data_Badjic_TrisNH _audit_creation_date 2021-06-03 _audit_creation_method ; Olex2 1.3-alpha (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C39 H21 N3 O6, 2(C H2 Cl2)' _chemical_formula_sum 'C41 H25 Cl4 N3 O6' _chemical_formula_weight 797.44 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 11 _space_group_name_H-M_alt 'P 1 21/m 1' _space_group_name_Hall '-P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.8486(7) _cell_length_b 14.6173(10) _cell_length_c 12.4874(9) _cell_angle_alpha 90 _cell_angle_beta 102.991(3) _cell_angle_gamma 90 _cell_volume 1751.7(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9968 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 26.362 _cell_measurement_theta_min 2.985 _shelx_estimated_absorpt_T_max 0.955 _shelx_estimated_absorpt_T_min 0.910 _exptl_absorpt_coefficient_mu 0.394 _exptl_absorpt_correction_T_max 0.0452 _exptl_absorpt_correction_T_min 0.0251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0555 before and 0.0484 after correction. The Ratio of minimum to maximum transmission is 0.5553. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour Colorless _exptl_crystal_colour_primary Colorless _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description Block _exptl_crystal_F_000 816 _exptl_crystal_preparation ? _exptl_crystal_size_max 0.243 _exptl_crystal_size_mid 0.226 _exptl_crystal_size_min 0.118 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_unetI/netI 0.0209 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 21428 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 26.374 _diffrn_reflns_theta_min 2.984 _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker Photon II area detector' _diffrn_detector_area_resol_mean 10.5 _diffrn_detector_type 'CMOS area detector' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Curved-Graphite, Bruker TRIUMPH' _diffrn_radiation_probe X-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_source 'sealed tube' _diffrn_source_current 30.0 _diffrn_source_power 1.35 _diffrn_source_type fine-focus _diffrn_source_voltage 45.0 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3114 _reflns_number_total 3728 _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 'SAINT v8.40A (Bruker, 2019)' _computing_data_collection 'APEX3 v2019.1-0 (Bruker, 2019)' _computing_data_reduction 'SAINT v8.40A (Bruker, 2019)' _computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.534 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.051 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 285 _refine_ls_number_reflns 3728 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0421 _refine_ls_restrained_S_all 1.027 _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^)+(0.0535P)^2^+1.4789P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1094 _refine_ls_wR_factor_ref 0.1172 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Restrained distances N1-H1 = N2-H2 0.95 with sigma of 0.02 3. Others Sof(Cl3B)=1-FVAR(1) Sof(C2SB)=Sof(H2SC)=Sof(H2SD)=0.5*(1-FVAR(2)) Sof(Cl3S)=Sof(Cl4S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=0.5*FVAR(2) Fixed Sof: H1SA(0.5) H1SB(0.5) 4.a Ternary CH refined with riding coordinates: C3(H3), C5(H5), C15(H15) 4.b Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C16(H16A,H16B), C2S(H2SA,H2SB), C1S(H1SA,H1SB), C2SB(H2SC,H2SD) 4.c Aromatic/amide H refined with riding coordinates: C8(H8), C11(H11), C18(H18) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.54877(16) 0.46638(11) 0.86277(13) 0.0395(4) Uani 1 1 d . . . . . O2 O 0.83566(17) 0.63580(10) 1.12859(12) 0.0400(4) Uani 1 1 d . . . . . O3 O 0.26313(15) 0.59318(11) 0.47664(12) 0.0376(4) Uani 1 1 d . . . . . N1 N 0.6712(2) 0.54644(13) 1.01332(14) 0.0354(4) Uani 1 1 d D . . . . H1 H 0.604(2) 0.545(2) 1.053(2) 0.064(9) Uiso 1 1 d D . . . . N2 N 0.2294(2) 0.750000 0.4808(2) 0.0341(6) Uani 1 2 d DS T P . . H2 H 0.140(2) 0.750000 0.492(3) 0.055(11) Uiso 1 2 d DS . P . . C1 C 1.07997(18) 0.70345(13) 0.70620(14) 0.0230(4) Uani 1 1 d . . . . . C2 C 0.99228(18) 0.65411(12) 0.61893(14) 0.0218(4) Uani 1 1 d . . . . . C3 C 1.00286(19) 0.55327(12) 0.65346(14) 0.0238(4) Uani 1 1 d . . . . . H3 H 0.970946 0.506657 0.594562 0.029 Uiso 1 1 calc R U . . . C4 C 1.15921(19) 0.55098(13) 0.71452(15) 0.0265(4) Uani 1 1 d . . . . . H4A H 1.185755 0.493198 0.755202 0.032 Uiso 1 1 calc R U . . . H4B H 1.222992 0.563575 0.665285 0.032 Uiso 1 1 calc R U . . . C5 C 1.14719(19) 