#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/05/2200532.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_2200532 loop_ _publ_author_name 'Li, Zhengkai' 'Zhou, Zhongyuan' _publ_section_title ; trans-Tetrachlorobis(triphenylphosphine)osmium(IV) ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m291 _journal_page_last m292 _journal_volume 57 _journal_year 2001 _chemical_formula_moiety 'C36 H30 Cl4 Os P2' _chemical_formula_sum 'C36 H30 Cl4 Os P2' _chemical_formula_weight 856.54 _chemical_name_systematic ; trans-Tetrachloro-bis(triphenylphosphine)osmium(IV) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90 _cell_angle_beta 117.425(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.3364(9) _cell_length_b 20.948(2) _cell_length_c 9.6251(9) _cell_measurement_reflns_used CCD _cell_measurement_temperature 294(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 1.0 _cell_volume 1670.9(3) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 294(2) _diffrn_measured_fraction_theta_full .997 _diffrn_measured_fraction_theta_max .997 _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .044 _diffrn_reflns_av_sigmaI/netI .046 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 11100 _diffrn_reflns_theta_full 27.6 _diffrn_reflns_theta_max 27.6 _diffrn_reflns_theta_min 1.9 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.257 _exptl_absorpt_correction_T_max .676 _exptl_absorpt_correction_T_min .483 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour orange-red _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 840 _exptl_crystal_size_max .20 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .10 _refine_diff_density_max .98 _refine_diff_density_min -.60 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .98 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 194 _refine_ls_number_reflns 3844 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .98 _refine_ls_R_factor_all .046 _refine_ls_R_factor_gt .032 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0409P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .078 _reflns_number_gt 2867 _reflns_number_total 3844 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file tk6024.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2200532 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Os1 .0000 .5000 .0000 .02692(8) Uani d S 1 . . Os Cl1 -.02973(14) .52136(6) -.24674(13) .0406(3) Uani d . 1 . . Cl Cl2 .23832(14) .55820(6) .11330(14) .0459(3) Uani d . 1 . . Cl P1 .16725(13) .40280(5) .02986(12) .0292(2) Uani d . 1 . . P C1 .3804(5) .4102(2) .1714(5) .0343(9) Uani d . 1 . . C C2 .5065(6) .3981(3) .1369(6) .0509(12) Uani d . 1 . . C H2A .4798 .3867 .0331 .042 Uiso d . 1 . . H C3 .6625(7) .4013(3) .2523(8) .0691(17) Uani d . 1 . . C H3A .7317 .3842 .2281 .062 Uiso d . 1 . . H C4 .6988(6) .4155(3) .4024(7) .0661(17) Uani d . 1 . . C H4A .8052 .4218 .4886 .081 Uiso d . 1 . . H C5 .5765(6) .4273(3) .4389(6) .0650(16) Uani d . 1 . . C H5A .5996 .4369 .5414 .078 Uiso calc R 1 . . H C6 .4184(6) .4251(3) .3236(6) .0555(14) Uani d . 1 . . C H6A .3359 .4339 .3493 .067 Uiso calc R 1 . . H C7 .1138(5) .32993(19) .0984(5) .0350(10) Uani d . 1 . . C C8 -.0207(6) .3227(2) .1166(7) .0556(14) Uani d . 1 . . C H8A -.0932 .3564 .0923 .067 Uiso calc R 1 . . H C9 -.0518(8) .2658(3) .1709(8) .0722(18) Uani d . 1 . . C H9A -.1450 .2623 .1826 .087 Uiso calc R 1 . . H C10 .0460(7) .2166(3) .2065(8) .0685(17) Uani d . 1 . . C H10A .0247 .1792 .2459 .082 Uiso calc R 1 . . H C11 .1791(8) .2218(3) .1842(9) .0893(19) Uani d . 1 . . C H11A .2588 .1883 .2088 .105 Uiso d . 1 . . H C12 .2146(7) .2783(3) .1329(8) .0730(15) Uani d . 1 . . C H12A .3101 .2831 .1071 .091 Uiso d . 