data_su1427 _publ_section_title SU1427/PO60837766 _publ_contact_author_name 'Cyril Bucher' _publ_contact_author_address 'Department of Chemistry, Stanford University' _publ_contact_author_email cbucher@stanford.edu _publ_contact_author_phone ? _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H16 Br2 Cl2 O2' _chemical_formula_sum 'C9 H16 Br2 Cl2 O2' _chemical_formula_weight 386.94 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.6424(10) _cell_length_b 7.2529(7) _cell_length_c 10.6701(10) _cell_angle_alpha 90 _cell_angle_beta 106.601(3) _cell_angle_gamma 90 _cell_volume 715.11(12) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6057 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 28.25 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.797 _exptl_crystal_F_000 380 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 6.023 _shelx_estimated_absorpt_T_min 0.410 _shelx_estimated_absorpt_T_max 0.753 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4473 _exptl_absorpt_correction_T_max 0.8643 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2014)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa X8-APEX-II' _diffrn_measurement_method 'combination of \w and \f-scans ' _diffrn_detector_area_resol_mean 8.33 _diffrn_reflns_number 12787 _diffrn_reflns_av_unetI/netI 0.0409 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.992 _diffrn_reflns_theta_max 28.500 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_point_group_measured_fraction_full 0.988 _reflns_number_total 3545 _reflns_number_gt 3273 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.815 _reflns_Friedel_fraction_max 0.950 _reflns_Friedel_fraction_full 0.974 _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. Hydroxyl hydrogen atoms were located from a difference Fourier map and subsequently refined as a riding model on the hydroxyl oxygen atom. ; _computing_data_collection 'Bruker APEX-II v2014-5.0' _computing_cell_refinement 'Bruker SAINT v8.34A' _computing_data_reduction 'Bruker SAINT v8.34A' _computing_structure_solution 'SHELXT-2014/2 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'Bruker XP' _computing_publication_material 'CIFTAB (Sheldrick, 2008)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0610P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary vecmap _atom_sites_solution_secondary dismap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 1368 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.019(5) _chemical_absolute_configuration rmad _refine_ls_number_reflns 3545 _refine_ls_number_parameters 139 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 Br1 Br 0.72502(6) 0.16104(9) 0.30913(6) 0.02719(16) Uani 1 1 d . . . . . Br2 Br 0.59483(8) 0.33344(9) 0.66664(6) 0.0396(2) Uani 