0.63274(13) 0.79133(15) 0.0258(4) Uani 1 1 d . . . . . H5 H 1.233885 0.651515 0.845321 0.031 Uiso 1 1 calc R U . . . C6 C 1.0256(2) 0.60009(13) 0.83779(15) 0.0256(4) Uani 1 1 d . . . . . C7 C 0.9360(2) 0.55054(12) 0.75321(15) 0.0252(4) Uani 1 1 d . . . . . C8 C 0.8108(2) 0.51525(13) 0.76688(15) 0.0268(4) Uani 1 1 d . . . . . H8 H 0.750682 0.480977 0.710988 0.032 Uiso 1 1 calc R U . . . C9 C 0.7781(2) 0.53324(13) 0.86833(16) 0.0291(4) Uani 1 1 d . . . . . C10 C 0.8649(2) 0.58409(13) 0.94922(15) 0.0286(4) Uani 1 1 d . . . . . C11 C 0.9917(2) 0.61874(13) 0.93723(15) 0.0280(4) Uani 1 1 d . . . . . H11 H 1.051249 0.652964 0.993482 0.034 Uiso 1 1 calc R U . . . C12 C 0.6514(2) 0.50888(14) 0.90921(17) 0.0331(5) Uani 1 1 d . . . . . C13 C 0.7962(2) 0.59469(14) 1.04354(16) 0.0327(5) Uani 1 1 d . . . . . C14 C 0.91594(17) 0.70117(12) 0.53097(14) 0.0216(4) Uani 1 1 d . . . . . C15 C 0.81713(18) 0.67189(13) 0.42374(14) 0.0221(4) Uani 1 1 d . . . . . H15 H 0.826623 0.607721 0.398626 0.026 Uiso 1 1 calc R U . . . C16 C 0.8467(3) 0.750000 0.3472(2) 0.0245(5) Uani 1 2 d S T P . . H16A H 0.944096 0.750000 0.338244 0.029 Uiso 1 2 calc R U P . . H16B H 0.780957 0.749999 0.274454 0.029 Uiso 1 2 calc R U P . . C17 C 0.67293(18) 0.70157(13) 0.43490(14) 0.0224(4) Uani 1 1 d . . . . . C18 C 0.55769(19) 0.65152(13) 0.44630(14) 0.0252(4) Uani 1 1 d . . . . . H18 H 0.557177 0.586526 0.446477 0.030 Uiso 1 1 calc R U . . . C19 C 0.44310(18) 0.70263(14) 0.45744(14) 0.0269(4) Uani 1 1 d . . . . . C20 C 0.3046(2) 0.67074(16) 0.47224(15) 0.0312(4) Uani 1 1 d . . . . . Cl3S Cl 0.72503(12) 0.750000 0.72409(10) 0.0330(4) Uani 0.620(3) 2 d S T P A 1 Cl4S Cl 0.4520(3) 0.6969(2) 0.75229(17) 0.0535(6) Uani 0.3099(14) 1 d . . P A 1 C2S C 0.5874(8) 0.7776(6) 0.7850(8) 0.054(3) Uani 0.3099(14) 1 d . . P A 1 H2SA H 0.550956 0.838833 0.759631 0.065 Uiso 0.3099(14) 1 calc R U P A 1 H2SB H 0.621876 0.780125 0.865771 0.065 Uiso 0.3099(14) 1 calc R U P A 1 Cl1S Cl 0.74390(12) 0.250000 0.82259(8) 0.0649(3) Uani 1 2 d S T P . . Cl2S Cl 0.55867(12) 0.250000 0.97638(8) 0.0610(3) Uani 1 2 d S T P . . C1S C 0.5685(4) 0.250000 0.8366(3) 0.0543(10) Uani 1 2 d S T P . . H1SA H 0.520187 0.304780 0.799837 0.065 Uiso 0.5 1 calc R U P . . H1SB H 0.520187 0.195220 0.799837 0.065 Uiso 0.5 1 calc R U P . . Cl3B Cl 0.50125(19) 0.65106(14) 0.72997(15) 0.0435(6) Uani 0.380(3) 1 d . . P A 2 C2SB C 0.6035(9) 0.750000 0.7297(8) 0.040(2) Uani 0.380(3) 2 d S T P A 2 H2SC H 0.681520 0.750000 0.795436 0.048 Uiso 0.380(3) 2 calc R U P A 2 H2SD H 0.643452 0.750001 0.663677 0.048 Uiso 0.380(3) 2 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0427(9) 0.0380(8) 0.0428(9) -0.0051(7) 0.0200(7) -0.0081(7) O2 0.0602(10) 0.0327(8) 0.0306(8) -0.0030(6) 0.0177(7) -0.0010(7) O3 0.0312(8) 0.0486(9) 0.0352(8) -0.0068(7) 0.0121(6) -0.0144(7) N1 0.0434(10) 0.0349(10) 0.0329(9) -0.0013(7) 0.0193(8) -0.0006(8) N2 0.0197(11) 0.0519(16) 0.0320(12) 0.000 0.0083(10) 0.000 C1 0.0202(8) 0.0269(9) 0.0224(8) 0.0014(7) 0.0060(7) 0.0020(7) C2 0.0204(8) 0.0232(9) 0.0232(8) -0.0006(7) 0.0081(7) 0.0013(7) C3 0.0260(9) 0.0228(9) 0.0233(9) 0.0014(7) 0.0073(7) 0.0028(7) C4 0.0272(9) 0.0280(10) 0.0244(9) 0.0015(7) 0.0061(7) 0.0046(8) C5 0.0257(9) 0.0269(9) 0.0238(9) 0.0009(7) 0.0033(7) 0.0042(7) C6 0.0293(9) 0.0210(9) 0.0265(9) 0.0039(7) 0.0060(7) 0.0053(7) C7 0.0313(10) 0.0209(9) 0.0243(9) 0.0027(7) 0.0083(7) 0.0054(7) C8 0.0329(10) 0.0207(9) 0.0279(9) 0.0006(7) 0.0094(8) 0.0001(7) C9 0.0353(11) 0.0235(9) 0.0312(10) 0.0042(8) 0.0133(8) 0.0027(8) C10 0.0397(11) 0.0218(9) 0.0257(9) 0.0027(7) 0.0103(8) 0.0050(8) C11 0.0354(10) 0.0244(9) 0.0239(9) 0.0021(7) 0.0058(8) 0.0052(8) C12 0.0413(12) 0.0267(10) 0.0348(11) 0.0016(8) 0.0162(9) 0.0005(9) C13 0.0446(12) 0.0265(10) 0.0296(10) 0.0048(8) 0.0137(9) 0.0036(9) C14 0.0187(8) 0.0257(9) 0.0216(8) -0.0024(7) 0.0070(7) -0.0002(7) C15 0.0208(8) 0.0245(9) 0.0212(8) -0.0021(7) 0.0054(7) 0.0002(7) C16 0.0240(13) 0.0296(14) 0.0206(12) 0.000 0.0063(10) 0.000 C17 0.0222(9) 0.0270(9) 0.0175(8) -0.0009(7) 0.0037(7) 0.0008(7) C18 0.0243(9) 0.0282(9) 0.0228(8) -0.0022(7) 0.0046(7) -0.0035(7) C19 0.0215(9) 0.0373(10) 0.0219(9) -0.0009(8) 0.0051(7) -0.0034(8) C20 0.0238(9) 0.0473(13) 0.0231(9) -0.0025(8) 0.0063(7) -0.0052(9) Cl3S 0.0301(7) 0.0336(6) 0.0380(6) 0.000 0.0134(5) 0.000 Cl4S 0.0375(11) 0.0835(18) 0.0426(11) -0.0105(11) 0.0153(9) -0.0239(12) C2S 0.041(4) 0.053(6) 0.079(6) -0.030(4) 0.036(4) -0.016(3) Cl1S 