####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_2_cr1_pristine_a _database_code_depnum_ccdc_archive 'CCDC 2352260' loop_ _audit_author_name _audit_author_address 'Michal Magott' ;Jagiellonian University Poland ; _audit_update_record ; 2024-04-30 deposited with the CCDC. 2025-01-11 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT971_2_cr1_pristine_a ; PROBLEM: Check Calcd Resid. Dens. 0.83Ang From Mo1A 6.12 eA-3 RESPONSE: The residual density near molybdenum is due to partial photoinduced changes in the crystal structure caused by a strong synchrotron X-ray source. ; _vrf_PLAT097_2_cr1_pristine_a ; PROBLEM: Large Reported Max. (Positive) Residual Density 6.20 eA-3 RESPONSE: The residual density near molybdenum is due to partial photoinduced changes in the crystal structure caused by a strong synchrotron X-ray source. ; _vrf_PLAT213_2_cr1_pristine_a ; PROBLEM: Atom N7A has ADP max/min Ratio ..... 5.0 prolat RESPONSE: This is due to the onset of cyanide dissociation induced by a powerful synchrotron X-ray source. ; _vrf_PLAT306_2_cr1_pristine_a ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1A Check RESPONSE: The water molecules in the structure are disordered, so we decided not to model the positions of the hydrogen atoms, since the refinement led to an unphysical result. ; # Added during the CSD deposition process: Tuesday 30 April 2024 11:40 AM # end Validation Reply Form _audit_creation_date 2024-04-28 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _shelx_SHELXL_version_number 2014/7 _audit_contact_author_address ? _audit_contact_author_email ? _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. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Evans, P. (2006) Acta Cryst. D62, 72-82. Evans, P. R. and Murshudov, G. N. (2013) Acta Cryst. D69, 1204-1214. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. Winn, M. D. et al. (2011) Acta Cryst. D67, 235-242. Winter, G. (2010) J. Appl. Cryst. 43, 186-190. Winter, G. et al. (2018) Acta Cryst. D74, 85-97. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic 'Tetrapotassium heptacyanidomolybdate(III) dihydrate' _chemical_formula_moiety 'C7 K4 Mo N7 O2' _chemical_formula_sum 'C7 K4 Mo N7 O2' _chemical_formula_weight 466.48 _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 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.1940 0.2390 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.8750 0.6620 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 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 triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9957(10) _cell_length_b 9.3395(11) _cell_length_c 9.7432(12) _cell_angle_alpha 86.908(11) _cell_angle_beta 82.149(11) _cell_angle_gamma 70.480(10) _cell_volume 764.27(16) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4698 _cell_measurement_temperature 30(1) _cell_measurement_theta_max 28.4275454375 _cell_measurement_theta_min 2.03144704502 _shelx_estimated_absorpt_T_max 0.982 _shelx_estimated_absorpt_T_min 0.916 _exptl_absorpt_coefficient_mu 1.779 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.998287942727 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; CCP4 7.0.058: AIMLESS, version 0.7.1 : 27/03/18 Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics ; _exptl_absorpt_special_details ? _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 450 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0926 _diffrn_reflns_av_unetI/netI 0.1032 _diffrn_reflns_Laue_measured_fraction_full 0.979 _diffrn_reflns_Laue_measured_fraction_max 0.898 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 15513 _diffrn_reflns_point_group_measured_fraction_full 0.979 _diffrn_reflns_point_group_measured_fraction_max 0.898 _diffrn_reflns_theta_full 24.415 _diffrn_reflns_theta_max 29.071 _diffrn_reflns_theta_min 2.243 _diffrn_ambient_temperature 30.0(10) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.898 _diffrn_measurement_device_type 'Diamond Light Source Beamline I19-1' _diffrn_measurement_method 'shutterless scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.6889 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2484 _reflns_number_total 4033 _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 'DIALS 2theta refinement, DIALS 1.10.2-g9c23cb36c-release' _computing_data_collection ? _computing_data_reduction ; aimless (Evans, P. R. and Murshudov, G. N., 2013) ccp4 (Winn, M. D. et al., 2011) DIALS 1.10.2-g9c23cb36c-release (Winter, G. et al., 2018) pointless (Evans, P., 2006) XIA2 0.5.580-g8b4a78df-dials-1.10 (Winter, G., 2010) ; _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 6.205 _refine_diff_density_min -2.444 _refine_diff_density_rms 0.221 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 200 _refine_ls_number_reflns 4033 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1220 _refine_ls_R_factor_gt 0.0788 _refine_ls_restrained_S_all 1.071 _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^)+(0.0528P)^2^+8.8399P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1878 _refine_ls_wR_factor_ref 0.2044 _refine_special_details ? _olex2_refinement_description ; 1. Others Sof(O3A)=1-FVAR(1) Sof(O2A)=FVAR(1) ; _atom_sites_solution_hydrogens . _atom_sites_solution_primary ? _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mo1A Mo 0.71361(10) 0.68734(8) 0.72598(7) 0.0222(2) Uani 1 1 d . . . . . K1A K 0.7237(2) 1.27924(19) 0.91723(17) 0.0184(4) Uani 1 1 d . . . A 4 O1A O 0.9916(9) 1.1096(8) 0.7194(10) 0.058(2) Uani 1 1 d . . . A 4 N2A N 0.6431(8) 1.0265(7) 0.8570(7) 0.0188(14) Uani 1 1 d . . . A 4 K2A K 0.71072(19) 0.48539(18) 1.32581(17) 0.0169(4) Uani 1 1 d . . . B 4 C2A C 0.6670(8) 0.9083(9) 0.8114(7) 0.0146(15) Uani 1 1 d . . . A 4 N3A N 0.6353(8) 0.5920(7) 1.0563(7) 0.0216(15) Uani 1 1 d . . . B 4 K3A K 0.7244(2) 0.08628(19) 0.53389(18) 0.0239(4) Uani 1 1 d . . . C 4 C3A C 0.6630(8) 0.6260(8) 0.9409(8) 0.0154(15) Uani 1 1 d . . . B 4 C4A C 0.6650(9) 0.4929(9) 0.6568(7) 0.0177(16) Uani 1 1 d . . . C 4 N4A N 0.6390(7) 0.3892(7) 0.6178(6) 0.0171(14) Uani 1 1 d . . . C 4 K4A K 0.7228(2) 0.8676(2) 0.13237(18) 0.0216(4) Uani 1 1 d . . . D 4 C5A C 0.6617(9) 0.7751(8) 0.5227(8) 0.0157(15) Uani 1 1 d . . . D 4 N5A N 