data_shelx _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H32 N10 Ni O10 W Y' _chemical_formula_weight 988.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Y' 'Y' -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.9506(5) _cell_length_b 13.9237(6) _cell_length_c 27.4023(15) _cell_angle_alpha 90 _cell_angle_beta 93.252(4) _cell_angle_gamma 90 _cell_volume 3409.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 57563 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 32.63 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.925 _exptl_crystal_F_000 1940 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_absorpt_coefficient_mu 5.669 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1450 _exptl_absorpt_correction_T_max 0.3411 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31808 _diffrn_reflns_av_unetI/netI 0.0641 _diffrn_reflns_av_R_equivalents 0.0932 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.670 _diffrn_reflns_theta_max 27.999 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 8193 _reflns_number_gt 6327 _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 'X-Area' _computing_cell_refinement 'X-Area' _computing_data_reduction 'X-Area' _computing_structure_solution 'SHELXS-2014 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0482P)^2^+20.7845P] 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 SHELXL _refine_ls_extinction_coef 0.00070(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8193 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _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 C1 C 0.6513(14) 0.3353(11) 0.0222(4) 0.075(4) Uani 1 1 d . . . . . H1A H 0.6016 0.2886 0.0012 0.112 Uiso 1 1 calc R U . . . H1B H 0.6652 0.3935 0.0043 0.112 Uiso 1 1 calc R U . . . H1C H 0.7469 0.3107 0.0340 0.112 Uiso 1 1 calc R U . . . O9 O 0.2993(7) 0.2636(4) 0.2275(2) 0.0416(13) Uani 1 1 d . . . . . C2 C 0.6192(10) 0.4219(7) 0.0971(3) 0.0410(18) Uani 1 1 d . . . . . C3 C 0.7435(12) 0.4792(8) 0.0904(4) 0.056(3) Uani 1 1 d . . . . . H3 H 0.7939 0.4755 0.0618 0.067 Uiso 1 1 calc R U . . . C4 C 0.7900(12) 0.5412(9) 0.1269(4) 0.063(3) Uani 1 1 d . . . . . H4 H 0.8723 0.5805 0.1227 0.075 Uiso 1 1 calc R U . . . C5 C 0.7171(12) 0.5464(8) 0.1696(4) 0.060(3) Uani 1 1 d . . . . . H5 H 0.7527 0.5875 0.1944 0.072 Uiso 1 1 calc R U . . . C6 C 0.5901(11) 0.4908(6) 0.1762(3) 0.0437(19) Uani 1 1 d . . . . . C7 C 0.5398(9) 0.4257(6) 0.1394(3) 0.0375(17) Uani 1 1 d . . . . . C8 C 0.5170(12) 0.5032(7) 0.2222(3) 0.049(2) Uani 1 1 d . . . . . H8 H 0.5704 0.5382 0.2463 0.059 Uiso 1 1 calc R U . . . C9 C 0.3383(14) 0.5056(9) 0.2810(4) 0.066(3) Uani 1 1 d . . . . . H9A H 0.4159 0.4914 0.3062 0.079 Uiso 1 1 calc R U . . . H9B H 0.3268 0.5748 0.2797 0.079 Uiso 1 1 calc R U . . . C10 C 0.1992(17) 0.4641(10) 0.2956(4) 0.079(4) Uani 1 1 d . . . . . H10A H 0.1778 0.4907 0.3272 0.095 Uiso 1 1 calc