#------------------------------------------------------------------------------ #$Date: 2009-11-14 14:09:05 +0100 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003282.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_2003282 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 401 _journal_page_last 403 _publ_section_title ; 8-(Ph~2~PCH~2~CH~2~PPh~2~)-8,7-nido-RhSB~9~H~10~.2CH~2~Cl~2~ ; _chemical_formula_moiety 'C28 H38 B9 Cl4 P2 Rh1 S1' _chemical_formula_sum 'C28 H38 B9 Cl4 P2 Rh1 S1' _chemical_formula_weight 810.63 loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 11.161(2) _cell_length_b 11.338(6) _cell_length_c 17.206(13) _cell_angle_alpha 98.726(56) _cell_angle_beta 107.306(40) _cell_angle_gamma 111.682(39) _cell_volume 1845.8 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_meas ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 10 _exptl_absorpt_coefficient_mu 0.91 _cell_measurement_temperature 210(1) _exptl_crystal_description 'rhombic block' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_size_rad ? _exptl_crystal_colour 'orange' _chemical_compound_source ;slow diffusion of n-hexane into dichloromethane solution at 243 K ; _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w-2\q' _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 6131 _reflns_number_total 5771 _reflns_number_observed 5364 _reflns_observed_criterion F>=2.0\s(F) _diffrn_reflns_av_R_equivalents 0.2280 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 480 _diffrn_standards_decay_% <3.5 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.0528 _refine_ls_wR_factor_obs 0.0846 _refine_ls_goodness_of_fit_obs 1.618 _refine_ls_number_reflns 5364 _refine_ls_number_parameters 359 _refine_ls_hydrogen_treatment 'H atoms: see text' _refine_ls_weighting_scheme '1/[\s^2^(F)+0.000391F^2^]' _refine_ls_shift/esd_max 0.001 _refine_diff_density_max '0.83 (near Rh,S)' _refine_diff_density_min -1.14 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _atom_type_scat_source 'IntTabIV(Rh);SHELX76 (Sheldrick, 1976)' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Rh(8) .10159(4) .23566(4) .18360(2) .0225(3) S(7) .11964(15) .23326(4) .04986(9) .0329(9) B(1) .4036(7) .2508(6) .1661(4) .034(4) B(2) .3064(7) .2417(6) .0623(5) .040(5) B(3) .2224(7) .1522(6) .1292(4) .036(4) B(4) .3169(7) .2520(7) .2379(4) .035(4) B(5) .4478(7) .4029(7) .2413(4) .038(5) B(6) .4354(7) .3974(6) .1346(5) .040(5) B(9) .2969(7) .4072(6) .2532(4) .031(4) B(10) .3738(7) .4957(6) .1842(5) .039(5) B(11) .2809(8) .3938(7) .0706(5) .048(5) P(1) -.06066(14) .32101(13) .17119(9) .0268(9) P(2) .06739(14) .20171(13) .30155(9) .0253(9) C(1) -.1253(6) .3010(6) .2570(3) .034(4) C(2) -.0118(6) .3051(5) .3363(3) .030(4) C(11) .0233(4) .4997(3) .18605(18) .032(4) C(12) .0528(4) .5403(3) .11858(18) .042(4) C(13) .1266(4) .6749(3) .12856(18) .051(5) C(14) .1709(4) .7690(4) .20602(18) .055(5) C(15) .1414(4) .7285(3) .27350(18) .059(5) C(16) .0676(4) .5938(3) .26352(18) .044(4) C(21) -.2162(3) .2552(3) .0744(2) .028(3) C(22) -.2937(3) .3264(3) .0542(2) .036(4) C(23) -.4158(3) .2711(3) -.0191(2) .045(5) C(24) -.4603(3) .1445(3) -.0722(2) .048(5) C(25) -.3828(3) .0733(3) -.0520(2) .059(5) C(26) -.2607(3) .1286(3) .0213(2) .042(4) C(31) .2028(4) .2187(3) .3993(2) .031(4) C(32) .2954(4) .3439(3) .4569(2) .036(4) C(33) .4010(4) .3566(3) .5305(2) .048(5) C(34) .4139(4) .2439(3) .5465(2) .054(5) C(35) .3213(4) .1187(3) .4889(2) .060(6) C(36) .2158(4) .1061(3) .4153(2) .045(5) C(41) -.0651(4) .0311(3) .2671(2) .029(4) C(42) -.1699(4) -.0077(4) .2992(2) .037(4) C(43) -.2717(4) -.1392(3) .2695(2) .047(5) C(44) -.2686(4) -.2319(3) .2077(2) .049(5) C(45) -.1637(4) -.1931(3) .1756(2) .043(4) C(46) -.0620(4) -.0616(3) .2053(2) .042(4) C(1S) .8552(7) .6712(7) .3824(4) .053(5) Cl(1S) .88088(18) .54710(16) .42582(10) .0528(12) Cl(2S) .9828(2) .83078(18) .44954(14) .0727(15) C(2S) .5842(8) .2122(9) .3942(6) .079(7) Cl(3S) .5329(4) .0492(3) .3362(2) .145(3) Cl(4S) .7290(3) .2621(3) .4889(3) .144(3) H(1) .47647 .20521 .17341 0.063(4) H(2) .31065 .19527 .00279 0.063(4) H(3) .16956 .04300 .11133 0.063(4) H(4) .32811 .21083 .29217 0.063(4) H(5) .54515 .46145 .29795 0.063(4) H(6) .52686 .45302 .12056 0.063(4) H(9) .29475 .46213 .31090 0.063(4) H(10) .41791 .60461 .20129 0.063(4) H(11) .26993 .44136 .01957 0.063(4) H(0) .27615 .47601 .19069 0.063(4) H(1A) -.2164 .2068 .2355 0.063(4) H(1B) -.1530 .3805 .2734 0.063(4) H(2A) .0671 .4062 .3683 0.063(4) H(2B) -.0585 .2667 .3792 0.063(4) H(12) .0186 .4674 .05861 0.063(4) H(13) .1495 .7063 .07632 0.063(4) H(14) .2280 .8733 .21375 0.063(4) H(15) .1756 .8013 .33347 0.063(4) H(16) .0447 .5624 .31576 0.063(4) H(22) -.2592 .4245 .09527 0.063(4) H(23) -.4759 .3263 -.03742 0.063(4) H(24) -.5549 .1017 -.12889 0.063(4) H(25) -.4172 -.0247 -.09309 0.063(4) H(26) -.2006 .0734 .03690 0.063(4) H(32) .2854 .4311 .44449 0.063(4) H(33) .4726 .4535 .57515 0.063(4) H(34) .4956 .2537 .60355 0.063(4) H(35) .3313 .0315 .50129 0.063(4) H(36) .1441 .0091 .37064 0.063(4) H(42) -.1724 .0641 .34699 0.063(4) H(43) -.3529 -.1692 .29434 0.063(4) H(44) -.3474 -.3337 .18474 0.063(4) H(45) -.1613 -.2649 .12780 0.063(4) H(46) .0192 -.0316 .18045 0.063(4) H(1S) .8629 .6573 .3209 0.063(4) H(2S) .7527 .6632 .3751 0.063(4) H(3S) .6113 .2776 .3563 0.063(4) H(4S) .4987 .2175 .4092 0.063(4)