#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:09:00 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180170 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/66/7106610.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_7106610
loop_
_publ_author_name
'David Schnaars'
'Enrique Batista'
'Andrew Gaunt'
'Trevor Hayton'
'Iain May'
'Sean Reilly'
'Brian Scott'
'Guang Wu'
_publ_section_title
;
 Differences in actinide metal-ligand orbital interactions: comparison of
 U(IV) and Pu(IV) B-ketoiminate N,O donor complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              7647
_journal_paper_doi               10.1039/c1cc12409a
_journal_volume                  47
_journal_year                    2011
_chemical_formula_sum            'C62 H74 I2 N2 O3 Pu'
_chemical_formula_weight         1388.09
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.2990(10)
_cell_angle_beta                 103.8160(10)
_cell_angle_gamma                93.7570(10)
_cell_formula_units_Z            1
_cell_length_a                   10.1318(10)
_cell_length_b                   11.8288(11)
_cell_length_c                   13.1117(13)
_cell_measurement_temperature    140(1)
_cell_volume                     1457.9(2)
_computing_cell_refinement       'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_data_collection       'APEX II, v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+, v. 7.66a (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.14, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      140(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω scans'
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16551
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.233
_exptl_absorpt_correction_T_max  0.8416
_exptl_absorpt_correction_T_min  0.5351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 1 (Sheldrick, 2008)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.243
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         6681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0311P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0574
_reflns_number_gt                5910
_reflns_number_total             6681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc12409a.txt
_cod_data_source_block           apx1147s
_cod_database_code               7106610
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 1.0000 1.0000 0.0000 0.01644(5) Uani 1 2 d S . .
I1 I 1.224401(17) 0.854463(16) 0.046960(16) 0.03110(6) Uani 1 1 d . . .
O1 O 1.02177(17) 1.06981(15) 0.17483(14) 0.0208(4) Uani 1 1 d . . .
N1 N 0.8543(2) 0.86893(18) 0.04655(17) 0.0180(4) Uani 1 1 d . . .
C1 C 0.7808(2) 0.7846(2) -0.0559(2) 0.0177(5) Uani 1 1 d . . .
C2 C 0.6514(3) 0.8036(2) -0.1098(2) 0.0204(5) Uani 1 1 d . . .
H2 H 0.6116 0.8674 -0.0774 0.025 Uiso 1 1 calc R . .
C3 C 0.5825(2) 0.7276(2) -0.2113(2) 0.0183(5) Uani 1 1 d . . .
C4 C 0.6451(2) 0.6317(2) -0.2560(2) 0.0187(5) Uani 1 1 d . . .
H4 H 0.5978 0.5786 -0.3231 0.022 Uiso 1 1 calc R . .
C5 C 0.7752(3) 0.6121(2) -0.2046(2) 0.0187(5) Uani 1 1 d . . .
C6 C 0.8431(2) 0.6924(2) -0.1032(2) 0.0188(5) Uani 1 1 d . . .
H6 H 0.9312 0.6835 -0.0674 0.023 Uiso 1 1 calc R . .
C7 C 0.8447(3) 0.5076(2) -0.2515(2) 0.0257(6) Uani 1 1 d . . .
C8 C 0.9836(3) 0.5535(3) -0.2645(3) 0.0365(7) Uani 1 1 d . . .
H8A H 0.9684 0.5932 -0.3205 0.055 Uiso 1 1 calc R . .
H8B H 1.0327 0.4881 -0.2848 0.055 Uiso 1 1 calc R . .
H8C H 1.0364 0.6077 -0.1962 0.055 Uiso 1 1 calc R . .
C9 C 0.7584(3) 0.4298(3) -0.3636(3) 0.0399(8) Uani 1 1 d . . .
H9A H 0.6728 0.3973 -0.3564 0.060 Uiso 1 1 calc R . .
H9B H 0.8071 0.3667 -0.3908 0.060 Uiso 1 1 calc R . .
H9C H 0.7409 0.4766 -0.4138 0.060 Uiso 1 1 calc R . .
C10 C 0.8683(3) 0.4311(3) -0.1718(3) 0.0329(7) Uani 1 1 d . . .
H10A H 0.9297 0.4766 -0.1030 0.049 Uiso 1 1 calc R . .
H10B H 0.9077 0.3628 -0.2025 0.049 Uiso 1 1 calc R . .
H10C H 0.7823 0.4063 -0.1603 0.049 Uiso 1 1 calc R . .
C11 C 0.4432(3) 0.7484(2) -0.2762(2) 0.0231(6) Uani 1 1 d . . .
C12 C 0.4561(3) 0.7600(3) -0.3868(3) 0.0363(7) Uani 1 1 d . . .
