data_twin4 _publ_section_related_literature ? _publ_contact_letter ; Please consider this CIF for publication. I certify that this contibution is the original work of those listed as authors; that it has not been published before (in any language or medium) and is not being considered for publication elsewhere; that all authors concur with and are aware of the submission; that all workers involved in the study are listed as authors or given proper credit in the acknowledgements; that I have obtained permission for and acknowledged the source of any excerpts from other copyright works; and that to the best of my knowledge the paper contains no statements which are libellous, unlawful or in any way actionable. All coauthors have made significant scientific contributions to the work reported, including the ideas and their execution, and share responsibility and accountability for the results. ; _publ_requested_category ? _publ_requested_journal ? _publ_contact_author_fax ? # Loop of author details loop_ _publ_author_name _publ_author_address _publ_author_footnote _publ_author_email 'Gervais, Anais' ; Boston University Center for Chemical Methodology and Library Development (CMLD-BU) Department of Chemistry, Boston University 590 Commonwealth Avenue, Boston, MA 02215 ; ; ? ; . 'Lazarski, Kiel' ; Boston University Center for Chemical Methodology and Library Development (CMLD-BU) Department of Chemistry, Boston University 590 Commonwealth Avenue, Boston, MA 02215 ; . . 'Porco, Jr., John A.' ; Boston University Center for Chemical Methodology and Library Development (CMLD-BU) Department of Chemistry, Boston University 590 Commonwealth Avenue, Boston, MA 02215 ; . ; porco@bu.edu ; _publ_section_abstract ; ? ; _publ_section_title ; Total Syntheses of Rhodomyrtosones A and B via Nickel-Mediated Conjugate Addition and Flow Photo-oxygenation ; #Added by publCIF _diffrn_radiation_monochromator Montel #Added by publCIF _audit_update_record ; 2015-02-02 # Formatted by publCIF ; _audit_creation_date 2015-02-02 _audit_creation_method ; Olex2 1.2 (compiled 2014.12.23 svn.r3118 for OlexSys, GUI svn.r4973) ; _shelxl_version_number 2013-4 _publ_contact_author_address ; Boston University Center for Chemical Methodology and Library Development (CMLD-BU) Department of Chemistry, Boston University 590 Commonwealth Avenue, Boston, MA 02215 ; _publ_contact_author_email 'porco@bu.edu' _publ_contact_author_name 'John A. Porco, Jr.' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339--341. Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8. Bruker (2009). SAINT. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Bruker (2009). APEX2. Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Dolmanov, O. V., et al. (2009). OLEX2: A complete structure solution, refinement and analysis program. J. Appl. Cryst. 42, 339-341 (2009). ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H36 O7' _chemical_formula_sum 'C26 H36 O7' _chemical_formula_weight 460.55 _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' 0.0181 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' _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. ; _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_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9488(3) _cell_length_b 11.2504(3) _cell_length_c 20.0504(5) _cell_angle_alpha 90 _cell_angle_beta 94.903(2) _cell_angle_gamma 90 _cell_volume 2460.74(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8058 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 66.347 _cell_measurement_theta_min 4.053 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_T_max 0.86422 _exptl_absorpt_correction_T_min 0.77250 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; TWINABS-2008/4 (Bruker,2010) was used for absorption correction. For component 1: wR2(int) was 0.1299 before and 0.0609 after correction. The Ratio of minimum to maximum transmission is 0.89. The \l/2 correction factor is Not present Final HKLF 4 output contains 81434 reflections, Rint = 0.0517 (35678 with I > 3sig(I), Rint = 0.0476) ; _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 992 _exptl_crystal_description block _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.113 _exptl_crystal_size_mid 0.051 _exptl_crystal_size_min 0.026 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_unetI/netI 0.0279 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 9339 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 66.985 _diffrn_reflns_theta_max 66.985 _diffrn_reflns_theta_min 4.052 _diffrn_ambient_temperature 99.98 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker Proteum-R' _diffrn_measurement_method '\f & \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'rotating anode' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6243 _reflns_number_total 9339 _reflns_special_details ; _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v7.68A (Bruker, 2009)' _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution ? _refine_diff_density_max 0.446 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.072 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 392 _refine_ls_number_reflns 9339 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0669 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+0.7826P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2020 _refine_ls_wR_factor_ref 0.2215 _refine_special_details ; Refined as a 2-component twin. CheckCIF Alerts and Discussion: PLAT413_ALERT_2_C Short Inter XH3 .. XHn H7B .. H26B .. 