#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/18/2011878.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_2011878 loop_ _publ_author_name 'Abou Rida, Maurice' 'Saikaili, Joseph' 'Smith, Anthony K.' 'Thozet, Alain' _publ_section_title ; Dicarbonyldi-\m-chloro-cis,cis-\h^4^-1,5-cyclooctadienedirhodium(I) ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 352 _journal_page_last 353 _journal_paper_doi 10.1107/S0108270100020035 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Rh2 Cl2 (CO)2 (C8 H12 )]' _chemical_formula_moiety 'C10 H12 Cl2 O2 Rh2' _chemical_formula_sum 'C10 H12 Cl2 O2 Rh2' _chemical_formula_weight 440.92 _chemical_name_systematic Di-\m-chloro-dicarbonyl-cis,cis-\h^4^-1,5-cyclooctadienedirhodium(I) _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' _cell_angle_alpha 90.00 _cell_angle_beta 92.19(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.6500(12) _cell_length_b 12.261(3) _cell_length_c 16.058(3) _cell_measurement_reflns_used 15389 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 30.02 _cell_measurement_theta_min 2.09 _cell_volume 1308.3(5) _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_collection 'Kappa CCD Software (Enraf-Nonius, 1997)' _computing_data_reduction DENZO _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'SHELXCIF-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .965 _diffrn_measured_fraction_theta_max .965 _diffrn_measurement_device_type ' NONIUS KAPPA CCD' _diffrn_measurement_method 'area detector' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71069 _diffrn_reflns_av_R_equivalents .0000 _diffrn_reflns_av_sigmaI/netI .0665 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 15389 _diffrn_reflns_theta_full 30.02 _diffrn_reflns_theta_max 30.02 _diffrn_reflns_theta_min 2.09 _exptl_absorpt_coefficient_mu 2.912 _exptl_absorpt_correction_type none _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 848 _exptl_crystal_size_max .15 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _refine_diff_density_max 1.013 _refine_diff_density_min -1.278 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 145 _refine_ls_number_reflns 3699 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.118 _refine_ls_R_factor_all .1182 _refine_ls_R_factor_gt .0671 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1960 _reflns_number_gt 2261 _reflns_number_total 3699 _reflns_threshold_expression I>2\s(I) _cod_data_source_file gd1124.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2011878 _cod_database_fobs_code 2011878 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 Rh1 .25775(9) .44712(4) .26378(4) .0429(2) Uani d . 1 . . Rh Rh2 -.08231(10) .43789(5) .40667(4) .0510(2) Uani d . 1 . . Rh Cl1 .0824(3) .58375(17) .34039(13) .0588(6) Uani d . 1 . . Cl Cl2 .2106(4) .33330(18) .38400(14) .0682(6) Uani d . 1 . . Cl O2 -.2848(11) .2460(5) .4799(4) .091(2) Uani d . 1 . . O O1 -.4441(10) .5760(5) .4245(5) .085(2) Uani d . 1 . . O C1 .3903(14) .5657(6) .1892(7) .063(2) Uani d . 1 . . C H1 .3750 .6158 .2319 .082 Uiso calc R 1 . . H C2 .6035(15) .5334(9) .1698(8) .087(3) Uani d . 1 . . C H2A .6323 .5601 .1147 .113 Uiso calc R 1 . . H H2B .6953 .5695 .2093 .113 Uiso calc R 1 . . H C3 .6446(14) .4151(8) .1727(7) .072(3) Uani d . 