# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_shelxl _database_code_depnum_ccdc_archive 'CCDC 915278' #TrackingRef '16079_web_deposit_cif_file_0_MarcD.Walter_1355237780.twin5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H57 P2 Pd, F6 Sb' _chemical_formula_sum 'C25 H57 F6 P2 Pd Sb' _chemical_formula_weight 761.80 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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' '-x, -y, -z' 'x-1/2, -y, z' _cell_length_a 14.5334(6) _cell_length_b 14.2796(5) _cell_length_c 15.2101(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.956(3) _cell_angle_gamma 90.00 _cell_volume 3152.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 532 _cell_measurement_theta_min 6.10 _cell_measurement_theta_max 68.68 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 12.782 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2501 _exptl_absorpt_correction_T_max 0.5674 _exptl_absorpt_process_details 'TWINABS Version 2008/4' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54185 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9649 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 65.64 _reflns_number_total 9649 _reflns_number_gt 6987 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1151P)^2^+3.2323P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9649 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1953 _refine_ls_wR_factor_gt 0.1785 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb01 Sb 0.2500 -0.22714(4) 1.0000 0.02325(18) Uani 1 2 d S . . Sb02 Sb 0.2500 -0.22319(5) 0.5000 0.02896(19) Uani 1 2 d S . . Pd1 Pd 0.25463(3) 0.26707(3) 0.74747(3) 0.01868(16) Uani 1 1 d . . . P2 P 0.38247(10) 0.37715(11) 0.74522(10) 0.0184(3) Uani 1 1 d . . . P1 P 0.14417(10) 0.14720(11) 0.74985(10) 0.0184(3) Uani 1 1 d . . . F2 F 0.2560(3) -0.2274(3) 0.8780(2) 0.0390(10) Uani 1 1 d . . . F5 F 0.2924(3) -0.2234(3) 0.6180(2) 0.0487(12) Uani 1 1 d . . . F4 F 0.1627(3) -0.3161(3) 0.5236(3) 0.0405(10) Uani 1 1 d . . . F3 F 0.1580(3) -0.3194(3) 0.9904(3) 0.0406(10) Uani 1 1 d . . . F6 F 0.3368(3) -0.1299(3) 0.4759(3) 0.0631(15) Uani 1 1 d . . . F1 F 0.3417(3) -0.1335(3) 1.0088(3) 0.0377(10) Uani 1 1 d . . . C21 C 0.4917(4) 0.3023(4) 0.7452(4) 0.0274(14) Uani 1 1 d . . . C5 C 0.0553(4) 0.1455(5) 0.8382(4) 0.0288(15) Uani 1 1 d . . . C12 C 0.1978(5) -0.0501(5) 0.7434(4) 0.0361(17) Uani 1 1 d . . . H12A H 0.2490 -0.0939 0.7545 0.054 Uiso 1 1 calc R . . H12B H 0.1796 -0.0501 0.6804 0.054 Uiso 1 1 calc R . . H12C H 0.1454 -0.0694 0.7771 0.054 Uiso 1 1 calc R . . C13 C 0.3806(5) 0.4572(5) 0.6444(4) 0.0276(15) Uani 1 1 d . . . C17 C 0.3867(5) 0.4535(5) 0.8484(4) 0.0301(16) Uani 1 1 d . . . C1 C 0.0831(4) 0.1342(4) 0.6372(4) 0.0244(14) Uani 1 1 d . . . C19 C 0.3590(5) 0.3934(5) 