data_cchwlc _nottingham_internal_coll_name CCHWLC _nottingham_internal_coll_number 15238 _nottingham_internal_coll_client CC/HWL _nottingham_internal_coll_type custom _nottingham_internal_coll_frame_method 'omega scans' _nottingham_internal_coll_frame_time 2.0000 _nottingham_internal_coll_frame_width 2.0000 _nottingham_internal_coll_user pczwl _nottingham_internal_coll_date 26/10/2015 _nottingham_internal_coll_location NOTTS _nottingham_internal_coll_instrument 'SN, XDA 017/09' _nottingham_internal_NCS_number ? _nottingham_internal_process_date 11/11/2015 _nottingham_internal_process_user pczwl _nottingham_internal_solution_date 11/11/2015 _nottingham_internal_solution_user pczwl _nottingham_internal_refinement_date 14/1/2016 _nottingham_internal_refinement_user pczwl _nottingham_internal_self_archive_date ? _nottingham_internal_self_validation_date ? _nottingham_internal_self_validation_user ? _nottingham_internal_validation_date 20/1/2016 _nottingham_internal_validation_user pczwl _nottingham_internal_archive_date 20/1/2016 _refine_special_details ? _vrf_PLAT420_cchwlc ; PROBLEM: D-H Without Acceptor O10 -- H10 ... Please Check RESPONSE: The packing of this molecule is such that O10 sits in a pocket where there are no potential hydrogen bond acceptors. There is the possibility of longer range OH-pi interactions. Refinement of O10 as anything other than and oxygen atom (C/N/F) results in poorer refinement statistics and poorer quality thermal parameters for the atom. ; _audit_creation_date 2016-01-20 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _shelx_SHELXL_version_number '2014/7' _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H. (2015). Acta Cryst. A71, 59-75. 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. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C25 H22 O2' _chemical_formula_sum 'C25 H22 O2' _chemical_formula_weight 354.42 _chemical_absolute_configuration ad _chemical_melting_point ? _chemical_oxdiff_formula 'C25 H22 O2' _chemical_oxdiff_usercomment 'CCHWLC #15238 SN-741 IN FOMBLIN FIML ON A MICROMOUNT FOR CC/HWL' 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 'orthorhombic' _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 5.8337(4) _cell_length_b 14.6798(10) _cell_length_c 20.8894(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1788.9(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4511 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 76.5110 _cell_measurement_theta_min 5.2060 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_correction_T_min 0.727 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 752 _exptl_crystal_size_max 0.6104 _exptl_crystal_size_mid 0.4891 _exptl_crystal_size_min 0.1907 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_unetI/netI 0.0263 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 8896 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.924 _diffrn_reflns_theta_min 5.197 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120(2) _diffrn_crystal_treatment 'flash frozen in gaseous N2' _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 5.1806 _diffrn_detector_type 'Agilent Diffraction Atlas detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 123.00 167.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 111.0000 30.0000 150.0000 22 #__ type_ start__ end____ width___ exp.time_ 2 omega 90.00 174.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 111.0000 30.0000 30.0000 42 #__ type_ start__ end____ width___ exp.time_ 3 omega 87.00 135.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 111.0000 61.0000 -30.0000 24 #__ type_ start__ end____ width___ exp.time_ 4 omega 118.00 178.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 111.0000 111.0000 -180.0000 30 #__ type_ start__ end____ width___ exp.time_ 5 omega 70.00 98.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 111.0000 -45.0000 -90.0000 14 #__ type_ start__ end____ width___ exp.time_ 6 omega 44.00 72.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 111.0000 -30.0000 0.0000 14 #__ type_ start__ end____ width___ exp.time_ 7 omega 36.00 116.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 111.0000 -111.0000 -90.0000 40 #__ type_ start__ end____ width___ exp.time_ 8 omega 38.00 90.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 111.0000 -30.0000 -150.0000 26 #__ type_ start__ end____ width___ exp.time_ 9 omega 41.00 117.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 43.1277 77.0000 0.0000 38 #__ type_ start__ end____ width___ exp.time_ 10 omega 60.00 96.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 111.0000 178.0000 -180.0000 18 #__ type_ start__ end____ width___ exp.time_ 11 omega 41.00 89.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 111.0000 -45.0000 120.0000 24 #__ type_ start__ end____ width___ exp.time_ 12 omega 39.00 105.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 111.0000 -111.0000 120.0000 33 #__ type_ start__ end____ width___ exp.time_ 13 omega 1.00 49.