0.6325(8) 0.8211(8) 0.4130(7) 0.0210(15) Uani 1 1 d . . . D 4 C6A C 0.9224(11) 0.5100(11) 0.7663(10) 0.033(2) Uani 1 1 d . . . E 4 N6A N 1.0321(8) 0.4093(11) 0.7935(10) 0.046(3) Uani 1 1 d . . . E 4 C7A C 0.9180(11) 0.7507(11) 0.6385(11) 0.038(2) Uani 1 1 d . . . F 2 O3A O 0.992(2) 0.941(3) 1.003(2) 0.051(9) Uani 0.335(15) 1 d . . P A 4 O2A O 0.9843(10) 1.2529(11) 1.0505(10) 0.029(3) Uani 0.665(15) 1 d . . P A 4 N7A N 1.0183(9) 0.7993(10) 0.5969(12) 0.059(3) Uani 1 1 d . . . F 2 N1A N 0.3164(12) 0.8163(10) 0.7743(8) 0.037(2) Uani 1 1 d . . . G 4 C1A C 0.4534(11) 0.7714(9) 0.7561(8) 0.0236(18) Uani 1 1 d . . . G 4 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 Mo1A 0.0428(5) 0.0118(3) 0.0098(3) -0.0005(3) -0.0071(3) -0.0047(3) K1A 0.0256(8) 0.0149(8) 0.0147(8) -0.0003(7) -0.0046(7) -0.0059(6) O1A 0.041(4) 0.033(4) 0.090(7) 0.009(4) 0.004(4) -0.007(4) N2A 0.024(3) 0.015(3) 0.017(3) -0.001(3) 0.001(3) -0.008(3) K2A 0.0214(8) 0.0150(8) 0.0112(8) 0.0006(6) -0.0021(6) -0.0019(6) C2A 0.016(3) 0.018(4) 0.011(3) 0.001(3) 0.001(3) -0.009(3) N3A 0.032(4) 0.016(3) 0.018(3) 0.001(3) -0.011(3) -0.007(3) K3A 0.0379(10) 0.0134(8) 0.0172(9) 0.0015(7) -0.0003(8) -0.0059(7) C3A 0.019(3) 0.010(3) 0.017(4) -0.004(3) -0.008(3) -0.001(3) C4A 0.023(4) 0.014(4) 0.008(3) 0.000(3) -0.002(3) 0.004(3) N4A 0.023(3) 0.015(3) 0.010(3) 0.001(3) -0.003(3) -0.002(3) K4A 0.0315(9) 0.0172(9) 0.0150(9) 0.0013(7) -0.0008(7) -0.0079(7) C5A 0.021(4) 0.013(3) 0.014(4) -0.006(3) 0.000(3) -0.008(3) N5A 0.032(4) 0.016(3) 0.015(3) 0.000(3) -0.003(3) -0.009(3) C6A 0.039(5) 0.032(5) 0.030(5) 0.005(4) -0.003(4) -0.018(4) N6A 0.012(4) 0.060(6) 0.055(6) 0.019(5) 0.001(4) -0.001(4) C7A 0.034(5) 0.033(5) 0.039(6) 0.009(5) -0.008(4) 0.000(4) O3A 0.027(11) 0.080(19) 0.060(16) 0.038(14) -0.017(10) -0.039(12) O2A 0.024(5) 0.036(6) 0.026(5) 0.002(4) -0.008(4) -0.006(4) N7A 0.010(3) 0.049(6) 0.113(9) 0.023(6) 0.007(4) -0.013(4) N1A 0.070(6) 0.036(5) 0.019(4) -0.002(3) -0.009(4) -0.034(5) C1A 0.046(5) 0.016(4) 0.013(4) -0.001(3) -0.004(4) -0.015(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 Mo1A K1A 4.1299(17) 1_545 ? Mo1A C2A 2.154(8) . ? Mo1A K3A 4.1029(18) 1_565 ? Mo1A C3A 2.169(7) . ? Mo1A C4A 2.165(8) . ? Mo1A C5A 2.153(7) . ? Mo1A C6A 2.116(10) . ? Mo1A C7A 2.168(10) . ? Mo1A C1A 2.189(10) . ? K1A O1A 2.923(8) . ? K1A N2A 2.802(7) . ? K1A N3A 3.025(7) 2_677 ? K1A N3A 3.095(7) 1_565 ? K1A C3A 3.115(7) 1_565 ? K1A C3A 3.399(8) 2_677 ? K1A C4A 3.133(7) 1_565 ? K1A N4A 3.148(6) 1_565 ? K1A C6A 3.394(8) 1_565 ? K1A O3A 2.87(2) 2_777 ? K1A O2A 2.767(9) . ? K1A N1A 3.097(8) 2_677 ? O1A K3A 3.407(9) 2_766 ? O1A K3A 3.267(9) 1_565 ? O1A K4A 3.185(9) 2_776 ? N2A C2A 1.153(10) . ? N2A K3A 3.196(7) 1_565 ? N2A K4A 3.049(6) 1_556 ? N2A K4A 3.093(7) 2_676 ? K2A N3A 2.846(6) . ? K2A C4A 3.299(8) 2_667 ? K2A C4A 3.196(7) 1_556 ? K2A N4A 2.951(7) 2_667 ? K2A N4A 2.988(6) 1_556 ? K2A K4A 3.973(2) 1_556 ? K2A C5A 3.275(8) 1_556 ? K2A N5A 3.114(7) 1_556 ? K2A C6A 3.313(9) 2_767 ? K2A N6A 2.887(8) 2_767 ? K2A N1A 3.126(8) 2_667 ? K2A C1A 3.386(8) 2_667 ? C2A K3A 3.170(7) 1_565 ? C2A K4A 3.416(8) 2_676 ? C2A K4A 3.217(7) 1_556 ? N3A K1A 3.025(7) 2_677 ? N3A K1A 3.095(7) 1_545 ? N3A C3A 1.169(10) . ? N3A K4A 3.085(7) 1_556 ? K3A Mo1A 4.1029(18) 1_545 ? K3A O1A 3.407(9) 2_766 ? K3A O1A 3.267(9) 1_545 ? K3A N2A 3.196(7) 1_545 ? K3A C2A 3.170(7) 1_545 ? K3A N4A 2.809(7) . ? K3A C5A 3.150(7) 1_545 ? K3A C5A 3.388(7) 2_666 ? K3A N5A 3.010(7) 2_666 ? K3A N5A 3.186(7) 1_545 ? K3A N1A 3.124(8) 2_666 ? K3A C1A 3.423(8) 2_666 ? C3A K1A 3.115(7) 1_545 ? C3A K1A 3.399(8) 2_677 ? C3A K4A 3.225(8) 1_556 ? C4A K1A 3.133(7) 1_545 ? C4A K2A 3.196(7) 1_554 ? C4A K2A 3.299(8) 2_667 ? C4A N4A 1.163(10) . ? N4A K1A 3.148(6) 1_545 ? N4A K2A 2.951(6) 2_667 ? N4A K2A 2.988(6) 1_554 ? K4A O1A 3.185(9) 2_776 ? K4A N2A 3.093(7) 2_676 ? K4A N2A 3.049(6) 1_554 ? K4A C2A 3.217(7) 1_554 ? K4A N3A 3.085(7) 1_554 ? K4A C3A 3.225(8) 1_554 ? K4A N5A 2.797(7) . ? K4A N6A 2.914(8) 2_766 ? K4A O3A 2.849(16) 1_554 ? K4A O2A 2.887(10) 2_776 ? K4A N1A 3.029(8) 2_676 ? K4A C1A 3.378(9) 2_676 ? C5A K2A 3.275(8) 1_554 ? C5A K3A 3.150(7) 1_565 ? C5A K3A 3.388(7) 2_666 ? C5A N5A 1.161(9) . ? N5A K2A 3.114(7) 1_554 ? N5A K3A 3.186(7) 1_565 ? N5A K3A 3.010(7) 2_666 ? C6A K1A 3.394(8) 1_545 ? C6A K2A 3.313(9) 2_767 ? C6A N6A 1.163(11) . ? N6A K1A 3.436(8) 1_545 ? N6A K2A 2.887(8) 2_767 ? N6A K4A 2.914(8) 2_766 ? C7A N7A 1.157(11) . ? O3A K1A 2.87(2) 2_777 ? O3A K4A 2.849(16) 1_556 ? O3A O3A 1.15(4) 2_777 ? O2A K4A 2.887(10) 2_776 ? N1A K1A 3.097(8) 2_677 ? N1A K2A 3.126(8) 2_667 ? N1A K3A 3.124(8) 2_666 ? N1A K4A 3.029(8) 2_676 ? N1A C1A 1.153(12) . ? C1A K1A 3.442(8) 2_677 ? C1A K2A 3.386(8) 2_667 ? C1A K3A 3.423(8) 2_666 ? C1A K4A 3.378(9) 2_676 ? 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 C2A Mo1A K1A 130.83(18) . 1_545 ? C2A Mo1A K3A 49.73(18) . 1_565 ? C2A Mo1A C3A 83.2(3) . . ? C2A Mo1A C4A 158.6(3) . . ? C2A Mo1A C1A 78.9(3) . . ? K3A Mo1A K1A 177.56(4) 1_565 1_545 ? C3A Mo1A K1A 47.7(2) . 1_545 ? C3A Mo1A K3A 132.9(2) . 1_565 ? C3A Mo1A C1A 78.5(3) . . ? C4A Mo1A K1A 48.15(17) . 1_545 ? C4A Mo1A K3A 132.49(17) . 1_565 ? C4A Mo1A C3A 91.0(3) . . ? C4A Mo1A C1A 79.7(3) . . ? C5A Mo1A K1A 131.5(2) . 1_545 ? C5A Mo1A C2A 94.0(3) . . ? C5A Mo1A K3A 49.2(2) . 1_565 ? C5A Mo1A C3A 156.9(3) . . ? C5A Mo1A C4A 83.3(3) . . ? C5A Mo1A C1A 78.5(3) . . ? C6A Mo1A K1A 55.0(2) . 1_545 ? C6A Mo1A C2A 118.7(3) . . ? C6A Mo1A K3A 122.5(2) . 1_565 ? C6A Mo1A C3A 75.8(3) . . ? C6A Mo1A C4A 79.3(3) . . ? C6A Mo1A C5A 124.5(3) . . ? C6A Mo1A C1A 146.3(3) . . ? C1A Mo1A K1A 91.44(19) . 1_545 ? C1A Mo1A K3A 91.00(19) . 1_565 ? O1A K1A N3A 139.5(2) . 2_677 ? O1A K1A N3A 132.8(2) . 1_565 ? O1A K1A C3A 151.6(2) . 2_677 ? O1A K1A C3A 117.0(2) . 1_565 ? O1A K1A C4A 79.6(2) . 1_565 ? O1A K1A N4A 72.5(2) . 1_565 ? O1A K1A C6A 69.5(2) . 1_565 ? O1A K1A N1A 122.4(2) . 2_677 ? N2A K1A O1A 76.6(2) . . ? N2A K1A N3A 150.2(2) . 1_565 ? N2A K1A N3A 77.97(19) . 2_677 ? N2A K1A C3A 77.34(19) . 2_677 ? N2A K1A C3A 154.07(19) . 1_565 ? N2A K1A C4A 105.6(2) . 1_565 ? N2A K1A N4A 84.28(18) . 1_565 ? N2A K1A C6A 140.5(2) . 1_565 ? N2A K1A O3A 84.9(5) . 2_777 ? N2A K1A N1A 86.8(2) . 