data_ninme2 _audit_creation_date 2018-12-03 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _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. Kratzert, D., Holstein, J.J. & Krossing, I. (2015). J. Appl. Cryst. 48, 933-938. 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 'C22 H32 Fe N3 Ni O3 S2, B F4' _chemical_formula_sum 'C22 H32 B F4 Fe N3 Ni O3 S2' _chemical_formula_weight 651.99 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.8354(7) _cell_length_b 9.9750(4) _cell_length_c 13.3013(5) _cell_angle_alpha 90 _cell_angle_beta 100.622(2) _cell_angle_gamma 90 _cell_volume 2586.67(17) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9933 _cell_measurement_temperature 100 _cell_measurement_theta_max 67.251 _cell_measurement_theta_min 5.579 _shelx_estimated_absorpt_T_max 0.765 _shelx_estimated_absorpt_T_min 0.223 _exptl_absorpt_coefficient_mu 7.448 _exptl_absorpt_correction_T_max 0.7529 _exptl_absorpt_correction_T_min 0.3285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1617 before and 0.0944 after correction. The Ratio of minimum to maximum transmission is 0.4363. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1344 _exptl_crystal_size_max 0.288 _exptl_crystal_size_mid 0.208 _exptl_crystal_size_min 0.038 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_av_unetI/netI 0.0391 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 30203 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 67.284 _diffrn_reflns_theta_max 67.284 _diffrn_reflns_theta_min 2.266 _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker CMOS area detector' _diffrn_detector_area_resol_mean 10.5 _diffrn_detector_type 'CMOS area detector' _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker CMOS area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_target Mo _diffrn_source_type 'Incoatec I\ms' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4176 _reflns_number_total 4592 _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 V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.164 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.107 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 423 _refine_ls_number_reflns 4592 _refine_ls_number_restraints 173 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0607 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+10.8049P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1529 _refine_ls_wR_factor_ref 0.1580 _refine_special_details ; Disorder was found for the cp ring. Two partial occupancy orientations were identified of ca. 59 and 41% occupancy, their geometries were restrained) to similar structures employing SADI/SIMU/DELU, and the non-hydrogen atoms of the major occupancy orientation were refined anisotropically to convergence. Disorder was found for the BF4 anion. Two partial occupancy orientations for the BF4 anion were refined to ca. 75 and 25% occupancy, their geometries and displacement parameters were restrained to similar structures employing SADI/SIMU/DELU and the non-hydrogen atoms were refined anisotropically to convergence. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid bond restraints C1A_1, C2A_1, C3A_1, C4A_1, C5A_1 C1A_2, C2A_2, C3A_2, C4A_2, C5A_2 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005 B1_3, F1_3, F2_3, F3_3, F4_3 B1_4, F1_4, F2_4, F3_4, F4_4 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 3. Uiso/Uaniso restraints and constraints C1A_1 \\sim C2A_1 \\sim C3A_1 \\sim C4A_1 \\sim C5A_1 \\sim C1A_2 \\sim C2A_2 \\sim C3A_2 \\sim C4A_2 \\sim C5A_2: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 B1_3 \\sim F1_3 \\sim F2_3 \\sim F3_3 \\sim F4_3 \\sim B1_4 \\sim F1_4 \\sim F2_4 \\sim F3_4 \\sim F4_4: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(B1_3) = Uanis(B1_4) 4. Same fragment restrains {C1A_2, C2A_2, C3A_2, C4A_2, C5A_2} as {C1A_1, C2A_1, C3A_1, C4A_1, C5A_1} sigma for 1-2: 0.005 1-3: 0.04 {B1_4, F1_4, F2_4, F3_4, F4_4} as {B1_3, F1_3, F2_3, F3_3, F4_3} sigma for 1-2: 0.001 1-3: 0.04 5. Others Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)= Sof(C5A)=Sof(H5A)=1-FVAR(1) Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)= Sof(C5A)=Sof(H5A)=FVAR(1) Sof(B1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=1-FVAR(2) Sof(B1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(2) 6.a Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B) 6.b Aromatic/amide H refined with riding coordinates: C11(H11), C12(H12), C14(H14), C15(H15), C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A) 6.c Idealised Me refined as rotating group: C2(H2A,H2B,H2C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.69624(3) 0.77178(7) 0.26734(5) 0.0210(2) Uani 1 1 d . . . . . Fe1 Fe 0.82718(4) 0.64182(7) 0.44046(5) 0.0284(2) Uani 1 1 d . . . . . S1 S 0.76514(6) 0.60331(12) 0.28303(9) 0.0295(3) Uani 1 1 d . . . . . S2 S 0.83613(5) 0.84327(10) 0.38298(7) 0.0201(2) Uani 1 1 d . . . . . O1 O 0.7116(2) 0.7097(4) 0.5365(3) 0.0437(9) Uani 1 1 d . . . . . O2 O 0.76774(14) 0.8907(3) 0.3192(2) 0.0229(6) Uani 1 1 d . . . . . O3 O 0.89274(16) 0.8622(3) 0.3276(2) 0.0294(7) Uani 1 1 d . . . . . N1 N 0.62655(17) 0.9117(4) 0.2437(3) 0.0236(8) Uani 1 1 d . . . . . N2 N 0.61914(19) 0.6581(4) 0.2279(3) 0.0273(8) Uani 1 1 d . . . . . N3 N 0.8857(3) 1.2482(4) 0.7177(3) 0.0468(12) Uani 1 1 d . . . . . C1 C 0.7565(3) 