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 43.1277 -99.0000 -30.0000 24 #__ type_ start__ end____ width___ exp.time_ 14 omega -111.00 -17.00 2.0000 2.0000 omega____ theta____ kappa____ phi______ frames - -38.5000 -38.0000 90.0000 47 ; _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'SuperNova-Duo, Atlas' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_orient_matrix_UB_11 -0.2402609000 _diffrn_orient_matrix_UB_12 0.0410922000 _diffrn_orient_matrix_UB_13 -0.0101914000 _diffrn_orient_matrix_UB_21 0.0197616000 _diffrn_orient_matrix_UB_22 0.0504220000 _diffrn_orient_matrix_UB_23 0.0644159000 _diffrn_orient_matrix_UB_31 0.1078275000 _diffrn_orient_matrix_UB_32 0.0823262000 _diffrn_orient_matrix_UB_33 -0.0344607000 _diffrn_radiation_collimation 'focusing mirrors' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_wavelength_determination fundamental _diffrn_source 'microfocus sealed tube' _diffrn_source_current 0.8 _diffrn_source_power 0.04 _diffrn_source_target Cu _diffrn_source_type 'Agilent Diffraction microfocus tube' _diffrn_source_voltage 50 _reflns_Friedel_coverage 0.706 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.973 _reflns_number_gt 3629 _reflns_number_total 3717 _reflns_odcompleteness_completeness 99.89 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _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 ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _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 'olex2.solve (Bourhis et al., 2015)' _refine_diff_density_max 0.160 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.049 _refine_ls_abs_structure_details ; Flack x determined using 1472 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.09(9) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 248 _refine_ls_number_reflns 3717 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0330 _refine_ls_restrained_S_all 1.110 _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^)+(0.0469P)^2^+0.3117P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.0846 _olex2_refinement_description ; 1. 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 2.a Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B) 2.b Aromatic/amide H refined with riding coordinates: C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26) 2.c Idealised Me refined as rotating group: C27(H27A,H27B,H27C) ; _atom_sites_solution_hydrogens mixed _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 C1 C 0.8054(3) 0.82299(11) 0.37117(8) 0.0165(3) Uani 1 1 d . . . . . C2 C 0.7886(3) 0.83899(12) 0.29999(8) 0.0203(4) Uani 1 1 d . . . . . H2A H 0.7828 0.9049 0.2902 0.024 Uiso 1 1 calc R . . . . H2B H 0.6507 0.8092 0.2820 0.024 Uiso 1 1 calc R . . . . C3 C 1.0073(3) 0.79592(12) 0.27366(8) 0.0179(4) Uani 1 1 d . . . . . H3A H 1.1366 0.8395 0.2754 0.021 Uiso 1 1 calc R . . . . H3B H 0.9854 0.7761 0.2288 0.021 Uiso 1 1 calc R . . . . C4 C 1.0521(3) 0.71414(12) 0.31732(8) 0.0152(3) Uani 1 1 d . . . . . C5 C 0.9041(3) 0.63055(11) 0.30433(8) 0.0143(3) Uani 1 1 d . . . . . C6 C 0.8017(3) 0.60150(11) 0.35887(8) 0.0154(3) Uani 1 1 d . . . . . C7 C 0.8475(3) 0.66451(11) 0.41438(8) 0.0192(4) Uani 1 1 d . . . . . H7A H 0.9429 0.6341 0.4472 0.023 Uiso 1 1 calc R . . . . H7B H 0.7022 0.6846 0.4344 0.023 Uiso 1 1 calc R . . . . C8 C 0.9754(3) 0.74555(11) 0.38478(8) 0.0156(3) Uani 1 1 d . . . . . O9 O 0.7035(2) 0.86451(9) 0.41247(6) 0.0234(3) Uani 1 1 d . . . . . O10 O 1.2922(2) 0.69271(9) 0.31270(6) 0.0207(3) Uani 1 1 d . . . . . H10 H 1.316(5) 0.6403(18) 0.3300(12) 0.031 Uiso 1 1 d R . . . . C11 C 0.8859(3) 0.59388(11) 0.23833(8) 0.0148(3) Uani 1 1 d . . . . . C12 C 1.0698(3) 0.60237(12) 0.19530(8) 0.0179(3) Uani 1 1 d . . . . . H12 H 1.2082 0.6302 0.2092 0.021 Uiso 1 1 calc R . . . . C13 C 1.0526(3) 0.57073(12) 0.13286(8) 0.0208(4) Uani 1 1 d . . . . . H13 H 1.1786 0.5773 0.1044 0.025 Uiso 1 1 calc R . . . . C14 C 0.8525(3) 0.52962(12) 0.11180(8) 0.0215(4) Uani 1 1 d . . . . . H14 H 0.8420 0.5071 0.0693 0.026 Uiso 1 1 calc R . . . . C15 C 0.6674(3) 0.52152(12) 0.15326(9) 0.0214(4) Uani 1 1 d . . . . . H15 H 0.5298 0.4936 0.1390 0.026 Uiso 1 1 calc R . . . . C16 C 0.6829(3) 0.55423(12) 0.21571(8) 0.0182(3) Uani 1 1 d . . . . . H16 H 0.5541 0.5496 0.2433 0.022 Uiso 1 1 calc R . . . . C17 C 0.6616(3) 0.51896(11) 0.37052(8) 0.0158(3) Uani 1 1 d . . . . . C18 C 0.4848(3) 0.52022(11) 0.41445(8) 0.0172(3) Uani 1 1 d . . . . . H18 H 0.4546 0.5748 0.4374 0.021 Uiso 1 1 calc R . . . . C19 C 0.3469(3) 0.44251(11) 0.42639(8) 0.0161(3) Uani 1 1 d . . . . . C20 C 0.1645(3) 0.44355(12) 0.47134(8) 0.0190(4) Uani 1 1 d . . . . . H20 H 0.1336 0.4975 0.4949 0.023 Uiso 1 1 calc R . . . . C21 C 0.0329(3) 0.36787(13) 0.48106(9) 0.0222(4) Uani 1 1 d . . . . . H21 H -0.0886 0.3695 0.5113 0.027 Uiso 1 1 calc R . . . . C22 C 0.0765(3) 0.28719(13) 0.44634(9) 0.0220(4) Uani 1 1 d . . . . . H22 H -0.0167 0.2350 0.4531 0.026 Uiso 1 1 calc R . . . . C23 C 0.2521(3) 0.28373(12) 0.40309(9) 0.0197(4) Uani 1 1 d . . . . . H23 H 0.2800 0.2290 0.3801 0.024 Uiso 1 1 calc R . . . . C24 C 0.3930(3) 0.36073(12) 0.39211(8) 0.0170(3) Uani 1 1 d . . . . . C25 C 0.5821(3) 0.35952(12) 0.34927(8) 0.0192(4) Uani 1 1 d . . . . . H25 H 0.6187 0.3048 0.3273 0.023 Uiso 1 1 calc R . . . . C26 C 0.7121(3) 0.43534(12) 0.33905(8) 0.0185(3) Uani 1 1 d . . . . . H26 H 0.8385 0.4323 0.3105 0.022 Uiso 1 1 calc R . . . . C27 C 1.1668(3) 0.78323(13) 0.42700(9) 0.0216(4) Uani 1 1 d . . . . . H27A H 1.2653 0.7331 0.4413 0.032 Uiso 1 1 calc GR . . . . H27B H 1.0999 0.8137 0.4643 0.032 Uiso 1 1 calc GR . . . . H27C H 1.2582 0.8270 0.4025 0.032 Uiso 1 1 calc GR . . . . 