R U . . . H10B H 0.2142 0.3956 0.3000 0.095 Uiso 1 1 calc R U . . . C11 C 0.0629(15) 0.4786(9) 0.2613(4) 0.067(3) Uani 1 1 d . . . . . H11A H -0.0263 0.4688 0.2792 0.080 Uiso 1 1 calc R U . . . H11B H 0.0616 0.5443 0.2496 0.080 Uiso 1 1 calc R U . . . C12 C -0.0583(11) 0.3655(7) 0.2093(3) 0.050(2) Uani 1 1 d . . . . . H12 H -0.1383 0.3766 0.2288 0.060 Uiso 1 1 calc R U . . . C13 C -0.0822(10) 0.2951(7) 0.1704(3) 0.0430(19) Uani 1 1 d . . . . . C14 C -0.2203(10) 0.2473(8) 0.1678(3) 0.050(2) Uani 1 1 d . . . . . H14 H -0.2907 0.2625 0.1903 0.060 Uiso 1 1 calc R U . . . C15 C -0.2543(12) 0.1786(9) 0.1331(4) 0.062(3) Uani 1 1 d . . . . . H15 H -0.3466 0.1478 0.1325 0.075 Uiso 1 1 calc R U . . . C16 C -0.1518(11) 0.1546(8) 0.0988(4) 0.054(2) Uani 1 1 d . . . . . H16 H -0.1744 0.1084 0.0750 0.065 Uiso 1 1 calc R U . . . C17 C -0.0152(10) 0.2015(7) 0.1010(3) 0.045(2) Uani 1 1 d . . . . . C18 C 0.0215(9) 0.2730(6) 0.1360(3) 0.0387(18) Uani 1 1 d . . . . . C19 C 0.0833(15) 0.0967(8) 0.0409(4) 0.069(3) Uani 1 1 d . . . . . H19A H 0.1657 0.0915 0.0201 0.104 Uiso 1 1 calc R U . . . H19B H 0.0837 0.0426 0.0627 0.104 Uiso 1 1 calc R U . . . H19C H -0.0090 0.0977 0.0213 0.104 Uiso 1 1 calc R U . . . C20 C 0.2043(9) 0.6086(6) 0.1383(3) 0.0376(17) Uani 1 1 d . . . . . C21 C 0.0779(10) 0.6757(7) 0.0618(3) 0.0437(19) Uani 1 1 d . . . . . C27 C 0.3348(10) 0.7501(7) 0.1865(3) 0.0423(19) Uani 1 1 d . . . . . C22 C 0.0311(9) 0.7388(6) 0.1772(3) 0.0369(16) Uani 1 1 d . . . . . N10 N 0.4170(10) 0.7475(7) 0.2192(3) 0.057(2) Uani 1 1 d . . . . . C23 C -0.0152(11) 0.8373(7) 0.0998(3) 0.046(2) Uani 1 1 d . . . . . C24 C 0.2342(12) 0.9028(6) 0.1477(3) 0.047(2) Uani 1 1 d . . . . . C25 C 0.2342(12) 0.8435(6) 0.0564(3) 0.044(2) Uani 1 1 d . . . . . C26 C 0.4067(10) 0.7223(8) 0.0966(3) 0.051(2) Uani 1 1 d . . . . . N1 N 0.3898(9) 0.4723(5) 0.2334(2) 0.0433(17) Uani 1 1 d . . . . . N2 N 0.0596(8) 0.4133(6) 0.2196(2) 0.0417(16) Uani 1 1 d . . . . . N3 N 0.2159(9) 0.5293(5) 0.1475(3) 0.0453(18) Uani 1 1 d . . . . . N4 N 0.0186(10) 0.6335(7) 0.0314(3) 0.054(2) Uani 1 1 d . . . . . N5 N -0.0541(9) 0.7280(6) 0.2070(3) 0.0492(18) Uani 1 1 d . . . . . N6 N -0.1229(11) 0.8776(7) 0.0871(3) 0.065(2) Uani 1 1 d . . . . . N7 N 0.2645(14) 0.9791(6) 0.1584(4) 0.073(3) Uani 1 1 d . . . . . N8 N 0.2621(12) 0.8872(7) 0.0233(3) 0.065(3) Uani 1 1 d . . . . . N9 N 0.5207(11) 0.7109(9) 0.0824(3) 0.078(3) Uani 1 1 d . . . . . Ni1 Ni 0.25241(12) 0.39916(8) 0.18551(4) 0.0357(2) Uani 1 1 d . . . . . O1 O 0.5604(7) 0.3550(5) 0.0635(2) 0.0477(15) Uani 1 1 d . . . . . O2 O 0.4235(7) 0.3679(4) 0.1419(2) 0.0397(13) Uani 1 1 d . . . . . O3 O 0.1533(6) 0.3156(4) 0.1331(2) 0.0378(12) Uani 1 1 d . . . . . O4 O 0.0974(7) 0.1845(5) 0.0691(2) 0.0470(15) Uani 1 1 d . . . . . O5 O 0.2114(9) 0.4208(5) 0.0488(2) 0.0596(19) Uani 1 1 d . . . . . O6 O 0.2886(7) 0.2709(5) -0.0078(2) 0.0523(16) Uani 