1 1 d . . . . . Cl1 Cl 0.73926(17) 0.7212(2) 0.13853(13) 0.0301(3) Uani 1 1 d . . . . . Cl2 Cl 0.83361(16) 0.8385(2) 0.62188(12) 0.0291(3) Uani 1 1 d . . . . . O1 O 0.8889(4) 0.3927(6) 0.0677(4) 0.0246(9) Uani 1 1 d . . . . . H1O H 0.9061 0.4699 0.0154 0.037 Uiso 1 1 calc R U . . . O2 O 0.9099(4) 0.6273(6) 0.8815(3) 0.0249(9) Uani 1 1 d . . . . . H2O H 0.9665 0.7179 0.8975 0.037 Uiso 1 1 calc R U . . . C1 C 0.7392(6) 0.3794(9) 0.0474(5) 0.0263(12) Uani 1 1 d . . . . . H1A H 0.7124 0.2477 0.0485 0.032 Uiso 1 1 calc R U . . . H1B H 0.6890 0.4294 -0.0401 0.032 Uiso 1 1 calc R U . . . C2 C 0.6876(6) 0.4826(8) 0.1500(5) 0.0213(11) Uani 1 1 d . . . . . C3 C 0.7646(6) 0.4246(8) 0.2875(5) 0.0192(10) Uani 1 1 d . . . . . H3 H 0.8710 0.4382 0.3001 0.023 Uiso 1 1 calc R U . . . C4 C 0.7276(6) 0.5284(8) 0.3978(5) 0.0208(11) Uani 1 1 d . . . . . H4A H 0.7270 0.6624 0.3803 0.025 Uiso 1 1 calc R U . . . H4B H 0.6294 0.4927 0.4003 0.025 Uiso 1 1 calc R U . . . C5 C 0.8345(5) 0.4884(9) 0.5291(5) 0.0206(11) Uani 1 1 d . . . . . H5A H 0.9329 0.5184 0.5238 0.025 Uiso 1 1 calc R U . . . H5B H 0.8321 0.3546 0.5466 0.025 Uiso 1 1 calc R U . . . C6 C 0.8088(6) 0.5933(8) 0.6452(5) 0.0191(10) Uani 1 1 d . . . . . C7 C 0.9230(6) 0.5350(8) 0.7693(5) 0.0214(11) Uani 1 1 d . . . . . H7A H 0.9151 0.4006 0.7816 0.026 Uiso 1 1 calc R U . . . H7B H 1.0201 0.5599 0.7589 0.026 Uiso 1 1 calc R U . . . C8 C 0.5230(6) 0.4750(11) 0.1157(6) 0.0337(15) Uani 1 1 d . . . . . H8A H 0.4812 0.5065 0.0233 0.051 Uiso 1 1 calc R U . . . H8B H 0.4892 0.5632 0.1701 0.051 Uiso 1 1 calc R U . . . H8C H 0.4927 0.3503 0.1317 0.051 Uiso 1 1 calc R U . . . C9 C 0.6576(6) 0.5859(9) 0.6565(5) 0.0257(12) Uani 1 1 d . . . . . H9A H 0.5912 0.6472 0.5797 0.031 Uiso 1 1 calc R U . . . H9B H 0.6532 0.6538 0.7358 0.031 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0350(3) 0.0206(3) 0.0315(3) 0.0011(2) 0.0183(2) -0.0003(2) Br2 0.0467(4) 0.0477(4) 0.0252(3) -0.0035(3) 0.0114(2) -0.0269(3) Cl1 0.0465(9) 0.0202(7) 0.0207(6) 0.0023(5) 0.0049(6) 0.0041(6) Cl2 0.0380(8) 0.0262(7) 0.0211(6) 0.0022(5) 0.0050(5) -0.0074(6) O1 0.035(2) 0.024(2) 0.0181(18) 0.0056(16) 0.0138(16) 0.0089(17) O2 0.033(2) 0.031(3) 0.0104(15) -0.0010(15) 0.0049(14) -0.0091(17) C1 0.035(3) 0.030(3) 0.014(2) -0.006(2) 0.008(2) -0.003(2) C2 0.027(3) 0.022(3) 0.013(2) 0.001(2) 0.003(2) 0.001(2) C3 0.022(3) 0.019(3) 0.017(2) 0.0011(19) 0.0063(19) -0.001(2) C4 0.020(3) 0.028(3) 0.013(2) 0.000(2) 0.0026(18) 0.007(2) C5 0.017(2) 0.031(3) 0.016(2) 0.000(2) 0.0065(19) 0.006(2) C6 0.019(3) 0.024(3) 0.016(2) -0.0004(19) 0.0068(19) -0.002(2) C7 0.025(3) 0.021(3) 0.016(2) 0.002(2) 0.0037(19) -0.001(2) C8 0.024(3) 0.046(4) 0.025(3) -0.010(3) -0.003(2) 0.006(3) C9 0.029(3) 0.038(3) 0.012(2) -0.002(2) 