#------------------------------------------------------------------------------ #$Date: 2014-10-05 13:32:10 +0300 (Sun, 05 Oct 2014) $ #$Revision: 124581 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/51/75/1517542.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_1517542 loop_ _publ_author_name 'Suh, Hee-Won' 'Guard, Louise M.' 'Hazari, Nilay' _publ_section_title ; A mechanistic study of allene carboxylation with CO2resulting in the development of a Pd(ii) pincer complex for the catalytic hydroboration of CO2 ; _journal_issue 10 _journal_name_full 'Chemical Science' _journal_page_first 3859 _journal_paper_doi 10.1039/C4SC01110D _journal_volume 5 _journal_year 2014 _chemical_formula_moiety 'C42 H64 P2 Pd Si, C5 H12' _chemical_formula_sum 'C47 H76 P2 Pd Si' _chemical_formula_weight 837.51 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _audit_creation_date 2013-04-16 _audit_creation_method ; Olex2 1.2 (compiled Apr 9 2013 14:10:59, GUI svn.r4458) ; _cell_angle_alpha 90.00 _cell_angle_beta 102.802(7) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 16.1665(11) _cell_length_b 10.3002(7) _cell_length_c 27.3994(19) _cell_measurement_reflns_used 21810 _cell_measurement_temperature 150 _cell_measurement_theta_max 23.8 _cell_measurement_theta_min 3.0 _cell_volume 4449.1(5) _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011) ; _computing_data_collection ; CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _diffrn_ambient_temperature 150 _diffrn_detector 'Image Plate' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'Rigaku IP' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details ; scan: Number of images: 90 Slice: 20.0000 - 200.0000 Image width: 2.0000 Exp time: 70.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 0.0000 Phi: 0.0000 XTD: 127.4000 2theta: -0.0057 scan: Number of images: 90 Slice: 20.0000 - 200.0000 Image width: 2.0000 Exp time: 70.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 54.0000 Phi: 120.0000 XTD: 127.4000 2theta: -0.0057 scan: Number of images: 90 Slice: 20.0000 - 200.0000 Image width: 2.0000 Exp time: 70.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 0.0000 Phi: 180.0000 XTD: 127.4000 2theta: -0.0057 scan: Number of images: 90 Slice: 20.0000 - 200.0000 Image width: 2.0000 Exp time: 70.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 54.0000 Phi: 0.0000 XTD: 127.4000 2theta: -0.0057 scan: Number of images: 90 Slice: 20.0000 - 200.0000 Image width: 2.0000 Exp time: 70.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 54.0000 Phi: 240.0000 XTD: 127.4000 2theta: -0.0057 scan: Number of images: 90 Slice: 20.0000 - 200.0000 Image width: 2.0000 Exp time: 70.