0.0715(7) 0.0659(6) 0.0454(5) 0.000 -0.0117(5) 0.000 Cl2S 0.0773(7) 0.0532(5) 0.0416(5) 0.000 -0.0095(4) 0.000 C1S 0.071(3) 0.0365(18) 0.0416(19) 0.000 -0.0165(17) 0.000 Cl3B 0.0397(9) 0.0484(11) 0.0409(9) 0.0111(7) 0.0061(7) -0.0024(8) C2SB 0.032(5) 0.050(6) 0.035(5) 0.000 0.002(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C12 1.217(3) . ? O2 C13 1.206(3) . ? O3 C20 1.211(3) . ? N1 H1 0.915(17) . ? N1 C12 1.384(3) . ? N1 C13 1.395(3) . ? N2 H2 0.927(19) . ? N2 C20 1.392(3) . ? N2 C20 1.392(3) 4_575 ? C1 C1 1.361(4) 4_575 ? C1 C2 1.425(2) . ? C1 C5 1.523(2) . ? C2 C3 1.533(2) . ? C2 C14 1.369(2) . ? C3 H3 1.0000 . ? C3 C4 1.558(3) . ? C3 C7 1.534(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.553(3) . ? C5 H5 1.0000 . ? C5 C6 1.520(3) . ? C6 C7 1.414(3) . ? C6 C11 1.383(3) . ? C7 C8 1.383(3) . ? C8 H8 0.9500 . ? C8 C9 1.400(3) . ? C9 C10 1.384(3) . ? C9 C12 1.494(3) . ? C10 C11 1.386(3) . ? C10 C13 1.492(3) . ? C11 H11 0.9500 . ? C14 C14 1.428(4) 4_575 ? C14 C15 1.529(2) . ? C15 H15 1.0000 . ? C15 C16 1.558(2) . ? C15 C17 1.521(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C17 1.416(4) 4_575 ? C17 C18 1.384(3) . ? C18 H18 0.9500 . ? C18 C19 1.386(3) . ? C19 C19 1.385(4) 4_575 ? C19 C20 1.491(3) . ? Cl3S C2S 1.744(8) 4_575 ? Cl3S C2S 1.744(8) . ? Cl4S Cl4S 1.551(7) 4_575 ? Cl4S C2S 1.356(9) 4_575 ? Cl4S C2S 1.758(8) . ? Cl4S H2SA 1.092(8) 4_575 ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? Cl1S C1S 1.775(5) . ? Cl2S C1S 1.769(4) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? Cl3B C2SB 1.763(6) . ? C2SB H2SC 0.9900 . ? C2SB H2SD 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 C12 N1 H1 122.5(19) . . ? C12 N1 C13 112.60(17) . . ? C13 N1 H1 124.5(19) . . ? C20 N2 H2 123.67(12) 4_575 . ? C20 N2 H2 123.67(12) . . ? C20 N2 C20 112.6(2) . 4_575 ? C1 C1 C2 120.41(10) 4_575 . ? C1 C1 C5 132.73(10) 4_575 . ? C2 C1 C5 106.49(15) . . ? C1 C2 C3 106.29(15) . . ? C14 C2 C1 119.24(17) . . ? C14 C2 C3 134.38(17) . . ? C2 C3 H3 117.3 . . ? C2 C3 C4 98.95(15) . . ? C2 C3 C7 103.82(14) . . ? C4 C3 H3 117.3 . . ? C7 C3 H3 117.3 . . ? C7 C3 C4 99.16(14) . . ? C3 C4 H4A 112.8 . . ? C3 C4 H4B 112.8 . . ? H4A C4 H4B 110.2 . . ? C5 C4 C3 94.68(14) . . ? C5 C4 H4A 112.8 . . ? C5 C4 H4B 112.8 . . ? C1 C5 C4 99.94(14) . . ? C1 C5 H5 117.1 . . ? C4 C5 H5 117.1 . . ? C6 C5 C1 102.90(14) . . ? C6 C5 C4 99.79(15) . . ? C6 C5 H5 117.1 . . ? C7 C6 C5 106.76(16) . . ? C11 C6 C5 130.56(18) . . ? C11 C6 C7 122.40(18) . . ? C6 C7 C3 106.49(16) . . ? C8 C7 C3 131.85(17) . . ? C8 C7 C6 121.52(17) . . ? C7 C8 H8 122.1 . . ? C7 C8 C9 115.75(18) . . ? C9 C8 H8 122.1 . . ? C8 C9 C12 130.09(19) . . ? C10 C9 C8 122.09(18) . . ? C10 C9 C12 107.77(17) . . ? C9 C10 C11 122.76(18) . . ? C9 C10 C13 108.45(18) . . ? C11 C10 C13 128.78(18) . . ? C6 C11 C10 115.45(18) . . ? C6 C11 H11 122.3 . . ? C10 C11 H11 122.3 . . ? O1 C12 N1 125.25(19) . . ? O1 C12 C9 128.84(19) . . ? N1 C12 C9 105.90(18) . . ? O2 C13 N1 125.44(19) . . ? O2 C13 C10 129.3(2) . . ? N1 C13 C10 105.25(17) . . ? C2 C14 C14 120.17(11) . 4_575 ? C2 C14 C15 133.53(17) . . ? C14 C14 C15 106.26(10) 4_575 . ? C14 C15 H15 116.8 . . ? C14 C15 C16 99.33(15) . . ? C16 C15 H15 116.8 . . ? C17 C15 C14 105.28(14) . . ? C17 C15 H15 116.8 . . ? C17 C15 C16 98.89(15) . . ? C15 C16 C15 94.24(19) 4_575 . ? C15 C16 H16A 112.9 4_575 . ? C15 C16 H16A 112.9 . . ? C15 C16 H16B 112.9 4_575 . ? C15 C16 H16B 112.9 . . ? H16A C16 H16B 110.3 . . ? C17 C17 C15 106.58(10) 4_575 . ? C18 C17 C15 131.49(17) . . ? C18 C17 C17 121.91(11) . 4_575 ? C17 C18 H18 122.3 . . ? C17 C18 C19 115.48(18) . . ? C19 C18 H18 122.3 . . ? C18 C19 C20 129.17(19) . . ? C19 C19 C18 122.61(11) 4_575 . ? C19 C19 C20 108.22(12) 4_575 . ? O3 C20 N2 125.79(18) . . ? O3 C20 C19 128.8(2) . . ? N2 C20 C19 105.46(18) . . ? C2S Cl3S C2S 26.7(5) 4_575 . ? Cl4S Cl4S C2S 47.9(3) 4_575 . ? Cl4S Cl4S H2SA 118.6(5) 4_575 4_575 ? C2S Cl4S Cl4S 74.0(4) 4_575 4_575 ? C2S Cl4S C2S 26.2(6) 4_575 . ? C2S Cl4S H2SA 71.6(8) . 4_575 ? C2S Cl4S H2SA 46.2(3) 4_575 4_575 ? Cl3S C2S Cl4S 111.5(5) . . ? Cl3S C2S H2SA 109.3 . . ? Cl3S C2S H2SB 109.3 . . ? Cl4S C2S H2SA 109.3 . . ? Cl4S C2S H2SB 109.3 . . ? H2SA C2S H2SB 108.0 . . ? Cl1S C1S H1SA 109.3 . . ? Cl1S C1S H1SB 109.3 . . ? Cl2S C1S Cl1S 111.56(19) . . ? Cl2S C1S H1SA 109.3 . . ? Cl2S C1S H1SB 109.3 . . ? H1SA C1S H1SB 108.0 . . ? Cl3B C2SB Cl3B 110.2(5) 4_575 . ? Cl3B C2SB H2SC 109.6 4_575 . ? Cl3B C2SB H2SC 109.6 . . ? Cl3B C2SB H2SD 109.6 4_575 . ? Cl3B C2SB H2SD 109.6 . . ? H2SC C2SB H2SD 108.1 . . ? 