#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007146.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2007146 loop_ _publ_author_name 'Farrugia, L. J.' 'Norman, N. C.' 'Pickett, N. L.' _publ_section_title ; Diiodotetrakis[tris(dimethylamino)phosphine oxide-O]bismuth(III) Pentaiodide, [BiI~2~{OP(NMe~2~)~3~}~4~][I~5~] ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 476 _journal_page_last 479 _journal_volume 54 _journal_year 1998 _chemical_formula_iupac '[Bi I2 (C6 H18 N3 O P)4](I5)' _chemical_formula_moiety 'C24 H72 Bi I2 N12 O4 P4,I5' _chemical_formula_sum 'C24 H72 Bi I7 N12 O4 P4' _chemical_formula_weight 1814.1 _chemical_name_systematic ; bis(iodo)tetrakis{tris(dimethylamido)phosphineoxide}bismuth(III) pentaiodide ; _space_group_IT_number 122 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I -4 2bw' _symmetry_space_group_name_H-M 'I -4 2 d' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.775(6) _cell_length_b 13.775(6) _cell_length_c 30.533(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 291(2) _cell_measurement_theta_max 15.1 _cell_measurement_theta_min 8.2 _cell_volume 5794(4) _computing_cell_refinement 'CAD4 Express' _computing_data_collection 'CAD4 Express (Enraf Nonius, 1992)' _computing_data_reduction 'XCAD-4 (Harms & Wocadlo, 1996)' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997), CAMERON (Watkin et al., 1993) ; _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al, 1996)' _diffrn_ambient_temperature 291(2) _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2751 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% 1 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 6.92 _exptl_absorpt_correction_T_max 0.304 _exptl_absorpt_correction_T_min 0.109 _exptl_absorpt_correction_type psi_scans _exptl_absorpt_process_details ; [local program based on the method of North, Phillips & Mathews (1968)] ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.08 _exptl_crystal_density_method none _exptl_crystal_description prism _exptl_crystal_F_000 3384 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.78 _refine_diff_density_min -1.10_(1.08\%A_from_Bi1) _refine_ls_abs_structure_details 'Flack (1983) parameter = -0.029(11)' _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.001 _refine_ls_goodness_of_fit_obs 1.081 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 133 _refine_ls_number_reflns 1422 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.001 _refine_ls_restrained_S_obs 1.081 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_obs 0.0305 _refine_ls_shift/esd_max -0.005 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0374P)^2^ ] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.0765 _refine_ls_wR_factor_obs 0.0659 _reflns_number_observed 950 _reflns_number_total 1422 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file bm1163.cif _[local]_cod_data_source_block bibl _cod_original_cell_volume 5793(3) _cod_database_code 2007146 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' '-x+1/2, y, -z+3/4' '-y+1/2, -x, z+3/4' 'x+1/2, -y, -z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'x+1, -y+1/2, -z+5/4' 'y+1, x+1/2, z+5/4' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Bi1 0.0332(2) 0.0332(2) 0.0377(3) 0.000 0.000 0.000 I1 0.0882(8) 0.0686(7) 0.0490(5) 0.0074(14) 0.000 0.000 P1 0.041(2) 0.048(2) 0.0588(14) -0.0026(15) -0.0076(13) -0.0049(14) O1 0.039(4) 0.063(5) 0.066(4) -0.007(4) -0.008(4) -0.004(4) N11 0.038(6) 0.078(8) 0.078(7) -0.011(5) -0.001(5) -0.013(6) N12 0.069(7) 0.053(7) 0.079(7) 0.013(6) -0.024(6) -0.017(6) N13 0.053(7) 0.057(6) 0.089(6) -0.008(6) 0.005(6) -0.016(6) C111 0.096(12) 0.121(14) 0.060(8) 0.003(11) 0.030(8) 0.008(8) C112 0.053(9) 0.139(17) 0.20(2) -0.002(11) 0.010(11) -0.042(16) C121 0.22(2) 0.066(11) 0.111(13) 0.058(13) -0.077(15) -0.024(9) C122 0.20(2) 0.116(16) 0.120(14) 0.016(17) -0.089(15) -0.028(12) C131 0.073(10) 0.086(11) 0.093(10) 0.012(9) 0.005(9) -0.024(9) C132 0.144(18) 0.070(11) 0.154(15) -0.048(12) 0.038(13) -0.035(11) I2 0.1276(14) 0.1276(14) 0.267(4) 0.000 0.000 0.000 I21 0.199(4) 0.0506(13) 0.182(3) -0.009(2) 0.117(3) -0.014(2) I22 0.214(5) 0.094(2) 0.175(4) 0.024(3) 0.096(4) 0.040(2) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Bi1 0.5000 0.0000 0.2500 0.0347(2) Uani d S 1 Bi I1 0.5000 0.0000 0.14958(3) 0.0686(3) Uani d S 1 I P1 0.2616(2) -0.1267(2) 0.23372(10) 0.0491(7) Uani d . 