1 1 d . . . . . O7 O 0.4548(9) 0.1382(5) 0.0487(3) 0.063(2) Uani 1 1 d . . . . . O8 O 0.3660(7) 0.1637(4) 0.1444(2) 0.0428(14) Uani 1 1 d . . . . . O10 O 0.5880(13) 0.9621(10) 0.0700(8) 0.200(9) Uani 1 1 d . . . . . W1 W 0.18773(4) 0.75975(2) 0.12089(2) 0.03246(11) Uani 1 1 d . . . . . Y1 Y 0.32800(9) 0.27482(6) 0.08002(3) 0.03573(18) Uani 1 1 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 C1 0.061(7) 0.109(10) 0.057(6) -0.021(7) 0.025(5) -0.004(7) O9 0.048(3) 0.042(3) 0.035(3) 0.002(2) 0.000(2) 0.002(3) C2 0.039(5) 0.044(5) 0.040(4) -0.004(4) 0.000(3) -0.002(4) C3 0.047(6) 0.067(7) 0.055(5) 0.001(5) 0.012(4) -0.011(5) C4 0.043(6) 0.069(7) 0.076(7) 0.000(6) 0.003(5) -0.021(5) C5 0.048(6) 0.063(7) 0.068(7) -0.011(5) -0.008(5) -0.012(5) C6 0.045(5) 0.040(5) 0.045(5) -0.001(4) -0.006(4) -0.005(4) C7 0.036(4) 0.038(4) 0.038(4) 0.001(3) 0.001(3) -0.003(3) C8 0.055(6) 0.049(5) 0.042(5) -0.008(4) -0.006(4) -0.006(4) C9 0.082(8) 0.072(7) 0.043(5) -0.017(5) 0.011(5) -0.022(6) C10 0.113(11) 0.077(8) 0.050(6) -0.018(6) 0.017(7) -0.022(8) C11 0.084(9) 0.062(7) 0.056(6) -0.014(5) 0.015(6) 0.005(6) C12 0.050(6) 0.057(6) 0.044(5) 0.008(4) 0.011(4) 0.017(5) C13 0.042(5) 0.051(5) 0.036(4) 0.006(4) 0.004(3) -0.001(4) C14 0.034(4) 0.066(6) 0.050(5) 0.010(5) 0.005(4) 0.005(4) C15 0.044(5) 0.084(8) 0.058(6) 0.019(6) -0.007(5) -0.021(5) C16 0.050(6) 0.061(6) 0.049(5) 0.000(5) -0.009(4) -0.018(5) C17 0.043(5) 0.051(5) 0.041(4) 0.001(4) -0.005(4) -0.004(4) C18 0.037(4) 0.044(5) 0.035(4) 0.012(3) -0.001(3) 0.000(3) C19 0.083(8) 0.059(7) 0.065(7) -0.027(6) 0.001(6) -0.014(6) C20 0.035(4) 0.038(4) 0.040(4) -0.003(3) 0.001(3) -0.006(3) C21 0.042(5) 0.048(5) 0.039(4) -0.005(4) -0.006(4) 0.000(4) C27 0.041(4) 0.053(5) 0.031(4) -0.002(4) -0.010(3) 0.002(4) C22 0.037(4) 0.041(4) 0.034(4) 0.001(3) 0.013(3) -0.004(3) N10 0.056(5) 0.066(6) 0.049(4) -0.006(4) -0.003(4) 0.003(4) C23 0.047(5) 0.047(5) 0.043(5) 0.001(4) -0.001(4) 0.005(4) C24 0.071(7) 0.032(4) 0.038(4) 0.002(3) 0.001(4) -0.008(4) C25 0.064(6) 0.034(4) 0.036(4) 0.006(3) 0.009(4) -0.004(4) C26 0.033(4) 0.080(7) 0.043(5) 0.010(5) 0.009(3) 0.002(4) N1 0.051(5) 0.045(4) 0.034(3) -0.006(3) 0.000(3) -0.003(3) N2 0.042(4) 0.046(4) 0.038(4) 0.004(3) 0.007(3) 0.006(3) N3 0.059(5) 0.039(4) 0.038(4) -0.001(3) 0.004(3) 0.005(3) N4 0.056(5) 0.062(5) 0.043(4) -0.003(4) -0.006(4) -0.001(4) N5 0.054(5) 0.046(4) 0.048(4) -0.003(3) 0.008(3) -0.001(4) N6 0.062(6) 0.072(6) 0.062(5) 0.005(5) 0.004(4) 0.013(5) N7 0.108(9) 0.037(5) 0.074(6) -0.011(4) 0.011(6) -0.007(5) N8 0.086(7) 0.065(6) 0.045(4) 0.010(4) 0.009(4) -0.010(5) N9 0.052(5) 0.124(10) 0.058(5) 0.020(6) 0.013(4) 0.018(6) Ni1 0.0395(6) 0.0349(5) 0.0329(5) -0.0016(4) 0.0022(4) -0.0003(4) O1 0.039(3) 0.062(4) 0.043(3) -0.007(3) 0.013(3) -0.004(3) O2 0.039(3) 0.045(3) 0.035(3) -0.005(2) 0.003(2) -0.004(3) O3 0.031(3) 0.045(3) 0.038(3) -0.006(2) 