data_tle1714 # start Validation Reply Form _vrf_PLAT417_tle1714 ; PROBLEM: Short Inter D-H..H-D H00U .. H00U .. 1.82 Ang. RESPONSE: Due to the highly disordered nature of the water molecule which is only in place due to h-bonding with a binding water molecule on the metal centre, the locations of the h atoms could not be accurately determined. ; # Added during the CSD deposition process: Friday 04 August 2017 03:22 PM # end Validation Reply Form _refine_special_details ? _audit_creation_date 2017-08-04 _audit_creation_method ; Olex2 1.2 (compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370) ; loop_ _publ_author_name _publ_author_email _publ_author_address 'Nevin, A.C.' nevina@cardiff.ac.uk ; Cardiff University Chemistry Main Building Cardiff CF10 3AT UK ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_id_orcid ? _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C14 H19 Mn N3 O8, 1.34(H2 O)' _chemical_formula_sum 'C14 H21.69 Mn N3 O9.34' _chemical_formula_weight 436.45 _chemical_melting_point ? _chemical_oxdiff_formula 'C11 H10 N2 O5 Mn' _chemical_oxdiff_usercomment "Adam Martin's Linker Manganese" loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 4.8941(4) _cell_length_b 16.6396(13) _cell_length_c 22.4311(15) _cell_angle_alpha 90 _cell_angle_beta 92.215(7) _cell_angle_gamma 90 _cell_volume 1825.3(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3233 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 26.9860 _cell_measurement_theta_min 3.6200 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.749 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 906 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 -21 -12 0.0377 0 22 12 0.0230 -6 5 -8 0.0836 6 -6 8 0.1475 0 7 -30 0.0213 0 -7 30 0.0280 0 -22 -12 0.0328 _exptl_crystal_recrystallization_method "Crystals grown in DMF with HCl at 80'C" _exptl_crystal_size_max 0.279 _exptl_crystal_size_mid 0.056 _exptl_crystal_size_min 0.049 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1.0062 -20.9942 -11.9546 0.1060 0.9783 0.0370 0.0081 22.0010 11.9458 -0.1397 -0.9955 0.1092 -5.9877 5.0290 -8.0454 0.0199 0.0090 0.9389 5.9872 -6.0282 8.0475 -0.0293 0.0314 -0.9487 0.0080 6.9464 -29.9945 0.9349 -0.0123 0.3379 -0.0080 -6.9464 29.9945 -0.9349 0.0123 -0.3379 -0.0081 -22.0010 -11.9458 0.1397 0.9955 -0.1092 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0857 _diffrn_reflns_av_unetI/netI 0.1076 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.870 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 16555 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.870 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.628 _diffrn_reflns_theta_min 2.989 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150.00(10) _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 10.5082 _diffrn_detector_type 'Agilent Diffraction Atlas detector' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.870 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -69.00 33.00 0.50 40.00 -- 10.66 -19.00 90.00 204 2 \w 2.00 49.00 0.50 40.00 -- 10.66 -99.00 0.00 94 3 \w -12.00 83.00 0.50 40.00 -- 10.66 38.00 -90.00 190 4 \w 43.00 89.00 0.50 40.00 -- 10.66 178.00 120.00 92 5 \w -11.00 34.00 0.50 40.00 -- -11.13-108.00 54.00 90 ; _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'SuperNova-Duo, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0435001000 _diffrn_orient_matrix_UB_12 0.0093731000 _diffrn_orient_matrix_UB_13 -0.0289877000 _diffrn_orient_matrix_UB_21 -0.0233961000 _diffrn_orient_matrix_UB_22 -0.0403826000 _diffrn_orient_matrix_UB_23 -0.0089469000 _diffrn_orient_matrix_UB_31 -0.1363768000 _diffrn_orient_matrix_UB_32 0.0099057000 _diffrn_orient_matrix_UB_33 -0.0090092000 _diffrn_radiation_collimation 'focusing mirrors' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_determination fundamental _diffrn_radiation_xray_symbol K-L~2,3~ _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_current 0.8 _diffrn_source_power 0.04 _diffrn_source_target Cu _diffrn_source_type 'SuperNova (Mo) X-ray Source' _diffrn_source_voltage 50 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2856 _reflns_number_total 4474 _reflns_odcompleteness_completeness 99.79 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _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 0.867 _refine_diff_density_min -0.876 _refine_diff_density_rms 0.117 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 284 _refine_ls_number_reflns 4474 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1340 _refine_ls_R_factor_gt 0.0834 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+6.1127P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1764 _refine_ls_wR_factor_ref 0.2041 _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, All O(H,H) groups 2. Restrained distances N00E-C1 \\sim N00E-C00Q \\sim N00E-C2 \\sim N00E-C00R with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C1 \\sim C2 \\sim C00R \\sim C00P: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 4. Others Sof(O1)=Sof(H1D)=Sof(H1E)=FVAR(1) Fixed Sof: C00Q(0.5) H00I(0.5) H00J(0.5) H00K(0.5) C00R(0.5) H00Q(0.5) H00R(0.5) H00S(0.5) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) 5.a Free rotating group: O00C(H00T,H00U), O1(H1D,H1E) 5.b Rotating group: O004(H00A,H00B), O005(H00C,H00D) 5.c Secondary CH2 refined with riding coordinates: C00F(H00E,H00F), C00K(H00G,H00H) 5.d Aromatic/amide H refined with riding coordinates: C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P) 5.e Idealised Me refined as rotating group: C00Q(H00I,H00J,H00K), C00R(H00Q,H00R,H00S), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C) ; _atom_sites_solution_hydrogens mixed _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 Mn01 Mn -0.36850(14) 0.71380(5) 0.81314(3) 0.0196(2) Uani 1 1 d . . . . . O002 O -0.0192(7) 0.7533(2) 0.76617(15) 0.0236(8) Uani 1 1 d . . . . . O003 O 0.3828(7) 0.7626(2) 0.39259(15) 0.0280(9) Uani 1 1 d . . . . . O004 O -0.6608(7) 0.6524(2) 0.87364(16) 0.0262(8) Uani 1 1 d . . . . . H00A H -0.7998 0.6833 0.8803 0.039 Uiso 1 1 d GR . . . . H00B H -0.5790 0.6410 0.9077 0.039 Uiso 1 1 d GR . . . . O005 O -0.5842(7) 0.8273(2) 0.82970(15) 0.0234(8) Uani 1 1 d . . . . . H00C H -0.5653 0.8418 0.8673 0.035 Uiso 1 1 d GR . . . . H00D H -0.7602 0.8225 0.8209 0.035 Uiso 1 1 d GR . . . . O006 O 0.0916(7) 0.6884(2) 0.44433(15) 0.0263(8) Uani 1 1 d . . . . . O007 O 0.3749(7) 0.7050(2) 0.73425(16) 0.0301(9) Uani 1 1 d . . . . . O008 O 0.0764(8) 0.7955(3) 0.57643(17) 0.0392(10) Uani 1 1 d . . . . . O009 O -0.2059(11) 0.5926(3) 0.8020(2) 0.0526(13) Uani 1 1 d . . . . . N00A N 0.1535(8) 0.6735(3) 0.62376(19) 0.0296(11) Uani 1 1 d . . . . . N00B N 0.4034(9) 0.7029(3) 0.54768(19) 0.0321(11) Uani 1 1 d . . . . . O00C O -0.4730(13) 0.5908(4) 0.9856(2) 0.0661(16) Uani 1 1 d . . . A 2 H00T H -0.4683 0.6281 1.0115 0.099 Uiso 1 1 d G . . A 2 H00U H -0.4210 0.5491 1.0048 0.099 Uiso 1 1 d G . . A 2 C00D C 0.1225(9) 0.7169(3) 0.7284(2) 0.0229(10) Uani 1 1 d . . . . . N00E N -0.1056(10) 0.4672(3) 0.8308(3) 0.0526(17) Uani 1 1 d D . . . . C00F C 0.4887(11) 0.7436(4) 0.4949(2) 0.0338(14) Uani 1 1 d . . . . . H00E H 0.6720 0.7261 0.4863 0.041 Uiso 1 1 calc R . . . . H00F H 0.4961 0.8009 0.5028 0.041 Uiso 1 1 calc R . . . . C00G C 0.3305(10) 0.6081(4) 0.6160(2) 0.0310(13) Uani 1 1 d . . . . . C00H C 0.1959(10) 0.7308(4) 0.5818(2) 0.0322(14) Uani 1 1 d . . . . . C00I C 0.3019(10) 0.7288(3) 0.4404(2) 0.0261(12) Uani 1 1 d . . . . . C00J C 0.4831(10) 0.6276(4) 0.5669(2) 0.0316(13) Uani 1 1 d . . . . . C00K C -0.0280(10) 0.6856(4) 0.6724(2) 0.0308(13) Uani 1 1 d . . . . . H00G H -0.1162 0.6351 0.6814 0.037 Uiso 1 1 calc R . . . . H00H H -0.1693 0.7237 0.6601 0.037 Uiso 1 1 calc R . . . . C00L C 0.6805(11) 0.5749(4) 0.5461(3) 0.0364(14) Uani 1 1 d . . . . . H00L H 0.7835 0.5875 0.5134 0.044 Uiso 1 1 calc R . . . . C00M C 0.5600(12) 0.4842(4) 0.6260(3) 0.0406(15) Uani 1 1 d . . . . . H00M H 0.5879 0.4354 0.6455 0.049 Uiso 1 1 calc R . . . . C00N C 0.3642(12) 0.5371(4) 0.6466(3) 