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 _geom_hbond_publ_flag N1 H1 O1 0.915(17) 2.025(18) 2.938(2) 176(3) 3_667 yes 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 C1 C2 C3 -171.98(9) 4_575 . . . ? C1 C1 C2 C14 4.9(2) 4_575 . . . ? C1 C1 C5 C4 -154.34(9) 4_575 . . . ? C1 C1 C5 C6 103.11(14) 4_575 . . . ? C1 C2 C3 C4 -35.73(17) . . . . ? C1 C2 C3 C7 66.09(17) . . . . ? C1 C2 C14 C14 -4.9(2) . . . 4_575 ? C1 C2 C14 C15 177.73(17) . . . . ? C1 C5 C6 C7 68.75(17) . . . . ? C1 C5 C6 C11 -105.1(2) . . . . ? C2 C1 C5 C4 32.86(18) . . . . ? C2 C1 C5 C6 -69.69(17) . . . . ? C2 C3 C4 C5 53.28(15) . . . . ? C2 C3 C7 C6 -67.34(17) . . . . ? C2 C3 C7 C8 108.4(2) . . . . ? C2 C14 C15 C16 -147.6(2) . . . . ? C2 C14 C15 C17 110.4(2) . . . . ? C3 C2 C14 C14 170.93(16) . . . 4_575 ? C3 C2 C14 C15 -6.4(3) . . . . ? C3 C4 C5 C1 -52.54(15) . . . . ? C3 C4 C5 C6 52.54(15) . . . . ? C3 C7 C8 C9 -174.07(18) . . . . ? C4 C3 C7 C6 34.32(17) . . . . ? C4 C3 C7 C8 -150.0(2) . . . . ? C4 C5 C6 C7 -33.91(17) . . . . ? C4 C5 C6 C11 152.24(19) . . . . ? C5 C1 C2 C3 1.89(18) . . . . ? C5 C1 C2 C14 178.80(15) . . . . ? C5 C6 C7 C3 -0.35(19) . . . . ? C5 C6 C7 C8 -176.61(17) . . . . ? C5 C6 C11 C10 174.15(18) . . . . ? C6 C7 C8 C9 1.1(3) . . . . ? C7 C3 C4 C5 -52.40(15) . . . . ? C7 C6 C11 C10 1.1(3) . . . . ? C7 C8 C9 C10 0.8(3) . . . . ? C7 C8 C9 C12 177.64(19) . . . . ? C8 C9 C10 C11 -1.8(3) . . . . ? C8 C9 C10 C13 176.90(17) . . . . ? C8 C9 C12 O1 1.2(4) . . . . ? C8 C9 C12 N1 -177.69(19) . . . . ? C9 C10 C11 C6 0.8(3) . . . . ? C9 C10 C13 O2 -178.1(2) . . . . ? C9 C10 C13 N1 1.4(2) . . . . ? C10 C9 C12 O1 178.4(2) . . . . ? C10 C9 C12 N1 -0.5(2) . . . . ? C11 C6 C7 C3 174.11(16) . . . . ? C11 C6 C7 C8 -2.1(3) . . . . ? C11 C10 C13 O2 0.5(4) . . . . ? C11 C10 C13 N1 -179.98(19) . . . . ? C12 N1 C13 O2 177.8(2) . . . . ? C12 N1 C13 C10 -1.8(2) . . . . ? C12 C9 C10 C11 -179.27(18) . . . . ? C12 C9 C10 C13 -0.6(2) . . . . ? C13 N1 C12 O1 -177.5(2) . . . . ? C13 N1 C12 C9 1.5(2) . . . . ? C13 C10 C11 C6 -177.63(18) . . . . ? C14 C2 C3 C4 148.0(2) . . . . ? C14 C2 C3 C7 -110.1(2) . . . . ? C14 C14 C15 C16 34.77(13) 4_575 . . . ? C14 C14 C15 C17 -67.19(13) 4_575 . . . ? C14 C15 C16 C15 -53.56(18) . . . 4_575 ? C14 C15 C17 C17 67.41(12) . . . 4_575 ? C14 C15 C17 C18 -111.0(2) . . . . ? C15 C17 C18 C19 178.27(17) . . . . ? C16 C15 C17 C17 -34.88(12) . . . 4_575 ? C16 C15 C17 C18 146.75(19) . . . . ? C17 C15 C16 C15 53.65(18) . . . 4_575 ? C17 C17 C18 C19 0.11(19) 4_575 . . . ? C17 C18 C19 C19 -0.1(2) . . . 4_575 ? C17 C18 C19 C20 -179.32(17) . . . . ? C18 C19 C20 O3 -0.7(3) . . . . ? C18 C19 C20 N2 179.0(2) . . . . ? C19 C19 C20 O3 179.97(18) 4_575 . . . ? C19 C19 C20 N2 -0.28(17) 4_575 . . . ? C20 N2 C20 O3 -179.76(13) 4_575 . . . ? C20 N2 C20 C19 0.5(3) 4_575 . . . ? Cl4S Cl4S C2S Cl3S -133.8(8) 4_575 . . . ? C2S Cl3S C2S Cl4S -33.4(6) 4_575 . . . ? C2S Cl4S C2S Cl3S 46.2(8) 4_575 . . . ? _shelx_res_file ; TITL badjic_trisnh_a.res in P2(1)/m badjic_trisnh.res created by SHELXL-2018/3 at 20:13:46 on 03-Jun-2021 REM Old TITL Badjic in P2(1)/m REM SHELXT solution in P2(1)/m: R1 0.179, Rweak 0.009, Alpha 0.038 REM 1.694 for 8 systematic absences, Orientation as input REM Formula found by SHELXT: C44 N O8 Cl3 CELL 0.71073 9.8486 14.6173 12.4874 90 102.991 90 ZERR 2 0.0007 0.001 0.0009 0 0.003 0 LATT 1 SYMM -X,0.5+Y,-Z SFAC C H Cl N O UNIT 82 50 8 6 12 EQIV $1 +X,1.5-Y,+Z EQIV $2 1-X,1-Y,2-Z DFIX 0.95 N1 H1 N2 H2 L.S. 10 0 0 PLAN 10 SIZE 0.243 0.226 0.118 TEMP -173.15 CONF HTAB N1 O1_$2 FREE C2S C2S_$1 FREE C2S Cl4S_$1 BOND list 4 MORE -1 BOND $H fmap 2 53 acta 50 REM REM REM WGHT 0.053500 1.478900 FVAR 0.49589 0.61987 O1 5 0.548770 0.466376 0.862766 11.00000 0.04271 0.03796 = 0.04284 -0.00511 0.02000 -0.00811 O2 5 0.835659 0.635800 1.128595 11.00000 0.06018 0.03270 = 0.03060 -0.00302 0.01771 -0.00102 O3 5 0.263127 0.593183 0.476637 11.00000 0.03119 0.04861 = 0.03516 -0.00682 0.01209 -0.01437 N1 4 0.671236 0.546443 1.013325 11.00000 0.04340 0.03489 = 0.03287 -0.00132 0.01933 -0.00058 H1 2 0.603759 0.545397 1.053068 11.00000 0.06412 N2 4 0.229429 0.750000 0.480844 10.50000 0.01969 0.05195 = 0.03197 0.00000 0.00830 0.00000 H2 2 0.139600 0.750000 0.492254 10.50000 0.05517 C1 1 1.079973 0.703453 0.706201 11.00000 0.02022 0.02686 = 0.02238 0.00144 0.00596 0.00198 