#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2210526.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_2210526 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Li Ma' 'Wen-Jie Zhao' 'Kui Lu' _publ_section_title ; Aquadichloro(\h~5~-pentamethylcyclopentadienyl)iridium(III) ; _journal_coeditor_code BV2032 _journal_issue 10 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m2524 _journal_page_last m2525 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac '[Ir (C10 H15) Cl2 (H2 O)]' _chemical_formula_moiety 'C10 H17 Cl2 Ir O' _chemical_formula_sum 'C10 H17 Cl2 Ir O' _chemical_formula_weight 416.34 _chemical_name_systematic ; Aquadichloro(\h~5~-pentamethylcyclopentadienyl)iridium(III) ; _symmetry_cell_setting Monoclinic _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 101.662(8) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.723(5) _cell_length_b 7.853(5) _cell_length_c 19.591(12) _cell_measurement_reflns_used 924 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.095 _cell_measurement_theta_min 2.802 _cell_volume 1314.3(14) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT-Plus (Bruker, 1998)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 5235 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.12 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 10.534 _exptl_absorpt_correction_T_max 0.4189 _exptl_absorpt_correction_T_min 0.3646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 1998)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.104 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 784 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.365 _refine_diff_density_min -1.423 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.258 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 132 _refine_ls_number_reflns 2303 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.258 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0371 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(13.7468P)^2^+14.5636P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.0834 _reflns_number_gt 2095 _reflns_number_total 2303 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bv2032.cif 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_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_type_symbol _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 Ir Ir1 0.20461(4) 0.05916(4) 0.399382(18) 0.03113(13) Uani d . 1 Cl Cl4 0.3950(3) -0.1625(3) 0.39442(15) 0.0517(7) Uani d . 1 Cl Cl5 0.0117(3) -0.1604(3) 0.40498(14) 0.0474(6) Uani d . 1 O O1 0.2651(10) 0.0112(11) 0.5099(4) 0.068(2) Uani d . 