#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003776.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_2003776 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1496 _journal_page_last 1498 _publ_section_title ; exo-2,7,11-\m~3~-[Dihydro(triphenylphosphine)cuprio-2Cu,7H,11H]-2- triphenylphosphine-closo-1,2-selenacupradodecaborane(8) ; _chemical_formula_sum 'C36 H40 B10 Cu2 P2 Se1' _chemical_formula_weight 848.76 _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 12.0905(15) _cell_length_b 12.0619(13) _cell_length_c 13.970(2) _cell_angle_alpha 89.416(8) _cell_angle_beta 81.601(8) _cell_angle_gamma 75.202(8) _cell_volume 1947.8(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.447 _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 32 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 15 _exptl_absorpt_coefficient_mu 2.135 _cell_measurement_temperature 200.0(10) _exptl_crystal_description prism _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _exptl_crystal_colour 'pale brown' _diffrn_measurement_device 'Stoe STADI4' _diffrn_measurement_method \w/\q _exptl_absorpt_correction_type 'empirical - \y scans for 8 reflections' _exptl_absorpt_correction_T_min 0.3350 _exptl_absorpt_correction_T_max 0.4857 _diffrn_reflns_number 6076 _reflns_number_total 6076 _reflns_number_observed 5379 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0246 _refine_ls_wR_factor_obs 0.0641 _refine_ls_wR_factor_all 0.0670 _refine_ls_goodness_of_fit_obs 1.115 _refine_ls_goodness_of_fit_all 1.090 _refine_ls_number_reflns 6076 _refine_ls_number_parameters 501 _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(F~o~^2^) + (0.0345P)^2^ + 1.3887P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max -0.001 _refine_diff_density_max 0.255 _refine_diff_density_min -0.668 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.0016 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.0000 'Cu' 'Cu' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.3201 1.2651 'B' 'B' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0013 0.0007 'P' 'P' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1023 0.0942 'Se' 'Se' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -0.0929 2.2259 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Se1 1 0.09685(2) 0.01501(2) 0.08437(2) 0.0298(2) Cu2 1 0.20589(2) 0.13230(2) 0.14398(2) 0.0233(2) Cu3 1 0.25974(3) 0.19226(2) 0.30948(2) 0.0300(2) P1 1 0.29354(5) 0.23162(5) 0.04130(4) 0.0202(3) P2 1 0.33700(5) 