#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008480.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_2008480 loop_ _publ_author_name 'Lee, S. W.' 'Lee, J.-G.' _publ_section_title ; Dichloro(2,6-diisopropylaniline-N)(\h^5^-pentamethylcyclopentadienyl)rhodium(III) ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 722 _journal_page_last 724 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '[Rh Cl2 (C10 H15) (C12 H19 N)]' _chemical_formula_moiety 'C10 H15 Rh Cl2 C12 H19 N' _chemical_formula_sum 'C22 H34 Cl2 N Rh' _chemical_formula_weight 486.31 _chemical_name_systematic ' Dichloro(pentamethylcyclopentadienyl)(2,6-diisopropylaniline)rhodium(III)' _space_group_IT_number 33 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.5557(13) _cell_length_b 9.8241(9) _cell_length_c 17.604(2) _cell_measurement_reflns_used 58 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 25.70 _cell_measurement_theta_min 2.34 _cell_volume 2344.4(4) _computing_cell_refinement XSCANS _computing_data_collection 'XSCANS (Siemens, 1995)' _computing_data_reduction 'SHELXTL (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution SHELXTL _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 3063 _diffrn_reflns_theta_max 25.0 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.962 _exptl_absorpt_correction_T_max 0.794 _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour orange-red _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1008 _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.24 _refine_diff_density_max 0.205 _refine_diff_density_min -0.455 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 244 _refine_ls_number_reflns 2265 _refine_ls_R_factor_gt 0.0232 _refine_ls_shift/su_max 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0364P)^2^+0.2111P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0611 _reflns_number_gt 2277 _reflns_number_total 2783 _reflns_threshold_expression F>4\s(F) _[local]_cod_data_source_file na1385.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'Pna21 ' _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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2008480 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' 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 Rh 0.02493(14) 0.03222(14) 0.0507(2) 0.00077(8) -0.0005(4) 0.0007(5) Cl1 0.0534(15) 0.0510(14) 0.0527(14) 0.0040(12) 0.0063(13) -0.0117(13) Cl2 0.0440(12) 0.0382(11) 0.0560(14) -0.0022(10) -0.0071(12) 0.0090(11) N1 0.0296(10) 0.0312(11) 0.0418(13) 0.0012(9) 0.000(5) 0.004(5) C1 0.0237(13) 0.049(2) 0.059(3) 0.0044(13) 0.000(4) 0.016(5) C2 0.031(5) 0.059(5) 0.072(8) -0.011(4) -0.015(5) 0.002(6) C3 0.024(4) 0.028(4) 0.130(9) -0.004(3) -0.010(4) -0.001(4) C4 0.028(4) 0.082(8) 0.105(9) -0.003(5) 0.013(5) 0.033(6) C5 0.030(5) 0.050(5) 0.073(8) 0.018(4) 0.012(5) 0.020(5) C6 0.039(2) 0.046(2) 0.083(3) 0.0081(15) 0.020(6) 0.004(7) C7 0.064(7) 0.120(11) 0.049(5) 0.005(6) -0.036(5) -0.008(6) C8 0.044(6) 0.066(6) 0.202(17) 0.004(5) -0.043(9) -0.060(9) C9 0.052(7) 0.060(6) 0.179(14) -0.009(4) 0.020(9) 0.043(8) C10 0.053(7) 0.094(9) 0.115(10) 0.023(6) 0.019(7) 0.040(8) C11 0.0276(13) 0.0306(14) 0.046(2) 0.0020(11) -0.006(4) -0.018(5) C12 0.034(4) 0.033(4) 0.057(5) -0.007(3) 0.000(3) 0.021(4) C13 0.047(5) 0.017(3) 0.066(5) 