2.09 Ang. Discussion: C26B is a methyl carbon in the minor component of the disorder. Refinement of the hydrogens for this group, including H26B, was done with a riding model with the hydrogens free to rotate about the C26B-C24B bond. This refinment may not have accurately located the hydrogens within the relatively diffuse electron density of this minor component group, leading to the short intermolecular H .. H distance. PLAT340_ALERT_3_C Low Bond Precision on C-C Bonds .. 0.0046 Ang. Discussion: In order to obtain a converged refinement, a number of DIST and DANG restraints were applied, as well as an EADP constraint for the disorder pair of tertiary carbons, C11A and C11B (restraints and constraints via SHELXL, Sheldrick, 2015). The C-C bond precision was degraded somewhat by the use of the constraint and restraints, leading to the alert. PLAT414_ALERT_2_C Short Intra D-H..H-X H4 .. H11B .. 1.98 Ang. Discussion: H11B belongs to the minor component of a disorder. The position of the intramolecularly hydrogen bonded H4 probably represents an average of two positions, one for each component of the C11B disorder; refining these two H4 positions was not undertaken in order to limit the already large number of parameters in the model and because exact identification of the two disordered positions was not necessary for the goals of the research. PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.5 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Uiso(max)/Uiso(min) .. 4.4 Ratio Discussion: These alerts arise due to C14B and C15B, terminal methyl carbons in the minor component (28%) of a disordered isobutyl group. Their positions are not well resolved within the diffuse electron density within this group. PLAT242_ALERT_2_C Low Ueq as Compared to Neighbors for .. C2 Check PLAT242_ALERT_2_C Low Ueq as Compared to Neighbors for .. C6 Check Discussion: The four methyl groups attached to C2 and C6 have somewhat enlarged ellipsoids, probably due to slight disorders in the torsional angles for the quaternary carbons C2 and C6. Modeling the torsional disorders was not practical given the already large number of parameters. Enlargement of the methyl groups relative to the quaternary carbons that bear them makes physical sense, and thus the two alerts do not indicate any deeper systematic error in the model. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.9334(6) 0.0666(6) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 3. Restrained distances C12A-C11A = C16-C11A = C4-C11A 1.54 with sigma of 0.02 C12B-C11B = C16-C11B = C4-C11B 1.54 with sigma of 0.02 C4-C12A 2.52 with sigma of 0.04 C4-C16 2.52 with sigma of 0.04 C16-C12A 2.52 with sigma of 0.04 C4-C12B 2.52 with sigma of 0.04 C16-C12B 2.52 with sigma of 0.04 C16-C4 2.52 with sigma of 0.04 4. Rigid bond restraints C11A, C12A, C13A, C14A, C14B, C11B, C12B, C13B, C15B with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Uiso/Uaniso restraints and constraints C11A \\sim C12A \\sim C13A \\sim C15A \\sim C14A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 C11B \\sim C12B \\sim C13B \\sim C15B \\sim C14B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C11A) \\sim Ueq, Uanis(C11B) \\sim Ueq, Uanis(C12B) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C13B) \\sim Ueq, Uanis(C14A) \\sim Ueq, Uanis(C15B) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C14B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C11B) = Uanis(C11A) 6. Others Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C23B)= Sof(H23C)=Sof(H23D)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1) Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)= Sof(H25B)=Sof(H25C)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1) Sof(C12B)=Sof(H12C)=Sof(H12D)=Sof(C13B)=Sof(H13B)=Sof(C11B)=Sof(H11B)= Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15B)=Sof(H15D)=Sof(H15E)= Sof(H15F)=1-FVAR(2) Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(C13A)=Sof(H13A)= Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C14A)=Sof(H14A)=Sof(H14B)= Sof(H14C)=FVAR(2) 7.a Ternary CH refined with riding coordinates: C11A(H11A), C24A(H24A), C13A(H13A), C13B(H13B), C11B(H11B), C24B(H24B) 7.b Secondary CH2 refined with riding coordinates: C23A(H23A,H23B), C12A(H12A,H12B), C12B(H12C,H12D), C23B(H23C,H23D) 7.c Aromatic/amide H refined with riding coordinates: C20(H20) 7.d Idealised Me refined as rotating group: C25A(H25A,H25B,H25C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C26A(H26A,H26B, H26C), C15A(H15A,H15B,H15C), C14A(H14A,H14B,H14C), C8(H8A,H8B,H8C), C7(H7A,H7B, H7C), C14B(H14D,H14E,H14F), C15B(H15D,H15E,H15F), C25B(H25D,H25E,H25F), C26B(H26D,H26E,H26F) 7.e Idealised tetrahedral OH refined as rotating group: O3(H3), O4(H4), O5(H5), O6(H6) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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 -0.2246(3) 0.7186(4) 0.56398(14) 0.1129(13) Uani 1 1 d . . . . . O2 O 0.4811(2) 1.0490(2) 0.43104(12) 0.0652(6) Uani 1 1 d . . . . . O3 O 0.2987(2) 1.15965(18) 0.25111(10) 0.0551(5) Uani 1 1 d . . . . . H3 H 0.2501 1.1741 0.2174 0.083 Uiso 1 1 calc GR . . . . O4 O 0.0175(2) 0.8473(2) 0.25934(10) 0.0628(6) Uani 1 1 d . . . . . H4 H -0.0323 0.8313 0.2877 0.094 Uiso 1 1 calc GR . . . . O5 O 0.33166(19) 0.89022(19) 0.43667(10) 0.0555(5) Uani 1 1 d . . . . . H5 H 0.3965 0.9292 0.4454 0.083 Uiso 1 1 calc GR . . . . O6 O 0.1739(2) 0.8199(2) 0.52130(11) 0.0597(6) Uani 1 1 d . . . . . H6 H 0.2091 0.8569 0.4920 0.090 Uiso 1 1 calc GR . . . . O7 O -0.1157(2) 0.72904(19) 0.34318(10) 0.0585(6) Uani 1 1 d . . . . . C1 C -0.1518(3) 0.7421(3) 0.52389(17) 0.0635(9) Uani 1 1 d . . . . . C2 C -0.0226(3) 0.7733(3) 0.54968(15) 0.0562(8) Uani 1 1 d . . . . . C3 C 0.0641(3) 0.7836(2) 0.49553(15) 0.0497(7) Uani 1 1 d . . . . . C4 C 0.0383(3) 0.7546(2) 0.42989(14) 0.0470(7) Uani 1 1 d D . . . . C11A C 0.1501(6) 0.7454(6) 0.3877(3) 0.0406(13) Uani 0.706(8) 1 d D U P A 1 H11A H 0.2228 0.7333 0.4208 0.049 Uiso 0.706(8) 1 calc R . P A 1 C16 C 0.1769(3) 0.8588(2) 0.34954(14) 0.0454(7) Uani 1 1 d D . . . . C17 C 0.2769(3) 0.9255(2) 0.37611(14) 0.0457(6) Uani 1 1 d . . . . . C18 C 0.3245(3) 1.0267(2) 0.34433(14) 0.0461(6) Uani 1 1 d . . . . . C22 C 0.4341(3) 1.0843(3) 0.37557(16) 0.0595(8) Uani 1 1 d . . . . . C23A C 0.4751(7) 1.2012(6) 0.3443(3) 0.0478(16) Uani 0.584(10) 1 d . . P B 1 H23A H 0.4931 1.1859 0.2975 0.057 Uiso 0.584(10) 1 calc R . P B 1 H23B H 0.4070 1.2592 0.3433 0.057 Uiso 0.584(10) 1 calc R . P B 1 C24A C 0.5867(6) 1.2546(6) 0.3819(3) 0.059(2) Uani 0.584(10) 1 d . . P B 1 H24A H 0.6480 1.1905 0.3940 0.071 Uiso 0.584(10) 1 calc R . P B 1 C25A C 0.5542(15) 1.3153(12) 0.4436(9) 0.069(3) Uani 0.584(10) 1 d . . P B 1 H25A H 0.4908 1.3750 0.4320 0.104 Uiso 0.584(10) 1 calc GR . P B 1 H25B H 0.6272 1.3542 0.4654 0.104 Uiso 0.584(10) 1 calc GR . P B 1 H25C H 0.5233 1.2567 0.4742 0.104 Uiso 0.584(10) 1 calc GR . P B 1 C6 C -0.1928(3) 0.7395(3) 0.44963(16) 0.0543(8) Uani 1 1 d . . . . . C10 C -0.2690(4) 0.8509(4) 0.4335(2) 0.0885(13) Uani 1 1 d . . . . . H10A H -0.3384 0.8527 0.4613 0.133 Uiso 1 1 calc GR . . . . H10B H -0.2998 0.8500 0.3862 0.133 Uiso 1 1 calc GR . . . . H10C H -0.2180 0.9215 0.4427 0.133 Uiso 1 1 calc GR . . . . C9 C -0.2699(4) 0.6280(4) 0.4353(2) 0.0791(11) Uani 1 1 d . . . . . H9A H -0.2179 0.5575 0.4422 0.119 Uiso 1 1 calc GR . . . . H9B H -0.3060 0.6299 0.3889 0.119 Uiso 1 1 calc GR . . . . H9C H -0.3354 0.6251 0.4656 0.119 Uiso 1 1 calc GR . . . . C5 C -0.0872(3) 0.7393(2) 0.40447(15) 0.0510(7) Uani 1 1 d . . . . . C26A C 0.6431(9) 1.3467(7) 0.3376(4) 0.078(2) Uani 0.584(10) 1 d . . P B 1 H26A H 0.6659 1.3084 0.2966 0.117 Uiso 0.584(10) 1 calc GR . P B 1 H26B H 0.7163 1.3810 0.3618 0.117 Uiso 0.584(10) 1 calc GR . P B 1 H26C H 0.5833 1.4098 0.3261 0.117 Uiso 0.584(10) 1 calc GR . P B 1 C19 C 0.2596(3) 1.0619(2) 0.28316(14) 0.0472(7) Uani 1 1 d . . . . . C20 C 0.1581(3) 1.0011(3) 0.25718(13) 0.0483(7) Uani 1 1 d . . . . . H20 H 0.1153 1.0272 0.2166 0.058 Uiso 1 1 calc R . . . . C21 C 0.1167(3) 0.9008(3) 0.28988(14) 0.0484(7) Uani 1 1 d . . . . . C12A C 0.1449(4) 0.6331(3) 0.3415(2) 0.0492(12) Uani 0.706(8) 1 d D U P A 1 H12A H 0.1303 0.5621 0.3689 0.059 Uiso 0.706(8) 1 calc R . P A 1 H12B H 0.0744 0.6411 0.3074 0.059 Uiso 0.706(8) 1 calc R . P A 1 C13A C 0.2607(8) 0.6134(8) 0.3061(4) 0.0512(18) Uani 0.706(8) 1 d . U P A 1 H13A H 0.2664 0.6818 0.2747 0.061 Uiso 0.706(8) 1 calc R . P A 1 C15A C 0.2505(5) 0.5020(5) 0.2630(3) 0.0678(15) Uani 0.706(8) 1 d . U P A 1 H15A H 0.2364 0.4330 0.2911 0.102 Uiso 0.706(8) 1 calc GR . P A 1 H15B H 0.3268 0.4907 0.2415 0.102 Uiso 0.706(8) 1 calc GR . P A 1 H15C H 0.1819 0.5106 0.2286 0.102 Uiso 0.706(8) 1 calc GR . P A 1 C14A C 0.3757(7) 0.6165(7) 0.3527(3) 0.085(2) Uani 0.706(8) 1 d . U P A 1 H14A H 0.3975 0.6992 0.3634 0.127 Uiso 0.706(8) 1 calc GR . P A 1 H14B H 0.4425 0.5785 0.3312 0.127 Uiso 0.706(8) 1 calc GR . P A 1 H14C H 0.3619 0.5738 0.3940 0.127 Uiso 0.706(8) 1 calc GR . P A 1 C8 C -0.0252(4) 0.8899(4) 0.5887(2) 0.0873(13) Uani 1 1 d . . . . . H8A H -0.0552 0.9539 0.5585 0.131 Uiso 1 1 calc GR . . . . H8B H 0.0578 0.9091 0.6080 0.131 Uiso 1 1 calc GR . . . . H8C H -0.0797 0.8815 0.6248 0.131 Uiso 1 1 calc GR . . . . C7 C 0.0270(4) 0.6718(4) 0.5971(2) 0.0954(15) Uani 1 1 d . . . . . H7A H -0.0270 0.6619 0.6332 