0.30664(5) 0.38421(4) 0.0237(4) B3 1 0.0119(2) 0.1605(2) 0.1833(2) 0.028(2) B4 1 -0.0430(3) 0.0285(2) 0.2011(2) 0.031(2) B5 1 0.0861(3) -0.1043(2) 0.1971(2) 0.030(2) B6 1 0.2270(2) -0.0587(2) 0.1737(2) 0.021(2) B7 1 0.0926(2) 0.1638(2) 0.2788(2) 0.0241(15) B8 1 -0.0349(3) 0.1138(2) 0.2991(2) 0.030(2) B9 1 0.0049(3) -0.0389(2) 0.3055(2) 0.030(2) B10 1 0.1587(3) -0.0852(2) 0.2921(2) 0.028(2) B11 1 0.2166(2) 0.0363(2) 0.2738(2) 0.022(2) B12 1 0.0859(3) 0.0456(2) 0.3557(2) 0.028(2) H3 1 -0.0361(22) 0.2258(22) 0.1508(18) 0.032(7) H4 1 -0.1193(25) 0.0225(21) 0.1752(18) 0.035(7) H5 1 0.0778(24) -0.1835(23) 0.1677(19) 0.042(8) H6 1 0.2872(25) -0.1101(23) 0.1407(20) 0.037(7) H7 1 0.0898(23) 0.2429(22) 0.3189(19) 0.035(7) H8 1 -0.1176(25) 0.1667(23) 0.3379(20) 0.042(7) H9 1 -0.0500(22) -0.0855(21) 0.3494(18) 0.032(7) H10 1 0.2053(22) -0.1611(22) 0.3261(18) 0.033(7) H11 1 0.2939(23) 0.0332(21) 0.3113(18) 0.031(7) H12 1 0.0866(23) 0.0553(21) 0.4342(19) 0.034(7) C111 1 0.4358(2) 0.2347(2) 0.06729(15) 0.0212(13) C112 1 0.5019(2) 0.1361(2) 0.1042(2) 0.033(2) H112 1 0.4699 0.0737 0.1194 0.0454(15) C113 1 0.6139(2) 0.1292(2) 0.1185(2) 0.038(2) H113 1 0.6581 0.0619 0.1425 0.0454(15) C114 1 0.6614(2) 0.2206(2) 0.0978(2) 0.0351(15) H114 1 0.7377 0.2160 0.1078 0.0454(15) C115 1 0.5959(2) 0.3192(2) 0.0620(2) 0.038(2) H115 1 0.6281 0.3817 0.0475 0.0454(15) C116 1 0.4839(2) 0.3269(2) 0.0476(2) 0.029(2) H116 1 0.4398 0.3949 0.0243 0.0454(15) C121 1 0.2127(2) 0.3811(2) 0.03352(15) 0.0219(13) C122 1 0.2325(2) 0.4447(2) -0.0482(2) 0.0266(13) H122 1 0.2894 0.4110 -0.1003 0.0454(15) C123 1 0.1689(2) 0.5572(2) -0.0531(2) 0.0299(15) H123 1 0.1820 0.5992 -0.1088 0.0454(15) C124 1 0.0864(2) 0.6077(2) 0.0236(2) 0.032(2) H124 1 0.0447 0.6847 0.0208 0.0454(15) C125 1 0.0651(2) 0.5455(2) 0.1044(2) 0.035(2) H125 1 0.0084 0.5798 0.1564 0.0454(15) C126 1 0.1273(2) 0.4319(2) 0.1092(2) 0.0287(15) H126 1 0.1115 0.3892 0.1638 0.0454(15) C131 1 0.3205(2) 0.1884(2) -0.0867(2) 0.0215(14) C132 1 0.2256(2) 0.1909(2) -0.1333(2) 0.030(2) H132 1 0.1514 0.2040 -0.0969 0.0454(15) C133 1 0.2393(3) 0.1742(2) -0.2324(2) 0.035(2) H133 1 0.1746 0.1771 -0.2633 0.0454(15) C134 1 0.3486(2) 0.1533(2) -0.2860(2) 0.040(2) H134 1 0.3578 0.1444 -0.3537 0.0454(15) C135 1 0.4436(2) 0.1455(2) -0.2407(2) 0.036(2) H135 1 0.5179 0.1280 -0.2772 0.0454(15) C136 1 0.4303(2) 0.1633(2) -0.1410(2) 0.0267(14) H136 1 0.4956 0.1584 -0.1104 0.0454(15) C211 1 0.4669(2) 0.2387(2) 0.43514(15) 0.0254(14) C212 1 0.4983(2) 