#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100981.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100981 _chemical_formula_moiety '[C42 H48 F6 N2 O2 Pd]+, (B F4)-' _chemical_formula_sum 'C42 H48 B F10 N2 O2 Pd' _chemical_formula_weight 920.03 _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'C2/c , No.15' 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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' _symmetry_cell_setting 'Monoclinic' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.5769(6) _cell_length_b 13.2251(3) _cell_length_c 30.9126(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.586(5) _cell_angle_gamma 90.00 _cell_volume 8779.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3768 _exptl_absorpt_coefficient_mu 0.501 _exptl_absorpt_correction_type 'not measured' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '553 images at 0.6 deg. in phi, 975 images at 0.6 deg. in \w, 42 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76289 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 28.28 _reflns_number_total 10873 _reflns_number_gt 8927 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+19.7222P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10873 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.009 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.854355(9) 1.602206(14) 1.126752(6) 0.01646(5) Uani 1 d . . . O1 O 0.87299(8) 1.46605(12) 1.10525(6) 0.0202(4) Uani 1 d . . . C1 C 0.93044(11) 1.45786(17) 1.09508(8) 0.0168(5) Uani 1 d . . . C2 C 0.95451(12) 1.36618(18) 1.07900(8) 0.0185(5) Uani 1 d . . . C3 C 1.01447(12) 1.36999(18) 1.06745(8) 0.0198(5) Uani 1 d . . . H3 H 1.0306 1.3109 1.0552 0.024 Uiso 1 calc R . . C4 C 1.05459(11) 1.45749(18) 1.07266(8) 0.0180(5) Uani 1 d . . . C5 C 1.03234(11) 1.54277(18) 1.09039(8) 0.0184(5) Uani 1 d . . . H5 H 1.0586 1.6000 1.0957 0.022 Uiso 1 calc R . . C6 C 0.96994(11) 1.54586(18) 1.10095(8) 0.0174(5) Uani 1 d . . . N7 N 0.94115(9) 1.62745(14) 1.11556(7) 0.0169(4) Uani 1 d . . . C8 C 0.97371(11) 1.71781(18) 1.13001(8) 0.0179(5) Uani 1 d . . . C9 C 0.97163(12) 1.80610(19) 1.10470(9) 0.0231(5) Uani 1 d . . . C10 C 1.00040(13) 1.8931(2) 1.12205(10) 0.0305(6) Uani 1 d . . . H10 H 0.9996 1.9531 1.1051 0.037 Uiso 1 calc R . . C11 C 1.03018(13) 1.8928(2) 1.16380(10) 0.0315(6) Uani 1 d . . . H11 H 1.0491 1.9529 1.1756 0.038 Uiso 1 calc R . . C12 C 1.03243(12) 1.8060(2) 1.18824(10) 0.0285(6) Uani 1 d . . . H12 H 1.0534 1.8061 1.2167 0.034 Uiso 1 calc R . . C13 C 1.00419(12) 1.71777(19) 1.17165(9) 0.0231(6) Uani 1 d . . . H13 H 1.0058 1.6579 1.1887 0.028 Uiso 1 calc R . . C14 C 0.91439(13) 1.26967(19) 1.07579(9) 0.0245(6) Uani 1 d . . . C15 C 0.89364(15) 1.2447(2) 1.12087(10) 0.0322(6) Uani 1 d . . . H15A H 0.9304 1.2373 1.1419 0.048 Uiso 1 calc R . . H15B H 0.8700 1.1813 1.1193 0.048 Uiso 1 calc R . . H15C H 0.8673 1.2994 1.1301 0.048 Uiso 1 calc R . . C16 C 0.95085(16) 1.1784(2) 