data_sarpong25 _audit_creation_method SHELXL-97 _chemical_name_systematic ; sarpong25 ; _chemical_name_common TL5-mullet _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H19 Br O5' _chemical_formula_weight 407.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8721(11) _cell_length_b 13.2210(12) _cell_length_c 13.4918(12) _cell_angle_alpha 118.274(2) _cell_angle_beta 101.488(2) _cell_angle_gamma 102.795(2) _cell_volume 1700.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9846 _cell_measurement_theta_min 3.98 _cell_measurement_theta_max 67.90 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 3.537 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7651 _exptl_absorpt_correction_T_max 0.8715 _exptl_absorpt_process_details SADABS _diffrn_refln_scan_width 1.0 _diffrn_refln_scan_rate 5 _space_group.centring_type primitive _space_group.IT_number 2 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'microfocus rotating anode' _diffrn_radiation_monochromator 'HELIOS multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 33120 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0136 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 68.24 _reflns_number_total 6052 _reflns_number_gt 5973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-2008' _computing_structure_refinement 'SHELXL-97' _computing_molecular_graphics 'ORTEP-32' _computing_publication_material 'WinGX' _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. ; _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^)+(0.0439P)^2^+2.5994P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6052 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.4020(2) 0.2735(2) 0.71013(19) 0.0202(4) Uani 1 1 d . . . H1 H 0.3919 0.3491 0.7708 0.024 Uiso 1 1 calc R . . C2 C 0.5319(2) 0.2693(2) 0.7445(2) 0.0224(5) Uani 1 1 d . . . H2A H 0.5966 0.3375 0.7527 0.027 Uiso 1 1 calc R . . H2B H 0.5544 0.2674 0.8181 0.027 Uiso 1 1 calc R . . C3 C 0.5021(2) 0.1440(2) 0.6292(2) 0.0232(5) Uani 1 1 d . . . H3 H 0.5722 0.1142 0.6220 0.028 Uiso 1 1 calc R . . C4 C 0.4456(2) 0.1622(2) 0.5309(2) 0.0212(5) Uani 1 1 d . . . C5 C 0.3810(2) 0.2559(2) 0.58391(19) 0.0192(4) Uani 1 1 d . . . C6 C 0.2436(2) 0.2108(2) 0.5131(2) 0.0222(5) Uani 1 1 d . . . H6 H 0.2101 0.2751 0.5572 0.027 Uiso 1 1 calc R . . C7 C 0.1692(2) 0.0901(2) 0.4944(2) 0.0269(5) Uani 1 1 d . . . H7A H 0.1969 0.0240 0.4449 0.032 Uiso 1 1 calc R . . H7B H 0.0807 0.0665 0.4512 0.032 Uiso 1 1 calc R . . C8 C 0.1863(2) 0.1043(2) 0.6162(2) 0.0274(5) Uani 1 1 d . . . H8A H 0.1485 0.1626 0.6609 0.033 Uiso 1 1 calc R . . H8B H 0.1429 0.0235 0.6032 0.033 Uiso 1 1 calc R . . C9 C 0.3221(2) 0.1515(2) 0.6912(2) 0.0230(5) Uani 1 1 d . . . H9 H 0.3279 0.1654 0.7719 0.028 Uiso 1 1 calc R . . C10 C 0.3910(2) 0.0629(2) 0.6355(2) 0.0256(5) Uani 1 1 d . . . H10A H 0.4194 0.0332 0.6873 0.031 Uiso 1 1 calc R . . H10B H 0.3369 -0.0091 0.5543 0.031 Uiso 1 1 calc R . . C11 C 0.4474(2) 0.3770(2) 0.59779(19) 0.0207(4) Uani 1 1 d . . . C12 C 0.6412(2) 0.5199(2) 0.6471(2) 0.0290(5) Uani 1 1 d . . . H12A H 0.6099 0.5283 0.5796 0.044 Uiso 1 1 calc R . . H12B H 0.7277 0.5275 0.6606 0.044 Uiso 1 1 calc R . . H12C H 0.6352 