#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2200160.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_2200160 loop_ _publ_author_name 'Sun, Shih-Sheng' 'Zavalij, Peter Y.' 'Lees, Alistair J.' _publ_section_title ; Acetonitriletricarbonyl(2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline)rhenium(I) hexafluorophosphate ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m119 _journal_page_last m121 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Re (C26 H20 N2) (C2 H3 N) (C O)3] (P F6)' _chemical_formula_moiety 'C31 H23 N3 O3 Re 1+, F6 P1 1-' _chemical_formula_structural '[((C6H5)2(CH3)2(C12H4N2))Re(CO)3(CH3CN)](PF6)' _chemical_formula_sum 'C31 H23 F6 N3 O3 P Re' _chemical_formula_weight 816.7 _chemical_name_systematic ; 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline tricarbonyl acetonitrile rhenium hexafluorophosphate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90.00 _cell_angle_beta 103.8470(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.2648(5) _cell_length_b 23.4667(11) _cell_length_c 13.2040(6) _cell_measurement_reflns_used 7718 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 54.646 _cell_measurement_theta_min 4.440 _cell_volume 3088.2(3) _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_collection 'SMART (Bruker, 1999)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .995 _diffrn_measured_fraction_theta_max .995 _diffrn_measurement_device_type 'CCD Smart Apex' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0469 _diffrn_reflns_av_sigmaI/netI .0577 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 26336 _diffrn_reflns_theta_full 30.55 _diffrn_reflns_theta_max 30.55 _diffrn_reflns_theta_min 1.74 _diffrn_standards_decay_% .04 _exptl_absorpt_coefficient_mu 4.060 _exptl_absorpt_correction_T_max .59 _exptl_absorpt_correction_T_min .46 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prizm _exptl_crystal_F_000 1592 _exptl_crystal_size_max .20 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .13 _refine_diff_density_max 1.028 _refine_diff_density_min -.502 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .933 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 409 _refine_ls_number_reflns 9420 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .933 _refine_ls_R_factor_all .0745 _refine_ls_R_factor_gt .0419 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0464P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0998 _reflns_number_gt 6049 _reflns_number_total 9420 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file cv6006.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2200160 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' 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_type_symbol Re1 .15826(2) .101610(10) .612690(10) .04285(7) Uani d . 1 Re P1 .39210(15) .06783(7) .24644(10) .0628(4) Uani d . 1 P F1 .3868(6) .0785(2) .3612(3) .156(2) Uani d . 1 F F2 .3990(6) .0556(2) .1335(3) .163(2) Uani d . 1 F F3 .5145(7) .1030(3) .2608(7) .233(4) Uani d . 1 F F4 .2646(5) .0327(3) .2325(5) .209(3) Uani d . 