#------------------------------------------------------------------------------ #$Date: 2011-02-11 12:37:22 +0200 (Fri, 11 Feb 2011) $ #$Revision: 10323 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4316815.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_4316815 loop_ _publ_author_name 'Claude Berthon' 'Nathalie Boubals' 'Iraida A. Charushnikova' 'David Collison' 'St\'ephanie M. Cornet' 'Christophe Den Auwer' 'Andrew J. Gaunt' 'Nikolas Kaltsoyannis' 'Iain May' 'Sebastien Petit' 'Michael P. Redmond' 'Sean D. Reilly' 'Brian L. Scott' _publ_section_title ; The Reaction Chemistry of Plutonyl(VI) Chloride Complexes with Triphenyl Phosphineoxide and Triphenyl Phosphinimine ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 9554 _journal_page_last 9562 _journal_volume 49 _journal_year 2010 _chemical_formula_moiety 'C36 H30 Cl4 O2 P2 Pu' _chemical_formula_sum 'C36 H30 Cl4 O2 P2 Pu' _chemical_formula_weight 940.34 _chemical_name_systematic ; 'Tetrachloro-bis(triphenylphosphine oxide) plutonium(iv)' ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _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 96.330(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.9751(9) _cell_length_b 13.1612(10) _cell_length_c 20.2217(15) _cell_measurement_reflns_used 12412 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 30 _cell_measurement_theta_min 2 _cell_volume 3696.7(5) _computing_cell_refinement 'HKL package (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_data_reduction 'HKL package (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997b)' _computing_publication_material 'SHELXTL (Sheldrick, 1997b)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f- \w-scans to cover a hemisphere of the reciprocal space' _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 0.0785 _diffrn_reflns_av_sigmaI/netI 0.1152 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 10053 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.03 _exptl_absorpt_coefficient_mu 2.189 _exptl_absorpt_correction_T_max 0.803 _exptl_absorpt_correction_T_min 0.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'MULABS (Blessing, 1995)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1816 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.764 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.139 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 204 _refine_ls_number_reflns 3630 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.884 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0479 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.0801 _reflns_number_gt 2220 _reflns_number_total 3630 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ic101251a_si_001.cif _[local]_cod_data_source_block pu24 _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_database_code 4316815 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' '-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_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 Pu1 Pu 0.5000 0.86301(2) 0.7500 0.04752(15) Uani 1 2 d S . . Cl1 Cl 0.32411(12) 0.84585(13) 0.69839(10) 0.0768(6) Uani 1 1 d . . . Cl2 Cl 0.44876(13) 1.00034(14) 0.82931(11) 0.0861(6) Uani 1 1 d . . . P1 P 0.47941(11) 