1 . . H C13 .1654(5) .3819(2) -.1535(5) .0331(9) Uani d . 1 . . C C14 .0885(6) .3280(2) -.2372(6) .0487(12) Uani d . 1 . . C H14A .0412 .2996 -.1963 .058 Uiso calc R 1 . . H C15 .0816(7) .3160(3) -.3819(6) .0635(15) Uani d . 1 . . C H15A .0293 .2796 -.4373 .076 Uiso calc R 1 . . H C16 .1505(7) .3570(3) -.4435(6) .0644(16) Uani d . 1 . . C H16A .1449 .3486 -.5408 .077 Uiso calc R 1 . . H C17 .2274(8) .4103(3) -.3629(6) .0604(16) Uani d . 1 . . C H17A .2790 .4386 -.3868 .071 Uiso d . 1 . . H C18 .2355(6) .4237(2) -.2182(6) .0483(12) Uani d . 1 . . C H18A .2875 .4605 -.1644 .058 Uiso calc R 1 . . H 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 Os1 .02432(12) .02939(13) .02396(12) -.00038(10) .00847(9) .00007(9) Cl1 .0425(6) .0490(6) .0307(6) .0083(5) .0172(5) .0058(5) Cl2 .0336(6) .0444(7) .0474(7) -.0097(5) .0081(5) -.0006(5) P1 .0265(5) .0317(6) .0287(5) .0011(4) .0121(4) .0014(4) C1 .025(2) .036(2) .038(2) -.0007(18) .0118(19) .0014(18) C2 .034(3) .071(3) .048(3) -.004(2) .018(2) -.007(2) C3 .035(3) .094(5) .080(4) .006(3) .027(3) -.001(4) C4 .031(3) .074(4) .069(4) .005(3) .001(3) -.012(3) C5 .044(3) .097(5) .036(3) .013(3) .003(2) -.007(3) C6 .032(3) .086(4) .038(3) .015(3) .007(2) .002(3) C7 .032(2) .033(2) .038(2) -.0003(19) .015(2) .0032(18) C8 .048(3) .041(3) .087(4) .003(2) .039(3) .010(3) C9 .065(4) .051(3) .118(6) -.002(3) .056(4) .016(3) C10 .056(4) .051(3) .097(5) -.003(3) .034(4) .025(3) C11 .065(4) .074(5) .107(5) .010(3) .021(4) .049(4) C12 .049(3) .073(4) .093(3) .012(3) .028(3) .040(3) C13 .030(2) .040(2) .028(2) .0116(18) .0121(18) .0027(18) C14 .041(3) .056(3) .049(3) .004(2) .021(2) -.004(2) C15 .055(4) .075(4) .050(3) .007(3) .015(3) -.020(3) C16 .069(4) .090(5) .035(3) .024(3) .025(3) .004(3) C17 .076(4) .069(4) .051(3) .024(3) .042(3) .020(3) C18 .062(3) .045(3) .046(3) .015(2) .033(3) .008(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Os1 Cl1 3_565 2.3044(11) ? Os1 Cl1 . 2.3044(11) ? Os1 Cl2 3_565 2.3220(11) ? Os1 Cl2 . 2.3220(11) ? Os1 P1 3_565 2.5007(11) ? Os1 P1 . 2.5007(11) ? P1 C13 . 1.811(4) ? P1 C7 . 1.822(4) ? P1 C1 . 1.829(4) ? C1 C6 . 1.375(6) ? C1 C2 . 1.385(6) ? C2 C3 . 1.367(7) ? C3 C4 . 1.356(8) ? C4 C5 . 1.363(7) ? C5 C6 . 1.380(7) ? C7 C8 . 1.354(6) ? C7 C12 . 1.370(7) ? C8 C9 . 1.385(7) ? C9 C10 . 1.314(8) ? C10 C11 . 1.359(8) ? C11 C12 . 1.381(8) ? C13 C14 . 1.380(6) ? C13 C18 . 1.400(6) ? C14 C15 . 1.387(7) ? C15 C16 . 1.362(8) ? C16 C17 . 1.360(8) ? C17 C18 . 1.388(7) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle Cl1 Os1 Cl1 3_565 . 180.00(6) Cl1 Os1 Cl2 3_565 3_565 90.95(4) Cl1 Os1 Cl2 . 3_565 89.05(4) Cl1 Os1 Cl2 3_565 . 89.05(4) Cl1 Os1 Cl2 . . 90.95(4) Cl2 Os1 Cl2 3_565 . 180.00(5) Cl1 Os1 P1 3_565 3_565 92.81(4) Cl1 Os1 P1 . 3_565 87.19(4) Cl2 Os1 P1 3_565 3_565 87.76(4) Cl2 Os1 P1 . 3_565 92.24(4) Cl1 Os1 P1 3_565 . 87.19(4) Cl1 Os1 P1 . . 92.81(4) Cl2 Os1 P1 3_565 . 92.24(4) Cl2 Os1 P1 . . 87.76(4) P1 Os1 P1 3_565 . 180.0 C13 P1 C7 . . 105.6(2) C13 P1 C1 . . 105.37(19) C7 P1 C1 . . 100.8(2) C13 P1 Os1 . . 111.06(13) C7 P1 Os1 . . 117.60(14) C1 P1 Os1 . . 115.10(14) C6 C1 C2 . . 117.8(4) C6 C1 P1 . . 118.1(3) C2 C1 P1 . . 124.0(3) C3 C2 C1 . . 120.1(5) C4 C3 C2 . . 121.7(5) C3 C4 C5 . . 119.1(5) C4 C5 C6 . . 120.0(5) C1 C6 C5 . . 121.3(5) C8 C7 C12 . . 117.1(4) C8 C7 P1 . . 124.4(3) C12 C7 P1 . . 118.5(4) C7 C8 C9 . . 120.9(5) C10 C9 C8 . . 122.2(5) C9 C10 C11 . . 118.1(5) C10 C11 C12 . . 120.9(6) C7 C12 C11 . . 120.8(5) C14 C13 C18 . . 118.4(4) C14 C13 P1 . . 122.3(3) C18 C13 P1 . . 119.1(3) C13 C14 C15 . . 120.4(5) C16 C15 C14 . . 120.7(5) C17 C16 C15 . . 120.0(5) C16 C17 C18 . . 120.7(5) C17 C18 C13 . . 119.9(5) _cod_database_fobs_code 2200532