0.6841(5) 0.4964(3) 0.0328(11) Uani 1 1 d . . . . . C2 C 0.6525(2) 1.0505(5) 0.2343(4) 0.0326(11) Uani 1 1 d . . . . . H2A H 0.677978 1.080147 0.300831 0.049 Uiso 1 1 calc GR . . . . H2B H 0.613646 1.111002 0.212089 0.049 Uiso 1 1 calc GR . . . . H2C H 0.682812 1.051725 0.183961 0.049 Uiso 1 1 calc GR . . . . C3 C 0.5889(2) 0.9087(6) 0.3313(3) 0.0307(10) Uani 1 1 d . . . . . H3A H 0.559324 0.989061 0.328254 0.037 Uiso 1 1 calc R . . . . H3B H 0.622386 0.911669 0.396358 0.037 Uiso 1 1 calc R . . . . C4 C 0.5450(2) 0.7839(6) 0.3294(4) 0.0371(12) Uani 1 1 d . . . . . H4A H 0.527226 0.779431 0.394224 0.045 Uiso 1 1 calc R . . . . H4B H 0.505016 0.792460 0.272951 0.045 Uiso 1 1 calc R . . . . C5 C 0.5814(3) 0.6541(6) 0.3161(4) 0.0351(12) Uani 1 1 d . . . . . H5A H 0.614357 0.634326 0.379759 0.042 Uiso 1 1 calc R . . . . H5B H 0.547312 0.580536 0.304905 0.042 Uiso 1 1 calc R . . . . C6 C 0.5804(2) 0.8748(5) 0.1453(3) 0.0309(11) Uani 1 1 d . . . . . H6A H 0.598996 0.911729 0.086894 0.037 Uiso 1 1 calc R . . . . H6B H 0.534249 0.913562 0.143493 0.037 Uiso 1 1 calc R . . . . C7 C 0.5751(2) 0.7218(6) 0.1361(3) 0.0331(11) Uani 1 1 d . . . . . H7A H 0.526810 0.693659 0.131725 0.040 Uiso 1 1 calc R . . . . H7B H 0.590544 0.692127 0.072975 0.040 Uiso 1 1 calc R . . . . C8 C 0.6396(3) 0.5196(6) 0.2032(4) 0.0404(12) Uani 1 1 d . . . . . H8A H 0.652855 0.518471 0.135013 0.049 Uiso 1 1 calc R . . . . H8B H 0.600595 0.457357 0.201850 0.049 Uiso 1 1 calc R . . . . C9 C 0.6997(3) 0.4755(5) 0.2840(5) 0.0439(13) Uani 1 1 d . . . . . H9A H 0.716577 0.386431 0.267083 0.053 Uiso 1 1 calc R . . . . H9B H 0.686231 0.470478 0.352034 0.053 Uiso 1 1 calc R . . . . C10 C 0.8485(2) 0.9657(4) 0.4816(3) 0.0223(9) Uani 1 1 d . . . . . C11 C 0.7943(2) 1.0324(4) 0.5119(3) 0.0256(9) Uani 1 1 d . . . . . H11 H 0.748590 1.012912 0.479612 0.031 Uiso 1 1 calc R . . . . C12 C 0.8064(3) 1.1261(5) 0.5881(4) 0.0335(11) Uani 1 1 d . . . . . H12 H 0.768620 1.172265 0.606571 0.040 Uiso 1 1 calc R . . . . C13 C 0.8735(3) 1.1564(5) 0.6404(3) 0.0322(11) Uani 1 1 d . . . . . C14 C 0.9277(3) 1.0870(5) 0.6078(4) 0.0406(13) Uani 1 1 d . . . . . H14 H 0.973637 1.105101 0.639812 0.049 Uiso 1 1 calc R . . . . C15 C 0.9151(2) 0.9938(5) 0.5306(4) 0.0360(12) Uani 1 1 d . . . . . H15 H 0.952451 0.947989 0.510481 0.043 Uiso 1 1 calc R . . . . C16 C 0.8298(4) 1.3132(8) 0.7535(6) 0.092(3) Uani 1 1 d . . . . . H16A H 0.795811 1.343198 0.694762 0.139 Uiso 1 1 calc GR . . . . H16B H 0.847250 1.390757 0.795615 0.139 Uiso 1 1 calc GR . . . . H16C H 0.808408 1.249982 0.794391 0.139 Uiso 1 1 calc GR . . . . C17 C 0.9539(4) 1.2955(7) 0.7574(5) 0.067(2) Uani 1 1 d . . . . . H17A H 0.982938 1.219717 0.785159 0.101 Uiso 1 1 calc GR . . . . H17B H 0.952301 1.361057 0.811726 0.101 Uiso 1 1 calc GR . . . . H17C H 0.972990 1.337803 0.702296 0.101 Uiso 1 1 calc GR . . . . B1_3 B 0.6129(5) 1.2842(8) 0.4721(8) 0.0413(7) Uani 0.742(9) 1 d D U P A 1 F1_3 F 0.6365(3) 1.1560(5) 0.4991(4) 0.0503(10) Uani 0.742(9) 1 d D U P A 1 F2_3 F 0.5910(7) 1.2934(11) 0.3693(5) 0.0398(9) Uani 0.742(9) 1 d D U P A 1 F3_3 F 0.5599(3) 1.3182(6) 0.5239(4) 0.0445(9) Uani 0.742(9) 1 d D U P A 1 F4_3 F 0.6671(3) 1.3770(6) 0.5034(4) 0.0431(9) Uani 0.742(9) 1 d D U P A 1 B1_4 B 0.6101(7) 1.2838(12) 0.4789(13) 0.0413(7) Uani 0.258(9) 1 d D U P A 2 F1_4 F 0.6000(8) 1.1534(12) 0.5087(9) 0.0449(11) Uani 0.258(9) 1 d D U P A 2 F2_4 F 0.6743(6) 1.3299(17) 0.5164(13) 0.0429(12) Uani 0.258(9) 1 d D U P A 2 F3_4 F 0.5579(7) 1.3622(15) 0.5067(12) 0.0407(11) Uani 0.258(9) 1 d D U P A 2 F4_4 F 0.593(2) 1.280(3) 0.3704(12) 0.0410(11) Uani 0.258(9) 1 d D U P A 2 C1A_1 C 0.9225(6) 0.5622(13) 0.4137(8) 0.050(2) Uani 0.591(15) 1 d D U P B 1 H1A_1 H 0.942536 0.581862 0.355836 0.060 Uiso 0.591(15) 1 calc R . P B 1 C2A_1 C 0.9302(9) 0.6294(19) 0.5073(9) 0.043(2) Uani 0.591(15) 1 d D U P B 1 H2A_1 H 0.960015 0.703982 0.523711 0.051 Uiso 0.591(15) 1 calc R . P B 1 C3A_1 C 0.8905(6) 0.5776(11) 0.5746(8) 0.040(2) Uani 0.591(15) 1 d D U P B 1 H3A_1 H 0.888049 0.608188 0.641454 0.048 Uiso 0.591(15) 1 calc R . P B 1 C4A_1 C 0.8520(7) 0.4607(15) 0.5164(9) 0.047(3) Uani 0.591(15) 1 d D U P B 1 H4A_1 H 0.818609 0.403067 0.536139 0.056 Uiso 0.591(15) 1 calc R . P B 1 C5A_1 C 0.8785(6) 0.4607(11) 0.4270(9) 0.052(3) Uani 0.591(15) 1 d D U P B 1 H5A_1 H 0.866602 0.392738 0.376830 0.063 Uiso 0.591(15) 1 calc R . P B 1 C1A_2 C 0.8563(8) 0.5248(14) 0.5774(11) 0.050(3) Uani 0.409(15) 1 d D U P B 2 H1A_2 H 0.826940 0.509056 0.625116 0.060 Uiso 0.409(15) 1 calc R . P B 2 C2A_2 C 0.9028(9) 0.6289(15) 0.5738(14) 0.049(3) Uani 0.409(15) 1 d D U P B 2 H2A_2 H 0.912202 0.695442 0.625566 0.059 Uiso 0.409(15) 1 calc R . P B 2 C3A_2 C 0.9345(13) 0.628(2) 0.4882(15) 0.045(3) Uani 0.409(15) 1 d D U P B 2 H3A_2 H 0.966831 0.690211 0.471061 0.054 Uiso 0.409(15) 1 calc R . P B 2 C4A_2 C 0.9052(8) 0.5040(16) 0.4288(11) 0.042(3) Uani 0.409(15) 1 d D U P B 2 H4A_2 H 0.912793 0.471420 0.364713 0.050 Uiso 0.409(15) 1 calc R . P B 2 C5A_2 C 0.8644(10) 0.4515(18) 0.4933(13) 0.045(3) Uani 0.409(15) 1 d D U P B 2 H5A_2 H 0.842614 0.366889 0.479611 0.054 Uiso 0.409(15) 1 calc R . P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0158(4) 0.0310(4) 0.0140(4) -0.0043(3) -0.0028(3) -0.0003(3) Fe1 0.0343(4) 0.0227(4) 0.0237(4) -0.0001(3) -0.0068(3) 0.0050(3) S1 0.0267(6) 0.0312(6) 