0.9270(4) 0.0369(17) Uani 1 1 d . . . H19A H 0.3455 0.4344 0.9765 0.055 Uiso 1 1 calc R . . H19B H 0.4098 0.3512 0.9448 0.055 Uiso 1 1 calc R . . H19C H 0.3041 0.3565 0.9099 0.055 Uiso 1 1 calc R . . C18 C 0.3175(5) 0.5338(5) 0.8394(5) 0.0431(19) Uani 1 1 d . . . H18A H 0.2571 0.5091 0.8195 0.065 Uiso 1 1 calc R . . H18B H 0.3382 0.5793 0.7965 0.065 Uiso 1 1 calc R . . H18C H 0.3128 0.5645 0.8966 0.065 Uiso 1 1 calc R . . C15 C 0.4482(5) 0.5387(5) 0.6499(4) 0.0370(18) Uani 1 1 d . . . H15A H 0.4484 0.5703 0.5927 0.055 Uiso 1 1 calc R . . H15B H 0.5102 0.5152 0.6659 0.055 Uiso 1 1 calc R . . H15C H 0.4296 0.5832 0.6948 0.055 Uiso 1 1 calc R . . C11 C 0.3147(4) 0.0757(5) 0.7225(5) 0.0380(18) Uani 1 1 d . . . H11A H 0.3639 0.0302 0.7361 0.057 Uiso 1 1 calc R . . H11B H 0.3353 0.1382 0.7415 0.057 Uiso 1 1 calc R . . H11C H 0.2999 0.0762 0.6589 0.057 Uiso 1 1 calc R . . C4 C 0.0101(4) 0.0563(5) 0.6297(4) 0.0321(17) Uani 1 1 d . . . H4A H -0.0431 0.0741 0.6631 0.048 Uiso 1 1 calc R . . H4B H 0.0365 -0.0021 0.6535 0.048 Uiso 1 1 calc R . . H4C H -0.0097 0.0473 0.5677 0.048 Uiso 1 1 calc R . . C20 C 0.4817(5) 0.4954(5) 0.8738(4) 0.0361(18) Uani 1 1 d . . . H20A H 0.5061 0.5265 0.8224 0.054 Uiso 1 1 calc R . . H20B H 0.5238 0.4453 0.8939 0.054 Uiso 1 1 calc R . . H20C H 0.4758 0.5411 0.9212 0.054 Uiso 1 1 calc R . . C23 C 0.5003(5) 0.2485(5) 0.8316(5) 0.0384(18) Uani 1 1 d . . . H23A H 0.5531 0.2059 0.8308 0.058 Uiso 1 1 calc R . . H23B H 0.4439 0.2122 0.8388 0.058 Uiso 1 1 calc R . . H23C H 0.5093 0.2926 0.8806 0.058 Uiso 1 1 calc R . . C2 C 0.1547(5) 0.1150(5) 0.5678(4) 0.0354(17) Uani 1 1 d . . . H2A H 0.1274 0.1288 0.5089 0.053 Uiso 1 1 calc R . . H2B H 0.1733 0.0491 0.5707 0.053 Uiso 1 1 calc R . . H2C H 0.2087 0.1549 0.5796 0.053 Uiso 1 1 calc R . . C10 C 0.2623(5) 0.0464(5) 0.8699(4) 0.0389(19) Uani 1 1 d . . . H10A H 0.2142 0.0199 0.9053 0.058 Uiso 1 1 calc R . . H10B H 0.2764 0.1103 0.8898 0.058 Uiso 1 1 calc R . . H10C H 0.3179 0.0077 0.8768 0.058 Uiso 1 1 calc R . . C8 C 0.0240(5) 0.0464(5) 0.8610(4) 0.0337(17) Uani 1 1 d . . . H8A H -0.0245 0.0500 0.9033 0.051 Uiso 1 1 calc R . . H8B H 0.0764 0.0110 0.8868 0.051 Uiso 1 1 calc R . . H8C H -0.0001 0.0150 0.8073 0.051 Uiso 1 1 calc R . . C16 C 0.2819(5) 0.4955(5) 0.6253(5) 0.0403(19) Uani 1 1 d . . . H16A H 0.2638 0.5335 0.6752 0.060 Uiso 1 1 calc R . . H16B H 0.2389 0.4430 0.6165 0.060 Uiso 1 1 calc R . . H16C H 0.2805 0.5342 0.5720 0.060 Uiso 1 1 calc R . . C9 C 0.2280(4) 0.0481(5) 0.7714(4) 0.0307(16) Uani 1 1 d . . . C22 C 0.4829(5) 0.2297(5) 0.6690(4) 0.0333(17) Uani 1 1 d . . . H22A H 0.5254 0.2463 0.6235 0.050 Uiso 1 1 calc R . . H22B H 0.4196 0.2299 0.6434 0.050 Uiso 1 1 calc R . . H22C H 0.4980 0.1671 0.6919 0.050 Uiso 1 1 calc R . . C14 C 0.4013(5) 0.3985(5) 0.5629(4) 