####################################################################### data_PCN-808 _audit_creation_date 2018-09-26 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '0.33(C288 H156 O108 Zr18)' _chemical_formula_sum 'C96 H52 O36 Zr6' _chemical_formula_weight 2328.69 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -0.1862 2.2449 '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 'hexagonal' _space_group_IT_number 191 _space_group_name_H-M_alt 'P 6/m m m' _space_group_name_Hall '-P 6 2' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' '-x+y, y, z' 'x, x-y, z' '-y, -x, z' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 40.5456(7) _cell_length_b 40.546 _cell_length_c 19.6333(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 27951.9(11) _cell_formula_units_Z 3 _cell_measurement_reflns_used 9940 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 62.1845 _cell_measurement_theta_min 2.5784 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.518 _exptl_absorpt_correction_T_max 0.7521 _exptl_absorpt_correction_T_min 0.5890 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1024 before and 0.0529 after correction. The Ratio of minimum to maximum transmission is 0.7831. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 0.415 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 3468 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_unetI/netI 0.0439 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 72653 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 62.360 _diffrn_reflns_theta_max 62.360 _diffrn_reflns_theta_min 2.179 _diffrn_ambient_temperature 99.98 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed tube' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5837 _reflns_number_total 8210 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _refine_diff_density_max 0.750 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.049 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 168 _refine_ls_number_reflns 8210 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0477 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0932P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1471 _refine_ls_wR_factor_ref 0.1547 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C14_$1-C13 = C15_$1-C13 = C14_$1-C14_$2 1.4 with sigma of 0.005 C15_$1-C13 1.4 with sigma of 0.005 C15-C15_$3 \\sim C15_$1-C15_$2 \\sim C14_$1-C14_$2 \\sim C14-C14_$3 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C11) = Uanis(C10) = Uanis(C9) = Uanis(C8) 4. Others Fixed Sof: H0AB(0.5) H0AC(0.5) C15(0.5) C14(0.5) 5.a Me refined with everything fixed: C0AA(H0AA,H0AB,H0AC) 5.b Aromatic/amide H refined with riding coordinates: C7(H7), C6(H6), C3(H3), C10(H10), C4(H4) ; _atom_sites_solution_hydrogens geom _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 Zr1 Zr 0.53482(2) 0.06963(2) 0.0000 0.03967(17) Uani 1 4 d S T P . . Zr2 Zr 0.54352(2) 0.0000 0.09009(2) 0.04697(16) Uani 1 2 d S T P . . O4 O 0.51730(4) 0.03460(8) 0.09009(18) 0.0739(11) Uani 1 2 d S T P . . O7 O 0.53833(9) 0.0000 0.20247(15) 0.0777(11) Uani 1 2 d S T P . . O1 O 0.58334(6) 0.10136(5) 0.06737(10) 0.0509(6) Uani 1 1 d . . . . . O5 O 0.56043(12) 0.03416(9) 0.0000 0.0871(12) Uani 1 2 d S T P . . O2 O 0.58921(6) 0.05666(6) 0.12603(11) 0.0705(7) Uani 1 1 d . . . . . C2 C 0.63339(9) 0.12098(9) 0.14663(16) 0.0679(10) Uani 1 1 d . . . . . O6 O 0.59798(8) 0.0000 0.0779(2) 0.0868(11) Uani 1 2 d S T P . . C1 C 0.59900(10) 0.09084(9) 0.11009(17) 0.0604(10) Uani 1 1 d . . . . . C7 C 0.65215(10) 0.11231(10) 0.19656(17) 0.0823(12) Uani 1 1 d . . . . . H7 H 0.6433 0.0866 0.2088 0.099 Uiso 1 1 calc R . . . . C6 C 0.68296(11) 0.14074(11) 0.22740(18) 0.0960(15) Uani 1 1 d . . . . . H6 H 0.6955 0.1346 0.2617 0.115 Uiso 1 1 calc R . . . . C5 C 0.69693(11) 0.17859(11) 0.21079(17) 0.0980(16) Uani 1 1 d . . . . . O3 O 0.75904(11) 0.24096(11) 0.1418(2) 0.162(3) Uani 1 2 d S T P . . C9 C 0.73018(11) 0.20979(11) 0.24662(18) 0.1109(10) Uani 1 1 d . . . . . C3 C 0.64667(11) 0.15877(10) 0.12935(18) 0.0916(14) Uani 1 1 d . . . . . H3 H 0.6336 0.1648 0.0958 0.110 Uiso 1 1 calc R . . . . C11 C 0.76174(11) 0.23826(11) 0.3531(3) 0.1109(10) Uani 1 2 d S T P . . C10 C 0.73226(11) 0.20963(11) 0.31720(17) 0.1109(10) Uani 1 1 d . . . . . H10 H 0.7125 0.1889 0.3416 0.133 Uiso 1 1 calc R . . . . C8 C 0.75951(11) 0.24049(11) 0.2124(3) 0.1109(10) Uani 1 2 d S T P . . C4 C 0.67843(12) 0.18742(11) 0.1603(2) 0.1108(17) Uani 1 1 d . . . . . H4 H 0.6878 0.2132 0.1473 0.133 Uiso 1 1 calc R . . . . C0AA C 0.7771(2) 0.2229(2) 0.1093(5) 0.226(7) Uani 1 2 d S T P . . H0AA H 0.7753 0.2247 0.0597 0.339 Uiso 1 2 calc S T P . . H0AB H 0.7645 0.1961 0.1228 0.339 Uiso 0.5 1 calc . . . . . H0AC H 0.8039 0.2355 0.1228 0.339 Uiso 0.5 1 calc . . . . . C13 C 0.76301(10) 0.23699(10) 0.4283(3) 0.099(2) Uani 1 2 d DS T P . . C15 C 0.7925(2) 0.2363(2) 0.4637(2) 0.118(3) Uani 0.5 1 d D . . . . C14 C 0.7618(2) 0.2660(2) 0.46424(12) 0.133(4) Uani 0.5 1 d D . . . . 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 Zr1 0.0533(3) 0.0184(3) 0.0356(3) 0.000 0.000 0.00921(13) Zr2 0.0598(2) 0.0228(2) 0.0460(2) 0.000 -0.01057(16) 0.01140(11) O4 0.0591(16) 0.0355(17) 0.119(3) 0.0391(18) 0.0195(9) 0.0177(9) O7 0.126(2) 0.0303(16) 0.0455(18) 0.000 -0.0208(17) 0.0152(8) O1 0.0599(14) 0.0246(11) 0.0471(12) -0.0009(9) -0.0113(11) 0.0053(10) O5 0.180(4) 0.073(2) 0.0401(17) 0.000 0.000 0.087(3) O2 0.0708(16) 0.0335(13) 0.0748(15) 0.0055(11) -0.0231(13) 0.0018(11) C2 0.061(2) 0.0394(19) 0.058(2) 0.0012(17) -0.0121(18) -0.0083(17) O6 0.0712(18) 0.058(2) 0.127(3) 0.000 -0.0196(19) 0.0289(11) C1 0.063(2) 0.0283(18) 0.057(2) 0.0014(16) 0.0078(18) -0.0016(16) C7 0.077(3) 0.053(2) 0.063(2) 0.0147(19) -0.025(2) -0.008(2) C6 0.080(3) 0.077(3) 0.063(2) 0.023(2) -0.029(2) -0.012(2) C5 0.082(3) 0.074(3) 0.050(2) 0.017(2) -0.021(2) -0.027(2) O3 0.126(3) 0.126(3) 0.060(3) 0.037(2) -0.037(2) -0.069(3) C9 0.0803(17) 0.0888(18) 0.0552(13) 0.0215(14) -0.0121(14) -0.0392(12) C3 0.089(3) 0.049(2) 0.074(2) 0.010(2) -0.034(2) -0.012(2) C11 0.0803(17) 0.0888(18) 0.0552(13) 0.0215(14) -0.0121(14) -0.0392(12) C10 0.0803(17) 0.0888(18) 0.0552(13) 0.0215(14) -0.0121(14) -0.0392(12) C8 0.0803(17) 0.0888(18) 0.0552(13) 0.0215(14) -0.0121(14) -0.0392(12) C4 0.108(3) 0.052(2) 0.087(3) 0.019(2) -0.031(3) -0.024(2) C0AA 0.242(9) 0.242(9) 0.088(6) -0.012(4) 0.012(4) 0.042(10) C13 0.077(3) 0.077(3) 0.056(3) 0.000(2) 0.000(2) -0.028(3) C15 0.127(7) 0.102(6) 0.049(4) -0.001(4) -0.023(4) 0.000(6) C14 0.106(6) 0.091(6) 0.101(6) 0.023(5) -0.014(5) -0.026(5) _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 Zr1 Zr2 3.4958(4) 16 ? Zr1 Zr2 3.4958(4) 4_655 ? Zr1 Zr2 3.4958(4) 13_655 ? Zr1 Zr2 3.4959(4) . ? Zr1 O4 2.154(3) . ? Zr1 O4 2.154(3) 16 ? Zr1 O1 2.1779(19) 19_655 ? Zr1 O1 2.1781(19) 16 ? Zr1 O1 2.1781(19) . ? Zr1 O1 2.1779(19) 11_655 ? Zr1 O5 2.154(3) . ? Zr1 O5 2.154(3) 19_655 ? Zr2 Zr1 3.4959(4) 13_655 ? Zr2 Zr2 3.5376(7) 16 ? Zr2 Zr2 3.5293(8) 4_655 ? Zr2 O4 2.1427(16) 4_655 ? Zr2 O4 2.1426(16) . ? Zr2 O7 2.216(3) . ? Zr2 O5 2.1372(19) . ? Zr2 O5 2.1371(19) 7 ? Zr2 O2 2.2252(19) 23 ? Zr2 O2 2.2251(19) . ? Zr2 O6 2.221(4) . ? O4 Zr2 2.1425(16) 4_655 ? O1 C1 1.249(4) . ? O5 Zr2 2.1371(19) 16 ? O2 C1 1.275(4) . ? C2 C1 1.500(4) . ? C2 C7 1.390(4) . ? C2 C3 1.388(4) . ? C7 C6 1.348(4) . ? C6 C5 1.383(5) . ? C5 C9 1.486(4) . ? C5 C4 1.394(5) . ? O3 C8 1.387(6) . ? O3 C0AA 1.419(13) . ? C9 C10 1.388(4) . ? C9 C8 1.391(4) . ? C3 C4 1.371(5) . ? C11 C10 1.373(4) . ? C11 C10 1.373(4) 21_665 ? C11 C13 1.479(7) . ? C8 C9 1.391(4) 21_665 ? C13 C15 1.396(3) 21_665 ? C13 C15 1.396(3) . ? C13 C14 1.397(4) . ? C13 C14 1.397(4) 21_665 ? C15 C15 1.166(15) 21_665 ? C15 C15 1.426(9) 16_556 ? C15 C15 1.842(12) 10_666 ? C14 C14 1.127(14) 21_665 ? C14 C14 1.801(10) 10_666 ? C14 C14 1.404(5) 16_556 ? 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 Zr2 Zr1 Zr2 60.792(13) 16 . ? Zr2 Zr1 Zr2 60.635(14) . 4_655 ? Zr2 Zr1 Zr2 91.239(13) 16 4_655 ? Zr2 Zr1 Zr2 60.792(13) 13_655 4_655 ? Zr2 Zr1 Zr2 91.240(13) . 13_655 ? Zr2 Zr1 Zr2 60.634(14) 16 13_655 ? O4 Zr1 Zr2 90.92(8) . 16 ? O4 Zr1 Zr2 35.44(4) 16 16 ? O4 Zr1 Zr2 90.92(8) . 13_655 ? O4 Zr1 Zr2 90.92(8) 16 . ? O4 Zr1 Zr2 35.44(4) 16 13_655 ? O4 Zr1 Zr2 90.92(8) 16 4_655 ? O4 Zr1 Zr2 35.44(4) . 4_655 ? O4 Zr1 Zr2 35.44(5) . . ? O4 Zr1 O4 110.37(18) 16 . ? O4 Zr1 O1 78.07(8) 16 16 ? O4 Zr1 O1 142.24(5) 16 19_655 ? O4 Zr1 O1 78.07(8) . 19_655 ? O4 Zr1 O1 142.24(5) 16 . ? O4 Zr1 O1 142.23(5) . 16 ? O4 Zr1 O1 78.08(8) 16 11_655 ? O4 Zr1 O1 142.24(5) . 11_655 ? O4 Zr1 O1 78.08(8) . . ? O1 Zr1 Zr2 75.14(5) 16 16 ? O1 Zr1 Zr2 75.14(5) 11_655 13_655 ? O1 Zr1 Zr2 110.94(5) 16 13_655 ? O1 Zr1 Zr2 110.94(5) . 4_655 ? O1 Zr1 Zr2 166.38(5) . 13_655 ? O1 Zr1 Zr2 75.14(5) 19_655 4_655 ? O1 Zr1 Zr2 110.98(5) 19_655 13_655 ? O1 Zr1 Zr2 166.38(5) 19_655 16 ? O1 Zr1 Zr2 110.98(5) . 16 ? O1 Zr1 Zr2 110.93(5) 11_655 16 ? O1 Zr1 Zr2 110.98(5) 16 . ? O1 Zr1 Zr2 166.37(5) 16 4_655 ? O1 Zr1 Zr2 110.93(5) 19_655 . ? O1 Zr1 Zr2 110.98(5) 11_655 4_655 ? O1 Zr1 Zr2 166.38(5) 11_655 . ? O1 Zr1 Zr2 75.14(5) . . ? O1 Zr1 O1 74.89(11) . 19_655 ? O1 Zr1 O1 118.49(10) 16 19_655 ? O1 Zr1 O1 74.79(10) 19_655 11_655 ? O1 Zr1 O1 118.48(10) . 11_655 ? O1 Zr1 O1 74.79(10) . 16 ? O1 Zr1 O1 74.89(11) 16 11_655 ? O5 Zr1 Zr2 35.29(5) . . ? O5 Zr1 Zr2 90.43(9) . 13_655 ? O5 Zr1 Zr2 35.29(5) 19_655 4_655 ? O5 Zr1 Zr2 90.42(9) 19_655 . ? O5 Zr1 Zr2 90.43(9) . 4_655 ? O5 Zr1 Zr2 35.29(5) . 