0.004(2) 0.000(2) O4 0.052(4) 0.048(4) 0.040(3) -0.008(3) 0.002(3) -0.012(3) O5 0.078(5) 0.052(4) 0.048(4) 0.006(3) 0.002(3) 0.013(4) O6 0.048(4) 0.074(5) 0.035(3) -0.004(3) 0.002(3) 0.000(3) O7 0.081(5) 0.056(4) 0.052(4) -0.004(3) 0.012(4) 0.018(4) O8 0.051(4) 0.038(3) 0.039(3) 0.001(2) -0.001(3) 0.000(3) O10 0.066(8) 0.091(9) 0.43(3) 0.087(13) -0.044(12) -0.009(7) W1 0.03442(17) 0.03293(17) 0.02986(16) 0.00010(12) 0.00032(10) -0.00096(13) Y1 0.0370(4) 0.0383(4) 0.0318(3) -0.0022(3) 0.0009(3) -0.0017(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 C1 O1 1.456(11) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? O9 Ni1 2.238(6) . ? C2 C3 1.390(13) . ? C2 O1 1.392(10) . ? C2 C7 1.393(12) . ? C3 C4 1.367(15) . ? C3 H3 0.9300 . ? C4 C5 1.375(15) . ? C4 H4 0.9300 . ? C5 C6 1.395(13) . ? C5 H5 0.9300 . ? C6 C7 1.411(12) . ? C6 C8 1.463(13) . ? C7 O2 1.320(10) . ? C8 N1 1.271(12) . ? C8 H8 0.9300 . ? C9 C10 1.449(17) . ? C9 N1 1.482(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.509(18) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.460(12) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.266(12) . ? C12 C13 1.455(13) . ? C12 H12 0.9300 . ? C13 C18 1.395(12) . ? C13 C14 1.402(13) . ? C14 C15 1.370(15) . ? C14 H14 0.9300 . ? C15 C16 1.392(16) . ? C15 H15 0.9300 . ? C16 C17 1.385(13) . ? C16 H16 0.9300 . ? C17 O4 1.393(11) . ? C17 C18 1.407(13) . ? C18 O3 1.327(10) . ? C19 O4 1.448(11) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N3 1.137(11) . ? C20 W1 2.160(9) . ? C21 N4 1.128(11) . ? C21 W1 2.185(9) . ? C27 N10 1.127(11) . ? C27 W1 2.171(7) . ? C22 N5 1.157(11) . ? C22 W1 2.164(7) . ? C23 N6 1.152(13) . ? C23 W1 2.163(10) . ? C24 N7 1.131(12) . ? C24 W1 2.156(9) . ? C25 N8 1.132(11) . ? C25 W1 2.178(8) . ? C26 N9 1.123(12) . ? C26 W1 2.169(9) . ? N1 Ni1 2.023(7) . ? N2 Ni1 2.018(7) . ? N3 Ni1 2.106(8) . ? Ni1 O3 2.014(6) . ? Ni1 O2 2.043(6) . ? Ni1 Y1 3.4690(13) . ? O1 Y1 2.426(6) . ? O2 Y1 2.263(6) . ? O3 Y1 2.269(5) . ? O4 Y1 2.421(6) . ? O5 Y1 2.419(7) . ? O6 Y1 2.412(6) . ? O7 Y1 2.398(7) . ? O8 Y1 2.357(6) . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 124.9(8) . . ? C3 C2 C7 122.5(8) . . ? O1 C2 C7 112.6(8) . . ? C4 C3 C2 118.7(9) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 121.0(10) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 120.7(10) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C7 119.6(9) . . ? C5 C6 C8 116.9(9) . . ? C7 C6 C8 123.5(8) . . ? O2 C7 C2 117.4(7) . . ? O2 C7 C6 125.1(8) . . ? C2 C7 C6 117.5(8) . . ? N1 C8 C6 128.2(9) . . ? N1 C8 H8 115.9 . . ? C6 C8 H8 115.9 . . ? C10 C9 N1 115.6(9) . . ? C10 C9 H9A 108.4 . . ? N1 C9 H9A 108.4 . . ? C10 C9 H9B 108.4 . . ? N1 C9 H9B 108.4 . . ? H9A C9 H9B 107.4 . . ? C9 C10 C11 116.9(11) . . ? C9 C10 H10A 108.1 . . ? C11 C10 H10A 108.1 . . ? C9 C10 H10B 108.1 . . ? C11 C10 H10B 108.1 . . ? H10A C10 H10B 