0.007(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C3 1.976(6) . ? Br2 C9 1.942(7) . ? Cl1 C2 1.815(6) . ? Cl2 C6 1.821(6) . ? O1 C1 1.400(7) . ? O2 C7 1.409(6) . ? C1 C2 1.523(8) . ? C2 C3 1.503(7) . ? C2 C8 1.525(8) . ? C3 C4 1.522(7) . ? C4 C5 1.511(6) . ? C5 C6 1.533(7) . ? C6 C9 1.497(8) . ? C6 C7 1.520(7) . ? O1 H1O 0.8400 . ? O2 H2O 0.8400 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 H3 1.0000 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? 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 O1 C1 C2 112.9(4) . . ? C3 C2 C1 113.1(5) . . ? C3 C2 C8 114.5(5) . . ? C1 C2 C8 109.9(4) . . ? C3 C2 Cl1 105.3(4) . . ? C1 C2 Cl1 105.5(4) . . ? C8 C2 Cl1 107.8(4) . . ? C2 C3 C4 117.2(5) . . ? C2 C3 Br1 109.0(4) . . ? C4 C3 Br1 107.0(4) . . ? C5 C4 C3 111.9(4) . . ? C4 C5 C6 115.4(4) . . ? C9 C6 C7 113.6(4) . . ? C9 C6 C5 115.7(4) . . ? C7 C6 C5 108.7(4) . . ? C9 C6 Cl2 102.4(4) . . ? C7 C6 Cl2 107.4(4) . . ? C5 C6 Cl2 108.4(4) . . ? O2 C7 C6 112.9(5) . . ? C6 C9 Br2 111.4(4) . . ? C1 O1 H1O 109.5 . . ? C7 O2 H2O 109.5 . . ? O1 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? O1 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C2 C3 H3 107.8 . . ? C4 C3 H3 107.8 . . ? Br1 C3 H3 107.8 . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 C5 H5A 108.4 . . ? C6 C5 H5A 108.4 . . ? C4 C5 H5B 108.4 . . ? C6 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? O2 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? O2 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.4 . . ? Br2 C9 H9A 109.4 . . ? C6 C9 H9B 109.4 . . ? Br2 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? 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 O1 C1 C2 C3 -55.1(7) . . . . ? O1 C1 C2 C8 175.5(5) . . . . ? O1 C1 C2 Cl1 59.5(5) . . . . ? C1 C2 C3 C4 176.2(5) . . . . ? C8 C2 C3 C4 -56.8(7) . . . . ? Cl1 C2 C3 C4 61.4(6) . . . . ? C1 C2 C3 Br1 -62.1(5) . . . . ? C8 C2 C3 Br1 64.9(6) . . . . ? Cl1 C2 C3 Br1 -176.9(3) . . . . ? C2 C3 C4 C5 -167.0(5) . . . . ? Br1 C3 C4 C5 70.3(5) . . . . ? C3 C4 C5 C6 177.7(5) . . . . ? C4 C5 C6 C9 49.7(7) . . . . ? C4 C5 C6 C7 178.9(5) . . . . ? C4 C5 C6 Cl2 -64.6(5) . . . . ? C9 C6 C7 O2 -50.8(6) . . . . ? C5 C6 C7 O2 178.8(5) . . . . ? Cl2 C6 C7 O2 61.7(5) . . . . ? C7 C6 C9 Br2 -69.7(5) . . . . ? C5 C6 C9 Br2 57.1(5) . . . . ? Cl2 C6 C9 Br2 174.8(2) . . . . ? 