0.0397(15) Uani 1 1 d . . . . . H00N H 0.2616 0.5249 0.6795 0.048 Uiso 1 1 calc R . . . . C00O C 0.7155(12) 0.5024(4) 0.5768(3) 0.0410(15) Uani 1 1 d . . . . . H00O H 0.8444 0.4656 0.5643 0.049 Uiso 1 1 calc R . . . . C00P C -0.1881(16) 0.5422(5) 0.8346(5) 0.077(3) Uani 1 1 d . U . . . H00P H -0.2431 0.5561 0.8725 0.092 Uiso 1 1 calc R . . . . C00Q C -0.093(2) 0.4312(7) 0.7758(4) 0.031(2) Uani 0.5 1 d D . P B 2 H00I H -0.2362 0.3922 0.7711 0.046 Uiso 0.5 1 calc GR . P B 2 H00J H 0.0813 0.4051 0.7727 0.046 Uiso 0.5 1 calc GR . P B 2 H00K H -0.1136 0.4712 0.7451 0.046 Uiso 0.5 1 calc GR . P B 2 C00R C -0.030(2) 0.4224(7) 0.8878(5) 0.035(3) Uani 0.5 1 d D U P B 2 H00Q H -0.0281 0.4592 0.9208 0.053 Uiso 0.5 1 calc GR . P B 2 H00R H 0.1473 0.3987 0.8847 0.053 Uiso 0.5 1 calc GR . P B 2 H00S H -0.1627 0.3810 0.8940 0.053 Uiso 0.5 1 calc GR . P B 2 C1 C 0.166(3) 0.4573(10) 0.8055(11) 0.097(7) Uani 0.5 1 d D U P B 1 H1A H 0.1498 0.4252 0.7700 0.146 Uiso 0.5 1 calc GR . P B 1 H1B H 0.2869 0.4312 0.8341 0.146 Uiso 0.5 1 calc GR . P B 1 H1C H 0.2387 0.5092 0.7959 0.146 Uiso 0.5 1 calc GR . P B 1 C2 C -0.222(4) 0.3847(9) 0.8290(13) 0.127(10) Uani 0.5 1 d D U P B 1 H2A H -0.1518 0.3546 0.8627 0.191 Uiso 0.5 1 calc GR . P B 1 H2B H -0.1730 0.3584 0.7929 0.191 Uiso 0.5 1 calc GR . P B 1 H2C H -0.4180 0.3877 0.8303 0.191 Uiso 0.5 1 calc GR . P B 1 O1 O -0.121(3) 0.4881(9) 0.9661(7) 0.051(5) Uani 0.344(14) 1 d . . P C 1 H1D H -0.0801 0.4590 0.9365 0.077 Uiso 0.344(14) 1 d G . P C 1 H1E H -0.0211 0.4752 0.9964 0.077 Uiso 0.344(14) 1 d G . P C 1 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 Mn01 0.0141(4) 0.0280(4) 0.0169(4) -0.0028(3) 0.0028(3) 0.0012(3) O002 0.0144(16) 0.044(2) 0.0130(16) -0.0048(15) 0.0025(14) -0.0022(14) O003 0.0139(16) 0.059(3) 0.0116(16) 0.0012(16) 0.0035(14) -0.0054(16) O004 0.0240(18) 0.032(2) 0.0227(18) -0.0015(15) 0.0066(15) -0.0027(15) O005 0.0193(17) 0.0269(19) 0.0238(19) -0.0025(14) -0.0001(15) 0.0003(13) O006 0.0160(17) 0.046(2) 0.0173(17) -0.0012(16) 0.0029(14) -0.0032(15) O007 0.0146(17) 0.054(2) 0.0220(18) -0.0123(18) 0.0004(15) -0.0016(16) O008 0.024(2) 0.069(3) 0.025(2) -0.002(2) 0.0053(17) 0.007(2) O009 0.092(4) 0.027(2) 0.041(3) 0.007(2) 0.034(3) 0.016(2) N00A 0.016(2) 0.058(3) 0.016(2) -0.011(2) 0.0087(18) -0.010(2) N00B 0.019(2) 0.064(3) 0.014(2) 0.000(2) 0.0044(18) 0.000(2) O00C 0.073(4) 0.093(4) 0.032(3) 0.018(3) -0.002(3) -0.007(3) C00D 0.016(2) 0.038(3) 0.015(2) -0.004(2) 0.0051(19) -0.008(2) N00E 0.024(3) 0.039(3) 0.095(5) 0.026(3) 0.006(3) 0.003(2) C00F 0.018(3) 0.069(4) 0.015(2) -0.002(3) 0.006(2) -0.005(2) C00G 0.020(3) 0.052(4) 0.021(3) -0.011(3) 0.000(2) -0.014(2) C00H 0.015(2) 0.068(4) 0.014(2) -0.015(3) 0.001(2) -0.008(3) C00I 0.013(2) 0.047(3) 0.018(2) -0.002(2) 0.000(2) 0.004(2) C00J 0.015(2) 0.061(4) 0.019(3) -0.014(3) -0.002(2) -0.011(2) C00K 0.019(2) 0.058(4) 0.016(2) -0.010(2) 0.008(2) -0.010(2) C00L 0.021(3) 0.062(4) 0.026(3) -0.014(3) 0.002(2) -0.008(3) C00M 0.035(3) 0.037(3) 0.050(4) -0.009(3) 0.005(3) -0.013(3) C00N 0.031(3) 0.050(4) 0.039(3) -0.016(3) 0.010(3) -0.020(3) C00O 0.027(3) 0.053(4) 0.043(4) -0.024(3) 0.004(3) -0.008(3) C00P 0.058(5) 0.060(5) 0.118(8) 0.042(5) 0.063(5) 0.026(4) C00Q 0.038(6) 0.035(6) 0.020(5) -0.003(5) 0.010(5) 0.006(5) C00R 0.036(6) 0.045(7) 0.025(6) 0.018(5) 0.007(5) 0.017(5) C1 0.092(14) 0.042(10) 0.16(2) 0.007(12) 0.051(15) 0.007(9) C2 0.093(15) 0.049(11) 0.24(3) -0.012(15) 0.077(18) -0.017(10) O1 0.031(8) 0.066(10) 0.057(10) -0.012(8) 0.000(7) 0.005(6) _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 Mn01 O002 2.146(4) . ? Mn01 O003 2.162(3) 4_576 ? Mn01 O004 2.255(4) . ? Mn01 O005 2.202(3) . ? Mn01 O007 2.135(3) 1_455 ? Mn01 O009 2.186(4) . ? O002 C00D 1.269(6) . ? O003 Mn01 2.162(3) 4_675 ? O003 C00I 1.286(6) . ? O004 H00A 0.8710 . ? O004 H00B 0.8695 . ? O005 H00C 0.8792 . ? O005 H00D 0.8801 . ? O006 C00I 1.236(6) . ? O007 Mn01 2.135(3) 1_655 ? O007 C00D 1.253(6) . ? O008 C00H 1.229(7) . ? O009 C00P 1.115(8) . ? N00A C00G 