107.3 . . ? N2 C11 C10 112.6(10) . . ? N2 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? N2 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? N2 C12 C13 127.1(9) . . ? N2 C12 H12 116.4 . . ? C13 C12 H12 116.4 . . ? C18 C13 C14 118.7(9) . . ? C18 C13 C12 124.6(9) . . ? C14 C13 C12 116.7(8) . . ? C15 C14 C13 121.8(9) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C16 120.6(9) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 118.1(10) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C16 C17 O4 124.1(9) . . ? C16 C17 C18 122.4(9) . . ? O4 C17 C18 113.5(8) . . ? O3 C18 C13 124.7(8) . . ? O3 C18 C17 116.8(8) . . ? C13 C18 C17 118.5(8) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 W1 178.7(8) . . ? N4 C21 W1 178.5(9) . . ? N10 C27 W1 176.3(9) . . ? N5 C22 W1 179.1(8) . . ? N6 C23 W1 177.8(9) . . ? N7 C24 W1 174.4(9) . . ? N8 C25 W1 178.3(10) . . ? N9 C26 W1 173.8(11) . . ? C8 N1 C9 115.7(8) . . ? C8 N1 Ni1 122.2(6) . . ? C9 N1 Ni1 121.4(7) . . ? C12 N2 C11 118.8(8) . . ? C12 N2 Ni1 124.7(6) . . ? C11 N2 Ni1 116.3(7) . . ? C20 N3 Ni1 163.0(7) . . ? O3 Ni1 N2 91.9(3) . . ? O3 Ni1 N1 168.7(3) . . ? N2 Ni1 N1 98.9(3) . . ? O3 Ni1 O2 77.0(2) . . ? N2 Ni1 O2 168.8(3) . . ? N1 Ni1 O2 92.2(3) . . ? O3 Ni1 N3 95.4(3) . . ? N2 Ni1 N3 91.8(3) . . ? N1 Ni1 N3 87.7(3) . . ? O2 Ni1 N3 89.7(3) . . ? O3 Ni1 O9 86.7(2) . . ? N2 Ni1 O9 89.1(3) . . ? N1 Ni1 O9 90.1(3) . . ? O2 Ni1 O9 89.8(2) . . ? N3 Ni1 O9 177.7(3) . . ? O3 Ni1 Y1 38.44(16) . . ? N2 Ni1 Y1 130.3(2) . . ? N1 Ni1 Y1 130.7(2) . . ? O2 Ni1 Y1 38.54(16) . . ? N3 Ni1 Y1 92.8(2) . . ? O9 Ni1 Y1 88.18(15) . . ? C2 O1 C1 115.7(8) . . ? C2 O1 Y1 118.7(5) . . ? C1 O1 Y1 125.5(7) . . ? C7 O2 Ni1 121.3(5) . . ? C7 O2 Y1 125.1(5) . . ? Ni1 O2 Y1 107.2(3) . . ? C18 O3 Ni1 125.0(5) . . ? C18 O3 Y1 125.0(5) . . ? Ni1 O3 Y1 108.1(2) . . ? C17 O4 C19 115.7(8) . . ? C17 O4 Y1 118.4(5) . . ? C19 O4 Y1 123.6(6) . . ? C24 W1 C20 144.7(3) . . ? C24 W1 C23 76.8(4) . . ? C20 W1 C23 126.2(3) . . ? C24 W1 C22 90.1(3) . . ? C20 W1 C22 75.5(3) . . ? C23 W1 C22 71.9(3) . . ? C24 W1 C26 99.6(4) . . ? C20 W1 C26 77.4(4) . . ? C23 W1 C26 142.9(4) . . ? C22 W1 C26 145.1(3) . . ? C24 W1 C27 71.3(4) . . ? C20 W1 C27 74.1(3) . . ? C23 W1 C27 135.4(3) . . ? C22 W1 C27 77.7(3) . . ? C26 W1 C27 73.9(3) . . ? C24 W1 C25 74.9(3) . . ? C20 W1 C25 133.4(3) . . ? C23 W1 C25 73.3(4) . . ? C22 W1 C25 144.4(3) . . ? C26 W1 C25 70.3(4) . . ? C27 W1 C25 124.8(4) . . ? C24 W1 C21 144.8(3) . . ? C20 W1 C21 70.3(3) . . ? C23 W1 C21 74.6(4) . . ? C22 W1 C21 100.0(3) . . ? C26 W1 C21 91.2(4) . . ? C27 W1 C21 143.7(4) . . ? C25 W1 C21 77.6(3) . . ? O2 Y1 O3 67.7(2) . . ? O2 Y1 O8 77.4(2) . . ? O3 Y1 O8 76.1(2) . . ? O2 Y1 O7 123.8(3) . . ? O3 Y1 O7 141.8(2) . . ? O8 Y1 O7 72.3(2) . . ? O2 Y1 O6 142.0(2) . . ? O3 Y1 O6 125.4(2) . . ? O8 Y1 O6 137.6(2) . . ? O7 Y1 O6 70.8(2) . . ? O2 Y1 O5 85.5(2) . . ? O3 