0.0383(18) Uani 1 1 d . . . H14A H 0.3896 0.4362 0.5096 0.057 Uiso 1 1 calc R . . H14B H 0.3616 0.3430 0.5602 0.057 Uiso 1 1 calc R . . H14C H 0.4660 0.3789 0.5668 0.057 Uiso 1 1 calc R . . C25 C 0.1579(5) 0.3659(5) 0.7685(5) 0.0413(19) Uani 1 1 d . . . H25A H 0.0965 0.3402 0.7540 0.062 Uiso 1 1 calc R . . H25B H 0.1683 0.4205 0.7313 0.062 Uiso 1 1 calc R . . H25C H 0.1622 0.3848 0.8305 0.062 Uiso 1 1 calc R . . C3 C 0.0391(4) 0.2277(5) 0.6102(4) 0.0297(16) Uani 1 1 d . . . H3A H 0.0050 0.2208 0.5533 0.045 Uiso 1 1 calc R . . H3B H 0.0874 0.2751 0.6053 0.045 Uiso 1 1 calc R . . H3C H -0.0033 0.2474 0.6548 0.045 Uiso 1 1 calc R . . C24 C 0.5815(4) 0.3530(5) 0.7331(5) 0.0394(18) Uani 1 1 d . . . H24A H 0.5888 0.4034 0.7766 0.059 Uiso 1 1 calc R . . H24B H 0.5810 0.3796 0.6737 0.059 Uiso 1 1 calc R . . H24C H 0.6328 0.3088 0.7411 0.059 Uiso 1 1 calc R . . C6 C 0.0979(5) 0.1933(5) 0.9222(4) 0.0425(19) Uani 1 1 d . . . H6A H 0.0513 0.1976 0.9664 0.064 Uiso 1 1 calc R . . H6B H 0.1190 0.2563 0.9075 0.064 Uiso 1 1 calc R . . H6C H 0.1502 0.1562 0.9458 0.064 Uiso 1 1 calc R . . C7 C -0.0308(4) 0.2027(6) 0.8106(5) 0.0420(19) Uani 1 1 d . . . H7A H -0.0633 0.1726 0.7601 0.063 Uiso 1 1 calc R . . H7B H -0.0125 0.2662 0.7942 0.063 Uiso 1 1 calc R . . H7C H -0.0717 0.2060 0.8598 0.063 Uiso 1 1 calc 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 Sb01 0.0231(3) 0.0206(4) 0.0260(3) 0.000 0.0001(3) 0.000 Sb02 0.0358(4) 0.0219(4) 0.0287(4) 0.000 -0.0029(3) 0.000 Pd1 0.0170(3) 0.0151(3) 0.0240(3) -0.00121(17) 0.0019(2) 0.00030(17) P2 0.0181(8) 0.0166(8) 0.0203(8) -0.0007(6) -0.0012(6) -0.0027(6) P1 0.0150(7) 0.0169(8) 0.0235(8) -0.0006(6) 0.0025(6) 0.0001(6) F2 0.041(2) 0.053(3) 0.023(2) 0.0013(17) -0.0003(18) 0.002(2) F5 0.061(3) 0.058(3) 0.026(2) -0.0070(19) -0.006(2) 0.012(2) F4 0.037(2) 0.033(2) 0.053(3) 0.0008(19) 0.018(2) -0.0070(19) F3 0.043(2) 0.029(2) 0.048(3) 0.0135(18) -0.0160(19) -0.0201(19) F6 0.068(3) 0.037(3) 0.082(4) 0.025(3) -0.023(3) -0.028(2) F1 0.031(2) 0.029(2) 0.053(3) -0.0069(19) 0.0009(18) -0.0113(18) C21 0.024(3) 0.024(4) 0.034(4) -0.001(3) 0.001(3) 0.002(3) C5 0.025(3) 0.037(4) 0.026(3) 0.003(3) 0.011(3) -0.004(3) C12 0.042(4) 0.029(4) 0.036(4) 0.001(3) -0.003(3) 0.007(3) C13 0.040(4) 0.021(4) 0.022(3) 0.007(3) 0.000(3) -0.007(3) C17 0.034(4) 0.026(4) 0.030(4) -0.007(3) -0.002(3) -0.003(3) C1 0.027(4) 0.018(4) 0.027(3) -0.002(3) -0.001(3) -0.007(3) C19 0.055(5) 0.030(4) 0.026(4) -0.006(3) 0.009(3) -0.003(4) C18 0.051(5) 0.042(5) 0.036(4) -0.012(3) -0.005(4) 0.006(4) C15 0.037(4) 0.042(5) 0.031(4) 0.013(3) -0.008(3) -0.012(4) C11 0.028(4) 0.036(4) 0.051(5) 0.006(3) 0.010(3) 0.004(3) C4 0.029(4) 0.033(4) 0.034(4) -0.005(3) -0.007(3) -0.006(3) C20 0.051(5) 0.035(4) 0.022(4) -0.007(3) -0.001(3) -0.012(4) C23 