#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003741.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_2003741 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1995 _journal_volume 51 _journal_page_first 1498 _journal_page_last 1500 _publ_section_title ; (3-tert-Butylisocyanide)-3,8-bis(dimethylphenylphosphine)octahydro- 1,2-diarsa-3-palla-closo-dodecaboron(1+) Hexafluoroantimonate ; _chemical_formula_moiety '(C21 H39 As2 B9 N P2 Pd) (Sb F6)' _chemical_formula_sum 'C21 H39 As2 B9 F6 N P2 Pd Sb' _chemical_formula_structural '((C4 H9 N C)(P(C H3)2 (C6 H5))2 (Pd As2 B9 H8)) 1+, Sb F6 1-' _chemical_formula_weight 956.75 _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 9.9342(8) _cell_length_b 13.0495(13) _cell_length_c 15.3141(14) _cell_angle_alpha 96.6120(9) _cell_angle_beta 102.2910(10) _cell_angle_gamma 105.039(8) _cell_volume 1842.5(3) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.725 _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 14.50 _cell_measurement_theta_max 21.00 _exptl_absorpt_coefficient_mu 3.136 _cell_measurement_temperature 291(1) _exptl_crystal_description block _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_size_rad ? _exptl_crystal_colour pink _chemical_compound_source 'synthesised by the authors' _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\q/2\q scan' _exptl_absorpt_correction_type 'empirical, 9 \y scans at 4\% steps' _exptl_absorpt_correction_T_min 0.5700 _exptl_absorpt_correction_T_max 0.7032 _diffrn_reflns_number 7201 _reflns_number_total 7201 _reflns_number_observed 4403 _reflns_observed_criterion >2\s(I) _diffrn_reflns_av_R_equivalents 0.0 _diffrn_reflns_theta_max 25.90 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'no decay, variation 1.0' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0430 _refine_ls_wR_factor_obs 0.1071 _refine_ls_wR_factor_all 0.1176 _refine_ls_goodness_of_fit_obs 1.216 _refine_ls_goodness_of_fit_all 1.026 _refine_ls_number_reflns 7201 _refine_ls_number_parameters 401 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^] where P=(Fo^2^+2F~c~^2^)/3' _refine_ls_shift/esd_max -0.003 _refine_diff_density_max 0.728 _refine_diff_density_min '-1.101 e \%A^-3^, 0.95\%A from As2' _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' '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 'As' 'As' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0499 2.0058 'B' 'B' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0013 0.0007 'F' 'F' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0171 0.0103 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.0033 'P' 'P' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1023 0.0942 'Pd' 'Pd' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -0.9988 1.0072 'Sb' 'Sb' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -0.5866 1.5461 ## 'DATRD2 in NRCVAX94 (Gabe, Le Page, Charland, Lee & White, 1989)' ##;NRCVAX94; PLATON (Spek, 1994a); PLUTON (Spek 1994b); ORTEPII (Johnson, ##1976) ##; 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 Pd3 1 0.21639(4) 0.80885(3) 0.18640(3) 0.05057(14) Sb 1 0.76973(6) 0.72643(4) 0.42038(3) 0.0866(2) As1 1 0.38647(6) 0.76139(6) 0.08680(5) 0.0681(2) As2 1 0.35995(8) 0.94647(5) 