data_2 _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H17 Br2 N2 O7 V' _chemical_formula_weight 632.13 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -z' _cell_length_a 9.7299(8) _cell_length_b 11.1554(10) _cell_length_c 11.4937(11) _cell_angle_alpha 69.3030(10) _cell_angle_beta 88.5750(10) _cell_angle_gamma 88.9520(10) _cell_volume 1166.60(18) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6138 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.37 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.800 _exptl_crystal_F_000 624 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.310 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.260 _exptl_absorpt_coefficient_mu 3.897 _shelx_estimated_absorpt_T_min 0.378 _shelx_estimated_absorpt_T_max 0.431 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3489 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker SMART 1000 CCD detector' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10918 _diffrn_reflns_av_unetI/netI 0.0541 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.188 _diffrn_reflns_theta_max 25.500 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.992 _reflns_number_total 4312 _reflns_number_gt 3227 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics SHELXL _computing_publication_material SHELXL _refine_special_details ? _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^)+(0.0319P)^2^+0.8848P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4312 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _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 V1 V 0.15263(6) 0.26958(6) 0.73904(6) 0.03521(18) Uani 1 1 d . . . . . N1 N 0.1902(3) 0.4440(3) 0.5954(3) 0.0341(7) Uani 1 1 d . . . . . N2 N 0.2911(3) 0.4415(3) 0.5076(3) 0.0408(8) Uani 1 1 d . . . . . O1 O 0.3082(3) 0.2373(2) 0.6478(2) 0.0423(6) Uani 1 1 d . . . . . O2 O 0.0435(3) 0.3682(2) 0.8046(2) 0.0465(7) Uani 1 1 d . . . . . O3 O 0.0389(3) 0.2144(3) 0.6762(2) 0.0474(7) Uani 1 1 d . . . . . O4 O 0.3219(3) 0.3308(3) 0.8364(3) 0.0508(7) Uani 1 1 d . . . . . O5 O 0.1791(2) 0.1241(2) 0.8799(2) 0.0343(6) Uani 1 1 d . . . . . O6 O 0.4067(3) 0.0213(3) 1.1384(3) 0.0576(8) Uani 1 1 d . . . . . O7 O 0.7496(3) 0.2095(2) 0.2425(2) 0.0458(7) Uani 1 1 d . . . . . Br1 Br -0.16402(4) 0.39282(4) 0.99597(4) 0.04972(15) Uani 1 1 d . . . . . Br2 Br -0.19221(5) 0.89987(5) 0.65952(5) 0.07205(19) Uani 1 1 d . . . . . C1 C 0.0297(4) 0.5803(3) 0.6564(3) 0.0344(8) Uani 1 1 d . . . . . C2 C -0.0105(4) 0.4847(3) 0.7678(3) 0.0350(8) Uani 1 1 d . . . . . C3 C -0.1094(4) 0.5174(4) 0.8420(3) 0.0372(9) Uani 1 1 d . . . . . C4 C -0.1643(4) 0.6386(4) 0.8093(4) 0.0441(10) Uani 1 1 d . . . . . H4 H -0.230419 0.658005 0.859980 0.053 Uiso 1 1 calc R U . . . C5 C -0.1203(4) 0.7306(4) 0.7008(4) 0.0439(10) Uani 1 1 d . . . . . C6 C -0.0255(4) 0.7038(4) 0.6231(3) 0.0410(9) Uani 1 1 d . . . . . H6 H 0.001724 0.767224 0.549057 0.049 Uiso 1 1 calc R U . . . C7 C 0.1330(4) 0.5541(4) 0.5753(3) 0.0392(9) Uani 1 1 d . . . . . H7 H 0.159754 0.621395 0.503983 0.047 Uiso 1 1 calc R U . . . C8 C 0.3462(4) 0.3283(3) 0.5442(3) 0.0360(9) Uani 1 1 d . . . . . C9 C 0.4565(4) 0.2979(3) 0.4682(3) 0.0330(8) Uani 1 1 d . . . . . C10 C 0.5165(4) 0.1768(3) 0.5071(3) 0.0400(9) Uani 1 1 d . . . . . H10 H 0.489716 0.116349 0.583181 0.048 Uiso 1 1 calc R U . . . C11 C 0.6153(4) 0.1445(3) 0.4348(3) 0.0388(9) Uani 1 1 d . . . . . H11 H 0.654028 0.062627 0.461716 0.047 Uiso 1 1 calc R U . . . C12 C 0.6561(4) 0.2337(3) 0.3229(3) 0.0339(8) Uani 1 1 d . . . . . C13 C 0.5999(4) 0.3556(3) 0.2837(4) 0.0432(10) Uani 1 1 d . . . . . H13 H 0.629029 0.416300 0.208680 0.052 Uiso 1 1 calc R U . . . C14 C 0.5005(4) 0.3877(3) 0.3557(4) 0.0424(10) Uani 1 1 d . . . . . H14 H 0.462824 0.469993 0.328739 0.051 Uiso 1 1 calc R U . . . C15 C 0.8156(4) 0.0865(4) 0.2806(4) 0.0551(11) Uani 1 1 d . . . . . H15A H 0.863549 0.072252 0.356343 0.083 Uiso 1 1 calc R U . . . H15B H 0.879748 0.083332 0.216881 0.083 Uiso 1 1 calc R U . . . H15C H 0.747707 0.021317 0.294024 0.083 Uiso 1 1 calc R U . . . C16 C 0.2779(4) 0.1222(3) 0.9601(3) 0.0352(9) Uani 1 1 d . . . . . C17 C 0.3538(4) 0.2381(4) 0.9313(4) 0.0427(10) Uani 1 1 d . . . . . C18 C 0.4593(4) 0.2347(5) 1.0173(5) 0.0588(12) Uani 1 1 d . . . . . H18 H 0.513097 0.306249 1.005293 0.071 Uiso 1 1 calc R U . . . C19 C 0.4790(5) 0.1282(5) 1.1141(5) 0.0658(13) Uani 1 1 d . . . . . H19 H 0.547953 0.127962 1.168778 0.079 Uiso 1 1 calc R U . . . C20 C 0.3033(4) 0.0180(4) 1.0621(4) 0.0413(9) Uani 1 1 d . . . . . C21 C 0.2272(5) -0.1054(4) 1.1052(4) 0.0557(11) Uani 1 1 d . . . . . H21A H 0.227497 -0.138239 1.037468 0.067 Uiso 1 1 calc R U . . . H21B H 0.132253 -0.087406 1.121706 0.067 Uiso 1 1 calc R U . . . C22 C 0.2804(5) -0.2093(4) 1.2188(4) 0.0635(12) Uani 1 1 d . . . . . H22A H 0.376374 -0.223892 1.206761 0.095 Uiso 1 1 calc R U . . . H22B H 0.230677 -0.286744 1.232413 0.095 Uiso 1 1 calc R U . . . H22C H 0.268167 -0.183488 1.289732 0.095 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 V1 0.0400(4) 0.0321(3) 0.0310(3) -0.0087(3) 0.0096(3) -0.0023(3) N1 0.0406(18) 0.0296(16) 0.0299(16) -0.0085(14) 0.0092(13) -0.0001(13) N2 0.049(2) 0.0367(18) 0.0357(18) -0.0121(15) 0.0181(15) -0.0015(14) O1 0.0490(16) 0.0342(14) 0.0392(15) -0.0083(12) 0.0162(12) -0.0004(11) O2 0.0589(17) 0.0372(15) 0.0372(15) -0.0073(12) 0.0209(13) 0.0054(12) O3 0.0483(17) 0.0553(17) 0.0359(15) -0.0124(13) -0.0009(12) -0.0063(13) O4 0.0577(19) 0.0419(16) 0.0532(18) -0.0171(15) 0.0085(15) -0.0174(14) O5 0.0362(14) 0.0343(13) 0.0317(13) -0.0108(11) 0.0034(11) -0.0064(11) O6 0.0490(18) 0.068(2) 0.0552(19) -0.0206(16) -0.0127(15) -0.0024(15) O7 0.0484(16) 0.0427(15) 0.0474(16) -0.0186(13) 0.0161(13) 0.0034(12) Br1 0.0536(3) 0.0549(3) 0.0426(3) -0.0205(2) 0.01939(19) -0.00939(19) Br2 0.0777(4) 0.0609(3) 0.0705(3) -0.0164(3) 0.0005(3) 0.0370(3) C1 0.036(2) 0.040(2) 0.031(2) -0.0167(18) 0.0002(16) 0.0034(16) C2 0.034(2) 0.042(2) 0.031(2) -0.0158(18) 0.0022(16) -0.0013(17) C3 0.034(2) 0.044(2) 0.033(2) -0.0140(18) 0.0058(16) -0.0034(17) C4 0.035(2) 0.058(3) 0.045(2) -0.025(2) 0.0028(18) 0.0046(19) C5 0.043(2) 0.042(2) 0.046(2) -0.016(2) -0.0080(19) 0.0160(18) C6 0.043(2) 0.044(2) 0.033(2) -0.0104(19) -0.0011(18) 0.0054(18) C7 0.045(2) 0.040(2) 0.029(2) -0.0077(18) 0.0051(17) -0.0029(17) C8 0.038(2) 0.035(2) 0.037(2) -0.0146(18) 0.0078(17) -0.0041(16) C9 0.037(2) 0.0295(19) 0.033(2) -0.0123(17) 0.0073(16) -0.0053(15) C10 0.044(2) 0.039(2) 0.030(2) -0.0040(18) 0.0095(17) -0.0044(17) C11 0.041(2) 0.031(2) 0.041(2) -0.0091(18) 0.0013(18) 0.0053(16) C12 0.034(2) 0.036(2) 0.036(2) -0.0178(18) 0.0048(16) -0.0046(16) C13 0.054(3) 0.031(2) 0.040(2) -0.0090(18) 0.0183(19) -0.0015(17) C14 0.051(2) 0.0282(19) 0.046(2) -0.0115(18) 0.0166(19) 0.0004(16) C15 0.053(3) 0.054(3) 0.061(3) -0.025(2) 0.007(2) 0.014(2) C16 0.031(2) 0.041(2) 0.037(2) -0.0192(19) 0.0075(17) -0.0024(16) C17 0.039(2) 0.048(2) 0.045(2) -0.021(2) 0.0129(19) -0.0089(18) C18 0.050(3) 0.067(3) 0.070(3) -0.037(3) 0.006(2) -0.022(2) C19 0.049(3) 0.087(4) 