#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/71/2007146.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 'Louis J. Farrugia' 'Nicholas C. Norman' 'Nigel L. Pickett' _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 '[BiI2 (C6 H18 N3 OP)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 .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 .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_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _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 .0332(2) .0332(2) .0377(3) .000 .000 .000 I1 .0882(8) .0686(7) .0490(5) .0074(14) .000 .000 P1 .041(2) .048(2) .0588(14) -.0026(15) -.0076(13) -.0049(14) O1 .039(4) .063(5) .066(4) -.007(4) -.008(4) -.004(4) N11 .038(6) .078(8) .078(7) -.011(5) -.001(5) -.013(6) N12 .069(7) .053(7) .079(7) .013(6) -.024(6) -.017(6) N13 .053(7) .057(6) .089(6) -.008(6) .005(6) -.016(6) C111 .096(12) .121(14) .060(8) .003(11) .030(8) .008(8) C112 .053(9) .139(17) .20(2) -.002(11) .010(11) -.042(16) C121 .22(2) .066(11) .111(13) .058(13) -.077(15) -.024(9) C122 .20(2) .116(16) .120(14) .016(17) -.089(15) -.028(12) C131 .073(10) .086(11) .093(10) .012(9) .005(9) -.024(9) C132 .144(18) .070(11) .154(15) -.048(12) .038(13) -.035(11) I2 .1276(14) .1276(14) .267(4) .000 .000 .000 I21 .199(4) .0506(13) .182(3) -.009(2) .117(3) -.014(2) I22 .214(5) .094(2) .175(4) .024(3) .096(4) .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_disorder_group _atom_site_type_symbol Bi1 .5000 .0000 .2500 .0347(2) Uani d S 1 . Bi I1 .5000 .0000 .14958(3) .0686(3) Uani d S 1 . I P1 .2616(2) -.1267(2) .23372(10) .0491(7) Uani d . 1 . P O1 .3509(5) -.0777(5) .2499(3) .056(2) Uani d . 1 . O N11 .1810(7) -.1270(9) .2723(3) .065(3) Uani d . 1 . N N12 .2155(8) -.0717(7) .1928(3) .067(3) Uani d . 1 . N N13 .2837(8) -.2362(8) .2184(4) .066(3) Uani d . 1 . N C111 .2133(12) -.1445(14) .3173(4) .092(5) Uani d . 1 . C H11A .279(3) -.122(7) .3207(10) .111 Uiso calc R 1 . H H11B .211(7) -.2128(16) .3234(12) .111 Uiso calc R 1 . H H11C .172(5) -.111(6) .3373(5) .111 Uiso calc R 1 . H C112 .0786(10) -.1316(17) .2641(7) .130(7) Uani d . 1 . C H11D .0440(10) -.113(9) .2900(14) .157 Uiso calc R 1 . H H11E .0610(17) -.197(3) .256(4) .157 Uiso calc R 1 . H H11F .0623(17) -.088(7) .241(3) .157 Uiso calc R 1 . H C121 .2042(16) .0365(11) .1939(6) .131(9) Uani d . 1 . C H12A .244(7) .0628(14) .217(3) .157 Uiso calc R 1 . H H12B .137(2) .0526(11) .199(4) .157 Uiso calc R 1 . H H12C .224(8) .0633(13) .1663(16) .157 Uiso calc R 1 . H C122 .1865(17) -.1087(14) .1520(6) .147(8) Uani d . 1 . C H12D .239(4) -.102(10) .1314(13) .176 Uiso calc R 1 . H H12E .131(7) -.073(7) .142(2) .176 Uiso calc R 1 . H H12F .170(10) -.176(3) .1550(11) .176 Uiso calc R 1 . H C131 .3709(11) -.2584(11) .1922(5) .084(5) Uani d . 1 . C H13A .391(4) -.201(2) .176(2) .101 Uiso calc R 1 . H H13B .356(2) -.310(5) .172(2) .101 Uiso calc R 1 . H H13C .422(2) -.279(7) .2113(6) .101 Uiso calc R 1 . H C132 .2223(14) -.3170(11) .2269(6) .122(7) Uani d . 1 . C H13D .173(5) -.298(2) .247(3) .147 Uiso calc R 1 . H H13E .260(2) -.369(3) .239(3) .147 Uiso calc R 1 . H H13F .193(6) -.338(5) .2001(9) .147 Uiso calc R 1 . H I2 .0000 .0000 .0000 .1741(13) Uani d S 1 . I I21 -.1435(3) .0395(2) -.07989(12) .144(2) Uani d P .50 . I I22 -.2786(4) .0613(3) -.14712(13) .161(2) Uani d P .50 . I 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 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