1 . . C H3A .7766 .4036 .1990 .093 Uiso calc R 1 . . H H3B .6487 .3879 .1160 .093 Uiso calc R 1 . . H C4 .4924(12) .3492(7) .2188(5) .057(2) Uani d . 1 . . C H4 .5250 .3315 .2740 .074 Uiso calc R 1 . . H C5 .3113(13) .3133(6) .1866(5) .055(2) Uani d . 1 . . C H5 .2286 .2745 .2214 .072 Uiso calc R 1 . . H C6 .2382(17) .3329(8) .0988(7) .081(3) Uani d . 1 . . C H6A .3281 .2966 .0615 .105 Uiso calc R 1 . . H H6B .1060 .3003 .0906 .105 Uiso calc R 1 . . H C7 .226(2) .4504(10) .0761(7) .104(4) Uani d . 1 . . C H7A .1073 .4613 .0398 .135 Uiso calc R 1 . . H H7B .3424 .4691 .0447 .135 Uiso calc R 1 . . H C8 .2148(15) .5272(7) .1488(6) .063(2) Uani d . 1 . . C H8 .0901 .5493 .1670 .082 Uiso calc R 1 . . H C9 -.3070(14) .5237(8) .4192(6) .060(2) Uani d . 1 . . C C10 -.2082(14) .3191(8) .4530(5) .062(2) 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 Rh1 .0454(4) .0412(3) .0426(4) .0020(2) .0078(3) .0023(2) Rh2 .0527(4) .0623(4) .0384(4) .0012(3) .0078(3) .0015(3) Cl1 .0612(13) .0526(11) .0640(14) .0080(9) .0200(11) -.0011(9) Cl2 .0786(15) .0684(13) .0590(13) .0218(11) .0204(11) .0205(10) O2 .113(6) .073(4) .091(5) -.021(4) .034(5) .010(4) O1 .053(4) .099(5) .103(6) .010(4) .012(4) .000(4) C1 .072(6) .054(5) .065(6) -.013(4) .016(5) .011(4) C2 .061(6) .100(8) .100(9) -.013(6) .025(6) .008(7) C3 .046(5) .086(7) .083(7) .001(5) .006(5) -.025(6) C4 .054(5) .072(5) .046(5) .018(4) .004(4) -.015(4) C5 .065(5) .047(4) .055(5) -.006(4) .011(4) -.010(4) C6 .082(7) .087(7) .073(7) -.007(6) -.007(5) -.019(6) C7 .122(11) .135(11) .053(7) .000(8) -.010(7) .013(6) C8 .072(6) .066(5) .054(5) .010(5) .019(5) .022(4) C9 .053(5) .074(5) .054(5) -.004(5) .006(4) .000(4) C10 .069(6) .069(6) .049(5) .002(5) .009(4) -.003(4) 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' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 .9187 '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 C5 Rh1 C1 96.9(4) no C5 Rh1 C8 82.3(4) no C1 Rh1 C8 38.8(4) no C5 Rh1 C4 37.8(3) no C1 Rh1 C4 82.4(4) no C8 Rh1 C4 92.5(4) no C5 Rh1 Cl1 160.8(2) no C1 Rh1 Cl1 91.8(3) no C8 Rh1 Cl1 94.1(3) no C4 Rh1 Cl1 161.3(2) no C5 Rh1 Cl2 92.9(2) no C1 Rh1 Cl2 158.1(3) no C8 Rh1 Cl2 163.0(3) no C4 Rh1 Cl2 93.7(3) no Cl1 Rh1 Cl2 85.03(8) yes C9 Rh2 C10 91.4(4) yes C9 Rh2 Cl1 90.5(3) yes C10 Rh2 Cl1 176.7(3) yes C9 Rh2 Cl2 176.8(3) yes C10 Rh2 Cl2 91.3(3) yes Cl1 Rh2 Cl2 86.71(8) yes Rh2 Cl1 Rh1 86.88(8) yes Rh2 Cl2 Rh1 86.71(7) yes C8 C1 C2 126.1(10) no C8 C1 Rh1 70.7(5) no C2 C1 Rh1 110.6(6) no C3 C2 C1 115.1(8) no C2 C3 C4 114.4(8) no C5 C4 C3 125.7(8) no C5 C4 Rh1 70.2(5) no C3 C4 Rh1 112.3(6) no C4 C5 C6 123.8(8) no C4 C5 Rh1 72.0(4) no C6 C5 Rh1 112.1(6) no C7 C6 C5 113.6(8) no C6 C7 C8 114.9(9) no C1 C8 C7 120.6(10) no C1 C8 Rh1 70.5(5) no C7 C8 Rh1 112.3(6) no O1 C9 Rh2 178.2(9) no O2 C10 Rh2 178.8(8) no 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 Rh1 C5 . 2.094(7) yes Rh1 C1 . 2.099(8) yes Rh1 C8 . 2.101(8) yes Rh1 C4 . 2.118(7) yes Rh1 Cl1 . 2.406(2) yes Rh1 Cl2 . 2.412(2) yes Rh2 C9 . 1.844(9) yes Rh2 C10 . 1.850(9) yes Rh2 Cl1 . 2.371(2) yes Rh2 Cl2 . 2.372(2) yes O2 C10 . 1.125(10) yes O1 C9 . 1.121(10) yes C1 C8 . 1.395(14) yes C1 C2 . 1.516(12) yes C2 C3 . 1.476(12) yes C3 C4 . 1.512(12) yes C4 C5 . 1.365(11) yes C5 C6 . 1.493(13) yes C6 C7 . 1.487(13) yes C7 C8 . 1.504(14) yes