2_677 ? N3A K1A N3A 74.7(2) 2_677 1_565 ? N3A K1A C3A 19.88(16) 2_677 2_677 ? N3A K1A C3A 21.69(18) 1_565 1_565 ? N3A K1A C3A 72.96(18) 1_565 2_677 ? N3A K1A C3A 78.10(18) 2_677 1_565 ? N3A K1A C4A 77.52(18) 2_677 1_565 ? N3A K1A C4A 79.97(19) 1_565 1_565 ? N3A K1A N4A 99.29(17) 1_565 1_565 ? N3A K1A N4A 74.08(17) 2_677 1_565 ? N3A K1A C6A 64.8(2) 1_565 1_565 ? N3A K1A C6A 116.1(2) 2_677 1_565 ? N3A K1A N1A 86.8(2) 2_677 2_677 ? N3A K1A N1A 80.1(2) 1_565 2_677 ? C3A K1A C3A 83.51(19) 1_565 2_677 ? C3A K1A C4A 59.3(2) 1_565 1_565 ? C3A K1A N4A 79.69(18) 1_565 1_565 ? C3A K1A C6A 47.5(2) 1_565 1_565 ? C4A K1A C3A 96.73(18) 1_565 2_677 ? C4A K1A N4A 21.34(18) 1_565 1_565 ? C4A K1A C6A 49.3(2) 1_565 1_565 ? N4A K1A C3A 93.83(17) 1_565 2_677 ? N4A K1A C6A 66.7(2) 1_565 1_565 ? C6A K1A C3A 128.6(2) 1_565 2_677 ? O3A K1A O1A 56.4(5) 2_777 . ? O3A K1A N3A 149.9(4) 2_777 2_677 ? O3A K1A N3A 113.8(5) 2_777 1_565 ? O3A K1A C3A 131.7(4) 2_777 2_677 ? O3A K1A C3A 121.0(5) 2_777 1_565 ? O3A K1A C4A 131.4(4) 2_777 1_565 ? O3A K1A N4A 128.9(5) 2_777 1_565 ? O3A K1A C6A 92.7(4) 2_777 1_565 ? O3A K1A N1A 67.6(5) 2_777 2_677 ? O2A K1A O1A 77.0(3) . . ? O2A K1A N2A 122.3(2) . . ? O2A K1A N3A 76.4(2) . 1_565 ? O2A K1A N3A 143.6(3) . 2_677 ? O2A K1A C3A 83.3(2) . 1_565 ? O2A K1A C3A 127.5(2) . 2_677 ? O2A K1A C4A 118.6(2) . 1_565 ? O2A K1A N4A 132.8(2) . 1_565 ? O2A K1A C6A 69.4(2) . 1_565 ? O2A K1A O3A 38.2(5) . 2_777 ? O2A K1A N1A 66.6(3) . 2_677 ? N1A K1A C3A 66.9(2) 2_677 2_677 ? N1A K1A C3A 101.7(2) 2_677 1_565 ? N1A K1A C4A 157.2(2) 2_677 1_565 ? N1A K1A N4A 160.2(2) 2_677 1_565 ? N1A K1A C6A 128.6(2) 2_677 1_565 ? K1A O1A K3A 174.0(3) . 2_766 ? K1A O1A K3A 86.07(19) . 1_565 ? K1A O1A K4A 99.5(3) . 2_776 ? K3A O1A K3A 88.0(2) 1_565 2_766 ? K4A O1A K3A 173.5(3) 2_776 1_565 ? K4A O1A K3A 86.37(18) 2_776 2_766 ? K1A N2A K3A 89.51(16) . 1_565 ? K1A N2A K4A 93.9(2) . 1_556 ? K1A N2A K4A 107.1(2) . 2_676 ? C2A N2A K1A 154.9(6) . . ? C2A N2A K3A 78.3(5) . 1_565 ? C2A N2A K4A 96.2(5) . 2_676 ? C2A N2A K4A 87.7(5) . 1_556 ? K4A N2A K3A 97.50(18) 2_676 1_565 ? K4A N2A K3A 153.1(2) 1_556 1_565 ? K4A N2A K4A 106.91(19) 1_556 2_676 ? N3A K2A C4A 155.2(2) . 1_556 ? N3A K2A C4A 77.34(18) . 2_667 ? N3A K2A N4A 154.7(2) . 1_556 ? N3A K2A N4A 79.80(19) . 2_667 ? N3A K2A K4A 50.56(14) . 1_556 ? N3A K2A C5A 109.46(19) . 1_556 ? N3A K2A N5A 88.72(19) . 1_556 ? N3A K2A C6A 89.4(2) . 2_767 ? N3A K2A N6A 75.3(2) . 2_767 ? N3A K2A N1A 83.5(2) . 2_667 ? N3A K2A C1A 80.05(19) . 2_667 ? C4A K2A C4A 87.93(19) 1_556 2_667 ? C4A K2A K4A 116.13(15) 1_556 1_556 ? C4A K2A K4A 103.69(13) 2_667 1_556 ? C4A K2A C5A 52.65(19) 1_556 1_556 ? C4A K2A C6A 104.6(2) 1_556 2_767 ? C4A K2A C6A 166.8(2) 2_667 2_767 ? C4A K2A C1A 49.3(2) 2_667 2_667 ? C4A K2A C1A 105.4(2) 1_556 2_667 ? N4A K2A C4A 21.33(18) 1_556 1_556 ? N4A K2A C4A 77.43(17) 1_556 2_667 ? N4A K2A C4A 79.60(19) 2_667 1_556 ? N4A K2A C4A 20.49(18) 2_667 2_667 ? N4A K2A N4A 76.12(18) 2_667 1_556 ? N4A K2A K4A 136.39(15) 1_556 1_556 ? N4A K2A K4A 90.50(12) 2_667 1_556 ? N4A K2A C5A 73.11(18) 1_556 1_556 ? N4A K2A C5A 78.43(19) 2_667 1_556 ? N4A K2A N5A 74.14(19) 2_667 1_556 ? N4A K2A N5A 91.97(18) 1_556 1_556 ? N4A K2A C6A 157.0(2) 2_667 2_767 ? N4A K2A C6A 115.8(2) 1_556 2_767 ? N4A K2A N1A 89.7(2) 2_667 2_667 ? N4A K2A N1A 88.8(2) 1_556 2_667 ? N4A K2A C1A 69.8(2) 2_667 2_667 ? N4A K2A C1A 84.53(19) 1_556 2_667 ? C5A K2A C4A 98.4(2) 1_556 2_667 ? C5A K2A K4A 63.52(13) 1_556 1_556 ? C5A K2A C6A 86.3(2) 1_556 2_767 ? C5A K2A C1A 144.7(2) 1_556 2_667 ? N5A K2A C4A 94.47(19) 1_556 2_667 ? N5A K2A C4A 72.51(18) 1_556 1_556 ? N5A K2A K4A 44.47(12) 1_556 1_556 ? N5A K2A C5A 20.75(16) 1_556 1_556 ? N5A K2A C6A 85.5(2) 1_556 2_767 ? N5A K2A N1A 163.1(2) 1_556 2_667 ? N5A K2A C1A 143.6(2) 1_556 2_667 ? C6A K2A K4A 67.20(16) 2_767 1_556 ? C6A K2A C1A 128.5(2) 2_767 2_667 ? N6A K2A C4A 112.0(3) 2_767 1_556 ? N6A K2A C4A 149.25(19) 2_767 2_667 ? N6A K2A N4A 137.3(2) 2_767 2_667 ? N6A K2A N4A 128.6(2) 2_767 1_556 ? N6A K2A K4A 47.06(16) 2_767 1_556 ? N6A K2A C5A 78.0(3) 2_767 1_556 ? N6A K2A N5A 71.2(2) 2_767 1_556 ? N6A K2A C6A 20.2(2) 2_767 2_767 ? N6A K2A N1A 120.7(3) 2_767 2_667 ? N6A K2A C1A 136.5(3) 2_767 2_667 ? N1A K2A C4A 109.9(2) 2_667 1_556 ? N1A K2A C4A 69.2(2) 2_667 2_667 ? N1A K2A K4A 133.15(14) 2_667 1_556 ? N1A K2A C5A 160.2(2) 2_667 1_556 ? N1A K2A C6A 109.4(3) 2_667 2_767 ? N1A K2A C1A 19.9(2) 2_667 2_667 ? C1A K2A K4A 129.78(13) 2_667 1_556 ? Mo1A C2A K3A 99.0(3) . 1_565 ? Mo1A C2A K4A 108.6(2) . 1_556 ? Mo1A C2A K4A 116.3(3) . 2_676 ? N2A C2A Mo1A 179.5(6) . . ? N2A C2A K3A 80.8(4) . 1_565 ? N2A C2A K4A 71.3(5) . 1_556 ? N2A C2A K4A 64.2(5) . 2_676 ? K3A C2A K4A 144.0(2) 1_565 1_556 ? K3A C2A K4A 91.70(17) 1_565 2_676 ? K4A C2A K4A 96.1(2) 1_556 2_676 ? K1A N3A K1A 105.3(2) 2_677 1_545 ? K1A N3A K4A 101.9(2) 2_677 1_556 ? K2A N3A K1A 97.96(18) . 1_545 ? K2A N3A K1A 105.8(2) . 2_677 ? K2A N3A K4A 84.00(18) . 1_556 ? C3A N3A K1A 98.5(5) . 2_677 ? C3A N3A K1A 80.1(5) . 1_545 ? C3A N3A K2A 155.2(6) . . ? C3A N3A K4A 86.2(5) . 1_556 ? K4A N3A K1A 151.0(3) 1_556 1_545 ? O1A K3A Mo1A 90.71(12) 2_766 1_545 ? O1A K3A Mo1A 91.77(13) 1_545 1_545 ? O1A K3A O1A 92.0(2) 1_545 2_766 ? O1A K3A C5A 146.2(2) 1_545 2_666 ? O1A K3A C1A 143.05(19) 1_545 2_666 ? O1A K3A C1A 79.0(2) 2_766 2_666 ? N2A K3A Mo1A 52.10(12) 1_545 1_545 ? N2A K3A O1A 133.80(18) 1_545 2_766 ? N2A K3A O1A 66.61(18) 1_545 1_545 ? N2A K3A C5A 94.19(17) 1_545 2_666 ? N2A K3A C1A 141.8(2) 1_545 2_666 ? C2A K3A Mo1A 31.23(15) 1_545 1_545 ? C2A K3A O1A 75.80(18) 1_545 1_545 ? C2A K3A O1A 117.47(19) 1_545 2_766 ? C2A K3A N2A 20.87(18) 1_545 1_545 ? C2A K3A C5A 96.15(18) 1_545 2_666 ? C2A K3A N5A 79.94(18) 1_545 1_545 ? C2A K3A C1A 140.0(2) 1_545 2_666 ? N4A K3A Mo1A 135.07(13) . 1_545 ? N4A K3A O1A 130.27(18) . 2_766 ? N4A K3A O1A 72.04(18) . 1_545 ? N4A K3A N2A 83.27(18) . 1_545 ? N4A K3A C2A 104.0(2) . 1_545 ? N4A K3A C5A 152.7(2) . 1_545 ? N4A K3A C5A 78.44(18) . 2_666 ? N4A K3A N5A 77.83(19) . 2_666 ? N4A K3A N5A 149.85(19) . 1_545 ? N4A K3A N1A 92.1(2) . 2_666 ? N4A K3A C1A 86.60(19) . 