0.0280(6) -0.0101(5) -0.0020(4) 0.0026(4) S2 0.0170(5) 0.0254(5) 0.0148(5) -0.0005(4) -0.0046(4) 0.0020(4) O1 0.059(2) 0.053(2) 0.0223(18) -0.0074(16) 0.0152(17) -0.0167(19) O2 0.0198(15) 0.0264(15) 0.0189(15) 0.0002(12) -0.0057(12) 0.0005(12) O3 0.0231(16) 0.0414(19) 0.0231(16) -0.0017(14) 0.0024(13) 0.0003(13) N1 0.0168(17) 0.039(2) 0.0125(17) 0.0003(15) -0.0041(13) 0.0017(15) N2 0.0238(19) 0.039(2) 0.0170(18) -0.0059(16) -0.0010(15) -0.0058(16) N3 0.078(4) 0.030(2) 0.031(2) -0.0105(19) 0.005(2) -0.004(2) C1 0.054(3) 0.028(2) 0.017(2) 0.0021(19) 0.005(2) -0.009(2) C2 0.031(2) 0.037(3) 0.026(2) 0.005(2) -0.0046(19) 0.008(2) C3 0.021(2) 0.054(3) 0.016(2) -0.001(2) 0.0018(17) 0.007(2) C4 0.022(2) 0.070(4) 0.020(2) -0.002(2) 0.0051(18) -0.004(2) C5 0.029(2) 0.055(3) 0.020(2) 0.005(2) -0.0002(19) -0.013(2) C6 0.021(2) 0.055(3) 0.013(2) 0.004(2) -0.0066(17) 0.006(2) C7 0.024(2) 0.057(3) 0.016(2) -0.006(2) -0.0035(18) -0.005(2) C8 0.036(3) 0.044(3) 0.038(3) -0.014(2) -0.001(2) -0.015(2) C9 0.043(3) 0.027(3) 0.056(4) -0.006(2) -0.003(3) -0.008(2) C10 0.025(2) 0.023(2) 0.017(2) 0.0023(17) -0.0036(16) 0.0023(17) C11 0.025(2) 0.027(2) 0.026(2) 0.0050(18) 0.0068(18) -0.0020(18) C12 0.043(3) 0.030(2) 0.031(3) 0.000(2) 0.015(2) -0.002(2) C13 0.056(3) 0.021(2) 0.017(2) 0.0048(18) -0.001(2) 0.000(2) C14 0.039(3) 0.036(3) 0.037(3) -0.009(2) -0.020(2) 0.008(2) C15 0.027(2) 0.038(3) 0.036(3) -0.009(2) -0.012(2) 0.010(2) C16 0.124(8) 0.085(6) 0.086(6) -0.060(5) 0.066(6) -0.046(6) C17 0.086(5) 0.047(4) 0.049(4) -0.021(3) -0.036(4) 0.017(3) B1_3 0.0338(12) 0.0596(17) 0.0277(11) 0.0011(12) -0.0015(9) -0.0003(12) F1_3 0.044(2) 0.0603(18) 0.0422(17) 0.0085(14) -0.0025(16) 0.0019(14) F2_3 0.0306(17) 0.060(2) 0.0259(11) -0.0013(12) -0.0012(10) 0.0012(17) F3_3 0.0363(14) 0.068(2) 0.0277(16) -0.0037(17) 0.0022(12) -0.0053(15) F4_3 0.0361(15) 0.063(2) 0.0274(16) 0.0011(17) -0.0017(12) -0.0050(15) B1_4 0.0338(12) 0.0596(17) 0.0277(11) 0.0011(12) -0.0015(9) -0.0003(12) F1_4 0.039(2) 0.060(2) 0.032(2) 0.0033(18) -0.002(2) 0.0015(18) F2_4 0.0334(15) 0.062(3) 0.029(2) 0.000(2) -0.0046(17) 0.0017(18) F3_4 0.0336(18) 0.059(2) 0.027(2) 0.001(2) -0.0015(18) -0.0004(19) F4_4 0.033(2) 0.060(3) 0.0273(13) -0.0005(17) -0.0024(16) 0.000(2) C1A_1 0.052(4) 0.059(4) 0.036(4) 0.011(3) 0.002(3) 0.032(3) C2A_1 0.038(4) 0.054(4) 0.031(4) 0.017(3) -0.007(3) 0.021(3) C3A_1 0.046(4) 0.042(4) 0.026(4) 0.015(3) -0.008(3) 0.009(3) C4A_1 0.060(5) 0.040(4) 0.034(4) 0.010(4) -0.006(3) 0.015(3) C5A_1 0.065(5) 0.049(4) 0.037(4) 0.007(3) -0.004(4) 0.028(3) C1A_2 0.057(6) 0.047(5) 0.041(6) 0.024(5) 0.002(4) 0.018(4) C2A_2 0.052(6) 0.047(5) 0.041(6) 0.022(5) -0.008(4) 0.019(4) C3A_2 0.042(6) 0.042(5) 0.045(6) 0.022(5) -0.008(4) 0.015(4) C4A_2 0.042(6) 0.036(5) 0.045(6) 0.024(5) 0.002(4) 0.013(4) C5A_2 0.053(6) 0.038(5) 0.045(6) 0.026(5) 0.008(5) 0.016(4) _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 Ni1 S1 2.1519(14) . ? Ni1 O2 1.880(3) . ? Ni1 N1 1.949(4) . ? Ni1 N2 1.898(4) . ? Fe1 S2 2.1689(13) . ? Fe1 C1 1.754(6) . ? Fe1 C1A_1 2.140(10) . ? Fe1 C2A_1 2.077(18) . ? Fe1 C3A_1 2.085(10) . ? Fe1 C4A_1 2.084(14) . ? Fe1 C5A_1 2.098(11) . ? Fe1 C1A_2 2.150(11) . ? Fe1 C2A_2 2.105(17) . ? Fe1 C3A_2 2.11(3) . ? Fe1 C4A_2 2.097(14) . ? Fe1 C5A_2 2.110(18) . ? S1 C9 1.822(5) . ? S2 O2 1.536(3) . ? S2 O3 1.464(3) . ? S2 C10 1.776(4) . ? O1 C1 1.150(6) . ? N1 C2 1.490(6) . ? N1 C3 1.495(5) . ? N1 C6 1.499(5) . ? N2 C5 1.505(6) . ? N2 C7 1.505(6) . ? N2 C8 1.494(7) . ? N3 C13 1.365(6) . ? N3 C16 1.439(9) . ? N3 C17 1.438(8) . ? C3 C4 1.517(7) . ? C4 C5 1.508(8) . ? C6 C7 1.533(8) . ? C8 C9 1.515(8) . ? C10 C11 1.386(6) . ? C10 C15 1.389(6) . ? C11 C12 1.367(7) . ? C12 C13 1.416(7) . ? C13 C14 1.412(8) . ? C14 C15 1.373(7) . ? B1_3 F1_3 1.386(8) . ? B1_3 F2_3 1.360(10) . ? B1_3 F3_3 1.400(8) . ? B1_3 F4_3 1.421(11) . ? B1_4 F1_4 1.386(8) . ? B1_4 F2_4 1.360(10) . ? B1_4 F3_4 1.400(8) . ? B1_4 F4_4 1.421(11) . ? C1A_1 C2A_1 1.397(14) . ? C1A_1 C5A_1 1.369(15) . ? C2A_1 C3A_1 1.396(13) . ? C3A_1 C4A_1 1.525(19) . ? C4A_1 C5A_1 1.385(13) . ? C1A_2 C2A_2 1.396(15) . ? C1A_2 C5A_2 1.370(15) . ? C2A_2 C3A_2 1.398(13) . ? C3A_2 C4A_2 1.524(19) . ? C4A_2 C5A_2 1.386(14) . ? 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 O2 Ni1 S1 91.96(10) . . ? O2 Ni1 N1 94.14(14) . . ? O2 Ni1 N2 173.29(15) . . ? N1 Ni1 S1 173.70(12) . . ? N2 Ni1 S1 91.45(13) . . ? N2 Ni1 N1 82.63(16) . . ? C1 Fe1 S2 92.88(16) . . ? C1 Fe1 C1A_1 163.5(3) . . ? C1 Fe1 C2A_1 129.3(3) . . ? C1 Fe1 C3A_1 96.5(4) . . ? C1 Fe1 C4A_1 98.0(4) . . ? C1 Fe1 C5A_1 132.9(4) . . ? C1 Fe1 C1A_2 83.2(4) . . ? C1 Fe1 C2A_2 99.1(6) . . ? C1 Fe1 C3A_2 136.7(5) . . ? C1 Fe1 C4A_2 147.9(5) . . ? C1 Fe1 C5A_2 109.4(4) . . ? C1A_1 Fe1 S2 98.8(4) . . ? C2A_1 Fe1 S2 93.9(5) . . ? C2A_1 Fe1 C1A_1 38.6(4) . . ? C2A_1 Fe1 C3A_1 39.2(4) . . ? C2A_1 Fe1 C4A_1 67.4(6) . . ? C2A_1 Fe1 C5A_1 62.0(6) . . ? C3A_1 Fe1 S2 120.7(3) . . ? C3A_1 Fe1 C1A_1 67.5(5) . . ? C3A_1 Fe1 C5A_1 65.3(4) . . ? C4A_1 Fe1 S2 161.2(4) . . ? C4A_1 Fe1 C1A_1 67.8(5) . . ? C4A_1 Fe1 C3A_1 42.9(5) . . ? C4A_1 Fe1 C5A_1 38.7(4) . . ? C5A_1 Fe1 S2 134.1(4) . . ? C5A_1 Fe1 C1A_1 37.7(4) . . ? C1A_2 Fe1 S2 140.8(5) . . ? C2A_2 Fe1 S2 105.2(4) . . ? C2A_2 Fe1 C1A_2 38.3(4) . . ? C2A_2 Fe1 C3A_2 38.7(4) . . ? C2A_2 Fe1 C5A_2 60.9(7) . . ? C3A_2 Fe1 S2 91.3(7) . . ? C3A_2 Fe1 C1A_2 