#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003569.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_2003569 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 1060 _journal_page_last 1063 _publ_section_title ; Dimorphism in Actinide Phosphides: Tetrakis[bis(2-dimethylphosphinoethyl)phosphido]thorium(IV) ; _chemical_formula_sum 'C32 H80 P12 Th' _chemical_formula_weight 1068.64 _space_group_IT_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _[local]_cod_cif_authors_sg_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,y+1/2,-z' _cell_length_a 15.919(5) _cell_length_b 10.307(9) _cell_length_c 16.23(2) _cell_angle_alpha 90 _cell_angle_beta 104.93(4) _cell_angle_gamma 90 _cell_volume 2574(3) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_meas ? _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 250 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 24.93 _exptl_absorpt_coefficient_mu 3.290 _cell_measurement_temperature 120 _exptl_crystal_description 'needle' _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_crystal_size_rad ? _exptl_crystal_colour 'red' _chemical_compound_source ? _diffrn_measurement_device 'Enraf-Nonius Fast Area' _diffrn_measurement_method 'MADNES' _exptl_absorpt_correction_type 'refdelf (DIFABS; Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.84 _diffrn_reflns_number 10577 _reflns_number_total 6696 _reflns_number_observed 3278 _reflns_observed_criterion 'F~o~ > 4\s(F~o~)' _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_theta_max 24.93 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0447 _refine_ls_wR_factor_obs 0.1026 _refine_ls_goodness_of_fit_obs 0.515 _refine_ls_number_reflns 6676 _refine_ls_number_parameters 380 _refine_ls_hydrogen_treatment 'refU' _refine_ls_weighting_scheme ;1/[\s^2^(F~o~^2^)+(0.0448P)^2^] where P = [max(F~o~^2^,0)+2(F~c~^2^)]/3 ; _refine_ls_shift/esd_max 0.004 _refine_diff_density_max 1.21 _refine_diff_density_min -0.93 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _atom_type_scat_source 'IntTabIV' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Th(1) .2488(1) 1.0002(1) .2537(1) .026(1) P(1) .3450(2) .8997(2) .4324(2) .030(1) P(2) .3821(2) .8074(2) .2632(2) .035(1) P(3) .5533(2) .6532(2) .0998(2) .045(1) P(4) .3893(2) 1.1817(2) .2187(2) .038(1) P(5) .2791(2) 1.2406(2) .3494(2) .041(1) P(6) .2787(2) 1.3968(2) .6142(2) .057(1) P(7) .1399(2) 1.1566(3) .0999(2) .043(1) P(8) .2266(2) .8947(2) .0851(2) .039(1) P(9) .2993(2) .5306(2) -.0416(1) .049(1) P(10) .1257(2) .7732(2) .2674(2) .036(1) P(11) .1011(2) 1.0560(2) .3184(2) .045(1) P(12) -.0615(2) 1.4184(3) .3154(2) .106(2) C(1) .4456(5) .9921(11) .4768(5) .047(2) C(2) .3018(6) .8941(9) .5223(6) .047(2) C(3) .3917(6) .7340(8) .4341(6) .036(2) C(4) .4462(6) .7323(8) .3645(5) .036(2) C(5) .4565(6) .7932(7) .1959(6) .038(3) C(6) .4802(3) .6543(8) .1712(2) .034(3) C(7) .5591(6) .4763(3) .0857(6) .060(4) C(8) .6588(3) .6808(9) .1762(5) .072(4) C(9) .4023(7) 1.1954(11) .1109(6) .067(4) C(10) .5017(6) 1.1432(9) .2832(8) .060(4) C(11) .3809(7) 1.3519(9) .2553(7) .060(4) C(12) .3646(7) 1.3552(8) .3435(7) .049(4) C(13) .2705(9) 1.2672(10) .4582(7) .084(4) C(14) .2581(7) 1.3938(9) .4970(2) .065(4) C(15) .1865(3) 1.2937(6) .6230(7) .080(4) C(16) .2202(4) 1.5505(4) .6115(8) .080(4) C(17) .1330(7) 1.3299(9) .1019(8) .073(3) C(18) .0233(7) 1.1109(9) .0764(8) .073(3) C(19) .1631(7) 1.1228(9) .0006(7) .053(4) C(20) .1694(7) .9768(9) -.0180(6) .056(4) C(21) .2289(7) .7203(8) .0472(7) .047(4) C(22) .2815(6) .7006(4) -.0154(6) .048(4) C(23) .1944(3) .4881(10) -.1151(4) .052(3) C(24) .3639(3) .5581(9) -.1188(3) .072(5) C(25) .1690(8) .6076(9) .2890(11) .109(7) C(26) .0378(9) .7433(13) .1675(8) .119(6) C(27) .0647(9) .7951(11) .3414(9) .087(4) C(28) .0153(8) .9321(10) .3306(9) .087(4) C(29) .0578(9) 