2_666 ? C5A K3A Mo1A 97.76(12) 2_666 1_545 ? C5A K3A Mo1A 31.15(13) 1_545 1_545 ? C5A K3A O1A 76.20(19) 1_545 2_766 ? C5A K3A O1A 119.21(18) 1_545 1_545 ? C5A K3A O1A 120.1(2) 2_666 2_766 ? C5A K3A N2A 79.79(18) 1_545 1_545 ? C5A K3A C2A 59.8(2) 1_545 1_545 ? C5A K3A C5A 81.6(2) 1_545 2_666 ? C5A K3A N5A 21.11(17) 1_545 1_545 ? C5A K3A C1A 47.6(2) 2_666 2_666 ? C5A K3A C1A 93.58(19) 1_545 2_666 ? N5A K3A Mo1A 52.26(11) 1_545 1_545 ? N5A K3A Mo1A 84.51(12) 2_666 1_545 ? N5A K3A O1A 132.7(2) 2_666 1_545 ? N5A K3A O1A 135.1(2) 2_666 2_766 ? N5A K3A O1A 68.19(19) 1_545 2_766 ? N5A K3A O1A 136.51(18) 1_545 1_545 ? N5A K3A N2A 74.44(17) 2_666 1_545 ? N5A K3A N2A 98.96(17) 1_545 1_545 ? N5A K3A C2A 77.22(17) 2_666 1_545 ? N5A K3A C5A 71.41(18) 1_545 2_666 ? N5A K3A C5A 77.10(19) 2_666 1_545 ? N5A K3A C5A 19.80(16) 2_666 2_666 ? N5A K3A N5A 73.9(2) 2_666 1_545 ? N5A K3A N1A 86.9(2) 2_666 2_666 ? N5A K3A C1A 67.4(2) 2_666 2_666 ? N5A K3A C1A 73.02(18) 1_545 2_666 ? N1A K3A Mo1A 128.07(15) 2_666 1_545 ? N1A K3A O1A 129.0(2) 2_666 1_545 ? N1A K3A O1A 61.6(2) 2_666 2_766 ? N1A K3A N2A 161.4(2) 2_666 1_545 ? N1A K3A C2A 154.2(2) 2_666 1_545 ? N1A K3A C5A 97.1(2) 2_666 1_545 ? N1A K3A C5A 67.2(2) 2_666 2_666 ? N1A K3A N5A 76.16(18) 2_666 1_545 ? N1A K3A C1A 19.6(2) 2_666 2_666 ? C1A K3A Mo1A 123.77(14) 2_666 1_545 ? Mo1A C3A K1A 118.2(2) . 2_677 ? Mo1A C3A K1A 101.3(3) . 1_545 ? Mo1A C3A K4A 108.0(3) . 1_556 ? K1A C3A K1A 96.49(19) 1_545 2_677 ? K1A C3A K4A 141.3(2) 1_545 1_556 ? N3A C3A Mo1A 179.4(7) . . ? N3A C3A K1A 61.7(5) . 2_677 ? N3A C3A K1A 78.2(5) . 1_545 ? N3A C3A K4A 72.6(5) . 1_556 ? K4A C3A K1A 91.5(2) 1_556 2_677 ? Mo1A C4A K1A 100.9(3) . 1_545 ? Mo1A C4A K2A 117.5(3) . 2_667 ? Mo1A C4A K2A 109.9(3) . 1_554 ? K1A C4A K2A 141.8(3) 1_545 1_554 ? K1A C4A K2A 93.4(2) 1_545 2_667 ? K2A C4A K2A 92.07(19) 1_554 2_667 ? N4A C4A Mo1A 179.1(6) . . ? N4A C4A K1A 80.1(4) . 1_545 ? N4A C4A K2A 62.6(5) . 2_667 ? N4A C4A K2A 69.2(4) . 1_554 ? K2A N4A K1A 100.30(19) 2_667 1_545 ? K2A N4A K1A 154.2(2) 1_554 1_545 ? K2A N4A K2A 103.88(18) 2_667 1_554 ? K3A N4A K1A 90.37(16) . 1_545 ? K3A N4A K2A 108.5(2) . 2_667 ? K3A N4A K2A 90.5(2) . 1_554 ? C4A N4A K1A 78.6(4) . 1_545 ? C4A N4A K2A 96.9(5) . 2_667 ? C4A N4A K2A 89.5(5) . 1_554 ? C4A N4A K3A 153.8(5) . . ? O1A K4A C2A 130.38(19) 2_776 1_554 ? O1A K4A C3A 136.8(2) 2_776 1_554 ? O1A K4A C1A 82.8(2) 2_776 2_676 ? N2A K4A O1A 144.5(2) 2_676 2_776 ? N2A K4A O1A 122.21(18) 1_554 2_776 ? N2A K4A N2A 73.09(19) 1_554 2_676 ? N2A K4A C2A 76.29(18) 2_676 1_554 ? N2A K4A C2A 20.99(18) 1_554 1_554 ? N2A K4A N3A 92.24(17) 1_554 1_554 ? N2A K4A C3A 73.02(18) 1_554 1_554 ? N2A K4A C3A 76.26(19) 2_676 1_554 ? N2A K4A C1A 80.47(19) 1_554 2_676 ? N2A K4A C1A 67.5(2) 2_676 2_676 ? C2A K4A C3A 52.92(18) 1_554 1_554 ? C2A K4A C1A 100.76(19) 1_554 2_676 ? N3A K4A O1A 131.67(18) 1_554 2_776 ? N3A K4A N2A 72.88(19) 1_554 2_676 ? N3A K4A C2A 73.18(17) 1_554 1_554 ? N3A K4A C3A 21.20(17) 1_554 1_554 ? N3A K4A C1A 140.2(2) 1_554 2_676 ? C3A K4A C1A 139.9(2) 1_554 2_676 ? N5A K4A O1A 76.1(2) . 2_776 ? N5A K4A N2A 79.08(19) . 2_676 ? N5A K4A N2A 149.9(2) . 1_554 ? N5A K4A C2A 153.43(19) . 1_554 ? N5A K4A N3A 90.21(19) . 1_554 ? N5A K4A C3A 111.31(19) . 1_554 ? N5A K4A N6A 75.6(2) . 2_766 ? N5A K4A O3A 129.6(5) . 1_554 ? N5A K4A O2A 133.3(2) . 2_776 ? N5A K4A N1A 83.7(2) . 2_676 ? N5A K4A C1A 78.6(2) . 2_676 ? N6A K4A O1A 60.4(2) 2_766 2_776 ? N6A K4A N2A 135.6(2) 2_766 2_676 ? N6A K4A N2A 133.3(2) 2_766 1_554 ? N6A K4A C2A 116.5(3) 2_766 1_554 ? N6A K4A N3A 71.4(2) 2_766 1_554 ? N6A K4A C3A 79.8(2) 2_766 1_554 ? N6A K4A N1A 124.9(3) 2_766 2_676 ? N6A K4A C1A 138.9(3) 2_766 2_676 ? O3A K4A O1A 53.7(5) 1_554 2_776 ? O3A K4A N2A 71.6(4) 1_554 1_554 ? O3A K4A N2A 140.9(4) 1_554 2_676 ? O3A K4A C2A 76.7(5) 1_554 1_554 ? O3A K4A N3A 124.4(6) 1_554 1_554 ? O3A K4A C3A 108.3(6) 1_554 1_554 ? O3A K4A N6A 82.2(5) 1_554 2_766 ? O3A K4A O2A 37.6(6) 1_554 2_776 ? O3A K4A N1A 73.0(6) 1_554 2_676 ? O3A K4A C1A 90.5(6) 1_554 2_676 ? O2A K4A O1A 71.2(3) 2_776 2_776 ? O2A K4A N2A 76.7(2) 2_776 1_554 ? O2A K4A N2A 142.9(2) 2_776 2_676 ? O2A K4A C2A 67.9(2) 2_776 1_554 ? O2A K4A N3A 87.5(2) 2_776 1_554 ? O2A K4A C3A 74.7(2) 2_776 1_554 ? O2A K4A N6A 59.6(2) 2_776 2_766 ? O2A K4A N1A 110.5(3) 2_776 2_676 ? O2A K4A C1A 127.6(2) 2_776 2_676 ? N1A K4A O1A 65.3(2) 2_676 2_776 ? N1A K4A N2A 87.2(2) 2_676 2_676 ? N1A K4A N2A 83.8(2) 2_676 1_554 ? N1A K4A C2A 104.7(2) 2_676 1_554 ? N1A K4A N3A 159.9(2) 2_676 1_554 ? N1A K4A C3A 154.5(2) 2_676 1_554 ? N1A K4A C1A 19.8(2) 2_676 2_676 ? Mo1A C5A K2A 107.6(3) . 1_554 ? Mo1A C5A K3A 99.7(3) . 1_565 ? Mo1A C5A K3A 118.1(3) . 2_666 ? K2A C5A K3A 89.09(18) 1_554 2_666 ? K3A C5A K2A 144.2(2) 1_565 1_554 ? K3A C5A K3A 98.4(2) 1_565 2_666 ? N5A C5A Mo1A 179.1(6) . . ? N5A C5A K2A 71.8(5) . 1_554 ? N5A C5A K3A 61.4(5) . 2_666 ? N5A C5A K3A 81.2(5) . 1_565 ? K2A N5A K3A 152.0(2) 1_554 1_565 ? K3A N5A K2A 99.51(19) 2_666 1_554 ? K3A N5A K3A 106.1(2) 2_666 1_565 ? K4A N5A K2A 84.3(2) . 1_554 ? K4A N5A K3A 97.73(18) . 1_565 ? K4A N5A K3A 109.0(2) . 2_666 ? C5A N5A K2A 87.5(5) . 1_554 ? C5A N5A K3A 98.8(5) . 2_666 ? C5A N5A K3A 77.7(5) . 1_565 ? C5A N5A K4A 151.9(6) . . ? Mo1A C6A K1A 94.2(3) . 1_545 ? Mo1A C6A K2A 124.8(3) . 2_767 ? K2A C6A K1A 140.9(3) 2_767 1_545 ? N6A C6A Mo1A 176.3(8) . . ? N6A C6A K1A 82.2(6) . 1_545 ? N6A C6A K2A 58.8(6) . 2_767 ? K2A N6A K1A 176.8(4) 2_767 1_545 ? K2A N6A K4A 86.44(19) 2_767 2_766 ? K4A N6A K1A 94.2(2) 2_766 1_545 ? C6A N6A K1A 78.2(6) . 1_545 ? C6A N6A K2A 101.1(6) . 2_767 ? C6A N6A K4A 172.1(7) . 2_766 ? N7A C7A Mo1A 173.0(10) . . ? K1A O3A K1A 161.3(7) 2_777 . ? K4A O3A K1A 85.7(5) 1_556 . ? K4A O3A K1A 109.3(6) 1_556 2_777 ? O3A O3A K1A 52.9(18) 2_777 . ? O3A O3A K1A 108.4(19) 2_777 2_777 ? O3A O3A K4A 127(3) 2_777 1_556 ? K1A O2A K4A 111.2(3) . 2_776 ? K1A N1A K2A 92.24(19) 2_677 2_667 ? K1A N1A K3A 166.7(3) 2_677 2_666 ? K3A N1A K2A 82.5(2) 2_666 2_667 ? K4A N1A K1A 88.7(2) 2_676 2_677 ? K4A N1A K2A 169.4(4) 2_676 2_667 ? K4A N1A K3A 94.4(2) 2_676 2_666 ? C1A N1A K1A 97.5(6) . 2_677 ? C1A N1A K2A 92.9(6) . 2_667 ? C1A N1A K3A 95.0(6) . 2_666 ? C1A N1A K4A 97.5(6) . 2_676 ? Mo1A C1A K1A 115.9(3) . 2_677 ? Mo1A C1A K2A 113.5(3) . 2_667 ? Mo1A C1A K3A 115.6(3) . 2_666 ? Mo1A C1A K4A 116.6(3) . 