#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003606.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_2003606 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 1139 _journal_page_last 1141 _publ_section_title ; 1,2-Diiod-1,2-bis(pentamethylcyclopentadienyl)diphosphan ; _chemical_formula_sum 'C20 H30 I2 P2' _chemical_formula_weight 586.18 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' 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' _cell_length_a 8.336(2) _cell_length_b 18.259(5) _cell_length_c 15.183(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.58(2) _cell_angle_gamma 90.00 _cell_volume 2310.1(10) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_absorpt_coefficient_mu 2.862 _cell_measurement_temperature 173(2) _exptl_crystal_description prism _exptl_crystal_size_max .4 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .15 _exptl_crystal_colour rot _chemical_compound_source ? _diffrn_measurement_device 'Siemens P2~1~ diffractometer ' _diffrn_measurement_method 'omega-scan' _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 4828 _reflns_number_total 4530 _reflns_number_observed 3181 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_theta_max 30.0 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0703 _refine_ls_wR_factor_obs 0.1456 _refine_ls_wR_factor_all 0.1830 _refine_ls_goodness_of_fit_obs 1.554 _refine_ls_goodness_of_fit_all 1.532 _refine_ls_number_reflns 4524 _refine_ls_number_parameters 218 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme calc _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 2.464 _refine_diff_density_min -2.157 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.0011(2) 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 'P' 'P' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' .1023 .0942 'I' 'I' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -.4742 1.811 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 I(1) 1 0.59151(10) 0.24400(4) 0.30394(5) 0.0393(2) I(2) 1 0.17515(9) 0.22628(4) 0.17682(6) 0.0409(2) P(1) 1 0.6272(3) 0.2551(2) 0.1429(2) 0.0260(6) P(2) 1 0.3971(3) 0.22873(15) 0.0709(2) 0.0264(6) C(1) 1 0.6261(13) 0.3576(6) 0.1209(6) 0.030(2) C(2) 1 0.4659(14) 0.3940(6) 0.1296(7) 0.030(2) C(3) 1 0.4055(12) 0.4067(6) 0.0473(7) 0.028(2) C(4) 1 0.5206(14) 0.3852(6) -0.0170(7) 0.033(3) C(5) 1 0.6550(12) 0.3571(6) 0.0231(7) 0.027(2) C(6) 1 0.7627(14) 0.3922(6) 0.1761(7) 0.036(3) H(6A) 1 0.7633(14) 0.4442(6) 0.1670(7) 0.054 H(6B) 1 0.7520(14) 0.3820(6) 0.2377(7) 0.054 H(6C) 1 0.8615(14) 0.3717(6) 0.1562(7) 0.054 C(7) 1 0.3920(14) 0.4117(6) 0.2151(7) 0.038(3) H(7A) 1 0.2893(14) 0.4345(6) 0.2054(7) 0.057 H(7B) 1 0.3788(14) 0.3670(6) 0.2473(7) 0.057 H(7C) 1 0.4613(14) 0.4442(6) 0.2482(7) 0.057 C(8) 1 0.2410(14) 0.4393(7) 0.0234(9) 0.051(4) H(8A) 1 0.1869(14) 0.4496(7) 0.0770(9) 0.076 H(8B) 1 0.2531(14) 0.4838(7) -0.0094(9) 0.076 H(8C) 1 0.1792(14) 0.4049(7) -0.0111(9) 0.076 C(9) 1 0.4923(16) 0.3955(7) -0.1164(8) 0.048(3) H(9A) 1 0.5830(16) 0.3771(7) -0.1471(8) 0.072 H(9B) 1 