0.143 Uiso 1 1 calc GR . . . . H7B H 0.1098 0.6920 0.6162 0.143 Uiso 1 1 calc GR . . . . H7C H 0.0297 0.5976 0.5717 0.143 Uiso 1 1 calc GR . . . . C12B C 0.2182(13) 0.6481(10) 0.3909(9) 0.081(5) Uani 0.294(8) 1 d D U P A 2 H12C H 0.1805 0.5738 0.4059 0.097 Uiso 0.294(8) 1 calc R . P A 2 H12D H 0.2738 0.6792 0.4285 0.097 Uiso 0.294(8) 1 calc R . P A 2 C13B C 0.296(2) 0.621(2) 0.3265(15) 0.089(7) Uani 0.294(8) 1 d . U P A 2 H13B H 0.3381 0.6955 0.3143 0.107 Uiso 0.294(8) 1 calc R . P A 2 C11B C 0.1210(15) 0.7370(15) 0.3718(8) 0.0406(13) Uani 0.294(8) 1 d D U P A 2 H11B H 0.0688 0.7045 0.3327 0.049 Uiso 0.294(8) 1 calc R . P A 2 C14B C 0.226(2) 0.575(2) 0.2671(13) 0.120(7) Uani 0.294(8) 1 d . U P A 2 H14D H 0.1780 0.5062 0.2791 0.180 Uiso 0.294(8) 1 calc GR . P A 2 H14E H 0.2820 0.5519 0.2339 0.180 Uiso 0.294(8) 1 calc GR . P A 2 H14F H 0.1704 0.6374 0.2482 0.180 Uiso 0.294(8) 1 calc GR . P A 2 C15B C 0.3830(17) 0.5455(14) 0.3611(12) 0.144(9) Uani 0.294(8) 1 d . U P A 2 H15D H 0.4657 0.5755 0.3560 0.216 Uiso 0.294(8) 1 calc GR . P A 2 H15E H 0.3749 0.4650 0.3427 0.216 Uiso 0.294(8) 1 calc GR . P A 2 H15F H 0.3689 0.5439 0.4087 0.216 Uiso 0.294(8) 1 calc GR . P A 2 C24B C 0.5021(8) 1.2853(8) 0.3536(4) 0.054(3) Uani 0.416(10) 1 d . . P B 2 H24B H 0.4120 1.2988 0.3439 0.065 Uiso 0.416(10) 1 calc R . P B 2 C25B C 0.5699(11) 1.3603(8) 0.3038(6) 0.071(3) Uani 0.416(10) 1 d . . P B 2 H25D H 0.6555 1.3711 0.3213 0.106 Uiso 0.416(10) 1 calc GR . P B 2 H25E H 0.5303 1.4381 0.2978 0.106 Uiso 0.416(10) 1 calc GR . P B 2 H25F H 0.5671 1.3192 0.2606 0.106 Uiso 0.416(10) 1 calc GR . P B 2 C23B C 0.5279(10) 1.1572(9) 0.3420(4) 0.055(2) Uani 0.416(10) 1 d . . P B 2 H23C H 0.6117 1.1370 0.3612 0.066 Uiso 0.416(10) 1 calc R . P B 2 H23D H 0.5223 1.1402 0.2934 0.066 Uiso 0.416(10) 1 calc R . P B 2 C26B C 0.541(2) 1.325(2) 0.4310(15) 0.098(10) Uani 0.416(10) 1 d . . P B 2 H26D H 0.6290 1.3125 0.4414 0.147 Uiso 0.416(10) 1 calc GR . P B 2 H26E H 0.4952 1.2774 0.4613 0.147 Uiso 0.416(10) 1 calc GR . P B 2 H26F H 0.5217 1.4095 0.4366 0.147 Uiso 0.416(10) 1 calc GR . P B 2 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 0.094(2) 0.187(4) 0.0639(17) -0.010(2) 0.0435(15) -0.049(2) O2 0.0628(14) 0.0707(14) 0.0623(14) 0.0121(11) 0.0060(11) -0.0070(11) O3 0.0696(13) 0.0467(11) 0.0516(12) 0.0121(9) 0.0201(10) -0.0024(10) O4 0.0705(14) 0.0733(14) 0.0460(11) -0.0046(10) 0.0139(10) -0.0188(12) O5 0.0568(12) 0.0540(12) 0.0562(12) 0.0159(10) 0.0077(9) -0.0009(10) O6 0.0655(14) 0.0644(13) 0.0511(12) 0.0077(10) 0.0151(10) -0.0008(11) O7 0.0697(14) 0.0599(12) 0.0488(12) -0.0116(10) 0.0216(10) -0.0120(10) C1 0.076(2) 0.0633(19) 0.0558(19) -0.0089(15) 0.0349(17) -0.0117(17) C2 0.076(2) 0.0496(16) 0.0465(16) -0.0007(13) 0.0265(15) -0.0039(15) C3 0.0622(18) 0.0373(14) 0.0521(16) 0.0032(12) 0.0202(14) 0.0034(13) C4 0.0617(18) 0.0339(12) 0.0488(16) -0.0018(11) 0.0237(13) -0.0030(12) C11A 0.050(3) 0.0365(17) 0.037(3) -0.007(2) 0.012(2) -0.005(2) C16 0.0575(16) 0.0377(13) 0.0441(14) 0.0004(11) 0.0226(12) 0.0034(12) C17 0.0507(15) 0.0430(14) 0.0458(14) 0.0045(12) 0.0180(12) 0.0063(12) C18 0.0552(16) 0.0394(13) 0.0459(15) 0.0018(11) 0.0181(12) -0.0004(12) C22 0.072(2) 0.0597(18) 0.0493(17) 0.0032(14) 0.0190(15) -0.0104(16) C23A 0.059(4) 0.040(4) 0.046(3) 0.000(2) 0.010(3) -0.010(3) C24A 0.054(4) 0.068(4) 0.058(4) -0.005(3) 0.016(3) -0.005(3) C25A 0.060(6) 0.061(6) 0.089(7) -0.027(5) 0.025(5) 0.008(5) C6 0.0632(18) 0.0468(15) 0.0569(18) -0.0071(13) 0.0283(14) -0.0064(14) C10 0.099(3) 0.083(3) 0.091(3) 0.012(2) 0.049(2) 0.028(2) C9 0.089(3) 0.083(2) 0.071(2) -0.0191(19) 0.036(2) -0.037(2) C5 0.0697(19) 0.0377(13) 0.0491(17) -0.0068(12) 0.0253(14) -0.0051(13) C26A 0.078(5) 0.078(5) 0.083(5) -0.020(4) 0.036(4) -0.029(4) C19 0.0601(17) 0.0407(13) 0.0443(14) 0.0028(11) 0.0248(13) 0.0032(13) C20 0.0610(17) 0.0487(15) 0.0373(13) 0.0017(12) 0.0178(12) 0.0029(13) C21 0.0552(16) 0.0494(15) 0.0435(14) -0.0071(12) 0.0201(12) -0.0022(13) C12A 0.059(3) 0.038(2) 0.054(3) -0.0050(18) 0.023(2) -0.0011(18) C13A 0.054(4) 0.049(4) 0.054(3) 0.000(3) 0.022(3) -0.001(3) C15A 0.072(3) 0.056(3) 0.079(3) -0.022(3) 0.027(3) 0.009(3) C14A 0.082(4) 0.093(5) 0.078(4) -0.026(4) -0.001(3) 0.036(4) C8 0.097(3) 0.087(3) 0.085(3) -0.042(2) 0.048(2) -0.023(2) C7 0.111(3) 0.109(3) 0.072(3) 0.041(2) 0.038(2) 0.011(3) C12B 0.091(9) 0.045(6) 0.113(11) 0.001(6) 0.052(9) -0.004(6) C13B 0.078(16) 0.059(10) 0.135(18) -0.039(11) 0.040(11) 0.007(10) C11B 0.050(3) 0.0365(17) 0.037(3) -0.007(2) 0.012(2) -0.005(2) C14B 0.103(13) 0.117(16) 0.150(14) -0.078(14) 0.068(11) -0.045(12) C15B 0.128(16) 0.077(12) 0.23(3) 0.040(15) 0.040(13) 0.028(12) C24B 0.047(5) 0.064(6) 0.054(4) 0.009(4) 0.014(4) 0.001(4) C25B 0.067(6) 0.058(5) 0.092(7) 0.017(5) 0.033(6) -0.009(5) C23B 0.060(6) 0.054(5) 0.053(4) 0.004(4) 0.015(4) 0.010(4) C26B 0.071(11) 0.089(12) 0.133(18) 0.032(11) 0.006(9) -0.024(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 C1 1.209(4) . ? O2 C22 1.250(4) . ? O3 H3 0.8400 . ? O3 C19 1.361(3) . ? O4 H4 0.8400 . ? O4 C21 1.343(4) . ? O5 H5 0.8400 . ? O5 C17 1.366(3) . ? O6 H6 0.8400 . ? O6 C3 1.332(4) . ? O7 C5 1.247(4) . ? C1 C2 1.506(5) . ? C1 C6 1.518(5) . ? C2 C3 1.506(4) . ? C2 C8 1.529(5) . ? C2 C7 1.554(5) . ? C3 C4 1.362(4) . ? C4 C11A 1.549(7) . ? C4 C5 1.435(5) . ? C4 C11B 1.548(18) . ? C11A H11A 1.0000 . ? C11A C16 1.529(7) . ? C11A C12A 1.565(7) . ? C16 C17 1.395(4) . ? C16 C21 1.398(4) . ? C16 C11B 1.581(18) . ? C17 C18 1.425(4) . ? C18 C22 1.458(5) . ? C18 C19 1.420(4) . ? C22 C23A 1.541(7) . ? C22 C23B 1.516(9) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C23A C24A 1.505(9) . ? C24A H24A 1.0000 . ? C24A C25A 1.483(14) . ? C24A C26A 1.529(9) . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? C6 C10 1.525(5) . ? C6 C9 1.525(5) . ? C6 C5 1.529(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C19 C20 1.370(4) . ? C20 H20 0.9500 . ? C20 C21 1.399(4) . ? C12A H12A 0.9900 . ? C12A H12B 0.9900 . ? C12A C13A 1.522(9) . ? C13A H13A 1.0000 . ? C13A C15A 1.521(10) . ? C13A C14A 1.502(9) . ? C15A H15A 0.9800 . ? C15A H15B 0.9800 . ? C15A H15C 0.9800 . ? C14A H14A 0.9800 . ? C14A H14B 0.9800 . ? C14A H14C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C12B H12C 0.9900 . ? C12B H12D 0.9900 . ? C12B C13B 1.64(3) . ? C12B C11B 1.486(19) . ? C13B H13B 1.0000 . ? C13B C14B 1.45(3) . ? C13B C15B 1.41(2) . ? C11B H11B 1.0000 . ? C14B H14D 0.9800 . ? C14B H14E 0.9800 . ? C14B H14F 0.9800 . ? C15B H15D 0.9800 . ? C15B H15E 0.9800 . ? C15B H15F 0.9800 . ? C24B H24B 1.0000 . ? C24B C25B 1.545(11) . ? C24B C23B 1.490(14) . ? C24B C26B 1.64(3) . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? 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 C19 O3 H3 109.5 . . ? C21 O4 H4 109.5 . . ? C17 O5 H5 109.5 . . ? C3 O6 H6 109.5 . . ? O1 C1 C2 118.5(3) . . ? O1 C1 C6 119.4(3) . . ? C2 C1 C6 122.1(3) . . ? C1 C2 C3 113.7(3) . . ? C1 C2 C8 108.6(3) . . ? C1 C2 C7 107.9(3) . . ? C3 C2 C8 110.1(3) . . ? C3 C2 C7 106.7(3) . . ? C8 C2 C7 109.8(3) . . ? O6 C3 C2 110.4(3) . . ? O6 C3 C4 123.6(3) . . ? C4 C3 C2 125.9(3) . . ? C3 C4 C11A 115.8(3) . . ? C3 C4 C5 119.0(2) . . ? C3 C4 C11B 132.2(7) . . ? C5 C4 C11A 125.1(3) . . ? C5 C4 C11B 108.8(6) . . ? C4 C11A H11A 105.6 . . ? C4 C11A C12A 112.7(4) . . ? C16 C11A C4 114.3(4) . . ? C16 C11A H11A 105.6 . . ? C16 C11A C12A 112.1(4) . . ? C12A C11A H11A 105.6 . . ? C17 C16 C11A 115.8(3) . . ? C17 C16 C21 116.3(2) . . ? C17 C16 C11B 132.0(6) . . ? C21 C16 C11A 127.9(3) . . ? C21 C16 C11B 111.7(6) . . ? O5 C17 C16 117.0(2) . . ? O5 C17 C18 118.7(3) . . ? C16 C17 C18 124.3(3) . . ? C17 C18 C22 118.8(3) . . ? C19 C18 C17 115.8(3) . . ? C19 C18 C22 125.4(2) . . ? O2 C22 C18 120.1(3) . . ? O2 C22 C23A 121.4(4) . . ? O2 C22 C23B 108.9(5) . . ? C18 C22 C23A 117.6(4) . . ? C18 C22 C23B 127.9(4) . . ? C22 C23A H23A 109.0 . . ? C22 C23A H23B 109.0 . . ? H23A C23A H23B 107.8 . . ? C24A C23A C22 112.9(5) . . ? C24A C23A H23A 109.0 . . ? C24A C23A H23B 109.0 . . ? C23A C24A H24A 109.5 . . ? C23A C24A C26A 109.3(6) . . ? C25A C24A C23A 111.1(9) . . ? C25A C24A H24A 109.5 . . ? C25A C24A C26A 108.0(8) . . ? C26A C24A H24A 109.5 . . ? C24A C25A H25A 109.5 . . ? C24A C25A H25B 109.5 . . ? C24A C25A H25C 109.5 . . ? H25A C25A H25B 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? C1 C6 C10 107.6(3) . . ? C1 C6 C9 108.2(3) . . ? C1 C6 C5 113.9(3) . . ? C10 C6 C5 107.7(3) . . ? C9 C6 C10 110.6(3) . . ? C9 C6 C5 108.8(2) . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O7 C5 C4 120.9(3) . . ? O7 C5 C6 116.4(3) . . ? C4 C5 C6 122.7(3) . . ? C24A C26A H26A 109.5 . . ? C24A C26A H26B 109.5 . . ? C24A C26A H26C 109.5 . . ? H26A C26A H26B 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? O3 C19 C18 118.6(3) . . ? O3 C19 C20 120.1(3) . . ? C20 C19 C18 121.2(2) . . ? C19 C20 H20 119.7 . . ? C19 C20 C21 120.6(3) . . ? C21 C20 H20 119.7 . . ? O4 C21 C16 122.9(3) . . ? O4 C21 C20 115.4(3) . . ? C16 C21 C20 121.7(3) . . ? C11A C12A H12A 108.8 . . ? C11A C12A H12B 108.8 . . ? H12A C12A H12B 107.7 . . ? C13A C12A C11A 113.8(5) . . ? C13A C12A H12A 108.8 . . ? C13A C12A H12B 108.8 . . ? C12A C13A H13A 106.3 . . ? C12A C13A C15A 111.2(6) . . ? C15A C13A H13A 106.3 . . ? C14A C13A C12A 113.2(6) . . ? C14A C13A H13A 106.3 . . ? C14A C13A C15A 112.9(7) . . ? C13A C15A H15A 109.5 . . ? C13A C15A H15B 109.5 . . ? C13A C15A H15C 109.5 . . ? H15A C15A H15B 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C13A C14A H14A 109.5 . . ? C13A C14A H14B 109.5 . . ? C13A C14A H14C 109.5 . . ? H14A C14A H14B 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? H12C C12B H12D 108.2 . . ? C13B C12B H12C 109.8 . . ? C13B C12B H12D 109.8 . . ? C11B C12B H12C 109.8 . . ? C11B C12B H12D 109.8 . . ? C11B C12B C13B 109.4(15) . . ? C12B C13B H13B 108.5 . . ? C14B C13B C12B 116(2) . . ? C14B C13B H13B 108.5 . . ? C15B C13B C12B 95.7(19) . . ? C15B C13B H13B 108.5 . . ? C15B C13B