2_676 ? K2A C1A K1A 82.12(18) 2_667 2_677 ? K2A C1A K3A 74.45(18) 2_667 2_666 ? K3A C1A K1A 128.3(3) 2_666 2_677 ? K4A C1A K1A 77.7(2) 2_676 2_677 ? K4A C1A K2A 129.9(3) 2_676 2_667 ? K4A C1A K3A 83.15(19) 2_676 2_666 ? N1A C1A Mo1A 178.8(8) . . ? N1A C1A K1A 63.1(5) . 2_677 ? N1A C1A K2A 67.2(6) . 2_667 ? N1A C1A K3A 65.4(5) . 2_666 ? N1A C1A K4A 62.7(6) . 2_676 ? 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 K1A N2A C2A K3A -62.4(12) . . . 1_565 ? K1A N2A C2A K4A 94.4(12) . . . 1_556 ? K1A N2A C2A K4A -158.8(13) . . . 2_676 ? K1A N3A C3A K1A -104.1(2) 2_677 . . 1_545 ? K1A N3A C3A K1A 104.1(2) 1_545 . . 2_677 ? K1A N3A C3A K4A -154.35(19) 1_545 . . 1_556 ? K1A N3A C3A K4A 101.5(2) 2_677 . . 1_556 ? K1A C4A N4A K2A -156.91(19) 1_545 . . 1_554 ? K1A C4A N4A K2A 99.17(19) 1_545 . . 2_667 ? K1A C4A N4A K3A -66.8(11) 1_545 . . . ? K1A C6A N6A K2A 176.8(4) 1_545 . . 2_767 ? K1A N1A C1A K2A 92.6(3) 2_677 . . 2_667 ? K1A N1A C1A K3A 175.3(4) 2_677 . . 2_666 ? K1A N1A C1A K4A -89.6(3) 2_677 . . 2_676 ? K2A N3A C3A K1A 87.6(13) . . . 1_545 ? K2A N3A C3A K1A -168.3(15) . . . 2_677 ? K2A N3A C3A K4A -66.7(13) . . . 1_556 ? K2A C4A N4A K1A -99.17(19) 2_667 . . 1_545 ? K2A C4A N4A K1A 156.91(19) 1_554 . . 1_545 ? K2A C4A N4A K2A -103.9(2) 1_554 . . 2_667 ? K2A C4A N4A K2A 103.9(2) 2_667 . . 1_554 ? K2A C4A N4A K3A 90.2(11) 1_554 . . . ? K2A C4A N4A K3A -165.9(12) 2_667 . . . ? K2A C5A N5A K3A -156.1(2) 1_554 . . 1_565 ? K2A C5A N5A K3A 99.2(2) 1_554 . . 2_666 ? K2A C5A N5A K4A -72.8(11) 1_554 . . . ? K2A C6A N6A K1A -176.8(4) 2_767 . . 1_545 ? K2A N1A C1A K1A -92.6(3) 2_667 . . 2_677 ? K2A N1A C1A K3A 82.7(2) 2_667 . . 2_666 ? K2A N1A C1A K4A 177.7(4) 2_667 . . 2_676 ? K3A N2A C2A K4A 156.83(18) 1_565 . . 1_556 ? K3A N2A C2A K4A -96.40(18) 1_565 . . 2_676 ? K3A C5A N5A K2A -99.2(2) 2_666 . . 1_554 ? K3A C5A N5A K2A 156.1(2) 1_565 . . 1_554 ? K3A C5A N5A K3A 104.6(2) 2_666 . . 1_565 ? K3A C5A N5A K3A -104.6(2) 1_565 . . 2_666 ? K3A C5A N5A K4A -172.0(13) 2_666 . . . ? K3A C5A N5A K4A 83.3(12) 1_565 . . . ? K3A N1A C1A K1A -175.3(4) 2_666 . . 2_677 ? K3A N1A C1A K2A -82.7(2) 2_666 . . 2_667 ? K3A N1A C1A K4A 95.1(3) 2_666 . . 2_676 ? K4A N2A C2A K3A -156.83(18) 1_556 . . 1_565 ? K4A N2A C2A K3A 96.40(18) 2_676 . . 1_565 ? K4A N2A C2A K4A -106.8(2) 2_676 . . 1_556 ? K4A N2A C2A K4A 106.8(2) 1_556 . . 2_676 ? K4A N3A C3A K1A -101.5(2) 1_556 . . 2_677 ? K4A N3A C3A K1A 154.35(19) 1_556 . . 1_545 ? K4A N1A C1A K1A 89.6(3) 2_676 . . 2_677 ? K4A N1A C1A K2A -177.7(4) 2_676 . . 2_667 ? K4A N1A C1A K3A -95.1(3) 2_676 . . 2_666 ? _shelx_res_file ; 2_cr1_pristine_a.res created by SHELXL-2014/7 TITL shelxt_a.res in P-1 REM Old TITL shelxt in P -1 REM SHELXT solution in P-1 REM R1 0.181, Rweak 0.006, Alpha 0.065, Orientation as input REM Formula found by SHELXT: Mo K4 C8 N O8 CELL 0.6889 8.9957 9.3395 9.7432 86.908 82.149 70.48 ZERR 2 0.001 0.0011 0.0012 0.011 0.011 0.01 LATT 1 SFAC C K Mo N O DISP C 0.003 0.002 10.637 DISP K 0.194 0.239 950.887 DISP Mo -1.875 0.662 2734.371 DISP N 0.006 0.003 18.026 DISP O 0.011 0.006 29.595 UNIT 14 8 2 14 4 L.S. 50 PLAN 1 SIZE 0.01 0.03 0.05 TEMP -243.1(10) CONF list 4 MORE -1 BOND $H fmap 2 acta SHEL 99999 0.6 REM REM REM WGHT 0.052800 8.839900 FVAR 0.40058 0.66460 MO1A 3 0.713607 0.687336 0.725980 11.00000 0.04283 0.01185 = 0.00975 -0.00050 -0.00707 -0.00470 PART 4 K1A 2 0.723666 1.279242 0.917228 11.00000 0.02564 0.01494 = 0.01468 -0.00034 -0.00463 -0.00588 O1A 5 0.991634 1.109648 0.719386 11.00000 0.04124 0.03258 = 0.09003 0.00851 0.00394 -0.00675 N2A 4 0.643112 1.026499 0.857050 11.00000 0.02432 0.01534 = 0.01678 -0.00118 0.00066 -0.00788 K2A 2 0.710717 0.485390 1.325814 11.00000 0.02144 0.01501 = 0.01121 0.00058 -0.00210 -0.00191 C2A 1 0.666977 0.908341 0.811430 11.00000 0.01587 0.01844 = 0.01085 0.00067 0.00080 -0.00873 N3A 4 0.635262 0.591954 1.056285 11.00000 0.03232 0.01629 = 0.01750 0.00101 -0.01119 -0.00700 K3A 2 0.724361 0.086283 0.533893 11.00000 0.03788 0.01344 = 0.01724 0.00150 -0.00029 -0.00588 C3A 1 0.663027 0.625985 0.940867 11.00000 0.01890 0.01010 = 0.01672 -0.00415 -0.00838 -0.00116 C4A 1 0.665009 0.492890 0.656810 11.00000 0.02341 0.01405 = 0.00784 -0.00033 -0.00237 0.00417 N4A 4 0.639005 0.389204 0.617786 11.00000 0.02258 0.01516 = 0.01031 0.00054 -0.00304 -0.00180 K4A 2 0.722826 0.867565 0.132369 11.00000 0.03155 0.01725 = 0.01497 0.00133 -0.00083 -0.00787 C5A 1 0.661677 0.775085 0.522704 11.00000 0.02128 0.01347 = 0.01394 -0.00600 -0.00034 -0.00767 N5A 4 0.632487 0.821148 0.412978 11.00000 0.03235 0.01637 = 0.01476 -0.00020 -0.00273 -0.00874 C6A 1 0.922447 0.510044 0.766339 11.00000 0.03947 0.03222 = 0.02991 0.00505 -0.00317 -0.01766 N6A 4 1.032099 0.409290 0.793515 11.00000 0.01237 0.06010 = 0.05503 0.01890 0.00121 -0.00132 PART 2 C7A 1 0.918005 0.750732 0.638544 11.00000 0.03421 0.03342 = 0.03855 0.00865 -0.00779 -0.00018 PART 4 O3A 5 0.991974 0.941149 1.002613 -21.00000 0.02744 0.08010 = 0.06048 0.03825 -0.01653 -0.03916 O2A 5 0.984296 1.252887 1.050466 21.00000 0.02422 0.03599 = 0.02593 0.00159 -0.00756 -0.00565 PART 2 N7A 4 1.018252 0.799316 0.596852 11.00000 0.00980 0.04901 = 0.11262 0.02334 0.00682 -0.01260 PART 4 N1A 4 0.316351 0.816343 0.774287 11.00000 0.07043 0.03585 = 0.01869 -0.00219 -0.00859 -0.03417 C1A 1 0.453401 0.771433 0.756115 11.00000 0.04578 0.01643 = 0.01261 -0.00082 -0.00384 -0.01544 HKLF 4 REM shelxt_a.res in P-1 REM R1 = 0.0788 for 2484 Fo > 4sig(Fo) and 0.1220 for all 4033 data REM 200 parameters refined using 0 restraints END WGHT 0.0546 8.7680 REM Highest difference peak 6.205, deepest hole -2.444, 1-sigma level 0.221 Q1 1 0.6209 0.6927 0.7471 11.00000 0.05 6.21 ; _shelx_res_checksum 55503 _shelx_hkl_file ; -12 -2 1 1.77 14.54 -11 -9 1 7.11 16.22 -11 -8 1 5.28 16.28 11 8 -2 4.22 9.67 -11 -7 1 97.65 23.26 -11 -7 1 132.58 19.54 11 7 -1 179.41 17.11 11 7 -1 139.88 19.08 -11 -7 2 0.30 16.52 -11 -7 2 11.80 9.65 11 7 -2 3.82 9.66 -11 -7 3 4.69 9.46 11 7 -3 17.62 9.97 -11 -6 1 5.47 8.15 -11 -6 1 -3.69 15.25 -11 -6 1 8.50 10.24 11 6 -1 10.77 4.87 11 6 -1 7.60 7.53 -11 -6 2 0.00 8.52 -11 -6 2 -13.29 15.99 -11 -6 2 0.00 9.29 11 6 -2 0.25 4.62 11 6 -2 5.00 9.04 -11 -6 3 10.89 9.52 -11 -6 3 13.49 15.52 -11 -6 3 14.43 9.90 11 6 -3 10.53 5.06 11 6 -3 8.10 10.25 -11 -5 1 5.25 8.19 -11 -5 1 2.64 13.27 -11 -5 1 9.70 10.46 11 5 -1 8.19 5.25 11 5 -1 2.70 7.25 -11 -5 2 8.49 9.15 -11 -5 2 0.30 13.75 -11 -5 2 7.39 10.16 11 5 -2 14.81 5.68 -11 -5 3 2.09 9.23 -11 -5 3 2.62 13.97 -11 -5 3 1.49 9.69 11 5 -3 0.86 4.99 -11 -5 4 26.88 14.77 -11 -5 4 29.93 11.45 -11 -4 1 23.51 8.80 -11 -4 1 14.45 11.76 -11 -4 1 9.45 20.70 -11 -4 1 24.31 11.09 11 4 -1 26.69 6.73 11 4 -1 13.69 7.49 -11 -4 2 20.92 9.37 -11 -4 2 -4.67 11.71 -11 -4 2 4.63 11.03 11 4 -2 12.37 5.68 -11 -4 3 42.79 10.53 -11 -4 3 18.64 12.78 -11 -4 3 19.20 11.27 11 4 -3 27.22 6.65 -11 -4 4 2.78 12.53 -11 -4 4 0.00 10.32 -11 -4 5 23.73 13.59 11 4 -5 25.27 13.94 -11 -3 1 11.79 7.89 -11 -3 1 0.03 9.98 -11 -3 1 0.00 16.75 -11 -3 1 11.39 11.57 11 3 -1 4.26 5.96 -11 -3 2 56.93 11.41 -11 -3 2 50.75 12.77 -11 -3 2 38.37 13.47 11 3 -2 68.39 9.34 -11 -3 3 7.45 9.29 -11 -3 3 -3.38 10.89 -11 -3 3 3.17 11.07 -11 -3 4 75.88 14.44 -11 -3 4 64.53 14.61 11 3 -4 71.50 20.98 -11 -2 1 228.75 23.97 -11 -2 1 212.33 24.46 -11 -2 1 198.96 27.87 -11 -2 1 180.05 25.74 11 2 -1 194.93 22.27 -11 -2 2 10.45 8.58 -11 -2 2 5.23 10.17 -11 -2 2 18.69 12.69 11 2 -2 2.45 6.91 -11 -2 3 35.35 12.12 -11 -2 3 23.20 12.40 11 2 -3 23.08 19.47 -11 -2 4 4.18 10.71 11 2 -4 5.31 19.31 -11 -1 1 16.98 7.92 -11 -1 1 21.73 9.94 -11 -1 1 12.93 12.75 -11 -1 1 17.68 12.85 11 1 -1 11.02 8.02 -11 -1 2 10.50 8.23 -11 -1 2 1.01 9.84 -11 -1 2 4.90 13.17 11 1 -2 1.30 19.28 -11 -1 3 158.76 20.04 11 1 -3 125.28 27.07 -11 0 1 2.79 8.24 -11 0 1 6.39 8.87 -11 0 1 0.00 11.18 -11 0 1 8.14 14.49 11 0 -1 16.73 20.76 -11 0 2 12.29 9.25 -11 0 2 -5.14 10.32 -11 0 2 5.70 13.55 11 0 -2 0.87 19.48 11 0 -3 5.71 18.65 -11 1 1 0.64 15.57 11 -1 -1 12.95 22.36 11 -1 -2 -0.69 20.60 -10 -10 1 21.20 17.22 -10 -10 2 7.28 16.68 -10 -9 1 -3.58 16.05 -10 -9 1 -3.88 8.00 10 9 -1 -1.04 4.05 10 9 -1 2.49 3.94 -10 -9 2 43.87 17.75 -10 -9 2 84.37 11.30 10 9 -2 53.59 13.16 -10 -9 3 -7.21 16.58 10 9 -3 1.31 10.19 -10 -8 1 14.16 16.04 -10 -8 1 19.55 8.25 -10 -8 2 0.27 15.49 -10 -8 2 0.00 7.52 10 8 -2 4.82 3.54 10 8 -2 -1.26 9.37 -10 -8 3 35.34 17.97 -10 -8 3 21.50 8.43 10 8 -3 26.17 4.95 10 8 -3 12.72 10.51 -10 -8 4 20.64 16.94 10 8 -4 0.00 9.94 -10 -7 1 0.34 15.13 -10 -7 1 -2.60 8.27 10 7 -1 -2.69 4.25 10 7 -1 0.06 7.37 -10 -7 2 5.58 16.50 -10 -7 2 4.13 8.59 10 7 -2 13.23 4.38 10 7 -2 6.75 9.22 -10 -7 3 6.73 10.55 -10 -7 3 15.54 16.55 -10 -7 3 4.43 7.78 10 7 -3 2.40 4.12 10 7 -3 7.89 9.21 -10 -7 4 6.59 9.42 -10 -7 4 0.50 16.75 -10 -7 4 5.47 7.59 10 7 -4 13.77 4.62 10 7 -4 7.15 9.84 -10 -7 5 8.68 10.01 -10 -7 5 12.71 17.12 10 7 -5 5.36 4.25 10 7 -5 8.22 11.01 -10 -6 1 24.09 8.97 -10 -6 1 6.14 15.07 -10 -6 1 8.18 20.27 -10 -6 1 10.37 8.84 10 6 -1 15.44 4.68 10 6 -1 17.81 7.60 -10 -6 2 4.08 8.60 -10 -6 2 9.62 14.80 -10 -6 2 4.75 8.51 10 6 -2 11.23 4.58 10 6 -2 6.32 9.93 -10 -6 3 193.97 19.41 -10 -6 3 122.83 17.79 10 6 -3 135.35 15.21 10 6 -3 124.17 18.69 -10 -6 4 9.68 9.77 -10 -6 4 8.36 15.90 -10 -6 4 22.56 9.64 10 6 -4 18.58 5.06 10 6 -4 30.31 11.38 -10 -6 5 14.76 10.13 -10 -6 5 3.22 16.20 -10 -6 5 6.67 8.54 10 6 -5 9.73 11.00 -10 -6 6 11.67 17.14 10 6 -6 6.53 6.54 -10 -5 1 20.48 9.15 -10 -5 1 13.00 13.18 -10 -5 1 16.20 21.83 -10 -5 1 7.63 9.67 10 5 -1 13.09 5.30 10 5 -1 10.92 7.12 -10 -5 2 20.62 9.62 -10 -5 2 17.90 13.38 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44.52 5.72 8 10 -2 33.07 6.33 8 10 -2 16.41 10.01 8 10 -2 15.55 11.70 -8 -10 3 5.35 16.45 8 10 -3 -0.39 3.58 8 10 -3 -0.92 4.59 8 10 -3 -9.24 9.94 8 10 -3 -10.85 12.52 -8 -10 4 0.00 16.74 8 10 -4 0.72 4.37 8 10 -4 -0.14 11.35 8 10 -4 7.25 13.34 -8 -9 1 -1.84 15.58 8 9 -1 2.33 3.83 8 9 -1 2.23 4.72 8 9 -1 -1.95 7.88 -8 -9 2 254.96 35.55 8 9 -2 350.45 30.62 8 9 -2 294.18 30.91 8 9 -2 234.62 33.19 8 9 -2 270.12 34.90 -8 -9 3 14.74 16.50 8 9 -3 21.01 4.63 8 9 -3 17.47 5.26 8 9 -3 12.92 10.45 8 9 -3 13.11 10.48 -8 -9 4 38.18 18.25 8 9 -4 62.18 7.50 8 9 -4 55.96 7.76 8 9 -4 45.74 12.34 8 9 -4 47.96 13.29 -8 -9 5 1.51 17.01 8 9 -5 3.09 3.93 8 9 -5 0.00 3.91 8 9 -5 -3.16 11.88 8 9 -5 1.16 11.05 -8 -8 1 9.86 15.67 -8 -8 1 12.16 31.46 -8 -8 1 6.49 6.13 8 8 -1 23.73 4.66 8 8 -1 11.37 4.91 8 8 -1 10.08 7.04 -8 -8 2 0.00 15.00 -8 -8 2 -0.05 5.51 8 8 -2 1.16 3.81 8 8 -2 0.00 4.12 8 8 -2 4.77 9.06 -8 -8 3 1.76 15.75 8 8 -3 1.21 3.86 8 8 -3 2.83 3.79 8 8 -3 6.71 9.39 -8 -8 4 32.06 17.83 8 8 -4 60.19 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2 143.05 27.05 0 9 -2 110.58 22.14 0 9 -2 132.73 22.53 0 -9 3 35.08 17.17 0 -9 3 51.00 24.54 0 -9 3 43.89 18.53 0 9 -3 47.83 15.77 0 9 -3 41.50 18.07 0 -9 4 38.00 17.95 0 -9 4 31.63 22.26 0 9 -4 47.83 7.92 0 9 -4 29.39 13.60 0 9 -4 29.80 17.43 0 -9 5 2.53 7.94 0 -9 5 4.54 7.83 0 -9 5 -11.40 17.00 0 -9 5 -2.40 19.51 0 9 -5 -3.06 5.94 0 9 -5 2.89 18.00 0 -9 6 68.67 12.19 0 -9 6 57.05 11.02 0 -9 6 47.18 18.82 0 9 -6 65.75 8.81 0 9 -6 26.41 18.52 0 -9 7 452.26 51.15 0 -9 7 438.33 50.89 0 -9 7 525.24 70.13 0 9 -7 511.32 48.25 0 9 -7 474.54 53.57 0 -9 8 71.69 12.09 0 -9 8 51.36 11.39 0 -9 8 23.86 24.27 0 9 -8 53.41 7.52 0 9 -8 42.32 18.31 0 9 -9 55.05 19.96 0 -8 1 25.44 22.98 0 -8 1 0.95 24.09 0 8 -1 17.86 15.99 0 -8 2 -2.65 13.83 0 -8 2 -1.84 19.81 0 -8 2 2.33 21.69 0 8 -2 -2.96 5.75 0 -8 3 34.91 17.54 0 8 -3 26.89 17.31 0 -8 4 687.69 71.72 0 -8 4 608.36 70.26 0 -8 4 626.07 74.28 0 8 -4 713.79 66.95 0 8 -4 644.98 70.92 0 -8 5 25.24 9.44 0 -8 5 31.29 9.23 0 -8 5 24.58 21.86 0 8 -5 33.52 6.95 0 8 -5 48.11 18.27 0 -8 6 60.12 12.78 0 -8 6 56.92 11.60 0 -8 6 37.96 22.79 0 8 -6 66.37 8.65 0 8 -6 116.27 18.40 0 8 -6 45.32 18.78 0 -8 7 40.89 11.86 0 -8 7 42.49 10.01 0 -8 7 34.61 21.99 0 8 -7 40.35 6.42 0 8 -7 42.94 16.64 0 8 -7 32.36 17.60 0 -8 8 6.52 10.81 0 -8 8 2.73 8.10 0 -8 8 1.71 20.64 0 8 -8 1.05 4.27 0 8 -8 4.26 17.88 0 8 -8 20.19 16.87 0 -8 9 280.90 30.15 0 -8 9 269.33 38.65 0 8 -9 266.65 27.11 0 8 -9 277.85 35.49 0 8 -9 264.13 34.24 0 8 -10 24.04 18.97 0 -7 1 1258.80 147.08 0 -7 1 1423.53 151.64 0 -7 1 1319.56 152.65 0 7 -1 1531.08 143.95 0 7 -1 1531.07 149.45 0 7 -1 1649.06 147.73 0 -7 2 118.19 19.50 0 -7 2 115.28 22.50 0 -7 2 81.37 24.91 0 7 -2 93.42 12.22 0 7 -2 98.55 18.83 0 7 -2 114.73 14.87 0 7 -2 118.66 19.57 0 -7 3 207.27 23.52 0 -7 3 199.68 23.46 0 -7 3 174.84 27.73 0 -7 3 233.33 31.58 0 7 -3 193.17 21.46 0 7 -3 216.70 26.64 0 7 -3 199.30 23.94 0 7 -3 222.98 27.62 0 -7 4 10.87 18.66 