67.1(7) . . ? C4A_2 Fe1 S2 118.2(5) . . ? C4A_2 Fe1 C1A_2 67.7(6) . . ? C4A_2 Fe1 C2A_2 66.5(6) . . ? C4A_2 Fe1 C3A_2 42.5(5) . . ? C4A_2 Fe1 C5A_2 38.5(4) . . ? C5A_2 Fe1 S2 154.8(5) . . ? C5A_2 Fe1 C1A_2 37.5(4) . . ? C5A_2 Fe1 C3A_2 64.5(7) . . ? Ni1 S1 Fe1 100.66(5) . . ? C9 S1 Ni1 96.11(19) . . ? C9 S1 Fe1 112.3(2) . . ? O2 S2 Fe1 111.00(13) . . ? O2 S2 C10 100.62(18) . . ? O3 S2 Fe1 114.63(14) . . ? O3 S2 O2 111.35(18) . . ? O3 S2 C10 105.6(2) . . ? C10 S2 Fe1 112.70(14) . . ? S2 O2 Ni1 122.58(18) . . ? C2 N1 Ni1 115.7(3) . . ? C2 N1 C3 108.3(4) . . ? C2 N1 C6 108.6(4) . . ? C3 N1 Ni1 107.5(3) . . ? C3 N1 C6 111.3(3) . . ? C6 N1 Ni1 105.4(3) . . ? C5 N2 Ni1 107.0(3) . . ? C5 N2 C7 110.3(4) . . ? C7 N2 Ni1 106.8(3) . . ? C8 N2 Ni1 112.0(3) . . ? C8 N2 C5 110.0(4) . . ? C8 N2 C7 110.7(4) . . ? C13 N3 C16 120.7(6) . . ? C13 N3 C17 121.4(5) . . ? C17 N3 C16 117.4(5) . . ? O1 C1 Fe1 177.3(5) . . ? N1 C3 C4 111.9(4) . . ? C5 C4 C3 114.8(4) . . ? N2 C5 C4 112.8(4) . . ? N1 C6 C7 109.6(4) . . ? N2 C7 C6 109.5(4) . . ? N2 C8 C9 108.8(4) . . ? C8 C9 S1 105.0(4) . . ? C11 C10 S2 122.4(3) . . ? C11 C10 C15 119.2(4) . . ? C15 C10 S2 118.4(3) . . ? C12 C11 C10 120.3(4) . . ? C11 C12 C13 122.0(5) . . ? N3 C13 C12 122.3(5) . . ? N3 C13 C14 121.4(5) . . ? C14 C13 C12 116.3(4) . . ? C15 C14 C13 121.2(5) . . ? C14 C15 C10 120.9(5) . . ? F1_3 B1_3 F3_3 110.1(6) . . ? F1_3 B1_3 F4_3 108.9(7) . . ? F2_3 B1_3 F1_3 110.7(8) . . ? F2_3 B1_3 F3_3 110.4(8) . . ? F2_3 B1_3 F4_3 109.6(7) . . ? F3_3 B1_3 F4_3 107.1(7) . . ? F1_4 B1_4 F3_4 107.2(11) . . ? F1_4 B1_4 F4_4 104.2(17) . . ? F2_4 B1_4 F1_4 112.8(13) . . ? F2_4 B1_4 F3_4 113.8(14) . . ? F2_4 B1_4 F4_4 114.1(18) . . ? F3_4 B1_4 F4_4 103.8(17) . . ? C2A_1 C1A_1 Fe1 68.3(9) . . ? C5A_1 C1A_1 Fe1 69.5(6) . . ? C5A_1 C1A_1 C2A_1 102.0(13) . . ? C1A_1 C2A_1 Fe1 73.1(8) . . ? C3A_1 C2A_1 Fe1 70.7(8) . . ? C3A_1 C2A_1 C1A_1 114.3(16) . . ? C2A_1 C3A_1 Fe1 70.1(9) . . ? C2A_1 C3A_1 C4A_1 104.3(12) . . ? C4A_1 C3A_1 Fe1 68.5(6) . . ? C3A_1 C4A_1 Fe1 68.6(6) . . ? C5A_1 C4A_1 Fe1 71.2(7) . . ? C5A_1 C4A_1 C3A_1 101.7(11) . . ? C1A_1 C5A_1 Fe1 72.8(6) . . ? C1A_1 C5A_1 C4A_1 117.5(13) . . ? C4A_1 C5A_1 Fe1 70.1(8) . . ? C2A_2 C1A_2 Fe1 69.1(8) . . ? C5A_2 C1A_2 Fe1 69.7(9) . . ? C5A_2 C1A_2 C2A_2 101.0(15) . . ? C1A_2 C2A_2 Fe1 72.6(8) . . ? C1A_2 C2A_2 C3A_2 115.0(19) . . ? C3A_2 C2A_2 Fe1 70.9(14) . . ? C2A_2 C3A_2 Fe1 70.4(12) . . ? C2A_2 C3A_2 C4A_2 104.0(16) . . ? C4A_2 C3A_2 Fe1 68.3(11) . . ? C3A_2 C4A_2 Fe1 69.3(12) . . ? C5A_2 C4A_2 Fe1 71.3(10) . . ? C5A_2 C4A_2 C3A_2 101.3(13) . . ? C1A_2 C5A_2 Fe1 72.9(9) . . ? C1A_2 C5A_2 C4A_2 118.2(16) . . ? C4A_2 C5A_2 Fe1 70.2(9) . . ? _shelx_res_file ; TITL try_a.res in P2(1)/c ninme2.res created by SHELXL-2018/3 at 09:55:29 on 27-Nov-2018 REM Old TITL try in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.157, Rweak 0.008, Alpha 0.064 REM 0.769 for 287 systematic absences, Orientation as input REM Formula found by SHELXT: C24 Fe2 N2 O6 S2 CELL 1.54178 19.8354 9.975 13.3013 90 100.622 90 ZERR 4 0.0007 0.0004 0.0005 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B F Fe N Ni O S UNIT 88 128 4 16 4 12 4 12 8 DELU_CP 0.005 0.005 C1A > C5A DELU_BF4 0.001 0.001 B1 > F4 SIMU_CP 0.005 0.01 2 C1A > C5A SIMU_BF4 0.001 0.002 2 B1 > F4 EADP B1_3 B1_4 SAME_CP 0.005 0.04 C1A > C5A SAME_BF4 0.001 0.04 B1 > F4 L.S. 10 PLAN 20 SIZE 0.038 0.208 0.288 TEMP -173.15 BIND Fe1 S1 BUMP fmap 2 acta REM REM REM WGHT 0.078300 10.804900 FVAR 0.55402 0.59055 0.74219 NI1 7 0.696240 0.771783 0.267337 11.00000 0.01582 0.03104 = 0.01398 -0.00430 -0.00275 -0.00027 FE1 5 0.827175 0.641821 0.440455 11.00000 0.03426 0.02273 = 0.02368 -0.00006 -0.00676 0.00498 S1 9 0.765144 0.603309 0.283030 11.00000 0.02671 0.03121 = 0.02800 -0.01013 -0.00199 0.00264 S2 9 0.836127 0.843274 0.382978 11.00000 0.01705 0.02543 = 0.01484 -0.00054 -0.00459 0.00202 O1 8 0.711562 0.709713 0.536512 11.00000 0.05893 0.05269 = 0.02227 -0.00736 0.01519 -0.01666 O2 8 0.767743 0.890654 0.319228 11.00000 0.01978 0.02641 = 0.01891 0.00018 -0.00569 0.00051 O3 8 0.892741 0.862173 0.327629 11.00000 0.02310 0.04139 = 0.02315 -0.00166 0.00244 0.00030 N1 6 0.626551 0.911699 0.243722 11.00000 0.01684 0.03888 = 0.01247 0.00033 -0.00411 0.00171 N2 6 0.619140 0.658127 0.227905 11.00000 0.02376 0.03942 = 0.01700 -0.00595 -0.00100 -0.00584 N3 6 0.885720 1.248222 0.717663 11.00000 0.07771 0.02975 = 0.03104 -0.01046 0.00507 -0.00418 C1 1 0.756544 0.684116 0.496369 11.00000 0.05390 0.02759 = 0.01659 0.00207 0.00534 -0.00920 C2 1 0.652465 1.050528 0.234348 11.00000 0.03051 0.03727 = 0.02615 0.00513 -0.00464 0.00788 AFIX 137 H2A 2 0.677978 1.080147 0.300831 11.00000 -1.50000 H2B 2 0.613646 1.111002 0.212089 11.00000 -1.50000 H2C 2 0.682812 1.051725 0.183961 11.00000 -1.50000 AFIX 0 C3 1 0.588894 0.908666 0.331251 11.00000 0.02134 0.05369 = 0.01629 -0.00093 0.00181 0.00721 AFIX 23 H3A 2 0.559324 0.989061 0.328254 11.00000 -1.20000 H3B 2 0.622386 0.911669 0.396358 11.00000 -1.20000 AFIX 0 C4 1 0.544960 0.783893 0.329436 11.00000 0.02184 0.06965 = 0.02038 -0.00231 0.00505 -0.00367 AFIX 23 H4A 2 0.527226 0.779431 0.394224 11.00000 -1.20000 H4B 2 0.505016 0.792460 0.272951 11.00000 -1.20000 AFIX 0 C5 1 0.581353 0.654142 0.316108 11.00000 0.02851 0.05522 = 0.01969 0.00516 -0.00018 -0.01333 AFIX 23 H5A 2 0.614357 0.634326 0.379759 