1 P O1 0.3509(5) -0.0777(5) 0.2499(3) 0.056(2) Uani d . 1 O N11 0.1810(7) -0.1270(9) 0.2723(3) 0.065(3) Uani d . 1 N N12 0.2155(8) -0.0717(7) 0.1928(3) 0.067(3) Uani d . 1 N N13 0.2837(8) -0.2362(8) 0.2184(4) 0.066(3) Uani d . 1 N C111 0.2133(12) -0.1445(14) 0.3173(4) 0.092(5) Uani d . 1 C H11A 0.279(3) -0.122(7) 0.3207(10) 0.111 Uiso calc R 1 H H11B 0.211(7) -0.2128(16) 0.3234(12) 0.111 Uiso calc R 1 H H11C 0.172(5) -0.111(6) 0.3373(5) 0.111 Uiso calc R 1 H C112 0.0786(10) -0.1316(17) 0.2641(7) 0.130(7) Uani d . 1 C H11D 0.0440(10) -0.113(9) 0.2900(14) 0.157 Uiso calc R 1 H H11E 0.0610(17) -0.197(3) 0.256(4) 0.157 Uiso calc R 1 H H11F 0.0623(17) -0.088(7) 0.241(3) 0.157 Uiso calc R 1 H C121 0.2042(16) 0.0365(11) 0.1939(6) 0.131(9) Uani d . 1 C H12A 0.244(7) 0.0628(14) 0.217(3) 0.157 Uiso calc R 1 H H12B 0.137(2) 0.0526(11) 0.199(4) 0.157 Uiso calc R 1 H H12C 0.224(8) 0.0633(13) 0.1663(16) 0.157 Uiso calc R 1 H C122 0.1865(17) -0.1087(14) 0.1520(6) 0.147(8) Uani d . 1 C H12D 0.239(4) -0.102(10) 0.1314(13) 0.176 Uiso calc R 1 H H12E 0.131(7) -0.073(7) 0.142(2) 0.176 Uiso calc R 1 H H12F 0.170(10) -0.176(3) 0.1550(11) 0.176 Uiso calc R 1 H C131 0.3709(11) -0.2584(11) 0.1922(5) 0.084(5) Uani d . 1 C H13A 0.391(4) -0.201(2) 0.176(2) 0.101 Uiso calc R 1 H H13B 0.356(2) -0.310(5) 0.172(2) 0.101 Uiso calc R 1 H H13C 0.422(2) -0.279(7) 0.2113(6) 0.101 Uiso calc R 1 H C132 0.2223(14) -0.3170(11) 0.2269(6) 0.122(7) Uani d . 1 C H13D 0.173(5) -0.298(2) 0.247(3) 0.147 Uiso calc R 1 H H13E 0.260(2) -0.369(3) 0.239(3) 0.147 Uiso calc R 1 H H13F 0.193(6) -0.338(5) 0.2001(9) 0.147 Uiso calc R 1 H I2 0.0000 0.0000 0.0000 0.1741(13) Uani d S 1 I I21 -0.1435(3) 0.0395(2) -0.07989(12) 0.144(2) Uani d P 0.50 I I22 -0.2786(4) 0.0613(3) -0.14712(13) 0.161(2) Uani d P 0.50 I loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 0 -20 4 -6 -8 5 5 10 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Bi1 O1 10 3_655 90.0010(10) no O1 Bi1 O1 10 . 90.0010(10) no O1 Bi1 O1 3_655 . 179.9(4) yes O1 Bi1 O1 10 12_545 179.9(4) no O1 Bi1 O1 3_655 12_545 90.0010(10) no O1 Bi1 O1 . 12_545 90.00(2) yes O1 Bi1 I1 10 . 90.1(2) no O1 Bi1 I1 3_655 . 89.9(2) no O1 Bi1 I1 . . 89.9(2) yes O1 Bi1 I1 12_545 . 90.1(2) no O1 Bi1 I1 10 10 89.9(2) no O1 Bi1 I1 3_655 10 90.1(2) no O1 Bi1 I1 . 10 90.1(2) no O1 Bi1 I1 12_545 10 89.9(2) no I1 Bi1 I1 . 10 180.0 no O1 P1 N12 . . 112.0(5) yes O1 P1 N13 . . 111.4(5) yes N12 P1 N13 . . 107.0(6) yes O1 P1 N11 . . 109.1(5) yes N12 P1 N11 . . 107.3(6) yes N13 P1 N11 . . 109.8(6) yes P1 O1 Bi1 . . 160.6(5) yes C112 N11 C111 . . 117.0(14) no C112 N11 P1 . . 123.3(11) no C111 N11 P1 . . 118.3(9) no C122 N12 C121 . . 110.5(13) no C122 N12 P1 . . 129.6(11) no C121 N12 P1 . . 119.8(10) no C132 N13 C131 . . 114.9(11) no C132 N13 P1 . . 124.6(9) no C131 N13 P1 . . 120.4(10) no I21 I2 I21 . 3 80.09(11) yes I21 I2 I21 . 4 125.88(7) yes I21 I2 I21 3 4 125.88(7) no I21 I2 I21 . 2 125.88(7) no I21 I2 I21 3 2 125.88(7) no I21 I2 I21 4 2 80.09(11) no I22 I21 I22 5_454 . 16.0(3) no I22 I21 I2 5_454 . 162.2(3) no I22 I21 I2 . . 175.2(2) yes I21 I22 I22 5_454 5_454 150.6(5) no I21 I22 I21 5_454 . 155.8(3) no I22 I22 I21 5_454 . 13.4(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Bi1 O1 10 2.316(7) no Bi1 O1 3_655 2.316(7) no Bi1 O1 . 2.316(7) yes Bi1 O1 12_545 2.316(7) no Bi1 I1 . 3.0661(9) yes Bi1 I1 10 3.0663(9) no P1 O1 . 1.488(7) yes P1 N12 . 1.593(10) yes P1 N13 . 1.609(11) yes P1 N11 . 1.618(10) yes N11 C112 . 1.43(2) yes N11 C111 . 1.47(2) yes N12 C122 . 1.41(2) yes N12 C121 . 1.50(2) yes N13 C132 . 1.42(2) yes N13 C131 . 1.47(2) yes I2 I21 . 3.186(5) yes I2 I21 3 3.186(5) no I2 I21 4 3.186(5) no I2 I21 2 3.186(5) no I21 I22 5_454 1.317(5) no I21 I22 . 2.787(8) yes I22 I21 5_454 1.317(5) no I22 I22 5_454 1.564(9) no