#------------------------------------------------------------------------------ #$Date: 2015-01-23 14:30:19 +0200 (Fri, 23 Jan 2015) $ #$Revision: 130086 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/06/89/4068967.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_4068967 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_paper_doi 10.1021/om801184k _journal_volume 28 _journal_year 2009 _chemical_absolute_configuration ad _chemical_compound_source ' from UNSW ' _chemical_formula_moiety 'C16 H38 O4 P4 Ru' _chemical_formula_sum 'C16 H38 O4 P4 Ru' _chemical_formula_weight 519.44 _chemical_name_systematic ; ? ; _space_group_IT_number 96 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'P 4nw 2abw' _symmetry_space_group_name_H-M 'P 43 21 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 06-06-16 _audit_creation_method CRYSTALS_ver_12.18 _audit_update_record ; 2006-06-16 - Report on C16 H38 O4 P4 Ru by Anthony C. Willis for Olivia Allen and Les Field (UNSW) 2006-06-16 - passes checkcif tests with minor warnings ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.0425(1) _cell_length_b 9.0425(1) _cell_length_c 29.0790(4) _cell_measurement_reflns_used 37124 _cell_measurement_temperature 200 _cell_measurement_theta_max 27 _cell_measurement_theta_min 3 _cell_volume 2377.70(5) _computing_cell_refinement 'Denzo/Scalepack ' _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_molecular_graphics ; ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997) ; _computing_publication_material 'CRYSTALS ' _computing_structure_refinement 'CRYSTALS (Watkin et al 2003)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _diffrn_ambient_temperature 200 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ' \f and \w scans with CCD ' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 37225 _diffrn_reflns_theta_full 27.480 _diffrn_reflns_theta_max 27.480 _diffrn_reflns_theta_min 3.081 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.945 _exptl_absorpt_correction_T_max 0.892 _exptl_absorpt_correction_T_min 0.843 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details ; via Gaussian method (Coppens, 1970) implemented in maXus (2000) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_meas ? _exptl_crystal_description plate _exptl_crystal_F_000 1080 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.43 _refine_diff_density_min -0.82 _refine_ls_abs_structure_details 'Flack (1983), 1056 Friedel-pairs' _refine_ls_abs_structure_Flack 0.31(3) _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 0.8941 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 2729 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0186 _refine_ls_R_factor_gt 0.0164 _refine_ls_shift/su_max 0.001047 