#------------------------------------------------------------------------------ #$Date: 2008-03-04 18:06:22 +0000 (Tue, 04 Mar 2008) $ #$Revision: 230 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003600.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_2003600 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1209 _journal_page_last 1211 _publ_section_title ; 1,1-Dichloro-3,3,5,5-tetraphenyl-1\l^4^,2,6,3\l^5^,5\l^5^selenadiazadiphosphorin ; _chemical_formula_moiety 'C25 H22 Cl2 N2 P2 Se,2(C H Cl3)' _chemical_formula_sum 'C27 H24 Cl8 N2 P2 Se' _chemical_formula_weight 800.98 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _symmetry_space_group_name_H-M 'P 21/n' _cell_length_a 10.785(5) _cell_length_b 15.709(6) _cell_length_c 20.884(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.89(3) _cell_angle_gamma 90.00 _cell_volume 3474.5(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 40 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_absorpt_coefficient_mu 1.810 _cell_measurement_temperature 293 _exptl_crystal_description 'transparent block' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_colour yellow _chemical_compound_source 'dimethylformamide/chloroform' _diffrn_measurement_device 'Stoe four circle' _diffrn_measurement_method '\w/2\q scans, profile fitting (Clegg, 1981)' _exptl_absorpt_correction_type 'empirical, using \y-scans' _exptl_absorpt_correction_T_min 0.36 _exptl_absorpt_correction_T_max 0.41 _diffrn_reflns_number 8144 _reflns_number_total 6084 _reflns_number_observed 2845 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0736 _diffrn_reflns_theta_max 25 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.1048 _refine_ls_wR_factor_obs 0.2524 _refine_ls_wR_factor_all 0.2991 _refine_ls_goodness_of_fit_obs 1.278 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_number_reflns 6084 _refine_ls_number_parameters 328 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1460P)^2^] where P=(F' _refine_ls_shift/esd_max 0.000 _refine_diff_density_max .903 _refine_diff_density_min -.695 _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' .0033 .0016 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0000 .0000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .0061 .0033 'P' 'P' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .1023 .0942 'Cl' 'Cl' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .1484 .158 'Se' 'Se' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -.0929 2.2 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 Se 1 0.09771(9) 0.15020(6) 0.25122(6) 0.0567(4) Cl1 1 -0.0789(3) 0.1253(2) 0.3027(2) 0.1031(14) Cl2 1 0.2740(3) 0.2343(2) 0.1843(2) 0.0695(9) N1 1 0.0654(8) 0.0740(5) 0.1915(5) 0.061(3) N2 1 0.2149(8) 0.1191(5) 0.3155(4) 0.055(2) P1 1 0.0890(2) -0.0268(2) 