#------------------------------------------------------------------------------ #$Date: 2020-10-06 12:14:50 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257582 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/04/7240444.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7240444 loop_ _publ_author_name 'Hadian, Mojgan' 'Shaabani, Shabnam' 'Patil, Pravin' 'Shishkina, Svitlana V.' 'B\"oltz, Harry' 'D\"omling, Alexander' _publ_section_title ; Sustainability by design: automated nanoscale 2,3,4-trisubstituted quinazoline diversity ; _journal_issue 8 _journal_name_full 'Green Chemistry' _journal_page_first 2459 _journal_page_last 2467 _journal_paper_doi 10.1039/D0GC00363H _journal_volume 22 _journal_year 2020 _chemical_formula_sum 'C11 H11 N O5' _chemical_formula_weight 237.21 _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2019-11-29 deposited with the CCDC. 2020-02-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 20.486(2) _cell_length_b 3.9298(4) _cell_length_c 13.6374(12) _cell_measurement_reflns_used 1117 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.2390 _cell_measurement_theta_min 4.232 _cell_volume 1097.89(18) _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 16.1827 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_unetI/netI 0.0591 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 10062 _diffrn_reflns_point_group_measured_fraction_full 0.870 _diffrn_reflns_point_group_measured_fraction_max 0.823 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.996 _diffrn_reflns_theta_min 3.589 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.115 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.92966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.435 _exptl_crystal_description parallelepiped _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.214 _refine_diff_density_min -0.163 _refine_diff_density_rms 0.042 _refine_ls_abs_structure_details ; Flack x determined using 442 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.6(10) _refine_ls_extinction_coef 0.033(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 163 _refine_ls_number_reflns 2644 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.003 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0542 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0715P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1367 _refine_ls_wR_factor_ref 0.1603 _reflns_Friedel_coverage 0.586 _reflns_Friedel_fraction_full 0.730 _reflns_Friedel_fraction_max 0.634 _reflns_number_gt 1685 _reflns_number_total 2644 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0gc00363h2.cif _cod_data_source_block add24 _cod_depositor_comments 'Adding full bibliography for 7240443--7240446.cif.' _cod_original_cell_volume 1097.91(19) _cod_database_code 7240444 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.966 _shelx_estimated_absorpt_t_max 0.986 _shelx_res_file ; TITL add24_a.res in Pca2(1) add24.res created by SHELXL-2016/6 at 11:44:16 on 11-Jul-2019 CELL 0.71073 20.4863 3.9298 13.6374 90 90 90 ZERR 4 0.0021 0.0004 0.0012 