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 15.8 24.8 14.4 6.06 1.23 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0421 _refine_ls_wR_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0421 _reflns_limit_h_max 8 _reflns_limit_h_min -7 _reflns_limit_k_max 11 _reflns_limit_k_min 0 _reflns_limit_l_max 37 _reflns_limit_l_min 0 _reflns_number_gt 2499 _reflns_number_total 2734 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 1.56 _oxford_diffrn_Wilson_scale 9.98 _oxford_refine_ls_scale 0.3542(2) _oxford_structure_analysis_title '6161026 nsw0614' _[local]_cod_data_source_file om801184k_si_001.cif _[local]_cod_data_source_block nsw0614 _[local]_cod_cif_authors_sg_H-M 'P 43 21 2 ' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' 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 The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 4068967 loop_ _symmetry_equiv_pos_as_xyz x,y,z -y+1/2,x+1/2,z+3/4 -x,-y,z+1/2 y+1/2,-x+1/2,z+1/4 -x+1/2,y+1/2,-z+3/4 y,x,-z x+1/2,-y+1/2,-z+1/4 -y,-x,-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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Ru1 Ru 0.480814(11) 0.519186(11) 0.2500 0.0169 1.0000 Uani S T P1 P 0.35317(5) 0.63355(6) 0.190598(15) 0.0249 1.0000 Uani . . P2 P 0.59270(5) 0.38842(5) 0.190405(14) 0.0241 1.0000 Uani . . O1 O 0.30656(13) 0.36354(13) 0.24280(4) 0.0241 1.0000 Uani . . O2 O 0.29779(18) 0.25532(18) 0.31220(5) 0.0422 1.0000 Uani . . C1 C 0.3782(3) 0.5234(3) 0.13801(6) 0.0365 1.0000 Uani . . C2 C 0.5376(2) 0.4682(2) 0.13466(5) 0.0350 1.0000 Uani . . C3 C 0.1523(2) 0.6451(3) 0.19440(10) 0.0469 1.0000 Uani . . C4 C 0.4018(3) 0.8209(2) 0.17287(8) 0.0401 1.0000 Uani . . C5 C 0.5268(3) 0.1972(2) 0.18464(7) 0.0380 1.0000 Uani . . C6 C 0.7917(3) 0.3601(3) 0.18438(9) 0.0427 1.0000 Uani . . C7 C 0.2554(2) 0.2726(2) 0.27239(6) 0.0262 1.0000 Uani . . C8 C 0.1295(2) 0.1773(2) 0.25394(8) 0.0408 1.0000 Uani . . H11 H 0.3552(3) 0.5861(3) 0.11059(6) 0.0438 1.0000 Uiso R . H12 H 0.3096(3) 0.4367(3) 0.13876(6) 0.0438 1.0000 Uiso R . H21 H 0.6044(2) 0.5527(2) 0.12686(5) 0.0420 1.0000 Uiso R . H22 H 0.5448(2) 0.3909(2) 0.11017(5) 0.0420 1.0000 Uiso R . H31 H 0.1241(2) 0.7037(3) 0.22222(10) 0.0563 1.0000 Uiso R . H32 H 0.1127(2) 0.6948(3) 0.16625(10) 0.0563 1.0000 Uiso R . H33 H 0.1099(2) 0.5433(3) 0.19681(10) 0.0563 1.0000 Uiso R . H41 H 0.3913(3) 0.8895(2) 0.19964(8) 0.0481 1.0000 Uiso R . H42 H 0.5063(3) 0.8225(2) 0.16169(8) 0.0481 1.0000 Uiso R . H43 H 0.3343(3) 0.8533(2) 0.14755(8) 0.0481 1.0000 Uiso R . H51 H 0.5506(3) 0.1409(2) 0.21331(7) 0.0456 1.0000 Uiso R . H52 H 0.5766(3) 0.1493(2) 0.15779(7) 0.0456 1.0000 Uiso R . H53 H 0.4174(3) 0.1973(2) 0.17967(7) 0.0456 1.0000 Uiso R . H61 H 0.8320(3) 0.3165(3) 0.21340(9) 