data_g140929c _audit_creation_date 2014-10-06 _audit_creation_method ; Olex2 1.2 (compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874) ; _shelxl_version_number 2014/6 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C28 H36 N2 O10 Pd3' _chemical_formula_sum 'C28 H36 N2 O10 Pd3' _chemical_formula_weight 879.79 _chemical_melting_point ? _chemical_oxdiff_formula CHONPd 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.2684(4) _cell_length_b 13.1049(5) _cell_length_c 14.9823(6) _cell_angle_alpha 90 _cell_angle_beta 98.209(4) _cell_angle_gamma 90 _cell_volume 1606.80(12) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4674 _cell_measurement_temperature 223.00(10) _cell_measurement_theta_max 29.9510 _cell_measurement_theta_min 3.9810 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.716 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.69711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear light yellow' _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 872 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_unetI/netI 0.0311 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 9785 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.994 _diffrn_reflns_theta_min 2.935 _diffrn_ambient_temperature 223.00(10) _diffrn_detector_area_resol_mean 10.4471 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -45.00 26.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 13.8077 -37.0000 120.0000 71 #__ type_ start__ end____ width___ exp.time_ 2 omega -59.00 12.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 13.8077 -57.0000 60.0000 71 #__ type_ start__ end____ width___ exp.time_ 3 omega 44.00 96.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 13.8077 178.0000 -60.0000 52 #__ type_ start__ end____ width___ exp.time_ 4 omega -87.00 -53.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -14.5889 178.0000 -120.0000 34 #__ type_ start__ end____ width___ exp.time_ 5 omega -1.00 27.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -14.5889 -99.0000 -150.0000 28 ; _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0284475000 _diffrn_orient_matrix_UB_12 0.0439155000 _diffrn_orient_matrix_UB_13 0.0251886000 _diffrn_orient_matrix_UB_21 0.0818317000 _diffrn_orient_matrix_UB_22 -0.0165326000 _diffrn_orient_matrix_UB_23 0.0003011000 _diffrn_orient_matrix_UB_31 0.0036750000 _diffrn_orient_matrix_UB_32 0.0270143000 _diffrn_orient_matrix_UB_33 -0.0406152000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3024 _reflns_number_total 3504 _reflns_odcompleteness_completeness 99.84 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 27.42 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.922 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.089 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 3504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0367 _refine_ls_R_factor_gt 0.0288 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+0.2770P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.0733 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, {H14A,H14B,H14C} of C14, All C(H,H) groups At 1.5 times of: {H8A,H8B,H8C} of C8, {H10A,H10B,H10C} of C10, {H12A,H12B,H12C} of C12 2.a Riding coordinates: C14(H14A,H14B,H14C) 2.