1 F F5 .4679(5) .0110(2) .2817(3) .1388(18) Uani d . 1 F F6 .3117(7) .1231(3) .2162(4) .180(3) Uani d . 1 F C1 .0113(5) .1011(2) .4918(4) .0605(13) Uani d . 1 C O1 -.0826(4) .09915(18) .4241(3) .0863(14) Uani d . 1 O C2 .0435(5) .0503(3) .6618(4) .0679(16) Uani d . 1 C O2 -.0330(4) .0203(3) .6862(3) .118(2) Uani d . 1 O C3 .0735(5) .1628(3) .6659(4) .0712(16) Uani d . 1 C O3 .0143(4) .1977(2) .6969(4) .1159(18) Uani d . 1 O N1 .2529(4) .03391(17) .5509(3) .0493(9) Uani d . 1 N C4 .2920(5) -.0038(2) .5138(4) .0534(12) Uani d . 1 C C5 .3409(6) -.0520(2) .4648(4) .0711(15) Uani d . 1 C H5A .2903 -.0854 .4728 .107 Uiso calc R 1 H H5B .4340 -.0582 .4972 .107 Uiso calc R 1 H H5C .3307 -.0442 .3919 .107 Uiso calc R 1 H C6 .1546(5) .1865(3) .3953(4) .085(2) Uani d . 1 C H6A .1563 .2136 .3410 .128 Uiso calc R 1 H H6B .0887 .1979 .4320 .128 Uiso calc R 1 H H6C .1323 .1495 .3651 .128 Uiso calc R 1 H C7 .2885(4) .1843(2) .4689(3) .0518(12) Uani d . 1 C C8 .3957(5) .2117(2) .4416(3) .0551(12) Uani d . 1 C H8 .3800 .2305 .3779 .066 Uiso calc R 1 H C9 .5223(4) .2120(2) .5037(3) .0461(10) Uani d . 1 C C10 .6350(4) .2394(2) .4704(3) .0488(11) Uani d . 1 C C11 .6770(5) .2171(2) .3872(4) .0604(13) Uani d . 1 C H11 .6309 .1867 .3495 .073 Uiso calc R 1 H C12 .7890(6) .2401(3) .3596(5) .0727(15) Uani d . 1 C H12 .8188 .2245 .3044 .087 Uiso calc R 1 H C13 .8546(5) .2850(3) .4129(5) .0697(15) Uani d . 1 C H13 .9282 .3006 .3933 .084 Uiso calc R 1 H C14 .8130(6) .3076(3) .4954(4) .0764(16) Uani d . 1 C H14 .8582 .3385 .5318 .092 Uiso calc R 1 H C15 .7057(5) .2848(2) .5241(4) .0662(14) Uani d . 1 C H15 .6791 .3000 .5810 .079 Uiso calc R 1 H N2 .3056(3) .15518(16) .5589(3) .0419(8) Uani d . 1 N C16 .4328(4) .15575(17) .6251(3) .0372(9) Uani d . 1 C C17 .5410(4) .18393(18) .6013(3) .0412(9) Uani d . 1 C C18 .6688(4) .1818(2) .6741(3) .0474(11) Uani d . 1 C H18 .7419 .1999 .6580 .057 Uiso calc R 1 H C19 .6850(4) .1541(2) .7653(3) .0466(10) Uani d . 1 C H19 .7690 .1540 .8117 .056 Uiso calc R 1 H C20 .5770(4) .12494(19) .7926(3) .0377(9) Uani d . 1 C C21 .4498(4) .12524(18) .7222(3) .0360(8) Uani d . 1 C N3 .3395(3) .09939(14) .7434(3) .0388(8) Uani d . 1 N C22 .2369(5) .0478(3) .8665(4) .0731(17) Uani d . 1 C H22A .1625 .0738 .8510 .110 Uiso calc R 1 H H22B .2594 .0394 .9398 .110 Uiso calc R 1 H H22C .2128 .0132 .8278 .110 Uiso calc R 1 H C23 .3544(4) .0741(2) .8372(3) .0438(10) Uani d . 1 C C24 .4770(4) .0734(2) .9088(3) .0451(10) Uani d . 1 C H24 .4830 .0558 .9728 .054 Uiso calc R 1 H C25 .5901(4) .09747(19) .8897(3) .0420(10) Uani d . 1 C C26 .7172(4) .0964(2) .9719(3) .0488(11) Uani d . 1 C C27 .7171(6) .1155(3) 1.0708(4) .0695(16) Uani d . 1 C H27 .6383 .1296 1.0843 .083 Uiso calc R 1 H C28 .8330(7) .1139(3) 1.1499(5) .093(2) Uani d . 1 C H28 .8312 .1265 1.2164 .112 Uiso calc R 1 H C29 .9501(6) .0940(3) 1.1311(5) .084(2) Uani d . 1 C H29 1.0285 .0941 1.1839 .101 Uiso calc R 1 H C30 .9512(5) .0740(3) 1.0337(5) .0729(16) Uani d . 1 C H30 1.0305 .0599 1.0211 .088 Uiso calc R 1 H C31 .8354(4) .0744(3) .9539(4) .0576(13) Uani d . 