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 54.0000 Phi: 90.0000 XTD: 127.4000 2theta: -0.0057 scan: Number of images: 90 Slice: 20.0000 - 200.0000 Image width: 2.0000 Exp time: 70.0000 Rotation axis: Omega Omega: 0.0000 Kappa: 54.0000 Phi: 180.0000 XTD: 127.4000 2theta: -0.0057 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IP' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support Unknown _diffrn_orient_matrix_type FS_PROCESS _diffrn_orient_matrix_UB_11 0.010187 _diffrn_orient_matrix_UB_12 -0.083158 _diffrn_orient_matrix_UB_13 -0.016569 _diffrn_orient_matrix_UB_21 0.057330 _diffrn_orient_matrix_UB_22 -0.007000 _diffrn_orient_matrix_UB_23 0.022892 _diffrn_orient_matrix_UB_31 -0.025164 _diffrn_orient_matrix_UB_32 -0.049613 _diffrn_orient_matrix_UB_33 0.024541 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_reflns_av_R_equivalents 0.1570 _diffrn_reflns_av_unetI/netI 0.1017 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 37324 _diffrn_reflns_theta_full 23.82 _diffrn_reflns_theta_max 23.82 _diffrn_reflns_theta_min 3.02 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40.0 _diffrn_source_power 2.0 _diffrn_source_target Mo _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 0.546 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R (1998) Private Communication' _exptl_crystal_colour Colorless _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 1792 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.645 _refine_diff_density_min -1.200 _refine_diff_density_rms 0.105 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 495 _refine_ls_number_reflns 6808 _refine_ls_number_restraints 80 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.1038 _refine_ls_R_factor_gt 0.0628 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+1.3362P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1269 _refine_ls_wR_factor_ref 0.1453 _reflns_number_gt 4558 _reflns_number_total 6808 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c4sc01110d2.cif _[local]_cod_data_source_block s12103 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius ; _cod_database_code 1517542 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C44-C45 \\sim C45-C46 with sigma of 0.02 C45-C46 \\sim C46-C47 with sigma of 0.02 C45-C44 \\sim C44-C43 with sigma of 0.02 C43A-C44A \\sim C44A-C45A with sigma of 0.02 C44A-C45A \\sim C45A-C46A with sigma of 0.02 C45A-C46A \\sim C46A-C47A with sigma of 0.02 3. Rigid bond restraints C43, C44, C45, C46, C47 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C43A, C44A, C45A, C46A, C47A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C43, C46, C44, C47, C45 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 C47A \\sim C46A \\sim C45A \\sim C44A \\sim C43A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 C43 \\sim C46 \\sim C44 \\sim C47 \\sim