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B) 2.c Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6) 2.d Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C) ; _atom_sites_solution_hydrogens mixed _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 Pd1 Pd -0.05340(3) 0.20538(2) 0.57298(2) 0.02941(9) Uani 1 1 d . . . . . Pd2 Pd 0.0000 0.0000 0.5000 0.02878(10) Uani 1 2 d S T P . . O1 O 0.1044(3) 0.33644(18) 0.44392(15) 0.0450(6) Uani 1 1 d . . . . . O2 O -0.2249(3) 0.11421(16) 0.61896(14) 0.0383(5) Uani 1 1 d . . . . . O3 O -0.2197(3) -0.02897(17) 0.53786(15) 0.0379(5) Uani 1 1 d . . . . . O4 O 0.1270(3) 0.13819(17) 0.67681(14) 0.0415(5) Uani 1 1 d . . . . . O5 O 0.1052(3) -0.02387(16) 0.62702(13) 0.0355(5) Uani 1 1 d . . . . . N1 N 0.0940(3) 0.3173(2) 0.53578(19) 0.0379(6) Uani 1 1 d . . . . . C1 C -0.2199(4) 0.2521(2) 0.4749(2) 0.0317(7) Uani 1 1 d . . . . . C2 C -0.1674(4) 0.2683(2) 0.3916(2) 0.0357(7) Uani 1 1 d . . . . . C3 C -0.2803(5) 0.2887(3) 0.3161(3) 0.0510(10) Uani 1 1 d . . . . . H3 H -0.2448 0.2996 0.2607 0.061 Uiso 1 1 calc R . . . . C4 C -0.4447(6) 0.2931(3) 0.3227(3) 0.0598(11) Uani 1 1 d . . . . . H4 H -0.5202 0.3040 0.2714 0.072 Uiso 1 1 calc R . . . . C5 C -0.4965(5) 0.2814(3) 0.4043(3) 0.0551(11) Uani 1 1 d . . . . . H5 H -0.6071 0.2876 0.4087 0.066 Uiso 1 1 calc R . . . . C6 C -0.3859(4) 0.2603(3) 0.4816(3) 0.0445(8) Uani 1 1 d . . . . . H6 H -0.4226 0.2518 0.5370 0.053 Uiso 1 1 calc R . . . . C7 C 0.0115(4) 0.2622(3) 0.3858(2) 0.0404(8) Uani 1 1 d . . . . . H7A H 0.0507 0.1942 0.4029 0.049 Uiso 1 1 calc R . . . . H7B H 0.0290 0.2738 0.3240 0.049 Uiso 1 1 calc R . . . . C8 C 0.2778(6) 0.4636(3) 0.5508(3) 0.0675(12) Uani 1 1 d . . . . . H8A H 0.3603 0.4331 0.5204 0.101 Uiso 1 1 calc GR . . . . H8B H 0.3289 0.5050 0.5998 0.101 Uiso 1 1 calc GR . . . . H8C H 0.2078 0.5054 0.5092 0.101 Uiso 1 1 calc GR . . . . C9 C 0.1791(4) 0.3818(3) 0.5867(3) 0.0442(8) Uani 1 1 d . . . . . C10 C 0.1751(6) 0.3775(3) 0.6853(3) 0.0604(11) Uani 1 1 d . . . . . H10A H 0.0891 0.3325 0.6974 0.091 Uiso 1 1 calc GR . . . . H10B H 0.1555 0.4446 0.7071 0.091 Uiso 1 1 calc GR . . . . H10C H 0.2779 0.3526 0.7152 0.091 Uiso 1 1 calc GR . . . . C11 C -0.2815(4) 0.0306(2) 0.59122(19) 0.0323(7) Uani 1 1 d . . . . . C12 C -0.4381(4) -0.0017(3) 0.6215(2) 0.0458(8) Uani 1 1 d . . . . . H12A H -0.5269 0.0365 0.5892 0.069 Uiso 1 1 calc GR . . . . H12B H -0.4328 0.0109 0.6849 0.069 Uiso 1 1 calc GR . . . . H12C H -0.4553 -0.0731 0.6097 0.069 Uiso 1 1 calc GR . . . . C13 C 0.1478(4) 0.0447(2) 0.6858(2) 0.0321(7) Uani 1 1 d . . . . . C14 C 0.2328(5) 0.0036(3) 0.7750(2) 0.0450(8) Uani 1 1 d . . . . . H14A H 0.2205 -0.0692 0.7779 0.054 Uiso 1 1 d R . . . . H14B H 0.1882 0.0350 0.8239 0.054 Uiso 1 1 d R . . . . H14C H 0.3473 0.0201 0.7796 0.054 Uiso 1 1 d R . . . . 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 Pd1 0.03406(15) 0.02613(14) 0.02855(14) -0.00369(9) 0.00614(10) -0.00144(9) Pd2 0.02795(18) 0.02902(18) 0.02756(18) -0.00840(13) -0.00229(13) 0.00375(13) O1 0.0533(15) 0.0428(13) 0.0414(13) -0.0007(11) 0.0148(11) -0.0148(12) O2 0.0463(13) 0.0357(12) 0.0360(12) -0.0043(10) 0.0171(10) -0.0067(10) O3 0.0302(12) 0.0417(12) 0.0404(12) -0.0095(10) 0.0005(10) 0.0000(10) O4 0.0532(15) 0.0356(12) 0.0318(12) -0.0048(10) -0.0065(10) -0.0027(11) O5 0.0398(13) 0.0337(11) 0.0298(11) -0.0042(9) -0.0056(9) 0.0042(9) N1 0.0375(15) 0.0355(14) 0.0417(16) -0.0038(12) 0.0093(12) -0.0042(12) C1 0.0361(17) 0.0220(14) 0.0364(17) -0.0017(13) 0.0034(13) 0.0010(13) C2 0.0483(19) 0.0248(14) 0.0329(17) -0.0001(13) 0.0018(15) -0.0013(14) C3 0.073(3) 0.0342(19) 0.042(2) 0.0039(15) -0.0043(19) 0.0002(18) C4 0.062(3) 0.043(2) 0.066(3) 0.0035(18) -0.019(2) 0.0038(18) C5 0.0319(19) 0.042(2) 0.088(3) 