1 C H31 .8368 .0601 .8886 .069 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 Re1 .03226(9) .05381(12) .04068(10) -.00301(8) .00519(6) .00153(8) P1 .0658(9) .0751(11) .0457(7) .0005(8) .0099(6) .0000(7) F1 .270(6) .138(4) .071(3) .074(4) .060(3) .001(3) F2 .295(7) .146(5) .059(2) .019(4) .065(3) .000(3) F3 .166(6) .255(9) .305(9) -.146(6) .106(6) -.105(6) F4 .102(4) .265(8) .243(7) -.070(4) .011(4) .029(6) F5 .194(5) .122(4) .098(3) .074(4) .030(3) .001(3) F6 .266(7) .163(5) .122(4) .111(5) .066(4) .068(4) C1 .048(3) .065(4) .063(3) -.011(2) .003(2) .011(3) O1 .059(2) .110(4) .071(3) -.019(2) -.0224(19) .021(2) C2 .045(3) .095(5) .056(3) -.022(3) -.004(2) .014(3) O2 .070(3) .181(6) .091(3) -.069(3) -.002(2) .044(3) C3 .041(3) .094(5) .075(4) .010(3) .009(2) -.015(3) O3 .074(3) .137(5) .133(4) .035(3) .018(3) -.043(3) N1 .053(2) .047(2) .046(2) .0042(19) .0080(17) -.0009(18) C4 .051(3) .058(3) .045(3) .001(2) .001(2) .007(2) C5 .081(4) .067(4) .063(3) .010(3) .013(3) -.012(3) C6 .048(3) .117(6) .078(4) -.005(3) -.009(3) .045(4) C7 .043(2) .061(3) .048(3) -.001(2) .0039(19) .010(2) C8 .055(3) .065(3) .044(3) -.001(2) .009(2) .020(2) C9 .047(2) .047(3) .046(2) -.003(2) .0143(19) .005(2) C10 .050(3) .046(3) .051(3) -.003(2) .013(2) .007(2) C11 .069(3) .053(3) .063(3) -.008(3) .023(3) .002(2) C12 .081(4) .065(4) .084(4) -.002(3) .044(3) .005(3) C13 .062(3) .063(4) .090(4) -.014(3) .031(3) .013(3) C14 .091(4) .066(4) .075(4) -.032(3) .027(3) -.002(3) C15 .076(4) .059(4) .071(3) -.016(3) .031(3) -.003(3) N2 .0352(17) .045(2) .0429(19) .0007(15) .0050(14) .0039(16) C16 .036(2) .036(2) .038(2) .0002(17) .0073(16) -.0023(17) C17 .037(2) .043(3) .045(2) .0000(18) .0121(17) .0025(18) C18 .038(2) .054(3) .051(3) -.006(2) .0129(18) .000(2) C19 .036(2) .055(3) .046(2) -.0055(19) .0023(17) -.002(2) C20 .034(2) .044(2) .035(2) .0004(17) .0065(16) -.0041(17) C21 .0341(19) .040(2) .034(2) .0000(17) .0084(15) -.0029(17) N3 .0348(17) .046(2) .0360(18) -.0047(15) .0092(13) .0001(15) C22 .053(3) .115(5) .050(3) -.026(3) .009(2) .024(3) C23 .041(2) .054(3) .037(2) -.004(2) .0107(17) .001(2) C24 .047(2) .055(3) .032(2) .003(2) .0069(17) .0074(19) C25 .037(2) .052(3) .036(2) .0039(19) .0078(16) .0001(19) C26 .039(2) .060(3) .042(2) .004(2) .0010(18) .005(2) C27 .067(3) .090(5) .048(3) .013(3) .006(2) -.009(3) C28 .087(5) .129(6) .049(3) .016(4) -.013(3) -.021(3) C29 .057(4) .105(6) .075(4) -.003(3) -.013(3) .002(4) C30 .036(3) .096(5) .081(4) .004(3) .003(2) .015(3) C31 .042(3) .080(4) .050(3) .008(2) .008(2) .004(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 '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' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C3 Re1 C2 88.7(3) ? C3 Re1 C1 88.5(2) ? C2 Re1 C1 81.5(2) ? C3 Re1 N1 179.1(2) yes C2 Re1 N1 92.0(2) ? C1 Re1 N1 91.0(2) ? C3 Re1 N2 95.6(2) ? C2 Re1 N2 174.82(19) yes C1 Re1 N2 101.47(17) ? N1 Re1 N2 83.73(15) ? C3 Re1 N3 95.91(18) ? C2 Re1 N3 101.09(16) ? C1 Re1 N3 174.91(18) yes N1 Re1 N3 84.58(13) ? N2 