#------------------------------------------------------------------------------ #$Date: 2008-01-13 23:15:36 +0100 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2002998.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_2002998 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 1998 _journal_volume B54 _journal_page_first 443 _journal_page_last 449 _publ_section_title ; Refinement of Twinned Structures with SHELXL-97 ; loop_ _publ_author_name 'Herbst-Irmer, Regine' 'Sheldrick, George M. ' _chemical_formula_sum 'C57 H52 Cl O2 Os P3' _chemical_formula_weight 1087.55 _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 31' _symmetry_space_group_name_Hall 'P 31' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 12.623(2) _cell_length_b 12.623(2) _cell_length_c 26.325(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3632.7(11) _cell_formula_units_Z 3 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _cell_measurement_temperature 293(2) _exptl_crystal_description blocks _exptl_crystal_colour 'not recorded' _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .20 _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1644 _exptl_absorpt_coefficient_mu 2.829 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min .4840 _exptl_absorpt_correction_T_max .6015 _diffrn_ambient_temperature 293(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method 'omega-2 theta' _diffrn_reflns_number 6576 _diffrn_reflns_av_R_equivalents .0671 _diffrn_reflns_av_sigmaI/netI .0806 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _reflns_number_total 4384 _reflns_number_gt 3802 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all .0589 _refine_ls_R_factor_gt .0462 _refine_ls_wR_factor_ref .1019 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all .946 _refine_ls_number_reflns 4384 _refine_ls_number_parameters 606 _refine_ls_number_restraints 1354 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+8.2393P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_diff_density_max 1.190 _refine_diff_density_min -.977 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef .00083(11) _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack .026(13) 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' 'O' 'O' .0106 .0060 '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_ _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 .11632(6) .37628(6) .50058(6) .03443(14) Uani d . 1 . . Os Cl1 .2110(4) .3740(4) .41885(18) .0529(11) Uani d . 1 . . Cl C1 .0602(17) .3737(13) .5653(10) .057(6) Uani d . 1 . . C O1 .0255(17) .3792(13) .6018(5) .078(5) Uani d . 1 . . O P1 .0545(4) .1643(4) .50377(18) .0370(11) Uani d . 1 . . P C111 .1869(13) .1407(13) .5220(5) .041(3) Uani d DU 1 . . C C112 .2989(13) .2105(14) .4985(6) .060(5) Uani d DU 1 . . C H112 .3088 .2681 .4742 .072 Uiso calc R 1 . . H C113 .3954(14) .1945(15) .5113(7) .073(5) Uani d DU 1 . . C H113 .4703 .2407 .4950 .087 Uiso calc R 1 . . H C114 .3829(15) .1124(17) .5472(7) .071(5) Uani d DU 1 . . C H114 .4499 .1049 .5565 .085 Uiso calc R 1 . . H C115 .2729(15) .0410(15) .5695(6) .070(5) Uani d DU 1 . . C H115 .2632 -.0186 .5928 .085 Uiso calc R 1 . . H C116 .1750(14) .0566(16) .5576(7) .063(5) Uani d DU 1 . . C H116 .1004 .0096 .5740 .076 