Y1 O5 73.6(2) . . ? O8 Y1 O5 149.0(2) . . ? O7 Y1 O5 138.0(2) . . ? O6 Y1 O5 68.3(2) . . ? O2 Y1 O4 132.3(2) . . ? O3 Y1 O4 66.2(2) . . ? O8 Y1 O4 80.7(2) . . ? O7 Y1 O4 87.8(3) . . ? O6 Y1 O4 77.8(2) . . ? O5 Y1 O4 92.6(3) . . ? O2 Y1 O1 65.5(2) . . ? O3 Y1 O1 129.3(2) . . ? O8 Y1 O1 110.7(2) . . ? O7 Y1 O1 82.5(3) . . ? O6 Y1 O1 84.4(2) . . ? O5 Y1 O1 84.5(3) . . ? O4 Y1 O1 161.8(2) . . ? O2 Y1 Ni1 34.22(15) . . ? O3 Y1 Ni1 33.49(14) . . ? O8 Y1 Ni1 74.36(15) . . ? O7 Y1 Ni1 144.33(17) . . ? O6 Y1 Ni1 144.89(18) . . ? O5 Y1 Ni1 77.00(16) . . ? O4 Y1 Ni1 99.05(15) . . ? O1 Y1 Ni1 97.80(15) . . ? _refine_diff_density_max 2.373 _refine_diff_density_min -2.289 _refine_diff_density_rms 0.162 _shelxl_version_number 2014-3 _shelx_res_file ; TITL tr12 in P 21/c CELL 0.71073 8.9506 13.9237 27.4023 90.000 93.252 90.000 ZERR 4.00 0.0005 0.0006 0.0015 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N NI O W Y UNIT 108 128 40 4 40 4 4 MERG 2 OMIT -3.00 56.00 OMIT -4 3 1 OMIT 3 5 1 OMIT 1 0 0 OMIT 1 0 2 OMIT -10 1 1 OMIT -4 4 9 OMIT -3 5 3 OMIT -1 0 2 FMAP 2 PLAN 20 ACTA BOND $H L.S. 8 WGHT 0.048200 20.784500 EXTI 0.000704 FVAR 0.44532 C1 1 0.651274 0.335282 0.022211 11.00000 0.06061 0.10878 = 0.05739 -0.02056 0.02534 -0.00425 AFIX 33 H1A 2 0.601635 0.288624 0.001210 11.00000 -1.50000 H1B 2 0.665212 0.393496 0.004255 11.00000 -1.50000 H1C 2 0.746881 0.310720 0.033957 11.00000 -1.50000 AFIX 0 O9 5 0.299280 0.263598 0.227548 11.00000 0.04755 0.04161 = 0.03524 0.00249 -0.00042 0.00167 C2 1 0.619181 0.421861 0.097147 11.00000 0.03934 0.04374 = 0.03983 -0.00422 0.00020 -0.00178 C3 1 0.743479 0.479231 0.090446 11.00000 0.04707 0.06676 = 0.05523 0.00137 0.01235 -0.01124 AFIX 43 H3 2 0.793940 0.475488 0.061760 11.00000 -1.20000 AFIX 0 C4 1 0.790018 0.541241 0.126864 11.00000 0.04291 0.06856 = 0.07639 -0.00032 0.00271 -0.02107 AFIX 43 H4 2 0.872312 0.580544 0.122663 11.00000 -1.20000 AFIX 0 C5 1 0.717070 0.546439 0.169632 11.00000 0.04776 0.06260 = 0.06751 -0.01063 -0.00846 -0.01244 AFIX 43 H5 2 0.752714 0.587473 0.194417 11.00000 -1.20000 AFIX 0 C6 1 0.590135 0.490784 0.176220 11.00000 0.04486 0.04024 = 0.04490 -0.00086 -0.00583 -0.00466 C7 1 0.539758 0.425712 0.139372 11.00000 0.03644 0.03794 = 0.03781 0.00093 0.00061 -0.00322 C8 1 0.517021 0.503226 0.222231 11.00000 0.05482 0.04899 = 0.04209 -0.00836 -0.00560 -0.00611 AFIX 43 H8 2 0.570359 0.538203 0.246316 11.00000 -1.20000 AFIX 0 C9 1 0.338312 0.505569 0.281045 11.00000 0.08190 0.07247 = 0.04319 -0.01661 0.01109 -0.02184 AFIX 23 H9A 2 0.415855 0.491351 0.306175 11.00000 -1.20000 H9B 2 0.326827 0.574808 0.279706 11.00000 -1.20000 AFIX 0 C10 1 0.199174 0.464147 0.295583 11.00000 0.11320 0.07671 = 0.04994 -0.01802 0.01676 -0.02221 AFIX 23 H10A 2 0.177761 0.490687 0.327162 11.00000 -1.20000 H10B 2 0.214233 0.395633 0.299976 11.00000 -1.20000 AFIX 0 C11 1 0.062939 0.478615 0.261349 