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 0.0159(7) 0.0149(7) 0.0188(8) -0.0001(6) -0.0002(7) -0.0040(7) C2 0.0241(9) 0.0169(8) 0.0198(8) 0.0018(6) -0.0024(7) 0.0029(7) C3 0.0214(9) 0.0166(8) 0.0158(8) 0.0025(6) 0.0008(6) -0.0037(7) C4 0.0127(7) 0.0174(7) 0.0156(7) -0.0004(6) 0.0000(6) -0.0003(7) C5 0.0134(7) 0.0140(7) 0.0156(8) 0.0001(6) -0.0003(6) 0.0020(6) C6 0.0170(8) 0.0141(7) 0.0151(8) -0.0001(6) 0.0005(6) 0.0018(7) C7 0.0264(9) 0.0158(8) 0.0153(8) 0.0000(6) 0.0013(7) -0.0017(7) C8 0.0170(8) 0.0156(7) 0.0142(7) -0.0010(6) -0.0002(6) -0.0009(7) O9 0.0230(6) 0.0226(6) 0.0247(6) -0.0029(5) 0.0053(5) 0.0034(5) O10 0.0132(6) 0.0248(6) 0.0241(6) -0.0018(5) 0.0007(5) 0.0004(5) C11 0.0166(8) 0.0126(7) 0.0152(8) 0.0008(6) 0.0015(6) 0.0024(6) C12 0.0165(8) 0.0183(8) 0.0188(8) 0.0022(6) 0.0023(7) 0.0020(7) C13 0.0245(9) 0.0205(8) 0.0175(8) 0.0015(7) 0.0046(7) 0.0072(7) C14 0.0317(10) 0.0180(8) 0.0146(8) -0.0020(6) -0.0027(7) 0.0064(7) C15 0.0241(9) 0.0189(8) 0.0210(9) -0.0014(7) -0.0051(7) -0.0005(8) C16 0.0186(8) 0.0186(8) 0.0173(8) 0.0009(6) -0.0005(7) 0.0000(7) C17 0.0191(8) 0.0149(7) 0.0133(7) 0.0019(6) 0.0003(6) 0.0008(7) C18 0.0213(9) 0.0136(7) 0.0166(8) -0.0011(6) 0.0012(7) 0.0011(7) C19 0.0183(8) 0.0166(7) 0.0135(7) 0.0014(6) -0.0005(6) 0.0013(7) C20 0.0214(9) 0.0173(8) 0.0184(8) 0.0004(7) 0.0021(7) 0.0029(7) C21 0.0193(8) 0.0253(9) 0.0218(9) 0.0036(7) 0.0037(7) 0.0002(7) C22 0.0217(9) 0.0198(8) 0.0245(9) 0.0040(7) -0.0005(7) -0.0052(7) C23 0.0227(9) 0.0159(8) 0.0203(8) 0.0001(6) -0.0022(7) -0.0002(7) C24 0.0196(8) 0.0166(8) 0.0149(7) 0.0018(6) -0.0015(6) 0.0017(7) C25 0.0242(9) 0.0157(8) 0.0175(8) -0.0016(6) 0.0016(7) 0.0017(7) C26 0.0212(8) 0.0180(8) 0.0164(8) 0.0005(6) 0.0039(7) 0.0023(7) C27 0.0219(9) 0.0226(8) 0.0202(8) -0.0037(7) -0.0049(7) -0.0005(7) _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 1.508(2) . ? C1 C8 1.535(2) . ? C1 O9 1.212(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.527(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.530(2) . ? C4 C5 1.525(2) . ? C4 C8 1.549(2) . ? C4 O10 1.439(2) . ? C5 C6 1.355(2) . ? C5 C11 1.484(2) . ? C6 C7 1.507(2) . ? C6 C17 1.482(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.534(2) . ? C8 C27 1.527(2) . ? O10 H10 0.86(3) . ? C11 C12 1.405(2) . ? C11 C16 1.402(2) . ? C12 H12 0.9500 . ? C12 C13 1.388(2) . ? C13 H13 0.9500 . ? C13 C14 1.385(3) . ? C14 H14 0.9500 . ? C14 C15 1.389(3) . ? C15 H15 0.9500 . ? C15 C16 1.393(2) . ? C16 H16 0.9500 . ? C17 C18 1.381(2) . ? C17 C26 1.423(2) . ? C18 H18 0.9500 . ? C18 C19 1.418(2) . ? C19 C20 1.419(2) . ? C19 C24 1.424(2) . ? C20 H20 0.9500 . ? C20 C21 1.366(3) . ? C21 H21 0.9500 . ? C21 C22 1.412(3) . ? C22 H22 0.9500 . ? C22 C23 1.367(3) . ? C23 H23 0.9500 . ? C23 C24 1.416(2) . ? C24 C25 1.420(2) . ? C25 H25 0.9500 . ? C25 C26 1.364(3) . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 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 C2 C1 C8 109.88(14) . . ? O9 C1 C2 126.24(16) . . ? O9 C1 C8 123.87(16) . . ? C1 C2 H2A 111.0 . . ? C1 C2 H2B 111.0 . . ? C1 C2 C3 103.66(14) . . ? H2A C2 H2B 109.0 . . ? C3 C2 H2A 111.0 . . ? C3 C2 H2B 111.0 . . ? C2 C3 H3A 110.8 . . ? C2 C3 H3B 110.8 . . ? C2 C3 C4 104.65(13) . . ? H3A C3 H3B 108.9 . . ? C4 C3 H3A 110.8 . . ? C4 C3 H3B 110.8 . . ? C3 C4 C8 105.03(13) . . ? C5 C4 C3 115.38(14) . . ? C5 C4 C8 103.77(13) . . ? O10 C4 C3 107.33(14) . . ? O10 C4 C5 111.31(13) . . ? O10 C4 C8 114.03(13) . . ? C6 C5 C4 110.69(14) . . ? C6 C5 C11 129.44(16) . . ? C11 C5 C4 119.86(14) . . ? C5 C6 C7 112.04(15) . . ? C5 C6 C17 129.69(15) . . ? C17 C6 C7 118.26(14) . . ? C6 C7 H7A 110.8 . . ? C6 C7 H7B 110.8 . . ? C6 C7 C8 104.61(14) . . ? H7A C7 H7B 108.9 . . ? C8 C7 H7A 110.8 . . ? C8 C7 H7B 110.8 . . ? C1 C8 C4 103.80(13) . . ? C7 C8 C1 109.55(14) . . ? C7 C8 C4 106.04(13) . . ? C27 C8 C1 108.13(14) . . ? C27 C8 C4 114.98(14) . . ? C27 C8 C7 113.82(14) . . ? C4 O10 H10 109.0(18) . . ? C12 C11 C5 120.49(15) . . ? C16 C11 C5 121.62(15) . . ? C16 C11 C12 117.80(16) . . ? C11 C12 H12 119.5 . . ? C13 C12 C11 121.06(17) . . ? C13 C12 H12 119.5 . . ? C12 C13 H13 119.8 . . ? C14 C13 C12 120.34(17) . . ? C14 C13 H13 119.8 . . ? C13 C14 H14 120.2 . . ? C13 C14 C15 119.60(16) . . ? C15 C14 H14 120.2 . . ? C14 C15 H15 119.9 . . ? C14 C15 C16 120.27(17) . . ? C16 C15 H15 119.9 . . ? C11 C16 H16 119.6 . . ? C15 C16 C11 120.89(17) . . ? C15 C16 H16 119.6 . . ? C18 C17 C6 120.68(15) . . ? C18 C17 C26 118.25(15) . . ? C26 C17 C6 121.01(15) . . ? C17 C18 H18 119.0 . . ? C17 C18 C19 122.00(15) . . ? C19 C18 H18 119.0 . . ? C18 C19 C20 122.21(15) . . ? C18 C19 C24 118.85(15) . . ? C20 C19 C24 118.93(16) . . ? C19 C20 H20 119.6 . . ? C21 C20 C19 120.74(16) . . ? C21 C20 H20 119.6 . . ? C20 C21 H21 119.8 . . ? C20 C21 C22 120.31(17) . . ? C22 C21 H21 119.8 . . ? C21 C22 H22 119.8 . . ? C23 C22 C21 120.39(17) . . ? C23 C22 H22 119.8 . . ? C22 C23 H23 119.6 . . ? C22 C23 C24 120.83(16) . . ? C24 C23 H23 119.6 . . ? C23 C24 C19 118.79(15) . . ? C23 C24 C25 122.87(16) . . ? C25 C24 C19 118.32(16) . . ? C24 C25 H25 119.3 . . ? C26 C25 C24 121.36(16) . . ? C26 C25 H25 119.3 . . ? C17 C26 H26 119.5 . . ? C25 C26 C17 121.08(16) . . ? C25 C26 H26 119.5 . . ? C8 C27 H27A 109.5 . . ? C8 C27 H27B 109.5 . . ? C8 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? 