0.0513 1.0000 Uiso R . H62 H 0.8410(3) 0.4571(3) 0.17828(9) 0.0513 1.0000 Uiso R . H63 H 0.8111(3) 0.2911(3) 0.15818(9) 0.0513 1.0000 Uiso R . H81 H 0.0946(2) 0.1088(2) 0.27865(8) 0.0490 0.5000 Uiso R . H82 H 0.0460(2) 0.2423(2) 0.24398(8) 0.0490 0.5000 Uiso R . H83 H 0.1655(2) 0.1183(2) 0.22709(8) 0.0490 0.5000 Uiso R . H84 H 0.1087(2) 0.2050(2) 0.22128(8) 0.0490 0.5000 Uiso R . H85 H 0.0389(2) 0.1937(2) 0.27296(8) 0.0490 0.5000 Uiso R . H86 H 0.1585(2) 0.0707(2) 0.25548(8) 0.0490 0.5000 Uiso 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 Ru1 0.01767(6) 0.01767(6) 0.01533(8) 0.00035(4) 0.00035(4) -0.00004(6) P1 0.0258(3) 0.0254(2) 0.0234(2) 0.00516(19) -0.00534(18) 0.00055(16) P2 0.0256(2) 0.0250(2) 0.02175(19) -0.00517(18) 0.00275(17) 0.00034(17) O1 0.0241(6) 0.0254(6) 0.0227(6) 0.0014(5) -0.0019(5) -0.0068(4) O2 0.0464(9) 0.0501(10) 0.0301(7) 0.0127(7) -0.0067(6) -0.0185(7) C1 0.0476(11) 0.0387(10) 0.0233(9) 0.0003(8) -0.0116(8) -0.0016(10) C2 0.0478(11) 0.0379(10) 0.0194(7) -0.0044(7) 0.0017(7) -0.0060(8) C3 0.0287(11) 0.0585(16) 0.0536(15) 0.0131(12) -0.0105(10) 0.0050(10) C4 0.0519(14) 0.0279(10) 0.0404(12) 0.0122(9) -0.0059(10) -0.0018(10) C5 0.0474(12) 0.0269(9) 0.0398(11) -0.0102(8) 0.0032(10) -0.0015(10) C6 0.0308(11) 0.0482(14) 0.0492(13) -0.0152(11) 0.0100(10) 0.0054(10) C7 0.0237(9) 0.0259(9) 0.0289(8) 0.0013(7) 0.0009(7) -0.0042(6) C8 0.0347(10) 0.0374(10) 0.0504(12) 0.0067(10) -0.0071(10) -0.0157(8) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.060 0 0 -1 0.100 1 -1 0 0.050 -1 1 0 0.140 0 -1 1 0.080 0 1 -1 0.120 0 1 1 0.090 0 -1 -1 0.110 1 0 1 0.080 -1 0 -1 0.130 -1 0 3 0.075 1 0 -3 0.091 loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag P1 8_665 Ru1 P1 96.36(2) yes P2 8_665 Ru1 P2 96.46(2) yes P1 8_665 Ru1 P2 179.13(2) yes P1 . Ru1 P2 83.597(14) yes O1 8_665 Ru1 O1 173.58(7) yes P2 8_665 Ru1 O1 99.33(3) yes P1 8_665 Ru1 O1 94.15(4) yes P1 . Ru1 O1 81.54(4) yes P2 . Ru1 O1 84.98(3) yes Ru1 . P1 C1 108.45(7) yes Ru1 . P1 C3 118.43(9) yes C1 . P1 C3 101.77(12) yes Ru1 . P1 C4 120.29(8) yes C1 . P1 C4 103.79(11) yes C3 . P1 C4 101.76(12) yes Ru1 . P2 C2 109.76(6) yes Ru1 . P2 C5 113.89(7) yes C2 . P2 C5 101.56(10) yes Ru1 . P2 C6 124.80(8) yes C2 . P2 C6 103.72(11) yes C5 . P2 C6 100.30(12) yes Ru1 . O1 C7 129.01(11) yes P1 . C1 C2 110.23(12) yes P1 . C1 H11 109.3 no C2 . C1 H11 109.3 no P1 . C1 H12 109.3 no C2 . C1 H12 109.3 no H11 . C1 H12 109.5 no C1 . C2 P2 109.08(12) yes C1 . C2 H21 109.6 no P2 . C2 H21 109.6 no C1 . C2 H22 109.6 no P2 . C2 H22 109.6 no H21 . C2 H22 109.5 no P1 . C3 H31 109.5 no P1 . C3 H32 109.5 no H31 . C3 H32 109.5 no P1 . C3 H33 109.5 no H31 . C3 H33 109.5 no H32 . C3 H33 109.5 no P1 . C4 H41 109.5 no P1 . C4 H42 109.5 no