0.071(3) -0.039(3) -0.015(3) -0.011(3) C20 0.032(2) 0.053(3) 0.041(2) -0.019(2) -0.0030(18) 0.0016(18) C21 0.057(3) 0.049(3) 0.055(3) -0.010(2) -0.010(2) -0.006(2) C22 0.066(3) 0.058(3) 0.055(3) -0.006(2) 0.001(2) -0.001(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 V1 O3 1.583(3) . ? V1 O2 1.847(2) . ? V1 O5 1.863(2) . ? V1 O1 1.921(2) . ? V1 N1 2.091(3) . ? V1 O4 2.259(3) . ? N1 C7 1.286(4) . ? N1 N2 1.397(4) . ? N2 C8 1.293(5) . ? O1 C8 1.312(4) . ? O2 C2 1.320(4) . ? O4 C17 1.251(5) . ? O5 C16 1.343(4) . ? O6 C19 1.335(5) . ? O6 C20 1.360(5) . ? O7 C12 1.371(4) . ? O7 C15 1.430(4) . ? Br1 C3 1.894(4) . ? Br2 C5 1.902(4) . ? C1 C6 1.394(5) . ? C1 C2 1.398(5) . ? C1 C7 1.449(5) . ? C2 C3 1.397(5) . ? C3 C4 1.371(5) . ? C4 C5 1.370(5) . ? C4 H4 0.9300 . ? C5 C6 1.369(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.475(5) . ? C9 C10 1.387(5) . ? C9 C14 1.390(5) . ? C10 C11 1.380(5) . ? C10 H10 0.9300 . ? C11 C12 1.373(5) . ? C11 H11 0.9300 . ? C12 C13 1.380(5) . ? C13 C14 1.380(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C20 1.352(5) . ? C16 C17 1.430(5) . ? C17 C18 1.433(6) . ? C18 C19 1.324(6) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.492(5) . ? C21 C22 1.503(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? 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 O3 V1 O2 99.93(13) . . ? O3 V1 O5 98.05(12) . . ? O2 V1 O5 100.77(11) . . ? O3 V1 O1 97.23(12) . . ? O2 V1 O1 154.62(11) . . ? O5 V1 O1 95.16(10) . . ? O3 V1 N1 99.59(13) . . ? O2 V1 N1 83.99(11) . . ? O5 V1 N1 160.64(12) . . ? O1 V1 N1 74.79(11) . . ? O3 V1 O4 175.04(13) . . ? O2 V1 O4 83.34(11) . . ? O5 V1 O4 77.60(10) . . ? O1 V1 O4 80.93(11) . . ? N1 V1 O4 84.41(11) . . ? C7 N1 N2 114.8(3) . . ? C7 N1 V1 129.3(2) . . ? N2 N1 V1 116.0(2) . . ? C8 N2 N1 108.0(3) . . ? C8 O1 V1 118.2(2) . . ? C2 O2 V1 138.2(2) . . ? C17 O4 V1 108.7(2) . . ? C16 O5 V1 120.0(2) . . ? C19 O6 C20 119.8(4) . . ? C12 O7 C15 118.1(3) . . ? C6 C1 C2 120.7(3) . . ? C6 C1 C7 118.7(3) . . ? C2 C1 C7 120.6(3) . . ? O2 C2 C3 120.2(3) . . ? O2 C2 C1 122.3(3) . . ? C3 C2 C1 117.5(3) . . ? C4 C3 C2 122.0(3) . . ? C4 C3 Br1 118.7(3) . . ? C2 C3 Br1 119.2(3) . . ? C5 C4 C3 118.9(3) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C6 C5 C4 121.8(4) . . ? C6 C5 Br2 119.7(3) . . ? C4 C5 Br2 118.5(3) . . ? C5 C6 C1 119.2(3) . . ? C5 C6 H6 120.4 . . ? C1 C6 H6 120.4 . . ? N1 C7 C1 124.4(3) . . ? N1 C7 H7 117.8 . . ? C1 C7 H7 117.8 . . ? N2 C8 O1 122.5(3) . . ? N2 C8 C9 119.8(3) . . ? O1 C8 C9 117.7(3) . . ? C10 C9 C14 118.5(3) . . ? C10 C9 C8 120.1(3) . . ? C14 C9 C8 121.4(3) . . ? C11 C10 C9 121.1(3) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 119.7(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? O7 C12 C11 124.1(3) . . ? O7 C12 C13 115.7(3) . . ? C11 C12 C13 120.1(3) . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C9 120.4(3) . . ? C13 C14 H14 119.8 . . ? C9 C14 H14 119.8 . . ? O7 C15 H15A 109.5 . . ? O7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C16 C20 122.2(3) . . ? O5 C16 C17 115.7(3) . . ? C20 C16 C17 122.1(4) . . ? O4 C17 C16 118.0(4) . . ? O4 C17 C18 126.9(4) . . ? C16 C17 C18 115.1(4) . . ? C19 C18 C17 119.1(4) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 O6 124.4(4) . . ? C18 C19 H19 117.8 . . ? O6 C19 H19 117.8 . . ? C16 C20 O6 119.4(3) . . ? C16 C20 C21 127.0(4) . . ? O6 C20 C21 113.6(4) . . ? C20 C21 C22 116.6(4) . . ? C20 C21 H21A 108.1 . . ? C22 C21 H21A 108.1 . . ? C20 C21 H21B 108.1 . . ? C22 C21 H21B 108.1 . . ? H21A C21 H21B 107.