0.5848 0.7198 0.044 Uiso 1 1 calc R . . C13 C 0.1373(2) 0.2155(2) 0.3476(2) 0.0222(5) Uani 1 1 d . . . C14 C 0.1305(2) 0.1886(2) 0.2257(2) 0.0205(4) Uani 1 1 d . . . C15 C 0.0372(2) 0.2070(2) 0.1633(2) 0.0294(5) Uani 1 1 d . . . H15 H -0.0184 0.2376 0.2000 0.035 Uiso 1 1 calc R . . C16 C 0.0242(2) 0.1815(3) 0.0491(2) 0.0308(5) Uani 1 1 d . . . H16 H -0.0394 0.1947 0.0072 0.037 Uiso 1 1 calc R . . C17 C 0.1053(2) 0.1364(2) -0.0031(2) 0.0227(5) Uani 1 1 d . . . C18 C 0.1980(2) 0.1155(2) 0.0562(2) 0.0286(5) Uani 1 1 d . . . H18 H 0.2523 0.0832 0.0184 0.034 Uiso 1 1 calc R . . C19 C 0.2105(2) 0.1422(2) 0.1711(2) 0.0259(5) Uani 1 1 d . . . H19 H 0.2740 0.1287 0.2128 0.031 Uiso 1 1 calc R . . C20 C 0.4059(2) 0.7237(2) 0.7308(2) 0.0211(5) Uani 1 1 d . . . H20 H 0.4600 0.6758 0.7041 0.025 Uiso 1 1 calc R . . C21 C 0.4708(2) 0.8644(2) 0.7985(2) 0.0233(5) Uani 1 1 d . . . H21A H 0.5015 0.8908 0.7483 0.028 Uiso 1 1 calc R . . H21B H 0.5384 0.8987 0.8749 0.028 Uiso 1 1 calc R . . C22 C 0.3559(2) 0.8940(2) 0.8182(2) 0.0235(5) Uani 1 1 d . . . H22 H 0.3682 0.9836 0.8630 0.028 Uiso 1 1 calc R . . C23 C 0.3182(2) 0.8266(2) 0.8776(2) 0.0220(5) Uani 1 1 d . . . C24 C 0.3547(2) 0.7103(2) 0.8233(2) 0.0201(4) Uani 1 1 d . . . C25 C 0.2459(2) 0.5878(2) 0.7662(2) 0.0216(5) Uani 1 1 d . . . H25 H 0.2760 0.5176 0.7376 0.026 Uiso 1 1 calc R . . C26 C 0.1421(2) 0.5649(2) 0.6630(2) 0.0240(5) Uani 1 1 d . . . H26A H 0.1023 0.6260 0.6946 0.029 Uiso 1 1 calc R . . H26B H 0.0790 0.4816 0.6238 0.029 Uiso 1 1 calc R . . C27 C 0.1910(2) 0.5752(2) 0.5707(2) 0.0243(5) Uani 1 1 d . . . H27A H 0.1228 0.5664 0.5078 0.029 Uiso 1 1 calc R . . H27B H 0.2205 0.5069 0.5315 0.029 Uiso 1 1 calc R . . C28 C 0.2962(2) 0.6978(2) 0.6271(2) 0.0221(5) Uani 1 1 d . . . H28 H 0.3271 0.6971 0.5631 0.027 Uiso 1 1 calc R . . C29 C 0.2611(2) 0.8144(2) 0.6875(2) 0.0241(5) Uani 1 1 d . . . H29A H 0.2690 0.8590 0.6460 0.029 Uiso 1 1 calc R . . H29B H 0.1756 0.7915 0.6867 0.029 Uiso 1 1 calc R . . C30 C 0.4560(2) 0.7211(2) 0.9215(2) 0.0212(5) Uani 1 1 d . . . C31 C 0.5870(2) 0.6229(2) 0.9600(2) 0.0278(5) Uani 1 1 d . . . H31A H 0.6588 0.7004 1.0080 0.042 Uiso 1 1 calc R . . H31B H 0.6134 0.5543 0.9165 0.042 Uiso 1 1 calc R . . H31C H 0.5493 0.6098 1.0134 0.042 Uiso 1 1 calc R . . C32 C 0.2118(2) 0.5289(2) 0.9064(2) 0.0248(5) Uani 1 1 d . . . C33 C 0.1797(2) 0.5747(2) 1.0177(2) 0.0240(5) Uani 1 1 d . . . C34 C 0.1459(2) 0.4959(2) 1.0566(2) 0.0258(5) Uani 1 1 d . . . H34 H 0.1414 0.4131 1.0115 0.031 Uiso 1 1 calc R . . C35 C 0.1188(2) 0.5387(2) 1.1617(2) 0.0269(5) Uani 1 1 d . . . H35 H 0.0943 0.4852 1.1883 0.032 Uiso 1 1 calc R . . C36 C 0.1280(2) 0.6603(2) 1.2267(2) 0.0274(5) Uani 1 1 d . . . C37 C 0.1625(2) 0.7404(2) 1.1898(2) 0.0271(5) Uani 1 1 d . . . H37 H 0.1686 0.8237 1.2360 0.033 Uiso 1 1 calc R . . C38 C 0.1880(2) 0.6966(2) 1.0844(2) 0.0250(5) Uani 1 1 d . . . H38 H 0.2112 0.7500 1.0575 0.030 Uiso 1 1 calc R . . O1 O 0.44469(17) 0.11259(16) 0.42914(15) 0.0284(4) Uani 1 1 d . . . O2 O 0.39821(15) 0.44511(15) 0.59231(15) 0.0265(4) Uani 1 1 d . . . O3 O 0.56832(15) 0.39992(15) 0.61940(16) 0.0257(3) Uani 1 1 d . . . O4 O 0.23229(14) 0.19441(15) 0.39684(14) 