0.66602(13) 0.87853(9) 0.0520(5) Uani 1 1 d . . . O1 O 0.4700(3) 0.7428(3) 0.8220(2) 0.0536(11) Uani 1 1 d . . . C1 C 0.3622(4) 0.6393(4) 0.9012(3) 0.0505(16) Uani 1 1 d . . . C2 C 0.2872(5) 0.6293(4) 0.8506(4) 0.068(2) Uani 1 1 d . . . H1 H 0.2986 0.6381 0.8065 0.082 Uiso 1 1 calc R . . C3 C 0.1959(5) 0.6063(6) 0.8657(5) 0.090(3) Uani 1 1 d . . . H2 H 0.1457 0.5982 0.8319 0.108 Uiso 1 1 calc R . . C4 C 0.1796(6) 0.5954(7) 0.9304(6) 0.107(3) Uani 1 1 d . . . H3 H 0.1179 0.5804 0.9405 0.128 Uiso 1 1 calc R . . C5 C 0.2520(7) 0.6063(6) 0.9804(5) 0.108(3) Uani 1 1 d . . . H4 H 0.2397 0.5990 1.0244 0.129 Uiso 1 1 calc R . . C6 C 0.3440(5) 0.6282(5) 0.9657(4) 0.077(2) Uani 1 1 d . . . H5 H 0.3937 0.6353 1.0000 0.092 Uiso 1 1 calc R . . C7 C 0.5359(5) 0.5533(5) 0.8535(3) 0.0573(19) Uani 1 1 d . . . C8 C 0.6236(5) 0.5584(6) 0.8297(4) 0.078(2) Uani 1 1 d . . . H6 H 0.6522 0.6216 0.8259 0.094 Uiso 1 1 calc R . . C9 C 0.6715(6) 0.4723(7) 0.8112(4) 0.092(3) Uani 1 1 d . . . H7 H 0.7304 0.4776 0.7940 0.110 Uiso 1 1 calc R . . C10 C 0.6300(8) 0.3803(7) 0.8187(5) 0.110(3) Uani 1 1 d . . . H8 H 0.6621 0.3219 0.8075 0.132 Uiso 1 1 calc R . . C11 C 0.5425(8) 0.3713(6) 0.8422(5) 0.114(3) Uani 1 1 d . . . H9 H 0.5150 0.3076 0.8461 0.136 Uiso 1 1 calc R . . C12 C 0.4942(5) 0.4592(6) 0.8604(4) 0.086(3) Uani 1 1 d . . . H10 H 0.4349 0.4539 0.8769 0.104 Uiso 1 1 calc R . . C13 C 0.5493(4) 0.7141(5) 0.9497(3) 0.0535(17) Uani 1 1 d . . . C14 C 0.6134(5) 0.6536(5) 0.9896(4) 0.071(2) Uani 1 1 d . . . H11 H 0.6227 0.5864 0.9776 0.085 Uiso 1 1 calc R . . C15 C 0.6637(5) 0.6922(8) 1.0470(4) 0.090(3) Uani 1 1 d . . . H12 H 0.7063 0.6512 1.0737 0.108 Uiso 1 1 calc R . . C16 C 0.6501(6) 0.7914(9) 1.0641(4) 0.094(3) Uani 1 1 d . . . H13 H 0.6831 0.8174 1.1029 0.112 Uiso 1 1 calc R . . C17 C 0.5882(6) 0.8530(6) 1.0248(5) 0.088(2) Uani 1 1 d . . . H14 H 0.5795 0.9202 1.0369 0.105 Uiso 1 1 calc R . . C18 C 0.5386(5) 0.8149(6) 0.9670(4) 0.079(2) Uani 1 1 d . . . H15 H 0.4981 0.8571 0.9397 0.095 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 Pu1 0.0416(2) 0.0530(2) 0.0474(3) 0.000 0.00237(16) 0.000 Cl1 0.0520(10) 0.0969(14) 0.0776(15) -0.0093(12) -0.0103(9) 0.0054(9) Cl2 0.0753(13) 0.0892(13) 0.0925(18) -0.0377(12) 0.0039(12) 0.0049(10) P1 0.0471(10) 0.0627(12) 0.0465(13) 0.0043(10) 0.0058(9) -0.0016(8) O1 0.057(3) 0.065(3) 0.039(3) 0.001(2) 0.002(2) -0.003(2) C1 0.044(4) 0.055(4) 0.053(5) -0.004(4) 0.007(3) -0.006(3) C2 0.060(5) 0.076(5) 0.068(6) -0.006(4) 0.001(4) -0.018(4) C3 0.054(5) 0.092(6) 0.122(9) -0.006(6) -0.001(5) -0.021(4) C4 0.063(6) 0.120(8) 0.143(11) 0.000(8) 0.035(7) -0.024(5) C5 0.090(7) 0.136(8) 0.103(9) 0.024(6) 0.036(6) -0.007(6) C6 0.055(5) 0.105(6) 0.072(6) 0.010(5) 0.015(4) -0.003(4) C7 0.055(4) 0.056(4) 0.060(5) 0.008(4) 0.005(4) 0.005(4) C8 0.046(4) 0.095(6) 0.095(7) 0.014(5) 0.015(4) 0.001(4) C9 0.078(6) 0.106(7) 0.095(8) 0.001(6) 0.025(5) 0.025(6) C10 0.119(8) 0.092(7) 0.127(9) 0.006(6) 0.041(7) 0.031(6) C11 0.129(8) 0.071(6) 0.148(10) -0.003(6) 0.052(7) 0.009(6) C12 0.083(6) 0.085(6) 0.095(7) -0.005(5) 0.027(5) 0.003(5) C13 0.049(4) 0.072(5) 0.041(5) 0.003(4) 0.006(3) 0.000(4) C14 0.064(5) 0.093(6) 0.052(5) 0.003(5) -0.007(4) -0.010(4) C15 0.065(5) 0.135(8) 0.066(7) 0.004(6) -0.010(5) -0.014(5) C16 0.082(6) 0.149(9) 0.050(6) -0.030(7) 0.003(5) -0.035(6) C17 0.089(6) 0.106(7) 0.069(7) -0.022(6) 0.010(5) 0.001(5) C18 0.081(5) 0.105(7) 0.047(6) -0.008(5) -0.014(4) -0.002(5) 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' 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' Pu Pu -9.4100 4.3056 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pu1 O1 89.18(19) . 