1 H H1A 0.1935 -0.0375 0.4805 0.081 Uiso d R 1 H H1B 0.3391 0.0666 0.5352 0.081 Uiso d R 1 C C3 0.2144(12) 0.3282(11) 0.4063(5) 0.035(2) Uani d . 1 C C4 0.2611(16) 0.4270(15) 0.4729(6) 0.060(3) Uani d . 1 H H4A 0.2688 0.5457 0.4624 0.090 Uiso calc R 1 H H4B 0.3606 0.3869 0.4980 0.090 Uiso calc R 1 H H4C 0.1837 0.4117 0.5010 0.090 Uiso calc R 1 C C5 0.0648(12) 0.1908(12) 0.3109(4) 0.037(2) Uani d . 1 C C6 0.0592(12) 0.2786(11) 0.3769(5) 0.036(2) Uani d . 1 C C7 0.3158(12) 0.2720(13) 0.3636(5) 0.040(2) Uani d . 1 C C8 0.2224(13) 0.1879(13) 0.3039(5) 0.040(2) Uani d . 1 C C9 -0.0730(15) 0.1203(15) 0.2619(6) 0.062(3) Uani d . 1 H H9A -0.1244 0.2099 0.2326 0.093 Uiso calc R 1 H H9B -0.1446 0.0718 0.2879 0.093 Uiso calc R 1 H H9C -0.0392 0.0338 0.2337 0.093 Uiso calc R 1 C C10 0.4871(14) 0.312(2) 0.3723(7) 0.075(4) Uani d . 1 H H10A 0.4996 0.4174 0.3489 0.113 Uiso calc R 1 H H10B 0.5385 0.2223 0.3526 0.113 Uiso calc R 1 H H10C 0.5325 0.3233 0.4210 0.113 Uiso calc R 1 C C11 0.2847(17) 0.1157(18) 0.2445(6) 0.069(4) Uani d . 1 H H11A 0.2037 0.0523 0.2147 0.103 Uiso calc R 1 H H11B 0.3711 0.0415 0.2622 0.103 Uiso calc R 1 H H11C 0.3193 0.2066 0.2186 0.103 Uiso calc R 1 C C12 -0.0845(15) 0.3186(17) 0.4029(6) 0.062(3) Uani d . 1 H H12A -0.0647 0.3044 0.4526 0.093 Uiso calc R 1 H H12B -0.1670 0.2431 0.3817 0.093 Uiso calc R 1 H H12C -0.1150 0.4341 0.3913 0.093 Uiso calc R 1 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 Ir1 0.0359(2) 0.02371(19) 0.0320(2) 0.00030(18) 0.00266(14) 0.00026(17) Cl4 0.0477(15) 0.0376(15) 0.0672(18) 0.0110(12) 0.0054(13) -0.0030(13) Cl5 0.0493(15) 0.0388(15) 0.0536(15) -0.0092(12) 0.0088(12) 0.0012(12) O1 0.078(6) 0.065(6) 0.051(5) -0.012(5) -0.009(4) 0.009(4) C3 0.046(6) 0.022(4) 0.034(5) 0.002(4) 0.003(4) 0.010(4) C4 0.086(9) 0.034(6) 0.056(7) 0.007(6) 0.004(6) -0.012(6) C5 0.053(6) 0.026(5) 0.027(4) 0.001(4) -0.003(4) 0.010(4) C6 0.043(6) 0.019(5) 0.044(5) 0.005(4) 0.006(4) 0.011(4) C7 0.046(6) 0.034(6) 0.040(5) -0.003(5) 0.007(5) 0.009(5) C8 0.058(7) 0.034(5) 0.033(5) 0.009(5) 0.015(5) 0.008(4) C9 0.069(8) 0.048(7) 0.056(7) -0.007(6) -0.018(6) 0.003(6) C10 0.049(7) 0.097(11) 0.077(9) -0.007(8) 0.006(7) 0.036(9) C11 0.096(10) 0.069(9) 0.047(7) 0.018(8) 0.028(7) 0.004(6) C12 0.075(9) 0.055(8) 0.060(7) 0.028(7) 0.021(6) 0.024(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ir1 C3 2.118(9) ? Ir1 C7 2.122(10) ? Ir1 C6 2.132(9) ? Ir1 O1 2.156(8) y Ir1 C8 2.159(9) ? Ir1 C5 2.169(9) ? Ir1 Cl4 2.421(3) y Ir1 Cl5 2.428(3) y Ir1 H1A 1.7822 ? O1 H1A 0.8501 ? O1 H1B 0.8500 ? C3 C7 1.407(14) ? C3 C6 1.414(14) ? C3 C4 1.502(14) ? C4 H4A 0.9600 ? C4 H4B 0.9600 ? C4 H4C 0.9600 ? C5 C8 1.409(14) ? C5 C6 1.474(13) ? C5 C9 1.486(14) ? C6 C12 1.479(15) ? C7 C8 1.442(14) ? C7 C10 1.503(15) ? C8 C11 1.492(14) ? C9 H9A 0.9600 ? C9 H9B 0.9600 ? C9 H9C 0.9600 ? C10 H10A 0.9600 ? C10 H10B 0.9600 ? C10 H10C 0.9600 ? C11 H11A 0.9600 ? C11 H11B 0.9600 ? C11 H11C 0.9600 ? C12 H12A 0.9600 ? C12 H12B 0.9600 ? C12 H12C 0.9600 ? 