0.002(2) -0.004(2) 0.0023(15) C6 0.040(2) 0.0320(17) 0.062(2) 0.0005(16) 0.0116(17) 0.0040(15) C7 0.052(2) 0.0385(18) 0.0334(18) -0.0009(15) 0.0149(16) -0.0063(16) C8 0.071(3) 0.045(2) 0.090(3) -0.017(2) 0.022(3) -0.026(2) C9 0.043(2) 0.0326(17) 0.057(2) -0.0087(16) 0.0067(17) -0.0045(15) C10 0.077(3) 0.047(2) 0.053(2) -0.0139(18) -0.005(2) -0.011(2) C11 0.0338(17) 0.0346(16) 0.0265(15) 0.0046(13) -0.0021(13) 0.0017(13) C12 0.0382(19) 0.056(2) 0.043(2) 0.0026(16) 0.0066(15) -0.0040(16) C13 0.0285(16) 0.0378(17) 0.0288(16) -0.0044(13) -0.0002(12) -0.0037(13) C14 0.052(2) 0.047(2) 0.0321(18) -0.0011(14) -0.0064(15) -0.0032(16) _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 Pd1 Pd2 2.9618(2) . ? Pd1 O2 2.047(2) . ? Pd1 O4 2.181(2) . ? Pd1 N1 2.035(3) . ? Pd1 C1 1.963(3) . ? Pd2 Pd1 2.9619(2) 3_556 ? Pd2 O3 2.015(2) 3_556 ? Pd2 O3 2.015(2) . ? Pd2 O5 2.001(2) . ? Pd2 O5 2.001(2) 3_556 ? O1 N1 1.413(3) . ? O1 C7 1.450(4) . ? O2 C11 1.239(4) . ? O3 C11 1.275(4) . ? O4 C13 1.242(4) . ? O5 C13 1.273(4) . ? N1 C9 1.279(4) . ? C1 C2 1.395(4) . ? C1 C6 1.395(5) . ? C2 C3 1.385(5) . ? C2 C7 1.496(5) . ? C3 H3 0.9300 . ? C3 C4 1.378(6) . ? C4 H4 0.9300 . ? C4 C5 1.361(6) . ? C5 H5 0.9300 . ? C5 C6 1.397(6) . ? C6 H6 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C8 C9 1.493(5) . ? C9 C10 1.484(5) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.493(5) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.517(4) . ? C14 H14A 0.9599 . ? C14 H14B 0.9586 . ? C14 H14C 0.9639 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Pd1 Pd2 74.98(6) . . ? O2 Pd1 O4 87.73(9) . . ? O4 Pd1 Pd2 76.92(6) . . ? N1 Pd1 Pd2 115.30(7) . . ? N1 Pd1 O2 169.54(9) . . ? N1 Pd1 O4 96.37(10) . . ? C1 Pd1 Pd2 97.60(8) . . ? C1 Pd1 O2 89.34(11) . . ? C1 Pd1 O4 174.30(10) . . ? C1 Pd1 N1 87.35(12) . . ? Pd1 Pd2 Pd1 180.0 . 3_556 ? O3 Pd2 Pd1 96.93(6) 3_556 . ? O3 Pd2 Pd1 83.07(6) 3_556 3_556 ? O3 Pd2 Pd1 83.07(6) . . ? O3 Pd2 Pd1 96.93(6) . 3_556 ? O3 Pd2 O3 180.00(12) 3_556 . ? O5 Pd2 Pd1 98.14(6) . 3_556 ? O5 Pd2 Pd1 98.14(6) 3_556 . ? O5 Pd2 Pd1 81.86(6) 3_556 3_556 ? O5 Pd2 Pd1 81.86(6) . . ? O5 Pd2 O3 90.59(9) . 3_556 ? O5 Pd2 O3 89.41(9) . . ? O5 Pd2 O3 90.59(9) 3_556 . ? O5 Pd2 O3 89.41(9) 3_556 3_556 ? O5 Pd2 O5 180.0 . 3_556 ? N1 O1 C7 111.4(2) . . ? C11 O2 Pd1 130.5(2) . . ? C11 O3 Pd2 121.3(2) . . ? C13 O4 Pd1 123.07(19) . . ? C13 O5 Pd2 126.0(2) . . ? O1 N1 Pd1 121.07(19) . . ? C9 N1 Pd1 127.8(2) . . ? C9 N1 O1 111.0(3) . . ? C2 C1 Pd1 116.3(2) . . ? C6 C1 Pd1 124.2(3) . . ? C6 C1 C2 119.2(3) . . ? C1 C2 C7 118.7(3) . . ? C3 C2 C1 120.0(3) . . ? C3 C2 C7 121.3(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3 119.8 . . ? C3 C4 H4 120.0 . . ? C5 C4 C3 120.0(4) . . ? C5 C4 H4 120.0 . . ? C4 C5 H5 119.5 . . ? C4 C5 C6 121.0(4) . . ? C6 C5 H5 119.5 . . ? C1 C6 C5 119.3(4) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? O1 C7 C2 111.9(3) . . ? O1 C7 H7A 109.2 . . ? O1 C7 H7B 109.2 . . ? C2 C7 H7A 109.2 . . ? C2 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? N1 C9 C8 122.8(3) . . ? N1 C9 C10 118.7(3) . . ? C10 C9 C8 118.5(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O2 C11 O3 125.8(3) . . ? O2 C11 C12 116.8(3) . . ? O3 C11 C12 117.3(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C13 O5 127.0(3) . . ? O4 C13 C14 119.1(3) . . ? O5 C13 C14 114.0(3) . . ? C13 C14 H14A 110.7 . . ? C13 C14 H14B 109.9 . . ? C13 C14 H14C 108.1 . . ? H14A C14 H14B 109.7 . . ? H14A C14 H14C 109.2 . . ? H14B C14 H14C 109.