#------------------------------------------------------------------------------ #$Date: 2008-03-04 17:31:11 +0000 (Tue, 04 Mar 2008) $ #$Revision: 226 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003689.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_2003689 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1275 _journal_page_last 1278 _publ_section_title ; A Hexacobalt Sulfide Cluster Compound, [Co~6~(\m-S)~8~(PPh~3~)~6~].2PPh~3~.2C~2~H~4~Cl~2~.H~2~O ; _chemical_formula_moiety 'C108 H90 Co6 P6 S8 , 2C18 H15 P , 2C2 H4 Cl2 , H2' _chemical_formula_sum 'C148 H130 Cl4 Co6 O P8 S8' _chemical_formula_weight 2924.34 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 15.347(7) _cell_length_b 17.493(5) _cell_length_c 15.0003(8) _cell_angle_alpha 102.80(3) _cell_angle_beta 116.77(3) _cell_angle_gamma 79.94(3) _cell_volume 3494(3) _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.39 _exptl_crystal_density_meas ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 6 _cell_measurement_theta_max 12 _exptl_absorpt_coefficient_mu 1.026 _cell_measurement_temperature 296 _exptl_crystal_description 'pyramid' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_size_rad ? _exptl_crystal_colour 'black' _chemical_compound_source ? _diffrn_measurement_device 'Rigaku MSC/AFC-5R' _diffrn_measurement_method '\w/2\q' _exptl_absorpt_correction_type 'empirical (DIFABS; Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.866 _exptl_absorpt_correction_T_max 1.000 _diffrn_reflns_number 12793 _reflns_number_total 12280 _reflns_number_observed 6624 _reflns_observed_criterion I>3\s(I) _diffrn_reflns_av_R_equivalents 0.065 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.2 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.058 _refine_ls_wR_factor_obs 0.069 _refine_ls_goodness_of_fit_obs 1.40 _refine_ls_number_reflns 6624 _refine_ls_number_parameters 811 _refine_ls_hydrogen_treatment 'noref' _refine_ls_weighting_scheme 'unit' _refine_ls_shift/esd_max 0.41 _refine_diff_density_max 0.97 _refine_diff_density_min -0.63 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _atom_type_scat_source 'IntTabIV' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_B_iso_or_equiv Co(1) .05075(7) -.09951(6) -.06549(8) 1.77(4) Co(2) .12968(7) .00054(6) .12862(8) 1.78(4) Co(3) .05463(7) .06532(6) -.05566(8) 1.81(4) S(1) .1779(1) -.0265(1) .0046(1) 2.05(7) S(2) .0996(1) .1243(1) .1024(1) 2.00(7) S(3) .0171(1) .0262(1) .1888(1) 2.04(8) S(4) .0968(1) -.1251(1) .0914(2) 