0.0220(3) Uani 1 1 d . . . O5 O 0.06614(15) 0.25106(17) 0.39573(15) 0.0293(4) Uani 1 1 d . . . O6 O 0.26775(16) 0.85501(15) 0.95068(15) 0.0269(4) Uani 1 1 d . . . O7 O 0.49299(18) 0.79857(17) 1.02682(16) 0.0367(4) Uani 1 1 d . . . O8 O 0.49773(15) 0.62909(16) 0.87468(15) 0.0274(4) Uani 1 1 d . . . O9 O 0.19751(14) 0.59744(15) 0.86025(15) 0.0234(3) Uani 1 1 d . . . O10 O 0.2468(2) 0.44408(19) 0.86520(19) 0.0399(5) Uani 1 1 d . . . Br1 Br 0.08745(2) 0.09971(2) -0.16048(2) 0.03102(9) Uani 1 1 d . . . Br2 Br 0.09308(3) 0.72123(3) 1.37183(2) 0.03723(10) 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 0.0196(11) 0.0237(11) 0.0158(10) 0.0105(9) 0.0055(8) 0.0063(9) C2 0.0201(11) 0.0245(11) 0.0229(11) 0.0150(10) 0.0049(9) 0.0058(9) C3 0.0226(11) 0.0240(11) 0.0263(12) 0.0158(10) 0.0091(9) 0.0085(9) C4 0.0192(10) 0.0190(10) 0.0249(12) 0.0123(9) 0.0086(9) 0.0042(8) C5 0.0187(10) 0.0222(11) 0.0169(10) 0.0109(9) 0.0065(9) 0.0068(9) C6 0.0194(11) 0.0302(12) 0.0166(10) 0.0132(10) 0.0062(9) 0.0075(9) C7 0.0196(11) 0.0331(13) 0.0221(12) 0.0152(10) 0.0039(9) 0.0021(10) C8 0.0209(12) 0.0355(13) 0.0257(12) 0.0192(11) 0.0081(10) 0.0040(10) C9 0.0214(11) 0.0279(12) 0.0206(11) 0.0153(10) 0.0074(9) 0.0051(9) C10 0.0259(12) 0.0249(11) 0.0279(12) 0.0171(10) 0.0088(10) 0.0068(10) C11 0.0223(11) 0.0235(11) 0.0159(10) 0.0110(9) 0.0065(9) 0.0072(9) C12 0.0271(12) 0.0274(12) 0.0329(13) 0.0201(11) 0.0092(10) 0.0028(10) C13 0.0196(11) 0.0224(11) 0.0201(11) 0.0105(9) 0.0050(9) 0.0042(9) C14 0.0185(10) 0.0197(10) 0.0199(11) 0.0110(9) 0.0042(9) 0.0034(8) C15 0.0270(12) 0.0416(14) 0.0269(12) 0.0198(12) 0.0122(10) 0.0192(11) C16 0.0263(12) 0.0449(15) 0.0299(13) 0.0255(12) 0.0080(10) 0.0169(11) C17 0.0232(11) 0.0242(11) 0.0183(11) 0.0137(9) 0.0049(9) 0.0020(9) C18 0.0293(12) 0.0392(14) 0.0256(12) 0.0199(11) 0.0136(10) 0.0176(11) C19 0.0249(12) 0.0344(13) 0.0245(12) 0.0189(11) 0.0087(10) 0.0143(10) C20 0.0194(10) 0.0237(11) 0.0212(11) 0.0134(10) 0.0068(9) 0.0071(9) C21 0.0221(11) 0.0240(11) 0.0236(11) 0.0142(10) 0.0078(9) 0.0053(9) C22 0.0243(11) 0.0212(11) 0.0264(12) 0.0139(10) 0.0094(10) 0.0081(9) C23 0.0192(10) 0.0209(11) 0.0222(11) 0.0107(9) 0.0042(9) 0.0063(9) C24 0.0194(10) 0.0218(11) 0.0199(11) 0.0122(9) 0.0065(9) 0.0075(9) C25 0.0203(11) 0.0238(11) 0.0223(11) 0.0142(10) 0.0077(9) 0.0068(9) C26 0.0188(11) 0.0249(11) 0.0260(12) 0.0150(10) 0.0042(9) 0.0047(9) C27 0.0233(11) 0.0254(11) 0.0211(11) 0.0133(10) 0.0032(9) 0.0060(9) C28 0.0222(11) 0.0256(11) 0.0208(11) 0.0143(10) 0.0070(9) 0.0090(9) C29 0.0235(11) 0.0263(12) 0.0265(12) 0.0180(10) 0.0075(10) 0.0086(9) C30 0.0205(11) 0.0215(11) 0.0226(12) 0.0142(10) 0.0068(9) 0.0048(9) C31 0.0250(12) 0.0292(12) 0.0261(12) 0.0150(10) 0.0026(10) 0.0103(10) C32 0.0181(11) 0.0290(12) 0.0308(12) 0.0202(11) 0.0067(9) 0.0066(9) C33 0.0137(10) 0.0317(12) 0.0272(12) 0.0192(11) 0.0026(9) 0.0061(9) C34 0.0176(10) 0.0292(12) 0.0307(13) 0.0192(11) 0.0034(9) 0.0059(9) C35 0.0189(11) 0.0338(13) 0.0298(12) 0.0229(11) 0.0037(9) 0.0035(9) C36 0.0220(11) 0.0367(13) 0.0202(11) 0.0164(11) 0.0049(9) 0.0053(10) C37 0.0245(12) 0.0289(12) 0.0259(12) 0.0168(11) 0.0044(10) 0.0058(10) C38 0.0195(11) 0.0317(12) 0.0275(12) 