C45: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C43A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C43A) = Uanis(C44A) = Uanis(C45A) Uanis(C47) = Uanis(C46) 5. Others 1-1*Sof(C43)=1-1*Sof(H43D)=1-1*Sof(H43E)=1-1*Sof(H43F)=1-1*Sof(C46)=1-1* Sof(H46C)=1-1*Sof(H46D)=1-1*Sof(C44)=1-1*Sof(H44C)=1-1*Sof(H44D)=1-1*Sof(C47)= 1-1*Sof(H47D)=1-1*Sof(H47E)=1-1*Sof(H47F)=1-1*Sof(C45)=1-1*Sof(H45C)=1-1* Sof(H45D)=1*Sof(C44A)=1*Sof(H44A)=1*Sof(H44B)=1*Sof(C47A)=1*Sof(H47A)=1* Sof(H47B)=1*Sof(H47C)=1*Sof(C46A)=1*Sof(H46A)=1*Sof(H46B)=1*Sof(C43A)=1* Sof(H43A)=1*Sof(H43B)=1*Sof(H43C)=1*Sof(C45A)=1*Sof(H45A)=1*Sof(H45B) 6.a Ternary CH refined with riding coordinates: C12(H12), C6(H6), C37(H37), C31(H31) 6.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C7(H7A,H7B), C17(H17A,H17B), C11(H11A,H11B), C14(H14A,H14B), C38(H38A,H38B), C13(H13A,H13B), C32(H32A,H32B), C39(H39A,H39B), C42(H42A,H42B), C9(H9A,H9B), C10(H10A,H10B), C8(H8A,H8B), C41(H41A,H41B), C34(H34A,H34B), C36(H36A,H36B), C33(H33A,H33B), C35(H35A,H35B), C15(H15A,H15B), C16(H16A,H16B), C40(H40A,H40B), C46(H46C,H46D), C44(H44C,H44D), C45(H45C,H45D), C44A(H44A, H44B), C46A(H46A,H46B), C45A(H45A,H45B) 6.c Aromatic/amide H refined with riding coordinates: C21(H21), C19(H19), C29(H29), C28(H28), C26(H26), C22(H22), C27(H27), C2(H2), C20(H20) 6.d Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C43(H43D,H43E,H43F), C47(H47D,H47E,H47F), C47A(H47A,H47B,H47C), C43A(H43A,H43B,H43C) ; loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' 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 Pd1 Pd 0.25261(3) 0.45664(4) 0.857904(18) 0.02706(17) Uani 1 1 d . . . P2 P 0.25716(10) 0.47608(16) 0.77591(6) 0.0296(4) Uani 1 1 d . . . Si2 Si 0.28736(11) 0.67645(16) 0.86062(7) 0.0294(4) Uani 1 1 d . . . P1 P 0.20378(10) 0.50654(15) 0.92856(6) 0.0288(4) Uani 1 1 d . . . C1 C 0.2457(4) 0.2421(6) 0.8581(2) 0.0374(16) Uani 1 1 d . . . H1A H 0.1881 0.2128 0.8567 0.045 Uiso 1 1 calc R . . H1B H 0.2653 0.2056 0.8301 0.045 Uiso 1 1 calc R . . C12 C 0.0991(3) 0.4393(5) 0.9306(2) 0.0276(15) Uani 1 1 d . . . H12 H 0.0798 0.4828 0.9579 0.033 Uiso 1 1 calc R . . C6 C 0.2712(4) 0.4676(6) 0.9904(2) 0.0308(15) Uani 1 1 d . . . H6 H 0.2801 0.3735 0.9907 0.037 Uiso 1 1 calc R . . C18 C 0.1817(4) 0.6813(6) 0.9297(2) 0.0288(15) Uani 1 1 d . . . C7 C 0.3593(4) 0.5295(7) 0.9956(3) 0.0458(18) Uani 1 1 d . . . H7A H 0.3831 0.5031 0.9676 0.055 Uiso 1 1 calc R . . H7B H 0.3537 0.6233 0.9947 0.055 Uiso 1 1 calc R . . C17 C 0.0349(4) 0.4686(6) 0.8822(3) 0.0418(18) Uani 1 1 d . . . H17A H 0.0532 0.4278 0.8545 0.050 Uiso 1 1 calc R . . H17B H 0.0328 0.5616 0.8765 0.050 Uiso 1 1 calc R . . C11 C 0.2356(4) 0.4989(7) 1.0365(2) 0.0396(17) Uani 1 1 d . . . H11A H 0.1813 0.4562 1.0335 0.047 Uiso 1 1 calc R . . H11B H 