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 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 C7 N1 N2 C8 175.4(3) . . . . ? V1 N1 N2 C8 -5.0(4) . . . . ? O3 V1 O2 C2 -85.2(4) . . . . ? O5 V1 O2 C2 174.6(4) . . . . ? O1 V1 O2 C2 46.7(5) . . . . ? N1 V1 O2 C2 13.6(4) . . . . ? O4 V1 O2 C2 98.6(4) . . . . ? O3 V1 O5 C16 175.0(2) . . . . ? O2 V1 O5 C16 -83.3(2) . . . . ? O1 V1 O5 C16 76.9(2) . . . . ? N1 V1 O5 C16 19.4(4) . . . . ? O4 V1 O5 C16 -2.6(2) . . . . ? V1 O2 C2 C3 169.1(3) . . . . ? V1 O2 C2 C1 -12.3(6) . . . . ? C6 C1 C2 O2 -177.3(4) . . . . ? C7 C1 C2 O2 0.5(5) . . . . ? C6 C1 C2 C3 1.4(5) . . . . ? C7 C1 C2 C3 179.2(3) . . . . ? O2 C2 C3 C4 177.6(3) . . . . ? C1 C2 C3 C4 -1.1(5) . . . . ? O2 C2 C3 Br1 0.3(5) . . . . ? C1 C2 C3 Br1 -178.4(3) . . . . ? C2 C3 C4 C5 -0.3(6) . . . . ? Br1 C3 C4 C5 177.0(3) . . . . ? C3 C4 C5 C6 1.5(6) . . . . ? C3 C4 C5 Br2 -177.7(3) . . . . ? C4 C5 C6 C1 -1.2(6) . . . . ? Br2 C5 C6 C1 178.0(3) . . . . ? C2 C1 C6 C5 -0.3(6) . . . . ? C7 C1 C6 C5 -178.1(3) . . . . ? N2 N1 C7 C1 -177.6(3) . . . . ? V1 N1 C7 C1 2.9(6) . . . . ? C6 C1 C7 N1 -179.2(4) . . . . ? C2 C1 C7 N1 2.9(6) . . . . ? N1 N2 C8 O1 -0.4(5) . . . . ? N1 N2 C8 C9 179.7(3) . . . . ? V1 O1 C8 N2 6.3(5) . . . . ? V1 O1 C8 C9 -173.8(2) . . . . ? N2 C8 C9 C10 179.7(4) . . . . ? O1 C8 C9 C10 -0.2(5) . . . . ? N2 C8 C9 C14 -1.7(6) . . . . ? O1 C8 C9 C14 178.4(3) . . . . ? C14 C9 C10 C11 -1.6(6) . . . . ? C8 C9 C10 C11 177.0(3) . . . . ? C9 C10 C11 C12 0.6(6) . . . . ? C15 O7 C12 C11 -4.2(5) . . . . ? C15 O7 C12 C13 177.3(3) . . . . ? C10 C11 C12 O7 -177.5(3) . . . . ? C10 C11 C12 C13 0.9(6) . . . . ? O7 C12 C13 C14 177.3(3) . . . . ? C11 C12 C13 C14 -1.2(6) . . . . ? C12 C13 C14 C9 0.2(6) . . . . ? C10 C9 C14 C13 1.2(6) . . . . ? C8 C9 C14 C13 -177.3(4) . . . . ? V1 O5 C16 C20 -178.4(3) . . . . ? V1 O5 C16 C17 2.1(4) . . . . ? V1 O4 C17 C16 -2.6(4) . . . . ? V1 O4 C17 C18 178.0(3) . . . . ? O5 C16 C17 O4 0.8(5) . . . . ? C20 C16 C17 O4 -178.7(3) . . . . ? O5 C16 C17 C18 -179.8(3) . . . . ? C20 C16 C17 C18 0.8(5) . . . . ? O4 C17 C18 C19 179.6(4) . . . . ? C16 C17 C18 C19 0.2(6) . . . . ? C17 C18 C19 O6 0.0(7) . . . . ? C20 O6 C19 C18 -1.1(7) . . . . ? O5 C16 C20 O6 178.7(3) . . . . ? C17 C16 C20 O6 -1.9(5) . . . . ? O5 C16 C20 C21 -2.6(6) . . . . ? C17 C16 C20 C21 176.8(4) . . . . ? C19 O6 C20 C16 2.0(5) . . . . ? C19 O6 C20 C21 -176.8(4) . . . . ? C16 C20 C21 C22 177.1(4) . . . . ? O6 C20 C21 C22 -4.1(5) . . . . ? _refine_diff_density_max 0.530 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.074 _shelx_res_file ; TITL mo_Y_4_2_2_0m in P1 New: P-1 mo_Y_4_2_2_0m.res created by SHELXL-2018/3 at 09:38:13 on 07-Nov-2020 CELL 0.71073 9.7299 11.1554 11.4937 69.303 88.575 88.952 ZERR 2 0.0008 0.0010 0.0011 0.001 0.001 0.001 LATT 1 SFAC C H Br N O V UNIT 44 34 4 4 14 2 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! OMIT -3.00 51.00 L.S. 4 ACTA BOND $H FMAP 2 PLAN 0 CONF SIZE 0.31 0.27 0.26 TEMP 25 WGHT 0.031900 0.884800 FVAR 0.54306 V1 6 0.152633 0.269575 0.739045 11.00000 0.04004 0.03215 = 0.03097 -0.00866 0.00956 -0.00230 N1 4 0.190218 0.443958 0.595370 11.00000 0.04062 0.02960 = 0.02992 -0.00845 0.00919 -0.00009 N2 4 0.291116 0.441496 0.507613 11.00000 0.04854 0.03671 = 0.03568 -0.01210 0.01807 -0.00152 O1 5 0.308182 0.237279 0.647771 11.00000 0.04896 0.03417 = 0.03917 -0.00833 0.01615 -0.00042 O2 5 0.043488 0.368241 0.804581 11.00000 0.05888 0.03722 = 0.03723 -0.00731 0.02089 0.00537 O3 5 0.038909 0.214365 0.676177 