data_global # 1. SUBMISSION DETAILS #---------------------- _publ_contact_author_name 'Skelton, B. W.' _publ_contact_author_address ; Centre for Microscopy, Characterisation and Analysis, M313, University of Western Australia, Perth, WA 6009, Australia ; _publ_contact_author_email brian.skelton@uwa.edu.au _publ_contact_author_fax (+61)_08_6488_1118 _publ_contact_author_phone (+61)_08_6488_7107 loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Skelton, Brian W.' . ; Centre for Microscopy, Characterisation and Analysis, M313, University of Western Australia, Perth, WA 6009, Australia ; _publ_section_references ; Brandenburg, K. ,(1999).DIAMOND.Crystal Impact GbR, Bonn, Germany. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Oxford Diffraction (2006). CrysAlis CCD. Oxford Diffraction Ltd, Abingdon, England. Oxford Diffraction (2006). CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England. Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_jg0408 _audit_creation_date 2014-09-15T10:33:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C64 H78 N2 O4 Si2' _chemical_formula_moiety 'C64 H78 N2 O4 Si2' _chemical_formula_weight 995.46 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3075(2) _cell_length_b 23.9449(3) _cell_length_c 11.5539(2) _cell_angle_alpha 90 _cell_angle_beta 111.656(2) _cell_angle_gamma 90 _cell_volume 2907.49(8) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 5309 _cell_measurement_theta_min 3.673 _cell_measurement_theta_max 66.974 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.095 _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -2 -1 0.0954 0 2 1 0.1339 0 -1 1 0.1576 0 -1 0 0.1467 1 0 0 0.0138 -1 0 0 0.0818 0 3 -1 0.087 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.915 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. ; _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.918 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'sealed X-ray tube' _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 0.133162 _diffrn_orient_matrix_ub_12 0.0191926 _diffrn_orient_matrix_ub_13 0.0871107 _diffrn_orient_matrix_ub_21 0.060914 _diffrn_orient_matrix_ub_22 -0.0367312 _diffrn_orient_matrix_ub_23 -0.0724718 _diffrn_orient_matrix_ub_31 -0.0064369 _diffrn_orient_matrix_ub_32 0.0492032 _diffrn_orient_matrix_ub_33 -0.087993 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction Gemini diffractometer' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_unetI/netI 0.0258 _diffrn_reflns_number 14045 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 67.34 _diffrn_reflns_theta_full 67.34 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 5186 _reflns_number_gt 4009 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Brandenburg, K., (1999)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The data were collected at 250K since the crystals appeared to shatter at lower temperatures and deteriorate at room temperature when left in contact with air. The isopropyl groups were modelled as being disordered over two sets of sites with occupancies constrained to be equal after trial refinement. Geometries of the disordered atoms were restrained to ideal values with some of the displacement parameters restrained to reasonable values. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1212P)^2^+0.4074P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5186 _refine_ls_number_parameters 408 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.073 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1995 _refine_ls_wR_factor_gt 0.1817 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.384 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.041 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 '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_ _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5192(2) 0.47308(9) 0.5155(2) 0.0676(5) Uani 1 1 d . . . C2 C 0.4693(2) 0.43999(9) 0.5911(2) 0.0697(6) Uani 1 1 d . . . C3 C 0.4351(2) 0.40926(9) 0.6551(2) 0.0749(6) Uani 1 1 d . A . C4 C 0.6147(2) 0.44385(8) 0.4768(2) 0.0677(5) Uani 1 1 d . . . C5 C 0.5987(2) 0.38755(9) 0.4439(3) 0.0788(7) Uani 1 1 d . . . H5 H 0.5267 0.3686 0.446 0.095 Uiso 1 1 calc R . . C6 C 0.6858(3) 0.35897(9) 0.4084(3) 0.0818(7) Uani 1 1 d . . . H6 H 0.6713 0.3212 0.3853 0.098 Uiso 1 1 calc R . . C7 C 0.7947(2) 0.38515(9) 0.4063(3) 0.0758(6) Uani 1 1 d . . . C8 C 0.8137(2) 0.44086(9) 0.4426(2) 0.0740(6) Uani 1 1 d . . . H8 H 0.8873 0.4594 0.4435 0.089 Uiso 1 1 calc R . . C9 C 0.7254(2) 0.46931(9) 0.4777(2) 0.0703(6) Uani 1 1 d . . . H9 H 0.7409 0.5068 0.5027 0.084 Uiso 1 1 calc R . . Si1 Si 0.38794(7) 0.36365(3) 0.75888(7) 0.0849(3) Uani 1 1 d . . . C10 C 0.5446(14) 0.3671(7) 0.9057(12) 0.202(8) Uani 0.5 1 d PD A 1 H10 H 0.6122 0.3499 0.8823 0.242 Uiso 0.5 1 calc PR A 1 C11 C 0.585(2) 0.4251(8) 0.9448(14) 0.294(15) Uani 0.5 1 d PD A 1 H11A H 0.5892 0.446 0.8743 0.44 Uiso 0.5 1 calc PR A 1 H11B H 0.6687 0.4247 1.0109 0.44 Uiso 0.5 1 calc PR A 1 H11C H 0.5246 0.4426 0.9747 0.44 Uiso 0.5 1 calc PR A 1 C12 C 0.5458(14) 0.3378(8) 1.0196(13) 0.273(11) Uani 0.5 1 d PD A 1 H12A H 0.5169 0.2996 0.9988 0.41 Uiso 0.5 1 calc PR A 1 H12B H 0.4897 0.3569 1.0529 0.41 Uiso 0.5 1 calc PR A 1 H12C H 0.6317 0.3376 1.0814 0.41 Uiso 0.5 1 calc PR A 1 C13 C 0.2508(7) 0.4052(4) 0.7872(6) 0.0903(19) Uani 0.5 1 d PD A 1 H13 H 0.2852 0.4422 0.8216 0.108 Uiso 0.5 1 calc PR A 1 C14 C 0.1386(7) 0.4151(4) 0.6607(7) 0.093(2) Uani 0.5 1 d PD A 1 H14A H 0.1705 0.4329 0.6026 0.14 Uiso 0.5 1 calc PR A 1 H14B H 0.0755 0.4391 0.6739 0.14 Uiso 0.5 1 calc PR A 1 H14C H 0.0999 0.3796 0.6268 0.14 Uiso 0.5 1 calc PR A 1 C15 C 0.1937(11) 0.3789(6) 0.8752(9) 0.168(5) Uani 0.5 1 d PD A 1 H15A H 0.2607 0.3717 0.9551 0.252 Uiso 0.5 1 calc PR A 1 H15B H 0.1522 0.344 0.84 0.252 Uiso 0.5 1 calc PR A 1 H15C H 0.1318 0.4042 0.8863 0.252 Uiso 0.5 1 calc PR A 1 C16 C 0.3121(10) 0.2988(3) 0.6640(8) 0.124(2) Uani 0.5 1 d PD A 1 H16 H 0.2304 0.3137 0.6051 0.149 Uiso 0.5 1 calc PR A 1 C17 C 0.2695(13) 0.2565(5) 0.7323(13) 0.198(6) Uani 0.5 1 d PDU A 1 H17A H 0.2364 0.2749 0.7888 0.297 Uiso 0.5 1 calc PR A 1 H17B H 0.3408 0.2329 0.7794 0.297 Uiso 0.5 1 calc PR A 1 H17C H 0.2033 0.2338 0.6737 0.297 Uiso 0.5 1 calc PR A 1 C18 C 0.3686(13) 0.2776(3) 0.5829(9) 0.179(5) Uani 0.5 1 d PD A 1 H18A H 0.3944 0.3084 0.5429 0.269 Uiso 0.5 1 calc PR A 1 H18B H 0.3077 0.2544 0.5201 0.269 Uiso 0.5 1 calc PR A 1 H18C H 0.4426 0.2555 0.63 0.269 Uiso 0.5 1 calc PR A 1 C10' C 0.4924(7) 0.3653(5) 0.9207(8) 0.120(3) Uani 0.5 1 d PD A 2 H10' H 0.45 0.3448 0.969 0.144 Uiso 0.5 1 calc PR A 2 C11' C 0.5180(15) 0.4229(7) 0.9709(16) 0.220(9) Uani 0.5 1 d PD A 2 H11D H 0.438 0.4415 0.9583 0.329 Uiso 0.5 1 calc PR A 2 H11E H 0.5637 0.4433 0.9281 0.329 Uiso 0.5 1 calc PR A 2 H11F H 0.5689 0.4214 1.0593 0.329 Uiso 0.5 1 calc PR A 2 C12' C 0.6137(12) 0.3340(8) 0.9338(19) 0.284(12) Uani 0.5 1 d PD A 2 H12D H 0.5924 0.2966 0.9002 0.426 Uiso 0.5 1 calc PR A 2 H12E H 0.6681 0.3317 1.0211 0.426 Uiso 0.5 1 calc PR A 2 H12F H 0.6581 0.3536 0.8885 0.426 Uiso 0.5 1 calc PR A 2 C13' C 0.2250(8) 0.3710(4) 0.7378(11) 0.123(3) Uani 0.5 1 d PD A 2 H13' H 0.1767 0.3564 0.6533 0.147 Uiso 0.5 1 calc PR A 2 C14' C 0.1815(9) 0.3362(4) 0.8256(11) 0.144(4) Uani 0.5 1 d PD A 2 H14D H 0.2053 0.2975 0.8224 0.215 Uiso 0.5 1 calc PR A 2 H14E H 0.0898 0.3389 0.8003 0.215 Uiso 0.5 1 calc PR A 2 H14F H 0.2218 0.3501 0.91 0.215 Uiso 0.5 1 calc PR A 2 C15' C 0.1851(16) 0.4295(5) 0.7362(16) 0.168(5) Uani 0.5 1 d PDU A 2 H15D H 0.2142 0.4508 0.6805 0.253 Uiso 0.5 1 calc PR A 2 H15E H 0.2218 0.4449 0.8196 0.253 Uiso 0.5 1 calc PR A 2 H15F H 0.093 0.4313 0.7075 0.253 Uiso 0.5 1 calc PR A 2 C16' C 0.4165(9) 0.2876(3) 0.7168(10) 0.128(3) Uani 0.5 1 d PD A 2 H16' H 0.3528 0.2844 0.631 0.154 Uiso 0.5 1 calc PR A 2 C17' C 0.5271(16) 0.2761(5) 0.6981(18) 0.224(6) Uani 0.5 1 d PDU A 2 H17D H 0.5484 0.3074 0.6561 0.337 Uiso 0.5 1 calc PR A 2 H17E H 0.5156 0.2429 0.6472 0.337 Uiso 0.5 1 calc PR A 2 H17F H 0.5954 0.27 0.7778 0.337 Uiso 0.5 1 calc PR A 2 C18' C 0.375(2) 0.2430(6) 0.780(2) 0.256(10) Uani 0.5 1 d PD A 2 H18D H 0.3008 0.2551 0.7954 0.384 Uiso 0.5 1 calc PR A 2 H18E H 0.4435 0.2344 0.8583 0.384 Uiso 0.5 1 calc PR A 2 H18F H 0.3549 0.21 0.7276 0.384 Uiso 0.5 1 calc PR A 2 C19 C 0.8842(2) 0.29603(9) 0.3723(2) 0.0752(6) Uani 1 1 d . . . C20 C 0.9294(3) 0.26771(10) 0.4833(2) 0.0784(6) Uani 1 1 d . . . H20 H 0.9587 0.2877 0.5586 0.094 Uiso 1 1 calc R . . C21 C 0.9322(3) 0.21012(10) 0.4851(3) 0.0808(7) Uani 1 1 d . . . H21 H 0.9647 0.1911 0.5615 0.097 Uiso 1 1 calc R . . C22 C 0.8872(2) 0.18034(9) 0.3747(2) 0.0741(6) Uani 1 1 d . . . C23 C 0.8422(3) 0.20821(11) 0.2636(3) 0.0849(7) Uani 1 1 d . . . H23 H 0.8121 0.1883 0.1882 0.102 Uiso 1 1 calc R . . C24 C 0.8414(3) 0.26637(11) 0.2635(3) 0.0890(8) Uani 1 1 d . . . H24 H 0.8109 0.2856 0.1872 0.107 Uiso 1 1 calc R . . C25 C 0.8349(4) 0.09193(12) 0.2745(4) 0.1123(10) Uani 1 1 d . . . H25A H 0.7469 0.1032 0.2331 0.168 Uiso 1 1 calc R . . H25B H 0.8386 0.0525 0.295 0.168 Uiso 1 1 calc R . . H25C H 0.881 0.0985 0.2197 0.168 Uiso 1 1 calc R . . C26 C 0.9586(2) 0.38311(9) 0.3112(2) 0.0733(6) Uani 1 1 d . . . C27 C 1.0818(3) 0.36652(12) 0.3390(3) 0.0882(8) Uani 1 1 d . . . H27 H 1.1161 0.3384 0.3988 0.106 Uiso 1 1 calc R . . C28 C 1.1569(3) 0.39047(12) 0.2808(3) 0.0866(7) Uani 1 1 d . . . H28 H 1.2418 0.3789 0.3021 0.104 Uiso 1 1 calc R . . C29 C 1.1078(2) 0.43067(10) 0.1931(2) 0.0760(6) Uani 1 1 d . . . C30 C 0.9832(3) 0.44742(10) 0.1635(3) 0.0834(7) Uani 1 1 d . . . H30 H 0.9483 0.4751 0.1028 0.1 Uiso 1 1 calc R . . C31 C 0.9100(2) 0.42380(10) 0.2223(3) 0.0781(6) Uani 1 1 d . . . H31 H 0.8254 0.4356 0.2016 0.094 Uiso 1 1 calc R . . C32 C 1.3050(4) 0.44409(19) 0.1664(5) 0.1390(15) Uani 1 1 d . . . H32A H 1.3459 0.4507 0.2552 0.208 Uiso 1 1 calc R . . H32B H 1.3427 0.4682 0.1219 0.208 Uiso 1 1 calc R . . H32C H 1.3167 0.4054 0.1484 0.208 Uiso 1 1 calc R . . N1 N 0.8834(2) 0.35602(8) 0.3703(3) 0.0898(7) Uani 1 1 d . . . O1 O 0.8912(2) 0.12354(7) 0.3855(2) 0.0952(6) Uani 1 1 d . . . O2 O 1.1727(2) 0.45590(8) 0.1280(2) 0.1053(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0722(12) 0.0581(10) 0.0886(14) 0.0048(10) 0.0484(11) 0.0108(9) C2 0.0737(13) 0.0567(11) 0.0943(15) 0.0057(10) 0.0491(12) 0.0154(9) C3 0.0775(14) 0.0636(12) 0.0986(16) 0.0133(12) 0.0500(13) 0.0146(10) C4 0.0759(13) 0.0560(11) 0.0868(14) 0.0064(10) 0.0482(11) 0.0128(9) C5 0.0849(15) 0.0600(12) 0.1135(18) 0.0013(12) 0.0622(14) 0.0071(11) C6 0.0946(17) 0.0557(11) 0.119(2) -0.0025(12) 0.0675(16) 0.0072(11) C7 0.0913(15) 0.0564(11) 0.1055(17) 0.0099(11) 0.0666(14) 0.0177(10) C8 0.0776(13) 0.0567(11) 0.1064(17) 0.0090(11) 0.0559(13) 0.0118(10) C9 0.0794(13) 0.0537(10) 0.0927(15) 0.0074(10) 0.0491(12) 0.0137(9) Si1 0.0942(5) 0.0762(5) 0.0927(5) 0.0172(3) 0.0444(4) -0.0040(3) C10 0.119(10) 0.31(2) 0.176(12) 0.138(13) 0.059(9) 0.015(12) C11 0.29(2) 0.37(3) 0.128(10) 0.024(13) -0.028(12) -0.21(2) C12 0.157(10) 0.40(2) 0.208(13) 0.200(16) 0.002(10) -0.031(13) C13 0.101(5) 0.080(4) 0.111(5) -0.013(4) 0.062(4) -0.020(4) C14 0.079(4) 0.096(4) 0.112(5) 0.002(4) 0.044(4) -0.007(3) C15 0.138(7) 0.269(15) 0.127(7) 0.001(9) 0.083(6) -0.020(10) C16 0.152(7) 0.086(4) 0.125(6) 