C14B 119(2) . . ? C4 C11B C16 111.5(11) . . ? C4 C11B H11B 107.8 . . ? C16 C11B H11B 107.8 . . ? C12B C11B C4 110.1(12) . . ? C12B C11B C16 111.7(12) . . ? C12B C11B H11B 107.8 . . ? C13B C14B H14D 109.5 . . ? C13B C14B H14E 109.5 . . ? C13B C14B H14F 109.5 . . ? H14D C14B H14E 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C13B C15B H15D 109.5 . . ? C13B C15B H15E 109.5 . . ? C13B C15B H15F 109.5 . . ? H15D C15B H15E 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C25B C24B H24B 108.3 . . ? C25B C24B C26B 111.3(12) . . ? C23B C24B H24B 108.3 . . ? C23B C24B C25B 108.6(7) . . ? C23B C24B C26B 112.0(10) . . ? C26B C24B H24B 108.3 . . ? C24B C25B H25D 109.5 . . ? C24B C25B H25E 109.5 . . ? C24B C25B H25F 109.5 . . ? H25D C25B H25E 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C22 C23B H23C 110.1 . . ? C22 C23B H23D 110.1 . . ? C24B C23B C22 108.0(8) . . ? C24B C23B H23C 110.1 . . ? C24B C23B H23D 110.1 . . ? H23C C23B H23D 108.4 . . ? C24B C26B H26D 109.5 . . ? C24B C26B H26E 109.5 . . ? C24B C26B H26F 109.5 . . ? H26D C26B H26E 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? _shelx_res_file ; TITL twin4 in P2(1)/c CELL 1.54178 10.9488 11.2504 20.0504 90 94.903 90 ZERR 4 0.0003 0.0003 0.0005 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H O UNIT 104 144 28 DFIX 1.54 C12A C11A C16 C11A C4 C11A DFIX 1.54 C12B C11B C16 C11B C4 C11B DANG 2.52 C4 C12A DANG 2.52 C4 C16 DANG 2.52 C16 C12A DANG 2.52 C4 C12B DANG 2.52 C16 C12B DANG 2.52 C16 C4 DELU C11A C12A C13A C14A C14B C11B C12B C13B C15B SIMU 0.04 0.08 1.7 C11A C12A C13A C15A C14A SIMU 0.04 0.08 1.7 C11B C12B C13B C15B C14B ISOR C11A C11B C12B C12A C13A C13B C14A C15B C15A C14B EADP C11B C11A L.S. 30 PLAN -30 0 0 TEMP -173.17 BUMP BOND $H fmap 2 acta REM REM REM WGHT 0.103200 0.782600 BASF 0.06660 FVAR 0.59350 0.58429 0.70581 O1 3 -0.224628 0.718554 0.563982 11.00000 0.09425 0.18675 = 0.06393 -0.00982 0.04348 -0.04921 O2 3 0.481098 1.049038 0.431041 11.00000 0.06282 0.07072 = 0.06230 0.01215 0.00601 -0.00700 O3 3 0.298691 1.159647 0.251113 11.00000 0.06958 0.04666 = 0.05155 0.01212 0.02014 -0.00243 AFIX 147 H3 2 0.250086 1.174091 0.217378 11.00000 -1.50000 AFIX 0 O4 3 0.017454 0.847296 0.259338 11.00000 0.07048 0.07334 = 0.04600 -0.00456 0.01392 -0.01875 AFIX 147 H4 2 -0.032318 0.831345 0.287703 11.00000 -1.50000 AFIX 0 O5 3 0.331658 0.890222 0.436666 11.00000 0.05678 0.05401 = 0.05616 0.01589 0.00775 -0.00094 AFIX 147 H5 2 0.396470 0.929209 0.445450 11.00000 -1.50000 AFIX 0 O6 3 0.173941 0.819883 0.521299 11.00000 0.06546 0.06439 = 0.05109 0.00772 0.01514 -0.00080 AFIX 147 H6 2 0.209129 0.856854 0.491985 11.00000 -1.50000 AFIX 0 O7 3 -0.115742 0.729035 0.343185 11.00000 0.06967 0.05988 = 0.04882 -0.01165 0.02165 -0.01197 C1 1 -0.151820 0.742081 0.523895 11.00000 0.07627 0.06334 = 0.05581 -0.00892 0.03490 -0.01167 C2 1 -0.022621 0.773318 0.549681 11.00000 0.07620 0.04956 = 0.04655 -0.00074 0.02649 -0.00395 C3 1 0.064079 0.783599 0.495532 11.00000 0.06220 0.03732 = 0.05212 0.00318 0.02020 0.00339 C4 1 0.038332 0.754633 0.429890 11.00000 0.06168 0.03387 = 0.04876 -0.00181 0.02371 -0.00300 PART 1 C11A 1 0.150135 0.745430 0.387740 31.00000 0.05009 0.03653 = 0.03653 -0.00674 0.01235 -0.00520 AFIX 13 H11A 2 0.222817 0.733347 0.420760 31.00000 -1.20000 AFIX 0 PART 0 C16 1 0.176929 0.858827 0.349544 11.00000 0.05748 0.03773 = 0.04415 0.00037 0.02256 0.00341 C17 1 0.276895 0.925500 0.376112 11.00000 0.05067 0.04296 = 0.04579 0.00447 0.01799 0.00626 C18 1 0.324457 1.026662 0.344330 11.00000 0.05523 0.03940 = 0.04594 0.00177 0.01812 -0.00044 C22 1 0.434122 1.084320 0.375565 11.00000 0.07185 0.05968 = 0.04934 0.00316 0.01899 -0.01044 PART 1 C23A 1 0.475109 1.201248 0.344272 21.00000 0.05895 0.03969 = 0.04568 0.00005 0.01015 -0.00966 AFIX 23 H23A 2 0.493059 1.185944 0.297477 21.00000 -1.20000 H23B 2 0.406971 1.259242 0.343265 21.00000 -1.20000 AFIX 0 C24A 1 0.586718 1.254558 0.381883 21.00000 0.05381 0.06813 = 0.05805 -0.00542 0.01602 -0.00512 AFIX 13 H24A 2 0.647976 1.190510 0.393969 21.00000 -1.20000 AFIX 0 C25A 1 0.554246 1.315259 0.443586 21.00000 0.05994 0.06118 = 0.08927 -0.02718 0.02483 0.00764 AFIX 137 H25A 2 0.490821 1.374995 0.431982 21.00000 -1.50000 H25B 2 0.627174 1.354167 0.465374 21.00000 -1.50000 H25C 2 0.523280 1.256733 0.474183 21.00000 -1.50000 AFIX 0 PART 0 C6 1 -0.192804 0.739489 0.449632 11.00000 0.06317 0.04683 = 0.05688 -0.00705 0.02830 -0.00644 C10 1 -0.269048 0.850874 0.433520 11.00000 0.09866 0.08323 = 0.09052 0.01194 0.04871 0.02785 AFIX 137 H10A 2 -0.338380 0.852709 0.461349 11.00000 -1.50000 H10B 2 -0.299785 0.849989 0.386162 11.00000 -1.50000 H10C 2 -0.217977 0.921507 0.442697 11.00000 -1.50000 AFIX 0 C9 1 -0.269917 0.628045 0.435292 11.00000 0.08884 0.08273 = 0.07061 -0.01911 0.03566 -0.03652 AFIX 137 H9A 2 -0.217858 0.557498 0.442169 11.00000 -1.50000 H9B 2 -0.306005 0.629901 0.388860 11.00000 -1.50000 H9C 2 -0.335438 0.625127 0.465634 11.00000 -1.50000 