Re1 N3 75.66(12) yes F3 P1 F4 178.8(5) yes F3 P1 F2 89.6(4) ? F4 P1 F2 91.1(4) ? F3 P1 F6 87.1(5) ? F4 P1 F6 91.9(4) ? F2 P1 F6 93.0(3) ? F3 P1 F1 90.7(4) ? F4 P1 F1 88.6(4) ? F2 P1 F1 178.4(3) yes F6 P1 F1 88.6(3) ? F3 P1 F5 95.3(4) ? F4 P1 F5 85.7(4) ? F2 P1 F5 89.7(3) ? F6 P1 F5 176.5(3) yes F1 P1 F5 88.7(2) ? O1 C1 Re1 174.8(5) yes O2 C2 Re1 175.5(5) yes O3 C3 Re1 175.3(5) yes C4 N1 Re1 173.8(4) yes N1 C4 C5 179.2(5) yes N2 C7 C8 121.2(4) ? N2 C7 C6 120.1(4) ? C8 C7 C6 118.7(4) ? C9 C8 C7 123.1(4) ? C8 C9 C17 116.6(4) ? C8 C9 C10 121.7(4) ? C17 C9 C10 121.7(4) ? C11 C10 C15 118.4(4) ? C11 C10 C9 119.2(4) ? C15 C10 C9 122.2(4) ? C10 C11 C12 119.7(5) ? C13 C12 C11 120.3(5) ? C12 C13 C14 120.2(5) ? C15 C14 C13 119.9(5) ? C14 C15 C10 121.4(5) ? C7 N2 C16 117.2(4) ? C7 N2 Re1 128.2(3) ? C16 N2 Re1 114.6(3) ? N2 C16 C17 122.9(4) ? N2 C16 C21 116.8(3) ? C17 C16 C21 120.3(3) ? C16 C17 C9 118.9(4) ? C16 C17 C18 119.0(4) ? C9 C17 C18 122.0(4) ? C19 C18 C17 121.1(4) ? C18 C19 C20 121.6(4) ? C21 C20 C25 118.1(4) ? C21 C20 C19 119.1(4) ? C25 C20 C19 122.7(4) ? N3 C21 C20 122.9(4) ? N3 C21 C16 118.1(3) ? C20 C21 C16 118.9(4) ? C23 N3 C21 117.7(3) ? C23 N3 Re1 128.0(3) ? C21 N3 Re1 114.3(2) ? N3 C23 C24 121.2(4) ? N3 C23 C22 120.1(4) ? C24 C23 C22 118.7(4) ? C25 C24 C23 122.9(4) ? C24 C25 C20 117.1(4) ? C24 C25 C26 119.6(4) ? C20 C25 C26 123.2(4) ? C27 C26 C31 118.7(4) ? C27 C26 C25 119.1(4) ? C31 C26 C25 122.1(4) ? C26 C27 C28 120.7(5) ? C29 C28 C27 120.5(6) ? C28 C29 C30 119.5(5) ? C29 C30 C31 120.8(5) ? C30 C31 C26 119.9(5) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Re1 C3 1.899(6) yes Re1 C2 1.904(5) yes Re1 C1 1.916(5) yes Re1 N1 2.125(4) yes Re1 N2 2.211(3) yes Re1 N3 2.215(3) yes P1 F1 1.549(4) yes P1 F2 1.536(4) yes P1 F3 1.477(5) yes P1 F4 1.521(5) yes P1 F5 1.558(4) yes P1 F6 1.537(5) yes C1 O1 1.148(6) yes C2 O2 1.156(6) yes C3 O3 1.152(6) yes N1 C4 1.132(6) yes C4 C5 1.450(7) yes C6 C7 1.482(6) yes C7 N2 1.345(5) yes C7 C8 1.394(6) yes C8 C9 1.360(6) yes C9 C17 1.419(6) yes C9 C10 1.480(6) yes C10 C11 1.377(6) yes C10 C15 1.384(7) yes C11 C12 1.395(7) yes C12 C13 1.355(8) yes C13 C14 1.368(7) yes C14 C15 1.358(7) yes N2 C16 1.387(5) yes C16 C17 1.392(5) yes C16 C21 1.442(5) yes C17 C18 1.429(6) yes C18 C19 1.343(6) yes C19 C20 1.420(6) yes C20 C21 1.410(5) yes C20 C25 1.412(6) yes C21 N3 1.371(5) yes N3 C23 1.348(5) yes C22 C23 1.486(6) yes C23 C24 1.382(5) yes C24 C25 1.367(6) yes C25 C26 1.484(6) yes C26 C27 1.381(7) yes C26 C31 1.390(6) yes C27 C28 1.384(7) yes C28 C29 1.366(9) yes C29 C30 1.371(8) yes C30 C31 1.387(6) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C5 H5B F1 3_656 .960(6) 2.337(5) 3.226(8) 153.7(3) C11 H11 F3 . .932(5) 2.447(8) 3.377(9) 176.2(4) C24 H24 F2 1_556 .929(4) 2.474(5) 3.280(6) 145.1(3) 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 _geom_torsion_publ_flag C24 C25 C26 C27 -51.4(7) yes C8 C9 C10 C11 -65.9(6) yes H6A C6 C7 N2 171 no H6B C6 C7 N2 51 no H6C C6 C7 N2 -69 no H22A C22 C23 N3 -47 no H22B C22 C23 N3 -167 no H22C C22 C23 N3 72 no