C2 1 0.992276 0.654110 0.618931 11.00000 0.02037 0.02319 = 0.02324 -0.00058 0.00806 0.00127 C3 1 1.002856 0.553269 0.653460 11.00000 0.02604 0.02280 = 0.02332 0.00138 0.00725 0.00281 AFIX 13 H3 2 0.970946 0.506657 0.594562 11.00000 -1.20000 AFIX 0 C4 1 1.159213 0.550981 0.714522 11.00000 0.02719 0.02801 = 0.02444 0.00152 0.00608 0.00458 AFIX 23 H4A 2 1.185755 0.493198 0.755202 11.00000 -1.20000 H4B 2 1.222992 0.563575 0.665285 11.00000 -1.20000 AFIX 0 C5 1 1.147195 0.632735 0.791334 11.00000 0.02565 0.02686 = 0.02376 0.00094 0.00326 0.00422 AFIX 13 H5 2 1.233885 0.651515 0.845321 11.00000 -1.20000 AFIX 0 C6 1 1.025566 0.600087 0.837788 11.00000 0.02927 0.02104 = 0.02647 0.00387 0.00600 0.00527 C7 1 0.936038 0.550540 0.753208 11.00000 0.03129 0.02090 = 0.02430 0.00266 0.00834 0.00539 C8 1 0.810766 0.515249 0.766875 11.00000 0.03287 0.02070 = 0.02793 0.00056 0.00939 0.00012 AFIX 43 H8 2 0.750682 0.480977 0.710988 11.00000 -1.20000 AFIX 0 C9 1 0.778094 0.533236 0.868331 11.00000 0.03527 0.02347 = 0.03124 0.00417 0.01333 0.00273 C10 1 0.864912 0.584092 0.949218 11.00000 0.03971 0.02181 = 0.02568 0.00271 0.01033 0.00503 C11 1 0.991686 0.618740 0.937233 11.00000 0.03545 0.02440 = 0.02385 0.00211 0.00576 0.00520 AFIX 43 H11 2 1.051249 0.652964 0.993482 11.00000 -1.20000 AFIX 0 C12 1 0.651390 0.508876 0.909211 11.00000 0.04134 0.02668 = 0.03479 0.00162 0.01616 0.00050 C13 1 0.796236 0.594690 1.043543 11.00000 0.04458 0.02649 = 0.02961 0.00478 0.01370 0.00362 C14 1 0.915938 0.701169 0.530974 11.00000 0.01871 0.02573 = 0.02165 -0.00238 0.00703 -0.00021 C15 1 0.817132 0.671887 0.423742 11.00000 0.02081 0.02447 = 0.02124 -0.00213 0.00544 0.00023 AFIX 13 H15 2 0.826623 0.607721 0.398626 11.00000 -1.20000 AFIX 0 C16 1 0.846734 0.750000 0.347190 10.50000 0.02397 0.02960 = 0.02062 0.00000 0.00629 0.00000 AFIX 23 H16A 2 0.944096 0.750000 0.338244 10.50000 -1.20000 H16B 2 0.780957 0.749999 0.274454 10.50000 -1.20000 AFIX 0 C17 1 0.672925 0.701574 0.434899 11.00000 0.02224 0.02704 = 0.01751 -0.00089 0.00369 0.00080 C18 1 0.557695 0.651516 0.446298 11.00000 0.02430 0.02819 = 0.02278 -0.00220 0.00464 -0.00353 AFIX 43 H18 2 0.557177 0.586526 0.446477 11.00000 -1.20000 AFIX 0 C19 1 0.443097 0.702633 0.457435 11.00000 0.02154 0.03728 = 0.02189 -0.00095 0.00512 -0.00342 C20 1 0.304646 0.670736 0.472240 11.00000 0.02382 0.04731 = 0.02306 -0.00254 0.00633 -0.00520 PART 1 CL3S 3 0.725034 0.750000 0.724088 20.50000 0.03013 0.03355 = 0.03797 0.00000 0.01345 0.00000 CL4S 3 0.451982 0.696935 0.752286 20.50000 0.03746 0.08348 = 0.04261 -0.01053 0.01526 -0.02387 C2S 1 0.587389 0.777563 0.784998 20.50000 0.04140 0.05297 = 0.07946 -0.03034 0.03590 -0.01644 AFIX 23 H2SA 2 0.550956 0.838833 0.759631 20.50000 -1.20000 H2SB 2 0.621876 0.780125 0.865771 20.50000 -1.20000 AFIX 0 PART 0 CL1S 3 0.743901 0.250000 0.822593 10.50000 0.07151 0.06586 = 0.04544 0.00000 -0.01168 0.00000 CL2S 3 0.558671 0.250000 0.976379 10.50000 0.07732 0.05315 = 0.04157 0.00000 -0.00953 0.00000 C1S 1 0.568465 0.250000 0.836627 10.50000 0.07099 0.03649 = 0.04156 0.00000 -0.01648 0.00000 AFIX 23 H1SA 2 0.520187 0.304780 0.799837 10.50000 -1.20000 H1SB 2 0.520187 0.195220 0.799837 10.50000 -1.20000 AFIX 0 PART 2 CL3B 3 0.501247 0.651060 0.729967 -21.00000 0.03973 0.04835 = 0.04089 0.01114 0.00606 -0.00237 C2SB 1 0.603540 0.750000 0.729707 -20.50000 0.03188 0.04952 = 0.03511 0.00000 0.00181 0.00000 AFIX 23 H2SC 2 0.681520 0.750000 0.795436 -20.50000 -1.20000 H2SD 2 0.643452 0.750001 0.663677 -20.50000 -1.20000 AFIX 0 HKLF 4 REM badjic_trisnh_a.res in P2(1)/m REM wR2 = 0.1172, GooF = S = 1.027, Restrained GooF = 1.027 for all data REM R1 = 0.0421 for 3114 Fo > 4sig(Fo) and 0.0525 for all 3728 data REM 285 parameters refined using 2 restraints END WGHT 0.0535 1.4789 REM Highest difference peak 0.534, deepest hole -0.574, 1-sigma level 0.051 Q1 1 0.5230 0.7500 0.8757 10.50000 0.05 0.53 Q2 1 0.8444 0.2500 0.7908 10.50000 0.05 0.42 Q3 1 0.6589 0.2500 0.9470 10.50000 0.05 0.36 Q4 1 0.8731 0.6799 0.4841 11.00000 0.05 0.31 Q5 1 0.9631 0.5464 0.7018 11.00000 0.05 0.29 Q6 1 0.3815 0.6812 0.4597 11.00000 0.05 0.29 Q7 1 1.0906 0.6170 0.8247 11.00000 0.05 0.26 Q8 1 0.9084 0.7500 0.5404 10.50000 0.05 0.26 Q9 1 0.7439 0.6812 0.4323 11.00000 0.05 0.25 Q10 1 1.0802 0.5517 0.6737 11.00000 0.05 0.25 ; _shelx_res_checksum 67023 _shelx_hkl_file ; -2 0 0 9.04711 1.01073 6 2 0 0 11.6478 1.31007 2 2 0 0 8.96763 1.73547 3 2 0 0 12.1094 