AFIX 0 C5 1 -0.087183 0.739321 0.404469 11.00000 0.06972 0.03768 = 0.04909 -0.00683 0.02535 -0.00515 PART 1 C26A 1 0.643132 1.346699 0.337619 21.00000 0.07801 0.07811 = 0.08282 -0.01957 0.03632 -0.02901 AFIX 137 H26A 2 0.665920 1.308350 0.296585 21.00000 -1.50000 H26B 2 0.716319 1.381019 0.361835 21.00000 -1.50000 H26C 2 0.583319 1.409789 0.326066 21.00000 -1.50000 AFIX 0 PART 0 C19 1 0.259589 1.061948 0.283163 11.00000 0.06006 0.04066 = 0.04430 0.00281 0.02480 0.00320 C20 1 0.158055 1.001099 0.257181 11.00000 0.06101 0.04875 = 0.03735 0.00174 0.01781 0.00292 AFIX 43 H20 2 0.115346 1.027212 0.216583 11.00000 -1.20000 AFIX 0 C21 1 0.116665 0.900847 0.289878 11.00000 0.05518 0.04940 = 0.04350 -0.00711 0.02011 -0.00217 PART 1 C12A 1 0.144855 0.633069 0.341534 31.00000 0.05859 0.03832 = 0.05366 -0.00499 0.02285 -0.00113 AFIX 23 H12A 2 0.130270 0.562097 0.368944 31.00000 -1.20000 H12B 2 0.074412 0.641081 0.307442 31.00000 -1.20000 AFIX 0 C13A 1 0.260727 0.613416 0.306114 31.00000 0.05423 0.04876 = 0.05365 -0.00036 0.02150 -0.00132 AFIX 13 H13A 2 0.266350 0.681816 0.274674 31.00000 -1.20000 AFIX 0 C15A 1 0.250541 0.502040 0.262988 31.00000 0.07176 0.05594 = 0.07915 -0.02163 0.02699 0.00857 AFIX 137 H15A 2 0.236372 0.432997 0.291113 31.00000 -1.50000 H15B 2 0.326759 0.490750 0.241460 31.00000 -1.50000 H15C 2 0.181928 0.510619 0.228604 31.00000 -1.50000 AFIX 0 C14A 1 0.375658 0.616490 0.352729 31.00000 0.08187 0.09300 = 0.07817 -0.02604 -0.00069 0.03571 AFIX 137 H14A 2 0.397493 0.699219 0.363393 31.00000 -1.50000 H14B 2 0.442549 0.578457 0.331171 31.00000 -1.50000 H14C 2 0.361901 0.573799 0.394029 31.00000 -1.50000 AFIX 0 PART 0 C8 1 -0.025179 0.889926 0.588748 11.00000 0.09679 0.08713 = 0.08477 -0.04175 0.04772 -0.02319 AFIX 137 H8A 2 -0.055229 0.953937 0.558508 11.00000 -1.50000 H8B 2 0.057770 0.909054 0.608016 11.00000 -1.50000 H8C 2 -0.079718 0.881504 0.624753 11.00000 -1.50000 AFIX 0 C7 1 0.027046 0.671827 0.597070 11.00000 0.11074 0.10859 = 0.07205 0.04102 0.03764 0.01061 AFIX 137 H7A 2 -0.027015 0.661948 0.633188 11.00000 -1.50000 H7B 2 0.109810 0.691960 0.616221 11.00000 -1.50000 H7C 2 0.029670 0.597557 0.571693 11.00000 -1.50000 AFIX 0 PART 2 C12B 1 0.218157 0.648149 0.390947 -31.00000 0.09133 0.04515 = 0.11254 0.00094 0.05179 -0.00426 AFIX 23 H12C 2 0.180470 0.573849 0.405905 -31.00000 -1.20000 H12D 2 0.273764 0.679211 0.428454 -31.00000 -1.20000 AFIX 0 C13B 1 0.295879 0.620772 0.326523 -31.00000 0.07750 0.05947 = 0.13491 -0.03864 0.04008 0.00666 AFIX 13 H13B 2 0.338087 0.695523 0.314320 -31.00000 -1.20000 AFIX 0 C11B 1 0.121035 0.737008 0.371819 -31.00000 0.05009 0.03653 = 0.03653 -0.00674 0.01235 -0.00520 AFIX 13 H11B 2 0.068794 0.704471 0.332689 -31.00000 -1.20000 AFIX 0 C14B 1 0.225854 0.575392 0.267110 -31.00000 0.10296 0.11696 = 0.15016 -0.07806 0.06774 -0.04466 AFIX 137 H14D 2 0.177952 0.506220 0.279131 -31.00000 -1.50000 H14E 2 0.282029 0.551944 0.233930 -31.00000 -1.50000 H14F 2 0.170355 0.637407 0.248198 -31.00000 -1.50000 AFIX 0 C15B 1 0.383027 0.545515 0.361130 -31.00000 0.12759 0.07653 = 0.23266 0.03969 0.03959 0.02833 AFIX 137 H15D 2 0.465733 0.575484 0.355968 -31.00000 -1.50000 H15E 2 0.374898 0.464951 0.342699 -31.00000 -1.50000 H15F 2 0.368909 0.543902 0.408732 -31.00000 -1.50000 AFIX 0 C24B 1 0.502080 1.285320 0.353572 -21.00000 0.04732 0.06360 = 0.05395 0.00881 0.01356 0.00136 AFIX 13 H24B 2 0.412015 1.298764 0.343945 -21.00000 -1.20000 AFIX 0 C25B 1 0.569944 1.360273 0.303781 -21.00000 0.06667 0.05821 = 0.09162 0.01743 0.03340 -0.00913 AFIX 137 H25D 2 0.655531 1.371057 0.321341 -21.00000 -1.50000 H25E 2 0.530269 1.438087 0.297849 -21.00000 -1.50000 H25F 2 0.567082 1.319223 0.260566 -21.00000 -1.50000 AFIX 0 C23B 1 0.527929 1.157244 0.342045 -21.00000 0.05952 0.05434 = 0.05335 0.00433 0.01503 0.01029 AFIX 23 H23C 2 0.611674 1.137041 0.361234 -21.00000 -1.20000 H23D 2 0.522260 1.140165 0.293442 -21.00000 -1.20000 AFIX 0 C26B 1 0.540884 1.325168 0.430957 -21.00000 0.07106 0.08854 = 0.13345 0.03245 0.00631 -0.02412 AFIX 137 H26D 2 0.629006 1.312494 0.441370 -21.00000 -1.50000 H26E 2 0.495211 1.277416 0.461284 -21.00000 -1.50000 H26F 2 0.521679 1.409467 0.436575 -21.00000 -1.50000 AFIX 0 HKLF 5 REM twin4 in P2(1)/c REM R1 = 0.0669 for 6243 Fo > 4sig(Fo) and 0.0904 for all 9339 data REM 392 parameters refined using 144 restraints END WGHT 0.1025 0.7897 REM Highest difference peak 0.446, deepest hole -0.318, 1-sigma level 0.072 Q1 1 0.0926 0.7530 0.4091 11.00000 0.05 0.45 Q2 1 -0.2614 0.7918 0.5369 11.00000 0.05 0.38 Q3 1 0.0033 0.7839 0.2878 11.00000 0.05 0.38 Q4 1 0.2026 0.6143 0.3328 11.00000 0.05 0.37 Q5 1 0.1803 0.7943 0.3746 11.00000 0.05 0.31 Q6 1 0.3925 1.0870 0.3096 11.00000 0.05 0.29 Q7 1 -0.1350 0.7412 0.4292 11.00000 0.05 0.29 Q8 1 0.5382 1.1686 0.2850 11.00000 0.05 0.28 Q9 1 0.3957 1.0989 0.3872 11.00000 0.05 0.27 Q10 1 -0.1178 0.7066 0.5120 11.00000 0.05 0.26 Q11 1 0.5438 1.2168 0.3125 11.00000 0.05 0.26 Q12 1 0.5159 