16 ? O5 Zr1 Zr2 90.42(9) 19_655 16 ? O5 Zr1 Zr2 35.29(5) 19_655 13_655 ? O5 Zr1 O4 70.73(7) . . ? O5 Zr1 O4 70.73(7) 19_655 16 ? O5 Zr1 O4 70.72(7) . 16 ? O5 Zr1 O4 70.72(7) 19_655 . ? O5 Zr1 O1 142.35(5) 19_655 . ? O5 Zr1 O1 78.44(10) . 16 ? O5 Zr1 O1 142.35(5) . 19_655 ? O5 Zr1 O1 78.45(10) 19_655 19_655 ? O5 Zr1 O1 142.35(5) 19_655 16 ? O5 Zr1 O1 142.35(5) . 11_655 ? O5 Zr1 O1 78.44(10) . . ? O5 Zr1 O1 78.45(10) 19_655 11_655 ? O5 Zr1 O5 109.3(2) . 19_655 ? Zr1 Zr2 Zr1 88.761(13) . 13_655 ? Zr1 Zr2 Zr2 59.683(7) 13_655 4_655 ? Zr1 Zr2 Zr2 59.682(7) . 4_655 ? Zr1 Zr2 Zr2 59.603(6) . 16 ? Zr1 Zr2 Zr2 59.604(6) 13_655 16 ? Zr2 Zr2 Zr2 90.0 4_655 16 ? O4 Zr2 Zr1 88.90(8) . 13_655 ? O4 Zr2 Zr1 35.67(8) 4_655 13_655 ? O4 Zr2 Zr1 35.67(8) . . ? O4 Zr2 Zr1 88.90(8) 4_655 . ? O4 Zr2 Zr2 34.55(6) 4_655 4_655 ? O4 Zr2 Zr2 90.00(9) 4_655 16 ? O4 Zr2 Zr2 34.55(6) . 4_655 ? O4 Zr2 Zr2 90.00(9) . 16 ? O4 Zr2 O4 69.09(12) . 4_655 ? O4 Zr2 O7 85.51(13) . . ? O4 Zr2 O7 85.51(13) 4_655 . ? O4 Zr2 O2 75.72(9) 4_655 23 ? O4 Zr2 O2 75.72(9) . . ? O4 Zr2 O2 140.13(9) 4_655 . ? O4 Zr2 O2 140.13(9) . 23 ? O4 Zr2 O6 144.97(6) 4_655 . ? O4 Zr2 O6 144.97(6) . . ? O7 Zr2 Zr1 117.11(6) . 13_655 ? O7 Zr2 Zr1 117.11(6) . . ? O7 Zr2 Zr2 84.54(10) . 4_655 ? O7 Zr2 Zr2 174.54(10) . 16 ? O7 Zr2 O2 73.41(7) . 23 ? O7 Zr2 O2 73.41(7) . . ? O7 Zr2 O6 101.63(14) . . ? O5 Zr2 Zr1 88.40(9) 7 . ? O5 Zr2 Zr1 88.40(9) . 13_655 ? O5 Zr2 Zr1 35.61(9) . . ? O5 Zr2 Zr1 35.61(9) 7 13_655 ? O5 Zr2 Zr2 34.14(7) 7 16 ? O5 Zr2 Zr2 89.81(10) . 4_655 ? O5 Zr2 Zr2 34.14(7) . 16 ? O5 Zr2 Zr2 89.81(10) 7 4_655 ? O5 Zr2 O4 108.39(15) . 4_655 ? O5 Zr2 O4 71.28(12) . . ? O5 Zr2 O4 108.39(15) 7 . ? O5 Zr2 O4 71.27(12) 7 4_655 ? O5 Zr2 O7 145.45(7) 7 . ? O5 Zr2 O7 145.44(7) . . ? O5 Zr2 O5 68.28(15) 7 . ? O5 Zr2 O2 76.21(10) 7 23 ? O5 Zr2 O2 76.21(10) . . ? O5 Zr2 O2 139.93(10) . 23 ? O5 Zr2 O2 139.93(10) 7 . ? O5 Zr2 O6 85.08(13) . . ? O5 Zr2 O6 85.08(13) 7 . ? O2 Zr2 Zr1 160.98(6) 23 . ? O2 Zr2 Zr1 72.22(6) 23 13_655 ? O2 Zr2 Zr1 160.99(6) . 13_655 ? O2 Zr2 Zr1 72.22(6) . . ? O2 Zr2 Zr2 108.49(6) 23 16 ? O2 Zr2 Zr2 108.49(6) . 16 ? O2 Zr2 Zr2 108.43(7) . 4_655 ? O2 Zr2 Zr2 108.43(7) 23 4_655 ? O2 Zr2 O2 126.79(11) . 23 ? O6 Zr2 Zr1 116.58(6) . . ? O6 Zr2 Zr1 116.58(6) . 13_655 ? O6 Zr2 Zr2 83.83(10) . 16 ? O6 Zr2 Zr2 173.82(10) . 4_655 ? O6 Zr2 O2 73.72(8) . . ? O6 Zr2 O2 73.72(8) . 23 ? Zr2 O4 Zr1 108.89(11) 4_655 . ? Zr2 O4 Zr1 108.89(11) . . ? Zr2 O4 Zr2 110.90(12) 4_655 . ? C1 O1 Zr1 132.04(18) . . ? Zr2 O5 Zr1 109.10(12) . . ? Zr2 O5 Zr1 109.10(12) 16 . ? Zr2 O5 Zr2 111.71(15) 16 . ? C1 O2 Zr2 133.7(2) . . ? C7 C2 C1 122.3(3) . . ? C3 C2 C1 118.2(3) . . ? C3 C2 C7 119.5(3) . . ? O1 C1 O2 126.9(3) . . ? O1 C1 C2 117.9(3) . . ? O2 C1 C2 115.2(3) . . ? C6 C7 C2 119.4(3) . . ? C7 C6 C5 122.2(4) . . ? C6 C5 C9 121.8(4) . . ? C6 C5 C4 118.6(3) . . ? C4 C5 C9 119.6(4) . . ? C8 O3 C0AA 115.4(8) . . ? C10 C9 C5 120.0(3) . . ? C10 C9 C8 117.3(4) . . ? C8 C9 C5 122.6(3) . . ? C4 C3 C2 120.6(4) . . ? C10 C11 C10 118.2(5) 21_665 . ? C10 C11 C13 120.9(2) 21_665 . ? C10 C11 C13 120.9(2) . . ? C11 C10 C9 122.5(4) . . ? O3 C8 C9 118.9(2) . . ? O3 C8 C9 118.9(2) . 21_665 ? C9 C8 C9 122.1(5) 21_665 . ? C3 C4 C5 119.7(4) . . ? C15 C13 C11 122.9(5) . . ? C15 C13 C11 122.9(5) 21_665 . ? C15 C13 C15 49.3(7) . 21_665 ? C15 C13 C14 99.1(5) 21_665 21_665 ? C15 C13 C14 119.7(6) . 21_665 ? C15 C13 C14 119.7(6) 21_665 . ? C15 C13 C14 99.1(5) . . ? C14 C13 C11 117.3(5) 21_665 . ? C14 C13 C11 117.3(5) . . ? C14 C13 C14 47.6(7) . 21_665 ? C13 C15 C15 119.9(3) . 16_556 ? C13 C15 C15 97.0(5) . 10_666 ? C15 C15 C13 65.3(3) 21_665 . ? C15 C15 C15 50.7(4) 21_665 10_666 ? C15 C15 C15 90.000(2) 21_665 16_556 ? C15 C15 C15 39.3(4) 16_556 10_666 ? C13 C14 C14 98.2(5) . 10_666 ? C13 C14 C14 120.4(3) . 16_556 ? C14 C14 C13 66.2(3) 21_665 . ? C14 C14 C14 38.8(4) 16_556 10_666 ? C14 C14 C14 90.000(2) 21_665 16_556 ? C14 C14 C14 51.2(4) 21_665 10_666 ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.483 -0.333 -0.946 22845.9 3480.9 ? _shelx_res_file ; p.res created by SHELXL-2014/7 TITL p in P6/mmm #191 CELL 1.54184 40.5456 40.5456 19.6333 90 90 120 ZERR 3 0.0007 0 0.0004 0 0 0 LATT 1 SYMM -Y+X,+X,+Z SYMM -Y,+X-Y,+Z SYMM -X,-Y,+Z SYMM +Y-X,-X,+Z SYMM +Y,-X+Y,+Z SYMM -Y+X,-Y,-Z SYMM -X,-X+Y,-Z SYMM +Y,+X,-Z SYMM -Y,-X,-Z SYMM +Y-X,+Y,-Z SYMM +X,+X-Y,-Z SFAC C H O Zr UNIT 288 156 108 18 EQIV $1 1-Y,1-X,+Z EQIV $2 1-Y,1-X,1-Z EQIV $3 +X,+Y,1-Z DFIX 1.4 0.005 C14_$1 C13 C15_$1 C13 C14_$1 C14_$2 DFIX 1.4 0.005 C15_$1 C13 SADI C15 C15_$3 C15_$1 C15_$2 C14_$1 C14_$2 C14 C14_$3 EADP C11 C10 C9 C8 L.S. 10 PLAN 5 0 0 TEMP -173.17 BOND fmap 2 53 53 acta ABIN REM REM REM WGHT 0.093200 FVAR 0.15691 ZR1 4 0.534816 0.069633 0.000000 10.25000 0.05333 0.01841 = 0.03561 0.00000 0.00000 0.00921 ZR2 4 0.543524 0.000000 0.090093 10.50000 0.05980 0.02280 = 0.04597 0.00000 -0.01057 0.01140 O4 3 0.517302 0.034604 0.090090 10.50000 0.05914 0.03547 = 0.11930 0.03909 0.01955 0.01774 O7 3 0.538326 0.000000 0.202466 10.50000 0.12565 0.03033 = 0.04549 0.00000 -0.02077 0.01516 O1 3 0.583338 0.101357 0.067373 11.00000 0.05990 0.02461 = 0.04711 -0.00088 -0.01128 0.00535 O5 3 0.560431 0.034160 0.000000 10.50000 0.18049 0.07284 = 0.04009 0.00000 0.00000 0.08749 O2 3 0.589207 0.056659 0.126031 11.00000 0.07081 0.03345 = 0.07475 0.00548 -0.02312 0.00177 C2 1 0.633390 0.120982 0.146632 11.00000 0.06141 0.03940 = 0.05824 0.00124 -0.01206 -0.00826 O6 3 0.597979 0.000000 0.077927 10.50000 0.07124 0.05779 = 0.12675 0.00000 -0.01961 0.02890 C1 1 0.598999 0.090842 0.110086 11.00000 0.06309 0.02833 = 0.05719 0.00141 0.00783 -0.00156 C7 1 0.652152 0.112307 0.196559 11.00000 0.07677 0.05334 = 0.06294 0.01468 -0.02510 -0.00776 AFIX 43 H7 2 0.643338 0.086561 0.208842 11.00000 -1.20000 AFIX 0 C6 1 0.682964 0.140740 0.227400 11.00000 0.07956 0.07668 = 0.06306 0.02288 -0.02881 -0.01237 AFIX 43 H6 2 0.695515 0.134578 0.261717 11.00000 -1.20000 AFIX 0 C5 1 0.696933 0.178590 0.210787 11.00000 0.08194 0.07400 = 0.04961 0.01724 -0.02102 -0.02724 O3 3 0.759039 0.240961 0.141794 10.50000 0.12570 0.12570 = 0.05970 0.03654 -0.03654 -0.06904 C9 1 0.730183 0.209789 0.246622 11.00000 0.08026 0.08877 = 0.05516 0.02149 -0.01206 -0.03915 C3 1 0.646670 0.158766 0.129353 11.00000 0.08882 0.04910 = 0.07437 0.01043 -0.03396 -0.01232 AFIX 43 H3 2 0.633643 0.164827 0.095823 11.00000 -1.20000 AFIX 0 C11 1 0.761737 0.238263 0.353071 10.50000 0.08026 0.08877 = 0.05516 0.02149 -0.01206 -0.03915 C10 1 0.732255 0.209635 0.317199 11.00000 0.08026 0.08877 = 0.05516 0.02149 -0.01206 -0.03915 AFIX 43 H10 2 0.712523 0.188932 0.341593 11.00000 -1.20000 AFIX 0 C8 1 0.759509 0.240491 0.212416 10.50000 0.08026 0.08877 = 0.05516 0.02149 -0.01206 -0.03915 C4 1 0.678431 0.187416 0.160273 11.00000 0.10815 0.05185 = 0.08723 0.01927 -0.03125 -0.02396 AFIX 43 H4 2 0.687784 0.213165 0.147323 11.00000 -1.20000 AFIX 0 C0AA 1 0.777084 0.222916 0.109255 10.50000 0.24225 0.24225 = 0.08835 -0.01245 0.01245 0.04191 AFIX 31 H0AA 2 0.775309 0.224681 0.059743 10.50000 -1.50000 H0AB 2 0.764467 0.196068 0.122784 10.50000 -1.50000 H0AC 2 0.803935 0.235540 0.122768 10.50000 -1.50000 AFIX 0 C13 1 0.763015 0.236985 0.428263 10.50000 0.07657 0.07657 = 0.05628 0.00009 -0.00009 -0.02772 C15 1 0.792504 0.236251 0.463692 10.50000 0.12701 0.10174 = 0.04911 -0.00080 -0.02307 0.00040 C14 1 0.761753 0.266048 0.464240 10.50000 0.10576 0.09109 = 0.10096 0.02344 -0.01430 -0.02572 HKLF 4 REM p in P6/mmm #191 REM R1 = 0.0477 for 5837 Fo > 4sig(Fo) and 0.0612 for all 8210 data REM 168 parameters refined using 10 restraints END WGHT 0.0932 0.0000 REM Highest difference peak 0.750, deepest hole -0.492, 1-sigma level 0.049 Q1 1 0.5416 0.0195 0.2423 11.00000 0.05 0.75 Q2 1 0.6072 0.0000 0.0000 10.25000 0.05 0.73 Q3 1 0.5000 0.0000 0.2219 10.25000 0.05 0.65 Q4 1 0.6235 0.0196 0.0641 11.00000 0.05 0.53 Q5 1 0.5448 0.0694 0.0000 10.50000 0.05 0.52 ; _shelx_res_checksum 14802 _shelx_hkl_file ; _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7521 _exptl_absorpt_correction_T_min 0.5890 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.54184 40.594 40.566 19.639 90.004 90.016 120.041 ) ; _shelx_hkl_checksum 65035 _shelx_fab_file ; 0 0 0 0.0 0.0 ; _shelx_fab_checksum 22969 _olex2_submission_special_instructions 'No special instructions were received' # start Validation Reply Form _vrf_PLAT132_PCN-808 ; PROBLEM: Trigonal/Hexagonal a and b Differ .............. Please Check RESPONSE: a and b are equal ; # end Validation Reply Form ####################################################################### data_PCN-808-BPDC _audit_creation_date 2018-10-30 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C13.75 H8.5 O4.5 Zr0.75' _chemical_formula_sum 'C14.25 H10 F1.50 O4.50 Zr0.75' _chemical_formula_weight 350.14 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -0.1862 2.2449 '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 'hexagonal' _space_group_IT_number 191 _space_group_name_H-M_alt 'P 6/m m m' _space_group_name_Hall '-P 6 2' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' '-x+y, y, z' 'x, x-y, z' '-y, -x, z' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 41.321(4) _cell_length_b 41.321 _cell_length_c 19.208(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 28403(6) _cell_formula_units_Z 24 _cell_measurement_reflns_used 9997 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 65.0720 _cell_measurement_theta_min 2.6108 