0.030(4) 0.030(4) 0.055(5) 0.002(3) -0.003(3) 0.010(3) C2 0.049(4) 0.038(4) 0.020(3) -0.008(3) 0.003(3) -0.004(4) C10 0.034(4) 0.045(5) 0.037(4) 0.007(4) -0.003(3) 0.004(4) C8 0.026(4) 0.046(5) 0.030(4) 0.007(3) 0.003(3) -0.010(3) C16 0.041(4) 0.031(5) 0.048(5) 0.010(3) -0.006(3) -0.001(4) C9 0.029(4) 0.028(4) 0.036(4) 0.004(3) 0.012(3) 0.004(3) C22 0.029(4) 0.032(5) 0.039(4) -0.003(3) 0.007(3) 0.004(3) C14 0.058(5) 0.035(5) 0.022(4) 0.001(3) -0.001(3) -0.006(4) C25 0.037(4) 0.015(4) 0.073(6) -0.012(4) 0.010(4) 0.007(3) C3 0.024(4) 0.031(4) 0.032(4) 0.004(3) -0.007(3) -0.002(3) C24 0.022(3) 0.042(5) 0.055(5) -0.009(4) 0.004(3) -0.001(3) C6 0.046(5) 0.047(5) 0.036(4) -0.005(3) 0.011(3) -0.007(4) C7 0.025(4) 0.060(6) 0.042(4) -0.008(4) 0.013(3) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb01 F2 1.862(4) 2_557 ? Sb01 F2 1.862(4) . ? Sb01 F3 1.877(4) 2_557 ? Sb01 F3 1.877(4) . ? Sb01 F1 1.888(4) . ? Sb01 F1 1.888(4) 2_557 ? Sb02 F5 1.868(4) . ? Sb02 F5 1.868(4) 2_556 ? Sb02 F4 1.882(4) 2_556 ? Sb02 F4 1.882(4) . ? Sb02 F6 1.883(4) . ? Sb02 F6 1.883(4) 2_556 ? Pd1 C25 2.029(6) . ? Pd1 P1 2.3483(15) . ? Pd1 P2 2.4353(15) . ? P2 C17 1.909(6) . ? P2 C13 1.911(6) . ? P2 C21 1.914(6) . ? P1 C9 1.886(7) . ? P1 C1 1.898(6) . ? P1 C5 1.912(6) . ? C21 C24 1.511(8) . ? C21 C23 1.521(9) . ? C21 C22 1.557(8) . ? C5 C8 1.530(9) . ? C5 C7 1.536(9) . ? C5 C6 1.549(9) . ? C12 C9 1.524(9) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.524(9) . ? C13 C14 1.539(8) . ? C13 C16 1.549(9) . ? C17 C18 1.526(9) . ? C17 C20 1.536(9) . ? C17 C19 1.543(9) . ? C1 C3 1.528(9) . ? C1 C4 1.537(8) . ? C1 C2 1.545(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C11 C9 1.547(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C10 C9 1.555(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? 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 F2 Sb01 F2 179.8(3) 2_557 . ? F2 Sb01 F3 89.46(17) 2_557 2_557 ? F2 Sb01 F3 90.36(17) . 2_557 ? F2 Sb01 F3 90.36(17) 2_557 . ? F2 Sb01 F3 89.46(17) . . ? F3 Sb01 F3 90.9(3) 2_557 . ? F2 Sb01 F1 89.99(17) 2_557 . ? F2 Sb01 F1 90.18(17) . . ? F3 Sb01 F1 89.63(18) 2_557 . ? F3 Sb01 F1 179.37(17) . . ? F2 Sb01 F1 90.18(17) 2_557 2_557 ? F2 Sb01 F1 89.99(17) . 2_557 ? F3 Sb01 F1 179.37(18) 2_557 2_557 ? F3 Sb01 F1 89.63(18) . 2_557 ? F1 Sb01 F1 89.9(2) . 2_557 ? F5 Sb02 F5 179.8(3) . 2_556 ? F5 Sb02 F4 89.43(18) . 2_556 ? F5 Sb02 F4 90.45(19) 2_556 2_556 ? F5 Sb02 F4 90.5(2) . . ? F5 Sb02 F4 89.43(18) 2_556 . ? F4 Sb02 F4 90.4(2) 2_556 . ? F5 Sb02 F6 89.8(2) . . ? F5 Sb02 F6 90.28(19) 2_556 . ? F4 Sb02 F6 89.8(2) 2_556 . ? F4 Sb02 F6 179.6(2) . . ? F5 Sb02 F6 90.28(19) . 2_556 ? F5 Sb02 F6 89.8(2) 2_556 2_556 ? F4 Sb02 F6 179.6(2) 2_556 2_556 ? F4 Sb02 F6 89.8(2) . 2_556 ? F6 Sb02 F6 90.0(3) . 