1.35888 6 -2 0 0 8.36302 1.72347 3 -2 0 0 8.82231 1.26156 2 3 0 0 704.072 15.6313 3 -3 0 0 726.460 14.6792 6 3 0 0 721.924 14.2510 6 -3 0 0 712.876 14.7245 2 -3 0 0 714.666 15.6688 3 3 0 0 703.917 14.6495 2 4 0 0 1334.73 25.2851 6 -4 0 0 1290.72 25.8981 2 -4 0 0 1287.33 27.1089 3 4 0 0 1244.71 27.0010 3 4 0 0 1303.75 25.8661 2 -4 0 0 1317.53 25.2214 6 -5 0 0 114.903 3.76031 6 5 0 0 104.486 5.23951 3 -5 0 0 108.119 6.19588 3 5 0 0 116.657 3.95415 6 5 0 0 111.665 4.34140 2 -5 0 0 113.084 4.43075 2 -6 0 0 147.137 7.17914 3 6 0 0 151.944 4.71401 6 6 0 0 145.470 6.52790 3 -6 0 0 158.269 5.55067 2 -6 0 0 149.610 4.52588 6 -7 0 0 348.266 9.34935 2 -7 0 0 339.490 8.28485 6 7 0 0 343.344 8.41612 6 7 0 0 341.419 10.8408 3 -8 0 0 92.4637 4.82184 2 -8 0 0 96.7822 3.68316 6 8 0 0 97.0981 3.94275 6 8 0 0 97.5366 6.04853 3 -9 0 0 66.5813 3.09293 6 9 0 0 64.3382 5.15231 3 9 0 0 65.6939 3.28136 6 -9 0 0 69.1135 4.17233 2 10 0 0 43.0267 2.72654 6 -10 0 0 38.5939 3.70508 2 10 0 0 40.8048 4.33433 3 11 0 0 105.689 6.66726 3 11 0 0 111.723 3.77985 6 -11 0 0 95.4871 5.04471 2 2 -1 0 729.300 14.3381 2 -2 -1 0 726.868 13.4967 6 -2 -1 0 719.278 14.3967 2 2 -1 0 728.681 14.7745 3 2 -1 0 713.674 14.3560 6 -2 -1 0 724.311 15.3105 3 -2 1 0 719.789 14.4096 6 2 1 0 721.384 14.3901 2 2 1 0 718.666 15.4054 3 2 1 0 695.036 13.4880 6 -2 1 0 701.508 15.3625 3 -2 1 0 711.266 14.2773 2 -3 -1 0 7.26889 1.42654 2 -3 -1 0 5.33351 1.91567 3 3 -1 0 7.47651 1.48131 2 -3 -1 0 6.33588 0.79352 6 3 -1 0 5.91107 1.83951 3 3 -1 0 5.55137 1.56621 6 -3 1 0 8.35110 1.89797 3 -3 1 0 4.25941 1.19438 6 -3 1 0 5.36948 1.33850 2 3 1 0 5.13774 2.02999 3 3 1 0 5.72230 0.83014 6 3 1 0 4.44450 1.33111 2 4 -1 0 68.9138 3.24448 2 -4 -1 0 72.1352 3.37540 2 4 -1 0 65.8469 3.82882 3 -4 -1 0 70.2288 4.36149 3 4 -1 0 75.2136 3.48730 6 4 1 0 72.2692 2.59653 6 -4 1 0 70.8543 3.11678 6 -4 1 0 69.7584 3.85651 3 4 1 0 70.3244 3.31402 2 4 1 0 67.2441 4.35279 3 -4 1 0 71.1041 3.33778 2 5 -1 0 1117.54 23.3374 2 -5 -1 0 1169.05 22.1968 6 -5 -1 0 1141.05 25.1422 3 5 -1 0 1103.85 24.6237 3 -5 -1 0 1105.91 23.4773 2 5 -1 0 1172.53 23.1669 6 5 1 0 1135.37 23.4669 2 -5 1 0 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10.1697 6 -2 -4 0 420.746 9.61211 4 -2 -4 0 423.686 8.69303 6 -2 -4 0 417.985 9.67317 2 2 -4 0 406.178 8.99648 4 -2 -4 0 416.575 9.39748 1 2 4 0 423.087 8.72715 6 -2 4 0 411.403 9.02125 3 2 4 0 420.262 9.62555 2 -2 4 0 422.183 9.40996 4 2 4 0 425.606 10.7025 3 -2 4 0 414.914 9.95807 6 -3 -4 0 50.5479 4.02041 3 3 -4 0 46.5543 2.65404 3 -3 -4 0 47.8482 2.99377 2 -3 -4 0 40.9273 3.00054 1 3 -4 0 45.7473 2.38497 4 3 -4 0 49.7914 3.50716 6 3 4 0 42.5566 3.85331 3 -3 4 0 44.2529 2.34239 4 3 4 0 48.9345 1.50550 6 3 4 0 49.3847 2.98104 2 -3 4 0 37.9851 3.12860 6 -3 4 0 40.3081 2.48886 3 -4 -4 0 20.8266 2.48651 2 -4 -4 0 26.2366 3.84125 3 4 -4 0 17.0158 2.60032 6 4 -4 0 20.2277 2.41278 3 4 -4 0 17.3167 2.45756 2 -4 4 0 15.1871 2.72454 6 4 4 0 23.6576 2.44260 2 -4 4 0 18.9553 1.99908 4 -4 4 0 18.3458 2.39574 3 4 4 0 19.8322 3.61827 3 5 -4 0 25.9751 2.74998 3 5 -4 0 28.7469 3.16315 6 5 -4 0 26.2323 2.42956 2 -5 -4 0 26.1473 3.00475 1 -5 -4 0 21.9577 2.55721 2 -5 4 0 29.3641 2.13913 4 5 4 0 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6 -3 -2 14 27.1630 2.95969 4 3 -2 -14 16.3251 3.11004 1 3 2 -14 19.6997 3.33469 1 -3 2 14 14.3241 2.51070 4 2 -2 -14 19.2575 3.12473 6 -2 -2 14 21.0028 2.46883 4 2 -2 -14 14.4468 2.87764 1 2 2 -14 15.7618 3.17898 1 -1 -2 14 8.26160 1.82036 4 1 -2 -14 8.84579 2.43199 6 1 -2 -14 6.62354 2.36623 1 -1 2 14 9.67918 2.15514 4 1 2 -14 9.32798 2.68711 1 0 -2 14 22.7081 2.36033 4 0 -2 -14 16.3536 2.86223 1 0 2 -14 14.5529 3.13126 1 0 2 14 21.3459 2.55443 4 -1 -2 -14 18.8550 3.02104 1 1 -2 14 22.5975 2.11387 4 -1 2 -14 24.4200 3.49300 1 1 2 14 22.6134 2.43373 4 -2 -2 -14 0.56579 1.84142 1 2 -2 14 0.98685 1.05159 4 -2 2 -14 -0.5903 1.93217 1 2 2 14 1.13633 1.38578 4 -7 -3 14 26.0022 3.46287 4 7 -3 -14 19.7252 3.34548 6 7 -3 -14 16.4721 3.17857 1 7 3 -14 14.3296 3.32996 1 7 3 -14 24.2944 3.41852 6 -7 3 14 18.5189 2.94989 4 -6 -3 14 66.8488 4.29669 4 6 -3 -14 63.5717 5.05110 1 6 -3 -14 65.6039 5.09158 6 6 3 -14 58.5402 5.28379 1 -6 3 14 70.6299 4.56465 4 5 -3 -14 1.07217 2.59568 1 -5 -3 14 6.73162 2.05841 4 5 -3 -14 7.42315 2.54365 6 5 3 -14 5.02294 2.66762 1 -5 3 14 6.32383 2.07091 4 4 -3 -14 8.90528 2.56557 6 4 -3 -14 6.47263 2.52568 1 -4 -3 14 8.73339 2.12473 4 4 3 -14 5.27259 2.55601 