1.0485 0.4338 11.00000 0.05 0.26 Q13 1 -0.0705 0.7460 0.5486 11.00000 0.05 0.26 Q14 1 -0.0014 0.7145 0.4597 11.00000 0.05 0.25 Q15 1 -0.1866 0.7026 0.5604 11.00000 0.05 0.25 Q16 1 -0.1807 0.7373 0.3492 11.00000 0.05 0.25 Q17 1 0.0224 0.7783 0.5334 11.00000 0.05 0.25 Q18 1 -0.0281 0.7451 0.4103 11.00000 0.05 0.25 Q19 1 0.2378 0.9329 0.3884 11.00000 0.05 0.25 Q20 1 0.0109 0.7920 0.5072 11.00000 0.05 0.25 Q21 1 0.0662 0.9065 0.2949 11.00000 0.05 0.24 Q22 1 0.0931 0.7237 0.4717 11.00000 0.05 0.24 Q23 1 0.3351 0.9765 0.3494 11.00000 0.05 0.24 Q24 1 0.2035 1.0746 0.2899 11.00000 0.05 0.24 Q25 1 0.2234 0.8633 0.3470 11.00000 0.05 0.23 Q26 1 0.2565 0.8154 0.4964 11.00000 0.05 0.23 Q27 1 0.4905 1.0650 0.2907 11.00000 0.05 0.23 Q28 1 -0.2480 0.6969 0.5737 11.00000 0.05 0.23 Q29 1 0.3089 1.0337 0.2895 11.00000 0.05 0.23 Q30 1 -0.2410 0.7735 0.4557 11.00000 0.05 0.22 ; _shelx_res_checksum 25751 _shelx_hkl_file ; 1 0 0 2246.60 34.0020 1 1 0 0 2517.83 71.4450 -2 1 0 0 2517.83 71.4450 1 1 0 0 197.402 4.28714 2 2 0 0 37.9396 0.97493 2 2 0 0 526.647 7.56576 1 2 0 0 578.118 21.3747 -2 2 0 0 578.118 21.3747 1 3 0 0 33.1304 0.71858 1 3 0 0 5.30713 0.35031 2 4 0 0 1128.86 17.7213 1 4 0 0 108.213 3.74320 2 5 0 0 173.229 3.71230 1 5 0 0 13.3581 0.74081 2 6 0 0 26.8519 1.39451 2 6 0 0 400.001 8.42081 1 7 0 0 20.0285 0.87407 2 7 0 0 364.165 8.49871 1 8 0 0 11.4419 0.55809 1 8 0 0 0.70187 0.45765 2 9 0 0 0.96163 0.53123 2 9 0 0 16.4768 0.69858 1 10 0 0 0.34245 0.46513 2 10 0 0 18.7288 0.74249 1 11 0 0 -0.3317 0.39555 2 11 0 0 1.39056 0.44473 1 12 0 0 6.06767 0.45072 1 12 0 0 0.39388 0.39632 2 0 1 0 0.05005 0.11279 2 0 1 0 1.57044 0.12682 1 1 1 0 2.67646 0.19058 1 1 1 0 0.26228 0.10739 2 1 1 0 2.33490 1.73869 -2 1 1 0 2.33490 1.73869 1 2 1 0 8.36833 0.27846 2 2 1 0 108.524 1.42769 1 2 1 0 116.456 4.17837 -2 2 1 0 116.456 4.17837 1 3 1 0 1887.11 21.5796 1 3 1 0 163.664 3.37149 2 4 1 0 84.2317 1.10195 1 4 1 0 6.82871 0.28904 2 5 1 0 150.762 2.65128 1 5 1 0 7.88642 0.54000 2 6 1 0 13.3169 0.51061 2 6 1 0 197.438 3.20588 1 7 1 0 205.798 3.55319 1 7 1 0 11.6635 0.51403 2 -7 1 1 219.022 11.2223 -2 7 1 0 219.022 11.2223 1 8 1 0 72.1150 1.18107 1 8 1 0 2.76744 0.29968 2 9 1 0 25.9749 0.65162 1 9 1 0 1.25737 0.31582 2 10 1 0 -0.2880 0.32994 1 10 1 0 -0.2874 0.33569 2 11 1 0 0.98567 0.32580 2 11 1 0 25.9172 0.64325 1 12 1 0 0.09046 0.27119 1 12 1 0 -0.2189 0.29804 2 0 2 0 9999.99 257.265 -2 0 2 0 9999.99 257.265 1 0 2 0 750.298 19.2783 2 0 2 0 9102.88 234.100 1 1 2 0 5121.97 74.9882 1 1 2 0 5655.20 123.401 -2 1 2 0 5655.20 123.401 1 1 2 0 434.897 10.0065 2 2 2 0 1298.55 18.2076 1 2 2 0 110.393 2.47037 2 2 2 0 1359.14 52.6890 -2 2 2 0 1359.14 52.6890 1 3 2 0 19.4603 0.49150 2 3 2 0 261.526 3.39051 1 4 2 0 48.9088 0.86818 1 4 2 0 3.98847 0.32477 2 5 2 0 16.6236 0.62064 2 5 2 0 208.353 3.69099 1 -5 2 1 208.150 8.12238 -2 5 2 0 208.150 8.12238 1 6 2 0 0.24482 0.32261 2 6 2 0 13.7181 0.50045 1 -6 2 1 23.1209 2.12075 -2 6 2 0 23.1209 2.12075 1 7 2 0 -0.1786 0.26106 2 7 2 0 0.39395 0.26150 1 8 2 0 24.0529 0.57638 1 8 2 0 1.00864 0.31298 2 9 2 0 0.02990 0.37229 2 9 2 0 1.31416 0.32769 1 10 2 0 -0.0379 0.34659 2 10 2 0 7.52793 0.40458 1 11 2 0 2.01750 0.31326 1 11 2 0 -0.3169 0.30402 2 12 2 0 -0.1623 0.34103 2 12 2 0 5.52712 0.37142 1 0 3 0 0.71877 0.32661 1 0 3 0 -0.2480 0.35270 2 1 3 0 121.195 2.21464 2 1 3 0 1499.39 21.3256 1 1 3 0 1492.65 40.0782 -2 1 3 0 1492.65 40.0782 1 2 3 0 641.198 25.0359 -2 2 3 0 641.198 25.0359 1 2 3 0 621.436 9.47554 1 2 3 0 41.6755 0.94928 2 3 3 0 0.34366 0.37302 2 3 3 0 15.9574 0.52927 1 4 3 0 0.34813 0.43309 2 4 3 0 2.87580 0.42689 1 5 3 0 49.0734 1.42028 2 5 3 0 651.120 12.8241 1 -5 3 1 736.432 42.7868 -2 5 3 0 736.432 42.7868 1 6 3 0 6.05699 0.33200 1 6 3 0 0.14465 0.31258 2 7 3 0 73.5156 1.09509 1 7 3 0 4.55174 0.29072 2 8 3 0 2.79702 0.33240 2 8 3 0 53.0027 1.00071 1 9 3 0 1.67331 0.38684 1 9 3 0 -0.8038 0.37325 2 10 3 0 1.24760 0.39383 1 10 3 0 -0.6013 0.40685 2 11 3 0 0.44356 0.32593 2 11 3 0 16.1765 0.56249 1 12 3 0 0.87312 0.37712 2 12 3 0 7.78658 0.56067 1 0 4 0 7.21925 0.38323 2 0 4 0 65.0870 1.41472 1 0 4 0 76.3107 3.59524 -2 0 4 0 76.3107 3.59524 1 1 4 0 889.820 11.8929 1 1 4 0 80.0829 1.44547 2 1 4 0 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1.82494 2 -3 2 23 0.27208 0.72308 2 -3 2 23 -0.3707 0.72567 1 -2 2 23 0.21401 0.46398 2 -2 2 23 0.16127 0.46022 1 -1 2 23 1.77365 0.47090 2 -1 2 23 14.3177 0.73725 1 0 2 23 2.74000 0.45242 1 0 2 23 0.73052 0.41899 2 1 2 23 0.22987 0.47915 1 1 2 23 0.52765 0.45643 2 -3 3 23 2.93857 0.91287 1 -3 3 23 1.13803 0.91034 2 -2 3 23 3.25966 0.76865 1 -2 3 23 0.42494 0.59379 2 -1 3 23 0.01204 0.70419 2 -1 3 23 1.13195 0.68029 1 0 3 23 0.18992 0.51083 2 0 3 23 -0.0300 0.57772 1 1 3 23 -2.3347 1.32898 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 6054 _olex2_submission_special_instructions 'No special instructions were received' loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.9334(6) 2 0.0666(6)