2_556 ? C25 Pd1 P1 91.4(2) . . ? C25 Pd1 P2 95.1(2) . . ? P1 Pd1 P2 173.40(5) . . ? C17 P2 C13 108.4(3) . . ? C17 P2 C21 109.1(3) . . ? C13 P2 C21 108.1(3) . . ? C17 P2 Pd1 110.4(2) . . ? C13 P2 Pd1 114.7(2) . . ? C21 P2 Pd1 105.9(2) . . ? C9 P1 C1 110.6(3) . . ? C9 P1 C5 108.8(3) . . ? C1 P1 C5 109.4(3) . . ? C9 P1 Pd1 96.5(2) . . ? C1 P1 Pd1 110.2(2) . . ? C5 P1 Pd1 120.5(2) . . ? C24 C21 C23 108.4(5) . . ? C24 C21 C22 105.5(5) . . ? C23 C21 C22 107.8(6) . . ? C24 C21 P2 117.0(5) . . ? C23 C21 P2 108.2(4) . . ? C22 C21 P2 109.6(4) . . ? C8 C5 C7 107.8(6) . . ? C8 C5 C6 109.4(6) . . ? C7 C5 C6 106.0(6) . . ? C8 C5 P1 113.0(5) . . ? C7 C5 P1 111.8(4) . . ? C6 C5 P1 108.6(4) . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 107.9(5) . . ? C15 C13 C16 109.2(6) . . ? C14 C13 C16 105.0(5) . . ? C15 C13 P2 115.5(4) . . ? C14 C13 P2 109.0(5) . . ? C16 C13 P2 109.7(4) . . ? C18 C17 C20 108.0(6) . . ? C18 C17 C19 106.9(6) . . ? C20 C17 C19 106.8(5) . . ? C18 C17 P2 111.3(5) . . ? C20 C17 P2 114.8(4) . . ? C19 C17 P2 108.7(5) . . ? C3 C1 C4 109.6(5) . . ? C3 C1 C2 105.0(5) . . ? C4 C1 C2 107.9(5) . . ? C3 C1 P1 109.0(4) . . ? C4 C1 P1 115.3(4) . . ? C2 C1 P1 109.5(4) . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C9 C11 109.3(6) . . ? C12 C9 C10 109.2(5) . . ? C11 C9 C10 103.9(6) . . ? C12 C9 P1 117.9(5) . . ? C11 C9 P1 105.1(4) . . ? C10 C9 P1 110.6(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Pd1 C25 H25A 109.5 . . ? Pd1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Pd1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? 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 C25 Pd1 P2 C17 52.7(3) . . . . ? P1 Pd1 P2 C17 -117.4(5) . . . . ? C25 Pd1 P2 C13 -70.1(3) . . . . ? P1 Pd1 P2 C13 119.7(5) . . . . ? C25 Pd1 P2 C21 170.7(3) . . . . ? P1 Pd1 P2 C21 0.5(5) . . . . ? C25 Pd1 P1 C9 -160.9(3) . . . . ? P2 Pd1 P1 C9 9.3(5) . . . . ? C25 Pd1 P1 C1 84.3(3) . . . . ? P2 Pd1 P1 C1 -105.5(5) . . . . ? C25 Pd1 P1 C5 -44.6(3) . . . . ? P2 Pd1 P1 C5 125.6(5) . . . . ? C17 P2 C21 C24 -68.2(6) . . . . ? C13 P2 C21 C24 49.6(6) . . . . ? Pd1 P2 C21 C24 172.9(5) . . . . ? C17 P2 C21 C23 54.5(5) . . . . ? C13 P2 C21 C23 172.3(5) . . . . ? Pd1 P2 C21 C23 -64.3(5) . . . . ? C17 P2 C21 C22 171.9(4) . . . . ? C13 P2 C21 C22 -70.4(5) . . . . ? Pd1 P2 C21 C22 53.0(5) . . . . ? C9 P1 C5 C8 -40.6(5) . . . . ? C1 P1 C5 C8 80.3(5) . . . . ? Pd1 P1 C5 C8 -150.5(4) . . . . ? C9 P1 C5 C7 -162.5(5) . . . . ? C1 P1 C5 C7 -41.6(6) . . . . ? Pd1 P1 C5 C7 87.7(5) . . . . ? C9 P1 C5 C6 80.9(5) . . . . ? C1 P1 C5 C6 -158.2(5) . . . . ? Pd1 P1 C5 C6 -29.0(6) . . . . ? C17 P2 C13 C15 44.4(6) . . . . ? C21 P2 C13 C15 -73.8(6) . . . . ? Pd1 P2 C13 C15 168.4(4) . . . . ? C17 P2 C13 C14 166.1(4) . . . . ? C21 P2 C13 C14 47.9(5) . . . . ? Pd1 P2 