11.00000 -1.20000 H5B 2 0.547312 0.580536 0.304905 11.00000 -1.20000 AFIX 0 C6 1 0.580396 0.874787 0.145255 11.00000 0.02056 0.05537 = 0.01304 0.00393 -0.00661 0.00608 AFIX 23 H6A 2 0.598996 0.911729 0.086894 11.00000 -1.20000 H6B 2 0.534249 0.913562 0.143493 11.00000 -1.20000 AFIX 0 C7 1 0.575122 0.721810 0.136065 11.00000 0.02406 0.05652 = 0.01596 -0.00603 -0.00354 -0.00520 AFIX 23 H7A 2 0.526810 0.693659 0.131725 11.00000 -1.20000 H7B 2 0.590544 0.692127 0.072975 11.00000 -1.20000 AFIX 0 C8 1 0.639632 0.519599 0.203234 11.00000 0.03623 0.04404 = 0.03814 -0.01450 -0.00075 -0.01483 AFIX 23 H8A 2 0.652855 0.518471 0.135013 11.00000 -1.20000 H8B 2 0.600595 0.457357 0.201850 11.00000 -1.20000 AFIX 0 C9 1 0.699660 0.475461 0.284044 11.00000 0.04326 0.02717 = 0.05642 -0.00575 -0.00314 -0.00761 AFIX 23 H9A 2 0.716577 0.386431 0.267083 11.00000 -1.20000 H9B 2 0.686231 0.470478 0.352034 11.00000 -1.20000 AFIX 0 C10 1 0.848532 0.965711 0.481616 11.00000 0.02478 0.02256 = 0.01672 0.00229 -0.00361 0.00235 C11 1 0.794346 1.032395 0.511937 11.00000 0.02498 0.02655 = 0.02607 0.00504 0.00679 -0.00198 AFIX 43 H11 2 0.748590 1.012912 0.479612 11.00000 -1.20000 AFIX 0 C12 1 0.806417 1.126061 0.588124 11.00000 0.04285 0.02983 = 0.03117 -0.00031 0.01544 -0.00203 AFIX 43 H12 2 0.768620 1.172265 0.606571 11.00000 -1.20000 AFIX 0 C13 1 0.873499 1.156374 0.640412 11.00000 0.05588 0.02074 = 0.01734 0.00480 -0.00053 0.00019 C14 1 0.927664 1.086986 0.607782 11.00000 0.03884 0.03577 = 0.03665 -0.00857 -0.02034 0.00846 AFIX 43 H14 2 0.973637 1.105101 0.639812 11.00000 -1.20000 AFIX 0 C15 1 0.915117 0.993833 0.530630 11.00000 0.02742 0.03785 = 0.03599 -0.00939 -0.01182 0.00992 AFIX 43 H15 2 0.952451 0.947989 0.510481 11.00000 -1.20000 AFIX 0 C16 1 0.829843 1.313221 0.753462 11.00000 0.12423 0.08539 = 0.08559 -0.05979 0.06603 -0.04562 AFIX 137 H16A 2 0.795811 1.343198 0.694762 11.00000 -1.50000 H16B 2 0.847250 1.390757 0.795615 11.00000 -1.50000 H16C 2 0.808408 1.249982 0.794391 11.00000 -1.50000 AFIX 0 C17 1 0.953916 1.295460 0.757372 11.00000 0.08637 0.04688 = 0.04934 -0.02134 -0.03631 0.01689 AFIX 137 H17A 2 0.982938 1.219717 0.785159 11.00000 -1.50000 H17B 2 0.952301 1.361057 0.811726 11.00000 -1.50000 H17C 2 0.972990 1.337803 0.702296 11.00000 -1.50000 AFIX 0 RESI BF4 3 PART 1 B1 3 0.612914 1.284191 0.472101 31.00000 0.03380 0.05956 = 0.02767 0.00108 -0.00154 -0.00027 F1 4 0.636479 1.156040 0.499137 31.00000 0.04438 0.06030 = 0.04215 0.00849 -0.00252 0.00189 F2 4 0.590966 1.293380 0.369293 31.00000 0.03063 0.06029 = 0.02594 -0.00127 -0.00123 0.00116 F3 4 0.559931 1.318153 0.523862 31.00000 0.03632 0.06820 = 0.02767 -0.00370 0.00216 -0.00534 F4 4 0.667119 1.376968 0.503367 31.00000 0.03606 0.06290 = 0.02735 0.00114 -0.00166 -0.00503 RESI BF4 4 PART 0 PART 2 B1 3 0.610102 1.283841 0.478949 -31.00000 0.03380 0.05956 = 0.02767 0.00108 -0.00154 -0.00027 F1 4 0.600008 1.153352 0.508692 -31.00000 0.03920 0.05976 = 0.03238 0.00328 -0.00204 0.00152 F2 4 0.674320 1.329944 0.516448 -31.00000 0.03340 0.06229 = 0.02921 0.00005 -0.00457 0.00172 F3 4 0.557887 1.362164 0.506700 -31.00000 0.03357 0.05913 = 0.02657 0.00127 -0.00150 -0.00035 F4 4 0.593416 1.279925 0.370374 -31.00000 0.03265 0.06010 = 0.02730 -0.00051 -0.00235 0.00005 RESI CP 1 PART 0 PART 1 C1A 1 0.922483 0.562204 0.413726 21.00000 0.05220 0.05887 = 0.03642 0.01095 0.00184 0.03176 AFIX 43 H1A 2 0.942536 0.581862 0.355836 21.00000 -1.20000 AFIX 0 C2A 1 0.930245 0.629390 0.507276 21.00000 0.03801 0.05379 = 0.03095 0.01723 -0.00686 0.02062 AFIX 43 H2A 2 0.960015 0.703982 0.523711 21.00000 -1.20000 AFIX 0 C3A 1 0.890515 0.577581 0.574596 21.00000 0.04564 0.04228 = 0.02625 0.01525 -0.00820 0.00900 AFIX 43 H3A 2 0.888049 0.608188 0.641454 21.00000 -1.20000 AFIX 0 C4A 1 0.851996 0.460700 0.516360 21.00000 0.06027 0.03994 = 0.03437 0.01046 -0.00602 0.01453 AFIX 43 H4A 2 0.818609 0.403067 0.536139 21.00000 -1.20000 AFIX 0 C5A 1 0.878500 0.460676 0.427018 21.00000 0.06478 0.04933 = 0.03700 0.00724 -0.00418 0.02827 AFIX 43 H5A 2 0.866602 0.392738 0.376830 21.00000 -1.20000 AFIX 0 RESI CP 2 PART 0 PART 2 C1A 1 0.856258 0.524793 0.577360 -21.00000 0.05748 0.04746 = 0.04108 0.02441 0.00191 0.01846 AFIX 43 H1A 2 0.826940 0.509056 0.625116 -21.00000 -1.20000 AFIX 0 C2A 1 0.902791 0.628928 0.573758 -21.00000 0.05246 0.04735 = 0.04147 0.02220 -0.00782 0.01899 AFIX 43 H2A 2 0.912202 0.695442 0.625566 -21.00000 -1.20000 AFIX 0 C3A 1 0.934496 0.627987 0.488201 -21.00000 0.04203 0.04199 = 0.04503 0.02219 -0.00845 0.01548 AFIX 43 H3A 2 0.966831 0.690211 0.471061 -21.00000 -1.20000 AFIX 0 C4A 1 0.905163 0.503992 0.428792 -21.00000 0.04194 0.03607 = 0.04467 0.02421 0.00244 0.01319 AFIX 43 H4A 2 0.912793 0.471420 0.364713 -21.00000 -1.20000 AFIX 0 C5A 1 0.864371 0.451483 0.493315 -21.00000 0.05286 0.03772 = 0.04469 0.02626 0.00798 0.01592 AFIX 43 H5A 2 0.842614 0.366889 0.479611 -21.00000 -1.20000 AFIX 0 HKLF 4 REM try_a.res in P2(1)/c REM wR2 = 0.1580, GooF = S = 1.038, Restrained GooF = 1.053 for all data REM R1 = 0.0607 for 4176 Fo > 4sig(Fo) and 0.0664 for all 4592 data REM 423 parameters refined using 173 restraints END WGHT 0.0785 10.7799 REM Highest difference peak 1.164, deepest hole -0.850, 1-sigma level 0.107 Q1 1 0.5582 1.1253 0.5067 11.00000 0.05 1.16 Q2 1 0.6603 1.2388 0.5359 11.00000 0.05 1.02 Q3 1 0.7525 0.5499 