#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/03/2200353.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_2200353 loop_ _publ_author_name 'Staples, Richard J.' 'Segal, Brent M.' _publ_section_title ; Triisopropylphosphine sulfide ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o432 _journal_page_last o433 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac 'C9 H21 P S' _chemical_formula_moiety 'C9 H21 P S' _chemical_formula_sum 'C9 H21 P S' _chemical_formula_weight 192.29 _chemical_name_common 'Triisopropylphosphine sulfide' _chemical_name_systematic ; Triisopropylphosphine sulfide ; _space_group_IT_number 72 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-I 2 2c' _symmetry_space_group_name_H-M 'I b a m' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 13.5730(10) _cell_length_b 13.8717(9) _cell_length_c 12.6880(10) _cell_measurement_reflns_used 89 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 18.78 _cell_measurement_theta_min 2.46 _cell_volume 2388.9(3) _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_collection 'ASTRO (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material 'CIFTAB in SHELXL97' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .999 _diffrn_measured_fraction_theta_max .999 _diffrn_measurement_device_type 'Bruker CCD' _diffrn_measurement_method '0.3\% \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0970 _diffrn_reflns_av_sigmaI/netI .0733 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 6072 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.10 _diffrn_standards_decay_% <1 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu .355 _exptl_absorpt_correction_type none _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 848 _exptl_crystal_size_max .15 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .10 _refine_diff_density_max .250 _refine_diff_density_min -.306 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 55 _refine_ls_number_reflns 1108 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.143 _refine_ls_R_factor_all .1434 _refine_ls_R_factor_gt .0694 _refine_ls_shift/su_max .052 _refine_ls_shift/su_mean .015 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0861P)^2^+1.4788P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .2179 _reflns_number_gt 525 _reflns_number_total 1108 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wn6010.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2200353 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1, y+1, -z+1/2' 'x+1, -y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x, -y, z+1/2' '-x, y, z+1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol P1 .18403(12) .23903(13) .0000 .0658(8) Uani d S 1 . . P S1 .29883(13) .32501(15) .0000 .1018(11) Uani d S 1 . . S C4 .0689(5) .3047(6) .0000 .082(3) Uani d S 1 . . C H4A .0158 .2589 .0000 .098 Uiso d SR 1 . . H C1 .1801(4) .1698(5) .1221(7) .120(3) Uani d . 1 . . C H1A .1754 .2184 .1780 .144 Uiso calc R 1 . . H C5 .0585(4) .3666(4) .1002(7) .133(3) Uani d . 1 . . C H5A -.0033 .4001 .0987 .200 Uiso calc R 1 . . H H5B .1114 .4125 .1031 .200 Uiso calc R 1 . . H H5C .0611 .3257 .1612 .200 Uiso calc R 1 . . H C3 .0872(6) .1046(6) .1374(8) .215(6) Uani d . 1 . . C H3A .0910 .0726 .2044 .323 Uiso calc R 1 . . H H3B .0845 .0575 .0821 .323 Uiso calc R 1 . . H H3C .0289 .1439 .1352 .323 Uiso calc R 1 . . H C2 .2698(5) .1158(5) .1464(7) .143(3) Uani d . 1 . . C H2A .2618 .0830 .2125 .214 Uiso calc R 1 . . H H2B .3245 .1595 .1510 .214 Uiso calc R 1 . . H H2C .2819 .0695 .0917 .214 Uiso calc R 1 . . H 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 P1 .0429(10) .0582(12) .0963(17) -.0076(8) .000 .000 S1 .0470(11) .0755(15) .183(3) -.0175(9) .000 .000 C4 .044(4) .079(5) .121(8) -.017(4) .000 .000 C1 .086(5) .115(5) .159(7) -.012(4) -.024(5) .041(5) C5 .084(4) .131(6) .185(8) -.002(4) .038(5) -.061(6) C3 .119(6) .217(9) .310(15) -.056(6) -.017(7) .183(10) C2 .143(6) .105(5) .181(10) .018(5) -.064(6) .015(6) 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 P1 C4 . 1.809(8) ? P1 C1 10 1.824(8) ? P1 C1 . 1.824(8) ? P1 S1 . 1.962(2) ? C4 C5 . 1.540(7) ? C4 C5 10 1.540(7) ? C1 C2 . 1.462(8) ? C1 C3 . 1.564(8) ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C4 P1 C1 . 10 103.9(2) C4 P1 C1 . . 103.9(2) C1 P1 C1 10 . 116.3(5) C4 P1 S1 . . 112.3(3) C1 P1 S1 10 . 110.1(2) C1 P1 S1 . . 110.1(2) C5 C4 C5 . 10 111.2(7) C5 C4 P1 . . 111.1(4) C5 C4 P1 10 . 111.1(4) C2 C1 C3 . . 110.4(6) C2 C1 P1 . . 115.2(6) C3 C1 P1 . . 115.7(6) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion C1 P1 C4 C5 10 . 178.9(5) C1 P1 C4 C5 . . 56.8(5) S1 P1 C4 C5 . . -62.2(4) C1 P1 C4 C5 10 10 -56.8(5) C1 P1 C4 C5 . 10 -178.9(5) S1 P1 C4 C5 . 10 62.2(4) C4 P1 C1 C2 . . -174.9(5) C1 P1 C1 C2 10 . 71.7(6) S1 P1 C1 C2 . . -54.4(6) C4 P1 C1 C3 . . 54.3(7) C1 P1 C1 C3 10 . -59.2(8) S1 P1 C1 C3 . . 174.8(5)