1.06121(11) 0.0365(7) Uani 1 d . . . H16A H 0.9882 1.1683 1.0814 0.055 Uiso 1 calc R . . H16B H 0.9630 1.1905 1.0319 0.055 Uiso 1 calc R . . H16C H 0.9246 1.1178 1.0610 0.055 Uiso 1 calc R . . C17 C 0.85668(15) 1.2849(2) 1.04312(10) 0.0353(7) Uani 1 d . . . H17A H 0.8699 1.2992 1.0143 0.053 Uiso 1 calc R . . H17B H 0.8321 1.3418 1.0525 0.053 Uiso 1 calc R . . H17C H 0.8313 1.2233 1.0418 0.053 Uiso 1 calc R . . C18 C 1.11911(12) 1.45270(19) 1.05632(8) 0.0209(5) Uani 1 d . . . C19 C 1.11048(14) 1.4583(2) 1.00643(9) 0.0291(6) Uani 1 d . . . H19A H 1.1512 1.4548 0.9950 0.044 Uiso 1 calc R . . H19B H 1.0901 1.5221 0.9974 0.044 Uiso 1 calc R . . H19C H 1.0846 1.4015 0.9950 0.044 Uiso 1 calc R . . C20 C 1.16022(12) 1.5419(2) 1.07328(10) 0.0290(6) Uani 1 d . . . H20A H 1.2015 1.5353 1.0629 0.044 Uiso 1 calc R . . H20B H 1.1644 1.5416 1.1051 0.044 Uiso 1 calc R . . H20C H 1.1410 1.6055 1.0627 0.044 Uiso 1 calc R . . C21 C 1.15314(14) 1.3541(2) 1.07039(11) 0.0354(7) Uani 1 d . . . H21A H 1.1954 1.3557 1.0614 0.053 Uiso 1 calc R . . H21B H 1.1305 1.2964 1.0567 0.053 Uiso 1 calc R . . H21C H 1.1552 1.3474 1.1021 0.053 Uiso 1 calc R . . C22 C 0.94153(16) 1.8068(2) 1.05932(10) 0.0339(7) Uani 1 d . . . F23 F 0.94060(12) 1.89938(14) 1.04153(6) 0.0603(6) Uani 1 d . . . F24 F 0.88232(8) 1.77404(14) 1.05539(6) 0.0389(4) Uani 1 d . . . F25 F 0.97225(10) 1.74746(15) 1.03304(6) 0.0465(5) Uani 1 d . . . O31 O 0.83599(8) 1.74006(12) 1.14857(6) 0.0191(4) Uani 1 d . . . C31 C 0.78344(11) 1.74987(18) 1.16224(8) 0.0171(5) Uani 1 d . . . C32 C 0.76266(11) 1.84365(17) 1.18039(8) 0.0167(5) Uani 1 d . . . C33 C 0.70556(11) 1.84133(18) 1.19473(8) 0.0175(5) Uani 1 d . . . H33 H 0.6914 1.9013 1.2075 0.021 Uiso 1 calc R . . C34 C 0.66332(11) 1.75306(18) 1.19209(8) 0.0176(5) Uani 1 d . . . C35 C 0.68188(11) 1.66561(19) 1.17461(8) 0.0191(5) Uani 1 d . . . H35 H 0.6551 1.6084 1.1728 0.023 Uiso 1 calc R . . C36 C 0.74167(11) 1.65982(18) 1.15892(8) 0.0179(5) Uani 1 d . . . N37 N 0.76609(9) 1.58146(14) 1.14058(7) 0.0172(4) Uani 1 d . . . C38 C 0.73432(11) 1.48523(18) 1.13747(8) 0.0182(5) Uani 1 d . . . C39 C 0.70020(12) 1.45347(19) 1.09921(9) 0.0237(6) Uani 1 d . . . C40 C 0.67240(14) 1.3578(2) 1.09826(10) 0.0311(7) Uani 1 d . . . H40 H 0.6489 1.3353 1.0725 0.037 Uiso 1 calc R . . C41 C 0.67872(14) 1.2958(2) 1.13418(10) 0.0313(7) Uani 1 d . . . H41 H 0.6595 1.2311 1.1331 0.038 Uiso 1 calc R . . C42 C 0.71295(14) 1.3277(2) 1.17180(10) 0.0294(6) Uani 1 d . . . H42 H 0.7173 1.2849 1.1966 0.035 Uiso 1 calc R . . C43 C 0.74110(13) 1.42236(19) 1.17335(9) 0.0251(6) Uani 1 d . . . H43 H 0.7650 1.4439 1.1991 0.030 Uiso 1 calc R . . C44 C 0.80665(11) 1.93518(18) 1.18294(9) 0.0197(5) Uani 1 d . . . C45 C 0.82525(13) 1.9617(2) 1.13750(9) 0.0267(6) Uani 1 d . . . H45A H 0.8470 1.9042 1.1259 0.040 Uiso 1 calc R . . H45B H 0.8528 2.0208 1.1395 0.040 Uiso 1 calc R . . H45C H 0.7878 1.9770 1.1181 0.040 Uiso 1 calc R . . C46 C 