#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/01/2200145.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_2200145 loop_ _publ_author_name 'Cabeza, Javier A.' 'del R\'io, Ignacio' 'Zu\~niga-Villarreal, No\'e' 'Garc\'ia-Granda, Santiago' _publ_section_title ; (Benzophenone imine-N)nonacarbonyldirhenium(0)(Re---Re) ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m130 _journal_page_last m131 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Re2 (C13 H11 N1) (C1 O1)9]' _chemical_formula_moiety 'C22 H11 N O9 Re2' _chemical_formula_sum 'C22 H11 N O9 Re2' _chemical_formula_weight 805.72 _chemical_name_systematic ; (N-benzophenoneimine) enea-carbonyl dirhenium(0) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 102.780(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.8071(6) _cell_length_b 13.6951(8) _cell_length_c 16.4285(11) _cell_measurement_reflns_used 2241 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 1 _cell_volume 2371.3(3) _computing_cell_refinement 'CRYSDA (Beurskens et al., 1992)' _computing_data_collection 'CAD-4 EXPRESS (Enraf-Nonius, 1994)' _computing_data_reduction 'REFLEX (Garcia-Granda et al., 1999)' _computing_molecular_graphics 'EUCLID (Spek, 1982)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'DIRDIF (Beurskens et al., 1992)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .966 _diffrn_measured_fraction_theta_max .966 _diffrn_measurement_device_type 'Nonius CAD-4' _diffrn_measurement_method \w-2\q _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 .054 _diffrn_reflns_av_sigmaI/netI .083 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 7361 _diffrn_reflns_theta_full 25.97 _diffrn_reflns_theta_max 25.97 _diffrn_reflns_theta_min 1.93 _diffrn_standards_decay_% 2.36 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 10.251 _exptl_absorpt_correction_T_max .485 _exptl_absorpt_correction_T_min .113 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(XABS2; Parkin et al., 1995)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.275 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 1488 _exptl_crystal_size_max .26 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .07 _refine_diff_density_max .94 _refine_diff_density_min -1.28 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .995 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 307 _refine_ls_number_reflns 4499 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .995 _refine_ls_R_factor_all .117 _refine_ls_R_factor_gt .034 _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^)+(0.0426P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .094 _reflns_number_gt 2349 _reflns_number_total 4499 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ci6007.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_original_cell_volume 2371.3(2) _cod_database_code 2200145 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Re1 .25591(4) .23125(4) .33923(2) .03652(13) Uani d . 