11.00000 0.04832 0.05535 = 0.03586 -0.01242 -0.00089 -0.00628 O4 5 0.321896 0.330825 0.836385 11.00000 0.05773 0.04185 = 0.05317 -0.01712 0.00852 -0.01744 O5 5 0.179074 0.124123 0.879917 11.00000 0.03615 0.03426 = 0.03169 -0.01079 0.00343 -0.00642 O6 5 0.406727 0.021294 1.138390 11.00000 0.04904 0.06834 = 0.05523 -0.02059 -0.01274 -0.00238 O7 5 0.749599 0.209502 0.242473 11.00000 0.04844 0.04269 = 0.04736 -0.01862 0.01610 0.00345 BR1 3 -0.164023 0.392817 0.995972 11.00000 0.05356 0.05488 = 0.04265 -0.02050 0.01939 -0.00939 BR2 3 -0.192206 0.899867 0.659518 11.00000 0.07766 0.06092 = 0.07048 -0.01639 0.00047 0.03696 C1 1 0.029654 0.580289 0.656371 11.00000 0.03577 0.03964 = 0.03110 -0.01666 0.00017 0.00340 C2 1 -0.010492 0.484747 0.767762 11.00000 0.03442 0.04197 = 0.03085 -0.01583 0.00216 -0.00129 C3 1 -0.109390 0.517353 0.842017 11.00000 0.03421 0.04429 = 0.03305 -0.01401 0.00580 -0.00339 C4 1 -0.164346 0.638553 0.809327 11.00000 0.03477 0.05837 = 0.04452 -0.02536 0.00284 0.00456 AFIX 43 H4 2 -0.230419 0.658005 0.859980 11.00000 -1.20000 AFIX 0 C5 1 -0.120313 0.730561 0.700787 11.00000 0.04348 0.04196 = 0.04647 -0.01626 -0.00797 0.01599 C6 1 -0.025516 0.703808 0.623090 11.00000 0.04288 0.04405 = 0.03313 -0.01037 -0.00113 0.00540 AFIX 43 H6 2 0.001724 0.767224 0.549057 11.00000 -1.20000 AFIX 0 C7 1 0.133021 0.554070 0.575292 11.00000 0.04542 0.03971 = 0.02875 -0.00766 0.00511 -0.00292 AFIX 43 H7 2 0.159754 0.621395 0.503983 11.00000 -1.20000 AFIX 0 C8 1 0.346237 0.328263 0.544184 11.00000 0.03789 0.03458 = 0.03676 -0.01460 0.00781 -0.00414 C9 1 0.456484 0.297938 0.468217 11.00000 0.03721 0.02952 = 0.03304 -0.01225 0.00730 -0.00530 C10 1 0.516494 0.176767 0.507129 11.00000 0.04354 0.03919 = 0.03034 -0.00401 0.00949 -0.00444 AFIX 43 H10 2 0.489716 0.116349 0.583181 11.00000 -1.20000 AFIX 0 C11 1 0.615265 0.144461 0.434807 11.00000 0.04102 0.03118 = 0.04105 -0.00915 0.00131 0.00529 AFIX 43 H11 2 0.654028 0.062627 0.461716 11.00000 -1.20000 AFIX 0 C12 1 0.656101 0.233655 0.322912 11.00000 0.03402 0.03610 = 0.03551 -0.01779 0.00475 -0.00460 C13 1 0.599880 0.355632 0.283741 11.00000 0.05434 0.03122 = 0.04004 -0.00895 0.01825 -0.00145 AFIX 43 H13 2 0.629029 0.416300 0.208680 11.00000 -1.20000 AFIX 0 C14 1 0.500545 0.387746 0.355688 11.00000 0.05085 0.02823 = 0.04591 -0.01155 0.01657 0.00043 AFIX 43 H14 2 0.462824 0.469993 0.328739 11.00000 -1.20000 AFIX 0 C15 1 0.815568 0.086501 0.280557 11.00000 0.05334 0.05404 = 0.06088 -0.02529 0.00657 0.01399 AFIX 137 H15A 2 0.863549 0.072252 0.356343 11.00000 -1.50000 H15B 2 0.879748 0.083332 0.216881 11.00000 -1.50000 H15C 2 0.747707 0.021317 0.294024 11.00000 -1.50000 AFIX 0 C16 1 0.277886 0.122238 0.960113 11.00000 0.03120 0.04142 = 0.03698 -0.01921 0.00750 -0.00243 C17 1 0.353786 0.238080 0.931299 11.00000 0.03900 0.04754 = 0.04533 -0.02141 0.01288 -0.00893 C18 1 0.459266 0.234663 1.017303 11.00000 0.05021 0.06651 = 0.07003 -0.03653 0.00645 -0.02240 AFIX 43 H18 2 0.513097 0.306249 1.005293 11.00000 -1.20000 AFIX 0 C19 1 0.479027 0.128236 1.114056 11.00000 0.04909 0.08713 = 0.07100 -0.03856 -0.01472 -0.01105 AFIX 43 H19 2 0.547953 0.127962 1.168778 11.00000 -1.20000 AFIX 0 C20 1 0.303334 0.017972 1.062111 11.00000 0.03182 0.05339 = 0.04066 -0.01915 -0.00297 0.00164 C21 1 0.227175 -0.105396 1.105160 11.00000 0.05656 0.04946 = 0.05497 -0.00985 -0.01033 -0.00612 AFIX 23 H21A 2 0.227497 -0.138239 1.037468 11.00000 -1.20000 H21B 2 0.132253 -0.087406 1.121706 11.00000 -1.20000 AFIX 0 C22 1 0.280404 -0.209257 