2.12(7) P(1) .0780(2) -.2002(1) -.1655(2) 2.13(8) P(2) .2686(2) -.0018(1) .2619(2) 2.15(8) P(3) .1175(2) .1463(1) -.0952(2) 2.30(8) C(111) .1470(6) -.2882(5) -.1092(6) 2.7(3) C(112) .2209(7) -.2774(5) -.0135(7) 3.5(4) C(113) .2802(8) -.3417(6) .0313(8) 5.4(5) C(114) .2646(9) -.4167(6) -.0224(9) 5.2(5) C(115) .1918(8) -.4293(5) -.1173(8) 4.6(5) C(116) .1335(7) -.3645(5) -.1622(7) 3.7(4) C(121) -.0337(6) -.2387(5) -.2694(6) 2.7(3) C(122) -.0842(7) -.2909(5) -.2583(7) 3.7(4) C(123) -.1675(8) -.3195(6) -.338(1) 5.4(5) C(124) -.2034(9) -.2942(9) -.427(1) 7.2(6) C(125) -.159(1) -.2396(8) -.4403(8) 6.0(6) C(126) -.0736(7) -.2109(6) -.3619(8) 4.2(4) C(131) .1486(6) -.1887(5) -.2335(6) 2.7(3) C(132) .1974(7) -.1235(5) -.2090(6) 3.4(4) C(133) .2518(8) -.1174(6) -.2610(8) 4.5(5) C(134) .2562(8) -.1771(7) -.3360(8) 4.6(5) C(135) .2088(8) -.2434(6) -.3598(7) 4.2(5) C(136) .1544(7) -.2494(5) -.3090(7) 3.7(4) C(211) .2607(6) .0107(5) .3825(6) 2.5(3) C(212) .3146(7) .0622(5) .4658(7) 3.8(4) C(213) .3120(8) .0661(6) .5581(7) 4.9(5) C(214) .2543(8) .0203(7) .5676(7) 4.9(5) C(215) .2005(7) -.0303(7) .4835(8) 4.7(5) C(216) .2023(6) -.0362(6) .3907(7) 3.5(4) C(221) .3535(6) .0719(5) .2888(6) 2.5(3) C(222) .3186(6) .1498(5) .2900(6) 3.1(3) C(223) .3818(7) .2075(5) .3161(8) 4.3(4) C(224) .4794(8) .1872(6) .3412(9) 4.9(5) C(225) .5138(7) .1101(6) .3411(9) 5.0(5) C(226) .4523(6) .0525(6) .3159(8) 4.1(4) C(231) .3511(6) -.0920(5) .2688(6) 2.6(3) C(232) .3685(7) -.1258(5) .1862(7) 3.9(4) C(233) .4395(8) -.1896(6) .1921(8) 4.7(5) C(234) .4919(8) -.2202(6) .280(1) 4.9(5) C(235) .4734(7) -.1864(6) .3632(8) 4.4(4) C(236) .4035(7) -.1226(5) .3577(7) 3.9(4) C(311) .0651(6) .1545(6) -.2293(6) 3.0(4) C(312) .0642(8) .0859(7) -.2960(7) 4.6(5) C(313) .039(1) .090(1) -.397(1) 6.8(7) C(314) .010(1) .163(1) -.428(1) 8(1) C(315) .009(1) .229(1) -.364(1) 8.5(9) C(316) .0374(8) .2252(7) -.2640(8) 5.7(6) C(321) .2487(6) .1239(5) -.0657(7) 2.7(3) C(322) .3132(7) .1087(5) .0279(8) 3.6(4) C(323) .4116(7) .0927(6) .0522(8) 4.4(4) C(324) .4478(7) .0913(6) -.015(1) 4.9(5) C(325) .3840(9) .1065(7) -.110(1) 5.2(5) C(326) .2845(7) .1243(6) -.1361(7) 4.1(4) C(331) .1134(7) .2508(5) -.0366(7) 2.9(4) C(332) .1875(9) .2964(6) -.013(1) 7.2(6) C(333) .181(1) .3757(7) .024(1) 9.6(8) C(334) .101(1) .4094(6) .040(1) 6.8(6) C(335) .0285(8) .3655(6) .0192(8) 4.4(5) C(336) .0347(7) .2855(5) -.0182(7) 3.6(4) P(01) .4919(4) .4610(3) .7602(4) 4.2(2) P(01') .3104(4) .5210(3) .6742(4) 4.2(2) C(011) .411(1) .430(1) .815(2) 