0.029(4) 0.042(5) -0.004(4) C17 0.193(10) 0.099(7) 0.248(12) 0.038(7) 0.017(9) -0.053(7) C18 0.306(15) 0.084(4) 0.135(7) -0.049(5) 0.066(8) 0.036(6) C10' 0.077(5) 0.199(9) 0.099(5) 0.034(5) 0.050(4) -0.022(5) C11' 0.210(14) 0.30(2) 0.185(13) -0.105(13) 0.115(11) -0.146(14) C12' 0.130(9) 0.38(3) 0.34(2) 0.22(2) 0.089(12) 0.132(13) C13' 0.106(5) 0.133(7) 0.157(7) 0.058(6) 0.081(5) 0.020(5) C14' 0.112(6) 0.182(9) 0.170(9) 0.061(7) 0.091(7) 0.018(6) C15' 0.187(12) 0.125(8) 0.251(14) 0.055(9) 0.149(11) 0.058(8) C16' 0.120(6) 0.074(4) 0.180(8) 0.027(5) 0.045(6) 0.006(4) C17' 0.262(14) 0.119(7) 0.338(16) 0.015(9) 0.165(13) 0.032(8) C18' 0.37(3) 0.115(9) 0.30(2) 0.055(11) 0.15(2) -0.009(14) C19 0.0914(15) 0.0568(11) 0.1040(17) 0.0085(11) 0.0671(14) 0.0178(10) C20 0.0946(16) 0.0669(13) 0.0887(16) -0.0012(12) 0.0512(13) 0.0031(11) C21 0.0955(16) 0.0691(13) 0.0859(16) 0.0127(12) 0.0429(13) 0.0101(12) C22 0.0858(15) 0.0555(11) 0.0959(16) 0.0048(11) 0.0512(13) 0.0128(10) C23 0.1135(19) 0.0706(14) 0.0851(16) 0.0013(12) 0.0535(15) 0.0140(13) C24 0.119(2) 0.0734(15) 0.0915(17) 0.0187(13) 0.0584(16) 0.0291(14) C25 0.137(3) 0.0653(15) 0.147(3) -0.0208(17) 0.068(2) -0.0042(16) C26 0.0856(15) 0.0585(11) 0.0972(16) 0.0036(11) 0.0587(13) 0.0119(10) C27 0.0912(17) 0.0902(17) 0.1044(19) 0.0230(14) 0.0608(15) 0.0292(13) C28 0.0786(15) 0.0961(18) 0.1019(18) -0.0016(15) 0.0529(14) 0.0093(13) C29 0.0934(16) 0.0635(12) 0.0910(15) -0.0109(12) 0.0572(13) -0.0110(11) C30 0.1004(18) 0.0694(13) 0.0922(17) 0.0090(12) 0.0493(14) 0.0025(13) C31 0.0774(14) 0.0692(13) 0.0993(16) 0.0063(12) 0.0461(13) 0.0093(11) C32 0.124(3) 0.152(3) 0.185(4) -0.019(3) 0.109(3) -0.037(2) N1 0.1125(16) 0.0538(10) 0.145(2) 0.0135(11) 0.0959(16) 0.0185(10) O1 0.1223(15) 0.0577(9) 0.1178(14) 0.0068(9) 0.0586(12) 0.0090(9) O2 0.1282(16) 0.0899(12) 0.1335(16) -0.0056(11) 0.0902(14) -0.0208(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C1 1.365(4) 3_666 ? C1 C2 1.440(3) . ? C1 C4 1.488(3) . ? C2 C3 1.204(3) . ? C3 Si1 1.840(2) . ? C4 C9 1.389(3) . ? C4 C5 1.394(3) . ? C5 C6 1.381(3) . ? C5 H5 0.94 . ? C6 C7 1.389(3) . ? C6 H6 0.94 . ? C7 C8 1.391(3) . ? C7 N1 1.405(3) . ? C8 C9 1.387(3) . ? C8 H8 0.94 . ? C9 H9 0.94 . ? Si1 C13' 1.775(7) . ? Si1 C10' 1.806(9) . ? Si1 C16 1.911(8) . ? Si1 C16' 1.944(8) . ? Si1 C10 1.950(14) . ? Si1 C13 1.968(8) . ? C10 C11 1.481(17) . ? C10 C12 1.487(13) . ? C10 H10 0.99 . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C11 H11C 0.97 . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C12 H12C 0.97 . ? C13 C15 1.527(10) . ? C13 C14 1.561(10) . ? C13 H13 0.99 . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C14 H14C 0.97 . ? C15 H15A 0.97 . ? C15 H15B 0.97 . ? C15 H15C 0.97 . ? C16 C18 1.410(11) . ? C16 C17 1.470(11) . ? C16 H16 0.99 . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? C17 H17C 0.97 . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C18 H18C 0.97 . ? C10' C11' 1.482(14) . ? C10' C12' 1.522(12) . ? C10' H10' 0.99 . ? C11' H11D 0.97 . ? C11' H11E 0.97 . ? C11' H11F 0.97 . ? C12' H12D 0.97 . ? C12' H12E 0.97 . ? C12' H12F 0.97 . ? C13' C15' 1.469(11) . ? C13' C14' 1.528(9) . ? C13' H13' 0.99 . ? C14' H14D 0.97 . ? C14' H14E 0.97 . ? C14' H14F 0.97 . ? C15' H15D 0.97 . ? C15' H15E 0.97 . ? C15' H15F 0.97 . ? C16' C17' 1.372(12) . ? C16' C18' 1.460(12) . ? C16' H16' 0.99 . ? C17' H17D 0.97 . ? C17' H17E 0.97 . ? C17' H17F 0.97 . ? C18' H18D 0.97 . ? C18' H18E 0.97 . ? C18' H18F 0.97 . ? C19 C24 1.367(4) . ? C19 C20 1.372(4) . ? C19 N1 1.437(3) . ? C20 C21 1.379(3) . ? C20 H20 0.94 . ? C21 C22 1.383(4) . ? C21 H21 0.94 . ? C22 O1 1.365(3) . ? C22 C23 1.367(4) . ? C23 C24 1.393(4) . ? C23 H23 0.94 . ? C24 H24 0.94 . ? C25 O1 1.421(4) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C25 H25C 0.97 . ? C26 C27 1.367(3) . ? C26 C31 1.374(3) . ? C26 N1 1.428(3) . ? C27 C28 1.388(4) . ? C27 H27 0.94 . ? C28 C29 1.359(4) . ? C28 H28 0.94 . ? C29 O2 1.371(3) . ? C29 C30 1.381(4) . ? C30 C31 1.372(3) . ? C30 H30 0.94 . ? C31 H31 0.94 . ? C32 O2 1.423(5) . ? C32 H32A 0.97 . ? C32 H32B 0.97 . ? C32 H32C 0.97 . ? 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 C1 C1 C2 121.4(2) 3_666 . ? C1 C1 C4 124.1(2) 3_666 . ? C2 C1 C4 114.47(17) . . ? C3 C2 C1 174.7(2) . . ? C2 C3 Si1 177.6(3) . . ? C9 C4 C5 116.96(18) . . ? C9 C4 C1 122.94(19) . . ? C5 C4 C1 120.0(2) . . ? C6 C5 C4 121.6(2) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 121.0(2) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C6 C7 C8 117.82(19) . . ? C6 C7 N1 121.0(2) . . ? C8 C7 N1 121.2(2) . . ? C9 C8 C7 120.8(2) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C4 121.7(2) . . ? C8 C9 H9 119.1 . . ? C4 C9 H9 119.1 . . ? C13' Si1 C10' 112.9(5) . . ? C13' Si1 C3 112.8(2) . . ? C10' Si1 C3 115.2(3) . . ? C3 Si1 C16 106.6(2) . . ? C13' Si1 C16' 108.6(5) . . ? C10' Si1 C16' 100.0(5) . . ? C3 Si1 C16' 106.2(3) . . ? C3 Si1 C10 98.8(4) . . ? C16 Si1 C10 127.2(6) . . ? C3 Si1 C13 104.1(2) . . ? C16 Si1 C13 106.9(4) . . ? C10 Si1 C13 110.6(6) . . ? C11 C10 C12 105.8(13) . . ? C11 C10 Si1 112.6(10) . . ? C12 C10 Si1 117.3(10) . . ? C11 C10 H10 106.8 . . ? C12 C10 H10 106.8 . . ? Si1 C10 H10 106.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 106.8(7) . . ? C15 C13 Si1 117.1(7) . . ? C14 C13 Si1 109.9(5) . . ? C15 C13 H13 107.6 . . ? C14 C13 H13 107.6 . . ? Si1 C13 H13 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C17 115.3(8) . . ? C18 C16 Si1 117.2(7) . . ? C17 C16 Si1 114.7(7) . . ? C18 C16 H16 102.1 . . ? C17 C16 H16 102.1 . . ? Si1 C16 H16 102.1 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C11' C10' C12' 112.4(10) . . ? C11' C10' Si1 112.6(9) . . ? C12' C10' Si1 108.3(10) . . ? C11' C10' H10' 107.8 . . ? C12' C10' H10' 107.8 . . ? Si1 C10' H10' 107.8 . . ? C10' C11' H11D 109.5 . . ? C10' C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C10' C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C10' C12' H12D 109.5 . . ? C10' C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C10' C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? C15' C13' C14' 110.8(8) . . ? C15' C13' Si1 113.2(9) . . ? C14' C13' Si1 115.3(6) . . ? C15' C13' H13' 105.5 . . ? C14' C13' H13' 105.5 . . ? Si1 C13' H13' 105.5 . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? C13' C15' H15D 109.5 . . ? C13' C15' H15E 109.5 . . ? H15D C15' H15E 109.5 . . ? C13' C15' H15F 109.5 . . ? H15D C15' H15F 109.5 . . ? H15E C15' H15F 109.5 . . ? C17' C16' C18' 114.1(10) . . ? C17' C16' Si1 118.1(7) . . ? C18' C16' Si1 116.5(9) . . ? C17' C16' H16' 101.3 . . ? C18' C16' H16' 101.3 . . ? Si1 C16' H16' 101.3 . . ? C16' C17' H17D 109.5 . . ? C16' C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? C16' C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? C16' C18' H18D 109.5 . . ? C16' C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C16' C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? C24 C19 C20 119.1(2) . . ? C24 C19 N1 120.5(2) . . ? C20 C19 N1 120.5(2) . . ? C19 C20 C21 120.5(2) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 120.2(2) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? O1 C22 C23 124.1(2) . . ? O1 C22 C21 116.2(2) . . ? C23 C22 C21 119.8(2) . . ? C22 C23 C24 119.3(3) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C19 C24 C23 121.2(2) . . ? C19 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? O1 C25 H25A 109.5 . . ? O1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 118.3(2) . . ? C27 C26 N1 119.3(2) . . ? C31 C26 N1 122.3(2) . . ? C26 C27 C28 121.2(2) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C29 C28 C27 119.9(2) . . ? C29 C28 H28 120 . . ? C27 C28 H28 120 . . ? C28 C29 O2 124.5(2) . . ? C28 C29 C30 119.3(2) . . ? O2 C29 C30 116.2(2) . . ? C31 C30 C29 120.3(2) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C26 120.9(2) . . ? C30 C31 H31 119.5 . . ? C26 C31 H31 119.5 . . ? O2 C32 H32A 109.5 . . ? O2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? O2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C7 N1 C26 122.17(18) . . ? C7 N1 C19 119.48(18) . . ? C26 N1 C19 117.44(17) . . ? C22 O1 C25 117.4(2) . . ? C29 O2 C32 117.1(3) . . ? _iucr_refine_instructions_details ; TITL crystal3 in P2(1)/c CELL 1.54178 11.3075 23.9449 11.5539 90.000 111.656 90.000 ZERR 2.00 0.0002 0.0003 0.0002 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O SI UNIT 128 156 4 8 4 MERG 2 dfix 1.52 .02 C10 C11 C10 C12 C13 C14 C13 C15 C16 C17 C16 C18 dfix 2.45 .02 C11 C12 C14 C15 C17 C18 dfix 1.52 .02 C10' C11' C10' C12' C13' C14' C13' C15' C16' C17' C16' C18' dfix 2.45 .02 C11' C12' C14' C15' C17' C18' isor .02 .02 C15' C17 C17' FMAP 2 PLAN 12 ACTA BOND $H WGHT 0.12120 0.40740 L.S. 20 TEMP -23.00 FVAR 4.11326 C1 1 0.519153 0.473080 0.515456 11.00000 0.07216 0.05812 = 0.08860 0.00485 0.04840 0.01082 C2 1 0.469265 0.439991 0.591107 11.00000 0.07369 0.05669 = 0.09423 0.00565 0.04911 0.01540 C3 1 0.435077 0.409253 0.655117 11.00000 0.07747 0.06358 = 0.09863 0.01335 0.04997 0.01459 C4 1 0.614743 0.443854 0.476759 11.00000 0.07584 0.05603 = 0.08681 0.00640 0.04815 0.01284 C5 1 0.598650 0.387546 0.443931 11.00000 0.08486 0.05998 = 0.11343 0.00127 0.06215 0.00710 AFIX 43 H5 2 0.526699 0.368569 0.446037 11.00000 -1.20000 AFIX 0 C6 1 0.685824 0.358969 0.408397 11.00000 0.09456 0.05571 = 0.11903 -0.00251 0.06752 0.00720 AFIX 43 H6 2 0.671296 0.321206 0.385276 11.00000 -1.20000 AFIX 0 C7 1 0.794671 0.385153 0.406280 11.00000 0.09132 0.05637 = 0.10549 0.00990 0.06658 0.01768 C8 1 0.813703 0.440866 0.442635 11.00000 0.07758 0.05666 = 0.10637 0.00897 0.05588 0.01180 AFIX 43 H8 2 0.887252 0.459435 0.443457 11.00000 -1.20000 AFIX 0 C9 1 0.725413 0.469313 0.477669 11.00000 0.07936 0.05369 = 0.09270 0.00744 0.04913 0.01375 AFIX 43 H9 2 0.740890 0.506823 0.502696 11.00000 -1.20000 AFIX 0 SI1 5 0.387938 0.363648 0.758881 11.00000 0.09417 0.07618 = 0.09263 0.01723 0.04438 -0.00400 PART 1 C10 1 0.544582 0.367070 0.905693 10.50000 0.11898 0.31383 = 0.17662 0.13843 0.05846 0.01509 AFIX 13 H10 2 0.612170 0.349847 0.882265 10.50000 -1.20000 AFIX 0 C11 1 0.585298 0.425108 0.944754 10.50000 0.29402 0.36904 = 0.12747 0.02393 -0.02769 -0.21107 AFIX 33 H11a 2 0.589242 0.445987 0.874323 10.50000 -1.50000 H11b 2 0.668679 0.424715 1.010861 10.50000 -1.50000 H11c 2 0.524637 0.442634 0.974659 10.50000 -1.50000 AFIX 0 C12 1 0.545810 0.337787 1.019629 10.50000 0.15710 0.39752 = 0.20794 0.19921 0.00194 -0.03053 AFIX 33 H12a 2 0.516849 0.299644 0.998895 10.50000 -1.50000 H12b 2 0.489710 0.356978 1.052872 10.50000 -1.50000 H12c 2 0.631671 0.337639 1.081442 10.50000 -1.50000 AFIX 0 C13 1 0.250790 0.405152 0.787187 10.50000 0.10035 0.08011 = 0.11027 -0.01344 0.06228 -0.02026 AFIX 13 H13 2 0.285156 0.442160 0.821561 10.50000 -1.20000 AFIX 0 C14 1 0.138558 0.415126 0.660674 10.50000 0.07926 0.09612 = 0.11211 0.00194 0.04416 -0.00691 AFIX 33 H14A 2 0.170517 0.432893 0.602592 10.50000 -1.50000 H14B 2 0.075524 0.439067 0.673953 10.50000 -1.50000 H14C 2 0.099868 0.379618 0.626834 10.50000 -1.50000 AFIX 0 C15 1 0.193632 0.378854 0.875167 10.50000 0.13780 0.26839 = 0.12704 0.00074 0.08280 -0.02060 AFIX 33 H15A 2 0.260665 0.371650 0.955124 10.50000 -1.50000 H15B 2 0.152165 0.344005 0.839955 10.50000 -1.50000 H15C 2 