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pd1 O2 C11 O3 16.0(5) . . . . ? Pd1 O2 C11 C12 -162.4(2) . . . . ? Pd1 O4 C13 O5 19.8(4) . . . . ? Pd1 O4 C13 C14 -160.4(2) . . . . ? Pd1 N1 C9 C8 -177.4(3) . . . . ? Pd1 N1 C9 C10 0.4(5) . . . . ? Pd1 C1 C2 C3 171.9(2) . . . . ? Pd1 C1 C2 C7 -7.6(4) . . . . ? Pd1 C1 C6 C5 -171.6(2) . . . . ? Pd2 O3 C11 O2 6.5(4) . . . . ? Pd2 O3 C11 C12 -175.0(2) . . . . ? Pd2 O5 C13 O4 2.9(5) . . . . ? Pd2 O5 C13 C14 -177.0(2) . . . . ? O1 N1 C9 C8 -1.4(5) . . . . ? O1 N1 C9 C10 176.4(3) . . . . ? N1 O1 C7 C2 63.9(3) . . . . ? C1 C2 C3 C4 0.0(5) . . . . ? C1 C2 C7 O1 -60.0(4) . . . . ? C2 C1 C6 C5 2.0(5) . . . . ? C2 C3 C4 C5 2.7(5) . . . . ? C3 C2 C7 O1 120.6(3) . . . . ? C3 C4 C5 C6 -2.9(6) . . . . ? C4 C5 C6 C1 0.6(5) . . . . ? C6 C1 C2 C3 -2.3(5) . . . . ? C6 C1 C2 C7 178.3(3) . . . . ? C7 O1 N1 Pd1 -5.1(3) . . . . ? C7 O1 N1 C9 178.6(3) . . . . ? C7 C2 C3 C4 179.4(3) . . . . ? _shelx_res_file ; TITL g140929c P 1 c 1 R = 0.03 New: P21/c CELL 0.71073 8.268408 13.104886 14.982289 90 98.2086 90 ZERR 2 0.000385 0.000498 0.000594 0 0.0041 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O Pd UNIT 56 72 4 20 6 L.S. 5 PLAN -20 BOND $H CONF fmap 2 acta OMIT 0 54 REM E:/Dropbox/C-H/Crystal/g140929c/g140929c.hkl WGHT 0.036000 0.277000 FVAR 3.97512 PD1 5 -0.053405 0.205380 0.572980 11.00000 0.03406 0.02613 = 0.02855 -0.00369 0.00614 -0.00144 PD2 5 0.000000 0.000000 0.500000 10.50000 0.02795 0.02902 = 0.02756 -0.00840 -0.00229 0.00375 O1 4 0.104355 0.336439 0.443919 11.00000 0.05329 0.04276 = 0.04143 -0.00073 0.01481 -0.01477 O2 4 -0.224868 0.114206 0.618964 11.00000 0.04629 0.03570 = 0.03604 -0.00431 0.01712 -0.00669 O3 4 -0.219742 -0.028969 0.537864 11.00000 0.03018 0.04172 = 0.04041 -0.00951 0.00050 0.00005 O4 4 0.127046 0.138189 0.676815 11.00000 0.05322 0.03563 = 0.03184 -0.00479 -0.00650 -0.00266 O5 4 0.105191 -0.023871 0.627020 11.00000 0.03976 0.03370 = 0.02981 -0.00424 -0.00561 0.00417 N1 3 0.093997 0.317344 0.535781 11.00000 0.03749 0.03548 = 0.04167 -0.00385 0.00927 -0.00423 C1 1 -0.219927 0.252051 0.474868 11.00000 0.03612 0.02200 = 0.03643 -0.00174 0.00338 0.00105 C2 1 -0.167427 0.268288 0.391572 11.00000 0.04833 0.02476 = 0.03286 -0.00008 0.00180 -0.00125 C3 1 -0.280253 0.288733 0.316105 11.00000 0.07345 0.03419 = 0.04158 0.00387 -0.00434 0.00019 AFIX 43 H3 2 -0.244847 0.299569 0.260678 11.00000 -1.20000 AFIX 0 C4 1 -0.444667 0.293106 0.322702 11.00000 0.06235 0.04293 = 0.06581 0.00346 -0.01911 0.00377 AFIX 43 H4 2 -0.520203 0.304039 0.271370 11.00000 -1.20000 AFIX 0 C5 1 -0.496483 0.281430 0.404302 11.00000 0.03191 0.04186 = 0.08801 0.00236 -0.00352 0.00233 AFIX 43 H5 2 -0.607123 0.287599 0.408686 11.00000 -1.20000 AFIX 0 C6 1 -0.385905 0.260313 0.481580 11.00000 0.04030 0.03200 = 0.06230 0.00050 0.01159 0.00402 AFIX 43 H6 2 -0.422605 0.251845 0.536966 11.00000 -1.20000 AFIX 0 C7 1 0.011519 0.262167 0.385820 11.00000 0.05197 0.03851 = 0.03342 -0.00086 0.01491 -0.00634 AFIX 23 H7A 2 0.050694 0.194177 0.402944 11.00000 -1.20000 H7B 2 0.028952 0.273821 0.323971 11.00000 -1.20000 AFIX 0 C8 1 0.277836 0.463621 0.550787 11.00000 0.07084 0.04454 = 0.09021 -0.01720 0.02213 -0.02589 AFIX 137 H8A 2 0.360316 0.433079 0.520378 11.00000 -1.50000 H8B 2 0.328894 0.504952 0.599765 11.00000 -1.50000 H8C 2 0.207768 0.505428 0.509160 11.00000 -1.50000 AFIX 0 C9 1 0.179096 0.381800 0.586660 11.00000 0.04309 0.03257 = 0.05683 -0.00868 0.00666 -0.00453 C10 1 0.175070 0.377475 0.685300 11.00000 0.07725 0.04715 = 0.05283 -0.01393 -0.00482 -0.01110 AFIX 137 H10A 2 0.089144 0.332492 0.697361 11.00000 -1.50000 H10B 2 0.155549 0.444579 0.707148 11.00000 -1.50000 H10C 2 0.277913 0.352558 0.715198 11.00000 -1.50000 AFIX 0 C11 1 -0.281499 0.030624 0.591220 11.00000 0.03383 0.03458 = 0.02654 0.00463 -0.00211 0.00167 C12 1 -0.438113 -0.001661 0.621472 11.00000 0.03816 0.05631 = 0.04305 0.00258 0.00659 -0.00401 AFIX 137 H12A 2 -0.526894 0.036491 0.589172 11.00000 -1.50000 H12B 2 -0.432830 0.010913 0.684947 11.00000 -1.50000 H12C 2 -0.455321 -0.073148 0.609749 11.00000 -1.50000 AFIX 0 C13 1 0.147813 0.044706 0.685822 11.00000 0.02854 0.03785 = 0.02877 -0.00437 -0.00019 -0.00366 C14 1 0.232844 0.003556 0.774966 11.00000 0.05226 0.04692 = 0.03208 -0.00106 -0.00640 -0.00319 AFIX 3 H14A 2 0.220534 -0.069154 0.777866 11.00000 -1.20000 H14B 2 0.188244 0.034956 0.823856 11.00000 -1.20000 H14C 2 0.347344 0.020056 0.779556 11.00000 -1.20000 AFIX 0 HKLF 4 REM g140929c P 1 c 1 R = 0.03 New: P21/c REM R1 = 0.0288 for 3024 Fo > 4sig(Fo) and 0.0367 for all 3504 data REM 199 parameters refined using 0 restraints END WGHT 0.0363 0.2770 REM Highest difference peak 0.922, deepest hole -0.667, 1-sigma level 0.089 Q1 1 -0.0804 0.1650 0.6094 11.00000 0.05 0.92 Q2 1 -0.0425 0.1556 0.5287 11.00000 0.05 0.54 Q3 1 0.3020 -0.0742 0.7678 11.00000 0.05 0.50 Q4 1 -0.4153 0.2793 0.5918 11.00000 0.05 0.46 Q5 1 -0.1476 -0.0086 0.3585 11.00000 0.05 0.39 Q6 1 0.0124 0.1228 0.5927 11.00000 0.05 0.39 Q7 1 -0.0976 0.2394 0.6294 11.00000 0.05 0.39 Q8 1 -0.0155 0.0452 0.5439 11.00000 0.05 0.38 Q9 1 -0.0691 0.2558 0.6189 11.00000 0.05 0.36 Q10 1 -0.2056 0.2426 0.4267 11.00000 0.05 0.36 Q11 1 -0.0032 0.4149 0.4980 11.00000 0.05 0.36 Q12 1 -0.4436 0.0653 0.6255 11.00000 0.05 0.35 Q13 1 0.0518 0.2813 0.5753 11.00000 0.05 0.35 Q14 1 -0.0662 0.2753 0.5311 11.00000 0.05 0.34 Q15 1 0.0512 0.1057 0.6892 11.00000 0.05 0.33 Q16 1 0.1864 0.1337 0.7024 11.00000 0.05 0.33 Q17 1 0.1236 -0.0827 0.8429 11.00000 0.05 0.32 Q18 1 0.2069 0.4349 0.5879 11.00000 0.05 0.31 Q19 1 0.0949 0.3788 0.5675 11.00000 0.05 0.30 Q20 1 0.1050 0.0000 0.3596 11.00000 0.05 0.30 ; _shelx_res_checksum 83032 _shelx_hkl_file ; 0 0 -3 59.3719 146.562 3 0 0 -3 75.3249 160.885 5 0 0 -3 316.309 137.079 1 0 0 -4 12947.5 628.893 1 0 0 -4 14474.4 775.701 5 0 0 -4 12683.5 639.632 3 0 0 -5 453.270 169.656 1 0 0 -5 25.8740 159.123 5 0 0 5 214.282 138.135 1 0 0 -5 86.0968 169.635 3 0 0 -6 44685.4 1622.74 5 0 0 -6 41230.3 1386.06 1 0 0 6 43654.6 1403.11 1 0 0 -6 44888.0 1466.01 3 0 0 -7-195.396 223.698 5 0 0 -7 18.3288 170.767 1 0 0 7 572.778 204.369 1 0 0 -7 77.9812 189.932 3 0 0 -8 44266.6 1681.75 1 0 0 -8 45391.6 1716.52 3 0 0 -8 47327.2 1962.03 5 0 0 8 46772.4 1703.06 1 0 0 -9 304.861 281.803 3 0 0 -9 63.5162 194.657 1 0 0 -9-216.482 331.362 5 0 0 9-2.77379 219.960 1 0 0 -10 44807.5 1955.78 3 0 0 -10 48074.3 2017.51 1 0 0 10 48987.4 1992.45 1 0 0 -11 286.018 333.719 3 0 0 -11-199.119 252.093 1 0 0 11-277.826 341.751 1 0 0 -12 66271.8 2679.98 1 0 0 -12 61272.6 2569.36 3 0 0 -13-113.456 282.173 1 0 0 -13 214.957 353.521 3 0 0 -14 39071.2 2274.37 3 0 0 -14 40952.7 2337.79 1 0 0 -15 358.497 446.491 3 0 0 -16 44961.6 2681.15 3 0 0 -17-141.332 478.142 3 0 0 -18 883.236 436.752 3 0 0 -19-745.802 659.509 3 0 1 -2 118166. 1428.29 3 0 -1 -3 22135.9 775.584 3 0 1 -3 20126.4 627.576 1 0 -1 -3 20426.6 757.816 1 0 1 -3 20435.6 717.252 3 0 -1 3 20839.3 620.953 1 0 1 -4 176790. 2369.14 3 0 -1 -4 174519. 2477.18 1 0 1 -4 172758. 2152.52 1 0 -1 4 171320. 