#------------------------------------------------------------------------------ #$Date: 2012-03-07 19:39:41 +0200 (Wed, 07 Mar 2012) $ #$Revision: 40069 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/06/89/4068969.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_4068969 loop_ _publ_author_name 'Allen, Olivia R.' 'Dalgarno, Scott J.' 'Field, Leslie D.' 'Jensen, Paul' 'Willis, Anthony C.' _publ_section_title ; Insertion of CO2into the Ru−C Bonds ofcis-andtrans-Ru(dmpe)2Me2(dmpe = Me2PCH2CH2PMe2) ; _journal_issue 8 _journal_name_full Organometallics _journal_page_first 2385 _journal_volume 28 _journal_year 2009 _chemical_formula_sum 'C13 H36 P4 Ru' _chemical_formula_weight 417.37 _chemical_name_systematic ; ? ; _space_group_IT_number 33 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 17.6025(14) _cell_length_b 9.1856(7) _cell_length_c 12.2908(9) _cell_measurement_temperature 100(2) _cell_volume 1987.3(3) _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker Nonius X8Apex2' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 68720 _diffrn_reflns_theta_full 30.48 _diffrn_reflns_theta_max 30.48 _diffrn_reflns_theta_min 2.50 _exptl_absorpt_coefficient_mu 1.097 _exptl_absorpt_correction_T_max 0.8440 _exptl_absorpt_correction_T_min 0.7343 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS' _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 872 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.391 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.059 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 1.01(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 176 _refine_ls_number_reflns 5960 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0241 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+1.9888P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.0542 _reflns_number_gt 5592 _reflns_number_total 5960 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file om801184k_si_001.cif _[local]_cod_data_source_block oa626 _[local]_cod_cif_authors_sg_H-M Pna21 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 4068969 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' 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 Ru1 Ru 0.889302(8) 0.110441(15) 0.037550(14) 0.01033(4) Uani 1 1 d . P1 P 0.80543(3) -0.05619(7) -0.03022(4) 0.01446(11) Uani 1 1 d . P2 P 0.81013(3) 0.27705(7) -0.03981(5) 0.01496(11) Uani 1 1 d . P4 P 0.97406(3) -0.05730(7) 0.10147(4) 0.01476(11) Uani 1 1 d . P3 P 0.97908(3) 0.27529(6) 0.09004(4) 0.01411(11) Uani 1 1 d . C5 C 0.76983(13) 0.4281(2) 