#------------------------------------------------------------------------------ #$Date: 2020-10-06 10:16:49 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257341 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557999.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_1557999 loop_ _publ_author_name 'Eichenberger, Sarah' 'H\"onig, Moritz' 'Richter, Matthieu J. R.' 'Gershoni-Poranne, Renana' 'Carreira, Erick M.' _publ_section_title ; Ring-fused cyclobutanes via cycloisomerization of alkylidenecyclopropane acylsilanes ; _journal_issue 20 _journal_name_full 'Chemical Science' _journal_page_first 5294 _journal_page_last 5298 _journal_paper_doi 10.1039/D0SC02224A _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C28 H30 Br N O2 Si, C3 H7' _chemical_formula_sum 'C31 H37 Br N O2 Si' _chemical_formula_weight 563.61 _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 2019-07-01 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-04-17 deposited with the CCDC. 2020-05-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.5460(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.00200(10) _cell_length_b 8.35050(10) _cell_length_c 18.65040(10) _cell_measurement_reflns_used 57270 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 79.3500 _cell_measurement_theta_min 2.4230 _cell_volume 2836.83(4) _computing_cell_refinement 'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.42a (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 100.0(1) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.8140 _diffrn_detector_type 'Pilatus 300K' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.986 _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 1.00 33.00 0.50 0.17 -- 34.00 96.00 116.03 64 2 \w 29.00 120.00 0.50 0.17 -- 54.00 81.00 101.51 182 3 \w 120.00 175.00 0.50 0.68 -- 110.00 77.00 120.00 110 4 \w 131.00 168.00 0.50 0.68 -- 110.00 77.00 60.00 74 5 \w 118.00 175.00 0.50 0.68 -- 110.00 77.00 150.00 114 6 \w 121.00 175.00 0.50 0.68 -- 110.00 77.00 30.00 108 7 \w 120.00 176.00 0.50 0.68 -- 110.00 77.00 0.00 112 8 \w 125.00 176.00 0.50 0.68 -- 110.00 77.00 -30.00 102 9 \w 97.00 147.00 0.50 0.68 -- 110.00 56.00 -17.60 100 10 \w 94.00 138.00 0.50 0.68 -- 110.00 57.00 -60.00 88 11 \w 97.00 127.00 0.50 0.68 -- 110.00 57.00 -30.00 60 12 \w 97.00 178.00 0.50 0.68 -- 110.00 57.00 -90.00 162 13 \w 99.00 126.00 0.50 0.68 -- 110.00 57.00-150.00 54 14 \w 98.00 151.00 0.50 0.68 -- 110.00 38.00-180.00 106 15 \w 94.00 122.00 0.50 0.68 -- 110.00 57.00-120.00 56 16 \w 100.00 126.00 0.50 0.68 -- 110.00 38.00-150.00 52 17 \w 86.00 175.00 0.50 0.68 -- 110.00 77.00-180.00 178 18 \w 88.00 176.00 0.50 0.68 -- 110.00 77.00 -60.00 176 19 \w 95.00 149.00 0.50 0.68 -- 110.00 57.00 60.00 108 20 \w 98.00 126.00 0.50 0.68 -- 110.00 38.00 150.00 56 21 \w 98.00 145.00 0.50 0.68 -- 110.00 38.00 120.00 94 22 \w 94.00 134.00 0.50 0.68 -- 110.00 57.00 30.00 80 23 \w 86.00 114.00 0.50 0.68 -- 110.00 77.00 120.00 56 24 \w 86.00 171.00 0.50 0.68 -- 110.00 77.00 90.00 170 25 \w 86.00 112.00 0.50 0.68 -- 110.00 77.00 150.00 52 26 \w 86.00 116.00 0.50 0.68 -- 110.00 77.00 60.00 60 27 \w 86.00 114.00 0.50 0.68 -- 110.00 77.00 0.00 56 28 \w 86.00 112.00 0.50 0.68 -- 110.00 77.00 -30.00 52 29 \w 87.00 113.00 0.50 0.68 -- 110.00 77.00 30.00 52 30 \w 59.00 88.00 0.50 0.17 -- 78.00 66.00 29.61 58 31 \w 34.00 121.00 0.50 0.17 -- 49.37 57.00 -60.00 174 32 \w 62.00 98.00 0.50 0.68 -- 86.00 79.00 -65.63 72 33 \w 86.00 174.00 0.50 0.68 -- 110.00 77.00-120.00 176 34 \w 86.00 176.00 0.50 0.68 -- 110.00 77.00-150.00 180 35 \w 70.00 96.00 0.50 0.68 -- 110.00 -99.00-120.00 52 36 \w 61.00 102.00 0.50 0.68 -- 110.00-125.00 -90.00 82 37 \w 83.00 108.00 0.50 0.68 -- 110.00 -99.00 -30.00 50 38 \w 79.00 110.00 0.50 0.68 -- 110.00 -99.00 60.00 62 39 \w 79.00 110.00 0.50 0.68 -- 110.00 -99.00 150.00 62 40 \w 57.00 122.00 0.50 0.17 -- 49.37-178.00 120.00 130 41 \w 44.00 97.00 0.50 0.68 -- 110.00 -99.00 0.00 106 42 \w 48.00 76.00 0.50 0.68 -- 110.00 -99.00 -30.00 56 43 \w 45.00 92.00 0.50 0.68 -- 110.00 -99.00 -60.00 94 44 \w 41.00 90.00 0.50 0.68 -- 110.00 -99.00-180.00 98 45 \w 37.00 125.00 0.50 0.17 -- 49.37 38.00 -60.00 176 46 \w 34.00 121.00 0.50 0.17 -- 49.37 57.00 0.00 174 47 \w 34.00 121.00 0.50 0.17 -- 49.37 57.00 30.00 174 48 \w 37.00 125.00 0.50 0.17 -- 49.37 38.00-120.00 176 49 \w 30.00 120.00 0.50 0.17 -- 54.00 79.00 44.96 180 50 \w 25.00 116.00 0.50 0.17 -- 50.00 80.00-107.59 182 51 \w 29.00 120.00 0.50 0.17 -- 54.00 80.00 -28.26 182 52 \w 20.00 46.00 0.50 0.17 -- 50.00 90.00 -73.30 52 53 \w -74.00 18.00 0.50 0.17 -- -38.00 102.00 129.21 184 54 \w 28.00 121.00 0.50 0.17 -- 54.00 82.00 165.28 186 55 \w 45.00 75.00 0.50 0.68 -- 110.00 -99.00 60.00 60 56 \w 50.00 95.00 0.50 0.68 -- 110.00 -99.00 90.00 90 57 \w 46.00 73.00 0.50 0.68 -- 110.00 -99.00 150.00 54 58 \w -93.00 -25.00 0.50 0.17 -- -26.00 156.00 175.55 136 59 \w -67.00 2.00 0.50 0.68 -- -70.00 57.00 30.00 138 60 \w -92.00 -24.00 0.50 0.17 -- -26.00 154.00 108.86 136 61 \w -125.00 -37.00 0.50 0.17 -- -49.87 -38.00 -90.00 176 62 \w -72.00 -44.00 0.50 0.68 -- -70.00 -82.00 -33.15 56 63 \w -71.00 -46.00 0.50 0.68 -- -70.00 -77.00 -90.00 50 64 \w -70.00 -43.00 0.50 0.68 -- -70.00 -83.00 -97.07 54 65 \w -76.00 -46.00 0.50 0.68 -- -70.00 -77.00 0.00 60 66 \w -72.00 -46.00 0.50 0.68 -- -70.00 -77.00 30.00 52 67 \w -77.00 -46.00 0.50 0.68 -- -70.00 -77.00 90.00 62 68 \w -81.00 -51.00 0.50 0.68 -- -70.00 -66.00 162.40 60 69 \w -92.00 -46.00 0.50 0.68 -- -70.00 -80.00 168.81 92 70 \w -85.00 -51.00 0.50 0.68 -- -70.00 -66.00 97.05 68 71 \w -96.00 -50.00 0.50 0.68 -- -70.00 -67.00 124.65 92 72 \w -133.00-102.00 0.50 0.68 -- -70.00 -66.00 97.05 62 73 \w -136.00 -46.00 0.50 0.68 -- -70.00 -77.00 60.00 180 74 \w -127.00-101.00 0.50 0.68 -- -70.00 -83.00 -97.07 52 75 \w -89.00 -47.00 0.50 0.68 -- -70.00 -75.00-159.21 84 76 \w -125.00 -37.00 0.50 0.17 -- -49.87 -38.00-180.00 176 77 \w -136.00 -47.00 0.50 0.68 -- -70.00 -74.00 -74.92 178 78 \w -136.00 -47.00 0.50 0.68 -- -70.00 -76.00-130.42 178 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 300K' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0064746000 _diffrn_orient_matrix_UB_12 -0.0009342000 _diffrn_orient_matrix_UB_13 0.0804840000 _diffrn_orient_matrix_UB_21 -0.0842810000 _diffrn_orient_matrix_UB_22 -0.0051905000 _diffrn_orient_matrix_UB_23 -0.0307914000 _diffrn_orient_matrix_UB_31 0.0024470000 _diffrn_orient_matrix_UB_32 -0.1844264000 _diffrn_orient_matrix_UB_33 0.0004909000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_unetI/netI 0.0173 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 84976 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 79.771 _diffrn_reflns_theta_min 2.426 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.589 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.640 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.42a (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 colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.320 _exptl_crystal_description plank _exptl_crystal_F_000 1180 _exptl_crystal_size_max 0.225 _exptl_crystal_size_mid 0.082 _exptl_crystal_size_min 0.042 _refine_diff_density_max 0.538 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.058 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 331 _refine_ls_number_reflns 6092 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0347 _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^)+(0.0445P)^2^+2.4260P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0922 _refine_ls_wR_factor_ref 0.0933 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5761 _reflns_number_total 6092 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc02224a2.cif _cod_data_source_block ca230619_2_1 _cod_depositor_comments ;Adding full bibliography for 1557999.cif. Adding full bibliography for 1557999.cif. ; _cod_database_code 1557999 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C28H30BrNO2Si _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. ; _diffrn_oxdiff_digest_frames ; 0189204a43a5b5c0d87bd6a43b39bdbed808198dade ; _diffrn_oxdiff_digest_hkl ; 01c4f1d5028d6304c763d8cf878e0ea407a937 ; _reflns_odcompleteness_completeness 100.00 _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, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances N1-H1 0.93 with sigma of 0.02 3.a Ternary CH refined with riding coordinates: C8(H8) 3.b Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C17(H17A,H17B), C2A(H2AA, H2AB), C3A(H3AA,H3AB) 3.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28) 3.d Idealised Me refined as rotating group: C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C1A(H1AA,H1AB,H1AC) ; _shelx_res_file ; TITL ca230619_2_1_a.res in P2(1)/c ca230619_2_1.res created by SHELXL-2018/3 at 10:16:52 on 01-Jul-2019 REM Old TITL ca230619_2_1 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.113, Rweak 0.011, Alpha 0.031, Orientation as input REM Formula found by SHELXT: C31 N O2 Si Br CELL 1.54184 19.002 8.3505 18.6504 90 106.546 90 ZERR 4 0.0001 0.0001 0.0001 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Br N O Si UNIT 124 148 4 4 8 4 DFIX 0.93 N1 H1 L.S. 8 PLAN 20 BOND $H list 4 fmap 2 acta OMIT -18 7 2 REM REM REM WGHT 0.044500 2.426000 FVAR 0.43503 BR1 3 0.183213 0.049180 0.486365 11.00000 0.03302 0.04019 = 0.04379 -0.00515 0.00831 -0.00894 SI1 6 0.706551 0.184989 0.774540 11.00000 0.02076 0.01897 = 0.02481 0.00159 0.00835 0.00009 O1 5 0.562270 0.174967 0.567276 11.00000 0.03083 0.03272 = 0.02911 -0.00265 0.01086 0.00895 O2 5 0.602165 0.409223 0.627313 11.00000 0.02140 0.02806 = 0.03599 0.00193 0.00727 0.00471 N1 4 0.483413 0.363906 0.590088 11.00000 0.02433 0.02239 = 0.03028 -0.00444 0.00676 0.00381 H1 2 0.484120 0.454414 0.615525 11.00000 -1.20000 C1 1 0.278065 0.145118 0.518904 11.00000 0.02789 0.02466 = 0.02536 0.00243 0.00463 -0.00119 C2 1 0.290230 0.267028 0.571155 11.00000 0.02812 0.02909 = 0.02669 -0.00040 0.01049 0.00303 AFIX 43 H2 2 0.252768 0.301950 0.590341 11.00000 -1.20000 AFIX 0 C3 1 0.333181 0.091139 0.490122 11.00000 0.03634 0.02144 = 0.02231 -0.00149 0.00721 0.00170 AFIX 43 H3 2 0.324046 0.008024 0.455502 11.00000 -1.20000 AFIX 0 C4 1 0.359263 0.336168 0.594387 11.00000 0.02961 0.02606 = 0.02303 -0.00377 0.00739 0.00411 AFIX 43 H4 2 0.368316 0.417849 0.629737 11.00000 -1.20000 AFIX 0 C5 1 0.402079 0.161058 0.512931 11.00000 0.03124 0.02441 = 0.02239 0.00100 0.00934 0.00562 AFIX 43 H5 2 0.439207 0.125679 0.493362 11.00000 -1.20000 AFIX 0 C6 1 0.415523 0.284356 0.565203 11.00000 0.02587 0.02158 = 0.02095 0.00193 0.00549 0.00448 C7 1 0.550412 0.303291 0.592062 11.00000 0.02602 0.02703 = 0.02049 0.00422 0.00744 0.00613 C8 1 0.678582 0.369514 0.636099 11.00000 0.02172 0.03610 = 0.03491 0.01159 0.01187 0.00749 AFIX 13 H8 2 0.681993 0.266086 0.612482 11.00000 -1.20000 AFIX 0 C9 1 0.722500 0.364557 0.718945 11.00000 0.01969 0.02321 = 0.03619 0.00518 0.01025 -0.00017 C10 1 0.714175 0.499957 0.600997 11.00000 0.03342 0.05901 = 0.05468 0.03347 0.01764 0.00884 AFIX 23 H10A 2 0.700048 0.605824 0.613265 11.00000 -1.20000 H10B 2 0.701284 