0.0206(11) 0.0055(9) 0.0074(9) O1 0.0368(9) 0.0296(9) 0.0251(9) 0.0155(7) 0.0164(7) 0.0163(7) O2 0.0288(9) 0.0263(8) 0.0300(9) 0.0179(7) 0.0107(7) 0.0129(7) O3 0.0209(8) 0.0251(8) 0.0357(9) 0.0208(8) 0.0096(7) 0.0061(7) O4 0.0207(8) 0.0293(8) 0.0171(8) 0.0136(7) 0.0057(6) 0.0095(7) O5 0.0245(8) 0.0413(10) 0.0222(8) 0.0155(8) 0.0089(7) 0.0158(8) O6 0.0300(9) 0.0275(8) 0.0285(9) 0.0161(7) 0.0150(7) 0.0129(7) O7 0.0460(11) 0.0314(9) 0.0227(9) 0.0098(8) 0.0009(8) 0.0187(8) O8 0.0254(8) 0.0322(9) 0.0214(8) 0.0123(7) 0.0036(7) 0.0148(7) O9 0.0230(8) 0.0259(8) 0.0270(8) 0.0176(7) 0.0110(7) 0.0092(7) O10 0.0553(12) 0.0466(11) 0.0507(12) 0.0374(10) 0.0336(10) 0.0349(10) Br1 0.02977(15) 0.03973(16) 0.02061(14) 0.01897(12) 0.00653(10) 0.00367(11) Br2 0.04413(17) 0.03620(16) 0.02541(15) 0.01748(12) 0.01170(12) 0.00332(12) _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 C1 C2 1.541(3) . ? C1 C9 1.550(3) . ? C1 C5 1.564(3) . ? C1 H1 1.0000 . ? C2 C3 1.539(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.513(3) . ? C3 C10 1.550(3) . ? C3 H3 1.0000 . ? C4 O1 1.205(3) . ? C4 C5 1.560(3) . ? C5 C11 1.523(3) . ? C5 C6 1.529(3) . ? C6 O4 1.451(3) . ? C6 C7 1.516(3) . ? C6 H6 1.0000 . ? C7 C8 1.527(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.524(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.562(3) . ? C9 H9 1.0000 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O2 1.198(3) . ? C11 O3 1.339(3) . ? C12 O3 1.451(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O5 1.210(3) . ? C13 O4 1.344(3) . ? C13 C14 1.489(3) . ? C14 C19 1.390(3) . ? C14 C15 1.391(3) . ? C15 C16 1.379(4) . ? C15 H15 0.9500 . ? C16 C17 1.380(3) . ? C16 H16 0.9500 . ? C17 C18 1.386(3) . ? C17 Br1 1.895(2) . ? C18 C19 1.385(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.537(3) . ? C20 C28 1.548(3) . ? C20 C24 1.556(3) . ? C20 H20 1.0000 . ? C21 C22 1.539(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.509(3) . ? C22 C29 1.552(3) . ? C22 H22 1.0000 . ? C23 O6 1.207(3) . ? C23 C24 1.564(3) . ? C24 C30 1.527(3) . ? C24 C25 1.543(3) . ? C25 O9 1.458(3) . ? C25 C26 1.518(3) . ? C25 H25 1.0000 . ? C26 C27 1.523(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.524(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.562(3) . ? C28 H28 1.0000 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O7 1.198(3) . ? C30 O8 1.337(3) . ? C31 O8 1.449(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 O10 1.204(3) . ? C32 O9 1.341(3) . ? C32 C33 1.494(3) . ? C33 C38 1.393(4) . ? C33 C34 1.392(4) . ? C34 C35 1.391(4) . ? C34 H34 0.9500 . ? C35 C36 1.384(4) . ? C35 H35 0.9500 . ? C36 C37 1.388(4) . ? C36 Br2 1.905(2) . ? C37 C38 1.385(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? 