0.0387(3) 0.0234(4) Uani 1 1 d . H5A H 0.8103 0.4967 0.0580 0.035 Uiso 1 1 calc R H5B H 0.7463 0.3901 0.1051 0.035 Uiso 1 1 calc R H5C H 0.7314 0.4781 -0.0052 0.035 Uiso 1 1 calc R C1 C 0.73375(14) -0.1403(3) 0.0587(2) 0.0257(6) Uani 1 1 d . H1A H 0.7013 -0.2050 0.0156 0.038 Uiso 1 1 calc R H1B H 0.7026 -0.0641 0.0921 0.038 Uiso 1 1 calc R H1C H 0.7592 -0.1967 0.1157 0.038 Uiso 1 1 calc R C9 C 1.06928(13) 0.1783(3) 0.11511(19) 0.0185(4) Uani 1 1 d . H9A H 1.0950 0.1575 0.0452 0.022 Uiso 1 1 calc R H9B H 1.1034 0.2394 0.1600 0.022 Uiso 1 1 calc R C2 C 0.83592(14) -0.2185(3) -0.1044(2) 0.0200(5) Uani 1 1 d . H2A H 0.8581 -0.2886 -0.0534 0.030 Uiso 1 1 calc R H2B H 0.8739 -0.1912 -0.1590 0.030 Uiso 1 1 calc R H2C H 0.7920 -0.2627 -0.1407 0.030 Uiso 1 1 calc R C10 C 1.05179(13) 0.0355(3) 0.1746(2) 0.0205(5) Uani 1 1 d . H10A H 1.0364 0.0559 0.2505 0.025 Uiso 1 1 calc R H10B H 1.0975 -0.0272 0.1761 0.025 Uiso 1 1 calc R C6 C 0.84103(15) 0.3727(3) -0.1635(2) 0.0237(5) Uani 1 1 d . H6A H 0.8008 0.4391 -0.1875 0.036 Uiso 1 1 calc R H6B H 0.8515 0.3015 -0.2210 0.036 Uiso 1 1 calc R H6C H 0.8872 0.4284 -0.1478 0.036 Uiso 1 1 calc R C8 C 1.01221(15) 0.4217(3) -0.0002(2) 0.0229(5) Uani 1 1 d . H8A H 0.9722 0.4952 -0.0078 0.034 Uiso 1 1 calc R H8B H 1.0244 0.3811 -0.0718 0.034 Uiso 1 1 calc R H8C H 1.0577 0.4669 0.0310 0.034 Uiso 1 1 calc R C3 C 0.74410(14) 0.0341(3) -0.1325(2) 0.0228(5) Uani 1 1 d . H3A H 0.7715 0.0432 -0.2025 0.027 Uiso 1 1 calc R H3B H 0.6976 -0.0241 -0.1448 0.027 Uiso 1 1 calc R C12 C 1.02845(14) -0.1649(3) 0.0031(2) 0.0257(5) Uani 1 1 d . H12A H 1.0629 -0.2306 0.0420 0.039 Uiso 1 1 calc R H12B H 1.0581 -0.0995 -0.0435 0.039 Uiso 1 1 calc R H12C H 0.9935 -0.2221 -0.0419 0.039 Uiso 1 1 calc R C7 C 0.96849(16) 0.3790(3) 0.2169(2) 0.0252(5) Uani 1 1 d . H7A H 1.0137 0.4394 0.2284 0.038 Uiso 1 1 calc R H7B H 0.9627 0.3114 0.2781 0.038 Uiso 1 1 calc R H7C H 0.9235 0.4414 0.2120 0.038 Uiso 1 1 calc R C11 C 0.94770(16) -0.1983(3) 0.1995(2) 0.0270(6) Uani 1 1 d . H11A H 0.9129 -0.2675 0.1649 0.041 Uiso 1 1 calc R H11B H 0.9226 -0.1532 0.2622 0.041 Uiso 1 1 calc R H11C H 0.9935 -0.2496 0.2238 0.041 Uiso 1 1 calc R C4 C 0.72314(14) 0.1852(3) -0.0890(2) 0.0243(5) Uani 1 1 d . H4A H 0.6862 0.1757 -0.0288 0.029 Uiso 1 1 calc R H4B H 0.6994 0.2436 -0.1476 0.029 Uiso 1 1 calc R C13 C 0.82673(15) 0.1235(3) 0.1964(2) 0.0222(5) Uani 1 1 d . H13A H 0.8448 0.2079 0.2377 0.033 Uiso 1 1 calc R H13B H 0.8359 0.0345 0.2384 0.033 Uiso 1 1 calc R H13C H 0.7722 0.1337 0.1824 0.033 Uiso 1 1 calc R H100 H 0.9378(19) 0.103(3) -0.078(3) 