1 . . Re Re2 .48456(4) .26694(4) .48277(3) .04584(15) Uani d . 1 . . Re N1 .1550(7) .1688(6) .4302(4) .0341(19) Uani d . 1 . . N H1 .1893 .1150 .4508 .041 Uiso calc R 1 . . H O14 .1700(8) .4435(7) .3689(5) .068(3) Uani d . 1 . . O O15 .0416(8) .1908(7) .1867(4) .068(2) Uani d . 1 . . O O16 .3742(8) .0282(7) .3178(5) .066(2) Uani d . 1 . . O O17 .4138(9) .3160(7) .2217(5) .085(3) Uani d . 1 . . O O18 .7111(10) .3128(9) .6285(6) .105(4) Uani d . 1 . . O O19 .4194(9) .0615(7) .5402(5) .072(3) Uani d . 1 . . O O20 .2814(8) .3488(6) .5735(5) .074(3) Uani d . 1 . . O O21 .4950(9) .4674(8) .3963(6) .085(3) Uani d . 1 . . O O22 .6364(8) .1639(7) .3649(5) .078(3) Uani d . 1 . . O C1 .0589(9) .1908(8) .4608(5) .035(2) Uani d . 1 . . C C2 .0347(10) .1340(7) .5339(5) .037(2) Uani d . 1 . . C C3 -.0879(11) .1317(8) .5449(6) .049(3) Uani d . 1 . . C H3 -.1516 .1641 .5074 .059 Uiso calc R 1 . . H C4 -.1176(13) .0811(8) .6120(7) .056(3) Uani d . 1 . . C H4 -.2002 .0799 .6199 .067 Uiso calc R 1 . . H C5 -.0220(14) .0334(9) .6658(8) .063(4) Uani d . 1 . . C H5 -.0409 -.0012 .7102 .076 Uiso calc R 1 . . H C6 .0991(12) .0349(8) .6563(6) .052(3) Uani d . 1 . . C H6 .1625 .0022 .6939 .063 Uiso calc R 1 . . H C7 .1276(11) .0857(8) .5899(5) .049(3) Uani d . 1 . . C H7 .2108 .0871 .5832 .059 Uiso calc R 1 . . H C8 -.0300(9) .2707(8) .4255(6) .039(2) Uani d . 1 . . C C9 -.0470(11) .3485(8) .4760(6) .049(3) Uani d . 1 . . C H9 -.0013 .3517 .5310 .059 Uiso calc R 1 . . H C10 -.1319(12) .4206(9) .4439(7) .060(3) Uani d . 1 . . C H10 -.1450 .4723 .4777 .072 Uiso calc R 1 . . H C11 -.1963(12) .4175(10) .3640(7) .064(4) Uani d . 1 . . C H11 -.2506 .4683 .3420 .076 Uiso calc R 1 . . H C12 -.1820(11) .3400(10) .3152(6) .055(3) Uani d . 1 . . C H12 -.2299 .3363 .2607 .066 Uiso calc R 1 . . H C13 -.0980(9) .2675(9) .3455(6) .045(3) Uani d . 1 . . C H13 -.0871 .2157 .3112 .054 Uiso calc R 1 . . H C14 .1985(11) .3651(9) .3593(6) .044(3) Uani d . 1 . . C C15 .1190(11) .2073(8) .2463(6) .044(3) Uani d . 1 . . C C16 .3304(11) .1019(8) .3264(6) .045(3) Uani d . 1 . . C C17 .3547(11) .2867(9) .2662(6) .054(3) Uani d . 1 . . C C18 .6254(13) .2947(11) .5735(8) .071(4) Uani d . 1 . . C C19 .4484(11) .1363(11) .5217(7) .053(3) Uani d . 1 . . C C20 .3577(12) .3186(9) .5398(6) .054(3) Uani d . 1 . . C C21 .4927(11) .3932(10) .4280(7) .058(3) Uani d . 1 . . C C22 .5853(11) .2033(9) .4093(7) .056(3) Uani d . 