2090.03 1 0 -1 -4 175241. 2433.16 3 0 -1 5 627.675 165.006 1 0 -1 -5 594.494 201.623 3 0 1 -5 111.831 165.356 5 0 1 -5 632.812 175.180 1 0 -1 -5 713.955 222.435 1 0 1 -5 586.695 202.700 3 0 -1 6 38872.6 1251.77 1 0 -1 -6 37832.6 1382.02 3 0 1 -6 39562.5 1388.63 3 0 1 -6 40304.2 1542.90 5 0 -1 -6 37799.0 1405.58 1 0 -1 -6 39445.1 1538.70 5 0 1 -6 39610.8 1302.75 1 0 1 6 37800.7 1391.42 1 0 1 7 96125.6 2382.32 1 0 -1 7 95743.0 2146.24 1 0 -1 -7 90170.8 2305.84 3 0 1 -7 96152.2 2597.44 5 0 -1 -7 96775.8 2610.00 5 0 1 -7 91706.6 2169.38 1 0 1 -7 92147.7 2274.78 3 0 -1 -7 88221.5 2307.11 1 0 -1 -8 45156.8 1923.54 5 0 1 -8 43987.9 1708.99 3 0 -1 -8 44216.8 1731.65 3 0 -1 -8 44375.8 1763.06 1 0 -1 8 45481.2 1620.07 1 0 1 8 47257.5 1797.00 1 0 1 -8 47922.0 1708.75 1 0 1 -8 46048.3 1955.39 5 0 1 -9 37752.4 1684.48 3 0 -1 9 38240.5 1591.02 1 0 1 -9 37630.5 1632.93 1 0 -1 -9 39359.8 1773.69 1 0 -1 -9 41489.8 1949.87 5 0 1 9 41071.6 1788.18 1 0 1 -9 36727.1 1860.65 5 0 -1 -9 39380.6 1742.10 3 0 -1 -10 140678. 3490.10 3 0 -1 -10 142312. 3578.55 1 0 1 -10 145295. 3401.49 1 0 1 -10 144385. 3491.05 3 0 -1 10 150746. 3361.13 1 0 -1 -11 40736.2 2039.24 1 0 1 -11 39482.7 1948.74 3 0 -1 -11 40386.1 1996.70 3 0 1 -11 41306.2 1930.16 1 0 -1 11 42109.8 1908.01 1 0 1 -12 47371.2 2243.66 3 0 -1 -12 49263.0 2314.98 3 0 -1 -12 48254.2 2339.46 1 0 -1 -13 14967.1 1357.19 3 0 -1 -13 13435.5 1322.02 1 0 1 -13 14610.9 1329.08 3 0 -1 -14 462.385 340.181 3 0 1 -14 21.6290 282.145 3 0 -1 -14 678.301 416.541 1 0 -1 -15 23458.3 1909.67 1 0 1 -15 23341.8 1848.67 3 0 -1 -15 24165.4 1879.11 3 0 -1 -16 25436.7 2058.02 1 0 1 -16 23239.9 1924.65 3 0 -1 -16 22926.5 1919.06 3 0 -1 -17 7104.54 1193.46 3 0 1 -17 7280.41 1190.18 3 0 -1 -18 14955.5 1703.24 3 0 1 -18 13097.3 1611.85 3 0 -1 -19-558.770 587.449 3 0 1 -19-362.578 556.865 3 0 -2 0 75780.9 964.514 1 0 -2 -1 124366. 1614.25 1 0 -2 -2 21153.6 771.035 1 0 -2 2 21251.3 799.587 4 0 -2 2 19856.3 437.048 2 0 -2 3 139870. 2264.80 4 0 -2 -3 124831. 2078.79 1 0 -2 -4 123994. 2279.73 1 0 -2 4 135221. 1760.94 1 0 2 -4 134859. 2146.50 3 0 -2 4 139105. 2494.29 4 0 -2 -4 127496. 2240.52 3 0 2 -5 4459.83 445.866 3 0 -2 5 5330.25 542.044 4 0 -2 -5 4334.19 479.612 3 0 -2 5 4430.98 368.400 1 0 -2 6 322279. 4400.27 4 0 -2 -6 314243. 4262.41 1 0 -2 6 322567. 3433.97 1 0 -2 -6 311275. 4116.23 3 0 2 -6 320741. 3976.37 3 0 -2 -7 933.259 276.714 3 0 -2 7 1027.21 250.877 1 0 -2 -7 1479.50 375.045 1 0 2 -7 839.438 276.928 3 0 -2 -8 308549. 5038.95 5 0 -2 8 308511. 4001.81 1 0 2 -8 299836. 4480.74 3 0 -2 -8 297058. 4738.48 1 0 -2 -8 307860. 4639.06 3 0 -2 -9 51514.9 2199.45 5 0 -2 9 54873.7 1835.30 1 0 -2 -9 51944.3 2026.75 3 0 -2 -9 53042.5 2138.79 1 0 2 -9 54281.6 2036.74 3 0 -2 9 50332.5 2153.71 5 0 2 9 55635.7 2174.08 1 0 -2 10 31433.0 1497.12 1 0 -2 10 34150.8 1875.52 5 0 -2 -10 27144.8 1608.18 1 0 2 -10 30059.8 1605.22 3 0 -2 -10 29826.5 1642.14 3 0 -2 -11 28221.2 1663.47 3 0 -2 11 30169.6 1871.28 5 0 -2 11 27604.8 1488.93 1 0 -2 -11 28261.2 1729.28 1 0 2 -11 26730.8 1618.33 3 0 -2 -12 6168.25 918.846 1 0 -2 -12 4114.12 710.668 3 0 -2 12 6042.22 763.426 1 0 2 -12 3975.85 721.054 3 0 -2 -13 261.414 352.725 1 0 -2 -13 435.036 342.974 3 0 2 -13 636.520 413.248 3 0 2 -14 309.081 351.026 3 0 -2 -14 355.014 341.883 3 0 -2 -14 577.207 346.792 1 0 -2 -15 795.106 393.439 1 0 2 -15-540.870 574.761 3 0 -2 -15-389.458 431.162 3 0 2 -16-713.927 608.425 3 0 -2 -16 224.497 325.434 3 0 -2 -16-400.637 462.438 1 0 -2 -17 6014.74 1107.87 1 0 2 -17 5738.99 1024.25 3 0 -2 -17 6937.16 1171.14 3 0 -2 -18 11094.4 1501.61 3 0 2 -18 12190.4 1534.99 3 0 -2 -19 5570.01 1147.12 3 0 -3 0 154.542 110.579 1 0 -3 -1 144873. 