0.488571 0.547053 11.00000 -1.20000 AFIX 0 C11 1 0.717508 0.524199 0.761250 11.00000 0.02614 0.01986 = 0.05241 0.00142 0.00754 -0.00277 AFIX 23 H11A 2 0.684993 0.602936 0.730515 11.00000 -1.20000 H11B 2 0.705855 0.508227 0.808112 11.00000 -1.20000 AFIX 0 C12 1 0.803776 0.416425 0.718790 11.00000 0.02120 0.03514 = 0.05319 0.01671 0.01351 -0.00051 C13 1 0.796068 0.469439 0.636985 11.00000 0.03059 0.06462 = 0.06520 0.03986 0.02117 0.00585 AFIX 23 H13A 2 0.824157 0.566162 0.636365 11.00000 -1.20000 H13B 2 0.813663 0.386032 0.610230 11.00000 -1.20000 AFIX 0 C14 1 0.615544 0.211786 0.795229 11.00000 0.02417 0.01781 = 0.02365 0.00226 0.00939 -0.00078 C15 1 0.700838 -0.010266 0.723757 11.00000 0.03202 0.02327 = 0.03661 -0.00191 0.01570 0.00236 AFIX 137 H15A 2 0.686789 -0.093461 0.752448 11.00000 -1.50000 H15B 2 0.747846 -0.035206 0.716976 11.00000 -1.50000 H15C 2 0.664952 -0.002201 0.675820 11.00000 -1.50000 AFIX 0 C16 1 0.779412 0.174618 0.866554 11.00000 0.02599 0.03565 = 0.03118 0.00398 0.00560 -0.00149 AFIX 137 H16A 2 0.790031 0.280600 0.886672 11.00000 -1.50000 H16B 2 0.823113 0.128155 0.859357 11.00000 -1.50000 H16C 2 0.762396 0.109789 0.900742 11.00000 -1.50000 AFIX 0 C17 1 0.799528 0.557900 0.771178 11.00000 0.02861 0.02737 = 0.07942 0.00665 0.00947 -0.00620 AFIX 23 H17A 2 0.830126 0.543409 0.822126 11.00000 -1.20000 H17B 2 0.808593 0.661348 0.751870 11.00000 -1.20000 AFIX 0 C18 1 0.866224 0.298106 0.744901 11.00000 0.02234 0.04509 = 0.04793 0.01997 0.01626 0.00340 C19 1 0.550885 0.143940 0.749353 11.00000 0.02619 0.01987 = 0.02176 0.00099 0.00794 -0.00119 AFIX 43 H19 2 0.552358 0.089996 0.706179 11.00000 -1.20000 AFIX 0 C20 1 0.610773 0.291246 0.859934 11.00000 0.02756 0.02431 = 0.02678 -0.00380 0.00915 -0.00431 AFIX 43 H20 2 0.652783 0.337046 0.891682 11.00000 -1.20000 AFIX 0 C21 1 0.863299 0.152255 0.707654 11.00000 0.03113 0.05581 = 0.04229 0.00950 0.01974 0.01149 AFIX 43 H21 2 0.823362 0.130229 0.666606 11.00000 -1.20000 AFIX 0 C22 1 0.927745 0.329062 0.804672 11.00000 0.02526 0.05000 = 0.06136 0.01508 0.01229 -0.00277 AFIX 43 H22 2 0.931560 0.425799 0.830205 11.00000 -1.20000 AFIX 0 C23 1 0.484503 0.155208 0.766743 11.00000 0.02213 0.02463 = 0.02858 0.00305 0.00661 -0.00104 AFIX 43 H23 2 0.442294 0.109469 0.735320 11.00000 -1.20000 AFIX 0 C24 1 0.544572 0.303174 0.877761 11.00000 0.03458 0.02274 = 0.02956 -0.00353 0.01579 -0.00173 AFIX 43 H24 2 0.542698 0.356833 0.920875 11.00000 -1.20000 AFIX 0 C25 1 0.918819 0.039324 0.730643 11.00000 0.04411 0.06467 = 0.05333 0.01049 0.02755 0.02252 AFIX 43 H25 2 0.915157 -0.058297 0.705847 11.00000 -1.20000 AFIX 0 C26 1 0.983958 0.215481 0.826631 11.00000 0.02204 0.07508 = 0.05869 0.02730 0.01096 0.00371 AFIX 43 H26 2 1.024976 0.237829 0.866488 11.00000 -1.20000 AFIX 0 C27 1 0.481496 0.235010 0.831197 11.00000 0.02648 0.02227 = 0.03546 0.00472 0.01570 0.00272 AFIX 43 H27 2 0.437279 0.242665 0.843062 11.00000 -1.20000 AFIX 0 C28 1 0.979280 0.071602 0.790077 11.00000 0.03581 0.06815 = 0.06003 0.02386 0.02517 0.02259 AFIX 43 H28 2 1.016671 -0.003593 0.805326 11.00000 -1.20000 AFIX 0 C1A 1 0.995734 0.667214 0.921745 11.00000 0.05887 0.11242 = 0.07428 0.00912 0.00996 -0.00004 AFIX 137 H1AA 2 0.971517 0.705633 0.872360 11.00000 -1.50000 H1AB 2 0.960085 0.622162 0.943501 11.00000 -1.50000 H1AC 2 1.030874 0.586583 0.918966 11.00000 -1.50000 AFIX 0 C2A 1 1.033978 0.802185 0.968775 11.00000 0.04651 0.12051 = 0.05826 0.01729 0.00554 0.00110 AFIX 23 H2AA 2 1.069014 0.849008 0.945856 11.00000 -1.20000 H2AB 2 1.061081 0.761464 1.017528 11.00000 -1.20000 AFIX 0 C3A 1 0.981290 0.930967 0.978650 11.00000 0.04756 0.12533 = 0.05031 0.03369 0.01694 0.01388 AFIX 23 H3AA 2 0.952156 0.966987 0.929758 