0.20428(14) 0.0450(7) P2 1 0.2532(2) 0.0220(2) 0.33248(14) 0.0493(7) C1 1 0.1381(8) -0.0512(6) 0.2900(5) 0.048(3) H1A 1 0.0645(8) -0.0507(6) 0.3104(5) 0.057 H1B 1 0.1733(8) -0.1082(6) 0.2943(5) 0.057 C11 1 0.2021(9) -0.0636(7) 0.1594(5) 0.047(2) C12 1 0.2696(11) -0.0062(9) 0.1290(7) 0.083(4) H12 1 0.2590(11) 0.0519(9) 0.1346(7) 0.099 C13 1 0.3516(13) -0.0338(11) 0.0908(8) 0.100(5) H13 1 0.3935(13) 0.0058(11) 0.0695(8) 0.120 C14 1 0.3732(13) -0.1201(11) 0.0834(8) 0.094(5) H14 1 0.4277(13) -0.1390(11) 0.0569(8) 0.113 C15 1 0.3121(13) -0.1763(9) 0.1163(7) 0.084(4) H15 1 0.3285(13) -0.2342(9) 0.1138(7) 0.101 C16 1 0.2271(11) -0.1493(8) 0.1529(6) 0.067(3) H16 1 0.1853(11) -0.1892(8) 0.1739(6) 0.081 C11' 1 -0.0575(9) -0.0847(7) 0.1778(5) 0.052(3) C12' 1 -0.0699(11) -0.1668(7) 0.1983(7) 0.071(4) H12' 1 -0.0036(11) -0.1933(7) 0.2261(7) 0.085 C13' 1 -0.1827(13) -0.2095(8) 0.1772(7) 0.085(4) H13' 1 -0.1921(13) -0.2652(8) 0.1905(7) 0.102 C14' 1 -0.2800(12) -0.1698(9) 0.1368(7) 0.086(4) H14' 1 -0.3556(12) -0.1987(9) 0.1231(7) 0.103 C15' 1 -0.2676(12) -0.0881(10) 0.1164(7) 0.094(5) H15' 1 -0.3341(12) -0.0622(10) 0.0883(7) 0.113 C16' 1 -0.1546(9) -0.0431(8) 0.1377(6) 0.066(3) H16' 1 -0.1458(9) 0.0130(8) 0.1251(6) 0.080 C21 1 0.4016(10) -0.0034(7) 0.3104(5) 0.053(3) C22 1 0.4708(10) 0.0620(8) 0.2881(6) 0.073(4) H22 1 0.4415(10) 0.1178(8) 0.2861(6) 0.087 C23 1 0.5850(11) 0.0418(11) 0.2689(8) 0.100(5) H23 1 0.6303(11) 0.0846(11) 0.2528(8) 0.120 C24 1 0.6299(12) -0.0377(10) 0.2733(7) 0.083(4) H24 1 0.7074(12) -0.0496(10) 0.2619(7) 0.100 C25 1 0.5619(13) -0.1015(10) 0.2945(8) 0.092(5) H25 1 0.5922(13) -0.1570(10) 0.2960(8) 0.110 C26 1 0.4476(10) -0.0846(8) 0.3139(6) 0.066(3) H26 1 0.4029(10) -0.1284(8) 0.3291(6) 0.080 C21' 0.50 0.2582(10) 0.0052(7) 0.4166(4) 0.062(3) C22' 0.546(12) 0.3633(11) -0.0245(11) 0.4605(7) 0.115(10) C23' 0.546(12) 0.3559(20) -0.0382(14) 0.5256(6) 0.160(15) C24' 0.546(12) 0.2432(25) -0.0221(13) 0.5471(5) 0.095(12) C25' 0.546(12) 0.1381(19) 0.0076(13) 0.5034(8) 0.131(12) C26' 0.546(12) 0.1455(10) 0.0213(11) 0.4382(7) 0.108(10) H22' 0.546(12) 0.4408(12) -0.0355(17) 0.4457(11) 0.130 H23' 0.546(12) 0.4283(26) -0.0586(20) 0.5557(9) 0.200 H24' 0.546(12) 0.2381(34) -0.0315(18) 0.5920(6) 0.110 H25' 0.546(12) 0.0606(23) 0.0187(19) 0.5182(13) 0.160 H26' 0.546(12) 0.0731(12) 0.0417(17) 0.4082(11) 0.120 C21" 0.50 0.2582(10) 0.0052(7) 0.4166(4) 0.062(3) C22" 0.454(12) 0.2797(16) 0.0740(7) 0.4594(7) 0.099(11) C23" 0.454(12) 0.2888(20) 0.0608(12) 0.5262(6) 0.092(10) C24" 0.454(12) 0.2765(21) -0.0210(15) 0.5501(4) 0.084(13) C25" 0.454(12) 0.2550(22) -0.0898(11) 0.5071(8) 0.118(13) C26" 0.454(12) 0.2458(17) -0.0766(6) 0.4403(7) 0.098(11) H22" 0.454(12) 0.2882(25) 0.1304(7) 0.4430(10) 0.120 H23" 0.454(12) 0.3037(29) 0.1082(15) 0.5558(9) 0.120 H24" 