Uiso calc R 1 . . H C121 -.0016(12) .0704(11) .4475(5) .035(3) Uani d DU 1 . . C C122 -.0743(13) .0898(14) .4141(5) .050(4) Uani d DU 1 . . C H122 -.0861 .1561 .4192 .060 Uiso calc R 1 . . H C123 -.1299(15) .0134(15) .3735(6) .066(5) Uani d DU 1 . . C H123 -.1789 .0280 .3515 .079 Uiso calc R 1 . . H C124 -.1129(17) -.0829(15) .3658(6) .069(5) Uani d DU 1 . . C H124 -.1499 -.1340 .3381 .083 Uiso calc R 1 . . H C125 -.0429(17) -.1060(14) .3977(6) .068(5) Uani d DU 1 . . C H125 -.0320 -.1727 .3922 .081 Uiso calc R 1 . . H C126 .0121(15) -.0294(13) .4385(6) .047(4) Uani d DU 1 . . C H126 .0599 -.0456 .4605 .057 Uiso calc R 1 . . H C131 -.0562(14) .0672(13) .5510(5) .046(4) Uani d DU 1 . . C C132 -.1552(14) -.0443(13) .5394(5) .052(4) Uani d DU 1 . . C H132 -.1685 -.0695 .5056 .063 Uiso calc R 1 . . H C133 -.2360(15) -.1209(15) .5758(6) .074(5) Uani d DU 1 . . C H133 -.3018 -.1964 .5666 .089 Uiso calc R 1 . . H C134 -.2179(16) -.0844(15) .6250(6) .066(5) Uani d DU 1 . . C H134 -.2711 -.1351 .6500 .079 Uiso calc R 1 . . H C135 -.1220(15) .0263(16) .6375(6) .065(5) Uani d DU 1 . . C H135 -.1127 .0533 .6710 .079 Uiso calc R 1 . . H C136 -.0388(14) .0990(14) .6018(5) .050(4) Uani d DU 1 . . C H136 .0306 .1709 .6119 .060 Uiso calc R 1 . . H P2 -.0598(4) .3876(4) .46636(16) .0435(10) Uani d . 1 . . P C211 -.0653(17) .4413(18) .4023(5) .055(4) Uani d DU 1 . . C C212 -.1281(16) .5015(17) .3908(6) .075(5) Uani d DU 1 . . C H212 -.1697 .5165 .4164 .090 Uiso calc R 1 . . H C213 -.130(2) .539(2) .3426(7) .093(7) Uani d DU 1 . . C H213 -.1742 .5780 .3353 .112 Uiso calc R 1 . . H C214 -.068(2) .520(2) .3051(7) .100(7) Uani d DU 1 . . C H214 -.0630 .5523 .2729 .120 Uiso calc R 1 . . H C215 -.0126(19) .4539(19) .3144(5) .087(6) Uani d DU 1 . . C H215 .0212 .4320 .2879 .105 Uiso calc R 1 . . H C216 -.0066(15) .4192(17) .3632(5) .069(5) Uani d DU 1 . . C H216 .0377 .3800 .3699 .082 Uiso calc R 1 . . H C221 -.2046(15) .2434(18) .4663(9) .095(7) Uani d DU 1 . . C C222 -.2356(15) .1721(16) .5090(9) .094(7) Uani d DU 1 . . C H222 -.1804 .1982 .5358 .113 Uiso calc R 1 . . H C223 -.3430(17) .0649(15) .5141(9) .114(8) Uani d DU 1 . . C H223 -.3605 .0189 .5437 .137 Uiso calc R 1 . . H C224 -.4242(19) .027(2) .4748(10) .158(12) Uani d DU 1 . . C H224 -.4991 -.0452 .4777 .189 Uiso calc R 1 . . H C225 -.3960(17) .0932(19) .4314(10) .134(9) Uani d DU 1 . . C H225 -.4483 .0627 .4037 .161 Uiso calc R 1 . . H C226 -.2907(16) .2056(17) .4279(9) .115(8) Uani d DU 1 . . C H226 -.2777 .2555 .3999 .137 Uiso calc R 1 . . H C231 -.0908(17) .4881(16) .5073(6) .049(4) Uani d DU 1 . . C C232 -.1647(16) .4473(16) .5492(6) .074(5) Uani d DU 1 . . C H232 -.2056 .3640 .5565 .089 Uiso calc R 1 . . H C233 -.181(2) .5239(19) .5809(6) .088(6) Uani d DU 1 . . C H233 -.2298 .4929 .6096 .105 Uiso calc R 1 . . H C234 -.125(2) .6453(18) .5704(8) .093(7) Uani d DU 1 . . C H234 -.1380 .6978 .5910 .111 Uiso calc R 1 . . H C235 -.051(2) .6882(15) .5291(7) .075(6) Uani d DU 1 . . C H235 -.0139 .7709 .5211 .090 Uiso calc R 1 . . H C236 -.031(2) .6123(17) .4994(6) .075(7) Uani d DU 1 . . C H236 .0254 .6454 .4730 .090 Uiso calc R 1 . . H P3 .2650(4) .5875(4) .50199(18) .0364(11) Uani d . 