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 C3 C4 33.88(17) . . . . ? C2 C1 C8 C4 -1.95(18) . . . . ? C2 C1 C8 C7 -114.85(16) . . . . ? C2 C1 C8 C27 120.59(16) . . . . ? C2 C3 C4 C5 77.83(17) . . . . ? C2 C3 C4 C8 -35.76(17) . . . . ? C2 C3 C4 O10 -157.47(13) . . . . ? C3 C4 C5 C6 -128.06(16) . . . . ? C3 C4 C5 C11 50.8(2) . . . . ? C3 C4 C8 C1 22.96(16) . . . . ? C3 C4 C8 C7 138.37(14) . . . . ? C3 C4 C8 C27 -94.94(16) . . . . ? C4 C5 C6 C7 4.9(2) . . . . ? C4 C5 C6 C17 -173.74(17) . . . . ? C4 C5 C11 C12 30.7(2) . . . . ? C4 C5 C11 C16 -145.91(16) . . . . ? C5 C4 C8 C1 -98.56(14) . . . . ? C5 C4 C8 C7 16.84(17) . . . . ? C5 C4 C8 C27 143.54(15) . . . . ? C5 C6 C7 C8 6.2(2) . . . . ? C5 C6 C17 C18 -147.48(19) . . . . ? C5 C6 C17 C26 35.5(3) . . . . ? C5 C11 C12 C13 -178.10(15) . . . . ? C5 C11 C16 C15 178.90(15) . . . . ? C6 C5 C11 C12 -150.62(18) . . . . ? C6 C5 C11 C16 32.8(3) . . . . ? C6 C7 C8 C1 97.12(16) . . . . ? C6 C7 C8 C4 -14.31(17) . . . . ? C6 C7 C8 C27 -141.70(15) . . . . ? C6 C17 C18 C19 179.62(16) . . . . ? C6 C17 C26 C25 -179.39(16) . . . . ? C7 C6 C17 C18 33.9(2) . . . . ? C7 C6 C17 C26 -143.13(17) . . . . ? C8 C1 C2 C3 -19.72(18) . . . . ? C8 C4 C5 C6 -13.74(18) . . . . ? C8 C4 C5 C11 165.16(14) . . . . ? O9 C1 C2 C3 159.71(17) . . . . ? O9 C1 C8 C4 178.59(17) . . . . ? O9 C1 C8 C7 65.7(2) . . . . ? O9 C1 C8 C27 -58.9(2) . . . . ? O10 C4 C5 C6 109.33(16) . . . . ? O10 C4 C5 C11 -71.77(19) . . . . ? O10 C4 C8 C1 140.18(14) . . . . ? O10 C4 C8 C7 -104.41(16) . . . . ? O10 C4 C8 C27 22.3(2) . . . . ? C11 C5 C6 C7 -173.85(16) . . . . ? C11 C5 C6 C17 7.5(3) . . . . ? C11 C12 C13 C14 -0.2(3) . . . . ? C12 C11 C16 C15 2.2(2) . . . . ? C12 C13 C14 C15 1.0(3) . . . . ? C13 C14 C15 C16 -0.2(3) . . . . ? C14 C15 C16 C11 -1.5(3) . . . . ? C16 C11 C12 C13 -1.4(2) . . . . ? C17 C6 C7 C8 -174.99(15) . . . . ? C17 C18 C19 C20 -179.80(17) . . . . ? C17 C18 C19 C24 0.2(3) . . . . ? C18 C17 C26 C25 3.5(3) . . . . ? C18 C19 C20 C21 179.09(18) . . . . ? C18 C19 C24 C23 -178.69(16) . . . . ? C18 C19 C24 C25 2.6(2) . . . . ? C19 C20 C21 C22 0.0(3) . . . . ? C19 C24 C25 C26 -2.4(3) . . . . ? C20 C19 C24 C23 1.3(2) . . . . ? C20 C19 C24 C25 -177.38(16) . . . . ? C20 C21 C22 C23 0.6(3) . . . . ? C21 C22 C23 C24 -0.2(3) . . . . ? C22 C23 C24 C19 -0.8(3) . . . . ? C22 C23 C24 C25 177.84(17) . . . . ? C23 C24 C25 C26 178.95(17) . . . . ? C24 C19 C20 C21 -0.9(3) . . . . ? C24 C25 C26 C17 -0.7(3) . . . . ? C26 C17 C18 C19 -3.2(3) . . . . ? _shelx_res_file ; cchwlc.res created by SHELXL-2014/7 TITL CELL 1.54184 5.833721 14.679818 20.889359 90 90 90 ZERR 4 0.000388 0.001003 0.001537 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H O UNIT 100 88 8 L.S. 12 PLAN 20 TEMP -153(2) MORE -1 BOND $H CONF fmap 2 acta OMIT 0 0 2 OMIT 0 1 1 OMIT 5 13 1 REM REM REM WGHT 0.046900 0.311700 FVAR 11.36491 C1 1 0.805447 0.822986 0.371165 11.00000 0.01592 0.01492 = 0.01879 -0.00015 -0.00024 -0.00395 C2 1 0.788584 0.838989 0.299990 11.00000 0.02405 0.01693 = 0.01984 0.00177 -0.00245 0.00290 AFIX 23 H2A 2 0.782782 0.904923 0.290164 11.00000 -1.20000 H2B 2 0.650730 0.809164 0.281972 11.00000 -1.20000 AFIX 0 C3 1 1.007300 0.795918 0.273661 11.00000 0.02136 0.01659 = 0.01578 0.00252 0.00077 -0.00374 AFIX 23 H3A 2 1.136564 0.839543 0.275412 11.00000 -1.20000 H3B 2 0.985436 0.776064 0.228782 11.00000 -1.20000 AFIX 0 C4 1 1.052092 0.714136 0.317321 11.00000 0.01274 0.01740 = 0.01559 -0.00040 -0.00005 -0.00033 C5 1 0.904115 0.630552 0.304330 11.00000 0.01335 0.01401 = 0.01556 0.00006 -0.00028 0.00201 C6 1 0.801650 0.601502 0.358870 11.00000 0.01699 0.01409 = 0.01508 -0.00009 0.00053 0.00176 C7 1 0.847497 0.664515 0.414376 11.00000 0.02642 0.01578 = 0.01528 0.00002 0.00128 -0.00168 AFIX 23 H7A 2 0.942944 0.634066 0.447204 11.00000 -1.20000 H7B 2 0.702195 0.684602 0.434381 11.00000 -1.20000 AFIX 0 C8 1 0.975425 0.745551 0.384779 11.00000 0.01704 0.01565 = 0.01422 -0.00096 -0.00019 -0.00093 O9 3 0.703522 0.864511 0.412469 11.00000 0.02301 0.02260 = 0.02474 -0.00286 0.00528 0.00340 O10 3 1.292187 0.692709 0.312704 11.00000 0.01323 0.02481 = 0.02408 -0.00176 0.00072 0.00044 H10 2 1.316192 0.640294 0.329965 11.00000 -1.50000 C11 1 0.885902 0.593880 0.238327 11.00000 0.01662 0.01255 = 0.01520 0.00083 0.00146 0.00240 C12 1 1.069836 0.602365 0.195299 11.00000 0.01653 0.01829 = 0.01884 0.00219 0.00232 0.00201 AFIX 43 H12 2 1.208213 0.630201 0.209163 11.00000 -1.20000 AFIX 0 C13 1 1.052573 0.570725 0.132859 11.00000 0.02446 0.02052 = 0.01749 0.00146 0.00463 0.00716 AFIX 43 H13 2 1.178582 0.577290 0.104423 11.00000 -1.20000 AFIX 0 C14 1 0.852531 0.529625 0.111798 11.00000 0.03171 0.01805 = 0.01464 -0.00196 -0.00273 0.00643 AFIX 43 H14 2 0.841982 0.507120 0.069261 11.00000 -1.20000 AFIX 0 C15 1 0.667448 0.521519 0.153263 11.00000 0.02410 0.01893 = 0.02103 -0.00136 -0.00510 -0.00050 AFIX 43 H15 2 0.529800 0.493555 0.138968 11.00000 -1.20000 AFIX 0 C16 1 0.682877 0.554227 0.215714 11.00000 0.01860 0.01865 = 0.01734 0.00093 -0.00051 -0.00003 AFIX 43 H16 2 0.554070 0.549596 0.243349 11.00000 -1.20000 AFIX 0 C17 1 0.661587 0.518960 0.370520 11.00000 0.01912 0.01493 = 0.01335 0.00195 0.00031 0.00078 C18 1 0.484795 0.520221 0.414445 11.00000 0.02129 0.01362 = 0.01658 -0.00108 0.00124 0.00115 AFIX 43 H18 2 0.454622 0.574810 0.437371 11.00000 -1.20000 AFIX 0 C19 1 0.346857 0.442506 0.426385 11.00000 0.01829 0.01662 = 0.01351 0.00139 -0.00051 0.00127 C20 1 0.164496 0.443547 0.471341 11.00000 0.02139 0.01734 = 0.01838 0.00037 0.00213 0.00290 AFIX 43 H20 2 0.133626 0.497492 0.494938 11.00000 -1.20000 AFIX 0 C21 1 0.032890 0.367866 0.481061 11.00000 0.01934 0.02532 = 0.02180 0.00359 0.00372 0.00016 AFIX 43 H21 2 -0.088583 0.369509 0.511327 11.00000 -1.20000 AFIX 0 C22 1 0.076517 0.287188 0.446336 11.00000 0.02167 0.01979 = 0.02453 0.00396 -0.00050 -0.00521 AFIX 43 H22 2 -0.016728 0.235005 0.453071 11.00000 -1.20000 AFIX 0 C23 1 0.252093 0.283728 0.403094 11.00000 0.02271 0.01593 = 0.02034 0.00006 -0.00225 -0.00020 AFIX 43 H23 2 0.279975 0.228992 0.380116 11.00000 -1.20000 AFIX 0 C24 1 0.393023 0.360729 0.392107 11.00000 0.01961 0.01659 = 0.01491 0.00179 -0.00154 0.00169 C25 1 0.582062 0.359515 0.349273 11.00000 0.02425 0.01571 = 0.01755 -0.00161 0.00159 0.00174 AFIX 43 H25 2 0.618669 0.304763 0.327291 11.00000 -1.20000 AFIX 0 C26 1 0.712134 0.435340 0.339047 11.00000 0.02118 0.01803 = 0.01639 0.00053 0.00385 0.00228 AFIX 43 H26 2 0.838528 0.432293 0.310452 11.00000 -1.20000 AFIX 0 C27 1 1.166842 0.783232 0.426999 11.00000 0.02188 0.02262 = 0.02019 -0.00370 -0.00491 -0.00046 AFIX 137 H27A 2 1.265326 0.733138 0.441324 11.00000 -1.50000 H27B 2 1.099877 0.813705 0.464316 11.00000 -1.50000 H27C 2 1.258196 0.827040 0.402458 11.00000 -1.50000 AFIX 0 HKLF 4 REM REM R1 = 0.0330 for 3629 Fo > 4sig(Fo) and 0.0342 for all 3717 data REM 248 parameters refined using 0 restraints END WGHT 0.0469 0.3118 REM Highest difference peak 0.160, deepest hole -0.208, 1-sigma level 0.049 Q1 1 1.0165 0.7319 0.3534 11.00000 0.05 0.16 Q2 1 0.2291 0.1621 0.3549 11.00000 0.05 0.16 Q3 1 0.7677 0.5588 0.3676 11.00000 0.05 0.16 Q4 1 0.7136 0.4782 0.3620 11.00000 0.05 0.16 Q5 1 0.9840 0.6687 0.3087 11.00000 0.05 0.15 Q6 1 0.2315 0.1426 0.4203 11.00000 0.05 0.14 Q7 1 0.9052 0.5995 0.3335 11.00000 0.05 0.14 Q8 1 0.3643 0.4029 0.4085 11.00000 0.05 0.14 Q9 1 0.5888 0.7284 0.3728 11.00000 0.05 0.14 Q10 1 0.3251 0.3226 0.3998 11.00000 0.05 0.14 Q11 1 0.8951 0.7812 0.3782 11.00000 0.05 0.14 Q12 1 0.6454 0.7828 0.2975 11.00000 0.05 0.13 Q13 1 1.0119 0.7580 0.2959 11.00000 0.05 0.13 Q14 1 0.5846 0.2232 0.3832 11.00000 0.05 0.13 Q15 1 0.4217 0.4804 0.4209 11.00000 0.05 0.12 Q16 1 0.3428 0.5225 0.1468 11.00000 0.05 0.12 Q17 1 0.2618 0.4772 0.1336 11.00000 0.05 0.12 Q18 1 0.6289 0.2374 0.3279 11.00000 0.05 0.12 Q19 1 0.7248 0.2594 0.2908 11.00000 0.05 0.12 Q20 1 0.8839 0.6187 0.2717 11.00000 0.05 0.12 ; _shelx_res_checksum 59778 _shelx_hkl_file ; 0 0 -2 120.355 339.680 14 0 0 -3 1367.47 81.4206 14 0 0 -5-0.37310 65.7357 14 0 0 -6 169212. 3274.99 14 0 0 -7 297.543 83.3459 14 0 0 -8 58769.5 1348.07 14 0 0 -9 121.871 81.7457 14 0 0 -10 283370. 5524.82 14 0 0 -11 140.731 95.2896 14 0 0 -12 8325.76 442.881 14 0 0 -13 138.178 77.6514 14 0 0 -14 23407.4 1029.97 13 0 0 -15-6.54180 159.431 13 0 0 -16 2353.42 343.501 13 0 0 -17 398.604 239.368 8 0 0 -17 85.8208 159.919 13 0 0 -18 142642. 3761.50 13 0 0 -18 147042. 3859.90 8 0 0 -19 206.990 230.771 8 0 0 -20 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2885.30 457.778 12 -3 11 -1 2826.59 531.419 5 -3 11 -1 2681.66 346.995 4 3 11 1 2776.05 417.897 4 3 -11 -1 2640.72 401.021 2 3 11 2 11733.1 876.180 12 3 -11 -2 12880.5 813.297 2 -3 11 -2 12116.5 914.785 5 3 11 2 13291.3 895.519 4 3 -11 -3 7772.80 626.184 2 -3 11 -3 7171.73 754.429 5 3 11 3 6819.92 626.492 4 3 11 3 7473.40 707.907 12 -3 11 -4 38005.7 1699.43 5 3 11 4 38222.9 1545.71 4 3 -11 -4 37182.3 1478.00 2 3 -11 -5 13061.6 802.987 2 3 11 5 14148.7 953.030 12 -3 11 -5 12319.3 945.977 5 3 11 5 12257.7 788.416 4 3 11 6 2467.03 446.052 12 -3 11 -6 3063.00 494.067 5 3 -11 -6 3328.26 426.548 2 3 11 7 3504.75 477.804 12 -3 11 -7 3837.78 560.335 5 3 -11 -7 4344.03 469.174 2 3 11 8 33445.0 1527.89 12 3 11 8 31069.0 1449.76 10 -3 11 -8 31225.7 1516.09 5 3 -11 -8 32526.0 1302.41 2 3 11 9 12196.7 894.161 12 3 11 9 10950.7 824.429 10 -3 11 -9 11688.3 920.144 5 3 -11 -9 11595.8 727.859 2 3 11 10 5378.82 600.134 12 3 11 10 5464.85 581.549 10 -3 11 -10 6299.06 660.893 5 3 -11 -10 6577.82 541.987 2 3 11 11 9414.50 761.504 12 3 11 11 10672.4 792.616 10 -3 11 -11 9981.20 816.223 5 3 -11 -11 11781.0 707.920 2 3 11 12 348.456 202.246 12 3 11 12 755.107 228.657 10 -3 11 -12 479.025 282.732 5 3 -11 -12 924.089 264.045 2 3 11 13 32835.6 1337.91 12 3 11 13 32056.9 1340.93 10 -3 11 -13 32139.4 1398.11 5 