#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100876.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_1100876 loop_ _publ_author_name 'Baya, M.' 'Buil, M. L.' 'Esteruelas, M. A.' 'O\~nate, E.' _journal_name_full ; Organometallics ; _publ_section_title ; Ene-type reactions between an a-alkenylphosphine and terminal alkynes promoted by osmium-cyclopentadienyl fragments ; _chemical_formula_sum 'C22 H30 Cl Os P' _chemical_formula_weight 551.08 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' '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' _symmetry_space_group_name_H-M 'P21/n' 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 12.3343(10) _cell_length_b 12.6118(10) _cell_length_c 13.4358(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.913(2) _cell_angle_gamma 90.00 _cell_volume 2078.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2872 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 20 _exptl_crystal_description 'irregular blok' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 6.342 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details ; Absorption correction performed with SADABS program. This is based on the method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33. SADABS: Area-Detector Absorption Correction. Bruker-AXS within SAINT+ package, v. 6.1 (2000). ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 24944 _diffrn_reflns_av_R_equivalents 0.0729 _diffrn_reflns_av_sigmaI/netI 0.0965 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.57 _reflns_number_total 4983 _reflns_number_gt 3232 _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^)+(0.0000P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4983 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0402 _refine_ls_wR_factor_gt 0.0365 _refine_ls_goodness_of_fit_ref 0.655 _refine_ls_restrained_S_all 0.655 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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 Os Os 0.840105(14) 0.216209(14) 0.836456(14) 0.03316(6) Uani 1 1 d . . . Cl Cl 0.88837(10) 0.40251(9) 0.83097(9) 0.0497(3) Uani 1 1 d . . . P P 0.75584(9) 0.25483(9) 0.97695(9) 0.0375(3) Uani 1 1 d . . . C1 C 0.6197(3) 0.2903(4) 0.9243(3) 0.0423(12) Uani 1 1 d . . . C2 C 0.5825(4) 0.2051(5) 0.8499(4) 0.0486(14) Uani 1 1 d . . . H2A H 0.563(3) 0.134(3) 0.894(3) 0.052(14) Uiso 1 1 d . . . H2B H 0.514(3) 0.223(3) 0.810(3) 0.048(13) Uiso 1 1 d . . . C3 C 0.6697(4) 0.1820(4) 0.7798(3) 0.0368(12) Uani 1 1 d . . . H3 H 0.671(3) 0.109(3) 0.753(3) 0.045(14) Uiso 1 1 d . . . C4 C 0.7101(3) 0.2659(4) 0.7234(3) 0.0343(12) Uani 1 1 d . . . H4 H 0.686(3) 0.326(3) 0.738(3) 0.022(12) Uiso 1 1 d . . . C5 C 0.7370(3) 0.2573(3) 0.6206(3) 0.0367(12) Uani 1 1 d . . . C6 C 0.7126(4) 0.1689(4) 0.5609(3) 0.0465(13) Uani 1 1 d . . . H6 H 0.6770 0.1117 0.5867 0.056 Uiso 1 1 calc R . . C7 C 0.7403(4) 0.1640(4) 0.4635(4) 0.0588(15) Uani 1 1 d . . . H7 H 0.7232 0.1039 0.4248 0.071 Uiso 1 1 calc R . . C8 C 0.7928(4) 0.2471(4) 0.4242(4) 0.0583(16) Uani 1 1 d . . . H8 H 0.8120 0.2434 0.3591 0.070 Uiso 1 1 calc R . . C9 C 0.8173(4) 0.3366(4) 0.4815(4) 0.0546(14) Uani 1 1 d . . . H9 H 0.8522 0.3938 0.4550 0.065 Uiso 1 1 calc R . . C10 C 0.7897(4) 0.3406(4) 0.5784(3) 0.0489(14) Uani 1 1 d . . . H10 H 0.8069 0.4009 0.6166 0.059 Uiso 1 1 calc R . . C11 C 0.5697(5) 0.3796(5) 0.9332(5) 0.0592(17) Uani 1 1 d . . . H11A H 0.598(3) 0.433(3) 0.972(3) 0.042(16) Uiso 1 1 d . . . H11B H 0.505(3) 0.397(3) 0.892(3) 0.040(13) Uiso 1 1 d . . . C12 C 0.7317(4) 0.1366(3) 1.0554(3) 0.0472(13) Uani 1 1 d . . . H12 H 0.7185 0.0781 1.0077 0.057 Uiso 1 1 calc R . . C13 C 0.6300(4) 0.1410(4) 1.1112(3) 0.0656(16) Uani 1 1 d . . . H13A H 0.6090 0.0704 1.1276 0.098 Uiso 1 1 calc R . . H13B H 0.5717 0.1741 1.0696 0.098 Uiso 1 1 calc R . . H13C H 0.6454 0.1814 1.1716 0.098 Uiso 1 1 calc R . . C14 C 0.8321(4) 0.1036(4) 1.1237(3) 0.0695(17) Uani 1 1 d . . . H14A H 0.8397 0.1484 1.1817 0.104 Uiso 1 1 calc R . . H14B H 0.8956 0.1102 1.0884 0.104 Uiso 1 1 calc R . . H14C H 0.8244 0.0312 1.1440 0.104 Uiso 1 1 calc R . . C15 C 0.8073(4) 0.3652(3) 1.0594(3) 0.0463(13) Uani 1 1 d . . . H15 H 0.7948 0.4295 1.0189 0.056 Uiso 1 1 calc R . . C16 C 0.7483(4) 0.3837(4) 1.1519(3) 0.0709(18) Uani 1 1 d . . . H16A H 0.7619 0.3252 1.1972 0.106 Uiso 1 1 calc R . . H16B H 0.6714 0.3895 1.1325 0.106 Uiso 1 1 calc R . . H16C H 0.7744 0.4480 1.1842 0.106 Uiso 1 1 calc R . . C17 C 0.9311(4) 0.3593(4) 1.0860(3) 0.0690(17) Uani 1 1 d . . . H17A H 0.9558 0.4220 1.1219 0.104 Uiso 1 1 calc R . . H17B H 0.9664 0.3541 1.0257 0.104 Uiso 1 1 calc R . . H17C H 0.9487 0.2980 1.1269 0.104 Uiso 1 1 calc R . . C18 C 0.9057(4) 0.0602(4) 0.8757(4) 0.0532(14) Uani 1 1 d . . . H18 H 0.8716 0.0161 0.9184 0.064 Uiso 1 1 calc R . . C19 C 0.9898(4) 0.1328(4) 0.9042(4) 0.0484(14) Uani 1 1 d . . . H19 H 1.0214 0.1458 0.9688 0.058 Uiso 1 1 calc R . . C20 C 1.0173(4) 0.1823(4) 0.8151(4) 0.0524(14) Uani 1 1 d . . . H20 H 1.0711 0.2335 0.8122 0.063 Uiso 1 1 calc R . . C21 C 0.9512(4) 0.1424(4) 0.7325(4) 0.0472(13) Uani 1 1 d . . . H21 H 0.9524 0.1620 0.6659 0.057 Uiso 1 1 calc R . . C22 C 0.8824(4) 0.0664(4) 0.7711(4) 0.0538(15) Uani 1 1 d . . . H22 H 0.8298 0.0266 0.7331 0.065 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 Os 0.03366(10) 0.03158(10) 0.03445(10) -0.00006(11) 0.00445(7) 0.00095(11) Cl 0.0605(9) 0.0351(7) 0.0533(9) 0.0003(6) 0.0042(7) -0.0115(6) P 0.0422(8) 0.0361(8) 0.0346(7) -0.0007(6) 0.0059(6) 0.0007(6) C1 0.039(3) 0.047(3) 0.042(3) 0.001(3) 0.010(2) 0.002(3) C2 0.039(3) 0.061(4) 0.046(3) -0.001(3) 0.003(3) -0.007(3) C3 0.032(3) 0.042(3) 0.036(3) -0.002(2) 0.002(2) 0.000(2) C4 0.029(3) 0.033(3) 0.040(3) -0.008(2) 0.000(2) 0.004(2) C5 0.028(3) 0.040(3) 0.040(3) 0.009(2) -0.005(2) 0.001(2) C6 0.050(3) 0.047(3) 0.042(3) 0.002(3) 0.005(3) -0.005(3) C7 0.083(4) 0.060(4) 0.034(3) -0.004(3) 0.006(3) 0.009(3) C8 0.072(4) 0.064(4) 0.041(3) 0.014(3) 0.014(3) 0.020(3) C9 0.059(4) 0.058(4) 0.047(4) 0.018(3) 0.003(3) -0.004(3) C10 0.058(4) 0.052(3) 0.037(3) 0.009(3) 0.007(3) 0.001(3) C11 0.047(4) 0.068(5) 0.062(5) -0.005(4) 0.001(3) 0.015(4) C12 0.062(4) 0.034(3) 0.048(3) 0.004(2) 0.015(3) 0.004(3) C13 0.081(4) 0.065(4) 0.057(4) 0.004(3) 0.032(3) 0.000(3) C14 0.093(5) 0.067(4) 0.050(4) 0.020(3) 0.015(3) 0.023(3) C15 0.064(4) 0.041(3) 0.034(3) -0.009(2) 0.007(3) 0.000(3) C16 0.114(5) 0.061(4) 0.040(4) -0.016(3) 0.022(3) -0.009(3) C17 0.060(4) 0.090(4) 0.053(4) -0.011(3) -0.016(3) -0.020(3) C18 0.061(4) 0.045(3) 0.057(4) -0.002(3) 0.023(3) 0.008(3) C19 0.045(3) 0.054(4) 0.047(4) -0.004(3) 0.003(3) 0.017(3) C20 0.031(3) 0.059(4) 0.069(4) -0.005(3) 0.014(3) 0.011(3) C21 0.041(3) 0.059(4) 0.043(3) 0.000(3) 0.006(3) 0.013(3) C22 0.054(4) 0.035(3) 0.072(4) -0.010(3) 0.005(3) -0.001(3)