0.131762 0.404206 0.886302 10.50000 -1.50000 AFIX 0 C16 1 0.312124 0.298827 0.664084 10.50000 0.15285 0.08561 = 0.12529 0.02840 0.04179 -0.00397 AFIX 13 H16 2 0.230384 0.313701 0.605171 10.50000 -1.20000 AFIX 0 C17 1 0.269550 0.256508 0.732383 10.50000 0.19276 0.09924 = 0.24712 0.03789 0.01728 -0.05342 AFIX 33 H17A 2 0.236415 0.274870 0.788912 10.50000 -1.50000 H17B 2 0.340845 0.232938 0.779504 10.50000 -1.50000 H17C 2 0.203301 0.233796 0.673791 10.50000 -1.50000 AFIX 0 C18 1 0.368613 0.277612 0.582902 10.50000 0.30643 0.08377 = 0.13525 -0.04871 0.06589 0.03583 AFIX 33 H18A 2 0.394364 0.308369 0.542841 10.50000 -1.50000 H18B 2 0.307718 0.254398 0.520096 10.50000 -1.50000 H18C 2 0.442621 0.255473 0.629920 10.50000 -1.50000 AFIX 0 PART 2 C10' 1 0.492388 0.365316 0.920659 10.50000 0.07726 0.19898 = 0.09885 0.03445 0.04931 -0.02197 AFIX 13 H10' 2 0.450026 0.344802 0.968998 10.50000 -1.20000 AFIX 0 C11' 1 0.518010 0.422864 0.970989 10.50000 0.20951 0.30084 = 0.18459 -0.10549 0.11505 -0.14575 AFIX 33 H11d 2 0.438081 0.441538 0.958400 10.50000 -1.50000 H11e 2 0.563748 0.443324 0.928182 10.50000 -1.50000 H11f 2 0.568970 0.421396 1.059326 10.50000 -1.50000 AFIX 0 C12' 1 0.613726 0.333969 0.933794 10.50000 0.13014 0.38103 = 0.34028 0.21994 0.08840 0.13176 AFIX 33 H12d 2 0.592387 0.296595 0.900161 10.50000 -1.50000 H12e 2 0.668078 0.331694 1.021114 10.50000 -1.50000 H12f 2 0.658064 0.353633 0.888480 10.50000 -1.50000 AFIX 0 C13' 1 0.225029 0.370978 0.737776 10.50000 0.10574 0.13328 = 0.15658 0.05798 0.08053 0.01992 AFIX 13 H13' 2 0.176685 0.356436 0.653233 10.50000 -1.20000 AFIX 0 C14' 1 0.181523 0.336206 0.825618 10.50000 0.11213 0.18149 = 0.17008 0.06084 0.09110 0.01781 AFIX 33 H14D 2 0.205293 0.297483 0.822351 10.50000 -1.50000 H14E 2 0.089834 0.338935 0.800300 10.50000 -1.50000 H14F 2 0.221818 0.350123 0.909980 10.50000 -1.50000 AFIX 0 C15' 1 0.185135 0.429469 0.736216 10.50000 0.18674 0.12497 = 0.25074 0.05430 0.14868 0.05789 AFIX 33 H15D 2 0.214204 0.450843 0.680480 10.50000 -1.50000 H15E 2 0.221799 0.444867 0.819584 10.50000 -1.50000 H15F 2 0.093070 0.431306 0.707553 10.50000 -1.50000 AFIX 0 C16' 1 0.416592 0.287551 0.716800 10.50000 0.12007 0.07430 = 0.18008 0.02731 0.04438 0.00568 AFIX 13 H16' 2 0.352843 0.284373 0.631037 10.50000 -1.20000 AFIX 0 C17' 1 0.527143 0.276107 0.697995 10.50000 0.26202 0.11894 = 0.33818 0.01428 0.16481 0.03219 AFIX 33 H17D 2 0.548431 0.307403 0.656019 10.50000 -1.50000 H17E 2 0.515592 0.242855 0.647036 10.50000 -1.50000 H17F 2 0.595502 0.269978 0.777645 10.50000 -1.50000 AFIX 0 C18' 1 0.375541 0.243038 0.779900 10.50000 0.36878 0.11454 = 0.30402 0.05452 0.14743 -0.00861 AFIX 33 H18D 2 0.300883 0.255132 0.795462 10.50000 -1.50000 H18E 2 0.443500 0.234453 0.858395 10.50000 -1.50000 H18F 2 0.354975 0.209963 0.727754 10.50000 -1.50000 AFIX 0 PART 0 C19 1 0.884159 0.296028 0.372248 11.00000 0.09138 0.05677 = 0.10404 0.00846 0.06712 0.01784 C20 1 0.929417 0.267714 0.483261 11.00000 0.09452 0.06690 = 0.08871 -0.00118 0.05122 0.00306 AFIX 43 H20 2 0.958735 0.287697 0.558603 11.00000 -1.20000 AFIX 0 C21 1 0.932189 0.210121 0.485065 11.00000 0.09553 0.06907 = 0.08589 0.01269 0.04292 0.01008 AFIX 43 H21 2 0.964730 0.191054 0.561483 11.00000 -1.20000 AFIX 0 C22 1 0.887212 0.180342 0.374722 11.00000 0.08582 0.05551 = 0.09590 0.00477 0.05118 0.01281 C23 1 0.842193 0.208211 0.263638 11.00000 0.11348 0.07058 = 0.08513 0.00131 0.05353 0.01404 AFIX 43 H23 2 0.812096 0.188327 0.188181 11.00000 -1.20000 AFIX 0 C24 1 0.841404 0.266369 0.263477 11.00000 0.11871 0.07340 = 0.09149 0.01872 0.05836 0.02908 AFIX 43 H24 2 0.810911 0.285588 0.187170 11.00000 -1.20000 AFIX 0 C25 1 0.834941 0.091930 0.274517 11.00000 0.13738 0.06523 = 0.14741 -0.02076 0.06805 -0.00421 AFIX 137 H25A 2 0.746881 0.103148 0.233121 11.00000 -1.50000 H25B 2 0.838604 0.052523 0.295005 11.00000 -1.50000 H25C 2 0.880971 0.098543 0.219675 11.00000 -1.50000 AFIX 0 C26 1 0.958632 0.383108 0.311180 11.00000 0.08559 0.05849 = 0.09715 0.00359 0.05871 0.01194 C27 1 1.081748 0.366519 0.339045 11.00000 0.09115 0.09017 = 0.10449 0.02297 0.06083 0.02918 AFIX 43 H27 2 1.116125 0.338365 0.398757 11.00000 -1.20000 AFIX 0 C28 1 1.156950 0.390466 0.280824 11.00000 0.07859 0.09607 = 0.10184 -0.00161 0.05286 0.00930 AFIX 43 H28 2 1.241794 0.378899 0.302054 11.00000 -1.20000 AFIX 0 C29 1 1.107750 0.430672 0.193057 11.00000 0.09340 0.06345 = 0.09099 -0.01092 0.05717 -0.01101 C30 1 0.983157 0.447417 0.163488 11.00000 0.10034 0.06942 = 0.09218 0.00897 0.04927 0.00243 AFIX 43 H30 2 0.948329 0.475122 0.102756 11.00000 -1.20000 AFIX 0 C31 1 0.909974 0.423802 0.222347 11.00000 0.07740 0.06920 = 0.09930 0.00625 0.04611 0.00930 AFIX 43 H31 2 0.825368 0.435622 0.201625 11.00000 -1.20000 AFIX 0 C32 1 1.305027 0.444098 0.166406 11.00000 0.12413 0.15173 = 0.18495 -0.01903 0.10859 -0.03698 AFIX 137 H32A 2 1.345866 0.450664 0.255205 11.00000 -1.50000 H32B 2 1.342723 0.468204 0.121911 11.00000 -1.50000 H32C 2 1.316682 0.405380 0.148314 11.00000 -1.50000 AFIX 0 N1 3 0.883454 0.356021 0.370298 11.00000 0.11246 0.05379 = 0.14466 0.01349 0.09595 0.01853 O1 4 0.891154 0.123543 0.385507 11.00000 0.12224 0.05767 = 0.11775 0.00676 0.05856 0.00902 O2 4 1.172729 0.455899 0.127956 11.00000 0.12819 0.08987 = 0.13349 -0.00562 0.09013 -0.02080 HKLF 4 END ; #===END data_6_13srv321 _audit_creation_date 2013-12-14 _audit_creation_method ; Olex2 1.2-beta (compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C72 H52 N4 O4' _chemical_formula_sum 'C72 H52 N4 O4' _chemical_formula_weight 1037.18 _chemical_melting_point ? 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' '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' _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.9916(6) _cell_length_b 15.6617(9) _cell_length_c 18.6841(11) _cell_angle_alpha 67.994(2) _cell_angle_beta 85.859(2) _cell_angle_gamma 89.203(2) _cell_volume 2703.4(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9959 _cell_measurement_temperature 120.0 _cell_measurement_theta_max 30.95 _cell_measurement_theta_min 2.25 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0778 before and 0.0403 after correction. The Ratio of minimum to maximum transmission is 0.9585. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'clear light red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1088 _exptl_crystal_size_max 0.357 _exptl_crystal_size_mid 0.209 _exptl_crystal_size_min 0.102 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_unetI/netI 0.0509 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 42578 _diffrn_reflns_theta_full 29.50 _diffrn_reflns_theta_max 29.50 _diffrn_reflns_theta_min 2.25 _diffrn_ambient_temperature 120.0 _diffrn_detector 'Bruker PHOTON 100 CMOS' _diffrn_detector_area_resol_mean ? _diffrn_detector_type 'CMOS sensor' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'Bruker D8 Venture' _diffrn_measurement_device_type D8Venture _diffrn_measurement_method \w-scan _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_probe X-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_special_details ? _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_number_gt 10034 _reflns_number_total 15058 _reflns_threshold_expression >2sigma(I) _computing.bruker_data_scaling 'SADABS V2012/1 (Bruker AXS Inc.)' _computing_cell_refinement 'APEX2 v.2013.4_1 (Bruker, 2013)' _computing_data_collection 'APEX2 v.2013.4_1 (Bruker, 2013)' _computing_data_reduction 'SAINT v8.30C (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _refine_diff_density_max 0.392 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.055 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 929 _refine_ls_number_reflns 15058 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0949 _refine_ls_R_factor_gt 0.0563 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.2300P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1321 _refine_ls_wR_factor_ref 0.1490 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; ; _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_refinement_flags_posn O1 O -0.03033(11) -0.11130(8) 0.49902(6) 0.0339(3) Uani 1 1 d . . . O2 O 0.35827(11) -0.20785(7) 0.07533(6) 0.0283(2) Uani 1 1 d . . . O3 O 0.16163(13) 1.17489(7) -0.09780(6) 0.0350(3) Uani 1 1 d . . . O4 O 0.53474(12) 0.88835(8) -0.46243(7) 0.0378(3) Uani 1 1 d . . . N1 N -0.55391(16) 0.30041(12) 0.71306(8) 0.0446(4) Uani 1 1 d . . . N2 N 1.02143(15) 0.67857(11) -0.67723(8) 0.0372(3) Uani 1 1 d . . . N3 N 0.22537(13) 0.05310(8) 0.20394(7) 0.0259(3) Uani 1 1 d . . . N4 N 0.25970(13) 0.87550(8) -0.18719(7) 0.0273(3) Uani 1 1 d . . . C1 C 0.27763(14) 0.43567(9) 0.01674(8) 0.0198(3) Uani 1 1 d . . . C2 C 0.21046(14) 0.50531(9) 0.03103(8) 0.0198(3) Uani 1 1 d . . . C3 C 0.11666(14) 0.48424(9) 0.09675(8) 0.0215(3) Uani 1 1 d . . . C4 C 0.03965(15) 0.46590(10) 0.15284(8) 0.0239(3) Uani 1 1 d . . . C5 C -0.04295(15) 0.43934(10) 0.22380(8) 0.0238(3) Uani 1 1 d . . . C6 C -0.16214(16) 0.48519(11) 0.22829(9) 0.0273(3) Uani 1 1 d . . . C7 C -0.23757(17) 0.46208(12) 0.29807(9) 0.0311(4) Uani 1 1 d . . . C8 C -0.19528(16) 0.39316(11) 0.36460(9) 0.0300(4) Uani 1 1 d . . . C9 C -0.07875(18) 0.34557(12) 0.35969(9) 0.0335(4) Uani 1 1 d . . . C10 C -0.00361(17) 0.36837(11) 0.28995(9) 0.0309(4) Uani 1 1 d . . . C11 C -0.27088(18) 0.37301(12) 0.43756(10) 0.0349(4) Uani 1 1 d . . . C12 C -0.33289(17) 0.35987(12) 0.49794(9) 0.0340(4) Uani 1 1 d . . . C13 C -0.40736(16) 0.34113(11) 0.57064(9) 0.0271(3) Uani 1 1 d . . . C14 C -0.53480(18) 0.37628(13) 0.57511(10) 0.0387(4) Uani 1 1 d . . . C15 C -0.60212(19) 0.35339(14) 0.64755(11) 0.0416(4) Uani 1 1 d . . . C16 C -0.4324(2) 0.26781(15) 0.70765(11) 0.0500(5) Uani 1 1 d . . . C17 C -0.35637(19) 0.28597(12) 0.63932(10) 0.0378(4) Uani 1 1 d . . . C18 C 0.36186(15) 0.45493(9) -0.05266(8) 0.0217(3) Uani 1 1 d . . . C19 C 0.43601(15) 0.47004(10) -0.10973(8) 0.0239(3) Uani 1 1 d . . . C20 C 0.52022(15) 0.49839(10) -0.18006(8) 0.0247(3) Uani 1 1 d . . . C21 C 0.51378(16) 0.58906(11) -0.23315(9) 0.0270(3) Uani 1 1 d . . . C22 C 0.59020(16) 0.61749(11) -0.30306(9) 0.0286(3) Uani 1 1 d . . . C23 C 0.67354(16) 0.55555(11) -0.32169(9) 0.0280(3) Uani 1 1 d . . . C24 C 0.68298(19) 0.46606(12) -0.26789(10) 0.0372(4) Uani 1 1 d . . . C25 C 0.60781(18) 0.43776(12) -0.19770(10) 0.0350(4) Uani 1 1 d . . . C26 C 0.74754(17) 0.58352(11) -0.39579(9) 0.0303(4) Uani 1 1 d . . . C27 C 0.80746(16) 0.60531(11) -0.45796(9) 0.0295(3) Uani 1 1 d . . . C28 C 0.87990(15) 0.63030(11) -0.53205(8) 0.0264(3) Uani 1 1 d . . . C29 C 0.92040(18) 0.72065(12) -0.57477(9) 0.0323(4) Uani 1 1 d . . . C30 C 0.98968(18) 0.74068(13) -0.64606(10) 0.0371(4) Uani 1 1 d . . . C31 C 0.98084(17) 0.59269(13) -0.63631(10) 0.0335(4) Uani 1 1 d . . . C32 C 0.91053(16) 0.56521(11) -0.56478(9) 0.0289(3) Uani 1 1 d . . . C33 C 0.26206(14) 0.33688(9) 0.06762(8) 0.0194(3) Uani 1 1 d . . . C34 C 0.24589(15) 0.27170(10) 0.03455(8) 0.0218(3) Uani 1 1 d . . . C35 C 0.23043(15) 0.17903(10) 0.07899(8) 0.0218(3) Uani 1 1 d . . . C36 C 0.23431(14) 0.14759(9) 0.15925(8) 0.0210(3) Uani 1 1 d . . . C37 C 0.25150(15) 0.21208(10) 0.19314(8) 0.0231(3) Uani 1 1 d . . . C38 C 0.26399(15) 0.30487(10) 0.14833(8) 0.0215(3) Uani 1 1 d . . . C39 C 0.15954(15) 