3 -11 -13 32533.1 1183.05 2 3 11 14 20698.1 942.992 12 3 11 14 20004.7 966.107 10 -3 11 -14 18486.5 991.329 5 3 -11 -14 19971.9 847.815 2 3 11 15 4756.73 389.206 12 3 11 15 4762.56 415.330 10 -3 11 -15 3659.75 423.288 5 3 -11 -15 4867.75 386.499 2 -3 11 -16 12039.3 661.883 5 3 -11 -16 12599.3 581.867 2 3 -11 -17 6457.06 365.714 2 -3 11 -17 5730.91 404.909 5 -3 11 -18 23259.7 763.359 5 -3 12 16 10457.9 438.890 4 3 12 -16 10712.3 517.698 7 -3 12 15 18229.2 618.041 6 -3 12 15 18881.2 719.264 4 3 12 -15 18577.2 785.273 7 -3 12 14 254.201 118.592 6 -3 12 14 148.037 146.350 4 3 -12 14 122.761 89.7890 2 3 12 -14 139.407 157.459 7 3 12 -13 6309.44 510.646 7 -3 12 13 6765.01 429.812 6 3 12 -12 8295.71 604.910 7 3 12 -11 6584.86 555.468 7 3 12 -10 1282.61 310.982 12 3 12 -10 761.061 238.615 7 3 12 -9 12200.5 780.552 12 3 12 -9 11171.9 779.296 7 3 12 -8 4464.53 508.823 12 3 12 -8 4392.16 497.786 7 3 12 -7 758.566 266.636 7 3 12 -7 500.841 289.721 12 3 -12 7 481.057 194.998 2 3 12 -6 14414.9 919.521 12 3 -12 6 14007.1 854.713 2 3 12 -6 13937.4 858.959 7 3 -12 5 23800.4 1155.17 2 3 12 -5 24603.6 1165.64 7 3 12 -5 26484.0 1277.60 12 3 12 -4 50145.6 1854.14 12 3 -12 4 47517.9 1731.74 2 3 12 -3 9025.05 752.478 12 3 -12 3 8503.58 661.917 2 3 12 -2 1279.57 358.577 12 3 -12 2 1277.62 312.313 2 -3 12 2 1622.11 328.628 4 3 12 -1 47569.7 1821.76 12 3 -12 1 42855.2 1602.64 2 3 12 -1 45233.9 1752.84 4 -3 12 1 40265.7 1538.95 4 3 12 0 190.232 343.519 12 3 12 0-103.666 226.332 4 -3 12 0 85.7195 137.399 4 3 12 1 44875.9 1771.32 12 3 -12 -1 43876.6 1598.96 2 -3 12 -1 45070.1 1824.77 5 3 12 1 43993.5 1737.16 4 -3 12 -1 40765.9 1476.90 4 3 12 2 1286.01 362.020 12 -3 12 -2 1844.46 503.498 5 3 12 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3697.66 398.278 2 3 13 -6 3403.45 399.827 7 -3 13 6 3447.98 434.831 4 3 -13 5 6292.61 513.161 2 3 13 -5 6653.49 614.283 12 -3 13 5 5824.73 531.730 4 3 13 -4 4976.83 564.147 12 3 -13 4 5282.52 469.140 2 -3 13 4 4968.82 487.098 4 3 13 -3 1876.09 372.795 12 3 -13 3 1604.96 287.396 2 -3 13 3 2084.67 321.228 4 3 13 -2 872.518 307.988 12 -3 13 2 377.267 181.526 4 3 -13 2 606.236 228.701 2 3 -13 1 703.588 251.214 2 -3 13 1 1169.96 247.275 4 3 -13 0 1307.25 283.288 2 -3 13 0 1890.98 291.421 4 3 13 0 1789.74 391.276 12 3 13 1 488.346 301.191 12 3 -13 -1 431.140 207.350 2 -3 13 -1 314.705 159.875 4 3 13 2 198.284 233.178 12 3 -13 -2 469.247 205.671 2 3 13 3 2124.58 412.313 12 -3 13 -3 1605.24 394.131 5 3 -13 -3 1689.72 280.547 2 3 13 4 4961.73 574.842 12 -3 13 -4 4366.69 558.254 5 3 -13 -4 4466.42 432.632 2 3 13 5 6111.80 608.756 12 -3 13 -5 5909.42 644.621 5 3 -13 -5 5719.49 484.811 2 3 13 6 3186.42 459.843 12 -3 13 -6 4337.32 559.335 5 3 -13 -6 3717.17 381.909 2 3 13 7 31382.2 1386.83 12 -3 13 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1041.20 11 -6 -3 -7 24281.9 1009.01 1 6 -3 7 25339.5 1190.05 3 6 3 -6 18030.9 854.234 11 6 -3 6 15885.4 732.518 11 6 -3 6 18288.3 997.352 3 6 3 -5 1176.24 292.400 11 6 -3 5 1357.51 226.236 11 -6 -3 -5 1893.72 272.672 1 6 -3 5 1817.34 398.670 3 -6 -3 -4 7260.75 478.886 1 6 3 -4 7223.81 572.203 11 6 -3 4 6955.72 494.758 11 6 -3 4 8507.12 701.248 3 6 3 -3 9432.97 657.846 11 6 -3 3 8129.12 547.435 11 6 -3 2 36296.5 1289.73 11 6 3 -2 39136.2 1437.27 11 -6 3 1 23560.8 962.737 1 6 -3 1 23700.7 1006.83 11 6 3 -1 24028.2 1103.99 11 -6 3 0 4016.44 400.956 1 6 -3 0 4336.09 420.717 11 6 3 0 4208.79 509.009 11 6 -3 -1 24752.9 1012.97 11 6 3 1 22639.4 1105.01 11 -6 3 -1 23557.2 1010.48 1 6 -3 -2 38746.0 1339.37 11 -6 3 -2 36489.7 1344.50 1 6 -3 -3 8293.03 581.839 11 -6 3 -3 8098.57 581.412 1 6 -3 -4 6476.48 512.481 11 -6 3 -4 7453.61 579.310 1 -6 3 -5 1091.35 266.050 1 6 -3 -5 1330.14 254.955 11 6 -3 -6 15893.2 790.669 11 -6 3 -6 15636.2 846.053 1 6 -3 -7 25575.5 1016.51 11 -6 3 -7 26115.1 1108.95 1 6 -3 -8 3763.09 384.931 11 -6 3 -8 4255.10 449.508 1 6 -3 -9 1820.34 272.418 11 -6 3 -9 1735.09 293.632 1 -6 3 -10 4571.45 416.153 1 -6 3 -11 9392.56 550.575 1 -6 3 -12 13743.7 628.337 1 -6 3 -13 51.0541 106.049 1 -6 3 -14 4105.76 258.780 1 -6 -4 -14 2880.27 206.345 1 -6 -4 -13 10417.6 469.712 1 6 -4 13 10443.2 498.613 3 -6 -4 -12 12846.8 576.953 1 6 -4 12 12459.9 617.950 3 6 -4 11 18694.7 846.147 3 -6 -4 -11 18728.4 750.800 1 -6 -4 -10 3904.88 345.818 1 6 4 -10 3924.73 324.504 11 6 -4 10 4096.21 417.074 3 -6 -4 -9 13045.5 669.735 1 6 4 -9 14552.6 672.380 11 6 -4 9 15421.6 839.744 3 6 -4 8 1158.27 317.495 3 6 4 -8 1155.09 220.596 11 -6 -4 -8 1265.55 224.893 1 6 -4 8 891.211 205.610 2 6 4 -7 5074.50 420.813 11 6 -4 7 4818.15 403.821 2 -6 -4 -7 3921.24 360.048 1 6 -4 7 5203.19 533.323 3 6 4 -6 6561.41 499.689 11 6 -4 6 5763.72 456.874 2 -6 -4 -6 5437.73 406.643 1 6 -4 6 6096.61 578.217 3 6 4 -5 39868.6 1361.70 11 6 -4 5 36937.5 1300.73 2 6 -4 5 36864.2 1505.10 3 6 4 -4 18833.6 879.311 11 6 -4 4 16981.0 827.684 2 6 -4 4 18547.5 1082.80 3 6 -4 3 19015.3 880.592 2 6 -4 3 20049.3 817.915 11 6 4 -3 20203.8 966.902 11 6 -4 2 59980.8 1764.60 2 6 -4 2 58886.0 1700.30 11 6 4 -2 61394.3 1888.82 11 -6 4 2 60838.0 1719.02 1 -6 4 1 22811.3 975.670 1 6 -4 1 24622.9 968.500 11 6 4 -1 24361.5 1128.48 11 6 -4 0 87940.6 2264.65 