11.00000 -1.20000 H3AB 2 0.948054 0.885346 1.004136 11.00000 -1.20000 AFIX 0 HKLF 4 REM ca230619_2_1_a.res in P2(1)/c REM wR2 = 0.0933, GooF = S = 1.044, Restrained GooF = 1.045 for all data REM R1 = 0.0347 for 5761 Fo > 4sig(Fo) and 0.0362 for all 6092 data REM 331 parameters refined using 1 restraints END WGHT 0.0445 2.4266 REM Highest difference peak 0.538, deepest hole -0.645, 1-sigma level 0.058 Q1 1 0.9109 0.8629 0.9418 11.00000 0.05 0.54 Q2 1 0.9211 0.9907 1.0079 11.00000 0.05 0.42 Q3 1 1.0920 0.9165 0.9670 11.00000 0.05 0.38 Q4 1 0.6490 0.2034 0.7832 11.00000 0.05 0.36 Q5 1 1.0410 0.9140 0.9942 11.00000 0.05 0.35 Q6 1 0.7459 0.1743 0.8333 11.00000 0.05 0.31 Q7 1 0.1897 0.0749 0.4477 11.00000 0.05 0.30 Q8 1 0.9808 0.7616 0.9475 11.00000 0.05 0.29 Q9 1 0.5192 0.1306 0.7684 11.00000 0.05 0.29 Q10 1 0.6978 0.3566 0.6820 11.00000 0.05 0.28 Q11 1 0.8003 0.4343 0.6808 11.00000 0.05 0.27 Q12 1 0.6109 0.2306 0.8285 11.00000 0.05 0.27 Q13 1 0.9881 0.7139 0.9718 11.00000 0.05 0.27 Q14 1 0.7024 0.0661 0.7477 11.00000 0.05 0.26 Q15 1 0.2493 0.1137 0.5073 11.00000 0.05 0.26 Q16 1 0.7632 0.3781 0.7190 11.00000 0.05 0.26 Q17 1 0.2998 0.1162 0.4953 11.00000 0.05 0.24 Q18 1 0.7125 0.2854 0.7415 11.00000 0.05 0.24 Q19 1 0.8323 0.3618 0.7346 11.00000 0.05 0.23 Q20 1 0.4841 0.2046 0.7958 11.00000 0.05 0.23 ; _shelx_res_checksum 91928 _olex2_date_sample_data_collection 2019-06-28 _olex2_date_sample_submission 2019-06-27 _olex2_submission_original_sample_id ca230619_2_1 _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 - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.485 _oxdiff_exptl_absorpt_empirical_full_min 0.703 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.18321(2) 0.04918(3) 0.48636(2) 0.03955(8) Uani 1 1 d . . . . . Si1 Si 0.70655(2) 0.18499(5) 0.77454(2) 0.02113(10) Uani 1 1 d . . . . . O1 O 0.56227(7) 0.17497(16) 0.56728(7) 0.0304(3) Uani 1 1 d . . . . . O2 O 0.60216(7) 0.40922(16) 0.62731(7) 0.0287(3) Uani 1 1 d . . . . . N1 N 0.48341(8) 0.36391(18) 0.59009(8) 0.0259(3) Uani 1 1 d D . . . . H1 H 0.4841(13) 0.454(2) 0.6155(12) 0.031 Uiso 1 1 d DR . . . . C1 C 0.27806(10) 0.1451(2) 0.51890(10) 0.0266(3) Uani 1 1 d . . . . . C2 C 0.29023(10) 0.2670(2) 0.57115(10) 0.0274(4) Uani 1 1 d . . . . . H2 H 0.252768 0.301950 0.590341 0.033 Uiso 1 1 calc R . . . . C3 C 0.33318(10) 0.0911(2) 0.49012(9) 0.0269(4) Uani 1 1 d . . . . . H3 H 0.324046 0.008024 0.455502 0.032 Uiso 1 1 calc R . . . . C4 C 0.35926(10) 0.3362(2) 0.59439(9) 0.0263(3) Uani 1 1 d . . . . . H4 H 0.368316 0.417849 0.629737 0.032 Uiso 1 1 calc R . . . . C5 C 0.40208(10) 0.1611(2) 0.51293(9) 0.0257(3) Uani 1 1 d . . . . . H5 H 0.439207 0.125679 0.493362 0.031 Uiso 1 1 calc R . . . . C6 C 0.41552(9) 0.2844(2) 0.56520(9) 0.0230(3) Uani 1 1 d . . . . . C7 C 0.55041(9) 0.3033(2) 0.59206(9) 0.0243(3) Uani 1 1 d . . . . . C8 C 0.67858(9) 0.3695(2) 0.63610(11) 0.0301(4) Uani 1 1 d . . . . . H8 H 0.681993 0.266086 0.612482 0.036 Uiso 1 1 calc R . . . . C9 C 0.72250(9) 0.3646(2) 0.71894(10) 0.0259(3) Uani 1 1 d . . . . . C10 C 0.71417(12) 0.5000(3) 0.60100(14) 0.0480(6) Uani 1 1 d . . . . . H10A H 0.700048 0.605824 0.613265 0.058 Uiso 1 1 calc R . . . . H10B H 0.701284 0.488571 0.547053 0.058 Uiso 1 1 calc R . . . . C11 C 0.71751(10) 0.5242(2) 0.76125(13) 0.0336(4) Uani 1 1 d . . . . . H11A H 0.684993 0.602936 0.730515 0.040 Uiso 1 1 calc R . . . . H11B H 0.705855 0.508227 0.808112 0.040 Uiso 1 1 calc R . . . . C12 C 0.80378(10) 0.4164(3) 0.71879(13) 0.0359(4) Uani 1 1 d . . . . . C13 C 0.79607(12) 0.4694(3) 0.63698(15) 0.0519(7) Uani 1 1 d . . . . . H13A H 0.824157 0.566162 0.636365 0.062 Uiso 1 1 calc R . . . . H13B H 0.813663 0.386032 0.610230 0.062 Uiso 1 