1.407(8) . ? N00A C00H 1.361(8) . ? N00A C00K 1.447(6) . ? N00B C00F 1.439(7) . ? N00B C00H 1.376(7) . ? N00B C00J 1.377(8) . ? O00C H00T 0.8502 . ? O00C H00U 0.8500 . ? C00D C00K 1.524(6) . ? N00E C00P 1.316(9) . ? N00E C00Q 1.376(10) . ? N00E C00R 1.512(9) . ? N00E C1 1.476(13) . ? N00E C2 1.487(13) . ? C00F H00E 0.9700 . ? C00F H00F 0.9700 . ? C00F C00I 1.519(7) . ? C00G C00J 1.393(8) . ? C00G C00N 1.373(9) . ? C00J C00L 1.397(8) . ? C00K H00G 0.9700 . ? C00K H00H 0.9700 . ? C00L H00L 0.9300 . ? C00L C00O 1.396(9) . ? C00M H00M 0.9300 . ? C00M C00N 1.393(9) . ? C00M C00O 1.398(9) . ? C00N H00N 0.9300 . ? C00O H00O 0.9300 . ? C00P H00P 0.9300 . ? C00Q H00I 0.9600 . ? C00Q H00J 0.9600 . ? C00Q H00K 0.9600 . ? C00R H00Q 0.9600 . ? C00R H00R 0.9600 . ? C00R H00S 0.9600 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? O1 H1D 0.8502 . ? O1 H1E 0.8495 . ? 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 O002 Mn01 O003 84.86(13) . 4_576 ? O002 Mn01 O004 166.06(14) . . ? O002 Mn01 O005 102.50(14) . . ? O002 Mn01 O009 85.73(16) . . ? O003 Mn01 O004 86.58(13) 4_576 . ? O003 Mn01 O005 88.08(13) 4_576 . ? O003 Mn01 O009 93.66(17) 4_576 . ? O005 Mn01 O004 88.17(14) . . ? O007 Mn01 O002 93.92(13) 1_455 . ? O007 Mn01 O003 173.43(16) 1_455 4_576 ? O007 Mn01 O004 95.80(14) 1_455 . ? O007 Mn01 O005 85.88(14) 1_455 . ? O007 Mn01 O009 92.69(17) 1_455 . ? O009 Mn01 O004 83.86(16) . . ? O009 Mn01 O005 171.72(17) . . ? C00D O002 Mn01 130.4(3) . . ? C00I O003 Mn01 125.6(3) . 4_675 ? Mn01 O004 H00A 110.7 . . ? Mn01 O004 H00B 110.3 . . ? H00A O004 H00B 108.3 . . ? Mn01 O005 H00C 111.3 . . ? Mn01 O005 H00D 110.8 . . ? H00C O005 H00D 107.8 . . ? C00D O007 Mn01 128.5(3) . 1_655 ? C00P O009 Mn01 129.7(6) . . ? C00G N00A C00K 126.9(5) . . ? C00H N00A C00G 110.2(5) . . ? C00H N00A C00K 122.6(5) . . ? C00H N00B C00F 122.9(5) . . ? C00H N00B C00J 109.8(5) . . ? C00J N00B C00F 126.7(5) . . ? H00T O00C H00U 104.5 . . ? O002 C00D C00K 117.0(4) . . ? O007 C00D O002 124.6(4) . . ? O007 C00D C00K 118.4(4) . . ? C00P N00E C00Q 119.7(8) . . ? C00P N00E C00R 118.5(8) . . ? C00P N00E C1 114.4(8) . . ? C00P N00E C2 139.4(10) . . ? C00Q N00E C00R 121.7(8) . . ? C1 N00E C2 103.8(11) . . ? N00B C00F H00E 108.8 . . ? N00B C00F H00F 108.8 . . ? N00B C00F C00I 113.7(5) . . ? H00E C00F H00F 107.7 . . ? C00I C00F H00E 108.8 . . ? C00I C00F H00F 108.8 . . ? C00J C00G N00A 105.6(5) . . ? C00N C00G N00A 131.8(5) . . ? C00N C00G C00J 122.6(6) . . ? O008 C00H N00A 126.6(5) . . ? O008 C00H N00B 126.8(6) . . ? N00A C00H N00B 106.5(5) . . ? O003 C00I C00F 113.9(4) . . ? O006 C00I O003 125.6(4) . . ? O006 C00I C00F 120.5(5) . . ? N00B C00J C00G 107.8(5) . . ? N00B C00J C00L 131.1(5) . . ? C00G C00J C00L 121.1(6) . . ? N00A C00K C00D 112.2(4) . . ? N00A C00K H00G 109.2 . . ? N00A C00K H00H 109.2 . . ? C00D C00K H00G 109.2 . . ? C00D C00K H00H 109.2 . . ? H00G C00K H00H 107.9 . . ? C00J C00L H00L 121.6 . . ? C00O C00L C00J 116.8(6) . . ? C00O C00L H00L 121.6 . . ? C00N C00M H00M 119.1 . . ? C00N C00M C00O 121.9(6) . . ? C00O C00M H00M 119.1 . . ? C00G C00N C00M 116.6(6) . . ? C00G C00N H00N 121.7 . . ? C00M C00N H00N 121.7 . . ? C00L C00O C00M 121.1(6) . . ? C00L C00O H00O 119.5 . . ? C00M C00O H00O 119.5 . . ? O009 C00P N00E 133.5(10) . . ? O009 C00P H00P 113.3 . . ? N00E C00P H00P 113.3 . . ? N00E C00Q H00I 109.5 . . ? N00E C00Q H00J 109.5 . . ? N00E C00Q H00K 109.5 . . ? H00I C00Q H00J 109.5 . . ? H00I C00Q H00K 109.5 . . ? H00J C00Q H00K 109.5 . . ? N00E C00R H00Q 109.5 . . ? N00E C00R H00R 109.5 . . ? N00E C00R H00S 109.5 . . ? H00Q C00R H00R 109.5 . . ? H00Q C00R H00S 109.5 . . ? H00R C00R H00S 109.5 . . ? N00E C1 H1A 109.5 . . ? N00E C1 H1B 109.5 . . ? N00E C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N00E C2 H2A 109.5 . . ? N00E C2 H2B 109.5 . . ? N00E C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? H1D O1 H1E 109.5 . . ? _shelx_res_file ; tle1714.res created by SHELXL-2014/7 TITL tle1714_a.res in P2(1)/n REM Old TITL TLE1714 in P21/n #14 REM SHELXT solution