0.2266 0.5918 1.0381 0.047 Uiso 1 1 calc R . . C21 C 0.1505(5) 0.9469(7) 0.9271(3) 0.051(2) Uani 1 1 d . . . H21 H 0.1401 1.0357 0.9261 0.061 Uiso 1 1 calc R . . C14 C 0.0121(4) 0.2445(6) 0.9429(3) 0.0414(18) Uani 1 1 d . . . H14A H -0.0053 0.2841 0.9711 0.050 Uiso 1 1 calc R . . H14B H 0.0142 0.1512 0.9480 0.050 Uiso 1 1 calc R . . C38 C 0.0838(4) 0.5066(7) 0.7393(3) 0.0426(18) Uani 1 1 d . . . H38A H 0.0950 0.5966 0.7326 0.051 Uiso 1 1 calc R . . H38B H 0.0781 0.5008 0.7737 0.051 Uiso 1 1 calc R . . C13 C 0.0996(4) 0.2932(6) 0.9406(2) 0.0357(16) Uani 1 1 d . . . H13A H 0.1191 0.2478 0.9143 0.043 Uiso 1 1 calc R . . H13B H 0.1389 0.2745 0.9721 0.043 Uiso 1 1 calc R . . C37 C 0.1587(4) 0.4235(6) 0.7328(2) 0.0309(15) Uani 1 1 d . . . H37 H 0.1660 0.4365 0.6986 0.037 Uiso 1 1 calc R . . C19 C 0.1301(4) 0.7360(6) 0.9587(2) 0.0380(17) Uani 1 1 d . . . H19 H 0.1068 0.6829 0.9796 0.046 Uiso 1 1 calc R . . C25 C 0.2693(4) 0.7402(6) 0.7940(2) 0.0313(15) Uani 1 1 d . . . C23 C 0.2191(4) 0.7601(6) 0.8988(2) 0.0281(15) Uani 1 1 d . . . C29 C 0.2558(4) 0.6837(6) 0.7067(2) 0.0336(16) Uani 1 1 d . . . H29 H 0.2502 0.6207 0.6819 0.040 Uiso 1 1 calc R . . C32 C 0.4296(4) 0.4414(7) 0.7858(3) 0.0454(19) Uani 1 1 d . . . H32A H 0.4303 0.4400 0.8213 0.054 Uiso 1 1 calc R . . H32B H 0.4360 0.5309 0.7762 0.054 Uiso 1 1 calc R . . C28 C 0.2571(4) 0.8133(6) 0.6943(2) 0.0372(17) Uani 1 1 d . . . H28 H 0.2537 0.8376 0.6612 0.045 Uiso 1 1 calc R . . C39 C 0.0006(4) 0.4645(7) 0.7045(3) 0.053(2) Uani 1 1 d . . . H39A H -0.0456 0.5169 0.7111 0.063 Uiso 1 1 calc R . . H39B H 0.0040 0.4789 0.6700 0.063 Uiso 1 1 calc R . . C24 C 0.3991(4) 0.7276(6) 0.8887(2) 0.0384(17) Uani 1 1 d . . . H24A H 0.4120 0.7095 0.9239 0.058 Uiso 1 1 calc R . . H24B H 0.4051 0.8189 0.8835 0.058 Uiso 1 1 calc R . . H24C H 0.4375 0.6804 0.8730 0.058 Uiso 1 1 calc R . . C42 C 0.1393(4) 0.2800(6) 0.7386(3) 0.0420(18) Uani 1 1 d . . . H42A H 0.1362 0.2631 0.7730 0.050 Uiso 1 1 calc R . . H42B H 0.1851 0.2280 0.7312 0.050 Uiso 1 1 calc R . . C26 C 0.2702(4) 0.8714(6) 0.7805(3) 0.0397(17) Uani 1 1 d . . . H26 H 0.2754 0.9351 0.8051 0.048 Uiso 1 1 calc R . . C30 C 0.2629(4) 0.6464(6) 0.7568(2) 0.0320(16) Uani 1 1 d . . . C22 C 0.2036(4) 0.8939(6) 0.8989(3) 0.0410(17) Uani 1 1 d . . . H22 H 0.2293 0.9483 0.8796 0.049 Uiso 1 1 calc R . . C31 C 0.3445(4) 0.3893(7) 0.7566(2) 0.0385(17) Uani 1 1 d . . . H31 H 0.3415 0.3000 0.7684 0.046 Uiso 1 1 calc R . . C9 C 0.3827(5) 0.5159(7) 1.0895(3) 0.055(2) Uani 1 1 d . . . H9A H 0.3777 0.6090 1.0935 0.066 Uiso 1 1 calc R . . H9B H 0.4212 0.4827 1.1191 0.066 Uiso 1 1 calc R . . C27 C 0.2636(4) 0.9073(7) 0.7312(3) 0.0426(18) Uani 1 1 d . . . H27 H 0.2634 0.9947 0.7227 0.051 Uiso 1 1 calc R . . C10 C 0.2966(4) 0.4539(7) 1.0847(2) 0.0477(19) Uani 1 