1 . . P C311 .2538(14) .6947(12) .4595(5) .040(4) Uani d DU 1 . . C C312 .2614(12) .8030(11) .4748(5) .044(4) Uani d DU 1 . . C H312 .2717 .8239 .5090 .053 Uiso calc R 1 . . H C313 .2539(16) .8798(14) .4404(5) .057(3) Uani d DU 1 . . C H313 .2591 .9519 .4519 .068 Uiso calc R 1 . . H C314 .2391(16) .8549(13) .3902(5) .058(4) Uani d DU 1 . . C H314 .2348 .9085 .3672 .069 Uiso calc R 1 . . H C315 .2306(18) .7480(15) .3746(6) .064(5) Uani d DU 1 . . C H315 .2204 .7286 .3402 .076 Uiso calc R 1 . . H C316 .2367(16) .6683(14) .4083(5) .049(4) Uani d DU 1 . . C H316 .2292 .5954 .3965 .058 Uiso calc R 1 . . H C321 .4170(11) .6137(11) .4868(5) .040(4) Uani d DU 1 . . C C322 .4962(12) .7076(12) .4566(5) .048(4) Uani d DU 1 . . C H322 .4703 .7568 .4411 .058 Uiso calc R 1 . . H C323 .6130(13) .7310(16) .4486(5) .065(4) Uani d DU 1 . . C H323 .6660 .7971 .4285 .078 Uiso calc R 1 . . H C324 .6523(15) .6587(17) .4697(7) .071(5) Uani d DU 1 . . C H324 .7303 .6720 .4628 .085 Uiso calc R 1 . . H C325 .5759(15) .5664(18) .5013(8) .078(6) Uani d DU 1 . . C H325 .6038 .5196 .5175 .093 Uiso calc R 1 . . H C326 .4578(13) .5414(15) .5095(7) .057(5) Uani d DU 1 . . C H326 .4057 .4762 .5302 .069 Uiso calc R 1 . . H C331 .2897(12) .6645(13) .5641(5) .045(4) Uani d DU 1 . . C C332 .4051(14) .7358(14) .5831(6) .060(4) Uani d DU 1 . . C H332 .4724 .7421 .5659 .072 Uiso calc R 1 . . H C333 .4210(16) .7983(16) .6281(6) .072(6) Uani d DU 1 . . C H333 .4993 .8479 .6410 .086 Uiso calc R 1 . . H C334 .3224(16) .7876(18) .6536(6) .075(5) Uani d DU 1 . . C H334 .3335 .8261 .6848 .090 Uiso calc R 1 . . H C335 .2085(16) .7216(17) .6341(6) .069(5) Uani d DU 1 . . C H335 .1419 .7173 .6511 .082 Uiso calc R 1 . . H C336 .1926(14) .6611(16) .5890(6) .054(4) Uani d DU 1 . . C H336 .1146 .6170 .5750 .064 Uiso calc R 1 . . H C1S .772(5) .558(5) .036(2) .074(14) Uani d PDU .50 A 1 C H1S1 .7738 .5942 .0680 .112 Uiso calc PR .50 A 1 H H1S2 .6908 .4911 .0295 .112 Uiso calc PR .50 A 1 H H1S3 .7927 .6188 .0094 .112 Uiso calc PR .50 A 1 H C2S .874(5) .507(6) .035(2) .118(13) Uani d PDU .50 A 1 C H2S1 .9542 .5751 .0432 .142 Uiso calc PR .50 A 1 H H2S2 .8514 .4463 .0617 .142 Uiso calc PR .50 A 1 H O3S .880(3) .452(3) -.0149(18) .165(19) Uani d PDU .50 A 1 O H3S .8127 .3927 -.0212 .248 Uiso calc PR .50 A 1 H C1'S .900(5) .456(5) .044(3) .106(14) Uani d PDU .50 B 2 C H1'1 .9464 .4704 .0746 .160 Uiso calc PR .50 B 2 H H1'2 .9537 .4794 .0151 .160 Uiso calc PR .50 B 2 H H1'3 .8392 .3714 .0415 .160 Uiso calc PR .50 B 2 H C2'S .831(5) .541(5) .0450(18) .097(11) Uani d PDU .50 B 2 C H2'1 .7795 .5192 .0750 .117 Uiso calc PR .50 B 2 H H2'2 .8932 .6265 .0483 .117 Uiso calc PR .50 B 2 H O3'S .753(3) .528(3) -.0007(17) .127(17) Uani d PDU .50 B 2 O H3'S .6831 .4730 .0043 .190 Uiso calc PR .50 B 2 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 .0294(4) .0331(4) .0393(2) .0145(4) .0016(4) -.0003(4) Cl1 .048(2) .050(3) .058(3) .023(2) -.001(2) -.003(2) C1 .053(11) .007(8) .103(18) .008(8) -.024(11) -.002(9) O1 .121(15) .054(9) .054(9) .041(10) .020(9) -.004(7) P1 .035(2) .037(3) .038(3) .018(2) .003(2) -.0007(19) C111 .045(8) .045(9) .036(8) .025(8) -.007(7) -.010(6) C112 .036(9) .057(12) .094(14) .028(9) .006(9) .003(9) C113 .047(9) .076(13) .103(15) .037(10) -.003(9) -.007(9) C114 .079(10) .104(14) .074(12) .079(11) -.007(9) -.020(9) C115 .091(12) .096(14) .065(11) .077(11) -.001(10) -.003(8) C116 .065(10) .076(12) .066(12) .049(10) .000(9) .014(8) C121 .037(9) .028(7) .040(8) .017(7) .006(6) .009(6) C122 .047(10) .056(10) .050(10) .028(8) -.005(8) .002(7) C123 .055(11) .061(11) .055(10) .007(9) -.005(8) -.001(9) C124 .058(12) .054(10) .052(10) -.003(9) .016(8) -.008(8) C125 .090(14) .029(9) .066(11) .015(9) .027(9) .002(7) C126 .051(10) .039(9) .056(10) .025(8) .009(8) .010(7) C131 .053(10) .044(8) .057(8) .037(7) .020(8) .013(7) C132 .071(11) .051(9) .044(8) .036(7) .007(7) .011(7) C133 .054(11) .076(11) .075(9) .020(9) .011(10) .027(8) C134 .052(10) .095(12) .060(8) .044(8) .019(9) .047(9) C135 .054(10) .107(13) .055(9) .055(8) .018(8) .010(8) C136 .053(10) .058(9) .053(8) .039(7) .009(7) .005(7) P2 .029(2) .043(3) .055(2) .015(2) .005(2) -.001(2) C211 .055(11) .073(12) .052(8) .043(8) -.008(9) -.002(10) C212 .075(13) .116(16) .064(9) .071(11) -.039(10) -.015(11) C213 .108(17) .140(19) .069(11) .091(14) -.030(12) -.001(13) C214 .086(16) .16(2) .078(11) .078(15) -.026(11) -.008(13) C215 .091(15) .145(19) .047(7) .074(13) -.023(10) -.028(9) C216 .062(11) .095(13) .054(8) .043(10) -.013(8) -.019(9) C221 .030(10) .076(15) .18(2) .030(9) -.002(10) -.019(12) C222 .030(9) .032(10) .22(2) .017(7) .022(11) -.006(11) C223 .042(10) .019(9) .28(2) .014(7) .008(13) -.024(12) C224 .043(13) .070(16) .31(3) -.009(12) -.012(15) -.024(15) C225 .030(11) .070(15) .29(3) .013(9) -.018(15) -.042(15) C226 .030(10) .062(13) .24(2) .014(8) -.031(12) -.042(13) C231 .061(11) .062(9) .047(9) .049(10) -.009(8) -.021(8) C232 .118(16) .080(11) .053(11) .071(12) .007(9) .005(9) C233 .129(18) .117(13) .066(12) .098(14) .033(12) .012(11) C234 .124(19) .103(12) .096(15) .090(15) .013(12) -.020(13) C235 .112(16) .053(10) .080(13) .055(11) -.015(10) -.013(9) C236 .106(16) .075(10) .034(10) .037(11) .005(9) -.026(9) P3 .032(3) .028(2) .046(3) .012(2) -.001(2) -.0026(19) C311 .042(9) .030(7) .048(7) .017(7) .001(8) -.001(7) C312 .035(8) .046(8) .048(8) .018(8) .002(7) -.007(6) C313 .059(10) .040(9) .075(8) .028(9) .012(10) .005(8) C314 .047(10) .050(9) .069(8) .019(9) -.009(10) .016(7) C315 .068(12) .069(11) .054(9) .034(10) -.014(10) -.002(7) C316 .058(11) .053(9) .041(8) .032(9) .005(8) -.002(7) C321 .026(7) .032(8) .052(10) .007(6) .007(6) .009(7) C322 .035(7) .065(10) .019(7) .006(8) -.005(6) .008(6) C323 .040(8) .070(11) .062(9) .010(9) .019(9) .010(9) C324 .043(10) .085(13) .080(13) .029(9) .005(9) -.014(9) C325 .035(8) .072(13) .126(15) .027(8) -.014(9) .011(10) C326 .040(9) .059(11) .075(13) .027(9) -.007(9) .003(9) C331 .058(9) .035(9) .030(8) .014(7) .003(6) .000(6) C332 .058(8) .057(11) .054(10) .020(8) -.005(9) -.011(9) C333 .076(10) .064(12) .066(12) .028(11) -.015(9) -.023(9) C334 .097(12) .075(13) .053(11) .043(12) .000(9) -.011(9) C335 .084(10) .072(12) .045(10) .036(10) .015(9) -.002(8) C336 .063(9) .061(11) .043(9) .035(9) .005(8) .006(8) C1S .05(3) .08(3) .11(4) .03(2) .02(3) .00(3) C2S .06(2) .12(3) .18(3) .061(18) .01(2) -.07(2) O3S .055(19) .08(2) .27(4) -.033(16) .09(2) -.12(3) C1'S .06(3) .06(3) .20(4) .025(17) -.02(3) .04(3) C2'S .04(2) .13(3) .14(3) .053(17) -.05(2) -.03(2) O3'S .07(2) .09(2) .16(3) -.004(17) -.06(2) .08(2)