in P2(1)/n REM R1 0.192, Rweak 0.038, Alpha 0.081, Orientation as input REM Formula found by SHELXT: C17 N3 O7 Mn CELL 0.71073 4.8941 16.6396 22.4311 90 92.215 90 ZERR 4 0.0004 0.0013 0.0015 0 0.007 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Mn N O UNIT 56 86.75 4 12 37.37 SADI N00E C1 N00E C00Q N00E C2 N00E C00R SIMU C1 C2 C00R C00P L.S. 16 PLAN 20 BOND $H list 4 fmap 2 acta OMIT 1 5 11 OMIT 1 6 0 OMIT 2 6 0 OMIT 0 6 0 REM REM REM WGHT 0.061300 6.112700 FVAR 0.53253 0.34353 MN01 3 -0.368502 0.713804 0.813145 11.00000 0.01409 0.02800 = 0.01691 -0.00279 0.00276 0.00122 O002 5 -0.019177 0.753275 0.766173 11.00000 0.01439 0.04372 = 0.01299 -0.00483 0.00254 -0.00223 O003 5 0.382840 0.762618 0.392586 11.00000 0.01389 0.05876 = 0.01159 0.00116 0.00345 -0.00544 O004 5 -0.660836 0.652357 0.873639 11.00000 0.02404 0.03243 = 0.02265 -0.00149 0.00656 -0.00270 AFIX 7 H00A 2 -0.799848 0.683333 0.880292 11.00000 -1.50000 H00B 2 -0.579021 0.640958 0.907690 11.00000 -1.50000 AFIX 0 O005 5 -0.584194 0.827311 0.829696 11.00000 0.01931 0.02691 = 0.02376 -0.00246 -0.00011 0.00035 AFIX 7 H00C 2 -0.565331 0.841782 0.867328 11.00000 -1.50000 H00D 2 -0.760247 0.822456 0.820909 11.00000 -1.50000 AFIX 0 O006 5 0.091621 0.688379 0.444327 11.00000 0.01603 0.04571 = 0.01734 -0.00118 0.00291 -0.00321 O007 5 0.374883 0.705007 0.734254 11.00000 0.01458 0.05374 = 0.02197 -0.01229 0.00044 -0.00158 O008 5 0.076369 0.795474 0.576432 11.00000 0.02378 0.06879 = 0.02535 -0.00226 0.00533 0.00679 O009 5 -0.205854 0.592617 0.801975 11.00000 0.09197 0.02689 = 0.04127 0.00721 0.03425 0.01620 N00A 4 0.153524 0.673511 0.623763 11.00000 0.01603 0.05785 = 0.01566 -0.01143 0.00871 -0.00954 N00B 4 0.403441 0.702939 0.547681 11.00000 0.01858 0.06398 = 0.01410 0.00042 0.00437 -0.00038 PART 2 AFIX 6 O00C 5 -0.472965 0.590820 0.985631 11.00000 0.07337 0.09281 = 0.03175 0.01808 -0.00175 -0.00732 H00T 2 -0.468260 0.628142 1.011537 11.00000 -1.50000 H00U 2 -0.420992 0.549138 1.004819 11.00000 -1.50000 AFIX 0 PART 0 C00D 1 0.122489 0.716895 0.728399 11.00000 0.01622 0.03808 = 0.01478 -0.00358 0.00507 -0.00788 N00E 4 -0.105635 0.467162 0.830805 11.00000 0.02437 0.03905 = 0.09476 0.02565 0.00557 0.00341 C00F 1 0.488707 0.743612 0.494901 11.00000 0.01832 0.06877 = 0.01481 -0.00234 0.00640 -0.00481 AFIX 23 H00E 2 0.672001 0.726076 0.486258 11.00000 -1.20000 H00F 2 0.496067 0.800912 0.502754 11.00000 -1.20000 AFIX 0 C00G 1 0.330490 0.608050 0.615980 11.00000 0.01981 0.05184 = 0.02140 -0.01142 0.00018 -0.01376 C00H 1 0.195923 0.730785 0.581802 11.00000 0.01489 0.06806 = 0.01358 -0.01502 0.00126 -0.00814 C00I 1 0.301894 0.728804 0.440353 11.00000 0.01345 0.04741 = 0.01751 -0.00240 -0.00026 0.00411 C00J 1 0.483137 0.627590 0.566885 11.00000 0.01456 0.06118 = 0.01883 -0.01351 -0.00167 -0.01070 C00K 1 -0.027986 0.685614 0.672368 11.00000 0.01873 0.05829 = 0.01589 -0.01022 0.00842 -0.01034 AFIX 23 H00G 2 -0.116209 0.635100 0.681416 11.00000 -1.20000 H00H 2 -0.169314 0.723674 0.660063 11.00000 -1.20000 AFIX 0 C00L 1 0.680453 0.574907 0.546108 11.00000 0.02143 0.06186 = 0.02601 -0.01422 0.00164 -0.00826 AFIX 43 H00L 2 0.783481 0.587535 0.513411 11.00000 -1.20000 AFIX 0 C00M 1 0.559952 0.484208 0.625979 11.00000 0.03472 0.03730 = 0.04988 -0.00888 0.00475 -0.01258 AFIX 43 H00M 2 0.587941 0.435404 0.645477 11.00000 -1.20000 AFIX 0 C00N 1 0.364173 0.537089 0.646635 11.00000 0.03081 0.04973 = 0.03917 -0.01557 0.01032 -0.01978 AFIX 43 H00N 2 0.261579 0.524948 0.679497 11.00000 -1.20000 AFIX 0 C00O 1 0.715484 0.502419 0.576788 11.00000 0.02733 0.05270 = 0.04303 -0.02370 0.00373 -0.00768 AFIX 43 H00O 2 0.844418 0.465642 0.564292 11.00000 -1.20000 AFIX 0 C00P 1 -0.188099 0.542210 0.834612 11.00000 0.05754 0.06005 = 0.11809 0.04189 0.06255 0.02589 AFIX 43 H00P 2 -0.243087 0.556086 0.872479 11.00000 -1.20000 AFIX 0 PART 2 C00Q 1 -0.092558 0.431207 0.775767 10.50000 0.03755 0.03544 = 0.02004 -0.00272 0.01036 0.00608 AFIX 137 H00I 2 -0.236221 0.392171 0.771077 10.50000 -1.50000 H00J 2 0.081264 0.405107 