0.2862(2) 0.5143(2) 0.035(2) H212 1 0.4469 0.3502 0.5482 0.0454(15) C213 1 0.6044(2) 0.2399(2) 0.5430(2) 0.041(2) H213 1 0.6247 0.2725 0.5965 0.0454(15) C214 1 0.6812(3) 0.1461(2) 0.4939(2) 0.042(2) H214 1 0.7534 0.1147 0.5138 0.0454(15) C215 1 0.6509(3) 0.0989(3) 0.4155(2) 0.052(2) H215 1 0.7033 0.0358 0.3811 0.0454(15) C216 1 0.5441(2) 0.1437(2) 0.3870(2) 0.042(2) H216 1 0.5235 0.1094 0.3345 0.0454(15) C221 1 0.2320(2) 0.3822(2) 0.4844(2) 0.0311(15) C222 1 0.1495(2) 0.3287(2) 0.5288(2) 0.042(2) H222 1 0.1501 0.2547 0.5078 0.0454(15) C223 1 0.0665(3) 0.3845(3) 0.6039(2) 0.061(2) H223 1 0.0110 0.3482 0.6342 0.0454(15) C224 1 0.0654(3) 0.4924(3) 0.6339(2) 0.071(3) H224 1 0.0082 0.5303 0.6842 0.0454(15) C225 1 0.1466(3) 0.5458(3) 0.5914(2) 0.069(3) H225 1 0.1457 0.6195 0.6134 0.0454(15) C226 1 0.2301(3) 0.4916(2) 0.5163(2) 0.048(2) H226 1 0.2854 0.5286 0.4868 0.0454(15) C231 1 0.3783(2) 0.4221(2) 0.3141(2) 0.027(2) C232 1 0.4871(2) 0.4417(2) 0.3065(2) 0.038(2) H232 1 0.5449 0.3930 0.3367 0.0454(15) C233 1 0.5108(3) 0.5337(3) 0.2539(2) 0.049(2) H233 1 0.5843 0.5477 0.2498 0.0454(15) C234 1 0.4278(3) 0.6041(2) 0.2083(2) 0.050(3) H234 1 0.4447 0.6657 0.1725 0.0454(15) C235 1 0.3200(3) 0.5849(2) 0.2148(2) 0.050(2) H235 1 0.2631 0.6333 0.1835 0.0454(15) C236 1 0.2951(3) 0.4944(2) 0.2674(2) 0.041(2) H236 1 0.2211 0.4817 0.2717 0.0454(15) 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 Se1 0.0325(2) -0.01599(11) -0.01200(10) 0.03947(14) 0.00443(10) 0.02367(12) Cu2 0.0217(2) -0.01042(12) -0.00426(11) 0.02722(15) 0.00531(11) 0.02335(14) Cu3 0.0335(2) -0.01681(13) -0.01019(13) 0.0320(2) -0.00073(12) 0.0309(2) P1 0.0172(3) -0.0051(2) -0.0028(2) 0.0201(3) 0.0034(2) 0.0235(3) P2 0.0244(4) -0.0087(2) -0.0047(2) 0.0253(3) -0.0018(2) 0.0231(3) B3 0.020(2) -0.0046(11) -0.0079(12) 0.0248(13) 0.0098(11) 0.0380(15) B4 0.022(2) -0.0128(12) -0.0096(13) 0.0355(15) 0.0075(12) 0.039(2) B5 0.037(2) -0.0142(12) -0.0129(12) 0.0258(13) 0.0046(11) 0.0317(14) B6 0.019(2) -0.0027(10) -0.0143(11) 0.0170(11) 0.0003(10) 0.0300(13) B7 0.0203(15) -0.0047(10) -0.0022(11) 0.0230(12) 0.0027(10) 0.0281(13) B8 0.023(2) -0.0095(12) 0.0006(12) 0.0316(14) 0.0016(12) 0.0367(15) B9 0.032(2) -0.0174(13) -0.0066(12) 0.0334(14) 0.0082(11) 0.0308(14) B10 0.035(2) -0.0106(12) -0.0153(12) 0.0230(13) 0.0070(10) 0.0309(14) B11 0.021(2) -0.0083(10) -0.0101(11) 0.0224(12) 0.0027(10) 0.0258(12) B12 0.034(2) -0.0142(12) -0.0050(12) 0.0312(14) 0.0039(10) 0.0230(13) C111 