1 -4 3 14 5.12137 2.12904 4 -3 -3 14 1.96883 1.79854 4 3 -3 -14 1.12823 2.16821 1 3 -3 -14 -0.6244 2.06253 6 3 3 -14 3.16363 2.53419 1 -3 3 14 2.60367 1.80215 4 -2 -3 14 2.88084 1.71837 4 2 -3 -14 3.91133 2.13642 6 2 -3 -14 -0.6743 2.20804 1 -2 3 14 -0.3056 1.42739 4 2 3 -14 0.83125 2.12277 1 1 -3 -14 10.2936 2.57712 1 1 -3 -14 10.5498 1.13439 2 1 -3 -14 10.1960 2.58687 6 -1 -3 14 11.4316 1.99835 4 -1 3 14 12.3665 2.59507 4 1 3 -14 11.0019 2.88891 1 0 -3 -14 8.50405 2.49747 1 0 -3 -14 11.8149 2.74512 6 0 -3 14 6.61286 1.55525 4 0 3 14 9.10320 1.91249 4 0 3 -14 9.82651 2.77475 1 -1 -3 -14 119.795 6.32284 1 -1 -3 -14 123.180 6.24033 6 1 3 14 127.288 4.96855 4 -1 3 -14 120.037 6.58732 1 -2 -3 -14 0.91566 1.76438 6 -2 -3 -14 -0.7909 1.70630 1 2 3 14 2.63865 1.39902 4 -2 3 -14 2.99113 2.22741 1 -7 -4 14 4.12875 1.62909 2 7 -4 -14 3.43436 2.27702 6 -7 -4 14 5.55244 2.18376 4 7 -4 -14 3.77321 2.45802 1 7 4 -14 3.48271 2.78741 1 -7 4 14 5.26705 2.03841 4 7 4 -14 4.58505 2.04627 6 6 -4 -14 0.26110 2.07832 6 -6 -4 14 -0.3822 1.65481 4 6 -4 -14 -2.2935 2.20729 1 -6 4 14 0.73216 1.86863 4 6 4 -14 0.49009 2.50814 1 -5 -4 14 -1.7404 1.39451 4 5 -4 -14 2.98784 2.24558 6 -5 4 14 -3.5137 1.57019 4 5 4 -14 -0.2651 2.29078 1 -4 -4 14 -0.4117 1.43352 4 4 -4 -14 -0.8877 2.32823 1 4 -4 -14 1.74895 2.08710 6 -4 4 14 -0.4592 1.81874 4 4 4 -14 -1.0352 2.26514 1 3 -4 -14 55.7323 4.58743 6 -3 -4 14 49.6910 3.55806 4 3 -4 -14 46.6144 4.21738 1 3 4 -14 46.1455 5.08946 1 -3 4 14 54.8615 3.79590 4 -2 -4 14 43.0212 3.13654 4 2 -4 -14 41.8784 4.14050 6 2 -4 -14 40.8299 4.30749 1 2 4 -14 30.8449 3.86767 1 -2 4 14 38.5982 3.20445 4 -1 -4 14 0.77546 1.39972 4 1 -4 -14 -0.6857 1.94691 6 1 -4 -14 -1.6225 0.79335 2 1 -4 -14 -3.8856 1.69057 1 -1 4 14 3.44810 1.82106 4 1 4 -14 -3.3172 1.81175 1 0 -4 14 0.87911 1.33538 4 0 -4 -14 1.16427 1.81276 1 0 -4 -14 -1.1771 1.68333 6 0 4 -14 1.57430 2.14942 1 -1 -4 -14 0.60756 1.80643 6 -1 -4 -14 0.34659 1.69702 1 1 -4 14 0.25315 1.00847 4 -1 4 -14 -0.1267 1.94542 1 1 4 14 -1.1976 1.32446 4 -2 -4 -14 5.40126 2.02517 6 -2 -4 -14 4.68693 2.22431 1 -2 4 -14 2.02946 2.41423 1 2 4 14 3.49824 1.62947 4 -6 -5 14 1.31256 1.48710 2 -6 -5 14 1.51551 2.09455 4 6 -5 -14 -1.7317 2.09324 1 6 -5 -14 3.79092 2.23036 6 6 5 -14 -0.3363 2.37434 1 -6 5 14 2.35627 1.92799 4 5 -5 -14 4.62724 2.55812 1 5 -5 -14 6.51473 2.43296 6 -5 -5 14 8.00858 2.21243 4 -5 -5 14 14.1725 1.92023 2 -5 5 14 9.37769 2.35317 4 5 5 -14 14.0761 3.28837 1 -4 -5 14 -0.2083 1.44976 4 4 -5 -14 -0.5393 2.13358 6 4 -5 -14 -0.9892 1.92852 1 -4 5 14 2.09189 2.11246 4 4 5 -14 -1.5128 2.26643 1 3 -5 -14 2.36829 2.07271 6 -3 -5 14 4.31709 1.79099 4 3 -5 -14 1.72539 2.34969 1 -3 5 14 1.38662 1.66284 4 3 5 -14 2.18342 2.44786 1 -2 -5 14 36.2696 2.88961 4 2 -5 -14 47.7424 4.26334 6 2 -5 -14 29.9091 3.55107 1 -2 5 14 42.2203 3.43478 4 2 5 -14 33.9556 4.03219 1 -1 -5 14 10.9490 1.90710 4 1 -5 -14 10.1247 1.43393 2 1 -5 -14 10.7060 2.55214 1 1 -5 -14 14.3788 2.78316 6 -1 5 14 16.3015 2.49691 4 1 5 -14 10.8808 2.85593 1 0 -5 -14 22.4342 1.74470 2 0 -5 14 21.8167 2.11714 4 0 -5 -14 18.2171 2.76437 1 0 -5 -14 19.5112 3.02220 6 0 5 14 18.9099 2.40352 4 0 5 -14 19.5299 3.24842 1 -1 -5 -14 -1.2111 1.63630 6 1 -5 14 1.54273 1.57403 4 -1 -5 -14 2.51632 2.06494 1 1 5 14 -2.0366 1.29083 4 -1 5 -14 0.06392 2.18452 1 -6 -6 14 -0.8673 1.53647 4 -6 -6 14 -2.4725 1.24512 2 -6 6 14 1.57223 1.83909 4 5 -6 -14 -1.8933 2.05962 1 5 -6 -14 0.32023 1.95160 6 -5 -6 14 0.41970 1.40094 2 -5 -6 14 1.17217 1.71560 4 5 6 -14 0.27836 2.47581 1 -5 6 14 0.55756 1.86661 4 -4 -6 14 8.40141 2.14572 4 4 -6 -14 10.8296 2.75505 6 -4 -6 14 8.94242 1.43952 2 4 -6 -14 1.46775 2.28849 1 -4 6 14 9.93209 2.48034 4 4 6 -14 7.35488 2.86965 1 -3 -6 14 62.7140 3.71913 4 3 -6 -14 62.2661 4.82541 6 3 6 -14 55.1968 5.10583 1 -3 6 14 55.9685 3.98060 4 2 -6 -14 -2.7364 1.80027 6 -2 -6 14 2.15837 1.45829 4 2 -6 -14 -1.2259 2.18793 1 2 6 -14 -3.3189 2.02201 1 -2 6 14 -0.6354 1.77367 4 -1 -6 14 13.2754 1.97184 4 1 -6 -14 9.78554 2.31411 1 1 -6 -14 10.8086 1.57386 2 1 -6 -14 12.3288 2.73182 6 1 6 -14 12.2804 2.85288 1 -1 6 14 12.1983 2.56704 4 0 -6 -14 7.40034 1.33101 2 0 -6 -14 7.69055 2.14666 1 0 -6 -14 10.9978 2.54751 6 0 -6 14 6.90056 1.42534 4 0 6 14 7.74991 2.04484 4 0 6 -14 6.86310 2.52489 1 -1 -6 -14 12.1434 2.59720 6 -1 -6 -14 8.91440 2.45714 1 1 6 14 12.3613 2.35695 4 -5 -7 14 14.0710 1.82924 2 5 -7 -14 4.59333 2.78482 6 5 7 -14 9.60009 3.41041 