C13 C14 -69.9(5) . . . . ? C17 P2 C13 C16 -79.4(5) . . . . ? C21 P2 C13 C16 162.4(5) . . . . ? Pd1 P2 C13 C16 44.5(5) . . . . ? C13 P2 C17 C18 45.7(6) . . . . ? C21 P2 C17 C18 163.3(5) . . . . ? Pd1 P2 C17 C18 -80.7(5) . . . . ? C13 P2 C17 C20 -77.4(6) . . . . ? C21 P2 C17 C20 40.2(6) . . . . ? Pd1 P2 C17 C20 156.2(4) . . . . ? C13 P2 C17 C19 163.1(5) . . . . ? C21 P2 C17 C19 -79.3(5) . . . . ? Pd1 P2 C17 C19 36.7(5) . . . . ? C9 P1 C1 C3 -162.9(4) . . . . ? C5 P1 C1 C3 77.3(5) . . . . ? Pd1 P1 C1 C3 -57.4(4) . . . . ? C9 P1 C1 C4 73.3(5) . . . . ? C5 P1 C1 C4 -46.5(5) . . . . ? Pd1 P1 C1 C4 178.9(4) . . . . ? C9 P1 C1 C2 -48.5(5) . . . . ? C5 P1 C1 C2 -168.3(4) . . . . ? Pd1 P1 C1 C2 57.0(5) . . . . ? C1 P1 C9 C12 -41.3(6) . . . . ? C5 P1 C9 C12 78.9(6) . . . . ? Pd1 P1 C9 C12 -155.8(5) . . . . ? C1 P1 C9 C11 80.7(5) . . . . ? C5 P1 C9 C11 -159.1(5) . . . . ? Pd1 P1 C9 C11 -33.8(5) . . . . ? C1 P1 C9 C10 -167.8(4) . . . . ? C5 P1 C9 C10 -47.7(5) . . . . ? Pd1 P1 C9 C10 77.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 65.64 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.171 _refine_diff_density_min -1.438 _refine_diff_density_rms 0.155 _iucr_refine_instructions_details ; TITL twin5 in P 2/m CELL 1.54185 14.5334 14.2796 15.2101 90.000 92.956 90.000 ZERR 4.00 0.0006 0.0005 0.0005 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, Y, - Z SFAC C H F P PD SB UNIT 100 228 24 8 4 4 MERG 0 ACTA CONF SIZE 0.15 0.10 0.05 BOND BOND $H TEMP -173 FMAP 2 PLAN 25 L.S. 8 WGHT 0.115100 3.232300 BASF 0.47637 FVAR 0.18973 SB01 6 0.250000 -0.227136 1.000000 10.50000 0.02306 0.02059 = 0.02599 0.00000 0.00014 0.00000 SB02 6 0.250000 -0.223192 0.500000 10.50000 0.03581 0.02191 = 0.02869 0.00000 -0.00291 0.00000 PD1 5 0.254634 0.267067 0.747465 11.00000 0.01698 0.01513 = 0.02403 -0.00121 0.00190 0.00030 P2 4 0.382472 0.377148 0.745223 11.00000 0.01808 0.01656 = 0.02026 -0.00074 -0.00117 -0.00266 P1 4 0.144172 0.147198 0.749852 11.00000 0.01501 0.01689 = 0.02347 -0.00058 0.00247 0.00009 F2 3 0.256022 -0.227421 0.877999 11.00000 0.04102 0.05297 = 0.02273 0.00128 -0.00029 0.00231 F5 3 0.292362 -0.223383 0.618039 11.00000 0.06141 0.05773 = 0.02592 -0.00704 -0.00648 0.01238 F4 3 0.162746 -0.316084 0.523563 11.00000 0.03704 0.03256 = 0.05346 0.00083 0.01751 -0.00697 F3 3 0.157981 -0.319378 0.990372 11.00000 0.04302 0.02942 = 0.04753 0.01350 -0.01604 -0.02012 F6 3 0.336802 -0.129923 0.475895 11.00000 0.06774 0.03684 = 0.08196 0.02497 -0.02268 -0.02846 F1 3 0.341737 -0.133545 1.008839 11.00000 0.03106 0.02860 = 0.05341 -0.00686 0.00089 -0.01132 C21 1 0.491726 0.302337 0.745232 11.00000 0.02381 0.02430 = 0.03408 -0.00071 0.00115 0.00220 C5 1 0.055307 0.145461 0.838228 11.00000 0.02475 0.03668 = 0.02603 0.00296 0.01087 -0.00370 C12 1 