#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100807.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100807 _publ_section_title ; Binding of organometallic ruthenium(II) and osmium(II) complexes to an oligonucleotide: a combined mass spectometric and theoretical study. ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M P2(1)/n loop_ _publ_author_name 'Dorcier, Antoine' 'Dyson, Paul J.' 'Gossens, Christian' 'Rothlisberger, Ursula' 'Scopelliti, Rosario' _chemical_formula_moiety 'C16 H26 Cl2 N3 Os P, 2(C H Cl3)' _chemical_formula_sum 'C18 H28 Cl8 N3 Os P' _chemical_formula_weight 791.20 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' 'P' 'P' 0.1023 0.0942 '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' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic 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' _cell_length_a 10.579(2) _cell_length_b 12.7402(9) _cell_length_c 20.977(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.171(16) _cell_angle_gamma 90.00 _cell_volume 2773.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 4157 _cell_measurement_theta_min 1.86985 _cell_measurement_theta_max 25.64935 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 5.439 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_absorpt_correction_T_min 0.306 _exptl_absorpt_correction_T_max 0.744 _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'marresearch mar345 IPDS' _diffrn_measurement_method '60 images with deltaphi = 3 deg. and exp. time = 180 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16359 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4836 _reflns_number_gt 4353 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+10.5637P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4836 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.28369(2) 0.436995(18) 0.207975(11) 0.02626(14) Uani 1 1 d . . . Cl1 Cl 0.44239(14) 0.31660(12) 0.26770(7) 0.0324(3) Uani 1 1 d . . . Cl2 Cl 0.12769(15) 0.29913(12) 0.21101(7) 0.0331(3) Uani 1 1 d . . . P1 P 0.25893(15) 0.47990(13) 0.31296(7) 0.0273(3) Uani 1 1 d . . . N1 N 0.1479(6) 0.5926(5) 0.3990(3) 0.0377(13) Uani 1 1 d . . . N2 N 0.2233(5) 0.4151(4) 0.4338(3) 0.0318(11) Uani 1 1 d . . . N3 N 0.3799(6) 0.5575(4) 0.4320(3) 0.0334(12) Uani 1 1 d . . . C1 C 0.1381(7) 0.5761(5) 0.3291(3) 0.0324(14) Uani 1 1 d . . . H1A H 0.1514 0.6437 0.3081 0.039 Uiso 1 1 calc R . . H1B H 0.0506 0.5504 0.3100 0.039 Uiso 1 1 calc R . . C2 C 0.2238(6) 0.3743(5) 0.3679(3) 0.0324(13) Uani 1 1 d . . . H2A H 0.1388 0.3429 0.3499 0.039 Uiso 1 1 calc R . . H2B H 0.2897 0.3184 0.3705 0.039 Uiso 1 1 calc R . . C3 C 0.4027(6) 0.5359(6) 0.3656(3) 0.0331(13) Uani 1 1 d . . . H3A H 0.4755 0.4862 0.3684 0.040 Uiso 1 1 calc R . . H3B H 0.4268 0.6020 0.3462 0.040 Uiso 1 1 calc R . . C4 C 0.1228(7) 0.4960(6) 0.4330(3) 0.0387(15) Uani 1 1 d . . . H4A H 0.0386 0.4668 0.4116 0.046 Uiso 1 1 calc R . . H4B H 0.1172 0.5136 0.4783 0.046 Uiso 1 1 calc R . . C5 C 0.3476(7) 0.4605(6) 0.4635(3) 0.0368(14) Uani 1 1 d . . . H5A H 0.4159 0.4079 0.4622 0.044 Uiso 1 1 calc R . . H5B H 0.3471 0.4758 0.5098 0.044 Uiso 1 1 calc R . . C6 C 0.2751(7) 0.6338(6) 0.4295(3) 0.0394(16) Uani 1 1 d . . . H6A H 0.2942 0.6963 0.4049 0.047 Uiso 1 1 calc R . . H6B H 0.2722 0.6566 0.4743 0.047 Uiso 1 1 calc R . . C7 C 0.4362(7) 0.4998(5) 0.1585(3) 0.0347(14) Uani 1 1 d . . . C8 C 0.3575(7) 0.4295(5) 0.1143(3) 0.0344(15) Uani 1 1 d . . . H8 H 0.3965 0.3744 0.0945 0.041 Uiso 1 1 calc R . . C9 C 0.2233(7) 0.4416(5) 0.1002(3) 0.0302(14) Uani 1 1 d . . . H9 H 0.1728 0.3937 0.0712 0.036 Uiso 1 1 calc R . . C10 C 0.1596(6) 0.5248(5) 0.1287(3) 