#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2001996.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2001996 loop_ _publ_author_name 'Chiaroni, A.' 'Riche, C.' 'El Firdoussi, L.' 'Benharref, A.' 'Karim, A.' _publ_contact_author ; Dr Claude Riche Institut de Chimie des Substances Naturelles C.N.R.S. 91198 Gif-sur-Yvette CEDEX France ; _publ_section_title ; Structure du bis(\p-allylhimachal\`ene)-\a,\a-dichlorodipalladium ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 365 _journal_page_last 368 _journal_volume 49 _journal_year 1993 _chemical_formula_sum 'C30 H46 Cl2 Pd2' _chemical_formula_weight 690.40 _chemical_name_systematic ; bis(\p-allylhimachal\`ene) \a,\a-dichlorodipalladium ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_type_scat_source ; International Tables for X-ray Crystallography (1974, Tome IV, Tableau 2.2B) ; _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.059(7) _cell_length_b 10.226(7) _cell_length_c 29.416(15) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293 _cell_measurement_theta_max 20.70 _cell_measurement_theta_min 4.00 _cell_volume 3026.(3) _computing_data_collection 'Philips PW1100/20 software 1974' _computing_data_reduction 'PHIL (Riche, 1981)' _computing_molecular_graphics 'R3M (Riche, 1983) et ORTEP (Johnson, 1965)' _computing_publication_material 'ACTACIF (Riche, 1992)' _computing_structure_refinement 'SHELX76 (Sheldrick, 1976)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 293 _diffrn_measurement_device 'Philips PW1100 diffractometer' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4109 _diffrn_reflns_theta_max 25.98 _diffrn_reflns_theta_min 2.43 _diffrn_standards_decay_% 5 _diffrn_standards_interval_time 180 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.37 _exptl_absorpt_correction_type none _exptl_crystal_colour jaune _exptl_crystal_density_diffrn 1.52 _exptl_crystal_description Prisme _exptl_crystal_F_000 1408.01 _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.86 _refine_diff_density_min -1.00 _refine_ls_goodness_of_fit_obs 1.15 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 169 _refine_ls_number_reflns 2720 _refine_ls_R_factor_obs 0.051 _refine_ls_shift/esd_max 0.05 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 1/[\s^2^(F)+0.0004F^2^] _refine_ls_wR_factor_obs 0.064 _reflns_number_observed 2797 _reflns_number_total 3245 _reflns_observed_criterion I>3.0\s(I) _[local]_cod_data_source_file pa1026.cif _[local]_cod_data_source_block a loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 3 0 -4 2 -4 2 -2 8 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Pd1 0.06460(10) 0.57150(10) 0.19630(10) 0.0330(10) Uani ? ? Pd2 0.17150(10) 0.30990(10) 0.21550(10) 0.0350(10) Uani ? ? Cl1 0.2320(3) 0.5131(3) 0.25340(10) 0.047(3) Uani ? ? Cl2 -0.0613(3) 0.3825(3) 0.22140(10) 0.045(3) Uani ? ? C1 0.1400(10) 0.6101(11) 0.0931(4) 0.035(3) Uiso ? ? C2 0.2919(12) 0.6230(12) 0.0956(5) 0.043(3) Uiso ? ? C3 0.3578(12) 0.6898(14) 0.1273(5) 