0.01724(9) 0.27956(8) 0.0221(3) Uani 1 1 d . . . C40 C 0.03908(16) 0.05159(10) 0.29801(9) 0.0258(3) Uani 1 1 d . . . C41 C -0.02688(16) 0.01102(11) 0.37102(9) 0.0267(3) Uani 1 1 d . . . C42 C 0.02680(15) -0.06521(10) 0.42578(8) 0.0245(3) Uani 1 1 d . . . C43 C 0.14770(15) -0.09985(10) 0.40781(9) 0.0251(3) Uani 1 1 d . . . C44 C 0.21363(15) -0.05875(10) 0.33570(8) 0.0232(3) Uani 1 1 d . . . C45 C -0.16729(19) -0.09183(15) 0.51354(12) 0.0407(4) Uani 1 1 d . . . C46 C 0.26128(15) -0.01153(9) 0.16864(8) 0.0220(3) Uani 1 1 d . . . C47 C 0.39067(15) -0.01282(10) 0.13740(8) 0.0232(3) Uani 1 1 d . . . C48 C 0.42697(15) -0.07603(10) 0.10398(8) 0.0231(3) Uani 1 1 d . . . C49 C 0.33236(15) -0.13987(9) 0.10362(8) 0.0217(3) Uani 1 1 d . . . C50 C 0.20189(16) -0.13847(10) 0.13436(9) 0.0254(3) Uani 1 1 d . . . C51 C 0.16612(16) -0.07433(10) 0.16619(9) 0.0246(3) Uani 1 1 d . . . C52 C 0.49116(18) -0.21118(12) 0.04372(11) 0.0334(4) Uani 1 1 d . . . C53 C 0.22459(14) 0.60359(9) -0.02179(8) 0.0201(3) Uani 1 1 d . . . C54 C 0.11238(15) 0.65896(10) -0.03921(9) 0.0251(3) Uani 1 1 d . . . C55 C 0.12265(16) 0.74861(10) -0.09299(9) 0.0280(3) Uani 1 1 d . . . C56 C 0.24691(15) 0.78463(9) -0.12901(8) 0.0239(3) Uani 1 1 d . . . C57 C 0.36033(15) 0.73143(10) -0.10930(9) 0.0244(3) Uani 1 1 d . . . C58 C 0.34955(15) 0.64196(10) -0.05628(8) 0.0227(3) Uani 1 1 d . . . C59 C 0.23690(14) 0.95283(10) -0.16666(8) 0.0230(3) Uani 1 1 d . . . C60 C 0.22022(16) 0.94269(11) -0.08888(9) 0.0274(3) Uani 1 1 d . . . C61 C 0.19415(17) 1.01734(11) -0.06844(9) 0.0288(3) Uani 1 1 d . . . C62 C 0.18735(16) 1.10527(10) -0.12451(9) 0.0258(3) Uani 1 1 d . . . C63 C 0.20675(16) 1.11685(10) -0.20187(9) 0.0260(3) Uani 1 1 d . . . C64 C 0.22858(15) 1.04126(10) -0.22243(9) 0.0256(3) Uani 1 1 d . . . C65 C 0.1447(2) 1.26452(11) -0.15428(10) 0.0331(4) Uani 1 1 d . . . C66 C 0.32776(15) 0.88135(10) -0.25870(8) 0.0241(3) Uani 1 1 d . . . C67 C 0.43905(16) 0.93889(11) -0.29213(9) 0.0280(3) Uani 1 1 d . . . C68 C 0.50470(17) 0.93933(11) -0.36002(9) 0.0304(4) Uani 1 1 d . . . C69 C 0.46146(15) 0.88248(10) -0.39567(9) 0.0269(3) Uani 1 1 d . . . C70 C 0.35242(16) 0.82418(11) -0.36262(9) 0.0280(3) Uani 1 1 d . . . C71 C 0.28666(16) 0.82450(10) -0.29473(10) 0.0286(3) Uani 1 1 d . . . C72 C 0.4964(2) 0.83059(14) -0.50055(11) 0.0388(4) Uani 1 1 d . . . H6 H -0.1902(17) 0.5330(12) 0.1819(10) 0.031(4) Uiso 1 1 d . . . H7 H -0.3218(19) 0.4945(12) 0.2994(10) 0.039(5) Uiso 1 1 d . . . H9 H -0.0481(19) 0.2970(13) 0.4050(11) 0.041(5) Uiso 1 1 d . . . H10 H 0.0792(19) 0.3381(13) 0.2858(10) 0.040(5) Uiso 1 1 d . . . H14 H -0.576(2) 0.4163(14) 0.5261(12) 0.053(6) Uiso 1 1 d . . . H15 H -0.691(2) 0.3749(15) 0.6503(12) 0.058(6) Uiso 1 1 d . . . H16 H -0.395(2) 0.2306(16) 0.7577(14) 0.067(7) Uiso 1 1 d . . . H17 H -0.265(2) 0.2608(14) 0.6396(11) 0.053(6) Uiso 1 1 d . . . H21 H 0.4549(18) 0.6329(12) -0.2206(10) 0.037(5) Uiso 1 1 d . . . H22 H 0.5808(18) 0.6826(13) -0.3419(10) 0.038(5) Uiso 1 1 d . . . H24 H 0.746(2) 0.4205(13) -0.2795(11) 0.049(6) Uiso 1 1 d . . . H25 H 0.6157(18) 0.3751(13) -0.1608(11) 0.041(5) Uiso 1 1 d . . . H29 H 0.8941(18) 0.7696(13) -0.5537(11) 0.043(5) Uiso 1 1 d . . . H30 H 1.0179(19) 0.8065(14) -0.6786(11) 0.048(5) Uiso 1 1 d . . . H31 H 1.0039(19) 0.5453(13) -0.6606(11) 0.047(5) Uiso 1 1 d . . . H32 H 0.8843(19) 0.5019(13) -0.5376(11) 0.041(5) Uiso 1 1 d . . . H34 H 0.2415(17) 0.2924(11) -0.0217(10) 0.031(4) Uiso 1 1 d . . . H35 H 0.2181(15) 0.1356(11) 0.0563(9) 0.022(4) Uiso 1 1 d . . . H37 H 0.2586(16) 0.1912(11) 0.2483(10) 0.025(4) Uiso 1 1 d . . . H38 H 0.2770(17) 0.3486(12) 0.1727(10) 0.031(4) Uiso 1 1 d . . . H40 H 0.0000(17) 0.1043(12) 0.2585(10) 0.031(4) Uiso 1 1 d . . . H41 H -0.1087(18) 0.0370(12) 0.3824(10) 0.034(5) Uiso 1 1 d . . . H43 H 0.1838(19) -0.1509(14) 0.4463(11) 0.046(5) Uiso 1 1 d . . . H44 H 0.2976(17) -0.0813(11) 0.3223(9) 0.029(4) Uiso 1 1 d . . . H45A H -0.2252(19) -0.1022(13) 0.4756(11) 0.040(5) Uiso 1 1 d . . . H45B H -0.1813(18) -0.0265(13) 0.5100(10) 0.040(5) Uiso 1 1 d . . . H45C H -0.195(2) -0.1377(14) 0.5662(13) 0.054(6) Uiso 1 1 d . . . H47 H 0.4548(17) 0.0312(11) 0.1395(9) 0.027(4) Uiso 1 1 d . . . H48 H 0.5186(16) -0.0767(10) 0.0828(8) 0.019(4) Uiso 1 1 d . . . H50 H 0.1347(18) -0.1837(12) 0.1322(10) 0.037(5) Uiso 1 1 d . . . H51 H 0.0759(18) -0.0704(11) 0.1857(10) 0.032(4) Uiso 1 1 d . . . H52A H 0.5554(18) -0.2203(11) 0.0830(10) 0.030(4) Uiso 1 1 d . . . H52B H 0.4893(16) -0.2646(12) 0.0278(9) 0.027(4) Uiso 1 1 d . . . H52C H 0.5120(19) -0.1506(14) -0.0007(11) 0.044(5) Uiso 1 1 d . . . H54 H 0.0208(19) 0.6346(12) -0.0144(10) 0.037(5) Uiso 1 1 d . . . H55 H 0.0463(18) 0.7855(12) -0.1057(10) 0.035(5) Uiso 1 1 d . . . H57 H 0.4479(16) 0.7571(11) -0.1314(9) 0.024(4) Uiso 1 1 d . . . H58 H 0.4291(17) 0.6066(11) -0.0420(9) 0.024(4) Uiso 1 1 d . . . H60 H 0.2270(17) 0.8850(12) -0.0493(10) 0.034(5) Uiso 1 1 d . . . H61 H 0.1789(16) 1.0130(11) -0.0178(10) 0.026(4) Uiso 1 1 d . . . H63 H 0.2030(18) 1.1753(13) -0.2414(11) 0.039(5) Uiso 1 1 d . . . H64 H 0.2403(16) 1.0520(11) -0.2773(10) 0.027(4) Uiso 1 1 d . . . H65A H 0.0700(18) 1.2641(11) -0.1882(10) 0.033(5) Uiso 1 1 d . . . H65B H 0.2317(19) 1.2884(12) -0.1839(11) 0.040(5) Uiso 1 1 d . . . H65C H 0.1095(17) 1.3012(12) -0.1246(10) 0.033(5) Uiso 1 1 d . . . H67 H 0.4688(16) 0.9786(11) -0.2680(9) 0.027(4) Uiso 1 1 d . . . H68 H 0.5820(18) 0.9803(12) -0.3842(10) 0.034(5) Uiso 1 1 d . . . H70 H 0.3247(17) 0.7835(12) -0.3848(10) 0.029(4) Uiso 1 1 d . . . H71 H 0.2147(19) 0.7857(13) -0.2722(10) 0.039(5) Uiso 1 1 d . . . H72A H 0.509(2) 0.7629(16) -0.4649(13) 0.058(6) Uiso 1 1 d . . . H72B H 0.402(2) 0.8432(13) -0.5163(11) 0.046(5) Uiso 1 1 d . . . H72C H 0.5622(19) 0.8438(13) -0.5486(12) 0.046(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0346(6) 0.0395(7) 0.0240(6) -0.0098(5) 0.0116(5) -0.0060(5) O2 0.0339(6) 0.0205(5) 0.0303(6) -0.0108(5) 0.0064(5) 0.0027(4) O3 0.0588(8) 0.0204(5) 0.0253(6) -0.0074(5) -0.0065(5) 0.0009(5) O4 0.0366(7) 0.0469(7) 0.0358(6) -0.0243(6) 0.0102(5) -0.0104(5) N1 0.0443(9) 0.0586(11) 0.0284(8) -0.0151(8) 0.0093(7) -0.0099(8) N2 0.0361(8) 0.0495(9) 0.0245(7) -0.0131(7) 0.0048(6) -0.0103(7) N3 0.0362(7) 0.0157(6) 0.0219(6) -0.0050(5) 0.0102(5) -0.0002(5) N4 0.0341(7) 0.0148(6) 0.0243(6) 0.0005(5) 0.0100(5) 0.0023(5) C1 0.0208(7) 0.0180(7) 0.0172(6) -0.0031(6) 0.0016(5) -0.0004(5) C2 0.0216(7) 0.0159(6) 0.0187(7) -0.0036(5) 0.0025(5) -0.0007(5) C3 0.0252(7) 0.0147(6) 0.0227(7) -0.0054(6) 0.0021(6) 0.0007(5) C4 0.0267(8) 0.0180(7) 0.0248(7) -0.0066(6) 0.0038(6) -0.0009(6) C5 0.0260(8) 0.0223(7) 0.0221(7) -0.0086(6) 0.0068(6) -0.0055(6) C6 0.0296(8) 0.0278(8) 0.0243(8) -0.0104(7) 0.0029(6) -0.0013(6) C7 0.0285(9) 0.0366(9) 0.0312(8) -0.0177(8) 0.0070(7) -0.0038(7) C8 0.0314(9) 0.0355(9) 0.0240(8) -0.0136(7) 0.0089(6) -0.0136(7) C9 0.0366(9) 0.0344(9) 0.0222(8) -0.0031(7) 0.0040(7) -0.0074(7) C10 0.0292(9) 0.0309(9) 0.0267(8) -0.0056(7) 0.0066(7) -0.0005(7) C11 0.0374(9) 0.0380(9) 0.0294(8) -0.0142(7) 0.0086(7) -0.0132(7) C12 0.0358(9) 0.0367(9) 0.0286(8) -0.0127(7) 0.0075(7) -0.0106(7) C13 0.0301(8) 0.0268(8) 0.0233(7) -0.0090(6) 0.0057(6) -0.0072(6) C14 0.0352(10) 0.0466(11) 0.0297(9) -0.0090(8) -0.0030(7) 0.0061(8) C15 0.0278(9) 0.0572(12) 0.0451(11) -0.0269(10) 0.0061(8) 0.0015(8) C16 0.0532(13) 0.0569(13) 0.0243(9) 0.0017(9) 0.0010(9) 0.0058(10) C17 0.0338(10) 0.0376(10) 0.0339(9) -0.0052(8) 0.0019(7) 0.0066(8) C18 0.0259(7) 0.0155(7) 0.0206(7) -0.0036(6) 0.0000(6) 0.0032(5) C19 0.0277(8) 0.0199(7) 0.0215(7) -0.0055(6) 0.0016(6) 0.0025(6) C20 0.0272(8) 0.0252(8) 0.0189(7) -0.0060(6) 0.0035(6) -0.0010(6) C21 0.0298(8) 0.0250(8) 0.0237(7) -0.0074(6) 0.0040(6) 0.0007(6) C22 0.0327(9) 0.0263(8) 0.0211(7) -0.0032(7) 0.0027(6) -0.0017(6) C23 0.0297(8) 0.0316(8) 0.0213(7) -0.0095(7) 0.0059(6) -0.0073(6) C24 0.0434(10) 0.0311(9) 0.0323(9) -0.0099(8) 0.0164(8) 0.0018(8) C25 0.0432(10) 0.0254(9) 0.0278(8) -0.0030(7) 0.0132(7) 0.0038(7) C26 0.0337(9) 0.0302(8) 0.0252(8) -0.0093(7) 0.0049(7) -0.0061(7) C27 0.0333(9) 0.0288(8) 0.0249(8) -0.0094(7) 0.0042(7) -0.0064(7) C28 0.0267(8) 0.0303(8) 0.0202(7) -0.0079(6) 0.0020(6) -0.0049(6) C29 0.0402(10) 0.0289(9) 0.0256(8) -0.0087(7) 0.0037(7) -0.0065(7) C30 0.0437(10) 0.0360(10) 0.0249(8) -0.0044(8) 0.0038(7) -0.0150(8) C31 0.0305(9) 0.0438(10) 0.0289(8) -0.0174(8) 0.0015(7) -0.0013(7) C32 0.0334(9) 0.0269(8) 0.0243(8) -0.0076(7) 0.0019(6) -0.0034(7) C33 0.0200(7) 0.0157(7) 0.0184(6) -0.0028(5) 0.0040(5) 0.0018(5) C34 0.0243(7) 0.0200(7) 0.0192(7) -0.0061(6) 0.0026(6) 0.0043(6) C35 0.0245(8) 0.0180(7) 0.0233(7) -0.0091(6) 0.0028(6) 0.0009(5) C36 0.0210(7) 0.0161(7) 0.0226(7) -0.0047(6) 0.0055(6) 0.0008(5) C37 0.0295(8) 0.0205(7) 0.0166(7) -0.0044(6) 0.0016(6) 0.0015(6) C38 0.0259(8) 0.0173(7) 0.0204(7) -0.0066(6) 0.0016(6) 0.0012(6) C39 0.0265(8) 0.0177(7) 0.0197(7) -0.0053(6) 0.0042(6) -0.0030(6) C40 0.0290(8) 0.0219(8) 0.0244(8) -0.0066(6) -0.0004(6) 0.0047(6) C41 0.0235(8) 0.0292(8) 0.0295(8) -0.0145(7) 0.0037(6) 0.0025(6) C42 0.0280(8) 0.0256(8) 0.0199(7) -0.0093(6) 0.0045(6) -0.0076(6) C43 0.0266(8) 0.0216(7) 0.0227(7) -0.0036(6) -0.0005(6) -0.0006(6) C44 0.0207(7) 0.0208(7) 0.0259(7) -0.0070(6) 0.0037(6) -0.0005(6) C45 0.0352(10) 0.0530(12) 0.0370(10) -0.0229(10) 0.0147(8) -0.0105(9) C46 0.0282(8) 0.0152(7) 0.0191(7) -0.0035(6) 0.0036(6) 0.0029(6) C47 0.0243(8) 0.0193(7) 0.0225(7) -0.0046(6) 0.0028(6) -0.0031(6) C48 0.0209(7) 0.0222(7) 0.0214(7) -0.0035(6) 0.0038(6) 0.0025(6) C49 0.0284(8) 0.0149(7) 0.0180(7) -0.0024(6) 0.0016(6) 0.0049(5) C50 0.0273(8) 0.0195(7) 0.0261(8) -0.0061(6) 0.0051(6) -0.0033(6) C51 0.0237(8) 0.0201(7) 0.0253(7) -0.0048(6) 0.0080(6) 0.0002(6) C52 0.0360(10) 0.0286(9) 0.0352(9) -0.0135(8) 0.0075(8) 0.0047(7) C53 0.0249(7) 0.0151(6) 0.0179(7) -0.0044(5) 0.0039(6) -0.0006(5) C54 0.0221(8) 0.0211(7) 0.0262(8) -0.0034(6) 0.0064(6) 0.0004(6) C55 0.0238(8) 0.0212(8) 0.0308(8) -0.0016(7) 0.0037(6) 0.0054(6) C56 0.0287(8) 0.0148(7) 0.0230(7) -0.0020(6) 0.0041(6) 0.0009(6) C57 0.0233(8) 0.0194(7) 0.0259(7) -0.0046(6) 0.0059(6) -0.0023(6) C58 0.0213(7) 0.0198(7) 0.0241(7) -0.0055(6) 0.0004(6) 0.0021(6) C59 0.0217(7) 0.0167(7) 0.0251(7) -0.0020(6) 0.0005(6) 0.0013(5) C60 0.0318(9) 0.0190(7) 0.0233(7) 0.0012(6) -0.0011(6) 0.0013(6) C61 0.0357(9) 0.0267(8) 0.0207(8) -0.0047(7) -0.0037(7) 0.0003(7) C62 0.0301(8) 0.0200(7) 0.0267(8) -0.0075(6) -0.0037(6) -0.0014(6) C63 0.0307(8) 0.0167(7) 0.0244(8) -0.0009(6) -0.0006(6) -0.0007(6) C64 0.0285(8) 0.0206(7) 0.0221(7) -0.0023(6) 0.0015(6) 0.0002(6) C65 0.0457(11) 0.0219(8) 0.0300(9) -0.0077(7) -0.0031(8) 0.0017(7) C66 0.0255(8) 0.0171(7) 0.0234(7) -0.0011(6) 0.0016(6) 0.0031(6) C67 0.0286(8) 0.0273(8) 0.0268(8) -0.0094(7) 0.0017(6) -0.0030(6) C68 0.0277(8) 0.0333(9) 0.0287(8) -0.0109(7) 0.0059(7) -0.0089(7) C69 0.0257(8) 0.0269(8) 0.0262(8) -0.0082(7) 0.0013(6) 0.0004(6) C70 0.0270(8) 0.0226(8) 0.0345(9) -0.0112(7) -0.0004(7) 0.0002(6) C71 0.0256(8) 0.0192(7) 0.0349(9) -0.0040(7) 0.0038(7) -0.0023(6) C72 0.0388(11) 0.0492(12) 0.0343(10) -0.0224(9) -0.0017(8) -0.0030(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C42 1.3704(17) . ? O1 C45 1.427(2) . ? O2 C49 1.3691(17) . ? O2 C52 1.422(2) . ? O3 C62 1.3731(18) . ? O3 C65 