11.00000 0.08355 0.06167 = 0.05629 -0.01352 0.01538 0.00493 AFIX 23 H11A 2 -0.026311 0.468801 0.279216 11.00000 -1.20000 H11B 2 0.061632 0.544314 0.249559 11.00000 -1.20000 AFIX 0 C12 1 -0.058257 0.365504 0.209326 11.00000 0.05043 0.05678 = 0.04395 0.00823 0.01109 0.01690 AFIX 43 H12 2 -0.138335 0.376561 0.228778 11.00000 -1.20000 AFIX 0 C13 1 -0.082216 0.295119 0.170405 11.00000 0.04220 0.05099 = 0.03614 0.00597 0.00418 -0.00085 C14 1 -0.220290 0.247251 0.167845 11.00000 0.03401 0.06646 = 0.05017 0.01049 0.00501 0.00539 AFIX 43 H14 2 -0.290681 0.262490 0.190310 11.00000 -1.20000 AFIX 0 C15 1 -0.254264 0.178622 0.133128 11.00000 0.04395 0.08409 = 0.05777 0.01871 -0.00707 -0.02062 AFIX 43 H15 2 -0.346566 0.147844 0.132515 11.00000 -1.20000 AFIX 0 C16 1 -0.151795 0.154592 0.098778 11.00000 0.05021 0.06107 = 0.04932 0.00043 -0.00915 -0.01791 AFIX 43 H16 2 -0.174419 0.108362 0.075001 11.00000 -1.20000 AFIX 0 C17 1 -0.015191 0.201520 0.101036 11.00000 0.04256 0.05150 = 0.04053 0.00119 -0.00522 -0.00376 C18 1 0.021500 0.273012 0.135982 11.00000 0.03717 0.04372 = 0.03491 0.01203 -0.00119 0.00025 C19 1 0.083258 0.096671 0.040909 11.00000 0.08291 0.05945 = 0.06542 -0.02735 0.00054 -0.01428 AFIX 33 H19A 2 0.165651 0.091455 0.020112 11.00000 -1.50000 H19B 2 0.083723 0.042649 0.062685 11.00000 -1.50000 H19C 2 -0.008995 0.097671 0.021255 11.00000 -1.50000 AFIX 0 C20 1 0.204292 0.608645 0.138256 11.00000 0.03484 0.03814 = 0.03975 -0.00280 0.00064 -0.00594 C21 1 0.077873 0.675654 0.061831 11.00000 0.04230 0.04840 = 0.03950 -0.00478 -0.00638 0.00026 C27 1 0.334811 0.750144 0.186496 11.00000 0.04129 0.05289 = 0.03120 -0.00229 -0.01002 0.00248 C22 1 0.031093 0.738769 0.177248 11.00000 0.03673 0.04107 = 0.03414 0.00144 0.01335 -0.00390 N10 3 0.416970 0.747522 0.219201 11.00000 0.05558 0.06629 = 0.04878 -0.00642 -0.00337 0.00316 C23 1 -0.015202 0.837337 0.099836 11.00000 0.04711 0.04707 = 0.04279 0.00082 -0.00094 0.00539 C24 1 0.234175 0.902843 0.147668 11.00000 0.07084 0.03216 = 0.03833 0.00182 0.00139 -0.00839 C25 1 0.234240 0.843535 0.056379 11.00000 0.06379 0.03426 = 0.03589 0.00579 0.00876 -0.00442 C26 1 0.406739 0.722269 0.096599 11.00000 0.03269 0.07976 = 0.04258 0.00960 0.00868 0.00217 N1 3 0.389811 0.472270 0.233445 11.00000 0.05071 0.04472 = 0.03419 -0.00596 -0.00018 -0.00313 N2 3 0.059617 0.413316 0.219603 11.00000 0.04165 0.04647 = 0.03759 0.00394 0.00696 0.00634 N3 3 0.215891 0.529318 0.147526 11.00000 0.05850 0.03950 = 0.03809 -0.00111 0.00442 0.00493 N4 3 0.018576 0.633480 0.031395 11.00000 0.05642 0.06221 = 0.04290 -0.00264 -0.00570 -0.00055 N5 3 -0.054146 0.728040 0.206971 11.00000 0.05388 0.04584 = 0.04844 -0.00250 0.00790 -0.00120 N6 3 -0.122945 0.877642 0.087133 11.00000 0.06176 0.07207 = 0.06215 0.00545 0.00364 0.01285 N7 3 0.264513 0.979119 0.158351 11.00000 0.10806 0.03729 = 0.07373 -0.01138 0.01096 -0.00691 N8 3 