1 calc R . . . . C14 C 0.61554(9) 0.21179(19) 0.79523(9) 0.0213(3) Uani 1 1 d . . . . . C15 C 0.70084(10) -0.0103(2) 0.72376(11) 0.0294(4) Uani 1 1 d . . . . . H15A H 0.686789 -0.093461 0.752448 0.044 Uiso 1 1 calc GR . . . . H15B H 0.747846 -0.035206 0.716976 0.044 Uiso 1 1 calc GR . . . . H15C H 0.664952 -0.002201 0.675820 0.044 Uiso 1 1 calc GR . . . . C16 C 0.77941(10) 0.1746(2) 0.86655(10) 0.0315(4) Uani 1 1 d . . . . . H16A H 0.790031 0.280600 0.886672 0.047 Uiso 1 1 calc GR . . . . H16B H 0.823113 0.128155 0.859357 0.047 Uiso 1 1 calc GR . . . . H16C H 0.762396 0.109789 0.900742 0.047 Uiso 1 1 calc GR . . . . C17 C 0.79953(12) 0.5579(3) 0.77118(16) 0.0464(6) Uani 1 1 d . . . . . H17A H 0.830126 0.543409 0.822126 0.056 Uiso 1 1 calc R . . . . H17B H 0.808593 0.661348 0.751870 0.056 Uiso 1 1 calc R . . . . C18 C 0.86622(10) 0.2981(3) 0.74490(12) 0.0372(5) Uani 1 1 d . . . . . C19 C 0.55089(9) 0.1439(2) 0.74935(9) 0.0224(3) Uani 1 1 d . . . . . H19 H 0.552358 0.089996 0.706179 0.027 Uiso 1 1 calc R . . . . C20 C 0.61077(10) 0.2912(2) 0.85993(10) 0.0259(3) Uani 1 1 d . . . . . H20 H 0.652783 0.337046 0.891682 0.031 Uiso 1 1 calc R . . . . C21 C 0.86330(12) 0.1523(3) 0.70765(12) 0.0412(5) Uani 1 1 d . . . . . H21 H 0.823362 0.130229 0.666606 0.049 Uiso 1 1 calc R . . . . C22 C 0.92774(11) 0.3291(3) 0.80467(14) 0.0455(5) Uani 1 1 d . . . . . H22 H 0.931560 0.425799 0.830205 0.055 Uiso 1 1 calc R . . . . C23 C 0.48450(9) 0.1552(2) 0.76674(10) 0.0252(3) Uani 1 1 d . . . . . H23 H 0.442294 0.109469 0.735320 0.030 Uiso 1 1 calc R . . . . C24 C 0.54457(10) 0.3032(2) 0.87776(10) 0.0276(4) Uani 1 1 d . . . . . H24 H 0.542698 0.356833 0.920875 0.033 Uiso 1 1 calc R . . . . C25 C 0.91882(14) 0.0393(3) 0.73064(15) 0.0512(6) Uani 1 1 d . . . . . H25 H 0.915157 -0.058297 0.705847 0.061 Uiso 1 1 calc R . . . . C26 C 0.98396(11) 0.2155(4) 0.82663(15) 0.0521(7) Uani 1 1 d . . . . . H26 H 1.024976 0.237829 0.866488 0.062 Uiso 1 1 calc R . . . . C27 C 0.48150(10) 0.2350(2) 0.83120(10) 0.0266(3) Uani 1 1 d . . . . . H27 H 0.437279 0.242665 0.843062 0.032 Uiso 1 1 calc R . . . . C28 C 0.97928(13) 0.0716(3) 0.79008(15) 0.0523(7) Uani 1 1 d . . . . . H28 H 1.016671 -0.003593 0.805326 0.063 Uiso 1 1 calc R . . . . C1A C 0.99573(19) 0.6672(5) 0.9217(2) 0.0837(10) Uani 1 1 d . . . . . H1AA H 0.971517 0.705633 0.872360 0.126 Uiso 1 1 calc GR . . . . H1AB H 0.960085 0.622162 0.943501 0.126 Uiso 1 1 calc GR . . . . H1AC H 1.030874 0.586583 0.918966 0.126 Uiso 1 1 calc GR . . . . C2A C 1.03398(16) 0.8022(5) 0.96877(18) 0.0770(10) Uani 1 1 d . . . . . H2AA H 1.069014 0.849008 0.945856 0.092 Uiso 1 1 calc R . . . . H2AB H 1.061081 0.761464 1.017528 0.092 Uiso 1 1 calc R . . . . C3A C 0.98129(16) 0.9310(5) 0.97865(16) 0.0738(10) Uani 1 1 d . . . . . H3AA H 0.952156 0.966987 0.929758 0.089 Uiso 1 1 calc R . . . . H3AB H 0.948054 0.885346 1.004136 0.089 Uiso 1 1 calc R . . . . 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 Br1 0.03302(12) 0.04019(14) 0.04379(14) -0.00515(9) 0.00831(9) -0.00894(8) Si1 0.0208(2) 0.0190(2) 0.0248(2) 0.00159(16) 0.00835(17) 0.00009(16) O1 0.0308(6) 0.0327(7) 0.0291(6) -0.0027(5) 0.0109(5) 0.0090(5) O2 0.0214(6) 0.0281(6) 0.0360(7) 0.0019(5) 0.0073(5) 0.0047(5) N1 0.0243(7) 0.0224(7) 0.0303(7) -0.0044(6) 0.0068(6) 0.0038(6) C1 0.0279(8) 0.0247(9) 0.0254(8) 0.0024(7) 0.0046(7) -0.0012(7) C2 0.0281(8) 0.0291(9) 0.0267(8) -0.0004(7) 0.0105(7) 0.0030(7) C3 0.0363(9) 0.0214(8) 0.0223(8) -0.0015(6) 0.0072(7) 0.0017(7) C4 0.0296(9) 0.0261(9) 0.0230(8) -0.0038(6) 0.0074(7) 0.0041(7) C5 0.0312(9) 0.0244(8) 0.0224(8) 0.0010(6) 0.0093(7) 0.0056(7) C6 0.0259(8) 0.0216(8) 0.0210(7) 0.0019(6) 0.0055(6) 0.0045(6) C7 0.0260(8) 