C24 1.527(9) . ? C25 C26 1.515(8) . ? C25 C27 1.546(7) . ? B1 N3 1.657(17) . ? B1 C30 1.632(17) . ? N3 C28 1.30(2) . ? C28 C29 1.50(2) . ? C28 C31 1.499(15) . ? C29 C30 1.367(15) . ? C29 C32 1.508(14) . ? O1 C32 1.224(18) . ? C32 O2 1.324(13) . ? O2 C33 1.477(19) . ? C34' O4' 1.301(17) . ? C34' O3' 1.189(18) . ? O4' C35' 1.44(4) . ? B1' N3' 1.497(14) . ? B1' C30' 1.592(14) . ? N3' C28' 1.23(2) . ? C28' C29' 1.51(2) . ? C28' C31' 1.494(15) . ? C29' C30' 1.316(14) . ? C29' C34 1.919(18) . ? C30' C34 1.528(11) . ? O1' C32' 1.230(17) . ? C32' O2' 1.321(14) . ? O2' C33' 1.399(18) . ? C34 O3 1.197(14) . ? C34 O4 1.327(13) . ? O4 C35 1.46(2) . ? C36 C37 1.377(9) . ? C36 C41 1.378(9) . ? C36 C42 1.511(9) . ? C37 C38 1.372(9) . ? C38 C39 1.357(9) . ? C39 C40 1.350(9) . ? C40 C41 1.409(9) . ? C1_1 C2_1 1.51(2) . ? C2_1 C3_1 1.382(12) . ? C2_1 C7_1 1.375(12) . ? C3_1 C4_1 1.372(13) . ? C4_1 C5_1 1.374(13) . ? C5_1 C6_1 1.373(14) . ? C6_1 C7_1 1.381(13) . ? 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 N1 C1 B1 N3 23.6(14) . . . . ? N1 C1 B1 C30 136.3(9) . . . . ? N1 C1 B1' N3' -7.8(15) . . . . ? N1 C1 B1' C30' 112.8(10) . . . . ? N1 C2 C3 N2 8.5(6) . . . . ? N1 C4 C5 C6 178.0(5) . . . . ? N1 C4 C5 C10 -0.3(8) . . . . ? N1 C4 C9 C8 -177.3(5) . . . . ? N1 C4 C9 C13 0.1(8) . . . . ? N2 C1 B1 N3 -169.1(8) . . . . ? N2 C1 B1 C30 -56.4(13) . . . . ? N2 C1 B1' N3' -176.2(9) . . . . ? N2 C1 B1' C30' -55.6(12) . . . . ? N2 C16 C17 C18 -178.5(5) . . . . ? N2 C16 C17 C22 4.3(8) . . . . ? N2 C16 C21 C20 178.0(4) . . . . ? N2 C16 C21 C25 -5.8(7) . . . . ? C1 N1 C2 C3 -7.8(6) . . . . ? C1 N1 C4 C5 79.3(7) . . . . ? C1 N1 C4 C9 -104.3(7) . . . . ? C1 N2 C3 C2 -7.3(6) . . . . ? C1 N2 C16 C17 110.7(6) . . . . ? C1 N2 C16 C21 -70.8(7) . . . . ? C1 B1 N3 C28 125.7(13) . . . . ? C1 B1 C30 C29 -120.9(12) . . . . ? C1 B1' N3' C28' 142.8(16) . . . . ? C1 B1' C30' C29' -136.3(10) . . . . ? C1 B1' C30' C34 -48.1(13) . . . . ? C2 N1 C1 N2 3.5(7) . . . . ? C2 N1 C1 B1 172.3(8) . . . . ? C2 N1 C1 B1' -165.9(8) . . . . ? C2 N1 C4 C5 -89.9(7) . . . . ? C2 N1 C4 C9 86.6(6) . . . . ? C3 N2 C1 N1 2.6(7) . . . . ? C3 N2 C1 B1 -166.6(8) . . . . ? C3 N2 C1 B1' 173.2(7) . . . . ? C3 N2 C16 C17 -79.6(6) . . . . ? C3 N2 C16 C21 98.8(6) . . . . ? C4 N1 C1 N2 -166.3(5) . . . . ? C4 N1 C1 B1 2.5(11) . . . . ? C4 N1 C1 B1' 24.3(11) . . . . ? C4 N1 C2 C3 163.0(5) . . . . ? C4 C5 C6 C7 -1.3(9) . . . . ? C4 C5 C10 C11 -117.0(7) . . . . ? C4 C5 C10 C12 120.9(6) . . . . ? C4 C9 C13 C14 127.1(6) . . . . ? C4 C9 C13 C15 -108.6(6) . . . . ? C5 C4 C9 C8 -1.0(8) . . . . ? C5 C4 C9 C13 176.4(5) . . . . ? C5 C6 C7 C8 0.4(10) . . . . ? C6 C5 C10 C11 64.8(7) . . . . ? C6 C5 C10 C12 -57.4(9) . . . . ? C6 C7 C8 C9 0.3(9) . . . . ? C7 C8 C9 C4 0.0(8) . . . . ? C7 C8 C9 C13 -177.5(5) . . . . ? C8 C9 C13 C14 -55.4(7) . . . . ? C8 C9 C13 C15 68.8(7) . . . . ? C9 C4 C5 C6 1.7(9) . . . . ? C9 C4 C5 C10 -176.7(6) . . . . ? C10 C5 C6 C7 177.0(6) . . . . ? C16 N2 C1 N1 173.2(5) . . . . ? C16 N2 C1 B1 4.0(10) . . . . ? C16 N2 C1 B1' -16.3(10) . . . . ? C16 N2 C3 C2 -178.2(5) . . . . ? C16 C17 C18 C19 -0.1(8) . . . . ? C16 C17 C22 C23 -130.6(6) . . . . ? C16 C17 C22 C24 105.4(6) . . . . ? C16 C21 C25 C26 140.1(5) . . . . ? C16 C21 C25 C27 -95.6(6) . . . . ? C17 C16 C21 C20 -3.6(7) . . . . ? C17 C16 C21 C25 172.6(5) . . . . ? C17 C18 C19 C20 -2.3(8) . . . . ? C18 C17 C22 C23 52.2(7) . . . . ? C18 C17 C22 C24 -71.7(6) . . . . ? C18 C19 C20 C21 1.7(8) . . . . ? C19 C20 C21 C16 1.2(8) . . . . ? C19 C20 C21 C25 -175.3(5) . . . . ? C20 C21 C25 C26 -43.7(6) . . . . ? C20 C21 C25 C27 80.7(6) . . . . ? C21 C16 C17 C18 3.1(8) . . . . ? C21 C16 C17 C22 -174.1(5) . . . . ? C22 C17 C18 C19 177.3(5) . . . . ? B1 N3 C28 C29 0(2) . . . . ? B1 N3 C28 C31 169.5(12) . . . . ? N3 B1 C30 C29 2.6(14) . . . . ? N3 C28 C29 C30 1.8(19) . . . . ? N3 C28 C29 C32 82.5(17) . . . . ? C28 C29 C30 B1 -2.7(15) . . . . ? C28 C29 C32 O1 30.2(17) . . . . ? C28 C29 C32 O2 -152.8(10) . . . . ? C29 C32 O2 C33 -178.2(10) . . . . ? C30 B1 N3 C28 -1.2(14) . . . . ? C30 C29 C32 O1 127.1(14) . . . . ? C30 C29 C32 O2 -56.0(10) . . . . ? O1 C32 O2 C33 -1.3(18) . . . . ? C31 C28 C29 C30 -166.9(15) . . . . ? C31 C28 C29 C32 -86.3(17) . . . . ? C32 C29 C30 B1 -110.3(12) . . . . ? O3' C34' O4' C35' 1(3) . . . . ? B1' N3' C28' C29' -6(2) . . . . ? B1' N3' C28' C31' -168(2) . . . . ? B1' C30' C34 C29' -99.1(9) . . . . ? B1' C30' C34 O3 44.3(13) . . . . ? B1' C30' C34 O4 -136.0(8) . . . . ? N3' B1' C30' C29' -8.2(12) . . . . ? N3' B1' C30' C34 80.0(11) . . . . ? N3' C28' C29' C30' -2(2) . . . . ? N3' C28' C29' C34 -62.4(16) . . . . ? C28' C29' C30' B1' 6.7(15) . . . . ? C28' C29' C30' C34 -104.2(13) . . . . ? C29' C30' C34 O3 143.3(10) . . . . ? C29' C30' C34 O4 -37.0(10) . . . . ? C29' C34 O4 C35 160.4(12) . . . . ? C30' B1' N3' C28' 9.5(19) . . . . ? C30' C34 O4 C35 -174.8(12) . . . . ? O1' C32' O2' C33' 4.4(18) . . . . ? C31' C28' C29' C30' 164.1(14) . . . . ? C31' C28' C29' C34 103.2(17) . . . . ? C34 C29' C30' B1' 110.9(8) . . . . ? O3 C34 O4 C35 4.9(16) . . . . ? C36 C37 C38 C39 0.5(10) . . . . ? C37 C36 C41 C40 -0.7(10) . . . . ? C37 C38 C39 C40 0.0(10) . . . . ? C38 C39 C40 C41 -0.9(10) . . . . ? C39 C40 C41 C36 1.2(10) . . . . ? C41 C36 C37 C38 -0.2(10) . . . . ? C42 C36 C37 C38 -179.8(6) . . . . ? C42 C36 C41 C40 178.9(6) . . . . ? C1_1 C2_1 C3_1 C4_1 -179.4(16) . . . . ? C1_1 C2_1 C7_1 C6_1 179.7(17) . . . . ? C2_1 C3_1 C4_1 C5_1 -2(3) . . . . ? C3_1 C2_1 C7_1 C6_1 -1(3) . . . . ? C3_1 C4_1 C5_1 C6_1 3(3) . . . . ? C4_1 C5_1 C6_1 C7_1 -3(3) . . . . ? C5_1 C6_1 C7_1 C2_1 2(3) . . . . ? C7_1 C2_1 C3_1 C4_1 1(3) . . . . ?