H41 . C4 H42 109.5 no P1 . C4 H43 109.5 no H41 . C4 H43 109.5 no H42 . C4 H43 109.5 no P2 . C5 H51 109.5 no P2 . C5 H52 109.5 no H51 . C5 H52 109.5 no P2 . C5 H53 109.5 no H51 . C5 H53 109.5 no H52 . C5 H53 109.5 no P2 . C6 H61 109.5 no P2 . C6 H62 109.5 no H61 . C6 H62 109.5 no P2 . C6 H63 109.5 no H61 . C6 H63 109.5 no H62 . C6 H63 109.5 no O1 . C7 O2 127.09(15) yes O1 . C7 C8 113.41(16) yes O2 . C7 C8 119.49(16) yes C7 . C8 H81 109.5 no C7 . C8 H82 109.5 no H81 . C8 H82 109.5 no C7 . C8 H83 109.5 no H81 . C8 H83 109.5 no H82 . C8 H83 109.5 no C7 . C8 H84 109.5 no C7 . C8 H85 109.5 no H84 . C8 H85 109.5 no C7 . C8 H86 109.5 no H84 . C8 H86 109.5 no H85 . C8 H86 109.5 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ru1 P1 2.3206(4) yes Ru1 P2 2.3292(4) yes Ru1 O1 2.1231(11) yes P1 C1 1.839(2) yes P1 C3 1.823(2) yes P1 C4 1.824(2) yes P2 C2 1.8431(18) yes P2 C5 1.836(2) yes P2 C6 1.826(2) yes O1 C7 1.277(2) yes O2 C7 1.229(2) yes C1 C2 1.528(3) yes C1 H11 1.000 no C1 H12 1.000 no C2 H21 1.000 no C2 H22 1.000 no C3 H31 1.000 no C3 H32 1.000 no C3 H33 1.000 no C4 H41 1.000 no C4 H42 1.000 no C4 H43 1.000 no C5 H51 1.000 no C5 H52 1.000 no C5 H53 1.000 no C6 H61 1.000 no C6 H62 1.000 no C6 H63 1.000 no C7 C8 1.525(2) yes C8 H81 1.000 no C8 H82 1.000 no C8 H83 1.000 no C8 H84 1.000 no C8 H85 1.000 no C8 H86 1.000 no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag O2 C4 3.524(3) 4_455 no O2 C1 3.532(3) 4_455 no 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_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Ru1 P1 C1 C2 . . -40.5(2) no Ru1 P2 C2 C1 . . -34.5(2) no Ru1 O1 C7 O2 . . -0.3(3) no Ru1 O1 C7 C8 . . -179.6(1) no P1 Ru1 P1 C1 8_665 8_665 -164.42(9) no P1 Ru1 P1 C3 8_665 8_665 -49.3(1) no P1 Ru1 P1 C4 8_665 8_665 76.53(9) no P1 Ru1 P2 C2 . . 8.08(6) no P1 Ru1 P2 C5 . . -105.01(8) no P1 Ru1 P2 C6 . . 131.9(1) no P1 Ru1 O1 C7 . . -155.8(1) no P1 Ru1 O1 C7 8_665 8_665 -59.9(1) no P1 C1 C2 P2 . . 47.5(2) no P2 Ru1 P1 C1 . . 14.70(9) no P2 Ru1 P1 C3 . . 129.9(1) no P2 Ru1 P1 C4 . . -104.35(9) no P2 Ru1 P2 C2 8_665 8_665 -171.04(7) no P2 Ru1 P2 C5 8_665 8_665 75.86(8) no P2 Ru1 P2 C6 8_665 8_665 -47.2(1) no P2 Ru1 O1 C7 . . 120.0(1) no P2 Ru1 O1 C7 8_665 8_665 24.2(1) no O1 Ru1 P1 C1 . . -71.1(1) no O1 Ru1 P1 C3 . . 44.0(1) no O1 Ru1 P1 C4 . . 169.8(1) no O1 Ru1 P1 C1 8_665 8_665 113.6(1) no O1 Ru1 P1 C3 8_665 8_665 -131.2(1) no O1 Ru1 P1 C4 8_665 8_665 -5.4(1) no O1 Ru1 P2 C2 . . 90.11(7) no O1 Ru1 P2 C5 . . -22.99(9) no O1 Ru1 P2 C6 . . -146.1(1) no O1 Ru1 P2 C2 8_665 8_665 -85.09(7) no O1 Ru1 P2 C5 8_665 8_665 161.81(9) no O1 Ru1 P2 C6 8_665 8_665 38.7(1) no C1 C2 P2 C5 . . 86.4(2) no C1 C2 P2 C6 . . -169.8(2) no C2 C1 P1 C3 . . -166.1(2) no C2 C1 P1 C4 . . 88.5(2) no