0.11186(4) 0.0685(2) P1 1 0.2783(2) 0.9402(2) 0.31649(12) 0.0875(7) P2 1 -0.15502(14) 0.70551(11) 0.08108(9) 0.0420(3) N 1 0.1883(6) 0.6222(4) 0.2993(3) 0.075(2) B4 1 0.1526(6) 0.6791(4) 0.0586(4) 0.0418(13) B5 1 0.2322(7) 0.7094(5) -0.0397(5) 0.055(2) B6 1 0.3352(8) 0.8502(5) -0.0237(5) 0.059(2) B7 1 0.1206(8) 0.9005(5) 0.0817(4) 0.054(2) B8 1 0.0298(6) 0.7607(4) 0.0572(4) 0.0372(12) B9 1 0.0506(7) 0.7024(5) -0.0448(4) 0.0481(15) B10 1 0.1594(8) 0.8042(5) -0.0904(4) 0.058(2) B11 1 0.2084(8) 0.9259(5) -0.0128(5) 0.059(2) B12 1 0.0348(8) 0.8320(5) -0.0329(4) 0.055(2) F1 1 0.6337(7) 0.7240(5) 0.3154(4) 0.155(2) F2 1 0.8999(7) 0.7211(6) 0.5223(4) 0.184(3) F3 1 0.7192(11) 0.5817(5) 0.3916(6) 0.255(5) F4 1 0.9111(9) 0.7339(8) 0.3577(5) 0.202(3) F5 1 0.8297(13) 0.8681(6) 0.4437(8) 0.294(6) F6 1 0.6434(10) 0.7276(13) 0.4858(6) 0.319(7) C11 1 0.4567(8) 1.0329(6) 0.3326(4) 0.074(2) C12 1 0.5709(9) 0.9920(7) 0.3326(5) 0.090(2) C13 1 0.7067(10) 1.0599(11) 0.3432(6) 0.124(4) C14 1 0.7266(14) 1.1677(12) 0.3524(7) 0.145(6) C15 1 0.6176(15) 1.2100(9) 0.3511(6) 0.133(5) C16 1 0.4807(10) 1.1430(6) 0.3421(4) 0.097(3) C17 1 0.2895(13) 0.8893(8) 0.4217(5) 0.179(6) C18 1 0.1534(10) 1.0189(9) 0.3189(8) 0.175(6) C21 1 -0.2980(5) 0.6588(4) -0.0216(3) 0.0432(12) C22 1 -0.3564(6) 0.7317(5) -0.0642(4) 0.0585(15) C23 1 -0.4609(7) 0.6980(5) -0.1452(4) 0.065(2) C24 1 -0.5051(7) 0.5896(6) -0.1859(4) 0.072(2) C25 1 -0.4488(7) 0.5180(5) -0.1437(5) 0.072(2) C26 1 -0.3470(6) 0.5506(5) -0.0628(4) 0.062(2) C27 1 -0.1972(6) 0.8075(5) 0.1518(4) 0.062(2) C28 1 -0.1579(6) 0.5955(5) 0.1402(4) 0.068(2) C31 1 0.2014(7) 0.6902(6) 0.2600(4) 0.072(2) C32 1 0.1760(7) 0.5337(5) 0.3518(4) 0.076(2) C33 0.795(13) 0.2160(12) 0.5844(7) 0.4481(5) 0.123(5) C34 0.795(13) 0.2688(11) 0.4678(9) 0.3294(7) 0.134(6) C35 0.795(13) 0.0179(8) 0.4657(7) 0.3228(6) 0.103(4) C33A 0.205(13) 0.090(3) 0.551(3) 0.4175(18) 0.107(11) C34A 0.205(13) 0.3324(15) 0.554(3) 0.402(2) 0.107(11) C35A 0.205(13) 0.118(3) 0.4232(17) 0.296(2) 0.107(11) H4 1 0.1284 0.5994 0.0787 0.050 H5 1 0.2585 0.6463 -0.0811 0.066 H6 1 0.4241 0.8774 -0.0557 0.071 H7 1 0.0750 0.9583 0.1143 0.065 H9 1 -0.0365 0.6341 -0.0888 0.058 H10 1 0.1428 0.8038 -0.1639 0.069 H11 1 0.2228 1.0042 -0.0354 0.071 H12 1 -0.0616 0.8495 -0.0705 0.066 H12A 1 0.5562 0.9178 0.3255 0.108 H13 1 0.7842 1.0322 0.3440 0.149 H14 1 0.8188 1.2135 0.3599 0.174 H15 1 0.6337 1.2842 0.3563 0.159 H16 1 0.4046 1.1721 0.3423 0.116 H17A 1 0.3544 0.8459 0.4264 0.268 H17B 1 0.1957 0.8463 0.4229 0.268 H17C 1 0.3243 0.9487 0.4719 0.268 H18A 1 0.1406 1.0495 0.2647 0.263 H18B 1 0.1909 1.0757 0.3711 0.263 H18C 1 0.0623 0.9733 0.3221 0.263 H22 1 -0.3245 0.8043 -0.0375 0.070 H23 1 -0.5013 0.7469 -0.1724 0.078 H24 1 -0.5728 0.5661 -0.2417 0.086 H25 1 -0.4805 0.4455 -0.1706 0.086 H26 1 -0.3101 0.5004 -0.0352 0.074 H27A 1 -0.1967 0.8685 0.1221 0.093 H27B 1 -0.1264 0.8298 0.2091 0.093 H27C 1 -0.2908 0.7784 0.1616 0.093 H28A 1 -0.0825 0.6182 0.1954 0.101 H28B 1 -0.1434 0.5372 0.1026 0.101 H28C 1 -0.2494 0.5718 0.1543 0.101 H33A 0.795(13) 0.1522 0.6261 0.4582 0.185 H33B 0.795(13) 0.3132 0.6308 0.4641 0.185 H33C 0.795(13) 0.2085 0.5295 0.4850 0.185 H34A 0.795(13) 0.2372 0.4369 0.2658 0.201 H34B 0.795(13) 