H12A H 0.4824 0.6886 -0.4268 0.054 Uiso 1 1 calc R . .
H12B H 0.5244 0.8256 -0.3751 0.054 Uiso 1 1 calc R . .
H12C H 0.3694 0.7731 -0.4280 0.054 Uiso 1 1 calc R . .
C13 C 0.3343(3) 0.6442(3) -0.2967(3) 0.0494(10) Uani 1 1 d . . .
H13A H 0.3232 0.6373 -0.2278 0.074 Uiso 1 1 calc R . .
H13B H 0.3624 0.5728 -0.3351 0.074 Uiso 1 1 calc R . .
H13C H 0.2488 0.6566 -0.3401 0.074 Uiso 1 1 calc R . .
C14 C 0.3979(4) 0.8620(3) -0.2179(3) 0.0473(9) Uani 1 1 d . . .
H14A H 0.3136 0.8743 -0.2630 0.071 Uiso 1 1 calc R . .
H14B H 0.4673 0.9274 -0.2042 0.071 Uiso 1 1 calc R . .
H14C H 0.3841 0.8560 -0.1494 0.071 Uiso 1 1 calc R . .
C15 C 0.7316(3) 0.7639(2) 0.1410(2) 0.0203(5) Uani 1 1 d . . .
C16 C 0.6145(3) 0.7851(3) 0.1751(3) 0.0346(7) Uani 1 1 d . . .
H16 H 0.5955 0.8622 0.1976 0.042 Uiso 1 1 calc R . .
C17 C 0.5253(3) 0.6917(3) 0.1759(3) 0.0461(9) Uani 1 1 d . . .
H17 H 0.4453 0.7062 0.1971 0.055 Uiso 1 1 calc R . .
C18 C 0.5546(3) 0.5772(3) 0.1454(3) 0.0425(9) Uani 1 1 d . . .
H18 H 0.4942 0.5149 0.1459 0.051 Uiso 1 1 calc R . .
C19 C 0.6723(3) 0.5554(3) 0.1145(2) 0.0352(8) Uani 1 1 d . . .
H19 H 0.6932 0.4785 0.0958 0.042 Uiso 1 1 calc R . .
C20 C 0.7604(3) 0.6485(2) 0.1111(2) 0.0268(6) Uani 1 1 d . . .
H20 H 0.8395 0.6334 0.0887 0.032 Uiso 1 1 calc R . .
C21 C 0.8278(2) 0.8646(2) 0.1392(2) 0.0161(5) Uani 1 1 d . . .
C22 C 0.8887(2) 0.9502(2) 0.2408(2) 0.0187(5) Uani 1 1 d . . .
H22 H 0.8655 0.9394 0.3024 0.022 Uiso 1 1 calc R . .
C23 C 0.9801(2) 1.0490(2) 0.25584(19) 0.0168(5) Uani 1 1 d . . .
C24 C 1.0401(2) 1.1344(2) 0.3652(2) 0.0173(5) Uani 1 1 d . . .
C25 C 1.1599(3) 1.2100(2) 0.3823(2) 0.0241(6) Uani 1 1 d . . .
H25 H 1.1985 1.2083 0.3244 0.029 Uiso 1 1 calc R . .
C26 C 1.2216(3) 1.2873(3) 0.4848(2) 0.0314(7) Uani 1 1 d . . .
H26 H 1.3023 1.3364 0.4954 0.038 Uiso 1 1 calc R . .
C27 C 1.1654(3) 1.2926(2) 0.5714(2) 0.0279(6) Uani 1 1 d . . .
H27 H 1.2078 1.3449 0.6402 0.033 Uiso 1 1 calc R . .
C28 C 1.0447(3) 1.2193(2) 0.5554(2) 0.0264(6) Uani 1 1 d . . .
H28 H 1.0056 1.2230 0.6134 0.032 Uiso 1 1 calc R . .
C29 C 0.9824(3) 1.1408(2) 0.4530(2) 0.0232(5) Uani 1 1 d . . .
H29 H 0.9017 1.0920 0.4427 0.028 Uiso 1 1 calc R . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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 180.0 . 2_775 ?
O1 Pu1 N1 106.70(7) . 2_775 ?
O1 Pu1 N1 73.29(7) 2_775 2_775 ?
O1 Pu1 N1 73.29(7) . . ?
O1 Pu1 N1 106.71(7) 2_775 . ?
N1 Pu1 N1 180.00(7) 2_775 . ?
O1 Pu1 I1 89.79(5) . . ?
O1 Pu1 I1 90.21(5) 2_775 . ?