1 . . C 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 .0405(2) .0380(3) .0323(2) -.0003(2) .01060(17) .00094(19) Re2 .0400(3) .0459(3) .0493(3) .0020(2) .0048(2) -.0043(2) N1 .042(5) .020(5) .039(4) -.001(4) .005(4) .003(4) O14 .089(7) .047(6) .075(6) .002(5) .033(5) .002(5) O15 .063(6) .088(7) .042(4) .007(5) -.007(4) .001(4) O16 .065(6) .054(6) .079(6) .011(5) .015(5) -.017(5) O17 .098(7) .099(8) .077(6) -.025(6) .061(6) .002(5) O18 .070(7) .126(11) .100(8) -.003(7) -.019(6) -.020(7) O19 .076(7) .061(7) .088(6) .017(6) .036(5) .006(5) O20 .084(7) .058(6) .088(6) .018(5) .035(6) -.004(5) O21 .096(8) .063(7) .096(7) -.018(6) .023(6) -.003(6) O22 .065(6) .089(8) .093(7) .000(5) .042(6) -.019(5) C1 .047(6) .032(6) .029(5) -.013(5) .014(5) -.005(4) C2 .046(6) .032(7) .034(5) -.011(5) .012(5) -.006(4) C3 .059(8) .042(8) .047(6) -.008(6) .015(6) -.006(5) C4 .079(10) .037(8) .059(7) -.013(7) .031(7) -.004(6) C5 .097(12) .034(8) .067(8) -.016(8) .039(8) -.007(6) C6 .077(9) .040(8) .033(5) .005(7) .000(6) .009(5) C7 .057(8) .055(9) .034(6) -.001(6) .006(5) .000(5) C8 .030(5) .039(7) .048(6) .006(5) .007(4) .006(5) C9 .076(9) .039(8) .035(6) .003(6) .017(6) -.003(5) C10 .077(9) .049(9) .060(7) .021(7) .025(7) .010(6) C11 .075(9) .059(10) .056(7) .029(7) .012(7) .021(6) C12 .049(7) .072(10) .040(6) .008(7) .001(5) .014(6) C13 .040(6) .053(7) .045(5) .005(6) .015(5) -.002(5) C14 .062(8) .034(8) .039(6) -.011(6) .016(5) -.008(5) C15 .060(8) .040(8) .035(6) -.002(6) .016(6) .001(5) C16 .052(7) .033(8) .047(6) -.007(6) .007(5) -.008(5) C17 .058(8) .063(10) .039(6) -.017(6) .003(5) -.010(5) C18 .064(9) .079(12) .069(9) .018(8) .010(7) .003(7) C19 .034(6) .067(10) .059(7) .002(6) .014(5) -.002(7) C20 .072(9) .043(8) .043(6) -.003(7) -.001(6) -.009(5) C21 .044(7) .055(10) .073(8) -.009(7) .006(6) .008(7) C22 .048(7) .050(9) .063(7) .002(6) .002(6) .007(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 Re1 C15 . 1.904(11) yes Re1 C17 . 1.929(11) yes Re1 C16 . 1.976(12) yes Re1 C14 . 1.986(12) yes Re1 N1 . 2.209(7) yes Re1 Re2 . 3.0542(6) yes Re2 C18 . 1.918(14) yes Re2 C20 . 1.956(12) yes Re2 C21 . 1.960(13) yes Re2 C19 . 1.968(14) yes Re2 C22 . 1.995(12) yes N1 C1 . 1.285(11) yes N1 H1 . .8600 ? O14 C14 . 1.137(13) yes O15 C15 . 1.160(12) yes O16 C16 . 1.136(12) yes O17 C17 . 1.146(11) yes O18 C18 . 1.169(15) yes O19 C19 . 1.133(13) yes O20 C20 . 1.166(12) yes O21 C21 . 1.145(13) yes O22 C22 . 1.143(12) yes C1 C8 . 1.486(14) ? C1 C2 . 1.501(12) ? C2 C7 . 1.373(14) ? C2 C3 . 1.377(13) ? C3 C4 . 1.398(13) ? C3 H3 . .9300 ? C4 C5 . 1.367(16) ? C4 H4 . .9300 ? C5 C6 . 1.352(16) ? C5 H5 . .9300 ? C6 C7 . 1.385(12) ? C6 H6 . .9300 ? C7 H7 . .9300 ? C8 C13 . 1.357(13) ? C8 C9 . 1.387(14) ? C9 C10 . 1.372(15) ? C9 H9 . .9300 ? C10 C11 . 1.344(15) ? C10 H10 . .9300 ? C11 C12 . 1.359(15) ? C11 H11 . .9300 ? C12 C13 . 1.363(14) ? C12 H12 . .9300 ? C13 H13 . .9300 ? 