0.2627 0.4111 0.3645 0.201 H34C 0.795(13) 0.3668 0.5125 0.3432 0.201 H35A 0.795(13) -0.0065 0.4335 0.2597 0.155 H35B 0.795(13) -0.0422 0.5109 0.3317 0.155 H35C 0.795(13) 0.0031 0.4101 0.3587 0.155 H33D 0.205(13) 0.1299 0.6233 0.4520 0.161 H33E 0.205(13) 0.0914 0.5004 0.4579 0.161 H33F 0.205(13) -0.0080 0.5416 0.3850 0.161 H34D 0.205(13) 0.3697 0.6264 0.4355 0.161 H34E 0.205(13) 0.3875 0.5447 0.3585 0.161 H34F 0.205(13) 0.3390 0.5040 0.4425 0.161 H35D 0.205(13) 0.1756 0.4150 0.2543 0.161 H35E 0.205(13) 0.0203 0.4125 0.2627 0.161 H35F 0.205(13) 0.1202 0.3709 0.3351 0.161 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 Pd3 0.0465(2) -0.0052(2) 0.0072(2) 0.0518(3) 0.0148(2) 0.0417(2) Sb 0.1127(4) 0.0274(3) 0.0250(3) 0.0903(4) 0.0116(2) 0.0566(3) As1 0.0407(3) 0.0157(3) 0.0273(3) 0.0753(4) 0.0398(4) 0.0981(5) As2 0.0784(5) -0.0203(3) 0.0227(3) 0.0473(3) 0.0065(3) 0.0590(4) P1 0.0788(13) -0.0248(11) 0.0125(9) 0.0979(14) -0.0095(9) 0.0488(9) P2 0.0367(7) 0.0139(6) 0.0111(6) 0.0451(7) 0.0165(6) 0.0474(7) N 0.075(4) 0.005(3) 0.013(3) 0.086(4) 0.036(3) 0.057(3) B4 0.037(3) 0.016(2) 0.025(3) 0.036(3) 0.016(3) 0.063(4) B5 0.064(4) 0.009(3) 0.040(3) 0.036(3) 0.001(3) 0.070(4) B6 0.065(4) 0.004(3) 0.037(4) 0.049(4) 0.010(3) 0.067(4) B7 0.075(5) 0.016(3) 0.039(4) 0.036(3) 0.018(3) 0.063(4) B8 0.034(3) 0.011(2) 0.009(2) 0.035(3) 0.013(2) 0.044(3) B9 0.054(4) 0.005(3) 0.020(3) 0.043(3) 0.006(3) 0.045(3) B10 0.068(4) 0.003(3) 0.023(3) 0.051(4) 0.012(3) 0.049(4) B11 0.092(5) 0.015(3) 0.030(4) 0.030(3) 0.022(3) 0.062(4) B12 0.066(4) 0.024(3) 0.016(3) 0.052(4) 0.026(3) 0.056(4) F1 0.174(6) 0.049(4) -0.013(4) 0.170(6) 0.034(4) 0.100(4) F2 0.169(6) 0.016(5) -0.030(4) 0.228(7) 0.052(4) 0.105(4) F3 0.316(11) 0.022(5) -0.105(8) 0.097(4) 0.013(5) 0.241(9) F4 0.185(7) 0.090(7) 0.066(5) 0.317(11) 0.059(6) 0.131(5) F5 0.383(15) 0.066(7) -0.024(12) 0.109(6) 0.017(7) 0.327(13) F6 0.191(8) 0.121(11) 0.099(6) 0.633(22) 0.009(10) 0.145(6) C11 0.081(5) -0.013(4) -0.005(3) 0.074(5) 0.008(3) 0.038(3) C12 0.079(5) -0.001(5) 0.001(4) 0.093(6) 0.011(4) 0.072(5) C13 0.079(6) 0.003(7) 0.006(5) 0.186(11) 0.026(7) 0.081(6) C14 0.136(10) -0.068(9) -0.006(7) 0.151(12) 0.041(7) 0.074(6) C15 0.177(12) -0.032(8) -0.024(7) 0.089(7) 0.021(5) 0.066(5) C16 0.125(7) -0.011(5) -0.011(4) 0.072(5) 0.013(3) 0.056(4) C17 0.221(12) -0.101(9) 0.034(6) 0.172(10) 0.006(5) 0.047(4) C18 0.085(7) 0.025(7) 0.018(6) 0.217(12) -0.121(9) 0.167(10) C21 0.033(3) 0.014(2) 0.012(2) 0.047(3) 0.009(2) 0.052(3) C22 0.061(4) 0.015(3) 0.006(3) 0.052(3) 0.010(3) 0.057(3) C23 0.067(4) 0.028(3) 0.004(3) 0.074(4) 0.012(3) 0.054(3) C24 0.050(4) 0.013(4) 0.007(3) 0.103(6) 0.003(4) 0.052(3) C25 0.062(4) 0.002(3) 0.010(4) 0.056(4) -0.008(3) 0.080(4) C26 0.044(3) 0.011(3) 0.006(3) 0.051(3) 0.010(3) 0.083(4) C27 0.053(4) 0.028(3) 0.015(3) 0.083(4) 0.010(3) 0.055(3) C28 0.043(3) 0.012(3) 0.020(3) 0.078(4) 0.050(4) 0.088(4) C31 0.062(4) 0.000(3) 0.004(3) 0.087(5) 0.029(3) 0.054(4) C32 0.085(5) 0.023(4) 0.025(3) 0.091(5) 0.046(4) 0.060(4) C33 0.213(15) 0.031(8) 0.034(7) 0.092(8) 0.038(5) 0.063(6) C34 0.181(14) 0.104(11) 0.102(11) 0.162(13) 0.085(10) 0.135(11) C35 0.104(8) 0.016(6) 0.027(7) 0.089(7) 0.065(7) 0.120(9) _cod_database_code 2003741