13(1) C(012) .427(1) .393(1) .887(1) 7.9(7) C(013) .361(1) .346(1) .874(1) 10(1) C(014) .279(1) .3384(9) .788(2) 10(1) C(015) .264(1) .378(1) .715(1) 8.9(9) C(016) .327(2) .429(2) .731(2) 14(2) C(021) .436(1) .439(1) .616(1) 12(1) C(022) .362(2) .493(1) .579(1) 10(1) C(023) .327(1) .5064(8) .484(1) 7.5(7) C(024) .362(1) .463(1) .421(1) 6.7(8) C(025) .435(1) .4070(9) .453(1) 7.2(8) C(026) .472(1) .3935(8) .551(1) 7.5(7) C(031) .483(2) .575(1) .786(2) 17(1) C(032) .546(1) .629(2) .813(1) 10(1) C(033) .529(2) .701(1) .860(1) 9(1) C(034) .451(2) .718(1) .874(1) 8.7(9) C(035) .384(1) .664(2) .841(2) 11(1) C(036) .403(1) .595(1) .795(2) 18(1) Cl(1) .7204(4) .2714(3) .5782(3) 10.7(3) Cl(2) .845(1) .4009(6) .7557(8) 15.3(7) Cl(2') .732(1) .4117(6) .7716(7) 13.5(8) C(41) .776(2) .263(1) .707(1) 11(1) C(42) .786(2) .326(2) .772(2) 14(2) O(1W) .974(1) .458(1) .600(2) 11(1) H(1) .2322 -.2256 .0232 4.2 H(2) .3306 -.3335 .0982 6.4 H(3) .3054 -.4602 .0074 6.3 H(4) .1803 -.4813 -.1532 5.6 H(5) .0841 -.3730 -.2297 4.4 H(6) -.0611 -.3075 -.1947 4.4 H(7) -.1999 -.3571 -.3295 6.5 H(8) -.2604 -.3149 -.4822 8.7 H(9) -.1863 -.2209 -.5032 7.1 H(10) -.0425 -.1727 -.3708 5.1 H(11) .1947 -.0824 -.1568 4.1 H(12) .2854 -.0718 -.2444 5.5 H(13) .2923 -.1725 -.3717 5.5 H(14) .2131 -.2851 -.4108 5.1 H(15) .1210 -.2951 -.3257 4.5 H(16) .3541 .0954 .4602 4.6 H(17) .3509 .1012 .6153 5.9 H(18) .2516 .0233 .6303 5.9 H(19) .1601 -.0627 .4890 5.7 H(20) .1639 -.0718 .3339 4.2 H(21) .2511 .1644 .2728 3.7 H(22) .3571 .2613 .3165 5.2 H(23) .5225 .2265 .3586 5.9 H(24) .5815 .0958 .3586 6.0 H(25) .4780 -.0010 .3172 4.9 H(26) .3321 -.1059 .1243 4.7 H(27) .4515 -.2117 .1344 5.7 H(28) .5396 -.2636 .2841 5.9 H(29) .5089 -.2068 .4248 5.3 H(30) .3916 -.1001 .4154 4.6 H(31) .0809 .0365 -.2735 5.6 H(32) .0407 .0433 -.4428 8.2 H(33) -.0092 .1653 -.4972 9.4 H(34) -.0106 .2785 -.3869 10.2 H(35) .0377 .2723 -.2180 6.8 H(36) .2901 .1091 .0772 4.4 H(37) .4553 .0823 .1182 5.3 H(38) .5159 .0801 .0028 5.9 H(39) .4082 .1048 -.1586 6.3 H(40) .2413 .1367 -.2013 4.9 H(41) .2443 .2730 -.0215 8.6 H(42) .2321 .4067 .0382 11.5 H(43) .0960 .4640 .0649 8.1 H(44) -.0270 .3891 .0305 5.2 H(45) -.0162 .2547 -.0312 4.3 H(46) .4855 .3989 .9489 9.5 H(47) .3727 .3175 .9262 11.8 H(48) .2318 .3055 .7793 11.6 H(49) .2089 .3704 .6508 10.7 H(50) .2762 .5470 .4612 9.0 H(51) .3362 .4725 .3532 8.1 H(52) .4613 .3766 .4083 8.6 H(53) .5231 .3528 .5729 9.0 H(54) .6012 .6172 .7980 12.4 H(55) .5751 .7388 .8824 10.4 H(56) .4391 .7684 .9076 10.4 H(57) .3261 .6757 .8508 12.7