1.2067(10) .3528(8) .084(4) C(30) -.0302(7) 1.2467(4) .3067(9) .132(7) C(31) -.1809(2) 1.3971(14) .2804(10) .144(6) C(32) -.0648(7) 1.3993(4) .4266(3) .144(6) H(1A) .4333(9) 1.0833(11) .4710(32) .070 H(1B) .4881(13) .9701(40) .4465(23) .070 H(1C) .4678(20) .9710(41) .5360(10) .070 H(2A) .2481(18) .8467(44) .5083(12) .070 H(2B) .2915(32) .9807(9) .5390(21) .070 H(2C) .3424(16) .8516(46) .5685(12) .070 H(3A) .4291(6) .7148(8) .4901(6) .043 H(3B) .3457(6) .6697(8) .4205(6) .043 H(4A) .4607(6) .6435(8) .3539(5) .043 H(4B) .5000(6) .7799(8) .3857(5) .043 H(5A) .4318(6) .8405(7) .1436(6) .045 H(5B) .5101(6) .8367(7) .2245(6) .045 H(6A) .4271(3) .6089(8) .1435(3) .040 H(6B) .5077(3) .6072(8) .2228(3) .040 H(7A) .5071(21) .4470(11) .0457(36) .090 H(7B) .5647(48) .4339(5) .1395(11) .090 H(7C) .6086(28) .4559(7) .0645(44) .090 H(8A) .6584(18) .7636(35) .2032(37) .107 H(8B) .7039(6) .6796(76) .1468(9) .107 H(8C) .6693(23) .6138(44) .2187(29) .107 H(9A) .3502(18) 1.2306(63) .0741(11) .100 H(9B) .4132(45) 1.1111(14) .0907(17) .100 H(9C) .4504(29) 1.2517(54) .1110(10) .100 H(10A) .5031(11) 1.1441(62) .3427(8) .090 H(10B) .5415(9) 1.2069(38) .2723(32) .090 H(10C) .5182(17) 1.0589(29) .2678(31) .090 H(11A) .4344(7) 1.3979(9) .2566(7) .072 H(11B) .3337(7) 1.3958(9) .2152(7) .072 H(12A) .3475(7) 1.4421(8) .3555(7) .059 H(12B) .4176(7) 1.3332(8) .3860(7) .059 H(13A) .2229(9) 1.2127(10) .4645(7) .101 H(13B) .3229(9) 1.2302(10) .4950(7) .101 H(14A) .1987(7) 1.4219(9) .4726(2) .079 H(14B) .2960(7) 1.4568(9) .4807(2) .079 H(15A) .1621(33) 1.3271(45) .6669(35) .120 H(15B) .2066(10) 1.2067(18) .6370(51) .120 H(15C) .1430(23) 1.2938(62) .5696(17) .120 H(16A) .2612(5) 1.6197(12) .6294(52) .120 H(16B) .1827(41) 1.5455(29) .6492(41) .120 H(16C) .1860(43) 1.5669(40) .5545(13) .120 H(17A) .1143(53) 1.3565(10) .1510(30) .110 H(17B) .0920(42) 1.3596(11) .0511(26) .110 H(17C) .1891(15) 1.3666(9) .1046(55) .110 H(18A) .0025(14) 1.1249(67) .1261(16) .110 H(18B) .0168(9) 1.0210(20) .0605(46) .110 H(18C) -.0096(10) 1.1632(50) .0303(31) .110 H(19A) .1179(7) 1.1611(9) -.0447(7) .064 H(19B) .2176(7) 1.1640(9) -.0001(7) .064 H(20A) .2018(7) .9640(9) -.0604(6) .067 H(20B) .1117(7) .9404(9) -.0397(6) .067 H(21A) .2521(7) .6654(8) .0963(7) .056 H(21B) .1697(7) .6925(8) .0215(7) .056 H(22A) .3377(6) .7412(4) .0068(6) .058 H(22B) .2530(6) .7453(4) -.0678(6) .058 H(23A) .1483(4) .5068(55) -.0887(15) .078 H(23B) .1938(15) .3974(16) -.1286(30) .078 H(23C) .1862(18) .5381(43) -.1665(16) .078 H(24A) .3799(41) .4761(9) -.1384(36) .107 H(24B) .4155(24) .6058(64) -.0919(14) .107 H(24C) .3302(18) .6067(63) -.1664(23) .107 H(25A) .2056(57) .6031(28) .3461(25) .163 H(25B) .2023(59) .5858(40) .2494(45) .163 H(25C) .1217(9) .5476(15) .2829(69) .163 H(26A) .0629(13) .7081(96) .1245(23) .179 H(26B) .0092(47) .8236(22) .1477(38) .179 H(26C) -.0036(38) .6830(81) .1792(17) .179 H(27A) .0222(9) .7258(11) .3349(9) .104 H(27B) .1028(9) .7893(11) .3985(9) .104 H(28A) -.0057(8) .9515(10) .3804(9) .104 H(28B) -.0337(8) .9318(10) .2806(9) .104 H(29A) .0589(9) 1.1973(10) .4125(8) .101 H(29B) .0972(9) 1.2767(10) .3488(8) .101 H(30A) -.0711(7) 1.1927(4) .3262(9) .159 H(30B) -.0375(7) 1.2276(4) .2467(9) .159 H(31A) -.2004(10) 1.4112(118) .2200(16) .216 H(31B) -.2084(4) 1.4585(81) .3094(59) .216 H(31C) -.1957(7) 1.3106(40) .2935(72) .216 H(32A) -.0722(79) 1.4827(19) .4501(23) .216 H(32B) -.0115(33) 1.3610(109) .4587(17) .216 H(32C) -.1127(48) 1.3441(96) .4292(7) .216 _cod_database_code 2003569