1.218774 11.00000 0.06628 0.05808 = 0.05499 -0.00615 0.00090 -0.00074 AFIX 137 H22A 2 0.376374 -0.223892 1.206761 11.00000 -1.50000 H22B 2 0.230677 -0.286744 1.232413 11.00000 -1.50000 H22C 2 0.268167 -0.183488 1.289732 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_Y_4_2_2_0m in P1 New: P-1 REM wR2 = 0.0924, GooF = S = 1.048, Restrained GooF = 1.048 for all data REM R1 = 0.0399 for 3227 Fo > 4sig(Fo) and 0.0644 for all 4312 data REM 309 parameters refined using 0 restraints END WGHT 0.0321 0.8728 REM Highest difference peak 0.530, deepest hole -0.449, 1-sigma level 0.074 Q1 1 -0.1719 0.8754 0.6001 11.00000 0.05 0.49 Q2 1 -0.0969 0.9198 0.6945 11.00000 0.05 0.47 Q3 1 -0.2025 0.4625 0.9363 11.00000 0.05 0.38 Q4 1 0.2419 0.2995 0.7965 11.00000 0.05 0.34 Q5 1 -0.0456 0.3921 1.0382 11.00000 0.05 0.34 Q6 1 -0.1355 0.8672 0.7300 11.00000 0.05 0.33 Q7 1 -0.1353 0.3181 0.9639 11.00000 0.05 0.33 Q8 1 0.0355 0.2719 0.6932 11.00000 0.05 0.30 Q9 1 0.1217 0.7774 0.4057 11.00000 0.05 0.30 Q10 1 -0.0187 0.2228 0.6424 11.00000 0.05 0.29 Q11 1 0.1783 -0.2434 1.0733 11.00000 0.05 0.28 Q12 1 0.0132 0.6655 0.6643 11.00000 0.05 0.28 Q13 1 0.1182 0.3590 0.7641 11.00000 0.05 0.28 Q14 1 0.1917 0.1840 0.8038 11.00000 0.05 0.27 Q15 1 -0.2959 0.9077 0.5785 11.00000 0.05 0.26 Q16 1 0.3435 0.0330 0.9935 11.00000 0.05 0.26 Q17 1 -0.2691 0.8635 0.7266 11.00000 0.05 0.26 Q18 1 -0.1627 0.7994 0.6772 11.00000 0.05 0.26 Q19 1 -0.2453 0.3883 0.9376 11.00000 0.05 0.26 Q20 1 -0.1279 0.5731 0.8650 11.00000 0.05 0.25 ; _shelx_res_checksum 2615 _shelx_hkl_file ; -2 0 0 2863.99 130.790 1 -2 0 0 2519.03 130.652 2 2 0 0 2948.24 130.809 1 -3 0 0 3922.17 177.378 1 -3 0 0 3533.72 177.148 2 3 0 0 3826.73 177.378 1 -4 0 0 132.175 7.51145 2 -4 0 0 145.953 8.04900 1 4 0 0 137.950 8.03711 1 4 0 0 142.446 7.14841 2 -5 0 0 623.635 30.4776 2 -5 0 0 636.787 31.1773 1 5 0 0 634.841 31.1739 1 5 0 0 641.321 30.2218 2 -6 0 0 2534.50 123.493 1 6 0 0 2652.29 122.478 2 6 0 0 2614.22 123.614 1 -7 0 0 188.384 12.4190 1 7 0 0 206.714 10.1425 2 7 0 0 191.271 12.2158 1 7 0 0 181.646 9.66889 2 8 0 0 105.866 10.0829 1 9 0 0 257.703 17.3107 1 10 0 0 18.7797 7.68689 1 11 0 0 -1.4560 8.71197 1 12 0 0 -6.9388 10.4312 1 12 -1 0 -4.2321 10.5096 1 11 -1 0 -1.0543 9.13987 1 10 -1 0 72.5029 13.3534 1 9 -1 0 4.32475 2.71245 2 9 -1 0 5.54590 5.77908 1 8 -1 0 30.1184 5.87829 1 8 -1 0 26.4710 3.34809 2 7 -1 0 24.8979 5.04940 1 7 -1 0 24.4062 3.07035 2 -7 1 0 25.9051 4.88446 1 -7 1 0 21.9500 6.03774 2 6 -1 0 234.501 12.1136 2 6 -1 0 260.353 13.7954 1 -6 1 0 218.378 13.0214 2 5 -1 0 25.7095 3.18619 2 -5 1 0 27.5840 3.62713 2 4 -1 0 240.548 12.7351 1 4 -1 0 244.335 11.9772 2 -4 1 0 230.201 12.2945 2 -4 1 0 243.835 12.7085 1 3 -1 0 56.9465 4.16143 1 3 -1 0 50.6758 3.48249 2 -3 1 0 65.1171 4.28348 1 -3 1 0 48.3920 3.67593 2 2 -1 0 58.2068 3.76159 1 2 -1 0 51.1383 3.21375 2 -2 1 0 45.1813 3.22343 2 -2 1 0 54.6540 3.69941 1 1 -1 0 4.67683 1.23763 1 1 -1 0 5.95472 1.10163 2 -1 1 0 4.45015 1.15255 2 -1 1 0 2.60142 1.09283 1 -2 -1 0 1908.07 90.2610 2 -2 -1 0 1972.58 90.5503 1 2 1 0 1926.71 90.2597 2 2 1 0 1861.62 90.5334 1 -3 -1 0 185.075 9.56848 1 3 1 0 186.959 8.95321 2 3 1 0 182.049 8.88529 2 -4 -1 0 181.857 9.46060 1 4 1 0 174.994 8.28533 2 4 1 0 173.807 9.31921 1 4 1 0 153.082 8.62338 2 -5 -1 0 208.788 11.2792 1 5 1 0 194.897 9.61834 2 5 1 0 190.302 9.83739 2 5 1 0 202.410 11.0753 1 -6 -1 0 171.358 10.6400 1 6 1 0 165.732 10.4013 1 -7 -1 0 987.182 47.9918 1 7 1 0 970.977 48.0248 1 8 1 0 20.0773 5.09604 1 9 1 0 11.7902 