1 -5 7 14 13.0504 2.52309 4 4 -7 -14 -5.7774 1.87670 1 -4 -7 14 1.32637 1.20846 2 -4 -7 14 2.00646 1.82371 4 4 -7 -14 0.61070 2.02879 6 -4 7 14 -0.2985 1.84087 4 4 7 -14 -2.1896 2.35041 1 3 -7 -14 5.60694 2.33164 1 3 -7 -14 10.8238 2.70463 6 -3 7 14 8.87198 2.32507 4 3 7 -14 5.49538 2.76058 1 -2 -7 14 13.0970 2.04739 4 2 -7 -14 14.5623 2.82674 6 -2 7 14 10.9496 2.39125 4 2 7 -14 12.7035 3.08945 1 1 -7 -14 -1.2452 1.65117 1 -1 -7 14 -2.2629 1.18883 4 1 -7 -14 1.29069 1.90481 6 1 -7 -14 1.49276 1.19153 2 1 7 -14 -1.5688 1.99293 1 -1 7 14 -1.8063 1.59152 4 0 -7 -14 -1.2909 1.80261 1 0 -7 14 0.57460 1.16475 4 0 -7 -14 -1.8759 0.96485 2 0 -7 -14 -0.5770 1.68177 6 0 7 14 0.63970 1.59826 4 0 7 -14 -3.9254 1.99998 1 3 -8 -14 -0.8067 1.94706 6 -3 -8 14 1.01021 1.59420 4 -3 8 14 1.14455 1.82005 4 2 -8 -14 11.4956 2.41057 1 2 -8 -14 11.7310 2.67373 6 -2 -8 14 15.3417 2.08797 4 2 8 -14 11.8937 2.94755 1 -2 8 14 12.4585 2.39592 4 5 0 -15 5.13808 2.37158 6 -5 0 15 7.40348 2.20797 4 5 0 -15 4.11629 2.66529 1 -4 0 15 0.22460 1.53402 4 4 0 -15 2.42079 2.06401 6 4 0 -15 -1.2086 2.28919 1 -3 0 15 34.4520 3.09970 4 3 0 -15 27.3071 3.70338 1 -2 0 15 84.2384 5.01362 4 2 0 -15 76.4835 5.72066 1 1 0 -15 -0.3769 2.40868 1 -1 0 15 2.84615 1.49049 4 0 0 15 3.94843 1.52490 4 0 0 -15 5.58119 2.41472 1 -5 -1 15 24.6766 3.00843 4 5 -1 -15 20.7856 3.69782 1 5 -1 -15 28.0627 3.86779 6 5 1 -15 18.8763 3.29790 6 5 1 -15 19.7968 3.72882 1 -5 1 15 27.3800 3.13420 4 4 -1 -15 5.45276 2.38642 6 -4 -1 15 5.05402 1.84733 4 4 -1 -15 2.12299 2.36178 1 -4 1 15 4.42622 1.90798 4 4 1 -15 -0.2421 2.44717 1 -3 -1 15 15.9773 2.50350 4 3 -1 -15 17.8401 3.10789 6 3 -1 -15 12.8348 2.91027 1 3 1 -15 15.7252 3.16725 1 -3 1 15 17.0465 2.47156 4 2 -1 -15 24.0831 3.45847 6 2 -1 -15 23.0094 3.43659 1 2 1 -15 19.5282 3.51054 1 -2 1 15 28.6205 2.78143 4 1 -1 -15 -2.8980 2.09212 1 -1 -1 15 3.47905 1.48561 4 1 1 -15 -1.3956 2.37813 1 -1 1 15 -2.0886 1.42624 4 0 -1 15 0.46204 1.23876 4 0 -1 -15 -1.2089 1.79444 1 0 1 -15 -1.1448 2.02535 1 0 1 15 1.11536 1.45179 4 5 -2 -15 0.89328 1.95892 6 5 -2 -15 -5.2311 2.00644 1 5 2 -15 -1.9360 2.29241 1 -5 2 15 1.40276 1.73145 4 5 2 -15 -2.3782 1.55724 6 4 -2 -15 -0.8877 2.00385 6 -4 -2 15 1.19308 1.76456 4 4 -2 -15 1.22871 2.57849 1 4 2 -15 4.26482 2.68314 1 -4 2 15 -0.5275 1.52946 4 -3 -2 15 1.20759 1.56974 4 3 -2 -15 1.98249 2.17849 6 3 -2 -15 3.52518 2.32559 1 3 2 -15 -0.9894 2.11295 1 -3 2 15 2.21108 1.60109 4 -2 -2 15 0.54908 1.51564 4 2 -2 -15 5.07644 2.41747 1 2 -2 -15 1.57900 2.00848 6 -2 2 15 -0.5884 1.53281 4 2 2 -15 2.27712 2.34228 1 1 -2 -15 9.42263 2.59988 6 -1 -2 15 12.3559 1.98936 4 1 -2 -15 17.1464 3.10579 1 -1 2 15 11.2176 2.13499 4 1 2 -15 10.2373 2.85995 1 0 -2 15 -0.9928 1.22156 4 0 -2 -15 1.23080 1.72705 6 0 -2 -15 0.04915 1.89931 1 0 2 -15 -1.2701 1.93596 1 0 2 15 0.92937 1.37950 4 5 -3 -15 120.205 6.62877 6 -5 -3 15 122.472 5.70651 4 5 -3 -15 128.325 6.85762 1 -5 3 15 129.317 6.00433 4 5 3 -15 114.620 6.73256 1 -4 -3 15 -1.2720 1.70047 4 4 -3 -15 1.82279 2.17516 6 4 -3 -15 -1.1299 2.48998 1 -4 3 15 6.54882 1.98214 4 4 3 -15 2.29503 2.62281 1 3 -3 -15 18.5812 3.26224 6 -3 -3 15 18.8834 2.55062 4 3 -3 -15 10.6042 2.89935 1 -3 3 15 15.0469 2.39143 4 3 3 -15 12.5369 3.06328 1 2 -3 -15 7.05021 2.48678 1 2 -3 -15 8.63507 2.61810 6 -2 -3 15 10.0702 2.00348 4 2 3 -15 7.97480 2.79812 1 -2 3 15 9.59255 2.26688 4 -1 -3 15 4.51838 1.51967 4 1 -3 -15 4.19604 2.40323 1 1 -3 -15 5.92312 2.28934 6 1 3 -15 4.29611 2.36018 1 -1 3 15 1.23675 1.56873 4 0 -3 -15 4.52816 1.94642 6 4 -4 -15 9.58572 2.64403 6 4 -4 -15 3.16072 2.59433 1 -4 -4 15 10.5777 2.09009 4 -4 4 15 5.30252 2.03938 4 4 4 -15 7.52987 2.80612 1 3 -4 -15 4.35964 2.51257 1 3 -4 -15 10.1612 2.60779 6 -3 -4 15 9.96997 2.06004 4 -3 4 15 8.14554 2.26951 4 3 4 -15 11.6791 3.06283 1 2 -4 -15 -1.9925 1.68570 6 2 -4 -15 -4.1451 1.92892 1 -2 -4 15 -1.8581 1.29217 4 2 4 -15 -1.5912 2.17980 1 -2 4 15 -1.8796 1.42756 4 -1 -4 15 -0.1710 1.26244 4 1 -4 -15 -1.5777 1.74094 1 -1 4 15 0.88798 1.65373 4 1 4 -15 -0.8168 2.01035 1 3 -5 -15 43.1278 4.40911 6 -3 -5 15 47.6202 3.37352 4 -3 5 15 45.8410 3.60873 4 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.0452 _exptl_absorpt_correction_T_min 0.0251 _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 0.71083 9.847 14.620 12.482 90.002 102.963 89.989 ) ; _shelx_hkl_checksum 45360 _olex2_submission_special_instructions 'No special instructions were received'