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' 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' Re Re -1.0185 7.2310 '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 C15 Re1 C17 90.5(4) yes C15 Re1 C16 91.3(4) yes C17 Re1 C16 89.6(5) yes C15 Re1 C14 94.4(5) yes C17 Re1 C14 88.6(4) yes C16 Re1 C14 174.0(5) yes C15 Re1 N1 93.6(3) yes C17 Re1 N1 175.9(4) yes C16 Re1 N1 89.9(4) yes C14 Re1 N1 91.5(4) yes C15 Re1 Re2 177.1(3) yes C17 Re1 Re2 87.3(3) yes C16 Re1 Re2 86.9(3) yes C14 Re1 Re2 87.3(3) yes N1 Re1 Re2 88.6(2) yes C18 Re2 C20 94.3(5) yes C18 Re2 C21 94.2(6) yes C20 Re2 C21 90.5(5) yes C18 Re2 C19 96.2(6) yes C20 Re2 C19 87.9(5) yes C21 Re2 C19 169.5(5) yes C18 Re2 C22 96.4(5) yes C20 Re2 C22 169.0(5) yes C21 Re2 C22 91.2(5) yes C19 Re2 C22 88.5(5) yes C18 Re2 Re1 177.6(4) yes C20 Re2 Re1 83.9(3) yes C21 Re2 Re1 84.1(4) yes C19 Re2 Re1 85.4(3) yes C22 Re2 Re1 85.4(3) yes C1 N1 Re1 137.4(7) yes C1 N1 H1 111.3 ? Re1 N1 H1 111.3 ? N1 C1 C8 122.0(8) ? N1 C1 C2 119.3(10) ? C8 C1 C2 118.7(8) ? C7 C2 C3 118.8(9) ? C7 C2 C1 123.7(9) ? C3 C2 C1 117.4(10) ? C2 C3 C4 120.8(11) ? C2 C3 H3 119.6 ? C4 C3 H3 119.6 ? C5 C4 C3 118.3(12) ? C5 C4 H4 120.9 ? C3 C4 H4 120.9 ? C6 C5 C4 122.0(11) ? C6 C5 H5 119.0 ? C4 C5 H5 119.0 ? C5 C6 C7 119.2(11) ? C5 C6 H6 120.4 ? C7 C6 H6 120.4 ? C2 C7 C6 120.9(10) ? C2 C7 H7 119.6 ? C6 C7 H7 119.6 ? C13 C8 C9 119.2(10) ? C13 C8 C1 121.2(10) ? C9 C8 C1 119.5(9) ? C10 C9 C8 119.3(10) ? C10 C9 H9 120.4 ? C8 C9 H9 120.4 ? C11 C10 C9 120.7(11) ? C11 C10 H10 119.6 ? C9 C10 H10 119.6 ? C10 C11 C12 119.9(12) ? C10 C11 H11 120.0 ? C12 C11 H11 120.0 ? C11 C12 C13 120.4(11) ? C11 C12 H12 119.8 ? C13 C12 H12 119.8 ? C8 C13 C12 120.3(11) ? C8 C13 H13 119.8 ? C12 C13 H13 119.8 ? O14 C14 Re1 176.7(10) ? O15 C15 Re1 175.4(9) ? O16 C16 Re1 178.6(10) ? O17 C17 Re1 177.3(11) ? O18 C18 Re2 179.2(14) ? O19 C19 Re2 175.0(11) ? O20 C20 Re2 179.4(11) ? O21 C21 Re2 178.5(12) ? O22 C22 Re2 175.8(11) ? 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 C17 Re1 Re2 C20 134.3(5) C16 Re1 Re2 C20 -136.0(5) C14 Re1 Re2 C20 45.5(5) N1 Re1 Re2 C20 -46.0(4) C17 Re1 Re2 C21 43.1(5) C16 Re1 Re2 C21 132.9(5) C14 Re1 Re2 C21 -45.6(5) N1 Re1 Re2 C21 -137.2(4) C17 Re1 Re2 C19 -137.4(5) C16 Re1 Re2 C19 -47.7(4) C14 Re1 Re2 C19 133.9(4) N1 Re1 Re2 C19 42.3(4) C17 Re1 Re2 C22 -48.6(5) C16 Re1 Re2 C22 41.1(4) C14 Re1 Re2 C22 -137.3(4) N1 Re1 Re2 C22 131.1(4) C15 Re1 N1 C1 -68.8(10) C16 Re1 N1 C1 -160.1(10) C14 Re1 N1 C1 25.7(10) Re2 Re1 N1 C1 113.0(10) Re1 N1 C1 C8 10.5(16) Re1 N1 C1 C2 -169.9(7) N1 C1 C2 C7 25.0(15) C8 C1 C2 C7 -155.4(10) N1 C1 C2 C3 -155.6(9) C8 C1 C2 C3 24.0(14) C7 C2 C3 C4 .0(16) C1 C2 C3 C4 -179.4(9) C2 C3 C4 C5 -.6(16) C3 C4 C5 C6 .8(18) C4 C5 C6 C7 -.4(18) C3 C2 C7 C6 .4(16) C1 C2 C7 C6 179.8(10) C5 C6 C7 C2 -.2(17) N1 C1 C8 C13 61.2(14) C2 C1 C8 C13 -118.4(10) N1 C1 C8 C9 -120.8(11) C2 C1 C8 C9 59.6(13) C13 C8 C9 C10 -.1(16) C1 C8 C9 C10 -178.1(10) C8 C9 C10 C11 -1.4(18) C9 C10 C11 C12 3(2) C10 C11 C12 C13 -3.3(19) C9 C8 C13 C12 -.1(16) C1 C8 C13 C12 177.9(9) C11 C12 C13 C8 1.8(17) _cod_database_fobs_code 2200145 _journal_paper_doi 10.1107/S1600536801003658