1 d . . . H10A H 0.2737 0.4773 1.1134 0.057 Uiso 1 1 calc R . . H10B H 0.3022 0.3602 1.0843 0.057 Uiso 1 1 calc R . . C3 C 0.3823(4) 0.1756(7) 0.9168(3) 0.0473(19) Uani 1 1 d . . . C2 C 0.3008(4) 0.2068(6) 0.9047(3) 0.0413(18) Uani 1 1 d . . . H2 H 0.2743 0.2056 0.9316 0.050 Uiso 1 1 calc R . . C8 C 0.4187(4) 0.4890(8) 1.0443(3) 0.055(2) Uani 1 1 d . . . H8A H 0.4305 0.3969 1.0429 0.066 Uiso 1 1 calc R . . H8B H 0.4720 0.5352 1.0477 0.066 Uiso 1 1 calc R . . C20 C 0.1128(4) 0.8673(7) 0.9571(3) 0.0476(19) Uani 1 1 d . . . H20 H 0.0765 0.9021 0.9757 0.057 Uiso 1 1 calc R . . C41 C 0.0551(4) 0.2393(7) 0.7035(3) 0.057(2) Uani 1 1 d . . . H41A H 0.0600 0.2474 0.6690 0.068 Uiso 1 1 calc R . . H41B H 0.0434 0.1491 0.7095 0.068 Uiso 1 1 calc R . . C34 C 0.5025(4) 0.3473(9) 0.7226(3) 0.063(2) Uani 1 1 d . . . H34A H 0.5480 0.2901 0.7183 0.076 Uiso 1 1 calc R . . H34B H 0.5120 0.4315 0.7090 0.076 Uiso 1 1 calc R . . C36 C 0.3443(4) 0.3772(8) 0.7025(3) 0.061(2) Uani 1 1 d . . . H36A H 0.3483 0.4630 0.6886 0.073 Uiso 1 1 calc R . . H36B H 0.2913 0.3385 0.6851 0.073 Uiso 1 1 calc R . . C33 C 0.5047(4) 0.3609(9) 0.7761(3) 0.065(2) Uani 1 1 d . . . H33A H 0.5574 0.4023 0.7925 0.078 Uiso 1 1 calc R . . H33B H 0.5033 0.2753 0.7907 0.078 Uiso 1 1 calc R . . C35 C 0.4188(4) 0.2934(8) 0.6942(3) 0.063(2) Uani 1 1 d . . . H35A H 0.4121 0.2053 0.7052 0.075 Uiso 1 1 calc R . . H35B H 0.4185 0.2907 0.6588 0.075 Uiso 1 1 calc R . . C15 C -0.0527(4) 0.2761(7) 0.8950(3) 0.055(2) Uani 1 1 d . . . H15A H -0.0389 0.2284 0.8673 0.066 Uiso 1 1 calc R . . H15B H -0.1086 0.2489 0.8985 0.066 Uiso 1 1 calc R . . C4 C 0.4347(5) 0.1641(8) 0.8778(3) 0.068(3) Uani 1 1 d . . . H4A H 0.3981 0.1682 0.8451 0.103 Uiso 1 1 calc R . . H4B H 0.4644 0.0828 0.8818 0.103 Uiso 1 1 calc R . . H4C H 0.4748 0.2341 0.8818 0.103 Uiso 1 1 calc R . . C16 C -0.0539(4) 0.4198(7) 0.8838(3) 0.058(2) Uani 1 1 d . . . H16A H -0.0746 0.4668 0.9094 0.070 Uiso 1 1 calc R . . H16B H -0.0923 0.4364 0.8519 0.070 Uiso 1 1 calc R . . C40 C -0.0175(4) 0.3230(8) 0.7119(3) 0.067(3) Uani 1 1 d . . . H40A H -0.0694 0.2979 0.6885 0.080 Uiso 1 1 calc R . . H40B H -0.0255 0.3096 0.7456 0.080 Uiso 1 1 calc R . . C5 C 0.4288(5) 0.1471(9) 0.9690(3) 0.084(3) Uani 1 1 d . . . H5A H 0.4753 0.2066 0.9785 0.126 Uiso 1 1 calc R . . H5B H 0.4501 0.0598 0.9708 0.126 Uiso 1 1 calc R . . H5C H 0.3910 0.1565 0.9912 0.126 Uiso 1 1 calc R . . C43 C 0.1274(11) 1.2103(16) 1.0841(6) 0.067(5) Uani 0.515(12) 1 d PDU A 1 H43D H 0.1536 1.2233 1.1188 0.100 Uiso 0.515(12) 1 calc PR A 1 H43E H 0.0700 1.2412 1.0776 0.100 Uiso 0.515(12) 1 calc PR A 1 H43F H 0.1585 1.2571 1.0637 0.100 Uiso 0.515(12) 1 calc PR A 1 C46 C 0.2419(13) 0.9740(16) 1.0888(7) 0.071(4) Uani 0.515(12) 1 d PDU A 1 H46C H 0.1945 0.9156 1.0879 0.085 Uiso 