0.0308(13) Uani 1 1 d . . . C11 C 0.2395(6) 0.5954(5) 0.1721(3) 0.0298(13) Uani 1 1 d . . . H11 H 0.2012 0.6505 0.1922 0.036 Uiso 1 1 calc R . . C12 C 0.3762(7) 0.5837(5) 0.1852(3) 0.0312(13) Uani 1 1 d . . . H12 H 0.4279 0.6333 0.2124 0.037 Uiso 1 1 calc R . . C13 C 0.5783(7) 0.4850(6) 0.1757(4) 0.0452(17) Uani 1 1 d . . . H13A H 0.6186 0.5165 0.1419 0.068 Uiso 1 1 calc R . . H13B H 0.5982 0.4098 0.1789 0.068 Uiso 1 1 calc R . . H13C H 0.6118 0.5189 0.2175 0.068 Uiso 1 1 calc R . . C14 C 0.0144(7) 0.5378(6) 0.1097(3) 0.0371(15) Uani 1 1 d . . . H14 H -0.0208 0.4740 0.0846 0.045 Uiso 1 1 calc R . . C15 C -0.0128(8) 0.6334(7) 0.0636(4) 0.0495(19) Uani 1 1 d . . . H15A H 0.0123 0.6980 0.0882 0.074 Uiso 1 1 calc R . . H15B H -0.1049 0.6360 0.0444 0.074 Uiso 1 1 calc R . . H15C H 0.0369 0.6267 0.0289 0.074 Uiso 1 1 calc R . . C16 C -0.0543(7) 0.5492(6) 0.1668(4) 0.0396(16) Uani 1 1 d . . . H16A H -0.0318 0.4899 0.1966 0.059 Uiso 1 1 calc R . . H16B H -0.1476 0.5503 0.1508 0.059 Uiso 1 1 calc R . . H16C H -0.0275 0.6149 0.1899 0.059 Uiso 1 1 calc R . . Cl3 Cl 0.07819(17) 0.29167(14) 0.57101(8) 0.0412(4) Uani 1 1 d . . . Cl4 Cl 0.34964(19) 0.23377(17) 0.59780(10) 0.0520(5) Uani 1 1 d . . . Cl5 Cl 0.1648(2) 0.10681(18) 0.51076(11) 0.0618(6) Uani 1 1 d . . . C17 C 0.2051(7) 0.2366(6) 0.5391(3) 0.0407(16) Uani 1 1 d . . . H17 H 0.2192 0.2805 0.5016 0.049 Uiso 1 1 calc R . . Cl6 Cl 0.7593(2) 0.4619(2) 0.36050(12) 0.0671(6) Uani 1 1 d . . . Cl7 Cl 0.8508(3) 0.3112(2) 0.27763(11) 0.0705(7) Uani 1 1 d . . . Cl8 Cl 0.8521(3) 0.2586(2) 0.41131(11) 0.0699(6) Uani 1 1 d . . . C18 C 0.7700(7) 0.3278(7) 0.3421(4) 0.0516(19) Uani 1 1 d . . . H18 H 0.6809 0.2986 0.3292 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.02813(18) 0.0254(2) 0.02553(18) -0.00013(8) 0.00601(11) -0.00019(8) Cl1 0.0307(7) 0.0292(8) 0.0367(8) 0.0015(6) 0.0051(6) 0.0017(6) Cl2 0.0327(8) 0.0313(8) 0.0348(8) 0.0007(6) 0.0054(6) -0.0040(6) P1 0.0280(8) 0.0283(8) 0.0260(7) 0.0006(6) 0.0060(6) -0.0005(6) N1 0.038(3) 0.043(3) 0.036(3) 0.003(3) 0.014(2) 0.006(3) N2 0.033(3) 0.037(3) 0.026(3) 0.003(2) 0.008(2) 0.000(2) N3 0.033(3) 0.040(3) 0.027(3) -0.003(2) 0.005(2) -0.006(2) C1 0.036(4) 0.032(3) 0.031(3) 0.001(2) 0.011(3) 0.008(3) C2 0.036(3) 0.029(3) 0.034(3) -0.001(3) 0.013(3) 0.003(3) C3 0.027(3) 0.040(4) 0.033(3) -0.001(3) 0.009(3) -0.005(3) C4 0.032(3) 0.050(4) 0.034(3) 0.004(3) 0.008(3) 0.001(3) C5 0.037(4) 0.044(4) 0.030(3) 0.001(3) 0.007(3) 0.005(3) C6 0.054(4) 0.037(4) 0.029(3) -0.006(3) 0.014(3) 0.002(3) C7 0.039(4) 0.034(3) 0.034(3) 0.007(3) 0.016(3) -0.006(3) C8 0.044(4) 0.041(4) 0.021(3) 0.001(2) 0.014(3) 0.006(3) C9 0.046(4) 0.030(3) 0.015(3) -0.002(2) 0.006(3) 0.000(3) C10 0.035(3) 0.027(3) 0.029(3) 0.006(2) 0.003(3) -0.003(3) C11 0.037(3) 0.024(3) 0.029(3) 0.006(2) 0.010(3) 0.001(3) C12 0.038(4) 0.025(3) 0.032(3) 0.006(2) 0.009(3) -0.001(3) C13 0.037(4) 0.049(5) 0.053(4) 0.008(3) 0.017(3) 0.000(3) C14 0.034(4) 0.040(4) 0.035(3) -0.004(3) 0.002(3) 0.001(3) C15 0.041(4) 0.065(5) 0.039(4) 0.011(4) -0.001(3) 0.007(4) C16 0.034(4) 0.040(4) 0.045(4) 0.003(3) 0.009(3) 0.002(3) Cl3 0.0423(9) 0.0403(9) 0.0438(9) -0.0009(7) 0.0156(7) 0.0025(7) Cl4 0.0426(10) 0.0566(11) 0.0545(11) -0.0003(9) 0.0037(8) 0.0061(8) Cl5 0.0750(15) 0.0509(12) 0.0596(12) -0.0202(10) 0.0132(11) 0.0030(10) C17 0.046(4) 0.043(4) 0.036(4) 0.004(3) 0.015(3) 0.009(3) Cl6 0.0482(12) 0.0822(15) 0.0673(14) -0.0220(12) 0.0025(10) 0.0068(11) Cl7 0.0766(15) 0.0914(18) 0.0500(12) 0.0082(11) 0.0283(11) 0.0312(13) Cl8 0.0736(15) 0.0850(17) 0.0503(12) 0.0045(11) 0.0094(11) -0.0106(12) C18 0.034(4) 0.073(6) 0.049(4) -0.014(4) 0.009(3) -0.001(4)