0.772692 10.50000 -1.50000 H00K 2 -0.113590 0.471250 0.745122 10.50000 -1.50000 AFIX 0 C00R 1 -0.030418 0.422411 0.887789 10.50000 0.03582 0.04503 = 0.02484 0.01776 0.00654 0.01739 AFIX 137 H00Q 2 -0.028109 0.459164 0.920794 10.50000 -1.50000 H00R 2 0.147319 0.398706 0.884721 10.50000 -1.50000 H00S 2 -0.162719 0.380956 0.894021 10.50000 -1.50000 AFIX 0 PART 0 PART 1 C1 1 0.166185 0.457339 0.805491 10.50000 0.09198 0.04151 = 0.16170 0.00663 0.05131 0.00684 AFIX 137 H1A 2 0.149795 0.425232 0.769975 10.50000 -1.50000 H1B 2 0.286941 0.431238 0.834143 10.50000 -1.50000 H1C 2 0.238666 0.509157 0.795885 10.50000 -1.50000 AFIX 0 C2 1 -0.222471 0.384682 0.829014 10.50000 0.09332 0.04899 = 0.24437 -0.01207 0.07679 -0.01686 AFIX 137 H2A 2 -0.151810 0.354615 0.862728 10.50000 -1.50000 H2B 2 -0.173003 0.358446 0.792872 10.50000 -1.50000 H2C 2 -0.418040 0.387727 0.830284 10.50000 -1.50000 AFIX 6 O1 5 -0.120926 0.488098 0.966073 21.00000 0.03096 0.06559 = 0.05680 -0.01150 -0.00017 0.00494 H1D 2 -0.080083 0.459032 0.936542 21.00000 -1.50000 H1E 2 -0.021076 0.475153 0.996382 21.00000 -1.50000 AFIX 0 HKLF 4 REM tle1714_a.res in P2(1)/n REM R1 = 0.0834 for 2856 Fo > 4sig(Fo) and 0.1340 for all 4474 data REM 284 parameters refined using 12 restraints END WGHT 0.0602 6.2441 REM Highest difference peak 0.867, deepest hole -0.876, 1-sigma level 0.117 Q1 1 0.1247 0.7808 0.4031 11.00000 0.05 0.87 Q2 1 -0.3431 0.5401 0.8110 11.00000 0.05 0.83 Q3 1 -0.3805 0.7798 0.8131 11.00000 0.05 0.76 Q4 1 0.6357 0.7136 0.7205 11.00000 0.05 0.74 Q5 1 -0.0750 0.4469 0.7967 11.00000 0.05 0.60 Q6 1 -0.3737 0.8801 0.8116 11.00000 0.05 0.57 Q7 1 0.1156 0.7656 0.4910 11.00000 0.05 0.49 Q8 1 -0.4104 0.7037 0.7640 11.00000 0.05 0.48 Q9 1 0.1133 0.6788 0.5286 11.00000 0.05 0.48 Q10 1 -0.3926 0.5592 0.9096 11.00000 0.05 0.44 Q11 1 -0.3817 0.7196 0.6216 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41.76 5 -11 -3 32.88 15.39 5 11 -2 1.69 15.26 5 -11 -2 -21.28 26.66 -5 -11 2 25.36 17.05 5 -11 -2 -18.55 19.93 5 11 -1 34.51 15.62 5 -11 -1 20.16 15.29 -5 -11 1 48.54 25.10 5 -11 -1 67.11 25.40 5 11 0 5.39 21.63 5 -11 0 8.80 12.15 5 -11 0 36.27 20.31 5 11 1 -26.07 26.23 5 -11 1 16.21 14.95 -5 -11 -1 23.91 22.37 5 11 2 -30.79 25.96 5 -11 2 17.46 23.58 -5 -11 -2 6.57 16.20 5 11 3 66.34 28.26 5 -11 3 57.02 26.73 -5 -11 -3 66.22 29.10 5 11 4 133.62 42.07 5 -11 4 85.54 31.10 -5 -11 -4 115.93 36.73 5 11 5 137.73 39.70 5 -11 5 124.85 38.74 -5 -11 -5 149.36 39.32 5 11 6 60.44 25.91 5 -11 6 54.01 23.92 -5 -11 -6 117.52 36.80 5 11 7 60.43 26.31 5 -11 7 105.25 35.13 -5 -11 -7 103.84 34.54 -5 -11 -8 50.98 26.39 5 11 8 26.28 22.66 5 -11 8 7.49 14.99 -5 -11 -9 71.90 31.43 5 11 9 30.50 26.82 5 -11 9 22.45 18.73 5 11 10 25.89 17.65 5 -11 10 15.52 21.10 -5 11 -10 45.51 32.28 5 11 11 4.75 9.14 5 -11 11 49.40 26.39 5 11 12 10.53 11.44 5 -11 12 87.40 35.72 5 11 13 57.61 24.97 5 -12 -10 9.11 10.48 5 -12 -9 61.80 28.88 -5 -12 8 -1.28 19.45 5 -12 -8 -49.52 27.22 -5 -12 7 75.55 36.50 5 -12 -7 38.48 19.97 -5 -12 6 63.06 28.76 5 -12 -6 44.21 16.78 -5 -12 5 12.71 12.25 5 -12 -5 27.78 11.51 -5 -12 4 4.48 14.98 5 -12 -4 -14.88 19.20 5 -12 -3 81.38 31.68 -5 -12 3 70.94 32.17 5 -12 -3 61.24 24.82 5 12 -3 38.59 28.06 5 12 -2 -9.27 25.34 5 -12 -2 -12.01 17.31 -5 -12 2 83.91 39.19 5 -12 -2 51.29 29.54 5 12 -1 128.92 40.98 5 -12 -1 12.94 16.90 5 -12 -1 58.66 26.72 -5 -12 1 89.00 32.94 5 12 0 25.34 17.53 5 -12 0 50.05 18.89 -5 -12 0 68.20 30.10 5 12 1 108.29 38.42 5 -12 1 135.73 39.29 -5 -12 -1 74.52 31.23 5 12 2 -6.40 11.53 5 -12 2 -15.85 15.60 -5 -12 -2 9.06 17.79 5 12 3 76.53 31.76 5 -12 3 43.79 24.15 -5 -12 -3 6.09 12.98 5 12 4 -11.28 18.19 5 -12 4 10.16 12.92 -5 -12 -4 8.21 9.55 5 12 5 -13.00 11.84 5 -12 5 8.06 13.69 -5 -12 -5 3.30 14.67 5 12 6 -9.18 13.96 5 -12 6 -6.44 14.35 -5 -12 -7 8.30 14.28 5 12 7 -7.20 16.71 5 -12 7 -12.48 15.46 -5 -12 -8 22.03 19.33 5 12 8 31.71 15.35 5 12 9 77.06 34.97 5 -12 9 74.97 31.22 -5 -12 -9 141.89 39.51 -5 12 -9 60.65 34.02 5 12 10 24.21 17.78 5 -12 10 33.20 23.56 5 