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 Ir1 C7 38.8(4) ? C3 Ir1 C6 38.9(4) ? C7 Ir1 C6 65.6(4) ? C3 Ir1 O1 96.4(3) ? C7 Ir1 O1 115.7(4) ? C6 Ir1 O1 111.3(4) ? C3 Ir1 C8 65.1(4) ? C7 Ir1 C8 39.4(4) ? C6 Ir1 C8 65.6(4) ? O1 Ir1 C8 155.0(4) ? C3 Ir1 C5 65.5(4) ? C7 Ir1 C5 65.2(4) ? C6 Ir1 C5 40.1(4) ? O1 Ir1 C5 150.4(4) ? C8 Ir1 C5 38.0(4) ? C3 Ir1 Cl4 134.5(3) ? C7 Ir1 Cl4 100.9(3) ? C6 Ir1 Cl4 163.1(3) ? O1 Ir1 Cl4 83.3(3) y C8 Ir1 Cl4 97.6(3) ? C5 Ir1 Cl4 126.2(3) ? C3 Ir1 Cl5 136.5(3) ? C7 Ir1 Cl5 160.4(3) ? C6 Ir1 Cl5 101.2(3) ? O1 Ir1 Cl5 82.0(2) y C8 Ir1 Cl5 122.9(3) ? C5 Ir1 Cl5 95.3(3) ? Cl4 Ir1 Cl5 88.76(10) y C3 Ir1 H1A 112.1 ? C7 Ir1 H1A 137.9 ? C6 Ir1 H1A 113.0 ? O1 Ir1 H1A 22.5 ? C8 Ir1 H1A 177.1 ? C5 Ir1 H1A 142.4 ? Cl4 Ir1 H1A 83.8 ? Cl5 Ir1 H1A 59.6 ? Ir1 O1 H1A 53.2 ? Ir1 O1 H1B 120.0 ? H1A O1 H1B 173.2 ? C7 C3 C6 109.6(9) ? C7 C3 C4 125.9(10) ? C6 C3 C4 124.5(10) ? C7 C3 Ir1 70.8(6) ? C6 C3 Ir1 71.1(5) ? C4 C3 Ir1 124.9(7) ? C3 C4 H4A 109.5 ? C3 C4 H4B 109.5 ? H4A C4 H4B 109.5 ? C3 C4 H4C 109.5 ? H4A C4 H4C 109.5 ? H4B C4 H4C 109.5 ? C8 C5 C6 107.4(8) ? C8 C5 C9 127.5(10) ? C6 C5 C9 125.1(10) ? C8 C5 Ir1 70.6(5) ? C6 C5 Ir1 68.6(5) ? C9 C5 Ir1 126.1(7) ? C3 C6 C5 106.7(9) ? C3 C6 C12 127.5(10) ? C5 C6 C12 125.6(10) ? C3 C6 Ir1 70.0(5) ? C5 C6 Ir1 71.3(5) ? C12 C6 Ir1 127.6(7) ? C3 C7 C8 107.8(9) ? C3 C7 C10 126.6(10) ? C8 C7 C10 125.1(10) ? C3 C7 Ir1 70.5(5) ? C8 C7 Ir1 71.7(6) ? C10 C7 Ir1 129.7(8) ? C5 C8 C7 108.4(8) ? C5 C8 C11 126.8(10) ? C7 C8 C11 124.8(11) ? C5 C8 Ir1 71.4(5) ? C7 C8 Ir1 68.9(5) ? C11 C8 Ir1 126.8(8) ? C5 C9 H9A 109.5 ? C5 C9 H9B 109.5 ? H9A C9 H9B 109.5 ? C5 C9 H9C 109.5 ? H9A C9 H9C 109.5 ? H9B C9 H9C 109.5 ? C7 C10 H10A 109.5 ? C7 C10 H10B 109.5 ? H10A C10 H10B 109.5 ? C7 C10 H10C 109.5 ? H10A C10 H10C 109.5 ? H10B C10 H10C 109.5 ? C8 C11 H11A 109.5 ? C8 C11 H11B 109.5 ? H11A C11 H11B 109.5 ? C8 C11 H11C 109.5 ? H11A C11 H11C 109.5 ? H11B C11 H11C 109.5 ? C6 C12 H12A 109.5 ? C6 C12 H12B 109.5 ? H12A C12 H12B 109.5 ? C6 C12 H12C 109.5 ? H12A C12 H12C 109.5 ? H12B C12 H12C 109.5 ? 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 O1 H1A Cl5 . 0.85 2.17 3.015(9) 179.5 O1 H1B Cl4 3_656 0.85 2.56 3.387(9) 164.4 _cod_database_code 2210526