0.197827 -0.050098 0.743359 11.00000 0.04241 0.02929 = 0.03603 0.00110 -0.00278 0.00669 AFIX 137 H12A 2 0.249032 -0.093882 0.754492 11.00000 -1.50000 H12B 2 0.179589 -0.050116 0.680424 11.00000 -1.50000 H12C 2 0.145422 -0.069448 0.777116 11.00000 -1.50000 AFIX 0 C13 1 0.380591 0.457151 0.644419 11.00000 0.03998 0.02086 = 0.02195 0.00706 0.00039 -0.00686 C17 1 0.386665 0.453517 0.848370 11.00000 0.03440 0.02571 = 0.02996 -0.00741 -0.00190 -0.00330 C1 1 0.083059 0.134173 0.637169 11.00000 0.02742 0.01840 = 0.02716 -0.00156 -0.00065 -0.00662 C19 1 0.359011 0.393430 0.927044 11.00000 0.05546 0.03007 = 0.02593 -0.00561 0.00866 -0.00302 AFIX 137 H19A 2 0.345536 0.434387 0.976456 11.00000 -1.50000 H19B 2 0.409784 0.351204 0.944793 11.00000 -1.50000 H19C 2 0.304142 0.356522 0.909869 11.00000 -1.50000 AFIX 0 C18 1 0.317493 0.533771 0.839447 11.00000 0.05056 0.04209 = 0.03598 -0.01181 -0.00468 0.00608 AFIX 137 H18A 2 0.257054 0.509089 0.819491 11.00000 -1.50000 H18B 2 0.338227 0.579264 0.796471 11.00000 -1.50000 H18C 2 0.312770 0.564504 0.896647 11.00000 -1.50000 AFIX 0 C15 1 0.448215 0.538733 0.649928 11.00000 0.03700 0.04161 = 0.03141 0.01343 -0.00755 -0.01163 AFIX 137 H15A 2 0.448353 0.570268 0.592709 11.00000 -1.50000 H15B 2 0.510186 0.515194 0.665866 11.00000 -1.50000 H15C 2 0.429601 0.583209 0.694754 11.00000 -1.50000 AFIX 0 C11 1 0.314717 0.075700 0.722503 11.00000 0.02754 0.03578 = 0.05142 0.00603 0.01042 0.00401 AFIX 137 H11A 2 0.363925 0.030230 0.736072 11.00000 -1.50000 H11B 2 0.335253 0.138198 0.741532 11.00000 -1.50000 H11C 2 0.299891 0.076172 0.658915 11.00000 -1.50000 AFIX 0 C4 1 0.010090 0.056304 0.629685 11.00000 0.02880 0.03296 = 0.03374 -0.00463 -0.00653 -0.00562 AFIX 137 H4A 2 -0.043080 0.074122 0.663082 11.00000 -1.50000 H4B 2 0.036477 -0.002132 0.653513 11.00000 -1.50000 H4C 2 -0.009659 0.047266 0.567686 11.00000 -1.50000 AFIX 0 C20 1 0.481705 0.495413 0.873762 11.00000 0.05067 0.03508 = 0.02232 -0.00689 -0.00100 -0.01220 AFIX 137 H20A 2 0.506075 0.526499 0.822438 11.00000 -1.50000 H20B 2 0.523830 0.445328 0.893854 11.00000 -1.50000 H20C 2 0.475840 0.541139 0.921192 11.00000 -1.50000 AFIX 0 C23 1 0.500260 0.248482 0.831552 11.00000 0.02963 0.03017 = 0.05496 0.00209 -0.00270 0.01023 AFIX 137 H23A 2 0.553097 0.205898 0.830849 11.00000 -1.50000 H23B 2 0.443908 0.212229 0.838844 11.00000 -1.50000 H23C 2 0.509272 0.292623 0.880577 11.00000 -1.50000 AFIX 0 C2 1 0.154681 0.114969 0.567751 11.00000 0.04856 0.03780 = 0.01989 -0.00779 0.00303 -0.00369 AFIX 137 H2A 2 0.127395 0.128750 0.508909 11.00000 -1.50000 H2B 2 0.173345 0.049051 0.570747 11.00000 -1.50000 H2C 2 0.208735 0.154925 0.579564 11.00000 -1.50000 AFIX 0 C10 1 0.262300 0.046363 0.869946 11.00000 0.03414 0.04480 = 0.03734 0.00687 -0.00342 0.00358 AFIX 137 H10A 