2_656 ? O1 Pu1 Cl2 90.34(11) . . ? O1 Pu1 Cl2 174.71(10) 2_656 . ? O1 Pu1 Cl2 174.71(10) . 2_656 ? O1 Pu1 Cl2 90.34(11) 2_656 2_656 ? Cl2 Pu1 Cl2 90.61(10) . 2_656 ? O1 Pu1 Cl1 87.85(10) . . ? O1 Pu1 Cl1 84.98(10) 2_656 . ? Cl2 Pu1 Cl1 89.74(6) . . ? Cl2 Pu1 Cl1 97.36(6) 2_656 . ? O1 Pu1 Cl1 84.98(10) . 2_656 ? O1 Pu1 Cl1 87.85(10) 2_656 2_656 ? Cl2 Pu1 Cl1 97.36(6) . 2_656 ? Cl2 Pu1 Cl1 89.74(6) 2_656 2_656 ? Cl1 Pu1 Cl1 169.93(8) . 2_656 ? O1 P1 C13 111.6(3) . . ? O1 P1 C7 110.2(3) . . ? C13 P1 C7 108.0(3) . . ? O1 P1 C1 108.6(3) . . ? C13 P1 C1 107.6(3) . . ? C7 P1 C1 110.9(3) . . ? P1 O1 Pu1 163.6(2) . . ? C6 C1 C2 119.3(6) . . ? C6 C1 P1 122.7(5) . . ? C2 C1 P1 117.9(5) . . ? C3 C2 C1 119.9(7) . . ? C3 C2 H1 120.0 . . ? C1 C2 H1 120.0 . . ? C4 C3 C2 119.6(8) . . ? C4 C3 H2 120.2 . . ? C2 C3 H2 120.2 . . ? C5 C4 C3 121.1(9) . . ? C5 C4 H3 119.5 . . ? C3 C4 H3 119.5 . . ? C4 C5 C6 119.8(9) . . ? C4 C5 H4 120.1 . . ? C6 C5 H4 120.1 . . ? C1 C6 C5 120.2(8) . . ? C1 C6 H5 119.9 . . ? C5 C6 H5 119.9 . . ? C8 C7 C12 118.9(6) . . ? C8 C7 P1 120.1(6) . . ? C12 C7 P1 120.9(6) . . ? C7 C8 C9 122.2(7) . . ? C7 C8 H6 118.9 . . ? C9 C8 H6 118.9 . . ? C10 C9 C8 118.2(8) . . ? C10 C9 H7 120.9 . . ? C8 C9 H7 120.9 . . ? C9 C10 C11 121.7(8) . . ? C9 C10 H8 119.1 . . ? C11 C10 H8 119.1 . . ? C10 C11 C12 119.6(8) . . ? C10 C11 H9 120.2 . . ? C12 C11 H9 120.2 . . ? C7 C12 C11 119.4(7) . . ? C7 C12 H10 120.3 . . ? C11 C12 H10 120.3 . . ? C18 C13 C14 118.9(7) . . ? C18 C13 P1 119.0(5) . . ? C14 C13 P1 122.1(6) . . ? C15 C14 C13 120.7(7) . . ? C15 C14 H11 119.6 . . ? C13 C14 H11 119.6 . . ? C16 C15 C14 119.3(8) . . ? C16 C15 H12 120.4 . . ? C14 C15 H12 120.4 . . ? C15 C16 C17 120.8(8) . . ? C15 C16 H13 119.6 . . ? C17 C16 H13 119.6 . . ? C16 C17 C18 120.0(8) . . ? C16 C17 H14 120.0 . . ? C18 C17 H14 120.0 . . ? C13 C18 C17 120.2(7) . . ? C13 C18 H15 119.9 . . ? C17 C18 H15 119.9 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pu1 O1 2.221(4) . ? Pu1 O1 2.221(4) 2_656 ? Pu1 Cl2 2.5700(18) . ? Pu1 Cl2 2.5700(18) 2_656 ? Pu1 Cl1 2.5723(16) . ? Pu1 Cl1 2.5723(16) 2_656 ? P1 O1 1.520(4) . ? P1 C13 1.765(7) . ? P1 C7 1.780(6) . ? P1 C1 1.784(6) . ? C1 C6 1.364(9) . ? C1 C2 1.388(8) . ? C2 C3 1.379(9) . ? C2 H1 0.9300 . ? C3 C4 1.359(11) . ? C3 H2 0.9300 . ? C4 C5 1.356(12) . ? C4 H3 0.9300 . ? C5 C6 1.381(10) . ? C5 H4 0.9300 . ? C6 H5 0.9300 . ? C7 C8 1.367(8) . ? C7 C12 1.382(8) . ? C8 C9 1.388(9) . ? C8 H6 0.9300 . ? C9 C10 1.359(10) . ? C9 H7 0.9300 . ? C10 C11 1.365(11) . ? C10 H8 0.9300 . ? C11 C12 1.408(9) . ? C11 H9 0.9300 . ? C12 H10 0.9300 . ? C13 C18 1.384(8) . ? C13 C14 1.389(8) . ? C14 C15 1.386(9) . ? C14 H11 0.9300 . ? C15 C16 1.369(10) . ? C15 H12 0.9300 . ? C16 C17 1.374(10) . ? C16 H13 0.9300 . ? C17 C18 1.385(9) . ? C17 H14 0.9300 . ? C18 H15 0.9300 . ?