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,-Y,+Z SYMM 0.5-X,+Y,0.5+Z SFAC C H N O UNIT 44 44 4 20 L.S. 4 0 0 PLAN 20 BOND $H list 4 fmap 2 53 acta OMIT 0 60 conf size 0.3 0.14 0.12 temp 20 htab n1 o1 eqiv $1 1-x,-y,-0.5+z htab o5 o2_$1 WGHT 0.071500 EXTI 0.032774 FVAR 0.80160 O1 4 0.719447 0.606402 0.415860 11.00000 0.07664 0.09990 = 0.06057 0.02988 -0.00450 -0.01240 O2 4 0.612523 0.083234 0.703502 11.00000 0.05093 0.09955 = 0.05674 0.01887 0.00622 -0.00556 O3 4 0.563345 0.546221 0.490046 11.00000 0.06067 0.04966 = 0.05746 0.00241 -0.01159 -0.00228 O4 4 0.446634 0.305257 0.415559 11.00000 0.04498 0.10981 = 0.08057 -0.02705 0.00739 0.00509 O5 4 0.498525 0.059129 0.291095 11.00000 0.04431 0.09602 = 0.05581 -0.01787 0.00010 -0.00480 H5O 2 0.457644 0.016688 0.263710 11.00000 0.07542 N1 3 0.670892 0.327002 0.579814 11.00000 0.04588 0.06090 = 0.04373 0.00889 0.00010 -0.00703 H1N 2 0.664644 0.431052 0.522143 11.00000 0.07479 C1 1 0.735810 0.239306 0.604674 11.00000 0.04773 0.05219 = 0.04540 0.00161 -0.00133 -0.00782 C2 1 0.752731 0.077307 0.690535 11.00000 0.05185 0.06836 = 0.04780 0.00934 0.00108 -0.00516 AFIX 43 H2 2 0.721040 0.020945 0.736582 11.00000 -1.20000 AFIX 0 C3 1 0.817690 -0.000186 0.707132 11.00000 0.05982 0.07438 = 0.05696 0.01161 -0.00765 0.00013 AFIX 43 H3 2 0.829091 -0.109191 0.765189 11.00000 -1.20000 AFIX 0 C4 1 0.865437 0.077338 0.641600 11.00000 0.04914 0.08034 = 0.07129 0.00835 -0.00664 0.00017 AFIX 43 H4 2 0.908676 0.021475 0.654726 11.00000 -1.20000 AFIX 0 C5 1 0.849205 0.237746 0.556518 11.00000 0.04723 0.07448 = 0.06765 0.00272 0.00831 -0.00948 AFIX 43 H5 2 0.881727 0.293212 0.511705 11.00000 -1.20000 AFIX 0 C6 1 0.784842 0.319434 0.535831 11.00000 0.05391 0.05786 = 0.04551 0.00145 0.00104 -0.01265 C7 1 0.772149 0.497073 0.444057 11.00000 0.06325 0.08750 = 0.05481 0.01857 0.00043 -0.01823 AFIX 43 H7 2 0.807667 0.530831 0.402716 11.00000 -1.20000 AFIX 0 C8 1 0.615453 0.246119 0.626506 11.00000 0.05283 0.05456 = 0.04855 0.00038 0.00207 -0.00535 C9 1 0.553628 0.365420 0.577976 11.00000 0.04976 0.06032 = 0.05634 -0.00065 0.00070 0.00033 AFIX 23 H9A 2 0.526422 0.168995 0.564375 11.00000 -1.20000 H9B 2 0.530066 0.509933 0.623496 11.00000 -1.20000 AFIX 0 C10 1 0.563569 0.341372 0.404946 11.00000 0.04127 0.05855 = 0.05562 -0.00277 0.00148 -0.00185 AFIX 23 H10A 2 0.589101 0.138157 0.417554 11.00000 -1.20000 H10B 2 0.584592 0.465244 0.352147 11.00000 -1.20000 AFIX 0 C11 1 0.496116 0.238358 0.372662 11.00000 0.04276 0.05858 = 0.04925 -0.00160 -0.00106 0.00154 HKLF 4 REM add24_a.res in Pca2(1) REM R1 = 0.0542 for 1685 Fo > 4sig(Fo) and 0.0852 for all 2644 data REM 163 parameters refined using 1 restraints END WGHT 0.0698 0.0000 REM Highest difference peak 0.214, deepest hole -0.163, 1-sigma level 0.042 Q1 1 0.8273 0.6445 0.4240 11.00000 0.05 0.16 Q2 1 0.6623 0.5491 0.4954 11.00000 0.05 0.15 Q3 1 0.4416 0.5422 0.4747 11.00000 0.05 0.14 Q4 1 0.6485 -0.1761 0.5995 11.00000 0.05 0.14 Q5 1 0.4603 0.5885 0.4167 11.00000 0.05 0.13 Q6 1 0.5580 -0.0355 0.2638 11.00000 0.05 0.13 Q7 1 0.4978 0.6423 0.5016 11.00000 0.05 0.12 Q8 1 0.6760 0.7668 0.5982 11.00000 0.05 