0.454(12) 0.2828(28) -0.0301(20) 0.5960(5) 0.110 H25" 0.454(12) 0.2465(32) -0.1461(12) 0.5235(11) 0.140 H26" 0.454(12) 0.2310(26) -0.1239(7) 0.4108(10) 0.120 C1A 1 0.5187(16) 0.2286(20) 0.1008(11) 0.169(10) H1C 1 0.4520(16) 0.2199(20) 0.1262(11) 0.203 Cl1A 1 0.6034(6) 0.3214(6) 0.1300(4) 0.214(3) Cl2A 1 0.6104(11) 0.1452(6) 0.1102(6) 0.288(6) Cl3A 1 0.4533(11) 0.2435(11) 0.0262(5) 0.436(12) C1B 1 1.0265(18) 0.1930(13) 0.0459(10) 0.133(7) H1D 1 1.0965(18) 0.1894(13) 0.0833(10) 0.160 Cl1B 1 0.8989(7) 0.2245(8) 0.0695(5) 0.282(6) Cl2B 1 0.9963(12) 0.0972(7) 0.0119(4) 0.304(6) Cl3B 1 1.0675(15) 0.2484(11) -0.0112(6) 0.426(11) 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 Se 0.0472(6) 0.0047(5) 0.0144(5) 0.0358(6) -0.0031(6) 0.0878(9) Cl1 0.075(2) 0.012(2) 0.058(2) 0.090(3) 0.001(3) 0.158(4) Cl2 0.068(2) -0.0086(14) 0.024(2) 0.049(2) -0.004(2) 0.094(2) N1 0.061(5) 0.000(4) 0.001(5) 0.035(5) -0.008(5) 0.083(7) N2 0.057(5) -0.001(4) -0.002(5) 0.039(5) -0.004(4) 0.063(6) P1 0.0414(13) -0.0051(11) 0.0056(12) 0.0399(14) -0.0010(13) 0.052(2) P2 0.0446(14) -0.0006(12) 0.0043(13) 0.044(2) -0.0058(14) 0.057(2) C1 0.043(5) 0.005(4) 0.007(5) 0.028(5) 0.005(5) 0.071(7) C11 0.042(5) -0.006(5) -0.002(5) 0.054(6) 0.000(5) 0.042(6) C12 0.085(9) -0.021(7) 0.059(8) 0.071(8) 0.000(8) 0.107(11) C13 0.089(10) -0.025(9) 0.056(10) 0.100(12) -0.008(11) 0.125(13) C14 0.080(9) 0.009(9) 0.051(9) 0.112(13) -0.017(10) 0.103(12) C15 0.095(10) 0.022(8) 0.035(9) 0.075(9) 0.008(8) 0.089(10) C16 0.080(8) 0.020(6) 0.033(7) 0.052(7) 0.003(6) 0.076(9) C11' 0.047(6) -0.010(5) 0.011(5) 0.051(6) -0.016(6) 0.058(7) C12' 0.059(7) -0.009(6) 0.001(7) 0.055(8) 0.008(7) 0.094(10) C13' 0.081(9) -0.028(7) 0.006(9) 0.051(8) -0.006(8) 0.117(12) C14' 0.058(7) -0.031(7) -0.002(8) 0.084(10) 0.005(9) 0.109(12) C15' 0.059(8) -0.004(8) -0.017(7) 0.110(12) 0.009(10) 0.100(12) C16' 0.038(5) 0.004(5) -0.016(6) 0.067(8) -0.002(7) 0.084(9) C21 0.058(6) -0.008(5) 0.009(5) 0.055(7) 0.000(5) 0.046(7) C22 0.052(7) -0.004(6) 0.009(7) 0.067(8) 0.012(7) 0.097(10) C23 0.049(7) -0.005(8) 0.024(8) 0.107(13) 0.017(11) 0.146(15) C24 0.053(7) -0.002(7) 0.008(7) 0.093(11) -0.006(9) 0.102(11) C25 0.070(8) 0.014(8) 0.001(9) 0.078(10) -0.001(9) 0.121(13) C26 0.043(6) 0.005(5) 0.010(6) 0.056(7) -0.005(7) 0.098(10) C1A 0.074(11) -0.023(16) 0.046(12) 0.290(33) -0.027(21) 0.153(20) Cl1A 0.149(5) -0.053(6) 0.082(6) 0.250(8) -0.075(7) 0.260(9) Cl2A 0.347(13) 0.032(9) 0.235(12) 0.191(8) 0.085(9) 0.389(15) Cl3A 0.349(14) 0.306(18) -0.067(10) 0.726(29) -0.191(14) 0.186(9) C1B 0.120(14) -0.033(13) 0.018(13) 0.137(16) -0.037(14) 0.140(17) Cl1B 0.168(7) 0.111(8) 0.013(6) 0.422(15) -0.098(9) 0.245(9) Cl2B 0.462(16) 0.053(11) -0.077(9) 0.236(10) -0.057(7) 0.160(7) Cl3B 0.478(20) -0.296(19) 0.150(14) 0.561(25) 0.000(15) 0.268(13)