0.3975(16) 0.3696(7) -0.1356(8) 0.072 H(9C) 1 0.4793(16) 0.4467(7) -0.1285(8) 0.072 C(10) 1 0.8076(14) 0.3338(7) -0.0165(8) 0.045(3) H(10A) 1 0.7988(14) 0.3373(7) -0.0795(8) 0.068 H(10B) 1 0.8930(14) 0.3649(7) 0.0049(8) 0.068 H(10C) 1 0.8302(14) 0.2840(7) 0.0001(8) 0.068 C(11) 1 0.4421(11) 0.1278(6) 0.0490(7) 0.027(2) C(12) 1 0.5708(13) 0.1380(6) -0.0174(7) 0.029(2) C(13) 1 0.7129(12) 0.1133(5) 0.0170(6) 0.022(2) C(14) 1 0.6843(12) 0.0848(6) 0.1056(7) 0.029(2) C(15) 1 0.5296(14) 0.0903(6) 0.1243(7) 0.031(2) C(16) 1 0.2907(14) 0.0888(6) 0.0139(8) 0.040(3) H(16A) 1 0.3134(14) 0.0380(6) 0.0033(8) 0.059 H(16B) 1 0.2079(14) 0.0927(6) 0.0564(8) 0.059 H(16C) 1 0.2555(14) 0.1116(6) -0.0401(8) 0.059 C(17) 1 0.5380(14) 0.1674(7) -0.1089(7) 0.045(3) H(17A) 1 0.6356(14) 0.1677(7) -0.1410(7) 0.067 H(17B) 1 0.4599(14) 0.1372(7) -0.1390(7) 0.067 H(17C) 1 0.4976(14) 0.2165(7) -0.1047(7) 0.067 C(18) 1 0.8729(12) 0.1143(6) -0.0250(7) 0.034(3) H(18A) 1 0.8637(12) 0.1348(6) -0.0831(7) 0.051 H(18B) 1 0.9459(12) 0.1433(6) 0.0105(7) 0.051 H(18C) 1 0.9127(12) 0.0650(6) -0.0285(7) 0.051 C(19) 1 0.8192(14) 0.0538(6) 0.1628(8) 0.039(3) H(19A) 1 0.7805(14) 0.0382(6) 0.2188(8) 0.059 H(19B) 1 0.8642(14) 0.0128(6) 0.1327(8) 0.059 H(19C) 1 0.9000(14) 0.0907(6) 0.1719(8) 0.059 C(20) 1 0.4451(15) 0.0604(7) 0.2042(8) 0.044(3) H(20A) 1 0.5227(15) 0.0382(7) 0.2438(8) 0.066 H(20B) 1 0.3908(15) 0.0991(7) 0.2341(8) 0.066 H(20C) 1 0.3684(15) 0.0242(7) 0.1848(8) 0.066 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 I(1) 0.0482(5) -0.0012(4) -0.0027(3) 0.0465(5) 0.0029(3) 0.0230(3) I(2) 0.0311(4) -0.0022(4) 0.0081(3) 0.0464(5) -0.0083(4) 0.0455(5) P(1) 0.0262(13) 0.0006(11) -0.0054(10) 0.0304(15) -0.0029(11) 0.0211(12) P(2) 0.0246(13) -0.0029(11) -0.0039(10) 0.0290(15) -0.0022(11) 0.0255(13) C(1) 0.032(6) 0.006(5) -0.001(4) 0.036(6) -0.008(4) 0.020(5) C(2) 0.048(7) -0.004(5) -0.003(5) 0.026(6) -0.003(4) 0.017(5) C(3) 0.028(6) -0.001(4) -0.010(5) 0.025(6) 0.000(5) 0.031(6) C(4) 0.044(7) -0.007(5) -0.001(5) 0.028(6) 0.001(5) 0.027(6) C(5) 0.026(6) -0.006(4) 0.000(4) 0.028(6) -0.009(5) 0.028(6) C(6) 0.043(7) -0.012(5) -0.014(5) 0.033(6) -0.001(5) 0.032(6) C(7) 0.042(7) 0.007(5) 0.000(6) 0.034(7) -0.013(5) 0.039(7) C(8) 0.041(8) -0.006(6) -0.012(7) 0.041(8) 0.007(7) 0.069(10) C(9) 0.058(8) -0.012(7) -0.005(6) 0.053(8) 0.015(6) 0.034(7) C(10) 0.041(7) -0.003(6) 0.001(6) 0.049(8) -0.006(6) 0.045(7) C(11) 0.012(5) 0.013(4) 0.000(4) 0.041(6) -0.010(5) 0.027(5) C(12) 0.032(6) -0.002(5) -0.005(4) 0.031(6) -0.006(4) 0.024(6) C(13) 0.026(5) 0.005(4) -0.003(4) 0.027(6) -0.011(4) 0.012(4) C(14) 0.023(5) -0.006(4) -0.006(4) 0.029(6) 0.006(5) 0.035(6) C(15) 0.040(7) 0.000(5) 0.004(5) 0.028(6) -0.003(5) 0.026(6) C(16) 0.036(7) -0.008(5) -0.006(6) 0.029(6) -0.017(6) 0.054(8) C(17) 0.040(7) 0.014(6) 0.007(5) 0.074(10) 0.008(6) 0.020(6) C(18) 0.018(5) -0.002(5) 0.008(4) 0.051(7) 0.000(5) 0.034(6) C(19) 0.042(7) 0.011(5) -0.013(5) 0.037(7) -0.001(5) 0.039(7) C(20) 0.043(7) -0.007(6) 0.006(6) 0.050(8) 0.014(6) 0.038(7) _cod_database_code 2003606