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 C2 C1 C9 100.59(18) . . ? C2 C1 C5 102.76(17) . . ? C9 C1 C5 108.14(17) . . ? C2 C1 H1 114.6 . . ? C9 C1 H1 114.6 . . ? C5 C1 H1 114.6 . . ? C3 C2 C1 95.30(17) . . ? C3 C2 H2A 112.7 . . ? C1 C2 H2A 112.7 . . ? C3 C2 H2B 112.7 . . ? C1 C2 H2B 112.7 . . ? H2A C2 H2B 110.2 . . ? C4 C3 C2 102.66(18) . . ? C4 C3 C10 104.73(18) . . ? C2 C3 C10 100.05(18) . . ? C4 C3 H3 115.8 . . ? C2 C3 H3 115.8 . . ? C10 C3 H3 115.8 . . ? O1 C4 C3 128.3(2) . . ? O1 C4 C5 124.9(2) . . ? C3 C4 C5 106.69(18) . . ? C11 C5 C6 108.75(18) . . ? C11 C5 C4 110.50(17) . . ? C6 C5 C4 115.41(18) . . ? C11 C5 C1 110.40(17) . . ? C6 C5 C1 111.31(17) . . ? C4 C5 C1 100.25(17) . . ? O4 C6 C7 109.25(18) . . ? O4 C6 C5 107.72(17) . . ? C7 C6 C5 112.76(19) . . ? O4 C6 H6 109.0 . . ? C7 C6 H6 109.0 . . ? C5 C6 H6 109.0 . . ? C6 C7 C8 109.67(19) . . ? C6 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? C6 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C9 C8 C7 111.89(19) . . ? C9 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? C9 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C8 C9 C1 114.12(19) . . ? C8 C9 C10 114.7(2) . . ? C1 C9 C10 102.80(17) . . ? C8 C9 H9 108.3 . . ? C1 C9 H9 108.3 . . ? C10 C9 H9 108.3 . . ? C3 C10 C9 103.87(18) . . ? C3 C10 H10A 111.0 . . ? C9 C10 H10A 111.0 . . ? C3 C10 H10B 111.0 . . ? C9 C10 H10B 111.0 . . ? H10A C10 H10B 109.0 . . ? O2 C11 O3 123.8(2) . . ? O2 C11 C5 124.2(2) . . ? O3 C11 C5 111.92(18) . . ? O3 C12 H12A 109.5 . . ? O3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O5 C13 O4 124.4(2) . . ? O5 C13 C14 124.3(2) . . ? O4 C13 C14 111.33(19) . . ? C19 C14 C15 119.3(2) . . ? C19 C14 C13 122.5(2) . . ? C15 C14 C13 118.1(2) . . ? C16 C15 C14 121.0(2) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 118.8(2) . . ? C15 C16 H16 120.6 . . ? C17 C16 H16 120.6 . . ? C16 C17 C18 121.5(2) . . ? C16 C17 Br1 119.11(18) . . ? C18 C17 Br1 119.33(18) . . ? C19 C18 C17 119.1(2) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C14 120.3(2) . . ? C18 C19 H19 119.9 . . ? C14 C19 H19 119.9 . . ? C21 C20 C28 101.87(18) . . ? C21 C20 C24 101.61(18) . . ? C28 C20 C24 108.21(18) . . ? C21 C20 H20 114.6 . . ? C28 C20 H20 114.6 . . ? C24 C20 H20 114.6 . . ? C20 C21 C22 95.32(17) . . ? C20 C21 H21A 112.7 . . ? C22 C21 H21A 112.7 . . ? C20 C21 H21B 112.7 . . ? C22 C21 H21B 112.7 . . ? H21A C21 H21B 110.2 . . ? C23 C22 C21 101.16(18) . . ? C23 C22 C29 105.32(19) . . ? C21 C22 C29 101.42(18) . . ? C23 C22 H22 115.6 . . ? C21 C22 H22 115.6 . . ? C29 C22 H22 115.6 . . ? O6 C23 C22 127.2(2) . . ? O6 C23 C24 126.5(2) . . ? C22 C23 C24 106.32(18) . . ? C30 C24 C25 108.28(18) . . ? C30 C24 C20 111.02(18) . . ? C25 C24 C20 113.62(18) . . ? C30 C24 C23 109.68(18) . . ? C25 C24 C23 113.61(18) . . ? C20 C24 C23 100.49(18) . . ? O9 C25 C26 107.95(18) . . ? O9 C25 C24 106.71(17) . . ? C26 C25 C24 112.60(19) . . ? O9 C25 H25 109.8 . . ? C26 C25 H25 109.8 . . ? C24 C25 H25 109.8 . . ? C25 C26 C27 110.78(19) . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C26 C27 C28 112.30(19) . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C20 113.50(19) . . ? C27 C28 C29 114.86(19) . . ? C20 C28 C29 102.80(18) . . ? C27 C28 H28 108.5 . . ? C20 C28 H28 108.5 . . ? C29 C28 H28 108.5 . . ? C22 C29 C28 103.74(18) . . ? C22 C29 H29A 111.0 . . ? C28 C29 H29A 111.0 . . ? C22 C29 H29B 111.0 . . ? C28 C29 H29B 111.0 . . ? H29A C29 H29B 109.0 . . ? O7 C30 O8 123.3(2) . . ? O7 C30 C24 126.0(2) . . ? O8 C30 C24 110.65(18) . . ? O8 C31 H31A 109.5 . . ? O8 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O8 