0.3239 11.00000 0.05 0.82 Q4 1 0.6873 0.7879 0.3415 11.00000 0.05 0.82 Q5 1 0.5664 1.2448 0.5468 11.00000 0.05 0.74 Q6 1 0.8724 0.6359 0.4658 11.00000 0.05 0.70 Q7 1 0.6454 0.7745 0.2428 11.00000 0.05 0.66 Q8 1 0.8349 0.8993 0.4370 11.00000 0.05 0.64 Q9 1 0.7464 0.7710 0.2902 11.00000 0.05 0.60 Q10 1 0.8200 0.6681 0.5006 11.00000 0.05 0.58 Q11 1 0.8489 0.4307 0.4367 11.00000 0.05 0.58 Q12 1 0.7745 0.6430 0.4185 11.00000 0.05 0.56 Q13 1 0.8104 0.5982 0.3059 11.00000 0.05 0.54 Q14 1 0.8294 0.5965 0.3855 11.00000 0.05 0.52 Q15 1 0.9404 0.6303 0.4300 11.00000 0.05 0.52 Q16 1 0.6971 0.7441 0.1940 11.00000 0.05 0.50 Q17 1 0.8335 0.6984 0.3826 11.00000 0.05 0.50 Q18 1 0.7854 0.8483 0.3578 11.00000 0.05 0.50 Q19 1 0.5881 1.2195 0.3943 11.00000 0.05 0.49 Q20 1 0.8344 0.7718 0.4238 11.00000 0.05 0.46 ; _shelx_res_checksum 1559 _shelx_hkl_file ; 0 0 1 0.70 0.40 0 0 2 420.06 30.00 0 0 3 1.50 1.10 0 0 5 -0.40 1.40 0 0 5 -1.20 2.80 0 0 6 43.90 3.50 0 0 6 39.60 4.00 0 0 6 27.90 6.30 0 0 7 -1.80 4.70 0 0 7 1.30 1.90 0 0 7 0.50 1.20 0 0 8 2072.99 147.49 0 0 -8 2098.19 148.59 0 0 -8 2368.86 151.48 0 0 -8 1773.32 153.58 0 0 -8 1775.52 149.09 0 0 -8 2171.48 148.89 0 0 -9 -15.10 8.30 0 0 -9 17.00 18.30 0 0 -9 4.40 7.80 0 0 -9 -7.30 11.50 0 0 -9 -3.10 9.20 0 0 -9 0.00 8.20 0 0 -9 2.00 10.60 0 0 -10 42.80 9.20 0 0 -10 58.89 20.60 0 0 -10 38.50 12.10 0 0 -10 49.10 17.70 0 0 -10 26.30 14.00 0 0 -10 50.69 12.50 0 0 -11 -3.50 9.00 0 0 -11 -0.30 18.80 0 0 -11 3.00 11.40 0 0 -11 -1.00 16.20 0 0 -11 -8.40 7.70 0 0 -11 -9.70 9.70 0 0 -11 -13.40 7.60 0 0 -12 40.60 22.10 0 0 -12 18.50 17.50 0 0 -12 24.10 12.70 0 0 -12 14.60 9.60 0 0 -12 27.10 13.80 0 0 -13 24.80 19.90 0 0 -13 -2.40 23.30 0 0 -13 18.20 13.80 0 0 -13 9.00 16.00 0 0 -14 154.78 21.90 0 0 -14 120.49 28.50 0 0 -14 154.08 29.00 0 0 -15 8.30 10.50 0 0 -15 -19.30 20.20 0 0 -15 3.90 15.10 0 1 0 1.50 0.50 0 1 0 1.00 0.70 0 1 0 1.80 0.70 0 -1 0 0.80 0.50 0 -1 0 0.50 0.70 0 -1 0 1.10 0.70 0 1 1 863.61 61.29 0 1 -1 847.42 61.29 0 1 -1 875.41 61.29 0 1 1 813.82 61.39 0 1 1 894.71 61.29 0 -1 1 862.11 61.29 0 -1 -1 852.91 61.39 0 -1 1 875.21 61.39 0 -1 -1 904.01 61.29 0 -1 -1 846.82 61.29 0 -1 1 832.42 61.29 0 1 3 1809.52 126.19 0 1 3 1900.61 125.89 0 1 3 1887.91 125.89 0 1 3 1623.04 126.19 0 -1 3 1668.03 126.09 0 -1 3 1733.73 125.89 0 1 4 648.34 43.70 0 1 4 569.54 44.20 0 1 4 613.74 43.60 0 1 4 625.44 44.10 0 -1 4 620.34 43.80 0 -1 4 601.64 43.70 0 1 5 18.50 1.50 0 1 5 13.60 3.20 0 1 5 14.80 3.10 0 -1 5 16.70 2.20 0 -1 5 11.60 3.60 0 -1 5 16.10 1.80 0 1 6 3163.38 213.18 0 1 6 2923.31 213.58 0 -1 6 2852.11 214.08 0 -1 6 3024.80 212.88 0 1 7 1799.22 129.49 0 1 7 1879.11 128.79 0 -1 7 1961.40 128.39 0 -1 7 1626.04 130.69 0 -1 7 1735.83 128.69 0 1 -8 697.33 67.59 0 1 8 770.42 57.39 0 1 -8 853.71 63.19 0 1 -8 809.92 58.59 0 1 -8 788.62 59.19 0 1 -8 810.92 59.89 0 -1 -8 781.22 60.29 0 -1 -8 857.61 58.09 0 -1 8 756.32 58.69 0 -1 -8 670.43 65.49 0 -1 -8 680.23 59.79 0 -1 -8 803.22 63.19 0 -1 -8 877.71 58.19 0 -1 -8 716.53 61.59 0 1 -9 75.49 24.00 0 1 -9 81.69 16.10 0 1 -9 49.80 22.20 0 1 -9 77.39 11.10 0 1 -9 64.19 14.40 0 1 -9 23.50 32.20 0 1 -9 75.69 15.20 0 -1 -9 41.20 11.60 0 -1 -9 49.50 9.20 0 -1 -9 46.10 15.30 0 -1 -9 71.79 20.10 0 -1 -9 60.99 14.70 0 -1 -9 80.59 16.10 0 -1 -9 51.09 10.80 0 1 -10 49.10 15.30 0 1 -10 57.19 11.60 0 1 -10 68.99 13.90 0 1 -10 83.09 11.70 0 1 -10 59.09 13.70 0 1 -10 71.09 25.10 0 -1 -10 98.19 19.30 0 -1 -10 85.09 12.80 0 -1 -10 75.99 14.50 0 -1 -10 90.29 21.90 0 -1 -10 75.19 21.30 0 -1 -10 56.09 17.20 0 -1 -10 87.29 16.40 0 1 -11 272.57 28.10 0 1 -11 243.98 33.20 0 1 -11 281.47 26.30 0 1 -11 237.28 39.20 0 1 -11 245.78 28.90 0 -1 -11 269.57 23.50 0 -1 -11 252.07 36.40 0 -1 -11 243.48 32.80 0 -1 -11 293.97 28.10 0 -1 -11 244.88 27.10 0 1 -12 92.39 20.30 0 1 -12 118.09 19.10 0 1 -12 105.89 21.40 0 1 -12 130.79 31.20 0 1 -12 98.29 21.60 0 -1 -12 105.49 20.60 0 -1 -12 149.88 33.00 0 -1 -12 77.19 19.20 0 -1 -12 147.89 22.40 0 -1 -12 109.09 15.50 0 1 -13 472.15 39.70 0 1 -13 434.96 45.40 0 1 -13 471.85 54.39 0 1 -13 475.45 42.90 0 -1 -13 364.96 47.40 0 -1 -13 424.46 49.10 0 1 -14 46.20 17.20 0 1 -14 76.99 12.70 0 1 -14 96.89 28.70 0 -1 -14 99.29 25.00 0 -1 -14 97.79 21.50 0 -1 -14 73.69 20.30 0 1 -15 194.48 20.40 0 1 -15 151.58 20.00 0 1 -15 175.98 32.70 0 1 -15 200.18 26.80 0 -1 -15 220.38 31.40 0 -1 -15 214.68 30.70 0 2 1 1042.50 71.69 0 2 -1 983.80 71.69 0 2 1 991.90 71.79 0 2 -1 1020.10 71.89 0 2 1 1047.10 71.89 0 2 -1 1044.60 71.79 0 -2 1 962.30 71.69 0 -2 1 1053.49 71.89 0 -2 -1 991.80 71.69 0 -2 1 983.70 71.69 0 -2 -1 1081.29 71.79 0 -2 -1 957.40 71.59 0 -2 -1 917.11 71.89 0 2 -2 2029.30 140.79 0 2 2 2005.70 140.79 0 2 -2 2127.49 140.69 0 2 2 1991.60 140.99 0 2 2 1942.61 140.69 0 -2 -2 1874.51 140.99 0 -2 2 1910.21 140.69 0 -2 -2 2007.60 140.59 0 -2 -2 1977.90 140.59 0 -2 2 1856.81 140.69 0 -2 2 2019.60 140.99 0 2 3 2026.00 137.89 0 2 3 2024.90 137.59 0 2 3 1946.61 137.49 0 -2 3 1803.62 137.59 0 -2 3 1992.70 137.79 0 -2 3 1798.12 137.39 0 2 4 280.37 19.40 0 2 4 269.97 19.30 0 2 4 268.37 19.90 0 2 4 270.67 19.40 0 -2 4 252.57 19.50 0 -2 4 268.77 19.90 0 2 5 6482.35 473.25 0 2 5 6782.52 473.75 0 2 5 6939.41 473.25 0 2 5 6637.74 473.45 0 -2 5 6515.25 473.35 0 -2 5 6581.84 473.65 0 2 6 379.96 28.00 0 2 6 404.16 27.60 0 2 6 398.56 29.60 0 -2 6 384.96 27.80 0 -2 6 344.57 29.60 