1.4218(19) . ? O4 C69 1.3729(18) . ? O4 C72 1.416(2) . ? N1 C15 1.316(2) . ? N1 C16 1.322(3) . ? N2 C30 1.332(2) . ? N2 C31 1.326(2) . ? N3 C36 1.4008(18) . ? N3 C39 1.4232(17) . ? N3 C46 1.4298(18) . ? N4 C56 1.4315(18) . ? N4 C59 1.4119(19) . ? N4 C66 1.4265(18) . ? C1 C2 1.3723(19) . ? C1 C18 1.4272(19) . ? C1 C33 1.4850(18) . ? C2 C3 1.4261(19) . ? C2 C53 1.4869(18) . ? C3 C4 1.1988(19) . ? C4 C5 1.4318(19) . ? C5 C6 1.396(2) . ? C5 C10 1.395(2) . ? C6 C7 1.382(2) . ? C6 H6 0.966(18) . ? C7 C8 1.395(2) . ? C7 H7 0.980(18) . ? C8 C9 1.390(2) . ? C8 C11 1.437(2) . ? C9 C10 1.381(2) . ? C9 H9 0.968(19) . ? C10 H10 0.960(19) . ? C11 C12 1.195(2) . ? C12 C13 1.430(2) . ? C13 C14 1.390(2) . ? C13 C17 1.380(2) . ? C14 C15 1.387(2) . ? C14 H14 1.01(2) . ? C15 H15 0.95(2) . ? C16 C17 1.372(3) . ? C16 H16 1.00(2) . ? C17 H17 0.98(2) . ? C18 C19 1.201(2) . ? C19 C20 1.4300(19) . ? C20 C21 1.398(2) . ? C20 C25 1.395(2) . ? C21 C22 1.385(2) . ? C21 H21 0.980(18) . ? C22 C23 1.394(2) . ? C22 H22 1.013(18) . ? C23 C24 1.392(2) . ? C23 C26 1.436(2) . ? C24 C25 1.383(2) . ? C24 H24 1.02(2) . ? C25 H25 0.971(19) . ? C26 C27 1.197(2) . ? C27 C28 1.432(2) . ? C28 C29 1.388(2) . ? C28 C32 1.392(2) . ? C29 C30 1.383(2) . ? C29 H29 1.008(19) . ? C30 H30 1.012(19) . ? C31 C32 1.381(2) . ? C31 H31 1.02(2) . ? C32 H32 0.959(19) . ? C33 C34 1.393(2) . ? C33 C38 1.4011(19) . ? C34 C35 1.380(2) . ? C34 H34 0.981(17) . ? C35 C36 1.395(2) . ? C35 H35 0.939(16) . ? C36 C37 1.396(2) . ? C37 C38 1.381(2) . ? C37 H37 0.965(16) . ? C38 H38 0.968(17) . ? C39 C40 1.385(2) . ? C39 C44 1.392(2) . ? C40 C41 1.390(2) . ? C40 H40 0.978(18) . ? C41 C42 1.381(2) . ? C41 H41 0.953(18) . ? C42 C43 1.388(2) . ? C43 C44 1.377(2) . ? C43 H43 0.94(2) . ? C44 H44 0.959(17) . ? C45 H45A 1.01(2) . ? C45 H45B 1.008(19) . ? C45 H45C 1.00(2) . ? C46 C47 1.383(2) . ? C46 C51 1.393(2) . ? C47 C48 1.386(2) . ? C47 H47 0.961(17) . ? C48 C49 1.388(2) . ? C48 H48 0.972(15) . ? C49 C50 1.389(2) . ? C50 C51 1.378(2) . ? C50 H50 0.996(18) . ? C51 H51 0.958(18) . ? C52 H52A 0.978(18) . ? C52 H52B 0.989(17) . ? C52 H52C 1.011(19) . ? C53 C54 1.389(2) . ? C53 C58 1.396(2) . ? C54 C55 1.387(2) . ? C54 H54 1.007(18) . ? C55 C56 1.388(2) . ? C55 H55 0.940(18) . ? C56 C57 1.385(2) . ? C57 C58 1.380(2) . ? C57 H57 0.965(16) . ? C58 H58 0.958(16) . ? C59 C60 1.399(2) . ? C59 C64 1.392(2) . ? C60 C61 1.376(2) . ? C60 H60 0.935(18) . ? C61 C62 1.387(2) . ? C61 H61 0.924(16) . ? C62 C63 1.387(2) . ? C63 C64 1.385(2) . ? C63 H63 0.938(19) . ? C64 H64 0.972(16) . ? C65 H65A 1.016(18) . ? C65 H65B 0.993(19) . ? C65 H65C 0.983(18) . ? C66 C67 1.394(2) . ? C66 C71 1.383(2) . ? C67 C68 1.383(2) . ? C67 H67 0.955(17) . ? C68 C69 1.386(2) . ? C68 H68 0.979(17) . ? C69 C70 1.382(2) . ? C70 C71 1.387(2) . ? C70 H70 0.935(17) . ? C71 H71 0.917(19) . ? C72 H72A 1.03(2) . ? C72 H72B 1.00(2) . ? C72 H72C 1.030(19) . ? 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 C42 O1 C45 116.75(14) . . ? C49 O2 C52 116.73(12) . . ? C62 O3 C65 116.95(12) . . ? C69 O4 C72 117.92(13) . . ? C15 N1 C16 116.20(15) . . ? C31 N2 C30 116.33(14) . . ? C36 N3 C39 122.66(11) . . ? C36 N3 C46 119.43(11) . . ? C39 N3 C46 116.95(11) . . ? C59 N4 C56 119.92(12) . . ? C59 N4 C66 123.03(12) . . ? C66 N4 C56 115.14(11) . . ? C2 C1 C18 120.47(12) . . ? C2 C1 C33 123.76(12) . . ? C18 C1 C33 115.65(12) . . ? C1 C2 C3 119.95(12) . . ? C1 C2 C53 122.93(12) . . ? C3 C2 C53 117.02(12) . . ? C4 C3 C2 178.83(17) . . ? C3 C4 C5 174.88(16) . . ? C6 C5 C4 120.65(14) . . ? C10 C5 C4 120.24(14) . . ? C10 C5 C6 119.09(14) . . ? C5 C6 H6 118.7(10) . . ? C7 C6 C5 120.12(15) . . ? C7 C6 H6 121.2(10) . . ? C6 C7 C8 120.48(16) . . ? C6 C7 H7 118.4(11) . . ? C8 C7 H7 121.1(11) . . ? C7 C8 C11 119.96(16) . . ? C9 C8 C7 119.41(14) . . ? C9 C8 C11 120.62(16) . . ? C8 C9 H9 120.8(11) . . ? C10 C9 C8 120.11(16) . . ? C10 C9 H9 119.0(11) . . ? C5 C10 H10 117.8(11) . . ? C9 C10 C5 120.71(16) . . ? C9 C10 H10 121.4(11) . . ? C12 C11 C8 177.33(18) . . ? C11 C12 C13 178.20(18) . . ? C14 C13 C12 121.57(15) . . ? C17 C13 C12 121.27(15) . . ? C17 C13 C14 117.15(15) . . ? C13 C14 H14 119.6(11) . . ? C15 C14 C13 118.27(17) . . ? C15 C14 H14 122.1(11) . . ? N1 C15 C14 124.64(18) . . ? N1 C15 H15 117.1(13) . . ? C14 C15 H15 118.2(13) . . ? N1 C16 C17 124.28(18) . . ? N1 C16 H16 115.5(13) . . ? C17 C16 H16 120.1(13) . . ? C13 C17 H17 120.5(12) . . ? C16 C17 C13 119.45(17) . . ? C16 C17 H17 120.1(12) . . ? C19 C18 C1 178.00(16) . . ? C18 C19 C20 173.72(15) . . ? C21 C20 C19 119.27(14) . . ? C25 C20 C19 121.82(14) . . ? C25 C20 C21 118.91(14) . . ? C20 C21 H21 119.7(10) . . ? C22 C21 C20 120.57(15) . . ? C22 C21 H21 119.8(10) . . ? C21 C22 C23 120.24(15) . . ? C21 C22 H22 119.4(10) . . ? C23 C22 H22 120.3(10) . . ? C22 C23 C26 120.36(14) . . ? C24 C23 C22 119.18(14) . . ? C24 C23 C26 120.46(15) . . ? C23 C24 H24 120.4(11) . . ? C25 C24 C23 120.66(16) . . ? C25 C24 H24 118.9(11) . . ? C20 C25 H25 120.0(10) . . ? C24 C25 C20 120.38(15) . . ? C24 C25 H25 119.6(10) . . ? C27 C26 C23 178.42(17) . . ? C26 C27 C28 179.30(19) . . ? C29 C28 C27 121.38(14) . . ? C29 C28 C32 117.27(14) . . ? C32 C28 C27 121.34(14) . . ? C28 C29 H29 118.6(10) . . ? C30 C29 C28 118.78(16) . . ? C30 C29 H29 122.6(10) . . ? N2 C30 C29 124.35(16) . . ? N2 C30 H30 115.9(11) . . ? C29 C30 H30 119.8(11) . . ? N2 C31 C32 124.10(16) . . ? N2 C31 H31 116.3(11) . . ? C32 C31 H31 119.6(11) . . ? C28 C32 H32 120.4(11) . . ? C31 C32 C28 119.16(15) . . ? C31 C32 H32 120.4(11) . . ? C34 C33 C1 119.33(12) . . ? C34 C33 C38 117.50(12) . . ? C38 C33 C1 123.17(13) . . ? C33 C34 H34 119.2(10) . . ? C35 C34 C33 121.85(13) . . ? C35 C34 H34 118.9(10) . . ? C34 C35 C36 120.27(13) . . ? C34 C35 H35 121.3(9) . . ? C36 C35 H35 118.4(9) . . ? C35 C36 N3 120.23(13) . . ? C35 C36 C37 118.48(13) . . ? C37 C36 N3 121.26(13) . . ? C36 C37 H37 119.5(9) . . ? C38 C37 C36 120.81(13) . . ? C38 C37 H37 119.7(10) . . ? C33 C38 H38 119.2(10) . . ? C37 C38 C33 121.06(13) . . ? C37 C38 H38 119.7(10) . . ? C40 C39 N3 122.33(13) . . ? C40 C39 C44 118.68(13) . . ? C44 C39 N3 118.86(13) . . ? C39 C40 C41 120.79(14) . . ? C39 C40 H40 118.9(10) . . ? C41 C40 H40 120.3(10) . . ? C40 C41 H41 118.9(10) . . ? C42 C41 C40 119.94(14) . . ? C42 C41 H41 121.2(10) . . ? O1 C42 C41 124.88(14) . . ? O1 C42 C43 115.52(14) . . ? C41 C42 C43 119.60(13) . . ? C42 C43 H43 118.4(12) . . ? C44 C43 C42 120.29(14) . . ? C44 C43 H43 121.3(12) . . ? C39 C44 H44 117.8(10) . . ? C43 C44 C39 120.68(14) . . ? C43 C44 H44 121.5(10) . . ? O1 C45 H45A 110.9(10) . . ? O1 C45 H45B 113.2(11) . . ? O1 C45 H45C 105.5(12) . . ? H45A C45 H45B 107.4(15) . . ? H45A C45 H45C 107.8(16) . . ? H45B C45 H45C 112.0(15) . . ? C47 C46 N3 120.41(13) . . ? C47 C46 C51 119.52(13) . . ? C51 C46 N3 120.06(13) . . ? C46 C47 C48 120.86(14) . . ? C46 C47 H47 118.3(10) . . ? C48 C47 H47 120.9(10) . . ? C47 C48 C49 119.18(14) . . ? C47 C48 H48 120.0(9) . . ? C49 C48 H48 120.8(9) . . ? O2 C49 C48 124.29(13) . . ? O2 C49 C50 115.47(13) . . ? C48 C49 C50 120.23(13) . . ? C49 C50 H50 119.0(10) . . ? C51 C50 C49 120.15(14) . . ? C51 C50 H50 120.8(10) . . ? C46 C51 H51 118.4(10) . . ? C50 C51 C46 120.02(14) . . ? C50 C51 H51 121.6(10) . . ? O2 C52 H52A 110.3(10) . . ? O2 C52 H52B 104.1(9) . . ? O2 C52 H52C 108.4(11) . . ? H52A C52 H52B 111.0(14) . . ? H52A C52 H52C 109.2(15) . . ? H52B C52 H52C 113.7(14) . . ? C54 C53 C2 120.35(12) . . ? C54 C53 C58 118.42(13) . . ? C58 C53 C2 121.21(13) . . ? C53 C54 H54 121.0(10) . . ? C55 C54 C53 120.93(14) . . ? C55 C54 H54 118.0(10) . . ? C54 C55 C56 119.89(14) . . ? C54 C55 H55 120.8(11) . . ? C56 C55 H55 119.3(11) . . ? C55 C56 N4 121.10(13) . . ? C57 C56 N4 119.30(13) . . ? C57 C56 C55 119.59(13) . . ? C56 C57 H57 120.3(9) . . ? C58 C57 C56 120.32(14) . . ? C58 C57 H57 119.3(9) . . ? C53 C58 H58 119.9(10) . . ? C57 C58 C53 120.72(14) . . ? C57 C58 H58 119.4(10) . . ? C60 C59 N4 120.71(13) . . ? C64 C59 N4 121.66(13) . . ? C64 C59 C60 117.63(14) . . ? C59 C60 H60 120.9(10) . . ? C61 C60 C59 121.05(14) . . ? C61 C60 H60 118.1(10) . . ? C60 C61 C62 120.81(15) . . ? C60 C61 H61 123.5(10) . . ? C62 C61 H61 115.7(10) . . ? O3 C62 C61 116.06(14) . . ? O3 C62 C63 125.05(13) . . ? C63 C62 C61 118.90(14) . . ? C62 C63 H63 121.3(11) . . ? C64 C63 C62 120.22(14) . . ? C64 C63 H63 118.4(11) . . ? C59 C64 H64 120.8(10) . . ? C63 C64 C59 121.34(14) . . ? C63 C64 H64 117.8(10) . . ? O3 C65 H65A 110.5(10) . . ? O3 C65 H65B 109.9(11) . . ? O3 C65 H65C 104.8(10) . . ? H65A C65 H65B 113.5(14) . . ? H65A C65 H65C 104.6(14) . . ? H65B C65 H65C 113.3(15) . . ? C67 C66 N4 122.63(14) . . ? C71 C66 N4 119.08(13) . . ? C71 C66 C67 118.21(14) . . ? C66 C67 H67 119.3(10) . . ? C68 C67 C66 120.37(15) . . ? C68 C67 H67 120.3(10) . . ? C67 C68 C69 120.64(15) . . ? C67 C68 H68 120.8(10) . . ? C69 C68 H68 118.6(10) . . ? O4 C69 C68 115.54(13) . . ? O4 C69 C70 124.84(14) . . ? C70 C69 C68 119.62(14) . . ? C69 C70 C71 119.39(15) . . ? C69 C70 H70 120.5(10) . . ? C71 C70 H70 120.0(10) . . ? C66 C71 C70 121.77(14) . . ? C66 C71 H71 118.3(11) . . ? C70 C71 H71 119.9(11) . . ? O4 C72 H72A 109.0(12) . . ? O4 C72 H72B 110.9(11) . . ? O4 C72 H72C 107.2(11) . . ? H72A C72 H72B 112.1(16) . . ? H72A C72 H72C 107.2(16) . . ? H72B C72 H72C 110.2(15) . . ? 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 C1 C2 C53 C54 137.06(15) . . . . ? C1 C2 C53 C58 -41.6(2) . . . . ? C2 C1 C33 C34 134.42(15) . . . . ? C2 C1 C33 C38 -46.2(2) . . . . ? C3 C2 C53 C54 -39.46(19) . . . . ? C3 C2 C53 C58 141.90(14) . . . . ? C18 C1 C33 C34 -41.53(19) . . . . ? C18 C1 C33 C38 137.85(14) . . . . ? C35 C36 N3 C39 -145.52(14) . . . . ? C35 C36 N3 C46 22.9(2) . . . . ? C37 C36 N3 C39 36.5(2) . . . . ? C37 C36 N3 C46 -155.07(14) . . . . ? C40 C39 N3 C36 41.5(2) . . . . ? C40 C39 N3 C46 -127.20(15) . . . . ? C41 C42 O1 C45 14.4(2) . . . . ? C43 C42 O1 C45 -165.77(14) . . . . ? C44 C39 N3 C36 -142.68(15) . . . . ? C44 C39 N3 C46 48.66(19) . . . . ? C47 C46 N3 C36 62.04(19) . . . . ? C47 C46 N3 C39 -128.92(15) . . . . ? C48 C49 O2 C52 -0.8(2) . . . . ? C50 C49 O2 C52 -179.80(14) . . . . ? C51 C46 N3 C36 -118.58(15) . . . . ? C51 C46 N3 C39 50.46(19) . . . . ? C55 C56 N4 C59 69.0(2) . . . . ? C55 C56 N4 C66 -126.32(16) . . . . ? C57 C56 N4 C59 -112.02(16) . . . . ? C57 C56 N4 C66 52.71(19) . . . . ? C60 C59 N4 C56 8.9(2) . . . . ? C60 C59 N4 C66 -154.54(15) . . . . ? C61 C62 O3 C65 -175.63(15) . . . . ? C63 C62 O3 C65 4.5(2) . . . . ? C64 C59 N4 C56 -170.28(14) . . . . ? C64 C59 N4 C66 26.2(2) . . . . ? C67 C66 N4 C56 -125.18(16) . . . . ? C67 C66 N4 C59 39.0(2) . . . . ? C68 C69 O4 C72 178.92(15) . . . . ? C70 C69 O4 C72 0.0(2) . . . . ? C71 C66 N4 C56 51.42(19) . . . . ? C71 C66 N4 C59 -144.38(15) . . . . ? _iucr_refine_instructions_details ; TITL 13srv321 in P-1 CELL 0.71073 9.9916 15.6617 18.6841 67.994 85.859 89.203 ZERR 2 0.0006 0.0009 0.0011 0.002 0.002 0.002 LATT 1 SFAC C H N O UNIT 144 104 8 8 L.S. 9 PLAN 5 CONF C2 C1 C33 C34 CONF C18 C1 C33 C34 CONF C2 C1 C33 C38 CONF C18 C1 C33 C38 CONF C1 C2 C53 C54 CONF C3 C2 C53 C54 CONF C1 C2 C53 C58 CONF C3 C2 C53 C58 CONF C35 C36 N3 C39 CONF C37 C36 N3 C39 CONF C35 C36 N3 C46 CONF C37 C36 N3 C46 CONF C40 C39 N3 C36 CONF C44 C39 N3 C36 CONF