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O10 C32 O9 125.0(2) . . ? O10 C32 C33 125.0(2) . . ? O9 C32 C33 110.0(2) . . ? C38 C33 C34 120.2(2) . . ? C38 C33 C32 120.2(2) . . ? C34 C33 C32 119.6(2) . . ? C35 C34 C33 120.0(2) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 118.8(2) . . ? C36 C35 H35 120.6 . . ? C34 C35 H35 120.6 . . ? C35 C36 C37 122.0(2) . . ? C35 C36 Br2 119.54(19) . . ? C37 C36 Br2 118.46(19) . . ? C38 C37 C36 118.7(2) . . ? C38 C37 H37 120.6 . . ? C36 C37 H37 120.6 . . ? C37 C38 C33 120.3(2) . . ? C37 C38 H38 119.8 . . ? C33 C38 H38 119.8 . . ? C11 O3 C12 115.55(18) . . ? C13 O4 C6 116.06(17) . . ? C30 O8 C31 116.06(18) . . ? C32 O9 C25 120.52(18) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.319 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.065 _iucr_refine_instructions_details ; TITL sarpong25_0m in P-1 CELL 1.54178 11.8721 13.2210 13.4918 118.274 101.488 102.795 ZERR 4.00 0.0011 0.0012 0.0012 0.002 0.002 0.002 LATT 1 SFAC C H O BR UNIT 76 76 20 4 MERG 2 FMAP 2 PLAN 25 SIZE 0.04 0.06 0.08 ACTA 134.00 BOND $H LIST 4 WPDB -2 L.S. 8 TEMP -173.00 WGHT 0.043900 2.599400 FVAR 0.19030 C1 1 0.401994 0.273486 0.710134 11.00000 0.01962 0.02367 = 0.01580 0.01051 0.00550 0.00635 AFIX 13 H1 2 0.391885 0.349054 0.770796 11.00000 -1.20000 AFIX 0 C2 1 0.531905 0.269325 0.744520 11.00000 0.02007 0.02448 = 0.02293 0.01503 0.00488 0.00582 AFIX 23 H2A 2 0.596628 0.337499 0.752710 11.00000 -1.20000 H2B 2 0.554406 0.267359 0.818127 11.00000 -1.20000 AFIX 0 C3 1 0.502101 0.144023 0.629210 11.00000 0.02260 0.02404 = 0.02628 0.01579 0.00914 0.00847 AFIX 13 H3 2 0.572225 0.114153 0.621990 11.00000 -1.20000 AFIX 0 C4 1 0.445566 0.162227 0.530858 11.00000 0.01921 0.01897 = 0.02487 0.01233 0.00863 0.00420 C5 1 0.381002 0.255883 0.583907 11.00000 0.01873 0.02218 = 0.01691 0.01094 0.00646 0.00685 C6 1 0.243621 0.210790 0.513066 11.00000 0.01941 0.03024 = 0.01659 0.01323 0.00620 0.00747 AFIX 13 H6 2 0.210132 0.275121 0.557158 11.00000 -1.20000 AFIX 0 C7 1 0.169175 0.090058 0.494421 11.00000 0.01955 0.03306 = 0.02209 0.01523 0.00387 0.00215 AFIX 23 H7A 2 0.196917 0.023974 0.444924 11.00000 -1.20000 H7B 2 0.080670 0.066487 0.451177 11.00000 -1.20000 AFIX 0 C8 1 0.186261 0.104301 0.616170 11.00000 0.02093 0.03553 = 0.02570 0.01921 0.00810 0.00397 AFIX 23 H8A 2 0.148470 0.162616 0.660893 11.00000 -1.20000 H8B 2 0.142927 0.023482 0.603163 11.00000 -1.20000 AFIX 0 C9 1 0.322144 0.151478 0.691188 11.00000 0.02136 0.02786 = 0.02056 0.01527 0.00739 0.00512 AFIX 13 H9 2 0.327906 0.165391 0.771925 11.00000 -1.20000 AFIX 0 C10 1 0.391006 0.062925 0.635533 11.00000 0.02593 0.02487 = 0.02791 0.01705 0.00883 0.00681 AFIX 23 H10A 2 0.419411 0.033243 0.687306 11.00000 -1.20000 H10B 2 0.336872 -0.009083 0.554329 11.00000 -1.20000 AFIX 0 C11 1 0.447435 0.377048 0.597792 11.00000 0.02234 0.02347 = 0.01589 0.01101 0.00648 0.00720 C12 1 0.641165 0.519870 0.647097 11.00000 0.02709 0.02739 = 0.03285 0.02012 0.00918 0.00279 AFIX 137 H12A 2 0.609862 0.528348 0.579596 11.00000 -1.50000 H12B 2 0.727686 0.527529 0.660639 11.00000 -1.50000 H12C 2 0.635152 0.584757 0.719762 11.00000 -1.50000 AFIX 0 C13 