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.574 _exptl_absorpt_correction_T_max 0.7529 _exptl_absorpt_correction_T_min 0.6163 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 0.491 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 4200 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0948 _diffrn_reflns_av_unetI/netI 0.1076 _diffrn_reflns_Laue_measured_fraction_full 0.923 _diffrn_reflns_Laue_measured_fraction_max 0.923 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 51030 _diffrn_reflns_point_group_measured_fraction_full 0.923 _diffrn_reflns_point_group_measured_fraction_max 0.923 _diffrn_reflns_theta_full 66.240 _diffrn_reflns_theta_max 66.240 _diffrn_reflns_theta_min 2.138 _diffrn_ambient_temperature 293.38 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.923 _diffrn_measured_fraction_theta_max 0.923 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed tube' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5184 _reflns_number_total 8479 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _refine_diff_density_max 1.682 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.068 _refine_ls_extinction_coef 0.000033(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 183 _refine_ls_number_reflns 8479 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0589 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0797P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1622 _refine_ls_wR_factor_ref 0.1712 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C12-C14 1.39 with sigma of 0.02 C14-C14_$1 1.39 with sigma of 0.02 C13-C12 1.39 with sigma of 0.02 C12-C14_$1 2.4 with sigma of 0.02 C14-C12_$1 2.4 with sigma of 0.02 C13-C14 2.4 with sigma of 0.02 C12-C12_$1 2.8 with sigma of 0.02 C14-C13_$1 2.8 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(O3) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C15) = Uanis(O3) = Uanis(C8) Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C20) 4. Others Fixed Sof: H15A(0.5) H15B(0.5) H15C(0.5) 5.a Aromatic/amide H refined with riding coordinates: C7(H7), C6(H6), C19(H19), C10(H10), C3(H3), C18(H18), C4(H4), C14(H14), C13(H13) 5.b Idealised Me refined as rotating group: C15(H15A,H15B,H15C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _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 Zr1 Zr 0.45747(2) 0.0000 0.40753(3) 0.02661(18) Uani 1 2 d S T P . . Zr2 Zr 0.53461(2) 0.06923(2) 0.5000 0.0263(2) Uani 1 4 d S T P . . O7 O 0.40372(9) 0.0000 0.4424(3) 0.0863(18) Uani 1 2 d S T P . . O1 O 0.46697(7) 0.05536(7) 0.36901(14) 0.0394(8) Uani 1 1 d . . . . . O6 O 0.47458(11) 0.03395(13) 0.5000 0.0695(15) Uani 1 2 d S T P . . O2 O 0.51700(8) 0.09944(7) 0.43026(15) 0.0375(8) Uani 1 1 d . . . . . O4 O 0.47192(10) 0.0000 0.2947(2) 0.0412(11) Uani 1 2 d S T P . . C17 C 0.5000 0.0000 0.1841(5) 0.0820(16) Uani 1 4 d S T P . . C2 C 0.48416(14) 0.11894(12) 0.3553(3) 0.0534(14) Uani 1 1 d . . . . . C7 C 0.45767(15) 0.11092(13) 0.3041(3) 0.0672(17) Uani 1 1 d . . . . . H7 H 0.4425 0.0863 0.2897 0.081 Uiso 1 1 calc R . . . . C16 C 0.5000 0.0000 0.2638(5) 0.044(3) Uani 1 4 d S T P . . C1 C 0.49060(14) 0.08901(12) 0.3877(2) 0.0422(13) Uani 1 1 d . . . . . C6 C 0.45355(16) 0.13934(14) 0.2739(3) 0.0816(19) Uani 1 1 d . . . . . H6 H 0.4359 0.1339 0.2391 0.098 Uiso 1 1 calc R . . . . C20 C 0.5000 0.0000 0.0382(5) 0.0820(16) Uani 1 4 d S T P . . C19 C 0.47259(19) 0.0000 0.0791(4) 0.0820(16) Uani 1 2 d S T P . . H19 H 0.4528 0.0000 0.0562 0.098 Uiso 1 2 calc RS T P . . C11 C 0.4713(3) 0.23567(13) 0.1506(4) 0.088(3) Uani 1 2 d S T P . . C5 C 0.47606(18) 0.17576(15) 0.2961(3) 0.0799(19) Uani 1 1 d . . . . . C9 C 0.47357(17) 0.20695(14) 0.2595(3) 0.083(2) Uani 1 1 d . . . . . C10 C 0.47195(18) 0.20693(14) 0.1869(3) 0.091(2) Uani 1 1 d . . . . . H10 H 0.4713 0.1872 0.1623 0.109 Uiso 1 1 calc R . . . . C3 C 0.50723(16) 0.15590(13) 0.3770(3) 0.0810(19) Uani 1 1 d . . . . . H3 H 0.5253 0.1614 0.4109 0.097 Uiso 1 1 calc R . . . . C18 C 0.47187(18) 0.0000 0.1511(4) 0.0820(16) Uani 1 2 d S TU P . . H18 H 0.4524 0.0000 0.1753 0.098 Uiso 1 2 calc RS T P . . C4 C 0.50306(18) 0.18396(14) 0.3482(3) 0.108(3) Uani 1 1 d . . . . . H4 H 0.5181 0.2085 0.3631 0.129 Uiso 1 1 calc R . . . . C8 C 0.4754(3) 0.23771(17) 0.2938(5) 0.133(2) Uani 1 2 d S T P . . O3 O 0.4797(2) 0.23983(12) 0.3665(4) 0.133(2) Uani 1 2 d S TU P . . C12 C 0.4678(3) 0.23388(16) 0.0726(3) 0.081(3) Uani 1 2 d DS T P . . C14 C 0.4364(3) 0.21818(16) 0.0373(3) 0.229(8) Uani 1 2 d DS T P . . H14 H 0.4137 0.2069 0.0611 0.274 Uiso 1 2 calc RS T P . . C15 C 0.4458(3) 0.22291(16) 0.3990(5) 0.133(2) Uani 1 2 d S T P . . H15A H 0.4491 0.2304 0.4470 0.199 Uiso 0.5 1 calc GR . . A -1 H15B H 0.4350 0.1963 0.3963 0.199 Uiso 0.5 1 calc GR . . A -1 H15C H 0.4296 0.2301 0.3768 0.199 Uiso 0.5 1 calc GR . . A -1 C13 C 0.5005(3) 0.25026(17) 0.0400(5) 0.226(7) Uani 1 2 d DS T P . . H13 H 0.5228 0.2614 0.0648 0.271 Uiso 1 2 calc RS T P . . O5 O 0.51722(5) 0.03445(11) 0.4091(2) 0.0581(15) Uani 1 2 d S T P . . 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 Zr1 0.0327(2) 0.0193(3) 0.0235(4) 0.000 -0.0028(2) 0.00964(13) Zr2 0.0324(3) 0.0155(3) 0.0254(5) 0.000 0.000 0.00774(17) O7 0.0396(19) 0.026(2) 0.189(5) 0.000 -0.058(3) 0.0131(11) O1 0.060(2) 0.0263(16) 0.033(2) -0.0037(14) -0.0072(15) 0.0228(15) O6 0.047(3) 0.087(4) 0.012(3) 0.000 0.000 -0.014(3) O2 0.0541(19) 0.0226(15) 0.035(2) -0.0001(14) -0.0089(16) 0.0184(14) O4 0.056(2) 0.040(2) 0.022(3) 0.000 -0.001(2) 0.0200(12) C17 0.090(2) 0.160(5) 0.019(3) 0.000 0.000 0.080(2) C2 0.091(4) 0.039(3) 0.048(4) 0.002(3) -0.012(3) 0.046(3) C7 0.117(5) 0.050(3) 0.058(4) -0.010(3) -0.040(3) 0.060(3) C16 0.045(5) 0.020(5) 0.058(8) 0.000 0.000 0.010(2) C1 0.076(4) 0.029(3) 0.029(3) 0.004(2) 0.016(3) 0.032(3) C6 0.135(5) 0.057(3) 0.070(4) -0.017(3) -0.045(4) 0.060(4) C20 0.090(2) 0.160(5) 0.019(3) 0.000 0.000 0.080(2) C19 0.090(2) 0.160(5) 0.019(3) 0.000 0.000 0.080(2) C11 0.186(9) 0.064(3) 0.055(6) -0.007(3) -0.013(6) 0.093(5) C5 0.171(6) 0.067(4) 0.042(4) -0.019(3) -0.038(4) 0.089(4) C9 0.162(6) 0.050(3) 0.070(5) -0.021(3) -0.044(4) 0.078(4) C10 0.196(7) 0.069(4) 0.050(4) -0.020(3) -0.043(4) 0.098(5) C3 0.133(5) 0.045(3) 0.082(4) -0.011(3) -0.049(4) 0.058(4) C18 0.090(2) 0.160(5) 0.019(3) 0.000 0.000 0.080(2) C4 0.185(7) 0.037(3) 0.112(6) -0.023(3) -0.078(5) 0.063(4) C8 0.266(8) 0.114(2) 0.070(5) -0.016(2) -0.031(5) 0.133(4) O3 0.266(8) 0.114(2) 0.070(5) -0.016(2) -0.031(5) 0.133(4) C12 0.154(10) 0.066(4) 0.052(7) 0.008(3) 0.016(7) 0.077(5) C14 0.169(12) 0.348(16) 0.109(12) -0.032(5) -0.063(9) 0.084(6) C15 0.266(8) 0.114(2) 0.070(5) -0.016(2) -0.031(5) 0.133(4) C13 0.176(13) 0.355(16) 0.087(10) -0.011(4) -0.023(9) 0.088(7) O5 0.0364(18) 0.041(3) 0.099(4) -0.050(3) -0.0251(13) 0.0203(13) _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 Zr1 Zr1 3.5145(10) 4_655 ? Zr1 Zr1 3.5526(11) 16_556 ? Zr1 Zr2 3.5186(6) . ? Zr1 Zr2 3.5185(6) 13_656 ? Zr1 O7 2.320(4) . ? Zr1 O1 2.244(2) . ? Zr1 O1 2.244(2) 23 ? Zr1 O6 2.152(3) 7_556 ? Zr1 O6 2.152(3) . ? Zr1 O4 2.247(4) . ? Zr1 O5 2.147(2) 4_655 ? Zr1 O5 2.147(2) . ? Zr2 Zr1 3.5185(6) 4_655 ? Zr2 Zr1 3.5185(6) 16_556 ? Zr2 Zr1 3.5185(6) 13_656 ? Zr2 O6 2.159(4) . ? Zr2 O6 2.159(4) 19_655 ? Zr2 O2 2.189(3) 11_656 ? Zr2 O2 2.189(3) 16_556 ? Zr2 O2 2.189(3) 19_655 ? Zr2 O2 2.189(3) . ? Zr2 O5 2.145(4) . ? Zr2 O5 2.145(4) 16_556 ? O1 C1 1.288(5) . ? O6 Zr1 2.152(3) 16_556 ? O2 C1 1.254(5) . ? O4 C16 1.303(5) . ? C17 C16 1.530(13) . ? C17 C18 1.324(8) . ? C17 C18 1.324(8) 4_655 ? C2 C7 1.383(6) . ? C2 C1 1.522(5) . ? C2 C3 1.399(6) . ? C7 C6 1.395(6) . ? C16 O4 1.303(5) 4_655 ? C6 C5 1.383(6) . ? C20 C20 1.467(18) 13_655 ? C20 C19 1.378(8) 4_655 ? C20 C19 1.378(8) . ? C19 C18 1.384(9) . ? C11 C10 1.388(6) . ? C11 C10 1.388(6) 20 ? C11 C12 1.504(9) . ? C5 C9 1.516(6) . ? C5 C4 1.408(6) . ? C9 C10 1.396(7) . ? C9 C8 1.399(6) . ? C3 C4 1.371(6) . ? C8 C9 1.399(6) 20 ? C8 O3 1.405(10) . ? O3 C15 1.363(11) . ? C12 C14 1.312(9) . ? C12 C13 1.330(10) . ? C14 C14 1.433(13) 12 ? C13 C13 1.53(2) 12 ? O5 Zr1 2.147(2) 4_655 ? 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 Zr1 Zr1 Zr1 90.0 4_655 16_556 ? Zr1 Zr1 Zr2 60.039(8) 4_655 13_656 ? Zr1 Zr1 Zr2 60.037(10) 4_655 . ? Zr2 Zr1 Zr1 59.677(9) 13_656 16_556 ? Zr2 Zr1 Zr1 59.679(9) . 16_556 ? Zr2 Zr1 Zr2 89.509(18) 13_656 . ? O7 Zr1 Zr1 163.23(12) . 4_655 ? O7 Zr1 Zr1 73.24(12) . 16_556 ? O7 Zr1 Zr2 109.43(8) . . ? O7 Zr1 Zr2 109.42(8) . 13_656 ? O1 Zr1 Zr1 109.55(7) . 4_655 ? O1 Zr1 Zr1 109.25(7) . 16_556 ? O1 Zr1 Zr1 109.55(7) 23 4_655 ? O1 Zr1 Zr1 109.25(7) 23 16_556 ? O1 Zr1 Zr2 73.26(7) . . ? O1 Zr1 Zr2 162.77(7) 23 . ? O1 Zr1 Zr2 73.26(7) 23 13_656 ? O1 Zr1 Zr2 162.77(7) . 13_656 ? O1 Zr1 O7 76.97(9) 23 . ? O1 Zr1 O7 76.98(9) . . ? O1 Zr1 O1 123.96(14) . 23 ? O6 Zr1 Zr1 34.37(10) . 16_556 ? O6 Zr1 Zr1 89.85(13) . 4_655 ? O6 Zr1 Zr1 34.37(10) 7_556 16_556 ? O6 Zr1 Zr1 89.85(13) 7_556 4_655 ? O6 Zr1 Zr2 35.37(10) 7_556 13_656 ? O6 Zr1 Zr2 88.82(12) 7_556 . ? O6 Zr1 Zr2 35.37(10) . . ? O6 Zr1 Zr2 88.82(12) . 13_656 ? O6 Zr1 O7 76.37(16) . . ? O6 Zr1 O7 76.37(16) 7_556 . ? O6 Zr1 O1 76.98(13) . . ? O6 Zr1 O1 76.97(13) 7_556 23 ? O6 Zr1 O1 140.47(12) 7_556 . ? O6 Zr1 O1 140.47(12) . 23 ? O6 Zr1 O6 68.7(2) . 7_556 ? O6 Zr1 O4 142.66(10) . . ? O6 Zr1 O4 142.66(10) 7_556 . ? O4 Zr1 Zr1 164.59(10) . 16_556 ? O4 Zr1 Zr1 74.59(10) . 4_655 ? O4 Zr1 Zr2 110.73(7) . 13_656 ? O4 Zr1 Zr2 110.73(7) . . ? O4 Zr1 O7 122.18(16) . . ? O4 Zr1 O1 76.77(8) . 