0.515(12) 1 calc PR A 1 H46D H 0.2647 0.9965 1.1235 0.085 Uiso 0.515(12) 1 calc PR A 1 C44 C 0.1277(15) 1.0760(19) 1.0727(10) 0.088(7) Uani 0.515(12) 1 d PDU A 1 H44C H 0.0849 1.0519 1.0433 0.105 Uiso 0.515(12) 1 calc PR A 1 H44D H 0.1245 1.0204 1.1007 0.105 Uiso 0.515(12) 1 calc PR A 1 C47 C 0.3056(12) 0.9057(18) 1.0707(7) 0.071(4) Uani 0.515(12) 1 d PDU A 1 H47D H 0.3260 0.9591 1.0471 0.106 Uiso 0.515(12) 1 calc PR A 1 H47E H 0.2819 0.8272 1.0545 0.106 Uiso 0.515(12) 1 calc PR A 1 H47F H 0.3517 0.8847 1.0982 0.106 Uiso 0.515(12) 1 calc PR A 1 C45 C 0.2116(12) 1.0850(16) 1.0634(7) 0.069(5) Uani 0.515(12) 1 d PDU A 1 H45C H 0.2118 1.0802 1.0281 0.083 Uiso 0.515(12) 1 calc PR A 1 H45D H 0.2416 1.1621 1.0781 0.083 Uiso 0.515(12) 1 calc PR A 1 C44A C 0.1956(11) 1.009(2) 1.0922(7) 0.068(4) Uani 0.485(12) 1 d PDU A 2 H44A H 0.2201 1.0015 1.1278 0.082 Uiso 0.485(12) 1 calc PR A 2 H44B H 0.1669 0.9285 1.0809 0.082 Uiso 0.485(12) 1 calc PR A 2 C47A C 0.3355(11) 0.8955(17) 1.0363(7) 0.073(6) Uani 0.485(12) 1 d PDU A 2 H47A H 0.3316 0.9598 1.0106 0.110 Uiso 0.485(12) 1 calc PR A 2 H47B H 0.2871 0.8392 1.0284 0.110 Uiso 0.485(12) 1 calc PR A 2 H47C H 0.3863 0.8455 1.0386 0.110 Uiso 0.485(12) 1 calc PR A 2 C46A C 0.3378(13) 0.958(3) 1.0829(9) 0.114(9) Uani 0.485(12) 1 d PDU A 2 H46A H 0.3871 1.0133 1.0932 0.137 Uiso 0.485(12) 1 calc PR A 2 H46B H 0.3346 0.8967 1.1094 0.137 Uiso 0.485(12) 1 calc PR A 2 C43A C 0.1337(16) 1.117(2) 1.0836(10) 0.068(4) Uani 0.485(12) 1 d PDU A 2 H43A H 0.1206 1.1394 1.0487 0.102 Uiso 0.485(12) 1 calc PR A 2 H43B H 0.1575 1.1909 1.1030 0.102 Uiso 0.485(12) 1 calc PR A 2 H43C H 0.0829 1.0903 1.0934 0.102 Uiso 0.485(12) 1 calc PR A 2 C45A C 0.2600(10) 1.031(2) 1.0666(7) 0.068(4) Uani 0.485(12) 1 d PDU A 2 H45A H 0.2742 1.1227 1.0692 0.082 Uiso 0.485(12) 1 calc PR A 2 H45B H 0.2376 1.0123 1.0315 0.082 Uiso 0.485(12) 1 calc PR A 2 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 0.0232(3) 0.0252(3) 0.0321(3) -0.0001(2) 0.0045(2) 0.0010(2) P2 0.0228(9) 0.0297(9) 0.0358(10) -0.0029(8) 0.0053(7) -0.0006(7) Si2 0.0252(9) 0.0276(9) 0.0349(11) -0.0013(8) 0.0059(8) -0.0010(8) P1 0.0253(9) 0.0257(9) 0.0348(10) 0.0017(7) 0.0052(8) 0.0022(7) C1 0.049(4) 0.038(4) 0.027(4) -0.001(3) 0.011(3) -0.006(4) C12 0.022(3) 0.022(3) 0.038(4) 0.002(3) 0.004(3) 0.000(3) C6 0.028(3) 0.030(4) 0.034(4) -0.001(3) 0.006(3) 0.005(3) C18 0.025(3) 0.022(3) 0.039(4) -0.001(3) 0.005(3) -0.002(3) C7 0.028(4) 0.062(5) 0.045(4) 0.005(4) 0.004(3) -0.004(4) C17 0.027(4) 0.038(4) 0.057(5) 0.003(4) 0.002(3) -0.009(3) C11 0.036(4) 0.047(4) 0.033(4) -0.001(3) 0.001(3) 0.000(3) C21 0.063(5) 0.029(4) 0.061(5) 0.004(4) 0.014(4) -0.001(4) C14 0.031(4) 0.034(4) 0.061(5) 0.012(4) 0.014(3) 0.000(3) C38 0.023(4) 0.058(5) 0.044(4) -0.001(4) 0.002(3) -0.002(3) C13 