1 0.137346 0.215464 0.347563 11.00000 0.01955 0.02241 = 0.02012 0.01046 0.00499 0.00420 C14 1 0.130458 0.188606 0.225697 11.00000 0.01852 0.01974 = 0.01991 0.01096 0.00419 0.00341 C15 1 0.037194 0.207013 0.163348 11.00000 0.02704 0.04155 = 0.02685 0.01981 0.01224 0.01920 AFIX 43 H15 2 -0.018396 0.237621 0.199995 11.00000 -1.20000 AFIX 0 C16 1 0.024220 0.181499 0.049143 11.00000 0.02633 0.04488 = 0.02993 0.02550 0.00801 0.01691 AFIX 43 H16 2 -0.039354 0.194707 0.007182 11.00000 -1.20000 AFIX 0 C17 1 0.105316 0.136418 -0.003058 11.00000 0.02318 0.02424 = 0.01833 0.01371 0.00485 0.00199 C18 1 0.198045 0.115458 0.056169 11.00000 0.02927 0.03916 = 0.02558 0.01989 0.01360 0.01756 AFIX 43 H18 2 0.252296 0.083208 0.018428 11.00000 -1.20000 AFIX 0 C19 1 0.210509 0.142178 0.171103 11.00000 0.02493 0.03443 = 0.02453 0.01887 0.00873 0.01427 AFIX 43 H19 2 0.274046 0.128714 0.212803 11.00000 -1.20000 AFIX 0 C20 1 0.405879 0.723662 0.730812 11.00000 0.01936 0.02367 = 0.02123 0.01340 0.00680 0.00713 AFIX 13 H20 2 0.460003 0.675759 0.704127 11.00000 -1.20000 AFIX 0 C21 1 0.470769 0.864370 0.798477 11.00000 0.02206 0.02401 = 0.02356 0.01417 0.00776 0.00534 AFIX 23 H21A 2 0.501450 0.890846 0.748286 11.00000 -1.20000 H21B 2 0.538433 0.898692 0.874921 11.00000 -1.20000 AFIX 0 C22 1 0.355865 0.894013 0.818189 11.00000 0.02434 0.02120 = 0.02641 0.01388 0.00936 0.00805 AFIX 13 H22 2 0.368189 0.983625 0.863047 11.00000 -1.20000 AFIX 0 C23 1 0.318157 0.826649 0.877560 11.00000 0.01919 0.02088 = 0.02220 0.01067 0.00416 0.00632 C24 1 0.354709 0.710286 0.823325 11.00000 0.01938 0.02183 = 0.01992 0.01217 0.00653 0.00750 C25 1 0.245938 0.587791 0.766236 11.00000 0.02032 0.02378 = 0.02233 0.01416 0.00775 0.00677 AFIX 13 H25 2 0.275975 0.517572 0.737623 11.00000 -1.20000 AFIX 0 C26 1 0.142077 0.564943 0.663022 11.00000 0.01884 0.02487 = 0.02603 0.01502 0.00424 0.00468 AFIX 23 H26A 2 0.102252 0.625993 0.694623 11.00000 -1.20000 H26B 2 0.078985 0.481568 0.623844 11.00000 -1.20000 AFIX 0 C27 1 0.190979 0.575232 0.570696 11.00000 0.02328 0.02535 = 0.02111 0.01326 0.00323 0.00595 AFIX 23 H27A 2 0.122822 0.566448 0.507784 11.00000 -1.20000 H27B 2 0.220499 0.506906 0.531471 11.00000 -1.20000 AFIX 0 C28 1 0.296152 0.697810 0.627086 11.00000 0.02224 0.02560 = 0.02079 0.01433 0.00700 0.00902 AFIX 13 H28 2 0.327091 0.697102 0.563118 11.00000 -1.20000 AFIX 0 C29 1 0.261147 0.814377 0.687544 11.00000 0.02355 0.02632 = 0.02646 0.01799 0.00753 0.00859 AFIX 23 H29A 2 0.269025 0.858965 0.645992 11.00000 -1.20000 H29B 2 0.175575 0.791472 0.686736 11.00000 -1.20000 AFIX 0 C30 1 0.455959 0.721088 0.921512 11.00000 0.02055 0.02146 = 0.02258 0.01419 0.00677 0.00482 C31 1 0.587030 0.622899 0.960037 11.00000 0.02496 0.02919 = 0.02611 0.01501 0.00260 0.01032 AFIX 137 H31A 2 0.658813 0.700406 1.007964 11.00000 -1.50000 H31B 2 0.613406 0.554272 0.916521 11.00000 -1.50000 H31C 2 0.549285 0.609829 1.013371 11.00000 -1.50000 AFIX 0 C32 1 0.211757 0.528923 0.906446 11.00000 0.01814 0.02900 = 0.03075 0.02019 0.00669 0.00662 C33 1 0.179729 0.574676 1.017655 11.00000 0.01372 0.03171 = 0.02721 0.01920 0.00263 0.00607 C34 1 0.145920 0.495944 1.056640 11.00000 0.01758 