12 11 57.03 23.98 5 -12 11 101.29 34.42 5 12 12 14.87 15.73 5 -12 12 1.80 11.66 5 -13 -9 12.96 18.15 5 -13 -8 -12.48 15.46 5 -13 -7 -11.79 21.27 -5 -13 6 5.00 19.19 5 -13 -6 -34.12 28.74 -5 -13 5 94.85 36.64 5 -13 -5 129.47 41.95 5 -13 -5 96.89 33.74 5 -13 -4 17.87 16.63 -5 -13 4 -9.49 10.37 5 13 -4 -7.18 14.80 5 13 -3 60.66 34.03 5 -13 -3 46.34 16.79 -5 -13 3 51.18 31.04 5 -13 -3 84.34 33.23 5 13 -2 -14.95 19.27 5 -13 -2 -21.87 15.25 5 -13 -2 25.33 23.77 -5 -13 2 -1.10 9.96 5 13 -1 -42.09 25.67 5 -13 -1 7.46 16.06 -5 -13 1 -20.43 22.08 5 13 0 26.93 23.56 5 -13 0 -38.99 22.66 -5 -13 0 22.41 26.65 5 13 1 -26.62 20.37 5 -13 1 1.20 19.81 -5 -13 -1 -4.70 17.13 5 13 2 1.24 9.16 5 -13 2 1.13 16.86 -5 -13 -2 25.34 22.14 5 13 3 27.69 13.92 5 -13 3 58.76 29.86 -5 -13 -3 -12.83 9.08 5 13 4 -2.10 12.44 5 -13 4 -29.94 25.59 -5 -13 -4 9.71 15.64 5 13 5 182.78 44.96 5 -13 5 110.48 32.68 -5 -13 -5 210.53 52.52 -5 -13 -6 28.29 21.62 5 13 6 4.40 10.74 5 -13 6 -18.39 21.95 -5 -13 -7 26.03 19.79 5 13 7 18.60 8.49 5 -13 7 58.70 26.59 -5 -13 -8 15.58 23.24 5 13 8 34.29 16.38 5 -13 8 29.38 18.54 -5 13 -8 24.49 31.50 5 13 9 13.60 14.11 5 -13 9 23.85 23.35 -5 -13 -9 61.55 29.09 5 13 10 -0.36 6.84 5 -13 10 43.63 25.33 5 13 11 -14.20 14.18 5 -14 -7 142.41 47.09 5 -14 -6 19.35 23.14 5 -14 -5 50.37 29.52 5 14 -5 12.50 16.14 5 14 -4 -72.91 33.60 5 -14 -4 23.00 20.49 5 14 -3 -7.16 17.77 5 -14 -3 36.83 24.49 5 14 -2 -6.93 21.85 -5 -14 2 11.93 9.10 5 14 -1 55.96 28.48 -5 -14 1 58.30 31.99 5 14 0 -31.31 21.66 -5 -14 0 -1.41 16.96 5 14 1 131.40 39.18 -5 -14 -1 149.59 45.44 5 14 2 -15.99 15.74 -5 -14 -2 -15.32 21.37 5 14 3 -27.33 19.21 -5 -14 -3 26.21 17.37 5 14 4 -23.02 17.75 -5 -14 -4 2.64 19.45 5 14 5 -12.22 14.45 -5 -14 -5 30.13 24.73 -5 -14 -6 32.98 25.84 5 14 6 5.13 10.98 -5 -14 -7 -18.89 7.64 -5 -14 -8 78.24 35.06 5 -15 -6 0.60 8.08 5 -15 -5 43.37 26.93 5 -15 -4 67.45 29.95 6 0 -11 -43.73 15.69 6 0 -10 9.54 29.52 6 0 -9 -5.29 12.37 6 0 -8 69.80 46.08 6 0 -7 -9.91 23.90 6 0 -6 298.25 68.78 6 0 -5 -4.45 13.22 6 0 -4 12.38 23.16 6 0 -3 -8.95 17.91 6 0 -2 83.55 33.93 6 0 -1 -8.50 17.83 6 0 -1 -8.00 28.50 6 0 0 66.60 35.85 6 0 0 67.72 27.32 6 0 1 -48.86 34.81 6 0 2 167.91 51.63 6 0 3 -7.84 26.74 6 0 4 20.80 23.48 6 -1 -11 21.57 29.37 6 1 -11 10.13 15.49 6 -1 -10 -6.29 26.25 6 1 -10 22.31 27.43 6 -1 -9 21.98 26.02 6 1 -9 32.41 16.43 6 1 -8 116.01 42.80 6 -1 -8 159.38 53.77 6 1 -7 12.07 22.15 6 -1 -7 -17.17 28.15 6 1 -6 76.33 36.61 6 -1 -6 13.10 15.93 6 1 -5 -4.23 25.63 6 -1 -5 10.87 17.23 6 1 -4 22.88 17.79 6 -1 -4 -8.38 24.58 6 1 -3 -2.77 25.93 6 -1 -3 16.61 22.51 6 1 -2 72.97 37.93 6 -1 -2 86.81 28.71 6 1 -1 -13.28 29.80 6 -1 -1 -9.25 22.44 6 1 -1 -46.54 32.59 6 -1 -1 -8.36 20.62 6 1 0 241.94 66.95 6 -1 0 277.91 67.63 6 1 0 231.60 61.48 6 1 1 6.45 18.42 6 -1 1 -15.49 22.38 6 1 2 200.81 57.18 6 -1 2 141.67 45.93 6 1 3 -14.48 30.52 6 -1 3 3.69 23.61 6 1 4 -8.91 13.44 6 -1 4 66.71 36.26 6 2 -11 6.20 19.30 6 -2 -11 69.15 17.62 6 2 -10 15.93 17.78 6 -2 -10 28.15 24.94 6 2 -9 20.83 31.94 6 -2 -9 -62.57 35.18 6 2 -8 75.06 38.56 6 -2 -8 -25.64 22.60 6 2 -7 38.46 34.78 6 -2 -7 48.61 34.28 6 2 -6 318.41 76.73 6 -2 -6 300.95 68.20 6 2 -5 114.46 43.30 -6 -2 5 93.70 30.88 6 -2 -5 113.09 38.70 6 2 -4 37.57 20.64 -6 -2 4 38.34 17.29 6 -2 -4 39.22 13.37 6 2 -3 142.59 47.14 6 -2 -3 146.71 44.12 6 2 -2 17.82 19.25 6 -2 -2 26.02 14.23 6 2 -1 138.41 49.33 6 -2 -1 103.81 38.48 6 2 -1 138.41 54.68 6 -2 -1 57.75 34.36 6 2 0 -29.18 24.25 6 -2 0 25.38 29.58 6 2 0 34.16 31.91 6 2 1 109.07 46.39 6 -2 1 36.71 31.08 6 2 2 141.94 55.18 6 -2 2 34.31 19.27 6 2 3 -24.61 27.53 6 -2 3 4.30 13.88 6 2 4 100.17 44.76 6 -2 4 149.60 51.11 6 -3 -11 -50.49 32.44 6 3 -10 -31.30 27.82 -6 -3 10 -7.90 13.99 6 -3 -10 -52.50 32.66 6 3 -9 201.48 62.54 -6 -3 9 118.76 39.52 6 -3 -9 160.04 51.78 6 3 -8 55.75 31.30 -6 -3 8 13.12 15.94 6 -3 -8 54.15 38.68 6 3 -7 108.98 43.29 -6 -3 7 84.52 27.41 6 -3 -7 28.25 28.11 6 3 -6 28.95 28.58 -6 -3 6 -20.25 18.93 6 -3 -6 25.34 21.00 6 3 -5 6.20 24.63 -6 -3 5 15.92 14.06 