0.050(3) Uiso ? ? C4 0.2948(11) 0.7609(12) 0.1658(5) 0.043(3) Uiso ? ? C5 0.1483(12) 0.7450(12) 0.1670(4) 0.042(3) Uiso ? ? C6 0.0741(10) 0.6715(10) 0.1342(4) 0.031(2) Uiso ? ? C7 -0.0597(11) 0.6448(9) 0.1452(4) 0.033(2) Uiso ? ? C8 -0.1382(11) 0.5469(11) 0.1153(4) 0.040(3) Uiso ? ? C9 -0.1641(13) 0.5997(13) 0.0692(5) 0.055(3) Uiso ? ? C10 -0.0509(14) 0.5899(14) 0.0374(5) 0.059(3) Uiso ? ? C11 0.0822(12) 0.6599(11) 0.0479(4) 0.044(3) Uiso ? ? C12 0.5073(13) 0.6955(17) 0.1259(6) 0.067(4) Uiso ? ? C13 -0.1469(12) 0.7503(13) 0.1659(5) 0.049(3) Uiso ? ? C14 0.0623(15) 0.8059(14) 0.0474(5) 0.064(4) Uiso ? ? C15 0.1750(17) 0.6163(17) 0.0079(6) 0.078(5) Uiso ? ? C1' 0.2814(11) 0.2499(12) 0.1202(4) 0.042(3) Uiso ? ? C2' 0.1557(12) 0.2369(12) 0.0943(5) 0.046(3) Uiso ? ? C3' 0.0486(12) 0.1760(12) 0.1073(4) 0.047(3) Uiso ? ? C4' 0.0416(12) 0.1016(13) 0.1500(5) 0.050(3) Uiso ? ? C5' 0.1558(12) 0.1262(11) 0.1804(5) 0.045(3) Uiso ? ? C6' 0.2692(10) 0.1916(11) 0.1679(4) 0.036(2) Uiso ? ? C7' 0.3603(12) 0.2286(13) 0.2015(5) 0.055(3) Uiso ? ? C8' 0.4716(11) 0.3228(13) 0.1911(5) 0.053(3) Uiso ? ? C9' 0.5797(17) 0.2621(16) 0.1596(6) 0.074(4) Uiso ? ? C11' 0.4020(14) 0.1927(16) 0.0952(5) 0.061(4) Uiso ? ? C12' -0.0789(17) 0.1734(19) 0.0802(6) 0.086(5) Uiso ? ? C13' 0.3959(14) 0.1358(14) 0.2405(6) 0.061(4) Uiso ? ? C10' 0.532(3) 0.277(3) 0.1113(11) 0.061(8) Uiso ? ? C14' 0.420(3) 0.047(3) 0.0990(10) 0.054(7) Uiso ? ? C15' 0.398(3) 0.233(3) 0.0422(11) 0.062(8) Uiso ? ? C10" 0.522(4) 0.148(3) 0.1272(14) 0.081(10) Uiso ? ? C14" 0.365(3) 0.040(4) 0.0773(14) 0.078(10) Uiso ? ? C15" 0.465(4) 0.272(5) 0.0569(16) 0.106(14) Uiso ? ? H1 0.11920 0.51447 0.09380 0.041 Uiso calc C1 H2 0.34543 0.57771 0.07171 0.047 Uiso calc C2 H4a 0.31573 0.85610 0.16269 0.046 Uiso calc C4 H4b 0.33280 0.72713 0.19490 0.046 Uiso calc C4 H5 0.09847 0.78820 0.19231 0.047 Uiso calc C5 H8a -0.22512 0.52784 0.13040 0.045 Uiso calc C8 H8b -0.08580 0.46415 0.11245 0.045 Uiso calc C8 H9a -0.18822 0.69417 0.07226 0.062 Uiso calc C9 H9b -0.24064 0.55066 0.05578 0.062 Uiso calc C9 H10a -0.02985 0.49469 0.03435 0.066 Uiso calc C10 H10b -0.08244 0.62445 0.00745 0.066 Uiso calc C10 H12a 0.54012 0.74953 0.15194 0.074 Uiso calc C12 H12b 0.53721 0.73565 0.09665 0.074 Uiso calc C12 H12c 0.54394 0.60491 0.12845 0.074 Uiso calc C12 H13a -0.23796 0.71437 0.17135 0.054 Uiso calc C13 H13b -0.15268 0.82682 0.14484 0.054 Uiso calc C13 H13c -0.10736 0.77897 0.19549 0.054 Uiso calc C13 H14a 0.14862 0.85023 0.05428 0.070 Uiso calc C14 H14b -0.00488 0.83047 0.07098 0.070 Uiso calc C14 H14c 0.03008 0.83389 0.01679 0.070 Uiso calc C14 H15a 0.26463 0.65719 0.01175 0.087 Uiso calc C15 H15b 0.13555 0.64490 -0.02164 0.087 Uiso calc C15 H15c 0.18409 0.51893 0.00817 0.087 Uiso calc C15 H1' 0.29788 0.34604 0.12295 0.046 Uiso calc C1' H2' 0.15259 0.27980 0.06379 0.051 Uiso calc C2' H4'a 0.03891 0.00621 0.14254 0.055 Uiso calc C4' H4'b -0.04169 0.12674 0.16634 0.055 Uiso calc C4' H5' 0.15038 0.09266 0.21225 0.048 Uiso calc C5' H8'a 