#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003745.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_2003745 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1501 _journal_page_last 1503 _publ_section_title ; Di-\m-bromo-3:3'\k^4^Br-bis[\m-(2-phenyl-3-phenylamino-3-sulfido-2-azoniaprop- 2-en-1-yl-3\kS:8\kC^1^)-1,2-dicarba-3-rhoda-closo-dodecaborane], a Novel Dimeric Metallacarborane Containing a Rh~2~Br~2~ Bridging Section and the {-SC(NHPh)-N(Ph)CH~2~-} Ligand ; _chemical_formula_moiety 'C32 H46 B18 Br2 N4 Rh2 S2 ' _chemical_formula_sum 'C32 H46 B18 Br2 N4 Rh2 S2 ' _chemical_formula_weight 1111.05 _symmetry_cell_setting Triclinic loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _symmetry_space_group_name_H-M 'P -1' _cell_length_a 8.2971(11) _cell_length_b 10.0909(13) _cell_length_c 13.863(4) _cell_angle_alpha 78.330(14) _cell_angle_beta 86.203(14) _cell_angle_gamma 87.326(8) _cell_volume 1133.5(4) _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.0 _cell_measurement_theta_max 23.5 _exptl_absorpt_coefficient_mu 2.58 _cell_measurement_temperature 293 _exptl_crystal_description plate _exptl_crystal_size_max 0.375 _exptl_crystal_size_mid 0.153 _exptl_crystal_size_min 0.056 _exptl_crystal_size_rad ? _exptl_crystal_colour orange _chemical_compound_source 'synthesized by the authors' _diffrn_measurement_device 'Nonius CAD-4 ' _diffrn_measurement_method '\q/2\q scans' _exptl_absorpt_correction_type 'empirical, \y-scans at 4\% steps' _exptl_absorpt_correction_T_min 0.7775 _exptl_absorpt_correction_T_max 0.9963 _diffrn_reflns_number 4905 _reflns_number_total 4905 _reflns_number_observed 3318 _reflns_observed_criterion 'Inet > 3.0\s(Inet)' _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_theta_max 26.88 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 'none, variation 1.0' _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.027 _refine_ls_wR_factor_obs 0.033 _refine_ls_wR_factor_all 0.038 _refine_ls_goodness_of_fit_obs 0.97 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 3318 _refine_ls_number_parameters 271 _refine_ls_hydrogen_treatment ;H atoms included as riding atoms, C---H and B---H in C~2~H~11~B~9~ 1.04\%A; other C---H, N---H 0.95\%A ; _refine_ls_weighting_scheme 'w = 1/[\s^2^(F) + 0.0005F^2^]' _refine_ls_shift/esd_max 0.001 _refine_diff_density_max 0.45 _refine_diff_density_min -0.32 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C ? 'International Tables Vol. IV Table 2.2B' 0.002 0.002 H ? 'International Tables Vol. IV Table 2.2B' 0.000 0.000 B ? 'International Tables Vol. IV Table 2.2B' 0.000 0.001 Br ? 'International Tables Vol. IV Table 2.2B' -0.374 2.456 N ? 'International Tables Vol. IV Table 2.2B' 0.004 0.003 Rh ? 'International Tables Vol. IV Table 2.2B' -1.287 0.919 S ? 'International Tables Vol. IV Table 2.2B' 0.110 0.124 'DATRD2 in NRCVAX94 (Gabe, Le Page, Charland, Lee & White, 1989)' ;ORTEPII (Johnson, 1976) as implemented in PLATON (Spek, 1994a) and NRCVAX94 and PLUTON (Spek, 1994b) ; loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Rh3 0.50939(4) 0.48183(3) 0.64116(2) 0.02951(15) Br1 0.28825(5) 0.53550(4) 0.51413(3) 0.0407(2) C1 0.3989(5) 0.2914(4) 0.7058(3) 0.041(2) C2 0.5914(5) 0.2765(4) 0.6981(3) 0.040(2) B4 0.3332(6) 0.4306(5) 0.7597(3) 0.039(3) B5 0.3262(7) 0.2547(5) 0.8229(4) 0.049(3) B6 0.4875(7) 0.1580(5) 0.7828(4) 0.050(3) B7 0.6852(6) 0.4009(4) 0.7464(3) 0.037(2) B8 0.5169(5) 0.4982(4) 0.7939(3) 0.034(2) B9 0.4010(6) 0.3762(5) 0.8820(3) 0.042(3) B10 