23 ? O4 Zr1 O1 76.77(8) . . ? O5 Zr1 Zr1 35.05(8) 4_655 4_655 ? O5 Zr1 Zr1 89.21(12) . 16_556 ? O5 Zr1 Zr1 89.21(12) 4_655 16_556 ? O5 Zr1 Zr1 35.06(8) . 4_655 ? O5 Zr1 Zr2 34.91(10) 4_655 13_656 ? O5 Zr1 Zr2 89.34(11) 4_655 . ? O5 Zr1 Zr2 34.91(10) . . ? O5 Zr1 Zr2 89.35(11) . 13_656 ? O5 Zr1 O7 141.25(9) . . ? O5 Zr1 O7 141.25(9) 4_655 . ? O5 Zr1 O1 76.80(12) . . ? O5 Zr1 O1 76.80(12) 4_655 23 ? O5 Zr1 O1 141.76(11) 4_655 . ? O5 Zr1 O1 141.76(11) . 23 ? O5 Zr1 O6 108.11(18) . 7_556 ? O5 Zr1 O6 70.27(14) 4_655 7_556 ? O5 Zr1 O6 70.27(14) . . ? O5 Zr1 O6 108.10(19) 4_655 . ? O5 Zr1 O4 78.21(14) 4_655 . ? O5 Zr1 O4 78.21(14) . . ? O5 Zr1 O5 70.09(17) 4_655 . ? Zr1 Zr2 Zr1 60.641(18) 16_556 . ? Zr1 Zr2 Zr1 59.923(17) 4_655 . ? Zr1 Zr2 Zr1 60.641(18) 4_655 13_656 ? Zr1 Zr2 Zr1 90.489(18) 16_556 4_655 ? Zr1 Zr2 Zr1 90.490(18) 13_656 . ? Zr1 Zr2 Zr1 59.921(17) 16_556 13_656 ? O6 Zr2 Zr1 35.23(7) . . ? O6 Zr2 Zr1 35.23(7) 19_655 13_656 ? O6 Zr2 Zr1 89.63(12) . 13_656 ? O6 Zr2 Zr1 35.23(7) . 16_556 ? O6 Zr2 Zr1 35.23(7) 19_655 4_655 ? O6 Zr2 Zr1 89.63(12) 19_655 . ? O6 Zr2 Zr1 89.63(12) . 4_655 ? O6 Zr2 Zr1 89.63(12) 19_655 16_556 ? O6 Zr2 O6 108.4(3) 19_655 . ? O6 Zr2 O2 77.75(13) 19_655 19_655 ? O6 Zr2 O2 142.17(7) . 11_656 ? O6 Zr2 O2 77.75(13) 19_655 11_656 ? O6 Zr2 O2 77.75(13) . 16_556 ? O6 Zr2 O2 142.17(7) 19_655 . ? O6 Zr2 O2 142.17(7) . 19_655 ? O6 Zr2 O2 142.17(7) 19_655 16_556 ? O6 Zr2 O2 77.75(13) . . ? O2 Zr2 Zr1 74.36(7) 16_556 16_556 ? O2 Zr2 Zr1 74.36(7) 11_656 13_656 ? O2 Zr2 Zr1 164.84(7) 11_656 . ? O2 Zr2 Zr1 110.32(7) 11_656 16_556 ? O2 Zr2 Zr1 164.84(7) . 13_656 ? O2 Zr2 Zr1 164.84(7) 19_655 16_556 ? O2 Zr2 Zr1 74.36(7) . . ? O2 Zr2 Zr1 110.38(7) . 16_556 ? O2 Zr2 Zr1 110.38(7) 19_655 13_656 ? O2 Zr2 Zr1 164.84(7) 16_556 4_655 ? O2 Zr2 Zr1 110.38(7) 16_556 . ? O2 Zr2 Zr1 110.38(7) 11_656 4_655 ? O2 Zr2 Zr1 110.32(7) 19_655 . ? O2 Zr2 Zr1 74.36(7) 19_655 4_655 ? O2 Zr2 Zr1 110.32(7) 16_556 13_656 ? O2 Zr2 Zr1 110.32(7) . 4_655 ? O2 Zr2 O2 76.28(15) 16_556 11_656 ? O2 Zr2 O2 120.80(14) 16_556 19_655 ? O2 Zr2 O2 120.80(14) 11_656 . ? O2 Zr2 O2 76.28(15) 19_655 . ? O2 Zr2 O2 75.47(14) 16_556 . ? O2 Zr2 O2 75.47(14) 11_656 19_655 ? O5 Zr2 Zr1 34.95(6) 16_556 13_656 ? O5 Zr2 Zr1 90.15(11) . 16_556 ? O5 Zr2 Zr1 34.94(6) 16_556 16_556 ? O5 Zr2 Zr1 34.94(6) . 4_655 ? O5 Zr2 Zr1 90.15(11) 16_556 4_655 ? O5 Zr2 Zr1 90.15(11) 16_556 . ? O5 Zr2 Zr1 34.95(6) . . ? O5 Zr2 Zr1 90.15(11) . 13_656 ? O5 Zr2 O6 70.17(10) . . ? O5 Zr2 O6 70.16(10) 16_556 . ? O5 Zr2 O6 70.17(10) . 19_655 ? O5 Zr2 O6 70.17(10) 16_556 19_655 ? O5 Zr2 O2 77.76(12) 16_556 16_556 ? O5 Zr2 O2 141.73(7) . 11_656 ? O5 Zr2 O2 77.77(12) . . ? O5 Zr2 O2 77.77(12) . 19_655 ? O5 Zr2 O2 141.72(7) 16_556 . ? O5 Zr2 O2 141.73(7) . 16_556 ? O5 Zr2 O2 141.73(7) 16_556 19_655 ? O5 Zr2 O2 77.77(12) 16_556 11_656 ? O5 Zr2 O5 109.1(2) 16_556 . ? C1 O1 Zr1 131.3(3) . . ? Zr1 O6 Zr1 111.3(2) . 16_556 ? Zr1 O6 Zr2 109.39(14) 16_556 . ? Zr1 O6 Zr2 109.40(14) . . ? C1 O2 Zr2 133.0(3) . . ? C16 O4 Zr1 132.5(5) . . ? C18 C17 C16 118.7(6) 4_655 . ? C18 C17 C16 118.6(6) . . ? C18 C17 C18 122.7(11) 4_655 . ? C7 C2 C1 122.3(4) . . ? C7 C2 C3 119.9(4) . . ? C3 C2 C1 117.7(4) . . ? C6 C7 C2 120.6(5) . . ? O4 C16 O4 125.8(9) 4_655 . ? O4 C16 C17 117.1(4) . . ? O4 C16 C17 117.1(4) 4_655 . ? O1 C1 C2 114.6(4) . . ? O2 C1 O1 127.8(4) . . ? O2 C1 C2 117.5(4) . . ? C7 C6 C5 119.3(5) . . ? C19 C20 C20 124.7(5) . 13_655 ? C19 C20 C20 124.7(5) 4_655 13_655 ? C19 C20 C19 110.5(10) . 4_655 ? C18 C19 C20 126.0(8) . . ? C10 C11 C10 119.6(8) . 20 ? C10 C11 C12 120.1(4) . . ? C10 C11 C12 120.1(4) 20 . ? C6 C5 C9 119.2(5) . . ? C6 C5 C4 120.1(5) . . ? C4 C5 C9 120.5(5) . . ? C10 C9 C5 119.1(4) . . ? C10 C9 C8 116.8(6) . . ? C8 C9 C5 123.9(6) . . ? C11 C10 C9 121.5(5) . . ? C4 C3 C2 119.8(5) . . ? C17 C18 C19 117.4(8) . . ? C3 C4 C5 120.2(5) . . ? C9 C8 C9 123.6(9) . 20 ? O3 C8 C9 118.2(4) . 20 ? O3 C8 C9 118.2(4) . . ? C15 O3 C8 111.2(11) . . ? C14 C12 C11 126.0(8) . . ? C14 C12 C13 120.8(7) . . ? C13 C12 C11 113.2(9) . . ? C12 C14 C14 121.1(5) . 12 ? C12 C13 C13 118.1(5) . 12 ? Zr1 O5 Zr1 109.89(17) 4_655 . ? Zr1 O5 Zr2 110.14(14) 4_655 . ? Zr1 O5 Zr2 110.14(14) . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.722 -0.283 -0.517 22873.7 3796.0 ? _olex2_submission_special_instructions 'No special instructions were received' # start Validation Reply Form _vrf_PLAT029_PCN-808-BPDC ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.923 Why? RESPONSE: The limited quality of the crystals after linker installation gives rise to the weak diffraction at high angle, leading to the relatively low data completeness. ; # end Validation Reply Form ####################################################################### data_PCN-808-BDBR _audit_creation_date 2019-01-27 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C14.65 H8 N0.45 O4.75 Ru0.13 Zr0.75' _chemical_formula_sum 'C14.65 H8.20 Cl0 N0.45 O4.75 Ru0.12 Zr0.75' _chemical_formula_weight 347.56 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 '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 'hexagonal' _space_group_IT_number 191 _space_group_name_H-M_alt 'P 6/m m m' _space_group_name_Hall '-P 6 2' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x-y, x, z' '-y, x-y, z' '-x, -y, z' '-x+y, -x, z' 'y, -x+y, z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, -z' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' '-x+y, -x, -z' 'y, -x+y, -z' 'x, y, -z' 'x-y, x, -z' '-y, x-y, -z' '-x+y, y, z' 'x, x-y, z' '-y, -x, z' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 40.8928(8) _cell_length_b 40.893 _cell_length_c 19.2023(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 27808.5(12) _cell_formula_units_Z 24 _cell_measurement_reflns_used 9913 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 59.2788 _cell_measurement_theta_min 2.3009 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.878 _exptl_absorpt_correction_T_max 0.7518 _exptl_absorpt_correction_T_min 0.6000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1082 before and 0.0534 after correction. The Ratio of minimum to maximum transmission is 0.7981. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour Red _exptl_crystal_density_diffrn 0.498 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 4146 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1180 _diffrn_reflns_av_unetI/netI 0.0887 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 61099 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 60.148 _diffrn_reflns_theta_max 60.148 _diffrn_reflns_theta_min 2.161 _diffrn_ambient_temperature 99.99 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed tube' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4484 _reflns_number_total 7699 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _refine_diff_density_max 1.610 _refine_diff_density_min -1.556 _refine_diff_density_rms 0.127 _refine_ls_extinction_coef 0.00008(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 178 _refine_ls_number_reflns 7699 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.1354 _refine_ls_R_factor_gt 0.1002 _refine_ls_restrained_S_all 1.337 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3012 _refine_ls_wR_factor_ref 0.3272 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C11-C8 1.4 with sigma of 0.005 O8-C10 1.42 with sigma of 0.005 C21-C20 2.2 with sigma of 0.005 C20-C20_$1 1.5 with sigma of 0.005 O3-C16 1.25 with sigma of 0.005 O3-O4 2.24 with sigma of 0.005 C18-C17 1.4 with sigma of 0.005 C19-C17 2.2 with sigma of 0.005 Ru1-C28_$2 2.95 with sigma of 0.005 C29-C29_$2 2.2 with sigma of 0.005 C28-C28_$2 2.2 with sigma of 0.005 Ru1-C27_$2 3.1 with sigma of 0.005 Ru1-N1 2.1 with sigma of 0.005 N2-C28_$2 1.4 with sigma of 0.005 C30-N2 2.78 with sigma of 0.005 C13-C15 1.39 with sigma of 0.02 C15-C15_$3 1.39 with sigma of 0.02 C15_$3-C13_$3 1.39 with sigma of 0.02 C13_$3-C14_$3 1.39 with sigma of 0.02 C14_$3-C14 1.39 with sigma of 0.02 C14-C13 1.39 with sigma of 0.02 C13-C15_$3 2.4 with sigma of 0.02 C15-C13_$3 2.4 with sigma of 0.02 C15_$3-C14_$3 2.4 with sigma of 0.02 C13_$3-C14 2.4 with sigma of 0.02 C14_$3-C13 2.4 with sigma of 0.02 C14-C15 2.4 with sigma of 0.02 C13-C13_$3 2.8 with sigma of 0.02 C15-C14_$3 2.8 with sigma of 0.02 C15_$3-C14 2.8 with sigma of 0.02 3. Restrained planarity O8, C9, C8, C11, C12 with sigma of 0.1 N1, C20, C19, C18, C17, C21, C16 with sigma of 0.1 N2, Ru1, N1, C20, C19, C21, C17, C18 with sigma of 0.1 C30, C29, C28, N2, Ru1 with sigma of 0.1 C13, C15, C15_$3, C13_$3, C14_$3, C14 with sigma of 0.1 4. Uiso/Uaniso restraints and constraints Uanis(C10) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(O4) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C21) = Uanis(N1) = Uanis(C20) = Uanis(C19) Uanis(C15) = Uanis(C13) = Uanis(C14) = Uanis(C12) = Uanis(C11) = Uanis(C9) = Uanis(C8) Uanis(N26) = Uanis(C3) = Uanis(C22) = Uanis(C23) = Uanis(C25) = Uanis(C24) = Uanis(Ru1) = Uanis(N2) = Uanis(C28) = Uanis(C27) = Uanis(C29) = Uanis(C30) Uanis(C13) = Uanis(C14) = Uanis(C14) = Uanis(C13) = Uanis(C15) = Uanis(C15) Uanis(C10) = Uanis(O8) = Uanis(C9) = Uanis(C8) = Uanis(C11) = Uanis(C12) = Uanis(C11) = Uanis(C8) 5. Others Fixed Sof: H10A(0.5) H10B(0.5) H10C(0.5) Ru1(0.125) O4(0.25) N1(0.25) C21(0.25) C17(0.25) C18(0.25) C19(0.25) C20(0.5) C16(0.25) N2(0.1) C28(0.1) C30(0.1) C29(0.1) C27(0.1) C3(0.1) H3(0.1) C22(0.1) H22(0.1) C23(0.1) H23(0.1) C24(0.1) H24(0.1) C25(0.1) H25(0.1) N26(0.1) 