0.43326 0.40133 0.17566 0.057 Uiso calc C8' H8'b 0.51434 0.34992 0.22031 0.057 Uiso calc C8' H12'a -0.14718 0.12059 0.09671 0.095 Uiso calc C12' H12'b -0.06164 0.13328 0.04974 0.095 Uiso calc C12' H12'c -0.11224 0.26477 0.07607 0.095 Uiso calc C12' H13'a 0.31959 0.07542 0.24630 0.068 Uiso calc C13' H13'b 0.41515 0.18748 0.26857 0.068 Uiso calc C13' H13'c 0.47613 0.08370 0.23189 0.068 Uiso calc C13' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd1 0.0338(4) 0.0341(4) 0.0304(5) -0.0007(4) 0.0008(4) 0.0027(4) Pd2 0.0403(5) 0.0363(4) 0.0295(5) 0.0045(4) 0.0015(4) -0.0005(4) Cl1 0.053(2) 0.0440(10) 0.042(2) 0.0020(10) -0.017(2) -0.0010(10) Cl2 0.0410(10) 0.0390(10) 0.054(2) -0.0010(10) 0.011(2) 0.0090(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pd1 Pd2 . . 2.9390(10) yes Pd1 Cl1 . . 2.451(3) yes Pd1 Cl2 . . 2.426(3) yes Pd1 C5 . . 2.144(12) yes Pd1 C6 . . 2.096(10) yes Pd1 C7 . . 2.094(11) yes Pd2 Cl1 . . 2.435(3) yes Pd2 Cl2 . . 2.463(3) yes Pd2 C5' . . 2.150(12) yes Pd2 C6' . . 2.095(11) yes Pd2 C7' . . 2.113(13) yes C1 C2 . . 1.535(15) yes C1 C6 . . 1.515(15) yes C1 C11 . . 1.540(17) yes C2 C3 . . 1.333(19) yes C3 C4 . . 1.486(19) yes C3 C12 . . 1.506(18) yes C4 C5 . . 1.483(16) yes C5 C6 . . 1.433(16) yes C6 C7 . . 1.411(15) yes C7 C8 . . 1.549(16) yes C7 C13 . . 1.519(17) yes C8 C9 . . 1.483(19) yes C9 C10 . . 1.48(2) yes C10 C11 . . 1.549(18) yes C11 C14 . . 1.506(18) yes C11 C15 . . 1.57(2) yes C1' C2' . . 1.481(17) yes C1' C6' . . 1.530(17) yes C1' C11' . . 1.534(19) yes C2' C3' . . 1.302(17) yes C3' C4' . . 1.468(19) yes C3' C12' . . 1.51(2) yes C4' C5' . . 1.478(18) yes C5' C6' . . 1.373(16) yes C6' C7' . . 1.401(17) yes C7' C8' . . 1.509(18) yes C7' C13' . . 1.53(2) yes C8' C9' . . 1.56(2) yes C9' C10' . . 1.51(4) yes C9' C10" . . 1.61(4) yes C11' C10' . . 1.64(3) yes C11' C14' . . 1.51(3) yes C11' C15' . . 1.62(4) yes C11' C10" . . 1.60(4) yes C11' C14" . . 1.69(4) yes C11' C15" . . 1.53(5) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 Pd1 Cl2 . . . 87.50(10) yes Cl1 Pd1 C5 . . . 101.9(3) yes Cl1 Pd1 C6 . . . 133.2(3) yes Cl1 Pd1 C7 . . . 171.5(3) yes Cl2 Pd1 C5 . . . 170.5(3) yes Cl2 Pd1 C6 . . . 132.6(3) yes Cl2 Pd1 C7 . . . 101.1(3) yes C5 Pd1 C6 . . . 39.5(4) yes C5 Pd1 C7 . . . 69.5(4) yes C6 Pd1 C7 . . . 39.3(4) yes Cl1 Pd2 Cl2 . . . 87.00(10) yes Cl1 Pd2 C5' . . . 169.7(3) yes Cl1 Pd2 C6' . . . 132.9(3) yes Cl1 Pd2 C7' . . . 101.5(4) yes Cl2 Pd2 C5' . . . 103.1(3) yes Cl2 Pd2 C6' . . . 131.8(3) yes Cl2 Pd2 C7' . . . 170.6(4) yes C5' Pd2 C6' . . . 37.7(4) yes C5' Pd2 C7' . . . 68.2(5) yes C6' Pd2 C7' . . . 38.9(5) yes Pd1 Cl1 Pd2 . . . 73.90(10) yes Pd1 Cl2 Pd2 . . . 73.90(10) yes C2 C1 C6 . . . 111.2(9) yes C2 C1 C11 . . . 112.9(9) yes C6 C1 C11 . . . 112.8(9) yes C1 C2 C3 . . . 124.9(11) yes C2 C3 C4 . . . 124.8(12) yes C2 C3 C12 . . . 119.8(12) yes C4 C3 C12 . . . 115.3(12) yes C3 C4 C5 . . . 112.9(11) yes Pd1 C5 C4 . . . 119.4(8) yes Pd1 C5 C6 . . . 68.4(6) yes C4 C5 C6 . . . 123.9(10) yes Pd1 C6 C1 . . . 