0 -7 4 9.65 13.17 0 7 -4 8.05 10.87 0 7 -4 17.39 11.46 0 -7 5 12.49 8.97 0 -7 5 10.18 8.33 0 7 -5 20.67 5.66 0 7 -5 7.94 9.48 0 7 -5 8.11 12.30 0 7 -5 33.82 15.95 0 -7 6 662.01 68.11 0 -7 6 658.12 67.63 0 -7 6 609.38 73.30 0 7 -6 701.89 65.95 0 7 -6 616.65 70.40 0 -7 7 14.54 6.46 0 -7 7 7.58 7.16 0 -7 7 0.00 19.20 0 7 -7 10.81 4.51 0 7 -7 -2.82 15.10 0 7 -7 0.01 15.53 0 -7 8 103.69 12.65 0 -7 8 91.17 14.83 0 -7 8 84.04 12.93 0 -7 8 146.13 25.47 0 7 -8 82.75 9.92 0 7 -8 77.96 20.78 0 7 -8 55.18 19.63 0 -7 9 15.78 8.07 0 -7 9 15.10 8.18 0 -7 9 21.16 22.15 0 7 -9 12.21 3.75 0 7 -9 1.92 17.61 0 7 -9 7.89 15.58 0 -7 10 31.24 8.31 0 -7 10 23.38 8.30 0 -7 10 19.96 23.79 0 7 -10 23.71 18.35 0 7 -10 29.17 16.59 0 -7 11 12.96 23.93 0 -6 1 93.71 15.18 0 -6 1 77.10 19.76 0 -6 1 82.32 25.58 0 6 -1 74.95 10.05 0 6 -1 90.50 19.34 0 6 -1 84.11 11.73 0 6 -1 101.18 16.66 0 -6 2 81.97 11.02 0 -6 2 78.05 11.09 0 -6 2 57.82 15.60 0 -6 2 91.50 23.19 0 6 -2 61.27 9.04 0 6 -2 73.82 16.06 0 6 -2 69.65 11.87 0 6 -2 87.14 16.20 0 -6 3 1115.95 107.96 0 -6 3 996.03 107.22 0 -6 3 1054.36 119.40 0 -6 3 1028.01 112.45 0 6 -3 1148.46 105.40 0 6 -3 1011.56 107.66 0 6 -3 1083.93 107.00 0 6 -3 1048.70 107.92 0 -6 4 3.77 8.33 0 -6 4 6.49 7.45 0 -6 4 4.77 17.96 0 -6 4 8.80 11.01 0 6 -4 7.36 5.30 0 6 -4 13.72 10.00 0 6 -4 9.99 11.46 0 6 -4 18.55 14.53 0 -6 5 108.35 14.49 0 -6 5 94.60 12.49 0 -6 5 125.84 22.84 0 6 -5 74.66 13.02 0 6 -5 95.47 17.00 0 6 -5 97.67 19.14 0 -6 6 6.83 9.35 0 -6 6 2.59 18.99 0 6 -6 -1.30 4.50 0 6 -6 -2.77 14.12 0 -6 7 132.14 16.73 0 -6 7 138.75 16.63 0 6 -7 145.70 15.36 0 6 -7 153.15 22.82 0 6 -7 189.95 24.60 0 -6 8 63.04 9.27 0 -6 8 46.85 9.06 0 -6 8 32.90 21.93 0 6 -8 48.54 6.37 0 6 -8 30.46 15.77 0 6 -8 32.70 17.46 0 -6 9 2.69 7.67 0 -6 9 3.60 6.76 0 -6 9 10.51 21.66 0 6 -9 1.17 2.89 0 6 -9 4.26 15.38 0 6 -9 2.72 15.61 0 -6 10 26.33 8.10 0 -6 10 19.50 7.47 0 6 -10 0.66 17.50 0 -6 11 14.96 8.90 0 6 -11 0.17 19.10 0 -5 1 29.03 6.56 0 -5 1 31.08 7.49 0 -5 1 26.05 12.52 0 -5 1 0.00 13.86 0 -5 1 19.84 25.48 0 5 -1 25.68 5.64 0 5 -1 25.73 15.65 0 5 -1 26.30 12.42 0 -5 2 233.95 25.64 0 -5 2 248.80 26.05 0 -5 2 241.40 32.06 0 -5 2 264.38 34.04 0 5 -2 228.47 24.55 0 5 -2 245.19 28.64 0 5 -2 238.09 26.03 0 5 -2 259.41 29.05 0 -5 3 9.64 7.99 0 -5 3 17.70 5.98 0 -5 3 14.57 15.42 0 -5 3 37.16 14.03 0 5 -3 9.44 4.91 0 5 -3 12.87 10.11 0 5 -3 6.05 8.66 0 5 -3 16.46 13.15 0 -5 4 224.49 25.67 0 -5 4 233.69 24.50 0 -5 4 268.24 31.00 0 5 -4 222.81 23.89 0 5 -4 220.74 25.65 0 5 -4 243.62 26.81 0 5 -4 259.89 29.15 0 -5 5 158.58 20.17 0 -5 5 164.76 18.34 0 -5 5 166.44 26.10 0 5 -5 181.48 17.88 0 5 -5 160.41 18.74 0 5 -5 177.03 21.92 0 5 -5 144.83 23.71 0 -5 6 9.86 9.20 0 -5 6 11.10 6.18 0 -5 6 13.35 17.88 0 5 -6 12.98 4.17 0 5 -6 20.53 12.66 0 5 -6 20.23 14.50 0 -5 7 110.43 20.95 0 5 -7 56.11 17.30 0 -5 8 1.16 6.20 0 -5 8 -1.10 5.98 0 -5 8 -1.82 17.97 0 5 -8 -0.44 2.93 0 5 -8 -6.34 15.81 0 5 -8 -6.07 15.69 0 -5 9 26.37 7.55 0 -5 9 19.30 6.59 0 5 -9 12.96 16.63 0 5 -9 20.26 15.47 0 -5 10 197.37 22.50 0 -5 10 194.59 21.54 0 5 -10 209.63 29.14 0 -5 11 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10 9 4 10.32 11.51 -10 -9 -4 12.84 32.25 10 9 5 65.07 22.96 -10 -9 -5 19.29 35.03 -10 -9 -6 4.93 36.11 10 10 0 149.63 16.31 10 10 1 20.73 5.25 10 10 1 19.82 5.01 10 10 1 27.14 8.90 -10 -10 -1 3.29 41.40 -10 -10 -1 12.60 8.00 10 10 2 38.56 6.15 10 10 2 21.30 9.65 -10 -10 -2 4.02 37.28 -10 -10 -2 28.00 9.25 10 10 3 1.59 18.85 10 10 3 8.09 9.91 -10 -10 -3 -18.55 37.17 -10 -10 -3 8.63 8.95 10 10 4 -11.94 20.08 -10 -10 -4 7.93 37.84 -10 -11 -1 5.28 43.81 11 -2 0 26.53 25.78 11 -2 1 26.28 27.37 11 -1 0 0.64 8.75 11 -1 0 -3.48 23.37 -11 1 0 -0.78 6.61 -11 1 0 1.97 15.85 11 -1 1 0.30 9.43 -11 1 -1 0.11 7.17 -11 1 -1 3.22 9.28 -11 1 -1 19.06 17.42 -11 1 -2 12.30 7.93 -11 1 -2 4.30 9.09 11 -1 3 120.49 16.70 -11 1 -3 114.76 15.82 -11 1 -3 94.24 17.68 11 -1 4 1.97 11.09 -11 1 -4 0.00 8.70 11 0 0 203.38 22.58 -11 0 0 198.89 22.34 -11 0 0 198.63 24.23 -11 0 0 191.04 26.26 -11 0 0 166.77 25.38 11 0 1 0.47 8.22 -11 0 -1 0.82 6.65 -11 0 -1 1.73 8.78 -11 0 -1 0.00 9.97 -11 0 -1 1.85 13.96 11 0 2 9.94 8.76 11 0 2 21.54 10.07 -11 0 -2 20.33 7.18 -11 0 -2 17.09 8.81 -11 0 -2 10.58 11.85 -11 0 -2 -1.33 15.14 11 0 3 21.33 9.50 11 0 3 29.67 11.21 -11 0 -3 34.89 7.86 -11 0 -3 28.17 10.05 -11 0 -3 27.63 12.90 -11 0 -3 28.08 16.68 11 0 4 -0.34 9.03 11 0 4 1.53 11.01 -11 0 -4 -0.27 6.71 -11 0 -4 -3.22 9.20 -11 0 -4 -9.37 13.25 -11 0 -4 4.90 18.44 11 0 5 110.89 19.73 -11 0 -5 138.28 17.29 -11 0 -5 126.42 21.04 11 1 0 -4.78 7.43 -11 -1 0 3.38 8.37 -11 -1 0 4.23 9.17 -11 -1 0 9.34 12.06 -11 -1 0 4.88 11.90 11 1 1 14.90 8.35 11 1 1 14.89 9.63 -11 -1 -1 16.77 7.54 -11 -1 -1 22.44 10.01 -11 -1 -1 15.23 13.18 -11 -1 -1 -0.72 12.79 11 1 2 199.38 22.07 11 1 2 173.98 22.72 -11 -1 -2 198.55 22.05 -11 -1 -2 201.23 23.34 -11 -1 -2 180.80 26.00 -11 -1 -2 203.67 26.35 11 1 3 14.35 8.25 11 1 3 23.43 11.02 -11 -1 -3 13.71 6.91 -11 -1 -3 7.12 9.49 -11 -1 -3 14.50 14.12 -11 -1 -3 13.28 14.82 11 1 4 64.79 10.59 11 1 4 54.09 13.39 -11 -1 -4 59.91 9.87 -11 -1 -4 56.03 11.66 -11 -1 -4 33.87 16.14 -11 -1 -4 40.81 17.22 11 1 5 4.68 8.66 11 1 5 2.23 12.15 -11 -1 -5 3.99 6.14 -11 -1 -5 0.00 9.36 -11 -1 -5 3.89 15.86 -11 -1 -5 8.52 15.57 11 1 6 18.46 8.65 11 1 6 15.28 13.42 -11 -1 -6 23.31 17.76 11 2 0 9.82 7.11 -11 -2 0 11.65 7.53 -11 -2 0 9.30 9.76 -11 -2 0 3.22 13.88 -11 -2 0 7.58 11.39 11 2 1 54.58 9.29 11 2 1 57.46 11.51 -11 -2 -1 62.36 10.57 -11 -2 -1 51.08 11.76 -11 -2 -1 39.87 16.25 -11 -2 -1 41.68 14.43 11 2 2 4.40 6.52 11 2 2 0.00 9.70 -11 -2 -2 5.16 6.57 -11 -2 -2 -2.16 9.68 -11 -2 -2 -8.21 13.82 -11 -2 -2 0.00 13.02 11 2 3 90.28 12.49 11 2 3 106.49 15.18 -11 -2 -3 92.56 12.70 -11 -2 -3 76.05 14.05 -11 -2 -3 108.30 20.46 -11 -2 -3 90.84 17.38 11 2 4 20.39 7.78 11 2 4 11.86 11.74 -11 -2 -4 46.47 8.22 -11 -2 -4 15.17 10.59 -11 -2 -4 10.14 17.93 -11 -2 -4 14.91 13.57 11 2 5 13.40 7.30 11 2 5 10.38 12.09 -11 -2 -5 6.50 6.86 -11 -2 -5 5.07 17.67 -11 -2 -5 6.77 14.34 11 2 6 11.56 7.75 11 2 6 7.40 12.65 -11 -2 -6 14.47 5.69 -11 -2 -6 8.62 20.29 -11 -2 -6 19.62 16.14 11 2 7 -1.70 7.37 11 2 7 -1.61 14.62 -11 -2 -7 -1.84 5.32 -11 -2 -7 11.90 20.85 -11 -2 -7 0.00 17.65 11 3 0 