2 -6 4 0 85044.3 2298.72 1 6 -4 0 84963.4 2237.31 11 6 4 0 89512.7 2453.03 11 -6 4 -1 23951.1 1019.78 1 6 -4 -1 24115.5 979.520 11 6 4 1 23584.6 1113.84 11 6 -4 -2 57147.4 1707.50 11 -6 4 -2 59971.2 1808.36 1 6 4 2 58660.5 1898.30 11 6 -4 -3 19256.6 861.609 11 -6 4 -3 19262.8 925.340 1 6 -4 -4 16675.6 780.863 11 -6 4 -4 15906.5 837.099 1 6 -4 -5 34943.2 1222.78 11 -6 4 -5 36363.8 1348.25 1 6 -4 -6 5803.61 452.819 11 -6 4 -6 5421.66 487.719 1 6 -4 -7 4306.14 381.001 11 -6 4 -7 4373.57 433.181 1 -6 4 -8 680.545 229.256 1 6 -4 -8 1134.89 223.797 11 -6 4 -9 13941.3 732.616 1 -6 4 -10 5074.17 414.722 1 -6 4 -11 17958.0 751.528 1 -6 4 -12 13110.3 580.549 1 -6 4 -13 9548.86 436.589 1 -6 -5 -13 13993.0 506.835 1 6 -5 13 14703.0 562.254 3 -6 -5 -12 31043.0 917.204 1 6 -5 12 32668.6 1037.74 3 6 -5 11 859.596 210.488 3 -6 -5 -11 666.943 139.153 1 -6 -5 -10 2224.53 237.773 1 6 -5 10 1708.08 274.728 3 6 -5 10 1757.16 221.901 2 6 -5 9 1415.96 283.952 3 -6 -5 -9 1217.71 184.645 1 6 5 -9 1666.18 205.128 11 6 -5 9 1240.18 208.388 2 6 5 -8 8617.19 489.477 11 6 -5 8 7912.73 512.107 2 -6 -5 -8 7865.64 459.672 1 6 -5 8 9116.97 644.551 3 -6 -5 -7 613.303 145.833 1 6 -5 7 1060.67 294.964 3 6 5 -7 948.907 201.301 11 6 -5 7 755.253 196.854 2 6 5 -6 19546.1 834.927 11 6 -5 6 19043.0 862.904 2 6 -5 6 20462.2 1015.64 3 6 5 -5 4694.02 409.664 11 6 -5 5 3884.68 400.359 2 6 -5 5 3817.48 477.739 3 6 5 -4 5272.17 456.660 11 6 -5 4 4874.67 434.362 2 6 -5 4 6030.62 576.408 3 6 -5 3 13041.1 717.363 2 6 5 -3 14757.8 750.034 11 6 -5 2 24942.7 1020.58 2 6 5 -2 22902.2 1003.06 11 6 5 -1 12692.0 731.473 11 -6 5 1 11495.4 648.859 1 -6 5 0 6007.86 467.466 1 6 -5 0 5156.72 430.191 2 6 5 0 5484.38 499.448 11 6 -5 -1 12636.1 679.817 2 -6 5 -1 11174.7 653.735 1 6 -5 -1 11917.1 595.297 11 6 5 1 12181.0 750.127 11 6 -5 -2 22976.4 924.512 2 -6 5 -2 21582.2 962.956 1 6 -5 -2 23153.1 882.522 11 6 5 2 23451.4 1061.22 11 6 -5 -3 14084.8 669.007 11 -6 5 -3 14422.0 760.198 1 6 -5 -3 14215.9 691.419 2 6 -5 -4 4244.64 361.022 11 -6 5 -4 5254.73 465.392 1 6 -5 -4 5214.22 397.088 2 6 -5 -5 4041.32 346.307 11 -6 5 -5 4281.26 427.757 1 6 -5 -5 4321.96 347.986 2 6 -5 -6 18601.7 773.914 11 -6 5 -6 18843.2 889.854 1 6 -5 -7 734.542 172.228 11 -6 5 -7 905.205 244.467 1 -6 5 -8 8320.20 545.270 1 -6 5 -9 1268.52 225.367 1 -6 5 -10 2451.20 280.513 1 -6 5 -11 532.207 147.521 1 -6 5 -12 32468.8 949.182 1 -6 5 -13 13559.5 482.482 1 6 -6 12 4111.71 292.561 3 6 -6 11 19171.7 666.769 2 -6 -6 -11 17862.8 599.719 1 6 -6 11 20150.3 770.059 3 6 -6 10 839.925 201.915 3 -6 -6 -10 833.505 134.487 1 6 -6 10 745.643 156.495 2 6 -6 9 16443.6 716.566 2 -6 -6 -9 15814.5 589.917 1 6 -6 8 2716.29 297.153 2 -6 -6 -8 2566.87 218.584 1 6 -6 8 3340.08 380.791 3 6 -6 7 364.857 229.876 3 6 6 -7 429.307 134.744 11 6 -6 7 340.813 159.682 2 6 6 -6 4318.34 341.765 11 6 -6 6 3981.25 378.316 2 6 -6 6 3970.88 438.419 3 6 6 -5 11132.5 576.583 11 6 -6 5 10020.8 604.044 2 6 -6 5 11596.8 718.494 3 6 -6 4 11140.5 640.752 2 6 6 -4 12583.8 628.238 11 6 6 -3 2038.07 272.520 11 6 -6 3 1878.99 294.873 2 6 6 -2 2095.11 292.615 11 6 -6 2 1685.89 307.961 2 6 -6 1 6921.10 505.789 2 6 6 -1 7944.05 526.132 11 6 -6 0 11668.8 658.475 2 6 6 0 11730.4 664.278 11 -6 6 0 10842.2 625.964 1 -6 6 -1 7260.73 507.215 1 6 -6 -1 6450.42 515.650 2 6 6 1 6687.44 515.421 11 6 6 2 1333.86 253.405 11 -6 6 -2 1596.65 276.200 1 6 -6 -2 1593.71 240.810 2 6 6 3 1924.65 321.005 11 -6 6 -3 2009.97 304.877 1 6 -6 -3 2276.29 276.382 2 -6 6 -4 11788.0 655.588 1 6 -6 -4 11413.7 599.436 2 -6 6 -5 10108.2 611.132 1 6 -6 -5 10028.1 540.900 2 -6 6 -6 3841.03 374.200 1 6 -6 -6 4119.68 332.157 2 -6 6 -7 179.165 172.405 1 -6 6 -8 3160.20 324.052 1 -6 6 -9 16406.8 708.407 1 -6 6 -10 1012.71 188.849 1 -6 6 -11 18611.1 664.777 1 -6 6 -12 3983.01 243.853 1 6 -7 10 1196.15 162.489 2 6 -7 10 1288.06 199.679 3 6 -7 9 106.714 103.555 2 6 -7 9 87.6130 141.205 3 6 -7 8 33413.1 1091.84 2 6 -7 8 35972.3 1193.25 3 6 -7 7 762.453 176.190 2 6 -7 7 347.440 179.174 3 6 -7 6 6238.18 434.844 2 6 -7 5 2878.00 318.147 2 6 -7 4 12633.0 656.289 2 6 7 -4 12454.0 564.422 11 6 -7 3 3673.11 417.793 2 6 7 -3 3468.78 301.264 11 6 -7 2 12776.9 680.443 2 6 7 -2 12856.3 628.479 11 6 -7 1 6929.59 570.631 2 6 7 -1 5848.36 422.398 11 6 -7 0 11307.1 624.358 2 6 7 0 11773.3 605.995 11 6 -7 -1 7394.60 540.082 2 6 7 1 4752.16 405.753 11 6 7 2 13837.9 682.774 11 -6 7 -2 12595.9 655.836 1 6 -7 -2 12086.3 625.083 2 6 7 3 3511.88 358.697 11 6 -7 -3 4219.15 361.594 2 -6 7 -3 3576.28 349.386 1 -6 7 -4 12328.7 649.749 1 6 7 4 12440.6 662.218 11 6 -7 -4 12559.5 607.814 2 6 7 5 3138.17 338.614 11 -6 7 -5 3036.88 324.012 1 6 -7 -5 2952.26 284.650 2 -6 7 -6 5904.95 435.311 1 6 -7 -6 6300.41 394.644 2 -6 7 -7 86.7099 153.161 1 6 -7 -7 591.218 133.550 2 -6 7 -8 33377.0 1057.91 1 -6 7 -9 167.550 118.405 1 -6 7 -10 1258.10 170.376 1 -6 7 -11 27340.1 773.116 1 6 -8 9 9580.08 434.822 2 6 -8 8 9661.51 473.813 2 6 -8 7 3432.40 292.003 2 6 -8 6 1334.52 206.980 2 6 -8 5 8513.02 490.010 2 6 -8 4 20955.8 836.795 2 6 -8 3 2476.27 313.195 2 6 -8 2 10435.0 702.232 2 6 -8 1 45568.5 1371.60 2 6 -8 0 20230.4 832.281 2 6 -8 -1 50004.2 1409.95 2 6 8 1 