0.86534(12) 1.9110(2) 1.21385(9) 0.0262(6) Uani 1 d . . . H46A H 0.8863 1.8517 1.2030 0.039 Uiso 1 calc R . . H46B H 0.8533 1.8967 1.2430 0.039 Uiso 1 calc R . . H46C H 0.8937 1.9691 1.2151 0.039 Uiso 1 calc R . . C47 C 0.77500(12) 2.02810(19) 1.20066(10) 0.0263(6) Uani 1 d . . . H47A H 0.7648 2.0143 1.2303 0.039 Uiso 1 calc R . . H47B H 0.7367 2.0433 1.1820 0.039 Uiso 1 calc R . . H47C H 0.8033 2.0862 1.2010 0.039 Uiso 1 calc R . . C48 C 0.60027(11) 1.76581(18) 1.20980(8) 0.0182(5) Uani 1 d . . . C49 C 0.56516(12) 1.8562(2) 1.18731(9) 0.0246(6) Uani 1 d . . . H49A H 0.5247 1.8639 1.1988 0.037 Uiso 1 calc R . . H49B H 0.5588 1.8439 1.1559 0.037 Uiso 1 calc R . . H49C H 0.5897 1.9180 1.1929 0.037 Uiso 1 calc R . . C50 C 0.61083(12) 1.7847(2) 1.25907(8) 0.0228(5) Uani 1 d . . . H50A H 0.5705 1.7929 1.2708 0.034 Uiso 1 calc R . . H50B H 0.6357 1.8462 1.2646 0.034 Uiso 1 calc R . . H50C H 0.6330 1.7270 1.2732 0.034 Uiso 1 calc R . . C51 C 0.56004(12) 1.67041(19) 1.20173(9) 0.0235(6) Uani 1 d . . . H51A H 0.5196 1.6810 1.2129 0.035 Uiso 1 calc R . . H51B H 0.5811 1.6128 1.2167 0.035 Uiso 1 calc R . . H51C H 0.5538 1.6567 1.1705 0.035 Uiso 1 calc R . . C52 C 0.69129(16) 1.5211(2) 1.06018(10) 0.0376(7) Uani 1 d . . . F53 F 0.65912(13) 1.60310(16) 1.06804(7) 0.0724(7) Uani 1 d . . . F54 F 0.66042(11) 1.47640(15) 1.02624(6) 0.0595(6) Uani 1 d . . . F55 F 0.74460(11) 1.5536(2) 1.04721(7) 0.0730(8) Uani 1 d . . . B60 B 0.63959(14) 0.8833(2) 0.74469(10) 0.0232(6) Uani 1 d . . . F61 F 0.65324(8) 0.97835(12) 0.76269(6) 0.0352(4) Uani 1 d . . . F62 F 0.58787(8) 0.84406(14) 0.76166(6) 0.0383(4) Uani 1 d . . . F63 F 0.69102(8) 0.82012(12) 0.75559(5) 0.0318(4) Uani 1 d . . . F64 F 0.62969(7) 0.89196(13) 0.69971(5) 0.0319(4) Uani 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 Pd1 0.01739(9) 0.01081(8) 0.02177(10) -0.00314(8) 0.00498(6) -0.00234(8) O1 0.0224(9) 0.0125(8) 0.0265(10) -0.0046(7) 0.0070(7) -0.0020(7) C1 0.0231(12) 0.0122(11) 0.0149(12) 0.0006(9) 0.0010(10) 0.0008(9) C2 0.0296(14) 0.0120(11) 0.0137(12) 0.0008(9) 0.0012(10) -0.0014(10) C3 0.0295(14) 0.0132(11) 0.0170(12) -0.0019(9) 0.0030(10) 0.0041(10) C4 0.0222(12) 0.0178(12) 0.0141(12) 0.0033(9) 0.0014(9) 0.0045(10) C5 0.0205(12) 0.0151(12) 0.0194(13) -0.0005(10) 0.0018(10) -0.0009(9) C6 0.0228(13) 0.0122(11) 0.0173(12) 0.0002(9) 0.0027(10) 0.0002(9) N7 0.0177(10) 0.0105(9) 0.0228(11) -0.0031(8) 0.0042(8) -0.0020(8) C8 0.0162(12) 0.0131(11) 0.0255(13) -0.0041(10) 0.0073(10) -0.0018(9) C9 0.0261(13) 0.0162(12) 0.0279(14) -0.0004(11) 0.0071(11) -0.0018(10) C10 0.0364(15) 0.0140(12) 0.0419(17) 0.0011(13) 0.0081(13) -0.0060(12) C11 0.0286(14) 0.0174(13) 0.0477(18) -0.0095(13) -0.0004(12) -0.0048(12) C12 0.0226(13) 0.0274(14) 0.0339(16) -0.0067(12) -0.0055(12) 0.0000(11) C13 0.0210(13) 0.0181(12) 0.0301(15) -0.0011(11) 0.0020(11) 0.0007(10) C14 0.0349(15) 0.0120(12) 0.0270(15) -0.0010(10) 0.0042(12) -0.0029(10) C15 0.0476(18) 0.0169(13) 