2 0.214159 0.019945 0.905335 11.00000 -1.50000 H10B 2 0.276381 0.110314 0.889775 11.00000 -1.50000 H10C 2 0.317949 0.007748 0.876831 11.00000 -1.50000 AFIX 0 C8 1 0.023985 0.046440 0.860955 11.00000 0.02624 0.04563 = 0.02955 0.00683 0.00329 -0.01022 AFIX 137 H8A 2 -0.024461 0.049957 0.903326 11.00000 -1.50000 H8B 2 0.076432 0.011000 0.886770 11.00000 -1.50000 H8C 2 -0.000072 0.014955 0.807323 11.00000 -1.50000 AFIX 0 C16 1 0.281879 0.495488 0.625295 11.00000 0.04108 0.03060 = 0.04834 0.01038 -0.00607 -0.00128 AFIX 137 H16A 2 0.263761 0.533464 0.675209 11.00000 -1.50000 H16B 2 0.238886 0.443046 0.616528 11.00000 -1.50000 H16C 2 0.280539 0.534209 0.572048 11.00000 -1.50000 AFIX 0 C9 1 0.228045 0.048082 0.771409 11.00000 0.02945 0.02785 = 0.03604 0.00382 0.01247 0.00364 C22 1 0.482858 0.229669 0.668956 11.00000 0.02884 0.03247 = 0.03898 -0.00305 0.00682 0.00406 AFIX 137 H22A 2 0.525406 0.246273 0.623513 11.00000 -1.50000 H22B 2 0.419557 0.229872 0.643419 11.00000 -1.50000 H22C 2 0.498030 0.167123 0.691923 11.00000 -1.50000 AFIX 0 C14 1 0.401331 0.398504 0.562859 11.00000 0.05753 0.03496 = 0.02205 0.00084 -0.00090 -0.00595 AFIX 137 H14A 2 0.389561 0.436238 0.509646 11.00000 -1.50000 H14B 2 0.361598 0.343020 0.560222 11.00000 -1.50000 H14C 2 0.466039 0.378917 0.566785 11.00000 -1.50000 AFIX 0 C25 1 0.157912 0.365912 0.768529 11.00000 0.03682 0.01474 = 0.07307 -0.01238 0.00996 0.00721 AFIX 137 H25A 2 0.096510 0.340152 0.753951 11.00000 -1.50000 H25B 2 0.168300 0.420499 0.731269 11.00000 -1.50000 H25C 2 0.162213 0.384824 0.830541 11.00000 -1.50000 AFIX 0 C3 1 0.039109 0.227747 0.610211 11.00000 0.02438 0.03137 = 0.03240 0.00378 -0.00691 -0.00200 AFIX 137 H3A 2 0.005038 0.220768 0.553293 11.00000 -1.50000 H3B 2 0.087360 0.275117 0.605266 11.00000 -1.50000 H3C 2 -0.003259 0.247373 0.654785 11.00000 -1.50000 AFIX 0 C24 1 0.581485 0.353007 0.733068 11.00000 0.02157 0.04166 = 0.05510 -0.00933 0.00407 -0.00129 AFIX 137 H24A 2 0.588813 0.403413 0.776592 11.00000 -1.50000 H24B 2 0.580998 0.379627 0.673660 11.00000 -1.50000 H24C 2 0.632842 0.308835 0.741066 11.00000 -1.50000 AFIX 0 C6 1 0.097871 0.193299 0.922187 11.00000 0.04573 0.04712 = 0.03560 -0.00510 0.01134 -0.00744 AFIX 137 H6A 2 0.051340 0.197638 0.966404 11.00000 -1.50000 H6B 2 0.118958 0.256308 0.907502 11.00000 -1.50000 H6C 2 0.150250 0.156222 0.945780 11.00000 -1.50000 AFIX 0 C7 1 -0.030836 0.202735 0.810583 11.00000 0.02512 0.05984 = 0.04219 -0.00766 0.01325 0.00119 AFIX 137 H7A 2 -0.063315 0.172571 0.760106 11.00000 -1.50000 H7B 2 -0.012503 0.266168 0.794201 11.00000 -1.50000 H7C 2 -0.071657 0.206012 0.859801 11.00000 -1.50000 HKLF 5 REM twin5 in P 2/m REM R1 = 0.0564 for 6987 Fo > 4sig(Fo) and 0.0807 for all 9649 data REM 337 parameters refined using 0 restraints END ;