0.031(4) 0.035(4) 0.043(4) 0.006(3) 0.011(3) -0.001(3) C37 0.026(3) 0.033(4) 0.035(4) -0.003(3) 0.007(3) 0.000(3) C19 0.039(4) 0.034(4) 0.048(5) 0.003(3) 0.023(3) 0.002(3) C25 0.023(3) 0.027(4) 0.042(4) 0.007(3) 0.001(3) -0.004(3) C23 0.021(3) 0.025(3) 0.036(4) -0.003(3) 0.001(3) -0.002(3) C29 0.030(4) 0.041(4) 0.030(4) -0.002(3) 0.007(3) 0.000(3) C32 0.027(4) 0.062(5) 0.047(5) -0.017(4) 0.008(3) 0.002(3) C28 0.031(4) 0.043(4) 0.038(4) 0.014(3) 0.008(3) -0.002(3) C39 0.026(4) 0.067(5) 0.060(5) -0.001(4) 0.000(4) -0.008(4) C24 0.034(4) 0.044(4) 0.036(4) -0.001(3) 0.004(3) -0.001(3) C42 0.033(4) 0.045(4) 0.046(5) -0.009(3) 0.003(3) -0.015(3) C26 0.036(4) 0.039(4) 0.046(5) 0.001(3) 0.013(3) -0.004(3) C30 0.020(3) 0.041(4) 0.037(4) -0.001(3) 0.009(3) -0.008(3) C22 0.049(4) 0.029(4) 0.048(5) 0.006(3) 0.019(4) -0.002(3) C31 0.028(4) 0.044(4) 0.046(5) -0.010(4) 0.014(3) 0.006(3) C9 0.055(5) 0.061(5) 0.041(5) 0.008(4) -0.009(4) 0.002(4) C27 0.040(4) 0.035(4) 0.053(5) 0.012(4) 0.009(4) -0.001(3) C10 0.058(5) 0.051(5) 0.033(4) 0.000(4) 0.008(4) -0.003(4) C3 0.038(4) 0.039(4) 0.062(5) 0.008(4) 0.004(4) 0.000(3) C2 0.044(5) 0.026(4) 0.050(5) -0.001(3) 0.003(4) -0.005(3) C8 0.038(4) 0.072(5) 0.047(5) 0.013(4) -0.007(4) -0.002(4) C20 0.056(5) 0.037(4) 0.056(5) -0.008(4) 0.024(4) 0.002(4) C41 0.052(5) 0.052(5) 0.058(5) -0.003(4) -0.005(4) -0.019(4) C34 0.033(4) 0.099(7) 0.058(6) -0.021(5) 0.010(4) 0.006(4) C36 0.039(4) 0.096(7) 0.049(5) -0.014(5) 0.012(4) 0.008(4) C33 0.033(4) 0.097(7) 0.062(6) -0.026(5) 0.007(4) 0.007(4) C35 0.045(5) 0.096(7) 0.049(5) -0.021(5) 0.016(4) 0.016(4) C15 0.032(4) 0.058(5) 0.074(6) 0.009(4) 0.008(4) -0.018(4) C4 0.048(5) 0.082(6) 0.077(6) 0.032(5) 0.020(5) 0.016(4) C16 0.034(4) 0.055(5) 0.079(6) 0.018(4) -0.003(4) -0.007(4) C40 0.032(4) 0.093(7) 0.066(6) 0.006(5) -0.011(4) -0.023(4) C5 0.073(6) 0.102(8) 0.065(6) 0.020(5) -0.012(5) 0.029(6) C43 0.064(11) 0.067(10) 0.070(13) 0.026(9) 0.018(9) -0.006(9) C46 0.113(13) 0.068(9) 0.037(8) 0.015(7) 0.028(8) -0.025(7) C44 0.111(12) 0.092(12) 0.061(16) -0.023(11) 0.023(12) -0.032(11) C47 0.113(13) 0.068(9) 0.037(8) 0.015(7) 0.028(8) -0.025(7) C45 0.084(11) 0.068(10) 0.049(11) -0.007(8) 0.003(10) -0.020(8) C44A 0.069(8) 0.086(10) 0.040(7) -0.010(7) -0.010(6) 0.016(7) C47A 0.061(12) 0.061(12) 0.103(15) 0.020(10) 0.029(11) 0.012(9) C46A 0.052(11) 0.18(2) 0.099(16) -0.012(15) -0.009(12) 0.017(13) C43A 0.069(8) 0.086(10) 0.040(7) -0.010(7) -0.010(6) 0.016(7) C45A 0.069(8) 0.086(10) 0.040(7) -0.010(7) -0.010(6) 0.016(7) 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' P P 0.1023 0.0942 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle P2 Pd1 Si2 83.43(6) P2 Pd1 P1 154.52(6) P1 Pd1 Si2 83.19(6) C1 Pd1 P2 95.96(17) C1 Pd1 Si2 169.23(18) C1 Pd1 P1 