5.77198 1 10 1 0 22.0096 7.43376 1 11 1 0 -0.3825 8.92010 1 12 1 0 9.62400 10.5209 1 12 -2 0 0.76967 10.8299 1 11 -2 0 2.15671 9.28790 1 10 -2 0 16.7096 7.96800 1 -10 2 0 24.1667 6.04503 2 9 -2 0 43.7398 6.44627 2 9 -2 0 50.4643 7.74459 1 -9 2 0 51.4638 8.16553 2 8 -2 0 5.64562 3.57103 2 8 -2 0 16.9807 5.83134 1 -8 2 0 9.30524 5.10645 2 7 -2 0 183.483 12.3421 1 -7 2 0 166.868 12.0730 1 -7 2 0 160.428 11.0070 2 6 -2 0 17.1673 4.03739 1 6 -2 0 15.3022 3.02277 2 -6 2 0 16.9401 4.16069 1 -6 2 0 11.5678 3.95351 2 5 -2 0 11.8543 3.36775 1 5 -2 0 8.37551 2.52270 2 -5 2 0 6.97699 3.03019 2 -5 2 0 14.8450 3.61080 1 4 -2 0 1590.50 75.0624 1 4 -2 0 1640.49 74.3897 2 -4 2 0 1584.15 74.5401 2 -4 2 0 1454.23 74.8490 1 3 -2 0 357.168 16.9092 2 3 -2 0 352.150 17.6618 1 -3 2 0 324.267 17.4070 1 -3 2 0 337.506 17.0253 2 2 -2 0 1367.54 58.9493 2 2 -2 0 1162.36 59.4169 1 -2 2 0 1054.95 59.2434 1 -2 2 0 1381.04 58.9580 2 1 -2 0 1906.24 89.4047 2 1 -2 0 1866.62 89.6819 1 -1 2 0 1978.51 89.6005 1 -1 2 0 1819.79 89.3807 2 0 -2 0 920.951 43.1457 1 0 -2 0 913.195 43.2618 2 0 -2 0 925.257 43.1348 1 0 2 0 887.804 43.2515 2 -1 -2 0 139.335 6.96036 2 -1 -2 0 135.796 6.91568 1 1 2 0 135.367 6.91576 1 1 2 0 142.289 6.97380 2 -2 -2 0 2314.77 107.696 2 -2 -2 0 2325.25 107.870 1 2 2 0 2216.98 107.864 1 2 2 0 2293.49 107.695 2 -3 -2 0 70.0744 4.68638 1 -3 -2 0 73.5963 3.93817 2 3 2 0 69.9929 3.94731 2 -4 -2 0 1819.55 85.4826 2 -4 -2 0 1890.78 86.1318 1 4 2 0 1765.59 86.0939 1 4 2 0 1784.25 85.4553 2 -5 -2 0 942.033 45.3344 1 5 2 0 961.981 44.4617 2 5 2 0 931.379 44.3158 2 5 2 0 919.230 45.3475 1 -6 -2 0 195.891 11.7645 1 6 2 0 194.192 11.7443 1 -7 -2 0 278.746 15.9185 1 7 2 0 274.453 16.0390 1 8 2 0 234.691 15.1501 1 9 2 0 21.6667 6.09541 1 10 2 0 321.660 21.3239 1 11 2 0 8.56160 8.55571 1 12 2 0 3.26249 10.3142 1 12 -3 0 37.4897 12.1185 1 11 -3 0 -5.8736 8.77201 1 10 -3 0 77.8262 10.8561 1 -10 3 0 79.4382 10.7584 2 9 -3 0 299.216 17.1960 2 9 -3 0 315.196 20.7595 1 -9 3 0 338.774 18.7684 2 8 -3 0 293.455 18.2214 1 8 -3 0 266.340 15.3321 2 -8 3 0 280.465 16.5576 2 7 -3 0 26.6522 4.32241 2 7 -3 0 27.0548 6.00592 1 -7 3 0 26.2429 5.40094 2 -7 3 0 25.8207 5.22608 1 6 -3 0 545.042 25.8050 2 6 -3 0 556.297 27.2916 1 -6 3 0 504.024 26.0676 2 -6 3 0 461.135 26.6289 1 5 -3 0 458.424 21.8392 2 5 -3 0 453.418 23.1345 1 -5 3 0 443.103 22.0022 2 -5 3 0 383.232 22.5101 1 4 -3 0 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1 -1 4 13 87.4770 11.5716 1 -1 4 13 116.823 16.2294 2 0 4 13 11.3489 6.31452 1 0 4 13 12.5234 9.45743 2 1 4 13 13.7364 10.1333 2 1 4 13 29.9138 7.39471 1 2 4 13 54.4880 8.96625 1 2 4 13 50.1453 11.3099 2 3 4 13 47.4431 9.36047 1 3 4 13 27.1091 10.5985 2 4 4 13 -10.286 8.81909 1 4 4 13 -11.467 10.7131 2 5 4 13 -17.092 10.8276 2 5 4 13 -3.8798 10.3104 1 6 4 13 -9.5308 10.6438 1 6 4 13 -10.525 12.9220 2 -5 5 13 18.8782 8.80736 2 -4 5 13 74.6487 13.9083 2 -3 5 13 153.311 16.1234 2 -3 5 13 165.185 13.1907 1 -2 5 13 51.1989 9.65258 1 -2 5 13 59.0069 10.8659 2 -1 5 13 45.6505 9.65674 2 -1 5 13 36.4825 6.38440 1 0 5 13 121.611 16.2377 2 0 5 13 96.0173 11.6304 1 1 5 13 51.5775 8.13332 1 1 5 13 91.7901 15.7904 2 2 5 13 195.248 16.2894 1 2 5 13 188.009 19.9078 2 3 5 13 171.433 17.0314 1 3 5 13 149.813 19.2651 2 4 5 13 -10.505 8.80355 1 4 5 13 0.79351 11.8431 2 5 5 13 4.27494 13.5859 2 5 5 13 0.23967 9.87432 1 6 5 13 -10.497 10.8343 1 6 5 13 -0.8976 12.2513 2 -5 6 13 4.38784 8.43162 2 -4 6 13 21.4798 9.20103 2 -3 6 13 9.05972 8.99789 2 -2 6 13 11.7065 9.23593 2 -1 6 13 1.21366 