44483.3 1276.66 11 6 8 2 3694.63 310.749 11 6 -8 -2 4333.40 351.848 2 6 8 3 1157.39 187.288 11 6 -8 -3 1570.56 221.635 2 6 8 4 19884.0 777.299 11 6 -8 -4 20312.5 762.886 2 6 8 5 7789.54 451.940 11 6 -8 -5 8447.59 445.183 2 6 8 6 1762.23 214.091 11 6 -8 -6 1606.73 197.392 2 6 8 7 3781.30 298.328 11 6 -8 -7 3836.32 272.131 2 6 8 8 8659.02 437.986 11 6 -8 -8 8913.60 386.670 2 6 8 9 9453.11 431.982 11 6 -9 7 11587.5 490.222 2 6 -9 6 10149.1 483.511 2 6 -9 5 25090.8 844.004 2 6 -9 4 35300.0 1080.56 2 6 -9 3 14760.7 640.263 2 6 -9 2 10722.7 581.962 2 6 -9 1 13943.8 634.724 2 6 -9 0 2624.84 460.108 2 6 -9 -1 11555.3 549.551 2 6 -9 -2 9290.08 491.371 2 6 -9 -3 14469.6 604.989 2 6 -9 -4 35239.7 1026.43 2 6 -9 -5 26003.3 814.074 2 6 -9 -6 10894.9 455.026 2 6 -9 -7 11633.6 439.045 2 6 -10 5 8899.67 393.204 2 6 -10 4 31679.9 901.422 2 6 -10 3 39154.5 1079.91 2 6 -10 2 7790.15 417.441 2 6 -10 1 15373.0 598.430 2 6 -10 0 10745.7 508.058 2 6 -10 -1 14241.3 559.400 2 6 -10 -2 9544.40 474.019 2 6 -10 -3 38977.9 1042.59 2 6 -10 -4 30276.7 849.134 2 7 0 0 20.2976 107.472 11 7 0 -1 114.751 105.452 11 7 0 1 438.202 132.453 11 7 0 -2 3212.32 285.775 11 7 0 2 3239.52 290.442 11 7 0 -3-175.869 149.328 11 7 0 3 293.389 124.714 11 7 0 -4 10629.6 493.998 11 7 0 4 9891.17 477.007 11 7 0 -5 4329.08 306.195 11 7 0 5 4701.87 305.154 11 7 0 -6 104076. 2219.86 11 7 0 6 95305.5 2126.47 11 7 0 -7 5494.72 308.632 11 7 1 -7 10963.5 455.602 11 7 1 -6 7004.21 378.905 11 7 1 -5 28349.6 869.468 11 7 -1 5 26298.7 766.802 11 7 1 -4 23902.0 806.772 11 7 -1 4 22198.5 726.837 11 7 1 -3 8617.32 455.909 11 7 -1 3 8156.19 417.273 11 7 1 -2 3540.41 305.153 11 7 -1 2 4195.98 296.005 11 7 -1 1 4909.55 339.443 11 7 1 -1 5149.94 368.411 11 7 -1 0 3514.85 291.225 11 7 1 0 3712.53 317.376 11 7 -1 -1 5144.53 349.552 11 7 1 1 5393.41 379.083 11 7 -1 -2 3815.40 304.530 11 7 1 2 3627.52 316.474 11 7 -1 -3 7456.86 422.113 11 7 1 3 8500.11 457.080 11 7 -1 -4 23373.6 787.658 11 7 1 4 24079.4 822.091 11 7 -1 -5 27151.7 855.801 11 7 1 5 27766.1 868.232 11 7 -1 -6 7879.77 389.308 11 7 1 6 7567.36 378.119 11 7 -1 -7 11747.2 458.335 11 7 2 -7 15147.3 533.989 11 7 2 -6 10885.3 464.663 11 7 2 -5 135.790 110.387 11 7 2 -4 13294.6 563.878 11 7 2 -3 16352.7 660.770 11 7 -2 3 15885.0 545.918 11 7 -2 2 6713.10 348.302 11 7 2 -2 6731.07 413.011 11 7 -2 1 6608.08 367.757 11 7 2 -1 7612.27 437.345 11 7 -2 0 10588.7 476.659 11 7 2 0 11612.1 549.838 11 7 -2 -1 6599.13 368.113 11 7 2 1 7350.59 432.972 11 7 -2 -2 6280.89 359.241 11 7 2 2 6928.55 421.063 11 7 -2 -3 15475.6 597.692 11 7 2 3 16983.7 673.312 11 7 -2 -4 12706.4 513.392 11 7 2 4 13192.0 575.965 11 7 -2 -5 238.071 89.8056 11 7 2 5 351.217 124.940 11 7 -2 -6 11023.2 441.282 11 7 2 6 11721.5 491.509 11 7 2 7 15380.0 540.536 11 7 3 -6 28882.8 820.184 11 7 3 -5 2906.21 233.633 11 7 3 -4 582.376 124.604 11 7 3 -3 15393.4 603.667 11 7 3 -2 20432.6 740.240 11 7 3 -1 5797.18 379.428 11 7 3 0 11566.5 534.520 11 7 -3 -1 5104.63 278.044 11 7 3 1 6282.92 390.851 11 7 -3 -2 17997.0 597.112 11 7 3 2 21097.5 744.050 11 7 -3 -3 13171.5 487.205 11 7 3 3 15538.6 620.995 11 7 -3 -4 353.727 80.0564 11 7 3 4 792.561 156.963 11 7 3 5 3483.33 270.718 11 7 3 6 30406.9 885.580 11 7 4 -4 7879.78 367.133 11 7 4 -3 13891.9 534.439 11 7 4 -2 3348.27 260.766 11 7 4 -1 9259.76 443.216 11 7 4 0 26304.3 842.055 11 7 4 1 9796.59 469.623 11 7 4 2 3435.20 274.847 11 7 4 3 14319.0 567.448 11 7 4 4 7993.59 399.977 11 7 4 5 2582.49 210.903 11 7 5 -1 4178.85 255.832 11 7 5 0 15621.5 550.956 11 7 5 1 4150.43 266.326 11 7 5 2 413.863 103.950 11 7 5 3 2504.36 199.338 11 0 0 0 0.00 0.00 0 TITL CCHWLC in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 1.54184 5.833721 14.679818 20.889359 90.0000 90.0000 90.0000 ZERR 4.00 0.000388 0.001003 0.001537 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H O UNIT 100.00 88.00 8.00 TREF HKLF 4 END ; _shelx_hkl_checksum 95384 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 0 -1 0.0954 0.0001 -0.0005 -0.9994 0.0101 -0.0644 0.0344 0 0 1 0.0954 -0.0001 0.0005 0.9994 -0.0101 0.0644 -0.0344 0 -2 -5 0.1673 0.0014 -2.0015 -4.9965 -0.0317 -0.4227 0.0076 0 2 5 0.1673 -0.0014 2.0015 4.9965 0.0317 0.4227 -0.0076 -1 0 0 0.2583 -0.9991 0.0006 0.0014 0.2401 -0.0196 -0.1077 3 -5 -3 0.2396 3.0002 -5.0004 -3.0014 -0.8957 -0.3862 0.0153 0 1 -5 0.1206 -0.0001 0.9968 -4.9971 0.0919 -0.2716 0.2543 0 4 -5 0.1913 -0.0016 3.9952 -4.9977 0.2155 -0.1205 0.5010 0 -4 5 0.1913 0.0016 -3.9952 4.9977 -0.2155 0.1205 -0.5010 -2 1 -5 0.2306 -1.9984 0.9979 -4.9942 0.5720 -0.3109 0.0388 2 -2 5 0.2506 1.9989 -1.9974 4.9944 -0.6132 0.2605 -0.1210 2 1 2 0.3379 1.9976 0.9994 1.9957 -0.4592 0.2184 0.2289 3 5 -2 0.3588 2.9950 4.9945 -2.0041 -0.4939 0.1819 0.8032 0 -1 0 0.2370 0.0005 -0.9994 0.0002 -0.0412 -0.0504 -0.0822 1 -5 -5 0.1822 1.0021 -5.0004 -4.9973 -0.3953 -0.5542 -0.1314 0 5 1 0.2492 -0.0026 4.9977 0.9983 0.1958 0.3163 0.3768 1 3 -5 0.2926 0.9980 2.9952 -4.9989 -0.0658 -0.1513 0.5265 1 0 -5 0.2624 0.9995 -0.0032 -4.9983 -0.1893 -0.3024 0.2798 _olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount' _olex2_submission_special_instructions 'No special instructions were received'