0.0186(13) -0.0045(9) -0.0035(9) 0.0231(11) 0.0014(8) 0.0215(10) C112 0.025(2) -0.0070(10) -0.0098(12) 0.0263(12) 0.0089(11) 0.0479(15) C113 0.028(2) -0.0019(11) -0.0168(13) 0.0324(13) 0.0068(11) 0.053(2) C114 0.0227(15) -0.0088(11) -0.0115(12) 0.0385(14) -0.0016(11) 0.0465(15) C115 0.032(2) -0.0166(12) -0.0157(13) 0.0338(14) 0.0082(12) 0.055(2) C116 0.026(2) -0.0078(10) -0.0141(11) 0.0258(12) 0.0067(10) 0.0395(14) C121 0.0170(13) -0.0058(9) -0.0069(9) 0.0222(11) 0.0018(9) 0.0280(11) C122 0.0195(13) -0.0051(10) -0.0029(10) 0.0274(12) 0.0043(9) 0.0321(12) C123 0.0255(15) -0.0077(10) -0.0112(11) 0.0259(12) 0.0094(10) 0.0406(14) C124 0.029(2) -0.0012(10) -0.0132(11) 0.0216(11) -0.0023(10) 0.0450(15) C125 0.031(2) 0.0020(11) -0.0040(11) 0.0312(13) -0.0077(10) 0.0359(13) C126 0.0285(15) -0.0049(10) -0.0061(10) 0.0310(12) 0.0009(9) 0.0258(12) C131 0.0214(14) -0.0049(9) -0.0046(10) 0.0168(10) 0.0031(8) 0.0266(11) C132 0.024(2) -0.0077(10) -0.0063(11) 0.0299(12) 0.0012(10) 0.0354(13) C133 0.041(2) -0.0152(12) -0.0191(12) 0.0353(13) 0.0043(11) 0.0368(14) C134 0.058(2) -0.0186(13) -0.0048(13) 0.0387(14) -0.0004(11) 0.0272(13) C135 0.037(2) -0.0091(11) 0.0067(12) 0.0337(13) -0.0032(10) 0.0333(13) C136 0.0239(14) -0.0062(10) -0.0004(10) 0.0236(11) -0.0007(9) 0.0316(12) C211 0.0272(14) -0.0102(10) -0.0037(10) 0.0283(12) 0.0011(9) 0.0224(11) C212 0.032(2) -0.0052(12) -0.0073(11) 0.0429(14) -0.0070(11) 0.0267(12) C213 0.039(2) -0.0126(14) -0.0134(12) 0.059(2) -0.0034(12) 0.0262(13) C214 0.030(2) -0.0040(13) -0.0150(12) 0.053(2) 0.0041(13) 0.043(2) C215 0.035(2) 0.0063(14) -0.016(2) 0.049(2) -0.0205(15) 0.066(2) C216 0.037(2) -0.0023(13) -0.0147(13) 0.0421(15) -0.0186(12) 0.047(2) C221 0.0279(15) -0.0007(11) -0.0040(10) 0.0338(13) 0.0007(10) 0.0276(12) C222 0.038(2) -0.0091(13) -0.0006(12) 0.048(2) 0.0074(12) 0.0371(14) C223 0.047(2) 0.001(2) 0.014(2) 0.073(2) 0.017(2) 0.047(2) C224 0.071(3) 0.020(2) 0.024(2) 0.066(2) 0.004(2) 0.045(2) C225 0.094(3) 0.008(2) 0.012(2) 0.040(2) -0.0118(15) 0.052(2) C226 0.058(2) -0.0083(14) 0.0038(14) 0.0382(15) -0.0095(12) 0.041(2) C231 0.034(2) -0.0114(11) -0.0059(10) 0.0267(12) -0.0030(9) 0.0222(11) C232 0.038(2) -0.0182(13) -0.0040(12) 0.047(2) 0.0050(11) 0.0324(13) C233 0.053(2) -0.035(2) -0.0014(14) 0.060(2) 0.0042(14) 0.043(2) C234 0.083(3) -0.029(2) -0.0035(15) 0.0375(15) 0.0060(12) 0.0340(14) C235 0.070(2) -0.0112(15) -0.020(2) 0.0368(15) 0.0115(12) 0.045(2) C236 0.043(2) -0.0146(13) -0.0164(13) 0.0401(15) 0.0063(12) 0.043(2)