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 O1 H1O O2 0.84 1.84 2.667(6) 169.3 1_554 O2 H2O O1 0.84 1.84 2.676(6) 171.8 2_756 _refine_diff_density_max 1.564 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.115 _shelx_res_file ; su1427.res created by SHELXL-2014/7 TITL su1427 in P2(1) CELL 0.71073 9.64240 7.25290 10.67010 90.0000 106.6008 90.0000 ZERR 2.00 0.00100 0.00070 0.00100 0.0000 0.0030 0.0000 LATT -1 SYMM -X, 0.5+Y, -Z SFAC C H O CL BR UNIT 18 32 4 4 4 TEMP -153.150 SIZE 0.18 0.06 0.05 REM Colorless rod L.S. 10 BOND $H FMAP 2 PLAN 20 CONF ACTA EQIV $1 x, y, z-1 HTAB O1 O2_$1 EQIV $2 -x+2, y+1/2, -z+1 HTAB O2 O1_$2 WGHT 0.061000 FVAR 0.21830 BR1 5 0.725023 0.161037 0.309126 11.00000 0.03496 0.02064 = 0.03146 0.00107 0.01828 -0.00028 BR2 5 0.594826 0.333435 0.666638 11.00000 0.04674 0.04765 = 0.02522 -0.00345 0.01135 -0.02694 CL1 4 0.739259 0.721221 0.138533 11.00000 0.04646 0.02015 = 0.02068 0.00233 0.00491 0.00412 CL2 4 0.833609 0.838506 0.621880 11.00000 0.03801 0.02620 = 0.02107 0.00221 0.00505 -0.00741 O1 3 0.888926 0.392734 0.067742 11.00000 0.03509 0.02447 = 0.01808 0.00563 0.01381 0.00890 AFIX 147 H1O 2 0.906097 0.469920 0.015397 11.00000 -1.50000 AFIX 0 O2 3 0.909884 0.627279 0.881535 11.00000 0.03266 0.03077 = 0.01041 -0.00097 0.00486 -0.00911 AFIX 147 H2O 2 0.966475 0.717893 0.897522 11.00000 -1.50000 AFIX 0 C1 1 0.739217 0.379359 0.047393 11.00000 0.03521 0.02972 = 0.01447 -0.00569 0.00772 -0.00262 AFIX 23 H1A 2 0.712426 0.247723 0.048472 11.00000 -1.20000 H1B 2 0.688969 0.429413 -0.040128 11.00000 -1.20000 AFIX 0 C2 1 0.687648 0.482562 0.150029 11.00000 0.02695 0.02203 = 0.01345 0.00066 0.00341 0.00106 C3 1 0.764646 0.424610 0.287540 11.00000 0.02203 0.01877 = 0.01718 0.00111 0.00631 -0.00105 AFIX 13 H3 2 0.870958 0.438243 0.300121 11.00000 -1.20000 AFIX 0 C4 1 0.727644 0.528369 0.397811 11.00000 0.01994 0.02804 = 0.01300 -0.00027 0.00256 0.00699 AFIX 23 H4A 2 0.727023 0.662441 0.380251 11.00000 -1.20000 H4B 2 0.629368 0.492717 0.400328 11.00000 -1.20000 AFIX 0 C5 1 0.834515 0.488447 0.529101 11.00000 0.01658 0.03104 = 0.01550 0.00002 0.00652 0.00569 AFIX 23 H5A 2 0.932871 0.518367 0.523840 11.00000 -1.20000 H5B 2 0.832090 0.354612 0.546588 11.00000 -1.20000 AFIX 0 C6 1 0.808757 0.593306 0.645215 11.00000 0.01910 0.02355 = 0.01578 -0.00040 0.00683 -0.00215 C7 1 0.923001 0.535018 0.769269 11.00000 0.02544 0.02133 = 0.01591 0.00166 0.00367 -0.00091 AFIX 23 H7A 2 0.915080 0.400552 0.781620 11.00000 -1.20000 H7B 2 1.020100 0.559860 0.758948 11.00000 -1.20000 AFIX 0 C8 1 0.522988 0.474978 0.115715 11.00000 0.02379 0.04634 = 0.02466 -0.00958 -0.00315 0.00579 AFIX 137 H8A 2 0.481238 0.506498 0.023270 11.00000 -1.50000 H8B 2 0.489240 0.563231 0.170111 11.00000 -1.50000 H8C 2 0.492673 0.350331 0.131713 11.00000 -1.50000 AFIX 0 C9 1 0.657644 0.585930 0.656514 11.00000 0.02867 0.03757 = 0.01155 -0.00227 0.00701 -0.00165 AFIX 23 H9A 2 0.591232 0.647223 0.579661 11.00000 -1.20000 H9B 2 0.653235 0.653821 0.735777 11.00000 -1.20000 AFIX 0 HKLF 4 REM su1427 in P2(1) REM R1 = 0.0356 for 3273 Fo > 4sig(Fo) and 0.0398 for all 3545 data REM 139 parameters refined using 1 restraints