6.a Free rotating group: C3(C22,C23,C24,C25,N26) 6.b Aromatic/amide H refined with riding coordinates: C0AA(H0AA), C4(H4), C11(H11), C6(H6), C7(H7), C14(H14), C15(H15), C3(H3), C22(H22), C23(H23), C24(H24), C25(H25) 6.c Fitted hexagon refined as free rotating group: N1(C21,C17,C18,C19,C20) 6.d Idealised Me refined as rotating group: C10(H10A,H10B,H10C) ; _atom_sites_solution_hydrogens geom _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 Zr1 Zr 0.54312(2) 0.0000 0.09234(4) 0.0402(4) Uani 1 2 d S T P . . Zr2 Zr 0.53443(2) 0.06886(3) 0.0000 0.0385(4) Uani 1 4 d S T P . . O3 O 0.54454(19) 0.0000 0.2047(3) 0.057(2) Uani 1 2 d DS T P B . O5 O 0.51708(10) 0.03417(19) 0.0929(5) 0.071(3) Uani 1 2 d S T P . . O1 O 0.58223(14) 0.10088(13) 0.0691(2) 0.0466(13) Uani 1 1 d . . . . . O6 O 0.5610(3) 0.0346(3) 0.0000 0.092(3) Uani 1 2 d S T P . . O7 O 0.5984(2) 0.0000 0.0846(4) 0.076(3) Uani 1 2 d S T P . . C0AA C 0.6523(3) 0.1132(3) 0.1943(5) 0.099(4) Uani 1 1 d . . . . . H0AA H 0.6433 0.0878 0.2080 0.118 Uiso 1 1 calc R . . . . O8 O 0.7574(2) 0.2426(2) 0.1362(7) 0.183(3) Uani 1 2 d DS T P . . C1 C 0.5992(2) 0.0911(3) 0.1111(4) 0.065(3) Uani 1 1 d . . . . . C2 C 0.6345(2) 0.1208(2) 0.1429(5) 0.082(3) Uani 1 1 d . . . . . C4 C 0.6834(3) 0.1422(3) 0.2271(6) 0.140(6) Uani 1 1 d . . . . . H4 H 0.6941 0.1369 0.2662 0.168 Uiso 1 1 calc R . . . . C8 C 0.7303(4) 0.2085(4) 0.2415(6) 0.183(3) Uani 1 1 d D . . . . C5 C 0.6983(3) 0.1774(3) 0.2042(6) 0.143(6) Uani 1 1 d . . . . . C13 C 0.7620(3) 0.2380(3) 0.4273(4) 0.183(3) Uani 1 2 d DS T P . . C12 C 0.7626(4) 0.2374(4) 0.3513(11) 0.183(3) Uani 1 2 d S T P . . C11 C 0.7324(4) 0.2088(4) 0.3141(6) 0.183(3) Uani 1 1 d D . . . . H11 H 0.7125 0.1887 0.3393 0.220 Uiso 1 1 calc R . . . . C6 C 0.6804(4) 0.1851(4) 0.1546(7) 0.187(8) Uani 1 1 d . . . . . H6 H 0.6906 0.2105 0.1397 0.225 Uiso 1 1 calc R . . . . C7 C 0.6466(3) 0.1567(3) 0.1231(6) 0.137(6) Uani 1 1 d . . . . . H7 H 0.6333 0.1628 0.0898 0.164 Uiso 1 1 calc R . . . . C9 C 0.7594(2) 0.2406(2) 0.2121(11) 0.183(3) Uani 1 2 d S T P . . O2 O 0.58875(15) 0.05653(16) 0.1263(3) 0.0705(18) Uani 1 1 d . . . . . C14 C 0.7787(2) 0.2213(2) 0.4636(4) 0.183(3) Uani 1 2 d DS T P . . H14 H 0.7903 0.2097 0.4390 0.220 Uiso 1 2 calc RS T P . . C15 C 0.7449(3) 0.2551(3) 0.4630(4) 0.183(3) Uani 1 2 d DS T P . . H15 H 0.7333 0.2667 0.4381 0.220 Uiso 1 2 calc RS T P . . C10 C 0.7763(2) 0.2237(2) 0.1113(10) 0.183(3) Uani 1 2 d DS TU P . . H10A H 0.7873 0.2339 0.0655 0.275 Uiso 0.5 1 calc GR . . A -1 H10B H 0.7582 0.1966 0.1071 0.275 Uiso 0.5 1 calc GR . . A -1 H10C H 0.7963 0.2276 0.1439 0.275 Uiso 0.5 1 calc GR . . A -1 Ru1 Ru 0.63221(10) 0.0000 0.5000 0.1362(18) Uani 0.5 4 d DS T P . . O4 O 0.5992(2) 0.0000 0.2194(7) 0.099(3) Uani 0.5 2 d DS T P B . N1 N 0.5902(2) 0.0000 0.4372(6) 0.099(3) Uani 0.5 2 d DS T P B . C21 C 0.5963(2) 0.0002(5) 0.3658(7) 0.099(3) Uani 0.5 2 d DG . . . . C17 C 0.5678(4) -0.0043(7) 0.3199(3) 0.099(3) Uani 0.25 1 d DG . . B . C18 C 0.5333(4) -0.0106(7) 0.3454(5) 0.099(3) Uani 0.25 1 d DG . . . . C19 C 0.5273(3) -0.0118(7) 0.4168(6) 0.099(3) Uani 0.25 1 d DG . . B . C20 C 0.5557(4) -0.0067(4) 0.4627(3) 0.099(3) Uani 0.5 1 d DG . . . . C16 C 0.5694(4) 0.0000 0.2430(11) 0.099(3) Uani 0.5 2 d DS T P . . N2 N 0.6646(8) 0.0000 0.5695(15) 0.1362(18) Uani 0.2 2 d DS T P B . C28 C 0.663(2) -0.03108(7) 0.602(4) 0.1362(18) Uani 0.1 1 d D . . . . C30 C 0.7127(13) 0.0000 0.672(3) 0.1362(18) Uani 0.2 2 d DS T P . . C29 C 0.693(3) -0.03107(7) 0.666(5) 0.1362(18) Uani 0.1 1 d D . . B . C27 C 0.661(3) -0.037(3) 0.606(6) 0.1362(18) Uani 0.1 1 d D . . B . C3 C 0.6236(17) -0.067(2) 0.442(4) 0.1362(18) Uani 0.1 1 d . . . B -1 H3 H 0.6483 -0.0467 0.4320 0.163 Uiso 0.1 1 calc R . . B -1 C22 C 0.610(2) -0.101(3) 0.408(3) 0.1362(18) Uani 0.1 1 d G . . B -1 H22 H 0.6249 -0.1047 0.3741 0.163 Uiso 0.1 1 calc R . . B -1 C23 C 0.574(2) -0.131(2) 0.423(4) 0.1362(18) Uani 0.1 1 d G . . B -1 H23 H 0.5641 -0.1545 0.3991 0.163 Uiso 0.1 1 calc R . . B -1 C24 C 0.5513(17) -0.126(2) 0.472(4) 0.1362(18) Uani 0.1 1 d G . . B -1 H24 H 0.5266 -0.1463 0.4819 0.163 Uiso 0.1 1 calc R . . B -1 C25 C 0.565(2) -0.092(3) 0.506(4) 0.1362(18) Uani 0.1 1 d G . . B -1 H25 H 0.5500 -0.0884 0.5399 0.163 Uiso 0.1 1 calc R . . B -1 N26 N 0.601(2) -0.0621(18) 0.491(4) 0.1362(18) Uani 0.1 1 d G . . B -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 Zr1 0.0567(6) 0.0403(6) 0.0180(5) 0.000 -0.0028(3) 0.0201(3) Zr2 0.0561(7) 0.0353(8) 0.0172(6) 0.000 0.000 0.0176(4) O3 0.101(5) 0.036(4) 0.011(3) 0.000 -0.015(3) 0.018(2) O5 0.054(4) 0.026(4) 0.125(8) 0.009(5) 0.005(2) 0.013(2) O1 0.056(3) 0.045(3) 0.028(3) 0.004(2) 0.000(2) 0.017(3) O6 0.194(10) 0.102(7) 0.018(4) 0.000 0.000 0.101(8) O7 0.090(5) 0.090(7) 0.047(5) 0.000 -0.010(4) 0.045(3) C0AA 0.066(7) 0.089(7) 0.073(7) 0.039(6) -0.031(5) -0.013(6) O8 0.149(3) 0.149(3) 0.131(6) 0.050(3) -0.050(3) -0.016(4) C1 0.061(6) 0.067(7) 0.035(5) 0.017(4) -0.004(4) 0.007(5) C2 0.058(6) 0.049(6) 0.075(6) 0.030(5) -0.033(5) -0.020(5) C4 0.114(9) 0.087(8) 0.102(9) 0.048(7) -0.067(7) -0.037(7) C8 0.149(3) 0.149(3) 0.131(6) 0.050(3) -0.050(3) -0.016(4) C5 0.102(9) 0.090(9) 0.120(10) 0.056(8) -0.075(8) -0.040(7) C13 0.149(3) 0.149(3) 0.131(6) 0.050(3) -0.050(3) -0.016(4) C12 0.149(3) 0.149(3) 0.131(6) 0.050(3) -0.050(3) -0.016(4) C11 0.149(3) 0.149(3) 0.131(6) 0.050(3) -0.050(3) -0.016(4) C6 0.154(13) 0.093(10) 0.165(14) 0.073(10) -0.073(11) -0.051(9) C7 0.098(9) 0.081(8) 0.120(9) 0.046(7) -0.067(8) -0.039(7) C9 0.149(3) 0.149(3) 0.131(6) 0.050(3) -0.050(3) -0.016(4) O2 0.049(4) 0.069(4) 0.060(4) 0.027(3) -0.017(3) 0.004(3) C14 0.149(3) 0.149(3) 0.131(6) 0.050(3) -0.050(3) -0.016(4) C15 0.149(3) 0.149(3) 0.131(6) 0.050(3) -0.050(3) -0.016(4) C10 0.149(3) 0.149(3) 0.131(6) 0.050(3) -0.050(3) -0.016(4) Ru1 0.141(3) 0.228(5) 0.069(2) 0.000 0.000 0.114(3) O4 0.137(7) 0.134(8) 0.024(4) 0.000 0.001(4) 0.067(4) N1 0.137(7) 0.134(8) 0.024(4) 0.000 0.001(4) 0.067(4) C21 0.137(7) 0.134(8) 0.024(4) 0.000 0.001(4) 0.067(4) C17 0.137(7) 0.134(8) 0.024(4) 0.000 0.001(4) 0.067(4) C18 0.137(7) 0.134(8) 0.024(4) 0.000 0.001(4) 0.067(4) C19 0.137(7) 0.134(8) 0.024(4) 0.000 0.001(4) 0.067(4) C20 0.137(7) 0.134(8) 0.024(4) 0.000 0.001(4) 0.067(4) C16 0.137(7) 0.134(8) 0.024(4) 0.000 0.001(4) 0.067(4) N2 0.141(3) 0.228(5) 0.069(2) 0.000 0.000 0.114(3) C28 0.141(3) 0.228(5) 0.069(2) 0.000 0.000 0.114(3) C30 0.141(3) 0.228(5) 0.069(2) 0.000 0.000 0.114(3) C29 0.141(3) 0.228(5) 0.069(2) 0.000 0.000 0.114(3) C27 0.141(3) 0.228(5) 0.069(2) 0.000 0.000 0.114(3) C3 0.141(3) 0.228(5) 0.069(2) 0.000 0.000 0.114(3) C22 0.141(3) 0.228(5) 0.069(2) 0.000 0.000 0.114(3) C23 0.141(3) 0.228(5) 0.069(2) 0.000 0.000 0.114(3) C24 0.141(3) 0.228(5) 0.069(2) 0.000 0.000 0.114(3) C25 0.141(3) 0.228(5) 0.069(2) 0.000 0.000 0.114(3) N26 0.141(3) 0.228(5) 0.069(2) 0.000 0.000 0.114(3) _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 Zr1 Zr1 3.5267(19) 4_655 ? Zr1 Zr1 3.5464(15) 16 ? Zr1 Zr2 3.4930(11) 13_655 ? Zr1 Zr2 3.4929(11) . ? Zr1 O3 2.158(6) . ? Zr1 O5 2.139(4) . ? Zr1 O5 2.139(4) 4_655 ? Zr1 O6 2.155(5) 7 ? Zr1 O6 2.155(5) . ? Zr1 O7 2.266(9) . ? Zr1 O2 2.222(6) 23 ? Zr1 O2 2.222(6) . ? Zr2 Zr1 3.4930(11) 13_655 ? Zr2 Zr1 3.4930(11) 16 ? Zr2 Zr1 3.4930(11) 4_655 ? Zr2 O5 2.166(8) 16 ? Zr2 O5 2.166(8) . ? Zr2 O1 2.177(5) 16 ? Zr2 O1 2.177(5) 19_655 ? Zr2 O1 2.177(5) 11_655 ? Zr2 O1 2.177(5) . ? Zr2 O6 2.163(9) . ? Zr2 O6 2.163(9) 19_655 ? O3 C16 1.253(5) . ? O5 Zr1 2.139(4) 4_655 ? O1 C1 1.251(9) . ? O6 Zr1 2.155(5) 16 ? C0AA C2 1.350(11) . ? C0AA C4 1.383(12) . ? O8 C9 1.47(2) . ? O8 C10 1.420(5) . ? C1 C2 1.474(11) . ? C1 O2 1.291(10) . ? C2 C7 1.350(13) . ? C4 C5 1.327(14) . ? C8 C5 1.476(15) . ? C8 C11 1.396(5) . ? C8 C9 1.378(14) . ? C5 C6 1.332(15) . ? C13 C12 1.46(2) . ? C13 C14 1.374(10) . ? C13 C15 1.393(11) . ? C12 C11 1.400(14) . ? C12 C11 1.400(14) 21_665 ? C6 C7 1.420(14) . ? C9 C8 1.378(14) 21_665 ? C14 C14 1.400(14) 16_556 ? C15 C15 1.420(15) 16_556 ? Ru1 N1 2.098(5) 16_556 ? Ru1 N1 2.098(5) . ? Ru1 N2 1.879(10) 16_556 ? Ru1 N2 1.879(10) . ? Ru1 N26 2.21(6) . ? O4 C16 1.30(2) . ? N1 C21 1.3930 . ? N1 C20 1.385(5) 23 ? N1 C20 1.3846 . ? C21 C17 1.3965 . ? C21 C17 1.395(5) 23 ? C17 C17 0.30(5) 23 ? C17 C18 1.470(19) 23 ? C17 C18 1.3900 . ? C17 C16 1.49(2) . ? C18 C17 1.470(18) 23 ? C18 C18 0.75(5) 23 ? C18 C19 1.60(2) 23 ? C18 C19 1.3900 . ? C19 C18 1.60(3) 23 ? C19 C19 0.84(5) 23 ? C19 C20 1.527(14) 23 ? C19 C20 1.3900 . ? C20 C19 1.53(2) 23 ? C20 C20 1.509(5) 7_556 ? C20 C20 0.48(3) 23 ? C20 C20 1.431(11) 16_556 ? C16 C17 1.49(2) 23 ? N2 C28 1.396(5) 23 ? N2 C28 1.396(5) . ? N2 C27 1.60(6) . ? N2 C27 1.60(6) 23 ? C28 C29 1.73(11) . ? C28 C27 0.21(8) . ? C30 C29 1.12(2) . ? C30 C29 1.12(2) 23 ? C29 C27 1.66(12) . ? C3 C22 1.3943 . ? C3 N26 1.3945 . ? C22 C23 1.3944 . ? C23 C24 1.3946 . ? C24 C25 1.3945 . ? C25 N26 1.3934 . ? 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 Zr1 Zr1 Zr1 90.0 4_655 16 ? Zr2 Zr1 Zr1 59.681(16) 13_655 4_655 ? Zr2 Zr1 Zr1 59.493(15) . 16 ? Zr2 Zr1 Zr1 59.494(15) 13_655 16 ? Zr2 Zr1 Zr1 59.680(16) . 4_655 ? Zr2 Zr1 Zr2 88.56(3) . 13_655 ? O3 Zr1 Zr1 91.5(2) . 4_655 ? O3 Zr1 Zr1 178.5(2) . 16 ? O3 Zr1 Zr2 121.40(12) . 13_655 ? O3 Zr1 Zr2 121.40(12) . . ? O3 Zr1 O7 92.2(3) . . ? O3 Zr1 O2 72.41(15) . . ? O3 Zr1 O2 72.41(15) . 23 ? O5 Zr1 Zr1 34.46(15) . 4_655 ? O5 Zr1 Zr1 90.3(2) . 