0.003(3) -0.004(4) 0.020(3) C14 0.058(2) 0.0273(15) 0.080(3) 0.0073(14) 0.000(9) 0.015(7) C15 0.055(6) 0.070(6) 0.065(6) 0.004(4) 0.002(5) -0.002(5) C16 0.035(4) 0.042(4) 0.032(3) 0.011(3) 0.003(3) 0.010(3) C17 0.046(5) 0.039(4) 0.055(5) 0.005(4) 0.004(4) 0.013(4) C18 0.062(7) 0.092(8) 0.063(7) 0.005(6) -0.025(5) 0.025(6) C19 0.065(5) 0.109(8) 0.056(5) 0.002(5) 0.017(4) -0.027(5) C20 0.070(6) 0.066(6) 0.033(5) -0.010(5) -0.003(4) 0.020(4) C21 0.128(8) 0.076(6) 0.048(5) 0.008(6) -0.013(5) -0.001(5) C22 0.086(9) 0.067(6) 0.070(8) 0.003(6) 0.007(6) 0.003(6) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Rh 0.126842(14) 0.11939(2) 0.8454(2) 0.03595(10) Uani d . 1 Rh Cl1 0.0217(2) 0.2063(3) 0.94531(7) 0.0524(6) Uani d . 1 Cl Cl2 0.0207(2) 0.2070(2) 0.74635(7) 0.0461(6) Uani d . 1 Cl N1 0.0133(2) -0.0426(2) 0.8461(8) 0.0342(5) Uani d . 1 N H1A -0.0250(2) -0.0227(2) 0.8864(8) 0.041 Uiso calc R 1 H H1B -0.0240(2) -0.0251(2) 0.8050(8) 0.041 Uiso calc R 1 H C1 0.2614(2) 0.0034(4) 0.8494(9) 0.0439(12) Uani d . 1 C C2 0.2592(8) 0.0863(12) 0.9094(8) 0.054(3) Uani d . 1 C C3 0.2543(7) 0.2312(9) 0.8825(8) 0.061(3) Uani d . 1 C C4 0.2541(8) 0.2215(12) 0.8012(8) 0.072(4) Uani d . 1 C C5 0.2563(8) 0.0887(11) 0.7779(7) 0.051(3) Uani d . 1 C C6 0.2683(3) -0.1487(4) 0.8426(10) 0.0560(11) Uani d . 1 C H6A 0.3326(8) -0.1782(5) 0.8585(18) 0.084 Uiso calc R 1 H H6B 0.258(2) -0.1749(4) 0.7907(10) 0.084 Uiso calc R 1 H H6C 0.2191(15) -0.1902(4) 0.8742(17) 0.084 Uiso calc R 1 H C7 0.2666(9) 0.0419(14) 0.9923(6) 0.078(4) Uani d . 1 C H7A 0.239(3) -0.048(2) 0.9979(8) 0.116 Uiso calc R 1 H H7B 0.231(3) 0.105(3) 1.0237(7) 0.116 Uiso calc R 1 H H7C 0.3346(9) 0.041(5) 1.0076(10) 0.116 Uiso calc R 1 H C8 0.2534(10) 0.3425(15) 0.9405(13) 0.104(6) Uani d . 1 C H8A 0.226(5) 0.309(2) 0.9872(15) 0.156 Uiso calc R 1 H H8B 0.214(4) 0.417(3) 0.9225(19) 0.156 Uiso calc R 1 H H8C 0.3196(11) 0.374(5) 0.949(3) 0.156 Uiso calc R 1 H C9 0.2503(11) 0.3558(14) 0.7574(13) 0.097(5) Uani d . 1 C H9A 0.312(2) 0.369(3) 0.731(3) 0.146 Uiso calc R 1 H H9B 0.240(4) 0.4295(15) 0.7923(13) 0.146 Uiso calc R 1 H H9C 0.197(3) 0.353(3) 0.721(3) 0.146 Uiso calc R 1 H C10 0.2644(9) 0.0444(13) 0.7005(9) 0.087(5) Uani d . 1 C H10A 0.2048(17) 0.067(5) 0.6737(11) 0.131 Uiso calc R 1 H H10B 0.275(4) -0.0523(15) 0.6992(9) 0.131 Uiso calc R 1 H H10C 0.319(2) 0.089(4) 0.6767(12) 0.131 Uiso calc R 1 H C11 0.0216(2) -0.1899(3) 0.8476(8) 0.0346(9) Uani d . 1 C C12 0.0256(5) -0.2541(8) 0.9181(5) 0.041(2) Uani d . 1 C C13 0.0257(7) -0.4016(7) 0.9097(6) 0.043(2) Uani d . 1 C H13 0.0240(7) -0.4523(7) 0.9543(6) 0.052 Uiso calc R 1 H C14 0.0278(3) -0.4697(3) 0.8464(11) 0.0552(11) Uani d . 1 C H14 0.0266(3) -0.5643(3) 0.8473(11) 0.066 Uiso calc R 1 H C15 0.0321(9) -0.3981(12) 0.7741(8) 0.063(3) Uani d . 1 C H15 0.0381(9) -0.4438(12) 0.7281(8) 0.076 Uiso calc R 1 H C16 0.0268(5) -0.2596(9) 0.7781(4) 0.036(2) Uani d . 1 C C17 0.0264(6) -0.1788(9) 0.7001(6) 0.047(2) Uani d . 1 C H17 0.0551(6) -0.0883(9) 0.7078(6) 0.056 Uiso calc R 1 H C18 -0.0824(9) -0.1636(14) 0.6724(7) 0.072(4) Uani d . 1 C H18A -0.0835(10) -0.115(7) 0.625(2) 0.109 Uiso calc R 1 H H18B -0.1197(15) -0.114(6) 0.7096(19) 0.109 Uiso calc R 1 H H18C -0.111(2) -0.2522(14) 0.665(4) 0.109 Uiso calc R 1 H C19 0.0858(8) -0.2556(14) 0.6369(6) 0.076(3) Uani d . 