N1 Pu1 I1 91.36(5) 2_775 . ?
N1 Pu1 I1 88.64(5) . . ?
O1 Pu1 I1 90.21(5) . 2_775 ?
O1 Pu1 I1 89.79(5) 2_775 2_775 ?
N1 Pu1 I1 88.64(5) 2_775 2_775 ?
N1 Pu1 I1 91.36(5) . 2_775 ?
I1 Pu1 I1 180.0 . 2_775 ?
C23 O1 Pu1 142.69(16) . . ?
C21 N1 C1 120.7(2) . . ?
C21 N1 Pu1 133.84(16) . . ?
C1 N1 Pu1 105.33(14) . . ?
C6 C1 C2 121.1(2) . . ?
C6 C1 N1 119.7(2) . . ?
C2 C1 N1 119.0(2) . . ?
C3 C2 C1 119.9(2) . . ?
C2 C3 C4 118.1(2) . . ?
C2 C3 C11 121.8(2) . . ?
C4 C3 C11 120.0(2) . . ?
C5 C4 C3 122.9(2) . . ?
C4 C5 C6 117.3(2) . . ?
C4 C5 C7 123.7(2) . . ?
C6 C5 C7 118.9(2) . . ?
C1 C6 C5 120.5(2) . . ?
C5 C7 C9 112.4(2) . . ?
C5 C7 C8 109.5(2) . . ?
C9 C7 C8 108.3(3) . . ?
C5 C7 C10 108.9(2) . . ?
C9 C7 C10 108.4(2) . . ?
C8 C7 C10 109.4(2) . . ?
C14 C11 C13 109.7(3) . . ?
C14 C11 C12 107.3(2) . . ?
C13 C11 C12 108.6(3) . . ?
C14 C11 C3 112.0(2) . . ?
C13 C11 C3 110.3(2) . . ?
C12 C11 C3 108.9(2) . . ?
C16 C15 C20 119.1(2) . . ?
C16 C15 C21 120.3(2) . . ?
C20 C15 C21 120.7(2) . . ?
C15 C16 C17 120.1(3) . . ?
C18 C17 C16 120.3(3) . . ?
C19 C18 C17 120.2(3) . . ?
C18 C19 C20 119.7(3) . . ?
C15 C20 C19 120.6(3) . . ?
N1 C21 C22 123.2(2) . . ?
N1 C21 C15 120.2(2) . . ?
C22 C21 C15 116.5(2) . . ?
C23 C22 C21 125.1(2) . . ?
O1 C23 C22 121.8(2) . . ?
O1 C23 C24 116.3(2) . . ?
C22 C23 C24 121.8(2) . . ?
C25 C24 C29 118.6(2) . . ?
C25 C24 C23 119.0(2) . . ?
C29 C24 C23 122.3(2) . . ?
C26 C25 C24 120.4(3) . . ?
C27 C26 C25 120.9(3) . . ?
C26 C27 C28 119.5(3) . . ?
C29 C28 C27 120.1(3) . . ?
C28 C29 C24 120.5(2) . . ?
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 2.1727(17) . ?
Pu1 O1 2.1728(17) 2_775 ?
Pu1 N1 2.3634(19) 2_775 ?
Pu1 N1 2.3635(19) . ?
Pu1 I1 2.9859(3) . ?
Pu1 I1 2.9859(3) 2_775 ?
O1 C23 1.306(3) . ?
N1 C21 1.318(3) . ?
N1 C1 1.439(3) . ?
C1 C6 1.376(4) . ?
C1 C2 1.396(3) . ?
C2 C3 1.382(4) . ?
C3 C4 1.398(4) . ?
C3 C11 1.536(3) . ?
C4 C5 1.395(3) . ?
C5 C6 1.399(3) . ?
C5 C7 1.523(4) . ?
C7 C9 1.529(4) . ?
C7 C8 1.539(4) . ?
C7 C10 1.541(4) . ?
C11 C14 1.519(4) . ?
C11 C13 1.522(4) . ?
C11 C12 1.526(4) . ?
C15 C16 1.379(4) . ?
C15 C20 1.388(4) . ?
C15 C21 1.498(3) . ?
C16 C17 1.384(4) . ?
C17 C18 1.381(5) . ?
C18 C19 1.366(5) . ?
C19 C20 1.388(4) . ?
C21 C22 1.413(3) . ?
C22 C23 1.382(3) . ?
C23 C24 1.478(3) . ?
C24 C25 1.395(3) . ?
C24 C29 1.397(3) . ?
C25 C26 1.381(4) . ?
C26 C27 1.377(4) . ?
C27 C28 1.390(4) . ?
C28 C29 1.387(4) . ?