16 ? O5 Zr1 Zr1 90.3(2) 4_655 16 ? O5 Zr1 Zr1 34.46(15) 4_655 4_655 ? O5 Zr1 Zr2 88.93(19) 4_655 . ? O5 Zr1 Zr2 36.0(2) 4_655 13_655 ? O5 Zr1 Zr2 36.0(2) . . ? O5 Zr1 Zr2 88.94(19) . 13_655 ? O5 Zr1 O3 91.0(3) . . ? O5 Zr1 O3 91.0(3) 4_655 . ? O5 Zr1 O5 68.9(3) 4_655 . ? O5 Zr1 O6 109.6(4) . 7 ? O5 Zr1 O6 109.6(4) 4_655 . ? O5 Zr1 O6 72.1(3) 4_655 7 ? O5 Zr1 O6 72.1(3) . . ? O5 Zr1 O7 145.40(15) . . ? O5 Zr1 O7 145.40(15) 4_655 . ? O5 Zr1 O2 75.6(2) . . ? O5 Zr1 O2 140.5(3) . 23 ? O5 Zr1 O2 140.5(3) 4_655 . ? O5 Zr1 O2 75.6(2) 4_655 23 ? O6 Zr1 Zr1 34.6(2) 7 16 ? O6 Zr1 Zr1 90.7(3) 7 4_655 ? O6 Zr1 Zr1 90.7(3) . 4_655 ? O6 Zr1 Zr1 34.6(2) . 16 ? O6 Zr1 Zr2 89.1(2) . 13_655 ? O6 Zr1 Zr2 89.1(2) 7 . ? O6 Zr1 Zr2 36.1(2) . . ? O6 Zr1 Zr2 36.1(2) 7 13_655 ? O6 Zr1 O3 145.3(2) 7 . ? O6 Zr1 O3 145.3(2) . . ? O6 Zr1 O6 69.2(4) . 7 ? O6 Zr1 O7 86.2(3) . . ? O6 Zr1 O7 86.2(3) 7 . ? O6 Zr1 O2 138.6(3) . 23 ? O6 Zr1 O2 74.1(3) . . ? O6 Zr1 O2 74.1(3) 7 23 ? O6 Zr1 O2 138.6(3) 7 . ? O7 Zr1 Zr1 86.26(19) . 16 ? O7 Zr1 Zr1 176.26(19) . 4_655 ? O7 Zr1 Zr2 118.07(12) . 13_655 ? O7 Zr1 Zr2 118.07(12) . . ? O2 Zr1 Zr1 108.63(17) . 4_655 ? O2 Zr1 Zr1 107.08(14) . 16 ? O2 Zr1 Zr1 108.63(17) 23 4_655 ? O2 Zr1 Zr1 107.08(14) 23 16 ? O2 Zr1 Zr2 159.95(14) . 13_655 ? O2 Zr1 Zr2 71.42(14) . . ? O2 Zr1 Zr2 71.42(14) 23 13_655 ? O2 Zr1 Zr2 159.95(14) 23 . ? O2 Zr1 O7 72.57(18) 23 . ? O2 Zr1 O7 72.57(18) . . ? O2 Zr1 O2 128.6(3) 23 . ? Zr1 Zr2 Zr1 61.02(3) 13_655 4_655 ? Zr1 Zr2 Zr1 91.44(3) . 13_655 ? Zr1 Zr2 Zr1 61.02(3) . 16 ? Zr1 Zr2 Zr1 60.64(3) 13_655 16 ? Zr1 Zr2 Zr1 60.64(3) . 4_655 ? Zr1 Zr2 Zr1 91.44(3) 16 4_655 ? O5 Zr2 Zr1 91.27(18) . 16 ? O5 Zr2 Zr1 35.50(10) . 4_655 ? O5 Zr2 Zr1 35.50(11) . . ? O5 Zr2 Zr1 35.50(11) 16 16 ? O5 Zr2 Zr1 91.27(18) 16 4_655 ? O5 Zr2 Zr1 91.27(18) . 13_655 ? O5 Zr2 Zr1 35.50(10) 16 13_655 ? O5 Zr2 Zr1 91.27(18) 16 . ? O5 Zr2 O5 110.9(4) . 16 ? O5 Zr2 O1 78.1(2) . 19_655 ? O5 Zr2 O1 142.93(13) . 11_655 ? O5 Zr2 O1 78.1(2) 16 11_655 ? O5 Zr2 O1 142.92(13) . 16 ? O5 Zr2 O1 78.1(2) 16 16 ? O5 Zr2 O1 142.93(13) 16 19_655 ? O5 Zr2 O1 78.1(2) . . ? O5 Zr2 O1 142.92(13) 16 . ? O1 Zr2 Zr1 75.68(13) 19_655 4_655 ? O1 Zr2 Zr1 75.67(13) 16 16 ? O1 Zr2 Zr1 111.84(13) 19_655 13_655 ? O1 Zr2 Zr1 110.83(12) . 4_655 ? O1 Zr2 Zr1 110.82(12) 16 13_655 ? O1 Zr2 Zr1 167.11(13) 11_655 . ? O1 Zr2 Zr1 111.83(13) 16 . ? O1 Zr2 Zr1 111.83(13) . 16 ? O1 Zr2 Zr1 75.68(13) 11_655 13_655 ? O1 Zr2 Zr1 111.84(13) 11_655 4_655 ? O1 Zr2 Zr1 167.11(13) . 13_655 ? O1 Zr2 Zr1 167.11(13) 16 4_655 ? O1 Zr2 Zr1 167.11(13) 19_655 16 ? O1 Zr2 Zr1 75.68(13) . . ? O1 Zr2 Zr1 110.82(12) 11_655 16 ? O1 Zr2 Zr1 110.82(12) 19_655 . ? O1 Zr2 O1 73.3(3) 19_655 . ? O1 Zr2 O1 75.2(2) 19_655 11_655 ? O1 Zr2 O1 73.3(3) 11_655 16 ? O1 Zr2 O1 117.2(3) 11_655 . ? O1 Zr2 O1 117.2(3) 19_655 16 ? O1 Zr2 O1 75.2(2) . 16 ? O6 Zr2 Zr1 35.93(14) 19_655 13_655 ? O6 Zr2 Zr1 35.93(14) . 16 ? O6 Zr2 Zr1 91.5(2) 19_655 16 ? O6 Zr2 Zr1 91.5(2) 19_655 . ? O6 Zr2 Zr1 91.5(2) . 13_655 ? O6 Zr2 Zr1 91.5(2) . 4_655 ? O6 Zr2 Zr1 35.93(14) 19_655 4_655 ? O6 Zr2 Zr1 35.93(14) . . ? O6 Zr2 O5 71.43(18) . 16 ? O6 Zr2 O5 71.43(18) 19_655 . ? O6 Zr2 O5 71.43(18) 19_655 16 ? O6 Zr2 O5 71.43(18) . . ? O6 Zr2 O1 141.87(13) . 11_655 ? O6 Zr2 O1 78.4(3) . 16 ? O6 Zr2 O1 141.87(13) 19_655 . ? O6 Zr2 O1 141.87(13) 19_655 16 ? O6 Zr2 O1 141.87(13) . 19_655 ? O6 Zr2 O1 78.4(3) 19_655 19_655 ? O6 Zr2 O1 78.4(3) 19_655 11_655 ? O6 Zr2 O1 78.4(3) . . ? O6 Zr2 O6 111.7(6) . 19_655 ? C16 O3 Zr1 127.5(13) . . ? Zr1 O5 Zr1 111.1(3) . 4_655 ? Zr1 O5 Zr2 108.5(3) . . ? Zr1 O5 Zr2 108.5(3) 4_655 . ? C1 O1 Zr2 132.5(5) . . ? Zr1 O6 Zr1 110.7(4) . 16 ? Zr1 O6 Zr2 108.0(3) . . ? Zr1 O6 Zr2 108.0(3) 16 . ? C2 C0AA C4 120.6(9) . . ? C9 O8 C10 104.2(14) . . ? O1 C1 C2 118.4(8) . . ? O1 C1 O2 124.2(8) . . ? O2 C1 C2 117.3(8) . . ? C0AA C2 C1 122.2(8) . . ? C7 C2 C0AA 120.5(9) . . ? C7 C2 C1 117.1(8) . . ? C5 C4 C0AA 120.3(10) . . ? C11 C8 C5 121.1(12) . . ? C11 C8 C9 112.4(15) . . ? C9 C8 C5 126.4(12) . . ? C4 C5 C8 120.1(10) . . ? C4 C5 C6 119.1(10) . . ? C6 C5 C8 120.0(12) . . ? C14 C13 C12 118.7(14) . . ? C14 C13 C15 120.0(7) . . ? C15 C13 C12 121.3(14) . . ? C11 C12 C13 120.6(10) 21_665 . ? C11 C12 C13 120.6(10) . . ? C11 C12 C11 118.4(19) . 21_665 ? C8 C11 C12 122.8(15) . . ? C5 C6 C7 122.4(12) . . ? C2 C7 C6 116.7(10) . . ? C8 C9 O8 114.5(10) . . ? C8 C9 O8 114.5(10) 21_665 . ? C8 C9 C8 130.7(19) . 21_665 ? C1 O2 Zr1 136.0(5) . . ? C13 C14 C14 120.5(5) . 16_556 ? C13 C15 C15 119.5(5) . 16_556 ? N1 Ru1 N1 70.1(7) 16_556 . ? N1 Ru1 N26 93(2) 16_556 . ? N1 Ru1 N26 87.7(18) . . ? N2 Ru1 N1 169.8(13) . . ? N2 Ru1 N1 169.8(13) 16_556 16_556 ? N2 Ru1 N1 99.7(13) . 16_556 ? N2 Ru1 N1 99.7(13) 16_556 . ? N2 Ru1 N2 90(2) 16_556 . ? N2 Ru1 N26 92.9(18) . . ? N2 Ru1 N26 87(2) 16_556 . ? C21 N1 Ru1 115.0(8) . . ? C21 N1 C20 120.6 . . ? C21 N1 C20 120.48(14) . 23 ? C20 N1 Ru1 123.3(8) . . ? C20 N1 Ru1 123.3(8) 23 . ? C20 N1 C20 19.8(13) . 23 ? C17 C21 N1 119.30(11) 23 . ? C17 C21 N1 119.2 . . ? C17 C21 C17 13(2) 23 . ? C21 C17 C18 120.2 . . ? C21 C17 C18 114.6(6) . 23 ? C21 C17 C16 128.9(12) . . ? C17 C17 C21 83.38(13) 23 . ? C17 C17 C18 99.29(15) 23 . ? C17 C17 C18 69(2) 23 23 ? C17 C17 C16 84.1(16) 23 . ? C18 C17 C18 30.3(19) . 23 ? C18 C17 C16 106.3(16) 23 . ? C18 C17 C16 110.6(12) . . ? C17 C18 C17 11.8(18) . 23 ? C17 C18 C19 103.2(16) 23 23 ? C17 C18 C19 110.5(6) . 23 ? C18 C18 C17 69.0(18) 23 23 ? C18 C18 C17 80.7 23 . ? C18 C18 C19 60.2(15) 23 23 ? C18 C18 C19 91.8 23 . ? C19 C18 C17 118.6(3) . 23 ? C19 C18 C17 120.0 . . ? C19 C18 C19 31.6(15) . 23 ? C18 C19 C18 28.0(16) . 23 ? C18 C19 C20 116.5(3) . 23 ? C18 C19 C20 120.0 . . ? C19 C19 C18 88.2 23 . ? C19 C19 C18 60.2(16) 23 23 ? C19 C19 C20 64.5(11) 23 23 ? C19 C19 C20 82.5 23 . ? C20 C19 C18 111.9(6) . 23 ? C20 C19 C18 100.6(14) 23 23 ? C20 C19 C20 18.0(11) . 23 ? N1 C20 C19 111.1(6) . 23 ? N1 C20 C20 110.7 . 16_556 ? N1 C20 C20 106.3(6) . 7_556 ? C19 C20 N1 119.9 . . ? C19 C20 C19 33.0(16) . 23 ? C19 C20 C20 130.0(2) . 7_556 ? C19 C20 C20 129.4 . 16_556 ? C20 C20 N1 80.1 23 . ? C20 C20 C19 64.5(17) 23 23 ? C20 C20 C19 114(2) 7_556 23 ? C20 C20 C19 97.5 23 . ? C20 C20 C19 125.3(6) 16_556 23 ? C20 C20 C20 18(2) 16_556 7_556 ? C20 C20 C20 90.0 23 16_556 ? C20 C20 C20 72(2) 23 7_556 ? O3 C16 O4 123.7(19) . . ? O3 C16 C17 126.6(19) . 23 ? O3 C16 C17 126.6(19) . . ? O4 C16 C17 109.3(10) . 23 ? O4 C16 C17 109.3(10) . . ? C17 C16 C17 12(2) . 23 ? C28 N2 Ru1 128.0(4) 23 . ? C28 N2 Ru1 128.0(4) . . ? C28 N2 C28 104.0(6) 23 . ? C28 N2 C27 106(4) 23 . ? C28 N2 C27 2(4) 23 23 ? C28 N2 C27 106(4) . 23 ? C28 N2 C27 2(4) . . ? C27 N2 Ru1 126(4) 23 . ? C27 N2 Ru1 126(4) . . ? C27 N2 C27 109(7) 23 . ? N2 C28 C29 128.0(4) . . ? C27 C28 N2 162(10) . . ? C27 C28 C29 70(10) . . ? C29 C30 C29 160(10) . 23 ? C28 C29 C27 7(4) . . ? C30 C29 C28 100(6) . . ? C30 C29 C27 107(8) . . ? N2 C27 C29 119(7) . . ? C28 C27 N2 16(10) . . ? C28 C27 C29 103(10) . . ? C22 C3 N26 119.9 . . ? C3 C22 C23 120.1 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? N26 C25 C24 120.0 . . ? C3 N26 Ru1 100(5) . . ? C25 N26 Ru1 137(5) . . ? C25 N26 C3 120.1 . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.755 -0.888 -0.894 18871.5 2135.7 ? _olex2_submission_special_instructions 'No special instructions were received' # start Validation Reply Form _vrf_PLAT132_PCN-808-BDBR ; PROBLEM: Trigonal/Hexagonal a and b Differ .............. Please Check RESPONSE: a and b are equal ; # end Validation Reply Form ####################################################################### data_BDBR _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H28 N6 O7 Ru' _chemical_formula_weight 709.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'orthorhombic' _space_group_IT_number 61 _space_group_name_H-M_alt 'P c a b' _space_group_name_Hall '-P 2bc 2ac' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 14.4913(4) _cell_length_b 18.0990(5) _cell_length_c 25.5467(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6700.3(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9555 _cell_measurement_theta_min 4.2744 _cell_measurement_theta_max 72.5789 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_F_000 2896 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_absorpt_coefficient_mu 4.246 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5988 _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 79275 _diffrn_reflns_av_unetI/netI 0.0156 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.460 _diffrn_reflns_theta_max 72.579 _diffrn_reflns_theta_full 67.684 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 6637 _reflns_number_gt 6310 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT+ ver. (Bruker, 2001)' _computing_data_reduction 'SAINT+ ver. (Bruker, 2001)' _computing_structure_solution 'XS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0813P)^2^+39.9705P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6637 _refine_ls_number_parameters 427 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.1865 _refine_ls_wR_factor_gt 0.1853 _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.11155(3) 0.03736(2) 0.33281(2) 0.02076(15) Uani 1 1 d . . . . . O1 O 0.0818(3) 0.38036(19) 0.42153(16) 0.0288(8) Uani 1 1 d . . . . . O2 O 0.2096(2) 0.3129(2) 0.41287(16) 0.0299(8) Uani 1 1 d . . . . . O3 O -0.2626(4) -0.1742(2) 0.3487(2) 0.0581(14) Uani 1 1 d . . . . . O4 O -0.1178(4) -0.2115(2) 0.33535(18) 0.0494(13) Uani 1 1 d . . . . . O5 O -0.1506(10) -0.1980(6) 