0.0336(16) 0.0007(11) 0.0114(13) -0.0045(12) C16 0.052(2) 0.0151(13) 0.0447(19) -0.0065(13) 0.0149(15) -0.0029(13) C17 0.0459(18) 0.0210(14) 0.0376(18) -0.0053(13) -0.0027(14) -0.0106(13) C18 0.0230(13) 0.0192(13) 0.0207(13) 0.0004(10) 0.0040(10) 0.0050(10) C19 0.0335(15) 0.0325(16) 0.0222(14) -0.0010(12) 0.0079(12) -0.0018(12) C20 0.0201(13) 0.0340(16) 0.0331(16) -0.0092(13) 0.0034(11) 0.0001(12) C21 0.0333(16) 0.0285(15) 0.0460(19) 0.0088(14) 0.0118(14) 0.0142(13) C22 0.055(2) 0.0189(14) 0.0284(16) 0.0028(12) 0.0060(14) -0.0055(13) F23 0.1083(18) 0.0285(10) 0.0405(11) 0.0168(9) -0.0106(11) -0.0148(11) F24 0.0429(11) 0.0407(10) 0.0312(10) 0.0041(8) -0.0069(8) -0.0051(8) F25 0.0662(13) 0.0461(11) 0.0294(10) -0.0074(9) 0.0165(9) -0.0110(10) O31 0.0183(9) 0.0127(8) 0.0270(10) -0.0028(7) 0.0062(7) -0.0017(7) C31 0.0186(12) 0.0148(11) 0.0181(12) 0.0007(10) 0.0025(10) -0.0015(9) C32 0.0184(12) 0.0114(11) 0.0200(13) 0.0004(9) 0.0012(9) 0.0002(9) C33 0.0205(12) 0.0120(11) 0.0197(13) -0.0018(9) 0.0008(10) -0.0006(9) C34 0.0188(12) 0.0175(12) 0.0163(12) 0.0012(10) 0.0002(9) -0.0014(9) C35 0.0186(12) 0.0178(12) 0.0211(13) -0.0007(10) 0.0025(10) -0.0039(9) C36 0.0198(12) 0.0143(11) 0.0196(13) -0.0008(10) 0.0014(10) -0.0006(9) N37 0.0198(10) 0.0105(10) 0.0215(11) -0.0016(8) 0.0025(8) -0.0027(8) C38 0.0179(12) 0.0120(11) 0.0258(13) -0.0040(10) 0.0076(10) -0.0015(9) C39 0.0239(13) 0.0188(13) 0.0281(15) -0.0030(11) 0.0011(11) -0.0026(10) C40 0.0330(16) 0.0245(14) 0.0347(17) -0.0101(13) -0.0023(13) -0.0093(12) C41 0.0336(16) 0.0161(13) 0.0454(18) -0.0046(12) 0.0100(13) -0.0092(11) C42 0.0359(16) 0.0190(13) 0.0343(16) 0.0025(12) 0.0092(13) -0.0036(12) C43 0.0299(14) 0.0209(14) 0.0246(14) -0.0017(11) 0.0028(11) -0.0033(11) C44 0.0195(12) 0.0113(11) 0.0281(14) -0.0012(10) 0.0013(10) -0.0016(9) C45 0.0272(14) 0.0184(13) 0.0355(16) 0.0047(12) 0.0082(12) -0.0008(11) C46 0.0219(13) 0.0191(13) 0.0368(16) -0.0040(12) -0.0022(11) -0.0023(10) C47 0.0229(13) 0.0125(12) 0.0438(17) -0.0069(12) 0.0042(12) -0.0013(10) C48 0.0165(12) 0.0159(12) 0.0227(13) 0.0002(10) 0.0049(10) -0.0008(9) C49 0.0207(13) 0.0230(13) 0.0300(15) 0.0041(11) 0.0020(11) 0.0011(11) C50 0.0260(14) 0.0204(13) 0.0227(14) 0.0000(10) 0.0059(11) 0.0012(10) C51 0.0193(12) 0.0191(13) 0.0331(15) -0.0040(11) 0.0080(11) -0.0029(10) C52 0.049(2) 0.0304(16) 0.0313(17) -0.0015(13) -0.0081(14) -0.0101(14) F53 0.122(2) 0.0354(11) 0.0558(14) 0.0081(11) -0.0125(13) 0.0267(13) F54 0.0872(17) 0.0476(12) 0.0371(11) 0.0006(10) -0.0273(11) -0.0155(11) F55 0.0657(15) 0.108(2) 0.0429(13) 0.0351(13) -0.0051(11) -0.0366(14) B60 0.0248(14) 0.0174(14) 0.0276(16) 0.0001(12) 0.0033(12) -0.0042(11) F61 0.0405(10) 0.0185(8) 0.0455(11) -0.0052(7) -0.0010(8) -0.0026(7) F62 0.0348(10) 0.0417(10) 0.0401(10) 0.0000(8) 0.0122(8) -0.0134(8) F63 0.0392(10) 0.0259(9) 0.0303(9) 0.0050(7) 0.0039(7) 0.0079(7) F64 0.0288(8) 0.0382(9) 0.0280(8) 0.0048(8) -0.0016(7) -0.0062(8)