0.0270(9) 0.0205(7) 0.0042(6) 0.0074(6) 0.0061(7) C8 0.0217(8) 0.0361(10) 0.0349(9) 0.0116(8) 0.0119(7) 0.0075(7) C9 0.0197(7) 0.0232(8) 0.0362(9) 0.0052(7) 0.0103(7) -0.0002(6) C10 0.0334(10) 0.0590(14) 0.0547(13) 0.0335(12) 0.0176(10) 0.0088(10) C11 0.0261(9) 0.0199(8) 0.0524(12) 0.0014(8) 0.0075(8) -0.0028(7) C12 0.0212(8) 0.0351(10) 0.0532(12) 0.0167(9) 0.0135(8) -0.0005(7) C13 0.0306(10) 0.0646(16) 0.0652(15) 0.0399(13) 0.0212(10) 0.0059(10) C14 0.0242(8) 0.0178(7) 0.0236(8) 0.0023(6) 0.0094(6) -0.0008(6) C15 0.0320(9) 0.0233(8) 0.0366(9) -0.0019(7) 0.0157(8) 0.0024(7) C16 0.0260(9) 0.0356(10) 0.0312(9) 0.0040(8) 0.0056(7) -0.0015(7) C17 0.0286(10) 0.0274(10) 0.0794(17) 0.0066(10) 0.0095(10) -0.0062(8) C18 0.0223(8) 0.0451(12) 0.0479(11) 0.0200(9) 0.0163(8) 0.0034(8) C19 0.0262(8) 0.0199(8) 0.0218(7) 0.0010(6) 0.0079(6) -0.0012(6) C20 0.0276(8) 0.0243(8) 0.0268(8) -0.0038(7) 0.0092(7) -0.0043(7) C21 0.0311(10) 0.0558(13) 0.0423(11) 0.0095(10) 0.0197(9) 0.0115(9) C22 0.0253(9) 0.0500(13) 0.0614(14) 0.0151(11) 0.0123(9) -0.0028(9) C23 0.0221(8) 0.0246(8) 0.0286(8) 0.0030(7) 0.0066(6) -0.0010(6) C24 0.0346(9) 0.0227(8) 0.0296(9) -0.0035(7) 0.0158(7) -0.0017(7) C25 0.0441(13) 0.0647(16) 0.0533(14) 0.0105(12) 0.0276(11) 0.0225(11) C26 0.0220(9) 0.0751(18) 0.0587(14) 0.0273(13) 0.0110(9) 0.0037(10) C27 0.0265(8) 0.0223(8) 0.0355(9) 0.0047(7) 0.0157(7) 0.0027(7) C28 0.0358(11) 0.0682(17) 0.0600(15) 0.0239(13) 0.0252(11) 0.0226(11) C1A 0.0589(18) 0.112(3) 0.074(2) 0.009(2) 0.0100(16) 0.0000(19) C2A 0.0465(15) 0.121(3) 0.0583(17) 0.0173(18) 0.0055(13) 0.0011(17) C3A 0.0476(15) 0.125(3) 0.0503(16) 0.0337(17) 0.0169(12) 0.0139(16) 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' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.0270 1 0 0 0.0153 0 -1 0 0.1108 -1 2 0 0.1073 0 0 1 0.0387 0 0 -1 0.0315 10 -3 -5 0.0709 7 4 -4 0.1042 4 0 10 0.0333 3 -2 10 0.0478 -7 0 11 0.0432 11 2 2 0.0459 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 C14 Si1 C9 108.43(7) . . ? C15 Si1 C9 114.03(8) . . ? C15 Si1 C14 106.36(8) . . ? C15 Si1 C16 110.12(9) . . ? C16 Si1 C9 110.22(8) . . ? C16 Si1 C14 107.38(8) . . ? C7 O2 C8 118.21(14) . . ? C6 N1 H1 116.7(15) . . ? C7 N1 H1 115.4(15) . . ? C7 N1 C6 126.59(15) . . ? C2 C1 Br1 119.14(14) . . ? C3 C1 Br1 119.46(14) . . ? C3 C1 C2 121.41(17) . . ? C1 C2 H2 120.6 . . ? C1 C2 C4 118.74(16) . . ? C4 C2 H2 120.6 . . ? C1 C3 H3 120.1 . . ? C1 C3 C5 119.87(16) . . ? C5 C3 H3 120.1 . . ? C2 C4 H4 119.7 . . ? C2 C4 C6 120.66(16) . . ? C6 C4 H4 119.7 . . ? C3 C5 H5 120.1 . . ? C3 C5 C6 119.75(16) . . ? C6 C5 H5 120.1 . . ? C4 C6 N1 117.13(15) . . ? C5 C6 N1 123.29(15) . . ? C5 C6 C4 119.57(16) . . ? O1 C7 O2 125.25(16) . . ? O1 C7 N1 126.30(17) . . ? O2 C7 N1 108.44(15) . . ? O2 C8 H8 110.0 . . ? O2 C8 C9 111.07(14) . . ? O2 C8 C10 109.87(15) . . ? C9 C8 H8 110.0 . . ? C10 C8 H8 110.0 . . ? C10 C8 C9 105.74(17) . . ? C8 C9 Si1 116.52(13) . . ? C8 C9 C11 113.03(15) . . ? C8 C9 C12 103.81(14) . . ? C11 C9 Si1 110.84(13) . . ? C11 C9 C12 88.14(14) . . ? C12 C9 Si1 121.22(12) . . ? C8 C10 H10A 111.3 . . ? C8 C10 H10B 111.3 . . ? C8 C10 C13 102.28(16) . . ? H10A C10 H10B 109.2 . . ? C13 C10 H10A 111.3 . . ? C13 C10 H10B 111.3 . . ? C9 C11 H11A 113.5 . . ? C9 C11 H11B 113.5 . . ? H11A C11 H11B 110.8 . . ? C17 C11 C9 90.67(15) . . ? C17 C11 H11A 113.5 . . ? C17 C11 H11B 113.5 . . ? C13 C12 C9 104.88(16) . . ? C17 C12 C9 88.95(15) . . ? C17 C12 C13 113.22(19) . . ? C18 C12 C9 119.33(16) . . ? C18 C12 C13 110.34(18) . . ? C18 C12 C17 118.13(19) . . ? C10 C13 C12 106.12(17) . . ? C10 C13 H13A 110.5 . . ? C10 C13 H13B 110.5 . . ? C12 C13 H13A 110.5 . . ? C12 C13 H13B 110.5 . . ? H13A C13 H13B 108.7 . . ? C19 C14 Si1 121.45(12) . . ? C19 C14 C20 117.15(15) . . ? C20 C14 Si1 121.26(13) . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C11 C17 C12 91.00(16) . . ? C11 C17 H17A 113.5 . . ? C11 C17 H17B 113.5 . . ? C12 C17 H17A 113.5 . . ? C12 C17 H17B 113.5 . . ? H17A C17 H17B 110.8 . . ? C21 C18 C12 119.54(19) . . ? C22 C18 C12 122.6(2) . . ? C22 C18 C21 117.8(2) . . ? C14 C19 H19 119.2 . . ? C23 C19 C14 121.70(15) . . ? C23 C19 H19 119.2 . . ? C14 C20 H20 119.2 . . ? C24 C20 C14 121.54(16) . . ? C24 C20 H20 119.2 . . ? C18 C21 H21 119.3 . . ? C25 C21 C18 121.3(2) . . ? C25 C21 H21 119.3 . . ? C18 C22 H22 119.8 . . ? C18 C22 C26 120.4(3) . . ? C26 C22 H22 119.8 . . ? C19 C23 H23 120.1 . . ? C27 C23 C19 119.81(16) . . ? C27 C23 H23 120.1 . . ? C20 C24 H24 120.0 . . ? C27 C24 C20 119.96(16) . . ? C27 C24 H24 120.0 . . ? C21 C25 H25 119.9 . . ? C28 C25 C21 120.1(3) . . ? C28 C25 H25 119.9 . . ? C22 C26 H26 119.6 . . ? C28 C26 C22 120.8(2) . . ? C28 C26 H26 119.6 . . ? C23 C27 H27 120.1 . . ? C24 C27 C23 119.84(16) . . ? C24 C27 H27 120.1 . . ? C25 C28 H28 120.2 . . ? C26 C28 C25 119.5(2) . . ? C26 C28 H28 120.2 . . ? H1AA C1A H1AB 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C2A C1A H1AA 109.5 . . ? C2A C1A H1AB 109.5 . . ? C2A C1A H1AC 109.5 . . ? C1A C2A H2AA 109.1 . . ? C1A C2A H2AB 109.1 . . ? C1A C2A C3A 112.4(3) . . ? H2AA C2A H2AB 107.9 . . ? C3A C2A H2AA 109.1 . . ? C3A C2A H2AB 109.1 . . ? C2A C3A H3AA 109.0 . . ? C2A C3A H3AB 109.0 . . ? C3A C3A C2A 112.9(3) 3_777 . ? C3A C3A H3AA 109.0 3_777 . ? C3A C3A H3AB 109.0 3_777 . ? H3AA C3A H3AB 107.8 . . ? 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 Br1 C1 1.9067(18) . ? Si1 C9 1.8959(18) . ? Si1 C14 1.8893(17) . ? Si1 C15 1.8732(19) . ? Si1 C16 1.8751(19) . ? O1 C7 1.213(2) . ? O2 C7 1.347(2) . ? O2 C8 1.453(2) . ? N1 H1 0.890(16) . ? N1 C6 1.407(2) . ? N1 C7 1.361(2) . ? C1 C2 1.382(3) . ? C1 C3 1.381(3) . ? C2 H2 0.9300 . ? C2 C4 1.385(3) . ? C3 H3 0.9300 . ? C3 C5 1.385(3) . ? C4 H4 0.9300 . ? C4 C6 1.399(2) . ? C5 H5 0.9300 . ? C5 C6 1.391(2) . ? C8 H8 0.9800 . ? C8 C9 1.533(3) . ? C8 C10 1.525(3) . ? C9 C11 1.566(3) . ? C9 C12 1.605(2) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C13 1.530(3) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C17 1.542(3) . ? C12 C13 1.555(3) . ? C12 C17 1.550(3) . ? C12 C18 1.514(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.401(2) . ? C14 C20 1.403(2) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C21 1.395(3) . ? C18 C22 1.391(3) . ? C19 H19 0.9300 . ? C19 C23 1.392(2) . ? C20 H20 0.9300 . ? C20 C24 1.393(2) . ? C21 H21 0.9300 . ? C21 C25 1.389(3) . ? C22 H22 0.9300 . ? C22 C26 1.400(3) . ? C23 H23 0.9300 . ? C23 C27 1.390(3) . ? C24 H24 0.9300 . ? C24 C27 1.386(3) . ? C25 H25 0.9300 . ? C25 C28 1.377(4) . ? C26 H26 0.9300 . ? C26 C28 1.372(4) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C1A H1AA 0.9600 . ? C1A H1AB 0.9600 . ? C1A H1AC 0.9600 . ? C1A C2A 1.485(5) . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C2A C3A 1.516(5) . ? C3A C3A 1.465(8) 3_777 ? C3A H3AA 0.9700 . ? C3A H3AB 0.9700 . ? 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 -1.0001 0.0002 0.0002 0.0065 0.0843 -0.0025 1.0001 -0.0002 -0.0002 -0.0065 -0.0843 0.0025 -0.0001 -1.0001 0.0019 0.0011 0.0051 0.1844 -0.9998 2.0003 -0.0035 0.0043 0.0740 -0.3714 0.0002 0.0002 0.9998 0.0805 -0.0308 0.0005 -0.0002 -0.0002 -0.9998 -0.0805 0.0308 -0.0005 9.7383 -3.0896 -5.3577 -0.4914 -0.6397 0.5910 6.8592 4.4055 -3.9405 -0.3657 -0.4796 -0.7976 3.5073 0.0244 10.1452 0.7938 -0.6081 0.0091 3.4594 -1.5053 9.6939 0.7592 -0.5822 0.2908 -7.4910 -0.2313 11.2999 0.9582 0.2846 0.0299 10.6352 1.5882 1.8290 0.0769 -0.9609 -0.2660