120.9(7) yes Pd1 C6 C5 . . . 72.1(6) yes Pd1 C6 C7 . . . 70.3(6) yes C1 C6 C5 . . . 121.8(9) yes C1 C6 C7 . . . 121.4(9) yes C5 C6 C7 . . . 116.3(10) yes Pd1 C7 C6 . . . 70.4(6) yes Pd1 C7 C8 . . . 118.7(7) yes Pd1 C7 C13 . . . 108.1(7) yes C6 C7 C8 . . . 118.8(9) yes C6 C7 C13 . . . 120.4(10) yes C8 C7 C13 . . . 113.2(9) yes C7 C8 C9 . . . 111.9(10) yes C8 C9 C10 . . . 114.8(11) yes C9 C10 C11 . . . 120.5(12) yes C1 C11 C10 . . . 110.2(10) yes C1 C11 C14 . . . 112.7(10) yes C1 C11 C15 . . . 109.2(10) yes C10 C11 C14 . . . 110.0(11) yes C10 C11 C15 . . . 103.6(11) yes C14 C11 C15 . . . 110.8(11) yes C2' C1' C6' . . . 111.6(10) yes C2' C1' C11' . . . 113.3(11) yes C6' C1' C11' . . . 110.7(10) yes C1' C2' C3' . . . 126.7(12) yes C2' C3' C4' . . . 122.6(12) yes C2' C3' C12' . . . 123.7(13) yes C4' C3' C12' . . . 113.7(12) yes C3' C4' C5' . . . 113.0(11) yes Pd2 C5' C4' . . . 119.8(9) yes Pd2 C5' C6' . . . 69.0(7) yes C4' C5' C6' . . . 124.5(11) yes Pd2 C6' C1' . . . 115.2(8) yes Pd2 C6' C5' . . . 73.3(7) yes Pd2 C6' C7' . . . 71.2(7) yes C1' C6' C5' . . . 120.1(10) yes C1' C6' C7' . . . 119.4(10) yes C5' C6' C7' . . . 119.0(11) yes Pd2 C7' C6' . . . 69.9(7) yes Pd2 C7' C8' . . . 117.1(9) yes Pd2 C7' C13' . . . 108.0(9) yes C6' C7' C8' . . . 120.9(11) yes C6' C7' C13' . . . 121.0(12) yes C8' C7' C13' . . . 112.0(11) yes C7' C8' C9' . . . 112.6(11) yes C8' C9' C10' . . . 107.3(16) yes C8' C9' C10" . . . 112.8(17) yes C9' C10' C11' . . . 118.(2) yes C1' C11' C10' . . . 106.9(14) yes C1' C11' C14' . . . 116.0(15) yes C1' C11' C15' . . . 110.1(15) yes C1' C11' C10" . . . 115.1(17) yes C1' C11' C14" . . . 109.2(16) yes C1' C11' C15" . . . 119.(2) yes C10' C11' C14' . . . 113.8(18) yes C10' C11' C15' . . . 99.4(17) yes C14' C11' C15' . . . 109.3(18) yes C10" C11' C14" . . . 95.(2) yes C10" C11' C15" . . . 106.(2) yes C14" C11' C15" . . . 110.(2) yes C9' C10" C11' . . . 115.(2) yes 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_publ_flag C6 C1 C2 C3 -5.9(10) yes C1 C2 C3 C4 0.9(12) yes C2 C3 C4 C5 2.9(11) yes C3 C4 C5 C6 -1.4(10) yes C4 C5 C6 C1 -4.0(10) yes C5 C6 C1 C2 7.1(9) yes C1 C2 C3 C12 -179.7(17) yes C11 C1 C6 C7 67.6(10) yes C1 C6 C7 C8 2.1(9) yes C6 C7 C8 C9 -69.0(11) yes C7 C8 C9 C10 80.1(12) yes C8 C9 C10 C11 -61.1(12) yes C9 C10 C11 C1 59.6(12) yes C10 C11 C1 C6 -79.2(11) yes C5 C6 C7 C13 42.8(10) yes C6' C1' C2' C3' -5.0(11) yes C1' C2' C3' C4' -4.4(12) yes C2' C3' C4' C5' 12.2(11) yes C3' C4' C5' C6' -11.3(11) yes C4' C5' C6' C1' 2.5(11) yes C5' C6' C1' C2' 5.7(10) yes C1' C2' C3' C12' 176.4(18) yes C11' C1' C6' C7' 72.2(12) yes C1' C6' C7' C8' -1.3(11) yes C6' C7' C8' C9' -70.1(13) yes C7' C8' C9' C10' 84.0(17) yes C8' C9' C10' C11' -68.1(19) yes C9' C10' C11' C1' 69.5(19) yes C10' C11' C1' C6' -83.7(16) yes C7' C8' C9' C10" 27.1(16) yes C8' C9' C10" C11' 57.(2) yes C9' C10" C11' C1' -57.(2) yes C10" C11' C1' C6' -29.0(16) yes Pd1 Cl1 Cl2 Pd2 119.40(10) yes Cl1 Pd1 Pd2 Cl1 112.3(2) yes _cod_database_code 2001996