END WGHT 0.0610 0.0000 REM Highest difference peak 1.564, deepest hole -0.993, 1-sigma level 0.115 Q1 1 0.7864 0.7303 0.2461 11.00000 0.05 1.56 Q2 1 0.6760 0.2805 0.6805 11.00000 0.05 1.39 Q3 1 0.7423 0.9017 0.6232 11.00000 0.05 1.39 Q4 1 0.6544 0.1472 0.2027 11.00000 0.05 1.25 Q5 1 0.8150 0.1712 0.3276 11.00000 0.05 0.52 Q6 1 0.8595 0.2448 0.5750 11.00000 0.05 0.50 Q7 1 0.6551 0.0705 0.6757 11.00000 0.05 0.46 Q8 1 0.7566 0.4125 0.6318 11.00000 0.05 0.44 Q9 1 0.9010 0.7750 0.7765 11.00000 0.05 0.43 Q10 1 0.5158 0.7684 0.7281 11.00000 0.05 0.40 Q11 1 0.7839 0.4826 0.4523 11.00000 0.05 0.38 Q12 1 0.5838 0.4999 0.1220 11.00000 0.05 0.38 Q13 1 0.7965 0.4282 0.3094 11.00000 0.05 0.37 Q14 1 0.9036 0.7541 0.8803 11.00000 0.05 0.37 Q15 1 0.7896 0.9189 0.2519 11.00000 0.05 0.37 Q16 1 0.7892 0.5814 0.2517 11.00000 0.05 0.37 Q17 1 0.6992 0.4014 -0.0003 11.00000 0.05 0.36 Q18 1 0.8004 0.4159 0.0456 11.00000 0.05 0.36 Q19 1 0.8694 0.6191 0.8641 11.00000 0.05 0.35 Q20 1 0.7355 0.4649 0.2280 11.00000 0.05 0.34 ; _shelx_res_checksum 36119 _shelx_hkl_file ; 0 1 0 0.06 0.11 0 1 0 0.23 0.09 0 1 0 0.09 0.07 0 1 0 0.27 0.15 0 1 0 0.03 0.12 0 -1 0 0.09 0.07 0 -1 0 -0.11 0.11 0 -1 0 0.09 0.13 0 -1 0 0.26 0.09 0 2 0 60.09 3.18 0 2 0 60.28 3.08 0 2 0 60.37 3.16 0 2 0 60.67 3.05 0 -2 0 50.32 3.17 0 -2 0 49.60 3.14 0 -2 0 50.59 3.05 0 3 0 -0.26 0.32 0 3 0 -0.08 0.31 0 3 0 -0.25 0.26 0 3 0 -0.16 0.17 0 3 0 -0.25 0.11 0 -3 0 -0.19 0.12 0 -3 0 -0.46 0.25 0 4 0 115.69 6.46 0 4 0 113.31 6.26 0 4 0 112.53 6.42 0 -4 0 116.49 6.43 0 5 0 0.50 0.27 0 5 0 -0.07 0.45 0 5 0 -0.36 0.41 0 -5 0 -0.15 0.39 0 6 0 140.22 7.62 0 6 0 144.90 7.92 0 6 0 141.26 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9 4 1.76 1.20 -4 9 4 1.34 0.85 -4 8 4 0.37 0.69 -4 8 4 0.29 1.06 -4 7 4 21.09 1.70 -4 7 4 23.53 2.17 -4 6 4 19.26 1.52 -4 6 4 20.68 1.87 -4 6 4 19.77 1.45 -4 5 4 57.51 3.61 -4 5 4 54.81 3.24 -4 5 4 56.86 3.37 -4 4 4 25.01 1.71 -4 4 4 24.93 1.52 -4 4 4 24.96 1.60 -4 3 4 17.47 1.19 -4 3 4 17.27 1.26 -4 3 4 17.21 1.06 -4 3 4 16.48 1.03 -4 2 4 28.59 1.85 -4 2 4 29.10 1.65 -4 2 4 30.18 1.84 -4 2 4 28.25 1.65 4 -1 -4 247.39 12.90 -4 1 4 236.42 12.89 -4 1 4 234.06 12.97 -4 1 4 233.51 13.01 -4 1 4 240.61 12.87 -4 1 4 233.37 12.96 4 0 -4 43.62 2.50 4 0 -4 43.07 2.48 -4 0 4 43.74 2.51 -4 0 4 44.12 2.51 -4 0 4 43.80 2.62 -4 0 4 41.46 2.51 -4 0 4 42.74 2.49 4 1 -4 246.10 13.53 4 1 -4 232.51 13.62 4 1 -4 234.24 13.51 -4 -1 4 249.29 13.44 -4 -1 4 262.78 13.54 -4 -1 4 253.81 13.45 -4 -1 4 256.02 13.60 4 2 -4 29.38 1.87 4 2 -4 31.10 1.99 4 2 -4 30.17 1.94 -4 -2 4 29.30 1.93 -4 -2 4 29.83 1.81 -4 -2 4 30.30 1.80 -4 -2 4 28.89 1.91 4 3 -4 15.96 1.27 4 3 -4 15.61 1.29 4 3 -4 15.76 1.19 -4 -3 4 14.62 1.22 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