C40 C39 N3 C46 CONF C44 C39 N3 C46 CONF C47 C46 N3 C36 CONF C51 C46 N3 C36 CONF C47 C46 N3 C39 CONF C51 C46 N3 C39 CONF C41 C42 O1 C45 CONF C43 C42 O1 C45 CONF C48 C49 O2 C52 CONF C50 C49 O2 C52 CONF C55 C56 N4 C59 CONF C57 C56 N4 C59 CONF C55 C56 N4 C66 CONF C57 C56 N4 C66 CONF C60 C59 N4 C56 CONF C64 C59 N4 C56 CONF C60 C59 N4 C66 CONF C64 C59 N4 C66 CONF C67 C66 N4 C56 CONF C71 C66 N4 C56 CONF C67 C66 N4 C59 CONF C71 C66 N4 C59 CONF C61 C62 O3 C65 CONF C63 C62 O3 C65 CONF C68 C69 O4 C72 CONF C70 C69 O4 C72 BOND $h fmap 2 53 acta OMIT -2 59 OMIT 1 0 0 OMIT 0 2 1 REM Q:/Struc/13S/13srv321/13srv321.hkl WGHT 0.08 0.23 FVAR 0.11259 O1 4 -0.03033 -0.11130 0.49902 11.00000 0.03459 0.03949 0.02396 = -0.00982 0.01161 -0.00604 O2 4 0.35827 -0.20785 0.07533 11.00000 0.03391 0.02050 0.03027 = -0.01082 0.00643 0.00266 O3 4 0.16163 1.17489 -0.09780 11.00000 0.05881 0.02045 0.02535 = -0.00735 -0.00650 0.00088 O4 4 0.53474 0.88835 -0.46243 11.00000 0.03665 0.04688 0.03581 = -0.02431 0.01019 -0.01043 N1 3 -0.55391 0.30041 0.71306 11.00000 0.04431 0.05855 0.02845 = -0.01506 0.00925 -0.00986 N2 3 1.02143 0.67857 -0.67723 11.00000 0.03610 0.04950 0.02449 = -0.01306 0.00480 -0.01025 N3 3 0.22537 0.05310 0.20394 11.00000 0.03624 0.01574 0.02190 = -0.00504 0.01024 -0.00020 N4 3 0.25970 0.87550 -0.18719 11.00000 0.03413 0.01480 0.02430 = 0.00050 0.01001 0.00230 C1 1 0.27763 0.43567 0.01674 11.00000 0.02084 0.01797 0.01717 = -0.00309 0.00159 -0.00042 C2 1 0.21046 0.50531 0.03103 11.00000 0.02162 0.01594 0.01869 = -0.00360 0.00247 -0.00066 C3 1 0.11666 0.48424 0.09675 11.00000 0.02517 0.01473 0.02267 = -0.00539 0.00211 0.00074 C4 1 0.03965 0.46590 0.15285 11.00000 0.02673 0.01800 0.02482 = -0.00665 0.00379 -0.00090 C5 1 -0.04295 0.43934 0.22380 11.00000 0.02602 0.02234 0.02214 = -0.00862 0.00684 -0.00548 C6 1 -0.16214 0.48519 0.22830 11.00000 0.02963 0.02775 0.02432 = -0.01036 0.00294 -0.00126 C7 1 -0.23757 0.46208 0.29807 11.00000 0.02850 0.03657 0.03117 = -0.01767 0.00699 -0.00382 C8 1 -0.19528 0.39316 0.36460 11.00000 0.03141 0.03550 0.02395 = -0.01358 0.00890 -0.01356 C9 1 -0.07875 0.34557 0.35969 11.00000 0.03662 0.03443 0.02223 = -0.00310 0.00402 -0.00738 C10 1 -0.00361 0.36837 0.28995 11.00000 0.02919 0.03087 0.02672 = -0.00556 0.00664 -0.00050 C11 1 -0.27088 0.37301 0.43756 11.00000 0.03740 0.03798 0.02938 = -0.01415 0.00862 -0.01315 C12 1 -0.33289 0.35987 0.49794 11.00000 0.03584 0.03671 0.02863 = -0.01265 0.00747 -0.01058 C13 1 -0.40736 0.34113 0.57064 11.00000 0.03006 0.02677 0.02332 = -0.00905 0.00573 -0.00719 C14 1 -0.53480 0.37628 0.57511 11.00000 0.03519 0.04661 0.02973 = -0.00901 -0.00297 0.00614 C15 1 -0.60212 0.35339 0.64755 11.00000 0.02775 0.05723 0.04510 = -0.02692 0.00609 0.00151 C16 1 -0.43241 0.26781 0.70765 11.00000 0.05325 0.05690 0.02428 = 0.00167 0.00097 0.00583 C17 1 -0.35637 0.28597 0.63932 11.00000 0.03383 0.03759 0.03391 = -0.00518 0.00193 0.00660 C18 1 0.36186 0.45493 -0.05266 11.00000 0.02587 0.01554 0.02064 = -0.00360 0.00000 0.00317 C19 1 0.43601 0.47004 -0.10973 11.00000 0.02772 0.01989 0.02155 = -0.00550 0.00162 0.00249 C20 1 0.52022 0.49839 -0.18005 11.00000 0.02722 0.02520 0.01890 = -0.00596 0.00345 -0.00096 C21 1 0.51378 0.58906 -0.23315 11.00000 0.02976 0.02503 0.02369 = -0.00740 0.00396 0.00069 C22 1 0.59020 0.61749 -0.30306 11.00000 0.03273 0.02631 0.02113 = -0.00322 0.00266 -0.00167 C23 1 0.67354 0.55555 -0.32169 11.00000 0.02971 0.03159 0.02127 = -0.00954 0.00588 -0.00730 C24 1 0.68298 0.46606 -0.26789 11.00000 0.04341 0.03114 0.03235 = -0.00985 0.01640 0.00176 C25 1 0.60781 0.43776 -0.19770 11.00000 0.04321 0.02539 0.02778 = -0.00299 0.01321 0.00380 C26 1 0.74754 0.58352 -0.39579 11.00000 0.03370 0.03023 0.02518 = -0.00930 0.00493 -0.00606 C27 1 0.80746 0.60531 -0.45796 11.00000 0.03334 0.02877 0.02494 = -0.00940 0.00425 -0.00638 C28 1 0.87990 0.63030 -0.53205 11.00000 0.02671 0.03034 0.02024 = -0.00795 0.00204 -0.00490 C29 1 0.92040 0.72065 -0.57477 11.00000 0.04016 0.02894 0.02564 = -0.00874 0.00370 -0.00653 C30 1 0.98968 0.74068 -0.64606 11.00000 0.04372 0.03602 0.02487 = -0.00441 0.00376 -0.01496 C31 1 0.98084 0.59269 -0.63631 11.00000 0.03055 0.04380 0.02893 = -0.01743 0.00147 -0.00125 C32 1 0.91053 0.56521 -0.56478 11.00000 0.03342 0.02689 0.02429 = -0.00763 0.00191 -0.00343 C33 1 0.26206 0.33688 0.06762 11.00000 0.02004 0.01572 0.01835 = -0.00281 0.00403 0.00176 C34 1 0.24589 0.27170 0.03455 11.00000 0.02431 0.01996 0.01919 = -0.00607 0.00256 0.00434 C35 1 0.23043 0.17903 0.07899 11.00000 0.02447 0.01800 0.02327 = -0.00907 0.00280 0.00093 C36 1 0.23432 0.14760 0.15925 11.00000 0.02104 0.01611 0.02257 = -0.00475 0.00552 0.00075 C37 1 0.25150 0.21208 0.19314 11.00000 0.02946 0.02052 0.01657 = -0.00443 0.00162 0.00147 C38 1 0.26399 0.30487 0.14833 11.00000 0.02594 0.01728 0.02045 = -0.00659 0.00158 0.00117 C39 1 0.15954 0.01724 0.27956 11.00000 0.02649 0.01772 0.01973 = -0.00531 0.00415 -0.00303 C40 1 0.03908 0.05159 0.29801 11.00000 0.02901 0.02191 0.02438 = -0.00660 -0.00041 0.00474 C41 1 -0.02688 0.01102 0.37101 11.00000 0.02348 0.02918 0.02951 = -0.01453 0.00370 0.00251 C42 1 0.02680 -0.06521 0.42578 11.00000 0.02797 0.02562 0.01987 = -0.00927 0.00452 -0.00757 C43 1 0.14770 -0.09985 0.40781 11.00000 0.02657 0.02164 0.02274 = -0.00359 -0.00049 -0.00063 C44 1 0.21363 -0.05875 0.33570 11.00000 0.02069 0.02079 0.02594 = -0.00702 0.00365 -0.00048 C45 1 -0.16729 -0.09183 0.51354 11.00000 0.03516 0.05295 0.03696 = -0.02291 0.01473 -0.01051 C46 1 0.26128 -0.01153 0.16864 11.00000 0.02818 0.01522 0.01906 = -0.00352 0.00360 0.00290 C47 1 0.39067 -0.01282 0.13740 11.00000 0.02429 0.01935 0.02245 = -0.00456 0.00277 -0.00311 C48 1 0.42697 -0.07603 0.10398 11.00000 0.02092 0.02215 0.02139 = -0.00353 0.00377 0.00251 C49 1 0.33236 -0.13987 0.10362 11.00000 0.02840 0.01492 0.01799 = -0.00241 0.00159 0.00492 C50 1 0.20189 -0.13847 0.13436 11.00000 0.02730 0.01950 0.02612 = -0.00609 0.00506 -0.00330 C51 1 0.16612 -0.07433 0.16619 11.00000 0.02367 0.02015 0.02533 = -0.00484 0.00795 0.00020 C52 1 0.49116 -0.21118 0.04372 11.00000 0.03602 0.02858 0.03518 = -0.01348 0.00754 0.00467 C53 1 0.22459 0.60359 -0.02179 11.00000 0.02487 0.01512 0.01794 = -0.00440 0.00388 -0.00062 C54 1 0.11238 0.65896 -0.03921 11.00000 0.02210 0.02113 0.02615 = -0.00345 0.00641 0.00041 C55 1 0.12265 0.74861 -0.09299 11.00000 0.02377 0.02116 0.03084 = -0.00155 0.00368 0.00539 C56 1 0.24691 0.78463 -0.12901 11.00000 0.02866 0.01476 0.02303 = -0.00202 0.00410 0.00094 C57 1 0.36033 0.73143 -0.10930 11.00000 0.02330 0.01943 0.02591 = -0.00463 0.00592 -0.00233 C58 1 0.34955 0.64196 -0.05628 11.00000 0.02129 0.01976 0.02414 = -0.00545 0.00043 0.00209 C59 1 0.23691 0.95283 -0.16666 11.00000 0.02169 0.01673 0.02513 = -0.00204 0.00052 0.00132 C60 1 0.22022 0.94269 -0.08888 11.00000 0.03182 0.01899 0.02327 = 0.00119 -0.00107 0.00132 C61 1 0.19415 1.01734 -0.06844 11.00000 0.03572 0.02671 0.02072 = -0.00470 -0.00370 0.00032 C62 1 0.18735 1.10527 -0.12451 11.00000 0.03011 0.01997 0.02667 = -0.00748 -0.00372 -0.00135 C63 1 0.20675 1.11685 -0.20187 11.00000 0.03068 0.01675 0.02441 = -0.00087 -0.00055 -0.00073 C64 1 0.22858 1.04126 -0.22243 11.00000 0.02854 0.02061 0.02210 = -0.00234 0.00149 0.00018 C65 1 0.14473 1.26452 -0.15428 11.00000 0.04569 0.02192 0.02997 = -0.00766 -0.00310 0.00171 C66 1 0.32776 0.88135 -0.25870 11.00000 0.02551 0.01708 0.02340 = -0.00112 0.00161 0.00308 C67 1 0.43905 0.93889 -0.29213 11.00000 0.02863 0.02733 0.02684 = -0.00944 0.00168 -0.00298 C68 1 0.50470 0.93933 -0.36002 11.00000 0.02769 0.03333 0.02870 = -0.01090 0.00591 -0.00888 C69 1 0.46146 0.88248 -0.39567 11.00000 0.02571 0.02692 0.02619 = -0.00824 0.00131 0.00035 C70 1 0.35242 0.82418 -0.36262 11.00000 0.02702 0.02263 0.03445 = -0.01124 -0.00044 0.00018 C71 1 0.28666 0.82450 -0.29473 11.00000 0.02556 0.01919 0.03492 = -0.00401 0.00383 -0.00229 C72 1 0.49640 0.83059 -0.50055 11.00000 0.03885 0.04920 0.03431 = -0.02244 -0.00172 -0.00300 H6 2 -0.19023 0.53302 0.18192 11.00000 0.03090 H7 2 -0.32176 0.49445 0.29937 11.00000 0.03860 H9 2 -0.04814 0.29696 0.40495 11.00000 0.04132 H10 2 0.07916 0.33813 0.28581 11.00000 0.03950 H14 2 -0.57615 0.41630 0.52611 11.00000 0.05333 H15 2 -0.69064 0.37485 0.65032 11.00000 0.05842 H16 2 -0.39499 0.23058 0.75775 11.00000 0.06739 H17 2 -0.26545 0.26082 0.63960 11.00000 0.05283 H21 2 0.45490 0.63288 -0.22063 11.00000 0.03652 H22 2 0.58079 0.68256 -0.34185 11.00000 0.03770 H24 2 0.74611 0.42049 -0.27952 11.00000 0.04931 H25 2 0.61575 0.37515 -0.16082 11.00000 0.04053 H29 2 0.89410 0.76960 -0.55373 11.00000 0.04310 H30 2 1.01789 0.80648 -0.67855 11.00000 0.04828 H31 2 1.00392 0.54527 -0.66065 11.00000 0.04674 H32 2 0.88428 0.50191 -0.53765 11.00000 0.04085 H34 2 0.24150 0.29241 -0.02168 11.00000 0.03098 H35 2 0.21812 0.13564 0.05634 11.00000 0.02154 H37 2 0.25864 0.19119 0.24827 11.00000 0.02548 H38 2 0.27699 0.34856 0.17274 11.00000 0.03122 H40 2 -0.00003 0.10429 0.25845 11.00000 0.03143 H41 2 -0.10873 0.03696 0.38236 11.00000 0.03402 H43 2 0.18380 -0.15095 0.44633 11.00000 0.04635 H44 2 0.29763 -0.08133 0.32234 11.00000 0.02852 H45a 2 -0.22522 -0.10218 0.47563 11.00000 0.04038 H45b 2 -0.18134 -0.02655 0.51000 11.00000 0.04010 H45c 2 -0.19536 -0.13773 0.56623 11.00000 0.05410 H47 2 0.45479 0.03117 0.13951 11.00000 0.02675 H48 2 0.51862 -0.07666 0.08283 11.00000 0.01851 H50 2 0.13474 -0.18371 0.13217 11.00000 0.03719 H51 2 0.07589 -0.07040 0.18568 11.00000 0.03205 H52a 2 0.55537 -0.22034 0.08300 11.00000 0.02973 H52b 2 0.48935 -0.26465 0.02777 11.00000 0.02747 H52c 2 0.51204 -0.15061 -0.00068 11.00000 0.04415 H54 2 0.02080 0.63463 -0.01438 11.00000 0.03736 H55 2 0.04625 0.78546 -0.10569 11.00000 0.03525 H57 2 0.44788 0.75706 -0.13141 11.00000 0.02398 H58 2 0.42911 0.60664 -0.04197 11.00000 0.02431 H60 2 0.22701 0.88496 -0.04927 11.00000 0.03445 H61 2 0.17892 1.01302 -0.01780 11.00000 0.02562 H63 2 0.20303 1.17526 -0.24142 11.00000 0.03913 H64 2 0.24034 1.05204 -0.27725 11.00000 0.02742 H65a 2 0.07000 1.26407 -0.18822 11.00000 0.03277 H65b 2 0.23174 1.28844 -0.18392 11.00000 0.03957 H65c 2 0.10951 1.30116 -0.12455 11.00000 0.03301 H67 2 0.46880 0.97860 -0.26805 11.00000 0.02709 H68 2 0.58199 0.98029 -0.38424 11.00000 0.03436 H70 2 0.32466 0.78345 -0.38476 11.00000 0.02923 H71 2 0.21469 0.78570 -0.27222 11.00000 0.03911 H72a 2 0.50865 0.76291 -0.46489 11.00000 0.05751 H72b 2 0.40223 0.84321 -0.51634 11.00000 0.04650 H72c 2 0.56220 0.84380 -0.54865 11.00000 0.04585 HKLF 4 END ; #===END data_9_13srv145 _audit_creation_date 2013-04-28 _audit_creation_method ; Olex2 1.2-beta (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H26 Br2 Si2' _chemical_formula_sum 'C24 H26 Br2 Si2' _chemical_formula_weight 530.45 _chemical_melting_point ? 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 7.5780(5) _cell_length_b 9.1129(6) _cell_length_c 9.9879(7) _cell_angle_alpha 114.280(2) _cell_angle_beta 94.306(2) _cell_angle_gamma 95.903(2) _cell_volume 620.13(7) _cell_formula_units_Z 1 _cell_measurement_reflns_used 2325 _cell_measurement_temperature 120 _cell_measurement_theta_max 28.03 _cell_measurement_theta_min 2.25 _exptl_absorpt_coefficient_mu 3.372 _exptl_absorpt_correction_T_max 0.9559 _exptl_absorpt_correction_T_min 0.2019 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2006/1 (Bruker,2006) was used for absorption correction. R(int) was 0.0470 before and 0.0250 after correction. The Ratio of minimum to maximum transmission is 0.2112. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'plate' _exptl_crystal_F_000 268 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_special_details ; The data collection nominally covered a full sphere of reciprocal space by a combination of 3 sets of \w scans each set at different \f angles and each scan (7 s exposure) covering -0.300\% degrees in \w. The crystal to detector distance was 4.85 cm. ; _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_unetI/netI 0.0470 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 8019 _diffrn_reflns_theta_full 29.49 _diffrn_reflns_theta_max 29.49 _diffrn_reflns_theta_min 2.26 _diffrn_ambient_temperature 120 _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 5.6 _diffrn_detector_type 'Bruker SMART CCD 6000 area detector' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD 6000 area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_source 'sealed X-ray tube' _diffrn_source_current 10.0 _diffrn_source_power 0.3 _diffrn_source_target Mo _diffrn_source_type 'sealed X-ray tube' _diffrn_source_voltage 30.0 _diffrn_special_details ? _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 2589 _reflns_number_total 3449 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_collection 'SMART v5.625 (Bruker, 2001)' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _refine_diff_density_max 1.160 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.087 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 179 _refine_ls_number_reflns 3449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0363 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.4500P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.0887 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; ; _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 1.29237(4) 0.83854(4) 0.46576(4) 0.03491(11) Uani 1 1 d . . . Si1 Si 0.28932(11) 0.20850(9) -0.03162(8) 0.02622(17) Uani 1 1 d . . . C1 C 0.5386(3) 0.4944(3) 0.4388(3) 0.0209(5) Uani 1 1 d . . . C2 C 0.4506(3) 0.3959(3) 0.2913(3) 0.0217(5) Uani 1 1 d . . . C3 C 0.3885(3) 0.3210(3) 0.1637(3) 0.0237(5) Uani 1 1 d . . . C4 C 0.2404(5) -0.0108(4) -0.0713(4) 0.0364(7) Uani 1 1 d . . . C5 C 0.0795(5) 0.2897(4) -0.0552(4) 0.0422(8) Uani 1 1 d . . . C6 C 0.4496(6) 0.2416(5) -0.1502(4) 0.0504(9) Uani 1 1 d . . . C7 C 0.7193(3) 0.5816(3) 0.4461(3) 0.0205(5) Uani 1 1 d . . . C8 C 0.7728(3) 0.7447(3) 0.5426(3) 0.0224(5) Uani 1 1 d . . . C9 C 0.9421(3) 0.8222(3) 0.5471(3) 0.0230(5) Uani 1 1 d . . . C10 C 1.0582(3) 0.7351(3) 0.4552(3) 0.0233(5) Uani 1 1 d . . . C11 C 1.0076(4) 0.5745(3) 0.3565(3) 0.0248(5) Uani 1 1 d . . . C12 C 0.8383(3) 0.4994(3) 0.3515(3) 0.0232(5) Uani 1 1 d . . . H4A H 0.342(5) -0.052(4) -0.072(4) 0.046(10) Uiso 1 1 d . . . H4B H 0.164(6) -0.065(5) -0.157(5) 0.066(13) Uiso 1 1 d . . . H4C H 0.177(6) -0.024(5) 0.006(5) 0.070(13) Uiso 1 1 d . . . H5A H 0.025(5) 0.233(5) -0.152(5) 0.059(12) Uiso 1 1 d . . . H5B H 0.113(5) 0.394(5) -0.037(4) 0.062(12) Uiso 1 1 d . . . H5C H -0.011(5) 0.282(5) 0.024(4) 0.060(12) Uiso 1 1 d . . . H6A H 0.557(5) 0.214(4) -0.139(4) 0.039(10) Uiso 1 1 d . . . H6B H 0.402(6) 0.185(6) -0.245(6) 0.084(15) Uiso 1 1 d . . . H6C H 0.494(6) 0.365(6) -0.122(5) 0.088(15) Uiso 1 1 d . . . H8 H 0.697(4) 0.801(4) 0.603(3) 0.032(8) Uiso 1 1 d . . . H9 H 0.978(4) 0.937(4) 0.614(3) 0.031(8) Uiso 1 1 d . . . H11 H 1.084(4) 0.516(4) 0.290(4) 0.036(9) Uiso 1 1 d . . . H12 H 0.798(4) 0.389(4) 0.287(3) 0.030(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.02337(14) 0.03373(17) 0.0514(2) 0.02083(14) 0.00924(12) 0.00477(11) Si1 0.0375(4) 0.0224(4) 0.0156(3) 0.0056(3) -0.0002(3) 0.0040(3) C1 0.0215(11) 0.0180(11) 0.0222(12) 0.0076(10) 0.0003(9) 0.0051(9) C2 0.0232(12) 0.0209(12) 0.0219(12) 0.0090(10) 0.0051(10) 0.0053(10) C3 0.0256(12) 0.0236(12) 0.0205(12) 0.0084(10) 0.0033(10) 0.0018(10) C4 0.0389(17) 0.0260(15) 0.0376(18) 0.0087(13) -0.0077(14) 0.0053(13) C5 0.056(2) 0.0320(17) 0.0336(18) 0.0106(14) -0.0113(16) 0.0121(15) C6 0.068(3) 0.053(2) 0.0277(18) 0.0147(17) 0.0168(18) 0.002(2) C7 0.0221(11) 0.0226(12) 0.0181(12) 0.0097(10) 0.0021(9) 0.0040(9) C8 0.0245(12) 0.0222(12) 0.0212(12) 0.0087(10) 0.0051(10) 0.0071(10) C9 0.0252(12) 0.0202(12) 0.0219(12) 0.0079(10) 0.0000(10) 0.0030(10) C10 0.0215(11) 0.0273(13) 0.0249(13) 0.0148(11) 0.0032(10) 0.0028(10) C11 0.0287(13) 0.0283(13) 0.0207(13) 0.0114(11) 0.0083(10) 0.0098(11) C12 0.0263(12) 0.0197(12) 0.0229(13) 0.0076(10) 0.0058(10) 0.0052(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C10 1.896(2) . ? Si1 C3 1.844(3) . ? Si1 C4 1.861(3) . ? Si1 C5 1.860(3) . ? Si1 C6 1.845(4) . ? C1 C1 1.365(5) 2_666 ? C1 C2 1.436(3) . ? C1 C7 1.492(3) . ? C2 C3 1.200(4) . ? C4 H4A 0.89(4) . ? C4 H4B 0.91(4) . ? C4 H4C 0.98(4) . ? C5 H5A 0.93(4) . ? C5 H5B 0.90(4) . ? C5 H5C 1.10(4) . ? C6 H6A 0.89(4) . ? C6 H6B 0.90(5) . ? C6 H6C 1.05(5) . ? C7 C8 1.394(3) . ? C7 C12 1.397(3) . ? C8 C9 1.388(4) . ? C8 H8 0.91(3) . ? C9 C10 1.383(4) . ? C9 H9 0.98(3) . ? C10 C11 1.379(4) . ? C11 C12 1.378(4) . ? C11 H11 0.95(3) . ? C12 H12 0.95(3) . ? 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 C3 Si1 C4 107.99(14) . . ? C3 Si1 C5 107.54(14) . . ? C3 Si1 C6 108.78(17) . . ? C5 Si1 C4 110.65(17) . . ? C6 Si1 C4 111.24(19) . . ? C6 Si1 C5 110.5(2) . . ? C1 C1 C2 122.0(3) 2_666 . ? C1 C1 C7 123.5(3) 2_666 . ? C2 C1 C7 114.5(2) . . ? C3 C2 C1 174.1(3) . . ? C2 C3 Si1 178.8(2) . . ? Si1 C4 H4A 110(2) . . ? Si1 C4 H4B 110(3) . . ? Si1 C4 H4C 110(2) . . ? H4A C4 H4B 113(3) . . ? H4A C4 H4C 108(3) . . ? H4B C4 H4C 106(3) . . ? Si1 C5 H5A 109(2) . . ? Si1 C5 H5B 106(3) . . ? Si1 C5 H5C 111(2) . . ? H5A C5 H5B 110(3) . . ? H5A C5 H5C 111(3) . . ? H5B C5 H5C 110(3) . . ? Si1 C6 H6A 116(2) . . ? Si1 C6 H6B 109(3) . . ? Si1 C6 H6C 114(3) . . ? H6A C6 H6B 108(4) . . ? H6A C6 H6C 96(3) . . ? H6B C6 H6C 114(4) . . ? C8 C7 C1 122.1(2) . . ? C8 C7 C12 118.4(2) . . ? C12 C7 C1 119.5(2) . . ? C7 C8 H8 120(2) . . ? C9 C8 C7 120.7(2) . . ? C9 C8 H8 119(2) . . ? C8 C9 H9 119.9(18) . . ? C10 C9 C8 119.1(2) . . ? C10 C9 H9 120.9(18) . . ? C9 C10 Br1 119.3(2) . . ? C11 C10 Br1 119.27(19) . . ? C11 C10 C9 121.5(2) . . ? C10 C11 H11 122(2) . . ? C12 C11 C10 118.9(2) . . ? C12 C11 H11 119(2) . . ? C7 C12 H12 116.6(18) . . ? C11 C12 C7 121.4(2) . . ? C11 C12 H12 122.0(18) . . ? 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 C2 C1 C7 C8 135.1(2) . . . . ? C2 C1 C7 C12 -43.4(3) . . . . ? _iucr_refine_instructions_details ; TITL CELL 0.71073 7.578 9.1129 9.9879 114.28 94.306 95.903 ZERR 1 0.0005 0.0006 0.0007 0.002 0.002 0.002 LATT 1 SFAC C H Br Si UNIT 24 26 2 2 L.S. 9 PLAN 5 TEMP 120 BOND $h CONF C2 C1 C7 C8 CONF C2 C1 C7 C12 fmap 2 acta OMIT -2 59 REM Q:/Struc/13S/13srv145/sad.hkl WGHT 0.035 0.45 FVAR 0.82737 Br1 3 1.29237 0.83854 0.46576 11.00000 0.02337 0.03373 0.05140 = 0.02083 0.00924 0.00477 Si1 4 0.28932 0.20850 -0.03162 11.00000 0.03754 0.02236 0.01563 = 0.00563 -0.00025 0.00398 C1 1 0.53863 0.49439 0.43883 11.00000 0.02149 0.01803 0.02223 = 0.00756 0.00028 0.00514 C2 1 0.45062 0.39593 0.29130 11.00000 0.02319 0.02095 0.02190 = 0.00898 0.00514 0.00534 C3 1 0.38848 0.32097 0.16372 11.00000 0.02563 0.02361 0.02045 = 0.00840 0.00332 0.00175 C4 1 0.24037 -0.01081 -0.07130 11.00000 0.03891 0.02600 0.03756 = 0.00868 -0.00772 0.00531 C5 1 0.07952 0.28968 -0.05519 11.00000 0.05605 0.03197 0.03363 = 0.01061 -0.01127 0.01215 C6 1 0.44957 0.24160 -0.15023 11.00000 0.06841 0.05301 0.02767 = 0.01472 0.01677 0.00229 C7 1 0.71929 0.58160 0.44612 11.00000 0.02209 0.02257 0.01810 = 0.00971 0.00214 0.00405 C8 1 0.77275 0.74474 0.54256 11.00000 0.02451 0.02216 0.02122 = 0.00867 0.00505 0.00707 C9 1 0.94209 0.82224 0.54712 11.00000 0.02518 0.02024 0.02194 = 0.00787 0.00001 0.00301 C10 1 1.05816 0.73515 0.45520 11.00000 0.02145 0.02727 0.02489 = 0.01477 0.00325 0.00284 C11 1 1.00762 0.57454 0.35645 11.00000 0.02871 0.02826 0.02072 = 0.01135 0.00834 0.00980 C12 1 0.83832 0.49941 0.35155 11.00000 0.02631 0.01969 0.02294 = 0.00763 0.00576 0.00523 H4a 2 0.34211 -0.05214 -0.07201 11.00000 0.04640 H4b 2 0.16433 -0.06490 -0.15693 11.00000 0.06628 H4c 2 0.17702 -0.02354 0.00608 11.00000 0.07024 H5a 2 0.02514 0.23295 -0.15197 11.00000 0.05944 H5b 2 0.11273 0.39398 -0.03701 11.00000 0.06228 H5c 2 -0.01098 0.28164 0.02378 11.00000 0.06007 H6a 2 0.55674 0.21433 -0.13917 11.00000 0.03936 H6b 2 0.40244 0.18514 -0.24544 11.00000 0.08414 H6c 2 0.49448 0.36508 -0.12194 11.00000 0.08810 H8 2 0.69666 0.80148 0.60284 11.00000 0.03243 H9 2 0.97764 0.93719 0.61443 11.00000 0.03091 H11 2 1.08436 0.51621 0.28984 11.00000 0.03598 H12 2 0.79826 0.38880 0.28696 11.00000 0.03044 HKLF 4 END ; #===END data_13srv192 _audit_creation_date 2013-07-11 _audit_creation_method ; Olex2 1.2-beta (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H50 Br2 Si2' _chemical_formula_sum 'C36 H50 Br2 Si2' _chemical_formula_weight 698.76 _chemical_melting_point ? 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 10.5232(5) _cell_length_b 8.0808(4) _cell_length_c 20.8850(11) _cell_angle_alpha 90.00 _cell_angle_beta 102.194(2) _cell_angle_gamma 90.00 _cell_volume 1735.90(15) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7235 _cell_measurement_temperature 120 _cell_measurement_theta_max 32.71 _cell_measurement_theta_min 2.71 _exptl_absorpt_coefficient_mu 2.427 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1256 before and 0.0446 after correction. The Ratio of minimum to maximum transmission is 0.8668. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'prism' _exptl_crystal_F_000 728 _exptl_crystal_size_max 0.235 _exptl_crystal_size_mid 0.157 _exptl_crystal_size_min 0.146 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_unetI/netI 0.0422 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 18956 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 1.98 _diffrn_ambient_temperature 120 _diffrn_detector 'Bruker PHOTON 100 CMOS' _diffrn_detector_area_resol_mean ? _diffrn_detector_type 'CMOS sensor' _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device 'Bruker D8 Venture' _diffrn_measurement_device_type '3-circle diffractometer' _diffrn_measurement_method \w-scan _diffrn_radiation_monochromator 'focusing mirrors' _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'ImuS microsource' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_number_gt 3959 _reflns_number_total 5025 _reflns_threshold_expression >2sigma(I) _computing.bruker_data_scaling 'SADABS V2012/1 (Bruker AXS Inc.)' _computing_cell_refinement 'APEX2 v.2013.4_1 (Bruker, 2013)' _computing_data_collection 'APEX2 v.2013.4_1 (Bruker, 2013)' _computing_data_reduction 'SAINT v8.30C (Bruker, 2013)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.619 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.080 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 281 _refine_ls_number_reflns 5025 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0339 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0300P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0711 _refine_ls_wR_factor_ref 0.0764 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; ; _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.272086(18) -0.71592(2) 0.380443(9) 0.02425(7) Uani 1 1 d . . . Si1 Si 0.75598(4) 0.17205(5) 0.34042(2) 0.01219(10) Uani 1 1 d . . . C1 C 0.51088(16) -0.03834(19) 0.47282(8) 0.0150(3) Uani 1 1 d . . . C2 C 0.59258(16) 0.03305(19) 0.43276(8) 0.0149(3) Uani 1 1 d . . . C3 C 0.65669(16) 0.08692(19) 0.39601(8) 0.0152(3) Uani 1 1 d . . . C4 C 0.45153(17) -0.20129(19) 0.44955(8) 0.0150(3) Uani 1 1 d . . . C5 C 0.53012(17) -0.3301(2) 0.43579(8) 0.0173(3) Uani 1 1 d . . . C6 C 0.47699(18) -0.4834(2) 0.41549(8) 0.0183(3) Uani 1 1 d . . . C7 C 0.34451(17) -0.5059(2) 0.40761(8) 0.0166(3) Uani 1 1 d . . . C8 C 0.26406(17) -0.3794(2) 0.41946(8) 0.0186(3) Uani 1 1 d . . . C9 C 0.31854(17) -0.2272(2) 0.44086(8) 0.0175(3) Uani 1 1 d . . . C10 C 0.89705(17) 0.2854(2) 0.39250(8) 0.0170(3) Uani 1 1 d . . . C11 C 0.9754(2) 0.1756(3) 0.44637(10) 0.0258(4) Uani 1 1 d . . . C12 C 0.8520(2) 0.4429(2) 0.42206(10) 0.0248(4) Uani 1 1 d . . . C13 C 0.65018(16) 0.3202(2) 0.28297(8) 0.0152(3) Uani 1 1 d . . . C14 C 0.7215(2) 0.3934(2) 0.23301(10) 0.0237(4) Uani 1 1 d . . . C15 C 0.5220(2) 0.2433(3) 0.24851(11) 0.0279(4) Uani 1 1 d . . . C16 C 0.81134(17) -0.0051(2) 0.29384(9) 0.0174(3) Uani 1 1 d . . . C17 C 0.8313(2) -0.1683(2) 0.33135(11) 0.0266(4) Uani 1 1 d . . . C18 C 0.9332(2) 0.0383(3) 0.26786(11) 0.0254(4) Uani 1 1 d . . . H5 H 0.6202(19) -0.312(2) 0.4405(9) 0.011(4) Uiso 1 1 d . . . H6 H 0.5273(18) -0.569(2) 0.4084(9) 0.018(5) Uiso 1 1 d . . . H8 H 0.1737(18) -0.398(2) 0.4117(8) 0.015(5) Uiso 1 1 d . . . H9 H 0.2660(18) -0.140(2) 0.4489(8) 0.014(4) Uiso 1 1 d . . . H10 H 0.950(2) 0.317(2) 0.3621(10) 0.023(5) Uiso 1 1 d . . . H11A H 1.043(2) 0.239(3) 0.4713(11) 0.028(6) Uiso 1 1 d . . . H11B H 0.922(2) 0.136(3) 0.4748(10) 0.031(6) Uiso 1 1 d . . . H11C H 1.013(2) 0.078(3) 0.4300(10) 0.031(6) Uiso 1 1 d . . . H12A H 0.798(2) 0.417(3) 0.4513(11) 0.037(6) Uiso 1 1 d . . . H12B H 0.924(2) 0.499(3) 0.4460(11) 0.035(6) Uiso 1 1 d . . . H12C H 0.804(2) 0.520(3) 0.3871(9) 0.026(5) Uiso 1 1 d . . . H13 H 0.6310(17) 0.413(2) 0.3091(8) 0.015(5) Uiso 1 1 d . . . H14A H 0.666(2) 0.475(3) 0.2036(10) 0.031(6) Uiso 1 1 d . . . H14B H 0.803(2) 0.444(2) 0.2524(9) 0.023(5) Uiso 1 1 d . . . H14C H 0.744(2) 0.309(2) 0.2036(10) 0.021(5) Uiso 1 1 d . . . H15A H 0.540(2) 0.151(3) 0.2241(11) 0.038(6) Uiso 1 1 d . . . H15B H 0.470(2) 0.321(3) 0.2173(12) 0.048(7) Uiso 1 1 d . . . H15C H 0.469(3) 0.210(3) 0.2787(14) 0.050(8) Uiso 1 1 d . . . H16 H 0.740(2) -0.024(2) 0.2574(10) 0.026(5) Uiso 1 1 d . . . H17A H 0.899(2) -0.163(3) 0.3681(10) 0.025(5) Uiso 1 1 d . . . H17B H 0.753(2) -0.202(2) 0.3472(11) 0.028(6) Uiso 1 1 d . . . H17C H 0.857(2) -0.257(3) 0.3060(12) 0.037(6) Uiso 1 1 d . . . H18A H 0.955(2) -0.054(3) 0.2398(11) 0.040(6) Uiso 1 1 d . . . H18B H 0.922(2) 0.139(3) 0.2415(10) 0.033(6) Uiso 1 1 d . . . H18C H 1.006(2) 0.050(3) 0.3015(10) 0.029(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.02744(11) 0.01729(9) 0.02825(12) -0.00383(7) 0.00641(8) -0.00606(7) Si1 0.0129(2) 0.0123(2) 0.0126(2) 0.00097(16) 0.00555(17) -0.00036(16) C1 0.0166(8) 0.0141(7) 0.0154(8) 0.0018(6) 0.0059(6) -0.0002(6) C2 0.0176(8) 0.0131(7) 0.0148(8) -0.0012(6) 0.0047(6) 0.0015(6) C3 0.0175(8) 0.0137(8) 0.0150(8) 0.0003(6) 0.0048(6) 0.0008(6) C4 0.0212(8) 0.0148(8) 0.0107(8) 0.0020(6) 0.0070(6) -0.0013(6) C5 0.0178(9) 0.0184(8) 0.0179(9) 0.0015(6) 0.0090(7) -0.0014(7) C6 0.0236(9) 0.0163(8) 0.0174(9) -0.0009(6) 0.0099(7) 0.0031(7) C7 0.0231(9) 0.0142(7) 0.0134(8) -0.0017(6) 0.0059(6) -0.0055(7) C8 0.0172(9) 0.0212(8) 0.0178(9) -0.0005(7) 0.0050(7) -0.0021(7) C9 0.0193(9) 0.0178(8) 0.0165(9) 0.0008(6) 0.0058(7) 0.0030(7) C10 0.0175(8) 0.0187(8) 0.0145(9) 0.0025(6) 0.0029(7) -0.0030(7) C11 0.0219(10) 0.0286(10) 0.0242(11) 0.0047(8) -0.0009(8) -0.0001(8) C12 0.0314(11) 0.0191(9) 0.0216(10) -0.0039(7) 0.0004(8) -0.0032(8) C13 0.0164(8) 0.0160(8) 0.0140(8) 0.0009(6) 0.0053(6) 0.0014(6) C14 0.0260(10) 0.0253(10) 0.0219(10) 0.0095(8) 0.0096(8) 0.0042(8) C15 0.0193(10) 0.0317(11) 0.0298(11) 0.0048(9) -0.0011(8) -0.0015(8) C16 0.0172(8) 0.0163(8) 0.0206(9) -0.0014(6) 0.0083(7) 0.0000(7) C17 0.0287(11) 0.0166(8) 0.0369(12) 0.0003(8) 0.0122(9) 0.0041(8) C18 0.0223(10) 0.0253(10) 0.0337(12) -0.0027(8) 0.0176(9) 0.0014(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C7 1.8974(16) . ? Si1 C3 1.8508(17) . ? Si1 C10 1.8824(18) . ? Si1 C13 1.8838(17) . ? Si1 C16 1.8904(17) . ? C1 C1 1.355(3) 3_656 ? C1 C2 1.441(2) . ? C1 C4 1.494(2) . ? C2 C3 1.205(2) . ? C4 C5 1.397(2) . ? C4 C9 1.389(2) . ? C5 C6 1.388(2) . ? C5 H5 0.944(19) . ? C6 C7 1.381(2) . ? C6 H6 0.900(19) . ? C7 C8 1.383(2) . ? C8 C9 1.390(2) . ? C8 H8 0.942(18) . ? C9 H9 0.931(19) . ? C10 C11 1.530(3) . ? C10 C12 1.533(2) . ? C10 H10 0.96(2) . ? C11 H11A 0.94(2) . ? C11 H11B 0.95(2) . ? C11 H11C 0.98(2) . ? C12 H12A 0.94(2) . ? C12 H12B 0.94(2) . ? C12 H12C 1.01(2) . ? C13 C14 1.527(2) . ? C13 C15 1.521(3) . ? C13 H13 0.971(18) . ? C14 H14A 1.00(2) . ? C14 H14B 0.96(2) . ? C14 H14C 0.98(2) . ? C15 H15A 0.95(2) . ? C15 H15B 0.99(3) . ? C15 H15C 0.96(3) . ? C16 C17 1.526(3) . ? C16 C18 1.535(2) . ? C16 H16 0.96(2) . ? C17 H17A 0.93(2) . ? C17 H17B 0.99(2) . ? C17 H17C 0.96(2) . ? C18 H18A 1.00(2) . ? C18 H18B 0.97(2) . ? C18 H18C 0.93(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Si1 C10 107.41(8) . . ? C3 Si1 C13 107.44(7) . . ? C3 Si1 C16 108.52(7) . . ? C10 Si1 C13 110.28(8) . . ? C10 Si1 C16 112.00(8) . . ? C13 Si1 C16 111.00(8) . . ? C1 C1 C2 122.06(19) 3_656 . ? C1 C1 C4 122.87(18) 3_656 . ? C2 C1 C4 115.07(14) . . ? C3 C2 C1 175.87(17) . . ? C2 C3 Si1 179.18(15) . . ? C5 C4 C1 119.93(15) . . ? C9 C4 C1 121.06(15) . . ? C9 C4 C5 119.01(15) . . ? C4 C5 H5 119.1(11) . . ? C6 C5 C4 120.67(16) . . ? C6 C5 H5 120.2(11) . . ? C5 C6 H6 121.4(12) . . ? C7 C6 C5 119.05(16) . . ? C7 C6 H6 119.6(12) . . ? C6 C7 Br1 119.03(13) . . ? C6 C7 C8 121.46(16) . . ? C8 C7 Br1 119.51(13) . . ? C7 C8 C9 119.03(16) . . ? C7 C8 H8 118.8(11) . . ? C9 C8 H8 122.1(11) . . ? C4 C9 C8 120.75(16) . . ? C4 C9 H9 118.9(11) . . ? C8 C9 H9 120.3(11) . . ? Si1 C10 H10 103.9(12) . . ? C11 C10 Si1 112.30(13) . . ? C11 C10 C12 110.47(15) . . ? C11 C10 H10 110.0(12) . . ? C12 C10 Si1 111.33(13) . . ? C12 C10 H10 108.6(11) . . ? C10 C11 H11A 108.5(13) . . ? C10 C11 H11B 110.7(13) . . ? C10 C11 H11C 114.0(12) . . ? H11A C11 H11B 108.3(18) . . ? H11A C11 H11C 108.6(18) . . ? H11B C11 H11C 106.4(17) . . ? C10 C12 H12A 110.8(13) . . ? C10 C12 H12B 109.5(13) . . ? C10 C12 H12C 111.9(11) . . ? H12A C12 H12B 107.4(18) . . ? H12A C12 H12C 108.8(17) . . ? H12B C12 H12C 108.3(18) . . ? Si1 C13 H13 107.1(10) . . ? C14 C13 Si1 111.83(12) . . ? C14 C13 H13 106.1(10) . . ? C15 C13 Si1 112.79(12) . . ? C15 C13 C14 110.46(16) . . ? C15 C13 H13 108.2(10) . . ? C13 C14 H14A 111.7(12) . . ? C13 C14 H14B 113.7(12) . . ? C13 C14 H14C 112.3(11) . . ? H14A C14 H14B 109.4(16) . . ? H14A C14 H14C 105.2(16) . . ? H14B C14 H14C 103.9(16) . . ? C13 C15 H15A 108.7(14) . . ? C13 C15 H15B 111.4(15) . . ? C13 C15 H15C 112.4(16) . . ? H15A C15 H15B 107(2) . . ? H15A C15 H15C 110.1(19) . . ? H15B C15 H15C 107(2) . . ? Si1 C16 H16 104.8(12) . . ? C17 C16 Si1 114.47(13) . . ? C17 C16 C18 110.13(15) . . ? C17 C16 H16 105.7(12) . . ? C18 C16 Si1 112.34(12) . . ? C18 C16 H16 109.0(12) . . ? C16 C17 H17A 112.2(13) . . ? C16 C17 H17B 112.0(12) . . ? C16 C17 H17C 112.6(14) . . ? H17A C17 H17B 106.8(18) . . ? H17A C17 H17C 103.4(19) . . ? H17B C17 H17C 109.3(18) . . ? C16 C18 H18A 110.2(13) . . ? C16 C18 H18B 112.4(12) . . ? C16 C18 H18C 111.9(13) . . ? H18A C18 H18B 107.6(17) . . ? H18A C18 H18C 105.5(18) . . ? H18B C18 H18C 108.9(18) . . ? _iucr_refine_instructions_details ; TITL 13srv192 in P21/c #14 CELL 0.71073 10.5232 8.0808 20.885 90 102.194 90 ZERR 2 0.0005 0.0004 0.0011 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Si Br UNIT 72 100 4 4 L.S. 9 PLAN 5 TEMP -153.15 REM reset to P21/c #14 BOND $h fmap 2 acta OMIT -2 60 OMIT 0 0 2 REM Q:/Struc/13S/13srv192/13srv192.hkl WGHT 0.04 0.03 FVAR 0.15455 Br1 4 0.27209 -0.71592 0.38044 11.00000 0.02744 0.01729 0.02825 = -0.00383 0.00641 -0.00606 Si1 3 0.75598 0.17205 0.34042 11.00000 0.01289 0.01231 0.01264 = 0.00097 0.00555 -0.00036 C1 1 0.51088 -0.03834 0.47282 11.00000 0.01661 0.01410 0.01544 = 0.00181 0.00586 -0.00019 C2 1 0.59258 0.03305 0.43276 11.00000 0.01755 0.01307 0.01476 = -0.00120 0.00467 0.00147 C3 1 0.65669 0.08692 0.39601 11.00000 0.01745 0.01367 0.01496 = 0.00026 0.00477 0.00081 C4 1 0.45154 -0.20129 0.44955 11.00000 0.02120 0.01477 0.01068 = 0.00197 0.00702 -0.00126 C5 1 0.53012 -0.33011 0.43579 11.00000 0.01783 0.01840 0.01793 = 0.00153 0.00903 -0.00141 C6 1 0.47700 -0.48337 0.41549 11.00000 0.02364 0.01625 0.01740 = -0.00087 0.00985 0.00308 C7 1 0.34451 -0.50591 0.40761 11.00000 0.02305 0.01422 0.01343 = -0.00168 0.00592 -0.00554 C8 1 0.26406 -0.37936 0.41946 11.00000 0.01724 0.02124 0.01776 = -0.00055 0.00500 -0.00214 C9 1 0.31854 -0.22720 0.44086 11.00000 0.01926 0.01781 0.01648 = 0.00080 0.00581 0.00302 C10 1 0.89705 0.28539 0.39250 11.00000 0.01750 0.01875 0.01450 = 0.00248 0.00294 -0.00300 C11 1 0.97541 0.17559 0.44638 11.00000 0.02190 0.02857 0.02423 = 0.00466 -0.00091 -0.00014 C12 1 0.85204 0.44294 0.42206 11.00000 0.03138 0.01910 0.02161 = -0.00390 0.00040 -0.00324 C13 1 0.65018 0.32022 0.28297 11.00000 0.01635 0.01599 0.01405 = 0.00094 0.00531 0.00143 C14 1 0.72147 0.39343 0.23301 11.00000 0.02601 0.02532 0.02185 = 0.00950 0.00956 0.00424 C15 1 0.52196 0.24329 0.24851 11.00000 0.01930 0.03166 0.02982 = 0.00475 -0.00110 -0.00154 C16 1 0.81134 -0.00507 0.29384 11.00000 0.01718 0.01631 0.02064 = -0.00136 0.00827 0.00002 C17 1 0.83133 -0.16825 0.33135 11.00000 0.02865 0.01664 0.03685 = 0.00030 0.01218 0.00412 C18 1 0.93319 0.03833 0.26786 11.00000 0.02228 0.02528 0.03368 = -0.00275 0.01763 0.00143 H5 2 0.62017 -0.31177 0.44046 11.00000 0.01123 H6 2 0.52728 -0.56858 0.40836 11.00000 0.01808 H8 2 0.17374 -0.39835 0.41166 11.00000 0.01480 H9 2 0.26597 -0.14030 0.44894 11.00000 0.01424 H10 2 0.94960 0.31661 0.36210 11.00000 0.02273 H11A 2 1.04337 0.23924 0.47133 11.00000 0.02776 H11B 2 0.92209 0.13645 0.47478 11.00000 0.03102 H11C 2 1.01287 0.07768 0.43005 11.00000 0.03060 H12A 2 0.79754 0.41682 0.45126 11.00000 0.03732 H12B 2 0.92443 0.49923 0.44603 11.00000 0.03518 H12C 2 0.80365 0.52038 0.38707 11.00000 0.02563 H13 2 0.63104 0.41253 0.30915 11.00000 0.01508 H14A 2 0.66629 0.47509 0.20361 11.00000 0.03104 H14B 2 0.80346 0.44367 0.25240 11.00000 0.02347 H14C 2 0.74425 0.30904 0.20362 11.00000 0.02112 H15A 2 0.53988 0.15073 0.22412 11.00000 0.03775 H15B 2 0.46985 0.32148 0.21728 11.00000 0.04808 H15C 2 0.46908 0.21035 0.27872 11.00000 0.04966 H16 2 0.74029 -0.02389 0.25742 11.00000 0.02573 H17A 2 0.89944 -0.16254 0.36812 11.00000 0.02543 H17B 2 0.75278 -0.20204 0.34718 11.00000 0.02825 H17C 2 0.85716 -0.25702 0.30597 11.00000 0.03671 H18A 2 0.95459 -0.05360 0.23978 11.00000 0.03956 H18B 2 0.92219 0.13889 0.24154 11.00000 0.03253 H18C 2 1.00599 0.04997 0.30150 11.00000 0.02865 HKLF 4 END ; #===END