2000.34 1 0 -3 -2 52651.8 1361.57 1 0 -3 3 31751.3 1194.87 4 0 -3 3 33075.5 684.581 2 0 -3 -3 32272.6 1164.20 1 0 -3 4 180399. 1930.42 2 0 -3 4 189231. 3133.82 4 0 -3 -4 182009. 3001.32 1 0 -3 -5 182264. 3210.08 1 0 -3 5 182421. 2255.13 1 0 -3 -5 174868. 3039.41 3 0 -3 6 19485.3 819.841 1 0 -3 -6 19835.8 1133.08 1 0 -3 6 22228.6 1231.61 4 0 3 -6 18188.6 1000.84 3 0 -3 -6 22067.7 1162.33 3 0 -3 -7 267519. 4202.76 3 0 -3 7 275428. 4595.09 4 0 -3 7 276509. 3376.95 1 0 -3 -7 265081. 4374.23 1 0 3 -7 268205. 4056.31 3 0 3 -8 2491.82 455.157 3 0 -3 8 3262.84 412.166 1 0 -3 8 3702.16 582.308 4 0 -3 -8 1913.64 447.522 3 0 -3 -8 1911.57 438.709 1 0 -3 -9 85431.3 2794.30 1 0 -3 9 88295.4 2235.88 1 0 -3 -9 91063.8 2752.33 3 0 -3 9 93509.1 2957.45 4 0 3 9 92792.6 2914.56 1 0 3 -9 86141.4 2613.18 3 0 -3 9 93628.5 2989.18 5 0 -3 10 33057.0 1900.17 5 0 -3 10 33718.4 1493.75 1 0 -3 -10 31062.0 1777.00 1 0 -3 -10 30466.8 1689.50 3 0 3 -10 30571.1 1640.14 3 0 -3 11 4267.90 786.178 5 0 -3 -11 4689.85 723.796 3 0 -3 11 5645.33 663.804 1 0 -3 -11 4245.98 744.970 1 0 3 -11 5219.47 750.399 3 0 -3 12 64991.6 2348.40 1 0 -3 -12 60763.4 2767.48 1 0 -3 -12 62585.1 2646.15 3 0 -3 12 67807.3 2961.39 5 0 3 -12 63131.6 2622.65 3 0 -3 -13 16180.2 1510.34 1 0 -3 -13 15092.0 1391.59 3 0 3 -13 15231.8 1367.51 3 0 -3 13 15627.5 1535.41 5 0 -3 -14 25.3312 314.335 1 0 -3 -14-98.4820 362.930 3 0 3 -14 25.4816 277.615 3 0 3 -15-259.464 399.881 3 0 -3 -15 81.2114 415.679 1 0 -3 -15 119.705 403.729 3 0 3 -16 14216.8 1528.24 3 0 -3 -16 14563.5 1564.18 3 0 -3 -16 15601.0 1692.32 1 0 -3 -17 2778.46 802.399 3 0 -3 -17 3887.45 979.257 1 0 -3 -18 4892.31 984.703 3 0 -3 -18 4791.98 1005.63 1 0 -3 -19 11050.9 1553.89 3 0 -4 0 948052. 4840.79 1 0 4 -1 193260. 1547.53 2 0 -4 -1 223780. 2848.59 1 0 -4 -2 378970. 4008.74 1 0 4 -2 373700. 1934.04 2 0 -4 3 388964. 2280.24 2 0 -4 -3 395050. 4375.74 1 0 -4 -4 53156.3 1731.30 1 0 -4 4 54111.2 1024.73 2 0 -4 4 54813.8 1815.55 4 0 -4 -5 127665. 2842.52 1 0 -4 5 123715. 1864.11 1 0 -4 5 129972. 1812.21 2 0 -4 6 119.778 91.4535 1 0 -4 6 136.930 189.967 4 0 -4 -6 922.501 352.808 1 0 -4 6 1491.51 232.553 2 0 -4 -6 1935.07 413.010 3 0 -4 7 717.588 188.752 1 0 -4 7 1182.27 361.455 4 0 -4 -7 1131.77 364.922 1 0 -4 -7 902.512 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19269.3 1807.57 4 0 11 -8 17876.4 1801.68 4 0 -11 8 18727.7 719.279 1 0 -11 -8 22046.2 1755.67 1 0 11 -9 30060.7 2377.50 4 0 -11 -9 29915.5 1942.07 3 0 -11 -9 27074.8 2019.35 1 0 -11 -10 43254.3 2619.38 1 0 -11 -10 39809.0 2266.33 3 0 -11 -11 11183.0 1258.24 3 0 -11 -11 12083.0 1449.75 1 0 -11 -12 12627.7 1359.96 3 0 -11 -12 12410.9 1524.57 1 0 -11 13 2407.53 706.385 5 0 -11 -13 3306.48 768.192 3 0 -11 -13 2945.16 818.327 1 0 -11 14-121.789 536.589 5 0 -11 -14-287.525 485.045 1 0 -11 -14 230.995 378.274 3 0 -11 -15 2781.30 652.968 3 0 -11 -16 7397.32 1161.76 3 0 -12 0 33883.9 1659.81 1 0 12 0 32008.2 1292.12 2 0 -12 -1 744.389 307.115 1 0 -12 1 1246.77 344.511 1 0 12 -1 1042.16 236.590 2 0 -12 2 657.313 293.743 1 0 -12 -2 839.697 353.689 1 0 12 -2 536.887 399.030 4 0 12 -2 540.732 141.521 2 0 -12 3 448.470 247.358 1 0 12 -3 1013.31 479.390 4 0 -12 -3 169.905 239.535 1 0 -12 4 54179.7 1741.03 1 0 -12 -4 53368.6 2430.67 1 0 12 -4 50338.8 2901.33 4 0 12 -5 57.0064 432.941 4 0 -12 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3102.94 