1 C H19A 0.055(2) -0.342(2) 0.627(2) 0.115 Uiso calc R 1 H H19B 0.1522(14) -0.271(5) 0.6539(14) 0.115 Uiso calc R 1 H H19C 0.087(3) -0.202(3) 0.5914(11) 0.115 Uiso calc R 1 H C20 0.0250(8) -0.1852(11) 0.9893(5) 0.056(3) Uani d . 1 C H20 0.0519(8) -0.0945(11) 0.9788(5) 0.067 Uiso calc R 1 H C21 0.0925(9) -0.2459(13) 1.0472(7) 0.084(3) Uani d . 1 C H21A 0.0577(15) -0.314(4) 1.076(2) 0.126 Uiso calc R 1 H H21B 0.115(3) -0.1759(15) 1.081(2) 0.126 Uiso calc R 1 H H21C 0.148(2) -0.286(5) 1.0222(7) 0.126 Uiso calc R 1 H C22 -0.0775(10) -0.1604(13) 1.0202(8) 0.075(4) Uani d . 1 C H22A -0.1185(17) -0.123(7) 0.9808(13) 0.112 Uiso calc R 1 H H22B -0.0741(12) -0.097(6) 1.062(3) 0.112 Uiso calc R 1 H H22C -0.105(2) -0.2448(18) 1.038(4) 0.112 Uiso calc R 1 H 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' N N 0.0061 0.0033 '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' Rh Rh -1.1178 0.9187 '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 C2 Rh C4 65.6(5) no C2 Rh C5 65.4(2) no C4 Rh C5 37.3(4) no C2 Rh C1 36.2(5) no C4 Rh C1 65.0(4) no C5 Rh C1 41.3(5) no C2 Rh C3 41.0(4) no C4 Rh C3 39.1(2) no C5 Rh C3 65.3(5) no C1 Rh C3 65.1(3) no C2 Rh N1 118.0(4) no C4 Rh N1 154.0(5) no C5 Rh N1 118.2(4) no C1 Rh N1 102.04(12) no C3 Rh N1 157.6(4) no C2 Rh Cl2 158.6(3) no C4 Rh Cl2 92.9(3) no C5 Rh Cl2 97.9(3) no C1 Rh Cl2 135.8(5) no C3 Rh Cl2 121.0(3) no N1 Rh Cl2 81.2(3) yes C2 Rh Cl1 99.5(4) no C4 Rh Cl1 125.0(4) no C5 Rh Cl1 159.4(4) no C1 Rh Cl1 131.5(5) no C3 Rh Cl1 94.1(3) no N1 Rh Cl1 80.8(3) yes Cl2 Rh Cl1 92.74(3) yes C11 N1 Rh 131.5(2) yes C2 C1 C6 132.2(14) no C2 C1 C5 108.6(4) no C6 C1 C5 119.1(14) no C2 C1 Rh 71.6(5) no C6 C1 Rh 125.2(3) no C5 C1 Rh 69.0(4) no C1 C2 C3 109.3(11) no C1 C2 C7 125.5(11) no C3 C2 C7 125.1(12) no C1 C2 Rh 72.3(6) no C3 C2 Rh 69.7(6) no C7 C2 Rh 126.9(8) no C4 C3 C2 104.6(12) no C4 C3 C8 136.9(14) no C2 C3 C8 118.5(14) no C4 C3 Rh 70.2(8) no C2 C3 Rh 69.3(5) no C8 C3 Rh 125.1(8) no C5 C4 C3 111.2(12) no C5 C4 C9 132.3(14) no C3 C4 C9 116.5(15) no C5 C4 Rh 71.3(6) no C3 C4 Rh 70.7(7) no C9 C4 Rh 124.1(8) no C4 C5 C10 125.1(11) no C4 C5 C1 106.2(11) no C10 C5 C1 128.2(10) no C4 C5 Rh 71.4(6) no C10 C5 Rh 129.2(9) no C1 C5 Rh 69.7(5) no C12 C11 C16 123.6(3) no C12 C11 N1 118.0(9) no C16 C11 N1 118.4(10) no C11 C12 C20 124.6(8) no C11 C12 C13 111.1(7) no C20 C12 C13 124.2(8) no C14 C13 C12 126.8(8) no C13 C14 C15 120.1(3) no C16 C15 C14 115.8(10) no C15 C16 C11 122.3(8) no C15 C16 C17 117.0(8) no C11 C16 C17 120.6(8) no C18 C17 C19 108.1(9) no C18 C17 C16 108.7(7) no C19 C17 C16 111.9(8) no C12 C20 C21 114.0(9) no C12 C20 C22 113.5(9) no C21 C20 C22 112.4(10) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Rh C2 2.144(11) yes Rh C4 2.142(10) yes Rh C5 2.141(11) yes Rh C1 2.152(3) yes Rh C3 2.149(9) yes Rh N1 2.214(2) yes Rh Cl2 2.419(3) yes Rh Cl1 2.420(3) yes N1 C11 1.451(4) yes C1 C2 1.33(2) no C1 C6 1.502(6) no C1 C5 1.51(2) no C2 C3 1.502(14) no C2 C7 1.53(2) no C3 C4 1.43(2) no C3 C8 1.50(2) no C4 C5 1.37(2) no C4 C9 1.53(2) no C5 C10 1.44(2) no C11 C12 1.395(15) no C11 C16 1.403(14) no C12 C20 1.424(14) no C12 C13 1.456(10) no C13 C14 1.30(2) no C14 C15 1.46(2) no C15 C16 1.364(12) no C16 C17 1.587(12) no C17 C18 1.560(13) no C17 C19 1.567(14) no C20 C21 1.494(15) no C20 C22 1.512(15) no