0 2 -7 774.52 57.89 0 2 -7 650.63 53.69 0 2 -7 674.73 53.99 0 2 7 712.93 50.99 0 2 7 763.02 50.49 0 2 7 758.42 51.39 0 2 -7 664.03 63.39 0 -2 -7 706.53 52.39 0 -2 7 776.92 50.69 0 -2 7 675.73 51.29 0 -2 -7 753.82 52.49 0 -2 -7 584.84 53.69 0 -2 7 640.44 52.79 0 2 -8 1055.69 82.69 0 2 -8 1147.89 83.49 0 2 -8 1237.68 86.29 0 2 -8 1050.89 90.99 0 2 -8 1153.08 81.79 0 2 8 1189.98 80.99 0 -2 -8 995.50 87.39 0 -2 -8 1106.09 84.89 0 -2 -8 1172.08 81.59 0 -2 -8 1186.28 81.69 0 -2 -8 1037.30 83.19 0 -2 -8 1126.09 82.99 0 -2 -8 1050.99 86.89 0 2 -9 265.97 24.60 0 2 -9 276.47 37.40 0 2 -9 227.28 42.40 0 2 -9 254.67 25.60 0 2 -9 293.37 25.50 0 2 -9 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1 14.30 7.70 -11 5 0 829.62 76.29 -11 -5 0 922.41 65.99 11 -5 0 793.72 66.59 11 -5 0 977.30 66.19 11 5 1 140.19 32.10 -11 5 -1 135.09 25.80 11 -5 1 103.39 15.40 -11 -5 -1 92.89 14.90 -11 -5 -1 103.89 15.70 -11 5 -2 258.77 22.90 -11 5 -2 206.38 36.90 11 -5 2 214.68 21.00 -11 -5 -2 229.08 22.30 -11 -5 -2 190.38 21.80 -11 5 -3 80.39 22.80 -11 -5 -3 73.89 12.90 11 -5 3 74.29 13.30 -11 -5 -3 84.39 11.90 -11 -5 -3 55.59 13.80 -11 -5 -3 71.19 14.00 -11 5 -4 354.66 43.50 -11 -5 -4 362.06 30.70 11 -5 4 357.86 29.50 -11 -5 -4 323.77 31.80 -11 -5 -4 344.07 31.10 -11 -5 -4 395.86 32.80 -11 5 -5 -19.90 21.20 -11 5 -5 15.10 11.10 -11 5 -5 -2.20 17.60 -11 -5 -5 46.10 20.50 -11 -5 -5 7.80 9.60 11 -5 5 8.10 6.80 -11 -5 -5 -6.30 8.00 -11 5 -6 1107.19 96.59 -11 5 -6 1423.96 101.69 -11 -5 -6 1221.98 90.79 11 -5 6 1131.79 89.59 -11 -5 -6 1412.16 92.29 -11 -5 -6 1099.59 91.09 -11 5 -7 137.99 32.20 -11 5 -7 166.78 36.40 -11 -5 -7 117.59 17.60 -11 -5 -7 84.79 13.70 -11 -5 -7 109.99 20.50 -11 5 -8 83.49 20.20 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-6 -2 359.66 30.70 -11 -6 2 388.56 30.10 -11 6 1 64.99 22.10 11 6 -1 29.50 15.90 11 -6 -1 16.60 8.50 -11 -6 1 28.90 8.50 -11 -6 1 14.10 8.50 -11 -6 1 9.10 7.00 11 -6 -1 26.20 8.90 -11 6 0 921.21 93.09 11 6 0 1231.28 88.89 11 -6 0 1139.69 80.99 -11 -6 0 1105.99 80.79 -11 -6 0 1035.60 80.29 -11 6 -1 313.37 43.00 11 6 1 388.16 43.00 11 -6 1 333.57 29.70 -11 -6 -1 366.66 29.40 -11 -6 -1 316.47 29.70 -11 6 -2 139.09 25.00 11 -6 2 114.59 16.50 -11 -6 -2 90.79 17.20 -11 -6 -2 126.29 16.20 -11 6 -3 48.80 19.80 -11 -6 -3 62.19 12.30 -11 -6 -3 68.19 11.60 -11 -6 -3 79.19 14.70 -11 -6 -3 89.39 20.60 11 -6 3 72.09 10.40 -11 6 -4 208.88 36.50 -11 -6 -4 253.97 24.80 -11 -6 -4 195.28 23.70 -11 -6 -4 206.58 21.80 -11 -6 -4 222.58 22.70 11 -6 4 195.38 20.80 -11 6 -5 61.99 21.40 -11 -6 -5 38.00 10.30 -11 -6 -5 53.39 12.70 -11 -6 -5 24.10 12.30 -11 -6 -5 53.29 11.20 -11 6 -6 279.37 58.19 -11 6 -6 357.46 43.10 -11 -6 -6 363.26 31.50 -11 -6 -6 261.47 28.70 -11 -6 -6 309.77 29.60 -11 -6 -6 294.17 27.20 -11 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8.00 6.00 21 3 -8 38.30 14.00 -21 3 8 35.30 7.30 21 3 -8 32.60 11.30 21 -3 -8 43.60 12.80 -21 -3 8 21.90 5.20 21 -3 -8 22.40 8.20 21 3 -7 66.89 13.60 -21 3 7 50.99 8.90 21 3 -7 30.40 13.30 -21 -3 7 51.59 7.50 21 -3 -7 87.89 16.40 -21 3 6 12.90 7.50 21 -3 -6 18.50 9.60 -21 -3 6 18.60 6.00 -21 3 5 7.70 8.10 21 -3 -5 12.60 9.60 -21 -3 5 7.10 6.20 -21 3 4 0.50 8.00 -21 -3 4 -2.00 6.40 -21 -3 4 12.30 6.80 21 -3 -4 -11.20 9.00 -21 3 3 63.09 10.30 -21 3 3 55.49 10.10 21 -3 -3 64.69 12.30 -21 -3 3 71.29 13.50 -21 -3 3 78.19 12.00 -21 3 2 146.49 18.00 21 3 -2 100.09 22.70 21 -3 -2 147.39 19.30 -21 -3 2 147.09 16.90 -21 -3 2 151.28 15.40 -21 3 1 59.09 9.90 -21 -3 1 51.99 8.70 -21 -3 1 60.59 8.60 21 -3 -1 35.50 10.90 21 3 0 358.56 36.90 -21 3 0 449.26 34.00 -21 -3 0 430.46 32.60 21 -3 0 413.56 36.60 -21 -3 0 423.06 33.20 -21 3 -1 213.78 20.00 21 3 1 157.88 22.80 -21 -3 -1 212.58 19.40 -21 -3 -1 227.48 18.40 21 -3 1 197.08 22.40 21 3 2 228.68 25.60 -21 3 -2 303.57 23.80 -21 -3 -2 263.97 22.80 21 -3 2 269.27 24.80 -21 3 -3 15.70 9.90 21 3 3 2.40 7.10 -21 -3 -3 17.60 5.60 21 -3 3 5.20 6.60 21 4 -7 146.29 18.70 -21 4 7 173.68 15.70 21 -4 -7 129.99 17.10 -21 -4 7 141.79 13.30 -21 -4 7 169.78 15.50 21 4 -6 405.26 33.40 -21 4 6 395.36 30.80 -21 -4 6 374.96 29.50 21 -4 -6 357.76 31.90 -21 -4 6 419.06 30.00 21 -4 -6 363.16 33.90 21 4 -5 35.60 11.80 21 4 -5 3.60 10.00 -21 4 5 18.60 7.00 21 -4 -5 19.70 9.30 -21 -4 5 14.50 5.20 -21 -4 5 21.60 8.90 21 4 -4 314.97 27.00 -21 4 4 268.47 23.90 -21 -4 4 264.37 22.20 21 -4 -4 254.97 25.80 -21 4 3 8.70 7.40 21 4 -3 -10.30 9.80 21 -4 -3 17.00 9.40 -21 -4 3 8.40 5.60 -21 -4 3 22.20 6.00 -21 4 2 826.22 58.79 21 4 -2 701.23 61.49 -21 -4 2 841.72 57.79 -21 -4 2 770.12 57.79 -21 4 1 263.87 22.80 -21 -4 1 242.28 21.40 -21 -4 1 247.98 21.10 -21 4 0 61.09 9.10 -21 -4 0 61.49 10.10 -21 -4 0 43.00 7.40 -21 4 -1 29.30 7.80 -21 -4 -1 37.20 6.90 -21 -4 -1 34.70 6.70 -21 4 -2 477.95 35.30 21 -4 2 406.16 34.80 -21 -4 -2 413.86 32.50 -21 -4 -2 418.86 34.90 -21 5 5 -9.80 5.40 21 -5 -5 -2.00 7.40 -21 -5 5 -2.50 4.20 -21 5 4 22.90 6.50 21 5 -4 2.20 8.70 -21 -5 4 11.50 4.90 21 -5 -4 6.70 5.80 21 -5 -4 11.70 8.30 -21 5 3 32.70 7.10 21 -5 -3 44.60 9.60 21 -5 -3 36.00 6.80 -21 -5 3 44.90 8.20 21 5 -2 41.70 10.40 -21 5 2 65.89 10.70 -21 -5 2 36.50 6.40 -21 -5 2 50.79 8.60 -21 5 1 12.20 6.50 21 5 -1 5.80 8.10 -21 -5 1 12.10 5.40 -21 -5 1 15.30 6.30 -21 5 0 27.50 7.20 -21 -5 0 26.00 5.50 -21 -5 0 14.90 8.40 -22 0 8 65.49 9.00 -22 0 7 0.80 7.40 22 0 -7 21.80 9.50 -22 0 7 2.90 