18.90 6.41 11 3 0 20.90 8.34 -11 -3 0 18.17 8.60 -11 -3 0 2.83 10.07 -11 -3 0 10.14 17.95 -11 -3 0 13.31 12.14 11 3 1 9.84 6.22 11 3 1 5.29 9.25 -11 -3 -1 11.71 7.35 -11 -3 -1 5.61 10.57 -11 -3 -1 6.98 17.08 -11 -3 -1 9.55 11.68 11 3 2 18.39 6.80 11 3 2 11.01 10.42 -11 -3 -2 22.17 7.36 -11 -3 -2 5.68 10.47 -11 -3 -2 8.61 17.50 -11 -3 -2 12.93 12.19 11 3 3 18.83 6.87 11 3 3 25.49 11.25 -11 -3 -3 20.40 7.40 -11 -3 -3 22.90 11.67 -11 -3 -3 -9.65 19.79 -11 -3 -3 18.81 12.83 11 3 4 1.43 5.88 11 3 4 -3.71 11.90 -11 -3 -4 0.44 6.95 -11 -3 -4 0.00 11.74 -11 -3 -4 -3.41 18.92 -11 -3 -4 2.65 13.02 11 3 5 4.78 6.79 11 3 5 15.38 12.92 -11 -3 -5 11.17 6.77 -11 -3 -5 22.97 20.62 -11 -3 -5 0.81 14.18 11 3 6 17.81 12.38 -11 -3 -6 3.24 5.26 -11 -3 -6 27.93 21.94 -11 -3 -6 3.83 13.70 11 3 7 0.00 7.86 11 3 7 5.84 14.69 -11 -3 -7 5.29 22.25 -11 -3 -7 10.23 15.99 11 4 0 1.83 5.55 11 4 0 -1.39 8.15 -11 -4 0 10.58 7.98 -11 -4 0 0.19 11.90 -11 -4 0 2.96 19.35 -11 -4 0 9.33 10.91 11 4 1 2.36 5.25 11 4 1 1.69 9.20 -11 -4 -1 -0.30 6.94 -11 -4 -1 2.68 11.76 -11 -4 -1 -7.05 20.47 -11 -4 -1 1.39 10.73 11 4 2 -3.25 5.53 11 4 2 3.61 10.41 -11 -4 -2 1.61 6.73 -11 -4 -2 -4.28 12.20 -11 -4 -2 0.01 20.34 -11 -4 -2 8.42 11.14 11 4 3 6.73 5.96 11 4 3 17.20 11.19 -11 -4 -3 12.25 7.08 -11 -4 -3 10.01 13.16 -11 -4 -3 18.07 22.14 -11 -4 -3 15.24 11.67 11 4 4 6.13 5.89 11 4 4 -0.44 11.04 -11 -4 -4 4.89 6.29 -11 -4 -4 13.88 22.45 -11 -4 -4 -5.51 11.75 11 4 5 5.24 6.14 11 4 5 -1.67 11.71 -11 -4 -5 -0.75 6.50 -11 -4 -5 -2.52 20.67 -11 -4 -5 5.54 12.43 11 4 6 0.14 9.30 11 4 6 -2.20 12.50 -11 -4 -6 -1.23 4.80 -11 -4 -6 17.31 22.14 -11 -4 -6 1.15 12.83 11 4 7 -5.55 8.97 11 4 7 0.00 13.87 -11 -4 -7 0.00 21.58 -11 -4 -7 5.94 14.38 11 4 8 159.59 24.65 11 5 0 16.32 5.75 11 5 0 17.40 8.25 -11 -5 0 14.37 8.03 -11 -5 0 18.02 13.56 -11 -5 0 20.94 23.47 -11 -5 0 21.06 11.39 11 5 1 1.29 5.17 11 5 1 -1.67 8.91 -11 -5 -1 0.97 6.59 -11 -5 -1 0.65 13.01 -11 -5 -1 -0.04 21.93 -11 -5 -1 5.29 10.71 11 5 2 11.03 6.23 11 5 2 10.14 9.93 -11 -5 -2 12.34 7.32 -11 -5 -2 10.53 14.35 -11 -5 -2 27.97 20.51 -11 -5 -2 12.92 11.48 11 5 3 6.37 5.38 11 5 3 3.98 10.52 -11 -5 -3 0.89 6.67 -11 -5 -3 -16.88 21.85 -11 -5 -3 -1.71 11.20 11 5 4 8.63 5.70 11 5 4 -0.53 11.42 -11 -5 -4 8.06 6.66 -11 -5 -4 0.00 20.91 -11 -5 -4 6.21 11.55 11 5 5 135.35 20.25 -11 -5 -5 158.82 18.36 -11 -5 -5 140.06 30.78 -11 -5 -5 144.64 21.21 11 5 6 4.65 10.10 11 5 6 -7.61 13.43 -11 -5 -6 -1.14 21.55 -11 -5 -6 -5.48 12.91 11 5 7 27.67 10.80 11 5 7 18.44 14.69 -11 -5 -7 15.76 22.28 11 6 0 4.97 5.05 11 6 0 9.14 7.81 -11 -6 0 17.21 8.10 -11 -6 0 5.15 14.71 -11 -6 0 10.02 21.24 -11 -6 0 0.00 9.64 11 6 1 4.26 4.94 11 6 1 2.74 8.96 -11 -6 -1 12.85 7.46 -11 -6 -1 3.05 15.27 -11 -6 -1 -4.28 21.31 -11 -6 -1 1.32 9.95 11 6 2 174.86 17.72 11 6 2 159.90 20.54 -11 -6 -2 103.25 22.89 -11 -6 -2 78.76 28.94 -11 -6 -2 183.22 22.04 11 6 3 0.71 5.54 11 6 3 13.51 10.61 -11 -6 -3 17.43 21.04 -11 -6 -3 5.09 11.14 11 6 4 28.45 11.75 -11 -6 -4 10.32 21.83 -11 -6 -4 25.41 12.07 11 6 5 2.24 11.46 -11 -6 -5 20.70 22.88 -11 -6 -5 2.18 11.46 11 6 6 1.46 11.34 11 6 6 6.04 13.43 -11 -6 -6 -3.53 23.40 -11 -6 -6 9.02 12.18 -11 -6 -7 58.66 26.48 11 7 0 0.00 4.41 11 7 0 -0.63 7.64 -11 -7 0 -1.62 15.50 -11 -7 0 9.42 21.29 -11 -7 0 2.84 9.38 11 7 1 24.63 6.04 11 7 1 21.32 9.21 -11 -7 -1 12.17 15.68 -11 -7 -1 31.82 23.66 -11 -7 -1 26.56 10.79 11 7 2 11.94 5.01 11 7 2 12.60 10.24 -11 -7 -2 2.23 21.89 -11 -7 -2 3.79 10.19 11 7 3 9.66 5.10 11 7 3 3.42 10.40 -11 -7 -3 0.84 22.42 -11 -7 -3 6.22 10.83 11 7 4 152.83 17.97 -11 -7 -4 67.05 28.17 -11 -7 -4 93.80 17.52 11 7 5 31.69 14.65 11 7 5 26.32 12.54 -11 -7 -5 52.55 26.02 -11 -7 -5 31.93 12.10 11 7 6 15.63 12.38 11 7 6 5.95 12.17 -11 -7 -6 -6.91 24.44 11 8 0 26.69 5.39 11 8 0 28.29 8.53 -11 -8 0 22.36 16.12 -11 -8 0 27.39 28.72 -11 -8 0 23.56 10.16 11 8 1 141.76 14.28 11 8 1 118.75 16.20 -11 -8 -1 69.68 31.20 -11 -8 -1 92.48 16.95 11 8 2 15.67 4.84 11 8 2 8.36 10.23 -11 -8 -2 38.33 28.12 -11 -8 -2 28.88 10.96 11 8 3 2.81 10.17 -11 -8 -3 -18.50 28.89 -11 -8 -3 0.78 10.53 11 8 4 6.45 11.43 -11 -8 -4 -8.74 27.70 -11 -8 -4 5.17 10.84 11 8 5 -1.07 14.85 11 8 5 0.43 12.01 -11 -8 -5 13.49 30.71 -11 -9 -1 -31.21 35.38 11 9 2 1.09 8.88 -11 -9 -2 2.67 31.91 11 9 3 5.92 10.40 -11 -9 -3 -8.66 33.48 -11 -9 -3 5.42 10.32 11 9 4 8.75 11.19 -11 -9 -4 12.82 10.75 12 1 2 0.71 9.68 -12 -2 0 9.62 14.81 -12 -2 -1 0.00 10.49 -12 -2 -1 0.00 14.97 12 2 2 -0.57 9.69 -12 -2 -2 6.43 10.19 -12 -2 -2 2.65 15.00 12 2 3 -0.48 10.40 -12 -2 -3 0.00 9.82 -12 -2 -3 -0.67 15.49 -12 -2 -4 125.07 17.89 -12 -3 0 0.88 10.67 -12 -3 0 -14.13 19.24 12 3 1 129.50 17.01 -12 -3 -1 145.42 18.60 -12 -3 -1 87.69 25.07 12 3 2 -0.82 9.33 -12 -3 -2 1.91 10.82 -12 -3 -2 6.23 19.49 12 3 3 6.48 10.61 -12 -3 -3 24.99 12.01 -12 -3 -3 11.31 20.52 -12 -3 -4 11.62 12.74 -12 -3 -4 7.57 21.41 12 4 0 9.72 7.77 -12 -4 0 1.13 12.62 -12 -4 0 1.44 23.48 12 4 1 8.36 8.95 -12 -4 -1 10.57 7.51 -12 -4 -1 7.01 12.58 -12 -4 -1 6.01 20.95 12 4 2 2.84 9.59 -12 -4 -2 1.23 6.58 -12 -4 -2 9.69 12.55 -12 -4 -2 12.54 20.90 12 4 3 84.39 16.00 -12 -4 -3 140.14 14.86 -12 -4 -3 76.49 18.35 -12 -4 -3 99.32 26.42 12 4 4 11.93 11.26 -12 -4 -4 5.61 6.68 -12 -4 -4 24.84 21.28 12 5 0 93.20 13.49 -12 -5 0 115.55 14.27 -12 -5 0 62.88 18.10 -12 -5 0 89.77 27.46 12 5 1 7.44 8.88 -12 -5 -1 20.62 7.80 -12 -5 -1 7.77 14.19 -12 -5 -1 23.05 21.35 12 5 2 16.71 10.27 -12 -5 -2 21.80 7.75 -12 -5 -2 14.95 14.93 -12 -5 -2 18.51 22.30 12 5 3 3.63 5.87 12 5 3 4.66 10.56 -12 -5 -3 8.17 7.20 -12 -5 -3 0.00 20.89 12 5 4 18.57 6.59 12 5 4 12.43 10.99 -12 -5 -4 23.31 7.51 -12 -5 -4 35.03 21.80 12 6 0 0.52 7.42 -12 -6 0 -5.00 7.45 -12 -6 0 -1.09 15.32 -12 -6 0 0.57 23.69 12 6 1 16.56 9.43 -12 -6 -1 28.18 8.23 -12 -6 -1 12.04 15.82 -12 -6 -1 25.66 22.90 12 6 2 5.62 9.67 -12 -6 -2 8.31 15.50 -12 -6 -2 17.20 22.48 12 6 3 7.83 11.18 -12 -6 -3 11.36 21.85 12 6 4 18.43 6.40 -12 -7 -1 -1.68 15.40 -12 -7 -1 4.02 22.63 -12 -7 -2 -14.27 22.56 -12 -8 -1 8.20 30.68 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 13060 _olex2_submission_special_instructions 'No special instructions were received' _chemical_properties_physical Oxygen-sensitive,Photo-sensitive _exptl_crystal_preparation 'Magnetic properties'