866.336 2 10 -3 -6 302.264 384.895 2 10 3 -6-361.498 351.995 2 10 -3 -5 20.8865 446.970 2 10 3 -5 1106.87 564.799 2 10 -3 -4 4219.84 890.276 2 10 3 -4 4656.31 972.195 2 10 3 -3 5065.02 1047.38 2 10 -3 -3 4902.53 966.311 2 10 3 -2 4966.33 1074.18 2 10 -3 -2 4906.92 930.112 2 10 -3 -1 22107.7 1992.26 2 10 3 -1 24644.8 2246.51 2 10 3 0 813.247 471.639 2 10 -3 0 394.263 347.596 2 10 -3 1 31267.1 2365.05 2 10 3 1 30452.1 2538.09 2 10 -3 2 3294.26 888.503 2 10 3 2 3061.97 880.892 2 10 -3 3 13159.2 1578.58 2 10 3 3 11162.6 1578.17 2 10 -3 4 10839.6 1445.71 2 10 3 4 10086.8 1486.57 2 10 -3 5 584.042 475.177 2 10 -3 6 1661.12 638.393 2 10 -3 7 1233.43 565.181 2 10 -4 -10 2177.01 680.235 1 10 4 -8 7675.94 1334.59 2 10 -4 -7 1652.55 651.957 2 10 4 -7 284.372 445.480 2 10 -4 -6 9752.71 1354.58 2 10 4 -6 10464.9 1490.74 2 10 -4 -5 4091.30 909.955 2 10 4 -5 3395.85 903.263 2 10 4 -4 8664.57 1363.34 2 10 -4 -4 10243.3 1366.44 2 10 4 -3 8194.92 1318.61 2 10 -4 -3 6634.49 1136.79 2 10 4 -2 2411.59 818.733 2 10 -4 -2 2762.07 719.244 2 10 4 -1 315.409 387.696 2 10 -4 -1 184.427 330.948 2 10 4 0 765.682 503.829 2 10 -4 0-31.3165 305.042 2 10 4 1 1802.47 763.976 2 10 -4 1 1061.95 512.374 2 10 -4 2 309.195 372.601 2 10 4 2 2601.50 797.061 2 10 -4 3 5901.10 1059.93 2 10 4 3 6788.52 1207.19 2 10 -4 4 3411.40 837.414 2 10 -4 5 5330.72 993.147 2 10 5 -7 21906.3 2189.32 2 10 -5 -6 524.458 423.361 2 10 5 -6-731.331 662.940 2 10 -5 -5 22184.2 1977.76 2 10 5 -5 20416.7 2131.33 2 10 5 -4-437.810 568.663 2 10 -5 -4-221.151 444.707 2 10 5 -3 2900.85 929.962 2 10 -5 -3 3861.42 872.856 2 10 5 -2 1548.58 692.001 2 10 -5 -2 1628.08 580.370 2 10 5 -1 308.543 459.626 2 10 -5 -1 913.665 407.673 2 10 5 0 2043.40 727.321 2 10 -5 0 1045.24 498.033 2 10 5 1 2205.25 814.297 2 10 -5 1 2479.39 687.863 2 10 -5 2-451.477 361.635 2 10 -5 3-770.305 438.628 2 10 6 -5 4701.83 1105.68 2 10 6 -4 1472.01 634.530 2 10 -6 -4 3941.69 883.636 2 10 -6 -3 16036.4 1634.19 2 10 6 -3 14798.2 1800.34 2 10 6 -2 4983.40 1126.21 2 10 -6 -2 4196.14 852.476 2 10 6 -1 6075.14 1225.90 2 10 -6 -1 6770.18 1085.86 2 10 -6 0 1753.70 619.813 2 10 -6 1 49.4126 301.552 2 10 -7 -3 1975.82 598.312 2 10 -7 -2 2508.75 700.276 2 11 -1 -3 3324.57 954.906 2 11 -1 -2 8452.09 1352.13 2 11 -1 -1 339.305 352.144 2 11 -1 0 1295.46 615.168 2 11 -1 1 769.537 560.189 2 11 -2 -4 183.235 326.515 2 11 -2 -3 3613.17 928.072 2 11 -2 -2 7061.83 1220.73 2 11 -2 -1 2190.01 794.763 2 11 -2 0 14583.6 1780.26 2 11 -2 1 936.076 529.528 2 11 -2 2 15247.4 1812.37 2 11 -3 -4-502.456 542.092 2 11 -3 -3-655.575 462.338 2 11 -3 -2 1248.30 490.770 2 11 -3 -1 11146.1 1561.46 2 11 -3 0 1351.42 681.953 2 11 -3 1 18316.1 1924.43 2 11 -3 2 983.146 502.230 2 11 -3 3 5671.40 1047.95 2 11 -4 -4 2087.60 653.319 2 11 -4 -3 3918.21 890.351 2 11 -4 -2 876.775 439.682 2 11 -4 -1 2273.58 705.393 2 11 -4 0-423.519 422.974 2 11 -4 1 221.014 309.874 2 11 -4 2-197.334 296.183 2 11 -5 -4 1100.47 541.952 2 11 -5 -3 5263.45 1006.48 2 11 -5 -2 634.882 428.034 2 11 -5 -1-560.005 415.670 2 11 -5 0-1680.29 630.899 2 11 -6 -4 2086.11 658.003 2 0 0 0 0.00 0.00 0 TITL g140929c in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 8.268408 13.104886 14.982289 90.0000 98.2086 90.0000 ZERR 23.00 0.000385 0.000498 0.000594 0.0000 0.0041 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C D Ho Np UNIT 23.00 23.00 23.00 23.00 TREF HKLF 4 END ; _shelx_hkl_checksum 38697 _olex2_submission_special_instructions 'No special instructions were received'