0.4710(4) 0.073(2) Uani 0.543(9) 1 d . U P A 1 O6 O -0.0672(12) -0.1588(9) 0.4751(5) 0.063(2) Uani 0.382(9) 1 d . . P B 2 O7 O -0.1376(11) -0.2745(7) 0.4516(5) 0.073(2) Uani 0.457(9) 1 d . U P A 2 O8 O -0.4138(11) -0.2769(8) 0.3823(8) 0.108(6) Uani 0.5 1 d . . P . . O9 O -0.030(2) 0.4239(18) 0.5226(12) 0.196(12) Uiso 0.5 1 d . . P . . O10 O -0.0459(7) -0.1035(5) 0.4896(3) 0.063(2) Uani 0.618(9) 1 d . . P B 1 N1 N 0.0600(3) 0.1290(2) 0.37016(16) 0.0208(8) Uani 1 1 d . . . . . N2 N -0.0195(3) 0.0020(2) 0.35104(16) 0.0238(9) Uani 1 1 d . . . . . N3 N 0.0656(3) 0.0656(2) 0.25911(16) 0.0230(9) Uani 1 1 d . . . . . N4 N 0.1525(3) -0.0536(2) 0.28997(16) 0.0235(9) Uani 1 1 d . . . . . N5 N 0.1728(4) 0.0032(3) 0.40108(17) 0.0322(11) Uani 1 1 d . . . . . N6 N 0.2426(3) 0.0795(2) 0.32339(16) 0.0241(9) Uani 1 1 d . . . . . C1 C 0.1245(3) 0.3213(3) 0.41444(19) 0.0218(10) Uani 1 1 d . . . . . C2 C 0.0667(3) 0.2519(3) 0.40513(18) 0.0202(9) Uani 1 1 d . . . . . C3 C 0.1066(3) 0.1907(3) 0.38171(19) 0.0204(9) Uani 1 1 d . . . . . H3 H 0.170470 0.192594 0.373420 0.024 Uiso 1 1 calc R U . . . C4 C -0.0261(3) 0.2485(3) 0.41785(19) 0.0225(10) Uani 1 1 d . . . . . H4 H -0.055580 0.289709 0.433741 0.027 Uiso 1 1 calc R U . . . C5 C -0.0757(3) 0.1849(3) 0.4073(2) 0.0214(10) Uani 1 1 d . . . . . H5 H -0.139269 0.181793 0.416065 0.026 Uiso 1 1 calc R U . . . C6 C -0.0310(3) 0.1252(2) 0.38358(18) 0.0190(9) Uani 1 1 d . . . . . C7 C -0.0766(4) 0.0540(3) 0.37241(19) 0.0211(10) Uani 1 1 d . . . . . C8 C -0.1685(4) 0.0386(3) 0.38432(19) 0.0214(10) Uani 1 1 d . . . . . H8 H -0.207778 0.076005 0.397896 0.026 Uiso 1 1 calc R U . . . C9 C -0.2015(4) -0.0322(3) 0.3760(2) 0.0255(11) Uani 1 1 d . . . . . H9 H -0.263807 -0.043917 0.384013 0.031 Uiso 1 1 calc R U . . . C10 C -0.1430(4) -0.0859(3) 0.35593(19) 0.0273(11) Uani 1 1 d . . . . . C11 C -0.0538(4) -0.0666(3) 0.3434(2) 0.0271(11) Uani 1 1 d . . . . . H11 H -0.014540 -0.103160 0.328808 0.033 Uiso 1 1 calc R U . . . C12 C -0.1776(5) -0.1650(3) 0.3462(2) 0.0381(14) Uani 1 1 d . . . . . C13 C 0.0155(4) 0.1259(3) 0.2464(2) 0.0278(11) Uani 1 1 d . . . . . H13 H -0.000174 0.159706 0.273436 0.033 Uiso 1 1 calc R U . . . C14 C -0.0139(4) 0.1406(3) 0.1963(2) 0.0359(13) Uani 1 1 d . . . . . H14 H -0.048410 0.184024 0.188836 0.043 Uiso 1 1 calc R U . . . C15 C 0.0079(4) 0.0905(3) 0.1567(2) 0.0366(13) Uani 1 1 d . . . . . H15 H -0.012145 0.098912 0.121767 0.044 Uiso 1 1 calc R U . . . C16 C 0.0594(4) 0.0281(3) 0.1688(2) 0.0275(11) Uani 1 1 d . . . . . H16 H 0.075620 -0.006372 0.142380 0.033 Uiso 1 1 calc R U . . . C17 C 0.0868(3) 0.0169(3) 0.2204(2) 0.0221(10) Uani 1 1 d . . . . . C18 C 0.1383(3) -0.0489(3) 0.2376(2) 0.0213(10) Uani 1 1 d . . . . . C19 C 0.1710(4) -0.1033(3) 0.2035(2) 0.0258(10) Uani 1 1 d . . . . . H19 H 0.161828 -0.098467 0.166821 0.031 Uiso 1 1 calc R U . . . C20 C 0.2162(4) -0.1638(3) 0.2232(2) 0.0302(12) Uani 1 1 d . . . . . H20 H 0.239362 -0.200911 0.200393 0.036 Uiso 1 1 calc R U . . . C21 C 0.2278(5) -0.1701(3) 0.2770(2) 0.0372(14) Uani 1 1 d . . . . . H21 H 0.257088 -0.212307 0.291573 0.045 Uiso 1 1 calc R U . . . C22 C 0.1957(4) -0.1138(3) 0.3091(2) 0.0333(13) Uani 1 1 d . . . . . H22 H 0.204609 -0.117768 0.345868 0.040 Uiso 1 1 calc R U . . . C23 C 0.2733(4) 0.1211(3) 0.2832(2) 0.0275(11) Uani 1 1 d . . . . . H23 H 0.232352 0.131328 0.255030 0.033 Uiso 1 1 calc R U . . . C24 C 0.3614(4) 0.1493(3) 0.2812(2) 0.0337(12) Uani 1 1 d . . . . . H24 H 0.380666 0.178378 0.252249 0.040 Uiso 1 1 calc R U . . . C25 C 0.4215(4) 0.1350(4) 0.3219(3) 0.0422(16) Uani 1 1 d . . . . . H25 H 0.482136 0.154925 0.321836 0.051 Uiso 1 1 calc R U . . . C26 C 0.3913(4) 0.0908(4) 0.3630(3) 0.0415(16) Uani 1 1 d . . . . . H26 H 0.432056 0.078982 0.390919 0.050 Uiso 1 1 calc R U . . . C27 C 0.3024(4) 0.0642(3) 0.3632(2) 0.0305(12) Uani 1 1 d . . . . . C28 C 0.2640(4) 0.0192(3) 0.4056(2) 0.0358(13) Uani 1 1 d . . . . . C29 C 0.3158(6) -0.0058(4) 0.4485(3) 0.0520(19) Uani 1 1 d . . . . . H29 H 0.379778 0.005000 0.451288 0.062 Uiso 1 1 calc R U . . . C30 C 0.2706(7) -0.0470(4) 0.4870(3) 0.055(2) Uani 1 1 d . . . . . H30 H 0.303832 -0.064590 0.516498 0.066 Uiso 1 1 calc R U . . . C31 C 0.1795(6) -0.0618(4) 0.4821(3) 0.0523(19) Uani 1 1 d . . . . . H31 H 0.149103 -0.090401 0.508097 0.063 Uiso 1 1 calc R U . . . C32 C 0.1299(6) -0.0353(3) 0.4393(2) 0.0403(15) Uani 1 1 d . . . . . H32 H 0.065473 -0.044492 0.436967 0.048 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0264(2) 0.0176(2) 0.0182(2) -0.00088(13) 0.00057(14) 0.00898(14) O1 0.0240(18) 0.0204(18) 0.042(2) -0.0052(15) -0.0086(16) -0.0020(14) O2 0.0194(17) 0.0281(19) 0.042(2) 0.0026(16) 0.0009(16) -0.0024(15) O3 0.073(4) 0.027(2) 0.074(3) -0.014(2) 0.013(3) -0.021(2) O4 0.085(4) 0.016(2) 0.047(3) -0.0082(17) 0.005(2) 0.002(2) O5 0.123(6) 0.049(4) 0.046(4) 0.013(3) -0.009(4) -0.016(4) O6 0.094(6) 0.058(4) 0.039(4) 0.009(3) -0.017(4) -0.006(4) O7 0.123(6) 0.049(4) 0.046(4) 0.013(3) -0.009(4) -0.016(4) O8 0.087(10) 0.073(9) 0.164(17) 0.053(10) -0.033(11) -0.018(8) O10 0.094(6) 0.058(4) 0.039(4) 0.009(3) -0.017(4) -0.006(4) N1 0.024(2) 0.0175(18) 0.0206(19) -0.0010(15) 0.0011(16) 0.0032(16) N2 0.035(2) 0.0151(19) 0.021(2) -0.0019(16) 0.0016(17) 0.0045(17) N3 0.023(2) 0.020(2) 0.026(2) 0.0016(17) 0.0001(17) 0.0034(16) N4 0.027(2) 0.022(2) 0.022(2) -0.0027(16) -0.0034(17) 0.0089(17) N5 0.052(3) 0.026(2) 0.019(2) -0.0016(17) -0.004(2) 0.016(2) N6 0.025(2) 0.025(2) 0.0217(19) -0.0054(17) -0.0014(17) 0.0125(18) C1 0.026(2) 0.019(2) 0.021(2) 0.0029(18) -0.0030(19) -0.0031(19) C2 0.021(2) 0.019(2) 0.020(2) 0.0009(18) -0.0005(18) -0.0002(18) C3 0.018(2) 0.020(2) 0.023(2) 0.0002(19) 0.0023(18) 0.0038(18) C4 0.024(2) 0.016(2) 0.027(2) -0.0043(19) -0.0017(19) 0.0018(18) C5 0.021(2) 0.016(2) 0.028(2) -0.0029(18) -0.0023(19) 0.0007(18) C6 0.020(2) 0.016(2) 0.021(2) -0.0006(17) -0.0031(18) 0.0031(18) C7 0.027(2) 0.016(2) 0.020(2) -0.0016(18) -0.0025(19) 0.0041(19) C8 0.026(2) 0.018(2) 0.021(2) -0.0006(17) -0.001(2) -0.0007(18) C9 0.033(3) 0.019(2) 0.025(3) 0.0011(19) -0.004(2) -0.003(2) C10 0.047(3) 0.015(2) 0.019(2) -0.0003(18) -0.004(2) -0.002(2) C11 0.043(3) 0.015(2) 0.023(2) -0.0018(19) 0.003(2) 0.002(2) C12 0.068(4) 0.019(3) 0.027(3) -0.002(2) 0.004(3) -0.010(3) C13 0.027(3) 0.024(2) 0.032(3) 0.000(2) -0.005(2) 0.009(2) C14 0.036(3) 0.027(3) 0.045(3) 0.008(2) -0.012(3) 0.010(2) C15 0.043(3) 0.034(3) 0.033(3) 0.004(2) -0.014(3) 0.005(3) C16 0.027(3) 0.027(3) 0.029(3) 0.002(2) -0.004(2) -0.002(2) C17 0.020(2) 0.021(2) 0.025(2) 0.001(2) 0.0000(19) 0.0006(19) C18 0.018(2) 0.022(2) 0.024(2) 0.0004(19) 0.0029(19) -0.0006(18) C19 0.027(3) 0.024(2) 0.026(3) -0.005(2) 0.000(2) -0.001(2) C20 0.028(3) 0.025(3) 0.037(3) -0.009(2) 0.004(2) 0.007(2) C21 0.049(4) 0.023(3) 0.040(3) -0.003(2) -0.009(3) 0.019(2) C22 0.045(3) 0.026(3) 0.029(3) 0.000(2) -0.006(2) 0.017(2) C23 0.025(3) 0.033(3) 0.025(2) -0.007(2) -0.002(2) 0.003(2) C24 0.030(3) 0.040(3) 0.031(3) -0.014(2) 0.007(2) 0.001(2) C25 0.024(3) 0.061(4) 0.041(3) -0.024(3) -0.005(3) 0.006(3) C26 0.035(3) 0.055(4) 0.034(3) -0.018(3) -0.010(3) 0.022(3) C27 0.029(3) 0.036(3) 0.027(3) -0.010(2) -0.010(2) 0.020(2) C28 0.045(3) 0.035(3) 0.027(3) -0.009(2) -0.011(3) 0.021(3) C29 0.073(5) 0.052(4) 0.031(3) -0.005(3) -0.017(3) 0.030(4) C30 0.092(6) 0.046(4) 0.027(3) 0.004(3) -0.011(4) 0.029(4) C31 0.093(6) 0.040(4) 0.025(3) 0.004(3) -0.005(3) 0.012(4) C32 0.068(5) 0.028(3) 0.025(3) 0.003(2) 0.001(3) 0.005(3) _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 Ru1 N5 2.052(4) . ? Ru1 N1 2.055(4) . ? Ru1 N2 2.058(5) . ? Ru1 N6 2.061(5) . ? Ru1 N3 2.062(4) . ? Ru1 N4 2.064(4) . ? O1 C1 1.248(6) . ? O2 C1 1.244(6) . ? O3 C12 1.244(9) . ? O4 C12 1.240(8) . ? N1 C3 1.337(6) . ? N1 C6 1.364(6) . ? N2 C11 1.351(7) . ? N2 C7 1.366(6) . ? N3 C13 1.349(6) . ? N3 C17 1.360(7) . ? N4 C22 1.348(7) . ? N4 C18 1.356(7) . ? N5 C32 1.352(8) . ? N5 C28 1.358(8) . ? N6 C23 1.349(7) . ? N6 C27 1.365(7) . ? C1 C2 1.528(7) . ? C2 C4 1.384(7) . ? C2 C3 1.386(7) . ? C4 C5 1.384(7) . ? C5 C6 1.397(7) . ? C6 C7 1.476(7) . ? C7 C8 1.395(7) . ? C8 C9 1.383(7) . ? C9 C10 1.388(8) . ? C10 C11 1.376(8) . ? C10 C12 1.537(7) . ? C13 C14 1.376(8) . ? C14 C15 1.397(9) . ? C15 C16 1.388(8) . ? C16 C17 1.390(7) . ? C17 C18 1.473(7) . ? C18 C19 1.398(7) . ? C19 C20 1.373(8) . ? C20 C21 1.389(8) . ? C21 C22 1.389(8) . ? C23 C24 1.377(8) . ? C24 C25 1.380(9) . ? C25 C26 1.391(11) . ? C26 C27 1.375(9) . ? C27 C28 1.463(9) . ? C28 C29 1.404(8) . ? C29 C30 1.397(12) . ? C30 C31 1.353(12) . ? C31 C32 1.393(9) . ? 