101.14(17) C37 P2 Pd1 113.3(2) C37 P2 C31 106.3(3) C30 P2 Pd1 112.4(2) C30 P2 C37 100.9(3) C30 P2 C31 106.9(3) C31 P2 Pd1 115.8(2) C25 Si2 Pd1 108.7(2) C23 Si2 Pd1 107.1(2) C23 Si2 C25 113.0(3) C24 Si2 Pd1 119.3(2) C24 Si2 C25 103.1(3) C24 Si2 C23 105.8(3) C12 P1 Pd1 115.5(2) C12 P1 C6 104.5(3) C6 P1 Pd1 118.7(2) C18 P1 Pd1 109.7(2) C18 P1 C12 100.6(3) C18 P1 C6 106.0(3) C2 C1 Pd1 103.5(4) C17 C12 P1 110.6(4) C17 C12 C13 109.1(5) C13 C12 P1 114.1(4) C7 C6 P1 110.0(4) C11 C6 P1 117.2(4) C11 C6 C7 110.2(5) C19 C18 P1 123.4(5) C19 C18 C23 120.2(6) C23 C18 P1 116.4(5) C8 C7 C6 111.1(6) C12 C17 C16 111.9(6) C6 C11 C10 111.0(5) C22 C21 C20 120.2(7) C13 C14 C15 111.4(5) C37 C38 C39 112.3(6) C14 C13 C12 111.5(5) C38 C37 P2 110.8(4) C38 C37 C42 110.2(5) C42 C37 P2 112.8(4) C20 C19 C18 121.5(6) C26 C25 Si2 125.3(5) C30 C25 Si2 115.7(5) C30 C25 C26 118.7(6) C18 C23 Si2 117.0(4) C22 C23 Si2 125.1(5) C22 C23 C18 117.9(6) C28 C29 C30 120.2(6) C31 C32 C33 111.9(5) C29 C28 C27 119.9(6) C40 C39 C38 111.2(6) C37 C42 C41 111.9(5) C27 C26 C25 120.8(7) C25 C30 P2 117.0(5) C25 C30 C29 120.2(6) C29 C30 P2 122.7(5) C21 C22 C23 121.3(6) C32 C31 P2 109.7(4) C36 C31 P2 119.6(5) C36 C31 C32 110.8(5) C8 C9 C10 111.6(6) C26 C27 C28 120.2(6) C9 C10 C11 110.5(6) C2 C3 C4 121.7(7) C2 C3 C5 123.3(7) C5 C3 C4 114.9(7) C3 C2 C1 132.2(7) C9 C8 C7 112.7(6) C19 C20 C21 118.9(7) C40 C41 C42 111.0(6) C33 C34 C35 111.8(6) C31 C36 C35 111.4(6) C34 C33 C32 112.3(6) C34 C35 C36 111.0(6) C16 C15 C14 111.1(6) C15 C16 C17 111.0(6) C39 C40 C41 110.5(6) C45 C46 C47 116(2) C43 C44 C45 91.5(17) C46 C45 C44 96(2) C45A C44A C43A 111(2) C47A C46A C45A 96.3(18) C44A C45A C46A 117(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pd1 P2 2.2729(18) Pd1 Si2 2.3300(18) Pd1 P1 2.3048(17) Pd1 C1 2.213(6) P2 C37 1.841(6) P2 C30 1.839(6) P2 C31 1.846(6) Si2 C25 1.901(6) Si2 C23 1.889(6) Si2 C24 1.876(6) P1 C12 1.841(6) P1 C6 1.844(6) P1 C18 1.836(6) C1 C2 1.432(8) C12 C17 1.522(8) C12 C13 1.529(7) C6 C7 1.536(8) C6 C11 1.534(8) C18 C19 1.391(8) C18 C23 1.402(8) C7 C8 1.520(9) C17 C16 1.531(9) C11 C10 1.535(9) C21 C22 1.389(9) C21 C20 1.392(9) C14 C13 1.515(8) C14 C15 1.522(9) C38 C37 1.525(8) C38 C39 1.530(9) C37 C42 1.526(8) C19 C20 1.380(9) C25 C26 1.402(8) C25 C30 1.392(8) C23 C22 1.401(8) C29 C28 1.379(8) C29 C30 1.404(8) C32 C31 1.528(8) C32 C33 1.541(9) C28 C27 1.387(9) C39 C40 1.509(10) C42 C41 1.541(8) C26 C27 1.383(9) C31 C36 1.485(9) C9 C10 1.511(9) C9 C8 1.507(10) C3 C2 1.326(9) C3 C4 1.507(10) C3 C5 1.489(10) C41 C40 1.514(10) C34 C33 1.464(9) C34 C35 1.510(9) C36 C35 1.540(9) C15 C16 1.511(9) C43 C44 1.418(17) C46 C47 1.424(16) C46 C45 1.370(16) C44 C45 1.438(19) C44A C43A 1.476(19) C44A C45A 1.397(19) C47A C46A 1.422(19) C46A C45A 1.449(19) _cod_duplicate_entry 1516327