0.12 Q9 1 0.7171 -0.0551 0.6215 11.00000 0.05 0.12 Q10 1 0.8210 0.4804 0.5075 11.00000 0.05 0.12 Q11 1 0.6771 0.6666 0.5994 11.00000 0.05 0.11 Q12 1 0.7208 -0.3433 0.7093 11.00000 0.05 0.11 Q13 1 0.8814 0.0730 0.7769 11.00000 0.05 0.11 Q14 1 0.9025 0.3705 0.5836 11.00000 0.05 0.11 Q15 1 0.6034 0.6980 0.4808 11.00000 0.05 0.11 Q16 1 0.6813 0.6091 0.3618 11.00000 0.05 0.11 Q17 1 0.8375 -0.3467 0.7410 11.00000 0.05 0.11 Q18 1 0.6017 0.5905 0.4563 11.00000 0.05 0.11 Q19 1 0.7586 -0.2307 0.5994 11.00000 0.05 0.10 Q20 1 0.5180 0.6598 0.4295 11.00000 0.05 0.10 ; _shelx_res_checksum 6381 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.71945(18) 0.6064(8) 0.4159(2) 0.0790(10) Uani 1 1 d . . . . . O2 O 0.61252(14) 0.0832(8) 0.7035(2) 0.0691(9) Uani 1 1 d . . . . . O3 O 0.56335(13) 0.5462(5) 0.4900(2) 0.0559(7) Uani 1 1 d . . . . . O4 O 0.44663(15) 0.3053(8) 0.4156(3) 0.0785(9) Uani 1 1 d . . . . . O5 O 0.49853(16) 0.0591(7) 0.2911(2) 0.0654(8) Uani 1 1 d . . . . . H5O H 0.458(3) 0.017(10) 0.264(4) 0.075(14) Uiso 1 1 d . . . . . N1 N 0.67089(15) 0.3270(7) 0.5798(2) 0.0502(7) Uani 1 1 d . . . . . H1N H 0.665(2) 0.431(12) 0.522(4) 0.075(13) Uiso 1 1 d . . . . . C1 C 0.73581(17) 0.2393(8) 0.6047(3) 0.0484(8) Uani 1 1 d . . . . . C2 C 0.7527(2) 0.0773(9) 0.6905(3) 0.0560(9) Uani 1 1 d . . . . . H2 H 0.721040 0.020945 0.736582 0.067 Uiso 1 1 calc R U . . . C3 C 0.8177(2) -0.0002(11) 0.7071(3) 0.0637(10) Uani 1 1 d . . . . . H3 H 0.829091 -0.109191 0.765189 0.076 Uiso 1 1 calc R U . . . C4 C 0.8654(2) 0.0773(10) 0.6416(3) 0.0669(11) Uani 1 1 d . . . . . H4 H 0.908676 0.021475 0.654726 0.080 Uiso 1 1 calc R U . . . C5 C 0.8492(2) 0.2377(10) 0.5565(3) 0.0631(10) Uani 1 1 d . . . . . H5 H 0.881727 0.293212 0.511705 0.076 Uiso 1 1 calc R U . . . C6 C 0.78484(19) 0.3194(9) 0.5358(3) 0.0524(9) Uani 1 1 d . . . . . C7 C 0.7721(2) 0.4971(12) 0.4441(4) 0.0685(11) Uani 1 1 d . . . . . H7 H 0.807667 0.530831 0.402716 0.082 Uiso 1 1 calc R U . . . C8 C 0.61545(18) 0.2461(8) 0.6265(3) 0.0520(9) Uani 1 1 d . . . . . C9 C 0.55363(19) 0.3654(9) 0.5780(3) 0.0555(9) Uani 1 1 d . . . . . H9A H 0.526422 0.168995 0.564375 0.067 Uiso 1 1 calc R U . . . H9B H 0.530066 0.509933 0.623496 0.067 Uiso 1 1 calc R U . . . C10 C 0.56357(17) 0.3414(9) 0.4049(3) 0.0518(8) Uani 1 1 d . . . . . H10A H 0.589101 0.138157 0.417554 0.062 Uiso 1 1 calc R U . . . H10B H 0.584592 0.465244 0.352147 0.062 Uiso 1 1 calc R U . . . C11 C 0.49612(17) 0.2384(8) 0.3727(3) 0.0502(8) 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 O1 0.077(2) 0.100(2) 0.0606(19) 0.0299(16) -0.0045(15) -0.0124(17) O2 0.0509(17) 0.100(2) 0.0567(17) 0.0189(15) 0.0062(13) -0.0056(13) O3 0.0607(17) 0.0497(11) 0.0575(15) 0.0024(12) -0.0116(13) -0.0023(10) O4 0.0450(16) 0.110(2) 0.081(2) -0.0271(19) 0.0074(15) 0.0051(15) O5 0.0443(16) 0.096(2) 0.0558(17) -0.0179(16) 0.0001(13) -0.0048(14) N1 0.0459(17) 0.0609(16) 0.0437(16) 0.0089(14) 0.0001(13) -0.0070(12) C1 0.048(2) 0.0522(15) 0.0454(17) 0.0016(14) -0.0013(16) -0.0078(13) C2 0.052(2) 0.0684(19) 0.0478(19) 0.0093(17) 0.0011(16) -0.0052(16) C3 0.060(3) 0.074(3) 0.057(2) 