6 -3 -5 7.65 14.42 6 3 -4 28.99 15.72 -6 -3 4 -11.33 12.16 6 -3 -4 15.86 30.87 6 3 -3 5.26 12.98 6 -3 -3 22.55 19.90 6 3 -2 174.36 55.43 6 -3 -2 131.00 43.20 6 3 -1 56.81 26.06 6 3 -1 128.02 53.12 6 -3 -1 111.21 40.57 6 3 0 69.80 38.08 6 -3 0 111.78 42.31 6 3 0 136.84 47.66 6 3 1 49.22 26.15 6 -3 1 85.53 36.23 6 3 1 88.18 36.30 6 3 2 -18.95 27.56 6 -3 2 -18.41 25.74 6 3 3 7.80 28.78 6 -3 3 23.90 17.45 6 3 4 -3.37 25.29 6 -3 4 34.19 21.15 -6 -4 13 55.42 29.68 -6 -4 12 33.56 23.07 -6 -4 11 65.77 31.17 6 -4 -11 123.53 50.98 6 4 -10 53.18 38.83 -6 -4 10 32.64 33.10 6 -4 -10 32.59 13.91 6 4 -9 -20.63 33.74 -6 -4 9 16.68 9.60 6 -4 -9 -1.55 20.95 6 4 -8 7.25 18.34 -6 -4 8 -27.03 19.44 6 -4 -8 27.05 24.67 6 4 -7 73.83 35.47 -6 -4 7 33.39 19.47 6 -4 -7 50.27 33.26 6 4 -6 88.94 41.42 6 -4 -6 136.65 48.81 -6 -4 6 130.05 38.47 6 4 -5 92.99 52.62 6 -4 -5 107.74 42.83 -6 -4 5 114.30 35.94 6 4 -4 31.38 22.07 6 -4 -4 -8.28 13.96 -6 -4 4 2.40 10.87 6 4 -3 34.35 35.33 6 -4 -3 55.44 30.41 -6 -4 3 16.25 7.49 6 4 -2 69.07 38.39 6 -4 -2 69.16 37.53 6 -4 -2 3.07 8.83 6 4 -1 66.61 30.45 6 4 -1 68.42 27.96 6 -4 -1 30.67 24.04 6 4 0 -21.23 22.27 6 -4 0 33.63 23.26 6 4 0 31.95 25.93 6 4 1 -6.07 12.16 6 -4 1 32.26 22.95 6 4 1 27.55 33.06 6 4 2 168.95 56.52 6 -4 2 166.99 50.19 6 4 3 -12.15 18.11 6 -4 3 10.42 11.71 6 4 4 120.73 45.63 -6 -5 12 97.51 36.55 -6 -5 11 20.35 22.83 6 -5 -10 83.45 42.69 -6 -5 10 -10.17 14.41 6 5 -9 154.55 61.62 6 -5 -9 163.03 53.29 -6 -5 9 141.97 40.79 6 5 -8 15.41 21.14 6 -5 -8 4.15 13.16 -6 -5 8 -0.97 12.81 6 5 -7 103.16 45.42 6 -5 -7 64.37 33.15 -6 -5 7 70.04 27.82 6 5 -6 2.07 22.66 6 -5 -6 -6.21 13.23 -6 -5 6 6.34 10.19 6 5 -5 29.25 16.70 6 -5 -5 21.51 14.66 -6 -5 5 36.49 18.86 6 -5 -4 72.57 36.86 -6 -5 4 45.51 25.67 6 -5 -3 101.71 38.69 -6 -5 3 133.79 37.27 6 5 -2 166.54 52.95 6 -5 -2 50.35 27.75 6 5 -1 219.70 61.54 6 -5 -1 141.76 46.56 6 5 0 -23.22 30.70 6 -5 0 54.61 25.47 6 5 1 -17.21 21.30 6 -5 1 -51.00 28.63 6 5 2 -46.19 25.04 6 -5 2 5.94 17.88 6 5 3 91.47 36.19 6 -5 3 43.16 22.10 -6 -6 11 132.84 45.48 6 -6 -10 65.41 34.70 -6 -6 10 75.70 43.80 6 -6 -9 56.39 31.94 -6 -6 9 -42.57 25.53 6 -6 -8 37.51 42.39 -6 -6 8 -32.82 22.42 6 -6 -7 77.43 39.41 -6 -6 7 64.37 29.27 -6 -6 6 -15.64 22.64 6 -6 -6 35.24 24.46 -6 -6 5 190.55 47.51 6 -6 -5 191.93 52.02 -6 -6 4 -0.99 14.39 6 -6 -4 -38.20 24.50 -6 -6 3 110.53 38.10 -6 -6 2 26.57 21.00 6 6 -2 17.31 20.70 6 -6 -2 62.94 31.06 6 6 -1 40.42 26.87 6 -6 -1 -28.55 19.69 6 6 0 33.84 22.44 6 -6 0 31.07 15.97 6 6 1 89.25 37.42 6 -6 1 105.80 39.63 6 6 2 -27.53 37.73 6 -6 2 -37.13 24.78 -6 -7 10 0.40 18.17 6 -7 -9 190.31 55.71 -6 -7 9 144.29 44.15 -6 -7 8 -69.29 31.85 6 -7 -8 -66.06 34.41 -6 -7 7 57.40 31.68 6 -7 -7 66.82 33.94 -6 -7 6 34.14 21.23 6 -7 -6 27.43 21.63 -6 -7 5 87.85 36.43 6 -7 -5 60.25 26.70 -6 -7 4 104.91 39.77 6 -7 -4 113.45 40.45 -6 -7 3 33.13 20.68 6 -7 -2 6.52 14.16 6 7 -2 -4.41 17.06 6 7 -1 36.49 22.45 6 -7 -1 27.03 24.66 6 7 0 24.75 22.93 6 -7 0 -7.65 9.10 6 7 1 107.77 43.51 -6 -8 9 -13.36 22.81 6 -8 -9 18.72 15.53 -6 -8 8 2.74 18.40 6 -8 -8 3.92 11.49 -6 -8 7 84.95 38.03 6 -8 -7 20.62 10.37 -6 -8 6 20.04 17.08 6 -8 -6 84.68 41.20 -6 -8 5 7.50 20.35 6 -8 -5 44.93 27.92 -6 -8 4 19.59 17.17 -6 -8 3 46.35 27.83 -6 -8 2 40.22 24.60 -6 -8 1 30.39 21.20 6 -9 -8 49.05 29.58 -6 -9 7 91.48 37.27 6 -9 -7 98.78 41.58 -6 -9 6 97.71 45.06 6 -9 -6 76.15 35.59 -6 -9 5 -10.71 10.96 -6 -9 4 40.21 30.59 -6 -9 3 97.79 33.57 -6 -9 2 75.85 31.14 -6 -9 1 37.21 28.31 -6 -10 5 173.78 53.08 -6 -10 4 -85.20 35.32 -6 -10 3 48.93 27.97 -6 -10 2 34.97 26.52 -6 -10 1 8.60 16.82 TITL TLE1714 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 4.894056 16.639571 22.431082 90.0000 92.2153 90.0000 ZERR 4.00 0.000367 0.001291 0.001514 0.0000 0.0069 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O Mn UNIT 44.00 40.00 8.00 20.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 1828 _shelx_SHELXL_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.548 _oxdiff_exptl_absorpt_empirical_full_min 0.768