0.02921 = 0.03067 0.01923 0.00342 0.00594 AFIX 43 H34 2 0.141384 0.413089 1.011520 11.00000 -1.20000 AFIX 0 C35 1 0.118789 0.538653 1.161677 11.00000 0.01888 0.03379 = 0.02978 0.02290 0.00370 0.00352 AFIX 43 H35 2 0.094339 0.485243 1.188277 11.00000 -1.20000 AFIX 0 C36 1 0.128036 0.660304 1.226748 11.00000 0.02197 0.03666 = 0.02023 0.01636 0.00487 0.00525 C37 1 0.162533 0.740425 1.189820 11.00000 0.02448 0.02894 = 0.02586 0.01678 0.00445 0.00581 AFIX 43 H37 2 0.168556 0.823681 1.235966 11.00000 -1.20000 AFIX 0 C38 1 0.187997 0.696642 1.084412 11.00000 0.01949 0.03173 = 0.02751 0.02058 0.00551 0.00742 AFIX 43 H38 2 0.211211 0.750044 1.057514 11.00000 -1.20000 AFIX 0 O1 3 0.444686 0.112590 0.429139 11.00000 0.03679 0.02955 = 0.02506 0.01545 0.01638 0.01632 O2 3 0.398209 0.445114 0.592306 11.00000 0.02884 0.02626 = 0.02998 0.01788 0.01074 0.01294 O3 3 0.568318 0.399917 0.619403 11.00000 0.02089 0.02511 = 0.03568 0.02084 0.00965 0.00611 O4 3 0.232295 0.194408 0.396840 11.00000 0.02074 0.02930 = 0.01707 0.01361 0.00574 0.00955 O5 3 0.066143 0.251063 0.395734 11.00000 0.02455 0.04132 = 0.02221 0.01553 0.00888 0.01577 O6 3 0.267751 0.855011 0.950677 11.00000 0.03005 0.02745 = 0.02848 0.01610 0.01497 0.01290 O7 3 0.492987 0.798571 1.026820 11.00000 0.04596 0.03141 = 0.02266 0.00982 0.00087 0.01873 O8 3 0.497730 0.629094 0.874679 11.00000 0.02544 0.03223 = 0.02144 0.01233 0.00364 0.01481 O9 3 0.197512 0.597443 0.860252 11.00000 0.02302 0.02593 = 0.02703 0.01759 0.01099 0.00920 O10 3 0.246804 0.444076 0.865200 11.00000 0.05533 0.04664 = 0.05067 0.03739 0.03357 0.03490 BR1 4 0.087447 0.099713 -0.160483 11.00000 0.02977 0.03973 = 0.02061 0.01897 0.00653 0.00367 BR2 4 0.093085 0.721230 1.371831 11.00000 0.04413 0.03620 = 0.02541 0.01748 0.01170 0.00332 HKLF 4 REM sarpong25_0m in P-1 REM R1 = 0.0340 for 5973 Fo > 4sig(Fo) and 0.0343 for all 6052 data REM 453 parameters refined using 0 restraints END WGHT 0.0439 2.6152 REM Highest difference peak 1.319, deepest hole -0.952, 1-sigma level 0.065 Q1 1 0.1229 0.6608 1.3496 11.00000 0.05 1.32 Q2 1 0.1167 0.0452 -0.1823 11.00000 0.05 0.95 Q3 1 0.0418 0.7637 1.4275 11.00000 0.05 0.49 Q4 1 0.4144 0.2193 0.5593 11.00000 0.05 0.39 Q5 1 0.3342 0.7624 0.8512 11.00000 0.05 0.38 Q6 1 0.3205 0.2354 0.5547 11.00000 0.05 0.34 Q7 1 0.4016 0.7126 0.8707 11.00000 0.05 0.34 Q8 1 0.3527 0.1062 0.6635 11.00000 0.05 0.33 Q9 1 0.3036 0.6502 0.7993 11.00000 0.05 0.33 Q10 1 0.3883 0.2625 0.6431 11.00000 0.05 0.31 Q11 1 0.3579 0.2176 0.7009 11.00000 0.05 0.31 Q12 1 0.2417 0.6413 0.5986 11.00000 0.05 0.31 Q13 1 0.3796 0.7128 0.7816 11.00000 0.05 0.31 Q14 1 0.4102 0.8820 0.8123 11.00000 0.05 0.31 Q15 1 0.2775 0.7518 0.6609 11.00000 0.05 0.31 Q16 1 0.1036 0.2139 0.2029 11.00000 0.05 0.30 Q17 1 0.0771 0.1864 0.0285 11.00000 0.05 0.30 Q18 1 0.1800 0.5409 0.9571 11.00000 0.05 0.30 Q19 1 0.2021 0.1461 0.4967 11.00000 0.05 0.29 Q20 1 0.5228 0.2064 0.6839 11.00000 0.05 0.29 Q21 1 0.4470 0.1014 0.6301 11.00000 0.05 0.29 Q22 1 0.2971 0.8455 0.7519 11.00000 0.05 0.29 Q23 1 0.3498 0.7040 0.6742 11.00000 0.05 0.28 Q24 1 0.0133 0.0648 -0.1774 11.00000 0.05 0.28 Q25 1 0.1452 0.2193 0.2899 11.00000 0.05 0.28 ;