0.0116(19) -0.0077(19) 0.0001(17) C4 0.049(2) 0.080(3) 0.071(3) 0.008(2) -0.007(2) 0.0002(18) C5 0.047(2) 0.074(2) 0.068(3) 0.003(2) 0.008(2) -0.0095(16) C6 0.054(2) 0.0579(18) 0.0455(19) 0.0015(15) 0.0010(16) -0.0127(14) C7 0.063(3) 0.088(3) 0.055(2) 0.019(2) 0.000(2) -0.018(2) C8 0.053(2) 0.0546(17) 0.049(2) 0.0004(16) 0.0021(16) -0.0053(14) C9 0.050(2) 0.0603(18) 0.056(2) -0.0006(18) 0.0007(16) 0.0003(14) C10 0.0413(19) 0.0585(18) 0.056(2) -0.0028(17) 0.0015(16) -0.0019(14) C11 0.0428(19) 0.0586(18) 0.049(2) -0.0016(15) -0.0011(16) 0.0015(14) 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' 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 C9 O3 C10 114.4(2) . . ? C11 O5 H5O 114(3) . . ? C8 N1 C1 128.7(3) . . ? C8 N1 H1N 114(3) . . ? C1 N1 H1N 117(3) . . ? C2 C1 C6 119.3(3) . . ? C2 C1 N1 123.6(3) . . ? C6 C1 N1 117.1(3) . . ? C1 C2 C3 118.9(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 122.3(4) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C5 119.2(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C4 C5 C6 120.9(4) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 119.4(4) . . ? C5 C6 C7 117.1(4) . . ? C1 C6 C7 123.5(4) . . ? O1 C7 C6 126.6(4) . . ? O1 C7 H7 116.7 . . ? C6 C7 H7 116.7 . . ? O2 C8 N1 124.7(3) . . ? O2 C8 C9 119.8(3) . . ? N1 C8 C9 115.5(3) . . ? O3 C9 C8 114.4(3) . . ? O3 C9 H9A 108.7 . . ? C8 C9 H9A 108.7 . . ? O3 C9 H9B 108.7 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? O3 C10 C11 113.0(3) . . ? O3 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? O3 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? O4 C11 O5 124.1(4) . . ? O4 C11 C10 125.0(4) . . ? O5 C11 C10 110.9(3) . . ? 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 C7 1.224(6) . ? O2 C8 1.231(4) . ? O3 C9 1.408(5) . ? O3 C10 1.412(5) . ? O4 C11 1.200(4) . ? O5 C11 1.318(5) . ? O5 H5O 0.93(6) . ? N1 C8 1.340(5) . ? N1 C1 1.415(5) . ? N1 H1N 0.90(5) . ? C1 C2 1.377(5) . ? C1 C6 1.411(5) . ? C2 C3 1.384(6) . ? C2 H2 0.9300 . ? C3 C4 1.360(6) . ? C3 H3 0.9300 . ? C4 C5 1.362(6) . ? C4 H4 0.9300 . ? C5 C6 1.386(6) . ? C5 H5 0.9300 . ? C6 C7 1.456(6) . ? C7 H7 0.9300 . ? C8 C9 1.504(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.506(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N O1 0.90(5) 1.96(5) 2.682(4) 137(4) . O5 H5O O2 0.93(6) 1.70(6) 2.630(4) 174(5) 2_654 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 C8 N1 C1 C2 -7.0(6) . . . . ? C8 N1 C1 C6 171.8(3) . . . . ? C6 C1 C2 C3 0.5(5) . . . . ? N1 C1 C2 C3 179.3(3) . . . . ? C1 C2 C3 C4 -0.1(6) . . . . ? C2 C3 C4 C5 0.2(7) . . . . ? C3 C4 C5 C6 -0.6(6) . . . . ? C4 C5 C6 C1 0.9(6) . . . . ? C4 C5 C6 C7 178.8(4) . . . . ? C2 C1 C6 C5 -0.9(5) . . . . ? N1 C1 C6 C5 -179.8(3) . . . . ? C2 C1 C6 C7 -178.6(3) . . . . ? N1 C1 C6 C7 2.5(5) . . . . ? C5 C6 C7 O1 -175.6(4) . . . . ? C1 C6 C7 O1 2.1(7) . . . . ? C1 N1 C8 O2 2.3(6) . . . . ? C1 N1 C8 C9 -177.1(3) . . . . ? C10 O3 C9 C8 90.7(4) . . . . ? O2 C8 C9 O3 -179.5(3) . . . . ? N1 C8 C9 O3 -0.1(5) . . . . ? C9 O3 C10 C11 77.8(4) . . . . ? O3 C10 C11 O4 -3.4(6) . . . . ? O3 C10 C11 O5 177.6(3) . . . . ?