5.20 -22 0 6 117.59 14.40 -22 0 6 102.89 12.50 -22 0 5 1.20 6.00 22 0 -5 -8.30 15.20 -22 0 5 6.00 7.50 -22 0 4 359.16 28.50 -22 0 4 337.27 26.40 22 0 -4 284.37 36.90 -22 0 3 0.80 8.00 -22 0 3 -6.10 6.00 22 0 -3 -4.80 10.50 22 0 -2 204.48 26.40 -22 0 2 283.37 23.50 -22 0 2 247.88 20.90 -22 0 1 3.40 6.60 -22 0 1 7.00 8.30 22 0 -1 -2.00 9.00 22 0 0 65.89 17.40 -22 0 -1 -6.70 7.00 22 0 1 -7.10 7.50 22 0 2 16.60 7.60 -22 0 -2 26.30 6.60 22 0 3 0.00 6.20 -22 0 -3 8.10 5.80 -22 0 -3 -5.70 5.20 22 1 -8 128.19 16.10 -22 1 8 109.09 10.70 22 -1 -8 95.79 16.00 22 -1 -8 100.79 14.30 -22 -1 8 95.29 10.80 -22 1 7 123.89 15.10 22 1 -7 112.39 27.70 -22 1 7 104.19 11.50 -22 -1 7 113.29 12.10 22 -1 -7 146.49 16.60 22 -1 -7 90.19 17.50 -22 1 6 61.59 9.40 -22 1 6 70.19 12.50 22 1 -6 40.60 17.30 -22 -1 6 62.29 10.50 22 -1 -6 68.19 13.90 -22 -1 6 50.19 10.10 -22 1 4 6.20 5.90 -22 1 4 4.30 7.40 22 -1 -4 38.70 16.30 -22 -1 4 18.80 7.70 -22 1 3 112.99 15.80 -22 1 3 108.09 12.80 -22 -1 3 110.39 13.00 22 -1 -3 86.09 16.60 -22 -1 3 129.39 15.70 22 1 -2 -1.30 10.10 -22 1 2 4.40 6.20 -22 1 2 7.80 7.90 -22 -1 2 8.50 6.50 -22 -1 2 9.10 7.90 22 -1 -2 -4.00 9.70 22 1 -1 20.90 9.90 22 -1 -1 34.90 10.40 -22 1 0 38.20 8.90 22 1 0 15.30 9.30 -22 -1 0 29.40 7.50 -22 -1 0 13.20 8.00 -22 -1 0 36.30 8.30 22 -1 0 26.30 9.40 -22 1 -1 2.60 6.90 22 1 1 -2.70 7.50 -22 -1 -1 9.70 6.10 -22 -1 -1 8.20 6.60 22 -1 1 3.80 8.20 22 1 2 16.30 7.40 22 -1 2 29.60 7.80 -22 -1 -2 46.00 9.50 -22 2 7 9.30 6.70 22 2 -7 23.60 10.30 22 2 -7 0.70 13.30 22 -2 -7 12.10 9.80 -22 -2 7 6.90 4.90 22 -2 -7 1.20 8.60 -22 2 6 9.20 6.80 22 2 -6 25.10 10.00 22 2 -6 1.90 12.70 22 -2 -6 16.00 8.80 -22 -2 6 6.90 5.40 -22 2 5 9.80 5.10 -22 2 5 12.50 7.30 22 2 -5 -4.40 10.30 -22 -2 5 27.20 7.30 22 -2 -5 7.00 8.60 -22 -2 5 3.70 5.70 -22 2 4 4.50 5.30 22 2 -4 2.30 9.90 -22 2 4 9.90 7.30 -22 -2 4 8.80 6.30 22 -2 -4 2.30 9.40 -22 -2 4 12.90 6.60 -22 2 3 238.68 19.90 -22 2 3 278.07 22.70 -22 -2 3 229.88 21.50 -22 -2 3 233.08 20.30 22 -2 -3 258.97 29.80 22 -2 -3 188.68 29.20 -22 2 2 6.80 6.50 -22 2 2 35.60 8.40 22 -2 -2 31.00 11.50 -22 -2 2 22.50 6.70 -22 -2 2 20.20 6.90 -22 2 1 79.89 14.10 22 -2 -1 52.89 12.00 -22 -2 1 67.59 11.00 -22 -2 1 73.59 12.70 -22 2 0 79.99 13.80 22 2 0 61.19 11.90 -22 -2 0 86.99 12.90 22 -2 0 96.89 17.90 -22 -2 0 91.39 12.10 22 2 1 8.80 7.50 22 -2 1 15.50 8.20 -22 2 -2 210.48 17.10 22 2 2 148.79 18.90 -22 -2 -2 183.88 16.30 22 -2 2 154.08 18.60 22 3 -7 309.67 25.20 22 -3 -7 268.77 30.00 22 -3 -7 274.37 26.10 -22 -3 7 290.37 22.20 -22 3 6 160.28 15.50 22 3 -6 115.39 22.40 22 3 -6 159.78 18.20 22 -3 -6 157.78 24.60 22 -3 -6 129.39 16.50 -22 -3 6 159.18 14.80 -22 -3 6 149.88 13.30 22 3 -5 39.90 11.10 -22 3 5 26.20 7.10 -22 3 5 29.00 5.60 22 -3 -5 37.60 9.10 -22 -3 5 18.10 5.70 22 3 -4 394.76 38.00 -22 3 4 475.25 34.80 -22 3 4 436.96 33.00 -22 -3 4 503.55 33.70 -22 -3 4 412.36 37.00 22 -3 -4 416.46 35.20 -22 3 3 414.76 31.30 22 3 -3 326.67 34.00 -22 -3 3 435.86 30.10 -22 -3 3 409.96 30.30 22 -3 -3 346.87 31.60 -22 3 2 750.42 51.89 22 3 -2 590.24 53.99 -22 -3 2 748.03 51.09 -22 -3 2 751.12 50.79 22 -3 -2 583.84 55.69 22 3 -1 140.89 21.00 -22 3 1 184.48 17.60 -22 -3 1 173.98 15.90 -22 -3 1 189.08 16.70 -22 3 0 368.36 29.60 -22 -3 0 363.26 29.30 -22 -3 0 360.26 28.80 22 -3 0 374.46 32.70 -22 3 -1 15.80 6.50 22 3 1 2.70 7.30 -22 -3 -1 17.10 5.60 -22 -3 -1 15.90 9.00 22 -3 1 24.70 8.10 22 4 -5 -5.00 7.80 22 4 -5 -6.20 10.10 -22 4 5 0.50 5.50 -22 4 5 -6.90 4.60 -22 -4 5 -4.10 4.00 22 -4 -5 12.20 12.50 22 -4 -5 4.80 12.10 22 4 -4 20.50 9.40 -22 4 4 35.10 7.00 -22 4 4 33.40 6.80 -22 -4 4 47.20 7.90 22 -4 -4 61.59 13.30 22 4 -3 -4.80 7.40 -22 4 3 3.80 5.90 22 4 -3 11.90 10.40 -22 -4 3 11.80 5.70 22 -4 -3 2.20 14.90 -22 -4 3 2.50 5.00 22 4 -2 28.30 12.10 22 4 -2 25.80 8.50 22 -4 -2 36.70 8.30 -22 4 1 11.90 6.10 22 4 -1 -5.20 7.30 -22 -4 1 9.40 6.20 22 -4 -1 -6.60 7.90 -22 -4 1 11.50 5.30 -23 0 6 152.98 14.00 -23 0 6 165.78 15.50 -23 0 5 -1.20 6.10 -23 0 5 -1.20 4.90 23 0 -5 18.10 16.70 -23 0 4 10.80 6.80 -23 0 4 3.70 5.10 -23 0 3 8.50 5.30 23 0 -3 -8.60 10.90 -23 0 3 0.80 6.50 23 0 -2 0.60 9.80 -23 0 2 -6.30 6.30 23 0 -1 -0.60 7.80 -23 0 1 8.20 6.20 -23 0 1 9.00 6.90 23 0 0 3.10 7.50 -23 0 0 13.30 5.60 -23 0 0 8.10 6.40 -23 0 -1 9.70 5.70 -23 1 6 -1.20 4.60 23 1 -6 -8.50 13.60 23 1 -6 9.00 8.40 -23 1 6 8.40 7.50 -23 -1 6 5.50 4.80 -23 1 5 9.90 5.00 23 1 -5 22.50 13.70 -23 1 5 27.00 6.90 -23 -1 5 9.90 5.30 -23 -1 5 -0.80 6.30 23 1 -3 -2.40 9.60 -23 1 3 0.10 6.60 -23 1 3 8.10 6.50 -23 -1 3 10.80 5.50 -23 -1 3 7.70 6.40 23 -1 -3 42.70 20.60 -23 1 2 34.60 7.00 -23 1 2 36.10 7.70 -23 -1 2 31.30 6.60 -23 -1 2 39.00 7.50 23 -1 -2 42.20 12.10 -23 1 1 91.19 13.40 -23 -1 1 102.89 11.90 -23 -1 1 84.29 12.70 -23 1 0 182.28 16.40 23 1 0 135.59 18.90 23 -1 0 155.88 19.60 -23 -1 0 190.78 16.10 -23 2 5 37.20 9.00 23 2 -5 68.99 12.20 -23 2 5 48.50 7.60 -23 -2 5 43.30 8.10 -23 2 4 92.39 12.50 -23 2 4 81.59 10.60 -23 -2 4 84.19 11.60 -23 -2 4 81.49 10.20 23 2 -3 244.58 27.80 -23 2 3 294.67 23.70 -23 2 3 287.97 22.40 -23 -2 3 286.67 22.40 -23 -2 3 295.67 23.30 -23 2 2 118.99 14.40 -23 -2 2 138.99 14.00 -23 -2 2 134.49 12.60 -23 2 1 3.60 6.00 -23 -2 1 18.70 5.90 -23 -2 1 7.50 5.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 70359 _olex2_submission_special_instructions 'No special instructions were received'