0.036(9) Uiso 1 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 Ru1 0.00991(6) 0.01120(6) 0.00988(6) -0.00064(9) 0.00034(6) -0.00071(5) P1 0.0126(3) 0.0162(3) 0.0146(2) -0.0033(2) 0.0007(2) -0.0030(2) P2 0.0136(3) 0.0151(3) 0.0162(2) -0.0010(2) -0.0015(2) 0.0024(2) P4 0.0136(3) 0.0127(3) 0.0180(3) 0.0034(2) -0.0010(2) -0.0007(2) P3 0.0148(3) 0.0131(3) 0.0144(2) 0.0007(2) -0.0017(2) -0.0028(2) C5 0.0233(10) 0.0183(10) 0.0287(10) -0.0015(13) 0.0016(13) 0.0041(8) C1 0.0202(11) 0.0304(13) 0.0263(15) -0.0061(10) 0.0077(9) -0.0104(9) C9 0.0142(10) 0.0204(11) 0.0209(10) 0.0043(9) -0.0038(8) -0.0039(9) C2 0.0224(12) 0.0158(11) 0.0217(10) -0.0041(9) 0.0019(9) -0.0041(9) C10 0.0171(11) 0.0211(12) 0.0233(11) 0.0064(9) -0.0063(9) -0.0031(9) C6 0.0276(13) 0.0247(13) 0.0188(11) 0.0079(9) -0.0023(9) 0.0064(10) C8 0.0243(12) 0.0187(12) 0.0257(11) 0.0072(9) -0.0026(10) -0.0069(9) C3 0.0185(11) 0.0271(13) 0.0227(11) -0.0051(9) -0.0079(9) -0.0004(10) C12 0.0220(11) 0.0207(12) 0.0344(13) -0.0017(10) 0.0032(10) 0.0060(10) C7 0.0307(14) 0.0232(13) 0.0218(11) -0.0057(9) -0.0019(10) -0.0061(10) C11 0.0249(13) 0.0216(13) 0.0345(13) 0.0128(11) -0.0028(11) -0.0043(10) C4 0.0164(11) 0.0265(13) 0.0299(12) -0.0030(10) -0.0078(9) 0.0026(10) C13 0.0264(12) 0.0231(12) 0.0171(10) -0.0028(9) 0.0067(9) -0.0028(10) 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' Ru Ru -1.2594 0.8363 '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 C13 Ru1 P2 91.55(7) C13 Ru1 P3 93.35(7) P2 Ru1 P3 95.50(2) C13 Ru1 P1 92.05(7) P2 Ru1 P1 84.41(2) P3 Ru1 P1 174.60(2) C13 Ru1 P4 93.28(7) P2 Ru1 P4 175.17(2) P3 Ru1 P4 84.15(2) P1 Ru1 P4 95.48(2) C2 P1 C1 98.93(11) C2 P1 C3 101.40(12) C1 P1 C3 101.03(12) C2 P1 Ru1 122.59(8) C1 P1 Ru1 120.55(8) C3 P1 Ru1 108.90(9) C6 P2 C5 100.84(13) C6 P2 C4 101.10(13) C5 P2 C4 101.36(11) C6 P2 Ru1 119.03(8) C5 P2 Ru1 121.72(10) C4 P2 Ru1 109.66(9) C12 P4 C11 100.68(13) C12 P4 C10 100.55(12) C11 P4 C10 101.22(12) C12 P4 Ru1 118.58(9) C11 P4 Ru1 122.59(9) C10 P4 Ru1 109.88(8) C8 P3 C7 99.49(12) C8 P3 C9 100.42(11) C7 P3 C9 101.30(12) C8 P3 Ru1 122.33(8) C7 P3 Ru1 120.92(9) C9 P3 Ru1 108.81(8) C10 C9 P3 108.65(16) C9 C10 P4 108.17(15) C4 C3 P1 108.04(16) C3 C4 P2 109.14(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ru1 C13 2.245(2) Ru1 P2 2.2778(6) Ru1 P3 2.2818(6) Ru1 P1 2.2839(6) Ru1 P4 2.2841(6) P1 C2 1.828(2) P1 C1 1.839(2) P1 C3 1.853(2) P2 C6 1.838(2) P2 C5 1.832(3) P2 C4 1.850(3) P4 C12 1.832(3) P4 C11 1.828(3) P4 C10 1.846(2) P3 C8 1.838(2) P3 C7 1.837(3) P3 C9 1.847(2) C9 C10 1.532(3) C3 C4 1.532(4)