9.01801 2 0 6 13 13.4258 10.2265 2 1 6 13 25.4484 10.8960 2 1 6 13 8.48192 7.83825 1 2 6 13 -6.3145 7.45029 1 2 6 13 18.5413 10.7804 2 3 6 13 12.2824 11.2856 2 3 6 13 -3.4701 7.54150 1 4 6 13 -14.425 8.22496 1 4 6 13 -1.6261 11.5328 2 5 6 13 -16.236 9.41529 1 5 6 13 -3.5552 12.6546 2 6 6 13 -18.140 13.4206 2 -5 7 13 16.4121 8.52035 2 -4 7 13 6.89986 8.63564 2 -3 7 13 28.5715 9.73648 2 -2 7 13 78.0045 11.9672 2 -1 7 13 27.7157 9.98670 2 0 7 13 20.4300 10.5402 2 1 7 13 164.112 19.6406 2 2 7 13 17.9733 11.2278 2 3 7 13 2.28807 12.0735 2 4 7 13 13.0250 13.6926 2 5 7 13 11.3934 14.4903 2 6 7 13 -23.050 14.4536 2 -4 8 13 1.65593 8.45001 2 -3 8 13 83.1775 14.8981 2 -2 8 13 75.6396 11.9507 2 -1 8 13 13.6874 10.2407 2 0 8 13 52.3943 11.9999 2 1 8 13 15.2991 11.5127 2 2 8 13 19.7115 10.8345 2 3 8 13 1.79985 10.3899 2 4 8 13 46.5003 14.0931 2 5 8 13 35.2676 14.8424 2 -4 9 13 2.14722 9.43829 2 -3 9 13 17.4460 9.59900 2 -2 9 13 23.4205 10.3860 2 -1 9 13 36.8739 10.4608 2 0 9 13 33.2981 11.2125 2 1 9 13 29.6729 11.6059 2 2 9 13 2.88288 11.4191 2 3 9 13 1.12916 12.2300 2 4 9 13 11.3753 14.5454 2 -3 10 13 -1.6553 9.65030 2 -2 10 13 58.5768 11.1623 2 -1 10 13 61.6278 11.4193 2 0 10 13 12.3391 10.6371 2 1 10 13 2.14040 10.9663 2 2 10 13 37.5036 11.6217 2 3 10 13 18.9197 12.3344 2 0 11 13 44.2024 15.3495 2 -2 1 14 51.5365 12.8534 2 -1 1 14 110.318 18.5875 2 0 1 14 98.3070 17.0936 1 1 1 14 23.4662 9.84433 1 1 1 14 -8.4261 10.9484 2 2 1 14 101.974 18.2013 1 -3 2 14 5.82253 10.8896 2 -3 2 14 6.21634 7.53220 1 -2 2 14 18.2035 10.5454 2 -2 2 14 24.0563 8.26949 1 1 2 14 9.80208 11.5546 2 1 2 14 19.9696 8.71451 1 2 2 14 1.04395 10.5524 2 2 2 14 26.7137 9.47158 1 3 2 14 9.01701 9.52131 1 3 2 14 -8.0321 11.6601 2 -3 3 14 50.3114 11.5241 2 -3 3 14 68.4740 12.8679 1 -2 3 14 30.0007 7.90938 1 -2 3 14 32.4335 11.7054 2 -1 3 14 10.6046 10.5889 2 0 3 14 57.3033 11.9993 2 1 3 14 46.7725 12.1959 2 2 3 14 -2.3543 10.6977 2 2 3 14 -0.4939 8.39966 1 3 3 14 18.2701 11.0404 2 3 3 14 25.6731 9.72352 1 4 3 14 -14.338 18.4188 2 4 3 14 3.91606 10.0532 1 -4 4 14 10.8185 9.48439 2 -3 4 14 129.674 17.7547 2 -2 4 14 16.2324 10.1361 2 -2 4 14 25.9099 9.00744 1 -1 4 14 25.7067 6.74737 1 -1 4 14 9.54302 10.3767 2 0 4 14 16.9298 11.5310 2 0 4 14 30.5508 7.44310 1 1 4 14 77.3882 13.7920 2 1 4 14 71.2079 12.4515 1 2 4 14 40.0692 9.15416 1 2 4 14 25.1832 11.8649 2 3 4 14 11.4229 9.04966 1 3 4 14 -11.958 10.2860 2 4 4 14 -1.1488 12.4586 2 4 4 14 14.9086 10.4327 1 -4 5 14 3.07679 9.10686 2 -3 5 14 31.5242 10.1933 2 -2 5 14 22.6682 11.0958 2 -1 5 14 17.4402 10.7184 2 0 5 14 28.5294 11.4945 2 1 5 14 5.68100 11.4721 2 2 5 14 8.26576 12.2749 2 3 5 14 3.45433 12.3725 2 4 5 14 -1.6688 12.3682 2 -3 6 14 14.9830 9.64744 2 -2 6 14 42.9738 10.9824 2 -1 6 14 11.7874 10.3936 2 0 6 14 6.39786 11.1738 2 1 6 14 25.3274 12.7922 2 2 6 14 10.7440 11.5220 2 3 6 14 6.82951 12.2523 2 4 6 14 13.7359 14.4199 2 -3 7 14 25.9198 10.7286 2 -2 7 14 199.442 20.6249 2 -1 7 14 103.135 17.5119 2 0 7 14 -4.4160 10.3192 2 1 7 14 50.4275 12.7342 2 2 7 14 83.5337 16.1671 2 3 7 14 24.9802 15.0732 2 4 7 14 14.1091 22.1819 2 -2 8 14 -6.4395 10.7041 2 -1 8 14 30.1589 12.1421 2 0 8 14 9.25635 11.7766 2 1 8 14 5.37293 11.8944 2 2 8 14 13.3060 12.8253 2 3 8 14 15.1079 15.8375 2 -1 9 14 37.7783 11.4157 2 0 9 14 59.8482 14.0225 2 1 9 14 0.13229 14.2796 2 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.3489 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71061 9.726 11.154 11.498 69.322 88.543 88.894 ) ; _shelx_hkl_checksum 41964