0.4978(7) 0.2132(5) 0.8942(4) 0.051(3) B11 0.6685(6) 0.2264(5) 0.8099(4) 0.046(3) B12 0.6164(6) 0.3589(5) 0.8738(3) 0.042(2) S1 0.53903(13) 0.71674(10) 0.59497(7) 0.0378(5) N1 0.7936(4) 0.8468(3) 0.6252(2) 0.0462(19) N2 0.6713(4) 0.7190(3) 0.7657(2) 0.0351(16) C11 0.8294(5) 0.8826(4) 0.5209(3) 0.041(2) C12 0.7724(6) 1.0041(4) 0.4691(3) 0.053(3) C13 0.8127(7) 1.0394(5) 0.3686(4) 0.064(3) C14 0.9049(6) 0.9553(6) 0.3218(3) 0.060(3) C15 0.9613(6) 0.8330(6) 0.3735(4) 0.063(3) C16 0.9242(5) 0.7967(4) 0.4742(3) 0.050(3) C17 0.6792(5) 0.7613(4) 0.6682(3) 0.035(2) C21 0.7989(5) 0.7458(4) 0.8248(3) 0.037(2) C22 0.9359(6) 0.6646(5) 0.8340(4) 0.061(3) C23 1.0523(6) 0.6862(6) 0.8943(4) 0.071(3) C24 1.0321(6) 0.7909(5) 0.9449(4) 0.060(3) C25 0.8954(6) 0.8720(4) 0.9352(3) 0.051(3) C26 0.7776(5) 0.8500(4) 0.8749(3) 0.043(2) C27 0.5310(5) 0.6450(4) 0.8165(3) 0.037(2) H1n 0.855 0.887 0.667 0.0565 H12p 0.707 1.063 0.502 0.0624 H13 0.775 1.124 0.332 0.0716 H14 0.931 0.981 0.253 0.0700 H15 1.026 0.774 0.340 0.0750 H16 0.963 0.713 0.511 0.0594 H22 0.950 0.593 0.799 0.0742 H23 1.147 0.629 0.901 0.0835 H24 1.113 0.806 0.987 0.0706 H25 0.881 0.944 0.970 0.0624 H26 0.683 0.907 0.868 0.0538 H27a 0.539 0.636 0.886 0.0468 H27b 0.436 0.697 0.796 0.0468 H1 0.337 0.265 0.650 0.0508 H2 0.643 0.233 0.641 0.0499 H4 0.221 0.481 0.750 0.0486 H5 0.218 0.203 0.837 0.0575 H6 0.474 0.063 0.767 0.0588 H7 0.803 0.431 0.724 0.0472 H9 0.339 0.403 0.943 0.0516 H10 0.484 0.147 0.962 0.0594 H11 0.777 0.171 0.805 0.0554 H12 0.691 0.386 0.924 0.0513 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Rh3 0.03331(17) -0.0005(1) -0.0052(1) 0.03315(16) -0.0032(1) 0.02154(15) Br1 0.0359(2) 0.00290(19) -0.00703(17) 0.0556(3) -0.00742(18) 0.0303(2) C1 0.044(2) -0.0049(18) -0.0057(18) 0.041(2) -0.0066(17) 0.038(2) C2 0.054(3) 0.0047(18) -0.0060(18) 0.032(2) -0.0044(16) 0.034(2) B4 0.040(3) -0.001(2) -0.0034(19) 0.045(3) -0.0045(19) 0.031(2) B5 0.058(3) -0.015(2) -0.004(2) 0.046(3) 0.002(2) 0.038(3) B6 0.062(3) -0.008(2) -0.012(3) 0.037(3) 0.002(2) 0.047(3) B7 0.042(3) 0.005(2) -0.0102(19) 0.040(2) -0.0041(18) 0.030(2) B8 0.034(2) 0.0017(19) -0.0051(17) 0.042(2) -0.0023(17) 0.024(2) B9 0.052(3) -0.004(2) -0.002(2) 0.047(3) -0.0020(19) 0.026(2) B10 0.065(4) -0.009(3) -0.005(2) 0.048(3) 0.006(2) 0.034(3) B11 0.051(3) 0.003(2) -0.008(2) 0.041(3) -0.000(2) 0.044(3) B12 0.052(3) -0.001(2) -0.012(2) 0.044(3) 0.0026(19) 0.028(2) S1 0.0462(6) -0.0034(4) -0.0118(4) 0.0367(5) -0.0007(4) 0.0296(5) N1 0.053(2) -0.0233(17) -0.0070(16) 0.053(2) -0.0045(16) 0.0333(18) N2 0.0385(18) -0.0045(14) -0.0064(14) 0.0380(17) -0.0081(13) 0.0301(16) C11 0.039(2) -0.0101(18) -0.0042(17) 0.046(2) -0.0032(18) 0.035(2) C12 0.054(3) 0.002(2) -0.002(2) 0.049(3) -0.007(2) 0.054(3) C13 0.075(4) -0.012(3) -0.014(3) 0.060(3) 0.013(2) 0.050(3) C14 0.060(3) -0.022(3) 0.000(2) 0.081(4) -0.007(2) 0.039(2) C15 0.048(3) -0.014(3) 0.011(3) 0.079(4) -0.032(3) 0.068(3) C16 0.049(3) -0.003(2) -0.001(2) 0.046(3) -0.004(2) 0.053(3) C17 0.043(2) 0.0007(16) -0.0054(17) 0.0301(19) -0.0078(15) 0.032(2) C21 0.042(2) -0.0034(17) -0.0091(17) 0.039(2) -0.0049(16) 0.0288(19) C22 0.054(3) 0.013(2) -0.017(3) 0.072(3) -0.038(3) 0.066(3) C23 0.056(3) 0.020(3) -0.032(3) 0.081(4) -0.032(3) 0.084(4) C24 0.065(3) -0.011(3) -0.029(2) 0.064(3) -0.008(2) 0.053(3) C25 0.068(3) -0.005(2) -0.018(2) 0.045(2) -0.015(2) 0.044(2) C26 0.053(3) 0.0052(18) -0.015(2) 0.036(2) -0.0086(18) 0.043(2) C27 0.038(2) -0.0026(17) -0.0009(16) 0.046(2) -0.0079(16) 0.0267(19)