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 N5 Ru1 N1 90.33(17) . . ? N5 Ru1 N2 96.49(19) . . ? N1 Ru1 N2 79.07(16) . . ? N5 Ru1 N6 79.17(19) . . ? N1 Ru1 N6 95.21(16) . . ? N2 Ru1 N6 172.87(16) . . ? N5 Ru1 N3 172.14(18) . . ? N1 Ru1 N3 96.10(16) . . ? N2 Ru1 N3 89.18(17) . . ? N6 Ru1 N3 95.70(17) . . ? N5 Ru1 N4 94.93(17) . . ? N1 Ru1 N4 174.20(16) . . ? N2 Ru1 N4 97.89(17) . . ? N6 Ru1 N4 88.18(17) . . ? N3 Ru1 N4 78.85(16) . . ? C3 N1 C6 118.4(4) . . ? C3 N1 Ru1 126.3(3) . . ? C6 N1 Ru1 115.3(3) . . ? C11 N2 C7 117.9(5) . . ? C11 N2 Ru1 126.4(4) . . ? C7 N2 Ru1 115.8(3) . . ? C13 N3 C17 118.1(4) . . ? C13 N3 Ru1 126.4(4) . . ? C17 N3 Ru1 115.5(3) . . ? C22 N4 C18 118.7(4) . . ? C22 N4 Ru1 125.8(4) . . ? C18 N4 Ru1 115.4(3) . . ? C32 N5 C28 119.8(5) . . ? C32 N5 Ru1 124.8(5) . . ? C28 N5 Ru1 115.4(4) . . ? C23 N6 C27 118.2(5) . . ? C23 N6 Ru1 126.8(4) . . ? C27 N6 Ru1 115.0(4) . . ? O2 C1 O1 126.9(5) . . ? O2 C1 C2 116.0(4) . . ? O1 C1 C2 117.1(4) . . ? C4 C2 C3 118.1(4) . . ? C4 C2 C1 122.1(4) . . ? C3 C2 C1 119.7(4) . . ? N1 C3 C2 123.5(4) . . ? C5 C4 C2 119.7(5) . . ? C4 C5 C6 119.2(4) . . ? N1 C6 C5 121.2(4) . . ? N1 C6 C7 115.3(4) . . ? C5 C6 C7 123.5(4) . . ? N2 C7 C8 121.9(4) . . ? N2 C7 C6 114.1(4) . . ? C8 C7 C6 124.0(4) . . ? C9 C8 C7 118.8(5) . . ? C8 C9 C10 119.6(5) . . ? C11 C10 C9 118.8(5) . . ? C11 C10 C12 120.4(5) . . ? C9 C10 C12 120.8(5) . . ? N2 C11 C10 123.1(5) . . ? O4 C12 O3 127.7(6) . . ? O4 C12 C10 116.1(6) . . ? O3 C12 C10 116.1(6) . . ? N3 C13 C14 123.2(5) . . ? C13 C14 C15 118.6(5) . . ? C16 C15 C14 119.2(5) . . ? C15 C16 C17 119.0(5) . . ? N3 C17 C16 122.0(5) . . ? N3 C17 C18 114.9(4) . . ? C16 C17 C18 123.0(5) . . ? N4 C18 C19 121.3(5) . . ? N4 C18 C17 115.0(4) . . ? C19 C18 C17 123.7(5) . . ? C20 C19 C18 119.7(5) . . ? C19 C20 C21 119.1(5) . . ? C20 C21 C22 119.0(5) . . ? N4 C22 C21 122.2(5) . . ? N6 C23 C24 122.7(5) . . ? C23 C24 C25 119.2(6) . . ? C24 C25 C26 118.6(6) . . ? C27 C26 C25 119.9(6) . . ? N6 C27 C26 121.3(6) . . ? N6 C27 C28 115.0(5) . . ? C26 C27 C28 123.7(5) . . ? N5 C28 C29 121.2(7) . . ? N5 C28 C27 115.2(5) . . ? C29 C28 C27 123.6(6) . . ? C30 C29 C28 118.1(8) . . ? C31 C30 C29 119.9(6) . . ? C30 C31 C32 120.5(7) . . ? N5 C32 C31 120.5(7) . . ? _refine_diff_density_max 2.247 _refine_diff_density_min -1.308 _refine_diff_density_rms 0.172 _shelx_res_file ; TITL p in Pcab #61 C:\SINGLE~1\Ru-BPy\2\p.res created by SHELXL-2016/6 at 14:38:04 on 28-Jan-2019 CELL 1.54184 14.4913 18.0990 25.5467 90.000 90.000 90.000 ZERR 8.0000 0.0004 0.0005 0.0007 0.000 0.000 0.000 LATT 1 SYMM -X, 0.5-Y, 0.5+Z SYMM 0.5+X, -Y, 0.5-Z SYMM 0.5-X, 0.5+Y, -Z SFAC C H O N RU UNIT 256 224 56 48 8 BOND eadp o6 o10 eadp o5 o7 isor 0.005 o5 o7 ACTA FMAP 2 53 53 PLAN 20 0 0 TEMP -173.15 L.S. 24 WGHT 0.081300 39.970501 FVAR 0.22488 0.61846 0.54323 RU1 5 0.111551 0.037360 0.332810 11.00000 0.02642 0.01762 = 0.01823 -0.00088 0.00057 0.00898 O1 3 0.081849 0.380355 0.421526 11.00000 0.02396 0.02041 = 0.04206 -0.00517 -0.00861 -0.00198 O2 3 0.209628 0.312852 0.412871 11.00000 0.01943 0.02808 = 0.04232 0.00257 0.00086 -0.00236 O3 3 -0.262561 -0.174244 0.348655 11.00000 0.07323 0.02721 = 0.07384 -0.01359 0.01342 -0.02084 O4 3 -0.117818 -0.211536 0.335349 11.00000 0.08506 0.01614 = 0.04710 -0.00819 0.00517 0.00172 PART 1 O5 3 -0.150601 -0.198040 0.471005 31.00000 0.12297 0.04861 = 0.04602 0.01263 -0.00948 -0.01565 PART 2 O6 3 -0.067234 -0.158759 0.475110 -21.00000 0.09409 0.05773 = 0.03855 0.00910 -0.01739 -0.00562 O7 3 -0.137552 -0.274510 0.451635 -31.00000 0.12297 0.04861 = 0.04602 0.01263 -0.00948 -0.01565 PART 0 O8 3 -0.413799 -0.276869 0.382322 10.50000 0.08677 0.07307 = 0.16416 0.05331 -0.03310 -0.01809 O9 3 -0.030449 0.423854 0.522639 10.50000 0.19644 PART 1 O10 3 -0.045937 -0.103532 0.489553 21.00000 0.09409 0.05773 = 0.03855 0.00910 -0.01739 -0.00562 PART 0 N1 4 0.059988 0.129026 0.370158 11.00000 0.02430 0.01751 = 0.02061 -0.00098 0.00108 0.00323 N2 4 -0.019520 0.001996 0.351041 11.00000 0.03523 0.01510 = 0.02098 -0.00195 0.00165 0.00452 N3 4 0.065584 0.065616 0.259111 11.00000 0.02311 0.02024 = 0.02570 0.00163 0.00013 0.00342 N4 4 0.152503 -0.053622 0.289974 11.00000 0.02704 0.02185 = 0.02156 -0.00273 -0.00340 0.00892 N5 4 0.172786 0.003203 0.401084 11.00000 0.05194 0.02598 = 0.01880 -0.00159 -0.00383 0.01603 N6 4 0.242626 0.079481 0.323387 11.00000 0.02515 0.02547 = 0.02171 -0.00543 -0.00137 0.01254 C1 1 0.124485 0.321280 0.414444 11.00000 0.02594 0.01883 = 0.02059 0.00292 -0.00301 -0.00310 C2 1 0.066678 0.251895 0.405129 11.00000 0.02126 0.01944 = 0.01982 0.00090 -0.00049 -0.00021 C3 1 0.106607 0.190668 0.381708 11.00000 0.01824 0.01994 = 0.02293 0.00023 0.00232 0.00376 AFIX 43 H3 2 0.170470 0.192594 0.373420 11.00000 -1.20000 AFIX 0 C4 1 -0.026098 0.248541 0.417851 11.00000 0.02395 0.01638 = 0.02711 -0.00426 -0.00165 0.00184 AFIX 43 H4 2 -0.055580 0.289709 0.433741 11.00000 -1.20000 AFIX 0 C5 1 -0.075679 0.184875 0.407293 11.00000 0.02075 0.01575 = 0.02780 -0.00286 -0.00227 0.00073 AFIX 43 H5 2 -0.139269 0.181793 0.416065 11.00000 -1.20000 AFIX 0 C6 1 -0.031015 0.125217 0.383576 11.00000 0.01993 0.01595 = 0.02121 -0.00061 -0.00306 0.00311 C7 1 -0.076594 0.053983 0.372405 11.00000 0.02733 0.01554 = 0.02035 -0.00160 -0.00247 0.00412 C8 1 -0.168525 0.038585 0.384322 11.00000 0.02569 0.01802 = 0.02063 -0.00062 -0.00125 -0.00072 AFIX 43 H8 2 -0.207778 0.076005 0.397896 11.00000 -1.20000 AFIX 0 C9 1 -0.201492 -0.032154 0.376017 11.00000 0.03269 0.01890 = 0.02480 0.00108 -0.00419 -0.00338 AFIX 43 H9 2 -0.263807 -0.043917 0.384013 11.00000 -1.20000 AFIX 0 C10 1 -0.143000 -0.085884 0.355928 11.00000 0.04698 0.01545 = 0.01942 -0.00028 -0.00425 -0.00202 C11 1 -0.053814 -0.066564 0.343447 11.00000 0.04318 0.01522 = 0.02297 -0.00183 0.00339 0.00185 AFIX 43 H11 2 -0.014540 -0.103160 0.328808 11.00000 -1.20000 AFIX 0 C12 1 -0.177643 -0.164979 0.346213 11.00000 0.06803 0.01896 = 0.02729 -0.00183 0.00367 -0.01002 C13 1 0.015512 0.125855 0.246445 11.00000 0.02725 0.02362 = 0.03246 0.00009 -0.00474 0.00944 AFIX 43 H13 2 -0.000174 0.159706 0.273436 11.00000 -1.20000 AFIX 0 C14 1 -0.013944 0.140640 0.196313 11.00000 0.03552 0.02738 = 0.04466 0.00785 -0.01217 0.00960 AFIX 43 H14 2 -0.048410 0.184024 0.188836 11.00000 -1.20000 AFIX 0 C15 1 0.007943 0.090461 0.156655 11.00000 0.04349 0.03356 = 0.03280 0.00392 -0.01381 0.00455 AFIX 43 H15 2 -0.012145 0.098912 0.121767 11.00000 -1.20000 AFIX 0 C16 1 0.059383 0.028129 0.168848 11.00000 0.02682 0.02704 = 0.02873 0.00151 -0.00434 -0.00199 AFIX 43 H16 2 0.075620 -0.006372 0.142380 11.00000 -1.20000 AFIX 0 C17 1 0.086796 0.016942 0.220395 11.00000 0.01978 0.02115 = 0.02525 0.00097 0.00005 0.00060 C18 1 0.138343 -0.048884 0.237599 11.00000 0.01771 0.02232 = 0.02380 0.00038 0.00286 -0.00063 C19 1 0.170954 -0.103324 0.203485 11.00000 0.02733 0.02377 = 0.02639 -0.00503 -0.00035 -0.00055 AFIX 43 H19 2 0.161828 -0.098467 0.166821 11.00000 -1.20000 AFIX 0 C20 1 0.216230 -0.163838 0.223215 11.00000 0.02814 0.02532 = 0.03707 -0.00893 0.00409 0.00733 AFIX 43 H20 2 0.239362 -0.200911 0.200393 11.00000 -1.20000 AFIX 0 C21 1 0.227755 -0.170120 0.276988 11.00000 0.04870 0.02320 = 0.03964 -0.00347 -0.00885 0.01855 AFIX 43 H21 2 0.257088 -0.212307 0.291573 11.00000 -1.20000 AFIX 0 C22 1 0.195737 -0.113776 0.309132 11.00000 0.04458 0.02641 = 0.02894 0.00009 -0.00601 0.01687 AFIX 43 H22 2 0.204609 -0.117768 0.345868 11.00000 -1.20000 AFIX 0 C23 1 0.273266 0.121099 0.283167 11.00000 0.02544 0.03264 = 0.02453 -0.00695 -0.00157 0.00314 AFIX 43 H23 2 0.232352 0.131328 0.255030 11.00000 -1.20000 AFIX 0 C24 1 0.361412 0.149349 0.281243 11.00000 0.03023 0.03951 = 0.03144 -0.01389 0.00676 0.00088 AFIX 43 H24 2 0.380666 0.178378 0.252249 11.00000 -1.20000 AFIX 0 C25 1 0.421479 0.135014 0.321912 11.00000 0.02399 0.06128 = 0.04126 -0.02420 -0.00478 0.00556 AFIX 43 H25 2 0.482136 0.154925 0.321836 11.00000 -1.20000 AFIX 0 C26 1 0.391300 0.090785 0.363018 11.00000 0.03536 0.05536 = 0.03388 -0.01785 -0.00987 0.02180 AFIX 43 H26 2 0.432056 0.078982 0.390919 11.00000 -1.20000 AFIX 0 C27 1 0.302403 0.064152 0.363238 11.00000 0.02910 0.03573 = 0.02672 -0.00987 -0.00965 0.01970 C28 1 0.264000 0.019176 0.405553 11.00000 0.04504 0.03502 = 0.02724 -0.00886 -0.01126 0.02107 C29 1 0.315815 -0.005802 0.448488 11.00000 0.07269 0.05197 = 0.03135 -0.00530 -0.01749 0.02976 AFIX 43 H29 2 0.379778 0.005000 0.451288 11.00000 -1.20000 AFIX 0 C30 1 0.270626 -0.046985 0.486960 11.00000 0.09201 0.04596 = 0.02735 0.00378 -0.01102 0.02860 AFIX 43 H30 2 0.303832 -0.064590 0.516498 11.00000 -1.20000 AFIX 0 C31 1 0.179488 -0.061785 0.482120 11.00000 0.09270 0.03954 = 0.02462 0.00362 -0.00526 0.01189 AFIX 43 H31 2 0.149103 -0.090401 0.508097 11.00000 -1.20000 AFIX 0 C32 1 0.129896 -0.035350 0.439306 11.00000 0.06847 0.02772 = 0.02474 0.00298 0.00140 0.00515 AFIX 43 H32 2 0.065473 -0.044492 0.436967 11.00000 -1.20000 AFIX 0 HKLF 4 REM p in Pcab #61 REM R1 = 0.0632 for 6310 Fo > 4sig(Fo) and 0.0651 for all 6637 data REM 427 parameters refined using 12 restraints END WGHT 0.0814 39.9161 REM Highest difference peak 2.247, deepest hole -1.308, 1-sigma level 0.172 Q1 1 -0.2276 -0.1603 0.4867 11.00000 0.05 2.25 Q2 1 -0.0686 -0.2213 0.4592 11.00000 0.05 1.90 Q3 1 -0.1213 -0.1395 0.4842 11.00000 0.05 1.88 Q4 1 -0.1041 0.3569 0.5456 11.00000 0.05 1.43 Q5 1 -0.4816 -0.2732 0.4406 11.00000 0.05 1.39 Q6 1 -0.0986 0.4175 0.5424 11.00000 0.05 1.39 Q7 1 -0.2943 -0.1816 0.4745 11.00000 0.05 1.38 Q8 1 -0.4557 -0.2004 0.4443 11.00000 0.05 1.28 Q9 1 -0.0578 -0.2933 0.4582 11.00000 0.05 1.13 Q10 1 -0.0246 -0.1478 0.4755 11.00000 0.05 0.87 Q11 1 -0.0092 0.4340 0.5028 11.00000 0.05 0.83 Q12 1 0.0576 -0.0374 0.1649 11.00000 0.05 0.81 Q13 1 -0.2046 -0.2645 0.4589 11.00000 0.05 0.76 Q14 1 -0.3093 -0.2609 0.4602 11.00000 0.05 0.70 Q15 1 0.2075 -0.0376 0.1660 11.00000 0.05 0.67 Q16 1 -0.4231 -0.2602 0.4261 11.00000 0.05 0.59 Q17 1 0.1222 -0.0354 0.1634 11.00000 0.05 0.49 Q18 1 0.1423 0.0243 0.3835 11.00000 0.05 0.43 Q19 1 -0.0256 0.3564 0.5359 11.00000 0.05 0.42 Q20 1 -0.0376 0.4973 0.5384 11.00000 0.05 0.40 ; _shelx_res_checksum 28480 _shelx_hkl_file ; _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_correction_T_min 0.5988 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.54184 14.487 18.096 25.567 90.020 90.016 90.005 ) ; _shelx_hkl_checksum 97385