0.262116 0.887225 0.023266 11.00000 0.08645 0.06495 = 0.04513 0.00989 0.00891 -0.00976 N9 3 0.520659 0.710888 0.082396 11.00000 0.05186 0.12397 = 0.05833 0.01989 0.01280 0.01825 NI1 4 0.252409 0.399162 0.185512 11.00000 0.03946 0.03487 = 0.03289 -0.00160 0.00220 -0.00033 O1 5 0.560385 0.355014 0.063492 11.00000 0.03941 0.06192 = 0.04307 -0.00681 0.01285 -0.00365 O2 5 0.423542 0.367887 0.141897 11.00000 0.03881 0.04508 = 0.03542 -0.00506 0.00308 -0.00447 O3 5 0.153280 0.315643 0.133142 11.00000 0.03055 0.04493 = 0.03814 -0.00646 0.00428 -0.00006 O4 5 0.097429 0.184518 0.069077 11.00000 0.05244 0.04848 = 0.04012 -0.00830 0.00220 -0.01228 O5 5 0.211355 0.420803 0.048759 11.00000 0.07829 0.05217 = 0.04811 0.00646 0.00167 0.01306 O6 5 0.288630 0.270907 -0.007788 11.00000 0.04776 0.07379 = 0.03538 -0.00366 0.00203 0.00049 O7 5 0.454821 0.138205 0.048722 11.00000 0.08083 0.05573 = 0.05193 -0.00355 0.01195 0.01818 O8 5 0.366009 0.163684 0.144430 11.00000 0.05123 0.03769 = 0.03899 0.00068 -0.00058 0.00014 O10 5 0.587958 0.962111 0.070035 11.00000 0.06598 0.09144 = 0.43498 0.08681 -0.04379 -0.00938 W1 6 0.187728 0.759752 0.120886 11.00000 0.03442 0.03293 = 0.02986 0.00010 0.00032 -0.00096 Y1 7 0.327996 0.274821 0.080016 11.00000 0.03701 0.03828 = 0.03177 -0.00218 0.00085 -0.00173 HKLF 4 REM tr12 in P 21/c REM R1 = 0.0597 for 6327 Fo > 4sig(Fo) and 0.0840 for all 8193 data REM 452 parameters refined using 0 restraints END WGHT 0.0481 20.7870 REM Highest difference peak 2.373, deepest hole -2.289, 1-sigma level 0.162 Q1 1 0.1996 0.7614 0.1602 11.00000 0.05 2.37 Q2 1 0.2941 0.7610 0.1308 11.00000 0.05 2.25 Q3 1 0.1688 0.7623 0.0840 11.00000 0.05 2.16 Q4 1 0.0817 0.7614 0.1112 11.00000 0.05 2.01 Q5 1 0.1958 0.6981 0.1251 11.00000 0.05 1.83 Q6 1 0.3073 0.2788 0.0419 11.00000 0.05 1.07 Q7 1 0.1919 0.8180 0.1218 11.00000 0.05 1.07 Q8 1 0.3341 0.1994 0.0859 11.00000 0.05 0.95 Q9 1 0.2778 0.4009 0.2270 11.00000 0.05 0.86 Q10 1 0.6411 0.9761 0.0379 11.00000 0.05 0.84 Q11 1 0.1504 0.4030 0.1782 11.00000 0.05 0.83 Q12 1 0.3369 0.2786 0.1184 11.00000 0.05 0.83 Q13 1 0.2437 0.8463 0.1265 11.00000 0.05 0.78 Q14 1 0.2322 0.4016 0.1453 11.00000 0.05 0.77 Q15 1 0.4313 0.2772 0.0883 11.00000 0.05 0.75 Q16 1 0.3263 0.7092 0.1102 11.00000 0.05 0.74 Q17 1 0.2823 0.7241 0.1624 11.00000 0.05 0.72 Q18 1 0.2211 0.2781 0.0709 11.00000 0.05 0.70 Q19 1 0.3576 0.4008 0.1925 11.00000 0.05 0.68 Q20 1 0.0985 0.7197 0.1590 11.00000 0.05 0.67 ; _shelx_res_checksum 53008 _shelx_hkl_file ; -13 0 1 -22.51 61.86 13 0 -1 8.01 60.37 -13 0 2 216.64 69.01 13 0 -2 115.85 59.08 -13 0 3 23.28 60.04 13 0 -3 -13.23 59.00 13 0 -4 64.46 55.70 -13 0 4 13.99 59.19 -13 0 5 -6.27 60.53 13 0 -5 -28.10 58.05 13 0 -6 -53.24 57.69 -13 0 6 7.02 60.78 -13 0 7 -26.64 58.43 13 0 -7 47.47 54.17 -13 0 8 137.65 51.72 13 0 -8 91.48 55.82 -13 0 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